# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Peng Cheng' _publ_contact_author_email PCHENG@NANKAI.EDU.CN _publ_section_title ; A Porous 3D Heterometal-Organic Framework Containing Both Lanthanide and High-Spin Fe(II) Ions ; loop_ _publ_author_name 'Peng Cheng' 'Xiao-Yan Chen' 'Zhi Chen' 'Dai-Zheng Liao' 'Wei Shi' ; Shi-Ping Yan ; 'Bin Zhao' # Attachment '1.cif' data_030128b _database_code_depnum_ccdc_archive 'CCDC 694298' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H18 Eu Fe1.50 N3 O16.50' _chemical_formula_weight 812.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6/mcc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 15.238(3) _cell_length_b 15.238(3) _cell_length_c 15.663(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3149.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 847 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 26.21 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 2.728 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.7721 _exptl_absorpt_correction_T_max 0.8987 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 . _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8226 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.02 _reflns_number_total 960 _reflns_number_gt 670 _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^)+(0.0328P)^2^+6.1385P] 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 960 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 0.3333 0.6667 0.2500 0.01742(17) Uani 1 6 d S . . Fe1 Fe 0.5000 0.5000 0.0000 0.0200(3) Uani 1 4 d S . . O1 O 0.4133(2) 0.6120(2) 0.14351(19) 0.0314(8) Uani 1 1 d . . . O2 O 0.5525(3) 0.6157(3) 0.0915(2) 0.0414(9) Uani 1 1 d . . . O3 O 0.6509(3) 0.5122(4) 0.0000 0.0321(11) Uani 1 2 d S . . N1 N 0.5227(3) 0.76134(17) 0.2500 0.0240(10) Uani 1 2 d S . . C1 C 0.7300(5) 0.8650(2) 0.2500 0.052(2) Uani 1 2 d S . . H1 H 0.8005 0.9002 0.2500 0.062 Uiso 1 2 calc SR . . C2 C 0.6783(4) 0.7868(4) 0.1936(4) 0.0423(14) Uani 1 1 d . . . H2 H 0.7127 0.7689 0.1547 0.051 Uiso 1 1 calc R . . C3 C 0.5740(3) 0.7357(3) 0.1961(3) 0.0275(10) Uani 1 1 d . . . C4 C 0.5084(4) 0.6475(3) 0.1387(3) 0.0282(11) Uani 1 1 d . . . O4 O 0.7903(13) 0.7392(12) 0.0000 0.114(7) Uani 0.50 2 d SP . . 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 0.0193(2) 0.0193(2) 0.0137(2) 0.000 0.000 0.00964(10) Fe1 0.0263(8) 0.0219(7) 0.0166(5) 0.000 0.000 0.0156(5) O1 0.0309(19) 0.038(2) 0.0269(16) -0.0113(15) -0.0010(15) 0.0183(17) O2 0.037(2) 0.049(2) 0.041(2) -0.0207(19) 0.0002(18) 0.0246(18) O3 0.028(3) 0.036(3) 0.035(3) 0.000 0.000 0.018(2) N1 0.026(2) 0.0231(17) 0.024(2) -0.003(3) 0.000 0.0128(12) C1 0.023(3) 0.043(3) 0.083(6) -0.017(6) 0.000 0.0114(16) C2 0.031(3) 0.040(3) 0.056(4) -0.013(3) 0.003(3) 0.019(2) C3 0.028(2) 0.030(3) 0.029(3) -0.005(2) 0.002(2) 0.018(2) C4 0.037(3) 0.030(3) 0.020(2) -0.003(2) 0.000(2) 0.018(2) O4 0.114(13) 0.090(11) 0.053(9) 0.000 0.000 -0.013(10) _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 O1 2.444(3) 12_565 ? Eu1 O1 2.444(3) 3_565 ? Eu1 O1 2.444(3) 11 ? Eu1 O1 2.444(3) 2_665 ? Eu1 O1 2.444(3) . ? Eu1 O1 2.444(3) 10_665 ? Eu1 N1 2.499(4) 2_665 ? Eu1 N1 2.499(4) 3_565 ? Eu1 N1 2.499(5) . ? Fe1 O2 2.096(3) 13_665 ? Fe1 O2 2.096(3) . ? Fe1 O2 2.096(3) 16 ? Fe1 O2 2.096(3) 4_665 ? Fe1 O3 2.212(4) . ? Fe1 O3 2.212(4) 13_665 ? O1 C4 1.270(6) . ? O2 C4 1.249(6) . ? N1 C3 1.336(5) . ? N1 C3 1.336(5) 12_565 ? C1 C2 1.372(6) 12_565 ? C1 C2 1.372(6) . ? C1 H1 0.9300 . ? C2 C3 1.376(6) . ? C2 H2 0.9300 . ? C3 C4 1.507(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 O1 Eu1 O1 145.68(15) 12_565 3_565 ? O1 Eu1 O1 78.55(11) 12_565 11 ? O1 Eu1 O1 86.77(15) 3_565 11 ? O1 Eu1 O1 86.77(15) 12_565 2_665 ? O1 Eu1 O1 78.55(11) 3_565 2_665 ? O1 Eu1 O1 128.85(15) 11 2_665 ? O1 Eu1 O1 128.85(15) 12_565 . ? O1 Eu1 O1 78.55(11) 3_565 . ? O1 Eu1 O1 145.68(15) 11 . ? O1 Eu1 O1 78.55(11) 2_665 . ? O1 Eu1 O1 78.55(11) 12_565 10_665 ? O1 Eu1 O1 128.85(15) 3_565 10_665 ? O1 Eu1 O1 78.55(11) 11 10_665 ? O1 Eu1 O1 145.68(15) 2_665 10_665 ? O1 Eu1 O1 86.77(15) . 10_665 ? O1 Eu1 N1 72.84(8) 12_565 2_665 ? O1 Eu1 N1 72.84(8) 3_565 2_665 ? O1 Eu1 N1 64.43(8) 11 2_665 ? O1 Eu1 N1 64.43(8) 2_665 2_665 ? O1 Eu1 N1 136.61(8) . 2_665 ? O1 Eu1 N1 136.61(8) 10_665 2_665 ? O1 Eu1 N1 136.61(8) 12_565 3_565 ? O1 Eu1 N1 64.43(8) 3_565 3_565 ? O1 Eu1 N1 72.84(8) 11 3_565 ? O1 Eu1 N1 136.61(8) 2_665 3_565 ? O1 Eu1 N1 72.84(8) . 3_565 ? O1 Eu1 N1 64.43(8) 10_665 3_565 ? N1 Eu1 N1 120.0 2_665 3_565 ? O1 Eu1 N1 64.43(8) 12_565 . ? O1 Eu1 N1 136.61(8) 3_565 . ? O1 Eu1 N1 136.61(8) 11 . ? O1 Eu1 N1 72.84(8) 2_665 . ? O1 Eu1 N1 64.43(8) . . ? O1 Eu1 N1 72.84(8) 10_665 . ? N1 Eu1 N1 120.0 2_665 . ? N1 Eu1 N1 120.0 3_565 . ? O2 Fe1 O2 180.0(2) 13_665 . ? O2 Fe1 O2 93.7(2) 13_665 16 ? O2 Fe1 O2 86.3(2) . 16 ? O2 Fe1 O2 86.3(2) 13_665 4_665 ? O2 Fe1 O2 93.7(2) . 4_665 ? O2 Fe1 O2 180.0 16 4_665 ? O2 Fe1 O3 90.83(13) 13_665 . ? O2 Fe1 O3 89.17(13) . . ? O2 Fe1 O3 89.17(13) 16 . ? O2 Fe1 O3 90.83(13) 4_665 . ? O2 Fe1 O3 89.17(13) 13_665 13_665 ? O2 Fe1 O3 90.83(13) . 13_665 ? O2 Fe1 O3 90.83(13) 16 13_665 ? O2 Fe1 O3 89.17(13) 4_665 13_665 ? O3 Fe1 O3 180.0 . 13_665 ? C4 O1 Eu1 123.5(3) . . ? C4 O2 Fe1 132.7(3) . . ? C3 N1 C3 119.0(5) . 12_565 ? C3 N1 Eu1 120.5(3) . . ? C3 N1 Eu1 120.5(3) 12_565 . ? C2 C1 C2 120.3(6) 12_565 . ? C2 C1 H1 119.8 12_565 . ? C2 C1 H1 119.8 . . ? C1 C2 C3 118.2(5) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? N1 C3 C2 122.1(5) . . ? N1 C3 C4 114.4(4) . . ? C2 C3 C4 123.5(4) . . ? O2 C4 O1 126.2(4) . . ? O2 C4 C3 116.9(4) . . ? O1 C4 C3 116.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Eu1 O1 C4 4.8(3) 12_565 . . . ? O1 Eu1 O1 C4 161.6(4) 3_565 . . . ? O1 Eu1 O1 C4 -131.9(4) 11 . . . ? O1 Eu1 O1 C4 81.1(4) 2_665 . . . ? O1 Eu1 O1 C4 -67.7(3) 10_665 . . . ? N1 Eu1 O1 C4 112.3(3) 2_665 . . . ? N1 Eu1 O1 C4 -131.9(4) 3_565 . . . ? N1 Eu1 O1 C4 4.8(3) . . . . ? O2 Fe1 O2 C4 0(100) 13_665 . . . ? O2 Fe1 O2 C4 103.8(5) 16 . . . ? O2 Fe1 O2 C4 -76.2(5) 4_665 . . . ? O3 Fe1 O2 C4 -167.0(5) . . . . ? O3 Fe1 O2 C4 13.0(5) 13_665 . . . ? O1 Eu1 N1 C3 178.0(2) 12_565 . . . ? O1 Eu1 N1 C3 -36.2(3) 3_565 . . . ? O1 Eu1 N1 C3 143.8(3) 11 . . . ? O1 Eu1 N1 C3 -87.2(3) 2_665 . . . ? O1 Eu1 N1 C3 -2.0(2) . . . . ? O1 Eu1 N1 C3 92.8(3) 10_665 . . . ? N1 Eu1 N1 C3 -132.8(2) 2_665 . . . ? N1 Eu1 N1 C3 47.2(2) 3_565 . . . ? O1 Eu1 N1 C3 -2.0(2) 12_565 . . 12_565 ? O1 Eu1 N1 C3 143.8(3) 3_565 . . 12_565 ? O1 Eu1 N1 C3 -36.2(3) 11 . . 12_565 ? O1 Eu1 N1 C3 92.8(3) 2_665 . . 12_565 ? O1 Eu1 N1 C3 178.0(2) . . . 12_565 ? O1 Eu1 N1 C3 -87.2(3) 10_665 . . 12_565 ? N1 Eu1 N1 C3 47.2(2) 2_665 . . 12_565 ? N1 Eu1 N1 C3 -132.8(2) 3_565 . . 12_565 ? C2 C1 C2 C3 -0.7(4) 12_565 . . . ? C3 N1 C3 C2 -0.8(4) 12_565 . . . ? Eu1 N1 C3 C2 179.2(4) . . . . ? C3 N1 C3 C4 179.7(5) 12_565 . . . ? Eu1 N1 C3 C4 -0.3(5) . . . . ? C1 C2 C3 N1 1.5(8) . . . . ? C1 C2 C3 C4 -179.0(4) . . . . ? Fe1 O2 C4 O1 2.0(8) . . . . ? Fe1 O2 C4 C3 -178.8(3) . . . . ? Eu1 O1 C4 O2 172.4(4) . . . . ? Eu1 O1 C4 C3 -6.8(6) . . . . ? N1 C3 C4 O2 -174.8(4) . . . . ? C2 C3 C4 O2 5.6(8) . . . . ? N1 C3 C4 O1 4.4(6) . . . . ? C2 C3 C4 O1 -175.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.014 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.091 # Attachment '2.cif' data_030128a _database_code_depnum_ccdc_archive 'CCDC 694299' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H18 Fe1.50 Gd N3 O16.50' _chemical_formula_weight 817.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6/mcc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 15.291(4) _cell_length_b 15.291(4) _cell_length_c 15.573(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3153.4(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 851 _cell_measurement_theta_min 3.73 _cell_measurement_theta_max 26.39 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 2.839 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.7644 _exptl_absorpt_correction_T_max 0.8949 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 7195 _diffrn_reflns_av_R_equivalents 0.1206 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.01 _reflns_number_total 948 _reflns_number_gt 610 _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^)+(0.0561P)^2^+1.4071P] 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 948 _refine_ls_number_parameters 76 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Gd1 Gd 0.3333 0.6667 0.2500 0.0190(3) Uani 1 6 d S . . Fe1 Fe 0.5000 0.5000 0.0000 0.0194(4) Uani 1 4 d S . . O1 O 0.4138(3) 0.6131(3) 0.1433(3) 0.0292(11) Uani 1 1 d . . . O2 O 0.5529(3) 0.6153(3) 0.0921(3) 0.0374(13) Uani 1 1 d . . . O3 O 0.6489(4) 0.5118(5) 0.0000 0.0293(15) Uani 1 2 d S . . N1 N 0.5223(5) 0.7611(2) 0.2500 0.0234(15) Uani 1 2 d S . . C1 C 0.7297(7) 0.8649(3) 0.2500 0.049(3) Uani 1 2 d S . . H1 H 0.7999 0.9000 0.2500 0.19(9) Uiso 1 2 calc SR . . C2 C 0.6785(5) 0.7858(5) 0.1952(6) 0.044(2) Uani 1 1 d . . . H2 H 0.7131 0.7659 0.1581 0.031(18) Uiso 1 1 calc R . . C3 C 0.5740(5) 0.7357(5) 0.1959(5) 0.0278(15) Uani 1 1 d . . . C4 C 0.5084(5) 0.6473(5) 0.1385(4) 0.0279(15) Uani 1 1 d . . . O4 O 0.7919(17) 0.7350(14) 0.0000 0.103(8) Uani 0.50 2 d SP . . 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 0.0200(3) 0.0200(3) 0.0169(4) 0.000 0.000 0.01001(14) Fe1 0.0246(11) 0.0206(10) 0.0170(9) 0.000 0.000 0.0144(6) O1 0.025(3) 0.032(3) 0.027(3) -0.011(2) -0.002(2) 0.012(2) O2 0.030(3) 0.042(3) 0.043(3) -0.019(3) 0.001(2) 0.020(2) O3 0.024(3) 0.031(4) 0.035(4) 0.000 0.000 0.015(3) N1 0.025(3) 0.024(2) 0.022(4) -0.006(4) 0.000 0.0127(17) C1 0.019(4) 0.043(4) 0.078(8) -0.018(7) 0.000 0.010(2) C2 0.031(4) 0.044(5) 0.057(6) -0.012(4) 0.004(4) 0.019(4) C3 0.024(3) 0.031(4) 0.027(4) -0.006(3) 0.004(3) 0.013(3) C4 0.037(4) 0.025(3) 0.022(4) -0.005(3) 0.002(3) 0.015(3) O4 0.134(18) 0.065(13) 0.029(11) 0.000 0.000 -0.010(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.440(4) 12_565 ? Gd1 O1 2.440(4) 3_565 ? Gd1 O1 2.440(4) 11 ? Gd1 O1 2.440(4) 2_665 ? Gd1 O1 2.440(4) 10_665 ? Gd1 O1 2.440(4) . ? Gd1 N1 2.502(6) 2_665 ? Gd1 N1 2.502(6) 3_565 ? Gd1 N1 2.502(6) . ? Fe1 O2 2.096(4) 13_665 ? Fe1 O2 2.096(4) . ? Fe1 O2 2.096(4) 16 ? Fe1 O2 2.096(4) 4_665 ? Fe1 O3 2.192(6) 13_665 ? Fe1 O3 2.192(6) . ? O1 C4 1.270(8) . ? O2 C4 1.248(7) . ? N1 C3 1.339(7) 12_565 ? N1 C3 1.339(7) . ? C1 C2 1.362(9) . ? C1 C2 1.362(9) 12_565 ? C1 H1 0.9300 . ? C2 C3 1.385(8) . ? C2 H2 0.9300 . ? C3 C4 1.509(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Gd1 O1 146.23(19) 12_565 3_565 ? O1 Gd1 O1 78.70(16) 12_565 11 ? O1 Gd1 O1 86.7(2) 3_565 11 ? O1 Gd1 O1 86.7(2) 12_565 2_665 ? O1 Gd1 O1 78.70(16) 3_565 2_665 ? O1 Gd1 O1 128.20(19) 11 2_665 ? O1 Gd1 O1 78.70(16) 12_565 10_665 ? O1 Gd1 O1 128.20(19) 3_565 10_665 ? O1 Gd1 O1 78.70(16) 11 10_665 ? O1 Gd1 O1 146.23(19) 2_665 10_665 ? O1 Gd1 O1 128.20(19) 12_565 . ? O1 Gd1 O1 78.70(16) 3_565 . ? O1 Gd1 O1 146.23(19) 11 . ? O1 Gd1 O1 78.70(16) 2_665 . ? O1 Gd1 O1 86.7(2) 10_665 . ? O1 Gd1 N1 73.11(9) 12_565 2_665 ? O1 Gd1 N1 73.11(9) 3_565 2_665 ? O1 Gd1 N1 64.10(9) 11 2_665 ? O1 Gd1 N1 64.10(9) 2_665 2_665 ? O1 Gd1 N1 136.66(10) 10_665 2_665 ? O1 Gd1 N1 136.66(10) . 2_665 ? O1 Gd1 N1 136.66(10) 12_565 3_565 ? O1 Gd1 N1 64.10(9) 3_565 3_565 ? O1 Gd1 N1 73.11(9) 11 3_565 ? O1 Gd1 N1 136.66(10) 2_665 3_565 ? O1 Gd1 N1 64.10(9) 10_665 3_565 ? O1 Gd1 N1 73.11(9) . 3_565 ? N1 Gd1 N1 120.0 2_665 3_565 ? O1 Gd1 N1 64.10(9) 12_565 . ? O1 Gd1 N1 136.66(10) 3_565 . ? O1 Gd1 N1 136.66(10) 11 . ? O1 Gd1 N1 73.11(9) 2_665 . ? O1 Gd1 N1 73.11(9) 10_665 . ? O1 Gd1 N1 64.10(9) . . ? N1 Gd1 N1 120.000(1) 2_665 . ? N1 Gd1 N1 120.0 3_565 . ? O2 Fe1 O2 180.0(3) 13_665 . ? O2 Fe1 O2 93.6(3) 13_665 16 ? O2 Fe1 O2 86.4(3) . 16 ? O2 Fe1 O2 86.4(3) 13_665 4_665 ? O2 Fe1 O2 93.6(3) . 4_665 ? O2 Fe1 O2 180.0 16 4_665 ? O2 Fe1 O3 89.00(17) 13_665 13_665 ? O2 Fe1 O3 91.00(17) . 13_665 ? O2 Fe1 O3 91.00(17) 16 13_665 ? O2 Fe1 O3 89.00(17) 4_665 13_665 ? O2 Fe1 O3 91.00(17) 13_665 . ? O2 Fe1 O3 89.00(17) . . ? O2 Fe1 O3 89.00(17) 16 . ? O2 Fe1 O3 91.00(17) 4_665 . ? O3 Fe1 O3 180.0 13_665 . ? C4 O1 Gd1 124.3(4) . . ? C4 O2 Fe1 132.0(4) . . ? C3 N1 C3 118.5(7) 12_565 . ? C3 N1 Gd1 120.7(4) 12_565 . ? C3 N1 Gd1 120.7(4) . . ? C2 C1 C2 120.3(9) . 12_565 ? C2 C1 H1 119.8 . . ? C2 C1 H1 119.8 12_565 . ? C1 C2 C3 118.6(7) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? N1 C3 C2 122.0(6) . . ? N1 C3 C4 114.1(5) . . ? C2 C3 C4 123.9(6) . . ? O2 C4 O1 127.2(6) . . ? O2 C4 C3 116.4(6) . . ? O1 C4 C3 116.3(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Gd1 O1 C4 5.6(5) 12_565 . . . ? O1 Gd1 O1 C4 162.8(5) 3_565 . . . ? O1 Gd1 O1 C4 -131.1(5) 11 . . . ? O1 Gd1 O1 C4 82.2(6) 2_665 . . . ? O1 Gd1 O1 C4 -67.2(5) 10_665 . . . ? N1 Gd1 O1 C4 112.8(5) 2_665 . . . ? N1 Gd1 O1 C4 -131.1(5) 3_565 . . . ? N1 Gd1 O1 C4 5.6(5) . . . . ? O2 Fe1 O2 C4 0(100) 13_665 . . . ? O2 Fe1 O2 C4 102.9(6) 16 . . . ? O2 Fe1 O2 C4 -77.1(6) 4_665 . . . ? O3 Fe1 O2 C4 11.9(6) 13_665 . . . ? O3 Fe1 O2 C4 -168.1(6) . . . . ? O1 Gd1 N1 C3 -2.2(4) 12_565 . . 12_565 ? O1 Gd1 N1 C3 144.1(4) 3_565 . . 12_565 ? O1 Gd1 N1 C3 -35.9(4) 11 . . 12_565 ? O1 Gd1 N1 C3 92.4(4) 2_665 . . 12_565 ? O1 Gd1 N1 C3 -87.6(4) 10_665 . . 12_565 ? O1 Gd1 N1 C3 177.8(4) . . . 12_565 ? N1 Gd1 N1 C3 47.0(3) 2_665 . . 12_565 ? N1 Gd1 N1 C3 -133.0(3) 3_565 . . 12_565 ? O1 Gd1 N1 C3 177.8(4) 12_565 . . . ? O1 Gd1 N1 C3 -35.9(4) 3_565 . . . ? O1 Gd1 N1 C3 144.1(4) 11 . . . ? O1 Gd1 N1 C3 -87.6(4) 2_665 . . . ? O1 Gd1 N1 C3 92.4(4) 10_665 . . . ? O1 Gd1 N1 C3 -2.2(4) . . . . ? N1 Gd1 N1 C3 -133.0(3) 2_665 . . . ? N1 Gd1 N1 C3 47.0(3) 3_565 . . . ? C2 C1 C2 C3 0.8(5) 12_565 . . . ? C3 N1 C3 C2 0.8(6) 12_565 . . . ? Gd1 N1 C3 C2 -179.2(6) . . . . ? C3 N1 C3 C4 179.5(7) 12_565 . . . ? Gd1 N1 C3 C4 -0.5(7) . . . . ? C1 C2 C3 N1 -1.6(11) . . . . ? C1 C2 C3 C4 179.8(6) . . . . ? Fe1 O2 C4 O1 2.8(11) . . . . ? Fe1 O2 C4 C3 -177.9(4) . . . . ? Gd1 O1 C4 O2 171.3(5) . . . . ? Gd1 O1 C4 C3 -8.0(8) . . . . ? N1 C3 C4 O2 -174.1(5) . . . . ? C2 C3 C4 O2 4.5(11) . . . . ? N1 C3 C4 O1 5.3(9) . . . . ? C2 C3 C4 O1 -176.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.311 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.120 # Attachment '3.cif' data_030109b _database_code_depnum_ccdc_archive 'CCDC 694300' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H18 Fe1.50 N3 O16.50 Tb' _chemical_formula_weight 819.08 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6/mcc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 15.199(2) _cell_length_b 15.199(2) _cell_length_c 15.589(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3118.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 881 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 26.33 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1604 _exptl_absorpt_coefficient_mu 3.012 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.7527 _exptl_absorpt_correction_T_max 0.8890 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 11486 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.03 _reflns_number_total 948 _reflns_number_gt 707 _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^)+(0.0349P)^2^+7.7317P] 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 948 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0673 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 Tb1 Tb 0.3333 0.6667 0.2500 0.01860(18) Uani 1 6 d S . . Fe1 Fe 0.5000 0.5000 0.0000 0.0186(3) Uani 1 4 d S . . O1 O 0.4136(2) 0.6125(2) 0.14348(19) 0.0287(7) Uani 1 1 d . . . O2 O 0.5521(3) 0.6152(3) 0.0920(2) 0.0378(9) Uani 1 1 d . . . O3 O 0.6505(3) 0.5127(4) 0.0000 0.0287(11) Uani 1 2 d S . . N1 N 0.5222(4) 0.76111(18) 0.2500 0.0221(10) Uani 1 2 d S . . C1 C 0.7306(5) 0.8653(3) 0.2500 0.053(2) Uani 1 2 d S . . H1 H 0.8013 0.9006 0.2500 0.064 Uiso 1 2 calc SR . . C2 C 0.6778(4) 0.7863(4) 0.1940(4) 0.0398(13) Uani 1 1 d . . . H2 H 0.7121 0.7676 0.1553 0.048 Uiso 1 1 calc R . . C3 C 0.5736(3) 0.7353(3) 0.1961(3) 0.0265(10) Uani 1 1 d . . . C4 C 0.5082(4) 0.6471(4) 0.1388(3) 0.0265(10) Uani 1 1 d . . . O4 O 0.7879(13) 0.7391(12) 0.0000 0.103(7) Uani 0.50 2 d SP . . 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 0.0204(2) 0.0204(2) 0.0149(2) 0.000 0.000 0.01021(10) Fe1 0.0247(7) 0.0205(7) 0.0152(5) 0.000 0.000 0.0148(5) O1 0.0255(18) 0.034(2) 0.0260(16) -0.0117(15) -0.0021(14) 0.0146(16) O2 0.0340(19) 0.045(2) 0.0387(19) -0.0199(18) -0.0006(17) 0.0225(18) O3 0.027(3) 0.034(3) 0.030(2) 0.000 0.000 0.019(2) N1 0.026(3) 0.0218(17) 0.020(2) -0.004(2) 0.000 0.0132(13) C1 0.021(3) 0.048(3) 0.081(6) -0.024(5) 0.000 0.0104(16) C2 0.027(3) 0.040(3) 0.051(3) -0.018(3) 0.003(3) 0.016(2) C3 0.026(2) 0.028(3) 0.028(2) -0.005(2) 0.004(2) 0.015(2) C4 0.035(3) 0.029(3) 0.019(2) -0.007(2) 0.000(2) 0.018(2) O4 0.104(12) 0.084(11) 0.043(7) 0.000 0.000 -0.011(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 Tb1 O1 2.434(3) 3_565 ? Tb1 O1 2.434(3) 12_565 ? Tb1 O1 2.434(3) 11 ? Tb1 O1 2.434(3) 2_665 ? Tb1 O1 2.434(3) . ? Tb1 O1 2.434(3) 10_665 ? Tb1 N1 2.486(5) 2_665 ? Tb1 N1 2.486(5) 3_565 ? Tb1 N1 2.486(5) . ? Fe1 O2 2.090(3) . ? Fe1 O2 2.090(3) 13_665 ? Fe1 O2 2.090(3) 16 ? Fe1 O2 2.090(3) 4_665 ? Fe1 O3 2.198(4) 13_665 ? Fe1 O3 2.198(4) . ? O1 C4 1.262(6) . ? O2 C4 1.239(5) . ? N1 C3 1.333(5) 12_565 ? N1 C3 1.333(5) . ? C1 C2 1.373(6) . ? C1 C2 1.373(6) 12_565 ? C1 H1 0.9300 . ? C2 C3 1.372(6) . ? C2 H2 0.9300 . ? C3 C4 1.500(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 O1 Tb1 O1 145.94(15) 3_565 12_565 ? O1 Tb1 O1 86.78(15) 3_565 11 ? O1 Tb1 O1 78.58(11) 12_565 11 ? O1 Tb1 O1 78.58(11) 3_565 2_665 ? O1 Tb1 O1 86.78(15) 12_565 2_665 ? O1 Tb1 O1 128.58(15) 11 2_665 ? O1 Tb1 O1 78.58(11) 3_565 . ? O1 Tb1 O1 128.58(15) 12_565 . ? O1 Tb1 O1 145.94(15) 11 . ? O1 Tb1 O1 78.58(11) 2_665 . ? O1 Tb1 O1 128.58(15) 3_565 10_665 ? O1 Tb1 O1 78.58(11) 12_565 10_665 ? O1 Tb1 O1 78.58(11) 11 10_665 ? O1 Tb1 O1 145.94(15) 2_665 10_665 ? O1 Tb1 O1 86.78(15) . 10_665 ? O1 Tb1 N1 72.97(7) 3_565 2_665 ? O1 Tb1 N1 72.97(7) 12_565 2_665 ? O1 Tb1 N1 64.29(7) 11 2_665 ? O1 Tb1 N1 64.29(7) 2_665 2_665 ? O1 Tb1 N1 136.61(7) . 2_665 ? O1 Tb1 N1 136.61(7) 10_665 2_665 ? O1 Tb1 N1 64.29(7) 3_565 3_565 ? O1 Tb1 N1 136.61(7) 12_565 3_565 ? O1 Tb1 N1 72.97(7) 11 3_565 ? O1 Tb1 N1 136.61(7) 2_665 3_565 ? O1 Tb1 N1 72.97(7) . 3_565 ? O1 Tb1 N1 64.29(7) 10_665 3_565 ? N1 Tb1 N1 120.0 2_665 3_565 ? O1 Tb1 N1 136.61(7) 3_565 . ? O1 Tb1 N1 64.29(7) 12_565 . ? O1 Tb1 N1 136.61(7) 11 . ? O1 Tb1 N1 72.97(7) 2_665 . ? O1 Tb1 N1 64.29(7) . . ? O1 Tb1 N1 72.97(7) 10_665 . ? N1 Tb1 N1 120.0 2_665 . ? N1 Tb1 N1 120.0 3_565 . ? O2 Fe1 O2 180.0 . 13_665 ? O2 Fe1 O2 86.7(2) . 16 ? O2 Fe1 O2 93.3(2) 13_665 16 ? O2 Fe1 O2 93.3(2) . 4_665 ? O2 Fe1 O2 86.7(2) 13_665 4_665 ? O2 Fe1 O2 180.0 16 4_665 ? O2 Fe1 O3 90.88(13) . 13_665 ? O2 Fe1 O3 89.12(13) 13_665 13_665 ? O2 Fe1 O3 90.88(13) 16 13_665 ? O2 Fe1 O3 89.12(13) 4_665 13_665 ? O2 Fe1 O3 89.12(13) . . ? O2 Fe1 O3 90.88(13) 13_665 . ? O2 Fe1 O3 89.12(13) 16 . ? O2 Fe1 O3 90.88(13) 4_665 . ? O3 Fe1 O3 180.0 13_665 . ? C4 O1 Tb1 123.9(3) . . ? C4 O2 Fe1 132.8(3) . . ? C3 N1 C3 119.0(5) 12_565 . ? C3 N1 Tb1 120.5(3) 12_565 . ? C3 N1 Tb1 120.5(3) . . ? C2 C1 C2 119.2(7) . 12_565 ? C2 C1 H1 120.4 . . ? C2 C1 H1 120.4 12_565 . ? C3 C2 C1 119.0(5) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? N1 C3 C2 121.9(4) . . ? N1 C3 C4 114.5(4) . . ? C2 C3 C4 123.6(4) . . ? O2 C4 O1 126.5(4) . . ? O2 C4 C3 117.0(4) . . ? O1 C4 C3 116.5(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Tb1 O1 C4 162.3(4) 3_565 . . . ? O1 Tb1 O1 C4 5.4(3) 12_565 . . . ? O1 Tb1 O1 C4 -131.3(4) 11 . . . ? O1 Tb1 O1 C4 81.8(4) 2_665 . . . ? O1 Tb1 O1 C4 -67.2(3) 10_665 . . . ? N1 Tb1 O1 C4 112.8(3) 2_665 . . . ? N1 Tb1 O1 C4 -131.3(4) 3_565 . . . ? N1 Tb1 O1 C4 5.4(3) . . . . ? O2 Fe1 O2 C4 15(100) 13_665 . . . ? O2 Fe1 O2 C4 103.2(5) 16 . . . ? O2 Fe1 O2 C4 -76.8(5) 4_665 . . . ? O3 Fe1 O2 C4 12.4(5) 13_665 . . . ? O3 Fe1 O2 C4 -167.6(5) . . . . ? O1 Tb1 N1 C3 143.8(3) 3_565 . . 12_565 ? O1 Tb1 N1 C3 -2.2(2) 12_565 . . 12_565 ? O1 Tb1 N1 C3 -36.2(3) 11 . . 12_565 ? O1 Tb1 N1 C3 92.5(3) 2_665 . . 12_565 ? O1 Tb1 N1 C3 177.8(2) . . . 12_565 ? O1 Tb1 N1 C3 -87.5(3) 10_665 . . 12_565 ? N1 Tb1 N1 C3 47.0(2) 2_665 . . 12_565 ? N1 Tb1 N1 C3 -133.0(2) 3_565 . . 12_565 ? O1 Tb1 N1 C3 -36.2(3) 3_565 . . . ? O1 Tb1 N1 C3 177.8(2) 12_565 . . . ? O1 Tb1 N1 C3 143.8(3) 11 . . . ? O1 Tb1 N1 C3 -87.5(3) 2_665 . . . ? O1 Tb1 N1 C3 -2.2(2) . . . . ? O1 Tb1 N1 C3 92.5(3) 10_665 . . . ? N1 Tb1 N1 C3 -133.0(2) 2_665 . . . ? N1 Tb1 N1 C3 47.0(2) 3_565 . . . ? C2 C1 C2 C3 -0.4(4) 12_565 . . . ? C3 N1 C3 C2 -0.5(4) 12_565 . . . ? Tb1 N1 C3 C2 179.5(4) . . . . ? C3 N1 C3 C4 179.6(5) 12_565 . . . ? Tb1 N1 C3 C4 -0.4(5) . . . . ? C1 C2 C3 N1 0.9(8) . . . . ? C1 C2 C3 C4 -179.2(4) . . . . ? Fe1 O2 C4 O1 2.1(8) . . . . ? Fe1 O2 C4 C3 -178.2(3) . . . . ? Tb1 O1 C4 O2 172.0(4) . . . . ? Tb1 O1 C4 C3 -7.6(6) . . . . ? N1 C3 C4 O2 -174.7(4) . . . . ? C2 C3 C4 O2 5.4(8) . . . . ? N1 C3 C4 O1 5.0(6) . . . . ? C2 C3 C4 O1 -174.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.054 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.093