# Electronic Supplementary Material (ESI) for Chemical Communications # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H68 N12 Sc3, C30 H70 N12 Sc3, C6 H14' _chemical_formula_sum 'C66 H152 N24 Sc6' _chemical_formula_weight 1551.88 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' 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' _symmetry_space_group_name_Hall '-P 2YBC' 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 18.0667(9) _cell_length_b 19.2883(10) _cell_length_c 28.4424(11) _cell_angle_alpha 90.00 _cell_angle_beta 125.387(2) _cell_angle_gamma 90.00 _cell_volume 8080.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4724 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 20.89 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3368 _exptl_absorpt_coefficient_mu 0.529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8617 _exptl_absorpt_correction_T_max 0.9296 _exptl_absorpt_process_details 'Sadabs Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86450 _diffrn_reflns_av_R_equivalents 0.0935 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.10 _reflns_number_total 14355 _reflns_number_gt 10391 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Altomare 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1999)' _computing_publication_material ? _refine_special_details ; The structure contains severely disordered hexane. This was included with three split positions and was refined with C-C distance restraints and a common isotropic displacement parameter for all carbon atoms of each hexane molecule. Of course the geometry within the strongly disordered hexane molecule is not discussed. ; _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^)+(0.0599P)^2^+2.0618P] 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 14355 _refine_ls_number_parameters 892 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1414 _refine_ls_wR_factor_gt 0.1250 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc1 Sc 0.60216(4) 0.44848(3) 0.69418(3) 0.01610(16) Uani 1 1 d . A . Sc2 Sc 0.47609(4) 0.49608(3) 0.73752(3) 0.01514(16) Uani 1 1 d . A . Sc3 Sc 0.56718(4) 0.61338(3) 0.70399(3) 0.01646(16) Uani 1 1 d . A . H1 H 0.612(2) 0.5192(17) 0.7567(14) 0.020 Uiso 1 1 d . . . H2 H 0.486(2) 0.5198(17) 0.6665(14) 0.020 Uiso 1 1 d . . . N1 N 0.5261(2) 0.39895(14) 0.72387(13) 0.0200(7) Uani 1 1 d . . . N2 N 0.7238(2) 0.39483(15) 0.78309(12) 0.0216(7) Uani 1 1 d . . . N3 N 0.6608(2) 0.37398(16) 0.67198(13) 0.0233(7) Uani 1 1 d . . . N4 N 0.4783(2) 0.38628(16) 0.60599(13) 0.0250(7) Uani 1 1 d . . . N5 N 0.4833(2) 0.61196(14) 0.73815(12) 0.0189(7) Uani 1 1 d . . . N6 N 0.3165(2) 0.53413(17) 0.66176(15) 0.0347(9) Uani 1 1 d . . . N7 N 0.3954(2) 0.45461(16) 0.76031(13) 0.0252(7) Uani 1 1 d . . . N8 N 0.5518(2) 0.52227(16) 0.83936(13) 0.0241(7) Uani 1 1 d . . . N9 N 0.6479(2) 0.55047(15) 0.68248(13) 0.0242(7) Uani 1 1 d . . . N10 N 0.4889(2) 0.63387(16) 0.60051(13) 0.0339(9) Uani 1 1 d . . . N11 N 0.5734(2) 0.71940(15) 0.69289(13) 0.0256(7) Uani 1 1 d . . . N12 N 0.7189(2) 0.65199(16) 0.77861(13) 0.0260(7) Uani 1 1 d . . . C1 C 0.6134(3) 0.3333(2) 0.61977(16) 0.0277(9) Uani 1 1 d . . . H1A H 0.6078 0.2848 0.6288 0.033 Uiso 1 1 calc R . . H1B H 0.6484 0.3330 0.6030 0.033 Uiso 1 1 calc R . . C2 C 0.5213(3) 0.3627(2) 0.57724(17) 0.0327(10) Uani 1 1 d . . . H2A H 0.5262 0.4023 0.5571 0.039 Uiso 1 1 calc R . . H2B H 0.4825 0.3270 0.5481 0.039 Uiso 1 1 calc R . . C3 C 0.4651(3) 0.3283(2) 0.63484(18) 0.0342(10) Uani 1 1 d . . . H3A H 0.5194 0.2980 0.6547 0.041 Uiso 1 1 calc R . . H3B H 0.4122 0.3000 0.6056 0.041 Uiso 1 1 calc R . . C4 C 0.4493(3) 0.3564(2) 0.67845(18) 0.0308(10) Uani 1 1 d . . . H4A H 0.3934 0.3849 0.6580 0.037 Uiso 1 1 calc R . . H4B H 0.4397 0.3171 0.6968 0.037 Uiso 1 1 calc R . . C5 C 0.5882(3) 0.3616(2) 0.77875(18) 0.0330(10) Uani 1 1 d . . . H5A H 0.5557 0.3214 0.7804 0.040 Uiso 1 1 calc R . . H5B H 0.6053 0.3928 0.8112 0.040 Uiso 1 1 calc R . . C6 C 0.6736(3) 0.3362(2) 0.78629(18) 0.0333(10) Uani 1 1 d . . . H6A H 0.7130 0.3128 0.8241 0.040 Uiso 1 1 calc R . . H6B H 0.6575 0.3020 0.7558 0.040 Uiso 1 1 calc R . . C7 C 0.7912(3) 0.3701(2) 0.77210(17) 0.0320(10) Uani 1 1 d . . . H7A H 0.8283 0.4098 0.7748 0.038 Uiso 1 1 calc R . . H7B H 0.8324 0.3358 0.8019 0.038 Uiso 1 1 calc R . . C8 C 0.7445(3) 0.3379(2) 0.71408(16) 0.0310(10) Uani 1 1 d . . . H8A H 0.7853 0.3388 0.7015 0.037 Uiso 1 1 calc R . . H8B H 0.7307 0.2888 0.7163 0.037 Uiso 1 1 calc R . . C9 C 0.7767(3) 0.4310(2) 0.83878(16) 0.0347(10) Uani 1 1 d . . . H9A H 0.7356 0.4571 0.8441 0.052 Uiso 1 1 calc R . . H9B H 0.8195 0.4629 0.8395 0.052 Uiso 1 1 calc R . . H9C H 0.8104 0.3970 0.8699 0.052 Uiso 1 1 calc R . . C10 C 0.3881(3) 0.4135(3) 0.55982(19) 0.0462(12) Uani 1 1 d . . . H10A H 0.3948 0.4479 0.5371 0.069 Uiso 1 1 calc R . . H10B H 0.3600 0.4354 0.5770 0.069 Uiso 1 1 calc R . . H10C H 0.3496 0.3754 0.5347 0.069 Uiso 1 1 calc R . . C11A C 0.3936(4) 0.6454(3) 0.7076(3) 0.0261(16) Uiso 0.66 1 d P A 1 H11A H 0.3732 0.6462 0.7333 0.031 Uiso 0.66 1 calc PR A 1 H11B H 0.3992 0.6940 0.6989 0.031 Uiso 0.66 1 calc PR A 1 C12A C 0.3258(5) 0.6105(3) 0.6545(3) 0.0379(16) Uiso 0.66 1 d P A 1 H12A H 0.3417 0.6160 0.6267 0.045 Uiso 0.66 1 calc PR A 1 H12B H 0.2663 0.6332 0.6377 0.045 Uiso 0.66 1 calc PR A 1 C13A C 0.2673(4) 0.5203(3) 0.6890(3) 0.0257(13) Uiso 0.66 1 d P A 1 H13A H 0.2008 0.5214 0.6597 0.031 Uiso 0.66 1 calc PR A 1 H13B H 0.2838 0.5552 0.7191 0.031 Uiso 0.66 1 calc PR A 1 C14A C 0.2986(5) 0.4474(4) 0.7156(3) 0.0247(19) Uiso 0.66 1 d P A 1 H14A H 0.2661 0.4322 0.7323 0.030 Uiso 0.66 1 calc PR A 1 H14B H 0.2875 0.4133 0.6861 0.030 Uiso 0.66 1 calc PR A 1 C11B C 0.3996(8) 0.6439(6) 0.6906(6) 0.027(3) Uiso 0.34 1 d P A 2 H11C H 0.3969 0.6415 0.6549 0.032 Uiso 0.34 1 calc PR A 2 H11D H 0.3977 0.6932 0.6994 0.032 Uiso 0.34 1 calc PR A 2 C12B C 0.3156(8) 0.6037(6) 0.6817(5) 0.026(3) Uiso 0.34 1 d P A 2 H12C H 0.3214 0.6012 0.7185 0.031 Uiso 0.34 1 calc PR A 2 H12D H 0.2582 0.6277 0.6528 0.031 Uiso 0.34 1 calc PR A 2 C13B C 0.2591(13) 0.4807(10) 0.6658(8) 0.080(6) Uiso 0.34 1 d P A 2 H13C H 0.1968 0.4989 0.6469 0.096 Uiso 0.34 1 calc PR A 2 H13D H 0.2556 0.4381 0.6452 0.096 Uiso 0.34 1 calc PR A 2 C14B C 0.2962(11) 0.4642(9) 0.7242(7) 0.037(5) Uiso 0.34 1 d P A 2 H14C H 0.2674 0.4211 0.7252 0.044 Uiso 0.34 1 calc PR A 2 H14D H 0.2808 0.5018 0.7409 0.044 Uiso 0.34 1 calc PR A 2 C15 C 0.4164(3) 0.4589(2) 0.81724(17) 0.0302(10) Uani 1 1 d . A . H15A H 0.3985 0.4152 0.8264 0.036 Uiso 1 1 calc R . . H15B H 0.3814 0.4973 0.8188 0.036 Uiso 1 1 calc R . . C16 C 0.5151(3) 0.4711(2) 0.86065(17) 0.0305(10) Uani 1 1 d . A . H16A H 0.5481 0.4267 0.8695 0.037 Uiso 1 1 calc R . . H16B H 0.5254 0.4888 0.8967 0.037 Uiso 1 1 calc R . . C17 C 0.5152(3) 0.59194(19) 0.83454(16) 0.0296(9) Uani 1 1 d . A . H17A H 0.5453 0.6126 0.8734 0.035 Uiso 1 1 calc R . . H17B H 0.4493 0.5889 0.8168 0.035 Uiso 1 1 calc R . . C18 C 0.5314(3) 0.63748(19) 0.79767(17) 0.0301(9) Uani 1 1 d . A . H18A H 0.5108 0.6852 0.7971 0.036 Uiso 1 1 calc R . . H18B H 0.5973 0.6393 0.8152 0.036 Uiso 1 1 calc R . . C19A C 0.2654(5) 0.5049(4) 0.6030(3) 0.0337(16) Uiso 0.66 1 d P A 1 H19A H 0.2580 0.4548 0.6048 0.051 Uiso 0.66 1 calc PR A 1 H19B H 0.2988 0.5135 0.5861 0.051 Uiso 0.66 1 calc PR A 1 H19C H 0.2055 0.5269 0.5792 0.051 Uiso 0.66 1 calc PR A 1 C19B C 0.2756(12) 0.5385(9) 0.6002(7) 0.060(5) Uiso 0.34 1 d P A 2 H19D H 0.2728 0.4921 0.5852 0.090 Uiso 0.34 1 calc PR A 2 H19E H 0.3124 0.5688 0.5937 0.090 Uiso 0.34 1 calc PR A 2 H19F H 0.2141 0.5574 0.5803 0.090 Uiso 0.34 1 calc PR A 2 C20 C 0.6509(3) 0.5220(2) 0.88308(16) 0.0290(9) Uani 1 1 d . A . H20A H 0.6800 0.5510 0.8698 0.044 Uiso 1 1 calc R . . H20B H 0.6738 0.4744 0.8890 0.044 Uiso 1 1 calc R . . H20C H 0.6648 0.5404 0.9195 0.044 Uiso 1 1 calc R . . C21 C 0.6500(3) 0.7635(2) 0.73103(16) 0.0305(9) Uani 1 1 d . A . H21A H 0.6287 0.8075 0.7374 0.037 Uiso 1 1 calc R . . H21B H 0.6825 0.7746 0.7135 0.037 Uiso 1 1 calc R . . C22 C 0.7124(3) 0.72748(19) 0.78711(16) 0.0291(9) Uani 1 1 d . A . H22A H 0.6901 0.7336 0.8115 0.035 Uiso 1 1 calc R . . H22B H 0.7735 0.7486 0.8075 0.035 Uiso 1 1 calc R . . C23 C 0.7629(3) 0.6402(2) 0.74865(19) 0.0340(10) Uani 1 1 d . A . H23A H 0.8290 0.6485 0.7756 0.041 Uiso 1 1 calc R . . H23B H 0.7380 0.6729 0.7160 0.041 Uiso 1 1 calc R . . C24 C 0.7457(3) 0.5650(2) 0.7262(2) 0.0379(11) Uani 1 1 d . A . H24A H 0.7792 0.5565 0.7089 0.046 Uiso 1 1 calc R . . H24B H 0.7695 0.5327 0.7590 0.046 Uiso 1 1 calc R . . C25 C 0.6213(4) 0.5645(2) 0.62391(19) 0.0495(13) Uani 1 1 d . A . H25A H 0.5866 0.5244 0.5990 0.059 Uiso 1 1 calc R B 1 H25B H 0.6768 0.5693 0.6250 0.059 Uiso 1 1 calc R B 1 C26A C 0.5631(4) 0.6306(3) 0.5967(3) 0.0349(15) Uiso 0.66 1 d P A 1 H26A H 0.6022 0.6717 0.6161 0.042 Uiso 0.66 1 calc PR A 1 H26B H 0.5402 0.6326 0.5556 0.042 Uiso 0.66 1 calc PR A 1 C27A C 0.4480(4) 0.7056(3) 0.5906(3) 0.0388(16) Uiso 0.66 1 d P A 1 H27A H 0.3962 0.7047 0.5937 0.047 Uiso 0.66 1 calc PR A 1 H27B H 0.4263 0.7230 0.5518 0.047 Uiso 0.66 1 calc PR A 1 C28A C 0.5240(6) 0.7520(4) 0.6375(4) 0.033(3) Uiso 0.66 1 d P A 1 H28A H 0.5662 0.7636 0.6272 0.039 Uiso 0.66 1 calc PR A 1 H28B H 0.4973 0.7959 0.6394 0.039 Uiso 0.66 1 calc PR A 1 C26B C 0.5383(8) 0.5796(7) 0.5852(5) 0.031(3) Uiso 0.34 1 d P A 2 H26C H 0.5030 0.5360 0.5731 0.037 Uiso 0.34 1 calc PR A 2 H26D H 0.5346 0.5976 0.5513 0.037 Uiso 0.34 1 calc PR A 2 C27B C 0.5198(9) 0.7055(6) 0.5966(5) 0.033(3) Uiso 0.34 1 d P A 2 H27C H 0.4836 0.7221 0.5562 0.039 Uiso 0.34 1 calc PR A 2 H27D H 0.5847 0.7050 0.6114 0.039 Uiso 0.34 1 calc PR A 2 C28B C 0.5042(11) 0.7536(7) 0.6353(6) 0.017(4) Uiso 0.34 1 d P A 2 H28C H 0.5190 0.8027 0.6343 0.021 Uiso 0.34 1 calc PR A 2 H28D H 0.4416 0.7499 0.6247 0.021 Uiso 0.34 1 calc PR A 2 C29 C 0.7765(3) 0.6214(2) 0.83691(16) 0.0317(10) Uani 1 1 d . A . H29A H 0.7771 0.5708 0.8338 0.048 Uiso 1 1 calc R . . H29B H 0.7520 0.6337 0.8588 0.048 Uiso 1 1 calc R . . H29C H 0.8384 0.6393 0.8568 0.048 Uiso 1 1 calc R . . C30A C 0.4122(5) 0.5895(4) 0.5555(3) 0.052(2) Uiso 0.66 1 d P A 1 H30A H 0.3599 0.5955 0.5571 0.078 Uiso 0.66 1 calc PR A 1 H30B H 0.4311 0.5407 0.5627 0.078 Uiso 0.66 1 calc PR A 1 H30C H 0.3955 0.6031 0.5173 0.078 Uiso 0.66 1 calc PR A 1 C30B C 0.3943(8) 0.6243(6) 0.5575(5) 0.025(3) Uiso 0.34 1 d P A 2 H30D H 0.3598 0.6581 0.5633 0.038 Uiso 0.34 1 calc PR A 2 H30E H 0.3768 0.5773 0.5605 0.038 Uiso 0.34 1 calc PR A 2 H30F H 0.3812 0.6309 0.5192 0.038 Uiso 0.34 1 calc PR A 2 Sc4 Sc 0.20293(4) 0.53823(3) 0.91956(3) 0.01511(16) Uani 1 1 d . . . H3 H 0.219(2) 0.4473(16) 0.9638(14) 0.018 Uiso 1 1 d . . . H4 H 0.097(2) 0.4707(16) 0.8752(14) 0.018 Uiso 1 1 d . . . Sc5 Sc 0.16232(4) 0.38168(3) 0.89651(3) 0.01343(15) Uani 1 1 d . . . Sc6 Sc 0.08039(4) 0.24582(3) 0.90466(3) 0.01563(16) Uani 1 1 d . . . H5 H 0.047(2) 0.3441(17) 0.8790(14) 0.019 Uiso 1 1 d . . . H6 H 0.175(2) 0.3163(17) 0.9516(14) 0.019 Uiso 1 1 d . . . N13 N 0.2888(2) 0.59201(15) 0.99959(12) 0.0205(7) Uani 1 1 d . . . N14 N 0.1033(2) 0.57476(15) 0.94794(12) 0.0207(7) Uani 1 1 d . . . N15 N 0.11303(19) 0.61113(14) 0.85409(12) 0.0187(7) Uani 1 1 d . . . N16 N 0.30243(19) 0.62817(15) 0.90679(12) 0.0196(7) Uani 1 1 d . . . N17 N 0.24890(18) 0.45810(14) 0.88432(12) 0.0160(6) Uani 1 1 d . . . N18 N 0.31589(18) 0.33150(14) 0.95088(11) 0.0155(6) Uani 1 1 d . . . N19 N 0.14610(19) 0.27132(14) 0.85885(11) 0.0161(6) Uani 1 1 d . . . N20 N 0.07836(19) 0.39780(14) 0.79237(12) 0.0176(6) Uani 1 1 d . . . N21 N 0.1655(2) 0.17007(14) 0.96920(12) 0.0196(7) Uani 1 1 d . . . N22 N 0.0313(2) 0.12991(16) 0.85083(13) 0.0273(8) Uani 1 1 d . . . N23 N -0.0571(2) 0.22534(16) 0.87336(13) 0.0260(7) Uani 1 1 d . . . N24 N 0.0726(2) 0.27358(15) 0.98493(13) 0.0222(7) Uani 1 1 d . . . C31 C 0.2488(3) 0.63077(19) 1.02288(15) 0.0252(9) Uani 1 1 d . . . H31A H 0.2321 0.6777 1.0057 0.030 Uiso 1 1 calc R . . H31B H 0.2932 0.6357 1.0651 0.030 Uiso 1 1 calc R . . C32 C 0.1651(3) 0.5932(2) 1.00954(15) 0.0255(9) Uani 1 1 d . . . H32A H 0.1837 0.5505 1.0331 0.031 Uiso 1 1 calc R . . H32B H 0.1325 0.6232 1.0202 0.031 Uiso 1 1 calc R . . C33 C 0.0545(2) 0.63567(18) 0.91099(15) 0.0223(8) Uani 1 1 d . . . H33A H 0.0931 0.6775 0.9279 0.027 Uiso 1 1 calc R . . H33B H -0.0018 0.6437 0.9085 0.027 Uiso 1 1 calc R . . C34 C 0.0311(2) 0.62238(18) 0.85073(15) 0.0215(8) Uani 1 1 d . . . H34A H -0.0087 0.5812 0.8336 0.026 Uiso 1 1 calc R . . H34B H -0.0022 0.6627 0.8256 0.026 Uiso 1 1 calc R . . C35 C 0.1466(2) 0.67604(18) 0.84803(15) 0.0227(8) Uani 1 1 d . . . H35A H 0.1579 0.7086 0.8784 0.027 Uiso 1 1 calc R . . H35B H 0.1004 0.6969 0.8101 0.027 Uiso 1 1 calc R . . C36 C 0.2327(2) 0.66470(19) 0.85284(15) 0.0228(8) Uani 1 1 d . . . H36A H 0.2193 0.6372 0.8194 0.027 Uiso 1 1 calc R . . H36B H 0.2571 0.7101 0.8516 0.027 Uiso 1 1 calc R . . C37 C 0.3404(2) 0.67271(18) 0.95805(15) 0.0230(8) Uani 1 1 d . . . H37A H 0.2944 0.7069 0.9515 0.028 Uiso 1 1 calc R . . H37B H 0.3939 0.6983 0.9657 0.028 Uiso 1 1 calc R . . C38 C 0.3681(2) 0.62649(19) 1.00938(15) 0.0247(9) Uani 1 1 d . . . H38A H 0.4125 0.5914 1.0148 0.030 Uiso 1 1 calc R . . H38B H 0.3975 0.6549 1.0448 0.030 Uiso 1 1 calc R . . C39 C 0.0379(3) 0.52274(19) 0.94101(18) 0.0286(9) Uani 1 1 d . . . H39A H 0.0041 0.5418 0.9553 0.043 Uiso 1 1 calc R . . H39B H 0.0706 0.4810 0.9630 0.043 Uiso 1 1 calc R . . H39C H -0.0046 0.5109 0.9001 0.043 Uiso 1 1 calc R . . C40 C 0.3771(2) 0.6081(2) 0.90298(17) 0.0266(9) Uani 1 1 d . . . H40A H 0.4014 0.6494 0.8963 0.040 Uiso 1 1 calc R . . H40B H 0.3546 0.5755 0.8709 0.040 Uiso 1 1 calc R . . H40C H 0.4252 0.5859 0.9391 0.040 Uiso 1 1 calc R . . C41 C 0.3461(2) 0.44306(17) 0.92358(15) 0.0180(8) Uani 1 1 d . . . H41A H 0.3702 0.4630 0.9620 0.022 Uiso 1 1 calc R . . H41B H 0.3783 0.4652 0.9088 0.022 Uiso 1 1 calc R . . C42 C 0.3640(2) 0.36561(18) 0.92946(15) 0.0191(8) Uani 1 1 d . . . H42A H 0.3432 0.3459 0.8915 0.023 Uiso 1 1 calc R . . H42B H 0.4300 0.3570 0.9566 0.023 Uiso 1 1 calc R . . C43 C 0.3055(2) 0.25644(17) 0.93914(15) 0.0193(8) Uani 1 1 d . . . H43A H 0.2898 0.2335 0.9634 0.023 Uiso 1 1 calc R . . H43B H 0.3639 0.2370 0.9496 0.023 Uiso 1 1 calc R . . C44 C 0.2323(2) 0.24131(18) 0.87623(15) 0.0201(8) Uani 1 1 d . . . H44A H 0.2504 0.2607 0.8521 0.024 Uiso 1 1 calc R . . H44B H 0.2254 0.1905 0.8701 0.024 Uiso 1 1 calc R . . C45 C 0.0819(2) 0.27074(18) 0.79588(14) 0.0205(8) Uani 1 1 d . . . H45A H 0.0192 0.2683 0.7853 0.025 Uiso 1 1 calc R . . H45B H 0.0925 0.2288 0.7804 0.025 Uiso 1 1 calc R . . C46 C 0.0914(2) 0.33462(18) 0.76871(14) 0.0208(8) Uani 1 1 d . . . H46A H 0.1524 0.3353 0.7766 0.025 Uiso 1 1 calc R . . H46B H 0.0456 0.3332 0.7264 0.025 Uiso 1 1 calc R . . C47 C 0.1173(2) 0.45919(18) 0.78302(14) 0.0190(8) Uani 1 1 d . . . H47A H 0.0921 0.5018 0.7882 0.023 Uiso 1 1 calc R . . H47B H 0.0997 0.4587 0.7429 0.023 Uiso 1 1 calc R . . C48 C 0.2196(2) 0.46050(18) 0.82440(14) 0.0192(8) Uani 1 1 d . . . H48A H 0.2452 0.4203 0.8167 0.023 Uiso 1 1 calc R . . H48B H 0.2431 0.5033 0.8181 0.023 Uiso 1 1 calc R . . C49 C 0.3667(2) 0.34117(19) 1.01375(14) 0.0216(8) Uani 1 1 d . . . H49A H 0.3320 0.3213 1.0272 0.032 Uiso 1 1 calc R . . H49B H 0.3762 0.3908 1.0228 0.032 Uiso 1 1 calc R . . H49C H 0.4256 0.3178 1.0331 0.032 Uiso 1 1 calc R . . C50 C -0.0195(2) 0.4103(2) 0.76397(16) 0.0252(9) Uani 1 1 d . . . H50A H -0.0491 0.4190 0.7228 0.038 Uiso 1 1 calc R . . H50B H -0.0275 0.4506 0.7816 0.038 Uiso 1 1 calc R . . H50C H -0.0469 0.3694 0.7687 0.038 Uiso 1 1 calc R . . C51 C 0.1583(3) 0.09930(19) 0.94902(17) 0.0317(10) Uani 1 1 d . . . H51A H 0.1781 0.0665 0.9811 0.038 Uiso 1 1 calc R . . H51B H 0.1989 0.0934 0.9365 0.038 Uiso 1 1 calc R . . C52 C 0.0616(3) 0.0827(2) 0.89921(17) 0.0328(10) Uani 1 1 d . . . H52A H 0.0582 0.0343 0.8866 0.039 Uiso 1 1 calc R . . H52B H 0.0211 0.0872 0.9119 0.039 Uiso 1 1 calc R . . C53 C -0.0703(3) 0.1343(2) 0.81207(18) 0.0400(11) Uani 1 1 d . . . H53A H -0.0890 0.1619 0.7775 0.048 Uiso 1 1 calc R . . H53B H -0.0958 0.0871 0.7991 0.048 Uiso 1 1 calc R . . C54 C -0.1084(3) 0.1665(2) 0.84106(19) 0.0407(11) Uani 1 1 d . . . H54A H -0.1721 0.1805 0.8118 0.049 Uiso 1 1 calc R . . H54B H -0.1082 0.1322 0.8670 0.049 Uiso 1 1 calc R . . C55 C -0.0848(3) 0.2523(2) 0.90923(18) 0.0407(12) Uani 1 1 d . . . H55A H -0.1399 0.2275 0.8997 0.049 Uiso 1 1 calc R . . H55B H -0.1000 0.3021 0.9008 0.049 Uiso 1 1 calc R . . C56 C -0.0116(3) 0.2434(3) 0.9714(2) 0.0497(13) Uani 1 1 d . . . H56A H -0.0293 0.2664 0.9947 0.060 Uiso 1 1 calc R . . H56B H -0.0025 0.1935 0.9812 0.060 Uiso 1 1 calc R . . C57 C 0.1535(3) 0.2387(2) 1.03516(19) 0.0499(13) Uani 1 1 d . . . H57A H 0.2070 0.2690 1.0504 0.060 Uiso 1 1 calc R . . H57B H 0.1440 0.2331 1.0659 0.060 Uiso 1 1 calc R . . C58 C 0.1728(3) 0.1714(2) 1.02204(16) 0.0342(10) Uani 1 1 d . . . H58A H 0.2350 0.1574 1.0540 0.041 Uiso 1 1 calc R . . H58B H 0.1302 0.1370 1.0198 0.041 Uiso 1 1 calc R . . C59 C 0.0614(3) 0.1033(2) 0.81610(18) 0.0365(11) Uani 1 1 d . . . H59A H 0.1276 0.1072 0.8381 0.055 Uiso 1 1 calc R . . H59B H 0.0331 0.1304 0.7805 0.055 Uiso 1 1 calc R . . H59C H 0.0436 0.0545 0.8065 0.055 Uiso 1 1 calc R . . C60 C 0.0785(3) 0.3466(2) 0.99942(18) 0.0380(11) Uani 1 1 d . . . H60A H 0.0269 0.3716 0.9668 0.057 Uiso 1 1 calc R . . H60B H 0.1352 0.3659 1.0080 0.057 Uiso 1 1 calc R . . H60C H 0.0773 0.3516 1.0333 0.057 Uiso 1 1 calc R . . C61A C 0.2278(7) 0.5640(5) 0.4018(5) 0.0415(10) Uiso 0.50 1 d PD C -1 H61A H 0.2729 0.5430 0.4393 0.062 Uiso 0.50 1 calc PR C -1 H61B H 0.2565 0.5757 0.3823 0.062 Uiso 0.50 1 calc PR C -1 H61C H 0.1782 0.5311 0.3781 0.062 Uiso 0.50 1 calc PR C -1 C62A C 0.1919(8) 0.6269(7) 0.4102(6) 0.0415(10) Uiso 0.50 1 d PD C -1 H62A H 0.1418 0.6460 0.3725 0.050 Uiso 0.50 1 calc PR C -1 H62B H 0.2401 0.6624 0.4306 0.050 Uiso 0.50 1 calc PR C -1 C63A C 0.1568(6) 0.6063(4) 0.4466(4) 0.0415(10) Uiso 0.50 1 d PD C -1 H63A H 0.1163 0.5657 0.4282 0.050 Uiso 0.50 1 calc PR C -1 H63B H 0.2094 0.5914 0.4852 0.050 Uiso 0.50 1 calc PR C -1 C64A C 0.1073(5) 0.6604(5) 0.4547(4) 0.0415(10) Uiso 0.50 1 d PD C -1 H64A H 0.1449 0.7029 0.4686 0.050 Uiso 0.50 1 calc PR C -1 H64B H 0.1017 0.6449 0.4857 0.050 Uiso 0.50 1 calc PR C -1 C65A C 0.0157(5) 0.6791(4) 0.4040(4) 0.0415(10) Uiso 0.50 1 d PD C -1 H65A H -0.0044 0.7211 0.4137 0.050 Uiso 0.50 1 calc PR C -1 H65B H 0.0205 0.6917 0.3721 0.050 Uiso 0.50 1 calc PR C -1 C66A C -0.0550(6) 0.6267(4) 0.3827(4) 0.0415(10) Uiso 0.50 1 d PD C -1 H66A H -0.0460 0.5906 0.3622 0.062 Uiso 0.50 1 calc PR C -1 H66B H -0.1146 0.6482 0.3564 0.062 Uiso 0.50 1 calc PR C -1 H66C H -0.0517 0.6059 0.4153 0.062 Uiso 0.50 1 calc PR C -1 C61B C 0.2525(17) 0.5526(12) 0.3995(11) 0.063(3) Uiso 0.25 1 d PD D -2 H61D H 0.2698 0.5036 0.4051 0.094 Uiso 0.25 1 calc PR D -2 H61E H 0.3070 0.5814 0.4163 0.094 Uiso 0.25 1 calc PR D -2 H61F H 0.2109 0.5625 0.3581 0.094 Uiso 0.25 1 calc PR D -2 C62B C 0.2108(15) 0.5672(9) 0.4257(10) 0.063(3) Uiso 0.25 1 d PD D -2 H62C H 0.2520 0.5561 0.4673 0.075 Uiso 0.25 1 calc PR D -2 H62D H 0.1554 0.5385 0.4086 0.075 Uiso 0.25 1 calc PR D -2 C63B C 0.1859(15) 0.6425(10) 0.4180(12) 0.063(3) Uiso 0.25 1 d PD D -2 H63C H 0.2396 0.6703 0.4468 0.075 Uiso 0.25 1 calc PR D -2 H63D H 0.1656 0.6578 0.3790 0.075 Uiso 0.25 1 calc PR D -2 C64B C 0.1148(12) 0.6527(10) 0.4252(10) 0.063(3) Uiso 0.25 1 d PD D -2 H64C H 0.1381 0.6364 0.4645 0.075 Uiso 0.25 1 calc PR D -2 H64D H 0.1061 0.7034 0.4249 0.075 Uiso 0.25 1 calc PR D -2 C65B C 0.0304(12) 0.6242(12) 0.3887(8) 0.063(3) Uiso 0.25 1 d PD D -2 H65C H 0.0338 0.5855 0.3672 0.075 Uiso 0.25 1 calc PR D -2 H65D H -0.0114 0.6596 0.3603 0.075 Uiso 0.25 1 calc PR D -2 C66B C -0.0082(14) 0.5969(12) 0.4222(9) 0.063(3) Uiso 0.25 1 d PD D -2 H66D H -0.0063 0.5461 0.4231 0.094 Uiso 0.25 1 calc PR D -2 H66E H -0.0712 0.6124 0.4027 0.094 Uiso 0.25 1 calc PR D -2 H66F H 0.0285 0.6149 0.4617 0.094 Uiso 0.25 1 calc PR D -2 C61C C 0.1699(12) 0.6257(13) 0.4077(10) 0.0341(18) Uiso 0.25 1 d PD E -3 H61G H 0.1836 0.5775 0.4045 0.051 Uiso 0.25 1 calc PR E -3 H61H H 0.2174 0.6438 0.4459 0.051 Uiso 0.25 1 calc PR E -3 H61I H 0.1672 0.6537 0.3780 0.051 Uiso 0.25 1 calc PR E -3 C62C C 0.0777(10) 0.6290(9) 0.3992(7) 0.0341(18) Uiso 0.25 1 d PD E -3 H62E H 0.0567 0.6776 0.3943 0.041 Uiso 0.25 1 calc PR E -3 H62F H 0.0313 0.6020 0.3648 0.041 Uiso 0.25 1 calc PR E -3 C63C C 0.0945(10) 0.5980(9) 0.4533(6) 0.0341(18) Uiso 0.25 1 d PD E -3 H63E H 0.1344 0.5571 0.4645 0.041 Uiso 0.25 1 calc PR E -3 H63F H 0.1268 0.6324 0.4848 0.041 Uiso 0.25 1 calc PR E -3 C64C C 0.0099(10) 0.5767(8) 0.4466(6) 0.0341(18) Uiso 0.25 1 d PD E -3 H64E H -0.0284 0.6187 0.4356 0.041 Uiso 0.25 1 calc PR E -3 H64F H -0.0227 0.5446 0.4133 0.041 Uiso 0.25 1 calc PR E -3 C65C C 0.0120(11) 0.5496(7) 0.4854(7) 0.0341(18) Uiso 0.25 1 d PD E -3 H65E H -0.0301 0.5795 0.4881 0.041 Uiso 0.25 1 calc PR E -3 H65F H 0.0732 0.5629 0.5191 0.041 Uiso 0.25 1 calc PR E -3 C66C C -0.0002(15) 0.4846(7) 0.5038(9) 0.0341(18) Uiso 0.25 1 d PD E -3 H66G H -0.0376 0.4910 0.5182 0.051 Uiso 0.25 1 calc PR E -3 H66H H 0.0591 0.4659 0.5346 0.051 Uiso 0.25 1 calc PR E -3 H66I H -0.0304 0.4523 0.4711 0.051 Uiso 0.25 1 calc PR E -3 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 Sc1 0.0166(4) 0.0162(4) 0.0174(3) -0.0015(3) 0.0110(3) -0.0001(3) Sc2 0.0170(4) 0.0131(3) 0.0175(3) 0.0002(3) 0.0113(3) 0.0004(3) Sc3 0.0189(4) 0.0140(3) 0.0156(3) 0.0012(3) 0.0095(3) -0.0015(3) N1 0.0228(17) 0.0133(15) 0.0285(17) 0.0008(13) 0.0175(15) 0.0009(13) N2 0.0245(17) 0.0189(16) 0.0223(16) 0.0024(13) 0.0142(15) 0.0075(13) N3 0.0199(17) 0.0286(18) 0.0216(17) -0.0039(14) 0.0120(15) 0.0025(14) N4 0.0199(17) 0.0279(18) 0.0232(17) -0.0070(14) 0.0102(15) -0.0020(14) N5 0.0223(17) 0.0140(15) 0.0207(16) -0.0007(12) 0.0126(14) 0.0024(13) N6 0.0206(18) 0.034(2) 0.039(2) 0.0089(17) 0.0114(17) -0.0005(15) N7 0.0275(18) 0.0273(18) 0.0266(17) -0.0018(14) 0.0190(16) -0.0049(14) N8 0.0269(18) 0.0274(18) 0.0215(17) -0.0006(14) 0.0161(15) 0.0017(14) N9 0.0332(19) 0.0216(17) 0.0308(18) 0.0011(14) 0.0260(16) -0.0023(14) N10 0.046(2) 0.0231(18) 0.0166(17) 0.0012(14) 0.0090(16) -0.0092(16) N11 0.0297(19) 0.0170(17) 0.0253(17) 0.0023(14) 0.0132(15) -0.0032(14) N12 0.0260(18) 0.0245(18) 0.0242(17) 0.0006(14) 0.0126(15) -0.0051(14) C1 0.030(2) 0.030(2) 0.028(2) -0.0068(18) 0.0195(19) -0.0016(18) C2 0.032(2) 0.036(2) 0.028(2) -0.0134(19) 0.017(2) -0.0067(19) C3 0.034(2) 0.029(2) 0.044(3) -0.015(2) 0.025(2) -0.0141(19) C4 0.033(2) 0.025(2) 0.048(3) -0.0156(19) 0.031(2) -0.0152(18) C5 0.044(3) 0.025(2) 0.044(3) 0.0130(19) 0.033(2) 0.0092(19) C6 0.037(3) 0.032(2) 0.033(2) 0.0120(19) 0.022(2) 0.0105(19) C7 0.026(2) 0.040(3) 0.029(2) 0.0049(19) 0.016(2) 0.0125(19) C8 0.024(2) 0.040(3) 0.032(2) 0.0000(19) 0.0178(19) 0.0081(19) C9 0.036(3) 0.032(2) 0.023(2) 0.0021(18) 0.010(2) 0.0128(19) C10 0.024(2) 0.056(3) 0.040(3) -0.010(2) 0.008(2) -0.002(2) C15 0.045(3) 0.023(2) 0.038(2) -0.0011(18) 0.033(2) -0.0028(19) C16 0.045(3) 0.029(2) 0.029(2) 0.0063(18) 0.027(2) 0.0032(19) C17 0.041(3) 0.026(2) 0.027(2) -0.0053(17) 0.023(2) -0.0001(19) C18 0.044(3) 0.020(2) 0.037(2) -0.0081(18) 0.029(2) -0.0088(18) C20 0.028(2) 0.037(2) 0.020(2) -0.0030(17) 0.0128(18) 0.0008(18) C21 0.040(3) 0.022(2) 0.034(2) -0.0055(18) 0.024(2) -0.0077(18) C22 0.033(2) 0.022(2) 0.033(2) -0.0089(18) 0.019(2) -0.0113(18) C23 0.027(2) 0.035(2) 0.046(3) -0.007(2) 0.025(2) -0.0065(19) C24 0.034(3) 0.027(2) 0.071(3) -0.006(2) 0.041(3) -0.0034(19) C25 0.091(4) 0.039(3) 0.046(3) -0.001(2) 0.055(3) 0.002(3) C29 0.020(2) 0.032(2) 0.032(2) 0.0044(18) 0.0084(19) -0.0027(18) Sc4 0.0148(3) 0.0142(3) 0.0165(3) -0.0012(3) 0.0091(3) -0.0013(3) Sc5 0.0128(3) 0.0138(3) 0.0140(3) -0.0014(3) 0.0079(3) -0.0013(3) Sc6 0.0152(4) 0.0152(4) 0.0153(3) -0.0003(3) 0.0081(3) -0.0020(3) N13 0.0223(17) 0.0189(16) 0.0207(16) -0.0037(13) 0.0128(14) -0.0030(13) N14 0.0216(17) 0.0192(16) 0.0225(16) 0.0011(13) 0.0135(14) 0.0009(13) N15 0.0173(16) 0.0152(15) 0.0221(16) 0.0012(13) 0.0105(14) -0.0018(12) N16 0.0182(16) 0.0190(16) 0.0186(16) -0.0008(13) 0.0089(14) -0.0022(13) N17 0.0137(15) 0.0192(16) 0.0152(15) 0.0009(12) 0.0084(13) 0.0012(12) N18 0.0135(15) 0.0162(15) 0.0156(15) -0.0009(12) 0.0077(13) 0.0009(12) N19 0.0172(16) 0.0167(15) 0.0142(15) -0.0025(12) 0.0089(13) -0.0013(12) N20 0.0168(16) 0.0187(16) 0.0179(15) 0.0005(12) 0.0104(14) -0.0009(12) N21 0.0232(17) 0.0167(16) 0.0170(15) -0.0001(12) 0.0106(14) -0.0005(13) N22 0.035(2) 0.0228(18) 0.0212(17) -0.0066(14) 0.0144(16) -0.0101(15) N23 0.0185(17) 0.0280(18) 0.0265(18) 0.0034(14) 0.0102(15) -0.0025(14) N24 0.0273(18) 0.0185(16) 0.0268(17) 0.0029(14) 0.0192(15) 0.0020(14) C31 0.030(2) 0.020(2) 0.0165(19) -0.0025(16) 0.0084(18) 0.0023(17) C32 0.029(2) 0.029(2) 0.023(2) 0.0012(17) 0.0176(19) 0.0084(17) C33 0.021(2) 0.0187(19) 0.031(2) -0.0001(16) 0.0169(18) 0.0017(16) C34 0.0175(19) 0.0190(19) 0.022(2) 0.0025(15) 0.0083(17) 0.0010(15) C35 0.024(2) 0.019(2) 0.0197(19) 0.0034(15) 0.0096(17) 0.0013(16) C36 0.026(2) 0.020(2) 0.0207(19) 0.0039(16) 0.0126(18) -0.0031(16) C37 0.021(2) 0.019(2) 0.022(2) -0.0013(16) 0.0088(17) -0.0069(16) C38 0.023(2) 0.024(2) 0.0176(19) -0.0030(16) 0.0060(17) -0.0080(16) C39 0.031(2) 0.023(2) 0.044(2) 0.0003(18) 0.029(2) -0.0006(17) C40 0.023(2) 0.026(2) 0.030(2) -0.0051(17) 0.0152(19) -0.0068(17) C41 0.0161(19) 0.0178(19) 0.0211(19) -0.0011(15) 0.0113(16) -0.0027(15) C42 0.0133(18) 0.024(2) 0.0219(19) -0.0027(16) 0.0112(16) -0.0016(15) C43 0.0181(19) 0.0156(19) 0.026(2) 0.0001(15) 0.0138(17) 0.0008(15) C44 0.022(2) 0.0166(19) 0.025(2) -0.0044(15) 0.0155(17) -0.0009(15) C45 0.022(2) 0.0191(19) 0.0166(18) -0.0057(15) 0.0091(17) -0.0048(16) C46 0.023(2) 0.024(2) 0.0142(18) -0.0050(15) 0.0099(16) -0.0044(16) C47 0.022(2) 0.0208(19) 0.0131(17) 0.0004(15) 0.0096(16) -0.0002(16) C48 0.021(2) 0.0202(19) 0.0198(19) -0.0015(15) 0.0134(17) -0.0031(15) C49 0.019(2) 0.025(2) 0.0151(18) -0.0015(15) 0.0063(16) -0.0015(16) C50 0.017(2) 0.031(2) 0.024(2) 0.0016(17) 0.0096(17) -0.0010(17) C51 0.027(2) 0.019(2) 0.035(2) 0.0011(18) 0.010(2) 0.0020(17) C52 0.044(3) 0.017(2) 0.033(2) -0.0028(18) 0.020(2) -0.0058(18) C53 0.034(3) 0.038(3) 0.028(2) -0.009(2) 0.007(2) -0.015(2) C54 0.024(2) 0.028(2) 0.050(3) 0.004(2) 0.010(2) -0.0049(19) C55 0.021(2) 0.062(3) 0.044(3) 0.023(2) 0.022(2) 0.013(2) C56 0.052(3) 0.059(3) 0.063(3) -0.014(3) 0.047(3) -0.012(3) C57 0.066(3) 0.053(3) 0.034(3) 0.014(2) 0.031(3) 0.024(3) C58 0.029(2) 0.048(3) 0.023(2) 0.0095(19) 0.0135(19) 0.017(2) C59 0.054(3) 0.022(2) 0.042(3) -0.0090(19) 0.033(2) -0.009(2) C60 0.059(3) 0.029(2) 0.040(3) -0.010(2) 0.037(2) -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 N3 2.088(3) . ? Sc1 N1 2.204(3) . ? Sc1 N9 2.232(3) . ? Sc1 N2 2.421(3) . ? Sc1 N4 2.498(3) . ? Sc1 Sc3 3.2860(9) . ? Sc1 Sc2 3.2865(9) . ? Sc1 H1 2.16(3) . ? Sc1 H2 2.23(3) . ? Sc2 N7 2.069(3) . ? Sc2 N1 2.210(3) . ? Sc2 N5 2.238(3) . ? Sc2 N8 2.435(3) . ? Sc2 N6 2.510(3) . ? Sc2 Sc3 3.2488(9) . ? Sc2 H1 2.24(3) . ? Sc2 H2 2.18(3) . ? Sc3 N11 2.082(3) . ? Sc3 N5 2.224(3) . ? Sc3 N9 2.238(3) . ? Sc3 N12 2.415(3) . ? Sc3 N10 2.449(3) . ? Sc3 H1 2.19(3) . ? Sc3 H2 2.17(3) . ? N1 C5 1.479(5) . ? N1 C4 1.481(5) . ? N2 C9 1.468(5) . ? N2 C6 1.485(5) . ? N2 C7 1.499(5) . ? N3 C1 1.443(4) . ? N3 C8 1.452(5) . ? N4 C10 1.476(5) . ? N4 C3 1.487(5) . ? N4 C2 1.488(5) . ? N5 C11B 1.458(12) . ? N5 C18 1.470(4) . ? N5 C11A 1.472(7) . ? N6 C19B 1.456(16) . ? N6 C12B 1.460(11) . ? N6 C19A 1.475(7) . ? N6 C13A 1.502(7) . ? N6 C12A 1.510(7) . ? N6 C13B 1.513(19) . ? N7 C15 1.436(5) . ? N7 C14A 1.456(8) . ? N7 C14B 1.473(16) . ? N8 C17 1.469(5) . ? N8 C20 1.474(5) . ? N8 C16 1.498(5) . ? N9 C25 1.467(5) . ? N9 C24 1.484(5) . ? N10 C26A 1.408(7) . ? N10 C30B 1.425(12) . ? N10 C30A 1.496(8) . ? N10 C27A 1.517(7) . ? N10 C27B 1.519(12) . ? N10 C26B 1.591(12) . ? N11 C28A 1.430(9) . ? N11 C21 1.441(5) . ? N11 C28B 1.520(15) . ? N12 C29 1.477(5) . ? N12 C23 1.482(5) . ? N12 C22 1.492(5) . ? C1 C2 1.490(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.525(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.511(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.486(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11A C12A 1.448(9) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C13A C14A 1.540(9) . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C11B C12B 1.588(17) . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? C13B C14B 1.42(2) . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15 C16 1.487(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.520(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.489(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.541(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26B 1.278(12) . ? C25 C26A 1.544(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? C27A C28A 1.531(11) . ? C27A H27A 0.9900 . ? C27A H27B 0.9900 . ? C28A H28A 0.9900 . ? C28A H28B 0.9900 . ? C26B H26C 0.9900 . ? C26B H26D 0.9900 . ? C27B C28B 1.585(19) . ? C27B H27C 0.9900 . ? C27B H27D 0.9900 . ? C28B H28C 0.9900 . ? C28B H28D 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30A H30A 0.9800 . ? C30A H30B 0.9800 . ? C30A H30C 0.9800 . ? C30B H30D 0.9800 . ? C30B H30E 0.9800 . ? C30B H30F 0.9800 . ? Sc4 N13 2.139(3) . ? Sc4 N15 2.140(3) . ? Sc4 N17 2.246(3) . ? Sc4 N14 2.464(3) . ? Sc4 N16 2.670(3) . ? Sc4 Sc5 3.0869(9) . ? Sc4 H3 2.08(3) . ? Sc4 H4 2.04(3) . ? Sc5 N17 2.317(3) . ? Sc5 N19 2.324(3) . ? Sc5 N20 2.443(3) . ? Sc5 N18 2.461(3) . ? Sc5 Sc6 3.0837(9) . ? Sc5 H3 2.01(3) . ? Sc5 H4 1.97(3) . ? Sc5 H5 1.98(3) . ? Sc5 H6 1.92(3) . ? Sc6 N23 2.135(3) . ? Sc6 N21 2.145(3) . ? Sc6 N19 2.267(3) . ? Sc6 N24 2.427(3) . ? Sc6 N22 2.561(3) . ? Sc6 H5 1.99(3) . ? Sc6 H6 1.98(3) . ? N13 C31 1.440(4) . ? N13 C38 1.453(4) . ? N14 C39 1.474(5) . ? N14 C32 1.476(4) . ? N14 C33 1.480(4) . ? N15 C34 1.444(4) . ? N15 C35 1.444(4) . ? N16 C40 1.467(5) . ? N16 C37 1.475(4) . ? N16 C36 1.483(4) . ? N17 C48 1.464(4) . ? N17 C41 1.464(4) . ? N18 C43 1.473(4) . ? N18 C42 1.474(4) . ? N18 C49 1.475(4) . ? N19 C44 1.454(4) . ? N19 C45 1.465(4) . ? N20 C46 1.475(4) . ? N20 C50 1.478(4) . ? N20 C47 1.478(4) . ? N21 C58 1.431(5) . ? N21 C51 1.457(5) . ? N22 C52 1.466(5) . ? N22 C59 1.469(5) . ? N22 C53 1.500(5) . ? N23 C54 1.416(5) . ? N23 C55 1.468(5) . ? N24 C60 1.454(5) . ? N24 C56 1.457(5) . ? N24 C57 1.487(5) . ? C31 C32 1.514(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.531(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.497(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.526(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? 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 C42 1.517(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.515(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.516(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.510(5) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? 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 C52 1.514(5) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.482(6) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.483(6) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.447(6) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61A C62A 1.459(12) . ? C61A H61A 0.9800 . ? C61A H61B 0.9800 . ? C61A H61C 0.9800 . ? C62A C63A 1.548(11) . ? C62A H62A 0.9900 . ? C62A H62B 0.9900 . ? C63A C64A 1.477(10) . ? C63A H63A 0.9900 . ? C63A H63B 0.9900 . ? C64A C65A 1.478(10) . ? C64A H64A 0.9900 . ? C64A H64B 0.9900 . ? C65A C66A 1.458(10) . ? C65A H65A 0.9900 . ? C65A H65B 0.9900 . ? C66A H66A 0.9800 . ? C66A H66B 0.9800 . ? C66A H66C 0.9800 . ? C61B C62B 1.362(17) . ? C61B H61D 0.9800 . ? C61B H61E 0.9800 . ? C61B H61F 0.9800 . ? C62B C63B 1.499(17) . ? C62B H62C 0.9900 . ? C62B H62D 0.9900 . ? C63B C64B 1.427(16) . ? C63B H63C 0.9900 . ? C63B H63D 0.9900 . ? C64B C65B 1.369(16) . ? C64B H64C 0.9900 . ? C64B H64D 0.9900 . ? C65B C66B 1.563(16) . ? C65B H65C 0.9900 . ? C65B H65D 0.9900 . ? C66B H66D 0.9800 . ? C66B H66E 0.9800 . ? C66B H66F 0.9800 . ? C61C C62C 1.539(16) . ? C61C H61G 0.9800 . ? C61C H61H 0.9800 . ? C61C H61I 0.9800 . ? C62C C63C 1.508(15) . ? C62C H62E 0.9900 . ? C62C H62F 0.9900 . ? C63C C64C 1.485(14) . ? C63C H63E 0.9900 . ? C63C H63F 0.9900 . ? C64C C65C 1.203(13) . ? C64C H64E 0.9900 . ? C64C H64F 0.9900 . ? C65C C66C 1.421(14) . ? C65C H65E 0.9900 . ? C65C H65F 0.9900 . ? C66C H66G 0.9800 . ? C66C H66H 0.9800 . ? C66C H66I 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 N3 Sc1 N1 110.84(12) . . ? N3 Sc1 N9 105.35(12) . . ? N1 Sc1 N9 143.70(11) . . ? N3 Sc1 N2 73.09(11) . . ? N1 Sc1 N2 78.75(11) . . ? N9 Sc1 N2 110.00(11) . . ? N3 Sc1 N4 71.46(11) . . ? N1 Sc1 N4 77.40(11) . . ? N9 Sc1 N4 117.86(11) . . ? N2 Sc1 N4 125.96(10) . . ? N3 Sc1 Sc3 147.98(9) . . ? N1 Sc1 Sc3 101.18(8) . . ? N9 Sc1 Sc3 42.74(8) . . ? N2 Sc1 Sc3 115.34(7) . . ? N4 Sc1 Sc3 116.47(7) . . ? N3 Sc1 Sc2 152.72(9) . . ? N1 Sc1 Sc2 41.94(7) . . ? N9 Sc1 Sc2 101.92(8) . . ? N2 Sc1 Sc2 97.75(7) . . ? N4 Sc1 Sc2 95.66(7) . . ? Sc3 Sc1 Sc2 59.247(19) . . ? N3 Sc1 H1 150.0(9) . . ? N1 Sc1 H1 74.6(9) . . ? N9 Sc1 H1 72.8(9) . . ? N2 Sc1 H1 79.5(9) . . ? N4 Sc1 H1 136.8(9) . . ? Sc3 Sc1 H1 41.3(9) . . ? Sc2 Sc1 H1 42.5(9) . . ? N3 Sc1 H2 148.6(8) . . ? N1 Sc1 H2 74.7(8) . . ? N9 Sc1 H2 76.0(8) . . ? N2 Sc1 H2 136.9(8) . . ? N4 Sc1 H2 80.2(8) . . ? Sc3 Sc1 H2 41.1(8) . . ? Sc2 Sc1 H2 41.2(8) . . ? H1 Sc1 H2 61.1(12) . . ? N7 Sc2 N1 99.28(12) . . ? N7 Sc2 N5 115.60(12) . . ? N1 Sc2 N5 145.09(11) . . ? N7 Sc2 N8 73.73(11) . . ? N1 Sc2 N8 112.32(11) . . ? N5 Sc2 N8 78.07(10) . . ? N7 Sc2 N6 73.40(12) . . ? N1 Sc2 N6 118.71(12) . . ? N5 Sc2 N6 75.39(11) . . ? N8 Sc2 N6 122.36(11) . . ? N7 Sc2 Sc3 158.42(9) . . ? N1 Sc2 Sc3 102.17(8) . . ? N5 Sc2 Sc3 43.09(8) . . ? N8 Sc2 Sc3 100.00(8) . . ? N6 Sc2 Sc3 94.01(8) . . ? N7 Sc2 Sc1 140.96(9) . . ? N1 Sc2 Sc1 41.81(8) . . ? N5 Sc2 Sc1 103.41(8) . . ? N8 Sc2 Sc1 118.05(8) . . ? N6 Sc2 Sc1 117.45(9) . . ? Sc3 Sc2 Sc1 60.37(2) . . ? N7 Sc2 H1 151.2(8) . . ? N1 Sc2 H1 73.0(8) . . ? N5 Sc2 H1 75.4(8) . . ? N8 Sc2 H1 83.6(8) . . ? N6 Sc2 H1 134.9(8) . . ? Sc3 Sc2 H1 42.2(8) . . ? Sc1 Sc2 H1 40.8(8) . . ? N7 Sc2 H2 145.5(9) . . ? N1 Sc2 H2 75.7(9) . . ? N5 Sc2 H2 76.2(9) . . ? N8 Sc2 H2 140.2(9) . . ? N6 Sc2 H2 79.3(9) . . ? Sc3 Sc2 H2 41.7(9) . . ? Sc1 Sc2 H2 42.5(9) . . ? H1 Sc2 H2 60.8(12) . . ? N11 Sc3 N5 100.89(12) . . ? N11 Sc3 N9 112.95(12) . . ? N5 Sc3 N9 146.05(11) . . ? N11 Sc3 N12 72.35(11) . . ? N5 Sc3 N12 109.47(11) . . ? N9 Sc3 N12 79.62(11) . . ? N11 Sc3 N10 72.76(11) . . ? N5 Sc3 N10 117.51(12) . . ? N9 Sc3 N10 76.87(12) . . ? N12 Sc3 N10 125.30(11) . . ? N11 Sc3 Sc2 144.06(9) . . ? N5 Sc3 Sc2 43.45(7) . . ? N9 Sc3 Sc2 102.93(8) . . ? N12 Sc3 Sc2 117.82(8) . . ? N10 Sc3 Sc2 115.29(8) . . ? N11 Sc3 Sc1 155.20(9) . . ? N5 Sc3 Sc1 103.79(8) . . ? N9 Sc3 Sc1 42.61(8) . . ? N12 Sc3 Sc1 101.35(8) . . ? N10 Sc3 Sc1 93.42(8) . . ? Sc2 Sc3 Sc1 60.38(2) . . ? N11 Sc3 H1 152.5(9) . . ? N5 Sc3 H1 76.6(9) . . ? N9 Sc3 H1 72.2(9) . . ? N12 Sc3 H1 82.6(9) . . ? N10 Sc3 H1 133.1(9) . . ? Sc2 Sc3 H1 43.4(9) . . ? Sc1 Sc3 H1 40.7(8) . . ? N11 Sc3 H2 145.2(9) . . ? N5 Sc3 H2 76.6(9) . . ? N9 Sc3 H2 77.0(9) . . ? N12 Sc3 H2 141.8(9) . . ? N10 Sc3 H2 77.8(9) . . ? Sc2 Sc3 H2 41.8(9) . . ? Sc1 Sc3 H2 42.5(9) . . ? H1 Sc3 H2 61.7(12) . . ? C5 N1 C4 113.9(3) . . ? C5 N1 Sc1 110.8(2) . . ? C4 N1 Sc1 112.6(2) . . ? C5 N1 Sc2 111.4(2) . . ? C4 N1 Sc2 110.6(2) . . ? Sc1 N1 Sc2 96.25(11) . . ? C9 N2 C6 109.6(3) . . ? C9 N2 C7 106.0(3) . . ? C6 N2 C7 111.6(3) . . ? C9 N2 Sc1 123.7(2) . . ? C6 N2 Sc1 99.9(2) . . ? C7 N2 Sc1 105.9(2) . . ? C1 N3 C8 107.6(3) . . ? C1 N3 Sc1 125.6(2) . . ? C8 N3 Sc1 123.3(2) . . ? C10 N4 C3 108.1(3) . . ? C10 N4 C2 106.2(3) . . ? C3 N4 C2 112.0(3) . . ? C10 N4 Sc1 127.4(2) . . ? C3 N4 Sc1 98.3(2) . . ? C2 N4 Sc1 104.5(2) . . ? C11B N5 C18 122.0(6) . . ? C18 N5 C11A 104.3(4) . . ? C11B N5 Sc3 101.1(6) . . ? C18 N5 Sc3 113.7(2) . . ? C11A N5 Sc3 122.2(3) . . ? C11B N5 Sc2 112.9(5) . . ? C18 N5 Sc2 109.7(2) . . ? C11A N5 Sc2 113.2(3) . . ? Sc3 N5 Sc2 93.45(11) . . ? C19B N6 C12B 107.6(8) . . ? C19A N6 C13A 110.3(4) . . ? C19A N6 C12A 105.3(4) . . ? C13A N6 C12A 113.0(4) . . ? C19B N6 C13B 103.8(10) . . ? C12B N6 C13B 115.7(10) . . ? C19B N6 Sc2 125.4(7) . . ? C12B N6 Sc2 101.6(5) . . ? C19A N6 Sc2 121.0(3) . . ? C13A N6 Sc2 103.5(3) . . ? C12A N6 Sc2 103.8(3) . . ? C13B N6 Sc2 103.4(8) . . ? C15 N7 C14A 113.0(4) . . ? C15 N7 C14B 101.5(7) . . ? C15 N7 Sc2 123.8(2) . . ? C14A N7 Sc2 118.1(3) . . ? C14B N7 Sc2 121.8(6) . . ? C17 N8 C20 110.1(3) . . ? C17 N8 C16 111.1(3) . . ? C20 N8 C16 105.2(3) . . ? C17 N8 Sc2 99.6(2) . . ? C20 N8 Sc2 125.0(2) . . ? C16 N8 Sc2 105.6(2) . . ? C25 N9 C24 111.4(3) . . ? C25 N9 Sc1 115.2(3) . . ? C24 N9 Sc1 114.0(2) . . ? C25 N9 Sc3 111.9(3) . . ? C24 N9 Sc3 108.5(2) . . ? Sc1 N9 Sc3 94.65(11) . . ? C26A N10 C30A 111.1(5) . . ? C26A N10 C27A 114.2(4) . . ? C30A N10 C27A 104.7(5) . . ? C30B N10 C27B 111.4(7) . . ? C30B N10 C26B 105.3(7) . . ? C27B N10 C26B 106.9(7) . . ? C26A N10 Sc3 99.9(3) . . ? C30B N10 Sc3 125.5(5) . . ? C30A N10 Sc3 122.6(4) . . ? C27A N10 Sc3 104.5(3) . . ? C27B N10 Sc3 104.7(5) . . ? C26B N10 Sc3 101.4(5) . . ? C28A N11 C21 106.5(4) . . ? C21 N11 C28B 112.8(6) . . ? C28A N11 Sc3 123.0(4) . . ? C21 N11 Sc3 125.4(2) . . ? C28B N11 Sc3 120.4(6) . . ? C29 N12 C23 108.7(3) . . ? C29 N12 C22 106.2(3) . . ? C23 N12 C22 111.2(3) . . ? C29 N12 Sc3 124.5(2) . . ? C23 N12 Sc3 99.3(2) . . ? C22 N12 Sc3 106.7(2) . . ? N3 C1 C2 110.3(3) . . ? N3 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? N3 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? N4 C2 C1 111.3(3) . . ? N4 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N4 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N4 C3 C4 110.3(3) . . ? N4 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N4 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? N1 C4 C3 112.6(3) . . ? N1 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? N1 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? N1 C5 C6 113.4(3) . . ? N1 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N1 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N2 C6 C5 110.7(3) . . ? N2 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 N2 110.9(3) . . ? C8 C7 H7A 109.5 . . ? N2 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 108.0 . . ? N3 C8 C7 111.4(3) . . ? N3 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? N3 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N4 C10 H10A 109.5 . . ? N4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12A C11A N5 112.9(5) . . ? C12A C11A H11A 109.0 . . ? N5 C11A H11A 109.0 . . ? C12A C11A H11B 109.0 . . ? N5 C11A H11B 109.0 . . ? H11A C11A H11B 107.8 . . ? C11A C12A N6 113.9(5) . . ? C11A C12A H12A 108.8 . . ? N6 C12A H12A 108.8 . . ? C11A C12A H12B 108.8 . . ? N6 C12A H12B 108.8 . . ? H12A C12A H12B 107.7 . . ? N6 C13A C14A 104.9(5) . . ? N6 C13A H13A 110.8 . . ? C14A C13A H13A 110.8 . . ? N6 C13A H13B 110.8 . . ? C14A C13A H13B 110.8 . . ? H13A C13A H13B 108.8 . . ? N7 C14A C13A 104.8(5) . . ? N7 C14A H14A 110.8 . . ? C13A C14A H14A 110.8 . . ? N7 C14A H14B 110.8 . . ? C13A C14A H14B 110.8 . . ? H14A C14A H14B 108.9 . . ? N5 C11B C12B 108.9(9) . . ? N5 C11B H11C 109.9 . . ? C12B C11B H11C 109.9 . . ? N5 C11B H11D 109.9 . . ? C12B C11B H11D 109.9 . . ? H11C C11B H11D 108.3 . . ? N6 C12B C11B 106.6(9) . . ? N6 C12B H12C 110.4 . . ? C11B C12B H12C 110.4 . . ? N6 C12B H12D 110.4 . . ? C11B C12B H12D 110.4 . . ? H12C C12B H12D 108.6 . . ? C14B C13B N6 111.2(14) . . ? C14B C13B H13C 109.4 . . ? N6 C13B H13C 109.4 . . ? C14B C13B H13D 109.4 . . ? N6 C13B H13D 109.4 . . ? H13C C13B H13D 108.0 . . ? C13B C14B N7 113.8(13) . . ? C13B C14B H14C 108.8 . . ? N7 C14B H14C 108.8 . . ? C13B C14B H14D 108.8 . . ? N7 C14B H14D 108.8 . . ? H14C C14B H14D 107.7 . . ? N7 C15 C16 110.6(3) . . ? N7 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? N7 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C15 C16 N8 111.6(3) . . ? C15 C16 H16A 109.3 . . ? N8 C16 H16A 109.3 . . ? C15 C16 H16B 109.3 . . ? N8 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? N8 C17 C18 109.7(3) . . ? N8 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? N8 C17 H17B 109.7 . . ? C18 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? N5 C18 C17 112.3(3) . . ? N5 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? N5 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? N6 C19A H19A 109.5 . . ? N6 C19A H19B 109.5 . . ? N6 C19A H19C 109.5 . . ? N6 C19B H19D 109.5 . . ? N6 C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? N6 C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? N8 C20 H20A 109.5 . . ? N8 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N8 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N11 C21 C22 109.4(3) . . ? N11 C21 H21A 109.8 . . ? C22 C21 H21A 109.8 . . ? N11 C21 H21B 109.8 . . ? C22 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? C21 C22 N12 111.4(3) . . ? C21 C22 H22A 109.4 . . ? N12 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? N12 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? N12 C23 C24 109.7(3) . . ? N12 C23 H23A 109.7 . . ? C24 C23 H23A 109.7 . . ? N12 C23 H23B 109.7 . . ? C24 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? N9 C24 C23 112.4(3) . . ? N9 C24 H24A 109.1 . . ? C23 C24 H24A 109.1 . . ? N9 C24 H24B 109.1 . . ? C23 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? C26B C25 N9 118.1(7) . . ? N9 C25 C26A 113.7(4) . . ? N9 C25 H25A 108.8 . . ? C26A C25 H25A 108.8 . . ? N9 C25 H25B 108.8 . . ? C26A C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? N10 C26A C25 113.6(5) . . ? N10 C26A H26A 108.8 . . ? C25 C26A H26A 108.8 . . ? N10 C26A H26B 108.8 . . ? C25 C26A H26B 108.8 . . ? H26A C26A H26B 107.7 . . ? N10 C27A C28A 106.1(5) . . ? N10 C27A H27A 110.5 . . ? C28A C27A H27A 110.5 . . ? N10 C27A H27B 110.5 . . ? C28A C27A H27B 110.5 . . ? H27A C27A H27B 108.7 . . ? N11 C28A C27A 112.1(6) . . ? N11 C28A H28A 109.2 . . ? C27A C28A H28A 109.2 . . ? N11 C28A H28B 109.2 . . ? C27A C28A H28B 109.2 . . ? H28A C28A H28B 107.9 . . ? C25 C26B N10 118.5(9) . . ? C25 C26B H26C 107.7 . . ? N10 C26B H26C 107.7 . . ? C25 C26B H26D 107.7 . . ? N10 C26B H26D 107.7 . . ? H26C C26B H26D 107.1 . . ? N10 C27B C28B 105.1(9) . . ? N10 C27B H27C 110.7 . . ? C28B C27B H27C 110.7 . . ? N10 C27B H27D 110.7 . . ? C28B C27B H27D 110.7 . . ? H27C C27B H27D 108.8 . . ? N11 C28B C27B 97.3(9) . . ? N11 C28B H28C 112.3 . . ? C27B C28B H28C 112.3 . . ? N11 C28B H28D 112.3 . . ? C27B C28B H28D 112.3 . . ? H28C C28B H28D 109.9 . . ? N12 C29 H29A 109.5 . . ? N12 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N12 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N10 C30A H30A 109.5 . . ? N10 C30A H30B 109.5 . . ? N10 C30A H30C 109.5 . . ? N10 C30B H30D 109.5 . . ? N10 C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? N10 C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? N13 Sc4 N15 108.95(11) . . ? N13 Sc4 N17 125.49(11) . . ? N15 Sc4 N17 110.75(11) . . ? N13 Sc4 N14 74.34(10) . . ? N15 Sc4 N14 76.51(10) . . ? N17 Sc4 N14 150.67(10) . . ? N13 Sc4 N16 72.48(10) . . ? N15 Sc4 N16 71.71(10) . . ? N17 Sc4 N16 86.24(10) . . ? N14 Sc4 N16 122.40(10) . . ? N13 Sc4 Sc5 129.58(8) . . ? N15 Sc4 Sc5 119.38(8) . . ? N17 Sc4 Sc5 48.40(7) . . ? N14 Sc4 Sc5 102.73(7) . . ? N16 Sc4 Sc5 134.64(7) . . ? N13 Sc4 H3 90.2(9) . . ? N15 Sc4 H3 148.3(9) . . ? N17 Sc4 H3 74.4(9) . . ? N14 Sc4 H3 85.2(9) . . ? N16 Sc4 H3 139.6(9) . . ? Sc5 Sc4 H3 40.2(9) . . ? N13 Sc4 H4 144.2(9) . . ? N15 Sc4 H4 85.0(9) . . ? N17 Sc4 H4 75.1(9) . . ? N14 Sc4 H4 77.4(9) . . ? N16 Sc4 H4 142.8(9) . . ? Sc5 Sc4 H4 38.9(9) . . ? H3 Sc4 H4 65.7(13) . . ? N17 Sc5 N19 115.44(10) . . ? N17 Sc5 N20 74.72(10) . . ? N19 Sc5 N20 74.56(9) . . ? N17 Sc5 N18 74.40(9) . . ? N19 Sc5 N18 74.02(9) . . ? N20 Sc5 N18 119.63(9) . . ? N17 Sc5 Sc6 161.26(7) . . ? N19 Sc5 Sc6 47.03(7) . . ? N20 Sc5 Sc6 102.20(7) . . ? N18 Sc5 Sc6 91.96(7) . . ? N17 Sc5 Sc4 46.48(7) . . ? N19 Sc5 Sc4 160.89(7) . . ? N20 Sc5 Sc4 92.14(7) . . ? N18 Sc5 Sc4 102.03(7) . . ? Sc6 Sc5 Sc4 151.73(3) . . ? N17 Sc5 H3 74.1(9) . . ? N19 Sc5 H3 150.9(9) . . ? N20 Sc5 H3 133.6(9) . . ? N18 Sc5 H3 83.2(9) . . ? Sc6 Sc5 H3 117.8(9) . . ? Sc4 Sc5 H3 41.8(9) . . ? N17 Sc5 H4 74.8(10) . . ? N19 Sc5 H4 139.7(9) . . ? N20 Sc5 H4 71.0(9) . . ? N18 Sc5 H4 142.6(10) . . ? Sc6 Sc5 H4 122.3(10) . . ? Sc4 Sc5 H4 40.6(9) . . ? H3 Sc5 H4 68.2(13) . . ? N17 Sc5 H5 154.1(9) . . ? N19 Sc5 H5 73.5(9) . . ? N20 Sc5 H5 85.3(9) . . ? N18 Sc5 H5 130.8(9) . . ? Sc6 Sc5 H5 39.3(9) . . ? Sc4 Sc5 H5 119.9(9) . . ? H3 Sc5 H5 110.6(13) . . ? H4 Sc5 H5 83.3(13) . . ? N17 Sc5 H6 140.2(10) . . ? N19 Sc5 H6 72.4(10) . . ? N20 Sc5 H6 140.4(10) . . ? N18 Sc5 H6 70.7(10) . . ? Sc6 Sc5 H6 38.3(10) . . ? Sc4 Sc5 H6 124.7(10) . . ? H3 Sc5 H6 83.3(13) . . ? H4 Sc5 H6 126.2(13) . . ? H5 Sc5 H6 64.9(13) . . ? N23 Sc6 N21 108.37(12) . . ? N23 Sc6 N19 132.10(11) . . ? N21 Sc6 N19 106.58(11) . . ? N23 Sc6 N24 75.27(11) . . ? N21 Sc6 N24 75.44(10) . . ? N19 Sc6 N24 145.86(10) . . ? N23 Sc6 N22 70.88(12) . . ? N21 Sc6 N22 75.25(11) . . ? N19 Sc6 N22 87.78(10) . . ? N24 Sc6 N22 124.49(10) . . ? N23 Sc6 Sc5 128.25(9) . . ? N21 Sc6 Sc5 120.39(8) . . ? N19 Sc6 Sc5 48.59(7) . . ? N24 Sc6 Sc5 100.09(7) . . ? N22 Sc6 Sc5 135.42(7) . . ? N23 Sc6 H5 89.4(9) . . ? N21 Sc6 H5 151.1(9) . . ? N19 Sc6 H5 74.5(9) . . ? N24 Sc6 H5 87.9(9) . . ? N22 Sc6 H5 133.2(9) . . ? Sc5 Sc6 H5 39.0(9) . . ? N23 Sc6 H6 138.8(9) . . ? N21 Sc6 H6 88.8(9) . . ? N19 Sc6 H6 72.7(9) . . ? N24 Sc6 H6 73.3(9) . . ? N22 Sc6 H6 150.2(9) . . ? Sc5 Sc6 H6 37.0(9) . . ? H5 Sc6 H6 63.6(13) . . ? C31 N13 C38 112.1(3) . . ? C31 N13 Sc4 119.6(2) . . ? C38 N13 Sc4 116.9(2) . . ? C39 N14 C32 108.6(3) . . ? C39 N14 C33 110.1(3) . . ? C32 N14 C33 112.4(3) . . ? C39 N14 Sc4 116.3(2) . . ? C32 N14 Sc4 105.3(2) . . ? C33 N14 Sc4 104.0(2) . . ? C34 N15 C35 110.3(3) . . ? C34 N15 Sc4 112.9(2) . . ? C35 N15 Sc4 120.9(2) . . ? C40 N16 C37 107.8(3) . . ? C40 N16 C36 108.4(3) . . ? C37 N16 C36 112.1(3) . . ? C40 N16 Sc4 124.0(2) . . ? C37 N16 Sc4 102.0(2) . . ? C36 N16 Sc4 102.4(2) . . ? C48 N17 C41 111.1(3) . . ? C48 N17 Sc4 121.3(2) . . ? C41 N17 Sc4 112.7(2) . . ? C48 N17 Sc5 112.0(2) . . ? C41 N17 Sc5 112.0(2) . . ? Sc4 N17 Sc5 85.12(10) . . ? C43 N18 C42 111.9(3) . . ? C43 N18 C49 107.9(3) . . ? C42 N18 C49 110.0(3) . . ? C43 N18 Sc5 107.15(19) . . ? C42 N18 Sc5 106.55(19) . . ? C49 N18 Sc5 113.3(2) . . ? C44 N19 C45 110.3(3) . . ? C44 N19 Sc6 122.2(2) . . ? C45 N19 Sc6 113.2(2) . . ? C44 N19 Sc5 112.6(2) . . ? C45 N19 Sc5 111.7(2) . . ? Sc6 N19 Sc5 84.38(9) . . ? C46 N20 C50 110.0(3) . . ? C46 N20 C47 111.2(3) . . ? C50 N20 C47 108.4(3) . . ? C46 N20 Sc5 107.27(19) . . ? C50 N20 Sc5 112.9(2) . . ? C47 N20 Sc5 107.11(19) . . ? C58 N21 C51 111.3(3) . . ? C58 N21 Sc6 118.1(2) . . ? C51 N21 Sc6 116.4(2) . . ? C52 N22 C59 109.4(3) . . ? C52 N22 C53 111.0(3) . . ? C59 N22 C53 107.4(3) . . ? C52 N22 Sc6 99.8(2) . . ? C59 N22 Sc6 124.9(2) . . ? C53 N22 Sc6 104.0(2) . . ? C54 N23 C55 112.1(3) . . ? C54 N23 Sc6 125.9(3) . . ? C55 N23 Sc6 115.3(2) . . ? C60 N24 C56 110.8(3) . . ? C60 N24 C57 107.2(3) . . ? C56 N24 C57 111.6(3) . . ? C60 N24 Sc6 116.5(2) . . ? C56 N24 Sc6 106.5(2) . . ? C57 N24 Sc6 104.1(2) . . ? N13 C31 C32 109.3(3) . . ? N13 C31 H31A 109.8 . . ? C32 C31 H31A 109.8 . . ? N13 C31 H31B 109.8 . . ? C32 C31 H31B 109.8 . . ? H31A C31 H31B 108.3 . . ? N14 C32 C31 111.8(3) . . ? N14 C32 H32A 109.2 . . ? C31 C32 H32A 109.2 . . ? N14 C32 H32B 109.2 . . ? C31 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? N14 C33 C34 109.1(3) . . ? N14 C33 H33A 109.9 . . ? C34 C33 H33A 109.9 . . ? N14 C33 H33B 109.9 . . ? C34 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? N15 C34 C33 110.1(3) . . ? N15 C34 H34A 109.6 . . ? C33 C34 H34A 109.6 . . ? N15 C34 H34B 109.6 . . ? C33 C34 H34B 109.6 . . ? H34A C34 H34B 108.2 . . ? N15 C35 C36 110.4(3) . . ? N15 C35 H35A 109.6 . . ? C36 C35 H35A 109.6 . . ? N15 C35 H35B 109.6 . . ? C36 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? N16 C36 C35 112.3(3) . . ? N16 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? N16 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? N16 C37 C38 108.2(3) . . ? N16 C37 H37A 110.1 . . ? C38 C37 H37A 110.1 . . ? N16 C37 H37B 110.1 . . ? C38 C37 H37B 110.1 . . ? H37A C37 H37B 108.4 . . ? N13 C38 C37 110.1(3) . . ? N13 C38 H38A 109.6 . . ? C37 C38 H38A 109.6 . . ? N13 C38 H38B 109.6 . . ? C37 C38 H38B 109.6 . . ? H38A C38 H38B 108.2 . . ? N14 C39 H39A 109.5 . . ? N14 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N14 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N16 C40 H40A 109.5 . . ? N16 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N16 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N17 C41 C42 111.4(3) . . ? N17 C41 H41A 109.4 . . ? C42 C41 H41A 109.4 . . ? N17 C41 H41B 109.4 . . ? C42 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? N18 C42 C41 110.2(3) . . ? N18 C42 H42A 109.6 . . ? C41 C42 H42A 109.6 . . ? N18 C42 H42B 109.6 . . ? C41 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? N18 C43 C44 111.5(3) . . ? N18 C43 H43A 109.3 . . ? C44 C43 H43A 109.3 . . ? N18 C43 H43B 109.3 . . ? C44 C43 H43B 109.3 . . ? H43A C43 H43B 108.0 . . ? N19 C44 C43 110.8(3) . . ? N19 C44 H44A 109.5 . . ? C43 C44 H44A 109.5 . . ? N19 C44 H44B 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? N19 C45 C46 111.9(3) . . ? N19 C45 H45A 109.2 . . ? C46 C45 H45A 109.2 . . ? N19 C45 H45B 109.2 . . ? C46 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? N20 C46 C45 110.1(3) . . ? N20 C46 H46A 109.6 . . ? C45 C46 H46A 109.6 . . ? N20 C46 H46B 109.6 . . ? C45 C46 H46B 109.6 . . ? H46A C46 H46B 108.1 . . ? N20 C47 C48 111.6(3) . . ? N20 C47 H47A 109.3 . . ? C48 C47 H47A 109.3 . . ? N20 C47 H47B 109.3 . . ? C48 C47 H47B 109.3 . . ? H47A C47 H47B 108.0 . . ? N17 C48 C47 111.2(3) . . ? N17 C48 H48A 109.4 . . ? C47 C48 H48A 109.4 . . ? N17 C48 H48B 109.4 . . ? C47 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? N18 C49 H49A 109.5 . . ? N18 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N18 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N20 C50 H50A 109.5 . . ? N20 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N20 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N21 C51 C52 111.0(3) . . ? N21 C51 H51A 109.4 . . ? C52 C51 H51A 109.4 . . ? N21 C51 H51B 109.4 . . ? C52 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? N22 C52 C51 110.4(3) . . ? N22 C52 H52A 109.6 . . ? C51 C52 H52A 109.6 . . ? N22 C52 H52B 109.6 . . ? C51 C52 H52B 109.6 . . ? H52A C52 H52B 108.1 . . ? C54 C53 N22 112.3(3) . . ? C54 C53 H53A 109.1 . . ? N22 C53 H53A 109.1 . . ? C54 C53 H53B 109.1 . . ? N22 C53 H53B 109.1 . . ? H53A C53 H53B 107.9 . . ? N23 C54 C53 110.8(4) . . ? N23 C54 H54A 109.5 . . ? C53 C54 H54A 109.5 . . ? N23 C54 H54B 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 108.1 . . ? N23 C55 C56 111.2(3) . . ? N23 C55 H55A 109.4 . . ? C56 C55 H55A 109.4 . . ? N23 C55 H55B 109.4 . . ? C56 C55 H55B 109.4 . . ? H55A C55 H55B 108.0 . . ? N24 C56 C55 110.0(4) . . ? N24 C56 H56A 109.7 . . ? C55 C56 H56A 109.7 . . ? N24 C56 H56B 109.7 . . ? C55 C56 H56B 109.7 . . ? H56A C56 H56B 108.2 . . ? C58 C57 N24 114.1(4) . . ? C58 C57 H57A 108.7 . . ? N24 C57 H57A 108.7 . . ? C58 C57 H57B 108.7 . . ? N24 C57 H57B 108.7 . . ? H57A C57 H57B 107.6 . . ? N21 C58 C57 113.4(3) . . ? N21 C58 H58A 108.9 . . ? C57 C58 H58A 108.9 . . ? N21 C58 H58B 108.9 . . ? C57 C58 H58B 108.9 . . ? H58A C58 H58B 107.7 . . ? N22 C59 H59A 109.5 . . ? N22 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? N22 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N24 C60 H60A 109.5 . . ? N24 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N24 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62A C61A H61A 109.5 . . ? C62A C61A H61B 109.5 . . ? H61A C61A H61B 109.5 . . ? C62A C61A H61C 109.5 . . ? H61A C61A H61C 109.5 . . ? H61B C61A H61C 109.5 . . ? C61A C62A C63A 106.9(9) . . ? C61A C62A H62A 110.3 . . ? C63A C62A H62A 110.3 . . ? C61A C62A H62B 110.3 . . ? C63A C62A H62B 110.3 . . ? H62A C62A H62B 108.6 . . ? C64A C63A C62A 116.3(8) . . ? C64A C63A H63A 108.2 . . ? C62A C63A H63A 108.2 . . ? C64A C63A H63B 108.2 . . ? C62A C63A H63B 108.2 . . ? H63A C63A H63B 107.4 . . ? C63A C64A C65A 117.2(7) . . ? C63A C64A H64A 108.0 . . ? C65A C64A H64A 108.0 . . ? C63A C64A H64B 108.0 . . ? C65A C64A H64B 108.0 . . ? H64A C64A H64B 107.2 . . ? C66A C65A C64A 116.8(7) . . ? C66A C65A H65A 108.1 . . ? C64A C65A H65A 108.1 . . ? C66A C65A H65B 108.1 . . ? C64A C65A H65B 108.1 . . ? H65A C65A H65B 107.3 . . ? C65A C66A H66A 109.5 . . ? C65A C66A H66B 109.5 . . ? H66A C66A H66B 109.5 . . ? C65A C66A H66C 109.5 . . ? H66A C66A H66C 109.5 . . ? H66B C66A H66C 109.5 . . ? C62B C61B H61D 109.5 . . ? C62B C61B H61E 109.5 . . ? H61D C61B H61E 109.5 . . ? C62B C61B H61F 109.5 . . ? H61D C61B H61F 109.5 . . ? H61E C61B H61F 109.5 . . ? C61B C62B C63B 109.5(16) . . ? C61B C62B H62C 109.8 . . ? C63B C62B H62C 109.8 . . ? C61B C62B H62D 109.8 . . ? C63B C62B H62D 109.8 . . ? H62C C62B H62D 108.2 . . ? C64B C63B C62B 109.4(15) . . ? C64B C63B H63C 109.8 . . ? C62B C63B H63C 109.8 . . ? C64B C63B H63D 109.8 . . ? C62B C63B H63D 109.8 . . ? H63C C63B H63D 108.2 . . ? C65B C64B C63B 122.3(18) . . ? C65B C64B H64C 106.7 . . ? C63B C64B H64C 106.7 . . ? C65B C64B H64D 106.7 . . ? C63B C64B H64D 106.7 . . ? H64C C64B H64D 106.6 . . ? C64B C65B C66B 111.5(15) . . ? C64B C65B H65C 109.3 . . ? C66B C65B H65C 109.3 . . ? C64B C65B H65D 109.3 . . ? C66B C65B H65D 109.3 . . ? H65C C65B H65D 108.0 . . ? C65B C66B H66D 109.5 . . ? C65B C66B H66E 109.5 . . ? H66D C66B H66E 109.5 . . ? C65B C66B H66F 109.5 . . ? H66D C66B H66F 109.5 . . ? H66E C66B H66F 109.5 . . ? C62C C61C H61G 109.5 . . ? C62C C61C H61H 109.5 . . ? H61G C61C H61H 109.5 . . ? C62C C61C H61I 109.5 . . ? H61G C61C H61I 109.5 . . ? H61H C61C H61I 109.5 . . ? C63C C62C C61C 105.3(12) . . ? C63C C62C H62E 110.7 . . ? C61C C62C H62E 110.7 . . ? C63C C62C H62F 110.7 . . ? C61C C62C H62F 110.7 . . ? H62E C62C H62F 108.8 . . ? C64C C63C C62C 113.3(12) . . ? C64C C63C H63E 108.9 . . ? C62C C63C H63E 108.9 . . ? C64C C63C H63F 108.9 . . ? C62C C63C H63F 108.9 . . ? H63E C63C H63F 107.7 . . ? C65C C64C C63C 121.4(14) . . ? C65C C64C H64E 107.0 . . ? C63C C64C H64E 107.0 . . ? C65C C64C H64F 107.0 . . ? C63C C64C H64F 107.0 . . ? H64E C64C H64F 106.7 . . ? C64C C65C C66C 142.2(16) . . ? C64C C65C H65E 101.4 . . ? C66C C65C H65E 101.4 . . ? C64C C65C H65F 101.4 . . ? C66C C65C H65F 101.4 . . ? H65E C65C H65F 104.6 . . ? C65C C66C H66G 109.5 . . ? C65C C66C H66H 109.5 . . ? H66G C66C H66H 109.5 . . ? C65C C66C H66I 109.5 . . ? H66G C66C H66I 109.5 . . ? H66H C66C H66I 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 N3 Sc1 Sc2 N7 -1.6(2) . . . . ? N1 Sc1 Sc2 N7 -5.95(18) . . . . ? N9 Sc1 Sc2 N7 178.12(16) . . . . ? N2 Sc1 Sc2 N7 -69.46(16) . . . . ? N4 Sc1 Sc2 N7 58.06(16) . . . . ? Sc3 Sc1 Sc2 N7 175.60(15) . . . . ? N3 Sc1 Sc2 N1 4.4(2) . . . . ? N9 Sc1 Sc2 N1 -175.93(15) . . . . ? N2 Sc1 Sc2 N1 -63.51(14) . . . . ? N4 Sc1 Sc2 N1 64.01(14) . . . . ? Sc3 Sc1 Sc2 N1 -178.45(12) . . . . ? N3 Sc1 Sc2 N5 -179.3(2) . . . . ? N1 Sc1 Sc2 N5 176.32(14) . . . . ? N9 Sc1 Sc2 N5 0.39(12) . . . . ? N2 Sc1 Sc2 N5 112.81(11) . . . . ? N4 Sc1 Sc2 N5 -119.67(11) . . . . ? Sc3 Sc1 Sc2 N5 -2.13(8) . . . . ? N3 Sc1 Sc2 N8 97.2(2) . . . . ? N1 Sc1 Sc2 N8 92.85(14) . . . . ? N9 Sc1 Sc2 N8 -83.08(12) . . . . ? N2 Sc1 Sc2 N8 29.34(11) . . . . ? N4 Sc1 Sc2 N8 156.86(11) . . . . ? Sc3 Sc1 Sc2 N8 -85.60(9) . . . . ? N3 Sc1 Sc2 N6 -99.0(2) . . . . ? N1 Sc1 Sc2 N6 -103.37(15) . . . . ? N9 Sc1 Sc2 N6 80.70(12) . . . . ? N2 Sc1 Sc2 N6 -166.88(11) . . . . ? N4 Sc1 Sc2 N6 -39.36(12) . . . . ? Sc3 Sc1 Sc2 N6 78.18(9) . . . . ? N3 Sc1 Sc2 Sc3 -177.20(19) . . . . ? N1 Sc1 Sc2 Sc3 178.45(12) . . . . ? N9 Sc1 Sc2 Sc3 2.52(9) . . . . ? N2 Sc1 Sc2 Sc3 114.94(8) . . . . ? N4 Sc1 Sc2 Sc3 -117.54(8) . . . . ? N7 Sc2 Sc3 N11 1.8(3) . . . . ? N1 Sc2 Sc3 N11 175.30(17) . . . . ? N5 Sc2 Sc3 N11 -8.79(18) . . . . ? N8 Sc2 Sc3 N11 -69.07(17) . . . . ? N6 Sc2 Sc3 N11 54.79(17) . . . . ? Sc1 Sc2 Sc3 N11 174.24(15) . . . . ? N7 Sc2 Sc3 N5 10.6(3) . . . . ? N1 Sc2 Sc3 N5 -175.91(14) . . . . ? N8 Sc2 Sc3 N5 -60.29(13) . . . . ? N6 Sc2 Sc3 N5 63.57(14) . . . . ? Sc1 Sc2 Sc3 N5 -176.97(11) . . . . ? N7 Sc2 Sc3 N9 -175.0(3) . . . . ? N1 Sc2 Sc3 N9 -1.46(12) . . . . ? N5 Sc2 Sc3 N9 174.45(14) . . . . ? N8 Sc2 Sc3 N9 114.16(11) . . . . ? N6 Sc2 Sc3 N9 -121.98(12) . . . . ? Sc1 Sc2 Sc3 N9 -2.52(9) . . . . ? N7 Sc2 Sc3 N12 100.1(3) . . . . ? N1 Sc2 Sc3 N12 -86.42(12) . . . . ? N5 Sc2 Sc3 N12 89.49(14) . . . . ? N8 Sc2 Sc3 N12 29.20(12) . . . . ? N6 Sc2 Sc3 N12 153.06(12) . . . . ? Sc1 Sc2 Sc3 N12 -87.48(9) . . . . ? N7 Sc2 Sc3 N10 -93.6(3) . . . . ? N1 Sc2 Sc3 N10 79.95(13) . . . . ? N5 Sc2 Sc3 N10 -104.14(15) . . . . ? N8 Sc2 Sc3 N10 -164.42(12) . . . . ? N6 Sc2 Sc3 N10 -40.56(13) . . . . ? Sc1 Sc2 Sc3 N10 78.89(10) . . . . ? N7 Sc2 Sc3 Sc1 -172.5(2) . . . . ? N1 Sc2 Sc3 Sc1 1.06(8) . . . . ? N5 Sc2 Sc3 Sc1 176.97(11) . . . . ? N8 Sc2 Sc3 Sc1 116.68(8) . . . . ? N6 Sc2 Sc3 Sc1 -119.46(9) . . . . ? N3 Sc1 Sc3 N11 5.6(3) . . . . ? N1 Sc1 Sc3 N11 -173.0(2) . . . . ? N9 Sc1 Sc3 N11 11.7(2) . . . . ? N2 Sc1 Sc3 N11 104.3(2) . . . . ? N4 Sc1 Sc3 N11 -91.6(2) . . . . ? Sc2 Sc1 Sc3 N11 -171.9(2) . . . . ? N3 Sc1 Sc3 N5 179.72(18) . . . . ? N1 Sc1 Sc3 N5 1.09(11) . . . . ? N9 Sc1 Sc3 N5 -174.22(15) . . . . ? N2 Sc1 Sc3 N5 -81.64(11) . . . . ? N4 Sc1 Sc3 N5 82.46(11) . . . . ? Sc2 Sc1 Sc3 N5 2.15(8) . . . . ? N3 Sc1 Sc3 N9 -6.1(2) . . . . ? N1 Sc1 Sc3 N9 175.31(15) . . . . ? N2 Sc1 Sc3 N9 92.58(15) . . . . ? N4 Sc1 Sc3 N9 -103.32(15) . . . . ? Sc2 Sc1 Sc3 N9 176.37(12) . . . . ? N3 Sc1 Sc3 N12 -66.74(18) . . . . ? N1 Sc1 Sc3 N12 114.63(11) . . . . ? N9 Sc1 Sc3 N12 -60.68(14) . . . . ? N2 Sc1 Sc3 N12 31.90(11) . . . . ? N4 Sc1 Sc3 N12 -164.00(11) . . . . ? Sc2 Sc1 Sc3 N12 115.69(8) . . . . ? N3 Sc1 Sc3 N10 60.30(18) . . . . ? N1 Sc1 Sc3 N10 -118.33(12) . . . . ? N9 Sc1 Sc3 N10 66.36(15) . . . . ? N2 Sc1 Sc3 N10 158.94(12) . . . . ? N4 Sc1 Sc3 N10 -36.96(12) . . . . ? Sc2 Sc1 Sc3 N10 -117.27(9) . . . . ? N3 Sc1 Sc3 Sc2 177.58(16) . . . . ? N1 Sc1 Sc3 Sc2 -1.06(8) . . . . ? N9 Sc1 Sc3 Sc2 -176.37(12) . . . . ? N2 Sc1 Sc3 Sc2 -83.79(8) . . . . ? N4 Sc1 Sc3 Sc2 80.32(9) . . . . ? N3 Sc1 N1 C5 66.3(3) . . . . ? N9 Sc1 N1 C5 -109.1(3) . . . . ? N2 Sc1 N1 C5 -0.5(2) . . . . ? N4 Sc1 N1 C5 130.6(2) . . . . ? Sc3 Sc1 N1 C5 -114.4(2) . . . . ? Sc2 Sc1 N1 C5 -115.8(3) . . . . ? N3 Sc1 N1 C4 -62.5(3) . . . . ? N9 Sc1 N1 C4 122.1(3) . . . . ? N2 Sc1 N1 C4 -129.4(2) . . . . ? N4 Sc1 N1 C4 1.8(2) . . . . ? Sc3 Sc1 N1 C4 116.7(2) . . . . ? Sc2 Sc1 N1 C4 115.4(3) . . . . ? N3 Sc1 N1 Sc2 -177.87(11) . . . . ? N9 Sc1 N1 Sc2 6.7(2) . . . . ? N2 Sc1 N1 Sc2 115.28(12) . . . . ? N4 Sc1 N1 Sc2 -113.57(12) . . . . ? Sc3 Sc1 N1 Sc2 1.36(10) . . . . ? N7 Sc2 N1 C5 -68.5(2) . . . . ? N5 Sc2 N1 C5 109.0(3) . . . . ? N8 Sc2 N1 C5 7.6(3) . . . . ? N6 Sc2 N1 C5 -144.6(2) . . . . ? Sc3 Sc2 N1 C5 113.9(2) . . . . ? Sc1 Sc2 N1 C5 115.3(3) . . . . ? N7 Sc2 N1 C4 59.3(2) . . . . ? N5 Sc2 N1 C4 -123.2(3) . . . . ? N8 Sc2 N1 C4 135.4(2) . . . . ? N6 Sc2 N1 C4 -16.8(3) . . . . ? Sc3 Sc2 N1 C4 -118.3(2) . . . . ? Sc1 Sc2 N1 C4 -116.9(3) . . . . ? N7 Sc2 N1 Sc1 176.21(12) . . . . ? N5 Sc2 N1 Sc1 -6.3(2) . . . . ? N8 Sc2 N1 Sc1 -107.67(12) . . . . ? N6 Sc2 N1 Sc1 100.13(13) . . . . ? Sc3 Sc2 N1 Sc1 -1.38(11) . . . . ? N3 Sc1 N2 C9 149.6(3) . . . . ? N1 Sc1 N2 C9 -94.3(3) . . . . ? N9 Sc1 N2 C9 49.0(3) . . . . ? N4 Sc1 N2 C9 -159.5(3) . . . . ? Sc3 Sc1 N2 C9 2.8(3) . . . . ? Sc2 Sc1 N2 C9 -56.7(3) . . . . ? N3 Sc1 N2 C6 -88.7(2) . . . . ? N1 Sc1 N2 C6 27.3(2) . . . . ? N9 Sc1 N2 C6 170.7(2) . . . . ? N4 Sc1 N2 C6 -37.9(3) . . . . ? Sc3 Sc1 N2 C6 124.5(2) . . . . ? Sc2 Sc1 N2 C6 64.9(2) . . . . ? N3 Sc1 N2 C7 27.3(2) . . . . ? N1 Sc1 N2 C7 143.4(2) . . . . ? N9 Sc1 N2 C7 -73.3(2) . . . . ? N4 Sc1 N2 C7 78.2(3) . . . . ? Sc3 Sc1 N2 C7 -119.5(2) . . . . ? Sc2 Sc1 N2 C7 -179.0(2) . . . . ? N1 Sc1 N3 C1 76.3(3) . . . . ? N9 Sc1 N3 C1 -106.5(3) . . . . ? N2 Sc1 N3 C1 146.8(3) . . . . ? N4 Sc1 N3 C1 8.3(3) . . . . ? Sc3 Sc1 N3 C1 -102.2(3) . . . . ? Sc2 Sc1 N3 C1 73.2(4) . . . . ? N1 Sc1 N3 C8 -79.9(3) . . . . ? N9 Sc1 N3 C8 97.3(3) . . . . ? N2 Sc1 N3 C8 -9.4(3) . . . . ? N4 Sc1 N3 C8 -148.0(3) . . . . ? Sc3 Sc1 N3 C8 101.5(3) . . . . ? Sc2 Sc1 N3 C8 -83.0(3) . . . . ? N3 Sc1 N4 C10 -151.5(4) . . . . ? N1 Sc1 N4 C10 91.1(3) . . . . ? N9 Sc1 N4 C10 -53.5(4) . . . . ? N2 Sc1 N4 C10 157.0(3) . . . . ? Sc3 Sc1 N4 C10 -5.2(4) . . . . ? Sc2 Sc1 N4 C10 53.1(3) . . . . ? N3 Sc1 N4 C3 88.0(2) . . . . ? N1 Sc1 N4 C3 -29.4(2) . . . . ? N9 Sc1 N4 C3 -174.1(2) . . . . ? N2 Sc1 N4 C3 36.5(3) . . . . ? Sc3 Sc1 N4 C3 -125.7(2) . . . . ? Sc2 Sc1 N4 C3 -67.4(2) . . . . ? N3 Sc1 N4 C2 -27.4(2) . . . . ? N1 Sc1 N4 C2 -144.8(2) . . . . ? N9 Sc1 N4 C2 70.6(3) . . . . ? N2 Sc1 N4 C2 -78.9(3) . . . . ? Sc3 Sc1 N4 C2 118.9(2) . . . . ? Sc2 Sc1 N4 C2 177.2(2) . . . . ? N11 Sc3 N5 C11B 60.6(5) . . . . ? N9 Sc3 N5 C11B -123.9(6) . . . . ? N12 Sc3 N5 C11B 135.6(5) . . . . ? N10 Sc3 N5 C11B -15.5(6) . . . . ? Sc2 Sc3 N5 C11B -114.2(5) . . . . ? Sc1 Sc3 N5 C11B -116.9(5) . . . . ? N11 Sc3 N5 C18 -72.0(2) . . . . ? N9 Sc3 N5 C18 103.5(3) . . . . ? N12 Sc3 N5 C18 3.0(3) . . . . ? N10 Sc3 N5 C18 -148.1(2) . . . . ? Sc2 Sc3 N5 C18 113.2(3) . . . . ? Sc1 Sc3 N5 C18 110.5(2) . . . . ? N11 Sc3 N5 C11A 54.5(4) . . . . ? N9 Sc3 N5 C11A -130.0(4) . . . . ? N12 Sc3 N5 C11A 129.5(3) . . . . ? N10 Sc3 N5 C11A -21.6(4) . . . . ? Sc2 Sc3 N5 C11A -120.3(4) . . . . ? Sc1 Sc3 N5 C11A -123.0(3) . . . . ? N11 Sc3 N5 Sc2 174.76(11) . . . . ? N9 Sc3 N5 Sc2 -9.7(2) . . . . ? N12 Sc3 N5 Sc2 -110.27(11) . . . . ? N10 Sc3 N5 Sc2 98.66(12) . . . . ? Sc1 Sc3 N5 Sc2 -2.71(10) . . . . ? N7 Sc2 N5 C11B -72.1(6) . . . . ? N1 Sc2 N5 C11B 110.6(6) . . . . ? N8 Sc2 N5 C11B -137.3(6) . . . . ? N6 Sc2 N5 C11B -9.0(6) . . . . ? Sc3 Sc2 N5 C11B 103.6(6) . . . . ? Sc1 Sc2 N5 C11B 106.3(6) . . . . ? N7 Sc2 N5 C18 67.6(3) . . . . ? N1 Sc2 N5 C18 -109.7(3) . . . . ? N8 Sc2 N5 C18 2.4(2) . . . . ? N6 Sc2 N5 C18 130.7(3) . . . . ? Sc3 Sc2 N5 C18 -116.7(3) . . . . ? Sc1 Sc2 N5 C18 -114.0(2) . . . . ? N7 Sc2 N5 C11A -48.3(4) . . . . ? N1 Sc2 N5 C11A 134.4(4) . . . . ? N8 Sc2 N5 C11A -113.6(4) . . . . ? N6 Sc2 N5 C11A 14.8(3) . . . . ? Sc3 Sc2 N5 C11A 127.4(4) . . . . ? Sc1 Sc2 N5 C11A 130.1(3) . . . . ? N7 Sc2 N5 Sc3 -175.71(11) . . . . ? N1 Sc2 N5 Sc3 7.0(2) . . . . ? N8 Sc2 N5 Sc3 119.05(11) . . . . ? N6 Sc2 N5 Sc3 -112.60(12) . . . . ? Sc1 Sc2 N5 Sc3 2.71(10) . . . . ? N7 Sc2 N6 C19B -140.9(9) . . . . ? N1 Sc2 N6 C19B -49.2(9) . . . . ? N5 Sc2 N6 C19B 96.2(9) . . . . ? N8 Sc2 N6 C19B 161.5(9) . . . . ? Sc3 Sc2 N6 C19B 57.0(9) . . . . ? Sc1 Sc2 N6 C19B -1.5(9) . . . . ? N7 Sc2 N6 C12B 97.5(5) . . . . ? N1 Sc2 N6 C12B -170.9(5) . . . . ? N5 Sc2 N6 C12B -25.4(5) . . . . ? N8 Sc2 N6 C12B 39.8(5) . . . . ? Sc3 Sc2 N6 C12B -64.7(5) . . . . ? Sc1 Sc2 N6 C12B -123.2(5) . . . . ? N7 Sc2 N6 C19A -108.6(4) . . . . ? N1 Sc2 N6 C19A -17.0(4) . . . . ? N5 Sc2 N6 C19A 128.5(4) . . . . ? N8 Sc2 N6 C19A -166.2(4) . . . . ? Sc3 Sc2 N6 C19A 89.3(4) . . . . ? Sc1 Sc2 N6 C19A 30.7(4) . . . . ? N7 Sc2 N6 C13A 15.5(3) . . . . ? N1 Sc2 N6 C13A 107.2(3) . . . . ? N5 Sc2 N6 C13A -107.4(3) . . . . ? N8 Sc2 N6 C13A -42.1(3) . . . . ? Sc3 Sc2 N6 C13A -146.6(3) . . . . ? Sc1 Sc2 N6 C13A 154.8(3) . . . . ? N7 Sc2 N6 C12A 133.7(3) . . . . ? N1 Sc2 N6 C12A -134.6(3) . . . . ? N5 Sc2 N6 C12A 10.8(3) . . . . ? N8 Sc2 N6 C12A 76.1(3) . . . . ? Sc3 Sc2 N6 C12A -28.4(3) . . . . ? Sc1 Sc2 N6 C12A -86.9(3) . . . . ? N7 Sc2 N6 C13B -22.8(8) . . . . ? N1 Sc2 N6 C13B 68.8(8) . . . . ? N5 Sc2 N6 C13B -145.7(8) . . . . ? N8 Sc2 N6 C13B -80.5(8) . . . . ? Sc3 Sc2 N6 C13B 175.0(8) . . . . ? Sc1 Sc2 N6 C13B 116.5(8) . . . . ? N1 Sc2 N7 C15 110.7(3) . . . . ? N5 Sc2 N7 C15 -67.7(3) . . . . ? N8 Sc2 N7 C15 0.0(3) . . . . ? N6 Sc2 N7 C15 -132.0(3) . . . . ? Sc3 Sc2 N7 C15 -75.7(4) . . . . ? Sc1 Sc2 N7 C15 114.7(3) . . . . ? N1 Sc2 N7 C14A -96.3(4) . . . . ? N5 Sc2 N7 C14A 85.2(4) . . . . ? N8 Sc2 N7 C14A 153.0(4) . . . . ? N6 Sc2 N7 C14A 21.0(4) . . . . ? Sc3 Sc2 N7 C14A 77.2(5) . . . . ? Sc1 Sc2 N7 C14A -92.3(4) . . . . ? N1 Sc2 N7 C14B -115.0(8) . . . . ? N5 Sc2 N7 C14B 66.6(8) . . . . ? N8 Sc2 N7 C14B 134.3(8) . . . . ? N6 Sc2 N7 C14B 2.3(8) . . . . ? Sc3 Sc2 N7 C14B 58.6(9) . . . . ? Sc1 Sc2 N7 C14B -111.0(8) . . . . ? N7 Sc2 N8 C17 -94.2(2) . . . . ? N1 Sc2 N8 C17 172.3(2) . . . . ? N5 Sc2 N8 C17 27.3(2) . . . . ? N6 Sc2 N8 C17 -36.7(3) . . . . ? Sc3 Sc2 N8 C17 64.6(2) . . . . ? Sc1 Sc2 N8 C17 126.3(2) . . . . ? N7 Sc2 N8 C20 142.9(3) . . . . ? N1 Sc2 N8 C20 49.4(3) . . . . ? N5 Sc2 N8 C20 -95.6(3) . . . . ? N6 Sc2 N8 C20 -159.6(3) . . . . ? Sc3 Sc2 N8 C20 -58.3(3) . . . . ? Sc1 Sc2 N8 C20 3.3(3) . . . . ? N7 Sc2 N8 C16 21.0(2) . . . . ? N1 Sc2 N8 C16 -72.5(2) . . . . ? N5 Sc2 N8 C16 142.5(2) . . . . ? N6 Sc2 N8 C16 78.5(2) . . . . ? Sc3 Sc2 N8 C16 179.8(2) . . . . ? Sc1 Sc2 N8 C16 -118.5(2) . . . . ? N3 Sc1 N9 C25 59.8(3) . . . . ? N1 Sc1 N9 C25 -124.7(3) . . . . ? N2 Sc1 N9 C25 137.0(3) . . . . ? N4 Sc1 N9 C25 -17.0(3) . . . . ? Sc3 Sc1 N9 C25 -116.9(3) . . . . ? Sc2 Sc1 N9 C25 -120.1(3) . . . . ? N3 Sc1 N9 C24 -70.7(3) . . . . ? N1 Sc1 N9 C24 104.8(3) . . . . ? N2 Sc1 N9 C24 6.5(3) . . . . ? N4 Sc1 N9 C24 -147.6(2) . . . . ? Sc3 Sc1 N9 C24 112.6(3) . . . . ? Sc2 Sc1 N9 C24 109.4(2) . . . . ? N3 Sc1 N9 Sc3 176.67(11) . . . . ? N1 Sc1 N9 Sc3 -7.8(2) . . . . ? N2 Sc1 N9 Sc3 -106.10(12) . . . . ? N4 Sc1 N9 Sc3 99.84(12) . . . . ? Sc2 Sc1 N9 Sc3 -3.19(11) . . . . ? N11 Sc3 N9 C25 -55.1(3) . . . . ? N5 Sc3 N9 C25 129.7(3) . . . . ? N12 Sc3 N9 C25 -120.8(3) . . . . ? N10 Sc3 N9 C25 9.5(3) . . . . ? Sc2 Sc3 N9 C25 122.8(3) . . . . ? Sc1 Sc3 N9 C25 119.6(3) . . . . ? N11 Sc3 N9 C24 68.1(3) . . . . ? N5 Sc3 N9 C24 -107.1(3) . . . . ? N12 Sc3 N9 C24 2.5(2) . . . . ? N10 Sc3 N9 C24 132.7(3) . . . . ? Sc2 Sc3 N9 C24 -113.9(2) . . . . ? Sc1 Sc3 N9 C24 -117.2(3) . . . . ? N11 Sc3 N9 Sc1 -174.70(11) . . . . ? N5 Sc3 N9 Sc1 10.1(3) . . . . ? N12 Sc3 N9 Sc1 119.65(12) . . . . ? N10 Sc3 N9 Sc1 -110.12(13) . . . . ? Sc2 Sc3 N9 Sc1 3.24(11) . . . . ? N11 Sc3 N10 C26A 86.7(3) . . . . ? N5 Sc3 N10 C26A -179.8(3) . . . . ? N9 Sc3 N10 C26A -32.7(3) . . . . ? N12 Sc3 N10 C26A 34.2(4) . . . . ? Sc2 Sc3 N10 C26A -131.0(3) . . . . ? Sc1 Sc3 N10 C26A -72.3(3) . . . . ? N11 Sc3 N10 C30B -113.7(7) . . . . ? N5 Sc3 N10 C30B -20.2(7) . . . . ? N9 Sc3 N10 C30B 126.8(7) . . . . ? N12 Sc3 N10 C30B -166.2(6) . . . . ? Sc2 Sc3 N10 C30B 28.5(7) . . . . ? Sc1 Sc3 N10 C30B 87.3(7) . . . . ? N11 Sc3 N10 C30A -150.1(5) . . . . ? N5 Sc3 N10 C30A -56.6(5) . . . . ? N9 Sc3 N10 C30A 90.4(5) . . . . ? N12 Sc3 N10 C30A 157.4(4) . . . . ? Sc2 Sc3 N10 C30A -7.9(5) . . . . ? Sc1 Sc3 N10 C30A 50.9(5) . . . . ? N11 Sc3 N10 C27A -31.7(3) . . . . ? N5 Sc3 N10 C27A 61.8(3) . . . . ? N9 Sc3 N10 C27A -151.1(3) . . . . ? N12 Sc3 N10 C27A -84.2(3) . . . . ? Sc2 Sc3 N10 C27A 110.6(3) . . . . ? Sc1 Sc3 N10 C27A 169.3(3) . . . . ? N11 Sc3 N10 C27B 16.8(5) . . . . ? N5 Sc3 N10 C27B 110.3(5) . . . . ? N9 Sc3 N10 C27B -102.6(5) . . . . ? N12 Sc3 N10 C27B -35.7(5) . . . . ? Sc2 Sc3 N10 C27B 159.1(5) . . . . ? Sc1 Sc3 N10 C27B -142.2(5) . . . . ? N11 Sc3 N10 C26B 127.9(5) . . . . ? N5 Sc3 N10 C26B -138.6(5) . . . . ? N9 Sc3 N10 C26B 8.4(5) . . . . ? N12 Sc3 N10 C26B 75.4(5) . . . . ? Sc2 Sc3 N10 C26B -89.8(5) . . . . ? Sc1 Sc3 N10 C26B -31.1(5) . . . . ? N5 Sc3 N11 C28A -106.5(5) . . . . ? N9 Sc3 N11 C28A 76.2(5) . . . . ? N12 Sc3 N11 C28A 146.3(5) . . . . ? N10 Sc3 N11 C28A 9.1(5) . . . . ? Sc2 Sc3 N11 C28A -100.4(5) . . . . ? Sc1 Sc3 N11 C28A 67.6(6) . . . . ? N5 Sc3 N11 C21 102.1(3) . . . . ? N9 Sc3 N11 C21 -75.1(3) . . . . ? N12 Sc3 N11 C21 -5.0(3) . . . . ? N10 Sc3 N11 C21 -142.2(3) . . . . ? Sc2 Sc3 N11 C21 108.3(3) . . . . ? Sc1 Sc3 N11 C21 -83.7(4) . . . . ? N5 Sc3 N11 C28B -92.5(7) . . . . ? N9 Sc3 N11 C28B 90.3(7) . . . . ? N12 Sc3 N11 C28B 160.4(8) . . . . ? N10 Sc3 N11 C28B 23.2(7) . . . . ? Sc2 Sc3 N11 C28B -86.3(8) . . . . ? Sc1 Sc3 N11 C28B 81.7(8) . . . . ? N11 Sc3 N12 C29 148.4(3) . . . . ? N5 Sc3 N12 C29 52.8(3) . . . . ? N9 Sc3 N12 C29 -93.2(3) . . . . ? N10 Sc3 N12 C29 -158.9(3) . . . . ? Sc2 Sc3 N12 C29 6.0(3) . . . . ? Sc1 Sc3 N12 C29 -56.4(3) . . . . ? N11 Sc3 N12 C23 -91.1(2) . . . . ? N5 Sc3 N12 C23 173.3(2) . . . . ? N9 Sc3 N12 C23 27.2(2) . . . . ? N10 Sc3 N12 C23 -38.4(3) . . . . ? Sc2 Sc3 N12 C23 126.4(2) . . . . ? Sc1 Sc3 N12 C23 64.1(2) . . . . ? N11 Sc3 N12 C22 24.5(2) . . . . ? N5 Sc3 N12 C22 -71.1(2) . . . . ? N9 Sc3 N12 C22 142.8(2) . . . . ? N10 Sc3 N12 C22 77.2(3) . . . . ? Sc2 Sc3 N12 C22 -118.0(2) . . . . ? Sc1 Sc3 N12 C22 179.7(2) . . . . ? C8 N3 C1 C2 172.7(3) . . . . ? Sc1 N3 C1 C2 13.3(5) . . . . ? C10 N4 C2 C1 -179.6(3) . . . . ? C3 N4 C2 C1 -61.7(4) . . . . ? Sc1 N4 C2 C1 43.6(4) . . . . ? N3 C1 C2 N4 -39.9(4) . . . . ? C10 N4 C3 C4 -80.9(4) . . . . ? C2 N4 C3 C4 162.4(3) . . . . ? Sc1 N4 C3 C4 53.1(3) . . . . ? C5 N1 C4 C3 -99.8(4) . . . . ? Sc1 N1 C4 C3 27.4(4) . . . . ? Sc2 N1 C4 C3 133.8(3) . . . . ? N4 C3 C4 N1 -59.6(4) . . . . ? C4 N1 C5 C6 100.1(4) . . . . ? Sc1 N1 C5 C6 -28.0(4) . . . . ? Sc2 N1 C5 C6 -133.9(3) . . . . ? C9 N2 C6 C5 80.5(4) . . . . ? C7 N2 C6 C5 -162.4(3) . . . . ? Sc1 N2 C6 C5 -50.8(3) . . . . ? N1 C5 C6 N2 57.7(4) . . . . ? C9 N2 C7 C8 -175.0(3) . . . . ? C6 N2 C7 C8 65.7(4) . . . . ? Sc1 N2 C7 C8 -42.1(4) . . . . ? C1 N3 C8 C7 -171.2(3) . . . . ? Sc1 N3 C8 C7 -11.3(5) . . . . ? N2 C7 C8 N3 37.0(5) . . . . ? C11B N5 C11A C12A 52.7(16) . . . . ? C18 N5 C11A C12A -160.4(5) . . . . ? Sc3 N5 C11A C12A 69.0(6) . . . . ? Sc2 N5 C11A C12A -41.3(6) . . . . ? N5 C11A C12A N6 54.2(8) . . . . ? C19B N6 C12A C11A -160.5(9) . . . . ? C12B N6 C12A C11A 54.1(9) . . . . ? C19A N6 C12A C11A -164.6(6) . . . . ? C13A N6 C12A C11A 75.0(7) . . . . ? C13B N6 C12A C11A 102.1(14) . . . . ? Sc2 N6 C12A C11A -36.5(6) . . . . ? C19B N6 C13A C14A 110.8(10) . . . . ? C12B N6 C13A C14A -144.8(7) . . . . ? C19A N6 C13A C14A 85.5(6) . . . . ? C12A N6 C13A C14A -157.0(5) . . . . ? C13B N6 C13A C14A 49.2(13) . . . . ? Sc2 N6 C13A C14A -45.3(5) . . . . ? C15 N7 C14A C13A 101.9(5) . . . . ? C14B N7 C14A C13A 54(3) . . . . ? Sc2 N7 C14A C13A -53.9(6) . . . . ? N6 C13A C14A N7 64.6(6) . . . . ? C18 N5 C11B C12B -93.4(9) . . . . ? C11A N5 C11B C12B -54.7(15) . . . . ? Sc3 N5 C11B C12B 139.3(8) . . . . ? Sc2 N5 C11B C12B 40.7(11) . . . . ? C19B N6 C12B C11B -80.5(11) . . . . ? C19A N6 C12B C11B -97.4(9) . . . . ? C13A N6 C12B C11B 154.6(9) . . . . ? C12A N6 C12B C11B -44.9(8) . . . . ? C13B N6 C12B C11B 164.0(10) . . . . ? Sc2 N6 C12B C11B 52.8(8) . . . . ? N5 C11B C12B N6 -66.7(11) . . . . ? C19B N6 C13B C14B 173.4(15) . . . . ? C12B N6 C13B C14B -68.9(17) . . . . ? C19A N6 C13B C14B 160.8(16) . . . . ? C13A N6 C13B C14B -53.6(13) . . . . ? C12A N6 C13B C14B -97.5(18) . . . . ? Sc2 N6 C13B C14B 41.2(16) . . . . ? N6 C13B C14B N7 -44(2) . . . . ? C15 N7 C14B C13B 164.0(14) . . . . ? C14A N7 C14B C13B -61(3) . . . . ? Sc2 N7 C14B C13B 21.4(18) . . . . ? C14A N7 C15 C16 -176.0(4) . . . . ? C14B N7 C15 C16 -163.5(7) . . . . ? Sc2 N7 C15 C16 -21.8(4) . . . . ? N7 C15 C16 N8 40.9(4) . . . . ? C17 N8 C16 C15 68.1(4) . . . . ? C20 N8 C16 C15 -172.8(3) . . . . ? Sc2 N8 C16 C15 -38.9(3) . . . . ? C20 N8 C17 C18 79.8(4) . . . . ? C16 N8 C17 C18 -164.1(3) . . . . ? Sc2 N8 C17 C18 -53.1(3) . . . . ? C11B N5 C18 C17 102.6(7) . . . . ? C11A N5 C18 C17 88.8(4) . . . . ? Sc3 N5 C18 C17 -135.8(3) . . . . ? Sc2 N5 C18 C17 -32.7(4) . . . . ? N8 C17 C18 N5 63.1(4) . . . . ? C28A N11 C21 C22 -171.2(5) . . . . ? C28B N11 C21 C22 177.6(7) . . . . ? Sc3 N11 C21 C22 -16.0(5) . . . . ? N11 C21 C22 N12 38.4(4) . . . . ? C29 N12 C22 C21 -175.7(3) . . . . ? C23 N12 C22 C21 66.2(4) . . . . ? Sc3 N12 C22 C21 -41.1(4) . . . . ? C29 N12 C23 C24 78.6(4) . . . . ? C22 N12 C23 C24 -164.8(3) . . . . ? Sc3 N12 C23 C24 -52.8(3) . . . . ? C25 N9 C24 C23 90.8(4) . . . . ? Sc1 N9 C24 C23 -136.7(3) . . . . ? Sc3 N9 C24 C23 -32.7(4) . . . . ? N12 C23 C24 N9 63.1(5) . . . . ? C24 N9 C25 C26B -154.4(7) . . . . ? Sc1 N9 C25 C26B 73.8(8) . . . . ? Sc3 N9 C25 C26B -32.8(8) . . . . ? C24 N9 C25 C26A -107.2(5) . . . . ? Sc1 N9 C25 C26A 121.1(4) . . . . ? Sc3 N9 C25 C26A 14.4(5) . . . . ? C30B N10 C26A C25 -106.1(8) . . . . ? C30A N10 C26A C25 -79.0(6) . . . . ? C27A N10 C26A C25 162.9(5) . . . . ? C27B N10 C26A C25 153.9(7) . . . . ? C26B N10 C26A C25 -44.1(7) . . . . ? Sc3 N10 C26A C25 51.9(5) . . . . ? C26B C25 C26A N10 56.3(9) . . . . ? N9 C25 C26A N10 -50.0(7) . . . . ? C26A N10 C27A C28A -60.4(7) . . . . ? C30B N10 C27A C28A 171.3(7) . . . . ? C30A N10 C27A C28A 177.9(6) . . . . ? C27B N10 C27A C28A -48.9(8) . . . . ? C26B N10 C27A C28A -93.2(11) . . . . ? Sc3 N10 C27A C28A 47.8(6) . . . . ? C21 N11 C28A C27A 172.0(6) . . . . ? C28B N11 C28A C27A -66(4) . . . . ? Sc3 N11 C28A C27A 16.1(9) . . . . ? N10 C27A C28A N11 -44.3(8) . . . . ? N9 C25 C26B N10 45.1(12) . . . . ? C26A C25 C26B N10 -50.2(8) . . . . ? C26A N10 C26B C25 61.2(9) . . . . ? C30B N10 C26B C25 -162.8(10) . . . . ? C30A N10 C26B C25 -152.0(11) . . . . ? C27A N10 C26B C25 110.8(11) . . . . ? C27B N10 C26B C25 78.6(11) . . . . ? Sc3 N10 C26B C25 -30.8(10) . . . . ? C26A N10 C27B C28B -145.4(10) . . . . ? C30B N10 C27B C28B 88.0(10) . . . . ? C30A N10 C27B C28B 115.0(10) . . . . ? C27A N10 C27B C28B 45.9(8) . . . . ? C26B N10 C27B C28B -157.5(9) . . . . ? Sc3 N10 C27B C28B -50.4(9) . . . . ? C28A N11 C28B C27B 51(4) . . . . ? C21 N11 C28B C27B 111.8(8) . . . . ? Sc3 N11 C28B C27B -55.3(11) . . . . ? N10 C27B C28B N11 65.4(11) . . . . ? N13 Sc4 Sc5 N17 -105.87(14) . . . . ? N15 Sc4 Sc5 N17 92.51(13) . . . . ? N14 Sc4 Sc5 N17 174.04(12) . . . . ? N16 Sc4 Sc5 N17 -0.36(13) . . . . ? N13 Sc4 Sc5 N19 -127.3(2) . . . . ? N15 Sc4 Sc5 N19 71.1(2) . . . . ? N17 Sc4 Sc5 N19 -21.4(2) . . . . ? N14 Sc4 Sc5 N19 152.6(2) . . . . ? N16 Sc4 Sc5 N19 -21.8(3) . . . . ? N13 Sc4 Sc5 N20 -172.35(13) . . . . ? N15 Sc4 Sc5 N20 26.03(12) . . . . ? N17 Sc4 Sc5 N20 -66.48(11) . . . . ? N14 Sc4 Sc5 N20 107.56(10) . . . . ? N16 Sc4 Sc5 N20 -66.84(11) . . . . ? N13 Sc4 Sc5 N18 -51.44(13) . . . . ? N15 Sc4 Sc5 N18 146.94(11) . . . . ? N17 Sc4 Sc5 N18 54.44(11) . . . . ? N14 Sc4 Sc5 N18 -131.52(10) . . . . ? N16 Sc4 Sc5 N18 54.08(11) . . . . ? N13 Sc4 Sc5 Sc6 66.59(13) . . . . ? N15 Sc4 Sc5 Sc6 -95.03(11) . . . . ? N17 Sc4 Sc5 Sc6 172.46(11) . . . . ? N14 Sc4 Sc5 Sc6 -13.49(10) . . . . ? N16 Sc4 Sc5 Sc6 172.10(9) . . . . ? N17 Sc5 Sc6 N23 -139.7(2) . . . . ? N19 Sc5 Sc6 N23 -116.30(15) . . . . ? N20 Sc5 Sc6 N23 -61.31(13) . . . . ? N18 Sc5 Sc6 N23 177.79(13) . . . . ? Sc4 Sc5 Sc6 N23 57.55(13) . . . . ? N17 Sc5 Sc6 N21 62.3(2) . . . . ? N19 Sc5 Sc6 N21 85.63(13) . . . . ? N20 Sc5 Sc6 N21 140.62(11) . . . . ? N18 Sc5 Sc6 N21 19.72(11) . . . . ? Sc4 Sc5 Sc6 N21 -100.53(11) . . . . ? N17 Sc5 Sc6 N19 -23.4(2) . . . . ? N20 Sc5 Sc6 N19 54.99(12) . . . . ? N18 Sc5 Sc6 N19 -65.91(11) . . . . ? Sc4 Sc5 Sc6 N19 173.84(11) . . . . ? N17 Sc5 Sc6 N24 141.2(2) . . . . ? N19 Sc5 Sc6 N24 164.57(12) . . . . ? N20 Sc5 Sc6 N24 -140.44(10) . . . . ? N18 Sc5 Sc6 N24 98.67(10) . . . . ? Sc4 Sc5 Sc6 N24 -21.58(10) . . . . ? N17 Sc5 Sc6 N22 -37.8(3) . . . . ? N19 Sc5 Sc6 N22 -14.42(14) . . . . ? N20 Sc5 Sc6 N22 40.56(13) . . . . ? N18 Sc5 Sc6 N22 -80.33(13) . . . . ? Sc4 Sc5 Sc6 N22 159.42(11) . . . . ? N15 Sc4 N13 C31 58.4(3) . . . . ? N17 Sc4 N13 C31 -166.8(2) . . . . ? N14 Sc4 N13 C31 -11.0(2) . . . . ? N16 Sc4 N13 C31 121.3(3) . . . . ? Sc5 Sc4 N13 C31 -104.7(2) . . . . ? N15 Sc4 N13 C38 -82.2(3) . . . . ? N17 Sc4 N13 C38 52.6(3) . . . . ? N14 Sc4 N13 C38 -151.6(3) . . . . ? N16 Sc4 N13 C38 -19.4(2) . . . . ? Sc5 Sc4 N13 C38 114.7(2) . . . . ? N13 Sc4 N14 C39 -136.2(3) . . . . ? N15 Sc4 N14 C39 109.3(3) . . . . ? N17 Sc4 N14 C39 0.8(4) . . . . ? N16 Sc4 N14 C39 167.0(2) . . . . ? Sc5 Sc4 N14 C39 -8.3(3) . . . . ? N13 Sc4 N14 C32 -15.9(2) . . . . ? N15 Sc4 N14 C32 -130.3(2) . . . . ? N17 Sc4 N14 C32 121.2(3) . . . . ? N16 Sc4 N14 C32 -72.6(2) . . . . ? Sc5 Sc4 N14 C32 112.1(2) . . . . ? N13 Sc4 N14 C33 102.5(2) . . . . ? N15 Sc4 N14 C33 -11.9(2) . . . . ? N17 Sc4 N14 C33 -120.4(2) . . . . ? N16 Sc4 N14 C33 45.8(2) . . . . ? Sc5 Sc4 N14 C33 -129.5(2) . . . . ? N13 Sc4 N15 C34 -87.1(2) . . . . ? N17 Sc4 N15 C34 131.1(2) . . . . ? N14 Sc4 N15 C34 -19.1(2) . . . . ? N16 Sc4 N15 C34 -150.4(2) . . . . ? Sc5 Sc4 N15 C34 78.0(2) . . . . ? N13 Sc4 N15 C35 46.7(3) . . . . ? N17 Sc4 N15 C35 -95.1(3) . . . . ? N14 Sc4 N15 C35 114.6(3) . . . . ? N16 Sc4 N15 C35 -16.6(2) . . . . ? Sc5 Sc4 N15 C35 -148.2(2) . . . . ? N13 Sc4 N16 C40 107.9(3) . . . . ? N15 Sc4 N16 C40 -134.5(3) . . . . ? N17 Sc4 N16 C40 -21.2(3) . . . . ? N14 Sc4 N16 C40 165.6(2) . . . . ? Sc5 Sc4 N16 C40 -20.9(3) . . . . ? N13 Sc4 N16 C37 -13.4(2) . . . . ? N15 Sc4 N16 C37 104.1(2) . . . . ? N17 Sc4 N16 C37 -142.6(2) . . . . ? N14 Sc4 N16 C37 44.2(2) . . . . ? Sc5 Sc4 N16 C37 -142.28(18) . . . . ? N13 Sc4 N16 C36 -129.6(2) . . . . ? N15 Sc4 N16 C36 -12.0(2) . . . . ? N17 Sc4 N16 C36 101.3(2) . . . . ? N14 Sc4 N16 C36 -71.9(2) . . . . ? Sc5 Sc4 N16 C36 101.6(2) . . . . ? N13 Sc4 N17 C48 -132.8(2) . . . . ? N15 Sc4 N17 C48 1.4(3) . . . . ? N14 Sc4 N17 C48 100.9(3) . . . . ? N16 Sc4 N17 C48 -67.5(2) . . . . ? Sc5 Sc4 N17 C48 112.8(3) . . . . ? N13 Sc4 N17 C41 2.5(3) . . . . ? N15 Sc4 N17 C41 136.7(2) . . . . ? N14 Sc4 N17 C41 -123.8(2) . . . . ? N16 Sc4 N17 C41 67.9(2) . . . . ? Sc5 Sc4 N17 C41 -111.9(2) . . . . ? N13 Sc4 N17 Sc5 114.42(12) . . . . ? N15 Sc4 N17 Sc5 -111.43(10) . . . . ? N14 Sc4 N17 Sc5 -11.9(2) . . . . ? N16 Sc4 N17 Sc5 179.74(9) . . . . ? N19 Sc5 N17 C48 50.5(2) . . . . ? N20 Sc5 N17 C48 -13.7(2) . . . . ? N18 Sc5 N17 C48 113.8(2) . . . . ? Sc6 Sc5 N17 C48 69.3(3) . . . . ? Sc4 Sc5 N17 C48 -121.9(2) . . . . ? N19 Sc5 N17 C41 -75.0(2) . . . . ? N20 Sc5 N17 C41 -139.2(2) . . . . ? N18 Sc5 N17 C41 -11.7(2) . . . . ? Sc6 Sc5 N17 C41 -56.3(3) . . . . ? Sc4 Sc5 N17 C41 112.6(2) . . . . ? N19 Sc5 N17 Sc4 172.40(9) . . . . ? N20 Sc5 N17 Sc4 108.22(10) . . . . ? N18 Sc5 N17 Sc4 -124.31(10) . . . . ? Sc6 Sc5 N17 Sc4 -168.85(16) . . . . ? N17 Sc5 N18 C43 -137.5(2) . . . . ? N19 Sc5 N18 C43 -14.6(2) . . . . ? N20 Sc5 N18 C43 -75.8(2) . . . . ? Sc6 Sc5 N18 C43 29.4(2) . . . . ? Sc4 Sc5 N18 C43 -175.31(19) . . . . ? N17 Sc5 N18 C42 -17.61(19) . . . . ? N19 Sc5 N18 C42 105.3(2) . . . . ? N20 Sc5 N18 C42 44.1(2) . . . . ? Sc6 Sc5 N18 C42 149.36(19) . . . . ? Sc4 Sc5 N18 C42 -55.4(2) . . . . ? N17 Sc5 N18 C49 103.6(2) . . . . ? N19 Sc5 N18 C49 -133.5(2) . . . . ? N20 Sc5 N18 C49 165.3(2) . . . . ? Sc6 Sc5 N18 C49 -89.5(2) . . . . ? Sc4 Sc5 N18 C49 65.8(2) . . . . ? N23 Sc6 N19 C44 -138.4(2) . . . . ? N21 Sc6 N19 C44 -3.0(3) . . . . ? N24 Sc6 N19 C44 85.4(3) . . . . ? N22 Sc6 N19 C44 -76.9(2) . . . . ? Sc5 Sc6 N19 C44 113.2(3) . . . . ? N23 Sc6 N19 C45 -2.8(3) . . . . ? N21 Sc6 N19 C45 132.6(2) . . . . ? N24 Sc6 N19 C45 -139.0(2) . . . . ? N22 Sc6 N19 C45 58.7(2) . . . . ? Sc5 Sc6 N19 C45 -111.2(2) . . . . ? N23 Sc6 N19 Sc5 108.40(14) . . . . ? N21 Sc6 N19 Sc5 -116.19(10) . . . . ? N24 Sc6 N19 Sc5 -27.8(2) . . . . ? N22 Sc6 N19 Sc5 169.92(10) . . . . ? N17 Sc5 N19 C44 49.3(2) . . . . ? N20 Sc5 N19 C44 113.6(2) . . . . ? N18 Sc5 N19 C44 -14.2(2) . . . . ? Sc6 Sc5 N19 C44 -122.6(2) . . . . ? Sc4 Sc5 N19 C44 66.3(3) . . . . ? N17 Sc5 N19 C45 -75.4(2) . . . . ? N20 Sc5 N19 C45 -11.1(2) . . . . ? N18 Sc5 N19 C45 -138.9(2) . . . . ? Sc6 Sc5 N19 C45 112.7(2) . . . . ? Sc4 Sc5 N19 C45 -58.4(4) . . . . ? N17 Sc5 N19 Sc6 171.88(9) . . . . ? N20 Sc5 N19 Sc6 -123.85(10) . . . . ? N18 Sc5 N19 Sc6 108.37(10) . . . . ? Sc4 Sc5 N19 Sc6 -171.08(16) . . . . ? N17 Sc5 N20 C46 104.8(2) . . . . ? N19 Sc5 N20 C46 -17.7(2) . . . . ? N18 Sc5 N20 C46 43.3(2) . . . . ? Sc6 Sc5 N20 C46 -56.1(2) . . . . ? Sc4 Sc5 N20 C46 148.4(2) . . . . ? N17 Sc5 N20 C50 -133.8(2) . . . . ? N19 Sc5 N20 C50 103.6(2) . . . . ? N18 Sc5 N20 C50 164.6(2) . . . . ? Sc6 Sc5 N20 C50 65.2(2) . . . . ? Sc4 Sc5 N20 C50 -90.3(2) . . . . ? N17 Sc5 N20 C47 -14.6(2) . . . . ? N19 Sc5 N20 C47 -137.1(2) . . . . ? N18 Sc5 N20 C47 -76.2(2) . . . . ? Sc6 Sc5 N20 C47 -175.57(19) . . . . ? Sc4 Sc5 N20 C47 29.0(2) . . . . ? N23 Sc6 N21 C58 -66.8(3) . . . . ? N19 Sc6 N21 C58 146.5(3) . . . . ? N24 Sc6 N21 C58 1.9(3) . . . . ? N22 Sc6 N21 C58 -130.4(3) . . . . ? Sc5 Sc6 N21 C58 95.2(3) . . . . ? N23 Sc6 N21 C51 69.7(3) . . . . ? N19 Sc6 N21 C51 -77.0(3) . . . . ? N24 Sc6 N21 C51 138.4(3) . . . . ? N22 Sc6 N21 C51 6.1(3) . . . . ? Sc5 Sc6 N21 C51 -128.3(2) . . . . ? N23 Sc6 N22 C52 -92.7(2) . . . . ? N21 Sc6 N22 C52 23.1(2) . . . . ? N19 Sc6 N22 C52 130.9(2) . . . . ? N24 Sc6 N22 C52 -37.1(3) . . . . ? Sc5 Sc6 N22 C52 141.7(2) . . . . ? N23 Sc6 N22 C59 145.3(3) . . . . ? N21 Sc6 N22 C59 -98.9(3) . . . . ? N19 Sc6 N22 C59 8.9(3) . . . . ? N24 Sc6 N22 C59 -159.1(3) . . . . ? Sc5 Sc6 N22 C59 19.7(4) . . . . ? N23 Sc6 N22 C53 22.0(2) . . . . ? N21 Sc6 N22 C53 137.8(3) . . . . ? N19 Sc6 N22 C53 -114.4(2) . . . . ? N24 Sc6 N22 C53 77.6(3) . . . . ? Sc5 Sc6 N22 C53 -103.6(2) . . . . ? N21 Sc6 N23 C54 -67.1(3) . . . . ? N19 Sc6 N23 C54 67.8(4) . . . . ? N24 Sc6 N23 C54 -135.9(3) . . . . ? N22 Sc6 N23 C54 -0.6(3) . . . . ? Sc5 Sc6 N23 C54 132.8(3) . . . . ? N21 Sc6 N23 C55 81.7(3) . . . . ? N19 Sc6 N23 C55 -143.5(2) . . . . ? N24 Sc6 N23 C55 12.8(3) . . . . ? N22 Sc6 N23 C55 148.1(3) . . . . ? Sc5 Sc6 N23 C55 -78.5(3) . . . . ? N23 Sc6 N24 C60 -109.4(3) . . . . ? N21 Sc6 N24 C60 136.7(3) . . . . ? N19 Sc6 N24 C60 38.6(4) . . . . ? N22 Sc6 N24 C60 -163.1(3) . . . . ? Sc5 Sc6 N24 C60 17.7(3) . . . . ? N23 Sc6 N24 C56 14.8(3) . . . . ? N21 Sc6 N24 C56 -99.1(3) . . . . ? N19 Sc6 N24 C56 162.7(3) . . . . ? N22 Sc6 N24 C56 -38.9(3) . . . . ? Sc5 Sc6 N24 C56 141.9(3) . . . . ? N23 Sc6 N24 C57 132.8(3) . . . . ? N21 Sc6 N24 C57 18.9(3) . . . . ? N19 Sc6 N24 C57 -79.2(3) . . . . ? N22 Sc6 N24 C57 79.1(3) . . . . ? Sc5 Sc6 N24 C57 -100.1(3) . . . . ? C38 N13 C31 C32 178.2(3) . . . . ? Sc4 N13 C31 C32 35.8(4) . . . . ? C39 N14 C32 C31 164.5(3) . . . . ? C33 N14 C32 C31 -73.4(4) . . . . ? Sc4 N14 C32 C31 39.3(3) . . . . ? N13 C31 C32 N14 -50.4(4) . . . . ? C39 N14 C33 C34 -86.4(3) . . . . ? C32 N14 C33 C34 152.4(3) . . . . ? Sc4 N14 C33 C34 38.9(3) . . . . ? C35 N15 C34 C33 -90.4(3) . . . . ? Sc4 N15 C34 C33 48.3(3) . . . . ? N14 C33 C34 N15 -59.9(4) . . . . ? C34 N15 C35 C36 178.7(3) . . . . ? Sc4 N15 C35 C36 43.9(4) . . . . ? C40 N16 C36 C35 169.7(3) . . . . ? C37 N16 C36 C35 -71.4(4) . . . . ? Sc4 N16 C36 C35 37.2(3) . . . . ? N15 C35 C36 N16 -54.5(4) . . . . ? C40 N16 C37 C38 -90.9(3) . . . . ? C36 N16 C37 C38 149.9(3) . . . . ? Sc4 N16 C37 C38 41.0(3) . . . . ? C31 N13 C38 C37 -92.2(4) . . . . ? Sc4 N13 C38 C37 51.2(4) . . . . ? N16 C37 C38 N13 -62.9(4) . . . . ? C48 N17 C41 C42 -86.0(3) . . . . ? Sc4 N17 C41 C42 134.1(2) . . . . ? Sc5 N17 C41 C42 40.1(3) . . . . ? C43 N18 C42 C41 160.9(3) . . . . ? C49 N18 C42 C41 -79.1(3) . . . . ? Sc5 N18 C42 C41 44.1(3) . . . . ? N17 C41 C42 N18 -58.5(4) . . . . ? C42 N18 C43 C44 -75.3(3) . . . . ? C49 N18 C43 C44 163.5(3) . . . . ? Sc5 N18 C43 C44 41.1(3) . . . . ? C45 N19 C44 C43 166.8(3) . . . . ? Sc6 N19 C44 C43 -56.5(3) . . . . ? Sc5 N19 C44 C43 41.3(3) . . . . ? N18 C43 C44 N19 -57.0(4) . . . . ? C44 N19 C45 C46 -86.9(3) . . . . ? Sc6 N19 C45 C46 132.3(3) . . . . ? Sc5 N19 C45 C46 39.1(3) . . . . ? C50 N20 C46 C45 -79.6(3) . . . . ? C47 N20 C46 C45 160.4(3) . . . . ? Sc5 N20 C46 C45 43.6(3) . . . . ? N19 C45 C46 N20 -57.3(4) . . . . ? C46 N20 C47 C48 -76.0(3) . . . . ? C50 N20 C47 C48 163.0(3) . . . . ? Sc5 N20 C47 C48 40.9(3) . . . . ? C41 N17 C48 C47 166.7(3) . . . . ? Sc4 N17 C48 C47 -57.3(3) . . . . ? Sc5 N17 C48 C47 40.6(3) . . . . ? N20 C47 C48 N17 -56.4(4) . . . . ? C58 N21 C51 C52 104.1(4) . . . . ? Sc6 N21 C51 C52 -35.3(4) . . . . ? C59 N22 C52 C51 84.3(4) . . . . ? C53 N22 C52 C51 -157.5(3) . . . . ? Sc6 N22 C52 C51 -48.2(3) . . . . ? N21 C51 C52 N22 60.0(4) . . . . ? C52 N22 C53 C54 65.6(4) . . . . ? C59 N22 C53 C54 -175.0(3) . . . . ? Sc6 N22 C53 C54 -40.8(4) . . . . ? C55 N23 C54 C53 -171.7(3) . . . . ? Sc6 N23 C54 C53 -22.1(5) . . . . ? N22 C53 C54 N23 43.3(5) . . . . ? C54 N23 C55 C56 113.4(4) . . . . ? Sc6 N23 C55 C56 -39.6(4) . . . . ? C60 N24 C56 C55 88.3(4) . . . . ? C57 N24 C56 C55 -152.3(4) . . . . ? Sc6 N24 C56 C55 -39.3(4) . . . . ? N23 C55 C56 N24 53.3(5) . . . . ? C60 N24 C57 C58 -162.4(4) . . . . ? C56 N24 C57 C58 76.0(5) . . . . ? Sc6 N24 C57 C58 -38.5(4) . . . . ? C51 N21 C58 C57 -162.8(4) . . . . ? Sc6 N21 C58 C57 -24.3(5) . . . . ? N24 C57 C58 N21 43.8(6) . . . . ? C61A C62A C63A C64A -173.0(9) . . . . ? C62A C63A C64A C65A 71.1(11) . . . . ? C63A C64A C65A C66A 67.9(11) . . . . ? C61B C62B C63B C64B 158(2) . . . . ? C62B C63B C64B C65B -64(3) . . . . ? C63B C64B C65B C66B 140(2) . . . . ? C61C C62C C63C C64C -162.3(16) . . . . ? C62C C63C C64C C65C 178.2(17) . . . . ? C63C C64C C65C C66C -107(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.275 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.077 _shelx_res_file ; TITL 2 REM transformed to space group : P121/c1:b1 CELL 0.71073 18.0667 19.2883 28.4424 90.000 125.387 90.000 ZERR 4 0.0009 0.0010 0.0011 0.000 0.002 0.000 LATT 1 SYMM -X,1/2+Y,1/2-Z SFAC C H N SC UNIT 264 608 96 24 SIZE 0.14 0.23 0.29 TEMP -173 REM colourless block DFIX 1.5 C61A C62A DFIX 1.5 C62A C63A DFIX 1.5 C63A C64A DFIX 1.5 C64A C65A DFIX 1.5 C65A C66A DFIX 2.4 C61A C63A DFIX 2.4 C62A C64A DFIX 2.4 C63A C65A DFIX 2.4 C64A C66A DFIX 1.5 C61B C62B DFIX 1.5 C62B C63B DFIX 1.5 C63B C64B DFIX 1.5 C64B C65B DFIX 1.5 C65B C66B DFIX 2.4 C61B C63B DFIX 2.4 C62B C64B DFIX 2.4 C63B C65B DFIX 2.4 C64B C66B DFIX 1.5 C61C C62C DFIX 1.5 C62C C63C DFIX 1.5 C63C C64C DFIX 1.5 C64C C65C DFIX 1.5 C65C C66C DFIX 2.4 C61C C63C DFIX 2.4 C62C C64C DFIX 2.4 C63C C65C DFIX 2.4 C64C C66C OMIT 0 -2 0 L.S. 16 FMAP 2 PLAN -25 ACTA CONF BOND $H REM no correction for extinction WGHT 0.059900 2.061800 FVAR 0.04000 0.04145 0.06282 0.03407 MOLE 1 SC1 4 0.602157 0.448480 0.694183 11.00000 0.01664 0.01624 = 0.01736 -0.00147 0.01096 -0.00015 SC2 4 0.476087 0.496081 0.737517 11.00000 0.01704 0.01310 = 0.01748 0.00020 0.01125 0.00037 SC3 4 0.567183 0.613382 0.703990 11.00000 0.01891 0.01401 = 0.01561 0.00120 0.00952 -0.00152 H1 2 0.612378 0.519202 0.756694 11.00000 -1.20000 H2 2 0.486233 0.519807 0.666533 11.00000 -1.20000 N1 3 0.526084 0.398949 0.723867 11.00000 0.02277 0.01327 = 0.02847 0.00083 0.01747 0.00090 N2 3 0.723805 0.394832 0.783093 11.00000 0.02454 0.01894 = 0.02233 0.00242 0.01422 0.00753 N3 3 0.660806 0.373982 0.671976 11.00000 0.01988 0.02860 = 0.02156 -0.00387 0.01200 0.00254 N4 3 0.478313 0.386279 0.605988 11.00000 0.01987 0.02792 = 0.02322 -0.00701 0.01016 -0.00201 N5 3 0.483331 0.611961 0.738150 11.00000 0.02234 0.01403 = 0.02066 -0.00067 0.01261 0.00239 N6 3 0.316464 0.534134 0.661757 11.00000 0.02057 0.03374 = 0.03944 0.00887 0.01137 -0.00053 N7 3 0.395376 0.454607 0.760307 11.00000 0.02748 0.02728 = 0.02662 -0.00178 0.01895 -0.00490 N8 3 0.551793 0.522269 0.839363 11.00000 0.02690 0.02742 = 0.02150 -0.00062 0.01609 0.00169 N9 3 0.647900 0.550468 0.682482 11.00000 0.03317 0.02162 = 0.03081 0.00111 0.02599 -0.00232 N10 3 0.488942 0.633868 0.600506 11.00000 0.04599 0.02314 = 0.01664 0.00117 0.00897 -0.00916 N11 3 0.573445 0.719400 0.692895 11.00000 0.02968 0.01696 = 0.02534 0.00233 0.01322 -0.00318 N12 3 0.718893 0.651985 0.778614 11.00000 0.02596 0.02449 = 0.02418 0.00057 0.01255 -0.00507 C1 1 0.613378 0.333288 0.619773 11.00000 0.02997 0.03009 = 0.02798 -0.00678 0.01954 -0.00164 AFIX 23 H1A 2 0.607751 0.284838 0.628817 11.00000 -1.20000 H1B 2 0.648409 0.333015 0.602953 11.00000 -1.20000 AFIX 0 C2 1 0.521296 0.362651 0.577243 11.00000 0.03201 0.03629 = 0.02843 -0.01340 0.01677 -0.00671 AFIX 23 H2A 2 0.526174 0.402292 0.557072 11.00000 -1.20000 H2B 2 0.482495 0.326955 0.548077 11.00000 -1.20000 AFIX 0 C3 1 0.465058 0.328258 0.634836 11.00000 0.03388 0.02924 = 0.04406 -0.01451 0.02527 -0.01414 AFIX 23 H3A 2 0.519383 0.298035 0.654725 11.00000 -1.20000 H3B 2 0.412201 0.300041 0.605588 11.00000 -1.20000 AFIX 0 C4 1 0.449264 0.356383 0.678451 11.00000 0.03339 0.02455 = 0.04811 -0.01559 0.03140 -0.01517 AFIX 23 H4A 2 0.393368 0.384888 0.657975 11.00000 -1.20000 H4B 2 0.439732 0.317051 0.696756 11.00000 -1.20000 AFIX 0 C5 1 0.588218 0.361562 0.778746 11.00000 0.04395 0.02471 = 0.04385 0.01302 0.03324 0.00916 AFIX 23 H5A 2 0.555748 0.321356 0.780417 11.00000 -1.20000 H5B 2 0.605272 0.392766 0.811206 11.00000 -1.20000 AFIX 0 C6 1 0.673611 0.336166 0.786290 11.00000 0.03668 0.03215 = 0.03326 0.01196 0.02150 0.01052 AFIX 23 H6A 2 0.712962 0.312777 0.824104 11.00000 -1.20000 H6B 2 0.657506 0.301972 0.755784 11.00000 -1.20000 AFIX 0 C7 1 0.791175 0.370114 0.772095 11.00000 0.02596 0.04005 = 0.02947 0.00492 0.01583 0.01250 AFIX 23 H7A 2 0.828276 0.409757 0.774803 11.00000 -1.20000 H7B 2 0.832412 0.335812 0.801906 11.00000 -1.20000 AFIX 0 C8 1 0.744473 0.337873 0.714082 11.00000 0.02374 0.04013 = 0.03208 -0.00003 0.01783 0.00809 AFIX 23 H8A 2 0.785341 0.338817 0.701489 11.00000 -1.20000 H8B 2 0.730690 0.288803 0.716309 11.00000 -1.20000 AFIX 0 C9 1 0.776718 0.430963 0.838781 11.00000 0.03625 0.03250 = 0.02337 0.00211 0.01045 0.01276 AFIX 137 H9A 2 0.735593 0.457088 0.844141 11.00000 -1.50000 H9B 2 0.819473 0.462942 0.839454 11.00000 -1.50000 H9C 2 0.810413 0.396980 0.869927 11.00000 -1.50000 AFIX 0 C10 1 0.388099 0.413539 0.559824 11.00000 0.02351 0.05605 = 0.04049 -0.01017 0.00797 -0.00211 AFIX 137 H10A 2 0.394763 0.447918 0.537141 11.00000 -1.50000 H10B 2 0.360039 0.435400 0.577003 11.00000 -1.50000 H10C 2 0.349593 0.375401 0.534676 11.00000 -1.50000 AFIX 0 PART 1 C11A 1 0.393603 0.645402 0.707637 10.66154 0.02606 AFIX 23 H11A 2 0.373165 0.646220 0.733273 10.66154 -1.20000 H11B 2 0.399157 0.694011 0.698879 10.66154 -1.20000 AFIX 0 C12A 1 0.325783 0.610454 0.654459 10.66154 0.03786 AFIX 23 H12A 2 0.341676 0.615999 0.626695 10.66154 -1.20000 H12B 2 0.266349 0.633200 0.637725 10.66154 -1.20000 AFIX 0 C13A 1 0.267325 0.520304 0.688977 10.66154 0.02567 AFIX 23 H13A 2 0.200774 0.521423 0.659679 10.66154 -1.20000 H13B 2 0.283763 0.555194 0.719091 10.66154 -1.20000 AFIX 0 C14A 1 0.298597 0.447436 0.715566 10.66154 0.02466 AFIX 23 H14A 2 0.266076 0.432247 0.732271 10.66154 -1.20000 H14B 2 0.287511 0.413296 0.686139 10.66154 -1.20000 AFIX 0 PART 2 C11B 1 0.399578 0.643859 0.690608 10.33846 0.02683 AFIX 23 H11C 2 0.396898 0.641535 0.654878 10.33846 -1.20000 H11D 2 0.397714 0.693227 0.699396 10.33846 -1.20000 AFIX 0 C12B 1 0.315610 0.603682 0.681736 10.33846 0.02555 AFIX 23 H12C 2 0.321394 0.601229 0.718502 10.33846 -1.20000 H12D 2 0.258164 0.627710 0.652793 10.33846 -1.20000 AFIX 0 C13B 1 0.259136 0.480692 0.665830 10.33846 0.08032 AFIX 23 H13C 2 0.196757 0.498855 0.646926 10.33846 -1.20000 H13D 2 0.255584 0.438112 0.645175 10.33846 -1.20000 AFIX 0 C14B 1 0.296164 0.464164 0.724166 10.33846 0.03681 AFIX 23 H14C 2 0.267357 0.421059 0.725168 10.33846 -1.20000 H14D 2 0.280831 0.501761 0.740851 10.33846 -1.20000 AFIX 0 PART 0 C15 1 0.416406 0.458929 0.817245 11.00000 0.04469 0.02309 = 0.03804 -0.00108 0.03268 -0.00276 AFIX 23 H15A 2 0.398495 0.415247 0.826405 11.00000 -1.20000 H15B 2 0.381442 0.497287 0.818772 11.00000 -1.20000 AFIX 0 C16 1 0.515108 0.471149 0.860649 11.00000 0.04466 0.02860 = 0.02882 0.00626 0.02730 0.00323 AFIX 23 H16A 2 0.548146 0.426711 0.869534 11.00000 -1.20000 H16B 2 0.525449 0.488757 0.896706 11.00000 -1.20000 AFIX 0 C17 1 0.515202 0.591944 0.834543 11.00000 0.04112 0.02595 = 0.02700 -0.00530 0.02283 -0.00009 AFIX 23 H17A 2 0.545271 0.612588 0.873408 11.00000 -1.20000 H17B 2 0.449298 0.588934 0.816829 11.00000 -1.20000 AFIX 0 C18 1 0.531352 0.637481 0.797665 11.00000 0.04355 0.01955 = 0.03698 -0.00814 0.02894 -0.00883 AFIX 23 H18A 2 0.510768 0.685230 0.797122 11.00000 -1.20000 H18B 2 0.597267 0.639273 0.815212 11.00000 -1.20000 AFIX 0 PART 1 C19A 1 0.265396 0.504867 0.603015 10.66154 0.03370 AFIX 137 H19A 2 0.257964 0.454814 0.604782 10.66154 -1.50000 H19B 2 0.298760 0.513454 0.586052 10.66154 -1.50000 H19C 2 0.205536 0.526887 0.579187 10.66154 -1.50000 AFIX 0 PART 2 C19B 1 0.275585 0.538468 0.600213 10.33846 0.05990 AFIX 137 H19D 2 0.272780 0.492071 0.585215 10.33846 -1.50000 H19E 2 0.312380 0.568817 0.593735 10.33846 -1.50000 H19F 2 0.214075 0.557433 0.580260 10.33846 -1.50000 AFIX 0 PART 0 C20 1 0.650898 0.521983 0.883077 11.00000 0.02820 0.03728 = 0.01972 -0.00302 0.01280 0.00081 AFIX 137 H20A 2 0.679982 0.550985 0.869827 11.00000 -1.50000 H20B 2 0.673751 0.474412 0.888956 11.00000 -1.50000 H20C 2 0.664839 0.540361 0.919506 11.00000 -1.50000 AFIX 0 C21 1 0.649964 0.763538 0.731033 11.00000 0.03982 0.02207 = 0.03386 -0.00550 0.02378 -0.00774 AFIX 23 H21A 2 0.628671 0.807519 0.737356 11.00000 -1.20000 H21B 2 0.682479 0.774622 0.713472 11.00000 -1.20000 AFIX 0 C22 1 0.712381 0.727479 0.787105 11.00000 0.03295 0.02207 = 0.03251 -0.00889 0.01913 -0.01128 AFIX 23 H22A 2 0.690052 0.733570 0.811461 11.00000 -1.20000 H22B 2 0.773494 0.748628 0.807515 11.00000 -1.20000 AFIX 0 C23 1 0.762911 0.640173 0.748647 11.00000 0.02705 0.03523 = 0.04605 -0.00735 0.02471 -0.00646 AFIX 23 H23A 2 0.829030 0.648528 0.775627 11.00000 -1.20000 H23B 2 0.737987 0.672914 0.715985 11.00000 -1.20000 AFIX 0 C24 1 0.745692 0.565033 0.726166 11.00000 0.03440 0.02694 = 0.07075 -0.00556 0.04095 -0.00336 AFIX 23 H24A 2 0.779243 0.556511 0.708905 11.00000 -1.20000 H24B 2 0.769534 0.532731 0.759003 11.00000 -1.20000 AFIX 0 C25 1 0.621284 0.564549 0.623912 11.00000 0.09065 0.03886 = 0.04560 -0.00087 0.05473 0.00177 AFIX 23 H25A 2 0.586639 0.524370 0.599033 11.00000 -1.20000 H25B 2 0.676792 0.569271 0.624965 11.00000 -1.20000 AFIX 0 PART 1 C26A 1 0.563144 0.630580 0.596697 10.66154 0.03486 AFIX 23 H26A 2 0.602174 0.671688 0.616139 10.66154 -1.20000 H26B 2 0.540172 0.632606 0.555565 10.66154 -1.20000 AFIX 0 C27A 1 0.448009 0.705649 0.590604 10.66154 0.03883 AFIX 23 H27A 2 0.396173 0.704667 0.593684 10.66154 -1.20000 H27B 2 0.426323 0.722958 0.551843 10.66154 -1.20000 AFIX 0 C28A 1 0.523955 0.752028 0.637512 10.66154 0.03286 AFIX 23 H28A 2 0.566225 0.763578 0.627156 10.66154 -1.20000 H28B 2 0.497349 0.795880 0.639444 10.66154 -1.20000 AFIX 0 PART 2 C26B 1 0.538304 0.579633 0.585183 10.33846 0.03124 AFIX 23 H26C 2 0.503012 0.535972 0.573119 10.33846 -1.20000 H26D 2 0.534569 0.597629 0.551269 10.33846 -1.20000 AFIX 0 C27B 1 0.519841 0.705549 0.596583 10.33846 0.03287 AFIX 23 H27C 2 0.483568 0.722074 0.556165 10.33846 -1.20000 H27D 2 0.584748 0.705009 0.611426 10.33846 -1.20000 AFIX 0 C28B 1 0.504153 0.753599 0.635304 10.33846 0.01717 AFIX 23 H28C 2 0.518956 0.802748 0.634281 10.33846 -1.20000 H28D 2 0.441569 0.749927 0.624731 10.33846 -1.20000 AFIX 0 PART 0 C29 1 0.776452 0.621403 0.836915 11.00000 0.01980 0.03244 = 0.03155 0.00437 0.00838 -0.00274 AFIX 137 H29A 2 0.777142 0.570842 0.833794 11.00000 -1.50000 H29B 2 0.751954 0.633739 0.858827 11.00000 -1.50000 H29C 2 0.838449 0.639338 0.856804 11.00000 -1.50000 AFIX 0 PART 1 C30A 1 0.412233 0.589460 0.555529 10.66154 0.05216 AFIX 137 H30A 2 0.359876 0.595501 0.557133 10.66154 -1.50000 H30B 2 0.431079 0.540734 0.562665 10.66154 -1.50000 H30C 2 0.395488 0.603051 0.517322 10.66154 -1.50000 AFIX 0 PART 2 C30B 1 0.394292 0.624283 0.557529 10.33846 0.02526 AFIX 137 H30D 2 0.359798 0.658107 0.563333 10.33846 -1.50000 H30E 2 0.376765 0.577263 0.560467 10.33846 -1.50000 H30F 2 0.381234 0.630888 0.519239 10.33846 -1.50000 AFIX 0 PART 0 MOLE 2 SC4 4 0.202934 0.538228 0.919560 11.00000 0.01475 0.01422 = 0.01647 -0.00120 0.00911 -0.00128 H3 2 0.219074 0.447339 0.963788 11.00000 -1.20000 H4 2 0.096718 0.470666 0.875155 11.00000 -1.20000 SC5 4 0.162318 0.381678 0.896511 11.00000 0.01277 0.01380 = 0.01403 -0.00137 0.00792 -0.00133 SC6 4 0.080392 0.245820 0.904663 11.00000 0.01519 0.01520 = 0.01527 -0.00034 0.00811 -0.00197 H5 2 0.046878 0.344065 0.879015 11.00000 -1.20000 H6 2 0.175106 0.316255 0.951562 11.00000 -1.20000 N13 3 0.288830 0.592005 0.999595 11.00000 0.02235 0.01887 = 0.02074 -0.00371 0.01275 -0.00301 N14 3 0.103301 0.574760 0.947937 11.00000 0.02162 0.01924 = 0.02248 0.00108 0.01347 0.00089 N15 3 0.113030 0.611131 0.854088 11.00000 0.01731 0.01524 = 0.02205 0.00118 0.01046 -0.00179 N16 3 0.302432 0.628169 0.906790 11.00000 0.01823 0.01897 = 0.01860 -0.00079 0.00894 -0.00220 N17 3 0.248901 0.458103 0.884324 11.00000 0.01369 0.01918 = 0.01525 0.00095 0.00836 0.00121 N18 3 0.315892 0.331497 0.950878 11.00000 0.01345 0.01623 = 0.01560 -0.00091 0.00768 0.00093 N19 3 0.146100 0.271319 0.858850 11.00000 0.01717 0.01666 = 0.01425 -0.00254 0.00891 -0.00128 N20 3 0.078363 0.397802 0.792369 11.00000 0.01676 0.01873 = 0.01787 0.00053 0.01043 -0.00087 N21 3 0.165485 0.170067 0.969204 11.00000 0.02321 0.01673 = 0.01703 -0.00012 0.01063 -0.00049 N22 3 0.031284 0.129908 0.850833 11.00000 0.03474 0.02285 = 0.02125 -0.00656 0.01444 -0.01013 N23 3 -0.057099 0.225342 0.873357 11.00000 0.01854 0.02799 = 0.02649 0.00343 0.01019 -0.00253 N24 3 0.072572 0.273577 0.984933 11.00000 0.02728 0.01850 = 0.02684 0.00292 0.01921 0.00196 C31 1 0.248841 0.630766 1.022885 11.00000 0.03019 0.02014 = 0.01650 -0.00250 0.00842 0.00232 AFIX 23 H31A 2 0.232121 0.677739 1.005696 11.00000 -1.20000 H31B 2 0.293202 0.635662 1.065141 11.00000 -1.20000 AFIX 0 C32 1 0.165080 0.593241 1.009542 11.00000 0.02887 0.02864 = 0.02333 0.00117 0.01756 0.00841 AFIX 23 H32A 2 0.183701 0.550526 1.033108 11.00000 -1.20000 H32B 2 0.132474 0.623215 1.020203 11.00000 -1.20000 AFIX 0 C33 1 0.054490 0.635672 0.910993 11.00000 0.02078 0.01874 = 0.03076 -0.00010 0.01689 0.00170 AFIX 23 H33A 2 0.093105 0.677496 0.927878 11.00000 -1.20000 H33B 2 -0.001811 0.643679 0.908505 11.00000 -1.20000 AFIX 0 C34 1 0.031075 0.622382 0.850730 11.00000 0.01747 0.01903 = 0.02237 0.00248 0.00834 0.00101 AFIX 23 H34A 2 -0.008683 0.581160 0.833625 11.00000 -1.20000 H34B 2 -0.002205 0.662703 0.825571 11.00000 -1.20000 AFIX 0 C35 1 0.146583 0.676041 0.848029 11.00000 0.02386 0.01928 = 0.01975 0.00342 0.00959 0.00132 AFIX 23 H35A 2 0.157895 0.708642 0.878428 11.00000 -1.20000 H35B 2 0.100357 0.696905 0.810090 11.00000 -1.20000 AFIX 0 C36 1 0.232712 0.664704 0.852835 11.00000 0.02597 0.02015 = 0.02071 0.00387 0.01264 -0.00315 AFIX 23 H36A 2 0.219312 0.637152 0.819371 11.00000 -1.20000 H36B 2 0.257111 0.710101 0.851608 11.00000 -1.20000 AFIX 0 C37 1 0.340399 0.672709 0.958051 11.00000 0.02130 0.01939 = 0.02191 -0.00128 0.00880 -0.00686 AFIX 23 H37A 2 0.294422 0.706870 0.951528 11.00000 -1.20000 H37B 2 0.393852 0.698272 0.965681 11.00000 -1.20000 AFIX 0 C38 1 0.368133 0.626495 1.009384 11.00000 0.02283 0.02369 = 0.01761 -0.00298 0.00603 -0.00803 AFIX 23 H38A 2 0.412492 0.591424 1.014829 11.00000 -1.20000 H38B 2 0.397501 0.654942 1.044846 11.00000 -1.20000 AFIX 0 C39 1 0.037863 0.522735 0.941007 11.00000 0.03137 0.02294 = 0.04358 0.00032 0.02858 -0.00059 AFIX 137 H39A 2 0.004086 0.541776 0.955312 11.00000 -1.50000 H39B 2 0.070569 0.480994 0.962990 11.00000 -1.50000 H39C 2 -0.004564 0.510854 0.900111 11.00000 -1.50000 AFIX 0 C40 1 0.377105 0.608087 0.902978 11.00000 0.02291 0.02597 = 0.03043 -0.00510 0.01522 -0.00681 AFIX 137 H40A 2 0.401412 0.649430 0.896340 11.00000 -1.50000 H40B 2 0.354579 0.575539 0.870946 11.00000 -1.50000 H40C 2 0.425219 0.585877 0.939103 11.00000 -1.50000 AFIX 0 C41 1 0.346104 0.443056 0.923577 11.00000 0.01611 0.01782 = 0.02113 -0.00108 0.01134 -0.00271 AFIX 23 H41A 2 0.370217 0.463000 0.961988 11.00000 -1.20000 H41B 2 0.378335 0.465205 0.908837 11.00000 -1.20000 AFIX 0 C42 1 0.364020 0.365610 0.929463 11.00000 0.01332 0.02373 = 0.02190 -0.00267 0.01123 -0.00159 AFIX 23 H42A 2 0.343153 0.345900 0.891520 11.00000 -1.20000 H42B 2 0.430047 0.356967 0.956590 11.00000 -1.20000 AFIX 0 C43 1 0.305508 0.256438 0.939141 11.00000 0.01805 0.01555 = 0.02617 0.00007 0.01379 0.00082 AFIX 23 H43A 2 0.289768 0.233530 0.963414 11.00000 -1.20000 H43B 2 0.363926 0.236977 0.949578 11.00000 -1.20000 AFIX 0 C44 1 0.232309 0.241309 0.876226 11.00000 0.02211 0.01657 = 0.02479 -0.00442 0.01546 -0.00087 AFIX 23 H44A 2 0.250445 0.260717 0.852074 11.00000 -1.20000 H44B 2 0.225422 0.190530 0.870087 11.00000 -1.20000 AFIX 0 C45 1 0.081891 0.270735 0.795879 11.00000 0.02205 0.01908 = 0.01663 -0.00573 0.00907 -0.00479 AFIX 23 H45A 2 0.019197 0.268349 0.785261 11.00000 -1.20000 H45B 2 0.092470 0.228841 0.780422 11.00000 -1.20000 AFIX 0 C46 1 0.091366 0.334618 0.768710 11.00000 0.02304 0.02363 = 0.01422 -0.00503 0.00990 -0.00441 AFIX 23 H46A 2 0.152389 0.335340 0.776574 11.00000 -1.20000 H46B 2 0.045623 0.333199 0.726399 11.00000 -1.20000 AFIX 0 C47 1 0.117326 0.459187 0.783016 11.00000 0.02205 0.02081 = 0.01314 0.00037 0.00956 -0.00016 AFIX 23 H47A 2 0.092135 0.501771 0.788151 11.00000 -1.20000 H47B 2 0.099675 0.458722 0.742939 11.00000 -1.20000 AFIX 0 C48 1 0.219577 0.460499 0.824396 11.00000 0.02055 0.02017 = 0.01980 -0.00153 0.01338 -0.00308 AFIX 23 H48A 2 0.245190 0.420303 0.816714 11.00000 -1.20000 H48B 2 0.243061 0.503277 0.818132 11.00000 -1.20000 AFIX 0 C49 1 0.366696 0.341167 1.013753 11.00000 0.01873 0.02481 = 0.01514 -0.00152 0.00627 -0.00155 AFIX 137 H49A 2 0.332034 0.321341 1.027160 11.00000 -1.50000 H49B 2 0.376211 0.390783 1.022801 11.00000 -1.50000 H49C 2 0.425607 0.317804 1.033085 11.00000 -1.50000 AFIX 0 C50 1 -0.019518 0.410269 0.763967 11.00000 0.01695 0.03091 = 0.02388 0.00163 0.00956 -0.00103 AFIX 137 H50A 2 -0.049102 0.419048 0.722802 11.00000 -1.50000 H50B 2 -0.027488 0.450612 0.781569 11.00000 -1.50000 H50C 2 -0.046886 0.369416 0.768691 11.00000 -1.50000 AFIX 0 C51 1 0.158253 0.099296 0.949016 11.00000 0.02728 0.01906 = 0.03474 0.00115 0.01000 0.00204 AFIX 23 H51A 2 0.178073 0.066548 0.981066 11.00000 -1.20000 H51B 2 0.198876 0.093422 0.936516 11.00000 -1.20000 AFIX 0 C52 1 0.061609 0.082698 0.899208 11.00000 0.04377 0.01747 = 0.03267 -0.00282 0.01956 -0.00580 AFIX 23 H52A 2 0.058170 0.034252 0.886584 11.00000 -1.20000 H52B 2 0.021133 0.087200 0.911939 11.00000 -1.20000 AFIX 0 C53 1 -0.070340 0.134332 0.812074 11.00000 0.03414 0.03831 = 0.02799 -0.00901 0.00669 -0.01481 AFIX 23 H53A 2 -0.088952 0.161909 0.777498 11.00000 -1.20000 H53B 2 -0.095754 0.087116 0.799106 11.00000 -1.20000 AFIX 0 C54 1 -0.108444 0.166495 0.841062 11.00000 0.02430 0.02763 = 0.05029 0.00368 0.01026 -0.00490 AFIX 23 H54A 2 -0.172125 0.180450 0.811767 11.00000 -1.20000 H54B 2 -0.108243 0.132208 0.867037 11.00000 -1.20000 AFIX 0 C55 1 -0.084823 0.252283 0.909229 11.00000 0.02148 0.06170 = 0.04434 0.02332 0.02225 0.01255 AFIX 23 H55A 2 -0.139924 0.227503 0.899682 11.00000 -1.20000 H55B 2 -0.099991 0.302103 0.900753 11.00000 -1.20000 AFIX 0 C56 1 -0.011621 0.243435 0.971427 11.00000 0.05177 0.05938 = 0.06287 -0.01404 0.04747 -0.01155 AFIX 23 H56A 2 -0.029253 0.266385 0.994706 11.00000 -1.20000 H56B 2 -0.002512 0.193485 0.981248 11.00000 -1.20000 AFIX 0 C57 1 0.153471 0.238675 1.035163 11.00000 0.06634 0.05290 = 0.03380 0.01404 0.03096 0.02406 AFIX 23 H57A 2 0.207045 0.268964 1.050407 11.00000 -1.20000 H57B 2 0.143972 0.233087 1.065917 11.00000 -1.20000 AFIX 0 C58 1 0.172790 0.171418 1.022043 11.00000 0.02893 0.04772 = 0.02317 0.00949 0.01351 0.01733 AFIX 23 H58A 2 0.235050 0.157405 1.053985 11.00000 -1.20000 H58B 2 0.130167 0.136992 1.019754 11.00000 -1.20000 AFIX 0 C59 1 0.061422 0.103292 0.816099 11.00000 0.05448 0.02173 = 0.04215 -0.00895 0.03312 -0.00855 AFIX 137 H59A 2 0.127612 0.107181 0.838133 11.00000 -1.50000 H59B 2 0.033115 0.130404 0.780501 11.00000 -1.50000 H59C 2 0.043640 0.054541 0.806495 11.00000 -1.50000 AFIX 0 C60 1 0.078474 0.346621 0.999422 11.00000 0.05906 0.02914 = 0.03994 -0.00961 0.03684 -0.01044 AFIX 137 H60A 2 0.026862 0.371551 0.966761 11.00000 -1.50000 H60B 2 0.135233 0.365944 1.007990 11.00000 -1.50000 H60C 2 0.077304 0.351587 1.033277 11.00000 -1.50000 AFIX 0 MOLE 3 PART -1 C61A 1 0.227827 0.564034 0.401790 10.50000 21.00000 AFIX 33 H61A 2 0.272946 0.543035 0.439327 10.50000 -1.50000 H61B 2 0.256483 0.575710 0.382260 10.50000 -1.50000 H61C 2 0.178203 0.531137 0.378141 10.50000 -1.50000 AFIX 0 C62A 1 0.191885 0.626869 0.410190 10.50000 21.00000 AFIX 23 H62A 2 0.141767 0.646007 0.372532 10.50000 -1.20000 H62B 2 0.240083 0.662428 0.430580 10.50000 -1.20000 AFIX 0 C63A 1 0.156811 0.606300 0.446646 10.50000 21.00000 AFIX 23 H63A 2 0.116299 0.565673 0.428230 10.50000 -1.20000 H63B 2 0.209428 0.591443 0.485174 10.50000 -1.20000 AFIX 0 C64A 1 0.107255 0.660403 0.454710 10.50000 21.00000 AFIX 23 H64A 2 0.144898 0.702925 0.468570 10.50000 -1.20000 H64B 2 0.101651 0.644911 0.485705 10.50000 -1.20000 AFIX 0 C65A 1 0.015650 0.679132 0.403985 10.50000 21.00000 AFIX 23 H65A 2 -0.004352 0.721135 0.413741 10.50000 -1.20000 H65B 2 0.020511 0.691661 0.372112 10.50000 -1.20000 AFIX 0 C66A 1 -0.054964 0.626658 0.382745 10.50000 21.00000 AFIX 33 H66A 2 -0.046042 0.590593 0.362201 10.50000 -1.50000 H66B 2 -0.114614 0.648216 0.356415 10.50000 -1.50000 H66C 2 -0.051715 0.605882 0.415338 10.50000 -1.50000 AFIX 0 PART -2 C61B 1 0.252545 0.552647 0.399477 10.25000 31.00000 AFIX 33 H61D 2 0.269783 0.503585 0.405110 10.25000 -1.50000 H61E 2 0.307015 0.581446 0.416334 10.25000 -1.50000 H61F 2 0.210885 0.562467 0.358125 10.25000 -1.50000 AFIX 0 C62B 1 0.210790 0.567159 0.425686 10.25000 31.00000 AFIX 23 H62C 2 0.252000 0.556054 0.467291 10.25000 -1.20000 H62D 2 0.155429 0.538451 0.408580 10.25000 -1.20000 AFIX 0 C63B 1 0.185931 0.642467 0.418013 10.25000 31.00000 AFIX 23 H63C 2 0.239618 0.670348 0.446766 10.25000 -1.20000 H63D 2 0.165613 0.657824 0.379038 10.25000 -1.20000 AFIX 0 C64B 1 0.114828 0.652739 0.425235 10.25000 31.00000 AFIX 23 H64C 2 0.138139 0.636394 0.464517 10.25000 -1.20000 H64D 2 0.106089 0.703449 0.424927 10.25000 -1.20000 AFIX 0 C65B 1 0.030354 0.624237 0.388662 10.25000 31.00000 AFIX 23 H65C 2 0.033836 0.585477 0.367197 10.25000 -1.20000 H65D 2 -0.011416 0.659592 0.360305 10.25000 -1.20000 AFIX 0 C66B 1 -0.008243 0.596851 0.422150 10.25000 31.00000 AFIX 33 H66D 2 -0.006305 0.546065 0.423102 10.25000 -1.50000 H66E 2 -0.071170 0.612432 0.402691 10.25000 -1.50000 H66F 2 0.028541 0.614879 0.461659 10.25000 -1.50000 AFIX 0 PART -3 C61C 1 0.169861 0.625693 0.407687 10.25000 41.00000 AFIX 33 H61G 2 0.183592 0.577469 0.404547 10.25000 -1.50000 H61H 2 0.217445 0.643784 0.445914 10.25000 -1.50000 H61I 2 0.167220 0.653703 0.378001 10.25000 -1.50000 AFIX 0 C62C 1 0.077703 0.629031 0.399203 10.25000 41.00000 AFIX 23 H62E 2 0.056686 0.677606 0.394286 10.25000 -1.20000 H62F 2 0.031311 0.602032 0.364842 10.25000 -1.20000 AFIX 0 C63C 1 0.094456 0.598041 0.453256 10.25000 41.00000 AFIX 23 H63E 2 0.134415 0.557085 0.464503 10.25000 -1.20000 H63F 2 0.126793 0.632424 0.484834 10.25000 -1.20000 AFIX 0 C64C 1 0.009868 0.576703 0.446623 10.25000 41.00000 AFIX 23 H64E 2 -0.028416 0.618653 0.435565 10.25000 -1.20000 H64F 2 -0.022680 0.544643 0.413325 10.25000 -1.20000 AFIX 0 C65C 1 0.011959 0.549572 0.485446 10.25000 41.00000 AFIX 23 H65E 2 -0.030051 0.579478 0.488075 10.25000 -1.20000 H65F 2 0.073196 0.562924 0.519104 10.25000 -1.20000 AFIX 0 C66C 1 -0.000176 0.484648 0.503760 10.25000 41.00000 AFIX 33 H66G 2 -0.037607 0.490988 0.518151 10.25000 -1.50000 H66H 2 0.059128 0.465854 0.534607 10.25000 -1.50000 H66I 2 -0.030417 0.452332 0.471149 10.25000 -1.50000 HKLF 4 1 1 0 0 0 1 0 0 0 1 1.3 REM w13_a37sadm in P2(1)/n REM R1 = 0.0526 for 10391 Fo > 4sig(Fo) and 0.0793 for all 14355 data REM 892 parameters refined using 27 restraints END WGHT 0.0625 2.4104 REM Highest difference peak 1.275, deepest hole -0.762, 1-sigma level 0.077 Q1 1 0.0178 0.5735 0.4744 11.00000 0.05 1.28 Q2 1 0.0923 0.2098 1.0141 11.00000 0.05 1.25 Q3 1 -0.0415 0.2909 0.9472 11.00000 0.05 0.97 Q4 1 -0.0567 0.5750 0.4145 11.00000 0.05 0.88 Q5 1 -0.0215 0.6418 0.3991 11.00000 0.05 0.69 Q6 1 0.3390 0.6299 0.6893 11.00000 0.05 0.66 Q7 1 0.2673 0.4956 0.7027 11.00000 0.05 0.58 Q8 1 0.6011 0.6182 0.6070 11.00000 0.05 0.56 Q9 1 0.4414 0.5770 0.5512 11.00000 0.05 0.56 Q10 1 0.6586 0.3707 0.8037 11.00000 0.05 0.51 Q11 1 0.0530 0.6006 0.4509 11.00000 0.05 0.51 Q12 1 0.1893 0.6386 0.4517 11.00000 0.05 0.50 Q13 1 -0.0916 0.2051 0.8960 11.00000 0.05 0.47 Q14 1 0.2651 0.5364 0.6238 11.00000 0.05 0.47 Q15 1 0.2688 0.5319 0.6712 11.00000 0.05 0.46 Q16 1 0.1297 0.0746 0.9038 11.00000 0.05 0.44 Q17 1 0.5016 0.7326 0.6132 11.00000 0.05 0.43 Q18 1 0.7423 0.3306 0.7592 11.00000 0.05 0.42 Q19 1 0.1404 0.3331 1.0259 11.00000 0.05 0.38 Q20 1 -0.0321 0.0978 0.8486 11.00000 0.05 0.38 Q21 1 0.1489 0.5809 0.8783 11.00000 0.05 0.36 Q22 1 0.6468 0.5302 0.6104 11.00000 0.05 0.35 Q23 1 0.0375 0.4881 0.4991 11.00000 0.05 0.35 Q24 1 0.1237 0.2860 0.8751 11.00000 0.05 0.34 Q25 1 0.4771 0.6860 0.5898 11.00000 0.05 0.34 ; _database_code_depnum_ccdc_archive 'CCDC 961424' ####################################################################### # # 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_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H50 N8 Sc2' _chemical_formula_sum 'C22 H50 N8 Sc2' _chemical_formula_weight 516.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _symmetry_space_group_name_Hall '-P 2ybc' 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 14.1746(9) _cell_length_b 11.2268(7) _cell_length_c 17.1826(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.8428(10) _cell_angle_gamma 90.00 _cell_volume 2734.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5912 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.08 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8387 _exptl_absorpt_correction_T_max 0.9121 _exptl_absorpt_process_details 'Mulabs Platon' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37144 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 28.43 _reflns_number_total 6838 _reflns_number_gt 5477 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Altomare 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1999)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^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 6838 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc1 Sc 0.33913(2) -0.19448(3) 0.67188(2) 0.01367(10) Uani 1 1 d . . . Sc2 Sc 0.19718(2) 0.04576(3) 0.66027(2) 0.01327(10) Uani 1 1 d . . . H1 H 0.2134(15) -0.1241(19) 0.6960(13) 0.027(6) Uiso 1 1 d . . . N1 N 0.32462(11) -0.02611(14) 0.59874(9) 0.0160(3) Uani 1 1 d . . . N2 N 0.24291(11) -0.27070(15) 0.56987(10) 0.0204(4) Uani 1 1 d . . . N3 N 0.42841(11) -0.30208(14) 0.60804(10) 0.0192(4) Uani 1 1 d . . . N4 N 0.48634(11) -0.10785(14) 0.68833(10) 0.0179(3) Uani 1 1 d . . . N5 N 0.05806(11) 0.04874(15) 0.62090(10) 0.0220(4) Uani 1 1 d . . . N6 N 0.10673(11) 0.01990(15) 0.77677(10) 0.0206(4) Uani 1 1 d . . . N7 N 0.22979(11) 0.19650(14) 0.72622(10) 0.0192(4) Uani 1 1 d . . . N8 N 0.18765(11) 0.20566(14) 0.56395(10) 0.0185(4) Uani 1 1 d . . . C1 C 0.34115(14) -0.26658(18) 0.79483(12) 0.0204(4) Uani 1 1 d . . . H1A H 0.4045 -0.2965 0.8100 0.025 Uiso 1 1 calc R . . H1B H 0.3211 -0.2055 0.8327 0.025 Uiso 1 1 calc R . . C2 C 0.26929(15) -0.36810(19) 0.78836(13) 0.0269(5) Uani 1 1 d . . . H2A H 0.2054 -0.3348 0.7851 0.040 Uiso 1 1 calc R . . H2B H 0.2749 -0.4194 0.8343 0.040 Uiso 1 1 calc R . . H2C H 0.2816 -0.4150 0.7415 0.040 Uiso 1 1 calc R . . C3 C 0.32106(14) -0.08062(18) 0.52077(12) 0.0199(4) Uani 1 1 d . . . H3A H 0.3814 -0.1221 0.5110 0.024 Uiso 1 1 calc R . . H3B H 0.3132 -0.0174 0.4810 0.024 Uiso 1 1 calc R . . C4 C 0.23967(14) -0.16930(19) 0.51318(12) 0.0230(4) Uani 1 1 d . . . H4A H 0.1796 -0.1257 0.5199 0.028 Uiso 1 1 calc R . . H4B H 0.2393 -0.2024 0.4598 0.028 Uiso 1 1 calc R . . C5 C 0.29283(15) -0.3773(2) 0.53931(14) 0.0283(5) Uani 1 1 d . . . H5A H 0.2689 -0.3947 0.4861 0.034 Uiso 1 1 calc R . . H5B H 0.2783 -0.4468 0.5725 0.034 Uiso 1 1 calc R . . C6 C 0.39842(15) -0.36101(19) 0.53697(13) 0.0263(5) Uani 1 1 d . . . H6A H 0.4299 -0.4394 0.5326 0.032 Uiso 1 1 calc R . . H6B H 0.4155 -0.3122 0.4913 0.032 Uiso 1 1 calc R . . C7 C 0.52892(14) -0.28635(19) 0.61257(13) 0.0231(4) Uani 1 1 d . . . H7A H 0.5514 -0.2481 0.5644 0.028 Uiso 1 1 calc R . . H7B H 0.5603 -0.3648 0.6178 0.028 Uiso 1 1 calc R . . C8 C 0.55363(13) -0.20869(18) 0.68260(13) 0.0231(5) Uani 1 1 d . . . H8A H 0.5514 -0.2571 0.7307 0.028 Uiso 1 1 calc R . . H8B H 0.6186 -0.1775 0.6774 0.028 Uiso 1 1 calc R . . C9 C 0.49894(13) -0.02446(18) 0.62245(12) 0.0200(4) Uani 1 1 d . . . H9A H 0.5138 -0.0701 0.5749 0.024 Uiso 1 1 calc R . . H9B H 0.5526 0.0295 0.6340 0.024 Uiso 1 1 calc R . . C10 C 0.41016(13) 0.04865(17) 0.60838(12) 0.0186(4) Uani 1 1 d . . . H10A H 0.4014 0.1035 0.6528 0.022 Uiso 1 1 calc R . . H10B H 0.4182 0.0976 0.5610 0.022 Uiso 1 1 calc R . . C11 C 0.14477(14) -0.3059(2) 0.58752(14) 0.0285(5) Uani 1 1 d . . . H11A H 0.1103 -0.2367 0.6071 0.043 Uiso 1 1 calc R . . H11B H 0.1455 -0.3688 0.6271 0.043 Uiso 1 1 calc R . . H11C H 0.1136 -0.3355 0.5401 0.043 Uiso 1 1 calc R . . C12 C 0.49853(16) -0.04607(19) 0.76352(13) 0.0262(5) Uani 1 1 d . . . H12A H 0.4902 -0.1030 0.8061 0.039 Uiso 1 1 calc R . . H12B H 0.4515 0.0175 0.7675 0.039 Uiso 1 1 calc R . . H12C H 0.5620 -0.0117 0.7669 0.039 Uiso 1 1 calc R . . C13 C -0.01697(15) 0.0224(2) 0.67398(14) 0.0353(6) Uani 1 1 d . . . H13A H -0.0624 -0.0326 0.6485 0.042 Uiso 1 1 calc R . . H13B H -0.0509 0.0969 0.6865 0.042 Uiso 1 1 calc R . . C14 C 0.01898(17) -0.0324(2) 0.74707(15) 0.0401(6) Uani 1 1 d . . . H14A H -0.0298 -0.0246 0.7874 0.048 Uiso 1 1 calc R . . H14B H 0.0293 -0.1184 0.7380 0.048 Uiso 1 1 calc R . . C15 C 0.09455(16) 0.1447(2) 0.80384(14) 0.0328(5) Uani 1 1 d . . . H15A H 0.0702 0.1448 0.8576 0.039 Uiso 1 1 calc R . . H15B H 0.0481 0.1861 0.7698 0.039 Uiso 1 1 calc R . . C16 C 0.18700(16) 0.2086(2) 0.80196(13) 0.0277(5) Uani 1 1 d . . . H16A H 0.1771 0.2940 0.8136 0.033 Uiso 1 1 calc R . . H16B H 0.2299 0.1753 0.8424 0.033 Uiso 1 1 calc R . . C17 C 0.23544(15) 0.30911(18) 0.68408(13) 0.0241(5) Uani 1 1 d . . . H17A H 0.3004 0.3210 0.6652 0.029 Uiso 1 1 calc R . . H17B H 0.2201 0.3758 0.7194 0.029 Uiso 1 1 calc R . . C18 C 0.16643(14) 0.30809(17) 0.61527(13) 0.0224(4) Uani 1 1 d . . . H18A H 0.1010 0.3016 0.6343 0.027 Uiso 1 1 calc R . . H18B H 0.1719 0.3834 0.5857 0.027 Uiso 1 1 calc R . . C19 C 0.10636(15) 0.17260(19) 0.51328(12) 0.0266(5) Uani 1 1 d . . . H19A H 0.1260 0.1098 0.4765 0.032 Uiso 1 1 calc R . . H19B H 0.0862 0.2429 0.4825 0.032 Uiso 1 1 calc R . . C20 C 0.02422(14) 0.1280(2) 0.56003(13) 0.0277(5) Uani 1 1 d . . . H20A H -0.0093 0.1963 0.5834 0.033 Uiso 1 1 calc R . . H20B H -0.0208 0.0851 0.5255 0.033 Uiso 1 1 calc R . . C21 C 0.1443(2) -0.0529(3) 0.83947(15) 0.0495(8) Uani 1 1 d . . . H21A H 0.0998 -0.0537 0.8826 0.074 Uiso 1 1 calc R . . H21B H 0.2047 -0.0200 0.8576 0.074 Uiso 1 1 calc R . . H21C H 0.1537 -0.1344 0.8207 0.074 Uiso 1 1 calc R . . C22 C 0.26700(15) 0.2385(2) 0.51409(13) 0.0279(5) Uani 1 1 d . . . H22A H 0.2825 0.1713 0.4802 0.042 Uiso 1 1 calc R . . H22B H 0.3220 0.2585 0.5467 0.042 Uiso 1 1 calc R . . H22C H 0.2494 0.3075 0.4822 0.042 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 Sc1 0.01037(17) 0.01368(18) 0.01701(19) -0.00045(14) 0.00229(13) 0.00047(13) Sc2 0.01027(17) 0.01574(18) 0.01382(19) -0.00058(14) 0.00086(13) 0.00138(13) N1 0.0138(8) 0.0180(8) 0.0162(8) -0.0003(6) 0.0026(6) -0.0006(6) N2 0.0147(8) 0.0220(9) 0.0247(9) -0.0026(7) 0.0013(7) -0.0036(7) N3 0.0140(8) 0.0191(8) 0.0248(9) -0.0029(7) 0.0032(7) 0.0018(6) N4 0.0156(8) 0.0186(8) 0.0196(9) 0.0008(7) -0.0015(6) -0.0019(6) N5 0.0129(8) 0.0303(10) 0.0225(9) 0.0003(7) -0.0024(7) -0.0006(7) N6 0.0198(8) 0.0219(9) 0.0201(9) -0.0001(7) 0.0038(7) 0.0027(7) N7 0.0186(8) 0.0208(9) 0.0182(9) -0.0026(7) 0.0000(7) -0.0012(7) N8 0.0185(8) 0.0186(8) 0.0183(9) 0.0016(7) -0.0008(7) 0.0014(6) C1 0.0186(10) 0.0197(10) 0.0231(11) 0.0018(8) 0.0024(8) 0.0027(8) C2 0.0234(11) 0.0271(11) 0.0303(12) 0.0037(9) 0.0025(9) -0.0002(9) C3 0.0181(9) 0.0233(10) 0.0183(10) -0.0011(8) 0.0039(8) 0.0001(8) C4 0.0190(10) 0.0309(11) 0.0192(10) -0.0032(9) -0.0008(8) -0.0010(8) C5 0.0269(11) 0.0245(11) 0.0333(13) -0.0121(10) -0.0023(9) -0.0019(9) C6 0.0255(11) 0.0231(11) 0.0306(12) -0.0099(9) 0.0061(9) 0.0041(9) C7 0.0154(9) 0.0240(10) 0.0300(12) 0.0032(9) 0.0066(8) 0.0041(8) C8 0.0111(9) 0.0262(11) 0.0321(12) 0.0046(9) -0.0008(8) 0.0011(8) C9 0.0138(9) 0.0214(10) 0.0248(11) 0.0015(8) 0.0018(8) -0.0041(7) C10 0.0161(9) 0.0186(10) 0.0213(10) 0.0014(8) 0.0016(8) -0.0019(7) C11 0.0186(10) 0.0334(12) 0.0335(13) -0.0005(10) -0.0010(9) -0.0093(9) C12 0.0281(11) 0.0250(11) 0.0251(12) -0.0007(9) -0.0062(9) -0.0063(9) C13 0.0137(10) 0.0568(16) 0.0356(14) -0.0045(12) 0.0017(9) -0.0102(10) C14 0.0272(13) 0.0516(16) 0.0421(15) -0.0005(12) 0.0141(11) -0.0121(11) C15 0.0330(12) 0.0340(13) 0.0315(13) -0.0073(10) 0.0093(10) 0.0023(10) C16 0.0343(12) 0.0273(11) 0.0216(11) -0.0076(9) 0.0029(9) -0.0022(9) C17 0.0250(11) 0.0202(10) 0.0271(11) -0.0026(9) -0.0009(9) -0.0062(8) C18 0.0215(10) 0.0150(9) 0.0308(12) 0.0020(8) 0.0009(9) 0.0007(8) C19 0.0327(12) 0.0256(11) 0.0211(11) 0.0028(9) -0.0113(9) 0.0025(9) C20 0.0197(10) 0.0276(11) 0.0353(13) -0.0039(10) -0.0123(9) 0.0022(9) C21 0.0571(18) 0.0595(18) 0.0326(14) 0.0217(13) 0.0196(13) 0.0268(14) C22 0.0286(11) 0.0305(12) 0.0246(11) 0.0112(10) 0.0067(9) 0.0049(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 N3 2.0748(16) . ? Sc1 C1 2.262(2) . ? Sc1 N1 2.2775(16) . ? Sc1 N4 2.3156(16) . ? Sc1 N2 2.3652(17) . ? Sc1 Sc2 3.3691(5) . ? Sc1 H1 2.00(2) . ? Sc2 N5 2.0755(16) . ? Sc2 N7 2.0848(16) . ? Sc2 N1 2.2557(16) . ? Sc2 N6 2.4105(17) . ? Sc2 N8 2.4440(16) . ? Sc2 H1 2.02(2) . ? N1 C3 1.473(2) . ? N1 C10 1.482(2) . ? N2 C11 1.482(3) . ? N2 C5 1.490(3) . ? N2 C4 1.498(3) . ? N3 C7 1.437(2) . ? N3 C6 1.447(3) . ? N4 C12 1.474(3) . ? N4 C9 1.482(2) . ? N4 C8 1.485(2) . ? N5 C13 1.442(3) . ? N5 C20 1.449(3) . ? N6 C21 1.448(3) . ? N6 C14 1.461(3) . ? N6 C15 1.487(3) . ? N7 C16 1.450(3) . ? N7 C17 1.460(3) . ? N8 C22 1.471(3) . ? N8 C19 1.481(2) . ? N8 C18 1.483(3) . ? C1 C2 1.532(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.528(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.509(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.523(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.519(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.482(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.495(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.523(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.510(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 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 N3 Sc1 C1 106.61(7) . . ? N3 Sc1 N1 104.03(6) . . ? C1 Sc1 N1 144.30(7) . . ? N3 Sc1 N4 75.73(6) . . ? C1 Sc1 N4 92.14(6) . . ? N1 Sc1 N4 78.03(6) . . ? N3 Sc1 N2 75.36(6) . . ? C1 Sc1 N2 124.18(7) . . ? N1 Sc1 N2 81.08(6) . . ? N4 Sc1 N2 138.69(6) . . ? N3 Sc1 Sc2 143.44(5) . . ? C1 Sc1 Sc2 109.94(5) . . ? N1 Sc1 Sc2 41.75(4) . . ? N4 Sc1 Sc2 101.96(4) . . ? N2 Sc1 Sc2 84.74(4) . . ? N3 Sc1 H1 153.2(6) . . ? C1 Sc1 H1 86.9(6) . . ? N1 Sc1 H1 73.3(6) . . ? N4 Sc1 H1 127.8(6) . . ? N2 Sc1 H1 77.9(6) . . ? Sc2 Sc1 H1 33.1(6) . . ? N5 Sc2 N7 111.47(7) . . ? N5 Sc2 N1 128.07(7) . . ? N7 Sc2 N1 111.86(6) . . ? N5 Sc2 N6 76.01(6) . . ? N7 Sc2 N6 76.27(6) . . ? N1 Sc2 N6 141.77(6) . . ? N5 Sc2 N8 74.02(6) . . ? N7 Sc2 N8 77.38(6) . . ? N1 Sc2 N8 88.97(6) . . ? N6 Sc2 N8 128.76(6) . . ? N5 Sc2 Sc1 126.58(5) . . ? N7 Sc2 Sc1 119.35(5) . . ? N1 Sc2 Sc1 42.24(4) . . ? N6 Sc2 Sc1 100.30(4) . . ? N8 Sc2 Sc1 130.93(4) . . ? N5 Sc2 H1 102.6(6) . . ? N7 Sc2 H1 125.4(6) . . ? N1 Sc2 H1 73.5(6) . . ? N6 Sc2 H1 72.1(6) . . ? N8 Sc2 H1 155.0(6) . . ? Sc1 Sc2 H1 32.8(6) . . ? C3 N1 C10 110.73(15) . . ? C3 N1 Sc2 123.91(12) . . ? C10 N1 Sc2 113.87(11) . . ? C3 N1 Sc1 99.13(11) . . ? C10 N1 Sc1 109.96(11) . . ? Sc2 N1 Sc1 96.01(6) . . ? C11 N2 C5 108.06(16) . . ? C11 N2 C4 108.41(16) . . ? C5 N2 C4 113.03(17) . . ? C11 N2 Sc1 118.53(13) . . ? C5 N2 Sc1 106.27(12) . . ? C4 N2 Sc1 102.63(11) . . ? C7 N3 C6 112.37(16) . . ? C7 N3 Sc1 120.79(13) . . ? C6 N3 Sc1 122.57(12) . . ? C12 N4 C9 110.99(16) . . ? C12 N4 C8 110.47(16) . . ? C9 N4 C8 110.26(15) . . ? C12 N4 Sc1 113.48(12) . . ? C9 N4 Sc1 106.90(11) . . ? C8 N4 Sc1 104.50(11) . . ? C13 N5 C20 110.06(17) . . ? C13 N5 Sc2 119.78(14) . . ? C20 N5 Sc2 123.22(13) . . ? C21 N6 C14 109.6(2) . . ? C21 N6 C15 110.02(19) . . ? C14 N6 C15 112.68(18) . . ? C21 N6 Sc2 119.47(14) . . ? C14 N6 Sc2 102.65(13) . . ? C15 N6 Sc2 102.24(12) . . ? C16 N7 C17 113.02(16) . . ? C16 N7 Sc2 118.12(13) . . ? C17 N7 Sc2 116.53(12) . . ? C22 N8 C19 108.38(16) . . ? C22 N8 C18 108.41(16) . . ? C19 N8 C18 112.40(16) . . ? C22 N8 Sc2 122.90(12) . . ? C19 N8 Sc2 104.41(12) . . ? C18 N8 Sc2 100.17(11) . . ? C2 C1 Sc1 101.49(13) . . ? C2 C1 H1A 111.5 . . ? Sc1 C1 H1A 111.5 . . ? C2 C1 H1B 111.5 . . ? Sc1 C1 H1B 111.5 . . ? H1A C1 H1B 109.3 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 111.35(16) . . ? N1 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N2 C4 C3 115.06(16) . . ? N2 C4 H4A 108.5 . . ? C3 C4 H4A 108.5 . . ? N2 C4 H4B 108.5 . . ? C3 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? N2 C5 C6 112.86(17) . . ? N2 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? N2 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N3 C6 C5 108.19(17) . . ? N3 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? N3 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? N3 C7 C8 109.25(16) . . ? N3 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? N3 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? N4 C8 C7 110.40(16) . . ? N4 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? N4 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? N4 C9 C10 110.74(16) . . ? N4 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N4 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N1 C10 C9 112.73(16) . . ? N1 C10 H10A 109.0 . . ? C9 C10 H10A 109.0 . . ? N1 C10 H10B 109.0 . . ? C9 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 H12A 109.5 . . ? N4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 C14 111.93(18) . . ? N5 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? N5 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N6 C14 C13 114.2(2) . . ? N6 C14 H14A 108.7 . . ? C13 C14 H14A 108.7 . . ? N6 C14 H14B 108.7 . . ? C13 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? N6 C15 C16 109.84(18) . . ? N6 C15 H15A 109.7 . . ? C16 C15 H15A 109.7 . . ? N6 C15 H15B 109.7 . . ? C16 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N7 C16 C15 110.67(17) . . ? N7 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? N7 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N7 C17 C18 109.83(16) . . ? N7 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? N7 C17 H17B 109.7 . . ? C18 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? N8 C18 C17 109.51(16) . . ? N8 C18 H18A 109.8 . . ? C17 C18 H18A 109.8 . . ? N8 C18 H18B 109.8 . . ? C17 C18 H18B 109.8 . . ? H18A C18 H18B 108.2 . . ? N8 C19 C20 111.70(17) . . ? N8 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? N8 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? N5 C20 C19 109.75(16) . . ? N5 C20 H20A 109.7 . . ? C19 C20 H20A 109.7 . . ? N5 C20 H20B 109.7 . . ? C19 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? N6 C21 H21A 109.5 . . ? N6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N8 C22 H22A 109.5 . . ? N8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 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 N3 Sc1 Sc2 N5 83.09(10) . . . . ? C1 Sc1 Sc2 N5 -98.05(8) . . . . ? N1 Sc1 Sc2 N5 108.97(9) . . . . ? N4 Sc1 Sc2 N5 165.20(7) . . . . ? N2 Sc1 Sc2 N5 26.47(8) . . . . ? N3 Sc1 Sc2 N7 -116.81(10) . . . . ? C1 Sc1 Sc2 N7 62.05(8) . . . . ? N1 Sc1 Sc2 N7 -90.93(8) . . . . ? N4 Sc1 Sc2 N7 -34.69(7) . . . . ? N2 Sc1 Sc2 N7 -173.42(7) . . . . ? N3 Sc1 Sc2 N1 -25.88(10) . . . . ? C1 Sc1 Sc2 N1 152.98(8) . . . . ? N4 Sc1 Sc2 N1 56.24(7) . . . . ? N2 Sc1 Sc2 N1 -82.49(7) . . . . ? N3 Sc1 Sc2 N6 163.24(9) . . . . ? C1 Sc1 Sc2 N6 -17.91(7) . . . . ? N1 Sc1 Sc2 N6 -170.89(7) . . . . ? N4 Sc1 Sc2 N6 -114.65(6) . . . . ? N2 Sc1 Sc2 N6 106.62(6) . . . . ? N3 Sc1 Sc2 N8 -17.85(10) . . . . ? C1 Sc1 Sc2 N8 161.01(7) . . . . ? N1 Sc1 Sc2 N8 8.03(8) . . . . ? N4 Sc1 Sc2 N8 64.27(7) . . . . ? N2 Sc1 Sc2 N8 -74.46(7) . . . . ? N5 Sc2 N1 C3 -0.03(18) . . . . ? N7 Sc2 N1 C3 -144.65(14) . . . . ? N6 Sc2 N1 C3 119.83(15) . . . . ? N8 Sc2 N1 C3 -68.70(15) . . . . ? Sc1 Sc2 N1 C3 105.24(15) . . . . ? N5 Sc2 N1 C10 139.77(12) . . . . ? N7 Sc2 N1 C10 -4.85(14) . . . . ? N6 Sc2 N1 C10 -100.37(14) . . . . ? N8 Sc2 N1 C10 71.10(13) . . . . ? Sc1 Sc2 N1 C10 -114.96(14) . . . . ? N5 Sc2 N1 Sc1 -105.28(8) . . . . ? N7 Sc2 N1 Sc1 110.11(7) . . . . ? N6 Sc2 N1 Sc1 14.59(12) . . . . ? N8 Sc2 N1 Sc1 -173.94(6) . . . . ? N3 Sc1 N1 C3 38.65(12) . . . . ? C1 Sc1 N1 C3 -172.85(12) . . . . ? N4 Sc1 N1 C3 110.43(11) . . . . ? N2 Sc1 N1 C3 -33.72(11) . . . . ? Sc2 Sc1 N1 C3 -125.81(12) . . . . ? N3 Sc1 N1 C10 -77.44(13) . . . . ? C1 Sc1 N1 C10 71.07(16) . . . . ? N4 Sc1 N1 C10 -5.66(12) . . . . ? N2 Sc1 N1 C10 -149.80(13) . . . . ? Sc2 Sc1 N1 C10 118.10(14) . . . . ? N3 Sc1 N1 Sc2 164.45(6) . . . . ? C1 Sc1 N1 Sc2 -47.04(12) . . . . ? N4 Sc1 N1 Sc2 -123.76(7) . . . . ? N2 Sc1 N1 Sc2 92.09(6) . . . . ? N3 Sc1 N2 C11 140.45(15) . . . . ? C1 Sc1 N2 C11 40.10(17) . . . . ? N1 Sc1 N2 C11 -112.41(15) . . . . ? N4 Sc1 N2 C11 -172.64(13) . . . . ? Sc2 Sc1 N2 C11 -70.48(14) . . . . ? N3 Sc1 N2 C5 18.69(13) . . . . ? C1 Sc1 N2 C5 -81.66(15) . . . . ? N1 Sc1 N2 C5 125.83(14) . . . . ? N4 Sc1 N2 C5 65.60(16) . . . . ? Sc2 Sc1 N2 C5 167.76(13) . . . . ? N3 Sc1 N2 C4 -100.19(12) . . . . ? C1 Sc1 N2 C4 159.45(11) . . . . ? N1 Sc1 N2 C4 6.94(11) . . . . ? N4 Sc1 N2 C4 -53.29(15) . . . . ? Sc2 Sc1 N2 C4 48.87(11) . . . . ? C1 Sc1 N3 C7 -79.37(16) . . . . ? N1 Sc1 N3 C7 82.08(16) . . . . ? N4 Sc1 N3 C7 8.58(14) . . . . ? N2 Sc1 N3 C7 158.76(16) . . . . ? Sc2 Sc1 N3 C7 99.51(15) . . . . ? C1 Sc1 N3 C6 125.60(16) . . . . ? N1 Sc1 N3 C6 -72.95(16) . . . . ? N4 Sc1 N3 C6 -146.45(16) . . . . ? N2 Sc1 N3 C6 3.73(15) . . . . ? Sc2 Sc1 N3 C6 -55.52(19) . . . . ? N3 Sc1 N4 C12 -150.13(14) . . . . ? C1 Sc1 N4 C12 -43.52(14) . . . . ? N1 Sc1 N4 C12 101.84(13) . . . . ? N2 Sc1 N4 C12 163.08(12) . . . . ? Sc2 Sc1 N4 C12 67.38(13) . . . . ? N3 Sc1 N4 C9 87.18(13) . . . . ? C1 Sc1 N4 C9 -166.22(13) . . . . ? N1 Sc1 N4 C9 -20.85(12) . . . . ? N2 Sc1 N4 C9 40.38(16) . . . . ? Sc2 Sc1 N4 C9 -55.32(12) . . . . ? N3 Sc1 N4 C8 -29.72(12) . . . . ? C1 Sc1 N4 C8 76.88(13) . . . . ? N1 Sc1 N4 C8 -137.75(13) . . . . ? N2 Sc1 N4 C8 -76.52(15) . . . . ? Sc2 Sc1 N4 C8 -172.21(11) . . . . ? N7 Sc2 N5 C13 -75.71(18) . . . . ? N1 Sc2 N5 C13 139.56(16) . . . . ? N6 Sc2 N5 C13 -6.86(17) . . . . ? N8 Sc2 N5 C13 -144.80(18) . . . . ? Sc1 Sc2 N5 C13 85.70(17) . . . . ? N7 Sc2 N5 C20 72.19(17) . . . . ? N1 Sc2 N5 C20 -72.53(18) . . . . ? N6 Sc2 N5 C20 141.05(17) . . . . ? N8 Sc2 N5 C20 3.10(15) . . . . ? Sc1 Sc2 N5 C20 -126.39(15) . . . . ? N5 Sc2 N6 C21 146.89(19) . . . . ? N7 Sc2 N6 C21 -96.42(19) . . . . ? N1 Sc2 N6 C21 11.6(2) . . . . ? N8 Sc2 N6 C21 -157.43(17) . . . . ? Sc1 Sc2 N6 C21 21.52(19) . . . . ? N5 Sc2 N6 C14 25.50(14) . . . . ? N7 Sc2 N6 C14 142.19(15) . . . . ? N1 Sc2 N6 C14 -109.78(15) . . . . ? N8 Sc2 N6 C14 81.17(15) . . . . ? Sc1 Sc2 N6 C14 -99.88(14) . . . . ? N5 Sc2 N6 C15 -91.44(13) . . . . ? N7 Sc2 N6 C15 25.25(13) . . . . ? N1 Sc2 N6 C15 133.28(13) . . . . ? N8 Sc2 N6 C15 -35.77(15) . . . . ? Sc1 Sc2 N6 C15 143.18(12) . . . . ? N5 Sc2 N7 C16 69.35(16) . . . . ? N1 Sc2 N7 C16 -139.98(14) . . . . ? N6 Sc2 N7 C16 0.66(14) . . . . ? N8 Sc2 N7 C16 136.31(15) . . . . ? Sc1 Sc2 N7 C16 -93.57(15) . . . . ? N5 Sc2 N7 C17 -70.32(15) . . . . ? N1 Sc2 N7 C17 80.35(14) . . . . ? N6 Sc2 N7 C17 -139.00(15) . . . . ? N8 Sc2 N7 C17 -3.35(13) . . . . ? Sc1 Sc2 N7 C17 126.76(13) . . . . ? N5 Sc2 N8 C22 -148.30(17) . . . . ? N7 Sc2 N8 C22 94.68(16) . . . . ? N1 Sc2 N8 C22 -18.01(16) . . . . ? N6 Sc2 N8 C22 155.23(14) . . . . ? Sc1 Sc2 N8 C22 -23.40(17) . . . . ? N5 Sc2 N8 C19 -24.67(13) . . . . ? N7 Sc2 N8 C19 -141.69(13) . . . . ? N1 Sc2 N8 C19 105.62(13) . . . . ? N6 Sc2 N8 C19 -81.13(14) . . . . ? Sc1 Sc2 N8 C19 100.23(12) . . . . ? N5 Sc2 N8 C18 91.81(12) . . . . ? N7 Sc2 N8 C18 -25.21(11) . . . . ? N1 Sc2 N8 C18 -137.90(11) . . . . ? N6 Sc2 N8 C18 35.34(14) . . . . ? Sc1 Sc2 N8 C18 -143.29(10) . . . . ? N3 Sc1 C1 C2 -82.75(13) . . . . ? N1 Sc1 C1 C2 129.18(13) . . . . ? N4 Sc1 C1 C2 -158.50(13) . . . . ? N2 Sc1 C1 C2 0.57(16) . . . . ? Sc2 Sc1 C1 C2 97.96(12) . . . . ? C10 N1 C3 C4 173.33(16) . . . . ? Sc2 N1 C3 C4 -45.8(2) . . . . ? Sc1 N1 C3 C4 57.84(16) . . . . ? C11 N2 C4 C3 148.45(17) . . . . ? C5 N2 C4 C3 -91.8(2) . . . . ? Sc1 N2 C4 C3 22.26(18) . . . . ? N1 C3 C4 N2 -59.3(2) . . . . ? C11 N2 C5 C6 -166.50(19) . . . . ? C4 N2 C5 C6 73.5(2) . . . . ? Sc1 N2 C5 C6 -38.3(2) . . . . ? C7 N3 C6 C5 177.89(17) . . . . ? Sc1 N3 C6 C5 -25.2(2) . . . . ? N2 C5 C6 N3 42.0(3) . . . . ? C6 N3 C7 C8 171.95(17) . . . . ? Sc1 N3 C7 C8 14.6(2) . . . . ? C12 N4 C8 C7 169.25(16) . . . . ? C9 N4 C8 C7 -67.7(2) . . . . ? Sc1 N4 C8 C7 46.85(17) . . . . ? N3 C7 C8 N4 -42.2(2) . . . . ? C12 N4 C9 C10 -79.8(2) . . . . ? C8 N4 C9 C10 157.50(16) . . . . ? Sc1 N4 C9 C10 44.48(18) . . . . ? C3 N1 C10 C9 -76.6(2) . . . . ? Sc2 N1 C10 C9 138.29(14) . . . . ? Sc1 N1 C10 C9 31.89(19) . . . . ? N4 C9 C10 N1 -53.2(2) . . . . ? C20 N5 C13 C14 -165.6(2) . . . . ? Sc2 N5 C13 C14 -13.9(3) . . . . ? C21 N6 C14 C13 -169.8(2) . . . . ? C15 N6 C14 C13 67.4(3) . . . . ? Sc2 N6 C14 C13 -41.9(2) . . . . ? N5 C13 C14 N6 40.1(3) . . . . ? C21 N6 C15 C16 80.8(2) . . . . ? C14 N6 C15 C16 -156.65(19) . . . . ? Sc2 N6 C15 C16 -47.2(2) . . . . ? C17 N7 C16 C15 113.5(2) . . . . ? Sc2 N7 C16 C15 -27.6(2) . . . . ? N6 C15 C16 N7 52.1(2) . . . . ? C16 N7 C17 C18 -109.73(19) . . . . ? Sc2 N7 C17 C18 31.9(2) . . . . ? C22 N8 C18 C17 -80.79(19) . . . . ? C19 N8 C18 C17 159.43(16) . . . . ? Sc2 N8 C18 C17 49.10(16) . . . . ? N7 C17 C18 N8 -57.5(2) . . . . ? C22 N8 C19 C20 175.33(17) . . . . ? C18 N8 C19 C20 -64.9(2) . . . . ? Sc2 N8 C19 C20 42.77(19) . . . . ? C13 N5 C20 C19 169.95(18) . . . . ? Sc2 N5 C20 C19 19.4(2) . . . . ? N8 C19 C20 N5 -42.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.150 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.072 _shelx_res_file ; TITL 5 CELL 0.71073 14.1746 11.2268 17.1826 90.000 90.8428 90.000 ZERR 4.00 0.0009 0.0007 0.0010 0.000 0.0010 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N SC UNIT 88 200 32 8 SIZE 0.18 0.20 0.35 REM colourless block TEMP -173 MERG 2 L.S. 16 FMAP 2 PLAN -10 ACTA CONF BOND $H REM no refinement for extinction WGHT 0.059500 FVAR 0.76537 SC1 4 0.339130 -0.194477 0.671875 11.00000 0.01037 0.01368 = 0.01701 -0.00045 0.00229 0.00047 SC2 4 0.197179 0.045758 0.660267 11.00000 0.01027 0.01574 = 0.01382 -0.00058 0.00086 0.00138 H1 2 0.213405 -0.124117 0.696036 11.00000 0.02697 N1 3 0.324623 -0.026107 0.598742 11.00000 0.01382 0.01798 = 0.01625 -0.00034 0.00261 -0.00057 N2 3 0.242906 -0.270699 0.569870 11.00000 0.01466 0.02198 = 0.02468 -0.00262 0.00132 -0.00365 N3 3 0.428410 -0.302082 0.608043 11.00000 0.01396 0.01905 = 0.02477 -0.00293 0.00324 0.00184 N4 3 0.486335 -0.107851 0.688327 11.00000 0.01556 0.01855 = 0.01958 0.00080 -0.00149 -0.00187 N5 3 0.058062 0.048745 0.620902 11.00000 0.01289 0.03035 = 0.02254 0.00027 -0.00235 -0.00057 N6 3 0.106733 0.019898 0.776766 11.00000 0.01978 0.02193 = 0.02013 -0.00015 0.00376 0.00266 N7 3 0.229792 0.196497 0.726224 11.00000 0.01863 0.02079 = 0.01819 -0.00258 -0.00004 -0.00118 N8 3 0.187649 0.205659 0.563952 11.00000 0.01855 0.01861 = 0.01834 0.00158 -0.00075 0.00144 C1 1 0.341149 -0.266578 0.794825 11.00000 0.01864 0.01967 = 0.02307 0.00183 0.00242 0.00267 AFIX 23 H1A 2 0.404494 -0.296519 0.809977 11.00000 -1.20000 H1B 2 0.321081 -0.205487 0.832692 11.00000 -1.20000 AFIX 0 C2 1 0.269290 -0.368100 0.788357 11.00000 0.02340 0.02714 = 0.03025 0.00373 0.00248 -0.00019 AFIX 137 H2A 2 0.205432 -0.334841 0.785102 11.00000 -1.50000 H2B 2 0.274859 -0.419409 0.834337 11.00000 -1.50000 H2C 2 0.281599 -0.415013 0.741492 11.00000 -1.50000 AFIX 0 C3 1 0.321065 -0.080620 0.520770 11.00000 0.01811 0.02333 = 0.01833 -0.00115 0.00386 0.00010 AFIX 23 H3A 2 0.381366 -0.122133 0.511013 11.00000 -1.20000 H3B 2 0.313245 -0.017404 0.481027 11.00000 -1.20000 AFIX 0 C4 1 0.239668 -0.169305 0.513180 11.00000 0.01902 0.03086 = 0.01922 -0.00318 -0.00081 -0.00105 AFIX 23 H4A 2 0.179622 -0.125730 0.519930 11.00000 -1.20000 H4B 2 0.239282 -0.202382 0.459766 11.00000 -1.20000 AFIX 0 C5 1 0.292829 -0.377304 0.539306 11.00000 0.02689 0.02454 = 0.03329 -0.01207 -0.00233 -0.00192 AFIX 23 H5A 2 0.268897 -0.394687 0.486092 11.00000 -1.20000 H5B 2 0.278290 -0.446790 0.572515 11.00000 -1.20000 AFIX 0 C6 1 0.398421 -0.361008 0.536968 11.00000 0.02546 0.02311 = 0.03057 -0.00993 0.00615 0.00411 AFIX 23 H6A 2 0.429930 -0.439371 0.532594 11.00000 -1.20000 H6B 2 0.415544 -0.312185 0.491323 11.00000 -1.20000 AFIX 0 C7 1 0.528923 -0.286354 0.612571 11.00000 0.01539 0.02401 = 0.02997 0.00316 0.00659 0.00409 AFIX 23 H7A 2 0.551401 -0.248051 0.564372 11.00000 -1.20000 H7B 2 0.560281 -0.364793 0.617849 11.00000 -1.20000 AFIX 0 C8 1 0.553635 -0.208692 0.682597 11.00000 0.01113 0.02619 = 0.03208 0.00457 -0.00079 0.00113 AFIX 23 H8A 2 0.551390 -0.257136 0.730677 11.00000 -1.20000 H8B 2 0.618558 -0.177470 0.677414 11.00000 -1.20000 AFIX 0 C9 1 0.498943 -0.024462 0.622455 11.00000 0.01384 0.02140 = 0.02476 0.00150 0.00175 -0.00405 AFIX 23 H9A 2 0.513802 -0.070058 0.574866 11.00000 -1.20000 H9B 2 0.552595 0.029468 0.634039 11.00000 -1.20000 AFIX 0 C10 1 0.410158 0.048650 0.608379 11.00000 0.01607 0.01864 = 0.02128 0.00137 0.00162 -0.00188 AFIX 23 H10A 2 0.401379 0.103462 0.652822 11.00000 -1.20000 H10B 2 0.418167 0.097638 0.561026 11.00000 -1.20000 AFIX 0 C11 1 0.144773 -0.305897 0.587519 11.00000 0.01862 0.03337 = 0.03352 -0.00047 -0.00105 -0.00932 AFIX 137 H11A 2 0.110287 -0.236700 0.607091 11.00000 -1.50000 H11B 2 0.145531 -0.368770 0.627088 11.00000 -1.50000 H11C 2 0.113594 -0.335501 0.540052 11.00000 -1.50000 AFIX 0 C12 1 0.498535 -0.046065 0.763520 11.00000 0.02812 0.02504 = 0.02513 -0.00073 -0.00623 -0.00633 AFIX 137 H12A 2 0.490205 -0.103014 0.806095 11.00000 -1.50000 H12B 2 0.451507 0.017542 0.767532 11.00000 -1.50000 H12C 2 0.562001 -0.011655 0.766914 11.00000 -1.50000 AFIX 0 C13 1 -0.016971 0.022394 0.673980 11.00000 0.01367 0.05678 = 0.03559 -0.00453 0.00167 -0.01017 AFIX 23 H13A 2 -0.062405 -0.032645 0.648489 11.00000 -1.20000 H13B 2 -0.050947 0.096876 0.686451 11.00000 -1.20000 AFIX 0 C14 1 0.018981 -0.032377 0.747074 11.00000 0.02716 0.05160 = 0.04206 -0.00046 0.01415 -0.01211 AFIX 23 H14A 2 -0.029847 -0.024582 0.787367 11.00000 -1.20000 H14B 2 0.029264 -0.118448 0.737977 11.00000 -1.20000 AFIX 0 C15 1 0.094546 0.144673 0.803844 11.00000 0.03301 0.03401 = 0.03149 -0.00733 0.00931 0.00231 AFIX 23 H15A 2 0.070203 0.144831 0.857553 11.00000 -1.20000 H15B 2 0.048125 0.186106 0.769805 11.00000 -1.20000 AFIX 0 C16 1 0.187004 0.208563 0.801960 11.00000 0.03426 0.02730 = 0.02160 -0.00758 0.00291 -0.00224 AFIX 23 H16A 2 0.177140 0.293985 0.813602 11.00000 -1.20000 H16B 2 0.229932 0.175336 0.842412 11.00000 -1.20000 AFIX 0 C17 1 0.235440 0.309108 0.684080 11.00000 0.02502 0.02016 = 0.02713 -0.00260 -0.00091 -0.00621 AFIX 23 H17A 2 0.300431 0.320994 0.665234 11.00000 -1.20000 H17B 2 0.220112 0.375821 0.719388 11.00000 -1.20000 AFIX 0 C18 1 0.166434 0.308088 0.615274 11.00000 0.02153 0.01499 = 0.03082 0.00196 0.00094 0.00074 AFIX 23 H18A 2 0.101036 0.301612 0.634274 11.00000 -1.20000 H18B 2 0.171896 0.383357 0.585663 11.00000 -1.20000 AFIX 0 C19 1 0.106362 0.172605 0.513280 11.00000 0.03265 0.02561 = 0.02112 0.00283 -0.01129 0.00251 AFIX 23 H19A 2 0.126021 0.109802 0.476466 11.00000 -1.20000 H19B 2 0.086213 0.242914 0.482490 11.00000 -1.20000 AFIX 0 C20 1 0.024221 0.127988 0.560026 11.00000 0.01972 0.02762 = 0.03525 -0.00387 -0.01233 0.00223 AFIX 23 H20A 2 -0.009254 0.196256 0.583443 11.00000 -1.20000 H20B 2 -0.020759 0.085061 0.525473 11.00000 -1.20000 AFIX 0 C21 1 0.144271 -0.052935 0.839466 11.00000 0.05712 0.05949 = 0.03259 0.02168 0.01962 0.02682 AFIX 137 H21A 2 0.099752 -0.053659 0.882564 11.00000 -1.50000 H21B 2 0.204750 -0.020008 0.857565 11.00000 -1.50000 H21C 2 0.153725 -0.134445 0.820718 11.00000 -1.50000 AFIX 0 C22 1 0.267001 0.238452 0.514092 11.00000 0.02863 0.03050 = 0.02465 0.01116 0.00670 0.00492 AFIX 137 H22A 2 0.282471 0.171256 0.480185 11.00000 -1.50000 H22B 2 0.322036 0.258461 0.546717 11.00000 -1.50000 H22C 2 0.249372 0.307492 0.482150 11.00000 -1.50000 HKLF 4 REM w13_a59sadm in P2(1)/c REM R1 = 0.0433 for 5477 Fo > 4sig(Fo) and 0.0542 for all 6838 data REM 298 parameters refined using 0 restraints END WGHT 0.0596 0.0000 REM Highest difference peak 1.150, deepest hole -0.603, 1-sigma level 0.072 Q1 1 0.1452 0.0922 0.8396 11.00000 0.05 1.15 Q2 1 0.0032 0.0476 0.7550 11.00000 0.05 1.07 Q3 1 0.0993 -0.1190 0.8166 11.00000 0.05 1.02 Q4 1 0.2228 0.1232 0.7053 11.00000 0.05 0.41 Q5 1 0.3199 -0.0544 0.5677 11.00000 0.05 0.40 Q6 1 0.4538 0.0140 0.6316 11.00000 0.05 0.36 Q7 1 0.1782 0.2458 0.5797 11.00000 0.05 0.35 Q8 1 0.5380 -0.2425 0.6394 11.00000 0.05 0.35 Q9 1 0.3553 -0.2014 0.7283 11.00000 0.05 0.35 Q10 1 0.2651 -0.3385 0.5574 11.00000 0.05 0.35 ; _database_code_depnum_ccdc_archive 'CCDC 961425' ####################################################################### # # 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_4 # Start Validation Reply Form _vrf_PLAT305_4 ; PROBLEM: Isolated Hydrogen Atom (Outside Bond Range ??) H2A RESPONSE: This is a hydride atom bound to a metal atom. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C30 H68 N12 Sc3), 3(C6 H5 S), 3(C4 H8 O)' _chemical_formula_sum 'C120 H243 N36 O3 S3 Sc9' _chemical_formula_weight 2739.32 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' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 63' _symmetry_space_group_name_Hall 'P 6c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z' '-x+y, -x, z' 'x-y, x, z+1/2' 'y, -x+y, z+1/2' _cell_length_a 19.2442(17) _cell_length_b 19.2442(17) _cell_length_c 21.4089(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6866.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9856 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.46 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 0.523 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8380 _exptl_absorpt_correction_T_max 0.8935 _exptl_absorpt_process_details 'Sadabs Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82918 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 26.46 _reflns_number_total 9437 _reflns_number_gt 8291 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Altomare 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1999)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydride atoms H1A, H1B, H2A, H2B, H3A, H3B were located in a Difference Fourier map and were fixed in their position. All other H-atoms were included in calculated positions and treated as riding. The structure includes thf in the crystal lattice that is disordered against a C6H5S - anion. The atoms of the disordered groups could only be refined with isotropic displacement parameters. One of the three crystallogaraphically independent cationic fragments show a small disorder (C26, C27, C30). These atoms were included in the refinement with split positions and isotropic displacement parameters. ; _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^)+(0.1071P)^2^+6.2341P] 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 0.13(4) _refine_ls_number_reflns 9437 _refine_ls_number_parameters 492 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1845 _refine_ls_wR_factor_gt 0.1758 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.015 _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 Sc1 Sc 0.43077(4) 0.76430(4) 0.79711(3) 0.0194(2) Uani 1 1 d . . . H1A H 0.3333 0.6667 0.7483 0.023 Uiso 1 3 d SR . . H1B H 0.3333 0.6667 0.8498 0.023 Uiso 1 3 d SR . . N1 N 0.3323(2) 0.79390(19) 0.80492(18) 0.0206(7) Uani 1 1 d . . . N2 N 0.4606(2) 0.8292(2) 0.89852(17) 0.0227(8) Uani 1 1 d . . . N3 N 0.5438(2) 0.8663(2) 0.78856(19) 0.0299(9) Uani 1 1 d . . . N4 N 0.4354(2) 0.8295(2) 0.69627(19) 0.0308(9) Uani 1 1 d . . . C1 C 0.3397(3) 0.8328(3) 0.8662(2) 0.0274(10) Uani 1 1 d . . . H1C H 0.3082 0.7910 0.8977 0.033 Uiso 1 1 calc R . . H1D H 0.3165 0.8685 0.8631 0.033 Uiso 1 1 calc R . . C2 C 0.4267(3) 0.8818(3) 0.8882(2) 0.0269(10) Uani 1 1 d . . . H2C H 0.4589 0.9228 0.8564 0.032 Uiso 1 1 calc R . . H2D H 0.4290 0.9099 0.9276 0.032 Uiso 1 1 calc R . . C3 C 0.5507(3) 0.8762(3) 0.9021(2) 0.0294(10) Uani 1 1 d . . . H3C H 0.5673 0.9162 0.9362 0.035 Uiso 1 1 calc R . . H3D H 0.5711 0.8394 0.9121 0.035 Uiso 1 1 calc R . . C4 C 0.5866(3) 0.9181(2) 0.8422(3) 0.0305(10) Uani 1 1 d . . . H4A H 0.5838 0.9681 0.8399 0.037 Uiso 1 1 calc R . . H4B H 0.6439 0.9330 0.8406 0.037 Uiso 1 1 calc R . . C5 C 0.5736(3) 0.9111(3) 0.7313(3) 0.0373(12) Uani 1 1 d . . . H5A H 0.6270 0.9178 0.7221 0.045 Uiso 1 1 calc R . . H5B H 0.5804 0.9651 0.7372 0.045 Uiso 1 1 calc R . . C6 C 0.5211(5) 0.8730(5) 0.6776(4) 0.070(2) Uani 1 1 d . . . H6A H 0.5349 0.8349 0.6579 0.084 Uiso 1 1 calc R . . H6B H 0.5299 0.9145 0.6463 0.084 Uiso 1 1 calc R . . C7 C 0.4096(4) 0.8843(4) 0.7160(3) 0.0513(16) Uani 1 1 d . . . H7A H 0.4025 0.9107 0.6789 0.062 Uiso 1 1 calc R . . H7B H 0.4517 0.9264 0.7426 0.062 Uiso 1 1 calc R . . C8 C 0.3305(3) 0.8417(3) 0.7527(3) 0.0387(13) Uani 1 1 d . . . H8A H 0.3180 0.8824 0.7688 0.046 Uiso 1 1 calc R . . H8B H 0.2868 0.8062 0.7239 0.046 Uiso 1 1 calc R . . C9 C 0.4329(3) 0.7896(3) 0.9587(2) 0.0339(11) Uani 1 1 d . . . H9A H 0.4516 0.8300 0.9919 0.051 Uiso 1 1 calc R . . H9B H 0.4543 0.7535 0.9657 0.051 Uiso 1 1 calc R . . H9C H 0.3741 0.7586 0.9590 0.051 Uiso 1 1 calc R . . C10 C 0.3961(7) 0.7909(5) 0.6379(3) 0.095(3) Uani 1 1 d . . . H10A H 0.3968 0.8311 0.6094 0.143 Uiso 1 1 calc R . . H10B H 0.3404 0.7496 0.6464 0.143 Uiso 1 1 calc R . . H10C H 0.4246 0.7661 0.6187 0.143 Uiso 1 1 calc R . . Sc2 Sc 0.67292(4) 0.43477(4) 0.80386(3) 0.01710(18) Uani 1 1 d . . . H2A H 0.6667 0.3333 0.8568 0.021 Uiso 1 3 d SR . . H2B H 0.6667 0.3333 0.7473 0.021 Uiso 1 3 d SR . . N5 N 0.54333(19) 0.34077(19) 0.80592(17) 0.0198(7) Uani 1 1 d . . . N6 N 0.6324(2) 0.4602(2) 0.90496(17) 0.0241(8) Uani 1 1 d . . . N7 N 0.6899(2) 0.5512(2) 0.8010(2) 0.0268(8) Uani 1 1 d . . . N8 N 0.6241(3) 0.4515(2) 0.7026(2) 0.0320(9) Uani 1 1 d . . . C11 C 0.5078(3) 0.3462(3) 0.8662(2) 0.0309(11) Uani 1 1 d . . . H11A H 0.5131 0.3111 0.8973 0.037 Uiso 1 1 calc R . . H11B H 0.4498 0.3262 0.8601 0.037 Uiso 1 1 calc R . . C12 C 0.5470(3) 0.4307(3) 0.8916(2) 0.0246(9) Uani 1 1 d . . . H12A H 0.5421 0.4664 0.8607 0.030 Uiso 1 1 calc R . . H12B H 0.5193 0.4316 0.9303 0.030 Uiso 1 1 calc R . . C13 C 0.6770(3) 0.5496(3) 0.9130(2) 0.0321(11) Uani 1 1 d . . . H13A H 0.6509 0.5643 0.9462 0.038 Uiso 1 1 calc R . . H13B H 0.7326 0.5673 0.9265 0.038 Uiso 1 1 calc R . . C14 C 0.6794(3) 0.5923(3) 0.8541(2) 0.0292(10) Uani 1 1 d . . . H14A H 0.6287 0.5934 0.8494 0.035 Uiso 1 1 calc R . . H14B H 0.7243 0.6483 0.8558 0.035 Uiso 1 1 calc R . . C15 C 0.6828(3) 0.5869(3) 0.7433(3) 0.0376(12) Uani 1 1 d . . . H15A H 0.6366 0.5959 0.7468 0.045 Uiso 1 1 calc R . . H15B H 0.7318 0.6399 0.7377 0.045 Uiso 1 1 calc R . . C16 C 0.6723(6) 0.5393(4) 0.6900(4) 0.083(3) Uani 1 1 d . . . H16A H 0.7257 0.5520 0.6740 0.099 Uiso 1 1 calc R . . H16B H 0.6454 0.5533 0.6570 0.099 Uiso 1 1 calc R . . C17 C 0.5435(4) 0.4272(4) 0.7179(3) 0.0523(16) Uani 1 1 d . . . H17A H 0.5139 0.4236 0.6791 0.063 Uiso 1 1 calc R . . H17B H 0.5426 0.4686 0.7448 0.063 Uiso 1 1 calc R . . C18 C 0.5004(3) 0.3464(3) 0.7517(3) 0.0407(13) Uani 1 1 d . . . H18A H 0.4470 0.3364 0.7654 0.049 Uiso 1 1 calc R . . H18B H 0.4917 0.3036 0.7217 0.049 Uiso 1 1 calc R . . C19 C 0.6392(3) 0.4282(3) 0.9650(2) 0.0357(11) Uani 1 1 d . . . H19A H 0.6170 0.3701 0.9615 0.054 Uiso 1 1 calc R . . H19B H 0.6093 0.4393 0.9968 0.054 Uiso 1 1 calc R . . H19C H 0.6958 0.4538 0.9771 0.054 Uiso 1 1 calc R . . C20 C 0.6370(5) 0.4248(6) 0.6418(3) 0.073(2) Uani 1 1 d . . . H20A H 0.6020 0.4290 0.6106 0.110 Uiso 1 1 calc R . . H20B H 0.6244 0.3689 0.6449 0.110 Uiso 1 1 calc R . . H20C H 0.6931 0.4587 0.6293 0.110 Uiso 1 1 calc R . . Sc3 Sc 0.92882(4) 0.04021(4) 0.84301(5) 0.02496(19) Uani 1 1 d . . . H3A H 1.0000 0.0000 0.8978 0.030 Uiso 1 3 d SR . . H3B H 1.0000 0.0000 0.7804 0.030 Uiso 1 3 d SR . . N9 N 0.8546(2) -0.0929(2) 0.8376(2) 0.0297(8) Uani 1 1 d . B . N10 N 0.8648(2) 0.0230(2) 0.7412(2) 0.0321(9) Uani 1 1 d . . . N11 N 0.8600(2) 0.0944(2) 0.8490(2) 0.0356(9) Uani 1 1 d . B . N12 N 0.8583(3) 0.0003(3) 0.9459(2) 0.0398(10) Uani 1 1 d . . . C21 C 0.8143(3) -0.1159(3) 0.7759(3) 0.0361(11) Uani 1 1 d . . . H21A H 0.7655 -0.1694 0.7792 0.043 Uiso 1 1 calc R . . H21B H 0.8507 -0.1200 0.7453 0.043 Uiso 1 1 calc R . . C22 C 0.7915(3) -0.0566(3) 0.7526(3) 0.0347(11) Uani 1 1 d . . . H22A H 0.7606 -0.0766 0.7133 0.042 Uiso 1 1 calc R . . H22B H 0.7569 -0.0506 0.7838 0.042 Uiso 1 1 calc R . . C23 C 0.8445(3) 0.0887(3) 0.7374(3) 0.0349(11) Uani 1 1 d . . . H23A H 0.8930 0.1393 0.7250 0.042 Uiso 1 1 calc R . . H23B H 0.8033 0.0751 0.7047 0.042 Uiso 1 1 calc R . . C24 C 0.8140(3) 0.1010(3) 0.7979(3) 0.0360(11) Uani 1 1 d . . . H24A H 0.8188 0.1547 0.7985 0.043 Uiso 1 1 calc R . . H24B H 0.7566 0.0602 0.8028 0.043 Uiso 1 1 calc R . . C25 C 0.8288(4) 0.1014(3) 0.9093(3) 0.0483(15) Uani 1 1 d . . . H25A H 0.7871 0.1166 0.9034 0.058 Uiso 0.50 1 d PR A 1 H25B H 0.8725 0.1432 0.9349 0.058 Uiso 0.50 1 d PR A 1 H25C H 0.8488 0.1590 0.9172 0.058 Uiso 0.50 1 d PR A 2 H25D H 0.7696 0.0749 0.9058 0.058 Uiso 0.50 1 d PR A 2 C26A C 0.7931(5) 0.0199(5) 0.9421(4) 0.0245(17) Uiso 0.50 1 d P B 1 H26A H 0.7740 0.0229 0.9844 0.029 Uiso 0.50 1 calc PR B 1 H26B H 0.7472 -0.0217 0.9179 0.029 Uiso 0.50 1 calc PR B 1 C27A C 0.8208(5) -0.0916(5) 0.9467(4) 0.0245(17) Uiso 0.50 1 d P B 1 H27A H 0.8607 -0.1049 0.9636 0.029 Uiso 0.50 1 calc PR B 1 H27B H 0.7743 -0.1147 0.9755 0.029 Uiso 0.50 1 calc PR B 1 C26B C 0.8443(11) 0.0734(11) 0.9564(8) 0.077(4) Uiso 0.50 1 d P B 2 H26C H 0.7996 0.0567 0.9864 0.092 Uiso 0.50 1 calc PR B 2 H26D H 0.8930 0.1172 0.9763 0.092 Uiso 0.50 1 calc PR B 2 C27B C 0.7848(8) -0.0651(8) 0.9260(7) 0.058(3) Uiso 0.50 1 d P B 2 H27C H 0.7563 -0.0448 0.8999 0.070 Uiso 0.50 1 calc PR B 2 H27D H 0.7510 -0.0916 0.9631 0.070 Uiso 0.50 1 calc PR B 2 C28 C 0.7954(3) -0.1278(3) 0.8882(3) 0.0467(15) Uani 1 1 d . . . H28A H 0.7472 -0.1253 0.8759 0.056 Uiso 0.50 1 d PR B 1 H28B H 0.7793 -0.1852 0.8923 0.056 Uiso 0.50 1 d PR B 1 H28C H 0.8118 -0.1574 0.9169 0.056 Uiso 0.50 1 d PR B 2 H28D H 0.7429 -0.1670 0.8699 0.056 Uiso 0.50 1 d PR B 2 C29 C 0.8991(3) 0.0205(4) 0.6799(3) 0.0414(13) Uani 1 1 d . . . H29A H 0.9436 0.0741 0.6697 0.062 Uiso 1 1 calc R . . H29B H 0.8576 0.0034 0.6476 0.062 Uiso 1 1 calc R . . H29C H 0.9189 -0.0175 0.6818 0.062 Uiso 1 1 calc R . . C30A C 0.9002(7) 0.0296(7) 1.0061(5) 0.031(2) Uiso 0.50 1 d P B 1 H30A H 0.8721 0.0480 1.0338 0.047 Uiso 0.50 1 calc PR B 1 H30B H 0.8940 0.0418 0.9627 0.047 Uiso 0.50 1 calc PR B 1 H30C H 0.9573 0.0571 1.0170 0.047 Uiso 0.50 1 calc PR B 1 C30B C 0.8880(13) -0.0013(12) 1.0087(10) 0.084(6) Uiso 0.50 1 d P B . H30D H 0.9312 -0.0143 1.0074 0.127 Uiso 0.50 1 calc PR C 1 H30E H 0.8501 -0.0292 0.9746 0.127 Uiso 0.50 1 calc PR C 1 H30F H 0.8599 -0.0185 1.0488 0.127 Uiso 0.50 1 calc PR C 1 S1A S 0.44234(10) 0.99571(10) 0.54592(10) 0.0382(4) Uiso 0.70 1 d P D 1 C31A C 0.3411(5) 0.9463(5) 0.5646(3) 0.0347(16) Uiso 0.70 1 d P D 1 C32A C 0.2898(4) 0.8665(4) 0.5415(3) 0.0279(13) Uiso 0.70 1 d P D 1 H32A H 0.3116 0.8434 0.5142 0.033 Uiso 0.70 1 calc PR D 1 C33A C 0.2057(5) 0.8201(5) 0.5586(4) 0.0351(16) Uiso 0.70 1 d P D 1 H33A H 0.1736 0.7678 0.5418 0.042 Uiso 0.70 1 calc PR D 1 C34A C 0.1718(6) 0.8505(6) 0.5987(4) 0.043(2) Uiso 0.70 1 d P D 1 H34A H 0.1171 0.8198 0.6108 0.051 Uiso 0.70 1 calc PR D 1 C35A C 0.2210(6) 0.9284(6) 0.6211(4) 0.0436(19) Uiso 0.70 1 d P D 1 H35A H 0.1991 0.9512 0.6487 0.052 Uiso 0.70 1 calc PR D 1 C36A C 0.3019(6) 0.9737(5) 0.6038(4) 0.0412(18) Uiso 0.70 1 d P D 1 H36A H 0.3322 1.0267 0.6198 0.049 Uiso 0.70 1 calc PR D 1 O1A O 0.6719(14) 1.0646(14) 0.5260(10) 0.228(9) Uiso 0.70 1 d P E 1 C37A C 0.7377(14) 1.1574(14) 0.5395(12) 0.150(7) Uiso 0.70 1 d P E 1 H37A H 0.7645 1.1872 0.5009 0.180 Uiso 0.70 1 calc PR E 1 H37B H 0.7150 1.1859 0.5628 0.180 Uiso 0.70 1 calc PR E 1 C38A C 0.7925(9) 1.1395(9) 0.5799(6) 0.086(4) Uiso 0.70 1 d P E 1 H38A H 0.8492 1.1804 0.5718 0.103 Uiso 0.70 1 calc PR E 1 H38B H 0.7811 1.1429 0.6245 0.103 Uiso 0.70 1 calc PR E 1 C39A C 0.7815(6) 1.0639(6) 0.5675(4) 0.049(2) Uiso 0.70 1 d P E 1 H39A H 0.8205 1.0684 0.5354 0.058 Uiso 0.70 1 calc PR E 1 H39B H 0.7919 1.0420 0.6059 0.058 Uiso 0.70 1 calc PR E 1 C40A C 0.7043(9) 1.0117(9) 0.5466(8) 0.097(4) Uiso 0.70 1 d P E 1 H40A H 0.6711 0.9754 0.5807 0.116 Uiso 0.70 1 calc PR E 1 H40B H 0.7053 0.9789 0.5114 0.116 Uiso 0.70 1 calc PR E 1 S1B S 0.5297(3) 1.0150(3) 0.5515(3) 0.0467(10) Uiso 0.30 1 d P F 2 C31B C 0.6407(7) 1.0568(9) 0.5583(9) 0.056(5) Uiso 0.30 1 d PG F 2 C32B C 0.6959(8) 1.1379(8) 0.5507(9) 0.063(6) Uiso 0.30 1 d PG F 2 H32B H 0.6777 1.1752 0.5450 0.076 Uiso 0.30 1 calc PR F 2 C33B C 0.7776(8) 1.1645(8) 0.5515(9) 0.050(4) Uiso 0.30 1 d PG F 2 H33B H 0.8153 1.2199 0.5464 0.060 Uiso 0.30 1 calc PR F 2 C34B C 0.8042(8) 1.1099(12) 0.5598(11) 0.089(9) Uiso 0.30 1 d PG F 2 H34B H 0.8601 1.1281 0.5604 0.106 Uiso 0.30 1 calc PR F 2 C35B C 0.7491(12) 1.0288(11) 0.5674(11) 0.098(11) Uiso 0.30 1 d PG F 2 H35B H 0.7673 0.9916 0.5731 0.117 Uiso 0.30 1 calc PR F 2 C36B C 0.6673(10) 1.0023(7) 0.5666(9) 0.065(6) Uiso 0.30 1 d PG F 2 H36B H 0.6296 0.9468 0.5718 0.078 Uiso 0.30 1 calc PR F 2 O1B O 0.312(2) 0.912(2) 0.5503(18) 0.137(10) Uiso 0.30 1 d P G 2 C37B C 0.326(3) 0.990(3) 0.567(2) 0.116(13) Uiso 0.30 1 d P G 2 H37C H 0.3148 1.0177 0.5327 0.140 Uiso 0.30 1 calc PR G 2 H37D H 0.3801 1.0257 0.5846 0.140 Uiso 0.30 1 calc PR G 2 C38B C 0.2622(14) 0.9583(11) 0.6157(8) 0.032(4) Uiso 0.30 1 d P G 2 H38C H 0.2873 0.9655 0.6573 0.039 Uiso 0.30 1 calc PR G 2 H38D H 0.2339 0.9895 0.6150 0.039 Uiso 0.30 1 calc PR G 2 C39B C 0.2064(18) 0.8772(18) 0.6068(13) 0.064(7) Uiso 0.30 1 d P G 2 H39C H 0.1545 0.8701 0.5920 0.076 Uiso 0.30 1 calc PR G 2 H39D H 0.1973 0.8468 0.6462 0.076 Uiso 0.30 1 calc PR G 2 C40B C 0.2444(19) 0.8492(16) 0.5573(13) 0.061(6) Uiso 0.30 1 d P G 2 H40C H 0.2501 0.8037 0.5724 0.073 Uiso 0.30 1 calc PR G 2 H40D H 0.2130 0.8336 0.5180 0.073 Uiso 0.30 1 calc PR G 2 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 Sc1 0.0172(4) 0.0167(4) 0.0239(5) -0.0008(3) 0.0025(3) 0.0081(3) N1 0.0230(16) 0.0142(15) 0.0250(17) 0.0028(14) 0.0007(15) 0.0096(13) N2 0.0235(18) 0.0173(17) 0.026(2) -0.0024(14) 0.0017(14) 0.0094(15) N3 0.0229(18) 0.0217(18) 0.036(2) -0.0047(16) 0.0071(16) 0.0045(15) N4 0.033(2) 0.030(2) 0.026(2) 0.0041(16) 0.0053(17) 0.0132(18) C1 0.025(2) 0.022(2) 0.037(3) -0.0048(18) 0.0093(19) 0.0142(18) C2 0.027(2) 0.015(2) 0.033(2) -0.0033(17) 0.0040(19) 0.0066(18) C3 0.023(2) 0.026(2) 0.037(3) -0.0058(19) -0.0056(19) 0.0102(19) C4 0.021(2) 0.020(2) 0.045(3) -0.003(2) -0.003(2) 0.0065(16) C5 0.024(2) 0.036(3) 0.044(3) 0.006(2) 0.008(2) 0.009(2) C6 0.066(5) 0.074(5) 0.069(5) 0.021(4) 0.029(4) 0.036(4) C7 0.062(4) 0.057(4) 0.049(3) 0.022(3) 0.011(3) 0.040(3) C8 0.025(2) 0.041(3) 0.051(3) 0.023(3) 0.011(2) 0.017(2) C9 0.041(3) 0.030(2) 0.030(3) -0.006(2) 0.001(2) 0.017(2) C10 0.170(10) 0.071(5) 0.026(3) -0.001(3) -0.004(4) 0.046(6) Sc2 0.0161(3) 0.0159(3) 0.0188(4) 0.0001(3) 0.0005(3) 0.0077(3) N5 0.0178(15) 0.0182(15) 0.0235(17) -0.0006(14) -0.0026(15) 0.0091(13) N6 0.0262(19) 0.029(2) 0.0232(19) -0.0008(15) 0.0030(15) 0.0186(17) N7 0.0309(19) 0.0207(17) 0.032(2) 0.0054(16) 0.0016(17) 0.0155(15) N8 0.046(2) 0.033(2) 0.025(2) 0.0070(17) 0.0021(18) 0.026(2) C11 0.023(2) 0.022(2) 0.051(3) 0.003(2) 0.015(2) 0.0136(18) C12 0.029(2) 0.025(2) 0.028(2) 0.0029(18) 0.0051(18) 0.019(2) C13 0.031(3) 0.030(2) 0.036(3) -0.018(2) -0.011(2) 0.016(2) C14 0.024(2) 0.021(2) 0.042(3) -0.0066(19) -0.0043(19) 0.0109(17) C15 0.030(2) 0.023(2) 0.051(3) 0.012(2) -0.009(2) 0.007(2) C16 0.126(8) 0.049(4) 0.068(5) 0.004(4) -0.035(5) 0.040(5) C17 0.044(3) 0.061(4) 0.047(3) 0.012(3) -0.008(3) 0.022(3) C18 0.031(3) 0.026(2) 0.052(3) 0.009(2) -0.021(2) 0.005(2) C19 0.044(3) 0.056(3) 0.021(2) -0.002(2) 0.001(2) 0.035(3) C20 0.094(6) 0.145(8) 0.021(3) 0.006(4) 0.007(3) 0.089(6) Sc3 0.0200(4) 0.0199(4) 0.0358(4) -0.0024(4) -0.0009(4) 0.0105(3) N9 0.0238(17) 0.0256(18) 0.039(2) -0.0002(18) 0.0043(19) 0.0119(15) N10 0.0238(19) 0.033(2) 0.039(2) -0.0007(17) -0.0018(16) 0.0141(17) N11 0.036(2) 0.033(2) 0.044(2) -0.001(2) 0.001(2) 0.0229(17) N12 0.037(2) 0.043(2) 0.042(3) -0.006(2) 0.0036(19) 0.022(2) C21 0.029(2) 0.025(2) 0.058(3) -0.013(2) -0.008(2) 0.016(2) C22 0.022(2) 0.032(2) 0.050(3) -0.012(2) -0.006(2) 0.013(2) C23 0.033(3) 0.028(2) 0.047(3) 0.002(2) -0.009(2) 0.017(2) C24 0.025(2) 0.025(2) 0.060(3) -0.002(2) -0.001(2) 0.0139(18) C25 0.056(4) 0.034(3) 0.066(4) -0.002(3) 0.019(3) 0.031(3) C28 0.033(3) 0.032(3) 0.072(4) 0.006(3) 0.023(3) 0.014(2) C29 0.033(3) 0.054(3) 0.036(3) -0.004(2) -0.002(2) 0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sc1 N3 2.085(4) . ? Sc1 H1A 2.1487 . ? Sc1 H1B 2.1902 . ? Sc1 N1 2.222(3) 4_565 ? Sc1 N1 2.242(3) . ? Sc1 N2 2.426(4) . ? Sc1 N4 2.476(4) . ? Sc1 Sc1 3.2512(13) 3_665 ? Sc1 Sc1 3.2512(13) 4_565 ? N1 C8 1.459(6) . ? N1 C1 1.482(6) . ? N1 Sc1 2.222(3) 3_665 ? N2 C9 1.456(6) . ? N2 C2 1.468(6) . ? N2 C3 1.505(6) . ? N3 C5 1.443(7) . ? N3 C4 1.474(6) . ? N4 C7 1.435(7) . ? N4 C10 1.457(8) . ? N4 C6 1.483(8) . ? C1 C2 1.529(7) . ? C3 C4 1.488(7) . ? C5 C6 1.462(10) . ? C7 C8 1.536(8) . ? Sc2 N7 2.098(3) . ? Sc2 H2A 2.2081 . ? Sc2 N5 2.216(3) 4_665 ? Sc2 N5 2.232(3) . ? Sc2 H2B 2.2481 . ? Sc2 N6 2.432(4) . ? Sc2 N8 2.447(4) . ? Sc2 Sc2 3.2818(12) 3_655 ? Sc2 Sc2 3.2818(12) 4_665 ? N5 C18 1.460(6) . ? N5 C11 1.489(6) . ? N5 Sc2 2.216(3) 3_655 ? N6 C19 1.460(6) . ? N6 C12 1.473(6) . ? N6 C13 1.499(6) . ? N7 C15 1.452(7) . ? N7 C14 1.456(6) . ? N8 C17 1.418(8) . ? N8 C20 1.464(7) . ? N8 C16 1.490(9) . ? C11 C12 1.511(6) . ? C13 C14 1.493(7) . ? C15 C16 1.414(10) . ? C17 C18 1.529(8) . ? Sc3 N11 2.059(4) . ? Sc3 H3A 2.2159 . ? Sc3 N9 2.226(4) . ? Sc3 N9 2.227(4) 4_765 ? Sc3 H3B 2.3093 . ? Sc3 N10 2.443(4) . ? Sc3 N12 2.499(5) . ? Sc3 Sc3 3.2565(13) 3_645 ? Sc3 Sc3 3.2565(13) 4_765 ? N9 C28 1.467(7) . ? N9 C21 1.483(7) . ? N9 Sc3 2.227(4) 3_645 ? N10 C29 1.481(7) . ? N10 C22 1.496(6) . ? N10 C23 1.500(6) . ? N11 C24 1.452(7) . ? N11 C25 1.459(7) . ? N12 C30B 1.47(2) . ? N12 C27B 1.409(14) . ? N12 C30A 1.474(12) . ? N12 C26A 1.484(9) . ? N12 C27A 1.540(9) . ? N12 C26B 1.577(18) . ? C21 C22 1.498(7) . ? C23 C24 1.489(8) . ? C25 C26B 1.248(18) . ? C25 C26A 1.532(10) . ? C27A C28 1.398(11) . ? C27A C30B 2.05(2) . ? C27B C28 1.550(15) . ? C30A C30B 0.52(2) . ? S1A C31A 1.734(8) . ? C31A C36A 1.396(13) . ? C31A C32A 1.435(11) . ? C32A C33A 1.451(10) . ? C33A C34A 1.375(11) . ? C34A C35A 1.398(14) . ? C35A C36A 1.402(12) . ? O1A C40A 1.50(2) . ? O1A C37A 1.62(3) . ? C37A C38A 1.53(2) . ? C38A C39A 1.387(17) . ? C39A C40A 1.386(18) . ? S1B C31B 1.875(13) . ? C31B C32B 1.3900 . ? C31B C36B 1.3900 . ? C32B C33B 1.3900 . ? C33B C34B 1.3900 . ? C34B C35B 1.3900 . ? C35B C36B 1.3900 . ? O1B C40B 1.27(4) . ? O1B C37B 1.44(5) . ? C37B C38B 1.48(5) . ? C38B C39B 1.40(4) . ? C39B C40B 1.53(4) . ? 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 N3 Sc1 H1A 145.5 . . ? N3 Sc1 H1B 153.6 . . ? H1A Sc1 H1B 60.1 . . ? N3 Sc1 N1 101.81(14) . 4_565 ? H1A Sc1 N1 77.7 . 4_565 ? H1B Sc1 N1 73.5 . 4_565 ? N3 Sc1 N1 112.59(14) . . ? H1A Sc1 N1 77.3 . . ? H1B Sc1 N1 73.1 . . ? N1 Sc1 N1 145.12(13) 4_565 . ? N3 Sc1 N2 74.17(14) . . ? H1A Sc1 N2 139.8 . . ? H1B Sc1 N2 82.0 . . ? N1 Sc1 N2 105.68(13) 4_565 . ? N1 Sc1 N2 79.31(13) . . ? N3 Sc1 N4 71.95(15) . . ? H1A Sc1 N4 79.2 . . ? H1B Sc1 N4 133.0 . . ? N1 Sc1 N4 122.18(14) 4_565 . ? N1 Sc1 N4 75.94(13) . . ? N2 Sc1 N4 125.43(13) . . ? N3 Sc1 Sc1 154.71(12) . 3_665 ? H1A Sc1 Sc1 40.8 . 3_665 ? H1B Sc1 Sc1 42.1 . 3_665 ? N1 Sc1 Sc1 103.27(9) 4_565 3_665 ? N1 Sc1 Sc1 43.02(8) . 3_665 ? N2 Sc1 Sc1 101.85(9) . 3_665 ? N4 Sc1 Sc1 91.84(10) . 3_665 ? N3 Sc1 Sc1 144.50(12) . 4_565 ? H1A Sc1 Sc1 40.8 . 4_565 ? H1B Sc1 Sc1 42.1 . 4_565 ? N1 Sc1 Sc1 43.49(9) 4_565 4_565 ? N1 Sc1 Sc1 102.81(8) . 4_565 ? N2 Sc1 Sc1 116.49(9) . 4_565 ? N4 Sc1 Sc1 116.06(10) . 4_565 ? Sc1 Sc1 Sc1 60.0 3_665 4_565 ? C8 N1 C1 112.8(3) . . ? C8 N1 Sc1 111.5(3) . 3_665 ? C1 N1 Sc1 116.1(3) . 3_665 ? C8 N1 Sc1 113.1(3) . . ? C1 N1 Sc1 108.4(3) . . ? Sc1 N1 Sc1 93.49(12) 3_665 . ? C9 N2 C2 108.7(4) . . ? C9 N2 C3 106.2(4) . . ? C2 N2 C3 111.7(4) . . ? C9 N2 Sc1 126.3(3) . . ? C2 N2 Sc1 98.5(3) . . ? C3 N2 Sc1 105.0(3) . . ? C5 N3 C4 109.7(4) . . ? C5 N3 Sc1 123.6(3) . . ? C4 N3 Sc1 122.4(3) . . ? C7 N4 C10 110.2(6) . . ? C7 N4 C6 111.1(5) . . ? C10 N4 C6 101.8(6) . . ? C7 N4 Sc1 100.2(3) . . ? C10 N4 Sc1 127.7(4) . . ? C6 N4 Sc1 105.6(4) . . ? N1 C1 C2 112.5(3) . . ? N2 C2 C1 110.4(4) . . ? C4 C3 N2 111.4(4) . . ? N3 C4 C3 110.7(3) . . ? N3 C5 C6 113.6(5) . . ? C5 C6 N4 111.5(5) . . ? N4 C7 C8 111.9(5) . . ? N1 C8 C7 113.5(4) . . ? N7 Sc2 H2A 150.5 . . ? N7 Sc2 N5 102.80(13) . 4_665 ? H2A Sc2 N5 74.6 . 4_665 ? N7 Sc2 N5 112.36(13) . . ? H2A Sc2 N5 74.2 . . ? N5 Sc2 N5 144.83(13) 4_665 . ? N7 Sc2 H2B 145.5 . . ? H2A Sc2 H2B 63.5 . . ? N5 Sc2 H2B 76.1 4_665 . ? N5 Sc2 H2B 75.8 . . ? N7 Sc2 N6 72.87(15) . . ? H2A Sc2 N6 80.8 . . ? N5 Sc2 N6 111.68(13) 4_665 . ? N5 Sc2 N6 78.74(13) . . ? H2B Sc2 N6 140.4 . . ? N7 Sc2 N8 72.43(15) . . ? H2A Sc2 N8 135.8 . . ? N5 Sc2 N8 116.24(14) 4_665 . ? N5 Sc2 N8 77.13(14) . . ? H2B Sc2 N8 77.3 . . ? N6 Sc2 N8 125.38(13) . . ? N7 Sc2 Sc2 154.55(11) . 3_655 ? H2A Sc2 Sc2 42.0 . 3_655 ? N5 Sc2 Sc2 102.63(9) 4_665 3_655 ? N5 Sc2 Sc2 42.28(8) . 3_655 ? H2B Sc2 Sc2 43.1 . 3_655 ? N6 Sc2 Sc2 98.69(10) . 3_655 ? N8 Sc2 Sc2 95.10(10) . 3_655 ? N7 Sc2 Sc2 145.36(11) . 4_665 ? H2A Sc2 Sc2 42.0 . 4_665 ? N5 Sc2 Sc2 42.64(9) 4_665 4_665 ? N5 Sc2 Sc2 102.26(8) . 4_665 ? H2B Sc2 Sc2 43.1 . 4_665 ? N6 Sc2 Sc2 116.64(9) . 4_665 ? N8 Sc2 Sc2 116.01(10) . 4_665 ? Sc2 Sc2 Sc2 60.0 3_655 4_665 ? C18 N5 C11 112.7(4) . . ? C18 N5 Sc2 114.7(3) . 3_655 ? C11 N5 Sc2 112.3(3) . 3_655 ? C18 N5 Sc2 111.6(3) . . ? C11 N5 Sc2 109.1(3) . . ? Sc2 N5 Sc2 95.08(13) 3_655 . ? C19 N6 C12 109.1(4) . . ? C19 N6 C13 105.2(4) . . ? C12 N6 C13 110.7(3) . . ? C19 N6 Sc2 126.4(3) . . ? C12 N6 Sc2 99.1(3) . . ? C13 N6 Sc2 106.0(3) . . ? C15 N7 C14 109.6(4) . . ? C15 N7 Sc2 122.0(3) . . ? C14 N7 Sc2 124.5(3) . . ? C17 N8 C20 116.0(5) . . ? C17 N8 C16 112.0(6) . . ? C20 N8 C16 96.8(6) . . ? C17 N8 Sc2 100.4(3) . . ? C20 N8 Sc2 126.7(4) . . ? C16 N8 Sc2 104.3(4) . . ? N5 C11 C12 112.8(4) . . ? N6 C12 C11 110.2(4) . . ? C14 C13 N6 112.1(4) . . ? N7 C14 C13 109.6(4) . . ? C16 C15 N7 113.3(5) . . ? C15 C16 N8 113.3(7) . . ? N8 C17 C18 113.1(5) . . ? N5 C18 C17 114.4(4) . . ? N11 Sc3 H3A 144.2 . . ? N11 Sc3 N9 112.39(15) . . ? H3A Sc3 N9 77.2 . . ? N11 Sc3 N9 102.03(15) . 4_765 ? H3A Sc3 N9 77.2 . 4_765 ? N9 Sc3 N9 145.36(14) . 4_765 ? N11 Sc3 H3B 147.7 . . ? H3A Sc3 H3B 67.5 . . ? N9 Sc3 H3B 74.4 . . ? N9 Sc3 H3B 74.4 4_765 . ? N11 Sc3 N10 73.46(17) . . ? H3A Sc3 N10 141.5 . . ? N9 Sc3 N10 78.93(15) . . ? N9 Sc3 N10 108.33(16) 4_765 . ? H3B Sc3 N10 77.3 . . ? N11 Sc3 N12 73.36(17) . . ? H3A Sc3 N12 76.2 . . ? N9 Sc3 N12 75.76(16) . . ? N9 Sc3 N12 119.63(16) 4_765 . ? H3B Sc3 N12 136.9 . . ? N10 Sc3 N12 125.84(13) . . ? N11 Sc3 Sc3 154.97(12) . 3_645 ? H3A Sc3 Sc3 42.7 . 3_645 ? N9 Sc3 Sc3 43.02(10) . 3_645 ? N9 Sc3 Sc3 102.90(9) 4_765 3_645 ? H3B Sc3 Sc3 45.2 . 3_645 ? N10 Sc3 Sc3 100.63(10) . 3_645 ? N12 Sc3 Sc3 92.22(10) . 3_645 ? N11 Sc3 Sc3 144.64(12) . 4_765 ? H3A Sc3 Sc3 42.7 . 4_765 ? N9 Sc3 Sc3 102.92(9) . 4_765 ? N9 Sc3 Sc3 43.00(9) 4_765 4_765 ? H3B Sc3 Sc3 45.2 . 4_765 ? N10 Sc3 Sc3 116.72(10) . 4_765 ? N12 Sc3 Sc3 115.24(11) . 4_765 ? Sc3 Sc3 Sc3 60.0 3_645 4_765 ? C28 N9 C21 110.5(4) . . ? C28 N9 Sc3 113.2(3) . . ? C21 N9 Sc3 109.2(3) . . ? C28 N9 Sc3 116.6(3) . 3_645 ? C21 N9 Sc3 112.3(3) . 3_645 ? Sc3 N9 Sc3 93.98(14) . 3_645 ? C29 N10 C22 108.6(4) . . ? C29 N10 C23 106.7(4) . . ? C22 N10 C23 111.2(4) . . ? C29 N10 Sc3 126.3(3) . . ? C22 N10 Sc3 98.4(3) . . ? C23 N10 Sc3 105.1(3) . . ? C24 N11 C25 111.2(4) . . ? C24 N11 Sc3 124.9(3) . . ? C25 N11 Sc3 120.0(4) . . ? C30B N12 C27B 119.1(11) . . ? C27B N12 C30A 136.0(8) . . ? C30B N12 C26A 116.4(10) . . ? C30A N12 C26A 108.7(6) . . ? C30A N12 C27A 106.5(6) . . ? C26A N12 C27A 108.8(6) . . ? C30B N12 C26B 97.5(11) . . ? C27B N12 C26B 107.3(9) . . ? C30B N12 Sc3 131.1(9) . . ? C27B N12 Sc3 99.0(6) . . ? C30A N12 Sc3 123.0(5) . . ? C26A N12 Sc3 105.7(4) . . ? C27A N12 Sc3 103.5(4) . . ? C26B N12 Sc3 99.2(7) . . ? N9 C21 C22 112.2(4) . . ? N10 C22 C21 110.4(4) . . ? C24 C23 N10 112.1(4) . . ? N11 C24 C23 109.6(4) . . ? C26B C25 N11 118.5(9) . . ? N11 C25 C26A 107.8(5) . . ? N12 C26A C25 106.4(6) . . ? C28 C27A N12 114.1(6) . . ? C25 C26B N12 117.1(13) . . ? N12 C27B C28 112.9(9) . . ? C27A C28 N9 115.8(6) . . ? N9 C28 C27B 113.8(7) . . ? C36A C31A C32A 113.5(7) . . ? C36A C31A S1A 127.0(7) . . ? C32A C31A S1A 119.4(6) . . ? C31A C32A C33A 122.1(7) . . ? C34A C33A C32A 121.1(8) . . ? C33A C34A C35A 117.4(9) . . ? C34A C35A C36A 121.4(9) . . ? C31A C36A C35A 124.5(8) . . ? C40A O1A C37A 109.6(18) . . ? C38A C37A O1A 95.7(16) . . ? C39A C38A C37A 111.5(14) . . ? C40A C39A C38A 111.7(11) . . ? C39A C40A O1A 105.1(14) . . ? C32B C31B C36B 120.0 . . ? C32B C31B S1B 122.6(9) . . ? C36B C31B S1B 117.2(9) . . ? C33B C32B C31B 120.0 . . ? C34B C33B C32B 120.0 . . ? C33B C34B C35B 120.0 . . ? C36B C35B C34B 120.0 . . ? C35B C36B C31B 120.0 . . ? C40B O1B C37B 122(3) . . ? O1B C37B C38B 93(3) . . ? C39B C38B C37B 112(2) . . ? C38B C39B C40B 105(2) . . ? O1B C40B C39B 101(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Sc1 N1 C8 56.5(4) . . . . ? H1A Sc1 N1 C8 -88.7 . . . . ? H1B Sc1 N1 C8 -151.0 . . . . ? N1 Sc1 N1 C8 -133.7(4) 4_565 . . . ? N2 Sc1 N1 C8 124.2(3) . . . . ? N4 Sc1 N1 C8 -6.7(3) . . . . ? Sc1 Sc1 N1 C8 -115.2(4) 3_665 . . . ? Sc1 Sc1 N1 C8 -120.8(3) 4_565 . . . ? N3 Sc1 N1 C1 -69.3(3) . . . . ? H1A Sc1 N1 C1 145.5 . . . . ? H1B Sc1 N1 C1 83.2 . . . . ? N1 Sc1 N1 C1 100.5(3) 4_565 . . . ? N2 Sc1 N1 C1 -1.6(2) . . . . ? N4 Sc1 N1 C1 -132.5(3) . . . . ? Sc1 Sc1 N1 C1 119.0(3) 3_665 . . . ? Sc1 Sc1 N1 C1 113.4(2) 4_565 . . . ? N3 Sc1 N1 Sc1 171.72(14) . . . 3_665 ? H1A Sc1 N1 Sc1 26.5 . . . 3_665 ? H1B Sc1 N1 Sc1 -35.8 . . . 3_665 ? N1 Sc1 N1 Sc1 -18.4(4) 4_565 . . 3_665 ? N2 Sc1 N1 Sc1 -120.57(14) . . . 3_665 ? N4 Sc1 N1 Sc1 108.47(15) . . . 3_665 ? Sc1 Sc1 N1 Sc1 -5.58(13) 4_565 . . 3_665 ? N3 Sc1 N2 C9 -149.6(4) . . . . ? H1A Sc1 N2 C9 37.9 . . . . ? H1B Sc1 N2 C9 18.8 . . . . ? N1 Sc1 N2 C9 -51.4(4) 4_565 . . . ? N1 Sc1 N2 C9 93.1(4) . . . . ? N4 Sc1 N2 C9 157.1(3) . . . . ? Sc1 Sc1 N2 C9 56.2(4) 3_665 . . . ? Sc1 Sc1 N2 C9 -6.0(4) 4_565 . . . ? N3 Sc1 N2 C2 89.5(3) . . . . ? H1A Sc1 N2 C2 -83.0 . . . . ? H1B Sc1 N2 C2 -102.1 . . . . ? N1 Sc1 N2 C2 -172.3(2) 4_565 . . . ? N1 Sc1 N2 C2 -27.8(3) . . . . ? N4 Sc1 N2 C2 36.2(3) . . . . ? Sc1 Sc1 N2 C2 -64.7(3) 3_665 . . . ? Sc1 Sc1 N2 C2 -126.9(2) 4_565 . . . ? N3 Sc1 N2 C3 -25.7(3) . . . . ? H1A Sc1 N2 C3 161.7 . . . . ? H1B Sc1 N2 C3 142.7 . . . . ? N1 Sc1 N2 C3 72.4(3) 4_565 . . . ? N1 Sc1 N2 C3 -143.1(3) . . . . ? N4 Sc1 N2 C3 -79.1(3) . . . . ? Sc1 Sc1 N2 C3 180.0(3) 3_665 . . . ? Sc1 Sc1 N2 C3 117.8(3) 4_565 . . . ? H1A Sc1 N3 C5 23.1 . . . . ? H1B Sc1 N3 C5 -175.0 . . . . ? N1 Sc1 N3 C5 108.4(4) 4_565 . . . ? N1 Sc1 N3 C5 -77.5(4) . . . . ? N2 Sc1 N3 C5 -148.4(4) . . . . ? N4 Sc1 N3 C5 -11.8(4) . . . . ? Sc1 Sc1 N3 C5 -64.2(5) 3_665 . . . ? Sc1 Sc1 N3 C5 98.0(4) 4_565 . . . ? H1A Sc1 N3 C4 177.3 . . . . ? H1B Sc1 N3 C4 -20.7 . . . . ? N1 Sc1 N3 C4 -97.3(3) 4_565 . . . ? N1 Sc1 N3 C4 76.8(4) . . . . ? N2 Sc1 N3 C4 5.9(3) . . . . ? N4 Sc1 N3 C4 142.4(4) . . . . ? Sc1 Sc1 N3 C4 90.1(4) 3_665 . . . ? Sc1 Sc1 N3 C4 -107.8(3) 4_565 . . . ? N3 Sc1 N4 C7 -88.2(4) . . . . ? H1A Sc1 N4 C7 111.1 . . . . ? H1B Sc1 N4 C7 81.6 . . . . ? N1 Sc1 N4 C7 179.0(3) 4_565 . . . ? N1 Sc1 N4 C7 31.7(4) . . . . ? N2 Sc1 N4 C7 -33.9(4) . . . . ? Sc1 Sc1 N4 C7 72.0(3) 3_665 . . . ? Sc1 Sc1 N4 C7 129.3(3) 4_565 . . . ? N3 Sc1 N4 C10 146.2(7) . . . . ? H1A Sc1 N4 C10 -14.5 . . . . ? H1B Sc1 N4 C10 -44.0 . . . . ? N1 Sc1 N4 C10 53.4(7) 4_565 . . . ? N1 Sc1 N4 C10 -93.9(7) . . . . ? N2 Sc1 N4 C10 -159.5(6) . . . . ? Sc1 Sc1 N4 C10 -53.6(7) 3_665 . . . ? Sc1 Sc1 N4 C10 3.7(7) 4_565 . . . ? N3 Sc1 N4 C6 27.3(4) . . . . ? H1A Sc1 N4 C6 -133.4 . . . . ? H1B Sc1 N4 C6 -162.9 . . . . ? N1 Sc1 N4 C6 -65.5(4) 4_565 . . . ? N1 Sc1 N4 C6 147.2(4) . . . . ? N2 Sc1 N4 C6 81.5(4) . . . . ? Sc1 Sc1 N4 C6 -172.5(4) 3_665 . . . ? Sc1 Sc1 N4 C6 -115.3(4) 4_565 . . . ? C8 N1 C1 C2 -94.2(4) . . . . ? Sc1 N1 C1 C2 135.3(3) 3_665 . . . ? Sc1 N1 C1 C2 31.7(4) . . . . ? C9 N2 C2 C1 -79.4(5) . . . . ? C3 N2 C2 C1 163.7(4) . . . . ? Sc1 N2 C2 C1 53.7(4) . . . . ? N1 C1 C2 N2 -63.6(5) . . . . ? C9 N2 C3 C4 178.5(4) . . . . ? C2 N2 C3 C4 -63.1(5) . . . . ? Sc1 N2 C3 C4 42.7(4) . . . . ? C5 N3 C4 C3 173.6(4) . . . . ? Sc1 N3 C4 C3 16.2(5) . . . . ? N2 C3 C4 N3 -40.5(5) . . . . ? C4 N3 C5 C6 -164.0(5) . . . . ? Sc1 N3 C5 C6 -6.9(7) . . . . ? N3 C5 C6 N4 33.6(8) . . . . ? C7 N4 C6 C5 68.0(7) . . . . ? C10 N4 C6 C5 -174.7(6) . . . . ? Sc1 N4 C6 C5 -39.8(6) . . . . ? C10 N4 C7 C8 84.3(6) . . . . ? C6 N4 C7 C8 -163.6(5) . . . . ? Sc1 N4 C7 C8 -52.4(5) . . . . ? C1 N1 C8 C7 104.3(5) . . . . ? Sc1 N1 C8 C7 -122.9(5) 3_665 . . . ? Sc1 N1 C8 C7 -19.0(6) . . . . ? N4 C7 C8 N1 53.0(7) . . . . ? N7 Sc2 N5 C18 58.3(4) . . . . ? H2A Sc2 N5 C18 -152.2 . . . . ? N5 Sc2 N5 C18 -123.9(4) 4_665 . . . ? H2B Sc2 N5 C18 -86.2 . . . . ? N6 Sc2 N5 C18 124.3(3) . . . . ? N8 Sc2 N5 C18 -6.3(3) . . . . ? Sc2 Sc2 N5 C18 -119.1(4) 3_655 . . . ? Sc2 Sc2 N5 C18 -120.6(3) 4_665 . . . ? N7 Sc2 N5 C11 -66.9(3) . . . . ? H2A Sc2 N5 C11 82.6 . . . . ? N5 Sc2 N5 C11 110.9(3) 4_665 . . . ? H2B Sc2 N5 C11 148.5 . . . . ? N6 Sc2 N5 C11 -0.9(3) . . . . ? N8 Sc2 N5 C11 -131.6(3) . . . . ? Sc2 Sc2 N5 C11 115.7(3) 3_655 . . . ? Sc2 Sc2 N5 C11 114.2(2) 4_665 . . . ? N7 Sc2 N5 Sc2 177.38(14) . . . 3_655 ? H2A Sc2 N5 Sc2 -33.1 . . . 3_655 ? N5 Sc2 N5 Sc2 -4.8(4) 4_665 . . 3_655 ? H2B Sc2 N5 Sc2 32.8 . . . 3_655 ? N6 Sc2 N5 Sc2 -116.62(15) . . . 3_655 ? N8 Sc2 N5 Sc2 112.76(15) . . . 3_655 ? Sc2 Sc2 N5 Sc2 -1.49(13) 4_665 . . 3_655 ? N7 Sc2 N6 C19 -148.1(4) . . . . ? H2A Sc2 N6 C19 18.4 . . . . ? N5 Sc2 N6 C19 -50.8(4) 4_665 . . . ? N5 Sc2 N6 C19 94.1(4) . . . . ? H2B Sc2 N6 C19 43.5 . . . . ? N8 Sc2 N6 C19 159.3(4) . . . . ? Sc2 Sc2 N6 C19 56.6(4) 3_655 . . . ? Sc2 Sc2 N6 C19 -4.1(4) 4_665 . . . ? N7 Sc2 N6 C12 90.0(3) . . . . ? H2A Sc2 N6 C12 -103.5 . . . . ? N5 Sc2 N6 C12 -172.7(2) 4_665 . . . ? N5 Sc2 N6 C12 -27.8(2) . . . . ? H2B Sc2 N6 C12 -78.4 . . . . ? N8 Sc2 N6 C12 37.3(3) . . . . ? Sc2 Sc2 N6 C12 -65.3(3) 3_655 . . . ? Sc2 Sc2 N6 C12 -126.0(2) 4_665 . . . ? N7 Sc2 N6 C13 -24.7(3) . . . . ? H2A Sc2 N6 C13 141.8 . . . . ? N5 Sc2 N6 C13 72.6(3) 4_665 . . . ? N5 Sc2 N6 C13 -142.6(3) . . . . ? H2B Sc2 N6 C13 166.8 . . . . ? N8 Sc2 N6 C13 -77.4(3) . . . . ? Sc2 Sc2 N6 C13 180.0(3) 3_655 . . . ? Sc2 Sc2 N6 C13 119.3(3) 4_665 . . . ? H2A Sc2 N7 C15 -177.8 . . . . ? N5 Sc2 N7 C15 101.0(4) 4_665 . . . ? N5 Sc2 N7 C15 -80.3(4) . . . . ? H2B Sc2 N7 C15 17.1 . . . . ? N6 Sc2 N7 C15 -150.0(4) . . . . ? N8 Sc2 N7 C15 -12.8(3) . . . . ? Sc2 Sc2 N7 C15 -76.2(5) 3_655 . . . ? Sc2 Sc2 N7 C15 97.8(4) 4_665 . . . ? H2A Sc2 N7 C14 -22.2 . . . . ? N5 Sc2 N7 C14 -103.4(3) 4_665 . . . ? N5 Sc2 N7 C14 75.3(4) . . . . ? H2B Sc2 N7 C14 172.7 . . . . ? N6 Sc2 N7 C14 5.6(3) . . . . ? N8 Sc2 N7 C14 142.8(4) . . . . ? Sc2 Sc2 N7 C14 79.4(5) 3_655 . . . ? Sc2 Sc2 N7 C14 -106.7(3) 4_665 . . . ? N7 Sc2 N8 C17 -88.4(4) . . . . ? H2A Sc2 N8 C17 81.1 . . . . ? N5 Sc2 N8 C17 175.7(4) 4_665 . . . ? N5 Sc2 N8 C17 30.4(4) . . . . ? H2B Sc2 N8 C17 108.5 . . . . ? N6 Sc2 N8 C17 -35.5(4) . . . . ? Sc2 Sc2 N8 C17 68.9(4) 3_655 . . . ? Sc2 Sc2 N8 C17 127.9(4) 4_665 . . . ? N7 Sc2 N8 C20 137.7(6) . . . . ? H2A Sc2 N8 C20 -52.8 . . . . ? N5 Sc2 N8 C20 41.8(6) 4_665 . . . ? N5 Sc2 N8 C20 -103.5(6) . . . . ? H2B Sc2 N8 C20 -25.5 . . . . ? N6 Sc2 N8 C20 -169.4(6) . . . . ? Sc2 Sc2 N8 C20 -65.0(6) 3_655 . . . ? Sc2 Sc2 N8 C20 -6.0(6) 4_665 . . . ? N7 Sc2 N8 C16 27.7(5) . . . . ? H2A Sc2 N8 C16 -162.8 . . . . ? N5 Sc2 N8 C16 -68.2(5) 4_665 . . . ? N5 Sc2 N8 C16 146.5(5) . . . . ? H2B Sc2 N8 C16 -135.5 . . . . ? N6 Sc2 N8 C16 80.5(5) . . . . ? Sc2 Sc2 N8 C16 -175.0(5) 3_655 . . . ? Sc2 Sc2 N8 C16 -116.0(5) 4_665 . . . ? C18 N5 C11 C12 -93.6(5) . . . . ? Sc2 N5 C11 C12 135.1(3) 3_655 . . . ? Sc2 N5 C11 C12 31.0(4) . . . . ? C19 N6 C12 C11 -80.4(4) . . . . ? C13 N6 C12 C11 164.3(4) . . . . ? Sc2 N6 C12 C11 53.3(4) . . . . ? N5 C11 C12 N6 -62.3(5) . . . . ? C19 N6 C13 C14 177.2(4) . . . . ? C12 N6 C13 C14 -65.2(5) . . . . ? Sc2 N6 C13 C14 41.3(4) . . . . ? C15 N7 C14 C13 173.4(4) . . . . ? Sc2 N7 C14 C13 15.3(5) . . . . ? N6 C13 C14 N7 -38.5(5) . . . . ? C14 N7 C15 C16 -165.2(6) . . . . ? Sc2 N7 C15 C16 -6.4(7) . . . . ? N7 C15 C16 N8 34.6(9) . . . . ? C17 N8 C16 C15 66.3(8) . . . . ? C20 N8 C16 C15 -172.1(7) . . . . ? Sc2 N8 C16 C15 -41.4(8) . . . . ? C20 N8 C17 C18 89.5(7) . . . . ? C16 N8 C17 C18 -160.7(5) . . . . ? Sc2 N8 C17 C18 -50.6(6) . . . . ? C11 N5 C18 C17 104.7(6) . . . . ? Sc2 N5 C18 C17 -125.2(5) 3_655 . . . ? Sc2 N5 C18 C17 -18.5(6) . . . . ? N8 C17 C18 N5 51.6(7) . . . . ? N11 Sc3 N9 C28 -53.0(4) . . . . ? H3A Sc3 N9 C28 90.6 . . . . ? N9 Sc3 N9 C28 133.9(4) 4_765 . . . ? H3B Sc3 N9 C28 160.5 . . . . ? N10 Sc3 N9 C28 -119.8(4) . . . . ? N12 Sc3 N9 C28 11.9(4) . . . . ? Sc3 Sc3 N9 C28 121.2(4) 3_645 . . . ? Sc3 Sc3 N9 C28 125.0(4) 4_765 . . . ? N11 Sc3 N9 C21 70.6(3) . . . . ? H3A Sc3 N9 C21 -145.8 . . . . ? N9 Sc3 N9 C21 -102.5(4) 4_765 . . . ? H3B Sc3 N9 C21 -76.0 . . . . ? N10 Sc3 N9 C21 3.8(3) . . . . ? N12 Sc3 N9 C21 135.5(3) . . . . ? Sc3 Sc3 N9 C21 -115.2(3) 3_645 . . . ? Sc3 Sc3 N9 C21 -111.4(3) 4_765 . . . ? N11 Sc3 N9 Sc3 -174.20(17) . . . 3_645 ? H3A Sc3 N9 Sc3 -30.5 . . . 3_645 ? N9 Sc3 N9 Sc3 12.7(5) 4_765 . . 3_645 ? H3B Sc3 N9 Sc3 39.3 . . . 3_645 ? N10 Sc3 N9 Sc3 119.01(17) . . . 3_645 ? N12 Sc3 N9 Sc3 -109.30(18) . . . 3_645 ? Sc3 Sc3 N9 Sc3 3.85(16) 4_765 . . 3_645 ? N11 Sc3 N10 C29 147.3(4) . . . . ? H3A Sc3 N10 C29 -42.6 . . . . ? N9 Sc3 N10 C29 -95.1(4) . . . . ? N9 Sc3 N10 C29 49.8(4) 4_765 . . . ? H3B Sc3 N10 C29 -18.8 . . . . ? N12 Sc3 N10 C29 -158.4(4) . . . . ? Sc3 Sc3 N10 C29 -57.7(4) 3_645 . . . ? Sc3 Sc3 N10 C29 3.9(4) 4_765 . . . ? N11 Sc3 N10 C22 -92.1(3) . . . . ? H3A Sc3 N10 C22 78.0 . . . . ? N9 Sc3 N10 C22 25.5(3) . . . . ? N9 Sc3 N10 C22 170.4(3) 4_765 . . . ? H3B Sc3 N10 C22 101.8 . . . . ? N12 Sc3 N10 C22 -37.8(3) . . . . ? Sc3 Sc3 N10 C22 62.9(3) 3_645 . . . ? Sc3 Sc3 N10 C22 124.5(2) 4_765 . . . ? N11 Sc3 N10 C23 22.7(3) . . . . ? H3A Sc3 N10 C23 -167.2 . . . . ? N9 Sc3 N10 C23 140.3(3) . . . . ? N9 Sc3 N10 C23 -74.8(3) 4_765 . . . ? H3B Sc3 N10 C23 -143.4 . . . . ? N12 Sc3 N10 C23 77.0(3) . . . . ? Sc3 Sc3 N10 C23 177.7(3) 3_645 . . . ? Sc3 Sc3 N10 C23 -120.7(3) 4_765 . . . ? H3A Sc3 N11 C24 -172.0 . . . . ? N9 Sc3 N11 C24 -72.7(4) . . . . ? N9 Sc3 N11 C24 103.3(4) 4_765 . . . ? H3B Sc3 N11 C24 23.5 . . . . ? N10 Sc3 N11 C24 -2.5(4) . . . . ? N12 Sc3 N11 C24 -139.1(4) . . . . ? Sc3 Sc3 N11 C24 -82.1(5) 3_645 . . . ? Sc3 Sc3 N11 C24 110.6(4) 4_765 . . . ? H3A Sc3 N11 C25 -16.2 . . . . ? N9 Sc3 N11 C25 83.1(4) . . . . ? N9 Sc3 N11 C25 -100.9(4) 4_765 . . . ? H3B Sc3 N11 C25 179.3 . . . . ? N10 Sc3 N11 C25 153.3(4) . . . . ? N12 Sc3 N11 C25 16.7(4) . . . . ? Sc3 Sc3 N11 C25 73.7(5) 3_645 . . . ? Sc3 Sc3 N11 C25 -93.6(4) 4_765 . . . ? N11 Sc3 N12 C30B -133.6(11) . . . . ? H3A Sc3 N12 C30B 27.3 . . . . ? N9 Sc3 N12 C30B 107.3(11) . . . . ? N9 Sc3 N12 C30B -39.0(11) 4_765 . . . ? H3B Sc3 N12 C30B 60.0 . . . . ? N10 Sc3 N12 C30B 172.0(11) . . . . ? Sc3 Sc3 N12 C30B 67.2(11) 3_645 . . . ? Sc3 Sc3 N12 C30B 9.6(11) 4_765 . . . ? N11 Sc3 N12 C27B 84.1(6) . . . . ? H3A Sc3 N12 C27B -115.0 . . . . ? N9 Sc3 N12 C27B -34.9(6) . . . . ? N9 Sc3 N12 C27B 178.7(6) 4_765 . . . ? H3B Sc3 N12 C27B -82.3 . . . . ? N10 Sc3 N12 C27B 29.7(7) . . . . ? Sc3 Sc3 N12 C27B -75.1(6) 3_645 . . . ? Sc3 Sc3 N12 C27B -132.7(6) 4_765 . . . ? N11 Sc3 N12 C30A -109.9(6) . . . . ? H3A Sc3 N12 C30A 51.0 . . . . ? N9 Sc3 N12 C30A 131.0(6) . . . . ? N9 Sc3 N12 C30A -15.3(6) 4_765 . . . ? H3B Sc3 N12 C30A 83.6 . . . . ? N10 Sc3 N12 C30A -164.3(6) . . . . ? Sc3 Sc3 N12 C30A 90.9(6) 3_645 . . . ? Sc3 Sc3 N12 C30A 33.2(6) 4_765 . . . ? N11 Sc3 N12 C26A 15.5(4) . . . . ? H3A Sc3 N12 C26A 176.4 . . . . ? N9 Sc3 N12 C26A -103.5(4) . . . . ? N9 Sc3 N12 C26A 110.1(4) 4_765 . . . ? H3B Sc3 N12 C26A -150.9 . . . . ? N10 Sc3 N12 C26A -38.9(5) . . . . ? Sc3 Sc3 N12 C26A -143.7(4) 3_645 . . . ? Sc3 Sc3 N12 C26A 158.7(4) 4_765 . . . ? N11 Sc3 N12 C27A 129.9(4) . . . . ? H3A Sc3 N12 C27A -69.2 . . . . ? N9 Sc3 N12 C27A 10.8(4) . . . . ? N9 Sc3 N12 C27A -135.5(4) 4_765 . . . ? H3B Sc3 N12 C27A -36.6 . . . . ? N10 Sc3 N12 C27A 75.5(4) . . . . ? Sc3 Sc3 N12 C27A -29.3(4) 3_645 . . . ? Sc3 Sc3 N12 C27A -87.0(4) 4_765 . . . ? N11 Sc3 N12 C26B -25.1(7) . . . . ? H3A Sc3 N12 C26B 135.7 . . . . ? N9 Sc3 N12 C26B -144.2(7) . . . . ? N9 Sc3 N12 C26B 69.5(7) 4_765 . . . ? H3B Sc3 N12 C26B 168.4 . . . . ? N10 Sc3 N12 C26B -79.5(7) . . . . ? Sc3 Sc3 N12 C26B 175.7(7) 3_645 . . . ? Sc3 Sc3 N12 C26B 118.0(7) 4_765 . . . ? C28 N9 C21 C22 90.4(5) . . . . ? Sc3 N9 C21 C22 -34.7(5) . . . . ? Sc3 N9 C21 C22 -137.5(4) 3_645 . . . ? C29 N10 C22 C21 80.5(5) . . . . ? C23 N10 C22 C21 -162.3(4) . . . . ? Sc3 N10 C22 C21 -52.4(4) . . . . ? N9 C21 C22 N10 64.3(6) . . . . ? C29 N10 C23 C24 -176.4(4) . . . . ? C22 N10 C23 C24 65.3(5) . . . . ? Sc3 N10 C23 C24 -40.2(4) . . . . ? C25 N11 C24 C23 -176.6(4) . . . . ? Sc3 N11 C24 C23 -19.0(5) . . . . ? N10 C23 C24 N11 40.1(5) . . . . ? C24 N11 C25 C26B 158.4(11) . . . . ? Sc3 N11 C25 C26B -0.4(12) . . . . ? C24 N11 C25 C26A 112.7(6) . . . . ? Sc3 N11 C25 C26A -46.2(7) . . . . ? C30B N12 C26A C25 113.0(10) . . . . ? C27B N12 C26A C25 -134.7(9) . . . . ? C30A N12 C26A C25 92.4(8) . . . . ? C27A N12 C26A C25 -152.1(6) . . . . ? C26B N12 C26A C25 44.2(11) . . . . ? Sc3 N12 C26A C25 -41.4(6) . . . . ? C26B C25 C26A N12 -56.3(13) . . . . ? N11 C25 C26A N12 56.7(7) . . . . ? C30B N12 C27A C28 -165.8(11) . . . . ? C27B N12 C27A C28 54.8(10) . . . . ? C30A N12 C27A C28 -165.3(7) . . . . ? C26A N12 C27A C28 77.7(8) . . . . ? C26B N12 C27A C28 96.7(15) . . . . ? Sc3 N12 C27A C28 -34.4(7) . . . . ? C27B N12 C27A C30B -139.4(13) . . . . ? C30A N12 C27A C30B 0.5(12) . . . . ? C26A N12 C27A C30B -116.5(10) . . . . ? C26B N12 C27A C30B -97.5(16) . . . . ? Sc3 N12 C27A C30B 131.3(9) . . . . ? N11 C25 C26B N12 -28.5(18) . . . . ? C26A C25 C26B N12 57.4(12) . . . . ? C30B N12 C26B C25 170.2(16) . . . . ? C27B N12 C26B C25 -66.1(16) . . . . ? C30A N12 C26B C25 158.5(16) . . . . ? C26A N12 C26B C25 -67.2(14) . . . . ? C27A N12 C26B C25 -95.7(18) . . . . ? Sc3 N12 C26B C25 36.4(15) . . . . ? C30B N12 C27B C28 -94.9(14) . . . . ? C30A N12 C27B C28 -109.8(12) . . . . ? C26A N12 C27B C28 156.6(12) . . . . ? C27A N12 C27B C28 -47.0(8) . . . . ? C26B N12 C27B C28 155.8(10) . . . . ? Sc3 N12 C27B C28 53.2(10) . . . . ? N12 C27A C28 N9 50.5(8) . . . . ? C30B C27A C28 N9 24(2) . . . . ? N12 C27A C28 C27B -48.1(9) . . . . ? C30B C27A C28 C27B -74(2) . . . . ? C21 N9 C28 C27A -160.6(6) . . . . ? Sc3 N9 C28 C27A -37.8(7) . . . . ? Sc3 N9 C28 C27A 69.6(6) 3_645 . . . ? C21 N9 C28 C27B -110.8(7) . . . . ? Sc3 N9 C28 C27B 12.0(8) . . . . ? Sc3 N9 C28 C27B 119.4(7) 3_645 . . . ? N12 C27B C28 C27A 53.7(9) . . . . ? N12 C27B C28 N9 -49.7(12) . . . . ? C27B N12 C30A C30B 40(4) . . . . ? C26A N12 C30A C30B 116(3) . . . . ? C27A N12 C30A C30B -1(3) . . . . ? C26B N12 C30A C30B 145(3) . . . . ? Sc3 N12 C30A C30B -120(3) . . . . ? N12 C30A C30B C27A 1(3) . . . . ? C27B N12 C30B C30A -149(3) . . . . ? C26A N12 C30B C30A -72(3) . . . . ? C27A N12 C30B C30A 179(3) . . . . ? C26B N12 C30B C30A -35(3) . . . . ? Sc3 N12 C30B C30A 74(3) . . . . ? C27B N12 C30B C27A 31.8(9) . . . . ? C30A N12 C30B C27A -179(3) . . . . ? C26A N12 C30B C27A 109.0(7) . . . . ? C26B N12 C30B C27A 146.4(8) . . . . ? Sc3 N12 C30B C27A -104.4(8) . . . . ? C28 C27A C30B C30A 33(6) . . . . ? N12 C27A C30B C30A -2(4) . . . . ? C28 C27A C30B N12 34(2) . . . . ? C36A C31A C32A C33A -0.6(10) . . . . ? S1A C31A C32A C33A 176.0(6) . . . . ? C31A C32A C33A C34A -0.9(11) . . . . ? C32A C33A C34A C35A 1.4(12) . . . . ? C33A C34A C35A C36A -0.4(12) . . . . ? C32A C31A C36A C35A 1.6(12) . . . . ? S1A C31A C36A C35A -174.7(7) . . . . ? C34A C35A C36A C31A -1.2(13) . . . . ? C40A O1A C37A C38A -12(2) . . . . ? O1A C37A C38A C39A 22.7(19) . . . . ? C37A C38A C39A C40A -28.1(18) . . . . ? C38A C39A C40A O1A 18.1(18) . . . . ? C37A O1A C40A C39A -3(2) . . . . ? C36B C31B C32B C33B 0.0 . . . . ? S1B C31B C32B C33B -175.0(14) . . . . ? C31B C32B C33B C34B 0.0 . . . . ? C32B C33B C34B C35B 0.0 . . . . ? C33B C34B C35B C36B 0.0 . . . . ? C34B C35B C36B C31B 0.0 . . . . ? C32B C31B C36B C35B 0.0 . . . . ? S1B C31B C36B C35B 175.3(13) . . . . ? C40B O1B C37B C38B 27(5) . . . . ? O1B C37B C38B C39B -20(4) . . . . ? C37B C38B C39B C40B 12(3) . . . . ? C37B O1B C40B C39B -21(5) . . . . ? C38B C39B C40B O1B 4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.901 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.095 _shelx_res_file ; TITL 4 CELL 0.71073 19.2442 19.2442 21.4089 90.000 90.000 120.000 ZERR 2.00 0.0017 0.0017 0.0019 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM - Y, X - Y, Z SYMM - X + Y, - X, Z SYMM X - Y, X, 1/2 + Z SYMM Y, - X + Y, 1/2 + Z SFAC C H N O S SC UNIT 240 486 72 6 6 18 SIZE 0.22 0.25 0.35 TEMP -176 REM colourless block L.S. 16 FMAP 2 PLAN -20 OMIT 0 1 -1 BIND SC1 H1A BIND SC1 H1B BIND SC2 H2A BIND SC2 H2B BIND SC3 H3A BIND SC3 H3B ACTA CONF REM no correction for extinction WGHT 0.107100 6.234100 FVAR 0.17974 MOLE 1 SC1 6 0.430773 0.764304 0.797105 11.00000 0.01725 0.01667 = 0.02388 -0.00080 0.00251 0.00808 AFIX 3 H1A 2 0.333335 0.666667 0.748262 10.33333 -1.20000 H1B 2 0.333335 0.666667 0.849820 10.33333 -1.20000 AFIX 0 N1 3 0.332283 0.793902 0.804919 11.00000 0.02299 0.01416 = 0.02501 0.00278 0.00067 0.00964 N2 3 0.460570 0.829236 0.898518 11.00000 0.02346 0.01729 = 0.02615 -0.00244 0.00174 0.00937 N3 3 0.543774 0.866263 0.788555 11.00000 0.02288 0.02167 = 0.03638 -0.00470 0.00711 0.00445 N4 3 0.435409 0.829515 0.696269 11.00000 0.03333 0.02983 = 0.02579 0.00406 0.00526 0.01316 C1 1 0.339653 0.832795 0.866215 11.00000 0.02521 0.02249 = 0.03748 -0.00482 0.00931 0.01421 AFIX 23 H1C 2 0.308239 0.791005 0.897690 11.00000 -1.20000 H1D 2 0.316519 0.868479 0.863051 11.00000 -1.20000 AFIX 0 C2 1 0.426713 0.881819 0.888225 11.00000 0.02703 0.01540 = 0.03285 -0.00329 0.00399 0.00661 AFIX 23 H2C 2 0.458880 0.922751 0.856406 11.00000 -1.20000 H2D 2 0.429016 0.909948 0.927559 11.00000 -1.20000 AFIX 0 C3 1 0.550737 0.876212 0.902107 11.00000 0.02292 0.02561 = 0.03702 -0.00580 -0.00557 0.01019 AFIX 23 H3C 2 0.567323 0.916194 0.936169 11.00000 -1.20000 H3D 2 0.571109 0.839362 0.912071 11.00000 -1.20000 AFIX 0 C4 1 0.586644 0.918147 0.842221 11.00000 0.02097 0.02047 = 0.04486 -0.00310 -0.00253 0.00652 AFIX 23 H4A 2 0.583824 0.968057 0.839876 11.00000 -1.20000 H4B 2 0.643854 0.933020 0.840639 11.00000 -1.20000 AFIX 0 C5 1 0.573575 0.911055 0.731280 11.00000 0.02396 0.03582 = 0.04365 0.00579 0.00820 0.00870 AFIX 23 H5A 2 0.627047 0.917823 0.722143 11.00000 -1.20000 H5B 2 0.580417 0.965147 0.737228 11.00000 -1.20000 AFIX 0 C6 1 0.521087 0.873009 0.677613 11.00000 0.06644 0.07433 = 0.06897 0.02114 0.02948 0.03567 AFIX 23 H6A 2 0.534900 0.834920 0.657944 11.00000 -1.20000 H6B 2 0.529889 0.914515 0.646325 11.00000 -1.20000 AFIX 0 C7 1 0.409614 0.884274 0.716014 11.00000 0.06196 0.05669 = 0.04941 0.02173 0.01132 0.04032 AFIX 23 H7A 2 0.402463 0.910738 0.678890 11.00000 -1.20000 H7B 2 0.451660 0.926387 0.742616 11.00000 -1.20000 AFIX 0 C8 1 0.330491 0.841650 0.752684 11.00000 0.02517 0.04082 = 0.05069 0.02300 0.01072 0.01703 AFIX 23 H8A 2 0.318021 0.882409 0.768800 11.00000 -1.20000 H8B 2 0.286777 0.806196 0.723857 11.00000 -1.20000 AFIX 0 C9 1 0.432875 0.789610 0.958705 11.00000 0.04059 0.03029 = 0.03032 -0.00637 0.00088 0.01728 AFIX 137 H9A 2 0.451602 0.830040 0.991917 11.00000 -1.50000 H9B 2 0.454277 0.753526 0.965721 11.00000 -1.50000 H9C 2 0.374104 0.758591 0.958991 11.00000 -1.50000 AFIX 0 C10 1 0.396078 0.790899 0.637915 11.00000 0.17035 0.07132 = 0.02552 -0.00065 -0.00421 0.04623 AFIX 137 H10A 2 0.396769 0.831065 0.609386 11.00000 -1.50000 H10B 2 0.340425 0.749597 0.646384 11.00000 -1.50000 H10C 2 0.424590 0.766064 0.618729 11.00000 -1.50000 AFIX 0 MOLE 2 SC2 6 0.672916 0.434766 0.803863 11.00000 0.01611 0.01595 = 0.01881 0.00014 0.00048 0.00769 AFIX 3 H2A 2 0.666667 0.333337 0.856831 10.33333 -1.20000 H2B 2 0.666667 0.333337 0.747342 10.33333 -1.20000 AFIX 0 N5 3 0.543330 0.340772 0.805918 11.00000 0.01784 0.01823 = 0.02347 -0.00060 -0.00257 0.00909 N6 3 0.632357 0.460236 0.904964 11.00000 0.02616 0.02938 = 0.02320 -0.00084 0.00302 0.01861 N7 3 0.689878 0.551199 0.800951 11.00000 0.03092 0.02075 = 0.03228 0.00540 0.00158 0.01549 N8 3 0.624122 0.451482 0.702598 11.00000 0.04605 0.03296 = 0.02524 0.00698 0.00214 0.02589 C11 1 0.507751 0.346231 0.866194 11.00000 0.02268 0.02209 = 0.05111 0.00298 0.01546 0.01361 AFIX 23 H11A 2 0.513130 0.311128 0.897287 11.00000 -1.20000 H11B 2 0.449792 0.326222 0.860057 11.00000 -1.20000 AFIX 0 C12 1 0.546981 0.430723 0.891592 11.00000 0.02861 0.02522 = 0.02778 0.00287 0.00512 0.01930 AFIX 23 H12A 2 0.542149 0.466358 0.860700 11.00000 -1.20000 H12B 2 0.519335 0.431554 0.930344 11.00000 -1.20000 AFIX 0 C13 1 0.677024 0.549606 0.912971 11.00000 0.03106 0.02988 = 0.03586 -0.01779 -0.01074 0.01572 AFIX 23 H13A 2 0.650908 0.564341 0.946151 11.00000 -1.20000 H13B 2 0.732596 0.567262 0.926535 11.00000 -1.20000 AFIX 0 C14 1 0.679363 0.592254 0.854078 11.00000 0.02374 0.02144 = 0.04177 -0.00659 -0.00433 0.01087 AFIX 23 H14A 2 0.628746 0.593362 0.849395 11.00000 -1.20000 H14B 2 0.724282 0.648323 0.855788 11.00000 -1.20000 AFIX 0 C15 1 0.682819 0.586923 0.743313 11.00000 0.02958 0.02317 = 0.05132 0.01167 -0.00877 0.00675 AFIX 23 H15A 2 0.636593 0.595889 0.746769 11.00000 -1.20000 H15B 2 0.731752 0.639888 0.737736 11.00000 -1.20000 AFIX 0 C16 1 0.672339 0.539278 0.689985 11.00000 0.12588 0.04918 = 0.06782 0.00373 -0.03510 0.03975 AFIX 23 H16A 2 0.725710 0.552027 0.674007 11.00000 -1.20000 H16B 2 0.645439 0.553294 0.656965 11.00000 -1.20000 AFIX 0 C17 1 0.543463 0.427217 0.717908 11.00000 0.04393 0.06098 = 0.04667 0.01219 -0.00776 0.02213 AFIX 23 H17A 2 0.513892 0.423575 0.679074 11.00000 -1.20000 H17B 2 0.542632 0.468648 0.744798 11.00000 -1.20000 AFIX 0 C18 1 0.500398 0.346415 0.751692 11.00000 0.03141 0.02608 = 0.05224 0.00902 -0.02061 0.00507 AFIX 23 H18A 2 0.447039 0.336411 0.765412 11.00000 -1.20000 H18B 2 0.491662 0.303594 0.721735 11.00000 -1.20000 AFIX 0 C19 1 0.639169 0.428226 0.965034 11.00000 0.04411 0.05573 = 0.02107 -0.00156 0.00126 0.03527 AFIX 137 H19A 2 0.616980 0.370137 0.961493 11.00000 -1.50000 H19B 2 0.609312 0.439303 0.996795 11.00000 -1.50000 H19C 2 0.695787 0.453752 0.977139 11.00000 -1.50000 AFIX 0 C20 1 0.636965 0.424802 0.641845 11.00000 0.09356 0.14545 = 0.02074 0.00588 0.00721 0.08940 AFIX 137 H20A 2 0.601976 0.428991 0.610642 11.00000 -1.50000 H20B 2 0.624390 0.368885 0.644908 11.00000 -1.50000 H20C 2 0.693126 0.458671 0.629316 11.00000 -1.50000 AFIX 0 MOLE 3 SC3 6 0.928825 0.040211 0.843008 11.00000 0.02001 0.01987 = 0.03576 -0.00244 -0.00095 0.01054 AFIX 3 H3A 2 0.999992 -0.000011 0.897790 10.33333 -1.20000 H3B 2 0.999992 -0.000011 0.780379 10.33333 -1.20000 AFIX 0 N9 3 0.854569 -0.092893 0.837641 11.00000 0.02381 0.02555 = 0.03934 -0.00021 0.00433 0.01194 N10 3 0.864815 0.023024 0.741207 11.00000 0.02377 0.03334 = 0.03900 -0.00067 -0.00183 0.01415 N11 3 0.860031 0.094432 0.848960 11.00000 0.03646 0.03345 = 0.04418 -0.00137 0.00131 0.02290 N12 3 0.858317 0.000253 0.945945 11.00000 0.03726 0.04277 = 0.04232 -0.00594 0.00365 0.02225 C21 1 0.814329 -0.115917 0.775901 11.00000 0.02882 0.02529 = 0.05764 -0.01278 -0.00757 0.01622 AFIX 23 H21A 2 0.765519 -0.169405 0.779244 11.00000 -1.20000 H21B 2 0.850743 -0.119953 0.745323 11.00000 -1.20000 AFIX 0 C22 1 0.791458 -0.056649 0.752600 11.00000 0.02173 0.03215 = 0.04961 -0.01179 -0.00627 0.01294 AFIX 23 H22A 2 0.760579 -0.076626 0.713307 11.00000 -1.20000 H22B 2 0.756877 -0.050618 0.783812 11.00000 -1.20000 AFIX 0 C23 1 0.844509 0.088673 0.737396 11.00000 0.03271 0.02770 = 0.04748 0.00222 -0.00859 0.01742 AFIX 23 H23A 2 0.892992 0.139269 0.725038 11.00000 -1.20000 H23B 2 0.803282 0.075126 0.704715 11.00000 -1.20000 AFIX 0 C24 1 0.813985 0.100984 0.797902 11.00000 0.02529 0.02479 = 0.05970 -0.00194 -0.00087 0.01389 AFIX 23 H24A 2 0.818832 0.154676 0.798483 11.00000 -1.20000 H24B 2 0.756607 0.060151 0.802809 11.00000 -1.20000 AFIX 0 C25 1 0.828768 0.101377 0.909289 11.00000 0.05573 0.03436 = 0.06593 -0.00204 0.01913 0.03090 PART 1 AFIX 3 H25A 2 0.787053 0.116553 0.903390 10.50000 -1.20000 H25B 2 0.872504 0.143175 0.934943 10.50000 -1.20000 AFIX 3 PART 2 H25C 2 0.848847 0.159036 0.917151 10.50000 -1.20000 H25D 2 0.769644 0.074889 0.905763 10.50000 -1.20000 AFIX 0 PART 1 C26A 1 0.793057 0.019874 0.942084 10.50000 0.02455 AFIX 23 H26A 2 0.774000 0.022878 0.984409 10.50000 -1.20000 H26B 2 0.747232 -0.021664 0.917887 10.50000 -1.20000 AFIX 0 C27A 1 0.820832 -0.091621 0.946744 10.50000 0.02451 AFIX 23 H27A 2 0.860737 -0.104853 0.963585 10.50000 -1.20000 H27B 2 0.774277 -0.114685 0.975465 10.50000 -1.20000 AFIX 0 PART 2 C26B 1 0.844304 0.073446 0.956406 10.50000 0.07672 AFIX 23 H26C 2 0.799606 0.056663 0.986450 10.50000 -1.20000 H26D 2 0.893010 0.117246 0.976285 10.50000 -1.20000 AFIX 0 C27B 1 0.784832 -0.065116 0.926039 10.50000 0.05799 AFIX 23 H27C 2 0.756342 -0.044846 0.899887 10.50000 -1.20000 H27D 2 0.751029 -0.091646 0.963066 10.50000 -1.20000 AFIX 0 PART 0 C28 1 0.795445 -0.127827 0.888181 11.00000 0.03334 0.03208 = 0.07190 0.00603 0.02272 0.01430 PART 1 AFIX 3 H28A 2 0.747188 -0.125250 0.875898 10.50000 -1.20000 H28B 2 0.779286 -0.185197 0.892309 10.50000 -1.20000 AFIX 3 PART 2 H28C 2 0.811785 -0.157391 0.916924 10.50000 -1.20000 H28D 2 0.742942 -0.167007 0.869938 10.50000 -1.20000 AFIX 0 PART 0 C29 1 0.899136 0.020527 0.679892 11.00000 0.03319 0.05391 = 0.03580 -0.00412 -0.00183 0.02075 AFIX 137 H29A 2 0.943642 0.074060 0.669671 11.00000 -1.50000 H29B 2 0.857609 0.003404 0.647648 11.00000 -1.50000 H29C 2 0.918866 -0.017534 0.681784 11.00000 -1.50000 AFIX 0 PART 1 C30A 1 0.900183 0.029646 1.006101 10.50000 0.03146 AFIX 33 H30A 2 0.872084 0.047992 1.033830 10.50000 -1.50000 H30B 2 0.894014 0.041840 0.962700 10.50000 -1.50000 H30C 2 0.957290 0.057146 1.016976 10.50000 -1.50000 AFIX 0 PART 0 C30B 1 0.888006 -0.001304 1.008660 10.50000 0.08445 AFIX 33 H30D 2 0.931168 -0.014279 1.007419 10.50000 -1.50000 H30E 2 0.850119 -0.029210 0.974592 10.50000 -1.50000 H30F 2 0.859892 -0.018465 1.048768 10.50000 -1.50000 AFIX 0 PART 0 MOLE 4 PART 1 S1A 5 0.442337 0.995712 0.545922 10.70000 0.03815 C31A 1 0.341094 0.946278 0.564573 10.70000 0.03469 C32A 1 0.289787 0.866521 0.541512 10.70000 0.02786 AFIX 43 H32A 2 0.311563 0.843408 0.514169 10.70000 -1.20000 AFIX 0 C33A 1 0.205729 0.820067 0.558624 10.70000 0.03513 AFIX 43 H33A 2 0.173598 0.767751 0.541842 10.70000 -1.20000 AFIX 0 C34A 1 0.171817 0.850525 0.598732 10.70000 0.04276 AFIX 43 H34A 2 0.117083 0.819825 0.610759 10.70000 -1.20000 AFIX 0 C35A 1 0.220989 0.928440 0.621145 10.70000 0.04357 AFIX 43 H35A 2 0.199097 0.951203 0.648722 10.70000 -1.20000 AFIX 0 C36A 1 0.301940 0.973700 0.603780 10.70000 0.04122 AFIX 43 H36A 2 0.332216 1.026675 0.619806 10.70000 -1.20000 AFIX 0 O1A 4 0.671923 1.064552 0.526000 10.70000 0.22805 C37A 1 0.737695 1.157375 0.539485 10.70000 0.14969 AFIX 23 H37A 2 0.764452 1.187189 0.500933 10.70000 -1.20000 H37B 2 0.715040 1.185933 0.562763 10.70000 -1.20000 AFIX 0 C38A 1 0.792506 1.139518 0.579899 10.70000 0.08599 AFIX 23 H38A 2 0.849157 1.180432 0.571806 10.70000 -1.20000 H38B 2 0.781120 1.142900 0.624545 10.70000 -1.20000 AFIX 0 C39A 1 0.781456 1.063915 0.567489 10.70000 0.04859 AFIX 23 H39A 2 0.820489 1.068384 0.535362 10.70000 -1.20000 H39B 2 0.791868 1.041991 0.605933 10.70000 -1.20000 AFIX 0 C40A 1 0.704342 1.011702 0.546647 10.70000 0.09653 AFIX 23 H40A 2 0.671143 0.975446 0.580681 10.70000 -1.20000 H40B 2 0.705262 0.978880 0.511394 10.70000 -1.20000 AFIX 0 PART 2 S1B 5 0.529711 1.015010 0.551454 10.30000 0.04669 AFIX 66 C31B 1 0.640746 1.056800 0.558258 10.30000 0.05578 C32B 1 0.695902 1.137903 0.550713 10.30000 0.06292 AFIX 43 H32B 2 0.677729 1.175175 0.545012 10.30000 -1.20000 AFIX 65 C33B 1 0.777647 1.164472 0.551509 10.30000 0.04996 AFIX 43 H33B 2 0.815344 1.219903 0.546351 10.30000 -1.20000 AFIX 65 C34B 1 0.804237 1.109939 0.559850 10.30000 0.08854 AFIX 43 H34B 2 0.860106 1.128098 0.560394 10.30000 -1.20000 AFIX 65 C35B 1 0.749081 1.028835 0.567395 10.30000 0.09769 AFIX 43 H35B 2 0.767254 0.991564 0.573096 10.30000 -1.20000 AFIX 65 C36B 1 0.667336 1.002265 0.566600 10.30000 0.06483 AFIX 43 H36B 2 0.629639 0.946834 0.571757 10.30000 -1.20000 AFIX 0 O1B 4 0.312075 0.912193 0.550297 10.30000 0.13694 C37B 1 0.325869 0.990401 0.567210 10.30000 0.11636 AFIX 23 H37C 2 0.314841 1.017719 0.532660 10.30000 -1.20000 H37D 2 0.380127 1.025657 0.584558 10.30000 -1.20000 AFIX 0 C38B 1 0.262158 0.958337 0.615699 10.30000 0.03246 AFIX 23 H38C 2 0.287276 0.965532 0.657326 10.30000 -1.20000 H38D 2 0.233901 0.989453 0.615003 10.30000 -1.20000 AFIX 0 C39B 1 0.206413 0.877180 0.606820 10.30000 0.06368 AFIX 23 H39C 2 0.154529 0.870103 0.592004 10.30000 -1.20000 H39D 2 0.197333 0.846753 0.646151 10.30000 -1.20000 AFIX 0 C40B 1 0.244365 0.849155 0.557250 10.30000 0.06061 AFIX 23 H40C 2 0.250107 0.803670 0.572385 10.30000 -1.20000 H40D 2 0.212996 0.833649 0.517982 10.30000 -1.20000 HKLF 4 1 1 0 0 0 1 0 0 0 1 1.8 REM c13_a52 in P6(3)/m REM R1 = 0.0665 for 8291 Fo > 4sig(Fo) and 0.0743 for all 9437 data REM 492 parameters refined using 1 restraints END WGHT 0.1060 6.4682 REM Highest difference peak 1.901, deepest hole -0.633, 1-sigma level 0.095 Q1 1 0.4739 0.4725 0.0454 11.00000 0.05 1.90 Q2 1 0.5332 0.3722 0.6993 11.00000 0.05 1.47 Q3 1 0.6095 0.5203 0.7090 11.00000 0.05 1.38 Q4 1 0.3595 0.8329 0.6986 11.00000 0.05 1.20 Q5 1 0.5081 0.9121 0.7068 11.00000 0.05 1.10 Q6 1 0.5286 0.3683 0.9034 11.00000 0.05 0.74 Q7 1 0.3715 0.8374 0.9006 11.00000 0.05 0.69 Q8 1 0.6034 0.5158 0.8953 11.00000 0.05 0.66 Q9 1 0.5883 1.0111 0.5511 11.00000 0.05 0.65 Q10 1 0.7161 1.1316 0.5749 11.00000 0.05 0.65 Q11 1 -0.0013 0.4718 0.1469 11.00000 0.05 0.62 Q12 1 0.4495 0.8090 0.6369 11.00000 0.05 0.58 Q13 1 0.6768 1.1044 0.5532 11.00000 0.05 0.58 Q14 1 0.5144 0.9093 0.8924 11.00000 0.05 0.56 Q15 1 0.7682 1.1335 0.4895 11.00000 0.05 0.48 Q16 1 0.7619 0.4586 0.8001 11.00000 0.05 0.42 Q17 1 0.8924 -0.0749 0.8045 11.00000 0.05 0.41 Q18 1 0.9262 0.0417 0.7997 11.00000 0.05 0.41 Q19 1 0.7189 1.0658 0.5944 11.00000 0.05 0.40 Q20 1 0.7201 1.0594 0.4960 11.00000 0.05 0.39 ; #==END _database_code_depnum_ccdc_archive 'CCDC 961426'