Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Xian-He Bu' _publ_contact_author_address ; Department of Chemistry Nankai University Tianjin 300071 CHINA ; _publ_contact_author_email BUXH@NANKAI.EDU.CN _publ_section_title ; Arenedisulfonate-Lanthanide Supramolecular Architectures with Phenanthroline as Co-ligand: Syntheses, Structures, and Fluorescence Properties ; loop_ _publ_author_name 'Xian-He Bu' 'Bo-Wen Hu' 'Xin Hu' 'Fu-Chen Liu' 'Yong-Fei Zeng' ; Jiong-Peng Zhao ; data_1 _database_code_depnum_ccdc_archive 'CCDC 637255' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H35 Eu N4 O14 S3' _chemical_formula_weight 1031.85 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9869(10) _cell_length_b 12.7263(10) _cell_length_c 13.6184(11) _cell_angle_alpha 88.2440(10) _cell_angle_beta 75.7960(10) _cell_angle_gamma 77.0680(10) _cell_volume 1962.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6186 _cell_measurement_theta_min 2.2246 _cell_measurement_theta_max 28.4702 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 1.740 _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 1.835 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 10253 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6794 _reflns_number_gt 6034 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^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 6794 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 1.605720(15) 0.826980(13) 0.728188(13) 0.02583(8) Uani 1 1 d . . . S1 S 1.53987(10) 0.75848(9) 1.00293(8) 0.0411(3) Uani 1 1 d . . . O1 O 1.5964(3) 0.7638(2) 0.8947(2) 0.0446(7) Uani 1 1 d . . . N1 N 1.7510(3) 0.9240(2) 0.7949(3) 0.0361(8) Uani 1 1 d . . . C1 C 1.7685(4) 0.9126(4) 0.8870(3) 0.0479(11) Uani 1 1 d . . . H1A H 1.7401 0.8588 0.9264 0.057 Uiso 1 1 calc R . . O1W O 1.5026(3) 0.9871(3) 0.8387(4) 0.1013(16) Uani 1 1 d . . . S2 S 1.91386(8) 0.67911(8) 0.70284(8) 0.0341(2) Uani 1 1 d . . . N2 N 1.7442(3) 0.9316(2) 0.5957(2) 0.0340(7) Uani 1 1 d . . . O2W O 1.4855(3) 0.9710(2) 0.6427(3) 0.0645(10) Uani 1 1 d . . . O2 O 1.6281(3) 0.7306(3) 1.0613(2) 0.0548(8) Uani 1 1 d . . . C2 C 1.8268(4) 0.9761(4) 0.9293(4) 0.0555(12) Uani 1 1 d . . . H2A H 1.8383 0.9635 0.9941 0.067 Uiso 1 1 calc R . . S3 S 1.54871(9) 0.75622(8) 0.47978(7) 0.0337(2) Uani 1 1 d . . . N3 N 1.5629(3) 0.6288(2) 0.7384(2) 0.0288(7) Uani 1 1 d . . . O3 O 1.4513(3) 0.8546(2) 1.0401(2) 0.0552(8) Uani 1 1 d . . . O3W O 1.6824(3) 0.8389(2) 0.2070(2) 0.0641(9) Uani 1 1 d . . . C3 C 1.8663(4) 1.0567(4) 0.8735(4) 0.0583(14) Uani 1 1 d . . . H3A H 1.9013 1.1028 0.9012 0.070 Uiso 1 1 calc R . . O4 O 1.7907(2) 0.70928(19) 0.69360(19) 0.0334(6) Uani 1 1 d . . . N4 N 1.3833(3) 0.8085(2) 0.7804(2) 0.0340(7) Uani 1 1 d . . . C4 C 1.8539(4) 1.0701(3) 0.7742(4) 0.0474(11) Uani 1 1 d . . . O4W O 1.9374(5) 0.7864(5) 0.1257(4) 0.1264(19) Uani 1 1 d . . . O5 O 1.9187(3) 0.6554(2) 0.8063(2) 0.0524(8) Uani 1 1 d . . . C5 C 1.8982(4) 1.1502(4) 0.7084(5) 0.0613(14) Uani 1 1 d . . . H5A H 1.9292 1.2009 0.7344 0.074 Uiso 1 1 calc R . . O5W O 1.9191(6) 0.6100(5) 1.0074(4) 0.145(2) Uani 1 1 d . . . O6 O 1.9830(2) 0.7541(2) 0.6549(2) 0.0507(8) Uani 1 1 d . . . C6 C 1.8957(4) 1.1531(4) 0.6112(5) 0.0616(15) Uani 1 1 d . . . H6A H 1.9250 1.2058 0.5707 0.074 Uiso 1 1 calc R . . O7 O 1.6047(2) 0.7569(2) 0.5644(2) 0.0394(7) Uani 1 1 d . . . C7 C 1.8490(4) 1.0767(3) 0.5672(4) 0.0472(11) Uani 1 1 d . . . O8 O 1.6363(3) 0.7324(2) 0.3849(2) 0.0457(7) Uani 1 1 d . . . C8 C 1.8569(4) 1.0692(4) 0.4638(4) 0.0533(13) Uani 1 1 d . . . H8A H 1.8931 1.1157 0.4196 0.064 Uiso 1 1 calc R . . O9 O 1.4605(3) 0.8549(2) 0.4786(2) 0.0440(7) Uani 1 1 d . . . C9 C 1.8117(4) 0.9938(4) 0.4275(4) 0.0494(11) Uani 1 1 d . . . H9A H 1.8187 0.9863 0.3584 0.059 Uiso 1 1 calc R . . C10 C 1.7546(4) 0.9279(3) 0.4968(3) 0.0432(10) Uani 1 1 d . . . H10A H 1.7217 0.8782 0.4717 0.052 Uiso 1 1 calc R . . C11 C 1.7945(3) 1.0028(3) 0.6319(3) 0.0361(9) Uani 1 1 d . . . C12 C 1.7979(3) 0.9995(3) 0.7360(3) 0.0364(9) Uani 1 1 d . . . C13 C 1.6473(4) 0.5407(3) 0.7172(3) 0.0365(9) Uani 1 1 d . . . H13A H 1.7249 0.5487 0.6993 0.044 Uiso 1 1 calc R . . C14 C 1.6289(4) 0.4360(3) 0.7197(3) 0.0397(10) Uani 1 1 d . . . H14A H 1.6924 0.3768 0.7053 0.048 Uiso 1 1 calc R . . C15 C 1.5156(4) 0.4227(3) 0.7437(3) 0.0403(10) Uani 1 1 d . . . H15A H 1.5008 0.3539 0.7454 0.048 Uiso 1 1 calc R . . C16 C 1.4218(4) 0.5132(3) 0.7658(3) 0.0338(9) Uani 1 1 d . . . C17 C 1.3015(4) 0.5048(4) 0.7908(3) 0.0453(11) Uani 1 1 d . . . H17A H 1.2840 0.4371 0.7926 0.054 Uiso 1 1 calc R . . C18 C 1.2131(4) 0.5927(4) 0.8119(3) 0.0464(11) Uani 1 1 d . . . H18A H 1.1353 0.5851 0.8284 0.056 Uiso 1 1 calc R . . C19 C 1.2371(3) 0.6981(3) 0.8092(3) 0.0361(9) Uani 1 1 d . . . C20 C 1.1472(4) 0.7920(4) 0.8309(3) 0.0469(11) Uani 1 1 d . . . H20A H 1.0684 0.7873 0.8471 0.056 Uiso 1 1 calc R . . C21 C 1.1751(4) 0.8894(4) 0.8284(3) 0.0455(11) Uani 1 1 d . . . H21A H 1.1160 0.9520 0.8435 0.055 Uiso 1 1 calc R . . C22 C 1.2944(3) 0.8947(3) 0.8026(3) 0.0421(10) Uani 1 1 d . . . H22A H 1.3124 0.9622 0.8009 0.050 Uiso 1 1 calc R . . C23 C 1.3550(3) 0.7100(3) 0.7842(3) 0.0296(8) Uani 1 1 d . . . C24 C 1.4496(3) 0.6159(3) 0.7617(3) 0.0301(8) Uani 1 1 d . . . C25 C 1.4671(4) 0.6508(3) 1.0129(3) 0.0345(9) Uani 1 1 d . . . C26 C 1.3470(4) 0.6760(3) 1.0419(3) 0.0423(10) Uani 1 1 d . . . H26A H 1.3066 0.7477 1.0530 0.051 Uiso 1 1 calc R . . C27 C 1.2837(4) 0.5931(3) 1.0551(3) 0.0439(10) Uani 1 1 d . . . H27A H 1.2016 0.6102 1.0741 0.053 Uiso 1 1 calc R . . C28 C 1.3429(4) 0.4886(4) 1.0400(3) 0.0417(10) Uani 1 1 d . . . H28A H 1.3003 0.4348 1.0516 0.050 Uiso 1 1 calc R . . C29 C 1.4673(3) 0.4587(3) 1.0073(3) 0.0340(9) Uani 1 1 d . . . C30 C 1.9723(3) 0.5549(3) 0.6321(3) 0.0313(8) Uani 1 1 d . . . C31 C 2.0168(3) 0.4662(3) 0.6803(3) 0.0368(9) Uani 1 1 d . . . H31A H 2.0136 0.4706 0.7490 0.044 Uiso 1 1 calc R . . C32 C 2.0677(3) 0.3676(3) 0.6261(3) 0.0390(9) Uani 1 1 d . . . H32A H 2.0987 0.3074 0.6595 0.047 Uiso 1 1 calc R . . C33 C 2.0723(3) 0.3592(3) 0.5266(3) 0.0339(9) Uani 1 1 d . . . H33A H 2.1067 0.2933 0.4924 0.041 Uiso 1 1 calc R . . C34 C 2.0255(3) 0.4495(3) 0.4734(3) 0.0296(8) Uani 1 1 d . . . C35 C 1.4718(3) 0.6504(3) 0.5018(3) 0.0289(8) Uani 1 1 d . . . C36 C 1.3519(3) 0.6784(3) 0.5271(3) 0.0365(9) Uani 1 1 d . . . H36A H 1.3136 0.7509 0.5350 0.044 Uiso 1 1 calc R . . C37 C 1.2852(3) 0.5987(3) 0.5415(3) 0.0382(9) Uani 1 1 d . . . H37A H 1.2032 0.6185 0.5580 0.046 Uiso 1 1 calc R . . C38 C 1.3406(3) 0.4934(3) 0.5315(3) 0.0337(9) Uani 1 1 d . . . H38A H 1.2956 0.4415 0.5405 0.040 Uiso 1 1 calc R . . C39 C 1.4654(3) 0.4598(3) 0.5075(3) 0.0275(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02448(11) 0.02211(11) 0.03208(12) 0.00130(7) -0.00737(8) -0.00721(7) S1 0.0527(7) 0.0447(6) 0.0310(5) -0.0007(5) -0.0099(5) -0.0215(5) O1 0.0562(19) 0.0487(17) 0.0343(16) 0.0007(13) -0.0087(14) -0.0253(15) N1 0.0333(18) 0.0331(18) 0.045(2) -0.0053(15) -0.0105(15) -0.0113(15) C1 0.044(3) 0.051(3) 0.052(3) -0.009(2) -0.010(2) -0.016(2) O1W 0.057(2) 0.082(3) 0.168(4) -0.085(3) -0.059(3) 0.026(2) S2 0.0253(5) 0.0330(5) 0.0440(6) -0.0066(4) -0.0081(4) -0.0058(4) N2 0.0302(18) 0.0301(17) 0.044(2) 0.0071(15) -0.0100(15) -0.0117(14) O2W 0.0457(19) 0.0500(19) 0.076(2) 0.0271(17) 0.0058(17) 0.0076(15) O2 0.069(2) 0.064(2) 0.0452(18) 0.0023(16) -0.0269(16) -0.0297(18) C2 0.044(3) 0.068(3) 0.058(3) -0.018(3) -0.016(2) -0.015(2) S3 0.0434(6) 0.0301(5) 0.0343(5) 0.0076(4) -0.0155(4) -0.0164(4) N3 0.0313(17) 0.0256(16) 0.0314(17) 0.0031(13) -0.0085(13) -0.0099(14) O3 0.065(2) 0.0444(18) 0.0525(19) -0.0098(15) -0.0029(16) -0.0168(16) O3W 0.098(3) 0.0401(18) 0.058(2) 0.0032(16) -0.0204(19) -0.0211(18) C3 0.036(3) 0.053(3) 0.090(4) -0.029(3) -0.019(3) -0.011(2) O4 0.0241(13) 0.0300(14) 0.0453(16) -0.0025(12) -0.0080(12) -0.0044(11) N4 0.0308(18) 0.0320(17) 0.0406(19) 0.0016(14) -0.0102(15) -0.0085(14) C4 0.028(2) 0.033(2) 0.080(3) -0.012(2) -0.011(2) -0.0069(18) O4W 0.123(4) 0.171(5) 0.122(4) 0.009(4) -0.049(3) -0.091(4) O5 0.0518(19) 0.0554(19) 0.0486(18) -0.0135(15) -0.0225(15) 0.0041(15) C5 0.039(3) 0.036(3) 0.109(5) -0.011(3) -0.010(3) -0.017(2) O5W 0.207(6) 0.164(5) 0.069(3) -0.002(3) 0.006(3) -0.095(5) O6 0.0375(17) 0.0408(17) 0.074(2) -0.0110(15) -0.0021(15) -0.0193(14) C6 0.043(3) 0.031(2) 0.110(5) 0.008(3) -0.008(3) -0.019(2) O7 0.0492(17) 0.0373(15) 0.0426(16) 0.0086(13) -0.0230(14) -0.0203(13) C7 0.028(2) 0.030(2) 0.079(3) 0.011(2) -0.006(2) -0.0065(17) O8 0.0563(19) 0.0437(17) 0.0396(17) 0.0080(13) -0.0090(14) -0.0203(15) C8 0.033(2) 0.041(3) 0.079(4) 0.026(2) -0.002(2) -0.011(2) O9 0.0517(18) 0.0298(15) 0.0573(19) 0.0121(13) -0.0236(15) -0.0131(13) C9 0.037(2) 0.052(3) 0.057(3) 0.019(2) -0.007(2) -0.011(2) C10 0.037(2) 0.044(2) 0.053(3) 0.012(2) -0.015(2) -0.0144(19) C11 0.024(2) 0.0233(19) 0.059(3) 0.0015(18) -0.0070(18) -0.0051(16) C12 0.024(2) 0.0228(19) 0.061(3) -0.0061(18) -0.0065(18) -0.0051(15) C13 0.035(2) 0.032(2) 0.043(2) 0.0038(18) -0.0092(18) -0.0103(18) C14 0.049(3) 0.028(2) 0.043(2) 0.0003(18) -0.014(2) -0.0059(18) C15 0.066(3) 0.028(2) 0.036(2) 0.0066(17) -0.021(2) -0.020(2) C16 0.047(2) 0.037(2) 0.027(2) 0.0070(17) -0.0150(18) -0.0227(19) C17 0.052(3) 0.045(3) 0.049(3) 0.009(2) -0.014(2) -0.031(2) C18 0.039(2) 0.059(3) 0.050(3) 0.006(2) -0.012(2) -0.028(2) C19 0.037(2) 0.048(2) 0.030(2) 0.0053(18) -0.0116(17) -0.0189(19) C20 0.026(2) 0.067(3) 0.049(3) -0.002(2) -0.0070(19) -0.015(2) C21 0.029(2) 0.050(3) 0.054(3) -0.005(2) -0.0063(19) -0.0034(19) C22 0.031(2) 0.038(2) 0.054(3) -0.001(2) -0.0073(19) -0.0063(19) C23 0.032(2) 0.035(2) 0.0249(19) 0.0054(16) -0.0094(16) -0.0127(16) C24 0.038(2) 0.035(2) 0.0226(19) 0.0060(16) -0.0125(16) -0.0155(17) C25 0.043(2) 0.038(2) 0.025(2) 0.0025(17) -0.0084(17) -0.0146(18) C26 0.047(3) 0.043(2) 0.036(2) -0.0003(19) -0.010(2) -0.007(2) C27 0.036(2) 0.052(3) 0.046(3) 0.001(2) -0.011(2) -0.012(2) C28 0.038(2) 0.053(3) 0.041(2) 0.004(2) -0.0112(19) -0.022(2) C29 0.036(2) 0.048(2) 0.0224(19) 0.0037(17) -0.0082(16) -0.0153(18) C30 0.0195(18) 0.029(2) 0.043(2) -0.0023(17) -0.0033(16) -0.0057(15) C31 0.032(2) 0.040(2) 0.038(2) 0.0030(18) -0.0077(18) -0.0089(18) C32 0.036(2) 0.032(2) 0.048(3) 0.0077(19) -0.0109(19) -0.0047(18) C33 0.028(2) 0.0237(19) 0.048(2) 0.0015(17) -0.0065(18) -0.0048(16) C34 0.0193(18) 0.0269(18) 0.041(2) -0.0002(16) -0.0030(16) -0.0072(15) C35 0.035(2) 0.0294(19) 0.0259(19) 0.0022(15) -0.0094(16) -0.0125(16) C36 0.037(2) 0.029(2) 0.042(2) 0.0019(17) -0.0113(18) -0.0027(17) C37 0.024(2) 0.041(2) 0.048(2) 0.0054(19) -0.0079(18) -0.0068(17) C38 0.029(2) 0.037(2) 0.039(2) 0.0047(17) -0.0077(17) -0.0156(17) C39 0.029(2) 0.0287(19) 0.0274(19) 0.0028(15) -0.0088(15) -0.0102(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O4 2.330(2) . ? Eu1 O1 2.368(3) . ? Eu1 O7 2.431(3) . ? Eu1 O1W 2.469(3) . ? Eu1 O2W 2.511(3) . ? Eu1 N4 2.647(3) . ? Eu1 N2 2.675(3) . ? Eu1 N3 2.677(3) . ? Eu1 N1 2.681(3) . ? S1 O3 1.439(3) . ? S1 O2 1.450(3) . ? S1 O1 1.469(3) . ? S1 C25 1.767(4) . ? N1 C1 1.321(5) . ? N1 C12 1.364(5) . ? C1 C2 1.396(6) . ? C1 H1A 0.9300 . ? S2 O6 1.440(3) . ? S2 O5 1.445(3) . ? S2 O4 1.475(2) . ? S2 C30 1.784(4) . ? N2 C10 1.323(5) . ? N2 C11 1.359(5) . ? C2 C3 1.359(7) . ? C2 H2A 0.9300 . ? S3 O8 1.442(3) . ? S3 O9 1.452(3) . ? S3 O7 1.470(3) . ? S3 C35 1.774(4) . ? N3 C13 1.317(5) . ? N3 C24 1.364(5) . ? C3 C4 1.397(7) . ? C3 H3A 0.9300 . ? N4 C22 1.330(5) . ? N4 C23 1.367(5) . ? C4 C12 1.413(5) . ? C4 C5 1.442(6) . ? C5 C6 1.332(7) . ? C5 H5A 0.9300 . ? C6 C7 1.435(6) . ? C6 H6A 0.9300 . ? C7 C8 1.394(7) . ? C7 C11 1.424(5) . ? C8 C9 1.360(6) . ? C8 H8A 0.9300 . ? C9 C10 1.398(5) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.426(6) . ? C13 C14 1.396(5) . ? C13 H13A 0.9300 . ? C14 C15 1.366(6) . ? C14 H14A 0.9300 . ? C15 C16 1.398(6) . ? C15 H15A 0.9300 . ? C16 C24 1.415(5) . ? C16 C17 1.426(6) . ? C17 C18 1.340(6) . ? C17 H17A 0.9300 . ? C18 C19 1.431(6) . ? C18 H18A 0.9300 . ? C19 C20 1.402(6) . ? C19 C23 1.412(5) . ? C20 C21 1.351(6) . ? C20 H20A 0.9300 . ? C21 C22 1.404(6) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.434(6) . ? C25 C26 1.361(6) . ? C25 C29 1.436(6) 2_867 ? C26 C27 1.415(6) . ? C26 H26A 0.9300 . ? C27 C28 1.355(6) . ? C27 H27A 0.9300 . ? C28 C29 1.413(5) . ? C28 H28A 0.9300 . ? C29 C29 1.428(7) 2_867 ? C29 C25 1.436(6) 2_867 ? C30 C31 1.359(5) . ? C30 C34 1.432(5) 2_966 ? C31 C32 1.408(6) . ? C31 H31A 0.9300 . ? C32 C33 1.349(5) . ? C32 H32A 0.9300 . ? C33 C34 1.423(5) . ? C33 H33A 0.9300 . ? C34 C34 1.428(7) 2_966 ? C34 C30 1.432(5) 2_966 ? C35 C36 1.359(5) . ? C35 C39 1.428(5) 2_866 ? C36 C37 1.407(5) . ? C36 H36A 0.9300 . ? C37 C38 1.350(5) . ? C37 H37A 0.9300 . ? C38 C39 1.418(5) . ? C38 H38A 0.9300 . ? C39 C35 1.428(5) 2_866 ? C39 C39 1.435(7) 2_866 ? 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 O4 Eu1 O1 82.91(10) . . ? O4 Eu1 O7 81.64(9) . . ? O1 Eu1 O7 137.86(9) . . ? O4 Eu1 O1W 137.13(10) . . ? O1 Eu1 O1W 75.54(13) . . ? O7 Eu1 O1W 137.51(11) . . ? O4 Eu1 O2W 139.39(9) . . ? O1 Eu1 O2W 137.09(10) . . ? O7 Eu1 O2W 71.25(10) . . ? O1W Eu1 O2W 66.87(13) . . ? O4 Eu1 N4 136.20(9) . . ? O1 Eu1 N4 80.38(10) . . ? O7 Eu1 N4 84.26(9) . . ? O1W Eu1 N4 76.11(11) . . ? O2W Eu1 N4 71.36(10) . . ? O4 Eu1 N2 75.79(9) . . ? O1 Eu1 N2 136.18(10) . . ? O7 Eu1 N2 76.32(9) . . ? O1W Eu1 N2 94.83(14) . . ? O2W Eu1 N2 68.91(10) . . ? N4 Eu1 N2 139.57(9) . . ? O4 Eu1 N3 74.56(9) . . ? O1 Eu1 N3 70.78(9) . . ? O7 Eu1 N3 67.37(8) . . ? O1W Eu1 N3 129.15(13) . . ? O2W Eu1 N3 118.89(10) . . ? N4 Eu1 N3 61.74(9) . . ? N2 Eu1 N3 135.66(10) . . ? O4 Eu1 N1 72.80(9) . . ? O1 Eu1 N1 75.99(9) . . ? O7 Eu1 N1 134.44(9) . . ? O1W Eu1 N1 66.28(11) . . ? O2W Eu1 N1 105.52(11) . . ? N4 Eu1 N1 139.36(10) . . ? N2 Eu1 N1 61.34(10) . . ? N3 Eu1 N1 135.57(9) . . ? O3 S1 O2 113.51(19) . . ? O3 S1 O1 112.18(18) . . ? O2 S1 O1 110.57(19) . . ? O3 S1 C25 107.27(19) . . ? O2 S1 C25 107.05(18) . . ? O1 S1 C25 105.77(17) . . ? S1 O1 Eu1 154.37(19) . . ? C1 N1 C12 117.4(3) . . ? C1 N1 Eu1 123.5(3) . . ? C12 N1 Eu1 118.5(2) . . ? N1 C1 C2 124.4(4) . . ? N1 C1 H1A 117.8 . . ? C2 C1 H1A 117.8 . . ? O6 S2 O5 115.01(19) . . ? O6 S2 O4 112.68(17) . . ? O5 S2 O4 111.12(17) . . ? O6 S2 C30 106.89(17) . . ? O5 S2 C30 106.68(18) . . ? O4 S2 C30 103.51(16) . . ? C10 N2 C11 117.7(3) . . ? C10 N2 Eu1 123.2(3) . . ? C11 N2 Eu1 118.5(3) . . ? C3 C2 C1 118.5(5) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? O8 S3 O9 113.10(17) . . ? O8 S3 O7 110.92(17) . . ? O9 S3 O7 111.68(17) . . ? O8 S3 C35 107.78(17) . . ? O9 S3 C35 106.31(17) . . ? O7 S3 C35 106.65(15) . . ? C13 N3 C24 116.9(3) . . ? C13 N3 Eu1 122.9(2) . . ? C24 N3 Eu1 120.1(2) . . ? C2 C3 C4 119.6(4) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? S2 O4 Eu1 150.84(16) . . ? C22 N4 C23 117.2(3) . . ? C22 N4 Eu1 121.4(3) . . ? C23 N4 Eu1 121.3(2) . . ? C3 C4 C12 118.2(4) . . ? C3 C4 C5 123.1(4) . . ? C12 C4 C5 118.7(5) . . ? C6 C5 C4 121.3(4) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C7 121.6(4) . . ? C5 C6 H6A 119.2 . . ? C7 C6 H6A 119.2 . . ? S3 O7 Eu1 150.91(18) . . ? C8 C7 C11 118.1(4) . . ? C8 C7 C6 123.2(4) . . ? C11 C7 C6 118.6(5) . . ? C9 C8 C7 119.9(4) . . ? C9 C8 H8A 120.1 . . ? C7 C8 H8A 120.1 . . ? C8 C9 C10 118.3(4) . . ? C8 C9 H9A 120.8 . . ? C10 C9 H9A 120.8 . . ? N2 C10 C9 124.4(4) . . ? N2 C10 H10A 117.8 . . ? C9 C10 H10A 117.8 . . ? N2 C11 C7 121.4(4) . . ? N2 C11 C12 119.1(3) . . ? C7 C11 C12 119.4(4) . . ? N1 C12 C4 121.7(4) . . ? N1 C12 C11 118.2(3) . . ? C4 C12 C11 120.0(4) . . ? N3 C13 C14 124.8(4) . . ? N3 C13 H13A 117.6 . . ? C14 C13 H13A 117.6 . . ? C15 C14 C13 118.4(4) . . ? C15 C14 H14A 120.8 . . ? C13 C14 H14A 120.8 . . ? C14 C15 C16 119.6(4) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C15 C16 C24 117.7(4) . . ? C15 C16 C17 122.3(4) . . ? C24 C16 C17 119.9(4) . . ? C18 C17 C16 121.3(4) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C19 120.7(4) . . ? C17 C18 H18A 119.7 . . ? C19 C18 H18A 119.7 . . ? C20 C19 C23 117.7(4) . . ? C20 C19 C18 122.5(4) . . ? C23 C19 C18 119.8(4) . . ? C21 C20 C19 119.9(4) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C20 C21 C22 119.1(4) . . ? C20 C21 H21A 120.5 . . ? C22 C21 H21A 120.5 . . ? N4 C22 C21 123.6(4) . . ? N4 C22 H22A 118.2 . . ? C21 C22 H22A 118.2 . . ? N4 C23 C19 122.5(4) . . ? N4 C23 C24 118.1(3) . . ? C19 C23 C24 119.5(3) . . ? N3 C24 C16 122.5(4) . . ? N3 C24 C23 118.7(3) . . ? C16 C24 C23 118.8(3) . . ? C26 C25 C29 121.8(4) . 2_867 ? C26 C25 S1 117.2(3) . . ? C29 C25 S1 121.0(3) 2_867 . ? C25 C26 C27 120.0(4) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C28 C27 C26 119.8(4) . . ? C28 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? C27 C28 C29 122.2(4) . . ? C27 C28 H28A 118.9 . . ? C29 C28 H28A 118.9 . . ? C28 C29 C29 118.8(5) . 2_867 ? C28 C29 C25 123.8(4) . 2_867 ? C29 C29 C25 117.4(4) 2_867 2_867 ? C31 C30 C34 121.4(4) . 2_966 ? C31 C30 S2 118.3(3) . . ? C34 C30 S2 120.3(3) 2_966 . ? C30 C31 C32 120.0(4) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C33 C32 C31 121.0(4) . . ? C33 C32 H32A 119.5 . . ? C31 C32 H32A 119.5 . . ? C32 C33 C34 121.0(4) . . ? C32 C33 H33A 119.5 . . ? C34 C33 H33A 119.5 . . ? C33 C34 C34 118.9(4) . 2_966 ? C33 C34 C30 123.3(3) . 2_966 ? C34 C34 C30 117.8(4) 2_966 2_966 ? C36 C35 C39 121.8(3) . 2_866 ? C36 C35 S3 117.5(3) . . ? C39 C35 S3 120.8(3) 2_866 . ? C35 C36 C37 120.5(4) . . ? C35 C36 H36A 119.7 . . ? C37 C36 H36A 119.7 . . ? C38 C37 C36 119.9(4) . . ? C38 C37 H37A 120.1 . . ? C36 C37 H37A 120.1 . . ? C37 C38 C39 121.8(3) . . ? C37 C38 H38A 119.1 . . ? C39 C38 H38A 119.1 . . ? C38 C39 C35 124.0(3) . 2_866 ? C38 C39 C39 118.9(4) . 2_866 ? C35 C39 C39 117.1(4) 2_866 2_866 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 S1 O1 Eu1 -23.8(4) . . . . ? O2 S1 O1 Eu1 -151.6(4) . . . . ? C25 S1 O1 Eu1 92.9(4) . . . . ? O4 Eu1 O1 S1 -179.7(4) . . . . ? O7 Eu1 O1 S1 -110.5(4) . . . . ? O1W Eu1 O1 S1 37.7(4) . . . . ? O2W Eu1 O1 S1 8.5(5) . . . . ? N4 Eu1 O1 S1 -40.3(4) . . . . ? N2 Eu1 O1 S1 119.5(4) . . . . ? N3 Eu1 O1 S1 -103.6(4) . . . . ? N1 Eu1 O1 S1 106.4(4) . . . . ? O4 Eu1 N1 C1 -88.9(3) . . . . ? O1 Eu1 N1 C1 -2.1(3) . . . . ? O7 Eu1 N1 C1 -147.7(3) . . . . ? O1W Eu1 N1 C1 78.1(3) . . . . ? O2W Eu1 N1 C1 133.5(3) . . . . ? N4 Eu1 N1 C1 54.2(4) . . . . ? N2 Eu1 N1 C1 -171.8(3) . . . . ? N3 Eu1 N1 C1 -44.4(4) . . . . ? O4 Eu1 N1 C12 99.8(3) . . . . ? O1 Eu1 N1 C12 -173.4(3) . . . . ? O7 Eu1 N1 C12 40.9(3) . . . . ? O1W Eu1 N1 C12 -93.3(3) . . . . ? O2W Eu1 N1 C12 -37.8(3) . . . . ? N4 Eu1 N1 C12 -117.1(3) . . . . ? N2 Eu1 N1 C12 16.9(2) . . . . ? N3 Eu1 N1 C12 144.3(2) . . . . ? C12 N1 C1 C2 3.2(6) . . . . ? Eu1 N1 C1 C2 -168.3(3) . . . . ? O4 Eu1 N2 C10 94.2(3) . . . . ? O1 Eu1 N2 C10 157.6(3) . . . . ? O7 Eu1 N2 C10 9.5(3) . . . . ? O1W Eu1 N2 C10 -128.3(3) . . . . ? O2W Eu1 N2 C10 -65.4(3) . . . . ? N4 Eu1 N2 C10 -54.1(4) . . . . ? N3 Eu1 N2 C10 44.9(3) . . . . ? N1 Eu1 N2 C10 172.1(3) . . . . ? O4 Eu1 N2 C11 -94.5(3) . . . . ? O1 Eu1 N2 C11 -31.2(3) . . . . ? O7 Eu1 N2 C11 -179.2(3) . . . . ? O1W Eu1 N2 C11 43.0(3) . . . . ? O2W Eu1 N2 C11 105.9(3) . . . . ? N4 Eu1 N2 C11 117.2(3) . . . . ? N3 Eu1 N2 C11 -143.9(2) . . . . ? N1 Eu1 N2 C11 -16.6(2) . . . . ? N1 C1 C2 C3 1.5(7) . . . . ? O4 Eu1 N3 C13 -4.0(3) . . . . ? O1 Eu1 N3 C13 -91.8(3) . . . . ? O7 Eu1 N3 C13 83.2(3) . . . . ? O1W Eu1 N3 C13 -143.1(3) . . . . ? O2W Eu1 N3 C13 134.3(3) . . . . ? N4 Eu1 N3 C13 179.0(3) . . . . ? N2 Eu1 N3 C13 45.7(3) . . . . ? N1 Eu1 N3 C13 -48.0(3) . . . . ? O4 Eu1 N3 C24 179.1(3) . . . . ? O1 Eu1 N3 C24 91.4(3) . . . . ? O7 Eu1 N3 C24 -93.6(3) . . . . ? O1W Eu1 N3 C24 40.0(3) . . . . ? O2W Eu1 N3 C24 -42.5(3) . . . . ? N4 Eu1 N3 C24 2.2(2) . . . . ? N2 Eu1 N3 C24 -131.2(2) . . . . ? N1 Eu1 N3 C24 135.2(2) . . . . ? C1 C2 C3 C4 -3.7(7) . . . . ? O6 S2 O4 Eu1 -64.3(4) . . . . ? O5 S2 O4 Eu1 66.4(4) . . . . ? C30 S2 O4 Eu1 -179.5(3) . . . . ? O1 Eu1 O4 S2 -69.8(3) . . . . ? O7 Eu1 O4 S2 149.6(3) . . . . ? O1W Eu1 O4 S2 -10.0(4) . . . . ? O2W Eu1 O4 S2 101.7(3) . . . . ? N4 Eu1 O4 S2 -137.8(3) . . . . ? N2 Eu1 O4 S2 71.7(3) . . . . ? N3 Eu1 O4 S2 -141.7(3) . . . . ? N1 Eu1 O4 S2 7.7(3) . . . . ? O4 Eu1 N4 C22 174.8(3) . . . . ? O1 Eu1 N4 C22 105.8(3) . . . . ? O7 Eu1 N4 C22 -113.6(3) . . . . ? O1W Eu1 N4 C22 28.4(3) . . . . ? O2W Eu1 N4 C22 -41.5(3) . . . . ? N2 Eu1 N4 C22 -52.6(4) . . . . ? N3 Eu1 N4 C22 179.0(3) . . . . ? N1 Eu1 N4 C22 50.8(4) . . . . ? O4 Eu1 N4 C23 -6.1(3) . . . . ? O1 Eu1 N4 C23 -75.2(3) . . . . ? O7 Eu1 N4 C23 65.4(3) . . . . ? O1W Eu1 N4 C23 -152.5(3) . . . . ? O2W Eu1 N4 C23 137.6(3) . . . . ? N2 Eu1 N4 C23 126.5(3) . . . . ? N3 Eu1 N4 C23 -1.9(2) . . . . ? N1 Eu1 N4 C23 -130.1(3) . . . . ? C2 C3 C4 C12 1.2(6) . . . . ? C2 C3 C4 C5 -177.0(4) . . . . ? C3 C4 C5 C6 172.9(5) . . . . ? C12 C4 C5 C6 -5.4(7) . . . . ? C4 C5 C6 C7 0.0(7) . . . . ? O8 S3 O7 Eu1 146.1(3) . . . . ? O9 S3 O7 Eu1 19.0(4) . . . . ? C35 S3 O7 Eu1 -96.8(3) . . . . ? O4 Eu1 O7 S3 -176.0(3) . . . . ? O1 Eu1 O7 S3 114.4(3) . . . . ? O1W Eu1 O7 S3 -16.6(4) . . . . ? O2W Eu1 O7 S3 -26.7(3) . . . . ? N4 Eu1 O7 S3 45.6(3) . . . . ? N2 Eu1 O7 S3 -98.7(3) . . . . ? N3 Eu1 O7 S3 107.3(3) . . . . ? N1 Eu1 O7 S3 -120.3(3) . . . . ? C5 C6 C7 C8 -172.5(5) . . . . ? C5 C6 C7 C11 5.8(7) . . . . ? C11 C7 C8 C9 0.9(6) . . . . ? C6 C7 C8 C9 179.2(4) . . . . ? C7 C8 C9 C10 2.1(6) . . . . ? C11 N2 C10 C9 -1.3(6) . . . . ? Eu1 N2 C10 C9 170.0(3) . . . . ? C8 C9 C10 N2 -2.0(6) . . . . ? C10 N2 C11 C7 4.6(5) . . . . ? Eu1 N2 C11 C7 -167.2(3) . . . . ? C10 N2 C11 C12 -172.1(4) . . . . ? Eu1 N2 C11 C12 16.1(4) . . . . ? C8 C7 C11 N2 -4.4(6) . . . . ? C6 C7 C11 N2 177.2(4) . . . . ? C8 C7 C11 C12 172.3(4) . . . . ? C6 C7 C11 C12 -6.1(6) . . . . ? C1 N1 C12 C4 -5.7(5) . . . . ? Eu1 N1 C12 C4 166.2(3) . . . . ? C1 N1 C12 C11 171.4(4) . . . . ? Eu1 N1 C12 C11 -16.7(4) . . . . ? C3 C4 C12 N1 3.6(6) . . . . ? C5 C4 C12 N1 -178.1(4) . . . . ? C3 C4 C12 C11 -173.4(4) . . . . ? C5 C4 C12 C11 4.9(6) . . . . ? N2 C11 C12 N1 0.4(5) . . . . ? C7 C11 C12 N1 -176.4(3) . . . . ? N2 C11 C12 C4 177.6(3) . . . . ? C7 C11 C12 C4 0.8(6) . . . . ? C24 N3 C13 C14 -1.8(6) . . . . ? Eu1 N3 C13 C14 -178.8(3) . . . . ? N3 C13 C14 C15 1.4(6) . . . . ? C13 C14 C15 C16 -0.5(6) . . . . ? C14 C15 C16 C24 0.2(5) . . . . ? C14 C15 C16 C17 179.6(4) . . . . ? C15 C16 C17 C18 179.9(4) . . . . ? C24 C16 C17 C18 -0.7(6) . . . . ? C16 C17 C18 C19 0.4(6) . . . . ? C17 C18 C19 C20 -179.8(4) . . . . ? C17 C18 C19 C23 0.0(6) . . . . ? C23 C19 C20 C21 -0.6(6) . . . . ? C18 C19 C20 C21 179.2(4) . . . . ? C19 C20 C21 C22 0.8(7) . . . . ? C23 N4 C22 C21 -0.6(6) . . . . ? Eu1 N4 C22 C21 178.5(3) . . . . ? C20 C21 C22 N4 -0.2(7) . . . . ? C22 N4 C23 C19 0.8(5) . . . . ? Eu1 N4 C23 C19 -178.3(3) . . . . ? C22 N4 C23 C24 -179.3(3) . . . . ? Eu1 N4 C23 C24 1.6(4) . . . . ? C20 C19 C23 N4 -0.2(5) . . . . ? C18 C19 C23 N4 179.9(4) . . . . ? C20 C19 C23 C24 179.9(3) . . . . ? C18 C19 C23 C24 0.0(5) . . . . ? C13 N3 C24 C16 1.4(5) . . . . ? Eu1 N3 C24 C16 178.5(3) . . . . ? C13 N3 C24 C23 -179.4(3) . . . . ? Eu1 N3 C24 C23 -2.4(4) . . . . ? C15 C16 C24 N3 -0.7(5) . . . . ? C17 C16 C24 N3 179.9(3) . . . . ? C15 C16 C24 C23 -179.9(3) . . . . ? C17 C16 C24 C23 0.7(5) . . . . ? N4 C23 C24 N3 0.5(5) . . . . ? C19 C23 C24 N3 -179.6(3) . . . . ? N4 C23 C24 C16 179.7(3) . . . . ? C19 C23 C24 C16 -0.4(5) . . . . ? O3 S1 C25 C26 6.3(4) . . . . ? O2 S1 C25 C26 128.4(3) . . . . ? O1 S1 C25 C26 -113.6(3) . . . . ? O3 S1 C25 C29 -172.8(3) . . . 2_867 ? O2 S1 C25 C29 -50.7(3) . . . 2_867 ? O1 S1 C25 C29 67.3(3) . . . 2_867 ? C29 C25 C26 C27 1.5(6) 2_867 . . . ? S1 C25 C26 C27 -177.6(3) . . . . ? C25 C26 C27 C28 0.8(6) . . . . ? C26 C27 C28 C29 -2.6(6) . . . . ? C27 C28 C29 C29 2.0(7) . . . 2_867 ? C27 C28 C29 C25 -177.7(4) . . . 2_867 ? O6 S2 C30 C31 119.0(3) . . . . ? O5 S2 C30 C31 -4.5(4) . . . . ? O4 S2 C30 C31 -121.8(3) . . . . ? O6 S2 C30 C34 -59.4(3) . . . 2_966 ? O5 S2 C30 C34 177.1(3) . . . 2_966 ? O4 S2 C30 C34 59.8(3) . . . 2_966 ? C34 C30 C31 C32 0.8(6) 2_966 . . . ? S2 C30 C31 C32 -177.6(3) . . . . ? C30 C31 C32 C33 -0.6(6) . . . . ? C31 C32 C33 C34 -0.3(6) . . . . ? C32 C33 C34 C34 0.9(6) . . . 2_966 ? C32 C33 C34 C30 -179.8(3) . . . 2_966 ? O8 S3 C35 C36 -130.6(3) . . . . ? O9 S3 C35 C36 -9.1(3) . . . . ? O7 S3 C35 C36 110.2(3) . . . . ? O8 S3 C35 C39 49.0(3) . . . 2_866 ? O9 S3 C35 C39 170.6(3) . . . 2_866 ? O7 S3 C35 C39 -70.1(3) . . . 2_866 ? C39 C35 C36 C37 -2.3(6) 2_866 . . . ? S3 C35 C36 C37 177.3(3) . . . . ? C35 C36 C37 C38 0.8(6) . . . . ? C36 C37 C38 C39 0.7(6) . . . . ? C37 C38 C39 C35 178.5(4) . . . 2_866 ? C37 C38 C39 C39 -0.7(6) . . . 2_866 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.992 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.088 #============================================================END data_2 _database_code_depnum_ccdc_archive 'CCDC 637256' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H35 Gd N4 O14 S3' _chemical_formula_weight 1037.14 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 Triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9725(10) _cell_length_b 12.7153(10) _cell_length_c 13.5923(11) _cell_angle_alpha 88.2990(10) _cell_angle_beta 75.8550(10) _cell_angle_gamma 77.1280(10) _cell_volume 1955.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6396 _cell_measurement_theta_min 2.2265 _cell_measurement_theta_max 28.2400 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 1.758 _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1042 _exptl_absorpt_coefficient_mu 1.933 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 10106 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6728 _reflns_number_gt 6009 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^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 6728 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.003 _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 1.605848(15) 0.826703(12) 0.727930(13) 0.02714(7) Uani 1 1 d . . . S1 S 1.53990(10) 0.75898(9) 1.00165(7) 0.0446(3) Uani 1 1 d . . . O1 O 1.5968(3) 0.7635(2) 0.89299(19) 0.0462(7) Uani 1 1 d . . . N1 N 1.7502(3) 0.9233(2) 0.7953(2) 0.0391(8) Uani 1 1 d . . . C1 C 1.7678(4) 0.9118(4) 0.8878(3) 0.0490(11) Uani 1 1 d . . . H1A H 1.7396 0.8578 0.9272 0.059 Uiso 1 1 calc R . . O1W O 1.5032(3) 0.9847(3) 0.8395(3) 0.0993(15) Uani 1 1 d . . . S2 S 1.91301(8) 0.68018(8) 0.70259(8) 0.0375(2) Uani 1 1 d . . . N2 N 1.7437(3) 0.9302(2) 0.5958(2) 0.0379(7) Uani 1 1 d . . . O2W O 1.4868(3) 0.9708(2) 0.6433(3) 0.0675(10) Uani 1 1 d . . . O2 O 1.6283(3) 0.7313(3) 1.0603(2) 0.0594(8) Uani 1 1 d . . . C2 C 1.8262(4) 0.9758(4) 0.9301(4) 0.0590(13) Uani 1 1 d . . . H2A H 1.8376 0.9634 0.9951 0.071 Uiso 1 1 calc R . . S3 S 1.54831(9) 0.75667(7) 0.48052(7) 0.0357(2) Uani 1 1 d . . . N3 N 1.5643(3) 0.6285(2) 0.7376(2) 0.0321(7) Uani 1 1 d . . . O3 O 1.4514(3) 0.8557(2) 1.0381(2) 0.0594(8) Uani 1 1 d . . . O3W O 1.6807(4) 0.8396(2) 0.2076(2) 0.0700(10) Uani 1 1 d . . . C3 C 1.8659(4) 1.0561(4) 0.8744(4) 0.0611(14) Uani 1 1 d . . . H3A H 1.9011 1.1020 0.9025 0.073 Uiso 1 1 calc R . . O4 O 1.7900(2) 0.71004(19) 0.69275(19) 0.0369(6) Uani 1 1 d . . . N4 N 1.3844(3) 0.8088(2) 0.7798(2) 0.0355(7) Uani 1 1 d . . . C4 C 1.8540(4) 1.0701(3) 0.7743(4) 0.0493(11) Uani 1 1 d . . . O5 O 1.9178(3) 0.6567(2) 0.8067(2) 0.0562(8) Uani 1 1 d . . . C5 C 1.8981(4) 1.1498(4) 0.7091(5) 0.0684(15) Uani 1 1 d . . . H5A H 1.9293 1.2004 0.7352 0.082 Uiso 1 1 calc R . . O5W O 1.9201(6) 0.6106(5) 1.0072(4) 0.154(2) Uani 1 1 d . . . O6 O 1.9821(3) 0.7552(2) 0.6544(2) 0.0556(8) Uani 1 1 d . . . C6 C 1.8955(4) 1.1528(4) 0.6106(5) 0.0670(15) Uani 1 1 d . . . H6A H 1.9246 1.2056 0.5700 0.080 Uiso 1 1 calc R . . O7 O 1.6044(2) 0.75717(19) 0.56544(19) 0.0400(6) Uani 1 1 d . . . C7 C 1.8486(4) 1.0759(3) 0.5669(4) 0.0497(11) Uani 1 1 d . . . O8 O 1.6354(3) 0.7331(2) 0.3853(2) 0.0476(7) Uani 1 1 d . . . C8 C 1.8574(4) 1.0688(4) 0.4638(4) 0.0563(12) Uani 1 1 d . . . H8A H 1.8937 1.1153 0.4196 0.068 Uiso 1 1 calc R . . O9 O 1.4603(3) 0.8554(2) 0.4796(2) 0.0463(7) Uani 1 1 d . . . C9 C 1.8123(4) 0.9929(4) 0.4279(4) 0.0533(11) Uani 1 1 d . . . H9A H 1.8197 0.9851 0.3586 0.064 Uiso 1 1 calc R . . C10 C 1.7550(4) 0.9271(3) 0.4964(3) 0.0463(10) Uani 1 1 d . . . H10A H 1.7222 0.8774 0.4707 0.056 Uiso 1 1 calc R . . C11 C 1.7945(3) 1.0021(3) 0.6316(3) 0.0408(10) Uani 1 1 d . . . C12 C 1.7972(3) 0.9988(3) 0.7371(3) 0.0409(10) Uani 1 1 d . . . C13 C 1.6483(4) 0.5403(3) 0.7171(3) 0.0396(9) Uani 1 1 d . . . H13A H 1.7261 0.5480 0.6999 0.048 Uiso 1 1 calc R . . C14 C 1.6290(4) 0.4356(3) 0.7192(3) 0.0428(10) Uani 1 1 d . . . H14A H 1.6923 0.3761 0.7042 0.051 Uiso 1 1 calc R . . C15 C 1.5159(4) 0.4226(3) 0.7438(3) 0.0427(10) Uani 1 1 d . . . H15A H 1.5009 0.3538 0.7461 0.051 Uiso 1 1 calc R . . C16 C 1.4219(4) 0.5135(3) 0.7659(3) 0.0362(9) Uani 1 1 d . . . C17 C 1.3010(4) 0.5061(4) 0.7912(3) 0.0485(11) Uani 1 1 d . . . H17A H 1.2830 0.4384 0.7938 0.058 Uiso 1 1 calc R . . C18 C 1.2142(4) 0.5929(4) 0.8112(3) 0.0520(11) Uani 1 1 d . . . H18A H 1.1363 0.5856 0.8271 0.062 Uiso 1 1 calc R . . C19 C 1.2387(4) 0.6984(3) 0.8085(3) 0.0401(9) Uani 1 1 d . . . C20 C 1.1477(4) 0.7915(4) 0.8300(3) 0.0501(11) Uani 1 1 d . . . H20A H 1.0690 0.7865 0.8458 0.060 Uiso 1 1 calc R . . C21 C 1.1765(4) 0.8892(4) 0.8273(3) 0.0498(11) Uani 1 1 d . . . H21A H 1.1175 0.9519 0.8424 0.060 Uiso 1 1 calc R . . C22 C 1.2944(4) 0.8949(3) 0.8018(3) 0.0452(10) Uani 1 1 d . . . H22A H 1.3119 0.9627 0.8000 0.054 Uiso 1 1 calc R . . C23 C 1.3562(3) 0.7104(3) 0.7834(3) 0.0312(8) Uani 1 1 d . . . C24 C 1.4513(3) 0.6158(3) 0.7611(3) 0.0319(8) Uani 1 1 d . . . C25 C 1.4669(4) 0.6510(3) 1.0120(3) 0.0375(9) Uani 1 1 d . . . C26 C 1.3469(4) 0.6753(3) 1.0409(3) 0.0462(10) Uani 1 1 d . . . H26A H 1.3063 0.7471 1.0516 0.055 Uiso 1 1 calc R . . C27 C 1.2834(4) 0.5932(3) 1.0549(3) 0.0482(10) Uani 1 1 d . . . H27A H 1.2012 0.6104 1.0739 0.058 Uiso 1 1 calc R . . C28 C 1.3430(4) 0.4883(4) 1.0405(3) 0.0459(10) Uani 1 1 d . . . H28A H 1.3006 0.4342 1.0530 0.055 Uiso 1 1 calc R . . C29 C 1.4672(3) 0.4590(3) 1.0070(3) 0.0373(9) Uani 1 1 d . . . C30 C 1.9717(3) 0.5560(3) 0.6323(3) 0.0344(8) Uani 1 1 d . . . C31 C 2.0161(3) 0.4668(3) 0.6809(3) 0.0394(9) Uani 1 1 d . . . H31A H 2.0127 0.4712 0.7498 0.047 Uiso 1 1 calc R . . C32 C 2.0672(4) 0.3678(3) 0.6267(3) 0.0430(10) Uani 1 1 d . . . H32A H 2.0980 0.3077 0.6602 0.052 Uiso 1 1 calc R . . C33 C 2.0718(3) 0.3592(3) 0.5273(3) 0.0378(9) Uani 1 1 d . . . H33A H 2.1059 0.2931 0.4933 0.045 Uiso 1 1 calc R . . C34 C 2.0256(3) 0.4496(3) 0.4729(3) 0.0326(8) Uani 1 1 d . . . C35 C 1.4721(3) 0.6503(3) 0.5021(3) 0.0316(8) Uani 1 1 d . . . C36 C 1.3515(3) 0.6783(3) 0.5275(3) 0.0390(9) Uani 1 1 d . . . H36A H 1.3131 0.7507 0.5354 0.047 Uiso 1 1 calc R . . C37 C 1.2852(3) 0.5989(3) 0.5418(3) 0.0409(9) Uani 1 1 d . . . H37A H 1.2031 0.6187 0.5583 0.049 Uiso 1 1 calc R . . C38 C 1.3407(3) 0.4928(3) 0.5316(3) 0.0360(9) Uani 1 1 d . . . H38A H 1.2959 0.4406 0.5407 0.043 Uiso 1 1 calc R . . C39 C 1.4656(3) 0.4602(3) 0.5074(3) 0.0298(8) Uani 1 1 d . . . O4W O 1.9350(5) 0.7879(5) 0.1257(4) 0.138(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 Gd1 0.02636(11) 0.02485(10) 0.03247(11) 0.00151(7) -0.00926(7) -0.00818(7) S1 0.0579(7) 0.0511(6) 0.0322(5) 0.0002(4) -0.0128(5) -0.0252(5) O1 0.0601(19) 0.0524(16) 0.0333(15) 0.0029(13) -0.0097(13) -0.0295(15) N1 0.0374(19) 0.0358(17) 0.048(2) -0.0036(15) -0.0119(15) -0.0134(15) C1 0.046(3) 0.054(3) 0.051(3) -0.007(2) -0.014(2) -0.016(2) O1W 0.055(2) 0.084(2) 0.162(4) -0.078(3) -0.055(2) 0.0201(19) S2 0.0286(5) 0.0372(5) 0.0479(6) -0.0065(4) -0.0111(4) -0.0068(4) N2 0.0340(18) 0.0338(17) 0.049(2) 0.0064(15) -0.0109(15) -0.0133(14) O2W 0.0474(19) 0.0523(18) 0.084(2) 0.0292(17) 0.0018(17) 0.0036(15) O2 0.077(2) 0.072(2) 0.0461(18) 0.0044(15) -0.0307(16) -0.0359(18) C2 0.046(3) 0.074(3) 0.063(3) -0.022(3) -0.018(2) -0.018(3) S3 0.0460(6) 0.0336(5) 0.0358(5) 0.0082(4) -0.0182(4) -0.0177(4) N3 0.0355(18) 0.0309(16) 0.0320(16) 0.0035(13) -0.0090(13) -0.0112(14) O3 0.068(2) 0.0482(17) 0.059(2) -0.0127(15) -0.0034(16) -0.0172(16) O3W 0.111(3) 0.0447(18) 0.061(2) 0.0028(16) -0.027(2) -0.0237(19) C3 0.040(3) 0.054(3) 0.096(4) -0.029(3) -0.022(3) -0.013(2) O4 0.0258(14) 0.0348(13) 0.0503(16) -0.0053(12) -0.0103(12) -0.0052(11) N4 0.0329(18) 0.0345(17) 0.0421(18) 0.0020(14) -0.0110(14) -0.0118(14) C4 0.032(2) 0.033(2) 0.084(3) -0.015(2) -0.013(2) -0.0079(18) O5 0.058(2) 0.0622(18) 0.0483(17) -0.0130(15) -0.0253(15) 0.0036(16) C5 0.049(3) 0.039(3) 0.122(5) -0.008(3) -0.018(3) -0.022(2) O5W 0.212(7) 0.179(5) 0.079(3) 0.003(4) -0.005(4) -0.096(5) O6 0.0409(17) 0.0448(16) 0.082(2) -0.0115(15) -0.0041(15) -0.0216(14) C6 0.047(3) 0.036(2) 0.118(5) 0.011(3) -0.012(3) -0.021(2) O7 0.0516(17) 0.0385(14) 0.0414(15) 0.0077(12) -0.0237(13) -0.0213(13) C7 0.030(2) 0.032(2) 0.086(4) 0.011(2) -0.010(2) -0.0088(17) O8 0.0580(19) 0.0486(16) 0.0394(16) 0.0066(13) -0.0092(14) -0.0220(14) C8 0.039(3) 0.048(3) 0.076(3) 0.026(2) -0.004(2) -0.012(2) O9 0.0545(18) 0.0313(14) 0.0609(18) 0.0107(13) -0.0268(15) -0.0125(13) C9 0.042(3) 0.057(3) 0.056(3) 0.022(2) -0.006(2) -0.011(2) C10 0.039(2) 0.050(2) 0.051(3) 0.014(2) -0.013(2) -0.013(2) C11 0.029(2) 0.0252(19) 0.068(3) 0.0010(18) -0.0105(19) -0.0068(16) C12 0.030(2) 0.0274(19) 0.065(3) -0.0053(18) -0.0106(19) -0.0062(16) C13 0.036(2) 0.038(2) 0.046(2) 0.0018(18) -0.0114(18) -0.0093(18) C14 0.055(3) 0.032(2) 0.044(2) 0.0012(17) -0.018(2) -0.0070(19) C15 0.066(3) 0.032(2) 0.039(2) 0.0051(17) -0.021(2) -0.021(2) C16 0.050(2) 0.041(2) 0.028(2) 0.0063(16) -0.0167(17) -0.0237(19) C17 0.055(3) 0.050(3) 0.052(3) 0.006(2) -0.016(2) -0.032(2) C18 0.044(3) 0.067(3) 0.054(3) 0.004(2) -0.015(2) -0.029(2) C19 0.040(2) 0.057(2) 0.032(2) 0.0042(18) -0.0142(17) -0.025(2) C20 0.028(2) 0.073(3) 0.052(3) -0.002(2) -0.0104(19) -0.015(2) C21 0.036(2) 0.054(3) 0.056(3) -0.005(2) -0.009(2) -0.004(2) C22 0.037(2) 0.041(2) 0.056(3) -0.0032(19) -0.011(2) -0.0063(19) C23 0.033(2) 0.040(2) 0.0252(18) 0.0041(15) -0.0116(15) -0.0146(16) C24 0.039(2) 0.038(2) 0.0249(18) 0.0061(15) -0.0129(16) -0.0166(17) C25 0.045(2) 0.048(2) 0.0257(19) 0.0022(17) -0.0116(17) -0.0203(19) C26 0.050(3) 0.049(2) 0.040(2) -0.0004(19) -0.013(2) -0.009(2) C27 0.040(2) 0.057(3) 0.050(3) 0.001(2) -0.013(2) -0.014(2) C28 0.044(2) 0.059(3) 0.042(2) 0.004(2) -0.0134(19) -0.024(2) C29 0.039(2) 0.052(2) 0.0246(19) 0.0029(17) -0.0104(16) -0.0167(19) C30 0.0245(19) 0.035(2) 0.044(2) -0.0015(17) -0.0063(16) -0.0094(16) C31 0.033(2) 0.045(2) 0.041(2) 0.0032(18) -0.0104(17) -0.0093(18) C32 0.040(2) 0.035(2) 0.053(3) 0.0094(19) -0.0150(19) -0.0048(18) C33 0.037(2) 0.0280(19) 0.047(2) 0.0021(17) -0.0098(18) -0.0055(16) C34 0.0219(18) 0.0307(18) 0.044(2) -0.0001(16) -0.0057(16) -0.0059(15) C35 0.039(2) 0.0311(18) 0.0304(19) 0.0016(15) -0.0149(16) -0.0131(16) C36 0.038(2) 0.035(2) 0.044(2) 0.0013(17) -0.0137(18) -0.0043(18) C37 0.030(2) 0.043(2) 0.050(2) 0.0019(19) -0.0101(18) -0.0080(18) C38 0.032(2) 0.040(2) 0.042(2) 0.0062(17) -0.0114(17) -0.0169(17) C39 0.034(2) 0.0331(19) 0.0263(18) 0.0030(15) -0.0121(15) -0.0110(16) O4W 0.134(5) 0.189(5) 0.133(4) 0.020(4) -0.057(4) -0.100(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 Gd1 O4 2.315(2) . ? Gd1 O1 2.346(3) . ? Gd1 O7 2.409(2) . ? Gd1 O1W 2.453(3) . ? Gd1 O2W 2.495(3) . ? Gd1 N4 2.631(3) . ? Gd1 N2 2.657(3) . ? Gd1 N1 2.668(3) . ? Gd1 N3 2.669(3) . ? S1 O3 1.442(3) . ? S1 O2 1.452(3) . ? S1 O1 1.473(3) . ? S1 C25 1.770(4) . ? N1 C1 1.323(5) . ? N1 C12 1.357(5) . ? C1 C2 1.399(6) . ? C1 H1A 0.9300 . ? S2 O6 1.440(3) . ? S2 O5 1.450(3) . ? S2 O4 1.475(2) . ? S2 C30 1.780(4) . ? N2 C10 1.326(5) . ? N2 C11 1.363(5) . ? C2 C3 1.355(7) . ? C2 H2A 0.9300 . ? S3 O8 1.441(3) . ? S3 O9 1.450(3) . ? S3 O7 1.471(2) . ? S3 C35 1.774(4) . ? N3 C13 1.314(5) . ? N3 C24 1.357(5) . ? C3 C4 1.404(7) . ? C3 H3A 0.9300 . ? N4 C22 1.335(5) . ? N4 C23 1.363(4) . ? C4 C12 1.418(5) . ? C4 C5 1.432(7) . ? C5 C6 1.346(7) . ? C5 H5A 0.9300 . ? C6 C7 1.437(6) . ? C6 H6A 0.9300 . ? C7 C8 1.384(7) . ? C7 C11 1.420(5) . ? C8 C9 1.361(6) . ? C8 H8A 0.9300 . ? C9 C10 1.391(6) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.442(6) . ? C13 C14 1.400(5) . ? C13 H13A 0.9300 . ? C14 C15 1.360(6) . ? C14 H14A 0.9300 . ? C15 C16 1.403(6) . ? C15 H15A 0.9300 . ? C16 C24 1.417(5) . ? C16 C17 1.428(6) . ? C17 C18 1.320(6) . ? C17 H17A 0.9300 . ? C18 C19 1.433(6) . ? C18 H18A 0.9300 . ? C19 C20 1.401(6) . ? C19 C23 1.407(5) . ? C20 C21 1.359(6) . ? C20 H20A 0.9300 . ? C21 C22 1.387(6) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.441(5) . ? C25 C26 1.360(6) . ? C25 C29 1.441(5) 2_867 ? C26 C27 1.406(6) . ? C26 H26A 0.9300 . ? C27 C28 1.361(6) . ? C27 H27A 0.9300 . ? C28 C29 1.411(6) . ? C28 H28A 0.9300 . ? C29 C29 1.420(7) 2_867 ? C29 C25 1.441(5) 2_867 ? C30 C31 1.365(5) . ? C30 C34 1.425(5) 2_966 ? C31 C32 1.411(5) . ? C31 H31A 0.9300 . ? C32 C33 1.346(5) . ? C32 H32A 0.9300 . ? C33 C34 1.428(5) . ? C33 H33A 0.9300 . ? C34 C30 1.425(5) 2_966 ? C34 C34 1.430(7) 2_966 ? C35 C36 1.365(5) . ? C35 C39 1.430(5) 2_866 ? C36 C37 1.399(5) . ? C36 H36A 0.9300 . ? C37 C38 1.359(5) . ? C37 H37A 0.9300 . ? C38 C39 1.416(5) . ? C38 H38A 0.9300 . ? C39 C39 1.422(7) 2_866 ? C39 C35 1.430(5) 2_866 ? 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 O4 Gd1 O1 83.07(10) . . ? O4 Gd1 O7 81.52(9) . . ? O1 Gd1 O7 137.62(8) . . ? O4 Gd1 O1W 137.05(9) . . ? O1 Gd1 O1W 75.13(13) . . ? O7 Gd1 O1W 137.92(11) . . ? O4 Gd1 O2W 139.13(10) . . ? O1 Gd1 O2W 137.13(10) . . ? O7 Gd1 O2W 71.53(10) . . ? O1W Gd1 O2W 67.13(13) . . ? O4 Gd1 N4 136.51(9) . . ? O1 Gd1 N4 80.41(9) . . ? O7 Gd1 N4 84.22(9) . . ? O1W Gd1 N4 75.79(11) . . ? O2W Gd1 N4 71.46(10) . . ? O4 Gd1 N2 75.45(9) . . ? O1 Gd1 N2 136.35(10) . . ? O7 Gd1 N2 76.27(9) . . ? O1W Gd1 N2 95.51(13) . . ? O2W Gd1 N2 68.78(10) . . ? N4 Gd1 N2 139.47(9) . . ? O4 Gd1 N1 72.90(9) . . ? O1 Gd1 N1 75.93(9) . . ? O7 Gd1 N1 134.75(10) . . ? O1W Gd1 N1 66.17(10) . . ? O2W Gd1 N1 105.22(11) . . ? N4 Gd1 N1 139.08(10) . . ? N2 Gd1 N1 61.66(10) . . ? O4 Gd1 N3 74.37(9) . . ? O1 Gd1 N3 70.62(9) . . ? O7 Gd1 N3 67.26(8) . . ? O1W Gd1 N3 128.94(13) . . ? O2W Gd1 N3 119.47(10) . . ? N4 Gd1 N3 62.22(9) . . ? N2 Gd1 N3 135.25(9) . . ? N1 Gd1 N3 135.28(9) . . ? O3 S1 O2 113.66(19) . . ? O3 S1 O1 112.08(18) . . ? O2 S1 O1 110.50(19) . . ? O3 S1 C25 107.44(19) . . ? O2 S1 C25 107.03(18) . . ? O1 S1 C25 105.61(16) . . ? S1 O1 Gd1 153.99(19) . . ? C1 N1 C12 117.1(3) . . ? C1 N1 Gd1 123.7(3) . . ? C12 N1 Gd1 118.7(2) . . ? N1 C1 C2 124.1(4) . . ? N1 C1 H1A 117.9 . . ? C2 C1 H1A 117.9 . . ? O6 S2 O5 115.07(19) . . ? O6 S2 O4 112.55(17) . . ? O5 S2 O4 111.33(17) . . ? O6 S2 C30 106.89(17) . . ? O5 S2 C30 106.55(18) . . ? O4 S2 C30 103.49(15) . . ? C10 N2 C11 116.7(3) . . ? C10 N2 Gd1 123.9(3) . . ? C11 N2 Gd1 118.9(3) . . ? C3 C2 C1 118.6(5) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? O8 S3 O9 112.94(17) . . ? O8 S3 O7 111.23(17) . . ? O9 S3 O7 111.55(16) . . ? O8 S3 C35 107.45(17) . . ? O9 S3 C35 106.71(17) . . ? O7 S3 C35 106.54(15) . . ? C13 N3 C24 116.9(3) . . ? C13 N3 Gd1 123.4(2) . . ? C24 N3 Gd1 119.7(2) . . ? C2 C3 C4 120.1(4) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? S2 O4 Gd1 150.53(15) . . ? C22 N4 C23 116.8(3) . . ? C22 N4 Gd1 122.1(2) . . ? C23 N4 Gd1 121.1(2) . . ? C3 C4 C12 117.0(4) . . ? C3 C4 C5 123.5(4) . . ? C12 C4 C5 119.4(4) . . ? C6 C5 C4 121.3(4) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C7 121.2(5) . . ? C5 C6 H6A 119.4 . . ? C7 C6 H6A 119.4 . . ? S3 O7 Gd1 150.93(17) . . ? C8 C7 C11 118.7(4) . . ? C8 C7 C6 122.5(4) . . ? C11 C7 C6 118.8(5) . . ? C9 C8 C7 119.1(4) . . ? C9 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? C8 C9 C10 119.0(5) . . ? C8 C9 H9A 120.5 . . ? C10 C9 H9A 120.5 . . ? N2 C10 C9 124.6(4) . . ? N2 C10 H10A 117.7 . . ? C9 C10 H10A 117.7 . . ? N2 C11 C7 121.8(4) . . ? N2 C11 C12 118.3(3) . . ? C7 C11 C12 119.8(4) . . ? N1 C12 C4 122.8(4) . . ? N1 C12 C11 118.2(3) . . ? C4 C12 C11 119.0(4) . . ? N3 C13 C14 124.6(4) . . ? N3 C13 H13A 117.7 . . ? C14 C13 H13A 117.7 . . ? C15 C14 C13 118.6(4) . . ? C15 C14 H14A 120.7 . . ? C13 C14 H14A 120.7 . . ? C14 C15 C16 119.7(3) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C15 C16 C24 117.1(4) . . ? C15 C16 C17 122.8(4) . . ? C24 C16 C17 120.1(4) . . ? C18 C17 C16 121.6(4) . . ? C18 C17 H17A 119.2 . . ? C16 C17 H17A 119.2 . . ? C17 C18 C19 120.7(4) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? C20 C19 C23 118.4(4) . . ? C20 C19 C18 121.6(4) . . ? C23 C19 C18 120.1(4) . . ? C21 C20 C19 118.8(4) . . ? C21 C20 H20A 120.6 . . ? C19 C20 H20A 120.6 . . ? C20 C21 C22 119.6(4) . . ? C20 C21 H21A 120.2 . . ? C22 C21 H21A 120.2 . . ? N4 C22 C21 124.0(4) . . ? N4 C22 H22A 118.0 . . ? C21 C22 H22A 118.0 . . ? N4 C23 C19 122.4(4) . . ? N4 C23 C24 118.2(3) . . ? C19 C23 C24 119.4(3) . . ? N3 C24 C16 123.1(3) . . ? N3 C24 C23 118.8(3) . . ? C16 C24 C23 118.1(3) . . ? C26 C25 C29 121.3(4) . 2_867 ? C26 C25 S1 117.7(3) . . ? C29 C25 S1 121.0(3) 2_867 . ? C25 C26 C27 120.7(4) . . ? C25 C26 H26A 119.6 . . ? C27 C26 H26A 119.6 . . ? C28 C27 C26 119.5(4) . . ? C28 C27 H27A 120.3 . . ? C26 C27 H27A 120.3 . . ? C27 C28 C29 121.9(4) . . ? C27 C28 H28A 119.0 . . ? C29 C28 H28A 119.0 . . ? C28 C29 C29 119.3(5) . 2_867 ? C28 C29 C25 123.5(4) . 2_867 ? C29 C29 C25 117.3(4) 2_867 2_867 ? C31 C30 C34 120.8(3) . 2_966 ? C31 C30 S2 118.5(3) . . ? C34 C30 S2 120.7(3) 2_966 . ? C30 C31 C32 120.0(4) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C33 C32 C31 121.0(3) . . ? C33 C32 H32A 119.5 . . ? C31 C32 H32A 119.5 . . ? C32 C33 C34 121.3(4) . . ? C32 C33 H33A 119.3 . . ? C34 C33 H33A 119.3 . . ? C30 C34 C33 123.2(3) 2_966 . ? C30 C34 C34 118.8(4) 2_966 2_966 ? C33 C34 C34 118.0(4) . 2_966 ? C36 C35 C39 121.5(3) . 2_866 ? C36 C35 S3 117.2(3) . . ? C39 C35 S3 121.3(3) 2_866 . ? C35 C36 C37 120.6(3) . . ? C35 C36 H36A 119.7 . . ? C37 C36 H36A 119.7 . . ? C38 C37 C36 120.0(4) . . ? C38 C37 H37A 120.0 . . ? C36 C37 H37A 120.0 . . ? C37 C38 C39 121.3(3) . . ? C37 C38 H38A 119.4 . . ? C39 C38 H38A 119.4 . . ? C38 C39 C39 119.5(4) . 2_866 ? C38 C39 C35 123.3(3) . 2_866 ? C39 C39 C35 117.2(4) 2_866 2_866 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 S1 O1 Gd1 -22.6(4) . . . . ? O2 S1 O1 Gd1 -150.5(3) . . . . ? C25 S1 O1 Gd1 94.1(4) . . . . ? O4 Gd1 O1 S1 179.2(4) . . . . ? O7 Gd1 O1 S1 -111.5(4) . . . . ? O1W Gd1 O1 S1 36.5(4) . . . . ? O2W Gd1 O1 S1 7.8(4) . . . . ? N4 Gd1 O1 S1 -41.2(4) . . . . ? N2 Gd1 O1 S1 118.8(4) . . . . ? N1 Gd1 O1 S1 105.1(4) . . . . ? N3 Gd1 O1 S1 -105.0(4) . . . . ? O4 Gd1 N1 C1 -89.1(3) . . . . ? O1 Gd1 N1 C1 -2.1(3) . . . . ? O7 Gd1 N1 C1 -147.6(3) . . . . ? O1W Gd1 N1 C1 77.6(3) . . . . ? O2W Gd1 N1 C1 133.5(3) . . . . ? N4 Gd1 N1 C1 54.4(4) . . . . ? N2 Gd1 N1 C1 -171.5(3) . . . . ? N3 Gd1 N1 C1 -44.4(4) . . . . ? O4 Gd1 N1 C12 99.5(3) . . . . ? O1 Gd1 N1 C12 -173.6(3) . . . . ? O7 Gd1 N1 C12 41.0(3) . . . . ? O1W Gd1 N1 C12 -93.8(3) . . . . ? O2W Gd1 N1 C12 -37.9(3) . . . . ? N4 Gd1 N1 C12 -117.0(3) . . . . ? N2 Gd1 N1 C12 17.1(2) . . . . ? N3 Gd1 N1 C12 144.1(2) . . . . ? C12 N1 C1 C2 3.3(6) . . . . ? Gd1 N1 C1 C2 -168.3(3) . . . . ? O4 Gd1 N2 C10 94.1(3) . . . . ? O1 Gd1 N2 C10 157.2(3) . . . . ? O7 Gd1 N2 C10 9.5(3) . . . . ? O1W Gd1 N2 C10 -128.6(3) . . . . ? O2W Gd1 N2 C10 -65.8(3) . . . . ? N4 Gd1 N2 C10 -54.1(3) . . . . ? N1 Gd1 N2 C10 172.3(3) . . . . ? N3 Gd1 N2 C10 45.2(3) . . . . ? O4 Gd1 N2 C11 -94.9(3) . . . . ? O1 Gd1 N2 C11 -31.8(3) . . . . ? O7 Gd1 N2 C11 -179.5(3) . . . . ? O1W Gd1 N2 C11 42.4(3) . . . . ? O2W Gd1 N2 C11 105.3(3) . . . . ? N4 Gd1 N2 C11 117.0(3) . . . . ? N1 Gd1 N2 C11 -16.7(2) . . . . ? N3 Gd1 N2 C11 -143.8(2) . . . . ? N1 C1 C2 C3 1.2(7) . . . . ? O4 Gd1 N3 C13 -3.4(3) . . . . ? O1 Gd1 N3 C13 -91.4(3) . . . . ? O7 Gd1 N3 C13 83.8(3) . . . . ? O1W Gd1 N3 C13 -142.0(3) . . . . ? O2W Gd1 N3 C13 134.7(3) . . . . ? N4 Gd1 N3 C13 179.4(3) . . . . ? N2 Gd1 N3 C13 45.9(3) . . . . ? N1 Gd1 N3 C13 -47.6(3) . . . . ? O4 Gd1 N3 C24 179.1(3) . . . . ? O1 Gd1 N3 C24 91.1(2) . . . . ? O7 Gd1 N3 C24 -93.7(2) . . . . ? O1W Gd1 N3 C24 40.4(3) . . . . ? O2W Gd1 N3 C24 -42.8(3) . . . . ? N4 Gd1 N3 C24 1.9(2) . . . . ? N2 Gd1 N3 C24 -131.6(2) . . . . ? N1 Gd1 N3 C24 134.9(2) . . . . ? C1 C2 C3 C4 -3.5(7) . . . . ? O6 S2 O4 Gd1 -65.4(4) . . . . ? O5 S2 O4 Gd1 65.5(4) . . . . ? C30 S2 O4 Gd1 179.6(3) . . . . ? O1 Gd1 O4 S2 -69.1(3) . . . . ? O7 Gd1 O4 S2 150.5(3) . . . . ? O1W Gd1 O4 S2 -9.8(4) . . . . ? O2W Gd1 O4 S2 101.9(3) . . . . ? N4 Gd1 O4 S2 -137.3(3) . . . . ? N2 Gd1 O4 S2 72.6(3) . . . . ? N1 Gd1 O4 S2 8.2(3) . . . . ? N3 Gd1 O4 S2 -140.9(3) . . . . ? O4 Gd1 N4 C22 175.5(3) . . . . ? O1 Gd1 N4 C22 106.3(3) . . . . ? O7 Gd1 N4 C22 -113.3(3) . . . . ? O1W Gd1 N4 C22 29.3(3) . . . . ? O2W Gd1 N4 C22 -40.9(3) . . . . ? N2 Gd1 N4 C22 -52.4(3) . . . . ? N1 Gd1 N4 C22 51.1(3) . . . . ? N3 Gd1 N4 C22 179.4(3) . . . . ? O4 Gd1 N4 C23 -5.9(3) . . . . ? O1 Gd1 N4 C23 -75.0(3) . . . . ? O7 Gd1 N4 C23 65.4(3) . . . . ? O1W Gd1 N4 C23 -152.0(3) . . . . ? O2W Gd1 N4 C23 137.8(3) . . . . ? N2 Gd1 N4 C23 126.3(2) . . . . ? N1 Gd1 N4 C23 -130.2(2) . . . . ? N3 Gd1 N4 C23 -2.0(2) . . . . ? C2 C3 C4 C12 1.3(6) . . . . ? C2 C3 C4 C5 -177.1(4) . . . . ? C3 C4 C5 C6 173.0(5) . . . . ? C12 C4 C5 C6 -5.4(7) . . . . ? C4 C5 C6 C7 -0.2(7) . . . . ? O8 S3 O7 Gd1 145.7(3) . . . . ? O9 S3 O7 Gd1 18.6(4) . . . . ? C35 S3 O7 Gd1 -97.5(3) . . . . ? O4 Gd1 O7 S3 -175.4(3) . . . . ? O1 Gd1 O7 S3 114.7(3) . . . . ? O1W Gd1 O7 S3 -15.5(4) . . . . ? O2W Gd1 O7 S3 -26.6(3) . . . . ? N4 Gd1 O7 S3 45.8(3) . . . . ? N2 Gd1 O7 S3 -98.4(3) . . . . ? N1 Gd1 O7 S3 -119.9(3) . . . . ? N3 Gd1 O7 S3 108.1(3) . . . . ? C5 C6 C7 C8 -172.1(5) . . . . ? C5 C6 C7 C11 5.8(7) . . . . ? C11 C7 C8 C9 1.2(6) . . . . ? C6 C7 C8 C9 179.0(4) . . . . ? C7 C8 C9 C10 2.2(6) . . . . ? C11 N2 C10 C9 -1.3(6) . . . . ? Gd1 N2 C10 C9 169.9(3) . . . . ? C8 C9 C10 N2 -2.3(6) . . . . ? C10 N2 C11 C7 4.8(5) . . . . ? Gd1 N2 C11 C7 -166.8(3) . . . . ? C10 N2 C11 C12 -172.3(3) . . . . ? Gd1 N2 C11 C12 16.0(4) . . . . ? C8 C7 C11 N2 -4.9(6) . . . . ? C6 C7 C11 N2 177.1(4) . . . . ? C8 C7 C11 C12 172.3(4) . . . . ? C6 C7 C11 C12 -5.7(5) . . . . ? C1 N1 C12 C4 -5.6(5) . . . . ? Gd1 N1 C12 C4 166.4(3) . . . . ? C1 N1 C12 C11 171.0(4) . . . . ? Gd1 N1 C12 C11 -17.0(4) . . . . ? C3 C4 C12 N1 3.4(6) . . . . ? C5 C4 C12 N1 -178.1(4) . . . . ? C3 C4 C12 C11 -173.2(4) . . . . ? C5 C4 C12 C11 5.3(6) . . . . ? N2 C11 C12 N1 0.7(5) . . . . ? C7 C11 C12 N1 -176.5(3) . . . . ? N2 C11 C12 C4 177.5(3) . . . . ? C7 C11 C12 C4 0.2(5) . . . . ? C24 N3 C13 C14 -0.9(6) . . . . ? Gd1 N3 C13 C14 -178.5(3) . . . . ? N3 C13 C14 C15 0.2(6) . . . . ? C13 C14 C15 C16 0.3(6) . . . . ? C14 C15 C16 C24 -0.1(5) . . . . ? C14 C15 C16 C17 179.3(4) . . . . ? C15 C16 C17 C18 -179.7(4) . . . . ? C24 C16 C17 C18 -0.3(6) . . . . ? C16 C17 C18 C19 -0.4(7) . . . . ? C17 C18 C19 C20 -179.7(4) . . . . ? C17 C18 C19 C23 0.7(6) . . . . ? C23 C19 C20 C21 -1.0(6) . . . . ? C18 C19 C20 C21 179.3(4) . . . . ? C19 C20 C21 C22 1.1(6) . . . . ? C23 N4 C22 C21 -0.2(6) . . . . ? Gd1 N4 C22 C21 178.5(3) . . . . ? C20 C21 C22 N4 -0.5(7) . . . . ? C22 N4 C23 C19 0.3(5) . . . . ? Gd1 N4 C23 C19 -178.5(2) . . . . ? C22 N4 C23 C24 -179.3(3) . . . . ? Gd1 N4 C23 C24 1.9(4) . . . . ? C20 C19 C23 N4 0.4(5) . . . . ? C18 C19 C23 N4 180.0(3) . . . . ? C20 C19 C23 C24 179.9(3) . . . . ? C18 C19 C23 C24 -0.4(5) . . . . ? C13 N3 C24 C16 1.1(5) . . . . ? Gd1 N3 C24 C16 178.8(2) . . . . ? C13 N3 C24 C23 -179.5(3) . . . . ? Gd1 N3 C24 C23 -1.8(4) . . . . ? C15 C16 C24 N3 -0.6(5) . . . . ? C17 C16 C24 N3 180.0(3) . . . . ? C15 C16 C24 C23 180.0(3) . . . . ? C17 C16 C24 C23 0.6(5) . . . . ? N4 C23 C24 N3 0.0(5) . . . . ? C19 C23 C24 N3 -179.6(3) . . . . ? N4 C23 C24 C16 179.4(3) . . . . ? C19 C23 C24 C16 -0.2(5) . . . . ? O3 S1 C25 C26 6.0(4) . . . . ? O2 S1 C25 C26 128.4(3) . . . . ? O1 S1 C25 C26 -113.8(3) . . . . ? O3 S1 C25 C29 -172.5(3) . . . 2_867 ? O2 S1 C25 C29 -50.1(3) . . . 2_867 ? O1 S1 C25 C29 67.7(3) . . . 2_867 ? C29 C25 C26 C27 1.2(6) 2_867 . . . ? S1 C25 C26 C27 -177.3(3) . . . . ? C25 C26 C27 C28 0.8(6) . . . . ? C26 C27 C28 C29 -3.1(6) . . . . ? C27 C28 C29 C29 3.3(7) . . . 2_867 ? C27 C28 C29 C25 -178.1(4) . . . 2_867 ? O6 S2 C30 C31 119.3(3) . . . . ? O5 S2 C30 C31 -4.2(4) . . . . ? O4 S2 C30 C31 -121.7(3) . . . . ? O6 S2 C30 C34 -59.4(3) . . . 2_966 ? O5 S2 C30 C34 177.1(3) . . . 2_966 ? O4 S2 C30 C34 59.6(3) . . . 2_966 ? C34 C30 C31 C32 1.0(6) 2_966 . . . ? S2 C30 C31 C32 -177.7(3) . . . . ? C30 C31 C32 C33 -0.8(6) . . . . ? C31 C32 C33 C34 0.1(6) . . . . ? C32 C33 C34 C30 -179.8(4) . . . 2_966 ? C32 C33 C34 C34 0.4(6) . . . 2_966 ? O8 S3 C35 C36 -130.4(3) . . . . ? O9 S3 C35 C36 -9.0(3) . . . . ? O7 S3 C35 C36 110.3(3) . . . . ? O8 S3 C35 C39 49.2(3) . . . 2_866 ? O9 S3 C35 C39 170.6(3) . . . 2_866 ? O7 S3 C35 C39 -70.1(3) . . . 2_866 ? C39 C35 C36 C37 -2.2(6) 2_866 . . . ? S3 C35 C36 C37 177.5(3) . . . . ? C35 C36 C37 C38 0.8(6) . . . . ? C36 C37 C38 C39 0.5(6) . . . . ? C37 C38 C39 C39 -0.5(6) . . . 2_866 ? C37 C38 C39 C35 178.7(4) . . . 2_866 ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.940 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.082 #===================================================END data_3 _database_code_depnum_ccdc_archive 'CCDC 637257' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H35 N4 Nd O14 S3' _chemical_formula_weight 1024.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0480(10) _cell_length_b 12.7670(10) _cell_length_c 13.6822(11) _cell_angle_alpha 88.2590(10) _cell_angle_beta 75.7810(10) _cell_angle_gamma 77.0320(10) _cell_volume 1987.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4475 _cell_measurement_theta_min 2.2157 _cell_measurement_theta_max 26.1070 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 1.705 _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1034 _exptl_absorpt_coefficient_mu 1.540 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 10902 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.45 _reflns_number_total 7940 _reflns_number_gt 6304 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^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 7940 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 1.60558(2) 0.827302(18) 0.728346(17) 0.02082(8) Uani 1 1 d . . . S1 S 1.53998(11) 0.75794(10) 1.00484(8) 0.0362(3) Uani 1 1 d . . . O1 O 1.5968(3) 0.7636(3) 0.8970(2) 0.0412(8) Uani 1 1 d . . . N1 N 1.7514(3) 0.9253(3) 0.7944(3) 0.0335(9) Uani 1 1 d . . . C1 C 1.7673(4) 0.9151(4) 0.8866(4) 0.0428(13) Uani 1 1 d . . . H1A H 1.7370 0.8630 0.9266 0.051 Uiso 1 1 calc R . . O1W O 1.5003(4) 0.9889(4) 0.8409(4) 0.103(2) Uani 1 1 d . . . S2 S 1.91538(10) 0.67796(9) 0.70301(9) 0.0313(3) Uani 1 1 d . . . N2 N 1.7448(3) 0.9327(3) 0.5951(3) 0.0318(9) Uani 1 1 d . . . O2W O 1.4839(3) 0.9729(3) 0.6426(3) 0.0661(12) Uani 1 1 d . . . O2 O 1.6273(3) 0.7296(3) 1.0633(2) 0.0510(10) Uani 1 1 d . . . C2 C 1.8271(5) 0.9779(5) 0.9281(4) 0.0542(15) Uani 1 1 d . . . H2A H 1.8392 0.9652 0.9924 0.065 Uiso 1 1 calc R . . S3 S 1.54915(10) 0.75567(9) 0.47857(8) 0.0293(3) Uani 1 1 d . . . N3 N 1.5619(3) 0.6283(3) 0.7386(3) 0.0260(8) Uani 1 1 d . . . O3 O 1.4521(3) 0.8531(3) 1.0425(3) 0.0511(9) Uani 1 1 d . . . O3W O 1.6848(4) 0.8382(3) 0.2067(3) 0.0591(11) Uani 1 1 d . . . C3 C 1.8669(5) 1.0579(4) 0.8721(5) 0.0540(16) Uani 1 1 d . . . H3A H 1.9021 1.1037 0.8995 0.065 Uiso 1 1 calc R . . O4 O 1.7929(2) 0.7082(2) 0.6943(2) 0.0306(7) Uani 1 1 d . . . N4 N 1.3822(3) 0.8075(3) 0.7817(3) 0.0281(8) Uani 1 1 d . . . C4 C 1.8546(4) 1.0711(4) 0.7733(4) 0.0440(13) Uani 1 1 d . . . O4W O 1.9189(7) 0.6105(6) 1.0071(4) 0.151(3) Uani 1 1 d . . . O5 O 1.9210(3) 0.6540(3) 0.8057(3) 0.0498(9) Uani 1 1 d . . . C5 C 1.8994(5) 1.1503(4) 0.7076(6) 0.0596(17) Uani 1 1 d . . . H5A H 1.9303 1.2009 0.7333 0.072 Uiso 1 1 calc R . . O5W O 1.9389(5) 0.7864(5) 0.1248(4) 0.123(2) Uani 1 1 d . . . O6 O 1.9843(3) 0.7534(3) 0.6545(3) 0.0484(9) Uani 1 1 d . . . C6 C 1.8975(5) 1.1527(4) 0.6105(6) 0.0592(17) Uani 1 1 d . . . H6A H 1.9279 1.2045 0.5702 0.071 Uiso 1 1 calc R . . O7 O 1.6055(3) 0.7564(2) 0.5626(2) 0.0355(8) Uani 1 1 d . . . C7 C 1.8494(4) 1.0769(4) 0.5653(4) 0.0427(13) Uani 1 1 d . . . O8 O 1.6366(3) 0.7318(3) 0.3836(2) 0.0410(8) Uani 1 1 d . . . C8 C 1.8569(4) 1.0712(4) 0.4632(4) 0.0472(14) Uani 1 1 d . . . H8A H 1.8922 1.1181 0.4195 0.057 Uiso 1 1 calc R . . O9 O 1.4614(3) 0.8543(2) 0.4771(2) 0.0411(8) Uani 1 1 d . . . C9 C 1.8117(4) 0.9955(4) 0.4271(4) 0.0462(13) Uani 1 1 d . . . H9A H 1.8187 0.9877 0.3583 0.055 Uiso 1 1 calc R . . C10 C 1.7547(4) 0.9301(4) 0.4961(4) 0.0393(12) Uani 1 1 d . . . H10A H 1.7212 0.8812 0.4710 0.047 Uiso 1 1 calc R . . C11 C 1.7952(4) 1.0039(3) 0.6309(4) 0.0333(11) Uani 1 1 d . . . C12 C 1.7991(4) 0.9997(3) 0.7347(4) 0.0330(11) Uani 1 1 d . . . C13 C 1.6459(4) 0.5398(3) 0.7172(3) 0.0317(10) Uani 1 1 d . . . H13A H 1.7232 0.5475 0.6995 0.038 Uiso 1 1 calc R . . C14 C 1.6270(4) 0.4361(4) 0.7195(3) 0.0351(11) Uani 1 1 d . . . H14A H 1.6902 0.3771 0.7045 0.042 Uiso 1 1 calc R . . C15 C 1.5156(4) 0.4222(4) 0.7437(3) 0.0360(11) Uani 1 1 d . . . H15A H 1.5014 0.3534 0.7458 0.043 Uiso 1 1 calc R . . C16 C 1.4212(4) 0.5127(3) 0.7657(3) 0.0277(10) Uani 1 1 d . . . C17 C 1.3008(5) 0.5050(4) 0.7911(4) 0.0442(13) Uani 1 1 d . . . H17A H 1.2834 0.4375 0.7932 0.053 Uiso 1 1 calc R . . C18 C 1.2126(4) 0.5925(4) 0.8120(4) 0.0408(12) Uani 1 1 d . . . H18A H 1.1352 0.5850 0.8280 0.049 Uiso 1 1 calc R . . C19 C 1.2367(4) 0.6974(4) 0.8099(3) 0.0327(11) Uani 1 1 d . . . C20 C 1.1464(4) 0.7901(4) 0.8320(4) 0.0431(13) Uani 1 1 d . . . H20A H 1.0683 0.7850 0.8481 0.052 Uiso 1 1 calc R . . C21 C 1.1744(4) 0.8880(4) 0.8296(4) 0.0425(12) Uani 1 1 d . . . H21A H 1.1156 0.9504 0.8448 0.051 Uiso 1 1 calc R . . C22 C 1.2927(4) 0.8933(4) 0.8039(4) 0.0387(12) Uani 1 1 d . . . H22A H 1.3102 0.9608 0.8023 0.046 Uiso 1 1 calc R . . C23 C 1.3540(4) 0.7095(3) 0.7858(3) 0.0249(9) Uani 1 1 d . . . C24 C 1.4481(4) 0.6154(3) 0.7623(3) 0.0239(9) Uani 1 1 d . . . C25 C 1.4670(4) 0.6504(4) 1.0145(3) 0.0304(10) Uani 1 1 d . . . C26 C 1.3485(4) 0.6749(4) 1.0422(4) 0.0404(12) Uani 1 1 d . . . H26A H 1.3084 0.7465 1.0528 0.049 Uiso 1 1 calc R . . C27 C 1.2839(4) 0.5926(4) 1.0554(4) 0.0403(12) Uani 1 1 d . . . H27A H 1.2022 0.6099 1.0747 0.048 Uiso 1 1 calc R . . C28 C 1.3430(4) 0.4890(4) 1.0395(3) 0.0377(12) Uani 1 1 d . . . H28A H 1.3006 0.4354 1.0502 0.045 Uiso 1 1 calc R . . C29 C 1.4677(4) 0.4586(4) 1.0069(3) 0.0293(10) Uani 1 1 d . . . C30 C 1.9731(3) 0.5545(3) 0.6325(3) 0.0269(10) Uani 1 1 d . . . C31 C 2.0183(4) 0.4651(4) 0.6792(4) 0.0329(11) Uani 1 1 d . . . H31A H 2.0159 0.4691 0.7475 0.039 Uiso 1 1 calc R . . C32 C 2.0685(4) 0.3669(4) 0.6253(4) 0.0347(11) Uani 1 1 d . . . H32A H 2.0995 0.3066 0.6581 0.042 Uiso 1 1 calc R . . C33 C 2.0722(4) 0.3596(3) 0.5257(3) 0.0310(10) Uani 1 1 d . . . H33A H 2.1057 0.2940 0.4913 0.037 Uiso 1 1 calc R . . C34 C 2.0259(3) 0.4498(3) 0.4728(3) 0.0269(10) Uani 1 1 d . . . C35 C 1.4723(4) 0.6504(3) 0.5010(3) 0.0255(9) Uani 1 1 d . . . C36 C 1.3531(4) 0.6790(4) 0.5269(3) 0.0327(11) Uani 1 1 d . . . H36A H 1.3153 0.7514 0.5344 0.039 Uiso 1 1 calc R . . C37 C 1.2868(4) 0.5996(4) 0.5424(3) 0.0352(11) Uani 1 1 d . . . H37A H 1.2052 0.6196 0.5596 0.042 Uiso 1 1 calc R . . C38 C 1.3413(4) 0.4940(4) 0.5324(3) 0.0304(10) Uani 1 1 d . . . H38A H 1.2963 0.4424 0.5417 0.036 Uiso 1 1 calc R . . C39 C 1.4654(4) 0.4606(3) 0.5079(3) 0.0226(9) 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 Nd1 0.02129(13) 0.01877(12) 0.02474(13) 0.00119(8) -0.00711(9) -0.00776(9) S1 0.0502(8) 0.0399(7) 0.0249(6) 0.0001(5) -0.0109(5) -0.0213(6) O1 0.058(2) 0.048(2) 0.0240(17) 0.0028(15) -0.0087(16) -0.0267(18) N1 0.033(2) 0.033(2) 0.038(2) -0.0045(17) -0.0101(18) -0.0122(18) C1 0.041(3) 0.048(3) 0.046(3) -0.006(2) -0.012(2) -0.021(2) O1W 0.053(3) 0.082(3) 0.178(5) -0.090(3) -0.062(3) 0.030(2) S2 0.0224(6) 0.0315(6) 0.0409(7) -0.0076(5) -0.0086(5) -0.0060(5) N2 0.026(2) 0.031(2) 0.040(2) 0.0063(17) -0.0098(17) -0.0104(17) O2W 0.042(2) 0.055(3) 0.079(3) 0.036(2) 0.006(2) 0.0076(18) O2 0.070(3) 0.062(2) 0.036(2) 0.0042(17) -0.0276(19) -0.031(2) C2 0.045(3) 0.069(4) 0.056(4) -0.021(3) -0.020(3) -0.016(3) S3 0.0402(7) 0.0264(6) 0.0290(6) 0.0072(5) -0.0159(5) -0.0160(5) N3 0.028(2) 0.0261(19) 0.027(2) 0.0045(15) -0.0081(16) -0.0113(16) O3 0.066(3) 0.037(2) 0.048(2) -0.0077(17) -0.0060(19) -0.0151(18) O3W 0.091(3) 0.037(2) 0.053(2) 0.0038(17) -0.019(2) -0.020(2) C3 0.035(3) 0.046(3) 0.087(5) -0.028(3) -0.022(3) -0.010(3) O4 0.0217(16) 0.0280(16) 0.0412(18) -0.0042(14) -0.0061(14) -0.0047(13) N4 0.024(2) 0.027(2) 0.035(2) 0.0009(16) -0.0099(16) -0.0073(16) C4 0.028(3) 0.028(3) 0.076(4) -0.013(3) -0.010(3) -0.007(2) O4W 0.224(8) 0.178(7) 0.063(4) -0.007(4) 0.007(4) -0.113(6) O5 0.051(2) 0.057(2) 0.041(2) -0.0110(17) -0.0225(18) 0.0018(18) C5 0.037(3) 0.035(3) 0.110(6) -0.012(3) -0.015(3) -0.018(3) O5W 0.118(5) 0.172(6) 0.120(5) 0.009(4) -0.047(4) -0.097(5) O6 0.036(2) 0.036(2) 0.074(3) -0.0112(18) -0.0021(18) -0.0215(16) C6 0.039(3) 0.025(3) 0.115(6) 0.016(3) -0.013(3) -0.019(2) O7 0.050(2) 0.0352(18) 0.0317(18) 0.0063(14) -0.0216(15) -0.0190(15) C7 0.021(3) 0.028(3) 0.074(4) 0.009(2) -0.003(2) -0.005(2) O8 0.051(2) 0.044(2) 0.0316(18) 0.0069(15) -0.0057(16) -0.0224(17) C8 0.028(3) 0.040(3) 0.068(4) 0.021(3) -0.001(3) -0.009(2) O9 0.052(2) 0.0264(17) 0.052(2) 0.0087(15) -0.0231(18) -0.0128(15) C9 0.039(3) 0.049(3) 0.048(3) 0.021(3) -0.007(2) -0.012(3) C10 0.032(3) 0.042(3) 0.047(3) 0.013(2) -0.013(2) -0.013(2) C11 0.018(2) 0.021(2) 0.059(3) 0.005(2) -0.006(2) -0.0043(18) C12 0.023(2) 0.022(2) 0.056(3) -0.004(2) -0.010(2) -0.0077(19) C13 0.029(3) 0.028(2) 0.039(3) 0.002(2) -0.011(2) -0.006(2) C14 0.046(3) 0.025(2) 0.036(3) -0.001(2) -0.013(2) -0.008(2) C15 0.058(3) 0.027(2) 0.031(3) 0.0039(19) -0.018(2) -0.019(2) C16 0.036(3) 0.033(2) 0.020(2) 0.0055(18) -0.0114(19) -0.018(2) C17 0.052(3) 0.049(3) 0.048(3) 0.010(2) -0.019(3) -0.038(3) C18 0.035(3) 0.051(3) 0.046(3) 0.003(2) -0.011(2) -0.027(3) C19 0.032(3) 0.044(3) 0.028(2) 0.003(2) -0.014(2) -0.016(2) C20 0.027(3) 0.059(4) 0.047(3) -0.003(3) -0.012(2) -0.015(3) C21 0.027(3) 0.044(3) 0.051(3) -0.006(2) -0.004(2) -0.001(2) C22 0.034(3) 0.034(3) 0.049(3) -0.001(2) -0.011(2) -0.009(2) C23 0.026(2) 0.033(2) 0.019(2) 0.0046(18) -0.0074(18) -0.0129(19) C24 0.031(2) 0.030(2) 0.016(2) 0.0044(17) -0.0097(18) -0.014(2) C25 0.039(3) 0.036(3) 0.022(2) 0.0056(19) -0.010(2) -0.015(2) C26 0.042(3) 0.042(3) 0.036(3) 0.000(2) -0.011(2) -0.005(2) C27 0.035(3) 0.047(3) 0.040(3) 0.001(2) -0.009(2) -0.011(2) C28 0.039(3) 0.044(3) 0.037(3) 0.002(2) -0.013(2) -0.020(2) C29 0.034(3) 0.041(3) 0.017(2) 0.0029(19) -0.0077(19) -0.015(2) C30 0.016(2) 0.028(2) 0.037(3) -0.0004(19) -0.0062(18) -0.0052(18) C31 0.024(2) 0.038(3) 0.036(3) -0.001(2) -0.007(2) -0.006(2) C32 0.032(3) 0.027(2) 0.044(3) 0.009(2) -0.011(2) -0.003(2) C33 0.030(3) 0.021(2) 0.041(3) 0.0038(19) -0.009(2) -0.0048(19) C34 0.015(2) 0.028(2) 0.038(3) 0.0011(19) -0.0059(19) -0.0054(18) C35 0.033(3) 0.023(2) 0.024(2) 0.0019(17) -0.0109(19) -0.0097(19) C36 0.035(3) 0.027(2) 0.036(3) 0.001(2) -0.012(2) -0.003(2) C37 0.020(2) 0.040(3) 0.044(3) 0.004(2) -0.004(2) -0.005(2) C38 0.024(2) 0.036(3) 0.035(3) 0.005(2) -0.0062(19) -0.015(2) C39 0.028(2) 0.024(2) 0.020(2) 0.0012(17) -0.0101(18) -0.0098(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O4 2.368(3) . ? Nd1 O1 2.409(3) . ? Nd1 O7 2.467(3) . ? Nd1 O1W 2.510(4) . ? Nd1 O2W 2.543(4) . ? Nd1 N4 2.678(3) . ? Nd1 N3 2.701(3) . ? Nd1 N2 2.703(4) . ? Nd1 N1 2.703(3) . ? S1 O3 1.433(4) . ? S1 O2 1.450(4) . ? S1 O1 1.473(3) . ? S1 C25 1.775(4) . ? N1 C1 1.320(6) . ? N1 C12 1.366(6) . ? C1 C2 1.404(6) . ? C1 H1A 0.9300 . ? S2 O5 1.444(4) . ? S2 O6 1.451(3) . ? S2 O4 1.473(3) . ? S2 C30 1.781(4) . ? N2 C10 1.331(6) . ? N2 C11 1.363(5) . ? C2 C3 1.361(8) . ? C2 H2A 0.9300 . ? S3 O8 1.449(3) . ? S3 O9 1.454(3) . ? S3 O7 1.473(3) . ? S3 C35 1.776(4) . ? N3 C13 1.321(5) . ? N3 C24 1.375(5) . ? C3 C4 1.396(8) . ? C3 H3A 0.9300 . ? N4 C22 1.335(6) . ? N4 C23 1.364(5) . ? C4 C12 1.427(6) . ? C4 C5 1.440(8) . ? C5 C6 1.333(8) . ? C5 H5A 0.9300 . ? C6 C7 1.455(8) . ? C6 H6A 0.9300 . ? C7 C8 1.381(7) . ? C7 C11 1.426(6) . ? C8 C9 1.368(7) . ? C8 H8A 0.9300 . ? C9 C10 1.396(6) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.431(7) . ? C13 C14 1.391(6) . ? C13 H13A 0.9300 . ? C14 C15 1.352(6) . ? C14 H14A 0.9300 . ? C15 C16 1.408(6) . ? C15 H15A 0.9300 . ? C16 C24 1.416(6) . ? C16 C17 1.432(6) . ? C17 C18 1.341(7) . ? C17 H17A 0.9300 . ? C18 C19 1.431(6) . ? C18 H18A 0.9300 . ? C19 C20 1.399(7) . ? C19 C23 1.413(6) . ? C20 C21 1.363(7) . ? C20 H20A 0.9300 . ? C21 C22 1.399(6) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.437(6) . ? C25 C26 1.350(6) . ? C25 C29 1.435(6) 2_867 ? C26 C27 1.424(7) . ? C26 H26A 0.9300 . ? C27 C28 1.350(7) . ? C27 H27A 0.9300 . ? C28 C29 1.423(6) . ? C28 H28A 0.9300 . ? C29 C29 1.430(8) 2_867 ? C29 C25 1.435(6) 2_867 ? C30 C31 1.362(6) . ? C30 C34 1.441(6) 2_966 ? C31 C32 1.407(6) . ? C31 H31A 0.9300 . ? C32 C33 1.358(6) . ? C32 H32A 0.9300 . ? C33 C34 1.421(6) . ? C33 H33A 0.9300 . ? C34 C34 1.434(8) 2_966 ? C34 C30 1.441(6) 2_966 ? C35 C36 1.358(6) . ? C35 C39 1.440(6) 2_866 ? C36 C37 1.407(6) . ? C36 H36A 0.9300 . ? C37 C38 1.356(6) . ? C37 H37A 0.9300 . ? C38 C39 1.416(6) . ? C38 H38A 0.9300 . ? C39 C39 1.425(8) 2_866 ? C39 C35 1.440(6) 2_866 ? 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 O4 Nd1 O1 82.50(11) . . ? O4 Nd1 O7 81.81(10) . . ? O1 Nd1 O7 138.12(10) . . ? O4 Nd1 O1W 136.93(11) . . ? O1 Nd1 O1W 75.24(16) . . ? O7 Nd1 O1W 137.70(14) . . ? O4 Nd1 O2W 139.82(11) . . ? O1 Nd1 O2W 137.01(12) . . ? O7 Nd1 O2W 71.43(12) . . ? O1W Nd1 O2W 66.89(16) . . ? O4 Nd1 N4 135.92(10) . . ? O1 Nd1 N4 80.27(11) . . ? O7 Nd1 N4 84.61(10) . . ? O1W Nd1 N4 75.97(13) . . ? O2W Nd1 N4 71.66(11) . . ? O4 Nd1 N3 74.84(10) . . ? O1 Nd1 N3 71.02(10) . . ? O7 Nd1 N3 67.45(10) . . ? O1W Nd1 N3 128.66(16) . . ? O2W Nd1 N3 118.69(12) . . ? N4 Nd1 N3 61.22(10) . . ? O4 Nd1 N2 75.91(10) . . ? O1 Nd1 N2 135.92(11) . . ? O7 Nd1 N2 76.15(10) . . ? O1W Nd1 N2 95.19(16) . . ? O2W Nd1 N2 69.04(11) . . ? N4 Nd1 N2 139.97(11) . . ? N3 Nd1 N2 135.76(11) . . ? O4 Nd1 N1 72.59(10) . . ? O1 Nd1 N1 76.04(11) . . ? O7 Nd1 N1 133.98(11) . . ? O1W Nd1 N1 66.54(12) . . ? O2W Nd1 N1 105.31(13) . . ? N4 Nd1 N1 139.51(11) . . ? N3 Nd1 N1 135.97(11) . . ? N2 Nd1 N1 61.04(11) . . ? O3 S1 O2 113.2(2) . . ? O3 S1 O1 112.6(2) . . ? O2 S1 O1 110.6(2) . . ? O3 S1 C25 107.1(2) . . ? O2 S1 C25 106.9(2) . . ? O1 S1 C25 105.97(19) . . ? S1 O1 Nd1 154.2(2) . . ? C1 N1 C12 117.8(4) . . ? C1 N1 Nd1 123.1(3) . . ? C12 N1 Nd1 118.5(3) . . ? N1 C1 C2 124.2(5) . . ? N1 C1 H1A 117.9 . . ? C2 C1 H1A 117.9 . . ? O5 S2 O6 115.1(2) . . ? O5 S2 O4 111.3(2) . . ? O6 S2 O4 112.5(2) . . ? O5 S2 C30 106.6(2) . . ? O6 S2 C30 106.9(2) . . ? O4 S2 C30 103.52(18) . . ? C10 N2 C11 117.0(4) . . ? C10 N2 Nd1 123.5(3) . . ? C11 N2 Nd1 118.8(3) . . ? C3 C2 C1 118.4(5) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? O8 S3 O9 112.9(2) . . ? O8 S3 O7 110.75(19) . . ? O9 S3 O7 111.80(19) . . ? O8 S3 C35 107.98(19) . . ? O9 S3 C35 106.3(2) . . ? O7 S3 C35 106.72(18) . . ? C13 N3 C24 116.7(4) . . ? C13 N3 Nd1 123.0(3) . . ? C24 N3 Nd1 120.2(3) . . ? C2 C3 C4 119.8(5) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? S2 O4 Nd1 151.30(17) . . ? C22 N4 C23 116.7(4) . . ? C22 N4 Nd1 121.6(3) . . ? C23 N4 Nd1 121.7(3) . . ? C3 C4 C12 118.2(5) . . ? C3 C4 C5 123.2(5) . . ? C12 C4 C5 118.6(5) . . ? C6 C5 C4 121.3(5) . . ? C6 C5 H5A 119.3 . . ? C4 C5 H5A 119.3 . . ? C5 C6 C7 122.3(5) . . ? C5 C6 H6A 118.8 . . ? C7 C6 H6A 118.8 . . ? S3 O7 Nd1 150.6(2) . . ? C8 C7 C11 119.6(5) . . ? C8 C7 C6 123.2(5) . . ? C11 C7 C6 117.3(5) . . ? C9 C8 C7 119.1(5) . . ? C9 C8 H8A 120.5 . . ? C7 C8 H8A 120.5 . . ? C8 C9 C10 118.3(5) . . ? C8 C9 H9A 120.8 . . ? C10 C9 H9A 120.8 . . ? N2 C10 C9 124.9(5) . . ? N2 C10 H10A 117.6 . . ? C9 C10 H10A 117.6 . . ? N2 C11 C7 120.9(5) . . ? N2 C11 C12 118.6(4) . . ? C7 C11 C12 120.4(4) . . ? N1 C12 C4 121.2(5) . . ? N1 C12 C11 119.0(4) . . ? C4 C12 C11 119.8(4) . . ? N3 C13 C14 124.8(4) . . ? N3 C13 H13A 117.6 . . ? C14 C13 H13A 117.6 . . ? C15 C14 C13 119.2(4) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C14 C15 C16 119.4(4) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C15 C16 C24 117.8(4) . . ? C15 C16 C17 122.9(4) . . ? C24 C16 C17 119.3(4) . . ? C18 C17 C16 121.7(4) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? C17 C18 C19 120.4(4) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C20 C19 C23 118.2(4) . . ? C20 C19 C18 121.7(4) . . ? C23 C19 C18 120.1(4) . . ? C21 C20 C19 119.3(4) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C20 C21 C22 119.1(5) . . ? C20 C21 H21A 120.4 . . ? C22 C21 H21A 120.4 . . ? N4 C22 C21 124.1(4) . . ? N4 C22 H22A 118.0 . . ? C21 C22 H22A 118.0 . . ? N4 C23 C19 122.7(4) . . ? N4 C23 C24 118.2(4) . . ? C19 C23 C24 119.1(4) . . ? N3 C24 C16 122.1(4) . . ? N3 C24 C23 118.6(4) . . ? C16 C24 C23 119.4(4) . . ? C26 C25 C29 121.5(4) . 2_867 ? C26 C25 S1 117.6(4) . . ? C29 C25 S1 120.9(3) 2_867 . ? C25 C26 C27 120.9(5) . . ? C25 C26 H26A 119.6 . . ? C27 C26 H26A 119.6 . . ? C28 C27 C26 119.0(5) . . ? C28 C27 H27A 120.5 . . ? C26 C27 H27A 120.5 . . ? C27 C28 C29 122.6(4) . . ? C27 C28 H28A 118.7 . . ? C29 C28 H28A 118.7 . . ? C28 C29 C29 118.3(5) . 2_867 ? C28 C29 C25 124.0(4) . 2_867 ? C29 C29 C25 117.6(5) 2_867 2_867 ? C31 C30 C34 120.8(4) . 2_966 ? C31 C30 S2 118.9(3) . . ? C34 C30 S2 120.3(3) 2_966 . ? C30 C31 C32 120.7(4) . . ? C30 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 . . ? C33 C32 C31 120.4(4) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C32 C33 C34 121.5(4) . . ? C32 C33 H33A 119.2 . . ? C34 C33 H33A 119.2 . . ? C33 C34 C34 118.5(5) . 2_966 ? C33 C34 C30 123.4(4) . 2_966 ? C34 C34 C30 118.1(5) 2_966 2_966 ? C36 C35 C39 121.8(4) . 2_866 ? C36 C35 S3 117.2(3) . . ? C39 C35 S3 121.0(3) 2_866 . ? C35 C36 C37 120.1(4) . . ? C35 C36 H36A 119.9 . . ? C37 C36 H36A 119.9 . . ? C38 C37 C36 120.3(4) . . ? C38 C37 H37A 119.8 . . ? C36 C37 H37A 119.8 . . ? C37 C38 C39 121.3(4) . . ? C37 C38 H38A 119.3 . . ? C39 C38 H38A 119.3 . . ? C38 C39 C39 119.5(5) . 2_866 ? C38 C39 C35 123.6(4) . 2_866 ? C39 C39 C35 116.9(5) 2_866 2_866 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 S1 O1 Nd1 -25.2(5) . . . . ? O2 S1 O1 Nd1 -153.0(4) . . . . ? C25 S1 O1 Nd1 91.5(4) . . . . ? O4 Nd1 O1 S1 -178.6(4) . . . . ? O7 Nd1 O1 S1 -109.8(4) . . . . ? O1W Nd1 O1 S1 38.6(4) . . . . ? O2W Nd1 O1 S1 10.0(5) . . . . ? N4 Nd1 O1 S1 -39.3(4) . . . . ? N3 Nd1 O1 S1 -102.1(4) . . . . ? N2 Nd1 O1 S1 120.7(4) . . . . ? N1 Nd1 O1 S1 107.6(4) . . . . ? O4 Nd1 N1 C1 -89.5(4) . . . . ? O1 Nd1 N1 C1 -3.1(4) . . . . ? O7 Nd1 N1 C1 -148.8(3) . . . . ? O1W Nd1 N1 C1 76.6(4) . . . . ? O2W Nd1 N1 C1 132.4(4) . . . . ? N4 Nd1 N1 C1 52.9(4) . . . . ? N3 Nd1 N1 C1 -45.4(4) . . . . ? N2 Nd1 N1 C1 -172.7(4) . . . . ? O4 Nd1 N1 C12 99.4(3) . . . . ? O1 Nd1 N1 C12 -174.2(3) . . . . ? O7 Nd1 N1 C12 40.0(4) . . . . ? O1W Nd1 N1 C12 -94.5(3) . . . . ? O2W Nd1 N1 C12 -38.7(3) . . . . ? N4 Nd1 N1 C12 -118.3(3) . . . . ? N3 Nd1 N1 C12 143.4(3) . . . . ? N2 Nd1 N1 C12 16.1(3) . . . . ? C12 N1 C1 C2 1.9(7) . . . . ? Nd1 N1 C1 C2 -169.3(4) . . . . ? O4 Nd1 N2 C10 95.2(4) . . . . ? O1 Nd1 N2 C10 158.3(3) . . . . ? O7 Nd1 N2 C10 10.3(3) . . . . ? O1W Nd1 N2 C10 -127.6(4) . . . . ? O2W Nd1 N2 C10 -64.8(4) . . . . ? N4 Nd1 N2 C10 -53.3(4) . . . . ? N3 Nd1 N2 C10 45.3(4) . . . . ? N1 Nd1 N2 C10 172.9(4) . . . . ? O4 Nd1 N2 C11 -94.2(3) . . . . ? O1 Nd1 N2 C11 -31.1(4) . . . . ? O7 Nd1 N2 C11 -179.0(3) . . . . ? O1W Nd1 N2 C11 43.0(3) . . . . ? O2W Nd1 N2 C11 105.8(3) . . . . ? N4 Nd1 N2 C11 117.3(3) . . . . ? N3 Nd1 N2 C11 -144.1(3) . . . . ? N1 Nd1 N2 C11 -16.5(3) . . . . ? N1 C1 C2 C3 3.1(8) . . . . ? O4 Nd1 N3 C13 -4.5(3) . . . . ? O1 Nd1 N3 C13 -91.7(3) . . . . ? O7 Nd1 N3 C13 82.8(3) . . . . ? O1W Nd1 N3 C13 -143.3(3) . . . . ? O2W Nd1 N3 C13 134.4(3) . . . . ? N4 Nd1 N3 C13 179.2(4) . . . . ? N2 Nd1 N3 C13 45.7(4) . . . . ? N1 Nd1 N3 C13 -48.0(4) . . . . ? O4 Nd1 N3 C24 178.5(3) . . . . ? O1 Nd1 N3 C24 91.4(3) . . . . ? O7 Nd1 N3 C24 -94.2(3) . . . . ? O1W Nd1 N3 C24 39.7(3) . . . . ? O2W Nd1 N3 C24 -42.5(3) . . . . ? N4 Nd1 N3 C24 2.2(3) . . . . ? N2 Nd1 N3 C24 -131.2(3) . . . . ? N1 Nd1 N3 C24 135.1(3) . . . . ? C1 C2 C3 C4 -4.2(8) . . . . ? O5 S2 O4 Nd1 67.2(4) . . . . ? O6 S2 O4 Nd1 -63.6(4) . . . . ? C30 S2 O4 Nd1 -178.6(4) . . . . ? O1 Nd1 O4 S2 -70.3(4) . . . . ? O7 Nd1 O4 S2 148.6(4) . . . . ? O1W Nd1 O4 S2 -11.5(5) . . . . ? O2W Nd1 O4 S2 100.6(4) . . . . ? N4 Nd1 O4 S2 -137.9(4) . . . . ? N3 Nd1 O4 S2 -142.6(4) . . . . ? N2 Nd1 O4 S2 70.9(4) . . . . ? N1 Nd1 O4 S2 7.3(4) . . . . ? O4 Nd1 N4 C22 174.3(3) . . . . ? O1 Nd1 N4 C22 105.9(3) . . . . ? O7 Nd1 N4 C22 -113.3(3) . . . . ? O1W Nd1 N4 C22 28.8(4) . . . . ? O2W Nd1 N4 C22 -41.1(3) . . . . ? N3 Nd1 N4 C22 179.5(4) . . . . ? N2 Nd1 N4 C22 -52.4(4) . . . . ? N1 Nd1 N4 C22 51.2(4) . . . . ? O4 Nd1 N4 C23 -6.8(4) . . . . ? O1 Nd1 N4 C23 -75.3(3) . . . . ? O7 Nd1 N4 C23 65.5(3) . . . . ? O1W Nd1 N4 C23 -152.3(3) . . . . ? O2W Nd1 N4 C23 137.7(3) . . . . ? N3 Nd1 N4 C23 -1.7(3) . . . . ? N2 Nd1 N4 C23 126.4(3) . . . . ? N1 Nd1 N4 C23 -130.0(3) . . . . ? C2 C3 C4 C12 0.5(7) . . . . ? C2 C3 C4 C5 -176.9(5) . . . . ? C3 C4 C5 C6 172.5(5) . . . . ? C12 C4 C5 C6 -4.9(8) . . . . ? C4 C5 C6 C7 0.7(9) . . . . ? O8 S3 O7 Nd1 146.8(3) . . . . ? O9 S3 O7 Nd1 19.9(4) . . . . ? C35 S3 O7 Nd1 -95.9(4) . . . . ? O4 Nd1 O7 S3 -176.8(4) . . . . ? O1 Nd1 O7 S3 114.2(4) . . . . ? O1W Nd1 O7 S3 -17.0(5) . . . . ? O2W Nd1 O7 S3 -27.2(4) . . . . ? N4 Nd1 O7 S3 45.3(4) . . . . ? N3 Nd1 O7 S3 106.3(4) . . . . ? N2 Nd1 O7 S3 -99.4(4) . . . . ? N1 Nd1 O7 S3 -120.8(4) . . . . ? C5 C6 C7 C8 -173.5(5) . . . . ? C5 C6 C7 C11 4.7(8) . . . . ? C11 C7 C8 C9 0.2(7) . . . . ? C6 C7 C8 C9 178.4(5) . . . . ? C7 C8 C9 C10 2.9(7) . . . . ? C11 N2 C10 C9 -0.7(7) . . . . ? Nd1 N2 C10 C9 170.1(4) . . . . ? C8 C9 C10 N2 -2.9(8) . . . . ? C10 N2 C11 C7 4.0(6) . . . . ? Nd1 N2 C11 C7 -167.3(3) . . . . ? C10 N2 C11 C12 -172.3(4) . . . . ? Nd1 N2 C11 C12 16.4(5) . . . . ? C8 C7 C11 N2 -3.8(7) . . . . ? C6 C7 C11 N2 177.9(4) . . . . ? C8 C7 C11 C12 172.4(4) . . . . ? C6 C7 C11 C12 -5.8(7) . . . . ? C1 N1 C12 C4 -5.8(7) . . . . ? Nd1 N1 C12 C4 165.8(3) . . . . ? C1 N1 C12 C11 172.8(4) . . . . ? Nd1 N1 C12 C11 -15.6(5) . . . . ? C3 C4 C12 N1 4.7(7) . . . . ? C5 C4 C12 N1 -177.8(4) . . . . ? C3 C4 C12 C11 -173.9(4) . . . . ? C5 C4 C12 C11 3.6(7) . . . . ? N2 C11 C12 N1 -0.5(6) . . . . ? C7 C11 C12 N1 -176.8(4) . . . . ? N2 C11 C12 C4 178.1(4) . . . . ? C7 C11 C12 C4 1.8(7) . . . . ? C24 N3 C13 C14 -1.5(6) . . . . ? Nd1 N3 C13 C14 -178.5(3) . . . . ? N3 C13 C14 C15 0.9(7) . . . . ? C13 C14 C15 C16 0.3(7) . . . . ? C14 C15 C16 C24 -0.6(6) . . . . ? C14 C15 C16 C17 179.4(4) . . . . ? C15 C16 C17 C18 179.8(4) . . . . ? C24 C16 C17 C18 -0.1(7) . . . . ? C16 C17 C18 C19 -0.3(8) . . . . ? C17 C18 C19 C20 -179.6(5) . . . . ? C17 C18 C19 C23 -0.1(7) . . . . ? C23 C19 C20 C21 0.0(7) . . . . ? C18 C19 C20 C21 179.5(5) . . . . ? C19 C20 C21 C22 0.8(7) . . . . ? C23 N4 C22 C21 -0.7(7) . . . . ? Nd1 N4 C22 C21 178.2(4) . . . . ? C20 C21 C22 N4 -0.4(8) . . . . ? C22 N4 C23 C19 1.5(6) . . . . ? Nd1 N4 C23 C19 -177.4(3) . . . . ? C22 N4 C23 C24 180.0(4) . . . . ? Nd1 N4 C23 C24 1.0(5) . . . . ? C20 C19 C23 N4 -1.1(6) . . . . ? C18 C19 C23 N4 179.3(4) . . . . ? C20 C19 C23 C24 -179.6(4) . . . . ? C18 C19 C23 C24 0.8(6) . . . . ? C13 N3 C24 C16 1.0(6) . . . . ? Nd1 N3 C24 C16 178.2(3) . . . . ? C13 N3 C24 C23 -179.9(4) . . . . ? Nd1 N3 C24 C23 -2.8(5) . . . . ? C15 C16 C24 N3 0.0(6) . . . . ? C17 C16 C24 N3 179.9(4) . . . . ? C15 C16 C24 C23 -179.1(4) . . . . ? C17 C16 C24 C23 0.9(6) . . . . ? N4 C23 C24 N3 1.2(6) . . . . ? C19 C23 C24 N3 179.7(4) . . . . ? N4 C23 C24 C16 -179.8(4) . . . . ? C19 C23 C24 C16 -1.2(6) . . . . ? O3 S1 C25 C26 7.1(4) . . . . ? O2 S1 C25 C26 128.7(4) . . . . ? O1 S1 C25 C26 -113.3(4) . . . . ? O3 S1 C25 C29 -173.1(3) . . . 2_867 ? O2 S1 C25 C29 -51.5(4) . . . 2_867 ? O1 S1 C25 C29 66.6(4) . . . 2_867 ? C29 C25 C26 C27 2.7(7) 2_867 . . . ? S1 C25 C26 C27 -177.5(4) . . . . ? C25 C26 C27 C28 -0.2(7) . . . . ? C26 C27 C28 C29 -1.9(7) . . . . ? C27 C28 C29 C29 1.6(8) . . . 2_867 ? C27 C28 C29 C25 -177.5(4) . . . 2_867 ? O5 S2 C30 C31 -4.5(4) . . . . ? O6 S2 C30 C31 119.1(4) . . . . ? O4 S2 C30 C31 -121.9(3) . . . . ? O5 S2 C30 C34 176.8(3) . . . 2_966 ? O6 S2 C30 C34 -59.6(4) . . . 2_966 ? O4 S2 C30 C34 59.4(4) . . . 2_966 ? C34 C30 C31 C32 0.9(6) 2_966 . . . ? S2 C30 C31 C32 -177.7(3) . . . . ? C30 C31 C32 C33 -0.4(7) . . . . ? C31 C32 C33 C34 0.0(7) . . . . ? C32 C33 C34 C34 -0.2(7) . . . 2_966 ? C32 C33 C34 C30 -179.4(4) . . . 2_966 ? O8 S3 C35 C36 -131.0(3) . . . . ? O9 S3 C35 C36 -9.6(4) . . . . ? O7 S3 C35 C36 109.9(4) . . . . ? O8 S3 C35 C39 49.2(4) . . . 2_866 ? O9 S3 C35 C39 170.6(3) . . . 2_866 ? O7 S3 C35 C39 -69.9(4) . . . 2_866 ? C39 C35 C36 C37 -2.3(7) 2_866 . . . ? S3 C35 C36 C37 177.9(3) . . . . ? C35 C36 C37 C38 0.5(7) . . . . ? C36 C37 C38 C39 1.1(7) . . . . ? C37 C38 C39 C39 -0.9(7) . . . 2_866 ? C37 C38 C39 C35 178.3(4) . . . 2_866 ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.319 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.112 #==================================================END data_4 _database_code_depnum_ccdc_archive 'CCDC 637258' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H35 N4 O14 S3 Tb' _chemical_formula_weight 1038.81 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.175(3) _cell_length_b 12.937(3) _cell_length_c 13.847(3) _cell_angle_alpha 88.391(3) _cell_angle_beta 76.116(3) _cell_angle_gamma 77.176(3) _cell_volume 2063.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 6133 _cell_measurement_theta_min 2.5894 _cell_measurement_theta_max 26.4957 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 1.665 _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 1.938 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 11483 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.66 _reflns_number_total 8285 _reflns_number_gt 7070 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.9162P] 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 8285 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Tb1 Tb 0.606211(15) 0.826414(13) 0.727736(13) 0.02448(6) Uani 1 1 d . . . S1 S 0.54058(10) 0.75874(9) 1.00056(8) 0.0422(3) Uani 1 1 d . . . O1 O 0.5977(3) 0.7626(2) 0.8925(2) 0.0449(7) Uani 1 1 d . . . N1 N 0.7434(3) 0.9299(3) 0.5962(3) 0.0354(8) Uani 1 1 d . . . C1 C 0.7544(4) 0.9260(4) 0.4969(3) 0.0443(11) Uani 1 1 d . . . H1A H 0.7222 0.8770 0.4717 0.053 Uiso 1 1 calc R . . O1W O 0.5040(3) 0.9833(3) 0.8392(4) 0.0959(17) Uani 1 1 d . . . S2 S 0.91275(8) 0.68035(8) 0.70247(8) 0.0337(2) Uani 1 1 d . . . N2 N 0.7506(3) 0.9219(3) 0.7954(3) 0.0372(8) Uani 1 1 d . . . O2 O 0.6295(3) 0.7314(3) 1.0593(2) 0.0566(9) Uani 1 1 d . . . O2W O 0.4872(3) 0.9697(3) 0.6430(3) 0.0620(10) Uani 1 1 d . . . C2 C 0.8119(4) 0.9922(4) 0.4283(4) 0.0490(12) Uani 1 1 d . . . H2A H 0.8195 0.9843 0.3603 0.059 Uiso 1 1 calc R . . S3 S 0.54801(9) 0.75695(8) 0.48103(7) 0.0329(2) Uani 1 1 d . . . N3 N 0.3850(3) 0.8088(3) 0.7791(2) 0.0323(7) Uani 1 1 d . . . O3 O 0.4517(3) 0.8560(3) 1.0366(3) 0.0591(9) Uani 1 1 d . . . O3W O 0.6786(4) 0.8393(3) 0.2071(3) 0.0701(11) Uani 1 1 d . . . C3 C 0.8564(4) 1.0683(4) 0.4646(4) 0.0520(13) Uani 1 1 d . . . H3A H 0.8913 1.1144 0.4213 0.062 Uiso 1 1 calc R . . N4 N 0.5651(3) 0.6287(2) 0.7373(2) 0.0299(7) Uani 1 1 d . . . O4 O 0.7898(2) 0.7105(2) 0.6924(2) 0.0335(6) Uani 1 1 d . . . C4 C 0.8951(4) 1.1526(4) 0.6123(5) 0.0614(15) Uani 1 1 d . . . H4A H 0.9242 1.2043 0.5727 0.074 Uiso 1 1 calc R . . O4W O 0.9191(7) 0.6099(6) 1.0082(4) 0.154(3) Uani 1 1 d . . . O5 O 0.9818(3) 0.7550(2) 0.6544(3) 0.0526(8) Uani 1 1 d . . . C5 C 0.8969(4) 1.1496(4) 0.7100(5) 0.0621(15) Uani 1 1 d . . . H5A H 0.9268 1.1997 0.7362 0.074 Uiso 1 1 calc R . . O5W O 0.9341(5) 0.7876(6) 0.1278(5) 0.139(2) Uani 1 1 d . . . O6 O 0.9179(3) 0.6570(3) 0.8057(2) 0.0541(9) Uani 1 1 d . . . C6 C 0.8660(4) 1.0560(4) 0.8744(4) 0.0582(14) Uani 1 1 d . . . H6A H 0.9009 1.1011 0.9018 0.070 Uiso 1 1 calc R . . O7 O 0.6047(3) 0.7569(2) 0.5655(2) 0.0385(7) Uani 1 1 d . . . C7 C 0.8261(4) 0.9746(4) 0.9304(4) 0.0564(13) Uani 1 1 d . . . H7A H 0.8369 0.9625 0.9943 0.068 Uiso 1 1 calc R . . O8 O 0.6359(3) 0.7331(2) 0.3855(2) 0.0467(8) Uani 1 1 d . . . C8 C 0.7685(4) 0.9106(4) 0.8874(4) 0.0475(11) Uani 1 1 d . . . H8A H 0.7414 0.8572 0.9256 0.057 Uiso 1 1 calc R . . O9 O 0.4595(3) 0.8557(2) 0.4804(2) 0.0442(7) Uani 1 1 d . . . C9 C 0.8482(4) 1.0758(3) 0.5683(4) 0.0455(11) Uani 1 1 d . . . C10 C 0.8528(4) 1.0693(3) 0.7747(4) 0.0502(12) Uani 1 1 d . . . C11 C 0.7938(3) 1.0015(3) 0.6318(3) 0.0366(10) Uani 1 1 d . . . C12 C 0.7969(3) 0.9989(3) 0.7369(3) 0.0365(9) Uani 1 1 d . . . C13 C 0.2959(4) 0.8955(3) 0.8010(3) 0.0414(10) Uani 1 1 d . . . H13A H 0.3136 0.9619 0.7990 0.050 Uiso 1 1 calc R . . C14 C 0.1772(4) 0.8902(4) 0.8268(3) 0.0467(11) Uani 1 1 d . . . H14A H 0.1194 0.9519 0.8418 0.056 Uiso 1 1 calc R . . C15 C 0.1478(4) 0.7921(4) 0.8295(3) 0.0447(11) Uani 1 1 d . . . H15A H 0.0705 0.7874 0.8451 0.054 Uiso 1 1 calc R . . C16 C 0.2148(4) 0.5928(4) 0.8108(3) 0.0487(12) Uani 1 1 d . . . H16A H 0.1382 0.5855 0.8264 0.058 Uiso 1 1 calc R . . C17 C 0.3020(4) 0.5053(4) 0.7909(3) 0.0446(11) Uani 1 1 d . . . H17A H 0.2842 0.4388 0.7936 0.053 Uiso 1 1 calc R . . C18 C 0.5166(4) 0.4224(3) 0.7440(3) 0.0391(10) Uani 1 1 d . . . H18A H 0.5018 0.3547 0.7462 0.047 Uiso 1 1 calc R . . C19 C 0.6301(4) 0.4355(3) 0.7197(3) 0.0404(10) Uani 1 1 d . . . H19A H 0.6921 0.3770 0.7055 0.048 Uiso 1 1 calc R . . C20 C 0.6495(4) 0.5403(3) 0.7168(3) 0.0369(9) Uani 1 1 d . . . H20A H 0.7259 0.5479 0.6996 0.044 Uiso 1 1 calc R . . C21 C 0.2389(4) 0.6983(3) 0.8080(3) 0.0369(9) Uani 1 1 d . . . C22 C 0.4232(4) 0.5128(3) 0.7654(3) 0.0356(9) Uani 1 1 d . . . C23 C 0.3568(3) 0.7103(3) 0.7832(3) 0.0296(8) Uani 1 1 d . . . C24 C 0.4514(3) 0.6158(3) 0.7613(3) 0.0281(8) Uani 1 1 d . . . C25 C 0.4671(4) 0.6509(3) 1.0117(3) 0.0364(9) Uani 1 1 d . . . C26 C 0.5332(4) 0.5412(3) 0.9921(3) 0.0352(9) Uani 1 1 d . . . C27 C 0.6575(4) 0.5113(4) 0.9595(3) 0.0436(10) Uani 1 1 d . . . H27A H 0.6995 0.5641 0.9480 0.052 Uiso 1 1 calc R . . C28 C 0.7160(4) 0.4070(4) 0.9449(3) 0.0483(11) Uani 1 1 d . . . H28A H 0.7967 0.3902 0.9258 0.058 Uiso 1 1 calc R . . C29 C 0.3465(4) 0.6759(4) 1.0409(3) 0.0442(10) Uani 1 1 d . . . H29A H 0.3066 0.7463 1.0512 0.053 Uiso 1 1 calc R . . C30 C 0.9713(3) 0.5558(3) 0.6322(3) 0.0310(8) Uani 1 1 d . . . C31 C 0.9741(3) 0.5504(3) 0.5269(3) 0.0286(8) Uani 1 1 d . . . C32 C 0.9281(3) 0.6403(3) 0.4720(3) 0.0349(9) Uani 1 1 d . . . H32A H 0.8943 0.7052 0.5055 0.042 Uiso 1 1 calc R . . C33 C 0.9329(4) 0.6325(3) 0.3722(3) 0.0390(10) Uani 1 1 d . . . H33A H 0.9032 0.6918 0.3391 0.047 Uiso 1 1 calc R . . C34 C 1.0163(3) 0.4667(3) 0.6810(3) 0.0373(9) Uani 1 1 d . . . H34A H 1.0134 0.4716 0.7485 0.045 Uiso 1 1 calc R . . C35 C 0.4719(3) 0.6505(3) 0.5027(3) 0.0297(8) Uani 1 1 d . . . C36 C 0.5344(3) 0.5400(3) 0.4926(3) 0.0269(8) Uani 1 1 d . . . C37 C 0.6595(3) 0.5072(3) 0.4686(3) 0.0341(9) Uani 1 1 d . . . H37A H 0.7036 0.5584 0.4602 0.041 Uiso 1 1 calc R . . C38 C 0.7151(3) 0.4012(3) 0.4577(3) 0.0394(10) Uani 1 1 d . . . H38A H 0.7957 0.3820 0.4405 0.047 Uiso 1 1 calc R . . C39 C 0.3507(3) 0.6786(3) 0.5274(3) 0.0360(9) Uani 1 1 d . . . H39A H 0.3129 0.7498 0.5342 0.043 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 Tb1 0.02291(9) 0.02220(9) 0.03058(10) 0.00172(6) -0.00807(7) -0.00799(7) S1 0.0545(7) 0.0491(6) 0.0299(5) 0.0010(5) -0.0105(5) -0.0252(5) O1 0.0558(19) 0.0541(19) 0.0313(16) 0.0033(13) -0.0085(14) -0.0279(16) N1 0.0315(17) 0.0292(17) 0.049(2) 0.0097(15) -0.0118(16) -0.0122(14) C1 0.037(2) 0.047(3) 0.052(3) 0.012(2) -0.016(2) -0.013(2) O1W 0.059(2) 0.077(3) 0.157(4) -0.071(3) -0.060(3) 0.019(2) S2 0.0249(5) 0.0329(5) 0.0447(6) -0.0069(4) -0.0101(4) -0.0066(4) N2 0.0354(18) 0.0351(18) 0.045(2) -0.0025(15) -0.0113(16) -0.0139(15) O2 0.071(2) 0.070(2) 0.0455(19) 0.0057(16) -0.0286(17) -0.0340(19) O2W 0.0439(19) 0.049(2) 0.077(2) 0.0269(17) 0.0024(17) 0.0028(15) C2 0.034(2) 0.054(3) 0.057(3) 0.021(2) -0.006(2) -0.013(2) S3 0.0421(6) 0.0308(5) 0.0342(5) 0.0089(4) -0.0172(4) -0.0177(4) N3 0.0278(17) 0.0331(17) 0.0385(19) 0.0031(14) -0.0086(14) -0.0114(14) O3 0.070(2) 0.047(2) 0.058(2) -0.0114(16) -0.0061(18) -0.0185(17) O3W 0.114(3) 0.042(2) 0.058(2) 0.0051(16) -0.022(2) -0.024(2) C3 0.031(2) 0.044(3) 0.074(4) 0.028(2) -0.001(2) -0.011(2) N4 0.0331(17) 0.0275(16) 0.0325(17) 0.0044(13) -0.0104(14) -0.0116(14) O4 0.0232(13) 0.0316(14) 0.0462(16) -0.0034(12) -0.0095(12) -0.0053(11) C4 0.042(3) 0.033(2) 0.112(5) 0.014(3) -0.012(3) -0.022(2) O4W 0.224(8) 0.178(6) 0.075(4) 0.003(4) -0.007(4) -0.104(6) O5 0.0359(17) 0.0414(18) 0.081(2) -0.0106(16) -0.0025(16) -0.0204(14) C5 0.047(3) 0.038(3) 0.107(5) -0.009(3) -0.013(3) -0.024(2) O5W 0.145(5) 0.185(6) 0.137(5) 0.024(4) -0.066(4) -0.107(5) O6 0.053(2) 0.059(2) 0.0507(19) -0.0136(16) -0.0260(16) 0.0026(16) C6 0.036(2) 0.054(3) 0.089(4) -0.029(3) -0.019(3) -0.010(2) O7 0.0506(17) 0.0352(15) 0.0408(16) 0.0076(12) -0.0230(14) -0.0205(13) C7 0.047(3) 0.068(3) 0.061(3) -0.019(3) -0.018(2) -0.019(3) O8 0.057(2) 0.0482(18) 0.0400(17) 0.0098(14) -0.0090(15) -0.0255(16) C8 0.041(2) 0.053(3) 0.054(3) -0.007(2) -0.014(2) -0.017(2) O9 0.0523(18) 0.0317(15) 0.0579(19) 0.0108(14) -0.0273(16) -0.0143(14) C9 0.027(2) 0.030(2) 0.077(3) 0.013(2) -0.007(2) -0.0097(17) C10 0.033(2) 0.035(2) 0.085(4) -0.015(2) -0.015(2) -0.0102(19) C11 0.0223(19) 0.0223(19) 0.063(3) 0.0065(18) -0.0056(19) -0.0058(15) C12 0.0233(19) 0.027(2) 0.058(3) -0.0035(18) -0.0088(19) -0.0059(16) C13 0.033(2) 0.037(2) 0.054(3) 0.001(2) -0.011(2) -0.0053(18) C14 0.028(2) 0.053(3) 0.055(3) 0.000(2) -0.007(2) -0.004(2) C15 0.027(2) 0.060(3) 0.050(3) 0.001(2) -0.0117(19) -0.011(2) C16 0.044(3) 0.061(3) 0.052(3) 0.004(2) -0.011(2) -0.035(2) C17 0.052(3) 0.048(3) 0.047(3) 0.008(2) -0.016(2) -0.034(2) C18 0.059(3) 0.033(2) 0.034(2) 0.0051(17) -0.017(2) -0.023(2) C19 0.054(3) 0.024(2) 0.042(2) -0.0009(17) -0.015(2) -0.0052(19) C20 0.034(2) 0.032(2) 0.047(2) 0.0035(18) -0.0121(19) -0.0099(18) C21 0.036(2) 0.048(2) 0.032(2) 0.0022(18) -0.0092(18) -0.0195(19) C22 0.048(2) 0.039(2) 0.029(2) 0.0085(17) -0.0143(18) -0.024(2) C23 0.0308(19) 0.037(2) 0.0252(19) 0.0019(15) -0.0086(16) -0.0135(16) C24 0.038(2) 0.0291(19) 0.0250(19) 0.0066(15) -0.0150(16) -0.0162(17) C25 0.045(2) 0.046(2) 0.025(2) 0.0070(17) -0.0124(18) -0.021(2) C26 0.042(2) 0.049(3) 0.0227(19) 0.0056(17) -0.0125(17) -0.022(2) C27 0.039(2) 0.055(3) 0.042(2) 0.005(2) -0.010(2) -0.021(2) C28 0.037(2) 0.062(3) 0.049(3) 0.007(2) -0.013(2) -0.015(2) C29 0.044(3) 0.049(3) 0.040(2) 0.004(2) -0.010(2) -0.013(2) C30 0.0209(18) 0.029(2) 0.044(2) 0.0021(17) -0.0090(16) -0.0064(15) C31 0.0207(17) 0.0254(18) 0.040(2) 0.0009(16) -0.0061(16) -0.0078(14) C32 0.030(2) 0.0256(19) 0.047(2) 0.0011(17) -0.0086(18) -0.0034(16) C33 0.033(2) 0.035(2) 0.048(3) 0.0087(19) -0.0104(19) -0.0056(18) C34 0.033(2) 0.042(2) 0.039(2) 0.0008(18) -0.0086(18) -0.0119(18) C35 0.037(2) 0.0282(19) 0.030(2) 0.0029(15) -0.0134(17) -0.0134(17) C36 0.0301(19) 0.0293(19) 0.0262(18) 0.0036(15) -0.0113(15) -0.0124(16) C37 0.030(2) 0.038(2) 0.041(2) 0.0072(17) -0.0112(17) -0.0175(17) C38 0.0234(19) 0.043(2) 0.051(3) 0.003(2) -0.0088(18) -0.0078(18) C39 0.033(2) 0.031(2) 0.044(2) 0.0005(17) -0.0136(19) -0.0038(17) _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 Tb1 O4 2.348(3) . ? Tb1 O1 2.391(3) . ? Tb1 O7 2.449(3) . ? Tb1 O1W 2.486(4) . ? Tb1 O2W 2.532(3) . ? Tb1 N3 2.675(3) . ? Tb1 N1 2.702(3) . ? Tb1 N2 2.705(3) . ? Tb1 N4 2.707(3) . ? S1 O3 1.474(4) . ? S1 O2 1.481(3) . ? S1 O1 1.495(3) . ? S1 C25 1.802(4) . ? N1 C1 1.350(6) . ? N1 C11 1.378(5) . ? C1 C2 1.424(6) . ? C1 H1A 0.9300 . ? S2 O5 1.462(3) . ? S2 O6 1.466(3) . ? S2 O4 1.501(3) . ? S2 C30 1.816(4) . ? N2 C8 1.341(6) . ? N2 C12 1.397(5) . ? C2 C3 1.382(7) . ? C2 H2A 0.9300 . ? S3 O9 1.479(3) . ? S3 O8 1.479(3) . ? S3 O7 1.494(3) . ? S3 C35 1.804(4) . ? N3 C13 1.360(5) . ? N3 C23 1.388(5) . ? C3 C9 1.421(7) . ? C3 H3A 0.9300 . ? N4 C20 1.342(5) . ? N4 C24 1.390(5) . ? C4 C5 1.358(8) . ? C4 C9 1.461(7) . ? C4 H4A 0.9300 . ? C5 C10 1.461(7) . ? C5 H5A 0.9300 . ? C6 C7 1.395(8) . ? C6 C10 1.430(7) . ? C6 H6A 0.9300 . ? C7 C8 1.419(6) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? C9 C11 1.446(6) . ? C10 C12 1.428(6) . ? C11 C12 1.464(6) . ? C13 C14 1.420(6) . ? C13 H13A 0.9300 . ? C14 C15 1.389(6) . ? C14 H14A 0.9300 . ? C15 C21 1.434(6) . ? C15 H15A 0.9300 . ? C16 C17 1.352(7) . ? C16 C21 1.456(6) . ? C16 H16A 0.9300 . ? C17 C22 1.458(6) . ? C17 H17A 0.9300 . ? C18 C19 1.389(6) . ? C18 C22 1.420(6) . ? C18 H18A 0.9300 . ? C19 C20 1.425(5) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C23 1.437(5) . ? C22 C24 1.444(5) . ? C23 C24 1.463(6) . ? C25 C29 1.392(6) . ? C25 C26 1.465(6) . ? C26 C27 1.437(6) . ? C26 C26 1.456(8) 2_667 ? C27 C28 1.374(7) . ? C27 H27A 0.9300 . ? C28 C29 1.430(6) 2_667 ? C28 H28A 0.9300 . ? C29 C28 1.430(6) 2_667 ? C29 H29A 0.9300 . ? C30 C34 1.392(6) . ? C30 C31 1.453(6) . ? C31 C32 1.453(5) . ? C31 C31 1.455(7) 2_766 ? C32 C33 1.375(6) . ? C32 H32A 0.9300 . ? C33 C34 1.434(6) 2_766 ? C33 H33A 0.9300 . ? C34 C33 1.434(6) 2_766 ? C34 H34A 0.9300 . ? C35 C39 1.398(5) . ? C35 C36 1.456(5) . ? C36 C37 1.445(5) . ? C36 C36 1.452(7) 2_666 ? C37 C38 1.382(6) . ? C37 H37A 0.9300 . ? C38 C39 1.423(6) 2_666 ? C38 H38A 0.9300 . ? C39 C38 1.423(6) 2_666 ? C39 H39A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Tb1 O1 83.20(10) . . ? O4 Tb1 O7 81.28(9) . . ? O1 Tb1 O7 137.50(9) . . ? O4 Tb1 O1W 137.14(10) . . ? O1 Tb1 O1W 75.08(15) . . ? O7 Tb1 O1W 138.10(12) . . ? O4 Tb1 O2W 138.86(10) . . ? O1 Tb1 O2W 137.32(11) . . ? O7 Tb1 O2W 71.44(11) . . ? O1W Tb1 O2W 67.41(14) . . ? O4 Tb1 N3 136.70(10) . . ? O1 Tb1 N3 80.41(10) . . ? O7 Tb1 N3 84.37(10) . . ? O1W Tb1 N3 75.58(12) . . ? O2W Tb1 N3 71.35(10) . . ? O4 Tb1 N1 75.29(10) . . ? O1 Tb1 N1 136.48(10) . . ? O7 Tb1 N1 76.13(10) . . ? O1W Tb1 N1 95.75(15) . . ? O2W Tb1 N1 68.75(10) . . ? N3 Tb1 N1 139.37(10) . . ? O4 Tb1 N2 72.75(10) . . ? O1 Tb1 N2 75.84(10) . . ? O7 Tb1 N2 134.71(10) . . ? O1W Tb1 N2 66.37(11) . . ? O2W Tb1 N2 105.59(11) . . ? N3 Tb1 N2 139.05(10) . . ? N1 Tb1 N2 61.87(11) . . ? O4 Tb1 N4 74.39(9) . . ? O1 Tb1 N4 70.39(10) . . ? O7 Tb1 N4 67.37(9) . . ? O1W Tb1 N4 128.73(14) . . ? O2W Tb1 N4 119.45(11) . . ? N3 Tb1 N4 62.38(10) . . ? N1 Tb1 N4 135.24(10) . . ? N2 Tb1 N4 134.93(10) . . ? O3 S1 O2 113.8(2) . . ? O3 S1 O1 112.2(2) . . ? O2 S1 O1 110.1(2) . . ? O3 S1 C25 107.2(2) . . ? O2 S1 C25 107.03(19) . . ? O1 S1 C25 106.00(18) . . ? S1 O1 Tb1 153.5(2) . . ? C1 N1 C11 117.0(3) . . ? C1 N1 Tb1 123.6(3) . . ? C11 N1 Tb1 118.8(3) . . ? N1 C1 C2 124.1(4) . . ? N1 C1 H1A 117.9 . . ? C2 C1 H1A 117.9 . . ? O5 S2 O6 115.1(2) . . ? O5 S2 O4 112.47(18) . . ? O6 S2 O4 111.43(18) . . ? O5 S2 C30 106.70(18) . . ? O6 S2 C30 106.50(19) . . ? O4 S2 C30 103.61(16) . . ? C8 N2 C12 117.2(4) . . ? C8 N2 Tb1 123.9(3) . . ? C12 N2 Tb1 118.3(3) . . ? C3 C2 C1 118.9(5) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? O9 S3 O8 113.33(18) . . ? O9 S3 O7 111.82(17) . . ? O8 S3 O7 110.82(18) . . ? O9 S3 C35 106.60(18) . . ? O8 S3 C35 107.59(18) . . ? O7 S3 C35 106.23(16) . . ? C13 N3 C23 117.3(3) . . ? C13 N3 Tb1 121.6(3) . . ? C23 N3 Tb1 121.0(2) . . ? C2 C3 C9 119.5(4) . . ? C2 C3 H3A 120.2 . . ? C9 C3 H3A 120.2 . . ? C20 N4 C24 117.0(3) . . ? C20 N4 Tb1 123.4(2) . . ? C24 N4 Tb1 119.6(2) . . ? S2 O4 Tb1 150.60(16) . . ? C5 C4 C9 121.0(4) . . ? C5 C4 H4A 119.5 . . ? C9 C4 H4A 119.5 . . ? C4 C5 C10 121.3(5) . . ? C4 C5 H5A 119.4 . . ? C10 C5 H5A 119.4 . . ? C7 C6 C10 119.4(4) . . ? C7 C6 H6A 120.3 . . ? C10 C6 H6A 120.3 . . ? S3 O7 Tb1 150.51(18) . . ? C6 C7 C8 118.4(5) . . ? C6 C7 H7A 120.8 . . ? C8 C7 H7A 120.8 . . ? N2 C8 C7 124.6(5) . . ? N2 C8 H8A 117.7 . . ? C7 C8 H8A 117.7 . . ? C3 C9 C11 117.7(4) . . ? C3 C9 C4 122.9(4) . . ? C11 C9 C4 119.3(5) . . ? C12 C10 C6 118.0(4) . . ? C12 C10 C5 119.3(5) . . ? C6 C10 C5 122.6(4) . . ? N1 C11 C9 122.5(4) . . ? N1 C11 C12 118.7(3) . . ? C9 C11 C12 118.8(4) . . ? N2 C12 C10 122.2(4) . . ? N2 C12 C11 117.8(3) . . ? C10 C12 C11 119.8(4) . . ? N3 C13 C14 123.6(4) . . ? N3 C13 H13A 118.2 . . ? C14 C13 H13A 118.2 . . ? C15 C14 C13 119.5(4) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C14 C15 C21 118.9(4) . . ? C14 C15 H15A 120.6 . . ? C21 C15 H15A 120.6 . . ? C17 C16 C21 120.9(4) . . ? C17 C16 H16A 119.5 . . ? C21 C16 H16A 119.5 . . ? C16 C17 C22 121.5(4) . . ? C16 C17 H17A 119.2 . . ? C22 C17 H17A 119.2 . . ? C19 C18 C22 119.7(4) . . ? C19 C18 H18A 120.2 . . ? C22 C18 H18A 120.2 . . ? C18 C19 C20 118.7(4) . . ? C18 C19 H19A 120.7 . . ? C20 C19 H19A 120.7 . . ? N4 C20 C19 124.5(4) . . ? N4 C20 H20A 117.8 . . ? C19 C20 H20A 117.8 . . ? C15 C21 C23 118.2(4) . . ? C15 C21 C16 121.9(4) . . ? C23 C21 C16 119.9(4) . . ? C18 C22 C24 117.7(4) . . ? C18 C22 C17 122.7(4) . . ? C24 C22 C17 119.5(4) . . ? N3 C23 C21 122.4(4) . . ? N3 C23 C24 118.3(3) . . ? C21 C23 C24 119.3(3) . . ? N4 C24 C22 122.5(3) . . ? N4 C24 C23 118.7(3) . . ? C22 C24 C23 118.8(3) . . ? C29 C25 C26 121.8(4) . . ? C29 C25 S1 117.6(3) . . ? C26 C25 S1 120.6(3) . . ? C27 C26 C26 119.2(5) . 2_667 ? C27 C26 C25 124.0(4) . . ? C26 C26 C25 116.8(5) 2_667 . ? C28 C27 C26 122.0(4) . . ? C28 C27 H27A 119.0 . . ? C26 C27 H27A 119.0 . . ? C27 C28 C29 120.3(4) . 2_667 ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 2_667 . ? C25 C29 C28 119.9(4) . 2_667 ? C25 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 2_667 . ? C34 C30 C31 121.1(4) . . ? C34 C30 S2 118.3(3) . . ? C31 C30 S2 120.6(3) . . ? C32 C31 C30 123.6(3) . . ? C32 C31 C31 118.0(4) . 2_766 ? C30 C31 C31 118.4(4) . 2_766 ? C33 C32 C31 122.0(4) . . ? C33 C32 H32A 119.0 . . ? C31 C32 H32A 119.0 . . ? C32 C33 C34 120.2(4) . 2_766 ? C32 C33 H33A 119.9 . . ? C34 C33 H33A 119.9 2_766 . ? C30 C34 C33 120.3(4) . 2_766 ? C30 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 2_766 . ? C39 C35 C36 121.5(3) . . ? C39 C35 S3 117.2(3) . . ? C36 C35 S3 121.3(3) . . ? C37 C36 C36 119.3(4) . 2_666 ? C37 C36 C35 123.5(3) . . ? C36 C36 C35 117.2(4) 2_666 . ? C38 C37 C36 121.4(3) . . ? C38 C37 H37A 119.3 . . ? C36 C37 H37A 119.3 . . ? C37 C38 C39 120.2(4) . 2_666 ? C37 C38 H38A 119.9 . . ? C39 C38 H38A 119.9 2_666 . ? C35 C39 C38 120.3(4) . 2_666 ? C35 C39 H39A 119.8 . . ? C38 C39 H39A 119.8 2_666 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 S1 O1 Tb1 -22.3(5) . . . . ? O2 S1 O1 Tb1 -150.1(4) . . . . ? C25 S1 O1 Tb1 94.4(4) . . . . ? O4 Tb1 O1 S1 178.9(4) . . . . ? O7 Tb1 O1 S1 -112.0(4) . . . . ? O1W Tb1 O1 S1 36.2(4) . . . . ? O2W Tb1 O1 S1 7.2(5) . . . . ? N3 Tb1 O1 S1 -41.3(4) . . . . ? N1 Tb1 O1 S1 118.7(4) . . . . ? N2 Tb1 O1 S1 105.0(4) . . . . ? N4 Tb1 O1 S1 -105.3(4) . . . . ? O4 Tb1 N1 C1 93.7(3) . . . . ? O1 Tb1 N1 C1 156.7(3) . . . . ? O7 Tb1 N1 C1 9.2(3) . . . . ? O1W Tb1 N1 C1 -129.0(3) . . . . ? O2W Tb1 N1 C1 -66.0(3) . . . . ? N3 Tb1 N1 C1 -54.5(4) . . . . ? N2 Tb1 N1 C1 171.7(3) . . . . ? N4 Tb1 N1 C1 45.0(4) . . . . ? O4 Tb1 N1 C11 -95.0(3) . . . . ? O1 Tb1 N1 C11 -32.0(3) . . . . ? O7 Tb1 N1 C11 -179.5(3) . . . . ? O1W Tb1 N1 C11 42.3(3) . . . . ? O2W Tb1 N1 C11 105.3(3) . . . . ? N3 Tb1 N1 C11 116.8(3) . . . . ? N2 Tb1 N1 C11 -17.0(2) . . . . ? N4 Tb1 N1 C11 -143.7(2) . . . . ? C11 N1 C1 C2 -1.4(6) . . . . ? Tb1 N1 C1 C2 170.0(3) . . . . ? O4 Tb1 N2 C8 -89.5(3) . . . . ? O1 Tb1 N2 C8 -2.3(3) . . . . ? O7 Tb1 N2 C8 -147.4(3) . . . . ? O1W Tb1 N2 C8 77.4(4) . . . . ? O2W Tb1 N2 C8 133.5(3) . . . . ? N3 Tb1 N2 C8 54.1(4) . . . . ? N1 Tb1 N2 C8 -171.7(4) . . . . ? N4 Tb1 N2 C8 -44.5(4) . . . . ? O4 Tb1 N2 C12 99.8(3) . . . . ? O1 Tb1 N2 C12 -173.0(3) . . . . ? O7 Tb1 N2 C12 41.9(3) . . . . ? O1W Tb1 N2 C12 -93.3(3) . . . . ? O2W Tb1 N2 C12 -37.2(3) . . . . ? N3 Tb1 N2 C12 -116.6(3) . . . . ? N1 Tb1 N2 C12 17.6(3) . . . . ? N4 Tb1 N2 C12 144.8(3) . . . . ? N1 C1 C2 C3 -2.4(7) . . . . ? O4 Tb1 N3 C13 175.6(3) . . . . ? O1 Tb1 N3 C13 106.3(3) . . . . ? O7 Tb1 N3 C13 -113.5(3) . . . . ? O1W Tb1 N3 C13 29.4(3) . . . . ? O2W Tb1 N3 C13 -41.2(3) . . . . ? N1 Tb1 N3 C13 -52.5(4) . . . . ? N2 Tb1 N3 C13 51.3(4) . . . . ? N4 Tb1 N3 C13 179.1(3) . . . . ? O4 Tb1 N3 C23 -5.2(3) . . . . ? O1 Tb1 N3 C23 -74.5(3) . . . . ? O7 Tb1 N3 C23 65.7(3) . . . . ? O1W Tb1 N3 C23 -151.4(3) . . . . ? O2W Tb1 N3 C23 138.0(3) . . . . ? N1 Tb1 N3 C23 126.7(3) . . . . ? N2 Tb1 N3 C23 -129.5(3) . . . . ? N4 Tb1 N3 C23 -1.7(2) . . . . ? C1 C2 C3 C9 2.7(6) . . . . ? O4 Tb1 N4 C20 -3.2(3) . . . . ? O1 Tb1 N4 C20 -91.4(3) . . . . ? O7 Tb1 N4 C20 83.7(3) . . . . ? O1W Tb1 N4 C20 -141.9(3) . . . . ? O2W Tb1 N4 C20 134.5(3) . . . . ? N3 Tb1 N4 C20 179.3(3) . . . . ? N1 Tb1 N4 C20 45.8(3) . . . . ? N2 Tb1 N4 C20 -47.7(3) . . . . ? O4 Tb1 N4 C24 179.1(3) . . . . ? O1 Tb1 N4 C24 90.9(3) . . . . ? O7 Tb1 N4 C24 -94.0(3) . . . . ? O1W Tb1 N4 C24 40.4(3) . . . . ? O2W Tb1 N4 C24 -43.2(3) . . . . ? N3 Tb1 N4 C24 1.6(2) . . . . ? N1 Tb1 N4 C24 -131.9(2) . . . . ? N2 Tb1 N4 C24 134.6(2) . . . . ? O5 S2 O4 Tb1 -66.2(4) . . . . ? O6 S2 O4 Tb1 64.8(4) . . . . ? C30 S2 O4 Tb1 178.9(3) . . . . ? O1 Tb1 O4 S2 -68.6(3) . . . . ? O7 Tb1 O4 S2 151.1(4) . . . . ? O1W Tb1 O4 S2 -9.3(5) . . . . ? O2W Tb1 O4 S2 102.7(4) . . . . ? N3 Tb1 O4 S2 -136.8(3) . . . . ? N1 Tb1 O4 S2 73.2(3) . . . . ? N2 Tb1 O4 S2 8.6(3) . . . . ? N4 Tb1 O4 S2 -140.1(4) . . . . ? C9 C4 C5 C10 0.4(8) . . . . ? O9 S3 O7 Tb1 18.3(4) . . . . ? O8 S3 O7 Tb1 145.8(3) . . . . ? C35 S3 O7 Tb1 -97.6(3) . . . . ? O4 Tb1 O7 S3 -175.2(3) . . . . ? O1 Tb1 O7 S3 115.0(3) . . . . ? O1W Tb1 O7 S3 -15.2(4) . . . . ? O2W Tb1 O7 S3 -26.4(3) . . . . ? N3 Tb1 O7 S3 45.8(3) . . . . ? N1 Tb1 O7 S3 -98.3(3) . . . . ? N2 Tb1 O7 S3 -120.2(3) . . . . ? N4 Tb1 O7 S3 108.2(3) . . . . ? C10 C6 C7 C8 -2.9(7) . . . . ? C12 N2 C8 C7 3.2(7) . . . . ? Tb1 N2 C8 C7 -167.6(4) . . . . ? C6 C7 C8 N2 0.8(7) . . . . ? C2 C3 C9 C11 0.5(6) . . . . ? C2 C3 C9 C4 178.7(4) . . . . ? C5 C4 C9 C3 -172.7(5) . . . . ? C5 C4 C9 C11 5.4(7) . . . . ? C7 C6 C10 C12 1.0(7) . . . . ? C7 C6 C10 C5 -177.2(5) . . . . ? C4 C5 C10 C12 -5.9(7) . . . . ? C4 C5 C10 C6 172.3(5) . . . . ? C1 N1 C11 C9 4.9(6) . . . . ? Tb1 N1 C11 C9 -167.0(3) . . . . ? C1 N1 C11 C12 -172.3(4) . . . . ? Tb1 N1 C11 C12 15.8(4) . . . . ? C3 C9 C11 N1 -4.6(6) . . . . ? C4 C9 C11 N1 177.2(4) . . . . ? C3 C9 C11 C12 172.7(4) . . . . ? C4 C9 C11 C12 -5.6(6) . . . . ? C8 N2 C12 C10 -5.1(6) . . . . ? Tb1 N2 C12 C10 166.2(3) . . . . ? C8 N2 C12 C11 170.8(4) . . . . ? Tb1 N2 C12 C11 -17.9(4) . . . . ? C6 C10 C12 N2 3.1(6) . . . . ? C5 C10 C12 N2 -178.6(4) . . . . ? C6 C10 C12 C11 -172.7(4) . . . . ? C5 C10 C12 C11 5.5(6) . . . . ? N1 C11 C12 N2 1.4(5) . . . . ? C9 C11 C12 N2 -175.9(3) . . . . ? N1 C11 C12 C10 177.5(4) . . . . ? C9 C11 C12 C10 0.1(6) . . . . ? C23 N3 C13 C14 -0.5(6) . . . . ? Tb1 N3 C13 C14 178.8(3) . . . . ? N3 C13 C14 C15 -0.6(7) . . . . ? C13 C14 C15 C21 1.2(7) . . . . ? C21 C16 C17 C22 -0.4(7) . . . . ? C22 C18 C19 C20 -0.1(6) . . . . ? C24 N4 C20 C19 -1.1(6) . . . . ? Tb1 N4 C20 C19 -178.9(3) . . . . ? C18 C19 C20 N4 0.9(6) . . . . ? C14 C15 C21 C23 -0.8(6) . . . . ? C14 C15 C21 C16 179.1(4) . . . . ? C17 C16 C21 C15 -179.5(4) . . . . ? C17 C16 C21 C23 0.4(6) . . . . ? C19 C18 C22 C24 -0.3(6) . . . . ? C19 C18 C22 C17 179.6(4) . . . . ? C16 C17 C22 C18 -179.8(4) . . . . ? C16 C17 C22 C24 0.1(6) . . . . ? C13 N3 C23 C21 0.9(5) . . . . ? Tb1 N3 C23 C21 -178.4(3) . . . . ? C13 N3 C23 C24 -179.1(3) . . . . ? Tb1 N3 C23 C24 1.6(4) . . . . ? C15 C21 C23 N3 -0.3(6) . . . . ? C16 C21 C23 N3 179.8(4) . . . . ? C15 C21 C23 C24 179.7(4) . . . . ? C16 C21 C23 C24 -0.2(6) . . . . ? C20 N4 C24 C22 0.7(5) . . . . ? Tb1 N4 C24 C22 178.5(3) . . . . ? C20 N4 C24 C23 -179.4(3) . . . . ? Tb1 N4 C24 C23 -1.5(4) . . . . ? C18 C22 C24 N4 0.0(5) . . . . ? C17 C22 C24 N4 -179.9(4) . . . . ? C18 C22 C24 C23 -179.9(3) . . . . ? C17 C22 C24 C23 0.1(5) . . . . ? N3 C23 C24 N4 0.0(5) . . . . ? C21 C23 C24 N4 180.0(3) . . . . ? N3 C23 C24 C22 179.9(3) . . . . ? C21 C23 C24 C22 -0.1(5) . . . . ? O3 S1 C25 C29 5.8(4) . . . . ? O2 S1 C25 C29 128.2(3) . . . . ? O1 S1 C25 C29 -114.3(3) . . . . ? O3 S1 C25 C26 -173.2(3) . . . . ? O2 S1 C25 C26 -50.8(4) . . . . ? O1 S1 C25 C26 66.7(3) . . . . ? C29 C25 C26 C27 178.5(4) . . . . ? S1 C25 C26 C27 -2.6(5) . . . . ? C29 C25 C26 C26 -2.0(6) . . . 2_667 ? S1 C25 C26 C26 176.9(3) . . . 2_667 ? C26 C26 C27 C28 -1.5(7) 2_667 . . . ? C25 C26 C27 C28 178.0(4) . . . . ? C26 C27 C28 C29 2.0(7) . . . 2_667 ? C26 C25 C29 C28 1.7(6) . . . 2_667 ? S1 C25 C29 C28 -177.3(3) . . . 2_667 ? O5 S2 C30 C34 119.0(3) . . . . ? O6 S2 C30 C34 -4.4(4) . . . . ? O4 S2 C30 C34 -122.1(3) . . . . ? O5 S2 C30 C31 -59.2(3) . . . . ? O6 S2 C30 C31 177.3(3) . . . . ? O4 S2 C30 C31 59.7(3) . . . . ? C34 C30 C31 C32 179.7(4) . . . . ? S2 C30 C31 C32 -2.1(5) . . . . ? C34 C30 C31 C31 -0.5(6) . . . 2_766 ? S2 C30 C31 C31 177.7(3) . . . 2_766 ? C30 C31 C32 C33 179.5(4) . . . . ? C31 C31 C32 C33 -0.3(6) 2_766 . . . ? C31 C32 C33 C34 0.5(6) . . . 2_766 ? C31 C30 C34 C33 0.3(6) . . . 2_766 ? S2 C30 C34 C33 -177.9(3) . . . 2_766 ? O9 S3 C35 C39 -8.4(4) . . . . ? O8 S3 C35 C39 -130.2(3) . . . . ? O7 S3 C35 C39 111.0(3) . . . . ? O9 S3 C35 C36 170.4(3) . . . . ? O8 S3 C35 C36 48.5(3) . . . . ? O7 S3 C35 C36 -70.2(3) . . . . ? C39 C35 C36 C37 -179.1(4) . . . . ? S3 C35 C36 C37 2.2(5) . . . . ? C39 C35 C36 C36 1.3(6) . . . 2_666 ? S3 C35 C36 C36 -177.4(3) . . . 2_666 ? C36 C36 C37 C38 1.1(7) 2_666 . . . ? C35 C36 C37 C38 -178.5(4) . . . . ? C36 C37 C38 C39 -1.6(6) . . . 2_666 ? C36 C35 C39 C38 -0.8(6) . . . 2_666 ? S3 C35 C39 C38 178.0(3) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 26.66 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.018 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.096 #================================================================END data_5 _database_code_depnum_ccdc_archive 'CCDC 637259' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H58 Eu2 N8 O20 S4' _chemical_formula_weight 1739.38 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7529(13) _cell_length_b 12.5987(15) _cell_length_c 13.7199(16) _cell_angle_alpha 83.876(2) _cell_angle_beta 68.643(2) _cell_angle_gamma 75.372(2) _cell_volume 1674.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5883 _cell_measurement_theta_min 2.3806 _cell_measurement_theta_max 26.3203 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 1.714 _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 2.063 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 9517 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.38 _reflns_number_total 6737 _reflns_number_gt 5778 _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^)+(0.0665P)^2^+3.4101P] 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 6737 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1167 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.84501(2) 0.607226(18) 0.570109(17) 0.03084(10) Uani 1 1 d . . . S1 S 0.53742(14) 0.82121(13) 0.72675(14) 0.0540(4) Uani 1 1 d . . . S2 S 0.94529(19) 1.21727(13) 0.81517(14) 0.0614(4) Uani 1 1 d . . . O1 O 0.9639(3) 0.4317(3) 0.5765(2) 0.0340(7) Uani 1 1 d . . . O1W O 0.7895(5) 0.7625(3) 0.4571(3) 0.0606(11) Uani 1 1 d . . . O2 O 0.6460(4) 0.7324(4) 0.6780(4) 0.0626(12) Uani 1 1 d . . . O2W O 0.6571(10) 0.8733(8) 1.2523(9) 0.172(4) Uani 1 1 d . . . O3 O 0.4174(6) 0.7887(8) 0.7862(6) 0.163(5) Uani 1 1 d . . . O3W O 0.6521(12) 0.3660(8) 1.0478(10) 0.207(6) Uani 1 1 d . . . O4 O 0.5267(12) 0.9033(5) 0.6478(9) 0.198(6) Uani 1 1 d . . . O5 O 1.0778(7) 1.1587(6) 0.7576(10) 0.183(5) Uani 1 1 d . . . O6 O 0.8888(8) 1.2843(5) 0.7428(4) 0.107(2) Uani 1 1 d . . . O7 O 0.9312(8) 1.2784(5) 0.8996(4) 0.106(2) Uani 1 1 d . . . C1 C 0.6599(6) 0.9591(5) 0.7773(4) 0.0469(13) Uani 1 1 d . . . H1A H 0.6685 0.9893 0.7110 0.056 Uiso 1 1 calc R . . C2 C 0.5950(5) 0.8764(5) 0.8123(5) 0.0458(13) Uani 1 1 d . . . C3 C 0.5782(6) 0.8298(5) 0.9132(5) 0.0553(15) Uani 1 1 d . . . H3A H 0.5332 0.7729 0.9364 0.066 Uiso 1 1 calc R . . C4 C 0.6285(6) 0.8690(5) 0.9762(5) 0.0523(14) Uani 1 1 d . . . H4A H 0.6160 0.8392 1.0432 0.063 Uiso 1 1 calc R . . C5 C 0.7576(7) 0.9937(5) 1.0044(4) 0.0505(14) Uani 1 1 d . . . H5A H 0.7468 0.9650 1.0715 0.061 Uiso 1 1 calc R . . C6 C 0.8290(7) 1.0732(5) 0.9671(4) 0.0504(14) Uani 1 1 d . . . H6A H 0.8671 1.0978 1.0088 0.060 Uiso 1 1 calc R . . C7 C 0.8457(6) 1.1185(4) 0.8663(4) 0.0450(12) Uani 1 1 d . . . C8 C 0.7879(6) 1.0835(4) 0.8057(4) 0.0450(12) Uani 1 1 d . . . H8A H 0.7968 1.1154 0.7398 0.054 Uiso 1 1 calc R . . C9 C 0.6994(6) 0.9541(4) 0.9417(4) 0.0408(11) Uani 1 1 d . . . C10 C 0.7155(5) 1.0005(4) 0.8409(4) 0.0403(11) Uani 1 1 d . . . C11 C 0.5977(6) 0.4815(6) 0.7616(5) 0.0580(15) Uani 1 1 d . . . H11A H 0.6044 0.5306 0.8044 0.070 Uiso 1 1 calc R . . C12 C 0.5280(8) 0.3993(7) 0.8097(7) 0.076(2) Uani 1 1 d . . . H12A H 0.4922 0.3930 0.8822 0.091 Uiso 1 1 calc R . . C13 C 0.5139(8) 0.3299(7) 0.7489(8) 0.081(2) Uani 1 1 d . . . H13A H 0.4697 0.2736 0.7793 0.097 Uiso 1 1 calc R . . C14 C 0.5429(8) 0.2787(6) 0.5694(9) 0.080(3) Uani 1 1 d . . . H14A H 0.4973 0.2225 0.5962 0.097 Uiso 1 1 calc R . . C15 C 0.5859(7) 0.2989(6) 0.4658(9) 0.080(3) Uani 1 1 d . . . H15A H 0.5682 0.2572 0.4225 0.096 Uiso 1 1 calc R . . C16 C 0.7016(7) 0.4080(7) 0.3148(6) 0.071(2) Uani 1 1 d . . . H16A H 0.6842 0.3688 0.2693 0.086 Uiso 1 1 calc R . . C17 C 0.7684(7) 0.4884(7) 0.2767(5) 0.068(2) Uani 1 1 d . . . H17A H 0.7963 0.5059 0.2056 0.081 Uiso 1 1 calc R . . C18 C 0.7957(6) 0.5460(6) 0.3469(5) 0.0553(15) Uani 1 1 d . . . H18A H 0.8435 0.6009 0.3201 0.066 Uiso 1 1 calc R . . C19 C 0.5657(6) 0.3418(5) 0.6395(7) 0.0625(18) Uani 1 1 d . . . C20 C 0.6580(5) 0.3825(5) 0.4207(6) 0.060(2) Uani 1 1 d . . . C21 C 0.6371(5) 0.4261(4) 0.5970(5) 0.0458(13) Uani 1 1 d . . . C22 C 0.6868(5) 0.4457(5) 0.4859(5) 0.0467(14) Uani 1 1 d . . . C23 C 0.8475(6) 0.5425(4) 0.8288(4) 0.0459(12) Uani 1 1 d . . . H23A H 0.8145 0.4850 0.8179 0.055 Uiso 1 1 calc R . . C24 C 0.8540(7) 0.5511(5) 0.9281(5) 0.0547(14) Uani 1 1 d . . . H24A H 0.8245 0.5015 0.9817 0.066 Uiso 1 1 calc R . . C25 C 0.9046(7) 0.6340(5) 0.9435(5) 0.0543(15) Uani 1 1 d . . . H25A H 0.9075 0.6427 1.0091 0.065 Uiso 1 1 calc R . . C26 C 1.0168(7) 0.7887(5) 0.8714(5) 0.0540(15) Uani 1 1 d . . . H26A H 1.0229 0.7985 0.9356 0.065 Uiso 1 1 calc R . . C27 C 1.0683(7) 0.8518(5) 0.7899(5) 0.0550(15) Uani 1 1 d . . . H27A H 1.1114 0.9040 0.7979 0.066 Uiso 1 1 calc R . . C28 C 1.1162(6) 0.9028(5) 0.6028(5) 0.0539(14) Uani 1 1 d . . . H28A H 1.1596 0.9560 0.6081 0.065 Uiso 1 1 calc R . . C29 C 1.1084(7) 0.8850(5) 0.5098(5) 0.0564(15) Uani 1 1 d . . . H29A H 1.1481 0.9247 0.4504 0.068 Uiso 1 1 calc R . . C30 C 1.0403(6) 0.8064(5) 0.5041(4) 0.0502(13) Uani 1 1 d . . . H30A H 1.0360 0.7952 0.4396 0.060 Uiso 1 1 calc R . . C31 C 0.9520(6) 0.7058(4) 0.8619(4) 0.0416(12) Uani 1 1 d . . . C32 C 1.0588(5) 0.8409(4) 0.6904(5) 0.0424(12) Uani 1 1 d . . . C33 C 0.9389(5) 0.6925(4) 0.7652(4) 0.0350(10) Uani 1 1 d . . . C34 C 0.9918(5) 0.7629(4) 0.6781(4) 0.0350(10) Uani 1 1 d . . . N1 N 0.6546(4) 0.4939(4) 0.6593(4) 0.0457(10) Uani 1 1 d . . . N2 N 0.7567(4) 0.5254(4) 0.4481(4) 0.0441(10) Uani 1 1 d . . . N3 N 0.8855(4) 0.6114(3) 0.7503(3) 0.0367(9) Uani 1 1 d . . . N4 N 0.9811(4) 0.7466(3) 0.5858(3) 0.0384(9) Uani 1 1 d . . . H1B H 0.9508 0.3886 0.6275 0.046 Uiso 1 1 d R . . H1WA H 0.8000 0.8077 0.4048 0.046 Uiso 1 1 d R . . H1WB H 0.7159 0.7931 0.5057 0.046 Uiso 1 1 d R . . H3WA H 0.6381 0.3166 1.1001 0.046 Uiso 1 1 d R . . H3WB H 0.7324 0.3329 1.0039 0.046 Uiso 1 1 d 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 Eu1 0.03041(14) 0.03527(15) 0.02984(14) -0.00965(9) -0.01071(10) -0.00883(10) S1 0.0384(7) 0.0526(8) 0.0776(10) -0.0335(7) -0.0275(7) 0.0021(6) S2 0.0688(11) 0.0486(8) 0.0721(11) -0.0038(7) -0.0195(9) -0.0297(8) O1 0.0373(18) 0.0371(17) 0.0273(16) -0.0021(13) -0.0093(14) -0.0101(14) O1W 0.068(3) 0.055(3) 0.063(3) 0.006(2) -0.034(2) -0.006(2) O2 0.046(2) 0.074(3) 0.067(3) -0.040(2) -0.017(2) -0.003(2) O2W 0.132(7) 0.149(8) 0.219(11) 0.052(7) -0.040(7) -0.059(6) O3 0.063(4) 0.295(11) 0.142(6) -0.152(7) 0.022(4) -0.086(5) O3W 0.193(10) 0.122(7) 0.229(12) -0.057(8) 0.040(9) -0.050(7) O4 0.367(14) 0.048(3) 0.327(13) -0.004(5) -0.321(13) -0.007(5) O5 0.070(4) 0.082(5) 0.348(14) -0.013(7) -0.006(6) -0.033(4) O6 0.200(7) 0.104(4) 0.062(3) 0.038(3) -0.064(4) -0.104(5) O7 0.209(7) 0.094(4) 0.069(3) 0.022(3) -0.075(4) -0.102(5) C1 0.046(3) 0.056(3) 0.044(3) -0.015(2) -0.019(2) -0.009(3) C2 0.038(3) 0.049(3) 0.053(3) -0.023(2) -0.015(2) -0.005(2) C3 0.050(3) 0.047(3) 0.071(4) -0.013(3) -0.017(3) -0.017(3) C4 0.057(4) 0.053(3) 0.047(3) 0.000(3) -0.013(3) -0.020(3) C5 0.076(4) 0.049(3) 0.038(3) -0.001(2) -0.027(3) -0.024(3) C6 0.069(4) 0.052(3) 0.047(3) -0.005(2) -0.033(3) -0.021(3) C7 0.057(3) 0.036(3) 0.048(3) -0.005(2) -0.022(3) -0.013(2) C8 0.058(3) 0.044(3) 0.037(3) -0.001(2) -0.020(3) -0.015(3) C9 0.046(3) 0.042(3) 0.036(3) -0.007(2) -0.014(2) -0.011(2) C10 0.043(3) 0.043(3) 0.037(3) -0.010(2) -0.014(2) -0.012(2) C11 0.045(3) 0.073(4) 0.057(4) 0.003(3) -0.018(3) -0.020(3) C12 0.059(4) 0.092(6) 0.076(5) 0.023(4) -0.022(4) -0.032(4) C13 0.054(4) 0.071(5) 0.115(7) 0.024(5) -0.024(4) -0.029(4) C14 0.049(4) 0.056(4) 0.149(9) -0.023(5) -0.038(5) -0.019(3) C15 0.051(4) 0.065(4) 0.142(8) -0.051(5) -0.044(5) -0.010(3) C16 0.049(4) 0.091(5) 0.087(5) -0.049(4) -0.040(4) 0.007(4) C17 0.053(4) 0.099(6) 0.050(4) -0.031(4) -0.027(3) 0.009(4) C18 0.045(3) 0.074(4) 0.049(3) -0.017(3) -0.023(3) -0.001(3) C19 0.036(3) 0.048(3) 0.104(6) -0.009(3) -0.023(3) -0.011(3) C20 0.037(3) 0.060(4) 0.094(6) -0.043(4) -0.035(3) 0.006(3) C21 0.028(2) 0.039(3) 0.072(4) -0.014(3) -0.016(2) -0.008(2) C22 0.029(3) 0.047(3) 0.073(4) -0.026(3) -0.027(3) 0.000(2) C23 0.058(3) 0.042(3) 0.047(3) -0.001(2) -0.023(3) -0.021(3) C24 0.071(4) 0.055(3) 0.047(3) 0.003(3) -0.027(3) -0.021(3) C25 0.074(4) 0.057(3) 0.043(3) -0.004(3) -0.033(3) -0.016(3) C26 0.071(4) 0.058(4) 0.052(3) -0.011(3) -0.036(3) -0.023(3) C27 0.062(4) 0.056(4) 0.064(4) -0.014(3) -0.033(3) -0.023(3) C28 0.056(4) 0.049(3) 0.066(4) -0.006(3) -0.023(3) -0.023(3) C29 0.066(4) 0.059(4) 0.048(3) 0.003(3) -0.015(3) -0.031(3) C30 0.063(4) 0.055(3) 0.036(3) -0.004(2) -0.012(3) -0.024(3) C31 0.048(3) 0.042(3) 0.042(3) -0.012(2) -0.024(2) -0.007(2) C32 0.038(3) 0.041(3) 0.054(3) -0.013(2) -0.020(2) -0.009(2) C33 0.034(2) 0.038(3) 0.039(3) -0.013(2) -0.018(2) -0.006(2) C34 0.030(2) 0.034(2) 0.043(3) -0.011(2) -0.014(2) -0.0030(19) N1 0.035(2) 0.053(3) 0.049(3) -0.009(2) -0.012(2) -0.012(2) N2 0.037(2) 0.056(3) 0.045(3) -0.017(2) -0.017(2) -0.010(2) N3 0.040(2) 0.036(2) 0.040(2) -0.0080(17) -0.0190(19) -0.0091(18) N4 0.042(2) 0.041(2) 0.037(2) -0.0089(18) -0.0144(19) -0.0139(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O1 2.268(3) . ? Eu1 O1 2.280(3) 2_766 ? Eu1 O2 2.397(4) . ? Eu1 O1W 2.455(4) . ? Eu1 N2 2.605(4) . ? Eu1 N4 2.623(4) . ? Eu1 N1 2.647(5) . ? Eu1 N3 2.670(4) . ? Eu1 Eu1 3.7417(5) 2_766 ? Eu1 H1WB 2.6462 . ? S1 O3 1.388(7) . ? S1 O2 1.412(4) . ? S1 O4 1.431(8) . ? S1 C2 1.780(5) . ? S2 O7 1.401(5) . ? S2 O5 1.404(8) . ? S2 O6 1.439(6) . ? S2 C7 1.768(6) . ? O1 Eu1 2.280(3) 2_766 ? O1 H1B 0.8300 . ? O1W H1WA 0.8584 . ? O1W H1WB 0.8577 . ? O3W H3WA 0.8932 . ? O3W H3WB 0.8808 . ? C1 C2 1.348(8) . ? C1 C10 1.423(7) . ? C1 H1A 0.9300 . ? C2 C3 1.411(9) . ? C3 C4 1.359(8) . ? C3 H3A 0.9300 . ? C4 C9 1.413(8) . ? C4 H4A 0.9300 . ? C5 C6 1.358(8) . ? C5 C9 1.422(7) . ? C5 H5A 0.9300 . ? C6 C7 1.406(8) . ? C6 H6A 0.9300 . ? C7 C8 1.365(7) . ? C8 C10 1.402(8) . ? C8 H8A 0.9300 . ? C9 C10 1.410(7) . ? C11 N1 1.321(8) . ? C11 C12 1.398(10) . ? C11 H11A 0.9300 . ? C12 C13 1.341(12) . ? C12 H12A 0.9300 . ? C13 C19 1.403(11) . ? C13 H13A 0.9300 . ? C14 C15 1.343(13) . ? C14 C19 1.433(11) . ? C14 H14A 0.9300 . ? C15 C20 1.420(11) . ? C15 H15A 0.9300 . ? C16 C17 1.340(12) . ? C16 C20 1.384(11) . ? C16 H16A 0.9300 . ? C17 C18 1.414(9) . ? C17 H17A 0.9300 . ? C18 N2 1.314(8) . ? C18 H18A 0.9300 . ? C19 C21 1.418(8) . ? C20 C22 1.417(7) . ? C21 N1 1.360(7) . ? C21 C22 1.436(9) . ? C22 N2 1.352(8) . ? C23 N3 1.319(7) . ? C23 C24 1.406(8) . ? C23 H23A 0.9300 . ? C24 C25 1.360(8) . ? C24 H24A 0.9300 . ? C25 C31 1.390(8) . ? C25 H25A 0.9300 . ? C26 C27 1.331(9) . ? C26 C31 1.434(8) . ? C26 H26A 0.9300 . ? C27 C32 1.429(8) . ? C27 H27A 0.9300 . ? C28 C29 1.354(9) . ? C28 C32 1.391(9) . ? C28 H28A 0.9300 . ? C29 C30 1.396(8) . ? C29 H29A 0.9300 . ? C30 N4 1.331(7) . ? C30 H30A 0.9300 . ? C31 C33 1.416(7) . ? C32 C34 1.413(7) . ? C33 N3 1.357(6) . ? C33 C34 1.440(7) . ? C34 N4 1.352(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Eu1 O1 69.31(13) . 2_766 ? O1 Eu1 O2 138.99(15) . . ? O1 Eu1 O2 151.55(16) 2_766 . ? O1 Eu1 O1W 146.05(13) . . ? O1 Eu1 O1W 80.11(13) 2_766 . ? O2 Eu1 O1W 73.13(17) . . ? O1 Eu1 N2 83.30(13) . . ? O1 Eu1 N2 77.78(13) 2_766 . ? O2 Eu1 N2 104.31(14) . . ? O1W Eu1 N2 75.96(15) . . ? O1 Eu1 N4 110.98(13) . . ? O1 Eu1 N4 79.00(12) 2_766 . ? O2 Eu1 N4 85.21(14) . . ? O1W Eu1 N4 75.90(14) . . ? N2 Eu1 N4 146.04(14) . . ? O1 Eu1 N1 75.23(13) . . ? O1 Eu1 N1 128.97(13) 2_766 . ? O2 Eu1 N1 73.32(15) . . ? O1W Eu1 N1 116.35(15) . . ? N2 Eu1 N1 62.44(15) . . ? N4 Eu1 N1 149.58(14) . . ? O1 Eu1 N3 80.34(12) . . ? O1 Eu1 N3 116.77(12) 2_766 . ? O2 Eu1 N3 74.72(14) . . ? O1W Eu1 N3 128.27(14) . . ? N2 Eu1 N3 151.86(15) . . ? N4 Eu1 N3 61.97(13) . . ? N1 Eu1 N3 91.18(14) . . ? O1 Eu1 Eu1 34.76(8) . 2_766 ? O1 Eu1 Eu1 34.55(8) 2_766 2_766 ? O2 Eu1 Eu1 173.39(12) . 2_766 ? O1W Eu1 Eu1 113.47(11) . 2_766 ? N2 Eu1 Eu1 78.48(10) . 2_766 ? N4 Eu1 Eu1 95.78(9) . 2_766 ? N1 Eu1 Eu1 103.22(10) . 2_766 ? N3 Eu1 Eu1 99.95(9) . 2_766 ? O1 Eu1 H1WB 162.5 . . ? O1 Eu1 H1WB 98.9 2_766 . ? O2 Eu1 H1WB 54.3 . . ? O1W Eu1 H1WB 18.9 . . ? N2 Eu1 H1WB 81.5 . . ? N4 Eu1 H1WB 78.0 . . ? N1 Eu1 H1WB 105.0 . . ? N3 Eu1 H1WB 117.0 . . ? Eu1 Eu1 H1WB 132.3 2_766 . ? O3 S1 O2 112.7(4) . . ? O3 S1 O4 116.0(6) . . ? O2 S1 O4 107.5(5) . . ? O3 S1 C2 108.3(3) . . ? O2 S1 C2 105.0(2) . . ? O4 S1 C2 106.6(3) . . ? O7 S2 O5 117.4(6) . . ? O7 S2 O6 111.5(4) . . ? O5 S2 O6 107.9(6) . . ? O7 S2 C7 107.2(3) . . ? O5 S2 C7 106.1(3) . . ? O6 S2 C7 106.1(3) . . ? Eu1 O1 Eu1 110.69(13) . 2_766 ? Eu1 O1 H1B 127.1 . . ? Eu1 O1 H1B 121.5 2_766 . ? Eu1 O1W H1WA 159.7 . . ? Eu1 O1W H1WB 93.3 . . ? H1WA O1W H1WB 106.2 . . ? S1 O2 Eu1 169.0(3) . . ? H3WA O3W H3WB 101.4 . . ? C2 C1 C10 120.6(5) . . ? C2 C1 H1A 119.7 . . ? C10 C1 H1A 119.7 . . ? C1 C2 C3 121.2(5) . . ? C1 C2 S1 119.0(5) . . ? C3 C2 S1 119.7(4) . . ? C4 C3 C2 119.4(6) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C9 121.2(6) . . ? C3 C4 H4A 119.4 . . ? C9 C4 H4A 119.4 . . ? C6 C5 C9 120.6(5) . . ? C6 C5 H5A 119.7 . . ? C9 C5 H5A 119.7 . . ? C5 C6 C7 120.7(5) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? C8 C7 C6 119.7(5) . . ? C8 C7 S2 119.5(4) . . ? C6 C7 S2 120.8(4) . . ? C7 C8 C10 121.2(5) . . ? C7 C8 H8A 119.4 . . ? C10 C8 H8A 119.4 . . ? C10 C9 C4 119.1(5) . . ? C10 C9 C5 118.5(5) . . ? C4 C9 C5 122.4(5) . . ? C8 C10 C9 119.3(5) . . ? C8 C10 C1 122.2(5) . . ? C9 C10 C1 118.5(5) . . ? N1 C11 C12 124.3(7) . . ? N1 C11 H11A 117.9 . . ? C12 C11 H11A 117.9 . . ? C13 C12 C11 118.5(7) . . ? C13 C12 H12A 120.7 . . ? C11 C12 H12A 120.7 . . ? C12 C13 C19 120.2(7) . . ? C12 C13 H13A 119.9 . . ? C19 C13 H13A 119.9 . . ? C15 C14 C19 121.4(7) . . ? C15 C14 H14A 119.3 . . ? C19 C14 H14A 119.3 . . ? C14 C15 C20 121.5(6) . . ? C14 C15 H15A 119.2 . . ? C20 C15 H15A 119.2 . . ? C17 C16 C20 120.9(6) . . ? C17 C16 H16A 119.5 . . ? C20 C16 H16A 119.5 . . ? C16 C17 C18 118.7(7) . . ? C16 C17 H17A 120.7 . . ? C18 C17 H17A 120.7 . . ? N2 C18 C17 123.0(7) . . ? N2 C18 H18A 118.5 . . ? C17 C18 H18A 118.5 . . ? C13 C19 C21 117.7(7) . . ? C13 C19 C14 123.7(7) . . ? C21 C19 C14 118.4(8) . . ? C16 C20 C22 116.8(7) . . ? C16 C20 C15 123.5(6) . . ? C22 C20 C15 119.6(7) . . ? N1 C21 C19 121.6(6) . . ? N1 C21 C22 118.0(5) . . ? C19 C21 C22 120.3(6) . . ? N2 C22 C20 122.7(6) . . ? N2 C22 C21 118.5(5) . . ? C20 C22 C21 118.7(6) . . ? N3 C23 C24 123.7(5) . . ? N3 C23 H23A 118.2 . . ? C24 C23 H23A 118.2 . . ? C25 C24 C23 118.2(6) . . ? C25 C24 H24A 120.9 . . ? C23 C24 H24A 120.9 . . ? C24 C25 C31 120.4(5) . . ? C24 C25 H25A 119.8 . . ? C31 C25 H25A 119.8 . . ? C27 C26 C31 121.1(5) . . ? C27 C26 H26A 119.4 . . ? C31 C26 H26A 119.4 . . ? C26 C27 C32 121.3(5) . . ? C26 C27 H27A 119.3 . . ? C32 C27 H27A 119.3 . . ? C29 C28 C32 119.5(5) . . ? C29 C28 H28A 120.3 . . ? C32 C28 H28A 120.3 . . ? C28 C29 C30 119.3(6) . . ? C28 C29 H29A 120.3 . . ? C30 C29 H29A 120.3 . . ? N4 C30 C29 123.6(5) . . ? N4 C30 H30A 118.2 . . ? C29 C30 H30A 118.2 . . ? C25 C31 C33 117.6(5) . . ? C25 C31 C26 122.7(5) . . ? C33 C31 C26 119.7(5) . . ? C28 C32 C34 117.7(5) . . ? C28 C32 C27 122.6(5) . . ? C34 C32 C27 119.7(5) . . ? N3 C33 C31 122.1(5) . . ? N3 C33 C34 118.9(4) . . ? C31 C33 C34 118.9(4) . . ? N4 C34 C32 123.0(5) . . ? N4 C34 C33 117.7(4) . . ? C32 C34 C33 119.3(5) . . ? C11 N1 C21 117.5(5) . . ? C11 N1 Eu1 123.7(4) . . ? C21 N1 Eu1 117.1(4) . . ? C18 N2 C22 117.8(5) . . ? C18 N2 Eu1 122.1(4) . . ? C22 N2 Eu1 119.2(4) . . ? C23 N3 C33 118.0(4) . . ? C23 N3 Eu1 123.0(3) . . ? C33 N3 Eu1 118.9(3) . . ? C30 N4 C34 116.8(4) . . ? C30 N4 Eu1 121.6(3) . . ? C34 N4 Eu1 121.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Eu1 O1 Eu1 0.0 2_766 . . 2_766 ? O2 Eu1 O1 Eu1 -176.44(15) . . . 2_766 ? O1W Eu1 O1 Eu1 27.2(3) . . . 2_766 ? N2 Eu1 O1 Eu1 79.43(15) . . . 2_766 ? N4 Eu1 O1 Eu1 -68.71(16) . . . 2_766 ? N1 Eu1 O1 Eu1 142.64(17) . . . 2_766 ? N3 Eu1 O1 Eu1 -123.55(15) . . . 2_766 ? O3 S1 O2 Eu1 150.9(14) . . . . ? O4 S1 O2 Eu1 21.8(15) . . . . ? C2 S1 O2 Eu1 -91.4(14) . . . . ? O1 Eu1 O2 S1 171.2(13) . . . . ? O1 Eu1 O2 S1 -1.8(16) 2_766 . . . ? O1W Eu1 O2 S1 -22.3(14) . . . . ? N2 Eu1 O2 S1 -92.5(14) . . . . ? N4 Eu1 O2 S1 54.4(14) . . . . ? N1 Eu1 O2 S1 -147.4(14) . . . . ? N3 Eu1 O2 S1 116.6(14) . . . . ? Eu1 Eu1 O2 S1 153.3(9) 2_766 . . . ? C10 C1 C2 C3 1.0(8) . . . . ? C10 C1 C2 S1 -175.8(4) . . . . ? O3 S1 C2 C1 -146.8(6) . . . . ? O2 S1 C2 C1 92.5(5) . . . . ? O4 S1 C2 C1 -21.3(7) . . . . ? O3 S1 C2 C3 36.3(7) . . . . ? O2 S1 C2 C3 -84.4(5) . . . . ? O4 S1 C2 C3 161.8(7) . . . . ? C1 C2 C3 C4 -0.1(9) . . . . ? S1 C2 C3 C4 176.8(5) . . . . ? C2 C3 C4 C9 -1.2(9) . . . . ? C9 C5 C6 C7 0.5(10) . . . . ? C5 C6 C7 C8 1.0(9) . . . . ? C5 C6 C7 S2 -177.0(5) . . . . ? O7 S2 C7 C8 149.7(6) . . . . ? O5 S2 C7 C8 -84.1(8) . . . . ? O6 S2 C7 C8 30.5(6) . . . . ? O7 S2 C7 C6 -32.3(6) . . . . ? O5 S2 C7 C6 93.9(8) . . . . ? O6 S2 C7 C6 -151.5(5) . . . . ? C6 C7 C8 C10 -2.0(9) . . . . ? S2 C7 C8 C10 176.0(4) . . . . ? C3 C4 C9 C10 1.4(9) . . . . ? C3 C4 C9 C5 -177.5(6) . . . . ? C6 C5 C9 C10 -1.1(9) . . . . ? C6 C5 C9 C4 177.8(6) . . . . ? C7 C8 C10 C9 1.4(8) . . . . ? C7 C8 C10 C1 -177.0(5) . . . . ? C4 C9 C10 C8 -178.8(5) . . . . ? C5 C9 C10 C8 0.1(8) . . . . ? C4 C9 C10 C1 -0.4(8) . . . . ? C5 C9 C10 C1 178.6(5) . . . . ? C2 C1 C10 C8 177.6(5) . . . . ? C2 C1 C10 C9 -0.8(8) . . . . ? N1 C11 C12 C13 -1.9(11) . . . . ? C11 C12 C13 C19 -1.4(11) . . . . ? C19 C14 C15 C20 1.1(11) . . . . ? C20 C16 C17 C18 1.0(10) . . . . ? C16 C17 C18 N2 -1.1(10) . . . . ? C12 C13 C19 C21 2.5(10) . . . . ? C12 C13 C19 C14 -173.3(7) . . . . ? C15 C14 C19 C13 174.9(7) . . . . ? C15 C14 C19 C21 -0.9(10) . . . . ? C17 C16 C20 C22 0.4(9) . . . . ? C17 C16 C20 C15 179.5(6) . . . . ? C14 C15 C20 C16 -178.5(7) . . . . ? C14 C15 C20 C22 0.7(10) . . . . ? C13 C19 C21 N1 -0.4(9) . . . . ? C14 C19 C21 N1 175.7(6) . . . . ? C13 C19 C21 C22 -177.1(6) . . . . ? C14 C19 C21 C22 -1.0(8) . . . . ? C16 C20 C22 N2 -1.8(8) . . . . ? C15 C20 C22 N2 179.0(5) . . . . ? C16 C20 C22 C21 176.7(5) . . . . ? C15 C20 C22 C21 -2.5(8) . . . . ? N1 C21 C22 N2 4.5(7) . . . . ? C19 C21 C22 N2 -178.7(5) . . . . ? N1 C21 C22 C20 -174.1(5) . . . . ? C19 C21 C22 C20 2.7(8) . . . . ? N3 C23 C24 C25 -1.2(10) . . . . ? C23 C24 C25 C31 -1.9(10) . . . . ? C31 C26 C27 C32 1.2(10) . . . . ? C32 C28 C29 C30 1.4(10) . . . . ? C28 C29 C30 N4 0.1(10) . . . . ? C24 C25 C31 C33 3.2(9) . . . . ? C24 C25 C31 C26 -174.6(6) . . . . ? C27 C26 C31 C25 176.0(6) . . . . ? C27 C26 C31 C33 -1.8(9) . . . . ? C29 C28 C32 C34 -1.3(9) . . . . ? C29 C28 C32 C27 177.2(6) . . . . ? C26 C27 C32 C28 -177.5(6) . . . . ? C26 C27 C32 C34 0.9(9) . . . . ? C25 C31 C33 N3 -1.7(8) . . . . ? C26 C31 C33 N3 176.2(5) . . . . ? C25 C31 C33 C34 -177.7(5) . . . . ? C26 C31 C33 C34 0.2(8) . . . . ? C28 C32 C34 N4 -0.2(8) . . . . ? C27 C32 C34 N4 -178.7(5) . . . . ? C28 C32 C34 C33 176.0(5) . . . . ? C27 C32 C34 C33 -2.5(7) . . . . ? N3 C33 C34 N4 2.2(7) . . . . ? C31 C33 C34 N4 178.4(4) . . . . ? N3 C33 C34 C32 -174.3(4) . . . . ? C31 C33 C34 C32 1.9(7) . . . . ? C12 C11 N1 C21 4.0(9) . . . . ? C12 C11 N1 Eu1 -161.1(5) . . . . ? C19 C21 N1 C11 -2.7(8) . . . . ? C22 C21 N1 C11 174.0(5) . . . . ? C19 C21 N1 Eu1 163.4(4) . . . . ? C22 C21 N1 Eu1 -19.9(6) . . . . ? O1 Eu1 N1 C11 93.4(5) . . . . ? O1 Eu1 N1 C11 140.3(4) 2_766 . . . ? O2 Eu1 N1 C11 -59.9(5) . . . . ? O1W Eu1 N1 C11 -120.8(5) . . . . ? N2 Eu1 N1 C11 -176.5(5) . . . . ? N4 Eu1 N1 C11 -13.0(6) . . . . ? N3 Eu1 N1 C11 13.7(5) . . . . ? Eu1 Eu1 N1 C11 114.2(5) 2_766 . . . ? O1 Eu1 N1 C21 -71.7(4) . . . . ? O1 Eu1 N1 C21 -24.8(5) 2_766 . . . ? O2 Eu1 N1 C21 134.9(4) . . . . ? O1W Eu1 N1 C21 74.0(4) . . . . ? N2 Eu1 N1 C21 18.3(4) . . . . ? N4 Eu1 N1 C21 -178.1(3) . . . . ? N3 Eu1 N1 C21 -151.4(4) . . . . ? Eu1 Eu1 N1 C21 -50.9(4) 2_766 . . . ? C17 C18 N2 C22 -0.3(8) . . . . ? C17 C18 N2 Eu1 168.8(4) . . . . ? C20 C22 N2 C18 1.8(8) . . . . ? C21 C22 N2 C18 -176.8(5) . . . . ? C20 C22 N2 Eu1 -167.7(4) . . . . ? C21 C22 N2 Eu1 13.8(6) . . . . ? O1 Eu1 N2 C18 -108.5(4) . . . . ? O1 Eu1 N2 C18 -38.3(4) 2_766 . . . ? O2 Eu1 N2 C18 112.5(4) . . . . ? O1W Eu1 N2 C18 44.4(4) . . . . ? N4 Eu1 N2 C18 9.5(6) . . . . ? N1 Eu1 N2 C18 174.6(5) . . . . ? N3 Eu1 N2 C18 -163.2(4) . . . . ? Eu1 Eu1 N2 C18 -73.7(4) 2_766 . . . ? O1 Eu1 N2 C22 60.5(4) . . . . ? O1 Eu1 N2 C22 130.7(4) 2_766 . . . ? O2 Eu1 N2 C22 -78.5(4) . . . . ? O1W Eu1 N2 C22 -146.6(4) . . . . ? N4 Eu1 N2 C22 178.5(3) . . . . ? N1 Eu1 N2 C22 -16.3(3) . . . . ? N3 Eu1 N2 C22 5.8(5) . . . . ? Eu1 Eu1 N2 C22 95.3(4) 2_766 . . . ? C24 C23 N3 C33 2.7(8) . . . . ? C24 C23 N3 Eu1 -172.6(5) . . . . ? C31 C33 N3 C23 -1.2(7) . . . . ? C34 C33 N3 C23 174.8(5) . . . . ? C31 C33 N3 Eu1 174.3(4) . . . . ? C34 C33 N3 Eu1 -9.7(6) . . . . ? O1 Eu1 N3 C23 -55.8(4) . . . . ? O1 Eu1 N3 C23 -116.6(4) 2_766 . . . ? O2 Eu1 N3 C23 91.4(4) . . . . ? O1W Eu1 N3 C23 144.6(4) . . . . ? N2 Eu1 N3 C23 -0.5(6) . . . . ? N4 Eu1 N3 C23 -175.9(5) . . . . ? N1 Eu1 N3 C23 19.0(4) . . . . ? Eu1 Eu1 N3 C23 -84.6(4) 2_766 . . . ? O1 Eu1 N3 C33 129.0(4) . . . . ? O1 Eu1 N3 C33 68.2(4) 2_766 . . . ? O2 Eu1 N3 C33 -83.9(4) . . . . ? O1W Eu1 N3 C33 -30.6(4) . . . . ? N2 Eu1 N3 C33 -175.7(3) . . . . ? N4 Eu1 N3 C33 8.9(3) . . . . ? N1 Eu1 N3 C33 -156.2(4) . . . . ? Eu1 Eu1 N3 C33 100.1(3) 2_766 . . . ? C29 C30 N4 C34 -1.5(9) . . . . ? C29 C30 N4 Eu1 177.0(5) . . . . ? C32 C34 N4 C30 1.6(7) . . . . ? C33 C34 N4 C30 -174.7(5) . . . . ? C32 C34 N4 Eu1 -177.0(4) . . . . ? C33 C34 N4 Eu1 6.7(6) . . . . ? O1 Eu1 N4 C30 107.6(4) . . . . ? O1 Eu1 N4 C30 45.0(4) 2_766 . . . ? O2 Eu1 N4 C30 -111.2(4) . . . . ? O1W Eu1 N4 C30 -37.4(4) . . . . ? N2 Eu1 N4 C30 -2.6(6) . . . . ? N1 Eu1 N4 C30 -155.9(4) . . . . ? N3 Eu1 N4 C30 173.6(5) . . . . ? Eu1 Eu1 N4 C30 75.3(4) 2_766 . . . ? O1 Eu1 N4 C34 -73.9(4) . . . . ? O1 Eu1 N4 C34 -136.5(4) 2_766 . . . ? O2 Eu1 N4 C34 67.3(4) . . . . ? O1W Eu1 N4 C34 141.0(4) . . . . ? N2 Eu1 N4 C34 175.9(3) . . . . ? N1 Eu1 N4 C34 22.6(5) . . . . ? N3 Eu1 N4 C34 -8.0(3) . . . . ? Eu1 Eu1 N4 C34 -106.2(4) 2_766 . . . ? 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 O1 H1B O6 0.83 1.98 2.796(6) 169.2 1_545 O1W H1WA O5 0.86 2.20 2.955(12) 147.3 2_776 O1W H1WB O2 0.86 2.31 2.891(7) 124.9 . O3W H3WA O3 0.89 1.96 2.845(16) 172.2 2_667 O3W H3WB O7 0.88 2.08 2.953(13) 170.7 1_545 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.796 _refine_diff_density_min -1.038 _refine_diff_density_rms 0.138 #============================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 637260' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H58 Gd2 N8 O20 S4' _chemical_formula_weight 1749.96 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6498(13) _cell_length_b 12.6501(16) _cell_length_c 13.682(2) _cell_angle_alpha 84.050(3) _cell_angle_beta 68.256(2) _cell_angle_gamma 75.975(2) _cell_volume 1660.9(4) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5118 _cell_measurement_theta_min 0.0000 _cell_measurement_theta_max 0.0000 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 1.742 _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 2.189 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 9406 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.43 _reflns_number_total 6712 _reflns_number_gt 5545 _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^)+(0.0634P)^2^+3.2312P] 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 6712 _refine_ls_number_parameters 464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1054 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.019 _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 0.84455(3) 0.605307(19) 0.571166(18) 0.03121(10) Uani 1 1 d . . . S1 S 0.53779(16) 0.81889(13) 0.72581(14) 0.0535(4) Uani 1 1 d . . . S2 S 0.9478(2) 1.21740(14) 0.81329(15) 0.0648(5) Uani 1 1 d . . . O1W O 0.7873(5) 0.7575(3) 0.4595(3) 0.0556(11) Uani 1 1 d . . . O1 O 0.9635(4) 0.4318(3) 0.5763(3) 0.0341(8) Uani 1 1 d . . . O2 O 0.6454(4) 0.7290(4) 0.6805(4) 0.0608(12) Uani 1 1 d . . . O2W O 1.3442(12) 1.1186(10) 0.7448(12) 0.234(6) Uani 1 1 d . . . O3 O 0.4143(6) 0.7906(8) 0.7850(6) 0.158(4) Uani 1 1 d . . . O3W O 0.3485(12) 0.6361(9) 0.9524(10) 0.221(6) Uani 1 1 d . . . O4 O 0.5377(12) 0.8989(5) 0.6400(8) 0.186(6) Uani 1 1 d . . . O5 O 1.0798(8) 1.1608(6) 0.7528(9) 0.178(5) Uani 1 1 d . . . O6 O 0.8874(9) 1.2852(5) 0.7429(4) 0.115(3) Uani 1 1 d . . . O7 O 0.9352(8) 1.2784(5) 0.8976(4) 0.095(2) Uani 1 1 d . . . C1 C 0.7929(7) 0.5423(6) 0.3494(5) 0.0545(16) Uani 1 1 d . . . H1A H 0.8406 0.5976 0.3216 0.065 Uiso 1 1 calc R . . C2 C 0.7653(7) 0.4844(7) 0.2806(6) 0.064(2) Uani 1 1 d . . . H2A H 0.7931 0.5017 0.2091 0.077 Uiso 1 1 calc R . . C3 C 0.6984(7) 0.4038(7) 0.3189(6) 0.068(2) Uani 1 1 d . . . H3B H 0.6804 0.3644 0.2738 0.081 Uiso 1 1 calc R . . C4 C 0.5839(8) 0.2952(6) 0.4707(9) 0.080(3) Uani 1 1 d . . . H4B H 0.5665 0.2528 0.4275 0.096 Uiso 1 1 calc R . . C5 C 0.5399(8) 0.2756(6) 0.5762(9) 0.078(3) Uani 1 1 d . . . H5A H 0.4942 0.2192 0.6039 0.094 Uiso 1 1 calc R . . C6 C 0.5082(8) 0.3315(7) 0.7555(8) 0.081(2) Uani 1 1 d . . . H6A H 0.4618 0.2762 0.7870 0.097 Uiso 1 1 calc R . . C7 C 0.5219(8) 0.4012(7) 0.8157(6) 0.072(2) Uani 1 1 d . . . H7B H 0.4859 0.3951 0.8887 0.086 Uiso 1 1 calc R . . C8 C 0.5919(6) 0.4840(6) 0.7664(5) 0.0545(15) Uani 1 1 d . . . H8A H 0.5966 0.5350 0.8085 0.065 Uiso 1 1 calc R . . C9 C 0.6557(6) 0.3788(5) 0.4255(6) 0.0561(18) Uani 1 1 d . . . C10 C 0.5624(7) 0.3404(5) 0.6459(6) 0.0588(17) Uani 1 1 d . . . C11 C 0.6843(6) 0.4432(5) 0.4902(5) 0.0450(14) Uani 1 1 d . . . C12 C 0.6343(5) 0.4247(5) 0.6024(5) 0.0445(13) Uani 1 1 d . . . C13 C 0.8474(6) 0.5397(5) 0.8285(4) 0.0458(13) Uani 1 1 d . . . H13A H 0.8144 0.4821 0.8174 0.055 Uiso 1 1 calc R . . C14 C 0.8542(7) 0.5480(5) 0.9280(5) 0.0540(15) Uani 1 1 d . . . H14A H 0.8246 0.4978 0.9814 0.065 Uiso 1 1 calc R . . C15 C 0.9044(7) 0.6301(5) 0.9448(5) 0.0534(15) Uani 1 1 d . . . H15A H 0.9082 0.6379 1.0105 0.064 Uiso 1 1 calc R . . C16 C 1.0157(7) 0.7865(5) 0.8726(5) 0.0542(16) Uani 1 1 d . . . H16A H 1.0222 0.7958 0.9370 0.065 Uiso 1 1 calc R . . C17 C 1.0673(7) 0.8514(5) 0.7909(5) 0.0542(16) Uani 1 1 d . . . H17A H 1.1106 0.9038 0.7990 0.065 Uiso 1 1 calc R . . C18 C 1.1144(7) 0.9034(5) 0.6044(5) 0.0524(15) Uani 1 1 d . . . H18A H 1.1569 0.9574 0.6101 0.063 Uiso 1 1 calc R . . C19 C 1.1079(7) 0.8850(5) 0.5105(5) 0.0541(15) Uani 1 1 d . . . H19A H 1.1482 0.9249 0.4508 0.065 Uiso 1 1 calc R . . C20 C 1.0400(7) 0.8053(5) 0.5046(5) 0.0487(14) Uani 1 1 d . . . H20A H 1.0361 0.7938 0.4398 0.058 Uiso 1 1 calc R . . C21 C 0.9504(6) 0.7031(5) 0.8632(4) 0.0426(13) Uani 1 1 d . . . C22 C 1.0565(6) 0.8405(4) 0.6924(5) 0.0414(12) Uani 1 1 d . . . C23 C 0.9378(5) 0.6902(4) 0.7662(4) 0.0347(11) Uani 1 1 d . . . C24 C 0.9904(5) 0.7610(4) 0.6794(4) 0.0358(11) Uani 1 1 d . . . C25 C 0.6596(6) 0.9576(5) 0.7773(5) 0.0477(14) Uani 1 1 d . . . H25A H 0.6683 0.9872 0.7106 0.057 Uiso 1 1 calc R . . C26 C 0.5947(6) 0.8752(5) 0.8123(5) 0.0459(14) Uani 1 1 d . . . C27 C 0.5775(7) 0.8301(5) 0.9127(5) 0.0543(15) Uani 1 1 d . . . H27A H 0.5316 0.7733 0.9363 0.065 Uiso 1 1 calc R . . C28 C 0.6278(7) 0.8691(5) 0.9758(5) 0.0511(15) Uani 1 1 d . . . H28A H 0.6150 0.8393 1.0429 0.061 Uiso 1 1 calc R . . C29 C 0.7579(7) 0.9945(5) 1.0041(5) 0.0524(15) Uani 1 1 d . . . H29A H 0.7462 0.9660 1.0716 0.063 Uiso 1 1 calc R . . C30 C 0.8303(7) 1.0734(5) 0.9668(5) 0.0510(15) Uani 1 1 d . . . H30A H 0.8690 1.0983 1.0084 0.061 Uiso 1 1 calc R . . C31 C 0.8473(7) 1.1181(4) 0.8649(4) 0.0447(13) Uani 1 1 d . . . C32 C 0.7889(7) 1.0831(5) 0.8046(4) 0.0460(14) Uani 1 1 d . . . H32A H 0.7981 1.1146 0.7385 0.055 Uiso 1 1 calc R . . C33 C 0.7157(6) 1.0008(5) 0.8405(4) 0.0408(12) Uani 1 1 d . . . C34 C 0.6994(6) 0.9544(5) 0.9412(4) 0.0427(13) Uani 1 1 d . . . N1 N 0.7547(5) 0.5223(4) 0.4517(3) 0.0402(10) Uani 1 1 d . . . N2 N 0.6513(5) 0.4933(4) 0.6636(4) 0.0438(11) Uani 1 1 d . . . N3 N 0.8851(5) 0.6087(3) 0.7504(3) 0.0362(9) Uani 1 1 d . . . N4 N 0.9806(5) 0.7451(3) 0.5866(3) 0.0376(10) Uani 1 1 d . . . H3WA H 0.3627 0.6866 0.9007 0.045 Uiso 1 1 d R . . H3WB H 0.2690 0.6700 0.9985 0.045 Uiso 1 1 d R . . H1WA H 0.7226 0.8113 0.4915 0.045 Uiso 1 1 d R . . H1WB H 0.8272 0.7814 0.3970 0.045 Uiso 1 1 d R . . H1B H 0.943(6) 0.387(5) 0.624(5) 0.045(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.03299(15) 0.03303(15) 0.03019(14) -0.01067(9) -0.01193(10) -0.00671(10) S1 0.0432(8) 0.0482(9) 0.0771(11) -0.0330(8) -0.0314(8) 0.0045(7) S2 0.0802(13) 0.0477(9) 0.0673(11) -0.0060(8) -0.0156(10) -0.0310(9) O1W 0.058(3) 0.047(2) 0.061(3) -0.002(2) -0.027(2) 0.000(2) O1 0.0373(19) 0.0338(19) 0.0277(17) -0.0044(15) -0.0076(15) -0.0067(16) O2 0.047(2) 0.070(3) 0.064(3) -0.039(2) -0.017(2) 0.000(2) O2W 0.152(10) 0.206(12) 0.309(16) 0.113(11) -0.065(10) -0.054(9) O3 0.062(4) 0.280(11) 0.138(6) -0.152(7) 0.016(4) -0.071(5) O3W 0.193(11) 0.142(9) 0.234(12) -0.067(8) 0.055(9) -0.053(8) O4 0.358(14) 0.049(3) 0.294(12) 0.007(5) -0.298(12) -0.021(6) O5 0.089(5) 0.081(5) 0.299(12) -0.011(6) 0.021(7) -0.042(4) O6 0.225(8) 0.103(5) 0.067(3) 0.042(3) -0.073(5) -0.111(5) O7 0.182(7) 0.082(4) 0.066(3) 0.016(3) -0.069(4) -0.082(4) C1 0.049(4) 0.072(4) 0.045(3) -0.016(3) -0.027(3) 0.005(3) C2 0.054(4) 0.089(5) 0.052(4) -0.031(4) -0.032(3) 0.011(4) C3 0.047(4) 0.084(5) 0.084(5) -0.051(4) -0.041(4) 0.014(4) C4 0.048(4) 0.068(5) 0.137(8) -0.054(5) -0.038(5) -0.005(4) C5 0.051(4) 0.051(4) 0.143(8) -0.020(5) -0.037(5) -0.018(3) C6 0.059(5) 0.065(5) 0.119(7) 0.021(5) -0.029(5) -0.028(4) C7 0.061(4) 0.093(6) 0.066(4) 0.018(4) -0.023(4) -0.029(4) C8 0.047(3) 0.064(4) 0.054(4) 0.003(3) -0.018(3) -0.016(3) C9 0.037(3) 0.055(4) 0.085(5) -0.038(4) -0.032(3) 0.005(3) C10 0.038(3) 0.049(4) 0.090(5) -0.009(3) -0.020(3) -0.010(3) C11 0.032(3) 0.043(3) 0.067(4) -0.024(3) -0.027(3) 0.004(2) C12 0.028(3) 0.038(3) 0.069(4) -0.016(3) -0.016(3) -0.005(2) C13 0.058(4) 0.039(3) 0.048(3) -0.001(3) -0.026(3) -0.015(3) C14 0.072(4) 0.052(4) 0.043(3) 0.003(3) -0.027(3) -0.015(3) C15 0.070(4) 0.054(4) 0.045(3) -0.006(3) -0.031(3) -0.010(3) C16 0.074(4) 0.055(4) 0.053(4) -0.012(3) -0.038(3) -0.020(3) C17 0.061(4) 0.055(4) 0.063(4) -0.016(3) -0.033(3) -0.020(3) C18 0.053(4) 0.046(3) 0.066(4) -0.010(3) -0.024(3) -0.018(3) C19 0.066(4) 0.053(4) 0.047(3) 0.002(3) -0.016(3) -0.025(3) C20 0.060(4) 0.051(3) 0.040(3) -0.006(3) -0.018(3) -0.018(3) C21 0.052(3) 0.044(3) 0.038(3) -0.011(2) -0.023(3) -0.005(3) C22 0.039(3) 0.038(3) 0.052(3) -0.013(2) -0.020(3) -0.005(2) C23 0.035(3) 0.033(3) 0.040(3) -0.012(2) -0.019(2) -0.001(2) C24 0.034(3) 0.031(3) 0.045(3) -0.014(2) -0.019(2) 0.001(2) C25 0.052(3) 0.052(3) 0.045(3) -0.014(3) -0.023(3) -0.008(3) C26 0.038(3) 0.047(3) 0.057(3) -0.023(3) -0.020(3) -0.003(3) C27 0.052(4) 0.041(3) 0.070(4) -0.008(3) -0.020(3) -0.013(3) C28 0.058(4) 0.052(4) 0.046(3) -0.001(3) -0.017(3) -0.021(3) C29 0.079(5) 0.051(4) 0.039(3) 0.000(3) -0.031(3) -0.021(3) C30 0.074(4) 0.053(4) 0.043(3) -0.005(3) -0.033(3) -0.021(3) C31 0.060(4) 0.034(3) 0.045(3) -0.004(2) -0.022(3) -0.012(3) C32 0.064(4) 0.043(3) 0.035(3) -0.002(2) -0.021(3) -0.014(3) C33 0.045(3) 0.040(3) 0.039(3) -0.011(2) -0.015(2) -0.007(2) C34 0.051(3) 0.042(3) 0.038(3) -0.008(2) -0.017(3) -0.009(3) N1 0.036(2) 0.049(3) 0.041(2) -0.014(2) -0.017(2) -0.007(2) N2 0.036(2) 0.046(3) 0.050(3) -0.008(2) -0.014(2) -0.010(2) N3 0.041(2) 0.035(2) 0.038(2) -0.0071(19) -0.019(2) -0.0093(19) N4 0.042(2) 0.036(2) 0.038(2) -0.0088(19) -0.016(2) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.261(4) . ? Gd1 O1 2.268(3) 2_766 ? Gd1 O2 2.390(4) . ? Gd1 O1W 2.435(4) . ? Gd1 N1 2.587(4) . ? Gd1 N4 2.612(4) . ? Gd1 N2 2.637(5) . ? Gd1 N3 2.649(4) . ? Gd1 Gd1 3.7251(6) 2_766 ? S1 O3 1.376(7) . ? S1 O2 1.407(4) . ? S1 O4 1.469(8) . ? S1 C26 1.786(5) . ? S2 O5 1.395(8) . ? S2 O7 1.401(5) . ? S2 O6 1.448(7) . ? S2 C31 1.769(6) . ? O1W H1WA 0.8600 . ? O1W H1WB 0.8608 . ? O1 Gd1 2.268(3) 2_766 ? O1 H1B 0.82(6) . ? O3W H3WA 0.8971 . ? O3W H3WB 0.8848 . ? C1 N1 1.320(8) . ? C1 C2 1.401(9) . ? C1 H1A 0.9300 . ? C2 C3 1.336(11) . ? C2 H2A 0.9300 . ? C3 C9 1.384(10) . ? C3 H3B 0.9300 . ? C4 C5 1.358(13) . ? C4 C9 1.412(11) . ? C4 H4B 0.9300 . ? C5 C10 1.437(11) . ? C5 H5A 0.9300 . ? C6 C7 1.335(11) . ? C6 C10 1.397(11) . ? C6 H6A 0.9300 . ? C7 C8 1.402(10) . ? C7 H7B 0.9300 . ? C8 N2 1.317(8) . ? C8 H8A 0.9300 . ? C9 C11 1.417(7) . ? C10 C12 1.416(9) . ? C11 N1 1.342(8) . ? C11 C12 1.441(9) . ? C12 N2 1.352(7) . ? C13 N3 1.313(7) . ? C13 C14 1.405(8) . ? C13 H13A 0.9300 . ? C14 C15 1.353(9) . ? C14 H14A 0.9300 . ? C15 C21 1.393(9) . ? C15 H15A 0.9300 . ? C16 C17 1.341(9) . ? C16 C21 1.436(8) . ? C16 H16A 0.9300 . ? C17 C22 1.419(8) . ? C17 H17A 0.9300 . ? C18 C19 1.358(9) . ? C18 C22 1.397(9) . ? C18 H18A 0.9300 . ? C19 C20 1.400(8) . ? C19 H19A 0.9300 . ? C20 N4 1.330(7) . ? C20 H20A 0.9300 . ? C21 C23 1.412(7) . ? C22 C24 1.417(7) . ? C23 N3 1.356(6) . ? C23 C24 1.433(8) . ? C24 N4 1.350(6) . ? C25 C26 1.339(9) . ? C25 C33 1.429(7) . ? C25 H25A 0.9300 . ? C26 C27 1.396(9) . ? C27 C28 1.354(9) . ? C27 H27A 0.9300 . ? C28 C34 1.412(8) . ? C28 H28A 0.9300 . ? C29 C30 1.352(9) . ? C29 C34 1.423(8) . ? C29 H29A 0.9300 . ? C30 C31 1.414(8) . ? C30 H30A 0.9300 . ? C31 C32 1.361(8) . ? C32 C33 1.392(8) . ? C32 H32A 0.9300 . ? C33 C34 1.408(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Gd1 O1 69.35(16) . 2_766 ? O1 Gd1 O2 139.18(15) . . ? O1 Gd1 O2 151.28(16) 2_766 . ? O1 Gd1 O1W 145.96(14) . . ? O1 Gd1 O1W 80.35(14) 2_766 . ? O2 Gd1 O1W 72.88(16) . . ? O1 Gd1 N1 82.75(14) . . ? O1 Gd1 N1 78.21(13) 2_766 . ? O2 Gd1 N1 104.60(14) . . ? O1W Gd1 N1 76.03(15) . . ? O1 Gd1 N4 111.44(13) . . ? O1 Gd1 N4 79.15(13) 2_766 . ? O2 Gd1 N4 84.51(14) . . ? O1W Gd1 N4 76.30(14) . . ? N1 Gd1 N4 146.66(14) . . ? O1 Gd1 N2 75.50(14) . . ? O1 Gd1 N2 129.84(14) 2_766 . ? O2 Gd1 N2 73.03(15) . . ? O1W Gd1 N2 115.86(15) . . ? N1 Gd1 N2 62.59(15) . . ? N4 Gd1 N2 148.63(14) . . ? O1 Gd1 N3 80.28(13) . . ? O1 Gd1 N3 116.75(13) 2_766 . ? O2 Gd1 N3 74.62(14) . . ? O1W Gd1 N3 128.89(14) . . ? N1 Gd1 N3 150.98(15) . . ? N4 Gd1 N3 62.23(13) . . ? N2 Gd1 N3 90.33(14) . . ? O1 Gd1 Gd1 34.74(9) . 2_766 ? O1 Gd1 Gd1 34.62(9) 2_766 2_766 ? O2 Gd1 Gd1 173.44(12) . 2_766 ? O1W Gd1 Gd1 113.64(10) . 2_766 ? N1 Gd1 Gd1 78.40(10) . 2_766 ? N4 Gd1 Gd1 96.16(10) . 2_766 ? N2 Gd1 Gd1 103.77(10) . 2_766 ? N3 Gd1 Gd1 99.88(10) . 2_766 ? O3 S1 O2 113.3(4) . . ? O3 S1 O4 117.5(6) . . ? O2 S1 O4 106.0(5) . . ? O3 S1 C26 107.8(3) . . ? O2 S1 C26 104.7(3) . . ? O4 S1 C26 106.6(3) . . ? O5 S2 O7 118.1(6) . . ? O5 S2 O6 108.0(6) . . ? O7 S2 O6 110.6(4) . . ? O5 S2 C31 106.0(4) . . ? O7 S2 C31 107.8(3) . . ? O6 S2 C31 105.7(3) . . ? Gd1 O1W H1WA 115.7 . . ? Gd1 O1W H1WB 136.3 . . ? H1WA O1W H1WB 105.8 . . ? Gd1 O1 Gd1 110.65(16) . 2_766 ? Gd1 O1 H1B 126(4) . . ? Gd1 O1 H1B 123(4) 2_766 . ? S1 O2 Gd1 166.8(3) . . ? H3WA O3W H3WB 100.8 . . ? N1 C1 C2 123.2(7) . . ? N1 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C3 C2 C1 119.2(7) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C9 120.3(6) . . ? C2 C3 H3B 119.8 . . ? C9 C3 H3B 119.8 . . ? C5 C4 C9 121.0(7) . . ? C5 C4 H4B 119.5 . . ? C9 C4 H4B 119.5 . . ? C4 C5 C10 121.3(7) . . ? C4 C5 H5A 119.3 . . ? C10 C5 H5A 119.3 . . ? C7 C6 C10 120.9(7) . . ? C7 C6 H6A 119.6 . . ? C10 C6 H6A 119.6 . . ? C6 C7 C8 118.5(7) . . ? C6 C7 H7B 120.8 . . ? C8 C7 H7B 120.8 . . ? N2 C8 C7 123.5(7) . . ? N2 C8 H8A 118.2 . . ? C7 C8 H8A 118.2 . . ? C3 C9 C4 122.9(6) . . ? C3 C9 C11 117.0(7) . . ? C4 C9 C11 120.1(7) . . ? C6 C10 C12 117.0(6) . . ? C6 C10 C5 124.1(7) . . ? C12 C10 C5 118.7(7) . . ? N1 C11 C9 122.8(6) . . ? N1 C11 C12 118.2(5) . . ? C9 C11 C12 119.0(6) . . ? N2 C12 C10 121.9(6) . . ? N2 C12 C11 118.2(5) . . ? C10 C12 C11 119.8(6) . . ? N3 C13 C14 123.7(5) . . ? N3 C13 H13A 118.1 . . ? C14 C13 H13A 118.1 . . ? C15 C14 C13 118.8(6) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? C14 C15 C21 119.6(5) . . ? C14 C15 H15A 120.2 . . ? C21 C15 H15A 120.2 . . ? C17 C16 C21 121.6(5) . . ? C17 C16 H16A 119.2 . . ? C21 C16 H16A 119.2 . . ? C16 C17 C22 120.4(5) . . ? C16 C17 H17A 119.8 . . ? C22 C17 H17A 119.8 . . ? C19 C18 C22 119.4(5) . . ? C19 C18 H18A 120.3 . . ? C22 C18 H18A 120.3 . . ? C18 C19 C20 119.2(6) . . ? C18 C19 H19A 120.4 . . ? C20 C19 H19A 120.4 . . ? N4 C20 C19 123.6(5) . . ? N4 C20 H20A 118.2 . . ? C19 C20 H20A 118.2 . . ? C15 C21 C23 118.0(5) . . ? C15 C21 C16 122.5(5) . . ? C23 C21 C16 119.4(5) . . ? C18 C22 C24 117.8(5) . . ? C18 C22 C17 121.9(5) . . ? C24 C22 C17 120.2(6) . . ? N3 C23 C21 122.1(5) . . ? N3 C23 C24 118.7(4) . . ? C21 C23 C24 119.0(5) . . ? N4 C24 C22 122.7(5) . . ? N4 C24 C23 118.0(4) . . ? C22 C24 C23 119.3(5) . . ? C26 C25 C33 121.2(6) . . ? C26 C25 H25A 119.4 . . ? C33 C25 H25A 119.4 . . ? C25 C26 C27 120.9(5) . . ? C25 C26 S1 118.8(5) . . ? C27 C26 S1 120.2(5) . . ? C28 C27 C26 120.0(6) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C27 C28 C34 121.0(6) . . ? C27 C28 H28A 119.5 . . ? C34 C28 H28A 119.5 . . ? C30 C29 C34 120.7(5) . . ? C30 C29 H29A 119.6 . . ? C34 C29 H29A 119.6 . . ? C29 C30 C31 120.1(5) . . ? C29 C30 H30A 119.9 . . ? C31 C30 H30A 119.9 . . ? C32 C31 C30 120.1(5) . . ? C32 C31 S2 119.4(4) . . ? C30 C31 S2 120.5(4) . . ? C31 C32 C33 120.9(5) . . ? C31 C32 H32A 119.5 . . ? C33 C32 H32A 119.5 . . ? C32 C33 C34 119.7(5) . . ? C32 C33 C25 122.6(5) . . ? C34 C33 C25 117.7(5) . . ? C33 C34 C28 119.2(5) . . ? C33 C34 C29 118.4(5) . . ? C28 C34 C29 122.4(5) . . ? C1 N1 C11 117.4(5) . . ? C1 N1 Gd1 122.4(4) . . ? C11 N1 Gd1 119.4(4) . . ? C8 N2 C12 118.0(5) . . ? C8 N2 Gd1 123.9(4) . . ? C12 N2 Gd1 116.7(4) . . ? C13 N3 C23 117.7(4) . . ? C13 N3 Gd1 123.2(3) . . ? C23 N3 Gd1 118.9(3) . . ? C20 N4 C24 117.4(5) . . ? C20 N4 Gd1 121.6(3) . . ? C24 N4 Gd1 121.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Gd1 O1 Gd1 0.0 2_766 . . 2_766 ? O2 Gd1 O1 Gd1 -175.95(15) . . . 2_766 ? O1W Gd1 O1 Gd1 28.6(3) . . . 2_766 ? N1 Gd1 O1 Gd1 80.09(16) . . . 2_766 ? N4 Gd1 O1 Gd1 -68.65(17) . . . 2_766 ? N2 Gd1 O1 Gd1 143.58(18) . . . 2_766 ? N3 Gd1 O1 Gd1 -123.54(17) . . . 2_766 ? O3 S1 O2 Gd1 145.7(12) . . . . ? O4 S1 O2 Gd1 15.4(13) . . . . ? C26 S1 O2 Gd1 -97.1(12) . . . . ? O1 Gd1 O2 S1 176.0(11) . . . . ? O1 Gd1 O2 S1 3.9(14) 2_766 . . . ? O1W Gd1 O2 S1 -18.1(12) . . . . ? N1 Gd1 O2 S1 -88.2(12) . . . . ? N4 Gd1 O2 S1 59.2(12) . . . . ? N2 Gd1 O2 S1 -143.0(12) . . . . ? N3 Gd1 O2 S1 121.9(12) . . . . ? Gd1 Gd1 O2 S1 155.3(7) 2_766 . . . ? N1 C1 C2 C3 -0.8(10) . . . . ? C1 C2 C3 C9 0.7(10) . . . . ? C9 C4 C5 C10 1.1(12) . . . . ? C10 C6 C7 C8 0.1(12) . . . . ? C6 C7 C8 N2 -3.7(11) . . . . ? C2 C3 C9 C4 179.6(6) . . . . ? C2 C3 C9 C11 1.0(9) . . . . ? C5 C4 C9 C3 -177.8(7) . . . . ? C5 C4 C9 C11 0.7(10) . . . . ? C7 C6 C10 C12 1.2(11) . . . . ? C7 C6 C10 C5 -173.4(8) . . . . ? C4 C5 C10 C6 173.5(8) . . . . ? C4 C5 C10 C12 -1.1(11) . . . . ? C3 C9 C11 N1 -2.9(8) . . . . ? C4 C9 C11 N1 178.5(6) . . . . ? C3 C9 C11 C12 176.2(5) . . . . ? C4 C9 C11 C12 -2.4(8) . . . . ? C6 C10 C12 N2 0.6(9) . . . . ? C5 C10 C12 N2 175.6(6) . . . . ? C6 C10 C12 C11 -175.6(6) . . . . ? C5 C10 C12 C11 -0.7(9) . . . . ? N1 C11 C12 N2 5.1(8) . . . . ? C9 C11 C12 N2 -174.0(5) . . . . ? N1 C11 C12 C10 -178.5(5) . . . . ? C9 C11 C12 C10 2.4(8) . . . . ? N3 C13 C14 C15 -1.2(10) . . . . ? C13 C14 C15 C21 -1.2(10) . . . . ? C21 C16 C17 C22 1.2(11) . . . . ? C22 C18 C19 C20 1.7(10) . . . . ? C18 C19 C20 N4 -0.2(11) . . . . ? C14 C15 C21 C23 2.3(9) . . . . ? C14 C15 C21 C16 -174.6(6) . . . . ? C17 C16 C21 C15 175.6(7) . . . . ? C17 C16 C21 C23 -1.2(10) . . . . ? C19 C18 C22 C24 -1.3(9) . . . . ? C19 C18 C22 C17 176.1(6) . . . . ? C16 C17 C22 C18 -177.2(6) . . . . ? C16 C17 C22 C24 0.2(10) . . . . ? C15 C21 C23 N3 -1.2(8) . . . . ? C16 C21 C23 N3 175.8(5) . . . . ? C15 C21 C23 C24 -177.1(5) . . . . ? C16 C21 C23 C24 -0.1(8) . . . . ? C18 C22 C24 N4 -0.6(8) . . . . ? C17 C22 C24 N4 -178.1(5) . . . . ? C18 C22 C24 C23 176.0(5) . . . . ? C17 C22 C24 C23 -1.5(8) . . . . ? N3 C23 C24 N4 2.2(7) . . . . ? C21 C23 C24 N4 178.2(5) . . . . ? N3 C23 C24 C22 -174.6(5) . . . . ? C21 C23 C24 C22 1.4(7) . . . . ? C33 C25 C26 C27 1.2(9) . . . . ? C33 C25 C26 S1 -175.7(4) . . . . ? O3 S1 C26 C25 -144.1(7) . . . . ? O2 S1 C26 C25 95.0(5) . . . . ? O4 S1 C26 C25 -17.1(7) . . . . ? O3 S1 C26 C27 39.0(7) . . . . ? O2 S1 C26 C27 -81.9(6) . . . . ? O4 S1 C26 C27 166.1(7) . . . . ? C25 C26 C27 C28 -0.5(10) . . . . ? S1 C26 C27 C28 176.3(5) . . . . ? C26 C27 C28 C34 -0.8(10) . . . . ? C34 C29 C30 C31 0.8(10) . . . . ? C29 C30 C31 C32 1.1(10) . . . . ? C29 C30 C31 S2 -177.4(5) . . . . ? O5 S2 C31 C32 -82.7(8) . . . . ? O7 S2 C31 C32 150.0(6) . . . . ? O6 S2 C31 C32 31.7(6) . . . . ? O5 S2 C31 C30 95.7(8) . . . . ? O7 S2 C31 C30 -31.6(7) . . . . ? O6 S2 C31 C30 -149.8(6) . . . . ? C30 C31 C32 C33 -2.1(10) . . . . ? S2 C31 C32 C33 176.4(5) . . . . ? C31 C32 C33 C34 1.2(9) . . . . ? C31 C32 C33 C25 -176.4(6) . . . . ? C26 C25 C33 C32 177.1(6) . . . . ? C26 C25 C33 C34 -0.5(9) . . . . ? C32 C33 C34 C28 -178.5(6) . . . . ? C25 C33 C34 C28 -0.8(9) . . . . ? C32 C33 C34 C29 0.7(9) . . . . ? C25 C33 C34 C29 178.4(6) . . . . ? C27 C28 C34 C33 1.4(9) . . . . ? C27 C28 C34 C29 -177.7(6) . . . . ? C30 C29 C34 C33 -1.7(10) . . . . ? C30 C29 C34 C28 177.5(6) . . . . ? C2 C1 N1 C11 -0.9(9) . . . . ? C2 C1 N1 Gd1 168.6(5) . . . . ? C9 C11 N1 C1 2.8(8) . . . . ? C12 C11 N1 C1 -176.2(5) . . . . ? C9 C11 N1 Gd1 -167.1(4) . . . . ? C12 C11 N1 Gd1 13.9(6) . . . . ? O1 Gd1 N1 C1 -108.8(5) . . . . ? O1 Gd1 N1 C1 -38.4(4) 2_766 . . . ? O2 Gd1 N1 C1 112.2(5) . . . . ? O1W Gd1 N1 C1 44.4(4) . . . . ? N4 Gd1 N1 C1 9.7(6) . . . . ? N2 Gd1 N1 C1 173.9(5) . . . . ? N3 Gd1 N1 C1 -163.3(4) . . . . ? Gd1 Gd1 N1 C1 -73.8(4) 2_766 . . . ? O1 Gd1 N1 C11 60.6(4) . . . . ? O1 Gd1 N1 C11 130.9(4) 2_766 . . . ? O2 Gd1 N1 C11 -78.4(4) . . . . ? O1W Gd1 N1 C11 -146.2(4) . . . . ? N4 Gd1 N1 C11 179.1(3) . . . . ? N2 Gd1 N1 C11 -16.8(4) . . . . ? N3 Gd1 N1 C11 6.1(6) . . . . ? Gd1 Gd1 N1 C11 95.6(4) 2_766 . . . ? C7 C8 N2 C12 5.5(9) . . . . ? C7 C8 N2 Gd1 -160.3(5) . . . . ? C10 C12 N2 C8 -3.9(8) . . . . ? C11 C12 N2 C8 172.5(5) . . . . ? C10 C12 N2 Gd1 163.0(4) . . . . ? C11 C12 N2 Gd1 -20.7(6) . . . . ? O1 Gd1 N2 C8 95.7(5) . . . . ? O1 Gd1 N2 C8 142.0(5) 2_766 . . . ? O2 Gd1 N2 C8 -58.0(5) . . . . ? O1W Gd1 N2 C8 -118.7(5) . . . . ? N1 Gd1 N2 C8 -175.1(5) . . . . ? N4 Gd1 N2 C8 -11.9(6) . . . . ? N3 Gd1 N2 C8 15.8(5) . . . . ? Gd1 Gd1 N2 C8 116.0(5) 2_766 . . . ? O1 Gd1 N2 C12 -70.3(4) . . . . ? O1 Gd1 N2 C12 -24.0(5) 2_766 . . . ? O2 Gd1 N2 C12 136.0(4) . . . . ? O1W Gd1 N2 C12 75.3(4) . . . . ? N1 Gd1 N2 C12 18.9(4) . . . . ? N4 Gd1 N2 C12 -177.8(3) . . . . ? N3 Gd1 N2 C12 -150.2(4) . . . . ? Gd1 Gd1 N2 C12 -49.9(4) 2_766 . . . ? C14 C13 N3 C23 2.3(9) . . . . ? C14 C13 N3 Gd1 -172.6(5) . . . . ? C21 C23 N3 C13 -1.1(8) . . . . ? C24 C23 N3 C13 174.8(5) . . . . ? C21 C23 N3 Gd1 174.1(4) . . . . ? C24 C23 N3 Gd1 -10.0(6) . . . . ? O1 Gd1 N3 C13 -55.3(4) . . . . ? O1 Gd1 N3 C13 -116.1(4) 2_766 . . . ? O2 Gd1 N3 C13 92.2(5) . . . . ? O1W Gd1 N3 C13 144.3(4) . . . . ? N1 Gd1 N3 C13 -0.2(6) . . . . ? N4 Gd1 N3 C13 -175.9(5) . . . . ? N2 Gd1 N3 C13 19.9(5) . . . . ? Gd1 Gd1 N3 C13 -84.1(4) 2_766 . . . ? O1 Gd1 N3 C23 129.9(4) . . . . ? O1 Gd1 N3 C23 69.0(4) 2_766 . . . ? O2 Gd1 N3 C23 -82.6(4) . . . . ? O1W Gd1 N3 C23 -30.5(4) . . . . ? N1 Gd1 N3 C23 -175.1(3) . . . . ? N4 Gd1 N3 C23 9.2(3) . . . . ? N2 Gd1 N3 C23 -154.9(4) . . . . ? Gd1 Gd1 N3 C23 101.0(4) 2_766 . . . ? C19 C20 N4 C24 -1.7(9) . . . . ? C19 C20 N4 Gd1 176.7(5) . . . . ? C22 C24 N4 C20 2.1(8) . . . . ? C23 C24 N4 C20 -174.6(5) . . . . ? C22 C24 N4 Gd1 -176.3(4) . . . . ? C23 C24 N4 Gd1 7.1(6) . . . . ? O1 Gd1 N4 C20 107.7(4) . . . . ? O1 Gd1 N4 C20 45.2(4) 2_766 . . . ? O2 Gd1 N4 C20 -111.1(5) . . . . ? O1W Gd1 N4 C20 -37.4(4) . . . . ? N1 Gd1 N4 C20 -2.8(6) . . . . ? N2 Gd1 N4 C20 -155.0(4) . . . . ? N3 Gd1 N4 C20 173.4(5) . . . . ? Gd1 Gd1 N4 C20 75.4(4) 2_766 . . . ? O1 Gd1 N4 C24 -74.0(4) . . . . ? O1 Gd1 N4 C24 -136.6(4) 2_766 . . . ? O2 Gd1 N4 C24 67.2(4) . . . . ? O1W Gd1 N4 C24 140.9(4) . . . . ? N1 Gd1 N4 C24 175.5(3) . . . . ? N2 Gd1 N4 C24 23.3(5) . . . . ? N3 Gd1 N4 C24 -8.3(4) . . . . ? Gd1 Gd1 N4 C24 -106.3(4) 2_766 . . . ? 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 O3W H3WA O3 0.90 1.95 2.846(16) 174.0 . O3W H3WB O7 0.88 2.10 2.965(12) 167.4 2_677 O1W H1WA O4 0.86 2.38 3.180(12) 154.3 . O1W H1WB O5 0.86 2.06 2.923(11) 179.2 2_776 O1 H1B O6 0.82(6) 1.97(6) 2.789(6) 177(6) 1_545 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.468 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.120 #============================================================================== data_7 _database_code_depnum_ccdc_archive 'CCDC 637262' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H58 N8 O20 S4 Tb2' _chemical_formula_weight 1753.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.685(3) _cell_length_b 12.699(4) _cell_length_c 13.698(4) _cell_angle_alpha 84.405(4) _cell_angle_beta 68.237(4) _cell_angle_gamma 75.866(4) _cell_volume 1673.9(8) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 4812 _cell_measurement_theta_min 2.2930 _cell_measurement_theta_max 26.3994 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 1.731 _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 2.303 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 9523 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 26.44 _reflns_number_total 6758 _reflns_number_gt 5507 _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^)+(0.0680P)^2^+2.0924P] 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 6758 _refine_ls_number_parameters 460 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1223 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.068 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.84549(3) 0.60487(2) 0.571176(18) 0.03082(10) Uani 1 1 d . . . S1 S 0.53974(16) 0.81789(14) 0.72622(14) 0.0510(4) Uani 1 1 d . . . S2 S 0.9482(2) 1.21751(15) 0.81077(15) 0.0623(5) Uani 1 1 d . . . O1W O 0.7875(5) 0.7559(4) 0.4616(4) 0.0534(11) Uani 1 1 d . . . O1 O 1.0363(4) 0.5671(3) 0.4249(3) 0.0335(8) Uani 1 1 d . . . H1B H 1.0402 0.6228 0.3849 0.040 Uiso 1 1 d R . . O2 O 0.6483(5) 0.7277(4) 0.6806(4) 0.0591(13) Uani 1 1 d . . . O2W O 1.3474(10) 1.1250(9) 0.7525(10) 0.176(4) Uani 1 1 d . . . O3 O 0.4171(6) 0.7888(8) 0.7858(6) 0.153(4) Uani 1 1 d . . . O3W O 0.3434(10) 0.6372(8) 0.9564(9) 0.198(6) Uani 1 1 d D . . O4 O 0.5380(12) 0.8974(5) 0.6417(9) 0.177(5) Uani 1 1 d . . . O5 O 1.0787(8) 1.1606(6) 0.7464(8) 0.140(3) Uani 1 1 d . . . O6 O 0.8850(9) 1.2867(5) 0.7411(5) 0.108(3) Uani 1 1 d . . . O7 O 0.9383(8) 1.2775(5) 0.8953(4) 0.089(2) Uani 1 1 d . . . C1 C 0.5939(7) 0.4835(6) 0.7654(6) 0.0573(17) Uani 1 1 d . . . H1A H 0.5999 0.5332 0.8082 0.069 Uiso 1 1 calc R . . C2 C 0.5234(8) 0.4040(8) 0.8139(7) 0.074(2) Uani 1 1 d . . . H2A H 0.4858 0.3998 0.8868 0.089 Uiso 1 1 calc R . . C3 C 0.5097(8) 0.3330(7) 0.7548(8) 0.075(2) Uani 1 1 d . . . H3A H 0.4650 0.2775 0.7864 0.091 Uiso 1 1 calc R . . C4 C 0.5420(8) 0.2772(7) 0.5751(10) 0.079(3) Uani 1 1 d . . . H4A H 0.4985 0.2200 0.6021 0.095 Uiso 1 1 calc R . . C5 C 0.5846(8) 0.2974(7) 0.4705(10) 0.084(3) Uani 1 1 d . . . H5A H 0.5664 0.2556 0.4275 0.100 Uiso 1 1 calc R . . C6 C 0.6998(8) 0.4064(7) 0.3178(7) 0.067(2) Uani 1 1 d . . . H6A H 0.6821 0.3675 0.2722 0.080 Uiso 1 1 calc R . . C7 C 0.7673(8) 0.4869(7) 0.2800(6) 0.064(2) Uani 1 1 d . . . H7A H 0.7948 0.5045 0.2088 0.077 Uiso 1 1 calc R . . C8 C 0.7955(7) 0.5438(6) 0.3488(5) 0.0533(17) Uani 1 1 d . . . H8A H 0.8437 0.5983 0.3216 0.064 Uiso 1 1 calc R . . C9 C 0.5629(7) 0.3423(6) 0.6451(7) 0.061(2) Uani 1 1 d . . . C10 C 0.6565(6) 0.3809(6) 0.4246(6) 0.058(2) Uani 1 1 d . . . C11 C 0.6359(6) 0.4260(5) 0.6021(5) 0.0460(15) Uani 1 1 d . . . C12 C 0.6861(6) 0.4444(5) 0.4894(5) 0.0454(15) Uani 1 1 d . . . C13 C 1.0380(7) 0.8043(5) 0.5057(5) 0.0484(15) Uani 1 1 d . . . H13A H 1.0345 0.7928 0.4408 0.058 Uiso 1 1 calc R . . C14 C 1.1054(7) 0.8845(6) 0.5127(5) 0.0545(17) Uani 1 1 d . . . H14A H 1.1445 0.9248 0.4536 0.065 Uiso 1 1 calc R . . C15 C 1.1128(7) 0.9022(5) 0.6055(5) 0.0503(16) Uani 1 1 d . . . H15A H 1.1557 0.9556 0.6113 0.060 Uiso 1 1 calc R . . C16 C 1.0668(7) 0.8502(6) 0.7914(6) 0.0544(17) Uani 1 1 d . . . H16A H 1.1098 0.9025 0.7996 0.065 Uiso 1 1 calc R . . C17 C 1.0161(7) 0.7857(6) 0.8725(5) 0.0525(17) Uani 1 1 d . . . H17A H 1.0234 0.7948 0.9366 0.063 Uiso 1 1 calc R . . C18 C 0.9033(7) 0.6301(6) 0.9446(5) 0.0524(16) Uani 1 1 d . . . H18A H 0.9053 0.6386 1.0107 0.063 Uiso 1 1 calc R . . C19 C 0.8549(7) 0.5480(6) 0.9271(5) 0.0538(16) Uani 1 1 d . . . H19A H 0.8266 0.4977 0.9799 0.065 Uiso 1 1 calc R . . C20 C 0.8479(7) 0.5396(5) 0.8278(5) 0.0457(14) Uani 1 1 d . . . H20A H 0.8150 0.4823 0.8165 0.055 Uiso 1 1 calc R . . C21 C 1.0554(6) 0.8396(5) 0.6932(5) 0.0422(14) Uani 1 1 d . . . C22 C 0.9506(6) 0.7024(5) 0.8629(5) 0.0432(14) Uani 1 1 d . . . C23 C 0.9900(6) 0.7603(5) 0.6803(4) 0.0354(12) Uani 1 1 d . . . C24 C 0.9379(6) 0.6892(5) 0.7664(4) 0.0349(12) Uani 1 1 d . . . C25 C 0.6605(7) 0.9575(5) 0.7767(5) 0.0469(15) Uani 1 1 d . . . H25A H 0.6683 0.9868 0.7103 0.056 Uiso 1 1 calc R . . C26 C 0.5964(6) 0.8751(5) 0.8121(5) 0.0466(15) Uani 1 1 d . . . C27 C 0.5790(7) 0.8304(5) 0.9131(6) 0.0522(16) Uani 1 1 d . . . H27A H 0.5337 0.7738 0.9368 0.063 Uiso 1 1 calc R . . C28 C 0.6288(7) 0.8705(6) 0.9758(5) 0.0504(15) Uani 1 1 d . . . H28A H 0.6158 0.8420 1.0431 0.061 Uiso 1 1 calc R . . C29 C 0.7592(7) 0.9967(5) 1.0016(5) 0.0494(16) Uani 1 1 d . . . H29A H 0.7475 0.9690 1.0690 0.059 Uiso 1 1 calc R . . C30 C 0.8314(7) 1.0749(5) 0.9641(5) 0.0510(16) Uani 1 1 d . . . H30A H 0.8703 1.0995 1.0055 0.061 Uiso 1 1 calc R . . C31 C 0.8481(7) 1.1189(5) 0.8640(5) 0.0457(14) Uani 1 1 d . . . C32 C 0.7896(7) 1.0837(5) 0.8029(5) 0.0461(15) Uani 1 1 d . . . H32A H 0.7984 1.1149 0.7371 0.055 Uiso 1 1 calc R . . C33 C 0.7014(6) 0.9563(5) 0.9395(5) 0.0421(13) Uani 1 1 d . . . C34 C 0.7166(6) 1.0006(5) 0.8393(4) 0.0418(13) Uani 1 1 d . . . N1 N 0.6531(5) 0.4943(4) 0.6637(4) 0.0431(11) Uani 1 1 d . . . N2 N 0.7566(5) 0.5236(4) 0.4509(4) 0.0406(11) Uani 1 1 d . . . N3 N 0.9792(5) 0.7443(4) 0.5872(4) 0.0374(10) Uani 1 1 d . . . N4 N 0.8850(4) 0.6079(4) 0.7503(3) 0.0348(10) Uani 1 1 d . . . H2WA H 1.2699 1.1340 0.7406 0.042 Uiso 1 1 d R . . H2WB H 1.3923 1.0589 0.7239 0.042 Uiso 1 1 d R . . H3WA H 0.3613 0.6863 0.9045 0.042 Uiso 1 1 d RD . . H3WB H 0.2663 0.6704 1.0015 0.042 Uiso 1 1 d RD . . H1WA H 0.7219 0.8093 0.4938 0.042 Uiso 1 1 d R . . H1WB H 0.8285 0.7804 0.4000 0.042 Uiso 1 1 d 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 Tb1 0.03399(16) 0.03260(15) 0.02947(15) -0.00907(10) -0.01422(11) -0.00607(10) S1 0.0416(8) 0.0480(9) 0.0695(11) -0.0287(8) -0.0287(8) 0.0036(7) S2 0.0775(13) 0.0491(10) 0.0625(11) -0.0059(8) -0.0169(10) -0.0292(10) O1W 0.054(3) 0.046(3) 0.056(3) 0.000(2) -0.025(2) 0.003(2) O1 0.040(2) 0.0303(19) 0.0289(18) -0.0012(15) -0.0116(16) -0.0066(16) O2 0.052(3) 0.070(3) 0.055(3) -0.033(2) -0.018(2) -0.003(2) O2W 0.131(8) 0.158(9) 0.252(12) 0.066(8) -0.088(8) -0.050(7) O3 0.063(4) 0.268(11) 0.133(6) -0.138(7) 0.018(4) -0.078(6) O3W 0.162(9) 0.110(7) 0.230(12) -0.045(7) 0.042(8) -0.026(7) O4 0.329(13) 0.049(4) 0.285(12) -0.002(5) -0.282(12) -0.008(6) O5 0.087(5) 0.083(5) 0.216(9) -0.005(5) -0.002(6) -0.038(4) O6 0.211(8) 0.097(5) 0.064(4) 0.039(3) -0.073(5) -0.099(5) O7 0.169(6) 0.077(4) 0.063(3) 0.016(3) -0.065(4) -0.074(4) C1 0.047(4) 0.069(5) 0.057(4) 0.002(3) -0.017(3) -0.017(3) C2 0.060(5) 0.090(6) 0.068(5) 0.020(5) -0.017(4) -0.026(5) C3 0.061(5) 0.063(5) 0.101(7) 0.020(5) -0.025(5) -0.026(4) C4 0.053(5) 0.051(5) 0.140(9) -0.024(5) -0.033(5) -0.017(4) C5 0.055(5) 0.065(5) 0.149(9) -0.053(6) -0.047(5) -0.010(4) C6 0.053(4) 0.076(5) 0.083(6) -0.044(4) -0.045(4) 0.011(4) C7 0.054(4) 0.091(6) 0.050(4) -0.032(4) -0.031(3) 0.011(4) C8 0.051(4) 0.067(4) 0.047(4) -0.014(3) -0.027(3) -0.002(3) C9 0.044(4) 0.044(4) 0.100(6) -0.003(4) -0.027(4) -0.012(3) C10 0.038(3) 0.060(5) 0.084(6) -0.036(4) -0.032(4) 0.006(3) C11 0.033(3) 0.038(3) 0.071(4) -0.013(3) -0.021(3) -0.007(3) C12 0.032(3) 0.044(3) 0.066(4) -0.027(3) -0.027(3) 0.004(3) C13 0.061(4) 0.053(4) 0.038(3) -0.002(3) -0.020(3) -0.021(3) C14 0.062(4) 0.056(4) 0.050(4) 0.006(3) -0.019(3) -0.025(3) C15 0.056(4) 0.044(4) 0.062(4) -0.008(3) -0.025(3) -0.022(3) C16 0.066(4) 0.055(4) 0.063(4) -0.015(3) -0.038(4) -0.021(3) C17 0.070(4) 0.055(4) 0.051(4) -0.011(3) -0.038(3) -0.017(3) C18 0.070(4) 0.056(4) 0.042(3) -0.007(3) -0.035(3) -0.009(3) C19 0.072(5) 0.054(4) 0.042(3) 0.003(3) -0.027(3) -0.017(3) C20 0.058(4) 0.042(3) 0.048(3) 0.000(3) -0.030(3) -0.013(3) C21 0.044(3) 0.039(3) 0.050(4) -0.013(3) -0.024(3) -0.005(3) C22 0.051(4) 0.045(3) 0.041(3) -0.012(3) -0.027(3) -0.003(3) C23 0.036(3) 0.036(3) 0.039(3) -0.008(2) -0.019(2) -0.003(2) C24 0.036(3) 0.037(3) 0.038(3) -0.012(2) -0.022(2) -0.001(2) C25 0.051(4) 0.051(4) 0.043(3) -0.014(3) -0.023(3) -0.006(3) C26 0.043(3) 0.045(4) 0.053(4) -0.022(3) -0.020(3) 0.001(3) C27 0.052(4) 0.045(4) 0.064(4) -0.013(3) -0.019(3) -0.014(3) C28 0.060(4) 0.052(4) 0.044(4) 0.003(3) -0.019(3) -0.021(3) C29 0.073(5) 0.048(4) 0.039(3) 0.002(3) -0.029(3) -0.022(3) C30 0.076(5) 0.049(4) 0.044(3) -0.003(3) -0.035(3) -0.020(3) C31 0.061(4) 0.037(3) 0.043(3) -0.004(3) -0.020(3) -0.015(3) C32 0.066(4) 0.043(3) 0.035(3) -0.002(3) -0.024(3) -0.014(3) C33 0.050(4) 0.040(3) 0.038(3) -0.004(2) -0.018(3) -0.009(3) C34 0.051(4) 0.041(3) 0.036(3) -0.009(2) -0.018(3) -0.009(3) N1 0.037(3) 0.046(3) 0.048(3) -0.008(2) -0.015(2) -0.009(2) N2 0.040(3) 0.045(3) 0.043(3) -0.014(2) -0.021(2) -0.005(2) N3 0.043(3) 0.038(3) 0.036(3) -0.007(2) -0.019(2) -0.010(2) N4 0.040(3) 0.033(2) 0.037(2) -0.0048(19) -0.020(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O1 2.247(4) 2_766 ? Tb1 O1 2.255(3) . ? Tb1 O2 2.372(4) . ? Tb1 O1W 2.422(4) . ? Tb1 N2 2.579(4) . ? Tb1 N3 2.602(4) . ? Tb1 N1 2.633(5) . ? Tb1 N4 2.644(4) . ? Tb1 Tb1 3.7070(8) 2_766 ? S1 O3 1.380(6) . ? S1 O2 1.414(5) . ? S1 O4 1.462(9) . ? S1 C26 1.784(6) . ? S2 O5 1.401(8) . ? S2 O7 1.405(5) . ? S2 O6 1.471(7) . ? S2 C31 1.773(6) . ? O1W H1WA 0.8615 . ? O1W H1WB 0.8604 . ? O1 Tb1 2.247(4) 2_766 ? O1 H1B 0.8499 . ? O2W H2WA 0.8804 . ? O2W H2WB 0.9034 . ? O3W H3WA 0.8951 . ? O3W H3WB 0.8623 . ? C1 N1 1.308(8) . ? C1 C2 1.377(10) . ? C1 H1A 0.9300 . ? C2 C3 1.336(12) . ? C2 H2A 0.9300 . ? C3 C9 1.400(12) . ? C3 H3A 0.9300 . ? C4 C5 1.352(14) . ? C4 C9 1.434(12) . ? C4 H4A 0.9300 . ? C5 C10 1.421(12) . ? C5 H5A 0.9300 . ? C6 C7 1.346(12) . ? C6 C10 1.391(11) . ? C6 H6A 0.9300 . ? C7 C8 1.397(9) . ? C7 H7A 0.9300 . ? C8 N2 1.321(8) . ? C8 H8A 0.9300 . ? C9 C11 1.424(9) . ? C10 C12 1.418(8) . ? C11 N1 1.354(7) . ? C11 C12 1.451(9) . ? C12 N2 1.352(8) . ? C13 N3 1.330(8) . ? C13 C14 1.413(9) . ? C13 H13A 0.9300 . ? C14 C15 1.346(9) . ? C14 H14A 0.9300 . ? C15 C21 1.399(9) . ? C15 H15A 0.9300 . ? C16 C17 1.338(10) . ? C16 C21 1.417(9) . ? C16 H16A 0.9300 . ? C17 C22 1.444(9) . ? C17 H17A 0.9300 . ? C18 C19 1.347(9) . ? C18 C22 1.399(9) . ? C18 H18A 0.9300 . ? C19 C20 1.406(8) . ? C19 H19A 0.9300 . ? C20 N4 1.309(7) . ? C20 H20A 0.9300 . ? C21 C23 1.416(8) . ? C22 C24 1.408(7) . ? C23 N3 1.361(7) . ? C23 C24 1.438(8) . ? C24 N4 1.363(7) . ? C25 C26 1.343(9) . ? C25 C34 1.425(8) . ? C25 H25A 0.9300 . ? C26 C27 1.407(9) . ? C27 C28 1.354(9) . ? C27 H27A 0.9300 . ? C28 C33 1.434(9) . ? C28 H28A 0.9300 . ? C29 C30 1.351(9) . ? C29 C33 1.412(8) . ? C29 H29A 0.9300 . ? C30 C31 1.394(8) . ? C30 H30A 0.9300 . ? C31 C32 1.374(8) . ? C32 C34 1.408(9) . ? C32 H32A 0.9300 . ? C33 C34 1.398(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O1 69.14(15) 2_766 . ? O1 Tb1 O2 139.18(16) 2_766 . ? O1 Tb1 O2 151.47(17) . . ? O1 Tb1 O1W 146.11(14) 2_766 . ? O1 Tb1 O1W 80.78(14) . . ? O2 Tb1 O1W 72.72(17) . . ? O1 Tb1 N2 82.97(14) 2_766 . ? O1 Tb1 N2 78.15(14) . . ? O2 Tb1 N2 104.68(15) . . ? O1W Tb1 N2 75.69(16) . . ? O1 Tb1 N3 111.84(14) 2_766 . ? O1 Tb1 N3 79.30(14) . . ? O2 Tb1 N3 84.14(15) . . ? O1W Tb1 N3 76.03(15) . . ? N2 Tb1 N3 146.15(16) . . ? O1 Tb1 N1 75.53(14) 2_766 . ? O1 Tb1 N1 130.02(14) . . ? O2 Tb1 N1 72.92(16) . . ? O1W Tb1 N1 115.82(16) . . ? N2 Tb1 N1 63.18(16) . . ? N3 Tb1 N1 148.33(15) . . ? O1 Tb1 N4 80.29(13) 2_766 . ? O1 Tb1 N4 116.76(13) . . ? O2 Tb1 N4 74.42(15) . . ? O1W Tb1 N4 128.93(14) . . ? N2 Tb1 N4 151.13(16) . . ? N3 Tb1 N4 62.63(14) . . ? N1 Tb1 N4 89.83(15) . . ? O1 Tb1 Tb1 34.64(9) 2_766 2_766 ? O1 Tb1 Tb1 34.50(9) . 2_766 ? O2 Tb1 Tb1 173.28(13) . 2_766 ? O1W Tb1 Tb1 113.94(11) . 2_766 ? N2 Tb1 Tb1 78.51(11) . 2_766 ? N3 Tb1 Tb1 96.47(11) . 2_766 ? N1 Tb1 Tb1 103.87(11) . 2_766 ? N4 Tb1 Tb1 99.88(9) . 2_766 ? O3 S1 O2 112.9(5) . . ? O3 S1 O4 117.6(6) . . ? O2 S1 O4 106.5(5) . . ? O3 S1 C26 108.0(3) . . ? O2 S1 C26 104.6(3) . . ? O4 S1 C26 106.2(3) . . ? O5 S2 O7 119.0(5) . . ? O5 S2 O6 106.9(5) . . ? O7 S2 O6 110.9(4) . . ? O5 S2 C31 106.0(4) . . ? O7 S2 C31 107.2(3) . . ? O6 S2 C31 106.1(3) . . ? Tb1 O1W H1WA 115.9 . . ? Tb1 O1W H1WB 135.8 . . ? H1WA O1W H1WB 105.7 . . ? Tb1 O1 Tb1 110.86(15) 2_766 . ? Tb1 O1 H1B 139.9 2_766 . ? Tb1 O1 H1B 109.3 . . ? S1 O2 Tb1 166.7(4) . . ? H2WA O2W H2WB 100.6 . . ? H3WA O3W H3WB 102.7 . . ? N1 C1 C2 124.9(7) . . ? N1 C1 H1A 117.6 . . ? C2 C1 H1A 117.6 . . ? C3 C2 C1 119.2(8) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C9 119.9(7) . . ? C2 C3 H3A 120.1 . . ? C9 C3 H3A 120.1 . . ? C5 C4 C9 121.1(8) . . ? C5 C4 H4A 119.4 . . ? C9 C4 H4A 119.5 . . ? C4 C5 C10 121.8(7) . . ? C4 C5 H5A 119.1 . . ? C10 C5 H5A 119.1 . . ? C7 C6 C10 120.6(6) . . ? C7 C6 H6A 119.7 . . ? C10 C6 H6A 119.7 . . ? C6 C7 C8 119.3(7) . . ? C6 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? N2 C8 C7 122.9(7) . . ? N2 C8 H8A 118.6 . . ? C7 C8 H8A 118.6 . . ? C3 C9 C11 116.9(7) . . ? C3 C9 C4 124.2(8) . . ? C11 C9 C4 118.8(8) . . ? C6 C10 C12 116.5(7) . . ? C6 C10 C5 123.9(7) . . ? C12 C10 C5 119.5(8) . . ? N1 C11 C9 122.1(7) . . ? N1 C11 C12 118.1(5) . . ? C9 C11 C12 119.7(6) . . ? N2 C12 C10 122.8(6) . . ? N2 C12 C11 118.2(5) . . ? C10 C12 C11 118.9(6) . . ? N3 C13 C14 123.3(6) . . ? N3 C13 H13A 118.3 . . ? C14 C13 H13A 118.3 . . ? C15 C14 C13 119.6(6) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C14 C15 C21 119.4(6) . . ? C14 C15 H15A 120.3 . . ? C21 C15 H15A 120.3 . . ? C17 C16 C21 120.5(6) . . ? C17 C16 H16A 119.7 . . ? C21 C16 H16A 119.7 . . ? C16 C17 C22 121.7(6) . . ? C16 C17 H17A 119.2 . . ? C22 C17 H17A 119.2 . . ? C19 C18 C22 119.6(6) . . ? C19 C18 H18A 120.2 . . ? C22 C18 H18A 120.2 . . ? C18 C19 C20 118.9(6) . . ? C18 C19 H19A 120.5 . . ? C20 C19 H19A 120.5 . . ? N4 C20 C19 123.8(6) . . ? N4 C20 H20A 118.1 . . ? C19 C20 H20A 118.1 . . ? C15 C21 C16 122.0(6) . . ? C15 C21 C23 117.9(5) . . ? C16 C21 C23 120.0(6) . . ? C18 C22 C24 117.7(6) . . ? C18 C22 C17 122.9(5) . . ? C24 C22 C17 119.3(6) . . ? N3 C23 C21 122.7(5) . . ? N3 C23 C24 117.5(5) . . ? C21 C23 C24 119.8(5) . . ? N4 C24 C22 122.2(5) . . ? N4 C24 C23 119.0(5) . . ? C22 C24 C23 118.7(5) . . ? C26 C25 C34 120.9(6) . . ? C26 C25 H25A 119.5 . . ? C34 C25 H25A 119.5 . . ? C25 C26 C27 121.3(6) . . ? C25 C26 S1 118.8(5) . . ? C27 C26 S1 119.9(5) . . ? C28 C27 C26 119.5(6) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C27 C28 C33 120.8(6) . . ? C27 C28 H28A 119.6 . . ? C33 C28 H28A 119.6 . . ? C30 C29 C33 120.8(6) . . ? C30 C29 H29A 119.6 . . ? C33 C29 H29A 119.6 . . ? C29 C30 C31 120.6(6) . . ? C29 C30 H30A 119.7 . . ? C31 C30 H30A 119.7 . . ? C32 C31 C30 120.0(6) . . ? C32 C31 S2 118.4(5) . . ? C30 C31 S2 121.5(5) . . ? C31 C32 C34 120.4(6) . . ? C31 C32 H32A 119.8 . . ? C34 C32 H32A 119.8 . . ? C34 C33 C29 119.0(6) . . ? C34 C33 C28 119.0(5) . . ? C29 C33 C28 122.0(6) . . ? C33 C34 C32 119.1(5) . . ? C33 C34 C25 118.4(6) . . ? C32 C34 C25 122.4(6) . . ? C1 N1 C11 117.0(6) . . ? C1 N1 Tb1 125.0(4) . . ? C11 N1 Tb1 116.5(4) . . ? C8 N2 C12 117.9(5) . . ? C8 N2 Tb1 122.3(4) . . ? C12 N2 Tb1 119.0(4) . . ? C13 N3 C23 117.0(5) . . ? C13 N3 Tb1 121.8(4) . . ? C23 N3 Tb1 121.2(4) . . ? C20 N4 C24 117.6(5) . . ? C20 N4 Tb1 123.6(4) . . ? C24 N4 Tb1 118.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Tb1 O1 Tb1 0.0 2_766 . . 2_766 ? O2 Tb1 O1 Tb1 174.1(2) . . . 2_766 ? O1W Tb1 O1 Tb1 -164.10(18) . . . 2_766 ? N2 Tb1 O1 Tb1 -86.91(17) . . . 2_766 ? N3 Tb1 O1 Tb1 118.50(18) . . . 2_766 ? N1 Tb1 O1 Tb1 -48.0(2) . . . 2_766 ? N4 Tb1 O1 Tb1 66.77(18) . . . 2_766 ? O3 S1 O2 Tb1 144.3(12) . . . . ? O4 S1 O2 Tb1 13.7(13) . . . . ? C26 S1 O2 Tb1 -98.5(12) . . . . ? O1 Tb1 O2 S1 177.9(11) 2_766 . . . ? O1 Tb1 O2 S1 6.3(14) . . . . ? O1W Tb1 O2 S1 -16.2(12) . . . . ? N2 Tb1 O2 S1 -85.8(12) . . . . ? N3 Tb1 O2 S1 60.9(12) . . . . ? N1 Tb1 O2 S1 -141.2(13) . . . . ? N4 Tb1 O2 S1 124.1(13) . . . . ? Tb1 Tb1 O2 S1 156.5(7) 2_766 . . . ? N1 C1 C2 C3 -1.7(13) . . . . ? C1 C2 C3 C9 -2.1(13) . . . . ? C9 C4 C5 C10 2.5(13) . . . . ? C10 C6 C7 C8 1.0(11) . . . . ? C6 C7 C8 N2 -1.3(11) . . . . ? C2 C3 C9 C11 3.0(11) . . . . ? C2 C3 C9 C4 -173.7(8) . . . . ? C5 C4 C9 C3 173.4(8) . . . . ? C5 C4 C9 C11 -3.2(12) . . . . ? C7 C6 C10 C12 0.6(10) . . . . ? C7 C6 C10 C5 179.9(7) . . . . ? C4 C5 C10 C6 -178.6(8) . . . . ? C4 C5 C10 C12 0.7(11) . . . . ? C3 C9 C11 N1 -0.4(10) . . . . ? C4 C9 C11 N1 176.5(6) . . . . ? C3 C9 C11 C12 -176.2(6) . . . . ? C4 C9 C11 C12 0.7(10) . . . . ? C6 C10 C12 N2 -2.2(9) . . . . ? C5 C10 C12 N2 178.5(6) . . . . ? C6 C10 C12 C11 176.2(6) . . . . ? C5 C10 C12 C11 -3.1(9) . . . . ? N1 C11 C12 N2 4.9(8) . . . . ? C9 C11 C12 N2 -179.2(6) . . . . ? N1 C11 C12 C10 -173.6(5) . . . . ? C9 C11 C12 C10 2.4(9) . . . . ? N3 C13 C14 C15 0.5(11) . . . . ? C13 C14 C15 C21 1.1(11) . . . . ? C21 C16 C17 C22 1.0(11) . . . . ? C22 C18 C19 C20 -2.5(10) . . . . ? C18 C19 C20 N4 -0.5(11) . . . . ? C14 C15 C21 C16 176.4(7) . . . . ? C14 C15 C21 C23 -0.8(10) . . . . ? C17 C16 C21 C15 -177.0(7) . . . . ? C17 C16 C21 C23 0.1(10) . . . . ? C19 C18 C22 C24 3.5(10) . . . . ? C19 C18 C22 C17 -173.8(7) . . . . ? C16 C17 C22 C18 176.5(7) . . . . ? C16 C17 C22 C24 -0.8(10) . . . . ? C15 C21 C23 N3 -1.0(9) . . . . ? C16 C21 C23 N3 -178.2(6) . . . . ? C15 C21 C23 C24 175.8(6) . . . . ? C16 C21 C23 C24 -1.4(9) . . . . ? C18 C22 C24 N4 -1.6(9) . . . . ? C17 C22 C24 N4 175.8(5) . . . . ? C18 C22 C24 C23 -178.0(6) . . . . ? C17 C22 C24 C23 -0.6(9) . . . . ? N3 C23 C24 N4 2.1(8) . . . . ? C21 C23 C24 N4 -174.9(5) . . . . ? N3 C23 C24 C22 178.6(5) . . . . ? C21 C23 C24 C22 1.6(8) . . . . ? C34 C25 C26 C27 1.8(10) . . . . ? C34 C25 C26 S1 -175.4(5) . . . . ? O3 S1 C26 C25 -144.4(7) . . . . ? O2 S1 C26 C25 95.0(6) . . . . ? O4 S1 C26 C25 -17.4(7) . . . . ? O3 S1 C26 C27 38.4(7) . . . . ? O2 S1 C26 C27 -82.1(6) . . . . ? O4 S1 C26 C27 165.4(7) . . . . ? C25 C26 C27 C28 -0.6(10) . . . . ? S1 C26 C27 C28 176.5(5) . . . . ? C26 C27 C28 C33 -1.3(10) . . . . ? C33 C29 C30 C31 1.2(11) . . . . ? C29 C30 C31 C32 0.7(10) . . . . ? C29 C30 C31 S2 -177.4(6) . . . . ? O5 S2 C31 C32 -80.5(7) . . . . ? O7 S2 C31 C32 151.5(6) . . . . ? O6 S2 C31 C32 32.9(7) . . . . ? O5 S2 C31 C30 97.6(7) . . . . ? O7 S2 C31 C30 -30.4(7) . . . . ? O6 S2 C31 C30 -149.0(6) . . . . ? C30 C31 C32 C34 -2.1(10) . . . . ? S2 C31 C32 C34 176.0(5) . . . . ? C30 C29 C33 C34 -1.7(10) . . . . ? C30 C29 C33 C28 177.6(7) . . . . ? C27 C28 C33 C34 1.9(10) . . . . ? C27 C28 C33 C29 -177.4(7) . . . . ? C29 C33 C34 C32 0.3(9) . . . . ? C28 C33 C34 C32 -179.0(6) . . . . ? C29 C33 C34 C25 178.6(6) . . . . ? C28 C33 C34 C25 -0.8(9) . . . . ? C31 C32 C34 C33 1.6(10) . . . . ? C31 C32 C34 C25 -176.6(6) . . . . ? C26 C25 C34 C33 -1.1(9) . . . . ? C26 C25 C34 C32 177.1(6) . . . . ? C2 C1 N1 C11 4.3(10) . . . . ? C2 C1 N1 Tb1 -161.2(6) . . . . ? C9 C11 N1 C1 -3.1(9) . . . . ? C12 C11 N1 C1 172.7(6) . . . . ? C9 C11 N1 Tb1 163.6(5) . . . . ? C12 C11 N1 Tb1 -20.5(7) . . . . ? O1 Tb1 N1 C1 95.1(5) 2_766 . . . ? O1 Tb1 N1 C1 141.0(5) . . . . ? O2 Tb1 N1 C1 -58.6(5) . . . . ? O1W Tb1 N1 C1 -119.0(5) . . . . ? N2 Tb1 N1 C1 -175.5(6) . . . . ? N3 Tb1 N1 C1 -13.2(7) . . . . ? N4 Tb1 N1 C1 15.1(5) . . . . ? Tb1 Tb1 N1 C1 115.3(5) 2_766 . . . ? O1 Tb1 N1 C11 -70.4(4) 2_766 . . . ? O1 Tb1 N1 C11 -24.6(5) . . . . ? O2 Tb1 N1 C11 135.9(5) . . . . ? O1W Tb1 N1 C11 75.5(5) . . . . ? N2 Tb1 N1 C11 19.0(4) . . . . ? N3 Tb1 N1 C11 -178.7(4) . . . . ? N4 Tb1 N1 C11 -150.4(4) . . . . ? Tb1 Tb1 N1 C11 -50.3(4) 2_766 . . . ? C7 C8 N2 C12 -0.2(9) . . . . ? C7 C8 N2 Tb1 169.0(5) . . . . ? C10 C12 N2 C8 2.0(8) . . . . ? C11 C12 N2 C8 -176.4(6) . . . . ? C10 C12 N2 Tb1 -167.6(4) . . . . ? C11 C12 N2 Tb1 14.0(7) . . . . ? O1 Tb1 N2 C8 -108.6(5) 2_766 . . . ? O1 Tb1 N2 C8 -38.5(5) . . . . ? O2 Tb1 N2 C8 112.3(5) . . . . ? O1W Tb1 N2 C8 44.8(5) . . . . ? N3 Tb1 N2 C8 10.7(6) . . . . ? N1 Tb1 N2 C8 174.1(5) . . . . ? N4 Tb1 N2 C8 -163.4(4) . . . . ? Tb1 Tb1 N2 C8 -73.8(5) 2_766 . . . ? O1 Tb1 N2 C12 60.5(4) 2_766 . . . ? O1 Tb1 N2 C12 130.6(4) . . . . ? O2 Tb1 N2 C12 -78.6(4) . . . . ? O1W Tb1 N2 C12 -146.1(4) . . . . ? N3 Tb1 N2 C12 179.8(4) . . . . ? N1 Tb1 N2 C12 -16.8(4) . . . . ? N4 Tb1 N2 C12 5.6(6) . . . . ? Tb1 Tb1 N2 C12 95.3(4) 2_766 . . . ? C14 C13 N3 C23 -2.2(9) . . . . ? C14 C13 N3 Tb1 176.8(5) . . . . ? C21 C23 N3 C13 2.5(8) . . . . ? C24 C23 N3 C13 -174.4(5) . . . . ? C21 C23 N3 Tb1 -176.5(4) . . . . ? C24 C23 N3 Tb1 6.6(7) . . . . ? O1 Tb1 N3 C13 107.6(5) 2_766 . . . ? O1 Tb1 N3 C13 45.4(5) . . . . ? O2 Tb1 N3 C13 -111.3(5) . . . . ? O1W Tb1 N3 C13 -37.7(5) . . . . ? N2 Tb1 N3 C13 -3.6(6) . . . . ? N1 Tb1 N3 C13 -154.5(4) . . . . ? N4 Tb1 N3 C13 173.3(5) . . . . ? Tb1 Tb1 N3 C13 75.5(5) 2_766 . . . ? O1 Tb1 N3 C23 -73.5(4) 2_766 . . . ? O1 Tb1 N3 C23 -135.7(4) . . . . ? O2 Tb1 N3 C23 67.6(4) . . . . ? O1W Tb1 N3 C23 141.2(4) . . . . ? N2 Tb1 N3 C23 175.4(4) . . . . ? N1 Tb1 N3 C23 24.4(6) . . . . ? N4 Tb1 N3 C23 -7.8(4) . . . . ? Tb1 Tb1 N3 C23 -105.6(4) 2_766 . . . ? C19 C20 N4 C24 2.4(9) . . . . ? C19 C20 N4 Tb1 -172.9(5) . . . . ? C22 C24 N4 C20 -1.3(8) . . . . ? C23 C24 N4 C20 175.0(5) . . . . ? C22 C24 N4 Tb1 174.2(4) . . . . ? C23 C24 N4 Tb1 -9.4(6) . . . . ? O1 Tb1 N4 C20 -55.2(4) 2_766 . . . ? O1 Tb1 N4 C20 -115.8(4) . . . . ? O2 Tb1 N4 C20 92.5(5) . . . . ? O1W Tb1 N4 C20 144.0(4) . . . . ? N2 Tb1 N4 C20 0.2(6) . . . . ? N3 Tb1 N4 C20 -176.1(5) . . . . ? N1 Tb1 N4 C20 20.2(5) . . . . ? Tb1 Tb1 N4 C20 -83.9(4) 2_766 . . . ? O1 Tb1 N4 C24 129.6(4) 2_766 . . . ? O1 Tb1 N4 C24 69.0(4) . . . . ? O2 Tb1 N4 C24 -82.8(4) . . . . ? O1W Tb1 N4 C24 -31.2(4) . . . . ? N2 Tb1 N4 C24 -175.0(4) . . . . ? N3 Tb1 N4 C24 8.7(4) . . . . ? N1 Tb1 N4 C24 -155.1(4) . . . . ? Tb1 Tb1 N4 C24 100.9(4) 2_766 . . . ? 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 O1 H1B O6 0.85 1.99 2.800(6) 157.8 2_776 O1W H1WA O4 0.86 2.37 3.174(12) 154.6 . O1W H1WA S1 0.86 3.05 3.632(5) 126.8 . O1W H1WB O5 0.86 2.04 2.901(10) 178.7 2_776 O3W H3WB O7 0.86 2.10 2.944(10) 167.0 2_677 O3W H3WA O3 0.90 1.99 2.878(16) 175.3 . _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 2.305 _refine_diff_density_min -1.008 _refine_diff_density_rms 0.139 #eof================================================================