# 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_name 'Jian Zhou' _publ_contact_author_email jianzhou888888@163.com _publ_author_name 'Jian Zhou' # Attachment '- 5.CIF' data_5 _database_code_depnum_ccdc_archive 'CCDC 844290' #TrackingRef '- 5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H48 Eu2 N10 O2 S8 Sb2, 2(C16 H47 Eu2 N10 O S3 Sb), 2(Cl)' _chemical_formula_sum 'C48 H142 Cl2 Eu6 N30 O4 S14 Sb4 ' _chemical_formula_weight 3122.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 41.616(8) _cell_length_b 15.670(3) _cell_length_c 15.670(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10219(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.90 _cell_measurement_theta_max 25.09 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6032 _exptl_absorpt_coefficient_mu 5.051 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5038 _exptl_absorpt_correction_T_max 0.6810 _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 39442 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.0955 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.09 _reflns_number_total 8735 _reflns_number_gt 5321 _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^)+(0.0218P)^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 8735 _refine_ls_number_parameters 487 _refine_ls_number_restraints 658 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 0.897 _refine_ls_restrained_S_all 0.904 _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 Sb2 Sb 0.429154(14) 0.62657(4) 0.21447(4) 0.02876(15) Uani 1 1 d . . . Sb1 Sb 0.248852(14) 0.49188(4) 0.42198(4) 0.04149(17) Uani 1 1 d . . . Eu3 Eu 0.496011(10) 0.44476(3) 0.10601(3) 0.02550(11) Uani 1 1 d . . . Eu2 Eu 0.326668(11) 0.59014(3) 0.49742(3) 0.02611(11) Uani 1 1 d . . . Eu1 Eu 0.326541(11) 0.40752(3) 0.32024(3) 0.02891(12) Uani 1 1 d . . . Cl1 Cl 0.38071(7) 0.21685(17) 0.12226(19) 0.0633(8) Uani 1 1 d . . . S7 S 0.38306(6) 0.70807(16) 0.19723(18) 0.0512(7) Uani 1 1 d . . . S6 S 0.47519(6) 0.70845(14) 0.18962(15) 0.0376(6) Uani 1 1 d . . . S5 S 0.42833(6) 0.56493(16) 0.34893(15) 0.0414(6) Uani 1 1 d . . . S4 S 0.42974(5) 0.50888(14) 0.12020(14) 0.0342(5) Uani 1 1 d . . . S3 S 0.26548(6) 0.4761(2) 0.27714(18) 0.0586(8) Uani 1 1 d . . . S2 S 0.26374(6) 0.63663(16) 0.45111(19) 0.0494(7) Uani 1 1 d . . . S1 S 0.29565(6) 0.42354(15) 0.48667(15) 0.0363(6) Uani 1 1 d . . . C1 C 0.4688(2) 0.2311(6) 0.0929(6) 0.047(2) Uani 1 1 d U . . H1C H 0.4555 0.1909 0.0619 0.057 Uiso 1 1 calc R . . H1D H 0.4686 0.2152 0.1527 0.057 Uiso 1 1 calc R . . C2 C 0.5025(2) 0.2280(6) 0.0593(6) 0.049(2) Uani 1 1 d U . . H2B H 0.5024 0.2386 -0.0017 0.058 Uiso 1 1 calc R . . H2C H 0.5115 0.1717 0.0690 0.058 Uiso 1 1 calc R . . C3 C 0.5566(2) 0.2977(7) 0.0699(7) 0.052(2) Uani 1 1 d U . . H3B H 0.5563 0.3062 0.0085 0.062 Uiso 1 1 calc R . . H3C H 0.5675 0.2443 0.0817 0.062 Uiso 1 1 calc R . . C4 C 0.5742(2) 0.3710(7) 0.1128(7) 0.0526(19) Uani 1 1 d U . . H4B H 0.5742 0.3629 0.1741 0.063 Uiso 1 1 calc R . . H4C H 0.5963 0.3727 0.0933 0.063 Uiso 1 1 calc R . . C5 C 0.5737(3) 0.5266(7) 0.1310(6) 0.057(2) Uani 1 1 d DU . . H5C H 0.5967 0.5172 0.1346 0.069 Uiso 1 1 calc R . . H5D H 0.5699 0.5771 0.0966 0.069 Uiso 1 1 calc R . . C6 C 0.5605(2) 0.5388(7) 0.2156(6) 0.056(2) Uani 1 1 d DU . . H6C H 0.5682 0.5930 0.2374 0.068 Uiso 1 1 calc R . . H6D H 0.5690 0.4944 0.2524 0.068 Uiso 1 1 calc R . . C7 C 0.5154(2) 0.5219(6) 0.3110(6) 0.049(2) Uani 1 1 d U . . H7B H 0.5322 0.5407 0.3496 0.059 Uiso 1 1 calc R . . H7C H 0.4963 0.5554 0.3229 0.059 Uiso 1 1 calc R . . C8 C 0.5085(2) 0.4324(6) 0.3270(6) 0.050(2) Uani 1 1 d U . . H8B H 0.4996 0.4261 0.3838 0.060 Uiso 1 1 calc R . . H8C H 0.5283 0.3998 0.3243 0.060 Uiso 1 1 calc R . . C9 C 0.4072(2) 0.5936(6) 0.5712(6) 0.0380(19) Uani 1 1 d U . . H9B H 0.4073 0.6145 0.6295 0.046 Uiso 1 1 calc R . . H9C H 0.4290 0.5971 0.5493 0.046 Uiso 1 1 calc R . . C10 C 0.3962(2) 0.5026(6) 0.5698(5) 0.0367(17) Uani 1 1 d U . . H10C H 0.3989 0.4794 0.5129 0.044 Uiso 1 1 calc R . . H10D H 0.4092 0.4691 0.6088 0.044 Uiso 1 1 calc R . . C11 C 0.3561(2) 0.5074(7) 0.6862(5) 0.0406(17) Uani 1 1 d U . . H11C H 0.3661 0.5598 0.7056 0.049 Uiso 1 1 calc R . . H11D H 0.3654 0.4602 0.7177 0.049 Uiso 1 1 calc R . . C12 C 0.3199(2) 0.5111(6) 0.7021(6) 0.0407(18) Uani 1 1 d U . . H12B H 0.3103 0.4573 0.6852 0.049 Uiso 1 1 calc R . . H12C H 0.3160 0.5189 0.7626 0.049 Uiso 1 1 calc R . . C13 C 0.3070(2) 0.6643(6) 0.7001(6) 0.0398(17) Uani 1 1 d U . . H13B H 0.3290 0.6733 0.7185 0.048 Uiso 1 1 calc R . . H13C H 0.2934 0.6629 0.7504 0.048 Uiso 1 1 calc R . . C14 C 0.2968(2) 0.7359(6) 0.6431(6) 0.0400(17) Uani 1 1 d U . . H14B H 0.2968 0.7893 0.6743 0.048 Uiso 1 1 calc R . . H14C H 0.2753 0.7257 0.6216 0.048 Uiso 1 1 calc R . . C15 C 0.3115(2) 0.8083(6) 0.5070(6) 0.0418(19) Uani 1 1 d U . . H15C H 0.2898 0.7991 0.4864 0.050 Uiso 1 1 calc R . . H15D H 0.3124 0.8640 0.5339 0.050 Uiso 1 1 calc R . . C16 C 0.3349(2) 0.8041(6) 0.4342(6) 0.0488(19) Uani 1 1 d U . . H16A H 0.3297 0.8478 0.3926 0.059 Uiso 1 1 calc R . . H16B H 0.3564 0.8150 0.4552 0.059 Uiso 1 1 calc R . . C17 C 0.3373(3) 0.4681(7) 0.1096(7) 0.062(2) Uani 1 1 d U . . H17A H 0.3578 0.4403 0.0996 0.074 Uiso 1 1 calc R . . H17B H 0.3341 0.5105 0.0653 0.074 Uiso 1 1 calc R . . C18 C 0.3112(3) 0.4047(7) 0.1071(7) 0.062(2) Uani 1 1 d U . . H18A H 0.3100 0.3793 0.0507 0.075 Uiso 1 1 calc R . . H18B H 0.2908 0.4325 0.1186 0.075 Uiso 1 1 calc R . . C19 C 0.2917(3) 0.2723(8) 0.1737(7) 0.072(2) Uani 1 1 d DU . . H19A H 0.2711 0.3011 0.1694 0.086 Uiso 1 1 calc R . . H19B H 0.2940 0.2358 0.1241 0.086 Uiso 1 1 calc R . . C20 C 0.2918(3) 0.2221(8) 0.2466(7) 0.082(2) Uani 1 1 d DU . . H20A H 0.3076 0.1775 0.2380 0.099 Uiso 1 1 calc R . . H20B H 0.2710 0.1944 0.2501 0.099 Uiso 1 1 calc R . . C21 C 0.3142(3) 0.1957(9) 0.3766(9) 0.084(2) Uani 1 1 d DU . . H21A H 0.2988 0.1719 0.4164 0.101 Uiso 1 1 calc R . . H21B H 0.3202 0.1502 0.3378 0.101 Uiso 1 1 calc R . . C22 C 0.3406(3) 0.2172(8) 0.4215(8) 0.084(2) Uani 1 1 d DU . . H22A H 0.3562 0.1724 0.4111 0.101 Uiso 1 1 calc R . . H22B H 0.3346 0.2127 0.4812 0.101 Uiso 1 1 calc R . . C23 C 0.3902(3) 0.2823(9) 0.3890(8) 0.086(2) Uani 1 1 d DU . . H23A H 0.4029 0.2937 0.4396 0.103 Uiso 1 1 calc R . . H23B H 0.3926 0.2219 0.3771 0.103 Uiso 1 1 calc R . . C24 C 0.4054(3) 0.3249(8) 0.3224(7) 0.071(2) Uani 1 1 d DU . . H24A H 0.4158 0.2829 0.2863 0.085 Uiso 1 1 calc R . . H24B H 0.4221 0.3608 0.3463 0.085 Uiso 1 1 calc R . . N1 N 0.45609(18) 0.3173(5) 0.0829(5) 0.0463(18) Uani 1 1 d U . . H1A H 0.4397 0.3236 0.1197 0.056 Uiso 1 1 calc R . . H1B H 0.4479 0.3217 0.0299 0.056 Uiso 1 1 calc R . . N2 N 0.52288(18) 0.2939(5) 0.1031(5) 0.0426(15) Uani 1 1 d U . . H2A H 0.5244 0.2770 0.1585 0.051 Uiso 1 1 calc R . . N3 N 0.55786(18) 0.4516(5) 0.0911(5) 0.0455(16) Uani 1 1 d U . . H3A H 0.5613 0.4583 0.0342 0.055 Uiso 1 1 calc R . . N4 N 0.52570(18) 0.5378(5) 0.2227(5) 0.0417(15) Uani 1 1 d U . . H4A H 0.5196 0.5924 0.2116 0.050 Uiso 1 1 calc R . . N5 N 0.4851(2) 0.3980(5) 0.2624(5) 0.0465(16) Uani 1 1 d U . . H5A H 0.4652 0.4151 0.2771 0.056 Uiso 1 1 calc R . . H5B H 0.4854 0.3407 0.2649 0.056 Uiso 1 1 calc R . . N6 N 0.38576(17) 0.6474(5) 0.5187(5) 0.0382(15) Uani 1 1 d U . . H6A H 0.3948 0.6538 0.4669 0.046 Uiso 1 1 calc R . . H6B H 0.3846 0.6994 0.5428 0.046 Uiso 1 1 calc R . . N7 N 0.36189(16) 0.4962(5) 0.5951(4) 0.0346(15) Uani 1 1 d U . . H7A H 0.3560 0.4414 0.5834 0.042 Uiso 1 1 calc R . . N8 N 0.30453(18) 0.5818(4) 0.6538(4) 0.0345(15) Uani 1 1 d U . . H8A H 0.2832 0.5691 0.6500 0.041 Uiso 1 1 calc R . . N9 N 0.32043(18) 0.7399(4) 0.5703(5) 0.0379(15) Uani 1 1 d U . . H9A H 0.3399 0.7541 0.5926 0.045 Uiso 1 1 calc R . . N10 N 0.33381(19) 0.7198(5) 0.3932(5) 0.0438(17) Uani 1 1 d U . . H10A H 0.3521 0.7123 0.3636 0.053 Uiso 1 1 calc R . . H10B H 0.3175 0.7193 0.3556 0.053 Uiso 1 1 calc R . . N11 N 0.3373(2) 0.5084(6) 0.1920(5) 0.0533(18) Uani 1 1 d U . . H11A H 0.3223 0.5497 0.1921 0.064 Uiso 1 1 calc R . . H11B H 0.3565 0.5337 0.1998 0.064 Uiso 1 1 calc R . . N12 N 0.3172(2) 0.3359(6) 0.1731(5) 0.0550(17) Uani 1 1 d U . . H12A H 0.3357 0.3087 0.1584 0.066 Uiso 1 1 calc R . . N13 N 0.2980(2) 0.2596(6) 0.3279(6) 0.0618(19) Uani 1 1 d U . . H13A H 0.2786 0.2683 0.3532 0.074 Uiso 1 1 calc R . . N14 N 0.3573(2) 0.2941(6) 0.4135(6) 0.0569(18) Uani 1 1 d U . . H14A H 0.3580 0.3165 0.4671 0.068 Uiso 1 1 calc R . . N15 N 0.38503(19) 0.3772(5) 0.2696(5) 0.0509(17) Uani 1 1 d U . . H15A H 0.3839 0.3524 0.2178 0.061 Uiso 1 1 calc R . . H15B H 0.3949 0.4278 0.2625 0.061 Uiso 1 1 calc R . . O1 O 0.35102(14) 0.5211(4) 0.3865(3) 0.0359(15) Uani 1 1 d . . . O2 O 0.49736(14) 0.4236(3) -0.0393(3) 0.0303(14) 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 Sb2 0.0285(4) 0.0256(3) 0.0321(3) 0.0002(2) 0.0044(3) 0.0016(2) Sb1 0.0219(3) 0.0422(4) 0.0604(5) -0.0136(3) -0.0009(3) -0.0034(3) Eu3 0.0256(3) 0.0256(2) 0.0253(2) 0.00298(18) 0.0013(2) 0.00256(17) Eu2 0.0231(3) 0.0281(2) 0.0272(3) -0.00117(18) -0.0007(2) -0.00088(18) Eu1 0.0276(3) 0.0273(2) 0.0319(3) -0.00422(18) -0.0039(2) -0.00022(18) Cl1 0.061(2) 0.0511(17) 0.078(2) -0.0216(14) 0.0127(16) 0.0007(13) S7 0.0411(17) 0.0439(16) 0.069(2) 0.0072(13) 0.0003(14) 0.0185(12) S6 0.0409(15) 0.0320(13) 0.0399(14) -0.0033(10) 0.0051(12) -0.0093(10) S5 0.0465(17) 0.0475(15) 0.0301(13) 0.0072(11) 0.0059(12) -0.0023(11) S4 0.0315(14) 0.0329(12) 0.0383(14) -0.0080(10) 0.0044(11) -0.0016(9) S3 0.0419(17) 0.082(2) 0.0515(17) -0.0259(15) -0.0181(14) 0.0242(14) S2 0.0352(16) 0.0396(15) 0.073(2) -0.0145(13) -0.0173(14) 0.0068(11) S1 0.0319(14) 0.0352(14) 0.0419(15) 0.0013(10) 0.0012(11) -0.0040(10) C1 0.053(4) 0.039(4) 0.050(4) 0.010(4) 0.001(4) -0.003(4) C2 0.059(5) 0.040(4) 0.047(4) 0.007(4) 0.004(4) 0.015(4) C3 0.053(4) 0.049(4) 0.054(4) 0.009(4) 0.005(4) 0.018(3) C4 0.046(4) 0.055(4) 0.057(4) 0.005(3) -0.001(4) 0.009(3) C5 0.053(4) 0.059(4) 0.060(4) 0.001(4) -0.002(4) -0.001(4) C6 0.056(4) 0.057(4) 0.056(4) -0.003(3) -0.006(4) -0.003(3) C7 0.051(4) 0.048(4) 0.048(4) 0.001(3) -0.005(4) -0.004(3) C8 0.057(5) 0.051(4) 0.043(4) 0.008(4) -0.008(4) 0.008(4) C9 0.029(4) 0.050(4) 0.035(4) 0.000(3) -0.001(4) -0.001(3) C10 0.032(4) 0.043(4) 0.035(4) -0.001(3) -0.004(3) 0.007(3) C11 0.038(3) 0.046(4) 0.038(3) 0.003(3) 0.000(3) 0.000(3) C12 0.041(4) 0.042(4) 0.038(4) 0.006(3) 0.005(3) -0.007(3) C13 0.039(4) 0.043(4) 0.038(4) -0.003(3) 0.004(3) -0.002(3) C14 0.039(4) 0.040(4) 0.040(4) -0.004(3) 0.002(3) -0.006(3) C15 0.045(4) 0.034(4) 0.047(4) 0.004(3) 0.002(4) 0.002(3) C16 0.052(4) 0.047(4) 0.047(4) 0.009(3) 0.003(4) -0.004(3) C17 0.068(4) 0.065(4) 0.053(4) 0.006(4) -0.005(4) 0.008(4) C18 0.068(5) 0.069(5) 0.051(4) -0.009(4) -0.011(4) 0.005(4) C19 0.071(4) 0.074(4) 0.071(4) -0.005(4) -0.009(4) -0.016(4) C20 0.084(4) 0.078(4) 0.084(4) -0.003(4) -0.010(4) -0.018(4) C21 0.076(5) 0.080(5) 0.097(5) 0.017(4) -0.010(4) -0.011(4) C22 0.086(5) 0.078(4) 0.089(4) 0.016(4) -0.021(4) -0.001(4) C23 0.079(5) 0.092(5) 0.088(5) 0.028(4) -0.002(4) 0.021(4) C24 0.061(4) 0.071(4) 0.082(5) 0.023(4) -0.002(4) 0.001(4) N1 0.051(4) 0.038(4) 0.049(4) 0.007(3) 0.002(3) 0.000(3) N2 0.046(3) 0.041(3) 0.041(3) 0.008(3) 0.004(3) 0.008(3) N3 0.044(4) 0.046(4) 0.047(4) -0.001(3) 0.000(3) 0.002(3) N4 0.042(3) 0.041(3) 0.041(3) 0.003(3) -0.005(3) 0.006(3) N5 0.047(3) 0.046(3) 0.046(3) 0.011(3) 0.005(3) 0.003(3) N6 0.037(3) 0.039(3) 0.039(3) -0.004(3) 0.005(3) -0.002(3) N7 0.032(3) 0.039(3) 0.033(3) 0.000(3) -0.004(3) -0.001(3) N8 0.033(3) 0.037(3) 0.034(3) -0.001(3) 0.004(3) -0.005(3) N9 0.038(3) 0.036(3) 0.040(3) -0.004(3) 0.005(3) -0.001(3) N10 0.047(4) 0.047(4) 0.037(4) 0.005(3) 0.004(3) 0.008(3) N11 0.058(4) 0.055(4) 0.047(4) 0.004(3) -0.012(4) 0.001(3) N12 0.058(4) 0.056(4) 0.052(4) -0.009(3) -0.007(3) -0.006(3) N13 0.060(4) 0.058(4) 0.067(4) 0.003(3) -0.004(4) -0.004(3) N14 0.054(4) 0.055(4) 0.062(4) 0.015(3) 0.001(3) -0.001(3) N15 0.052(4) 0.050(4) 0.051(4) 0.004(3) 0.003(3) 0.003(3) O1 0.038(4) 0.045(4) 0.025(3) -0.009(3) 0.002(3) -0.008(3) O2 0.036(4) 0.029(3) 0.025(3) 0.003(2) 0.004(3) 0.001(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 Sb2 S5 2.318(2) . ? Sb2 S7 2.320(2) . ? Sb2 S6 2.338(2) . ? Sb2 S4 2.363(2) . ? Sb1 S3 2.386(3) . ? Sb1 S2 2.395(3) . ? Sb1 S1 2.443(2) . ? Sb1 Eu2 3.7757(9) . ? Sb1 Eu1 3.8396(9) . ? Eu3 O2 2.302(5) . ? Eu3 O2 2.328(5) 5_665 ? Eu3 N3 2.587(8) . ? Eu3 N5 2.598(7) . ? Eu3 N2 2.616(7) . ? Eu3 N1 2.624(8) . ? Eu3 N4 2.644(7) . ? Eu3 S4 2.943(2) . ? Eu3 Eu3 3.7610(10) 5_665 ? Eu2 O1 2.285(5) . ? Eu2 N7 2.580(7) . ? Eu2 N8 2.622(7) . ? Eu2 N9 2.622(7) . ? Eu2 N10 2.623(7) . ? Eu2 N6 2.639(7) . ? Eu2 S2 2.813(3) . ? Eu2 S1 2.917(2) . ? Eu2 Eu1 3.9872(8) . ? Eu1 O1 2.298(5) . ? Eu1 N12 2.594(8) . ? Eu1 N11 2.596(8) . ? Eu1 N15 2.604(8) . ? Eu1 N13 2.607(9) . ? Eu1 N14 2.633(8) . ? Eu1 S3 2.840(3) . ? Eu1 S1 2.919(2) . ? C1 N1 1.459(11) . ? C1 C2 1.498(13) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 N2 1.502(12) . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 N2 1.497(11) . ? C3 C4 1.519(14) . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 N3 1.474(12) . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 C6 1.447(11) . ? C5 N3 1.485(12) . ? C5 H5C 0.9700 . ? C5 H5D 0.9700 . ? C6 N4 1.453(11) . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C7 C8 1.453(13) . ? C7 N4 1.470(11) . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 N5 1.505(12) . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 N6 1.478(11) . ? C9 C10 1.500(12) . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 N7 1.484(10) . ? C10 H10C 0.9700 . ? C10 H10D 0.9700 . ? C11 N7 1.458(10) . ? C11 C12 1.527(11) . ? C11 H11C 0.9700 . ? C11 H11D 0.9700 . ? C12 N8 1.487(11) . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 N8 1.485(11) . ? C13 C14 1.495(12) . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 N9 1.507(11) . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 C16 1.501(12) . ? C15 N9 1.506(11) . ? C15 H15C 0.9700 . ? C15 H15D 0.9700 . ? C16 N10 1.469(12) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N11 1.437(12) . ? C17 C18 1.472(15) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N12 1.516(13) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.387(12) . ? C19 N12 1.456(13) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 N13 1.426(13) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.346(12) . ? C21 N13 1.429(14) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N14 1.397(14) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.392(12) . ? C23 N14 1.433(14) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N15 1.439(12) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 H2A 0.9100 . ? N3 H3A 0.9100 . ? N4 H4A 0.9100 . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? N7 H7A 0.9100 . ? N8 H8A 0.9100 . ? N9 H9A 0.9100 . ? N10 H10A 0.9000 . ? N10 H10B 0.9000 . ? N11 H11A 0.9000 . ? N11 H11B 0.9000 . ? N12 H12A 0.9100 . ? N13 H13A 0.9100 . ? N14 H14A 0.9100 . ? N15 H15A 0.9000 . ? N15 H15B 0.9000 . ? O2 Eu3 2.328(5) 5_665 ? 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 S5 Sb2 S7 108.85(10) . . ? S5 Sb2 S6 113.08(9) . . ? S7 Sb2 S6 110.85(9) . . ? S5 Sb2 S4 104.07(9) . . ? S7 Sb2 S4 111.43(9) . . ? S6 Sb2 S4 108.40(8) . . ? S3 Sb1 S2 101.79(11) . . ? S3 Sb1 S1 96.78(9) . . ? S2 Sb1 S1 97.46(8) . . ? S3 Sb1 Eu2 95.23(7) . . ? S2 Sb1 Eu2 48.11(6) . . ? S1 Sb1 Eu2 50.58(6) . . ? S3 Sb1 Eu1 47.55(6) . . ? S2 Sb1 Eu1 100.80(7) . . ? S1 Sb1 Eu1 49.46(6) . . ? Eu2 Sb1 Eu1 63.140(17) . . ? O2 Eu3 O2 71.4(2) . 5_665 ? O2 Eu3 N3 83.8(2) . . ? O2 Eu3 N3 78.7(2) 5_665 . ? O2 Eu3 N5 153.8(2) . . ? O2 Eu3 N5 133.9(2) 5_665 . ? N3 Eu3 N5 105.7(3) . . ? O2 Eu3 N2 80.9(2) . . ? O2 Eu3 N2 137.9(2) 5_665 . ? N3 Eu3 N2 67.1(2) . . ? N5 Eu3 N2 80.6(2) . . ? O2 Eu3 N1 76.7(2) . . ? O2 Eu3 N1 133.4(2) 5_665 . ? N3 Eu3 N1 130.5(2) . . ? N5 Eu3 N1 78.7(2) . . ? N2 Eu3 N1 65.2(2) . . ? O2 Eu3 N4 138.7(2) . . ? O2 Eu3 N4 76.5(2) 5_665 . ? N3 Eu3 N4 64.8(2) . . ? N5 Eu3 N4 65.5(2) . . ? N2 Eu3 N4 108.1(2) . . ? N1 Eu3 N4 144.2(2) . . ? O2 Eu3 S4 98.43(15) . . ? O2 Eu3 S4 80.95(15) 5_665 . ? N3 Eu3 S4 157.66(18) . . ? N5 Eu3 S4 82.00(19) . . ? N2 Eu3 S4 135.26(18) . . ? N1 Eu3 S4 71.16(17) . . ? N4 Eu3 S4 101.38(17) . . ? O2 Eu3 Eu3 35.91(13) . 5_665 ? O2 Eu3 Eu3 35.44(13) 5_665 5_665 ? N3 Eu3 Eu3 79.25(17) . 5_665 ? N5 Eu3 Eu3 168.09(18) . 5_665 ? N2 Eu3 Eu3 111.27(16) . 5_665 ? N1 Eu3 Eu3 106.53(17) . 5_665 ? N4 Eu3 Eu3 108.40(16) . 5_665 ? S4 Eu3 Eu3 89.56(5) . 5_665 ? O1 Eu2 N7 85.9(2) . . ? O1 Eu2 N8 147.5(2) . . ? N7 Eu2 N8 67.5(2) . . ? O1 Eu2 N9 143.0(2) . . ? N7 Eu2 N9 108.0(2) . . ? N8 Eu2 N9 66.6(2) . . ? O1 Eu2 N10 81.0(2) . . ? N7 Eu2 N10 138.3(2) . . ? N8 Eu2 N10 131.3(2) . . ? N9 Eu2 N10 65.7(2) . . ? O1 Eu2 N6 81.0(2) . . ? N7 Eu2 N6 65.8(2) . . ? N8 Eu2 N6 103.1(2) . . ? N9 Eu2 N6 74.5(2) . . ? N10 Eu2 N6 73.1(2) . . ? O1 Eu2 S2 109.83(15) . . ? N7 Eu2 S2 146.04(17) . . ? N8 Eu2 S2 85.81(18) . . ? N9 Eu2 S2 77.79(17) . . ? N10 Eu2 S2 75.19(18) . . ? N6 Eu2 S2 144.29(17) . . ? O1 Eu2 S1 74.25(15) . . ? N7 Eu2 S1 76.99(17) . . ? N8 Eu2 S1 81.60(16) . . ? N9 Eu2 S1 141.45(17) . . ? N10 Eu2 S1 135.01(18) . . ? N6 Eu2 S1 136.38(17) . . ? S2 Eu2 S1 78.75(7) . . ? O1 Eu2 Sb1 87.08(14) . . ? N7 Eu2 Sb1 116.11(16) . . ? N8 Eu2 Sb1 88.34(16) . . ? N9 Eu2 Sb1 114.61(16) . . ? N10 Eu2 Sb1 102.60(18) . . ? N6 Eu2 Sb1 167.82(16) . . ? S2 Eu2 Sb1 39.33(5) . . ? S1 Eu2 Sb1 40.31(5) . . ? O1 Eu2 Eu1 29.64(14) . . ? N7 Eu2 Eu1 90.24(16) . . ? N8 Eu2 Eu1 127.94(15) . . ? N9 Eu2 Eu1 160.95(16) . . ? N10 Eu2 Eu1 97.04(17) . . ? N6 Eu2 Eu1 109.46(16) . . ? S2 Eu2 Eu1 90.29(5) . . ? S1 Eu2 Eu1 46.92(5) . . ? Sb1 Eu2 Eu1 59.212(15) . . ? O1 Eu1 N12 143.4(2) . . ? O1 Eu1 N11 78.6(2) . . ? N12 Eu1 N11 66.5(3) . . ? O1 Eu1 N15 82.2(2) . . ? N12 Eu1 N15 77.9(3) . . ? N11 Eu1 N15 73.3(3) . . ? O1 Eu1 N13 150.4(2) . . ? N12 Eu1 N13 65.6(3) . . ? N11 Eu1 N13 131.0(3) . . ? N15 Eu1 N13 106.1(3) . . ? O1 Eu1 N14 93.2(3) . . ? N12 Eu1 N14 105.9(3) . . ? N11 Eu1 N14 139.2(3) . . ? N15 Eu1 N14 65.9(3) . . ? N13 Eu1 N14 66.1(3) . . ? O1 Eu1 S3 102.18(16) . . ? N12 Eu1 S3 79.5(2) . . ? N11 Eu1 S3 74.94(19) . . ? N15 Eu1 S3 146.38(19) . . ? N13 Eu1 S3 86.6(2) . . ? N14 Eu1 S3 145.3(2) . . ? O1 Eu1 S1 74.05(14) . . ? N12 Eu1 S1 139.96(19) . . ? N11 Eu1 S1 135.7(2) . . ? N15 Eu1 S1 134.43(19) . . ? N13 Eu1 S1 80.5(2) . . ? N14 Eu1 S1 77.1(2) . . ? S3 Eu1 S1 77.63(8) . . ? O1 Eu1 Sb1 85.37(14) . . ? N12 Eu1 Sb1 113.1(2) . . ? N11 Eu1 Sb1 104.92(19) . . ? N15 Eu1 Sb1 167.57(19) . . ? N13 Eu1 Sb1 84.5(2) . . ? N14 Eu1 Sb1 114.27(19) . . ? S3 Eu1 Sb1 38.29(6) . . ? S1 Eu1 Sb1 39.50(5) . . ? O1 Eu1 Eu2 29.45(14) . . ? N12 Eu1 Eu2 158.4(2) . . ? N11 Eu1 Eu2 95.85(19) . . ? N15 Eu1 Eu2 110.01(19) . . ? N13 Eu1 Eu2 127.4(2) . . ? N14 Eu1 Eu2 95.6(2) . . ? S3 Eu1 Eu2 83.98(6) . . ? S1 Eu1 Eu2 46.89(5) . . ? Sb1 Eu1 Eu2 57.648(14) . . ? Sb2 S4 Eu3 108.86(8) . . ? Sb1 S3 Eu1 94.16(9) . . ? Sb1 S2 Eu2 92.56(8) . . ? Sb1 S1 Eu2 89.11(7) . . ? Sb1 S1 Eu1 91.03(8) . . ? Eu2 S1 Eu1 86.19(6) . . ? N1 C1 C2 109.4(7) . . ? N1 C1 H1C 109.8 . . ? C2 C1 H1C 109.8 . . ? N1 C1 H1D 109.8 . . ? C2 C1 H1D 109.8 . . ? H1C C1 H1D 108.3 . . ? C1 C2 N2 110.2(8) . . ? C1 C2 H2B 109.6 . . ? N2 C2 H2B 109.6 . . ? C1 C2 H2C 109.6 . . ? N2 C2 H2C 109.6 . . ? H2B C2 H2C 108.1 . . ? N2 C3 C4 109.1(8) . . ? N2 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? N2 C3 H3C 109.9 . . ? C4 C3 H3C 109.9 . . ? H3B C3 H3C 108.3 . . ? N3 C4 C3 108.9(8) . . ? N3 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? N3 C4 H4C 109.9 . . ? C3 C4 H4C 109.9 . . ? H4B C4 H4C 108.3 . . ? C6 C5 N3 108.8(8) . . ? C6 C5 H5C 109.9 . . ? N3 C5 H5C 109.9 . . ? C6 C5 H5D 109.9 . . ? N3 C5 H5D 109.9 . . ? H5C C5 H5D 108.3 . . ? C5 C6 N4 116.5(9) . . ? C5 C6 H6C 108.2 . . ? N4 C6 H6C 108.2 . . ? C5 C6 H6D 108.2 . . ? N4 C6 H6D 108.2 . . ? H6C C6 H6D 107.3 . . ? C8 C7 N4 112.5(8) . . ? C8 C7 H7B 109.1 . . ? N4 C7 H7B 109.1 . . ? C8 C7 H7C 109.1 . . ? N4 C7 H7C 109.1 . . ? H7B C7 H7C 107.8 . . ? C7 C8 N5 111.0(8) . . ? C7 C8 H8B 109.4 . . ? N5 C8 H8B 109.4 . . ? C7 C8 H8C 109.4 . . ? N5 C8 H8C 109.4 . . ? H8B C8 H8C 108.0 . . ? N6 C9 C10 110.4(7) . . ? N6 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? N6 C9 H9C 109.6 . . ? C10 C9 H9C 109.6 . . ? H9B C9 H9C 108.1 . . ? N7 C10 C9 110.8(7) . . ? N7 C10 H10C 109.5 . . ? C9 C10 H10C 109.5 . . ? N7 C10 H10D 109.5 . . ? C9 C10 H10D 109.5 . . ? H10C C10 H10D 108.1 . . ? N7 C11 C12 109.1(7) . . ? N7 C11 H11C 109.9 . . ? C12 C11 H11C 109.9 . . ? N7 C11 H11D 109.9 . . ? C12 C11 H11D 109.9 . . ? H11C C11 H11D 108.3 . . ? N8 C12 C11 111.7(7) . . ? N8 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? N8 C12 H12C 109.3 . . ? C11 C12 H12C 109.3 . . ? H12B C12 H12C 107.9 . . ? N8 C13 C14 110.0(7) . . ? N8 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? N8 C13 H13C 109.7 . . ? C14 C13 H13C 109.7 . . ? H13B C13 H13C 108.2 . . ? C13 C14 N9 107.4(7) . . ? C13 C14 H14B 110.2 . . ? N9 C14 H14B 110.2 . . ? C13 C14 H14C 110.2 . . ? N9 C14 H14C 110.2 . . ? H14B C14 H14C 108.5 . . ? C16 C15 N9 108.0(8) . . ? C16 C15 H15C 110.1 . . ? N9 C15 H15C 110.1 . . ? C16 C15 H15D 110.1 . . ? N9 C15 H15D 110.1 . . ? H15C C15 H15D 108.4 . . ? N10 C16 C15 110.6(8) . . ? N10 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? N10 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N11 C17 C18 108.7(9) . . ? N11 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? N11 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C17 C18 N12 109.8(9) . . ? C17 C18 H18A 109.7 . . ? N12 C18 H18A 109.7 . . ? C17 C18 H18B 109.7 . . ? N12 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? C20 C19 N12 113.0(10) . . ? C20 C19 H19A 109.0 . . ? N12 C19 H19A 109.0 . . ? C20 C19 H19B 109.0 . . ? N12 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C19 C20 N13 120.1(11) . . ? C19 C20 H20A 107.3 . . ? N13 C20 H20A 107.3 . . ? C19 C20 H20B 107.3 . . ? N13 C20 H20B 107.3 . . ? H20A C20 H20B 106.9 . . ? C22 C21 N13 119.2(12) . . ? C22 C21 H21A 107.5 . . ? N13 C21 H21A 107.5 . . ? C22 C21 H21B 107.5 . . ? N13 C21 H21B 107.5 . . ? H21A C21 H21B 107.0 . . ? C21 C22 N14 125.1(11) . . ? C21 C22 H22A 106.0 . . ? N14 C22 H22A 106.0 . . ? C21 C22 H22B 106.0 . . ? N14 C22 H22B 106.0 . . ? H22A C22 H22B 106.3 . . ? C24 C23 N14 124.9(11) . . ? C24 C23 H23A 106.1 . . ? N14 C23 H23A 106.1 . . ? C24 C23 H23B 106.1 . . ? N14 C23 H23B 106.1 . . ? H23A C23 H23B 106.3 . . ? C23 C24 N15 116.0(10) . . ? C23 C24 H24A 108.3 . . ? N15 C24 H24A 108.3 . . ? C23 C24 H24B 108.3 . . ? N15 C24 H24B 108.3 . . ? H24A C24 H24B 107.4 . . ? C1 N1 Eu3 117.4(6) . . ? C1 N1 H1A 108.0 . . ? Eu3 N1 H1A 108.0 . . ? C1 N1 H1B 108.0 . . ? Eu3 N1 H1B 108.0 . . ? H1A N1 H1B 107.2 . . ? C3 N2 C2 113.4(7) . . ? C3 N2 Eu3 111.8(5) . . ? C2 N2 Eu3 112.8(6) . . ? C3 N2 H2A 106.0 . . ? C2 N2 H2A 106.0 . . ? Eu3 N2 H2A 106.0 . . ? C4 N3 C5 112.2(8) . . ? C4 N3 Eu3 113.7(6) . . ? C5 N3 Eu3 115.8(6) . . ? C4 N3 H3A 104.5 . . ? C5 N3 H3A 104.5 . . ? Eu3 N3 H3A 104.5 . . ? C6 N4 C7 111.3(8) . . ? C6 N4 Eu3 114.8(6) . . ? C7 N4 Eu3 115.0(6) . . ? C6 N4 H4A 104.8 . . ? C7 N4 H4A 104.8 . . ? Eu3 N4 H4A 104.8 . . ? C8 N5 Eu3 114.8(6) . . ? C8 N5 H5A 108.6 . . ? Eu3 N5 H5A 108.6 . . ? C8 N5 H5B 108.6 . . ? Eu3 N5 H5B 108.6 . . ? H5A N5 H5B 107.5 . . ? C9 N6 Eu2 116.1(5) . . ? C9 N6 H6A 108.3 . . ? Eu2 N6 H6A 108.3 . . ? C9 N6 H6B 108.3 . . ? Eu2 N6 H6B 108.3 . . ? H6A N6 H6B 107.4 . . ? C11 N7 C10 114.3(7) . . ? C11 N7 Eu2 114.7(5) . . ? C10 N7 Eu2 110.5(5) . . ? C11 N7 H7A 105.5 . . ? C10 N7 H7A 105.5 . . ? Eu2 N7 H7A 105.5 . . ? C13 N8 C12 111.8(7) . . ? C13 N8 Eu2 112.9(5) . . ? C12 N8 Eu2 111.2(5) . . ? C13 N8 H8A 106.9 . . ? C12 N8 H8A 106.9 . . ? Eu2 N8 H8A 106.9 . . ? C15 N9 C14 111.5(7) . . ? C15 N9 Eu2 112.0(5) . . ? C14 N9 Eu2 110.9(5) . . ? C15 N9 H9A 107.4 . . ? C14 N9 H9A 107.4 . . ? Eu2 N9 H9A 107.4 . . ? C16 N10 Eu2 115.3(5) . . ? C16 N10 H10A 108.4 . . ? Eu2 N10 H10A 108.4 . . ? C16 N10 H10B 108.4 . . ? Eu2 N10 H10B 108.4 . . ? H10A N10 H10B 107.5 . . ? C17 N11 Eu1 115.3(7) . . ? C17 N11 H11A 108.4 . . ? Eu1 N11 H11A 108.4 . . ? C17 N11 H11B 108.4 . . ? Eu1 N11 H11B 108.4 . . ? H11A N11 H11B 107.5 . . ? C19 N12 C18 111.8(9) . . ? C19 N12 Eu1 113.5(7) . . ? C18 N12 Eu1 108.9(6) . . ? C19 N12 H12A 107.5 . . ? C18 N12 H12A 107.5 . . ? Eu1 N12 H12A 107.5 . . ? C20 N13 C21 105.9(10) . . ? C20 N13 Eu1 114.1(7) . . ? C21 N13 Eu1 115.7(7) . . ? C20 N13 H13A 106.9 . . ? C21 N13 H13A 106.9 . . ? Eu1 N13 H13A 106.9 . . ? C22 N14 C23 112.8(10) . . ? C22 N14 Eu1 112.9(7) . . ? C23 N14 Eu1 113.7(6) . . ? C22 N14 H14A 105.5 . . ? C23 N14 H14A 105.5 . . ? Eu1 N14 H14A 105.5 . . ? C24 N15 Eu1 118.6(6) . . ? C24 N15 H15A 107.7 . . ? Eu1 N15 H15A 107.7 . . ? C24 N15 H15B 107.7 . . ? Eu1 N15 H15B 107.7 . . ? H15A N15 H15B 107.1 . . ? Eu2 O1 Eu1 120.9(2) . . ? Eu3 O2 Eu3 108.6(2) . 5_665 ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 1.258 _refine_diff_density_min -1.061 _refine_diff_density_rms 0.163 data_1 _database_code_depnum_ccdc_archive 'CCDC 865323' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H36 Eu N8, S4 Sb ' _chemical_formula_sum 'C12 H36 Eu N8 S4 Sb ' _chemical_formula_weight 694.50 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' Eu Eu -0.1578 3.6682 '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 Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 26.089(5) _cell_length_b 13.499(3) _cell_length_c 13.337(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4697.0(17) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 25.10 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.964 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 4.167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1353 _exptl_absorpt_correction_T_max 0.6571 _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 25143 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4173 _reflns_number_gt 3714 _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^)+(0.0041P)^2^+4.5790P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00090(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4173 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0435 _refine_ls_wR_factor_gt 0.0416 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.624755(5) 0.470769(9) 0.710390(10) 0.01889(6) Uani 1 1 d . . . N1 N 0.64341(11) 0.31770(19) 0.8224(2) 0.0430(7) Uani 1 1 d . . . H1C H 0.6271 0.3241 0.8816 0.052 Uiso 1 1 calc R . . H1D H 0.6319 0.2624 0.7922 0.052 Uiso 1 1 calc R . . N2 N 0.71620(9) 0.41310(17) 0.69536(19) 0.0297(6) Uani 1 1 d . . . H2C H 0.7340 0.4561 0.7346 0.036 Uiso 1 1 calc R . . N3 N 0.66668(10) 0.53323(17) 0.55078(19) 0.0291(6) Uani 1 1 d . . . H3C H 0.6575 0.4898 0.5018 0.035 Uiso 1 1 calc R . . N4 N 0.57410(9) 0.61548(17) 0.6337(2) 0.0332(6) Uani 1 1 d . . . H4C H 0.5403 0.6022 0.6367 0.040 Uiso 1 1 calc R . . H4D H 0.5800 0.6710 0.6693 0.040 Uiso 1 1 calc R . . N5 N 0.59231(9) 0.34530(17) 0.58140(19) 0.0311(6) Uani 1 1 d . . . H5C H 0.5985 0.3690 0.5195 0.037 Uiso 1 1 calc R . . H5D H 0.6102 0.2887 0.5883 0.037 Uiso 1 1 calc R . . N6 N 0.53330(9) 0.41701(18) 0.74492(18) 0.0280(6) Uani 1 1 d . . . H6C H 0.5130 0.4619 0.7129 0.034 Uiso 1 1 calc R . . N7 N 0.59429(10) 0.53084(17) 0.87970(18) 0.0301(6) Uani 1 1 d . . . H7C H 0.6068 0.4866 0.9250 0.036 Uiso 1 1 calc R . . N8 N 0.67682(9) 0.62084(16) 0.77667(18) 0.0266(5) Uani 1 1 d . . . H8C H 0.7102 0.6123 0.7622 0.032 Uiso 1 1 calc R . . H8D H 0.6661 0.6764 0.7459 0.032 Uiso 1 1 calc R . . C1 C 0.69914(13) 0.3100(2) 0.8391(3) 0.0428(9) Uani 1 1 d . . . H1A H 0.7070 0.2479 0.8723 0.051 Uiso 1 1 calc R . . H1B H 0.7105 0.3637 0.8821 0.051 Uiso 1 1 calc R . . C2 C 0.72659(14) 0.3150(2) 0.7408(3) 0.0437(9) Uani 1 1 d . . . H2A H 0.7631 0.3065 0.7510 0.052 Uiso 1 1 calc R . . H2B H 0.7146 0.2627 0.6968 0.052 Uiso 1 1 calc R . . C3 C 0.73842(13) 0.4270(2) 0.5946(2) 0.0413(8) Uani 1 1 d . . . H3A H 0.7257 0.3764 0.5494 0.050 Uiso 1 1 calc R . . H3B H 0.7755 0.4216 0.5978 0.050 Uiso 1 1 calc R . . C4 C 0.72335(12) 0.5281(2) 0.5572(3) 0.0390(8) Uani 1 1 d . . . H4A H 0.7360 0.5786 0.6026 0.047 Uiso 1 1 calc R . . H4B H 0.7383 0.5397 0.4916 0.047 Uiso 1 1 calc R . . C5 C 0.64686(14) 0.6308(2) 0.5187(2) 0.0387(8) Uani 1 1 d . . . H5A H 0.6566 0.6434 0.4497 0.046 Uiso 1 1 calc R . . H5B H 0.6614 0.6826 0.5603 0.046 Uiso 1 1 calc R . . C6 C 0.58939(14) 0.6315(2) 0.5279(2) 0.0420(9) Uani 1 1 d . . . H6A H 0.5761 0.6946 0.5047 0.050 Uiso 1 1 calc R . . H6B H 0.5749 0.5797 0.4862 0.050 Uiso 1 1 calc R . . C7 C 0.53703(12) 0.3228(2) 0.5906(3) 0.0396(8) Uani 1 1 d . . . H7A H 0.5299 0.2593 0.5596 0.048 Uiso 1 1 calc R . . H7B H 0.5173 0.3730 0.5555 0.048 Uiso 1 1 calc R . . C8 C 0.52108(12) 0.3201(2) 0.6992(3) 0.0369(8) Uani 1 1 d . . . H8A H 0.4846 0.3071 0.7043 0.044 Uiso 1 1 calc R . . H8B H 0.5393 0.2677 0.7340 0.044 Uiso 1 1 calc R . . C9 C 0.52001(13) 0.4249(3) 0.8527(2) 0.0449(9) Uani 1 1 d . . . H9A H 0.5369 0.3728 0.8904 0.054 Uiso 1 1 calc R . . H9B H 0.4833 0.4183 0.8618 0.054 Uiso 1 1 calc R . . C10 C 0.53783(13) 0.5253(3) 0.8889(3) 0.0486(10) Uani 1 1 d . . . H10A H 0.5221 0.5771 0.8490 0.058 Uiso 1 1 calc R . . H10B H 0.5278 0.5348 0.9583 0.058 Uiso 1 1 calc R . . C11 C 0.61464(12) 0.6282(2) 0.9107(2) 0.0356(8) Uani 1 1 d . . . H11A H 0.6097 0.6374 0.9822 0.043 Uiso 1 1 calc R . . H11B H 0.5966 0.6807 0.8757 0.043 Uiso 1 1 calc R . . C12 C 0.67050(12) 0.6317(2) 0.8859(2) 0.0348(7) Uani 1 1 d . . . H12A H 0.6850 0.6942 0.9077 0.042 Uiso 1 1 calc R . . H12B H 0.6884 0.5786 0.9202 0.042 Uiso 1 1 calc R . . Sb1 Sb 0.625851(7) 1.016829(13) 0.733725(15) 0.02069(6) Uani 1 1 d . . . S1 S 0.56027(3) 1.07735(6) 0.83680(6) 0.03436(18) Uani 1 1 d . . . S2 S 0.70056(3) 1.05169(6) 0.82163(6) 0.03370(18) Uani 1 1 d . . . S3 S 0.61962(3) 0.84717(5) 0.70643(7) 0.0357(2) Uani 1 1 d . . . S4 S 0.62771(4) 1.10378(6) 0.58283(6) 0.0446(2) 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 0.01805(9) 0.01995(8) 0.01865(9) 0.00075(5) 0.00037(6) -0.00027(5) N1 0.0455(18) 0.0331(14) 0.0505(19) 0.0123(13) 0.0025(15) 0.0016(12) N2 0.0259(14) 0.0293(12) 0.0341(14) -0.0053(11) 0.0022(11) 0.0012(10) N3 0.0349(15) 0.0308(13) 0.0216(13) -0.0010(10) 0.0045(11) -0.0089(11) N4 0.0262(14) 0.0278(13) 0.0456(17) 0.0058(11) -0.0035(12) -0.0026(11) N5 0.0321(15) 0.0296(13) 0.0317(15) -0.0054(11) -0.0004(12) -0.0030(11) N6 0.0258(14) 0.0319(13) 0.0264(14) 0.0053(10) 0.0019(11) -0.0014(11) N7 0.0331(15) 0.0378(14) 0.0195(13) -0.0006(10) 0.0024(11) -0.0008(11) N8 0.0235(13) 0.0248(12) 0.0315(14) -0.0018(10) 0.0008(11) 0.0018(10) C1 0.047(2) 0.0320(16) 0.049(2) 0.0053(15) -0.0182(18) 0.0046(15) C2 0.034(2) 0.0312(17) 0.066(3) -0.0036(16) -0.0042(18) 0.0125(15) C3 0.0285(18) 0.058(2) 0.037(2) -0.0149(16) 0.0078(15) 0.0038(15) C4 0.0329(19) 0.055(2) 0.0290(18) -0.0024(15) 0.0111(15) -0.0135(16) C5 0.058(2) 0.0324(17) 0.0261(17) 0.0073(13) 0.0023(16) -0.0079(16) C6 0.060(2) 0.0295(16) 0.037(2) 0.0081(14) -0.0167(17) -0.0005(16) C7 0.0312(19) 0.0401(17) 0.048(2) -0.0097(15) -0.0097(16) -0.0066(14) C8 0.0270(17) 0.0315(16) 0.052(2) 0.0028(15) -0.0002(15) -0.0086(13) C9 0.0329(19) 0.071(2) 0.0304(18) 0.0066(17) 0.0102(15) -0.0149(17) C10 0.037(2) 0.076(3) 0.033(2) -0.0140(17) 0.0172(17) -0.0050(18) C11 0.049(2) 0.0351(16) 0.0225(17) -0.0092(13) 0.0042(15) 0.0062(15) C12 0.043(2) 0.0311(16) 0.0307(17) -0.0079(13) -0.0085(15) -0.0017(14) Sb1 0.02196(12) 0.01933(10) 0.02078(11) -0.00029(7) -0.00126(8) 0.00006(7) S1 0.0268(4) 0.0387(4) 0.0376(5) -0.0082(4) 0.0046(3) 0.0037(3) S2 0.0240(4) 0.0453(4) 0.0319(4) -0.0041(4) -0.0038(3) -0.0061(3) S3 0.0358(5) 0.0194(4) 0.0519(5) -0.0034(3) -0.0026(4) -0.0005(3) S4 0.0787(7) 0.0322(4) 0.0230(4) 0.0052(3) -0.0028(4) 0.0063(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 Eu1 N2 2.518(2) . ? Eu1 N7 2.527(2) . ? Eu1 N6 2.536(2) . ? Eu1 N3 2.537(2) . ? Eu1 N5 2.558(2) . ? Eu1 N4 2.571(2) . ? Eu1 N8 2.594(2) . ? Eu1 N1 2.596(3) . ? N1 C1 1.474(4) . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 C3 1.475(4) . ? N2 C2 1.481(4) . ? N2 H2C 0.9100 . ? N3 C5 1.478(4) . ? N3 C4 1.483(4) . ? N3 H3C 0.9100 . ? N4 C6 1.482(4) . ? N4 H4C 0.9000 . ? N4 H4D 0.9000 . ? N5 C7 1.479(4) . ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N6 C8 1.478(4) . ? N6 C9 1.483(4) . ? N6 H6C 0.9100 . ? N7 C11 1.477(4) . ? N7 C10 1.480(4) . ? N7 H7C 0.9100 . ? N8 C12 1.473(4) . ? N8 H8C 0.9000 . ? N8 H8D 0.9000 . ? C1 C2 1.495(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.505(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.504(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.508(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.513(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.495(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? Sb1 S2 2.3226(9) . ? Sb1 S3 2.3246(9) . ? Sb1 S4 2.3302(9) . ? Sb1 S1 2.3420(8) . ? 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 N2 Eu1 N7 117.93(8) . . ? N2 Eu1 N6 144.84(8) . . ? N7 Eu1 N6 68.52(8) . . ? N2 Eu1 N3 68.13(8) . . ? N7 Eu1 N3 141.12(8) . . ? N6 Eu1 N3 130.76(8) . . ? N2 Eu1 N5 93.17(8) . . ? N7 Eu1 N5 135.17(8) . . ? N6 Eu1 N5 67.75(8) . . ? N3 Eu1 N5 78.37(8) . . ? N2 Eu1 N4 133.67(8) . . ? N7 Eu1 N4 87.13(8) . . ? N6 Eu1 N4 78.81(8) . . ? N3 Eu1 N4 68.62(8) . . ? N5 Eu1 N4 93.76(8) . . ? N2 Eu1 N8 76.84(7) . . ? N7 Eu1 N8 67.03(8) . . ? N6 Eu1 N8 130.86(8) . . ? N3 Eu1 N8 78.50(8) . . ? N5 Eu1 N8 156.83(8) . . ? N4 Eu1 N8 79.13(8) . . ? N2 Eu1 N1 67.79(8) . . ? N7 Eu1 N1 78.47(9) . . ? N6 Eu1 N1 81.03(8) . . ? N3 Eu1 N1 131.80(9) . . ? N5 Eu1 N1 85.53(9) . . ? N4 Eu1 N1 158.47(9) . . ? N8 Eu1 N1 109.10(9) . . ? C1 N1 Eu1 109.14(18) . . ? C1 N1 H1C 109.9 . . ? Eu1 N1 H1C 109.9 . . ? C1 N1 H1D 109.9 . . ? Eu1 N1 H1D 109.9 . . ? H1C N1 H1D 108.3 . . ? C3 N2 C2 114.5(2) . . ? C3 N2 Eu1 113.93(19) . . ? C2 N2 Eu1 114.65(19) . . ? C3 N2 H2C 104.0 . . ? C2 N2 H2C 104.0 . . ? Eu1 N2 H2C 104.0 . . ? C5 N3 C4 114.0(2) . . ? C5 N3 Eu1 112.86(18) . . ? C4 N3 Eu1 111.47(18) . . ? C5 N3 H3C 105.9 . . ? C4 N3 H3C 105.9 . . ? Eu1 N3 H3C 105.9 . . ? C6 N4 Eu1 110.56(18) . . ? C6 N4 H4C 109.5 . . ? Eu1 N4 H4C 109.5 . . ? C6 N4 H4D 109.5 . . ? Eu1 N4 H4D 109.5 . . ? H4C N4 H4D 108.1 . . ? C7 N5 Eu1 113.76(18) . . ? C7 N5 H5C 108.8 . . ? Eu1 N5 H5C 108.8 . . ? C7 N5 H5D 108.8 . . ? Eu1 N5 H5D 108.8 . . ? H5C N5 H5D 107.7 . . ? C8 N6 C9 114.4(2) . . ? C8 N6 Eu1 112.41(18) . . ? C9 N6 Eu1 112.06(18) . . ? C8 N6 H6C 105.7 . . ? C9 N6 H6C 105.7 . . ? Eu1 N6 H6C 105.7 . . ? C11 N7 C10 112.3(2) . . ? C11 N7 Eu1 115.01(18) . . ? C10 N7 Eu1 111.78(19) . . ? C11 N7 H7C 105.6 . . ? C10 N7 H7C 105.6 . . ? Eu1 N7 H7C 105.6 . . ? C12 N8 Eu1 110.84(17) . . ? C12 N8 H8C 109.5 . . ? Eu1 N8 H8C 109.5 . . ? C12 N8 H8D 109.5 . . ? Eu1 N8 H8D 109.5 . . ? H8C N8 H8D 108.1 . . ? N1 C1 C2 109.7(3) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 108.2(3) . . ? N2 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? N2 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? N2 C3 C4 108.4(2) . . ? N2 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? N2 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? N3 C4 C3 108.8(2) . . ? N3 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? N3 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? N3 C5 C6 109.3(2) . . ? N3 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? N3 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? N4 C6 C5 110.2(3) . . ? N4 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? N4 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? N5 C7 C8 110.7(3) . . ? N5 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? N5 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? N6 C8 C7 108.3(2) . . ? N6 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? N6 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? N6 C9 C10 107.6(3) . . ? N6 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? N6 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? N7 C10 C9 108.9(3) . . ? N7 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? N7 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? N7 C11 C12 108.4(2) . . ? N7 C11 H11A 110.0 . . ? C12 C11 H11A 110.0 . . ? N7 C11 H11B 110.0 . . ? C12 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? N8 C12 C11 109.0(2) . . ? N8 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? N8 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? S2 Sb1 S3 109.72(3) . . ? S2 Sb1 S4 108.44(3) . . ? S3 Sb1 S4 111.25(3) . . ? S2 Sb1 S1 104.25(3) . . ? S3 Sb1 S1 112.61(3) . . ? S4 Sb1 S1 110.27(3) . . ? 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 N2 Eu1 N1 C1 20.3(2) . . . . ? N7 Eu1 N1 C1 -106.5(2) . . . . ? N6 Eu1 N1 C1 -176.3(2) . . . . ? N3 Eu1 N1 C1 45.5(3) . . . . ? N5 Eu1 N1 C1 115.6(2) . . . . ? N4 Eu1 N1 C1 -155.5(2) . . . . ? N8 Eu1 N1 C1 -46.0(2) . . . . ? N7 Eu1 N2 C3 -151.01(19) . . . . ? N6 Eu1 N2 C3 117.1(2) . . . . ? N3 Eu1 N2 C3 -13.58(19) . . . . ? N5 Eu1 N2 C3 62.6(2) . . . . ? N4 Eu1 N2 C3 -35.7(2) . . . . ? N8 Eu1 N2 C3 -96.3(2) . . . . ? N1 Eu1 N2 C3 146.4(2) . . . . ? N7 Eu1 N2 C2 74.3(2) . . . . ? N6 Eu1 N2 C2 -17.5(3) . . . . ? N3 Eu1 N2 C2 -148.2(2) . . . . ? N5 Eu1 N2 C2 -72.1(2) . . . . ? N4 Eu1 N2 C2 -170.4(2) . . . . ? N8 Eu1 N2 C2 129.1(2) . . . . ? N1 Eu1 N2 C2 11.8(2) . . . . ? N2 Eu1 N3 C5 -148.4(2) . . . . ? N7 Eu1 N3 C5 -40.6(3) . . . . ? N6 Eu1 N3 C5 66.8(2) . . . . ? N5 Eu1 N3 C5 113.3(2) . . . . ? N4 Eu1 N3 C5 14.58(19) . . . . ? N8 Eu1 N3 C5 -68.1(2) . . . . ? N1 Eu1 N3 C5 -173.55(19) . . . . ? N2 Eu1 N3 C4 -18.57(18) . . . . ? N7 Eu1 N3 C4 89.3(2) . . . . ? N6 Eu1 N3 C4 -163.36(17) . . . . ? N5 Eu1 N3 C4 -116.81(19) . . . . ? N4 Eu1 N3 C4 144.4(2) . . . . ? N8 Eu1 N3 C4 61.73(19) . . . . ? N1 Eu1 N3 C4 -43.7(2) . . . . ? N2 Eu1 N4 C6 38.7(2) . . . . ? N7 Eu1 N4 C6 165.6(2) . . . . ? N6 Eu1 N4 C6 -125.7(2) . . . . ? N3 Eu1 N4 C6 16.69(19) . . . . ? N5 Eu1 N4 C6 -59.3(2) . . . . ? N8 Eu1 N4 C6 98.5(2) . . . . ? N1 Eu1 N4 C6 -146.6(2) . . . . ? N2 Eu1 N5 C7 157.6(2) . . . . ? N7 Eu1 N5 C7 21.5(3) . . . . ? N6 Eu1 N5 C7 8.09(19) . . . . ? N3 Eu1 N5 C7 -135.5(2) . . . . ? N4 Eu1 N5 C7 -68.2(2) . . . . ? N8 Eu1 N5 C7 -139.1(2) . . . . ? N1 Eu1 N5 C7 90.2(2) . . . . ? N2 Eu1 N6 C8 -39.0(3) . . . . ? N7 Eu1 N6 C8 -147.3(2) . . . . ? N3 Eu1 N6 C8 72.7(2) . . . . ? N5 Eu1 N6 C8 22.54(18) . . . . ? N4 Eu1 N6 C8 121.3(2) . . . . ? N8 Eu1 N6 C8 -173.82(17) . . . . ? N1 Eu1 N6 C8 -66.3(2) . . . . ? N2 Eu1 N6 C9 91.5(2) . . . . ? N7 Eu1 N6 C9 -16.9(2) . . . . ? N3 Eu1 N6 C9 -156.81(19) . . . . ? N5 Eu1 N6 C9 153.0(2) . . . . ? N4 Eu1 N6 C9 -108.2(2) . . . . ? N8 Eu1 N6 C9 -43.4(2) . . . . ? N1 Eu1 N6 C9 64.2(2) . . . . ? N2 Eu1 N7 C11 72.5(2) . . . . ? N6 Eu1 N7 C11 -145.7(2) . . . . ? N3 Eu1 N7 C11 -16.7(3) . . . . ? N5 Eu1 N7 C11 -159.07(18) . . . . ? N4 Eu1 N7 C11 -66.6(2) . . . . ? N8 Eu1 N7 C11 12.78(19) . . . . ? N1 Eu1 N7 C11 129.5(2) . . . . ? N2 Eu1 N7 C10 -157.9(2) . . . . ? N6 Eu1 N7 C10 -16.2(2) . . . . ? N3 Eu1 N7 C10 112.9(2) . . . . ? N5 Eu1 N7 C10 -29.5(3) . . . . ? N4 Eu1 N7 C10 62.9(2) . . . . ? N8 Eu1 N7 C10 142.4(2) . . . . ? N1 Eu1 N7 C10 -101.0(2) . . . . ? N2 Eu1 N8 C12 -109.02(19) . . . . ? N7 Eu1 N8 C12 19.40(18) . . . . ? N6 Eu1 N8 C12 46.2(2) . . . . ? N3 Eu1 N8 C12 -179.0(2) . . . . ? N5 Eu1 N8 C12 -175.3(2) . . . . ? N4 Eu1 N8 C12 110.89(19) . . . . ? N1 Eu1 N8 C12 -48.5(2) . . . . ? Eu1 N1 C1 C2 -50.9(3) . . . . ? C3 N2 C2 C1 -176.6(3) . . . . ? Eu1 N2 C2 C1 -42.2(3) . . . . ? N1 C1 C2 N2 62.7(3) . . . . ? C2 N2 C3 C4 178.2(3) . . . . ? Eu1 N2 C3 C4 43.5(3) . . . . ? C5 N3 C4 C3 177.6(3) . . . . ? Eu1 N3 C4 C3 48.4(3) . . . . ? N2 C3 C4 N3 -61.0(3) . . . . ? C4 N3 C5 C6 -172.6(3) . . . . ? Eu1 N3 C5 C6 -44.1(3) . . . . ? Eu1 N4 C6 C5 -46.4(3) . . . . ? N3 C5 C6 N4 61.3(3) . . . . ? Eu1 N5 C7 C8 -37.3(3) . . . . ? C9 N6 C8 C7 -179.5(3) . . . . ? Eu1 N6 C8 C7 -50.2(3) . . . . ? N5 C7 C8 N6 58.1(3) . . . . ? C8 N6 C9 C10 176.6(3) . . . . ? Eu1 N6 C9 C10 47.1(3) . . . . ? C11 N7 C10 C9 178.2(3) . . . . ? Eu1 N7 C10 C9 47.2(3) . . . . ? N6 C9 C10 N7 -63.1(4) . . . . ? C10 N7 C11 C12 -172.4(3) . . . . ? Eu1 N7 C11 C12 -43.1(3) . . . . ? Eu1 N8 C12 C11 -49.4(3) . . . . ? N7 C11 C12 N8 61.5(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 N1 H1C S4 0.90 2.86 3.654(3) 148.7 8_576 N2 H2C S2 0.91 2.43 3.324(3) 166.3 7_755 N3 H3C S2 0.91 2.71 3.382(3) 131.3 8_575 N4 H4C S1 0.90 2.67 3.565(3) 173.4 4_646 N4 H4D S3 0.90 2.64 3.483(3) 156.3 . N5 H5C S1 0.90 2.73 3.526(3) 148.0 8_575 N5 H5D S4 0.90 2.54 3.389(3) 157.7 1_545 N6 H6C S1 0.91 2.55 3.440(3) 164.3 4_646 N7 H7C S4 0.91 2.49 3.377(3) 163.7 8_576 N8 H8C S2 0.90 2.59 3.386(3) 147.6 7_755 N8 H8D S3 0.90 2.66 3.527(2) 162.8 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.820 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.121 # Attachment '- 2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 865324' #TrackingRef '- 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H36 Gd N8, S4 Sb ' _chemical_formula_sum 'C12 H36 Gd N8 S4 Sb' _chemical_formula_weight 699.78 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' Cl Cl 0.1484 0.1585 '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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.440(3) _cell_length_b 13.324(3) _cell_length_c 26.002(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4656.3(17) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.57 _cell_measurement_theta_max 25.10 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.997 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 4.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1868 _exptl_absorpt_correction_T_max 0.2838 _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 24785 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4145 _reflns_number_gt 3139 _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^)+(0.0156P)^2^+4.2708P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000285(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4145 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0500 _refine_ls_wR_factor_gt 0.0456 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 Gd1 Gd 0.028945(14) 0.710206(15) 0.124643(7) 0.01958(7) Uani 1 1 d . . . Sb1 Sb 0.016451(19) 0.23352(2) 0.125922(12) 0.02281(8) Uani 1 1 d . . . S4 S -0.15338(8) 0.20640(10) 0.11967(4) 0.0374(3) Uani 1 1 d . . . S3 S 0.10426(9) 0.08236(9) 0.12806(6) 0.0448(3) Uani 1 1 d . . . S2 S 0.07720(9) 0.33731(9) 0.06036(4) 0.0357(3) Uani 1 1 d . . . S1 S 0.05093(9) 0.32122(9) 0.20074(4) 0.0368(3) Uani 1 1 d . . . N1 N -0.1203(2) 0.7754(3) 0.17668(13) 0.0272(8) Uani 1 1 d . . . H1C H -0.1761 0.7445 0.1660 0.033 Uiso 1 1 calc R . . H1D H -0.1114 0.7607 0.2102 0.033 Uiso 1 1 calc R . . N8 N -0.1152(2) 0.6351(3) 0.07394(13) 0.0324(9) Uani 1 1 d . . . H8C H -0.1708 0.6709 0.0800 0.039 Uiso 1 1 calc R . . H8D H -0.1017 0.6387 0.0401 0.039 Uiso 1 1 calc R . . N6 N 0.0875(3) 0.6952(3) 0.21578(13) 0.0312(9) Uani 1 1 d . . . H6C H 0.0446 0.7345 0.2339 0.037 Uiso 1 1 calc R . . N2 N -0.0306(3) 0.8790(3) 0.09456(13) 0.0310(9) Uani 1 1 d . . . H2C H 0.0140 0.9241 0.1072 0.037 Uiso 1 1 calc R . . N7 N -0.0332(3) 0.5509(3) 0.16613(13) 0.0300(9) Uani 1 1 d . . . H7C H 0.0104 0.5018 0.1569 0.036 Uiso 1 1 calc R . . N4 N 0.1543(3) 0.5816(3) 0.09270(13) 0.0331(9) Uani 1 1 d . . . H4C H 0.2112 0.5888 0.1106 0.040 Uiso 1 1 calc R . . H4D H 0.1305 0.5197 0.0991 0.040 Uiso 1 1 calc R . . C1 C -0.1316(3) 0.8845(3) 0.17063(16) 0.0344(11) Uani 1 1 d . . . H1A H -0.0785 0.9190 0.1887 0.041 Uiso 1 1 calc R . . H1B H -0.1946 0.9059 0.1852 0.041 Uiso 1 1 calc R . . C11 C -0.1312(3) 0.5192(4) 0.14663(18) 0.0389(12) Uani 1 1 d . . . H11A H -0.1829 0.5609 0.1614 0.047 Uiso 1 1 calc R . . H11B H -0.1439 0.4501 0.1564 0.047 Uiso 1 1 calc R . . N5 N 0.1815(3) 0.8212(3) 0.14319(14) 0.0429(11) Uani 1 1 d . . . H5C H 0.2368 0.7910 0.1313 0.052 Uiso 1 1 calc R . . H5D H 0.1748 0.8804 0.1269 0.052 Uiso 1 1 calc R . . N3 N 0.0828(3) 0.7448(3) 0.03347(13) 0.0307(9) Uani 1 1 d . . . H3C H 0.0375 0.7131 0.0131 0.037 Uiso 1 1 calc R . . C12 C -0.1319(4) 0.5290(4) 0.08868(18) 0.0433(13) Uani 1 1 d . . . H12A H -0.0801 0.4872 0.0740 0.052 Uiso 1 1 calc R . . H12B H -0.1954 0.5063 0.0753 0.052 Uiso 1 1 calc R . . C5 C 0.1801(3) 0.6984(4) 0.02110(17) 0.0378(12) Uani 1 1 d . . . H5A H 0.2330 0.7331 0.0392 0.045 Uiso 1 1 calc R . . H5B H 0.1928 0.7031 -0.0155 0.045 Uiso 1 1 calc R . . C10 C -0.0286(4) 0.5573(3) 0.22301(17) 0.0404(12) Uani 1 1 d . . . H10A H -0.0405 0.4917 0.2380 0.048 Uiso 1 1 calc R . . H10B H -0.0791 0.6031 0.2356 0.048 Uiso 1 1 calc R . . C2 C -0.1280(3) 0.9103(3) 0.11471(16) 0.0348(11) Uani 1 1 d . . . H2A H -0.1809 0.8758 0.0965 0.042 Uiso 1 1 calc R . . H2B H -0.1369 0.9819 0.1101 0.042 Uiso 1 1 calc R . . C9 C 0.0734(4) 0.5945(4) 0.23767(17) 0.0413(12) Uani 1 1 d . . . H9A H 0.0796 0.5971 0.2748 0.050 Uiso 1 1 calc R . . H9B H 0.1238 0.5491 0.2245 0.050 Uiso 1 1 calc R . . C7 C 0.1909(3) 0.8384(4) 0.19869(19) 0.0457(14) Uani 1 1 d . . . H7A H 0.1377 0.8819 0.2105 0.055 Uiso 1 1 calc R . . H7B H 0.2539 0.8710 0.2061 0.055 Uiso 1 1 calc R . . C4 C 0.0753(4) 0.8518(3) 0.02034(17) 0.0427(13) Uani 1 1 d . . . H4A H 0.0822 0.8609 -0.0165 0.051 Uiso 1 1 calc R . . H4B H 0.1276 0.8893 0.0373 0.051 Uiso 1 1 calc R . . C6 C 0.1769(4) 0.5901(4) 0.03732(16) 0.0413(12) Uani 1 1 d . . . H6A H 0.1264 0.5550 0.0176 0.050 Uiso 1 1 calc R . . H6B H 0.2406 0.5588 0.0302 0.050 Uiso 1 1 calc R . . C8 C 0.1857(4) 0.7395(4) 0.2260(2) 0.0452(14) Uani 1 1 d . . . H8A H 0.2378 0.6952 0.2137 0.054 Uiso 1 1 calc R . . H8B H 0.1947 0.7491 0.2627 0.054 Uiso 1 1 calc R . . C3 C -0.0253(4) 0.8886(4) 0.03791(17) 0.0487(14) Uani 1 1 d . . . H3A H -0.0343 0.9581 0.0280 0.058 Uiso 1 1 calc R . . H3B H -0.0774 0.8490 0.0220 0.058 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 Gd1 0.02025(11) 0.01963(12) 0.01886(10) 0.00023(9) 0.00014(9) -0.00082(8) Sb1 0.02086(14) 0.02337(16) 0.02421(15) -0.00127(13) -0.00003(14) -0.00004(11) S4 0.0200(5) 0.0551(8) 0.0373(7) -0.0013(6) -0.0009(5) -0.0040(5) S3 0.0317(6) 0.0242(6) 0.0785(9) -0.0050(7) 0.0076(7) 0.0045(5) S2 0.0407(7) 0.0406(7) 0.0258(6) 0.0045(5) 0.0032(5) -0.0070(6) S1 0.0490(7) 0.0357(7) 0.0257(6) -0.0039(5) -0.0063(5) -0.0042(6) N1 0.027(2) 0.030(2) 0.0242(19) 0.0016(16) 0.0001(16) 0.0029(17) N8 0.027(2) 0.045(3) 0.026(2) -0.0039(17) 0.0008(16) -0.0042(18) N6 0.031(2) 0.036(2) 0.0274(19) 0.0024(17) -0.0024(16) 0.0057(18) N2 0.038(2) 0.023(2) 0.032(2) 0.0006(16) 0.0036(18) -0.0010(17) N7 0.030(2) 0.021(2) 0.039(2) 0.0017(16) 0.0065(17) 0.0007(17) N4 0.031(2) 0.034(2) 0.034(2) 0.0012(18) 0.0048(17) 0.0050(18) C1 0.029(2) 0.034(3) 0.040(3) -0.005(2) 0.002(2) 0.011(2) C11 0.034(3) 0.029(3) 0.054(3) 0.004(2) 0.008(2) -0.008(2) N5 0.035(2) 0.052(3) 0.042(2) -0.001(2) -0.0021(18) -0.013(2) N3 0.034(2) 0.033(2) 0.025(2) 0.0012(15) 0.0036(18) -0.0061(17) C12 0.032(3) 0.038(3) 0.060(4) -0.018(3) 0.001(2) -0.005(2) C5 0.031(3) 0.056(4) 0.026(2) 0.000(2) 0.0046(19) -0.002(2) C10 0.060(3) 0.030(3) 0.032(3) 0.011(2) 0.013(2) 0.007(3) C2 0.034(3) 0.026(3) 0.045(3) 0.006(2) -0.001(2) 0.006(2) C9 0.058(3) 0.040(3) 0.026(3) 0.009(2) -0.004(2) 0.011(3) C7 0.026(3) 0.055(4) 0.055(3) -0.023(3) -0.004(2) -0.003(2) C4 0.067(4) 0.032(3) 0.029(3) 0.010(2) 0.013(2) -0.001(3) C6 0.038(3) 0.054(4) 0.031(3) -0.008(2) 0.008(2) 0.014(3) C8 0.033(3) 0.065(4) 0.037(3) -0.002(3) -0.013(2) -0.001(3) C3 0.071(4) 0.035(3) 0.039(3) 0.017(2) 0.006(3) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 N6 2.505(3) . ? Gd1 N2 2.511(3) . ? Gd1 N3 2.521(3) . ? Gd1 N7 2.523(3) . ? Gd1 N4 2.542(3) . ? Gd1 N8 2.548(3) . ? Gd1 N1 2.570(3) . ? Gd1 N5 2.574(4) . ? Sb1 S1 2.3162(12) . ? Sb1 S4 2.3168(11) . ? Sb1 S3 2.3350(12) . ? Sb1 S2 2.3421(12) . ? N1 C1 1.470(5) . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N8 C12 1.483(6) . ? N8 H8C 0.9000 . ? N8 H8D 0.9000 . ? N6 C8 1.470(6) . ? N6 C9 1.470(5) . ? N6 H6C 0.9100 . ? N2 C2 1.471(5) . ? N2 C3 1.480(5) . ? N2 H2C 0.9100 . ? N7 C11 1.473(5) . ? N7 C10 1.483(5) . ? N7 H7C 0.9100 . ? N4 C6 1.476(5) . ? N4 H4C 0.9000 . ? N4 H4D 0.9000 . ? C1 C2 1.495(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C11 C12 1.512(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N5 C7 1.467(6) . ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N3 C4 1.470(5) . ? N3 C5 1.482(5) . ? N3 H3C 0.9100 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C5 C6 1.504(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C10 C9 1.507(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C7 C8 1.500(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C4 C3 1.508(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 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 Gd1 N2 117.79(12) . . ? N6 Gd1 N3 144.49(12) . . ? N2 Gd1 N3 68.58(11) . . ? N6 Gd1 N7 68.43(12) . . ? N2 Gd1 N7 141.35(12) . . ? N3 Gd1 N7 130.60(11) . . ? N6 Gd1 N4 92.69(11) . . ? N2 Gd1 N4 135.44(11) . . ? N3 Gd1 N4 68.03(11) . . ? N7 Gd1 N4 78.00(11) . . ? N6 Gd1 N8 134.20(11) . . ? N2 Gd1 N8 87.03(12) . . ? N3 Gd1 N8 78.65(11) . . ? N7 Gd1 N8 68.86(12) . . ? N4 Gd1 N8 94.03(12) . . ? N6 Gd1 N1 76.95(11) . . ? N2 Gd1 N1 67.23(11) . . ? N3 Gd1 N1 131.08(11) . . ? N7 Gd1 N1 78.52(11) . . ? N4 Gd1 N1 156.45(11) . . ? N8 Gd1 N1 79.16(11) . . ? N6 Gd1 N5 67.56(12) . . ? N2 Gd1 N5 78.31(13) . . ? N3 Gd1 N5 80.94(12) . . ? N7 Gd1 N5 131.84(12) . . ? N4 Gd1 N5 85.45(13) . . ? N8 Gd1 N5 158.16(12) . . ? N1 Gd1 N5 109.18(12) . . ? S1 Sb1 S4 109.56(4) . . ? S1 Sb1 S3 108.30(5) . . ? S4 Sb1 S3 111.42(5) . . ? S1 Sb1 S2 104.11(5) . . ? S4 Sb1 S2 112.61(4) . . ? S3 Sb1 S2 110.51(5) . . ? C1 N1 Gd1 111.0(2) . . ? C1 N1 H1C 109.4 . . ? Gd1 N1 H1C 109.4 . . ? C1 N1 H1D 109.4 . . ? Gd1 N1 H1D 109.4 . . ? H1C N1 H1D 108.0 . . ? C12 N8 Gd1 110.9(3) . . ? C12 N8 H8C 109.5 . . ? Gd1 N8 H8C 109.5 . . ? C12 N8 H8D 109.5 . . ? Gd1 N8 H8D 109.5 . . ? H8C N8 H8D 108.1 . . ? C8 N6 C9 114.3(4) . . ? C8 N6 Gd1 114.9(3) . . ? C9 N6 Gd1 113.5(3) . . ? C8 N6 H6C 104.1 . . ? C9 N6 H6C 104.1 . . ? Gd1 N6 H6C 104.1 . . ? C2 N2 C3 111.9(4) . . ? C2 N2 Gd1 115.2(3) . . ? C3 N2 Gd1 111.8(3) . . ? C2 N2 H2C 105.7 . . ? C3 N2 H2C 105.7 . . ? Gd1 N2 H2C 105.7 . . ? C11 N7 C10 113.4(4) . . ? C11 N7 Gd1 113.0(3) . . ? C10 N7 Gd1 111.4(3) . . ? C11 N7 H7C 106.2 . . ? C10 N7 H7C 106.2 . . ? Gd1 N7 H7C 106.2 . . ? C6 N4 Gd1 113.8(3) . . ? C6 N4 H4C 108.8 . . ? Gd1 N4 H4C 108.8 . . ? C6 N4 H4D 108.8 . . ? Gd1 N4 H4D 108.8 . . ? H4C N4 H4D 107.7 . . ? N1 C1 C2 109.1(3) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N7 C11 C12 108.9(4) . . ? N7 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? N7 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C7 N5 Gd1 110.1(3) . . ? C7 N5 H5C 109.6 . . ? Gd1 N5 H5C 109.6 . . ? C7 N5 H5D 109.6 . . ? Gd1 N5 H5D 109.6 . . ? H5C N5 H5D 108.2 . . ? C4 N3 C5 114.5(4) . . ? C4 N3 Gd1 112.1(3) . . ? C5 N3 Gd1 112.4(3) . . ? C4 N3 H3C 105.6 . . ? C5 N3 H3C 105.6 . . ? Gd1 N3 H3C 105.6 . . ? N8 C12 C11 109.8(4) . . ? N8 C12 H12A 109.7 . . ? C11 C12 H12A 109.7 . . ? N8 C12 H12B 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? N3 C5 C6 108.3(4) . . ? N3 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? N3 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? N7 C10 C9 108.0(4) . . ? N7 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? N7 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? N2 C2 C1 108.1(3) . . ? N2 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? N2 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? N6 C9 C10 108.6(4) . . ? N6 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? N6 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.3 . . ? N5 C7 C8 109.0(4) . . ? N5 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? N5 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? N3 C4 C3 107.8(4) . . ? N3 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? N3 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.5 . . ? N4 C6 C5 110.6(4) . . ? N4 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? N4 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N6 C8 C7 108.0(4) . . ? N6 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 . . ? N6 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? N2 C3 C4 108.5(4) . . ? N2 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? N2 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.526 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.095 # Attachment '- 3.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 865325' #TrackingRef '- 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H36 Er N8, S4 Sb ' _chemical_formula_sum 'C12 H36 Er N8 S4 Sb ' _chemical_formula_weight 709.79 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 '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 Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.441(3) _cell_length_b 13.312(3) _cell_length_c 26.026(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4656.7(17) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 25.10 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.025 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 5.114 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1767 _exptl_absorpt_correction_T_max 0.3505 _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 25151 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4142 _reflns_number_gt 2915 _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^)+(0.0198P)^2^+6.2292P] 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 4142 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0600 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Er1 Er 0.527569(18) 0.289383(17) 0.375344(9) 0.01944(8) Uani 1 1 d . . . Sb1 Sb 0.51665(3) 0.76638(2) 0.374142(15) 0.01839(9) Uani 1 1 d . . . S4 S 0.34661(11) 0.79397(12) 0.38038(6) 0.0327(4) Uani 1 1 d . . . S3 S 0.60426(12) 0.91766(11) 0.37246(7) 0.0415(4) Uani 1 1 d . . . S2 S 0.57718(12) 0.66222(12) 0.43974(5) 0.0313(4) Uani 1 1 d . . . S1 S 0.55105(12) 0.67851(11) 0.29923(5) 0.0309(4) Uani 1 1 d . . . N5 N 0.3803(3) 0.2252(3) 0.32309(16) 0.0216(10) Uani 1 1 d . . . H5C H 0.3245 0.2566 0.3335 0.026 Uiso 1 1 calc R . . H5D H 0.3898 0.2401 0.2897 0.026 Uiso 1 1 calc R . . N4 N 0.3852(3) 0.3630(3) 0.42622(17) 0.0277(12) Uani 1 1 d . . . H4C H 0.3298 0.3269 0.4203 0.033 Uiso 1 1 calc R . . H4D H 0.3992 0.3588 0.4600 0.033 Uiso 1 1 calc R . . N2 N 0.5860(3) 0.3047(3) 0.28505(16) 0.0260(11) Uani 1 1 d . . . H2C H 0.5432 0.2653 0.2670 0.031 Uiso 1 1 calc R . . N6 N 0.4684(4) 0.1217(3) 0.40469(16) 0.0254(11) Uani 1 1 d . . . H6C H 0.5128 0.0766 0.3918 0.030 Uiso 1 1 calc R . . N8 N 0.6526(3) 0.4167(3) 0.40593(16) 0.0274(11) Uani 1 1 d . . . H8C H 0.7092 0.4089 0.3878 0.033 Uiso 1 1 calc R . . H8D H 0.6290 0.4786 0.3994 0.033 Uiso 1 1 calc R . . N3 N 0.4654(3) 0.4475(3) 0.33424(17) 0.0262(11) Uani 1 1 d . . . H3C H 0.5091 0.4963 0.3437 0.031 Uiso 1 1 calc R . . C5 C 0.3673(5) 0.4801(4) 0.3545(2) 0.0315(15) Uani 1 1 d . . . H5A H 0.3148 0.4395 0.3395 0.038 Uiso 1 1 calc R . . H5B H 0.3554 0.5497 0.3454 0.038 Uiso 1 1 calc R . . C7 C 0.3672(4) 0.1160(4) 0.3286(2) 0.0289(14) Uani 1 1 d . . . H7A H 0.4197 0.0808 0.3104 0.035 Uiso 1 1 calc R . . H7B H 0.3038 0.0957 0.3142 0.035 Uiso 1 1 calc R . . N1 N 0.6791(4) 0.1791(4) 0.35810(18) 0.0363(13) Uani 1 1 d . . . H1C H 0.7342 0.2096 0.3700 0.044 Uiso 1 1 calc R . . H1D H 0.6723 0.1201 0.3746 0.044 Uiso 1 1 calc R . . C6 C 0.3671(5) 0.4684(5) 0.4126(2) 0.0370(16) Uani 1 1 d . . . H6A H 0.4184 0.5105 0.4275 0.044 Uiso 1 1 calc R . . H6B H 0.3033 0.4897 0.4262 0.044 Uiso 1 1 calc R . . N7 N 0.5816(4) 0.2553(3) 0.46598(17) 0.0247(12) Uani 1 1 d . . . H7C H 0.5367 0.2874 0.4863 0.030 Uiso 1 1 calc R . . C8 C 0.3710(4) 0.0903(4) 0.3849(2) 0.0293(14) Uani 1 1 d . . . H8A H 0.3183 0.1250 0.4032 0.035 Uiso 1 1 calc R . . H8B H 0.3622 0.0186 0.3897 0.035 Uiso 1 1 calc R . . C11 C 0.6790(4) 0.3011(5) 0.4782(2) 0.0321(15) Uani 1 1 d . . . H11A H 0.7317 0.2658 0.4603 0.039 Uiso 1 1 calc R . . H11B H 0.6917 0.2969 0.5148 0.039 Uiso 1 1 calc R . . C4 C 0.4706(5) 0.4431(4) 0.2775(2) 0.0351(16) Uani 1 1 d . . . H4A H 0.4596 0.5094 0.2631 0.042 Uiso 1 1 calc R . . H4B H 0.4198 0.3982 0.2643 0.042 Uiso 1 1 calc R . . C3 C 0.5722(5) 0.4054(4) 0.2627(2) 0.0328(15) Uani 1 1 d . . . H3A H 0.5780 0.4022 0.2256 0.039 Uiso 1 1 calc R . . H3B H 0.6229 0.4508 0.2756 0.039 Uiso 1 1 calc R . . C1 C 0.6890(4) 0.1613(5) 0.3024(2) 0.0351(15) Uani 1 1 d . . . H1A H 0.6358 0.1178 0.2906 0.042 Uiso 1 1 calc R . . H1B H 0.7519 0.1287 0.2952 0.042 Uiso 1 1 calc R . . C12 C 0.6761(5) 0.4090(5) 0.4616(2) 0.0351(15) Uani 1 1 d . . . H12A H 0.6261 0.4448 0.4813 0.042 Uiso 1 1 calc R . . H12B H 0.7401 0.4401 0.4682 0.042 Uiso 1 1 calc R . . C10 C 0.5738(5) 0.1476(4) 0.4796(2) 0.0365(16) Uani 1 1 d . . . H10A H 0.5796 0.1391 0.5165 0.044 Uiso 1 1 calc R . . H10B H 0.6267 0.1099 0.4631 0.044 Uiso 1 1 calc R . . C9 C 0.4738(5) 0.1104(5) 0.4614(2) 0.0431(18) Uani 1 1 d . . . H9A H 0.4654 0.0404 0.4708 0.052 Uiso 1 1 calc R . . H9B H 0.4211 0.1490 0.4775 0.052 Uiso 1 1 calc R . . C2 C 0.6839(5) 0.2599(5) 0.2752(2) 0.0405(18) Uani 1 1 d . . . H2A H 0.7360 0.3041 0.2876 0.049 Uiso 1 1 calc R . . H2B H 0.6932 0.2501 0.2386 0.049 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 Er1 0.01916(14) 0.02006(13) 0.01911(13) 0.00022(11) -0.00024(12) 0.00061(10) Sb1 0.0162(2) 0.01924(18) 0.01977(18) -0.00101(17) -0.00002(19) 0.00030(14) S4 0.0168(8) 0.0480(9) 0.0334(8) -0.0023(8) 0.0000(7) 0.0030(7) S3 0.0279(9) 0.0214(8) 0.0752(12) -0.0053(9) -0.0041(10) -0.0043(6) S2 0.0331(9) 0.0371(9) 0.0238(8) 0.0038(7) -0.0031(7) 0.0078(7) S1 0.0389(10) 0.0329(9) 0.0209(7) -0.0048(6) 0.0054(7) 0.0040(7) N5 0.023(3) 0.026(2) 0.016(2) 0.001(2) 0.003(2) -0.001(2) N4 0.021(3) 0.041(3) 0.021(3) -0.001(2) -0.001(2) 0.001(2) N2 0.026(3) 0.031(3) 0.021(2) 0.000(2) 0.005(2) -0.006(2) N6 0.027(3) 0.022(3) 0.027(3) 0.0023(19) -0.002(2) 0.003(2) N8 0.023(3) 0.031(3) 0.029(3) 0.000(2) -0.001(2) -0.007(2) N3 0.021(3) 0.024(3) 0.033(3) 0.003(2) -0.002(2) 0.002(2) C5 0.030(4) 0.020(3) 0.045(4) -0.001(3) -0.007(3) 0.007(3) C7 0.023(4) 0.029(3) 0.035(4) -0.009(3) -0.003(3) -0.006(3) N1 0.026(3) 0.044(3) 0.038(3) 0.002(2) 0.000(2) 0.011(3) C6 0.023(4) 0.037(4) 0.051(4) -0.014(3) -0.002(3) 0.007(3) N7 0.026(3) 0.025(3) 0.023(3) 0.0003(19) -0.001(2) 0.004(2) C8 0.027(4) 0.024(3) 0.036(4) 0.004(3) 0.007(3) -0.008(3) C11 0.030(4) 0.046(4) 0.020(3) -0.002(3) -0.003(3) 0.005(3) C4 0.050(5) 0.030(3) 0.026(3) 0.009(3) -0.011(3) -0.007(3) C3 0.042(4) 0.033(4) 0.023(3) 0.006(3) 0.003(3) -0.010(3) C1 0.022(4) 0.037(4) 0.047(4) -0.014(3) -0.001(3) 0.002(3) C12 0.031(4) 0.046(4) 0.028(3) -0.004(3) -0.002(3) -0.009(3) C10 0.055(5) 0.030(3) 0.024(3) 0.008(3) -0.011(3) 0.002(3) C9 0.066(5) 0.031(4) 0.032(4) 0.016(3) -0.015(4) -0.010(3) C2 0.032(5) 0.063(5) 0.026(4) -0.006(3) 0.007(3) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 N2 2.486(4) . ? Er1 N6 2.490(4) . ? Er1 N3 2.504(4) . ? Er1 N7 2.510(5) . ? Er1 N8 2.516(4) . ? Er1 N4 2.524(4) . ? Er1 N5 2.550(4) . ? Er1 N1 2.550(5) . ? Sb1 S1 2.3202(15) . ? Sb1 S4 2.3205(15) . ? Sb1 S3 2.3332(15) . ? Sb1 S2 2.3449(15) . ? N5 C7 1.471(6) . ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N4 C6 1.468(7) . ? N4 H4C 0.9000 . ? N4 H4D 0.9000 . ? N2 C2 1.467(8) . ? N2 C3 1.473(7) . ? N2 H2C 0.9100 . ? N6 C8 1.468(7) . ? N6 C9 1.485(7) . ? N6 H6C 0.9100 . ? N8 C12 1.485(7) . ? N8 H8C 0.9000 . ? N8 H8D 0.9000 . ? N3 C4 1.480(7) . ? N3 C5 1.485(7) . ? N3 H3C 0.9100 . ? C5 C6 1.519(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C7 C8 1.506(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? N1 C1 1.475(7) . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? N7 C11 1.478(7) . ? N7 C10 1.479(7) . ? N7 H7C 0.9100 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C11 C12 1.501(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C4 C3 1.505(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C1 C2 1.493(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C10 C9 1.508(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 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 N2 Er1 N6 117.67(15) . . ? N2 Er1 N3 68.45(15) . . ? N6 Er1 N3 141.08(16) . . ? N2 Er1 N7 144.26(16) . . ? N6 Er1 N7 69.02(14) . . ? N3 Er1 N7 130.56(14) . . ? N2 Er1 N8 91.87(14) . . ? N6 Er1 N8 136.07(14) . . ? N3 Er1 N8 77.99(15) . . ? N7 Er1 N8 68.35(14) . . ? N2 Er1 N4 134.71(15) . . ? N6 Er1 N4 86.85(15) . . ? N3 Er1 N4 69.22(15) . . ? N7 Er1 N4 78.27(15) . . ? N8 Er1 N4 94.53(15) . . ? N2 Er1 N5 76.64(14) . . ? N6 Er1 N5 67.36(14) . . ? N3 Er1 N5 78.16(14) . . ? N7 Er1 N5 131.73(14) . . ? N8 Er1 N5 155.97(14) . . ? N4 Er1 N5 79.71(15) . . ? N2 Er1 N1 68.19(15) . . ? N6 Er1 N1 78.05(16) . . ? N3 Er1 N1 132.44(15) . . ? N7 Er1 N1 80.21(15) . . ? N8 Er1 N1 84.83(16) . . ? N4 Er1 N1 157.05(14) . . ? N5 Er1 N1 109.47(15) . . ? S1 Sb1 S4 109.56(6) . . ? S1 Sb1 S3 108.59(6) . . ? S4 Sb1 S3 111.21(6) . . ? S1 Sb1 S2 104.16(6) . . ? S4 Sb1 S2 112.60(6) . . ? S3 Sb1 S2 110.42(6) . . ? C7 N5 Er1 111.8(3) . . ? C7 N5 H5C 109.3 . . ? Er1 N5 H5C 109.3 . . ? C7 N5 H5D 109.3 . . ? Er1 N5 H5D 109.3 . . ? H5C N5 H5D 107.9 . . ? C6 N4 Er1 111.7(3) . . ? C6 N4 H4C 109.3 . . ? Er1 N4 H4C 109.3 . . ? C6 N4 H4D 109.3 . . ? Er1 N4 H4D 109.3 . . ? H4C N4 H4D 107.9 . . ? C2 N2 C3 114.5(5) . . ? C2 N2 Er1 114.6(4) . . ? C3 N2 Er1 114.0(3) . . ? C2 N2 H2C 104.0 . . ? C3 N2 H2C 104.0 . . ? Er1 N2 H2C 104.0 . . ? C8 N6 C9 111.3(5) . . ? C8 N6 Er1 115.6(3) . . ? C9 N6 Er1 112.3(3) . . ? C8 N6 H6C 105.6 . . ? C9 N6 H6C 105.6 . . ? Er1 N6 H6C 105.6 . . ? C12 N8 Er1 113.9(3) . . ? C12 N8 H8C 108.8 . . ? Er1 N8 H8C 108.8 . . ? C12 N8 H8D 108.8 . . ? Er1 N8 H8D 108.8 . . ? H8C N8 H8D 107.7 . . ? C4 N3 C5 114.0(5) . . ? C4 N3 Er1 112.2(3) . . ? C5 N3 Er1 113.0(3) . . ? C4 N3 H3C 105.6 . . ? C5 N3 H3C 105.6 . . ? Er1 N3 H3C 105.6 . . ? N3 C5 C6 108.9(5) . . ? N3 C5 H5A 109.9 . . ? C6 C5 H5A 109.9 . . ? N3 C5 H5B 109.9 . . ? C6 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? N5 C7 C8 108.4(4) . . ? N5 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? N5 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? C1 N1 Er1 109.7(3) . . ? C1 N1 H1C 109.7 . . ? Er1 N1 H1C 109.7 . . ? C1 N1 H1D 109.7 . . ? Er1 N1 H1D 109.7 . . ? H1C N1 H1D 108.2 . . ? N4 C6 C5 109.8(5) . . ? N4 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? N4 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C11 N7 C10 114.3(5) . . ? C11 N7 Er1 112.5(3) . . ? C10 N7 Er1 112.3(3) . . ? C11 N7 H7C 105.6 . . ? C10 N7 H7C 105.6 . . ? Er1 N7 H7C 105.6 . . ? N6 C8 C7 107.8(4) . . ? N6 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 . . ? N6 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 . . ? H8A C8 H8B 108.5 . . ? N7 C11 C12 108.1(5) . . ? N7 C11 H11A 110.1 . . ? C12 C11 H11A 110.1 . . ? N7 C11 H11B 110.1 . . ? C12 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? N3 C4 C3 108.1(5) . . ? N3 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? N3 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? N2 C3 C4 108.5(4) . . ? N2 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? N2 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? N1 C1 C2 108.7(5) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N8 C12 C11 110.6(5) . . ? N8 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? N8 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? N7 C10 C9 107.9(5) . . ? N7 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? N7 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? N6 C9 C10 108.8(5) . . ? N6 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? N6 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N2 C2 C1 108.4(5) . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.534 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.123 # Attachment '- 4.CIF' data_4 _database_code_depnum_ccdc_archive 'CCDC 865326' #TrackingRef '- 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H48 N10 O2 S8 Sb2 Y2, 2(C16 H47 N10 O S3 Sb Y2), 2(Cl) ' _chemical_formula_sum 'C48 H142 Cl2 N30 O4 S14 Sb4 Y6 ' _chemical_formula_weight 2744.04 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 '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 Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.543(3) _cell_length_b 15.647(3) _cell_length_c 41.256(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10034(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 25.10 _exptl_crystal_description block _exptl_crystal_colour yellow _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 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5456 _exptl_absorpt_coefficient_mu 4.881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2711 _exptl_absorpt_correction_T_max 0.4497 _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 53992 _diffrn_reflns_av_R_equivalents 0.1127 _diffrn_reflns_av_sigmaI/netI 0.0763 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.10 _reflns_number_total 8926 _reflns_number_gt 5886 _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^)+(0.0420P)^2^+35.5910P] 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 8926 _refine_ls_number_parameters 487 _refine_ls_number_restraints 687 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1121 _refine_ls_wR_factor_gt 0.0977 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.063 _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 0.48803(4) 0.42854(4) 0.751422(13) 0.04334(19) Uani 1 1 d . . . Sb2 Sb 0.62591(3) 0.21379(3) 0.571225(12) 0.02460(14) Uani 1 1 d . . . Y1 Y 0.58737(5) 0.50025(5) 0.672888(17) 0.02491(19) Uani 1 1 d . . . Y2 Y 0.40558(5) 0.32621(5) 0.673290(18) 0.0285(2) Uani 1 1 d . . . Y3 Y 0.44510(5) 0.10378(5) 0.502821(17) 0.02193(18) Uani 1 1 d . . . S1 S 0.42167(14) 0.49213(15) 0.70382(5) 0.0365(5) Uani 1 1 d . . . S2 S 0.63272(16) 0.45477(17) 0.73570(5) 0.0486(7) Uani 1 1 d . . . S3 S 0.4685(2) 0.28418(17) 0.73497(6) 0.0590(8) Uani 1 1 d . . . S4 S 0.50629(13) 0.12232(13) 0.56900(5) 0.0314(5) Uani 1 1 d . . . S5 S 0.56645(15) 0.34948(13) 0.57250(5) 0.0368(5) Uani 1 1 d . . . S6 S 0.71025(14) 0.18927(14) 0.52562(5) 0.0352(5) Uani 1 1 d . . . S7 S 0.70435(16) 0.19378(17) 0.61792(6) 0.0495(7) Uani 1 1 d . . . Cl1 Cl 0.28119(17) 0.62569(18) 0.61822(6) 0.0614(7) Uani 1 1 d . . . O2 O 0.4251(3) -0.0385(3) 0.50217(11) 0.0250(12) Uani 1 1 d . . . O1 O 0.5170(3) 0.3917(3) 0.64934(12) 0.0309(13) Uani 1 1 d . . . N1 N 0.7092(4) 0.3925(4) 0.66631(16) 0.0396(16) Uani 1 1 d U . . H1C H 0.7075 0.3560 0.6832 0.048 Uiso 1 1 calc R . . H1D H 0.6995 0.3619 0.6482 0.048 Uiso 1 1 calc R . . N2 N 0.7362(4) 0.5673(4) 0.68007(15) 0.0321(14) Uani 1 1 d U . . H2C H 0.7508 0.5900 0.6605 0.038 Uiso 1 1 calc R . . N3 N 0.5807(4) 0.6528(4) 0.69492(15) 0.0323(14) Uani 1 1 d U . . H3C H 0.5672 0.6474 0.7163 0.039 Uiso 1 1 calc R . . N4 N 0.4943(4) 0.5965(4) 0.63792(15) 0.0338(14) Uani 1 1 d U . . H4C H 0.4390 0.5848 0.6435 0.041 Uiso 1 1 calc R . . N5 N 0.6449(4) 0.5201(4) 0.61501(14) 0.0335(14) Uani 1 1 d U . . H5C H 0.6981 0.5426 0.6164 0.040 Uiso 1 1 calc R . . H5D H 0.6502 0.4681 0.6059 0.040 Uiso 1 1 calc R . . N6 N 0.3783(5) 0.2740(5) 0.61543(16) 0.0453(16) Uani 1 1 d U . . H6C H 0.4294 0.2685 0.6054 0.054 Uiso 1 1 calc R . . H6D H 0.3544 0.2217 0.6165 0.054 Uiso 1 1 calc R . . N7 N 0.2975(5) 0.4183(5) 0.64163(17) 0.0508(17) Uani 1 1 d U . . H7C H 0.3164 0.4731 0.6435 0.061 Uiso 1 1 calc R . . N8 N 0.2592(5) 0.3361(5) 0.70124(19) 0.0540(17) Uani 1 1 d U . . H8C H 0.2690 0.3585 0.7213 0.065 Uiso 1 1 calc R . . N9 N 0.3351(5) 0.1806(5) 0.68241(18) 0.0499(16) Uani 1 1 d U . . H9C H 0.3093 0.1656 0.6634 0.060 Uiso 1 1 calc R . . N10 N 0.5091(5) 0.2034(5) 0.66426(19) 0.0517(18) Uani 1 1 d U . . H10C H 0.5363 0.2116 0.6452 0.062 Uiso 1 1 calc R . . H10D H 0.5492 0.2046 0.6800 0.062 Uiso 1 1 calc R . . N11 N 0.3980(5) 0.2559(4) 0.51412(17) 0.0415(15) Uani 1 1 d U . . H11C H 0.3402 0.2576 0.5139 0.050 Uiso 1 1 calc R . . H11D H 0.4154 0.2701 0.5342 0.050 Uiso 1 1 calc R . . N12 N 0.5407(5) 0.2205(4) 0.47580(15) 0.0372(14) Uani 1 1 d U . . H12C H 0.5953 0.2094 0.4826 0.045 Uiso 1 1 calc R . . N13 N 0.4545(5) 0.0885(5) 0.44213(15) 0.0370(15) Uani 1 1 d U . . H13C H 0.4622 0.0315 0.4389 0.044 Uiso 1 1 calc R . . N14 N 0.2973(4) 0.1030(5) 0.47568(16) 0.0385(15) Uani 1 1 d U . . H14C H 0.2810 0.1587 0.4740 0.046 Uiso 1 1 calc R . . N15 N 0.3203(4) 0.0824(5) 0.54260(16) 0.0407(16) Uani 1 1 d U . . H15C H 0.3242 0.0292 0.5508 0.049 Uiso 1 1 calc R . . H15D H 0.3272 0.1192 0.5591 0.049 Uiso 1 1 calc R . . C1 C 0.7962(6) 0.4291(5) 0.6644(2) 0.0419(18) Uani 1 1 d DU . . H1A H 0.8076 0.4485 0.6425 0.050 Uiso 1 1 calc R . . H1B H 0.8385 0.3860 0.6700 0.050 Uiso 1 1 calc R . . C2 C 0.8021(6) 0.5037(5) 0.6878(2) 0.0415(18) Uani 1 1 d DU . . H2A H 0.7941 0.4835 0.7098 0.050 Uiso 1 1 calc R . . H2B H 0.8587 0.5297 0.6864 0.050 Uiso 1 1 calc R . . C3 C 0.7358(6) 0.6376(5) 0.7031(2) 0.0393(17) Uani 1 1 d DU . . H3A H 0.7904 0.6675 0.7024 0.047 Uiso 1 1 calc R . . H3B H 0.7272 0.6160 0.7249 0.047 Uiso 1 1 calc R . . C4 C 0.6635(5) 0.6980(5) 0.6942(2) 0.0392(17) Uani 1 1 d DU . . H4A H 0.6622 0.7454 0.7093 0.047 Uiso 1 1 calc R . . H4B H 0.6734 0.7209 0.6726 0.047 Uiso 1 1 calc R . . C5 C 0.5103(6) 0.7025(6) 0.68060(18) 0.0420(17) Uani 1 1 d DU . . H5A H 0.5194 0.7628 0.6848 0.050 Uiso 1 1 calc R . . H5B H 0.4562 0.6858 0.6904 0.050 Uiso 1 1 calc R . . C6 C 0.5068(6) 0.6870(5) 0.64454(18) 0.0381(16) Uani 1 1 d DU . . H6A H 0.4597 0.7195 0.6352 0.046 Uiso 1 1 calc R . . H6B H 0.5599 0.7062 0.6346 0.046 Uiso 1 1 calc R . . C7 C 0.5022(5) 0.5731(6) 0.60346(19) 0.0403(18) Uani 1 1 d DU . . H7A H 0.4694 0.6131 0.5904 0.048 Uiso 1 1 calc R . . H7B H 0.4784 0.5165 0.6001 0.048 Uiso 1 1 calc R . . C8 C 0.5935(5) 0.5742(6) 0.59290(19) 0.0371(18) Uani 1 1 d DU . . H8A H 0.5980 0.5526 0.5709 0.045 Uiso 1 1 calc R . . H8B H 0.6153 0.6323 0.5932 0.045 Uiso 1 1 calc R . . C9 C 0.3248(7) 0.3265(7) 0.5960(2) 0.064(2) Uani 1 1 d DU . . H9A H 0.3556 0.3377 0.5760 0.077 Uiso 1 1 calc R . . H9B H 0.2745 0.2930 0.5903 0.077 Uiso 1 1 calc R . . C10 C 0.2977(8) 0.3990(7) 0.6068(3) 0.080(2) Uani 1 1 d DU . . H10A H 0.2391 0.4060 0.5992 0.096 Uiso 1 1 calc R . . H10B H 0.3317 0.4430 0.5963 0.096 Uiso 1 1 calc R . . C11 C 0.2139(8) 0.4175(8) 0.6550(3) 0.077(2) Uani 1 1 d DU . . H11A H 0.1902 0.4744 0.6525 0.092 Uiso 1 1 calc R . . H11B H 0.1791 0.3795 0.6418 0.092 Uiso 1 1 calc R . . C12 C 0.2037(8) 0.3954(8) 0.6846(3) 0.079(2) Uani 1 1 d DU . . H12A H 0.1459 0.3724 0.6862 0.095 Uiso 1 1 calc R . . H12B H 0.2043 0.4477 0.6972 0.095 Uiso 1 1 calc R . . C13 C 0.2185(8) 0.2545(8) 0.7063(3) 0.081(2) Uani 1 1 d U . . H13A H 0.1865 0.2580 0.7264 0.097 Uiso 1 1 calc R . . H13B H 0.1768 0.2468 0.6890 0.097 Uiso 1 1 calc R . . C14 C 0.2668(7) 0.1829(7) 0.7076(3) 0.069(2) Uani 1 1 d U . . H14A H 0.2297 0.1335 0.7048 0.083 Uiso 1 1 calc R . . H14B H 0.2933 0.1789 0.7288 0.083 Uiso 1 1 calc R . . C15 C 0.4014(7) 0.1158(7) 0.6891(2) 0.060(2) Uani 1 1 d U . . H15A H 0.3753 0.0595 0.6895 0.072 Uiso 1 1 calc R . . H15B H 0.4268 0.1265 0.7102 0.072 Uiso 1 1 calc R . . C16 C 0.4693(7) 0.1184(6) 0.6639(3) 0.058(2) Uani 1 1 d U . . H16A H 0.5123 0.0750 0.6682 0.070 Uiso 1 1 calc R . . H16B H 0.4443 0.1072 0.6428 0.070 Uiso 1 1 calc R . . C17 C 0.4307(6) 0.3209(6) 0.4911(2) 0.0445(19) Uani 1 1 d U . . H17A H 0.3999 0.3164 0.4707 0.053 Uiso 1 1 calc R . . H17B H 0.4210 0.3776 0.4999 0.053 Uiso 1 1 calc R . . C18 C 0.5234(6) 0.3079(6) 0.4855(2) 0.0439(19) Uani 1 1 d U . . H18A H 0.5431 0.3467 0.4687 0.053 Uiso 1 1 calc R . . H18B H 0.5549 0.3207 0.5052 0.053 Uiso 1 1 calc R . . C19 C 0.5431(7) 0.2133(6) 0.4401(2) 0.0509(19) Uani 1 1 d U . . H19A H 0.4982 0.2493 0.4310 0.061 Uiso 1 1 calc R . . H19B H 0.5979 0.2349 0.4324 0.061 Uiso 1 1 calc R . . C20 C 0.5317(6) 0.1280(6) 0.4283(2) 0.0483(18) Uani 1 1 d U . . H20A H 0.5818 0.0940 0.4338 0.058 Uiso 1 1 calc R . . H20B H 0.5268 0.1291 0.4048 0.058 Uiso 1 1 calc R . . C21 C 0.3752(6) 0.1087(6) 0.4244(2) 0.0461(17) Uani 1 1 d U . . H21A H 0.3783 0.0861 0.4025 0.055 Uiso 1 1 calc R . . H21B H 0.3678 0.1702 0.4231 0.055 Uiso 1 1 calc R . . C22 C 0.3010(6) 0.0692(6) 0.4422(2) 0.0469(18) Uani 1 1 d U . . H22A H 0.2477 0.0822 0.4310 0.056 Uiso 1 1 calc R . . H22B H 0.3078 0.0076 0.4428 0.056 Uiso 1 1 calc R . . C23 C 0.2309(6) 0.0606(6) 0.4950(2) 0.0440(18) Uani 1 1 d U . . H23A H 0.2405 -0.0006 0.4949 0.053 Uiso 1 1 calc R . . H23B H 0.1748 0.0716 0.4856 0.053 Uiso 1 1 calc R . . C24 C 0.2334(6) 0.0936(6) 0.5295(2) 0.0470(19) Uani 1 1 d U . . H24A H 0.2179 0.1537 0.5298 0.056 Uiso 1 1 calc R . . H24B H 0.1923 0.0626 0.5426 0.056 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 0.0419(4) 0.0649(4) 0.0232(3) 0.0006(3) 0.0039(3) -0.0122(3) Sb2 0.0222(3) 0.0267(3) 0.0249(3) -0.0035(2) -0.0021(2) 0.0003(2) Y1 0.0257(4) 0.0273(4) 0.0217(4) 0.0011(3) 0.0014(3) -0.0009(4) Y2 0.0257(5) 0.0322(5) 0.0275(4) 0.0039(4) 0.0002(4) -0.0038(4) Y3 0.0223(4) 0.0212(4) 0.0223(4) -0.0017(3) -0.0026(3) 0.0018(3) S1 0.0331(14) 0.0449(14) 0.0315(12) -0.0031(10) 0.0029(10) -0.0005(11) S2 0.0398(15) 0.0738(19) 0.0321(12) 0.0185(12) -0.0067(11) -0.0152(14) S3 0.082(2) 0.0528(16) 0.0422(14) 0.0183(13) -0.0261(14) -0.0263(16) S4 0.0315(13) 0.0340(12) 0.0286(11) -0.0066(10) 0.0017(9) -0.0089(10) S5 0.0439(14) 0.0259(12) 0.0406(13) -0.0050(10) 0.0026(11) 0.0050(10) S6 0.0281(13) 0.0384(13) 0.0392(12) -0.0082(10) 0.0079(10) -0.0039(10) S7 0.0457(16) 0.0658(18) 0.0369(13) -0.0002(12) -0.0168(11) 0.0119(13) Cl1 0.0513(17) 0.0720(19) 0.0610(16) -0.0104(14) 0.0037(13) 0.0224(14) O2 0.029(3) 0.020(3) 0.026(3) -0.003(2) 0.001(2) 0.005(2) O1 0.033(3) 0.028(3) 0.031(3) 0.003(3) 0.004(3) -0.008(3) N1 0.041(4) 0.042(4) 0.036(3) -0.003(3) 0.000(3) 0.007(3) N2 0.033(3) 0.036(3) 0.027(3) 0.001(3) 0.007(3) -0.001(3) N3 0.037(3) 0.035(3) 0.026(3) -0.005(3) 0.004(3) -0.003(3) N4 0.036(3) 0.037(3) 0.029(3) -0.003(3) 0.004(3) 0.000(3) N5 0.035(3) 0.037(3) 0.029(3) -0.002(3) 0.002(3) 0.000(3) N6 0.044(3) 0.050(3) 0.042(3) 0.001(3) -0.003(3) 0.009(3) N7 0.052(4) 0.058(4) 0.043(3) -0.005(3) -0.003(3) 0.013(3) N8 0.054(4) 0.055(4) 0.053(3) 0.000(3) 0.011(3) 0.001(3) N9 0.050(4) 0.048(3) 0.051(3) 0.006(3) 0.005(3) -0.009(3) N10 0.048(4) 0.047(4) 0.060(4) 0.013(3) 0.004(3) 0.000(3) N11 0.039(3) 0.044(3) 0.041(3) -0.001(3) -0.001(3) 0.008(3) N12 0.036(3) 0.040(3) 0.036(3) 0.003(3) -0.003(3) 0.002(3) N13 0.038(3) 0.044(3) 0.029(3) -0.002(3) -0.005(3) 0.001(3) N14 0.034(3) 0.041(3) 0.041(3) -0.007(3) -0.007(3) 0.006(3) N15 0.032(4) 0.046(4) 0.044(3) -0.003(3) 0.000(3) 0.004(3) C1 0.036(4) 0.044(4) 0.045(4) 0.001(3) 0.005(3) 0.007(3) C2 0.034(4) 0.048(4) 0.043(4) -0.002(3) 0.004(3) 0.000(3) C3 0.040(4) 0.042(4) 0.035(3) -0.005(3) 0.005(3) -0.003(3) C4 0.046(4) 0.035(4) 0.037(3) -0.009(3) 0.006(3) -0.007(3) C5 0.048(4) 0.037(4) 0.041(3) -0.004(3) 0.004(3) 0.004(3) C6 0.043(4) 0.035(3) 0.036(3) 0.000(3) -0.003(3) 0.006(3) C7 0.042(4) 0.041(4) 0.037(3) 0.004(3) -0.004(3) 0.001(3) C8 0.047(4) 0.036(4) 0.028(4) 0.002(3) 0.005(3) -0.001(4) C9 0.067(4) 0.076(4) 0.050(4) -0.003(4) 0.000(4) 0.027(4) C10 0.093(5) 0.081(5) 0.065(4) -0.008(4) -0.025(4) 0.027(4) C11 0.070(4) 0.082(4) 0.078(4) 0.017(4) 0.002(4) 0.013(4) C12 0.070(4) 0.098(4) 0.070(4) -0.002(4) 0.006(4) 0.020(4) C13 0.073(4) 0.080(4) 0.089(4) 0.002(4) 0.019(4) -0.005(4) C14 0.069(4) 0.063(4) 0.075(4) 0.015(4) 0.011(4) -0.007(4) C15 0.064(4) 0.050(4) 0.067(4) 0.012(4) -0.004(4) -0.013(4) C16 0.055(4) 0.051(4) 0.069(4) 0.010(4) -0.002(4) 0.003(4) C17 0.044(4) 0.036(4) 0.054(4) 0.006(4) -0.007(4) 0.002(4) C18 0.042(4) 0.041(4) 0.048(4) 0.004(3) -0.002(3) -0.001(3) C19 0.052(4) 0.054(4) 0.047(4) -0.001(3) 0.004(3) -0.001(4) C20 0.050(4) 0.056(4) 0.039(3) -0.001(3) 0.002(3) -0.001(3) C21 0.047(4) 0.054(4) 0.037(3) -0.005(3) -0.010(3) 0.006(3) C22 0.040(4) 0.057(4) 0.044(3) -0.011(3) -0.018(3) 0.006(3) C23 0.031(4) 0.049(4) 0.052(4) -0.005(4) -0.012(3) 0.008(3) C24 0.034(4) 0.053(4) 0.054(4) 0.000(4) 0.000(3) 0.005(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 2.376(3) . ? Sb1 S3 2.378(3) . ? Sb1 S1 2.431(2) . ? Sb2 S7 2.301(2) . ? Sb2 S5 2.316(2) . ? Sb2 S6 2.325(2) . ? Sb2 S4 2.348(2) . ? Y1 O1 2.242(5) . ? Y1 N4 2.538(7) . ? Y1 N1 2.550(7) . ? Y1 N3 2.556(6) . ? Y1 N2 2.557(7) . ? Y1 N5 2.569(6) . ? Y1 S2 2.778(2) . ? Y1 S1 2.877(2) . ? Y1 Y2 3.9242(12) . ? Y2 O1 2.241(5) . ? Y2 N10 2.534(7) . ? Y2 N8 2.555(8) . ? Y2 N9 2.556(7) . ? Y2 N6 2.558(7) . ? Y2 N7 2.570(7) . ? Y2 S3 2.805(2) . ? Y2 S1 2.896(2) . ? Y3 O2 2.248(5) . ? Y3 O2 2.271(5) 5_656 ? Y3 N13 2.520(6) . ? Y3 N11 2.533(7) . ? Y3 N14 2.555(7) . ? Y3 N15 2.563(7) . ? Y3 N12 2.604(7) . ? Y3 S4 2.906(2) . ? Y3 Y3 3.6761(16) 5_656 ? O2 Y3 2.271(5) 5_656 ? N1 C1 1.470(11) . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 C3 1.454(10) . ? N2 C2 1.464(10) . ? N2 H2C 0.9100 . ? N3 C5 1.466(10) . ? N3 C4 1.470(10) . ? N3 H3C 0.9100 . ? N4 C6 1.454(10) . ? N4 C7 1.473(10) . ? N4 H4C 0.9100 . ? N5 C8 1.478(10) . ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N6 C9 1.418(11) . ? N6 H6C 0.9000 . ? N6 H6D 0.9000 . ? N7 C11 1.411(13) . ? N7 C10 1.468(12) . ? N7 H7C 0.9100 . ? N8 C13 1.440(13) . ? N8 C12 1.442(12) . ? N8 H8C 0.9100 . ? N9 C15 1.473(12) . ? N9 C14 1.484(12) . ? N9 H9C 0.9100 . ? N10 C16 1.467(11) . ? N10 H10C 0.9000 . ? N10 H10D 0.9000 . ? N11 C17 1.481(10) . ? N11 H11C 0.9000 . ? N11 H11D 0.9000 . ? N12 C18 1.451(10) . ? N12 C19 1.479(10) . ? N12 H12C 0.9100 . ? N13 C20 1.467(11) . ? N13 C21 1.467(10) . ? N13 H13C 0.9100 . ? N14 C23 1.463(11) . ? N14 C22 1.479(10) . ? N14 H14C 0.9100 . ? N15 C24 1.466(10) . ? N15 H15C 0.9000 . ? N15 H15D 0.9000 . ? C1 C2 1.520(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.514(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.508(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.485(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.290(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.279(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.349(14) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.482(13) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.474(12) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.431(12) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.502(12) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.514(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 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 S3 101.93(11) . . ? S2 Sb1 S1 96.33(8) . . ? S3 Sb1 S1 95.98(8) . . ? S7 Sb2 S5 108.49(9) . . ? S7 Sb2 S6 110.87(9) . . ? S5 Sb2 S6 113.24(8) . . ? S7 Sb2 S4 111.67(9) . . ? S5 Sb2 S4 104.10(8) . . ? S6 Sb2 S4 108.31(8) . . ? O1 Y1 N4 85.7(2) . . ? O1 Y1 N1 79.4(2) . . ? N4 Y1 N1 139.0(2) . . ? O1 Y1 N3 147.3(2) . . ? N4 Y1 N3 68.0(2) . . ? N1 Y1 N3 133.3(2) . . ? O1 Y1 N2 143.4(2) . . ? N4 Y1 N2 109.7(2) . . ? N1 Y1 N2 67.2(2) . . ? N3 Y1 N2 67.2(2) . . ? O1 Y1 N5 81.9(2) . . ? N4 Y1 N5 66.3(2) . . ? N1 Y1 N5 73.9(2) . . ? N3 Y1 N5 103.4(2) . . ? N2 Y1 N5 75.1(2) . . ? O1 Y1 S2 109.50(14) . . ? N4 Y1 S2 145.77(16) . . ? N1 Y1 S2 75.02(16) . . ? N3 Y1 S2 85.28(16) . . ? N2 Y1 S2 76.55(15) . . ? N5 Y1 S2 144.06(16) . . ? O1 Y1 S1 73.85(14) . . ? N4 Y1 S1 76.60(16) . . ? N1 Y1 S1 133.06(17) . . ? N3 Y1 S1 81.21(16) . . ? N2 Y1 S1 140.94(15) . . ? N5 Y1 S1 136.83(16) . . ? S2 Y1 S1 78.59(7) . . ? O1 Y1 Y2 28.91(13) . . ? N4 Y1 Y2 90.23(16) . . ? N1 Y1 Y2 94.37(17) . . ? N3 Y1 Y2 128.11(15) . . ? N2 Y1 Y2 159.31(15) . . ? N5 Y1 Y2 109.79(16) . . ? S2 Y1 Y2 90.06(6) . . ? S1 Y1 Y2 47.39(5) . . ? O1 Y2 N10 77.9(2) . . ? O1 Y2 N8 149.2(2) . . ? N10 Y2 N8 132.7(2) . . ? O1 Y2 N9 143.5(2) . . ? N10 Y2 N9 67.6(3) . . ? N8 Y2 N9 66.8(3) . . ? O1 Y2 N6 82.1(2) . . ? N10 Y2 N6 74.1(2) . . ? N8 Y2 N6 107.0(3) . . ? N9 Y2 N6 77.4(2) . . ? O1 Y2 N7 91.4(2) . . ? N10 Y2 N7 140.0(2) . . ? N8 Y2 N7 67.3(3) . . ? N9 Y2 N7 107.1(3) . . ? N6 Y2 N7 66.2(2) . . ? O1 Y2 S3 103.75(15) . . ? N10 Y2 S3 74.57(19) . . ? N8 Y2 S3 85.1(2) . . ? N9 Y2 S3 78.88(19) . . ? N6 Y2 S3 146.05(17) . . ? N7 Y2 S3 145.15(18) . . ? O1 Y2 S1 73.47(14) . . ? N10 Y2 S1 133.53(19) . . ? N8 Y2 S1 80.01(19) . . ? N9 Y2 S1 140.53(18) . . ? N6 Y2 S1 134.93(17) . . ? N7 Y2 S1 76.99(18) . . ? S3 Y2 S1 77.62(7) . . ? O1 Y2 Y1 28.93(13) . . ? N10 Y2 Y1 93.91(18) . . ? N8 Y2 Y1 126.95(18) . . ? N9 Y2 Y1 158.11(19) . . ? N6 Y2 Y1 109.70(18) . . ? N7 Y2 Y1 94.55(19) . . ? S3 Y2 Y1 85.14(6) . . ? S1 Y2 Y1 46.97(5) . . ? O2 Y3 O2 71.1(2) . 5_656 ? O2 Y3 N13 84.4(2) . . ? O2 Y3 N13 79.4(2) 5_656 . ? O2 Y3 N11 153.2(2) . . ? O2 Y3 N11 134.1(2) 5_656 . ? N13 Y3 N11 106.8(2) . . ? O2 Y3 N14 82.3(2) . . ? O2 Y3 N14 139.17(19) 5_656 . ? N13 Y3 N14 67.4(2) . . ? N11 Y3 N14 80.0(2) . . ? O2 Y3 N15 76.9(2) . . ? O2 Y3 N15 132.2(2) 5_656 . ? N13 Y3 N15 131.9(2) . . ? N11 Y3 N15 77.7(2) . . ? N14 Y3 N15 66.4(2) . . ? O2 Y3 N12 140.2(2) . . ? O2 Y3 N12 76.7(2) 5_656 . ? N13 Y3 N12 66.9(2) . . ? N11 Y3 N12 65.5(2) . . ? N14 Y3 N12 109.2(2) . . ? N15 Y3 N12 142.9(2) . . ? O2 Y3 S4 98.94(13) . . ? O2 Y3 S4 80.75(13) 5_656 . ? N13 Y3 S4 157.56(17) . . ? N11 Y3 S4 80.08(16) . . ? N14 Y3 S4 134.95(16) . . ? N15 Y3 S4 70.06(16) . . ? N12 Y3 S4 98.37(15) . . ? O2 Y3 Y3 35.76(13) . 5_656 ? O2 Y3 Y3 35.35(12) 5_656 5_656 ? N13 Y3 Y3 79.99(16) . 5_656 ? N11 Y3 Y3 167.35(17) . 5_656 ? N14 Y3 Y3 112.66(16) . 5_656 ? N15 Y3 Y3 106.04(16) . 5_656 ? N12 Y3 Y3 109.11(16) . 5_656 ? S4 Y3 Y3 89.76(5) . 5_656 ? Sb1 S1 Y1 89.80(7) . . ? Sb1 S1 Y2 91.21(8) . . ? Y1 S1 Y2 85.64(6) . . ? Sb1 S2 Y1 93.37(8) . . ? Sb1 S3 Y2 94.63(9) . . ? Sb2 S4 Y3 110.90(8) . . ? Y3 O2 Y3 108.9(2) . 5_656 ? Y2 O1 Y1 122.2(2) . . ? C1 N1 Y1 115.6(5) . . ? C1 N1 H1C 108.4 . . ? Y1 N1 H1C 108.4 . . ? C1 N1 H1D 108.4 . . ? Y1 N1 H1D 108.4 . . ? H1C N1 H1D 107.5 . . ? C3 N2 C2 112.0(6) . . ? C3 N2 Y1 112.5(5) . . ? C2 N2 Y1 112.4(5) . . ? C3 N2 H2C 106.5 . . ? C2 N2 H2C 106.5 . . ? Y1 N2 H2C 106.5 . . ? C5 N3 C4 112.9(7) . . ? C5 N3 Y1 112.5(5) . . ? C4 N3 Y1 114.0(5) . . ? C5 N3 H3C 105.5 . . ? C4 N3 H3C 105.5 . . ? Y1 N3 H3C 105.5 . . ? C6 N4 C7 114.3(6) . . ? C6 N4 Y1 113.3(5) . . ? C7 N4 Y1 110.7(5) . . ? C6 N4 H4C 105.9 . . ? C7 N4 H4C 105.9 . . ? Y1 N4 H4C 105.9 . . ? C8 N5 Y1 117.0(5) . . ? C8 N5 H5C 108.0 . . ? Y1 N5 H5C 108.0 . . ? C8 N5 H5D 108.0 . . ? Y1 N5 H5D 108.0 . . ? H5C N5 H5D 107.3 . . ? C9 N6 Y2 116.1(6) . . ? C9 N6 H6C 108.3 . . ? Y2 N6 H6C 108.3 . . ? C9 N6 H6D 108.3 . . ? Y2 N6 H6D 108.3 . . ? H6C N6 H6D 107.4 . . ? C11 N7 C10 112.5(9) . . ? C11 N7 Y2 113.5(6) . . ? C10 N7 Y2 112.4(6) . . ? C11 N7 H7C 105.9 . . ? C10 N7 H7C 105.9 . . ? Y2 N7 H7C 105.9 . . ? C13 N8 C12 112.1(9) . . ? C13 N8 Y2 113.7(6) . . ? C12 N8 Y2 110.9(6) . . ? C13 N8 H8C 106.5 . . ? C12 N8 H8C 106.5 . . ? Y2 N8 H8C 106.5 . . ? C15 N9 C14 112.7(8) . . ? C15 N9 Y2 109.9(6) . . ? C14 N9 Y2 112.9(6) . . ? C15 N9 H9C 107.0 . . ? C14 N9 H9C 107.0 . . ? Y2 N9 H9C 107.0 . . ? C16 N10 Y2 114.9(6) . . ? C16 N10 H10C 108.6 . . ? Y2 N10 H10C 108.6 . . ? C16 N10 H10D 108.6 . . ? Y2 N10 H10D 108.6 . . ? H10C N10 H10D 107.5 . . ? C17 N11 Y3 115.4(5) . . ? C17 N11 H11C 108.4 . . ? Y3 N11 H11C 108.4 . . ? C17 N11 H11D 108.4 . . ? Y3 N11 H11D 108.4 . . ? H11C N11 H11D 107.5 . . ? C18 N12 C19 110.6(7) . . ? C18 N12 Y3 115.9(5) . . ? C19 N12 Y3 112.8(5) . . ? C18 N12 H12C 105.5 . . ? C19 N12 H12C 105.5 . . ? Y3 N12 H12C 105.5 . . ? C20 N13 C21 113.7(7) . . ? C20 N13 Y3 113.3(5) . . ? C21 N13 Y3 115.2(5) . . ? C20 N13 H13C 104.4 . . ? C21 N13 H13C 104.4 . . ? Y3 N13 H13C 104.4 . . ? C23 N14 C22 111.9(7) . . ? C23 N14 Y3 113.4(5) . . ? C22 N14 Y3 112.1(5) . . ? C23 N14 H14C 106.2 . . ? C22 N14 H14C 106.2 . . ? Y3 N14 H14C 106.2 . . ? C24 N15 Y3 116.4(5) . . ? C24 N15 H15C 108.2 . . ? Y3 N15 H15C 108.2 . . ? C24 N15 H15D 108.2 . . ? Y3 N15 H15D 108.2 . . ? H15C N15 H15D 107.3 . . ? N1 C1 C2 108.7(7) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C1 109.9(7) . . ? 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 . . ? N2 C3 C4 108.5(7) . . ? N2 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? N2 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? N3 C4 C3 110.1(7) . . ? N3 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N3 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.2 . . ? N3 C5 C6 109.9(7) . . ? N3 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? N3 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? N4 C6 C5 110.3(7) . . ? N4 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? N4 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? N4 C7 C8 111.1(7) . . ? N4 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? N4 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N5 C8 C7 109.2(7) . . ? N5 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? N5 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.3 . . ? C10 C9 N6 120.4(10) . . ? C10 C9 H9A 107.2 . . ? N6 C9 H9A 107.2 . . ? C10 C9 H9B 107.2 . . ? N6 C9 H9B 107.2 . . ? H9A C9 H9B 106.9 . . ? C9 C10 N7 121.3(10) . . ? C9 C10 H10A 107.0 . . ? N7 C10 H10A 107.0 . . ? C9 C10 H10B 107.0 . . ? N7 C10 H10B 107.0 . . ? H10A C10 H10B 106.7 . . ? C12 C11 N7 119.3(11) . . ? C12 C11 H11A 107.5 . . ? N7 C11 H11A 107.5 . . ? C12 C11 H11B 107.5 . . ? N7 C11 H11B 107.5 . . ? H11A C11 H11B 107.0 . . ? C11 C12 N8 123.7(11) . . ? C11 C12 H12A 106.4 . . ? N8 C12 H12A 106.4 . . ? C11 C12 H12B 106.4 . . ? N8 C12 H12B 106.4 . . ? H12A C12 H12B 106.5 . . ? C14 C13 N8 119.9(10) . . ? C14 C13 H13A 107.4 . . ? N8 C13 H13A 107.4 . . ? C14 C13 H13B 107.4 . . ? N8 C13 H13B 107.4 . . ? H13A C13 H13B 106.9 . . ? C13 C14 N9 112.9(9) . . ? C13 C14 H14A 109.0 . . ? N9 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? N9 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? N9 C15 C16 110.3(8) . . ? N9 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? N9 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? N10 C16 C15 108.6(8) . . ? N10 C16 H16A 110.0 . . ? C15 C16 H16A 110.0 . . ? N10 C16 H16B 110.0 . . ? C15 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? C18 C17 N11 109.9(7) . . ? C18 C17 H17A 109.7 . . ? N11 C17 H17A 109.7 . . ? C18 C17 H17B 109.7 . . ? N11 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? N12 C18 C17 110.7(8) . . ? N12 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? N12 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C20 C19 N12 114.0(8) . . ? C20 C19 H19A 108.8 . . ? N12 C19 H19A 108.8 . . ? C20 C19 H19B 108.8 . . ? N12 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? C19 C20 N13 111.2(8) . . ? C19 C20 H20A 109.4 . . ? N13 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? N13 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N13 C21 C22 108.2(7) . . ? N13 C21 H21A 110.1 . . ? C22 C21 H21A 110.1 . . ? N13 C21 H21B 110.1 . . ? C22 C21 H21B 110.1 . . ? H21A C21 H21B 108.4 . . ? N14 C22 C21 109.8(7) . . ? N14 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? N14 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? N14 C23 C24 109.8(7) . . ? N14 C23 H23A 109.7 . . ? C24 C23 H23A 109.7 . . ? N14 C23 H23B 109.7 . . ? C24 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? N15 C24 C23 109.2(7) . . ? N15 C24 H24A 109.8 . . ? C23 C24 H24A 109.8 . . ? N15 C24 H24B 109.8 . . ? C23 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? 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 N4 Y1 Y2 O1 80.7(3) . . . . ? N1 Y1 Y2 O1 -58.5(3) . . . . ? N3 Y1 Y2 O1 142.4(3) . . . . ? N2 Y1 Y2 O1 -84.5(5) . . . . ? N5 Y1 Y2 O1 15.9(3) . . . . ? S2 Y1 Y2 O1 -133.5(3) . . . . ? S1 Y1 Y2 O1 152.1(3) . . . . ? O1 Y1 Y2 N10 56.2(3) . . . . ? N4 Y1 Y2 N10 136.9(2) . . . . ? N1 Y1 Y2 N10 -2.4(2) . . . . ? N3 Y1 Y2 N10 -161.4(3) . . . . ? N2 Y1 Y2 N10 -28.3(4) . . . . ? N5 Y1 Y2 N10 72.1(2) . . . . ? S2 Y1 Y2 N10 -77.36(19) . . . . ? S1 Y1 Y2 N10 -151.71(19) . . . . ? O1 Y1 Y2 N8 -149.5(4) . . . . ? N4 Y1 Y2 N8 -68.8(3) . . . . ? N1 Y1 Y2 N8 151.9(3) . . . . ? N3 Y1 Y2 N8 -7.1(3) . . . . ? N2 Y1 Y2 N8 126.0(5) . . . . ? N5 Y1 Y2 N8 -133.6(3) . . . . ? S2 Y1 Y2 N8 77.0(2) . . . . ? S1 Y1 Y2 N8 2.6(2) . . . . ? O1 Y1 Y2 N9 87.3(5) . . . . ? N4 Y1 Y2 N9 168.0(5) . . . . ? N1 Y1 Y2 N9 28.7(5) . . . . ? N3 Y1 Y2 N9 -130.3(5) . . . . ? N2 Y1 Y2 N9 2.8(6) . . . . ? N5 Y1 Y2 N9 103.1(5) . . . . ? S2 Y1 Y2 N9 -46.3(5) . . . . ? S1 Y1 Y2 N9 -120.6(5) . . . . ? O1 Y1 Y2 N6 -18.3(3) . . . . ? N4 Y1 Y2 N6 62.4(2) . . . . ? N1 Y1 Y2 N6 -76.9(2) . . . . ? N3 Y1 Y2 N6 124.1(3) . . . . ? N2 Y1 Y2 N6 -102.8(4) . . . . ? N5 Y1 Y2 N6 -2.5(2) . . . . ? S2 Y1 Y2 N6 -151.86(18) . . . . ? S1 Y1 Y2 N6 133.79(18) . . . . ? O1 Y1 Y2 N7 -84.7(3) . . . . ? N4 Y1 Y2 N7 -4.0(2) . . . . ? N1 Y1 Y2 N7 -143.2(2) . . . . ? N3 Y1 Y2 N7 57.8(2) . . . . ? N2 Y1 Y2 N7 -169.1(4) . . . . ? N5 Y1 Y2 N7 -68.8(2) . . . . ? S2 Y1 Y2 N7 141.81(17) . . . . ? S1 Y1 Y2 N7 67.46(17) . . . . ? O1 Y1 Y2 S3 130.3(3) . . . . ? N4 Y1 Y2 S3 -149.00(16) . . . . ? N1 Y1 Y2 S3 71.75(17) . . . . ? N3 Y1 Y2 S3 -87.3(2) . . . . ? N2 Y1 Y2 S3 45.8(4) . . . . ? N5 Y1 Y2 S3 146.18(17) . . . . ? S2 Y1 Y2 S3 -3.23(9) . . . . ? S1 Y1 Y2 S3 -77.58(9) . . . . ? O1 Y1 Y2 S1 -152.1(3) . . . . ? N4 Y1 Y2 S1 -71.42(15) . . . . ? N1 Y1 Y2 S1 149.33(17) . . . . ? N3 Y1 Y2 S1 -9.69(19) . . . . ? N2 Y1 Y2 S1 123.4(4) . . . . ? N5 Y1 Y2 S1 -136.24(17) . . . . ? S2 Y1 Y2 S1 74.35(8) . . . . ? S2 Sb1 S1 Y1 11.04(9) . . . . ? S3 Sb1 S1 Y1 -91.72(9) . . . . ? S2 Sb1 S1 Y2 96.68(8) . . . . ? S3 Sb1 S1 Y2 -6.08(9) . . . . ? O1 Y1 S1 Sb1 104.84(15) . . . . ? N4 Y1 S1 Sb1 -165.78(16) . . . . ? N1 Y1 S1 Sb1 47.1(2) . . . . ? N3 Y1 S1 Sb1 -96.48(16) . . . . ? N2 Y1 S1 Sb1 -60.9(3) . . . . ? N5 Y1 S1 Sb1 163.3(2) . . . . ? S2 Y1 S1 Sb1 -9.56(8) . . . . ? Y2 Y1 S1 Sb1 91.23(7) . . . . ? O1 Y1 S1 Y2 13.61(14) . . . . ? N4 Y1 S1 Y2 102.99(15) . . . . ? N1 Y1 S1 Y2 -44.1(2) . . . . ? N3 Y1 S1 Y2 172.30(16) . . . . ? N2 Y1 S1 Y2 -152.1(2) . . . . ? N5 Y1 S1 Y2 72.0(2) . . . . ? S2 Y1 S1 Y2 -100.78(8) . . . . ? O1 Y2 S1 Sb1 -103.36(15) . . . . ? N10 Y2 S1 Sb1 -49.0(3) . . . . ? N8 Y2 S1 Sb1 92.41(19) . . . . ? N9 Y2 S1 Sb1 60.0(3) . . . . ? N6 Y2 S1 Sb1 -163.5(2) . . . . ? N7 Y2 S1 Sb1 161.19(19) . . . . ? S3 Y2 S1 Sb1 5.25(8) . . . . ? Y1 Y2 S1 Sb1 -89.71(7) . . . . ? O1 Y2 S1 Y1 -13.65(14) . . . . ? N10 Y2 S1 Y1 40.7(2) . . . . ? N8 Y2 S1 Y1 -177.87(19) . . . . ? N9 Y2 S1 Y1 149.7(3) . . . . ? N6 Y2 S1 Y1 -73.7(3) . . . . ? N7 Y2 S1 Y1 -109.10(19) . . . . ? S3 Y2 S1 Y1 94.96(8) . . . . ? S3 Sb1 S2 Y1 86.04(9) . . . . ? S1 Sb1 S2 Y1 -11.46(9) . . . . ? O1 Y1 S2 Sb1 -58.33(17) . . . . ? N4 Y1 S2 Sb1 54.0(3) . . . . ? N1 Y1 S2 Sb1 -131.01(19) . . . . ? N3 Y1 S2 Sb1 91.76(17) . . . . ? N2 Y1 S2 Sb1 159.43(17) . . . . ? N5 Y1 S2 Sb1 -161.8(3) . . . . ? S1 Y1 S2 Sb1 9.80(8) . . . . ? Y2 Y1 S2 Sb1 -36.50(8) . . . . ? S2 Sb1 S3 Y2 -91.49(9) . . . . ? S1 Sb1 S3 Y2 6.30(10) . . . . ? O1 Y2 S3 Sb1 63.91(17) . . . . ? N10 Y2 S3 Sb1 137.0(2) . . . . ? N8 Y2 S3 Sb1 -86.2(2) . . . . ? N9 Y2 S3 Sb1 -153.4(2) . . . . ? N6 Y2 S3 Sb1 160.2(3) . . . . ? N7 Y2 S3 Sb1 -49.4(4) . . . . ? S1 Y2 S3 Sb1 -5.38(8) . . . . ? Y1 Y2 S3 Sb1 41.58(8) . . . . ? S7 Sb2 S4 Y3 -159.78(9) . . . . ? S5 Sb2 S4 Y3 83.36(9) . . . . ? S6 Sb2 S4 Y3 -37.41(10) . . . . ? O2 Y3 S4 Sb2 135.49(15) . . . . ? O2 Y3 S4 Sb2 66.44(14) 5_656 . . . ? N13 Y3 S4 Sb2 38.5(5) . . . . ? N11 Y3 S4 Sb2 -71.65(18) . . . . ? N14 Y3 S4 Sb2 -136.5(2) . . . . ? N15 Y3 S4 Sb2 -152.02(19) . . . . ? N12 Y3 S4 Sb2 -8.50(18) . . . . ? Y3 Y3 S4 Sb2 100.79(8) 5_656 . . . ? O2 Y3 O2 Y3 0.000(2) 5_656 . . 5_656 ? N13 Y3 O2 Y3 80.7(2) . . . 5_656 ? N11 Y3 O2 Y3 -162.6(4) . . . 5_656 ? N14 Y3 O2 Y3 148.6(2) . . . 5_656 ? N15 Y3 O2 Y3 -143.9(2) . . . 5_656 ? N12 Y3 O2 Y3 37.8(4) . . . 5_656 ? S4 Y3 O2 Y3 -76.95(17) . . . 5_656 ? N10 Y2 O1 Y1 -122.1(3) . . . . ? N8 Y2 O1 Y1 52.4(6) . . . . ? N9 Y2 O1 Y1 -141.3(3) . . . . ? N6 Y2 O1 Y1 162.6(3) . . . . ? N7 Y2 O1 Y1 96.9(3) . . . . ? S3 Y2 O1 Y1 -51.5(3) . . . . ? S1 Y2 O1 Y1 20.9(2) . . . . ? N4 Y1 O1 Y2 -98.3(3) . . . . ? N1 Y1 O1 Y2 120.1(3) . . . . ? N3 Y1 O1 Y2 -62.7(5) . . . . ? N2 Y1 O1 Y2 143.9(3) . . . . ? N5 Y1 O1 Y2 -164.9(3) . . . . ? S2 Y1 O1 Y2 50.3(3) . . . . ? S1 Y1 O1 Y2 -21.0(2) . . . . ? O1 Y1 N1 C1 154.4(6) . . . . ? N4 Y1 N1 C1 83.8(6) . . . . ? N3 Y1 N1 C1 -23.5(7) . . . . ? N2 Y1 N1 C1 -10.4(5) . . . . ? N5 Y1 N1 C1 69.9(5) . . . . ? S2 Y1 N1 C1 -91.9(5) . . . . ? S1 Y1 N1 C1 -149.8(5) . . . . ? Y2 Y1 N1 C1 179.2(5) . . . . ? O1 Y1 N2 C3 -173.5(4) . . . . ? N4 Y1 N2 C3 76.0(5) . . . . ? N1 Y1 N2 C3 -148.0(5) . . . . ? N3 Y1 N2 C3 21.7(5) . . . . ? N5 Y1 N2 C3 133.6(5) . . . . ? S2 Y1 N2 C3 -68.8(5) . . . . ? S1 Y1 N2 C3 -16.9(6) . . . . ? Y2 Y1 N2 C3 -119.7(5) . . . . ? O1 Y1 N2 C2 -46.0(6) . . . . ? N4 Y1 N2 C2 -156.5(5) . . . . ? N1 Y1 N2 C2 -20.5(5) . . . . ? N3 Y1 N2 C2 149.2(5) . . . . ? N5 Y1 N2 C2 -99.0(5) . . . . ? S2 Y1 N2 C2 58.7(5) . . . . ? S1 Y1 N2 C2 110.6(5) . . . . ? Y2 Y1 N2 C2 7.7(8) . . . . ? O1 Y1 N3 C5 -23.2(7) . . . . ? N4 Y1 N3 C5 15.5(5) . . . . ? N1 Y1 N3 C5 153.0(5) . . . . ? N2 Y1 N3 C5 139.9(6) . . . . ? N5 Y1 N3 C5 72.7(5) . . . . ? S2 Y1 N3 C5 -142.7(5) . . . . ? S1 Y1 N3 C5 -63.5(5) . . . . ? Y2 Y1 N3 C5 -56.3(6) . . . . ? O1 Y1 N3 C4 -153.4(5) . . . . ? N4 Y1 N3 C4 -114.7(5) . . . . ? N1 Y1 N3 C4 22.9(6) . . . . ? N2 Y1 N3 C4 9.8(5) . . . . ? N5 Y1 N3 C4 -57.5(5) . . . . ? S2 Y1 N3 C4 87.1(5) . . . . ? S1 Y1 N3 C4 166.3(5) . . . . ? Y2 Y1 N3 C4 173.5(4) . . . . ? O1 Y1 N4 C6 175.4(5) . . . . ? N1 Y1 N4 C6 -116.3(5) . . . . ? N3 Y1 N4 C6 15.2(5) . . . . ? N2 Y1 N4 C6 -38.7(6) . . . . ? N5 Y1 N4 C6 -101.6(6) . . . . ? S2 Y1 N4 C6 56.3(7) . . . . ? S1 Y1 N4 C6 101.0(5) . . . . ? Y2 Y1 N4 C6 146.8(5) . . . . ? O1 Y1 N4 C7 -54.7(5) . . . . ? N1 Y1 N4 C7 13.7(7) . . . . ? N3 Y1 N4 C7 145.1(6) . . . . ? N2 Y1 N4 C7 91.2(5) . . . . ? N5 Y1 N4 C7 28.3(5) . . . . ? S2 Y1 N4 C7 -173.7(4) . . . . ? S1 Y1 N4 C7 -129.1(5) . . . . ? Y2 Y1 N4 C7 -83.2(5) . . . . ? O1 Y1 N5 C8 87.9(6) . . . . ? N4 Y1 N5 C8 -1.0(5) . . . . ? N1 Y1 N5 C8 169.1(6) . . . . ? N3 Y1 N5 C8 -59.3(6) . . . . ? N2 Y1 N5 C8 -120.9(6) . . . . ? S2 Y1 N5 C8 -159.9(4) . . . . ? S1 Y1 N5 C8 32.1(7) . . . . ? Y2 Y1 N5 C8 80.2(5) . . . . ? O1 Y2 N6 C9 -90.0(7) . . . . ? N10 Y2 N6 C9 -169.6(8) . . . . ? N8 Y2 N6 C9 59.9(8) . . . . ? N9 Y2 N6 C9 120.5(8) . . . . ? N7 Y2 N6 C9 5.1(7) . . . . ? S3 Y2 N6 C9 167.1(6) . . . . ? S1 Y2 N6 C9 -32.9(8) . . . . ? Y1 Y2 N6 C9 -81.1(7) . . . . ? O1 Y2 N7 C11 -163.2(7) . . . . ? N10 Y2 N7 C11 124.0(7) . . . . ? N8 Y2 N7 C11 -6.0(7) . . . . ? N9 Y2 N7 C11 48.8(8) . . . . ? N6 Y2 N7 C11 116.1(8) . . . . ? S3 Y2 N7 C11 -46.3(9) . . . . ? S1 Y2 N7 C11 -90.5(7) . . . . ? Y1 Y2 N7 C11 -134.4(7) . . . . ? O1 Y2 N7 C10 67.8(7) . . . . ? N10 Y2 N7 C10 -5.0(9) . . . . ? N8 Y2 N7 C10 -135.0(8) . . . . ? N9 Y2 N7 C10 -80.2(8) . . . . ? N6 Y2 N7 C10 -12.9(7) . . . . ? S3 Y2 N7 C10 -175.3(6) . . . . ? S1 Y2 N7 C10 140.5(8) . . . . ? Y1 Y2 N7 C10 96.6(7) . . . . ? O1 Y2 N8 C13 170.7(7) . . . . ? N10 Y2 N8 C13 -16.7(9) . . . . ? N9 Y2 N8 C13 -0.5(7) . . . . ? N6 Y2 N8 C13 67.2(8) . . . . ? N7 Y2 N8 C13 121.3(8) . . . . ? S3 Y2 N8 C13 -80.5(8) . . . . ? S1 Y2 N8 C13 -158.7(8) . . . . ? Y1 Y2 N8 C13 -160.7(7) . . . . ? O1 Y2 N8 C12 43.2(9) . . . . ? N10 Y2 N8 C12 -144.1(7) . . . . ? N9 Y2 N8 C12 -127.9(8) . . . . ? N6 Y2 N8 C12 -60.3(7) . . . . ? N7 Y2 N8 C12 -6.1(7) . . . . ? S3 Y2 N8 C12 152.1(7) . . . . ? S1 Y2 N8 C12 73.8(7) . . . . ? Y1 Y2 N8 C12 71.9(7) . . . . ? O1 Y2 N9 C15 41.8(8) . . . . ? N10 Y2 N9 C15 21.4(6) . . . . ? N8 Y2 N9 C15 -145.8(7) . . . . ? N6 Y2 N9 C15 99.2(6) . . . . ? N7 Y2 N9 C15 159.1(6) . . . . ? S3 Y2 N9 C15 -56.4(6) . . . . ? S1 Y2 N9 C15 -110.7(6) . . . . ? Y1 Y2 N9 C15 -12.5(9) . . . . ? O1 Y2 N9 C14 168.5(6) . . . . ? N10 Y2 N9 C14 148.1(7) . . . . ? N8 Y2 N9 C14 -19.1(6) . . . . ? N6 Y2 N9 C14 -134.1(7) . . . . ? N7 Y2 N9 C14 -74.2(7) . . . . ? S3 Y2 N9 C14 70.3(6) . . . . ? S1 Y2 N9 C14 16.0(8) . . . . ? Y1 Y2 N9 C14 114.2(7) . . . . ? O1 Y2 N10 C16 -158.2(7) . . . . ? N8 Y2 N10 C16 25.6(8) . . . . ? N9 Y2 N10 C16 9.5(6) . . . . ? N6 Y2 N10 C16 -73.1(6) . . . . ? N7 Y2 N10 C16 -80.6(7) . . . . ? S3 Y2 N10 C16 93.7(6) . . . . ? S1 Y2 N10 C16 149.0(6) . . . . ? Y1 Y2 N10 C16 177.5(6) . . . . ? O2 Y3 N11 C17 -146.0(5) . . . . ? O2 Y3 N11 C17 57.2(7) 5_656 . . . ? N13 Y3 N11 C17 -34.2(6) . . . . ? N14 Y3 N11 C17 -96.8(6) . . . . ? N15 Y3 N11 C17 -164.6(6) . . . . ? N12 Y3 N11 C17 19.8(5) . . . . ? S4 Y3 N11 C17 123.8(6) . . . . ? Y3 Y3 N11 C17 86.8(9) 5_656 . . . ? O2 Y3 N12 C18 178.7(5) . . . . ? O2 Y3 N12 C18 -144.7(6) 5_656 . . . ? N13 Y3 N12 C18 131.4(6) . . . . ? N11 Y3 N12 C18 8.7(5) . . . . ? N14 Y3 N12 C18 77.5(6) . . . . ? N15 Y3 N12 C18 1.5(8) . . . . ? S4 Y3 N12 C18 -66.3(6) . . . . ? Y3 Y3 N12 C18 -159.0(5) 5_656 . . . ? O2 Y3 N12 C19 49.8(7) . . . . ? O2 Y3 N12 C19 86.3(6) 5_656 . . . ? N13 Y3 N12 C19 2.4(6) . . . . ? N11 Y3 N12 C19 -120.3(6) . . . . ? N14 Y3 N12 C19 -51.5(6) . . . . ? N15 Y3 N12 C19 -127.4(6) . . . . ? S4 Y3 N12 C19 164.7(6) . . . . ? Y3 Y3 N12 C19 72.0(6) 5_656 . . . ? O2 Y3 N13 C20 -128.2(6) . . . . ? O2 Y3 N13 C20 -56.4(6) 5_656 . . . ? N11 Y3 N13 C20 76.7(6) . . . . ? N14 Y3 N13 C20 147.9(6) . . . . ? N15 Y3 N13 C20 165.0(5) . . . . ? N12 Y3 N13 C20 23.6(6) . . . . ? S4 Y3 N13 C20 -28.4(9) . . . . ? Y3 Y3 N13 C20 -92.3(6) 5_656 . . . ? O2 Y3 N13 C21 98.5(6) . . . . ? O2 Y3 N13 C21 170.3(6) 5_656 . . . ? N11 Y3 N13 C21 -56.6(6) . . . . ? N14 Y3 N13 C21 14.6(6) . . . . ? N15 Y3 N13 C21 31.8(7) . . . . ? N12 Y3 N13 C21 -109.7(6) . . . . ? S4 Y3 N13 C21 -161.6(5) . . . . ? Y3 Y3 N13 C21 134.4(6) 5_656 . . . ? O2 Y3 N14 C23 57.7(5) . . . . ? O2 Y3 N14 C23 106.6(6) 5_656 . . . ? N13 Y3 N14 C23 144.7(6) . . . . ? N11 Y3 N14 C23 -102.2(6) . . . . ? N15 Y3 N14 C23 -21.4(5) . . . . ? N12 Y3 N14 C23 -161.7(5) . . . . ? S4 Y3 N14 C23 -37.3(6) . . . . ? Y3 Y3 N14 C23 76.9(6) 5_656 . . . ? O2 Y3 N14 C22 -70.3(6) . . . . ? O2 Y3 N14 C22 -21.4(7) 5_656 . . . ? N13 Y3 N14 C22 16.8(6) . . . . ? N11 Y3 N14 C22 129.8(6) . . . . ? N15 Y3 N14 C22 -149.4(6) . . . . ? N12 Y3 N14 C22 70.3(6) . . . . ? S4 Y3 N14 C22 -165.3(5) . . . . ? Y3 Y3 N14 C22 -51.1(6) 5_656 . . . ? O2 Y3 N15 C24 -95.8(6) . . . . ? O2 Y3 N15 C24 -144.5(5) 5_656 . . . ? N13 Y3 N15 C24 -25.9(7) . . . . ? N11 Y3 N15 C24 75.7(6) . . . . ? N14 Y3 N15 C24 -8.6(6) . . . . ? N12 Y3 N15 C24 82.4(7) . . . . ? S4 Y3 N15 C24 159.5(6) . . . . ? Y3 Y3 N15 C24 -116.8(6) 5_656 . . . ? Y1 N1 C1 C2 38.5(8) . . . . ? C3 N2 C2 C1 176.5(7) . . . . ? Y1 N2 C2 C1 48.7(8) . . . . ? N1 C1 C2 N2 -57.6(9) . . . . ? C2 N2 C3 C4 -177.6(7) . . . . ? Y1 N2 C3 C4 -49.9(7) . . . . ? C5 N3 C4 C3 -168.9(6) . . . . ? Y1 N3 C4 C3 -39.0(7) . . . . ? N2 C3 C4 N3 59.2(8) . . . . ? C4 N3 C5 C6 87.1(8) . . . . ? Y1 N3 C5 C6 -43.6(8) . . . . ? C7 N4 C6 C5 -171.8(7) . . . . ? Y1 N4 C6 C5 -43.7(8) . . . . ? N3 C5 C6 N4 58.6(10) . . . . ? C6 N4 C7 C8 74.3(9) . . . . ? Y1 N4 C7 C8 -55.1(8) . . . . ? Y1 N5 C8 C7 -25.9(8) . . . . ? N4 C7 C8 N5 53.3(9) . . . . ? Y2 N6 C9 C10 4.9(15) . . . . ? N6 C9 C10 N7 -19(2) . . . . ? C11 N7 C10 C9 -106.8(14) . . . . ? Y2 N7 C10 C9 22.7(16) . . . . ? C10 N7 C11 C12 149.2(12) . . . . ? Y2 N7 C11 C12 20.3(15) . . . . ? N7 C11 C12 N8 -30(2) . . . . ? C13 N8 C12 C11 -106.8(15) . . . . ? Y2 N8 C12 C11 21.5(16) . . . . ? C12 N8 C13 C14 150.4(11) . . . . ? Y2 N8 C13 C14 23.6(15) . . . . ? N8 C13 C14 N9 -42.7(16) . . . . ? C15 N9 C14 C13 164.4(10) . . . . ? Y2 N9 C14 C13 39.1(12) . . . . ? C14 N9 C15 C16 -178.1(9) . . . . ? Y2 N9 C15 C16 -51.3(9) . . . . ? Y2 N10 C16 C15 -39.0(10) . . . . ? N9 C15 C16 N10 60.6(11) . . . . ? Y3 N11 C17 C18 -46.3(9) . . . . ? C19 N12 C18 C17 94.4(9) . . . . ? Y3 N12 C18 C17 -35.7(9) . . . . ? N11 C17 C18 N12 53.1(10) . . . . ? C18 N12 C19 C20 -160.8(8) . . . . ? Y3 N12 C19 C20 -29.1(10) . . . . ? N12 C19 C20 N13 52.0(11) . . . . ? C21 N13 C20 C19 85.0(9) . . . . ? Y3 N13 C20 C19 -49.0(9) . . . . ? C20 N13 C21 C22 -176.4(7) . . . . ? Y3 N13 C21 C22 -43.3(8) . . . . ? C23 N14 C22 C21 -174.7(7) . . . . ? Y3 N14 C22 C21 -45.9(8) . . . . ? N13 C21 C22 N14 58.9(9) . . . . ? C22 N14 C23 C24 176.6(7) . . . . ? Y3 N14 C23 C24 48.6(8) . . . . ? Y3 N15 C24 C23 36.0(9) . . . . ? N14 C23 C24 N15 -55.3(10) . . . . ? 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 N1 H1D S7 0.90 2.91 3.696(7) 146.2 . N2 H2C S7 0.91 2.49 3.368(7) 161.7 8_765 N3 H3C S3 0.91 2.99 3.630(7) 128.9 3_656 N4 H4C Cl1 0.91 2.74 3.442(7) 134.6 . N4 H4C S1 0.91 2.89 3.367(7) 114.1 . N5 H5C S7 0.90 2.81 3.590(7) 145.7 8_765 N5 H5D S5 0.90 2.65 3.419(7) 143.6 . N6 H6C S5 0.90 2.83 3.618(8) 147.5 . N6 H6C S4 0.90 2.99 3.641(7) 131.2 . N6 H6D Cl1 0.90 2.59 3.397(8) 149.8 8_655 N7 H7C Cl1 0.91 2.66 3.395(8) 138.3 . N9 H9C Cl1 0.91 2.42 3.319(8) 170.5 8_655 N10 H10C S7 0.90 2.86 3.589(8) 139.3 . N11 H11C S6 0.90 2.73 3.456(7) 139.0 4_456 N12 H12C S6 0.91 2.54 3.378(7) 153.4 . N13 H13C S4 0.91 2.48 3.385(7) 176.0 5_656 N14 H14C S6 0.91 2.62 3.521(7) 170.1 4_456 N15 H15D Cl1 0.90 2.96 3.561(7) 125.3 8_655 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.276 _refine_diff_density_min -1.196 _refine_diff_density_rms 0.138 # Attachment '- 6.CIF' data_6 _database_code_depnum_ccdc_archive 'CCDC 865327' #TrackingRef '- 6.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H48 Er2 N10 O2 S8 Sb2, 2(C16 H47 Er2 N10 O S3 Sb), 2(Cl)' _chemical_formula_sum 'C48 H142 Cl2 Er6 N30 O4 S14 Sb4 ' _chemical_formula_weight 3214.16 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' Cl Cl 0.1484 0.1585 '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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.548(3) _cell_length_b 15.682(3) _cell_length_c 41.220(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10050(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 25.10 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6152 _exptl_absorpt_coefficient_mu 6.402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0311 _exptl_absorpt_correction_T_max 0.3231 _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 54840 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.10 _reflns_number_total 8957 _reflns_number_gt 8042 _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^)+(0.0187P)^2^+94.2360P] 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 8957 _refine_ls_number_parameters 487 _refine_ls_number_restraints 672 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0800 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.185 _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 Er1 Er 1.09517(2) 0.67240(2) 0.673479(8) 0.02485(8) Uani 1 1 d . . . Er2 Er 0.91305(2) 0.49891(2) 0.672949(7) 0.02207(8) Uani 1 1 d . . . Er3 Er 0.55499(2) 0.603637(19) 0.497370(7) 0.02034(8) Uani 1 1 d . . . Sb1 Sb 1.01284(4) 0.56981(4) 0.751427(12) 0.03777(14) Uani 1 1 d . . . Sb2 Sb 0.37444(3) 0.71355(3) 0.428674(11) 0.02191(11) Uani 1 1 d . . . S1 S 1.07848(12) 0.50674(13) 0.70364(5) 0.0324(4) Uani 1 1 d . . . S2 S 1.03290(18) 0.71417(16) 0.73499(6) 0.0543(7) Uani 1 1 d . . . S3 S 0.86784(14) 0.54432(16) 0.73553(5) 0.0435(5) Uani 1 1 d . . . S4 S 0.49470(12) 0.62294(12) 0.43142(4) 0.0275(4) Uani 1 1 d . . . S5 S 0.29656(15) 0.69265(16) 0.38168(5) 0.0473(6) Uani 1 1 d . . . S6 S 0.28940(12) 0.68931(13) 0.47417(5) 0.0322(4) Uani 1 1 d . . . S7 S 0.43296(14) 0.84966(12) 0.42719(5) 0.0353(5) Uani 1 1 d . . . Cl1 Cl 1.21911(16) 0.37373(17) 0.61807(6) 0.0584(7) Uani 1 1 d . . . O2 O 0.5748(3) 0.4626(3) 0.49786(11) 0.0234(10) Uani 1 1 d . . . O1 O 0.9840(3) 0.6065(3) 0.64950(11) 0.0281(11) Uani 1 1 d . . . N1 N 0.9907(5) 0.7939(4) 0.66450(18) 0.0455(16) Uani 1 1 d U . . H1C H 0.9633 0.7852 0.6456 0.055 Uiso 1 1 calc R . . H1D H 0.9509 0.7924 0.6803 0.055 Uiso 1 1 calc R . . N2 N 1.1642(5) 0.8171(5) 0.68256(18) 0.0456(14) Uani 1 1 d U . . H2C H 1.1899 0.8320 0.6636 0.055 Uiso 1 1 calc R . . N3 N 1.2406(5) 0.6620(5) 0.70124(18) 0.0488(15) Uani 1 1 d U . . H3C H 1.2312 0.6416 0.7216 0.059 Uiso 1 1 calc R . . N4 N 1.2019(5) 0.5800(5) 0.64134(17) 0.0478(15) Uani 1 1 d U . . H4C H 1.1839 0.5252 0.6439 0.057 Uiso 1 1 calc R . . N5 N 1.1210(5) 0.7242(5) 0.61592(17) 0.0453(14) Uani 1 1 d U . . H5C H 1.0698 0.7278 0.6058 0.054 Uiso 1 1 calc R . . H5D H 1.1429 0.7773 0.6170 0.054 Uiso 1 1 calc R . . N6 N 0.7935(4) 0.6084(4) 0.66616(17) 0.0409(15) Uani 1 1 d U . . H6C H 0.7959 0.6453 0.6829 0.049 Uiso 1 1 calc R . . H6D H 0.8033 0.6382 0.6479 0.049 Uiso 1 1 calc R . . N7 N 0.7643(4) 0.4341(4) 0.67981(15) 0.0318(12) Uani 1 1 d U . . H7C H 0.7493 0.4122 0.6602 0.038 Uiso 1 1 calc R . . N8 N 0.9192(4) 0.3482(4) 0.69506(15) 0.0304(12) Uani 1 1 d U . . H8C H 0.9323 0.3538 0.7165 0.036 Uiso 1 1 calc R . . N9 N 1.0059(4) 0.4032(4) 0.63816(15) 0.0321(13) Uani 1 1 d U . . H9C H 1.0613 0.4149 0.6438 0.039 Uiso 1 1 calc R . . N10 N 0.8556(4) 0.4791(4) 0.61532(15) 0.0337(12) Uani 1 1 d U . . H10C H 0.8026 0.4563 0.6167 0.040 Uiso 1 1 calc R . . H10D H 0.8498 0.5311 0.6063 0.040 Uiso 1 1 calc R . . N11 N 0.6792(4) 0.5816(5) 0.45755(16) 0.0372(14) Uani 1 1 d U . . H11C H 0.6753 0.5286 0.4494 0.045 Uiso 1 1 calc R . . H11D H 0.6725 0.6184 0.4410 0.045 Uiso 1 1 calc R . . N12 N 0.7013(4) 0.6023(4) 0.52475(16) 0.0356(13) Uani 1 1 d U . . H12C H 0.7176 0.6578 0.5267 0.043 Uiso 1 1 calc R . . N13 N 0.5441(4) 0.5879(4) 0.55779(15) 0.0364(13) Uani 1 1 d U . . H13C H 0.5367 0.5310 0.5609 0.044 Uiso 1 1 calc R . . N14 N 0.4595(4) 0.7196(4) 0.52405(16) 0.0369(13) Uani 1 1 d U . . H14C H 0.4051 0.7083 0.5170 0.044 Uiso 1 1 calc R . . N15 N 0.6030(4) 0.7545(4) 0.48599(16) 0.0364(13) Uani 1 1 d U . . H15C H 0.6608 0.7560 0.4867 0.044 Uiso 1 1 calc R . . H15D H 0.5869 0.7682 0.4657 0.044 Uiso 1 1 calc R . . C1 C 1.0290(6) 0.8799(6) 0.6639(2) 0.0543(19) Uani 1 1 d U . . H1A H 0.9854 0.9225 0.6685 0.065 Uiso 1 1 calc R . . H1B H 1.0530 0.8916 0.6426 0.065 Uiso 1 1 calc R . . C2 C 1.0989(6) 0.8829(6) 0.6893(2) 0.0536(18) Uani 1 1 d U . . H2A H 1.1256 0.9388 0.6893 0.064 Uiso 1 1 calc R . . H2B H 1.0740 0.8733 0.7106 0.064 Uiso 1 1 calc R . . C3 C 1.2331(7) 0.8150(7) 0.7077(3) 0.0630(19) Uani 1 1 d U . . H3A H 1.2685 0.8655 0.7056 0.076 Uiso 1 1 calc R . . H3B H 1.2070 0.8156 0.7290 0.076 Uiso 1 1 calc R . . C4 C 1.2848(7) 0.7426(7) 0.7046(3) 0.072(2) Uani 1 1 d U . . H4A H 1.3216 0.7392 0.7236 0.087 Uiso 1 1 calc R . . H4B H 1.3217 0.7502 0.6859 0.087 Uiso 1 1 calc R . . C5 C 1.2963(7) 0.5991(8) 0.6843(3) 0.072(2) Uani 1 1 d U . . H5A H 1.3553 0.6180 0.6869 0.087 Uiso 1 1 calc R . . H5B H 1.2911 0.5455 0.6958 0.087 Uiso 1 1 calc R . . C6 C 1.2854(7) 0.5827(8) 0.6537(3) 0.0706(19) Uani 1 1 d U . . H6A H 1.3121 0.5280 0.6493 0.085 Uiso 1 1 calc R . . H6B H 1.3171 0.6251 0.6415 0.085 Uiso 1 1 calc R . . C7 C 1.1980(8) 0.5973(8) 0.6059(3) 0.074(2) Uani 1 1 d U . . H7A H 1.2540 0.5840 0.5969 0.089 Uiso 1 1 calc R . . H7B H 1.1573 0.5576 0.5965 0.089 Uiso 1 1 calc R . . C8 C 1.1773(7) 0.6732(7) 0.5962(2) 0.064(2) Uani 1 1 d U . . H8A H 1.1507 0.6676 0.5750 0.077 Uiso 1 1 calc R . . H8B H 1.2301 0.7051 0.5932 0.077 Uiso 1 1 calc R . . C9 C 0.7059(5) 0.5723(6) 0.6646(2) 0.0417(16) Uani 1 1 d U . . H9A H 0.6939 0.5529 0.6427 0.050 Uiso 1 1 calc R . . H9B H 0.6641 0.6159 0.6702 0.050 Uiso 1 1 calc R . . C10 C 0.6986(5) 0.4986(5) 0.6880(2) 0.0386(16) Uani 1 1 d U . . H10A H 0.7071 0.5186 0.7100 0.046 Uiso 1 1 calc R . . H10B H 0.6417 0.4735 0.6865 0.046 Uiso 1 1 calc R . . C11 C 0.7645(5) 0.3622(5) 0.70282(18) 0.0355(15) Uani 1 1 d U . . H11A H 0.7099 0.3324 0.7018 0.043 Uiso 1 1 calc R . . H11B H 0.7723 0.3833 0.7247 0.043 Uiso 1 1 calc R . . C12 C 0.8362(5) 0.3026(5) 0.6942(2) 0.0380(15) Uani 1 1 d U . . H12A H 0.8374 0.2556 0.7095 0.046 Uiso 1 1 calc R . . H12B H 0.8266 0.2794 0.6727 0.046 Uiso 1 1 calc R . . C13 C 0.9901(6) 0.2970(5) 0.68093(19) 0.0385(15) Uani 1 1 d U . . H13A H 0.9805 0.2369 0.6853 0.046 Uiso 1 1 calc R . . H13B H 1.0443 0.3133 0.6908 0.046 Uiso 1 1 calc R . . C14 C 0.9939(6) 0.3122(5) 0.64423(19) 0.0384(15) Uani 1 1 d U . . H14A H 1.0412 0.2802 0.6349 0.046 Uiso 1 1 calc R . . H14B H 0.9409 0.2929 0.6342 0.046 Uiso 1 1 calc R . . C15 C 0.9985(5) 0.4263(5) 0.60354(18) 0.0346(15) Uani 1 1 d U . . H15A H 1.0308 0.3860 0.5905 0.041 Uiso 1 1 calc R . . H15B H 1.0229 0.4825 0.6001 0.041 Uiso 1 1 calc R . . C16 C 0.9066(5) 0.4261(5) 0.59298(18) 0.0367(16) Uani 1 1 d U . . H16A H 0.9021 0.4485 0.5711 0.044 Uiso 1 1 calc R . . H16B H 0.8846 0.3682 0.5930 0.044 Uiso 1 1 calc R . . C17 C 0.7669(5) 0.5930(6) 0.4711(2) 0.0419(16) Uani 1 1 d U . . H17A H 0.7822 0.6530 0.4709 0.050 Uiso 1 1 calc R . . H17B H 0.8082 0.5623 0.4579 0.050 Uiso 1 1 calc R . . C18 C 0.7690(5) 0.5598(6) 0.5053(2) 0.0413(16) Uani 1 1 d U . . H18A H 0.7595 0.4987 0.5053 0.050 Uiso 1 1 calc R . . H18B H 0.8249 0.5709 0.5149 0.050 Uiso 1 1 calc R . . C19 C 0.6985(6) 0.5676(6) 0.5580(2) 0.0444(16) Uani 1 1 d U . . H19A H 0.7518 0.5805 0.5692 0.053 Uiso 1 1 calc R . . H19B H 0.6915 0.5062 0.5573 0.053 Uiso 1 1 calc R . . C20 C 0.6229(6) 0.6083(6) 0.5757(2) 0.0442(16) Uani 1 1 d U . . H20A H 0.6192 0.5862 0.5976 0.053 Uiso 1 1 calc R . . H20B H 0.6306 0.6696 0.5768 0.053 Uiso 1 1 calc R . . C21 C 0.4666(6) 0.6270(6) 0.5721(2) 0.0474(17) Uani 1 1 d U . . H21A H 0.4165 0.5929 0.5667 0.057 Uiso 1 1 calc R . . H21B H 0.4721 0.6283 0.5955 0.057 Uiso 1 1 calc R . . C22 C 0.4549(6) 0.7137(6) 0.5599(2) 0.0492(17) Uani 1 1 d U . . H22A H 0.4988 0.7502 0.5692 0.059 Uiso 1 1 calc R . . H22B H 0.3994 0.7348 0.5671 0.059 Uiso 1 1 calc R . . C23 C 0.4761(6) 0.8073(6) 0.5141(2) 0.0442(17) Uani 1 1 d U . . H23A H 0.4563 0.8461 0.5308 0.053 Uiso 1 1 calc R . . H23B H 0.4445 0.8197 0.4943 0.053 Uiso 1 1 calc R . . C24 C 0.5693(6) 0.8205(5) 0.5084(2) 0.0439(17) Uani 1 1 d U . . H24A H 0.5787 0.8766 0.4991 0.053 Uiso 1 1 calc R . . H24B H 0.6000 0.8176 0.5289 0.053 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 Er1 0.02063(17) 0.03096(18) 0.02297(16) -0.00394(13) -0.00003(13) -0.00349(13) Er2 0.02118(17) 0.02646(17) 0.01857(15) -0.00089(12) -0.00057(12) -0.00098(13) Er3 0.01850(16) 0.02276(15) 0.01976(15) 0.00147(12) -0.00268(12) -0.00217(12) Sb1 0.0341(3) 0.0611(4) 0.0181(2) 0.0003(2) -0.0038(2) -0.0105(3) Sb2 0.0177(2) 0.0264(2) 0.0216(2) 0.00407(18) -0.00224(18) -0.00063(19) S1 0.0269(10) 0.0427(11) 0.0275(9) 0.0039(8) -0.0036(8) 0.0001(9) S2 0.0727(17) 0.0522(14) 0.0378(12) -0.0194(11) 0.0223(12) -0.0260(13) S3 0.0329(11) 0.0701(15) 0.0276(10) -0.0179(10) 0.0054(9) -0.0132(11) S4 0.0268(10) 0.0332(10) 0.0223(9) 0.0049(7) 0.0005(7) 0.0077(8) S5 0.0417(13) 0.0650(15) 0.0351(11) 0.0027(10) -0.0179(10) -0.0152(11) S6 0.0244(10) 0.0382(11) 0.0340(10) 0.0068(8) 0.0092(8) 0.0049(8) S7 0.0409(12) 0.0272(10) 0.0379(11) 0.0049(8) 0.0060(9) -0.0052(9) Cl1 0.0478(14) 0.0683(16) 0.0590(15) 0.0113(12) -0.0038(11) 0.0215(12) O2 0.021(3) 0.023(2) 0.027(3) 0.006(2) -0.002(2) -0.005(2) O1 0.028(3) 0.032(3) 0.025(3) 0.001(2) -0.004(2) -0.007(2) N1 0.039(3) 0.044(3) 0.053(3) -0.008(3) -0.004(3) 0.002(3) N2 0.042(3) 0.048(3) 0.047(3) -0.002(3) -0.005(3) -0.008(3) N3 0.039(3) 0.059(3) 0.048(3) 0.006(3) -0.009(3) -0.003(3) N4 0.044(3) 0.056(3) 0.044(3) 0.006(3) 0.007(3) 0.012(3) N5 0.040(3) 0.054(3) 0.042(3) 0.003(3) 0.001(3) 0.007(3) N6 0.039(3) 0.042(3) 0.041(3) 0.001(3) 0.001(3) 0.003(3) N7 0.030(3) 0.037(3) 0.029(3) -0.001(2) -0.002(2) -0.004(2) N8 0.033(3) 0.034(3) 0.025(3) 0.003(2) -0.003(2) -0.002(2) N9 0.033(3) 0.035(3) 0.029(3) -0.001(2) 0.003(2) 0.004(2) N10 0.034(3) 0.038(3) 0.029(3) 0.003(2) -0.002(2) -0.001(2) N11 0.025(3) 0.046(3) 0.040(3) 0.004(3) -0.001(3) -0.005(3) N12 0.030(3) 0.039(3) 0.039(3) 0.008(2) -0.008(2) -0.006(2) N13 0.036(3) 0.044(3) 0.029(3) 0.001(2) -0.004(2) 0.000(3) N14 0.036(3) 0.040(3) 0.034(3) -0.003(2) -0.004(2) 0.002(3) N15 0.032(3) 0.041(3) 0.037(3) 0.003(3) -0.002(2) -0.006(3) C1 0.050(4) 0.049(4) 0.064(4) -0.006(3) 0.002(3) 0.008(3) C2 0.052(4) 0.049(4) 0.060(4) -0.011(3) 0.000(3) -0.008(3) C3 0.058(4) 0.066(4) 0.066(4) -0.010(3) -0.015(3) -0.007(3) C4 0.060(4) 0.078(4) 0.080(4) 0.001(4) -0.015(4) -0.005(4) C5 0.058(4) 0.091(4) 0.068(4) 0.005(4) -0.006(4) 0.019(4) C6 0.058(4) 0.081(4) 0.072(4) -0.011(4) 0.001(3) 0.012(3) C7 0.078(4) 0.082(4) 0.061(4) 0.006(4) 0.019(4) 0.020(4) C8 0.063(4) 0.081(5) 0.048(4) 0.006(4) 0.006(4) 0.027(4) C9 0.036(3) 0.046(3) 0.044(3) -0.001(3) -0.003(3) 0.004(3) C10 0.028(3) 0.049(3) 0.039(3) 0.000(3) 0.000(3) -0.002(3) C11 0.035(3) 0.042(3) 0.030(3) 0.003(3) -0.001(3) -0.009(3) C12 0.040(3) 0.037(3) 0.037(3) 0.008(3) -0.004(3) -0.007(3) C13 0.043(3) 0.034(3) 0.038(3) 0.004(3) -0.004(3) 0.005(3) C14 0.041(3) 0.038(3) 0.036(3) -0.001(3) 0.002(3) 0.005(3) C15 0.038(3) 0.034(3) 0.031(3) -0.002(3) 0.006(3) 0.001(3) C16 0.044(4) 0.040(3) 0.027(3) -0.005(3) 0.000(3) -0.002(3) C17 0.025(3) 0.051(4) 0.050(3) 0.002(3) 0.002(3) -0.007(3) C18 0.026(3) 0.047(3) 0.050(3) 0.005(3) -0.013(3) -0.004(3) C19 0.038(3) 0.053(3) 0.042(3) 0.008(3) -0.017(3) -0.006(3) C20 0.044(3) 0.053(3) 0.036(3) 0.003(3) -0.010(3) -0.005(3) C21 0.047(3) 0.057(4) 0.037(3) 0.000(3) 0.005(3) 0.003(3) C22 0.049(4) 0.052(3) 0.047(3) -0.004(3) 0.005(3) 0.006(3) C23 0.044(4) 0.045(3) 0.044(3) -0.002(3) -0.001(3) 0.001(3) C24 0.042(4) 0.036(3) 0.053(4) -0.006(3) -0.006(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O1 2.243(5) . ? Er1 N1 2.532(7) . ? Er1 N2 2.538(7) . ? Er1 N3 2.540(7) . ? Er1 N5 2.540(7) . ? Er1 N4 2.571(7) . ? Er1 S2 2.792(2) . ? Er1 S1 2.892(2) . ? Er1 Er2 3.9269(7) . ? Er2 O1 2.235(5) . ? Er2 N9 2.529(6) . ? Er2 N8 2.535(6) . ? Er2 N7 2.542(6) . ? Er2 N6 2.546(7) . ? Er2 N10 2.557(6) . ? Er2 S3 2.767(2) . ? Er2 S1 2.869(2) . ? Er3 O2 2.233(5) . ? Er3 O2 2.278(5) 5_666 ? Er3 N13 2.508(6) . ? Er3 N15 2.525(7) . ? Er3 N12 2.539(6) . ? Er3 N11 2.558(6) . ? Er3 N14 2.593(7) . ? Er3 S4 2.8913(19) . ? Er3 Er3 3.6791(8) 5_666 ? Sb1 S3 2.382(2) . ? Sb1 S2 2.384(3) . ? Sb1 S1 2.429(2) . ? Sb2 S5 2.308(2) . ? Sb2 S7 2.321(2) . ? Sb2 S6 2.3258(19) . ? Sb2 S4 2.3512(19) . ? O2 Er3 2.278(5) 5_666 ? N1 C1 1.474(12) . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 C2 1.474(12) . ? N2 C3 1.489(12) . ? N2 H2C 0.9100 . ? N3 C4 1.445(13) . ? N3 C5 1.488(13) . ? N3 H3C 0.9100 . ? N4 C6 1.396(13) . ? N4 C7 1.485(12) . ? N4 H4C 0.9100 . ? N5 C8 1.438(12) . ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N6 C9 1.476(11) . ? N6 H6C 0.9000 . ? N6 H6D 0.9000 . ? N7 C11 1.473(10) . ? N7 C10 1.476(10) . ? N7 H7C 0.9100 . ? N8 C12 1.475(10) . ? N8 C13 1.484(10) . ? N8 H8C 0.9100 . ? N9 C14 1.460(10) . ? N9 C15 1.477(9) . ? N9 H9C 0.9100 . ? N10 C16 1.472(10) . ? N10 H10C 0.9000 . ? N10 H10D 0.9000 . ? N11 C17 1.484(10) . ? N11 H11C 0.9000 . ? N11 H11D 0.9000 . ? N12 C19 1.474(10) . ? N12 C18 1.480(11) . ? N12 H12C 0.9100 . ? N13 C20 1.465(10) . ? N13 C21 1.476(11) . ? N13 H13C 0.9100 . ? N14 C23 1.458(11) . ? N14 C22 1.483(11) . ? N14 H14C 0.9100 . ? N15 C24 1.483(10) . ? N15 H15C 0.9000 . ? N15 H15D 0.9000 . ? C1 C2 1.511(13) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.397(15) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.295(14) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.297(14) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.510(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.497(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.533(11) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.494(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.505(11) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.524(12) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.461(13) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.483(12) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 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 O1 Er1 N1 77.8(2) . . ? O1 Er1 N2 143.4(2) . . ? N1 Er1 N2 67.6(2) . . ? O1 Er1 N3 148.7(2) . . ? N1 Er1 N3 133.3(2) . . ? N2 Er1 N3 67.3(2) . . ? O1 Er1 N5 81.8(2) . . ? N1 Er1 N5 74.0(2) . . ? N2 Er1 N5 77.6(2) . . ? N3 Er1 N5 107.5(2) . . ? O1 Er1 N4 90.6(2) . . ? N1 Er1 N4 139.8(2) . . ? N2 Er1 N4 107.9(3) . . ? N3 Er1 N4 67.7(2) . . ? N5 Er1 N4 66.2(2) . . ? O1 Er1 S2 103.95(14) . . ? N1 Er1 S2 74.55(18) . . ? N2 Er1 S2 78.63(18) . . ? N3 Er1 S2 85.10(19) . . ? N5 Er1 S2 145.90(18) . . ? N4 Er1 S2 145.50(17) . . ? O1 Er1 S1 72.91(13) . . ? N1 Er1 S1 132.97(18) . . ? N2 Er1 S1 141.06(17) . . ? N3 Er1 S1 80.11(18) . . ? N5 Er1 S1 134.70(18) . . ? N4 Er1 S1 76.90(18) . . ? S2 Er1 S1 77.83(7) . . ? O1 Er1 Er2 28.68(12) . . ? N1 Er1 Er2 93.33(17) . . ? N2 Er1 Er2 157.69(17) . . ? N3 Er1 Er2 126.86(18) . . ? N5 Er1 Er2 109.31(18) . . ? N4 Er1 Er2 94.15(19) . . ? S2 Er1 Er2 85.27(5) . . ? S1 Er1 Er2 46.79(4) . . ? O1 Er2 N9 85.45(19) . . ? O1 Er2 N8 147.18(19) . . ? N9 Er2 N8 68.2(2) . . ? O1 Er2 N7 143.03(19) . . ? N9 Er2 N7 110.2(2) . . ? N8 Er2 N7 67.8(2) . . ? O1 Er2 N6 78.7(2) . . ? N9 Er2 N6 139.0(2) . . ? N8 Er2 N6 134.1(2) . . ? N7 Er2 N6 67.5(2) . . ? O1 Er2 N10 82.09(19) . . ? N9 Er2 N10 66.5(2) . . ? N8 Er2 N10 103.5(2) . . ? N7 Er2 N10 74.7(2) . . ? N6 Er2 N10 74.0(2) . . ? O1 Er2 S3 109.53(13) . . ? N9 Er2 S3 145.74(15) . . ? N8 Er2 S3 85.09(15) . . ? N7 Er2 S3 76.59(15) . . ? N6 Er2 S3 75.13(17) . . ? N10 Er2 S3 143.96(15) . . ? O1 Er2 S1 73.48(13) . . ? N9 Er2 S1 76.32(16) . . ? N8 Er2 S1 81.24(15) . . ? N7 Er2 S1 141.61(14) . . ? N6 Er2 S1 132.38(17) . . ? N10 Er2 S1 136.74(15) . . ? S3 Er2 S1 78.79(6) . . ? O1 Er2 Er1 28.79(12) . . ? N9 Er2 Er1 90.15(15) . . ? N8 Er2 Er1 128.09(14) . . ? N7 Er2 Er1 158.81(15) . . ? N6 Er2 Er1 93.43(16) . . ? N10 Er2 Er1 109.95(15) . . ? S3 Er2 Er1 89.98(5) . . ? S1 Er2 Er1 47.27(4) . . ? O2 Er3 O2 70.7(2) . 5_666 ? O2 Er3 N13 84.4(2) . . ? O2 Er3 N13 79.04(19) 5_666 . ? O2 Er3 N15 152.8(2) . . ? O2 Er3 N15 134.84(19) 5_666 . ? N13 Er3 N15 107.2(2) . . ? O2 Er3 N12 82.21(19) . . ? O2 Er3 N12 138.71(18) 5_666 . ? N13 Er3 N12 67.6(2) . . ? N15 Er3 N12 79.9(2) . . ? O2 Er3 N11 76.6(2) . . ? O2 Er3 N11 131.51(19) 5_666 . ? N13 Er3 N11 132.4(2) . . ? N15 Er3 N11 77.5(2) . . ? N12 Er3 N11 66.9(2) . . ? O2 Er3 N14 140.34(19) . . ? O2 Er3 N14 77.04(19) 5_666 . ? N13 Er3 N14 67.0(2) . . ? N15 Er3 N14 65.8(2) . . ? N12 Er3 N14 109.3(2) . . ? N11 Er3 N14 143.1(2) . . ? O2 Er3 S4 99.02(12) . . ? O2 Er3 S4 80.90(12) 5_666 . ? N13 Er3 S4 157.21(16) . . ? N15 Er3 S4 79.80(15) . . ? N12 Er3 S4 135.16(15) . . ? N11 Er3 S4 69.85(15) . . ? N14 Er3 S4 98.02(15) . . ? O2 Er3 Er3 35.75(12) . 5_666 ? O2 Er3 Er3 34.96(12) 5_666 5_666 ? N13 Er3 Er3 79.83(16) . 5_666 ? N15 Er3 Er3 167.47(15) . 5_666 ? N12 Er3 Er3 112.51(15) . 5_666 ? N11 Er3 Er3 105.64(16) . 5_666 ? N14 Er3 Er3 109.18(15) . 5_666 ? S4 Er3 Er3 89.84(4) . 5_666 ? S3 Sb1 S2 101.83(10) . . ? S3 Sb1 S1 96.10(7) . . ? S2 Sb1 S1 95.81(7) . . ? S5 Sb2 S7 108.31(8) . . ? S5 Sb2 S6 110.81(8) . . ? S7 Sb2 S6 113.23(7) . . ? S5 Sb2 S4 111.83(8) . . ? S7 Sb2 S4 104.20(8) . . ? S6 Sb2 S4 108.33(7) . . ? Sb1 S1 Er2 89.90(6) . . ? Sb1 S1 Er1 91.18(7) . . ? Er2 S1 Er1 85.94(5) . . ? Sb1 S2 Er1 94.63(8) . . ? Sb1 S3 Er2 93.40(7) . . ? Sb2 S4 Er3 111.49(7) . . ? Er3 O2 Er3 109.29(19) . 5_666 ? Er2 O1 Er1 122.5(2) . . ? C1 N1 Er1 115.6(5) . . ? C1 N1 H1C 108.4 . . ? Er1 N1 H1C 108.4 . . ? C1 N1 H1D 108.4 . . ? Er1 N1 H1D 108.4 . . ? H1C N1 H1D 107.4 . . ? C2 N2 C3 112.4(7) . . ? C2 N2 Er1 111.3(5) . . ? C3 N2 Er1 112.7(6) . . ? C2 N2 H2C 106.7 . . ? C3 N2 H2C 106.7 . . ? Er1 N2 H2C 106.7 . . ? C4 N3 C5 110.4(9) . . ? C4 N3 Er1 114.2(6) . . ? C5 N3 Er1 110.5(6) . . ? C4 N3 H3C 107.1 . . ? C5 N3 H3C 107.1 . . ? Er1 N3 H3C 107.1 . . ? C6 N4 C7 113.1(9) . . ? C6 N4 Er1 113.3(6) . . ? C7 N4 Er1 112.1(6) . . ? C6 N4 H4C 105.8 . . ? C7 N4 H4C 105.8 . . ? Er1 N4 H4C 105.8 . . ? C8 N5 Er1 116.5(6) . . ? C8 N5 H5C 108.2 . . ? Er1 N5 H5C 108.2 . . ? C8 N5 H5D 108.2 . . ? Er1 N5 H5D 108.2 . . ? H5C N5 H5D 107.3 . . ? C9 N6 Er2 114.8(5) . . ? C9 N6 H6C 108.6 . . ? Er2 N6 H6C 108.6 . . ? C9 N6 H6D 108.6 . . ? Er2 N6 H6D 108.6 . . ? H6C N6 H6D 107.5 . . ? C11 N7 C10 112.2(6) . . ? C11 N7 Er2 112.0(5) . . ? C10 N7 Er2 112.4(5) . . ? C11 N7 H7C 106.5 . . ? C10 N7 H7C 106.5 . . ? Er2 N7 H7C 106.5 . . ? C12 N8 C13 112.3(6) . . ? C12 N8 Er2 114.2(5) . . ? C13 N8 Er2 113.0(4) . . ? C12 N8 H8C 105.4 . . ? C13 N8 H8C 105.4 . . ? Er2 N8 H8C 105.4 . . ? C14 N9 C15 113.3(6) . . ? C14 N9 Er2 114.2(5) . . ? C15 N9 Er2 110.9(4) . . ? C14 N9 H9C 105.9 . . ? C15 N9 H9C 105.9 . . ? Er2 N9 H9C 105.9 . . ? C16 N10 Er2 117.5(5) . . ? C16 N10 H10C 107.9 . . ? Er2 N10 H10C 107.9 . . ? C16 N10 H10D 107.9 . . ? Er2 N10 H10D 107.9 . . ? H10C N10 H10D 107.2 . . ? C17 N11 Er3 115.8(5) . . ? C17 N11 H11C 108.3 . . ? Er3 N11 H11C 108.3 . . ? C17 N11 H11D 108.3 . . ? Er3 N11 H11D 108.3 . . ? H11C N11 H11D 107.4 . . ? C19 N12 C18 110.9(6) . . ? C19 N12 Er3 112.9(5) . . ? C18 N12 Er3 113.6(5) . . ? C19 N12 H12C 106.3 . . ? C18 N12 H12C 106.3 . . ? Er3 N12 H12C 106.3 . . ? C20 N13 C21 113.0(7) . . ? C20 N13 Er3 115.0(5) . . ? C21 N13 Er3 114.3(5) . . ? C20 N13 H13C 104.3 . . ? C21 N13 H13C 104.3 . . ? Er3 N13 H13C 104.3 . . ? C23 N14 C22 110.4(7) . . ? C23 N14 Er3 116.1(5) . . ? C22 N14 Er3 114.0(5) . . ? C23 N14 H14C 105.0 . . ? C22 N14 H14C 105.0 . . ? Er3 N14 H14C 105.0 . . ? C24 N15 Er3 115.7(5) . . ? C24 N15 H15C 108.3 . . ? Er3 N15 H15C 108.3 . . ? C24 N15 H15D 108.3 . . ? Er3 N15 H15D 108.3 . . ? H15C N15 H15D 107.4 . . ? N1 C1 C2 107.9(8) . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C1 110.0(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 111.8(9) . . ? C4 C3 H3A 109.3 . . ? N2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? N2 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C3 C4 N3 116.5(9) . . ? C3 C4 H4A 108.2 . . ? N3 C4 H4A 108.2 . . ? C3 C4 H4B 108.2 . . ? N3 C4 H4B 108.2 . . ? H4A C4 H4B 107.3 . . ? C6 C5 N3 120.8(10) . . ? C6 C5 H5A 107.1 . . ? N3 C5 H5A 107.1 . . ? C6 C5 H5B 107.1 . . ? N3 C5 H5B 107.1 . . ? H5A C5 H5B 106.8 . . ? C5 C6 N4 118.9(10) . . ? C5 C6 H6A 107.6 . . ? N4 C6 H6A 107.6 . . ? C5 C6 H6B 107.6 . . ? N4 C6 H6B 107.6 . . ? H6A C6 H6B 107.0 . . ? C8 C7 N4 118.8(10) . . ? C8 C7 H7A 107.6 . . ? N4 C7 H7A 107.6 . . ? C8 C7 H7B 107.6 . . ? N4 C7 H7B 107.6 . . ? H7A C7 H7B 107.0 . . ? C7 C8 N5 119.1(10) . . ? C7 C8 H8A 107.5 . . ? N5 C8 H8A 107.5 . . ? C7 C8 H8B 107.5 . . ? N5 C8 H8B 107.5 . . ? H8A C8 H8B 107.0 . . ? N6 C9 C10 109.6(7) . . ? N6 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? N6 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? N7 C10 C9 109.1(7) . . ? N7 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? N7 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? N7 C11 C12 109.1(6) . . ? N7 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? N7 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N8 C12 C11 110.1(7) . . ? N8 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? N8 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.2 . . ? N8 C13 C14 109.4(6) . . ? N8 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? N8 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? H13A C13 H13B 108.2 . . ? N9 C14 C13 109.1(6) . . ? N9 C14 H14A 109.9 . . ? C13 C14 H14A 109.9 . . ? N9 C14 H14B 109.9 . . ? C13 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? N9 C15 C16 110.9(6) . . ? N9 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? N9 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? N10 C16 C15 109.4(6) . . ? N10 C16 H16A 109.8 . . ? C15 C16 H16A 109.8 . . ? N10 C16 H16B 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? N11 C17 C18 109.3(6) . . ? N11 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? N11 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.3 . . ? N12 C18 C17 109.7(7) . . ? N12 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? N12 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? N12 C19 C20 108.3(7) . . ? N12 C19 H19A 110.0 . . ? C20 C19 H19A 110.0 . . ? N12 C19 H19B 110.0 . . ? C20 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? N13 C20 C19 108.2(7) . . ? N13 C20 H20A 110.1 . . ? C19 C20 H20A 110.1 . . ? N13 C20 H20B 110.1 . . ? C19 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? C22 C21 N13 110.5(8) . . ? C22 C21 H21A 109.5 . . ? N13 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? N13 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C21 C22 N14 113.3(7) . . ? C21 C22 H22A 108.9 . . ? N14 C22 H22A 108.9 . . ? C21 C22 H22B 108.9 . . ? N14 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? N14 C23 C24 110.5(7) . . ? N14 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? N14 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? N15 C24 C23 110.2(7) . . ? N15 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? N15 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.030 _refine_diff_density_min -1.515 _refine_diff_density_rms 0.156 # Attachment '- 7.CIF' data_7 _database_code_depnum_ccdc_archive 'CCDC 865328' #TrackingRef '- 7.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H48 Gd2 N10 O2 S4 Sb, Cl, (H2 O)0.25' _chemical_formula_sum 'C16 H48.5 Cl Gd2 N10 O2.25 S4 Sb' _chemical_formula_weight 1017.13 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' Gd Gd -0.1653 3.9035 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.281(3) _cell_length_b 15.686(3) _cell_length_c 16.025(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.33(3) _cell_angle_gamma 90.00 _cell_volume 3478.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 25.10 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.941 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 4.889 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4648 _exptl_absorpt_correction_T_max 0.6738 _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 19374 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.10 _reflns_number_total 6183 _reflns_number_gt 5658 _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^)+(0.0166P)^2^+4.6229P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6183 _refine_ls_number_parameters 342 _refine_ls_number_restraints 426 _refine_ls_R_factor_all 0.0221 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0436 _refine_ls_wR_factor_gt 0.0423 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.091 _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 Gd1 Gd 0.356580(12) 0.463040(11) 0.262280(10) 0.02333(5) Uani 1 1 d . . . Gd2 Gd 0.192020(12) 0.656040(11) 0.224450(10) 0.02441(5) Uani 1 1 d . . . Sb1 Sb 0.602310(17) 0.302390(15) 0.422280(14) 0.02830(6) Uani 1 1 d . . . O1 O 0.28994(19) 0.57252(17) 0.32148(17) 0.0399(6) Uani 1 1 d . . . O2 O 0.22463(18) 0.52612(16) 0.16520(18) 0.0333(6) Uani 1 1 d . . . Cl1 Cl 0.01177(8) 0.35798(8) 0.16271(9) 0.0606(3) Uani 1 1 d . . . S1 S 0.70980(7) 0.19281(6) 0.41202(6) 0.0353(2) Uani 1 1 d . . . S2 S 0.69310(8) 0.42228(7) 0.47440(6) 0.0427(2) Uani 1 1 d . . . S3 S 0.50726(7) 0.33022(6) 0.28384(6) 0.0331(2) Uani 1 1 d . . . S4 S 0.50590(8) 0.25824(8) 0.51010(7) 0.0492(3) Uani 1 1 d . . . N1 N 0.3322(2) 0.3966(2) 0.4005(2) 0.0415(8) Uani 1 1 d U . . H1C H 0.3846 0.3657 0.4257 0.050 Uiso 1 1 calc R . . H1D H 0.3254 0.4382 0.4373 0.050 Uiso 1 1 calc R . . N2 N 0.2463(2) 0.3332(2) 0.2314(2) 0.0457(8) Uani 1 1 d U . . H2C H 0.1852 0.3545 0.2152 0.055 Uiso 1 1 calc R . . N3 N 0.3581(2) 0.3908(2) 0.1172(2) 0.0438(8) Uani 1 1 d U . . H3C H 0.4096 0.3546 0.1283 0.053 Uiso 1 1 calc R . . N4 N 0.4576(2) 0.5426(2) 0.1788(2) 0.0414(8) Uani 1 1 d U . . H4C H 0.4250 0.5921 0.1626 0.050 Uiso 1 1 calc R . . N6 N 0.1286(2) 0.6820(2) 0.3611(2) 0.0374(7) Uani 1 1 d U . . H6C H 0.1778 0.6740 0.4079 0.045 Uiso 1 1 calc R . . H6D H 0.1099 0.7367 0.3613 0.045 Uiso 1 1 calc R . . N5 N 0.4985(2) 0.5396(2) 0.3631(2) 0.0393(7) Uani 1 1 d U . . H5C H 0.4780 0.5647 0.4059 0.047 Uiso 1 1 calc R . . H5D H 0.5441 0.5012 0.3869 0.047 Uiso 1 1 calc R . . N7 N 0.0462(3) 0.5632(2) 0.2317(2) 0.0512(9) Uani 1 1 d U . . H7C H 0.0634 0.5101 0.2180 0.061 Uiso 1 1 calc R . . N8 N 0.0496(2) 0.6666(2) 0.0854(2) 0.0446(8) Uani 1 1 d U . . H8C H 0.0761 0.6618 0.0394 0.054 Uiso 1 1 calc R . . N9 N 0.1231(2) 0.8099(2) 0.1962(2) 0.0388(7) Uani 1 1 d U . . H9C H 0.0789 0.8164 0.2280 0.047 Uiso 1 1 calc R . . N10 N 0.3056(2) 0.7689(2) 0.3066(2) 0.0379(7) Uani 1 1 d U . . H10C H 0.3311 0.7496 0.3603 0.045 Uiso 1 1 calc R . . H10D H 0.3545 0.7758 0.2810 0.045 Uiso 1 1 calc R . . C1 C 0.2462(3) 0.3416(3) 0.3824(3) 0.0582(12) Uani 1 1 d U . . H1A H 0.1882 0.3763 0.3673 0.070 Uiso 1 1 calc R . . H1B H 0.2446 0.3087 0.4333 0.070 Uiso 1 1 calc R . . C2 C 0.2494(3) 0.2832(3) 0.3098(3) 0.0593(12) Uani 1 1 d U . . H2A H 0.3082 0.2495 0.3245 0.071 Uiso 1 1 calc R . . H2B H 0.1947 0.2444 0.2997 0.071 Uiso 1 1 calc R . . C3 C 0.2577(3) 0.2812(3) 0.1580(3) 0.0604(12) Uani 1 1 d U . . H3A H 0.2007 0.2461 0.1375 0.073 Uiso 1 1 calc R . . H3B H 0.3130 0.2438 0.1764 0.073 Uiso 1 1 calc R . . C4 C 0.2717(3) 0.3376(3) 0.0865(3) 0.0601(12) Uani 1 1 d U . . H4A H 0.2790 0.3030 0.0384 0.072 Uiso 1 1 calc R . . H4B H 0.2154 0.3738 0.0667 0.072 Uiso 1 1 calc R . . C5 C 0.3768(3) 0.4543(3) 0.0557(3) 0.0544(11) Uani 1 1 d U . . H5A H 0.3222 0.4927 0.0390 0.065 Uiso 1 1 calc R . . H5B H 0.3855 0.4259 0.0044 0.065 Uiso 1 1 calc R . . C6 C 0.4664(3) 0.5037(3) 0.0974(3) 0.0549(11) Uani 1 1 d U . . H6A H 0.5219 0.4659 0.1087 0.066 Uiso 1 1 calc R . . H6B H 0.4769 0.5480 0.0585 0.066 Uiso 1 1 calc R . . C7 C 0.5523(3) 0.5697(3) 0.2337(3) 0.0532(10) Uani 1 1 d U . . H7A H 0.5800 0.6133 0.2041 0.064 Uiso 1 1 calc R . . H7B H 0.5962 0.5215 0.2442 0.064 Uiso 1 1 calc R . . C8 C 0.5406(3) 0.6040(3) 0.3175(3) 0.0551(11) Uani 1 1 d U . . H8A H 0.6031 0.6212 0.3529 0.066 Uiso 1 1 calc R . . H8B H 0.4991 0.6538 0.3071 0.066 Uiso 1 1 calc R . . C9 C 0.0492(4) 0.6282(4) 0.3684(3) 0.0724(14) Uani 1 1 d U . . H9A H 0.0575 0.6141 0.4288 0.087 Uiso 1 1 calc R . . H9B H -0.0099 0.6610 0.3505 0.087 Uiso 1 1 calc R . . C10 C 0.0375(5) 0.5539(4) 0.3225(4) 0.0824(15) Uani 1 1 d U . . H10A H -0.0257 0.5306 0.3214 0.099 Uiso 1 1 calc R . . H10B H 0.0855 0.5132 0.3521 0.099 Uiso 1 1 calc R . . C11 C -0.0421(3) 0.5810(4) 0.1659(3) 0.0652(12) Uani 1 1 d U . . H11A H -0.0728 0.6319 0.1812 0.078 Uiso 1 1 calc R . . H11B H -0.0869 0.5338 0.1619 0.078 Uiso 1 1 calc R . . C12 C -0.0175(3) 0.5938(3) 0.0810(3) 0.0630(13) Uani 1 1 d U . . H12A H 0.0123 0.5424 0.0657 0.076 Uiso 1 1 calc R . . H12B H -0.0762 0.6044 0.0366 0.076 Uiso 1 1 calc R . . C13 C -0.0001(3) 0.7502(3) 0.0776(3) 0.0532(10) Uani 1 1 d U . . H13A H -0.0460 0.7504 0.1133 0.064 Uiso 1 1 calc R . . H13B H -0.0357 0.7591 0.0184 0.064 Uiso 1 1 calc R . . C14 C 0.0713(3) 0.8218(3) 0.1052(3) 0.0477(10) Uani 1 1 d U . . H14A H 0.1171 0.8222 0.0695 0.057 Uiso 1 1 calc R . . H14B H 0.0377 0.8760 0.0982 0.057 Uiso 1 1 calc R . . C15 C 0.1979(3) 0.8756(3) 0.2256(3) 0.0446(9) Uani 1 1 d U . . H15A H 0.1673 0.9303 0.2291 0.054 Uiso 1 1 calc R . . H15B H 0.2370 0.8808 0.1842 0.054 Uiso 1 1 calc R . . C16 C 0.2617(3) 0.8525(3) 0.3127(3) 0.0467(10) Uani 1 1 d U . . H16A H 0.3117 0.8952 0.3307 0.056 Uiso 1 1 calc R . . H16B H 0.2235 0.8505 0.3551 0.056 Uiso 1 1 calc R . . O3W O 0.1577(10) 0.5597(9) -0.0274(9) 0.069(4) Uani 0.25 1 d PU . . H2 H 0.187(3) 0.510(3) 0.115(3) 0.050(13) Uiso 1 1 d . . . H1 H 0.304(3) 0.589(3) 0.381(3) 0.050(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02291(9) 0.02382(9) 0.02309(9) -0.00037(7) 0.00536(7) 0.00256(7) Gd2 0.02215(9) 0.02422(9) 0.02606(9) 0.00082(7) 0.00444(7) 0.00262(7) Sb1 0.02888(13) 0.03142(13) 0.02330(12) -0.00297(10) 0.00400(9) 0.00723(10) O1 0.0466(16) 0.0412(16) 0.0294(14) -0.0013(12) 0.0045(12) 0.0219(13) O2 0.0307(14) 0.0286(14) 0.0395(15) -0.0001(12) 0.0066(12) 0.0065(11) Cl1 0.0383(6) 0.0531(7) 0.0909(9) 0.0002(6) 0.0173(6) -0.0088(5) S1 0.0359(5) 0.0340(5) 0.0375(5) 0.0003(4) 0.0118(4) 0.0112(4) S2 0.0496(6) 0.0357(5) 0.0359(5) -0.0102(4) -0.0023(5) 0.0025(5) S3 0.0318(5) 0.0380(5) 0.0259(4) -0.0043(4) 0.0005(4) 0.0116(4) S4 0.0429(6) 0.0674(8) 0.0409(6) 0.0144(5) 0.0175(5) 0.0128(6) N1 0.0470(18) 0.0369(18) 0.0449(18) 0.0091(14) 0.0196(15) 0.0136(15) N2 0.0332(17) 0.0344(17) 0.065(2) -0.0007(16) 0.0027(15) 0.0021(14) N3 0.0418(17) 0.0499(19) 0.0354(16) -0.0104(15) 0.0016(14) 0.0157(16) N4 0.0431(18) 0.0471(19) 0.0387(17) 0.0075(14) 0.0189(14) 0.0072(15) N6 0.0391(17) 0.0384(17) 0.0358(16) -0.0022(14) 0.0114(13) 0.0007(14) N5 0.0379(17) 0.0326(17) 0.0431(18) -0.0035(14) 0.0021(14) 0.0024(14) N7 0.056(2) 0.052(2) 0.0498(19) -0.0133(16) 0.0226(16) -0.0202(17) N8 0.0394(17) 0.0478(19) 0.0422(18) -0.0006(15) 0.0016(15) 0.0053(15) N9 0.0408(17) 0.0363(17) 0.0400(16) 0.0035(14) 0.0111(14) 0.0078(14) N10 0.0360(17) 0.0411(18) 0.0361(16) 0.0011(14) 0.0080(14) -0.0058(15) C1 0.049(2) 0.056(3) 0.076(3) 0.028(2) 0.027(2) 0.003(2) C2 0.047(2) 0.038(2) 0.089(3) 0.011(2) 0.010(2) -0.0075(19) C3 0.048(2) 0.045(2) 0.079(3) -0.021(2) -0.003(2) -0.001(2) C4 0.052(2) 0.062(3) 0.056(2) -0.028(2) -0.006(2) 0.012(2) C5 0.063(2) 0.070(3) 0.033(2) -0.0036(19) 0.0159(19) 0.021(2) C6 0.060(2) 0.069(3) 0.045(2) 0.005(2) 0.0307(19) 0.012(2) C7 0.043(2) 0.054(2) 0.067(3) 0.006(2) 0.023(2) -0.007(2) C8 0.052(2) 0.045(2) 0.067(3) 0.001(2) 0.012(2) -0.011(2) C9 0.077(3) 0.089(3) 0.060(3) -0.012(3) 0.032(2) -0.035(3) C10 0.101(3) 0.084(3) 0.075(3) -0.011(3) 0.045(3) -0.039(3) C11 0.044(2) 0.062(3) 0.092(3) -0.004(2) 0.023(2) -0.011(2) C12 0.045(2) 0.056(3) 0.069(3) -0.007(2) -0.022(2) -0.005(2) C13 0.043(2) 0.056(2) 0.053(2) 0.0072(19) -0.0032(18) 0.0126(19) C14 0.050(2) 0.044(2) 0.046(2) 0.0095(18) 0.0061(18) 0.0136(19) C15 0.049(2) 0.033(2) 0.054(2) 0.0018(18) 0.0158(19) 0.0015(18) C16 0.050(2) 0.040(2) 0.051(2) -0.0074(18) 0.0148(19) -0.0086(19) O3W 0.075(7) 0.066(7) 0.063(7) -0.002(6) 0.014(6) -0.021(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 Gd1 O1 2.281(3) . ? Gd1 O2 2.345(3) . ? Gd1 N4 2.527(3) . ? Gd1 N2 2.548(3) . ? Gd1 N1 2.548(3) . ? Gd1 N5 2.557(3) . ? Gd1 N3 2.592(3) . ? Gd1 S3 2.9534(10) . ? Gd1 Gd2 3.7882(6) . ? Gd2 O1 2.239(3) . ? Gd2 O2 2.343(3) . ? Gd2 N10 2.538(3) . ? Gd2 N7 2.568(3) . ? Gd2 N6 2.600(3) . ? Gd2 N9 2.603(3) . ? Gd2 N8 2.625(3) . ? Gd2 S1 2.9324(11) 2_655 ? Sb1 S4 2.3054(12) . ? Sb1 S2 2.3193(11) . ? Sb1 S1 2.3373(10) . ? Sb1 S3 2.3376(12) . ? O1 H1 0.96(4) . ? O2 H2 0.89(4) . ? S1 Gd2 2.9324(11) 2_645 ? N1 C1 1.470(6) . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 C3 1.472(6) . ? N2 C2 1.473(6) . ? N2 H2C 0.9100 . ? N3 C4 1.470(6) . ? N3 C5 1.471(6) . ? N3 H3C 0.9100 . ? N4 C6 1.472(5) . ? N4 C7 1.481(5) . ? N4 H4C 0.9100 . ? N6 C9 1.441(6) . ? N6 H6C 0.9000 . ? N6 H6D 0.9000 . ? N5 C8 1.460(5) . ? N5 H5C 0.9000 . ? N5 H5D 0.9000 . ? N7 C11 1.457(6) . ? N7 C10 1.498(6) . ? N7 H7C 0.9100 . ? N8 C12 1.481(6) . ? N8 C13 1.483(5) . ? N8 H8C 0.9100 . ? N9 C14 1.474(5) . ? N9 C15 1.476(5) . ? N9 H9C 0.9100 . ? N10 C16 1.468(5) . ? N10 H10C 0.9000 . ? N10 H10D 0.9000 . ? C1 C2 1.491(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.501(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.504(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.495(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.367(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.502(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.508(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.511(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 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 O1 Gd1 O2 66.96(9) . . ? O1 Gd1 N4 101.54(11) . . ? O2 Gd1 N4 84.88(10) . . ? O1 Gd1 N2 112.42(11) . . ? O2 Gd1 N2 81.48(10) . . ? N4 Gd1 N2 134.32(11) . . ? O1 Gd1 N1 77.62(10) . . ? O2 Gd1 N1 119.27(10) . . ? N4 Gd1 N1 151.74(11) . . ? N2 Gd1 N1 68.35(12) . . ? O1 Gd1 N5 74.37(10) . . ? O2 Gd1 N5 127.02(10) . . ? N4 Gd1 N5 68.62(11) . . ? N2 Gd1 N5 148.60(11) . . ? N1 Gd1 N5 84.28(11) . . ? O1 Gd1 N3 143.09(10) . . ? O2 Gd1 N3 76.90(10) . . ? N4 Gd1 N3 66.93(11) . . ? N2 Gd1 N3 67.55(12) . . ? N1 Gd1 N3 129.37(11) . . ? N5 Gd1 N3 126.21(11) . . ? O1 Gd1 S3 148.15(7) . . ? O2 Gd1 S3 144.87(7) . . ? N4 Gd1 S3 85.15(8) . . ? N2 Gd1 S3 81.73(8) . . ? N1 Gd1 S3 82.08(8) . . ? N5 Gd1 S3 79.44(8) . . ? N3 Gd1 S3 68.20(8) . . ? O1 Gd1 Gd2 32.71(7) . . ? O2 Gd1 Gd2 36.08(6) . . ? N4 Gd1 Gd2 86.18(8) . . ? N2 Gd1 Gd2 106.18(8) . . ? N1 Gd1 Gd2 104.66(7) . . ? N5 Gd1 Gd2 95.11(7) . . ? N3 Gd1 Gd2 110.40(8) . . ? S3 Gd1 Gd2 170.99(2) . . ? O1 Gd2 O2 67.66(10) . . ? O1 Gd2 N10 80.73(11) . . ? O2 Gd2 N10 130.64(10) . . ? O1 Gd2 N7 90.61(12) . . ? O2 Gd2 N7 76.68(11) . . ? N10 Gd2 N7 142.54(10) . . ? O1 Gd2 N6 78.13(10) . . ? O2 Gd2 N6 128.52(10) . . ? N10 Gd2 N6 76.42(10) . . ? N7 Gd2 N6 66.13(11) . . ? O1 Gd2 N9 143.85(10) . . ? O2 Gd2 N9 147.17(10) . . ? N10 Gd2 N9 66.99(10) . . ? N7 Gd2 N9 104.95(12) . . ? N6 Gd2 N9 78.82(10) . . ? O1 Gd2 N8 147.80(11) . . ? O2 Gd2 N8 84.30(10) . . ? N10 Gd2 N8 131.15(11) . . ? N7 Gd2 N8 66.88(12) . . ? N6 Gd2 N8 110.31(11) . . ? N9 Gd2 N8 67.28(10) . . ? O1 Gd2 S1 107.53(7) . 2_655 ? O2 Gd2 S1 71.89(7) . 2_655 ? N10 Gd2 S1 83.54(7) . 2_655 ? N7 Gd2 S1 133.49(8) . 2_655 ? N6 Gd2 S1 158.08(7) . 2_655 ? N9 Gd2 S1 85.29(7) . 2_655 ? N8 Gd2 S1 76.55(8) . 2_655 ? O1 Gd2 Gd1 33.40(7) . . ? O2 Gd2 Gd1 36.11(7) . . ? N10 Gd2 Gd1 100.54(8) . . ? N7 Gd2 Gd1 90.98(9) . . ? N6 Gd2 Gd1 108.76(7) . . ? N9 Gd2 Gd1 164.06(7) . . ? N8 Gd2 Gd1 120.40(8) . . ? S1 Gd2 Gd1 83.36(2) 2_655 . ? S4 Sb1 S2 112.88(4) . . ? S4 Sb1 S1 108.90(4) . . ? S2 Sb1 S1 107.65(4) . . ? S4 Sb1 S3 109.95(4) . . ? S2 Sb1 S3 109.38(4) . . ? S1 Sb1 S3 107.93(4) . . ? Gd2 O1 Gd1 113.89(11) . . ? Gd2 O1 H1 118(3) . . ? Gd1 O1 H1 128(3) . . ? Gd2 O2 Gd1 107.81(11) . . ? Gd2 O2 H2 118(3) . . ? Gd1 O2 H2 134(3) . . ? Sb1 S1 Gd2 129.84(4) . 2_645 ? Sb1 S3 Gd1 118.55(4) . . ? C1 N1 Gd1 110.9(3) . . ? C1 N1 H1C 109.5 . . ? Gd1 N1 H1C 109.5 . . ? C1 N1 H1D 109.5 . . ? Gd1 N1 H1D 109.5 . . ? H1C N1 H1D 108.1 . . ? C3 N2 C2 113.6(4) . . ? C3 N2 Gd1 114.4(3) . . ? C2 N2 Gd1 111.9(3) . . ? C3 N2 H2C 105.3 . . ? C2 N2 H2C 105.3 . . ? Gd1 N2 H2C 105.3 . . ? C4 N3 C5 115.9(3) . . ? C4 N3 Gd1 110.8(3) . . ? C5 N3 Gd1 110.4(2) . . ? C4 N3 H3C 106.4 . . ? C5 N3 H3C 106.4 . . ? Gd1 N3 H3C 106.4 . . ? C6 N4 C7 112.3(3) . . ? C6 N4 Gd1 116.7(3) . . ? C7 N4 Gd1 112.6(2) . . ? C6 N4 H4C 104.6 . . ? C7 N4 H4C 104.6 . . ? Gd1 N4 H4C 104.6 . . ? C9 N6 Gd2 115.0(3) . . ? C9 N6 H6C 108.5 . . ? Gd2 N6 H6C 108.5 . . ? C9 N6 H6D 108.5 . . ? Gd2 N6 H6D 108.5 . . ? H6C N6 H6D 107.5 . . ? C8 N5 Gd1 111.7(2) . . ? C8 N5 H5C 109.3 . . ? Gd1 N5 H5C 109.3 . . ? C8 N5 H5D 109.3 . . ? Gd1 N5 H5D 109.3 . . ? H5C N5 H5D 107.9 . . ? C11 N7 C10 117.1(4) . . ? C11 N7 Gd2 115.1(3) . . ? C10 N7 Gd2 111.2(3) . . ? C11 N7 H7C 103.8 . . ? C10 N7 H7C 103.8 . . ? Gd2 N7 H7C 103.8 . . ? C12 N8 C13 112.8(3) . . ? C12 N8 Gd2 110.4(3) . . ? C13 N8 Gd2 112.4(2) . . ? C12 N8 H8C 107.0 . . ? C13 N8 H8C 107.0 . . ? Gd2 N8 H8C 107.0 . . ? C14 N9 C15 111.9(3) . . ? C14 N9 Gd2 111.4(2) . . ? C15 N9 Gd2 112.3(2) . . ? C14 N9 H9C 106.9 . . ? C15 N9 H9C 106.9 . . ? Gd2 N9 H9C 106.9 . . ? C16 N10 Gd2 115.4(2) . . ? C16 N10 H10C 108.4 . . ? Gd2 N10 H10C 108.4 . . ? C16 N10 H10D 108.4 . . ? Gd2 N10 H10D 108.4 . . ? H10C N10 H10D 107.5 . . ? N1 C1 C2 109.2(4) . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C1 109.8(4) . . ? 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 . . ? N2 C3 C4 110.2(4) . . ? N2 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N2 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? N3 C4 C3 109.8(4) . . ? N3 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? N3 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? N3 C5 C6 109.1(4) . . ? N3 C5 H5A 109.9 . . ? C6 C5 H5A 109.9 . . ? N3 C5 H5B 109.9 . . ? C6 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? N4 C6 C5 110.9(3) . . ? N4 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? N4 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.0 . . ? N4 C7 C8 110.4(3) . . ? N4 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N4 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N5 C8 C7 110.6(4) . . ? N5 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? N5 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C10 C9 N6 116.7(5) . . ? C10 C9 H9A 108.1 . . ? N6 C9 H9A 108.1 . . ? C10 C9 H9B 108.1 . . ? N6 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? C9 C10 N7 114.3(5) . . ? C9 C10 H10A 108.7 . . ? N7 C10 H10A 108.7 . . ? C9 C10 H10B 108.7 . . ? N7 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? N7 C11 C12 109.0(4) . . ? N7 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? N7 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N8 C12 C11 110.7(4) . . ? N8 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? N8 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? N8 C13 C14 111.0(3) . . ? N8 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? N8 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? N9 C14 C13 109.4(3) . . ? N9 C14 H14A 109.8 . . ? C13 C14 H14A 109.8 . . ? N9 C14 H14B 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? N9 C15 C16 110.5(3) . . ? N9 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? N9 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? N10 C16 C15 108.8(3) . . ? N10 C16 H16A 109.9 . . ? C15 C16 H16A 109.9 . . ? N10 C16 H16B 109.9 . . ? C15 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Gd1 Gd2 O1 155.11(17) . . . . ? N4 Gd1 Gd2 O1 -118.35(16) . . . . ? N2 Gd1 Gd2 O1 106.43(16) . . . . ? N1 Gd1 Gd2 O1 35.17(16) . . . . ? N5 Gd1 Gd2 O1 -50.24(16) . . . . ? N3 Gd1 Gd2 O1 178.00(16) . . . . ? S3 Gd1 Gd2 O1 -102.60(18) . . . . ? O1 Gd1 Gd2 O2 -155.11(17) . . . . ? N4 Gd1 Gd2 O2 86.54(13) . . . . ? N2 Gd1 Gd2 O2 -48.68(14) . . . . ? N1 Gd1 Gd2 O2 -119.95(13) . . . . ? N5 Gd1 Gd2 O2 154.65(13) . . . . ? N3 Gd1 Gd2 O2 22.89(14) . . . . ? S3 Gd1 Gd2 O2 102.29(16) . . . . ? O1 Gd1 Gd2 N10 54.55(16) . . . . ? O2 Gd1 Gd2 N10 -150.33(13) . . . . ? N4 Gd1 Gd2 N10 -63.80(11) . . . . ? N2 Gd1 Gd2 N10 160.99(11) . . . . ? N1 Gd1 Gd2 N10 89.72(11) . . . . ? N5 Gd1 Gd2 N10 4.31(10) . . . . ? N3 Gd1 Gd2 N10 -127.45(11) . . . . ? S3 Gd1 Gd2 N10 -48.04(14) . . . . ? O1 Gd1 Gd2 N7 -89.61(16) . . . . ? O2 Gd1 Gd2 N7 65.50(13) . . . . ? N4 Gd1 Gd2 N7 152.04(11) . . . . ? N2 Gd1 Gd2 N7 16.82(12) . . . . ? N1 Gd1 Gd2 N7 -54.45(11) . . . . ? N5 Gd1 Gd2 N7 -139.85(11) . . . . ? N3 Gd1 Gd2 N7 88.39(12) . . . . ? S3 Gd1 Gd2 N7 167.79(14) . . . . ? O1 Gd1 Gd2 N6 -24.55(16) . . . . ? O2 Gd1 Gd2 N6 130.57(13) . . . . ? N4 Gd1 Gd2 N6 -142.90(11) . . . . ? N2 Gd1 Gd2 N6 81.89(12) . . . . ? N1 Gd1 Gd2 N6 10.62(11) . . . . ? N5 Gd1 Gd2 N6 -74.78(11) . . . . ? N3 Gd1 Gd2 N6 153.45(11) . . . . ? S3 Gd1 Gd2 N6 -127.14(14) . . . . ? O1 Gd1 Gd2 N9 91.8(3) . . . . ? O2 Gd1 Gd2 N9 -113.1(3) . . . . ? N4 Gd1 Gd2 N9 -26.6(3) . . . . ? N2 Gd1 Gd2 N9 -161.8(3) . . . . ? N1 Gd1 Gd2 N9 127.0(3) . . . . ? N5 Gd1 Gd2 N9 41.6(3) . . . . ? N3 Gd1 Gd2 N9 -90.2(3) . . . . ? S3 Gd1 Gd2 N9 -10.8(3) . . . . ? O1 Gd1 Gd2 N8 -153.18(17) . . . . ? O2 Gd1 Gd2 N8 1.93(14) . . . . ? N4 Gd1 Gd2 N8 88.47(12) . . . . ? N2 Gd1 Gd2 N8 -46.75(13) . . . . ? N1 Gd1 Gd2 N8 -118.01(13) . . . . ? N5 Gd1 Gd2 N8 156.58(12) . . . . ? N3 Gd1 Gd2 N8 24.82(13) . . . . ? S3 Gd1 Gd2 N8 104.22(15) . . . . ? O1 Gd1 Gd2 S1 136.68(14) . . . 2_655 ? O2 Gd1 Gd2 S1 -68.21(11) . . . 2_655 ? N4 Gd1 Gd2 S1 18.33(8) . . . 2_655 ? N2 Gd1 Gd2 S1 -116.89(9) . . . 2_655 ? N1 Gd1 Gd2 S1 171.85(8) . . . 2_655 ? N5 Gd1 Gd2 S1 86.44(8) . . . 2_655 ? N3 Gd1 Gd2 S1 -45.32(9) . . . 2_655 ? S3 Gd1 Gd2 S1 34.08(12) . . . 2_655 ? O2 Gd2 O1 Gd1 15.55(11) . . . . ? N10 Gd2 O1 Gd1 -125.76(14) . . . . ? N7 Gd2 O1 Gd1 90.87(14) . . . . ? N6 Gd2 O1 Gd1 156.30(15) . . . . ? N9 Gd2 O1 Gd1 -152.27(13) . . . . ? N8 Gd2 O1 Gd1 46.9(3) . . . . ? S1 Gd2 O1 Gd1 -45.62(14) 2_655 . . . ? O2 Gd1 O1 Gd2 -15.62(11) . . . . ? N4 Gd1 O1 Gd2 63.67(15) . . . . ? N2 Gd1 O1 Gd2 -85.16(15) . . . . ? N1 Gd1 O1 Gd2 -145.22(15) . . . . ? N5 Gd1 O1 Gd2 127.34(15) . . . . ? N3 Gd1 O1 Gd2 -3.1(3) . . . . ? S3 Gd1 O1 Gd2 163.17(5) . . . . ? O1 Gd2 O2 Gd1 -14.50(10) . . . . ? N10 Gd2 O2 Gd1 39.88(16) . . . . ? N7 Gd2 O2 Gd1 -110.77(13) . . . . ? N6 Gd2 O2 Gd1 -66.82(15) . . . . ? N9 Gd2 O2 Gd1 152.23(14) . . . . ? N8 Gd2 O2 Gd1 -178.32(12) . . . . ? S1 Gd2 O2 Gd1 103.99(10) 2_655 . . . ? O1 Gd1 O2 Gd2 14.31(10) . . . . ? N4 Gd1 O2 Gd2 -90.55(12) . . . . ? N2 Gd1 O2 Gd2 133.17(12) . . . . ? N1 Gd1 O2 Gd2 73.94(13) . . . . ? N5 Gd1 O2 Gd2 -32.28(16) . . . . ? N3 Gd1 O2 Gd2 -158.02(13) . . . . ? S3 Gd1 O2 Gd2 -164.58(4) . . . . ? S4 Sb1 S1 Gd2 154.69(5) . . . 2_645 ? S2 Sb1 S1 Gd2 -82.61(6) . . . 2_645 ? S3 Sb1 S1 Gd2 35.36(6) . . . 2_645 ? S4 Sb1 S3 Gd1 60.41(6) . . . . ? S2 Sb1 S3 Gd1 -64.07(5) . . . . ? S1 Sb1 S3 Gd1 179.07(4) . . . . ? O1 Gd1 S3 Sb1 10.29(16) . . . . ? O2 Gd1 S3 Sb1 -171.64(11) . . . . ? N4 Gd1 S3 Sb1 114.41(9) . . . . ? N2 Gd1 S3 Sb1 -109.47(9) . . . . ? N1 Gd1 S3 Sb1 -40.33(9) . . . . ? N5 Gd1 S3 Sb1 45.28(9) . . . . ? N3 Gd1 S3 Sb1 -178.52(10) . . . . ? Gd2 Gd1 S3 Sb1 98.63(11) . . . . ? O1 Gd1 N1 C1 101.7(3) . . . . ? O2 Gd1 N1 C1 47.4(3) . . . . ? N4 Gd1 N1 C1 -166.9(3) . . . . ? N2 Gd1 N1 C1 -18.7(3) . . . . ? N5 Gd1 N1 C1 177.0(3) . . . . ? N3 Gd1 N1 C1 -49.7(3) . . . . ? S3 Gd1 N1 C1 -102.9(3) . . . . ? Gd2 Gd1 N1 C1 83.2(3) . . . . ? O1 Gd1 N2 C3 150.3(3) . . . . ? O2 Gd1 N2 C3 89.6(3) . . . . ? N4 Gd1 N2 C3 15.5(3) . . . . ? N1 Gd1 N2 C3 -144.1(3) . . . . ? N5 Gd1 N2 C3 -113.0(3) . . . . ? N3 Gd1 N2 C3 10.4(3) . . . . ? S3 Gd1 N2 C3 -59.4(3) . . . . ? Gd2 Gd1 N2 C3 116.2(3) . . . . ? O1 Gd1 N2 C2 -78.6(3) . . . . ? O2 Gd1 N2 C2 -139.3(3) . . . . ? N4 Gd1 N2 C2 146.5(3) . . . . ? N1 Gd1 N2 C2 -13.1(3) . . . . ? N5 Gd1 N2 C2 18.1(4) . . . . ? N3 Gd1 N2 C2 141.4(3) . . . . ? S3 Gd1 N2 C2 71.7(3) . . . . ? Gd2 Gd1 N2 C2 -112.7(3) . . . . ? O1 Gd1 N3 C4 -77.6(3) . . . . ? O2 Gd1 N3 C4 -65.8(3) . . . . ? N4 Gd1 N3 C4 -155.8(3) . . . . ? N2 Gd1 N3 C4 20.2(3) . . . . ? N1 Gd1 N3 C4 51.5(3) . . . . ? N5 Gd1 N3 C4 167.6(3) . . . . ? S3 Gd1 N3 C4 110.1(3) . . . . ? Gd2 Gd1 N3 C4 -79.4(3) . . . . ? O1 Gd1 N3 C5 52.1(3) . . . . ? O2 Gd1 N3 C5 63.9(3) . . . . ? N4 Gd1 N3 C5 -26.1(3) . . . . ? N2 Gd1 N3 C5 150.0(3) . . . . ? N1 Gd1 N3 C5 -178.8(2) . . . . ? N5 Gd1 N3 C5 -62.7(3) . . . . ? S3 Gd1 N3 C5 -120.2(3) . . . . ? Gd2 Gd1 N3 C5 50.3(3) . . . . ? O1 Gd1 N4 C6 -146.0(3) . . . . ? O2 Gd1 N4 C6 -80.8(3) . . . . ? N2 Gd1 N4 C6 -8.0(4) . . . . ? N1 Gd1 N4 C6 128.7(3) . . . . ? N5 Gd1 N4 C6 146.0(3) . . . . ? N3 Gd1 N4 C6 -2.9(3) . . . . ? S3 Gd1 N4 C6 65.4(3) . . . . ? Gd2 Gd1 N4 C6 -117.0(3) . . . . ? O1 Gd1 N4 C7 82.0(3) . . . . ? O2 Gd1 N4 C7 147.2(3) . . . . ? N2 Gd1 N4 C7 -140.0(3) . . . . ? N1 Gd1 N4 C7 -3.3(4) . . . . ? N5 Gd1 N4 C7 14.0(3) . . . . ? N3 Gd1 N4 C7 -134.9(3) . . . . ? S3 Gd1 N4 C7 -66.6(3) . . . . ? Gd2 Gd1 N4 C7 111.0(3) . . . . ? O1 Gd2 N6 C9 -93.7(4) . . . . ? O2 Gd2 N6 C9 -45.2(4) . . . . ? N10 Gd2 N6 C9 -176.9(4) . . . . ? N7 Gd2 N6 C9 2.4(3) . . . . ? N9 Gd2 N6 C9 114.4(4) . . . . ? N8 Gd2 N6 C9 53.9(4) . . . . ? S1 Gd2 N6 C9 158.7(3) 2_655 . . . ? Gd1 Gd2 N6 C9 -80.1(3) . . . . ? O1 Gd1 N5 C8 -93.4(3) . . . . ? O2 Gd1 N5 C8 -49.4(3) . . . . ? N4 Gd1 N5 C8 16.1(3) . . . . ? N2 Gd1 N5 C8 159.1(3) . . . . ? N1 Gd1 N5 C8 -172.1(3) . . . . ? N3 Gd1 N5 C8 52.1(3) . . . . ? S3 Gd1 N5 C8 104.9(3) . . . . ? Gd2 Gd1 N5 C8 -67.8(3) . . . . ? O1 Gd2 N7 C11 -169.7(3) . . . . ? O2 Gd2 N7 C11 -102.8(3) . . . . ? N10 Gd2 N7 C11 114.9(3) . . . . ? N6 Gd2 N7 C11 113.6(3) . . . . ? N9 Gd2 N7 C11 43.3(3) . . . . ? N8 Gd2 N7 C11 -13.4(3) . . . . ? S1 Gd2 N7 C11 -54.5(4) 2_655 . . . ? Gd1 Gd2 N7 C11 -136.3(3) . . . . ? O1 Gd2 N7 C10 54.0(4) . . . . ? O2 Gd2 N7 C10 120.9(4) . . . . ? N10 Gd2 N7 C10 -21.4(4) . . . . ? N6 Gd2 N7 C10 -22.7(3) . . . . ? N9 Gd2 N7 C10 -93.0(4) . . . . ? N8 Gd2 N7 C10 -149.7(4) . . . . ? S1 Gd2 N7 C10 169.2(3) 2_655 . . . ? Gd1 Gd2 N7 C10 87.4(4) . . . . ? O1 Gd2 N8 C12 31.2(4) . . . . ? O2 Gd2 N8 C12 60.2(3) . . . . ? N10 Gd2 N8 C12 -158.4(3) . . . . ? N7 Gd2 N8 C12 -17.8(3) . . . . ? N6 Gd2 N8 C12 -68.9(3) . . . . ? N9 Gd2 N8 C12 -136.6(3) . . . . ? S1 Gd2 N8 C12 132.9(3) 2_655 . . . ? Gd1 Gd2 N8 C12 59.0(3) . . . . ? O1 Gd2 N8 C13 158.1(3) . . . . ? O2 Gd2 N8 C13 -172.9(3) . . . . ? N10 Gd2 N8 C13 -31.5(3) . . . . ? N7 Gd2 N8 C13 109.1(3) . . . . ? N6 Gd2 N8 C13 58.0(3) . . . . ? N9 Gd2 N8 C13 -9.7(3) . . . . ? S1 Gd2 N8 C13 -100.2(3) 2_655 . . . ? Gd1 Gd2 N8 C13 -174.1(2) . . . . ? O1 Gd2 N9 C14 169.7(2) . . . . ? O2 Gd2 N9 C14 10.8(4) . . . . ? N10 Gd2 N9 C14 141.1(3) . . . . ? N7 Gd2 N9 C14 -77.7(3) . . . . ? N6 Gd2 N9 C14 -139.1(3) . . . . ? N8 Gd2 N9 C14 -21.3(3) . . . . ? S1 Gd2 N9 C14 56.1(3) 2_655 . . . ? Gd1 Gd2 N9 C14 100.8(3) . . . . ? O1 Gd2 N9 C15 43.3(3) . . . . ? O2 Gd2 N9 C15 -115.7(3) . . . . ? N10 Gd2 N9 C15 14.7(2) . . . . ? N7 Gd2 N9 C15 155.8(2) . . . . ? N6 Gd2 N9 C15 94.5(3) . . . . ? N8 Gd2 N9 C15 -147.7(3) . . . . ? S1 Gd2 N9 C15 -70.3(2) 2_655 . . . ? Gd1 Gd2 N9 C15 -25.6(4) . . . . ? O1 Gd2 N10 C16 -147.2(3) . . . . ? O2 Gd2 N10 C16 163.2(2) . . . . ? N7 Gd2 N10 C16 -68.5(3) . . . . ? N6 Gd2 N10 C16 -67.3(3) . . . . ? N9 Gd2 N10 C16 16.2(2) . . . . ? N8 Gd2 N10 C16 38.0(3) . . . . ? S1 Gd2 N10 C16 103.8(3) 2_655 . . . ? Gd1 Gd2 N10 C16 -174.2(2) . . . . ? Gd1 N1 C1 C2 48.8(4) . . . . ? C3 N2 C2 C1 175.0(4) . . . . ? Gd1 N2 C2 C1 43.5(4) . . . . ? N1 C1 C2 N2 -62.6(5) . . . . ? C2 N2 C3 C4 -169.8(4) . . . . ? Gd1 N2 C3 C4 -39.6(4) . . . . ? C5 N3 C4 C3 -175.5(3) . . . . ? Gd1 N3 C4 C3 -48.7(4) . . . . ? N2 C3 C4 N3 59.4(5) . . . . ? C4 N3 C5 C6 179.2(3) . . . . ? Gd1 N3 C5 C6 52.2(4) . . . . ? C7 N4 C6 C5 163.2(4) . . . . ? Gd1 N4 C6 C5 31.1(5) . . . . ? N3 C5 C6 N4 -55.6(5) . . . . ? C6 N4 C7 C8 -176.6(4) . . . . ? Gd1 N4 C7 C8 -42.5(4) . . . . ? Gd1 N5 C8 C7 -44.6(4) . . . . ? N4 C7 C8 N5 58.9(5) . . . . ? Gd2 N6 C9 C10 21.3(7) . . . . ? N6 C9 C10 N7 -44.9(8) . . . . ? C11 N7 C10 C9 -90.5(6) . . . . ? Gd2 N7 C10 C9 44.9(6) . . . . ? C10 N7 C11 C12 176.2(4) . . . . ? Gd2 N7 C11 C12 42.6(5) . . . . ? C13 N8 C12 C11 -79.4(5) . . . . ? Gd2 N8 C12 C11 47.2(4) . . . . ? N7 C11 C12 N8 -60.5(5) . . . . ? C12 N8 C13 C14 165.2(4) . . . . ? Gd2 N8 C13 C14 39.6(4) . . . . ? C15 N9 C14 C13 176.9(3) . . . . ? Gd2 N9 C14 C13 50.3(4) . . . . ? N8 C13 C14 N9 -61.0(5) . . . . ? C14 N9 C15 C16 -169.4(3) . . . . ? Gd2 N9 C15 C16 -43.2(4) . . . . ? Gd2 N10 C16 C15 -44.3(4) . . . . ? N9 C15 C16 N10 57.9(4) . . . . ? 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 N1 H1C S4 0.90 2.55 3.434(3) 167.1 . N1 H1D S2 0.90 2.66 3.547(3) 170.8 3_666 N2 H2C Cl1 0.91 2.41 3.279(4) 159.5 . N3 H3C S3 0.91 2.57 3.123(3) 120.1 . N4 H4C S1 0.91 2.55 3.415(4) 159.6 2_655 N6 H6C S2 0.90 2.74 3.575(4) 154.5 3_666 N6 H6D Cl1 0.90 2.54 3.378(3) 155.1 2 N5 H5D S2 0.90 2.56 3.441(3) 166.5 . N7 H7C Cl1 0.91 2.59 3.399(4) 148.8 . N8 H8C O3W 0.91 2.39 3.138(15) 140.0 . N8 H8C S1 0.91 3.00 3.451(4) 112.2 2_655 N9 H9C Cl1 0.91 2.51 3.398(4) 165.8 2 N10 H10C S4 0.90 2.71 3.485(4) 144.6 3_666 N10 H10D S3 0.90 2.59 3.476(3) 167.5 2_655 O2 H2 O3W 0.89(4) 2.35(5) 3.043(14) 135(4) . O1 H1 S2 0.96(4) 2.32(4) 3.221(3) 157(4) 3_666 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.453 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.078