# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ligand _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 Fe N4 O4' _chemical_formula_sum 'C30 H30 Fe N4 O4' _chemical_formula_weight 566.43 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.396(5) _cell_length_b 18.625(5) _cell_length_c 12.487(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 117.298(5) _cell_angle_gamma 90.000(5) _cell_volume 2561.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 702 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.87 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.634 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.0734512 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13591 _diffrn_reflns_av_R_equivalents 0.1253 _diffrn_reflns_av_unetI/netI 0.1515 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4748 _reflns_number_gt 2502 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1122P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4748 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1397 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.2232 _refine_ls_wR_factor_gt 0.1579 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _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 C1 C 0.9230(5) 0.5550(3) 0.8645(5) 0.0238(13) Uani 1 1 d . . . C2 C 1.0302(5) 0.5932(3) 0.8824(5) 0.0272(14) Uani 1 1 d . . . H2A H 1.0775 0.5855 0.8385 0.033 Uiso 1 1 calc R . . C3 C 1.0570(6) 0.6433(3) 0.9775(6) 0.0319(15) Uani 1 1 d . . . H3 H 1.1257 0.6767 1.0100 0.038 Uiso 1 1 calc R . . C4 C 0.9654(6) 0.6373(3) 1.0160(5) 0.0303(15) Uani 1 1 d . . . H4 H 0.9605 0.6662 1.0793 0.036 Uiso 1 1 calc R . . C5 C 0.8822(6) 0.5843(3) 0.9471(5) 0.0278(14) Uani 1 1 d . . . H5 H 0.8102 0.5692 0.9544 0.033 Uiso 1 1 calc R . . C6 C 0.8741(5) 0.7197(3) 0.6886(5) 0.0232(13) Uani 1 1 d . . . H6 H 0.9249 0.7134 0.6479 0.028 Uiso 1 1 calc R . . C7 C 0.7622(5) 0.6825(3) 0.6605(5) 0.0227(13) Uani 1 1 d . . . C8 C 0.7192(5) 0.7080(3) 0.7432(5) 0.0288(15) Uani 1 1 d . . . H8 H 0.6455 0.6917 0.7463 0.035 Uiso 1 1 calc R . . C9 C 0.8015(5) 0.7604(3) 0.8195(5) 0.0281(14) Uani 1 1 d . . . H9 H 0.7950 0.7869 0.8841 0.034 Uiso 1 1 calc R . . C10 C 0.7034(5) 0.6288(3) 0.5638(5) 0.0238(13) Uani 1 1 d . . . C11 C 0.5853(5) 0.5974(3) 0.5496(6) 0.0312(15) Uani 1 1 d . . . H11A H 0.5736 0.5508 0.5133 0.047 Uiso 1 1 calc R . . H11B H 0.5194 0.6283 0.4991 0.047 Uiso 1 1 calc R . . H11C H 0.5876 0.5933 0.6272 0.047 Uiso 1 1 calc R . . C12 C 0.8645(5) 0.4985(3) 0.7742(5) 0.0235(13) Uani 1 1 d . . . C13 C 0.7492(5) 0.4646(3) 0.7652(6) 0.0305(15) Uani 1 1 d . . . H13A H 0.6945 0.4549 0.6822 0.046 Uiso 1 1 calc R . . H13B H 0.7114 0.4969 0.7977 0.046 Uiso 1 1 calc R . . H13C H 0.7689 0.4205 0.8099 0.046 Uiso 1 1 calc R . . C14 C 0.7401(5) 0.5538(3) 0.3356(5) 0.0253(14) Uani 1 1 d . . . H14 H 0.8103 0.5786 0.3488 0.030 Uiso 1 1 calc R . . C15 C 0.8870(5) 0.4154(3) 0.5443(5) 0.0257(14) Uani 1 1 d . . . H15 H 0.9500 0.4428 0.5449 0.031 Uiso 1 1 calc R . . C16 C 0.6849(5) 0.5054(3) 0.2339(5) 0.0249(14) Uani 1 1 d . . . C17 C 0.5826(5) 0.4640(3) 0.2147(5) 0.0242(14) Uani 1 1 d . . . C18 C 0.5323(5) 0.4166(3) 0.1165(6) 0.0274(14) Uani 1 1 d . . . C19 C 0.5815(6) 0.4124(3) 0.0378(5) 0.0324(15) Uani 1 1 d . . . H19 H 0.5469 0.3816 -0.0280 0.039 Uiso 1 1 calc R . . C20 C 0.6824(5) 0.4537(3) 0.0546(5) 0.0266(14) Uani 1 1 d . . . H20 H 0.7142 0.4503 0.0003 0.032 Uiso 1 1 calc R . . C21 C 0.7344(5) 0.4992(3) 0.1519(6) 0.0285(14) Uani 1 1 d . . . H21 H 0.8023 0.5261 0.1639 0.034 Uiso 1 1 calc R . . C22 C 0.8291(5) 0.3619(3) 0.4518(5) 0.0255(14) Uani 1 1 d . . . C23 C 0.7309(5) 0.3207(3) 0.4442(5) 0.0240(13) Uani 1 1 d . . . C24 C 0.8692(6) 0.3507(3) 0.3638(6) 0.0313(15) Uani 1 1 d . . . H24 H 0.9354 0.3764 0.3682 0.038 Uiso 1 1 calc R . . C25 C 0.8111(6) 0.3019(3) 0.2709(6) 0.0324(15) Uani 1 1 d . . . H25 H 0.8377 0.2953 0.2130 0.039 Uiso 1 1 calc R . . C26 C 0.7127(5) 0.2628(3) 0.2651(5) 0.0279(14) Uani 1 1 d . . . H26 H 0.6734 0.2305 0.2023 0.033 Uiso 1 1 calc R . . C27 C 0.6723(5) 0.2712(3) 0.3505(5) 0.0252(14) Uani 1 1 d . . . C28 C 0.8970(6) 0.7672(3) 0.7846(5) 0.0308(15) Uani 1 1 d . . . H28 H 0.9675 0.7990 0.8227 0.037 Uiso 1 1 calc R . . C29 C 0.3789(6) 0.3290(3) 0.0079(6) 0.0360(16) Uani 1 1 d . . . H29A H 0.3487 0.3558 -0.0660 0.054 Uiso 1 1 calc R . . H29B H 0.3130 0.3043 0.0121 0.054 Uiso 1 1 calc R . . H29C H 0.4379 0.2948 0.0105 0.054 Uiso 1 1 calc R . . C30 C 0.5135(6) 0.1863(3) 0.2571(6) 0.0350(16) Uani 1 1 d . . . H30A H 0.4836 0.2106 0.1811 0.053 Uiso 1 1 calc R . . H30B H 0.4466 0.1664 0.2660 0.053 Uiso 1 1 calc R . . H30C H 0.5674 0.1484 0.2602 0.053 Uiso 1 1 calc R . . N1 N 0.7571(4) 0.6139(3) 0.4995(4) 0.0252(12) Uani 1 1 d . . . N2 N 0.6943(4) 0.5631(3) 0.4076(4) 0.0250(11) Uani 1 1 d . . . N3 N 0.9144(4) 0.4810(3) 0.7080(4) 0.0258(12) Uani 1 1 d . . . N4 N 0.8526(4) 0.4258(3) 0.6262(4) 0.0269(12) Uani 1 1 d . . . O1 O 0.5305(4) 0.4680(2) 0.2878(4) 0.0314(10) Uani 1 1 d . . . H1 H 0.5669 0.4973 0.3413 0.047 Uiso 1 1 calc R . . O2 O 0.6890(4) 0.3276(2) 0.5267(4) 0.0296(10) Uani 1 1 d . . . H2 H 0.7213 0.3623 0.5699 0.044 Uiso 1 1 calc R . . O3 O 0.4344(4) 0.3772(2) 0.1080(4) 0.0335(11) Uani 1 1 d . . . O4 O 0.5770(4) 0.2356(2) 0.3517(4) 0.0298(10) Uani 1 1 d . . . Fe1 Fe 0.88870(7) 0.66346(4) 0.83632(7) 0.0232(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(3) 0.026(3) 0.017(3) 0.004(3) 0.008(3) 0.003(3) C2 0.024(3) 0.025(3) 0.026(4) 0.003(3) 0.005(3) 0.002(3) C3 0.031(3) 0.027(4) 0.027(4) -0.002(3) 0.004(3) 0.003(3) C4 0.042(4) 0.029(4) 0.020(3) 0.002(3) 0.014(3) 0.005(3) C5 0.036(4) 0.026(3) 0.024(3) 0.006(3) 0.016(3) 0.007(3) C6 0.022(3) 0.029(3) 0.019(3) 0.002(3) 0.009(3) -0.003(3) C7 0.027(3) 0.023(3) 0.015(3) 0.004(2) 0.007(3) 0.005(2) C8 0.027(3) 0.032(4) 0.027(4) 0.005(3) 0.012(3) 0.008(3) C9 0.038(4) 0.025(3) 0.022(3) -0.002(3) 0.014(3) 0.007(3) C10 0.026(3) 0.022(3) 0.021(3) 0.006(3) 0.008(3) 0.000(3) C11 0.030(3) 0.042(4) 0.024(3) -0.003(3) 0.014(3) -0.005(3) C12 0.022(3) 0.022(3) 0.022(3) 0.009(3) 0.006(3) 0.004(2) C13 0.027(3) 0.034(4) 0.028(4) -0.001(3) 0.011(3) -0.001(3) C14 0.021(3) 0.027(3) 0.026(3) 0.002(3) 0.010(3) 0.000(3) C15 0.017(3) 0.029(3) 0.027(3) 0.006(3) 0.007(3) 0.003(3) C16 0.018(3) 0.030(3) 0.027(3) 0.006(3) 0.011(3) 0.003(3) C17 0.023(3) 0.027(3) 0.023(3) 0.005(3) 0.011(3) 0.006(3) C18 0.024(3) 0.028(3) 0.029(4) 0.000(3) 0.011(3) 0.001(3) C19 0.032(4) 0.044(4) 0.014(3) -0.005(3) 0.005(3) 0.000(3) C20 0.027(3) 0.037(4) 0.019(3) -0.001(3) 0.014(3) 0.002(3) C21 0.027(3) 0.030(4) 0.029(4) 0.001(3) 0.014(3) -0.003(3) C22 0.022(3) 0.026(3) 0.026(3) 0.004(3) 0.009(3) 0.007(3) C23 0.030(3) 0.025(3) 0.020(3) 0.004(3) 0.014(3) 0.006(3) C24 0.029(3) 0.040(4) 0.031(4) 0.001(3) 0.019(3) 0.002(3) C25 0.034(4) 0.034(4) 0.032(4) -0.003(3) 0.018(3) 0.004(3) C26 0.028(3) 0.028(3) 0.025(3) -0.001(3) 0.009(3) 0.007(3) C27 0.023(3) 0.024(3) 0.024(3) 0.004(3) 0.007(3) 0.001(3) C28 0.036(4) 0.030(4) 0.023(4) -0.004(3) 0.010(3) -0.005(3) C29 0.035(4) 0.038(4) 0.030(4) -0.012(3) 0.010(3) -0.009(3) C30 0.033(4) 0.040(4) 0.031(4) -0.006(3) 0.014(3) -0.005(3) N1 0.028(3) 0.027(3) 0.022(3) 0.001(2) 0.014(2) -0.001(2) N2 0.026(3) 0.029(3) 0.020(3) -0.002(2) 0.010(2) -0.003(2) N3 0.029(3) 0.026(3) 0.024(3) -0.003(2) 0.014(2) 0.000(2) N4 0.026(3) 0.029(3) 0.023(3) -0.002(2) 0.009(2) 0.003(2) O1 0.027(2) 0.045(3) 0.028(3) -0.010(2) 0.017(2) -0.009(2) O2 0.035(2) 0.036(3) 0.023(2) -0.0055(19) 0.018(2) -0.008(2) O3 0.035(2) 0.037(3) 0.029(3) -0.005(2) 0.015(2) -0.011(2) O4 0.027(2) 0.033(2) 0.031(3) -0.007(2) 0.015(2) -0.0069(19) Fe1 0.0243(5) 0.0253(5) 0.0200(5) -0.0012(4) 0.0101(4) 0.0012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.431(8) . ? C1 C5 1.447(8) . ? C1 C12 1.468(8) . ? C1 Fe1 2.061(6) . ? C2 C3 1.426(8) . ? C2 Fe1 2.048(6) . ? C3 C4 1.426(9) . ? C3 Fe1 2.056(6) . ? C4 C5 1.402(8) . ? C4 Fe1 2.054(6) . ? C5 Fe1 2.048(6) . ? C6 C28 1.410(8) . ? C6 C7 1.444(8) . ? C6 Fe1 2.057(6) . ? C7 C8 1.443(8) . ? C7 C10 1.477(8) . ? C7 Fe1 2.061(6) . ? C8 C9 1.418(8) . ? C8 Fe1 2.053(6) . ? C9 C28 1.442(8) . ? C9 Fe1 2.065(6) . ? C10 N1 1.287(7) . ? C10 C11 1.510(8) . ? C12 N3 1.281(7) . ? C12 C13 1.518(8) . ? C14 N2 1.276(7) . ? C14 C16 1.448(8) . ? C15 N4 1.290(7) . ? C15 C22 1.443(8) . ? C16 C17 1.408(8) . ? C16 C21 1.419(8) . ? C17 O1 1.340(7) . ? C17 C18 1.404(8) . ? C18 C19 1.377(8) . ? C18 O3 1.379(7) . ? C19 C20 1.399(8) . ? C20 C21 1.375(8) . ? C22 C23 1.405(8) . ? C22 C24 1.414(8) . ? C23 O2 1.355(7) . ? C23 C27 1.403(8) . ? C24 C25 1.387(9) . ? C25 C26 1.394(8) . ? C26 C27 1.380(8) . ? C27 O4 1.360(7) . ? C28 Fe1 2.054(6) . ? C29 O3 1.433(7) . ? C30 O4 1.416(7) . ? N1 N2 1.414(6) . ? N3 N4 1.403(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 107.7(5) . . ? C2 C1 C12 124.9(5) . . ? C5 C1 C12 127.4(5) . . ? C2 C1 Fe1 69.1(3) . . ? C5 C1 Fe1 68.9(3) . . ? C12 C1 Fe1 125.5(4) . . ? C3 C2 C1 107.5(5) . . ? C3 C2 Fe1 70.0(3) . . ? C1 C2 Fe1 70.1(3) . . ? C2 C3 C4 108.2(5) . . ? C2 C3 Fe1 69.4(3) . . ? C4 C3 Fe1 69.7(3) . . ? C5 C4 C3 108.9(5) . . ? C5 C4 Fe1 69.8(3) . . ? C3 C4 Fe1 69.8(3) . . ? C4 C5 C1 107.7(5) . . ? C4 C5 Fe1 70.2(3) . . ? C1 C5 Fe1 69.9(3) . . ? C28 C6 C7 107.7(5) . . ? C28 C6 Fe1 69.8(3) . . ? C7 C6 Fe1 69.6(3) . . ? C8 C7 C6 107.3(5) . . ? C8 C7 C10 127.0(5) . . ? C6 C7 C10 125.6(5) . . ? C8 C7 Fe1 69.2(3) . . ? C6 C7 Fe1 69.3(3) . . ? C10 C7 Fe1 127.1(4) . . ? C9 C8 C7 108.6(5) . . ? C9 C8 Fe1 70.3(3) . . ? C7 C8 Fe1 69.8(3) . . ? C8 C9 C28 107.2(5) . . ? C8 C9 Fe1 69.4(3) . . ? C28 C9 Fe1 69.1(3) . . ? N1 C10 C7 117.0(5) . . ? N1 C10 C11 126.5(5) . . ? C7 C10 C11 116.5(5) . . ? N3 C12 C1 117.6(5) . . ? N3 C12 C13 124.3(6) . . ? C1 C12 C13 118.1(5) . . ? N2 C14 C16 121.2(5) . . ? N4 C15 C22 121.0(5) . . ? C17 C16 C21 119.1(6) . . ? C17 C16 C14 121.1(5) . . ? C21 C16 C14 119.8(5) . . ? O1 C17 C18 118.0(5) . . ? O1 C17 C16 122.2(5) . . ? C18 C17 C16 119.8(5) . . ? C19 C18 O3 125.2(6) . . ? C19 C18 C17 119.6(6) . . ? O3 C18 C17 115.1(5) . . ? C18 C19 C20 121.3(6) . . ? C21 C20 C19 119.8(6) . . ? C20 C21 C16 120.3(6) . . ? C23 C22 C24 118.0(6) . . ? C23 C22 C15 121.9(5) . . ? C24 C22 C15 120.1(6) . . ? O2 C23 C27 117.6(5) . . ? O2 C23 C22 121.3(5) . . ? C27 C23 C22 121.1(5) . . ? C25 C24 C22 120.9(6) . . ? C24 C25 C26 119.5(6) . . ? C27 C26 C25 121.4(6) . . ? O4 C27 C26 125.3(5) . . ? O4 C27 C23 115.6(5) . . ? C26 C27 C23 119.1(6) . . ? C6 C28 C9 109.2(5) . . ? C6 C28 Fe1 70.0(3) . . ? C9 C28 Fe1 69.9(3) . . ? C10 N1 N2 113.6(5) . . ? C14 N2 N1 113.9(5) . . ? C12 N3 N4 113.1(5) . . ? C15 N4 N3 114.8(5) . . ? C18 O3 C29 117.0(5) . . ? C27 O4 C30 117.4(5) . . ? C2 Fe1 C5 69.1(2) . . ? C2 Fe1 C8 160.0(2) . . ? C5 Fe1 C8 109.0(2) . . ? C2 Fe1 C28 122.0(2) . . ? C5 Fe1 C28 155.8(2) . . ? C8 Fe1 C28 68.2(2) . . ? C2 Fe1 C4 68.5(2) . . ? C5 Fe1 C4 40.0(2) . . ? C8 Fe1 C4 123.7(2) . . ? C28 Fe1 C4 120.1(2) . . ? C2 Fe1 C3 40.7(2) . . ? C5 Fe1 C3 68.2(3) . . ? C8 Fe1 C3 158.7(2) . . ? C28 Fe1 C3 105.3(3) . . ? C4 Fe1 C3 40.6(2) . . ? C2 Fe1 C6 106.8(2) . . ? C5 Fe1 C6 163.4(2) . . ? C8 Fe1 C6 68.9(2) . . ? C28 Fe1 C6 40.1(2) . . ? C4 Fe1 C6 155.1(2) . . ? C3 Fe1 C6 120.0(2) . . ? C2 Fe1 C7 123.0(2) . . ? C5 Fe1 C7 126.6(2) . . ? C8 Fe1 C7 41.1(2) . . ? C28 Fe1 C7 68.1(2) . . ? C4 Fe1 C7 161.7(2) . . ? C3 Fe1 C7 157.2(3) . . ? C6 Fe1 C7 41.1(2) . . ? C2 Fe1 C1 40.8(2) . . ? C5 Fe1 C1 41.2(2) . . ? C8 Fe1 C1 124.7(2) . . ? C28 Fe1 C1 159.9(2) . . ? C4 Fe1 C1 68.0(2) . . ? C3 Fe1 C1 68.1(2) . . ? C6 Fe1 C1 125.4(2) . . ? C7 Fe1 C1 110.3(2) . . ? C2 Fe1 C9 158.2(2) . . ? C5 Fe1 C9 121.2(2) . . ? C8 Fe1 C9 40.3(2) . . ? C28 Fe1 C9 41.0(2) . . ? C4 Fe1 C9 106.1(2) . . ? C3 Fe1 C9 121.6(2) . . ? C6 Fe1 C9 68.7(2) . . ? C7 Fe1 C9 68.5(2) . . ? C1 Fe1 C9 158.7(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.593 _refine_diff_density_min -1.017 _refine_diff_density_rms 0.175 _database_code_depnum_ccdc_archive 'CCDC 941857' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Zn-Dy _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H31 Dy Fe N6 O12 Zn' _chemical_formula_sum 'C32 H31 Dy Fe N6 O12 Zn' _chemical_formula_weight 975.37 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.282(5) _cell_length_b 11.873(5) _cell_length_c 13.438(5) _cell_angle_alpha 72.211(5) _cell_angle_beta 86.530(5) _cell_angle_gamma 88.731(5) _cell_volume 1710.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1677 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 22.49 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 966.0 _exptl_absorpt_coefficient_mu 3.349 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.809671 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9341 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_unetI/netI 0.0922 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6258 _reflns_number_gt 4463 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Carbon atoms C14, C17, C22 and C23 were having large anisotropic diplacement parameteres and hence refined isotropically. ; _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^)+(0.1075P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6258 _refine_ls_number_parameters 483 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1894 _refine_ls_wR_factor_gt 0.1357 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _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 0.79191(4) 0.08578(5) 0.22753(4) 0.02466(19) Uani 1 1 d . . . Zn1 Zn 0.55292(10) 0.25662(10) 0.26532(9) 0.0213(3) Uani 1 1 d . . . Fe1 Fe 0.16851(13) 0.59294(13) 0.32214(11) 0.0228(4) Uani 1 1 d . . . O1 O 0.6730(6) 0.1378(6) 0.3517(5) 0.0229(16) Uani 1 1 d . . . O2 O 0.8348(6) -0.0212(7) 0.4157(5) 0.0303(18) Uani 1 1 d . . . O4 O 0.7460(6) 0.0598(6) 0.0551(6) 0.0279(17) Uani 1 1 d . . . O8 O 0.8676(6) -0.1099(6) 0.2324(5) 0.0271(17) Uani 1 1 d . . . O11 O 0.9936(7) 0.1193(8) 0.2686(6) 0.038(2) Uani 1 1 d . . . O10 O 0.9705(7) 0.1190(8) 0.1109(7) 0.042(2) Uani 1 1 d . . . O5 O 0.6582(6) 0.3932(6) 0.1903(6) 0.0283(17) Uani 1 1 d . . . O7 O 0.6819(6) -0.1005(6) 0.2835(5) 0.0264(17) Uani 1 1 d . . . O3 O 0.6052(6) 0.1529(6) 0.1689(6) 0.0255(16) Uani 1 1 d . . . C13 C 0.7531(9) -0.0039(8) 0.4933(8) 0.021(2) Uani 1 1 d . . . C9 C 0.5843(8) 0.1095(8) 0.5243(8) 0.018(2) Uani 1 1 d . . . C10 C 0.5880(10) 0.0482(9) 0.6320(7) 0.024(2) Uani 1 1 d . . . H10 H 0.5316 0.0654 0.6788 0.029 Uiso 1 1 calc R . . N6 N 1.0391(8) 0.1377(9) 0.1760(7) 0.032(2) Uani 1 1 d . . . N1 N 0.3872(7) 0.3567(8) 0.4162(6) 0.0223(19) Uani 1 1 d . . . C26 C 0.1874(9) 0.5241(9) 0.1995(8) 0.024(2) Uani 1 1 d . . . O9 O 0.7579(7) -0.2711(7) 0.2811(7) 0.045(2) Uani 1 1 d . . . C6 C 0.4150(9) 0.4667(9) 0.3897(7) 0.020(2) Uani 1 1 d . . . C17 C 0.6420(9) 0.1054(8) 0.0139(7) 0.019(2) Uani 1 1 d U . . N3 N 0.3012(7) 0.3533(7) 0.2124(6) 0.0216(19) Uani 1 1 d . . . C18 C 0.6101(10) 0.1049(9) -0.0827(8) 0.028(2) Uani 1 1 d . . . H18 H 0.6607 0.0718 -0.1235 0.033 Uiso 1 1 calc R . . N4 N 0.4035(7) 0.2986(7) 0.1782(6) 0.0183(18) Uani 1 1 d . . . O6 O 0.8152(6) 0.2880(7) 0.1651(6) 0.0291(17) Uani 1 1 d . . . C14 C 0.6704(8) 0.0829(8) 0.4552(7) 0.017(2) Uani 1 1 d U . . C7 C 0.5287(9) 0.5235(9) 0.3474(8) 0.025(2) Uani 1 1 d . . . H7A H 0.5920 0.4676 0.3693 0.038 Uiso 1 1 calc R . . H7B H 0.5392 0.5897 0.3728 0.038 Uiso 1 1 calc R . . H7C H 0.5296 0.5503 0.2723 0.038 Uiso 1 1 calc R . . N5 N 0.7684(8) -0.1662(8) 0.2676(7) 0.030(2) Uani 1 1 d . . . C25 C 0.3895(9) 0.5414(9) 0.1003(7) 0.023(2) Uani 1 1 d . . . H25A H 0.4627 0.4981 0.1033 0.035 Uiso 1 1 calc R . . H25B H 0.4014 0.6111 0.1204 0.035 Uiso 1 1 calc R . . H25C H 0.3634 0.5638 0.0302 0.035 Uiso 1 1 calc R . . C16 C 0.8210(10) 0.0049(10) -0.0086(9) 0.031(3) Uani 1 1 d . . . H16A H 0.7770 -0.0553 -0.0243 0.047 Uiso 1 1 calc R . . H16B H 0.8891 -0.0300 0.0289 0.047 Uiso 1 1 calc R . . H16C H 0.8464 0.0637 -0.0726 0.047 Uiso 1 1 calc R . . C21 C 0.4634(9) 0.2108(8) 0.0384(7) 0.021(2) Uani 1 1 d . . . C19 C 0.4996(10) 0.1553(9) -0.1208(8) 0.025(2) Uani 1 1 d . . . H19 H 0.4756 0.1519 -0.1848 0.030 Uiso 1 1 calc R . . C22 C 0.5713(8) 0.1578(8) 0.0770(7) 0.017(2) Uani 1 1 d U . . C30 C 0.1586(9) 0.6478(9) 0.1607(7) 0.024(2) Uani 1 1 d . . . H30 H 0.2080 0.7088 0.1107 0.029 Uiso 1 1 calc R . . C24 C 0.2967(8) 0.4648(9) 0.1739(7) 0.017(2) Uani 1 1 d . . . C5 C 0.3077(9) 0.6728(9) 0.3596(7) 0.021(2) Uani 1 1 d . . . H5 H 0.3671 0.7224 0.3103 0.025 Uiso 1 1 calc R . . C3 C 0.1389(10) 0.6134(10) 0.4645(8) 0.030(3) Uani 1 1 d . . . H3 H 0.0610 0.6149 0.5006 0.036 Uiso 1 1 calc R . . C27 C 0.0920(8) 0.4674(10) 0.2717(9) 0.028(2) Uani 1 1 d . . . H27 H 0.0860 0.3828 0.3099 0.033 Uiso 1 1 calc R . . C23 C 0.3856(8) 0.2727(8) 0.0943(7) 0.018(2) Uani 1 1 d U . . H23 H 0.3129 0.2969 0.0655 0.021 Uiso 1 1 calc R . . O12 O 1.1413(7) 0.1709(8) 0.1515(7) 0.046(2) Uani 1 1 d . . . C4 C 0.2025(9) 0.7127(9) 0.4003(8) 0.024(2) Uani 1 1 d . . . H4 H 0.1745 0.7949 0.3816 0.028 Uiso 1 1 calc R . . C29 C 0.0499(9) 0.6670(10) 0.2090(8) 0.027(2) Uani 1 1 d . . . H29 H 0.0103 0.7437 0.1982 0.032 Uiso 1 1 calc R . . C11 C 0.6737(9) -0.0370(9) 0.6697(9) 0.029(2) Uani 1 1 d . . . H11 H 0.6748 -0.0766 0.7410 0.034 Uiso 1 1 calc R . . C20 C 0.4295(8) 0.2085(9) -0.0615(7) 0.018(2) Uani 1 1 d . . . H20 H 0.3584 0.2438 -0.0867 0.021 Uiso 1 1 calc R . . C1 C 0.3154(10) 0.5460(10) 0.4085(8) 0.029(3) Uani 1 1 d . . . C8 C 0.4965(8) 0.2013(9) 0.4968(7) 0.020(2) Uani 1 1 d . . . H8 H 0.4440 0.2068 0.5512 0.024 Uiso 1 1 calc R . . C15 C 0.9223(10) -0.1141(11) 0.4530(9) 0.037(3) Uani 1 1 d . . . H15A H 0.9565 -0.1049 0.5137 0.055 Uiso 1 1 calc R . . H15B H 0.9836 -0.1087 0.3990 0.055 Uiso 1 1 calc R . . H15C H 0.8845 -0.1898 0.4708 0.055 Uiso 1 1 calc R . . C32 C 0.8301(11) 0.4959(10) 0.0971(9) 0.037(3) Uani 1 1 d . . . H32A H 0.9137 0.4833 0.1057 0.056 Uiso 1 1 calc R . . H32B H 0.8035 0.5588 0.1241 0.056 Uiso 1 1 calc R . . H32C H 0.8153 0.5168 0.0241 0.056 Uiso 1 1 calc R . . C12 C 0.7581(10) -0.0626(9) 0.5999(8) 0.027(2) Uani 1 1 d . . . H12A H 0.8173 -0.1183 0.6242 0.032 Uiso 1 1 calc R . . C31 C 0.7632(9) 0.3829(10) 0.1564(8) 0.027(2) Uani 1 1 d . . . N2 N 0.4805(7) 0.2776(7) 0.4065(7) 0.0212(19) Uani 1 1 d . . . C28 C 0.0065(9) 0.5564(9) 0.2774(8) 0.026(2) Uani 1 1 d . . . H28 H -0.0682 0.5439 0.3204 0.032 Uiso 1 1 calc R . . C2 C 0.2110(10) 0.5102(9) 0.4720(8) 0.027(2) Uani 1 1 d . . . H2 H 0.1903 0.4288 0.5130 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0201(3) 0.0322(3) 0.0225(3) -0.0106(2) 0.0008(2) 0.0089(2) Zn1 0.0193(6) 0.0289(7) 0.0170(6) -0.0095(5) -0.0005(5) 0.0092(5) Fe1 0.0202(8) 0.0264(8) 0.0218(8) -0.0088(6) 0.0036(6) 0.0080(6) O1 0.014(3) 0.038(4) 0.020(4) -0.014(3) -0.004(3) 0.012(3) O2 0.025(4) 0.041(5) 0.025(4) -0.012(3) -0.003(3) 0.015(3) O4 0.024(4) 0.033(4) 0.035(4) -0.025(4) 0.009(3) 0.002(3) O8 0.016(4) 0.037(4) 0.024(4) -0.005(3) 0.004(3) 0.007(3) O11 0.027(4) 0.054(5) 0.030(5) -0.008(4) -0.006(4) -0.001(4) O10 0.022(4) 0.058(6) 0.057(6) -0.038(5) 0.012(4) 0.004(4) O5 0.019(4) 0.036(4) 0.030(4) -0.011(3) 0.006(3) 0.010(3) O7 0.018(4) 0.035(4) 0.025(4) -0.008(3) 0.002(3) 0.013(3) O3 0.022(4) 0.025(4) 0.031(4) -0.013(3) 0.007(3) 0.008(3) C13 0.017(5) 0.019(5) 0.027(6) -0.007(4) 0.004(4) -0.005(4) C9 0.010(4) 0.019(5) 0.028(5) -0.012(4) -0.005(4) -0.003(4) C10 0.038(6) 0.025(5) 0.009(5) -0.007(4) 0.008(4) -0.010(5) N6 0.019(5) 0.047(6) 0.035(6) -0.019(5) 0.001(4) 0.006(4) N1 0.021(4) 0.034(5) 0.013(4) -0.008(4) -0.004(3) 0.013(4) C26 0.019(5) 0.026(6) 0.030(6) -0.012(5) 0.000(4) 0.012(4) O9 0.041(5) 0.025(5) 0.068(6) -0.013(4) 0.003(5) 0.004(4) C6 0.018(5) 0.028(6) 0.013(5) -0.005(4) -0.005(4) 0.008(4) C17 0.019(2) 0.019(2) 0.019(2) -0.0056(11) -0.0010(10) 0.0000(10) N3 0.020(4) 0.026(5) 0.023(4) -0.015(4) 0.000(4) 0.009(4) C18 0.028(6) 0.025(6) 0.029(6) -0.009(5) 0.010(5) -0.005(5) N4 0.016(4) 0.024(4) 0.013(4) -0.004(3) 0.004(3) 0.006(3) O6 0.018(4) 0.035(4) 0.032(4) -0.008(3) 0.005(3) 0.005(3) C14 0.017(2) 0.018(2) 0.016(2) -0.0054(11) -0.0012(10) -0.0001(10) C7 0.032(6) 0.025(6) 0.025(6) -0.015(5) -0.011(5) 0.014(5) N5 0.033(5) 0.036(6) 0.020(5) -0.010(4) -0.003(4) 0.014(4) C25 0.017(5) 0.035(6) 0.015(5) -0.005(4) 0.005(4) 0.004(4) C16 0.027(6) 0.032(6) 0.038(7) -0.019(5) 0.018(5) 0.006(5) C21 0.021(5) 0.018(5) 0.017(5) 0.001(4) 0.007(4) 0.004(4) C19 0.035(6) 0.028(6) 0.013(5) -0.007(4) -0.011(4) -0.002(5) C22 0.017(2) 0.017(2) 0.017(2) -0.0053(11) -0.0008(10) -0.0002(10) C30 0.028(6) 0.033(6) 0.013(5) -0.010(4) -0.008(4) 0.015(5) C24 0.017(5) 0.024(5) 0.013(5) -0.011(4) -0.003(4) 0.002(4) C5 0.025(5) 0.020(5) 0.017(5) -0.005(4) -0.003(4) 0.014(4) C3 0.036(6) 0.039(7) 0.017(5) -0.012(5) -0.003(5) 0.022(5) C27 0.011(5) 0.037(6) 0.038(6) -0.016(5) 0.000(4) 0.004(4) C23 0.017(2) 0.018(2) 0.018(2) -0.0052(11) -0.0010(10) 0.0005(10) O12 0.020(4) 0.072(7) 0.048(5) -0.021(5) 0.008(4) -0.009(4) C4 0.028(6) 0.028(6) 0.017(5) -0.010(4) -0.004(4) 0.004(5) C29 0.019(5) 0.031(6) 0.030(6) -0.008(5) -0.009(5) 0.011(5) C11 0.027(6) 0.026(6) 0.033(6) -0.010(5) 0.003(5) -0.002(5) C20 0.007(4) 0.030(6) 0.019(5) -0.011(4) -0.007(4) 0.006(4) C1 0.036(6) 0.028(6) 0.025(6) -0.011(5) 0.010(5) -0.007(5) C8 0.010(5) 0.039(6) 0.009(5) -0.006(4) 0.003(4) 0.004(4) C15 0.023(6) 0.054(8) 0.035(7) -0.017(6) -0.008(5) 0.016(6) C32 0.038(7) 0.031(6) 0.039(7) -0.006(5) 0.001(6) -0.001(5) C12 0.033(6) 0.023(5) 0.026(6) -0.009(4) -0.002(5) -0.002(5) C31 0.022(6) 0.041(7) 0.019(5) -0.008(5) -0.005(4) 0.001(5) N2 0.013(4) 0.026(5) 0.028(5) -0.014(4) 0.005(4) 0.002(4) C28 0.023(5) 0.023(6) 0.031(6) -0.007(5) 0.003(5) 0.007(5) C2 0.039(6) 0.023(6) 0.018(5) -0.007(4) 0.010(5) 0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O1 2.299(6) . ? Dy1 O6 2.304(8) . ? Dy1 O3 2.332(7) . ? Dy1 O10 2.438(8) . ? Dy1 O8 2.440(7) . ? Dy1 O11 2.443(8) . ? Dy1 O7 2.448(8) . ? Dy1 O4 2.514(7) . ? Dy1 O2 2.529(7) . ? Dy1 N6 2.866(9) . ? Dy1 N5 2.888(10) . ? Dy1 Zn1 3.4443(16) . ? Zn1 O5 2.000(8) . ? Zn1 O1 2.068(6) . ? Zn1 N4 2.075(8) . ? Zn1 O3 2.096(7) . ? Zn1 N2 2.102(8) . ? Fe1 C3 2.008(10) . ? Fe1 C5 2.018(11) . ? Fe1 C2 2.034(10) . ? Fe1 C27 2.042(11) . ? Fe1 C1 2.050(12) . ? Fe1 C26 2.050(10) . ? Fe1 C28 2.054(11) . ? Fe1 C29 2.062(10) . ? Fe1 C4 2.063(10) . ? Fe1 C30 2.075(9) . ? O1 C14 1.342(11) . ? O2 C13 1.409(11) . ? O2 C15 1.455(12) . ? O4 C17 1.357(12) . ? O4 C16 1.450(10) . ? O8 N5 1.304(12) . ? O11 N6 1.273(12) . ? O10 N6 1.272(12) . ? O5 C31 1.260(12) . ? O7 N5 1.284(10) . ? O3 C22 1.299(11) . ? C13 C14 1.373(13) . ? C13 C12 1.393(14) . ? C9 C14 1.401(13) . ? C9 C10 1.410(13) . ? C9 C8 1.435(13) . ? C10 C11 1.384(14) . ? N6 O12 1.220(12) . ? N1 C6 1.286(13) . ? N1 N2 1.421(10) . ? C26 C27 1.435(15) . ? C26 C30 1.438(14) . ? C26 C24 1.481(12) . ? O9 N5 1.211(12) . ? C6 C7 1.463(15) . ? C6 C1 1.508(14) . ? C17 C18 1.369(14) . ? C17 C22 1.400(13) . ? N3 C24 1.267(12) . ? N3 N4 1.431(10) . ? C18 C19 1.425(15) . ? N4 C23 1.284(12) . ? O6 C31 1.235(12) . ? C25 C24 1.507(14) . ? C21 C22 1.411(13) . ? C21 C20 1.426(13) . ? C21 C23 1.450(13) . ? C19 C20 1.368(13) . ? C30 C29 1.399(14) . ? C5 C4 1.410(13) . ? C5 C1 1.450(14) . ? C3 C4 1.412(16) . ? C3 C2 1.436(13) . ? C27 C28 1.431(13) . ? C29 C28 1.430(15) . ? C11 C12 1.390(14) . ? C1 C2 1.406(15) . ? C8 N2 1.294(12) . ? C32 C31 1.524(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Dy1 O6 81.1(2) . . ? O1 Dy1 O3 67.4(2) . . ? O6 Dy1 O3 76.8(2) . . ? O1 Dy1 O10 149.3(3) . . ? O6 Dy1 O10 74.3(3) . . ? O3 Dy1 O10 122.5(3) . . ? O1 Dy1 O8 128.3(2) . . ? O6 Dy1 O8 148.1(2) . . ? O3 Dy1 O8 122.5(2) . . ? O10 Dy1 O8 73.9(3) . . ? O1 Dy1 O11 104.2(3) . . ? O6 Dy1 O11 75.5(3) . . ? O3 Dy1 O11 152.0(3) . . ? O10 Dy1 O11 52.3(3) . . ? O8 Dy1 O11 84.2(3) . . ? O1 Dy1 O7 85.6(2) . . ? O6 Dy1 O7 156.0(2) . . ? O3 Dy1 O7 79.7(2) . . ? O10 Dy1 O7 123.6(2) . . ? O8 Dy1 O7 52.9(2) . . ? O11 Dy1 O7 127.4(2) . . ? O1 Dy1 O4 131.3(2) . . ? O6 Dy1 O4 95.9(3) . . ? O3 Dy1 O4 64.7(2) . . ? O10 Dy1 O4 70.2(3) . . ? O8 Dy1 O4 74.3(2) . . ? O11 Dy1 O4 122.2(2) . . ? O7 Dy1 O4 78.2(2) . . ? O1 Dy1 O2 64.5(2) . . ? O6 Dy1 O2 119.0(3) . . ? O3 Dy1 O2 125.0(2) . . ? O10 Dy1 O2 112.5(3) . . ? O8 Dy1 O2 73.1(2) . . ? O11 Dy1 O2 67.3(3) . . ? O7 Dy1 O2 71.6(2) . . ? O4 Dy1 O2 144.7(2) . . ? O1 Dy1 N6 127.1(3) . . ? O6 Dy1 N6 71.2(3) . . ? O3 Dy1 N6 140.8(3) . . ? O10 Dy1 N6 26.2(3) . . ? O8 Dy1 N6 79.7(3) . . ? O11 Dy1 N6 26.2(3) . . ? O7 Dy1 N6 132.2(2) . . ? O4 Dy1 N6 96.3(2) . . ? O2 Dy1 N6 90.8(3) . . ? O1 Dy1 N5 107.5(3) . . ? O6 Dy1 N5 169.9(2) . . ? O3 Dy1 N5 101.3(3) . . ? O10 Dy1 N5 99.0(3) . . ? O8 Dy1 N5 26.7(2) . . ? O11 Dy1 N5 106.7(3) . . ? O7 Dy1 N5 26.2(2) . . ? O4 Dy1 N5 74.5(2) . . ? O2 Dy1 N5 70.3(2) . . ? N6 Dy1 N5 106.2(3) . . ? O1 Dy1 Zn1 35.64(16) . . ? O6 Dy1 Zn1 63.01(17) . . ? O3 Dy1 Zn1 36.52(17) . . ? O10 Dy1 Zn1 135.1(2) . . ? O8 Dy1 Zn1 147.75(17) . . ? O11 Dy1 Zn1 123.0(2) . . ? O7 Dy1 Zn1 94.90(15) . . ? O4 Dy1 Zn1 100.18(15) . . ? O2 Dy1 Zn1 100.09(15) . . ? N6 Dy1 Zn1 132.46(19) . . ? N5 Dy1 Zn1 121.10(18) . . ? O5 Zn1 O1 101.5(3) . . ? O5 Zn1 N4 100.8(3) . . ? O1 Zn1 N4 152.6(3) . . ? O5 Zn1 O3 95.4(3) . . ? O1 Zn1 O3 76.2(3) . . ? N4 Zn1 O3 86.1(3) . . ? O5 Zn1 N2 110.2(3) . . ? O1 Zn1 N2 88.1(3) . . ? N4 Zn1 N2 98.9(3) . . ? O3 Zn1 N2 152.3(3) . . ? O5 Zn1 Dy1 84.65(19) . . ? O1 Zn1 Dy1 40.38(18) . . ? N4 Zn1 Dy1 127.5(2) . . ? O3 Zn1 Dy1 41.5(2) . . ? N2 Zn1 Dy1 128.4(2) . . ? C3 Fe1 C5 69.3(5) . . ? C3 Fe1 C2 41.6(4) . . ? C5 Fe1 C2 69.3(4) . . ? C3 Fe1 C27 125.3(5) . . ? C5 Fe1 C27 153.8(4) . . ? C2 Fe1 C27 106.0(5) . . ? C3 Fe1 C1 69.0(4) . . ? C5 Fe1 C1 41.8(4) . . ? C2 Fe1 C1 40.3(4) . . ? C27 Fe1 C1 118.1(4) . . ? C3 Fe1 C26 164.0(5) . . ? C5 Fe1 C26 119.7(4) . . ? C2 Fe1 C26 126.1(4) . . ? C27 Fe1 C26 41.1(4) . . ? C1 Fe1 C26 108.0(4) . . ? C3 Fe1 C28 106.1(5) . . ? C5 Fe1 C28 164.4(4) . . ? C2 Fe1 C28 117.8(4) . . ? C27 Fe1 C28 40.9(4) . . ? C1 Fe1 C28 152.1(4) . . ? C26 Fe1 C28 68.7(4) . . ? C3 Fe1 C29 118.6(4) . . ? C5 Fe1 C29 127.3(4) . . ? C2 Fe1 C29 153.0(4) . . ? C27 Fe1 C29 68.4(4) . . ? C1 Fe1 C29 165.9(4) . . ? C26 Fe1 C29 68.0(4) . . ? C28 Fe1 C29 40.7(4) . . ? C3 Fe1 C4 40.5(4) . . ? C5 Fe1 C4 40.4(4) . . ? C2 Fe1 C4 68.4(4) . . ? C27 Fe1 C4 163.7(4) . . ? C1 Fe1 C4 68.3(4) . . ? C26 Fe1 C4 154.4(4) . . ? C28 Fe1 C4 126.8(4) . . ? C29 Fe1 C4 109.1(4) . . ? C3 Fe1 C30 152.9(4) . . ? C5 Fe1 C30 109.1(4) . . ? C2 Fe1 C30 165.0(4) . . ? C27 Fe1 C30 68.4(4) . . ? C1 Fe1 C30 128.8(4) . . ? C26 Fe1 C30 40.8(4) . . ? C28 Fe1 C30 67.8(4) . . ? C29 Fe1 C30 39.5(4) . . ? C4 Fe1 C30 120.7(4) . . ? C14 O1 Zn1 129.3(6) . . ? C14 O1 Dy1 125.4(5) . . ? Zn1 O1 Dy1 104.0(3) . . ? C13 O2 C15 115.2(8) . . ? C13 O2 Dy1 116.7(6) . . ? C15 O2 Dy1 127.2(6) . . ? C17 O4 C16 115.3(8) . . ? C17 O4 Dy1 117.5(5) . . ? C16 O4 Dy1 127.1(7) . . ? N5 O8 Dy1 96.2(5) . . ? N6 O11 Dy1 95.8(6) . . ? N6 O10 Dy1 96.0(6) . . ? C31 O5 Zn1 124.2(7) . . ? N5 O7 Dy1 96.4(6) . . ? C22 O3 Zn1 129.8(6) . . ? C22 O3 Dy1 123.6(6) . . ? Zn1 O3 Dy1 102.0(3) . . ? C14 C13 C12 121.9(9) . . ? C14 C13 O2 113.7(8) . . ? C12 C13 O2 124.3(9) . . ? C14 C9 C10 118.4(9) . . ? C14 C9 C8 125.7(9) . . ? C10 C9 C8 115.7(8) . . ? C11 C10 C9 121.4(9) . . ? O12 N6 O10 122.5(9) . . ? O12 N6 O11 122.2(10) . . ? O10 N6 O11 115.3(9) . . ? O12 N6 Dy1 174.0(8) . . ? O10 N6 Dy1 57.8(5) . . ? O11 N6 Dy1 58.0(5) . . ? C6 N1 N2 116.0(8) . . ? C27 C26 C30 107.4(8) . . ? C27 C26 C24 125.4(9) . . ? C30 C26 C24 127.1(10) . . ? C27 C26 Fe1 69.2(6) . . ? C30 C26 Fe1 70.5(5) . . ? C24 C26 Fe1 123.9(7) . . ? N1 C6 C7 129.2(9) . . ? N1 C6 C1 114.0(9) . . ? C7 C6 C1 116.8(9) . . ? O4 C17 C18 123.4(9) . . ? O4 C17 C22 114.2(8) . . ? C18 C17 C22 122.3(9) . . ? C24 N3 N4 114.9(8) . . ? C17 C18 C19 120.1(9) . . ? C23 N4 N3 111.5(8) . . ? C23 N4 Zn1 126.5(6) . . ? N3 N4 Zn1 121.8(6) . . ? C31 O6 Dy1 143.2(7) . . ? O1 C14 C13 118.6(8) . . ? O1 C14 C9 121.9(8) . . ? C13 C14 C9 119.5(9) . . ? O9 N5 O7 122.8(10) . . ? O9 N5 O8 122.7(8) . . ? O7 N5 O8 114.5(9) . . ? O9 N5 Dy1 178.0(7) . . ? O7 N5 Dy1 57.4(5) . . ? O8 N5 Dy1 57.1(5) . . ? C22 C21 C20 119.7(8) . . ? C22 C21 C23 122.9(9) . . ? C20 C21 C23 117.4(8) . . ? C20 C19 C18 118.8(9) . . ? O3 C22 C17 119.4(8) . . ? O3 C22 C21 122.7(8) . . ? C17 C22 C21 117.9(9) . . ? C29 C30 C26 108.3(10) . . ? C29 C30 Fe1 69.7(6) . . ? C26 C30 Fe1 68.7(6) . . ? N3 C24 C26 116.8(9) . . ? N3 C24 C25 125.9(9) . . ? C26 C24 C25 117.2(8) . . ? C4 C5 C1 107.6(9) . . ? C4 C5 Fe1 71.5(6) . . ? C1 C5 Fe1 70.3(6) . . ? C4 C3 C2 107.9(9) . . ? C4 C3 Fe1 71.8(6) . . ? C2 C3 Fe1 70.1(6) . . ? C28 C27 C26 107.8(10) . . ? C28 C27 Fe1 70.0(6) . . ? C26 C27 Fe1 69.8(6) . . ? N4 C23 C21 128.8(9) . . ? C5 C4 C3 108.5(9) . . ? C5 C4 Fe1 68.1(6) . . ? C3 C4 Fe1 67.6(6) . . ? C30 C29 C28 108.9(9) . . ? C30 C29 Fe1 70.7(6) . . ? C28 C29 Fe1 69.4(6) . . ? C10 C11 C12 119.3(10) . . ? C19 C20 C21 121.2(8) . . ? C2 C1 C5 107.6(9) . . ? C2 C1 C6 126.5(10) . . ? C5 C1 C6 125.8(9) . . ? C2 C1 Fe1 69.3(7) . . ? C5 C1 Fe1 67.9(6) . . ? C6 C1 Fe1 125.8(7) . . ? N2 C8 C9 128.8(8) . . ? C11 C12 C13 119.3(10) . . ? O6 C31 O5 125.0(11) . . ? O6 C31 C32 117.3(9) . . ? O5 C31 C32 117.7(10) . . ? C8 N2 N1 109.7(7) . . ? C8 N2 Zn1 122.8(6) . . ? N1 N2 Zn1 125.7(6) . . ? C29 C28 C27 107.6(9) . . ? C29 C28 Fe1 70.0(6) . . ? C27 C28 Fe1 69.1(6) . . ? C1 C2 C3 108.0(10) . . ? C1 C2 Fe1 70.5(6) . . ? C3 C2 Fe1 68.2(6) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.499 _refine_diff_density_min -1.352 _refine_diff_density_rms 0.273 _database_code_depnum_ccdc_archive 'CCDC 941858' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Zn-Tb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H31 Fe N6 O12 Tb Zn' _chemical_formula_sum 'C32 H31 Fe N6 O12 Tb Zn' _chemical_formula_weight 971.80 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.306(2) _cell_length_b 11.882(3) _cell_length_c 13.432(3) _cell_angle_alpha 72.214(4) _cell_angle_beta 86.364(4) _cell_angle_gamma 88.696(4) _cell_volume 1714.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2318 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 25.47 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.882 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964.0 _exptl_absorpt_coefficient_mu 3.224 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.578618 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9337 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_unetI/netI 0.0703 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6286 _reflns_number_gt 4950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6286 _refine_ls_number_parameters 483 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1402 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Tb1 Tb 0.70720(3) 0.41380(3) 0.77198(3) 0.02557(14) Uani 1 1 d . . . Zn1 Zn 0.94697(7) 0.24250(7) 0.73477(6) 0.0238(2) Uani 1 1 d . . . Fe1 Fe 1.33130(9) -0.09277(9) 0.67820(8) 0.0263(3) Uani 1 1 d . . . C25 C 0.9699(6) -0.0223(6) 0.6511(6) 0.0289(17) Uani 1 1 d . . . H25A H 0.9115 0.0385 0.6478 0.043 Uiso 1 1 calc R . . H25B H 0.9756 -0.0701 0.7225 0.043 Uiso 1 1 calc R . . H25C H 0.9471 -0.0708 0.6100 0.043 Uiso 1 1 calc R . . N5 N 0.7300(6) 0.6653(6) 0.7335(5) 0.0362(16) Uani 1 1 d . . . O10 O 0.5049(4) 0.3832(5) 0.7312(4) 0.0359(13) Uani 1 1 d . . . O2 O 0.7536(4) 0.4401(4) 0.9437(4) 0.0245(11) Uani 1 1 d . . . O3 O 0.8280(4) 0.3608(4) 0.6501(3) 0.0257(11) Uani 1 1 d . . . O11 O 0.5275(5) 0.3801(5) 0.8884(4) 0.0354(13) Uani 1 1 d . . . O1 O 0.8928(4) 0.3457(4) 0.8309(4) 0.0239(11) Uani 1 1 d . . . O4 O 0.6669(4) 0.5208(4) 0.5809(4) 0.0299(12) Uani 1 1 d . . . O9 O 0.6326(4) 0.6101(4) 0.7678(4) 0.0339(13) Uani 1 1 d . . . O8 O 0.7407(5) 0.7723(5) 0.7185(5) 0.0527(17) Uani 1 1 d . . . O7 O 0.8165(4) 0.6010(4) 0.7161(4) 0.0326(13) Uani 1 1 d . . . O5 O 0.8428(4) 0.1061(4) 0.8090(4) 0.0288(12) Uani 1 1 d . . . N1 N 1.1978(5) 0.1453(5) 0.7895(4) 0.0233(13) Uani 1 1 d . . . N2 N 1.0987(5) 0.1995(5) 0.8235(4) 0.0207(13) Uani 1 1 d . . . C3 C 1.4929(6) -0.0553(7) 0.7243(6) 0.0331(19) Uani 1 1 d . . . H3 H 1.5675 -0.0421 0.6812 0.040 Uiso 1 1 calc R . . O6 O 0.6830(4) 0.2112(4) 0.8316(4) 0.0339(13) Uani 1 1 d . . . C30 C 1.2907(7) -0.0098(7) 0.5279(5) 0.0292(17) Uani 1 1 d . . . H30 H 1.3122 0.0712 0.4866 0.035 Uiso 1 1 calc R . . C21 C 0.9160(6) 0.3886(6) 0.4774(6) 0.0236(16) Uani 1 1 d . . . C9 C 1.0359(6) 0.2892(6) 0.9620(5) 0.0225(15) Uani 1 1 d . . . C17 C 0.7470(6) 0.5034(6) 0.5076(6) 0.0256(16) Uani 1 1 d . . . C22 C 0.8328(6) 0.4156(6) 0.5446(5) 0.0191(14) Uani 1 1 d . . . C12 C 0.8915(6) 0.3938(6) 1.0852(5) 0.0241(16) Uani 1 1 d . . . H12 H 0.8419 0.4263 1.1273 0.029 Uiso 1 1 calc R . . N6 N 0.4591(6) 0.3635(6) 0.8236(6) 0.0435(19) Uani 1 1 d . . . O12 O 0.3577(5) 0.3306(6) 0.8481(5) 0.0557(18) Uani 1 1 d . . . C28 C 1.2971(7) -0.2114(7) 0.5982(6) 0.0363(19) Uani 1 1 d . . . H28 H 1.3249 -0.2935 0.6162 0.044 Uiso 1 1 calc R . . C11 C 0.9996(6) 0.3449(6) 1.1195(5) 0.0276(17) Uani 1 1 d . . . H11 H 1.0245 0.3487 1.1831 0.033 Uiso 1 1 calc R . . N3 N 1.1140(5) 0.1434(5) 0.5834(4) 0.0256(14) Uani 1 1 d . . . C31 C 0.7367(6) 0.1158(6) 0.8420(6) 0.0265(16) Uani 1 1 d . . . C13 C 0.8578(6) 0.3941(6) 0.9876(6) 0.0268(16) Uani 1 1 d . . . C14 C 0.9283(6) 0.3419(6) 0.9232(5) 0.0199(15) Uani 1 1 d . . . C15 C 0.6746(7) 0.4961(7) 1.0035(6) 0.0341(19) Uani 1 1 d . . . H15A H 0.6503 0.4392 1.0691 0.051 Uiso 1 1 calc R . . H15B H 0.6061 0.5259 0.9648 0.051 Uiso 1 1 calc R . . H15C H 0.7149 0.5601 1.0163 0.051 Uiso 1 1 calc R . . N4 N 1.0194(5) 0.2215(5) 0.5928(4) 0.0244(13) Uani 1 1 d . . . C19 C 0.8283(7) 0.5352(6) 0.3312(6) 0.0297(17) Uani 1 1 d . . . H19 H 0.8257 0.5726 0.2596 0.036 Uiso 1 1 calc R . . C20 C 0.9146(6) 0.4525(6) 0.3695(5) 0.0247(16) Uani 1 1 d . . . H20 H 0.9736 0.4382 0.3234 0.030 Uiso 1 1 calc R . . C5 C 1.3401(6) -0.1469(6) 0.8358(6) 0.0270(16) Uani 1 1 d . . . H5 H 1.2913 -0.2083 0.8858 0.032 Uiso 1 1 calc R . . C7 C 1.1104(6) -0.0442(6) 0.8992(6) 0.0286(17) Uani 1 1 d . . . H7A H 1.1356 -0.0681 0.9695 0.043 Uiso 1 1 calc R . . H7B H 1.0986 -0.1129 0.8776 0.043 Uiso 1 1 calc R . . H7C H 1.0373 -0.0008 0.8964 0.043 Uiso 1 1 calc R . . C23 C 1.0044(6) 0.2968(6) 0.5050(5) 0.0216(15) Uani 1 1 d . . . H23 H 1.0578 0.2924 0.4506 0.026 Uiso 1 1 calc R . . C1 C 1.3127(6) -0.0234(7) 0.7994(5) 0.0240(16) Uani 1 1 d . . . C8 C 1.1147(6) 0.2257(6) 0.9081(6) 0.0277(17) Uani 1 1 d . . . H8A H 1.1862 0.2007 0.9385 0.033 Uiso 1 1 calc R . . C24 C 1.0876(6) 0.0333(7) 0.6087(5) 0.0269(17) Uani 1 1 d . . . C10 C 1.0696(6) 0.2916(6) 1.0614(6) 0.0263(16) Uani 1 1 d . . . H10 H 1.1403 0.2562 1.0868 0.032 Uiso 1 1 calc R . . C6 C 1.2037(6) 0.0331(6) 0.8270(5) 0.0191(14) Uani 1 1 d . . . C2 C 1.4079(6) 0.0328(7) 0.7294(6) 0.0302(17) Uani 1 1 d . . . H2 H 1.4140 0.1174 0.6915 0.036 Uiso 1 1 calc R . . C32 C 0.6701(7) 0.0044(7) 0.9030(7) 0.042(2) Uani 1 1 d . . . H32A H 0.6545 0.0040 0.9742 0.063 Uiso 1 1 calc R . . H32B H 0.7172 -0.0635 0.9017 0.063 Uiso 1 1 calc R . . H32C H 0.5966 0.0020 0.8718 0.063 Uiso 1 1 calc R . . C16 C 0.5807(7) 0.6148(8) 0.5456(7) 0.046(2) Uani 1 1 d . . . H16A H 0.6212 0.6879 0.5120 0.069 Uiso 1 1 calc R . . H16B H 0.5322 0.6220 0.6047 0.069 Uiso 1 1 calc R . . H16C H 0.5317 0.5965 0.4968 0.069 Uiso 1 1 calc R . . C18 C 0.7452(6) 0.5617(6) 0.4016(5) 0.0277(17) Uani 1 1 d . . . H18 H 0.6878 0.6192 0.3771 0.033 Uiso 1 1 calc R . . C4 C 1.4511(7) -0.1639(7) 0.7891(6) 0.0331(18) Uani 1 1 d . . . H4 H 1.4919 -0.2400 0.7996 0.040 Uiso 1 1 calc R . . C26 C 1.1833(6) -0.0457(7) 0.5923(5) 0.0275(17) Uani 1 1 d . . . C29 C 1.3591(7) -0.1136(7) 0.5334(5) 0.0311(18) Uani 1 1 d . . . H29 H 1.4366 -0.1158 0.4970 0.037 Uiso 1 1 calc R . . C27 C 1.1903(7) -0.1718(7) 0.6388(7) 0.0367(19) Uani 1 1 d . . . H27 H 1.1309 -0.2218 0.6877 0.044 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 Tb1 0.0187(2) 0.0333(2) 0.0261(2) -0.01238(16) 0.00141(14) 0.00942(15) Zn1 0.0211(4) 0.0313(5) 0.0201(4) -0.0104(4) 0.0000(3) 0.0108(3) Fe1 0.0244(6) 0.0291(6) 0.0255(6) -0.0100(5) 0.0029(4) 0.0094(4) C25 0.030(4) 0.029(4) 0.028(4) -0.011(3) -0.003(3) 0.004(3) N5 0.031(4) 0.033(4) 0.048(4) -0.018(3) -0.001(3) 0.009(3) O10 0.030(3) 0.059(4) 0.023(3) -0.018(3) -0.003(2) 0.004(3) O2 0.023(3) 0.031(3) 0.023(3) -0.016(2) 0.004(2) 0.009(2) O3 0.024(3) 0.038(3) 0.016(2) -0.010(2) -0.004(2) 0.012(2) O11 0.026(3) 0.049(3) 0.041(3) -0.029(3) 0.001(2) 0.004(3) O1 0.022(3) 0.033(3) 0.021(3) -0.016(2) 0.000(2) 0.009(2) O4 0.029(3) 0.042(3) 0.020(3) -0.010(2) -0.007(2) 0.022(2) O9 0.016(3) 0.034(3) 0.053(4) -0.018(3) 0.009(2) 0.004(2) O8 0.042(4) 0.034(3) 0.077(5) -0.013(3) 0.007(3) 0.010(3) O7 0.022(3) 0.032(3) 0.044(3) -0.013(3) 0.000(2) 0.011(2) O5 0.023(3) 0.036(3) 0.026(3) -0.008(2) -0.002(2) 0.011(2) N1 0.020(3) 0.031(3) 0.019(3) -0.010(3) 0.001(2) 0.010(3) N2 0.023(3) 0.029(3) 0.010(3) -0.006(2) 0.000(2) 0.005(2) C3 0.022(4) 0.032(4) 0.043(5) -0.010(4) 0.008(3) 0.007(3) O6 0.030(3) 0.033(3) 0.035(3) -0.006(2) 0.005(2) 0.005(2) C30 0.038(4) 0.035(4) 0.016(4) -0.011(3) 0.002(3) 0.005(3) C21 0.011(3) 0.024(4) 0.041(4) -0.019(3) 0.004(3) 0.002(3) C9 0.021(4) 0.026(4) 0.021(4) -0.009(3) 0.001(3) 0.002(3) C17 0.017(4) 0.032(4) 0.034(4) -0.019(3) -0.003(3) 0.004(3) C22 0.016(3) 0.027(4) 0.018(3) -0.010(3) -0.009(3) 0.003(3) C12 0.025(4) 0.032(4) 0.021(4) -0.018(3) 0.007(3) 0.005(3) N6 0.028(4) 0.034(4) 0.075(6) -0.028(4) 0.009(4) 0.004(3) O12 0.025(3) 0.068(4) 0.086(5) -0.043(4) 0.012(3) -0.018(3) C28 0.030(4) 0.037(5) 0.048(5) -0.023(4) 0.000(4) 0.015(4) C11 0.032(4) 0.038(4) 0.013(3) -0.007(3) -0.003(3) -0.002(3) N3 0.026(3) 0.032(4) 0.019(3) -0.008(3) 0.000(2) 0.011(3) C31 0.025(4) 0.031(4) 0.025(4) -0.011(3) -0.002(3) 0.003(3) C13 0.023(4) 0.025(4) 0.031(4) -0.006(3) -0.001(3) 0.003(3) C14 0.027(4) 0.015(3) 0.020(4) -0.008(3) 0.002(3) 0.002(3) C15 0.028(4) 0.035(4) 0.045(5) -0.023(4) 0.013(4) 0.007(3) N4 0.019(3) 0.032(3) 0.024(3) -0.012(3) 0.006(2) 0.003(3) C19 0.037(4) 0.021(4) 0.026(4) 0.001(3) -0.001(3) -0.001(3) C20 0.029(4) 0.029(4) 0.021(4) -0.014(3) 0.003(3) -0.004(3) C5 0.019(4) 0.028(4) 0.032(4) -0.008(3) 0.001(3) 0.006(3) C7 0.021(4) 0.027(4) 0.033(4) -0.005(3) 0.008(3) 0.005(3) C23 0.022(4) 0.033(4) 0.012(3) -0.011(3) 0.003(3) 0.001(3) C1 0.019(4) 0.043(4) 0.009(3) -0.008(3) -0.005(3) 0.007(3) C8 0.017(4) 0.023(4) 0.041(5) -0.008(3) 0.005(3) 0.004(3) C24 0.031(4) 0.038(4) 0.017(4) -0.016(3) -0.007(3) 0.013(3) C10 0.015(3) 0.031(4) 0.035(4) -0.014(3) -0.003(3) 0.001(3) C6 0.022(3) 0.032(4) 0.005(3) -0.007(3) -0.007(3) 0.008(3) C2 0.023(4) 0.031(4) 0.039(5) -0.016(4) 0.001(3) 0.007(3) C32 0.032(5) 0.045(5) 0.050(5) -0.014(4) -0.005(4) 0.000(4) C16 0.041(5) 0.059(6) 0.045(5) -0.026(4) -0.010(4) 0.034(4) C18 0.026(4) 0.033(4) 0.023(4) -0.009(3) 0.000(3) 0.008(3) C4 0.032(4) 0.039(5) 0.031(4) -0.014(4) -0.008(3) 0.019(4) C26 0.026(4) 0.038(4) 0.018(4) -0.009(3) -0.007(3) 0.010(3) C29 0.029(4) 0.047(5) 0.021(4) -0.017(4) -0.004(3) 0.016(4) C27 0.032(4) 0.029(4) 0.053(5) -0.020(4) 0.004(4) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O3 2.292(5) . ? Tb1 O6 2.310(5) . ? Tb1 O1 2.330(4) . ? Tb1 O10 2.446(5) . ? Tb1 O11 2.447(5) . ? Tb1 O9 2.448(5) . ? Tb1 O7 2.455(5) . ? Tb1 O2 2.509(5) . ? Tb1 O4 2.557(5) . ? Tb1 N6 2.878(7) . ? Tb1 N5 2.887(7) . ? Tb1 Zn1 3.4554(9) . ? Zn1 O5 1.989(5) . ? Zn1 O3 2.052(4) . ? Zn1 O1 2.093(4) . ? Zn1 N4 2.110(6) . ? Zn1 N2 2.115(5) . ? Fe1 C5 2.024(7) . ? Fe1 C30 2.034(7) . ? Fe1 C1 2.036(7) . ? Fe1 C29 2.039(7) . ? Fe1 C27 2.045(8) . ? Fe1 C4 2.050(7) . ? Fe1 C2 2.052(8) . ? Fe1 C26 2.062(7) . ? Fe1 C3 2.066(8) . ? Fe1 C28 2.072(8) . ? C25 C24 1.499(10) . ? N5 O8 1.232(8) . ? N5 O9 1.280(8) . ? N5 O7 1.281(7) . ? O10 N6 1.268(9) . ? O2 C13 1.378(8) . ? O2 C15 1.446(8) . ? O3 C22 1.364(8) . ? O11 N6 1.262(9) . ? O1 C14 1.313(8) . ? O4 C17 1.355(8) . ? O4 C16 1.452(8) . ? O5 C31 1.268(8) . ? N1 C6 1.275(8) . ? N1 N2 1.400(7) . ? N2 C8 1.291(9) . ? C3 C4 1.391(11) . ? C3 C2 1.419(10) . ? O6 C31 1.247(8) . ? C30 C29 1.426(10) . ? C30 C26 1.438(10) . ? C21 C22 1.363(9) . ? C21 C20 1.416(10) . ? C21 C23 1.441(9) . ? C9 C14 1.411(9) . ? C9 C10 1.419(10) . ? C9 C8 1.452(9) . ? C17 C18 1.381(10) . ? C17 C22 1.406(9) . ? C12 C11 1.386(10) . ? C12 C13 1.388(10) . ? N6 O12 1.212(8) . ? C28 C29 1.393(11) . ? C28 C27 1.422(10) . ? C11 C10 1.356(10) . ? N3 C24 1.284(9) . ? N3 N4 1.425(7) . ? C31 C32 1.515(10) . ? C13 C14 1.409(9) . ? N4 C23 1.262(8) . ? C19 C20 1.375(10) . ? C19 C18 1.390(10) . ? C5 C4 1.405(10) . ? C5 C1 1.431(10) . ? C7 C6 1.505(9) . ? C1 C2 1.418(10) . ? C1 C6 1.472(9) . ? C24 C26 1.467(9) . ? C26 C27 1.439(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Tb1 O6 80.13(17) . . ? O3 Tb1 O1 66.53(16) . . ? O6 Tb1 O1 77.02(17) . . ? O3 Tb1 O10 105.52(17) . . ? O6 Tb1 O10 75.68(19) . . ? O1 Tb1 O10 152.52(19) . . ? O3 Tb1 O11 149.30(19) . . ? O6 Tb1 O11 74.51(18) . . ? O1 Tb1 O11 122.47(17) . . ? O10 Tb1 O11 51.67(17) . . ? O3 Tb1 O9 128.84(17) . . ? O6 Tb1 O9 148.62(17) . . ? O1 Tb1 O9 122.30(17) . . ? O10 Tb1 O9 83.74(18) . . ? O11 Tb1 O9 74.15(17) . . ? O3 Tb1 O7 85.87(17) . . ? O6 Tb1 O7 156.62(17) . . ? O1 Tb1 O7 80.26(16) . . ? O10 Tb1 O7 126.50(17) . . ? O11 Tb1 O7 123.51(17) . . ? O9 Tb1 O7 52.31(16) . . ? O3 Tb1 O2 130.21(15) . . ? O6 Tb1 O2 97.07(17) . . ? O1 Tb1 O2 64.49(15) . . ? O10 Tb1 O2 122.06(16) . . ? O11 Tb1 O2 70.78(17) . . ? O9 Tb1 O2 74.01(17) . . ? O7 Tb1 O2 77.84(16) . . ? O3 Tb1 O4 64.64(15) . . ? O6 Tb1 O4 117.78(18) . . ? O1 Tb1 O4 124.45(15) . . ? O10 Tb1 O4 67.60(17) . . ? O11 Tb1 O4 113.02(17) . . ? O9 Tb1 O4 73.92(17) . . ? O7 Tb1 O4 71.52(17) . . ? O2 Tb1 O4 144.93(16) . . ? O3 Tb1 N6 127.9(2) . . ? O6 Tb1 N6 71.50(18) . . ? O1 Tb1 N6 140.80(19) . . ? O10 Tb1 N6 25.97(19) . . ? O11 Tb1 N6 25.83(19) . . ? O9 Tb1 N6 79.59(17) . . ? O7 Tb1 N6 131.47(17) . . ? O2 Tb1 N6 96.6(2) . . ? O4 Tb1 N6 91.3(2) . . ? O3 Tb1 N5 108.16(18) . . ? O6 Tb1 N5 170.46(19) . . ? O1 Tb1 N5 101.62(18) . . ? O10 Tb1 N5 105.82(19) . . ? O11 Tb1 N5 98.85(18) . . ? O9 Tb1 N5 26.14(16) . . ? O7 Tb1 N5 26.17(16) . . ? O2 Tb1 N5 74.05(18) . . ? O4 Tb1 N5 70.92(18) . . ? N6 Tb1 N5 105.57(18) . . ? O3 Tb1 Zn1 34.95(11) . . ? O6 Tb1 Zn1 62.90(12) . . ? O1 Tb1 Zn1 36.24(11) . . ? O10 Tb1 Zn1 124.03(13) . . ? O11 Tb1 Zn1 135.04(13) . . ? O9 Tb1 Zn1 147.43(11) . . ? O7 Tb1 Zn1 95.17(11) . . ? O2 Tb1 Zn1 99.81(10) . . ? O4 Tb1 Zn1 99.53(10) . . ? N6 Tb1 Zn1 132.92(13) . . ? N5 Tb1 Zn1 121.31(13) . . ? O5 Zn1 O3 101.67(19) . . ? O5 Zn1 O1 95.37(19) . . ? O3 Zn1 O1 75.41(18) . . ? O5 Zn1 N4 109.8(2) . . ? O3 Zn1 N4 88.4(2) . . ? O1 Zn1 N4 152.5(2) . . ? O5 Zn1 N2 100.7(2) . . ? O3 Zn1 N2 152.5(2) . . ? O1 Zn1 N2 86.7(2) . . ? N4 Zn1 N2 99.0(2) . . ? O5 Zn1 Tb1 84.98(13) . . ? O3 Zn1 Tb1 39.78(13) . . ? O1 Zn1 Tb1 41.15(12) . . ? N4 Zn1 Tb1 128.08(16) . . ? N2 Zn1 Tb1 127.74(15) . . ? C5 Fe1 C30 165.4(3) . . ? C5 Fe1 C1 41.3(3) . . ? C30 Fe1 C1 125.9(3) . . ? C5 Fe1 C29 153.1(3) . . ? C30 Fe1 C29 41.0(3) . . ? C1 Fe1 C29 163.8(3) . . ? C5 Fe1 C27 109.4(3) . . ? C30 Fe1 C27 69.0(3) . . ? C1 Fe1 C27 120.1(3) . . ? C29 Fe1 C27 68.2(3) . . ? C5 Fe1 C4 40.3(3) . . ? C30 Fe1 C4 151.6(3) . . ? C1 Fe1 C4 68.2(3) . . ? C29 Fe1 C4 119.0(3) . . ? C27 Fe1 C4 129.0(3) . . ? C5 Fe1 C2 68.5(3) . . ? C30 Fe1 C2 106.0(3) . . ? C1 Fe1 C2 40.6(3) . . ? C29 Fe1 C2 126.0(3) . . ? C27 Fe1 C2 153.5(3) . . ? C4 Fe1 C2 67.5(3) . . ? C5 Fe1 C26 128.3(3) . . ? C30 Fe1 C26 41.1(3) . . ? C1 Fe1 C26 107.6(3) . . ? C29 Fe1 C26 68.6(3) . . ? C27 Fe1 C26 41.0(3) . . ? C4 Fe1 C26 166.7(3) . . ? C2 Fe1 C26 118.2(3) . . ? C5 Fe1 C3 67.6(3) . . ? C30 Fe1 C3 117.7(3) . . ? C1 Fe1 C3 67.9(3) . . ? C29 Fe1 C3 107.6(3) . . ? C27 Fe1 C3 165.3(3) . . ? C4 Fe1 C3 39.5(3) . . ? C2 Fe1 C3 40.3(3) . . ? C26 Fe1 C3 152.2(3) . . ? C5 Fe1 C28 121.0(3) . . ? C30 Fe1 C28 67.9(3) . . ? C1 Fe1 C28 155.2(3) . . ? C29 Fe1 C28 39.6(3) . . ? C27 Fe1 C28 40.4(3) . . ? C4 Fe1 C28 110.1(3) . . ? C2 Fe1 C28 163.6(3) . . ? C26 Fe1 C28 68.0(3) . . ? C3 Fe1 C28 127.6(3) . . ? O8 N5 O9 122.9(6) . . ? O8 N5 O7 122.0(7) . . ? O9 N5 O7 115.1(6) . . ? O8 N5 Tb1 178.9(6) . . ? O9 N5 Tb1 57.4(3) . . ? O7 N5 Tb1 57.7(3) . . ? N6 O10 Tb1 96.4(4) . . ? C13 O2 C15 116.9(6) . . ? C13 O2 Tb1 118.9(4) . . ? C15 O2 Tb1 124.1(4) . . ? C22 O3 Zn1 127.9(4) . . ? C22 O3 Tb1 125.6(4) . . ? Zn1 O3 Tb1 105.27(19) . . ? N6 O11 Tb1 96.5(4) . . ? C14 O1 Zn1 129.3(4) . . ? C14 O1 Tb1 124.1(4) . . ? Zn1 O1 Tb1 102.61(19) . . ? C17 O4 C16 117.0(6) . . ? C17 O4 Tb1 116.4(4) . . ? C16 O4 Tb1 125.4(4) . . ? N5 O9 Tb1 96.5(4) . . ? N5 O7 Tb1 96.1(4) . . ? C31 O5 Zn1 124.1(5) . . ? C6 N1 N2 116.2(6) . . ? C8 N2 N1 112.9(6) . . ? C8 N2 Zn1 125.6(5) . . ? N1 N2 Zn1 121.4(4) . . ? C4 C3 C2 108.4(7) . . ? C4 C3 Fe1 69.6(4) . . ? C2 C3 Fe1 69.3(4) . . ? C31 O6 Tb1 142.8(5) . . ? C29 C30 C26 107.6(7) . . ? C29 C30 Fe1 69.7(4) . . ? C26 C30 Fe1 70.5(4) . . ? C22 C21 C20 118.2(6) . . ? C22 C21 C23 126.0(7) . . ? C20 C21 C23 115.8(6) . . ? C14 C9 C10 120.0(6) . . ? C14 C9 C8 123.7(6) . . ? C10 C9 C8 116.2(6) . . ? O4 C17 C18 124.3(6) . . ? O4 C17 C22 115.8(6) . . ? C18 C17 C22 119.8(6) . . ? C21 C22 O3 122.8(6) . . ? C21 C22 C17 120.8(6) . . ? O3 C22 C17 116.5(6) . . ? C11 C12 C13 119.4(6) . . ? O12 N6 O11 122.4(8) . . ? O12 N6 O10 122.8(8) . . ? O11 N6 O10 114.8(6) . . ? O12 N6 Tb1 173.5(6) . . ? O11 N6 Tb1 57.6(3) . . ? O10 N6 Tb1 57.6(4) . . ? C29 C28 C27 108.8(7) . . ? C29 C28 Fe1 68.9(4) . . ? C27 C28 Fe1 68.8(5) . . ? C10 C11 C12 120.7(7) . . ? C24 N3 N4 116.1(6) . . ? O6 C31 O5 125.0(7) . . ? O6 C31 C32 116.6(6) . . ? O5 C31 C32 118.4(7) . . ? O2 C13 C12 125.5(6) . . ? O2 C13 C14 112.4(6) . . ? C12 C13 C14 122.1(6) . . ? O1 C14 C13 119.6(6) . . ? O1 C14 C9 123.4(6) . . ? C13 C14 C9 117.0(6) . . ? C23 N4 N3 110.0(5) . . ? C23 N4 Zn1 122.5(5) . . ? N3 N4 Zn1 125.3(4) . . ? C20 C19 C18 118.6(7) . . ? C19 C20 C21 121.8(6) . . ? C4 C5 C1 107.7(6) . . ? C4 C5 Fe1 70.8(4) . . ? C1 C5 Fe1 69.8(4) . . ? N4 C23 C21 128.9(6) . . ? C2 C1 C5 107.3(6) . . ? C2 C1 C6 126.7(7) . . ? C5 C1 C6 126.0(6) . . ? C2 C1 Fe1 70.3(4) . . ? C5 C1 Fe1 68.9(4) . . ? C6 C1 Fe1 124.2(5) . . ? N2 C8 C9 128.6(7) . . ? N3 C24 C26 115.9(7) . . ? N3 C24 C25 127.2(6) . . ? C26 C24 C25 116.9(7) . . ? C11 C10 C9 120.7(6) . . ? N1 C6 C1 116.5(6) . . ? N1 C6 C7 125.3(6) . . ? C1 C6 C7 118.2(6) . . ? C1 C2 C3 107.7(7) . . ? C1 C2 Fe1 69.1(4) . . ? C3 C2 Fe1 70.4(4) . . ? C17 C18 C19 120.6(7) . . ? C3 C4 C5 108.8(6) . . ? C3 C4 Fe1 70.9(4) . . ? C5 C4 Fe1 68.8(4) . . ? C30 C26 C27 107.0(6) . . ? C30 C26 C24 125.7(7) . . ? C27 C26 C24 127.3(7) . . ? C30 C26 Fe1 68.4(4) . . ? C27 C26 Fe1 68.9(4) . . ? C24 C26 Fe1 126.4(5) . . ? C28 C29 C30 108.8(7) . . ? C28 C29 Fe1 71.5(4) . . ? C30 C29 Fe1 69.3(4) . . ? C28 C27 C26 107.7(7) . . ? C28 C27 Fe1 70.8(5) . . ? C26 C27 Fe1 70.1(4) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.656 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.233 _database_code_depnum_ccdc_archive 'CCDC 941859' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Zn-Gd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C67 H64 Cl9 Fe2 Gd2 N12 O24 Zn2' _chemical_formula_sum 'C67 H64 Cl9 Fe2 Gd2 N12 O24 Zn2' _chemical_formula_weight 2297.33 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' Cl Cl 0.1484 0.1585 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.028(5) _cell_length_b 18.689(5) _cell_length_c 14.781(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 99.668(5) _cell_angle_gamma 90.000(5) _cell_volume 8177(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9434 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 28.31 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4540 _exptl_absorpt_coefficient_mu 2.897 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6005 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16438 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6802 _reflns_number_gt 6093 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+238.5352P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6802 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1363 _refine_ls_wR_factor_gt 0.1310 _refine_ls_goodness_of_fit_ref 1.216 _refine_ls_restrained_S_all 1.216 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.127080(12) 0.23504(2) 0.62764(3) 0.01652(13) Uani 1 1 d . . . Zn1 Zn 0.23954(3) 0.26084(5) 0.72977(6) 0.0153(2) Uani 1 1 d . . . Fe1 Fe 0.42595(4) 0.33650(6) 0.92396(8) 0.0196(3) Uani 1 1 d . . . O4 O 0.10740(17) 0.1327(3) 0.7257(4) 0.0205(12) Uani 1 1 d . . . Cl2 Cl 0.41712(19) -0.0458(2) 0.4726(3) 0.1003(16) Uani 1 1 d . . . O7 O 0.13646(17) 0.1217(3) 0.5392(4) 0.0179(12) Uani 1 1 d . . . O9 O 0.06885(18) 0.1659(3) 0.5250(4) 0.0222(12) Uani 1 1 d . . . O2 O 0.13497(18) 0.2732(3) 0.4648(4) 0.0221(12) Uani 1 1 d . . . Cl1 Cl 0.3813(2) -0.0275(2) 0.2879(3) 0.120(2) Uani 1 1 d . . . O10 O 0.05464(19) 0.2604(3) 0.6755(4) 0.0267(13) Uani 1 1 d . . . Cl3 Cl 0.3340(2) 0.0308(2) 0.4226(8) 0.225(5) Uani 1 1 d . . . O1 O 0.19918(17) 0.2751(3) 0.6055(3) 0.0173(11) Uani 1 1 d . . . O3 O 0.18824(17) 0.1847(3) 0.7280(4) 0.0167(11) Uani 1 1 d . . . O8 O 0.0816(2) 0.0754(3) 0.4394(4) 0.0285(14) Uani 1 1 d . . . O11 O 0.07705(19) 0.3336(3) 0.5763(4) 0.0247(13) Uani 1 1 d . . . O6 O 0.14335(19) 0.3201(3) 0.7447(4) 0.0271(14) Uani 1 1 d . . . C28 C 0.1418(3) 0.1020(4) 0.7878(5) 0.0158(16) Uani 1 1 d . . . O5 O 0.21486(17) 0.3272(3) 0.8147(4) 0.0198(12) Uani 1 1 d . . . N1 N 0.3344(2) 0.3334(4) 0.7315(4) 0.0176(14) Uani 1 1 d . . . C10 C 0.3874(3) 0.2529(4) 0.9531(6) 0.0186(17) Uani 1 1 d . . . C16 C 0.2476(3) 0.3455(4) 0.5264(5) 0.0181(17) Uani 1 1 d . . . N4 N 0.2794(2) 0.1936(3) 0.8246(4) 0.0151(13) Uani 1 1 d . . . N3 N 0.3265(2) 0.2051(3) 0.8501(4) 0.0153(13) Uani 1 1 d . . . N6 N 0.0497(3) 0.3183(4) 0.6291(6) 0.037(2) Uani 1 1 d . . . C2 C 0.3863(3) 0.4007(4) 0.8310(6) 0.0202(17) Uani 1 1 d . . . C20 C 0.1732(3) 0.3117(4) 0.4541(6) 0.0194(17) Uani 1 1 d . . . C17 C 0.2527(3) 0.3831(4) 0.4468(6) 0.0224(18) Uani 1 1 d . . . H17 H 0.2796 0.4070 0.4441 0.027 Uiso 1 1 calc R . . C29 C 0.0630(3) 0.1030(5) 0.7230(6) 0.0238(18) Uani 1 1 d . . . H29A H 0.0638 0.0525 0.7114 0.036 Uiso 1 1 calc R . . H29B H 0.0422 0.1256 0.6750 0.036 Uiso 1 1 calc R . . H29C H 0.0533 0.1110 0.7809 0.036 Uiso 1 1 calc R . . C22 C 0.0975(3) 0.2800(5) 0.3901(6) 0.031(2) Uani 1 1 d . . . H22A H 0.0896 0.3295 0.3810 0.047 Uiso 1 1 calc R . . H22B H 0.0720 0.2539 0.4044 0.047 Uiso 1 1 calc R . . H22C H 0.1059 0.2610 0.3350 0.047 Uiso 1 1 calc R . . C24 C 0.2215(3) 0.1073(4) 0.8509(5) 0.0161(16) Uani 1 1 d . . . C25 C 0.2140(3) 0.0506(4) 0.9092(6) 0.0200(17) Uani 1 1 d . . . H25 H 0.2384 0.0325 0.9500 0.024 Uiso 1 1 calc R . . C13 C 0.3384(3) 0.2449(4) 0.9223(5) 0.0165(16) Uani 1 1 d . . . C26 C 0.1725(3) 0.0215(4) 0.9081(5) 0.0183(17) Uani 1 1 d . . . H26 H 0.1686 -0.0155 0.9482 0.022 Uiso 1 1 calc R . . C27 C 0.1359(3) 0.0474(4) 0.8464(6) 0.0228(18) Uani 1 1 d . . . H27 H 0.1074 0.0276 0.8450 0.027 Uiso 1 1 calc R . . C18 C 0.2185(3) 0.3852(4) 0.3732(6) 0.0242(19) Uani 1 1 d . . . H18 H 0.2221 0.4112 0.3213 0.029 Uiso 1 1 calc R . . C19 C 0.1780(3) 0.3483(5) 0.3754(6) 0.0242(19) Uani 1 1 d . . . H19 H 0.1550 0.3486 0.3249 0.029 Uiso 1 1 calc R . . C32 C 0.3847(4) 0.0132(6) 0.3913(9) 0.060(4) Uani 1 1 d . . . H32 H 0.4013 0.0583 0.3899 0.073 Uiso 1 1 calc R . . N5 N 0.0955(2) 0.1196(4) 0.4992(5) 0.0210(15) Uani 1 1 d . . . C21 C 0.2074(3) 0.3106(4) 0.5315(5) 0.0166(16) Uani 1 1 d . . . C5 C 0.4493(3) 0.4399(5) 0.9322(6) 0.029(2) Uani 1 1 d . . . H5 H 0.4684 0.4618 0.9852 0.035 Uiso 1 1 calc R . . C30 C 0.1736(3) 0.3425(4) 0.8064(5) 0.0208(18) Uani 1 1 d . . . N2 N 0.2892(2) 0.3233(3) 0.6819(4) 0.0149(13) Uani 1 1 d . . . C46 C 0.1845(3) 0.1329(4) 0.7873(5) 0.0175(16) Uani 1 1 d . . . C6 C 0.4088(3) 0.2869(4) 1.0364(6) 0.0230(18) Uani 1 1 d . . . H6 H 0.3931 0.3093 1.0822 0.028 Uiso 1 1 calc R . . O12 O 0.0138(4) 0.3663(5) 0.6391(8) 0.088(3) Uani 1 1 d . . . C12 C 0.3033(3) 0.4357(4) 0.8103(5) 0.0184(17) Uani 1 1 d . . . H12A H 0.3045 0.4801 0.7782 0.028 Uiso 1 1 calc R . . H12B H 0.3080 0.4446 0.8752 0.028 Uiso 1 1 calc R . . H12C H 0.2743 0.4138 0.7917 0.028 Uiso 1 1 calc R . . C3 C 0.4262(3) 0.3794(5) 0.7968(6) 0.027(2) Uani 1 1 d . . . H3 H 0.4270 0.3524 0.7403 0.032 Uiso 1 1 calc R . . C31 C 0.1589(3) 0.3903(5) 0.8788(6) 0.033(2) Uani 1 1 d . . . H31A H 0.1831 0.4225 0.9022 0.050 Uiso 1 1 calc R . . H31B H 0.1517 0.3615 0.9280 0.050 Uiso 1 1 calc R . . H31C H 0.1328 0.4174 0.8520 0.050 Uiso 1 1 calc R . . C1 C 0.4014(3) 0.4396(4) 0.9146(6) 0.0233(18) Uani 1 1 d . . . H1 H 0.3818 0.4607 0.9541 0.028 Uiso 1 1 calc R . . C15 C 0.2864(3) 0.3465(4) 0.5990(5) 0.0182(17) Uani 1 1 d . . . H15 H 0.3127 0.3663 0.5840 0.022 Uiso 1 1 calc R . . C4 C 0.4645(3) 0.4032(5) 0.8598(6) 0.029(2) Uani 1 1 d . . . H4 H 0.4961 0.3953 0.8539 0.035 Uiso 1 1 calc R . . C11 C 0.3395(3) 0.3869(4) 0.7883(6) 0.0200(17) Uani 1 1 d . . . C23 C 0.2663(3) 0.1377(4) 0.8626(5) 0.0145(16) Uani 1 1 d . . . H23 H 0.2884 0.1136 0.9028 0.017 Uiso 1 1 calc R . . C9 C 0.4224(3) 0.2284(5) 0.9071(6) 0.0248(18) Uani 1 1 d . . . H9 H 0.4182 0.2031 0.8482 0.030 Uiso 1 1 calc R . . C14 C 0.3069(3) 0.2819(4) 0.9743(5) 0.0164(16) Uani 1 1 d . . . H14A H 0.2786 0.2899 0.9347 0.025 Uiso 1 1 calc R . . H14B H 0.3196 0.3270 0.9965 0.025 Uiso 1 1 calc R . . H14C H 0.3021 0.2528 1.0253 0.025 Uiso 1 1 calc R . . C8 C 0.4645(3) 0.2473(4) 0.9605(6) 0.0247(19) Uani 1 1 d . . . H8 H 0.4944 0.2375 0.9451 0.030 Uiso 1 1 calc R . . C7 C 0.4556(3) 0.2838(5) 1.0403(6) 0.0258(19) Uani 1 1 d . . . H7 H 0.4783 0.3037 1.0891 0.031 Uiso 1 1 calc R . . Cl4 Cl 0.0000 0.3165(2) 0.2500 0.0363(8) Uani 1 2 d S . . Cl5 Cl 0.02410(14) 0.4480(2) 0.3440(3) 0.0975(16) Uani 1 1 d . . . C33 C 0.0169(7) 0.4018(11) 0.2255(13) 0.037(5) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0114(2) 0.0176(2) 0.0194(2) -0.00176(16) -0.00077(14) 0.00050(15) Zn1 0.0127(4) 0.0171(4) 0.0152(4) 0.0011(4) 0.0003(3) -0.0008(3) Fe1 0.0123(6) 0.0232(6) 0.0224(6) -0.0002(5) 0.0007(5) -0.0025(5) O4 0.009(3) 0.023(3) 0.029(3) 0.000(2) 0.001(2) 0.000(2) Cl2 0.165(5) 0.088(3) 0.048(2) 0.0017(19) 0.020(2) -0.043(3) O7 0.008(3) 0.025(3) 0.019(3) -0.001(2) -0.001(2) 0.005(2) O9 0.019(3) 0.022(3) 0.025(3) -0.006(2) 0.001(2) 0.006(2) O2 0.019(3) 0.029(3) 0.017(3) 0.002(2) -0.002(2) 0.004(2) Cl1 0.248(7) 0.051(2) 0.050(2) -0.0128(17) -0.007(3) 0.016(3) O10 0.021(3) 0.025(3) 0.034(3) -0.004(3) 0.003(3) -0.004(3) Cl3 0.172(6) 0.0305(19) 0.540(15) 0.010(4) 0.249(8) 0.010(3) O1 0.015(3) 0.020(3) 0.017(3) 0.003(2) 0.000(2) 0.001(2) O3 0.013(3) 0.018(3) 0.018(3) 0.004(2) -0.001(2) -0.003(2) O8 0.025(3) 0.028(3) 0.032(3) -0.011(3) 0.002(3) 0.004(3) O11 0.023(3) 0.021(3) 0.030(3) -0.001(3) 0.003(3) 0.002(2) O6 0.020(3) 0.033(3) 0.027(3) -0.014(3) -0.001(3) 0.004(3) C28 0.019(4) 0.014(4) 0.014(4) -0.006(3) 0.004(3) 0.002(3) O5 0.013(3) 0.026(3) 0.019(3) -0.002(2) 0.000(2) 0.000(2) N1 0.013(3) 0.026(4) 0.013(3) 0.000(3) -0.001(3) 0.000(3) C10 0.022(4) 0.010(4) 0.024(4) 0.002(3) 0.004(3) 0.004(3) C16 0.017(4) 0.019(4) 0.017(4) -0.004(3) 0.002(3) 0.004(3) N4 0.010(3) 0.018(3) 0.017(3) -0.005(3) 0.000(3) -0.002(3) N3 0.011(3) 0.021(3) 0.014(3) 0.001(3) 0.003(3) 0.000(3) N6 0.028(4) 0.031(5) 0.049(5) -0.018(4) -0.005(4) 0.000(4) C2 0.022(4) 0.013(4) 0.024(4) 0.005(3) -0.002(3) -0.002(3) C20 0.017(4) 0.019(4) 0.023(4) 0.002(3) 0.004(3) 0.001(3) C17 0.021(4) 0.021(4) 0.026(5) 0.002(3) 0.005(4) 0.001(3) C29 0.012(4) 0.033(5) 0.025(5) 0.000(4) 0.000(3) -0.004(3) C22 0.027(5) 0.038(5) 0.023(5) 0.005(4) -0.012(4) 0.000(4) C24 0.014(4) 0.017(4) 0.017(4) -0.003(3) 0.001(3) -0.004(3) C25 0.017(4) 0.018(4) 0.024(4) -0.001(3) 0.000(3) 0.003(3) C13 0.017(4) 0.014(4) 0.017(4) 0.002(3) -0.001(3) 0.000(3) C26 0.015(4) 0.021(4) 0.020(4) 0.003(3) 0.008(3) -0.001(3) C27 0.020(4) 0.021(4) 0.028(5) -0.006(4) 0.005(4) -0.006(3) C18 0.031(5) 0.023(4) 0.017(4) 0.004(3) 0.001(4) 0.000(4) C19 0.023(4) 0.028(5) 0.019(4) -0.003(4) -0.003(3) 0.001(4) C32 0.073(9) 0.031(6) 0.088(10) -0.019(6) 0.044(8) -0.027(6) N5 0.022(4) 0.020(4) 0.021(4) 0.001(3) 0.004(3) 0.002(3) C21 0.016(4) 0.020(4) 0.013(4) 0.003(3) 0.001(3) 0.004(3) C5 0.023(5) 0.038(5) 0.025(5) 0.001(4) -0.002(4) -0.012(4) C30 0.028(5) 0.021(4) 0.014(4) -0.006(3) 0.004(3) 0.000(3) N2 0.016(3) 0.013(3) 0.015(3) -0.002(3) 0.002(3) -0.004(3) C46 0.017(4) 0.018(4) 0.019(4) -0.005(3) 0.007(3) 0.002(3) C6 0.025(4) 0.025(4) 0.017(4) 0.001(3) 0.000(3) 0.002(3) O12 0.077(7) 0.052(6) 0.131(9) -0.022(6) 0.007(6) 0.020(5) C12 0.013(4) 0.023(4) 0.020(4) -0.001(3) 0.006(3) -0.005(3) C3 0.015(4) 0.035(5) 0.030(5) 0.007(4) 0.001(4) -0.005(4) C31 0.031(5) 0.044(6) 0.023(5) -0.004(4) 0.000(4) 0.011(4) C1 0.027(5) 0.017(4) 0.026(4) -0.003(3) 0.003(4) -0.005(3) C15 0.017(4) 0.014(4) 0.025(4) -0.003(3) 0.008(3) -0.003(3) C4 0.015(4) 0.032(5) 0.040(5) 0.007(4) 0.006(4) -0.009(4) C11 0.014(4) 0.024(4) 0.023(4) 0.009(4) 0.006(3) -0.002(3) C23 0.016(4) 0.016(4) 0.010(4) -0.004(3) 0.002(3) -0.002(3) C9 0.026(5) 0.024(4) 0.024(4) -0.005(4) 0.001(4) 0.005(4) C14 0.018(4) 0.017(4) 0.011(4) -0.002(3) -0.004(3) -0.001(3) C8 0.009(4) 0.029(5) 0.036(5) -0.001(4) 0.003(3) -0.001(3) C7 0.020(4) 0.031(5) 0.022(4) 0.002(4) -0.008(3) 0.001(4) Cl4 0.0276(17) 0.049(2) 0.0290(17) 0.000 -0.0036(13) 0.000 Cl5 0.073(3) 0.075(3) 0.134(4) -0.063(3) -0.014(2) 0.016(2) C33 0.038(11) 0.042(11) 0.030(11) -0.006(9) 0.003(8) -0.012(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 Gd1 O6 2.340(6) . ? Gd1 O3 2.355(5) . ? Gd1 O1 2.365(5) . ? Gd1 O11 2.417(6) . ? Gd1 O10 2.444(6) . ? Gd1 O9 2.477(5) . ? Gd1 O4 2.529(6) . ? Gd1 O7 2.529(5) . ? Gd1 O2 2.559(6) . ? Gd1 N6 2.800(8) . ? Gd1 N5 2.925(7) . ? Gd1 Zn1 3.4933(10) . ? Zn1 O5 1.995(6) . ? Zn1 O1 2.041(5) . ? Zn1 O3 2.094(5) . ? Zn1 N4 2.101(6) . ? Zn1 N2 2.107(6) . ? Fe1 C10 2.034(8) . ? Fe1 C9 2.035(9) . ? Fe1 C4 2.040(8) . ? Fe1 C6 2.043(8) . ? Fe1 C3 2.045(9) . ? Fe1 C2 2.048(8) . ? Fe1 C8 2.050(8) . ? Fe1 C7 2.051(8) . ? Fe1 C5 2.053(9) . ? Fe1 C1 2.059(8) . ? O4 C28 1.387(9) . ? O4 C29 1.439(9) . ? Cl2 C32 1.794(15) . ? O7 N5 1.273(8) . ? O9 N5 1.280(9) . ? O2 C20 1.387(10) . ? O2 C22 1.445(9) . ? Cl1 C32 1.695(13) . ? O10 N6 1.276(10) . ? Cl3 C32 1.696(13) . ? O1 C21 1.336(9) . ? O3 C46 1.322(9) . ? O8 N5 1.230(9) . ? O11 N6 1.258(10) . ? O6 C30 1.247(10) . ? C28 C27 1.370(11) . ? C28 C46 1.407(11) . ? O5 C30 1.256(10) . ? N1 C11 1.297(11) . ? N1 N2 1.443(9) . ? C10 C9 1.421(12) . ? C10 C6 1.438(11) . ? C10 C13 1.472(11) . ? C16 C21 1.386(11) . ? C16 C17 1.401(11) . ? C16 C15 1.446(11) . ? N4 C23 1.278(10) . ? N4 N3 1.418(8) . ? N3 C13 1.301(10) . ? N6 O12 1.427(12) . ? C2 C3 1.433(12) . ? C2 C1 1.439(11) . ? C2 C11 1.464(11) . ? C20 C19 1.378(12) . ? C20 C21 1.402(11) . ? C17 C18 1.365(12) . ? C24 C25 1.408(11) . ? C24 C46 1.413(11) . ? C24 C23 1.444(10) . ? C25 C26 1.358(11) . ? C13 C14 1.487(11) . ? C26 C27 1.393(11) . ? C18 C19 1.401(12) . ? C5 C4 1.411(13) . ? C5 C1 1.418(12) . ? C30 C31 1.516(11) . ? N2 C15 1.289(10) . ? C6 C7 1.399(12) . ? C12 C11 1.496(11) . ? C3 C4 1.423(12) . ? C9 C8 1.418(12) . ? C8 C7 1.426(12) . ? Cl4 C33 1.73(2) 2 ? Cl4 C33 1.73(2) . ? Cl5 C33 1.70(2) 2 ? Cl5 C33 1.932(19) . ? C33 C33 1.34(4) 2 ? C33 Cl5 1.70(2) 2 ? 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 O6 Gd1 O3 76.22(19) . . ? O6 Gd1 O1 78.8(2) . . ? O3 Gd1 O1 65.06(17) . . ? O6 Gd1 O11 75.9(2) . . ? O3 Gd1 O11 151.65(19) . . ? O1 Gd1 O11 104.52(19) . . ? O6 Gd1 O10 74.9(2) . . ? O3 Gd1 O10 122.21(19) . . ? O1 Gd1 O10 149.19(19) . . ? O11 Gd1 O10 53.6(2) . . ? O6 Gd1 O9 147.71(19) . . ? O3 Gd1 O9 124.98(18) . . ? O1 Gd1 O9 130.43(18) . . ? O11 Gd1 O9 82.39(18) . . ? O10 Gd1 O9 72.98(19) . . ? O6 Gd1 O4 97.5(2) . . ? O3 Gd1 O4 64.48(17) . . ? O1 Gd1 O4 128.76(17) . . ? O11 Gd1 O4 124.29(19) . . ? O10 Gd1 O4 71.08(19) . . ? O9 Gd1 O4 75.41(18) . . ? O6 Gd1 O7 157.46(18) . . ? O3 Gd1 O7 81.29(17) . . ? O1 Gd1 O7 90.53(18) . . ? O11 Gd1 O7 126.38(18) . . ? O10 Gd1 O7 119.58(18) . . ? O9 Gd1 O7 51.33(17) . . ? O4 Gd1 O7 73.76(18) . . ? O6 Gd1 O2 117.7(2) . . ? O3 Gd1 O2 121.23(18) . . ? O1 Gd1 O2 63.26(17) . . ? O11 Gd1 O2 69.10(19) . . ? O10 Gd1 O2 116.46(19) . . ? O9 Gd1 O2 74.72(19) . . ? O4 Gd1 O2 144.81(18) . . ? O7 Gd1 O2 73.21(18) . . ? O6 Gd1 N6 71.8(2) . . ? O3 Gd1 N6 141.0(2) . . ? O1 Gd1 N6 127.3(2) . . ? O11 Gd1 N6 26.6(2) . . ? O10 Gd1 N6 27.1(2) . . ? O9 Gd1 N6 78.05(19) . . ? O4 Gd1 N6 98.1(2) . . ? O7 Gd1 N6 129.32(19) . . ? O2 Gd1 N6 93.5(2) . . ? O6 Gd1 N5 170.3(2) . . ? O3 Gd1 N5 104.36(18) . . ? O1 Gd1 N5 110.37(19) . . ? O11 Gd1 N5 103.99(19) . . ? O10 Gd1 N5 97.08(19) . . ? O9 Gd1 N5 25.73(18) . . ? O4 Gd1 N5 74.50(18) . . ? O7 Gd1 N5 25.70(17) . . ? O2 Gd1 N5 70.50(19) . . ? N6 Gd1 N5 103.6(2) . . ? O6 Gd1 Zn1 61.33(14) . . ? O3 Gd1 Zn1 35.68(12) . . ? O1 Gd1 Zn1 34.42(12) . . ? O11 Gd1 Zn1 122.36(14) . . ? O10 Gd1 Zn1 133.72(14) . . ? O9 Gd1 Zn1 150.26(12) . . ? O4 Gd1 Zn1 99.13(12) . . ? O7 Gd1 Zn1 98.95(11) . . ? O2 Gd1 Zn1 97.61(12) . . ? N6 Gd1 Zn1 131.57(15) . . ? N5 Gd1 Zn1 124.54(13) . . ? O5 Zn1 O1 105.0(2) . . ? O5 Zn1 O3 94.6(2) . . ? O1 Zn1 O3 75.7(2) . . ? O5 Zn1 N4 100.5(2) . . ? O1 Zn1 N4 149.8(2) . . ? O3 Zn1 N4 86.4(2) . . ? O5 Zn1 N2 103.0(2) . . ? O1 Zn1 N2 88.4(2) . . ? O3 Zn1 N2 158.9(2) . . ? N4 Zn1 N2 101.5(2) . . ? O5 Zn1 Gd1 85.61(15) . . ? O1 Zn1 Gd1 40.91(15) . . ? O3 Zn1 Gd1 40.99(14) . . ? N4 Zn1 Gd1 127.35(17) . . ? N2 Zn1 Gd1 128.19(17) . . ? C10 Fe1 C9 40.9(3) . . ? C10 Fe1 C4 162.9(4) . . ? C9 Fe1 C4 124.8(4) . . ? C10 Fe1 C6 41.3(3) . . ? C9 Fe1 C6 68.6(3) . . ? C4 Fe1 C6 153.6(4) . . ? C10 Fe1 C3 125.9(3) . . ? C9 Fe1 C3 106.5(4) . . ? C4 Fe1 C3 40.8(3) . . ? C6 Fe1 C3 165.0(3) . . ? C10 Fe1 C2 107.8(3) . . ? C9 Fe1 C2 119.1(3) . . ? C4 Fe1 C2 69.0(3) . . ? C6 Fe1 C2 127.9(3) . . ? C3 Fe1 C2 41.0(3) . . ? C10 Fe1 C8 68.6(3) . . ? C9 Fe1 C8 40.6(3) . . ? C4 Fe1 C8 106.3(4) . . ? C6 Fe1 C8 68.0(3) . . ? C3 Fe1 C8 118.2(4) . . ? C2 Fe1 C8 153.2(3) . . ? C10 Fe1 C7 68.6(3) . . ? C9 Fe1 C7 68.4(3) . . ? C4 Fe1 C7 118.9(4) . . ? C6 Fe1 C7 40.0(3) . . ? C3 Fe1 C7 153.0(4) . . ? C2 Fe1 C7 164.9(4) . . ? C8 Fe1 C7 40.7(3) . . ? C10 Fe1 C5 155.8(3) . . ? C9 Fe1 C5 162.1(4) . . ? C4 Fe1 C5 40.3(4) . . ? C6 Fe1 C5 120.6(4) . . ? C3 Fe1 C5 68.4(4) . . ? C2 Fe1 C5 69.0(3) . . ? C8 Fe1 C5 125.3(3) . . ? C7 Fe1 C5 107.9(3) . . ? C10 Fe1 C1 121.5(3) . . ? C9 Fe1 C1 155.4(3) . . ? C4 Fe1 C1 67.8(4) . . ? C6 Fe1 C1 110.0(3) . . ? C3 Fe1 C1 68.2(4) . . ? C2 Fe1 C1 41.0(3) . . ? C8 Fe1 C1 163.5(3) . . ? C7 Fe1 C1 127.3(3) . . ? C5 Fe1 C1 40.3(3) . . ? C28 O4 C29 116.3(6) . . ? C28 O4 Gd1 118.2(4) . . ? C29 O4 Gd1 125.5(5) . . ? N5 O7 Gd1 94.8(4) . . ? N5 O9 Gd1 97.1(4) . . ? C20 O2 C22 114.9(6) . . ? C20 O2 Gd1 117.5(4) . . ? C22 O2 Gd1 124.1(5) . . ? N6 O10 Gd1 92.2(5) . . ? C21 O1 Zn1 129.6(5) . . ? C21 O1 Gd1 124.7(4) . . ? Zn1 O1 Gd1 104.7(2) . . ? C46 O3 Zn1 129.3(5) . . ? C46 O3 Gd1 124.5(5) . . ? Zn1 O3 Gd1 103.3(2) . . ? N6 O11 Gd1 93.9(5) . . ? C30 O6 Gd1 143.5(5) . . ? C27 C28 O4 124.4(7) . . ? C27 C28 C46 121.7(7) . . ? O4 C28 C46 113.9(7) . . ? C30 O5 Zn1 122.9(5) . . ? C11 N1 N2 115.4(6) . . ? C9 C10 C6 107.0(7) . . ? C9 C10 C13 126.9(7) . . ? C6 C10 C13 126.1(7) . . ? C9 C10 Fe1 69.6(5) . . ? C6 C10 Fe1 69.7(5) . . ? C13 C10 Fe1 126.0(5) . . ? C21 C16 C17 120.0(7) . . ? C21 C16 C15 124.6(7) . . ? C17 C16 C15 115.4(7) . . ? C23 N4 N3 112.1(6) . . ? C23 N4 Zn1 126.7(5) . . ? N3 N4 Zn1 121.1(5) . . ? C13 N3 N4 115.4(6) . . ? O11 N6 O10 119.8(7) . . ? O11 N6 O12 120.3(9) . . ? O10 N6 O12 120.0(9) . . ? O11 N6 Gd1 59.5(4) . . ? O10 N6 Gd1 60.7(4) . . ? O12 N6 Gd1 172.3(6) . . ? C3 C2 C1 106.4(7) . . ? C3 C2 C11 126.8(8) . . ? C1 C2 C11 126.8(8) . . ? C3 C2 Fe1 69.4(5) . . ? C1 C2 Fe1 69.9(5) . . ? C11 C2 Fe1 126.4(6) . . ? C19 C20 O2 124.1(7) . . ? C19 C20 C21 122.0(7) . . ? O2 C20 C21 113.9(7) . . ? C18 C17 C16 120.6(8) . . ? C25 C24 C46 118.4(7) . . ? C25 C24 C23 117.6(7) . . ? C46 C24 C23 123.9(7) . . ? C26 C25 C24 122.3(7) . . ? N3 C13 C10 115.7(7) . . ? N3 C13 C14 125.4(7) . . ? C10 C13 C14 118.8(7) . . ? C25 C26 C27 119.4(7) . . ? C28 C27 C26 120.0(7) . . ? C17 C18 C19 120.4(8) . . ? C20 C19 C18 118.5(8) . . ? Cl1 C32 Cl3 114.3(9) . . ? Cl1 C32 Cl2 105.8(7) . . ? Cl3 C32 Cl2 110.3(8) . . ? O8 N5 O7 122.7(7) . . ? O8 N5 O9 121.0(7) . . ? O7 N5 O9 116.4(6) . . ? O8 N5 Gd1 174.6(5) . . ? O7 N5 Gd1 59.5(4) . . ? O9 N5 Gd1 57.2(4) . . ? O1 C21 C16 124.0(7) . . ? O1 C21 C20 117.7(7) . . ? C16 C21 C20 118.2(7) . . ? C4 C5 C1 107.8(8) . . ? C4 C5 Fe1 69.3(5) . . ? C1 C5 Fe1 70.1(5) . . ? O6 C30 O5 125.6(7) . . ? O6 C30 C31 116.8(8) . . ? O5 C30 C31 117.6(7) . . ? C15 N2 N1 110.1(6) . . ? C15 N2 Zn1 124.7(5) . . ? N1 N2 Zn1 124.0(5) . . ? O3 C46 C28 118.9(7) . . ? O3 C46 C24 123.0(7) . . ? C28 C46 C24 118.1(7) . . ? C7 C6 C10 108.5(8) . . ? C7 C6 Fe1 70.3(5) . . ? C10 C6 Fe1 69.0(5) . . ? C4 C3 C2 108.2(8) . . ? C4 C3 Fe1 69.4(5) . . ? C2 C3 Fe1 69.6(5) . . ? C5 C1 C2 108.8(8) . . ? C5 C1 Fe1 69.6(5) . . ? C2 C1 Fe1 69.1(4) . . ? N2 C15 C16 128.0(7) . . ? C5 C4 C3 108.7(8) . . ? C5 C4 Fe1 70.3(5) . . ? C3 C4 Fe1 69.8(5) . . ? N1 C11 C2 114.6(7) . . ? N1 C11 C12 126.8(7) . . ? C2 C11 C12 118.6(7) . . ? N4 C23 C24 128.2(7) . . ? C8 C9 C10 108.4(7) . . ? C8 C9 Fe1 70.3(5) . . ? C10 C9 Fe1 69.5(5) . . ? C9 C8 C7 107.8(7) . . ? C9 C8 Fe1 69.1(5) . . ? C7 C8 Fe1 69.7(5) . . ? C6 C7 C8 108.3(7) . . ? C6 C7 Fe1 69.7(5) . . ? C8 C7 Fe1 69.6(5) . . ? C33 Cl4 C33 45.6(14) 2 . ? C33 Cl5 C33 42.7(12) 2 . ? C33 C33 Cl5 77.9(15) 2 2 ? C33 C33 Cl4 67.2(7) 2 . ? Cl5 C33 Cl4 112.8(11) 2 . ? C33 C33 Cl5 59.4(13) 2 . ? Cl5 C33 Cl5 106.3(11) 2 . ? Cl4 C33 Cl5 102.4(10) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 2.706 _refine_diff_density_min -2.236 _refine_diff_density_rms 0.169 _database_code_depnum_ccdc_archive 'CCDC 941860' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Zn-Er _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H31 Er Fe N6 O12 Zn' _chemical_formula_sum 'C32 H31 Er Fe N6 O12 Zn' _chemical_formula_weight 980.13 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.259(5) _cell_length_b 11.864(5) _cell_length_c 13.429(5) _cell_angle_alpha 72.504(5) _cell_angle_beta 86.526(5) _cell_angle_gamma 88.687(5) _cell_volume 1707.7(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2574 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.83 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 970.0 _exptl_absorpt_coefficient_mu 3.624 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.665424 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9308 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_unetI/netI 0.0653 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6249 _reflns_number_gt 5065 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0832P)^2^+0.5786P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6249 _refine_ls_number_parameters 483 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1455 _refine_ls_wR_factor_gt 0.1180 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.70762(3) 0.41351(3) 0.77296(3) 0.02317(14) Uani 1 1 d . . . Zn1 Zn 0.94548(8) 0.24290(8) 0.73479(6) 0.0218(2) Uani 1 1 d . . . Fe1 Fe 1.33064(10) -0.09349(10) 0.67750(8) 0.0239(3) Uani 1 1 d . . . O9 O 0.6340(5) 0.6070(5) 0.7685(4) 0.0270(12) Uani 1 1 d . . . O2 O 0.7516(5) 0.4424(5) 0.9424(4) 0.0237(12) Uani 1 1 d . . . O4 O 0.6628(5) 0.5211(5) 0.5849(4) 0.0296(13) Uani 1 1 d . . . O3 O 0.8237(5) 0.3595(5) 0.6498(4) 0.0256(12) Uani 1 1 d . . . O11 O 0.5293(5) 0.3795(5) 0.8887(5) 0.0336(14) Uani 1 1 d . . . O10 O 0.5086(5) 0.3793(5) 0.7311(4) 0.0331(13) Uani 1 1 d . . . O7 O 0.8190(5) 0.5954(5) 0.7174(4) 0.0294(13) Uani 1 1 d . . . C21 C 0.9134(7) 0.3904(6) 0.4762(5) 0.0189(15) Uani 1 1 d . . . O1 O 0.8921(5) 0.3462(4) 0.8305(4) 0.0235(12) Uani 1 1 d . . . C20 C 0.9111(7) 0.4559(7) 0.3690(6) 0.0258(17) Uani 1 1 d . . . H20 H 0.9687 0.4411 0.3218 0.031 Uiso 1 1 calc R . . O8 O 0.7440(6) 0.7699(6) 0.7177(6) 0.0500(18) Uani 1 1 d . . . N3 N 1.1118(6) 0.1423(5) 0.5833(5) 0.0235(14) Uani 1 1 d . . . C15 C 0.6736(7) 0.4964(7) 1.0048(6) 0.0253(17) Uani 1 1 d U . . H15A H 0.6562 0.4404 1.0721 0.038 Uiso 1 1 calc R . . H15B H 0.6009 0.5206 0.9703 0.038 Uiso 1 1 calc R . . H15C H 0.7119 0.5642 1.0133 0.038 Uiso 1 1 calc R . . O5 O 0.8410(5) 0.1076(5) 0.8095(4) 0.0282(13) Uani 1 1 d . . . C13 C 0.8571(7) 0.3960(6) 0.9868(6) 0.0229(17) Uani 1 1 d . . . N1 N 1.1972(5) 0.1452(6) 0.7883(5) 0.0216(14) Uani 1 1 d . . . C22 C 0.8287(7) 0.4159(6) 0.5471(6) 0.0210(16) Uani 1 1 d . . . O6 O 0.6840(5) 0.2154(5) 0.8339(5) 0.0334(14) Uani 1 1 d . . . N6 N 0.4629(6) 0.3605(6) 0.8236(6) 0.0304(16) Uani 1 1 d . . . C5 C 1.3380(8) -0.1500(7) 0.8369(6) 0.0272(18) Uani 1 1 d . . . H5 H 1.2874 -0.2102 0.8860 0.033 Uiso 1 1 calc R . . C11 C 0.9976(7) 0.3460(7) 1.1202(6) 0.0260(17) Uani 1 1 d . . . H11 H 1.0215 0.3483 1.1846 0.031 Uiso 1 1 calc R . . C12 C 0.8915(7) 0.3969(7) 1.0840(6) 0.0244(17) Uani 1 1 d . . . H12 H 0.8426 0.4320 1.1248 0.029 Uiso 1 1 calc R . . C8 C 1.1146(7) 0.2264(6) 0.9076(5) 0.0188(15) Uani 1 1 d . . . H8A H 1.1868 0.2013 0.9372 0.023 Uiso 1 1 calc R . . C1 C 1.3125(7) -0.0225(6) 0.7994(5) 0.0185(15) Uani 1 1 d . . . C26 C 1.1815(7) -0.0486(7) 0.5927(6) 0.0262(18) Uani 1 1 d . . . C17 C 0.7428(7) 0.5040(7) 0.5086(6) 0.0237(17) Uani 1 1 d . . . C25 C 0.9690(7) -0.0212(6) 0.6526(6) 0.0255(17) Uani 1 1 d . . . H25A H 0.9665 -0.0444 0.7277 0.038 Uiso 1 1 calc R . . H25B H 0.9578 -0.0893 0.6299 0.038 Uiso 1 1 calc R . . H25C H 0.9070 0.0354 0.6279 0.038 Uiso 1 1 calc R . . O12 O 0.3603(6) 0.3298(6) 0.8467(5) 0.0448(16) Uani 1 1 d . . . C28 C 1.2973(8) -0.2104(7) 0.5991(6) 0.033(2) Uani 1 1 d . . . H28 H 1.3242 -0.2929 0.6179 0.039 Uiso 1 1 calc R . . C9 C 1.0357(7) 0.2883(6) 0.9623(6) 0.0213(16) Uani 1 1 d . . . C7 C 1.1091(7) -0.0482(7) 0.9010(6) 0.031(2) Uani 1 1 d . . . H7A H 1.1337 -0.0715 0.9715 0.046 Uiso 1 1 calc R . . H7B H 1.0999 -0.1171 0.8788 0.046 Uiso 1 1 calc R . . H7C H 1.0346 -0.0066 0.8977 0.046 Uiso 1 1 calc R . . C23 C 1.0031(7) 0.3006(6) 0.5038(6) 0.0212(16) Uani 1 1 d . . . H23 H 1.0588 0.2984 0.4504 0.025 Uiso 1 1 calc R . . C19 C 0.8262(7) 0.5400(7) 0.3332(6) 0.0266(18) Uani 1 1 d . . . H19 H 0.8249 0.5807 0.2623 0.032 Uiso 1 1 calc R . . C3 C 1.4918(7) -0.0570(7) 0.7233(7) 0.0285(18) Uani 1 1 d . . . H3 H 1.5665 -0.0433 0.6801 0.034 Uiso 1 1 calc R . . C2 C 1.4074(7) 0.0290(7) 0.7295(6) 0.0246(17) Uani 1 1 d . . . H2 H 1.4139 0.1132 0.6909 0.029 Uiso 1 1 calc R . . C14 C 0.9285(7) 0.3416(7) 0.9234(6) 0.0214(16) Uani 1 1 d . . . N2 N 1.0970(6) 0.2019(5) 0.8233(4) 0.0208(14) Uani 1 1 d . . . C24 C 1.0863(7) 0.0327(8) 0.6102(6) 0.032(2) Uani 1 1 d . . . C31 C 0.7349(8) 0.1164(8) 0.8446(6) 0.0299(19) Uani 1 1 d . . . C18 C 0.7409(7) 0.5646(7) 0.4045(6) 0.0274(18) Uani 1 1 d . . . H18 H 0.6830 0.6221 0.3810 0.033 Uiso 1 1 calc R . . N4 N 1.0169(6) 0.2229(6) 0.5922(5) 0.0247(15) Uani 1 1 d . . . C27 C 1.1902(8) -0.1699(8) 0.6357(6) 0.032(2) Uani 1 1 d . . . H27 H 1.1308 -0.2199 0.6844 0.039 Uiso 1 1 calc R . . C30 C 1.2911(8) -0.0078(8) 0.5276(6) 0.0308(19) Uani 1 1 d . . . H30 H 1.3119 0.0733 0.4864 0.037 Uiso 1 1 calc R . . C10 C 1.0694(7) 0.2910(7) 1.0602(6) 0.0253(17) Uani 1 1 d . . . H10 H 1.1406 0.2557 1.0855 0.030 Uiso 1 1 calc R . . C29 C 1.3567(8) -0.1160(7) 0.5304(6) 0.033(2) Uani 1 1 d . . . H29 H 1.4342 -0.1201 0.4942 0.040 Uiso 1 1 calc R . . C6 C 1.2041(6) 0.0333(6) 0.8284(5) 0.0176(15) Uani 1 1 d . . . C16 C 0.5755(8) 0.6106(8) 0.5503(7) 0.041(2) Uani 1 1 d . . . H16A H 0.6122 0.6869 0.5324 0.061 Uiso 1 1 calc R . . H16B H 0.5149 0.6043 0.6051 0.061 Uiso 1 1 calc R . . H16C H 0.5404 0.6011 0.4899 0.061 Uiso 1 1 calc R . . C4 C 1.4489(8) -0.1696(7) 0.7897(6) 0.031(2) Uani 1 1 d . . . H4 H 1.4890 -0.2461 0.7998 0.037 Uiso 1 1 calc R . . C32 C 0.6715(8) 0.0108(8) 0.9041(7) 0.036(2) Uani 1 1 d . . . H32A H 0.6837 -0.0044 0.9771 0.054 Uiso 1 1 calc R . . H32B H 0.7006 -0.0550 0.8819 0.054 Uiso 1 1 calc R . . H32C H 0.5881 0.0216 0.8928 0.054 Uiso 1 1 calc R . . N5 N 0.7316(6) 0.6614(6) 0.7341(5) 0.0295(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.0188(2) 0.0290(2) 0.0231(2) -0.01092(15) 0.00134(14) 0.00770(14) Zn1 0.0212(5) 0.0275(5) 0.0177(4) -0.0092(4) -0.0004(3) 0.0093(4) Fe1 0.0220(6) 0.0262(6) 0.0253(6) -0.0119(5) 0.0026(5) 0.0077(5) O9 0.019(3) 0.032(3) 0.032(3) -0.012(2) 0.001(2) 0.006(2) O2 0.019(3) 0.031(3) 0.026(3) -0.017(2) 0.000(2) 0.007(2) O4 0.029(3) 0.033(3) 0.030(3) -0.015(2) -0.002(2) 0.014(3) O3 0.026(3) 0.034(3) 0.019(3) -0.011(2) -0.003(2) 0.010(2) O11 0.024(3) 0.047(4) 0.039(3) -0.028(3) 0.004(3) -0.001(3) O10 0.028(3) 0.040(3) 0.033(3) -0.013(3) -0.003(3) 0.006(3) O7 0.018(3) 0.038(3) 0.029(3) -0.008(3) 0.002(2) 0.014(2) C21 0.022(4) 0.020(4) 0.019(4) -0.012(3) 0.000(3) -0.001(3) O1 0.026(3) 0.030(3) 0.017(3) -0.012(2) 0.000(2) 0.012(2) C20 0.026(4) 0.028(4) 0.027(4) -0.015(3) 0.004(3) -0.005(3) O8 0.046(4) 0.033(4) 0.069(5) -0.013(3) 0.000(4) 0.011(3) N3 0.026(4) 0.020(3) 0.026(3) -0.011(3) -0.002(3) 0.008(3) C15 0.0256(19) 0.0255(19) 0.0254(19) -0.0088(11) -0.0001(10) 0.0012(10) O5 0.022(3) 0.040(3) 0.023(3) -0.010(2) -0.002(2) 0.015(2) C13 0.024(4) 0.022(4) 0.022(4) -0.006(3) 0.004(3) 0.000(3) N1 0.015(3) 0.033(4) 0.018(3) -0.010(3) 0.001(2) 0.010(3) C22 0.019(4) 0.024(4) 0.024(4) -0.011(3) -0.005(3) 0.002(3) O6 0.021(3) 0.032(3) 0.044(3) -0.009(3) 0.009(3) 0.003(2) N6 0.021(4) 0.030(4) 0.044(4) -0.018(3) 0.003(3) 0.001(3) C5 0.036(5) 0.024(4) 0.023(4) -0.009(3) -0.003(3) 0.010(4) C11 0.031(5) 0.035(4) 0.017(4) -0.013(3) -0.005(3) 0.001(4) C12 0.030(5) 0.027(4) 0.021(4) -0.015(3) 0.005(3) -0.007(3) C8 0.016(4) 0.017(4) 0.023(4) -0.005(3) 0.002(3) -0.001(3) C1 0.022(4) 0.022(4) 0.013(3) -0.008(3) 0.002(3) 0.002(3) C26 0.029(5) 0.035(5) 0.020(4) -0.016(3) -0.006(3) 0.013(4) C17 0.020(4) 0.029(4) 0.025(4) -0.011(3) -0.002(3) 0.004(3) C25 0.027(4) 0.015(4) 0.038(5) -0.013(3) -0.005(3) -0.005(3) O12 0.026(4) 0.061(4) 0.052(4) -0.023(3) 0.005(3) -0.007(3) C28 0.040(5) 0.029(4) 0.031(4) -0.013(4) -0.004(4) 0.015(4) C9 0.025(4) 0.015(4) 0.021(4) -0.003(3) 0.002(3) -0.002(3) C7 0.030(5) 0.040(5) 0.016(4) -0.001(3) 0.006(3) 0.019(4) C23 0.024(4) 0.017(4) 0.023(4) -0.008(3) 0.003(3) -0.001(3) C19 0.032(5) 0.025(4) 0.022(4) -0.004(3) -0.003(3) -0.003(3) C3 0.018(4) 0.026(4) 0.043(5) -0.014(4) 0.006(4) -0.006(3) C2 0.023(4) 0.028(4) 0.025(4) -0.013(3) -0.002(3) 0.002(3) C14 0.017(4) 0.027(4) 0.020(4) -0.008(3) -0.001(3) 0.002(3) N2 0.022(4) 0.025(3) 0.015(3) -0.006(3) 0.005(2) 0.002(3) C24 0.026(5) 0.058(6) 0.016(4) -0.018(4) -0.007(3) 0.024(4) C31 0.031(5) 0.040(5) 0.021(4) -0.013(4) -0.007(3) 0.014(4) C18 0.029(5) 0.020(4) 0.032(4) -0.007(3) -0.006(4) 0.002(3) N4 0.022(4) 0.036(4) 0.018(3) -0.013(3) -0.002(3) 0.010(3) C27 0.034(5) 0.046(5) 0.024(4) -0.021(4) -0.006(4) 0.017(4) C30 0.038(5) 0.040(5) 0.017(4) -0.013(3) 0.000(3) 0.013(4) C10 0.022(4) 0.031(4) 0.025(4) -0.013(3) 0.000(3) 0.003(3) C29 0.036(5) 0.038(5) 0.032(4) -0.022(4) 0.005(4) 0.012(4) C6 0.020(4) 0.016(4) 0.020(4) -0.009(3) -0.001(3) -0.006(3) C16 0.030(5) 0.053(6) 0.042(5) -0.017(4) -0.012(4) 0.029(4) C4 0.030(5) 0.038(5) 0.023(4) -0.008(3) -0.002(3) 0.021(4) C32 0.025(5) 0.038(5) 0.041(5) -0.006(4) -0.006(4) 0.002(4) N5 0.027(4) 0.029(4) 0.033(4) -0.011(3) 0.003(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. Carbon atom C15 was having large anisotropic diplacement parameteres and hence refined isotropically. ; 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 Er1 O6 2.260(6) . ? Er1 O3 2.279(5) . ? Er1 O1 2.302(5) . ? Er1 O9 2.407(5) . ? Er1 O7 2.414(6) . ? Er1 O10 2.415(6) . ? Er1 O11 2.428(6) . ? Er1 O2 2.480(5) . ? Er1 O4 2.539(5) . ? Er1 N6 2.836(7) . ? Er1 N5 2.844(7) . ? Er1 Zn1 3.4265(14) . ? Zn1 O5 1.985(6) . ? Zn1 O3 2.061(5) . ? Zn1 O1 2.082(5) . ? Zn1 N2 2.102(6) . ? Zn1 N4 2.109(6) . ? Fe1 C2 2.021(8) . ? Fe1 C28 2.030(9) . ? Fe1 C27 2.029(9) . ? Fe1 C30 2.035(8) . ? Fe1 C3 2.047(8) . ? Fe1 C5 2.049(8) . ? Fe1 C1 2.052(7) . ? Fe1 C26 2.056(8) . ? Fe1 C4 2.057(8) . ? Fe1 C29 2.075(8) . ? O9 N5 1.276(9) . ? O2 C13 1.389(9) . ? O2 C15 1.447(8) . ? O4 C17 1.382(9) . ? O4 C16 1.422(9) . ? O3 C22 1.338(9) . ? O11 N6 1.256(9) . ? O10 N6 1.273(9) . ? O7 N5 1.294(8) . ? C21 C22 1.398(10) . ? C21 C20 1.418(10) . ? C21 C23 1.433(10) . ? O1 C14 1.322(9) . ? C20 C19 1.365(11) . ? O8 N5 1.248(9) . ? N3 C24 1.275(11) . ? N3 N4 1.441(8) . ? O5 C31 1.271(10) . ? C13 C12 1.387(10) . ? C13 C14 1.419(10) . ? N1 C6 1.276(9) . ? N1 N2 1.427(8) . ? C22 C17 1.410(10) . ? O6 C31 1.268(9) . ? N6 O12 1.214(9) . ? C5 C4 1.412(11) . ? C5 C1 1.470(10) . ? C11 C12 1.375(11) . ? C11 C10 1.393(10) . ? C8 N2 1.278(9) . ? C8 C9 1.445(10) . ? C1 C2 1.400(10) . ? C1 C6 1.463(10) . ? C26 C27 1.384(12) . ? C26 C30 1.471(12) . ? C26 C24 1.480(10) . ? C17 C18 1.367(11) . ? C25 C24 1.485(12) . ? C28 C29 1.375(12) . ? C28 C27 1.403(11) . ? C9 C10 1.400(10) . ? C9 C14 1.404(10) . ? C7 C6 1.544(10) . ? C23 N4 1.281(9) . ? C19 C18 1.402(11) . ? C3 C2 1.395(11) . ? C3 C4 1.441(11) . ? C31 C32 1.445(12) . ? C30 C29 1.459(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 O6 Er1 O3 80.59(19) . . ? O6 Er1 O1 76.7(2) . . ? O3 Er1 O1 67.62(18) . . ? O6 Er1 O9 148.23(19) . . ? O3 Er1 O9 128.65(18) . . ? O1 Er1 O9 122.48(19) . . ? O6 Er1 O7 155.45(19) . . ? O3 Er1 O7 85.59(19) . . ? O1 Er1 O7 79.33(18) . . ? O9 Er1 O7 53.42(18) . . ? O6 Er1 O10 75.0(2) . . ? O3 Er1 O10 102.89(19) . . ? O1 Er1 O10 151.3(2) . . ? O9 Er1 O10 85.03(19) . . ? O7 Er1 O10 128.17(18) . . ? O6 Er1 O11 73.7(2) . . ? O3 Er1 O11 148.1(2) . . ? O1 Er1 O11 122.40(19) . . ? O9 Er1 O11 74.58(19) . . ? O7 Er1 O11 124.89(18) . . ? O10 Er1 O11 52.58(19) . . ? O6 Er1 O2 96.6(2) . . ? O3 Er1 O2 132.38(18) . . ? O1 Er1 O2 65.54(16) . . ? O9 Er1 O2 73.39(17) . . ? O7 Er1 O2 77.97(18) . . ? O10 Er1 O2 122.44(18) . . ? O11 Er1 O2 70.23(18) . . ? O6 Er1 O4 119.2(2) . . ? O3 Er1 O4 64.99(17) . . ? O1 Er1 O4 125.43(17) . . ? O9 Er1 O4 72.74(17) . . ? O7 Er1 O4 71.70(18) . . ? O10 Er1 O4 66.71(19) . . ? O11 Er1 O4 112.11(19) . . ? O2 Er1 O4 143.74(17) . . ? O6 Er1 N6 70.5(2) . . ? O3 Er1 N6 125.9(2) . . ? O1 Er1 N6 140.4(2) . . ? O9 Er1 N6 80.54(19) . . ? O7 Er1 N6 133.52(18) . . ? O10 Er1 N6 26.5(2) . . ? O11 Er1 N6 26.17(19) . . ? O2 Er1 N6 96.38(19) . . ? O4 Er1 N6 90.5(2) . . ? O6 Er1 N5 169.8(2) . . ? O3 Er1 N5 108.12(19) . . ? O1 Er1 N5 101.5(2) . . ? O9 Er1 N5 26.49(19) . . ? O7 Er1 N5 26.94(18) . . ? O10 Er1 N5 107.2(2) . . ? O11 Er1 N5 99.60(19) . . ? O2 Er1 N5 73.77(18) . . ? O4 Er1 N5 70.16(19) . . ? N6 Er1 N5 106.86(19) . . ? O6 Er1 Zn1 63.15(14) . . ? O3 Er1 Zn1 35.67(13) . . ? O1 Er1 Zn1 36.35(12) . . ? O9 Er1 Zn1 147.49(13) . . ? O7 Er1 Zn1 94.09(12) . . ? O10 Er1 Zn1 122.35(14) . . ? O11 Er1 Zn1 134.77(14) . . ? O2 Er1 Zn1 100.98(11) . . ? O4 Er1 Zn1 100.55(12) . . ? N6 Er1 Zn1 131.88(14) . . ? N5 Er1 Zn1 121.02(14) . . ? O5 Zn1 O3 100.9(2) . . ? O5 Zn1 O1 95.0(2) . . ? O3 Zn1 O1 75.9(2) . . ? O5 Zn1 N2 100.8(2) . . ? O3 Zn1 N2 152.8(2) . . ? O1 Zn1 N2 86.1(2) . . ? O5 Zn1 N4 110.6(2) . . ? O3 Zn1 N4 87.7(2) . . ? O1 Zn1 N4 152.0(2) . . ? N2 Zn1 N4 99.8(2) . . ? O5 Zn1 Er1 84.74(15) . . ? O3 Zn1 Er1 40.14(14) . . ? O1 Zn1 Er1 40.94(14) . . ? N2 Zn1 Er1 126.93(16) . . ? N4 Zn1 Er1 127.81(17) . . ? C2 Fe1 C28 163.6(3) . . ? C2 Fe1 C27 153.7(3) . . ? C28 Fe1 C27 40.5(3) . . ? C2 Fe1 C30 105.5(3) . . ? C28 Fe1 C30 69.1(3) . . ? C27 Fe1 C30 69.1(4) . . ? C2 Fe1 C3 40.1(3) . . ? C28 Fe1 C3 127.2(3) . . ? C27 Fe1 C3 165.6(3) . . ? C30 Fe1 C3 116.8(4) . . ? C2 Fe1 C5 68.9(3) . . ? C28 Fe1 C5 120.1(3) . . ? C27 Fe1 C5 109.4(3) . . ? C30 Fe1 C5 165.0(3) . . ? C3 Fe1 C5 68.4(3) . . ? C2 Fe1 C1 40.2(3) . . ? C28 Fe1 C1 155.4(3) . . ? C27 Fe1 C1 120.7(3) . . ? C30 Fe1 C1 124.9(3) . . ? C3 Fe1 C1 68.0(3) . . ? C5 Fe1 C1 42.0(3) . . ? C2 Fe1 C26 119.3(3) . . ? C28 Fe1 C26 67.8(3) . . ? C27 Fe1 C26 39.6(3) . . ? C30 Fe1 C26 42.1(3) . . ? C3 Fe1 C26 153.0(3) . . ? C5 Fe1 C26 127.4(3) . . ? C1 Fe1 C26 107.8(3) . . ? C2 Fe1 C4 68.5(3) . . ? C28 Fe1 C4 108.6(3) . . ? C27 Fe1 C4 128.1(4) . . ? C30 Fe1 C4 152.1(3) . . ? C3 Fe1 C4 41.1(3) . . ? C5 Fe1 C4 40.2(3) . . ? C1 Fe1 C4 69.0(3) . . ? C26 Fe1 C4 164.6(3) . . ? C2 Fe1 C29 126.9(3) . . ? C28 Fe1 C29 39.1(3) . . ? C27 Fe1 C29 66.9(3) . . ? C30 Fe1 C29 41.6(3) . . ? C3 Fe1 C29 108.1(4) . . ? C5 Fe1 C29 152.7(3) . . ? C1 Fe1 C29 163.9(3) . . ? C26 Fe1 C29 68.2(3) . . ? C4 Fe1 C29 119.1(3) . . ? N5 O9 Er1 96.2(4) . . ? C13 O2 C15 115.4(6) . . ? C13 O2 Er1 118.2(4) . . ? C15 O2 Er1 126.2(4) . . ? C17 O4 C16 116.0(6) . . ? C17 O4 Er1 116.4(4) . . ? C16 O4 Er1 126.9(5) . . ? C22 O3 Zn1 128.3(5) . . ? C22 O3 Er1 125.3(4) . . ? Zn1 O3 Er1 104.2(2) . . ? N6 O11 Er1 95.4(4) . . ? N6 O10 Er1 95.5(5) . . ? N5 O7 Er1 95.4(4) . . ? C22 C21 C20 118.8(7) . . ? C22 C21 C23 124.6(7) . . ? C20 C21 C23 116.6(6) . . ? C14 O1 Zn1 128.9(4) . . ? C14 O1 Er1 124.3(4) . . ? Zn1 O1 Er1 102.7(2) . . ? C19 C20 C21 121.6(7) . . ? C24 N3 N4 117.1(7) . . ? C31 O5 Zn1 125.1(5) . . ? C12 C13 O2 125.6(7) . . ? C12 C13 C14 121.5(7) . . ? O2 C13 C14 112.9(6) . . ? C6 N1 N2 116.3(6) . . ? O3 C22 C21 123.4(6) . . ? O3 C22 C17 118.1(6) . . ? C21 C22 C17 118.5(7) . . ? C31 O6 Er1 144.7(6) . . ? O12 N6 O11 122.1(7) . . ? O12 N6 O10 121.9(7) . . ? O11 N6 O10 115.9(7) . . ? O12 N6 Er1 175.5(5) . . ? O11 N6 Er1 58.4(4) . . ? O10 N6 Er1 57.9(4) . . ? C4 C5 C1 107.6(7) . . ? C4 C5 Fe1 70.2(4) . . ? C1 C5 Fe1 69.1(4) . . ? C12 C11 C10 120.0(7) . . ? C11 C12 C13 120.0(7) . . ? N2 C8 C9 127.7(7) . . ? C2 C1 C6 128.9(7) . . ? C2 C1 C5 106.6(6) . . ? C6 C1 C5 124.4(7) . . ? C2 C1 Fe1 68.7(4) . . ? C6 C1 Fe1 124.8(5) . . ? C5 C1 Fe1 68.9(4) . . ? C27 C26 C30 107.7(7) . . ? C27 C26 C24 129.0(8) . . ? C30 C26 C24 123.2(7) . . ? C27 C26 Fe1 69.2(5) . . ? C30 C26 Fe1 68.2(4) . . ? C24 C26 Fe1 125.2(5) . . ? C18 C17 O4 124.6(7) . . ? C18 C17 C22 121.6(7) . . ? O4 C17 C22 113.8(6) . . ? C29 C28 C27 108.9(7) . . ? C29 C28 Fe1 72.2(5) . . ? C27 C28 Fe1 69.7(5) . . ? C10 C9 C14 120.1(7) . . ? C10 C9 C8 116.5(7) . . ? C14 C9 C8 123.4(7) . . ? N4 C23 C21 128.7(7) . . ? C20 C19 C18 119.4(7) . . ? C2 C3 C4 108.1(7) . . ? C2 C3 Fe1 69.0(5) . . ? C4 C3 Fe1 69.8(5) . . ? C3 C2 C1 110.1(7) . . ? C3 C2 Fe1 70.9(5) . . ? C1 C2 Fe1 71.1(4) . . ? O1 C14 C9 123.8(6) . . ? O1 C14 C13 118.4(7) . . ? C9 C14 C13 117.7(7) . . ? C8 N2 N1 112.5(6) . . ? C8 N2 Zn1 127.1(5) . . ? N1 N2 Zn1 120.4(4) . . ? N3 C24 C26 116.8(8) . . ? N3 C24 C25 126.6(7) . . ? C26 C24 C25 116.6(8) . . ? O6 C31 O5 122.3(8) . . ? O6 C31 C32 118.2(8) . . ? O5 C31 C32 119.4(7) . . ? C17 C18 C19 120.0(7) . . ? C23 N4 N3 110.5(6) . . ? C23 N4 Zn1 122.7(5) . . ? N3 N4 Zn1 124.5(4) . . ? C26 C27 C28 109.7(8) . . ? C26 C27 Fe1 71.2(5) . . ? C28 C27 Fe1 69.8(5) . . ? C29 C30 C26 104.5(7) . . ? C29 C30 Fe1 70.7(5) . . ? C26 C30 Fe1 69.7(4) . . ? C11 C10 C9 120.7(7) . . ? C28 C29 C30 108.9(7) . . ? C28 C29 Fe1 68.7(5) . . ? C30 C29 Fe1 67.8(4) . . ? N1 C6 C1 115.8(6) . . ? N1 C6 C7 126.8(7) . . ? C1 C6 C7 117.4(6) . . ? C5 C4 C3 107.6(7) . . ? C5 C4 Fe1 69.6(4) . . ? C3 C4 Fe1 69.1(4) . . ? O8 N5 O9 123.5(7) . . ? O8 N5 O7 121.5(7) . . ? O9 N5 O7 114.9(6) . . ? O8 N5 Er1 179.0(6) . . ? O9 N5 Er1 57.3(3) . . ? O7 N5 Er1 57.7(4) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.680 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.213 _database_code_depnum_ccdc_archive 'CCDC 941861' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Zn-Ho _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H31 Fe Ho N6 O12 Zn' _chemical_formula_sum 'C32 H31 Fe Ho N6 O12 Zn' _chemical_formula_weight 977.80 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2702(9) _cell_length_b 11.8757(10) _cell_length_c 13.4290(11) _cell_angle_alpha 72.480(2) _cell_angle_beta 86.528(2) _cell_angle_gamma 88.765(2) _cell_volume 1710.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1237 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 21.01 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.898 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968.0 _exptl_absorpt_coefficient_mu 3.477 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.590233 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9390 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_unetI/netI 0.1007 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6264 _reflns_number_gt 4587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Carbon atoms C4, C14 and C31 were having large anisotropic diplacement parameteres and hence refined isotropically. Oxygen atom O3 was having large anisotropic diplacement parameteres and hence refined isotropically. ; _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^)+(0.0419P)^2^+23.7228P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6264 _refine_ls_number_parameters 483 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1655 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.082 _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 Ho1 Ho 0.79264(4) 0.08643(5) 0.72748(4) 0.02279(17) Uani 1 1 d . . . Zn1 Zn 0.55393(11) 0.25745(11) 0.76544(10) 0.0216(3) Uani 1 1 d . . . Fe1 Fe 0.16925(14) 0.59299(14) 0.82265(13) 0.0228(4) Uani 1 1 d . . . O9 O 0.8663(6) -0.1089(7) 0.7334(7) 0.0291(19) Uani 1 1 d . . . O11 O 0.9702(6) 0.1190(7) 0.6122(6) 0.0269(18) Uani 1 1 d . . . O10 O 0.9916(7) 0.1190(7) 0.7698(5) 0.0276(19) Uani 1 1 d . . . O1 O 0.6756(6) 0.1395(6) 0.8505(5) 0.0223(17) Uani 1 1 d . . . O4 O 0.7475(6) 0.0586(6) 0.5574(6) 0.0244(17) Uani 1 1 d . . . O2 O 0.8362(6) -0.0204(7) 0.9174(6) 0.0284(19) Uani 1 1 d . . . O7 O 0.6821(6) -0.0981(7) 0.7862(6) 0.0284(19) Uani 1 1 d . . . O3 O 0.6062(6) 0.1525(6) 0.6706(5) 0.0205(16) Uani 1 1 d U . . O8 O 0.7579(7) -0.2704(7) 0.7831(7) 0.041(2) Uani 1 1 d . . . O5 O 0.6579(6) 0.3950(7) 0.6885(6) 0.0252(18) Uani 1 1 d . . . O6 O 0.8163(7) 0.2868(7) 0.6653(6) 0.0304(19) Uani 1 1 d . . . N4 N 0.4036(7) 0.2981(7) 0.6796(6) 0.0172(19) Uani 1 1 d . . . N3 N 0.3025(7) 0.3544(8) 0.7125(6) 0.019(2) Uani 1 1 d . . . N1 N 0.3881(8) 0.3568(8) 0.9174(7) 0.022(2) Uani 1 1 d . . . C10 C 0.5869(9) 0.0468(9) 1.1304(7) 0.017(2) Uani 1 1 d . . . H10 H 0.5298 0.0624 1.1775 0.021 Uiso 1 1 calc R . . C16 C 0.8247(10) 0.0008(11) 0.4970(9) 0.030(3) Uani 1 1 d . . . H16A H 0.7793 -0.0543 0.4754 0.045 Uiso 1 1 calc R . . H16B H 0.8871 -0.0404 0.5392 0.045 Uiso 1 1 calc R . . H16C H 0.8587 0.0590 0.4364 0.045 Uiso 1 1 calc R . . C7 C 0.5304(9) 0.5242(10) 0.8458(9) 0.025(3) Uani 1 1 d . . . H7A H 0.5720 0.4788 0.8064 0.037 Uiso 1 1 calc R . . H7B H 0.5769 0.5275 0.9023 0.037 Uiso 1 1 calc R . . H7C H 0.5172 0.6028 0.8010 0.037 Uiso 1 1 calc R . . O12 O 1.1405(7) 0.1720(8) 0.6503(8) 0.047(3) Uani 1 1 d . . . C21 C 0.4639(9) 0.2114(8) 0.5380(8) 0.015(2) Uani 1 1 d . . . N2 N 0.4824(7) 0.2786(8) 0.9072(7) 0.021(2) Uani 1 1 d . . . C17 C 0.6435(9) 0.1050(9) 0.5117(9) 0.021(2) Uani 1 1 d . . . C14 C 0.6708(9) 0.0834(9) 0.9538(8) 0.017(2) Uani 1 1 d U . . C18 C 0.6077(11) 0.1034(9) 0.4162(9) 0.026(3) Uani 1 1 d . . . H18 H 0.6549 0.0674 0.3753 0.031 Uiso 1 1 calc R . . C19 C 0.5003(10) 0.1561(10) 0.3811(9) 0.026(3) Uani 1 1 d . . . H19 H 0.4756 0.1551 0.3166 0.031 Uiso 1 1 calc R . . C31 C 0.7628(9) 0.3832(9) 0.6559(8) 0.021(2) Uani 1 1 d U . . C15 C 0.9218(10) -0.1148(12) 0.9517(9) 0.034(3) Uani 1 1 d . . . H15A H 0.9643 -0.1029 1.0075 0.052 Uiso 1 1 calc R . . H15B H 0.9768 -0.1151 0.8944 0.052 Uiso 1 1 calc R . . H15C H 0.8811 -0.1891 0.9761 0.052 Uiso 1 1 calc R . . C9 C 0.5854(9) 0.1086(10) 1.0246(8) 0.020(2) Uani 1 1 d . . . C13 C 0.7555(9) -0.0046(9) 0.9921(8) 0.019(2) Uani 1 1 d . . . C29 C 0.0070(10) 0.5564(10) 0.7758(9) 0.025(3) Uani 1 1 d . . . H29 H -0.0673 0.5431 0.8195 0.030 Uiso 1 1 calc R . . C6 C 0.4136(9) 0.4673(10) 0.8887(8) 0.021(2) Uani 1 1 d . . . N5 N 0.7679(9) -0.1632(9) 0.7698(8) 0.031(2) Uani 1 1 d . . . C5 C 0.3111(10) 0.6709(10) 0.8636(8) 0.023(2) Uani 1 1 d . . . H5 H 0.3707 0.7206 0.8148 0.028 Uiso 1 1 calc R . . C22 C 0.5716(9) 0.1565(9) 0.5764(9) 0.021(2) Uani 1 1 d . . . C1 C 0.3164(10) 0.5486(11) 0.9042(8) 0.024(3) Uani 1 1 d . . . C24 C 0.2954(9) 0.4677(9) 0.6733(8) 0.018(2) Uani 1 1 d . . . C20 C 0.4319(10) 0.2087(9) 0.4402(8) 0.020(2) Uani 1 1 d . . . H20 H 0.3609 0.2443 0.4149 0.024 Uiso 1 1 calc R . . C23 C 0.3864(9) 0.2765(9) 0.5908(8) 0.019(2) Uani 1 1 d . . . H23 H 0.3168 0.3064 0.5586 0.023 Uiso 1 1 calc R . . C2 C 0.2104(11) 0.5091(11) 0.9742(10) 0.033(3) Uani 1 1 d . . . H2 H 0.1901 0.4283 1.0165 0.039 Uiso 1 1 calc R . . C27 C 0.1598(9) 0.6475(10) 0.6647(8) 0.022(2) Uani 1 1 d . . . H27 H 0.2100 0.7083 0.6157 0.027 Uiso 1 1 calc R . . C4 C 0.2029(9) 0.7115(9) 0.9010(8) 0.018(2) Uani 1 1 d U . . H4 H 0.1756 0.7937 0.8824 0.022 Uiso 1 1 calc R . . C28 C 0.0480(10) 0.6680(10) 0.7107(9) 0.027(3) Uani 1 1 d . . . H28 H 0.0074 0.7441 0.7000 0.033 Uiso 1 1 calc R . . C11 C 0.6734(10) -0.0375(9) 1.1655(9) 0.025(3) Uani 1 1 d . . . H11 H 0.6746 -0.0779 1.2365 0.030 Uiso 1 1 calc R . . C25 C 0.3893(9) 0.5442(10) 0.5981(9) 0.026(3) Uani 1 1 d . . . H25A H 0.4621 0.5003 0.6002 0.039 Uiso 1 1 calc R . . H25B H 0.4026 0.6136 0.6183 0.039 Uiso 1 1 calc R . . H25C H 0.3621 0.5668 0.5284 0.039 Uiso 1 1 calc R . . C26 C 0.1880(10) 0.5244(10) 0.7007(8) 0.023(3) Uani 1 1 d . . . C30 C 0.0912(9) 0.4683(10) 0.7712(9) 0.022(3) Uani 1 1 d . . . H30 H 0.0844 0.3839 0.8089 0.027 Uiso 1 1 calc R . . C8 C 0.4966(9) 0.2025(9) 0.9953(8) 0.020(2) Uani 1 1 d . . . H8A H 0.4424 0.2072 1.0490 0.024 Uiso 1 1 calc R . . C32 C 0.8312(10) 0.4947(10) 0.5975(10) 0.032(3) Uani 1 1 d . . . H32A H 0.8319 0.5057 0.5237 0.048 Uiso 1 1 calc R . . H32B H 0.9113 0.4875 0.6192 0.048 Uiso 1 1 calc R . . H32C H 0.7935 0.5614 0.6128 0.048 Uiso 1 1 calc R . . C12 C 0.7582(10) -0.0624(10) 1.0961(9) 0.026(3) Uani 1 1 d . . . H12A H 0.8169 -0.1185 1.1205 0.031 Uiso 1 1 calc R . . N6 N 1.0381(8) 0.1384(9) 0.6743(9) 0.037(3) Uani 1 1 d . . . C3 C 0.1407(11) 0.6154(11) 0.9649(10) 0.035(3) Uani 1 1 d . . . H3 H 0.0625 0.6187 1.0001 0.042 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 Ho1 0.0181(3) 0.0281(3) 0.0230(3) -0.0096(2) 0.0000(2) 0.0059(2) Zn1 0.0198(7) 0.0273(7) 0.0187(7) -0.0091(6) -0.0008(5) 0.0074(5) Fe1 0.0220(8) 0.0237(9) 0.0239(9) -0.0101(7) 0.0014(7) 0.0055(7) O9 0.012(4) 0.028(4) 0.048(5) -0.014(4) 0.003(4) 0.007(3) O11 0.019(4) 0.043(5) 0.024(4) -0.019(4) 0.000(3) 0.000(4) O10 0.029(4) 0.047(5) 0.005(4) -0.005(4) -0.005(3) 0.009(4) O1 0.026(4) 0.026(4) 0.016(4) -0.008(3) -0.001(3) 0.014(3) O4 0.026(4) 0.026(4) 0.025(4) -0.013(3) -0.005(3) 0.009(3) O2 0.023(4) 0.042(5) 0.019(4) -0.007(4) -0.003(3) 0.009(4) O7 0.025(4) 0.029(4) 0.026(5) -0.001(4) 0.001(3) 0.019(4) O3 0.0209(18) 0.0213(18) 0.0193(18) -0.0062(10) -0.0017(10) 0.0010(10) O8 0.036(5) 0.028(5) 0.053(6) -0.005(4) 0.002(4) 0.007(4) O5 0.019(4) 0.029(4) 0.029(5) -0.011(4) -0.008(3) 0.007(3) O6 0.033(5) 0.029(5) 0.025(5) -0.003(4) 0.002(4) 0.007(4) N4 0.019(5) 0.019(5) 0.012(5) -0.004(4) 0.008(4) -0.004(4) N3 0.018(5) 0.035(6) 0.010(4) -0.013(4) -0.002(4) 0.003(4) N1 0.021(5) 0.019(5) 0.026(5) -0.007(4) -0.001(4) 0.010(4) C10 0.024(6) 0.023(6) 0.004(5) -0.002(4) -0.002(4) 0.001(5) C16 0.019(6) 0.043(8) 0.031(7) -0.019(6) 0.003(5) 0.012(5) C7 0.027(6) 0.029(6) 0.026(6) -0.020(5) 0.001(5) -0.002(5) O12 0.023(5) 0.057(6) 0.069(7) -0.032(5) 0.005(5) -0.010(4) C21 0.018(5) 0.012(5) 0.016(5) -0.005(4) -0.008(4) -0.001(4) N2 0.015(4) 0.026(5) 0.027(5) -0.012(4) -0.007(4) 0.010(4) C17 0.018(6) 0.008(5) 0.038(7) -0.012(5) 0.007(5) -0.002(4) C14 0.018(2) 0.018(2) 0.017(2) -0.0058(12) -0.0011(10) 0.0000(10) C18 0.042(7) 0.016(6) 0.021(6) -0.009(5) 0.002(5) -0.005(5) C19 0.032(6) 0.029(6) 0.018(6) -0.010(5) 0.001(5) -0.006(5) C31 0.021(3) 0.022(3) 0.021(3) -0.0064(12) -0.0017(10) 0.0003(10) C15 0.029(7) 0.061(9) 0.018(6) -0.019(6) -0.007(5) 0.023(6) C9 0.013(5) 0.031(6) 0.018(6) -0.009(5) -0.001(4) -0.008(5) C13 0.012(5) 0.028(6) 0.017(6) -0.005(5) -0.001(4) -0.003(4) C29 0.020(6) 0.029(6) 0.027(6) -0.009(5) 0.004(5) 0.007(5) C6 0.025(6) 0.026(6) 0.013(6) -0.006(5) -0.013(5) 0.015(5) N5 0.029(6) 0.025(6) 0.040(6) -0.013(5) -0.004(5) 0.010(5) C5 0.025(6) 0.031(7) 0.012(6) -0.006(5) -0.001(5) -0.002(5) C22 0.019(6) 0.019(6) 0.025(6) -0.005(5) -0.005(5) 0.001(4) C1 0.025(6) 0.040(7) 0.011(6) -0.013(5) 0.003(4) 0.000(5) C24 0.015(5) 0.021(6) 0.019(6) -0.009(5) -0.008(4) 0.005(4) C20 0.025(6) 0.017(6) 0.023(6) -0.012(5) -0.005(5) -0.001(5) C23 0.016(5) 0.029(6) 0.010(5) -0.002(5) -0.001(4) 0.002(5) C2 0.034(7) 0.034(7) 0.035(7) -0.018(6) 0.004(6) 0.005(6) C27 0.025(6) 0.034(7) 0.011(5) -0.012(5) 0.001(4) 0.003(5) C4 0.019(2) 0.018(2) 0.018(2) -0.0054(12) -0.0012(10) 0.0007(10) C28 0.032(7) 0.025(6) 0.029(7) -0.015(5) -0.006(5) 0.010(5) C11 0.039(7) 0.018(6) 0.021(6) -0.011(5) 0.004(5) -0.002(5) C25 0.021(6) 0.027(6) 0.024(6) 0.001(5) 0.010(5) -0.001(5) C26 0.034(6) 0.029(6) 0.008(5) -0.004(5) -0.010(5) 0.005(5) C30 0.011(5) 0.020(6) 0.031(7) -0.003(5) 0.007(5) 0.006(4) C8 0.024(6) 0.024(6) 0.017(6) -0.015(5) 0.000(5) 0.000(5) C32 0.031(7) 0.029(7) 0.033(7) -0.005(6) 0.007(5) -0.005(5) C12 0.030(6) 0.028(6) 0.022(6) -0.011(5) 0.000(5) 0.005(5) N6 0.014(5) 0.040(6) 0.061(8) -0.024(6) 0.003(5) 0.005(5) C3 0.030(7) 0.040(8) 0.046(8) -0.031(7) -0.003(6) 0.015(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O1 2.279(7) . ? Ho1 O6 2.288(8) . ? Ho1 O3 2.319(7) . ? Ho1 O10 2.414(8) . ? Ho1 O11 2.419(7) . ? Ho1 O9 2.426(7) . ? Ho1 O7 2.437(8) . ? Ho1 O4 2.487(7) . ? Ho1 O2 2.556(7) . ? Ho1 N6 2.849(10) . ? Ho1 N5 2.862(10) . ? Ho1 Zn1 3.4416(13) . ? Zn1 O5 2.007(8) . ? Zn1 O1 2.071(7) . ? Zn1 N4 2.074(9) . ? Zn1 O3 2.087(7) . ? Zn1 N2 2.105(9) . ? Fe1 C3 2.013(12) . ? Fe1 C1 2.015(11) . ? Fe1 C27 2.032(10) . ? Fe1 C26 2.036(11) . ? Fe1 C5 2.047(11) . ? Fe1 C30 2.047(12) . ? Fe1 C4 2.048(11) . ? Fe1 C2 2.055(13) . ? Fe1 C29 2.066(11) . ? Fe1 C28 2.076(11) . ? O9 N5 1.288(12) . ? O11 N6 1.240(12) . ? O10 N6 1.310(13) . ? O1 C14 1.344(12) . ? O4 C17 1.382(12) . ? O4 C16 1.453(12) . ? O2 C13 1.365(12) . ? O2 C15 1.448(13) . ? O7 N5 1.275(11) . ? O3 C22 1.332(13) . ? O8 N5 1.238(12) . ? O5 C31 1.256(12) . ? O6 C31 1.258(13) . ? N4 C23 1.319(13) . ? N4 N3 1.423(11) . ? N3 C24 1.292(13) . ? N1 C6 1.285(14) . ? N1 N2 1.423(11) . ? C10 C11 1.379(14) . ? C10 C9 1.391(14) . ? C7 C6 1.494(15) . ? O12 N6 1.221(12) . ? C21 C20 1.393(14) . ? C21 C22 1.416(14) . ? C21 C23 1.445(14) . ? N2 C8 1.271(13) . ? C17 C18 1.373(15) . ? C17 C22 1.413(15) . ? C14 C13 1.400(14) . ? C14 C9 1.403(14) . ? C18 C19 1.392(16) . ? C19 C20 1.349(15) . ? C31 C32 1.519(15) . ? C9 C8 1.462(15) . ? C13 C12 1.360(15) . ? C29 C30 1.410(14) . ? C29 C28 1.419(16) . ? C6 C1 1.491(15) . ? C5 C1 1.390(16) . ? C5 C4 1.421(15) . ? C1 C2 1.468(16) . ? C24 C26 1.454(15) . ? C24 C25 1.524(14) . ? C2 C3 1.448(16) . ? C27 C28 1.419(15) . ? C27 C26 1.430(15) . ? C4 C3 1.379(16) . ? C11 C12 1.385(15) . ? C26 C30 1.434(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ho1 O6 80.9(3) . . ? O1 Ho1 O3 67.2(2) . . ? O6 Ho1 O3 77.0(3) . . ? O1 Ho1 O10 103.4(3) . . ? O6 Ho1 O10 75.7(3) . . ? O3 Ho1 O10 152.3(3) . . ? O1 Ho1 O11 148.8(3) . . ? O6 Ho1 O11 74.1(3) . . ? O3 Ho1 O11 123.0(3) . . ? O10 Ho1 O11 52.7(2) . . ? O1 Ho1 O9 128.1(3) . . ? O6 Ho1 O9 148.5(3) . . ? O3 Ho1 O9 122.2(3) . . ? O10 Ho1 O9 84.5(3) . . ? O11 Ho1 O9 74.5(3) . . ? O1 Ho1 O7 85.0(3) . . ? O6 Ho1 O7 155.9(3) . . ? O3 Ho1 O7 79.6(2) . . ? O10 Ho1 O7 126.9(2) . . ? O11 Ho1 O7 124.5(3) . . ? O9 Ho1 O7 52.9(2) . . ? O1 Ho1 O4 131.7(2) . . ? O6 Ho1 O4 96.1(3) . . ? O3 Ho1 O4 65.3(2) . . ? O10 Ho1 O4 122.6(2) . . ? O11 Ho1 O4 70.3(2) . . ? O9 Ho1 O4 74.1(3) . . ? O7 Ho1 O4 78.9(3) . . ? O1 Ho1 O2 64.5(2) . . ? O6 Ho1 O2 119.0(3) . . ? O3 Ho1 O2 124.6(2) . . ? O10 Ho1 O2 66.6(2) . . ? O11 Ho1 O2 112.4(2) . . ? O9 Ho1 O2 72.9(3) . . ? O7 Ho1 O2 70.9(3) . . ? O4 Ho1 O2 144.5(3) . . ? O1 Ho1 N6 127.1(3) . . ? O6 Ho1 N6 70.9(3) . . ? O3 Ho1 N6 140.7(3) . . ? O10 Ho1 N6 27.3(3) . . ? O11 Ho1 N6 25.6(3) . . ? O9 Ho1 N6 80.3(3) . . ? O7 Ho1 N6 132.7(3) . . ? O4 Ho1 N6 95.8(3) . . ? O2 Ho1 N6 91.3(3) . . ? O1 Ho1 N5 107.1(3) . . ? O6 Ho1 N5 170.5(3) . . ? O3 Ho1 N5 101.2(3) . . ? O10 Ho1 N5 106.5(3) . . ? O11 Ho1 N5 99.7(3) . . ? O9 Ho1 N5 26.6(2) . . ? O7 Ho1 N5 26.3(2) . . ? O4 Ho1 N5 74.9(3) . . ? O2 Ho1 N5 69.8(3) . . ? N6 Ho1 N5 106.7(3) . . ? O1 Ho1 Zn1 35.64(17) . . ? O6 Ho1 Zn1 63.09(19) . . ? O3 Ho1 Zn1 36.30(18) . . ? O10 Ho1 Zn1 122.80(19) . . ? O11 Ho1 Zn1 135.10(19) . . ? O9 Ho1 Zn1 147.28(18) . . ? O7 Ho1 Zn1 94.42(16) . . ? O4 Ho1 Zn1 100.51(16) . . ? O2 Ho1 Zn1 100.06(17) . . ? N6 Ho1 Zn1 132.4(2) . . ? N5 Ho1 Zn1 120.7(2) . . ? O5 Zn1 O1 101.9(3) . . ? O5 Zn1 N4 100.3(3) . . ? O1 Zn1 N4 152.6(3) . . ? O5 Zn1 O3 95.6(3) . . ? O1 Zn1 O3 75.4(3) . . ? N4 Zn1 O3 86.6(3) . . ? O5 Zn1 N2 110.5(3) . . ? O1 Zn1 N2 88.2(3) . . ? N4 Zn1 N2 98.9(3) . . ? O3 Zn1 N2 151.7(3) . . ? O5 Zn1 Ho1 85.2(2) . . ? O1 Zn1 Ho1 39.88(19) . . ? N4 Zn1 Ho1 127.6(2) . . ? O3 Zn1 Ho1 41.12(19) . . ? N2 Zn1 Ho1 128.1(2) . . ? C3 Fe1 C1 70.0(4) . . ? C3 Fe1 C27 152.3(5) . . ? C1 Fe1 C27 127.4(4) . . ? C3 Fe1 C26 164.5(5) . . ? C1 Fe1 C26 107.1(4) . . ? C27 Fe1 C26 41.2(4) . . ? C3 Fe1 C5 68.1(5) . . ? C1 Fe1 C5 40.0(4) . . ? C27 Fe1 C5 109.8(4) . . ? C26 Fe1 C5 120.0(4) . . ? C3 Fe1 C30 126.0(5) . . ? C1 Fe1 C30 118.8(4) . . ? C27 Fe1 C30 68.6(4) . . ? C26 Fe1 C30 41.1(4) . . ? C5 Fe1 C30 153.8(4) . . ? C3 Fe1 C4 39.7(5) . . ? C1 Fe1 C4 68.5(4) . . ? C27 Fe1 C4 120.5(4) . . ? C26 Fe1 C4 154.6(4) . . ? C5 Fe1 C4 40.6(4) . . ? C30 Fe1 C4 163.4(4) . . ? C3 Fe1 C2 41.7(4) . . ? C1 Fe1 C2 42.3(4) . . ? C27 Fe1 C2 165.5(4) . . ? C26 Fe1 C2 126.1(4) . . ? C5 Fe1 C2 68.7(5) . . ? C30 Fe1 C2 106.1(5) . . ? C4 Fe1 C2 68.4(5) . . ? C3 Fe1 C29 107.3(5) . . ? C1 Fe1 C29 153.2(5) . . ? C27 Fe1 C29 67.3(4) . . ? C26 Fe1 C29 68.1(4) . . ? C5 Fe1 C29 165.4(4) . . ? C30 Fe1 C29 40.1(4) . . ? C4 Fe1 C29 127.3(4) . . ? C2 Fe1 C29 117.8(5) . . ? C3 Fe1 C28 117.8(5) . . ? C1 Fe1 C28 165.1(5) . . ? C27 Fe1 C28 40.4(4) . . ? C26 Fe1 C28 68.9(4) . . ? C5 Fe1 C28 128.5(5) . . ? C30 Fe1 C28 68.3(4) . . ? C4 Fe1 C28 108.6(4) . . ? C2 Fe1 C28 151.7(5) . . ? C29 Fe1 C28 40.1(4) . . ? N5 O9 Ho1 95.9(6) . . ? N6 O11 Ho1 97.0(6) . . ? N6 O10 Ho1 95.2(6) . . ? C14 O1 Zn1 128.3(6) . . ? C14 O1 Ho1 125.4(6) . . ? Zn1 O1 Ho1 104.5(3) . . ? C17 O4 C16 115.2(8) . . ? C17 O4 Ho1 119.3(6) . . ? C16 O4 Ho1 125.5(6) . . ? C13 O2 C15 116.4(8) . . ? C13 O2 Ho1 116.4(6) . . ? C15 O2 Ho1 125.7(6) . . ? N5 O7 Ho1 95.8(6) . . ? C22 O3 Zn1 129.6(6) . . ? C22 O3 Ho1 123.0(6) . . ? Zn1 O3 Ho1 102.6(3) . . ? C31 O5 Zn1 123.0(7) . . ? C31 O6 Ho1 142.9(7) . . ? C23 N4 N3 111.0(8) . . ? C23 N4 Zn1 126.8(7) . . ? N3 N4 Zn1 122.2(6) . . ? C24 N3 N4 116.9(9) . . ? C6 N1 N2 116.3(9) . . ? C11 C10 C9 119.9(10) . . ? C20 C21 C22 118.6(10) . . ? C20 C21 C23 116.7(9) . . ? C22 C21 C23 124.6(9) . . ? C8 N2 N1 109.6(9) . . ? C8 N2 Zn1 122.6(7) . . ? N1 N2 Zn1 125.5(7) . . ? C18 C17 O4 127.0(10) . . ? C18 C17 C22 121.1(10) . . ? O4 C17 C22 111.9(9) . . ? O1 C14 C13 118.1(9) . . ? O1 C14 C9 123.3(9) . . ? C13 C14 C9 118.6(9) . . ? C17 C18 C19 119.6(11) . . ? C20 C19 C18 120.3(11) . . ? O5 C31 O6 125.8(10) . . ? O5 C31 C32 117.6(10) . . ? O6 C31 C32 116.6(10) . . ? C10 C9 C14 119.7(10) . . ? C10 C9 C8 116.3(9) . . ? C14 C9 C8 123.9(9) . . ? C12 C13 O2 124.6(9) . . ? C12 C13 C14 121.2(10) . . ? O2 C13 C14 114.1(9) . . ? C30 C29 C28 109.8(10) . . ? C30 C29 Fe1 69.2(6) . . ? C28 C29 Fe1 70.3(7) . . ? N1 C6 C1 116.2(10) . . ? N1 C6 C7 127.9(10) . . ? C1 C6 C7 115.8(10) . . ? O8 N5 O7 123.2(10) . . ? O8 N5 O9 121.3(9) . . ? O7 N5 O9 115.4(9) . . ? O8 N5 Ho1 177.0(8) . . ? O7 N5 Ho1 57.9(5) . . ? O9 N5 Ho1 57.5(5) . . ? C1 C5 C4 108.9(10) . . ? C1 C5 Fe1 68.7(6) . . ? C4 C5 Fe1 69.7(6) . . ? O3 C22 C17 119.9(9) . . ? O3 C22 C21 122.0(10) . . ? C17 C22 C21 118.2(10) . . ? C5 C1 C2 108.1(10) . . ? C5 C1 C6 128.3(10) . . ? C2 C1 C6 123.4(10) . . ? C5 C1 Fe1 71.3(6) . . ? C2 C1 Fe1 70.3(7) . . ? C6 C1 Fe1 127.2(8) . . ? N3 C24 C26 116.9(10) . . ? N3 C24 C25 124.6(9) . . ? C26 C24 C25 118.4(9) . . ? C19 C20 C21 122.1(10) . . ? N4 C23 C21 127.1(9) . . ? C3 C2 C1 104.8(11) . . ? C3 C2 Fe1 67.6(7) . . ? C1 C2 Fe1 67.4(7) . . ? C28 C27 C26 109.5(10) . . ? C28 C27 Fe1 71.5(6) . . ? C26 C27 Fe1 69.6(6) . . ? C3 C4 C5 108.6(10) . . ? C3 C4 Fe1 68.8(7) . . ? C5 C4 Fe1 69.7(6) . . ? C27 C28 C29 106.4(10) . . ? C27 C28 Fe1 68.2(6) . . ? C29 C28 Fe1 69.6(6) . . ? C10 C11 C12 120.6(10) . . ? C27 C26 C30 106.7(9) . . ? C27 C26 C24 126.6(10) . . ? C30 C26 C24 126.8(10) . . ? C27 C26 Fe1 69.3(6) . . ? C30 C26 Fe1 69.9(6) . . ? C24 C26 Fe1 124.6(7) . . ? C29 C30 C26 107.7(10) . . ? C29 C30 Fe1 70.7(7) . . ? C26 C30 Fe1 69.0(6) . . ? N2 C8 C9 129.5(10) . . ? C13 C12 C11 119.8(11) . . ? O12 N6 O11 123.6(11) . . ? O12 N6 O10 121.9(11) . . ? O11 N6 O10 114.5(9) . . ? O12 N6 Ho1 173.8(8) . . ? O11 N6 Ho1 57.4(5) . . ? O10 N6 Ho1 57.6(5) . . ? C4 C3 C2 109.4(11) . . ? C4 C3 Fe1 71.5(7) . . ? C2 C3 Fe1 70.7(7) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.736 _refine_diff_density_min -1.141 _refine_diff_density_rms 0.257 _database_code_depnum_ccdc_archive 'CCDC 941862' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Zn-Eu _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H31 Eu Fe N6 O12 Zn' _chemical_formula_sum 'C32 H31 Eu Fe N6 O12 Zn' _chemical_formula_weight 964.84 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' Zn Zn 0.2839 1.4301 '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 Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.321(5) _cell_length_b 11.872(5) _cell_length_c 13.471(5) _cell_angle_alpha 72.297(5) _cell_angle_beta 86.370(5) _cell_angle_gamma 89.106(5) _cell_volume 1721.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3268 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 26.95 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960.0 _exptl_absorpt_coefficient_mu 2.980 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 0.812 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9341 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_unetI/netI 0.0565 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6294 _reflns_number_gt 5299 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6294 _refine_ls_number_parameters 483 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.000 _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 0.29376(2) 0.08601(2) 0.22878(2) 0.02101(11) Uani 1 1 d . . . Zn1 Zn 0.05287(5) 0.25753(5) 0.26584(4) 0.01948(16) Uani 1 1 d . . . Fe1 Fe -0.33126(7) 0.59192(7) 0.32168(6) 0.02101(19) Uani 1 1 d . . . O10 O 0.4980(4) 0.1165(4) 0.2697(3) 0.0308(10) Uani 1 1 d . . . O1 O 0.1703(3) 0.1388(3) 0.3530(3) 0.0216(8) Uani 1 1 d . . . O9 O 0.3683(3) -0.1130(3) 0.2326(3) 0.0260(9) Uani 1 1 d . . . N6 N 0.5441(4) 0.1355(4) 0.1778(4) 0.0292(11) Uani 1 1 d . . . O2 O 0.3324(3) -0.0200(3) 0.4202(3) 0.0259(9) Uani 1 1 d . . . O4 O 0.2467(3) 0.0610(3) 0.0559(3) 0.0234(9) Uani 1 1 d . . . O11 O 0.4763(4) 0.1197(4) 0.1117(3) 0.0311(10) Uani 1 1 d . . . C25 C -0.1119(5) 0.5429(5) 0.1000(4) 0.0239(12) Uani 1 1 d . . . H25A H -0.0376 0.5020 0.1058 0.036 Uiso 1 1 calc R . . H25B H -0.1038 0.6143 0.1183 0.036 Uiso 1 1 calc R . . H25C H -0.1351 0.5620 0.0295 0.036 Uiso 1 1 calc R . . O7 O 0.1843(3) -0.1042(3) 0.2827(3) 0.0264(9) Uani 1 1 d . . . C13 C 0.2515(5) -0.0013(5) 0.4952(4) 0.0204(12) Uani 1 1 d . . . C9 C 0.0816(5) 0.1120(4) 0.5260(4) 0.0187(11) Uani 1 1 d . . . O6 O 0.3173(3) 0.2896(3) 0.1706(3) 0.0289(9) Uani 1 1 d . . . O3 O 0.1070(3) 0.1549(3) 0.1696(3) 0.0210(8) Uani 1 1 d . . . O5 O 0.1568(3) 0.3950(3) 0.1910(3) 0.0227(8) Uani 1 1 d . . . N1 N -0.1144(4) 0.3578(4) 0.4155(3) 0.0206(10) Uani 1 1 d . . . N3 N -0.1974(4) 0.3529(4) 0.2134(3) 0.0187(9) Uani 1 1 d . . . C26 C -0.3126(5) 0.5215(5) 0.2009(4) 0.0194(11) Uani 1 1 d . . . O12 O 0.6475(4) 0.1656(4) 0.1544(4) 0.0427(12) Uani 1 1 d . . . O8 O 0.2607(4) -0.2751(4) 0.2789(4) 0.0464(12) Uani 1 1 d . . . C17 C 0.1422(5) 0.1074(4) 0.0126(4) 0.0186(11) Uani 1 1 d . . . C8 C -0.0063(5) 0.2041(5) 0.4971(4) 0.0197(11) Uani 1 1 d . . . H8A H -0.0601 0.2097 0.5505 0.024 Uiso 1 1 calc R . . C22 C 0.0716(5) 0.1584(4) 0.0763(4) 0.0173(11) Uani 1 1 d . . . C19 C 0.0004(5) 0.1548(5) -0.1179(4) 0.0226(12) Uani 1 1 d . . . H19 H -0.0240 0.1515 -0.1816 0.027 Uiso 1 1 calc R . . N4 N -0.0975(4) 0.2991(4) 0.1778(3) 0.0175(9) Uani 1 1 d . . . C21 C -0.0359(5) 0.2121(4) 0.0383(4) 0.0184(11) Uani 1 1 d . . . C6 C -0.0887(5) 0.4690(5) 0.3889(4) 0.0211(12) Uani 1 1 d . . . C10 C 0.0834(5) 0.0490(5) 0.6318(4) 0.0224(12) Uani 1 1 d . . . H10 H 0.0256 0.0636 0.6785 0.027 Uiso 1 1 calc R . . C27 C -0.4069(5) 0.4658(5) 0.2711(4) 0.0231(12) Uani 1 1 d . . . H27 H -0.4129 0.3812 0.3093 0.028 Uiso 1 1 calc R . . C7 C 0.0303(5) 0.5235(5) 0.3478(4) 0.0276(13) Uani 1 1 d . . . H7A H 0.0868 0.4622 0.3485 0.041 Uiso 1 1 calc R . . H7B H 0.0550 0.5687 0.3910 0.041 Uiso 1 1 calc R . . H7C H 0.0251 0.5743 0.2775 0.041 Uiso 1 1 calc R . . C18 C 0.1084(5) 0.1049(5) -0.0823(4) 0.0219(12) Uani 1 1 d . . . H18 H 0.1570 0.0702 -0.1230 0.026 Uiso 1 1 calc R . . C4 C -0.2986(5) 0.7114(5) 0.3999(4) 0.0288(13) Uani 1 1 d . . . H4 H -0.3262 0.7934 0.3817 0.035 Uiso 1 1 calc R . . C30 C -0.3391(5) 0.6463(5) 0.1619(4) 0.0220(12) Uani 1 1 d . . . H30 H -0.2900 0.7074 0.1116 0.026 Uiso 1 1 calc R . . C12 C 0.2518(5) -0.0609(5) 0.6003(4) 0.0236(12) Uani 1 1 d . . . H12 H 0.3077 -0.1191 0.6255 0.028 Uiso 1 1 calc R . . C14 C 0.1663(5) 0.0858(5) 0.4552(4) 0.0179(11) Uani 1 1 d . . . C15 C 0.4176(6) -0.1121(6) 0.4539(5) 0.0382(16) Uani 1 1 d . . . H15A H 0.4648 -0.0952 0.5044 0.057 Uiso 1 1 calc R . . H15B H 0.4678 -0.1165 0.3950 0.057 Uiso 1 1 calc R . . H15C H 0.3774 -0.1862 0.4848 0.057 Uiso 1 1 calc R . . N2 N -0.0194(4) 0.2795(4) 0.4064(3) 0.0195(10) Uani 1 1 d . . . C1 C -0.1846(5) 0.5474(5) 0.4057(4) 0.0217(12) Uani 1 1 d . . . C31 C 0.2639(5) 0.3856(5) 0.1587(4) 0.0247(12) Uani 1 1 d . . . C32 C 0.3282(5) 0.4988(5) 0.0965(5) 0.0341(15) Uani 1 1 d . . . H32A H 0.4094 0.4940 0.1141 0.051 Uiso 1 1 calc R . . H32B H 0.2911 0.5648 0.1129 0.051 Uiso 1 1 calc R . . H32C H 0.3247 0.5092 0.0232 0.051 Uiso 1 1 calc R . . C29 C -0.4505(5) 0.6633(5) 0.2106(4) 0.0269(13) Uani 1 1 d . . . H29 H -0.4912 0.7391 0.2004 0.032 Uiso 1 1 calc R . . N5 N 0.2713(4) -0.1666(4) 0.2655(4) 0.0268(11) Uani 1 1 d . . . C5 C -0.1904(5) 0.6720(5) 0.3627(4) 0.0256(13) Uani 1 1 d . . . H5 H -0.1307 0.7223 0.3141 0.031 Uiso 1 1 calc R . . C20 C -0.0696(5) 0.2088(4) -0.0588(4) 0.0193(11) Uani 1 1 d . . . H20 H -0.1403 0.2437 -0.0838 0.023 Uiso 1 1 calc R . . C16 C 0.3238(5) 0.0051(5) -0.0045(4) 0.0282(13) Uani 1 1 d . . . H16A H 0.2797 -0.0521 -0.0245 0.042 Uiso 1 1 calc R . . H16B H 0.3873 -0.0337 0.0367 0.042 Uiso 1 1 calc R . . H16C H 0.3558 0.0639 -0.0660 0.042 Uiso 1 1 calc R . . C24 C -0.2039(5) 0.4657(5) 0.1720(4) 0.0182(11) Uani 1 1 d . . . C3 C -0.3586(6) 0.6134(5) 0.4667(4) 0.0306(14) Uani 1 1 d . . . H3 H -0.4361 0.6153 0.5030 0.037 Uiso 1 1 calc R . . C28 C -0.4921(5) 0.5533(5) 0.2763(4) 0.0273(13) Uani 1 1 d . . . H28 H -0.5665 0.5395 0.3196 0.033 Uiso 1 1 calc R . . C2 C -0.2914(5) 0.5102(5) 0.4724(4) 0.0267(13) Uani 1 1 d . . . H2 H -0.3125 0.4292 0.5143 0.032 Uiso 1 1 calc R . . C23 C -0.1140(5) 0.2742(4) 0.0928(4) 0.0196(11) Uani 1 1 d . . . H23 H -0.1852 0.2994 0.0627 0.024 Uiso 1 1 calc R . . C11 C 0.1677(5) -0.0328(5) 0.6679(4) 0.0254(13) Uani 1 1 d . . . H11 H 0.1690 -0.0708 0.7392 0.030 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 Eu1 0.01773(17) 0.02646(17) 0.01979(17) -0.00895(12) -0.00026(11) 0.00656(12) Zn1 0.0181(3) 0.0249(3) 0.0163(3) -0.0080(3) -0.0009(3) 0.0075(3) Fe1 0.0207(4) 0.0214(4) 0.0207(4) -0.0068(3) 0.0019(3) 0.0057(3) O10 0.024(2) 0.043(2) 0.026(2) -0.0110(19) -0.0011(18) 0.0040(19) O1 0.021(2) 0.028(2) 0.0137(18) -0.0041(16) -0.0006(16) 0.0079(17) O9 0.020(2) 0.028(2) 0.030(2) -0.0099(18) 0.0022(17) 0.0064(18) N6 0.018(3) 0.035(3) 0.038(3) -0.016(2) -0.003(2) 0.002(2) O2 0.022(2) 0.038(2) 0.0179(19) -0.0087(17) -0.0010(16) 0.0139(18) O4 0.022(2) 0.029(2) 0.0221(19) -0.0132(17) 0.0014(16) 0.0065(17) O11 0.023(2) 0.042(2) 0.034(2) -0.020(2) -0.0020(19) 0.0003(19) C25 0.020(3) 0.028(3) 0.020(3) -0.002(2) 0.004(2) 0.002(2) O7 0.019(2) 0.034(2) 0.027(2) -0.0122(18) 0.0023(17) 0.0090(18) C13 0.015(3) 0.024(3) 0.026(3) -0.013(2) -0.002(2) 0.004(2) C9 0.019(3) 0.020(3) 0.021(3) -0.012(2) -0.004(2) 0.001(2) O6 0.017(2) 0.028(2) 0.040(2) -0.0082(19) 0.0042(18) 0.0030(18) O3 0.020(2) 0.027(2) 0.0182(18) -0.0110(16) -0.0019(16) 0.0091(17) O5 0.021(2) 0.024(2) 0.0207(19) -0.0026(16) 0.0010(16) 0.0014(17) N1 0.017(2) 0.026(2) 0.020(2) -0.011(2) -0.0030(19) 0.010(2) N3 0.016(2) 0.023(2) 0.017(2) -0.0060(19) 0.0017(18) 0.0019(19) C26 0.018(3) 0.023(3) 0.017(3) -0.007(2) -0.001(2) 0.002(2) O12 0.025(3) 0.055(3) 0.056(3) -0.030(3) 0.003(2) -0.006(2) O8 0.048(3) 0.028(2) 0.062(3) -0.014(2) 0.002(3) 0.005(2) C17 0.016(3) 0.020(3) 0.016(3) -0.001(2) 0.004(2) -0.001(2) C8 0.019(3) 0.027(3) 0.017(3) -0.012(2) 0.000(2) -0.001(2) C22 0.018(3) 0.018(2) 0.017(3) -0.007(2) -0.001(2) -0.001(2) C19 0.027(3) 0.028(3) 0.016(3) -0.012(2) 0.003(2) -0.005(3) N4 0.017(2) 0.017(2) 0.016(2) -0.0028(18) 0.0030(18) 0.0022(19) C21 0.023(3) 0.017(3) 0.013(2) -0.002(2) 0.005(2) 0.000(2) C6 0.024(3) 0.026(3) 0.014(2) -0.008(2) -0.001(2) 0.002(2) C10 0.021(3) 0.023(3) 0.023(3) -0.009(2) 0.006(2) -0.010(2) C27 0.026(3) 0.020(3) 0.024(3) -0.007(2) -0.002(2) 0.001(2) C7 0.029(3) 0.030(3) 0.030(3) -0.018(3) -0.009(3) 0.005(3) C18 0.024(3) 0.026(3) 0.016(3) -0.009(2) 0.007(2) 0.000(2) C4 0.034(3) 0.025(3) 0.029(3) -0.011(3) -0.001(3) 0.006(3) C30 0.022(3) 0.025(3) 0.019(3) -0.007(2) -0.004(2) 0.006(2) C12 0.027(3) 0.021(3) 0.018(3) 0.000(2) -0.004(2) 0.001(2) C14 0.015(3) 0.021(3) 0.019(3) -0.007(2) -0.005(2) -0.001(2) C15 0.032(4) 0.047(4) 0.038(4) -0.017(3) -0.010(3) 0.029(3) N2 0.018(2) 0.024(2) 0.018(2) -0.0093(19) -0.0014(19) 0.006(2) C1 0.022(3) 0.031(3) 0.015(3) -0.012(2) 0.002(2) 0.004(2) C31 0.022(3) 0.033(3) 0.021(3) -0.010(2) -0.004(2) -0.001(3) C32 0.027(3) 0.028(3) 0.039(4) 0.002(3) -0.001(3) 0.002(3) C29 0.027(3) 0.027(3) 0.029(3) -0.012(3) -0.002(3) 0.009(3) N5 0.024(3) 0.029(3) 0.027(3) -0.008(2) -0.002(2) 0.008(2) C5 0.029(3) 0.025(3) 0.028(3) -0.016(3) -0.003(3) 0.006(3) C20 0.017(3) 0.022(3) 0.017(3) -0.003(2) -0.003(2) -0.004(2) C16 0.029(3) 0.031(3) 0.025(3) -0.011(3) 0.005(3) 0.007(3) C24 0.019(3) 0.023(3) 0.014(2) -0.007(2) -0.002(2) 0.001(2) C3 0.030(3) 0.037(3) 0.030(3) -0.019(3) -0.001(3) 0.013(3) C28 0.024(3) 0.028(3) 0.027(3) -0.005(3) 0.002(3) 0.001(3) C2 0.033(3) 0.029(3) 0.018(3) -0.008(2) 0.001(2) 0.008(3) C23 0.012(3) 0.019(3) 0.024(3) -0.003(2) 0.001(2) 0.002(2) C11 0.033(3) 0.021(3) 0.020(3) -0.004(2) 0.001(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O6 2.317(4) . ? Eu1 O1 2.337(3) . ? Eu1 O3 2.353(4) . ? Eu1 O10 2.468(4) . ? Eu1 O7 2.478(4) . ? Eu1 O11 2.479(4) . ? Eu1 O9 2.484(4) . ? Eu1 O4 2.526(4) . ? Eu1 O2 2.564(4) . ? Eu1 N6 2.900(5) . ? Eu1 N5 2.900(5) . ? Eu1 Zn1 3.4792(12) . ? Zn1 O5 1.993(4) . ? Zn1 O1 2.065(4) . ? Zn1 O3 2.092(3) . ? Zn1 N2 2.103(4) . ? Zn1 N4 2.103(4) . ? Fe1 C1 2.040(6) . ? Fe1 C26 2.042(5) . ? Fe1 C2 2.043(5) . ? Fe1 C27 2.043(6) . ? Fe1 C3 2.050(6) . ? Fe1 C29 2.056(6) . ? Fe1 C5 2.057(6) . ? Fe1 C30 2.057(5) . ? Fe1 C4 2.058(6) . ? Fe1 C28 2.058(6) . ? O10 N6 1.267(6) . ? O1 C14 1.327(6) . ? O9 N5 1.263(6) . ? N6 O12 1.223(6) . ? N6 O11 1.270(6) . ? O2 C13 1.387(6) . ? O2 C15 1.433(6) . ? O4 C17 1.384(6) . ? O4 C16 1.444(6) . ? C25 C24 1.492(7) . ? O7 N5 1.275(6) . ? C13 C12 1.377(7) . ? C13 C14 1.409(7) . ? C9 C10 1.395(7) . ? C9 C14 1.408(7) . ? C9 C8 1.446(7) . ? O6 C31 1.253(7) . ? O3 C22 1.331(6) . ? O5 C31 1.277(7) . ? N1 C6 1.292(7) . ? N1 N2 1.434(6) . ? N3 C24 1.287(7) . ? N3 N4 1.418(6) . ? C26 C27 1.409(8) . ? C26 C30 1.447(7) . ? C26 C24 1.475(7) . ? O8 N5 1.252(6) . ? C17 C18 1.367(7) . ? C17 C22 1.399(7) . ? C8 N2 1.292(6) . ? C22 C21 1.416(7) . ? C19 C20 1.374(7) . ? C19 C18 1.398(8) . ? N4 C23 1.292(7) . ? C21 C20 1.398(7) . ? C21 C23 1.445(7) . ? C6 C1 1.471(7) . ? C6 C7 1.501(8) . ? C10 C11 1.354(8) . ? C27 C28 1.421(8) . ? C4 C3 1.391(8) . ? C4 C5 1.420(8) . ? C30 C29 1.424(8) . ? C12 C11 1.382(7) . ? C1 C5 1.417(8) . ? C1 C2 1.449(8) . ? C31 C32 1.519(8) . ? C29 C28 1.404(8) . ? C3 C2 1.417(8) . ? 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 O6 Eu1 O1 79.79(13) . . ? O6 Eu1 O3 76.51(13) . . ? O1 Eu1 O3 66.34(12) . . ? O6 Eu1 O10 76.24(14) . . ? O1 Eu1 O10 105.96(13) . . ? O3 Eu1 O10 152.62(14) . . ? O6 Eu1 O7 156.58(13) . . ? O1 Eu1 O7 86.40(13) . . ? O3 Eu1 O7 80.65(13) . . ? O10 Eu1 O7 126.14(13) . . ? O6 Eu1 O11 75.39(13) . . ? O1 Eu1 O11 149.75(14) . . ? O3 Eu1 O11 122.71(13) . . ? O10 Eu1 O11 51.43(13) . . ? O7 Eu1 O11 122.49(12) . . ? O6 Eu1 O9 149.25(13) . . ? O1 Eu1 O9 128.62(13) . . ? O3 Eu1 O9 122.42(13) . . ? O10 Eu1 O9 83.51(14) . . ? O7 Eu1 O9 51.61(13) . . ? O11 Eu1 O9 73.89(13) . . ? O6 Eu1 O4 96.99(13) . . ? O1 Eu1 O4 129.84(12) . . ? O3 Eu1 O4 64.32(11) . . ? O10 Eu1 O4 121.99(12) . . ? O7 Eu1 O4 77.47(12) . . ? O11 Eu1 O4 70.90(13) . . ? O9 Eu1 O4 74.36(12) . . ? O6 Eu1 O2 117.23(14) . . ? O1 Eu1 O2 64.13(12) . . ? O3 Eu1 O2 124.10(12) . . ? O10 Eu1 O2 67.73(13) . . ? O7 Eu1 O2 72.10(13) . . ? O11 Eu1 O2 113.11(13) . . ? O9 Eu1 O2 74.41(12) . . ? O4 Eu1 O2 145.66(13) . . ? O6 Eu1 N6 72.45(14) . . ? O1 Eu1 N6 128.29(13) . . ? O3 Eu1 N6 141.12(14) . . ? O10 Eu1 N6 25.73(13) . . ? O7 Eu1 N6 130.48(13) . . ? O11 Eu1 N6 25.82(13) . . ? O9 Eu1 N6 79.23(13) . . ? O4 Eu1 N6 96.69(13) . . ? O2 Eu1 N6 91.20(13) . . ? O6 Eu1 N5 170.50(14) . . ? O1 Eu1 N5 108.38(13) . . ? O3 Eu1 N5 101.98(13) . . ? O10 Eu1 N5 105.34(14) . . ? O7 Eu1 N5 25.94(12) . . ? O11 Eu1 N5 98.11(13) . . ? O9 Eu1 N5 25.67(13) . . ? O4 Eu1 N5 74.13(13) . . ? O2 Eu1 N5 71.53(13) . . ? N6 Eu1 N5 104.77(14) . . ? O6 Eu1 Zn1 62.39(10) . . ? O1 Eu1 Zn1 35.11(8) . . ? O3 Eu1 Zn1 35.90(8) . . ? O10 Eu1 Zn1 124.50(10) . . ? O7 Eu1 Zn1 95.71(9) . . ? O11 Eu1 Zn1 135.35(10) . . ? O9 Eu1 Zn1 147.28(9) . . ? O4 Eu1 Zn1 99.30(8) . . ? O2 Eu1 Zn1 99.20(8) . . ? N6 Eu1 Zn1 133.44(10) . . ? N5 Eu1 Zn1 121.62(10) . . ? O5 Zn1 O1 102.57(15) . . ? O5 Zn1 O3 95.15(15) . . ? O1 Zn1 O3 76.23(14) . . ? O5 Zn1 N2 109.65(16) . . ? O1 Zn1 N2 87.72(15) . . ? O3 Zn1 N2 152.99(16) . . ? O5 Zn1 N4 100.39(16) . . ? O1 Zn1 N4 152.29(16) . . ? O3 Zn1 N4 86.49(15) . . ? N2 Zn1 N4 98.99(17) . . ? O5 Zn1 Eu1 85.16(11) . . ? O1 Zn1 Eu1 40.61(10) . . ? O3 Zn1 Eu1 41.26(10) . . ? N2 Zn1 Eu1 128.25(12) . . ? N4 Zn1 Eu1 127.68(12) . . ? C1 Fe1 C26 107.6(2) . . ? C1 Fe1 C2 41.6(2) . . ? C26 Fe1 C2 126.2(2) . . ? C1 Fe1 C27 118.2(2) . . ? C26 Fe1 C27 40.4(2) . . ? C2 Fe1 C27 106.3(2) . . ? C1 Fe1 C3 68.6(2) . . ? C26 Fe1 C3 163.7(2) . . ? C2 Fe1 C3 40.5(2) . . ? C27 Fe1 C3 126.3(2) . . ? C1 Fe1 C29 166.0(2) . . ? C26 Fe1 C29 68.5(2) . . ? C2 Fe1 C29 151.6(2) . . ? C27 Fe1 C29 68.0(2) . . ? C3 Fe1 C29 119.1(2) . . ? C1 Fe1 C5 40.5(2) . . ? C26 Fe1 C5 120.7(2) . . ? C2 Fe1 C5 68.4(2) . . ? C27 Fe1 C5 153.6(2) . . ? C3 Fe1 C5 67.4(2) . . ? C29 Fe1 C5 129.0(2) . . ? C1 Fe1 C30 127.8(2) . . ? C26 Fe1 C30 41.3(2) . . ? C2 Fe1 C30 165.6(2) . . ? C27 Fe1 C30 68.6(2) . . ? C3 Fe1 C30 153.3(2) . . ? C29 Fe1 C30 40.5(2) . . ? C5 Fe1 C30 109.8(2) . . ? C1 Fe1 C4 68.4(2) . . ? C26 Fe1 C4 155.3(2) . . ? C2 Fe1 C4 67.9(2) . . ? C27 Fe1 C4 163.6(2) . . ? C3 Fe1 C4 39.6(2) . . ? C29 Fe1 C4 109.3(2) . . ? C5 Fe1 C4 40.4(2) . . ? C30 Fe1 C4 120.7(2) . . ? C1 Fe1 C28 152.4(2) . . ? C26 Fe1 C28 68.0(2) . . ? C2 Fe1 C28 117.6(2) . . ? C27 Fe1 C28 40.5(2) . . ? C3 Fe1 C28 107.7(2) . . ? C29 Fe1 C28 39.9(2) . . ? C5 Fe1 C28 165.3(2) . . ? C30 Fe1 C28 67.9(2) . . ? C4 Fe1 C28 127.2(2) . . ? N6 O10 Eu1 96.6(3) . . ? C14 O1 Zn1 129.2(3) . . ? C14 O1 Eu1 125.5(3) . . ? Zn1 O1 Eu1 104.28(14) . . ? N5 O9 Eu1 95.9(3) . . ? O12 N6 O10 122.4(5) . . ? O12 N6 O11 122.0(5) . . ? O10 N6 O11 115.6(5) . . ? O12 N6 Eu1 175.0(4) . . ? O10 N6 Eu1 57.7(3) . . ? O11 N6 Eu1 58.3(3) . . ? C13 O2 C15 117.5(4) . . ? C13 O2 Eu1 117.0(3) . . ? C15 O2 Eu1 124.5(3) . . ? C17 O4 C16 116.6(4) . . ? C17 O4 Eu1 118.8(3) . . ? C16 O4 Eu1 124.6(3) . . ? N6 O11 Eu1 95.9(3) . . ? N5 O7 Eu1 95.9(3) . . ? C12 C13 O2 124.4(5) . . ? C12 C13 C14 121.4(5) . . ? O2 C13 C14 114.2(4) . . ? C10 C9 C14 118.9(5) . . ? C10 C9 C8 116.8(5) . . ? C14 C9 C8 124.2(5) . . ? C31 O6 Eu1 143.7(4) . . ? C22 O3 Zn1 129.5(3) . . ? C22 O3 Eu1 123.8(3) . . ? Zn1 O3 Eu1 102.84(14) . . ? C31 O5 Zn1 123.9(4) . . ? C6 N1 N2 116.5(5) . . ? C24 N3 N4 115.0(4) . . ? C27 C26 C30 108.0(5) . . ? C27 C26 C24 127.2(5) . . ? C30 C26 C24 124.8(5) . . ? C27 C26 Fe1 69.9(3) . . ? C30 C26 Fe1 69.9(3) . . ? C24 C26 Fe1 124.9(4) . . ? C18 C17 O4 124.8(5) . . ? C18 C17 C22 122.0(5) . . ? O4 C17 C22 113.2(4) . . ? N2 C8 C9 128.2(5) . . ? O3 C22 C17 119.4(5) . . ? O3 C22 C21 122.5(5) . . ? C17 C22 C21 118.0(5) . . ? C20 C19 C18 120.0(5) . . ? C23 N4 N3 112.9(4) . . ? C23 N4 Zn1 126.3(4) . . ? N3 N4 Zn1 120.7(3) . . ? C20 C21 C22 119.4(5) . . ? C20 C21 C23 116.5(5) . . ? C22 C21 C23 124.0(5) . . ? N1 C6 C1 116.0(5) . . ? N1 C6 C7 126.1(5) . . ? C1 C6 C7 117.9(5) . . ? C11 C10 C9 121.4(5) . . ? C26 C27 C28 108.1(5) . . ? C26 C27 Fe1 69.8(3) . . ? C28 C27 Fe1 70.3(3) . . ? C17 C18 C19 119.6(5) . . ? C3 C4 C5 108.2(5) . . ? C3 C4 Fe1 69.9(3) . . ? C5 C4 Fe1 69.8(3) . . ? C29 C30 C26 106.8(5) . . ? C29 C30 Fe1 69.7(3) . . ? C26 C30 Fe1 68.8(3) . . ? C13 C12 C11 119.0(5) . . ? O1 C14 C9 123.5(5) . . ? O1 C14 C13 118.3(5) . . ? C9 C14 C13 118.2(5) . . ? C8 N2 N1 108.7(4) . . ? C8 N2 Zn1 123.7(4) . . ? N1 N2 Zn1 125.4(3) . . ? C5 C1 C2 107.0(5) . . ? C5 C1 C6 127.4(5) . . ? C2 C1 C6 125.6(5) . . ? C5 C1 Fe1 70.4(3) . . ? C2 C1 Fe1 69.3(3) . . ? C6 C1 Fe1 126.2(4) . . ? O6 C31 O5 124.6(5) . . ? O6 C31 C32 118.1(5) . . ? O5 C31 C32 117.2(5) . . ? C28 C29 C30 108.6(5) . . ? C28 C29 Fe1 70.1(3) . . ? C30 C29 Fe1 69.8(3) . . ? O8 N5 O9 121.7(5) . . ? O8 N5 O7 121.7(5) . . ? O9 N5 O7 116.6(4) . . ? O8 N5 Eu1 178.5(4) . . ? O9 N5 Eu1 58.4(2) . . ? O7 N5 Eu1 58.2(3) . . ? C1 C5 C4 108.5(5) . . ? C1 C5 Fe1 69.2(3) . . ? C4 C5 Fe1 69.9(4) . . ? C19 C20 C21 120.9(5) . . ? N3 C24 C26 115.7(5) . . ? N3 C24 C25 126.0(5) . . ? C26 C24 C25 118.3(5) . . ? C4 C3 C2 109.4(5) . . ? C4 C3 Fe1 70.5(3) . . ? C2 C3 Fe1 69.5(3) . . ? C29 C28 C27 108.5(5) . . ? C29 C28 Fe1 70.0(3) . . ? C27 C28 Fe1 69.2(3) . . ? C3 C2 C1 107.0(5) . . ? C3 C2 Fe1 70.0(3) . . ? C1 C2 Fe1 69.1(3) . . ? N4 C23 C21 128.4(5) . . ? C10 C11 C12 121.0(5) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.924 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.151 _database_code_depnum_ccdc_archive 'CCDC 941863'