# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p12032b-sr _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H51 N6 O3 Sc' _chemical_formula_weight 588.73 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' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.3553(3) _cell_length_b 10.4491(2) _cell_length_c 39.2700(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.841(2) _cell_angle_gamma 90.00 _cell_volume 7900.9(2) _cell_formula_units_Z 8 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 10590 _cell_measurement_theta_min 3.1114 _cell_measurement_theta_max 24.6591 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.990 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.218 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82703 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68199 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 24.71 _reflns_number_total 13441 _reflns_number_gt 10794 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ortep _computing_publication_material mercury _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+5.0193P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13441 _refine_ls_number_parameters 745 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0842 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1684 _refine_ls_wR_factor_gt 0.1575 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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 C1 C 0.7579(3) -0.2343(4) 0.11508(12) 0.0718(13) Uani 1 1 d . . . H1A H 0.7206 -0.2545 0.1293 0.108 Uiso 1 1 calc R . . H1B H 0.7892 -0.3079 0.1147 0.108 Uiso 1 1 calc R . . H1C H 0.7379 -0.2149 0.0917 0.108 Uiso 1 1 calc R . . C2 C 0.8387(2) -0.1513(4) 0.16384(12) 0.0687(13) Uani 1 1 d . . . H2A H 0.8633 -0.0749 0.1730 0.103 Uiso 1 1 calc R . . H2B H 0.8723 -0.2191 0.1605 0.103 Uiso 1 1 calc R . . H2C H 0.8066 -0.1807 0.1800 0.103 Uiso 1 1 calc R . . C3 C 0.79820(19) -0.1194(4) 0.12983(9) 0.0457(9) Uani 1 1 d . . . H3 H 0.8323 -0.0947 0.1135 0.055 Uiso 1 1 calc R . . C4 C 0.70397(19) -0.0002(4) 0.15710(9) 0.0494(10) Uani 1 1 d . . . H4 H 0.6949 -0.0624 0.1737 0.059 Uiso 1 1 calc R . . C5 C 0.67312(19) 0.1144(4) 0.15226(8) 0.0487(10) Uani 1 1 d . . . H5 H 0.6379 0.1488 0.1648 0.058 Uiso 1 1 calc R . . C6 C 0.75177(15) 0.0977(3) 0.11336(7) 0.0302(7) Uani 1 1 d . . . C7 C 0.68621(17) 0.3025(3) 0.11339(8) 0.0381(8) Uani 1 1 d . . . H7A H 0.7272 0.3578 0.1194 0.046 Uiso 1 1 calc R . . H7B H 0.6475 0.3364 0.1254 0.046 Uiso 1 1 calc R . . C8 C 0.66591(16) 0.3106(3) 0.07464(8) 0.0354(7) Uani 1 1 d . . . C9 C 0.60014(16) 0.2310(4) 0.06475(9) 0.0434(9) Uani 1 1 d . . . H9A H 0.5885 0.2342 0.0399 0.065 Uiso 1 1 calc R . . H9B H 0.5615 0.2660 0.0761 0.065 Uiso 1 1 calc R . . H9C H 0.6085 0.1420 0.0719 0.065 Uiso 1 1 calc R . . C10 C 0.6510(2) 0.4525(4) 0.06658(10) 0.0502(9) Uani 1 1 d . . . H10A H 0.6929 0.5031 0.0731 0.075 Uiso 1 1 calc R . . H10B H 0.6133 0.4823 0.0795 0.075 Uiso 1 1 calc R . . H10C H 0.6373 0.4627 0.0420 0.075 Uiso 1 1 calc R . . C11 C 0.6309(3) -0.1217(6) 0.03521(13) 0.0895(17) Uani 1 1 d . . . H11A H 0.6325 -0.2074 0.0252 0.134 Uiso 1 1 calc R . . H11B H 0.5826 -0.0981 0.0374 0.134 Uiso 1 1 calc R . . H11C H 0.6572 -0.1213 0.0579 0.134 Uiso 1 1 calc R . . C12 C 0.6203(2) -0.0180(5) -0.02228(12) 0.0735(14) Uani 1 1 d . . . H12A H 0.6445 0.0371 -0.0374 0.110 Uiso 1 1 calc R . . H12B H 0.5745 0.0181 -0.0195 0.110 Uiso 1 1 calc R . . H12C H 0.6148 -0.1038 -0.0323 0.110 Uiso 1 1 calc R . . C13 C 0.66253(18) -0.0265(4) 0.01237(10) 0.0546(11) Uani 1 1 d . . . H13 H 0.6617 0.0595 0.0235 0.066 Uiso 1 1 calc R . . C14 C 0.7581(2) -0.1594(5) -0.01006(12) 0.0722(14) Uani 1 1 d . . . H14 H 0.7298 -0.2209 -0.0227 0.087 Uiso 1 1 calc R . . C15 C 0.8276(2) -0.1532(4) -0.00723(11) 0.0630(12) Uani 1 1 d . . . H15 H 0.8582 -0.2093 -0.0174 0.076 Uiso 1 1 calc R . . C16 C 0.78953(15) 0.0103(3) 0.02373(7) 0.0304(7) Uani 1 1 d . . . C17 C 0.91687(16) -0.0081(3) 0.02365(8) 0.0336(7) Uani 1 1 d . . . H17A H 0.9222 0.0822 0.0168 0.040 Uiso 1 1 calc R . . H17B H 0.9494 -0.0604 0.0116 0.040 Uiso 1 1 calc R . . C18 C 0.93605(15) -0.0205(3) 0.06259(8) 0.0290(7) Uani 1 1 d . . . C19 C 0.93656(19) -0.1626(3) 0.07287(10) 0.0455(9) Uani 1 1 d . . . H19A H 0.9515 -0.1706 0.0974 0.068 Uiso 1 1 calc R . . H19B H 0.9688 -0.2096 0.0598 0.068 Uiso 1 1 calc R . . H19C H 0.8897 -0.1981 0.0680 0.068 Uiso 1 1 calc R . . C20 C 1.00940(16) 0.0351(3) 0.07032(9) 0.0402(8) Uani 1 1 d . . . H20A H 1.0091 0.1256 0.0637 0.060 Uiso 1 1 calc R . . H20B H 1.0417 -0.0120 0.0573 0.060 Uiso 1 1 calc R . . H20C H 1.0241 0.0272 0.0949 0.060 Uiso 1 1 calc R . . C21 C 0.8635(2) 0.2245(5) 0.19069(10) 0.0683(13) Uani 1 1 d . . . H21A H 0.8865 0.2910 0.2054 0.102 Uiso 1 1 calc R . . H21B H 0.8622 0.1445 0.2036 0.102 Uiso 1 1 calc R . . H21C H 0.8160 0.2516 0.1830 0.102 Uiso 1 1 calc R . . C22 C 0.9774(2) 0.1598(4) 0.16973(10) 0.0567(11) Uani 1 1 d . . . H22A H 1.0006 0.1464 0.1490 0.085 Uiso 1 1 calc R . . H22B H 0.9770 0.0794 0.1825 0.085 Uiso 1 1 calc R . . H22C H 1.0025 0.2251 0.1840 0.085 Uiso 1 1 calc R . . C23 C 0.90335(17) 0.2038(3) 0.15995(8) 0.0372(8) Uani 1 1 d . . . H23 H 0.8791 0.1345 0.1458 0.045 Uiso 1 1 calc R . . C24 C 0.93744(19) 0.4316(4) 0.14699(9) 0.0473(9) Uani 1 1 d . . . H24 H 0.9654 0.4494 0.1678 0.057 Uiso 1 1 calc R . . C25 C 0.9250(2) 0.5101(4) 0.12045(10) 0.0486(9) Uani 1 1 d . . . H25 H 0.9428 0.5942 0.1185 0.058 Uiso 1 1 calc R . . C26 C 0.86668(16) 0.3260(3) 0.10695(8) 0.0306(7) Uani 1 1 d . . . C27 C 0.86030(18) 0.4893(3) 0.06124(9) 0.0403(8) Uani 1 1 d . . . H27A H 0.8754 0.5790 0.0588 0.048 Uiso 1 1 calc R . . H27B H 0.8090 0.4871 0.0570 0.048 Uiso 1 1 calc R . . C28 C 0.97072(17) 0.4039(4) 0.04088(10) 0.0472(9) Uani 1 1 d . . . H28A H 0.9845 0.3642 0.0631 0.071 Uiso 1 1 calc R . . H28B H 0.9887 0.4916 0.0408 0.071 Uiso 1 1 calc R . . H28C H 0.9897 0.3543 0.0228 0.071 Uiso 1 1 calc R . . C29 C 0.89130(16) 0.4064(3) 0.03440(8) 0.0340(7) Uani 1 1 d . . . C30 C 0.86990(19) 0.4671(4) -0.00066(9) 0.0486(9) Uani 1 1 d . . . H30A H 0.8849 0.4120 -0.0187 0.073 Uiso 1 1 calc R . . H30B H 0.8918 0.5513 -0.0018 0.073 Uiso 1 1 calc R . . H30C H 0.8193 0.4767 -0.0039 0.073 Uiso 1 1 calc R . . C31 C 0.1194(2) 0.3220(5) 0.13256(13) 0.0725(14) Uani 1 1 d . . . H31A H 0.1187 0.2330 0.1247 0.109 Uiso 1 1 calc R . . H31B H 0.0757 0.3639 0.1242 0.109 Uiso 1 1 calc R . . H31C H 0.1252 0.3239 0.1576 0.109 Uiso 1 1 calc R . . C32 C 0.1745(3) 0.3864(6) 0.08042(11) 0.0810(16) Uani 1 1 d . . . H32A H 0.2139 0.4325 0.0724 0.122 Uiso 1 1 calc R . . H32B H 0.1310 0.4262 0.0708 0.122 Uiso 1 1 calc R . . H32C H 0.1755 0.2969 0.0730 0.122 Uiso 1 1 calc R . . C33 C 0.17938(16) 0.3921(3) 0.11892(8) 0.0360(8) Uani 1 1 d . . . H33 H 0.1768 0.4840 0.1258 0.043 Uiso 1 1 calc R . . C34 C 0.26485(19) 0.2131(3) 0.13478(10) 0.0477(9) Uani 1 1 d . . . H34 H 0.2377 0.1436 0.1253 0.057 Uiso 1 1 calc R . . C35 C 0.32882(19) 0.2065(3) 0.15168(10) 0.0472(9) Uani 1 1 d . . . H35 H 0.3557 0.1313 0.1564 0.057 Uiso 1 1 calc R . . C36 C 0.29736(15) 0.4156(3) 0.14963(7) 0.0275(7) Uani 1 1 d . . . C37 C 0.41260(16) 0.3700(3) 0.17996(9) 0.0375(8) Uani 1 1 d . . . H37A H 0.4391 0.2933 0.1884 0.045 Uiso 1 1 calc R . . H37B H 0.4020 0.4207 0.2001 0.045 Uiso 1 1 calc R . . C38 C 0.45754(16) 0.4506(3) 0.15811(9) 0.0379(8) Uani 1 1 d . . . C39 C 0.4833(2) 0.3674(4) 0.12974(12) 0.0661(12) Uani 1 1 d . . . H39A H 0.4434 0.3344 0.1150 0.099 Uiso 1 1 calc R . . H39B H 0.5105 0.2956 0.1401 0.099 Uiso 1 1 calc R . . H39C H 0.5125 0.4191 0.1161 0.099 Uiso 1 1 calc R . . C40 C 0.5194(2) 0.4997(4) 0.18235(12) 0.0687(14) Uani 1 1 d . . . H40A H 0.5526 0.5427 0.1690 0.103 Uiso 1 1 calc R . . H40B H 0.5422 0.4274 0.1948 0.103 Uiso 1 1 calc R . . H40C H 0.5026 0.5603 0.1987 0.103 Uiso 1 1 calc R . . C41 C 0.3661(3) 0.4301(5) 0.04712(12) 0.0764(14) Uani 1 1 d . . . H41A H 0.3344 0.3931 0.0624 0.115 Uiso 1 1 calc R . . H41B H 0.4059 0.3730 0.0460 0.115 Uiso 1 1 calc R . . H41C H 0.3417 0.4406 0.0242 0.115 Uiso 1 1 calc R . . C42 C 0.4463(2) 0.6176(5) 0.04078(11) 0.0685(13) Uani 1 1 d . . . H42A H 0.4276 0.6270 0.0168 0.103 Uiso 1 1 calc R . . H42B H 0.4869 0.5611 0.0423 0.103 Uiso 1 1 calc R . . H42C H 0.4600 0.7018 0.0502 0.103 Uiso 1 1 calc R . . C43 C 0.39143(19) 0.5607(4) 0.06094(9) 0.0462(9) Uani 1 1 d . . . H43 H 0.4128 0.5479 0.0850 0.055 Uiso 1 1 calc R . . C44 C 0.2925(2) 0.6985(5) 0.03365(9) 0.0558(11) Uani 1 1 d . . . H44 H 0.2958 0.6770 0.0104 0.067 Uiso 1 1 calc R . . C45 C 0.2483(2) 0.7807(4) 0.04544(9) 0.0556(11) Uani 1 1 d . . . H45 H 0.2135 0.8284 0.0322 0.067 Uiso 1 1 calc R . . C46 C 0.31484(16) 0.7010(3) 0.09148(8) 0.0324(7) Uani 1 1 d . . . C47 C 0.22905(18) 0.8671(3) 0.10372(10) 0.0451(9) Uani 1 1 d . . . H47A H 0.1975 0.9263 0.0900 0.054 Uiso 1 1 calc R . . H47B H 0.2650 0.9192 0.1170 0.054 Uiso 1 1 calc R . . C48 C 0.18770(17) 0.7942(3) 0.12850(9) 0.0405(8) Uani 1 1 d . . . C49 C 0.12612(18) 0.7239(4) 0.10839(11) 0.0534(10) Uani 1 1 d . . . H49A H 0.1437 0.6672 0.0913 0.080 Uiso 1 1 calc R . . H49B H 0.0943 0.7868 0.0968 0.080 Uiso 1 1 calc R . . H49C H 0.1014 0.6732 0.1243 0.080 Uiso 1 1 calc R . . C50 C 0.1599(2) 0.8943(4) 0.15195(12) 0.0606(11) Uani 1 1 d . . . H50A H 0.1328 0.8519 0.1684 0.091 Uiso 1 1 calc R . . H50B H 0.1302 0.9549 0.1382 0.091 Uiso 1 1 calc R . . H50C H 0.1989 0.9405 0.1643 0.091 Uiso 1 1 calc R . . C51 C 0.4770(3) 0.9969(5) 0.10338(11) 0.0706(13) Uani 1 1 d . . . H51A H 0.4328 1.0430 0.1026 0.106 Uiso 1 1 calc R . . H51B H 0.4881 0.9801 0.0800 0.106 Uiso 1 1 calc R . . H51C H 0.5139 1.0489 0.1154 0.106 Uiso 1 1 calc R . . C52 C 0.5384(2) 0.7991(5) 0.12472(11) 0.0661(12) Uani 1 1 d . . . H52A H 0.5751 0.8518 0.1367 0.099 Uiso 1 1 calc R . . H52B H 0.5506 0.7792 0.1017 0.099 Uiso 1 1 calc R . . H52C H 0.5336 0.7194 0.1374 0.099 Uiso 1 1 calc R . . C53 C 0.47116(17) 0.8709(4) 0.12213(8) 0.0400(8) Uani 1 1 d . . . H53 H 0.4352 0.8175 0.1087 0.048 Uiso 1 1 calc R . . C54 C 0.48037(19) 0.9751(3) 0.18075(9) 0.0446(9) Uani 1 1 d . . . H54 H 0.5212 1.0239 0.1789 0.054 Uiso 1 1 calc R . . C55 C 0.44314(19) 0.9705(3) 0.20759(9) 0.0426(9) Uani 1 1 d . . . H55 H 0.4527 1.0149 0.2287 0.051 Uiso 1 1 calc R . . C56 C 0.39042(15) 0.8395(3) 0.16686(7) 0.0290(7) Uani 1 1 d . . . C57 C 0.33614(18) 0.8514(3) 0.22104(8) 0.0398(8) Uani 1 1 d . . . H57A H 0.2894 0.8651 0.2088 0.048 Uiso 1 1 calc R . . H57B H 0.3404 0.9069 0.2416 0.048 Uiso 1 1 calc R . . C58 C 0.34287(18) 0.7102(3) 0.23249(7) 0.0360(8) Uani 1 1 d . . . C59 C 0.2820(2) 0.6828(5) 0.25296(10) 0.0637(12) Uani 1 1 d . . . H59A H 0.2384 0.6990 0.2387 0.096 Uiso 1 1 calc R . . H59B H 0.2848 0.7386 0.2731 0.096 Uiso 1 1 calc R . . H59C H 0.2836 0.5931 0.2603 0.096 Uiso 1 1 calc R . . C60 C 0.4112(2) 0.6900(4) 0.25487(9) 0.0533(10) Uani 1 1 d . . . H60A H 0.4159 0.5995 0.2612 0.080 Uiso 1 1 calc R . . H60B H 0.4115 0.7423 0.2756 0.080 Uiso 1 1 calc R . . H60C H 0.4500 0.7153 0.2421 0.080 Uiso 1 1 calc R . . N1 N 0.75172(14) -0.0099(3) 0.13316(6) 0.0372(7) Uani 1 1 d . . . N2 N 0.70241(13) 0.1728(3) 0.12557(6) 0.0343(6) Uani 1 1 d . . . N3 N 0.73541(14) -0.0593(3) 0.00893(7) 0.0447(7) Uani 1 1 d . . . N4 N 0.84576(13) -0.0498(3) 0.01325(6) 0.0342(6) Uani 1 1 d . . . N5 N 0.90193(14) 0.3190(3) 0.13870(6) 0.0347(6) Uani 1 1 d . . . N6 N 0.88136(14) 0.4457(2) 0.09622(7) 0.0362(6) Uani 1 1 d . . . N7 N 0.24646(13) 0.3408(2) 0.13389(7) 0.0325(6) Uani 1 1 d . . . N8 N 0.34762(13) 0.3295(2) 0.16077(7) 0.0320(6) Uani 1 1 d . . . N9 N 0.33291(15) 0.6500(3) 0.06206(6) 0.0396(7) Uani 1 1 d . . . N10 N 0.26258(14) 0.7837(3) 0.08063(7) 0.0394(7) Uani 1 1 d . . . N11 N 0.44759(13) 0.8946(2) 0.15611(6) 0.0329(6) Uani 1 1 d . . . N12 N 0.38830(13) 0.8890(2) 0.19879(6) 0.0308(6) Uani 1 1 d . . . O1 O 0.72040(10) 0.2681(2) 0.05711(5) 0.0320(5) Uani 1 1 d . . . O2 O 0.88895(10) 0.04482(19) 0.08045(5) 0.0280(5) Uani 1 1 d . . . O3 O 0.86514(10) 0.2831(2) 0.03523(5) 0.0313(5) Uani 1 1 d . . . O4 O 0.42029(10) 0.55424(19) 0.14378(5) 0.0285(5) Uani 1 1 d . . . O5 O 0.23071(10) 0.7075(2) 0.14721(5) 0.0341(5) Uani 1 1 d . . . O6 O 0.34107(11) 0.6315(2) 0.20414(5) 0.0312(5) Uani 1 1 d . . . Sc1 Sc 0.81326(3) 0.17630(5) 0.065942(13) 0.02211(15) Uani 1 1 d . . . Sc2 Sc 0.32874(3) 0.63951(5) 0.153198(13) 0.02174(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 C1 0.088(3) 0.052(3) 0.072(3) -0.003(2) -0.007(3) -0.002(2) C2 0.069(3) 0.055(3) 0.077(3) 0.016(2) -0.014(2) -0.002(2) C3 0.052(2) 0.042(2) 0.044(2) 0.0167(17) 0.0113(17) -0.0042(17) C4 0.047(2) 0.066(3) 0.0364(19) 0.0144(18) 0.0130(16) -0.014(2) C5 0.042(2) 0.077(3) 0.0294(18) 0.0007(18) 0.0137(15) -0.010(2) C6 0.0309(16) 0.0319(18) 0.0274(16) 0.0012(13) 0.0004(13) -0.0057(14) C7 0.0343(17) 0.043(2) 0.0385(18) -0.0097(16) 0.0096(14) 0.0009(15) C8 0.0297(16) 0.0384(19) 0.0386(18) -0.0048(15) 0.0063(14) 0.0051(14) C9 0.0314(17) 0.059(2) 0.0403(19) -0.0070(17) 0.0063(15) 0.0041(17) C10 0.051(2) 0.048(2) 0.054(2) 0.0006(18) 0.0121(18) 0.0156(18) C11 0.060(3) 0.131(5) 0.078(3) 0.014(3) 0.008(3) -0.013(3) C12 0.042(2) 0.090(4) 0.084(3) -0.001(3) -0.013(2) -0.008(2) C13 0.0333(19) 0.067(3) 0.062(2) -0.022(2) -0.0057(18) -0.0044(19) C14 0.052(3) 0.070(3) 0.091(3) -0.053(3) -0.008(2) -0.004(2) C15 0.054(2) 0.061(3) 0.072(3) -0.045(2) -0.005(2) 0.013(2) C16 0.0312(16) 0.0328(18) 0.0263(15) -0.0023(13) -0.0015(13) -0.0021(14) C17 0.0308(16) 0.0334(18) 0.0375(18) -0.0020(14) 0.0075(14) 0.0025(14) C18 0.0241(15) 0.0252(16) 0.0372(17) 0.0034(13) 0.0004(13) 0.0000(13) C19 0.044(2) 0.032(2) 0.061(2) 0.0073(17) 0.0053(17) 0.0062(16) C20 0.0325(17) 0.040(2) 0.047(2) 0.0027(16) 0.0010(15) 0.0017(15) C21 0.073(3) 0.087(3) 0.049(2) 0.008(2) 0.021(2) -0.001(3) C22 0.049(2) 0.064(3) 0.056(2) 0.013(2) -0.0006(19) -0.006(2) C23 0.0410(18) 0.043(2) 0.0268(16) 0.0029(15) -0.0016(14) -0.0111(16) C24 0.053(2) 0.044(2) 0.042(2) -0.0119(18) -0.0078(17) -0.0163(18) C25 0.059(2) 0.0301(19) 0.055(2) -0.0063(17) -0.0046(19) -0.0160(17) C26 0.0320(16) 0.0301(17) 0.0299(16) -0.0018(13) 0.0033(13) -0.0025(14) C27 0.046(2) 0.0222(17) 0.051(2) 0.0095(15) -0.0016(16) -0.0063(15) C28 0.0343(18) 0.049(2) 0.058(2) 0.0156(19) 0.0067(16) -0.0113(17) C29 0.0347(17) 0.0286(17) 0.0389(18) 0.0140(14) 0.0047(14) -0.0057(14) C30 0.054(2) 0.044(2) 0.048(2) 0.0229(18) 0.0031(17) -0.0079(18) C31 0.042(2) 0.085(4) 0.090(3) 0.024(3) 0.005(2) -0.003(2) C32 0.068(3) 0.125(5) 0.047(2) -0.003(3) -0.011(2) 0.015(3) C33 0.0337(17) 0.0305(18) 0.0420(18) -0.0003(15) -0.0056(14) -0.0036(14) C34 0.047(2) 0.0186(17) 0.075(3) -0.0056(17) -0.0035(19) -0.0046(15) C35 0.049(2) 0.0185(17) 0.073(3) 0.0026(17) 0.0040(19) 0.0043(15) C36 0.0269(15) 0.0280(16) 0.0278(15) 0.0013(13) 0.0035(12) -0.0002(13) C37 0.0312(17) 0.0342(19) 0.0453(19) 0.0125(15) -0.0057(14) 0.0078(14) C38 0.0287(16) 0.0283(18) 0.056(2) 0.0075(16) 0.0039(15) 0.0067(14) C39 0.063(3) 0.046(2) 0.096(3) 0.012(2) 0.037(2) 0.022(2) C40 0.039(2) 0.060(3) 0.101(3) 0.034(3) -0.025(2) -0.004(2) C41 0.098(4) 0.064(3) 0.069(3) -0.030(2) 0.016(3) -0.015(3) C42 0.061(3) 0.092(4) 0.053(2) -0.006(2) 0.012(2) -0.013(3) C43 0.055(2) 0.049(2) 0.0344(18) -0.0113(17) 0.0042(16) -0.0045(19) C44 0.058(2) 0.084(3) 0.0233(18) 0.0086(19) -0.0066(17) -0.021(2) C45 0.052(2) 0.076(3) 0.035(2) 0.026(2) -0.0148(18) -0.009(2) C46 0.0354(17) 0.0285(17) 0.0308(17) 0.0020(14) -0.0079(14) -0.0081(14) C47 0.044(2) 0.0276(18) 0.060(2) 0.0122(17) -0.0143(17) 0.0016(16) C48 0.0319(17) 0.0286(18) 0.059(2) 0.0018(16) -0.0079(16) 0.0085(14) C49 0.0311(18) 0.049(2) 0.076(3) 0.013(2) -0.0156(18) 0.0017(17) C50 0.052(2) 0.044(2) 0.083(3) -0.004(2) -0.003(2) 0.0218(19) C51 0.090(3) 0.075(3) 0.049(2) 0.019(2) 0.015(2) 0.008(3) C52 0.067(3) 0.070(3) 0.063(3) 0.005(2) 0.015(2) 0.013(2) C53 0.0383(18) 0.048(2) 0.0335(18) -0.0024(16) 0.0024(14) -0.0145(16) C54 0.051(2) 0.039(2) 0.041(2) -0.0029(16) -0.0108(17) -0.0205(17) C55 0.057(2) 0.035(2) 0.0333(18) -0.0084(15) -0.0078(16) -0.0128(17) C56 0.0318(16) 0.0233(16) 0.0304(16) 0.0009(13) -0.0042(13) 0.0029(13) C57 0.046(2) 0.040(2) 0.0335(17) -0.0091(15) 0.0011(15) 0.0053(16) C58 0.049(2) 0.0381(19) 0.0208(15) -0.0026(14) 0.0015(14) -0.0022(16) C59 0.081(3) 0.068(3) 0.047(2) -0.006(2) 0.028(2) -0.011(2) C60 0.069(3) 0.046(2) 0.039(2) -0.0014(17) -0.0201(19) -0.005(2) N1 0.0380(15) 0.0442(17) 0.0300(14) 0.0080(13) 0.0061(12) -0.0101(13) N2 0.0327(14) 0.0484(18) 0.0228(13) -0.0021(12) 0.0071(11) -0.0053(13) N3 0.0357(15) 0.0472(19) 0.0496(17) -0.0204(15) -0.0037(13) -0.0030(14) N4 0.0344(14) 0.0363(16) 0.0314(14) -0.0109(12) 0.0005(11) 0.0034(12) N5 0.0374(15) 0.0332(15) 0.0327(14) -0.0039(12) -0.0005(12) -0.0095(12) N6 0.0421(15) 0.0227(14) 0.0432(16) -0.0042(12) 0.0011(13) -0.0049(12) N7 0.0340(14) 0.0217(14) 0.0409(15) -0.0032(11) -0.0003(12) -0.0031(11) N8 0.0330(14) 0.0224(14) 0.0404(15) 0.0052(11) 0.0031(12) 0.0023(11) N9 0.0449(16) 0.0466(18) 0.0261(14) -0.0010(13) -0.0026(12) -0.0161(14) N10 0.0412(16) 0.0354(16) 0.0386(15) 0.0140(13) -0.0100(13) -0.0038(13) N11 0.0347(14) 0.0295(15) 0.0326(14) 0.0003(11) -0.0050(11) -0.0100(12) N12 0.0389(15) 0.0238(14) 0.0288(13) -0.0049(11) -0.0012(11) -0.0016(11) O1 0.0267(11) 0.0376(13) 0.0326(11) 0.0000(10) 0.0070(9) 0.0053(9) O2 0.0295(11) 0.0266(11) 0.0274(10) 0.0024(9) 0.0017(9) 0.0034(9) O3 0.0345(11) 0.0275(12) 0.0329(11) 0.0056(9) 0.0086(9) -0.0051(9) O4 0.0252(10) 0.0225(11) 0.0377(12) 0.0031(9) 0.0023(9) 0.0045(9) O5 0.0266(11) 0.0326(12) 0.0417(12) 0.0072(10) -0.0029(9) 0.0071(9) O6 0.0395(12) 0.0306(12) 0.0224(10) -0.0006(9) -0.0017(9) -0.0013(10) Sc1 0.0236(3) 0.0209(3) 0.0219(3) 0.0013(2) 0.0026(2) -0.0027(2) Sc2 0.0230(3) 0.0186(3) 0.0227(3) 0.0003(2) -0.0023(2) 0.0007(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C3 1.514(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.515(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 N1 1.469(5) . ? C3 H3 1.0000 . ? C4 C5 1.343(6) . ? C4 N1 1.388(4) . ? C4 H4 0.9500 . ? C5 N2 1.383(4) . ? C5 H5 0.9500 . ? C6 N2 1.361(4) . ? C6 N1 1.367(4) . ? C6 Sc1 2.452(3) . ? C7 N2 1.461(4) . ? C7 C8 1.535(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O1 1.390(4) . ? C8 C9 1.537(5) . ? C8 C10 1.538(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.510(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.516(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N3 1.471(4) . ? C13 H13 1.0000 . ? C14 C15 1.340(6) . ? C14 N3 1.381(5) . ? C14 H14 0.9500 . ? C15 N4 1.371(4) . ? C15 H15 0.9500 . ? C16 N4 1.356(4) . ? C16 N3 1.357(4) . ? C16 Sc1 2.411(3) . ? C17 N4 1.461(4) . ? C17 C18 1.542(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O2 1.385(4) . ? C18 C20 1.535(4) . ? C18 C19 1.538(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.513(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.517(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 N5 1.464(4) . ? C23 H23 1.0000 . ? C24 C25 1.329(5) . ? C24 N5 1.384(4) . ? C24 H24 0.9500 . ? C25 N6 1.382(4) . ? C25 H25 0.9500 . ? C26 N6 1.359(4) . ? C26 N5 1.361(4) . ? C26 Sc1 2.402(3) . ? C27 N6 1.465(4) . ? C27 C29 1.533(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.533(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 O3 1.386(4) . ? C29 C30 1.534(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.515(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.506(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 N7 1.471(4) . ? C33 H33 1.0000 . ? C34 C35 1.346(5) . ? C34 N7 1.380(4) . ? C34 H34 0.9500 . ? C35 N8 1.374(4) . ? C35 H35 0.9500 . ? C36 N7 1.357(4) . ? C36 N8 1.364(4) . ? C36 Sc2 2.417(3) . ? C37 N8 1.461(4) . ? C37 C38 1.534(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 O4 1.388(4) . ? C38 C39 1.536(5) . ? C38 C40 1.539(5) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C43 1.530(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.510(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 N9 1.472(5) . ? C43 H43 1.0000 . ? C44 C45 1.327(6) . ? C44 N9 1.391(5) . ? C44 H44 0.9500 . ? C45 N10 1.382(4) . ? C45 H45 0.9500 . ? C46 N9 1.351(4) . ? C46 N10 1.365(4) . ? C46 Sc2 2.495(3) . ? C47 N10 1.457(5) . ? C47 C48 1.525(5) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 O5 1.389(4) . ? C48 C50 1.528(5) . ? C48 C49 1.546(5) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C53 1.518(6) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.497(5) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 N11 1.474(4) . ? C53 H53 1.0000 . ? C54 C55 1.337(5) . ? C54 N11 1.386(4) . ? C54 H54 0.9500 . ? C55 N12 1.377(4) . ? C55 H55 0.9500 . ? C56 N11 1.352(4) . ? C56 N12 1.361(4) . ? C56 Sc2 2.439(3) . ? C57 N12 1.455(4) . ? C57 C58 1.544(5) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 O6 1.382(4) . ? C58 C59 1.520(5) . ? C58 C60 1.525(5) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? O1 Sc1 2.036(2) . ? O2 Sc1 2.046(2) . ? O3 Sc1 1.989(2) . ? O4 Sc2 2.051(2) . ? O5 Sc2 2.017(2) . ? O6 Sc2 1.9923(19) . ? 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 C3 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C1 110.8(3) . . ? N1 C3 C2 111.1(3) . . ? C1 C3 C2 111.2(3) . . ? N1 C3 H3 107.9 . . ? C1 C3 H3 107.9 . . ? C2 C3 H3 107.9 . . ? C5 C4 N1 106.7(3) . . ? C5 C4 H4 126.7 . . ? N1 C4 H4 126.7 . . ? C4 C5 N2 106.8(3) . . ? C4 C5 H5 126.6 . . ? N2 C5 H5 126.6 . . ? N2 C6 N1 103.5(3) . . ? N2 C6 Sc1 119.1(2) . . ? N1 C6 Sc1 137.4(2) . . ? N2 C7 C8 113.6(3) . . ? N2 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N2 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? O1 C8 C7 110.1(2) . . ? O1 C8 C9 110.7(3) . . ? C7 C8 C9 110.0(3) . . ? O1 C8 C10 110.0(3) . . ? C7 C8 C10 106.3(3) . . ? C9 C8 C10 109.7(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 H11A 109.5 . . ? C13 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C13 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C11 110.5(4) . . ? N3 C13 C12 111.4(3) . . ? C11 C13 C12 111.0(4) . . ? N3 C13 H13 107.9 . . ? C11 C13 H13 107.9 . . ? C12 C13 H13 107.9 . . ? C15 C14 N3 106.8(3) . . ? C15 C14 H14 126.6 . . ? N3 C14 H14 126.6 . . ? C14 C15 N4 106.4(3) . . ? C14 C15 H15 126.8 . . ? N4 C15 H15 126.8 . . ? N4 C16 N3 103.3(3) . . ? N4 C16 Sc1 116.0(2) . . ? N3 C16 Sc1 139.9(2) . . ? N4 C17 C18 112.2(3) . . ? N4 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? N4 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? O2 C18 C20 110.9(3) . . ? O2 C18 C19 109.3(3) . . ? C20 C18 C19 109.4(3) . . ? O2 C18 C17 110.9(2) . . ? C20 C18 C17 106.8(3) . . ? C19 C18 C17 109.6(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 H21A 109.5 . . ? C23 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C23 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N5 C23 C21 110.8(3) . . ? N5 C23 C22 110.9(3) . . ? C21 C23 C22 112.7(3) . . ? N5 C23 H23 107.4 . . ? C21 C23 H23 107.4 . . ? C22 C23 H23 107.4 . . ? C25 C24 N5 107.1(3) . . ? C25 C24 H24 126.4 . . ? N5 C24 H24 126.4 . . ? C24 C25 N6 106.8(3) . . ? C24 C25 H25 126.6 . . ? N6 C25 H25 126.6 . . ? N6 C26 N5 103.4(3) . . ? N6 C26 Sc1 118.7(2) . . ? N5 C26 Sc1 136.1(2) . . ? N6 C27 C29 112.2(3) . . ? N6 C27 H27A 109.2 . . ? C29 C27 H27A 109.2 . . ? N6 C27 H27B 109.2 . . ? C29 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C28 110.0(3) . . ? O3 C29 C27 109.8(2) . . ? C28 C29 C27 110.6(3) . . ? O3 C29 C30 109.8(3) . . ? C28 C29 C30 109.3(3) . . ? C27 C29 C30 107.2(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 H31A 109.5 . . ? C33 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C33 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C33 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N7 C33 C32 110.5(3) . . ? N7 C33 C31 111.1(3) . . ? C32 C33 C31 111.3(3) . . ? N7 C33 H33 107.9 . . ? C32 C33 H33 107.9 . . ? C31 C33 H33 107.9 . . ? C35 C34 N7 106.5(3) . . ? C35 C34 H34 126.7 . . ? N7 C34 H34 126.7 . . ? C34 C35 N8 106.6(3) . . ? C34 C35 H35 126.7 . . ? N8 C35 H35 126.7 . . ? N7 C36 N8 103.1(3) . . ? N7 C36 Sc2 138.7(2) . . ? N8 C36 Sc2 116.9(2) . . ? N8 C37 C38 112.2(3) . . ? N8 C37 H37A 109.2 . . ? C38 C37 H37A 109.2 . . ? N8 C37 H37B 109.2 . . ? C38 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? O4 C38 C37 110.8(2) . . ? O4 C38 C39 109.9(3) . . ? C37 C38 C39 109.9(3) . . ? O4 C38 C40 109.2(3) . . ? C37 C38 C40 106.6(3) . . ? C39 C38 C40 110.4(3) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C43 C41 H41A 109.5 . . ? C43 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C43 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 H42A 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C43 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N9 C43 C42 110.5(3) . . ? N9 C43 C41 110.9(3) . . ? C42 C43 C41 112.5(3) . . ? N9 C43 H43 107.6 . . ? C42 C43 H43 107.6 . . ? C41 C43 H43 107.6 . . ? C45 C44 N9 106.6(3) . . ? C45 C44 H44 126.7 . . ? N9 C44 H44 126.7 . . ? C44 C45 N10 107.1(3) . . ? C44 C45 H45 126.5 . . ? N10 C45 H45 126.5 . . ? N9 C46 N10 103.3(3) . . ? N9 C46 Sc2 135.9(2) . . ? N10 C46 Sc2 118.0(2) . . ? N10 C47 C48 113.2(3) . . ? N10 C47 H47A 108.9 . . ? C48 C47 H47A 108.9 . . ? N10 C47 H47B 108.9 . . ? C48 C47 H47B 108.9 . . ? H47A C47 H47B 107.7 . . ? O5 C48 C47 109.8(3) . . ? O5 C48 C50 110.9(3) . . ? C47 C48 C50 106.4(3) . . ? O5 C48 C49 110.5(3) . . ? C47 C48 C49 109.8(3) . . ? C50 C48 C49 109.4(3) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C53 C51 H51A 109.5 . . ? C53 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C53 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 H52A 109.5 . . ? C53 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C53 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N11 C53 C52 111.7(3) . . ? N11 C53 C51 109.8(3) . . ? C52 C53 C51 111.1(3) . . ? N11 C53 H53 108.0 . . ? C52 C53 H53 108.0 . . ? C51 C53 H53 108.0 . . ? C55 C54 N11 106.5(3) . . ? C55 C54 H54 126.8 . . ? N11 C54 H54 126.8 . . ? C54 C55 N12 106.7(3) . . ? C54 C55 H55 126.6 . . ? N12 C55 H55 126.6 . . ? N11 C56 N12 103.2(2) . . ? N11 C56 Sc2 133.9(2) . . ? N12 C56 Sc2 118.0(2) . . ? N12 C57 C58 113.0(3) . . ? N12 C57 H57A 109.0 . . ? C58 C57 H57A 109.0 . . ? N12 C57 H57B 109.0 . . ? C58 C57 H57B 109.0 . . ? H57A C57 H57B 107.8 . . ? O6 C58 C59 110.9(3) . . ? O6 C58 C60 109.3(3) . . ? C59 C58 C60 110.0(3) . . ? O6 C58 C57 109.8(2) . . ? C59 C58 C57 106.7(3) . . ? C60 C58 C57 110.0(3) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C6 N1 C4 111.3(3) . . ? C6 N1 C3 123.6(3) . . ? C4 N1 C3 125.0(3) . . ? C6 N2 C5 111.6(3) . . ? C6 N2 C7 123.7(3) . . ? C5 N2 C7 124.5(3) . . ? C16 N3 C14 111.3(3) . . ? C16 N3 C13 122.8(3) . . ? C14 N3 C13 125.9(3) . . ? C16 N4 C15 112.1(3) . . ? C16 N4 C17 122.6(3) . . ? C15 N4 C17 125.2(3) . . ? C26 N5 C24 111.1(3) . . ? C26 N5 C23 123.0(3) . . ? C24 N5 C23 125.8(3) . . ? C26 N6 C25 111.5(3) . . ? C26 N6 C27 122.0(3) . . ? C25 N6 C27 126.0(3) . . ? C36 N7 C34 111.9(3) . . ? C36 N7 C33 122.9(3) . . ? C34 N7 C33 125.2(3) . . ? C36 N8 C35 111.9(3) . . ? C36 N8 C37 121.5(3) . . ? C35 N8 C37 126.6(3) . . ? C46 N9 C44 111.6(3) . . ? C46 N9 C43 122.9(3) . . ? C44 N9 C43 125.4(3) . . ? C46 N10 C45 111.3(3) . . ? C46 N10 C47 123.2(3) . . ? C45 N10 C47 125.5(3) . . ? C56 N11 C54 111.8(3) . . ? C56 N11 C53 123.3(2) . . ? C54 N11 C53 124.9(3) . . ? C56 N12 C55 111.8(3) . . ? C56 N12 C57 122.5(3) . . ? C55 N12 C57 125.5(3) . . ? C8 O1 Sc1 140.14(19) . . ? C18 O2 Sc1 132.79(17) . . ? C29 O3 Sc1 138.1(2) . . ? C38 O4 Sc2 133.52(19) . . ? C48 O5 Sc2 142.9(2) . . ? C58 O6 Sc2 140.8(2) . . ? O3 Sc1 O1 97.10(9) . . ? O3 Sc1 O2 98.88(8) . . ? O1 Sc1 O2 163.42(9) . . ? O3 Sc1 C26 80.31(10) . . ? O1 Sc1 C26 96.87(10) . . ? O2 Sc1 C26 90.20(9) . . ? O3 Sc1 C16 93.41(10) . . ? O1 Sc1 C16 96.82(9) . . ? O2 Sc1 C16 77.84(9) . . ? C26 Sc1 C16 165.54(11) . . ? O3 Sc1 C6 164.33(10) . . ? O1 Sc1 C6 78.40(9) . . ? O2 Sc1 C6 87.29(9) . . ? C26 Sc1 C6 85.31(10) . . ? C16 Sc1 C6 102.00(10) . . ? O6 Sc2 O5 98.45(9) . . ? O6 Sc2 O4 98.37(8) . . ? O5 Sc2 O4 162.16(9) . . ? O6 Sc2 C36 91.22(9) . . ? O5 Sc2 C36 96.09(9) . . ? O4 Sc2 C36 77.63(9) . . ? O6 Sc2 C56 78.99(9) . . ? O5 Sc2 C56 99.07(10) . . ? O4 Sc2 C56 89.96(9) . . ? C36 Sc2 C56 162.99(10) . . ? O6 Sc2 C46 167.46(10) . . ? O5 Sc2 C46 77.82(10) . . ? O4 Sc2 C46 86.93(10) . . ? C36 Sc2 C46 101.04(10) . . ? C56 Sc2 C46 89.71(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C4 C5 N2 -0.1(4) . . . . ? N2 C7 C8 O1 -60.8(4) . . . . ? N2 C7 C8 C9 61.4(3) . . . . ? N2 C7 C8 C10 -179.9(3) . . . . ? N3 C14 C15 N4 -0.2(6) . . . . ? N4 C17 C18 O2 -55.1(3) . . . . ? N4 C17 C18 C20 -175.9(3) . . . . ? N4 C17 C18 C19 65.6(3) . . . . ? N5 C24 C25 N6 0.7(4) . . . . ? N6 C27 C29 O3 64.7(3) . . . . ? N6 C27 C29 C28 -56.9(3) . . . . ? N6 C27 C29 C30 -176.0(3) . . . . ? N7 C34 C35 N8 0.3(4) . . . . ? N8 C37 C38 O4 54.6(4) . . . . ? N8 C37 C38 C39 -67.0(4) . . . . ? N8 C37 C38 C40 173.3(3) . . . . ? N9 C44 C45 N10 1.0(4) . . . . ? N10 C47 C48 O5 56.7(4) . . . . ? N10 C47 C48 C50 176.7(3) . . . . ? N10 C47 C48 C49 -64.9(3) . . . . ? N11 C54 C55 N12 -0.6(4) . . . . ? N12 C57 C58 O6 -55.3(4) . . . . ? N12 C57 C58 C59 -175.6(3) . . . . ? N12 C57 C58 C60 65.1(3) . . . . ? N2 C6 N1 C4 -0.6(3) . . . . ? Sc1 C6 N1 C4 179.9(3) . . . . ? N2 C6 N1 C3 -178.8(3) . . . . ? Sc1 C6 N1 C3 1.6(5) . . . . ? C5 C4 N1 C6 0.4(4) . . . . ? C5 C4 N1 C3 178.7(3) . . . . ? C1 C3 N1 C6 -110.1(4) . . . . ? C2 C3 N1 C6 125.7(3) . . . . ? C1 C3 N1 C4 71.8(4) . . . . ? C2 C3 N1 C4 -52.3(5) . . . . ? N1 C6 N2 C5 0.5(3) . . . . ? Sc1 C6 N2 C5 -179.8(2) . . . . ? N1 C6 N2 C7 176.6(3) . . . . ? Sc1 C6 N2 C7 -3.7(4) . . . . ? C4 C5 N2 C6 -0.3(4) . . . . ? C4 C5 N2 C7 -176.3(3) . . . . ? C8 C7 N2 C6 56.4(4) . . . . ? C8 C7 N2 C5 -128.0(3) . . . . ? N4 C16 N3 C14 0.1(4) . . . . ? Sc1 C16 N3 C14 -169.0(3) . . . . ? N4 C16 N3 C13 -178.0(3) . . . . ? Sc1 C16 N3 C13 12.9(6) . . . . ? C15 C14 N3 C16 0.1(5) . . . . ? C15 C14 N3 C13 178.1(4) . . . . ? C11 C13 N3 C16 -108.6(4) . . . . ? C12 C13 N3 C16 127.6(4) . . . . ? C11 C13 N3 C14 73.6(5) . . . . ? C12 C13 N3 C14 -50.2(6) . . . . ? N3 C16 N4 C15 -0.2(4) . . . . ? Sc1 C16 N4 C15 172.0(3) . . . . ? N3 C16 N4 C17 -179.0(3) . . . . ? Sc1 C16 N4 C17 -6.7(4) . . . . ? C14 C15 N4 C16 0.2(5) . . . . ? C14 C15 N4 C17 179.0(4) . . . . ? C18 C17 N4 C16 63.7(4) . . . . ? C18 C17 N4 C15 -115.0(4) . . . . ? N6 C26 N5 C24 -0.3(4) . . . . ? Sc1 C26 N5 C24 163.7(3) . . . . ? N6 C26 N5 C23 -177.8(3) . . . . ? Sc1 C26 N5 C23 -13.8(5) . . . . ? C25 C24 N5 C26 -0.3(4) . . . . ? C25 C24 N5 C23 177.2(3) . . . . ? C21 C23 N5 C26 -111.0(4) . . . . ? C22 C23 N5 C26 123.0(3) . . . . ? C21 C23 N5 C24 71.9(4) . . . . ? C22 C23 N5 C24 -54.1(4) . . . . ? N5 C26 N6 C25 0.7(4) . . . . ? Sc1 C26 N6 C25 -166.7(2) . . . . ? N5 C26 N6 C27 172.7(3) . . . . ? Sc1 C26 N6 C27 5.3(4) . . . . ? C24 C25 N6 C26 -0.9(4) . . . . ? C24 C25 N6 C27 -172.5(3) . . . . ? C29 C27 N6 C26 -59.5(4) . . . . ? C29 C27 N6 C25 111.2(4) . . . . ? N8 C36 N7 C34 -0.8(4) . . . . ? Sc2 C36 N7 C34 164.9(3) . . . . ? N8 C36 N7 C33 177.3(3) . . . . ? Sc2 C36 N7 C33 -17.0(5) . . . . ? C35 C34 N7 C36 0.4(4) . . . . ? C35 C34 N7 C33 -177.7(3) . . . . ? C32 C33 N7 C36 109.2(4) . . . . ? C31 C33 N7 C36 -126.8(4) . . . . ? C32 C33 N7 C34 -73.0(5) . . . . ? C31 C33 N7 C34 51.1(5) . . . . ? N7 C36 N8 C35 1.0(4) . . . . ? Sc2 C36 N8 C35 -168.4(2) . . . . ? N7 C36 N8 C37 -179.0(3) . . . . ? Sc2 C36 N8 C37 11.5(4) . . . . ? C34 C35 N8 C36 -0.9(4) . . . . ? C34 C35 N8 C37 179.2(3) . . . . ? C38 C37 N8 C36 -66.7(4) . . . . ? C38 C37 N8 C35 113.3(4) . . . . ? N10 C46 N9 C44 -0.7(4) . . . . ? Sc2 C46 N9 C44 158.9(3) . . . . ? N10 C46 N9 C43 175.7(3) . . . . ? Sc2 C46 N9 C43 -24.7(5) . . . . ? C45 C44 N9 C46 -0.2(4) . . . . ? C45 C44 N9 C43 -176.4(3) . . . . ? C42 C43 N9 C46 -117.2(3) . . . . ? C41 C43 N9 C46 117.3(4) . . . . ? C42 C43 N9 C44 58.6(4) . . . . ? C41 C43 N9 C44 -66.8(5) . . . . ? N9 C46 N10 C45 1.3(4) . . . . ? Sc2 C46 N10 C45 -162.7(2) . . . . ? N9 C46 N10 C47 -176.4(3) . . . . ? Sc2 C46 N10 C47 19.6(4) . . . . ? C44 C45 N10 C46 -1.5(4) . . . . ? C44 C45 N10 C47 176.2(3) . . . . ? C48 C47 N10 C46 -66.2(4) . . . . ? C48 C47 N10 C45 116.4(4) . . . . ? N12 C56 N11 C54 0.5(3) . . . . ? Sc2 C56 N11 C54 -152.8(3) . . . . ? N12 C56 N11 C53 -179.3(3) . . . . ? Sc2 C56 N11 C53 27.4(4) . . . . ? C55 C54 N11 C56 0.1(4) . . . . ? C55 C54 N11 C53 179.8(3) . . . . ? C52 C53 N11 C56 -112.4(4) . . . . ? C51 C53 N11 C56 123.9(3) . . . . ? C52 C53 N11 C54 67.8(4) . . . . ? C51 C53 N11 C54 -55.9(4) . . . . ? N11 C56 N12 C55 -0.9(3) . . . . ? Sc2 C56 N12 C55 157.6(2) . . . . ? N11 C56 N12 C57 -177.1(3) . . . . ? Sc2 C56 N12 C57 -18.6(4) . . . . ? C54 C55 N12 C56 1.0(4) . . . . ? C54 C55 N12 C57 177.1(3) . . . . ? C58 C57 N12 C56 66.1(4) . . . . ? C58 C57 N12 C55 -109.6(3) . . . . ? C7 C8 O1 Sc1 11.2(5) . . . . ? C9 C8 O1 Sc1 -110.6(3) . . . . ? C10 C8 O1 Sc1 128.0(3) . . . . ? C20 C18 O2 Sc1 105.2(3) . . . . ? C19 C18 O2 Sc1 -134.1(2) . . . . ? C17 C18 O2 Sc1 -13.2(4) . . . . ? C28 C29 O3 Sc1 108.0(3) . . . . ? C27 C29 O3 Sc1 -13.9(4) . . . . ? C30 C29 O3 Sc1 -131.6(3) . . . . ? C37 C38 O4 Sc2 14.6(4) . . . . ? C39 C38 O4 Sc2 136.3(3) . . . . ? C40 C38 O4 Sc2 -102.5(3) . . . . ? C47 C48 O5 Sc2 -1.5(5) . . . . ? C50 C48 O5 Sc2 -118.8(4) . . . . ? C49 C48 O5 Sc2 119.7(3) . . . . ? C59 C58 O6 Sc2 114.2(3) . . . . ? C60 C58 O6 Sc2 -124.3(3) . . . . ? C57 C58 O6 Sc2 -3.4(5) . . . . ? C29 O3 Sc1 O1 71.0(3) . . . . ? C29 O3 Sc1 O2 -113.5(3) . . . . ? C29 O3 Sc1 C26 -24.8(3) . . . . ? C29 O3 Sc1 C16 168.3(3) . . . . ? C29 O3 Sc1 C6 -1.2(5) . . . . ? C8 O1 Sc1 O3 -139.3(3) . . . . ? C8 O1 Sc1 O2 56.4(5) . . . . ? C8 O1 Sc1 C26 -58.2(3) . . . . ? C8 O1 Sc1 C16 126.4(3) . . . . ? C8 O1 Sc1 C6 25.5(3) . . . . ? C18 O2 Sc1 O3 -42.6(2) . . . . ? C18 O2 Sc1 O1 121.7(3) . . . . ? C18 O2 Sc1 C26 -122.8(2) . . . . ? C18 O2 Sc1 C16 49.0(2) . . . . ? C18 O2 Sc1 C6 151.9(2) . . . . ? N6 C26 Sc1 O3 28.7(2) . . . . ? N5 C26 Sc1 O3 -133.5(3) . . . . ? N6 C26 Sc1 O1 -67.3(2) . . . . ? N5 C26 Sc1 O1 130.5(3) . . . . ? N6 C26 Sc1 O2 127.7(2) . . . . ? N5 C26 Sc1 O2 -34.5(3) . . . . ? N6 C26 Sc1 C16 93.8(5) . . . . ? N5 C26 Sc1 C16 -68.4(6) . . . . ? N6 C26 Sc1 C6 -145.0(2) . . . . ? N5 C26 Sc1 C6 52.8(3) . . . . ? N4 C16 Sc1 O3 62.0(2) . . . . ? N3 C16 Sc1 O3 -129.8(4) . . . . ? N4 C16 Sc1 O1 159.6(2) . . . . ? N3 C16 Sc1 O1 -32.2(4) . . . . ? N4 C16 Sc1 O2 -36.3(2) . . . . ? N3 C16 Sc1 O2 131.8(4) . . . . ? N4 C16 Sc1 C26 -1.6(6) . . . . ? N3 C16 Sc1 C26 166.6(4) . . . . ? N4 C16 Sc1 C6 -120.9(2) . . . . ? N3 C16 Sc1 C6 47.3(4) . . . . ? N2 C6 Sc1 O3 46.3(5) . . . . ? N1 C6 Sc1 O3 -134.2(4) . . . . ? N2 C6 Sc1 O1 -28.3(2) . . . . ? N1 C6 Sc1 O1 151.2(3) . . . . ? N2 C6 Sc1 O2 160.1(2) . . . . ? N1 C6 Sc1 O2 -20.4(3) . . . . ? N2 C6 Sc1 C26 69.7(2) . . . . ? N1 C6 Sc1 C26 -110.8(3) . . . . ? N2 C6 Sc1 C16 -122.9(2) . . . . ? N1 C6 Sc1 C16 56.6(3) . . . . ? C58 O6 Sc2 O5 -63.1(3) . . . . ? C58 O6 Sc2 O4 122.9(3) . . . . ? C58 O6 Sc2 C36 -159.4(3) . . . . ? C58 O6 Sc2 C56 34.6(3) . . . . ? C58 O6 Sc2 C46 8.6(6) . . . . ? C48 O5 Sc2 O6 138.3(3) . . . . ? C48 O5 Sc2 O4 -61.4(5) . . . . ? C48 O5 Sc2 C36 -129.6(3) . . . . ? C48 O5 Sc2 C56 58.2(3) . . . . ? C48 O5 Sc2 C46 -29.6(3) . . . . ? C38 O4 Sc2 O6 40.7(3) . . . . ? C38 O4 Sc2 O5 -119.7(3) . . . . ? C38 O4 Sc2 C36 -48.7(3) . . . . ? C38 O4 Sc2 C56 119.5(3) . . . . ? C38 O4 Sc2 C46 -150.8(3) . . . . ? N7 C36 Sc2 O6 130.0(3) . . . . ? N8 C36 Sc2 O6 -65.6(2) . . . . ? N7 C36 Sc2 O5 31.4(3) . . . . ? N8 C36 Sc2 O5 -164.2(2) . . . . ? N7 C36 Sc2 O4 -131.7(3) . . . . ? N8 C36 Sc2 O4 32.7(2) . . . . ? N7 C36 Sc2 C56 -175.6(3) . . . . ? N8 C36 Sc2 C56 -11.3(5) . . . . ? N7 C36 Sc2 C46 -47.3(3) . . . . ? N8 C36 Sc2 C46 117.0(2) . . . . ? N11 C56 Sc2 O6 129.1(3) . . . . ? N12 C56 Sc2 O6 -21.3(2) . . . . ? N11 C56 Sc2 O5 -134.0(3) . . . . ? N12 C56 Sc2 O5 75.6(2) . . . . ? N11 C56 Sc2 O4 30.5(3) . . . . ? N12 C56 Sc2 O4 -119.8(2) . . . . ? N11 C56 Sc2 C36 73.2(5) . . . . ? N12 C56 Sc2 C36 -77.1(4) . . . . ? N11 C56 Sc2 C46 -56.4(3) . . . . ? N12 C56 Sc2 C46 153.2(2) . . . . ? N9 C46 Sc2 O6 147.2(4) . . . . ? N10 C46 Sc2 O6 -55.4(6) . . . . ? N9 C46 Sc2 O5 -138.9(3) . . . . ? N10 C46 Sc2 O5 18.5(2) . . . . ? N9 C46 Sc2 O4 31.8(3) . . . . ? N10 C46 Sc2 O4 -170.8(2) . . . . ? N9 C46 Sc2 C36 -45.0(3) . . . . ? N10 C46 Sc2 C36 112.4(2) . . . . ? N9 C46 Sc2 C56 121.8(3) . . . . ? N10 C46 Sc2 C56 -80.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.329 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.061 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 0.000 -0.055 0.250 714 97 ' ' 2 1.000 -0.095 0.750 714 97 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 954361' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_po3005_refinalized _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H114 N12 O6 S4 Sc2' _chemical_formula_weight 1485.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.3119 1.5331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 24.272(5) _cell_length_b 15.167(5) _cell_length_c 24.651(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 107.109(5) _cell_angle_gamma 90.000(5) _cell_volume 8673(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 16186 _cell_measurement_theta_min 3.4600 _cell_measurement_theta_max 75.4320 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2283 _exptl_crystal_size_mid 0.1232 _exptl_crystal_size_min 0.0862 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 2.652 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.896 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 5.1574 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71477 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 76.57 _reflns_number_total 17775 _reflns_number_gt 13679 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ortep _computing_publication_material mercury _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^ > 2\s(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. DIFMX01_ALERT_2_B The maximum difference density is > 0.1*ZMAX*1.00 _refine_diff_density_max given = 2.186 Test value = 2.100 PLAT097_ALERT_2_B Large Reported Max. (Positive) Residual Density 2.19 eA-3 Residual peak 2.19 eA-3 high located 0.83 A from Sc1. RFACR01_ALERT_3_B The value of the weighted R factor is > 0.35 Weighted R factor given 0.375 PLAT084_ALERT_3_B High wR2 Value (i.e. > 0.25) ................... 0.37 PLAT341_ALERT_3_B Low Bond Precision on C-C Bonds ............... 0.0164 Ang. Crystal was badly twinned and therefore was treated as such but this may have affected quality of the data. This is reflected in the high wR2 factor and in the low precision of C-C bond. The thermal parameters are reasonable and actual molecule is well behaved. ; _vrf_DIFMX01_po3005_refinalized ; PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00 RESPONSE: See _refine_special_details ; _vrf_RFACR01_po3005_refinalized ; PROBLEM: The value of the weighted R factor is > 0.35 RESPONSE: See _refine_special_details ; _vrf_PLAT084_po3005_refinalized ; PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.37 RESPONSE: See _refine_special_details ; _vrf_PLAT097_po3005_refinalized ; PROBLEM: Large Reported Max. (Positive) Residual Density 2.19 eA-3 RESPONSE: See _refine_special_details ; _vrf_PLAT341_po3005_refinalized ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0164 Ang. RESPONSE: See _refine_special_details ; _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17775 _refine_ls_number_parameters 884 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1573 _refine_ls_R_factor_gt 0.1314 _refine_ls_wR_factor_ref 0.3747 _refine_ls_wR_factor_gt 0.3421 _refine_ls_goodness_of_fit_ref 1.483 _refine_ls_restrained_S_all 1.482 _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 C1 C 0.8458(5) 0.5882(7) 0.5321(5) 0.066(2) Uani 1 1 d . . . H8A H 0.8144 0.5470 0.5311 0.099 Uiso 1 1 calc R . . H8B H 0.8749 0.5851 0.5693 0.099 Uiso 1 1 calc R . . H8C H 0.8635 0.5725 0.5025 0.099 Uiso 1 1 calc R . . C2 C 0.8673(4) 0.7501(7) 0.5232(4) 0.061(2) Uani 1 1 d . . . H9A H 0.8492 0.8084 0.5162 0.091 Uiso 1 1 calc R . . H9B H 0.8857 0.7370 0.4936 0.091 Uiso 1 1 calc R . . H9C H 0.8965 0.7497 0.5604 0.091 Uiso 1 1 calc R . . C3 C 0.8220(3) 0.6812(6) 0.5221(4) 0.0507(19) Uani 1 1 d . . . H7 H 0.7932 0.6828 0.4835 0.061 Uiso 1 1 calc R . . C4 C 0.8171(3) 0.7094(5) 0.6225(3) 0.0428(16) Uani 1 1 d . . . H6 H 0.8568 0.7021 0.6423 0.051 Uiso 1 1 calc R . . C5 C 0.7741(4) 0.7287(4) 0.6454(3) 0.0433(16) Uani 1 1 d . . . H5 H 0.7783 0.7372 0.6846 0.052 Uiso 1 1 calc R . . C6 C 0.7350(3) 0.7192(4) 0.5530(3) 0.0405(15) Uani 1 1 d . . . C7 C 0.6662(3) 0.7545(5) 0.6080(4) 0.0442(17) Uani 1 1 d . . . H4A H 0.6385 0.7610 0.5696 0.053 Uiso 1 1 calc R . . H4B H 0.6681 0.8116 0.6279 0.053 Uiso 1 1 calc R . . C8 C 0.6440(4) 0.6831(5) 0.6408(4) 0.0490(18) Uani 1 1 d . . . C9 C 0.6400(4) 0.5937(6) 0.6096(4) 0.059(2) Uani 1 1 d . . . H3A H 0.6257 0.5484 0.6304 0.089 Uiso 1 1 calc R . . H3B H 0.6783 0.5768 0.6075 0.089 Uiso 1 1 calc R . . H3C H 0.6136 0.5992 0.5711 0.089 Uiso 1 1 calc R . . C10 C 0.5833(4) 0.7136(8) 0.6400(5) 0.069(3) Uani 1 1 d . . . H2A H 0.5665 0.6706 0.6602 0.103 Uiso 1 1 calc R . . H2B H 0.5589 0.7186 0.6006 0.103 Uiso 1 1 calc R . . H2C H 0.5859 0.7712 0.6587 0.103 Uiso 1 1 calc R . . C11 C 0.6927(3) 0.7205(5) 0.4950(3) 0.0414(15) Uani 1 1 d . . . C12 C 0.8512(6) 0.6132(7) 0.9298(5) 0.083(3) Uani 1 1 d . . . H19A H 0.8245 0.6592 0.9342 0.124 Uiso 1 1 calc R . . H19B H 0.8897 0.6384 0.9362 0.124 Uiso 1 1 calc R . . H19C H 0.8527 0.5661 0.9574 0.124 Uiso 1 1 calc R . . C13 C 0.8709(4) 0.5034(6) 0.8612(4) 0.061(2) Uani 1 1 d . . . H18A H 0.8566 0.4805 0.8224 0.091 Uiso 1 1 calc R . . H18B H 0.8726 0.4554 0.8883 0.091 Uiso 1 1 calc R . . H18C H 0.9096 0.5280 0.8673 0.091 Uiso 1 1 calc R . . C14 C 0.8304(4) 0.5755(5) 0.8700(4) 0.0518(19) Uani 1 1 d . . . H17 H 0.8284 0.6239 0.8420 0.062 Uiso 1 1 calc R . . C15 C 0.7582(5) 0.4661(5) 0.8904(4) 0.060(2) Uani 1 1 d . . . H16 H 0.7843 0.4332 0.9196 0.072 Uiso 1 1 calc R . . C16 C 0.7014(5) 0.4535(5) 0.8700(5) 0.068(3) Uani 1 1 d . . . H15 H 0.6792 0.4101 0.8820 0.082 Uiso 1 1 calc R . . C17 C 0.7246(4) 0.5707(4) 0.8223(4) 0.0456(17) Uani 1 1 d . . . C18 C 0.6212(5) 0.5318(6) 0.7958(5) 0.065(2) Uani 1 1 d . . . H14A H 0.5976 0.4819 0.8022 0.078 Uiso 1 1 calc R . . H14B H 0.6177 0.5337 0.7547 0.078 Uiso 1 1 calc R . . C19 C 0.5974(4) 0.6192(5) 0.8130(5) 0.061(2) Uani 1 1 d . . . C20 C 0.6024(6) 0.6198(7) 0.8763(5) 0.079(3) Uani 1 1 d . . . H13A H 0.6430 0.6135 0.8984 0.118 Uiso 1 1 calc R . . H13B H 0.5802 0.5707 0.8849 0.118 Uiso 1 1 calc R . . H13C H 0.5874 0.6756 0.8861 0.118 Uiso 1 1 calc R . . C21 C 0.5350(5) 0.6289(7) 0.7787(6) 0.081(3) Uani 1 1 d . . . H12A H 0.5319 0.6285 0.7382 0.121 Uiso 1 1 calc R . . H12B H 0.5199 0.6847 0.7884 0.121 Uiso 1 1 calc R . . H12C H 0.5126 0.5798 0.7872 0.121 Uiso 1 1 calc R . . C22 C 0.5659(6) 0.8862(8) 0.8364(7) 0.096(4) Uani 1 1 d . . . H29A H 0.5974 0.8594 0.8663 0.144 Uiso 1 1 calc R . . H29B H 0.5296 0.8566 0.8348 0.144 Uiso 1 1 calc R . . H29C H 0.5630 0.9489 0.8448 0.144 Uiso 1 1 calc R . . C23 C 0.5295(5) 0.9186(8) 0.7328(7) 0.087(4) Uani 1 1 d . . . H28A H 0.5380 0.9113 0.6965 0.130 Uiso 1 1 calc R . . H28B H 0.5268 0.9815 0.7406 0.130 Uiso 1 1 calc R . . H28C H 0.4928 0.8897 0.7307 0.130 Uiso 1 1 calc R . . C24 C 0.5777(4) 0.8767(6) 0.7803(5) 0.067(3) Uani 1 1 d . . . H27 H 0.5784 0.8123 0.7719 0.081 Uiso 1 1 calc R . . C25 C 0.6503(5) 1.0003(5) 0.7941(5) 0.066(3) Uani 1 1 d . . . H26 H 0.6275 1.0460 0.8029 0.080 Uiso 1 1 calc R . . C26 C 0.7039(4) 1.0084(5) 0.7914(4) 0.057(2) Uani 1 1 d . . . H25 H 0.7261 1.0611 0.7964 0.068 Uiso 1 1 calc R . . C27 C 0.6777(3) 0.8645(4) 0.7737(4) 0.0455(17) Uani 1 1 d . . . C28 C 0.7784(4) 0.9057(5) 0.7757(4) 0.054(2) Uani 1 1 d . . . H24A H 0.8025 0.9594 0.7846 0.065 Uiso 1 1 calc R . . H24B H 0.7750 0.8889 0.7360 0.065 Uiso 1 1 calc R . . C29 C 0.8087(4) 0.8313(5) 0.8151(5) 0.059(2) Uani 1 1 d . . . C30 C 0.8133(6) 0.8520(7) 0.8763(5) 0.087(4) Uani 1 1 d . . . H23A H 0.8329 0.8034 0.9006 0.131 Uiso 1 1 calc R . . H23B H 0.7745 0.8594 0.8803 0.131 Uiso 1 1 calc R . . H23C H 0.8353 0.9065 0.8877 0.131 Uiso 1 1 calc R . . C31 C 0.8682(4) 0.8187(7) 0.8052(7) 0.090(4) Uani 1 1 d . . . H22A H 0.8629 0.8059 0.7650 0.135 Uiso 1 1 calc R . . H22B H 0.8885 0.7696 0.8284 0.135 Uiso 1 1 calc R . . H22C H 0.8910 0.8728 0.8158 0.135 Uiso 1 1 calc R . . C32 C 0.0349(5) 0.6369(10) 0.8394(6) 0.110(6) Uani 1 1 d . . . H40A H 0.0337 0.5954 0.8086 0.165 Uiso 1 1 calc R . . H40B H 0.0048 0.6216 0.8570 0.165 Uiso 1 1 calc R . . H40C H 0.0727 0.6338 0.8680 0.165 Uiso 1 1 calc R . . C33 C 0.0262(5) 0.7973(14) 0.8601(6) 0.122(7) Uani 1 1 d . . . H39A H 0.0195 0.8556 0.8424 0.182 Uiso 1 1 calc R . . H39B H 0.0640 0.7963 0.8889 0.182 Uiso 1 1 calc R . . H39C H -0.0039 0.7844 0.8781 0.182 Uiso 1 1 calc R . . C34 C 0.0249(4) 0.7291(9) 0.8158(4) 0.073(3) Uani 1 1 d . . . H38 H -0.0139 0.7311 0.7869 0.088 Uiso 1 1 calc R . . C35 C 0.1276(3) 0.7588(5) 0.8138(4) 0.0429(16) Uani 1 1 d . . . H37 H 0.1462 0.7546 0.8534 0.051 Uiso 1 1 calc R . . C36 C 0.1530(3) 0.7747(4) 0.7736(3) 0.0372(15) Uani 1 1 d . . . H36 H 0.1930 0.7831 0.7792 0.045 Uiso 1 1 calc R . . C37 C 0.0586(3) 0.7609(4) 0.7315(3) 0.0384(15) Uani 1 1 d . . . C38 C 0.1182(3) 0.7975(5) 0.6664(3) 0.0431(16) Uani 1 1 d . . . H35A H 0.1399 0.8535 0.6694 0.052 Uiso 1 1 calc R . . H35B H 0.0800 0.8063 0.6383 0.052 Uiso 1 1 calc R . . C39 C 0.1508(3) 0.7244(4) 0.6450(3) 0.0402(15) Uani 1 1 d . . . C40 C 0.1177(4) 0.6376(5) 0.6392(4) 0.053(2) Uani 1 1 d . . . H33A H 0.1387 0.5916 0.6256 0.079 Uiso 1 1 calc R . . H33B H 0.0794 0.6450 0.6120 0.079 Uiso 1 1 calc R . . H33C H 0.1137 0.6205 0.6762 0.079 Uiso 1 1 calc R . . C41 C 0.1545(4) 0.7544(6) 0.5867(4) 0.0523(19) Uani 1 1 d . . . H34A H 0.1758 0.8101 0.5908 0.078 Uiso 1 1 calc R . . H34B H 0.1155 0.7630 0.5610 0.078 Uiso 1 1 calc R . . H34C H 0.1744 0.7094 0.5710 0.078 Uiso 1 1 calc R . . C42 C 0.0011(3) 0.7545(5) 0.6891(3) 0.0403(15) Uani 1 1 d . . . C43 C 0.2429(5) 0.9573(7) 0.5375(4) 0.064(2) Uani 1 1 d . . . H49A H 0.2048 0.9474 0.5426 0.097 Uiso 1 1 calc R . . H49B H 0.2446 0.9289 0.5023 0.097 Uiso 1 1 calc R . . H49C H 0.2495 1.0208 0.5353 0.097 Uiso 1 1 calc R . . C44 C 0.3490(5) 0.9306(6) 0.5826(5) 0.064(2) Uani 1 1 d . . . H50A H 0.3766 0.9039 0.6158 0.096 Uiso 1 1 calc R . . H50B H 0.3573 0.9937 0.5813 0.096 Uiso 1 1 calc R . . H50C H 0.3521 0.9020 0.5481 0.096 Uiso 1 1 calc R . . C45 C 0.2884(4) 0.9187(5) 0.5868(4) 0.0510(19) Uani 1 1 d . . . H48 H 0.2808 0.8541 0.5881 0.061 Uiso 1 1 calc R . . C46 C 0.2925(4) 1.0467(5) 0.6547(4) 0.0513(19) Uani 1 1 d . . . H47 H 0.2984 1.0931 0.6311 0.062 Uiso 1 1 calc R . . C47 C 0.2894(4) 1.0548(4) 0.7078(4) 0.0466(17) Uani 1 1 d . . . H46 H 0.2925 1.1077 0.7291 0.056 Uiso 1 1 calc R . . C48 C 0.2781(3) 0.9086(4) 0.6840(3) 0.0354(14) Uani 1 1 d . . . C49 C 0.2761(3) 0.9506(4) 0.7816(3) 0.0426(16) Uani 1 1 d . . . H45A H 0.2362 0.9313 0.7781 0.051 Uiso 1 1 calc R . . H45B H 0.2836 1.0050 0.8048 0.051 Uiso 1 1 calc R . . C50 C 0.3184(4) 0.8782(4) 0.8124(3) 0.0457(17) Uani 1 1 d . . . C51 C 0.3114(6) 0.8680(6) 0.8723(4) 0.073(3) Uani 1 1 d . . . H44A H 0.2715 0.8516 0.8692 0.109 Uiso 1 1 calc R . . H44B H 0.3206 0.9240 0.8929 0.109 Uiso 1 1 calc R . . H44C H 0.3375 0.8220 0.8931 0.109 Uiso 1 1 calc R . . C52 C 0.3806(4) 0.9036(5) 0.8164(5) 0.064(3) Uani 1 1 d . . . H43A H 0.4068 0.8570 0.8363 0.097 Uiso 1 1 calc R . . H43B H 0.3904 0.9591 0.8373 0.097 Uiso 1 1 calc R . . H43C H 0.3842 0.9108 0.7781 0.097 Uiso 1 1 calc R . . C53 C 0.4299(4) 0.6623(6) 0.8665(5) 0.059(2) Uani 1 1 d . . . H59A H 0.4354 0.7077 0.8403 0.089 Uiso 1 1 calc R . . H59B H 0.4604 0.6179 0.8723 0.089 Uiso 1 1 calc R . . H59C H 0.4314 0.6895 0.9030 0.089 Uiso 1 1 calc R . . C54 C 0.3615(4) 0.5462(6) 0.8818(5) 0.066(3) Uani 1 1 d . . . H60A H 0.3238 0.5186 0.8647 0.099 Uiso 1 1 calc R . . H60B H 0.3623 0.5725 0.9183 0.099 Uiso 1 1 calc R . . H60C H 0.3918 0.5015 0.8877 0.099 Uiso 1 1 calc R . . C55 C 0.3717(3) 0.6187(5) 0.8417(4) 0.0478(18) Uani 1 1 d . . . H58 H 0.3410 0.6646 0.8370 0.057 Uiso 1 1 calc R . . C56 C 0.3994(4) 0.5107(5) 0.7773(5) 0.056(2) Uani 1 1 d . . . H57 H 0.4265 0.4781 0.8060 0.068 Uiso 1 1 calc R . . C57 C 0.3853(4) 0.4965(5) 0.7208(5) 0.055(2) Uani 1 1 d . . . H56 H 0.3994 0.4511 0.7019 0.066 Uiso 1 1 calc R . . C58 C 0.3342(3) 0.6147(4) 0.7363(3) 0.0415(16) Uani 1 1 d . . . C59 C 0.3219(4) 0.5784(5) 0.6360(4) 0.058(2) Uani 1 1 d . . . H55A H 0.2793 0.5786 0.6260 0.069 Uiso 1 1 calc R . . H55B H 0.3334 0.5294 0.6150 0.069 Uiso 1 1 calc R . . C60 C 0.3421(4) 0.6659(5) 0.6169(4) 0.056(2) Uani 1 1 d . . . C61 C 0.4079(4) 0.6697(7) 0.6337(5) 0.068(3) Uani 1 1 d . . . H54A H 0.4236 0.6634 0.6750 0.102 Uiso 1 1 calc R . . H54B H 0.4200 0.7264 0.6220 0.102 Uiso 1 1 calc R . . H54C H 0.4223 0.6217 0.6150 0.102 Uiso 1 1 calc R . . C62 C 0.3160(5) 0.6752(8) 0.5532(5) 0.073(3) Uani 1 1 d . . . H53A H 0.3285 0.7310 0.5407 0.109 Uiso 1 1 calc R . . H53B H 0.2739 0.6744 0.5438 0.109 Uiso 1 1 calc R . . H53C H 0.3289 0.6261 0.5341 0.109 Uiso 1 1 calc R . . C63 C 0.9955(6) 0.5749(9) 0.4679(6) 0.112(5) Uani 1 1 d D . . H63 H 0.9930 0.6269 0.4458 0.134 Uiso 1 1 calc R . . C64 C 0.9925(5) 0.5813(8) 0.5227(5) 0.093(4) Uani 1 1 d D . . H64 H 0.9868 0.6369 0.5379 0.112 Uiso 1 1 calc R . . C65 C 0.9978(6) 0.5059(8) 0.5555(6) 0.102(4) Uani 1 1 d D . . H65 H 0.9968 0.5096 0.5937 0.122 Uiso 1 1 calc R . . C66 C 0.5010(5) 0.5846(7) 0.0219(4) 0.066(2) Uani 1 1 d . . . H66 H 0.5023 0.6424 0.0372 0.080 Uiso 1 1 calc R . . C67 C 0.4620(5) 0.5249(7) 0.0285(4) 0.066(2) Uani 1 1 d . . . H67 H 0.4350 0.5414 0.0478 0.079 Uiso 1 1 calc R . . C68 C 0.4611(5) 0.4407(7) 0.0075(4) 0.069(3) Uani 1 1 d . . . H68 H 0.4340 0.3992 0.0133 0.083 Uiso 1 1 calc R . . C69 C 0.0391(7) 1.0615(11) 0.9899(7) 0.127(6) Uani 1 1 d D . . H69 H 0.0655 1.1028 0.9826 0.152 Uiso 1 1 calc R . . C70 C 0.0306(7) 0.9798(9) 0.9637(7) 0.105(5) Uani 1 1 d D . . H70 H 0.0520 0.9650 0.9383 0.126 Uiso 1 1 calc R . . C71 C -0.0077(9) 0.9192(11) 0.9730(8) 0.141(8) Uani 1 1 d D . . H71 H -0.0127 0.8640 0.9540 0.169 Uiso 1 1 calc R . . C72 C 0.0003(9) 0.5811(13) 1.0304(8) 0.187(9) Uani 1 1 d DU . . H72 H 0.0001 0.6337 1.0513 0.224 Uiso 1 1 calc R . . C73 C 0.0267(9) 0.5753(19) 0.9878(9) 0.179(9) Uani 1 1 d DU . . H73 H 0.0452 0.6253 0.9778 0.214 Uiso 1 1 calc R . . C74 C 0.0259(7) 0.4961(18) 0.9600(9) 0.169(9) Uani 1 1 d DU . . H74 H 0.0451 0.4943 0.9315 0.202 Uiso 1 1 calc R . . N1 N 0.7915(3) 0.7022(4) 0.5637(3) 0.0423(13) Uani 1 1 d . . . N2 N 0.7236(3) 0.7337(3) 0.6024(3) 0.0392(13) Uani 1 1 d . . . N3 N 0.7722(3) 0.5372(4) 0.8604(3) 0.0485(15) Uani 1 1 d . . . N4 N 0.6807(3) 0.5172(4) 0.8276(3) 0.0539(17) Uani 1 1 d . . . N5 N 0.6333(3) 0.9128(4) 0.7817(3) 0.0538(18) Uani 1 1 d . . . N6 N 0.7212(3) 0.9262(3) 0.7800(3) 0.0470(15) Uani 1 1 d . . . N7 N 0.0690(3) 0.7496(4) 0.7871(3) 0.0423(13) Uani 1 1 d . . . N8 N 0.1101(3) 0.7767(3) 0.7224(3) 0.0386(13) Uani 1 1 d . . . N9 N 0.2855(3) 0.9576(4) 0.6404(3) 0.0472(15) Uani 1 1 d . . . N10 N 0.2808(3) 0.9705(3) 0.7253(3) 0.0381(12) Uani 1 1 d . . . N11 N 0.3674(3) 0.5808(4) 0.7854(3) 0.0467(15) Uani 1 1 d . . . N12 N 0.3454(3) 0.5629(4) 0.6959(3) 0.0491(16) Uani 1 1 d . . . O1 O 0.6805(2) 0.6761(3) 0.6943(3) 0.0491(12) Uani 1 1 d . . . O2 O 0.6300(2) 0.6887(3) 0.8016(3) 0.0519(14) Uani 1 1 d . . . O3 O 0.7769(2) 0.7518(3) 0.7985(3) 0.0562(16) Uani 1 1 d . . . O4 O 0.2051(2) 0.7163(3) 0.6830(2) 0.0440(11) Uani 1 1 d . . . O5 O 0.3038(3) 0.7989(3) 0.7829(2) 0.0468(12) Uani 1 1 d . . . O6 O 0.3217(2) 0.7348(3) 0.6443(3) 0.0467(13) Uani 1 1 d . . . S1 S 0.67422(10) 0.62356(13) 0.46401(10) 0.0548(5) Uani 1 1 d . . . S2 S 0.67302(10) 0.82308(12) 0.47062(9) 0.0510(5) Uani 1 1 d . . . S3 S -0.02866(8) 0.85235(12) 0.66433(9) 0.0476(5) Uani 1 1 d . . . S4 S -0.02443(8) 0.65332(12) 0.67407(9) 0.0479(5) Uani 1 1 d . . . Sc1 Sc 0.69745(6) 0.70858(8) 0.77399(6) 0.0402(3) Uani 1 1 d . . . Sc2 Sc 0.28545(5) 0.75266(8) 0.70520(6) 0.0356(3) 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 C1 0.070(6) 0.062(5) 0.066(6) -0.007(5) 0.020(5) 0.010(4) C2 0.059(5) 0.084(7) 0.044(5) 0.000(4) 0.021(4) -0.020(4) C3 0.044(4) 0.065(5) 0.039(4) -0.004(4) 0.005(3) -0.002(4) C4 0.047(4) 0.033(3) 0.047(4) 0.001(3) 0.011(3) -0.003(3) C5 0.060(4) 0.028(3) 0.047(4) 0.000(3) 0.022(4) -0.001(3) C6 0.049(4) 0.026(3) 0.051(4) 0.004(3) 0.021(3) 0.000(3) C7 0.049(4) 0.037(3) 0.053(5) 0.004(3) 0.024(4) 0.007(3) C8 0.053(4) 0.033(3) 0.065(5) 0.003(3) 0.024(4) 0.002(3) C9 0.066(5) 0.046(4) 0.066(6) -0.005(4) 0.019(5) -0.017(4) C10 0.059(5) 0.078(7) 0.080(7) 0.011(5) 0.038(5) 0.006(5) C11 0.044(4) 0.037(3) 0.042(4) 0.000(3) 0.012(3) -0.005(3) C12 0.115(9) 0.048(5) 0.070(7) -0.006(5) 0.005(6) 0.012(5) C13 0.067(5) 0.040(4) 0.069(6) -0.006(4) 0.009(4) 0.006(4) C14 0.064(5) 0.036(3) 0.048(5) 0.001(3) 0.004(4) 0.011(3) C15 0.098(7) 0.027(3) 0.062(5) 0.012(3) 0.036(5) 0.017(4) C16 0.113(8) 0.023(3) 0.091(7) 0.018(4) 0.065(7) 0.017(4) C17 0.066(5) 0.025(3) 0.055(5) -0.001(3) 0.031(4) 0.005(3) C18 0.082(6) 0.035(4) 0.087(7) 0.004(4) 0.040(6) -0.007(4) C19 0.071(5) 0.034(4) 0.099(7) 0.017(4) 0.057(5) 0.002(3) C20 0.109(8) 0.048(5) 0.107(9) 0.013(5) 0.073(8) 0.010(5) C21 0.069(6) 0.059(6) 0.126(10) 0.017(6) 0.048(7) -0.003(5) C22 0.111(9) 0.061(6) 0.148(13) 0.013(7) 0.088(10) 0.012(6) C23 0.064(6) 0.061(6) 0.135(11) 0.013(7) 0.030(7) 0.014(5) C24 0.070(6) 0.036(4) 0.112(8) 0.007(4) 0.050(6) 0.009(4) C25 0.095(7) 0.024(3) 0.093(7) 0.000(4) 0.047(6) 0.008(4) C26 0.078(6) 0.020(3) 0.071(6) 0.000(3) 0.020(5) 0.006(3) C27 0.054(4) 0.024(3) 0.066(5) 0.005(3) 0.028(4) 0.005(3) C28 0.062(5) 0.029(3) 0.069(6) 0.006(3) 0.015(4) 0.000(3) C29 0.051(4) 0.029(3) 0.089(7) 0.011(4) 0.008(4) -0.002(3) C30 0.102(8) 0.045(5) 0.086(8) 0.023(5) -0.017(7) -0.020(5) C31 0.056(5) 0.057(6) 0.152(13) 0.017(7) 0.022(7) -0.005(4) C32 0.084(8) 0.137(12) 0.089(9) 0.063(9) -0.006(7) -0.057(8) C33 0.050(6) 0.24(2) 0.086(9) -0.074(11) 0.042(6) -0.029(9) C34 0.043(4) 0.128(10) 0.044(5) 0.006(5) 0.006(4) -0.020(5) C35 0.040(4) 0.036(3) 0.048(4) 0.003(3) 0.005(3) -0.004(3) C36 0.034(3) 0.028(3) 0.051(4) -0.005(3) 0.013(3) -0.001(2) C37 0.051(4) 0.016(2) 0.051(4) 0.000(3) 0.019(3) 0.000(2) C38 0.043(4) 0.039(3) 0.048(4) 0.009(3) 0.015(3) 0.003(3) C39 0.043(4) 0.031(3) 0.048(4) 0.002(3) 0.015(3) -0.001(3) C40 0.049(4) 0.032(3) 0.076(6) -0.006(4) 0.017(4) -0.002(3) C41 0.055(4) 0.054(5) 0.053(5) 0.006(4) 0.025(4) 0.004(4) C42 0.045(4) 0.034(3) 0.046(4) 0.001(3) 0.020(3) 0.002(3) C43 0.083(6) 0.054(5) 0.055(5) 0.002(4) 0.019(5) -0.015(5) C44 0.087(7) 0.045(4) 0.074(6) 0.005(4) 0.046(6) -0.007(4) C45 0.071(5) 0.039(4) 0.050(5) 0.001(3) 0.027(4) -0.005(3) C46 0.063(5) 0.027(3) 0.069(6) 0.006(3) 0.028(4) -0.004(3) C47 0.060(4) 0.023(3) 0.058(5) -0.001(3) 0.019(4) -0.002(3) C48 0.047(4) 0.023(3) 0.039(4) 0.003(2) 0.018(3) 0.000(2) C49 0.056(4) 0.020(3) 0.051(4) -0.002(3) 0.016(3) 0.003(3) C50 0.064(4) 0.020(3) 0.047(4) 0.001(3) 0.007(4) 0.005(3) C51 0.118(9) 0.038(4) 0.062(6) -0.003(4) 0.027(6) 0.011(5) C52 0.057(5) 0.038(4) 0.078(6) -0.010(4) -0.013(5) 0.007(3) C53 0.054(4) 0.043(4) 0.078(6) 0.009(4) 0.013(4) -0.002(3) C54 0.061(5) 0.051(5) 0.079(7) 0.028(5) 0.011(5) 0.000(4) C55 0.047(4) 0.034(3) 0.058(5) 0.008(3) 0.010(4) 0.008(3) C56 0.053(4) 0.033(4) 0.089(7) 0.018(4) 0.030(4) 0.011(3) C57 0.061(5) 0.024(3) 0.093(7) 0.008(4) 0.040(5) 0.008(3) C58 0.040(3) 0.030(3) 0.058(5) 0.000(3) 0.021(3) 0.003(3) C59 0.076(6) 0.029(3) 0.075(6) -0.013(4) 0.033(5) -0.001(3) C60 0.069(5) 0.036(4) 0.072(6) -0.003(4) 0.038(5) 0.007(3) C61 0.071(6) 0.062(5) 0.083(7) 0.002(5) 0.042(5) 0.014(5) C62 0.089(7) 0.070(6) 0.063(6) -0.015(5) 0.028(5) 0.015(5) C63 0.082(8) 0.119(12) 0.114(12) -0.040(10) -0.002(8) 0.015(8) C64 0.080(8) 0.083(8) 0.092(9) -0.005(7) -0.013(7) 0.002(6) C65 0.103(10) 0.117(12) 0.091(9) -0.016(9) 0.037(8) -0.005(9) C66 0.085(7) 0.053(5) 0.057(6) 0.003(4) 0.014(5) 0.004(5) C67 0.077(6) 0.064(6) 0.057(6) -0.002(4) 0.020(5) 0.011(5) C68 0.093(7) 0.056(5) 0.061(6) 0.005(4) 0.026(5) -0.001(5) C69 0.119(12) 0.172(19) 0.100(11) -0.006(12) 0.049(10) -0.026(12) C70 0.129(11) 0.088(9) 0.120(12) -0.016(8) 0.072(10) 0.018(9) C71 0.21(2) 0.120(14) 0.122(14) 0.014(11) 0.096(16) -0.012(15) C72 0.104(10) 0.28(2) 0.152(14) 0.114(15) 0.001(9) 0.033(12) C73 0.082(7) 0.28(2) 0.155(14) 0.128(15) 0.006(8) 0.021(12) C74 0.064(6) 0.28(2) 0.152(14) 0.133(15) 0.021(8) 0.029(12) N1 0.044(3) 0.035(3) 0.044(3) 0.002(2) 0.006(3) -0.005(2) N2 0.049(3) 0.021(2) 0.051(4) 0.002(2) 0.020(3) 0.003(2) N3 0.076(4) 0.026(3) 0.048(4) 0.005(2) 0.025(3) 0.006(3) N4 0.079(5) 0.022(3) 0.072(5) 0.009(3) 0.040(4) 0.003(3) N5 0.072(4) 0.021(3) 0.077(5) 0.000(3) 0.035(4) 0.010(3) N6 0.062(4) 0.016(2) 0.065(4) 0.001(2) 0.023(3) 0.002(2) N7 0.042(3) 0.041(3) 0.042(4) 0.004(3) 0.009(3) -0.002(2) N8 0.046(3) 0.024(2) 0.050(4) 0.002(2) 0.020(3) 0.003(2) N9 0.064(4) 0.031(3) 0.051(4) 0.000(3) 0.022(3) -0.007(3) N10 0.050(3) 0.019(2) 0.049(4) 0.000(2) 0.021(3) 0.002(2) N11 0.046(3) 0.027(3) 0.072(5) 0.009(3) 0.025(3) 0.005(2) N12 0.058(4) 0.024(3) 0.070(5) 0.000(3) 0.026(3) 0.006(2) O1 0.059(3) 0.037(3) 0.055(3) 0.007(2) 0.022(3) 0.006(2) O2 0.060(3) 0.033(2) 0.078(4) 0.011(3) 0.044(3) 0.007(2) O3 0.045(3) 0.031(2) 0.088(5) 0.007(3) 0.013(3) 0.000(2) O4 0.041(3) 0.037(2) 0.055(3) 0.002(2) 0.017(2) 0.0012(19) O5 0.067(3) 0.022(2) 0.049(3) 0.003(2) 0.013(3) 0.002(2) O6 0.061(3) 0.032(2) 0.059(3) 0.001(2) 0.035(3) 0.008(2) S1 0.0631(12) 0.0353(9) 0.0582(13) -0.0056(8) 0.0056(10) -0.0035(8) S2 0.0649(12) 0.0336(8) 0.0476(11) 0.0054(7) 0.0057(9) -0.0003(8) S3 0.0437(9) 0.0320(8) 0.0608(12) 0.0020(7) 0.0057(8) 0.0046(6) S4 0.0447(9) 0.0322(8) 0.0614(12) -0.0003(7) 0.0072(8) -0.0065(6) Sc1 0.0467(7) 0.0278(6) 0.0515(8) 0.0071(5) 0.0228(6) 0.0037(5) Sc2 0.0382(6) 0.0269(5) 0.0447(8) 0.0002(5) 0.0171(5) 0.0023(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C3 1.517(13) . ? C1 H8A 0.9800 . ? C1 H8B 0.9800 . ? C1 H8C 0.9800 . ? C2 C3 1.511(12) . ? C2 H9A 0.9800 . ? C2 H9B 0.9800 . ? C2 H9C 0.9800 . ? C3 N1 1.467(11) . ? C3 H7 1.0000 . ? C4 C5 1.358(11) . ? C4 N1 1.403(10) . ? C4 H6 0.9500 . ? C5 N2 1.367(10) . ? C5 H5 0.9500 . ? C6 N2 1.343(10) . ? C6 N1 1.343(10) . ? C6 C11 1.495(11) . ? C7 N2 1.474(9) . ? C7 C8 1.541(11) . ? C7 H4A 0.9900 . ? C7 H4B 0.9900 . ? C8 O1 1.360(11) . ? C8 C10 1.539(12) . ? C8 C9 1.548(11) . ? C9 H3A 0.9800 . ? C9 H3B 0.9800 . ? C9 H3C 0.9800 . ? C10 H2A 0.9800 . ? C10 H2B 0.9800 . ? C10 H2C 0.9800 . ? C11 S1 1.656(7) . ? C11 S2 1.686(7) . ? C12 C14 1.521(13) . ? C12 H19A 0.9800 . ? C12 H19B 0.9800 . ? C12 H19C 0.9800 . ? C13 C14 1.529(11) . ? C13 H18A 0.9800 . ? C13 H18B 0.9800 . ? C13 H18C 0.9800 . ? C14 N3 1.481(12) . ? C14 H17 1.0000 . ? C15 C16 1.336(15) . ? C15 N3 1.403(10) . ? C15 H16 0.9500 . ? C16 N4 1.403(11) . ? C16 H15 0.9500 . ? C17 N3 1.355(11) . ? C17 N4 1.375(10) . ? C17 Sc1 2.401(7) . ? C18 N4 1.445(13) . ? C18 C19 1.554(12) . ? C18 H14A 0.9900 . ? C18 H14B 0.9900 . ? C19 O2 1.398(9) . ? C19 C21 1.509(16) . ? C19 C20 1.527(16) . ? C20 H13A 0.9800 . ? C20 H13B 0.9800 . ? C20 H13C 0.9800 . ? C21 H12A 0.9800 . ? C21 H12B 0.9800 . ? C21 H12C 0.9800 . ? C22 C24 1.501(17) . ? C22 H29A 0.9800 . ? C22 H29B 0.9800 . ? C22 H29C 0.9800 . ? C23 C24 1.529(16) . ? C23 H28A 0.9800 . ? C23 H28B 0.9800 . ? C23 H28C 0.9800 . ? C24 N5 1.448(12) . ? C24 H27 1.0000 . ? C25 C26 1.330(14) . ? C25 N5 1.397(10) . ? C25 H26 0.9500 . ? C26 N6 1.371(9) . ? C26 H25 0.9500 . ? C27 N5 1.364(10) . ? C27 N6 1.385(10) . ? C27 Sc1 2.412(7) . ? C28 N6 1.457(11) . ? C28 C29 1.530(11) . ? C28 H24A 0.9900 . ? C28 H24B 0.9900 . ? C29 O3 1.426(9) . ? C29 C30 1.513(17) . ? C29 C31 1.547(14) . ? C30 H23A 0.9800 . ? C30 H23B 0.9800 . ? C30 H23C 0.9800 . ? C31 H22A 0.9800 . ? C31 H22B 0.9800 . ? C31 H22C 0.9800 . ? C32 C34 1.506(19) . ? C32 H40A 0.9800 . ? C32 H40B 0.9800 . ? C32 H40C 0.9800 . ? C33 C34 1.497(18) . ? C33 H39A 0.9800 . ? C33 H39B 0.9800 . ? C33 H39C 0.9800 . ? C34 N7 1.481(11) . ? C34 H38 1.0000 . ? C35 C36 1.333(11) . ? C35 N7 1.386(10) . ? C35 H37 0.9500 . ? C36 N8 1.381(10) . ? C36 H36 0.9500 . ? C37 N7 1.331(10) . ? C37 N8 1.354(9) . ? C37 C42 1.480(11) . ? C38 N8 1.484(10) . ? C38 C39 1.543(10) . ? C38 H35A 0.9900 . ? C38 H35B 0.9900 . ? C39 O4 1.380(9) . ? C39 C40 1.526(10) . ? C39 C41 1.537(11) . ? C40 H33A 0.9800 . ? C40 H33B 0.9800 . ? C40 H33C 0.9800 . ? C41 H34A 0.9800 . ? C41 H34B 0.9800 . ? C41 H34C 0.9800 . ? C42 S4 1.656(7) . ? C42 S3 1.684(7) . ? C43 C45 1.501(13) . ? C43 H49A 0.9800 . ? C43 H49B 0.9800 . ? C43 H49C 0.9800 . ? C44 C45 1.515(13) . ? C44 H50A 0.9800 . ? C44 H50B 0.9800 . ? C44 H50C 0.9800 . ? C45 N9 1.466(11) . ? C45 H48 1.0000 . ? C46 C47 1.340(12) . ? C46 N9 1.394(9) . ? C46 H47 0.9500 . ? C47 N10 1.385(8) . ? C47 H46 0.9500 . ? C48 N9 1.363(9) . ? C48 N10 1.371(9) . ? C48 Sc2 2.417(6) . ? C49 N10 1.458(10) . ? C49 C50 1.542(9) . ? C49 H45A 0.9900 . ? C49 H45B 0.9900 . ? C50 O5 1.396(8) . ? C50 C52 1.532(13) . ? C50 C51 1.545(13) . ? C51 H44A 0.9800 . ? C51 H44B 0.9800 . ? C51 H44C 0.9800 . ? C52 H43A 0.9800 . ? C52 H43B 0.9800 . ? C52 H43C 0.9800 . ? C53 C55 1.517(12) . ? C53 H59A 0.9800 . ? C53 H59B 0.9800 . ? C53 H59C 0.9800 . ? C54 C55 1.545(11) . ? C54 H60A 0.9800 . ? C54 H60B 0.9800 . ? C54 H60C 0.9800 . ? C55 N11 1.477(11) . ? C55 H58 1.0000 . ? C56 C57 1.349(14) . ? C56 N11 1.368(10) . ? C56 H57 0.9500 . ? C57 N12 1.408(10) . ? C57 H56 0.9500 . ? C58 N11 1.343(10) . ? C58 N12 1.357(10) . ? C58 Sc2 2.415(7) . ? C59 N12 1.438(12) . ? C59 C60 1.536(12) . ? C59 H55A 0.9900 . ? C59 H55B 0.9900 . ? C60 O6 1.411(9) . ? C60 C62 1.516(15) . ? C60 C61 1.529(14) . ? C61 H54A 0.9800 . ? C61 H54B 0.9800 . ? C61 H54C 0.9800 . ? C62 H53A 0.9800 . ? C62 H53B 0.9800 . ? C62 H53C 0.9800 . ? C63 C64 1.379(9) . ? C63 C65 1.385(7) 3_766 ? C63 H63 0.9500 . ? C64 C65 1.384(9) . ? C64 H64 0.9500 . ? C65 C63 1.385(7) 3_766 ? C65 H65 0.9500 . ? C66 C67 1.354(15) . ? C66 C68 1.382(15) 3_665 ? C66 H66 0.9500 . ? C67 C68 1.377(15) . ? C67 H67 0.9500 . ? C68 C66 1.382(15) 3_665 ? C68 H68 0.9500 . ? C69 C71 1.382(7) 3_577 ? C69 C70 1.385(9) . ? C69 H69 0.9500 . ? C70 C71 1.375(9) . ? C70 H70 0.9500 . ? C71 C69 1.382(7) 3_577 ? C71 H71 0.9500 . ? C72 C73 1.384(10) . ? C72 C74 1.385(7) 3_567 ? C72 H72 0.9500 . ? C73 C74 1.381(10) . ? C73 H73 0.9500 . ? C74 C72 1.385(7) 3_567 ? C74 H74 0.9500 . ? O1 Sc1 1.948(6) . ? O2 Sc1 1.971(5) . ? O3 Sc1 1.956(6) . ? O4 Sc2 1.943(5) . ? O5 Sc2 1.964(6) . ? O6 Sc2 1.970(5) . ? 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 C3 C1 H8A 109.5 . . ? C3 C1 H8B 109.5 . . ? H8A C1 H8B 109.5 . . ? C3 C1 H8C 109.5 . . ? H8A C1 H8C 109.5 . . ? H8B C1 H8C 109.5 . . ? C3 C2 H9A 109.5 . . ? C3 C2 H9B 109.5 . . ? H9A C2 H9B 109.5 . . ? C3 C2 H9C 109.5 . . ? H9A C2 H9C 109.5 . . ? H9B C2 H9C 109.5 . . ? N1 C3 C2 110.7(7) . . ? N1 C3 C1 109.4(7) . . ? C2 C3 C1 113.6(8) . . ? N1 C3 H7 107.6 . . ? C2 C3 H7 107.6 . . ? C1 C3 H7 107.6 . . ? C5 C4 N1 106.6(7) . . ? C5 C4 H6 126.7 . . ? N1 C4 H6 126.7 . . ? C4 C5 N2 108.1(7) . . ? C4 C5 H5 125.9 . . ? N2 C5 H5 125.9 . . ? N2 C6 N1 109.0(7) . . ? N2 C6 C11 126.8(7) . . ? N1 C6 C11 124.3(7) . . ? N2 C7 C8 112.6(6) . . ? N2 C7 H4A 109.1 . . ? C8 C7 H4A 109.1 . . ? N2 C7 H4B 109.1 . . ? C8 C7 H4B 109.1 . . ? H4A C7 H4B 107.8 . . ? O1 C8 C10 112.6(8) . . ? O1 C8 C7 109.6(7) . . ? C10 C8 C7 105.2(7) . . ? O1 C8 C9 110.0(7) . . ? C10 C8 C9 109.8(8) . . ? C7 C8 C9 109.6(7) . . ? C8 C9 H3A 109.5 . . ? C8 C9 H3B 109.5 . . ? H3A C9 H3B 109.5 . . ? C8 C9 H3C 109.5 . . ? H3A C9 H3C 109.5 . . ? H3B C9 H3C 109.5 . . ? C8 C10 H2A 109.5 . . ? C8 C10 H2B 109.5 . . ? H2A C10 H2B 109.5 . . ? C8 C10 H2C 109.5 . . ? H2A C10 H2C 109.5 . . ? H2B C10 H2C 109.5 . . ? C6 C11 S1 116.5(5) . . ? C6 C11 S2 113.3(5) . . ? S1 C11 S2 130.2(5) . . ? C14 C12 H19A 109.5 . . ? C14 C12 H19B 109.5 . . ? H19A C12 H19B 109.5 . . ? C14 C12 H19C 109.5 . . ? H19A C12 H19C 109.5 . . ? H19B C12 H19C 109.5 . . ? C14 C13 H18A 109.5 . . ? C14 C13 H18B 109.5 . . ? H18A C13 H18B 109.5 . . ? C14 C13 H18C 109.5 . . ? H18A C13 H18C 109.5 . . ? H18B C13 H18C 109.5 . . ? N3 C14 C12 109.4(8) . . ? N3 C14 C13 108.7(7) . . ? C12 C14 C13 111.2(8) . . ? N3 C14 H17 109.2 . . ? C12 C14 H17 109.2 . . ? C13 C14 H17 109.2 . . ? C16 C15 N3 107.1(8) . . ? C16 C15 H16 126.4 . . ? N3 C15 H16 126.4 . . ? C15 C16 N4 106.5(8) . . ? C15 C16 H15 126.8 . . ? N4 C16 H15 126.8 . . ? N3 C17 N4 103.8(6) . . ? N3 C17 Sc1 136.4(6) . . ? N4 C17 Sc1 117.0(5) . . ? N4 C18 C19 112.1(8) . . ? N4 C18 H14A 109.2 . . ? C19 C18 H14A 109.2 . . ? N4 C18 H14B 109.2 . . ? C19 C18 H14B 109.2 . . ? H14A C18 H14B 107.9 . . ? O2 C19 C21 110.4(8) . . ? O2 C19 C20 108.7(9) . . ? C21 C19 C20 109.8(9) . . ? O2 C19 C18 108.0(6) . . ? C21 C19 C18 108.8(9) . . ? C20 C19 C18 111.1(8) . . ? C19 C20 H13A 109.5 . . ? C19 C20 H13B 109.5 . . ? H13A C20 H13B 109.5 . . ? C19 C20 H13C 109.5 . . ? H13A C20 H13C 109.5 . . ? H13B C20 H13C 109.5 . . ? C19 C21 H12A 109.5 . . ? C19 C21 H12B 109.5 . . ? H12A C21 H12B 109.5 . . ? C19 C21 H12C 109.5 . . ? H12A C21 H12C 109.5 . . ? H12B C21 H12C 109.5 . . ? C24 C22 H29A 109.5 . . ? C24 C22 H29B 109.5 . . ? H29A C22 H29B 109.5 . . ? C24 C22 H29C 109.5 . . ? H29A C22 H29C 109.5 . . ? H29B C22 H29C 109.5 . . ? C24 C23 H28A 109.5 . . ? C24 C23 H28B 109.5 . . ? H28A C23 H28B 109.5 . . ? C24 C23 H28C 109.5 . . ? H28A C23 H28C 109.5 . . ? H28B C23 H28C 109.5 . . ? N5 C24 C22 111.8(10) . . ? N5 C24 C23 111.1(8) . . ? C22 C24 C23 110.8(10) . . ? N5 C24 H27 107.6 . . ? C22 C24 H27 107.6 . . ? C23 C24 H27 107.6 . . ? C26 C25 N5 107.8(7) . . ? C26 C25 H26 126.1 . . ? N5 C25 H26 126.1 . . ? C25 C26 N6 106.8(7) . . ? C25 C26 H25 126.6 . . ? N6 C26 H25 126.6 . . ? N5 C27 N6 103.2(6) . . ? N5 C27 Sc1 133.7(5) . . ? N6 C27 Sc1 121.2(5) . . ? N6 C28 C29 113.7(7) . . ? N6 C28 H24A 108.8 . . ? C29 C28 H24A 108.8 . . ? N6 C28 H24B 108.8 . . ? C29 C28 H24B 108.8 . . ? H24A C28 H24B 107.7 . . ? O3 C29 C30 109.6(8) . . ? O3 C29 C28 108.8(7) . . ? C30 C29 C28 111.2(8) . . ? O3 C29 C31 107.7(8) . . ? C30 C29 C31 112.7(10) . . ? C28 C29 C31 106.7(8) . . ? C29 C30 H23A 109.5 . . ? C29 C30 H23B 109.5 . . ? H23A C30 H23B 109.5 . . ? C29 C30 H23C 109.5 . . ? H23A C30 H23C 109.5 . . ? H23B C30 H23C 109.5 . . ? C29 C31 H22A 109.5 . . ? C29 C31 H22B 109.5 . . ? H22A C31 H22B 109.5 . . ? C29 C31 H22C 109.5 . . ? H22A C31 H22C 109.5 . . ? H22B C31 H22C 109.5 . . ? C34 C32 H40A 109.5 . . ? C34 C32 H40B 109.5 . . ? H40A C32 H40B 109.5 . . ? C34 C32 H40C 109.5 . . ? H40A C32 H40C 109.5 . . ? H40B C32 H40C 109.5 . . ? C34 C33 H39A 109.5 . . ? C34 C33 H39B 109.5 . . ? H39A C33 H39B 109.5 . . ? C34 C33 H39C 109.5 . . ? H39A C33 H39C 109.5 . . ? H39B C33 H39C 109.5 . . ? N7 C34 C33 109.9(9) . . ? N7 C34 C32 108.8(10) . . ? C33 C34 C32 113.1(12) . . ? N7 C34 H38 108.3 . . ? C33 C34 H38 108.3 . . ? C32 C34 H38 108.3 . . ? C36 C35 N7 107.4(7) . . ? C36 C35 H37 126.3 . . ? N7 C35 H37 126.3 . . ? C35 C36 N8 107.2(6) . . ? C35 C36 H36 126.4 . . ? N8 C36 H36 126.4 . . ? N7 C37 N8 106.8(7) . . ? N7 C37 C42 125.0(7) . . ? N8 C37 C42 128.2(7) . . ? N8 C38 C39 112.7(6) . . ? N8 C38 H35A 109.1 . . ? C39 C38 H35A 109.1 . . ? N8 C38 H35B 109.1 . . ? C39 C38 H35B 109.1 . . ? H35A C38 H35B 107.8 . . ? O4 C39 C40 111.1(6) . . ? O4 C39 C41 110.7(6) . . ? C40 C39 C41 109.9(7) . . ? O4 C39 C38 108.4(6) . . ? C40 C39 C38 110.1(6) . . ? C41 C39 C38 106.5(6) . . ? C39 C40 H33A 109.5 . . ? C39 C40 H33B 109.5 . . ? H33A C40 H33B 109.5 . . ? C39 C40 H33C 109.5 . . ? H33A C40 H33C 109.5 . . ? H33B C40 H33C 109.5 . . ? C39 C41 H34A 109.5 . . ? C39 C41 H34B 109.5 . . ? H34A C41 H34B 109.5 . . ? C39 C41 H34C 109.5 . . ? H34A C41 H34C 109.5 . . ? H34B C41 H34C 109.5 . . ? C37 C42 S4 115.6(5) . . ? C37 C42 S3 114.4(5) . . ? S4 C42 S3 130.0(5) . . ? C45 C43 H49A 109.5 . . ? C45 C43 H49B 109.5 . . ? H49A C43 H49B 109.5 . . ? C45 C43 H49C 109.5 . . ? H49A C43 H49C 109.5 . . ? H49B C43 H49C 109.5 . . ? C45 C44 H50A 109.5 . . ? C45 C44 H50B 109.5 . . ? H50A C44 H50B 109.5 . . ? C45 C44 H50C 109.5 . . ? H50A C44 H50C 109.5 . . ? H50B C44 H50C 109.5 . . ? N9 C45 C43 110.8(7) . . ? N9 C45 C44 108.5(7) . . ? C43 C45 C44 113.3(8) . . ? N9 C45 H48 108.0 . . ? C43 C45 H48 108.0 . . ? C44 C45 H48 108.0 . . ? C47 C46 N9 107.3(7) . . ? C47 C46 H47 126.4 . . ? N9 C46 H47 126.4 . . ? C46 C47 N10 106.1(6) . . ? C46 C47 H46 126.9 . . ? N10 C47 H46 126.9 . . ? N9 C48 N10 102.9(5) . . ? N9 C48 Sc2 133.3(5) . . ? N10 C48 Sc2 121.7(5) . . ? N10 C49 C50 112.8(6) . . ? N10 C49 H45A 109.0 . . ? C50 C49 H45A 109.0 . . ? N10 C49 H45B 109.0 . . ? C50 C49 H45B 109.0 . . ? H45A C49 H45B 107.8 . . ? O5 C50 C52 110.1(7) . . ? O5 C50 C49 109.1(6) . . ? C52 C50 C49 110.8(6) . . ? O5 C50 C51 109.2(6) . . ? C52 C50 C51 110.3(8) . . ? C49 C50 C51 107.3(7) . . ? C50 C51 H44A 109.5 . . ? C50 C51 H44B 109.5 . . ? H44A C51 H44B 109.5 . . ? C50 C51 H44C 109.5 . . ? H44A C51 H44C 109.5 . . ? H44B C51 H44C 109.5 . . ? C50 C52 H43A 109.5 . . ? C50 C52 H43B 109.5 . . ? H43A C52 H43B 109.5 . . ? C50 C52 H43C 109.5 . . ? H43A C52 H43C 109.5 . . ? H43B C52 H43C 109.5 . . ? C55 C53 H59A 109.5 . . ? C55 C53 H59B 109.5 . . ? H59A C53 H59B 109.5 . . ? C55 C53 H59C 109.5 . . ? H59A C53 H59C 109.5 . . ? H59B C53 H59C 109.5 . . ? C55 C54 H60A 109.5 . . ? C55 C54 H60B 109.5 . . ? H60A C54 H60B 109.5 . . ? C55 C54 H60C 109.5 . . ? H60A C54 H60C 109.5 . . ? H60B C54 H60C 109.5 . . ? N11 C55 C53 110.4(7) . . ? N11 C55 C54 110.0(7) . . ? C53 C55 C54 111.0(7) . . ? N11 C55 H58 108.5 . . ? C53 C55 H58 108.5 . . ? C54 C55 H58 108.5 . . ? C57 C56 N11 107.0(8) . . ? C57 C56 H57 126.5 . . ? N11 C56 H57 126.5 . . ? C56 C57 N12 105.6(7) . . ? C56 C57 H56 127.2 . . ? N12 C57 H56 127.2 . . ? N11 C58 N12 104.2(6) . . ? N11 C58 Sc2 136.5(5) . . ? N12 C58 Sc2 117.0(5) . . ? N12 C59 C60 112.9(7) . . ? N12 C59 H55A 109.0 . . ? C60 C59 H55A 109.0 . . ? N12 C59 H55B 109.0 . . ? C60 C59 H55B 109.0 . . ? H55A C59 H55B 107.8 . . ? O6 C60 C62 109.2(7) . . ? O6 C60 C61 109.1(8) . . ? C62 C60 C61 111.2(8) . . ? O6 C60 C59 107.8(7) . . ? C62 C60 C59 108.9(8) . . ? C61 C60 C59 110.6(8) . . ? C60 C61 H54A 109.5 . . ? C60 C61 H54B 109.5 . . ? H54A C61 H54B 109.5 . . ? C60 C61 H54C 109.5 . . ? H54A C61 H54C 109.5 . . ? H54B C61 H54C 109.5 . . ? C60 C62 H53A 109.5 . . ? C60 C62 H53B 109.5 . . ? H53A C62 H53B 109.5 . . ? C60 C62 H53C 109.5 . . ? H53A C62 H53C 109.5 . . ? H53B C62 H53C 109.5 . . ? C64 C63 C65 121.1(15) . 3_766 ? C64 C63 H63 119.5 . . ? C65 C63 H63 119.5 3_766 . ? C63 C64 C65 119.5(13) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? C64 C65 C63 119.4(13) . 3_766 ? C64 C65 H65 120.3 . . ? C63 C65 H65 120.3 3_766 . ? C67 C66 C68 118.3(10) . 3_665 ? C67 C66 H66 120.8 . . ? C68 C66 H66 120.8 3_665 . ? C66 C67 C68 120.6(10) . . ? C66 C67 H67 119.7 . . ? C68 C67 H67 119.7 . . ? C66 C68 C67 121.0(11) 3_665 . ? C66 C68 H68 119.5 3_665 . ? C67 C68 H68 119.5 . . ? C71 C69 C70 117.5(14) 3_577 . ? C71 C69 H69 121.2 3_577 . ? C70 C69 H69 121.2 . . ? C71 C70 C69 122.4(13) . . ? C71 C70 H70 118.8 . . ? C69 C70 H70 118.8 . . ? C70 C71 C69 120.1(15) . 3_577 ? C70 C71 H71 119.9 . . ? C69 C71 H71 119.9 3_577 . ? C73 C72 C74 114.5(18) . 3_567 ? C73 C72 H72 122.8 . . ? C74 C72 H72 122.8 3_567 . ? C74 C73 C72 119(3) . . ? C74 C73 H73 120.3 . . ? C72 C73 H73 120.3 . . ? C73 C74 C72 126(2) . 3_567 ? C73 C74 H74 116.9 . . ? C72 C74 H74 116.9 3_567 . ? C6 N1 C4 107.7(6) . . ? C6 N1 C3 127.0(7) . . ? C4 N1 C3 125.3(6) . . ? C6 N2 C5 108.5(6) . . ? C6 N2 C7 124.9(7) . . ? C5 N2 C7 126.5(7) . . ? C17 N3 C15 111.4(8) . . ? C17 N3 C14 122.8(6) . . ? C15 N3 C14 125.7(8) . . ? C17 N4 C16 111.1(8) . . ? C17 N4 C18 122.5(7) . . ? C16 N4 C18 126.2(8) . . ? C27 N5 C25 110.4(7) . . ? C27 N5 C24 124.3(6) . . ? C25 N5 C24 125.2(7) . . ? C26 N6 C27 111.7(7) . . ? C26 N6 C28 124.3(7) . . ? C27 N6 C28 124.0(6) . . ? C37 N7 C35 109.5(6) . . ? C37 N7 C34 125.1(7) . . ? C35 N7 C34 125.5(7) . . ? C37 N8 C36 109.1(6) . . ? C37 N8 C38 125.0(6) . . ? C36 N8 C38 125.8(6) . . ? C48 N9 C46 111.4(7) . . ? C48 N9 C45 122.9(6) . . ? C46 N9 C45 125.6(7) . . ? C48 N10 C47 112.3(6) . . ? C48 N10 C49 124.4(5) . . ? C47 N10 C49 123.3(6) . . ? C58 N11 C56 112.4(8) . . ? C58 N11 C55 123.8(6) . . ? C56 N11 C55 123.7(7) . . ? C58 N12 C57 110.8(7) . . ? C58 N12 C59 123.7(6) . . ? C57 N12 C59 125.4(7) . . ? C8 O1 Sc1 147.4(5) . . ? C19 O2 Sc1 139.7(5) . . ? C29 O3 Sc1 140.7(5) . . ? C39 O4 Sc2 147.7(5) . . ? C50 O5 Sc2 140.0(5) . . ? C60 O6 Sc2 139.9(5) . . ? O1 Sc1 O3 107.0(3) . . ? O1 Sc1 O2 111.1(3) . . ? O3 Sc1 O2 141.9(3) . . ? O1 Sc1 C17 103.1(2) . . ? O3 Sc1 C17 92.1(3) . . ? O2 Sc1 C17 80.2(2) . . ? O1 Sc1 C27 105.2(3) . . ? O3 Sc1 C27 81.3(3) . . ? O2 Sc1 C27 88.1(2) . . ? C17 Sc1 C27 151.7(3) . . ? O4 Sc2 O5 107.3(2) . . ? O4 Sc2 O6 112.5(3) . . ? O5 Sc2 O6 140.2(3) . . ? O4 Sc2 C58 101.6(2) . . ? O5 Sc2 C58 92.9(2) . . ? O6 Sc2 C58 80.5(2) . . ? O4 Sc2 C48 102.3(2) . . ? O5 Sc2 C48 80.9(2) . . ? O6 Sc2 C48 89.5(2) . . ? C58 Sc2 C48 156.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C4 C5 N2 -0.3(8) . . . . ? N2 C7 C8 O1 61.2(8) . . . . ? N2 C7 C8 C10 -177.5(7) . . . . ? N2 C7 C8 C9 -59.6(9) . . . . ? N2 C6 C11 S1 -105.9(7) . . . . ? N1 C6 C11 S1 73.6(8) . . . . ? N2 C6 C11 S2 76.0(8) . . . . ? N1 C6 C11 S2 -104.6(7) . . . . ? N3 C15 C16 N4 0.0(10) . . . . ? N4 C18 C19 O2 61.0(10) . . . . ? N4 C18 C19 C21 -179.2(8) . . . . ? N4 C18 C19 C20 -58.2(10) . . . . ? N5 C25 C26 N6 -2.6(12) . . . . ? N6 C28 C29 O3 64.3(10) . . . . ? N6 C28 C29 C30 -56.6(10) . . . . ? N6 C28 C29 C31 -179.9(8) . . . . ? N7 C35 C36 N8 1.0(8) . . . . ? N8 C38 C39 O4 -62.1(8) . . . . ? N8 C38 C39 C40 59.6(9) . . . . ? N8 C38 C39 C41 178.7(6) . . . . ? N7 C37 C42 S4 -74.8(8) . . . . ? N8 C37 C42 S4 103.3(7) . . . . ? N7 C37 C42 S3 104.1(7) . . . . ? N8 C37 C42 S3 -77.7(8) . . . . ? N9 C46 C47 N10 0.2(10) . . . . ? N10 C49 C50 O5 -65.2(8) . . . . ? N10 C49 C50 C52 56.1(8) . . . . ? N10 C49 C50 C51 176.6(7) . . . . ? N11 C56 C57 N12 2.2(9) . . . . ? N12 C59 C60 O6 -62.7(10) . . . . ? N12 C59 C60 C62 178.9(7) . . . . ? N12 C59 C60 C61 56.4(10) . . . . ? C65 C63 C64 C65 2(2) 3_766 . . . ? C63 C64 C65 C63 -2(2) . . . 3_766 ? C68 C66 C67 C68 1.5(18) 3_665 . . . ? C66 C67 C68 C66 -1.5(18) . . . 3_665 ? C71 C69 C70 C71 1(3) 3_577 . . . ? C69 C70 C71 C69 -1(4) . . . 3_577 ? C74 C72 C73 C74 -1(3) 3_567 . . . ? C72 C73 C74 C72 1(4) . . . 3_567 ? N2 C6 N1 C4 -2.1(7) . . . . ? C11 C6 N1 C4 178.4(6) . . . . ? N2 C6 N1 C3 178.9(7) . . . . ? C11 C6 N1 C3 -0.6(11) . . . . ? C5 C4 N1 C6 1.5(8) . . . . ? C5 C4 N1 C3 -179.5(7) . . . . ? C2 C3 N1 C6 118.3(8) . . . . ? C1 C3 N1 C6 -115.8(8) . . . . ? C2 C3 N1 C4 -60.6(10) . . . . ? C1 C3 N1 C4 65.4(9) . . . . ? N1 C6 N2 C5 1.9(7) . . . . ? C11 C6 N2 C5 -178.6(6) . . . . ? N1 C6 N2 C7 -179.9(6) . . . . ? C11 C6 N2 C7 -0.5(10) . . . . ? C4 C5 N2 C6 -1.0(8) . . . . ? C4 C5 N2 C7 -179.1(6) . . . . ? C8 C7 N2 C6 116.5(8) . . . . ? C8 C7 N2 C5 -65.8(9) . . . . ? N4 C17 N3 C15 -2.1(8) . . . . ? Sc1 C17 N3 C15 157.4(6) . . . . ? N4 C17 N3 C14 -179.1(6) . . . . ? Sc1 C17 N3 C14 -19.6(12) . . . . ? C16 C15 N3 C17 1.4(10) . . . . ? C16 C15 N3 C14 178.3(7) . . . . ? C12 C14 N3 C17 114.0(8) . . . . ? C13 C14 N3 C17 -124.4(8) . . . . ? C12 C14 N3 C15 -62.6(10) . . . . ? C13 C14 N3 C15 59.0(10) . . . . ? N3 C17 N4 C16 2.1(9) . . . . ? Sc1 C17 N4 C16 -162.2(6) . . . . ? N3 C17 N4 C18 177.5(7) . . . . ? Sc1 C17 N4 C18 13.2(10) . . . . ? C15 C16 N4 C17 -1.4(10) . . . . ? C15 C16 N4 C18 -176.5(8) . . . . ? C19 C18 N4 C17 -65.9(11) . . . . ? C19 C18 N4 C16 108.7(9) . . . . ? N6 C27 N5 C25 -1.8(10) . . . . ? Sc1 C27 N5 C25 162.1(7) . . . . ? N6 C27 N5 C24 -178.9(9) . . . . ? Sc1 C27 N5 C24 -15.0(14) . . . . ? C26 C25 N5 C27 2.9(12) . . . . ? C26 C25 N5 C24 179.9(9) . . . . ? C22 C24 N5 C27 117.1(10) . . . . ? C23 C24 N5 C27 -118.5(10) . . . . ? C22 C24 N5 C25 -59.6(13) . . . . ? C23 C24 N5 C25 64.8(13) . . . . ? C25 C26 N6 C27 1.6(11) . . . . ? C25 C26 N6 C28 -177.6(8) . . . . ? N5 C27 N6 C26 0.2(10) . . . . ? Sc1 C27 N6 C26 -166.3(6) . . . . ? N5 C27 N6 C28 179.3(8) . . . . ? Sc1 C27 N6 C28 12.8(11) . . . . ? C29 C28 N6 C26 124.9(9) . . . . ? C29 C28 N6 C27 -54.2(11) . . . . ? N8 C37 N7 C35 0.5(7) . . . . ? C42 C37 N7 C35 179.0(6) . . . . ? N8 C37 N7 C34 -178.9(8) . . . . ? C42 C37 N7 C34 -0.4(12) . . . . ? C36 C35 N7 C37 -0.9(8) . . . . ? C36 C35 N7 C34 178.4(9) . . . . ? C33 C34 N7 C37 -123.4(11) . . . . ? C32 C34 N7 C37 112.3(9) . . . . ? C33 C34 N7 C35 57.4(14) . . . . ? C32 C34 N7 C35 -67.0(12) . . . . ? N7 C37 N8 C36 0.1(7) . . . . ? C42 C37 N8 C36 -178.3(6) . . . . ? N7 C37 N8 C38 -176.8(6) . . . . ? C42 C37 N8 C38 4.7(10) . . . . ? C35 C36 N8 C37 -0.7(7) . . . . ? C35 C36 N8 C38 176.2(6) . . . . ? C39 C38 N8 C37 -113.3(7) . . . . ? C39 C38 N8 C36 70.2(9) . . . . ? N10 C48 N9 C46 0.0(9) . . . . ? Sc2 C48 N9 C46 -163.0(6) . . . . ? N10 C48 N9 C45 177.3(7) . . . . ? Sc2 C48 N9 C45 14.3(12) . . . . ? C47 C46 N9 C48 -0.1(10) . . . . ? C47 C46 N9 C45 -177.4(8) . . . . ? C43 C45 N9 C48 122.6(8) . . . . ? C44 C45 N9 C48 -112.4(8) . . . . ? C43 C45 N9 C46 -60.5(11) . . . . ? C44 C45 N9 C46 64.5(11) . . . . ? N9 C48 N10 C47 0.2(8) . . . . ? Sc2 C48 N10 C47 165.7(5) . . . . ? N9 C48 N10 C49 -178.9(6) . . . . ? Sc2 C48 N10 C49 -13.4(9) . . . . ? C46 C47 N10 C48 -0.3(9) . . . . ? C46 C47 N10 C49 178.8(7) . . . . ? C50 C49 N10 C48 52.6(9) . . . . ? C50 C49 N10 C47 -126.4(7) . . . . ? N12 C58 N11 C56 0.9(8) . . . . ? Sc2 C58 N11 C56 -160.0(6) . . . . ? N12 C58 N11 C55 177.0(6) . . . . ? Sc2 C58 N11 C55 16.1(11) . . . . ? C57 C56 N11 C58 -2.0(9) . . . . ? C57 C56 N11 C55 -178.1(7) . . . . ? C53 C55 N11 C58 -108.2(8) . . . . ? C54 C55 N11 C58 129.0(7) . . . . ? C53 C55 N11 C56 67.6(9) . . . . ? C54 C55 N11 C56 -55.3(9) . . . . ? N11 C58 N12 C57 0.6(8) . . . . ? Sc2 C58 N12 C57 165.9(5) . . . . ? N11 C58 N12 C59 -175.9(7) . . . . ? Sc2 C58 N12 C59 -10.6(10) . . . . ? C56 C57 N12 C58 -1.8(9) . . . . ? C56 C57 N12 C59 174.6(7) . . . . ? C60 C59 N12 C58 63.5(10) . . . . ? C60 C59 N12 C57 -112.4(8) . . . . ? C10 C8 O1 Sc1 -19.2(13) . . . . ? C7 C8 O1 Sc1 97.6(10) . . . . ? C9 C8 O1 Sc1 -141.9(8) . . . . ? C21 C19 O2 Sc1 -122.3(9) . . . . ? C20 C19 O2 Sc1 117.3(9) . . . . ? C18 C19 O2 Sc1 -3.4(14) . . . . ? C30 C29 O3 Sc1 79.8(11) . . . . ? C28 C29 O3 Sc1 -42.0(14) . . . . ? C31 C29 O3 Sc1 -157.3(9) . . . . ? C40 C39 O4 Sc2 148.3(7) . . . . ? C41 C39 O4 Sc2 25.8(12) . . . . ? C38 C39 O4 Sc2 -90.6(10) . . . . ? C52 C50 O5 Sc2 -73.2(9) . . . . ? C49 C50 O5 Sc2 48.5(11) . . . . ? C51 C50 O5 Sc2 165.5(7) . . . . ? C62 C60 O6 Sc2 128.7(8) . . . . ? C61 C60 O6 Sc2 -109.5(9) . . . . ? C59 C60 O6 Sc2 10.6(13) . . . . ? C8 O1 Sc1 O3 -129.7(9) . . . . ? C8 O1 Sc1 O2 49.5(10) . . . . ? C8 O1 Sc1 C17 133.9(9) . . . . ? C8 O1 Sc1 C27 -44.3(10) . . . . ? C29 O3 Sc1 O1 110.5(10) . . . . ? C29 O3 Sc1 O2 -68.4(11) . . . . ? C29 O3 Sc1 C17 -145.2(10) . . . . ? C29 O3 Sc1 C27 7.2(10) . . . . ? C19 O2 Sc1 O1 68.1(10) . . . . ? C19 O2 Sc1 O3 -113.1(10) . . . . ? C19 O2 Sc1 C17 -32.3(10) . . . . ? C19 O2 Sc1 C27 173.6(10) . . . . ? N3 C17 Sc1 O1 118.8(8) . . . . ? N4 C17 Sc1 O1 -83.6(6) . . . . ? N3 C17 Sc1 O3 10.8(8) . . . . ? N4 C17 Sc1 O3 168.4(6) . . . . ? N3 C17 Sc1 O2 -131.7(8) . . . . ? N4 C17 Sc1 O2 25.9(6) . . . . ? N3 C17 Sc1 C27 -64.7(10) . . . . ? N4 C17 Sc1 C27 92.8(8) . . . . ? N5 C27 Sc1 O1 103.2(9) . . . . ? N6 C27 Sc1 O1 -95.2(7) . . . . ? N5 C27 Sc1 O3 -151.4(9) . . . . ? N6 C27 Sc1 O3 10.2(7) . . . . ? N5 C27 Sc1 O2 -8.1(9) . . . . ? N6 C27 Sc1 O2 153.5(7) . . . . ? N5 C27 Sc1 C17 -73.2(11) . . . . ? N6 C27 Sc1 C17 88.4(8) . . . . ? C39 O4 Sc2 O5 122.8(9) . . . . ? C39 O4 Sc2 O6 -56.0(9) . . . . ? C39 O4 Sc2 C58 -140.4(9) . . . . ? C39 O4 Sc2 C48 38.6(9) . . . . ? C50 O5 Sc2 O4 -113.3(8) . . . . ? C50 O5 Sc2 O6 64.9(9) . . . . ? C50 O5 Sc2 C58 143.5(8) . . . . ? C50 O5 Sc2 C48 -13.3(8) . . . . ? C60 O6 Sc2 O4 -73.0(9) . . . . ? C60 O6 Sc2 O5 108.9(9) . . . . ? C60 O6 Sc2 C58 25.8(9) . . . . ? C60 O6 Sc2 C48 -176.0(9) . . . . ? N11 C58 Sc2 O4 -114.9(7) . . . . ? N12 C58 Sc2 O4 85.9(6) . . . . ? N11 C58 Sc2 O5 -6.6(7) . . . . ? N12 C58 Sc2 O5 -165.8(6) . . . . ? N11 C58 Sc2 O6 133.8(8) . . . . ? N12 C58 Sc2 O6 -25.3(5) . . . . ? N11 C58 Sc2 C48 67.3(10) . . . . ? N12 C58 Sc2 C48 -91.8(8) . . . . ? N9 C48 Sc2 O4 -101.5(7) . . . . ? N10 C48 Sc2 O4 98.1(6) . . . . ? N9 C48 Sc2 O5 152.6(7) . . . . ? N10 C48 Sc2 O5 -7.8(5) . . . . ? N9 C48 Sc2 O6 11.4(7) . . . . ? N10 C48 Sc2 O6 -149.0(6) . . . . ? N9 C48 Sc2 C58 76.2(10) . . . . ? N10 C48 Sc2 C58 -84.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 76.57 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 2.186 _refine_diff_density_min -1.208 _refine_diff_density_rms 0.139 _database_code_depnum_ccdc_archive 'CCDC 954362' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_po2003 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H168 N12 O12 S8 Sc2' _chemical_formula_weight 2148.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.3119 1.5331 '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 15.0794(14) _cell_length_b 15.1041(11) _cell_length_c 15.2673(13) _cell_angle_alpha 72.737(7) _cell_angle_beta 60.940(9) _cell_angle_gamma 84.799(7) _cell_volume 2896.7(4) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 12248 _cell_measurement_theta_min 3.0672 _cell_measurement_theta_max 66.9633 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.6616 _exptl_crystal_size_mid 0.1615 _exptl_crystal_size_min 0.0900 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1154 _exptl_absorpt_coefficient_mu 2.835 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.227 _exptl_absorpt_correction_T_max 0.669 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3147 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49523 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 67.10 _reflns_number_total 10330 _reflns_number_gt 8186 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ortep _computing_publication_material mercury _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1584P)^2^+2.2665P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10330 _refine_ls_number_parameters 631 _refine_ls_number_restraints 165 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2433 _refine_ls_wR_factor_gt 0.2224 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.059 _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 C1 C 0.2783(4) 0.6282(3) 0.3884(4) 0.0547(10) Uani 1 1 d . . . H1A H 0.3515 0.6333 0.3397 0.082 Uiso 1 1 calc R . . H1B H 0.2640 0.5819 0.4550 0.082 Uiso 1 1 calc R . . H1C H 0.2566 0.6886 0.4007 0.082 Uiso 1 1 calc R . . C2 C 0.1070(3) 0.5947(3) 0.4125(3) 0.0487(9) Uani 1 1 d . . . H2A H 0.0872 0.6550 0.4257 0.073 Uiso 1 1 calc R . . H2B H 0.0880 0.5465 0.4791 0.073 Uiso 1 1 calc R . . H2C H 0.0721 0.5798 0.3781 0.073 Uiso 1 1 calc R . . C3 C 0.2211(3) 0.5988(2) 0.3422(3) 0.0405(8) Uani 1 1 d . . . H3 H 0.2402 0.5349 0.3361 0.049 Uiso 1 1 calc R . . C4 C 0.2184(3) 0.7487(3) 0.2144(3) 0.0506(10) Uani 1 1 d . . . H4 H 0.1693 0.7778 0.2636 0.061 Uiso 1 1 calc R . . C5 C 0.2688(4) 0.7845(3) 0.1096(4) 0.0559(11) Uani 1 1 d . . . H5 H 0.2625 0.8443 0.0704 0.067 Uiso 1 1 calc R . . C6 C 0.3225(3) 0.6405(2) 0.1480(3) 0.0418(8) Uani 1 1 d . . . C7 C 0.3965(3) 0.7266(3) -0.0416(3) 0.0499(10) Uani 1 1 d . . . H7A H 0.4042 0.7930 -0.0816 0.060 Uiso 1 1 calc R . . H7B H 0.3622 0.6923 -0.0641 0.060 Uiso 1 1 calc R . . C8 C 0.5031(3) 0.6904(2) -0.0695(3) 0.0433(8) Uani 1 1 d . . . C9 C 0.5648(3) 0.7236(3) -0.1883(3) 0.0480(9) Uani 1 1 d . . . H9A H 0.6331 0.7006 -0.2108 0.072 Uiso 1 1 calc R . . H9B H 0.5700 0.7917 -0.2121 0.072 Uiso 1 1 calc R . . H9C H 0.5312 0.6999 -0.2187 0.072 Uiso 1 1 calc R . . C10 C 0.5520(3) 0.7299(3) -0.0211(4) 0.0500(9) Uani 1 1 d . . . H10A H 0.5110 0.7090 0.0554 0.075 Uiso 1 1 calc R . . H10B H 0.5558 0.7979 -0.0456 0.075 Uiso 1 1 calc R . . H10C H 0.6207 0.7083 -0.0419 0.075 Uiso 1 1 calc R . . C11 C 0.3096(4) 0.0776(3) 0.6216(4) 0.0649(12) Uani 1 1 d . . . H11A H 0.3093 0.1137 0.6656 0.097 Uiso 1 1 calc R . . H11B H 0.3154 0.0118 0.6521 0.097 Uiso 1 1 calc R . . H11C H 0.2463 0.0850 0.6177 0.097 Uiso 1 1 calc R . . C12 C 0.4029(4) 0.0622(3) 0.4380(4) 0.0593(11) Uani 1 1 d . . . H12A H 0.3460 0.0792 0.4236 0.089 Uiso 1 1 calc R . . H12B H 0.3981 -0.0052 0.4697 0.089 Uiso 1 1 calc R . . H12C H 0.4672 0.0803 0.3723 0.089 Uiso 1 1 calc R . . C13 C 0.3988(4) 0.1120(3) 0.5130(4) 0.0528(10) Uani 1 1 d . . . H13 H 0.4627 0.1011 0.5184 0.063 Uiso 1 1 calc R . . C14 C 0.3156(3) 0.2558(3) 0.4568(3) 0.0437(8) Uani 1 1 d . . . H14 H 0.2543 0.2257 0.4736 0.052 Uiso 1 1 calc R . . C15 C 0.3403(3) 0.3469(3) 0.4174(3) 0.0437(8) Uani 1 1 d . . . H15 H 0.2996 0.3934 0.4008 0.052 Uiso 1 1 calc R . . C16 C 0.4682(3) 0.2791(3) 0.4370(3) 0.0429(8) Uani 1 1 d . . . C17 C 0.5649(3) 0.2622(3) 0.4401(4) 0.0502(10) Uani 1 1 d . . . C18 C 0.4882(3) 0.4537(3) 0.3645(3) 0.0452(9) Uani 1 1 d . . . H18A H 0.5424 0.4486 0.3843 0.054 Uiso 1 1 calc R . . H18B H 0.4396 0.4973 0.3980 0.054 Uiso 1 1 calc R . . C19 C 0.5358(3) 0.4939(3) 0.2453(3) 0.0459(9) Uani 1 1 d . . . C20 C 0.6240(3) 0.4375(3) 0.1896(4) 0.0565(10) Uani 1 1 d . . . H20A H 0.5998 0.3724 0.2128 0.085 Uiso 1 1 calc R . . H20B H 0.6780 0.4419 0.2066 0.085 Uiso 1 1 calc R . . H20C H 0.6506 0.4622 0.1138 0.085 Uiso 1 1 calc R . . C21 C 0.5766(4) 0.5937(3) 0.2170(4) 0.0572(11) Uani 1 1 d . . . H21A H 0.6124 0.6203 0.1407 0.086 Uiso 1 1 calc R . . H21B H 0.6237 0.5931 0.2443 0.086 Uiso 1 1 calc R . . H21C H 0.5198 0.6314 0.2480 0.086 Uiso 1 1 calc R . . C22 C -0.2267(3) 0.1097(3) 0.5754(4) 0.0551(10) Uani 1 1 d . . . H22A H -0.2199 0.1418 0.6192 0.083 Uiso 1 1 calc R . . H22B H -0.2516 0.0450 0.6160 0.083 Uiso 1 1 calc R . . H22C H -0.2750 0.1407 0.5526 0.083 Uiso 1 1 calc R . . C23 C -0.1297(4) 0.0725(3) 0.4024(4) 0.0542(10) Uani 1 1 d . . . H23A H -0.1789 0.1052 0.3820 0.081 Uiso 1 1 calc R . . H23B H -0.1511 0.0062 0.4346 0.081 Uiso 1 1 calc R . . H23C H -0.0625 0.0805 0.3403 0.081 Uiso 1 1 calc R . . C24 C -0.1243(3) 0.1121(2) 0.4806(3) 0.0437(8) Uani 1 1 d . . . H24 H -0.0779 0.0748 0.5049 0.052 Uiso 1 1 calc R . . C25 C -0.1237(3) 0.2828(3) 0.3848(3) 0.0456(9) Uani 1 1 d . . . H25 H -0.1876 0.2805 0.3872 0.055 Uiso 1 1 calc R . . C26 C -0.0583(3) 0.3577(2) 0.3403(3) 0.0416(8) Uani 1 1 d . . . H26 H -0.0676 0.4183 0.3055 0.050 Uiso 1 1 calc R . . C27 C 0.0093(3) 0.2394(2) 0.4081(3) 0.0381(8) Uani 1 1 d . . . C28 C 0.1178(3) 0.3873(2) 0.3146(3) 0.0406(8) Uani 1 1 d . . . H28A H 0.1616 0.3496 0.3413 0.049 Uiso 1 1 calc R . . H28B H 0.0988 0.4406 0.3440 0.049 Uiso 1 1 calc R . . C29 C 0.1808(3) 0.4250(2) 0.1942(3) 0.0415(8) Uani 1 1 d . . . C30 C 0.1822(3) 0.3523(3) 0.1420(3) 0.0503(9) Uani 1 1 d . . . H30A H 0.2294 0.3746 0.0667 0.075 Uiso 1 1 calc R . . H30B H 0.1138 0.3419 0.1533 0.075 Uiso 1 1 calc R . . H30C H 0.2043 0.2940 0.1727 0.075 Uiso 1 1 calc R . . C31 C 0.1412(3) 0.5152(3) 0.1511(3) 0.0476(9) Uani 1 1 d . . . H31A H 0.1412 0.5615 0.1845 0.071 Uiso 1 1 calc R . . H31B H 0.0718 0.5029 0.1660 0.071 Uiso 1 1 calc R . . H31C H 0.1853 0.5388 0.0753 0.071 Uiso 1 1 calc R . . C32 C 0.0768(3) 0.1840(2) 0.4460(3) 0.0408(8) Uani 1 1 d . . . C33 C 0.7792(6) 0.5815(5) 0.3238(7) 0.097(2) Uani 1 1 d . . . H33A H 0.7221 0.5572 0.3956 0.116 Uiso 1 1 calc R . . H33B H 0.7775 0.5460 0.2795 0.116 Uiso 1 1 calc R . . C34 C 0.7702(6) 0.6816(4) 0.2808(6) 0.090(2) Uani 1 1 d . . . H34A H 0.7665 0.6928 0.2154 0.109 Uiso 1 1 calc R . . H34B H 0.7082 0.7035 0.3319 0.109 Uiso 1 1 calc R . . C35 C 0.8619(5) 0.7302(4) 0.2599(6) 0.0804(16) Uani 1 1 d . . . H35A H 0.9042 0.7609 0.1841 0.097 Uiso 1 1 calc R . . H35B H 0.8436 0.7774 0.2981 0.097 Uiso 1 1 calc R . . C36 C 0.9151(7) 0.6565(5) 0.2980(9) 0.116(3) Uani 1 1 d . . . H36A H 0.9866 0.6598 0.2426 0.140 Uiso 1 1 calc R . . H36B H 0.9151 0.6661 0.3593 0.140 Uiso 1 1 calc R . . C37 C 0.4401(8) 0.9781(7) 0.1501(10) 0.164(3) Uani 1 1 d DU . . H37A H 0.4243 0.9867 0.0923 0.196 Uiso 1 1 calc R . . H37B H 0.3794 0.9913 0.2103 0.196 Uiso 1 1 calc R . . C38 C 0.4685(9) 0.8841(6) 0.1801(8) 0.143(3) Uani 1 1 d DU . . H38A H 0.4086 0.8407 0.2325 0.172 Uiso 1 1 calc R . . H38B H 0.5094 0.8604 0.1189 0.172 Uiso 1 1 calc R . . C39 C 0.5279(10) 0.9014(7) 0.2241(10) 0.169(3) Uani 1 1 d DU . . H39A H 0.4839 0.8983 0.2987 0.203 Uiso 1 1 calc R . . H39B H 0.5795 0.8548 0.2190 0.203 Uiso 1 1 calc R . . C40 C 0.5753(10) 0.9911(7) 0.1656(10) 0.164(3) Uani 1 1 d DU . . H40A H 0.5757 1.0246 0.2122 0.197 Uiso 1 1 calc R . . H40B H 0.6464 0.9874 0.1127 0.197 Uiso 1 1 calc R . . C45 C 0.8078(5) 0.9020(4) 0.8878(6) 0.140(3) Uani 1 1 d GU . . H45 H 0.7760 0.8677 0.8663 0.168 Uiso 1 1 calc R . . C46 C 0.8662(5) 0.9836(4) 0.8186(4) 0.107(2) Uani 1 1 d GU . . H46 H 0.8745 1.0050 0.7497 0.129 Uiso 1 1 calc R . . C47 C 0.9126(5) 1.0337(4) 0.8500(5) 0.121(2) Uani 1 1 d GU . . H47 H 0.9526 1.0895 0.8027 0.145 Uiso 1 1 calc R . . C48 C 0.9006(6) 1.0023(5) 0.9507(6) 0.153(3) Uani 1 1 d GU . . H48 H 0.9323 1.0366 0.9722 0.184 Uiso 1 1 calc R . . C49 C 0.8421(7) 0.9207(6) 1.0199(4) 0.173(3) Uani 1 1 d GU . . H49 H 0.8338 0.8993 1.0888 0.208 Uiso 1 1 calc R . . C50 C 0.7957(6) 0.8706(4) 0.9885(5) 0.171(3) Uani 1 1 d GU . . H50 H 0.7557 0.8148 1.0358 0.206 Uiso 1 1 calc R . . N1 N 0.2525(2) 0.6612(2) 0.2361(3) 0.0414(7) Uani 1 1 d . . . N2 N 0.3317(3) 0.7174(2) 0.0697(3) 0.0468(8) Uani 1 1 d . . . N3 N 0.3959(2) 0.2135(2) 0.4684(3) 0.0435(7) Uani 1 1 d . . . N4 N 0.4347(2) 0.3619(2) 0.4051(3) 0.0404(7) Uani 1 1 d . . . N5 N -0.0800(2) 0.2096(2) 0.4265(3) 0.0414(7) Uani 1 1 d . . . N6 N 0.0246(2) 0.3303(2) 0.3544(2) 0.0377(6) Uani 1 1 d . . . O1 O 0.49611(19) 0.59058(16) -0.0328(2) 0.0390(5) Uani 1 1 d . . . O2 O 0.4621(2) 0.49462(18) 0.2152(2) 0.0444(6) Uani 1 1 d . . . O3 O 0.2790(2) 0.44301(17) 0.1754(2) 0.0461(6) Uani 1 1 d . . . O4 O 0.8717(5) 0.5723(3) 0.3253(6) 0.127(2) Uani 1 1 d . . . O5 O 0.5212(7) 1.0355(5) 0.1185(7) 0.165(3) Uani 1 1 d DU . . S1 S 0.64961(9) 0.20890(8) 0.35543(11) 0.0628(3) Uani 1 1 d . . . S2 S 0.57327(11) 0.29925(10) 0.52865(12) 0.0723(4) Uani 1 1 d . . . S3 S 0.17299(8) 0.13841(7) 0.36114(8) 0.0481(3) Uani 1 1 d . . . S4 S 0.04600(8) 0.17900(7) 0.56908(8) 0.0469(3) Uani 1 1 d . . . Sc1 Sc 0.41057(5) 0.50348(4) 0.11890(5) 0.0362(2) Uani 1 1 d . . . O6 O 0.9506(9) 1.2386(12) 1.0168(9) 0.287(5) Uani 1 1 d DU . . C52 C 0.7972(11) 1.1526(14) 1.1076(11) 0.260(6) Uani 1 1 d DU . . H52A H 0.7324 1.1744 1.1545 0.312 Uiso 1 1 calc R . . H52B H 0.7826 1.1024 1.0860 0.312 Uiso 1 1 calc R . . C53 C 0.8584(12) 1.1226(15) 1.1562(12) 0.260(6) Uani 1 1 d DU . . H53A H 0.8907 1.0653 1.1399 0.312 Uiso 1 1 calc R . . H53B H 0.8157 1.1081 1.2331 0.312 Uiso 1 1 calc R . . C54 C 0.9353(13) 1.1939(15) 1.1193(11) 0.274(6) Uani 1 1 d DU . . H54A H 0.9112 1.2371 1.1629 0.329 Uiso 1 1 calc R . . H54B H 0.9982 1.1673 1.1181 0.329 Uiso 1 1 calc R . . C51 C 0.8597(12) 1.2270(15) 1.0190(13) 0.276(6) Uani 1 1 d DU . . H51A H 0.8733 1.2136 0.9541 0.331 Uiso 1 1 calc R . . H51B H 0.8237 1.2851 1.0221 0.331 Uiso 1 1 calc R . . C56 C 0.0267(14) 0.4089(10) 0.9911(15) 0.414(13) Uani 1 1 d DU . . H56 H 0.0450 0.3484 0.9847 0.497 Uiso 1 1 calc R . . C55 C -0.0652(11) 0.4227(12) 1.0736(12) 0.410(13) Uani 1 1 d DU . . H55 H -0.1105 0.3709 1.1244 0.492 Uiso 1 1 calc R . . C57 C 0.0908(10) 0.4875(15) 0.9184(11) 0.426(13) Uani 1 1 d DU . . H57 H 0.1535 0.4797 0.8617 0.511 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.055(3) 0.060(2) 0.055(3) -0.023(2) -0.028(2) 0.008(2) C2 0.047(2) 0.046(2) 0.044(2) -0.0169(17) -0.0131(18) 0.0009(17) C3 0.0396(19) 0.0356(17) 0.0411(19) -0.0139(15) -0.0143(16) 0.0037(14) C4 0.053(2) 0.041(2) 0.050(2) -0.0198(18) -0.018(2) 0.0153(17) C5 0.057(3) 0.044(2) 0.053(3) -0.0158(19) -0.018(2) 0.0194(19) C6 0.040(2) 0.0355(18) 0.044(2) -0.0107(15) -0.0160(17) 0.0010(14) C7 0.050(2) 0.0395(19) 0.044(2) -0.0078(16) -0.0144(18) 0.0125(17) C8 0.043(2) 0.0311(17) 0.042(2) -0.0086(15) -0.0119(17) 0.0059(14) C9 0.051(2) 0.0334(18) 0.045(2) -0.0062(16) -0.0151(18) 0.0064(16) C10 0.052(2) 0.0320(18) 0.056(2) -0.0155(17) -0.0162(19) 0.0017(16) C11 0.076(3) 0.043(2) 0.068(3) -0.003(2) -0.035(3) -0.006(2) C12 0.061(3) 0.043(2) 0.083(3) -0.023(2) -0.040(3) 0.0115(19) C13 0.054(2) 0.0360(19) 0.074(3) -0.0105(19) -0.038(2) 0.0041(17) C14 0.0373(19) 0.045(2) 0.049(2) -0.0095(17) -0.0222(17) -0.0007(15) C15 0.038(2) 0.045(2) 0.046(2) -0.0125(17) -0.0209(17) 0.0078(16) C16 0.045(2) 0.0405(19) 0.046(2) -0.0119(16) -0.0244(18) 0.0011(15) C17 0.050(2) 0.0391(19) 0.066(3) -0.0079(18) -0.036(2) 0.0002(17) C18 0.049(2) 0.0379(19) 0.051(2) -0.0133(17) -0.0246(19) 0.0016(16) C19 0.042(2) 0.043(2) 0.049(2) -0.0089(17) -0.0215(18) -0.0001(16) C20 0.044(2) 0.058(2) 0.058(3) -0.013(2) -0.020(2) 0.0034(19) C21 0.053(3) 0.048(2) 0.064(3) -0.003(2) -0.029(2) -0.0083(19) C22 0.054(3) 0.0364(19) 0.058(3) -0.0092(18) -0.015(2) -0.0044(17) C23 0.063(3) 0.0372(19) 0.069(3) -0.0190(19) -0.034(2) 0.0013(18) C24 0.043(2) 0.0297(17) 0.056(2) -0.0074(16) -0.0246(19) -0.0010(15) C25 0.043(2) 0.0376(18) 0.057(2) -0.0104(17) -0.0262(19) 0.0025(15) C26 0.0386(19) 0.0339(17) 0.047(2) -0.0084(15) -0.0180(17) 0.0014(14) C27 0.0373(19) 0.0342(17) 0.0407(19) -0.0131(15) -0.0158(16) 0.0014(14) C28 0.0374(19) 0.0344(17) 0.047(2) -0.0118(15) -0.0174(17) -0.0017(14) C29 0.039(2) 0.0341(17) 0.046(2) -0.0111(15) -0.0171(17) 0.0008(14) C30 0.053(2) 0.045(2) 0.048(2) -0.0163(18) -0.0183(19) 0.0028(17) C31 0.044(2) 0.042(2) 0.049(2) -0.0081(17) -0.0188(18) 0.0015(16) C32 0.0370(19) 0.0326(17) 0.051(2) -0.0113(15) -0.0199(17) 0.0000(14) C33 0.090(5) 0.069(4) 0.130(6) -0.033(4) -0.051(5) 0.014(3) C34 0.112(5) 0.068(3) 0.127(6) -0.030(4) -0.085(5) 0.013(3) C35 0.088(4) 0.067(3) 0.093(4) -0.024(3) -0.050(4) 0.010(3) C36 0.125(6) 0.081(4) 0.215(10) -0.078(6) -0.123(7) 0.042(4) C37 0.169(7) 0.130(5) 0.136(6) 0.003(5) -0.051(5) -0.017(5) C38 0.183(7) 0.098(4) 0.116(5) -0.048(4) -0.030(5) -0.037(5) C39 0.185(8) 0.124(6) 0.154(7) 0.010(5) -0.070(5) -0.027(5) C40 0.203(7) 0.116(6) 0.163(7) -0.016(5) -0.088(5) -0.030(5) C45 0.205(7) 0.107(5) 0.119(5) -0.046(4) -0.079(5) 0.007(5) C46 0.145(6) 0.089(4) 0.108(4) -0.042(3) -0.071(4) 0.027(4) C47 0.147(6) 0.110(5) 0.124(5) -0.038(4) -0.083(5) 0.035(4) C48 0.203(7) 0.150(6) 0.136(6) -0.040(5) -0.106(5) 0.029(5) C49 0.236(8) 0.169(7) 0.123(6) -0.022(5) -0.105(6) 0.019(6) C50 0.231(8) 0.143(6) 0.125(5) -0.020(5) -0.084(6) 0.005(6) N1 0.0415(17) 0.0345(15) 0.0450(18) -0.0141(13) -0.0176(14) 0.0054(12) N2 0.0436(18) 0.0394(16) 0.0452(18) -0.0123(14) -0.0136(15) 0.0106(13) N3 0.0397(17) 0.0396(16) 0.0522(19) -0.0099(14) -0.0244(15) 0.0002(13) N4 0.0415(17) 0.0373(15) 0.0437(17) -0.0123(13) -0.0213(14) 0.0036(13) N5 0.0387(17) 0.0344(15) 0.0500(18) -0.0090(13) -0.0217(15) -0.0012(12) N6 0.0352(16) 0.0326(14) 0.0411(16) -0.0112(12) -0.0146(13) 0.0008(12) O1 0.0380(13) 0.0299(12) 0.0405(13) -0.0093(10) -0.0132(11) 0.0031(10) O2 0.0432(15) 0.0413(13) 0.0441(14) -0.0097(11) -0.0190(12) 0.0019(11) O3 0.0348(13) 0.0361(13) 0.0543(16) -0.0092(12) -0.0134(12) 0.0000(10) O4 0.152(5) 0.062(3) 0.214(7) -0.034(3) -0.132(5) 0.029(3) O5 0.195(6) 0.090(4) 0.168(6) 0.003(4) -0.074(5) -0.011(4) S1 0.0497(6) 0.0545(6) 0.0864(9) -0.0233(6) -0.0345(6) 0.0129(5) S2 0.0793(9) 0.0792(8) 0.0887(9) -0.0285(7) -0.0615(8) 0.0082(7) S3 0.0469(6) 0.0433(5) 0.0494(6) -0.0153(4) -0.0200(5) 0.0117(4) S4 0.0463(5) 0.0486(5) 0.0467(5) -0.0158(4) -0.0225(4) 0.0069(4) Sc1 0.0336(4) 0.0305(3) 0.0366(4) -0.0091(3) -0.0115(3) 0.0029(3) O6 0.181(7) 0.471(15) 0.167(6) -0.013(8) -0.097(6) 0.019(9) C52 0.167(8) 0.453(16) 0.130(7) -0.022(9) -0.089(6) 0.045(9) C53 0.158(8) 0.456(16) 0.142(7) -0.034(8) -0.086(7) 0.032(9) C54 0.169(8) 0.462(16) 0.151(7) -0.016(9) -0.089(7) 0.024(9) C51 0.170(8) 0.464(16) 0.162(7) -0.015(9) -0.099(7) 0.019(10) C56 0.134(9) 0.97(4) 0.250(15) -0.33(2) -0.097(9) 0.068(17) C55 0.136(9) 0.97(4) 0.244(15) -0.33(2) -0.099(9) 0.068(17) C57 0.139(10) 0.97(4) 0.261(15) -0.32(2) -0.090(10) 0.069(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C3 1.513(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.517(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 N1 1.471(5) . ? C3 H3 1.0000 . ? C4 C5 1.345(6) . ? C4 N1 1.380(5) . ? C4 H4 0.9500 . ? C5 N2 1.389(5) . ? C5 H5 0.9500 . ? C6 N1 1.354(5) . ? C6 N2 1.357(5) . ? C6 Sc1 2.391(4) . ? C7 N2 1.461(5) . ? C7 C8 1.542(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O1 1.437(4) . ? C8 C9 1.521(6) . ? C8 C10 1.523(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.509(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.522(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N3 1.488(5) . ? C13 H13 1.0000 . ? C14 C15 1.333(6) . ? C14 N3 1.382(5) . ? C14 H14 0.9500 . ? C15 N4 1.373(5) . ? C15 H15 0.9500 . ? C16 N3 1.344(5) . ? C16 N4 1.349(5) . ? C16 C17 1.478(6) . ? C17 S1 1.667(5) . ? C17 S2 1.669(5) . ? C18 N4 1.471(5) . ? C18 C19 1.534(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 O2 1.392(5) . ? C19 C20 1.530(6) . ? C19 C21 1.537(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.513(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.522(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 N5 1.489(5) . ? C24 H24 1.0000 . ? C25 C26 1.345(5) . ? C25 N5 1.384(5) . ? C25 H25 0.9500 . ? C26 N6 1.376(5) . ? C26 H26 0.9500 . ? C27 N5 1.327(5) . ? C27 N6 1.348(5) . ? C27 C32 1.484(5) . ? C28 N6 1.471(5) . ? C28 C29 1.545(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O3 1.401(5) . ? C29 C30 1.529(5) . ? C29 C31 1.532(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 S3 1.668(4) . ? C32 S4 1.681(4) . ? C33 O4 1.399(9) . ? C33 C34 1.481(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.473(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.459(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O4 1.338(9) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 O5 1.362(8) . ? C37 C38 1.450(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.433(9) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.407(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 O5 1.349(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C45 C46 1.3900 . ? C45 C50 1.3900 . ? C45 H45 0.9500 . ? C46 C47 1.3900 . ? C46 H46 0.9500 . ? C47 C48 1.3900 . ? C47 H47 0.9500 . ? C48 C49 1.3900 . ? C48 H48 0.9500 . ? C49 C50 1.3900 . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? O1 Sc1 2.087(3) . ? O1 Sc1 2.162(2) 2_665 ? O2 Sc1 1.939(3) . ? O3 Sc1 1.927(3) . ? Sc1 O1 2.162(2) 2_665 ? Sc1 Sc1 3.3360(14) 2_665 ? O6 C51 1.381(9) . ? O6 C54 1.417(9) . ? C52 C53 1.413(9) . ? C52 C51 1.426(10) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.434(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C56 C55 1.3998(11) . ? C56 C57 1.3998(11) . ? C56 H56 0.9500 . ? C55 C57 1.3999(8) 2_567 ? C55 H55 0.9500 . ? C57 C55 1.3999(8) 2_567 ? C57 H57 0.9500 . ? 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 C3 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C1 109.8(3) . . ? N1 C3 C2 111.8(3) . . ? C1 C3 C2 111.5(3) . . ? N1 C3 H3 107.8 . . ? C1 C3 H3 107.8 . . ? C2 C3 H3 107.8 . . ? C5 C4 N1 106.2(3) . . ? C5 C4 H4 126.9 . . ? N1 C4 H4 126.9 . . ? C4 C5 N2 106.9(4) . . ? C4 C5 H5 126.5 . . ? N2 C5 H5 126.5 . . ? N1 C6 N2 103.9(3) . . ? N1 C6 Sc1 132.4(3) . . ? N2 C6 Sc1 123.6(3) . . ? N2 C7 C8 114.1(3) . . ? N2 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? N2 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? O1 C8 C9 110.4(3) . . ? O1 C8 C10 109.7(3) . . ? C9 C8 C10 110.1(3) . . ? O1 C8 C7 110.1(3) . . ? C9 C8 C7 105.9(3) . . ? C10 C8 C7 110.5(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 H11A 109.5 . . ? C13 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C13 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C11 110.4(4) . . ? N3 C13 C12 108.8(4) . . ? C11 C13 C12 113.0(4) . . ? N3 C13 H13 108.2 . . ? C11 C13 H13 108.2 . . ? C12 C13 H13 108.2 . . ? C15 C14 N3 107.1(3) . . ? C15 C14 H14 126.5 . . ? N3 C14 H14 126.5 . . ? C14 C15 N4 108.3(3) . . ? C14 C15 H15 125.9 . . ? N4 C15 H15 125.9 . . ? N3 C16 N4 107.3(3) . . ? N3 C16 C17 125.6(3) . . ? N4 C16 C17 127.1(3) . . ? C16 C17 S1 115.8(3) . . ? C16 C17 S2 115.0(3) . . ? S1 C17 S2 129.2(3) . . ? N4 C18 C19 113.3(3) . . ? N4 C18 H18A 108.9 . . ? C19 C18 H18A 108.9 . . ? N4 C18 H18B 108.9 . . ? C19 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? O2 C19 C20 110.2(3) . . ? O2 C19 C18 109.6(3) . . ? C20 C19 C18 110.9(3) . . ? O2 C19 C21 110.0(3) . . ? C20 C19 C21 109.1(4) . . ? C18 C19 C21 107.0(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 H22A 109.5 . . ? C24 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C24 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N5 C24 C22 109.6(3) . . ? N5 C24 C23 108.6(3) . . ? C22 C24 C23 113.1(4) . . ? N5 C24 H24 108.5 . . ? C22 C24 H24 108.5 . . ? C23 C24 H24 108.5 . . ? C26 C25 N5 106.9(3) . . ? C26 C25 H25 126.6 . . ? N5 C25 H25 126.6 . . ? C25 C26 N6 107.5(3) . . ? C25 C26 H26 126.3 . . ? N6 C26 H26 126.3 . . ? N5 C27 N6 107.7(3) . . ? N5 C27 C32 126.0(3) . . ? N6 C27 C32 126.2(3) . . ? N6 C28 C29 115.6(3) . . ? N6 C28 H28A 108.4 . . ? C29 C28 H28A 108.4 . . ? N6 C28 H28B 108.4 . . ? C29 C28 H28B 108.4 . . ? H28A C28 H28B 107.5 . . ? O3 C29 C30 110.0(3) . . ? O3 C29 C31 109.5(3) . . ? C30 C29 C31 110.1(3) . . ? O3 C29 C28 104.4(3) . . ? C30 C29 C28 110.9(3) . . ? C31 C29 C28 111.9(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 S3 116.4(3) . . ? C27 C32 S4 114.3(3) . . ? S3 C32 S4 129.3(2) . . ? O4 C33 C34 107.8(6) . . ? O4 C33 H33A 110.1 . . ? C34 C33 H33A 110.1 . . ? O4 C33 H33B 110.1 . . ? C34 C33 H33B 110.1 . . ? H33A C33 H33B 108.5 . . ? C35 C34 C33 106.1(5) . . ? C35 C34 H34A 110.5 . . ? C33 C34 H34A 110.5 . . ? C35 C34 H34B 110.5 . . ? C33 C34 H34B 110.5 . . ? H34A C34 H34B 108.7 . . ? C36 C35 C34 104.0(5) . . ? C36 C35 H35A 111.0 . . ? C34 C35 H35A 111.0 . . ? C36 C35 H35B 111.0 . . ? C34 C35 H35B 111.0 . . ? H35A C35 H35B 109.0 . . ? O4 C36 C35 111.9(6) . . ? O4 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? O4 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? O5 C37 C38 106.4(8) . . ? O5 C37 H37A 110.4 . . ? C38 C37 H37A 110.4 . . ? O5 C37 H37B 110.4 . . ? C38 C37 H37B 110.4 . . ? H37A C37 H37B 108.6 . . ? C39 C38 C37 98.5(8) . . ? C39 C38 H38A 112.1 . . ? C37 C38 H38A 112.1 . . ? C39 C38 H38B 112.1 . . ? C37 C38 H38B 112.1 . . ? H38A C38 H38B 109.7 . . ? C40 C39 C38 106.3(9) . . ? C40 C39 H39A 110.5 . . ? C38 C39 H39A 110.5 . . ? C40 C39 H39B 110.5 . . ? C38 C39 H39B 110.5 . . ? H39A C39 H39B 108.7 . . ? O5 C40 C39 106.8(9) . . ? O5 C40 H40A 110.4 . . ? C39 C40 H40A 110.4 . . ? O5 C40 H40B 110.4 . . ? C39 C40 H40B 110.4 . . ? H40A C40 H40B 108.6 . . ? C46 C45 C50 120.0 . . ? C46 C45 H45 120.0 . . ? C50 C45 H45 120.0 . . ? C45 C46 C47 120.0 . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C48 C47 C46 120.0 . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C49 120.0 . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C48 C49 C50 120.0 . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C49 C50 C45 120.0 . . ? C49 C50 H50 120.0 . . ? C45 C50 H50 120.0 . . ? C6 N1 C4 112.0(3) . . ? C6 N1 C3 123.3(3) . . ? C4 N1 C3 124.6(3) . . ? C6 N2 C5 110.9(3) . . ? C6 N2 C7 124.3(3) . . ? C5 N2 C7 124.7(3) . . ? C16 N3 C14 108.9(3) . . ? C16 N3 C13 126.1(3) . . ? C14 N3 C13 125.0(3) . . ? C16 N4 C15 108.4(3) . . ? C16 N4 C18 126.8(3) . . ? C15 N4 C18 124.8(3) . . ? C27 N5 C25 109.3(3) . . ? C27 N5 C24 125.0(3) . . ? C25 N5 C24 125.7(3) . . ? C27 N6 C26 108.7(3) . . ? C27 N6 C28 124.1(3) . . ? C26 N6 C28 127.2(3) . . ? C8 O1 Sc1 128.8(2) . . ? C8 O1 Sc1 127.2(2) . 2_665 ? Sc1 O1 Sc1 103.44(10) . 2_665 ? C19 O2 Sc1 156.3(3) . . ? C29 O3 Sc1 161.6(2) . . ? C36 O4 C33 109.6(5) . . ? C40 O5 C37 108.3(8) . . ? O3 Sc1 O2 117.33(12) . . ? O3 Sc1 O1 126.02(12) . . ? O2 Sc1 O1 116.25(11) . . ? O3 Sc1 O1 98.85(11) . 2_665 ? O2 Sc1 O1 101.34(11) . 2_665 ? O1 Sc1 O1 76.56(10) . 2_665 ? O3 Sc1 C6 86.40(12) . . ? O2 Sc1 C6 94.79(12) . . ? O1 Sc1 C6 83.24(11) . . ? O1 Sc1 C6 158.22(12) 2_665 . ? O3 Sc1 Sc1 117.88(9) . 2_665 ? O2 Sc1 Sc1 113.84(9) . 2_665 ? O1 Sc1 Sc1 39.08(7) . 2_665 ? O1 Sc1 Sc1 37.49(7) 2_665 2_665 ? C6 Sc1 Sc1 121.89(10) . 2_665 ? C51 O6 C54 106.6(13) . . ? C53 C52 C51 102.2(14) . . ? C53 C52 H52A 111.3 . . ? C51 C52 H52A 111.3 . . ? C53 C52 H52B 111.3 . . ? C51 C52 H52B 111.3 . . ? H52A C52 H52B 109.2 . . ? C52 C53 C54 109.7(16) . . ? C52 C53 H53A 109.7 . . ? C54 C53 H53A 109.7 . . ? C52 C53 H53B 109.7 . . ? C54 C53 H53B 109.7 . . ? H53A C53 H53B 108.2 . . ? O6 C54 C53 101.7(14) . . ? O6 C54 H54A 111.4 . . ? C53 C54 H54A 111.4 . . ? O6 C54 H54B 111.4 . . ? C53 C54 H54B 111.4 . . ? H54A C54 H54B 109.3 . . ? O6 C51 C52 110.5(13) . . ? O6 C51 H51A 109.5 . . ? C52 C51 H51A 109.5 . . ? O6 C51 H51B 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 108.1 . . ? C55 C56 C57 117.6(11) . . ? C55 C56 H56 121.2 . . ? C57 C56 H56 121.2 . . ? C56 C55 C57 120.3(12) . 2_567 ? C56 C55 H55 119.8 . . ? C57 C55 H55 119.8 2_567 . ? C56 C57 C55 122.1(12) . 2_567 ? C56 C57 H57 119.0 . . ? C55 C57 H57 119.0 2_567 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C4 C5 N2 0.7(5) . . . . ? N2 C7 C8 O1 71.9(4) . . . . ? N2 C7 C8 C9 -168.7(3) . . . . ? N2 C7 C8 C10 -49.5(5) . . . . ? N3 C14 C15 N4 -0.4(5) . . . . ? N3 C16 C17 S1 69.8(5) . . . . ? N4 C16 C17 S1 -111.8(4) . . . . ? N3 C16 C17 S2 -110.0(4) . . . . ? N4 C16 C17 S2 68.4(5) . . . . ? N4 C18 C19 O2 53.8(4) . . . . ? N4 C18 C19 C20 -68.0(4) . . . . ? N4 C18 C19 C21 173.1(3) . . . . ? N5 C25 C26 N6 0.2(4) . . . . ? N6 C28 C29 O3 -157.5(3) . . . . ? N6 C28 C29 C30 -39.1(4) . . . . ? N6 C28 C29 C31 84.2(4) . . . . ? N5 C27 C32 S3 98.8(4) . . . . ? N6 C27 C32 S3 -85.7(4) . . . . ? N5 C27 C32 S4 -82.8(4) . . . . ? N6 C27 C32 S4 92.7(4) . . . . ? O4 C33 C34 C35 -1.4(9) . . . . ? C33 C34 C35 C36 -3.4(9) . . . . ? C34 C35 C36 O4 7.7(10) . . . . ? O5 C37 C38 C39 35.6(13) . . . . ? C37 C38 C39 C40 -33.5(14) . . . . ? C38 C39 C40 O5 20.6(16) . . . . ? C50 C45 C46 C47 0.0 . . . . ? C45 C46 C47 C48 0.0 . . . . ? C46 C47 C48 C49 0.0 . . . . ? C47 C48 C49 C50 0.0 . . . . ? C48 C49 C50 C45 0.0 . . . . ? C46 C45 C50 C49 0.0 . . . . ? N2 C6 N1 C4 -0.2(4) . . . . ? Sc1 C6 N1 C4 -176.8(3) . . . . ? N2 C6 N1 C3 -177.3(3) . . . . ? Sc1 C6 N1 C3 6.1(6) . . . . ? C5 C4 N1 C6 -0.3(5) . . . . ? C5 C4 N1 C3 176.8(4) . . . . ? C1 C3 N1 C6 97.9(4) . . . . ? C2 C3 N1 C6 -137.8(4) . . . . ? C1 C3 N1 C4 -78.8(5) . . . . ? C2 C3 N1 C4 45.5(5) . . . . ? N1 C6 N2 C5 0.6(5) . . . . ? Sc1 C6 N2 C5 177.6(3) . . . . ? N1 C6 N2 C7 -177.4(4) . . . . ? Sc1 C6 N2 C7 -0.5(6) . . . . ? C4 C5 N2 C6 -0.8(5) . . . . ? C4 C5 N2 C7 177.2(4) . . . . ? C8 C7 N2 C6 -43.8(6) . . . . ? C8 C7 N2 C5 138.4(4) . . . . ? N4 C16 N3 C14 -0.5(4) . . . . ? C17 C16 N3 C14 178.2(4) . . . . ? N4 C16 N3 C13 -178.0(4) . . . . ? C17 C16 N3 C13 0.7(7) . . . . ? C15 C14 N3 C16 0.6(5) . . . . ? C15 C14 N3 C13 178.1(4) . . . . ? C11 C13 N3 C16 120.4(5) . . . . ? C12 C13 N3 C16 -115.0(4) . . . . ? C11 C13 N3 C14 -56.7(5) . . . . ? C12 C13 N3 C14 67.9(5) . . . . ? N3 C16 N4 C15 0.2(4) . . . . ? C17 C16 N4 C15 -178.4(4) . . . . ? N3 C16 N4 C18 179.7(3) . . . . ? C17 C16 N4 C18 1.1(7) . . . . ? C14 C15 N4 C16 0.1(5) . . . . ? C14 C15 N4 C18 -179.4(4) . . . . ? C19 C18 N4 C16 103.7(4) . . . . ? C19 C18 N4 C15 -76.9(5) . . . . ? N6 C27 N5 C25 -0.6(4) . . . . ? C32 C27 N5 C25 175.7(4) . . . . ? N6 C27 N5 C24 177.7(3) . . . . ? C32 C27 N5 C24 -6.0(6) . . . . ? C26 C25 N5 C27 0.2(5) . . . . ? C26 C25 N5 C24 -178.1(4) . . . . ? C22 C24 N5 C27 122.4(4) . . . . ? C23 C24 N5 C27 -113.6(4) . . . . ? C22 C24 N5 C25 -59.6(5) . . . . ? C23 C24 N5 C25 64.4(5) . . . . ? N5 C27 N6 C26 0.7(4) . . . . ? C32 C27 N6 C26 -175.5(4) . . . . ? N5 C27 N6 C28 -176.8(3) . . . . ? C32 C27 N6 C28 7.0(6) . . . . ? C25 C26 N6 C27 -0.6(4) . . . . ? C25 C26 N6 C28 176.8(3) . . . . ? C29 C28 N6 C27 115.2(4) . . . . ? C29 C28 N6 C26 -61.7(5) . . . . ? C9 C8 O1 Sc1 -173.2(2) . . . . ? C10 C8 O1 Sc1 65.2(4) . . . . ? C7 C8 O1 Sc1 -56.6(4) . . . . ? C9 C8 O1 Sc1 16.6(4) . . . 2_665 ? C10 C8 O1 Sc1 -105.0(3) . . . 2_665 ? C7 C8 O1 Sc1 133.2(3) . . . 2_665 ? C20 C19 O2 Sc1 -42.7(7) . . . . ? C18 C19 O2 Sc1 -165.0(5) . . . . ? C21 C19 O2 Sc1 77.6(7) . . . . ? C30 C29 O3 Sc1 104.9(8) . . . . ? C31 C29 O3 Sc1 -16.2(10) . . . . ? C28 C29 O3 Sc1 -136.1(7) . . . . ? C35 C36 O4 C33 -9.0(11) . . . . ? C34 C33 O4 C36 6.3(10) . . . . ? C39 C40 O5 C37 2.9(16) . . . . ? C38 C37 O5 C40 -25.1(14) . . . . ? C29 O3 Sc1 O2 140.5(8) . . . . ? C29 O3 Sc1 O1 -32.0(8) . . . . ? C29 O3 Sc1 O1 -111.7(8) . . . 2_665 ? C29 O3 Sc1 C6 47.0(8) . . . . ? C29 O3 Sc1 Sc1 -77.4(8) . . . 2_665 ? C19 O2 Sc1 O3 154.6(6) . . . . ? C19 O2 Sc1 O1 -32.1(6) . . . . ? C19 O2 Sc1 O1 48.4(6) . . . 2_665 ? C19 O2 Sc1 C6 -117.0(6) . . . . ? C19 O2 Sc1 Sc1 11.1(6) . . . 2_665 ? C8 O1 Sc1 O3 96.8(3) . . . . ? Sc1 O1 Sc1 O3 -91.25(14) 2_665 . . . ? C8 O1 Sc1 O2 -75.8(3) . . . . ? Sc1 O1 Sc1 O2 96.18(13) 2_665 . . . ? C8 O1 Sc1 O1 -172.0(3) . . . 2_665 ? Sc1 O1 Sc1 O1 0.0 2_665 . . 2_665 ? C8 O1 Sc1 C6 16.2(3) . . . . ? Sc1 O1 Sc1 C6 -171.79(14) 2_665 . . . ? C8 O1 Sc1 Sc1 -172.0(3) . . . 2_665 ? N1 C6 Sc1 O3 63.1(4) . . . . ? N2 C6 Sc1 O3 -112.9(3) . . . . ? N1 C6 Sc1 O2 -54.0(4) . . . . ? N2 C6 Sc1 O2 130.0(3) . . . . ? N1 C6 Sc1 O1 -169.9(4) . . . . ? N2 C6 Sc1 O1 14.1(3) . . . . ? N1 C6 Sc1 O1 168.1(3) . . . 2_665 ? N2 C6 Sc1 O1 -7.9(6) . . . 2_665 ? N1 C6 Sc1 Sc1 -176.0(3) . . . 2_665 ? N2 C6 Sc1 Sc1 8.0(4) . . . 2_665 ? C51 C52 C53 C54 19(2) . . . . ? C51 O6 C54 C53 29(2) . . . . ? C52 C53 C54 O6 -30(2) . . . . ? C54 O6 C51 C52 -19(3) . . . . ? C53 C52 C51 O6 0(3) . . . . ? C57 C56 C55 C57 -0.02(17) . . . 2_567 ? C55 C56 C57 C55 0.02(17) . . . 2_567 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 67.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.839 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.090 _database_code_depnum_ccdc_archive 'CCDC 954363' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_po9039 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C11H18N2S2O _chemical_formula_sum 'C11 H18 N2 O S2' _chemical_formula_weight 258.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.4671(5) _cell_length_b 11.5196(7) _cell_length_c 14.1073(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1375.99(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5770 _cell_measurement_theta_min 4.565 _cell_measurement_theta_max 60.728 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas 1.25 _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 0.370 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7230 _exptl_absorpt_correction_T_max 0.8787 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71080 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15595 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 30.48 _reflns_number_total 4154 _reflns_number_gt 3746 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen et al., 2004)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.2641P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(9) _refine_ls_number_reflns 4154 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _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 S1 S 0.56413(7) 0.98494(5) 0.57878(4) 0.03054(14) Uani 1 1 d . . . S2 S 0.37930(7) 0.98347(7) 0.39527(4) 0.03641(17) Uani 1 1 d . . . O1 O 0.17279(19) 0.63248(15) 0.71156(12) 0.0298(4) Uani 1 1 d . . . H1 H 0.1214 0.5900 0.6743 0.045 Uiso 1 1 calc R . . N1 N 0.1949(2) 0.84531(15) 0.58910(13) 0.0210(4) Uani 1 1 d . . . N2 N 0.1456(2) 1.02966(16) 0.59025(13) 0.0252(4) Uani 1 1 d . . . C1 C 0.2521(2) 0.94990(18) 0.56449(15) 0.0222(4) Uani 1 1 d . . . C8 C 0.3158(3) 0.6698(2) 0.66638(17) 0.0247(4) Uani 1 1 d . . . C7 C 0.2772(3) 0.73451(18) 0.57453(17) 0.0241(4) Uani 1 1 d . . . H7A H 0.3767 0.7495 0.5398 0.029 Uiso 1 1 calc R . . H7B H 0.2106 0.6840 0.5342 0.029 Uiso 1 1 calc R . . C3 C 0.0181(3) 0.9744(2) 0.63184(16) 0.0277(5) Uani 1 1 d . . . H3 H -0.0738 1.0106 0.6567 0.033 Uiso 1 1 calc R . . C10 C 0.3973(3) 0.7465(2) 0.73840(19) 0.0359(6) Uani 1 1 d . . . H10A H 0.4247 0.7004 0.7944 0.054 Uiso 1 1 calc R . . H10B H 0.3262 0.8097 0.7569 0.054 Uiso 1 1 calc R . . H10C H 0.4936 0.7790 0.7105 0.054 Uiso 1 1 calc R . . C11 C 0.4025(2) 0.97281(19) 0.51261(15) 0.0236(4) Uani 1 1 d . . . C2 C 0.0484(3) 0.8597(2) 0.63049(16) 0.0253(4) Uani 1 1 d . . . H2 H -0.0185 0.7999 0.6537 0.030 Uiso 1 1 calc R . . C4 C 0.1625(3) 1.15698(19) 0.57541(19) 0.0297(5) Uani 1 1 d . . . H4 H 0.2641 1.1709 0.5411 0.036 Uiso 1 1 calc R . . C5 C 0.1715(4) 1.2175(3) 0.6687(2) 0.0495(8) Uani 1 1 d . . . H5A H 0.2592 1.1854 0.7057 0.074 Uiso 1 1 calc R . . H5B H 0.0723 1.2061 0.7033 0.074 Uiso 1 1 calc R . . H5C H 0.1889 1.3006 0.6583 0.074 Uiso 1 1 calc R . . C9 C 0.4138(3) 0.5644(2) 0.6396(2) 0.0366(6) Uani 1 1 d . . . H9A H 0.3567 0.5183 0.5922 0.055 Uiso 1 1 calc R . . H9B H 0.4328 0.5169 0.6961 0.055 Uiso 1 1 calc R . . H9C H 0.5150 0.5898 0.6131 0.055 Uiso 1 1 calc R . . C6 C 0.0303(5) 1.1996(3) 0.5137(3) 0.0744(13) Uani 1 1 d . . . H6A H -0.0702 1.1908 0.5474 0.112 Uiso 1 1 calc R . . H6B H 0.0275 1.1542 0.4550 0.112 Uiso 1 1 calc R . . H6C H 0.0473 1.2817 0.4985 0.112 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0251(2) 0.0303(3) 0.0363(3) -0.0031(2) 0.0000(2) -0.0036(2) S2 0.0299(3) 0.0543(4) 0.0250(3) 0.0032(3) 0.0071(2) 0.0059(3) O1 0.0276(8) 0.0289(9) 0.0328(9) 0.0036(7) 0.0036(7) -0.0043(7) N1 0.0215(8) 0.0190(8) 0.0226(9) 0.0020(7) -0.0005(7) 0.0014(6) N2 0.0263(8) 0.0214(9) 0.0279(9) 0.0033(8) 0.0079(7) 0.0039(7) C1 0.0237(9) 0.0204(10) 0.0225(10) -0.0004(8) 0.0017(8) 0.0014(7) C8 0.0224(10) 0.0224(11) 0.0294(11) 0.0051(9) -0.0017(8) 0.0006(8) C7 0.0273(10) 0.0176(10) 0.0275(11) 0.0002(8) 0.0013(8) 0.0031(8) C3 0.0248(10) 0.0307(12) 0.0276(10) 0.0031(10) 0.0060(8) 0.0062(9) C10 0.0373(13) 0.0346(13) 0.0357(13) 0.0064(11) -0.0108(10) -0.0061(10) C11 0.0248(9) 0.0193(10) 0.0267(10) 0.0006(8) 0.0065(7) 0.0022(8) C2 0.0221(10) 0.0269(11) 0.0271(11) 0.0050(9) 0.0026(8) 0.0010(8) C4 0.0354(12) 0.0166(10) 0.0373(13) 0.0025(10) 0.0125(10) 0.0031(8) C5 0.070(2) 0.0353(16) 0.0429(16) -0.0069(13) 0.0013(15) -0.0179(14) C9 0.0380(13) 0.0260(12) 0.0458(15) 0.0070(11) 0.0030(11) 0.0120(10) C6 0.119(3) 0.0223(14) 0.082(3) 0.0143(16) -0.055(3) -0.0006(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C11 1.662(2) . ? S2 C11 1.672(2) . ? O1 C8 1.434(3) . ? O1 H1 0.8400 . ? N1 C1 1.344(3) . ? N1 C2 1.381(3) . ? N1 C7 1.468(3) . ? N2 C1 1.338(3) . ? N2 C3 1.384(3) . ? N2 C4 1.488(3) . ? C1 C11 1.492(3) . ? C8 C10 1.513(3) . ? C8 C9 1.518(3) . ? C8 C7 1.530(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C3 C2 1.345(3) . ? C3 H3 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C2 H2 0.9500 . ? C4 C5 1.491(4) . ? C4 C6 1.500(4) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? 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 C8 O1 H1 109.5 . . ? C1 N1 C2 108.96(17) . . ? C1 N1 C7 124.89(17) . . ? C2 N1 C7 126.14(18) . . ? C1 N2 C3 108.97(19) . . ? C1 N2 C4 125.00(18) . . ? C3 N2 C4 126.02(19) . . ? N2 C1 N1 107.60(18) . . ? N2 C1 C11 125.96(19) . . ? N1 C1 C11 126.35(18) . . ? O1 C8 C10 105.2(2) . . ? O1 C8 C9 109.40(19) . . ? C10 C8 C9 112.7(2) . . ? O1 C8 C7 109.97(17) . . ? C10 C8 C7 112.42(19) . . ? C9 C8 C7 107.2(2) . . ? N1 C7 C8 113.99(19) . . ? N1 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N1 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C2 C3 N2 107.26(19) . . ? C2 C3 H3 126.4 . . ? N2 C3 H3 126.4 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C1 C11 S1 116.23(16) . . ? C1 C11 S2 113.48(16) . . ? S1 C11 S2 130.29(12) . . ? C3 C2 N1 107.19(19) . . ? C3 C2 H2 126.4 . . ? N1 C2 H2 126.4 . . ? N2 C4 C5 110.0(2) . . ? N2 C4 C6 109.4(2) . . ? C5 C4 C6 113.4(3) . . ? N2 C4 H4 108.0 . . ? C5 C4 H4 108.0 . . ? C6 C4 H4 108.0 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N2 C1 N1 -0.1(3) . . . . ? C4 N2 C1 N1 -179.7(2) . . . . ? C3 N2 C1 C11 176.5(2) . . . . ? C4 N2 C1 C11 -3.1(4) . . . . ? C2 N1 C1 N2 0.6(2) . . . . ? C7 N1 C1 N2 -179.0(2) . . . . ? C2 N1 C1 C11 -176.1(2) . . . . ? C7 N1 C1 C11 4.4(4) . . . . ? C1 N1 C7 C8 117.5(2) . . . . ? C2 N1 C7 C8 -62.0(3) . . . . ? O1 C8 C7 N1 66.6(2) . . . . ? C10 C8 C7 N1 -50.2(3) . . . . ? C9 C8 C7 N1 -174.55(19) . . . . ? C1 N2 C3 C2 -0.3(3) . . . . ? C4 N2 C3 C2 179.2(2) . . . . ? N2 C1 C11 S1 96.7(2) . . . . ? N1 C1 C11 S1 -87.2(3) . . . . ? N2 C1 C11 S2 -82.7(3) . . . . ? N1 C1 C11 S2 93.3(2) . . . . ? N2 C3 C2 N1 0.6(3) . . . . ? C1 N1 C2 C3 -0.8(3) . . . . ? C7 N1 C2 C3 178.8(2) . . . . ? C1 N2 C4 C5 -115.4(3) . . . . ? C3 N2 C4 C5 65.1(3) . . . . ? C1 N2 C4 C6 119.4(3) . . . . ? C3 N2 C4 C6 -60.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.372 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.065 _database_code_depnum_ccdc_archive 'CCDC 954364'