# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm #TrackingRef 'compounds.txt' _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Sheng-Run, Zheng; Wei-guang, Zhang' _publ_contact_author_email 'zhengshngrun@gmail.com; wgzhang@scnu.edu.cn' _publ_section_title ; Construction of Luminescent Three-Dimensional Ln(III)-Zn(II) Heterometallic Coordination Polymers based on 2-Pyridyl Imidazole Dicarboxylate ; loop_ _publ_author_name 'Song-Liang, Cai' 'Shengrun Zheng' 'Jun Fan' 'Wei-Guang Zhang' data_1-Sm-Zn _database_code_depnum_ccdc_archive 'CCDC 879665' #TrackingRef 'compounds.txt' _database_code_CSD 879665 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H28 Cl3 N12 O22 Sm Zn6' _chemical_formula_weight 1677.66 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Fddd ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 12.313(2) _cell_length_b 22.626(5) _cell_length_c 34.702(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9668(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3435 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.04 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6568 _exptl_absorpt_coefficient_mu 4.387 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3528 _exptl_absorpt_correction_T_max 0.4453 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12489 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2378 _reflns_number_gt 1856 _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^)+(0.1809P)^2^+50.5254P] 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 2378 _refine_ls_number_parameters 199 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.2352 _refine_ls_wR_factor_gt 0.2122 _refine_ls_goodness_of_fit_ref 1.051 _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 Sm1 Sm -0.1250 0.3750 0.3750 0.0215(3) Uani 1 4 d S . . Zn1 Zn 0.24093(10) 0.32491(5) 0.24846(3) 0.0335(4) Uani 1 1 d . . . Zn2 Zn 0.3750 0.3750 0.10846(6) 0.0588(6) Uani 1 2 d S . . C1 C 0.0817(8) 0.3515(4) 0.3058(3) 0.033(2) Uani 1 1 d . . . C2 C 0.0751(7) 0.4027(4) 0.2793(2) 0.0263(18) Uani 1 1 d . . . C3 C 0.0278(7) 0.4573(4) 0.2812(2) 0.0244(18) Uani 1 1 d . . . C4 C -0.0395(8) 0.4871(4) 0.3103(3) 0.035(2) Uani 1 1 d . . . C5 C 0.1262(7) 0.4529(4) 0.2289(3) 0.029(2) Uani 1 1 d . . . C6 C 0.1798(8) 0.4688(4) 0.1934(3) 0.035(2) Uani 1 1 d . . . C7 C 0.1925(10) 0.5266(5) 0.1821(3) 0.049(3) Uani 1 1 d . . . H7 H 0.1622 0.5568 0.1968 0.059 Uiso 1 1 calc R . . C8 C 0.2515(11) 0.5406(5) 0.1482(3) 0.051(3) Uani 1 1 d . . . H8 H 0.2594 0.5793 0.1396 0.061 Uiso 1 1 calc R . . C9 C 0.2956(11) 0.4942(6) 0.1292(4) 0.059(3) Uani 1 1 d . . . H9 H 0.3353 0.5029 0.1071 0.070 Uiso 1 1 calc R . . C10 C 0.2286(10) 0.4256(4) 0.1709(3) 0.047(3) Uani 1 1 d . . . H10 H 0.2208 0.3862 0.1779 0.057 Uiso 1 1 calc R . . N1 N 0.1383(6) 0.4004(3) 0.2462(2) 0.0289(17) Uani 1 1 d . . . N2 N 0.0594(6) 0.4897(3) 0.2493(2) 0.0304(17) Uani 1 1 d . . . N3 N 0.2881(8) 0.4393(4) 0.1386(3) 0.048(2) Uani 1 1 d . . . Cl1 Cl 0.3750 0.3750 0.2428(4) 0.145(4) Uani 1 2 d S . . Cl2 Cl 0.2874(17) 0.2880(12) 0.0174(8) 0.133(9) Uani 0.25 1 d P . . O1 O 0.1548(6) 0.3128(3) 0.2978(2) 0.0434(19) Uani 1 1 d . . . O1W O 0.3750 0.3750 0.0464(3) 0.054(3) Uani 1 2 d S . . H1WB H 0.4352 0.3689 0.0352 0.098 Uiso 0.50 1 d PR . . H1WA H 0.3435 0.3419 0.0439 0.098 Uiso 0.50 1 d PR . . O2 O 0.0197(6) 0.3461(3) 0.3344(2) 0.0416(18) Uani 1 1 d . . . O2W O 0.2353(6) 0.3159(4) 0.1065(3) 0.083(3) Uani 1 1 d D . . H2WA H 0.1954 0.3077 0.0865 0.099 Uiso 1 1 d RD . . H2WB H 0.2143 0.2870 0.1232 0.099 Uiso 1 1 d RD . . O3 O -0.0627(6) 0.4633(3) 0.3416(2) 0.0414(17) Uani 1 1 d . . . O4 O -0.0660(6) 0.5409(3) 0.3025(2) 0.0437(18) 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 Sm1 0.0227(5) 0.0190(5) 0.0228(5) 0.000 0.000 0.000 Zn1 0.0433(8) 0.0244(7) 0.0328(7) -0.0016(4) 0.0035(5) 0.0085(5) Zn2 0.0647(14) 0.0652(14) 0.0464(12) 0.000 0.000 0.0148(10) C1 0.037(5) 0.022(5) 0.039(5) 0.000(4) 0.002(4) 0.006(4) C2 0.026(4) 0.025(4) 0.027(5) 0.000(4) 0.003(4) 0.006(3) C3 0.026(4) 0.025(4) 0.023(4) 0.005(3) 0.005(3) 0.006(3) C4 0.043(5) 0.026(5) 0.035(5) 0.003(4) 0.006(4) 0.010(4) C5 0.038(5) 0.026(4) 0.024(4) 0.008(4) 0.003(4) 0.005(4) C6 0.040(5) 0.028(5) 0.036(5) 0.003(4) 0.004(4) 0.008(4) C7 0.061(7) 0.032(5) 0.055(7) 0.009(5) 0.006(6) 0.002(5) C8 0.070(8) 0.039(6) 0.043(6) 0.007(5) 0.019(6) -0.007(5) C9 0.060(8) 0.060(8) 0.055(8) 0.021(6) 0.023(6) 0.006(6) C10 0.071(8) 0.033(5) 0.038(6) 0.010(5) 0.014(5) 0.002(5) N1 0.032(4) 0.019(4) 0.036(4) 0.001(3) 0.003(3) 0.007(3) N2 0.034(4) 0.025(4) 0.032(4) 0.006(3) 0.006(3) 0.009(3) N3 0.064(6) 0.037(5) 0.043(5) 0.006(4) 0.017(5) 0.011(4) Cl1 0.090(6) 0.121(7) 0.224(12) 0.000 0.000 -0.029(5) Cl2 0.078(13) 0.16(2) 0.16(2) 0.068(18) 0.030(14) 0.024(13) O1 0.051(4) 0.029(4) 0.049(4) 0.014(3) 0.018(4) 0.025(3) O1W 0.048(7) 0.087(9) 0.028(5) 0.000 0.000 0.020(6) O2 0.047(4) 0.034(4) 0.044(4) 0.011(3) 0.021(3) 0.017(3) O2W 0.067(6) 0.083(7) 0.098(8) 0.018(6) -0.040(6) -0.013(5) O3 0.055(4) 0.028(3) 0.041(4) 0.010(3) 0.019(3) 0.011(3) O4 0.064(5) 0.021(3) 0.045(4) 0.010(3) 0.020(4) 0.021(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 Sm1 O2 2.362(6) . ? Sm1 O2 2.362(6) 2_455 ? Sm1 O2 2.362(6) 4 ? Sm1 O2 2.362(6) 3_455 ? Sm1 O3 2.433(6) 2_455 ? Sm1 O3 2.433(6) . ? Sm1 O3 2.433(6) 4 ? Sm1 O3 2.433(6) 3_455 ? Zn1 Cl1 2.0120(18) . ? Zn1 O1 2.034(7) . ? Zn1 O4 2.052(7) 22_655 ? Zn1 N2 2.106(7) 22_655 ? Zn1 N1 2.126(7) . ? Zn2 N3 2.086(9) . ? Zn2 N3 2.086(9) 2 ? Zn2 O1W 2.153(11) . ? Zn2 O2W 2.180(8) 2 ? Zn2 O2W 2.180(8) . ? C1 O2 1.259(11) . ? C1 O1 1.286(11) . ? C1 C2 1.481(13) . ? C2 C3 1.368(12) . ? C2 N1 1.388(11) . ? C3 N2 1.383(11) . ? C3 C4 1.473(12) . ? C4 O3 1.244(11) . ? C4 O4 1.289(11) . ? C5 N1 1.339(12) . ? C5 N2 1.367(12) . ? C5 C6 1.444(13) . ? C6 C7 1.375(13) . ? C6 C10 1.386(14) . ? C7 C8 1.417(15) . ? C7 H7 0.9300 . ? C8 C9 1.354(17) . ? C8 H8 0.9300 . ? C9 N3 1.289(15) . ? C9 H9 0.9300 . ? C10 N3 1.374(14) . ? C10 H10 0.9300 . ? N2 Zn1 2.106(7) 26_565 ? Cl1 Zn1 2.0120(18) 2 ? Cl2 Cl2 2.30(6) 29 ? Cl2 H1WA 1.6736 . ? O1W H1WB 0.8495 . ? O1W H1WA 0.8492 . ? O2W H2WA 0.8705 . ? O2W H2WB 0.9112 . ? O4 Zn1 2.052(7) 26_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Sm1 O2 106.9(4) . 2_455 ? O2 Sm1 O2 82.1(4) . 4 ? O2 Sm1 O2 147.9(3) 2_455 4 ? O2 Sm1 O2 147.9(3) . 3_455 ? O2 Sm1 O2 82.1(4) 2_455 3_455 ? O2 Sm1 O2 106.9(4) 4 3_455 ? O2 Sm1 O3 74.1(3) . 2_455 ? O2 Sm1 O3 72.9(2) 2_455 2_455 ? O2 Sm1 O3 138.5(2) 4 2_455 ? O2 Sm1 O3 79.6(2) 3_455 2_455 ? O2 Sm1 O3 72.9(2) . . ? O2 Sm1 O3 74.1(3) 2_455 . ? O2 Sm1 O3 79.6(2) 4 . ? O2 Sm1 O3 138.5(2) 3_455 . ? O3 Sm1 O3 123.1(3) 2_455 . ? O2 Sm1 O3 79.6(2) . 4 ? O2 Sm1 O3 138.5(2) 2_455 4 ? O2 Sm1 O3 72.9(2) 4 4 ? O2 Sm1 O3 74.1(3) 3_455 4 ? O3 Sm1 O3 69.7(3) 2_455 4 ? O3 Sm1 O3 143.3(3) . 4 ? O2 Sm1 O3 138.5(2) . 3_455 ? O2 Sm1 O3 79.6(2) 2_455 3_455 ? O2 Sm1 O3 74.1(3) 4 3_455 ? O2 Sm1 O3 72.9(2) 3_455 3_455 ? O3 Sm1 O3 143.3(3) 2_455 3_455 ? O3 Sm1 O3 69.7(3) . 3_455 ? O3 Sm1 O3 123.1(3) 4 3_455 ? Cl1 Zn1 O1 125.9(4) . . ? Cl1 Zn1 O4 114.0(4) . 22_655 ? O1 Zn1 O4 119.8(3) . 22_655 ? Cl1 Zn1 N2 101.0(2) . 22_655 ? O1 Zn1 N2 93.1(3) . 22_655 ? O4 Zn1 N2 80.0(3) 22_655 22_655 ? Cl1 Zn1 N1 91.8(2) . . ? O1 Zn1 N1 80.2(3) . . ? O4 Zn1 N1 93.8(3) 22_655 . ? N2 Zn1 N1 167.1(3) 22_655 . ? N3 Zn2 N3 119.8(5) . 2 ? N3 Zn2 O1W 120.1(3) . . ? N3 Zn2 O1W 120.1(3) 2 . ? N3 Zn2 O2W 89.6(4) . 2 ? N3 Zn2 O2W 92.2(4) 2 2 ? O1W Zn2 O2W 88.2(3) . 2 ? N3 Zn2 O2W 92.2(4) . . ? N3 Zn2 O2W 89.6(4) 2 . ? O1W Zn2 O2W 88.2(3) . . ? O2W Zn2 O2W 176.5(6) 2 . ? O2 C1 O1 121.9(9) . . ? O2 C1 C2 122.2(8) . . ? O1 C1 C2 115.9(8) . . ? C3 C2 N1 108.2(8) . . ? C3 C2 C1 134.4(8) . . ? N1 C2 C1 117.0(8) . . ? C2 C3 N2 108.7(7) . . ? C2 C3 C4 133.4(8) . . ? N2 C3 C4 117.7(8) . . ? O3 C4 O4 122.4(9) . . ? O3 C4 C3 121.9(8) . . ? O4 C4 C3 115.5(8) . . ? N1 C5 N2 112.0(8) . . ? N1 C5 C6 123.6(8) . . ? N2 C5 C6 124.4(8) . . ? C7 C6 C10 117.5(10) . . ? C7 C6 C5 122.1(9) . . ? C10 C6 C5 120.2(9) . . ? C6 C7 C8 120.4(10) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 116.0(10) . . ? C9 C8 H8 122.0 . . ? C7 C8 H8 122.0 . . ? N3 C9 C8 126.5(11) . . ? N3 C9 H9 116.8 . . ? C8 C9 H9 116.8 . . ? N3 C10 C6 122.2(9) . . ? N3 C10 H10 118.9 . . ? C6 C10 H10 118.9 . . ? C5 N1 C2 106.0(7) . . ? C5 N1 Zn1 142.6(6) . . ? C2 N1 Zn1 109.4(6) . . ? C5 N2 C3 105.1(7) . . ? C5 N2 Zn1 144.8(6) . 26_565 ? C3 N2 Zn1 110.1(6) . 26_565 ? C9 N3 C10 117.5(10) . . ? C9 N3 Zn2 120.6(8) . . ? C10 N3 Zn2 121.7(7) . . ? Zn1 Cl1 Zn1 168.8(7) . 2 ? Cl2 Cl2 H1WA 178.1 29 . ? C1 O1 Zn1 117.0(6) . . ? Zn2 O1W H1WB 117.4 . . ? Zn2 O1W H1WA 96.0 . . ? H1WB O1W H1WA 102.0 . . ? C1 O2 Sm1 154.2(6) . . ? Zn2 O2W H2WA 127.0 . . ? Zn2 O2W H2WB 130.2 . . ? H2WA O2W H2WB 101.1 . . ? C4 O3 Sm1 147.6(7) . . ? C4 O4 Zn1 116.7(6) . 26_565 ? 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 O2 C1 C2 C3 15.8(17) . . . . ? O1 C1 C2 C3 -164.1(10) . . . . ? O2 C1 C2 N1 -172.3(9) . . . . ? O1 C1 C2 N1 7.7(13) . . . . ? N1 C2 C3 N2 0.6(10) . . . . ? C1 C2 C3 N2 173.0(10) . . . . ? N1 C2 C3 C4 -174.4(10) . . . . ? C1 C2 C3 C4 -2.1(19) . . . . ? C2 C3 C4 O3 1.8(18) . . . . ? N2 C3 C4 O3 -173.0(9) . . . . ? C2 C3 C4 O4 177.1(10) . . . . ? N2 C3 C4 O4 2.4(13) . . . . ? N1 C5 C6 C7 -160.5(10) . . . . ? N2 C5 C6 C7 18.0(16) . . . . ? N1 C5 C6 C10 14.0(16) . . . . ? N2 C5 C6 C10 -167.5(10) . . . . ? C10 C6 C7 C8 1.4(17) . . . . ? C5 C6 C7 C8 176.1(10) . . . . ? C6 C7 C8 C9 -1.9(18) . . . . ? C7 C8 C9 N3 1(2) . . . . ? C7 C6 C10 N3 0.3(17) . . . . ? C5 C6 C10 N3 -174.5(10) . . . . ? N2 C5 N1 C2 0.8(11) . . . . ? C6 C5 N1 C2 179.4(9) . . . . ? N2 C5 N1 Zn1 -160.3(8) . . . . ? C6 C5 N1 Zn1 18.4(17) . . . . ? C3 C2 N1 C5 -0.8(10) . . . . ? C1 C2 N1 C5 -174.7(8) . . . . ? C3 C2 N1 Zn1 167.1(6) . . . . ? C1 C2 N1 Zn1 -6.8(10) . . . . ? Cl1 Zn1 N1 C5 38.0(12) . . . . ? O1 Zn1 N1 C5 164.2(12) . . . . ? O4 Zn1 N1 C5 -76.2(11) 22_655 . . . ? N2 Zn1 N1 C5 -136.7(14) 22_655 . . . ? Cl1 Zn1 N1 C2 -122.7(7) . . . . ? O1 Zn1 N1 C2 3.5(6) . . . . ? O4 Zn1 N1 C2 123.1(6) 22_655 . . . ? N2 Zn1 N1 C2 62.6(16) 22_655 . . . ? N1 C5 N2 C3 -0.4(11) . . . . ? C6 C5 N2 C3 -179.0(9) . . . . ? N1 C5 N2 Zn1 177.4(8) . . . 26_565 ? C6 C5 N2 Zn1 -1.3(18) . . . 26_565 ? C2 C3 N2 C5 -0.2(10) . . . . ? C4 C3 N2 C5 175.8(8) . . . . ? C2 C3 N2 Zn1 -178.8(6) . . . 26_565 ? C4 C3 N2 Zn1 -2.8(10) . . . 26_565 ? C8 C9 N3 C10 1(2) . . . . ? C8 C9 N3 Zn2 -173.9(11) . . . . ? C6 C10 N3 C9 -1.4(19) . . . . ? C6 C10 N3 Zn2 173.2(9) . . . . ? N3 Zn2 N3 C9 133.0(12) 2 . . . ? O1W Zn2 N3 C9 -47.0(12) . . . . ? O2W Zn2 N3 C9 40.7(11) 2 . . . ? O2W Zn2 N3 C9 -136.2(11) . . . . ? N3 Zn2 N3 C10 -41.4(8) 2 . . . ? O1W Zn2 N3 C10 138.6(8) . . . . ? O2W Zn2 N3 C10 -133.7(10) 2 . . . ? O2W Zn2 N3 C10 49.4(10) . . . . ? O1 Zn1 Cl1 Zn1 13.1(2) . . . 2 ? O4 Zn1 Cl1 Zn1 -172.73(19) 22_655 . . 2 ? N2 Zn1 Cl1 Zn1 -88.9(2) 22_655 . . 2 ? N1 Zn1 Cl1 Zn1 92.3(2) . . . 2 ? O2 C1 O1 Zn1 175.7(8) . . . . ? C2 C1 O1 Zn1 -4.3(12) . . . . ? Cl1 Zn1 O1 C1 85.6(8) . . . . ? O4 Zn1 O1 C1 -88.2(8) 22_655 . . . ? N2 Zn1 O1 C1 -168.4(8) 22_655 . . . ? N1 Zn1 O1 C1 0.5(8) . . . . ? O1 C1 O2 Sm1 -177.2(11) . . . . ? C2 C1 O2 Sm1 3(2) . . . . ? O2 Sm1 O2 C1 43.6(16) 2_455 . . . ? O2 Sm1 O2 C1 -104.8(17) 4 . . . ? O2 Sm1 O2 C1 145.9(17) 3_455 . . . ? O3 Sm1 O2 C1 109.6(17) 2_455 . . . ? O3 Sm1 O2 C1 -23.3(16) . . . . ? O3 Sm1 O2 C1 -178.7(17) 4 . . . ? O3 Sm1 O2 C1 -49.7(18) 3_455 . . . ? O4 C4 O3 Sm1 139.3(9) . . . . ? C3 C4 O3 Sm1 -45.7(18) . . . . ? O2 Sm1 O3 C4 50.9(12) . . . . ? O2 Sm1 O3 C4 -62.9(12) 2_455 . . . ? O2 Sm1 O3 C4 135.7(13) 4 . . . ? O2 Sm1 O3 C4 -120.5(12) 3_455 . . . ? O3 Sm1 O3 C4 -6.3(12) 2_455 . . . ? O3 Sm1 O3 C4 94.0(12) 4 . . . ? O3 Sm1 O3 C4 -147.5(14) 3_455 . . . ? O3 C4 O4 Zn1 174.8(8) . . . 26_565 ? C3 C4 O4 Zn1 -0.5(12) . . . 26_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.900 _refine_diff_density_min -2.489 _refine_diff_density_rms 0.221 ######################################################################## data_2-Eu-Zn _database_code_depnum_ccdc_archive 'CCDC 879666' #TrackingRef 'compounds.txt' _database_code_CSD 879666 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H28 Cl3 Eu N12 O22 Zn6' _chemical_formula_weight 1679.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Fddd ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 12.284(2) _cell_length_b 22.733(4) _cell_length_c 34.400(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9606(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2361 _cell_measurement_theta_min 2.5618 _cell_measurement_theta_max 62.2511 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6576 _exptl_absorpt_coefficient_mu 14.894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1381 _exptl_absorpt_correction_T_max 0.1746 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4480 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 4.29 _diffrn_reflns_theta_max 62.35 _reflns_number_total 1885 _reflns_number_gt 1831 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _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. ISOR and SIMU were applied to O1W. ; _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^)+(0.1449P)^2^+17.0387P] 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 1885 _refine_ls_number_parameters 199 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1629 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.065 _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 0.8750 0.3750 -0.1250 0.0113(3) Uani 1 4 d S . . Zn1 Zn 0.99285(7) 0.17489(4) -0.00190(2) 0.0191(3) Uani 1 1 d . . . Zn2 Zn 1.3750 0.3750 0.14347(5) 0.0377(5) Uani 1 2 d S . . N2 N 1.0626(5) 0.2602(2) 0.00080(15) 0.0171(12) Uani 1 1 d . . . N1 N 1.1388(5) 0.3499(3) 0.00454(17) 0.0176(13) Uani 1 1 d . . . O4 O 0.9370(4) 0.2088(2) -0.05313(14) 0.0239(11) Uani 1 1 d . . . O3 O 0.9380(4) 0.2866(2) -0.09169(13) 0.0250(11) Uani 1 1 d . . . C5 C 1.1270(5) 0.2974(3) 0.0210(2) 0.0204(16) Uani 1 1 d . . . O2 O 1.0187(4) 0.4039(2) -0.08361(14) 0.0262(11) Uani 1 1 d . . . O1 O 1.1526(4) 0.4376(2) -0.04677(15) 0.0265(11) Uani 1 1 d . . . C2 C 1.0769(5) 0.3475(3) -0.02909(18) 0.0176(14) Uani 1 1 d . . . C3 C 1.0302(5) 0.2925(3) -0.03092(18) 0.0146(12) Uani 1 1 d . . . C6 C 1.1835(6) 0.2812(3) 0.0574(2) 0.0221(15) Uani 1 1 d . . . N3 N 1.2927(5) 0.3112(3) 0.11208(18) 0.0257(13) Uani 1 1 d . . . C1 C 1.0798(6) 0.3988(3) -0.05538(19) 0.0198(14) Uani 1 1 d . . . C8 C 1.2545(7) 0.2101(4) 0.1021(2) 0.0360(19) Uani 1 1 d . . . H8A H 1.2630 0.1714 0.1104 0.043 Uiso 1 1 calc R . . C7 C 1.1949(7) 0.2228(3) 0.0691(2) 0.0332(18) Uani 1 1 d . . . H7A H 1.1628 0.1927 0.0549 0.040 Uiso 1 1 calc R . . C9 C 1.3009(8) 0.2555(4) 0.1226(2) 0.034(2) Uani 1 1 d . . . H9A H 1.3401 0.2466 0.1450 0.041 Uiso 1 1 calc R . . C4 C 0.9625(5) 0.2623(3) -0.0608(2) 0.0188(14) Uani 1 1 d . . . O1W O 1.3750 0.3750 0.2055(2) 0.0277(18) Uani 1 2 d SU . . H1WA H 1.3824 0.3434 0.2186 0.042 Uiso 0.50 1 d PR . . H1WB H 1.3706 0.4034 0.2216 0.042 Uiso 0.50 1 d PR . . Cl1 Cl 1.1250 0.1250 -0.0042(3) 0.133(3) Uani 1 2 d S . . C10 C 1.2333(6) 0.3242(3) 0.0803(2) 0.0262(16) Uani 1 1 d . . . H10A H 1.2251 0.3634 0.0733 0.031 Uiso 1 1 calc R . . O2W O 1.2337(6) 0.4337(3) 0.1446(2) 0.0558(18) Uani 1 1 d . . . H2WB H 1.2214 0.4626 0.1267 0.084 Uiso 1 1 d R . . H2WA H 1.1957 0.4450 0.1642 0.084 Uiso 1 1 d R . . Cl2 Cl 1.2895(10) 0.4657(5) 0.2362(5) 0.080(4) Uani 0.25 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 Eu1 0.0166(5) 0.0087(5) 0.0087(5) 0.000 0.000 0.000 Zn1 0.0268(6) 0.0128(6) 0.0176(6) 0.0009(3) 0.0012(3) -0.0038(3) Zn2 0.0429(10) 0.0478(11) 0.0225(9) 0.000 0.000 -0.0158(6) N2 0.020(3) 0.012(2) 0.020(3) 0.004(2) -0.001(2) -0.006(2) N1 0.028(3) 0.011(3) 0.013(3) 0.001(2) -0.004(2) -0.005(2) O4 0.037(3) 0.013(2) 0.022(2) 0.0022(19) -0.009(2) -0.012(2) O3 0.041(3) 0.014(2) 0.020(2) 0.0082(19) -0.014(2) -0.003(2) C5 0.025(4) 0.015(4) 0.021(4) 0.006(3) -0.004(2) 0.000(2) O2 0.033(3) 0.022(3) 0.024(2) 0.008(2) -0.016(2) -0.012(2) O1 0.037(3) 0.019(3) 0.024(3) 0.008(2) -0.013(2) -0.016(2) C2 0.021(3) 0.020(3) 0.012(3) -0.001(3) -0.006(3) 0.001(3) C3 0.016(3) 0.014(3) 0.014(3) 0.003(2) -0.003(2) -0.005(2) C6 0.027(4) 0.021(3) 0.018(3) 0.007(3) -0.003(3) -0.004(3) N3 0.030(3) 0.025(3) 0.022(3) 0.004(3) -0.004(3) -0.004(3) C1 0.026(4) 0.014(4) 0.019(3) 0.003(3) -0.003(3) -0.007(3) C8 0.049(5) 0.029(4) 0.030(4) 0.015(4) -0.013(4) 0.002(4) C7 0.044(4) 0.023(4) 0.033(4) 0.007(3) -0.012(4) -0.005(3) C9 0.041(5) 0.040(5) 0.023(4) 0.009(3) -0.015(3) 0.002(4) C4 0.020(3) 0.010(3) 0.027(4) -0.003(3) 0.001(3) -0.004(3) O1W 0.028(2) 0.029(2) 0.026(2) 0.000 0.000 -0.0038(10) Cl1 0.104(5) 0.142(8) 0.153(7) 0.000 0.000 0.036(4) C10 0.045(4) 0.021(4) 0.012(3) 0.006(3) -0.011(3) -0.005(3) O2W 0.058(4) 0.053(4) 0.056(4) -0.002(3) 0.028(3) 0.004(3) Cl2 0.072(7) 0.056(7) 0.113(10) 0.022(7) -0.011(7) -0.012(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 Eu1 O2 2.361(4) 3_654 ? Eu1 O2 2.361(4) 4_554 ? Eu1 O2 2.361(4) . ? Eu1 O2 2.361(4) 2_655 ? Eu1 O3 2.440(4) 3_654 ? Eu1 O3 2.440(4) 2_655 ? Eu1 O3 2.440(4) . ? Eu1 O3 2.440(4) 4_554 ? Zn1 Cl1 1.9818(10) . ? Zn1 O1 2.029(5) 30 ? Zn1 O4 2.042(5) . ? Zn1 N2 2.122(6) . ? Zn1 N1 2.133(6) 30 ? Zn2 N3 2.072(6) . ? Zn2 N3 2.072(6) 2_755 ? Zn2 O1W 2.133(9) . ? Zn2 O2W 2.189(7) 2_755 ? Zn2 O2W 2.189(7) . ? N2 C5 1.350(10) . ? N2 C3 1.375(8) . ? N1 C5 1.329(10) . ? N1 C2 1.386(8) . ? N1 Zn1 2.133(6) 18_665 ? O4 C4 1.283(8) . ? O3 C4 1.235(9) . ? C5 C6 1.479(10) . ? O2 C1 1.233(8) . ? O1 C1 1.290(9) . ? O1 Zn1 2.029(5) 18_665 ? C2 C3 1.376(9) . ? C2 C1 1.476(9) . ? C3 C4 1.489(9) . ? C6 C10 1.396(10) . ? C6 C7 1.393(10) . ? N3 C10 1.347(10) . ? N3 C9 1.321(11) . ? C8 C7 1.381(11) . ? C8 C9 1.374(13) . ? C8 H8A 0.9300 . ? C7 H7A 0.9300 . ? C9 H9A 0.9300 . ? O1W H1WA 0.8527 . ? O1W H1WB 0.8528 . ? Cl1 Zn1 1.9818(10) 14_645 ? C10 H10A 0.9300 . ? O2W H2WB 0.9143 . ? O2W H2WA 0.8586 . ? Cl2 Cl2 2.07(3) 25_765 ? Cl2 H1WB 1.8032 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Eu1 O2 105.8(2) 3_654 4_554 ? O2 Eu1 O2 147.7(2) 3_654 . ? O2 Eu1 O2 83.2(3) 4_554 . ? O2 Eu1 O2 83.2(3) 3_654 2_655 ? O2 Eu1 O2 147.7(2) 4_554 2_655 ? O2 Eu1 O2 105.8(2) . 2_655 ? O2 Eu1 O3 73.09(16) 3_654 3_654 ? O2 Eu1 O3 74.01(18) 4_554 3_654 ? O2 Eu1 O3 138.55(17) . 3_654 ? O2 Eu1 O3 79.44(17) 2_655 3_654 ? O2 Eu1 O3 79.44(17) 3_654 2_655 ? O2 Eu1 O3 138.55(17) 4_554 2_655 ? O2 Eu1 O3 74.01(18) . 2_655 ? O2 Eu1 O3 73.09(16) 2_655 2_655 ? O3 Eu1 O3 143.0(2) 3_654 2_655 ? O2 Eu1 O3 138.55(17) 3_654 . ? O2 Eu1 O3 79.44(17) 4_554 . ? O2 Eu1 O3 73.09(16) . . ? O2 Eu1 O3 74.01(18) 2_655 . ? O3 Eu1 O3 69.0(2) 3_654 . ? O3 Eu1 O3 124.0(2) 2_655 . ? O2 Eu1 O3 74.01(18) 3_654 4_554 ? O2 Eu1 O3 73.09(16) 4_554 4_554 ? O2 Eu1 O3 79.44(17) . 4_554 ? O2 Eu1 O3 138.55(17) 2_655 4_554 ? O3 Eu1 O3 124.0(2) 3_654 4_554 ? O3 Eu1 O3 69.0(2) 2_655 4_554 ? O3 Eu1 O3 143.0(2) . 4_554 ? Cl1 Zn1 O1 124.2(3) . 30 ? Cl1 Zn1 O4 117.2(3) . . ? O1 Zn1 O4 118.3(2) 30 . ? Cl1 Zn1 N2 101.17(16) . . ? O1 Zn1 N2 93.1(2) 30 . ? O4 Zn1 N2 80.10(19) . . ? Cl1 Zn1 N1 91.83(17) . 30 ? O1 Zn1 N1 79.7(2) 30 30 ? O4 Zn1 N1 93.7(2) . 30 ? N2 Zn1 N1 167.0(2) . 30 ? N3 Zn2 N3 117.2(3) . 2_755 ? N3 Zn2 O1W 121.42(17) . . ? N3 Zn2 O1W 121.42(17) 2_755 . ? N3 Zn2 O2W 88.3(3) . 2_755 ? N3 Zn2 O2W 92.8(3) 2_755 2_755 ? O1W Zn2 O2W 89.0(2) . 2_755 ? N3 Zn2 O2W 92.8(3) . . ? N3 Zn2 O2W 88.3(3) 2_755 . ? O1W Zn2 O2W 89.0(2) . . ? O2W Zn2 O2W 178.0(4) 2_755 . ? C5 N2 C3 104.2(6) . . ? C5 N2 Zn1 146.2(5) . . ? C3 N2 Zn1 109.7(4) . . ? C5 N1 C2 105.1(6) . . ? C5 N1 Zn1 143.2(5) . 18_665 ? C2 N1 Zn1 109.0(4) . 18_665 ? C4 O4 Zn1 117.0(4) . . ? C4 O3 Eu1 148.2(5) . . ? N1 C5 N2 113.9(6) . . ? N1 C5 C6 122.3(6) . . ? N2 C5 C6 123.7(7) . . ? C1 O2 Eu1 154.7(4) . . ? C1 O1 Zn1 118.1(4) . 18_665 ? C3 C2 N1 107.6(6) . . ? C3 C2 C1 134.4(6) . . ? N1 C2 C1 117.8(6) . . ? C2 C3 N2 109.1(5) . . ? C2 C3 C4 133.0(6) . . ? N2 C3 C4 117.6(5) . . ? C10 C6 C7 117.4(7) . . ? C10 C6 C5 120.5(6) . . ? C7 C6 C5 122.0(7) . . ? C10 N3 C9 118.3(7) . . ? C10 N3 Zn2 122.3(5) . . ? C9 N3 Zn2 119.4(5) . . ? O2 C1 O1 122.5(6) . . ? O2 C1 C2 122.8(6) . . ? O1 C1 C2 114.6(6) . . ? C7 C8 C9 119.0(8) . . ? C7 C8 H8A 120.5 . . ? C9 C8 H8A 120.5 . . ? C8 C7 C6 119.4(7) . . ? C8 C7 H7A 120.3 . . ? C6 C7 H7A 120.3 . . ? N3 C9 C8 123.2(7) . . ? N3 C9 H9A 118.4 . . ? C8 C9 H9A 118.4 . . ? O3 C4 O4 122.7(6) . . ? O3 C4 C3 121.6(6) . . ? O4 C4 C3 115.5(6) . . ? Zn2 O1W H1WA 121.9 . . ? Zn2 O1W H1WB 130.6 . . ? H1WA O1W H1WB 107.5 . . ? Zn1 Cl1 Zn1 175.4(6) 14_645 . ? N3 C10 C6 122.7(6) . . ? N3 C10 H10A 118.6 . . ? C6 C10 H10A 118.6 . . ? Zn2 O2W H2WB 123.9 . . ? Zn2 O2W H2WA 128.8 . . ? H2WB O2W H2WA 102.9 . . ? Cl2 Cl2 H1WB 168.4 25_765 . ? 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 Cl1 Zn1 N2 C5 -61.4(9) . . . . ? O1 Zn1 N2 C5 64.4(9) 30 . . . ? O4 Zn1 N2 C5 -177.3(9) . . . . ? N1 Zn1 N2 C5 120.5(11) 30 . . . ? Cl1 Zn1 N2 C3 118.9(5) . . . . ? O1 Zn1 N2 C3 -115.3(4) 30 . . . ? O4 Zn1 N2 C3 2.9(4) . . . . ? N1 Zn1 N2 C3 -59.3(11) 30 . . . ? Cl1 Zn1 O4 C4 -99.2(5) . . . . ? O1 Zn1 O4 C4 86.5(5) 30 . . . ? N2 Zn1 O4 C4 -1.7(5) . . . . ? N1 Zn1 O4 C4 166.8(5) 30 . . . ? O2 Eu1 O3 C4 -122.8(8) 3_654 . . . ? O2 Eu1 O3 C4 135.2(9) 4_554 . . . ? O2 Eu1 O3 C4 49.1(8) . . . . ? O2 Eu1 O3 C4 -63.4(8) 2_655 . . . ? O3 Eu1 O3 C4 -148.0(10) 3_654 . . . ? O3 Eu1 O3 C4 -7.4(8) 2_655 . . . ? O3 Eu1 O3 C4 92.9(8) 4_554 . . . ? C2 N1 C5 N2 0.4(8) . . . . ? Zn1 N1 C5 N2 -157.2(6) 18_665 . . . ? C2 N1 C5 C6 178.1(6) . . . . ? Zn1 N1 C5 C6 20.5(13) 18_665 . . . ? C3 N2 C5 N1 -0.8(8) . . . . ? Zn1 N2 C5 N1 179.5(6) . . . . ? C3 N2 C5 C6 -178.4(6) . . . . ? Zn1 N2 C5 C6 1.8(13) . . . . ? O2 Eu1 O2 C1 147.4(12) 3_654 . . . ? O2 Eu1 O2 C1 -103.5(12) 4_554 . . . ? O2 Eu1 O2 C1 44.8(11) 2_655 . . . ? O3 Eu1 O2 C1 -47.1(13) 3_654 . . . ? O3 Eu1 O2 C1 111.5(12) 2_655 . . . ? O3 Eu1 O2 C1 -22.6(11) . . . . ? O3 Eu1 O2 C1 -177.5(12) 4_554 . . . ? C5 N1 C2 C3 0.1(7) . . . . ? Zn1 N1 C2 C3 166.2(4) 18_665 . . . ? C5 N1 C2 C1 -175.9(6) . . . . ? Zn1 N1 C2 C1 -9.8(7) 18_665 . . . ? N1 C2 C3 N2 -0.6(7) . . . . ? C1 C2 C3 N2 174.4(7) . . . . ? N1 C2 C3 C4 -175.1(7) . . . . ? C1 C2 C3 C4 -0.1(13) . . . . ? C5 N2 C3 C2 0.8(7) . . . . ? Zn1 N2 C3 C2 -179.3(4) . . . . ? C5 N2 C3 C4 176.3(6) . . . . ? Zn1 N2 C3 C4 -3.9(7) . . . . ? N1 C5 C6 C10 13.6(11) . . . . ? N2 C5 C6 C10 -169.0(7) . . . . ? N1 C5 C6 C7 -162.6(8) . . . . ? N2 C5 C6 C7 14.9(11) . . . . ? N3 Zn2 N3 C10 -42.4(5) 2_755 . . . ? O1W Zn2 N3 C10 137.6(5) . . . . ? O2W Zn2 N3 C10 -134.6(6) 2_755 . . . ? O2W Zn2 N3 C10 47.1(6) . . . . ? N3 Zn2 N3 C9 135.5(7) 2_755 . . . ? O1W Zn2 N3 C9 -44.5(7) . . . . ? O2W Zn2 N3 C9 43.2(7) 2_755 . . . ? O2W Zn2 N3 C9 -135.0(7) . . . . ? Eu1 O2 C1 O1 -177.6(8) . . . . ? Eu1 O2 C1 C2 3.3(16) . . . . ? Zn1 O1 C1 O2 177.4(5) 18_665 . . . ? Zn1 O1 C1 C2 -3.4(8) 18_665 . . . ? C3 C2 C1 O2 13.8(12) . . . . ? N1 C2 C1 O2 -171.5(6) . . . . ? C3 C2 C1 O1 -165.4(7) . . . . ? N1 C2 C1 O1 9.3(9) . . . . ? C9 C8 C7 C6 0.0(13) . . . . ? C10 C6 C7 C8 -0.4(12) . . . . ? C5 C6 C7 C8 175.9(7) . . . . ? C10 N3 C9 C8 1.9(13) . . . . ? Zn2 N3 C9 C8 -176.0(7) . . . . ? C7 C8 C9 N3 -0.8(14) . . . . ? Eu1 O3 C4 O4 140.2(7) . . . . ? Eu1 O3 C4 C3 -43.8(12) . . . . ? Zn1 O4 C4 O3 176.3(5) . . . . ? Zn1 O4 C4 C3 0.1(7) . . . . ? C2 C3 C4 O3 0.5(11) . . . . ? N2 C3 C4 O3 -173.6(6) . . . . ? C2 C3 C4 O4 176.9(7) . . . . ? N2 C3 C4 O4 2.7(9) . . . . ? O1 Zn1 Cl1 Zn1 -13.73(18) 30 . . 14_645 ? O4 Zn1 Cl1 Zn1 172.41(15) . . . 14_645 ? N2 Zn1 Cl1 Zn1 87.89(15) . . . 14_645 ? N1 Zn1 Cl1 Zn1 -92.52(16) 30 . . 14_645 ? C9 N3 C10 C6 -2.3(12) . . . . ? Zn2 N3 C10 C6 175.6(6) . . . . ? C7 C6 C10 N3 1.5(12) . . . . ? C5 C6 C10 N3 -174.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 62.35 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.148 _refine_diff_density_min -1.961 _refine_diff_density_rms 0.193 ########################################################################### data_3-Tb-Zn _database_code_depnum_ccdc_archive 'CCDC 879667' _database_code_CSD 879667 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H28 Cl3 N12 O22 Tb Zn6' _chemical_formula_weight 1686.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Fddd ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 12.1678(5) _cell_length_b 22.6910(8) _cell_length_c 34.3938(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9496.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2144 _cell_measurement_theta_min 2.5672 _cell_measurement_theta_max 62.4213 _exptl_crystal_description block _exptl_crystal_colour yellow _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 2.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6592 _exptl_absorpt_coefficient_mu 12.935 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3059 _exptl_absorpt_correction_T_max 0.3890 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0855 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4642 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 4.32 _diffrn_reflns_theta_max 62.51 _reflns_number_total 1883 _reflns_number_gt 1758 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _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. ISOR and SIMU were applied to O1W. ; _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^)+(0.1500P)^2^+10.0000P] 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 1883 _refine_ls_number_parameters 199 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1701 _refine_ls_wR_factor_gt 0.1634 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.988 _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 0.8750 0.3750 -0.1250 0.0145(3) Uani 1 4 d S . . Zn1 Zn 0.99281(7) 0.17487(4) -0.00201(2) 0.0192(4) Uani 1 1 d . . . Zn2 Zn 1.3750 0.3750 0.14368(5) 0.0446(5) Uani 1 2 d S . . N2 N 1.0625(5) 0.2602(3) 0.00069(16) 0.0191(12) Uani 1 1 d . . . N1 N 1.1382(5) 0.3495(3) 0.00424(17) 0.0199(13) Uani 1 1 d . . . O4 O 0.9373(4) 0.2088(2) -0.05375(14) 0.0260(12) Uani 1 1 d . . . O3 O 0.9378(4) 0.2868(2) -0.09195(14) 0.0264(12) Uani 1 1 d . . . C5 C 1.1268(5) 0.2970(3) 0.0211(2) 0.0203(16) Uani 1 1 d . . . O2 O 1.0185(4) 0.4035(2) -0.08402(15) 0.0267(12) Uani 1 1 d . . . O1 O 1.1516(5) 0.4379(2) -0.04699(16) 0.0303(12) Uani 1 1 d . . . C2 C 1.0763(6) 0.3472(3) -0.02921(19) 0.0196(14) Uani 1 1 d . . . C3 C 1.0302(5) 0.2924(3) -0.03123(19) 0.0178(13) Uani 1 1 d . . . C6 C 1.1839(6) 0.2806(3) 0.0573(2) 0.0242(16) Uani 1 1 d . . . N3 N 1.2926(5) 0.3109(3) 0.11219(19) 0.0295(14) Uani 1 1 d . . . C1 C 1.0795(6) 0.3989(3) -0.0555(2) 0.0207(15) Uani 1 1 d . . . C8 C 1.2539(8) 0.2095(4) 0.1024(3) 0.040(2) Uani 1 1 d . . . H8A H 1.2607 0.1708 0.1109 0.049 Uiso 1 1 calc R . . C7 C 1.1957(7) 0.2225(3) 0.0691(2) 0.0333(18) Uani 1 1 d . . . H7A H 1.1643 0.1923 0.0546 0.040 Uiso 1 1 calc R . . C9 C 1.3013(8) 0.2545(4) 0.1227(2) 0.039(2) Uani 1 1 d . . . H9A H 1.3417 0.2455 0.1448 0.047 Uiso 1 1 calc R . . C4 C 0.9621(6) 0.2623(3) -0.0614(2) 0.0212(15) Uani 1 1 d . . . O1W O 1.3750 0.3750 0.2058(2) 0.041(2) Uani 1 2 d SU . . H1WA H 1.3824 0.3434 0.2189 0.062 Uiso 0.50 1 d PR . . H1WB H 1.3706 0.4034 0.2219 0.062 Uiso 0.50 1 d PR . . Cl1 Cl 1.1250 0.1250 -0.0029(3) 0.151(4) Uani 1 2 d S . . C10 C 1.2342(7) 0.3235(3) 0.0800(2) 0.0302(18) Uani 1 1 d . . . H10A H 1.2273 0.3627 0.0726 0.036 Uiso 1 1 calc R . . O2W O 1.2337(6) 0.4330(3) 0.1446(2) 0.064(2) Uani 1 1 d . . . H2WB H 1.2214 0.4619 0.1267 0.096 Uiso 1 1 d R . . H2WA H 1.1958 0.4443 0.1642 0.096 Uiso 1 1 d R . . Cl2 Cl 1.2861(12) 0.4656(7) 0.2366(5) 0.093(5) Uani 0.25 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 Tb1 0.0158(5) 0.0160(5) 0.0118(5) 0.000 0.000 0.000 Zn1 0.0219(6) 0.0169(6) 0.0188(6) 0.0010(3) 0.0009(3) -0.0032(4) Zn2 0.0479(11) 0.0572(12) 0.0286(10) 0.000 0.000 -0.0148(8) N2 0.019(3) 0.018(3) 0.020(3) 0.002(2) -0.003(2) -0.004(2) N1 0.024(3) 0.019(3) 0.017(3) 0.003(2) -0.006(2) -0.006(2) O4 0.037(3) 0.015(2) 0.025(3) 0.002(2) -0.008(2) -0.010(2) O3 0.035(3) 0.021(2) 0.023(3) 0.007(2) -0.012(2) -0.006(2) C5 0.025(4) 0.018(4) 0.018(4) 0.002(3) -0.005(3) -0.007(3) O2 0.031(3) 0.021(3) 0.028(3) 0.008(2) -0.012(2) -0.011(2) O1 0.040(3) 0.025(3) 0.026(3) 0.006(2) -0.012(2) -0.015(2) C2 0.023(4) 0.024(4) 0.012(3) 0.003(3) -0.003(3) 0.001(3) C3 0.020(3) 0.019(3) 0.015(3) -0.001(3) -0.006(3) -0.002(3) C6 0.027(4) 0.025(4) 0.021(3) 0.009(3) -0.001(3) 0.000(3) N3 0.034(3) 0.032(3) 0.022(3) -0.002(3) -0.009(3) 0.000(3) C1 0.019(3) 0.018(4) 0.025(4) 0.002(3) -0.007(3) -0.008(3) C8 0.057(5) 0.031(4) 0.033(4) 0.012(4) -0.017(4) 0.000(4) C7 0.043(4) 0.022(4) 0.034(4) 0.008(3) -0.014(4) -0.004(3) C9 0.039(5) 0.052(6) 0.027(4) 0.015(4) -0.008(3) 0.006(4) C4 0.021(3) 0.020(3) 0.023(4) 0.003(3) -0.004(3) -0.004(3) O1W 0.046(5) 0.068(5) 0.009(3) 0.000 0.000 -0.036(4) Cl1 0.117(6) 0.185(10) 0.151(8) 0.000 0.000 0.050(6) C10 0.038(4) 0.027(4) 0.025(4) 0.007(3) -0.011(3) -0.007(3) O2W 0.070(5) 0.064(5) 0.057(5) 0.004(4) 0.029(4) 0.013(4) Cl2 0.079(9) 0.081(9) 0.119(12) 0.031(8) -0.030(8) -0.027(7) _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 O2 2.335(5) 3_654 ? Tb1 O2 2.335(5) 4_554 ? Tb1 O2 2.335(5) . ? Tb1 O2 2.335(5) 2_655 ? Tb1 O3 2.425(5) 3_654 ? Tb1 O3 2.425(5) 2_655 ? Tb1 O3 2.425(5) . ? Tb1 O3 2.425(5) 4_554 ? Zn1 Cl1 1.9669(9) . ? Zn1 O1 2.040(5) 30 ? Zn1 O4 2.053(5) . ? Zn1 N2 2.115(6) . ? Zn1 N1 2.134(6) 30 ? Zn2 N3 2.072(6) . ? Zn2 N3 2.072(6) 2_755 ? Zn2 O1W 2.136(8) . ? Zn2 O2W 2.165(8) 2_755 ? Zn2 O2W 2.165(8) . ? N2 C5 1.344(9) . ? N2 C3 1.377(9) . ? N1 C5 1.332(10) . ? N1 C2 1.377(9) . ? N1 Zn1 2.134(6) 18_665 ? O4 C4 1.279(8) . ? O3 C4 1.224(9) . ? C5 C6 1.473(10) . ? O2 C1 1.235(9) . ? O1 C1 1.280(9) . ? O1 Zn1 2.040(5) 18_665 ? C2 C3 1.365(10) . ? C2 C1 1.482(9) . ? C3 C4 1.494(9) . ? C6 C10 1.389(11) . ? C6 C7 1.387(11) . ? N3 C10 1.346(10) . ? N3 C9 1.333(12) . ? C8 C7 1.378(12) . ? C8 C9 1.364(14) . ? C8 H8A 0.9300 . ? C7 H7A 0.9300 . ? C9 H9A 0.9300 . ? O1W H1WA 0.8514 . ? O1W H1WB 0.8518 . ? Cl1 Zn1 1.9669(9) 14_645 ? C10 H10A 0.9300 . ? O2W H2WB 0.9131 . ? O2W H2WA 0.8560 . ? Cl2 Cl2 2.01(4) 25_765 ? Cl2 H1WB 1.8186 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Tb1 O2 105.8(3) 3_654 4_554 ? O2 Tb1 O2 147.8(2) 3_654 . ? O2 Tb1 O2 83.2(3) 4_554 . ? O2 Tb1 O2 83.2(3) 3_654 2_655 ? O2 Tb1 O2 147.8(2) 4_554 2_655 ? O2 Tb1 O2 105.8(3) . 2_655 ? O2 Tb1 O3 73.17(16) 3_654 3_654 ? O2 Tb1 O3 73.97(18) 4_554 3_654 ? O2 Tb1 O3 138.35(17) . 3_654 ? O2 Tb1 O3 79.55(17) 2_655 3_654 ? O2 Tb1 O3 79.55(17) 3_654 2_655 ? O2 Tb1 O3 138.35(17) 4_554 2_655 ? O2 Tb1 O3 73.97(18) . 2_655 ? O2 Tb1 O3 73.17(16) 2_655 2_655 ? O3 Tb1 O3 143.3(2) 3_654 2_655 ? O2 Tb1 O3 138.35(17) 3_654 . ? O2 Tb1 O3 79.55(17) 4_554 . ? O2 Tb1 O3 73.17(16) . . ? O2 Tb1 O3 73.97(18) 2_655 . ? O3 Tb1 O3 68.8(2) 3_654 . ? O3 Tb1 O3 124.1(2) 2_655 . ? O2 Tb1 O3 73.97(18) 3_654 4_554 ? O2 Tb1 O3 73.17(16) 4_554 4_554 ? O2 Tb1 O3 79.55(17) . 4_554 ? O2 Tb1 O3 138.35(17) 2_655 4_554 ? O3 Tb1 O3 124.1(2) 3_654 4_554 ? O3 Tb1 O3 68.8(2) 2_655 4_554 ? O3 Tb1 O3 143.3(2) . 4_554 ? Cl1 Zn1 O1 122.8(3) . 30 ? Cl1 Zn1 O4 118.1(3) . . ? O1 Zn1 O4 118.9(2) 30 . ? Cl1 Zn1 N2 101.50(16) . . ? O1 Zn1 N2 92.8(2) 30 . ? O4 Zn1 N2 80.0(2) . . ? Cl1 Zn1 N1 91.48(17) . 30 ? O1 Zn1 N1 79.7(2) 30 30 ? O4 Zn1 N1 94.2(2) . 30 ? N2 Zn1 N1 167.0(2) . 30 ? N3 Zn2 N3 117.0(4) . 2_755 ? N3 Zn2 O1W 121.51(19) . . ? N3 Zn2 O1W 121.51(19) 2_755 . ? N3 Zn2 O2W 88.0(3) . 2_755 ? N3 Zn2 O2W 92.8(3) 2_755 2_755 ? O1W Zn2 O2W 89.2(2) . 2_755 ? N3 Zn2 O2W 92.8(3) . . ? N3 Zn2 O2W 88.0(3) 2_755 . ? O1W Zn2 O2W 89.2(2) . . ? O2W Zn2 O2W 178.3(4) 2_755 . ? C5 N2 C3 104.7(6) . . ? C5 N2 Zn1 145.6(5) . . ? C3 N2 Zn1 109.7(4) . . ? C5 N1 C2 105.9(6) . . ? C5 N1 Zn1 142.6(5) . 18_665 ? C2 N1 Zn1 109.1(4) . 18_665 ? C4 O4 Zn1 117.2(4) . . ? C4 O3 Tb1 148.5(5) . . ? N1 C5 N2 112.8(6) . . ? N1 C5 C6 123.0(6) . . ? N2 C5 C6 124.1(6) . . ? C1 O2 Tb1 154.9(4) . . ? C1 O1 Zn1 117.5(4) . 18_665 ? C3 C2 N1 107.6(6) . . ? C3 C2 C1 134.5(6) . . ? N1 C2 C1 117.7(6) . . ? C2 C3 N2 109.0(6) . . ? C2 C3 C4 132.8(6) . . ? N2 C3 C4 118.0(6) . . ? C10 C6 C7 117.1(7) . . ? C10 C6 C5 120.4(6) . . ? C7 C6 C5 122.4(7) . . ? C10 N3 C9 117.9(7) . . ? C10 N3 Zn2 122.4(5) . . ? C9 N3 Zn2 119.6(5) . . ? O2 C1 O1 122.3(6) . . ? O2 C1 C2 122.4(6) . . ? O1 C1 C2 115.3(6) . . ? C7 C8 C9 118.8(8) . . ? C7 C8 H8A 120.6 . . ? C9 C8 H8A 120.6 . . ? C8 C7 C6 120.0(8) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? N3 C9 C8 123.2(8) . . ? N3 C9 H9A 118.4 . . ? C8 C9 H9A 118.4 . . ? O3 C4 O4 123.5(6) . . ? O3 C4 C3 121.5(6) . . ? O4 C4 C3 114.9(6) . . ? Zn2 O1W H1WA 121.9 . . ? Zn2 O1W H1WB 130.6 . . ? H1WA O1W H1WB 107.4 . . ? Zn1 Cl1 Zn1 178.3(6) 14_645 . ? N3 C10 C6 123.1(7) . . ? N3 C10 H10A 118.5 . . ? C6 C10 H10A 118.5 . . ? Zn2 O2W H2WB 123.9 . . ? Zn2 O2W H2WA 128.5 . . ? H2WB O2W H2WA 103.1 . . ? Cl2 Cl2 H1WB 167.2 25_765 . ? 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 Cl1 Zn1 N2 C5 -60.2(9) . . . . ? O1 Zn1 N2 C5 64.1(9) 30 . . . ? O4 Zn1 N2 C5 -177.1(9) . . . . ? N1 Zn1 N2 C5 118.5(11) 30 . . . ? Cl1 Zn1 N2 C3 119.9(5) . . . . ? O1 Zn1 N2 C3 -115.8(5) 30 . . . ? O4 Zn1 N2 C3 3.0(4) . . . . ? N1 Zn1 N2 C3 -61.5(12) 30 . . . ? Cl1 Zn1 O4 C4 -99.9(5) . . . . ? O1 Zn1 O4 C4 85.6(5) 30 . . . ? N2 Zn1 O4 C4 -2.1(5) . . . . ? N1 Zn1 O4 C4 166.1(5) 30 . . . ? O2 Tb1 O3 C4 -122.5(9) 3_654 . . . ? O2 Tb1 O3 C4 135.5(9) 4_554 . . . ? O2 Tb1 O3 C4 49.4(9) . . . . ? O2 Tb1 O3 C4 -63.0(9) 2_655 . . . ? O3 Tb1 O3 C4 -147.8(10) 3_654 . . . ? O3 Tb1 O3 C4 -7.0(8) 2_655 . . . ? O3 Tb1 O3 C4 93.2(9) 4_554 . . . ? C2 N1 C5 N2 0.8(8) . . . . ? Zn1 N1 C5 N2 -158.0(6) 18_665 . . . ? C2 N1 C5 C6 177.7(7) . . . . ? Zn1 N1 C5 C6 18.9(13) 18_665 . . . ? C3 N2 C5 N1 -0.8(8) . . . . ? Zn1 N2 C5 N1 179.3(6) . . . . ? C3 N2 C5 C6 -177.7(7) . . . . ? Zn1 N2 C5 C6 2.4(13) . . . . ? O2 Tb1 O2 C1 145.4(12) 3_654 . . . ? O2 Tb1 O2 C1 -105.6(13) 4_554 . . . ? O2 Tb1 O2 C1 42.8(12) 2_655 . . . ? O3 Tb1 O2 C1 -49.1(13) 3_654 . . . ? O3 Tb1 O2 C1 109.6(12) 2_655 . . . ? O3 Tb1 O2 C1 -24.5(12) . . . . ? O3 Tb1 O2 C1 -179.7(12) 4_554 . . . ? C5 N1 C2 C3 -0.5(8) . . . . ? Zn1 N1 C2 C3 166.1(5) 18_665 . . . ? C5 N1 C2 C1 -176.1(6) . . . . ? Zn1 N1 C2 C1 -9.5(8) 18_665 . . . ? N1 C2 C3 N2 0.0(8) . . . . ? C1 C2 C3 N2 174.6(8) . . . . ? N1 C2 C3 C4 -175.1(7) . . . . ? C1 C2 C3 C4 -0.6(14) . . . . ? C5 N2 C3 C2 0.4(8) . . . . ? Zn1 N2 C3 C2 -179.6(5) . . . . ? C5 N2 C3 C4 176.4(6) . . . . ? Zn1 N2 C3 C4 -3.6(7) . . . . ? N1 C5 C6 C10 13.8(11) . . . . ? N2 C5 C6 C10 -169.6(7) . . . . ? N1 C5 C6 C7 -162.3(8) . . . . ? N2 C5 C6 C7 14.3(12) . . . . ? N3 Zn2 N3 C10 -41.1(6) 2_755 . . . ? O1W Zn2 N3 C10 138.9(6) . . . . ? O2W Zn2 N3 C10 -133.3(7) 2_755 . . . ? O2W Zn2 N3 C10 48.2(7) . . . . ? N3 Zn2 N3 C9 135.4(7) 2_755 . . . ? O1W Zn2 N3 C9 -44.6(7) . . . . ? O2W Zn2 N3 C9 43.2(7) 2_755 . . . ? O2W Zn2 N3 C9 -135.3(7) . . . . ? Tb1 O2 C1 O1 -175.8(8) . . . . ? Tb1 O2 C1 C2 5.7(17) . . . . ? Zn1 O1 C1 O2 178.2(6) 18_665 . . . ? Zn1 O1 C1 C2 -3.2(9) 18_665 . . . ? C3 C2 C1 O2 13.4(13) . . . . ? N1 C2 C1 O2 -172.5(7) . . . . ? C3 C2 C1 O1 -165.2(8) . . . . ? N1 C2 C1 O1 9.0(10) . . . . ? C9 C8 C7 C6 -1.6(14) . . . . ? C10 C6 C7 C8 1.0(12) . . . . ? C5 C6 C7 C8 177.3(8) . . . . ? C10 N3 C9 C8 -0.2(14) . . . . ? Zn2 N3 C9 C8 -176.9(7) . . . . ? C7 C8 C9 N3 1.2(15) . . . . ? Tb1 O3 C4 O4 140.5(7) . . . . ? Tb1 O3 C4 C3 -43.6(13) . . . . ? Zn1 O4 C4 O3 176.9(6) . . . . ? Zn1 O4 C4 C3 0.8(8) . . . . ? C2 C3 C4 O3 0.7(12) . . . . ? N2 C3 C4 O3 -174.1(7) . . . . ? C2 C3 C4 O4 176.9(7) . . . . ? N2 C3 C4 O4 2.1(9) . . . . ? O1 Zn1 Cl1 Zn1 -13.36(18) 30 . . 14_645 ? O4 Zn1 Cl1 Zn1 172.34(15) . . . 14_645 ? N2 Zn1 Cl1 Zn1 87.61(16) . . . 14_645 ? N1 Zn1 Cl1 Zn1 -92.08(16) 30 . . 14_645 ? C9 N3 C10 C6 -0.4(13) . . . . ? Zn2 N3 C10 C6 176.1(6) . . . . ? C7 C6 C10 N3 0.0(12) . . . . ? C5 C6 C10 N3 -176.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 62.51 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.981 _refine_diff_density_min -1.766 _refine_diff_density_rms 0.194 ####################################################################### data_4-Tb-Zn _database_code_depnum_ccdc_archive 'CCDC 879668' #TrackingRef 'compounds.txt' _database_code_CSD 879668 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 N3 O11 S Tb Zn, 3(H2 O)' _chemical_formula_sum 'C10 H16 N3 O14 S Tb Zn' _chemical_formula_weight 658.61 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' 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 13.5730(18) _cell_length_b 11.7732(16) _cell_length_c 12.9248(17) _cell_angle_alpha 90.00 _cell_angle_beta 117.6530(10) _cell_angle_gamma 90.00 _cell_volume 1829.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9894 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 28.01 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 5.342 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2798 _exptl_absorpt_correction_T_max 0.3373 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17479 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3587 _reflns_number_gt 3221 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0223P)^2^+5.8815P] 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 3587 _refine_ls_number_parameters 271 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0572 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.488125(16) 0.446665(16) 1.149839(16) 0.01413(7) Uani 1 1 d . . . Zn1 Zn 0.15825(4) 0.25695(4) 0.95413(4) 0.01540(12) Uani 1 1 d . . . O1 O 0.3137(2) 0.3639(2) 1.0012(2) 0.0173(6) Uani 1 1 d . . . N1 N 0.1831(3) 0.2512(3) 0.8040(3) 0.0140(7) Uani 1 1 d . . . C5 C 0.1357(3) 0.2073(3) 0.6963(3) 0.0132(8) Uani 1 1 d . . . C2 C 0.2553(3) 0.3328(3) 0.8023(3) 0.0132(8) Uani 1 1 d . . . C1 C 0.3246(3) 0.3915(3) 0.9118(3) 0.0129(8) Uani 1 1 d . . . C6 C 0.0583(4) 0.1095(3) 0.6630(4) 0.0165(9) Uani 1 1 d . . . O4 O 0.2676(3) 0.3823(3) 0.5267(3) 0.0221(7) Uani 1 1 d . . . N2 N 0.1707(3) 0.2546(3) 0.6241(3) 0.0149(7) Uani 1 1 d . . . C4 C 0.3019(3) 0.4004(3) 0.6346(3) 0.0144(8) Uani 1 1 d . . . C3 C 0.2470(3) 0.3342(3) 0.6910(4) 0.0137(8) Uani 1 1 d . . . N3 N -0.0738(3) -0.0852(3) 0.6001(3) 0.0169(7) Uani 1 1 d . . . O3W O 0.0157(3) 0.1504(3) 0.8917(3) 0.0261(7) Uani 1 1 d . . . H3WA H -0.0116 0.1402 0.9383 0.031 Uiso 1 1 d R . . H3WB H -0.0412 0.1687 0.8290 0.031 Uiso 1 1 d R . . O2W O 0.3719(3) 0.4575(3) 1.2404(3) 0.0309(8) Uani 1 1 d . . . H2WA H 0.3346 0.5182 1.2295 0.037 Uiso 1 1 d R . . H2WB H 0.3592 0.4156 1.2864 0.037 Uiso 1 1 d R . . O2 O 0.3980(2) 0.4643(2) 0.9230(2) 0.0172(6) Uani 1 1 d . . . O1W O 0.5518(3) 0.2979(3) 1.0715(3) 0.0256(7) Uani 1 1 d D . . H1WA H 0.5676 0.3144 1.0194 0.031 Uiso 1 1 d RD . . H1WB H 0.6035 0.2603 1.1198 0.031 Uiso 1 1 d RD . . O7 O 0.4577(3) 0.7955(3) 1.2188(3) 0.0267(7) Uani 1 1 d . . . O5 O 0.4059(3) 0.6259(3) 1.1036(3) 0.0255(7) Uani 1 1 d . . . O8 O 0.3059(3) 0.6813(3) 1.2081(4) 0.0452(10) Uani 1 1 d . . . O6 O 0.2865(3) 0.7866(3) 1.0400(3) 0.0489(11) Uani 1 1 d . . . S1 S 0.36205(10) 0.72467(9) 1.14292(10) 0.0233(2) Uani 1 1 d . . . C10 C -0.1064(4) 0.0101(4) 0.5351(4) 0.0187(9) Uani 1 1 d . . . H10 H -0.1749 0.0098 0.4682 0.022 Uiso 1 1 calc R . . C9 C 0.0223(4) -0.0819(4) 0.6979(4) 0.0235(10) Uani 1 1 d . . . H9 H 0.0444 -0.1462 0.7451 0.028 Uiso 1 1 calc R . . C8 C -0.0437(4) 0.1080(4) 0.5625(4) 0.0188(9) Uani 1 1 d . . . H8 H -0.0690 0.1717 0.5148 0.023 Uiso 1 1 calc R . . C7 C 0.0915(4) 0.0126(4) 0.7330(4) 0.0219(10) Uani 1 1 d . . . H7 H 0.1584 0.0113 0.8017 0.026 Uiso 1 1 calc R . . O3 O 0.3783(3) 0.4696(3) 0.6923(3) 0.0266(7) Uani 1 1 d . . . O4W O 0.4342(3) 0.4027(3) 0.4652(3) 0.0416(9) Uani 1 1 d . . . H4WA H 0.3974 0.4072 0.5033 0.050 Uiso 1 1 d R . . H4WB H 0.4964 0.3719 0.5094 0.050 Uiso 1 1 d R . . O5W O 0.0898(3) 0.9041(3) 0.9806(4) 0.0486(11) Uani 1 1 d . . . H5WA H 0.1580 0.8856 1.0139 0.058 Uiso 1 1 d R . . H5WB H 0.0926 0.9735 0.9640 0.058 Uiso 1 1 d R . . O6W O 0.8162(3) 0.1853(4) 0.6988(4) 0.0555(12) Uani 1 1 d D . . H6WA H 0.7867 0.2032 0.6297 0.067 Uiso 1 1 d RD . . H6WB H 0.7790 0.2130 0.7275 0.067 Uiso 1 1 d RD . . 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 0.01455(12) 0.01448(11) 0.01241(11) -0.00208(7) 0.00545(8) -0.00406(8) Zn1 0.0175(3) 0.0161(2) 0.0135(2) 0.00365(18) 0.0079(2) 0.00405(19) O1 0.0164(15) 0.0216(15) 0.0144(15) -0.0017(12) 0.0074(12) -0.0046(12) N1 0.0132(17) 0.0146(17) 0.0123(17) -0.0009(13) 0.0044(14) -0.0029(13) C5 0.013(2) 0.0124(19) 0.014(2) 0.0007(15) 0.0062(17) -0.0010(16) C2 0.014(2) 0.0126(19) 0.014(2) -0.0014(15) 0.0075(17) -0.0031(16) C1 0.010(2) 0.0130(19) 0.016(2) -0.0010(16) 0.0064(17) 0.0022(15) C6 0.018(2) 0.018(2) 0.016(2) -0.0072(16) 0.0100(18) -0.0044(17) O4 0.0243(17) 0.0271(17) 0.0164(16) -0.0061(13) 0.0106(13) -0.0110(13) N2 0.0135(18) 0.0154(17) 0.0161(18) -0.0038(14) 0.0070(15) -0.0038(14) C4 0.012(2) 0.015(2) 0.014(2) -0.0015(16) 0.0044(17) -0.0021(16) C3 0.013(2) 0.0131(19) 0.016(2) -0.0020(16) 0.0077(17) -0.0025(16) N3 0.0175(19) 0.0167(17) 0.0180(18) -0.0055(14) 0.0095(15) -0.0062(15) O3W 0.0221(17) 0.0344(18) 0.0221(17) -0.0015(14) 0.0104(14) -0.0044(14) O2W 0.030(2) 0.037(2) 0.034(2) 0.0007(15) 0.0218(17) -0.0003(15) O2 0.0129(15) 0.0201(15) 0.0155(15) -0.0036(12) 0.0040(12) -0.0056(12) O1W 0.0313(19) 0.0255(17) 0.0252(17) 0.0052(14) 0.0175(15) 0.0057(14) O7 0.0300(19) 0.0239(17) 0.0268(18) -0.0083(14) 0.0137(15) -0.0040(14) O5 0.0321(19) 0.0205(16) 0.0293(18) -0.0056(14) 0.0188(16) 0.0016(14) O8 0.053(3) 0.036(2) 0.075(3) -0.015(2) 0.053(2) -0.0072(18) O6 0.047(2) 0.041(2) 0.037(2) -0.0063(18) 0.0019(19) 0.0210(19) S1 0.0229(6) 0.0212(6) 0.0250(6) -0.0072(4) 0.0105(5) 0.0030(5) C10 0.015(2) 0.020(2) 0.021(2) 0.0002(18) 0.0086(18) -0.0007(17) C9 0.027(3) 0.019(2) 0.018(2) 0.0013(18) 0.005(2) -0.0045(19) C8 0.020(2) 0.017(2) 0.023(2) 0.0015(17) 0.0126(19) -0.0014(17) C7 0.022(2) 0.022(2) 0.017(2) -0.0030(18) 0.0043(19) -0.0073(19) O3 0.0288(19) 0.0314(18) 0.0174(16) -0.0042(13) 0.0088(14) -0.0154(15) O4W 0.050(2) 0.044(2) 0.049(2) 0.0014(19) 0.038(2) 0.0009(19) O5W 0.047(3) 0.043(2) 0.070(3) 0.013(2) 0.039(2) 0.008(2) O6W 0.033(2) 0.090(3) 0.039(2) -0.008(2) 0.012(2) 0.008(2) _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 2.233(3) 3_667 ? Tb1 O7 2.330(3) 2_647 ? Tb1 O5 2.331(3) . ? Tb1 O2W 2.364(3) . ? Tb1 O1W 2.378(3) . ? Tb1 O2 2.393(3) 3_667 ? Tb1 O1 2.454(3) . ? Tb1 O2 2.609(3) . ? Zn1 O4 2.116(3) 4_566 ? Zn1 N1 2.119(3) . ? Zn1 N3 2.125(3) 2_556 ? Zn1 O3W 2.126(3) . ? Zn1 N2 2.128(3) 4_566 ? Zn1 O1 2.283(3) . ? O1 C1 1.275(5) . ? N1 C5 1.338(5) . ? N1 C2 1.380(5) . ? C5 N2 1.349(5) . ? C5 C6 1.481(6) . ? C2 C3 1.390(6) . ? C2 C1 1.459(5) . ? C1 O2 1.270(5) . ? C6 C8 1.391(6) . ? C6 C7 1.395(6) . ? O4 C4 1.267(5) . ? O4 Zn1 2.116(3) 4_565 ? N2 C3 1.366(5) . ? N2 Zn1 2.128(3) 4_565 ? C4 O3 1.256(5) . ? C4 C3 1.482(6) . ? N3 C9 1.331(6) . ? N3 C10 1.347(5) . ? N3 Zn1 2.125(3) 2_546 ? O3W H3WA 0.8489 . ? O3W H3WB 0.8480 . ? O2W H2WA 0.8499 . ? O2W H2WB 0.8499 . ? O2 Tb1 2.393(3) 3_667 ? O1W H1WA 0.8192 . ? O1W H1WB 0.8196 . ? O7 S1 1.470(3) . ? O7 Tb1 2.330(3) 2_657 ? O5 S1 1.499(3) . ? O8 S1 1.465(4) . ? O6 S1 1.445(4) . ? C10 C8 1.378(6) . ? C10 H10 0.9300 . ? C9 C7 1.389(6) . ? C9 H9 0.9300 . ? C8 H8 0.9300 . ? C7 H7 0.9300 . ? O3 Tb1 2.233(3) 3_667 ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? O5W H5WA 0.8491 . ? O5W H5WB 0.8492 . ? O6W H6WA 0.8193 . ? O6W H6WB 0.8190 . ? 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 O7 79.82(12) 3_667 2_647 ? O3 Tb1 O5 85.63(12) 3_667 . ? O7 Tb1 O5 146.05(11) 2_647 . ? O3 Tb1 O2W 88.23(12) 3_667 . ? O7 Tb1 O2W 74.81(12) 2_647 . ? O5 Tb1 O2W 74.23(12) . . ? O3 Tb1 O1W 114.39(12) 3_667 . ? O7 Tb1 O1W 72.15(11) 2_647 . ? O5 Tb1 O1W 141.53(11) . . ? O2W Tb1 O1W 135.11(11) . . ? O3 Tb1 O2 76.55(11) 3_667 3_667 ? O7 Tb1 O2 125.31(11) 2_647 3_667 ? O5 Tb1 O2 79.77(11) . 3_667 ? O2W Tb1 O2 150.76(11) . 3_667 ? O1W Tb1 O2 74.12(10) . 3_667 ? O3 Tb1 O1 165.79(11) 3_667 . ? O7 Tb1 O1 97.50(11) 2_647 . ? O5 Tb1 O1 89.19(11) . . ? O2W Tb1 O1 77.62(11) . . ? O1W Tb1 O1 77.49(11) . . ? O2 Tb1 O1 115.53(9) 3_667 . ? O3 Tb1 O2 138.61(10) 3_667 . ? O7 Tb1 O2 134.77(10) 2_647 . ? O5 Tb1 O2 73.81(10) . . ? O2W Tb1 O2 118.65(11) . . ? O1W Tb1 O2 69.72(10) . . ? O2 Tb1 O2 64.84(11) 3_667 . ? O1 Tb1 O2 51.19(9) . . ? O4 Zn1 N1 90.23(12) 4_566 . ? O4 Zn1 N3 169.73(14) 4_566 2_556 ? N1 Zn1 N3 90.96(13) . 2_556 ? O4 Zn1 O3W 92.23(13) 4_566 . ? N1 Zn1 O3W 97.89(13) . . ? N3 Zn1 O3W 97.71(13) 2_556 . ? O4 Zn1 N2 77.86(12) 4_566 4_566 ? N1 Zn1 N2 166.67(13) . 4_566 ? N3 Zn1 N2 99.71(13) 2_556 4_566 ? O3W Zn1 N2 88.64(13) . 4_566 ? O4 Zn1 O1 86.41(12) 4_566 . ? N1 Zn1 O1 75.04(11) . . ? N3 Zn1 O1 84.04(13) 2_556 . ? O3W Zn1 O1 172.78(11) . . ? N2 Zn1 O1 97.99(12) 4_566 . ? C1 O1 Zn1 112.4(2) . . ? C1 O1 Tb1 97.6(2) . . ? Zn1 O1 Tb1 149.76(13) . . ? C5 N1 C2 104.8(3) . . ? C5 N1 Zn1 139.6(3) . . ? C2 N1 Zn1 114.1(3) . . ? N1 C5 N2 114.0(3) . . ? N1 C5 C6 122.4(4) . . ? N2 C5 C6 123.4(4) . . ? N1 C2 C3 107.9(3) . . ? N1 C2 C1 117.3(3) . . ? C3 C2 C1 134.7(4) . . ? O2 C1 O1 118.9(4) . . ? O2 C1 C2 123.3(4) . . ? O1 C1 C2 117.7(3) . . ? C8 C6 C7 118.5(4) . . ? C8 C6 C5 123.0(4) . . ? C7 C6 C5 118.4(4) . . ? C4 O4 Zn1 116.2(3) . 4_565 ? C5 N2 C3 104.6(3) . . ? C5 N2 Zn1 143.4(3) . 4_565 ? C3 N2 Zn1 111.8(3) . 4_565 ? O3 C4 O4 122.9(4) . . ? O3 C4 C3 120.9(4) . . ? O4 C4 C3 116.2(3) . . ? N2 C3 C2 108.7(3) . . ? N2 C3 C4 117.1(3) . . ? C2 C3 C4 134.2(4) . . ? C9 N3 C10 117.5(4) . . ? C9 N3 Zn1 118.6(3) . 2_546 ? C10 N3 Zn1 123.5(3) . 2_546 ? Zn1 O3W H3WA 115.7 . . ? Zn1 O3W H3WB 118.5 . . ? H3WA O3W H3WB 102.2 . . ? Tb1 O2W H2WA 116.6 . . ? Tb1 O2W H2WB 135.6 . . ? H2WA O2W H2WB 107.7 . . ? C1 O2 Tb1 150.0(3) . 3_667 ? C1 O2 Tb1 90.5(2) . . ? Tb1 O2 Tb1 115.16(11) 3_667 . ? Tb1 O1W H1WA 117.4 . . ? Tb1 O1W H1WB 115.1 . . ? H1WA O1W H1WB 107.3 . . ? S1 O7 Tb1 143.3(2) . 2_657 ? S1 O5 Tb1 146.5(2) . . ? O6 S1 O8 111.7(3) . . ? O6 S1 O7 110.9(2) . . ? O8 S1 O7 110.3(2) . . ? O6 S1 O5 107.7(2) . . ? O8 S1 O5 108.6(2) . . ? O7 S1 O5 107.45(19) . . ? N3 C10 C8 123.4(4) . . ? N3 C10 H10 118.3 . . ? C8 C10 H10 118.3 . . ? N3 C9 C7 123.3(4) . . ? N3 C9 H9 118.3 . . ? C7 C9 H9 118.3 . . ? C10 C8 C6 118.6(4) . . ? C10 C8 H8 120.7 . . ? C6 C8 H8 120.7 . . ? C9 C7 C6 118.5(4) . . ? C9 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C4 O3 Tb1 157.7(3) . 3_667 ? H4WA O4W H4WB 107.7 . . ? H5WA O5W H5WB 102.1 . . ? H6WA O6W H6WB 107.5 . . ? 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 O4 Zn1 O1 C1 107.0(3) 4_566 . . . ? N1 Zn1 O1 C1 15.8(3) . . . . ? N3 Zn1 O1 C1 -76.8(3) 2_556 . . . ? N2 Zn1 O1 C1 -175.8(3) 4_566 . . . ? O4 Zn1 O1 Tb1 -65.5(3) 4_566 . . . ? N1 Zn1 O1 Tb1 -156.7(3) . . . . ? N3 Zn1 O1 Tb1 110.7(3) 2_556 . . . ? N2 Zn1 O1 Tb1 11.7(3) 4_566 . . . ? O3 Tb1 O1 C1 145.8(4) 3_667 . . . ? O7 Tb1 O1 C1 -136.1(2) 2_647 . . . ? O5 Tb1 O1 C1 77.3(2) . . . . ? O2W Tb1 O1 C1 151.3(2) . . . . ? O1W Tb1 O1 C1 -66.3(2) . . . . ? O2 Tb1 O1 C1 -0.9(3) 3_667 . . . ? O2 Tb1 O1 C1 7.6(2) . . . . ? O3 Tb1 O1 Zn1 -41.2(6) 3_667 . . . ? O7 Tb1 O1 Zn1 36.9(3) 2_647 . . . ? O5 Tb1 O1 Zn1 -109.7(3) . . . . ? O2W Tb1 O1 Zn1 -35.7(3) . . . . ? O1W Tb1 O1 Zn1 106.7(3) . . . . ? O2 Tb1 O1 Zn1 172.1(2) 3_667 . . . ? O2 Tb1 O1 Zn1 -179.4(3) . . . . ? O4 Zn1 N1 C5 95.1(4) 4_566 . . . ? N3 Zn1 N1 C5 -95.1(4) 2_556 . . . ? O3W Zn1 N1 C5 2.8(4) . . . . ? N2 Zn1 N1 C5 121.6(6) 4_566 . . . ? O1 Zn1 N1 C5 -178.6(4) . . . . ? O4 Zn1 N1 C2 -101.8(3) 4_566 . . . ? N3 Zn1 N1 C2 68.0(3) 2_556 . . . ? O3W Zn1 N1 C2 165.9(3) . . . . ? N2 Zn1 N1 C2 -75.4(6) 4_566 . . . ? O1 Zn1 N1 C2 -15.6(3) . . . . ? C2 N1 C5 N2 -0.6(5) . . . . ? Zn1 N1 C5 N2 163.4(3) . . . . ? C2 N1 C5 C6 175.0(4) . . . . ? Zn1 N1 C5 C6 -20.9(7) . . . . ? C5 N1 C2 C3 0.4(4) . . . . ? Zn1 N1 C2 C3 -168.4(3) . . . . ? C5 N1 C2 C1 -176.5(3) . . . . ? Zn1 N1 C2 C1 14.8(4) . . . . ? Zn1 O1 C1 O2 169.8(3) . . . . ? Tb1 O1 C1 O2 -14.0(4) . . . . ? Zn1 O1 C1 C2 -13.2(4) . . . . ? Tb1 O1 C1 C2 163.0(3) . . . . ? N1 C2 C1 O2 176.6(4) . . . . ? C3 C2 C1 O2 0.8(7) . . . . ? N1 C2 C1 O1 -0.2(5) . . . . ? C3 C2 C1 O1 -176.0(4) . . . . ? N1 C5 C6 C8 132.0(4) . . . . ? N2 C5 C6 C8 -52.8(6) . . . . ? N1 C5 C6 C7 -50.9(6) . . . . ? N2 C5 C6 C7 124.3(5) . . . . ? N1 C5 N2 C3 0.6(5) . . . . ? C6 C5 N2 C3 -175.0(4) . . . . ? N1 C5 N2 Zn1 175.0(3) . . . 4_565 ? C6 C5 N2 Zn1 -0.6(7) . . . 4_565 ? Zn1 O4 C4 O3 169.9(3) 4_565 . . . ? Zn1 O4 C4 C3 -9.6(5) 4_565 . . . ? C5 N2 C3 C2 -0.3(4) . . . . ? Zn1 N2 C3 C2 -176.7(3) 4_565 . . . ? C5 N2 C3 C4 179.3(3) . . . . ? Zn1 N2 C3 C4 2.8(4) 4_565 . . . ? N1 C2 C3 N2 -0.1(5) . . . . ? C1 C2 C3 N2 176.0(4) . . . . ? N1 C2 C3 C4 -179.5(4) . . . . ? C1 C2 C3 C4 -3.4(8) . . . . ? O3 C4 C3 N2 -175.1(4) . . . . ? O4 C4 C3 N2 4.5(6) . . . . ? O3 C4 C3 C2 4.3(7) . . . . ? O4 C4 C3 C2 -176.1(4) . . . . ? O1 C1 O2 Tb1 163.0(3) . . . 3_667 ? C2 C1 O2 Tb1 -13.8(8) . . . 3_667 ? O1 C1 O2 Tb1 13.0(4) . . . . ? C2 C1 O2 Tb1 -163.7(3) . . . . ? O3 Tb1 O2 C1 -173.2(2) 3_667 . . . ? O7 Tb1 O2 C1 48.3(3) 2_647 . . . ? O5 Tb1 O2 C1 -109.9(2) . . . . ? O2W Tb1 O2 C1 -48.7(3) . . . . ? O1W Tb1 O2 C1 82.5(2) . . . . ? O2 Tb1 O2 C1 164.0(3) 3_667 . . . ? O1 Tb1 O2 C1 -7.5(2) . . . . ? O3 Tb1 O2 Tb1 22.8(2) 3_667 . . 3_667 ? O7 Tb1 O2 Tb1 -115.68(15) 2_647 . . 3_667 ? O5 Tb1 O2 Tb1 86.10(13) . . . 3_667 ? O2W Tb1 O2 Tb1 147.34(12) . . . 3_667 ? O1W Tb1 O2 Tb1 -81.45(13) . . . 3_667 ? O2 Tb1 O2 Tb1 0.0 3_667 . . 3_667 ? O1 Tb1 O2 Tb1 -171.50(18) . . . 3_667 ? O3 Tb1 O5 S1 -56.1(4) 3_667 . . . ? O7 Tb1 O5 S1 8.3(5) 2_647 . . . ? O2W Tb1 O5 S1 33.3(3) . . . . ? O1W Tb1 O5 S1 179.2(3) . . . . ? O2 Tb1 O5 S1 -133.2(4) 3_667 . . . ? O1 Tb1 O5 S1 110.6(4) . . . . ? O2 Tb1 O5 S1 160.2(4) . . . . ? Tb1 O7 S1 O6 74.2(4) 2_657 . . . ? Tb1 O7 S1 O8 -50.1(4) 2_657 . . . ? Tb1 O7 S1 O5 -168.4(3) 2_657 . . . ? Tb1 O5 S1 O6 -158.8(4) . . . . ? Tb1 O5 S1 O8 -37.7(4) . . . . ? Tb1 O5 S1 O7 81.6(4) . . . . ? C9 N3 C10 C8 2.6(6) . . . . ? Zn1 N3 C10 C8 -170.7(3) 2_546 . . . ? C10 N3 C9 C7 -2.5(7) . . . . ? Zn1 N3 C9 C7 171.1(4) 2_546 . . . ? N3 C10 C8 C6 -0.7(7) . . . . ? C7 C6 C8 C10 -1.4(6) . . . . ? C5 C6 C8 C10 175.7(4) . . . . ? N3 C9 C7 C6 0.5(7) . . . . ? C8 C6 C7 C9 1.4(6) . . . . ? C5 C6 C7 C9 -175.8(4) . . . . ? O4 C4 O3 Tb1 -163.4(6) . . . 3_667 ? C3 C4 O3 Tb1 16.2(11) . . . 3_667 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.755 _refine_diff_density_min -1.200 _refine_diff_density_rms 0.145 ####################################################################