# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email jiadingxian@suda.edu.cn _publ_contact_author_name 'Dingxian Jia' loop_ _publ_author_name 'Weiwei Tang' 'Ruihong Chen' 'Jing Zhao' 'Wenqing Jiang' 'Yong Zhang' ; Dingxian Jia ; data_shelxl _database_code_depnum_ccdc_archive 'CCDC 863636' #TrackingRef 'cif of 1a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H26 N6 Pr S4 Sb' _chemical_formula_sum 'C8 H26 N6 Pr S4 Sb' _chemical_formula_weight 597.25 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' Pr Pr -0.2180 2.8214 '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' 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 orthorhombic _symmetry_space_group_name_H-M 'p bca' _symmetry_space_group_name_Hall '-p 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 8.6405(12) _cell_length_b 16.365(3) _cell_length_c 26.485(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3745.1(9) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 11898 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.35 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 4.459 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4692 _exptl_absorpt_correction_T_max 0.7168 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 34786 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3418 _reflns_number_gt 3338 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^+61.6399P] 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 3418 _refine_ls_number_parameters 188 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.145 _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 -0.00159(7) 0.73386(4) 0.38011(2) 0.01369(17) Uani 1 1 d . . . Pr1 Pr 0.44608(6) 0.74175(3) 0.383207(19) 0.01468(15) Uani 1 1 d . . . S1 S 0.1585(3) 0.83710(16) 0.34993(10) 0.0202(6) Uani 1 1 d . . . S2 S 0.1643(3) 0.66406(16) 0.43466(9) 0.0179(5) Uani 1 1 d . . . S3 S -0.2141(3) 0.78177(16) 0.42470(9) 0.0211(6) Uani 1 1 d . . . S4 S -0.0812(3) 0.65145(16) 0.31386(9) 0.0199(5) Uani 1 1 d . . . N1 N 0.3190(10) 0.6490(5) 0.3096(3) 0.0215(19) Uani 1 1 d . . . H1A H 0.2134 0.6557 0.3105 0.026 Uiso 1 1 calc R . . H1B H 0.3532 0.6681 0.2788 0.026 Uiso 1 1 calc R . . N2 N 0.5750(10) 0.5923(5) 0.3682(3) 0.023(2) Uani 1 1 d . . . H2 H 0.6812 0.6003 0.3652 0.028 Uiso 1 1 calc R . . N3 N 0.5236(10) 0.6608(6) 0.4685(3) 0.025(2) Uani 1 1 d . . . H3A H 0.5835 0.6943 0.4885 0.031 Uiso 1 1 calc R . . H3B H 0.4350 0.6485 0.4862 0.031 Uiso 1 1 calc R . . N4 N 0.4043(11) 0.8430(5) 0.4604(3) 0.025(2) Uani 1 1 d D . . H4A H 0.3074 0.8332 0.4735 0.030 Uiso 1 1 calc R . . H4B H 0.4749 0.8295 0.4850 0.030 Uiso 1 1 calc R . . N5 N 0.5199(12) 0.8987(5) 0.3668(3) 0.028(2) Uani 1 1 d D . . N6 N 0.5938(10) 0.7752(5) 0.2950(3) 0.0206(19) Uani 1 1 d D . . H6A H 0.6859 0.7470 0.2948 0.025 Uiso 1 1 calc R . . H6B H 0.5345 0.7550 0.2690 0.025 Uiso 1 1 calc R . . C1 C 0.3530(15) 0.5627(7) 0.3126(4) 0.032(3) Uani 1 1 d . . . H1C H 0.3206 0.5351 0.2811 0.039 Uiso 1 1 calc R . . H1D H 0.2954 0.5380 0.3411 0.039 Uiso 1 1 calc R . . C2 C 0.5219(14) 0.5518(7) 0.3204(4) 0.029(3) Uani 1 1 d . . . H2A H 0.5785 0.5755 0.2914 0.035 Uiso 1 1 calc R . . H2B H 0.5462 0.4927 0.3219 0.035 Uiso 1 1 calc R . . C3 C 0.5510(15) 0.5406(7) 0.4127(4) 0.031(3) Uani 1 1 d . . . H3C H 0.6068 0.4882 0.4084 0.038 Uiso 1 1 calc R . . H3D H 0.4394 0.5286 0.4167 0.038 Uiso 1 1 calc R . . C4 C 0.6098(15) 0.5842(7) 0.4581(5) 0.035(3) Uani 1 1 d . . . H4C H 0.6014 0.5477 0.4878 0.042 Uiso 1 1 calc R . . H4D H 0.7206 0.5973 0.4532 0.042 Uiso 1 1 calc R . . C5 C 0.417(2) 0.9291(7) 0.4511(5) 0.035(4) Uani 1 1 d D . . C6A C 0.526(2) 0.9532(10) 0.4113(6) 0.032(5) Uani 0.64 1 d PD . . C6B C 0.450(3) 0.9591(15) 0.3994(7) 0.032(5) Uani 0.36 1 d PD . . C7A C 0.634(2) 0.9161(10) 0.3291(6) 0.029(5) Uani 0.64 1 d PD . . C7B C 0.556(5) 0.9248(15) 0.3150(7) 0.029(5) Uani 0.36 1 d PD . . C8 C 0.628(2) 0.8618(7) 0.2841(4) 0.034(4) Uani 1 1 d 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 Sb1 0.0098(3) 0.0192(3) 0.0121(3) 0.0005(3) -0.0008(2) -0.0015(2) Pr1 0.0139(3) 0.0163(3) 0.0138(3) 0.0003(2) 0.0008(2) -0.0009(2) S1 0.0142(12) 0.0197(13) 0.0266(14) 0.0075(10) -0.0012(11) -0.0023(10) S2 0.0130(12) 0.0254(14) 0.0155(12) 0.0060(10) -0.0014(10) -0.0025(10) S3 0.0114(12) 0.0335(15) 0.0184(12) -0.0048(10) 0.0017(10) 0.0032(11) S4 0.0138(13) 0.0303(14) 0.0155(12) -0.0055(10) -0.0020(10) -0.0031(10) N1 0.026(5) 0.026(5) 0.013(4) -0.006(4) 0.004(4) -0.005(4) N2 0.017(5) 0.021(5) 0.032(5) -0.001(4) 0.005(4) -0.001(4) N3 0.018(5) 0.042(6) 0.016(4) 0.008(4) -0.002(4) -0.002(4) N4 0.030(5) 0.024(5) 0.021(5) -0.007(4) 0.008(4) -0.001(4) N5 0.043(6) 0.028(5) 0.014(4) -0.006(4) 0.003(4) -0.016(4) N6 0.013(4) 0.032(5) 0.017(4) -0.002(4) 0.004(3) -0.002(4) C1 0.045(8) 0.029(7) 0.023(6) -0.007(5) -0.007(5) -0.007(5) C2 0.032(7) 0.023(6) 0.033(6) -0.012(5) 0.005(5) 0.002(5) C3 0.033(7) 0.026(6) 0.034(7) 0.005(5) -0.004(5) -0.001(5) C4 0.042(7) 0.024(6) 0.040(7) 0.014(5) -0.020(6) -0.005(5) C5 0.048(14) 0.027(7) 0.029(7) -0.003(5) 0.014(8) -0.007(8) C6A 0.036(14) 0.027(6) 0.032(11) -0.007(7) 0.020(10) 0.003(9) C6B 0.038(14) 0.026(6) 0.034(11) -0.016(7) 0.010(10) 0.006(9) C7A 0.035(13) 0.033(7) 0.028(11) 0.009(7) 0.011(9) 0.006(9) C7B 0.037(13) 0.034(7) 0.023(11) 0.010(7) 0.013(9) 0.010(9) C8 0.048(13) 0.041(8) 0.023(6) -0.009(6) 0.006(7) -0.012(8) _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 S4 2.317(3) . ? Sb1 S3 2.320(3) . ? Sb1 S1 2.325(3) . ? Sb1 S2 2.334(3) . ? Pr1 N4 2.656(8) . ? Pr1 N5 2.682(9) . ? Pr1 N3 2.704(8) . ? Pr1 N1 2.704(8) . ? Pr1 N2 2.717(9) . ? Pr1 N6 2.718(8) . ? Pr1 S1 3.064(3) . ? Pr1 S2 3.066(3) . ? Pr1 S3 3.202(3) 1_655 ? S3 Pr1 3.202(3) 1_455 ? N1 C1 1.445(14) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C3 1.464(14) . ? N2 C2 1.501(14) . ? N2 H2 0.9300 . ? N3 C4 1.483(15) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? N4 C5 1.435(12) . ? N4 H4A 0.9200 . ? N4 H4B 0.9200 . ? N5 C7A 1.43(2) . ? N5 C6B 1.444(18) . ? N5 C7B 1.470(14) . ? N5 C6A 1.479(15) . ? N6 C8 1.476(12) . ? N6 H6A 0.9200 . ? N6 H6B 0.9200 . ? C1 C2 1.484(17) . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.489(16) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 H4C 0.9900 . ? C4 H4D 0.9900 . ? C5 C6A 1.469(16) . ? C5 C6B 1.483(18) . ? C7A C8 1.487(15) . ? C7B C8 1.454(18) . ? 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 S4 Sb1 S3 110.32(9) . . ? S4 Sb1 S1 109.82(10) . . ? S3 Sb1 S1 113.60(10) . . ? S4 Sb1 S2 111.47(10) . . ? S3 Sb1 S2 109.67(9) . . ? S1 Sb1 S2 101.72(9) . . ? N4 Pr1 N5 63.9(3) . . ? N4 Pr1 N3 72.3(3) . . ? N5 Pr1 N3 123.1(3) . . ? N4 Pr1 N1 148.2(3) . . ? N5 Pr1 N1 121.1(3) . . ? N3 Pr1 N1 115.4(3) . . ? N4 Pr1 N2 136.9(3) . . ? N5 Pr1 N2 137.8(3) . . ? N3 Pr1 N2 65.1(3) . . ? N1 Pr1 N2 63.6(3) . . ? N4 Pr1 N6 126.9(3) . . ? N5 Pr1 N6 63.7(2) . . ? N3 Pr1 N6 134.5(3) . . ? N1 Pr1 N6 71.5(3) . . ? N2 Pr1 N6 82.1(3) . . ? N4 Pr1 S1 78.1(2) . . ? N5 Pr1 S1 70.0(2) . . ? N3 Pr1 S1 133.7(2) . . ? N1 Pr1 S1 75.5(2) . . ? N2 Pr1 S1 138.5(2) . . ? N6 Pr1 S1 91.78(19) . . ? N4 Pr1 S2 79.0(2) . . ? N5 Pr1 S2 131.1(2) . . ? N3 Pr1 S2 67.8(2) . . ? N1 Pr1 S2 76.44(19) . . ? N2 Pr1 S2 91.00(19) . . ? N6 Pr1 S2 146.97(18) . . ? S1 Pr1 S2 72.24(7) . . ? N4 Pr1 S3 74.5(2) . 1_655 ? N5 Pr1 S3 69.0(2) . 1_655 ? N3 Pr1 S3 65.6(2) . 1_655 ? N1 Pr1 S3 137.3(2) . 1_655 ? N2 Pr1 S3 81.9(2) . 1_655 ? N6 Pr1 S3 79.83(18) . 1_655 ? S1 Pr1 S3 137.57(7) . 1_655 ? S2 Pr1 S3 131.32(7) . 1_655 ? Sb1 S1 Pr1 90.77(8) . . ? Sb1 S2 Pr1 90.55(8) . . ? Sb1 S3 Pr1 118.81(9) . 1_455 ? C1 N1 Pr1 115.2(6) . . ? C1 N1 H1A 108.5 . . ? Pr1 N1 H1A 108.5 . . ? C1 N1 H1B 108.5 . . ? Pr1 N1 H1B 108.5 . . ? H1A N1 H1B 107.5 . . ? C3 N2 C2 112.3(9) . . ? C3 N2 Pr1 110.1(6) . . ? C2 N2 Pr1 113.3(6) . . ? C3 N2 H2 106.9 . . ? C2 N2 H2 106.9 . . ? Pr1 N2 H2 106.9 . . ? C4 N3 Pr1 112.5(6) . . ? C4 N3 H3A 109.1 . . ? Pr1 N3 H3A 109.1 . . ? C4 N3 H3B 109.1 . . ? Pr1 N3 H3B 109.1 . . ? H3A N3 H3B 107.8 . . ? C5 N4 Pr1 118.1(7) . . ? C5 N4 H4A 107.8 . . ? Pr1 N4 H4A 107.8 . . ? C5 N4 H4B 107.8 . . ? Pr1 N4 H4B 107.8 . . ? H4A N4 H4B 107.1 . . ? C7A N5 C6B 124.7(14) . . ? C7A N5 C7B 31.2(15) . . ? C6B N5 C7B 116.6(13) . . ? C7A N5 C6A 114.2(11) . . ? C6B N5 C6A 29.2(7) . . ? C7B N5 C6A 124.1(15) . . ? C7A N5 Pr1 117.8(8) . . ? C6B N5 Pr1 117.3(12) . . ? C7B N5 Pr1 118.7(12) . . ? C6A N5 Pr1 117.2(8) . . ? C8 N6 Pr1 117.0(6) . . ? C8 N6 H6A 108.1 . . ? Pr1 N6 H6A 108.1 . . ? C8 N6 H6B 108.1 . . ? Pr1 N6 H6B 108.1 . . ? H6A N6 H6B 107.3 . . ? N1 C1 C2 109.0(10) . . ? N1 C1 H1C 109.9 . . ? C2 C1 H1C 109.9 . . ? N1 C1 H1D 109.9 . . ? C2 C1 H1D 109.9 . . ? H1C C1 H1D 108.3 . . ? C1 C2 N2 111.4(9) . . ? C1 C2 H2A 109.4 . . ? N2 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? N2 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N2 C3 C4 109.0(9) . . ? N2 C3 H3C 109.9 . . ? C4 C3 H3C 109.9 . . ? N2 C3 H3D 109.9 . . ? C4 C3 H3D 109.9 . . ? H3C C3 H3D 108.3 . . ? N3 C4 C3 112.6(9) . . ? N3 C4 H4C 109.1 . . ? C3 C4 H4C 109.1 . . ? N3 C4 H4D 109.1 . . ? C3 C4 H4D 109.1 . . ? H4C C4 H4D 107.8 . . ? N4 C5 C6A 115.8(12) . . ? N4 C5 C6B 119.9(13) . . ? C6A C5 C6B 29.0(7) . . ? C5 C6A N5 112.7(12) . . ? N5 C6B C5 113.9(16) . . ? N5 C7A C8 114.6(14) . . ? C8 C7B N5 114.2(14) . . ? C7B C8 N6 119.2(14) . . ? C7B C8 C7A 30.8(15) . . ? N6 C8 C7A 115.1(11) . . ? 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 S4 Sb1 S1 Pr1 -99.64(9) . . . . ? S3 Sb1 S1 Pr1 136.30(8) . . . . ? S2 Sb1 S1 Pr1 18.54(9) . . . . ? N4 Pr1 S1 Sb1 -96.5(2) . . . . ? N5 Pr1 S1 Sb1 -162.8(2) . . . . ? N3 Pr1 S1 Sb1 -45.7(3) . . . . ? N1 Pr1 S1 Sb1 65.7(2) . . . . ? N2 Pr1 S1 Sb1 56.0(3) . . . . ? N6 Pr1 S1 Sb1 136.14(19) . . . . ? S2 Pr1 S1 Sb1 -14.41(7) . . . . ? S3 Pr1 S1 Sb1 -147.03(8) 1_655 . . . ? S4 Sb1 S2 Pr1 98.46(9) . . . . ? S3 Sb1 S2 Pr1 -139.08(8) . . . . ? S1 Sb1 S2 Pr1 -18.52(10) . . . . ? N4 Pr1 S2 Sb1 95.2(2) . . . . ? N5 Pr1 S2 Sb1 55.3(3) . . . . ? N3 Pr1 S2 Sb1 170.5(2) . . . . ? N1 Pr1 S2 Sb1 -64.5(2) . . . . ? N2 Pr1 S2 Sb1 -127.0(2) . . . . ? N6 Pr1 S2 Sb1 -50.0(4) . . . . ? S1 Pr1 S2 Sb1 14.35(8) . . . . ? S3 Pr1 S2 Sb1 152.98(7) 1_655 . . . ? S4 Sb1 S3 Pr1 -5.31(14) . . . 1_455 ? S1 Sb1 S3 Pr1 118.49(11) . . . 1_455 ? S2 Sb1 S3 Pr1 -128.46(10) . . . 1_455 ? N4 Pr1 N1 C1 -119.2(8) . . . . ? N5 Pr1 N1 C1 150.9(7) . . . . ? N3 Pr1 N1 C1 -21.9(8) . . . . ? N2 Pr1 N1 C1 19.1(7) . . . . ? N6 Pr1 N1 C1 109.4(8) . . . . ? S1 Pr1 N1 C1 -153.7(8) . . . . ? S2 Pr1 N1 C1 -78.9(7) . . . . ? S3 Pr1 N1 C1 58.8(8) 1_655 . . . ? N4 Pr1 N2 C3 34.5(9) . . . . ? N5 Pr1 N2 C3 137.1(7) . . . . ? N3 Pr1 N2 C3 24.5(7) . . . . ? N1 Pr1 N2 C3 -114.7(7) . . . . ? N6 Pr1 N2 C3 172.1(7) . . . . ? S1 Pr1 N2 C3 -104.2(7) . . . . ? S2 Pr1 N2 C3 -40.4(7) . . . . ? S3 Pr1 N2 C3 91.3(7) 1_655 . . . ? N4 Pr1 N2 C2 161.2(6) . . . . ? N5 Pr1 N2 C2 -96.1(8) . . . . ? N3 Pr1 N2 C2 151.3(8) . . . . ? N1 Pr1 N2 C2 12.1(7) . . . . ? N6 Pr1 N2 C2 -61.2(7) . . . . ? S1 Pr1 N2 C2 22.5(8) . . . . ? S2 Pr1 N2 C2 86.4(7) . . . . ? S3 Pr1 N2 C2 -142.0(7) 1_655 . . . ? N4 Pr1 N3 C4 -166.2(8) . . . . ? N5 Pr1 N3 C4 -125.6(7) . . . . ? N1 Pr1 N3 C4 47.1(8) . . . . ? N2 Pr1 N3 C4 6.7(7) . . . . ? N6 Pr1 N3 C4 -41.5(9) . . . . ? S1 Pr1 N3 C4 141.0(6) . . . . ? S2 Pr1 N3 C4 108.8(7) . . . . ? S3 Pr1 N3 C4 -85.6(7) 1_655 . . . ? N5 Pr1 N4 C5 10.3(10) . . . . ? N3 Pr1 N4 C5 152.9(11) . . . . ? N1 Pr1 N4 C5 -97.3(11) . . . . ? N2 Pr1 N4 C5 143.4(10) . . . . ? N6 Pr1 N4 C5 20.0(12) . . . . ? S1 Pr1 N4 C5 -63.2(10) . . . . ? S2 Pr1 N4 C5 -137.1(11) . . . . ? S3 Pr1 N4 C5 84.1(10) 1_655 . . . ? N4 Pr1 N5 C7A 153.9(11) . . . . ? N3 Pr1 N5 C7A 110.2(10) . . . . ? N1 Pr1 N5 C7A -62.1(11) . . . . ? N2 Pr1 N5 C7A 21.8(12) . . . . ? N6 Pr1 N5 C7A -17.5(10) . . . . ? S1 Pr1 N5 C7A -120.0(11) . . . . ? S2 Pr1 N5 C7A -161.5(10) . . . . ? S3 Pr1 N5 C7A 71.3(10) 1_655 . . . ? N4 Pr1 N5 C6B -21.7(12) . . . . ? N3 Pr1 N5 C6B -65.3(13) . . . . ? N1 Pr1 N5 C6B 122.4(12) . . . . ? N2 Pr1 N5 C6B -153.7(12) . . . . ? N6 Pr1 N5 C6B 167.0(13) . . . . ? S1 Pr1 N5 C6B 64.5(13) . . . . ? S2 Pr1 N5 C6B 23.0(13) . . . . ? S3 Pr1 N5 C6B -104.2(13) 1_655 . . . ? N4 Pr1 N5 C7B -170.6(18) . . . . ? N3 Pr1 N5 C7B 145.7(18) . . . . ? N1 Pr1 N5 C7B -26.5(18) . . . . ? N2 Pr1 N5 C7B 57.4(19) . . . . ? N6 Pr1 N5 C7B 18.1(18) . . . . ? S1 Pr1 N5 C7B -84.4(18) . . . . ? S2 Pr1 N5 C7B -126.0(18) . . . . ? S3 Pr1 N5 C7B 106.9(18) 1_655 . . . ? N4 Pr1 N5 C6A 11.3(10) . . . . ? N3 Pr1 N5 C6A -32.3(11) . . . . ? N1 Pr1 N5 C6A 155.4(10) . . . . ? N2 Pr1 N5 C6A -120.7(10) . . . . ? N6 Pr1 N5 C6A -160.0(11) . . . . ? S1 Pr1 N5 C6A 97.5(11) . . . . ? S2 Pr1 N5 C6A 56.0(11) . . . . ? S3 Pr1 N5 C6A -71.2(10) 1_655 . . . ? N4 Pr1 N6 C8 -13.0(10) . . . . ? N5 Pr1 N6 C8 -3.2(9) . . . . ? N3 Pr1 N6 C8 -114.8(9) . . . . ? N1 Pr1 N6 C8 137.4(10) . . . . ? N2 Pr1 N6 C8 -157.8(10) . . . . ? S1 Pr1 N6 C8 63.4(9) . . . . ? S2 Pr1 N6 C8 122.6(9) . . . . ? S3 Pr1 N6 C8 -74.7(9) 1_655 . . . ? Pr1 N1 C1 C2 -48.3(11) . . . . ? N1 C1 C2 N2 60.0(12) . . . . ? C3 N2 C2 C1 83.5(12) . . . . ? Pr1 N2 C2 C1 -42.1(11) . . . . ? C2 N2 C3 C4 178.7(10) . . . . ? Pr1 N2 C3 C4 -54.0(11) . . . . ? Pr1 N3 C4 C3 -37.9(12) . . . . ? N2 C3 C4 N3 63.3(13) . . . . ? Pr1 N4 C5 C6A -31.5(19) . . . . ? Pr1 N4 C5 C6B 1(2) . . . . ? N4 C5 C6A N5 41(2) . . . . ? C6B C5 C6A N5 -65(2) . . . . ? C7A N5 C6A C5 -175.0(15) . . . . ? C6B N5 C6A C5 67(2) . . . . ? C7B N5 C6A C5 151(2) . . . . ? Pr1 N5 C6A C5 -31.2(19) . . . . ? C7A N5 C6B C5 -144.5(19) . . . . ? C7B N5 C6B C5 -180(2) . . . . ? C6A N5 C6B C5 -67(2) . . . . ? Pr1 N5 C6B C5 31(2) . . . . ? N4 C5 C6B N5 -21(3) . . . . ? C6A C5 C6B N5 69(2) . . . . ? C6B N5 C7A C8 -148.2(17) . . . . ? C7B N5 C7A C8 -63(2) . . . . ? C6A N5 C7A C8 -179.8(15) . . . . ? Pr1 N5 C7A C8 36.6(18) . . . . ? C7A N5 C7B C8 66(2) . . . . ? C6B N5 C7B C8 179(2) . . . . ? C6A N5 C7B C8 147(2) . . . . ? Pr1 N5 C7B C8 -31(4) . . . . ? N5 C7B C8 N6 28(4) . . . . ? N5 C7B C8 C7A -63(2) . . . . ? Pr1 N6 C8 C7B -12(2) . . . . ? Pr1 N6 C8 C7A 22.6(18) . . . . ? N5 C7A C8 C7B 66(2) . . . . ? N5 C7A C8 N6 -39(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6B S4 0.92 2.95 3.833(9) 162.4 8_656 N6 H6A S4 0.92 2.60 3.498(9) 166.1 1_655 N4 H4B S2 0.92 2.69 3.576(10) 163.0 6_676 N3 H3B S3 0.92 2.92 3.619(9) 133.9 6_676 N2 H2 S4 0.93 2.60 3.440(9) 150.4 1_655 N1 H1B S4 0.92 2.53 3.381(8) 153.1 8_656 N1 H1A S4 0.92 2.55 3.460(9) 171.5 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.808 _refine_diff_density_min -1.097 _refine_diff_density_rms 0.165 # Attachment 'cif of 1b.cif' data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 863637' #TrackingRef 'cif of 1b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H26 N6 Nd S4 Sb' _chemical_formula_sum 'C8 H26 N6 Nd S4 Sb' _chemical_formula_weight 600.58 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' Nd Nd -0.1943 3.0179 '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 orthorhombic _symmetry_space_group_name_H-M 'p bca' _symmetry_space_group_name_Hall '-p 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 8.6296(13) _cell_length_b 16.264(3) _cell_length_c 26.393(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3704.3(10) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 11648 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.35 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2328 _exptl_absorpt_coefficient_mu 4.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3341 _exptl_absorpt_correction_T_max 0.7353 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 34492 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3393 _reflns_number_gt 3253 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^+42.5276P] 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 3393 _refine_ls_number_parameters 200 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0818 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.138 _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 Sb1 Sb 0.99794(6) 0.23405(3) 0.620331(19) 0.01636(14) Uani 1 1 d . . . S1 S 0.8351(3) 0.33688(14) 0.65035(9) 0.0252(5) Uani 1 1 d . . . S2 S 0.8311(2) 0.16439(13) 0.56556(8) 0.0208(5) Uani 1 1 d . . . S3 S 1.2115(2) 0.28234(14) 0.57600(8) 0.0244(5) Uani 1 1 d . . . S4 S 1.0774(2) 0.15093(14) 0.68672(8) 0.0230(5) Uani 1 1 d . . . Nd1 Nd 0.55308(5) 0.24199(2) 0.616438(15) 0.01522(13) Uani 1 1 d . . . N1 N 0.4755(9) 0.1665(5) 0.5319(3) 0.0287(18) Uani 1 1 d . . . H1A H 0.4124 0.2005 0.5132 0.034 Uiso 1 1 calc R . . H1B H 0.5635 0.1566 0.5132 0.034 Uiso 1 1 calc R . . N2 N 0.4212(9) 0.0958(4) 0.6307(3) 0.0315(19) Uani 1 1 d . . . H2 H 0.3149 0.1041 0.6336 0.038 Uiso 1 1 calc R . . N3 N 0.6777(9) 0.1511(4) 0.6887(3) 0.0274(17) Uani 1 1 d . . . H3A H 0.7836 0.1567 0.6869 0.033 Uiso 1 1 calc R . . H3B H 0.6467 0.1720 0.7194 0.033 Uiso 1 1 calc R . . N4 N 0.4047(8) 0.2716(4) 0.7026(3) 0.0234(16) Uani 1 1 d . . . H4A H 0.3149 0.2411 0.7024 0.028 Uiso 1 1 calc R . . H4B H 0.4651 0.2521 0.7287 0.028 Uiso 1 1 calc R . . N5 N 0.4773(9) 0.3961(4) 0.6326(2) 0.0273(18) Uani 1 1 d D . . N6 N 0.6003(10) 0.3415(4) 0.5409(3) 0.0293(18) Uani 1 1 d . . . H6A H 0.7013 0.3349 0.5306 0.035 Uiso 1 1 calc R . . H6B H 0.5382 0.3245 0.5145 0.035 Uiso 1 1 calc R . . C1 C 0.3939(15) 0.0875(6) 0.5409(5) 0.051(3) Uani 1 1 d . . . H1C H 0.4096 0.0513 0.5112 0.062 Uiso 1 1 calc R . . H1D H 0.2814 0.0983 0.5439 0.062 Uiso 1 1 calc R . . C2 C 0.4472(14) 0.0432(7) 0.5875(4) 0.043(3) Uani 1 1 d . . . H2A H 0.3888 -0.0088 0.5915 0.052 Uiso 1 1 calc R . . H2B H 0.5588 0.0297 0.5846 0.052 Uiso 1 1 calc R . . C3 C 0.4767(13) 0.0541(6) 0.6794(4) 0.039(3) Uani 1 1 d . . . H3C H 0.4192 0.0772 0.7085 0.047 Uiso 1 1 calc R . . H3D H 0.4530 -0.0054 0.6775 0.047 Uiso 1 1 calc R . . C4 C 0.6415(14) 0.0648(7) 0.6877(4) 0.043(3) Uani 1 1 d . . . H4C H 0.6715 0.0392 0.7203 0.052 Uiso 1 1 calc R . . H4D H 0.7004 0.0375 0.6603 0.052 Uiso 1 1 calc R . . C5 C 0.3635(17) 0.3562(6) 0.7144(4) 0.040(4) Uani 1 1 d D . . C6A C 0.454(3) 0.4182(11) 0.6861(5) 0.036(6) Uani 0.48 1 d PD . . C6B C 0.363(2) 0.4158(10) 0.6716(6) 0.032(5) Uani 0.52 1 d PD . . C7A C 0.469(3) 0.4526(11) 0.5890(6) 0.034(7) Uani 0.48 1 d PD . . C7B C 0.545(3) 0.4585(9) 0.5994(5) 0.032(7) Uani 0.52 1 d PD . . C8 C 0.5748(17) 0.4265(6) 0.5478(4) 0.036(4) Uani 1 1 d 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 Sb1 0.0132(3) 0.0223(3) 0.0136(3) -0.0008(2) -0.0010(2) 0.0019(2) S1 0.0208(11) 0.0256(12) 0.0291(12) -0.0085(9) -0.0017(9) 0.0044(9) S2 0.0174(10) 0.0281(12) 0.0169(10) -0.0058(8) -0.0023(8) 0.0014(9) S3 0.0185(11) 0.0357(13) 0.0191(10) 0.0024(9) 0.0016(9) -0.0040(9) S4 0.0197(11) 0.0325(12) 0.0167(10) 0.0048(9) -0.0018(9) 0.0040(9) Nd1 0.0156(2) 0.0164(2) 0.0137(2) -0.00063(17) 0.00179(16) 0.00079(16) N1 0.019(4) 0.046(5) 0.021(4) -0.011(3) -0.001(3) 0.003(3) N2 0.025(4) 0.022(4) 0.048(5) -0.002(3) 0.011(4) -0.001(3) N3 0.031(4) 0.028(4) 0.022(4) 0.009(3) 0.012(3) 0.007(3) N4 0.021(4) 0.028(4) 0.022(4) 0.002(3) 0.001(3) 0.007(3) N5 0.045(5) 0.026(4) 0.011(4) 0.000(3) 0.003(3) 0.012(4) N6 0.038(5) 0.029(4) 0.021(4) 0.006(3) 0.009(4) 0.000(4) C1 0.066(8) 0.025(5) 0.063(8) -0.019(5) -0.009(7) 0.010(5) C2 0.047(7) 0.036(6) 0.047(7) -0.003(5) 0.000(5) -0.004(5) C3 0.044(7) 0.030(5) 0.043(6) 0.015(4) 0.007(5) 0.002(5) C4 0.063(8) 0.039(6) 0.028(5) 0.005(5) -0.005(5) 0.006(5) C5 0.055(12) 0.033(6) 0.033(6) 0.010(5) 0.016(7) 0.003(7) C6A 0.057(17) 0.026(12) 0.025(12) -0.012(9) 0.014(12) 0.002(12) C6B 0.039(14) 0.031(9) 0.027(12) 0.003(8) 0.023(11) -0.005(10) C7A 0.033(17) 0.026(10) 0.031(14) 0.012(9) 0.006(12) -0.007(11) C7B 0.033(14) 0.034(10) 0.035(16) 0.005(9) 0.019(11) -0.003(10) C8 0.048(12) 0.022(5) 0.029(6) 0.007(4) 0.014(7) 0.011(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 Sb1 S4 2.317(2) . ? Sb1 S3 2.320(2) . ? Sb1 S1 2.324(2) . ? Sb1 S2 2.334(2) . ? S1 Nd1 3.017(2) . ? S2 Nd1 3.025(2) . ? S3 Nd1 3.203(2) 1_655 ? Nd1 N6 2.601(7) . ? Nd1 N5 2.625(7) . ? Nd1 N1 2.633(7) . ? Nd1 N3 2.641(7) . ? Nd1 N4 2.653(7) . ? Nd1 N2 2.662(7) . ? Nd1 S3 3.203(2) 1_455 ? N1 C1 1.485(14) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C2 1.444(13) . ? N2 C3 1.530(12) . ? N2 H2 0.9300 . ? N3 C4 1.438(13) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? N4 C5 1.455(12) . ? N4 H4A 0.9200 . ? N4 H4B 0.9200 . ? N5 C7B 1.462(9) . ? N5 C6B 1.464(9) . ? N5 C6A 1.470(9) . ? N5 C7A 1.475(10) . ? N6 C8 1.411(12) . ? N6 H6A 0.9200 . ? N6 H6B 0.9200 . ? C1 C2 1.497(15) . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.450(15) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 H4C 0.9900 . ? C4 H4D 0.9900 . ? C5 C6A 1.476(10) . ? C5 C6B 1.487(9) . ? C7A C8 1.482(10) . ? C7B C8 1.481(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S4 Sb1 S3 110.10(8) . . ? S4 Sb1 S1 109.94(8) . . ? S3 Sb1 S1 114.13(8) . . ? S4 Sb1 S2 111.58(8) . . ? S3 Sb1 S2 110.01(8) . . ? S1 Sb1 S2 100.80(8) . . ? Sb1 S1 Nd1 91.06(7) . . ? Sb1 S2 Nd1 90.68(7) . . ? Sb1 S3 Nd1 119.59(8) . 1_655 ? N6 Nd1 N5 64.5(2) . . ? N6 Nd1 N1 71.3(2) . . ? N5 Nd1 N1 121.3(2) . . ? N6 Nd1 N3 146.9(3) . . ? N5 Nd1 N3 121.2(2) . . ? N1 Nd1 N3 117.0(2) . . ? N6 Nd1 N4 128.3(2) . . ? N5 Nd1 N4 64.4(2) . . ? N1 Nd1 N4 133.5(2) . . ? N3 Nd1 N4 71.3(2) . . ? N6 Nd1 N2 137.0(3) . . ? N5 Nd1 N2 136.3(2) . . ? N1 Nd1 N2 66.1(3) . . ? N3 Nd1 N2 64.7(3) . . ? N4 Nd1 N2 80.5(2) . . ? N6 Nd1 S1 77.46(19) . . ? N5 Nd1 S1 70.39(18) . . ? N1 Nd1 S1 134.02(17) . . ? N3 Nd1 S1 75.15(18) . . ? N4 Nd1 S1 92.42(17) . . ? N2 Nd1 S1 139.43(19) . . ? N6 Nd1 S2 78.18(18) . . ? N5 Nd1 S2 131.91(17) . . ? N1 Nd1 S2 68.35(17) . . ? N3 Nd1 S2 76.35(16) . . ? N4 Nd1 S2 147.01(16) . . ? N2 Nd1 S2 91.68(17) . . ? S1 Nd1 S2 72.87(6) . . ? N6 Nd1 S3 76.18(19) . 1_455 ? N5 Nd1 S3 68.25(18) . 1_455 ? N1 Nd1 S3 65.10(17) . 1_455 ? N3 Nd1 S3 136.88(17) . 1_455 ? N4 Nd1 S3 78.71(16) . 1_455 ? N2 Nd1 S3 80.59(18) . 1_455 ? S1 Nd1 S3 137.42(6) . 1_455 ? S2 Nd1 S3 131.87(6) . 1_455 ? C1 N1 Nd1 112.9(6) . . ? C1 N1 H1A 109.0 . . ? Nd1 N1 H1A 109.0 . . ? C1 N1 H1B 109.0 . . ? Nd1 N1 H1B 109.0 . . ? H1A N1 H1B 107.8 . . ? C2 N2 C3 110.5(8) . . ? C2 N2 Nd1 110.6(6) . . ? C3 N2 Nd1 112.4(6) . . ? C2 N2 H2 107.7 . . ? C3 N2 H2 107.7 . . ? Nd1 N2 H2 107.7 . . ? C4 N3 Nd1 116.5(6) . . ? C4 N3 H3A 108.2 . . ? Nd1 N3 H3A 108.2 . . ? C4 N3 H3B 108.2 . . ? Nd1 N3 H3B 108.2 . . ? H3A N3 H3B 107.3 . . ? C5 N4 Nd1 118.2(5) . . ? C5 N4 H4A 107.8 . . ? Nd1 N4 H4A 107.8 . . ? C5 N4 H4B 107.8 . . ? Nd1 N4 H4B 107.8 . . ? H4A N4 H4B 107.1 . . ? C7B N5 C6B 122.6(10) . . ? C7B N5 C6A 117.4(9) . . ? C6B N5 C6A 34.7(11) . . ? C7B N5 C7A 28.3(10) . . ? C6B N5 C7A 112.3(8) . . ? C6A N5 C7A 126.1(12) . . ? C7B N5 Nd1 117.8(8) . . ? C6B N5 Nd1 119.5(7) . . ? C6A N5 Nd1 115.1(9) . . ? C7A N5 Nd1 118.7(8) . . ? C8 N6 Nd1 119.0(5) . . ? C8 N6 H6A 107.6 . . ? Nd1 N6 H6A 107.6 . . ? C8 N6 H6B 107.6 . . ? Nd1 N6 H6B 107.6 . . ? H6A N6 H6B 107.0 . . ? N1 C1 C2 113.7(8) . . ? N1 C1 H1C 108.8 . . ? C2 C1 H1C 108.8 . . ? N1 C1 H1D 108.8 . . ? C2 C1 H1D 108.8 . . ? H1C C1 H1D 107.7 . . ? N2 C2 C1 108.4(9) . . ? N2 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? N2 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? C4 C3 N2 112.4(8) . . ? C4 C3 H3C 109.1 . . ? N2 C3 H3C 109.1 . . ? C4 C3 H3D 109.1 . . ? N2 C3 H3D 109.1 . . ? H3C C3 H3D 107.9 . . ? N3 C4 C3 109.5(9) . . ? N3 C4 H4C 109.8 . . ? C3 C4 H4C 109.8 . . ? N3 C4 H4D 109.8 . . ? C3 C4 H4D 109.8 . . ? H4C C4 H4D 108.2 . . ? N4 C5 C6A 114.1(11) . . ? N4 C5 C6B 117.1(9) . . ? C6A C5 C6B 34.3(10) . . ? N5 C6A C5 113.1(10) . . ? N5 C6B C5 112.8(9) . . ? N5 C7A C8 111.3(9) . . ? N5 C7B C8 112.1(9) . . ? N6 C8 C7B 119.4(10) . . ? N6 C8 C7A 118.2(11) . . ? C7B C8 C7A 28.0(10) . . ? 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 S4 Sb1 S1 Nd1 -99.70(8) . . . . ? S3 Sb1 S1 Nd1 136.02(7) . . . . ? S2 Sb1 S1 Nd1 18.18(8) . . . . ? S4 Sb1 S2 Nd1 98.54(8) . . . . ? S3 Sb1 S2 Nd1 -138.95(7) . . . . ? S1 Sb1 S2 Nd1 -18.13(8) . . . . ? S4 Sb1 S3 Nd1 -4.87(12) . . . 1_655 ? S1 Sb1 S3 Nd1 119.31(9) . . . 1_655 ? S2 Sb1 S3 Nd1 -128.25(9) . . . 1_655 ? Sb1 S1 Nd1 N6 -95.63(18) . . . . ? Sb1 S1 Nd1 N5 -162.74(16) . . . . ? Sb1 S1 Nd1 N1 -47.7(3) . . . . ? Sb1 S1 Nd1 N3 65.67(17) . . . . ? Sb1 S1 Nd1 N4 135.61(16) . . . . ? Sb1 S1 Nd1 N2 57.5(3) . . . . ? Sb1 S1 Nd1 S2 -14.32(7) . . . . ? Sb1 S1 Nd1 S3 -148.49(7) . . . 1_455 ? Sb1 S2 Nd1 N6 94.6(2) . . . . ? Sb1 S2 Nd1 N5 55.8(2) . . . . ? Sb1 S2 Nd1 N1 169.0(2) . . . . ? Sb1 S2 Nd1 N3 -64.14(19) . . . . ? Sb1 S2 Nd1 N4 -52.6(3) . . . . ? Sb1 S2 Nd1 N2 -127.56(19) . . . . ? Sb1 S2 Nd1 S1 14.26(7) . . . . ? Sb1 S2 Nd1 S3 153.59(6) . . . 1_455 ? N6 Nd1 N1 C1 -170.2(7) . . . . ? N5 Nd1 N1 C1 -127.6(6) . . . . ? N3 Nd1 N1 C1 44.7(7) . . . . ? N4 Nd1 N1 C1 -44.6(8) . . . . ? N2 Nd1 N1 C1 3.4(6) . . . . ? S1 Nd1 N1 C1 140.0(6) . . . . ? S2 Nd1 N1 C1 105.5(7) . . . . ? S3 Nd1 N1 C1 -87.1(6) 1_455 . . . ? N6 Nd1 N2 C2 35.9(8) . . . . ? N5 Nd1 N2 C2 137.9(6) . . . . ? N1 Nd1 N2 C2 26.8(6) . . . . ? N3 Nd1 N2 C2 -112.6(7) . . . . ? N4 Nd1 N2 C2 173.7(7) . . . . ? S1 Nd1 N2 C2 -103.8(7) . . . . ? S2 Nd1 N2 C2 -38.5(7) . . . . ? S3 Nd1 N2 C2 93.7(7) 1_455 . . . ? N6 Nd1 N2 C3 159.9(6) . . . . ? N5 Nd1 N2 C3 -98.1(6) . . . . ? N1 Nd1 N2 C3 150.9(7) . . . . ? N3 Nd1 N2 C3 11.5(6) . . . . ? N4 Nd1 N2 C3 -62.2(6) . . . . ? S1 Nd1 N2 C3 20.3(7) . . . . ? S2 Nd1 N2 C3 85.5(6) . . . . ? S3 Nd1 N2 C3 -142.3(6) 1_455 . . . ? N6 Nd1 N3 C4 -121.5(7) . . . . ? N5 Nd1 N3 C4 148.0(7) . . . . ? N1 Nd1 N3 C4 -24.3(7) . . . . ? N4 Nd1 N3 C4 105.7(7) . . . . ? N2 Nd1 N3 C4 17.6(7) . . . . ? S1 Nd1 N3 C4 -156.5(7) . . . . ? S2 Nd1 N3 C4 -80.9(7) . . . . ? S3 Nd1 N3 C4 57.3(7) 1_455 . . . ? N6 Nd1 N4 C5 -10.8(9) . . . . ? N5 Nd1 N4 C5 -1.7(8) . . . . ? N1 Nd1 N4 C5 -111.5(8) . . . . ? N3 Nd1 N4 C5 138.6(9) . . . . ? N2 Nd1 N4 C5 -155.1(9) . . . . ? S1 Nd1 N4 C5 65.1(8) . . . . ? S2 Nd1 N4 C5 126.7(8) . . . . ? S3 Nd1 N4 C5 -72.9(8) 1_455 . . . ? N6 Nd1 N5 C7B -19.4(11) . . . . ? N1 Nd1 N5 C7B -64.5(12) . . . . ? N3 Nd1 N5 C7B 123.5(11) . . . . ? N4 Nd1 N5 C7B 168.5(12) . . . . ? N2 Nd1 N5 C7B -151.7(11) . . . . ? S1 Nd1 N5 C7B 65.7(11) . . . . ? S2 Nd1 N5 C7B 23.5(12) . . . . ? S3 Nd1 N5 C7B -103.9(12) 1_455 . . . ? N6 Nd1 N5 C6B 156.5(11) . . . . ? N1 Nd1 N5 C6B 111.3(11) . . . . ? N3 Nd1 N5 C6B -60.7(11) . . . . ? N4 Nd1 N5 C6B -15.6(11) . . . . ? N2 Nd1 N5 C6B 24.2(12) . . . . ? S1 Nd1 N5 C6B -118.4(11) . . . . ? S2 Nd1 N5 C6B -160.6(11) . . . . ? S3 Nd1 N5 C6B 72.0(11) 1_455 . . . ? N6 Nd1 N5 C6A -164.6(11) . . . . ? N1 Nd1 N5 C6A 150.2(11) . . . . ? N3 Nd1 N5 C6A -21.8(12) . . . . ? N4 Nd1 N5 C6A 23.3(11) . . . . ? N2 Nd1 N5 C6A 63.1(12) . . . . ? S1 Nd1 N5 C6A -79.5(11) . . . . ? S2 Nd1 N5 C6A -121.8(11) . . . . ? S3 Nd1 N5 C6A 110.8(11) 1_455 . . . ? N6 Nd1 N5 C7A 12.8(12) . . . . ? N1 Nd1 N5 C7A -32.4(13) . . . . ? N3 Nd1 N5 C7A 155.6(12) . . . . ? N4 Nd1 N5 C7A -159.3(13) . . . . ? N2 Nd1 N5 C7A -119.5(13) . . . . ? S1 Nd1 N5 C7A 97.9(13) . . . . ? S2 Nd1 N5 C7A 55.7(13) . . . . ? S3 Nd1 N5 C7A -71.8(13) 1_455 . . . ? N5 Nd1 N6 C8 5.2(9) . . . . ? N1 Nd1 N6 C8 145.4(9) . . . . ? N3 Nd1 N6 C8 -103.4(9) . . . . ? N4 Nd1 N6 C8 14.3(10) . . . . ? N2 Nd1 N6 C8 136.7(9) . . . . ? S1 Nd1 N6 C8 -68.8(9) . . . . ? S2 Nd1 N6 C8 -143.7(9) . . . . ? S3 Nd1 N6 C8 77.4(9) 1_455 . . . ? Nd1 N1 C1 C2 -33.2(12) . . . . ? C3 N2 C2 C1 -178.9(9) . . . . ? Nd1 N2 C2 C1 -53.8(10) . . . . ? N1 C1 C2 N2 59.6(13) . . . . ? C2 N2 C3 C4 83.7(11) . . . . ? Nd1 N2 C3 C4 -40.4(10) . . . . ? Nd1 N3 C4 C3 -45.6(10) . . . . ? N2 C3 C4 N3 56.7(11) . . . . ? Nd1 N4 C5 C6A -19.7(16) . . . . ? Nd1 N4 C5 C6B 18.4(17) . . . . ? C7B N5 C6A C5 171.1(17) . . . . ? C6B N5 C6A C5 62.6(13) . . . . ? C7A N5 C6A C5 139.3(18) . . . . ? Nd1 N5 C6A C5 -44(2) . . . . ? N4 C5 C6A N5 41(2) . . . . ? C6B C5 C6A N5 -62.0(12) . . . . ? C7B N5 C6B C5 -153.7(16) . . . . ? C6A N5 C6B C5 -61.6(13) . . . . ? C7A N5 C6B C5 176.5(17) . . . . ? Nd1 N5 C6B C5 31(2) . . . . ? N4 C5 C6B N5 -32(2) . . . . ? C6A C5 C6B N5 62.1(12) . . . . ? C7B N5 C7A C8 67.9(14) . . . . ? C6B N5 C7A C8 -174.2(17) . . . . ? C6A N5 C7A C8 149.0(17) . . . . ? Nd1 N5 C7A C8 -28(2) . . . . ? C6B N5 C7B C8 -145.0(17) . . . . ? C6A N5 C7B C8 175.2(17) . . . . ? C7A N5 C7B C8 -68.8(14) . . . . ? Nd1 N5 C7B C8 31(2) . . . . ? Nd1 N6 C8 C7B 9.1(19) . . . . ? Nd1 N6 C8 C7A -23.0(18) . . . . ? N5 C7B C8 N6 -26(3) . . . . ? N5 C7B C8 C7A 69.3(14) . . . . ? N5 C7A C8 N6 33(3) . . . . ? N5 C7A C8 C7B -67.2(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4A S4 0.92 2.55 3.464(8) 170.4 1_455 N4 H4B S4 0.92 2.94 3.822(7) 161.6 8_557 N6 H6B S2 0.92 2.77 3.647(8) 158.6 6_566 N3 H3B S4 0.92 2.57 3.401(7) 150.3 8_557 N3 H3A S4 0.92 2.54 3.450(8) 171.7 . N1 H1B S3 0.92 2.86 3.599(8) 138.6 6_566 N1 H1B S2 0.92 2.69 3.195(8) 115.1 . N2 H2 S4 0.93 2.60 3.433(8) 149.8 1_455 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.913 _refine_diff_density_min -0.861 _refine_diff_density_rms 0.145 # Attachment 'cif of 1c.cif' data_shelxl3 _database_code_depnum_ccdc_archive 'CCDC 863638' #TrackingRef 'cif of 1c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H26 N6 S4 Sb Sm' _chemical_formula_sum 'C8 H26 N6 S4 Sb Sm' _chemical_formula_weight 606.69 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' Sb Sb -0.5866 1.5461 '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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 8.6501(5) _cell_length_b 16.2077(9) _cell_length_c 26.3582(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3695.4(4) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10826 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.35 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 5.060 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4310 _exptl_absorpt_correction_T_max 0.6316 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14709 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3375 _reflns_number_gt 3016 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0387P)^2^+22.8864P] 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 3375 _refine_ls_number_parameters 170 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.157 _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 Sb1 Sb 0.49555(6) 0.23444(3) 0.62035(2) 0.02337(17) Uani 1 1 d . . . S1 S 0.3286(2) 0.16405(14) 0.56588(8) 0.0284(5) Uani 1 1 d . . . S2 S 0.3323(3) 0.33666(14) 0.65084(9) 0.0340(5) Uani 1 1 d . . . S4 S 0.5765(2) 0.15114(14) 0.68677(9) 0.0315(5) Uani 1 1 d . . . S3 S 0.7080(2) 0.28357(15) 0.57586(9) 0.0339(5) Uani 1 1 d . . . Sm1 Sm 0.05379(5) 0.24201(2) 0.616601(16) 0.02257(15) Uani 1 1 d . . . N1 N -0.0239(10) 0.1691(5) 0.5321(3) 0.0489(15) Uani 1 1 d . . . H1A H -0.0853 0.2035 0.5138 0.059 Uiso 1 1 calc R . . H1B H 0.0629 0.1590 0.5136 0.059 Uiso 1 1 calc R . . N2 N -0.0789(9) 0.0978(4) 0.6307(3) 0.0366(19) Uani 1 1 d . . . H2 H -0.1837 0.1063 0.6338 0.044 Uiso 1 1 calc R . . N3 N 0.1771(9) 0.1518(5) 0.6883(3) 0.0366(18) Uani 1 1 d . . . H3A H 0.2817 0.1568 0.6861 0.044 Uiso 1 1 calc R . . H3B H 0.1478 0.1732 0.7187 0.044 Uiso 1 1 calc R . . N4 N 0.1035(9) 0.3403(4) 0.5411(3) 0.0374(19) Uani 1 1 d . . . H4A H 0.2049 0.3356 0.5325 0.045 Uiso 1 1 calc R . . H4B H 0.0472 0.3215 0.5144 0.045 Uiso 1 1 calc R . . N5 N -0.0253(9) 0.3946(4) 0.6319(3) 0.0330(18) Uani 1 1 d D . . N6 N -0.0941(8) 0.2698(4) 0.7018(3) 0.0323(17) Uani 1 1 d . . . H6A H -0.1812 0.2383 0.7016 0.039 Uiso 1 1 calc R . . H6B H -0.0337 0.2513 0.7276 0.039 Uiso 1 1 calc R . . C1 C -0.1084(12) 0.0888(6) 0.5411(4) 0.0489(15) Uani 1 1 d . . . H1C H -0.2194 0.1000 0.5442 0.059 Uiso 1 1 calc R . . H1D H -0.0935 0.0526 0.5117 0.059 Uiso 1 1 calc R . . C2 C -0.0533(13) 0.0452(7) 0.5881(4) 0.0489(15) Uani 1 1 d . . . H2A H -0.1100 -0.0066 0.5924 0.059 Uiso 1 1 calc R . . H2B H 0.0570 0.0324 0.5850 0.059 Uiso 1 1 calc R . . C3 C -0.0230(13) 0.0553(6) 0.6785(5) 0.054(3) Uani 1 1 d . . . H3C H -0.0807 0.0773 0.7075 0.064 Uiso 1 1 calc R . . H3D H -0.0462 -0.0037 0.6759 0.064 Uiso 1 1 calc R . . C4 C 0.1392(15) 0.0652(7) 0.6880(4) 0.054(3) Uani 1 1 d . . . H4C H 0.1989 0.0369 0.6616 0.065 Uiso 1 1 calc R . . H4D H 0.1658 0.0406 0.7208 0.065 Uiso 1 1 calc R . . C5 C 0.0706(16) 0.4258(6) 0.5468(4) 0.059(3) Uani 1 1 d D . . C6A C 0.046(3) 0.4564(12) 0.5989(7) 0.043(6) Uani 0.50 1 d PD . . C6B C -0.028(2) 0.4527(13) 0.5886(7) 0.043(6) Uani 0.50 1 d PD . . C7A C -0.047(3) 0.4136(12) 0.6854(6) 0.060(3) Uani 0.50 1 d PD . . C7B C -0.127(3) 0.4174(12) 0.6730(7) 0.060(3) Uani 0.50 1 d PD . . C8 C -0.1399(15) 0.3549(6) 0.7136(4) 0.060(3) Uani 1 1 d 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 Sb1 0.0211(3) 0.0283(3) 0.0207(3) -0.0006(2) -0.0008(2) 0.0016(2) S1 0.0251(10) 0.0344(12) 0.0257(12) -0.0056(9) -0.0026(9) 0.0009(9) S2 0.0316(11) 0.0315(12) 0.0388(14) -0.0097(10) -0.0035(10) 0.0066(9) S4 0.0272(11) 0.0381(12) 0.0292(12) 0.0073(10) -0.0029(9) 0.0032(9) S3 0.0287(12) 0.0453(14) 0.0278(12) 0.0018(10) 0.0016(9) -0.0062(10) Sm1 0.0238(2) 0.0226(2) 0.0213(2) -0.00023(17) 0.00296(16) 0.00068(16) N1 0.049(3) 0.047(3) 0.050(4) -0.011(3) -0.017(3) 0.002(3) N2 0.035(4) 0.028(4) 0.047(5) 0.000(3) 0.016(4) 0.000(3) N3 0.036(4) 0.039(5) 0.035(5) 0.011(4) 0.008(4) 0.009(3) N4 0.048(5) 0.032(4) 0.032(5) 0.006(3) 0.010(4) 0.002(4) N5 0.047(5) 0.031(4) 0.021(4) 0.000(3) 0.006(3) 0.014(3) N6 0.028(4) 0.039(4) 0.029(4) 0.002(3) -0.004(3) 0.000(3) C1 0.049(3) 0.047(3) 0.050(4) -0.011(3) -0.017(3) 0.002(3) C2 0.049(3) 0.047(3) 0.050(4) -0.011(3) -0.017(3) 0.002(3) C3 0.059(7) 0.036(6) 0.066(8) 0.021(5) 0.011(6) 0.006(5) C4 0.084(9) 0.046(7) 0.034(6) 0.004(5) 0.001(6) 0.013(6) C5 0.119(11) 0.029(5) 0.030(6) 0.002(4) 0.017(6) 0.013(6) C6A 0.043(14) 0.019(6) 0.066(11) 0.009(7) 0.030(11) -0.003(10) C6B 0.043(14) 0.019(6) 0.066(11) 0.009(7) 0.030(11) -0.003(10) C7A 0.098(9) 0.035(5) 0.046(6) 0.006(4) 0.027(6) 0.029(5) C7B 0.098(9) 0.035(5) 0.046(6) 0.006(4) 0.027(6) 0.029(5) C8 0.098(9) 0.035(5) 0.046(6) 0.006(4) 0.027(6) 0.029(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 S4 2.319(2) . ? Sb1 S2 2.320(2) . ? Sb1 S3 2.321(2) . ? Sb1 S1 2.334(2) . ? S1 Sm1 3.006(2) . ? S2 Sm1 2.995(2) . ? S3 Sm1 3.248(2) 1_655 ? Sm1 N4 2.585(7) . ? Sm1 N5 2.598(7) . ? Sm1 N1 2.609(8) . ? Sm1 N3 2.616(7) . ? Sm1 N6 2.623(7) . ? Sm1 N2 2.630(7) . ? Sm1 S3 3.248(2) 1_455 ? N1 C1 1.512(13) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 C2 1.428(13) . ? N2 C3 1.514(13) . ? N2 H2 0.9200 . ? N3 C4 1.442(13) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N4 C5 1.423(12) . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N5 C7B 1.443(15) . ? N5 C7A 1.455(16) . ? N5 C6A 1.464(16) . ? N5 C6B 1.481(16) . ? N6 C8 1.468(12) . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? C1 C2 1.503(15) . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.434(16) . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 H4C 0.9800 . ? C4 H4D 0.9800 . ? C5 C6B 1.459(16) . ? C5 C6A 1.476(17) . ? C7A C8 1.451(16) . ? C7B C8 1.480(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S4 Sb1 S2 109.75(9) . . ? S4 Sb1 S3 110.00(8) . . ? S2 Sb1 S3 114.32(9) . . ? S4 Sb1 S1 111.50(8) . . ? S2 Sb1 S1 100.70(8) . . ? S3 Sb1 S1 110.29(8) . . ? Sb1 S1 Sm1 90.59(7) . . ? Sb1 S2 Sm1 91.11(7) . . ? Sb1 S3 Sm1 119.40(9) . 1_655 ? N4 Sm1 N5 64.9(2) . . ? N4 Sm1 N1 70.4(3) . . ? N5 Sm1 N1 119.7(3) . . ? N4 Sm1 N3 146.4(2) . . ? N5 Sm1 N3 121.8(2) . . ? N1 Sm1 N3 117.9(3) . . ? N4 Sm1 N6 129.3(2) . . ? N5 Sm1 N6 64.8(2) . . ? N1 Sm1 N6 133.1(3) . . ? N3 Sm1 N6 71.1(2) . . ? N4 Sm1 N2 136.8(3) . . ? N5 Sm1 N2 135.2(2) . . ? N1 Sm1 N2 66.8(3) . . ? N3 Sm1 N2 65.1(3) . . ? N6 Sm1 N2 79.6(2) . . ? N4 Sm1 S2 77.43(19) . . ? N5 Sm1 S2 71.19(18) . . ? N1 Sm1 S2 134.1(2) . . ? N3 Sm1 S2 74.97(18) . . ? N6 Sm1 S2 92.67(17) . . ? N2 Sm1 S2 139.77(19) . . ? N4 Sm1 S1 77.60(17) . . ? N5 Sm1 S1 132.66(17) . . ? N1 Sm1 S1 68.5(2) . . ? N3 Sm1 S1 76.34(17) . . ? N6 Sm1 S1 147.01(16) . . ? N2 Sm1 S1 91.98(17) . . ? S2 Sm1 S1 73.33(6) . . ? N4 Sm1 S3 76.75(19) . 1_455 ? N5 Sm1 S3 67.13(18) . 1_455 ? N1 Sm1 S3 64.8(2) . 1_455 ? N3 Sm1 S3 136.88(17) . 1_455 ? N6 Sm1 S3 78.35(16) . 1_455 ? N2 Sm1 S3 80.17(18) . 1_455 ? S2 Sm1 S3 137.22(6) . 1_455 ? S1 Sm1 S3 131.94(6) . 1_455 ? C1 N1 Sm1 112.4(6) . . ? C1 N1 H1A 109.1 . . ? Sm1 N1 H1A 109.1 . . ? C1 N1 H1B 109.1 . . ? Sm1 N1 H1B 109.1 . . ? H1A N1 H1B 107.9 . . ? C2 N2 C3 109.5(8) . . ? C2 N2 Sm1 110.6(6) . . ? C3 N2 Sm1 112.5(6) . . ? C2 N2 H2 108.1 . . ? C3 N2 H2 108.1 . . ? Sm1 N2 H2 108.1 . . ? C4 N3 Sm1 116.6(6) . . ? C4 N3 H3A 108.1 . . ? Sm1 N3 H3A 108.1 . . ? C4 N3 H3B 108.1 . . ? Sm1 N3 H3B 108.1 . . ? H3A N3 H3B 107.3 . . ? C5 N4 Sm1 119.1(6) . . ? C5 N4 H4A 107.5 . . ? Sm1 N4 H4A 107.5 . . ? C5 N4 H4B 107.5 . . ? Sm1 N4 H4B 107.5 . . ? H4A N4 H4B 107.0 . . ? C7B N5 C7A 30.7(13) . . ? C7B N5 C6A 121.9(12) . . ? C7A N5 C6A 119.0(12) . . ? C7B N5 C6B 114.0(10) . . ? C7A N5 C6B 127.7(12) . . ? C6A N5 C6B 27.5(11) . . ? C7B N5 Sm1 121.4(8) . . ? C7A N5 Sm1 112.7(9) . . ? C6A N5 Sm1 116.6(9) . . ? C6B N5 Sm1 119.3(9) . . ? C8 N6 Sm1 118.4(6) . . ? C8 N6 H6A 107.7 . . ? Sm1 N6 H6A 107.7 . . ? C8 N6 H6B 107.7 . . ? Sm1 N6 H6B 107.7 . . ? H6A N6 H6B 107.1 . . ? C2 C1 N1 112.3(8) . . ? C2 C1 H1C 109.1 . . ? N1 C1 H1C 109.1 . . ? C2 C1 H1D 109.1 . . ? N1 C1 H1D 109.1 . . ? H1C C1 H1D 107.9 . . ? N2 C2 C1 108.6(9) . . ? N2 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? N2 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? C4 C3 N2 114.1(9) . . ? C4 C3 H3C 108.7 . . ? N2 C3 H3C 108.7 . . ? C4 C3 H3D 108.7 . . ? N2 C3 H3D 108.7 . . ? H3C C3 H3D 107.6 . . ? C3 C4 N3 109.3(9) . . ? C3 C4 H4C 109.8 . . ? N3 C4 H4C 109.8 . . ? C3 C4 H4D 109.8 . . ? N3 C4 H4D 109.8 . . ? H4C C4 H4D 108.3 . . ? N4 C5 C6B 119.1(11) . . ? N4 C5 C6A 117.0(11) . . ? C6B C5 C6A 27.6(11) . . ? N5 C6A C5 112.5(13) . . ? C5 C6B N5 112.6(13) . . ? C8 C7A N5 115.4(14) . . ? N5 C7B C8 114.4(12) . . ? C7A C8 N6 111.0(11) . . ? C7A C8 C7B 30.4(13) . . ? N6 C8 C7B 117.9(10) . . ? 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 S4 Sb1 S1 Sm1 98.90(8) . . . . ? S2 Sb1 S1 Sm1 -17.46(9) . . . . ? S3 Sb1 S1 Sm1 -138.57(7) . . . . ? S4 Sb1 S2 Sm1 -100.13(8) . . . . ? S3 Sb1 S2 Sm1 135.73(7) . . . . ? S1 Sb1 S2 Sm1 17.53(9) . . . . ? S4 Sb1 S3 Sm1 -4.44(13) . . . 1_655 ? S2 Sb1 S3 Sm1 119.56(10) . . . 1_655 ? S1 Sb1 S3 Sm1 -127.84(9) . . . 1_655 ? Sb1 S2 Sm1 N4 -94.50(18) . . . . ? Sb1 S2 Sm1 N5 -162.02(18) . . . . ? Sb1 S2 Sm1 N1 -48.5(3) . . . . ? Sb1 S2 Sm1 N3 66.06(18) . . . . ? Sb1 S2 Sm1 N6 135.73(17) . . . . ? Sb1 S2 Sm1 N2 58.8(3) . . . . ? Sb1 S2 Sm1 S1 -13.88(7) . . . . ? Sb1 S2 Sm1 S3 -148.59(7) . . . 1_455 ? Sb1 S1 Sm1 N4 94.2(2) . . . . ? Sb1 S1 Sm1 N5 56.6(2) . . . . ? Sb1 S1 Sm1 N1 167.8(2) . . . . ? Sb1 S1 Sm1 N3 -64.33(19) . . . . ? Sb1 S1 Sm1 N6 -54.4(3) . . . . ? Sb1 S1 Sm1 N2 -128.12(19) . . . . ? Sb1 S1 Sm1 S2 13.79(7) . . . . ? Sb1 S1 Sm1 S3 153.34(7) . . . 1_455 ? N4 Sm1 N1 C1 -170.5(7) . . . . ? N5 Sm1 N1 C1 -126.6(6) . . . . ? N3 Sm1 N1 C1 45.2(7) . . . . ? N6 Sm1 N1 C1 -44.5(8) . . . . ? N2 Sm1 N1 C1 3.4(6) . . . . ? S2 Sm1 N1 C1 141.3(6) . . . . ? S1 Sm1 N1 C1 105.5(6) . . . . ? S3 Sm1 N1 C1 -86.3(6) 1_455 . . . ? N4 Sm1 N2 C2 35.8(8) . . . . ? N5 Sm1 N2 C2 136.9(6) . . . . ? N1 Sm1 N2 C2 27.4(6) . . . . ? N3 Sm1 N2 C2 -112.1(7) . . . . ? N6 Sm1 N2 C2 173.9(7) . . . . ? S2 Sm1 N2 C2 -104.4(6) . . . . ? S1 Sm1 N2 C2 -38.2(6) . . . . ? S3 Sm1 N2 C2 94.1(6) 1_455 . . . ? N4 Sm1 N2 C3 158.5(6) . . . . ? N5 Sm1 N2 C3 -100.3(7) . . . . ? N1 Sm1 N2 C3 150.1(7) . . . . ? N3 Sm1 N2 C3 10.6(6) . . . . ? N6 Sm1 N2 C3 -63.3(6) . . . . ? S2 Sm1 N2 C3 18.4(7) . . . . ? S1 Sm1 N2 C3 84.6(6) . . . . ? S3 Sm1 N2 C3 -143.2(6) 1_455 . . . ? N4 Sm1 N3 C4 -121.8(7) . . . . ? N5 Sm1 N3 C4 146.3(7) . . . . ? N1 Sm1 N3 C4 -25.4(8) . . . . ? N6 Sm1 N3 C4 104.1(7) . . . . ? N2 Sm1 N3 C4 17.1(7) . . . . ? S2 Sm1 N3 C4 -157.7(7) . . . . ? S1 Sm1 N3 C4 -81.7(7) . . . . ? S3 Sm1 N3 C4 56.7(8) 1_455 . . . ? N5 Sm1 N4 C5 2.9(8) . . . . ? N1 Sm1 N4 C5 141.3(9) . . . . ? N3 Sm1 N4 C5 -107.4(9) . . . . ? N6 Sm1 N4 C5 11.1(10) . . . . ? N2 Sm1 N4 C5 133.1(8) . . . . ? S2 Sm1 N4 C5 -72.0(8) . . . . ? S1 Sm1 N4 C5 -147.4(8) . . . . ? S3 Sm1 N4 C5 73.6(8) 1_455 . . . ? N4 Sm1 N5 C7B 163.5(15) . . . . ? N1 Sm1 N5 C7B 117.4(15) . . . . ? N3 Sm1 N5 C7B -54.2(15) . . . . ? N6 Sm1 N5 C7B -9.5(15) . . . . ? N2 Sm1 N5 C7B 31.3(16) . . . . ? S2 Sm1 N5 C7B -111.9(15) . . . . ? S1 Sm1 N5 C7B -155.3(15) . . . . ? S3 Sm1 N5 C7B 77.9(15) 1_455 . . . ? N4 Sm1 N5 C7A -163.2(12) . . . . ? N1 Sm1 N5 C7A 150.6(11) . . . . ? N3 Sm1 N5 C7A -20.9(12) . . . . ? N6 Sm1 N5 C7A 23.7(11) . . . . ? N2 Sm1 N5 C7A 64.6(12) . . . . ? S2 Sm1 N5 C7A -78.6(11) . . . . ? S1 Sm1 N5 C7A -122.1(11) . . . . ? S3 Sm1 N5 C7A 111.2(11) 1_455 . . . ? N4 Sm1 N5 C6A -20.3(11) . . . . ? N1 Sm1 N5 C6A -66.5(11) . . . . ? N3 Sm1 N5 C6A 122.0(11) . . . . ? N6 Sm1 N5 C6A 166.6(11) . . . . ? N2 Sm1 N5 C6A -152.5(11) . . . . ? S2 Sm1 N5 C6A 64.2(11) . . . . ? S1 Sm1 N5 C6A 20.8(12) . . . . ? S3 Sm1 N5 C6A -105.9(11) 1_455 . . . ? N4 Sm1 N5 C6B 10.8(11) . . . . ? N1 Sm1 N5 C6B -35.4(12) . . . . ? N3 Sm1 N5 C6B 153.1(11) . . . . ? N6 Sm1 N5 C6B -162.3(12) . . . . ? N2 Sm1 N5 C6B -121.4(11) . . . . ? S2 Sm1 N5 C6B 95.4(11) . . . . ? S1 Sm1 N5 C6B 51.9(12) . . . . ? S3 Sm1 N5 C6B -74.8(11) 1_455 . . . ? N4 Sm1 N6 C8 -9.4(9) . . . . ? N5 Sm1 N6 C8 -1.3(7) . . . . ? N1 Sm1 N6 C8 -109.4(8) . . . . ? N3 Sm1 N6 C8 139.6(8) . . . . ? N2 Sm1 N6 C8 -153.3(8) . . . . ? S2 Sm1 N6 C8 66.5(8) . . . . ? S1 Sm1 N6 C8 129.4(7) . . . . ? S3 Sm1 N6 C8 -71.3(7) 1_455 . . . ? Sm1 N1 C1 C2 -33.1(11) . . . . ? C3 N2 C2 C1 -179.6(8) . . . . ? Sm1 N2 C2 C1 -55.1(9) . . . . ? N1 C1 C2 N2 60.1(12) . . . . ? C2 N2 C3 C4 84.5(11) . . . . ? Sm1 N2 C3 C4 -38.9(11) . . . . ? N2 C3 C4 N3 54.4(12) . . . . ? Sm1 N3 C4 C3 -43.5(11) . . . . ? Sm1 N4 C5 C6B -16.8(18) . . . . ? Sm1 N4 C5 C6A 14.5(16) . . . . ? C7B N5 C6A C5 -148.5(18) . . . . ? C7A N5 C6A C5 175.8(16) . . . . ? C6B N5 C6A C5 -68(2) . . . . ? Sm1 N5 C6A C5 35(2) . . . . ? N4 C5 C6A N5 -33(2) . . . . ? C6B C5 C6A N5 69(2) . . . . ? N4 C5 C6B N5 26(2) . . . . ? C6A C5 C6B N5 -68(2) . . . . ? C7B N5 C6B C5 -177.3(18) . . . . ? C7A N5 C6B C5 150.3(17) . . . . ? C6A N5 C6B C5 69(2) . . . . ? Sm1 N5 C6B C5 -23(2) . . . . ? C7B N5 C7A C8 66(2) . . . . ? C6A N5 C7A C8 170.8(16) . . . . ? C6B N5 C7A C8 139.3(16) . . . . ? Sm1 N5 C7A C8 -47(2) . . . . ? C7A N5 C7B C8 -63.1(19) . . . . ? C6A N5 C7B C8 -157.1(18) . . . . ? C6B N5 C7B C8 172.9(19) . . . . ? Sm1 N5 C7B C8 19(3) . . . . ? N5 C7A C8 N6 45(2) . . . . ? N5 C7A C8 C7B -65(2) . . . . ? Sm1 N6 C8 C7A -21.1(15) . . . . ? Sm1 N6 C8 C7B 11.4(19) . . . . ? N5 C7B C8 C7A 64.6(19) . . . . ? N5 C7B C8 N6 -19(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6B S4 0.91 2.94 3.809(8) 160.6 8_557 N6 H6A S4 0.91 2.56 3.461(8) 171.4 1_455 N4 H4B S1 0.91 2.85 3.690(9) 154.7 6_566 N3 H3B S4 0.91 2.59 3.407(8) 149.5 8_557 N3 H3A S4 0.91 2.55 3.455(8) 171.9 . N2 H2 S4 0.92 2.60 3.437(8) 150.8 1_455 N1 H1B S3 0.91 2.83 3.566(10) 138.9 6_566 N1 H1A S3 0.91 2.75 3.186(9) 110.6 1_455 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.345 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.241 # Attachment 'cif of 2a.cif' data_shelxl4 _database_code_depnum_ccdc_archive 'CCDC 863639' #TrackingRef 'cif of 2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H26 Eu N6 S4 Sb' _chemical_formula_sum 'C8 H26 Eu N6 S4 Sb' _chemical_formula_weight 608.30 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' Sb Sb -0.5866 1.5461 '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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 15.868(5) _cell_length_b 9.120(3) _cell_length_c 13.562(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.982(7) _cell_angle_gamma 90.00 _cell_volume 1855.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4447 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 5.253 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3420 _exptl_absorpt_correction_T_max 0.5062 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4460 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 25.35 _reflns_number_total 1677 _reflns_number_gt 1461 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0204P)^2^+11.9172P] 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 1677 _refine_ls_number_parameters 93 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _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 Sb1 Sb 0.5000 1.16289(6) 0.2500 0.01889(17) Uani 1 2 d S . . S1 S 0.39009(11) 1.00452(18) 0.14568(13) 0.0250(4) Uani 1 1 d . . . S2 S 0.43623(13) 1.2986(2) 0.35102(15) 0.0305(4) Uani 1 1 d . . . Eu1 Eu 0.5000 0.76842(5) 0.2500 0.01795(15) Uani 1 2 d S . . N1 N 0.4321(4) 0.6001(6) 0.0920(4) 0.0277(13) Uani 1 1 d . . . H1A H 0.4294 0.6517 0.0336 0.033 Uiso 1 1 calc R . . H1B H 0.4706 0.5244 0.0967 0.033 Uiso 1 1 calc R . . N2 N 0.3505(4) 0.6474(6) 0.2405(5) 0.0280(14) Uani 1 1 d . . . H2 H 0.3633 0.5551 0.2687 0.034 Uiso 1 1 calc R . . N3 N 0.4377(4) 0.8520(6) 0.3966(4) 0.0262(13) Uani 1 1 d . . . H3A H 0.4828 0.8498 0.4586 0.031 Uiso 1 1 calc R . . H3B H 0.4191 0.9467 0.3843 0.031 Uiso 1 1 calc R . . C1 C 0.3436(5) 0.5376(8) 0.0765(6) 0.0313(16) Uani 1 1 d . . . H1C H 0.3497 0.4371 0.1035 0.038 Uiso 1 1 calc R . . H1D H 0.3098 0.5342 0.0018 0.038 Uiso 1 1 calc R . . C2 C 0.2943(5) 0.6294(8) 0.1322(6) 0.0317(17) Uani 1 1 d . . . H2A H 0.2801 0.7255 0.0985 0.038 Uiso 1 1 calc R . . H2B H 0.2383 0.5812 0.1292 0.038 Uiso 1 1 calc R . . C3 C 0.3022(5) 0.7266(10) 0.3016(6) 0.039(2) Uani 1 1 d . . . H3C H 0.2762 0.8169 0.2651 0.047 Uiso 1 1 calc R . . H3D H 0.2536 0.6652 0.3081 0.047 Uiso 1 1 calc R . . C4 C 0.3634(5) 0.7628(10) 0.4059(6) 0.042(2) Uani 1 1 d . . . H4A H 0.3866 0.6723 0.4441 0.050 Uiso 1 1 calc R . . H4B H 0.3314 0.8172 0.4450 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 0.0221(3) 0.0162(3) 0.0182(3) 0.000 0.0064(3) 0.000 S1 0.0231(9) 0.0209(9) 0.0259(9) -0.0009(7) 0.0010(8) 0.0010(7) S2 0.0362(10) 0.0315(10) 0.0257(10) -0.0048(8) 0.0128(9) 0.0052(8) Eu1 0.0187(3) 0.0181(3) 0.0172(3) 0.000 0.0061(2) 0.000 N1 0.035(3) 0.024(3) 0.026(3) -0.005(3) 0.012(3) -0.006(3) N2 0.026(3) 0.031(3) 0.029(3) -0.007(3) 0.010(3) -0.007(3) N3 0.026(3) 0.032(3) 0.021(3) -0.004(3) 0.009(3) -0.007(3) C1 0.029(4) 0.032(4) 0.027(4) -0.006(3) 0.001(3) -0.007(4) C2 0.027(4) 0.031(4) 0.030(4) -0.004(3) -0.001(3) -0.003(3) C3 0.024(4) 0.055(5) 0.040(5) 0.000(4) 0.013(4) -0.010(4) C4 0.042(5) 0.058(6) 0.033(5) -0.012(4) 0.023(4) -0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 S2 2.3098(18) 2_655 ? Sb1 S2 2.3098(18) . ? Sb1 S1 2.3503(18) . ? Sb1 S1 2.3503(18) 2_655 ? S1 Eu1 2.8415(18) . ? Eu1 N1 2.570(5) . ? Eu1 N1 2.570(5) 2_655 ? Eu1 N2 2.581(6) . ? Eu1 N2 2.581(6) 2_655 ? Eu1 N3 2.605(5) 2_655 ? Eu1 N3 2.605(5) . ? Eu1 S1 2.8415(18) 2_655 ? N1 C1 1.466(9) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 C2 1.458(9) . ? N2 C3 1.487(9) . ? N2 H2 0.9200 . ? N3 C4 1.472(9) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? C1 C2 1.506(10) . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.469(11) . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? 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 S2 Sb1 S2 115.19(10) 2_655 . ? S2 Sb1 S1 110.78(7) 2_655 . ? S2 Sb1 S1 107.69(7) . . ? S2 Sb1 S1 107.69(7) 2_655 2_655 ? S2 Sb1 S1 110.78(7) . 2_655 ? S1 Sb1 S1 104.17(9) . 2_655 ? Sb1 S1 Eu1 87.18(6) . . ? N1 Eu1 N1 106.7(3) . 2_655 ? N1 Eu1 N2 64.76(17) . . ? N1 Eu1 N2 85.17(19) 2_655 . ? N1 Eu1 N2 85.17(19) . 2_655 ? N1 Eu1 N2 64.76(17) 2_655 2_655 ? N2 Eu1 N2 129.4(3) . 2_655 ? N1 Eu1 N3 72.49(18) . 2_655 ? N1 Eu1 N3 130.58(17) 2_655 2_655 ? N2 Eu1 N3 131.11(19) . 2_655 ? N2 Eu1 N3 65.96(17) 2_655 2_655 ? N1 Eu1 N3 130.58(17) . . ? N1 Eu1 N3 72.49(18) 2_655 . ? N2 Eu1 N3 65.96(17) . . ? N2 Eu1 N3 131.11(19) 2_655 . ? N3 Eu1 N3 146.0(3) 2_655 . ? N1 Eu1 S1 152.95(13) . 2_655 ? N1 Eu1 S1 90.83(14) 2_655 2_655 ? N2 Eu1 S1 138.95(13) . 2_655 ? N2 Eu1 S1 83.90(15) 2_655 2_655 ? N3 Eu1 S1 80.46(14) 2_655 2_655 ? N3 Eu1 S1 73.87(13) . 2_655 ? N1 Eu1 S1 90.83(14) . . ? N1 Eu1 S1 152.95(13) 2_655 . ? N2 Eu1 S1 83.90(14) . . ? N2 Eu1 S1 138.95(13) 2_655 . ? N3 Eu1 S1 73.87(13) 2_655 . ? N3 Eu1 S1 80.46(14) . . ? S1 Eu1 S1 81.47(7) 2_655 . ? C1 N1 Eu1 118.3(4) . . ? C1 N1 H1A 107.7 . . ? Eu1 N1 H1A 107.7 . . ? C1 N1 H1B 107.7 . . ? Eu1 N1 H1B 107.7 . . ? H1A N1 H1B 107.1 . . ? C2 N2 C3 111.0(6) . . ? C2 N2 Eu1 110.5(4) . . ? C3 N2 Eu1 113.4(4) . . ? C2 N2 H2 107.2 . . ? C3 N2 H2 107.2 . . ? Eu1 N2 H2 107.2 . . ? C4 N3 Eu1 114.7(4) . . ? C4 N3 H3A 108.6 . . ? Eu1 N3 H3A 108.6 . . ? C4 N3 H3B 108.6 . . ? Eu1 N3 H3B 108.6 . . ? H3A N3 H3B 107.6 . . ? N1 C1 C2 109.9(6) . . ? N1 C1 H1C 109.7 . . ? C2 C1 H1C 109.7 . . ? N1 C1 H1D 109.7 . . ? C2 C1 H1D 109.7 . . ? H1C C1 H1D 108.2 . . ? N2 C2 C1 108.7(6) . . ? N2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? N2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C4 C3 N2 110.3(6) . . ? C4 C3 H3C 109.6 . . ? N2 C3 H3C 109.6 . . ? C4 C3 H3D 109.6 . . ? N2 C3 H3D 109.6 . . ? H3C C3 H3D 108.1 . . ? C3 C4 N3 109.8(6) . . ? C3 C4 H4A 109.7 . . ? N3 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? N3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? 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 S2 Sb1 S1 Eu1 115.53(6) 2_655 . . . ? S2 Sb1 S1 Eu1 -117.68(6) . . . . ? S1 Sb1 S1 Eu1 0.0 2_655 . . . ? Sb1 S1 Eu1 N1 -153.96(13) . . . . ? Sb1 S1 Eu1 N1 74.8(3) . . . 2_655 ? Sb1 S1 Eu1 N2 141.53(13) . . . . ? Sb1 S1 Eu1 N2 -70.4(2) . . . 2_655 ? Sb1 S1 Eu1 N3 -82.47(15) . . . 2_655 ? Sb1 S1 Eu1 N3 74.95(13) . . . . ? Sb1 S1 Eu1 S1 0.0 . . . 2_655 ? N1 Eu1 N1 C1 81.4(5) 2_655 . . . ? N2 Eu1 N1 C1 5.2(5) . . . . ? N2 Eu1 N1 C1 143.2(5) 2_655 . . . ? N3 Eu1 N1 C1 -150.5(5) 2_655 . . . ? N3 Eu1 N1 C1 0.4(6) . . . . ? S1 Eu1 N1 C1 -150.4(4) 2_655 . . . ? S1 Eu1 N1 C1 -77.7(5) . . . . ? N1 Eu1 N2 C2 -33.0(4) . . . . ? N1 Eu1 N2 C2 -143.9(5) 2_655 . . . ? N2 Eu1 N2 C2 -92.5(4) 2_655 . . . ? N3 Eu1 N2 C2 -1.5(6) 2_655 . . . ? N3 Eu1 N2 C2 143.1(5) . . . . ? S1 Eu1 N2 C2 130.4(4) 2_655 . . . ? S1 Eu1 N2 C2 60.8(4) . . . . ? N1 Eu1 N2 C3 -158.3(6) . . . . ? N1 Eu1 N2 C3 90.7(5) 2_655 . . . ? N2 Eu1 N2 C3 142.2(5) 2_655 . . . ? N3 Eu1 N2 C3 -126.9(5) 2_655 . . . ? N3 Eu1 N2 C3 17.7(5) . . . . ? S1 Eu1 N2 C3 5.0(6) 2_655 . . . ? S1 Eu1 N2 C3 -64.5(5) . . . . ? N1 Eu1 N3 C4 16.9(6) . . . . ? N1 Eu1 N3 C4 -80.3(5) 2_655 . . . ? N2 Eu1 N3 C4 12.2(5) . . . . ? N2 Eu1 N3 C4 -110.0(5) 2_655 . . . ? N3 Eu1 N3 C4 141.0(5) 2_655 . . . ? S1 Eu1 N3 C4 -176.4(5) 2_655 . . . ? S1 Eu1 N3 C4 99.8(5) . . . . ? Eu1 N1 C1 C2 22.1(8) . . . . ? C3 N2 C2 C1 -175.1(6) . . . . ? Eu1 N2 C2 C1 58.2(6) . . . . ? N1 C1 C2 N2 -52.6(8) . . . . ? C2 N2 C3 C4 -171.7(6) . . . . ? Eu1 N2 C3 C4 -46.7(8) . . . . ? N2 C3 C4 N3 57.9(9) . . . . ? Eu1 N3 C4 C3 -41.0(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A S2 0.91 2.83 3.627(6) 147.4 5_676 N2 H2 S2 0.92 2.69 3.590(7) 167.6 1_545 N1 H1B S2 0.91 2.50 3.387(6) 165.1 2_645 N1 H1A S2 0.91 2.55 3.417(6) 158.5 6_575 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.246 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.151 # Attachment 'cif of 2b.cif' data_shelxl5 _database_code_depnum_ccdc_archive 'CCDC 863640' #TrackingRef 'cif of 2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H26 Dy N6 S4 Sb' _chemical_formula_sum 'C8 H26 Dy N6 S4 Sb' _chemical_formula_weight 618.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 15.820(3) _cell_length_b 9.1718(14) _cell_length_c 13.531(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.997(4) _cell_angle_gamma 90.00 _cell_volume 1856.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3562 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 5.898 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2013 _exptl_absorpt_correction_T_max 0.3850 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _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 8443 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 25.35 _reflns_number_total 1681 _reflns_number_gt 1601 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _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^)+(0.0373P)^2^+4.3233P] 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 1681 _refine_ls_number_parameters 93 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0259 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0627 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 Sb1 Sb 0.5000 0.33911(4) 0.7500 0.02046(12) Uani 1 2 d S . . S1 S 0.60971(7) 0.49743(12) 0.85426(9) 0.0278(2) Uani 1 1 d . . . S2 S 0.56413(8) 0.20351(14) 0.64911(9) 0.0346(3) Uani 1 1 d . . . Dy1 Dy 0.5000 0.72887(3) 0.7500 0.01864(11) Uani 1 2 d S . . N1 N 0.5632(3) 0.6438(4) 0.6062(3) 0.0330(9) Uani 1 1 d . . . H1A H 0.5828 0.5515 0.6199 0.040 Uiso 1 1 calc R . . H1B H 0.5186 0.6436 0.5446 0.040 Uiso 1 1 calc R . . N2 N 0.6460(2) 0.8516(5) 0.7587(3) 0.0351(9) Uani 1 1 d . . . H2 H 0.6325 0.9419 0.7302 0.042 Uiso 1 1 calc R . . N3 N 0.5633(3) 0.8965(4) 0.9054(3) 0.0336(9) Uani 1 1 d . . . H3A H 0.5249 0.9711 0.8987 0.040 Uiso 1 1 calc R . . H3B H 0.5645 0.8469 0.9632 0.040 Uiso 1 1 calc R . . C1 C 0.6370(4) 0.7344(7) 0.5959(5) 0.0511(15) Uani 1 1 d . . . H1C H 0.6697 0.6808 0.5583 0.061 Uiso 1 1 calc R . . H1D H 0.6130 0.8220 0.5566 0.061 Uiso 1 1 calc R . . C2 C 0.6970(4) 0.7739(7) 0.6993(5) 0.0519(15) Uani 1 1 d . . . H2A H 0.7443 0.8364 0.6926 0.062 Uiso 1 1 calc R . . H2B H 0.7242 0.6867 0.7369 0.062 Uiso 1 1 calc R . . C3 C 0.7027(3) 0.8706(6) 0.8673(4) 0.0402(11) Uani 1 1 d . . . H3C H 0.7575 0.9202 0.8698 0.048 Uiso 1 1 calc R . . H3D H 0.7181 0.7763 0.9007 0.048 Uiso 1 1 calc R . . C4 C 0.6531(3) 0.9585(5) 0.9231(4) 0.0390(12) Uani 1 1 d . . . H4A H 0.6861 0.9593 0.9974 0.047 Uiso 1 1 calc R . . H4B H 0.6477 1.0583 0.8981 0.047 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 0.0228(2) 0.0161(2) 0.0225(2) 0.000 0.00743(15) 0.000 S1 0.0216(5) 0.0251(5) 0.0300(6) -0.0009(5) -0.0006(4) 0.0012(4) S2 0.0408(7) 0.0344(6) 0.0326(6) -0.0054(5) 0.0174(5) 0.0045(5) Dy1 0.01716(16) 0.01831(17) 0.02066(17) 0.000 0.00644(11) 0.000 N1 0.037(2) 0.035(2) 0.0315(19) -0.0074(16) 0.0181(17) -0.0010(17) N2 0.032(2) 0.043(2) 0.0327(19) -0.0050(17) 0.0125(16) -0.0129(17) N3 0.039(2) 0.034(2) 0.0305(19) -0.0061(16) 0.0143(16) -0.0054(17) C1 0.050(3) 0.063(4) 0.054(4) -0.011(3) 0.035(3) -0.014(3) C2 0.031(3) 0.082(4) 0.051(3) -0.009(3) 0.025(3) -0.015(3) C3 0.024(2) 0.042(3) 0.047(3) -0.007(2) 0.001(2) -0.003(2) C4 0.033(3) 0.043(3) 0.033(3) -0.011(2) 0.001(2) -0.007(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 S2 2.3112(12) 2_656 ? Sb1 S2 2.3112(12) . ? Sb1 S1 2.3489(11) . ? Sb1 S1 2.3489(11) 2_656 ? S1 Dy1 2.8132(12) . ? Dy1 N3 2.533(4) . ? Dy1 N3 2.533(4) 2_656 ? Dy1 N2 2.537(4) . ? Dy1 N2 2.537(4) 2_656 ? Dy1 N1 2.581(3) . ? Dy1 N1 2.581(3) 2_656 ? Dy1 S1 2.8132(12) 2_656 ? N1 C1 1.475(6) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C3 1.461(6) . ? N2 C2 1.492(7) . ? N2 H2 0.9100 . ? N3 C4 1.476(6) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? C1 C2 1.458(8) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.490(7) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 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 S2 Sb1 S2 114.89(7) 2_656 . ? S2 Sb1 S1 111.01(4) 2_656 . ? S2 Sb1 S1 107.87(4) . . ? S2 Sb1 S1 107.87(4) 2_656 2_656 ? S2 Sb1 S1 111.01(4) . 2_656 ? S1 Sb1 S1 103.63(6) . 2_656 ? Sb1 S1 Dy1 87.17(4) . . ? N3 Dy1 N3 105.26(19) . 2_656 ? N3 Dy1 N2 65.45(12) . . ? N3 Dy1 N2 82.94(13) 2_656 . ? N3 Dy1 N2 82.94(13) . 2_656 ? N3 Dy1 N2 65.45(12) 2_656 2_656 ? N2 Dy1 N2 127.3(2) . 2_656 ? N3 Dy1 N1 131.59(12) . . ? N3 Dy1 N1 72.72(12) 2_656 . ? N2 Dy1 N1 66.35(12) . . ? N2 Dy1 N1 132.01(12) 2_656 . ? N3 Dy1 N1 72.72(12) . 2_656 ? N3 Dy1 N1 131.59(12) 2_656 2_656 ? N2 Dy1 N1 132.01(12) . 2_656 ? N2 Dy1 N1 66.35(12) 2_656 2_656 ? N1 Dy1 N1 144.82(18) . 2_656 ? N3 Dy1 S1 152.48(9) . 2_656 ? N3 Dy1 S1 91.67(10) 2_656 2_656 ? N2 Dy1 S1 139.61(9) . 2_656 ? N2 Dy1 S1 84.71(10) 2_656 2_656 ? N1 Dy1 S1 73.80(9) . 2_656 ? N1 Dy1 S1 79.80(9) 2_656 2_656 ? N3 Dy1 S1 91.67(10) . . ? N3 Dy1 S1 152.48(9) 2_656 . ? N2 Dy1 S1 84.71(10) . . ? N2 Dy1 S1 139.61(9) 2_656 . ? N1 Dy1 S1 79.80(9) . . ? N1 Dy1 S1 73.80(9) 2_656 . ? S1 Dy1 S1 82.03(5) 2_656 . ? C1 N1 Dy1 114.4(3) . . ? C1 N1 H1A 108.7 . . ? Dy1 N1 H1A 108.7 . . ? C1 N1 H1B 108.7 . . ? Dy1 N1 H1B 108.7 . . ? H1A N1 H1B 107.6 . . ? C3 N2 C2 109.6(4) . . ? C3 N2 Dy1 110.6(3) . . ? C2 N2 Dy1 114.0(3) . . ? C3 N2 H2 107.5 . . ? C2 N2 H2 107.5 . . ? Dy1 N2 H2 107.5 . . ? C4 N3 Dy1 117.9(3) . . ? C4 N3 H3A 107.8 . . ? Dy1 N3 H3A 107.8 . . ? C4 N3 H3B 107.8 . . ? Dy1 N3 H3B 107.8 . . ? H3A N3 H3B 107.2 . . ? C2 C1 N1 109.7(5) . . ? C2 C1 H1C 109.7 . . ? N1 C1 H1C 109.7 . . ? C2 C1 H1D 109.7 . . ? N1 C1 H1D 109.7 . . ? H1C C1 H1D 108.2 . . ? C1 C2 N2 109.7(5) . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? N2 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C4 108.8(4) . . ? N2 C3 H3C 109.9 . . ? C4 C3 H3C 109.9 . . ? N2 C3 H3D 109.9 . . ? C4 C3 H3D 109.9 . . ? H3C C3 H3D 108.3 . . ? N3 C4 C3 110.3(4) . . ? N3 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N3 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? 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 S2 Sb1 S1 Dy1 -115.55(4) 2_656 . . . ? S2 Sb1 S1 Dy1 117.76(4) . . . . ? S1 Sb1 S1 Dy1 0.0 2_656 . . . ? Sb1 S1 Dy1 N3 153.10(9) . . . . ? Sb1 S1 Dy1 N3 -78.2(2) . . . 2_656 ? Sb1 S1 Dy1 N2 -141.75(9) . . . . ? Sb1 S1 Dy1 N2 72.05(15) . . . 2_656 ? Sb1 S1 Dy1 N1 -74.87(9) . . . . ? Sb1 S1 Dy1 N1 81.63(10) . . . 2_656 ? Sb1 S1 Dy1 S1 0.0 . . . 2_656 ? N3 Dy1 N1 C1 -17.7(4) . . . . ? N3 Dy1 N1 C1 77.6(4) 2_656 . . . ? N2 Dy1 N1 C1 -12.1(4) . . . . ? N2 Dy1 N1 C1 107.7(4) 2_656 . . . ? N1 Dy1 N1 C1 -142.4(4) 2_656 . . . ? S1 Dy1 N1 C1 174.6(4) 2_656 . . . ? S1 Dy1 N1 C1 -100.8(4) . . . . ? N3 Dy1 N2 C3 33.7(3) . . . . ? N3 Dy1 N2 C3 144.1(3) 2_656 . . . ? N2 Dy1 N2 C3 92.5(3) 2_656 . . . ? N1 Dy1 N2 C3 -141.7(3) . . . . ? N1 Dy1 N2 C3 2.0(4) 2_656 . . . ? S1 Dy1 N2 C3 -131.7(3) 2_656 . . . ? S1 Dy1 N2 C3 -60.6(3) . . . . ? N3 Dy1 N2 C2 157.7(4) . . . . ? N3 Dy1 N2 C2 -91.9(4) 2_656 . . . ? N2 Dy1 N2 C2 -143.5(4) 2_656 . . . ? N1 Dy1 N2 C2 -17.7(3) . . . . ? N1 Dy1 N2 C2 126.0(3) 2_656 . . . ? S1 Dy1 N2 C2 -7.6(4) 2_656 . . . ? S1 Dy1 N2 C2 63.5(4) . . . . ? N3 Dy1 N3 C4 -81.7(3) 2_656 . . . ? N2 Dy1 N3 C4 -7.1(3) . . . . ? N2 Dy1 N3 C4 -143.8(3) 2_656 . . . ? N1 Dy1 N3 C4 -1.5(4) . . . . ? N1 Dy1 N3 C4 148.8(4) 2_656 . . . ? S1 Dy1 N3 C4 152.2(3) 2_656 . . . ? S1 Dy1 N3 C4 76.3(3) . . . . ? Dy1 N1 C1 C2 41.0(6) . . . . ? N1 C1 C2 N2 -57.3(6) . . . . ? C3 N2 C2 C1 171.1(5) . . . . ? Dy1 N2 C2 C1 46.6(6) . . . . ? C2 N2 C3 C4 175.6(4) . . . . ? Dy1 N2 C3 C4 -57.9(4) . . . . ? Dy1 N3 C4 C3 -19.7(5) . . . . ? N2 C3 C4 N3 50.5(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3B S2 0.90 2.56 3.419(4) 160.0 6_566 N3 H3A S2 0.90 2.52 3.401(4) 166.3 2_666 N2 H2 S2 0.91 2.71 3.612(5) 170.0 1_565 N1 H1B S2 0.90 2.88 3.664(4) 145.9 5_666 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.978 _refine_diff_density_min -1.110 _refine_diff_density_rms 0.134