# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jie Zhang' _publ_contact_author_email ZHANGJIE@FUDAN.EDU.CN _publ_section_title ; Facile Construction of the Guanidine Substituent or Guanidinate Anionic Ligands through Addition of the Adjacent Amino Group to Carbodiimide ; loop_ _publ_author_name 'Jie Zhang' 'Fuyan Han Ruifang Cai' 'Zhenxia Chen' 'Yanan Han' ; Liping Ma ; 'Xigeng Zhou' # Attachment 'complex 6.cif' data_f50516a _database_code_depnum_ccdc_archive 'CCDC 609334' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H56 N4 O2 S2 Y2' _chemical_formula_weight 890.85 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.520(4) _cell_length_b 19.120(5) _cell_length_c 30.856(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.055(4) _cell_angle_gamma 90.00 _cell_volume 8518(4) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 855 _cell_measurement_theta_min 2.549 _cell_measurement_theta_max 19.994 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 2.848 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5997 _exptl_absorpt_correction_T_max 0.7638 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.85 _diffrn_reflns_number 17785 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.0951 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7524 _reflns_number_gt 4425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^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 7524 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1125 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1087 _refine_ls_wR_factor_gt 0.0918 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _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 Y1 Y 0.22622(3) 0.31706(2) 0.138343(16) 0.03841(15) Uani 1 1 d . . . Y2 Y 0.05526(3) 0.14869(3) 0.083891(17) 0.04719(16) Uani 1 1 d . . . S1 S 0.05387(8) 0.25249(6) 0.14848(4) 0.0418(3) Uani 1 1 d . . . S2 S 0.24373(8) 0.19496(7) 0.09114(4) 0.0472(3) Uani 1 1 d . . . N1 N -0.1059(2) 0.1775(2) 0.10518(13) 0.0488(11) Uani 1 1 d . . . H1B H -0.1481 0.1609 0.0842 0.059 Uiso 1 1 calc R . . H1C H -0.1137 0.1543 0.1299 0.059 Uiso 1 1 calc R . . N2 N 0.2672(2) 0.22591(19) 0.18486(13) 0.0407(10) Uani 1 1 d . . . N3 N 0.2661(3) 0.2295(2) 0.26238(13) 0.0531(11) Uani 1 1 d . . . H3B H 0.2923 0.2516 0.2847 0.064 Uiso 1 1 calc R . . N4 N 0.2477(3) 0.3295(2) 0.21578(13) 0.0420(10) Uani 1 1 d . . . O1 O 0.3935(2) 0.32194(18) 0.14206(12) 0.0571(10) Uani 1 1 d . . . C1 C 0.2422(4) 0.4519(3) 0.1193(2) 0.0618(16) Uani 1 1 d . . . H1A H 0.2818 0.4855 0.1365 0.074 Uiso 1 1 calc R . . C2 C 0.1496(4) 0.4417(3) 0.1225(2) 0.0674(18) Uani 1 1 d . . . H2A H 0.1126 0.4672 0.1421 0.081 Uiso 1 1 calc R . . C3 C 0.1143(4) 0.4006(3) 0.0873(2) 0.0720(19) Uani 1 1 d . . . H3A H 0.0485 0.3921 0.0783 0.086 Uiso 1 1 calc R . . C4 C 0.1876(5) 0.3839(3) 0.0628(2) 0.0662(17) Uani 1 1 d . . . H4A H 0.1815 0.3622 0.0339 0.079 Uiso 1 1 calc R . . C5 C 0.2661(4) 0.4164(3) 0.0826(2) 0.0598(16) Uani 1 1 d . . . H5A H 0.3250 0.4211 0.0700 0.072 Uiso 1 1 calc R . . C6 C -0.0551(3) 0.2914(3) 0.13254(16) 0.0406(12) Uani 1 1 d . . . C7 C -0.0758(3) 0.3597(3) 0.14129(17) 0.0512(14) Uani 1 1 d . . . H7A H -0.0308 0.3876 0.1564 0.061 Uiso 1 1 calc R . . C8 C -0.1618(4) 0.3881(3) 0.1282(2) 0.0637(17) Uani 1 1 d . . . H8A H -0.1741 0.4345 0.1346 0.076 Uiso 1 1 calc R . . C9 C -0.2292(4) 0.3476(3) 0.1059(2) 0.0640(17) Uani 1 1 d . . . H9A H -0.2866 0.3666 0.0960 0.077 Uiso 1 1 calc R . . C10 C -0.2103(4) 0.2789(3) 0.09832(18) 0.0602(16) Uani 1 1 d . . . H10A H -0.2560 0.2510 0.0837 0.072 Uiso 1 1 calc R . . C11 C -0.1256(3) 0.2503(3) 0.11183(17) 0.0454(13) Uani 1 1 d . . . C12 C 0.3179(3) 0.1504(2) 0.13186(18) 0.0463(13) Uani 1 1 d . . . C13 C 0.3758(4) 0.0986(3) 0.1186(2) 0.0622(16) Uani 1 1 d . . . H13A H 0.3713 0.0852 0.0894 0.075 Uiso 1 1 calc R . . C14 C 0.4400(4) 0.0669(3) 0.1486(2) 0.0703(19) Uani 1 1 d . . . H14A H 0.4776 0.0315 0.1396 0.084 Uiso 1 1 calc R . . C15 C 0.4486(4) 0.0872(3) 0.1914(2) 0.0675(17) Uani 1 1 d . . . H15A H 0.4924 0.0660 0.2114 0.081 Uiso 1 1 calc R . . C16 C 0.3918(3) 0.1394(2) 0.20481(18) 0.0509(14) Uani 1 1 d . . . H16A H 0.3987 0.1534 0.2338 0.061 Uiso 1 1 calc R . . C17 C 0.3250(3) 0.1712(2) 0.17615(17) 0.0427(13) Uani 1 1 d . . . C18 C 0.2611(3) 0.2617(3) 0.22210(17) 0.0411(12) Uani 1 1 d . . . C19 C 0.2290(4) 0.1599(3) 0.26874(17) 0.0540(15) Uani 1 1 d . . . H19A H 0.2473 0.1291 0.2457 0.065 Uiso 1 1 calc R . . C20 C 0.1252(4) 0.1616(3) 0.2660(2) 0.0793(19) Uani 1 1 d . . . H20A H 0.1007 0.1781 0.2377 0.119 Uiso 1 1 calc R . . H20B H 0.1063 0.1925 0.2879 0.119 Uiso 1 1 calc R . . H20C H 0.1023 0.1154 0.2705 0.119 Uiso 1 1 calc R . . C21 C 0.2721(4) 0.1328(3) 0.31217(19) 0.0731(18) Uani 1 1 d . . . H21A H 0.3382 0.1322 0.3125 0.110 Uiso 1 1 calc R . . H21B H 0.2502 0.0863 0.3166 0.110 Uiso 1 1 calc R . . H21C H 0.2551 0.1628 0.3350 0.110 Uiso 1 1 calc R . . C22 C 0.2232(4) 0.3768(3) 0.25010(17) 0.0522(14) Uani 1 1 d . . . H22A H 0.2406 0.3542 0.2783 0.063 Uiso 1 1 calc R . . C23 C 0.1212(4) 0.3892(4) 0.2458(2) 0.110(3) Uani 1 1 d . . . H23A H 0.0895 0.3453 0.2471 0.165 Uiso 1 1 calc R . . H23B H 0.1026 0.4115 0.2184 0.165 Uiso 1 1 calc R . . H23C H 0.1059 0.4187 0.2692 0.165 Uiso 1 1 calc R . . C24 C 0.2754(5) 0.4432(3) 0.2494(2) 0.109(3) Uani 1 1 d . . . H24A H 0.3406 0.4335 0.2526 0.163 Uiso 1 1 calc R . . H24B H 0.2604 0.4726 0.2729 0.163 Uiso 1 1 calc R . . H24C H 0.2590 0.4666 0.2221 0.163 Uiso 1 1 calc R . . C25 C 0.0242(7) 0.2377(4) 0.0170(2) 0.103(3) Uani 1 1 d . . . H25A H 0.0241 0.2888 0.0196 0.124 Uiso 1 1 calc R . . C26 C -0.0528(5) 0.1967(5) 0.0138(2) 0.089(2) Uani 1 1 d . . . H26A H -0.1166 0.2133 0.0137 0.107 Uiso 1 1 calc R . . C27 C -0.0273(5) 0.1304(4) 0.0047(2) 0.092(2) Uani 1 1 d . . . H27A H -0.0701 0.0922 -0.0042 0.111 Uiso 1 1 calc R . . C28 C 0.0666(7) 0.1299(6) 0.0008(2) 0.117(3) Uani 1 1 d . . . H28A H 0.1006 0.0922 -0.0121 0.140 Uiso 1 1 calc R . . C29 C 0.0984(6) 0.1985(7) 0.0083(2) 0.123(4) Uani 1 1 d . . . H29A H 0.1590 0.2166 0.0026 0.148 Uiso 1 1 calc R . . C30 C 0.0350(7) 0.0552(3) 0.1461(3) 0.091(2) Uani 1 1 d . . . H30A H 0.0082 0.0647 0.1734 0.109 Uiso 1 1 calc R . . C31 C 0.1269(6) 0.0549(3) 0.1413(3) 0.088(2) Uani 1 1 d . . . H31A H 0.1769 0.0638 0.1646 0.106 Uiso 1 1 calc R . . C32 C 0.1381(6) 0.0279(4) 0.1016(4) 0.100(3) Uani 1 1 d . . . H32A H 0.1972 0.0134 0.0918 0.120 Uiso 1 1 calc R . . C33 C 0.0524(8) 0.0109(3) 0.0819(3) 0.111(3) Uani 1 1 d . . . H33A H 0.0407 -0.0175 0.0554 0.133 Uiso 1 1 calc R . . C34 C -0.0125(5) 0.0283(4) 0.1089(4) 0.093(3) Uani 1 1 d . . . H34A H -0.0778 0.0143 0.1053 0.112 Uiso 1 1 calc R . . C35 C 0.4518(4) 0.2979(4) 0.1103(2) 0.091(2) Uani 1 1 d . . . H35A H 0.4247 0.2573 0.0951 0.109 Uiso 1 1 calc R . . H35B H 0.4598 0.3343 0.0892 0.109 Uiso 1 1 calc R . . C36 C 0.5367(5) 0.2807(5) 0.1334(4) 0.164(5) Uani 1 1 d . . . H36A H 0.5869 0.2886 0.1155 0.196 Uiso 1 1 calc R . . H36B H 0.5374 0.2319 0.1420 0.196 Uiso 1 1 calc R . . C37 C 0.5466(5) 0.3251(5) 0.1710(3) 0.149(4) Uani 1 1 d . . . H37A H 0.5821 0.3666 0.1655 0.178 Uiso 1 1 calc R . . H37B H 0.5777 0.3005 0.1959 0.178 Uiso 1 1 calc R . . C38 C 0.4534(4) 0.3436(4) 0.1787(2) 0.098(2) Uani 1 1 d . . . H38A H 0.4368 0.3205 0.2047 0.117 Uiso 1 1 calc R . . H38B H 0.4486 0.3937 0.1827 0.117 Uiso 1 1 calc R . . C39 C 0.7219(6) 0.0837(5) 0.0103(3) 0.136(3) Uani 1 1 d . . . H39A H 0.7574 0.0409 0.0151 0.164 Uiso 1 1 calc R . . H39B H 0.7500 0.1115 -0.0111 0.164 Uiso 1 1 calc R . . C40 C 0.6266(6) 0.0670(5) -0.0060(3) 0.142(4) Uani 1 1 d . . . H40A H 0.6049 0.0978 -0.0299 0.171 Uiso 1 1 calc R . . H40B H 0.6220 0.0191 -0.0163 0.171 Uiso 1 1 calc R . . C41 C 0.5716(5) 0.0767(4) 0.0304(3) 0.113(3) Uani 1 1 d . . . H41A H 0.5564 0.0322 0.0429 0.135 Uiso 1 1 calc R . . H41B H 0.5148 0.1020 0.0214 0.135 Uiso 1 1 calc R . . C42 C 0.6342(6) 0.1183(4) 0.0615(3) 0.117(3) Uani 1 1 d . . . H42A H 0.6107 0.1656 0.0630 0.141 Uiso 1 1 calc R . . H42B H 0.6365 0.0977 0.0903 0.141 Uiso 1 1 calc R . . O2 O 0.7230(4) 0.1196(3) 0.0480(2) 0.1111(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0343(3) 0.0377(3) 0.0433(3) 0.0013(2) 0.0043(2) 0.0014(2) Y2 0.0438(3) 0.0490(3) 0.0496(4) -0.0132(3) 0.0087(2) -0.0061(2) S1 0.0344(7) 0.0418(8) 0.0491(9) -0.0065(6) 0.0038(6) -0.0017(6) S2 0.0406(8) 0.0523(9) 0.0495(9) -0.0079(7) 0.0085(6) 0.0019(6) N1 0.039(2) 0.055(3) 0.052(3) -0.003(2) 0.005(2) -0.011(2) N2 0.044(2) 0.037(2) 0.042(3) -0.001(2) 0.004(2) 0.0045(19) N3 0.070(3) 0.052(3) 0.035(3) 0.004(2) -0.006(2) -0.007(2) N4 0.044(2) 0.038(3) 0.043(3) -0.005(2) 0.004(2) 0.0011(19) O1 0.036(2) 0.078(3) 0.058(3) 0.004(2) 0.0058(19) -0.0010(18) C1 0.068(4) 0.040(3) 0.080(5) 0.002(3) 0.019(4) -0.002(3) C2 0.064(4) 0.048(4) 0.094(6) 0.019(4) 0.028(4) 0.019(3) C3 0.038(4) 0.079(5) 0.096(6) 0.044(4) -0.006(4) 0.004(3) C4 0.084(5) 0.060(4) 0.051(4) 0.022(3) -0.008(4) -0.008(4) C5 0.060(4) 0.052(4) 0.070(4) 0.022(3) 0.019(3) -0.006(3) C6 0.033(3) 0.043(3) 0.048(3) 0.004(2) 0.013(2) 0.005(2) C7 0.039(3) 0.052(4) 0.064(4) -0.005(3) 0.012(3) 0.000(3) C8 0.054(4) 0.046(4) 0.094(5) 0.006(3) 0.018(4) 0.011(3) C9 0.037(3) 0.060(4) 0.096(5) 0.006(4) 0.010(3) 0.008(3) C10 0.039(3) 0.065(4) 0.075(4) -0.005(3) 0.002(3) -0.005(3) C11 0.040(3) 0.038(3) 0.060(4) 0.005(3) 0.015(3) 0.000(3) C12 0.030(3) 0.044(3) 0.065(4) -0.007(3) 0.009(3) -0.001(2) C13 0.051(4) 0.061(4) 0.076(5) -0.020(3) 0.012(3) 0.002(3) C14 0.046(4) 0.050(4) 0.115(6) -0.014(4) 0.008(4) 0.018(3) C15 0.051(4) 0.060(4) 0.090(5) 0.007(4) -0.005(4) 0.011(3) C16 0.045(3) 0.045(3) 0.062(4) 0.005(3) 0.005(3) 0.010(3) C17 0.033(3) 0.040(3) 0.056(4) 0.001(3) 0.007(3) 0.003(2) C18 0.023(3) 0.052(4) 0.047(4) -0.002(3) 0.000(2) -0.001(2) C19 0.062(4) 0.050(4) 0.052(4) 0.003(3) 0.011(3) 0.000(3) C20 0.056(4) 0.096(5) 0.087(5) 0.014(4) 0.012(4) -0.008(3) C21 0.084(4) 0.069(4) 0.066(5) 0.025(3) 0.010(4) 0.010(3) C22 0.064(4) 0.046(3) 0.045(4) -0.010(3) 0.001(3) 0.007(3) C23 0.077(5) 0.155(7) 0.100(6) -0.058(5) 0.016(4) 0.036(5) C24 0.160(7) 0.059(5) 0.112(6) -0.039(4) 0.031(5) -0.029(5) C25 0.131(8) 0.113(7) 0.059(5) 0.026(4) -0.026(5) -0.046(6) C26 0.081(5) 0.141(8) 0.043(4) -0.001(4) -0.008(4) 0.010(5) C27 0.083(6) 0.117(7) 0.075(5) -0.043(5) -0.007(4) -0.023(5) C28 0.100(7) 0.200(10) 0.053(5) -0.046(6) 0.017(5) 0.022(7) C29 0.063(6) 0.256(14) 0.050(5) 0.025(6) 0.002(4) -0.052(7) C30 0.119(7) 0.050(4) 0.113(7) 0.015(4) 0.060(6) 0.009(4) C31 0.081(6) 0.055(5) 0.125(8) 0.025(5) -0.012(5) -0.002(4) C32 0.097(7) 0.051(5) 0.161(9) -0.002(5) 0.054(6) 0.024(4) C33 0.155(8) 0.045(4) 0.132(8) -0.039(4) 0.010(7) -0.014(5) C34 0.069(5) 0.052(5) 0.159(9) -0.001(5) 0.014(6) -0.025(4) C35 0.053(4) 0.130(6) 0.095(6) -0.013(4) 0.032(4) -0.012(4) C36 0.046(5) 0.196(10) 0.251(13) -0.101(9) 0.023(6) 0.021(5) C37 0.056(5) 0.214(11) 0.168(10) -0.040(8) -0.026(6) 0.009(6) C38 0.048(4) 0.146(7) 0.097(6) -0.018(5) -0.003(4) -0.016(4) C39 0.114(8) 0.167(9) 0.125(9) -0.007(7) -0.004(6) -0.046(6) C40 0.109(7) 0.194(10) 0.119(9) -0.031(7) -0.013(6) -0.053(7) C41 0.102(6) 0.102(6) 0.127(8) 0.017(5) -0.021(6) -0.024(5) C42 0.124(7) 0.112(7) 0.112(8) -0.015(5) -0.006(6) -0.018(6) O2 0.086(4) 0.114(4) 0.127(5) -0.017(4) -0.018(4) -0.035(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 Y1 N2 2.296(4) . ? Y1 N4 2.389(4) . ? Y1 O1 2.422(3) . ? Y1 C2 2.654(5) . ? Y1 C1 2.659(5) . ? Y1 C4 2.665(5) . ? Y1 C5 2.667(5) . ? Y1 C3 2.670(5) . ? Y1 S2 2.7774(14) . ? Y1 C18 2.789(5) . ? Y1 S1 2.8372(14) . ? Y2 N1 2.557(4) . ? Y2 C28 2.612(7) . ? Y2 C27 2.629(6) . ? Y2 C32 2.634(7) . ? Y2 C33 2.636(6) . ? Y2 C34 2.650(6) . ? Y2 C29 2.653(7) . ? Y2 C31 2.655(6) . ? Y2 C30 2.663(6) . ? Y2 C25 2.676(7) . ? Y2 C26 2.696(6) . ? Y2 S1 2.8142(14) . ? S1 C6 1.770(5) . ? S2 C12 1.783(5) . ? N1 C11 1.441(5) . ? N1 H1B 0.9000 . ? N1 H1C 0.9000 . ? N2 C18 1.348(6) . ? N2 C17 1.385(5) . ? N3 C18 1.382(6) . ? N3 C19 1.457(6) . ? N3 H3B 0.8600 . ? N4 C18 1.322(6) . ? N4 C22 1.465(6) . ? O1 C38 1.412(7) . ? O1 C35 1.435(6) . ? C1 C2 1.373(7) . ? C1 C5 1.395(7) . ? C1 H1A 0.9800 . ? C2 C3 1.395(8) . ? C2 H2A 0.9800 . ? C3 C4 1.406(8) . ? C3 H3A 0.9800 . ? C4 C5 1.383(7) . ? C4 H4A 0.9800 . ? C5 H5A 0.9800 . ? C6 C7 1.373(6) . ? C6 C11 1.392(6) . ? C7 C8 1.382(7) . ? C7 H7A 0.9300 . ? C8 C9 1.374(7) . ? C8 H8A 0.9300 . ? C9 C10 1.367(7) . ? C9 H9A 0.9300 . ? C10 C11 1.370(6) . ? C10 H10A 0.9300 . ? C12 C13 1.389(6) . ? C12 C17 1.417(7) . ? C13 C14 1.383(8) . ? C13 H13A 0.9300 . ? C14 C15 1.371(8) . ? C14 H14A 0.9300 . ? C15 C16 1.387(7) . ? C15 H15A 0.9300 . ? C16 C17 1.382(6) . ? C16 H16A 0.9300 . ? C19 C20 1.501(7) . ? C19 C21 1.509(7) . ? C19 H19A 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C24 1.479(7) . ? C22 C23 1.492(7) . ? C22 H22A 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.360(9) . ? C25 C29 1.362(11) . ? C25 H25A 0.9800 . ? C26 C27 1.358(9) . ? C26 H26A 0.9800 . ? C27 C28 1.381(9) . ? C27 H27A 0.9800 . ? C28 C29 1.402(11) . ? C28 H28A 0.9800 . ? C29 H29A 0.9800 . ? C30 C31 1.359(8) . ? C30 C34 1.376(9) . ? C30 H30A 0.9800 . ? C31 C32 1.354(9) . ? C31 H31A 0.9800 . ? C32 C33 1.366(10) . ? C32 H32A 0.9800 . ? C33 C34 1.363(9) . ? C33 H33A 0.9800 . ? C34 H34A 0.9800 . ? C35 C36 1.397(9) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.433(10) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.443(8) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 O2 1.350(9) . ? C39 C40 1.458(10) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.456(10) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.482(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 O2 1.397(8) . ? C42 H42A 0.9700 . ? C42 H42B 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 Y1 N4 56.80(13) . . ? N2 Y1 O1 78.89(12) . . ? N4 Y1 O1 85.64(12) . . ? N2 Y1 C2 150.76(17) . . ? N4 Y1 C2 95.87(18) . . ? O1 Y1 C2 111.90(16) . . ? N2 Y1 C1 148.30(17) . . ? N4 Y1 C1 96.83(16) . . ? O1 Y1 C1 82.09(15) . . ? C2 Y1 C1 29.95(15) . . ? N2 Y1 C4 158.01(17) . . ? N4 Y1 C4 145.12(16) . . ? O1 Y1 C4 98.06(17) . . ? C2 Y1 C4 50.47(19) . . ? C1 Y1 C4 50.04(18) . . ? N2 Y1 C5 152.17(15) . . ? N4 Y1 C5 124.03(17) . . ? O1 Y1 C5 73.63(15) . . ? C2 Y1 C5 49.98(17) . . ? C1 Y1 C5 30.37(15) . . ? C4 Y1 C5 30.06(15) . . ? N2 Y1 C3 157.53(15) . . ? N4 Y1 C3 122.5(2) . . ? O1 Y1 C3 123.35(15) . . ? C2 Y1 C3 30.37(17) . . ? C1 Y1 C3 49.61(18) . . ? C4 Y1 C3 30.56(17) . . ? C5 Y1 C3 49.73(17) . . ? N2 Y1 S2 69.99(10) . . ? N4 Y1 S2 126.78(10) . . ? O1 Y1 S2 84.86(9) . . ? C2 Y1 S2 135.93(17) . . ? C1 Y1 S2 133.16(14) . . ? C4 Y1 S2 88.08(14) . . ? C5 Y1 S2 102.86(14) . . ? C3 Y1 S2 106.09(18) . . ? N2 Y1 C18 28.71(13) . . ? N4 Y1 C18 28.26(12) . . ? O1 Y1 C18 83.55(12) . . ? C2 Y1 C18 122.86(18) . . ? C1 Y1 C18 124.11(17) . . ? C4 Y1 C18 173.27(17) . . ? C5 Y1 C18 146.86(17) . . ? C3 Y1 C18 144.40(18) . . ? S2 Y1 C18 98.58(11) . . ? N2 Y1 S1 76.94(9) . . ? N4 Y1 S1 87.53(9) . . ? O1 Y1 S1 154.63(9) . . ? C2 Y1 S1 93.08(14) . . ? C1 Y1 S1 123.02(13) . . ? C4 Y1 S1 101.45(14) . . ? C5 Y1 S1 129.43(13) . . ? C3 Y1 S1 80.59(13) . . ? S2 Y1 S1 79.78(4) . . ? C18 Y1 S1 78.97(9) . . ? N1 Y2 C28 115.8(2) . . ? N1 Y2 C27 85.9(2) . . ? C28 Y2 C27 30.5(2) . . ? N1 Y2 C32 123.07(18) . . ? C28 Y2 C32 90.5(3) . . ? C27 Y2 C32 103.3(3) . . ? N1 Y2 C33 102.1(3) . . ? C28 Y2 C33 80.9(3) . . ? C27 Y2 C33 80.8(3) . . ? C32 Y2 C33 30.0(2) . . ? N1 Y2 C34 74.6(2) . . ? C28 Y2 C34 103.3(4) . . ? C27 Y2 C34 90.4(3) . . ? C32 Y2 C34 49.7(2) . . ? C33 Y2 C34 29.9(2) . . ? N1 Y2 C29 117.1(3) . . ? C28 Y2 C29 30.9(2) . . ? C27 Y2 C29 50.1(2) . . ? C32 Y2 C29 110.6(4) . . ? C33 Y2 C29 110.1(4) . . ? C34 Y2 C29 134.2(4) . . ? N1 Y2 C31 106.2(2) . . ? C28 Y2 C31 120.1(3) . . ? C27 Y2 C31 129.7(3) . . ? C32 Y2 C31 29.7(2) . . ? C33 Y2 C31 49.0(2) . . ? C34 Y2 C31 49.5(2) . . ? C29 Y2 C31 135.8(3) . . ? N1 Y2 C30 77.6(2) . . ? C28 Y2 C30 129.7(3) . . ? C27 Y2 C30 120.4(3) . . ? C32 Y2 C30 49.0(2) . . ? C33 Y2 C30 48.9(2) . . ? C34 Y2 C30 30.0(2) . . ? C29 Y2 C30 158.3(3) . . ? C31 Y2 C30 29.62(19) . . ? N1 Y2 C25 88.7(3) . . ? C28 Y2 C25 49.7(3) . . ? C27 Y2 C25 49.1(2) . . ? C32 Y2 C25 138.9(3) . . ? C33 Y2 C25 128.1(3) . . ? C34 Y2 C25 137.7(3) . . ? C29 Y2 C25 29.6(2) . . ? C31 Y2 C25 165.1(3) . . ? C30 Y2 C25 163.9(3) . . ? N1 Y2 C26 70.24(18) . . ? C28 Y2 C26 49.5(2) . . ? C27 Y2 C26 29.52(19) . . ? C32 Y2 C26 132.8(3) . . ? C33 Y2 C26 108.4(3) . . ? C34 Y2 C26 109.1(3) . . ? C29 Y2 C26 49.0(2) . . ? C31 Y2 C26 156.8(3) . . ? C30 Y2 C26 135.1(3) . . ? C25 Y2 C26 29.34(19) . . ? N1 Y2 S1 65.86(9) . . ? C28 Y2 S1 143.0(2) . . ? C27 Y2 S1 135.7(2) . . ? C32 Y2 S1 120.5(3) . . ? C33 Y2 S1 136.1(2) . . ? C34 Y2 S1 112.1(2) . . ? C29 Y2 S1 112.9(3) . . ? C31 Y2 S1 92.0(2) . . ? C30 Y2 S1 87.31(18) . . ? C25 Y2 S1 94.85(19) . . ? C26 Y2 S1 106.35(19) . . ? C6 S1 Y2 99.95(17) . . ? C6 S1 Y1 123.99(16) . . ? Y2 S1 Y1 99.00(4) . . ? C12 S2 Y1 96.53(17) . . ? C12 S2 Y2 114.17(16) . . ? Y1 S2 Y2 99.28(4) . . ? C11 N1 Y2 116.5(3) . . ? C11 N1 H1B 108.2 . . ? Y2 N1 H1B 108.2 . . ? C11 N1 H1C 108.2 . . ? Y2 N1 H1C 108.2 . . ? H1B N1 H1C 107.3 . . ? C18 N2 C17 130.1(4) . . ? C18 N2 Y1 96.4(3) . . ? C17 N2 Y1 125.1(3) . . ? C18 N3 C19 122.9(4) . . ? C18 N3 H3B 118.6 . . ? C19 N3 H3B 118.6 . . ? C18 N4 C22 122.8(4) . . ? C18 N4 Y1 92.9(3) . . ? C22 N4 Y1 140.2(3) . . ? C38 O1 C35 106.4(4) . . ? C38 O1 Y1 125.4(3) . . ? C35 O1 Y1 128.0(3) . . ? C2 C1 C5 108.6(6) . . ? C2 C1 Y1 74.8(3) . . ? C5 C1 Y1 75.1(3) . . ? C2 C1 H1A 125.2 . . ? C5 C1 H1A 125.2 . . ? Y1 C1 H1A 125.2 . . ? C1 C2 C3 107.8(6) . . ? C1 C2 Y1 75.3(3) . . ? C3 C2 Y1 75.5(3) . . ? C1 C2 H2A 125.5 . . ? C3 C2 H2A 125.5 . . ? Y1 C2 H2A 125.5 . . ? C2 C3 C4 108.1(5) . . ? C2 C3 Y1 74.2(3) . . ? C4 C3 Y1 74.5(3) . . ? C2 C3 H3A 125.5 . . ? C4 C3 H3A 125.5 . . ? Y1 C3 H3A 125.5 . . ? C5 C4 C3 107.1(6) . . ? C5 C4 Y1 75.0(3) . . ? C3 C4 Y1 74.9(3) . . ? C5 C4 H4A 125.8 . . ? C3 C4 H4A 125.8 . . ? Y1 C4 H4A 125.8 . . ? C4 C5 C1 108.3(5) . . ? C4 C5 Y1 74.9(3) . . ? C1 C5 Y1 74.5(3) . . ? C4 C5 H5A 125.4 . . ? C1 C5 H5A 125.4 . . ? Y1 C5 H5A 125.4 . . ? C7 C6 C11 117.4(4) . . ? C7 C6 S1 123.6(4) . . ? C11 C6 S1 118.9(4) . . ? C6 C7 C8 121.7(5) . . ? C6 C7 H7A 119.1 . . ? C8 C7 H7A 119.1 . . ? C9 C8 C7 119.9(5) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C10 C9 C8 118.8(5) . . ? C10 C9 H9A 120.6 . . ? C8 C9 H9A 120.6 . . ? C9 C10 C11 121.4(5) . . ? C9 C10 H10A 119.3 . . ? C11 C10 H10A 119.3 . . ? C10 C11 C6 120.6(5) . . ? C10 C11 N1 121.8(5) . . ? C6 C11 N1 117.6(4) . . ? C13 C12 C17 120.1(5) . . ? C13 C12 S2 118.2(4) . . ? C17 C12 S2 121.5(4) . . ? C14 C13 C12 120.1(6) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C15 C14 C13 120.6(5) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C14 C15 C16 119.6(5) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C17 C16 C15 121.7(5) . . ? C17 C16 H16A 119.2 . . ? C15 C16 H16A 119.2 . . ? C16 C17 N2 127.3(5) . . ? C16 C17 C12 117.9(5) . . ? N2 C17 C12 114.5(4) . . ? N4 C18 N2 113.2(4) . . ? N4 C18 N3 124.2(5) . . ? N2 C18 N3 122.6(5) . . ? N4 C18 Y1 58.8(3) . . ? N2 C18 Y1 54.9(2) . . ? N3 C18 Y1 171.7(3) . . ? N3 C19 C20 110.8(4) . . ? N3 C19 C21 108.0(4) . . ? C20 C19 C21 112.2(5) . . ? N3 C19 H19A 108.6 . . ? C20 C19 H19A 108.6 . . ? C21 C19 H19A 108.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 C24 110.8(5) . . ? N4 C22 C23 110.4(4) . . ? C24 C22 C23 111.6(5) . . ? N4 C22 H22A 108.0 . . ? C24 C22 H22A 108.0 . . ? C23 C22 H22A 108.0 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C29 109.2(8) . . ? C26 C25 Y2 76.1(4) . . ? C29 C25 Y2 74.3(5) . . ? C26 C25 H25A 124.9 . . ? C29 C25 H25A 124.9 . . ? Y2 C25 H25A 124.9 . . ? C27 C26 C25 108.3(7) . . ? C27 C26 Y2 72.5(4) . . ? C25 C26 Y2 74.5(4) . . ? C27 C26 H26A 125.6 . . ? C25 C26 H26A 125.6 . . ? Y2 C26 H26A 125.6 . . ? C26 C27 C28 108.5(7) . . ? C26 C27 Y2 78.0(4) . . ? C28 C27 Y2 74.1(4) . . ? C26 C27 H27A 125.0 . . ? C28 C27 H27A 125.0 . . ? Y2 C27 H27A 125.0 . . ? C27 C28 C29 106.9(8) . . ? C27 C28 Y2 75.4(4) . . ? C29 C28 Y2 76.2(4) . . ? C27 C28 H28A 125.7 . . ? C29 C28 H28A 125.7 . . ? Y2 C28 H28A 125.7 . . ? C25 C29 C28 107.1(7) . . ? C25 C29 Y2 76.1(4) . . ? C28 C29 Y2 72.9(4) . . ? C25 C29 H29A 125.9 . . ? C28 C29 H29A 125.9 . . ? Y2 C29 H29A 125.9 . . ? C31 C30 C34 108.6(7) . . ? C31 C30 Y2 74.9(4) . . ? C34 C30 Y2 74.4(4) . . ? C31 C30 H30A 125.3 . . ? C34 C30 H30A 125.3 . . ? Y2 C30 H30A 125.3 . . ? C32 C31 C30 108.2(7) . . ? C32 C31 Y2 74.3(4) . . ? C30 C31 Y2 75.5(4) . . ? C32 C31 H31A 125.4 . . ? C30 C31 H31A 125.4 . . ? Y2 C31 H31A 125.4 . . ? C31 C32 C33 107.7(7) . . ? C31 C32 Y2 76.0(4) . . ? C33 C32 Y2 75.0(4) . . ? C31 C32 H32A 125.5 . . ? C33 C32 H32A 125.5 . . ? Y2 C32 H32A 125.5 . . ? C34 C33 C32 109.0(8) . . ? C34 C33 Y2 75.6(4) . . ? C32 C33 Y2 74.9(4) . . ? C34 C33 H33A 125.0 . . ? C32 C33 H33A 125.0 . . ? Y2 C33 H33A 125.0 . . ? C33 C34 C30 106.5(7) . . ? C33 C34 Y2 74.5(4) . . ? C30 C34 Y2 75.5(4) . . ? C33 C34 H34A 126.0 . . ? C30 C34 H34A 126.0 . . ? Y2 C34 H34A 126.0 . . ? C36 C35 O1 106.3(6) . . ? C36 C35 H35A 110.5 . . ? O1 C35 H35A 110.5 . . ? C36 C35 H35B 110.5 . . ? O1 C35 H35B 110.5 . . ? H35A C35 H35B 108.7 . . ? C35 C36 C37 106.3(7) . . ? C35 C36 H36A 110.5 . . ? C37 C36 H36A 110.5 . . ? C35 C36 H36B 110.5 . . ? C37 C36 H36B 110.5 . . ? H36A C36 H36B 108.7 . . ? C36 C37 C38 105.2(6) . . ? C36 C37 H37A 110.7 . . ? C38 C37 H37A 110.7 . . ? C36 C37 H37B 110.7 . . ? C38 C37 H37B 110.7 . . ? H37A C37 H37B 108.8 . . ? O1 C38 C37 107.8(6) . . ? O1 C38 H38A 110.2 . . ? C37 C38 H38A 110.2 . . ? O1 C38 H38B 110.2 . . ? C37 C38 H38B 110.2 . . ? H38A C38 H38B 108.5 . . ? O2 C39 C40 109.5(8) . . ? O2 C39 H39A 109.8 . . ? C40 C39 H39A 109.8 . . ? O2 C39 H39B 109.8 . . ? C40 C39 H39B 109.8 . . ? H39A C39 H39B 108.2 . . ? C41 C40 C39 106.5(8) . . ? C41 C40 H40A 110.4 . . ? C39 C40 H40A 110.4 . . ? C41 C40 H40B 110.4 . . ? C39 C40 H40B 110.4 . . ? H40A C40 H40B 108.6 . . ? C40 C41 C42 102.7(7) . . ? C40 C41 H41A 111.2 . . ? C42 C41 H41A 111.2 . . ? C40 C41 H41B 111.2 . . ? C42 C41 H41B 111.2 . . ? H41A C41 H41B 109.1 . . ? O2 C42 C41 109.8(7) . . ? O2 C42 H42A 109.7 . . ? C41 C42 H42A 109.7 . . ? O2 C42 H42B 109.7 . . ? C41 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? C39 O2 C42 108.7(6) . . ? 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 H1B O2 0.90 2.22 3.095(6) 163.8 1_455 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.417 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.071 # Attachment 'complex_8.cif' data_06322b _database_code_depnum_ccdc_archive 'CCDC 676382' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H110 Gd3 N7 O3 S3' _chemical_formula_weight 1797.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 25.853(9) _cell_length_b 12.257(4) _cell_length_c 28.459(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.485(5) _cell_angle_gamma 90.00 _cell_volume 9015(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 246 _cell_measurement_theta_min 2.268 _cell_measurement_theta_max 18.803 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3636 _exptl_absorpt_coefficient_mu 2.295 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7246 _exptl_absorpt_correction_T_max 0.8030 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30400 _diffrn_reflns_av_R_equivalents 0.1800 _diffrn_reflns_av_sigmaI/netI 0.1893 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 20.59 _reflns_number_total 9117 _reflns_number_gt 4207 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1339P)^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 9117 _refine_ls_number_parameters 403 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.1929 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.2705 _refine_ls_wR_factor_gt 0.1835 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.56228(5) 0.86970(10) -0.03124(4) 0.0508(4) Uani 1 1 d . . . S1 S 0.5055(3) 0.9338(5) 0.0449(2) 0.059(2) Uani 1 1 d . . . N1 N 0.5731(8) 0.7327(15) 0.0351(7) 0.055(6) Uiso 1 1 d . . . N2 N 0.6348(7) 0.7413(14) 0.0997(6) 0.051(6) Uiso 1 1 d . . . H2A H 0.6585 0.7036 0.1139 0.061 Uiso 1 1 calc R . . N3 N 0.6553(8) 0.6452(15) 0.0325(7) 0.063(6) Uiso 1 1 d . . . H3A H 0.6876 0.6582 0.0376 0.075 Uiso 1 1 calc R . . C1 C 0.5052(9) 0.6955(17) -0.0604(7) 0.115(12) Uiso 1 1 d G . . H1A H 0.4966 0.6467 -0.0369 0.138 Uiso 1 1 calc R . . C2 C 0.5481(8) 0.6907(16) -0.0873(8) 0.085(10) Uiso 1 1 d G . . H2B H 0.5739 0.6379 -0.0853 0.102 Uiso 1 1 calc R . . C3 C 0.5465(8) 0.7769(17) -0.1177(7) 0.100(11) Uiso 1 1 d G . . H3B H 0.5710 0.7931 -0.1400 0.120 Uiso 1 1 calc R . . C4 C 0.5025(8) 0.8351(15) -0.1096(7) 0.073(9) Uiso 1 1 d G . . H4A H 0.4919 0.8979 -0.1254 0.088 Uiso 1 1 calc R . . C5 C 0.4770(8) 0.7848(17) -0.0742(7) 0.087(10) Uiso 1 1 d G . . H5A H 0.4459 0.8074 -0.0617 0.104 Uiso 1 1 calc R . . C6 C 0.6624(8) 0.8811(16) -0.0569(8) 0.088(10) Uiso 1 1 d G . . H6A H 0.6739 0.8212 -0.0738 0.105 Uiso 1 1 calc R . . C7 C 0.6647(8) 0.8924(16) -0.0083(8) 0.098(11) Uiso 1 1 d G . . H7A H 0.6780 0.8415 0.0130 0.117 Uiso 1 1 calc R . . C8 C 0.6436(8) 0.9932(17) 0.0028(7) 0.100(11) Uiso 1 1 d G . . H8A H 0.6404 1.0215 0.0329 0.120 Uiso 1 1 calc R . . C9 C 0.6283(8) 1.0441(14) -0.0389(7) 0.072(8) Uiso 1 1 d G . . H9A H 0.6130 1.1126 -0.0416 0.086 Uiso 1 1 calc R . . C10 C 0.6399(8) 0.9748(17) -0.0758(6) 0.088(10) Uiso 1 1 d G . . H10A H 0.6337 0.9888 -0.1076 0.105 Uiso 1 1 calc R . . C11 C 0.5298(10) 0.7239(19) 0.0668(8) 0.054(7) Uiso 1 1 d . . . C12 C 0.4957(9) 0.8111(18) 0.0747(8) 0.047(7) Uiso 1 1 d . . . C13 C 0.4561(10) 0.798(2) 0.1074(9) 0.066(8) Uiso 1 1 d . . . H13A H 0.4346 0.8565 0.1140 0.079 Uiso 1 1 calc R . . C14 C 0.4488(11) 0.697(2) 0.1302(9) 0.066(8) Uiso 1 1 d . . . H14A H 0.4230 0.6890 0.1521 0.079 Uiso 1 1 calc R . . C15 C 0.4805(11) 0.610(2) 0.1194(9) 0.072(8) Uiso 1 1 d . . . H15A H 0.4747 0.5419 0.1331 0.086 Uiso 1 1 calc R . . C16 C 0.5215(10) 0.623(2) 0.0877(9) 0.064(8) Uiso 1 1 d . . . H16A H 0.5429 0.5640 0.0810 0.077 Uiso 1 1 calc R . . C17 C 0.6166(10) 0.7074(19) 0.0564(9) 0.057(7) Uiso 1 1 d . . . C18 C 0.6157(10) 0.8374(18) 0.1222(8) 0.054(7) Uiso 1 1 d . . . H18A H 0.5913 0.8733 0.1003 0.064 Uiso 1 1 calc R . . C19 C 0.5874(10) 0.8115(19) 0.1668(8) 0.062(8) Uiso 1 1 d . . . H19A H 0.6112 0.7776 0.1894 0.074 Uiso 1 1 calc R . . H19B H 0.5598 0.7600 0.1598 0.074 Uiso 1 1 calc R . . C20 C 0.5647(12) 0.914(2) 0.1883(10) 0.092(10) Uiso 1 1 d . . . H20A H 0.5390 0.9443 0.1666 0.110 Uiso 1 1 calc R . . H20B H 0.5473 0.8944 0.2169 0.110 Uiso 1 1 calc R . . C21 C 0.6041(11) 0.999(2) 0.1995(10) 0.076(9) Uiso 1 1 d . . . H21A H 0.6260 0.9751 0.2257 0.091 Uiso 1 1 calc R . . H21B H 0.5870 1.0660 0.2085 0.091 Uiso 1 1 calc R . . C22 C 0.6367(12) 1.019(2) 0.1571(10) 0.087(10) Uiso 1 1 d . . . H22A H 0.6650 1.0670 0.1664 0.105 Uiso 1 1 calc R . . H22B H 0.6157 1.0578 0.1337 0.105 Uiso 1 1 calc R . . C23 C 0.6592(10) 0.9181(19) 0.1340(9) 0.067(8) Uiso 1 1 d . . . H23A H 0.6845 0.8842 0.1551 0.080 Uiso 1 1 calc R . . H23B H 0.6765 0.9387 0.1055 0.080 Uiso 1 1 calc R . . C24 C 0.6382(11) 0.556(2) -0.0019(9) 0.068(8) Uiso 1 1 d . . . H24A H 0.6036 0.5714 -0.0152 0.082 Uiso 1 1 calc R . . C25 C 0.6400(11) 0.4473(19) 0.0217(9) 0.074(9) Uiso 1 1 d . . . H25A H 0.6147 0.4456 0.0463 0.089 Uiso 1 1 calc R . . H25B H 0.6739 0.4365 0.0363 0.089 Uiso 1 1 calc R . . C26 C 0.6288(11) 0.356(2) -0.0129(10) 0.080(9) Uiso 1 1 d . . . H26A H 0.6307 0.2860 0.0032 0.095 Uiso 1 1 calc R . . H26B H 0.5942 0.3639 -0.0264 0.095 Uiso 1 1 calc R . . C27 C 0.6678(11) 0.359(2) -0.0509(10) 0.081(9) Uiso 1 1 d . . . H27A H 0.7022 0.3477 -0.0374 0.097 Uiso 1 1 calc R . . H27B H 0.6607 0.3015 -0.0734 0.097 Uiso 1 1 calc R . . C28 C 0.6660(13) 0.466(2) -0.0753(11) 0.105(11) Uiso 1 1 d . . . H28A H 0.6317 0.4778 -0.0890 0.126 Uiso 1 1 calc R . . H28B H 0.6905 0.4664 -0.1005 0.126 Uiso 1 1 calc R . . C29 C 0.6794(11) 0.562(2) -0.0402(10) 0.084(9) Uiso 1 1 d . . . H29A H 0.7138 0.5517 -0.0264 0.101 Uiso 1 1 calc R . . H29B H 0.6781 0.6313 -0.0562 0.101 Uiso 1 1 calc R . . Gd2 Gd 0.63449(5) 0.15026(10) 0.38893(5) 0.0498(4) Uani 1 1 d . . . Gd3 Gd 0.55268(5) 0.38194(10) 0.29809(5) 0.0522(5) Uani 1 1 d . . . S2 S 0.5793(3) 0.3501(5) 0.3957(2) 0.0552(19) Uani 1 1 d . . . S3 S 0.6341(2) 0.2261(5) 0.2936(2) 0.0503(19) Uani 1 1 d . . . N4 N 0.5981(8) 0.1887(16) 0.4729(7) 0.072(7) Uiso 1 1 d . . . H4B H 0.6205 0.2054 0.4522 0.087 Uiso 1 1 calc R . . H4C H 0.6057 0.1413 0.4943 0.087 Uiso 1 1 calc R . . N5 N 0.6311(7) 0.4645(14) 0.3112(6) 0.044(5) Uiso 1 1 d . . . N6 N 0.5663(8) 0.5755(15) 0.3076(6) 0.052(6) Uiso 1 1 d . . . N7 N 0.6472(7) 0.6466(15) 0.3385(6) 0.056(6) Uiso 1 1 d . . . H7B H 0.6439 0.7131 0.3292 0.067 Uiso 1 1 calc R . . O1 O 0.5776(6) 0.4132(13) 0.2176(5) 0.071(5) Uiso 1 1 d D . . C30 C 0.7189(12) 0.230(3) 0.4381(11) 0.094(10) Uiso 1 1 d . . . H30A H 0.7141 0.2842 0.4604 0.113 Uiso 1 1 calc R . . C31 C 0.7297(11) 0.248(3) 0.3913(11) 0.088(10) Uiso 1 1 d . . . H31A H 0.7323 0.3145 0.3759 0.106 Uiso 1 1 calc R . . C32 C 0.7357(12) 0.143(2) 0.3724(11) 0.091(10) Uiso 1 1 d . . . H32A H 0.7447 0.1295 0.3415 0.109 Uiso 1 1 calc R . . C33 C 0.7272(12) 0.064(3) 0.4036(11) 0.093(10) Uiso 1 1 d . . . H33A H 0.7280 -0.0106 0.3986 0.111 Uiso 1 1 calc R . . C34 C 0.7164(12) 0.119(2) 0.4465(11) 0.095(10) Uiso 1 1 d . . . H34A H 0.7091 0.0866 0.4751 0.114 Uiso 1 1 calc R . . C35 C 0.6158(12) -0.046(2) 0.3499(10) 0.085(10) Uiso 1 1 d . . . H35A H 0.6418 -0.0729 0.3312 0.102 Uiso 1 1 calc R . . C36 C 0.5750(11) 0.015(2) 0.3336(10) 0.073(9) Uiso 1 1 d . . . H36A H 0.5680 0.0379 0.3030 0.088 Uiso 1 1 calc R . . C37 C 0.5450(11) 0.036(2) 0.3750(10) 0.075(9) Uiso 1 1 d . . . H37A H 0.5146 0.0763 0.3755 0.090 Uiso 1 1 calc R . . C38 C 0.5676(10) -0.0124(19) 0.4128(10) 0.063(8) Uiso 1 1 d . . . H38A H 0.5549 -0.0123 0.4431 0.075 Uiso 1 1 calc R . . C39 C 0.6132(11) -0.063(2) 0.3989(10) 0.072(8) Uiso 1 1 d . . . H39A H 0.6371 -0.0995 0.4180 0.086 Uiso 1 1 calc R . . C40 C 0.5496(11) 0.238(2) 0.4717(9) 0.061(8) Uiso 1 1 d . . . C41 C 0.5341(10) 0.3137(18) 0.4394(8) 0.050(7) Uiso 1 1 d . . . C42 C 0.4885(11) 0.375(2) 0.4437(10) 0.084(9) Uiso 1 1 d . . . H42A H 0.4812 0.4353 0.4246 0.101 Uiso 1 1 calc R . . C43 C 0.4539(14) 0.340(2) 0.4793(11) 0.103(11) Uiso 1 1 d . . . H43A H 0.4219 0.3741 0.4819 0.123 Uiso 1 1 calc R . . C44 C 0.4677(14) 0.255(3) 0.5107(12) 0.112(12) Uiso 1 1 d . . . H44A H 0.4441 0.2311 0.5326 0.135 Uiso 1 1 calc R . . C45 C 0.5172(11) 0.204(2) 0.5090(10) 0.077(9) Uiso 1 1 d . . . H45A H 0.5279 0.1520 0.5309 0.092 Uiso 1 1 calc R . . C46 C 0.4631(12) 0.285(3) 0.3232(12) 0.094(10) Uiso 1 1 d . . . H46A H 0.4636 0.2652 0.3547 0.113 Uiso 1 1 calc R . . C47 C 0.4469(13) 0.381(3) 0.3054(12) 0.110(12) Uiso 1 1 d . . . H47A H 0.4321 0.4361 0.3229 0.132 Uiso 1 1 calc R . . C48 C 0.4551(14) 0.386(3) 0.2583(13) 0.122(13) Uiso 1 1 d . . . H48A H 0.4491 0.4450 0.2385 0.146 Uiso 1 1 calc R . . C49 C 0.4733(12) 0.288(3) 0.2467(12) 0.103(11) Uiso 1 1 d . . . H49A H 0.4813 0.2661 0.2165 0.124 Uiso 1 1 calc R . . C50 C 0.4785(13) 0.224(3) 0.2876(12) 0.106(12) Uiso 1 1 d . . . H50A H 0.4904 0.1529 0.2893 0.127 Uiso 1 1 calc R . . C51 C 0.6786(9) 0.4342(17) 0.2921(8) 0.041(6) Uiso 1 1 d . . . C52 C 0.6846(9) 0.3184(17) 0.2822(8) 0.044(6) Uiso 1 1 d . . . C53 C 0.7278(9) 0.2814(18) 0.2588(7) 0.043(6) Uiso 1 1 d . . . H53A H 0.7306 0.2076 0.2518 0.052 Uiso 1 1 calc R . . C54 C 0.7676(10) 0.3538(18) 0.2453(8) 0.054(7) Uiso 1 1 d . . . H54A H 0.7972 0.3275 0.2313 0.065 Uiso 1 1 calc R . . C55 C 0.7614(10) 0.4639(19) 0.2535(8) 0.054(7) Uiso 1 1 d . . . H55A H 0.7862 0.5127 0.2432 0.065 Uiso 1 1 calc R . . C56 C 0.7189(8) 0.5030(17) 0.2767(7) 0.038(6) Uiso 1 1 d . . . H56A H 0.7167 0.5775 0.2825 0.046 Uiso 1 1 calc R . . C57 C 0.6163(10) 0.5693(18) 0.3189(8) 0.045(7) Uiso 1 1 d . . . C58 C 0.5359(10) 0.6756(19) 0.3159(8) 0.053(7) Uiso 1 1 d . . . H58A H 0.5600 0.7358 0.3226 0.064 Uiso 1 1 calc R . . C59 C 0.5009(11) 0.661(2) 0.3581(10) 0.081(9) Uiso 1 1 d . . . H59A H 0.5221 0.6484 0.3861 0.097 Uiso 1 1 calc R . . H59B H 0.4789 0.5981 0.3530 0.097 Uiso 1 1 calc R . . C60 C 0.4665(11) 0.763(2) 0.3660(10) 0.085(10) Uiso 1 1 d . . . H60A H 0.4439 0.7500 0.3921 0.102 Uiso 1 1 calc R . . H60B H 0.4880 0.8256 0.3734 0.102 Uiso 1 1 calc R . . C61 C 0.4357(12) 0.783(2) 0.3231(10) 0.088(10) Uiso 1 1 d . . . H61A H 0.4144 0.8475 0.3279 0.106 Uiso 1 1 calc R . . H61B H 0.4127 0.7221 0.3174 0.106 Uiso 1 1 calc R . . C62 C 0.4689(12) 0.802(2) 0.2787(10) 0.093(10) Uiso 1 1 d . . . H62A H 0.4892 0.8679 0.2824 0.112 Uiso 1 1 calc R . . H62B H 0.4465 0.8098 0.2511 0.112 Uiso 1 1 calc R . . C63 C 0.5056(11) 0.702(2) 0.2724(10) 0.082(9) Uiso 1 1 d . . . H63A H 0.4852 0.6388 0.2631 0.098 Uiso 1 1 calc R . . H63B H 0.5293 0.7175 0.2474 0.098 Uiso 1 1 calc R . . C64 C 0.6862(8) 0.6211(17) 0.3750(7) 0.041(6) Uiso 1 1 d . . . H64A H 0.7031 0.5514 0.3683 0.049 Uiso 1 1 calc R . . C65 C 0.7267(10) 0.715(2) 0.3773(9) 0.065(8) Uiso 1 1 d . . . H65A H 0.7439 0.7197 0.3475 0.078 Uiso 1 1 calc R . . H65B H 0.7093 0.7833 0.3829 0.078 Uiso 1 1 calc R . . C66 C 0.7668(12) 0.693(2) 0.4168(10) 0.087(10) Uiso 1 1 d . . . H66A H 0.7856 0.6266 0.4103 0.104 Uiso 1 1 calc R . . H66B H 0.7915 0.7529 0.4181 0.104 Uiso 1 1 calc R . . C67 C 0.7406(12) 0.683(2) 0.4636(10) 0.086(10) Uiso 1 1 d . . . H67A H 0.7665 0.6682 0.4880 0.103 Uiso 1 1 calc R . . H67B H 0.7241 0.7519 0.4710 0.103 Uiso 1 1 calc R . . C68 C 0.7006(12) 0.593(2) 0.4630(10) 0.096(10) Uiso 1 1 d . . . H68A H 0.6832 0.5914 0.4928 0.115 Uiso 1 1 calc R . . H68B H 0.7171 0.5234 0.4583 0.115 Uiso 1 1 calc R . . C69 C 0.6597(10) 0.616(2) 0.4217(8) 0.067(8) Uiso 1 1 d . . . H69A H 0.6340 0.5585 0.4208 0.080 Uiso 1 1 calc R . . H69B H 0.6421 0.6846 0.4273 0.080 Uiso 1 1 calc R . . C70 C 0.5794(11) 0.331(2) 0.1820(10) 0.105(11) Uiso 1 1 d D . . H70A H 0.5493 0.3357 0.1611 0.126 Uiso 1 1 calc R . . H70B H 0.5799 0.2586 0.1963 0.126 Uiso 1 1 calc R . . C71 C 0.6275(11) 0.349(2) 0.1556(10) 0.115(12) Uiso 1 1 d D . . H71A H 0.6217 0.3344 0.1224 0.138 Uiso 1 1 calc R . . H71B H 0.6552 0.3021 0.1674 0.138 Uiso 1 1 calc R . . C72 C 0.6405(10) 0.4657(19) 0.1637(9) 0.091(10) Uiso 1 1 d D . . H72A H 0.6390 0.5056 0.1342 0.109 Uiso 1 1 calc R . . H72B H 0.6750 0.4727 0.1775 0.109 Uiso 1 1 calc R . . C73 C 0.6010(10) 0.5090(16) 0.1966(9) 0.073(9) Uiso 1 1 d D . . H73A H 0.6174 0.5545 0.2206 0.087 Uiso 1 1 calc R . . H73B H 0.5751 0.5519 0.1797 0.087 Uiso 1 1 calc R . . O2 O 0.6278(14) 1.007(2) 0.5398(11) 0.191(13) Uiso 1 1 d D . . C74 C 0.5972(16) 0.987(5) 0.5802(18) 0.37(5) Uiso 1 1 d D . . H74A H 0.5671 0.9438 0.5718 0.446 Uiso 1 1 calc R . . H74B H 0.5857 1.0557 0.5936 0.446 Uiso 1 1 calc R . . C75 C 0.631(2) 0.928(5) 0.6146(11) 0.30(3) Uiso 1 1 d D . . H75A H 0.6520 0.9778 0.6337 0.366 Uiso 1 1 calc R . . H75B H 0.6114 0.8814 0.6350 0.366 Uiso 1 1 calc R . . C76 C 0.665(2) 0.861(4) 0.583(2) 0.32(4) Uiso 1 1 d D . . H76A H 0.6535 0.7858 0.5832 0.384 Uiso 1 1 calc R . . H76B H 0.7004 0.8645 0.5943 0.384 Uiso 1 1 calc R . . C77 C 0.659(2) 0.910(4) 0.5354(15) 0.31(4) Uiso 1 1 d D . . H77A H 0.6922 0.9276 0.5231 0.374 Uiso 1 1 calc R . . H77B H 0.6415 0.8585 0.5142 0.374 Uiso 1 1 calc R . . O3 O 0.6558(19) 0.325(3) 0.5462(13) 0.245(17) Uiso 1 1 d D . . C78 C 0.6247(18) 0.418(5) 0.558(2) 0.34(4) Uiso 1 1 d D . . H78A H 0.5928 0.3933 0.5717 0.411 Uiso 1 1 calc R . . H78B H 0.6162 0.4594 0.5299 0.411 Uiso 1 1 calc R . . C79 C 0.654(3) 0.487(3) 0.592(2) 0.27(3) Uiso 1 1 d D . . H79A H 0.6376 0.4876 0.6224 0.324 Uiso 1 1 calc R . . H79B H 0.6566 0.5613 0.5809 0.324 Uiso 1 1 calc R . . C80 C 0.707(2) 0.436(5) 0.596(2) 0.40(5) Uiso 1 1 d D . . H80A H 0.7198 0.4386 0.6286 0.482 Uiso 1 1 calc R . . H80B H 0.7309 0.4731 0.5764 0.482 Uiso 1 1 calc R . . C81 C 0.698(2) 0.321(4) 0.581(2) 0.38(5) Uiso 1 1 d D . . H81A H 0.7288 0.2915 0.5667 0.460 Uiso 1 1 calc R . . H81B H 0.6887 0.2750 0.6069 0.460 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 0.0498(9) 0.0477(9) 0.0550(9) -0.0044(7) 0.0063(7) 0.0020(7) S1 0.058(5) 0.047(4) 0.073(5) 0.001(4) 0.020(4) 0.010(4) Gd2 0.0443(9) 0.0444(8) 0.0616(9) 0.0016(7) 0.0199(7) -0.0019(7) Gd3 0.0466(9) 0.0484(9) 0.0622(10) -0.0010(7) 0.0147(7) -0.0055(7) S2 0.059(5) 0.044(4) 0.064(5) 0.007(3) 0.028(4) 0.006(4) S3 0.047(5) 0.036(4) 0.069(5) -0.006(3) 0.023(4) -0.005(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 N1 2.537(19) . ? Gd1 C5 2.70(2) . ? Gd1 C6 2.71(2) . ? Gd1 C4 2.713(19) . ? Gd1 C1 2.71(2) . ? Gd1 C7 2.72(2) . ? Gd1 C10 2.73(2) . ? Gd1 C3 2.73(2) . ? Gd1 C2 2.733(19) . ? Gd1 C8 2.75(2) . ? Gd1 C9 2.748(19) . ? Gd1 S1 2.762(7) . ? S1 C12 1.75(2) . ? S1 Gd1 2.998(6) 3_675 ? N1 C17 1.30(3) . ? N1 C11 1.46(3) . ? N2 C17 1.37(3) . ? N2 C18 1.43(3) . ? N2 H2A 0.8600 . ? N3 C17 1.44(3) . ? N3 C24 1.52(3) . ? N3 H3A 0.8600 . ? C1 C5 1.366(13) . ? C1 C2 1.366(13) . ? C1 H1A 0.9300 . ? C2 C3 1.365(13) . ? C2 H2B 0.9300 . ? C3 C4 1.366(13) . ? C3 H3B 0.9300 . ? C4 C5 1.366(13) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C10 1.390(13) . ? C6 C7 1.390(13) . ? C6 H6A 0.9300 . ? C7 C8 1.390(13) . ? C7 H7A 0.9300 . ? C8 C9 1.390(13) . ? C8 H8A 0.9300 . ? C9 C10 1.390(13) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C16 1.39(3) . ? C11 C12 1.41(3) . ? C12 C13 1.41(3) . ? C13 C14 1.42(3) . ? C13 H13A 0.9300 . ? C14 C15 1.39(3) . ? C14 H14A 0.9300 . ? C15 C16 1.42(3) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C18 C19 1.52(3) . ? C18 C23 1.53(3) . ? C18 H18A 0.9800 . ? C19 C20 1.52(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.48(3) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.51(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.53(3) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.50(3) . ? C24 C29 1.54(3) . ? C24 H24A 0.9800 . ? C25 C26 1.52(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.50(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.48(3) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.57(4) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? Gd2 N4 2.63(2) . ? Gd2 C33 2.64(3) . ? Gd2 C34 2.67(3) . ? Gd2 C32 2.67(3) . ? Gd2 C39 2.68(3) . ? Gd2 C35 2.69(3) . ? Gd2 C37 2.73(3) . ? Gd2 C36 2.73(3) . ? Gd2 C31 2.74(3) . ? Gd2 C38 2.74(2) . ? Gd2 C30 2.74(3) . ? Gd2 S2 2.844(6) . ? Gd3 N5 2.289(18) . ? Gd3 N6 2.412(18) . ? Gd3 O1 2.426(15) . ? Gd3 C46 2.71(3) . ? Gd3 C50 2.73(3) . ? Gd3 C48 2.74(4) . ? Gd3 C49 2.74(3) . ? Gd3 C47 2.75(3) . ? Gd3 S3 2.848(6) . ? Gd3 S2 2.870(7) . ? Gd3 C57 2.88(2) . ? S2 C41 1.78(2) . ? S3 C52 1.76(2) . ? N4 C40 1.39(3) . ? N4 H4B 0.8600 . ? N4 H4C 0.8600 . ? N5 C57 1.36(2) . ? N5 C51 1.41(3) . ? N6 C57 1.33(3) . ? N6 C58 1.48(3) . ? N7 C57 1.35(3) . ? N7 C64 1.46(3) . ? N7 H7B 0.8600 . ? O1 C70 1.435(18) . ? O1 C73 1.456(17) . ? C30 C34 1.38(3) . ? C30 C31 1.38(4) . ? C30 H30A 0.9300 . ? C31 C32 1.41(4) . ? C31 H31A 0.9300 . ? C32 C33 1.33(4) . ? C32 H32A 0.9300 . ? C33 C34 1.43(4) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 C36 1.36(3) . ? C35 C39 1.41(3) . ? C35 H35A 0.9300 . ? C36 C37 1.45(3) . ? C36 H36A 0.9300 . ? C37 C38 1.35(3) . ? C37 H37A 0.9300 . ? C38 C39 1.40(3) . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C40 C41 1.36(3) . ? C40 C45 1.43(3) . ? C41 C42 1.41(3) . ? C42 C43 1.44(4) . ? C42 H42A 0.9300 . ? C43 C44 1.42(4) . ? C43 H43A 0.9300 . ? C44 C45 1.42(4) . ? C44 H44A 0.9300 . ? C45 H45A 0.9300 . ? C46 C50 1.33(4) . ? C46 C47 1.34(4) . ? C46 H46A 0.9300 . ? C47 C48 1.37(4) . ? C47 H47A 0.9300 . ? C48 C49 1.33(4) . ? C48 H48A 0.9300 . ? C49 C50 1.41(4) . ? C49 H49A 0.9300 . ? C50 H50A 0.9300 . ? C51 C56 1.42(3) . ? C51 C52 1.46(3) . ? C52 C53 1.39(3) . ? C53 C54 1.42(3) . ? C53 H53A 0.9300 . ? C54 C55 1.38(3) . ? C54 H54A 0.9300 . ? C55 C56 1.38(3) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C58 C63 1.48(3) . ? C58 C59 1.53(3) . ? C58 H58A 0.9800 . ? C59 C60 1.55(3) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.46(3) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.56(4) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.56(3) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C69 1.51(3) . ? C64 C65 1.55(3) . ? C64 H64A 0.9800 . ? C65 C66 1.53(3) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.52(3) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C68 1.51(3) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C69 1.59(3) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.486(19) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C72 1.487(19) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 C73 1.500(18) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? O2 C74 1.433(15) . ? O2 C77 1.442(15) . ? C74 C75 1.492(16) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 C76 1.489(15) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 C77 1.496(15) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? O3 C78 1.432(15) . ? O3 C81 1.446(15) . ? C78 C79 1.488(15) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C79 C80 1.493(15) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? C80 C81 1.501(15) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C81 H81A 0.9700 . ? C81 H81B 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 N1 Gd1 C5 98.9(7) . . ? N1 Gd1 C6 98.4(7) . . ? C5 Gd1 C6 132.2(6) . . ? N1 Gd1 C4 123.9(6) . . ? C5 Gd1 C4 29.2(3) . . ? C6 Gd1 C4 108.3(7) . . ? N1 Gd1 C1 75.9(6) . . ? C5 Gd1 C1 29.2(3) . . ? C6 Gd1 C1 118.3(6) . . ? C4 Gd1 C1 48.1(4) . . ? N1 Gd1 C7 78.5(6) . . ? C5 Gd1 C7 157.6(6) . . ? C6 Gd1 C7 29.6(3) . . ? C4 Gd1 C7 137.9(7) . . ? C1 Gd1 C7 132.2(7) . . ? N1 Gd1 C10 126.2(6) . . ? C5 Gd1 C10 125.0(6) . . ? C6 Gd1 C10 29.6(3) . . ? C4 Gd1 C10 95.9(6) . . ? C1 Gd1 C10 129.1(6) . . ? C7 Gd1 C10 48.7(5) . . ? N1 Gd1 C3 113.9(6) . . ? C5 Gd1 C3 48.0(4) . . ? C6 Gd1 C3 84.3(6) . . ? C4 Gd1 C3 29.0(3) . . ? C1 Gd1 C3 47.9(4) . . ? C7 Gd1 C3 112.4(6) . . ? C10 Gd1 C3 82.7(6) . . ? N1 Gd1 C2 85.1(6) . . ? C5 Gd1 C2 48.0(5) . . ? C6 Gd1 C2 89.9(6) . . ? C4 Gd1 C2 47.9(4) . . ? C1 Gd1 C2 29.0(3) . . ? C7 Gd1 C2 109.7(6) . . ? C10 Gd1 C2 101.4(7) . . ? C3 Gd1 C2 28.9(3) . . ? N1 Gd1 C8 91.9(6) . . ? C5 Gd1 C8 168.6(7) . . ? C6 Gd1 C8 48.7(5) . . ? C4 Gd1 C8 142.2(6) . . ? C1 Gd1 C8 161.2(7) . . ? C7 Gd1 C8 29.4(3) . . ? C10 Gd1 C8 48.5(5) . . ? C3 Gd1 C8 130.0(6) . . ? C2 Gd1 C8 137.6(6) . . ? N1 Gd1 C9 121.1(6) . . ? C5 Gd1 C9 139.9(6) . . ? C6 Gd1 C9 48.7(5) . . ? C4 Gd1 C9 113.5(6) . . ? C1 Gd1 C9 157.2(6) . . ? C7 Gd1 C9 48.5(5) . . ? C10 Gd1 C9 29.4(3) . . ? C3 Gd1 C9 109.4(6) . . ? C2 Gd1 C9 130.8(7) . . ? C8 Gd1 C9 29.3(3) . . ? N1 Gd1 S1 69.8(5) . . ? C5 Gd1 S1 91.2(4) . . ? C6 Gd1 S1 136.6(5) . . ? C4 Gd1 S1 112.7(5) . . ? C1 Gd1 S1 99.7(5) . . ? C7 Gd1 S1 108.4(5) . . ? C10 Gd1 S1 130.0(5) . . ? C3 Gd1 S1 139.0(5) . . ? C2 Gd1 S1 128.3(5) . . ? C8 Gd1 S1 89.1(4) . . ? C9 Gd1 S1 100.6(4) . . ? C12 S1 Gd1 102.9(8) . . ? C12 S1 Gd1 131.4(9) . 3_675 ? Gd1 S1 Gd1 116.6(2) . 3_675 ? C17 N1 C11 111(2) . . ? C17 N1 Gd1 125.6(17) . . ? C11 N1 Gd1 115.9(15) . . ? C17 N2 C18 122(2) . . ? C17 N2 H2A 118.8 . . ? C18 N2 H2A 118.8 . . ? C17 N3 C24 119(2) . . ? C17 N3 H3A 120.3 . . ? C24 N3 H3A 120.3 . . ? C5 C1 C2 108.0 . . ? C5 C1 Gd1 74.9(7) . . ? C2 C1 Gd1 76.2(8) . . ? C5 C1 H1A 126.0 . . ? C2 C1 H1A 126.0 . . ? Gd1 C1 H1A 115.1 . . ? C3 C2 C1 108.0 . . ? C3 C2 Gd1 75.5(8) . . ? C1 C2 Gd1 74.7(8) . . ? C3 C2 H2B 126.0 . . ? C1 C2 H2B 126.0 . . ? Gd1 C2 H2B 115.9 . . ? C2 C3 C4 108.0 . . ? C2 C3 Gd1 75.6(8) . . ? C4 C3 Gd1 74.7(7) . . ? C2 C3 H3B 126.0 . . ? C4 C3 H3B 126.0 . . ? Gd1 C3 H3B 115.9 . . ? C3 C4 C5 108.0 . . ? C3 C4 Gd1 76.3(8) . . ? C5 C4 Gd1 74.9(8) . . ? C3 C4 H4A 126.0 . . ? C5 C4 H4A 126.0 . . ? Gd1 C4 H4A 115.0 . . ? C1 C5 C4 108.0 . . ? C1 C5 Gd1 75.9(8) . . ? C4 C5 Gd1 75.9(8) . . ? C1 C5 H5A 126.0 . . ? C4 C5 H5A 126.0 . . ? Gd1 C5 H5A 114.5 . . ? C10 C6 C7 108.0 . . ? C10 C6 Gd1 75.8(8) . . ? C7 C6 Gd1 75.7(8) . . ? C10 C6 H6A 126.0 . . ? C7 C6 H6A 126.0 . . ? Gd1 C6 H6A 114.8 . . ? C8 C7 C6 108.0 . . ? C8 C7 Gd1 76.2(8) . . ? C6 C7 Gd1 74.6(8) . . ? C8 C7 H7A 126.0 . . ? C6 C7 H7A 126.0 . . ? Gd1 C7 H7A 115.3 . . ? C9 C8 C7 108.0 . . ? C9 C8 Gd1 75.4(8) . . ? C7 C8 Gd1 74.4(8) . . ? C9 C8 H8A 126.0 . . ? C7 C8 H8A 126.0 . . ? Gd1 C8 H8A 116.4 . . ? C8 C9 C10 108.0 . . ? C8 C9 Gd1 75.3(8) . . ? C10 C9 Gd1 74.4(8) . . ? C8 C9 H9A 126.0 . . ? C10 C9 H9A 126.0 . . ? Gd1 C9 H9A 116.4 . . ? C9 C10 C6 108.0 . . ? C9 C10 Gd1 76.2(8) . . ? C6 C10 Gd1 74.6(8) . . ? C9 C10 H10A 126.0 . . ? C6 C10 H10A 126.0 . . ? Gd1 C10 H10A 115.4 . . ? C16 C11 C12 120(2) . . ? C16 C11 N1 117(2) . . ? C12 C11 N1 122(2) . . ? C11 C12 C13 119(2) . . ? C11 C12 S1 118.5(19) . . ? C13 C12 S1 122.4(19) . . ? C12 C13 C14 121(2) . . ? C12 C13 H13A 119.6 . . ? C14 C13 H13A 119.6 . . ? C15 C14 C13 119(3) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C14 C15 C16 121(3) . . ? C14 C15 H15A 119.7 . . ? C16 C15 H15A 119.7 . . ? C11 C16 C15 120(2) . . ? C11 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? N1 C17 N2 128(2) . . ? N1 C17 N3 120(2) . . ? N2 C17 N3 111(2) . . ? N2 C18 C19 112.4(19) . . ? N2 C18 C23 112(2) . . ? C19 C18 C23 109(2) . . ? N2 C18 H18A 107.9 . . ? C19 C18 H18A 107.9 . . ? C23 C18 H18A 107.9 . . ? C18 C19 C20 111(2) . . ? C18 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? C18 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C21 C20 C19 113(2) . . ? C21 C20 H20A 108.9 . . ? C19 C20 H20A 108.9 . . ? C21 C20 H20B 108.9 . . ? C19 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C20 C21 C22 110(2) . . ? C20 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? C20 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? C21 C22 C23 116(2) . . ? C21 C22 H22A 108.3 . . ? C23 C22 H22A 108.3 . . ? C21 C22 H22B 108.3 . . ? C23 C22 H22B 108.3 . . ? H22A C22 H22B 107.4 . . ? C22 C23 C18 109(2) . . ? C22 C23 H23A 109.8 . . ? C18 C23 H23A 109.8 . . ? C22 C23 H23B 109.8 . . ? C18 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? C25 C24 N3 110(2) . . ? C25 C24 C29 110(2) . . ? N3 C24 C29 103(2) . . ? C25 C24 H24A 111.1 . . ? N3 C24 H24A 111.1 . . ? C29 C24 H24A 111.1 . . ? C24 C25 C26 111(2) . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C27 C26 C25 109(2) . . ? C27 C26 H26A 109.9 . . ? C25 C26 H26A 109.9 . . ? C27 C26 H26B 109.9 . . ? C25 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? C28 C27 C26 111(2) . . ? C28 C27 H27A 109.5 . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 C29 111(3) . . ? C27 C28 H28A 109.5 . . ? C29 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C24 C29 C28 106(2) . . ? C24 C29 H29A 110.6 . . ? C28 C29 H29A 110.6 . . ? C24 C29 H29B 110.6 . . ? C28 C29 H29B 110.6 . . ? H29A C29 H29B 108.7 . . ? N4 Gd2 C33 105.8(8) . . ? N4 Gd2 C34 76.4(8) . . ? C33 Gd2 C34 31.2(8) . . ? N4 Gd2 C32 122.7(8) . . ? C33 Gd2 C32 29.0(8) . . ? C34 Gd2 C32 48.6(10) . . ? N4 Gd2 C39 89.9(7) . . ? C33 Gd2 C39 77.5(9) . . ? C34 Gd2 C39 87.7(9) . . ? C32 Gd2 C39 100.9(9) . . ? N4 Gd2 C35 118.0(8) . . ? C33 Gd2 C35 82.0(10) . . ? C34 Gd2 C35 105.0(9) . . ? C32 Gd2 C35 93.6(9) . . ? C39 Gd2 C35 30.5(7) . . ? N4 Gd2 C37 84.4(7) . . ? C33 Gd2 C37 125.5(9) . . ? C34 Gd2 C37 132.3(9) . . ? C32 Gd2 C37 142.0(9) . . ? C39 Gd2 C37 48.6(8) . . ? C35 Gd2 C37 48.4(9) . . ? N4 Gd2 C36 115.0(7) . . ? C33 Gd2 C36 110.1(9) . . ? C34 Gd2 C36 133.9(9) . . ? C32 Gd2 C36 114.7(9) . . ? C39 Gd2 C36 50.0(8) . . ? C35 Gd2 C36 29.1(7) . . ? C37 Gd2 C36 30.8(7) . . ? N4 Gd2 C31 104.0(8) . . ? C33 Gd2 C31 50.1(9) . . ? C34 Gd2 C31 49.3(9) . . ? C32 Gd2 C31 30.1(8) . . ? C39 Gd2 C31 127.5(9) . . ? C35 Gd2 C31 123.6(9) . . ? C37 Gd2 C31 171.2(9) . . ? C36 Gd2 C31 140.6(9) . . ? N4 Gd2 C38 70.2(7) . . ? C33 Gd2 C38 104.3(9) . . ? C34 Gd2 C38 103.9(9) . . ? C32 Gd2 C38 130.3(8) . . ? C39 Gd2 C38 29.9(7) . . ? C35 Gd2 C38 48.9(8) . . ? C37 Gd2 C38 28.5(7) . . ? C36 Gd2 C38 49.5(8) . . ? C31 Gd2 C38 152.4(9) . . ? N4 Gd2 C30 76.8(8) . . ? C33 Gd2 C30 49.8(9) . . ? C34 Gd2 C30 29.4(7) . . ? C32 Gd2 C30 48.1(9) . . ? C39 Gd2 C30 117.1(9) . . ? C35 Gd2 C30 131.4(9) . . ? C37 Gd2 C30 156.7(9) . . ? C36 Gd2 C30 159.9(9) . . ? C31 Gd2 C30 29.3(7) . . ? C38 Gd2 C30 129.2(8) . . ? N4 Gd2 S2 66.0(5) . . ? C33 Gd2 S2 142.0(7) . . ? C34 Gd2 S2 118.1(7) . . ? C32 Gd2 S2 122.5(6) . . ? C39 Gd2 S2 136.6(6) . . ? C35 Gd2 S2 135.5(7) . . ? C37 Gd2 S2 91.6(6) . . ? C36 Gd2 S2 106.6(6) . . ? C31 Gd2 S2 94.3(7) . . ? C38 Gd2 S2 106.8(6) . . ? C30 Gd2 S2 93.0(7) . . ? N5 Gd3 N6 54.6(6) . . ? N5 Gd3 O1 80.1(6) . . ? N6 Gd3 O1 84.8(6) . . ? N5 Gd3 C46 155.3(8) . . ? N6 Gd3 C46 121.5(8) . . ? O1 Gd3 C46 124.5(8) . . ? N5 Gd3 C50 161.2(9) . . ? N6 Gd3 C50 143.8(9) . . ? O1 Gd3 C50 102.2(8) . . ? C46 Gd3 C50 28.2(8) . . ? N5 Gd3 C48 149.6(9) . . ? N6 Gd3 C48 99.2(9) . . ? O1 Gd3 C48 82.6(9) . . ? C46 Gd3 C48 48.2(10) . . ? C50 Gd3 C48 47.9(10) . . ? N5 Gd3 C49 157.0(8) . . ? N6 Gd3 C49 125.2(8) . . ? O1 Gd3 C49 77.1(8) . . ? C46 Gd3 C49 47.6(10) . . ? C50 Gd3 C49 29.8(8) . . ? C48 Gd3 C49 28.0(8) . . ? N5 Gd3 C47 150.4(8) . . ? N6 Gd3 C47 98.0(8) . . ? O1 Gd3 C47 111.2(8) . . ? C46 Gd3 C47 28.3(8) . . ? C50 Gd3 C47 46.1(10) . . ? C48 Gd3 C47 28.8(9) . . ? C49 Gd3 C47 46.0(10) . . ? N5 Gd3 S3 69.6(5) . . ? N6 Gd3 S3 124.0(5) . . ? O1 Gd3 S3 81.3(4) . . ? C46 Gd3 S3 110.8(7) . . ? C50 Gd3 S3 92.2(7) . . ? C48 Gd3 S3 131.8(8) . . ? C49 Gd3 S3 103.9(7) . . ? C47 Gd3 S3 137.5(7) . . ? N5 Gd3 S2 73.3(5) . . ? N6 Gd3 S2 89.7(5) . . ? O1 Gd3 S2 150.7(4) . . ? C46 Gd3 S2 82.6(7) . . ? C50 Gd3 S2 99.2(7) . . ? C48 Gd3 S2 126.7(8) . . ? C49 Gd3 S2 128.1(7) . . ? C47 Gd3 S2 98.0(7) . . ? S3 Gd3 S2 78.05(19) . . ? N5 Gd3 C57 27.6(6) . . ? N6 Gd3 C57 27.3(6) . . ? O1 Gd3 C57 84.5(6) . . ? C46 Gd3 C57 141.4(8) . . ? C50 Gd3 C57 169.2(9) . . ? C48 Gd3 C57 125.9(9) . . ? C49 Gd3 C57 149.3(8) . . ? C47 Gd3 C57 123.6(8) . . ? S3 Gd3 C57 97.2(5) . . ? S2 Gd3 C57 77.8(5) . . ? C41 S2 Gd2 99.8(8) . . ? C41 S2 Gd3 124.3(9) . . ? Gd2 S2 Gd3 99.2(2) . . ? C52 S3 Gd3 97.4(8) . . ? C52 S3 Gd2 113.4(8) . . ? Gd3 S3 Gd2 99.21(19) . . ? C40 N4 Gd2 113.5(16) . . ? C40 N4 H4B 120.0 . . ? Gd2 N4 H4B 32.9 . . ? C40 N4 H4C 120.0 . . ? Gd2 N4 H4C 116.2 . . ? H4B N4 H4C 120.0 . . ? C57 N5 C51 124.4(19) . . ? C57 N5 Gd3 101.0(15) . . ? C51 N5 Gd3 126.8(14) . . ? C57 N6 C58 122(2) . . ? C57 N6 Gd3 96.3(15) . . ? C58 N6 Gd3 139.2(15) . . ? C57 N7 C64 122.2(19) . . ? C57 N7 H7B 118.9 . . ? C64 N7 H7B 118.9 . . ? C70 O1 C73 105.0(15) . . ? C70 O1 Gd3 124.7(14) . . ? C73 O1 Gd3 129.7(13) . . ? C34 C30 C31 110(3) . . ? C34 C30 Gd2 72.5(19) . . ? C31 C30 Gd2 75.1(18) . . ? C34 C30 H30A 125.2 . . ? C31 C30 H30A 125.2 . . ? Gd2 C30 H30A 118.9 . . ? C30 C31 C32 104(3) . . ? C30 C31 Gd2 75.6(18) . . ? C32 C31 Gd2 72.4(18) . . ? C30 C31 H31A 127.8 . . ? C32 C31 H31A 127.8 . . ? Gd2 C31 H31A 116.7 . . ? C33 C32 C31 113(3) . . ? C33 C32 Gd2 74(2) . . ? C31 C32 Gd2 77.4(18) . . ? C33 C32 H32A 123.7 . . ? C31 C32 H32A 123.7 . . ? Gd2 C32 H32A 116.2 . . ? C32 C33 C34 106(3) . . ? C32 C33 Gd2 77(2) . . ? C34 C33 Gd2 75.6(18) . . ? C32 C33 H33A 127.2 . . ? C34 C33 H33A 127.2 . . ? Gd2 C33 H33A 113.2 . . ? C30 C34 C33 108(3) . . ? C30 C34 Gd2 78.1(19) . . ? C33 C34 Gd2 73.2(18) . . ? C30 C34 H34A 126.1 . . ? C33 C34 H34A 126.1 . . ? Gd2 C34 H34A 114.8 . . ? C36 C35 C39 111(3) . . ? C36 C35 Gd2 77.3(17) . . ? C39 C35 Gd2 74.6(16) . . ? C36 C35 H35A 124.5 . . ? C39 C35 H35A 124.5 . . ? Gd2 C35 H35A 115.4 . . ? C35 C36 C37 104(3) . . ? C35 C36 Gd2 73.6(17) . . ? C37 C36 Gd2 74.3(15) . . ? C35 C36 H36A 127.9 . . ? C37 C36 H36A 127.9 . . ? Gd2 C36 H36A 116.7 . . ? C38 C37 C36 110(3) . . ? C38 C37 Gd2 76.2(16) . . ? C36 C37 Gd2 74.9(16) . . ? C38 C37 H37A 125.0 . . ? C36 C37 H37A 125.0 . . ? Gd2 C37 H37A 115.9 . . ? C37 C38 C39 109(3) . . ? C37 C38 Gd2 75.3(16) . . ? C39 C38 Gd2 72.9(15) . . ? C37 C38 H38A 125.7 . . ? C39 C38 H38A 125.7 . . ? Gd2 C38 H38A 118.0 . . ? C38 C39 C35 106(3) . . ? C38 C39 Gd2 77.2(15) . . ? C35 C39 Gd2 74.9(16) . . ? C38 C39 H39A 126.9 . . ? C35 C39 H39A 126.9 . . ? Gd2 C39 H39A 113.6 . . ? C41 C40 N4 124(3) . . ? C41 C40 C45 122(3) . . ? N4 C40 C45 114(2) . . ? C40 C41 C42 123(3) . . ? C40 C41 S2 117(2) . . ? C42 C41 S2 119(2) . . ? C41 C42 C43 116(3) . . ? C41 C42 H42A 122.0 . . ? C43 C42 H42A 122.0 . . ? C44 C43 C42 121(3) . . ? C44 C43 H43A 119.5 . . ? C42 C43 H43A 119.5 . . ? C43 C44 C45 121(3) . . ? C43 C44 H44A 119.6 . . ? C45 C44 H44A 119.6 . . ? C44 C45 C40 116(3) . . ? C44 C45 H45A 121.9 . . ? C40 C45 H45A 121.9 . . ? C50 C46 C47 107(3) . . ? C50 C46 Gd3 77(2) . . ? C47 C46 Gd3 77(2) . . ? C50 C46 H46A 126.3 . . ? C47 C46 H46A 126.3 . . ? Gd3 C46 H46A 112.3 . . ? C46 C47 C48 111(3) . . ? C46 C47 Gd3 74(2) . . ? C48 C47 Gd3 75(2) . . ? C46 C47 H47A 124.5 . . ? C48 C47 H47A 124.5 . . ? Gd3 C47 H47A 117.5 . . ? C49 C48 C47 106(4) . . ? C49 C48 Gd3 76(2) . . ? C47 C48 Gd3 76(2) . . ? C49 C48 H48A 127.2 . . ? C47 C48 H48A 127.2 . . ? Gd3 C48 H48A 113.6 . . ? C48 C49 C50 109(3) . . ? C48 C49 Gd3 76(2) . . ? C50 C49 Gd3 74.8(19) . . ? C48 C49 H49A 125.6 . . ? C50 C49 H49A 125.6 . . ? Gd3 C49 H49A 115.7 . . ? C46 C50 C49 107(3) . . ? C46 C50 Gd3 75(2) . . ? C49 C50 Gd3 75.4(19) . . ? C46 C50 H50A 126.4 . . ? C49 C50 H50A 126.4 . . ? Gd3 C50 H50A 115.4 . . ? N5 C51 C56 128(2) . . ? N5 C51 C52 115(2) . . ? C56 C51 C52 116(2) . . ? C53 C52 C51 120(2) . . ? C53 C52 S3 119.1(17) . . ? C51 C52 S3 120.5(18) . . ? C52 C53 C54 122(2) . . ? C52 C53 H53A 119.2 . . ? C54 C53 H53A 119.2 . . ? C55 C54 C53 118(2) . . ? C55 C54 H54A 120.8 . . ? C53 C54 H54A 120.8 . . ? C54 C55 C56 121(2) . . ? C54 C55 H55A 119.4 . . ? C56 C55 H55A 119.4 . . ? C55 C56 C51 123(2) . . ? C55 C56 H56A 118.6 . . ? C51 C56 H56A 118.6 . . ? N6 C57 N7 129(2) . . ? N6 C57 N5 107(2) . . ? N7 C57 N5 124(2) . . ? N6 C57 Gd3 56.5(12) . . ? N7 C57 Gd3 166.9(16) . . ? N5 C57 Gd3 51.3(12) . . ? N6 C58 C63 108(2) . . ? N6 C58 C59 111.0(19) . . ? C63 C58 C59 112(2) . . ? N6 C58 H58A 108.5 . . ? C63 C58 H58A 108.5 . . ? C59 C58 H58A 108.5 . . ? C58 C59 C60 112(2) . . ? C58 C59 H59A 109.2 . . ? C60 C59 H59A 109.2 . . ? C58 C59 H59B 109.2 . . ? C60 C59 H59B 109.2 . . ? H59A C59 H59B 107.9 . . ? C61 C60 C59 109(2) . . ? C61 C60 H60A 109.9 . . ? C59 C60 H60A 109.9 . . ? C61 C60 H60B 109.9 . . ? C59 C60 H60B 109.9 . . ? H60A C60 H60B 108.3 . . ? C60 C61 C62 114(3) . . ? C60 C61 H61A 108.9 . . ? C62 C61 H61A 108.9 . . ? C60 C61 H61B 108.9 . . ? C62 C61 H61B 108.9 . . ? H61A C61 H61B 107.7 . . ? C61 C62 C63 109(2) . . ? C61 C62 H62A 109.8 . . ? C63 C62 H62A 109.8 . . ? C61 C62 H62B 109.8 . . ? C63 C62 H62B 109.8 . . ? H62A C62 H62B 108.3 . . ? C58 C63 C62 113(2) . . ? C58 C63 H63A 109.1 . . ? C62 C63 H63A 109.1 . . ? C58 C63 H63B 109.1 . . ? C62 C63 H63B 109.1 . . ? H63A C63 H63B 107.8 . . ? N7 C64 C69 108.2(18) . . ? N7 C64 C65 108.9(18) . . ? C69 C64 C65 108.3(19) . . ? N7 C64 H64A 110.4 . . ? C69 C64 H64A 110.4 . . ? C65 C64 H64A 110.4 . . ? C66 C65 C64 110(2) . . ? C66 C65 H65A 109.6 . . ? C64 C65 H65A 109.6 . . ? C66 C65 H65B 109.6 . . ? C64 C65 H65B 109.6 . . ? H65A C65 H65B 108.1 . . ? C67 C66 C65 110(2) . . ? C67 C66 H66A 109.6 . . ? C65 C66 H66A 109.6 . . ? C67 C66 H66B 109.6 . . ? C65 C66 H66B 109.6 . . ? H66A C66 H66B 108.1 . . ? C68 C67 C66 112(2) . . ? C68 C67 H67A 109.3 . . ? C66 C67 H67A 109.3 . . ? C68 C67 H67B 109.3 . . ? C66 C67 H67B 109.3 . . ? H67A C67 H67B 107.9 . . ? C67 C68 C69 109(2) . . ? C67 C68 H68A 109.9 . . ? C69 C68 H68A 109.9 . . ? C67 C68 H68B 109.9 . . ? C69 C68 H68B 109.9 . . ? H68A C68 H68B 108.3 . . ? C64 C69 C68 111(2) . . ? C64 C69 H69A 109.5 . . ? C68 C69 H69A 109.5 . . ? C64 C69 H69B 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 108.1 . . ? O1 C70 C71 107.0(17) . . ? O1 C70 H70A 110.3 . . ? C71 C70 H70A 110.3 . . ? O1 C70 H70B 110.3 . . ? C71 C70 H70B 110.3 . . ? H70A C70 H70B 108.6 . . ? C70 C71 C72 104.9(16) . . ? C70 C71 H71A 110.8 . . ? C72 C71 H71A 110.8 . . ? C70 C71 H71B 110.8 . . ? C72 C71 H71B 110.8 . . ? H71A C71 H71B 108.8 . . ? C71 C72 C73 106.4(16) . . ? C71 C72 H72A 110.5 . . ? C73 C72 H72A 110.5 . . ? C71 C72 H72B 110.5 . . ? C73 C72 H72B 110.5 . . ? H72A C72 H72B 108.6 . . ? O1 C73 C72 105.6(15) . . ? O1 C73 H73A 110.6 . . ? C72 C73 H73A 110.6 . . ? O1 C73 H73B 110.6 . . ? C72 C73 H73B 110.6 . . ? H73A C73 H73B 108.8 . . ? C74 O2 C77 104(2) . . ? O2 C74 C75 106.2(15) . . ? O2 C74 H74A 110.5 . . ? C75 C74 H74A 110.5 . . ? O2 C74 H74B 110.5 . . ? C75 C74 H74B 110.5 . . ? H74A C74 H74B 108.7 . . ? C76 C75 C74 103(2) . . ? C76 C75 H75A 111.2 . . ? C74 C75 H75A 111.3 . . ? C76 C75 H75B 111.3 . . ? C74 C75 H75B 111.3 . . ? H75A C75 H75B 109.2 . . ? C75 C76 C77 106.3(13) . . ? C75 C76 H76A 110.5 . . ? C77 C76 H76A 110.5 . . ? C75 C76 H76B 110.5 . . ? C77 C76 H76B 110.5 . . ? H76A C76 H76B 108.7 . . ? O2 C77 C76 107.0(14) . . ? O2 C77 H77A 110.3 . . ? C76 C77 H77A 110.3 . . ? O2 C77 H77B 110.3 . . ? C76 C77 H77B 110.3 . . ? H77A C77 H77B 108.6 . . ? C78 O3 C81 106.7(19) . . ? O3 C78 C79 108.9(15) . . ? O3 C78 H78A 109.9 . . ? C79 C78 H78A 109.9 . . ? O3 C78 H78B 109.9 . . ? C79 C78 H78B 109.9 . . ? H78A C78 H78B 108.3 . . ? C78 C79 C80 105.2(15) . . ? C78 C79 H79A 110.7 . . ? C80 C79 H79A 110.7 . . ? C78 C79 H79B 110.7 . . ? C80 C79 H79B 110.7 . . ? H79A C79 H79B 108.8 . . ? C79 C80 C81 104(2) . . ? C79 C80 H80A 111.0 . . ? C81 C80 H80A 111.0 . . ? C79 C80 H80B 111.0 . . ? C81 C80 H80B 111.0 . . ? H80A C80 H80B 109.0 . . ? O3 C81 C80 105.7(15) . . ? O3 C81 H81A 110.6 . . ? C80 C81 H81A 110.6 . . ? O3 C81 H81B 110.6 . . ? C80 C81 H81B 110.6 . . ? H81A C81 H81B 108.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4C O2 0.86 2.16 3.02(3) 171.8 1_545 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 20.59 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.348 _refine_diff_density_min -1.298 _refine_diff_density_rms 0.244 # Attachment 'complex 5.cif' data_51128b _database_code_depnum_ccdc_archive 'CCDC 676383' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H80 N6 O2 S2 Y2' _chemical_formula_weight 1111.20 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' 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' H H 0.0000 0.0000 '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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.340(3) _cell_length_b 20.754(5) _cell_length_c 15.309(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.351(3) _cell_angle_gamma 90.00 _cell_volume 3241.6(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1814 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 18.45 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 1.884 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7653 _exptl_absorpt_correction_T_max 0.8639 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5702 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5702 _reflns_number_gt 3602 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5702 _refine_ls_number_parameters 310 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 0.934 _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 Y1 Y 0.61492(4) 1.048188(16) 0.60653(2) 0.03840(14) Uani 1 1 d . . . S1 S 0.65356(10) 0.97136(4) 0.46346(6) 0.0411(3) Uani 1 1 d . . . N1 N 0.6076(3) 0.94000(13) 0.64362(19) 0.0376(7) Uani 1 1 d . . . N2 N 0.5719(3) 1.01043(14) 0.74591(19) 0.0444(8) Uani 1 1 d . . . N3 N 0.5606(3) 0.89883(15) 0.78042(19) 0.0464(8) Uani 1 1 d D . . H3' H 0.564(4) 0.9121(18) 0.8326(14) 0.056 Uiso 1 1 d D . . C1 C 0.7532(6) 1.1585(2) 0.6368(4) 0.0872(18) Uani 1 1 d . . . H1A H 0.8355 1.1552 0.6716 0.105 Uiso 1 1 calc R . . C2 C 0.7250(6) 1.1529(2) 0.5470(4) 0.0728(14) Uani 1 1 d . . . H2A H 0.7858 1.1455 0.5095 0.087 Uiso 1 1 calc R . . C3 C 0.5934(6) 1.1598(2) 0.5211(3) 0.0655(13) Uani 1 1 d . . . H3A H 0.5495 1.1574 0.4632 0.079 Uiso 1 1 calc R . . C4 C 0.5362(5) 1.1710(2) 0.5945(4) 0.0717(14) Uani 1 1 d . . . H4A H 0.4476 1.1779 0.5954 0.086 Uiso 1 1 calc R . . C5 C 0.6346(8) 1.1700(2) 0.6663(4) 0.0847(17) Uani 1 1 d . . . H5A H 0.6239 1.1760 0.7249 0.102 Uiso 1 1 calc R . . C6 C 0.7168(4) 0.90338(17) 0.5276(2) 0.0427(9) Uani 1 1 d . . . C7 C 0.8001(4) 0.8607(2) 0.4943(3) 0.0584(12) Uani 1 1 d . . . H7A H 0.8173 0.8666 0.4371 0.070 Uiso 1 1 calc R . . C8 C 0.8579(5) 0.8100(2) 0.5439(3) 0.0705(14) Uani 1 1 d . . . H8A H 0.9140 0.7821 0.5207 0.085 Uiso 1 1 calc R . . C9 C 0.8313(4) 0.8011(2) 0.6282(3) 0.0660(13) Uani 1 1 d . . . H9A H 0.8698 0.7669 0.6622 0.079 Uiso 1 1 calc R . . C10 C 0.7492(4) 0.84187(18) 0.6626(3) 0.0512(11) Uani 1 1 d . . . H10A H 0.7334 0.8350 0.7199 0.061 Uiso 1 1 calc R . . C11 C 0.6883(4) 0.89358(17) 0.6141(2) 0.0400(9) Uani 1 1 d . . . C12 C 0.5803(4) 0.94901(18) 0.7251(2) 0.0401(9) Uani 1 1 d . . . C13 C 0.4758(4) 0.84465(17) 0.7494(2) 0.0438(10) Uani 1 1 d . . . H13A H 0.5023 0.8283 0.6949 0.053 Uiso 1 1 calc R . . C14 C 0.4958(4) 0.79152(19) 0.8175(3) 0.0592(12) Uani 1 1 d . . . H14A H 0.4798 0.8085 0.8738 0.071 Uiso 1 1 calc R . . H14B H 0.5864 0.7774 0.8251 0.071 Uiso 1 1 calc R . . C15 C 0.4076(5) 0.7341(2) 0.7928(3) 0.0758(15) Uani 1 1 d . . . H15A H 0.4300 0.7137 0.7403 0.091 Uiso 1 1 calc R . . H15B H 0.4202 0.7029 0.8406 0.091 Uiso 1 1 calc R . . C16 C 0.2669(5) 0.7553(2) 0.7755(4) 0.0897(17) Uani 1 1 d . . . H16A H 0.2429 0.7723 0.8296 0.108 Uiso 1 1 calc R . . H16B H 0.2114 0.7183 0.7576 0.108 Uiso 1 1 calc R . . C17 C 0.2438(5) 0.8063(3) 0.7038(4) 0.0928(17) Uani 1 1 d . . . H17A H 0.1531 0.8202 0.6958 0.111 Uiso 1 1 calc R . . H17B H 0.2604 0.7882 0.6483 0.111 Uiso 1 1 calc R . . C18 C 0.3336(4) 0.8642(2) 0.7284(3) 0.0684(13) Uani 1 1 d . . . H18A H 0.3223 0.8945 0.6796 0.082 Uiso 1 1 calc R . . H18B H 0.3086 0.8856 0.7794 0.082 Uiso 1 1 calc R . . C19 C 0.5120(4) 1.03244(18) 0.8206(2) 0.0529(11) Uani 1 1 d . . . H19A H 0.4823 0.9945 0.8499 0.064 Uiso 1 1 calc R . . C20 C 0.6111(5) 1.0676(3) 0.8866(3) 0.0854(17) Uani 1 1 d . . . H20A H 0.6504 1.1017 0.8565 0.103 Uiso 1 1 calc R . . H20B H 0.6802 1.0379 0.9108 0.103 Uiso 1 1 calc R . . C21 C 0.5501(6) 1.0970(3) 0.9632(3) 0.101(2) Uani 1 1 d . . . H21A H 0.5251 1.0625 0.9999 0.121 Uiso 1 1 calc R . . H21B H 0.6152 1.1233 0.9997 0.121 Uiso 1 1 calc R . . C22 C 0.4342(6) 1.1367(2) 0.9308(3) 0.0825(16) Uani 1 1 d . . . H22A H 0.4612 1.1745 0.9009 0.099 Uiso 1 1 calc R . . H22B H 0.3951 1.1513 0.9808 0.099 Uiso 1 1 calc R . . C23 C 0.3344(5) 1.0999(3) 0.8683(3) 0.0856(16) Uani 1 1 d . . . H23A H 0.2612 1.1279 0.8461 0.103 Uiso 1 1 calc R . . H23B H 0.3014 1.0644 0.8994 0.103 Uiso 1 1 calc R . . C24 C 0.3960(4) 1.0739(2) 0.7901(3) 0.0707(14) Uani 1 1 d . . . H24A H 0.3309 1.0491 0.7512 0.085 Uiso 1 1 calc R . . H24B H 0.4223 1.1098 0.7565 0.085 Uiso 1 1 calc R . . O1 O 0.8433(3) 1.02090(13) 0.65940(18) 0.0561(7) Uani 1 1 d . . . C25 C 0.8979(5) 1.0018(3) 0.7476(3) 0.0822(16) Uani 1 1 d . . . H25A H 0.8525 0.9641 0.7649 0.099 Uiso 1 1 calc R . . H25B H 0.8892 1.0363 0.7890 0.099 Uiso 1 1 calc R . . C26 C 1.0364(6) 0.9869(4) 0.7483(4) 0.135(3) Uani 1 1 d U . . H26A H 1.0599 0.9465 0.7787 0.162 Uiso 1 1 calc R . . H26B H 1.0918 1.0208 0.7777 0.162 Uiso 1 1 calc R . . C27 C 1.0508(6) 0.9823(4) 0.6549(4) 0.135(3) Uani 1 1 d U . . H27A H 1.1359 0.9984 0.6462 0.162 Uiso 1 1 calc R . . H27B H 1.0425 0.9379 0.6351 0.162 Uiso 1 1 calc R . . C28 C 0.9477(4) 1.0211(3) 0.6068(3) 0.0728(14) Uani 1 1 d . . . H28A H 0.9176 1.0029 0.5487 0.087 Uiso 1 1 calc R . . H28B H 0.9782 1.0647 0.5997 0.087 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 Y1 0.0454(2) 0.0322(2) 0.0390(2) -0.00062(17) 0.01072(16) -0.00431(19) S1 0.0460(6) 0.0390(5) 0.0403(5) -0.0003(4) 0.0136(5) 0.0005(4) N1 0.0439(19) 0.0331(18) 0.0386(17) 0.0014(14) 0.0150(14) 0.0002(14) N2 0.060(2) 0.036(2) 0.0411(19) -0.0045(15) 0.0179(16) -0.0028(16) N3 0.064(2) 0.042(2) 0.0340(17) 0.0030(16) 0.0110(17) -0.0098(17) C1 0.091(5) 0.043(3) 0.112(5) 0.006(3) -0.030(4) -0.029(3) C2 0.086(4) 0.047(3) 0.091(4) 0.005(3) 0.032(3) -0.018(3) C3 0.091(4) 0.041(3) 0.059(3) 0.009(2) -0.004(3) -0.014(3) C4 0.067(4) 0.036(3) 0.110(4) 0.000(3) 0.010(4) 0.002(2) C5 0.142(6) 0.040(3) 0.074(4) -0.011(3) 0.024(4) -0.019(3) C6 0.048(3) 0.037(2) 0.044(2) -0.0054(18) 0.0122(19) 0.0016(19) C7 0.068(3) 0.057(3) 0.057(3) 0.000(2) 0.029(2) 0.014(2) C8 0.070(3) 0.058(3) 0.089(4) 0.000(3) 0.031(3) 0.026(3) C9 0.068(3) 0.054(3) 0.081(3) 0.020(2) 0.026(3) 0.027(2) C10 0.051(3) 0.045(2) 0.060(3) 0.013(2) 0.017(2) 0.013(2) C11 0.040(2) 0.035(2) 0.046(2) 0.0033(18) 0.0095(18) -0.0001(18) C12 0.043(2) 0.036(2) 0.041(2) 0.0042(19) 0.0085(18) -0.0013(19) C13 0.055(3) 0.036(2) 0.043(2) 0.0040(18) 0.0159(19) -0.0025(19) C14 0.071(3) 0.047(3) 0.063(3) 0.011(2) 0.023(2) 0.001(2) C15 0.104(5) 0.049(3) 0.081(3) 0.011(2) 0.033(3) -0.014(3) C16 0.098(5) 0.069(4) 0.112(4) 0.002(3) 0.048(4) -0.032(3) C17 0.052(3) 0.086(4) 0.136(5) 0.007(4) 0.005(3) -0.013(3) C18 0.052(3) 0.057(3) 0.094(4) 0.005(3) 0.008(3) -0.001(2) C19 0.078(3) 0.043(2) 0.043(2) -0.0011(19) 0.028(2) 0.000(2) C20 0.085(4) 0.118(4) 0.051(3) -0.029(3) 0.005(3) 0.022(3) C21 0.107(5) 0.132(5) 0.062(3) -0.041(3) 0.006(3) 0.011(4) C22 0.102(4) 0.075(4) 0.079(3) -0.025(3) 0.038(3) 0.004(3) C23 0.082(4) 0.095(4) 0.086(4) -0.028(3) 0.032(3) 0.016(3) C24 0.061(3) 0.093(4) 0.062(3) -0.030(3) 0.021(2) 0.005(3) O1 0.0418(18) 0.0700(19) 0.0585(18) 0.0051(15) 0.0143(15) -0.0035(14) C25 0.053(3) 0.132(5) 0.059(3) 0.006(3) 0.000(2) 0.000(3) C26 0.057(4) 0.259(9) 0.089(4) 0.054(5) 0.014(3) 0.026(5) C27 0.063(4) 0.228(8) 0.121(5) 0.053(6) 0.034(4) 0.035(5) C28 0.042(3) 0.106(4) 0.074(3) 0.006(3) 0.022(3) -0.008(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 Y1 N1 2.320(3) . ? Y1 N2 2.382(3) . ? Y1 O1 2.435(3) . ? Y1 C3 2.652(4) . ? Y1 C4 2.672(4) . ? Y1 C2 2.680(4) . ? Y1 C5 2.685(4) . ? Y1 C1 2.699(4) . ? Y1 S1 2.7899(11) . ? Y1 C12 2.806(4) . ? Y1 S1 2.8377(13) 3_676 ? S1 C6 1.781(4) . ? S1 Y1 2.8376(13) 3_676 ? N1 C12 1.337(4) . ? N1 C11 1.396(4) . ? N2 C12 1.320(4) . ? N2 C19 1.460(4) . ? N3 C12 1.378(4) . ? N3 C13 1.457(5) . ? N3 H3' 0.842(18) . ? C1 C2 1.363(6) . ? C1 C5 1.395(7) . ? C1 H1A 0.9300 . ? C2 C3 1.362(6) . ? C2 H2A 0.9300 . ? C3 C4 1.371(6) . ? C3 H3A 0.9300 . ? C4 C5 1.371(7) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.388(5) . ? C6 C11 1.418(5) . ? C7 C8 1.377(5) . ? C7 H7A 0.9300 . ? C8 C9 1.375(5) . ? C8 H8A 0.9300 . ? C9 C10 1.363(5) . ? C9 H9A 0.9300 . ? C10 C11 1.395(5) . ? C10 H10A 0.9300 . ? C13 C14 1.508(5) . ? C13 C18 1.509(6) . ? C13 H13A 0.9800 . ? C14 C15 1.511(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.501(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.516(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.526(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C24 1.488(6) . ? C19 C20 1.506(6) . ? C19 H19A 0.9800 . ? C20 C21 1.544(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.473(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.498(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.542(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? O1 C25 1.433(5) . ? O1 C28 1.448(5) . ? C25 C26 1.463(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.465(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.439(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 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 N1 Y1 N2 56.23(10) . . ? N1 Y1 O1 76.23(10) . . ? N2 Y1 O1 86.43(10) . . ? N1 Y1 C3 164.30(12) . . ? N2 Y1 C3 135.74(14) . . ? O1 Y1 C3 111.49(14) . . ? N1 Y1 C4 156.64(14) . . ? N2 Y1 C4 106.05(15) . . ? O1 Y1 C4 120.84(13) . . ? C3 Y1 C4 29.84(13) . . ? N1 Y1 C2 154.18(15) . . ? N2 Y1 C2 136.28(14) . . ? O1 Y1 C2 81.90(15) . . ? C3 Y1 C2 29.59(14) . . ? C4 Y1 C2 49.07(16) . . ? N1 Y1 C5 146.25(14) . . ? N2 Y1 C5 91.11(13) . . ? O1 Y1 C5 95.17(18) . . ? C3 Y1 C5 48.77(15) . . ? C4 Y1 C5 29.65(15) . . ? C2 Y1 C5 48.68(16) . . ? N1 Y1 C1 144.69(14) . . ? N2 Y1 C1 107.22(16) . . ? O1 Y1 C1 71.46(15) . . ? C3 Y1 C1 48.96(15) . . ? C4 Y1 C1 49.46(17) . . ? C2 Y1 C1 29.35(14) . . ? C5 Y1 C1 30.04(16) . . ? N1 Y1 S1 69.73(7) . . ? N2 Y1 S1 125.92(8) . . ? O1 Y1 S1 82.72(7) . . ? C3 Y1 S1 97.10(11) . . ? C4 Y1 S1 124.87(13) . . ? C2 Y1 S1 94.22(12) . . ? C5 Y1 S1 142.47(12) . . ? C1 Y1 S1 118.68(17) . . ? N1 Y1 C12 28.25(10) . . ? N2 Y1 C12 27.98(9) . . ? O1 Y1 C12 80.38(10) . . ? C3 Y1 C12 161.93(15) . . ? C4 Y1 C12 132.44(15) . . ? C2 Y1 C12 157.00(16) . . ? C5 Y1 C12 118.74(13) . . ? C1 Y1 C12 129.11(15) . . ? S1 Y1 C12 97.95(8) . . ? N1 Y1 S1 83.41(8) . 3_676 ? N2 Y1 S1 88.72(8) . 3_676 ? O1 Y1 S1 158.20(7) . 3_676 ? C3 Y1 S1 86.57(12) . 3_676 ? C4 Y1 S1 80.91(12) . 3_676 ? C2 Y1 S1 115.53(14) . 3_676 ? C5 Y1 S1 106.17(17) . 3_676 ? C1 Y1 S1 130.15(13) . 3_676 ? S1 Y1 S1 82.99(3) . 3_676 ? C12 Y1 S1 85.40(8) . 3_676 ? C6 S1 Y1 96.12(12) . . ? C6 S1 Y1 110.11(13) . 3_676 ? Y1 S1 Y1 97.01(3) . 3_676 ? C12 N1 C11 128.8(3) . . ? C12 N1 Y1 96.5(2) . . ? C11 N1 Y1 122.9(2) . . ? C12 N2 C19 122.9(3) . . ? C12 N2 Y1 94.2(2) . . ? C19 N2 Y1 139.8(2) . . ? C12 N3 C13 121.6(3) . . ? C12 N3 H3' 110(3) . . ? C13 N3 H3' 119(3) . . ? C2 C1 C5 106.6(5) . . ? C2 C1 Y1 74.6(3) . . ? C5 C1 Y1 74.4(3) . . ? C2 C1 H1A 126.7 . . ? C5 C1 H1A 126.7 . . ? Y1 C1 H1A 116.6 . . ? C3 C2 C1 109.0(5) . . ? C3 C2 Y1 74.1(3) . . ? C1 C2 Y1 76.1(3) . . ? C3 C2 H2A 125.5 . . ? C1 C2 H2A 125.5 . . ? Y1 C2 H2A 116.3 . . ? C2 C3 C4 108.8(4) . . ? C2 C3 Y1 76.3(3) . . ? C4 C3 Y1 75.9(2) . . ? C2 C3 H3A 125.6 . . ? C4 C3 H3A 125.6 . . ? Y1 C3 H3A 114.4 . . ? C5 C4 C3 107.0(5) . . ? C5 C4 Y1 75.7(3) . . ? C3 C4 Y1 74.3(2) . . ? C5 C4 H4A 126.5 . . ? C3 C4 H4A 126.5 . . ? Y1 C4 H4A 115.8 . . ? C4 C5 C1 108.7(5) . . ? C4 C5 Y1 74.7(3) . . ? C1 C5 Y1 75.5(3) . . ? C4 C5 H5A 125.7 . . ? C1 C5 H5A 125.7 . . ? Y1 C5 H5A 116.1 . . ? C7 C6 C11 119.2(4) . . ? C7 C6 S1 119.8(3) . . ? C11 C6 S1 121.0(3) . . ? C8 C7 C6 121.6(4) . . ? C8 C7 H7A 119.2 . . ? C6 C7 H7A 119.2 . . ? C9 C8 C7 119.1(4) . . ? C9 C8 H8A 120.5 . . ? C7 C8 H8A 120.5 . . ? C10 C9 C8 120.7(4) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C9 C10 C11 121.9(4) . . ? C9 C10 H10A 119.0 . . ? C11 C10 H10A 119.0 . . ? C10 C11 N1 126.9(3) . . ? C10 C11 C6 117.5(3) . . ? N1 C11 C6 115.4(3) . . ? N2 C12 N1 113.1(3) . . ? N2 C12 N3 124.1(3) . . ? N1 C12 N3 122.9(3) . . ? N2 C12 Y1 57.84(18) . . ? N1 C12 Y1 55.24(17) . . ? N3 C12 Y1 177.6(3) . . ? N3 C13 C14 109.3(3) . . ? N3 C13 C18 112.1(3) . . ? C14 C13 C18 111.3(3) . . ? N3 C13 H13A 108.0 . . ? C14 C13 H13A 108.0 . . ? C18 C13 H13A 108.0 . . ? C13 C14 C15 113.2(4) . . ? C13 C14 H14A 108.9 . . ? C15 C14 H14A 108.9 . . ? C13 C14 H14B 108.9 . . ? C15 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C16 C15 C14 110.0(4) . . ? C16 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? C16 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C15 C16 C17 111.5(4) . . ? C15 C16 H16A 109.3 . . ? C17 C16 H16A 109.3 . . ? C15 C16 H16B 109.3 . . ? C17 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C16 C17 C18 110.7(4) . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? C13 C18 C17 112.0(4) . . ? C13 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? C13 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N2 C19 C24 111.0(3) . . ? N2 C19 C20 110.4(4) . . ? C24 C19 C20 110.9(4) . . ? N2 C19 H19A 108.2 . . ? C24 C19 H19A 108.2 . . ? C20 C19 H19A 108.2 . . ? C19 C20 C21 112.6(4) . . ? C19 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C20 112.1(4) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 C23 111.6(4) . . ? C21 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? C21 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C24 110.2(4) . . ? C22 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C19 C24 C23 111.9(4) . . ? C19 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? C19 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C25 O1 C28 108.0(3) . . ? C25 O1 Y1 126.2(3) . . ? C28 O1 Y1 125.8(3) . . ? O1 C25 C26 107.5(4) . . ? O1 C25 H25A 110.2 . . ? C26 C25 H25A 110.2 . . ? O1 C25 H25B 110.2 . . ? C26 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? C25 C26 C27 105.1(5) . . ? C25 C26 H26A 110.7 . . ? C27 C26 H26A 110.7 . . ? C25 C26 H26B 110.7 . . ? C27 C26 H26B 110.7 . . ? H26A C26 H26B 108.8 . . ? C28 C27 C26 106.2(5) . . ? C28 C27 H27A 110.5 . . ? C26 C27 H27A 110.5 . . ? C28 C27 H27B 110.5 . . ? C26 C27 H27B 110.5 . . ? H27A C27 H27B 108.7 . . ? C27 C28 O1 105.7(4) . . ? C27 C28 H28A 110.6 . . ? O1 C28 H28A 110.6 . . ? C27 C28 H28B 110.6 . . ? O1 C28 H28B 110.6 . . ? H28A C28 H28B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.518 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.065 # Attachment 'complex_2.cif' data_60110a _database_code_depnum_ccdc_archive 'CCDC 676384' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H38 N3 S Yb' _chemical_formula_weight 633.72 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 15.321(4) _cell_length_b 11.728(3) _cell_length_c 15.762(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.182(4) _cell_angle_gamma 90.00 _cell_volume 2757.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 376 _cell_measurement_theta_min 2.209 _cell_measurement_theta_max 23.768 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 3.488 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7218 _exptl_absorpt_correction_T_max 0.8449 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15818 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 26.01 _reflns_number_total 5412 _reflns_number_gt 3683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5412 _refine_ls_number_parameters 291 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1416 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Yb1 Yb 0.15390(2) 0.40749(3) 0.86386(2) 0.03808(14) Uani 1 1 d . A . S1 S 0.24881(15) 0.25689(19) 0.97173(13) 0.0495(5) Uani 1 1 d . . . N1 N 0.2742(4) 0.3667(5) 0.8037(4) 0.0350(14) Uani 1 1 d . A . N2 N 0.3155(5) 0.2368(6) 0.7063(4) 0.0502(18) Uani 1 1 d D A . H2' H 0.316(6) 0.224(8) 0.654(2) 0.060 Uiso 1 1 d D . . N3 N 0.2285(5) 0.3929(6) 0.6546(4) 0.0486(18) Uani 1 1 d D A . H3' H 0.231(6) 0.364(7) 0.608(3) 0.058 Uiso 1 1 d D . . C1 C 0.2335(8) 0.6045(7) 0.8915(7) 0.061(3) Uani 1 1 d . A . H1 H 0.2806 0.6180 0.8646 0.073 Uiso 1 1 calc R . . C2 C 0.2404(7) 0.5558(8) 0.9722(6) 0.060(3) Uani 1 1 d . A . H2 H 0.2931 0.5309 1.0094 0.072 Uiso 1 1 calc R . . C3 C 0.1553(7) 0.5502(9) 0.9884(6) 0.064(3) Uani 1 1 d . A . H3 H 0.1406 0.5197 1.0378 0.076 Uiso 1 1 calc R . . C4 C 0.0959(8) 0.5986(9) 0.9176(7) 0.077(3) Uani 1 1 d . A . H4 H 0.0346 0.6078 0.9123 0.092 Uiso 1 1 calc R . . C5 C 0.1427(7) 0.6305(9) 0.8566(6) 0.065(3) Uani 1 1 d . . . H5 H 0.1188 0.6631 0.8024 0.078 Uiso 1 1 calc R A . C6 C -0.0130(10) 0.3418(16) 0.8490(11) 0.042(5) Uiso 0.466(19) 1 d PG A 1 H6 H -0.0422 0.3680 0.8908 0.050 Uiso 0.466(19) 1 calc PR A 1 C7 C -0.0094(11) 0.3982(10) 0.7701(14) 0.064(6) Uiso 0.466(19) 1 d PG A 1 H7 H -0.0359 0.4678 0.7512 0.077 Uiso 0.466(19) 1 calc PR A 1 C8 C 0.0417(12) 0.330(2) 0.7251(7) 0.047(5) Uiso 0.466(19) 1 d PG A 1 H8 H 0.0546 0.3465 0.6716 0.057 Uiso 0.466(19) 1 calc PR A 1 C9 C 0.0698(10) 0.2309(14) 0.7762(14) 0.060(6) Uiso 0.466(19) 1 d PG A 1 H9 H 0.1043 0.1717 0.7620 0.072 Uiso 0.466(19) 1 calc PR A 1 C10 C 0.0360(11) 0.2384(13) 0.8527(10) 0.044(5) Uiso 0.466(19) 1 d PG A 1 H10 H 0.0444 0.1850 0.8974 0.053 Uiso 0.466(19) 1 calc PR A 1 C6' C 0.0577(12) 0.2246(10) 0.8189(14) 0.071(6) Uiso 0.534(19) 1 d PG A 2 H6' H 0.0836 0.1544 0.8370 0.086 Uiso 0.534(19) 1 calc PR A 2 C7' C 0.0096(14) 0.295(2) 0.8659(8) 0.071(6) Uiso 0.534(19) 1 d PG A 2 H7' H -0.0016 0.2783 0.9202 0.085 Uiso 0.534(19) 1 calc PR A 2 C8' C -0.0185(11) 0.3939(15) 0.8155(16) 0.087(7) Uiso 0.534(19) 1 d PG A 2 H8' H -0.0513 0.4540 0.8310 0.105 Uiso 0.534(19) 1 calc PR A 2 C9' C 0.0123(13) 0.3853(14) 0.7374(11) 0.064(6) Uiso 0.534(19) 1 d PG A 2 H9' H 0.0033 0.4388 0.6926 0.077 Uiso 0.534(19) 1 calc PR A 2 C10' C 0.0594(10) 0.2807(18) 0.7394(11) 0.055(5) Uiso 0.534(19) 1 d PG A 2 H10' H 0.0866 0.2536 0.6963 0.066 Uiso 0.534(19) 1 calc PR A 2 C11 C 0.3520(5) 0.3024(6) 0.9507(5) 0.0402(18) Uani 1 1 d . A . C12 C 0.4319(6) 0.2904(8) 1.0131(5) 0.056(2) Uani 1 1 d . . . H12A H 0.4312 0.2587 1.0671 0.068 Uiso 1 1 calc R . . C13 C 0.5104(7) 0.3245(10) 0.9961(6) 0.071(3) Uani 1 1 d . . . H13A H 0.5632 0.3166 1.0387 0.085 Uiso 1 1 calc R . . C14 C 0.5131(6) 0.3697(10) 0.9181(7) 0.071(3) Uani 1 1 d . . . H14A H 0.5681 0.3905 0.9072 0.085 Uiso 1 1 calc R . . C15 C 0.4372(6) 0.3855(8) 0.8553(6) 0.057(2) Uani 1 1 d . A . H15A H 0.4398 0.4210 0.8031 0.069 Uiso 1 1 calc R . . C16 C 0.3554(5) 0.3481(7) 0.8695(5) 0.0385(17) Uani 1 1 d . . . C17 C 0.2738(5) 0.3325(7) 0.7239(5) 0.0396(18) Uani 1 1 d . . . C18 C 0.3256(6) 0.1334(7) 0.7600(5) 0.046(2) Uani 1 1 d . . . H18A H 0.3076 0.1517 0.8142 0.056 Uiso 1 1 calc R A . C19 C 0.2655(8) 0.0403(8) 0.7147(7) 0.070(3) Uani 1 1 d . A . H19A H 0.2810 0.0225 0.6599 0.084 Uiso 1 1 calc R . . H19B H 0.2038 0.0666 0.7019 0.084 Uiso 1 1 calc R . . C20 C 0.2737(9) -0.0669(9) 0.7705(9) 0.090(4) Uani 1 1 d . . . H20A H 0.2529 -0.0508 0.8229 0.107 Uiso 1 1 calc R A . H20B H 0.2357 -0.1261 0.7384 0.107 Uiso 1 1 calc R . . C21 C 0.3661(10) -0.1080(9) 0.7945(9) 0.095(4) Uani 1 1 d . A . H21A H 0.3843 -0.1342 0.7428 0.114 Uiso 1 1 calc R . . H21B H 0.3698 -0.1721 0.8341 0.114 Uiso 1 1 calc R . . C22 C 0.4280(9) -0.0157(11) 0.8374(9) 0.100(4) Uani 1 1 d . . . H22A H 0.4893 -0.0430 0.8479 0.120 Uiso 1 1 calc R A . H22B H 0.4151 0.0022 0.8933 0.120 Uiso 1 1 calc R . . C23 C 0.4196(8) 0.0916(9) 0.7830(9) 0.084(4) Uani 1 1 d . A . H23A H 0.4579 0.1503 0.8152 0.101 Uiso 1 1 calc R . . H23B H 0.4397 0.0763 0.7301 0.101 Uiso 1 1 calc R . . C24 C 0.2060(8) 0.5135(9) 0.6561(6) 0.068(3) Uani 1 1 d . . . H24A H 0.1800 0.5258 0.7067 0.082 Uiso 1 1 calc R A . C25 C 0.1349(10) 0.5449(12) 0.5754(9) 0.104(4) Uani 1 1 d . A . H25A H 0.0898 0.4854 0.5635 0.124 Uiso 1 1 calc R . . H25B H 0.1057 0.6151 0.5862 0.124 Uiso 1 1 calc R . . C26 C 0.1748(13) 0.5602(13) 0.4971(8) 0.119(6) Uani 1 1 d . . . H26A H 0.1937 0.4865 0.4800 0.143 Uiso 1 1 calc R A . H26B H 0.1289 0.5893 0.4490 0.143 Uiso 1 1 calc R . . C27 C 0.2496(14) 0.6363(13) 0.5127(9) 0.128(6) Uani 1 1 d . A . H27A H 0.2298 0.7123 0.5238 0.153 Uiso 1 1 calc R . . H27B H 0.2744 0.6397 0.4614 0.153 Uiso 1 1 calc R . . C28 C 0.3232(12) 0.5962(12) 0.5920(13) 0.126(6) Uani 1 1 d . . . H28A H 0.3458 0.5222 0.5796 0.151 Uiso 1 1 calc R A . H28B H 0.3727 0.6498 0.6024 0.151 Uiso 1 1 calc R . . C29 C 0.2871(12) 0.5885(10) 0.6673(9) 0.108(5) Uani 1 1 d . A . H29A H 0.2713 0.6645 0.6829 0.129 Uiso 1 1 calc R . . H29B H 0.3331 0.5595 0.7152 0.129 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 Yb1 0.0314(2) 0.0505(2) 0.0326(2) -0.00236(16) 0.00769(13) -0.00162(18) S1 0.0562(14) 0.0586(14) 0.0356(11) 0.0120(10) 0.0144(9) -0.0014(11) N1 0.028(3) 0.049(4) 0.028(3) -0.003(3) 0.007(2) -0.005(3) N2 0.059(5) 0.063(5) 0.032(4) 0.001(3) 0.017(3) 0.008(4) N3 0.059(5) 0.063(5) 0.024(3) 0.000(3) 0.011(3) 0.010(4) C1 0.075(7) 0.045(5) 0.063(6) -0.015(4) 0.018(5) -0.011(5) C2 0.071(7) 0.050(5) 0.049(6) -0.015(4) -0.008(5) 0.007(5) C3 0.070(7) 0.076(6) 0.046(5) -0.006(5) 0.015(5) 0.012(6) C4 0.072(8) 0.095(8) 0.063(7) -0.016(6) 0.012(5) 0.035(6) C5 0.071(8) 0.061(6) 0.056(6) -0.008(5) 0.000(5) 0.022(5) C11 0.044(5) 0.044(5) 0.031(4) -0.006(3) 0.005(3) 0.005(4) C12 0.046(5) 0.078(6) 0.042(5) -0.001(4) 0.002(4) 0.010(5) C13 0.046(6) 0.102(9) 0.054(6) -0.007(6) -0.011(4) 0.004(6) C14 0.035(5) 0.106(8) 0.070(7) -0.003(6) 0.010(5) -0.008(5) C15 0.041(5) 0.076(7) 0.056(6) 0.002(5) 0.012(4) -0.006(5) C16 0.035(4) 0.047(5) 0.033(4) -0.006(3) 0.007(3) 0.000(4) C17 0.041(5) 0.052(5) 0.028(4) 0.002(3) 0.012(3) -0.004(4) C18 0.056(6) 0.050(5) 0.035(4) -0.002(4) 0.013(4) 0.005(4) C19 0.083(8) 0.056(6) 0.067(7) -0.010(5) 0.007(5) 0.004(6) C20 0.091(10) 0.068(8) 0.106(10) 0.007(6) 0.015(8) -0.009(7) C21 0.121(12) 0.059(7) 0.103(10) 0.014(6) 0.021(9) 0.015(7) C22 0.085(9) 0.084(9) 0.119(11) 0.023(8) -0.001(8) 0.016(8) C23 0.056(7) 0.066(7) 0.127(11) 0.020(6) 0.013(7) 0.002(6) C24 0.099(9) 0.069(7) 0.037(5) 0.010(5) 0.017(5) 0.018(6) C25 0.098(11) 0.108(9) 0.106(11) 0.038(9) 0.026(8) 0.037(9) C26 0.187(18) 0.102(10) 0.057(8) 0.021(7) 0.004(9) 0.045(11) C27 0.22(2) 0.087(9) 0.080(10) 0.025(8) 0.041(11) -0.032(12) C28 0.124(14) 0.107(11) 0.151(16) 0.048(10) 0.039(12) -0.041(9) C29 0.151(15) 0.074(8) 0.083(9) 0.005(7) -0.004(9) -0.028(9) _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 Yb1 N1 2.307(6) . ? Yb1 C3 2.577(9) . ? Yb1 C8' 2.581(17) . ? Yb1 C2 2.582(9) . ? Yb1 C7' 2.584(16) . ? Yb1 C7 2.602(16) . ? Yb1 C1 2.603(9) . ? Yb1 C9' 2.603(16) . ? Yb1 C6' 2.607(15) . ? Yb1 C8 2.618(15) . ? Yb1 C10' 2.619(14) . ? Yb1 C4 2.621(9) . ? S1 C11 1.770(8) . ? N1 C17 1.318(9) . ? N1 C16 1.443(9) . ? N2 C17 1.351(10) . ? N2 C18 1.466(10) . ? N2 H2' 0.83(2) . ? N3 C17 1.354(10) . ? N3 C24 1.458(11) . ? N3 H3' 0.82(2) . ? C1 C2 1.376(13) . ? C1 C5 1.408(13) . ? C1 H1 0.9300 . ? C2 C3 1.387(14) . ? C2 H2 0.9300 . ? C3 C4 1.390(14) . ? C3 H3 0.9300 . ? C4 C5 1.376(14) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.4200 . ? C6 C10 1.4200 . ? C6 H6 0.9300 . ? C7 C8 1.4200 . ? C7 H7 0.9300 . ? C8 C9 1.4200 . ? C8 H8 0.9300 . ? C9 C10 1.4200 . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C6' C10' 1.4200 . ? C6' C7' 1.4200 . ? C6' H6' 0.9300 . ? C7' C8' 1.4200 . ? C7' H7' 0.9300 . ? C8' C9' 1.4200 . ? C8' H8' 0.9300 . ? C9' C10' 1.4200 . ? C9' H9' 0.9300 . ? C10' H10' 0.9300 . ? C11 C12 1.392(11) . ? C11 C16 1.399(10) . ? C12 C13 1.352(13) . ? C12 H12A 0.9300 . ? C13 C14 1.348(14) . ? C13 H13A 0.9300 . ? C14 C15 1.357(13) . ? C14 H14A 0.9300 . ? C15 C16 1.394(11) . ? C15 H15A 0.9300 . ? C18 C23 1.486(14) . ? C18 C19 1.500(13) . ? C18 H18A 0.9800 . ? C19 C20 1.523(14) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.462(18) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.496(17) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.511(15) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C29 1.499(17) . ? C24 C25 1.520(16) . ? C24 H24A 0.9800 . ? C25 C26 1.508(18) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.43(2) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.55(2) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.42(2) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 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 N1 Yb1 C3 125.4(3) . . ? N1 Yb1 C8' 136.5(4) . . ? C3 Yb1 C8' 95.4(4) . . ? N1 Yb1 C2 94.2(3) . . ? C3 Yb1 C2 31.2(3) . . ? C8' Yb1 C2 125.0(4) . . ? N1 Yb1 C7' 131.7(5) . . ? C3 Yb1 C7' 100.5(5) . . ? C8' Yb1 C7' 31.92(18) . . ? C2 Yb1 C7' 130.4(4) . . ? N1 Yb1 C7 120.8(6) . . ? C3 Yb1 C7 107.4(5) . . ? C8' Yb1 C7 16.9(3) . . ? C2 Yb1 C7 133.3(4) . . ? C7' Yb1 C7 43.2(3) . . ? N1 Yb1 C1 82.2(3) . . ? C3 Yb1 C1 51.2(3) . . ? C8' Yb1 C1 120.9(4) . . ? C2 Yb1 C1 30.8(3) . . ? C7' Yb1 C1 145.3(6) . . ? C7 Yb1 C1 119.0(3) . . ? N1 Yb1 C9' 105.6(5) . . ? C3 Yb1 C9' 120.6(6) . . ? C8' Yb1 C9' 31.79(19) . . ? C2 Yb1 C9' 141.8(5) . . ? C7' Yb1 C9' 52.6(2) . . ? C7 Yb1 C9' 15.3(3) . . ? C1 Yb1 C9' 119.6(4) . . ? N1 Yb1 C6' 99.9(5) . . ? C3 Yb1 C6' 130.4(6) . . ? C8' Yb1 C6' 52.6(2) . . ? C2 Yb1 C6' 155.1(6) . . ? C7' Yb1 C6' 31.75(17) . . ? C7 Yb1 C6' 53.2(3) . . ? C1 Yb1 C6' 171.9(4) . . ? C9' Yb1 C6' 52.3(2) . . ? N1 Yb1 C8 91.0(4) . . ? C3 Yb1 C8 138.8(6) . . ? C8' Yb1 C8 45.5(3) . . ? C2 Yb1 C8 158.0(6) . . ? C7' Yb1 C8 55.3(3) . . ? C7 Yb1 C8 31.57(17) . . ? C1 Yb1 C8 130.0(5) . . ? C9' Yb1 C8 18.5(3) . . ? C6' Yb1 C8 42.6(3) . . ? N1 Yb1 C10' 86.1(3) . . ? C3 Yb1 C10' 147.8(4) . . ? C8' Yb1 C10' 52.4(2) . . ? C2 Yb1 C10' 172.1(6) . . ? C7' Yb1 C10' 52.4(2) . . ? C7 Yb1 C10' 41.9(3) . . ? C1 Yb1 C10' 141.9(5) . . ? C9' Yb1 C10' 31.56(16) . . ? C6' Yb1 C10' 31.53(16) . . ? C8 Yb1 C10' 14.3(3) . . ? N1 Yb1 C4 132.2(3) . . ? C3 Yb1 C4 31.0(3) . . ? C8' Yb1 C4 75.4(4) . . ? C2 Yb1 C4 51.0(4) . . ? C7' Yb1 C4 94.6(6) . . ? C7 Yb1 C4 82.3(5) . . ? C1 Yb1 C4 50.8(4) . . ? C9' Yb1 C4 92.8(6) . . ? C6' Yb1 C4 125.4(5) . . ? C8 Yb1 C4 111.2(6) . . ? C10' Yb1 C4 123.9(5) . . ? C11 S1 Yb1 93.5(3) . . ? C17 N1 C16 117.1(6) . . ? C17 N1 Yb1 128.7(5) . . ? C16 N1 Yb1 111.9(4) . . ? C17 N2 C18 124.1(6) . . ? C17 N2 H2' 117(6) . . ? C18 N2 H2' 114(6) . . ? C17 N3 C24 125.0(7) . . ? C17 N3 H3' 113(6) . . ? C24 N3 H3' 118(6) . . ? C2 C1 C5 108.2(10) . . ? C2 C1 Yb1 73.8(5) . . ? C5 C1 Yb1 75.1(6) . . ? C2 C1 H1 125.9 . . ? C5 C1 H1 125.9 . . ? Yb1 C1 H1 117.2 . . ? C1 C2 C3 108.2(9) . . ? C1 C2 Yb1 75.4(5) . . ? C3 C2 Yb1 74.2(6) . . ? C1 C2 H2 125.9 . . ? C3 C2 H2 125.9 . . ? Yb1 C2 H2 116.5 . . ? C2 C3 C4 107.6(10) . . ? C2 C3 Yb1 74.6(5) . . ? C4 C3 Yb1 76.2(6) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? Yb1 C3 H3 115.2 . . ? C5 C4 C3 108.8(10) . . ? C5 C4 Yb1 74.8(6) . . ? C3 C4 Yb1 72.7(6) . . ? C5 C4 H4 125.6 . . ? C3 C4 H4 125.6 . . ? Yb1 C4 H4 118.7 . . ? C4 C5 C1 107.1(10) . . ? C4 C5 Yb1 74.8(6) . . ? C1 C5 Yb1 73.6(5) . . ? C4 C5 H5 126.5 . . ? C1 C5 H5 126.5 . . ? Yb1 C5 H5 117.3 . . ? C7 C6 C10 108.0 . . ? C7 C6 Yb1 73.2(6) . . ? C10 C6 Yb1 75.7(6) . . ? C7 C6 H6 126.0 . . ? C10 C6 H6 126.0 . . ? Yb1 C6 H6 117.1 . . ? C8 C7 C6 108.0 . . ? C8 C7 Yb1 74.8(6) . . ? C6 C7 Yb1 75.3(5) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? Yb1 C7 H7 116.0 . . ? C7 C8 C9 108.0 . . ? C7 C8 Yb1 73.6(6) . . ? C9 C8 Yb1 75.8(6) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? Yb1 C8 H8 116.7 . . ? C8 C9 C10 108.0 . . ? C8 C9 Yb1 73.0(6) . . ? C10 C9 Yb1 74.8(5) . . ? C8 C9 H9 126.0 . . ? C10 C9 H9 126.0 . . ? Yb1 C9 H9 118.2 . . ? C6 C10 C9 108.0 . . ? C6 C10 Yb1 73.2(6) . . ? C9 C10 Yb1 74.3(5) . . ? C6 C10 H10 126.0 . . ? C9 C10 H10 126.0 . . ? Yb1 C10 H10 118.5 . . ? C10' C6' C7' 108.0 . . ? C10' C6' Yb1 74.7(6) . . ? C7' C6' Yb1 73.2(6) . . ? C10' C6' H6' 126.0 . . ? C7' C6' H6' 126.0 . . ? Yb1 C6' H6' 118.0 . . ? C8' C7' C6' 108.0 . . ? C8' C7' Yb1 73.9(6) . . ? C6' C7' Yb1 75.0(6) . . ? C8' C7' H7' 126.0 . . ? C6' C7' H7' 126.0 . . ? Yb1 C7' H7' 117.1 . . ? C7' C8' C9' 108.0 . . ? C7' C8' Yb1 74.1(6) . . ? C9' C8' Yb1 75.0(5) . . ? C7' C8' H8' 126.0 . . ? C9' C8' H8' 126.0 . . ? Yb1 C8' H8' 117.0 . . ? C8' C9' C10' 108.0 . . ? C8' C9' Yb1 73.3(6) . . ? C10' C9' Yb1 74.8(6) . . ? C8' C9' H9' 126.0 . . ? C10' C9' H9' 126.0 . . ? Yb1 C9' H9' 117.9 . . ? C9' C10' C6' 108.0 . . ? C9' C10' Yb1 73.6(6) . . ? C6' C10' Yb1 73.8(6) . . ? C9' C10' H10' 126.0 . . ? C6' C10' H10' 126.0 . . ? Yb1 C10' H10' 118.5 . . ? C12 C11 C16 118.4(8) . . ? C12 C11 S1 121.1(6) . . ? C16 C11 S1 120.5(6) . . ? C13 C12 C11 120.6(9) . . ? C13 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C14 C13 C12 120.7(9) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C13 C14 C15 121.3(9) . . ? C13 C14 H14A 119.3 . . ? C15 C14 H14A 119.3 . . ? C14 C15 C16 119.4(9) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C15 C16 C11 119.4(7) . . ? C15 C16 N1 119.7(7) . . ? C11 C16 N1 120.7(7) . . ? C15 C16 Yb1 147.0(6) . . ? C11 C16 Yb1 82.5(4) . . ? N1 C16 Yb1 42.9(3) . . ? N1 C17 N2 123.3(7) . . ? N1 C17 N3 120.1(7) . . ? N2 C17 N3 116.6(7) . . ? N2 C18 C23 112.5(8) . . ? N2 C18 C19 110.8(7) . . ? C23 C18 C19 109.4(8) . . ? N2 C18 H18A 108.0 . . ? C23 C18 H18A 108.0 . . ? C19 C18 H18A 108.0 . . ? C18 C19 C20 111.5(9) . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? C21 C20 C19 111.7(11) . . ? C21 C20 H20A 109.3 . . ? C19 C20 H20A 109.3 . . ? C21 C20 H20B 109.3 . . ? C19 C20 H20B 109.3 . . ? H20A C20 H20B 107.9 . . ? C20 C21 C22 110.8(10) . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C21 C22 C23 112.6(11) . . ? C21 C22 H22A 109.1 . . ? C23 C22 H22A 109.1 . . ? C21 C22 H22B 109.1 . . ? C23 C22 H22B 109.1 . . ? H22A C22 H22B 107.8 . . ? C18 C23 C22 111.5(10) . . ? C18 C23 H23A 109.3 . . ? C22 C23 H23A 109.3 . . ? C18 C23 H23B 109.3 . . ? C22 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? N3 C24 C29 112.3(10) . . ? N3 C24 C25 110.4(9) . . ? C29 C24 C25 111.9(10) . . ? N3 C24 H24A 107.3 . . ? C29 C24 H24A 107.3 . . ? C25 C24 H24A 107.3 . . ? C26 C25 C24 111.5(11) . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C27 C26 C25 113.1(13) . . ? C27 C26 H26A 109.0 . . ? C25 C26 H26A 109.0 . . ? C27 C26 H26B 109.0 . . ? C25 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? C26 C27 C28 110.9(11) . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C29 C28 C27 110.0(14) . . ? C29 C28 H28A 109.7 . . ? C27 C28 H28A 109.7 . . ? C29 C28 H28B 109.7 . . ? C27 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? C28 C29 C24 114.1(12) . . ? C28 C29 H29A 108.7 . . ? C24 C29 H29A 108.7 . . ? C28 C29 H29B 108.7 . . ? C24 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.530 _refine_diff_density_min -1.059 _refine_diff_density_rms 0.187 # Attachment 'complex 9.cif' data_f71204b _database_code_depnum_ccdc_archive 'CCDC 676385' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H53 N6 O S2 Yb' _chemical_formula_weight 810.99 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.186(8) _cell_length_b 14.485(7) _cell_length_c 16.207(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.977(8) _cell_angle_gamma 90.00 _cell_volume 3753(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3369 _cell_measurement_theta_min 3.093 _cell_measurement_theta_max 22.058 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 2.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6205 _exptl_absorpt_correction_T_max 0.6931 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15596 _diffrn_reflns_av_R_equivalents 0.0837 _diffrn_reflns_av_sigmaI/netI 0.1097 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6610 _reflns_number_gt 4042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0862P)^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 6610 _refine_ls_number_parameters 406 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0980 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1581 _refine_ls_wR_factor_gt 0.1456 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.912 _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 Yb1 Yb 0.04414(2) 0.28220(3) 0.37306(3) 0.04376(16) Uani 1 1 d . . . S1 S 0.16178(16) 0.18424(17) 0.30886(18) 0.0569(7) Uani 1 1 d . . . S2 S -0.08726(18) 0.39920(18) 0.36154(18) 0.0617(7) Uani 1 1 d . . . N1 N -0.0286(5) 0.1912(5) 0.2648(5) 0.0429(18) Uani 1 1 d . . . N2 N -0.1159(5) 0.0616(5) 0.2344(5) 0.052(2) Uani 1 1 d . . . H2B H -0.1662 0.0493 0.2111 0.062 Uiso 1 1 calc R . . N3 N -0.1587(5) 0.1908(5) 0.2967(5) 0.054(2) Uani 1 1 d . . . H3B H -0.1494 0.2480 0.3089 0.065 Uiso 1 1 calc R . . N4 N 0.0457(5) 0.3882(5) 0.2532(5) 0.0463(19) Uani 1 1 d . . . N5 N 0.0988(6) 0.5178(6) 0.1860(6) 0.072(3) Uani 1 1 d . . . H5B H 0.1320 0.5286 0.1507 0.087 Uiso 1 1 calc R . . N6 N 0.1833(5) 0.3972(6) 0.2370(6) 0.065(3) Uani 1 1 d . . . H6A H 0.1899 0.3464 0.2647 0.079 Uiso 1 1 calc R . . C1 C 0.1036(6) 0.1764(6) 0.2088(6) 0.048(2) Uani 1 1 d . . . C2 C 0.1431(8) 0.1711(7) 0.1378(8) 0.071(3) Uani 1 1 d . . . H2A H 0.2012 0.1722 0.1448 0.085 Uiso 1 1 calc R . . C3 C 0.0992(9) 0.1644(9) 0.0587(8) 0.080(4) Uani 1 1 d . . . H3A H 0.1275 0.1574 0.0133 0.096 Uiso 1 1 calc R . . C4 C 0.0138(10) 0.1679(8) 0.0463(7) 0.077(4) Uani 1 1 d . . . H4A H -0.0160 0.1659 -0.0076 0.092 Uiso 1 1 calc R . . C5 C -0.0283(7) 0.1746(7) 0.1140(6) 0.055(3) Uani 1 1 d . . . H5A H -0.0865 0.1769 0.1054 0.066 Uiso 1 1 calc R . . C6 C 0.0160(7) 0.1778(6) 0.1952(6) 0.049(2) Uani 1 1 d . . . C7 C -0.0999(6) 0.1471(6) 0.2641(5) 0.040(2) Uani 1 1 d . . . C8 C -0.0546(6) -0.0116(6) 0.2386(6) 0.050(2) Uani 1 1 d . . . H8A H 0.0008 0.0171 0.2438 0.059 Uiso 1 1 calc R . . C9 C -0.0674(9) -0.0667(8) 0.1601(8) 0.099(5) Uani 1 1 d . . . H9A H -0.0657 -0.0266 0.1133 0.148 Uiso 1 1 calc R . . H9B H -0.1208 -0.0969 0.1542 0.148 Uiso 1 1 calc R . . H9C H -0.0240 -0.1122 0.1623 0.148 Uiso 1 1 calc R . . C10 C -0.0559(9) -0.0714(8) 0.3128(8) 0.091(4) Uani 1 1 d . . . H10A H -0.0462 -0.0344 0.3625 0.137 Uiso 1 1 calc R . . H10B H -0.0128 -0.1174 0.3150 0.137 Uiso 1 1 calc R . . H10C H -0.1093 -0.1011 0.3088 0.137 Uiso 1 1 calc R . . C11 C -0.2388(6) 0.1528(7) 0.3146(7) 0.059(3) Uani 1 1 d . . . H11A H -0.2297 0.0879 0.3304 0.071 Uiso 1 1 calc R . . C12 C -0.3050(7) 0.1566(9) 0.2391(8) 0.088(4) Uani 1 1 d . . . H12A H -0.2870 0.1220 0.1946 0.132 Uiso 1 1 calc R . . H12B H -0.3145 0.2197 0.2220 0.132 Uiso 1 1 calc R . . H12C H -0.3559 0.1306 0.2523 0.132 Uiso 1 1 calc R . . C13 C -0.2626(9) 0.2040(10) 0.3890(10) 0.106(5) Uani 1 1 d . . . H13A H -0.2183 0.1986 0.4355 0.160 Uiso 1 1 calc R . . H13B H -0.3129 0.1779 0.4035 0.160 Uiso 1 1 calc R . . H13C H -0.2718 0.2680 0.3750 0.160 Uiso 1 1 calc R . . C14 C -0.1034(5) 0.4058(6) 0.2526(7) 0.049(3) Uani 1 1 d . . . C15 C -0.1841(7) 0.4142(7) 0.2085(9) 0.073(3) Uani 1 1 d . . . H15A H -0.2291 0.4186 0.2377 0.087 Uiso 1 1 calc R . . C16 C -0.1982(9) 0.4159(8) 0.1229(11) 0.093(5) Uani 1 1 d . . . H16A H -0.2523 0.4227 0.0944 0.112 Uiso 1 1 calc R . . C17 C -0.1342(9) 0.4079(9) 0.0803(8) 0.085(4) Uani 1 1 d . . . H17A H -0.1440 0.4084 0.0222 0.103 Uiso 1 1 calc R . . C18 C -0.0541(8) 0.3989(8) 0.1221(7) 0.072(3) Uani 1 1 d . . . H18A H -0.0101 0.3915 0.0920 0.086 Uiso 1 1 calc R . . C19 C -0.0378(6) 0.4007(6) 0.2090(6) 0.047(2) Uani 1 1 d . . . C20 C 0.1066(6) 0.4333(6) 0.2251(6) 0.052(3) Uani 1 1 d . . . C21 C 0.0409(8) 0.5897(7) 0.1980(7) 0.086(4) Uani 1 1 d DU . . H21A H -0.0119 0.5617 0.2076 0.103 Uiso 1 1 calc R . . C22 C 0.0252(12) 0.6469(11) 0.1228(10) 0.144(6) Uani 1 1 d DU . . H22A H 0.0044 0.6089 0.0756 0.216 Uiso 1 1 calc R . . H22B H 0.0764 0.6759 0.1137 0.216 Uiso 1 1 calc R . . H22C H -0.0154 0.6934 0.1296 0.216 Uiso 1 1 calc R . . C23 C 0.0722(11) 0.6498(11) 0.2691(11) 0.143(6) Uani 1 1 d DU . . H23A H 0.0828 0.6135 0.3192 0.214 Uiso 1 1 calc R . . H23B H 0.0311 0.6961 0.2751 0.214 Uiso 1 1 calc R . . H23C H 0.1231 0.6790 0.2595 0.214 Uiso 1 1 calc R . . C24 C 0.2571(8) 0.4352(9) 0.2077(10) 0.090(4) Uani 1 1 d . . . H24A H 0.2584 0.5022 0.2166 0.108 Uiso 1 1 calc R . . C25 C 0.2544(11) 0.4166(11) 0.1170(11) 0.131(6) Uani 1 1 d . . . H25A H 0.2061 0.4459 0.0860 0.196 Uiso 1 1 calc R . . H25B H 0.2513 0.3512 0.1073 0.196 Uiso 1 1 calc R . . H25C H 0.3040 0.4406 0.0992 0.196 Uiso 1 1 calc R . . C26 C 0.3329(10) 0.3934(14) 0.2587(14) 0.176(10) Uani 1 1 d . . . H26A H 0.3338 0.4086 0.3165 0.264 Uiso 1 1 calc R . . H26B H 0.3823 0.4171 0.2403 0.264 Uiso 1 1 calc R . . H26C H 0.3311 0.3275 0.2521 0.264 Uiso 1 1 calc R . . C27 C 0.0478(10) 0.2740(10) 0.5378(7) 0.085(4) Uani 1 1 d . . . H27A H 0.0592 0.3288 0.5673 0.101 Uiso 1 1 calc R . . C28 C 0.1054(9) 0.2111(13) 0.5195(9) 0.097(5) Uani 1 1 d . . . H28A H 0.1633 0.2153 0.5322 0.117 Uiso 1 1 calc R . . C29 C 0.0579(14) 0.1376(10) 0.4767(9) 0.101(5) Uani 1 1 d . . . H29A H 0.0795 0.0832 0.4584 0.121 Uiso 1 1 calc R . . C30 C -0.0203(11) 0.1599(10) 0.4678(8) 0.083(4) Uani 1 1 d . . . H30A H -0.0640 0.1247 0.4400 0.100 Uiso 1 1 calc R . . C31 C -0.0288(10) 0.2417(11) 0.5049(8) 0.086(4) Uani 1 1 d . . . H31A H -0.0793 0.2713 0.5075 0.103 Uiso 1 1 calc R . . C32 C 0.1318(9) 0.4790(9) 0.4532(9) 0.102(5) Uani 1 1 d . . . H32A H 0.1058 0.4764 0.5032 0.123 Uiso 1 1 calc R . . H32B H 0.0942 0.5107 0.4099 0.123 Uiso 1 1 calc R . . C33 C 0.2107(10) 0.5271(12) 0.4702(13) 0.133(7) Uani 1 1 d . . . H33A H 0.2186 0.5657 0.4232 0.159 Uiso 1 1 calc R . . H33B H 0.2126 0.5658 0.5193 0.159 Uiso 1 1 calc R . . C34 C 0.2728(13) 0.4593(13) 0.4837(15) 0.165(9) Uani 1 1 d . . . H34A H 0.2961 0.4565 0.5426 0.198 Uiso 1 1 calc R . . H34B H 0.3176 0.4740 0.4525 0.198 Uiso 1 1 calc R . . C35 C 0.2355(8) 0.3700(10) 0.4562(11) 0.112(5) Uani 1 1 d . . . H35A H 0.2624 0.3443 0.4119 0.135 Uiso 1 1 calc R . . H35B H 0.2413 0.3266 0.5023 0.135 Uiso 1 1 calc R . . O1 O 0.1492(4) 0.3882(5) 0.4266(5) 0.066(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 Yb1 0.0507(3) 0.0417(2) 0.0375(3) -0.0013(2) 0.00249(16) -0.0021(2) S1 0.0492(16) 0.0493(14) 0.070(2) -0.0002(13) 0.0023(12) 0.0082(11) S2 0.0692(19) 0.0533(16) 0.066(2) -0.0090(13) 0.0204(14) 0.0067(13) N1 0.048(5) 0.046(4) 0.034(5) -0.006(3) 0.003(3) -0.007(3) N2 0.047(5) 0.036(4) 0.069(6) -0.007(4) 0.001(4) -0.001(4) N3 0.043(5) 0.041(4) 0.080(7) 0.002(4) 0.017(4) -0.002(3) N4 0.038(5) 0.046(4) 0.057(6) 0.000(4) 0.013(4) -0.007(3) N5 0.075(7) 0.049(5) 0.102(8) 0.025(5) 0.043(5) 0.010(5) N6 0.048(6) 0.050(5) 0.101(8) 0.015(5) 0.021(5) 0.001(4) C1 0.056(7) 0.037(5) 0.052(7) 0.000(4) 0.016(5) -0.004(4) C2 0.076(8) 0.055(7) 0.092(10) -0.006(6) 0.040(7) 0.001(6) C3 0.100(11) 0.095(9) 0.052(9) -0.004(7) 0.034(7) -0.001(8) C4 0.126(12) 0.067(8) 0.040(7) -0.003(6) 0.018(7) 0.008(8) C5 0.066(7) 0.055(6) 0.044(7) -0.001(5) 0.008(5) -0.005(5) C6 0.076(8) 0.031(5) 0.044(7) 0.001(4) 0.021(5) -0.002(5) C7 0.044(6) 0.033(5) 0.040(6) 0.001(4) 0.002(4) 0.001(4) C8 0.055(6) 0.035(5) 0.058(7) 0.003(5) 0.006(5) 0.004(4) C9 0.135(12) 0.068(8) 0.083(10) -0.021(7) -0.014(8) 0.036(8) C10 0.114(11) 0.078(9) 0.088(10) 0.033(7) 0.034(8) 0.020(8) C11 0.052(7) 0.054(6) 0.076(8) 0.001(5) 0.023(5) -0.007(5) C12 0.058(8) 0.101(10) 0.104(11) 0.011(8) 0.009(7) 0.011(7) C13 0.096(11) 0.125(12) 0.112(13) -0.021(9) 0.059(9) -0.008(9) C14 0.027(5) 0.027(5) 0.090(8) -0.005(5) 0.004(5) 0.004(4) C15 0.058(8) 0.051(7) 0.110(12) 0.008(7) 0.017(7) 0.010(5) C16 0.066(9) 0.074(8) 0.127(14) -0.003(9) -0.028(9) 0.022(7) C17 0.099(11) 0.087(9) 0.060(9) 0.005(7) -0.019(8) 0.027(8) C18 0.088(9) 0.064(7) 0.063(9) 0.002(6) 0.010(6) 0.019(6) C19 0.058(7) 0.038(5) 0.046(7) 0.001(4) 0.009(5) 0.005(4) C20 0.060(7) 0.046(6) 0.051(7) 0.000(5) 0.014(5) 0.000(5) C21 0.110(9) 0.042(6) 0.115(10) 0.018(6) 0.049(8) 0.028(6) C22 0.188(14) 0.105(11) 0.146(14) 0.048(10) 0.051(11) 0.073(10) C23 0.168(14) 0.093(10) 0.162(15) -0.021(10) 0.011(11) 0.039(10) C24 0.066(9) 0.064(8) 0.145(14) 0.012(8) 0.036(8) -0.008(6) C25 0.149(16) 0.126(13) 0.137(17) -0.002(12) 0.086(13) -0.006(11) C26 0.048(10) 0.187(19) 0.29(3) 0.058(19) 0.015(13) -0.018(11) C27 0.102(11) 0.104(11) 0.045(8) 0.005(7) 0.001(7) -0.024(10) C28 0.073(9) 0.142(14) 0.070(10) 0.061(10) -0.008(7) 0.004(10) C29 0.168(17) 0.066(9) 0.071(11) 0.041(8) 0.026(10) 0.025(11) C30 0.117(12) 0.077(9) 0.048(8) 0.017(7) -0.010(7) -0.014(9) C31 0.103(12) 0.116(12) 0.045(8) 0.021(7) 0.031(7) 0.006(9) C32 0.110(12) 0.084(9) 0.118(13) -0.050(9) 0.032(9) -0.029(8) C33 0.100(13) 0.104(13) 0.21(2) -0.073(13) 0.075(13) -0.051(11) C34 0.129(17) 0.126(15) 0.21(2) -0.010(15) -0.061(15) -0.061(13) C35 0.071(10) 0.114(12) 0.134(14) 0.006(10) -0.039(8) -0.025(8) O1 0.063(5) 0.061(4) 0.069(5) -0.012(4) -0.008(4) -0.016(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 Yb1 O1 2.354(6) . ? Yb1 N1 2.356(7) . ? Yb1 N4 2.480(8) . ? Yb1 C28 2.634(11) . ? Yb1 C30 2.661(12) . ? Yb1 C31 2.663(11) . ? Yb1 C27 2.663(12) . ? Yb1 C29 2.672(11) . ? Yb1 S2 2.703(3) . ? Yb1 S1 2.709(3) . ? S1 C1 1.747(10) . ? S2 C14 1.747(11) . ? N1 C7 1.318(11) . ? N1 C6 1.444(12) . ? N2 C7 1.340(10) . ? N2 C8 1.446(11) . ? N2 H2B 0.8600 . ? N3 C7 1.321(11) . ? N3 C11 1.477(12) . ? N3 H3B 0.8600 . ? N4 C20 1.321(12) . ? N4 C19 1.438(12) . ? N5 C20 1.374(12) . ? N5 C21 1.435(13) . ? N5 H5B 0.8600 . ? N6 C20 1.333(12) . ? N6 C24 1.462(14) . ? N6 H6A 0.8600 . ? C1 C6 1.401(14) . ? C1 C2 1.403(14) . ? C2 C3 1.370(16) . ? C2 H2A 0.9300 . ? C3 C4 1.366(17) . ? C3 H3A 0.9300 . ? C4 C5 1.382(15) . ? C4 H4A 0.9300 . ? C5 C6 1.399(13) . ? C5 H5A 0.9300 . ? C8 C10 1.485(14) . ? C8 C9 1.488(14) . ? C8 H8A 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.496(14) . ? C11 C13 1.515(16) . ? C11 H11A 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C19 1.366(13) . ? C14 C15 1.392(14) . ? C15 C16 1.372(18) . ? C15 H15A 0.9300 . ? C16 C17 1.336(19) . ? C16 H16A 0.9300 . ? C17 C18 1.372(16) . ? C17 H17A 0.9300 . ? C18 C19 1.391(14) . ? C18 H18A 0.9300 . ? C21 C22 1.464(12) . ? C21 C23 1.470(12) . ? C21 H21A 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.49(2) . ? C24 C26 1.50(2) . ? C24 H24A 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C31 1.355(18) . ? C27 C28 1.369(19) . ? C27 H27A 0.9300 . ? C28 C29 1.43(2) . ? C28 H28A 0.9300 . ? C29 C30 1.292(19) . ? C29 H29A 0.9300 . ? C30 C31 1.345(18) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C32 O1 1.426(13) . ? C32 C33 1.442(17) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.40(2) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.467(18) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 O1 1.430(14) . ? C35 H35A 0.9700 . ? C35 H35B 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 Yb1 N1 152.5(3) . . ? O1 Yb1 N4 77.9(3) . . ? N1 Yb1 N4 80.1(2) . . ? O1 Yb1 C28 77.0(4) . . ? N1 Yb1 C28 121.7(5) . . ? N4 Yb1 C28 154.1(4) . . ? O1 Yb1 C30 123.2(3) . . ? N1 Yb1 C30 82.1(3) . . ? N4 Yb1 C30 156.5(4) . . ? C28 Yb1 C30 49.2(4) . . ? O1 Yb1 C31 103.5(4) . . ? N1 Yb1 C31 104.0(4) . . ? N4 Yb1 C31 145.6(4) . . ? C28 Yb1 C31 48.9(5) . . ? C30 Yb1 C31 29.3(4) . . ? O1 Yb1 C27 76.0(4) . . ? N1 Yb1 C27 130.7(3) . . ? N4 Yb1 C27 144.3(4) . . ? C28 Yb1 C27 30.0(4) . . ? C30 Yb1 C27 48.8(4) . . ? C31 Yb1 C27 29.5(4) . . ? O1 Yb1 C29 107.1(5) . . ? N1 Yb1 C29 90.7(5) . . ? N4 Yb1 C29 165.4(4) . . ? C28 Yb1 C29 31.2(4) . . ? C30 Yb1 C29 28.0(4) . . ? C31 Yb1 C29 47.7(5) . . ? C27 Yb1 C29 49.3(4) . . ? O1 Yb1 S2 97.56(19) . . ? N1 Yb1 S2 90.17(19) . . ? N4 Yb1 S2 70.23(18) . . ? C28 Yb1 S2 119.3(4) . . ? C30 Yb1 S2 94.7(4) . . ? C31 Yb1 S2 75.6(3) . . ? C27 Yb1 S2 89.5(4) . . ? C29 Yb1 S2 121.5(4) . . ? O1 Yb1 S1 88.4(2) . . ? N1 Yb1 S1 73.77(19) . . ? N4 Yb1 S1 85.96(18) . . ? C28 Yb1 S1 87.3(4) . . ? C30 Yb1 S1 103.6(4) . . ? C31 Yb1 S1 128.2(3) . . ? C27 Yb1 S1 117.0(4) . . ? C29 Yb1 S1 80.6(4) . . ? S2 Yb1 S1 153.43(9) . . ? C1 S1 Yb1 94.7(3) . . ? C14 S2 Yb1 95.5(3) . . ? C7 N1 C6 118.1(8) . . ? C7 N1 Yb1 127.8(6) . . ? C6 N1 Yb1 113.9(6) . . ? C7 N2 C8 124.6(8) . . ? C7 N2 H2B 117.7 . . ? C8 N2 H2B 117.7 . . ? C7 N3 C11 127.6(8) . . ? C7 N3 H3B 116.2 . . ? C11 N3 H3B 116.2 . . ? C20 N4 C19 117.4(8) . . ? C20 N4 Yb1 132.5(7) . . ? C19 N4 Yb1 110.1(5) . . ? C20 N5 C21 126.8(9) . . ? C20 N5 H5B 116.6 . . ? C21 N5 H5B 116.6 . . ? C20 N6 C24 126.6(9) . . ? C20 N6 H6A 116.7 . . ? C24 N6 H6A 116.7 . . ? C6 C1 C2 116.8(10) . . ? C6 C1 S1 122.1(7) . . ? C2 C1 S1 121.1(9) . . ? C3 C2 C1 122.4(12) . . ? C3 C2 H2A 118.8 . . ? C1 C2 H2A 118.8 . . ? C4 C3 C2 120.0(11) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 120.0(12) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C6 120.4(11) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 120.4(9) . . ? C5 C6 N1 119.7(9) . . ? C1 C6 N1 119.7(9) . . ? N1 C7 N3 116.7(8) . . ? N1 C7 N2 124.9(8) . . ? N3 C7 N2 118.4(8) . . ? N2 C8 C10 111.7(9) . . ? N2 C8 C9 110.4(8) . . ? C10 C8 C9 111.2(9) . . ? N2 C8 H8A 107.8 . . ? C10 C8 H8A 107.8 . . ? C9 C8 H8A 107.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C12 111.3(9) . . ? N3 C11 C13 108.3(9) . . ? C12 C11 C13 113.2(11) . . ? N3 C11 H11A 107.9 . . ? C12 C11 H11A 107.9 . . ? C13 C11 H11A 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 118.9(11) . . ? C19 C14 S2 120.9(7) . . ? C15 C14 S2 120.2(9) . . ? C16 C15 C14 121.0(12) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C17 C16 C15 120.1(12) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C18 120.1(13) . . ? C16 C17 H17A 119.9 . . ? C18 C17 H17A 119.9 . . ? C17 C18 C19 120.9(12) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? C14 C19 C18 118.9(10) . . ? C14 C19 N4 119.7(9) . . ? C18 C19 N4 121.1(9) . . ? N4 C20 N6 119.0(9) . . ? N4 C20 N5 125.4(9) . . ? N6 C20 N5 115.6(9) . . ? N5 C21 C22 109.3(10) . . ? N5 C21 C23 112.6(11) . . ? C22 C21 C23 108.2(12) . . ? N5 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? C23 C21 H21A 108.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N6 C24 C25 110.7(12) . . ? N6 C24 C26 108.0(12) . . ? C25 C24 C26 111.6(15) . . ? N6 C24 H24A 108.8 . . ? C25 C24 H24A 108.8 . . ? C26 C24 H24A 108.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C31 C27 C28 107.3(13) . . ? C31 C27 Yb1 75.2(7) . . ? C28 C27 Yb1 73.9(7) . . ? C31 C27 H27A 126.4 . . ? C28 C27 H27A 126.4 . . ? Yb1 C27 H27A 116.7 . . ? C27 C28 C29 105.6(13) . . ? C27 C28 Yb1 76.2(7) . . ? C29 C28 Yb1 75.9(7) . . ? C27 C28 H28A 127.2 . . ? C29 C28 H28A 127.2 . . ? Yb1 C28 H28A 113.5 . . ? C30 C29 C28 108.2(14) . . ? C30 C29 Yb1 75.5(8) . . ? C28 C29 Yb1 72.9(7) . . ? C30 C29 H29A 125.9 . . ? C28 C29 H29A 125.9 . . ? Yb1 C29 H29A 117.6 . . ? C29 C30 C31 109.7(14) . . ? C29 C30 Yb1 76.4(8) . . ? C31 C30 Yb1 75.4(7) . . ? C29 C30 H30A 125.1 . . ? C31 C30 H30A 125.1 . . ? Yb1 C30 H30A 115.0 . . ? C30 C31 C27 109.2(14) . . ? C30 C31 Yb1 75.3(7) . . ? C27 C31 Yb1 75.3(7) . . ? C30 C31 H31A 125.4 . . ? C27 C31 H31A 125.4 . . ? Yb1 C31 H31A 116.0 . . ? O1 C32 C33 107.0(12) . . ? O1 C32 H32A 110.3 . . ? C33 C32 H32A 110.3 . . ? O1 C32 H32B 110.3 . . ? C33 C32 H32B 110.3 . . ? H32A C32 H32B 108.6 . . ? C34 C33 C32 106.6(14) . . ? C34 C33 H33A 110.4 . . ? C32 C33 H33A 110.4 . . ? C34 C33 H33B 110.4 . . ? C32 C33 H33B 110.4 . . ? H33A C33 H33B 108.6 . . ? C33 C34 C35 108.6(14) . . ? C33 C34 H34A 110.0 . . ? C35 C34 H34A 110.0 . . ? C33 C34 H34B 110.0 . . ? C35 C34 H34B 110.0 . . ? H34A C34 H34B 108.3 . . ? O1 C35 C34 105.9(13) . . ? O1 C35 H35A 110.6 . . ? C34 C35 H35A 110.6 . . ? O1 C35 H35B 110.6 . . ? C34 C35 H35B 110.6 . . ? H35A C35 H35B 108.7 . . ? C32 O1 C35 107.3(9) . . ? C32 O1 Yb1 123.3(7) . . ? C35 O1 Yb1 127.9(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.807 _refine_diff_density_min -2.319 _refine_diff_density_rms 0.167 # Attachment 'complex 7.cif' data_f60509b _database_code_depnum_ccdc_archive 'CCDC 676386' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Gd2 N2 S2' _chemical_formula_weight 823.22 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' S S 0.1246 0.1234 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.413(6) _cell_length_b 10.823(4) _cell_length_c 17.526(6) _cell_angle_alpha 90.00 _cell_angle_beta 111.808(4) _cell_angle_gamma 90.00 _cell_volume 2890.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 942 _cell_measurement_theta_min 2.905 _cell_measurement_theta_max 27.030 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.892 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 4.718 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5380 _exptl_absorpt_correction_T_max 0.6498 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.92 _diffrn_reflns_number 11749 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5077 _reflns_number_gt 3556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^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 5077 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0684 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _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 Gd1 Gd 0.381820(18) 0.11440(3) 0.199307(18) 0.03778(10) Uani 1 1 d . . . Gd2 Gd 0.611627(18) 0.37819(3) 0.279421(19) 0.04166(10) Uani 1 1 d . . . S1 S 0.53997(11) 0.16152(15) 0.33390(10) 0.0486(4) Uani 1 1 d . . . S2 S 0.47760(12) 0.28826(15) 0.13617(11) 0.0531(4) Uani 1 1 d . . . N1 N 0.4003(3) -0.0074(4) 0.3289(3) 0.0448(13) Uani 1 1 d . . . H1B H 0.3496 -0.0458 0.3227 0.054 Uiso 1 1 calc R . . H1C H 0.4419 -0.0655 0.3370 0.054 Uiso 1 1 calc R . . N2 N 0.5949(3) 0.4936(4) 0.1482(3) 0.0514(14) Uani 1 1 d . . . H2B H 0.6272 0.5632 0.1612 0.062 Uiso 1 1 calc R . . H2C H 0.6161 0.4464 0.1175 0.062 Uiso 1 1 calc R . . C1 C 0.3567(8) -0.0056(7) 0.0609(5) 0.084(3) Uani 1 1 d . . . H1A H 0.3265 0.0281 0.0057 0.101 Uiso 1 1 calc R . . C2 C 0.3185(5) -0.0800(7) 0.1019(6) 0.076(2) Uani 1 1 d . . . H2A H 0.2573 -0.1080 0.0808 0.091 Uiso 1 1 calc R . . C3 C 0.3850(6) -0.1282(6) 0.1678(5) 0.067(2) Uani 1 1 d . . . H3A H 0.3784 -0.1947 0.2030 0.081 Uiso 1 1 calc R . . C4 C 0.4621(6) -0.0858(7) 0.1678(6) 0.078(3) Uani 1 1 d . . . H4A H 0.5201 -0.1165 0.2030 0.094 Uiso 1 1 calc R . . C5 C 0.4456(7) -0.0091(7) 0.1012(7) 0.088(3) Uani 1 1 d . . . H5A H 0.4892 0.0219 0.0800 0.105 Uiso 1 1 calc R . . C6 C 0.2437(4) 0.1675(7) 0.2428(5) 0.060(2) Uani 1 1 d . . . H6A H 0.2274 0.1208 0.2829 0.072 Uiso 1 1 calc R . . C7 C 0.2080(4) 0.1504(6) 0.1592(5) 0.061(2) Uani 1 1 d . . . H7A H 0.1616 0.0913 0.1301 0.073 Uiso 1 1 calc R . . C8 C 0.2371(4) 0.2468(6) 0.1231(5) 0.0565(18) Uani 1 1 d . . . H8A H 0.2136 0.2670 0.0643 0.068 Uiso 1 1 calc R . . C9 C 0.2906(4) 0.3243(6) 0.1855(5) 0.0533(18) Uani 1 1 d . . . H9A H 0.3105 0.4069 0.1774 0.064 Uiso 1 1 calc R . . C10 C 0.2951(4) 0.2752(6) 0.2604(5) 0.0577(19) Uani 1 1 d . . . H10A H 0.3193 0.3167 0.3139 0.069 Uiso 1 1 calc R . . C11 C 0.4245(4) 0.0721(5) 0.3985(4) 0.0440(15) Uani 1 1 d . . . C12 C 0.3838(5) 0.0693(6) 0.4550(4) 0.0572(18) Uani 1 1 d . . . H12A H 0.3392 0.0124 0.4484 0.069 Uiso 1 1 calc R . . C13 C 0.4079(5) 0.1484(6) 0.5201(4) 0.0610(19) Uani 1 1 d . . . H13A H 0.3791 0.1466 0.5569 0.073 Uiso 1 1 calc R . . C14 C 0.4744(5) 0.2304(6) 0.5310(4) 0.0585(19) Uani 1 1 d . . . H14A H 0.4920 0.2831 0.5761 0.070 Uiso 1 1 calc R . . C15 C 0.5154(4) 0.2355(6) 0.4755(4) 0.0527(17) Uani 1 1 d . . . H15A H 0.5607 0.2919 0.4837 0.063 Uiso 1 1 calc R . . C16 C 0.4909(4) 0.1587(5) 0.4079(4) 0.0451(15) Uani 1 1 d . . . C17 C 0.7220(6) 0.2342(10) 0.2352(7) 0.095(3) Uani 1 1 d . . . H17A H 0.7066 0.1864 0.1843 0.113 Uiso 1 1 calc R . . C18 C 0.7254(7) 0.1904(8) 0.3096(10) 0.107(4) Uani 1 1 d . . . H18A H 0.7130 0.1050 0.3205 0.129 Uiso 1 1 calc R . . C19 C 0.7657(6) 0.2750(11) 0.3677(7) 0.099(3) Uani 1 1 d . . . H19A H 0.7873 0.2602 0.4271 0.119 Uiso 1 1 calc R . . C20 C 0.7879(5) 0.3728(8) 0.3311(7) 0.081(3) Uani 1 1 d . . . H20A H 0.8275 0.4401 0.3597 0.098 Uiso 1 1 calc R . . C21 C 0.7609(6) 0.3480(9) 0.2500(7) 0.083(3) Uani 1 1 d . . . H21A H 0.7770 0.3960 0.2102 0.100 Uiso 1 1 calc R . . C22 C 0.5205(4) 0.4852(6) 0.3598(4) 0.0511(17) Uani 1 1 d . . . H22A H 0.4748 0.4451 0.3746 0.061 Uiso 1 1 calc R . . C23 C 0.6079(5) 0.4963(6) 0.4107(4) 0.0539(18) Uani 1 1 d . . . H23A H 0.6337 0.4661 0.4674 0.065 Uiso 1 1 calc R . . C24 C 0.6480(5) 0.5810(5) 0.3740(4) 0.0536(18) Uani 1 1 d . . . H24A H 0.7063 0.6177 0.4007 0.064 Uiso 1 1 calc R . . C25 C 0.5841(5) 0.6210(5) 0.3006(4) 0.0514(16) Uani 1 1 d . . . H25A H 0.5908 0.6890 0.2664 0.062 Uiso 1 1 calc R . . C26 C 0.5055(4) 0.5622(5) 0.2915(4) 0.0499(17) Uani 1 1 d . . . H26A H 0.4478 0.5825 0.2501 0.060 Uiso 1 1 calc R . . C27 C 0.5058(4) 0.5253(6) 0.1005(4) 0.0468(16) Uani 1 1 d . . . C28 C 0.4806(5) 0.6417(6) 0.0661(4) 0.0587(19) Uani 1 1 d . . . H28A H 0.5229 0.7024 0.0732 0.070 Uiso 1 1 calc R . . C29 C 0.3958(6) 0.6673(7) 0.0228(4) 0.064(2) Uani 1 1 d . . . H29A H 0.3798 0.7463 0.0016 0.076 Uiso 1 1 calc R . . C30 C 0.3337(5) 0.5795(7) 0.0097(5) 0.070(2) Uani 1 1 d . . . H30A H 0.2754 0.5978 -0.0212 0.084 Uiso 1 1 calc R . . C31 C 0.3568(5) 0.4617(7) 0.0422(4) 0.0600(19) Uani 1 1 d . . . H31A H 0.3136 0.4014 0.0317 0.072 Uiso 1 1 calc R . . C32 C 0.4424(4) 0.4326(6) 0.0897(4) 0.0487(16) 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 Gd1 0.03412(18) 0.03153(17) 0.0489(2) -0.00120(14) 0.01687(14) 0.00157(13) Gd2 0.03532(19) 0.03325(18) 0.0614(2) 0.00065(14) 0.02374(16) 0.00315(14) S1 0.0419(10) 0.0489(10) 0.0548(11) 0.0012(7) 0.0179(8) -0.0090(8) S2 0.0549(11) 0.0408(9) 0.0674(12) 0.0038(8) 0.0274(10) -0.0069(8) N1 0.045(3) 0.035(3) 0.054(3) -0.004(2) 0.018(3) -0.009(2) N2 0.048(4) 0.044(3) 0.071(4) -0.005(3) 0.033(3) -0.008(3) C1 0.153(10) 0.044(5) 0.054(6) -0.008(4) 0.039(6) 0.016(6) C2 0.057(5) 0.069(5) 0.095(7) -0.039(5) 0.021(5) -0.016(4) C3 0.105(7) 0.033(4) 0.080(6) -0.010(4) 0.053(5) -0.007(4) C4 0.061(6) 0.053(5) 0.109(8) -0.032(5) 0.019(5) 0.020(4) C5 0.115(8) 0.050(5) 0.150(10) -0.044(6) 0.109(8) -0.033(5) C6 0.046(4) 0.061(5) 0.085(6) 0.014(4) 0.037(4) 0.017(4) C7 0.031(4) 0.057(5) 0.089(6) 0.011(4) 0.017(4) 0.004(3) C8 0.034(4) 0.059(4) 0.070(5) 0.011(4) 0.011(4) 0.009(3) C9 0.045(4) 0.038(4) 0.080(6) 0.005(3) 0.026(4) 0.014(3) C10 0.046(4) 0.061(5) 0.072(5) -0.010(4) 0.028(4) 0.017(4) C11 0.038(4) 0.041(3) 0.049(4) 0.003(3) 0.012(3) -0.007(3) C12 0.054(5) 0.058(4) 0.063(5) -0.001(4) 0.025(4) -0.012(4) C13 0.068(5) 0.066(5) 0.058(5) -0.010(4) 0.033(4) -0.007(4) C14 0.067(5) 0.053(4) 0.053(5) -0.008(3) 0.018(4) -0.002(4) C15 0.051(4) 0.047(4) 0.051(5) 0.002(3) 0.008(3) -0.010(3) C16 0.042(4) 0.043(4) 0.047(4) 0.004(3) 0.014(3) -0.001(3) C17 0.062(6) 0.089(7) 0.149(10) -0.041(7) 0.058(7) 0.013(5) C18 0.077(7) 0.040(5) 0.236(16) 0.021(7) 0.095(9) 0.022(5) C19 0.068(7) 0.122(9) 0.118(9) 0.064(8) 0.048(7) 0.054(6) C20 0.034(4) 0.080(6) 0.123(8) 0.004(6) 0.021(5) 0.001(4) C21 0.056(5) 0.099(7) 0.113(8) 0.039(6) 0.053(6) 0.028(5) C22 0.048(4) 0.047(4) 0.069(5) -0.005(3) 0.034(4) 0.001(3) C23 0.059(5) 0.051(4) 0.052(5) 0.001(3) 0.022(4) -0.004(4) C24 0.052(5) 0.040(4) 0.068(5) -0.008(3) 0.022(4) -0.008(3) C25 0.064(5) 0.031(3) 0.068(5) 0.002(3) 0.034(4) 0.005(3) C26 0.048(4) 0.042(4) 0.061(5) -0.003(3) 0.021(4) 0.016(3) C27 0.058(5) 0.040(4) 0.054(4) -0.006(3) 0.034(4) -0.005(3) C28 0.085(6) 0.043(4) 0.060(5) -0.009(3) 0.040(4) -0.002(4) C29 0.085(6) 0.056(5) 0.059(5) 0.004(4) 0.037(5) 0.021(4) C30 0.062(5) 0.084(6) 0.066(5) 0.018(4) 0.026(4) 0.017(5) C31 0.053(5) 0.070(5) 0.057(5) 0.002(4) 0.022(4) -0.009(4) C32 0.052(4) 0.051(4) 0.047(4) -0.004(3) 0.022(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 Gd1 N1 2.545(5) . ? Gd1 C1 2.645(7) . ? Gd1 C2 2.666(7) . ? Gd1 C8 2.669(6) . ? Gd1 C5 2.679(7) . ? Gd1 C9 2.682(6) . ? Gd1 C3 2.687(6) . ? Gd1 C4 2.697(7) . ? Gd1 C7 2.701(6) . ? Gd1 C10 2.708(6) . ? Gd1 C6 2.708(6) . ? Gd1 S1 2.8307(18) . ? Gd2 N2 2.541(5) . ? Gd2 C23 2.653(6) . ? Gd2 C22 2.671(6) . ? Gd2 C19 2.670(8) . ? Gd2 C24 2.680(6) . ? Gd2 C18 2.677(8) . ? Gd2 C20 2.692(7) . ? Gd2 C26 2.706(6) . ? Gd2 C21 2.706(7) . ? Gd2 C17 2.711(7) . ? Gd2 C25 2.715(6) . ? Gd2 S2 2.826(2) . ? S1 C16 1.764(6) . ? S2 C32 1.758(7) . ? N1 C11 1.424(7) . ? N2 C27 1.431(8) . ? C1 C5 1.365(12) . ? C1 C2 1.375(11) . ? C2 C3 1.364(11) . ? C3 C4 1.346(10) . ? C4 C5 1.376(12) . ? C6 C7 1.374(10) . ? C6 C10 1.404(9) . ? C7 C8 1.394(8) . ? C8 C9 1.399(9) . ? C9 C10 1.393(9) . ? C11 C16 1.400(8) . ? C11 C12 1.385(8) . ? C12 C13 1.362(9) . ? C13 C14 1.364(9) . ? C14 C15 1.375(8) . ? C15 C16 1.379(8) . ? C17 C18 1.369(13) . ? C17 C21 1.368(11) . ? C18 C19 1.345(13) . ? C19 C20 1.356(11) . ? C20 C21 1.350(11) . ? C22 C23 1.384(9) . ? C22 C26 1.403(9) . ? C23 C24 1.415(8) . ? C24 C25 1.392(9) . ? C25 C26 1.394(9) . ? C27 C28 1.391(8) . ? C27 C32 1.406(8) . ? C28 C29 1.344(10) . ? C29 C30 1.349(10) . ? C30 C31 1.391(9) . ? C31 C32 1.377(9) . ? 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 N1 Gd1 C1 119.4(2) . . ? N1 Gd1 C2 93.0(2) . . ? C1 Gd1 C2 30.0(2) . . ? N1 Gd1 C8 120.92(19) . . ? C1 Gd1 C8 89.9(3) . . ? C2 Gd1 C8 92.3(2) . . ? N1 Gd1 C5 111.7(3) . . ? C1 Gd1 C5 29.7(3) . . ? C2 Gd1 C5 49.2(2) . . ? C8 Gd1 C5 115.7(3) . . ? N1 Gd1 C9 113.38(19) . . ? C1 Gd1 C9 116.2(3) . . ? C2 Gd1 C9 122.6(3) . . ? C8 Gd1 C9 30.31(19) . . ? C5 Gd1 C9 134.6(3) . . ? N1 Gd1 C3 70.9(2) . . ? C1 Gd1 C3 48.7(2) . . ? C2 Gd1 C3 29.5(2) . . ? C8 Gd1 C3 120.2(3) . . ? C5 Gd1 C3 48.6(2) . . ? C9 Gd1 C3 149.5(3) . . ? N1 Gd1 C4 82.0(3) . . ? C1 Gd1 C4 48.7(3) . . ? C2 Gd1 C4 48.6(2) . . ? C8 Gd1 C4 137.8(2) . . ? C5 Gd1 C4 29.7(3) . . ? C9 Gd1 C4 163.9(3) . . ? C3 Gd1 C4 29.0(2) . . ? N1 Gd1 C7 94.1(2) . . ? C1 Gd1 C7 92.4(3) . . ? C2 Gd1 C7 79.9(2) . . ? C8 Gd1 C7 30.09(18) . . ? C5 Gd1 C7 122.1(3) . . ? C9 Gd1 C7 49.8(2) . . ? C3 Gd1 C7 100.7(2) . . ? C4 Gd1 C7 127.7(2) . . ? N1 Gd1 C10 83.43(19) . . ? C1 Gd1 C10 138.8(3) . . ? C2 Gd1 C10 128.6(2) . . ? C8 Gd1 C10 49.6(2) . . ? C5 Gd1 C10 164.3(3) . . ? C9 Gd1 C10 29.95(19) . . ? C3 Gd1 C10 139.6(2) . . ? C4 Gd1 C10 164.9(3) . . ? C7 Gd1 C10 49.5(2) . . ? N1 Gd1 C6 72.13(19) . . ? C1 Gd1 C6 120.1(3) . . ? C2 Gd1 C6 100.4(2) . . ? C8 Gd1 C6 49.1(2) . . ? C5 Gd1 C6 148.7(3) . . ? C9 Gd1 C6 49.3(2) . . ? C3 Gd1 C6 110.3(2) . . ? C4 Gd1 C6 138.7(3) . . ? C7 Gd1 C6 29.4(2) . . ? C10 Gd1 C6 30.04(19) . . ? N1 Gd1 S1 65.25(11) . . ? C1 Gd1 S1 129.4(3) . . ? C2 Gd1 S1 134.0(2) . . ? C8 Gd1 S1 133.67(16) . . ? C5 Gd1 S1 99.7(3) . . ? C9 Gd1 S1 103.37(16) . . ? C3 Gd1 S1 105.4(2) . . ? C4 Gd1 S1 87.06(18) . . ? C7 Gd1 S1 138.07(18) . . ? C10 Gd1 S1 90.50(16) . . ? C6 Gd1 S1 109.35(18) . . ? N2 Gd2 C23 121.24(18) . . ? N2 Gd2 C22 111.78(18) . . ? C23 Gd2 C22 30.14(19) . . ? N2 Gd2 C19 119.4(2) . . ? C23 Gd2 C19 91.2(3) . . ? C22 Gd2 C19 118.1(3) . . ? N2 Gd2 C24 94.67(18) . . ? C23 Gd2 C24 30.78(18) . . ? C22 Gd2 C24 50.1(2) . . ? C19 Gd2 C24 92.2(3) . . ? N2 Gd2 C18 112.7(3) . . ? C23 Gd2 C18 115.7(4) . . ? C22 Gd2 C18 135.4(3) . . ? C19 Gd2 C18 29.1(3) . . ? C24 Gd2 C18 121.4(4) . . ? N2 Gd2 C20 93.2(3) . . ? C23 Gd2 C20 95.0(3) . . ? C22 Gd2 C20 125.1(3) . . ? C19 Gd2 C20 29.3(2) . . ? C24 Gd2 C20 81.1(2) . . ? C18 Gd2 C20 48.2(3) . . ? N2 Gd2 C26 81.54(18) . . ? C23 Gd2 C26 49.8(2) . . ? C22 Gd2 C26 30.24(18) . . ? C19 Gd2 C26 139.6(3) . . ? C24 Gd2 C26 49.5(2) . . ? C18 Gd2 C26 164.9(4) . . ? C20 Gd2 C26 129.2(2) . . ? N2 Gd2 C21 71.8(2) . . ? C23 Gd2 C21 122.6(3) . . ? C22 Gd2 C21 151.4(3) . . ? C19 Gd2 C21 47.9(3) . . ? C24 Gd2 C21 102.0(3) . . ? C18 Gd2 C21 48.0(3) . . ? C20 Gd2 C21 29.0(2) . . ? C26 Gd2 C21 139.4(2) . . ? N2 Gd2 C17 83.3(3) . . ? C23 Gd2 C17 139.3(3) . . ? C22 Gd2 C17 164.7(3) . . ? C19 Gd2 C17 48.4(3) . . ? C24 Gd2 C17 128.9(3) . . ? C18 Gd2 C17 29.4(3) . . ? C20 Gd2 C17 48.3(3) . . ? C26 Gd2 C17 164.4(3) . . ? C21 Gd2 C17 29.2(2) . . ? N2 Gd2 C25 71.36(18) . . ? C23 Gd2 C25 49.9(2) . . ? C22 Gd2 C25 49.75(19) . . ? C19 Gd2 C25 119.7(3) . . ? C24 Gd2 C25 29.90(19) . . ? C18 Gd2 C25 147.9(3) . . ? C20 Gd2 C25 100.8(2) . . ? C26 Gd2 C25 29.81(18) . . ? C21 Gd2 C25 110.6(3) . . ? C17 Gd2 C25 139.3(3) . . ? N2 Gd2 S2 65.06(12) . . ? C23 Gd2 S2 132.47(16) . . ? C22 Gd2 S2 102.38(16) . . ? C19 Gd2 S2 128.9(3) . . ? C24 Gd2 S2 138.79(16) . . ? C18 Gd2 S2 99.8(3) . . ? C20 Gd2 S2 132.5(2) . . ? C26 Gd2 S2 90.67(15) . . ? C21 Gd2 S2 104.5(3) . . ? C17 Gd2 S2 86.0(2) . . ? C25 Gd2 S2 109.92(15) . . ? C16 S1 Gd1 94.7(2) . . ? C16 S1 Gd2 126.9(2) . . ? Gd1 S1 Gd2 103.12(6) . . ? C32 S2 Gd2 96.8(2) . . ? C32 S2 Gd1 128.2(2) . . ? Gd2 S2 Gd1 103.66(6) . . ? C11 N1 Gd1 110.8(3) . . ? C27 N2 Gd2 112.9(4) . . ? C5 C1 C2 108.7(8) . . ? C5 C1 Gd1 76.5(5) . . ? C2 C1 Gd1 75.8(5) . . ? C3 C2 C1 106.9(8) . . ? C3 C2 Gd1 76.1(4) . . ? C1 C2 Gd1 74.2(4) . . ? C4 C3 C2 109.0(8) . . ? C4 C3 Gd1 75.9(4) . . ? C2 C3 Gd1 74.4(4) . . ? C3 C4 C5 108.5(8) . . ? C3 C4 Gd1 75.1(4) . . ? C5 C4 Gd1 74.5(4) . . ? C4 C5 C1 106.9(7) . . ? C4 C5 Gd1 75.9(4) . . ? C1 C5 Gd1 73.8(4) . . ? C7 C6 C10 109.3(6) . . ? C7 C6 Gd1 75.0(4) . . ? C10 C6 Gd1 75.0(3) . . ? C6 C7 C8 107.5(7) . . ? C6 C7 Gd1 75.6(4) . . ? C8 C7 Gd1 73.7(4) . . ? C9 C8 C7 108.4(7) . . ? C9 C8 Gd1 75.4(4) . . ? C7 C8 Gd1 76.2(4) . . ? C10 C9 C8 107.9(6) . . ? C10 C9 Gd1 76.1(3) . . ? C8 C9 Gd1 74.3(4) . . ? C9 C10 C6 107.0(7) . . ? C9 C10 Gd1 74.0(3) . . ? C6 C10 Gd1 75.0(4) . . ? C16 C11 C12 119.5(6) . . ? C16 C11 N1 117.6(5) . . ? C12 C11 N1 122.9(6) . . ? C13 C12 C11 121.2(7) . . ? C12 C13 C14 119.6(6) . . ? C13 C14 C15 120.3(6) . . ? C16 C15 C14 121.3(6) . . ? C15 C16 C11 118.1(6) . . ? C15 C16 S1 123.6(5) . . ? C11 C16 S1 118.2(5) . . ? C18 C17 C21 106.3(10) . . ? C18 C17 Gd2 73.9(5) . . ? C21 C17 Gd2 75.2(4) . . ? C19 C18 C17 108.6(9) . . ? C19 C18 Gd2 75.2(5) . . ? C17 C18 Gd2 76.7(5) . . ? C18 C19 C20 108.5(10) . . ? C18 C19 Gd2 75.7(6) . . ? C20 C19 Gd2 76.2(5) . . ? C21 C20 C19 107.6(9) . . ? C21 C20 Gd2 76.1(4) . . ? C19 C20 Gd2 74.5(5) . . ? C20 C21 C17 109.0(8) . . ? C20 C21 Gd2 75.0(4) . . ? C17 C21 Gd2 75.6(4) . . ? C23 C22 C26 108.0(6) . . ? C23 C22 Gd2 74.2(4) . . ? C26 C22 Gd2 76.2(3) . . ? C22 C23 C24 108.0(6) . . ? C22 C23 Gd2 75.7(4) . . ? C24 C23 Gd2 75.7(4) . . ? C25 C24 C23 107.7(6) . . ? C25 C24 Gd2 76.4(4) . . ? C23 C24 Gd2 73.5(4) . . ? C24 C25 C26 108.1(6) . . ? C24 C25 Gd2 73.7(4) . . ? C26 C25 Gd2 74.7(3) . . ? C25 C26 C22 108.2(6) . . ? C25 C26 Gd2 75.5(3) . . ? C22 C26 Gd2 73.5(3) . . ? C28 C27 C32 120.1(7) . . ? C28 C27 N2 123.0(6) . . ? C32 C27 N2 116.9(5) . . ? C29 C28 C27 120.6(7) . . ? C28 C29 C30 120.6(7) . . ? C29 C30 C31 120.2(8) . . ? C32 C31 C30 121.2(7) . . ? C31 C32 C27 117.1(6) . . ? C31 C32 S2 124.7(5) . . ? C27 C32 S2 118.2(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.460 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.117