# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jian Zhou ' _publ_contact_author_email jianzhou888888@yahoo.com.cn _publ_author_name 'Jian Zhou' data_1 _database_code_depnum_ccdc_archive 'CCDC 815913' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H26 Eu N6 S3 Sb' _chemical_formula_sum 'C8 H26 Eu N6 S3 Sb ' _chemical_formula_weight 576.29 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Iba2 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+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1, -y+1, z+1/2' '-x+1, y+1, z+1/2' _cell_length_a 30.125(11) _cell_length_b 9.449(3) _cell_length_c 12.692(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3613(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.10 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 5.279 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4035 _exptl_absorpt_correction_T_max 0.5252 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9542 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.10 _reflns_number_total 3184 _reflns_number_gt 2960 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0000P)^2^+2.0215P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(16) _refine_ls_number_reflns 3184 _refine_ls_number_parameters 172 _refine_ls_number_restraints 223 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.025 _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 Sb1 Sb 0.102724(15) -0.27403(4) -0.02786(5) 0.03364(15) Uani 1 1 d . . . Eu1 Eu 0.121071(9) 0.11387(3) -0.01751(3) 0.02340(11) Uani 1 1 d . . . S1 S 0.05756(6) -0.08480(19) 0.04124(19) 0.0341(5) Uani 1 1 d . . . S2 S 0.15614(7) -0.1277(2) -0.12100(17) 0.0340(5) Uani 1 1 d . . . S3 S 0.14217(8) -0.3576(2) 0.1219(2) 0.0413(5) Uani 1 1 d . . . C1 C 0.2140(3) 0.0178(11) 0.1295(8) 0.058(2) Uani 1 1 d U . . H1A H 0.2275 -0.0607 0.0921 0.070 Uiso 1 1 calc R . . H1B H 0.2256 0.0182 0.2008 0.070 Uiso 1 1 calc R . . C2 C 0.2260(3) 0.1524(11) 0.0766(10) 0.0619(19) Uani 1 1 d U . . H2A H 0.2157 0.2317 0.1186 0.074 Uiso 1 1 calc R . . H2B H 0.2580 0.1592 0.0700 0.074 Uiso 1 1 calc R . . C3 C 0.2180(4) 0.2720(11) -0.1029(10) 0.071(2) Uani 1 1 d U . . H3A H 0.2486 0.2994 -0.0901 0.085 Uiso 1 1 calc R . . H3B H 0.2162 0.2350 -0.1740 0.085 Uiso 1 1 calc R . . C4 C 0.1919(3) 0.3885(10) -0.0957(11) 0.065(2) Uani 1 1 d U . . H4A H 0.1994 0.4531 -0.1522 0.078 Uiso 1 1 calc R . . H4B H 0.1979 0.4360 -0.0295 0.078 Uiso 1 1 calc R . . C5 C 0.0689(3) 0.3061(8) 0.1716(7) 0.0378(16) Uani 1 1 d U . . H5A H 0.0665 0.3766 0.2269 0.045 Uiso 1 1 calc R . . H5B H 0.0564 0.2182 0.1976 0.045 Uiso 1 1 calc R . . C6 C 0.0433(3) 0.3555(9) 0.0738(7) 0.0360(15) Uani 1 1 d U . . H6A H 0.0124 0.3705 0.0918 0.043 Uiso 1 1 calc R . . H6B H 0.0554 0.4446 0.0491 0.043 Uiso 1 1 calc R . . C7 C 0.0323(3) 0.3058(9) -0.1110(7) 0.0378(15) Uani 1 1 d U . . H7A H 0.0515 0.3828 -0.1328 0.045 Uiso 1 1 calc R . . H7B H 0.0022 0.3419 -0.1065 0.045 Uiso 1 1 calc R . . C8 C 0.0343(3) 0.1888(9) -0.1906(7) 0.0415(17) Uani 1 1 d U . . H8A H 0.0132 0.1152 -0.1721 0.050 Uiso 1 1 calc R . . H8B H 0.0264 0.2250 -0.2597 0.050 Uiso 1 1 calc R . . N1 N 0.1655(2) -0.0019(7) 0.1327(6) 0.0408(15) Uani 1 1 d U . . H1C H 0.1554 0.0328 0.1942 0.049 Uiso 1 1 calc R . . H1D H 0.1598 -0.0954 0.1322 0.049 Uiso 1 1 calc R . . N2 N 0.2056(2) 0.1580(8) -0.0275(8) 0.0596(15) Uani 1 1 d U . . H2C H 0.2160 0.0783 -0.0593 0.071 Uiso 1 1 calc R . . N3 N 0.1436(2) 0.3553(7) -0.1015(7) 0.0468(14) Uani 1 1 d U . . H3C H 0.1353 0.3551 -0.1696 0.056 Uiso 1 1 calc R . . H3D H 0.1284 0.4248 -0.0690 0.056 Uiso 1 1 calc R . . N4 N 0.1154(2) 0.2853(7) 0.1430(5) 0.0354(13) Uani 1 1 d U . . H4C H 0.1303 0.2489 0.1981 0.042 Uiso 1 1 calc R . . H4D H 0.1277 0.3692 0.1264 0.042 Uiso 1 1 calc R . . N5 N 0.04647(18) 0.2528(5) -0.0070(5) 0.0301(11) Uani 1 1 d U . . H5C H 0.0259 0.1863 0.0103 0.036 Uiso 1 1 calc R . . N6 N 0.0799(2) 0.1289(7) -0.1935(6) 0.0420(15) Uani 1 1 d U . . H6C H 0.0962 0.1818 -0.2379 0.050 Uiso 1 1 calc R . . H6D H 0.0783 0.0412 -0.2209 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb1 0.0404(3) 0.0220(2) 0.0385(3) -0.0013(3) -0.0063(3) -0.00330(17) Eu1 0.02029(17) 0.02119(17) 0.0287(2) 0.0006(2) -0.00038(19) 0.00042(10) S1 0.0235(9) 0.0298(10) 0.0489(13) 0.0063(9) 0.0032(9) -0.0012(7) S2 0.0374(11) 0.0313(10) 0.0334(12) -0.0009(8) 0.0036(9) 0.0065(8) S3 0.0523(14) 0.0265(10) 0.0451(13) 0.0070(9) -0.0044(10) 0.0053(9) C1 0.040(4) 0.058(4) 0.076(5) 0.003(4) -0.019(4) 0.005(4) C2 0.045(4) 0.059(4) 0.082(4) 0.000(4) -0.012(4) -0.006(3) C3 0.057(4) 0.061(4) 0.094(5) 0.010(4) 0.004(4) -0.012(4) C4 0.050(4) 0.056(4) 0.090(5) 0.013(4) 0.007(4) -0.013(3) C5 0.042(3) 0.030(3) 0.040(3) -0.002(3) 0.002(3) 0.007(3) C6 0.032(3) 0.029(3) 0.047(3) 0.005(3) 0.008(3) 0.001(3) C7 0.035(3) 0.032(3) 0.047(3) 0.004(3) -0.001(3) 0.009(3) C8 0.035(3) 0.045(4) 0.044(4) 0.002(3) -0.011(3) 0.011(3) N1 0.034(3) 0.034(3) 0.054(4) -0.002(3) -0.010(3) 0.002(3) N2 0.041(3) 0.056(3) 0.082(4) 0.012(3) -0.006(3) -0.007(2) N3 0.043(3) 0.036(3) 0.062(3) 0.007(3) 0.001(3) -0.003(2) N4 0.033(3) 0.028(3) 0.045(3) 0.004(2) 0.000(2) 0.002(2) N5 0.030(2) 0.022(2) 0.038(3) 0.001(2) 0.004(3) 0.0030(19) N6 0.041(3) 0.041(3) 0.043(4) 0.000(3) 0.000(3) 0.009(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 Sb1 S3 2.377(2) . ? Sb1 S1 2.412(2) . ? Sb1 S2 2.429(2) . ? Sb1 Eu1 3.7089(14) . ? Eu1 N6 2.560(7) . ? Eu1 N1 2.573(7) . ? Eu1 N2 2.584(6) . ? Eu1 N5 2.606(5) . ? Eu1 N3 2.607(7) . ? Eu1 N4 2.608(7) . ? Eu1 S1 2.7821(19) . ? Eu1 S2 2.838(2) . ? C1 N1 1.474(11) . ? C1 C2 1.483(14) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.457(14) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.356(13) . ? C3 N2 1.489(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N3 1.490(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N4 1.461(10) . ? C5 C6 1.534(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N5 1.414(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N5 1.476(11) . ? C7 C8 1.499(12) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N6 1.486(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 H2C 0.9100 . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 H4C 0.9000 . ? N4 H4D 0.9000 . ? N5 H5C 0.9100 . ? N6 H6C 0.9000 . ? N6 H6D 0.9000 . ? 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 S3 Sb1 S1 103.73(8) . . ? S3 Sb1 S2 104.31(8) . . ? S1 Sb1 S2 97.40(7) . . ? S3 Sb1 Eu1 103.03(6) . . ? S1 Sb1 Eu1 48.59(5) . . ? S2 Sb1 Eu1 49.91(5) . . ? N6 Eu1 N1 157.3(2) . . ? N6 Eu1 N2 115.2(3) . . ? N1 Eu1 N2 65.9(2) . . ? N6 Eu1 N5 66.3(2) . . ? N1 Eu1 N5 128.7(2) . . ? N2 Eu1 N5 140.5(2) . . ? N6 Eu1 N3 73.8(2) . . ? N1 Eu1 N3 122.6(2) . . ? N2 Eu1 N3 65.3(2) . . ? N5 Eu1 N3 78.7(2) . . ? N6 Eu1 N4 128.0(2) . . ? N1 Eu1 N4 73.7(2) . . ? N2 Eu1 N4 90.2(3) . . ? N5 Eu1 N4 65.8(2) . . ? N3 Eu1 N4 78.0(2) . . ? N6 Eu1 S1 86.44(17) . . ? N1 Eu1 S1 82.67(16) . . ? N2 Eu1 S1 143.11(17) . . ? N5 Eu1 S1 74.52(13) . . ? N3 Eu1 S1 151.47(17) . . ? N4 Eu1 S1 99.48(15) . . ? N6 Eu1 S2 79.71(15) . . ? N1 Eu1 S2 78.90(17) . . ? N2 Eu1 S2 74.9(2) . . ? N5 Eu1 S2 138.59(14) . . ? N3 Eu1 S2 114.69(19) . . ? N4 Eu1 S2 152.33(15) . . ? S1 Eu1 S2 80.64(6) . . ? N6 Eu1 Sb1 87.24(15) . . ? N1 Eu1 Sb1 71.57(16) . . ? N2 Eu1 Sb1 107.73(17) . . ? N5 Eu1 Sb1 111.78(12) . . ? N3 Eu1 Sb1 152.71(19) . . ? N4 Eu1 Sb1 129.18(15) . . ? S1 Eu1 Sb1 40.56(4) . . ? S2 Eu1 Sb1 40.90(5) . . ? Sb1 S1 Eu1 90.85(7) . . ? Sb1 S2 Eu1 89.19(7) . . ? N1 C1 C2 111.1(7) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 109.9(8) . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 N2 113.5(10) . . ? C4 C3 H3A 108.9 . . ? N2 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? N2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C3 C4 N3 113.1(8) . . ? C3 C4 H4A 109.0 . . ? N3 C4 H4A 109.0 . . ? C3 C4 H4B 109.0 . . ? N3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? N4 C5 C6 108.7(7) . . ? N4 C5 H5A 109.9 . . ? C6 C5 H5A 109.9 . . ? N4 C5 H5B 109.9 . . ? C6 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? N5 C6 C5 110.1(6) . . ? N5 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? N5 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? N5 C7 C8 109.9(6) . . ? N5 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N5 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N6 C8 C7 109.5(7) . . ? N6 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? N6 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C1 N1 Eu1 116.2(6) . . ? C1 N1 H1C 108.2 . . ? Eu1 N1 H1C 108.2 . . ? C1 N1 H1D 108.2 . . ? Eu1 N1 H1D 108.2 . . ? H1C N1 H1D 107.4 . . ? C2 N2 C3 120.2(8) . . ? C2 N2 Eu1 111.4(6) . . ? C3 N2 Eu1 113.3(6) . . ? C2 N2 H2C 103.2 . . ? C3 N2 H2C 103.2 . . ? Eu1 N2 H2C 103.2 . . ? C4 N3 Eu1 114.7(6) . . ? C4 N3 H3C 108.6 . . ? Eu1 N3 H3C 108.6 . . ? C4 N3 H3D 108.6 . . ? Eu1 N3 H3D 108.6 . . ? H3C N3 H3D 107.6 . . ? C5 N4 Eu1 109.9(5) . . ? C5 N4 H4C 109.7 . . ? Eu1 N4 H4C 109.7 . . ? C5 N4 H4D 109.7 . . ? Eu1 N4 H4D 109.7 . . ? H4C N4 H4D 108.2 . . ? C6 N5 C7 113.3(5) . . ? C6 N5 Eu1 116.2(5) . . ? C7 N5 Eu1 112.0(4) . . ? C6 N5 H5C 104.6 . . ? C7 N5 H5C 104.6 . . ? Eu1 N5 H5C 104.6 . . ? C8 N6 Eu1 116.6(5) . . ? C8 N6 H6C 108.1 . . ? Eu1 N6 H6C 108.1 . . ? C8 N6 H6D 108.1 . . ? Eu1 N6 H6D 108.1 . . ? H6C N6 H6D 107.3 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.140 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.120 # Attachment '- 2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 815914' #TrackingRef '- 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H52 Eu2 N12 S5 Sb2, 2(Cl)' _chemical_formula_sum 'C16 H52 Cl2 Eu2 N12 S5 Sb2 ' _chemical_formula_weight 1191.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.566(7) _cell_length_b 8.4157(17) _cell_length_c 18.003(7) _cell_angle_alpha 90.00 _cell_angle_beta 116.71(3) _cell_angle_gamma 90.00 _cell_volume 3731(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 25.10 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296.0 _exptl_absorpt_coefficient_mu 5.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5540 _exptl_absorpt_correction_T_max 0.7143 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9760 _diffrn_reflns_av_R_equivalents 0.1331 _diffrn_reflns_av_sigmaI/netI 0.1546 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.10 _reflns_number_total 3305 _reflns_number_gt 1734 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0155P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3305 _refine_ls_number_parameters 177 _refine_ls_number_restraints 216 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.927 _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 -0.12140(2) -0.14611(7) -0.05355(3) 0.03091(16) Uani 1 1 d . . . Sb1 Sb -0.03009(3) -0.36049(10) 0.13778(4) 0.0416(2) Uani 1 1 d . . . S1 S -0.00916(12) -0.2273(4) 0.03791(15) 0.0504(9) Uani 1 1 d . . . S2 S -0.12490(11) -0.3158(4) 0.07678(15) 0.0463(8) Uani 1 1 d . . . S3 S 0.0000 -0.1609(5) 0.2500 0.0490(12) Uani 1 2 d S . . N1 N -0.1188(4) -0.4373(10) -0.0961(5) 0.060(2) Uani 1 1 d U . . H1A H -0.0888 -0.4826 -0.0564 0.072 Uiso 1 1 calc R . . H1B H -0.1475 -0.4877 -0.0961 0.072 Uiso 1 1 calc R . . N2 N -0.1152(4) -0.1880(12) -0.1908(5) 0.072(2) Uani 1 1 d U . . H2C H -0.1507 -0.1977 -0.2284 0.086 Uiso 1 1 calc R . . N3 N -0.1291(4) 0.1070(11) -0.1392(5) 0.065(2) Uani 1 1 d U . . H3A H -0.1595 0.1587 -0.1466 0.078 Uiso 1 1 calc R . . H3B H -0.1008 0.1704 -0.1086 0.078 Uiso 1 1 calc R . . N4 N -0.0762(3) 0.0800(11) 0.0530(4) 0.052(2) Uani 1 1 d U . . H4A H -0.0563 0.0355 0.1031 0.062 Uiso 1 1 calc R . . H4B H -0.0531 0.1317 0.0387 0.062 Uiso 1 1 calc R . . N5 N -0.1879(3) 0.0314(10) -0.0300(4) 0.0396(17) Uani 1 1 d U . . H5C H -0.1984 0.1079 -0.0699 0.047 Uiso 1 1 calc R . . N6 N -0.2199(3) -0.2339(11) -0.1357(4) 0.0513(19) Uani 1 1 d U . . H6A H -0.2276 -0.2403 -0.1897 0.062 Uiso 1 1 calc R . . H6B H -0.2233 -0.3322 -0.1188 0.062 Uiso 1 1 calc R . . C1 C -0.1191(5) -0.4673(15) -0.1761(7) 0.073(3) Uani 1 1 d U . . H1C H -0.1011 -0.5675 -0.1740 0.087 Uiso 1 1 calc R . . H1D H -0.1562 -0.4748 -0.2192 0.087 Uiso 1 1 calc R . . C2 C -0.0929(5) -0.3474(15) -0.1947(6) 0.067(2) Uani 1 1 d U . . H2A H -0.0963 -0.3641 -0.2501 0.080 Uiso 1 1 calc R . . H2B H -0.0546 -0.3504 -0.1558 0.080 Uiso 1 1 calc R . . C3 C -0.0989(5) -0.0541(14) -0.2197(6) 0.060(2) Uani 1 1 d U . . H3C H -0.1039 -0.0735 -0.2758 0.072 Uiso 1 1 calc R . . H3D H -0.0606 -0.0347 -0.1846 0.072 Uiso 1 1 calc R . . C4 C -0.1303(5) 0.0870(13) -0.2193(6) 0.055(2) Uani 1 1 d U . . H4C H -0.1152 0.1805 -0.2327 0.066 Uiso 1 1 calc R . . H4D H -0.1676 0.0754 -0.2614 0.066 Uiso 1 1 calc R . . C5 C -0.1125(5) 0.1976(13) 0.0618(6) 0.051(2) Uani 1 1 d U . . H5A H -0.1209 0.2805 0.0204 0.061 Uiso 1 1 calc R . . H5B H -0.0949 0.2462 0.1165 0.061 Uiso 1 1 calc R . . C6 C -0.1638(4) 0.1157(12) 0.0505(5) 0.046(2) Uani 1 1 d U . . H6C H -0.1557 0.0406 0.0954 0.055 Uiso 1 1 calc R . . H6D H -0.1893 0.1934 0.0520 0.055 Uiso 1 1 calc R . . C7 C -0.2376(4) -0.0539(13) -0.0430(5) 0.044(2) Uani 1 1 d U . . H7A H -0.2636 0.0192 -0.0392 0.053 Uiso 1 1 calc R . . H7B H -0.2292 -0.1353 -0.0009 0.053 Uiso 1 1 calc R . . C8 C -0.2609(4) -0.1281(13) -0.1278(5) 0.050(2) Uani 1 1 d U . . H8A H -0.2929 -0.1895 -0.1369 0.060 Uiso 1 1 calc R . . H8B H -0.2718 -0.0454 -0.1698 0.060 Uiso 1 1 calc R . . Cl1 Cl -0.23821(12) 0.3418(4) -0.16011(15) 0.0532(8) 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 Eu1 0.0331(3) 0.0350(4) 0.0245(2) 0.0005(3) 0.0128(2) -0.0008(3) Sb1 0.0444(5) 0.0463(6) 0.0302(4) 0.0044(4) 0.0134(3) 0.0056(4) S1 0.0413(19) 0.072(3) 0.0384(15) 0.0075(15) 0.0184(13) -0.0011(17) S2 0.0382(18) 0.059(2) 0.0414(15) 0.0110(14) 0.0179(13) -0.0056(16) S3 0.057(3) 0.054(3) 0.0295(19) 0.000 0.0140(18) 0.000 N1 0.070(5) 0.052(5) 0.062(4) 0.002(4) 0.033(4) 0.013(4) N2 0.094(4) 0.061(4) 0.067(4) 0.009(3) 0.042(3) 0.024(4) N3 0.083(4) 0.062(4) 0.066(3) 0.012(3) 0.047(3) 0.015(4) N4 0.058(4) 0.049(5) 0.047(4) 0.000(3) 0.023(3) -0.006(4) N5 0.051(4) 0.042(4) 0.039(3) 0.002(3) 0.033(3) 0.003(3) N6 0.061(4) 0.051(4) 0.049(3) 0.002(3) 0.032(3) 0.006(4) C1 0.085(5) 0.060(5) 0.068(4) 0.005(4) 0.029(4) 0.015(4) C2 0.094(5) 0.057(5) 0.063(4) 0.009(4) 0.048(4) 0.030(4) C3 0.084(5) 0.056(5) 0.063(4) 0.010(4) 0.053(4) 0.013(4) C4 0.086(5) 0.051(5) 0.050(4) 0.013(4) 0.050(4) 0.022(4) C5 0.063(5) 0.047(5) 0.046(4) -0.002(4) 0.028(4) -0.003(4) C6 0.058(4) 0.048(5) 0.040(4) -0.001(4) 0.030(3) 0.003(4) C7 0.053(4) 0.041(5) 0.045(4) 0.000(4) 0.029(3) 0.004(4) C8 0.053(5) 0.051(5) 0.048(4) 0.002(4) 0.026(4) 0.004(4) Cl1 0.056(2) 0.057(2) 0.0439(14) 0.0056(15) 0.0207(13) 0.0093(18) _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 N6 2.548(8) . ? Eu1 N5 2.545(8) . ? Eu1 N2 2.577(8) . ? Eu1 N3 2.582(8) . ? Eu1 N1 2.578(8) . ? Eu1 N4 2.589(8) . ? Eu1 S2 2.785(3) . ? Eu1 S1 2.859(3) . ? Eu1 Sb1 3.6961(16) . ? Sb1 S2 2.366(3) . ? Sb1 S1 2.399(3) . ? Sb1 S3 2.467(3) . ? S3 Sb1 2.467(3) 2 ? N1 C1 1.458(11) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C3 1.397(13) . ? N2 C2 1.489(12) . ? N2 H2C 0.9100 . ? N3 C4 1.437(10) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C5 1.465(12) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 C7 1.468(11) . ? N5 C6 1.476(10) . ? N5 H5C 0.9100 . ? N6 C8 1.496(11) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? C1 C2 1.366(14) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.471(13) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C5 C6 1.502(13) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C7 C8 1.500(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? 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 N6 Eu1 N5 66.9(3) . . ? N6 Eu1 N2 85.2(3) . . ? N5 Eu1 N2 127.2(3) . . ? N6 Eu1 N3 96.5(3) . . ? N5 Eu1 N3 75.2(3) . . ? N2 Eu1 N3 64.1(3) . . ? N6 Eu1 N1 73.5(3) . . ? N5 Eu1 N1 136.6(3) . . ? N2 Eu1 N1 64.0(3) . . ? N3 Eu1 N1 127.7(3) . . ? N6 Eu1 N4 132.5(3) . . ? N5 Eu1 N4 65.6(3) . . ? N2 Eu1 N4 126.4(3) . . ? N3 Eu1 N4 73.7(3) . . ? N1 Eu1 N4 148.3(3) . . ? N6 Eu1 S2 84.77(19) . . ? N5 Eu1 S2 81.95(18) . . ? N2 Eu1 S2 141.3(2) . . ? N3 Eu1 S2 154.38(19) . . ? N1 Eu1 S2 77.25(19) . . ? N4 Eu1 S2 86.57(19) . . ? N6 Eu1 S1 149.3(2) . . ? N5 Eu1 S1 135.96(18) . . ? N2 Eu1 S1 89.9(2) . . ? N3 Eu1 S1 108.5(2) . . ? N1 Eu1 S1 77.1(2) . . ? N4 Eu1 S1 73.3(2) . . ? S2 Eu1 S1 80.24(8) . . ? N6 Eu1 Sb1 120.05(19) . . ? N5 Eu1 Sb1 111.78(16) . . ? N2 Eu1 Sb1 121.1(2) . . ? N3 Eu1 Sb1 142.9(2) . . ? N1 Eu1 Sb1 73.43(18) . . ? N4 Eu1 Sb1 76.65(19) . . ? S2 Eu1 Sb1 39.79(6) . . ? S1 Eu1 Sb1 40.46(6) . . ? S2 Sb1 S1 99.53(10) . . ? S2 Sb1 S3 99.59(8) . . ? S1 Sb1 S3 100.97(10) . . ? S2 Sb1 Eu1 48.88(6) . . ? S1 Sb1 Eu1 50.65(7) . . ? S3 Sb1 Eu1 105.57(8) . . ? Sb1 S1 Eu1 88.89(9) . . ? Sb1 S2 Eu1 91.33(9) . . ? Sb1 S3 Sb1 94.17(16) . 2 ? C1 N1 Eu1 118.0(7) . . ? C1 N1 H1A 107.8 . . ? Eu1 N1 H1A 107.8 . . ? C1 N1 H1B 107.8 . . ? Eu1 N1 H1B 107.8 . . ? H1A N1 H1B 107.1 . . ? C3 N2 C2 120.1(10) . . ? C3 N2 Eu1 114.6(7) . . ? C2 N2 Eu1 112.0(6) . . ? C3 N2 H2C 102.3 . . ? C2 N2 H2C 102.3 . . ? Eu1 N2 H2C 102.3 . . ? C4 N3 Eu1 117.5(7) . . ? C4 N3 H3A 107.9 . . ? Eu1 N3 H3A 107.9 . . ? C4 N3 H3B 107.9 . . ? Eu1 N3 H3B 107.9 . . ? H3A N3 H3B 107.2 . . ? C5 N4 Eu1 116.9(6) . . ? C5 N4 H4A 108.1 . . ? Eu1 N4 H4A 108.1 . . ? C5 N4 H4B 108.1 . . ? Eu1 N4 H4B 108.1 . . ? H4A N4 H4B 107.3 . . ? C7 N5 C6 111.7(7) . . ? C7 N5 Eu1 112.1(6) . . ? C6 N5 Eu1 113.9(6) . . ? C7 N5 H5C 106.2 . . ? C6 N5 H5C 106.2 . . ? Eu1 N5 H5C 106.2 . . ? C8 N6 Eu1 115.2(6) . . ? C8 N6 H6A 108.5 . . ? Eu1 N6 H6A 108.5 . . ? C8 N6 H6B 108.5 . . ? Eu1 N6 H6B 108.5 . . ? H6A N6 H6B 107.5 . . ? C2 C1 N1 110.1(10) . . ? C2 C1 H1C 109.6 . . ? N1 C1 H1C 109.6 . . ? C2 C1 H1D 109.6 . . ? N1 C1 H1D 109.6 . . ? H1C C1 H1D 108.1 . . ? C1 C2 N2 112.3(11) . . ? C1 C2 H2A 109.1 . . ? N2 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? N2 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? N2 C3 C4 111.2(10) . . ? N2 C3 H3C 109.4 . . ? C4 C3 H3C 109.4 . . ? N2 C3 H3D 109.4 . . ? C4 C3 H3D 109.4 . . ? H3C C3 H3D 108.0 . . ? N3 C4 C3 110.5(8) . . ? N3 C4 H4C 109.6 . . ? C3 C4 H4C 109.6 . . ? N3 C4 H4D 109.6 . . ? C3 C4 H4D 109.6 . . ? H4C C4 H4D 108.1 . . ? N4 C5 C6 108.8(9) . . ? N4 C5 H5A 109.9 . . ? C6 C5 H5A 109.9 . . ? N4 C5 H5B 109.9 . . ? C6 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? N5 C6 C5 109.6(7) . . ? N5 C6 H6C 109.7 . . ? C5 C6 H6C 109.7 . . ? N5 C6 H6D 109.7 . . ? C5 C6 H6D 109.7 . . ? H6C C6 H6D 108.2 . . ? N5 C7 C8 108.0(7) . . ? N5 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? N5 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? N6 C8 C7 110.3(8) . . ? N6 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? N6 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.490 _refine_diff_density_min -1.533 _refine_diff_density_rms 0.196