# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Loiseau, Thierry' _publ_contact_author_email thierry.loiseau@ensc-lille.fr _publ_section_title ; Chain-like and dinuclear coordination polymers in lanthanide (Nd, Eu) oxochloride complexes with 2,2':6',2''-terpyridine: synthesis, XRD structure and magnetic property ; loop_ _publ_author_name J.Lhoste A.Perez-Campos N.Henry T.Loiseau P.Rabu F.Abraham # Attachment '- 1_Ndterpytetra.cif' data_apc2142 _database_code_depnum_ccdc_archive 'CCDC 818761' #TrackingRef '- 1_Ndterpytetra.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(Nd 3+). (C15 N3 H11). 5(Cl 1-). 1(OH 1-). 1(H2 O)' _chemical_formula_sum 'C15 H14 Cl5 N3 Nd2 O2' _chemical_formula_weight 734.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'C 1 2/m 1' _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.8993(5) _cell_length_b 20.8772(8) _cell_length_c 8.5239(3) _cell_angle_alpha 90.00 _cell_angle_beta 123.235(2) _cell_angle_gamma 90.00 _cell_volume 2068.87(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6172 _cell_measurement_theta_min 2.587 _cell_measurement_theta_max 31.203 _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 5.625 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4383 _exptl_absorpt_correction_T_max 0.7562 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; 'SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, Gottingen Germany (2006).' ; _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_reflns_number 21999 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 31.58 _reflns_number_total 3560 _reflns_number_gt 2856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SMART/SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0610P)^2^+3.7384P] 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 SHELXL _refine_ls_extinction_coef 0.00198(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3560 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.1145 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.198 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.002 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 Nd1 Nd 0.30677(3) 0.0000 1.33861(4) 0.02092(11) Uani 1 2 d S . . Nd2 Nd 0.0000 0.090555(15) 1.0000 0.01920(11) Uani 1 2 d S . . Cl3 Cl 0.09883(14) 0.0000 1.3517(2) 0.0265(3) Uani 1 2 d S . . Cl4 Cl 0.22328(10) 0.12781(5) 1.28471(16) 0.0273(2) Uani 1 1 d . . . Cl1 Cl 0.5000 0.08162(8) 1.5000 0.0327(4) Uani 1 2 d S . . Cl2 Cl 0.34891(17) 0.0000 1.0460(3) 0.0416(5) Uani 1 2 d S . . O1 O 0.1246(4) 0.0000 1.0366(6) 0.0194(8) Uani 1 2 d S . . O2 O 0.3761(5) 0.0000 1.6768(7) 0.0427(14) Uani 1 2 d S . . N1 N 0.0724(4) 0.1459(2) 0.8131(6) 0.0267(8) Uani 1 1 d . . . N2 N 0.0000 0.2152(3) 1.0000 0.0237(11) Uani 1 2 d S . . C1 C 0.1137(5) 0.1117(3) 0.7309(7) 0.0328(11) Uani 1 1 d . . . H1 H 0.1050 0.0674 0.7259 0.039 Uiso 1 1 calc R . . C2 C 0.1691(6) 0.1388(3) 0.6525(9) 0.0437(15) Uani 1 1 d . . . H2 H 0.1983 0.1133 0.5986 0.052 Uiso 1 1 calc R . . C3 C 0.1795(7) 0.2034(4) 0.6563(10) 0.0546(19) Uani 1 1 d . . . H3 H 0.2150 0.2228 0.6026 0.066 Uiso 1 1 calc R . . C4 C 0.1381(7) 0.2399(3) 0.7385(10) 0.0520(18) Uani 1 1 d . . . H4 H 0.1457 0.2842 0.7426 0.062 Uiso 1 1 calc R . . C5 C 0.0839(4) 0.2102(2) 0.8167(7) 0.0288(10) Uani 1 1 d . . . C6 C 0.0386(5) 0.2482(2) 0.9097(7) 0.0306(10) Uani 1 1 d . . . C7 C 0.0369(7) 0.3149(3) 0.9043(11) 0.0523(17) Uani 1 1 d . . . H7 H 0.0607 0.3369 0.8363 0.063 Uiso 1 1 calc R . . C8 C 0.0000 0.3474(5) 1.0000 0.063(3) Uani 1 2 d S . . H8 H 0.0000 0.3919 1.0000 0.075 Uiso 1 2 calc SR . . 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 Nd1 0.01687(19) 0.02049(19) 0.02503(18) 0.000 0.01124(14) 0.000 Nd2 0.01827(19) 0.01501(17) 0.02655(18) 0.000 0.01371(14) 0.000 Cl3 0.0244(8) 0.0290(8) 0.0307(7) 0.000 0.0180(6) 0.000 Cl4 0.0225(6) 0.0201(5) 0.0358(6) -0.0001(4) 0.0137(5) -0.0023(4) Cl1 0.0212(8) 0.0251(8) 0.0475(10) 0.000 0.0160(7) 0.000 Cl2 0.0287(10) 0.0679(14) 0.0335(8) 0.000 0.0205(8) 0.000 O1 0.021(2) 0.017(2) 0.0231(19) 0.000 0.0133(17) 0.000 O2 0.027(3) 0.071(4) 0.031(3) 0.000 0.016(2) 0.000 N1 0.030(2) 0.025(2) 0.0269(18) 0.0006(15) 0.0172(17) -0.0054(16) N2 0.022(3) 0.016(2) 0.029(3) 0.000 0.012(2) 0.000 C1 0.041(3) 0.030(3) 0.033(2) -0.004(2) 0.024(2) -0.006(2) C2 0.054(4) 0.049(4) 0.045(3) -0.009(3) 0.038(3) -0.016(3) C3 0.075(5) 0.051(4) 0.064(4) -0.006(3) 0.054(4) -0.023(4) C4 0.079(5) 0.035(3) 0.068(4) -0.006(3) 0.056(4) -0.026(3) C5 0.032(3) 0.024(2) 0.032(2) -0.0017(19) 0.019(2) -0.009(2) C6 0.034(3) 0.019(2) 0.037(2) 0.0021(19) 0.019(2) -0.003(2) C7 0.074(5) 0.020(3) 0.077(5) 0.008(3) 0.051(4) -0.002(3) C8 0.089(9) 0.019(4) 0.099(9) 0.000 0.063(7) 0.000 _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 Nd1 O1 2.428(4) . ? Nd1 O2 2.489(5) . ? Nd1 Cl1 2.8213(11) . ? Nd1 Cl1 2.8213(11) 5_658 ? Nd1 Cl4 2.8449(12) . ? Nd1 Cl4 2.8450(12) 6 ? Nd1 Cl2 2.8576(18) . ? Nd1 Cl3 2.9529(16) . ? Nd1 Nd2 4.0738(4) 5_557 ? Nd1 Nd2 4.0738(4) . ? Nd2 O1 2.466(3) . ? Nd2 O1 2.466(3) 5_557 ? Nd2 N1 2.577(4) . ? Nd2 N1 2.577(4) 2_557 ? Nd2 N2 2.601(6) . ? Nd2 Cl4 2.8054(12) . ? Nd2 Cl4 2.8054(12) 2_557 ? Nd2 Cl3 3.1520(13) 5_557 ? Nd2 Cl3 3.1520(13) . ? Nd2 Nd2 3.7811(6) 5_557 ? Nd2 Nd1 4.0738(4) 5_557 ? Cl3 Nd2 3.1520(13) 5_557 ? Cl1 Nd1 2.8213(11) 5_658 ? O1 Nd2 2.466(3) 5_557 ? N1 C1 1.331(7) . ? N1 C5 1.350(6) . ? N2 C6 1.345(6) 2_557 ? N2 C6 1.345(6) . ? C1 C2 1.387(7) . ? C1 H1 0.9300 . ? C2 C3 1.354(10) . ? C2 H2 0.9300 . ? C3 C4 1.358(10) . ? C3 H3 0.9300 . ? C4 C5 1.395(7) . ? C4 H4 0.9300 . ? C5 C6 1.483(7) . ? C6 C7 1.395(8) . ? C7 C8 1.359(8) . ? C7 H7 0.9300 . ? C8 C7 1.359(9) 2_557 ? C8 H8 0.9300 . ? 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 Nd1 O2 138.16(16) . . ? O1 Nd1 Cl1 132.68(6) . . ? O2 Nd1 Cl1 76.97(10) . . ? O1 Nd1 Cl1 132.68(6) . 5_658 ? O2 Nd1 Cl1 76.97(10) . 5_658 ? Cl1 Nd1 Cl1 74.32(6) . 5_658 ? O1 Nd1 Cl4 74.50(3) . . ? O2 Nd1 Cl4 92.97(5) . . ? Cl1 Nd1 Cl4 72.98(4) . . ? Cl1 Nd1 Cl4 147.17(4) 5_658 . ? O1 Nd1 Cl4 74.50(3) . 6 ? O2 Nd1 Cl4 92.97(5) . 6 ? Cl1 Nd1 Cl4 147.17(4) . 6 ? Cl1 Nd1 Cl4 72.98(4) 5_658 6 ? Cl4 Nd1 Cl4 139.42(5) . 6 ? O1 Nd1 Cl2 70.60(11) . . ? O2 Nd1 Cl2 151.24(14) . . ? Cl1 Nd1 Cl2 80.20(3) . . ? Cl1 Nd1 Cl2 80.20(3) 5_658 . ? Cl4 Nd1 Cl2 96.87(3) . . ? Cl4 Nd1 Cl2 96.87(3) 6 . ? O1 Nd1 Cl3 64.32(10) . . ? O2 Nd1 Cl3 73.84(13) . . ? Cl1 Nd1 Cl3 132.18(3) . . ? Cl1 Nd1 Cl3 132.18(3) 5_658 . ? Cl4 Nd1 Cl3 71.64(3) . . ? Cl4 Nd1 Cl3 71.64(3) 6 . ? Cl2 Nd1 Cl3 134.92(5) . . ? O1 Nd1 Nd2 33.94(6) . 5_557 ? O2 Nd1 Nd2 114.27(11) . 5_557 ? Cl1 Nd1 Nd2 166.60(2) . 5_557 ? Cl1 Nd1 Nd2 114.34(3) 5_658 5_557 ? Cl4 Nd1 Nd2 98.33(3) . 5_557 ? Cl4 Nd1 Nd2 43.48(2) 6 5_557 ? Cl2 Nd1 Nd2 90.99(4) . 5_557 ? Cl3 Nd1 Nd2 50.26(3) . 5_557 ? O1 Nd1 Nd2 33.94(5) . . ? O2 Nd1 Nd2 114.27(11) . . ? Cl1 Nd1 Nd2 114.34(3) . . ? Cl1 Nd1 Nd2 166.60(2) 5_658 . ? Cl4 Nd1 Nd2 43.48(2) . . ? Cl4 Nd1 Nd2 98.33(3) 6 . ? Cl2 Nd1 Nd2 90.99(4) . . ? Cl3 Nd1 Nd2 50.26(3) . . ? Nd2 Nd1 Nd2 55.301(9) 5_557 . ? O1 Nd2 O1 79.87(16) . 5_557 ? O1 Nd2 N1 86.37(13) . . ? O1 Nd2 N1 138.66(13) 5_557 . ? O1 Nd2 N1 138.66(13) . 2_557 ? O1 Nd2 N1 86.37(13) 5_557 2_557 ? N1 Nd2 N1 126.72(19) . 2_557 ? O1 Nd2 N2 140.06(8) . . ? O1 Nd2 N2 140.06(8) 5_557 . ? N1 Nd2 N2 63.36(9) . . ? N1 Nd2 N2 63.36(10) 2_557 . ? O1 Nd2 Cl4 74.69(9) . . ? O1 Nd2 Cl4 133.58(10) 5_557 . ? N1 Nd2 Cl4 77.81(10) . . ? N1 Nd2 Cl4 87.85(10) 2_557 . ? N2 Nd2 Cl4 73.90(2) . . ? O1 Nd2 Cl4 133.58(10) . 2_557 ? O1 Nd2 Cl4 74.69(9) 5_557 2_557 ? N1 Nd2 Cl4 87.85(10) . 2_557 ? N1 Nd2 Cl4 77.81(10) 2_557 2_557 ? N2 Nd2 Cl4 73.90(2) . 2_557 ? Cl4 Nd2 Cl4 147.80(5) . 2_557 ? O1 Nd2 Cl3 64.54(10) . 5_557 ? O1 Nd2 Cl3 60.67(9) 5_557 5_557 ? N1 Nd2 Cl3 78.19(9) . 5_557 ? N1 Nd2 Cl3 137.95(10) 2_557 5_557 ? N2 Nd2 Cl3 126.855(18) . 5_557 ? Cl4 Nd2 Cl3 133.47(4) . 5_557 ? Cl4 Nd2 Cl3 69.19(4) 2_557 5_557 ? O1 Nd2 Cl3 60.67(9) . . ? O1 Nd2 Cl3 64.54(10) 5_557 . ? N1 Nd2 Cl3 137.95(10) . . ? N1 Nd2 Cl3 78.19(9) 2_557 . ? N2 Nd2 Cl3 126.855(18) . . ? Cl4 Nd2 Cl3 69.19(4) . . ? Cl4 Nd2 Cl3 133.47(4) 2_557 . ? Cl3 Nd2 Cl3 106.29(4) 5_557 . ? O1 Nd2 Nd2 39.94(8) . 5_557 ? O1 Nd2 Nd2 39.94(8) 5_557 5_557 ? N1 Nd2 Nd2 116.64(9) . 5_557 ? N1 Nd2 Nd2 116.64(10) 2_557 5_557 ? N2 Nd2 Nd2 180.0 . 5_557 ? Cl4 Nd2 Nd2 106.10(2) . 5_557 ? Cl4 Nd2 Nd2 106.10(2) 2_557 5_557 ? Cl3 Nd2 Nd2 53.145(18) 5_557 5_557 ? Cl3 Nd2 Nd2 53.145(18) . 5_557 ? O1 Nd2 Nd1 33.35(9) . . ? O1 Nd2 Nd1 97.10(9) 5_557 . ? N1 Nd2 Nd1 91.97(10) . . ? N1 Nd2 Nd1 112.44(9) 2_557 . ? N2 Nd2 Nd1 117.650(5) . . ? Cl4 Nd2 Nd1 44.25(2) . . ? Cl4 Nd2 Nd1 166.81(3) 2_557 . ? Cl3 Nd2 Nd1 97.87(3) 5_557 . ? Cl3 Nd2 Nd1 46.09(3) . . ? Nd2 Nd2 Nd1 62.350(5) 5_557 . ? O1 Nd2 Nd1 97.10(9) . 5_557 ? O1 Nd2 Nd1 33.35(9) 5_557 5_557 ? N1 Nd2 Nd1 112.44(9) . 5_557 ? N1 Nd2 Nd1 91.97(10) 2_557 5_557 ? N2 Nd2 Nd1 117.650(5) . 5_557 ? Cl4 Nd2 Nd1 166.81(3) . 5_557 ? Cl4 Nd2 Nd1 44.25(2) 2_557 5_557 ? Cl3 Nd2 Nd1 46.09(3) 5_557 5_557 ? Cl3 Nd2 Nd1 97.87(3) . 5_557 ? Nd2 Nd2 Nd1 62.350(5) 5_557 5_557 ? Nd1 Nd2 Nd1 124.699(9) . 5_557 ? Nd1 Cl3 Nd2 83.65(3) . 5_557 ? Nd1 Cl3 Nd2 83.65(3) . . ? Nd2 Cl3 Nd2 73.71(4) 5_557 . ? Nd2 Cl4 Nd1 92.27(3) . . ? Nd1 Cl1 Nd1 105.69(6) 5_658 . ? Nd1 O1 Nd2 112.71(12) . 5_557 ? Nd1 O1 Nd2 112.71(12) . . ? Nd2 O1 Nd2 100.13(16) 5_557 . ? C1 N1 C5 117.8(4) . . ? C1 N1 Nd2 120.8(3) . . ? C5 N1 Nd2 120.9(3) . . ? C6 N2 C6 118.4(6) 2_557 . ? C6 N2 Nd2 120.8(3) 2_557 . ? C6 N2 Nd2 120.8(3) . . ? N1 C1 C2 123.2(5) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 118.4(6) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 120.1(6) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 119.3(6) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.3(5) . . ? N1 C5 C6 117.6(4) . . ? C4 C5 C6 121.0(5) . . ? N2 C6 C7 121.8(5) . . ? N2 C6 C5 116.8(4) . . ? C7 C6 C5 121.4(5) . . ? C8 C7 C6 118.9(6) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C7 C8 C7 120.2(9) 2_557 . ? C7 C8 H8 119.9 2_557 . ? C7 C8 H8 119.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 31.58 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.251 _refine_diff_density_min -1.201 _refine_diff_density_rms 0.337 # Attachment '- 2_Euterpytetra.cif' data_eutetraes _database_code_depnum_ccdc_archive 'CCDC 818762' #TrackingRef '- 2_Euterpytetra.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(Eu 3+). (C15 N3 H11). 5(Cl 1-). 1(OH 1-). 1(H2 O)' _chemical_formula_sum 'C15 H14 Cl5 Eu2 N3 O2' _chemical_formula_weight 746.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'C 1 2/m 1' _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.7211(8) _cell_length_b 20.7195(13) _cell_length_c 8.5408(5) _cell_angle_alpha 90.00 _cell_angle_beta 123.305(2) _cell_angle_gamma 90.00 _cell_volume 2029.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5885 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 26.20 _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 6.799 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4526 _exptl_absorpt_correction_T_max 0.8179 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; 'SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, G ttingen Germany (2006).' ; _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_reflns_number 18059 _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 26.30 _reflns_number_total 2105 _reflns_number_gt 1625 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SMART/SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0767P)^2^+8.8734P] 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 2105 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.1419 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 1.227 _refine_ls_restrained_S_all 1.227 _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 0.30577(6) 0.0000 0.33677(9) 0.0239(2) Uani 1 2 d S . . Eu2 Eu 0.0000 0.09045(3) 0.0000 0.0214(2) Uani 1 2 d S . . Cl3 Cl 0.0991(3) 0.0000 0.3512(5) 0.0301(8) Uani 1 2 d S . . Cl4 Cl 0.2228(2) 0.12715(12) 0.2818(3) 0.0291(5) Uani 1 1 d . . . Cl1 Cl 0.5000 0.08102(18) 0.5000 0.0363(8) Uani 1 2 d S . . Cl2 Cl 0.3504(3) 0.0000 0.0517(5) 0.0436(10) Uani 1 2 d S . . O1 O 0.1236(8) 0.0000 0.0372(11) 0.0216(19) Uani 1 2 d S . . O2 O 0.3728(9) 0.0000 0.6664(14) 0.043(3) Uani 1 2 d S . . N1 N 0.0732(7) 0.1437(4) -0.1842(10) 0.0274(18) Uani 1 1 d . . . N2 N 0.0000 0.2141(6) 0.0000 0.027(3) Uani 1 2 d S . . C1 C 0.1151(10) 0.1106(5) -0.2677(14) 0.034(2) Uani 1 1 d . . . H1 H 0.1071 0.0659 -0.2722 0.041 Uiso 1 1 calc R . . C2 C 0.1694(11) 0.1371(6) -0.3481(15) 0.042(3) Uani 1 1 d . . . H2 H 0.1984 0.1112 -0.4025 0.051 Uiso 1 1 calc R . . C3 C 0.1792(12) 0.2016(7) -0.3454(18) 0.055(4) Uani 1 1 d . . . H3 H 0.2149 0.2210 -0.3996 0.066 Uiso 1 1 calc R . . C4 C 0.1370(13) 0.2390(6) -0.2637(18) 0.052(3) Uani 1 1 d . . . H4 H 0.1434 0.2837 -0.2624 0.062 Uiso 1 1 calc R . . C5 C 0.0841(9) 0.2091(5) -0.1823(12) 0.029(2) Uani 1 1 d . . . C6 C 0.0395(9) 0.2474(5) -0.0900(13) 0.029(2) Uani 1 1 d . . . C7 C 0.0379(12) 0.3146(6) -0.0955(19) 0.051(3) Uani 1 1 d . . . H7 H 0.0622 0.3366 -0.1632 0.061 Uiso 1 1 calc R . . C8 C 0.0000 0.3480(8) 0.0000 0.057(5) Uani 1 2 d S . . H8 H 0.0000 0.3929 0.0000 0.068 Uiso 1 2 calc SR . . 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 0.0233(4) 0.0246(4) 0.0238(4) 0.000 0.0130(3) 0.000 Eu2 0.0239(4) 0.0195(4) 0.0242(4) 0.000 0.0153(3) 0.000 Cl3 0.0312(19) 0.036(2) 0.0293(17) 0.000 0.0202(15) 0.000 Cl4 0.0278(13) 0.0258(12) 0.0316(12) 0.0010(10) 0.0149(10) -0.0014(10) Cl1 0.032(2) 0.0301(19) 0.042(2) 0.000 0.0174(16) 0.000 Cl2 0.034(2) 0.070(3) 0.0315(19) 0.000 0.0210(16) 0.000 O1 0.027(5) 0.022(5) 0.017(4) 0.000 0.013(4) 0.000 O2 0.026(6) 0.065(8) 0.033(6) 0.000 0.013(5) 0.000 N1 0.030(5) 0.033(5) 0.018(4) 0.000(3) 0.012(3) -0.005(4) N2 0.021(6) 0.033(7) 0.020(5) 0.000 0.007(5) 0.000 C1 0.049(7) 0.028(6) 0.030(5) -0.003(4) 0.024(5) -0.004(5) C2 0.049(7) 0.056(8) 0.039(6) -0.016(5) 0.035(5) -0.022(6) C3 0.069(10) 0.056(9) 0.059(8) -0.003(7) 0.046(8) -0.023(7) C4 0.083(10) 0.038(7) 0.055(7) -0.009(6) 0.051(7) -0.027(7) C5 0.035(6) 0.029(6) 0.023(5) -0.004(4) 0.016(4) -0.009(5) C6 0.035(6) 0.022(5) 0.027(5) 0.000(4) 0.015(4) -0.008(4) C7 0.061(9) 0.038(7) 0.063(8) 0.005(6) 0.039(7) -0.002(6) C8 0.085(15) 0.018(9) 0.077(13) 0.000 0.052(12) 0.000 _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 2.403(9) . ? Eu1 O2 2.435(10) . ? Eu1 Cl1 2.790(2) 5_656 ? Eu1 Cl1 2.790(2) . ? Eu1 Cl4 2.805(2) . ? Eu1 Cl4 2.805(2) 6 ? Eu1 Cl2 2.818(4) . ? Eu1 Cl3 2.906(3) . ? Eu1 Eu2 4.0169(7) 5 ? Eu1 Eu2 4.0169(7) . ? Eu1 Eu1 4.4568(13) 5_656 ? Eu2 O1 2.428(6) . ? Eu2 O1 2.428(6) 5 ? Eu2 N1 2.538(8) . ? Eu2 N1 2.538(8) 2 ? Eu2 N2 2.562(13) . ? Eu2 Cl4 2.763(2) . ? Eu2 Cl4 2.763(2) 2 ? Eu2 Cl3 3.143(3) . ? Eu2 Cl3 3.143(3) 5 ? Eu2 Eu2 3.7483(13) 5 ? Eu2 Eu1 4.0169(7) 5 ? Cl3 Eu2 3.143(3) 5 ? Cl1 Eu1 2.790(2) 5_656 ? O1 Eu2 2.428(6) 5 ? N1 C1 1.326(13) . ? N1 C5 1.362(13) . ? N2 C6 1.348(11) . ? N2 C6 1.348(11) 2 ? C1 C2 1.375(15) . ? C1 H1 0.9300 . ? C2 C3 1.343(19) . ? C2 H2 0.9300 . ? C3 C4 1.366(19) . ? C3 H3 0.9300 . ? C4 C5 1.395(14) . ? C4 H4 0.9300 . ? C5 C6 1.467(14) . ? C6 C7 1.394(16) . ? C7 C8 1.371(15) . ? C7 H7 0.9300 . ? C8 C7 1.371(16) 2 ? C8 H8 0.9300 . ? 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 O2 138.0(3) . . ? O1 Eu1 Cl1 133.01(12) . 5_656 ? O2 Eu1 Cl1 76.8(2) . 5_656 ? O1 Eu1 Cl1 133.01(12) . . ? O2 Eu1 Cl1 76.8(2) . . ? Cl1 Eu1 Cl1 73.98(12) 5_656 . ? O1 Eu1 Cl4 74.48(7) . . ? O2 Eu1 Cl4 93.12(10) . . ? Cl1 Eu1 Cl4 146.85(8) 5_656 . ? Cl1 Eu1 Cl4 72.97(8) . . ? O1 Eu1 Cl4 74.48(7) . 6 ? O2 Eu1 Cl4 93.12(10) . 6 ? Cl1 Eu1 Cl4 72.97(8) 5_656 6 ? Cl1 Eu1 Cl4 146.85(8) . 6 ? Cl4 Eu1 Cl4 139.79(10) . 6 ? O1 Eu1 Cl2 70.9(2) . . ? O2 Eu1 Cl2 151.1(3) . . ? Cl1 Eu1 Cl2 80.25(7) 5_656 . ? Cl1 Eu1 Cl2 80.25(7) . . ? Cl4 Eu1 Cl2 96.67(6) . . ? Cl4 Eu1 Cl2 96.67(6) 6 . ? O1 Eu1 Cl3 64.9(2) . . ? O2 Eu1 Cl3 73.1(3) . . ? Cl1 Eu1 Cl3 131.73(6) 5_656 . ? Cl1 Eu1 Cl3 131.73(6) . . ? Cl4 Eu1 Cl3 72.01(5) . . ? Cl4 Eu1 Cl3 72.01(5) 6 . ? Cl2 Eu1 Cl3 135.79(11) . . ? O1 Eu1 Eu2 33.95(11) . 5 ? O2 Eu1 Eu2 114.3(2) . 5 ? Cl1 Eu1 Eu2 114.37(6) 5_656 5 ? Cl1 Eu1 Eu2 166.93(4) . 5 ? Cl4 Eu1 Eu2 98.62(5) . 5 ? Cl4 Eu1 Eu2 43.42(5) 6 5 ? Cl2 Eu1 Eu2 91.05(7) . 5 ? Cl3 Eu1 Eu2 50.97(5) . 5 ? O1 Eu1 Eu2 33.95(11) . . ? O2 Eu1 Eu2 114.3(2) . . ? Cl1 Eu1 Eu2 166.93(4) 5_656 . ? Cl1 Eu1 Eu2 114.37(6) . . ? Cl4 Eu1 Eu2 43.42(5) . . ? Cl4 Eu1 Eu2 98.62(5) 6 . ? Cl2 Eu1 Eu2 91.05(7) . . ? Cl3 Eu1 Eu2 50.97(5) . . ? Eu2 Eu1 Eu2 55.624(19) 5 . ? O1 Eu1 Eu1 148.6(2) . 5_656 ? O2 Eu1 Eu1 73.4(2) . 5_656 ? Cl1 Eu1 Eu1 36.99(6) 5_656 5_656 ? Cl1 Eu1 Eu1 36.99(6) . 5_656 ? Cl4 Eu1 Eu1 109.93(5) . 5_656 ? Cl4 Eu1 Eu1 109.93(5) 6 5_656 ? Cl2 Eu1 Eu1 77.76(8) . 5_656 ? Cl3 Eu1 Eu1 146.44(7) . 5_656 ? Eu2 Eu1 Eu1 150.236(12) 5 5_656 ? Eu2 Eu1 Eu1 150.236(12) . 5_656 ? O1 Eu2 O1 79.0(3) . 5 ? O1 Eu2 N1 86.0(3) . . ? O1 Eu2 N1 137.8(3) 5 . ? O1 Eu2 N1 137.8(3) . 2 ? O1 Eu2 N1 86.0(3) 5 2 ? N1 Eu2 N1 128.4(4) . 2 ? O1 Eu2 N2 140.52(16) . . ? O1 Eu2 N2 140.52(16) 5 . ? N1 Eu2 N2 64.22(19) . . ? N1 Eu2 N2 64.22(19) 2 . ? O1 Eu2 Cl4 74.90(18) . . ? O1 Eu2 Cl4 133.26(19) 5 . ? N1 Eu2 Cl4 78.18(18) . . ? N1 Eu2 Cl4 88.02(19) 2 . ? N2 Eu2 Cl4 74.03(5) . . ? O1 Eu2 Cl4 133.26(19) . 2 ? O1 Eu2 Cl4 74.90(18) 5 2 ? N1 Eu2 Cl4 88.02(19) . 2 ? N1 Eu2 Cl4 78.18(18) 2 2 ? N2 Eu2 Cl4 74.03(5) . 2 ? Cl4 Eu2 Cl4 148.06(11) . 2 ? O1 Eu2 Cl3 60.66(18) . . ? O1 Eu2 Cl3 64.51(19) 5 . ? N1 Eu2 Cl3 137.7(2) . . ? N1 Eu2 Cl3 77.21(18) 2 . ? N2 Eu2 Cl3 126.60(4) . . ? Cl4 Eu2 Cl3 68.96(7) . . ? Cl4 Eu2 Cl3 133.41(8) 2 . ? O1 Eu2 Cl3 64.51(19) . 5 ? O1 Eu2 Cl3 60.66(18) 5 5 ? N1 Eu2 Cl3 77.21(18) . 5 ? N1 Eu2 Cl3 137.7(2) 2 5 ? N2 Eu2 Cl3 126.60(4) . 5 ? Cl4 Eu2 Cl3 133.41(8) . 5 ? Cl4 Eu2 Cl3 68.96(7) 2 5 ? Cl3 Eu2 Cl3 106.79(7) . 5 ? O1 Eu2 Eu2 39.48(16) . 5 ? O1 Eu2 Eu2 39.48(16) 5 5 ? N1 Eu2 Eu2 115.78(19) . 5 ? N1 Eu2 Eu2 115.78(19) 2 5 ? N2 Eu2 Eu2 180.0 . 5 ? Cl4 Eu2 Eu2 105.97(5) . 5 ? Cl4 Eu2 Eu2 105.97(5) 2 5 ? Cl3 Eu2 Eu2 53.40(4) . 5 ? Cl3 Eu2 Eu2 53.40(4) 5 5 ? O1 Eu2 Eu1 96.50(17) . 5 ? O1 Eu2 Eu1 33.54(19) 5 5 ? N1 Eu2 Eu1 111.86(17) . 5 ? N1 Eu2 Eu1 91.92(19) 2 5 ? N2 Eu2 Eu1 117.812(9) . 5 ? Cl4 Eu2 Eu1 166.66(5) . 5 ? Cl4 Eu2 Eu1 44.25(5) 2 5 ? Cl3 Eu2 Eu1 98.02(5) . 5 ? Cl3 Eu2 Eu1 45.90(6) 5 5 ? Eu2 Eu2 Eu1 62.188(9) 5 5 ? O1 Eu2 Eu1 33.54(18) . . ? O1 Eu2 Eu1 96.50(17) 5 . ? N1 Eu2 Eu1 91.92(19) . . ? N1 Eu2 Eu1 111.86(17) 2 . ? N2 Eu2 Eu1 117.812(9) . . ? Cl4 Eu2 Eu1 44.25(5) . . ? Cl4 Eu2 Eu1 166.66(5) 2 . ? Cl3 Eu2 Eu1 45.90(6) . . ? Cl3 Eu2 Eu1 98.02(5) 5 . ? Eu2 Eu2 Eu1 62.188(9) 5 . ? Eu1 Eu2 Eu1 124.376(19) 5 . ? Eu1 Cl3 Eu2 83.12(7) . 5 ? Eu1 Cl3 Eu2 83.12(7) . . ? Eu2 Cl3 Eu2 73.21(7) 5 . ? Eu2 Cl4 Eu1 92.33(7) . . ? Eu1 Cl1 Eu1 106.02(12) . 5_656 ? Eu1 O1 Eu2 112.5(2) . 5 ? Eu1 O1 Eu2 112.5(2) . . ? Eu2 O1 Eu2 101.0(3) 5 . ? C1 N1 C5 116.4(9) . . ? C1 N1 Eu2 123.0(7) . . ? C5 N1 Eu2 120.2(6) . . ? C6 N2 C6 118.6(13) . 2 ? C6 N2 Eu2 120.7(6) . . ? C6 N2 Eu2 120.7(6) 2 . ? N1 C1 C2 125.2(11) . . ? N1 C1 H1 117.4 . . ? C2 C1 H1 117.4 . . ? C3 C2 C1 117.7(11) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C2 C3 C4 120.4(11) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C5 119.1(12) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.2(10) . . ? N1 C5 C6 117.9(8) . . ? C4 C5 C6 120.8(10) . . ? N2 C6 C7 121.7(11) . . ? N2 C6 C5 116.6(9) . . ? C7 C6 C5 121.7(9) . . ? C8 C7 C6 119.3(12) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C7 119.3(17) 2 . ? C7 C8 H8 120.3 2 . ? C7 C8 H8 120.3 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.731 _refine_diff_density_min -1.819 _refine_diff_density_rms 0.342 # Attachment '- 3_Ndterpydim.cif' data_apc2142tercon _database_code_depnum_ccdc_archive 'CCDC 818763' #TrackingRef '- 3_Ndterpydim.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Nd 3+). (C15 N3 H11). 3(Cl 1-). 1(H2 O)' _chemical_formula_sum 'C15 H13 Cl3 N3 Nd O' _chemical_formula_weight 501.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7770(3) _cell_length_b 9.9885(3) _cell_length_c 10.2489(3) _cell_angle_alpha 94.5230(10) _cell_angle_beta 109.8560(10) _cell_angle_gamma 112.8540(10) _cell_volume 841.43(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9867 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 35.891 _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.985 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 3.567 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.543 _exptl_absorpt_correction_T_max 0.6858 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; 'SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, G ttingen Germany (2006).' ; _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_reflns_number 71980 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 33.14 _reflns_number_total 6395 _reflns_number_gt 6007 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SMART/SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0302P)^2^+0.1242P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6395 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0187 _refine_ls_R_factor_gt 0.0159 _refine_ls_wR_factor_ref 0.0570 _refine_ls_wR_factor_gt 0.0465 _refine_ls_goodness_of_fit_ref 1.256 _refine_ls_restrained_S_all 1.256 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.028606(9) 0.723683(9) 0.121762(8) 0.01952(3) Uani 1 1 d . . . Cl1 Cl 0.08448(6) 0.99570(5) 0.27625(5) 0.02940(8) Uani 1 1 d . . . Cl2 Cl -0.00875(7) 0.42944(5) 0.13866(5) 0.03624(11) Uani 1 1 d . . . Cl3 Cl -0.26014(6) 0.70982(6) -0.05988(6) 0.03886(11) Uani 1 1 d . . . N1 N 0.33469(19) 0.8026(2) 0.19050(17) 0.0294(3) Uani 1 1 d . . . N2 N 0.20590(17) 0.75024(16) 0.38801(14) 0.0216(2) Uani 1 1 d . . . N3 N -0.12462(18) 0.64219(17) 0.28812(16) 0.0255(3) Uani 1 1 d . . . C1 C 0.3963(3) 0.8295(3) 0.0907(2) 0.0378(4) Uani 1 1 d . . . C12 C -0.1147(3) 0.6621(3) 0.5261(2) 0.0346(4) Uani 1 1 d . . . C11 C -0.0397(2) 0.67336(19) 0.43074(18) 0.0245(3) Uani 1 1 d . . . C5 C 0.4385(2) 0.82822(19) 0.32621(19) 0.0243(3) Uani 1 1 d . . . C10 C 0.1367(2) 0.71778(19) 0.48241(18) 0.0238(3) Uani 1 1 d . . . C6 C 0.3668(2) 0.79225(18) 0.43293(18) 0.0233(3) Uani 1 1 d . . . C9 C 0.2262(3) 0.7230(2) 0.6235(2) 0.0318(4) Uani 1 1 d . . . C7 C 0.4626(2) 0.8008(2) 0.5732(2) 0.0312(4) Uani 1 1 d . . . C15 C -0.2868(2) 0.5893(2) 0.2392(2) 0.0324(4) Uani 1 1 d . . . C8 C 0.3900(3) 0.7642(2) 0.6681(2) 0.0340(4) Uani 1 1 d . . . C14 C -0.3694(3) 0.5702(3) 0.3279(3) 0.0372(4) Uani 1 1 d . . . C2 C 0.5601(3) 0.8812(3) 0.1214(3) 0.0407(5) Uani 1 1 d . . . C13 C -0.2813(3) 0.6103(3) 0.4732(3) 0.0396(5) Uani 1 1 d . . . C3 C 0.6659(3) 0.9104(3) 0.2609(3) 0.0384(4) Uani 1 1 d . . . O1 O 0.12132(19) 0.92129(17) -0.01114(17) 0.0308(3) Uani 1 1 d . . . C4 C 0.6051(2) 0.8845(2) 0.3642(2) 0.0329(4) Uani 1 1 d . . . H1 H 0.323(3) 0.811(3) -0.003(3) 0.041(7) Uiso 1 1 d . . . H2 H 0.601(4) 0.908(3) 0.051(3) 0.051(8) Uiso 1 1 d . . . H3 H 0.780(4) 0.947(3) 0.292(3) 0.049(8) Uiso 1 1 d . . . H4 H 0.673(3) 0.904(3) 0.461(3) 0.039(7) Uiso 1 1 d . . . H7 H 0.585(4) 0.835(3) 0.600(3) 0.044(7) Uiso 1 1 d . . . H8 H 0.456(3) 0.773(3) 0.757(3) 0.041(7) Uiso 1 1 d . . . H9 H 0.174(4) 0.696(3) 0.687(3) 0.041(7) Uiso 1 1 d . . . H12 H -0.054(4) 0.713(4) 0.623(4) 0.060(9) Uiso 1 1 d . . . H13 H -0.325(4) 0.610(3) 0.547(3) 0.049(8) Uiso 1 1 d . . . H14 H -0.480(4) 0.527(3) 0.293(3) 0.050(8) Uiso 1 1 d . . . H15 H -0.338(4) 0.572(3) 0.150(3) 0.041(8) Uiso 1 1 d . . . H1W H 0.060(4) 0.919(4) -0.089(4) 0.052(9) Uiso 1 1 d . . . H2W H 0.162(4) 1.007(4) 0.033(3) 0.046(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.02018(5) 0.02179(5) 0.01680(4) 0.00555(3) 0.00722(3) 0.00953(3) Cl1 0.0325(2) 0.02637(19) 0.02493(18) 0.00293(14) 0.00610(15) 0.01404(16) Cl2 0.0654(3) 0.0273(2) 0.02457(19) 0.01044(16) 0.0250(2) 0.0222(2) Cl3 0.0251(2) 0.0440(3) 0.0362(2) 0.0089(2) 0.00215(17) 0.01334(19) N1 0.0248(7) 0.0402(8) 0.0268(7) 0.0109(6) 0.0124(6) 0.0157(6) N2 0.0241(6) 0.0216(6) 0.0197(6) 0.0058(5) 0.0085(5) 0.0108(5) N3 0.0259(7) 0.0259(7) 0.0244(6) 0.0065(5) 0.0110(5) 0.0103(5) C1 0.0329(10) 0.0547(13) 0.0326(9) 0.0154(9) 0.0184(8) 0.0208(9) C12 0.0415(10) 0.0397(10) 0.0302(9) 0.0116(8) 0.0221(8) 0.0183(9) C11 0.0296(8) 0.0229(7) 0.0237(7) 0.0076(6) 0.0135(6) 0.0115(6) C5 0.0224(7) 0.0245(7) 0.0275(7) 0.0070(6) 0.0091(6) 0.0126(6) C10 0.0294(8) 0.0223(7) 0.0204(6) 0.0071(5) 0.0106(6) 0.0115(6) C6 0.0238(7) 0.0218(7) 0.0227(7) 0.0058(5) 0.0065(5) 0.0109(6) C9 0.0394(10) 0.0355(9) 0.0212(7) 0.0109(7) 0.0116(7) 0.0171(8) C7 0.0286(8) 0.0320(9) 0.0261(8) 0.0065(7) 0.0031(6) 0.0137(7) C15 0.0260(8) 0.0342(9) 0.0342(9) 0.0081(7) 0.0120(7) 0.0108(7) C8 0.0370(10) 0.0369(10) 0.0214(7) 0.0080(7) 0.0037(7) 0.0166(8) C14 0.0302(9) 0.0357(10) 0.0494(12) 0.0121(9) 0.0214(9) 0.0134(8) C2 0.0375(11) 0.0514(13) 0.0486(12) 0.0183(10) 0.0291(10) 0.0233(10) C13 0.0427(11) 0.0425(11) 0.0487(12) 0.0168(9) 0.0322(10) 0.0205(9) C3 0.0266(9) 0.0410(11) 0.0543(13) 0.0146(9) 0.0207(9) 0.0170(8) O1 0.0346(7) 0.0309(7) 0.0319(7) 0.0144(6) 0.0153(6) 0.0166(6) C4 0.0230(8) 0.0338(9) 0.0398(10) 0.0086(8) 0.0096(7) 0.0133(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 Nd1 O1 2.5388(14) . ? Nd1 N1 2.5924(16) . ? Nd1 N3 2.6116(15) . ? Nd1 N2 2.6147(14) . ? Nd1 Cl3 2.7459(5) . ? Nd1 Cl1 2.7873(4) . ? Nd1 Cl2 2.8444(5) . ? Nd1 Cl2 2.8765(4) 2_565 ? Cl2 Nd1 2.8765(4) 2_565 ? N1 C5 1.347(2) . ? N1 C1 1.349(3) . ? N2 C10 1.350(2) . ? N2 C6 1.351(2) . ? N3 C15 1.346(2) . ? N3 C11 1.351(2) . ? C1 C2 1.385(3) . ? C1 H1 0.94(3) . ? C12 C13 1.384(3) . ? C12 C11 1.394(3) . ? C12 H12 0.94(3) . ? C11 C10 1.483(3) . ? C5 C4 1.394(2) . ? C5 C6 1.485(3) . ? C10 C9 1.398(2) . ? C6 C7 1.398(2) . ? C9 C8 1.380(3) . ? C9 H9 0.95(3) . ? C7 C8 1.381(3) . ? C7 H7 1.03(3) . ? C15 C14 1.386(3) . ? C15 H15 0.85(3) . ? C8 H8 0.90(3) . ? C14 C13 1.374(4) . ? C14 H14 0.91(3) . ? C2 C3 1.376(4) . ? C2 H2 0.95(3) . ? C13 H13 0.99(3) . ? C3 C4 1.376(3) . ? C3 H3 0.95(3) . ? O1 H1W 0.81(3) . ? O1 H2W 0.81(3) . ? C4 H4 0.94(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nd1 N1 73.40(5) . . ? O1 Nd1 N3 144.87(5) . . ? N1 Nd1 N3 125.74(5) . . ? O1 Nd1 N2 121.60(5) . . ? N1 Nd1 N2 62.72(5) . . ? N3 Nd1 N2 63.32(5) . . ? O1 Nd1 Cl3 77.93(4) . . ? N1 Nd1 Cl3 149.79(4) . . ? N3 Nd1 Cl3 83.74(4) . . ? N2 Nd1 Cl3 144.49(3) . . ? O1 Nd1 Cl1 72.43(4) . . ? N1 Nd1 Cl1 93.35(4) . . ? N3 Nd1 Cl1 76.91(4) . . ? N2 Nd1 Cl1 73.69(3) . . ? Cl3 Nd1 Cl1 86.837(16) . . ? O1 Nd1 Cl2 141.08(4) . . ? N1 Nd1 Cl2 87.65(4) . . ? N3 Nd1 Cl2 73.46(4) . . ? N2 Nd1 Cl2 74.87(3) . . ? Cl3 Nd1 Cl2 109.606(17) . . ? Cl1 Nd1 Cl2 143.923(13) . . ? O1 Nd1 Cl2 73.20(4) . 2_565 ? N1 Nd1 Cl2 80.90(4) . 2_565 ? N3 Nd1 Cl2 133.57(3) . 2_565 ? N2 Nd1 Cl2 130.05(3) . 2_565 ? Cl3 Nd1 Cl2 81.956(18) . 2_565 ? Cl1 Nd1 Cl2 145.354(14) . 2_565 ? Cl2 Nd1 Cl2 70.376(14) . 2_565 ? Nd1 Cl2 Nd1 109.624(14) . 2_565 ? C5 N1 C1 117.88(17) . . ? C5 N1 Nd1 122.07(12) . . ? C1 N1 Nd1 119.89(13) . . ? C10 N2 C6 118.76(14) . . ? C10 N2 Nd1 120.20(11) . . ? C6 N2 Nd1 121.01(11) . . ? C15 N3 C11 117.82(16) . . ? C15 N3 Nd1 121.65(13) . . ? C11 N3 Nd1 119.81(11) . . ? N1 C1 C2 123.1(2) . . ? N1 C1 H1 117.4(18) . . ? C2 C1 H1 119.5(18) . . ? C13 C12 C11 119.3(2) . . ? C13 C12 H12 118(2) . . ? C11 C12 H12 121(2) . . ? N3 C11 C12 121.62(18) . . ? N3 C11 C10 117.40(15) . . ? C12 C11 C10 120.98(17) . . ? N1 C5 C4 121.55(18) . . ? N1 C5 C6 116.76(15) . . ? C4 C5 C6 121.69(17) . . ? N2 C10 C9 121.70(17) . . ? N2 C10 C11 117.68(15) . . ? C9 C10 C11 120.61(16) . . ? N2 C6 C7 122.00(17) . . ? N2 C6 C5 117.11(14) . . ? C7 C6 C5 120.89(16) . . ? C8 C9 C10 119.16(18) . . ? C8 C9 H9 120.8(18) . . ? C10 C9 H9 120.0(18) . . ? C8 C7 C6 118.82(18) . . ? C8 C7 H7 123.4(16) . . ? C6 C7 H7 117.8(17) . . ? N3 C15 C14 123.3(2) . . ? N3 C15 H15 117(2) . . ? C14 C15 H15 120(2) . . ? C9 C8 C7 119.53(18) . . ? C9 C8 H8 124.3(19) . . ? C7 C8 H8 116.1(19) . . ? C13 C14 C15 118.4(2) . . ? C13 C14 H14 119(2) . . ? C15 C14 H14 122(2) . . ? C3 C2 C1 118.7(2) . . ? C3 C2 H2 119.7(19) . . ? C1 C2 H2 121.2(19) . . ? C14 C13 C12 119.31(19) . . ? C14 C13 H13 126.0(18) . . ? C12 C13 H13 114.6(18) . . ? C4 C3 C2 118.94(19) . . ? C4 C3 H3 116.7(19) . . ? C2 C3 H3 124.3(19) . . ? Nd1 O1 H1W 121(2) . . ? Nd1 O1 H2W 116(2) . . ? H1W O1 H2W 105(3) . . ? C3 C4 C5 119.79(19) . . ? C3 C4 H4 121.9(18) . . ? C5 C4 H4 118.3(18) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.636 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.141 # Attachment '- 4_Euterpydim.cif' data_euterpy _database_code_depnum_ccdc_archive 'CCDC 818764' #TrackingRef '- 4_Euterpydim.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Eu 3+). (C15 N3 H11). 3(Cl 1-). 1(H2 O)' _chemical_formula_sum 'C15 H13 Cl3 Eu N3 O' _chemical_formula_weight 509.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7389(3) _cell_length_b 9.9001(3) _cell_length_c 10.1406(3) _cell_angle_alpha 94.7180(10) _cell_angle_beta 109.8960(10) _cell_angle_gamma 112.4750(10) _cell_volume 823.77(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9938 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 29.53 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.055 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492.0 _exptl_absorpt_coefficient_mu 4.299 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0833 _exptl_absorpt_correction_T_max 0.2053 _exptl_absorpt_process_details 'empirical (SADABS)' _exptl_special_details ; 'SADABS,Scheldrick G.M., Bruker-Siemens Area Detector Absorption and Other Correction, Version 2006/1, G ttingen Germany (2006).' ; _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_reflns_number 27911 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 29.57 _reflns_number_total 4621 _reflns_number_gt 4340 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SMART/SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4621 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0206 _refine_ls_R_factor_gt 0.0182 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0498 _refine_ls_goodness_of_fit_ref 1.220 _refine_ls_restrained_S_all 1.220 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.031956(13) 0.723776(12) 0.122553(11) 0.01913(5) Uani 1 1 d . . . Cl1 Cl 0.08695(8) 0.99337(7) 0.27532(7) 0.03029(14) Uani 1 1 d . . . Cl2 Cl -0.00533(10) 0.43244(8) 0.13853(7) 0.03565(16) Uani 1 1 d . . . Cl3 Cl -0.25050(9) 0.71204(9) -0.05797(8) 0.03919(17) Uani 1 1 d . . . N1 N 0.3304(3) 0.7990(3) 0.1846(2) 0.0291(5) Uani 1 1 d . . . N2 N 0.2038(3) 0.7487(2) 0.3843(2) 0.0226(4) Uani 1 1 d . . . N3 N -0.1246(3) 0.6424(2) 0.2826(2) 0.0267(4) Uani 1 1 d . . . C1 C 0.3918(4) 0.8238(4) 0.0838(3) 0.0376(7) Uani 1 1 d . . . H1 H 0.3202 0.8045 -0.0115 0.045 Uiso 1 1 calc R . . C12 C -0.1188(4) 0.6599(4) 0.5212(3) 0.0350(6) Uani 1 1 d . . . H12 H -0.0581 0.6871 0.6206 0.042 Uiso 1 1 calc R . . C11 C -0.0417(3) 0.6723(3) 0.4267(3) 0.0265(5) Uani 1 1 d . . . C5 C 0.4361(3) 0.8255(3) 0.3218(3) 0.0247(5) Uani 1 1 d . . . C10 C 0.1359(3) 0.7185(3) 0.4802(3) 0.0252(5) Uani 1 1 d . . . C6 C 0.3655(3) 0.7914(3) 0.4304(3) 0.0248(5) Uani 1 1 d . . . C9 C 0.2249(4) 0.7239(3) 0.6230(3) 0.0326(6) Uani 1 1 d . . . H9 H 0.1746 0.6998 0.6866 0.039 Uiso 1 1 calc R . . C7 C 0.4615(4) 0.8011(3) 0.5720(3) 0.0319(6) Uani 1 1 d . . . H7 H 0.5724 0.8309 0.6014 0.038 Uiso 1 1 calc R . . C15 C -0.2868(3) 0.5881(3) 0.2322(3) 0.0335(6) Uani 1 1 d . . . H15 H -0.3458 0.5632 0.1327 0.040 Uiso 1 1 calc R . . C8 C 0.3890(4) 0.7656(3) 0.6676(3) 0.0346(6) Uani 1 1 d . . . H8 H 0.4506 0.7697 0.7621 0.042 Uiso 1 1 calc R . . C14 C -0.3711(4) 0.5672(3) 0.3211(4) 0.0381(7) Uani 1 1 d . . . H14 H -0.4839 0.5266 0.2818 0.046 Uiso 1 1 calc R . . C2 C 0.5548(4) 0.8762(4) 0.1135(4) 0.0401(7) Uani 1 1 d . . . H2 H 0.5916 0.8913 0.0400 0.048 Uiso 1 1 calc R . . C13 C -0.2845(4) 0.6077(4) 0.4680(4) 0.0405(7) Uani 1 1 d . . . H13 H -0.3369 0.5999 0.5304 0.049 Uiso 1 1 calc R . . C3 C 0.6617(4) 0.9057(4) 0.2538(4) 0.0381(7) Uani 1 1 d . . . H3 H 0.7723 0.9410 0.2770 0.046 Uiso 1 1 calc R . . O1 O 0.1190(3) 0.9151(3) -0.0118(2) 0.0318(4) Uani 1 1 d . . . C4 C 0.6027(3) 0.8823(3) 0.3594(3) 0.0320(6) Uani 1 1 d . . . H4 H 0.6736 0.9042 0.4554 0.038 Uiso 1 1 calc R . . H1W H 0.042(6) 0.897(5) -0.107(5) 0.073(14) Uiso 1 1 d . . . H2W H 0.157(4) 0.995(4) 0.031(4) 0.030(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01887(7) 0.02205(7) 0.01614(7) 0.00534(5) 0.00667(5) 0.00884(5) Cl1 0.0326(3) 0.0278(3) 0.0258(3) 0.0037(2) 0.0063(3) 0.0139(3) Cl2 0.0605(5) 0.0282(3) 0.0247(3) 0.0100(3) 0.0226(3) 0.0204(3) Cl3 0.0252(3) 0.0460(4) 0.0359(4) 0.0095(3) 0.0036(3) 0.0131(3) N1 0.0253(11) 0.0378(12) 0.0266(11) 0.0105(10) 0.0118(9) 0.0146(10) N2 0.0236(10) 0.0219(9) 0.0217(10) 0.0045(8) 0.0084(8) 0.0101(8) N3 0.0272(11) 0.0273(11) 0.0265(11) 0.0074(9) 0.0131(9) 0.0105(9) C1 0.0330(15) 0.0554(19) 0.0306(15) 0.0135(13) 0.0168(12) 0.0214(14) C12 0.0421(16) 0.0394(15) 0.0304(15) 0.0107(12) 0.0211(13) 0.0185(13) C11 0.0299(13) 0.0258(12) 0.0254(13) 0.0076(10) 0.0134(10) 0.0116(10) C5 0.0233(12) 0.0239(11) 0.0286(13) 0.0072(10) 0.0099(10) 0.0122(10) C10 0.0306(13) 0.0239(11) 0.0211(12) 0.0067(9) 0.0107(10) 0.0115(10) C6 0.0249(12) 0.0223(11) 0.0246(12) 0.0050(9) 0.0069(10) 0.0107(10) C9 0.0386(15) 0.0372(15) 0.0213(13) 0.0098(11) 0.0109(11) 0.0163(12) C7 0.0285(13) 0.0335(14) 0.0277(14) 0.0066(11) 0.0042(11) 0.0141(11) C15 0.0278(13) 0.0327(14) 0.0353(15) 0.0065(12) 0.0113(12) 0.0101(11) C8 0.0397(16) 0.0363(15) 0.0213(13) 0.0084(11) 0.0050(11) 0.0163(13) C14 0.0302(14) 0.0341(15) 0.0531(19) 0.0137(14) 0.0213(14) 0.0125(12) C2 0.0395(16) 0.0509(18) 0.0459(18) 0.0191(15) 0.0286(15) 0.0243(15) C13 0.0421(17) 0.0424(17) 0.0508(19) 0.0163(14) 0.0331(15) 0.0185(14) C3 0.0264(14) 0.0404(16) 0.0531(19) 0.0143(14) 0.0190(13) 0.0171(12) O1 0.0337(11) 0.0325(11) 0.0317(11) 0.0124(9) 0.0127(9) 0.0165(9) C4 0.0228(12) 0.0340(14) 0.0366(15) 0.0088(12) 0.0094(11) 0.0121(11) _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 2.479(2) . ? Eu1 N1 2.534(2) . ? Eu1 N2 2.541(2) . ? Eu1 N3 2.563(2) . ? Eu1 Cl3 2.6879(7) . ? Eu1 Cl1 2.7335(6) . ? Eu1 Cl2 2.7916(7) . ? Eu1 Cl2 2.8321(7) 2_565 ? Cl2 Eu1 2.8321(7) 2_565 ? N1 C1 1.345(4) . ? N1 C5 1.350(3) . ? N2 C10 1.344(3) . ? N2 C6 1.355(3) . ? N3 C15 1.342(4) . ? N3 C11 1.348(3) . ? C1 C2 1.378(4) . ? C1 H1 0.9300 . ? C12 C13 1.373(4) . ? C12 C11 1.392(4) . ? C12 H12 0.9300 . ? C11 C10 1.487(4) . ? C5 C4 1.393(4) . ? C5 C6 1.483(4) . ? C10 C9 1.395(4) . ? C6 C7 1.393(4) . ? C9 C8 1.379(4) . ? C9 H9 0.9300 . ? C7 C8 1.376(4) . ? C7 H7 0.9300 . ? C15 C14 1.391(4) . ? C15 H15 0.9300 . ? C8 H8 0.9300 . ? C14 C13 1.371(5) . ? C14 H14 0.9300 . ? C2 C3 1.372(5) . ? C2 H2 0.9300 . ? C13 H13 0.9300 . ? C3 C4 1.374(4) . ? C3 H3 0.9300 . ? O1 H1W 0.95(5) . ? O1 H2W 0.75(4) . ? C4 H4 0.9300 . ? 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 N1 73.12(7) . . ? O1 Eu1 N2 122.63(7) . . ? N1 Eu1 N2 64.15(7) . . ? O1 Eu1 N3 144.68(7) . . ? N1 Eu1 N3 128.21(7) . . ? N2 Eu1 N3 64.41(7) . . ? O1 Eu1 Cl3 77.02(5) . . ? N1 Eu1 Cl3 148.43(6) . . ? N2 Eu1 Cl3 144.58(5) . . ? N3 Eu1 Cl3 82.79(5) . . ? O1 Eu1 Cl1 72.80(6) . . ? N1 Eu1 Cl1 93.96(6) . . ? N2 Eu1 Cl1 73.88(5) . . ? N3 Eu1 Cl1 77.46(5) . . ? Cl3 Eu1 Cl1 86.79(2) . . ? O1 Eu1 Cl2 140.72(5) . . ? N1 Eu1 Cl2 87.88(6) . . ? N2 Eu1 Cl2 74.88(5) . . ? N3 Eu1 Cl2 73.53(5) . . ? Cl3 Eu1 Cl2 109.61(3) . . ? Cl1 Eu1 Cl2 144.17(2) . . ? O1 Eu1 Cl2 73.19(6) . 2_565 ? N1 Eu1 Cl2 80.88(6) . 2_565 ? N2 Eu1 Cl2 130.72(5) . 2_565 ? N3 Eu1 Cl2 131.78(5) . 2_565 ? Cl3 Eu1 Cl2 80.90(2) . 2_565 ? Cl1 Eu1 Cl2 145.62(2) . 2_565 ? Cl2 Eu1 Cl2 69.99(2) . 2_565 ? Eu1 Cl2 Eu1 110.01(2) . 2_565 ? C1 N1 C5 117.2(2) . . ? C1 N1 Eu1 121.27(19) . . ? C5 N1 Eu1 121.41(17) . . ? C10 N2 C6 118.3(2) . . ? C10 N2 Eu1 120.70(17) . . ? C6 N2 Eu1 120.96(17) . . ? C15 N3 C11 117.5(2) . . ? C15 N3 Eu1 122.65(19) . . ? C11 N3 Eu1 119.34(17) . . ? N1 C1 C2 123.8(3) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C13 C12 C11 120.0(3) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? N3 C11 C12 121.6(3) . . ? N3 C11 C10 117.0(2) . . ? C12 C11 C10 121.4(2) . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C6 116.5(2) . . ? C4 C5 C6 121.8(2) . . ? N2 C10 C9 122.3(3) . . ? N2 C10 C11 117.2(2) . . ? C9 C10 C11 120.5(2) . . ? N2 C6 C7 122.1(3) . . ? N2 C6 C5 116.7(2) . . ? C7 C6 C5 121.2(2) . . ? C8 C9 C10 118.6(3) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C8 C7 C6 118.7(3) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? N3 C15 C14 123.3(3) . . ? N3 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? C7 C8 C9 120.0(3) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C13 C14 C15 118.6(3) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C3 C2 C1 118.6(3) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C14 C13 C12 118.7(3) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C2 C3 C4 119.0(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? Eu1 O1 H1W 115(3) . . ? Eu1 O1 H2W 114(3) . . ? H1W O1 H2W 114(4) . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.516 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.158