############################################################### ##*******iacs chemical crystallography group******* ## this structure was solved by raju mondal on 23/03/2013 ## ############################################################# data_13sb016_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H80 Cl4 N28 O16 Tb8' _chemical_formula_weight 3054.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.2752(12) _cell_length_b 20.1097(10) _cell_length_c 24.1223(12) _cell_angle_alpha 90.00 _cell_angle_beta 101.093(2) _cell_angle_gamma 90.00 _cell_volume 11555.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11322 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 28.17 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5792 _exptl_absorpt_coefficient_mu 4.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4735 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS v.2.03 (Bruker, 2001), wR2(int)=0.1579 before correction' _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 APEX-2 CCD area detector' _diffrn_measurement_method '/w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 80093 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 28.30 _reflns_number_total 13954 _reflns_number_gt 9295 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX-2' _computing_cell_refinement 'Bruker APEX-2' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogen atoms for metal coordinated hydroxyl groups could not be located in the data and therefore have not been included in the refinement. This has led to a difference in calculated and reported formula and consequent alerts in the cif check. ; _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^)+(0.1007P)^2^+16.6183P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13954 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1737 _refine_ls_wR_factor_gt 0.1491 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.089178(15) 0.84699(2) 0.217337(16) 0.03239(12) Uani 1 1 d . . . Tb2 Tb 0.058406(16) 0.77953(2) 0.064289(16) 0.03477(12) Uani 1 1 d . . . Tb3 Tb 0.058163(15) 0.84804(2) 0.364100(16) 0.03267(12) Uani 1 1 d . . . Tb4 Tb 0.198048(16) 0.91895(2) 0.340521(17) 0.03727(12) Uani 1 1 d . . . C6 C 0.1901(3) 0.7242(4) 0.1207(4) 0.0382(19) Uani 1 1 d . . . C11 C 0.3260(4) 0.8820(5) 0.4198(4) 0.050(2) Uani 1 1 d . . . C2S C 0.1459(4) 0.7521(6) 0.4468(5) 0.061(3) Uani 1 1 d . . . H2SA H 0.1681 0.7124 0.4579 0.073 Uiso 1 1 calc R . . H2SB H 0.1294 0.7660 0.4785 0.073 Uiso 1 1 calc R . . O2W O 0.1026(2) 0.9131(3) 0.3003(2) 0.0356(13) Uani 1 1 d . . . O1W O 0.0261(2) 0.7810(3) 0.1505(2) 0.0346(12) Uani 1 1 d . . . O1 O 0.1816(2) 0.8251(3) 0.2809(2) 0.0389(13) Uani 1 1 d . . . N3 N 0.1492(3) 0.7620(4) 0.1872(3) 0.0393(16) Uani 1 1 d . . . N2A N 0.1962(3) 0.9555(4) 0.2447(3) 0.0455(18) Uani 1 1 d . . . N5 N 0.2781(3) 0.8428(4) 0.3333(3) 0.0470(19) Uani 1 1 d . . . N6 N 0.2792(3) 0.9156(4) 0.4262(3) 0.052(2) Uani 1 1 d . . . O1A O 0.0991(2) 0.8699(3) 0.1192(2) 0.0380(13) Uani 1 1 d . . . C7A C 0.2307(4) 0.9626(5) 0.1659(4) 0.046(2) Uani 1 1 d . . . H7AA H 0.2542 0.9714 0.1406 0.055 Uiso 1 1 calc R . . O2S O 0.0645(2) 0.7828(3) 0.2858(2) 0.0410(14) Uani 1 1 d . . . O1S O 0.1554(2) 0.8573(3) 0.4002(2) 0.0423(14) Uani 1 1 d . . . C2SA C 0.0038(4) 0.9938(5) 0.3899(4) 0.051(2) Uani 1 1 d . . . H2SC H 0.0076 1.0412 0.3970 0.061 Uiso 1 1 calc R . . H2SD H -0.0245 0.9767 0.4096 0.061 Uiso 1 1 calc R . . N4A N 0.1528(3) 0.9040(4) 0.0558(3) 0.0428(17) Uani 1 1 d . . . C11A C 0.0724(4) 0.8281(5) -0.0695(4) 0.048(2) Uani 1 1 d . . . N3A N 0.1573(3) 0.9291(4) 0.2026(3) 0.0420(18) Uani 1 1 d . . . C1A C 0.3229(4) 1.0310(5) 0.3556(5) 0.063(3) Uani 1 1 d . . . H1AA H 0.3212 1.0278 0.3937 0.076 Uiso 1 1 calc R . . C5 C 0.1896(4) 0.6995(5) 0.0631(4) 0.044(2) Uani 1 1 d . . . C10A C 0.1108(4) 0.8669(5) -0.0328(4) 0.047(2) Uani 1 1 d . . . H10A H 0.1343 0.8959 -0.0473 0.057 Uiso 1 1 calc R . . N5A N 0.1141(3) 0.8630(4) 0.0203(3) 0.0397(17) Uani 1 1 d . . . N4 N 0.2749(3) 0.8027(4) 0.2866(3) 0.0502(19) Uani 1 1 d . . . Cl2 Cl 0.17181(11) 1.03727(13) 0.37569(12) 0.0598(7) Uani 1 1 d . . . N1S N 0.1008(3) 0.7368(4) 0.3976(3) 0.0485(19) Uani 1 1 d . . . H1SE H 0.0742 0.7116 0.4095 0.058 Uiso 1 1 calc R . . N1 N 0.1417(3) 0.7093(4) 0.0252(3) 0.0458(18) Uani 1 1 d . . . C7 C 0.2326(4) 0.7384(5) 0.1656(4) 0.043(2) Uani 1 1 d . . . H7A H 0.2710 0.7325 0.1680 0.052 Uiso 1 1 calc R . . C1S C 0.1834(4) 0.8069(6) 0.4319(5) 0.064(3) Uani 1 1 d . . . H1SA H 0.2047 0.8255 0.4666 0.077 Uiso 1 1 calc R . . H1SB H 0.2101 0.7875 0.4113 0.077 Uiso 1 1 calc R . . N2 N 0.1394(3) 0.7381(4) 0.1333(3) 0.0422(17) Uani 1 1 d . . . C8A C 0.1773(4) 0.9342(4) 0.1544(4) 0.040(2) Uani 1 1 d . . . C3SA C 0.0706(4) 0.9472(5) 0.4725(4) 0.053(3) Uani 1 1 d . . . H3SA H 0.0674 0.9878 0.4933 0.064 Uiso 1 1 calc R . . H3SB H 0.1090 0.9315 0.4827 0.064 Uiso 1 1 calc R . . C9A C 0.1406(3) 0.9009(4) 0.1058(4) 0.0385(19) Uani 1 1 d . . . C6A C 0.2406(4) 0.9747(5) 0.2223(4) 0.045(2) Uani 1 1 d . . . C15 C 0.2795(5) 0.9502(7) 0.4733(5) 0.068(3) Uani 1 1 d . . . H15A H 0.2474 0.9734 0.4774 0.081 Uiso 1 1 calc R . . C10 C 0.3244(4) 0.8424(5) 0.3713(5) 0.055(3) Uani 1 1 d . . . H10B H 0.3551 0.8170 0.3666 0.066 Uiso 1 1 calc R . . C4S C 0.0766(5) 0.7151(5) 0.2965(4) 0.055(3) Uani 1 1 d . . . H4SA H 0.0912 0.6966 0.2651 0.065 Uiso 1 1 calc R . . H4SB H 0.0420 0.6918 0.2985 0.065 Uiso 1 1 calc R . . N1SA N 0.0566(3) 0.9612(4) 0.4102(3) 0.0417(17) Uani 1 1 d . . . H1SI H 0.0845 0.9865 0.4008 0.050 Uiso 1 1 calc R . . C9 C 0.2213(3) 0.7994(4) 0.2613(4) 0.0386(19) Uani 1 1 d . . . N6A N 0.0375(3) 0.7879(4) -0.0448(3) 0.0492(19) Uani 1 1 d . . . C12 C 0.3729(4) 0.8856(6) 0.4630(5) 0.069(3) Uani 1 1 d . . . H12A H 0.4053 0.8629 0.4591 0.083 Uiso 1 1 calc R . . C5A C 0.2867(4) 1.0049(5) 0.2626(4) 0.051(2) Uani 1 1 d . . . C8 C 0.2051(3) 0.7635(4) 0.2067(4) 0.0389(19) Uani 1 1 d . . . C13 C 0.3729(5) 0.9214(6) 0.5108(5) 0.077(4) Uani 1 1 d . . . H13A H 0.4049 0.9239 0.5389 0.092 Uiso 1 1 calc R . . N1A N 0.2835(3) 0.9989(4) 0.3169(3) 0.0464(18) Uani 1 1 d . . . C15A C -0.0008(5) 0.7534(7) -0.0788(5) 0.071(3) Uani 1 1 d . . . H15B H -0.0241 0.7260 -0.0624 0.085 Uiso 1 1 calc R . . C4A C 0.3305(5) 1.0390(6) 0.2462(5) 0.068(3) Uani 1 1 d . . . H4AB H 0.3336 1.0396 0.2084 0.082 Uiso 1 1 calc R . . C2A C 0.3647(5) 1.0677(6) 0.3401(6) 0.075(4) Uani 1 1 d . . . H2AA H 0.3904 1.0901 0.3673 0.090 Uiso 1 1 calc R . . C3A C 0.3684(6) 1.0712(7) 0.2846(6) 0.096(5) Uani 1 1 d . . . H3AA H 0.3969 1.0956 0.2735 0.116 Uiso 1 1 calc R . . C14A C -0.0091(7) 0.7549(8) -0.1369(5) 0.101(5) Uani 1 1 d . . . H14A H -0.0386 0.7321 -0.1592 0.121 Uiso 1 1 calc R . . C12A C 0.0685(6) 0.8298(6) -0.1263(5) 0.073(3) Uani 1 1 d . . . H12B H 0.0926 0.8563 -0.1424 0.088 Uiso 1 1 calc R . . C13A C 0.0277(7) 0.7911(8) -0.1602(5) 0.098(5) Uani 1 1 d . . . H13B H 0.0258 0.7901 -0.1991 0.118 Uiso 1 1 calc R . . C3S C 0.1190(5) 0.7030(6) 0.3512(5) 0.064(3) Uani 1 1 d . . . H3SC H 0.1223 0.6557 0.3589 0.077 Uiso 1 1 calc R . . H3SD H 0.1556 0.7195 0.3472 0.077 Uiso 1 1 calc R . . C1 C 0.1392(5) 0.6863(6) -0.0256(4) 0.061(3) Uani 1 1 d . . . H1A H 0.1059 0.6914 -0.0518 0.073 Uiso 1 1 calc R . . Cl1 Cl 0.00713(11) 0.66082(13) 0.04875(12) 0.0591(7) Uani 1 1 d . . . C14 C 0.3265(6) 0.9525(6) 0.5162(5) 0.077(4) Uani 1 1 d . . . H14B H 0.3252 0.9761 0.5491 0.092 Uiso 1 1 calc R . . C2 C 0.1845(5) 0.6540(6) -0.0428(5) 0.071(3) Uani 1 1 d . . . H2A H 0.1813 0.6377 -0.0794 0.085 Uiso 1 1 calc R . . C3 C 0.2320(5) 0.6474(6) -0.0055(5) 0.075(4) Uani 1 1 d . . . H3A H 0.2628 0.6275 -0.0163 0.089 Uiso 1 1 calc R . . C4 C 0.2362(4) 0.6695(6) 0.0486(5) 0.059(3) Uani 1 1 d . . . H4B H 0.2694 0.6645 0.0749 0.071 Uiso 1 1 calc R . . C4SA C 0.0309(4) 0.8950(5) 0.4879(4) 0.053(3) Uani 1 1 d . . . H4SC H 0.0462 0.8776 0.5252 0.064 Uiso 1 1 calc R . . H4SD H -0.0049 0.9156 0.4894 0.064 Uiso 1 1 calc R . . C1SA C -0.0142(4) 0.9811(4) 0.3264(4) 0.045(2) Uani 1 1 d . . . H1SC H -0.0514 0.9993 0.3131 0.054 Uiso 1 1 calc R . . H1SD H 0.0116 1.0031 0.3063 0.054 Uiso 1 1 calc R . . O1SA O -0.0147(2) 0.9124(3) 0.3152(2) 0.0369(13) Uani 1 1 d . . . O2SA O 0.0221(2) 0.8416(3) 0.4486(2) 0.0416(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.02463(19) 0.0409(2) 0.0337(2) -0.00305(16) 0.01077(16) -0.00127(15) Tb2 0.0303(2) 0.0419(3) 0.0344(2) -0.00258(17) 0.01215(16) -0.00057(16) Tb3 0.0262(2) 0.0392(2) 0.0346(2) -0.00182(16) 0.01103(16) -0.00006(15) Tb4 0.0262(2) 0.0466(3) 0.0401(2) -0.00731(18) 0.00889(17) -0.00193(16) C6 0.033(4) 0.043(5) 0.041(5) -0.005(4) 0.013(4) 0.009(4) C11 0.034(5) 0.056(6) 0.056(6) 0.007(5) 0.000(4) 0.004(4) C2S 0.049(6) 0.073(7) 0.060(6) 0.018(6) 0.004(5) 0.001(5) O2W 0.033(3) 0.041(3) 0.035(3) -0.006(2) 0.012(2) -0.002(2) O1W 0.026(3) 0.041(3) 0.038(3) 0.003(2) 0.011(2) 0.000(2) O1 0.026(3) 0.047(3) 0.044(3) -0.006(3) 0.009(2) 0.005(2) N3 0.033(4) 0.046(4) 0.040(4) -0.007(3) 0.009(3) 0.005(3) N2A 0.037(4) 0.053(5) 0.049(4) -0.009(4) 0.016(3) -0.013(3) N5 0.030(4) 0.063(5) 0.047(4) -0.011(4) 0.004(3) 0.007(3) N6 0.043(4) 0.063(6) 0.049(5) -0.003(4) 0.005(4) 0.000(4) O1A 0.036(3) 0.048(4) 0.036(3) -0.001(3) 0.021(3) -0.009(3) C7A 0.039(5) 0.049(6) 0.056(6) -0.001(4) 0.023(4) -0.013(4) O2S 0.049(3) 0.033(3) 0.047(4) 0.001(3) 0.024(3) -0.001(3) O1S 0.030(3) 0.058(4) 0.039(3) 0.004(3) 0.007(3) 0.004(3) C2SA 0.042(5) 0.045(6) 0.068(7) -0.016(5) 0.017(5) -0.005(4) N4A 0.038(4) 0.049(5) 0.046(4) 0.001(3) 0.021(3) -0.007(3) C11A 0.047(5) 0.055(6) 0.043(5) -0.003(4) 0.009(4) 0.000(5) N3A 0.037(4) 0.059(5) 0.033(4) -0.005(3) 0.013(3) -0.017(3) C1A 0.053(6) 0.052(6) 0.078(8) -0.004(5) -0.003(5) -0.017(5) C5 0.038(5) 0.049(5) 0.045(5) -0.014(4) 0.007(4) 0.009(4) C10A 0.043(5) 0.057(6) 0.048(5) 0.007(4) 0.027(4) 0.000(4) N5A 0.030(3) 0.055(5) 0.037(4) 0.003(3) 0.015(3) 0.003(3) N4 0.032(4) 0.065(5) 0.055(5) -0.006(4) 0.011(3) 0.006(4) Cl2 0.0528(14) 0.0570(16) 0.0753(17) -0.0225(13) 0.0265(13) -0.0066(11) N1S 0.037(4) 0.051(5) 0.058(5) 0.007(4) 0.011(4) 0.003(3) N1 0.043(4) 0.054(5) 0.045(4) -0.009(4) 0.019(4) 0.003(4) C7 0.036(4) 0.045(5) 0.048(5) -0.004(4) 0.005(4) 0.013(4) C1S 0.033(5) 0.078(8) 0.075(7) 0.018(6) -0.004(5) 0.004(5) N2 0.036(4) 0.047(4) 0.045(4) -0.007(3) 0.012(3) 0.007(3) C8A 0.039(4) 0.042(5) 0.043(5) 0.000(4) 0.022(4) 0.001(4) C3SA 0.043(5) 0.072(7) 0.047(5) -0.027(5) 0.015(4) -0.015(5) C9A 0.033(4) 0.042(5) 0.042(5) -0.002(4) 0.012(4) -0.004(4) C6A 0.045(5) 0.042(5) 0.051(5) 0.004(4) 0.014(4) -0.010(4) C15 0.051(6) 0.093(9) 0.057(7) -0.011(6) 0.005(5) -0.008(6) C10 0.035(5) 0.064(7) 0.062(7) -0.008(5) 0.000(5) -0.003(4) C4S 0.075(7) 0.039(6) 0.053(6) -0.005(4) 0.021(6) -0.001(5) N1SA 0.041(4) 0.045(4) 0.043(4) -0.009(3) 0.016(3) -0.009(3) C9 0.031(4) 0.040(5) 0.044(5) 0.003(4) 0.007(4) 0.012(4) N6A 0.040(4) 0.061(5) 0.049(5) -0.001(4) 0.015(4) 0.004(4) C12 0.041(6) 0.085(9) 0.072(8) -0.002(7) -0.013(5) 0.007(6) C5A 0.040(5) 0.055(6) 0.059(6) 0.003(5) 0.010(4) -0.014(4) C8 0.034(4) 0.044(5) 0.041(5) 0.002(4) 0.014(4) 0.012(4) C13 0.069(8) 0.077(9) 0.068(8) -0.017(6) -0.029(6) 0.013(6) N1A 0.040(4) 0.039(4) 0.059(5) -0.012(4) 0.006(4) -0.003(3) C15A 0.066(7) 0.095(9) 0.049(6) -0.006(6) 0.006(5) -0.018(7) C4A 0.052(6) 0.083(8) 0.070(7) 0.012(6) 0.013(5) -0.032(6) C2A 0.044(6) 0.067(8) 0.103(10) -0.014(7) -0.010(6) -0.022(5) C3A 0.071(8) 0.119(12) 0.091(10) 0.029(9) -0.005(7) -0.061(8) C14A 0.119(13) 0.129(13) 0.047(7) -0.017(8) -0.002(8) -0.039(11) C12A 0.094(9) 0.080(8) 0.042(6) -0.002(6) 0.002(6) -0.020(7) C13A 0.131(13) 0.119(12) 0.041(7) 0.004(7) 0.008(8) -0.022(10) C3S 0.057(6) 0.054(7) 0.088(8) 0.003(6) 0.029(6) 0.023(5) C1 0.062(6) 0.072(7) 0.046(6) -0.015(5) 0.007(5) 0.023(6) Cl1 0.0525(14) 0.0541(16) 0.0713(17) -0.0114(12) 0.0129(13) -0.0099(11) C14 0.089(9) 0.073(8) 0.058(7) -0.008(6) -0.011(7) -0.005(7) C2 0.069(8) 0.092(9) 0.053(6) -0.021(6) 0.014(6) 0.031(6) C3 0.066(7) 0.096(10) 0.068(8) -0.012(7) 0.028(6) 0.035(7) C4 0.037(5) 0.079(8) 0.065(7) -0.013(6) 0.021(5) 0.017(5) C4SA 0.058(6) 0.061(6) 0.043(5) -0.014(5) 0.018(5) -0.021(5) C1SA 0.038(5) 0.033(5) 0.065(6) 0.008(4) 0.012(4) 0.001(4) O1SA 0.030(3) 0.037(3) 0.048(3) -0.002(3) 0.017(3) -0.001(2) O2SA 0.032(3) 0.058(4) 0.035(3) -0.011(3) 0.007(2) -0.004(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 O1SA 2.251(5) 2 ? Tb1 O2S 2.267(6) . ? Tb1 O2W 2.372(5) . ? Tb1 O1W 2.398(6) . ? Tb1 N3A 2.411(7) . ? Tb1 N3 2.445(7) . ? Tb1 O1A 2.467(5) . ? Tb1 O1 2.501(5) . ? Tb1 Tb3 3.7348(6) 2 ? Tb1 Tb3 3.7585(6) . ? Tb1 Tb4 3.8583(6) . ? Tb1 Tb2 3.8688(6) . ? Tb2 O2SA 2.288(6) 2 ? Tb2 O1A 2.352(6) . ? Tb2 O1W 2.359(5) . ? Tb2 N2 2.465(7) . ? Tb2 N5A 2.515(7) . ? Tb2 N6A 2.588(8) . ? Tb2 Cl1 2.685(3) . ? Tb2 N1 2.777(7) . ? Tb2 Tb3 3.8433(5) 2 ? Tb3 O1SA 2.321(6) . ? Tb3 O2S 2.328(6) . ? Tb3 O1S 2.360(6) . ? Tb3 O2SA 2.372(6) . ? Tb3 O1W 2.419(5) 2 ? Tb3 O2W 2.425(5) . ? Tb3 N1S 2.531(8) . ? Tb3 N1SA 2.536(7) . ? Tb3 Tb1 3.7348(6) 2 ? Tb3 Tb4 3.8251(5) . ? Tb3 Tb2 3.8433(5) 2 ? Tb4 O1S 2.292(6) . ? Tb4 O2W 2.336(6) . ? Tb4 O1 2.361(6) . ? Tb4 N2A 2.418(8) . ? Tb4 N5 2.508(7) . ? Tb4 N6 2.568(8) . ? Tb4 Cl2 2.645(3) . ? Tb4 N1A 2.769(8) . ? C6 N2 1.353(10) . ? C6 C7 1.374(12) . ? C6 C5 1.474(12) . ? C11 N6 1.356(12) . ? C11 C12 1.390(13) . ? C11 C10 1.409(14) . ? C2S N1S 1.484(13) . ? C2S C1S 1.517(15) . ? C2S H2SA 0.9700 . ? C2S H2SB 0.9700 . ? O1W Tb3 2.419(5) 2 ? O1 C9 1.263(9) . ? N3 C8 1.349(11) . ? N3 N2 1.362(10) . ? N2A C6A 1.350(11) . ? N2A N3A 1.354(10) . ? N5 C10 1.305(12) . ? N5 N4 1.375(11) . ? N6 C15 1.330(13) . ? O1A C9A 1.280(9) . ? C7A C6A 1.357(13) . ? C7A C8A 1.394(12) . ? C7A H7AA 0.9300 . ? O2S C4S 1.407(11) . ? O1S C1S 1.371(12) . ? C2SA N1SA 1.439(12) . ? C2SA C1SA 1.532(14) . ? C2SA H2SC 0.9700 . ? C2SA H2SD 0.9700 . ? N4A C9A 1.297(11) . ? N4A N5A 1.410(10) . ? C11A C12A 1.355(14) . ? C11A N6A 1.386(12) . ? C11A C10A 1.395(14) . ? N3A C8A 1.346(10) . ? C1A C2A 1.363(16) . ? C1A N1A 1.364(12) . ? C1A H1AA 0.9300 . ? C5 N1 1.348(11) . ? C5 C4 1.385(12) . ? C10A N5A 1.269(11) . ? C10A H10A 0.9300 . ? N4 C9 1.327(11) . ? N1S C3S 1.450(13) . ? N1S H1SE 0.9100 . ? N1 C1 1.301(12) . ? C7 C8 1.394(11) . ? C7 H7A 0.9300 . ? C1S H1SA 0.9700 . ? C1S H1SB 0.9700 . ? C8A C9A 1.489(12) . ? C3SA N1SA 1.501(12) . ? C3SA C4SA 1.520(13) . ? C3SA H3SA 0.9700 . ? C3SA H3SB 0.9700 . ? C6A C5A 1.467(13) . ? C15 C14 1.387(16) . ? C15 H15A 0.9300 . ? C10 H10B 0.9300 . ? C4S C3S 1.530(15) . ? C4S H4SA 0.9700 . ? C4S H4SB 0.9700 . ? N1SA H1SI 0.9100 . ? C9 C8 1.486(12) . ? N6A C15A 1.313(13) . ? C12 C13 1.358(16) . ? C12 H12A 0.9300 . ? C5A N1A 1.331(13) . ? C5A C4A 1.385(13) . ? C13 C14 1.318(17) . ? C13 H13A 0.9300 . ? C15A C14A 1.378(17) . ? C15A H15B 0.9300 . ? C4A C3A 1.339(17) . ? C4A H4AB 0.9300 . ? C2A C3A 1.362(18) . ? C2A H2AA 0.9300 . ? C3A H3AA 0.9300 . ? C14A C13A 1.35(2) . ? C14A H14A 0.9300 . ? C12A C13A 1.393(18) . ? C12A H12B 0.9300 . ? C13A H13B 0.9300 . ? C3S H3SC 0.9700 . ? C3S H3SD 0.9700 . ? C1 C2 1.408(14) . ? C1 H1A 0.9300 . ? C14 H14B 0.9300 . ? C2 C3 1.326(16) . ? C2 H2A 0.9300 . ? C3 C4 1.362(15) . ? C3 H3A 0.9300 . ? C4 H4B 0.9300 . ? C4SA O2SA 1.421(10) . ? C4SA H4SC 0.9700 . ? C4SA H4SD 0.9700 . ? C1SA O1SA 1.407(10) . ? C1SA H1SC 0.9700 . ? C1SA H1SD 0.9700 . ? O1SA Tb1 2.251(5) 2 ? O2SA Tb2 2.288(6) 2 ? 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 O1SA Tb1 O2S 106.2(2) 2 . ? O1SA Tb1 O2W 86.4(2) 2 . ? O2S Tb1 O2W 73.5(2) . . ? O1SA Tb1 O1W 73.9(2) 2 . ? O2S Tb1 O1W 87.2(2) . . ? O2W Tb1 O1W 147.51(18) . . ? O1SA Tb1 N3A 94.4(2) 2 . ? O2S Tb1 N3A 141.5(2) . . ? O2W Tb1 N3A 75.8(2) . . ? O1W Tb1 N3A 130.3(2) . . ? O1SA Tb1 N3 142.1(2) 2 . ? O2S Tb1 N3 94.3(2) . . ? O2W Tb1 N3 130.5(2) . . ? O1W Tb1 N3 75.7(2) . . ? N3A Tb1 N3 88.3(3) . . ? O1SA Tb1 O1A 77.08(19) 2 . ? O2S Tb1 O1A 153.4(2) . . ? O2W Tb1 O1A 132.97(19) . . ? O1W Tb1 O1A 68.04(18) . . ? N3A Tb1 O1A 62.3(2) . . ? N3 Tb1 O1A 70.8(2) . . ? O1SA Tb1 O1 151.9(2) 2 . ? O2S Tb1 O1 77.6(2) . . ? O2W Tb1 O1 67.68(19) . . ? O1W Tb1 O1 134.07(19) . . ? N3A Tb1 O1 69.6(2) . . ? N3 Tb1 O1 62.9(2) . . ? O1A Tb1 O1 112.29(18) . . ? O1SA Tb1 Tb3 35.86(15) 2 2 ? O2S Tb1 Tb3 91.47(16) . 2 ? O2W Tb1 Tb3 113.76(13) . 2 ? O1W Tb1 Tb3 39.38(13) . 2 ? N3A Tb1 Tb3 122.22(18) . 2 ? N3 Tb1 Tb3 114.36(17) . 2 ? O1A Tb1 Tb3 75.79(13) . 2 ? O1 Tb1 Tb3 168.19(14) . 2 ? O1SA Tb1 Tb3 91.84(14) 2 . ? O2S Tb1 Tb3 35.65(15) . . ? O2W Tb1 Tb3 38.92(13) . . ? O1W Tb1 Tb3 114.76(12) . . ? N3A Tb1 Tb3 113.74(16) . . ? N3 Tb1 Tb3 121.55(17) . . ? O1A Tb1 Tb3 167.52(14) . . ? O1 Tb1 Tb3 75.08(13) . . ? Tb3 Tb1 Tb3 98.643(12) 2 . ? O1SA Tb1 Tb4 115.77(15) 2 . ? O2S Tb1 Tb4 83.70(16) . . ? O2W Tb1 Tb4 34.67(13) . . ? O1W Tb1 Tb4 168.26(13) . . ? N3A Tb1 Tb4 57.94(16) . . ? N3 Tb1 Tb4 97.61(17) . . ? O1A Tb1 Tb4 119.33(13) . . ? O1 Tb1 Tb4 36.22(13) . . ? Tb3 Tb1 Tb4 147.965(13) 2 . ? Tb3 Tb1 Tb4 60.273(10) . . ? O1SA Tb1 Tb2 82.96(15) 2 . ? O2S Tb1 Tb2 117.80(15) . . ? O2W Tb1 Tb2 166.31(14) . . ? O1W Tb1 Tb2 35.26(12) . . ? N3A Tb1 Tb2 96.39(16) . . ? N3 Tb1 Tb2 59.17(17) . . ? O1A Tb1 Tb2 35.60(13) . . ? O1 Tb1 Tb2 120.58(13) . . ? Tb3 Tb1 Tb2 60.693(10) 2 . ? Tb3 Tb1 Tb2 149.761(13) . . ? Tb4 Tb1 Tb2 147.603(13) . . ? O2SA Tb2 O1A 84.8(2) 2 . ? O2SA Tb2 O1W 72.14(19) 2 . ? O1A Tb2 O1W 70.61(18) . . ? O2SA Tb2 N2 145.6(2) 2 . ? O1A Tb2 N2 71.7(2) . . ? O1W Tb2 N2 76.4(2) . . ? O2SA Tb2 N5A 95.3(2) 2 . ? O1A Tb2 N5A 61.4(2) . . ? O1W Tb2 N5A 131.3(2) . . ? N2 Tb2 N5A 95.0(2) . . ? O2SA Tb2 N6A 80.3(2) 2 . ? O1A Tb2 N6A 120.1(2) . . ? O1W Tb2 N6A 149.5(2) . . ? N2 Tb2 N6A 133.2(2) . . ? N5A Tb2 N6A 62.8(2) . . ? O2SA Tb2 Cl1 96.02(16) 2 . ? O1A Tb2 Cl1 154.00(14) . . ? O1W Tb2 Cl1 84.87(15) . . ? N2 Tb2 Cl1 94.70(19) . . ? N5A Tb2 Cl1 143.80(18) . . ? N6A Tb2 Cl1 85.46(19) . . ? O2SA Tb2 N1 152.9(2) 2 . ? O1A Tb2 N1 109.3(2) . . ? O1W Tb2 N1 133.8(2) . . ? N2 Tb2 N1 61.2(2) . . ? N5A Tb2 N1 73.2(2) . . ? N6A Tb2 N1 72.6(2) . . ? Cl1 Tb2 N1 81.29(17) . . ? O2SA Tb2 Tb3 35.15(14) 2 2 ? O1A Tb2 Tb3 74.64(12) . 2 ? O1W Tb2 Tb3 37.00(13) . 2 ? N2 Tb2 Tb3 112.22(16) . 2 ? N5A Tb2 Tb3 116.90(16) . 2 ? N6A Tb2 Tb3 114.59(16) . 2 ? Cl1 Tb2 Tb3 91.14(6) . 2 ? N1 Tb2 Tb3 169.25(16) . 2 ? O2SA Tb2 Tb1 86.64(15) 2 . ? O1A Tb2 Tb1 37.63(13) . . ? O1W Tb2 Tb1 35.93(13) . . ? N2 Tb2 Tb1 59.42(16) . . ? N5A Tb2 Tb1 98.51(17) . . ? N6A Tb2 Tb1 155.73(18) . . ? Cl1 Tb2 Tb1 116.37(6) . . ? N1 Tb2 Tb1 118.87(16) . . ? Tb3 Tb2 Tb1 57.930(10) 2 . ? O1SA Tb3 O2S 93.7(2) . . ? O1SA Tb3 O1S 138.9(2) . . ? O2S Tb3 O1S 97.3(2) . . ? O1SA Tb3 O2SA 95.5(2) . . ? O2S Tb3 O2SA 139.3(2) . . ? O1S Tb3 O2SA 101.3(2) . . ? O1SA Tb3 O1W 72.31(19) . 2 ? O2S Tb3 O1W 75.73(19) . 2 ? O1S Tb3 O1W 148.8(2) . 2 ? O2SA Tb3 O1W 69.66(19) . 2 ? O1SA Tb3 O2W 76.44(19) . . ? O2S Tb3 O2W 71.50(19) . . ? O1S Tb3 O2W 69.9(2) . . ? O2SA Tb3 O2W 149.08(19) . . ? O1W Tb3 O2W 132.48(19) 2 . ? O1SA Tb3 N1S 151.6(2) . . ? O2S Tb3 N1S 71.0(2) . . ? O1S Tb3 N1S 68.5(2) . . ? O2SA Tb3 N1S 82.7(2) . . ? O1W Tb3 N1S 80.6(2) 2 . ? O2W Tb3 N1S 118.4(2) . . ? O1SA Tb3 N1SA 69.4(2) . . ? O2S Tb3 N1SA 150.5(2) . . ? O1S Tb3 N1SA 82.3(2) . . ? O2SA Tb3 N1SA 68.5(2) . . ? O1W Tb3 N1SA 118.7(2) 2 . ? O2W Tb3 N1SA 80.8(2) . . ? N1S Tb3 N1SA 133.8(3) . . ? O1SA Tb3 Tb1 34.62(14) . 2 ? O2S Tb3 Tb1 77.05(15) . 2 ? O1S Tb3 Tb1 169.35(14) . 2 ? O2SA Tb3 Tb1 88.68(14) . 2 ? O1W Tb3 Tb1 38.97(13) 2 2 ? O2W Tb3 Tb1 99.63(13) . 2 ? N1S Tb3 Tb1 117.03(18) . 2 ? N1SA Tb3 Tb1 98.17(17) . 2 ? O1SA Tb3 Tb1 78.21(13) . . ? O2S Tb3 Tb1 34.58(14) . . ? O1S Tb3 Tb1 88.88(14) . . ? O2SA Tb3 Tb1 169.46(14) . . ? O1W Tb3 Tb1 100.19(13) 2 . ? O2W Tb3 Tb1 37.92(13) . . ? N1S Tb3 Tb1 98.77(18) . . ? N1SA Tb3 Tb1 116.14(16) . . ? Tb1 Tb3 Tb1 81.353(12) 2 . ? O1SA Tb3 Tb4 109.15(13) . . ? O2S Tb3 Tb4 83.73(14) . . ? O1S Tb3 Tb4 34.12(14) . . ? O2SA Tb3 Tb4 129.32(14) . . ? O1W Tb3 Tb4 159.46(12) 2 . ? O2W Tb3 Tb4 35.76(13) . . ? N1S Tb3 Tb4 93.26(17) . . ? N1SA Tb3 Tb4 79.59(16) . . ? Tb1 Tb3 Tb4 135.368(14) 2 . ? Tb1 Tb3 Tb4 61.156(10) . . ? O1SA Tb3 Tb2 82.72(13) . 2 ? O2S Tb3 Tb2 109.35(14) . 2 ? O1S Tb3 Tb2 129.27(14) . 2 ? O2SA Tb3 Tb2 33.73(14) . 2 ? O1W Tb3 Tb2 35.93(13) 2 2 ? O2W Tb3 Tb2 159.14(13) . 2 ? N1S Tb3 Tb2 80.25(17) . 2 ? N1SA Tb3 Tb2 92.88(16) . 2 ? Tb1 Tb3 Tb2 61.377(10) 2 2 ? Tb1 Tb3 Tb2 136.022(14) . 2 ? Tb4 Tb3 Tb2 162.168(14) . 2 ? O1S Tb4 O2W 72.6(2) . . ? O1S Tb4 O1 84.6(2) . . ? O2W Tb4 O1 70.65(18) . . ? O1S Tb4 N2A 146.8(2) . . ? O2W Tb4 N2A 77.5(2) . . ? O1 Tb4 N2A 72.0(2) . . ? O1S Tb4 N5 99.4(2) . . ? O2W Tb4 N5 131.3(2) . . ? O1 Tb4 N5 60.8(2) . . ? N2A Tb4 N5 89.5(3) . . ? O1S Tb4 N6 81.4(2) . . ? O2W Tb4 N6 151.5(2) . . ? O1 Tb4 N6 118.9(2) . . ? N2A Tb4 N6 130.4(3) . . ? N5 Tb4 N6 63.6(3) . . ? O1S Tb4 Cl2 96.85(16) . . ? O2W Tb4 Cl2 84.14(15) . . ? O1 Tb4 Cl2 153.13(15) . . ? N2A Tb4 Cl2 94.1(2) . . ? N5 Tb4 Cl2 144.06(19) . . ? N6 Tb4 Cl2 87.7(2) . . ? O1S Tb4 N1A 152.9(2) . . ? O2W Tb4 N1A 131.8(2) . . ? O1 Tb4 N1A 112.6(2) . . ? N2A Tb4 N1A 60.3(2) . . ? N5 Tb4 N1A 73.6(2) . . ? N6 Tb4 N1A 72.0(3) . . ? Cl2 Tb4 N1A 77.30(16) . . ? O1S Tb4 Tb3 35.28(14) . . ? O2W Tb4 Tb3 37.34(13) . . ? O1 Tb4 Tb3 75.03(13) . . ? N2A Tb4 Tb3 113.68(17) . . ? N5 Tb4 Tb3 120.33(19) . . ? N6 Tb4 Tb3 115.87(18) . . ? Cl2 Tb4 Tb3 90.70(5) . . ? N1A Tb4 Tb3 165.64(16) . . ? O1S Tb4 Tb1 87.44(15) . . ? O2W Tb4 Tb1 35.28(13) . . ? O1 Tb4 Tb1 38.76(13) . . ? N2A Tb4 Tb1 59.57(17) . . ? N5 Tb4 Tb1 98.21(17) . . ? N6 Tb4 Tb1 156.37(19) . . ? Cl2 Tb4 Tb1 114.39(6) . . ? N1A Tb4 Tb1 119.24(17) . . ? Tb3 Tb4 Tb1 58.571(10) . . ? N2 C6 C7 111.0(7) . . ? N2 C6 C5 116.0(8) . . ? C7 C6 C5 132.9(8) . . ? N6 C11 C12 118.1(10) . . ? N6 C11 C10 119.1(9) . . ? C12 C11 C10 122.7(10) . . ? N1S C2S C1S 110.2(8) . . ? N1S C2S H2SA 109.6 . . ? C1S C2S H2SA 109.6 . . ? N1S C2S H2SB 109.6 . . ? C1S C2S H2SB 109.6 . . ? H2SA C2S H2SB 108.1 . . ? Tb4 O2W Tb1 110.1(2) . . ? Tb4 O2W Tb3 106.9(2) . . ? Tb1 O2W Tb3 103.2(2) . . ? Tb2 O1W Tb1 108.8(2) . . ? Tb2 O1W Tb3 107.1(2) . 2 ? Tb1 O1W Tb3 101.6(2) . 2 ? C9 O1 Tb4 120.2(5) . . ? C9 O1 Tb1 120.2(5) . . ? Tb4 O1 Tb1 105.0(2) . . ? C8 N3 N2 108.7(6) . . ? C8 N3 Tb1 119.8(5) . . ? N2 N3 Tb1 121.8(5) . . ? C6A N2A N3A 107.9(7) . . ? C6A N2A Tb4 126.8(6) . . ? N3A N2A Tb4 118.7(5) . . ? C10 N5 N4 118.6(8) . . ? C10 N5 Tb4 121.9(7) . . ? N4 N5 Tb4 119.4(5) . . ? C15 N6 C11 119.5(9) . . ? C15 N6 Tb4 123.3(7) . . ? C11 N6 Tb4 116.8(6) . . ? C9A O1A Tb2 119.9(5) . . ? C9A O1A Tb1 124.2(5) . . ? Tb2 O1A Tb1 106.8(2) . . ? C6A C7A C8A 104.5(7) . . ? C6A C7A H7AA 127.7 . . ? C8A C7A H7AA 127.7 . . ? C4S O2S Tb1 127.5(5) . . ? C4S O2S Tb3 116.2(5) . . ? Tb1 O2S Tb3 109.8(2) . . ? C1S O1S Tb4 121.0(6) . . ? C1S O1S Tb3 120.1(6) . . ? Tb4 O1S Tb3 110.6(2) . . ? N1SA C2SA C1SA 109.2(7) . . ? N1SA C2SA H2SC 109.8 . . ? C1SA C2SA H2SC 109.8 . . ? N1SA C2SA H2SD 109.8 . . ? C1SA C2SA H2SD 109.8 . . ? H2SC C2SA H2SD 108.3 . . ? C9A N4A N5A 107.0(7) . . ? C12A C11A N6A 121.3(10) . . ? C12A C11A C10A 122.4(10) . . ? N6A C11A C10A 116.3(8) . . ? C8A N3A N2A 107.6(7) . . ? C8A N3A Tb1 123.4(6) . . ? N2A N3A Tb1 123.8(5) . . ? C2A C1A N1A 121.9(12) . . ? C2A C1A H1AA 119.1 . . ? N1A C1A H1AA 119.1 . . ? N1 C5 C4 122.1(9) . . ? N1 C5 C6 116.1(7) . . ? C4 C5 C6 121.8(9) . . ? N5A C10A C11A 120.7(9) . . ? N5A C10A H10A 119.6 . . ? C11A C10A H10A 119.6 . . ? C10A N5A N4A 118.9(7) . . ? C10A N5A Tb2 122.1(6) . . ? N4A N5A Tb2 118.9(5) . . ? C9 N4 N5 107.7(7) . . ? C3S N1S C2S 115.2(8) . . ? C3S N1S Tb3 109.5(6) . . ? C2S N1S Tb3 105.5(6) . . ? C3S N1S H1SE 108.8 . . ? C2S N1S H1SE 108.8 . . ? Tb3 N1S H1SE 108.8 . . ? C1 N1 C5 117.8(8) . . ? C1 N1 Tb2 126.5(7) . . ? C5 N1 Tb2 115.7(5) . . ? C6 C7 C8 104.2(7) . . ? C6 C7 H7A 127.9 . . ? C8 C7 H7A 127.9 . . ? O1S C1S C2S 114.4(8) . . ? O1S C1S H1SA 108.7 . . ? C2S C1S H1SA 108.7 . . ? O1S C1S H1SB 108.7 . . ? C2S C1S H1SB 108.7 . . ? H1SA C1S H1SB 107.6 . . ? C6 N2 N3 106.7(7) . . ? C6 N2 Tb2 124.1(6) . . ? N3 N2 Tb2 119.6(5) . . ? N3A C8A C7A 109.6(8) . . ? N3A C8A C9A 112.7(7) . . ? C7A C8A C9A 137.1(8) . . ? N1SA C3SA C4SA 110.0(7) . . ? N1SA C3SA H3SA 109.7 . . ? C4SA C3SA H3SA 109.7 . . ? N1SA C3SA H3SB 109.7 . . ? C4SA C3SA H3SB 109.7 . . ? H3SA C3SA H3SB 108.2 . . ? O1A C9A N4A 126.3(8) . . ? O1A C9A C8A 113.5(7) . . ? N4A C9A C8A 120.2(7) . . ? N2A C6A C7A 110.4(8) . . ? N2A C6A C5A 114.8(8) . . ? C7A C6A C5A 134.7(8) . . ? N6 C15 C14 121.5(12) . . ? N6 C15 H15A 119.3 . . ? C14 C15 H15A 119.3 . . ? N5 C10 C11 117.6(9) . . ? N5 C10 H10B 121.2 . . ? C11 C10 H10B 121.2 . . ? O2S C4S C3S 113.2(8) . . ? O2S C4S H4SA 108.9 . . ? C3S C4S H4SA 108.9 . . ? O2S C4S H4SB 108.9 . . ? C3S C4S H4SB 108.9 . . ? H4SA C4S H4SB 107.8 . . ? C2SA N1SA C3SA 116.1(7) . . ? C2SA N1SA Tb3 110.3(5) . . ? C3SA N1SA Tb3 104.5(6) . . ? C2SA N1SA H1SI 108.5 . . ? C3SA N1SA H1SI 108.5 . . ? Tb3 N1SA H1SI 108.5 . . ? O1 C9 N4 124.0(8) . . ? O1 C9 C8 116.0(7) . . ? N4 C9 C8 120.0(7) . . ? C15A N6A C11A 117.2(9) . . ? C15A N6A Tb2 125.3(7) . . ? C11A N6A Tb2 117.3(6) . . ? C13 C12 C11 122.0(11) . . ? C13 C12 H12A 119.0 . . ? C11 C12 H12A 119.0 . . ? N1A C5A C4A 121.3(9) . . ? N1A C5A C6A 115.6(8) . . ? C4A C5A C6A 123.1(10) . . ? N3 C8 C7 109.3(8) . . ? N3 C8 C9 113.5(7) . . ? C7 C8 C9 136.5(8) . . ? C14 C13 C12 118.4(11) . . ? C14 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? C5A N1A C1A 117.7(9) . . ? C5A N1A Tb4 116.3(6) . . ? C1A N1A Tb4 126.0(7) . . ? N6A C15A C14A 124.7(12) . . ? N6A C15A H15B 117.6 . . ? C14A C15A H15B 117.6 . . ? C3A C4A C5A 120.3(12) . . ? C3A C4A H4AB 119.9 . . ? C5A C4A H4AB 119.9 . . ? C3A C2A C1A 119.5(11) . . ? C3A C2A H2AA 120.3 . . ? C1A C2A H2AA 120.3 . . ? C4A C3A C2A 119.2(11) . . ? C4A C3A H3AA 120.4 . . ? C2A C3A H3AA 120.4 . . ? C13A C14A C15A 117.1(13) . . ? C13A C14A H14A 121.4 . . ? C15A C14A H14A 121.4 . . ? C11A C12A C13A 118.9(12) . . ? C11A C12A H12B 120.6 . . ? C13A C12A H12B 120.6 . . ? C14A C13A C12A 120.4(12) . . ? C14A C13A H13B 119.8 . . ? C12A C13A H13B 119.8 . . ? N1S C3S C4S 109.7(8) . . ? N1S C3S H3SC 109.7 . . ? C4S C3S H3SC 109.7 . . ? N1S C3S H3SD 109.7 . . ? C4S C3S H3SD 109.7 . . ? H3SC C3S H3SD 108.2 . . ? N1 C1 C2 122.9(10) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C13 C14 C15 120.5(12) . . ? C13 C14 H14B 119.8 . . ? C15 C14 H14B 119.8 . . ? C3 C2 C1 118.2(10) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C2 C3 C4 120.9(10) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C3 C4 C5 118.0(10) . . ? C3 C4 H4B 121.0 . . ? C5 C4 H4B 121.0 . . ? O2SA C4SA C3SA 112.3(7) . . ? O2SA C4SA H4SC 109.1 . . ? C3SA C4SA H4SC 109.1 . . ? O2SA C4SA H4SD 109.1 . . ? C3SA C4SA H4SD 109.1 . . ? H4SC C4SA H4SD 107.9 . . ? O1SA C1SA C2SA 110.2(7) . . ? O1SA C1SA H1SC 109.6 . . ? C2SA C1SA H1SC 109.6 . . ? O1SA C1SA H1SD 109.6 . . ? C2SA C1SA H1SD 109.6 . . ? H1SC C1SA H1SD 108.1 . . ? C1SA O1SA Tb1 128.0(5) . 2 ? C1SA O1SA Tb3 118.2(5) . . ? Tb1 O1SA Tb3 109.5(2) 2 . ? C4SA O2SA Tb2 121.2(5) . 2 ? C4SA O2SA Tb3 119.9(5) . . ? Tb2 O2SA Tb3 111.1(2) 2 . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 3.573 _refine_diff_density_min -1.363 _refine_diff_density_rms 0.236