# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Wuping Liao' _publ_contact_author_email WPLIAO@CIAC.JL.CN _publ_section_title ; Macroscopic single-crystal tubes assembled with porous supramolecular architecture of water-soluble calixarene and phenanthroline ; _publ_author_address ; State Key Lab of Rare Earth Resource Utilization Changchun Institute of Applied Chemistry CAS, Changchun 130022 P.R. China ; _publ_contact_author 'Prof Dr Wuping Liao' loop_ _publ_author_name 'Wuping Liao' 'Yanfeng Bi' 'Yanling Li' 'Zhongmin Su' 'Xiaofei Wang' # Attachment 'ESI-non-squeezed-data.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 665652' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'H5 Gd (C24H8O24S8) (C12H8N2)4 (H2O)9.08' _chemical_melting_point ? _chemical_formula_moiety 'H5 Gd [C24H8O24S8] [C12H8N2]4 [H2O]9.08' _chemical_formula_sum 'C72 H63.16 Gd N8 O33.08 S8' _chemical_formula_weight 1983.48 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 14.3385(8) _cell_length_b 18.1828(10) _cell_length_c 19.2533(11) _cell_angle_alpha 112.5980(10) _cell_angle_beta 92.7530(10) _cell_angle_gamma 97.7220(10) _cell_volume 4564.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7983 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 26.52 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.993 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7208 _exptl_absorpt_correction_T_max 0.9338 _exptl_absorpt_process_details ; SADABS, Sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 AXS Apex CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 33441 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.00 _reflns_number_total 17622 _reflns_number_gt 14286 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (1998)' _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. All the non-hydrogen atoms were refined anisotropically except some isolated molecular atoms. All the oxygen atoms of the solvent water molecules were refined without hydrogen atoms. The oxygen atoms of two sulfonate groups (O17-O19, O26-O28) were refined with disordered positions and the same displacement parameters for all oxygen atoms on one sulfonate group. The short contact O25...C68, C57...O26A and C60...O26A might be due to the high mobility of the isolated phenanthroline molecules. ; _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^)+(0.1408P)^2^+32.8513P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17622 _refine_ls_number_parameters 1088 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.2448 _refine_ls_wR_factor_gt 0.2336 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.03242(2) 0.75770(2) 0.020473(19) 0.01944(13) Uani 1 1 d . . . S1 S 0.08536(13) 1.01248(11) 0.09128(11) 0.0222(4) Uani 1 1 d . . . S2 S -0.22246(13) 0.83338(11) 0.14609(11) 0.0232(4) Uani 1 1 d . . . S3 S 0.00421(14) 0.59932(11) 0.12262(11) 0.0260(4) Uani 1 1 d . . . S4 S 0.32087(13) 0.81817(11) 0.15561(10) 0.0218(4) Uani 1 1 d . . . S5 S 0.33916(17) 1.13357(13) 0.33803(12) 0.0380(5) Uani 1 1 d . . . S6 S -0.20602(14) 1.15475(12) 0.22637(11) 0.0273(4) Uani 1 1 d . . . S7 S -0.15932(18) 0.7370(2) 0.37573(14) 0.0511(7) Uani 1 1 d . . . S8 S 0.3266(2) 0.59802(16) 0.28242(17) 0.0500(7) Uani 1 1 d . . . N1 N -0.3730(5) 1.1536(4) 0.0586(4) 0.0295(15) Uani 1 1 d . . . N2 N -0.3138(4) 1.0093(4) 0.0102(4) 0.0263(14) Uani 1 1 d . . . N3 N 0.1061(5) 1.0591(6) 0.4574(4) 0.044(2) Uani 1 1 d . . . N4 N 0.1440(5) 0.9942(6) 0.5579(4) 0.049(2) Uani 1 1 d . . . N5 N 0.3468(5) 0.4390(4) 0.0732(5) 0.043(2) Uani 1 1 d . . . N6 N 0.5319(6) 0.4515(4) 0.1234(5) 0.047(2) Uani 1 1 d . . . N7 N -0.3636(6) 1.0300(6) 0.5567(5) 0.055(3) Uani 1 1 d . . . N8 N -0.3821(6) 0.8716(7) 0.4672(5) 0.057(3) Uani 1 1 d . . . O1 O 0.1686(4) 0.8549(3) 0.0598(3) 0.0226(11) Uani 1 1 d . A . O2 O -0.0168(3) 0.8686(3) 0.1124(3) 0.0215(10) Uani 1 1 d . . . O3 O -0.0974(4) 0.7082(3) 0.0658(3) 0.0227(11) Uani 1 1 d . . . O4 O 0.1068(4) 0.7528(3) 0.1280(3) 0.0239(11) Uani 1 1 d . B . O5 O 0.0670(5) 0.7860(4) -0.0897(4) 0.0443(16) Uani 1 1 d . . . O6 O -0.0291(4) 0.6304(3) -0.0858(3) 0.0308(12) Uani 1 1 d . . . O7 O 0.1647(4) 0.6840(3) -0.0241(3) 0.0304(12) Uani 1 1 d . . . O8 O -0.1119(4) 0.7817(3) -0.0408(3) 0.0290(12) Uani 1 1 d . . . O9 O 0.0726(4) 0.9539(3) 0.0152(3) 0.0303(12) Uani 1 1 d . . . O10 O 0.1103(4) 1.0966(3) 0.1038(3) 0.0291(12) Uani 1 1 d . . . O11 O -0.2468(4) 0.7899(3) 0.0653(3) 0.0279(12) Uani 1 1 d . . . O12 O -0.3012(4) 0.8526(3) 0.1905(3) 0.0330(13) Uani 1 1 d . . . O13 O -0.0204(4) 0.5294(3) 0.1404(4) 0.0344(13) Uani 1 1 d . . . O14 O 0.0042(4) 0.5870(3) 0.0446(3) 0.0346(13) Uani 1 1 d . . . O15 O 0.3208(4) 0.7789(3) 0.0744(3) 0.0257(11) Uani 1 1 d . . . O16 O 0.4120(4) 0.8413(3) 0.1999(3) 0.0295(12) Uani 1 1 d . . . O17A O 0.3965(15) 1.1854(12) 0.3093(11) 0.064(2) Uani 0.416(11) 1 d P A 1 O18A O 0.4071(15) 1.1062(12) 0.3819(11) 0.064(2) Uani 0.416(11) 1 d P A 1 O19A O 0.2713(15) 1.1695(13) 0.3836(11) 0.064(2) Uani 0.416(11) 1 d P A 1 O17B O 0.3126(10) 1.2032(8) 0.3228(7) 0.064(2) Uani 0.58 1 d P A 2 O18B O 0.4348(10) 1.1344(8) 0.3388(8) 0.064(2) Uani 0.58 1 d P A 2 O19B O 0.2953(10) 1.1277(9) 0.4012(8) 0.064(2) Uani 0.58 1 d P A 2 O20 O -0.2922(4) 1.1299(4) 0.2540(4) 0.0418(15) Uani 1 1 d . . . O21 O -0.1383(5) 1.2166(4) 0.2859(4) 0.0431(16) Uani 1 1 d . . . O22 O -0.2234(4) 1.1793(3) 0.1636(3) 0.0334(13) Uani 1 1 d . . . O23 O -0.2341(6) 0.6700(5) 0.3631(5) 0.064(2) Uani 1 1 d . . . O24 O -0.0705(6) 0.7283(8) 0.4103(5) 0.089(3) Uani 1 1 d . . . O25 O -0.1891(6) 0.8139(5) 0.4151(4) 0.062(2) Uani 1 1 d . . . O26A O 0.418(2) 0.5830(16) 0.2426(18) 0.078(3) Uani 0.379(15) 1 d P B 1 O27A O 0.276(3) 0.523(2) 0.2716(18) 0.078(3) Uani 0.379(15) 1 d P B 1 O28A O 0.361(2) 0.6580(16) 0.3621(16) 0.078(3) Uani 0.379(15) 1 d P B 1 O26B O 0.4249(14) 0.6179(10) 0.2723(11) 0.078(3) Uani 0.62 1 d P B 2 O27B O 0.2927(16) 0.5114(13) 0.2426(11) 0.078(3) Uani 0.62 1 d P B 2 O28B O 0.3027(13) 0.6283(10) 0.3578(10) 0.078(3) Uani 0.62 1 d P B 2 C1 C 0.1728(5) 0.9914(4) 0.1457(4) 0.0223(15) Uani 1 1 d . A . C2 C -0.0207(5) 1.0057(4) 0.1341(4) 0.0203(14) Uani 1 1 d . . . C3 C -0.0635(5) 1.0728(4) 0.1623(4) 0.0215(15) Uani 1 1 d . . . H3 H -0.0337 1.1227 0.1623 0.026 Uiso 1 1 calc R . . C4 C -0.1507(5) 1.0679(4) 0.1910(4) 0.0222(15) Uani 1 1 d . . . C5 C -0.1945(5) 0.9946(5) 0.1894(4) 0.0236(15) Uani 1 1 d . . . H5 H -0.2543 0.9908 0.2081 0.028 Uiso 1 1 calc R . . C6 C -0.1519(5) 0.9266(4) 0.1606(4) 0.0211(15) Uani 1 1 d . . . C7 C -0.1609(5) 0.7749(4) 0.1818(4) 0.0230(15) Uani 1 1 d . . . C8 C -0.1739(5) 0.7837(5) 0.2558(4) 0.0259(16) Uani 1 1 d . . . H8 H -0.2075 0.8239 0.2862 0.031 Uiso 1 1 calc R . . C9 C -0.1372(6) 0.7327(5) 0.2845(5) 0.0311(18) Uani 1 1 d . . . C10 C -0.0852(5) 0.6763(5) 0.2414(4) 0.0265(16) Uani 1 1 d . . . H10 H -0.0598 0.6420 0.2615 0.032 Uiso 1 1 calc R . . C11 C -0.0703(5) 0.6696(4) 0.1689(4) 0.0239(15) Uani 1 1 d . . . C12 C 0.1186(6) 0.6466(4) 0.1682(4) 0.0258(16) Uani 1 1 d . B . C13 C 0.1683(6) 0.6108(5) 0.2055(5) 0.0274(17) Uani 1 1 d . . . H13 H 0.1390 0.5642 0.2119 0.033 Uiso 1 1 calc R B . C14 C 0.2629(6) 0.6440(5) 0.2338(5) 0.0318(18) Uani 1 1 d . B . C15 C 0.3059(6) 0.7110(5) 0.2216(5) 0.0293(17) Uani 1 1 d . . . H15 H 0.3708 0.7323 0.2392 0.035 Uiso 1 1 calc R B . C16 C 0.2555(5) 0.7464(4) 0.1845(4) 0.0231(15) Uani 1 1 d . B . C17 C 0.2698(5) 0.9064(5) 0.1759(4) 0.0233(15) Uani 1 1 d . A . C18 C 0.3112(5) 0.9728(5) 0.2413(4) 0.0244(16) Uani 1 1 d . . . H18 H 0.3583 0.9665 0.2741 0.029 Uiso 1 1 calc R A . C19 C 0.2844(6) 1.0472(5) 0.2584(4) 0.0278(17) Uani 1 1 d . A . C20 C 0.2146(6) 1.0558(5) 0.2103(4) 0.0259(16) Uani 1 1 d . . . H20 H 0.1956 1.1070 0.2224 0.031 Uiso 1 1 calc R A . C21 C 0.2006(5) 0.9127(4) 0.1220(4) 0.0204(15) Uani 1 1 d . . . C22 C -0.0604(5) 0.9290(4) 0.1329(4) 0.0199(14) Uani 1 1 d . . . C23 C -0.1077(5) 0.7174(4) 0.1341(4) 0.0218(15) Uani 1 1 d . . . C24 C 0.1570(5) 0.7174(4) 0.1577(4) 0.0215(15) Uani 1 1 d . . . C25 C -0.4006(6) 1.2264(5) 0.0875(5) 0.0344(19) Uani 1 1 d . . . H25 H -0.3694 1.2666 0.1338 0.041 Uiso 1 1 calc R . . C26 C -0.4746(6) 1.2426(6) 0.0496(6) 0.040(2) Uani 1 1 d . . . H26 H -0.4940 1.2939 0.0700 0.048 Uiso 1 1 calc R . . C27 C -0.5194(6) 1.1852(6) -0.0167(6) 0.039(2) Uani 1 1 d . . . H27 H -0.5701 1.1967 -0.0425 0.046 Uiso 1 1 calc R . . C28 C -0.5333(6) 1.0449(6) -0.1178(5) 0.039(2) Uani 1 1 d . . . H28 H -0.5835 1.0537 -0.1460 0.046 Uiso 1 1 calc R . . C29 C -0.5038(6) 0.9737(6) -0.1442(5) 0.039(2) Uani 1 1 d . . . H29 H -0.5330 0.9331 -0.1911 0.047 Uiso 1 1 calc R . . C30 C -0.3954(6) 0.8830(5) -0.1247(5) 0.038(2) Uani 1 1 d . . . H30 H -0.4229 0.8396 -0.1705 0.046 Uiso 1 1 calc R . . C31 C -0.3243(6) 0.8732(5) -0.0805(5) 0.0345(19) Uani 1 1 d . . . H31 H -0.3020 0.8231 -0.0950 0.041 Uiso 1 1 calc R . . C32 C -0.2853(6) 0.9383(5) -0.0137(5) 0.0303(17) Uani 1 1 d . . . H32 H -0.2354 0.9312 0.0161 0.036 Uiso 1 1 calc R . . C33 C -0.3837(5) 1.0179(5) -0.0335(5) 0.0263(16) Uani 1 1 d . . . C34 C -0.4273(6) 0.9572(5) -0.1022(5) 0.0291(17) Uani 1 1 d . . . C35 C -0.4910(5) 1.1088(5) -0.0474(5) 0.0294(18) Uani 1 1 d . . . C36 C -0.4159(5) 1.0942(5) -0.0084(5) 0.0282(17) Uani 1 1 d . . . C37 C 0.0820(7) 1.0949(8) 0.4116(6) 0.056(3) Uani 1 1 d . . . H37 H 0.0790 1.1510 0.4315 0.067 Uiso 1 1 calc R . . C38 C 0.0610(7) 1.0475(9) 0.3328(6) 0.057(3) Uani 1 1 d . . . H38 H 0.0448 1.0721 0.2994 0.068 Uiso 1 1 calc R . . C39 C 0.0639(7) 0.9691(8) 0.3057(5) 0.051(3) Uani 1 1 d . . . H39 H 0.0495 0.9382 0.2529 0.061 Uiso 1 1 calc R . . C40 C 0.0915(7) 0.8486(7) 0.3273(6) 0.053(3) Uani 1 1 d . . . H40 H 0.0791 0.8155 0.2748 0.064 Uiso 1 1 calc R . . C41 C 0.1129(8) 0.8150(8) 0.3765(6) 0.060(3) Uani 1 1 d . . . H41 H 0.1159 0.7590 0.3576 0.073 Uiso 1 1 calc R . . C42 C 0.1500(9) 0.8306(9) 0.5103(7) 0.071(4) Uani 1 1 d . . . H42 H 0.1519 0.7746 0.4946 0.085 Uiso 1 1 calc R . . C43 C 0.1655(9) 0.8780(10) 0.5837(8) 0.071(4) Uani 1 1 d . . . H43 H 0.1784 0.8565 0.6204 0.086 Uiso 1 1 calc R . . C44 C 0.1622(8) 0.9604(10) 0.6053(6) 0.066(4) Uani 1 1 d . . . H44 H 0.1739 0.9941 0.6576 0.079 Uiso 1 1 calc R . . C45 C 0.1277(6) 0.9443(7) 0.4837(5) 0.045(3) Uani 1 1 d . . . C46 C 0.1308(7) 0.8612(8) 0.4553(6) 0.053(3) Uani 1 1 d . . . C47 C 0.0872(6) 0.9311(7) 0.3523(5) 0.045(3) Uani 1 1 d . . . C48 C 0.1072(6) 0.9812(7) 0.4323(5) 0.041(2) Uani 1 1 d . . . C49 C 0.2552(7) 0.4279(6) 0.0472(6) 0.053(3) Uani 1 1 d . . . H49 H 0.2137 0.3807 0.0432 0.063 Uiso 1 1 calc R . . C50 C 0.2208(7) 0.4855(7) 0.0260(6) 0.057(3) Uani 1 1 d . . . H50 H 0.1563 0.4778 0.0069 0.068 Uiso 1 1 calc R . . C51 C 0.2825(8) 0.5535(7) 0.0334(6) 0.051(3) Uani 1 1 d . . . H51 H 0.2600 0.5938 0.0203 0.061 Uiso 1 1 calc R . . C52 C 0.4471(8) 0.6348(6) 0.0698(6) 0.046(2) Uani 1 1 d . . . H52 H 0.4277 0.6757 0.0559 0.055 Uiso 1 1 calc R . . C53 C 0.5360(7) 0.6436(5) 0.0975(6) 0.043(2) Uani 1 1 d . . . H53 H 0.5789 0.6908 0.1036 0.052 Uiso 1 1 calc R . . C54 C 0.6623(7) 0.5901(6) 0.1478(7) 0.054(3) Uani 1 1 d . . . H54 H 0.7069 0.6375 0.1575 0.065 Uiso 1 1 calc R . . C55 C 0.6884(8) 0.5291(7) 0.1623(8) 0.069(4) Uani 1 1 d . . . H55 H 0.7518 0.5327 0.1816 0.083 Uiso 1 1 calc R . . C56 C 0.6218(7) 0.4595(6) 0.1491(8) 0.060(3) Uani 1 1 d . . . H56 H 0.6421 0.4165 0.1588 0.072 Uiso 1 1 calc R . . C57 C 0.5054(6) 0.5125(5) 0.1079(5) 0.0338(19) Uani 1 1 d . . . C58 C 0.5685(6) 0.5840(5) 0.1181(5) 0.038(2) Uani 1 1 d . . . C59 C 0.3781(7) 0.5643(5) 0.0601(5) 0.038(2) Uani 1 1 d . . . C60 C 0.4094(6) 0.5061(5) 0.0800(5) 0.0331(19) Uani 1 1 d . . . C61 C -0.3581(8) 1.1085(8) 0.5998(6) 0.055(3) Uani 1 1 d . . . H61 H -0.3463 1.1255 0.6531 0.067 Uiso 1 1 calc R . . C62 C -0.3682(9) 1.1651(8) 0.5717(6) 0.066(4) Uani 1 1 d . . . H62 H -0.3621 1.2205 0.6045 0.079 Uiso 1 1 calc R . . C63 C -0.3877(9) 1.1407(9) 0.4948(7) 0.071(4) Uani 1 1 d . . . H63 H -0.3968 1.1793 0.4741 0.085 Uiso 1 1 calc R . . C64 C -0.4132(8) 1.0297(9) 0.3657(7) 0.067(4) Uani 1 1 d . . . H64 H -0.4212 1.0663 0.3424 0.080 Uiso 1 1 calc R . . C65 C -0.4196(7) 0.9512(8) 0.3228(6) 0.055(3) Uani 1 1 d . . . H65 H -0.4304 0.9331 0.2693 0.066 Uiso 1 1 calc R . . C66 C -0.4225(7) 0.8118(8) 0.3135(6) 0.055(3) Uani 1 1 d . . . H66 H -0.4363 0.7900 0.2600 0.065 Uiso 1 1 calc R . . C67 C -0.4144(8) 0.7629(9) 0.3486(7) 0.067(4) Uani 1 1 d . . . H67 H -0.4249 0.7062 0.3201 0.081 Uiso 1 1 calc R . . C68 C -0.3913(9) 0.7925(9) 0.4254(7) 0.068(4) Uani 1 1 d . . . H68 H -0.3818 0.7564 0.4491 0.081 Uiso 1 1 calc R . . C69 C -0.3899(6) 0.9254(7) 0.4348(5) 0.048(3) Uani 1 1 d . . . C70 C -0.4108(7) 0.8956(8) 0.3544(5) 0.055(3) Uani 1 1 d . . . C71 C -0.3940(7) 1.0603(8) 0.4476(6) 0.056(3) Uani 1 1 d . . . C72 C -0.3817(6) 1.0076(7) 0.4820(6) 0.050(3) Uani 1 1 d . . . O001 O 0.3329(5) 0.4740(5) 0.4848(4) 0.0034(13) Uiso 0.481(12) 1 d P . . O002 O 0.3790(5) 0.4400(4) 0.4709(4) 0.0034(13) Uiso 0.52 1 d P . . O003 O 0.2167(5) 0.5448(4) 0.5099(4) 0.016(2) Uiso 0.71(2) 1 d P . . O004 O 0.3449(8) 0.3279(6) 0.1336(6) 0.076(4) Uiso 0.91(3) 1 d P . . O005 O 0.1932(10) 0.6439(8) -0.1744(8) 0.082(5) Uiso 0.76(3) 1 d P . . O006 O 0.1707(10) 0.3819(9) 0.1910(8) 0.058(5) Uiso 0.55(3) 1 d P . . O007 O 0.0493(12) 1.2242(10) 0.3363(9) 0.089(7) Uiso 0.66(3) 1 d P . . O008 O 0.0695(15) 1.3291(13) 0.4771(12) 0.087(9) Uiso 0.49(3) 1 d P . . 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 0.0187(2) 0.02014(19) 0.0200(2) 0.00790(14) 0.00379(13) 0.00458(13) S1 0.0193(9) 0.0259(9) 0.0292(10) 0.0176(8) 0.0076(7) 0.0077(7) S2 0.0165(8) 0.0250(9) 0.0288(10) 0.0115(8) 0.0038(7) 0.0025(7) S3 0.0261(10) 0.0216(9) 0.0322(10) 0.0127(8) 0.0045(8) 0.0032(7) S4 0.0189(9) 0.0258(9) 0.0264(9) 0.0150(7) 0.0045(7) 0.0071(7) S5 0.0457(13) 0.0342(11) 0.0275(10) 0.0048(9) -0.0006(9) 0.0083(10) S6 0.0257(10) 0.0285(9) 0.0283(10) 0.0093(8) 0.0043(8) 0.0123(8) S7 0.0396(13) 0.094(2) 0.0313(12) 0.0351(13) 0.0116(10) 0.0148(13) S8 0.0549(16) 0.0448(13) 0.0610(17) 0.0355(13) -0.0139(13) 0.0063(12) N1 0.026(3) 0.033(4) 0.038(4) 0.023(3) 0.007(3) 0.005(3) N2 0.020(3) 0.036(4) 0.030(3) 0.021(3) 0.006(3) 0.006(3) N3 0.034(4) 0.072(6) 0.025(4) 0.018(4) 0.012(3) 0.002(4) N4 0.028(4) 0.092(7) 0.022(4) 0.021(4) 0.002(3) 0.001(4) N5 0.027(4) 0.030(4) 0.055(5) 0.001(3) -0.003(3) 0.003(3) N6 0.036(4) 0.028(4) 0.070(6) 0.015(4) -0.015(4) 0.002(3) N7 0.029(4) 0.089(7) 0.029(4) 0.007(4) 0.005(3) -0.001(4) N8 0.037(5) 0.088(7) 0.033(4) 0.010(5) -0.002(4) 0.008(5) O1 0.020(3) 0.025(3) 0.028(3) 0.016(2) 0.005(2) 0.006(2) O2 0.021(3) 0.020(2) 0.024(3) 0.008(2) 0.005(2) 0.006(2) O3 0.022(3) 0.023(2) 0.023(3) 0.009(2) 0.002(2) -0.001(2) O4 0.021(3) 0.025(3) 0.031(3) 0.016(2) 0.008(2) 0.006(2) O5 0.038(4) 0.073(5) 0.049(4) 0.048(4) 0.017(3) 0.023(3) O6 0.037(3) 0.028(3) 0.027(3) 0.010(2) 0.003(2) 0.010(2) O7 0.033(3) 0.032(3) 0.029(3) 0.013(2) 0.006(2) 0.012(2) O8 0.030(3) 0.030(3) 0.029(3) 0.014(2) 0.002(2) 0.008(2) O9 0.031(3) 0.040(3) 0.028(3) 0.018(3) 0.008(2) 0.016(3) O10 0.023(3) 0.028(3) 0.046(3) 0.025(3) 0.009(2) 0.006(2) O11 0.024(3) 0.029(3) 0.029(3) 0.011(2) -0.001(2) 0.003(2) O12 0.023(3) 0.035(3) 0.044(3) 0.018(3) 0.010(2) 0.006(2) O13 0.034(3) 0.024(3) 0.049(4) 0.018(3) 0.008(3) 0.004(2) O14 0.038(3) 0.034(3) 0.029(3) 0.009(2) 0.002(3) 0.008(3) O15 0.021(3) 0.031(3) 0.030(3) 0.014(2) 0.008(2) 0.010(2) O16 0.020(3) 0.032(3) 0.040(3) 0.018(3) 0.001(2) 0.008(2) O17A 0.064(4) 0.059(4) 0.047(4) -0.001(3) -0.005(3) 0.001(3) O18A 0.064(4) 0.059(4) 0.047(4) -0.001(3) -0.005(3) 0.001(3) O19A 0.064(4) 0.059(4) 0.047(4) -0.001(3) -0.005(3) 0.001(3) O17B 0.064(4) 0.059(4) 0.047(4) -0.001(3) -0.005(3) 0.001(3) O18B 0.064(4) 0.059(4) 0.047(4) -0.001(3) -0.005(3) 0.001(3) O19B 0.064(4) 0.059(4) 0.047(4) -0.001(3) -0.005(3) 0.001(3) O20 0.035(3) 0.045(4) 0.056(4) 0.025(3) 0.022(3) 0.021(3) O21 0.044(4) 0.036(3) 0.038(3) 0.000(3) -0.009(3) 0.015(3) O22 0.036(3) 0.031(3) 0.038(3) 0.015(3) 0.003(3) 0.014(3) O23 0.066(5) 0.087(6) 0.059(5) 0.050(5) 0.027(4) 0.009(4) O24 0.057(5) 0.191(11) 0.048(5) 0.073(6) 0.014(4) 0.041(6) O25 0.059(5) 0.088(6) 0.025(3) 0.006(4) 0.015(3) 0.007(4) O26A 0.084(6) 0.073(6) 0.097(8) 0.059(6) -0.018(6) 0.013(5) O27A 0.084(6) 0.073(6) 0.097(8) 0.059(6) -0.018(6) 0.013(5) O28A 0.084(6) 0.073(6) 0.097(8) 0.059(6) -0.018(6) 0.013(5) O26B 0.084(6) 0.073(6) 0.097(8) 0.059(6) -0.018(6) 0.013(5) O27B 0.084(6) 0.073(6) 0.097(8) 0.059(6) -0.018(6) 0.013(5) O28B 0.084(6) 0.073(6) 0.097(8) 0.059(6) -0.018(6) 0.013(5) C1 0.015(3) 0.028(4) 0.035(4) 0.023(3) 0.008(3) 0.007(3) C2 0.017(3) 0.026(4) 0.020(3) 0.011(3) 0.003(3) 0.005(3) C3 0.023(4) 0.019(3) 0.024(4) 0.011(3) 0.000(3) 0.005(3) C4 0.019(3) 0.027(4) 0.025(4) 0.014(3) 0.003(3) 0.008(3) C5 0.017(3) 0.030(4) 0.021(4) 0.007(3) 0.003(3) 0.004(3) C6 0.013(3) 0.026(4) 0.024(4) 0.010(3) 0.003(3) 0.001(3) C7 0.018(3) 0.022(3) 0.028(4) 0.011(3) -0.001(3) -0.001(3) C8 0.020(4) 0.030(4) 0.024(4) 0.007(3) 0.005(3) 0.002(3) C9 0.023(4) 0.047(5) 0.024(4) 0.016(4) 0.005(3) 0.003(4) C10 0.020(4) 0.034(4) 0.032(4) 0.023(4) 0.002(3) -0.001(3) C11 0.021(4) 0.026(4) 0.028(4) 0.014(3) 0.004(3) 0.000(3) C12 0.027(4) 0.023(4) 0.029(4) 0.011(3) 0.006(3) 0.005(3) C13 0.032(4) 0.023(4) 0.033(4) 0.015(3) 0.007(3) 0.009(3) C14 0.040(5) 0.030(4) 0.031(4) 0.017(3) -0.001(4) 0.011(4) C15 0.027(4) 0.030(4) 0.029(4) 0.009(3) 0.001(3) 0.008(3) C16 0.022(4) 0.023(4) 0.028(4) 0.013(3) 0.006(3) 0.006(3) C17 0.020(4) 0.029(4) 0.027(4) 0.018(3) 0.005(3) 0.002(3) C18 0.023(4) 0.032(4) 0.024(4) 0.015(3) 0.004(3) 0.008(3) C19 0.028(4) 0.030(4) 0.024(4) 0.009(3) 0.008(3) 0.002(3) C20 0.028(4) 0.026(4) 0.028(4) 0.014(3) 0.010(3) 0.008(3) C21 0.014(3) 0.023(3) 0.031(4) 0.018(3) 0.008(3) 0.001(3) C22 0.016(3) 0.029(4) 0.017(3) 0.011(3) 0.002(3) 0.004(3) C23 0.017(3) 0.023(3) 0.024(4) 0.010(3) 0.001(3) -0.003(3) C24 0.020(4) 0.027(4) 0.022(4) 0.012(3) 0.008(3) 0.007(3) C25 0.033(4) 0.030(4) 0.048(5) 0.023(4) 0.010(4) 0.008(4) C26 0.033(5) 0.043(5) 0.059(6) 0.032(5) 0.016(4) 0.014(4) C27 0.022(4) 0.050(5) 0.065(6) 0.043(5) 0.013(4) 0.010(4) C28 0.019(4) 0.063(6) 0.047(5) 0.038(5) 0.001(4) 0.005(4) C29 0.028(4) 0.059(6) 0.031(4) 0.023(4) 0.001(4) -0.007(4) C30 0.037(5) 0.035(5) 0.037(5) 0.010(4) 0.018(4) -0.003(4) C31 0.033(5) 0.033(4) 0.039(5) 0.016(4) 0.011(4) 0.004(4) C32 0.029(4) 0.037(4) 0.034(4) 0.022(4) 0.014(3) 0.010(3) C33 0.024(4) 0.033(4) 0.030(4) 0.020(3) 0.012(3) 0.004(3) C34 0.022(4) 0.037(4) 0.034(4) 0.021(4) 0.006(3) 0.000(3) C35 0.019(4) 0.044(5) 0.037(4) 0.029(4) 0.005(3) 0.001(3) C36 0.016(4) 0.038(4) 0.040(5) 0.027(4) 0.004(3) 0.000(3) C37 0.042(6) 0.094(9) 0.038(6) 0.034(6) 0.005(5) 0.007(6) C38 0.034(5) 0.109(10) 0.034(5) 0.038(6) 0.009(4) 0.003(6) C39 0.031(5) 0.083(8) 0.027(5) 0.013(5) 0.004(4) -0.001(5) C40 0.034(5) 0.073(7) 0.028(5) -0.003(5) 0.002(4) 0.004(5) C41 0.049(6) 0.077(8) 0.045(6) 0.016(6) -0.001(5) 0.007(6) C42 0.064(8) 0.094(10) 0.059(8) 0.035(7) 0.007(6) 0.018(7) C43 0.053(7) 0.115(12) 0.059(8) 0.048(8) 0.005(6) 0.014(7) C44 0.038(6) 0.129(12) 0.035(6) 0.040(7) 0.003(4) 0.010(7) C45 0.017(4) 0.087(8) 0.030(5) 0.024(5) 0.007(3) 0.002(4) C46 0.034(5) 0.076(8) 0.045(6) 0.021(5) 0.006(4) 0.008(5) C47 0.020(4) 0.083(8) 0.024(4) 0.016(5) 0.006(3) 0.000(4) C48 0.025(4) 0.070(7) 0.022(4) 0.014(4) 0.008(3) 0.002(4) C49 0.029(5) 0.048(6) 0.057(6) -0.002(5) -0.007(4) 0.006(4) C50 0.035(5) 0.071(7) 0.042(6) -0.004(5) -0.011(4) 0.020(5) C51 0.048(6) 0.064(7) 0.039(5) 0.011(5) 0.003(5) 0.033(5) C52 0.067(7) 0.036(5) 0.047(6) 0.022(4) 0.021(5) 0.027(5) C53 0.051(6) 0.023(4) 0.052(6) 0.009(4) 0.018(5) 0.008(4) C54 0.039(6) 0.040(5) 0.072(7) 0.014(5) 0.002(5) -0.009(4) C55 0.037(6) 0.063(7) 0.096(10) 0.028(7) -0.033(6) -0.007(5) C56 0.040(6) 0.042(6) 0.096(9) 0.029(6) -0.021(6) 0.006(5) C57 0.031(4) 0.023(4) 0.042(5) 0.009(4) -0.004(4) 0.003(3) C58 0.034(5) 0.025(4) 0.047(5) 0.006(4) 0.005(4) 0.000(3) C59 0.038(5) 0.036(5) 0.038(5) 0.007(4) 0.006(4) 0.016(4) C60 0.028(4) 0.022(4) 0.039(5) 0.002(3) 0.001(4) 0.005(3) C61 0.042(6) 0.076(8) 0.035(5) 0.010(6) 0.010(4) -0.001(5) C62 0.059(7) 0.074(8) 0.040(6) -0.002(6) 0.017(5) -0.005(6) C63 0.061(8) 0.092(10) 0.052(7) 0.022(7) 0.020(6) 0.000(7) C64 0.046(7) 0.110(11) 0.047(7) 0.036(7) 0.009(5) 0.002(7) C65 0.025(5) 0.095(9) 0.028(5) 0.007(6) 0.003(4) 0.000(5) C66 0.025(5) 0.091(9) 0.026(5) 0.001(5) 0.001(4) 0.004(5) C67 0.037(6) 0.090(9) 0.047(7) -0.002(6) -0.002(5) 0.013(6) C68 0.053(7) 0.085(9) 0.050(7) 0.007(6) -0.003(5) 0.023(6) C69 0.021(4) 0.078(7) 0.025(5) -0.001(5) 0.007(3) 0.003(4) C70 0.023(5) 0.101(9) 0.026(5) 0.010(5) 0.005(4) 0.003(5) C71 0.026(5) 0.090(9) 0.036(5) 0.007(6) 0.012(4) 0.003(5) C72 0.022(4) 0.080(8) 0.037(5) 0.011(5) 0.010(4) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O3 2.312(5) . ? Gd1 O4 2.322(5) . ? Gd1 O1 2.326(5) . ? Gd1 O2 2.336(5) . ? Gd1 O5 2.425(6) . ? Gd1 O6 2.442(5) . ? Gd1 O7 2.467(6) . ? Gd1 O8 2.504(5) . ? S1 O9 1.427(6) . ? S1 O10 1.445(5) . ? S1 C1 1.769(7) . ? S1 C2 1.777(7) . ? S2 O11 1.448(6) . ? S2 O12 1.449(6) . ? S2 C6 1.768(7) . ? S2 C7 1.772(8) . ? S3 O14 1.430(6) . ? S3 O13 1.443(6) . ? S3 C12 1.762(8) . ? S3 C11 1.775(8) . ? S4 O16 1.442(6) . ? S4 O15 1.448(6) . ? S4 C17 1.767(8) . ? S4 C16 1.782(7) . ? S5 O18B 1.369(15) . ? S5 O19A 1.40(2) . ? S5 O19B 1.429(16) . ? S5 O17A 1.45(2) . ? S5 O17B 1.495(16) . ? S5 O18A 1.51(2) . ? S5 C19 1.771(8) . ? S6 O20 1.454(6) . ? S6 O21 1.459(6) . ? S6 O22 1.462(6) . ? S6 C4 1.775(7) . ? S7 O23 1.446(9) . ? S7 O25 1.446(9) . ? S7 O24 1.463(8) . ? S7 C9 1.774(8) . ? S8 O27A 1.38(4) . ? S8 O28B 1.418(19) . ? S8 O26B 1.45(2) . ? S8 O27B 1.46(2) . ? S8 O28A 1.51(3) . ? S8 O26A 1.55(4) . ? S8 C14 1.770(8) . ? N1 C25 1.347(11) . ? N1 C36 1.373(11) . ? N2 C32 1.322(11) . ? N2 C33 1.342(10) . ? N3 C48 1.312(14) . ? N3 C37 1.339(14) . ? N4 C44 1.316(15) . ? N4 C45 1.354(12) . ? N5 C49 1.343(12) . ? N5 C60 1.372(11) . ? N6 C56 1.326(12) . ? N6 C57 1.348(11) . ? N7 C61 1.336(15) . ? N7 C72 1.336(13) . ? N8 C68 1.335(16) . ? N8 C69 1.362(15) . ? O1 C21 1.265(9) . ? O2 C22 1.275(9) . ? O3 C23 1.279(9) . ? O4 C24 1.275(9) . ? C1 C20 1.379(11) . ? C1 C21 1.442(10) . ? C2 C3 1.372(10) . ? C2 C22 1.424(10) . ? C3 C4 1.398(10) . ? C3 H3 0.9500 . ? C4 C5 1.382(11) . ? C5 C6 1.385(11) . ? C5 H5 0.9500 . ? C6 C22 1.441(10) . ? C7 C8 1.396(11) . ? C7 C23 1.436(11) . ? C8 C9 1.392(12) . ? C8 H8 0.9500 . ? C9 C10 1.381(12) . ? C10 C11 1.384(11) . ? C10 H10 0.9500 . ? C11 C23 1.425(10) . ? C12 C13 1.372(11) . ? C12 C24 1.421(10) . ? C13 C14 1.398(12) . ? C13 H13 0.9500 . ? C14 C15 1.398(12) . ? C15 C16 1.369(11) . ? C15 H15 0.9500 . ? C16 C24 1.435(10) . ? C17 C18 1.402(11) . ? C17 C21 1.448(10) . ? C18 C19 1.377(11) . ? C18 H18 0.9500 . ? C19 C20 1.394(11) . ? C20 H20 0.9500 . ? C25 C26 1.384(13) . ? C25 H25 0.9500 . ? C26 C27 1.359(14) . ? C26 H26 0.9500 . ? C27 C35 1.411(13) . ? C27 H27 0.9500 . ? C28 C29 1.331(14) . ? C28 C35 1.441(13) . ? C28 H28 0.9500 . ? C29 C34 1.462(12) . ? C29 H29 0.9500 . ? C30 C31 1.370(13) . ? C30 C34 1.398(12) . ? C30 H30 0.9500 . ? C31 C32 1.397(12) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.404(11) . ? C33 C36 1.432(11) . ? C35 C36 1.394(11) . ? C37 C38 1.421(15) . ? C37 H37 0.9500 . ? C38 C39 1.325(17) . ? C38 H38 0.9500 . ? C39 C47 1.378(15) . ? C39 H39 0.9500 . ? C40 C41 1.353(17) . ? C40 C47 1.399(16) . ? C40 H40 0.9500 . ? C41 C46 1.414(15) . ? C41 H41 0.9500 . ? C42 C43 1.332(18) . ? C42 C46 1.403(17) . ? C42 H42 0.9500 . ? C43 C44 1.40(2) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.403(16) . ? C45 C48 1.433(14) . ? C47 C48 1.447(12) . ? C49 C50 1.399(16) . ? C49 H49 0.9500 . ? C50 C51 1.376(17) . ? C50 H50 0.9500 . ? C51 C59 1.401(13) . ? C51 H51 0.9500 . ? C52 C53 1.323(15) . ? C52 C59 1.454(14) . ? C52 H52 0.9500 . ? C53 C58 1.413(13) . ? C53 H53 0.9500 . ? C54 C55 1.337(16) . ? C54 C58 1.410(14) . ? C54 H54 0.9500 . ? C55 C56 1.407(15) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.421(12) . ? C57 C60 1.426(12) . ? C59 C60 1.376(13) . ? C61 C62 1.355(18) . ? C61 H61 0.9500 . ? C62 C63 1.374(17) . ? C62 H62 0.9500 . ? C63 C71 1.381(18) . ? C63 H63 0.9500 . ? C64 C65 1.334(18) . ? C64 C71 1.455(15) . ? C64 H64 0.9500 . ? C65 C70 1.381(18) . ? C65 H65 0.9500 . ? C66 C67 1.320(18) . ? C66 C70 1.403(17) . ? C66 H66 0.9500 . ? C67 C68 1.371(16) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C72 1.404(16) . ? C69 C70 1.429(13) . ? C71 C72 1.382(17) . ? O001 O002 0.944(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Gd1 O4 80.40(18) . . ? O3 Gd1 O1 141.90(18) . . ? O4 Gd1 O1 72.24(17) . . ? O3 Gd1 O2 72.92(17) . . ? O4 Gd1 O2 80.77(18) . . ? O1 Gd1 O2 76.88(18) . . ? O3 Gd1 O5 138.0(2) . . ? O4 Gd1 O5 141.4(2) . . ? O1 Gd1 O5 74.7(2) . . ? O2 Gd1 O5 110.4(2) . . ? O3 Gd1 O6 77.94(19) . . ? O4 Gd1 O6 118.27(18) . . ? O1 Gd1 O6 138.58(19) . . ? O2 Gd1 O6 141.77(18) . . ? O5 Gd1 O6 76.3(2) . . ? O3 Gd1 O7 123.90(18) . . ? O4 Gd1 O7 75.11(18) . . ? O1 Gd1 O7 74.13(18) . . ? O2 Gd1 O7 146.70(18) . . ? O5 Gd1 O7 77.2(2) . . ? O6 Gd1 O7 71.12(19) . . ? O3 Gd1 O8 72.75(18) . . ? O4 Gd1 O8 147.41(18) . . ? O1 Gd1 O8 120.14(17) . . ? O2 Gd1 O8 74.03(18) . . ? O5 Gd1 O8 68.6(2) . . ? O6 Gd1 O8 74.07(18) . . ? O7 Gd1 O8 135.73(18) . . ? O9 S1 O10 118.1(3) . . ? O9 S1 C1 110.3(3) . . ? O10 S1 C1 106.8(3) . . ? O9 S1 C2 109.6(3) . . ? O10 S1 C2 105.5(3) . . ? C1 S1 C2 105.8(3) . . ? O11 S2 O12 116.0(3) . . ? O11 S2 C6 107.3(3) . . ? O12 S2 C6 106.4(3) . . ? O11 S2 C7 109.2(3) . . ? O12 S2 C7 106.4(4) . . ? C6 S2 C7 111.6(3) . . ? O14 S3 O13 118.0(4) . . ? O14 S3 C12 107.8(4) . . ? O13 S3 C12 107.1(4) . . ? O14 S3 C11 111.2(4) . . ? O13 S3 C11 107.4(4) . . ? C12 S3 C11 104.4(4) . . ? O16 S4 O15 116.3(3) . . ? O16 S4 C17 107.6(3) . . ? O15 S4 C17 108.4(3) . . ? O16 S4 C16 105.3(3) . . ? O15 S4 C16 106.5(3) . . ? C17 S4 C16 112.9(3) . . ? O18B S5 O19A 141.4(9) . . ? O18B S5 O19B 117.8(9) . . ? O19A S5 O19B 42.8(10) . . ? O18B S5 O17A 60.1(10) . . ? O19A S5 O17A 115.1(13) . . ? O19B S5 O17A 146.4(9) . . ? O18B S5 O17B 110.8(9) . . ? O19A S5 O17B 67.9(11) . . ? O19B S5 O17B 110.2(9) . . ? O17A S5 O17B 52.3(10) . . ? O18B S5 O18A 48.4(9) . . ? O19A S5 O18A 110.2(12) . . ? O19B S5 O18A 71.8(11) . . ? O17A S5 O18A 106.5(12) . . ? O17B S5 O18A 146.2(9) . . ? O18B S5 C19 107.1(6) . . ? O19A S5 C19 110.5(8) . . ? O19B S5 C19 105.5(6) . . ? O17A S5 C19 106.8(7) . . ? O17B S5 C19 104.4(6) . . ? O18A S5 C19 107.5(7) . . ? O20 S6 O21 113.3(4) . . ? O20 S6 O22 113.4(4) . . ? O21 S6 O22 110.6(4) . . ? O20 S6 C4 105.7(4) . . ? O21 S6 C4 106.2(4) . . ? O22 S6 C4 107.0(3) . . ? O23 S7 O25 111.9(5) . . ? O23 S7 O24 112.3(6) . . ? O25 S7 O24 113.8(6) . . ? O23 S7 C9 105.7(4) . . ? O25 S7 C9 106.3(5) . . ? O24 S7 C9 106.1(4) . . ? O27A S8 O28B 89.0(14) . . ? O27A S8 O26B 128.2(16) . . ? O28B S8 O26B 116.4(10) . . ? O27A S8 O27B 23.7(16) . . ? O28B S8 O27B 112.3(10) . . ? O26B S8 O27B 110.7(10) . . ? O27A S8 O28A 119.0(16) . . ? O28B S8 O28A 36.1(11) . . ? O26B S8 O28A 81.4(14) . . ? O27B S8 O28A 138.5(11) . . ? O27A S8 O26A 107.2(17) . . ? O28B S8 O26A 137.1(12) . . ? O26B S8 O26A 25.3(11) . . ? O27B S8 O26A 86.7(13) . . ? O28A S8 O26A 105.0(15) . . ? O27A S8 C14 109.8(13) . . ? O28B S8 C14 106.2(6) . . ? O26B S8 C14 105.2(7) . . ? O27B S8 C14 105.0(8) . . ? O28A S8 C14 109.8(9) . . ? O26A S8 C14 105.0(10) . . ? C25 N1 C36 121.8(7) . . ? C32 N2 C33 116.8(7) . . ? C48 N3 C37 122.2(9) . . ? C44 N4 C45 116.1(11) . . ? C49 N5 C60 122.0(9) . . ? C56 N6 C57 117.5(8) . . ? C61 N7 C72 116.9(11) . . ? C68 N8 C69 121.4(10) . . ? C21 O1 Gd1 133.5(5) . . ? C22 O2 Gd1 152.4(5) . . ? C23 O3 Gd1 127.9(4) . . ? C24 O4 Gd1 149.1(5) . . ? C20 C1 C21 122.7(7) . . ? C20 C1 S1 115.4(6) . . ? C21 C1 S1 121.9(6) . . ? C3 C2 C22 123.3(7) . . ? C3 C2 S1 118.7(6) . . ? C22 C2 S1 117.9(5) . . ? C2 C3 C4 120.1(7) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 119.6(7) . . ? C5 C4 S6 120.6(6) . . ? C3 C4 S6 119.8(6) . . ? C4 C5 C6 120.5(7) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C22 122.3(7) . . ? C5 C6 S2 116.4(5) . . ? C22 C6 S2 120.6(6) . . ? C8 C7 C23 123.0(7) . . ? C8 C7 S2 116.0(6) . . ? C23 C7 S2 120.7(6) . . ? C9 C8 C7 119.2(7) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C10 C9 C8 120.5(7) . . ? C10 C9 S7 118.9(6) . . ? C8 C9 S7 120.6(6) . . ? C9 C10 C11 119.9(7) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C23 123.5(7) . . ? C10 C11 S3 114.9(6) . . ? C23 C11 S3 121.5(6) . . ? C13 C12 C24 123.8(7) . . ? C13 C12 S3 119.7(6) . . ? C24 C12 S3 116.3(6) . . ? C12 C13 C14 119.0(7) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C15 C14 C13 119.7(7) . . ? C15 C14 S8 121.3(7) . . ? C13 C14 S8 118.9(6) . . ? C16 C15 C14 120.6(7) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C24 122.0(7) . . ? C15 C16 S4 117.1(6) . . ? C24 C16 S4 120.0(6) . . ? C18 C17 C21 122.5(7) . . ? C18 C17 S4 115.3(6) . . ? C21 C17 S4 121.5(6) . . ? C19 C18 C17 120.5(7) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 119.4(7) . . ? C18 C19 S5 121.8(6) . . ? C20 C19 S5 118.8(6) . . ? C1 C20 C19 121.1(7) . . ? C1 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? O1 C21 C1 123.4(7) . . ? O1 C21 C17 123.0(7) . . ? C1 C21 C17 113.6(7) . . ? O2 C22 C2 123.0(6) . . ? O2 C22 C6 122.8(7) . . ? C2 C22 C6 114.2(6) . . ? O3 C23 C11 123.1(7) . . ? O3 C23 C7 123.0(7) . . ? C11 C23 C7 113.8(7) . . ? O4 C24 C12 122.1(7) . . ? O4 C24 C16 123.1(7) . . ? C12 C24 C16 114.7(7) . . ? N1 C25 C26 119.9(9) . . ? N1 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 120.3(9) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C35 120.3(8) . . ? C26 C27 H27 119.9 . . ? C35 C27 H27 119.9 . . ? C29 C28 C35 121.8(8) . . ? C29 C28 H28 119.1 . . ? C35 C28 H28 119.1 . . ? C28 C29 C34 120.9(8) . . ? C28 C29 H29 119.5 . . ? C34 C29 H29 119.5 . . ? C31 C30 C34 119.7(8) . . ? C31 C30 H30 120.2 . . ? C34 C30 H30 120.2 . . ? C30 C31 C32 118.7(8) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? N2 C32 C31 123.8(8) . . ? N2 C32 H32 118.1 . . ? C31 C32 H32 118.1 . . ? N2 C33 C34 124.5(7) . . ? N2 C33 C36 117.7(7) . . ? C34 C33 C36 117.8(7) . . ? C30 C34 C33 116.5(8) . . ? C30 C34 C29 124.2(8) . . ? C33 C34 C29 119.3(8) . . ? C36 C35 C27 118.4(8) . . ? C36 C35 C28 117.4(8) . . ? C27 C35 C28 124.1(8) . . ? N1 C36 C35 119.4(8) . . ? N1 C36 C33 117.8(7) . . ? C35 C36 C33 122.7(8) . . ? N3 C37 C38 118.8(12) . . ? N3 C37 H37 120.6 . . ? C38 C37 H37 120.6 . . ? C39 C38 C37 120.2(11) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C47 121.7(10) . . ? C38 C39 H39 119.1 . . ? C47 C39 H39 119.1 . . ? C41 C40 C47 121.3(9) . . ? C41 C40 H40 119.3 . . ? C47 C40 H40 119.3 . . ? C40 C41 C46 121.8(12) . . ? C40 C41 H41 119.1 . . ? C46 C41 H41 119.1 . . ? C43 C42 C46 121.9(14) . . ? C43 C42 H42 119.1 . . ? C46 C42 H42 119.1 . . ? C42 C43 C44 117.9(13) . . ? C42 C43 H43 121.0 . . ? C44 C43 H43 121.0 . . ? N4 C44 C43 124.5(12) . . ? N4 C44 H44 117.8 . . ? C43 C44 H44 117.8 . . ? N4 C45 C46 124.5(10) . . ? N4 C45 C48 115.9(10) . . ? C46 C45 C48 119.5(9) . . ? C42 C46 C45 115.1(11) . . ? C42 C46 C41 125.4(12) . . ? C45 C46 C41 119.5(11) . . ? C39 C47 C40 124.5(9) . . ? C39 C47 C48 116.5(11) . . ? C40 C47 C48 119.0(10) . . ? N3 C48 C45 120.5(8) . . ? N3 C48 C47 120.6(9) . . ? C45 C48 C47 118.9(10) . . ? N5 C49 C50 120.2(10) . . ? N5 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C51 C50 C49 118.4(9) . . ? C51 C50 H50 120.8 . . ? C49 C50 H50 120.8 . . ? C50 C51 C59 121.0(10) . . ? C50 C51 H51 119.5 . . ? C59 C51 H51 119.5 . . ? C53 C52 C59 121.8(9) . . ? C53 C52 H52 119.1 . . ? C59 C52 H52 119.1 . . ? C52 C53 C58 121.2(9) . . ? C52 C53 H53 119.4 . . ? C58 C53 H53 119.4 . . ? C55 C54 C58 119.9(9) . . ? C55 C54 H54 120.1 . . ? C58 C54 H54 120.1 . . ? C54 C55 C56 120.0(10) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? N6 C56 C55 122.8(10) . . ? N6 C56 H56 118.6 . . ? C55 C56 H56 118.6 . . ? N6 C57 C58 123.4(8) . . ? N6 C57 C60 119.3(8) . . ? C58 C57 C60 117.4(8) . . ? C54 C58 C53 123.7(9) . . ? C54 C58 C57 116.4(9) . . ? C53 C58 C57 119.9(8) . . ? C60 C59 C51 118.9(9) . . ? C60 C59 C52 117.2(8) . . ? C51 C59 C52 123.9(9) . . ? N5 C60 C59 119.6(8) . . ? N5 C60 C57 118.0(8) . . ? C59 C60 C57 122.5(8) . . ? N7 C61 C62 123.6(11) . . ? N7 C61 H61 118.2 . . ? C62 C61 H61 118.2 . . ? C61 C62 C63 118.6(13) . . ? C61 C62 H62 120.7 . . ? C63 C62 H62 120.7 . . ? C62 C63 C71 120.1(14) . . ? C62 C63 H63 119.9 . . ? C71 C63 H63 119.9 . . ? C65 C64 C71 121.1(13) . . ? C65 C64 H64 119.5 . . ? C71 C64 H64 119.5 . . ? C64 C65 C70 121.4(10) . . ? C64 C65 H65 119.3 . . ? C70 C65 H65 119.3 . . ? C67 C66 C70 120.6(10) . . ? C67 C66 H66 119.7 . . ? C70 C66 H66 119.7 . . ? C66 C67 C68 121.2(13) . . ? C66 C67 H67 119.4 . . ? C68 C67 H67 119.4 . . ? N8 C68 C67 120.4(14) . . ? N8 C68 H68 119.8 . . ? C67 C68 H68 119.8 . . ? N8 C69 C72 118.5(9) . . ? N8 C69 C70 118.7(11) . . ? C72 C69 C70 122.7(12) . . ? C65 C70 C66 124.7(10) . . ? C65 C70 C69 117.7(11) . . ? C66 C70 C69 117.6(12) . . ? C63 C71 C72 116.6(11) . . ? C63 C71 C64 123.5(14) . . ? C72 C71 C64 119.9(12) . . ? N7 C72 C71 124.1(11) . . ? N7 C72 C69 118.8(12) . . ? C71 C72 C69 117.1(10) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.773 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.203 ###END data_2 _database_code_depnum_ccdc_archive 'CCDC 665653' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'H5 Sm (C24H8O24S8) (C12H8N2)4 (H2O)7.90' _chemical_melting_point ? _chemical_formula_moiety 'H5 Sm [C24H8O24S8] [C12H8N2]4 [H2O]7.90' _chemical_formula_sum 'C72 H60.80 N8 O31.90 S8 Sm' _chemical_formula_weight 1955.24 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' Sm Sm -0.1638 3.4418 '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' _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 14.3503(18) _cell_length_b 17.955(2) _cell_length_c 19.182(2) _cell_angle_alpha 112.135(2) _cell_angle_beta 92.414(2) _cell_angle_gamma 97.789(2) _cell_volume 4512.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4567 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 23.87 _exptl_crystal_description tube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1988 _exptl_absorpt_coefficient_mu 0.918 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6844 _exptl_absorpt_correction_T_max 0.9260 _exptl_absorpt_process_details ; SADABS, Sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 AXS Apex CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 29922 _diffrn_reflns_av_R_equivalents 0.0908 _diffrn_reflns_av_sigmaI/netI 0.1588 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15599 _reflns_number_gt 9586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (1998)' _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. All the non-hydrogen atoms were refined anisotropically except some isolated molecular atoms. All the oxygen atoms of the solvent water molecules were refined without hydrogen atoms. The oxygen atoms of two sulfonate groups (O17-O19, O26-O28) were refined with disordered positions and the same displacement parameters for all oxygen atoms on one sulfonate group. ; _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^)+(0.1660P)^2^+1.0488P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15599 _refine_ls_number_parameters 1072 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1657 _refine_ls_R_factor_gt 0.1058 _refine_ls_wR_factor_ref 0.2957 _refine_ls_wR_factor_gt 0.2649 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.059 _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 Sm1 Sm 0.032131(15) 0.755759(13) 0.019395(13) 0.02058(6) Uani 1 1 d . . . S1 S 0.08402(7) 1.01393(6) 0.09253(7) 0.0243(3) Uani 1 1 d . . . S2 S -0.22444(7) 0.83158(6) 0.14617(7) 0.0239(3) Uani 1 1 d . . . S3 S 0.00331(8) 0.59564(6) 0.12215(7) 0.0268(3) Uani 1 1 d . . . S4 S 0.32011(7) 0.81654(6) 0.15584(7) 0.0255(3) Uani 1 1 d . . . S5 S 0.33713(10) 1.13504(8) 0.33794(7) 0.0403(4) Uani 1 1 d . . . S6 S -0.20711(8) 1.15737(6) 0.22910(7) 0.0282(3) Uani 1 1 d . . . S7 S -0.15827(10) 0.73452(9) 0.37702(8) 0.0463(5) Uani 1 1 d . . . S8 S 0.32067(11) 0.59626(7) 0.28901(8) 0.0520(5) Uani 1 1 d . . . N1 N -0.3767(3) 1.15320(19) 0.0584(2) 0.0304(12) Uani 1 1 d . . . N2 N -0.3117(3) 1.0111(2) 0.0120(2) 0.0273(12) Uani 1 1 d . . . N3 N 0.1040(3) 1.0604(3) 0.4572(2) 0.0441(15) Uani 1 1 d . . . N4 N 0.1443(3) 0.9915(3) 0.5566(2) 0.0467(16) Uani 1 1 d . . . N5 N 0.3437(3) 0.4374(2) 0.0809(3) 0.0426(15) Uani 1 1 d . . . N6 N 0.5294(3) 0.4509(2) 0.1310(3) 0.0542(17) Uani 1 1 d . . . N7 N -0.3644(3) 1.0296(3) 0.5577(2) 0.0510(17) Uani 1 1 d . . . N8 N -0.3821(3) 0.8700(3) 0.4680(3) 0.0528(17) Uani 1 1 d . . . O1 O 0.1687(2) 0.85586(15) 0.06084(16) 0.0220(9) Uani 1 1 d . A . O2 O -0.0195(2) 0.86691(16) 0.11134(16) 0.0238(9) Uani 1 1 d . . . O3 O -0.0988(2) 0.70472(16) 0.06598(16) 0.0229(9) Uani 1 1 d . . . O4 O 0.1062(2) 0.74989(16) 0.12692(16) 0.0266(9) Uani 1 1 d . B . O5 O 0.0702(2) 0.7907(2) -0.0882(2) 0.0522(11) Uani 1 1 d . . . O6 O -0.0287(2) 0.62848(17) -0.09067(18) 0.0332(10) Uani 1 1 d . . . O7 O 0.1679(2) 0.68262(17) -0.02751(18) 0.0336(10) Uani 1 1 d . . . O8 O -0.1146(2) 0.77924(16) -0.04229(17) 0.0267(9) Uani 1 1 d . . . O9 O 0.0725(2) 0.9550(2) 0.01692(19) 0.0437(11) Uani 1 1 d . . . O10 O 0.1083(2) 1.09917(17) 0.10517(18) 0.0306(10) Uani 1 1 d . . . O11 O -0.2481(2) 0.78857(17) 0.06561(17) 0.0265(10) Uani 1 1 d . . . O12 O -0.3038(2) 0.84895(19) 0.18947(18) 0.0327(10) Uani 1 1 d . . . O13 O -0.0236(2) 0.52614(17) 0.1413(2) 0.0366(11) Uani 1 1 d . . . O14 O 0.0063(3) 0.5856(3) 0.0461(2) 0.0646(15) Uani 1 1 d . . . O15 O 0.3201(2) 0.77817(17) 0.07596(17) 0.0271(9) Uani 1 1 d . . . O16 O 0.4109(2) 0.84101(17) 0.20033(18) 0.0311(10) Uani 1 1 d . . . O17A O 0.3969(9) 1.1861(7) 0.3147(6) 0.0647(14) Uani 0.360(4) 1 d P A 1 O18A O 0.4141(9) 1.1096(7) 0.3769(6) 0.0647(14) Uani 0.360(4) 1 d P A 1 O19A O 0.2838(9) 1.1619(7) 0.3927(6) 0.0647(14) Uani 0.360(4) 1 d P A 1 O17B O 0.3119(5) 1.2027(4) 0.3211(4) 0.0647(14) Uani 0.640(4) 1 d P A 2 O18B O 0.4366(5) 1.1347(4) 0.3399(4) 0.0647(14) Uani 0.640(4) 1 d P A 2 O19B O 0.2985(5) 1.1245(4) 0.4015(4) 0.0647(14) Uani 0.640(4) 1 d P A 2 O20 O -0.2927(2) 1.13176(18) 0.25809(19) 0.0409(11) Uani 1 1 d . . . O21 O -0.1382(3) 1.2190(2) 0.2856(2) 0.0472(13) Uani 1 1 d . . . O22 O -0.2263(2) 1.18174(17) 0.16555(18) 0.0330(10) Uani 1 1 d . . . O23 O -0.2311(3) 0.6666(2) 0.3658(2) 0.0558(14) Uani 1 1 d . . . O24 O -0.0703(3) 0.7276(3) 0.4118(2) 0.0684(15) Uani 1 1 d . . . O25 O -0.1895(3) 0.8128(2) 0.4165(2) 0.0592(15) Uani 1 1 d . . . O26A O 0.4179(6) 0.5881(5) 0.2560(4) 0.0663(11) Uani 0.503(4) 1 d P B 1 O27A O 0.2699(6) 0.5163(5) 0.2707(5) 0.0663(11) Uani 0.503(4) 1 d P B 1 O28A O 0.3376(6) 0.6438(5) 0.3624(5) 0.0663(11) Uani 0.503(4) 1 d P B 1 O26B O 0.4140(6) 0.6337(5) 0.3037(5) 0.0663(11) Uani 0.497(4) 1 d P B 2 O27B O 0.2963(6) 0.5078(5) 0.2428(5) 0.0663(11) Uani 0.497(4) 1 d P B 2 O28B O 0.2752(6) 0.6259(5) 0.3628(5) 0.0663(11) Uani 0.497(4) 1 d P B 2 C1 C 0.1706(3) 0.9920(2) 0.1468(2) 0.0218(12) Uani 1 1 d U A . C2 C -0.0214(3) 1.0069(2) 0.1369(2) 0.0187(11) Uani 1 1 d U . . C3 C -0.0629(3) 1.0754(2) 0.1655(2) 0.0211(12) Uani 1 1 d U . . H3 H -0.0329 1.1260 0.1658 0.025 Uiso 1 1 calc R . . C4 C -0.1511(3) 1.0686(2) 0.1943(2) 0.0245(13) Uani 1 1 d . . . C5 C -0.1950(3) 0.9952(2) 0.1908(2) 0.0218(12) Uani 1 1 d U . . H5 H -0.2554 0.9913 0.2088 0.026 Uiso 1 1 calc R . . C6 C -0.1537(3) 0.9258(2) 0.1615(2) 0.0215(12) Uani 1 1 d . . . C7 C -0.1619(3) 0.7749(2) 0.1835(2) 0.0211(12) Uani 1 1 d U . . C8 C -0.1741(3) 0.7825(3) 0.2568(2) 0.0272(14) Uani 1 1 d . . . H8 H -0.2072 0.8233 0.2875 0.033 Uiso 1 1 calc R . . C9 C -0.1388(3) 0.7316(3) 0.2859(3) 0.0343(16) Uani 1 1 d . . . C10 C -0.0856(3) 0.6725(3) 0.2413(3) 0.0249(14) Uani 1 1 d . . . H10 H -0.0610 0.6368 0.2606 0.030 Uiso 1 1 calc R . . C11 C -0.0709(3) 0.6683(2) 0.1706(3) 0.0240(13) Uani 1 1 d . . . C12 C 0.1187(3) 0.6423(2) 0.1688(2) 0.0271(13) Uani 1 1 d . B . C13 C 0.1650(3) 0.6078(3) 0.2070(3) 0.0298(15) Uani 1 1 d . . . H13 H 0.1337 0.5615 0.2143 0.036 Uiso 1 1 calc R B . C14 C 0.2593(4) 0.6392(2) 0.2365(2) 0.0309(14) Uani 1 1 d . B . C15 C 0.3047(3) 0.7086(3) 0.2247(3) 0.0291(14) Uani 1 1 d . . . H15 H 0.3688 0.7311 0.2436 0.035 Uiso 1 1 calc R B . C16 C 0.2524(3) 0.7433(2) 0.1843(2) 0.0258(13) Uani 1 1 d . B . C17 C 0.2679(3) 0.9067(2) 0.1761(2) 0.0253(13) Uani 1 1 d . A . C18 C 0.3075(3) 0.9713(3) 0.2419(3) 0.0328(14) Uani 1 1 d . . . H18 H 0.3519 0.9632 0.2755 0.039 Uiso 1 1 calc R A . C19 C 0.2823(3) 1.0482(3) 0.2590(3) 0.0270(14) Uani 1 1 d . A . C20 C 0.2113(3) 1.0567(2) 0.2110(3) 0.0258(13) Uani 1 1 d U . . H20 H 0.1911 1.1080 0.2232 0.031 Uiso 1 1 calc R A . C21 C 0.1997(3) 0.9125(2) 0.1228(2) 0.0225(12) Uani 1 1 d . . . C22 C -0.0623(3) 0.9296(2) 0.1329(2) 0.0198(12) Uani 1 1 d . . . C23 C -0.1090(3) 0.7137(2) 0.1336(2) 0.0197(12) Uani 1 1 d U . . C24 C 0.1562(3) 0.7148(3) 0.1577(3) 0.0266(14) Uani 1 1 d . . . C25 C -0.4026(3) 1.2274(3) 0.0889(3) 0.0319(15) Uani 1 1 d . . . H25 H -0.3713 1.2677 0.1349 0.038 Uiso 1 1 calc R . . C26 C -0.4792(3) 1.2428(3) 0.0491(3) 0.0457(17) Uani 1 1 d . . . H26 H -0.5008 1.2938 0.0689 0.055 Uiso 1 1 calc R . . C27 C -0.5211(3) 1.1842(3) -0.0172(3) 0.0413(16) Uani 1 1 d . . . H27 H -0.5716 1.1949 -0.0437 0.050 Uiso 1 1 calc R . . C28 C -0.5321(4) 1.0433(3) -0.1183(3) 0.0413(16) Uani 1 1 d U . . H28 H -0.5816 1.0518 -0.1475 0.050 Uiso 1 1 calc R . . C29 C -0.5023(4) 0.9739(3) -0.1429(3) 0.0418(18) Uani 1 1 d . . . H29 H -0.5313 0.9323 -0.1891 0.050 Uiso 1 1 calc R . . C30 C -0.3928(3) 0.8834(3) -0.1247(3) 0.0360(16) Uani 1 1 d . . . H30 H -0.4193 0.8406 -0.1710 0.043 Uiso 1 1 calc R . . C31 C -0.3219(4) 0.8726(3) -0.0798(3) 0.0345(16) Uani 1 1 d . . . H31 H -0.2994 0.8221 -0.0943 0.041 Uiso 1 1 calc R . . C32 C -0.2841(3) 0.9381(2) -0.0126(3) 0.0309(14) Uani 1 1 d . . . H32 H -0.2354 0.9300 0.0177 0.037 Uiso 1 1 calc R . . C33 C -0.3836(3) 1.0180(2) -0.0342(2) 0.0244(13) Uani 1 1 d . . . C34 C -0.4245(4) 0.9581(3) -0.1006(3) 0.0331(15) Uani 1 1 d . . . C35 C -0.4916(3) 1.1089(3) -0.0471(3) 0.0304(14) Uani 1 1 d . . . C36 C -0.4174(3) 1.0945(2) -0.0074(3) 0.0280(14) Uani 1 1 d . . . C37 C 0.0806(4) 1.1014(5) 0.4154(3) 0.065(2) Uani 1 1 d . . . H37 H 0.0797 1.1583 0.4370 0.078 Uiso 1 1 calc R . . C38 C 0.0568(4) 1.0538(4) 0.3355(3) 0.061(2) Uani 1 1 d . . . H38 H 0.0391 1.0794 0.3028 0.073 Uiso 1 1 calc R . . C39 C 0.0598(4) 0.9719(4) 0.3068(3) 0.051(2) Uani 1 1 d . . . H39 H 0.0440 0.9406 0.2543 0.061 Uiso 1 1 calc R . . C40 C 0.0893(4) 0.8503(4) 0.3266(4) 0.060(2) Uani 1 1 d . . . H40 H 0.0746 0.8176 0.2742 0.072 Uiso 1 1 calc R . . C41 C 0.1134(4) 0.8147(4) 0.3735(4) 0.062(2) Uani 1 1 d . . . H41 H 0.1201 0.7588 0.3535 0.075 Uiso 1 1 calc R . . C42 C 0.1514(5) 0.8258(4) 0.5037(4) 0.073(2) Uani 1 1 d . . . H42 H 0.1554 0.7694 0.4862 0.087 Uiso 1 1 calc R . . C43 C 0.1680(4) 0.8738(4) 0.5800(4) 0.069(2) Uani 1 1 d . . . H43 H 0.1821 0.8514 0.6160 0.083 Uiso 1 1 calc R . . C44 C 0.1631(4) 0.9580(4) 0.6025(3) 0.054(2) Uani 1 1 d . . . H44 H 0.1746 0.9915 0.6549 0.065 Uiso 1 1 calc R . . C45 C 0.1284(4) 0.9436(3) 0.4817(3) 0.0444(18) Uani 1 1 d . . . C46 C 0.1289(4) 0.8600(4) 0.4527(3) 0.054(2) Uani 1 1 d . . . C47 C 0.0847(3) 0.9364(4) 0.3525(3) 0.052(2) Uani 1 1 d . . . C48 C 0.1053(4) 0.9805(3) 0.4310(3) 0.0426(18) Uani 1 1 d . . . C49 C 0.2545(4) 0.4263(3) 0.0534(4) 0.055(2) Uani 1 1 d . . . H49 H 0.2138 0.3785 0.0503 0.066 Uiso 1 1 calc R . . C50 C 0.2189(4) 0.4782(3) 0.0301(3) 0.0540(18) Uani 1 1 d U . . H50 H 0.1538 0.4686 0.0125 0.065 Uiso 1 1 calc R . . C51 C 0.2779(4) 0.5466(3) 0.0318(3) 0.0546(18) Uani 1 1 d . . . H51 H 0.2543 0.5842 0.0145 0.066 Uiso 1 1 calc R . . C52 C 0.4426(4) 0.6308(3) 0.0658(3) 0.0498(19) Uani 1 1 d . . . H52 H 0.4226 0.6707 0.0499 0.060 Uiso 1 1 calc R . . C53 C 0.5325(5) 0.6400(3) 0.0936(3) 0.052(2) Uani 1 1 d . . . H53 H 0.5752 0.6864 0.0960 0.063 Uiso 1 1 calc R . . C54 C 0.6610(4) 0.5928(4) 0.1496(4) 0.071(3) Uani 1 1 d . . . H54 H 0.7055 0.6401 0.1570 0.085 Uiso 1 1 calc R . . C55 C 0.6866(5) 0.5281(4) 0.1685(4) 0.082(3) Uani 1 1 d . . . H55 H 0.7492 0.5309 0.1888 0.099 Uiso 1 1 calc R . . C56 C 0.6173(5) 0.4602(4) 0.1564(4) 0.081(3) Uani 1 1 d . . . H56 H 0.6364 0.4171 0.1679 0.098 Uiso 1 1 calc R . . C57 C 0.5009(4) 0.5122(3) 0.1134(3) 0.0407(17) Uani 1 1 d . . . C58 C 0.5668(4) 0.5835(3) 0.1194(3) 0.0390(17) Uani 1 1 d . . . C59 C 0.3755(3) 0.5599(3) 0.0600(3) 0.0371(16) Uani 1 1 d . . . C60 C 0.4050(3) 0.5037(3) 0.0834(3) 0.0332(16) Uani 1 1 d . . . C61 C -0.3598(4) 1.1075(4) 0.5990(3) 0.053(2) Uani 1 1 d . . . H61 H -0.3471 1.1251 0.6523 0.064 Uiso 1 1 calc R . . C62 C -0.3723(4) 1.1654(4) 0.5700(4) 0.068(3) Uani 1 1 d . . . H62 H -0.3686 1.2209 0.6028 0.081 Uiso 1 1 calc R . . C63 C -0.3900(5) 1.1423(4) 0.4940(4) 0.063(2) Uani 1 1 d . . . H63 H -0.3989 1.1814 0.4731 0.076 Uiso 1 1 calc R . . C64 C -0.4141(4) 1.0297(4) 0.3658(3) 0.0508(19) Uani 1 1 d . . . H64 H -0.4223 1.0669 0.3424 0.061 Uiso 1 1 calc R . . C65 C -0.4206(3) 0.9479(3) 0.3216(3) 0.0415(18) Uani 1 1 d . . . H65 H -0.4316 0.9290 0.2681 0.050 Uiso 1 1 calc R . . C66 C -0.4211(3) 0.8104(4) 0.3157(3) 0.0457(19) Uani 1 1 d . . . H66 H -0.4340 0.7894 0.2622 0.055 Uiso 1 1 calc R . . C67 C -0.4130(4) 0.7574(4) 0.3513(3) 0.061(2) Uani 1 1 d . . . H67 H -0.4214 0.7002 0.3230 0.073 Uiso 1 1 calc R . . C68 C -0.3928(4) 0.7884(4) 0.4277(4) 0.065(2) Uani 1 1 d . . . H68 H -0.3862 0.7527 0.4530 0.078 Uiso 1 1 calc R . . C69 C -0.3907(3) 0.9246(3) 0.4333(3) 0.0397(15) Uani 1 1 d U . . C70 C -0.4107(3) 0.8935(3) 0.3562(3) 0.0437(19) Uani 1 1 d . . . C71 C -0.3951(4) 1.0594(4) 0.4466(3) 0.052(2) Uani 1 1 d . . . C72 C -0.3812(4) 1.0084(3) 0.4799(3) 0.0429(18) Uani 1 1 d . . . O001 O 0.2344(16) 0.4536(12) 0.4817(12) 0.0485(12) Uiso 0.172(6) 1 d P . . O002 O 0.3230(3) 0.4757(2) 0.4859(3) 0.0485(12) Uiso 0.828(6) 1 d P . . O003 O 0.2444(2) 0.53831(18) 0.54585(18) 0.0319(9) Uiso 0.966(7) 1 d P . . O004 O 0.3442(4) 0.3287(3) 0.1458(3) 0.0839(15) Uiso 1 1 d . . . O005 O 0.1977(4) 0.6444(3) -0.1772(3) 0.0871(18) Uiso 0.927(9) 1 d P . . 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 Sm1 0.01082(9) 0.02627(9) 0.02791(11) 0.01111(8) 0.00499(8) 0.01104(7) S1 0.0103(5) 0.0358(5) 0.0362(6) 0.0215(4) 0.0049(4) 0.0118(4) S2 0.0080(5) 0.0335(5) 0.0325(6) 0.0139(4) 0.0022(4) 0.0081(4) S3 0.0195(5) 0.0292(5) 0.0340(6) 0.0117(4) 0.0060(5) 0.0122(4) S4 0.0119(5) 0.0352(5) 0.0390(6) 0.0214(4) 0.0060(4) 0.0136(4) S5 0.0445(7) 0.0484(6) 0.0299(7) 0.0114(5) 0.0020(6) 0.0247(5) S6 0.0215(5) 0.0366(5) 0.0309(6) 0.0116(4) 0.0075(5) 0.0216(4) S7 0.0352(7) 0.0814(8) 0.0309(6) 0.0269(6) 0.0100(6) 0.0204(6) S8 0.0557(8) 0.0444(6) 0.0642(8) 0.0324(5) -0.0214(7) 0.0096(6) N1 0.0151(18) 0.0319(15) 0.060(2) 0.0346(14) 0.0040(17) 0.0070(14) N2 0.0134(18) 0.0429(17) 0.0331(19) 0.0221(14) 0.0042(16) 0.0063(15) N3 0.025(2) 0.084(3) 0.034(2) 0.0296(19) 0.0183(18) 0.018(2) N4 0.014(2) 0.098(3) 0.022(2) 0.019(2) 0.0037(17) 0.005(2) N5 0.022(2) 0.0296(18) 0.067(3) 0.0112(18) -0.012(2) 0.0018(17) N6 0.025(2) 0.040(2) 0.098(3) 0.031(2) -0.018(2) 0.0002(18) N7 0.020(2) 0.087(3) 0.033(2) 0.013(2) 0.004(2) -0.006(2) N8 0.034(2) 0.083(3) 0.033(2) 0.012(2) 0.000(2) 0.014(2) O1 0.0128(14) 0.0258(12) 0.0288(15) 0.0099(11) 0.0015(12) 0.0095(11) O2 0.0128(14) 0.0302(13) 0.0324(16) 0.0138(11) 0.0060(12) 0.0106(11) O3 0.0209(15) 0.0322(13) 0.0148(14) 0.0085(11) 0.0022(12) 0.0031(12) O4 0.0147(14) 0.0437(13) 0.0385(15) 0.0299(11) 0.0105(12) 0.0180(11) O5 0.0276(17) 0.0875(17) 0.082(2) 0.0690(13) 0.0194(16) 0.0306(14) O6 0.0336(17) 0.0376(14) 0.0322(17) 0.0122(12) 0.0037(14) 0.0220(13) O7 0.0256(16) 0.0434(13) 0.0481(17) 0.0295(12) 0.0118(14) 0.0227(12) O8 0.0178(14) 0.0358(13) 0.0357(16) 0.0196(11) 0.0110(13) 0.0157(11) O9 0.0230(16) 0.0773(18) 0.0484(19) 0.0352(14) 0.0130(15) 0.0312(14) O10 0.0070(14) 0.0444(14) 0.0526(18) 0.0307(12) 0.0060(13) 0.0076(12) O11 0.0083(14) 0.0399(14) 0.0313(16) 0.0134(12) 0.0010(13) 0.0056(12) O12 0.0129(14) 0.0576(16) 0.0385(17) 0.0260(13) 0.0158(13) 0.0157(13) O13 0.0213(16) 0.0293(14) 0.060(2) 0.0154(14) 0.0066(16) 0.0123(12) O14 0.036(2) 0.110(3) 0.050(2) 0.027(2) 0.0017(18) 0.0338(19) O15 0.0168(14) 0.0383(13) 0.0344(16) 0.0180(12) 0.0100(13) 0.0176(11) O16 0.0122(14) 0.0401(14) 0.0452(18) 0.0190(12) -0.0034(13) 0.0128(12) O17A 0.069(2) 0.067(2) 0.0449(19) 0.0100(16) -0.0101(18) 0.0072(18) O18A 0.069(2) 0.067(2) 0.0449(19) 0.0100(16) -0.0101(18) 0.0072(18) O19A 0.069(2) 0.067(2) 0.0449(19) 0.0100(16) -0.0101(18) 0.0072(18) O17B 0.069(2) 0.067(2) 0.0449(19) 0.0100(16) -0.0101(18) 0.0072(18) O18B 0.069(2) 0.067(2) 0.0449(19) 0.0100(16) -0.0101(18) 0.0072(18) O19B 0.069(2) 0.067(2) 0.0449(19) 0.0100(16) -0.0101(18) 0.0072(18) O20 0.0288(16) 0.0549(15) 0.059(2) 0.0330(14) 0.0287(15) 0.0311(13) O21 0.047(2) 0.0389(17) 0.041(2) -0.0019(15) -0.0115(18) 0.0146(16) O22 0.0285(16) 0.0430(13) 0.0434(17) 0.0265(12) 0.0106(14) 0.0273(12) O23 0.052(2) 0.072(2) 0.062(2) 0.0429(16) 0.0256(19) 0.0146(19) O24 0.047(2) 0.137(3) 0.0425(19) 0.0520(18) 0.0027(18) 0.034(2) O25 0.050(2) 0.086(2) 0.036(2) 0.0115(19) 0.0154(19) 0.025(2) O26A 0.059(2) 0.0869(15) 0.0737(19) 0.0510(12) -0.0079(16) 0.0252(15) O27A 0.059(2) 0.0869(15) 0.0737(19) 0.0510(12) -0.0079(16) 0.0252(15) O28A 0.059(2) 0.0869(15) 0.0737(19) 0.0510(12) -0.0079(16) 0.0252(15) O26B 0.059(2) 0.0869(15) 0.0737(19) 0.0510(12) -0.0079(16) 0.0252(15) O27B 0.059(2) 0.0869(15) 0.0737(19) 0.0510(12) -0.0079(16) 0.0252(15) O28B 0.059(2) 0.0869(15) 0.0737(19) 0.0510(12) -0.0079(16) 0.0252(15) C1 0.0117(18) 0.0336(17) 0.027(2) 0.0167(14) -0.0013(16) 0.0131(14) C2 0.0109(17) 0.0269(16) 0.0247(19) 0.0142(14) 0.0015(15) 0.0114(14) C3 0.0143(18) 0.0284(16) 0.027(2) 0.0148(14) -0.0022(16) 0.0125(14) C4 0.022(2) 0.0367(19) 0.022(2) 0.0143(16) 0.0011(18) 0.0173(17) C5 0.0172(19) 0.0328(17) 0.0210(19) 0.0154(14) -0.0038(16) 0.0099(15) C6 0.013(2) 0.0265(17) 0.028(2) 0.0148(15) -0.0041(18) 0.0053(16) C7 0.0090(18) 0.0239(16) 0.032(2) 0.0111(15) 0.0027(16) 0.0071(14) C8 0.018(2) 0.039(2) 0.021(2) 0.0068(18) 0.0012(19) 0.0100(18) C9 0.017(2) 0.058(3) 0.022(2) 0.011(2) 0.001(2) 0.004(2) C10 0.0082(19) 0.036(2) 0.030(2) 0.0117(18) 0.0035(18) 0.0061(17) C11 0.018(2) 0.0242(18) 0.030(2) 0.0092(16) -0.0004(19) 0.0089(16) C12 0.025(2) 0.0451(19) 0.025(2) 0.0209(16) 0.0168(18) 0.0284(16) C13 0.030(3) 0.033(2) 0.030(2) 0.0150(18) 0.005(2) 0.0065(19) C14 0.044(3) 0.0328(18) 0.025(2) 0.0207(15) -0.009(2) 0.0117(19) C15 0.021(2) 0.044(2) 0.026(2) 0.0138(18) 0.0040(19) 0.0174(18) C16 0.018(2) 0.0376(18) 0.032(2) 0.0225(16) 0.0016(18) 0.0146(16) C17 0.018(2) 0.0355(18) 0.037(2) 0.0263(16) 0.0144(18) 0.0129(17) C18 0.024(2) 0.047(2) 0.042(2) 0.0293(18) 0.008(2) 0.0182(18) C19 0.020(2) 0.040(2) 0.029(2) 0.0191(17) 0.0098(19) 0.0145(18) C20 0.0130(18) 0.0323(17) 0.037(2) 0.0144(15) 0.0046(17) 0.0150(15) C21 0.0139(19) 0.0303(17) 0.040(2) 0.0273(15) 0.0179(17) 0.0139(15) C22 0.0095(18) 0.0350(19) 0.017(2) 0.0082(16) 0.0038(16) 0.0143(16) C23 0.0064(18) 0.0237(17) 0.026(2) 0.0076(15) -0.0015(16) -0.0020(15) C24 0.018(2) 0.0317(19) 0.031(2) 0.0124(17) 0.0011(19) 0.0088(17) C25 0.012(2) 0.042(2) 0.049(3) 0.0234(19) 0.004(2) 0.0113(18) C26 0.022(2) 0.059(2) 0.079(3) 0.044(2) 0.029(2) 0.025(2) C27 0.014(2) 0.052(2) 0.074(3) 0.044(2) -0.003(2) 0.0056(19) C28 0.020(2) 0.063(2) 0.042(2) 0.0229(19) -0.002(2) 0.005(2) C29 0.017(2) 0.066(3) 0.039(3) 0.020(2) 0.003(2) -0.001(2) C30 0.015(2) 0.056(3) 0.037(3) 0.019(2) 0.006(2) 0.001(2) C31 0.036(3) 0.031(2) 0.042(3) 0.0167(19) 0.022(2) 0.011(2) C32 0.022(2) 0.0408(18) 0.049(3) 0.0312(17) 0.0178(19) 0.0238(16) C33 0.017(2) 0.0359(19) 0.032(2) 0.0248(16) 0.0127(18) 0.0068(17) C34 0.031(3) 0.049(2) 0.028(2) 0.0243(18) 0.006(2) 0.009(2) C35 0.013(2) 0.050(2) 0.041(2) 0.0330(17) 0.0008(19) 0.0022(19) C36 0.013(2) 0.0372(19) 0.044(2) 0.0289(17) 0.0010(19) 0.0008(17) C37 0.033(3) 0.129(5) 0.037(3) 0.031(3) 0.015(3) 0.020(3) C38 0.030(3) 0.127(4) 0.043(3) 0.054(2) 0.000(2) 0.012(3) C39 0.022(3) 0.100(4) 0.031(3) 0.022(3) 0.010(2) 0.017(3) C40 0.021(3) 0.082(4) 0.050(4) -0.004(3) -0.006(3) 0.012(3) C41 0.028(3) 0.069(4) 0.071(4) 0.010(3) -0.001(3) 0.002(3) C42 0.063(4) 0.113(4) 0.063(4) 0.052(3) 0.011(3) 0.026(4) C43 0.040(3) 0.121(5) 0.056(4) 0.043(3) -0.001(3) 0.019(3) C44 0.028(3) 0.111(4) 0.030(3) 0.031(3) 0.002(2) 0.024(3) C45 0.016(2) 0.084(3) 0.042(3) 0.033(2) 0.005(2) 0.008(2) C46 0.031(3) 0.097(4) 0.041(3) 0.028(3) 0.012(2) 0.022(3) C47 0.008(2) 0.109(4) 0.029(3) 0.018(3) 0.004(2) 0.006(3) C48 0.024(3) 0.066(3) 0.034(3) 0.017(2) 0.007(2) 0.001(2) C49 0.022(3) 0.037(3) 0.084(4) -0.001(3) -0.007(3) 0.007(2) C50 0.030(2) 0.062(3) 0.057(3) 0.005(2) -0.007(2) 0.019(2) C51 0.061(3) 0.083(3) 0.033(3) 0.021(2) 0.008(2) 0.057(2) C52 0.056(3) 0.038(2) 0.068(3) 0.027(2) 0.017(3) 0.026(2) C53 0.069(4) 0.022(2) 0.062(4) 0.009(2) 0.017(3) 0.009(2) C54 0.024(3) 0.054(3) 0.098(5) -0.006(4) -0.009(3) -0.006(3) C55 0.037(3) 0.070(3) 0.138(6) 0.044(3) -0.031(4) 0.003(3) C56 0.050(4) 0.064(3) 0.144(5) 0.058(3) -0.027(4) 0.010(3) C57 0.023(3) 0.025(2) 0.068(3) 0.016(2) -0.011(2) -0.005(2) C58 0.028(3) 0.029(2) 0.047(3) -0.002(2) 0.008(2) 0.010(2) C59 0.033(2) 0.037(2) 0.041(3) 0.008(2) 0.004(2) 0.0256(18) C60 0.022(2) 0.027(2) 0.042(3) 0.0039(19) -0.010(2) 0.0078(18) C61 0.030(3) 0.068(4) 0.042(3) 0.004(3) 0.000(3) -0.004(3) C62 0.041(3) 0.087(4) 0.049(4) 0.001(3) 0.023(3) -0.003(3) C63 0.049(4) 0.071(4) 0.066(4) 0.026(3) 0.018(3) -0.004(3) C64 0.034(3) 0.092(3) 0.043(3) 0.044(2) 0.016(2) 0.009(3) C65 0.017(2) 0.077(3) 0.028(3) 0.016(2) 0.012(2) 0.006(2) C66 0.014(2) 0.095(4) 0.022(3) 0.017(2) -0.003(2) 0.011(2) C67 0.037(3) 0.076(4) 0.046(4) -0.003(3) 0.001(3) 0.010(3) C68 0.041(3) 0.104(4) 0.056(4) 0.032(3) -0.002(3) 0.027(3) C69 0.017(2) 0.055(2) 0.047(3) 0.0197(19) 0.007(2) 0.0072(19) C70 0.013(2) 0.081(3) 0.026(3) 0.007(3) -0.001(2) 0.013(2) C71 0.022(3) 0.085(4) 0.033(3) 0.007(3) 0.013(2) 0.005(3) C72 0.025(3) 0.071(3) 0.028(3) 0.013(2) 0.000(2) 0.012(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 Sm1 O4 2.325(3) . ? Sm1 O3 2.337(3) . ? Sm1 O2 2.345(3) . ? Sm1 O1 2.354(3) . ? Sm1 O5 2.435(4) . ? Sm1 O6 2.472(3) . ? Sm1 O7 2.506(3) . ? Sm1 O8 2.533(3) . ? S1 O9 1.424(3) . ? S1 O10 1.446(3) . ? S1 C1 1.764(5) . ? S1 C2 1.780(4) . ? S2 O12 1.437(3) . ? S2 O11 1.444(3) . ? S2 C7 1.759(5) . ? S2 C6 1.765(4) . ? S3 O14 1.404(5) . ? S3 O13 1.438(4) . ? S3 C12 1.783(4) . ? S3 C11 1.803(4) . ? S4 O15 1.424(3) . ? S4 O16 1.445(3) . ? S4 C16 1.791(5) . ? S4 C17 1.793(5) . ? S5 O19A 1.306(13) . ? S5 O17A 1.379(13) . ? S5 O19B 1.426(8) . ? S5 O18B 1.428(8) . ? S5 O17B 1.454(8) . ? S5 O18A 1.521(14) . ? S5 C19 1.770(4) . ? S6 O21 1.444(3) . ? S6 O20 1.458(4) . ? S6 O22 1.470(4) . ? S6 C4 1.796(4) . ? S7 O23 1.437(4) . ? S7 O24 1.445(5) . ? S7 O25 1.466(4) . ? S7 C9 1.764(6) . ? S8 O28A 1.334(8) . ? S8 O26B 1.381(8) . ? S8 O27A 1.425(8) . ? S8 O27B 1.480(8) . ? S8 O28B 1.522(9) . ? S8 O26A 1.558(9) . ? S8 C14 1.754(5) . ? N1 C36 1.346(5) . ? N1 C25 1.350(6) . ? N2 C32 1.337(6) . ? N2 C33 1.382(6) . ? N3 C48 1.333(7) . ? N3 C37 1.335(9) . ? N4 C44 1.278(9) . ? N4 C45 1.357(6) . ? N5 C49 1.323(7) . ? N5 C60 1.364(6) . ? N6 C56 1.298(8) . ? N6 C57 1.373(8) . ? N7 C61 1.313(7) . ? N7 C72 1.395(7) . ? N8 C68 1.357(8) . ? N8 C69 1.392(9) . ? O1 C21 1.252(4) . ? O2 C22 1.294(5) . ? O3 C23 1.263(6) . ? O4 C24 1.276(6) . ? C1 C20 1.372(5) . ? C1 C21 1.452(6) . ? C2 C3 1.373(6) . ? C2 C22 1.403(6) . ? C3 C4 1.412(6) . ? C3 H3 0.9500 . ? C4 C5 1.357(6) . ? C5 C6 1.386(6) . ? C5 H5 0.9500 . ? C6 C22 1.445(6) . ? C7 C8 1.384(7) . ? C7 C23 1.481(6) . ? C8 C9 1.374(8) . ? C8 H8 0.9500 . ? C9 C10 1.426(6) . ? C10 C11 1.356(7) . ? C10 H10 0.9500 . ? C11 C23 1.411(7) . ? C12 C13 1.333(7) . ? C12 C24 1.435(7) . ? C13 C14 1.399(7) . ? C13 H13 0.9500 . ? C14 C15 1.428(7) . ? C15 C16 1.412(7) . ? C15 H15 0.9500 . ? C16 C24 1.408(6) . ? C17 C18 1.385(5) . ? C17 C21 1.427(7) . ? C18 C19 1.397(7) . ? C18 H18 0.9500 . ? C19 C20 1.406(7) . ? C20 H20 0.9500 . ? C25 C26 1.428(8) . ? C25 H25 0.9500 . ? C26 C27 1.356(6) . ? C26 H26 0.9500 . ? C27 C35 1.388(7) . ? C27 H27 0.9500 . ? C28 C29 1.295(8) . ? C28 C35 1.458(6) . ? C28 H28 0.9500 . ? C29 C34 1.473(8) . ? C29 H29 0.9500 . ? C30 C31 1.386(8) . ? C30 C34 1.391(7) . ? C30 H30 0.9500 . ? C31 C32 1.402(6) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.363(5) . ? C33 C36 1.434(6) . ? C35 C36 1.391(7) . ? C37 C38 1.445(7) . ? C37 H37 0.9500 . ? C38 C39 1.369(9) . ? C38 H38 0.9500 . ? C39 C47 1.327(10) . ? C39 H39 0.9500 . ? C40 C41 1.344(11) . ? C40 C47 1.447(9) . ? C40 H40 0.9500 . ? C41 C46 1.417(8) . ? C41 H41 0.9500 . ? C42 C43 1.380(8) . ? C42 C46 1.385(11) . ? C42 H42 0.9500 . ? C43 C44 1.419(10) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.392(8) . ? C45 C48 1.419(9) . ? C47 C48 1.407(7) . ? C49 C50 1.325(9) . ? C49 H49 0.9500 . ? C50 C51 1.383(8) . ? C50 H50 0.9500 . ? C51 C59 1.435(7) . ? C51 H51 0.9500 . ? C52 C53 1.339(9) . ? C52 C59 1.453(7) . ? C52 H52 0.9500 . ? C53 C58 1.419(9) . ? C53 H53 0.9500 . ? C54 C58 1.410(8) . ? C54 C55 1.429(11) . ? C54 H54 0.9500 . ? C55 C56 1.403(9) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C60 1.434(7) . ? C57 C58 1.448(7) . ? C59 C60 1.357(8) . ? C61 C62 1.379(11) . ? C61 H61 0.9500 . ? C62 C63 1.358(9) . ? C62 H62 0.9500 . ? C63 C71 1.411(8) . ? C63 H63 0.9500 . ? C64 C65 1.379(7) . ? C64 C71 1.437(8) . ? C64 H64 0.9500 . ? C65 C70 1.392(9) . ? C65 H65 0.9500 . ? C66 C67 1.379(10) . ? C66 C70 1.381(8) . ? C66 H66 0.9500 . ? C67 C68 1.358(9) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.371(7) . ? C69 C72 1.416(7) . ? C71 C72 1.330(10) . ? O001 O002 1.27(2) . ? O001 O003 1.537(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Sm1 O3 80.25(11) . . ? O4 Sm1 O2 81.06(10) . . ? O3 Sm1 O2 72.37(10) . . ? O4 Sm1 O1 71.56(11) . . ? O3 Sm1 O1 140.75(9) . . ? O2 Sm1 O1 76.66(9) . . ? O4 Sm1 O5 140.22(11) . . ? O3 Sm1 O5 139.48(11) . . ? O2 Sm1 O5 108.87(12) . . ? O1 Sm1 O5 73.59(11) . . ? O4 Sm1 O6 119.87(11) . . ? O3 Sm1 O6 79.39(10) . . ? O2 Sm1 O6 141.33(10) . . ? O1 Sm1 O6 138.51(10) . . ? O5 Sm1 O6 76.69(11) . . ? O4 Sm1 O7 75.84(11) . . ? O3 Sm1 O7 125.08(11) . . ? O2 Sm1 O7 147.07(9) . . ? O1 Sm1 O7 73.97(9) . . ? O5 Sm1 O7 76.64(12) . . ? O6 Sm1 O7 71.46(10) . . ? O4 Sm1 O8 147.23(10) . . ? O3 Sm1 O8 72.38(11) . . ? O2 Sm1 O8 73.83(9) . . ? O1 Sm1 O8 120.94(10) . . ? O5 Sm1 O8 69.53(11) . . ? O6 Sm1 O8 72.76(10) . . ? O7 Sm1 O8 135.16(10) . . ? O9 S1 O10 118.7(2) . . ? O9 S1 C1 109.7(2) . . ? O10 S1 C1 107.05(18) . . ? O9 S1 C2 110.50(18) . . ? O10 S1 C2 105.11(18) . . ? C1 S1 C2 104.8(2) . . ? O12 S2 O11 115.13(18) . . ? O12 S2 C7 106.2(2) . . ? O11 S2 C7 110.57(19) . . ? O12 S2 C6 107.25(19) . . ? O11 S2 C6 107.9(2) . . ? C7 S2 C6 109.7(2) . . ? O14 S3 O13 120.2(2) . . ? O14 S3 C12 106.9(2) . . ? O13 S3 C12 106.7(2) . . ? O14 S3 C11 112.2(3) . . ? O13 S3 C11 105.6(2) . . ? C12 S3 C11 103.85(19) . . ? O15 S4 O16 116.84(19) . . ? O15 S4 C16 105.95(18) . . ? O16 S4 C16 106.9(2) . . ? O15 S4 C17 108.1(2) . . ? O16 S4 C17 106.91(18) . . ? C16 S4 C17 112.3(2) . . ? O19A S5 O17A 122.8(7) . . ? O19A S5 O19B 33.8(7) . . ? O17A S5 O19B 144.9(5) . . ? O19A S5 O18B 130.7(6) . . ? O17A S5 O18B 58.2(6) . . ? O19B S5 O18B 112.4(4) . . ? O19A S5 O17B 82.2(7) . . ? O17A S5 O17B 54.3(6) . . ? O19B S5 O17B 116.0(4) . . ? O18B S5 O17B 111.8(4) . . ? O19A S5 O18A 101.1(8) . . ? O17A S5 O18A 96.3(8) . . ? O19B S5 O18A 73.9(6) . . ? O18B S5 O18A 40.1(6) . . ? O17B S5 O18A 143.2(5) . . ? O19A S5 C19 114.8(5) . . ? O17A S5 C19 110.4(5) . . ? O19B S5 C19 104.7(3) . . ? O18B S5 C19 107.5(3) . . ? O17B S5 C19 103.4(3) . . ? O18A S5 C19 108.0(4) . . ? O21 S6 O20 114.9(2) . . ? O21 S6 O22 110.2(2) . . ? O20 S6 O22 113.2(2) . . ? O21 S6 C4 105.2(2) . . ? O20 S6 C4 104.9(2) . . ? O22 S6 C4 107.7(2) . . ? O23 S7 O24 112.2(3) . . ? O23 S7 O25 112.1(2) . . ? O24 S7 O25 113.0(2) . . ? O23 S7 C9 105.9(2) . . ? O24 S7 C9 107.8(2) . . ? O25 S7 C9 105.3(3) . . ? O28A S8 O26B 71.4(5) . . ? O28A S8 O27A 116.4(5) . . ? O26B S8 O27A 137.2(5) . . ? O28A S8 O27B 136.8(6) . . ? O26B S8 O27B 119.9(5) . . ? O27A S8 O27B 25.8(5) . . ? O28A S8 O28B 36.5(5) . . ? O26B S8 O28B 107.8(5) . . ? O27A S8 O28B 89.7(5) . . ? O27B S8 O28B 115.4(5) . . ? O28A S8 O26A 107.6(5) . . ? O26B S8 O26A 38.4(4) . . ? O27A S8 O26A 108.0(5) . . ? O27B S8 O26A 84.7(4) . . ? O28B S8 O26A 143.0(4) . . ? O28A S8 C14 113.1(4) . . ? O26B S8 C14 108.4(4) . . ? O27A S8 C14 106.1(4) . . ? O27B S8 C14 102.7(4) . . ? O28B S8 C14 100.6(4) . . ? O26A S8 C14 104.9(4) . . ? C36 N1 C25 123.9(4) . . ? C32 N2 C33 114.4(3) . . ? C48 N3 C37 125.2(5) . . ? C44 N4 C45 117.9(5) . . ? C49 N5 C60 119.8(5) . . ? C56 N6 C57 117.8(5) . . ? C61 N7 C72 114.9(6) . . ? C68 N8 C69 121.8(5) . . ? C21 O1 Sm1 133.9(3) . . ? C22 O2 Sm1 153.3(3) . . ? C23 O3 Sm1 127.9(2) . . ? C24 O4 Sm1 150.1(3) . . ? C20 C1 C21 122.7(4) . . ? C20 C1 S1 115.0(3) . . ? C21 C1 S1 122.1(3) . . ? C3 C2 C22 124.1(4) . . ? C3 C2 S1 117.8(3) . . ? C22 C2 S1 117.7(3) . . ? C2 C3 C4 118.3(4) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 120.3(4) . . ? C5 C4 S6 121.1(3) . . ? C3 C4 S6 118.4(3) . . ? C4 C5 C6 121.5(4) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C22 120.6(4) . . ? C5 C6 S2 117.3(3) . . ? C22 C6 S2 121.3(3) . . ? C8 C7 C23 122.1(4) . . ? C8 C7 S2 117.6(3) . . ? C23 C7 S2 119.9(4) . . ? C9 C8 C7 120.8(4) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 119.8(5) . . ? C8 C9 S7 122.6(4) . . ? C10 C9 S7 117.5(4) . . ? C11 C10 C9 118.5(5) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C10 C11 C23 126.2(4) . . ? C10 C11 S3 114.3(4) . . ? C23 C11 S3 119.5(4) . . ? C13 C12 C24 125.1(4) . . ? C13 C12 S3 120.4(4) . . ? C24 C12 S3 114.4(4) . . ? C12 C13 C14 120.5(5) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C15 118.6(5) . . ? C13 C14 S8 121.3(4) . . ? C15 C14 S8 120.1(4) . . ? C16 C15 C14 118.7(4) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C24 C16 C15 123.1(4) . . ? C24 C16 S4 120.7(4) . . ? C15 C16 S4 115.6(3) . . ? C18 C17 C21 124.1(4) . . ? C18 C17 S4 114.4(4) . . ? C21 C17 S4 121.1(3) . . ? C17 C18 C19 120.1(5) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C20 118.5(4) . . ? C18 C19 S5 122.4(4) . . ? C20 C19 S5 119.1(3) . . ? C1 C20 C19 121.1(4) . . ? C1 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? O1 C21 C17 124.1(4) . . ? O1 C21 C1 122.7(4) . . ? C17 C21 C1 113.2(3) . . ? O2 C22 C2 123.5(4) . . ? O2 C22 C6 121.1(4) . . ? C2 C22 C6 115.2(4) . . ? O3 C23 C11 124.5(4) . . ? O3 C23 C7 123.0(4) . . ? C11 C23 C7 112.4(4) . . ? O4 C24 C16 123.6(4) . . ? O4 C24 C12 122.7(4) . . ? C16 C24 C12 113.7(4) . . ? N1 C25 C26 117.1(4) . . ? N1 C25 H25 121.4 . . ? C26 C25 H25 121.4 . . ? C27 C26 C25 119.7(5) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C35 121.4(5) . . ? C26 C27 H27 119.3 . . ? C35 C27 H27 119.3 . . ? C29 C28 C35 121.9(5) . . ? C29 C28 H28 119.1 . . ? C35 C28 H28 119.1 . . ? C28 C29 C34 121.3(4) . . ? C28 C29 H29 119.3 . . ? C34 C29 H29 119.3 . . ? C31 C30 C34 118.7(4) . . ? C31 C30 H30 120.6 . . ? C34 C30 H30 120.6 . . ? C30 C31 C32 118.4(4) . . ? C30 C31 H31 120.8 . . ? C32 C31 H31 120.8 . . ? N2 C32 C31 124.7(5) . . ? N2 C32 H32 117.7 . . ? C31 C32 H32 117.7 . . ? C34 C33 N2 125.1(4) . . ? C34 C33 C36 119.3(4) . . ? N2 C33 C36 115.5(3) . . ? C33 C34 C30 118.6(5) . . ? C33 C34 C29 118.9(4) . . ? C30 C34 C29 122.5(4) . . ? C27 C35 C36 118.3(4) . . ? C27 C35 C28 124.7(5) . . ? C36 C35 C28 117.0(4) . . ? N1 C36 C35 119.6(4) . . ? N1 C36 C33 118.8(4) . . ? C35 C36 C33 121.6(4) . . ? N3 C37 C38 116.0(6) . . ? N3 C37 H37 122.0 . . ? C38 C37 H37 122.0 . . ? C39 C38 C37 120.0(7) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C47 C39 C38 119.9(5) . . ? C47 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C47 122.7(5) . . ? C41 C40 H40 118.7 . . ? C47 C40 H40 118.7 . . ? C40 C41 C46 120.4(6) . . ? C40 C41 H41 119.8 . . ? C46 C41 H41 119.8 . . ? C43 C42 C46 119.9(7) . . ? C43 C42 H42 120.1 . . ? C46 C42 H42 120.1 . . ? C42 C43 C44 117.5(7) . . ? C42 C43 H43 121.2 . . ? C44 C43 H43 121.2 . . ? N4 C44 C43 124.0(5) . . ? N4 C44 H44 118.0 . . ? C43 C44 H44 118.0 . . ? N4 C45 C46 123.6(6) . . ? N4 C45 C48 117.8(5) . . ? C46 C45 C48 118.5(5) . . ? C42 C46 C45 117.1(5) . . ? C42 C46 C41 122.8(6) . . ? C45 C46 C41 120.0(7) . . ? C39 C47 C48 121.4(6) . . ? C39 C47 C40 123.1(5) . . ? C48 C47 C40 115.4(6) . . ? N3 C48 C47 117.4(6) . . ? N3 C48 C45 119.8(5) . . ? C47 C48 C45 122.8(5) . . ? N5 C49 C50 123.5(5) . . ? N5 C49 H49 118.3 . . ? C50 C49 H49 118.3 . . ? C49 C50 C51 119.0(5) . . ? C49 C50 H50 120.5 . . ? C51 C50 H50 120.5 . . ? C50 C51 C59 119.0(6) . . ? C50 C51 H51 120.5 . . ? C59 C51 H51 120.5 . . ? C53 C52 C59 120.2(6) . . ? C53 C52 H52 119.9 . . ? C59 C52 H52 119.9 . . ? C52 C53 C58 122.9(5) . . ? C52 C53 H53 118.5 . . ? C58 C53 H53 118.5 . . ? C58 C54 C55 117.1(5) . . ? C58 C54 H54 121.4 . . ? C55 C54 H54 121.4 . . ? C56 C55 C54 118.4(6) . . ? C56 C55 H55 120.8 . . ? C54 C55 H55 120.8 . . ? N6 C56 C55 126.0(7) . . ? N6 C56 H56 117.0 . . ? C55 C56 H56 117.0 . . ? N6 C57 C60 119.7(4) . . ? N6 C57 C58 121.6(5) . . ? C60 C57 C58 118.6(5) . . ? C54 C58 C53 123.6(5) . . ? C54 C58 C57 118.9(6) . . ? C53 C58 C57 117.5(5) . . ? C60 C59 C51 117.6(5) . . ? C60 C59 C52 119.2(5) . . ? C51 C59 C52 123.2(5) . . ? C59 C60 N5 121.1(4) . . ? C59 C60 C57 121.7(4) . . ? N5 C60 C57 117.3(5) . . ? N7 C61 C62 124.1(6) . . ? N7 C61 H61 117.9 . . ? C62 C61 H61 117.9 . . ? C63 C62 C61 119.4(6) . . ? C63 C62 H62 120.3 . . ? C61 C62 H62 120.3 . . ? C62 C63 C71 119.2(7) . . ? C62 C63 H63 120.4 . . ? C71 C63 H63 120.4 . . ? C65 C64 C71 120.9(6) . . ? C65 C64 H64 119.6 . . ? C71 C64 H64 119.6 . . ? C64 C65 C70 119.3(5) . . ? C64 C65 H65 120.3 . . ? C70 C65 H65 120.3 . . ? C67 C66 C70 121.2(5) . . ? C67 C66 H66 119.4 . . ? C70 C66 H66 119.4 . . ? C68 C67 C66 118.7(6) . . ? C68 C67 H67 120.6 . . ? C66 C67 H67 120.6 . . ? N8 C68 C67 120.5(7) . . ? N8 C68 H68 119.8 . . ? C67 C68 H68 119.8 . . ? C70 C69 N8 117.9(5) . . ? C70 C69 C72 124.0(6) . . ? N8 C69 C72 118.1(5) . . ? C69 C70 C66 119.9(6) . . ? C69 C70 C65 117.9(5) . . ? C66 C70 C65 122.2(5) . . ? C72 C71 C63 117.0(6) . . ? C72 C71 C64 120.2(5) . . ? C63 C71 C64 122.8(7) . . ? C71 C72 N7 125.5(5) . . ? C71 C72 C69 117.5(5) . . ? N7 C72 C69 116.8(6) . . ? O002 O001 O003 80.6(10) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.758 _refine_diff_density_min -1.859 _refine_diff_density_rms 0.213 ###END data_3 _database_code_depnum_ccdc_archive 'CCDC 685585' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'H5 Tb (C24H8O24S8) (C12H8N2)4 (H2O)11.33' _chemical_melting_point ? _chemical_formula_moiety 'H5 Tb [C24H8O24S8] [C12H8N2]4 [H2O]11.33' _chemical_formula_sum 'C72 H67.65 N8 O35.33 S8 Tb' _chemical_formula_weight 2025.59 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' Tb Tb -0.1723 4.1537 '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' _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 14.3599(10) _cell_length_b 18.1656(12) _cell_length_c 19.2901(13) _cell_angle_alpha 112.7280(10) _cell_angle_beta 92.5900(10) _cell_angle_gamma 97.6210(10) _cell_volume 4574.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5126 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.62 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2063 _exptl_absorpt_coefficient_mu 1.042 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7276 _exptl_absorpt_correction_T_max 0.8799 _exptl_absorpt_process_details ; SADABS, Sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 AXS Apex CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 30983 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15908 _reflns_number_gt 12922 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (1998)' _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. All the non-hydrogen atoms were refined anisotropically except some isolated molecular atoms. All the oxygen atoms of the solvent water molecules were refined without hydrogen atoms. The oxygen atoms of two sulfonate groups (O17-O19, O26-O28) were refined with disordered positions and the same displacement parameters for all oxygen atoms on one sulfonate group. The short contact O25...C68 might be due to the high mobility of the isolated phenanthroline molecules. ; _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^)+(0.1395P)^2^+26.7858P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15908 _refine_ls_number_parameters 1097 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2339 _refine_ls_wR_factor_gt 0.2224 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.03321(2) 0.75899(2) 0.021626(19) 0.01986(14) Uani 1 1 d . . . S1 S 0.08519(13) 1.01365(12) 0.09230(11) 0.0221(4) Uani 1 1 d . . . S2 S -0.22197(13) 0.83362(12) 0.14602(11) 0.0236(4) Uani 1 1 d . . . S3 S 0.00503(14) 0.59922(12) 0.12202(11) 0.0249(4) Uani 1 1 d . . . S4 S 0.32056(13) 0.81894(12) 0.15578(11) 0.0224(4) Uani 1 1 d . . . S5 S 0.33712(17) 1.13419(14) 0.33925(12) 0.0379(5) Uani 1 1 d . . . S6 S -0.20731(14) 1.15543(13) 0.22674(11) 0.0281(5) Uani 1 1 d . . . S7 S -0.15875(18) 0.73676(19) 0.37476(13) 0.0482(7) Uani 1 1 d . . . S8 S 0.3261(2) 0.59878(17) 0.28247(17) 0.0518(7) Uani 1 1 d . . . N1 N -0.3753(5) 1.1538(4) 0.0592(4) 0.0295(16) Uani 1 1 d . . . N2 N -0.3147(5) 1.0097(4) 0.0096(4) 0.0292(16) Uani 1 1 d . . . N3 N 0.1055(5) 1.0593(5) 0.4573(4) 0.041(2) Uani 1 1 d . . . N4 N 0.1435(5) 0.9950(6) 0.5579(4) 0.045(2) Uani 1 1 d . . . N5 N 0.3459(5) 0.4390(5) 0.0728(5) 0.043(2) Uani 1 1 d . . . N6 N 0.5291(6) 0.4523(5) 0.1250(5) 0.047(2) Uani 1 1 d . . . N7 N -0.3642(6) 1.0307(7) 0.5563(5) 0.058(3) Uani 1 1 d . . . N8 N -0.3816(6) 0.8722(7) 0.4659(5) 0.059(3) Uani 1 1 d . . . O1 O 0.1678(4) 0.8560(3) 0.0605(3) 0.0220(11) Uani 1 1 d . A . O2 O -0.0160(4) 0.8693(3) 0.1128(3) 0.0231(11) Uani 1 1 d . . . O3 O -0.0960(4) 0.7088(3) 0.0657(3) 0.0223(11) Uani 1 1 d . . . O4 O 0.1066(3) 0.7532(3) 0.1278(3) 0.0225(11) Uani 1 1 d . B . O5 O 0.0696(5) 0.7902(5) -0.0861(4) 0.0448(17) Uani 1 1 d . . . O6 O -0.0261(4) 0.6328(4) -0.0842(3) 0.0350(14) Uani 1 1 d . . . O7 O 0.1646(4) 0.6854(3) -0.0233(3) 0.0304(13) Uani 1 1 d . . . O8 O -0.1091(4) 0.7828(4) -0.0394(3) 0.0297(13) Uani 1 1 d . . . O9 O 0.0730(4) 0.9555(4) 0.0160(3) 0.0297(13) Uani 1 1 d . . . O10 O 0.1094(4) 1.0985(3) 0.1053(3) 0.0300(13) Uani 1 1 d . . . O11 O -0.2460(4) 0.7907(3) 0.0663(3) 0.0285(13) Uani 1 1 d . . . O12 O -0.3008(4) 0.8524(4) 0.1904(3) 0.0333(14) Uani 1 1 d . . . O13 O -0.0188(4) 0.5295(3) 0.1401(3) 0.0344(14) Uani 1 1 d . . . O14 O 0.0050(4) 0.5861(4) 0.0438(3) 0.0339(14) Uani 1 1 d . . . O15 O 0.3215(4) 0.7803(3) 0.0748(3) 0.0253(12) Uani 1 1 d . . . O16 O 0.4114(4) 0.8424(4) 0.2004(3) 0.0301(13) Uani 1 1 d . . . O17A O 0.3980(19) 1.1847(16) 0.3115(14) 0.069(2) Uani 0.325(8) 1 d P A 1 O18A O 0.4000(19) 1.1056(16) 0.3865(15) 0.069(2) Uani 0.325(8) 1 d P A 1 O19A O 0.2665(19) 1.1747(17) 0.3782(15) 0.069(2) Uani 0.325(8) 1 d P A 1 O17B O 0.3120(9) 1.2022(8) 0.3256(7) 0.069(2) Uani 0.675(8) 1 d P A 2 O18B O 0.4340(9) 1.1345(8) 0.3402(7) 0.069(2) Uani 0.675(8) 1 d P A 2 O19B O 0.2964(9) 1.1277(8) 0.4016(7) 0.069(2) Uani 0.675(8) 1 d P A 2 O20 O -0.2923(5) 1.1312(4) 0.2552(4) 0.0443(16) Uani 1 1 d . . . O21 O -0.1408(5) 1.2175(4) 0.2851(4) 0.0440(17) Uani 1 1 d . . . O22 O -0.2269(4) 1.1788(4) 0.1638(3) 0.0369(14) Uani 1 1 d . . . O23 O -0.2339(6) 0.6701(5) 0.3620(4) 0.056(2) Uani 1 1 d . . . O24 O -0.0707(6) 0.7274(7) 0.4089(4) 0.085(3) Uani 1 1 d . . . O25 O -0.1875(6) 0.8142(5) 0.4144(4) 0.064(2) Uani 1 1 d . . . O26A O 0.4231(11) 0.5964(11) 0.2507(10) 0.062(2) Uani 0.564(11) 1 d P B 1 O27A O 0.2822(12) 0.5203(12) 0.2638(10) 0.062(2) Uani 0.564(11) 1 d P B 1 O28A O 0.3384(12) 0.6456(10) 0.3603(9) 0.062(2) Uani 0.564(11) 1 d P B 1 O26B O 0.4185(14) 0.6372(14) 0.2967(13) 0.062(2) Uani 0.436(11) 1 d P B 2 O27B O 0.3000(16) 0.5092(15) 0.2324(13) 0.062(2) Uani 0.436(11) 1 d P B 2 O28B O 0.2800(16) 0.6238(14) 0.3567(11) 0.062(2) Uani 0.436(11) 1 d P B 2 C1 C 0.1716(5) 0.9926(5) 0.1468(4) 0.0213(16) Uani 1 1 d . A . C2 C -0.0211(5) 1.0066(5) 0.1345(4) 0.0208(16) Uani 1 1 d . . . C3 C -0.0634(5) 1.0747(5) 0.1632(4) 0.0206(16) Uani 1 1 d . . . H3 H -0.0333 1.1248 0.1639 0.025 Uiso 1 1 calc R . . C4 C -0.1516(5) 1.0692(5) 0.1917(4) 0.0229(16) Uani 1 1 d . . . C5 C -0.1943(5) 0.9956(5) 0.1898(4) 0.0234(17) Uani 1 1 d . . . H5 H -0.2538 0.9921 0.2089 0.028 Uiso 1 1 calc R . . C6 C -0.1526(5) 0.9268(5) 0.1607(4) 0.0214(16) Uani 1 1 d . . . C7 C -0.1604(5) 0.7754(4) 0.1816(4) 0.0214(16) Uani 1 1 d . . . C8 C -0.1733(5) 0.7833(5) 0.2553(5) 0.0278(18) Uani 1 1 d . . . H8 H -0.2067 0.8237 0.2859 0.033 Uiso 1 1 calc R . . C9 C -0.1375(6) 0.7324(6) 0.2839(4) 0.0295(19) Uani 1 1 d . . . C10 C -0.0842(5) 0.6761(5) 0.2403(4) 0.0264(18) Uani 1 1 d . . . H10 H -0.0583 0.6420 0.2604 0.032 Uiso 1 1 calc R . . C11 C -0.0691(5) 0.6695(5) 0.1683(4) 0.0235(17) Uani 1 1 d . . . C12 C 0.1198(6) 0.6471(5) 0.1676(4) 0.0250(17) Uani 1 1 d . B . C13 C 0.1691(6) 0.6110(5) 0.2046(4) 0.0259(17) Uani 1 1 d . . . H13 H 0.1397 0.5644 0.2111 0.031 Uiso 1 1 calc R B . C14 C 0.2630(6) 0.6442(5) 0.2325(5) 0.0298(18) Uani 1 1 d . B . C15 C 0.3052(6) 0.7111(5) 0.2208(5) 0.0285(18) Uani 1 1 d . . . H15 H 0.3698 0.7327 0.2387 0.034 Uiso 1 1 calc R B . C16 C 0.2548(6) 0.7461(5) 0.1840(4) 0.0234(16) Uani 1 1 d . B . C17 C 0.2691(5) 0.9080(5) 0.1772(4) 0.0223(16) Uani 1 1 d . A . C18 C 0.3094(6) 0.9735(5) 0.2421(4) 0.0271(18) Uani 1 1 d . . . H18 H 0.3555 0.9667 0.2752 0.033 Uiso 1 1 calc R A . C19 C 0.2835(5) 1.0477(5) 0.2591(4) 0.0260(17) Uani 1 1 d . A . C20 C 0.2130(5) 1.0569(5) 0.2117(4) 0.0250(17) Uani 1 1 d . . . H20 H 0.1936 1.1081 0.2244 0.030 Uiso 1 1 calc R A . C21 C 0.2000(5) 0.9137(5) 0.1239(4) 0.0228(17) Uani 1 1 d . . . C22 C -0.0605(5) 0.9296(5) 0.1336(4) 0.0204(16) Uani 1 1 d . . . C23 C -0.1071(5) 0.7170(4) 0.1335(4) 0.0207(16) Uani 1 1 d . . . C24 C 0.1572(5) 0.7182(5) 0.1572(4) 0.0218(16) Uani 1 1 d . . . C25 C -0.4031(6) 1.2260(6) 0.0886(6) 0.036(2) Uani 1 1 d . . . H25 H -0.3723 1.2660 0.1351 0.043 Uiso 1 1 calc R . . C26 C -0.4769(6) 1.2424(6) 0.0512(6) 0.041(2) Uani 1 1 d . . . H26 H -0.4969 1.2937 0.0723 0.049 Uiso 1 1 calc R . . C27 C -0.5213(6) 1.1855(6) -0.0160(6) 0.039(2) Uani 1 1 d . . . H27 H -0.5714 1.1973 -0.0419 0.047 Uiso 1 1 calc R . . C28 C -0.5331(6) 1.0462(7) -0.1175(6) 0.040(2) Uani 1 1 d . . . H28 H -0.5823 1.0555 -0.1461 0.048 Uiso 1 1 calc R . . C29 C -0.5032(6) 0.9746(7) -0.1440(5) 0.041(2) Uani 1 1 d . . . H29 H -0.5324 0.9340 -0.1907 0.049 Uiso 1 1 calc R . . C30 C -0.3949(7) 0.8842(6) -0.1265(5) 0.042(2) Uani 1 1 d . . . H30 H -0.4217 0.8414 -0.1728 0.050 Uiso 1 1 calc R . . C31 C -0.3242(7) 0.8727(6) -0.0833(5) 0.039(2) Uani 1 1 d . . . H31 H -0.3018 0.8225 -0.0986 0.047 Uiso 1 1 calc R . . C32 C -0.2859(6) 0.9384(6) -0.0149(5) 0.034(2) Uani 1 1 d . . . H32 H -0.2366 0.9310 0.0151 0.041 Uiso 1 1 calc R . . C33 C -0.3839(6) 1.0182(5) -0.0339(5) 0.0283(18) Uani 1 1 d . . . C34 C -0.4277(6) 0.9574(6) -0.1035(5) 0.033(2) Uani 1 1 d . . . C35 C -0.4923(6) 1.1090(6) -0.0467(5) 0.032(2) Uani 1 1 d . . . C36 C -0.4171(6) 1.0952(5) -0.0070(5) 0.0285(18) Uani 1 1 d . . . C37 C 0.0825(8) 1.0951(8) 0.4127(6) 0.053(3) Uani 1 1 d . . . H37 H 0.0809 1.1515 0.4330 0.063 Uiso 1 1 calc R . . C38 C 0.0602(7) 1.0485(9) 0.3339(5) 0.054(3) Uani 1 1 d . . . H38 H 0.0428 1.0735 0.3012 0.065 Uiso 1 1 calc R . . C39 C 0.0640(7) 0.9689(8) 0.3058(5) 0.049(3) Uani 1 1 d . . . H39 H 0.0506 0.9382 0.2529 0.058 Uiso 1 1 calc R . . C40 C 0.0917(7) 0.8495(7) 0.3277(6) 0.050(3) Uani 1 1 d . . . H40 H 0.0795 0.8166 0.2752 0.060 Uiso 1 1 calc R . . C41 C 0.1133(8) 0.8155(8) 0.3764(6) 0.057(3) Uani 1 1 d . . . H41 H 0.1167 0.7594 0.3569 0.069 Uiso 1 1 calc R . . C42 C 0.1507(9) 0.8307(9) 0.5106(8) 0.071(4) Uani 1 1 d . . . H42 H 0.1537 0.7747 0.4949 0.085 Uiso 1 1 calc R . . C43 C 0.1654(8) 0.8776(9) 0.5837(7) 0.063(3) Uani 1 1 d . . . H43 H 0.1778 0.8562 0.6203 0.076 Uiso 1 1 calc R . . C44 C 0.1621(7) 0.9597(9) 0.6046(6) 0.060(4) Uani 1 1 d . . . H44 H 0.1741 0.9933 0.6570 0.072 Uiso 1 1 calc R . . C45 C 0.1284(6) 0.9440(7) 0.4840(5) 0.045(3) Uani 1 1 d . . . C46 C 0.1308(7) 0.8609(7) 0.4556(6) 0.050(3) Uani 1 1 d . . . C47 C 0.0873(6) 0.9306(7) 0.3529(5) 0.043(3) Uani 1 1 d . . . C48 C 0.1069(6) 0.9801(7) 0.4323(5) 0.040(2) Uani 1 1 d . . . C49 C 0.2543(7) 0.4287(7) 0.0458(6) 0.056(3) Uani 1 1 d . . . H49 H 0.2122 0.3818 0.0414 0.068 Uiso 1 1 calc R . . C50 C 0.2210(8) 0.4866(8) 0.0244(6) 0.057(3) Uani 1 1 d . . . H50 H 0.1567 0.4796 0.0056 0.069 Uiso 1 1 calc R . . C51 C 0.2835(8) 0.5538(8) 0.0310(6) 0.054(3) Uani 1 1 d . . . H51 H 0.2622 0.5934 0.0162 0.065 Uiso 1 1 calc R . . C52 C 0.4460(8) 0.6351(6) 0.0691(6) 0.046(3) Uani 1 1 d . . . H52 H 0.4269 0.6756 0.0546 0.056 Uiso 1 1 calc R . . C53 C 0.5345(8) 0.6439(6) 0.0980(6) 0.046(3) Uani 1 1 d . . . H53 H 0.5769 0.6917 0.1051 0.055 Uiso 1 1 calc R . . C54 C 0.6606(7) 0.5895(7) 0.1491(7) 0.055(3) Uani 1 1 d . . . H54 H 0.7055 0.6366 0.1589 0.066 Uiso 1 1 calc R . . C55 C 0.6856(8) 0.5293(8) 0.1640(8) 0.065(4) Uani 1 1 d . . . H55 H 0.7489 0.5324 0.1828 0.078 Uiso 1 1 calc R . . C56 C 0.6190(8) 0.4612(7) 0.1523(8) 0.067(4) Uani 1 1 d . . . H56 H 0.6384 0.4192 0.1644 0.080 Uiso 1 1 calc R . . C57 C 0.5036(6) 0.5126(5) 0.1080(5) 0.036(2) Uani 1 1 d . . . C58 C 0.5678(7) 0.5839(6) 0.1186(6) 0.043(2) Uani 1 1 d . . . C59 C 0.3783(7) 0.5645(6) 0.0593(5) 0.042(2) Uani 1 1 d . . . C60 C 0.4081(6) 0.5061(5) 0.0799(5) 0.035(2) Uani 1 1 d . . . C61 C -0.3584(8) 1.1090(9) 0.5998(6) 0.060(3) Uani 1 1 d . . . H61 H -0.3449 1.1265 0.6529 0.071 Uiso 1 1 calc R . . C62 C -0.3707(9) 1.1638(10) 0.5716(7) 0.078(5) Uani 1 1 d . . . H62 H -0.3659 1.2188 0.6053 0.093 Uiso 1 1 calc R . . C63 C -0.3901(9) 1.1433(10) 0.4957(8) 0.076(4) Uani 1 1 d . . . H63 H -0.3994 1.1825 0.4759 0.092 Uiso 1 1 calc R . . C64 C -0.4141(8) 1.0305(10) 0.3655(7) 0.070(4) Uani 1 1 d . . . H64 H -0.4216 1.0677 0.3429 0.084 Uiso 1 1 calc R . . C65 C -0.4207(7) 0.9529(8) 0.3220(6) 0.055(3) Uani 1 1 d . . . H65 H -0.4317 0.9351 0.2687 0.066 Uiso 1 1 calc R . . C66 C -0.4224(7) 0.8121(9) 0.3129(6) 0.058(4) Uani 1 1 d . . . H66 H -0.4361 0.7903 0.2595 0.070 Uiso 1 1 calc R . . C67 C -0.4140(8) 0.7627(9) 0.3473(7) 0.065(4) Uani 1 1 d . . . H67 H -0.4246 0.7058 0.3190 0.078 Uiso 1 1 calc R . . C68 C -0.3899(9) 0.7931(9) 0.4238(7) 0.067(4) Uani 1 1 d . . . H68 H -0.3789 0.7573 0.4473 0.081 Uiso 1 1 calc R . . C69 C -0.3899(6) 0.9255(8) 0.4341(5) 0.052(3) Uani 1 1 d . . . C70 C -0.4116(6) 0.8970(8) 0.3538(5) 0.053(3) Uani 1 1 d . . . C71 C -0.3954(8) 1.0605(9) 0.4482(6) 0.061(3) Uani 1 1 d . . . C72 C -0.3827(6) 1.0092(8) 0.4816(5) 0.050(3) Uani 1 1 d . . . O001 O 0.2205(3) 0.5479(3) 0.5094(2) 0.0112(6) Uiso 1 1 d . . . O002 O 0.3334(3) 0.4735(3) 0.4847(2) 0.0112(6) Uiso 1 1 d . . . O003 O 0.6625(7) 0.6712(6) 0.8669(6) 0.084(4) Uiso 0.97(3) 1 d P . . O004 O 0.1649(9) 0.3829(8) 0.1918(7) 0.057(5) Uiso 0.61(3) 1 d P . . O005 O 0.8077(9) 0.3547(8) 0.1727(7) 0.076(5) Uiso 0.74(3) 1 d P . . O006 O 0.9551(12) 0.7732(10) 0.6604(9) 0.094(7) Uiso 0.68(3) 1 d P . . O007 O 0.9302(14) 0.6666(12) 0.5194(11) 0.102(9) Uiso 0.60(3) 1 d P . . O008 O 0.5359(16) 0.5266(14) 0.3211(13) 0.135(11) Uiso 0.68(4) 1 d P . . O009 O 0.5975(14) 0.2394(12) 0.3443(11) 0.155(10) Uiso 0.88(4) 1 d P . . O010 O 0.0968(15) 0.5022(14) 0.5746(12) 0.003(8) Uiso 0.175(19) 1 d P . . 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 0.0200(2) 0.0209(2) 0.0183(2) 0.00690(15) 0.00183(14) 0.00500(14) S1 0.0196(9) 0.0251(10) 0.0280(10) 0.0162(8) 0.0049(7) 0.0071(7) S2 0.0166(9) 0.0239(10) 0.0310(10) 0.0120(8) 0.0024(7) 0.0020(7) S3 0.0263(10) 0.0191(10) 0.0291(10) 0.0096(8) 0.0008(8) 0.0037(8) S4 0.0179(9) 0.0261(10) 0.0276(10) 0.0146(8) 0.0026(7) 0.0065(7) S5 0.0454(13) 0.0339(13) 0.0282(11) 0.0052(9) -0.0042(10) 0.0098(10) S6 0.0274(10) 0.0283(11) 0.0283(10) 0.0083(9) 0.0030(8) 0.0124(8) S7 0.0430(14) 0.080(2) 0.0250(11) 0.0248(13) 0.0055(10) 0.0090(13) S8 0.0495(15) 0.0463(15) 0.0707(18) 0.0404(14) -0.0195(13) 0.0004(12) N1 0.029(4) 0.027(4) 0.035(4) 0.015(3) 0.003(3) 0.002(3) N2 0.023(3) 0.035(4) 0.037(4) 0.023(3) 0.004(3) 0.006(3) N3 0.037(4) 0.055(6) 0.028(4) 0.016(4) 0.008(3) 0.002(4) N4 0.031(4) 0.073(6) 0.027(4) 0.020(4) 0.001(3) -0.001(4) N5 0.026(4) 0.031(4) 0.057(5) 0.005(4) -0.004(4) -0.001(3) N6 0.035(4) 0.029(4) 0.070(6) 0.015(4) -0.013(4) 0.004(3) N7 0.032(5) 0.091(8) 0.031(4) 0.005(5) 0.005(4) 0.003(5) N8 0.037(5) 0.091(8) 0.032(4) 0.008(5) -0.004(4) 0.010(5) O1 0.021(3) 0.023(3) 0.023(3) 0.009(2) 0.003(2) 0.005(2) O2 0.022(3) 0.020(3) 0.027(3) 0.008(2) 0.005(2) 0.005(2) O3 0.025(3) 0.021(3) 0.021(3) 0.009(2) 0.001(2) 0.001(2) O4 0.018(3) 0.027(3) 0.028(3) 0.017(2) 0.000(2) 0.007(2) O5 0.040(4) 0.071(5) 0.042(4) 0.038(4) 0.014(3) 0.020(3) O6 0.046(4) 0.027(3) 0.029(3) 0.008(3) -0.003(3) 0.009(3) O7 0.032(3) 0.031(3) 0.029(3) 0.009(3) 0.002(2) 0.012(3) O8 0.029(3) 0.036(3) 0.026(3) 0.013(3) 0.002(2) 0.009(3) O9 0.031(3) 0.039(3) 0.027(3) 0.018(3) 0.006(2) 0.017(3) O10 0.023(3) 0.030(3) 0.045(3) 0.025(3) 0.004(2) 0.001(2) O11 0.020(3) 0.031(3) 0.032(3) 0.010(3) -0.003(2) 0.004(2) O12 0.020(3) 0.036(3) 0.048(4) 0.020(3) 0.016(3) 0.006(2) O13 0.037(3) 0.023(3) 0.044(4) 0.015(3) 0.003(3) 0.004(3) O14 0.039(3) 0.035(3) 0.024(3) 0.007(3) 0.001(2) 0.009(3) O15 0.024(3) 0.029(3) 0.031(3) 0.017(2) 0.007(2) 0.010(2) O16 0.021(3) 0.032(3) 0.043(3) 0.019(3) 0.000(2) 0.006(2) O17A 0.062(4) 0.062(5) 0.055(4) -0.004(3) -0.011(3) 0.003(3) O18A 0.062(4) 0.062(5) 0.055(4) -0.004(3) -0.011(3) 0.003(3) O19A 0.062(4) 0.062(5) 0.055(4) -0.004(3) -0.011(3) 0.003(3) O17B 0.062(4) 0.062(5) 0.055(4) -0.004(3) -0.011(3) 0.003(3) O18B 0.062(4) 0.062(5) 0.055(4) -0.004(3) -0.011(3) 0.003(3) O19B 0.062(4) 0.062(5) 0.055(4) -0.004(3) -0.011(3) 0.003(3) O20 0.039(4) 0.044(4) 0.060(4) 0.023(3) 0.023(3) 0.023(3) O21 0.048(4) 0.032(4) 0.037(4) -0.003(3) -0.009(3) 0.014(3) O22 0.040(4) 0.033(3) 0.038(3) 0.012(3) -0.001(3) 0.016(3) O23 0.062(5) 0.072(5) 0.051(4) 0.040(4) 0.019(4) 0.013(4) O24 0.056(5) 0.179(11) 0.043(4) 0.065(6) 0.011(4) 0.031(6) O25 0.065(5) 0.082(6) 0.029(4) 0.008(4) 0.009(3) 0.002(4) O26A 0.059(4) 0.086(5) 0.064(5) 0.051(5) -0.002(5) 0.022(4) O27A 0.059(4) 0.086(5) 0.064(5) 0.051(5) -0.002(5) 0.022(4) O28A 0.059(4) 0.086(5) 0.064(5) 0.051(5) -0.002(5) 0.022(4) O26B 0.059(4) 0.086(5) 0.064(5) 0.051(5) -0.002(5) 0.022(4) O27B 0.059(4) 0.086(5) 0.064(5) 0.051(5) -0.002(5) 0.022(4) O28B 0.059(4) 0.086(5) 0.064(5) 0.051(5) -0.002(5) 0.022(4) C1 0.020(4) 0.024(4) 0.024(4) 0.014(3) 0.003(3) 0.003(3) C2 0.020(4) 0.020(4) 0.024(4) 0.011(3) 0.004(3) 0.004(3) C3 0.021(4) 0.022(4) 0.019(4) 0.007(3) -0.001(3) 0.007(3) C4 0.019(4) 0.028(4) 0.024(4) 0.012(3) -0.001(3) 0.008(3) C5 0.021(4) 0.030(4) 0.020(4) 0.011(3) 0.001(3) 0.004(3) C6 0.022(4) 0.023(4) 0.018(4) 0.009(3) -0.004(3) 0.002(3) C7 0.020(4) 0.017(4) 0.025(4) 0.008(3) -0.002(3) -0.002(3) C8 0.019(4) 0.028(4) 0.029(4) 0.006(4) 0.002(3) -0.002(3) C9 0.027(4) 0.043(5) 0.019(4) 0.013(4) 0.004(3) 0.005(4) C10 0.024(4) 0.028(4) 0.028(4) 0.016(4) -0.007(3) -0.003(3) C11 0.020(4) 0.022(4) 0.025(4) 0.007(3) 0.000(3) 0.000(3) C12 0.027(4) 0.027(4) 0.024(4) 0.012(3) 0.003(3) 0.006(3) C13 0.031(4) 0.022(4) 0.029(4) 0.015(3) 0.004(3) 0.006(3) C14 0.032(4) 0.031(5) 0.030(4) 0.016(4) -0.002(3) 0.007(4) C15 0.023(4) 0.034(5) 0.033(4) 0.016(4) 0.005(3) 0.010(3) C16 0.029(4) 0.022(4) 0.022(4) 0.010(3) 0.003(3) 0.005(3) C17 0.021(4) 0.023(4) 0.032(4) 0.018(3) 0.008(3) 0.008(3) C18 0.023(4) 0.036(5) 0.028(4) 0.018(4) 0.002(3) 0.007(3) C19 0.023(4) 0.034(5) 0.024(4) 0.013(4) 0.004(3) 0.004(3) C20 0.022(4) 0.022(4) 0.033(4) 0.012(3) 0.010(3) 0.005(3) C21 0.017(4) 0.026(4) 0.034(4) 0.020(4) 0.008(3) 0.003(3) C22 0.021(4) 0.023(4) 0.018(3) 0.009(3) -0.002(3) 0.007(3) C23 0.015(3) 0.018(4) 0.028(4) 0.011(3) -0.002(3) -0.004(3) C24 0.028(4) 0.019(4) 0.020(4) 0.007(3) 0.004(3) 0.007(3) C25 0.030(5) 0.033(5) 0.058(6) 0.028(5) 0.015(4) 0.009(4) C26 0.033(5) 0.038(5) 0.067(7) 0.035(5) 0.017(5) 0.014(4) C27 0.023(4) 0.048(6) 0.065(6) 0.040(5) 0.010(4) 0.013(4) C28 0.021(4) 0.060(7) 0.047(6) 0.034(5) -0.005(4) -0.001(4) C29 0.027(5) 0.055(6) 0.037(5) 0.019(5) 0.003(4) -0.008(4) C30 0.041(5) 0.040(6) 0.039(5) 0.012(4) 0.017(4) -0.009(4) C31 0.037(5) 0.036(5) 0.048(6) 0.020(4) 0.019(4) 0.002(4) C32 0.029(4) 0.036(5) 0.045(5) 0.021(4) 0.009(4) 0.009(4) C33 0.024(4) 0.035(5) 0.032(4) 0.019(4) 0.009(3) 0.001(3) C34 0.027(4) 0.037(5) 0.034(5) 0.016(4) 0.007(4) -0.004(4) C35 0.018(4) 0.048(6) 0.043(5) 0.033(4) 0.003(3) 0.001(4) C36 0.024(4) 0.036(5) 0.033(4) 0.024(4) 0.006(3) 0.000(4) C37 0.051(6) 0.071(8) 0.039(5) 0.026(5) 0.007(5) 0.006(6) C38 0.036(5) 0.100(10) 0.025(5) 0.026(6) 0.004(4) 0.007(6) C39 0.037(5) 0.079(8) 0.017(4) 0.007(5) 0.007(4) 0.002(5) C40 0.040(6) 0.062(8) 0.030(5) 0.001(5) 0.004(4) -0.001(5) C41 0.045(6) 0.060(7) 0.053(7) 0.009(6) 0.005(5) 0.003(5) C42 0.059(8) 0.086(10) 0.075(9) 0.039(8) 0.008(7) 0.011(7) C43 0.054(7) 0.097(11) 0.051(7) 0.044(7) -0.005(5) 0.009(7) C44 0.036(6) 0.114(12) 0.033(5) 0.031(6) 0.006(4) 0.013(6) C45 0.026(5) 0.076(8) 0.027(5) 0.018(5) 0.006(4) 0.001(5) C46 0.041(6) 0.063(8) 0.044(6) 0.019(5) 0.005(5) 0.006(5) C47 0.016(4) 0.072(8) 0.027(5) 0.007(5) 0.005(3) -0.002(4) C48 0.021(4) 0.066(7) 0.024(4) 0.012(4) 0.003(3) -0.006(4) C49 0.025(5) 0.055(7) 0.059(7) -0.008(5) -0.006(5) 0.003(5) C50 0.035(6) 0.070(8) 0.047(6) 0.001(6) -0.010(5) 0.017(6) C51 0.059(7) 0.066(8) 0.036(5) 0.010(5) 0.007(5) 0.038(6) C52 0.067(7) 0.030(5) 0.049(6) 0.017(5) 0.025(5) 0.022(5) C53 0.048(6) 0.022(5) 0.066(7) 0.014(5) 0.016(5) 0.008(4) C54 0.037(6) 0.040(6) 0.071(7) 0.012(5) -0.005(5) -0.015(5) C55 0.035(6) 0.068(8) 0.089(9) 0.036(7) -0.020(6) -0.006(6) C56 0.051(7) 0.049(7) 0.091(9) 0.024(7) -0.035(6) 0.003(5) C57 0.032(5) 0.023(5) 0.048(5) 0.010(4) -0.005(4) -0.003(4) C58 0.034(5) 0.028(5) 0.053(6) 0.004(4) 0.007(4) 0.001(4) C59 0.046(6) 0.039(6) 0.040(5) 0.009(4) 0.009(4) 0.021(4) C60 0.032(5) 0.020(4) 0.042(5) 0.001(4) -0.002(4) 0.004(4) C61 0.049(7) 0.085(10) 0.038(6) 0.020(7) 0.013(5) -0.002(6) C62 0.055(8) 0.103(12) 0.044(7) 0.002(7) 0.016(6) -0.012(7) C63 0.063(8) 0.109(12) 0.066(8) 0.042(9) 0.024(7) 0.011(8) C64 0.042(6) 0.121(13) 0.044(6) 0.031(8) 0.008(5) 0.004(7) C65 0.032(5) 0.093(10) 0.026(5) 0.012(6) 0.002(4) 0.000(6) C66 0.025(5) 0.098(10) 0.029(5) 0.001(6) 0.005(4) 0.005(5) C67 0.044(6) 0.081(9) 0.046(7) -0.001(6) 0.002(5) 0.015(6) C68 0.056(7) 0.079(9) 0.054(7) 0.008(7) 0.000(6) 0.023(7) C69 0.017(4) 0.094(9) 0.031(5) 0.012(6) -0.001(4) 0.005(5) C70 0.022(5) 0.091(9) 0.029(5) 0.007(6) 0.003(4) 0.002(5) C71 0.036(6) 0.092(10) 0.039(6) 0.010(6) 0.013(5) 0.001(6) C72 0.024(5) 0.081(8) 0.030(5) 0.010(5) 0.006(4) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O3 2.300(5) . ? Tb1 O4 2.307(5) . ? Tb1 O1 2.313(5) . ? Tb1 O2 2.318(5) . ? Tb1 O5 2.417(6) . ? Tb1 O6 2.420(6) . ? Tb1 O7 2.453(6) . ? Tb1 O8 2.482(6) . ? S1 O9 1.428(6) . ? S1 O10 1.452(6) . ? S1 C1 1.762(8) . ? S1 C2 1.775(8) . ? S2 O11 1.430(6) . ? S2 O12 1.447(6) . ? S2 C6 1.759(8) . ? S2 C7 1.768(8) . ? S3 O14 1.433(6) . ? S3 O13 1.443(6) . ? S3 C11 1.767(8) . ? S3 C12 1.774(8) . ? S4 O16 1.446(6) . ? S4 O15 1.447(6) . ? S4 C17 1.778(8) . ? S4 C16 1.792(8) . ? S5 O18B 1.390(13) . ? S5 O19B 1.398(15) . ? S5 O19A 1.40(3) . ? S5 O17B 1.444(15) . ? S5 O17A 1.45(3) . ? S5 O18A 1.53(3) . ? S5 C19 1.774(8) . ? S6 O21 1.445(6) . ? S6 O20 1.445(7) . ? S6 O22 1.461(7) . ? S6 C4 1.766(8) . ? S7 O25 1.444(9) . ? S7 O23 1.446(8) . ? S7 O24 1.458(9) . ? S7 C9 1.767(8) . ? S8 O26B 1.38(2) . ? S8 O27A 1.380(19) . ? S8 O28A 1.399(16) . ? S8 O27B 1.52(3) . ? S8 O28B 1.54(2) . ? S8 O26A 1.546(16) . ? S8 C14 1.779(8) . ? N1 C25 1.337(12) . ? N1 C36 1.354(11) . ? N2 C32 1.325(12) . ? N2 C33 1.335(11) . ? N3 C37 1.317(14) . ? N3 C48 1.333(14) . ? N4 C44 1.329(15) . ? N4 C45 1.355(12) . ? N5 C49 1.354(12) . ? N5 C60 1.369(12) . ? N6 C56 1.337(13) . ? N6 C57 1.348(12) . ? N7 C61 1.333(16) . ? N7 C72 1.342(13) . ? N8 C68 1.336(16) . ? N8 C69 1.345(16) . ? O1 C21 1.280(9) . ? O2 C22 1.280(9) . ? O3 C23 1.278(9) . ? O4 C24 1.271(9) . ? C1 C20 1.380(11) . ? C1 C21 1.449(11) . ? C2 C3 1.380(11) . ? C2 C22 1.431(11) . ? C3 C4 1.409(11) . ? C3 H3 0.9500 . ? C4 C5 1.380(11) . ? C5 C6 1.386(11) . ? C5 H5 0.9500 . ? C6 C22 1.446(11) . ? C7 C8 1.397(11) . ? C7 C23 1.445(11) . ? C8 C9 1.384(12) . ? C8 H8 0.9500 . ? C9 C10 1.392(12) . ? C10 C11 1.379(11) . ? C10 H10 0.9500 . ? C11 C23 1.426(11) . ? C12 C13 1.371(11) . ? C12 C24 1.422(11) . ? C13 C14 1.393(12) . ? C13 H13 0.9500 . ? C14 C15 1.386(12) . ? C15 C16 1.363(11) . ? C15 H15 0.9500 . ? C16 C24 1.426(11) . ? C17 C18 1.386(11) . ? C17 C21 1.439(11) . ? C18 C19 1.366(12) . ? C18 H18 0.9500 . ? C19 C20 1.402(11) . ? C20 H20 0.9500 . ? C25 C26 1.383(13) . ? C25 H25 0.9500 . ? C26 C27 1.368(14) . ? C26 H26 0.9500 . ? C27 C35 1.413(14) . ? C27 H27 0.9500 . ? C28 C29 1.339(15) . ? C28 C35 1.434(13) . ? C28 H28 0.9500 . ? C29 C34 1.444(14) . ? C29 H29 0.9500 . ? C30 C31 1.372(14) . ? C30 C34 1.384(14) . ? C30 H30 0.9500 . ? C31 C32 1.418(13) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.418(12) . ? C33 C36 1.447(13) . ? C35 C36 1.400(12) . ? C37 C38 1.421(14) . ? C37 H37 0.9500 . ? C38 C39 1.342(17) . ? C38 H38 0.9500 . ? C39 C47 1.395(16) . ? C39 H39 0.9500 . ? C40 C41 1.352(17) . ? C40 C47 1.373(16) . ? C40 H40 0.9500 . ? C41 C46 1.419(15) . ? C41 H41 0.9500 . ? C42 C43 1.324(18) . ? C42 C46 1.406(17) . ? C42 H42 0.9500 . ? C43 C44 1.394(19) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.398(16) . ? C45 C48 1.431(15) . ? C47 C48 1.438(12) . ? C49 C50 1.398(18) . ? C49 H49 0.9500 . ? C50 C51 1.374(17) . ? C50 H50 0.9500 . ? C51 C59 1.404(15) . ? C51 H51 0.9500 . ? C52 C53 1.329(15) . ? C52 C59 1.445(15) . ? C52 H52 0.9500 . ? C53 C58 1.425(15) . ? C53 H53 0.9500 . ? C54 C55 1.320(17) . ? C54 C58 1.408(15) . ? C54 H54 0.9500 . ? C55 C56 1.395(16) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C60 1.424(13) . ? C57 C58 1.425(12) . ? C59 C60 1.377(14) . ? C61 C62 1.33(2) . ? C61 H61 0.9500 . ? C62 C63 1.370(18) . ? C62 H62 0.9500 . ? C63 C71 1.42(2) . ? C63 H63 0.9500 . ? C64 C65 1.321(19) . ? C64 C71 1.471(16) . ? C64 H64 0.9500 . ? C65 C70 1.391(18) . ? C65 H65 0.9500 . ? C66 C67 1.321(19) . ? C66 C70 1.418(18) . ? C66 H66 0.9500 . ? C67 C68 1.368(17) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C72 1.427(17) . ? C69 C70 1.433(13) . ? C71 C72 1.349(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Tb1 O4 80.54(18) . . ? O3 Tb1 O1 142.40(18) . . ? O4 Tb1 O1 72.67(18) . . ? O3 Tb1 O2 73.39(18) . . ? O4 Tb1 O2 81.11(19) . . ? O1 Tb1 O2 76.75(18) . . ? O3 Tb1 O5 138.5(2) . . ? O4 Tb1 O5 140.8(2) . . ? O1 Tb1 O5 73.4(2) . . ? O2 Tb1 O5 109.4(2) . . ? O3 Tb1 O6 77.9(2) . . ? O4 Tb1 O6 118.02(19) . . ? O1 Tb1 O6 138.2(2) . . ? O2 Tb1 O6 142.2(2) . . ? O5 Tb1 O6 77.2(2) . . ? O3 Tb1 O7 123.70(19) . . ? O4 Tb1 O7 75.08(19) . . ? O1 Tb1 O7 74.34(19) . . ? O2 Tb1 O7 146.83(18) . . ? O5 Tb1 O7 77.4(2) . . ? O6 Tb1 O7 70.7(2) . . ? O3 Tb1 O8 72.91(19) . . ? O4 Tb1 O8 147.84(19) . . ? O1 Tb1 O8 119.81(19) . . ? O2 Tb1 O8 74.22(18) . . ? O5 Tb1 O8 68.6(2) . . ? O6 Tb1 O8 74.1(2) . . ? O7 Tb1 O8 135.28(18) . . ? O9 S1 O10 117.9(4) . . ? O9 S1 C1 110.7(4) . . ? O10 S1 C1 107.0(3) . . ? O9 S1 C2 109.5(4) . . ? O10 S1 C2 105.2(3) . . ? C1 S1 C2 105.7(4) . . ? O11 S2 O12 115.7(4) . . ? O11 S2 C6 107.5(3) . . ? O12 S2 C6 106.4(4) . . ? O11 S2 C7 109.4(4) . . ? O12 S2 C7 106.2(4) . . ? C6 S2 C7 111.7(3) . . ? O14 S3 O13 117.8(4) . . ? O14 S3 C11 111.5(4) . . ? O13 S3 C11 107.5(4) . . ? O14 S3 C12 107.9(4) . . ? O13 S3 C12 106.9(4) . . ? C11 S3 C12 104.3(4) . . ? O16 S4 O15 116.2(3) . . ? O16 S4 C17 107.2(4) . . ? O15 S4 C17 108.7(3) . . ? O16 S4 C16 105.4(4) . . ? O15 S4 C16 106.6(3) . . ? C17 S4 C16 112.9(4) . . ? O18B S5 O19B 115.8(8) . . ? O18B S5 O19A 144.1(11) . . ? O19B S5 O19A 51.7(13) . . ? O18B S5 O17B 111.0(8) . . ? O19B S5 O17B 111.3(8) . . ? O19A S5 O17B 60.6(14) . . ? O18B S5 O17A 58.0(12) . . ? O19B S5 O17A 146.5(11) . . ? O19A S5 O17A 111.4(17) . . ? O17B S5 O17A 54.7(12) . . ? O18B S5 O18A 51.9(12) . . ? O19B S5 O18A 66.2(12) . . ? O19A S5 O18A 113.9(16) . . ? O17B S5 O18A 146.6(11) . . ? O17A S5 O18A 107.6(16) . . ? O18B S5 C19 106.6(6) . . ? O19B S5 C19 106.4(6) . . ? O19A S5 C19 109.3(10) . . ? O17B S5 C19 104.9(5) . . ? O17A S5 C19 106.8(10) . . ? O18A S5 C19 107.6(10) . . ? O21 S6 O20 112.9(4) . . ? O21 S6 O22 111.1(4) . . ? O20 S6 O22 112.7(4) . . ? O21 S6 C4 106.4(4) . . ? O20 S6 C4 106.0(4) . . ? O22 S6 C4 107.2(4) . . ? O25 S7 O23 112.1(5) . . ? O25 S7 O24 113.6(6) . . ? O23 S7 O24 112.4(6) . . ? O25 S7 C9 106.1(5) . . ? O23 S7 C9 105.3(4) . . ? O24 S7 C9 106.6(4) . . ? O26B S8 O27A 135.0(12) . . ? O26B S8 O28A 75.3(11) . . ? O27A S8 O28A 113.5(9) . . ? O26B S8 O27B 121.1(13) . . ? O27A S8 O27B 24.8(9) . . ? O28A S8 O27B 135.8(10) . . ? O26B S8 O28B 109.3(12) . . ? O27A S8 O28B 88.7(11) . . ? O28A S8 O28B 33.9(8) . . ? O27B S8 O28B 113.5(12) . . ? O26B S8 O26A 36.2(9) . . ? O27A S8 O26A 108.4(10) . . ? O28A S8 O26A 109.7(9) . . ? O27B S8 O26A 87.8(11) . . ? O28B S8 O26A 142.5(10) . . ? O26B S8 C14 106.9(8) . . ? O27A S8 C14 109.5(7) . . ? O28A S8 C14 111.6(7) . . ? O27B S8 C14 102.4(8) . . ? O28B S8 C14 101.3(7) . . ? O26A S8 C14 103.7(6) . . ? C25 N1 C36 122.0(8) . . ? C32 N2 C33 116.6(8) . . ? C37 N3 C48 123.0(9) . . ? C44 N4 C45 114.2(11) . . ? C49 N5 C60 121.0(10) . . ? C56 N6 C57 117.2(9) . . ? C61 N7 C72 116.5(12) . . ? C68 N8 C69 121.1(10) . . ? C21 O1 Tb1 133.1(5) . . ? C22 O2 Tb1 152.5(5) . . ? C23 O3 Tb1 128.2(4) . . ? C24 O4 Tb1 149.4(5) . . ? C20 C1 C21 121.7(7) . . ? C20 C1 S1 115.8(6) . . ? C21 C1 S1 122.4(6) . . ? C3 C2 C22 123.7(7) . . ? C3 C2 S1 118.2(6) . . ? C22 C2 S1 118.0(6) . . ? C2 C3 C4 119.4(7) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 119.3(7) . . ? C5 C4 S6 120.9(6) . . ? C3 C4 S6 119.7(6) . . ? C4 C5 C6 121.7(7) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C22 121.4(7) . . ? C5 C6 S2 117.5(6) . . ? C22 C6 S2 120.6(6) . . ? C8 C7 C23 122.2(7) . . ? C8 C7 S2 116.7(6) . . ? C23 C7 S2 120.8(6) . . ? C9 C8 C7 120.2(8) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 119.8(7) . . ? C8 C9 S7 121.3(7) . . ? C10 C9 S7 118.9(7) . . ? C11 C10 C9 120.2(8) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C23 123.4(8) . . ? C10 C11 S3 115.0(6) . . ? C23 C11 S3 121.6(6) . . ? C13 C12 C24 124.5(7) . . ? C13 C12 S3 119.2(6) . . ? C24 C12 S3 116.1(6) . . ? C12 C13 C14 118.5(8) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C15 C14 C13 119.9(8) . . ? C15 C14 S8 121.5(6) . . ? C13 C14 S8 118.6(6) . . ? C16 C15 C14 120.5(8) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C24 122.9(7) . . ? C15 C16 S4 116.8(6) . . ? C24 C16 S4 119.4(6) . . ? C18 C17 C21 123.0(7) . . ? C18 C17 S4 115.6(6) . . ? C21 C17 S4 120.8(6) . . ? C19 C18 C17 120.6(7) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 119.6(7) . . ? C18 C19 S5 122.1(6) . . ? C20 C19 S5 118.3(6) . . ? C1 C20 C19 121.0(8) . . ? C1 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? O1 C21 C17 124.1(7) . . ? O1 C21 C1 121.9(7) . . ? C17 C21 C1 114.0(7) . . ? O2 C22 C2 122.4(7) . . ? O2 C22 C6 123.2(7) . . ? C2 C22 C6 114.4(7) . . ? O3 C23 C11 123.4(7) . . ? O3 C23 C7 122.6(7) . . ? C11 C23 C7 114.1(7) . . ? O4 C24 C12 122.2(7) . . ? O4 C24 C16 124.4(7) . . ? C12 C24 C16 113.4(7) . . ? N1 C25 C26 119.8(9) . . ? N1 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 120.5(9) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C35 119.6(8) . . ? C26 C27 H27 120.2 . . ? C35 C27 H27 120.2 . . ? C29 C28 C35 121.2(9) . . ? C29 C28 H28 119.4 . . ? C35 C28 H28 119.4 . . ? C28 C29 C34 121.8(9) . . ? C28 C29 H29 119.1 . . ? C34 C29 H29 119.1 . . ? C31 C30 C34 120.8(9) . . ? C31 C30 H30 119.6 . . ? C34 C30 H30 119.6 . . ? C30 C31 C32 117.7(9) . . ? C30 C31 H31 121.1 . . ? C32 C31 H31 121.1 . . ? N2 C32 C31 123.8(9) . . ? N2 C32 H32 118.1 . . ? C31 C32 H32 118.1 . . ? N2 C33 C34 125.0(8) . . ? N2 C33 C36 117.0(8) . . ? C34 C33 C36 118.0(8) . . ? C30 C34 C33 116.1(8) . . ? C30 C34 C29 124.9(9) . . ? C33 C34 C29 119.0(9) . . ? C36 C35 C27 117.9(8) . . ? C36 C35 C28 118.5(9) . . ? C27 C35 C28 123.6(8) . . ? N1 C36 C35 120.1(8) . . ? N1 C36 C33 118.4(7) . . ? C35 C36 C33 121.4(8) . . ? N3 C37 C38 119.4(12) . . ? N3 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C39 C38 C37 119.7(11) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C47 121.2(9) . . ? C38 C39 H39 119.4 . . ? C47 C39 H39 119.4 . . ? C41 C40 C47 121.2(10) . . ? C41 C40 H40 119.4 . . ? C47 C40 H40 119.4 . . ? C40 C41 C46 122.2(12) . . ? C40 C41 H41 118.9 . . ? C46 C41 H41 118.9 . . ? C43 C42 C46 122.3(14) . . ? C43 C42 H42 118.9 . . ? C46 C42 H42 118.9 . . ? C42 C43 C44 117.3(12) . . ? C42 C43 H43 121.3 . . ? C44 C43 H43 121.3 . . ? N4 C44 C43 125.8(11) . . ? N4 C44 H44 117.1 . . ? C43 C44 H44 117.1 . . ? N4 C45 C46 125.6(10) . . ? N4 C45 C48 115.5(10) . . ? C46 C45 C48 118.9(9) . . ? C45 C46 C42 114.8(11) . . ? C45 C46 C41 118.8(11) . . ? C42 C46 C41 126.4(12) . . ? C40 C47 C39 124.0(9) . . ? C40 C47 C48 119.1(10) . . ? C39 C47 C48 116.9(10) . . ? N3 C48 C45 120.5(8) . . ? N3 C48 C47 119.8(9) . . ? C45 C48 C47 119.7(10) . . ? N5 C49 C50 120.6(11) . . ? N5 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? C51 C50 C49 118.5(10) . . ? C51 C50 H50 120.8 . . ? C49 C50 H50 120.8 . . ? C50 C51 C59 120.9(11) . . ? C50 C51 H51 119.6 . . ? C59 C51 H51 119.6 . . ? C53 C52 C59 120.9(10) . . ? C53 C52 H52 119.5 . . ? C59 C52 H52 119.5 . . ? C52 C53 C58 121.9(9) . . ? C52 C53 H53 119.0 . . ? C58 C53 H53 119.0 . . ? C55 C54 C58 120.2(10) . . ? C55 C54 H54 119.9 . . ? C58 C54 H54 119.9 . . ? C54 C55 C56 120.1(10) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? N6 C56 C55 123.1(11) . . ? N6 C56 H56 118.5 . . ? C55 C56 H56 118.5 . . ? N6 C57 C60 119.0(8) . . ? N6 C57 C58 122.7(9) . . ? C60 C57 C58 118.3(9) . . ? C54 C58 C57 116.7(10) . . ? C54 C58 C53 124.7(9) . . ? C57 C58 C53 118.6(9) . . ? C60 C59 C51 118.8(10) . . ? C60 C59 C52 118.4(9) . . ? C51 C59 C52 122.9(10) . . ? N5 C60 C59 120.3(9) . . ? N5 C60 C57 118.0(8) . . ? C59 C60 C57 121.7(9) . . ? C62 C61 N7 122.5(11) . . ? C62 C61 H61 118.7 . . ? N7 C61 H61 118.7 . . ? C61 C62 C63 122.1(15) . . ? C61 C62 H62 119.0 . . ? C63 C62 H62 119.0 . . ? C62 C63 C71 116.5(15) . . ? C62 C63 H63 121.8 . . ? C71 C63 H63 121.8 . . ? C65 C64 C71 121.5(14) . . ? C65 C64 H64 119.3 . . ? C71 C64 H64 119.3 . . ? C64 C65 C70 120.4(11) . . ? C64 C65 H65 119.8 . . ? C70 C65 H65 119.8 . . ? C67 C66 C70 121.5(10) . . ? C67 C66 H66 119.3 . . ? C70 C66 H66 119.3 . . ? C66 C67 C68 120.2(13) . . ? C66 C67 H67 119.9 . . ? C68 C67 H67 119.9 . . ? N8 C68 C67 121.2(14) . . ? N8 C68 H68 119.4 . . ? C67 C68 H68 119.4 . . ? N8 C69 C72 119.0(9) . . ? N8 C69 C70 119.8(11) . . ? C72 C69 C70 121.1(12) . . ? C65 C70 C66 125.0(10) . . ? C65 C70 C69 118.9(12) . . ? C66 C70 C69 116.1(12) . . ? C72 C71 C63 117.4(11) . . ? C72 C71 C64 120.5(13) . . ? C63 C71 C64 122.1(14) . . ? N7 C72 C71 125.1(12) . . ? N7 C72 C69 117.4(12) . . ? C71 C72 C69 117.6(10) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.204 _refine_diff_density_min -1.819 _refine_diff_density_rms 0.192 ###END # Attachment 'macro-data-squeeze-090115.CIF' data_1a _database_code_depnum_ccdc_archive 'CCDC 715073' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'H5 Gd(H2O)4 (C24H8O24S8) (C12H8N2)4' _chemical_melting_point ? _chemical_formula_moiety 'H5 Gd(H2O)4 [C24H8O24S8] [C12H8N2]4' _chemical_formula_sum 'C72 H53 Gd N8 O28 S8' _chemical_formula_weight 1891.95 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 14.3385(8) _cell_length_b 18.1828(10) _cell_length_c 19.2533(11) _cell_angle_alpha 112.5980(10) _cell_angle_beta 92.7530(10) _cell_angle_gamma 97.7220(10) _cell_volume 4564.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7983 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 26.52 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1914 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7224 _exptl_absorpt_correction_T_max 0.9342 _exptl_absorpt_process_details ; SADABS, Sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 AXS Apex CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 33441 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.00 _reflns_number_total 17622 _reflns_number_gt 14144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (1998)' _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. In order to subtract the contribution from the disordered solvent molecules, the SQUEEZE command was used. All the non-hydrogen atoms were refined anisotropically. The oxygen atoms of two sulfonate groups (O17-O19, O26-O28) were refined with disordered positions and the same displacement parameters for all oxygen atoms on one sulfonate group. The short contact O25...C68, C57...O26A, C37...O19A and C67...O26B might be due to the high mobility of the isolated phenanthroline molecules. ; _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^)+(0.0767P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17622 _refine_ls_number_parameters 1050 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1340 _refine_ls_wR_factor_gt 0.1274 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 0.032387(14) 0.757693(12) 0.020468(11) 0.02036(7) Uani 1 1 d . . . S1 S 0.08520(7) 1.01249(6) 0.09130(6) 0.0230(2) Uani 1 1 d . . . S2 S -0.22245(7) 0.83341(6) 0.14615(6) 0.0242(2) Uani 1 1 d . . . S3 S 0.00414(8) 0.59932(6) 0.12259(6) 0.0272(2) Uani 1 1 d . . . S4 S 0.32083(7) 0.81806(6) 0.15555(6) 0.0228(2) Uani 1 1 d . . . S5 S 0.33902(10) 1.13346(7) 0.33808(7) 0.0388(3) Uani 1 1 d . . . S6 S -0.20608(8) 1.15468(7) 0.22630(6) 0.0285(3) Uani 1 1 d . . . S7 S -0.15910(10) 0.73724(11) 0.37572(8) 0.0519(4) Uani 1 1 d . . . S8 S 0.32650(11) 0.59807(8) 0.28255(9) 0.0517(4) Uani 1 1 d . . . N1 N -0.3733(3) 1.1533(2) 0.0585(2) 0.0302(9) Uani 1 1 d . . . N2 N -0.3131(3) 1.0094(2) 0.0106(2) 0.0270(8) Uani 1 1 d . . . N3 N 0.1062(3) 1.0600(3) 0.4574(2) 0.0458(12) Uani 1 1 d . . . N4 N 0.1438(3) 0.9946(3) 0.5584(2) 0.0500(13) Uani 1 1 d . . . N5 N 0.3464(3) 0.4388(2) 0.0733(2) 0.0431(11) Uani 1 1 d . . . N6 N 0.5321(3) 0.4517(2) 0.1235(3) 0.0488(12) Uani 1 1 d . . . N7 N -0.3631(3) 1.0302(3) 0.5575(2) 0.0546(14) Uani 1 1 d . . . N8 N -0.3823(3) 0.8710(3) 0.4676(3) 0.0574(14) Uani 1 1 d . . . O1 O 0.1687(2) 0.85492(16) 0.05969(16) 0.0236(6) Uani 1 1 d . A . O2 O -0.01677(19) 0.86902(16) 0.11250(16) 0.0228(6) Uani 1 1 d . . . O3 O -0.0974(2) 0.70794(16) 0.06561(16) 0.0231(6) Uani 1 1 d . . . O4 O 0.1069(2) 0.75266(16) 0.12787(16) 0.0248(6) Uani 1 1 d . B . O5 O 0.0673(2) 0.7859(2) -0.0901(2) 0.0454(9) Uani 1 1 d . . . O6 O -0.0293(2) 0.63014(18) -0.08595(17) 0.0316(7) Uani 1 1 d . . . O7 O 0.1646(2) 0.68393(18) -0.02407(17) 0.0304(7) Uani 1 1 d . . . O8 O -0.1120(2) 0.78193(17) -0.04037(16) 0.0287(7) Uani 1 1 d . . . O9 O 0.0725(2) 0.95416(18) 0.01502(17) 0.0311(7) Uani 1 1 d . . . O10 O 0.1103(2) 1.09679(17) 0.10386(18) 0.0294(7) Uani 1 1 d . . . O11 O -0.2470(2) 0.79013(17) 0.06532(17) 0.0292(7) Uani 1 1 d . . . O12 O -0.3013(2) 0.85276(18) 0.19049(18) 0.0335(8) Uani 1 1 d . . . O13 O -0.0201(2) 0.52936(18) 0.14023(19) 0.0354(8) Uani 1 1 d . . . O14 O 0.0043(2) 0.58701(19) 0.04470(17) 0.0348(8) Uani 1 1 d . . . O15 O 0.3207(2) 0.77893(17) 0.07434(17) 0.0266(7) Uani 1 1 d . . . O16 O 0.4120(2) 0.84126(18) 0.20003(17) 0.0292(7) Uani 1 1 d . . . O17A O 0.3958(9) 1.1866(7) 0.3101(6) 0.0664(11) Uani 0.378(4) 1 d P A 1 O18A O 0.4075(9) 1.1061(7) 0.3825(6) 0.0664(11) Uani 0.378(4) 1 d P A 1 O19A O 0.2698(9) 1.1700(7) 0.3824(6) 0.0664(11) Uani 0.378(4) 1 d P A 1 O17B O 0.3131(5) 1.2033(4) 0.3224(4) 0.0664(11) Uani 0.622(4) 1 d P A 2 O18B O 0.4357(5) 1.1344(4) 0.3382(4) 0.0664(11) Uani 0.622(4) 1 d P A 2 O19B O 0.2969(5) 1.1278(4) 0.4012(4) 0.0664(11) Uani 0.622(4) 1 d P A 2 O20 O -0.2922(2) 1.1301(2) 0.2539(2) 0.0427(9) Uani 1 1 d . . . O21 O -0.1383(3) 1.2163(2) 0.28584(19) 0.0445(9) Uani 1 1 d . . . O22 O -0.2235(2) 1.17904(18) 0.16345(18) 0.0335(8) Uani 1 1 d . . . O23 O -0.2337(3) 0.6698(3) 0.3634(2) 0.0667(12) Uani 1 1 d . . . O24 O -0.0709(3) 0.7289(4) 0.4104(2) 0.0900(18) Uani 1 1 d . . . O25 O -0.1895(3) 0.8146(3) 0.4148(2) 0.0620(12) Uani 1 1 d . . . O26A O 0.4234(6) 0.5949(5) 0.2491(5) 0.0668(12) Uani 0.577(6) 1 d P B 1 O27A O 0.2813(8) 0.5204(6) 0.2655(5) 0.0668(12) Uani 0.577(6) 1 d P B 1 O28A O 0.3483(7) 0.6508(5) 0.3615(5) 0.0668(12) Uani 0.577(6) 1 d P B 1 O26B O 0.4189(9) 0.6339(7) 0.2947(7) 0.0668(12) Uani 0.423(6) 1 d P B 2 O27B O 0.2957(11) 0.5085(8) 0.2335(7) 0.0668(12) Uani 0.423(6) 1 d P B 2 O28B O 0.2885(9) 0.6229(7) 0.3563(7) 0.0668(12) Uani 0.423(6) 1 d P B 2 C1 C 0.1731(3) 0.9916(2) 0.1461(2) 0.0229(9) Uani 1 1 d . A . C2 C -0.0207(3) 1.0058(2) 0.1340(2) 0.0204(9) Uani 1 1 d . . . C3 C -0.0637(3) 1.0727(2) 0.1623(2) 0.0222(9) Uani 1 1 d . . . H3 H -0.0341 1.1226 0.1621 0.027 Uiso 1 1 calc R . . C4 C -0.1506(3) 1.0681(2) 0.1914(2) 0.0234(9) Uani 1 1 d . . . C5 C -0.1947(3) 0.9945(2) 0.1893(2) 0.0235(9) Uani 1 1 d . . . H5 H -0.2547 0.9905 0.2077 0.028 Uiso 1 1 calc R . . C6 C -0.1517(3) 0.9269(2) 0.1606(2) 0.0218(9) Uani 1 1 d . . . C7 C -0.1604(3) 0.7749(2) 0.1815(2) 0.0241(9) Uani 1 1 d . . . C8 C -0.1735(3) 0.7835(3) 0.2558(2) 0.0274(10) Uani 1 1 d . . . H8 H -0.2074 0.8235 0.2859 0.033 Uiso 1 1 calc R . . C9 C -0.1369(3) 0.7334(3) 0.2850(3) 0.0302(10) Uani 1 1 d . . . C10 C -0.0855(3) 0.6764(3) 0.2411(3) 0.0286(10) Uani 1 1 d . . . H10 H -0.0605 0.6420 0.2612 0.034 Uiso 1 1 calc R . . C11 C -0.0704(3) 0.6689(2) 0.1687(2) 0.0242(9) Uani 1 1 d . . . C12 C 0.1184(3) 0.6465(2) 0.1678(2) 0.0266(10) Uani 1 1 d . B . C13 C 0.1690(3) 0.6112(3) 0.2056(2) 0.0283(10) Uani 1 1 d . . . H13 H 0.1399 0.5645 0.2121 0.034 Uiso 1 1 calc R B . C14 C 0.2627(3) 0.6443(3) 0.2341(3) 0.0307(10) Uani 1 1 d . B . C15 C 0.3058(3) 0.7107(3) 0.2218(2) 0.0298(10) Uani 1 1 d . . . H15 H 0.3708 0.7318 0.2393 0.036 Uiso 1 1 calc R B . C16 C 0.2551(3) 0.7463(2) 0.1844(2) 0.0232(9) Uani 1 1 d . B . C17 C 0.2700(3) 0.9065(2) 0.1760(2) 0.0235(9) Uani 1 1 d . A . C18 C 0.3110(3) 0.9730(3) 0.2414(2) 0.0255(9) Uani 1 1 d . . . H18 H 0.3578 0.9668 0.2745 0.031 Uiso 1 1 calc R A . C19 C 0.2841(3) 1.0475(3) 0.2583(2) 0.0275(10) Uani 1 1 d . A . C20 C 0.2146(3) 1.0560(3) 0.2108(2) 0.0263(10) Uani 1 1 d . . . H20 H 0.1953 1.1071 0.2230 0.032 Uiso 1 1 calc R A . C21 C 0.2006(3) 0.9132(2) 0.1226(2) 0.0211(9) Uani 1 1 d . . . C22 C -0.0602(3) 0.9290(2) 0.1330(2) 0.0202(9) Uani 1 1 d . . . C23 C -0.1080(3) 0.7177(2) 0.1342(2) 0.0228(9) Uani 1 1 d . . . C24 C 0.1573(3) 0.7171(2) 0.1575(2) 0.0220(9) Uani 1 1 d . . . C25 C -0.4003(4) 1.2261(3) 0.0871(3) 0.0367(12) Uani 1 1 d . . . H25 H -0.3684 1.2663 0.1332 0.044 Uiso 1 1 calc R . . C26 C -0.4746(4) 1.2430(3) 0.0498(3) 0.0415(13) Uani 1 1 d . . . H26 H -0.4943 1.2942 0.0704 0.050 Uiso 1 1 calc R . . C27 C -0.5190(3) 1.1850(3) -0.0166(3) 0.0409(13) Uani 1 1 d . . . H27 H -0.5697 1.1962 -0.0425 0.049 Uiso 1 1 calc R . . C28 C -0.5335(3) 1.0446(3) -0.1175(3) 0.0390(12) Uani 1 1 d . . . H28 H -0.5843 1.0530 -0.1456 0.047 Uiso 1 1 calc R . . C29 C -0.5035(3) 0.9737(3) -0.1440(3) 0.0378(12) Uani 1 1 d . . . H29 H -0.5321 0.9332 -0.1911 0.045 Uiso 1 1 calc R . . C30 C -0.3951(4) 0.8834(3) -0.1246(3) 0.0372(12) Uani 1 1 d . . . H30 H -0.4219 0.8402 -0.1707 0.045 Uiso 1 1 calc R . . C31 C -0.3246(3) 0.8734(3) -0.0804(3) 0.0361(11) Uani 1 1 d . . . H31 H -0.3026 0.8232 -0.0949 0.043 Uiso 1 1 calc R . . C32 C -0.2854(3) 0.9383(3) -0.0137(3) 0.0308(10) Uani 1 1 d . . . H32 H -0.2357 0.9308 0.0162 0.037 Uiso 1 1 calc R . . C33 C -0.3838(3) 1.0179(3) -0.0341(3) 0.0266(10) Uani 1 1 d . . . C34 C -0.4276(3) 0.9572(3) -0.1021(3) 0.0308(10) Uani 1 1 d . . . C35 C -0.4909(3) 1.1087(3) -0.0476(3) 0.0308(11) Uani 1 1 d . . . C36 C -0.4156(3) 1.0941(3) -0.0082(3) 0.0286(10) Uani 1 1 d . . . C37 C 0.0831(4) 1.0953(4) 0.4112(3) 0.0533(15) Uani 1 1 d . . . H37 H 0.0822 1.1517 0.4309 0.064 Uiso 1 1 calc R . . C38 C 0.0602(4) 1.0493(4) 0.3340(3) 0.0552(17) Uani 1 1 d . . . H38 H 0.0422 1.0742 0.3013 0.066 Uiso 1 1 calc R . . C39 C 0.0635(4) 0.9701(4) 0.3059(3) 0.0525(16) Uani 1 1 d . . . H39 H 0.0494 0.9397 0.2530 0.063 Uiso 1 1 calc R . . C40 C 0.0917(4) 0.8477(4) 0.3273(3) 0.0529(16) Uani 1 1 d . . . H40 H 0.0798 0.8146 0.2748 0.064 Uiso 1 1 calc R . . C41 C 0.1127(4) 0.8148(4) 0.3763(3) 0.0608(17) Uani 1 1 d . . . H41 H 0.1156 0.7587 0.3576 0.073 Uiso 1 1 calc R . . C42 C 0.1496(5) 0.8306(5) 0.5093(4) 0.0701(19) Uani 1 1 d . . . H42 H 0.1512 0.7745 0.4935 0.084 Uiso 1 1 calc R . . C43 C 0.1658(5) 0.8793(5) 0.5840(4) 0.071(2) Uani 1 1 d . . . H43 H 0.1795 0.8581 0.6206 0.086 Uiso 1 1 calc R . . C44 C 0.1617(4) 0.9607(5) 0.6055(3) 0.0633(19) Uani 1 1 d . . . H44 H 0.1726 0.9942 0.6580 0.076 Uiso 1 1 calc R . . C45 C 0.1284(3) 0.9444(4) 0.4836(3) 0.0448(14) Uani 1 1 d . . . C46 C 0.1308(4) 0.8618(4) 0.4559(3) 0.0544(16) Uani 1 1 d . . . C47 C 0.0872(3) 0.9310(4) 0.3530(3) 0.0469(15) Uani 1 1 d . . . C48 C 0.1070(3) 0.9804(4) 0.4321(3) 0.0417(13) Uani 1 1 d . . . C49 C 0.2555(4) 0.4290(3) 0.0476(3) 0.0532(16) Uani 1 1 d . . . H49 H 0.2134 0.3822 0.0438 0.064 Uiso 1 1 calc R . . C50 C 0.2216(4) 0.4863(4) 0.0263(3) 0.0582(18) Uani 1 1 d . . . H50 H 0.1571 0.4786 0.0072 0.070 Uiso 1 1 calc R . . C51 C 0.2821(4) 0.5530(4) 0.0333(3) 0.0515(15) Uani 1 1 d . . . H51 H 0.2593 0.5930 0.0198 0.062 Uiso 1 1 calc R . . C52 C 0.4459(4) 0.6347(3) 0.0700(3) 0.0454(14) Uani 1 1 d . . . H52 H 0.4261 0.6755 0.0563 0.055 Uiso 1 1 calc R . . C53 C 0.5350(4) 0.6439(3) 0.0977(3) 0.0443(13) Uani 1 1 d . . . H53 H 0.5774 0.6915 0.1041 0.053 Uiso 1 1 calc R . . C54 C 0.6628(4) 0.5896(3) 0.1468(4) 0.0538(16) Uani 1 1 d . . . H54 H 0.7079 0.6360 0.1546 0.065 Uiso 1 1 calc R . . C55 C 0.6880(4) 0.5294(4) 0.1629(4) 0.066(2) Uani 1 1 d . . . H55 H 0.7511 0.5333 0.1831 0.079 Uiso 1 1 calc R . . C56 C 0.6210(4) 0.4603(3) 0.1499(4) 0.0612(19) Uani 1 1 d . . . H56 H 0.6409 0.4177 0.1606 0.073 Uiso 1 1 calc R . . C57 C 0.5057(3) 0.5129(3) 0.1081(3) 0.0352(11) Uani 1 1 d . . . C58 C 0.5683(4) 0.5836(3) 0.1181(3) 0.0397(12) Uani 1 1 d . . . C59 C 0.3781(4) 0.5644(3) 0.0601(3) 0.0391(12) Uani 1 1 d . . . C60 C 0.4091(3) 0.5058(3) 0.0796(3) 0.0334(11) Uani 1 1 d . . . C61 C -0.3573(4) 1.1078(4) 0.6000(3) 0.0600(18) Uani 1 1 d . . . H61 H -0.3444 1.1250 0.6532 0.072 Uiso 1 1 calc R . . C62 C -0.3690(4) 1.1659(4) 0.5714(4) 0.0653(19) Uani 1 1 d . . . H62 H -0.3644 1.2211 0.6044 0.078 Uiso 1 1 calc R . . C63 C -0.3870(5) 1.1423(5) 0.4950(4) 0.0689(19) Uani 1 1 d . . . H63 H -0.3949 1.1810 0.4741 0.083 Uiso 1 1 calc R . . C64 C -0.4123(4) 1.0311(5) 0.3661(3) 0.0637(18) Uani 1 1 d . . . H64 H -0.4191 1.0681 0.3430 0.076 Uiso 1 1 calc R . . C65 C -0.4199(4) 0.9523(4) 0.3228(3) 0.0586(18) Uani 1 1 d . . . H65 H -0.4316 0.9344 0.2694 0.070 Uiso 1 1 calc R . . C66 C -0.4223(4) 0.8109(4) 0.3138(3) 0.0566(18) Uani 1 1 d . . . H66 H -0.4362 0.7896 0.2603 0.068 Uiso 1 1 calc R . . C67 C -0.4141(4) 0.7612(5) 0.3481(3) 0.0651(19) Uani 1 1 d . . . H67 H -0.4229 0.7045 0.3197 0.078 Uiso 1 1 calc R . . C68 C -0.3924(5) 0.7928(5) 0.4263(4) 0.071(2) Uani 1 1 d . . . H68 H -0.3846 0.7570 0.4506 0.085 Uiso 1 1 calc R . . C69 C -0.3909(3) 0.9247(4) 0.4348(3) 0.0493(16) Uani 1 1 d . . . C70 C -0.4108(4) 0.8946(4) 0.3553(3) 0.0552(17) Uani 1 1 d . . . C71 C -0.3938(4) 1.0608(4) 0.4477(3) 0.0563(17) Uani 1 1 d . . . C72 C -0.3821(4) 1.0079(4) 0.4816(3) 0.0481(15) 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 0.01976(12) 0.02107(11) 0.02084(12) 0.00826(8) 0.00390(8) 0.00473(8) S1 0.0205(5) 0.0266(5) 0.0303(6) 0.0183(5) 0.0080(4) 0.0079(4) S2 0.0175(5) 0.0262(5) 0.0293(6) 0.0115(4) 0.0040(4) 0.0028(4) S3 0.0273(6) 0.0227(5) 0.0332(6) 0.0130(5) 0.0040(5) 0.0036(4) S4 0.0193(5) 0.0271(5) 0.0273(6) 0.0151(4) 0.0049(4) 0.0072(4) S5 0.0465(8) 0.0349(6) 0.0281(6) 0.0049(5) -0.0001(6) 0.0088(6) S6 0.0272(6) 0.0294(6) 0.0300(6) 0.0099(5) 0.0047(5) 0.0129(5) S7 0.0397(8) 0.0949(12) 0.0323(7) 0.0351(8) 0.0113(6) 0.0146(8) S8 0.0569(9) 0.0442(8) 0.0636(10) 0.0356(7) -0.0157(8) 0.0051(7) N1 0.027(2) 0.034(2) 0.038(2) 0.0230(18) 0.0080(17) 0.0060(17) N2 0.0206(19) 0.037(2) 0.033(2) 0.0226(17) 0.0072(16) 0.0076(16) N3 0.032(2) 0.078(3) 0.027(2) 0.020(2) 0.0104(18) 0.002(2) N4 0.025(2) 0.095(4) 0.025(2) 0.022(2) 0.0021(18) 0.002(2) N5 0.028(2) 0.031(2) 0.054(3) 0.0003(19) -0.005(2) 0.0027(18) N6 0.038(3) 0.030(2) 0.073(3) 0.018(2) -0.015(2) 0.0025(19) N7 0.032(3) 0.085(4) 0.030(2) 0.007(2) 0.006(2) 0.000(2) N8 0.038(3) 0.083(4) 0.035(3) 0.007(3) 0.001(2) 0.007(3) O1 0.0214(15) 0.0267(15) 0.0268(16) 0.0142(13) 0.0040(12) 0.0062(12) O2 0.0211(15) 0.0218(14) 0.0261(16) 0.0089(12) 0.0049(12) 0.0068(12) O3 0.0220(15) 0.0242(14) 0.0234(15) 0.0113(12) 0.0012(12) 0.0002(12) O4 0.0229(16) 0.0264(15) 0.0305(16) 0.0156(13) 0.0082(13) 0.0067(12) O5 0.040(2) 0.074(3) 0.051(2) 0.049(2) 0.0201(17) 0.0273(19) O6 0.0372(19) 0.0291(16) 0.0291(17) 0.0103(13) 0.0043(14) 0.0112(14) O7 0.0320(18) 0.0325(16) 0.0290(17) 0.0120(13) 0.0059(14) 0.0123(14) O8 0.0304(17) 0.0317(16) 0.0264(16) 0.0134(13) 0.0027(13) 0.0076(14) O9 0.0328(18) 0.0393(18) 0.0302(17) 0.0198(14) 0.0082(14) 0.0158(15) O10 0.0240(16) 0.0304(16) 0.0443(19) 0.0246(15) 0.0091(14) 0.0077(13) O11 0.0236(16) 0.0311(16) 0.0310(17) 0.0110(13) -0.0011(13) 0.0038(13) O12 0.0232(17) 0.0348(17) 0.046(2) 0.0190(15) 0.0103(14) 0.0058(14) O13 0.0322(18) 0.0262(16) 0.053(2) 0.0213(15) 0.0067(16) 0.0045(14) O14 0.0383(19) 0.0350(17) 0.0294(17) 0.0100(14) 0.0039(15) 0.0086(15) O15 0.0211(16) 0.0326(16) 0.0313(17) 0.0158(13) 0.0079(13) 0.0101(13) O16 0.0200(16) 0.0341(16) 0.0384(18) 0.0191(14) 0.0009(13) 0.0074(13) O17A 0.067(2) 0.058(2) 0.048(2) -0.0025(16) -0.0063(19) 0.0012(19) O18A 0.067(2) 0.058(2) 0.048(2) -0.0025(16) -0.0063(19) 0.0012(19) O19A 0.067(2) 0.058(2) 0.048(2) -0.0025(16) -0.0063(19) 0.0012(19) O17B 0.067(2) 0.058(2) 0.048(2) -0.0025(16) -0.0063(19) 0.0012(19) O18B 0.067(2) 0.058(2) 0.048(2) -0.0025(16) -0.0063(19) 0.0012(19) O19B 0.067(2) 0.058(2) 0.048(2) -0.0025(16) -0.0063(19) 0.0012(19) O20 0.037(2) 0.045(2) 0.057(2) 0.0254(18) 0.0249(17) 0.0216(16) O21 0.045(2) 0.0385(19) 0.039(2) 0.0010(15) -0.0084(17) 0.0159(16) O22 0.0349(18) 0.0325(17) 0.0359(18) 0.0138(14) 0.0027(15) 0.0145(14) O23 0.067(3) 0.091(3) 0.065(3) 0.054(3) 0.028(2) 0.010(3) O24 0.055(3) 0.199(6) 0.050(3) 0.077(3) 0.016(2) 0.042(3) O25 0.060(3) 0.087(3) 0.027(2) 0.010(2) 0.0156(18) 0.006(2) O26A 0.074(3) 0.076(3) 0.069(3) 0.047(3) -0.009(3) 0.022(2) O27A 0.074(3) 0.076(3) 0.069(3) 0.047(3) -0.009(3) 0.022(2) O28A 0.074(3) 0.076(3) 0.069(3) 0.047(3) -0.009(3) 0.022(2) O26B 0.074(3) 0.076(3) 0.069(3) 0.047(3) -0.009(3) 0.022(2) O27B 0.074(3) 0.076(3) 0.069(3) 0.047(3) -0.009(3) 0.022(2) O28B 0.074(3) 0.076(3) 0.069(3) 0.047(3) -0.009(3) 0.022(2) C1 0.016(2) 0.028(2) 0.034(2) 0.0210(19) 0.0102(18) 0.0071(17) C2 0.017(2) 0.026(2) 0.021(2) 0.0119(17) 0.0026(17) 0.0062(17) C3 0.023(2) 0.022(2) 0.024(2) 0.0114(17) -0.0003(17) 0.0044(17) C4 0.021(2) 0.029(2) 0.023(2) 0.0126(18) 0.0035(17) 0.0089(18) C5 0.018(2) 0.030(2) 0.022(2) 0.0090(18) 0.0038(17) 0.0048(18) C6 0.016(2) 0.026(2) 0.023(2) 0.0099(17) 0.0032(17) 0.0013(17) C7 0.019(2) 0.025(2) 0.028(2) 0.0119(18) 0.0014(18) -0.0007(17) C8 0.021(2) 0.032(2) 0.026(2) 0.0084(19) 0.0039(18) 0.0016(18) C9 0.022(2) 0.044(3) 0.026(2) 0.016(2) 0.0048(19) 0.003(2) C10 0.021(2) 0.036(2) 0.035(3) 0.023(2) 0.0005(19) -0.0010(19) C11 0.021(2) 0.027(2) 0.027(2) 0.0147(18) 0.0024(18) -0.0013(18) C12 0.027(2) 0.024(2) 0.031(2) 0.0121(18) 0.0051(19) 0.0058(18) C13 0.035(3) 0.023(2) 0.032(2) 0.0146(19) 0.009(2) 0.0104(19) C14 0.038(3) 0.030(2) 0.030(2) 0.017(2) -0.001(2) 0.010(2) C15 0.031(3) 0.030(2) 0.027(2) 0.0090(19) 0.000(2) 0.008(2) C16 0.023(2) 0.025(2) 0.027(2) 0.0142(18) 0.0082(18) 0.0074(17) C17 0.020(2) 0.029(2) 0.026(2) 0.0169(18) 0.0052(18) 0.0013(18) C18 0.024(2) 0.033(2) 0.024(2) 0.0146(19) 0.0039(18) 0.0073(19) C19 0.028(2) 0.030(2) 0.023(2) 0.0077(18) 0.0091(19) 0.0040(19) C20 0.029(2) 0.028(2) 0.028(2) 0.0147(19) 0.0120(19) 0.0087(19) C21 0.016(2) 0.025(2) 0.029(2) 0.0187(19) 0.0080(17) 0.0010(17) C22 0.017(2) 0.027(2) 0.017(2) 0.0090(17) 0.0015(16) 0.0035(17) C23 0.017(2) 0.023(2) 0.026(2) 0.0109(17) -0.0007(17) -0.0038(17) C24 0.023(2) 0.026(2) 0.022(2) 0.0122(17) 0.0082(17) 0.0107(18) C25 0.036(3) 0.032(2) 0.049(3) 0.022(2) 0.009(2) 0.010(2) C26 0.033(3) 0.043(3) 0.063(4) 0.033(3) 0.015(3) 0.014(2) C27 0.020(2) 0.056(3) 0.068(4) 0.044(3) 0.013(2) 0.010(2) C28 0.019(2) 0.067(4) 0.045(3) 0.039(3) 0.002(2) 0.003(2) C29 0.028(3) 0.054(3) 0.033(3) 0.023(2) 0.000(2) -0.006(2) C30 0.036(3) 0.035(3) 0.038(3) 0.013(2) 0.017(2) -0.004(2) C31 0.034(3) 0.033(2) 0.044(3) 0.017(2) 0.013(2) 0.006(2) C32 0.030(3) 0.038(3) 0.036(3) 0.024(2) 0.015(2) 0.010(2) C33 0.023(2) 0.032(2) 0.031(2) 0.019(2) 0.0101(19) 0.0023(19) C34 0.023(2) 0.042(3) 0.034(3) 0.023(2) 0.008(2) -0.001(2) C35 0.018(2) 0.045(3) 0.042(3) 0.031(2) 0.005(2) 0.001(2) C36 0.018(2) 0.036(2) 0.040(3) 0.026(2) 0.0034(19) -0.0007(19) C37 0.044(3) 0.081(4) 0.038(3) 0.028(3) 0.007(3) 0.006(3) C38 0.036(3) 0.103(5) 0.034(3) 0.036(3) 0.010(2) 0.006(3) C39 0.029(3) 0.091(5) 0.028(3) 0.017(3) 0.004(2) -0.001(3) C40 0.034(3) 0.071(4) 0.033(3) -0.001(3) 0.005(2) 0.003(3) C41 0.051(4) 0.080(4) 0.045(4) 0.017(3) 0.002(3) 0.014(3) C42 0.068(5) 0.094(5) 0.052(4) 0.031(4) 0.005(3) 0.019(4) C43 0.056(4) 0.111(6) 0.060(4) 0.048(4) 0.007(3) 0.014(4) C44 0.036(3) 0.123(6) 0.036(3) 0.038(4) 0.002(3) 0.008(4) C45 0.019(2) 0.086(4) 0.027(3) 0.021(3) 0.005(2) 0.002(3) C46 0.037(3) 0.078(4) 0.043(3) 0.020(3) 0.005(3) 0.009(3) C47 0.021(3) 0.090(4) 0.026(3) 0.021(3) 0.006(2) 0.001(3) C48 0.023(3) 0.071(4) 0.025(3) 0.013(3) 0.008(2) 0.001(2) C49 0.032(3) 0.049(3) 0.053(4) -0.007(3) -0.003(3) 0.007(3) C50 0.034(3) 0.075(4) 0.044(3) -0.004(3) -0.008(3) 0.024(3) C51 0.052(4) 0.059(4) 0.041(3) 0.010(3) 0.002(3) 0.033(3) C52 0.064(4) 0.035(3) 0.049(3) 0.023(2) 0.021(3) 0.026(3) C53 0.053(4) 0.025(2) 0.055(3) 0.013(2) 0.019(3) 0.009(2) C54 0.035(3) 0.040(3) 0.072(4) 0.012(3) 0.000(3) -0.009(3) C55 0.036(3) 0.057(4) 0.095(5) 0.027(4) -0.030(3) -0.006(3) C56 0.039(3) 0.045(3) 0.097(5) 0.030(3) -0.025(3) 0.004(3) C57 0.032(3) 0.024(2) 0.044(3) 0.009(2) -0.002(2) 0.003(2) C58 0.035(3) 0.026(2) 0.048(3) 0.005(2) 0.004(2) 0.001(2) C59 0.040(3) 0.037(3) 0.039(3) 0.009(2) 0.006(2) 0.017(2) C60 0.027(3) 0.023(2) 0.041(3) 0.003(2) 0.001(2) 0.0046(19) C61 0.044(4) 0.083(5) 0.036(3) 0.008(3) 0.013(3) -0.004(3) C62 0.055(4) 0.075(4) 0.043(4) 0.001(3) 0.019(3) -0.001(3) C63 0.055(4) 0.090(5) 0.053(4) 0.019(4) 0.016(3) 0.008(4) C64 0.046(4) 0.102(5) 0.041(3) 0.029(4) 0.006(3) 0.001(4) C65 0.027(3) 0.103(5) 0.031(3) 0.013(3) 0.006(2) 0.003(3) C66 0.024(3) 0.093(5) 0.028(3) 0.000(3) 0.001(2) 0.003(3) C67 0.044(4) 0.090(5) 0.041(4) 0.004(3) -0.002(3) 0.012(3) C68 0.058(4) 0.090(5) 0.049(4) 0.009(4) -0.004(3) 0.017(4) C69 0.020(3) 0.083(4) 0.026(3) 0.002(3) 0.008(2) 0.005(3) C70 0.021(3) 0.100(5) 0.028(3) 0.010(3) 0.005(2) 0.000(3) C71 0.028(3) 0.090(5) 0.035(3) 0.008(3) 0.012(2) 0.003(3) C72 0.023(3) 0.078(4) 0.034(3) 0.013(3) 0.009(2) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O3 2.312(3) . ? Gd1 O4 2.320(3) . ? Gd1 O1 2.328(3) . ? Gd1 O2 2.341(3) . ? Gd1 O5 2.431(3) . ? Gd1 O6 2.446(3) . ? Gd1 O7 2.466(3) . ? Gd1 O8 2.502(3) . ? S1 O9 1.428(3) . ? S1 O10 1.448(3) . ? S1 C2 1.773(4) . ? S1 C1 1.776(4) . ? S2 O11 1.448(3) . ? S2 O12 1.449(3) . ? S2 C6 1.772(4) . ? S2 C7 1.773(4) . ? S3 O14 1.429(3) . ? S3 O13 1.442(3) . ? S3 C12 1.758(4) . ? S3 C11 1.767(5) . ? S4 O16 1.445(3) . ? S4 O15 1.448(3) . ? S4 C17 1.768(4) . ? S4 C16 1.782(4) . ? S5 O18B 1.383(8) . ? S5 O19A 1.407(13) . ? S5 O19B 1.415(8) . ? S5 O17A 1.455(13) . ? S5 O17B 1.501(8) . ? S5 O18A 1.523(13) . ? S5 C19 1.770(4) . ? S6 O20 1.451(4) . ? S6 O21 1.459(3) . ? S6 O22 1.461(3) . ? S6 C4 1.772(4) . ? S7 O23 1.451(4) . ? S7 O24 1.455(4) . ? S7 O25 1.456(5) . ? S7 C9 1.768(5) . ? S8 O26B 1.362(13) . ? S8 O27A 1.377(11) . ? S8 O28A 1.442(9) . ? S8 O28B 1.472(13) . ? S8 O27B 1.524(14) . ? S8 O26A 1.558(10) . ? S8 C14 1.773(4) . ? N1 C25 1.343(6) . ? N1 C36 1.365(6) . ? N2 C32 1.319(6) . ? N2 C33 1.360(6) . ? N3 C37 1.335(7) . ? N3 C48 1.340(7) . ? N4 C44 1.311(8) . ? N4 C45 1.363(6) . ? N5 C49 1.335(7) . ? N5 C60 1.375(6) . ? N6 C56 1.315(7) . ? N6 C57 1.352(6) . ? N7 C61 1.321(8) . ? N7 C72 1.359(7) . ? N8 C68 1.320(8) . ? N8 C69 1.365(8) . ? O1 C21 1.276(5) . ? O2 C22 1.269(5) . ? O3 C23 1.283(5) . ? O4 C24 1.278(5) . ? C1 C20 1.377(6) . ? C1 C21 1.437(6) . ? C2 C3 1.371(6) . ? C2 C22 1.427(6) . ? C3 C4 1.396(6) . ? C3 H3 0.9500 . ? C4 C5 1.386(6) . ? C5 C6 1.383(6) . ? C5 H5 0.9500 . ? C6 C22 1.439(6) . ? C7 C8 1.401(6) . ? C7 C23 1.422(6) . ? C8 C9 1.383(6) . ? C8 H8 0.9500 . ? C9 C10 1.386(7) . ? C10 C11 1.377(6) . ? C10 H10 0.9500 . ? C11 C23 1.437(6) . ? C12 C13 1.379(6) . ? C12 C24 1.418(6) . ? C13 C14 1.387(6) . ? C13 H13 0.9500 . ? C14 C15 1.389(6) . ? C15 C16 1.378(6) . ? C15 H15 0.9500 . ? C16 C24 1.427(6) . ? C17 C18 1.401(6) . ? C17 C21 1.447(6) . ? C18 C19 1.379(6) . ? C18 H18 0.9500 . ? C19 C20 1.384(6) . ? C20 H20 0.9500 . ? C25 C26 1.389(7) . ? C25 H25 0.9500 . ? C26 C27 1.363(7) . ? C26 H26 0.9500 . ? C27 C35 1.406(7) . ? C27 H27 0.9500 . ? C28 C29 1.331(7) . ? C28 C35 1.438(7) . ? C28 H28 0.9500 . ? C29 C34 1.453(7) . ? C29 H29 0.9500 . ? C30 C31 1.365(7) . ? C30 C34 1.395(7) . ? C30 H30 0.9500 . ? C31 C32 1.395(7) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.397(6) . ? C33 C36 1.428(6) . ? C35 C36 1.402(6) . ? C37 C38 1.392(8) . ? C37 H37 0.9500 . ? C38 C39 1.337(9) . ? C38 H38 0.9500 . ? C39 C47 1.404(8) . ? C39 H39 0.9500 . ? C40 C41 1.337(9) . ? C40 C47 1.415(8) . ? C40 H40 0.9500 . ? C41 C46 1.430(8) . ? C41 H41 0.9500 . ? C42 C43 1.357(9) . ? C42 C46 1.383(9) . ? C42 H42 0.9500 . ? C43 C44 1.385(10) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.394(9) . ? C45 C48 1.426(8) . ? C47 C48 1.430(7) . ? C49 C50 1.390(9) . ? C49 H49 0.9500 . ? C50 C51 1.350(9) . ? C50 H50 0.9500 . ? C51 C59 1.407(7) . ? C51 H51 0.9500 . ? C52 C53 1.323(8) . ? C52 C59 1.440(7) . ? C52 H52 0.9500 . ? C53 C58 1.430(7) . ? C53 H53 0.9500 . ? C54 C55 1.334(8) . ? C54 C58 1.411(7) . ? C54 H54 0.9500 . ? C55 C56 1.406(8) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.406(6) . ? C57 C60 1.435(6) . ? C59 C60 1.375(7) . ? C61 C62 1.391(9) . ? C61 H61 0.9500 . ? C62 C63 1.365(9) . ? C62 H62 0.9500 . ? C63 C71 1.397(9) . ? C63 H63 0.9500 . ? C64 C65 1.338(9) . ? C64 C71 1.450(8) . ? C64 H64 0.9500 . ? C65 C70 1.430(9) . ? C65 H65 0.9500 . ? C66 C67 1.322(9) . ? C66 C70 1.402(9) . ? C66 H66 0.9500 . ? C67 C68 1.390(8) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.414(7) . ? C69 C72 1.416(8) . ? C71 C72 1.377(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Gd1 O4 80.46(10) . . ? O3 Gd1 O1 142.04(10) . . ? O4 Gd1 O1 72.25(10) . . ? O3 Gd1 O2 73.15(10) . . ? O4 Gd1 O2 80.89(10) . . ? O1 Gd1 O2 76.83(10) . . ? O3 Gd1 O5 137.99(11) . . ? O4 Gd1 O5 141.29(11) . . ? O1 Gd1 O5 74.62(11) . . ? O2 Gd1 O5 110.38(11) . . ? O3 Gd1 O6 77.84(10) . . ? O4 Gd1 O6 118.21(10) . . ? O1 Gd1 O6 138.53(11) . . ? O2 Gd1 O6 141.85(10) . . ? O5 Gd1 O6 76.26(12) . . ? O3 Gd1 O7 123.78(10) . . ? O4 Gd1 O7 75.00(10) . . ? O1 Gd1 O7 74.11(10) . . ? O2 Gd1 O7 146.65(10) . . ? O5 Gd1 O7 77.17(11) . . ? O6 Gd1 O7 71.10(10) . . ? O3 Gd1 O8 72.68(10) . . ? O4 Gd1 O8 147.34(10) . . ? O1 Gd1 O8 120.12(9) . . ? O2 Gd1 O8 73.86(10) . . ? O5 Gd1 O8 68.77(11) . . ? O6 Gd1 O8 74.22(10) . . ? O7 Gd1 O8 135.92(10) . . ? O9 S1 O10 117.86(19) . . ? O9 S1 C2 109.72(19) . . ? O10 S1 C2 105.44(19) . . ? O9 S1 C1 110.61(19) . . ? O10 S1 C1 106.58(18) . . ? C2 S1 C1 105.87(19) . . ? O11 S2 O12 115.78(19) . . ? O11 S2 C6 107.17(19) . . ? O12 S2 C6 106.37(19) . . ? O11 S2 C7 109.18(19) . . ? O12 S2 C7 106.9(2) . . ? C6 S2 C7 111.50(19) . . ? O14 S3 O13 117.91(19) . . ? O14 S3 C12 107.5(2) . . ? O13 S3 C12 107.1(2) . . ? O14 S3 C11 111.4(2) . . ? O13 S3 C11 107.3(2) . . ? C12 S3 C11 104.7(2) . . ? O16 S4 O15 116.41(19) . . ? O16 S4 C17 107.48(19) . . ? O15 S4 C17 108.42(18) . . ? O16 S4 C16 105.33(19) . . ? O15 S4 C16 106.44(19) . . ? C17 S4 C16 112.9(2) . . ? O18B S5 O19A 142.7(5) . . ? O18B S5 O19B 117.5(5) . . ? O19A S5 O19B 44.8(5) . . ? O18B S5 O17A 60.2(6) . . ? O19A S5 O17A 113.2(7) . . ? O19B S5 O17A 145.3(5) . . ? O18B S5 O17B 110.0(4) . . ? O19A S5 O17B 67.1(6) . . ? O19B S5 O17B 111.2(4) . . ? O17A S5 O17B 51.1(5) . . ? O18B S5 O18A 49.0(5) . . ? O19A S5 O18A 111.5(7) . . ? O19B S5 O18A 70.9(6) . . ? O17A S5 O18A 106.9(7) . . ? O17B S5 O18A 145.9(5) . . ? O18B S5 C19 107.0(3) . . ? O19A S5 C19 109.8(4) . . ? O19B S5 C19 106.1(3) . . ? O17A S5 C19 107.3(4) . . ? O17B S5 C19 104.1(3) . . ? O18A S5 C19 107.9(4) . . ? O20 S6 O21 113.3(2) . . ? O20 S6 O22 113.3(2) . . ? O21 S6 O22 110.8(2) . . ? O20 S6 C4 105.9(2) . . ? O21 S6 C4 105.8(2) . . ? O22 S6 C4 107.16(19) . . ? O23 S7 O24 112.0(3) . . ? O23 S7 O25 112.0(3) . . ? O24 S7 O25 113.9(3) . . ? O23 S7 C9 106.2(2) . . ? O24 S7 C9 106.3(2) . . ? O25 S7 C9 105.8(2) . . ? O26B S8 O27A 134.2(7) . . ? O26B S8 O28A 71.3(6) . . ? O27A S8 O28A 117.4(5) . . ? O26B S8 O28B 107.7(7) . . ? O27A S8 O28B 88.7(6) . . ? O28A S8 O28B 36.6(5) . . ? O26B S8 O27B 121.6(7) . . ? O27A S8 O27B 24.2(6) . . ? O28A S8 O27B 139.2(5) . . ? O28B S8 O27B 112.9(7) . . ? O26B S8 O26A 35.3(5) . . ? O27A S8 O26A 109.1(5) . . ? O28A S8 O26A 105.4(5) . . ? O28B S8 O26A 140.0(5) . . ? O27B S8 O26A 89.6(6) . . ? O26B S8 C14 107.5(4) . . ? O27A S8 C14 109.9(4) . . ? O28A S8 C14 110.2(3) . . ? O28B S8 C14 103.1(4) . . ? O27B S8 C14 102.3(5) . . ? O26A S8 C14 103.8(3) . . ? C25 N1 C36 122.0(4) . . ? C32 N2 C33 116.2(4) . . ? C37 N3 C48 121.9(5) . . ? C44 N4 C45 116.0(6) . . ? C49 N5 C60 121.0(5) . . ? C56 N6 C57 117.3(5) . . ? C61 N7 C72 116.4(6) . . ? C68 N8 C69 121.1(5) . . ? C21 O1 Gd1 133.2(3) . . ? C22 O2 Gd1 152.6(3) . . ? C23 O3 Gd1 127.9(2) . . ? C24 O4 Gd1 149.1(3) . . ? C20 C1 C21 122.8(4) . . ? C20 C1 S1 115.5(3) . . ? C21 C1 S1 121.7(3) . . ? C3 C2 C22 123.0(4) . . ? C3 C2 S1 119.0(3) . . ? C22 C2 S1 117.8(3) . . ? C2 C3 C4 120.5(4) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 119.4(4) . . ? C5 C4 S6 120.6(3) . . ? C3 C4 S6 119.9(3) . . ? C6 C5 C4 120.2(4) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C22 122.7(4) . . ? C5 C6 S2 116.1(3) . . ? C22 C6 S2 120.5(3) . . ? C8 C7 C23 122.9(4) . . ? C8 C7 S2 115.8(3) . . ? C23 C7 S2 121.1(3) . . ? C9 C8 C7 119.8(4) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 119.6(4) . . ? C8 C9 S7 121.2(4) . . ? C10 C9 S7 119.1(4) . . ? C11 C10 C9 120.9(4) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C23 122.5(4) . . ? C10 C11 S3 115.7(3) . . ? C23 C11 S3 121.8(3) . . ? C13 C12 C24 122.9(4) . . ? C13 C12 S3 120.1(3) . . ? C24 C12 S3 116.8(3) . . ? C12 C13 C14 119.6(4) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 119.8(4) . . ? C13 C14 S8 118.9(3) . . ? C15 C14 S8 121.2(4) . . ? C16 C15 C14 120.5(4) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C24 121.8(4) . . ? C15 C16 S4 117.1(3) . . ? C24 C16 S4 120.2(3) . . ? C18 C17 C21 121.9(4) . . ? C18 C17 S4 115.7(3) . . ? C21 C17 S4 121.7(3) . . ? C19 C18 C17 120.6(4) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 119.6(4) . . ? C18 C19 S5 121.4(3) . . ? C20 C19 S5 119.0(3) . . ? C1 C20 C19 121.0(4) . . ? C1 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? O1 C21 C1 123.5(4) . . ? O1 C21 C17 122.6(4) . . ? C1 C21 C17 113.9(4) . . ? O2 C22 C2 122.8(4) . . ? O2 C22 C6 123.1(4) . . ? C2 C22 C6 114.1(4) . . ? O3 C23 C7 123.4(4) . . ? O3 C23 C11 122.2(4) . . ? C7 C23 C11 114.3(4) . . ? O4 C24 C12 121.8(4) . . ? O4 C24 C16 123.0(4) . . ? C12 C24 C16 115.2(4) . . ? N1 C25 C26 120.4(5) . . ? N1 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C27 C26 C25 119.1(5) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C26 C27 C35 121.2(5) . . ? C26 C27 H27 119.4 . . ? C35 C27 H27 119.4 . . ? C29 C28 C35 121.7(4) . . ? C29 C28 H28 119.1 . . ? C35 C28 H28 119.1 . . ? C28 C29 C34 121.1(5) . . ? C28 C29 H29 119.4 . . ? C34 C29 H29 119.4 . . ? C31 C30 C34 119.9(5) . . ? C31 C30 H30 120.0 . . ? C34 C30 H30 120.0 . . ? C30 C31 C32 118.9(5) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? N2 C32 C31 124.0(4) . . ? N2 C32 H32 118.0 . . ? C31 C32 H32 118.0 . . ? N2 C33 C34 124.6(4) . . ? N2 C33 C36 116.9(4) . . ? C34 C33 C36 118.5(4) . . ? C30 C34 C33 116.4(4) . . ? C30 C34 C29 124.4(5) . . ? C33 C34 C29 119.2(4) . . ? C36 C35 C27 117.9(4) . . ? C36 C35 C28 117.4(4) . . ? C27 C35 C28 124.6(4) . . ? N1 C36 C35 119.4(4) . . ? N1 C36 C33 118.6(4) . . ? C35 C36 C33 122.0(4) . . ? N3 C37 C38 120.0(6) . . ? N3 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C39 C38 C37 120.0(6) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C47 121.5(5) . . ? C38 C39 H39 119.3 . . ? C47 C39 H39 119.3 . . ? C41 C40 C47 120.7(5) . . ? C41 C40 H40 119.7 . . ? C47 C40 H40 119.7 . . ? C40 C41 C46 121.9(6) . . ? C40 C41 H41 119.1 . . ? C46 C41 H41 119.1 . . ? C43 C42 C46 120.6(7) . . ? C43 C42 H42 119.7 . . ? C46 C42 H42 119.7 . . ? C42 C43 C44 118.5(7) . . ? C42 C43 H43 120.7 . . ? C44 C43 H43 120.7 . . ? N4 C44 C43 124.4(6) . . ? N4 C44 H44 117.8 . . ? C43 C44 H44 117.8 . . ? N4 C45 C46 124.2(5) . . ? N4 C45 C48 116.4(6) . . ? C46 C45 C48 119.4(5) . . ? C42 C46 C45 116.2(6) . . ? C42 C46 C41 124.3(7) . . ? C45 C46 C41 119.4(6) . . ? C39 C47 C40 124.5(5) . . ? C39 C47 C48 116.3(6) . . ? C40 C47 C48 119.2(5) . . ? N3 C48 C45 120.3(5) . . ? N3 C48 C47 120.2(5) . . ? C45 C48 C47 119.5(6) . . ? N5 C49 C50 121.0(6) . . ? N5 C49 H49 119.5 . . ? C50 C49 H49 119.5 . . ? C51 C50 C49 118.7(5) . . ? C51 C50 H50 120.6 . . ? C49 C50 H50 120.6 . . ? C50 C51 C59 121.2(5) . . ? C50 C51 H51 119.4 . . ? C59 C51 H51 119.4 . . ? C53 C52 C59 121.9(5) . . ? C53 C52 H52 119.1 . . ? C59 C52 H52 119.1 . . ? C52 C53 C58 121.1(5) . . ? C52 C53 H53 119.5 . . ? C58 C53 H53 119.5 . . ? C55 C54 C58 119.4(5) . . ? C55 C54 H54 120.3 . . ? C58 C54 H54 120.3 . . ? C54 C55 C56 119.8(5) . . ? C54 C55 H55 120.1 . . ? C56 C55 H55 120.1 . . ? N6 C56 C55 123.3(5) . . ? N6 C56 H56 118.4 . . ? C55 C56 H56 118.4 . . ? N6 C57 C58 123.2(4) . . ? N6 C57 C60 118.8(4) . . ? C58 C57 C60 117.9(4) . . ? C57 C58 C54 117.0(5) . . ? C57 C58 C53 119.4(5) . . ? C54 C58 C53 123.6(5) . . ? C60 C59 C51 118.2(5) . . ? C60 C59 C52 117.8(5) . . ? C51 C59 C52 124.0(5) . . ? N5 C60 C59 119.9(4) . . ? N5 C60 C57 118.2(4) . . ? C59 C60 C57 121.9(4) . . ? N7 C61 C62 123.8(6) . . ? N7 C61 H61 118.1 . . ? C62 C61 H61 118.1 . . ? C63 C62 C61 118.8(7) . . ? C63 C62 H62 120.6 . . ? C61 C62 H62 120.6 . . ? C62 C63 C71 119.4(7) . . ? C62 C63 H63 120.3 . . ? C71 C63 H63 120.3 . . ? C65 C64 C71 120.9(7) . . ? C65 C64 H64 119.6 . . ? C71 C64 H64 119.6 . . ? C64 C65 C70 121.4(6) . . ? C64 C65 H65 119.3 . . ? C70 C65 H65 119.3 . . ? C67 C66 C70 120.8(6) . . ? C67 C66 H66 119.6 . . ? C70 C66 H66 119.6 . . ? C66 C67 C68 119.3(7) . . ? C66 C67 H67 120.3 . . ? C68 C67 H67 120.3 . . ? N8 C68 C67 121.8(7) . . ? N8 C68 H68 119.1 . . ? C67 C68 H68 119.1 . . ? N8 C69 C70 118.4(6) . . ? N8 C69 C72 119.0(5) . . ? C70 C69 C72 122.5(7) . . ? C66 C70 C69 118.5(7) . . ? C66 C70 C65 124.4(5) . . ? C69 C70 C65 117.0(6) . . ? C72 C71 C63 117.4(6) . . ? C72 C71 C64 120.0(6) . . ? C63 C71 C64 122.6(7) . . ? N7 C72 C71 124.2(6) . . ? N7 C72 C69 117.6(6) . . ? C71 C72 C69 118.2(5) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.979 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.109 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.031 0.500 0.500 1171 239 ' ' _platon_squeeze_details ; P. van der Sluis and A. L. Spek, Acta Crystallogr., 1990, A46, 194. ; ###END data_2a _database_code_depnum_ccdc_archive 'CCDC 715074' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'H5 Sm(H2O)4 (C24H8O24S8) (C12H8N2)4' _chemical_melting_point ? _chemical_formula_moiety 'H5 Sm(H2O)4 [C24H8O24S8] [C12H8N2]4' _chemical_formula_sum 'C72 H53 N8 O28 S8 Sm' _chemical_formula_weight 1885.05 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' Sm Sm -0.1638 3.4418 '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' _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 14.3503(18) _cell_length_b 17.955(2) _cell_length_c 19.182(2) _cell_angle_alpha 112.135(2) _cell_angle_beta 92.414(2) _cell_angle_gamma 97.789(2) _cell_volume 4512.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4567 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 23.87 _exptl_crystal_description tube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1910 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6859 _exptl_absorpt_correction_T_max 0.9265 _exptl_absorpt_process_details ; SADABS, Sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 AXS Apex CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 29922 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_sigmaI/netI 0.1601 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15599 _reflns_number_gt 9313 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (1998)' _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. In order to subtract the contribution from the disordered solvent molecules, the SQUEEZE command was used. All the non-hydrogen atoms were refined anisotropically. The oxygen atoms of two sulfonate groups (O17-O19, O26-O28) were refined with disordered positions and the same displacement parameters for all oxygen atoms on one sulfonate group. The short contact O25...C68, C57...O26A, C64...O18A and C67...O26B might be due to the high mobility of the isolated phenanthroline molecules. ; _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^)+(0.0779P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15599 _refine_ls_number_parameters 1050 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1236 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1572 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.937 _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 Sm1 Sm 0.032119(11) 0.755824(9) 0.019452(10) 0.02208(4) Uani 1 1 d . . . S1 S 0.08393(5) 1.01402(4) 0.09242(4) 0.0259(2) Uani 1 1 d . . . S2 S -0.22448(5) 0.83180(4) 0.14615(4) 0.0253(2) Uani 1 1 d . . . S3 S 0.00315(5) 0.59562(4) 0.12208(5) 0.0283(2) Uani 1 1 d . . . S4 S 0.32007(5) 0.81656(4) 0.15597(5) 0.0269(2) Uani 1 1 d . . . S5 S 0.33713(7) 1.13482(5) 0.33766(5) 0.0426(3) Uani 1 1 d . . . S6 S -0.20710(5) 1.15739(4) 0.22904(5) 0.0298(2) Uani 1 1 d . . . S7 S -0.15806(7) 0.73482(6) 0.37707(5) 0.0484(3) Uani 1 1 d . . . S8 S 0.32056(7) 0.59596(5) 0.28873(6) 0.0553(3) Uani 1 1 d . . . N1 N -0.37624(17) 1.15280(13) 0.05776(15) 0.0297(8) Uani 1 1 d . . . N2 N -0.31159(17) 1.01004(14) 0.01162(14) 0.0277(8) Uani 1 1 d . . . N3 N 0.10449(18) 1.06190(17) 0.45819(15) 0.0437(10) Uani 1 1 d . . . N4 N 0.14447(19) 0.99253(18) 0.55694(15) 0.0471(11) Uani 1 1 d . . . N5 N 0.34420(18) 0.43708(15) 0.08137(17) 0.0441(10) Uani 1 1 d . . . N6 N 0.5281(2) 0.45242(16) 0.13247(18) 0.0549(11) Uani 1 1 d . . . N7 N -0.3646(2) 1.02864(18) 0.55766(16) 0.0495(11) Uani 1 1 d . . . N8 N -0.3815(2) 0.87004(18) 0.46864(17) 0.0524(11) Uani 1 1 d . . . O1 O 0.16881(13) 0.85609(10) 0.06067(11) 0.0257(6) Uani 1 1 d . A . O2 O -0.01907(13) 0.86787(10) 0.11168(11) 0.0247(6) Uani 1 1 d . . . O3 O -0.09858(14) 0.70440(11) 0.06564(10) 0.0238(6) Uani 1 1 d . . . O4 O 0.10635(13) 0.74976(11) 0.12693(11) 0.0293(6) Uani 1 1 d . B . O5 O 0.07030(16) 0.79096(13) -0.08833(13) 0.0535(8) Uani 1 1 d . . . O6 O -0.02940(15) 0.62853(11) -0.09011(12) 0.0336(7) Uani 1 1 d . . . O7 O 0.16757(14) 0.68222(11) -0.02787(12) 0.0360(7) Uani 1 1 d . . . O8 O -0.11446(13) 0.77995(10) -0.04180(11) 0.0265(6) Uani 1 1 d . . . O9 O 0.07233(15) 0.95505(13) 0.01667(13) 0.0471(8) Uani 1 1 d . . . O10 O 0.10868(13) 1.09910(11) 0.10559(12) 0.0313(7) Uani 1 1 d . . . O11 O -0.24773(13) 0.78922(11) 0.06552(11) 0.0289(7) Uani 1 1 d . . . O12 O -0.30387(14) 0.85003(12) 0.19001(12) 0.0332(7) Uani 1 1 d . . . O13 O -0.02308(14) 0.52590(11) 0.14091(13) 0.0356(7) Uani 1 1 d . . . O14 O 0.00557(18) 0.58531(15) 0.04647(15) 0.0630(10) Uani 1 1 d . . . O15 O 0.32041(13) 0.77811(11) 0.07572(11) 0.0289(6) Uani 1 1 d . . . O16 O 0.41143(13) 0.84060(11) 0.20093(12) 0.0324(7) Uani 1 1 d . . . O17A O 0.3932(6) 1.1895(4) 0.3137(4) 0.0658(9) Uani 0.349(2) 1 d P A 1 O18A O 0.4136(6) 1.1090(4) 0.3795(4) 0.0658(9) Uani 0.349(2) 1 d P A 1 O19A O 0.2795(6) 1.1658(5) 0.3915(4) 0.0658(9) Uani 0.349(2) 1 d P A 1 O17B O 0.3144(3) 1.2035(2) 0.3208(2) 0.0658(9) Uani 0.651(2) 1 d P A 2 O18B O 0.4358(3) 1.1337(2) 0.3395(2) 0.0658(9) Uani 0.651(2) 1 d P A 2 O19B O 0.2984(3) 1.1260(2) 0.4015(2) 0.0658(9) Uani 0.651(2) 1 d P A 2 O20 O -0.29267(15) 1.13206(12) 0.25813(12) 0.0430(8) Uani 1 1 d . . . O21 O -0.13854(17) 1.21947(13) 0.28637(13) 0.0480(8) Uani 1 1 d . . . O22 O -0.22596(14) 1.18194(11) 0.16606(12) 0.0344(7) Uani 1 1 d . . . O23 O -0.23027(18) 0.66573(14) 0.36583(14) 0.0586(9) Uani 1 1 d . . . O24 O -0.06977(18) 0.72848(17) 0.41191(14) 0.0730(10) Uani 1 1 d . . . O25 O -0.18955(19) 0.81245(16) 0.41622(13) 0.0603(10) Uani 1 1 d . . . O26A O 0.4178(4) 0.5879(3) 0.2537(3) 0.0678(7) Uani 0.516(3) 1 d P B 1 O27A O 0.2716(4) 0.5161(3) 0.2719(3) 0.0678(7) Uani 0.516(3) 1 d P B 1 O28A O 0.3353(4) 0.6438(3) 0.3630(3) 0.0678(7) Uani 0.516(3) 1 d P B 1 O26B O 0.4153(4) 0.6329(3) 0.3013(3) 0.0678(7) Uani 0.484(3) 1 d P B 2 O27B O 0.2963(4) 0.5088(3) 0.2433(3) 0.0678(7) Uani 0.484(3) 1 d P B 2 O28B O 0.2741(4) 0.6245(3) 0.3635(3) 0.0678(7) Uani 0.484(3) 1 d P B 2 C1 C 0.1707(2) 0.99225(15) 0.14694(16) 0.0217(3) Uani 1 1 d U A . C2 C -0.02191(19) 1.00645(15) 0.13594(16) 0.0203(8) Uani 1 1 d U . . C3 C -0.06403(19) 1.07519(16) 0.16492(16) 0.0241(9) Uani 1 1 d U . . H3 H -0.0342 1.1259 0.1653 0.029 Uiso 1 1 calc R . . C4 C -0.1515(2) 1.06864(16) 0.19372(16) 0.0251(9) Uani 1 1 d . . . C5 C -0.1956(2) 0.99547(15) 0.19111(15) 0.0223(9) Uani 1 1 d U . . H5 H -0.2558 0.9919 0.2095 0.027 Uiso 1 1 calc R . . C6 C -0.1540(2) 0.92553(15) 0.16191(16) 0.0214(9) Uani 1 1 d . . . C7 C -0.16063(19) 0.77391(16) 0.18318(16) 0.0227(9) Uani 1 1 d U . . C8 C -0.1747(2) 0.78141(18) 0.25645(17) 0.0293(10) Uani 1 1 d . . . H8 H -0.2101 0.8209 0.2861 0.035 Uiso 1 1 calc R . . C9 C -0.1373(2) 0.73133(18) 0.28660(17) 0.0312(10) Uani 1 1 d . . . C10 C -0.08504(19) 0.67268(18) 0.24156(17) 0.0264(10) Uani 1 1 d . . . H10 H -0.0601 0.6374 0.2612 0.032 Uiso 1 1 calc R . . C11 C -0.0704(2) 0.66667(15) 0.16974(17) 0.0233(9) Uani 1 1 d . . . C12 C 0.1185(2) 0.64237(17) 0.16772(17) 0.0277(10) Uani 1 1 d . B . C13 C 0.1652(2) 0.60662(17) 0.20686(17) 0.0308(10) Uani 1 1 d . . . H13 H 0.1346 0.5600 0.2139 0.037 Uiso 1 1 calc R B . C14 C 0.2591(2) 0.64014(17) 0.23644(17) 0.0318(10) Uani 1 1 d . B . C15 C 0.3036(2) 0.70788(16) 0.22453(17) 0.0301(10) Uani 1 1 d . . . H15 H 0.3679 0.7297 0.2434 0.036 Uiso 1 1 calc R B . C16 C 0.2529(2) 0.74399(16) 0.18428(17) 0.0267(9) Uani 1 1 d . B . C17 C 0.2684(2) 0.90710(16) 0.17721(16) 0.0244(9) Uani 1 1 d . A . C18 C 0.3089(2) 0.97299(17) 0.24263(18) 0.0335(10) Uani 1 1 d . . . H18 H 0.3549 0.9657 0.2756 0.040 Uiso 1 1 calc R A . C19 C 0.2827(2) 1.04876(17) 0.25979(17) 0.0282(10) Uani 1 1 d . A . C20 C 0.2112(2) 1.05605(16) 0.21004(17) 0.0272(9) Uani 1 1 d U . . H20 H 0.1913 1.1074 0.2215 0.033 Uiso 1 1 calc R A . C21 C 0.19919(19) 0.91340(15) 0.12246(17) 0.0243(9) Uani 1 1 d . . . C22 C -0.06231(19) 0.92915(16) 0.13350(16) 0.0207(9) Uani 1 1 d . . . C23 C -0.10936(19) 0.71408(15) 0.13362(16) 0.0208(9) Uani 1 1 d U . . C24 C 0.1558(2) 0.71407(16) 0.15801(17) 0.0269(10) Uani 1 1 d . . . C25 C -0.4028(2) 1.22725(18) 0.08856(19) 0.0365(11) Uani 1 1 d . . . H25 H -0.3712 1.2669 0.1348 0.044 Uiso 1 1 calc R . . C26 C -0.4778(2) 1.24466(19) 0.0508(2) 0.0447(12) Uani 1 1 d . . . H26 H -0.4984 1.2960 0.0709 0.054 Uiso 1 1 calc R . . C27 C -0.5207(2) 1.18460(18) -0.0167(2) 0.0450(11) Uani 1 1 d . . . H27 H -0.5719 1.1955 -0.0425 0.054 Uiso 1 1 calc R . . C28 C -0.5313(2) 1.0440(2) -0.11800(19) 0.0415(11) Uani 1 1 d U . . H28 H -0.5814 1.0525 -0.1467 0.050 Uiso 1 1 calc R . . C29 C -0.5014(2) 0.9748(2) -0.14310(19) 0.0413(12) Uani 1 1 d . . . H29 H -0.5300 0.9339 -0.1898 0.050 Uiso 1 1 calc R . . C30 C -0.3927(2) 0.88462(19) -0.12423(18) 0.0367(11) Uani 1 1 d . . . H30 H -0.4194 0.8414 -0.1702 0.044 Uiso 1 1 calc R . . C31 C -0.3210(2) 0.87368(18) -0.07981(18) 0.0360(11) Uani 1 1 d . . . H31 H -0.2979 0.8234 -0.0946 0.043 Uiso 1 1 calc R . . C32 C -0.2843(2) 0.93866(16) -0.01302(18) 0.0313(10) Uani 1 1 d . . . H32 H -0.2354 0.9307 0.0172 0.038 Uiso 1 1 calc R . . C33 C -0.3829(2) 1.01833(16) -0.03440(17) 0.0249(9) Uani 1 1 d . . . C34 C -0.4249(2) 0.95779(18) -0.10160(17) 0.0327(10) Uani 1 1 d . . . C35 C -0.4913(2) 1.10784(17) -0.04868(18) 0.0314(10) Uani 1 1 d . . . C36 C -0.4164(2) 1.09501(17) -0.00719(18) 0.0304(10) Uani 1 1 d . . . C37 C 0.0815(3) 1.1012(3) 0.4151(2) 0.0632(16) Uani 1 1 d . . . H37 H 0.0815 1.1583 0.4362 0.076 Uiso 1 1 calc R . . C38 C 0.0568(3) 1.0547(2) 0.3364(2) 0.0574(14) Uani 1 1 d . . . H38 H 0.0383 1.0806 0.3041 0.069 Uiso 1 1 calc R . . C39 C 0.0596(2) 0.9746(2) 0.3078(2) 0.0522(14) Uani 1 1 d . . . H39 H 0.0440 0.9445 0.2550 0.063 Uiso 1 1 calc R . . C40 C 0.0898(2) 0.8509(2) 0.3255(2) 0.0578(15) Uani 1 1 d . . . H40 H 0.0767 0.8191 0.2729 0.069 Uiso 1 1 calc R . . C41 C 0.1129(3) 0.8149(3) 0.3724(2) 0.0664(17) Uani 1 1 d . . . H41 H 0.1185 0.7588 0.3522 0.080 Uiso 1 1 calc R . . C42 C 0.1512(3) 0.8262(3) 0.5046(2) 0.0682(16) Uani 1 1 d . . . H42 H 0.1546 0.7697 0.4874 0.082 Uiso 1 1 calc R . . C43 C 0.1678(3) 0.8745(3) 0.5798(2) 0.0654(15) Uani 1 1 d . . . H43 H 0.1823 0.8521 0.6157 0.079 Uiso 1 1 calc R . . C44 C 0.1630(2) 0.9575(2) 0.6033(2) 0.0572(14) Uani 1 1 d . . . H44 H 0.1738 0.9903 0.6559 0.069 Uiso 1 1 calc R . . C45 C 0.1286(2) 0.9431(2) 0.48168(19) 0.0438(12) Uani 1 1 d . . . C46 C 0.1294(3) 0.8609(2) 0.4537(2) 0.0542(14) Uani 1 1 d . . . C47 C 0.0846(2) 0.9348(2) 0.35289(19) 0.0499(14) Uani 1 1 d . . . C48 C 0.1053(2) 0.9813(2) 0.43130(19) 0.0419(12) Uani 1 1 d . . . C49 C 0.2540(2) 0.4261(2) 0.0537(2) 0.0540(15) Uani 1 1 d . . . H49 H 0.2126 0.3788 0.0509 0.065 Uiso 1 1 calc R . . C50 C 0.2195(3) 0.4794(2) 0.0298(2) 0.0576(13) Uani 1 1 d U . . H50 H 0.1546 0.4703 0.0119 0.069 Uiso 1 1 calc R . . C51 C 0.2793(3) 0.5475(2) 0.0316(2) 0.0539(13) Uani 1 1 d . . . H51 H 0.2559 0.5854 0.0145 0.065 Uiso 1 1 calc R . . C52 C 0.4433(3) 0.63074(19) 0.0662(2) 0.0526(13) Uani 1 1 d . . . H52 H 0.4242 0.6710 0.0504 0.063 Uiso 1 1 calc R . . C53 C 0.5336(3) 0.63970(19) 0.0948(2) 0.0546(14) Uani 1 1 d . . . H53 H 0.5770 0.6864 0.0988 0.065 Uiso 1 1 calc R . . C54 C 0.6602(3) 0.5902(2) 0.1493(3) 0.0730(19) Uani 1 1 d . . . H54 H 0.7050 0.6369 0.1558 0.088 Uiso 1 1 calc R . . C55 C 0.6849(3) 0.5289(2) 0.1686(3) 0.0854(19) Uani 1 1 d . . . H55 H 0.7477 0.5324 0.1887 0.102 Uiso 1 1 calc R . . C56 C 0.6179(3) 0.4621(2) 0.1585(3) 0.0776(16) Uani 1 1 d . . . H56 H 0.6375 0.4199 0.1712 0.093 Uiso 1 1 calc R . . C57 C 0.5027(2) 0.51342(17) 0.1138(2) 0.0390(12) Uani 1 1 d . . . C58 C 0.5651(2) 0.58138(18) 0.1191(2) 0.0409(12) Uani 1 1 d . . . C59 C 0.3754(2) 0.56032(17) 0.05927(19) 0.0363(11) Uani 1 1 d . . . C60 C 0.4051(2) 0.50347(18) 0.0835(2) 0.0385(11) Uani 1 1 d . . . C61 C -0.3591(3) 1.1069(2) 0.5984(2) 0.0604(16) Uani 1 1 d . . . H61 H -0.3444 1.1251 0.6515 0.072 Uiso 1 1 calc R . . C62 C -0.3733(3) 1.1651(3) 0.5691(2) 0.0693(18) Uani 1 1 d . . . H62 H -0.3713 1.2203 0.6020 0.083 Uiso 1 1 calc R . . C63 C -0.3900(3) 1.1425(2) 0.4934(2) 0.0595(15) Uani 1 1 d . . . H63 H -0.3974 1.1817 0.4721 0.071 Uiso 1 1 calc R . . C64 C -0.4138(3) 1.0306(2) 0.3652(2) 0.0532(14) Uani 1 1 d . . . H64 H -0.4200 1.0681 0.3419 0.064 Uiso 1 1 calc R . . C65 C -0.4218(2) 0.9494(2) 0.32139(19) 0.0448(13) Uani 1 1 d . . . H65 H -0.4339 0.9308 0.2680 0.054 Uiso 1 1 calc R . . C66 C -0.4218(2) 0.8089(2) 0.3156(2) 0.0464(12) Uani 1 1 d U . . H66 H -0.4356 0.7874 0.2622 0.056 Uiso 1 1 calc R . . C67 C -0.4125(3) 0.7571(2) 0.3506(2) 0.0578(15) Uani 1 1 d . . . H67 H -0.4200 0.6999 0.3230 0.069 Uiso 1 1 calc R . . C68 C -0.3912(3) 0.7918(3) 0.4298(2) 0.0683(16) Uani 1 1 d . . . H68 H -0.3836 0.7569 0.4558 0.082 Uiso 1 1 calc R . . C69 C -0.3907(2) 0.9239(2) 0.4347(2) 0.0411(11) Uani 1 1 d U . . C70 C -0.4119(2) 0.8926(2) 0.3556(2) 0.0459(13) Uani 1 1 d . . . C71 C -0.3960(2) 1.0604(2) 0.4474(2) 0.0500(14) Uani 1 1 d . . . C72 C -0.3825(2) 1.0082(2) 0.48019(18) 0.0409(12) 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 Sm1 0.01096(6) 0.02829(6) 0.03006(8) 0.01169(6) 0.00479(6) 0.01130(5) S1 0.0104(3) 0.0376(3) 0.0395(4) 0.0229(3) 0.0056(3) 0.0116(3) S2 0.0102(3) 0.0350(3) 0.0329(4) 0.0141(3) 0.0029(3) 0.0085(3) S3 0.0196(4) 0.0321(3) 0.0349(4) 0.0122(3) 0.0053(3) 0.0115(3) S4 0.0123(3) 0.0381(3) 0.0389(4) 0.0210(3) 0.0048(3) 0.0139(3) S5 0.0460(5) 0.0510(4) 0.0338(5) 0.0141(4) 0.0022(4) 0.0248(4) S6 0.0228(4) 0.0377(3) 0.0331(4) 0.0123(3) 0.0074(3) 0.0211(3) S7 0.0360(5) 0.0843(6) 0.0336(5) 0.0281(4) 0.0099(4) 0.0207(4) S8 0.0560(6) 0.0476(4) 0.0701(6) 0.0342(4) -0.0233(5) 0.0097(4) N1 0.0155(12) 0.0302(10) 0.0554(15) 0.0295(10) 0.0048(12) 0.0051(10) N2 0.0163(12) 0.0416(12) 0.0338(14) 0.0230(10) 0.0057(11) 0.0071(10) N3 0.0207(14) 0.0887(17) 0.0330(15) 0.0322(13) 0.0138(12) 0.0177(13) N4 0.0179(14) 0.0923(19) 0.0278(15) 0.0197(14) 0.0034(12) 0.0081(14) N5 0.0181(14) 0.0336(13) 0.067(2) 0.0078(13) -0.0115(14) -0.0025(12) N6 0.0291(16) 0.0408(13) 0.093(2) 0.0288(13) -0.0198(15) 0.0001(12) N7 0.0230(15) 0.0762(19) 0.0354(17) 0.0113(15) 0.0028(14) -0.0071(15) N8 0.0340(17) 0.0692(18) 0.0406(18) 0.0054(15) -0.0005(15) 0.0118(15) O1 0.0115(9) 0.0291(9) 0.0343(12) 0.0084(8) -0.0001(9) 0.0086(8) O2 0.0132(10) 0.0318(9) 0.0336(11) 0.0147(8) 0.0048(9) 0.0117(8) O3 0.0214(10) 0.0316(9) 0.0187(10) 0.0104(8) 0.0003(9) 0.0035(8) O4 0.0149(10) 0.0458(9) 0.0426(11) 0.0301(8) 0.0101(9) 0.0152(8) O5 0.0270(12) 0.0919(12) 0.0797(14) 0.0667(10) 0.0182(11) 0.0330(10) O6 0.0289(11) 0.0393(10) 0.0373(12) 0.0152(9) 0.0079(10) 0.0188(9) O7 0.0266(11) 0.0422(9) 0.0497(13) 0.0226(9) 0.0113(10) 0.0247(8) O8 0.0171(10) 0.0357(9) 0.0340(11) 0.0170(8) 0.0067(9) 0.0165(8) O9 0.0257(11) 0.0816(13) 0.0518(13) 0.0370(10) 0.0126(10) 0.0310(10) O10 0.0077(9) 0.0443(9) 0.0569(12) 0.0334(8) 0.0108(9) 0.0109(8) O11 0.0061(9) 0.0461(10) 0.0366(12) 0.0172(9) 0.0001(9) 0.0081(8) O12 0.0131(10) 0.0536(11) 0.0429(12) 0.0258(9) 0.0140(9) 0.0146(9) O13 0.0197(11) 0.0287(9) 0.0588(14) 0.0147(9) 0.0087(10) 0.0108(8) O14 0.0385(14) 0.0920(16) 0.0604(16) 0.0257(13) 0.0020(13) 0.0287(12) O15 0.0149(10) 0.0454(10) 0.0359(11) 0.0216(8) 0.0102(9) 0.0172(8) O16 0.0118(10) 0.0460(10) 0.0454(12) 0.0216(9) -0.0014(9) 0.0143(8) O17A 0.0640(14) 0.0732(14) 0.0479(13) 0.0111(11) -0.0090(12) 0.0118(12) O18A 0.0640(14) 0.0732(14) 0.0479(13) 0.0111(11) -0.0090(12) 0.0118(12) O19A 0.0640(14) 0.0732(14) 0.0479(13) 0.0111(11) -0.0090(12) 0.0118(12) O17B 0.0640(14) 0.0732(14) 0.0479(13) 0.0111(11) -0.0090(12) 0.0118(12) O18B 0.0640(14) 0.0732(14) 0.0479(13) 0.0111(11) -0.0090(12) 0.0118(12) O19B 0.0640(14) 0.0732(14) 0.0479(13) 0.0111(11) -0.0090(12) 0.0118(12) O20 0.0304(11) 0.0617(11) 0.0551(13) 0.0314(10) 0.0276(10) 0.0344(9) O21 0.0445(14) 0.0412(11) 0.0443(14) -0.0005(10) -0.0108(12) 0.0163(10) O22 0.0265(11) 0.0479(9) 0.0447(12) 0.0284(8) 0.0096(10) 0.0257(8) O23 0.0518(16) 0.0796(14) 0.0641(15) 0.0458(11) 0.0244(13) 0.0171(13) O24 0.0416(15) 0.1526(19) 0.0472(14) 0.0561(12) 0.0059(12) 0.0378(14) O25 0.0552(16) 0.0832(16) 0.0326(14) 0.0081(13) 0.0129(13) 0.0180(14) O26A 0.0593(13) 0.0888(10) 0.0754(12) 0.0513(8) -0.0121(10) 0.0271(10) O27A 0.0593(13) 0.0888(10) 0.0754(12) 0.0513(8) -0.0121(10) 0.0271(10) O28A 0.0593(13) 0.0888(10) 0.0754(12) 0.0513(8) -0.0121(10) 0.0271(10) O26B 0.0593(13) 0.0888(10) 0.0754(12) 0.0513(8) -0.0121(10) 0.0271(10) O27B 0.0593(13) 0.0888(10) 0.0754(12) 0.0513(8) -0.0121(10) 0.0271(10) O28B 0.0593(13) 0.0888(10) 0.0754(12) 0.0513(8) -0.0121(10) 0.0271(10) C1 0.0212(5) 0.0223(5) 0.0221(5) 0.0089(3) 0.0015(4) 0.0049(4) C2 0.0089(13) 0.0298(12) 0.0275(15) 0.0141(10) 0.0027(11) 0.0110(10) C3 0.0162(14) 0.0320(12) 0.0313(15) 0.0183(11) -0.0017(12) 0.0110(11) C4 0.0242(15) 0.0367(13) 0.0228(15) 0.0161(11) 0.0031(13) 0.0194(11) C5 0.0148(13) 0.0341(12) 0.0238(14) 0.0154(10) 0.0005(12) 0.0115(11) C6 0.0147(14) 0.0273(12) 0.0269(15) 0.0158(11) -0.0022(12) 0.0046(11) C7 0.0094(13) 0.0305(13) 0.0308(15) 0.0137(11) 0.0026(12) 0.0058(11) C8 0.0183(15) 0.0402(16) 0.0233(17) 0.0047(13) 0.0044(14) 0.0066(13) C9 0.0193(16) 0.0488(16) 0.0245(16) 0.0142(13) -0.0025(14) 0.0040(14) C10 0.0080(14) 0.0442(15) 0.0293(16) 0.0167(12) 0.0011(13) 0.0050(12) C11 0.0145(14) 0.0245(12) 0.0317(17) 0.0107(11) 0.0001(13) 0.0071(11) C12 0.0209(15) 0.0388(14) 0.0313(17) 0.0166(12) 0.0124(13) 0.0191(12) C13 0.0331(17) 0.0362(14) 0.0302(17) 0.0177(12) 0.0073(14) 0.0129(13) C14 0.0387(18) 0.0383(14) 0.0258(16) 0.0190(11) -0.0075(14) 0.0142(13) C15 0.0279(16) 0.0389(14) 0.0294(17) 0.0156(12) 0.0018(14) 0.0180(12) C16 0.0152(14) 0.0407(13) 0.0347(16) 0.0225(12) 0.0046(13) 0.0158(11) C17 0.0180(14) 0.0315(13) 0.0333(16) 0.0198(11) 0.0105(13) 0.0123(11) C18 0.0205(16) 0.0540(15) 0.0412(17) 0.0315(13) 0.0087(14) 0.0160(13) C19 0.0210(15) 0.0407(14) 0.0334(17) 0.0211(12) 0.0141(13) 0.0161(12) C20 0.0137(13) 0.0354(13) 0.0406(16) 0.0196(11) 0.0054(12) 0.0158(11) C21 0.0108(13) 0.0288(12) 0.0463(17) 0.0253(11) 0.0165(13) 0.0098(11) C22 0.0117(13) 0.0340(13) 0.0178(15) 0.0086(11) 0.0020(12) 0.0124(11) C23 0.0089(13) 0.0231(12) 0.0289(15) 0.0120(11) -0.0043(12) -0.0060(11) C24 0.0191(15) 0.0361(14) 0.0302(17) 0.0152(12) 0.0016(13) 0.0128(12) C25 0.0113(15) 0.0518(16) 0.056(2) 0.0286(14) 0.0069(14) 0.0112(13) C26 0.0208(16) 0.0591(16) 0.077(2) 0.0446(14) 0.0225(16) 0.0209(13) C27 0.0128(16) 0.0640(16) 0.082(2) 0.0558(14) -0.0002(15) 0.0053(14) C28 0.0179(16) 0.0698(18) 0.0390(18) 0.0243(14) -0.0033(14) 0.0069(14) C29 0.0178(17) 0.066(2) 0.0395(19) 0.0243(16) -0.0009(15) -0.0044(16) C30 0.0216(17) 0.0535(18) 0.0322(18) 0.0159(15) 0.0068(15) -0.0021(15) C31 0.0364(19) 0.0308(14) 0.0428(19) 0.0135(13) 0.0169(16) 0.0099(14) C32 0.0225(15) 0.0413(13) 0.0473(18) 0.0299(12) 0.0154(14) 0.0202(12) C33 0.0176(15) 0.0320(13) 0.0328(16) 0.0220(11) 0.0111(13) -0.0007(12) C34 0.0277(17) 0.0492(16) 0.0312(17) 0.0259(13) 0.0067(14) 0.0073(14) C35 0.0121(15) 0.0464(14) 0.0492(18) 0.0346(12) 0.0026(14) 0.0019(13) C36 0.0123(15) 0.0413(14) 0.0503(18) 0.0339(12) 0.0024(14) -0.0016(12) C37 0.030(2) 0.116(3) 0.040(2) 0.024(2) 0.0166(18) 0.019(2) C38 0.030(2) 0.115(3) 0.044(2) 0.0493(17) 0.0081(17) 0.0139(19) C39 0.0200(18) 0.099(3) 0.034(2) 0.0198(19) 0.0062(16) 0.0131(18) C40 0.0196(18) 0.087(3) 0.047(2) 0.003(2) -0.0053(18) 0.0144(18) C41 0.025(2) 0.074(3) 0.078(3) 0.006(2) 0.004(2) 0.0057(19) C42 0.048(2) 0.114(3) 0.057(2) 0.045(2) 0.004(2) 0.024(2) C43 0.037(2) 0.113(3) 0.059(2) 0.0464(19) 0.0008(19) 0.020(2) C44 0.0255(19) 0.113(3) 0.035(2) 0.0273(19) 0.0004(16) 0.0220(19) C45 0.0157(17) 0.080(2) 0.0372(19) 0.0272(16) 0.0020(15) 0.0001(16) C46 0.033(2) 0.091(2) 0.039(2) 0.0230(19) 0.0117(17) 0.0158(19) C47 0.0130(16) 0.103(3) 0.0306(19) 0.0219(18) 0.0077(15) 0.0077(18) C48 0.0186(17) 0.073(2) 0.0351(19) 0.0223(16) 0.0063(15) 0.0049(16) C49 0.0267(19) 0.0419(19) 0.074(3) -0.0001(19) -0.001(2) 0.0079(16) C50 0.0286(17) 0.0695(19) 0.059(2) 0.0020(17) -0.0033(17) 0.0278(15) C51 0.059(2) 0.0703(19) 0.039(2) 0.0176(16) 0.0050(18) 0.0433(16) C52 0.067(2) 0.0396(15) 0.066(2) 0.0282(15) 0.021(2) 0.0304(15) C53 0.064(3) 0.0289(16) 0.069(3) 0.0147(16) 0.014(2) 0.0125(17) C54 0.030(2) 0.052(2) 0.103(4) -0.002(2) -0.004(2) -0.0076(19) C55 0.041(2) 0.056(2) 0.152(4) 0.039(2) -0.032(3) -0.0008(19) C56 0.048(2) 0.0609(19) 0.130(3) 0.0473(19) -0.030(2) 0.0085(18) C57 0.0250(17) 0.0210(14) 0.063(2) 0.0108(14) -0.0091(17) -0.0036(13) C58 0.0325(18) 0.0307(16) 0.048(2) 0.0011(15) 0.0089(17) 0.0095(14) C59 0.0345(17) 0.0351(13) 0.045(2) 0.0140(13) 0.0086(15) 0.0274(12) C60 0.0261(17) 0.0341(15) 0.047(2) 0.0061(14) -0.0083(16) 0.0108(13) C61 0.027(2) 0.091(3) 0.040(2) 0.005(2) 0.0057(18) -0.007(2) C62 0.038(2) 0.091(3) 0.058(3) 0.005(2) 0.020(2) 0.008(2) C63 0.044(2) 0.079(2) 0.054(2) 0.0270(19) 0.012(2) 0.002(2) C64 0.0307(19) 0.094(2) 0.048(2) 0.0403(17) 0.0166(17) 0.0120(18) C65 0.0152(16) 0.090(2) 0.0282(18) 0.0209(17) 0.0061(14) 0.0098(17) C66 0.0179(16) 0.079(2) 0.0317(18) 0.0100(15) -0.0041(14) 0.0071(15) C67 0.035(2) 0.077(2) 0.042(2) 0.001(2) 0.0002(19) 0.0091(19) C68 0.034(2) 0.120(3) 0.061(2) 0.043(2) -0.0036(19) 0.025(2) C69 0.0158(16) 0.0593(18) 0.0472(19) 0.0193(15) 0.0088(15) 0.0048(14) C70 0.0089(15) 0.084(2) 0.035(2) 0.0123(18) 0.0011(15) 0.0085(16) C71 0.0219(18) 0.083(2) 0.028(2) 0.0017(19) 0.0105(16) 0.0058(18) C72 0.0193(17) 0.073(2) 0.0234(18) 0.0109(16) 0.0035(15) 0.0055(16) _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 Sm1 O4 2.327(2) . ? Sm1 O3 2.333(2) . ? Sm1 O2 2.3547(17) . ? Sm1 O1 2.3566(17) . ? Sm1 O5 2.441(3) . ? Sm1 O6 2.4693(17) . ? Sm1 O7 2.508(2) . ? Sm1 O8 2.533(2) . ? S1 O9 1.426(2) . ? S1 O10 1.442(2) . ? S1 C1 1.768(3) . ? S1 C2 1.777(3) . ? S2 O11 1.444(2) . ? S2 O12 1.445(2) . ? S2 C6 1.754(3) . ? S2 C7 1.784(3) . ? S3 O14 1.394(3) . ? S3 O13 1.437(2) . ? S3 C11 1.773(3) . ? S3 C12 1.777(3) . ? S4 O15 1.431(2) . ? S4 O16 1.456(2) . ? S4 C16 1.778(3) . ? S4 C17 1.792(3) . ? S5 O19A 1.351(8) . ? S5 O17A 1.407(9) . ? S5 O18B 1.418(5) . ? S5 O19B 1.419(5) . ? S5 O17B 1.460(5) . ? S5 O18A 1.552(9) . ? S5 C19 1.750(3) . ? S6 O21 1.452(2) . ? S6 O20 1.457(2) . ? S6 O22 1.461(3) . ? S6 C4 1.792(3) . ? S7 O24 1.446(3) . ? S7 O23 1.446(3) . ? S7 O25 1.457(3) . ? S7 C9 1.752(4) . ? S8 O28A 1.347(5) . ? S8 O26B 1.398(6) . ? S8 O27A 1.420(5) . ? S8 O27B 1.460(5) . ? S8 O28B 1.544(6) . ? S8 O26A 1.576(6) . ? S8 C14 1.768(4) . ? N1 C36 1.328(3) . ? N1 C25 1.357(4) . ? N2 C32 1.310(4) . ? N2 C33 1.383(4) . ? N3 C37 1.330(6) . ? N3 C48 1.343(5) . ? N4 C44 1.305(6) . ? N4 C45 1.370(4) . ? N5 C49 1.338(4) . ? N5 C60 1.365(4) . ? N6 C56 1.326(5) . ? N6 C57 1.362(5) . ? N7 C61 1.315(5) . ? N7 C72 1.393(5) . ? N8 C68 1.303(5) . ? N8 C69 1.371(6) . ? O1 C21 1.253(3) . ? O2 C22 1.277(3) . ? O3 C23 1.268(4) . ? O4 C24 1.283(4) . ? C1 C20 1.353(3) . ? C1 C21 1.437(4) . ? C2 C3 1.382(4) . ? C2 C22 1.413(4) . ? C3 C4 1.400(4) . ? C3 H3 0.9500 . ? C4 C5 1.361(4) . ? C5 C6 1.396(4) . ? C5 H5 0.9500 . ? C6 C22 1.448(4) . ? C7 C8 1.387(5) . ? C7 C23 1.450(4) . ? C8 C9 1.389(5) . ? C8 H8 0.9500 . ? C9 C10 1.414(4) . ? C10 C11 1.368(5) . ? C10 H10 0.9500 . ? C11 C23 1.435(5) . ? C12 C13 1.365(5) . ? C12 C24 1.408(4) . ? C13 C14 1.400(4) . ? C13 H13 0.9500 . ? C14 C15 1.397(5) . ? C15 C16 1.416(5) . ? C15 H15 0.9500 . ? C16 C24 1.420(4) . ? C17 C18 1.395(4) . ? C17 C21 1.461(4) . ? C18 C19 1.383(4) . ? C18 H18 0.9500 . ? C19 C20 1.425(4) . ? C20 H20 0.9500 . ? C25 C26 1.407(5) . ? C25 H25 0.9500 . ? C26 C27 1.385(4) . ? C26 H26 0.9500 . ? C27 C35 1.413(4) . ? C27 H27 0.9500 . ? C28 C29 1.293(5) . ? C28 C35 1.421(4) . ? C28 H28 0.9500 . ? C29 C34 1.461(5) . ? C29 H29 0.9500 . ? C30 C34 1.371(5) . ? C30 C31 1.389(5) . ? C30 H30 0.9500 . ? C31 C32 1.390(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.381(4) . ? C33 C36 1.434(4) . ? C35 C36 1.406(5) . ? C37 C38 1.425(5) . ? C37 H37 0.9500 . ? C38 C39 1.340(6) . ? C38 H38 0.9500 . ? C39 C47 1.378(6) . ? C39 H39 0.9500 . ? C40 C41 1.344(7) . ? C40 C47 1.410(6) . ? C40 H40 0.9500 . ? C41 C46 1.455(5) . ? C41 H41 0.9500 . ? C42 C43 1.364(5) . ? C42 C46 1.388(7) . ? C42 H42 0.9500 . ? C43 C44 1.397(6) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.369(5) . ? C45 C48 1.432(6) . ? C47 C48 1.413(4) . ? C49 C50 1.345(6) . ? C49 H49 0.9500 . ? C50 C51 1.384(5) . ? C50 H50 0.9500 . ? C51 C59 1.414(5) . ? C51 H51 0.9500 . ? C52 C53 1.350(6) . ? C52 C59 1.447(5) . ? C52 H52 0.9500 . ? C53 C58 1.412(6) . ? C53 H53 0.9500 . ? C54 C55 1.368(7) . ? C54 C58 1.426(5) . ? C54 H54 0.9500 . ? C55 C56 1.377(6) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.380(5) . ? C57 C60 1.455(5) . ? C59 C60 1.378(5) . ? C61 C62 1.393(7) . ? C61 H61 0.9500 . ? C62 C63 1.353(6) . ? C62 H62 0.9500 . ? C63 C71 1.392(5) . ? C63 H63 0.9500 . ? C64 C65 1.367(5) . ? C64 C71 1.460(5) . ? C64 H64 0.9500 . ? C65 C70 1.423(6) . ? C65 H65 0.9500 . ? C66 C67 1.352(6) . ? C66 C70 1.391(5) . ? C66 H66 0.9500 . ? C67 C68 1.410(5) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.407(5) . ? C69 C72 1.420(5) . ? C71 C72 1.339(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 O4 Sm1 O3 80.33(7) . . ? O4 Sm1 O2 81.19(7) . . ? O3 Sm1 O2 72.87(6) . . ? O4 Sm1 O1 71.71(7) . . ? O3 Sm1 O1 141.03(6) . . ? O2 Sm1 O1 76.42(6) . . ? O4 Sm1 O5 140.16(7) . . ? O3 Sm1 O5 139.45(7) . . ? O2 Sm1 O5 108.62(8) . . ? O1 Sm1 O5 73.42(7) . . ? O4 Sm1 O6 119.71(7) . . ? O3 Sm1 O6 78.87(7) . . ? O2 Sm1 O6 141.29(7) . . ? O1 Sm1 O6 138.76(7) . . ? O5 Sm1 O6 77.01(7) . . ? O4 Sm1 O7 75.88(7) . . ? O3 Sm1 O7 124.82(7) . . ? O2 Sm1 O7 147.09(6) . . ? O1 Sm1 O7 74.17(6) . . ? O5 Sm1 O7 76.62(8) . . ? O6 Sm1 O7 71.49(6) . . ? O4 Sm1 O8 147.20(7) . . ? O3 Sm1 O8 72.43(7) . . ? O2 Sm1 O8 73.67(6) . . ? O1 Sm1 O8 120.64(7) . . ? O5 Sm1 O8 69.57(7) . . ? O6 Sm1 O8 72.91(6) . . ? O7 Sm1 O8 135.19(7) . . ? O9 S1 O10 119.03(15) . . ? O9 S1 C1 109.86(13) . . ? O10 S1 C1 106.48(12) . . ? O9 S1 C2 109.98(12) . . ? O10 S1 C2 105.37(12) . . ? C1 S1 C2 105.18(15) . . ? O11 S2 O12 115.68(12) . . ? O11 S2 C6 107.77(14) . . ? O12 S2 C6 106.61(13) . . ? O11 S2 C7 110.28(13) . . ? O12 S2 C7 106.78(15) . . ? C6 S2 C7 109.57(13) . . ? O14 S3 O13 119.68(14) . . ? O14 S3 C11 112.26(17) . . ? O13 S3 C11 105.84(14) . . ? O14 S3 C12 106.67(16) . . ? O13 S3 C12 107.00(15) . . ? C11 S3 C12 104.25(12) . . ? O15 S4 O16 116.74(12) . . ? O15 S4 C16 106.15(12) . . ? O16 S4 C16 106.39(14) . . ? O15 S4 C17 108.72(14) . . ? O16 S4 C17 106.82(12) . . ? C16 S4 C17 112.11(14) . . ? O19A S5 O17A 117.7(5) . . ? O19A S5 O18B 133.3(4) . . ? O17A S5 O18B 62.3(4) . . ? O19A S5 O19B 36.9(4) . . ? O17A S5 O19B 143.7(3) . . ? O18B S5 O19B 112.6(3) . . ? O19A S5 O17B 79.0(4) . . ? O17A S5 O17B 49.2(4) . . ? O18B S5 O17B 110.8(3) . . ? O19B S5 O17B 115.8(3) . . ? O19A S5 O18A 103.2(5) . . ? O17A S5 O18A 101.1(5) . . ? O18B S5 O18A 41.6(4) . . ? O19B S5 O18A 72.6(4) . . ? O17B S5 O18A 142.5(3) . . ? O19A S5 C19 114.4(3) . . ? O17A S5 C19 110.6(3) . . ? O18B S5 C19 107.17(18) . . ? O19B S5 C19 105.26(19) . . ? O17B S5 C19 104.32(19) . . ? O18A S5 C19 108.4(3) . . ? O21 S6 O20 114.20(14) . . ? O21 S6 O22 110.25(14) . . ? O20 S6 O22 113.29(14) . . ? O21 S6 C4 105.79(14) . . ? O20 S6 C4 105.19(14) . . ? O22 S6 C4 107.47(13) . . ? O24 S7 O23 111.76(18) . . ? O24 S7 O25 112.97(15) . . ? O23 S7 O25 112.62(16) . . ? O24 S7 C9 106.85(16) . . ? O23 S7 C9 106.16(14) . . ? O25 S7 C9 105.89(17) . . ? O28A S8 O26B 74.4(3) . . ? O28A S8 O27A 114.7(3) . . ? O26B S8 O27A 135.7(3) . . ? O28A S8 O27B 136.4(4) . . ? O26B S8 O27B 118.9(3) . . ? O27A S8 O27B 26.0(3) . . ? O28A S8 O28B 35.5(3) . . ? O26B S8 O28B 109.9(3) . . ? O27A S8 O28B 88.4(3) . . ? O27B S8 O28B 114.3(3) . . ? O28A S8 O26A 110.0(3) . . ? O26B S8 O26A 37.5(3) . . ? O27A S8 O26A 107.7(3) . . ? O27B S8 O26A 84.6(3) . . ? O28B S8 O26A 144.2(3) . . ? O28A S8 C14 112.0(3) . . ? O26B S8 C14 107.3(3) . . ? O27A S8 C14 108.0(2) . . ? O27B S8 C14 103.2(3) . . ? O28B S8 C14 101.0(3) . . ? O26A S8 C14 103.7(2) . . ? C36 N1 C25 123.7(3) . . ? C32 N2 C33 115.0(2) . . ? C37 N3 C48 123.5(3) . . ? C44 N4 C45 116.4(3) . . ? C49 N5 C60 119.2(3) . . ? C56 N6 C57 116.2(3) . . ? C61 N7 C72 113.6(4) . . ? C68 N8 C69 121.9(3) . . ? C21 O1 Sm1 133.76(19) . . ? C22 O2 Sm1 153.76(19) . . ? C23 O3 Sm1 127.83(16) . . ? C24 O4 Sm1 150.28(17) . . ? C20 C1 C21 123.2(3) . . ? C20 C1 S1 115.2(2) . . ? C21 C1 S1 121.49(19) . . ? C3 C2 C22 123.6(3) . . ? C3 C2 S1 118.0(2) . . ? C22 C2 S1 118.2(2) . . ? C2 C3 C4 118.8(3) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 120.6(3) . . ? C5 C4 S6 120.7(2) . . ? C3 C4 S6 118.6(2) . . ? C4 C5 C6 121.2(3) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C22 120.6(3) . . ? C5 C6 S2 117.4(2) . . ? C22 C6 S2 121.08(19) . . ? C8 C7 C23 123.4(3) . . ? C8 C7 S2 116.2(2) . . ? C23 C7 S2 119.7(2) . . ? C7 C8 C9 120.2(3) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C10 119.1(3) . . ? C8 C9 S7 122.0(2) . . ? C10 C9 S7 118.8(3) . . ? C11 C10 C9 120.2(3) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C23 124.1(3) . . ? C10 C11 S3 115.4(2) . . ? C23 C11 S3 120.5(2) . . ? C13 C12 C24 124.9(3) . . ? C13 C12 S3 119.5(2) . . ? C24 C12 S3 115.6(2) . . ? C12 C13 C14 118.6(3) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C15 C14 C13 120.0(3) . . ? C15 C14 S8 120.5(2) . . ? C13 C14 S8 119.5(3) . . ? C14 C15 C16 120.0(3) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C24 120.8(3) . . ? C15 C16 S4 116.7(2) . . ? C24 C16 S4 121.7(3) . . ? C18 C17 C21 123.3(3) . . ? C18 C17 S4 115.4(2) . . ? C21 C17 S4 120.60(18) . . ? C19 C18 C17 120.5(3) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 117.8(2) . . ? C18 C19 S5 122.2(2) . . ? C20 C19 S5 120.0(2) . . ? C1 C20 C19 122.1(3) . . ? C1 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? O1 C21 C1 124.0(3) . . ? O1 C21 C17 123.3(3) . . ? C1 C21 C17 112.8(2) . . ? O2 C22 C2 122.5(3) . . ? O2 C22 C6 122.2(3) . . ? C2 C22 C6 115.2(2) . . ? O3 C23 C11 122.8(3) . . ? O3 C23 C7 124.3(3) . . ? C11 C23 C7 112.9(3) . . ? O4 C24 C12 122.7(3) . . ? O4 C24 C16 122.0(3) . . ? C12 C24 C16 115.3(3) . . ? N1 C25 C26 118.8(3) . . ? N1 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C27 C26 C25 118.0(3) . . ? C27 C26 H26 121.0 . . ? C25 C26 H26 121.0 . . ? C26 C27 C35 122.5(3) . . ? C26 C27 H27 118.7 . . ? C35 C27 H27 118.7 . . ? C29 C28 C35 121.9(3) . . ? C29 C28 H28 119.1 . . ? C35 C28 H28 119.1 . . ? C28 C29 C34 121.8(3) . . ? C28 C29 H29 119.1 . . ? C34 C29 H29 119.1 . . ? C34 C30 C31 119.9(3) . . ? C34 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C30 C31 C32 117.9(3) . . ? C30 C31 H31 121.1 . . ? C32 C31 H31 121.1 . . ? N2 C32 C31 125.2(3) . . ? N2 C32 H32 117.4 . . ? C31 C32 H32 117.4 . . ? C34 C33 N2 124.7(3) . . ? C34 C33 C36 119.3(3) . . ? N2 C33 C36 116.0(2) . . ? C30 C34 C33 117.3(3) . . ? C30 C34 C29 124.2(3) . . ? C33 C34 C29 118.5(3) . . ? C36 C35 C27 116.0(3) . . ? C36 C35 C28 118.5(3) . . ? C27 C35 C28 125.4(3) . . ? N1 C36 C35 120.9(3) . . ? N1 C36 C33 119.0(3) . . ? C35 C36 C33 120.0(2) . . ? N3 C37 C38 117.8(4) . . ? N3 C37 H37 121.1 . . ? C38 C37 H37 121.1 . . ? C39 C38 C37 119.9(4) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C47 121.7(3) . . ? C38 C39 H39 119.1 . . ? C47 C39 H39 119.1 . . ? C41 C40 C47 121.4(3) . . ? C41 C40 H40 119.3 . . ? C47 C40 H40 119.3 . . ? C40 C41 C46 120.7(4) . . ? C40 C41 H41 119.6 . . ? C46 C41 H41 119.6 . . ? C43 C42 C46 118.9(4) . . ? C43 C42 H42 120.5 . . ? C46 C42 H42 120.5 . . ? C42 C43 C44 119.2(4) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? N4 C44 C43 123.6(3) . . ? N4 C44 H44 118.2 . . ? C43 C44 H44 118.2 . . ? C46 C45 N4 124.1(4) . . ? C46 C45 C48 119.7(3) . . ? N4 C45 C48 116.1(3) . . ? C45 C46 C42 117.8(3) . . ? C45 C46 C41 119.1(4) . . ? C42 C46 C41 123.0(4) . . ? C39 C47 C40 124.0(3) . . ? C39 C47 C48 117.5(4) . . ? C40 C47 C48 118.5(4) . . ? N3 C48 C47 119.6(4) . . ? N3 C48 C45 120.1(3) . . ? C47 C48 C45 120.3(3) . . ? N5 C49 C50 122.7(3) . . ? N5 C49 H49 118.7 . . ? C50 C49 H49 118.7 . . ? C49 C50 C51 119.5(3) . . ? C49 C50 H50 120.3 . . ? C51 C50 H50 120.3 . . ? C50 C51 C59 119.3(4) . . ? C50 C51 H51 120.3 . . ? C59 C51 H51 120.3 . . ? C53 C52 C59 120.6(4) . . ? C53 C52 H52 119.7 . . ? C59 C52 H52 119.7 . . ? C52 C53 C58 121.6(3) . . ? C52 C53 H53 119.2 . . ? C58 C53 H53 119.2 . . ? C55 C54 C58 117.8(4) . . ? C55 C54 H54 121.1 . . ? C58 C54 H54 121.1 . . ? C54 C55 C56 119.5(4) . . ? C54 C55 H55 120.3 . . ? C56 C55 H55 120.3 . . ? N6 C56 C55 124.8(4) . . ? N6 C56 H56 117.6 . . ? C55 C56 H56 117.6 . . ? N6 C57 C58 123.5(3) . . ? N6 C57 C60 117.3(3) . . ? C58 C57 C60 119.1(3) . . ? C57 C58 C53 119.7(3) . . ? C57 C58 C54 118.2(4) . . ? C53 C58 C54 122.1(3) . . ? C60 C59 C51 117.7(3) . . ? C60 C59 C52 118.3(3) . . ? C51 C59 C52 124.0(3) . . ? N5 C60 C59 121.6(3) . . ? N5 C60 C57 117.8(3) . . ? C59 C60 C57 120.6(3) . . ? N7 C61 C62 124.6(4) . . ? N7 C61 H61 117.7 . . ? C62 C61 H61 117.7 . . ? C63 C62 C61 119.7(4) . . ? C63 C62 H62 120.2 . . ? C61 C62 H62 120.2 . . ? C62 C63 C71 118.1(5) . . ? C62 C63 H63 120.9 . . ? C71 C63 H63 120.9 . . ? C65 C64 C71 120.9(4) . . ? C65 C64 H64 119.6 . . ? C71 C64 H64 119.6 . . ? C64 C65 C70 120.1(3) . . ? C64 C65 H65 119.9 . . ? C70 C65 H65 119.9 . . ? C67 C66 C70 121.9(3) . . ? C67 C66 H66 119.0 . . ? C70 C66 H66 119.0 . . ? C66 C67 C68 117.0(4) . . ? C66 C67 H67 121.5 . . ? C68 C67 H67 121.5 . . ? N8 C68 C67 122.3(5) . . ? N8 C68 H68 118.8 . . ? C67 C68 H68 118.8 . . ? N8 C69 C70 118.3(3) . . ? N8 C69 C72 119.3(3) . . ? C70 C69 C72 122.3(4) . . ? C66 C70 C69 118.6(4) . . ? C66 C70 C65 123.9(3) . . ? C69 C70 C65 117.5(3) . . ? C72 C71 C63 118.4(3) . . ? C72 C71 C64 119.7(3) . . ? C63 C71 C64 121.9(4) . . ? C71 C72 N7 125.5(3) . . ? C71 C72 C69 119.4(3) . . ? N7 C72 C69 115.1(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.313 _refine_diff_density_min -1.792 _refine_diff_density_rms 0.144 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.044 0.500 0.500 1132 293 ' ' _platon_squeeze_details ; P. van der Sluis and A. L. Spek, Acta Crystallogr., 1990, A46, 194. ; ###END data_3a _database_code_depnum_ccdc_archive 'CCDC 715075' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'H5 Tb(H2O)4 (C24H8O24S8) (C12H8N2)4' _chemical_melting_point ? _chemical_formula_moiety 'H5 Tb(H2O)4 [C24H8O24S8] [C12H8N2]4' _chemical_formula_sum 'C72 H53 N8 O28 S8 Tb' _chemical_formula_weight 1893.62 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' Tb Tb -0.1723 4.1537 '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' _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 14.3599(10) _cell_length_b 18.1656(12) _cell_length_c 19.2901(13) _cell_angle_alpha 112.7280(10) _cell_angle_beta 92.5900(10) _cell_angle_gamma 97.6210(10) _cell_volume 4574.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5126 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.62 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1916 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7298 _exptl_absorpt_correction_T_max 0.8811 _exptl_absorpt_process_details ; SADABS, Sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 AXS Apex CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 30983 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15908 _reflns_number_gt 12829 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXTL (Sheldrick, 1998)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL (1998)' _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. In order to subtract the contribution from the disordered solvent molecules, the SQUEEZE command was used. All the non-hydrogen atoms were refined anisotropically. The oxygen atoms of two sulfonate groups (O17-O19, O26-O28) were refined with disordered positions and the same displacement parameters for all oxygen atoms on one sulfonate group. The short contact O25...C68, C57...O26A and C67...O26B might be due to the high mobility of the isolated phenanthroline molecules. ; _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^)+(0.0775P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15908 _refine_ls_number_parameters 1050 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1245 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.033214(15) 0.758984(13) 0.021627(11) 0.02075(8) Uani 1 1 d . . . S1 S 0.08507(8) 1.01374(7) 0.09233(6) 0.0228(3) Uani 1 1 d . . . S2 S -0.22204(8) 0.83365(7) 0.14606(6) 0.0243(3) Uani 1 1 d . . . S3 S 0.00498(8) 0.59923(7) 0.12194(6) 0.0257(3) Uani 1 1 d . . . S4 S 0.32046(8) 0.81883(7) 0.15574(6) 0.0233(3) Uani 1 1 d . . . S5 S 0.33718(10) 1.13400(9) 0.33916(7) 0.0390(3) Uani 1 1 d . . . S6 S -0.20732(8) 1.15536(8) 0.22671(7) 0.0291(3) Uani 1 1 d . . . S7 S -0.15863(10) 0.73700(11) 0.37480(8) 0.0496(4) Uani 1 1 d . . . S8 S 0.32600(11) 0.59879(10) 0.28237(10) 0.0529(4) Uani 1 1 d . . . N1 N -0.3751(3) 1.1536(2) 0.0591(2) 0.0300(9) Uani 1 1 d . . . N2 N -0.3144(3) 1.0092(3) 0.0097(2) 0.0306(10) Uani 1 1 d . . . N3 N 0.1060(3) 1.0599(3) 0.4575(2) 0.0419(12) Uani 1 1 d . . . N4 N 0.1434(3) 0.9948(3) 0.5582(2) 0.0461(13) Uani 1 1 d . . . N5 N 0.3455(3) 0.4390(3) 0.0726(3) 0.0425(12) Uani 1 1 d . . . N6 N 0.5297(3) 0.4526(3) 0.1246(3) 0.0478(13) Uani 1 1 d . . . N7 N -0.3634(3) 1.0306(4) 0.5566(3) 0.0555(15) Uani 1 1 d . . . N8 N -0.3814(3) 0.8722(4) 0.4656(3) 0.0575(16) Uani 1 1 d . . . O1 O 0.1680(2) 0.85597(18) 0.06046(16) 0.0236(7) Uani 1 1 d . A . O2 O -0.0159(2) 0.86976(18) 0.11294(16) 0.0239(7) Uani 1 1 d . . . O3 O -0.0957(2) 0.70895(18) 0.06583(16) 0.0231(7) Uani 1 1 d . . . O4 O 0.1067(2) 0.75316(18) 0.12764(16) 0.0231(7) Uani 1 1 d . B . O5 O 0.0699(3) 0.7901(2) -0.0864(2) 0.0445(10) Uani 1 1 d . . . O6 O -0.0263(2) 0.6326(2) -0.08452(18) 0.0343(8) Uani 1 1 d . . . O7 O 0.1651(2) 0.6856(2) -0.02321(17) 0.0313(8) Uani 1 1 d . . . O8 O -0.1090(2) 0.7827(2) -0.03919(17) 0.0307(8) Uani 1 1 d . . . O9 O 0.0729(2) 0.9553(2) 0.01602(17) 0.0299(8) Uani 1 1 d . . . O10 O 0.1095(2) 1.0984(2) 0.10526(19) 0.0305(8) Uani 1 1 d . . . O11 O -0.2462(2) 0.79056(19) 0.06584(17) 0.0287(8) Uani 1 1 d . . . O12 O -0.3008(2) 0.8529(2) 0.19062(19) 0.0335(8) Uani 1 1 d . . . O13 O -0.0190(2) 0.5292(2) 0.13978(19) 0.0352(8) Uani 1 1 d . . . O14 O 0.0050(2) 0.5866(2) 0.04400(17) 0.0343(8) Uani 1 1 d . . . O15 O 0.3213(2) 0.78021(19) 0.07483(17) 0.0265(7) Uani 1 1 d . . . O16 O 0.4113(2) 0.8421(2) 0.20059(18) 0.0298(8) Uani 1 1 d . . . O17A O 0.3978(10) 1.1851(9) 0.3104(7) 0.0705(12) Uani 0.331(4) 1 d P A 1 O18A O 0.3974(10) 1.1061(9) 0.3876(8) 0.0705(12) Uani 0.331(4) 1 d P A 1 O19A O 0.2666(10) 1.1772(9) 0.3773(8) 0.0705(12) Uani 0.331(4) 1 d P A 1 O17B O 0.3121(5) 1.2029(4) 0.3249(4) 0.0705(12) Uani 0.669(4) 1 d P A 2 O18B O 0.4344(5) 1.1347(4) 0.3390(4) 0.0705(12) Uani 0.669(4) 1 d P A 2 O19B O 0.2973(5) 1.1275(4) 0.4019(4) 0.0705(12) Uani 0.669(4) 1 d P A 2 O20 O -0.2927(3) 1.1310(2) 0.2552(2) 0.0450(10) Uani 1 1 d . . . O21 O -0.1407(3) 1.2174(2) 0.28538(19) 0.0445(10) Uani 1 1 d . . . O22 O -0.2264(2) 1.1792(2) 0.16405(19) 0.0366(8) Uani 1 1 d . . . O23 O -0.2335(3) 0.6700(3) 0.3620(2) 0.0597(12) Uani 1 1 d . . . O24 O -0.0706(3) 0.7275(4) 0.4085(2) 0.0876(19) Uani 1 1 d . . . O25 O -0.1880(3) 0.8143(3) 0.4141(2) 0.0640(13) Uani 1 1 d . . . O26A O 0.4229(6) 0.5968(6) 0.2503(5) 0.0633(12) Uani 0.555(6) 1 d P B 1 O27A O 0.2821(7) 0.5195(7) 0.2640(5) 0.0633(12) Uani 0.555(6) 1 d P B 1 O28A O 0.3394(7) 0.6464(6) 0.3604(5) 0.0633(12) Uani 0.555(6) 1 d P B 1 O26B O 0.4181(8) 0.6348(8) 0.2963(7) 0.0633(12) Uani 0.445(6) 1 d P B 2 O27B O 0.2993(9) 0.5096(8) 0.2321(7) 0.0633(12) Uani 0.445(6) 1 d P B 2 O28B O 0.2818(8) 0.6242(7) 0.3568(6) 0.0633(12) Uani 0.445(6) 1 d P B 2 C1 C 0.1715(3) 0.9926(3) 0.1468(2) 0.0219(10) Uani 1 1 d . A . C2 C -0.0209(3) 1.0067(3) 0.1344(2) 0.0208(10) Uani 1 1 d . . . C3 C -0.0640(3) 1.0744(3) 0.1632(2) 0.0211(10) Uani 1 1 d . . . H3 H -0.0343 1.1246 0.1636 0.025 Uiso 1 1 calc R . . C4 C -0.1515(3) 1.0691(3) 0.1918(2) 0.0237(10) Uani 1 1 d . . . C5 C -0.1944(3) 0.9959(3) 0.1902(2) 0.0234(10) Uani 1 1 d . . . H5 H -0.2539 0.9922 0.2093 0.028 Uiso 1 1 calc R . . C6 C -0.1519(3) 0.9270(3) 0.1609(2) 0.0224(10) Uani 1 1 d . . . C7 C -0.1602(3) 0.7753(3) 0.1814(2) 0.0226(10) Uani 1 1 d . . . C8 C -0.1731(3) 0.7832(3) 0.2555(3) 0.0284(11) Uani 1 1 d . . . H8 H -0.2071 0.8232 0.2859 0.034 Uiso 1 1 calc R . . C9 C -0.1368(3) 0.7330(3) 0.2842(2) 0.0296(11) Uani 1 1 d . . . C10 C -0.0843(3) 0.6763(3) 0.2401(3) 0.0279(11) Uani 1 1 d . . . H10 H -0.0584 0.6423 0.2602 0.033 Uiso 1 1 calc R . . C11 C -0.0694(3) 0.6689(3) 0.1681(2) 0.0240(10) Uani 1 1 d . . . C12 C 0.1195(3) 0.6473(3) 0.1675(2) 0.0257(10) Uani 1 1 d . B . C13 C 0.1689(3) 0.6114(3) 0.2048(2) 0.0270(11) Uani 1 1 d . . . H13 H 0.1394 0.5648 0.2113 0.032 Uiso 1 1 calc R B . C14 C 0.2628(3) 0.6441(3) 0.2329(3) 0.0297(11) Uani 1 1 d . B . C15 C 0.3048(3) 0.7109(3) 0.2209(3) 0.0278(11) Uani 1 1 d . . . H15 H 0.3694 0.7324 0.2387 0.033 Uiso 1 1 calc R B . C16 C 0.2549(3) 0.7463(3) 0.1837(2) 0.0226(10) Uani 1 1 d . B . C17 C 0.2691(3) 0.9076(3) 0.1771(2) 0.0223(10) Uani 1 1 d . A . C18 C 0.3096(3) 0.9736(3) 0.2421(3) 0.0276(11) Uani 1 1 d . . . H18 H 0.3560 0.9671 0.2751 0.033 Uiso 1 1 calc R A . C19 C 0.2831(3) 1.0480(3) 0.2591(2) 0.0265(11) Uani 1 1 d . A . C20 C 0.2129(3) 1.0571(3) 0.2117(3) 0.0254(10) Uani 1 1 d . . . H20 H 0.1934 1.1083 0.2243 0.031 Uiso 1 1 calc R A . C21 C 0.1999(3) 0.9139(3) 0.1239(2) 0.0231(10) Uani 1 1 d . . . C22 C -0.0607(3) 0.9298(3) 0.1336(2) 0.0200(10) Uani 1 1 d . . . C23 C -0.1076(3) 0.7173(3) 0.1337(2) 0.0212(10) Uani 1 1 d . . . C24 C 0.1577(3) 0.7178(3) 0.1570(2) 0.0225(10) Uani 1 1 d . . . C25 C -0.4030(4) 1.2253(3) 0.0885(3) 0.0373(13) Uani 1 1 d . . . H25 H -0.3722 1.2649 0.1351 0.045 Uiso 1 1 calc R . . C26 C -0.4769(4) 1.2428(4) 0.0512(3) 0.0422(14) Uani 1 1 d . . . H26 H -0.4965 1.2942 0.0720 0.051 Uiso 1 1 calc R . . C27 C -0.5210(4) 1.1847(4) -0.0158(3) 0.0398(13) Uani 1 1 d . . . H27 H -0.5717 1.1959 -0.0416 0.048 Uiso 1 1 calc R . . C28 C -0.5337(4) 1.0455(4) -0.1171(3) 0.0403(14) Uani 1 1 d . . . H28 H -0.5840 1.0544 -0.1451 0.048 Uiso 1 1 calc R . . C29 C -0.5033(4) 0.9745(4) -0.1442(3) 0.0407(14) Uani 1 1 d . . . H29 H -0.5316 0.9343 -0.1914 0.049 Uiso 1 1 calc R . . C30 C -0.3950(4) 0.8843(3) -0.1266(3) 0.0426(15) Uani 1 1 d . . . H30 H -0.4211 0.8416 -0.1731 0.051 Uiso 1 1 calc R . . C31 C -0.3240(4) 0.8735(3) -0.0823(3) 0.0406(14) Uani 1 1 d . . . H31 H -0.3017 0.8232 -0.0972 0.049 Uiso 1 1 calc R . . C32 C -0.2859(4) 0.9382(3) -0.0151(3) 0.0357(12) Uani 1 1 d . . . H32 H -0.2364 0.9307 0.0146 0.043 Uiso 1 1 calc R . . C33 C -0.3843(3) 1.0186(3) -0.0344(3) 0.0294(11) Uani 1 1 d . . . C34 C -0.4281(3) 0.9576(3) -0.1031(3) 0.0338(12) Uani 1 1 d . . . C35 C -0.4921(3) 1.1091(3) -0.0465(3) 0.0329(12) Uani 1 1 d . . . C36 C -0.4169(3) 1.0947(3) -0.0074(3) 0.0287(11) Uani 1 1 d . . . C37 C 0.0835(4) 1.0957(4) 0.4122(3) 0.0503(16) Uani 1 1 d . . . H37 H 0.0838 1.1524 0.4321 0.060 Uiso 1 1 calc R . . C38 C 0.0593(4) 1.0493(5) 0.3346(3) 0.0531(18) Uani 1 1 d . . . H38 H 0.0403 1.0742 0.3023 0.064 Uiso 1 1 calc R . . C39 C 0.0632(4) 0.9694(5) 0.3058(3) 0.0515(18) Uani 1 1 d . . . H39 H 0.0493 0.9388 0.2530 0.062 Uiso 1 1 calc R . . C40 C 0.0923(4) 0.8484(4) 0.3273(3) 0.0488(16) Uani 1 1 d . . . H40 H 0.0802 0.8155 0.2748 0.059 Uiso 1 1 calc R . . C41 C 0.1136(4) 0.8158(4) 0.3761(4) 0.0609(19) Uani 1 1 d . . . H41 H 0.1174 0.7598 0.3569 0.073 Uiso 1 1 calc R . . C42 C 0.1511(5) 0.8300(5) 0.5090(4) 0.068(2) Uani 1 1 d . . . H42 H 0.1544 0.7740 0.4932 0.082 Uiso 1 1 calc R . . C43 C 0.1660(5) 0.8795(5) 0.5840(4) 0.065(2) Uani 1 1 d . . . H43 H 0.1786 0.8585 0.6209 0.078 Uiso 1 1 calc R . . C44 C 0.1625(4) 0.9605(5) 0.6050(3) 0.0568(19) Uani 1 1 d . . . H44 H 0.1749 0.9943 0.6573 0.068 Uiso 1 1 calc R . . C45 C 0.1288(4) 0.9434(4) 0.4834(3) 0.0435(15) Uani 1 1 d . . . C46 C 0.1310(4) 0.8614(4) 0.4557(3) 0.0511(16) Uani 1 1 d . . . C47 C 0.0876(3) 0.9310(4) 0.3535(3) 0.0434(16) Uani 1 1 d . . . C48 C 0.1068(3) 0.9798(4) 0.4319(3) 0.0389(14) Uani 1 1 d . . . C49 C 0.2540(4) 0.4300(4) 0.0460(3) 0.0565(19) Uani 1 1 d . . . H49 H 0.2112 0.3837 0.0421 0.068 Uiso 1 1 calc R . . C50 C 0.2221(4) 0.4872(5) 0.0244(3) 0.0580(19) Uani 1 1 d . . . H50 H 0.1581 0.4802 0.0051 0.070 Uiso 1 1 calc R . . C51 C 0.2833(5) 0.5530(4) 0.0310(3) 0.0548(17) Uani 1 1 d . . . H51 H 0.2616 0.5926 0.0164 0.066 Uiso 1 1 calc R . . C52 C 0.4453(5) 0.6344(4) 0.0689(3) 0.0491(15) Uani 1 1 d . . . H52 H 0.4261 0.6750 0.0545 0.059 Uiso 1 1 calc R . . C53 C 0.5344(4) 0.6438(3) 0.0981(3) 0.0458(15) Uani 1 1 d . . . H53 H 0.5767 0.6916 0.1052 0.055 Uiso 1 1 calc R . . C54 C 0.6609(4) 0.5895(4) 0.1481(4) 0.0550(17) Uani 1 1 d . . . H54 H 0.7064 0.6356 0.1554 0.066 Uiso 1 1 calc R . . C55 C 0.6854(4) 0.5295(4) 0.1655(4) 0.0632(19) Uani 1 1 d . . . H55 H 0.7479 0.5331 0.1863 0.076 Uiso 1 1 calc R . . C56 C 0.6179(4) 0.4620(4) 0.1526(4) 0.068(2) Uani 1 1 d . . . H56 H 0.6367 0.4198 0.1648 0.081 Uiso 1 1 calc R . . C57 C 0.5041(4) 0.5126(3) 0.1082(3) 0.0362(13) Uani 1 1 d . . . C58 C 0.5674(4) 0.5837(3) 0.1188(3) 0.0409(14) Uani 1 1 d . . . C59 C 0.3779(4) 0.5645(3) 0.0589(3) 0.0407(13) Uani 1 1 d . . . C60 C 0.4078(4) 0.5056(3) 0.0789(3) 0.0345(12) Uani 1 1 d . . . C61 C -0.3585(4) 1.1076(5) 0.5994(4) 0.064(2) Uani 1 1 d . . . H61 H -0.3457 1.1244 0.6525 0.077 Uiso 1 1 calc R . . C62 C -0.3709(5) 1.1657(5) 0.5719(4) 0.074(2) Uani 1 1 d . . . H62 H -0.3670 1.2207 0.6056 0.089 Uiso 1 1 calc R . . C63 C -0.3888(5) 1.1435(5) 0.4956(4) 0.074(2) Uani 1 1 d . . . H63 H -0.3968 1.1828 0.4756 0.089 Uiso 1 1 calc R . . C64 C -0.4139(4) 1.0309(5) 0.3658(4) 0.066(2) Uani 1 1 d . . . H64 H -0.4214 1.0680 0.3430 0.080 Uiso 1 1 calc R . . C65 C -0.4212(4) 0.9542(5) 0.3222(3) 0.059(2) Uani 1 1 d . . . H65 H -0.4326 0.9366 0.2689 0.070 Uiso 1 1 calc R . . C66 C -0.4219(4) 0.8123(5) 0.3128(3) 0.060(2) Uani 1 1 d . . . H66 H -0.4350 0.7910 0.2593 0.072 Uiso 1 1 calc R . . C67 C -0.4130(4) 0.7622(5) 0.3472(4) 0.065(2) Uani 1 1 d . . . H67 H -0.4222 0.7055 0.3187 0.077 Uiso 1 1 calc R . . C68 C -0.3903(5) 0.7934(5) 0.4252(4) 0.068(2) Uani 1 1 d . . . H68 H -0.3811 0.7580 0.4496 0.081 Uiso 1 1 calc R . . C69 C -0.3910(3) 0.9255(5) 0.4339(3) 0.0499(17) Uani 1 1 d . . . C70 C -0.4120(4) 0.8971(5) 0.3547(3) 0.0539(19) Uani 1 1 d . . . C71 C -0.3950(4) 1.0620(5) 0.4476(3) 0.060(2) Uani 1 1 d . . . C72 C -0.3828(4) 1.0088(4) 0.4812(3) 0.0475(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02098(12) 0.02172(13) 0.01916(12) 0.00715(9) 0.00191(8) 0.00520(9) S1 0.0205(6) 0.0259(6) 0.0288(6) 0.0167(5) 0.0055(5) 0.0072(5) S2 0.0177(5) 0.0248(6) 0.0311(6) 0.0121(5) 0.0026(5) 0.0019(5) S3 0.0269(6) 0.0203(6) 0.0301(6) 0.0103(5) 0.0008(5) 0.0040(5) S4 0.0182(5) 0.0273(7) 0.0285(6) 0.0148(5) 0.0030(4) 0.0062(5) S5 0.0464(8) 0.0354(8) 0.0291(7) 0.0059(6) -0.0043(6) 0.0100(6) S6 0.0276(6) 0.0297(7) 0.0301(6) 0.0093(5) 0.0039(5) 0.0124(5) S7 0.0436(8) 0.0823(12) 0.0262(7) 0.0255(8) 0.0050(6) 0.0089(8) S8 0.0515(9) 0.0468(10) 0.0714(11) 0.0407(8) -0.0203(8) 0.0001(7) N1 0.029(2) 0.028(2) 0.036(2) 0.0166(19) 0.0032(18) 0.0027(18) N2 0.026(2) 0.036(3) 0.040(2) 0.024(2) 0.0071(18) 0.0062(18) N3 0.038(3) 0.059(3) 0.028(2) 0.017(2) 0.0091(19) 0.004(2) N4 0.031(2) 0.077(4) 0.027(2) 0.018(2) 0.0036(19) 0.000(2) N5 0.027(2) 0.033(3) 0.053(3) 0.004(2) -0.006(2) -0.001(2) N6 0.036(3) 0.033(3) 0.068(3) 0.017(2) -0.014(2) 0.002(2) N7 0.033(3) 0.083(4) 0.029(2) 0.001(3) 0.005(2) 0.000(3) N8 0.036(3) 0.092(5) 0.029(3) 0.006(3) 0.001(2) 0.014(3) O1 0.0220(16) 0.0254(18) 0.0240(16) 0.0098(14) 0.0026(13) 0.0057(13) O2 0.0214(16) 0.0222(18) 0.0280(16) 0.0092(14) 0.0038(13) 0.0052(13) O3 0.0236(16) 0.0228(17) 0.0231(16) 0.0108(13) -0.0010(13) 0.0003(13) O4 0.0206(16) 0.0259(18) 0.0287(16) 0.0165(14) 0.0009(13) 0.0070(13) O5 0.043(2) 0.069(3) 0.043(2) 0.038(2) 0.0167(17) 0.023(2) O6 0.045(2) 0.029(2) 0.0271(17) 0.0083(15) -0.0020(15) 0.0093(16) O7 0.0325(18) 0.032(2) 0.0294(17) 0.0091(15) 0.0030(14) 0.0138(15) O8 0.0312(18) 0.036(2) 0.0258(17) 0.0126(15) 0.0012(14) 0.0084(15) O9 0.0308(18) 0.038(2) 0.0275(17) 0.0160(15) 0.0069(14) 0.0166(15) O10 0.0253(17) 0.0295(19) 0.046(2) 0.0251(16) 0.0050(15) 0.0038(14) O11 0.0215(16) 0.0307(19) 0.0317(17) 0.0107(15) -0.0016(13) 0.0037(14) O12 0.0208(17) 0.035(2) 0.049(2) 0.0195(17) 0.0144(15) 0.0053(15) O13 0.037(2) 0.0239(19) 0.046(2) 0.0162(16) 0.0019(16) 0.0044(15) O14 0.039(2) 0.035(2) 0.0253(17) 0.0076(15) 0.0018(15) 0.0083(16) O15 0.0241(17) 0.0298(19) 0.0320(17) 0.0169(15) 0.0059(13) 0.0101(14) O16 0.0194(16) 0.034(2) 0.0418(19) 0.0211(16) -0.0012(14) 0.0058(14) O17A 0.065(2) 0.064(3) 0.051(2) -0.0067(18) -0.0105(18) 0.002(2) O18A 0.065(2) 0.064(3) 0.051(2) -0.0067(18) -0.0105(18) 0.002(2) O19A 0.065(2) 0.064(3) 0.051(2) -0.0067(18) -0.0105(18) 0.002(2) O17B 0.065(2) 0.064(3) 0.051(2) -0.0067(18) -0.0105(18) 0.002(2) O18B 0.065(2) 0.064(3) 0.051(2) -0.0067(18) -0.0105(18) 0.002(2) O19B 0.065(2) 0.064(3) 0.051(2) -0.0067(18) -0.0105(18) 0.002(2) O20 0.042(2) 0.044(2) 0.061(2) 0.025(2) 0.0269(19) 0.0246(18) O21 0.050(2) 0.034(2) 0.035(2) -0.0026(17) -0.0091(17) 0.0139(18) O22 0.039(2) 0.034(2) 0.0373(19) 0.0122(16) -0.0025(16) 0.0166(16) O23 0.058(3) 0.080(3) 0.060(3) 0.045(2) 0.021(2) 0.013(2) O24 0.053(3) 0.187(6) 0.046(3) 0.068(3) 0.008(2) 0.029(3) O25 0.064(3) 0.079(3) 0.030(2) 0.003(2) 0.009(2) 0.003(2) O26A 0.060(3) 0.087(3) 0.063(3) 0.051(3) -0.006(3) 0.018(2) O27A 0.060(3) 0.087(3) 0.063(3) 0.051(3) -0.006(3) 0.018(2) O28A 0.060(3) 0.087(3) 0.063(3) 0.051(3) -0.006(3) 0.018(2) O26B 0.060(3) 0.087(3) 0.063(3) 0.051(3) -0.006(3) 0.018(2) O27B 0.060(3) 0.087(3) 0.063(3) 0.051(3) -0.006(3) 0.018(2) O28B 0.060(3) 0.087(3) 0.063(3) 0.051(3) -0.006(3) 0.018(2) C1 0.019(2) 0.026(3) 0.027(2) 0.016(2) 0.0028(18) 0.0041(19) C2 0.020(2) 0.022(2) 0.023(2) 0.0116(19) 0.0047(18) 0.0052(19) C3 0.022(2) 0.021(2) 0.020(2) 0.0079(19) -0.0023(18) 0.0060(19) C4 0.022(2) 0.027(3) 0.023(2) 0.010(2) 0.0000(18) 0.009(2) C5 0.020(2) 0.030(3) 0.023(2) 0.012(2) 0.0026(18) 0.005(2) C6 0.023(2) 0.023(3) 0.020(2) 0.0086(19) -0.0022(18) 0.0024(19) C7 0.023(2) 0.019(2) 0.025(2) 0.0088(19) -0.0008(18) -0.0002(19) C8 0.022(2) 0.026(3) 0.029(2) 0.005(2) 0.0015(19) -0.002(2) C9 0.025(2) 0.043(3) 0.021(2) 0.013(2) 0.0030(19) 0.004(2) C10 0.021(2) 0.034(3) 0.029(2) 0.017(2) -0.0077(19) -0.004(2) C11 0.020(2) 0.026(3) 0.025(2) 0.010(2) 0.0000(18) -0.0018(19) C12 0.028(2) 0.027(3) 0.025(2) 0.012(2) 0.0019(19) 0.007(2) C13 0.037(3) 0.021(3) 0.028(2) 0.015(2) 0.006(2) 0.006(2) C14 0.032(3) 0.032(3) 0.030(3) 0.017(2) -0.002(2) 0.008(2) C15 0.023(2) 0.032(3) 0.029(2) 0.012(2) 0.0035(19) 0.009(2) C16 0.027(2) 0.021(2) 0.023(2) 0.0112(19) 0.0053(19) 0.0081(19) C17 0.020(2) 0.024(3) 0.031(2) 0.017(2) 0.0066(18) 0.0079(19) C18 0.024(2) 0.038(3) 0.027(2) 0.018(2) 0.0036(19) 0.007(2) C19 0.024(2) 0.034(3) 0.023(2) 0.013(2) 0.0050(19) 0.004(2) C20 0.025(2) 0.021(3) 0.035(3) 0.014(2) 0.012(2) 0.0070(19) C21 0.017(2) 0.026(3) 0.031(2) 0.018(2) 0.0079(19) 0.0019(19) C22 0.021(2) 0.022(2) 0.018(2) 0.0083(18) -0.0018(17) 0.0056(19) C23 0.016(2) 0.020(2) 0.026(2) 0.0098(19) -0.0015(18) -0.0041(18) C24 0.027(2) 0.021(2) 0.021(2) 0.0081(19) 0.0033(18) 0.0076(19) C25 0.033(3) 0.036(3) 0.053(3) 0.027(3) 0.014(2) 0.009(2) C26 0.032(3) 0.043(3) 0.070(4) 0.038(3) 0.017(3) 0.015(3) C27 0.025(3) 0.052(4) 0.062(4) 0.042(3) 0.008(3) 0.011(3) C28 0.024(3) 0.063(4) 0.043(3) 0.034(3) -0.004(2) 0.000(3) C29 0.030(3) 0.055(4) 0.035(3) 0.020(3) 0.002(2) -0.007(3) C30 0.045(3) 0.039(3) 0.039(3) 0.012(3) 0.018(3) -0.007(3) C31 0.037(3) 0.036(3) 0.051(3) 0.018(3) 0.020(3) 0.003(2) C32 0.033(3) 0.040(3) 0.045(3) 0.025(3) 0.013(2) 0.013(2) C33 0.024(2) 0.037(3) 0.031(3) 0.018(2) 0.007(2) 0.000(2) C34 0.027(3) 0.042(3) 0.034(3) 0.018(2) 0.009(2) -0.002(2) C35 0.020(2) 0.044(3) 0.045(3) 0.030(3) 0.004(2) 0.000(2) C36 0.026(3) 0.035(3) 0.033(3) 0.023(2) 0.007(2) 0.001(2) C37 0.050(4) 0.066(4) 0.036(3) 0.021(3) 0.010(3) 0.009(3) C38 0.038(3) 0.094(6) 0.029(3) 0.026(3) 0.005(2) 0.007(3) C39 0.035(3) 0.086(5) 0.022(3) 0.013(3) 0.006(2) -0.001(3) C40 0.038(3) 0.061(4) 0.032(3) 0.004(3) 0.005(2) -0.001(3) C41 0.049(4) 0.063(5) 0.056(4) 0.010(4) 0.004(3) 0.006(3) C42 0.064(5) 0.082(6) 0.063(5) 0.034(4) 0.004(4) 0.014(4) C43 0.054(4) 0.097(6) 0.058(4) 0.049(4) -0.004(3) 0.008(4) C44 0.032(3) 0.105(6) 0.034(3) 0.030(4) 0.005(2) 0.009(3) C45 0.027(3) 0.070(4) 0.028(3) 0.016(3) 0.002(2) -0.001(3) C46 0.044(3) 0.061(5) 0.043(3) 0.016(3) 0.005(3) 0.007(3) C47 0.017(2) 0.073(5) 0.029(3) 0.010(3) 0.004(2) -0.001(3) C48 0.021(3) 0.061(4) 0.026(3) 0.012(3) 0.003(2) -0.005(2) C49 0.028(3) 0.055(4) 0.056(4) -0.009(3) -0.005(3) 0.002(3) C50 0.035(3) 0.076(5) 0.045(3) 0.001(3) -0.008(3) 0.024(3) C51 0.064(4) 0.062(5) 0.035(3) 0.008(3) 0.005(3) 0.035(4) C52 0.071(4) 0.035(3) 0.052(4) 0.021(3) 0.025(3) 0.026(3) C53 0.048(4) 0.026(3) 0.062(4) 0.015(3) 0.018(3) 0.008(3) C54 0.037(3) 0.038(4) 0.073(4) 0.011(3) 0.000(3) -0.013(3) C55 0.035(3) 0.058(4) 0.089(5) 0.027(4) -0.019(3) -0.004(3) C56 0.048(4) 0.055(4) 0.096(5) 0.031(4) -0.025(4) 0.003(3) C57 0.032(3) 0.025(3) 0.047(3) 0.011(2) -0.003(2) -0.001(2) C58 0.037(3) 0.024(3) 0.047(3) 0.000(2) 0.005(2) 0.002(2) C59 0.044(3) 0.038(3) 0.039(3) 0.009(3) 0.007(2) 0.020(3) C60 0.032(3) 0.022(3) 0.042(3) 0.005(2) -0.001(2) 0.004(2) C61 0.044(4) 0.100(6) 0.040(4) 0.024(4) 0.010(3) -0.007(4) C62 0.051(4) 0.096(6) 0.049(4) 0.005(4) 0.017(3) -0.008(4) C63 0.059(4) 0.108(7) 0.065(5) 0.043(5) 0.020(4) 0.014(4) C64 0.042(4) 0.110(7) 0.045(4) 0.031(4) 0.009(3) 0.005(4) C65 0.036(3) 0.100(6) 0.030(3) 0.019(4) 0.004(3) 0.001(4) C66 0.022(3) 0.096(6) 0.033(3) -0.003(4) 0.003(2) 0.004(3) C67 0.048(4) 0.083(6) 0.040(4) -0.001(4) 0.000(3) 0.015(4) C68 0.054(4) 0.087(6) 0.052(4) 0.014(4) 0.001(3) 0.020(4) C69 0.016(3) 0.093(5) 0.032(3) 0.015(3) 0.003(2) 0.006(3) C70 0.021(3) 0.091(5) 0.032(3) 0.008(3) 0.004(2) 0.001(3) C71 0.036(3) 0.084(5) 0.042(3) 0.008(4) 0.014(3) 0.001(3) C72 0.024(3) 0.076(5) 0.034(3) 0.014(3) 0.007(2) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O3 2.297(3) . ? Tb1 O4 2.304(3) . ? Tb1 O1 2.315(3) . ? Tb1 O2 2.323(3) . ? Tb1 O5 2.423(3) . ? Tb1 O6 2.425(3) . ? Tb1 O7 2.458(3) . ? Tb1 O8 2.478(3) . ? S1 O9 1.430(3) . ? S1 O10 1.451(3) . ? S1 C1 1.766(4) . ? S1 C2 1.770(4) . ? S2 O11 1.439(3) . ? S2 O12 1.449(3) . ? S2 C6 1.766(4) . ? S2 C7 1.769(5) . ? S3 O14 1.431(3) . ? S3 O13 1.446(3) . ? S3 C11 1.763(5) . ? S3 C12 1.771(5) . ? S4 O15 1.444(3) . ? S4 O16 1.448(3) . ? S4 C17 1.773(5) . ? S4 C16 1.783(4) . ? S5 O18B 1.395(7) . ? S5 O19B 1.401(8) . ? S5 O19A 1.420(16) . ? S5 O17B 1.465(8) . ? S5 O17A 1.467(16) . ? S5 O18A 1.512(16) . ? S5 C19 1.770(5) . ? S6 O21 1.448(3) . ? S6 O20 1.451(4) . ? S6 O22 1.460(4) . ? S6 C4 1.765(5) . ? S7 O25 1.445(5) . ? S7 O23 1.447(4) . ? S7 O24 1.455(5) . ? S7 C9 1.765(5) . ? S8 O26B 1.360(11) . ? S8 O27A 1.394(11) . ? S8 O28A 1.406(9) . ? S8 O27B 1.516(14) . ? S8 O28B 1.525(12) . ? S8 O26A 1.547(9) . ? S8 C14 1.773(5) . ? N1 C25 1.329(7) . ? N1 C36 1.359(6) . ? N2 C32 1.318(7) . ? N2 C33 1.357(6) . ? N3 C37 1.327(7) . ? N3 C48 1.345(7) . ? N4 C44 1.318(8) . ? N4 C45 1.371(7) . ? N5 C49 1.354(7) . ? N5 C60 1.367(6) . ? N6 C56 1.317(7) . ? N6 C57 1.336(7) . ? N7 C61 1.312(9) . ? N7 C72 1.356(7) . ? N8 C68 1.324(9) . ? N8 C69 1.348(8) . ? O1 C21 1.282(5) . ? O2 C22 1.279(5) . ? O3 C23 1.281(5) . ? O4 C24 1.279(5) . ? C1 C20 1.381(6) . ? C1 C21 1.443(7) . ? C2 C3 1.381(6) . ? C2 C22 1.432(6) . ? C3 C4 1.402(6) . ? C3 H3 0.9500 . ? C4 C5 1.378(6) . ? C5 C6 1.394(7) . ? C5 H5 0.9500 . ? C6 C22 1.436(6) . ? C7 C8 1.403(6) . ? C7 C23 1.432(6) . ? C8 C9 1.379(7) . ? C8 H8 0.9500 . ? C9 C10 1.393(7) . ? C10 C11 1.373(6) . ? C10 H10 0.9500 . ? C11 C23 1.434(6) . ? C12 C13 1.372(7) . ? C12 C24 1.417(6) . ? C13 C14 1.392(6) . ? C13 H13 0.9500 . ? C14 C15 1.387(7) . ? C15 C16 1.369(6) . ? C15 H15 0.9500 . ? C16 C24 1.421(6) . ? C17 C18 1.391(6) . ? C17 C21 1.444(6) . ? C18 C19 1.373(7) . ? C18 H18 0.9500 . ? C19 C20 1.398(7) . ? C20 H20 0.9500 . ? C25 C26 1.393(8) . ? C25 H25 0.9500 . ? C26 C27 1.372(8) . ? C26 H26 0.9500 . ? C27 C35 1.397(8) . ? C27 H27 0.9500 . ? C28 C29 1.333(8) . ? C28 C35 1.441(7) . ? C28 H28 0.9500 . ? C29 C34 1.445(8) . ? C29 H29 0.9500 . ? C30 C31 1.384(8) . ? C30 C34 1.386(8) . ? C30 H30 0.9500 . ? C31 C32 1.396(7) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.409(7) . ? C33 C36 1.428(7) . ? C35 C36 1.399(7) . ? C37 C38 1.405(8) . ? C37 H37 0.9500 . ? C38 C39 1.348(9) . ? C38 H38 0.9500 . ? C39 C47 1.412(9) . ? C39 H39 0.9500 . ? C40 C41 1.334(9) . ? C40 C47 1.398(9) . ? C40 H40 0.9500 . ? C41 C46 1.426(8) . ? C41 H41 0.9500 . ? C42 C43 1.364(9) . ? C42 C46 1.392(9) . ? C42 H42 0.9500 . ? C43 C44 1.375(10) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.381(9) . ? C45 C48 1.435(8) . ? C47 C48 1.417(7) . ? C49 C50 1.381(10) . ? C49 H49 0.9500 . ? C50 C51 1.345(9) . ? C50 H50 0.9500 . ? C51 C59 1.397(8) . ? C51 H51 0.9500 . ? C52 C53 1.336(8) . ? C52 C59 1.432(8) . ? C52 H52 0.9500 . ? C53 C58 1.425(8) . ? C53 H53 0.9500 . ? C54 C55 1.340(9) . ? C54 C58 1.409(8) . ? C54 H54 0.9500 . ? C55 C56 1.391(9) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.415(7) . ? C57 C60 1.441(7) . ? C59 C60 1.380(8) . ? C61 C62 1.378(11) . ? C61 H61 0.9500 . ? C62 C63 1.369(9) . ? C62 H62 0.9500 . ? C63 C71 1.399(10) . ? C63 H63 0.9500 . ? C64 C65 1.307(10) . ? C64 C71 1.453(8) . ? C64 H64 0.9500 . ? C65 C70 1.420(10) . ? C65 H65 0.9500 . ? C66 C67 1.333(10) . ? C66 C70 1.420(10) . ? C66 H66 0.9500 . ? C67 C68 1.392(9) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.412(7) . ? C69 C72 1.419(9) . ? C71 C72 1.380(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Tb1 O4 80.53(10) . . ? O3 Tb1 O1 142.36(10) . . ? O4 Tb1 O1 72.62(10) . . ? O3 Tb1 O2 73.48(10) . . ? O4 Tb1 O2 81.22(11) . . ? O1 Tb1 O2 76.71(10) . . ? O3 Tb1 O5 138.62(11) . . ? O4 Tb1 O5 140.68(11) . . ? O1 Tb1 O5 73.38(12) . . ? O2 Tb1 O5 109.36(12) . . ? O3 Tb1 O6 78.03(11) . . ? O4 Tb1 O6 118.09(11) . . ? O1 Tb1 O6 138.09(11) . . ? O2 Tb1 O6 142.20(11) . . ? O5 Tb1 O6 77.09(13) . . ? O3 Tb1 O7 123.83(11) . . ? O4 Tb1 O7 74.97(11) . . ? O1 Tb1 O7 74.11(11) . . ? O2 Tb1 O7 146.64(10) . . ? O5 Tb1 O7 77.26(12) . . ? O6 Tb1 O7 70.84(11) . . ? O3 Tb1 O8 72.89(11) . . ? O4 Tb1 O8 147.84(11) . . ? O1 Tb1 O8 119.91(11) . . ? O2 Tb1 O8 74.18(10) . . ? O5 Tb1 O8 68.75(11) . . ? O6 Tb1 O8 74.05(11) . . ? O7 Tb1 O8 135.42(10) . . ? O9 S1 O10 118.0(2) . . ? O9 S1 C1 110.6(2) . . ? O10 S1 C1 107.0(2) . . ? O9 S1 C2 109.5(2) . . ? O10 S1 C2 105.3(2) . . ? C1 S1 C2 105.7(2) . . ? O11 S2 O12 115.83(19) . . ? O11 S2 C6 107.43(19) . . ? O12 S2 C6 106.3(2) . . ? O11 S2 C7 109.4(2) . . ? O12 S2 C7 106.5(2) . . ? C6 S2 C7 111.4(2) . . ? O14 S3 O13 117.9(2) . . ? O14 S3 C11 111.4(2) . . ? O13 S3 C11 107.4(2) . . ? O14 S3 C12 107.8(2) . . ? O13 S3 C12 107.1(2) . . ? C11 S3 C12 104.4(2) . . ? O15 S4 O16 116.39(19) . . ? O15 S4 C17 108.7(2) . . ? O16 S4 C17 107.2(2) . . ? O15 S4 C16 106.47(19) . . ? O16 S4 C16 105.3(2) . . ? C17 S4 C16 112.8(2) . . ? O18B S5 O19B 116.3(4) . . ? O18B S5 O19A 143.9(6) . . ? O19B S5 O19A 54.2(7) . . ? O18B S5 O17B 109.9(5) . . ? O19B S5 O17B 112.0(4) . . ? O19A S5 O17B 58.9(7) . . ? O18B S5 O17A 57.7(7) . . ? O19B S5 O17A 146.6(6) . . ? O19A S5 O17A 109.0(9) . . ? O17B S5 O17A 53.9(7) . . ? O18B S5 O18A 54.4(6) . . ? O19B S5 O18A 64.1(6) . . ? O19A S5 O18A 113.9(8) . . ? O17B S5 O18A 146.6(6) . . ? O17A S5 O18A 109.5(8) . . ? O18B S5 C19 106.6(3) . . ? O19B S5 C19 106.7(3) . . ? O19A S5 C19 109.5(5) . . ? O17B S5 C19 104.5(3) . . ? O17A S5 C19 106.4(5) . . ? O18A S5 C19 108.3(5) . . ? O21 S6 O20 112.9(2) . . ? O21 S6 O22 110.9(2) . . ? O20 S6 O22 112.9(2) . . ? O21 S6 C4 106.2(2) . . ? O20 S6 C4 106.0(2) . . ? O22 S6 C4 107.4(2) . . ? O25 S7 O23 112.1(3) . . ? O25 S7 O24 114.1(3) . . ? O23 S7 O24 112.2(3) . . ? O25 S7 C9 105.9(3) . . ? O23 S7 C9 105.6(2) . . ? O24 S7 C9 106.1(2) . . ? O26B S8 O27A 133.1(7) . . ? O26B S8 O28A 75.1(6) . . ? O27A S8 O28A 113.7(5) . . ? O26B S8 O27B 120.1(7) . . ? O27A S8 O27B 25.0(5) . . ? O28A S8 O27B 136.6(5) . . ? O26B S8 O28B 108.7(6) . . ? O27A S8 O28B 89.0(6) . . ? O28A S8 O28B 33.7(4) . . ? O27B S8 O28B 114.0(6) . . ? O26B S8 O26A 35.4(5) . . ? O27A S8 O26A 108.6(5) . . ? O28A S8 O26A 109.2(5) . . ? O27B S8 O26A 88.3(6) . . ? O28B S8 O26A 141.8(5) . . ? O26B S8 C14 108.4(5) . . ? O27A S8 C14 109.9(4) . . ? O28A S8 C14 111.3(4) . . ? O27B S8 C14 102.0(5) . . ? O28B S8 C14 101.6(4) . . ? O26A S8 C14 103.5(3) . . ? C25 N1 C36 122.1(5) . . ? C32 N2 C33 116.7(4) . . ? C37 N3 C48 122.3(5) . . ? C44 N4 C45 114.8(6) . . ? C49 N5 C60 120.1(5) . . ? C56 N6 C57 117.2(5) . . ? C61 N7 C72 116.4(6) . . ? C68 N8 C69 122.4(6) . . ? C21 O1 Tb1 132.9(3) . . ? C22 O2 Tb1 152.5(3) . . ? C23 O3 Tb1 128.6(2) . . ? C24 O4 Tb1 149.3(3) . . ? C20 C1 C21 122.0(4) . . ? C20 C1 S1 115.6(4) . . ? C21 C1 S1 122.4(3) . . ? C3 C2 C22 122.9(4) . . ? C3 C2 S1 118.8(3) . . ? C22 C2 S1 118.3(3) . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.5(4) . . ? C5 C4 S6 120.8(3) . . ? C3 C4 S6 119.7(4) . . ? C4 C5 C6 121.1(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C22 121.7(4) . . ? C5 C6 S2 116.9(3) . . ? C22 C6 S2 120.8(3) . . ? C8 C7 C23 122.1(4) . . ? C8 C7 S2 116.6(4) . . ? C23 C7 S2 121.0(3) . . ? C9 C8 C7 120.3(5) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 119.4(4) . . ? C8 C9 S7 121.3(4) . . ? C10 C9 S7 119.2(4) . . ? C11 C10 C9 120.9(5) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C23 122.6(5) . . ? C10 C11 S3 115.4(4) . . ? C23 C11 S3 121.9(3) . . ? C13 C12 C24 123.9(4) . . ? C13 C12 S3 119.2(4) . . ? C24 C12 S3 116.6(3) . . ? C12 C13 C14 119.1(4) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C15 C14 C13 119.3(4) . . ? C15 C14 S8 121.7(4) . . ? C13 C14 S8 119.1(4) . . ? C16 C15 C14 121.2(4) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C24 121.9(4) . . ? C15 C16 S4 117.2(3) . . ? C24 C16 S4 120.0(3) . . ? C18 C17 C21 122.4(4) . . ? C18 C17 S4 115.8(3) . . ? C21 C17 S4 121.2(3) . . ? C19 C18 C17 120.6(4) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 119.7(4) . . ? C18 C19 S5 121.6(4) . . ? C20 C19 S5 118.7(4) . . ? C1 C20 C19 120.9(5) . . ? C1 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? O1 C21 C1 122.3(4) . . ? O1 C21 C17 123.4(4) . . ? C1 C21 C17 114.3(4) . . ? O2 C22 C2 121.9(4) . . ? O2 C22 C6 123.3(4) . . ? C2 C22 C6 114.7(4) . . ? O3 C23 C7 122.9(4) . . ? O3 C23 C11 122.5(4) . . ? C7 C23 C11 114.6(4) . . ? O4 C24 C12 121.7(4) . . ? O4 C24 C16 123.8(4) . . ? C12 C24 C16 114.5(4) . . ? N1 C25 C26 120.4(5) . . ? N1 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C27 C26 C25 119.1(6) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C26 C27 C35 120.5(5) . . ? C26 C27 H27 119.7 . . ? C35 C27 H27 119.7 . . ? C29 C28 C35 121.6(5) . . ? C29 C28 H28 119.2 . . ? C35 C28 H28 119.2 . . ? C28 C29 C34 121.3(5) . . ? C28 C29 H29 119.4 . . ? C34 C29 H29 119.4 . . ? C31 C30 C34 120.0(5) . . ? C31 C30 H30 120.0 . . ? C34 C30 H30 120.0 . . ? C30 C31 C32 118.3(5) . . ? C30 C31 H31 120.8 . . ? C32 C31 H31 120.8 . . ? N2 C32 C31 124.1(5) . . ? N2 C32 H32 117.9 . . ? C31 C32 H32 117.9 . . ? N2 C33 C34 124.2(5) . . ? N2 C33 C36 117.1(4) . . ? C34 C33 C36 118.7(5) . . ? C30 C34 C33 116.6(5) . . ? C30 C34 C29 124.4(5) . . ? C33 C34 C29 118.9(5) . . ? C27 C35 C36 118.3(5) . . ? C27 C35 C28 123.9(5) . . ? C36 C35 C28 117.8(5) . . ? N1 C36 C35 119.6(5) . . ? N1 C36 C33 118.8(4) . . ? C35 C36 C33 121.6(5) . . ? N3 C37 C38 119.7(6) . . ? N3 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C39 C38 C37 120.0(6) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C47 120.6(5) . . ? C38 C39 H39 119.7 . . ? C47 C39 H39 119.7 . . ? C41 C40 C47 120.0(6) . . ? C41 C40 H40 120.0 . . ? C47 C40 H40 120.0 . . ? C40 C41 C46 123.0(7) . . ? C40 C41 H41 118.5 . . ? C46 C41 H41 118.5 . . ? C43 C42 C46 120.1(8) . . ? C43 C42 H42 120.0 . . ? C46 C42 H42 120.0 . . ? C42 C43 C44 118.7(7) . . ? C42 C43 H43 120.7 . . ? C44 C43 H43 120.7 . . ? N4 C44 C43 125.1(6) . . ? N4 C44 H44 117.5 . . ? C43 C44 H44 117.5 . . ? N4 C45 C46 125.2(6) . . ? N4 C45 C48 115.4(6) . . ? C46 C45 C48 119.3(5) . . ? C45 C46 C42 116.2(6) . . ? C45 C46 C41 118.5(6) . . ? C42 C46 C41 125.3(7) . . ? C40 C47 C39 123.3(5) . . ? C40 C47 C48 119.6(6) . . ? C39 C47 C48 117.1(6) . . ? N3 C48 C47 120.2(5) . . ? N3 C48 C45 120.3(5) . . ? C47 C48 C45 119.5(6) . . ? N5 C49 C50 121.0(6) . . ? N5 C49 H49 119.5 . . ? C50 C49 H49 119.5 . . ? C51 C50 C49 118.9(6) . . ? C51 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? C50 C51 C59 121.6(6) . . ? C50 C51 H51 119.2 . . ? C59 C51 H51 119.2 . . ? C53 C52 C59 121.6(6) . . ? C53 C52 H52 119.2 . . ? C59 C52 H52 119.2 . . ? C52 C53 C58 121.4(5) . . ? C52 C53 H53 119.3 . . ? C58 C53 H53 119.3 . . ? C55 C54 C58 119.6(5) . . ? C55 C54 H54 120.2 . . ? C58 C54 H54 120.2 . . ? C54 C55 C56 119.0(6) . . ? C54 C55 H55 120.5 . . ? C56 C55 H55 120.5 . . ? N6 C56 C55 124.3(7) . . ? N6 C56 H56 117.8 . . ? C55 C56 H56 117.8 . . ? N6 C57 C58 123.0(5) . . ? N6 C57 C60 119.1(4) . . ? C58 C57 C60 117.9(5) . . ? C54 C58 C57 116.9(6) . . ? C54 C58 C53 123.9(5) . . ? C57 C58 C53 119.2(5) . . ? C60 C59 C51 118.0(6) . . ? C60 C59 C52 118.2(5) . . ? C51 C59 C52 123.8(6) . . ? N5 C60 C59 120.4(5) . . ? N5 C60 C57 117.9(5) . . ? C59 C60 C57 121.7(5) . . ? N7 C61 C62 123.8(6) . . ? N7 C61 H61 118.1 . . ? C62 C61 H61 118.1 . . ? C63 C62 C61 119.4(8) . . ? C63 C62 H62 120.3 . . ? C61 C62 H62 120.3 . . ? C62 C63 C71 118.9(8) . . ? C62 C63 H63 120.5 . . ? C71 C63 H63 120.5 . . ? C65 C64 C71 123.0(8) . . ? C65 C64 H64 118.5 . . ? C71 C64 H64 118.5 . . ? C64 C65 C70 119.8(6) . . ? C64 C65 H65 120.1 . . ? C70 C65 H65 120.1 . . ? C67 C66 C70 121.0(6) . . ? C67 C66 H66 119.5 . . ? C70 C66 H66 119.5 . . ? C66 C67 C68 119.7(7) . . ? C66 C67 H67 120.1 . . ? C68 C67 H67 120.1 . . ? N8 C68 C67 120.3(8) . . ? N8 C68 H68 119.8 . . ? C67 C68 H68 119.8 . . ? N8 C69 C70 119.5(6) . . ? N8 C69 C72 119.0(5) . . ? C70 C69 C72 121.4(7) . . ? C69 C70 C66 117.0(7) . . ? C69 C70 C65 118.7(7) . . ? C66 C70 C65 124.2(6) . . ? C72 C71 C63 116.9(6) . . ? C72 C71 C64 119.0(7) . . ? C63 C71 C64 124.1(8) . . ? N7 C72 C71 124.5(6) . . ? N7 C72 C69 117.5(6) . . ? C71 C72 C69 118.0(6) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.981 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.107 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.031 0.500 0.500 1180 245 ' ' _platon_squeeze_details ; P. van der Sluis and A. L. Spek, Acta Crystallogr., 1990, A46, 194. ; ###END