# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_p _database_code_depnum_ccdc_archive 'CCDC 881895' #TrackingRef '101109qx-submit-cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H106 Er N27 O38' _chemical_formula_weight 1980.98 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.9051(13) _cell_length_b 15.9844(13) _cell_length_c 18.1694(15) _cell_angle_alpha 74.805(3) _cell_angle_beta 89.245(3) _cell_angle_gamma 63.414(2) _cell_volume 3957.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2054 _exptl_absorpt_coefficient_mu 1.174 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7124 _exptl_absorpt_correction_T_max 0.7907 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38687 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.10 _reflns_number_total 13786 _reflns_number_gt 12748 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0770P)^2^+9.9705P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13786 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1257 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 O1W O 0.2416(2) 0.0524(2) 0.28516(16) 0.0247(6) Uani 1 1 d . . . O2W O 0.1057(2) 0.3787(2) 0.24602(17) 0.0247(6) Uani 1 1 d . . . O3W O 0.0605(2) 0.2256(2) 0.26606(17) 0.0263(6) Uani 1 1 d . . . O4W O 0.3755(2) 0.1181(2) 0.27341(18) 0.0278(7) Uani 1 1 d . . . Er1 Er 0.214665(12) 0.215979(12) 0.263465(9) 0.01920(8) Uani 1 1 d . . . C1 C 0.1892(3) 0.1680(3) 0.4594(2) 0.0134(7) Uani 1 1 d . . . C2 C 0.1702(3) 0.1232(3) 0.5896(2) 0.0150(7) Uani 1 1 d . . . C3 C 0.1652(3) 0.2273(3) 0.5666(2) 0.0159(8) Uani 1 1 d . . . C4 C 0.2964(3) 0.1185(3) 0.6605(2) 0.0176(8) Uani 1 1 d . . . C5 C 0.1630(3) 0.3374(3) 0.4339(2) 0.0142(7) Uani 1 1 d . . . H5A H 0.1173 0.3915 0.4517 0.017 Uiso 1 1 calc R . . H5B H 0.1376 0.3456 0.3822 0.017 Uiso 1 1 calc R . . C6 C 0.2736(3) 0.2880(3) 0.6161(2) 0.0210(8) Uani 1 1 d . . . H6A H 0.2149 0.3477 0.6129 0.025 Uiso 1 1 calc R . . H6B H 0.3097 0.2684 0.6663 0.025 Uiso 1 1 calc R . . C7 C 0.3086(3) 0.3149(3) 0.3752(2) 0.0147(7) Uani 1 1 d . . . C8 C 0.2891(3) 0.3787(3) 0.4804(2) 0.0144(7) Uani 1 1 d . . . C9 C 0.3804(3) 0.3768(3) 0.4439(2) 0.0143(7) Uani 1 1 d . . . C10 C 0.4237(3) 0.2783(3) 0.5724(2) 0.0185(8) Uani 1 1 d . . . C11 C 0.4476(3) 0.3256(3) 0.3231(2) 0.0166(8) Uani 1 1 d . . . H11A H 0.4531 0.3863 0.3085 0.020 Uiso 1 1 calc R . . H11B H 0.4184 0.3218 0.2777 0.020 Uiso 1 1 calc R . . C12 C 0.5527(3) 0.2972(3) 0.5079(2) 0.0184(8) Uani 1 1 d . . . H12A H 0.5807 0.2770 0.5612 0.022 Uiso 1 1 calc R . . H12B H 0.5534 0.3588 0.4817 0.022 Uiso 1 1 calc R . . C13 C 0.5722(3) 0.1705(3) 0.3107(2) 0.0151(7) Uani 1 1 d . . . C14 C 0.6197(3) 0.2421(3) 0.3896(2) 0.0144(7) Uani 1 1 d . . . C15 C 0.7067(3) 0.1432(3) 0.3856(2) 0.0156(8) Uani 1 1 d . . . C16 C 0.6721(3) 0.1299(3) 0.5131(2) 0.0170(8) Uani 1 1 d . . . C17 C 0.1882(3) 0.0104(3) 0.5048(2) 0.0169(8) Uani 1 1 d . . . H17A H 0.1763 0.0221 0.4494 0.020 Uiso 1 1 calc R . . H17B H 0.1348 0.0038 0.5282 0.020 Uiso 1 1 calc R . . C18 C 0.2787(3) -0.0318(3) 0.6997(2) 0.0166(8) Uani 1 1 d . . . H18A H 0.3159 -0.0414 0.7465 0.020 Uiso 1 1 calc R . . H18B H 0.2211 -0.0361 0.7148 0.020 Uiso 1 1 calc R . . C19 C 0.0785(3) 0.1251(3) 0.6160(2) 0.0224(9) Uani 1 1 d . . . H19A H 0.0869 0.0582 0.6337 0.027 Uiso 1 1 calc R . . H19B H 0.0284 0.1612 0.5724 0.027 Uiso 1 1 calc R . . C20 C 0.0478(3) 0.1731(3) 0.6813(3) 0.0294(10) Uani 1 1 d . . . H20A H -0.0186 0.1890 0.6866 0.035 Uiso 1 1 calc R . . H20B H 0.0858 0.1263 0.7296 0.035 Uiso 1 1 calc R . . C21 C 0.0586(3) 0.2665(3) 0.6680(2) 0.0252(9) Uani 1 1 d . . . H21A H 0.0016 0.3172 0.6803 0.030 Uiso 1 1 calc R . . H21B H 0.1125 0.2533 0.7028 0.030 Uiso 1 1 calc R . . C22 C 0.0741(3) 0.3041(3) 0.5851(2) 0.0205(8) Uani 1 1 d . . . H22A H 0.0203 0.3178 0.5499 0.025 Uiso 1 1 calc R . . H22B H 0.0784 0.3648 0.5783 0.025 Uiso 1 1 calc R . . C23 C 0.2187(3) 0.4807(3) 0.4832(3) 0.0237(9) Uani 1 1 d . . . H23A H 0.2468 0.5013 0.5183 0.028 Uiso 1 1 calc R . . H23B H 0.1616 0.4795 0.5030 0.028 Uiso 1 1 calc R . . C24 C 0.1919(3) 0.5546(3) 0.4028(3) 0.0285(10) Uani 1 1 d . . . H24A H 0.1497 0.5438 0.3718 0.034 Uiso 1 1 calc R . . H24B H 0.1570 0.6208 0.4077 0.034 Uiso 1 1 calc R . . C25 C 0.2782(3) 0.5465(3) 0.3612(3) 0.0290(10) Uani 1 1 d . . . H25A H 0.2740 0.6116 0.3414 0.035 Uiso 1 1 calc R . . H25B H 0.2774 0.5221 0.3172 0.035 Uiso 1 1 calc R . . C26 C 0.3719(3) 0.4787(3) 0.4129(2) 0.0224(9) Uani 1 1 d . . . H26A H 0.4248 0.4758 0.3836 0.027 Uiso 1 1 calc R . . H26B H 0.3749 0.5043 0.4558 0.027 Uiso 1 1 calc R . . C27 C 0.6370(3) 0.3301(3) 0.3572(2) 0.0220(8) Uani 1 1 d . . . H27A H 0.6843 0.3283 0.3924 0.026 Uiso 1 1 calc R . . H27B H 0.5781 0.3901 0.3526 0.026 Uiso 1 1 calc R . . C28 C 0.6718(3) 0.3309(3) 0.2784(3) 0.0271(9) Uani 1 1 d . . . H28A H 0.6819 0.3885 0.2586 0.033 Uiso 1 1 calc R . . H28B H 0.6230 0.3357 0.2428 0.033 Uiso 1 1 calc R . . C29 C 0.7641(3) 0.2392(3) 0.2814(3) 0.0319(10) Uani 1 1 d . . . H29A H 0.8155 0.2572 0.2723 0.038 Uiso 1 1 calc R . . H29B H 0.7577 0.2128 0.2400 0.038 Uiso 1 1 calc R . . C30 C 0.7908(3) 0.1595(3) 0.3581(2) 0.0227(9) Uani 1 1 d . . . H30A H 0.8412 0.0983 0.3524 0.027 Uiso 1 1 calc R . . H30B H 0.8156 0.1779 0.3969 0.027 Uiso 1 1 calc R . . C31 C 0.1861(3) 0.1845(3) 0.0829(2) 0.0146(7) Uani 1 1 d . . . C32 C 0.1619(3) 0.1558(3) -0.0329(2) 0.0171(8) Uani 1 1 d . . . C33 C 0.2577(3) 0.1613(3) -0.0281(2) 0.0165(8) Uani 1 1 d . . . C34 C 0.1530(3) 0.2890(3) -0.1321(2) 0.0205(8) Uani 1 1 d . . . C35 C 0.3448(3) 0.1745(3) 0.0835(2) 0.0166(8) Uani 1 1 d . . . H35A H 0.3489 0.1493 0.1393 0.020 Uiso 1 1 calc R . . H35B H 0.4025 0.1300 0.0669 0.020 Uiso 1 1 calc R . . C36 C 0.3092(3) 0.2822(3) -0.1150(2) 0.0224(9) Uani 1 1 d . . . H36A H 0.2924 0.3180 -0.1698 0.027 Uiso 1 1 calc R . . H36B H 0.3713 0.2253 -0.1090 0.027 Uiso 1 1 calc R . . C37 C 0.3012(3) 0.3305(3) 0.1103(2) 0.0152(8) Uani 1 1 d . . . C38 C 0.3762(3) 0.3124(3) -0.0001(2) 0.0165(8) Uani 1 1 d . . . C39 C 0.3602(3) 0.4116(3) 0.0136(2) 0.0162(8) Uani 1 1 d . . . C40 C 0.2801(3) 0.4437(3) -0.1061(2) 0.0187(8) Uani 1 1 d . . . C41 C 0.2915(3) 0.4811(3) 0.1270(2) 0.0171(8) Uani 1 1 d . . . H41A H 0.3465 0.4933 0.1287 0.021 Uiso 1 1 calc R . . H41B H 0.2861 0.4498 0.1798 0.021 Uiso 1 1 calc R . . C42 C 0.2725(3) 0.5871(3) -0.0765(2) 0.0196(8) Uani 1 1 d . . . H42A H 0.2557 0.6141 -0.1323 0.023 Uiso 1 1 calc R . . H42B H 0.3267 0.5961 -0.0630 0.023 Uiso 1 1 calc R . . C43 C 0.1308(3) 0.5996(3) 0.1394(2) 0.0190(8) Uani 1 1 d . . . C44 C 0.2004(3) 0.6569(3) 0.0355(2) 0.0178(8) Uani 1 1 d . . . C45 C 0.0987(3) 0.7406(3) 0.0375(2) 0.0169(8) Uani 1 1 d . . . C46 C 0.1038(3) 0.7005(3) -0.0792(2) 0.0178(8) Uani 1 1 d . . . C47 C 0.0448(3) 0.1625(3) 0.0681(2) 0.0179(8) Uani 1 1 d . . . H47A H 0.0511 0.1517 0.1239 0.022 Uiso 1 1 calc R . . H47B H 0.0476 0.1037 0.0588 0.022 Uiso 1 1 calc R . . C48 C 0.0172(3) 0.2551(3) -0.1390(2) 0.0206(8) Uani 1 1 d . . . H48A H 0.0091 0.2939 -0.1925 0.025 Uiso 1 1 calc R . . H48B H 0.0207 0.1925 -0.1398 0.025 Uiso 1 1 calc R . . C49 C 0.1775(3) 0.0561(3) -0.0388(3) 0.0281(10) Uani 1 1 d . . . H49A H 0.1162 0.0569 -0.0459 0.034 Uiso 1 1 calc R . . H49B H 0.2128 0.0057 0.0090 0.034 Uiso 1 1 calc R . . C50 C 0.2327(4) 0.0313(4) -0.1064(3) 0.0429(13) Uani 1 1 d . . . H50A H 0.2521 -0.0372 -0.1030 0.052 Uiso 1 1 calc R . . H50B H 0.1906 0.0716 -0.1545 0.052 Uiso 1 1 calc R . . C51 C 0.3202(4) 0.0472(4) -0.1092(3) 0.0394(12) Uani 1 1 d . . . H51A H 0.3103 0.1018 -0.1542 0.047 Uiso 1 1 calc R . . H51B H 0.3745 -0.0113 -0.1152 0.047 Uiso 1 1 calc R . . C52 C 0.3430(3) 0.0692(3) -0.0368(3) 0.0246(9) Uani 1 1 d . . . H52A H 0.3993 0.0796 -0.0411 0.030 Uiso 1 1 calc R . . H52B H 0.3561 0.0139 0.0085 0.030 Uiso 1 1 calc R . . C53 C 0.4810(3) 0.2460(3) -0.0046(2) 0.0232(9) Uani 1 1 d . . . H53A H 0.5016 0.2771 -0.0501 0.028 Uiso 1 1 calc R . . H53B H 0.4882 0.1837 -0.0099 0.028 Uiso 1 1 calc R . . C54 C 0.5438(3) 0.2268(3) 0.0677(3) 0.0301(10) Uani 1 1 d . . . H54A H 0.5344 0.1813 0.1109 0.036 Uiso 1 1 calc R . . H54B H 0.6104 0.1959 0.0590 0.036 Uiso 1 1 calc R . . C55 C 0.5218(3) 0.3205(3) 0.0891(3) 0.0271(9) Uani 1 1 d . . . H55A H 0.4942 0.3183 0.1377 0.033 Uiso 1 1 calc R . . H55B H 0.5810 0.3237 0.0969 0.033 Uiso 1 1 calc R . . C56 C 0.4535(3) 0.4126(3) 0.0277(2) 0.0226(9) Uani 1 1 d . . . H56A H 0.4418 0.4701 0.0442 0.027 Uiso 1 1 calc R . . H56B H 0.4822 0.4172 -0.0203 0.027 Uiso 1 1 calc R . . C57 C 0.2783(3) 0.6850(3) 0.0466(3) 0.0238(9) Uani 1 1 d . . . H57A H 0.2745 0.7360 0.0009 0.029 Uiso 1 1 calc R . . H57B H 0.3402 0.6280 0.0525 0.029 Uiso 1 1 calc R . . C58 C 0.2697(3) 0.7221(3) 0.1172(3) 0.0320(10) Uani 1 1 d . . . H58A H 0.3179 0.7439 0.1202 0.038 Uiso 1 1 calc R . . H58B H 0.2820 0.6683 0.1635 0.038 Uiso 1 1 calc R . . C59 C 0.1711(3) 0.8072(4) 0.1151(3) 0.0327(11) Uani 1 1 d . . . H59A H 0.1440 0.7902 0.1620 0.039 Uiso 1 1 calc R . . H59B H 0.1781 0.8652 0.1145 0.039 Uiso 1 1 calc R . . C60 C 0.1024(3) 0.8316(3) 0.0448(3) 0.0242(9) Uani 1 1 d . . . H60A H 0.0389 0.8798 0.0498 0.029 Uiso 1 1 calc R . . H60B H 0.1230 0.8604 -0.0018 0.029 Uiso 1 1 calc R . . N1 N 0.1917(2) 0.0946(2) 0.51826(17) 0.0145(6) Uani 1 1 d . . . N2 N 0.1717(2) 0.2464(2) 0.48454(18) 0.0156(6) Uani 1 1 d . . . N3 N 0.2515(2) 0.0660(2) 0.64988(18) 0.0168(7) Uani 1 1 d . . . N4 N 0.2497(2) 0.2112(2) 0.61150(18) 0.0169(7) Uani 1 1 d . . . N5 N 0.2515(2) 0.3433(2) 0.42937(18) 0.0148(6) Uani 1 1 d . . . N6 N 0.3854(2) 0.3299(2) 0.38310(18) 0.0149(6) Uani 1 1 d . . . N7 N 0.3283(2) 0.3094(2) 0.55645(18) 0.0172(7) Uani 1 1 d . . . N8 N 0.4553(2) 0.3138(2) 0.50741(18) 0.0172(7) Uani 1 1 d . . . N9 N 0.5422(2) 0.2435(2) 0.34500(18) 0.0150(6) Uani 1 1 d . . . N10 N 0.6668(2) 0.1108(2) 0.33335(18) 0.0157(6) Uani 1 1 d . . . N11 N 0.6108(2) 0.2235(2) 0.47091(18) 0.0169(7) Uani 1 1 d . . . N12 N 0.7258(2) 0.0812(2) 0.46472(18) 0.0157(6) Uani 1 1 d . . . N13 N 0.1246(2) 0.1758(2) 0.03790(18) 0.0161(7) Uani 1 1 d . . . N14 N 0.2639(2) 0.1743(2) 0.04786(18) 0.0162(7) Uani 1 1 d . . . N15 N 0.1069(2) 0.2362(2) -0.10132(18) 0.0181(7) Uani 1 1 d . . . N16 N 0.2398(2) 0.2486(2) -0.09024(19) 0.0188(7) Uani 1 1 d . . . N17 N 0.3411(2) 0.2698(2) 0.06538(18) 0.0160(7) Uani 1 1 d . . . N18 N 0.3086(2) 0.4138(2) 0.08154(18) 0.0160(7) Uani 1 1 d . . . N19 N 0.3166(2) 0.3452(2) -0.07255(18) 0.0185(7) Uani 1 1 d . . . N20 N 0.3009(2) 0.4842(2) -0.05611(18) 0.0168(7) Uani 1 1 d . . . N21 N 0.2071(2) 0.5742(2) 0.09869(18) 0.0177(7) Uani 1 1 d . . . N22 N 0.0659(2) 0.6942(2) 0.10351(19) 0.0190(7) Uani 1 1 d . . . N23 N 0.1930(2) 0.6426(2) -0.03961(18) 0.0185(7) Uani 1 1 d . . . N24 N 0.0477(2) 0.7555(2) -0.03494(18) 0.0178(7) Uani 1 1 d . . . O1 O 0.1995(2) 0.1652(2) 0.39226(15) 0.0183(6) Uani 1 1 d . . . O2 O 0.29238(19) 0.2832(2) 0.32496(15) 0.0193(6) Uani 1 1 d . . . O3 O 0.52292(19) 0.1616(2) 0.26472(16) 0.0208(6) Uani 1 1 d . . . O4 O 0.3650(2) 0.0885(2) 0.70785(17) 0.0270(7) Uani 1 1 d . . . O5 O 0.4711(2) 0.2275(2) 0.63447(16) 0.0252(6) Uani 1 1 d . . . O6 O 0.6768(2) 0.0979(2) 0.58281(16) 0.0249(6) Uani 1 1 d . . . O7 O 0.17307(19) 0.1982(2) 0.14716(15) 0.0193(6) Uani 1 1 d . . . O8 O 0.2659(2) 0.3114(2) 0.16937(15) 0.0195(6) Uani 1 1 d . . . O9 O 0.1233(2) 0.5475(2) 0.19904(16) 0.0246(6) Uani 1 1 d . . . O10 O 0.1222(2) 0.3596(2) -0.18975(17) 0.0278(7) Uani 1 1 d . . . O11 O 0.2360(2) 0.4888(2) -0.17059(16) 0.0258(6) Uani 1 1 d . . . O12 O 0.0803(2) 0.7029(2) -0.14383(16) 0.0248(6) Uani 1 1 d . . . N25 N 0.4909(3) 0.5554(3) 0.1966(2) 0.0303(9) Uani 1 1 d . . . N26 N 0.9337(3) 0.2813(3) 0.4138(3) 0.0418(10) Uani 1 1 d . . . N27 N 0.9062(5) 0.0633(4) 0.1672(3) 0.0550(14) Uani 1 1 d . . . O13 O 0.4542(3) 0.5481(3) 0.2564(2) 0.0476(10) Uani 1 1 d . . . O14 O 0.4901(3) 0.5088(3) 0.1518(2) 0.0534(11) Uani 1 1 d . . . O15 O 0.5278(3) 0.6097(4) 0.1802(3) 0.0607(12) Uani 1 1 d . . . O16 O 0.9730(3) 0.1920(3) 0.4299(3) 0.0587(11) Uani 1 1 d . . . O17 O 0.9544(5) 0.3296(4) 0.3589(3) 0.0858(19) Uani 1 1 d . . . O18 O 0.8748(4) 0.3233(4) 0.4539(3) 0.0812(17) Uani 1 1 d . . . O19 O 0.9666(3) 0.0030(3) 0.1325(2) 0.0585(11) Uani 1 1 d . . . O20 O 0.8265(4) 0.1294(4) 0.1319(3) 0.0743(14) Uani 1 1 d . . . O21 O 0.9239(5) 0.0546(4) 0.2322(3) 0.0885(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.0290(16) 0.0199(14) 0.0194(14) -0.0028(12) -0.0012(12) -0.0076(13) O2W 0.0227(15) 0.0219(15) 0.0264(15) -0.0028(12) 0.0011(12) -0.0097(13) O3W 0.0227(15) 0.0334(17) 0.0221(15) -0.0056(13) 0.0015(12) -0.0137(14) O4W 0.0225(15) 0.0290(16) 0.0342(17) -0.0094(14) 0.0049(13) -0.0137(13) Er1 0.02240(12) 0.02197(12) 0.01420(11) -0.00434(8) 0.00253(7) -0.01150(9) C1 0.0113(17) 0.0130(17) 0.0144(18) -0.0037(14) 0.0004(14) -0.0044(15) C2 0.0132(18) 0.0178(19) 0.0108(17) -0.0030(15) 0.0027(15) -0.0050(15) C3 0.0149(18) 0.0184(19) 0.0121(18) -0.0049(15) 0.0035(15) -0.0055(16) C4 0.0180(19) 0.0200(19) 0.0125(18) -0.0048(15) 0.0049(16) -0.0068(16) C5 0.0129(17) 0.0137(18) 0.0135(17) -0.0022(14) 0.0027(14) -0.0050(15) C6 0.030(2) 0.026(2) 0.0143(19) -0.0100(16) 0.0071(17) -0.0169(19) C7 0.0142(18) 0.0141(17) 0.0121(17) 0.0000(14) 0.0005(14) -0.0053(15) C8 0.0160(18) 0.0142(18) 0.0130(18) -0.0046(15) 0.0025(15) -0.0066(15) C9 0.0124(18) 0.0138(18) 0.0143(18) -0.0053(15) 0.0009(15) -0.0033(15) C10 0.021(2) 0.0211(19) 0.018(2) -0.0103(16) 0.0045(16) -0.0108(17) C11 0.0134(18) 0.0176(19) 0.0125(18) -0.0024(15) 0.0024(15) -0.0027(16) C12 0.0172(19) 0.022(2) 0.0176(19) -0.0093(16) 0.0011(15) -0.0087(17) C13 0.0136(18) 0.0174(18) 0.0120(17) 0.0013(14) 0.0010(15) -0.0081(15) C14 0.0121(18) 0.0181(19) 0.0134(18) -0.0049(15) 0.0020(14) -0.0071(16) C15 0.0144(18) 0.0137(18) 0.0139(18) -0.0006(15) 0.0001(15) -0.0043(15) C16 0.0152(18) 0.0180(19) 0.017(2) -0.0038(16) -0.0005(15) -0.0072(16) C17 0.0147(18) 0.0136(18) 0.0179(19) -0.0004(15) -0.0025(15) -0.0049(15) C18 0.0171(19) 0.0143(18) 0.0111(17) -0.0011(15) 0.0021(15) -0.0024(15) C19 0.018(2) 0.025(2) 0.022(2) -0.0038(17) 0.0077(17) -0.0092(17) C20 0.027(2) 0.034(2) 0.023(2) -0.0070(19) 0.0133(19) -0.011(2) C21 0.020(2) 0.031(2) 0.017(2) -0.0096(18) 0.0079(17) -0.0036(18) C22 0.0176(19) 0.021(2) 0.018(2) -0.0080(16) 0.0048(16) -0.0029(17) C23 0.020(2) 0.023(2) 0.031(2) -0.0154(18) 0.0091(18) -0.0081(18) C24 0.024(2) 0.020(2) 0.033(2) -0.0048(19) 0.0014(19) -0.0047(18) C25 0.032(2) 0.018(2) 0.026(2) 0.0003(17) 0.0015(19) -0.0054(19) C26 0.025(2) 0.019(2) 0.024(2) -0.0039(17) 0.0040(17) -0.0122(18) C27 0.020(2) 0.021(2) 0.025(2) -0.0022(17) 0.0030(17) -0.0117(17) C28 0.028(2) 0.024(2) 0.025(2) 0.0001(18) 0.0068(18) -0.0131(19) C29 0.030(2) 0.029(2) 0.030(2) -0.001(2) 0.016(2) -0.013(2) C30 0.0144(19) 0.024(2) 0.026(2) -0.0023(18) 0.0057(17) -0.0085(17) C31 0.0183(19) 0.0113(17) 0.0123(18) -0.0031(14) 0.0008(15) -0.0055(15) C32 0.0203(19) 0.0156(18) 0.0126(18) -0.0046(15) 0.0006(15) -0.0057(16) C33 0.021(2) 0.0161(18) 0.0107(17) -0.0050(15) 0.0007(15) -0.0065(16) C34 0.027(2) 0.021(2) 0.0144(19) -0.0094(17) 0.0036(17) -0.0094(18) C35 0.0172(19) 0.0159(18) 0.0145(18) -0.0030(15) 0.0017(15) -0.0066(16) C36 0.032(2) 0.026(2) 0.0141(19) -0.0085(17) 0.0106(17) -0.0164(19) C37 0.0156(18) 0.0176(18) 0.0107(18) -0.0009(15) -0.0009(15) -0.0079(16) C38 0.0155(19) 0.0180(19) 0.0156(19) -0.0042(15) 0.0041(15) -0.0078(16) C39 0.0182(19) 0.0168(18) 0.0115(18) -0.0004(15) 0.0026(15) -0.0082(16) C40 0.0175(19) 0.023(2) 0.0163(19) -0.0050(16) 0.0080(16) -0.0102(17) C41 0.0208(19) 0.0165(18) 0.0129(18) -0.0041(15) 0.0003(15) -0.0077(16) C42 0.023(2) 0.021(2) 0.0155(19) -0.0006(16) 0.0049(16) -0.0131(17) C43 0.023(2) 0.0195(19) 0.018(2) -0.0079(16) 0.0016(16) -0.0112(17) C44 0.021(2) 0.0164(19) 0.0159(19) -0.0011(15) -0.0005(16) -0.0102(16) C45 0.0174(19) 0.0169(19) 0.0144(18) -0.0009(15) -0.0025(15) -0.0079(16) C46 0.0191(19) 0.0157(18) 0.0171(19) 0.0021(15) -0.0019(16) -0.0105(16) C47 0.0192(19) 0.0182(19) 0.0165(19) -0.0004(15) 0.0005(16) -0.0111(16) C48 0.021(2) 0.025(2) 0.0127(18) -0.0093(16) -0.0013(16) -0.0054(17) C49 0.032(2) 0.017(2) 0.036(2) -0.0110(18) -0.005(2) -0.0095(19) C50 0.040(3) 0.036(3) 0.044(3) -0.030(2) -0.007(2) 0.001(2) C51 0.054(3) 0.030(3) 0.031(3) -0.021(2) 0.014(2) -0.010(2) C52 0.024(2) 0.020(2) 0.025(2) -0.0110(17) 0.0069(18) -0.0038(18) C53 0.019(2) 0.022(2) 0.025(2) -0.0049(17) 0.0073(17) -0.0072(17) C54 0.018(2) 0.029(2) 0.032(2) -0.0021(19) 0.0000(18) -0.0047(18) C55 0.019(2) 0.034(2) 0.028(2) -0.0041(19) 0.0000(18) -0.0144(19) C56 0.021(2) 0.028(2) 0.024(2) -0.0047(18) 0.0057(17) -0.0172(18) C57 0.021(2) 0.021(2) 0.030(2) -0.0018(17) -0.0032(18) -0.0128(18) C58 0.031(2) 0.030(2) 0.036(3) -0.009(2) -0.009(2) -0.015(2) C59 0.034(3) 0.033(2) 0.036(3) -0.015(2) -0.005(2) -0.017(2) C60 0.027(2) 0.0171(19) 0.028(2) -0.0054(17) -0.0047(18) -0.0104(18) N1 0.0160(15) 0.0157(15) 0.0099(15) -0.0025(12) 0.0018(12) -0.0063(13) N2 0.0187(16) 0.0167(16) 0.0100(15) -0.0039(13) 0.0048(13) -0.0069(14) N3 0.0171(16) 0.0174(16) 0.0110(15) -0.0008(13) -0.0017(13) -0.0054(14) N4 0.0196(17) 0.0188(16) 0.0131(15) -0.0035(13) 0.0009(13) -0.0100(14) N5 0.0145(15) 0.0206(16) 0.0118(15) -0.0069(13) 0.0035(12) -0.0090(14) N6 0.0150(15) 0.0202(16) 0.0117(15) -0.0077(13) 0.0059(13) -0.0085(13) N7 0.0184(16) 0.0233(17) 0.0101(15) -0.0042(13) 0.0028(13) -0.0102(14) N8 0.0142(16) 0.0221(17) 0.0147(16) -0.0065(13) 0.0023(13) -0.0072(14) N9 0.0085(15) 0.0188(16) 0.0142(15) -0.0051(13) 0.0000(12) -0.0030(13) N10 0.0148(16) 0.0172(16) 0.0131(15) -0.0052(13) 0.0007(13) -0.0051(13) N11 0.0149(16) 0.0171(16) 0.0143(16) -0.0046(13) 0.0014(13) -0.0035(13) N12 0.0158(16) 0.0149(15) 0.0124(15) -0.0004(13) -0.0004(13) -0.0055(13) N13 0.0200(17) 0.0199(16) 0.0117(15) -0.0054(13) 0.0032(13) -0.0116(14) N14 0.0162(16) 0.0209(16) 0.0117(15) -0.0057(13) 0.0009(13) -0.0082(14) N15 0.0193(17) 0.0207(17) 0.0109(15) -0.0031(13) 0.0009(13) -0.0071(14) N16 0.0242(18) 0.0190(17) 0.0124(16) -0.0031(13) 0.0008(14) -0.0099(15) N17 0.0192(16) 0.0188(16) 0.0113(15) -0.0026(13) 0.0032(13) -0.0108(14) N18 0.0197(16) 0.0194(16) 0.0114(15) -0.0043(13) 0.0060(13) -0.0114(14) N19 0.0237(18) 0.0202(17) 0.0109(15) -0.0026(13) 0.0021(13) -0.0106(15) N20 0.0190(16) 0.0155(16) 0.0124(15) -0.0006(13) 0.0008(13) -0.0068(14) N21 0.0192(17) 0.0165(16) 0.0135(16) 0.0002(13) -0.0004(13) -0.0073(14) N22 0.0201(17) 0.0178(16) 0.0149(16) -0.0025(13) 0.0016(13) -0.0064(14) N23 0.0205(17) 0.0189(16) 0.0139(16) -0.0029(13) 0.0002(13) -0.0081(14) N24 0.0191(17) 0.0188(16) 0.0141(16) -0.0021(13) -0.0035(13) -0.0089(14) O1 0.0253(15) 0.0212(14) 0.0117(13) -0.0074(11) 0.0068(11) -0.0121(12) O2 0.0208(14) 0.0275(15) 0.0143(13) -0.0107(12) 0.0053(11) -0.0127(12) O3 0.0179(14) 0.0242(15) 0.0196(14) -0.0083(12) 0.0018(12) -0.0079(12) O4 0.0283(16) 0.0250(15) 0.0211(15) -0.0006(12) -0.0082(13) -0.0096(13) O5 0.0262(16) 0.0294(16) 0.0143(14) -0.0027(12) -0.0060(12) -0.0099(13) O6 0.0258(16) 0.0248(15) 0.0155(14) -0.0027(12) 0.0021(12) -0.0058(13) O7 0.0215(14) 0.0245(15) 0.0126(13) -0.0034(11) 0.0033(11) -0.0124(12) O8 0.0285(15) 0.0229(14) 0.0138(13) -0.0067(11) 0.0084(12) -0.0170(13) O9 0.0305(16) 0.0221(15) 0.0186(15) -0.0022(12) 0.0069(12) -0.0119(13) O10 0.0347(17) 0.0249(16) 0.0170(15) 0.0027(13) -0.0042(13) -0.0123(14) O11 0.0308(16) 0.0284(16) 0.0146(14) -0.0023(12) 0.0005(12) -0.0125(14) O12 0.0245(15) 0.0299(16) 0.0159(14) -0.0052(12) -0.0029(12) -0.0095(13) N25 0.0248(19) 0.034(2) 0.023(2) 0.0011(17) -0.0030(16) -0.0108(17) N26 0.045(3) 0.044(3) 0.037(2) -0.016(2) 0.010(2) -0.018(2) N27 0.088(4) 0.055(3) 0.044(3) -0.016(3) 0.019(3) -0.051(3) O13 0.049(2) 0.051(2) 0.0306(19) -0.0002(17) 0.0139(17) -0.0187(19) O14 0.049(2) 0.061(3) 0.045(2) -0.022(2) -0.0111(19) -0.016(2) O15 0.072(3) 0.070(3) 0.057(3) -0.006(2) 0.014(2) -0.053(3) O16 0.062(3) 0.049(3) 0.056(3) -0.015(2) 0.000(2) -0.018(2) O17 0.137(5) 0.059(3) 0.077(4) -0.030(3) 0.068(4) -0.055(3) O18 0.094(4) 0.066(3) 0.080(4) -0.037(3) 0.057(3) -0.025(3) O19 0.070(3) 0.066(3) 0.044(2) -0.023(2) 0.019(2) -0.032(2) O20 0.069(3) 0.072(3) 0.072(3) -0.021(3) 0.006(3) -0.024(3) O21 0.112(5) 0.078(4) 0.051(3) -0.024(3) 0.015(3) -0.020(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 O1W Er1 2.375(3) . ? O2W Er1 2.327(3) . ? O3W Er1 2.388(3) . ? O4W Er1 2.304(3) . ? Er1 O1 2.314(3) . ? Er1 O7 2.346(3) . ? Er1 O8 2.371(3) . ? Er1 O2 2.405(3) . ? C1 O1 1.239(5) . ? C1 N1 1.350(5) . ? C1 N2 1.357(5) . ? C2 N3 1.470(5) . ? C2 N1 1.472(5) . ? C2 C19 1.519(5) . ? C2 C3 1.571(5) . ? C3 N2 1.453(5) . ? C3 N4 1.465(5) . ? C3 C22 1.527(5) . ? C4 O4 1.225(5) . ? C4 N4 1.371(5) . ? C4 N3 1.371(5) . ? C5 N2 1.450(5) . ? C5 N5 1.452(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.447(5) . ? C6 N4 1.461(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.235(5) . ? C7 N5 1.356(5) . ? C7 N6 1.362(5) . ? C8 N7 1.458(5) . ? C8 N5 1.460(5) . ? C8 C23 1.524(5) . ? C8 C9 1.580(5) . ? C9 N8 1.456(5) . ? C9 N6 1.472(5) . ? C9 C26 1.520(5) . ? C10 O5 1.223(5) . ? C10 N8 1.362(5) . ? C10 N7 1.377(5) . ? C11 N6 1.457(5) . ? C11 N9 1.456(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.449(5) . ? C12 N11 1.456(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.228(5) . ? C13 N9 1.362(5) . ? C13 N10 1.367(5) . ? C14 N11 1.447(5) . ? C14 N9 1.473(5) . ? C14 C27 1.520(5) . ? C14 C15 1.587(5) . ? C15 N10 1.464(5) . ? C15 N12 1.461(5) . ? C15 C30 1.527(5) . ? C16 O6 1.224(5) . ? C16 N12 1.362(5) . ? C16 N11 1.374(5) . ? C17 N1 1.454(5) . ? C17 N12 1.457(5) 2_656 ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N10 1.452(5) 2_656 ? C18 N3 1.453(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.536(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.535(7) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.529(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.540(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.530(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.529(6) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.528(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.529(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.530(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O7 1.241(5) . ? C31 N14 1.348(5) . ? C31 N13 1.359(5) . ? C32 N13 1.461(5) . ? C32 N15 1.466(5) . ? C32 C49 1.532(5) . ? C32 C33 1.570(5) . ? C33 N14 1.460(5) . ? C33 N16 1.459(5) . ? C33 C52 1.536(5) . ? C34 O10 1.228(5) . ? C34 N15 1.364(5) . ? C34 N16 1.369(5) . ? C35 N17 1.446(5) . ? C35 N14 1.450(5) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N16 1.450(5) . ? C36 N19 1.463(5) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O8 1.235(5) . ? C37 N18 1.355(5) . ? C37 N17 1.364(5) . ? C38 N17 1.445(5) . ? C38 N19 1.460(5) . ? C38 C53 1.540(5) . ? C38 C39 1.577(5) . ? C39 N20 1.457(5) . ? C39 N18 1.472(5) . ? C39 C56 1.517(5) . ? C40 O11 1.230(5) . ? C40 N20 1.364(5) . ? C40 N19 1.369(5) . ? C41 N18 1.454(5) . ? C41 N21 1.453(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N20 1.438(5) . ? C42 N23 1.454(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 O9 1.223(5) . ? C43 N21 1.371(5) . ? C43 N22 1.371(5) . ? C44 N23 1.457(5) . ? C44 N21 1.469(5) . ? C44 C57 1.525(5) . ? C44 C45 1.579(6) . ? C45 N24 1.461(5) . ? C45 N22 1.458(5) . ? C45 C60 1.523(5) . ? C46 O12 1.223(5) . ? C46 N24 1.365(5) . ? C46 N23 1.375(5) . ? C47 N13 1.456(5) . ? C47 N24 1.459(5) 2_565 ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 N22 1.454(5) 2_565 ? C48 N15 1.458(5) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.533(7) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.520(8) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.536(6) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.539(6) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.532(7) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.526(6) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C58 1.529(6) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 C59 1.540(7) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 C60 1.541(6) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? N10 C18 1.452(5) 2_656 ? N12 C17 1.457(5) 2_656 ? N22 C48 1.454(5) 2_565 ? N24 C47 1.459(5) 2_565 ? N25 O15 1.226(6) . ? N25 O13 1.231(5) . ? N25 O14 1.242(6) . ? N26 O16 1.225(6) . ? N26 O17 1.230(6) . ? N26 O18 1.239(6) . ? N27 O21 1.175(7) . ? N27 O20 1.266(8) . ? N27 O19 1.312(7) . ? 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 O4W Er1 O1 96.50(11) . . ? O4W Er1 O2W 140.41(10) . . ? O1 Er1 O2W 95.06(10) . . ? O4W Er1 O7 97.56(10) . . ? O1 Er1 O7 137.81(9) . . ? O2W Er1 O7 98.84(10) . . ? O4W Er1 O8 76.44(10) . . ? O1 Er1 O8 146.27(9) . . ? O2W Er1 O8 73.08(10) . . ? O7 Er1 O8 75.86(9) . . ? O4W Er1 O1W 71.95(10) . . ? O1 Er1 O1W 75.34(10) . . ? O2W Er1 O1W 147.61(10) . . ? O7 Er1 O1W 71.68(10) . . ? O8 Er1 O1W 130.43(10) . . ? O4W Er1 O3W 147.27(11) . . ? O1 Er1 O3W 74.71(10) . . ? O2W Er1 O3W 72.30(10) . . ? O7 Er1 O3W 72.07(10) . . ? O8 Er1 O3W 127.62(10) . . ? O1W Er1 O3W 75.32(11) . . ? O4W Er1 O2 72.34(10) . . ? O1 Er1 O2 76.09(9) . . ? O2W Er1 O2 73.99(10) . . ? O7 Er1 O2 146.08(9) . . ? O8 Er1 O2 70.32(9) . . ? O1W Er1 O2 130.66(10) . . ? O3W Er1 O2 132.57(10) . . ? O1 C1 N1 125.4(3) . . ? O1 C1 N2 124.9(3) . . ? N1 C1 N2 109.7(3) . . ? N3 C2 N1 111.7(3) . . ? N3 C2 C19 113.6(3) . . ? N1 C2 C19 112.9(3) . . ? N3 C2 C3 103.0(3) . . ? N1 C2 C3 102.2(3) . . ? C19 C2 C3 112.3(3) . . ? N2 C3 N4 113.4(3) . . ? N2 C3 C22 112.3(3) . . ? N4 C3 C22 112.5(3) . . ? N2 C3 C2 102.8(3) . . ? N4 C3 C2 102.7(3) . . ? C22 C3 C2 112.3(3) . . ? O4 C4 N4 125.7(4) . . ? O4 C4 N3 125.5(4) . . ? N4 C4 N3 108.7(3) . . ? N2 C5 N5 114.1(3) . . ? N2 C5 H5A 108.7 . . ? N5 C5 H5A 108.7 . . ? N2 C5 H5B 108.7 . . ? N5 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N7 C6 N4 113.7(3) . . ? N7 C6 H6A 108.8 . . ? N4 C6 H6A 108.8 . . ? N7 C6 H6B 108.8 . . ? N4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N5 125.5(3) . . ? O2 C7 N6 124.9(3) . . ? N5 C7 N6 109.5(3) . . ? N7 C8 N5 113.3(3) . . ? N7 C8 C23 113.0(3) . . ? N5 C8 C23 112.3(3) . . ? N7 C8 C9 102.6(3) . . ? N5 C8 C9 102.6(3) . . ? C23 C8 C9 112.1(3) . . ? N8 C9 N6 112.3(3) . . ? N8 C9 C26 113.7(3) . . ? N6 C9 C26 112.8(3) . . ? N8 C9 C8 102.6(3) . . ? N6 C9 C8 102.4(3) . . ? C26 C9 C8 112.0(3) . . ? O5 C10 N8 126.5(4) . . ? O5 C10 N7 125.2(4) . . ? N8 C10 N7 108.3(3) . . ? N6 C11 N9 114.2(3) . . ? N6 C11 H11A 108.7 . . ? N9 C11 H11A 108.7 . . ? N6 C11 H11B 108.7 . . ? N9 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N8 C12 N11 113.5(3) . . ? N8 C12 H12A 108.9 . . ? N11 C12 H12A 108.9 . . ? N8 C12 H12B 108.9 . . ? N11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 125.5(3) . . ? O3 C13 N10 125.5(4) . . ? N9 C13 N10 108.9(3) . . ? N11 C14 N9 112.5(3) . . ? N11 C14 C27 112.9(3) . . ? N9 C14 C27 113.7(3) . . ? N11 C14 C15 102.4(3) . . ? N9 C14 C15 101.8(3) . . ? C27 C14 C15 112.4(3) . . ? N10 C15 N12 111.8(3) . . ? N10 C15 C30 113.8(3) . . ? N12 C15 C30 113.2(3) . . ? N10 C15 C14 103.0(3) . . ? N12 C15 C14 102.6(3) . . ? C30 C15 C14 111.3(3) . . ? O6 C16 N12 126.8(4) . . ? O6 C16 N11 124.6(4) . . ? N12 C16 N11 108.6(3) . . ? N1 C17 N12 114.1(3) . 2_656 ? N1 C17 H17A 108.7 . . ? N12 C17 H17A 108.7 2_656 . ? N1 C17 H17B 108.7 . . ? N12 C17 H17B 108.7 2_656 . ? H17A C17 H17B 107.6 . . ? N10 C18 N3 115.5(3) 2_656 . ? N10 C18 H18A 108.4 2_656 . ? N3 C18 H18A 108.4 . . ? N10 C18 H18B 108.4 2_656 . ? N3 C18 H18B 108.4 . . ? H18A C18 H18B 107.5 . . ? C2 C19 C20 112.1(4) . . ? C2 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? C2 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C21 C20 C19 113.2(3) . . ? C21 C20 H20A 108.9 . . ? C19 C20 H20A 108.9 . . ? C21 C20 H20B 108.9 . . ? C19 C20 H20B 108.9 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C20 112.0(3) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C3 C22 C21 109.6(3) . . ? C3 C22 H22A 109.8 . . ? C21 C22 H22A 109.8 . . ? C3 C22 H22B 109.8 . . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? C8 C23 C24 110.9(3) . . ? C8 C23 H23A 109.5 . . ? C24 C23 H23A 109.5 . . ? C8 C23 H23B 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 108.0 . . ? C25 C24 C23 112.7(4) . . ? C25 C24 H24A 109.1 . . ? C23 C24 H24A 109.1 . . ? C25 C24 H24B 109.1 . . ? C23 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? C24 C25 C26 112.9(4) . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C9 C26 C25 110.0(3) . . ? C9 C26 H26A 109.7 . . ? C25 C26 H26A 109.7 . . ? C9 C26 H26B 109.7 . . ? C25 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C14 C27 C28 110.7(3) . . ? C14 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? C14 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 C29 112.2(4) . . ? C27 C28 H28A 109.2 . . ? C29 C28 H28A 109.2 . . ? C27 C28 H28B 109.2 . . ? C29 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C28 C29 C30 113.3(4) . . ? C28 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? C28 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C15 C30 C29 112.4(3) . . ? C15 C30 H30A 109.1 . . ? C29 C30 H30A 109.1 . . ? C15 C30 H30B 109.1 . . ? C29 C30 H30B 109.1 . . ? H30A C30 H30B 107.9 . . ? O7 C31 N14 125.2(3) . . ? O7 C31 N13 125.0(4) . . ? N14 C31 N13 109.7(3) . . ? N13 C32 N15 112.2(3) . . ? N13 C32 C49 113.1(3) . . ? N15 C32 C49 113.2(3) . . ? N13 C32 C33 102.8(3) . . ? N15 C32 C33 102.8(3) . . ? C49 C32 C33 111.7(3) . . ? N14 C33 N16 112.7(3) . . ? N14 C33 C52 112.1(3) . . ? N16 C33 C52 112.8(3) . . ? N14 C33 C32 102.5(3) . . ? N16 C33 C32 103.0(3) . . ? C52 C33 C32 112.8(3) . . ? O10 C34 N15 125.1(4) . . ? O10 C34 N16 125.8(4) . . ? N15 C34 N16 109.1(3) . . ? N17 C35 N14 113.8(3) . . ? N17 C35 H35A 108.8 . . ? N14 C35 H35A 108.8 . . ? N17 C35 H35B 108.8 . . ? N14 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? N16 C36 N19 113.6(3) . . ? N16 C36 H36A 108.8 . . ? N19 C36 H36A 108.8 . . ? N16 C36 H36B 108.8 . . ? N19 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? O8 C37 N18 125.1(4) . . ? O8 C37 N17 125.3(3) . . ? N18 C37 N17 109.6(3) . . ? N17 C38 N19 113.6(3) . . ? N17 C38 C53 112.1(3) . . ? N19 C38 C53 112.5(3) . . ? N17 C38 C39 103.0(3) . . ? N19 C38 C39 102.5(3) . . ? C53 C38 C39 112.3(3) . . ? N20 C39 N18 112.7(3) . . ? N20 C39 C56 114.0(3) . . ? N18 C39 C56 112.5(3) . . ? N20 C39 C38 102.9(3) . . ? N18 C39 C38 102.3(3) . . ? C56 C39 C38 111.4(3) . . ? O11 C40 N20 125.2(4) . . ? O11 C40 N19 126.1(4) . . ? N20 C40 N19 108.7(3) . . ? N18 C41 N21 114.6(3) . . ? N18 C41 H41A 108.6 . . ? N21 C41 H41A 108.6 . . ? N18 C41 H41B 108.6 . . ? N21 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? N20 C42 N23 114.8(3) . . ? N20 C42 H42A 108.6 . . ? N23 C42 H42A 108.6 . . ? N20 C42 H42B 108.6 . . ? N23 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? O9 C43 N21 125.5(4) . . ? O9 C43 N22 125.8(4) . . ? N21 C43 N22 108.6(3) . . ? N23 C44 N21 112.4(3) . . ? N23 C44 C57 113.1(3) . . ? N21 C44 C57 112.5(3) . . ? N23 C44 C45 103.1(3) . . ? N21 C44 C45 102.7(3) . . ? C57 C44 C45 112.2(3) . . ? N24 C45 N22 111.9(3) . . ? N24 C45 C60 113.7(3) . . ? N22 C45 C60 113.3(3) . . ? N24 C45 C44 102.4(3) . . ? N22 C45 C44 102.8(3) . . ? C60 C45 C44 111.8(3) . . ? O12 C46 N24 126.5(4) . . ? O12 C46 N23 125.0(4) . . ? N24 C46 N23 108.5(3) . . ? N13 C47 N24 114.3(3) . 2_565 ? N13 C47 H47A 108.7 . . ? N24 C47 H47A 108.7 2_565 . ? N13 C47 H47B 108.7 . . ? N24 C47 H47B 108.7 2_565 . ? H47A C47 H47B 107.6 . . ? N22 C48 N15 115.0(3) 2_565 . ? N22 C48 H48A 108.5 2_565 . ? N15 C48 H48A 108.5 . . ? N22 C48 H48B 108.5 2_565 . ? N15 C48 H48B 108.5 . . ? H48A C48 H48B 107.5 . . ? C32 C49 C50 110.7(4) . . ? C32 C49 H49A 109.5 . . ? C50 C49 H49A 109.5 . . ? C32 C49 H49B 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 108.1 . . ? C51 C50 C49 113.7(4) . . ? C51 C50 H50A 108.8 . . ? C49 C50 H50A 108.8 . . ? C51 C50 H50B 108.8 . . ? C49 C50 H50B 108.8 . . ? H50A C50 H50B 107.7 . . ? C50 C51 C52 112.5(4) . . ? C50 C51 H51A 109.1 . . ? C52 C51 H51A 109.1 . . ? C50 C51 H51B 109.1 . . ? C52 C51 H51B 109.1 . . ? H51A C51 H51B 107.8 . . ? C51 C52 C33 108.7(4) . . ? C51 C52 H52A 110.0 . . ? C33 C52 H52A 110.0 . . ? C51 C52 H52B 110.0 . . ? C33 C52 H52B 110.0 . . ? H52A C52 H52B 108.3 . . ? C38 C53 C54 110.9(3) . . ? C38 C53 H53A 109.5 . . ? C54 C53 H53A 109.5 . . ? C38 C53 H53B 109.5 . . ? C54 C53 H53B 109.5 . . ? H53A C53 H53B 108.0 . . ? C55 C54 C53 112.5(4) . . ? C55 C54 H54A 109.1 . . ? C53 C54 H54A 109.1 . . ? C55 C54 H54B 109.1 . . ? C53 C54 H54B 109.1 . . ? H54A C54 H54B 107.8 . . ? C56 C55 C54 112.8(4) . . ? C56 C55 H55A 109.0 . . ? C54 C55 H55A 109.0 . . ? C56 C55 H55B 109.0 . . ? C54 C55 H55B 109.0 . . ? H55A C55 H55B 107.8 . . ? C39 C56 C55 111.2(3) . . ? C39 C56 H56A 109.4 . . ? C55 C56 H56A 109.4 . . ? C39 C56 H56B 109.4 . . ? C55 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? C44 C57 C58 111.6(4) . . ? C44 C57 H57A 109.3 . . ? C58 C57 H57A 109.3 . . ? C44 C57 H57B 109.3 . . ? C58 C57 H57B 109.3 . . ? H57A C57 H57B 108.0 . . ? C57 C58 C59 112.4(4) . . ? C57 C58 H58A 109.1 . . ? C59 C58 H58A 109.1 . . ? C57 C58 H58B 109.1 . . ? C59 C58 H58B 109.1 . . ? H58A C58 H58B 107.9 . . ? C60 C59 C58 112.9(4) . . ? C60 C59 H59A 109.0 . . ? C58 C59 H59A 109.0 . . ? C60 C59 H59B 109.0 . . ? C58 C59 H59B 109.0 . . ? H59A C59 H59B 107.8 . . ? C45 C60 C59 111.1(3) . . ? C45 C60 H60A 109.4 . . ? C59 C60 H60A 109.4 . . ? C45 C60 H60B 109.4 . . ? C59 C60 H60B 109.4 . . ? H60A C60 H60B 108.0 . . ? C1 N1 C17 121.2(3) . . ? C1 N1 C2 112.1(3) . . ? C17 N1 C2 124.3(3) . . ? C1 N2 C5 122.5(3) . . ? C1 N2 C3 112.5(3) . . ? C5 N2 C3 125.0(3) . . ? C4 N3 C18 121.3(3) . . ? C4 N3 C2 112.4(3) . . ? C18 N3 C2 126.0(3) . . ? C4 N4 C6 121.5(3) . . ? C4 N4 C3 112.8(3) . . ? C6 N4 C3 124.7(3) . . ? C7 N5 C5 121.7(3) . . ? C7 N5 C8 112.9(3) . . ? C5 N5 C8 125.4(3) . . ? C7 N6 C11 120.9(3) . . ? C7 N6 C9 112.2(3) . . ? C11 N6 C9 124.6(3) . . ? C10 N7 C6 120.9(3) . . ? C10 N7 C8 112.6(3) . . ? C6 N7 C8 125.5(3) . . ? C10 N8 C12 120.8(3) . . ? C10 N8 C9 113.4(3) . . ? C12 N8 C9 125.5(3) . . ? C13 N9 C11 120.9(3) . . ? C13 N9 C14 113.2(3) . . ? C11 N9 C14 124.3(3) . . ? C13 N10 C18 121.8(3) . 2_656 ? C13 N10 C15 112.7(3) . . ? C18 N10 C15 125.1(3) 2_656 . ? C16 N11 C14 113.2(3) . . ? C16 N11 C12 121.4(3) . . ? C14 N11 C12 124.9(3) . . ? C16 N12 C17 120.3(3) . 2_656 ? C16 N12 C15 112.7(3) . . ? C17 N12 C15 123.9(3) 2_656 . ? C31 N13 C47 121.2(3) . . ? C31 N13 C32 112.0(3) . . ? C47 N13 C32 124.8(3) . . ? C31 N14 C35 122.8(3) . . ? C31 N14 C33 112.6(3) . . ? C35 N14 C33 124.6(3) . . ? C34 N15 C48 121.5(3) . . ? C34 N15 C32 112.4(3) . . ? C48 N15 C32 125.8(3) . . ? C34 N16 C36 121.4(3) . . ? C34 N16 C33 112.5(3) . . ? C36 N16 C33 125.4(3) . . ? C37 N17 C38 112.6(3) . . ? C37 N17 C35 121.6(3) . . ? C38 N17 C35 125.8(3) . . ? C37 N18 C41 120.8(3) . . ? C37 N18 C39 112.1(3) . . ? C41 N18 C39 124.9(3) . . ? C40 N19 C38 112.5(3) . . ? C40 N19 C36 120.6(3) . . ? C38 N19 C36 125.8(3) . . ? C40 N20 C42 121.2(3) . . ? C40 N20 C39 112.8(3) . . ? C42 N20 C39 125.8(3) . . ? C43 N21 C41 121.1(3) . . ? C43 N21 C44 112.5(3) . . ? C41 N21 C44 125.2(3) . . ? C43 N22 C48 120.8(3) . 2_565 ? C43 N22 C45 113.1(3) . . ? C48 N22 C45 125.0(3) 2_565 . ? C46 N23 C42 121.4(3) . . ? C46 N23 C44 112.6(3) . . ? C42 N23 C44 125.2(3) . . ? C46 N24 C45 113.2(3) . . ? C46 N24 C47 120.3(3) . 2_565 ? C45 N24 C47 124.5(3) . 2_565 ? C1 O1 Er1 158.8(2) . . ? C7 O2 Er1 156.0(3) . . ? C31 O7 Er1 155.2(3) . . ? C37 O8 Er1 155.3(3) . . ? O15 N25 O13 120.2(5) . . ? O15 N25 O14 119.3(5) . . ? O13 N25 O14 120.5(4) . . ? O16 N26 O17 120.2(5) . . ? O16 N26 O18 120.2(5) . . ? O17 N26 O18 119.6(5) . . ? O21 N27 O20 119.0(6) . . ? O21 N27 O19 120.5(6) . . ? O20 N27 O19 120.5(5) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.614 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.122 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 115 30 ' ' 2 0.036 0.485 0.659 18 9 ' ' 3 -0.036 0.515 0.341 20 9 ' ' 4 0.274 -0.126 0.280 205 69 ' ' 5 0.349 0.454 0.653 58 20 ' ' 6 0.500 0.000 0.500 108 25 ' ' 7 0.726 0.126 0.721 205 68 ' ' 8 0.653 0.544 0.347 56 20 ' ' _platon_squeeze_details ; ; data_p2 _database_code_depnum_ccdc_archive 'CCDC 881896' #TrackingRef '101111qx-submit-cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H106 Gd N27 O38' _chemical_formula_weight 1970.97 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.8697(13) _cell_length_b 15.9935(12) _cell_length_c 18.2482(14) _cell_angle_alpha 74.793(3) _cell_angle_beta 89.019(3) _cell_angle_gamma 63.367(2) _cell_volume 3968.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2046 _exptl_absorpt_coefficient_mu 0.949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7771 _exptl_absorpt_correction_T_max 0.8403 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41537 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 25.10 _reflns_number_total 13818 _reflns_number_gt 12049 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+12.5604P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13818 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1499 _refine_ls_wR_factor_gt 0.1385 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 O1W O 0.2579(3) 0.9515(2) 0.2140(2) 0.0275(8) Uani 1 1 d . . . O2W O 0.3980(2) 0.6191(3) 0.2531(2) 0.0283(8) Uani 1 1 d . . . O3W O 0.4432(2) 0.7754(3) 0.2348(2) 0.0290(8) Uani 1 1 d . . . O4W O 0.1205(3) 0.8854(3) 0.2261(2) 0.0319(8) Uani 1 1 d . . . Gd1 Gd 0.285541(17) 0.785590(17) 0.236006(13) 0.02059(10) Uani 1 1 d . . . C1 C 0.1992(3) 0.6689(3) 0.3895(3) 0.0177(9) Uani 1 1 d . . . C2 C 0.1396(3) 0.5872(3) 0.4854(3) 0.0198(10) Uani 1 1 d . . . C3 C 0.1231(3) 0.6861(4) 0.5008(3) 0.0219(10) Uani 1 1 d . . . C4 C 0.2195(3) 0.5544(4) 0.6058(3) 0.0210(10) Uani 1 1 d . . . C5 C 0.1549(3) 0.8247(3) 0.4171(3) 0.0197(10) Uani 1 1 d . . . H5A H 0.1517 0.8499 0.3616 0.024 Uiso 1 1 calc R . . H5B H 0.0967 0.8692 0.4334 0.024 Uiso 1 1 calc R . . C6 C 0.1895(4) 0.7158(4) 0.6153(3) 0.0246(11) Uani 1 1 d . . . H6A H 0.1269 0.7722 0.6095 0.029 Uiso 1 1 calc R . . H6B H 0.2063 0.6798 0.6697 0.029 Uiso 1 1 calc R . . C7 C 0.3129(3) 0.8160(3) 0.4189(3) 0.0177(9) Uani 1 1 d . . . C8 C 0.2406(3) 0.8375(3) 0.5292(3) 0.0201(10) Uani 1 1 d . . . C9 C 0.3364(3) 0.8440(3) 0.5346(3) 0.0203(10) Uani 1 1 d . . . C10 C 0.3455(4) 0.7096(4) 0.6324(3) 0.0222(10) Uani 1 1 d . . . C11 C 0.4546(3) 0.8385(3) 0.4340(3) 0.0206(10) Uani 1 1 d . . . H11A H 0.4488 0.8498 0.3784 0.025 Uiso 1 1 calc R . . H11B H 0.4517 0.8971 0.4437 0.025 Uiso 1 1 calc R . . C12 C 0.4810(4) 0.7441(4) 0.6392(3) 0.0248(11) Uani 1 1 d . . . H12A H 0.4775 0.8066 0.6401 0.030 Uiso 1 1 calc R . . H12B H 0.4888 0.7054 0.6923 0.030 Uiso 1 1 calc R . . C13 C 0.6032(4) 0.7012(4) 0.4230(3) 0.0219(10) Uani 1 1 d . . . C14 C 0.5978(3) 0.7409(3) 0.5392(3) 0.0206(10) Uani 1 1 d . . . C15 C 0.6989(3) 0.6580(3) 0.5363(3) 0.0187(9) Uani 1 1 d . . . C16 C 0.6298(4) 0.5998(4) 0.6401(3) 0.0226(10) Uani 1 1 d . . . C17 C 0.7903(3) 0.4817(4) 0.6278(3) 0.0223(10) Uani 1 1 d . . . H17A H 0.7837 0.4502 0.6798 0.027 Uiso 1 1 calc R . . H17B H 0.8455 0.4935 0.6307 0.027 Uiso 1 1 calc R . . C18 C 0.2278(4) 0.4111(4) 0.5746(3) 0.0224(10) Uani 1 1 d . . . H18A H 0.1739 0.4019 0.5606 0.027 Uiso 1 1 calc R . . H18B H 0.2442 0.3835 0.6301 0.027 Uiso 1 1 calc R . . C19 C 0.0462(4) 0.5865(4) 0.4712(3) 0.0265(11) Uani 1 1 d . . . H19A H 0.0170 0.5819 0.5189 0.032 Uiso 1 1 calc R . . H19B H 0.0578 0.5292 0.4545 0.032 Uiso 1 1 calc R . . C20 C -0.0216(4) 0.6791(4) 0.4101(3) 0.0301(12) Uani 1 1 d . . . H20A H 0.0068 0.6818 0.3620 0.036 Uiso 1 1 calc R . . H20B H -0.0809 0.6763 0.4015 0.036 Uiso 1 1 calc R . . C21 C -0.0440(4) 0.7722(4) 0.4323(3) 0.0335(12) Uani 1 1 d . . . H21A H -0.1108 0.8025 0.4413 0.040 Uiso 1 1 calc R . . H21B H -0.0351 0.8183 0.3896 0.040 Uiso 1 1 calc R . . C22 C 0.0187(4) 0.7530(4) 0.5041(3) 0.0296(12) Uani 1 1 d . . . H22A H 0.0119 0.8152 0.5090 0.036 Uiso 1 1 calc R . . H22B H -0.0028 0.7229 0.5494 0.036 Uiso 1 1 calc R . . C23 C 0.1543(4) 0.9297(4) 0.5377(3) 0.0280(11) Uani 1 1 d . . . H23A H 0.1421 0.9850 0.4929 0.034 Uiso 1 1 calc R . . H23B H 0.0978 0.9192 0.5408 0.034 Uiso 1 1 calc R . . C24 C 0.1741(5) 0.9521(4) 0.6101(3) 0.0393(14) Uani 1 1 d . . . H24A H 0.1811 0.8988 0.6548 0.047 Uiso 1 1 calc R . . H24B H 0.1199 1.0119 0.6144 0.047 Uiso 1 1 calc R . . C25 C 0.2640(5) 0.9651(4) 0.6096(4) 0.0424(15) Uani 1 1 d . . . H25A H 0.2463 1.0326 0.6084 0.051 Uiso 1 1 calc R . . H25B H 0.3054 0.9224 0.6573 0.051 Uiso 1 1 calc R . . C26 C 0.3196(4) 0.9424(4) 0.5426(3) 0.0310(12) Uani 1 1 d . . . H26A H 0.2843 0.9936 0.4954 0.037 Uiso 1 1 calc R . . H26B H 0.3808 0.9420 0.5503 0.037 Uiso 1 1 calc R . . C27 C 0.6009(4) 0.8314(4) 0.5475(3) 0.0264(11) Uani 1 1 d . . . H27A H 0.5372 0.8788 0.5533 0.032 Uiso 1 1 calc R . . H27B H 0.6207 0.8612 0.5010 0.032 Uiso 1 1 calc R . . C28 C 0.6692(4) 0.8078(4) 0.6161(3) 0.0347(13) Uani 1 1 d . . . H28A H 0.6421 0.7911 0.6630 0.042 Uiso 1 1 calc R . . H28B H 0.6761 0.8660 0.6150 0.042 Uiso 1 1 calc R . . C29 C 0.7680(4) 0.7228(4) 0.6182(3) 0.0339(13) Uani 1 1 d . . . H29A H 0.8163 0.7444 0.6216 0.041 Uiso 1 1 calc R . . H29B H 0.7799 0.6689 0.6641 0.041 Uiso 1 1 calc R . . C30 C 0.7771(4) 0.6862(4) 0.5475(3) 0.0268(11) Uani 1 1 d . . . H30A H 0.8393 0.6293 0.5531 0.032 Uiso 1 1 calc R . . H30B H 0.7734 0.7374 0.5022 0.032 Uiso 1 1 calc R . . C31 C 0.1914(3) 0.6866(3) 0.1235(3) 0.0186(10) Uani 1 1 d . . . C32 C 0.1205(3) 0.6238(3) 0.0553(3) 0.0182(9) Uani 1 1 d . . . C33 C 0.2110(3) 0.6229(3) 0.0185(3) 0.0186(9) Uani 1 1 d . . . C34 C 0.0768(3) 0.7230(3) -0.0718(3) 0.0210(10) Uani 1 1 d . . . C35 C 0.3376(3) 0.6641(3) 0.0647(3) 0.0157(9) Uani 1 1 d . . . H35A H 0.3628 0.6562 0.1161 0.019 Uiso 1 1 calc R . . H35B H 0.3834 0.6097 0.0471 0.019 Uiso 1 1 calc R . . C36 C 0.2266(4) 0.7139(4) -0.1168(3) 0.0230(10) Uani 1 1 d . . . H36A H 0.1900 0.7341 -0.1665 0.028 Uiso 1 1 calc R . . H36B H 0.2852 0.6543 -0.1141 0.028 Uiso 1 1 calc R . . C37 C 0.3118(3) 0.8333(3) 0.0390(3) 0.0153(9) Uani 1 1 d . . . C38 C 0.3355(3) 0.7735(3) -0.0675(2) 0.0166(9) Uani 1 1 d . . . C39 C 0.3306(3) 0.8784(3) -0.0908(3) 0.0162(9) Uani 1 1 d . . . C40 C 0.2045(3) 0.8825(3) -0.1610(3) 0.0191(10) Uani 1 1 d . . . C41 C 0.3133(3) 0.9910(3) -0.0066(3) 0.0181(9) Uani 1 1 d . . . H41A H 0.3258 0.9792 0.0485 0.022 Uiso 1 1 calc R . . H41B H 0.3665 0.9978 -0.0307 0.022 Uiso 1 1 calc R . . C42 C 0.2232(3) 1.0332(3) -0.2000(3) 0.0208(10) Uani 1 1 d . . . H42A H 0.2811 1.0376 -0.2146 0.025 Uiso 1 1 calc R . . H42B H 0.1865 1.0429 -0.2469 0.025 Uiso 1 1 calc R . . C43 C 0.1731(3) 1.1304(3) 0.0116(3) 0.0192(10) Uani 1 1 d . . . C44 C 0.2076(3) 1.1448(3) -0.1153(3) 0.0189(10) Uani 1 1 d . . . C45 C 0.1197(3) 1.2419(3) -0.1106(3) 0.0157(9) Uani 1 1 d . . . C46 C 0.0731(3) 1.1714(3) -0.1893(3) 0.0192(10) Uani 1 1 d . . . C47 C 0.0522(3) 0.6750(3) 0.1759(3) 0.0189(9) Uani 1 1 d . . . H47A H 0.0469 0.6142 0.1905 0.023 Uiso 1 1 calc R . . H47B H 0.0814 0.6791 0.2209 0.023 Uiso 1 1 calc R . . C48 C -0.0524(3) 0.7031(4) -0.0073(3) 0.0233(10) Uani 1 1 d . . . H48A H -0.0529 0.6413 0.0187 0.028 Uiso 1 1 calc R . . H48B H -0.0805 0.7232 -0.0603 0.028 Uiso 1 1 calc R . . C49 C 0.1287(4) 0.5223(3) 0.0862(3) 0.0254(11) Uani 1 1 d . . . H49A H 0.1254 0.4967 0.0437 0.030 Uiso 1 1 calc R . . H49B H 0.0758 0.5253 0.1158 0.030 Uiso 1 1 calc R . . C50 C 0.2237(4) 0.4539(4) 0.1378(3) 0.0321(12) Uani 1 1 d . . . H50A H 0.2251 0.4782 0.1815 0.039 Uiso 1 1 calc R . . H50B H 0.2283 0.3887 0.1575 0.039 Uiso 1 1 calc R . . C51 C 0.3087(4) 0.4469(4) 0.0948(3) 0.0309(12) Uani 1 1 d . . . H51A H 0.3433 0.3809 0.0893 0.037 Uiso 1 1 calc R . . H51B H 0.3516 0.4573 0.1253 0.037 Uiso 1 1 calc R . . C52 C 0.2814(4) 0.5209(4) 0.0155(3) 0.0239(10) Uani 1 1 d . . . H52A H 0.3385 0.5222 -0.0046 0.029 Uiso 1 1 calc R . . H52B H 0.2531 0.5006 -0.0193 0.029 Uiso 1 1 calc R . . C53 C 0.4268(3) 0.6962(3) -0.0863(3) 0.0222(10) Uani 1 1 d . . . H53A H 0.4809 0.6820 -0.0515 0.027 Uiso 1 1 calc R . . H53B H 0.4220 0.6357 -0.0796 0.027 Uiso 1 1 calc R . . C54 C 0.4424(4) 0.7336(4) -0.1688(3) 0.0282(11) Uani 1 1 d . . . H54A H 0.3879 0.7479 -0.2032 0.034 Uiso 1 1 calc R . . H54B H 0.4989 0.6826 -0.1814 0.034 Uiso 1 1 calc R . . C55 C 0.4548(4) 0.8261(4) -0.1818(3) 0.0312(12) Uani 1 1 d . . . H55A H 0.4173 0.8731 -0.2299 0.037 Uiso 1 1 calc R . . H55B H 0.5217 0.8092 -0.1870 0.037 Uiso 1 1 calc R . . C56 C 0.4244(3) 0.8744(4) -0.1168(3) 0.0221(10) Uani 1 1 d . . . H56A H 0.4742 0.8377 -0.0733 0.027 Uiso 1 1 calc R . . H56B H 0.4174 0.9409 -0.1343 0.027 Uiso 1 1 calc R . . C57 C 0.2913(3) 1.1610(4) -0.1430(3) 0.0257(11) Uani 1 1 d . . . H57A H 0.3414 1.1001 -0.1496 0.031 Uiso 1 1 calc R . . H57B H 0.3167 1.1785 -0.1041 0.031 Uiso 1 1 calc R . . C58 C 0.2638(4) 1.2418(4) -0.2188(3) 0.0360(13) Uani 1 1 d . . . H58A H 0.3151 1.2601 -0.2277 0.043 Uiso 1 1 calc R . . H58B H 0.2577 1.2159 -0.2604 0.043 Uiso 1 1 calc R . . C59 C 0.1712(4) 1.3330(4) -0.2213(3) 0.0298(12) Uani 1 1 d . . . H59A H 0.1812 1.3907 -0.2406 0.036 Uiso 1 1 calc R . . H59B H 0.1227 1.3381 -0.2571 0.036 Uiso 1 1 calc R . . C60 C 0.1356(4) 1.3319(3) -0.1434(3) 0.0227(10) Uani 1 1 d . . . H60A H 0.0758 1.3912 -0.1481 0.027 Uiso 1 1 calc R . . H60B H 0.1820 1.3313 -0.1083 0.027 Uiso 1 1 calc R . . N1 N 0.1912(3) 0.5854(3) 0.4182(2) 0.0190(8) Uani 1 1 d . . . N2 N 0.1582(3) 0.7294(3) 0.4345(2) 0.0179(8) Uani 1 1 d . . . N3 N 0.1985(3) 0.5143(3) 0.5556(2) 0.0214(8) Uani 1 1 d . . . N4 N 0.1831(3) 0.6526(3) 0.5725(2) 0.0214(8) Uani 1 1 d . . . N5 N 0.2350(3) 0.8251(3) 0.4531(2) 0.0186(8) Uani 1 1 d . . . N6 N 0.3738(3) 0.8256(3) 0.4634(2) 0.0188(8) Uani 1 1 d . . . N7 N 0.2585(3) 0.7506(3) 0.5909(2) 0.0221(9) Uani 1 1 d . . . N8 N 0.3913(3) 0.7632(3) 0.6019(2) 0.0214(9) Uani 1 1 d . . . N9 N 0.5462(3) 0.7572(3) 0.4666(2) 0.0206(8) Uani 1 1 d . . . N10 N 0.6922(3) 0.6432(3) 0.4621(2) 0.0204(8) Uani 1 1 d . . . N11 N 0.5646(3) 0.6935(3) 0.6043(2) 0.0223(9) Uani 1 1 d . . . N12 N 0.7063(3) 0.5753(3) 0.5997(2) 0.0210(8) Uani 1 1 d . . . N13 N 0.1147(3) 0.6706(3) 0.1160(2) 0.0180(8) Uani 1 1 d . . . N14 N 0.2487(3) 0.6585(3) 0.0693(2) 0.0174(8) Uani 1 1 d . . . N15 N 0.0449(3) 0.6868(3) -0.0073(2) 0.0198(8) Uani 1 1 d . . . N16 N 0.1720(3) 0.6926(3) -0.0569(2) 0.0189(8) Uani 1 1 d . . . N17 N 0.3297(3) 0.7541(3) 0.0143(2) 0.0180(8) Uani 1 1 d . . . N18 N 0.3093(3) 0.9069(3) -0.0198(2) 0.0157(8) Uani 1 1 d . . . N19 N 0.2510(3) 0.7906(3) -0.1119(2) 0.0194(8) Uani 1 1 d . . . N20 N 0.2503(3) 0.9347(3) -0.1504(2) 0.0164(8) Uani 1 1 d . . . N21 N 0.2270(3) 1.0815(3) -0.0362(2) 0.0161(8) Uani 1 1 d . . . N22 N -0.1110(3) 0.7762(3) 0.0295(2) 0.0192(8) Uani 1 1 d . . . N23 N 0.1682(3) 1.1117(3) -0.1675(2) 0.0191(8) Uani 1 1 d . . . N24 N 0.0418(3) 1.2440(3) -0.1545(2) 0.0173(8) Uani 1 1 d . . . O1 O 0.2338(2) 0.6888(3) 0.33102(18) 0.0239(7) Uani 1 1 d . . . O2 O 0.3263(2) 0.8045(2) 0.35404(18) 0.0213(7) Uani 1 1 d . . . O3 O 0.5796(2) 0.7044(3) 0.35805(19) 0.0265(8) Uani 1 1 d . . . O4 O 0.2628(3) 0.5098(3) 0.66930(19) 0.0281(8) Uani 1 1 d . . . O5 O 0.3753(3) 0.6390(3) 0.6891(2) 0.0315(8) Uani 1 1 d . . . O6 O 0.6223(3) 0.5473(3) 0.6998(2) 0.0274(8) Uani 1 1 d . . . O7 O 0.2080(2) 0.7173(3) 0.17351(18) 0.0230(7) Uani 1 1 d . . . O8 O 0.3030(2) 0.8354(2) 0.10609(18) 0.0221(7) Uani 1 1 d . . . O9 O 0.1774(2) 1.0978(3) 0.0814(2) 0.0278(8) Uani 1 1 d . . . O10 O 0.0293(3) 0.7738(3) -0.13412(19) 0.0283(8) Uani 1 1 d . . . O11 O 0.1362(3) 0.9133(3) -0.2080(2) 0.0307(8) Uani 1 1 d . . . O12 O 0.0240(2) 1.1626(3) -0.2356(2) 0.0257(8) Uani 1 1 d . . . N25 N 0.9900(3) 0.5569(4) 0.6960(3) 0.0340(11) Uani 1 1 d . . . N26 N 0.4045(5) 0.0647(4) 0.6648(3) 0.0476(14) Uani 1 1 d . . . N27 N 0.5665(4) 0.7198(4) 0.0851(3) 0.0399(12) Uani 1 1 d . . . O13 O 1.0273(4) 0.6107(4) 0.6819(3) 0.0652(15) Uani 1 1 d . . . O14 O 0.9538(3) 0.5469(3) 0.7568(2) 0.0497(11) Uani 1 1 d . . . O15 O 0.9892(4) 0.5104(4) 0.6515(3) 0.0592(13) Uani 1 1 d . . . O16 O 0.4637(4) 0.0052(4) 0.6317(3) 0.0589(13) Uani 1 1 d . . . O17 O 0.3251(4) 0.1290(4) 0.6312(3) 0.0676(14) Uani 1 1 d . . . O18 O 0.4246(5) 0.0570(5) 0.7305(3) 0.0803(18) Uani 1 1 d . . . O19 O 0.5273(4) 0.8073(3) 0.0688(3) 0.0545(12) Uani 1 1 d . . . O20 O 0.5477(5) 0.6705(4) 0.1420(3) 0.0802(19) Uani 1 1 d . . . O21 O 0.6224(5) 0.6769(4) 0.0438(3) 0.0791(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.034(2) 0.0211(17) 0.0234(18) -0.0044(14) -0.0033(15) -0.0094(16) O2W 0.0255(18) 0.0279(19) 0.031(2) -0.0042(16) 0.0016(15) -0.0145(16) O3W 0.0242(19) 0.040(2) 0.0252(19) -0.0089(16) -0.0005(15) -0.0170(17) O4W 0.0243(19) 0.035(2) 0.044(2) -0.0188(18) 0.0121(17) -0.0167(17) Gd1 0.02291(14) 0.02530(15) 0.01585(14) -0.00465(10) 0.00177(9) -0.01366(11) C1 0.016(2) 0.021(2) 0.017(2) -0.0043(19) -0.0020(18) -0.0087(19) C2 0.016(2) 0.025(2) 0.015(2) 0.0034(19) 0.0008(18) -0.011(2) C3 0.022(2) 0.026(3) 0.020(2) -0.005(2) 0.007(2) -0.015(2) C4 0.018(2) 0.028(3) 0.018(2) -0.004(2) 0.006(2) -0.013(2) C5 0.022(2) 0.021(2) 0.017(2) -0.0059(19) 0.0037(19) -0.011(2) C6 0.033(3) 0.028(3) 0.017(2) -0.009(2) 0.010(2) -0.017(2) C7 0.023(2) 0.017(2) 0.014(2) -0.0034(18) 0.0000(19) -0.011(2) C8 0.024(2) 0.019(2) 0.016(2) -0.0054(19) 0.0021(19) -0.008(2) C9 0.022(2) 0.018(2) 0.018(2) -0.0064(19) -0.0010(19) -0.005(2) C10 0.028(3) 0.024(3) 0.016(2) -0.009(2) 0.003(2) -0.011(2) C11 0.022(2) 0.023(2) 0.018(2) -0.0003(19) -0.0011(19) -0.014(2) C12 0.029(3) 0.031(3) 0.016(2) -0.009(2) -0.002(2) -0.014(2) C13 0.027(3) 0.026(3) 0.017(2) 0.002(2) -0.001(2) -0.020(2) C14 0.022(2) 0.022(2) 0.018(2) -0.0059(19) -0.0011(19) -0.010(2) C15 0.020(2) 0.015(2) 0.020(2) -0.0027(18) -0.0003(19) -0.0091(19) C16 0.027(3) 0.024(2) 0.021(3) -0.006(2) -0.002(2) -0.015(2) C17 0.024(2) 0.028(3) 0.020(2) -0.007(2) 0.002(2) -0.016(2) C18 0.027(3) 0.026(3) 0.015(2) 0.001(2) 0.003(2) -0.016(2) C19 0.023(3) 0.033(3) 0.029(3) -0.007(2) 0.006(2) -0.019(2) C20 0.021(3) 0.040(3) 0.027(3) 0.000(2) -0.002(2) -0.018(2) C21 0.020(3) 0.045(3) 0.035(3) -0.011(3) 0.004(2) -0.015(2) C22 0.029(3) 0.034(3) 0.030(3) -0.009(2) 0.012(2) -0.018(2) C23 0.026(3) 0.024(3) 0.029(3) -0.012(2) 0.006(2) -0.005(2) C24 0.056(4) 0.028(3) 0.027(3) -0.014(2) 0.008(3) -0.010(3) C25 0.047(4) 0.030(3) 0.041(3) -0.022(3) -0.004(3) -0.003(3) C26 0.038(3) 0.024(3) 0.037(3) -0.016(2) 0.000(2) -0.014(2) C27 0.030(3) 0.021(2) 0.031(3) -0.008(2) -0.003(2) -0.014(2) C28 0.035(3) 0.039(3) 0.038(3) -0.017(3) -0.005(3) -0.020(3) C29 0.037(3) 0.033(3) 0.034(3) -0.009(2) -0.011(2) -0.018(3) C30 0.026(3) 0.028(3) 0.031(3) -0.005(2) -0.001(2) -0.018(2) C31 0.018(2) 0.020(2) 0.015(2) 0.0007(19) -0.0008(18) -0.0088(19) C32 0.018(2) 0.021(2) 0.017(2) -0.0082(19) 0.0012(19) -0.0094(19) C33 0.019(2) 0.020(2) 0.019(2) -0.0063(19) 0.0025(19) -0.010(2) C34 0.024(2) 0.023(2) 0.020(2) -0.013(2) 0.004(2) -0.010(2) C35 0.014(2) 0.014(2) 0.014(2) -0.0028(18) 0.0017(17) -0.0039(18) C36 0.027(3) 0.029(3) 0.018(2) -0.011(2) 0.008(2) -0.015(2) C37 0.009(2) 0.016(2) 0.017(2) -0.0018(18) -0.0014(17) -0.0036(17) C38 0.020(2) 0.013(2) 0.012(2) -0.0018(17) 0.0023(18) -0.0046(19) C39 0.015(2) 0.014(2) 0.014(2) -0.0016(18) -0.0005(18) -0.0031(18) C40 0.018(2) 0.024(2) 0.011(2) -0.0030(19) 0.0022(19) -0.008(2) C41 0.018(2) 0.015(2) 0.020(2) -0.0055(18) -0.0006(19) -0.0055(19) C42 0.022(2) 0.024(2) 0.013(2) -0.0024(19) 0.0011(19) -0.008(2) C43 0.020(2) 0.018(2) 0.017(2) -0.0022(19) -0.0026(19) -0.008(2) C44 0.016(2) 0.020(2) 0.017(2) -0.0022(19) -0.0017(18) -0.0065(19) C45 0.012(2) 0.019(2) 0.019(2) -0.0065(19) 0.0049(18) -0.0094(19) C46 0.019(2) 0.024(2) 0.013(2) -0.0010(19) 0.0030(18) -0.011(2) C47 0.019(2) 0.023(2) 0.012(2) -0.0022(19) 0.0023(18) -0.009(2) C48 0.016(2) 0.033(3) 0.027(3) -0.013(2) 0.002(2) -0.013(2) C49 0.028(3) 0.019(2) 0.031(3) -0.005(2) 0.006(2) -0.014(2) C50 0.033(3) 0.021(3) 0.031(3) -0.001(2) 0.002(2) -0.006(2) C51 0.029(3) 0.021(3) 0.035(3) -0.006(2) 0.001(2) -0.006(2) C52 0.024(3) 0.025(3) 0.024(3) -0.011(2) 0.006(2) -0.011(2) C53 0.020(2) 0.022(2) 0.023(3) -0.010(2) 0.004(2) -0.006(2) C54 0.022(3) 0.032(3) 0.023(3) -0.012(2) 0.006(2) -0.005(2) C55 0.031(3) 0.033(3) 0.025(3) -0.009(2) 0.011(2) -0.010(2) C56 0.018(2) 0.031(3) 0.019(2) -0.009(2) 0.0064(19) -0.013(2) C57 0.017(2) 0.029(3) 0.029(3) 0.000(2) 0.004(2) -0.013(2) C58 0.028(3) 0.038(3) 0.040(3) -0.001(3) 0.012(3) -0.019(3) C59 0.030(3) 0.026(3) 0.030(3) -0.002(2) 0.005(2) -0.013(2) C60 0.027(3) 0.011(2) 0.025(3) 0.0026(19) -0.002(2) -0.008(2) N1 0.020(2) 0.023(2) 0.0162(19) -0.0036(16) 0.0046(16) -0.0131(17) N2 0.019(2) 0.020(2) 0.0115(18) 0.0030(15) 0.0013(15) -0.0105(17) N3 0.025(2) 0.022(2) 0.018(2) -0.0038(17) 0.0041(17) -0.0137(18) N4 0.026(2) 0.022(2) 0.017(2) -0.0054(17) 0.0024(17) -0.0116(18) N5 0.018(2) 0.026(2) 0.0146(19) -0.0058(16) 0.0019(16) -0.0134(17) N6 0.022(2) 0.025(2) 0.0147(19) -0.0079(16) 0.0040(16) -0.0150(18) N7 0.026(2) 0.024(2) 0.018(2) -0.0055(17) 0.0025(17) -0.0138(18) N8 0.022(2) 0.025(2) 0.0139(19) -0.0035(16) -0.0003(16) -0.0090(18) N9 0.022(2) 0.025(2) 0.016(2) -0.0026(17) -0.0039(16) -0.0128(18) N10 0.020(2) 0.022(2) 0.017(2) -0.0037(16) 0.0018(16) -0.0082(17) N11 0.024(2) 0.023(2) 0.018(2) -0.0046(17) 0.0018(17) -0.0102(18) N12 0.025(2) 0.023(2) 0.016(2) 0.0006(16) 0.0018(17) -0.0148(18) N13 0.0158(19) 0.024(2) 0.0152(19) -0.0069(16) 0.0001(15) -0.0086(16) N14 0.0177(19) 0.024(2) 0.0150(19) -0.0087(16) 0.0033(16) -0.0113(17) N15 0.0155(19) 0.025(2) 0.018(2) -0.0070(17) -0.0007(16) -0.0076(17) N16 0.020(2) 0.026(2) 0.0124(19) -0.0042(16) 0.0025(16) -0.0125(17) N17 0.021(2) 0.020(2) 0.0132(19) -0.0025(16) 0.0041(16) -0.0099(17) N18 0.0154(18) 0.0189(19) 0.0136(18) -0.0073(16) 0.0057(15) -0.0071(16) N19 0.019(2) 0.021(2) 0.017(2) -0.0062(16) 0.0014(16) -0.0087(17) N20 0.0150(19) 0.0149(18) 0.0139(19) 0.0005(15) 0.0004(15) -0.0047(16) N21 0.0143(18) 0.0150(18) 0.0134(18) -0.0013(15) 0.0001(15) -0.0033(15) N22 0.018(2) 0.022(2) 0.0137(19) -0.0055(16) 0.0012(16) -0.0059(17) N23 0.0158(19) 0.022(2) 0.018(2) -0.0099(16) 0.0029(16) -0.0050(16) N24 0.0124(18) 0.0192(19) 0.0158(19) -0.0017(16) -0.0018(15) -0.0050(16) O1 0.0304(19) 0.0347(19) 0.0158(17) -0.0098(15) 0.0112(14) -0.0218(16) O2 0.0245(18) 0.0276(18) 0.0177(17) -0.0087(14) 0.0072(14) -0.0160(15) O3 0.0245(18) 0.0310(19) 0.0193(18) -0.0059(15) -0.0030(14) -0.0092(16) O4 0.0295(19) 0.0315(19) 0.0190(18) -0.0026(15) -0.0019(15) -0.0127(16) O5 0.034(2) 0.030(2) 0.0231(19) 0.0020(16) -0.0047(16) -0.0134(17) O6 0.033(2) 0.0254(18) 0.0233(18) -0.0023(15) 0.0058(15) -0.0153(16) O7 0.0242(18) 0.036(2) 0.0156(16) -0.0118(15) 0.0042(14) -0.0178(16) O8 0.0293(18) 0.0272(18) 0.0153(17) -0.0075(14) 0.0077(14) -0.0170(15) O9 0.0259(19) 0.0292(19) 0.0201(18) -0.0015(15) 0.0021(15) -0.0086(16) O10 0.0271(19) 0.035(2) 0.0193(18) -0.0028(16) -0.0023(15) -0.0134(16) O11 0.030(2) 0.0274(19) 0.0259(19) -0.0001(15) -0.0103(16) -0.0097(16) O12 0.0193(17) 0.034(2) 0.0242(18) -0.0089(15) 0.0009(14) -0.0126(15) N25 0.032(3) 0.038(3) 0.024(2) -0.001(2) -0.005(2) -0.014(2) N26 0.068(4) 0.042(3) 0.042(3) -0.008(3) 0.011(3) -0.036(3) N27 0.038(3) 0.040(3) 0.033(3) -0.004(2) -0.002(2) -0.013(2) O13 0.073(4) 0.079(4) 0.065(3) -0.010(3) 0.019(3) -0.059(3) O14 0.048(3) 0.054(3) 0.035(2) 0.002(2) 0.010(2) -0.021(2) O15 0.055(3) 0.073(3) 0.046(3) -0.022(3) -0.012(2) -0.022(3) O16 0.070(3) 0.064(3) 0.047(3) -0.028(3) 0.025(3) -0.029(3) O17 0.064(4) 0.065(3) 0.066(4) -0.015(3) 0.004(3) -0.024(3) O18 0.093(5) 0.085(4) 0.048(3) -0.024(3) 0.005(3) -0.025(4) O19 0.056(3) 0.043(3) 0.052(3) -0.006(2) 0.000(2) -0.015(2) O20 0.131(6) 0.057(3) 0.058(3) -0.015(3) 0.047(4) -0.050(4) O21 0.096(5) 0.060(3) 0.071(4) -0.028(3) 0.051(4) -0.023(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 O1W Gd1 2.408(3) . ? O2W Gd1 2.387(4) . ? O3W Gd1 2.433(3) . ? O4W Gd1 2.357(4) . ? Gd1 O8 2.349(3) . ? Gd1 O2 2.390(3) . ? Gd1 O1 2.400(3) . ? Gd1 O7 2.431(3) . ? C1 O1 1.225(6) . ? C1 N1 1.364(6) . ? C1 N2 1.366(6) . ? C2 N1 1.462(6) . ? C2 N3 1.467(6) . ? C2 C19 1.515(6) . ? C2 C3 1.584(7) . ? C3 N4 1.457(6) . ? C3 N2 1.461(6) . ? C3 C22 1.529(7) . ? C4 O4 1.216(6) . ? C4 N4 1.366(6) . ? C4 N3 1.370(6) . ? C5 N5 1.443(6) . ? C5 N2 1.450(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.451(6) . ? C6 N4 1.466(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.244(6) . ? C7 N5 1.341(6) . ? C7 N6 1.358(6) . ? C8 N7 1.454(6) . ? C8 N5 1.463(6) . ? C8 C23 1.541(7) . ? C8 C9 1.576(7) . ? C9 N8 1.461(6) . ? C9 N6 1.465(6) . ? C9 C26 1.521(6) . ? C10 O5 1.223(6) . ? C10 N8 1.366(6) . ? C10 N7 1.370(6) . ? C11 N9 1.445(6) . ? C11 N6 1.460(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.449(7) . ? C12 N8 1.454(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.230(6) . ? C13 N10 1.370(6) . ? C13 N9 1.370(7) . ? C14 N11 1.457(6) . ? C14 N9 1.470(6) . ? C14 C27 1.516(6) . ? C14 C15 1.570(7) . ? C15 N10 1.448(6) . ? C15 N12 1.470(6) . ? C15 C30 1.532(6) . ? C16 O6 1.229(6) . ? C16 N11 1.364(6) . ? C16 N12 1.367(7) . ? C17 N12 1.453(6) . ? C17 N1 1.458(6) 2_666 ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N3 1.441(6) . ? C18 N10 1.449(6) 2_666 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.531(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.530(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.537(8) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.529(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.531(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.521(8) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.522(7) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.540(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.530(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O7 1.227(6) . ? C31 N14 1.357(6) . ? C31 N13 1.366(6) . ? C32 N15 1.456(6) . ? C32 N13 1.471(6) . ? C32 C49 1.517(6) . ? C32 C33 1.570(6) . ? C33 N16 1.457(6) . ? C33 N14 1.462(6) . ? C33 C52 1.525(7) . ? C34 O10 1.231(6) . ? C34 N15 1.365(6) . ? C34 N16 1.371(6) . ? C35 N17 1.443(6) . ? C35 N14 1.453(6) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N16 1.448(6) . ? C36 N19 1.464(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O8 1.238(6) . ? C37 N18 1.355(6) . ? C37 N17 1.363(6) . ? C38 N17 1.452(6) . ? C38 N19 1.457(6) . ? C38 C53 1.532(6) . ? C38 C39 1.585(6) . ? C39 N20 1.457(6) . ? C39 N18 1.470(6) . ? C39 C56 1.535(6) . ? C40 O11 1.218(6) . ? C40 N19 1.367(6) . ? C40 N20 1.377(6) . ? C41 N21 1.450(6) . ? C41 N18 1.454(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N23 1.442(6) . ? C42 N20 1.464(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 O9 1.234(6) . ? C43 N21 1.355(6) . ? C43 N22 1.372(6) 2_575 ? C44 N23 1.469(6) . ? C44 N21 1.475(6) . ? C44 C57 1.518(6) . ? C44 C45 1.577(6) . ? C45 N22 1.448(6) 2_575 ? C45 N24 1.467(5) . ? C45 C60 1.538(6) . ? C46 O12 1.234(6) . ? C46 N24 1.363(6) . ? C46 N23 1.370(6) . ? C47 N24 1.442(6) 2_575 ? C47 N13 1.456(6) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 N15 1.447(6) . ? C48 N22 1.449(6) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.545(7) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.523(8) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.532(7) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.527(7) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.535(8) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.537(7) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C58 1.533(7) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 C59 1.528(8) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 C60 1.520(7) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? N1 C17 1.458(6) 2_666 ? N10 C18 1.449(6) 2_666 ? N22 C43 1.372(6) 2_575 ? N22 C45 1.448(6) 2_575 ? N24 C47 1.442(6) 2_575 ? N25 O13 1.223(7) . ? N25 O15 1.239(7) . ? N25 O14 1.246(6) . ? N26 O18 1.207(8) . ? N26 O17 1.247(8) . ? N26 O16 1.278(7) . ? N27 O19 1.200(7) . ? N27 O21 1.237(7) . ? N27 O20 1.248(7) . ? 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 O8 Gd1 O4W 97.13(13) . . ? O8 Gd1 O2W 94.18(12) . . ? O4W Gd1 O2W 140.48(12) . . ? O8 Gd1 O2 138.00(11) . . ? O4W Gd1 O2 97.17(12) . . ? O2W Gd1 O2 99.31(12) . . ? O8 Gd1 O1 146.32(11) . . ? O4W Gd1 O1 76.51(13) . . ? O2W Gd1 O1 73.26(12) . . ? O2 Gd1 O1 75.58(11) . . ? O8 Gd1 O1W 75.67(12) . . ? O4W Gd1 O1W 72.00(12) . . ? O2W Gd1 O1W 147.48(12) . . ? O2 Gd1 O1W 71.67(11) . . ? O1 Gd1 O1W 130.50(12) . . ? O8 Gd1 O7 75.78(11) . . ? O4W Gd1 O7 72.58(12) . . ? O2W Gd1 O7 73.80(12) . . ? O2 Gd1 O7 146.22(11) . . ? O1 Gd1 O7 70.75(11) . . ? O1W Gd1 O7 130.59(12) . . ? O8 Gd1 O3W 74.94(12) . . ? O4W Gd1 O3W 147.46(12) . . ? O2W Gd1 O3W 72.05(12) . . ? O2 Gd1 O3W 71.88(11) . . ? O1 Gd1 O3W 126.91(12) . . ? O1W Gd1 O3W 75.47(13) . . ? O7 Gd1 O3W 132.57(12) . . ? O1 C1 N1 125.8(4) . . ? O1 C1 N2 125.1(4) . . ? N1 C1 N2 109.0(4) . . ? N1 C2 N3 113.3(4) . . ? N1 C2 C19 112.5(4) . . ? N3 C2 C19 113.7(4) . . ? N1 C2 C3 103.0(3) . . ? N3 C2 C3 102.1(4) . . ? C19 C2 C3 111.2(4) . . ? N4 C3 N2 113.9(4) . . ? N4 C3 C22 113.7(4) . . ? N2 C3 C22 110.9(4) . . ? N4 C3 C2 102.8(4) . . ? N2 C3 C2 102.0(4) . . ? C22 C3 C2 112.8(4) . . ? O4 C4 N4 126.2(4) . . ? O4 C4 N3 125.4(5) . . ? N4 C4 N3 108.4(4) . . ? N5 C5 N2 114.2(4) . . ? N5 C5 H5A 108.7 . . ? N2 C5 H5A 108.7 . . ? N5 C5 H5B 108.7 . . ? N2 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N7 C6 N4 113.8(4) . . ? N7 C6 H6A 108.8 . . ? N4 C6 H6A 108.8 . . ? N7 C6 H6B 108.8 . . ? N4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N5 125.2(4) . . ? O2 C7 N6 124.3(4) . . ? N5 C7 N6 110.5(4) . . ? N7 C8 N5 113.4(4) . . ? N7 C8 C23 112.9(4) . . ? N5 C8 C23 111.7(4) . . ? N7 C8 C9 102.9(4) . . ? N5 C8 C9 102.8(4) . . ? C23 C8 C9 112.4(4) . . ? N8 C9 N6 112.5(4) . . ? N8 C9 C26 112.9(4) . . ? N6 C9 C26 113.8(4) . . ? N8 C9 C8 102.6(4) . . ? N6 C9 C8 102.4(3) . . ? C26 C9 C8 111.6(4) . . ? O5 C10 N8 125.9(5) . . ? O5 C10 N7 125.2(5) . . ? N8 C10 N7 108.8(4) . . ? N9 C11 N6 114.6(4) . . ? N9 C11 H11A 108.6 . . ? N6 C11 H11A 108.6 . . ? N9 C11 H11B 108.6 . . ? N6 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? N11 C12 N8 115.7(4) . . ? N11 C12 H12A 108.4 . . ? N8 C12 H12A 108.4 . . ? N11 C12 H12B 108.4 . . ? N8 C12 H12B 108.4 . . ? H12A C12 H12B 107.4 . . ? O3 C13 N10 125.1(5) . . ? O3 C13 N9 125.7(4) . . ? N10 C13 N9 109.2(4) . . ? N11 C14 N9 111.5(4) . . ? N11 C14 C27 113.5(4) . . ? N9 C14 C27 113.4(4) . . ? N11 C14 C15 102.7(4) . . ? N9 C14 C15 102.3(4) . . ? C27 C14 C15 112.3(4) . . ? N10 C15 N12 112.8(4) . . ? N10 C15 C30 113.1(4) . . ? N12 C15 C30 111.7(4) . . ? N10 C15 C14 103.9(4) . . ? N12 C15 C14 102.7(4) . . ? C30 C15 C14 111.9(4) . . ? O6 C16 N11 125.9(5) . . ? O6 C16 N12 125.7(5) . . ? N11 C16 N12 108.4(4) . . ? N12 C17 N1 115.1(4) . 2_666 ? N12 C17 H17A 108.5 . . ? N1 C17 H17A 108.5 2_666 . ? N12 C17 H17B 108.5 . . ? N1 C17 H17B 108.5 2_666 . ? H17A C17 H17B 107.5 . . ? N3 C18 N10 115.1(4) . 2_666 ? N3 C18 H18A 108.5 . . ? N10 C18 H18A 108.5 2_666 . ? N3 C18 H18B 108.5 . . ? N10 C18 H18B 108.5 2_666 . ? H18A C18 H18B 107.5 . . ? C2 C19 C20 110.8(4) . . ? C2 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? C2 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C21 C20 C19 112.7(4) . . ? C21 C20 H20A 109.1 . . ? C19 C20 H20A 109.1 . . ? C21 C20 H20B 109.1 . . ? C19 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C20 C21 C22 112.8(5) . . ? C20 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? C20 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C3 C22 C21 111.6(4) . . ? C3 C22 H22A 109.3 . . ? C21 C22 H22A 109.3 . . ? C3 C22 H22B 109.3 . . ? C21 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C8 109.5(4) . . ? C24 C23 H23A 109.8 . . ? C8 C23 H23A 109.8 . . ? C24 C23 H23B 109.8 . . ? C8 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? C23 C24 C25 111.9(5) . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C24 114.0(5) . . ? C26 C25 H25A 108.7 . . ? C24 C25 H25A 108.7 . . ? C26 C25 H25B 108.7 . . ? C24 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? C9 C26 C25 111.0(5) . . ? C9 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C9 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C14 C27 C28 111.8(4) . . ? C14 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C14 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C29 113.1(5) . . ? C27 C28 H28A 109.0 . . ? C29 C28 H28A 109.0 . . ? C27 C28 H28B 109.0 . . ? C29 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C30 C29 C28 112.3(4) . . ? C30 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? C30 C29 H29B 109.1 . . ? C28 C29 H29B 109.1 . . ? H29A C29 H29B 107.9 . . ? C29 C30 C15 111.4(4) . . ? C29 C30 H30A 109.3 . . ? C15 C30 H30A 109.3 . . ? C29 C30 H30B 109.3 . . ? C15 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? O7 C31 N14 125.3(4) . . ? O7 C31 N13 125.2(4) . . ? N14 C31 N13 109.4(4) . . ? N15 C32 N13 111.9(4) . . ? N15 C32 C49 113.5(4) . . ? N13 C32 C49 112.4(4) . . ? N15 C32 C33 102.6(4) . . ? N13 C32 C33 102.8(3) . . ? C49 C32 C33 112.7(4) . . ? N16 C33 N14 112.8(4) . . ? N16 C33 C52 113.2(4) . . ? N14 C33 C52 112.5(4) . . ? N16 C33 C32 103.3(4) . . ? N14 C33 C32 102.7(3) . . ? C52 C33 C32 111.6(4) . . ? O10 C34 N15 126.4(4) . . ? O10 C34 N16 124.7(4) . . ? N15 C34 N16 109.0(4) . . ? N17 C35 N14 114.2(4) . . ? N17 C35 H35A 108.7 . . ? N14 C35 H35A 108.7 . . ? N17 C35 H35B 108.7 . . ? N14 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? N16 C36 N19 113.4(4) . . ? N16 C36 H36A 108.9 . . ? N19 C36 H36A 108.9 . . ? N16 C36 H36B 108.9 . . ? N19 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? O8 C37 N18 125.4(4) . . ? O8 C37 N17 124.4(4) . . ? N18 C37 N17 110.1(4) . . ? N17 C38 N19 113.9(4) . . ? N17 C38 C53 112.0(4) . . ? N19 C38 C53 112.6(4) . . ? N17 C38 C39 102.9(3) . . ? N19 C38 C39 102.2(3) . . ? C53 C38 C39 112.5(4) . . ? N20 C39 N18 112.3(4) . . ? N20 C39 C56 114.0(4) . . ? N18 C39 C56 112.9(4) . . ? N20 C39 C38 102.9(3) . . ? N18 C39 C38 102.2(3) . . ? C56 C39 C38 111.5(4) . . ? O11 C40 N19 126.7(4) . . ? O11 C40 N20 125.1(4) . . ? N19 C40 N20 108.1(4) . . ? N21 C41 N18 113.4(4) . . ? N21 C41 H41A 108.9 . . ? N18 C41 H41A 108.9 . . ? N21 C41 H41B 108.9 . . ? N18 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? N23 C42 N20 115.7(4) . . ? N23 C42 H42A 108.4 . . ? N20 C42 H42A 108.4 . . ? N23 C42 H42B 108.4 . . ? N20 C42 H42B 108.4 . . ? H42A C42 H42B 107.4 . . ? O9 C43 N21 126.5(4) . . ? O9 C43 N22 123.9(4) . 2_575 ? N21 C43 N22 109.6(4) . 2_575 ? N23 C44 N21 111.3(4) . . ? N23 C44 C57 113.4(4) . . ? N21 C44 C57 113.3(4) . . ? N23 C44 C45 102.8(3) . . ? N21 C44 C45 102.3(4) . . ? C57 C44 C45 112.6(4) . . ? N22 C45 N24 112.8(3) 2_575 . ? N22 C45 C60 112.3(4) 2_575 . ? N24 C45 C60 112.8(4) . . ? N22 C45 C44 103.1(3) 2_575 . ? N24 C45 C44 102.9(3) . . ? C60 C45 C44 112.0(4) . . ? O12 C46 N24 125.1(4) . . ? O12 C46 N23 125.1(4) . . ? N24 C46 N23 109.8(4) . . ? N24 C47 N13 114.3(4) 2_575 . ? N24 C47 H47A 108.7 2_575 . ? N13 C47 H47A 108.7 . . ? N24 C47 H47B 108.7 2_575 . ? N13 C47 H47B 108.7 . . ? H47A C47 H47B 107.6 . . ? N15 C48 N22 113.9(4) . . ? N15 C48 H48A 108.8 . . ? N22 C48 H48A 108.8 . . ? N15 C48 H48B 108.8 . . ? N22 C48 H48B 108.8 . . ? H48A C48 H48B 107.7 . . ? C32 C49 C50 109.8(4) . . ? C32 C49 H49A 109.7 . . ? C50 C49 H49A 109.7 . . ? C32 C49 H49B 109.7 . . ? C50 C49 H49B 109.7 . . ? H49A C49 H49B 108.2 . . ? C51 C50 C49 112.0(4) . . ? C51 C50 H50A 109.2 . . ? C49 C50 H50A 109.2 . . ? C51 C50 H50B 109.2 . . ? C49 C50 H50B 109.2 . . ? H50A C50 H50B 107.9 . . ? C50 C51 C52 113.3(4) . . ? C50 C51 H51A 108.9 . . ? C52 C51 H51A 108.9 . . ? C50 C51 H51B 108.9 . . ? C52 C51 H51B 108.9 . . ? H51A C51 H51B 107.7 . . ? C33 C52 C51 111.3(4) . . ? C33 C52 H52A 109.4 . . ? C51 C52 H52A 109.4 . . ? C33 C52 H52B 109.4 . . ? C51 C52 H52B 109.4 . . ? H52A C52 H52B 108.0 . . ? C54 C53 C38 109.6(4) . . ? C54 C53 H53A 109.8 . . ? C38 C53 H53A 109.8 . . ? C54 C53 H53B 109.8 . . ? C38 C53 H53B 109.8 . . ? H53A C53 H53B 108.2 . . ? C53 C54 C55 112.1(4) . . ? C53 C54 H54A 109.2 . . ? C55 C54 H54A 109.2 . . ? C53 C54 H54B 109.2 . . ? C55 C54 H54B 109.2 . . ? H54A C54 H54B 107.9 . . ? C54 C55 C56 113.3(4) . . ? C54 C55 H55A 108.9 . . ? C56 C55 H55A 108.9 . . ? C54 C55 H55B 108.9 . . ? C56 C55 H55B 108.9 . . ? H55A C55 H55B 107.7 . . ? C39 C56 C55 112.0(4) . . ? C39 C56 H56A 109.2 . . ? C55 C56 H56A 109.2 . . ? C39 C56 H56B 109.2 . . ? C55 C56 H56B 109.2 . . ? H56A C56 H56B 107.9 . . ? C44 C57 C58 112.2(4) . . ? C44 C57 H57A 109.2 . . ? C58 C57 H57A 109.2 . . ? C44 C57 H57B 109.2 . . ? C58 C57 H57B 109.2 . . ? H57A C57 H57B 107.9 . . ? C59 C58 C57 113.8(5) . . ? C59 C58 H58A 108.8 . . ? C57 C58 H58A 108.8 . . ? C59 C58 H58B 108.8 . . ? C57 C58 H58B 108.8 . . ? H58A C58 H58B 107.7 . . ? C60 C59 C58 112.5(4) . . ? C60 C59 H59A 109.1 . . ? C58 C59 H59A 109.1 . . ? C60 C59 H59B 109.1 . . ? C58 C59 H59B 109.1 . . ? H59A C59 H59B 107.8 . . ? C59 C60 C45 111.0(4) . . ? C59 C60 H60A 109.4 . . ? C45 C60 H60A 109.4 . . ? C59 C60 H60B 109.4 . . ? C45 C60 H60B 109.4 . . ? H60A C60 H60B 108.0 . . ? C1 N1 C17 120.0(4) . 2_666 ? C1 N1 C2 112.5(4) . . ? C17 N1 C2 125.5(4) 2_666 . ? C1 N2 C5 121.4(4) . . ? C1 N2 C3 113.1(4) . . ? C5 N2 C3 125.5(4) . . ? C4 N3 C18 121.4(4) . . ? C4 N3 C2 113.1(4) . . ? C18 N3 C2 125.4(4) . . ? C4 N4 C3 113.0(4) . . ? C4 N4 C6 120.5(4) . . ? C3 N4 C6 125.3(4) . . ? C7 N5 C5 123.0(4) . . ? C7 N5 C8 112.2(4) . . ? C5 N5 C8 124.8(4) . . ? C7 N6 C11 121.8(4) . . ? C7 N6 C9 111.9(4) . . ? C11 N6 C9 124.8(4) . . ? C10 N7 C6 121.1(4) . . ? C10 N7 C8 112.8(4) . . ? C6 N7 C8 125.6(4) . . ? C10 N8 C12 121.4(4) . . ? C10 N8 C9 112.7(4) . . ? C12 N8 C9 125.6(4) . . ? C13 N9 C11 120.9(4) . . ? C13 N9 C14 112.2(4) . . ? C11 N9 C14 125.0(4) . . ? C13 N10 C15 112.2(4) . . ? C13 N10 C18 121.7(4) . 2_666 ? C15 N10 C18 125.1(4) . 2_666 ? C16 N11 C12 121.0(4) . . ? C16 N11 C14 113.3(4) . . ? C12 N11 C14 124.4(4) . . ? C16 N12 C17 120.6(4) . . ? C16 N12 C15 112.6(4) . . ? C17 N12 C15 126.0(4) . . ? C31 N13 C47 120.8(4) . . ? C31 N13 C32 111.9(4) . . ? C47 N13 C32 125.1(4) . . ? C31 N14 C35 121.8(4) . . ? C31 N14 C33 112.8(4) . . ? C35 N14 C33 125.4(4) . . ? C34 N15 C48 121.2(4) . . ? C34 N15 C32 112.7(4) . . ? C48 N15 C32 125.7(4) . . ? C34 N16 C36 121.1(4) . . ? C34 N16 C33 111.9(4) . . ? C36 N16 C33 125.9(4) . . ? C37 N17 C35 122.5(4) . . ? C37 N17 C38 112.1(4) . . ? C35 N17 C38 125.3(4) . . ? C37 N18 C41 121.4(4) . . ? C37 N18 C39 112.0(4) . . ? C41 N18 C39 124.1(4) . . ? C40 N19 C38 113.6(4) . . ? C40 N19 C36 120.8(4) . . ? C38 N19 C36 124.5(4) . . ? C40 N20 C39 112.8(4) . . ? C40 N20 C42 121.4(4) . . ? C39 N20 C42 125.7(4) . . ? C43 N21 C41 120.8(4) . . ? C43 N21 C44 112.0(4) . . ? C41 N21 C44 123.9(4) . . ? C43 N22 C45 112.4(4) 2_575 2_575 ? C43 N22 C48 122.0(4) 2_575 . ? C45 N22 C48 125.3(4) 2_575 . ? C46 N23 C42 122.5(4) . . ? C46 N23 C44 112.0(4) . . ? C42 N23 C44 125.1(4) . . ? C46 N24 C47 121.2(4) . 2_575 ? C46 N24 C45 112.1(4) . . ? C47 N24 C45 125.0(4) 2_575 . ? C1 O1 Gd1 155.9(3) . . ? C7 O2 Gd1 154.9(3) . . ? C31 O7 Gd1 156.5(3) . . ? C37 O8 Gd1 159.0(3) . . ? O13 N25 O15 121.0(6) . . ? O13 N25 O14 119.6(5) . . ? O15 N25 O14 119.4(5) . . ? O18 N26 O17 119.1(6) . . ? O18 N26 O16 119.5(6) . . ? O17 N26 O16 121.3(6) . . ? O19 N27 O21 120.7(6) . . ? O19 N27 O20 120.5(6) . . ? O21 N27 O20 118.7(6) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.245 _refine_diff_density_min -0.885 _refine_diff_density_rms 0.131 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 108 22 ' ' 2 0.224 0.127 0.221 207 71 ' ' 3 -0.161 0.458 0.153 59 21 ' ' 4 0.157 0.545 0.846 60 21 ' ' 5 -0.225 0.874 0.779 204 70 ' ' 6 0.500 0.500 0.500 116 32 ' ' 7 0.473 0.513 0.845 19 9 ' ' 8 0.527 0.487 0.155 17 9 ' ' _platon_squeeze_details ; ; data_a _database_code_depnum_ccdc_archive 'CCDC 881897' #TrackingRef '110104qx2-submit-cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H106 N27 O38 Y' _chemical_formula_weight 1902.63 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.9003(8) _cell_length_b 15.9406(8) _cell_length_c 18.1921(9) _cell_angle_alpha 74.646(2) _cell_angle_beta 89.345(2) _cell_angle_gamma 63.329(2) _cell_volume 3942.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1996 _exptl_absorpt_coefficient_mu 0.853 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8279 _exptl_absorpt_correction_T_max 0.8685 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40438 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13704 _reflns_number_gt 9763 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1007P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13704 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1734 _refine_ls_wR_factor_gt 0.1600 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1W O -0.2582(2) 1.0502(2) 1.28659(15) 0.0335(7) Uani 1 1 d . . . O2W O -0.44014(19) 1.2246(2) 1.26684(16) 0.0352(7) Uani 1 1 d . . . O3W O -0.1228(2) 1.1156(2) 1.27500(17) 0.0379(7) Uani 1 1 d . . . O4W O -0.3955(2) 1.3797(2) 1.24620(15) 0.0327(7) Uani 1 1 d . . . Y1 Y -0.28521(3) 1.21535(3) 1.26424(2) 0.02643(13) Uani 1 1 d . . . C1 C -0.3118(3) 1.1832(3) 1.0832(2) 0.0197(8) Uani 1 1 d . . . C2 C -0.3351(3) 1.1546(3) 0.9672(2) 0.0238(8) Uani 1 1 d . . . C3 C -0.2395(3) 1.1600(3) 0.9726(2) 0.0251(9) Uani 1 1 d . . . C4 C -0.3458(3) 1.2891(3) 0.8690(2) 0.0282(9) Uani 1 1 d . . . C5 C -0.1548(3) 1.1750(3) 1.0843(2) 0.0232(8) Uani 1 1 d . . . H5A H -0.0967 1.1308 1.0679 0.028 Uiso 1 1 calc R . . H5B H -0.1506 1.1495 1.1402 0.028 Uiso 1 1 calc R . . C6 C -0.1901(3) 1.2834(3) 0.8867(2) 0.0308(10) Uani 1 1 d . . . H6A H -0.1276 1.2266 0.8933 0.037 Uiso 1 1 calc R . . H6B H -0.2067 1.3192 0.8319 0.037 Uiso 1 1 calc R . . C7 C -0.1999(3) 1.3320(3) 1.1105(2) 0.0207(8) Uani 1 1 d . . . C8 C -0.1248(3) 1.3151(3) 1.0004(2) 0.0251(9) Uani 1 1 d . . . C9 C -0.1415(3) 1.4135(3) 1.0140(2) 0.0227(8) Uani 1 1 d . . . C10 C -0.2208(3) 1.4452(3) 0.8948(2) 0.0283(9) Uani 1 1 d . . . C11 C -0.2113(3) 1.4841(3) 1.1270(2) 0.0246(9) Uani 1 1 d . . . H11A H -0.2164 1.4526 1.1798 0.029 Uiso 1 1 calc R . . H11B H -0.1565 1.4966 1.1287 0.029 Uiso 1 1 calc R . . C12 C -0.2308(3) 1.5908(3) 0.9238(2) 0.0277(9) Uani 1 1 d . . . H12A H -0.1770 1.6007 0.9368 0.033 Uiso 1 1 calc R . . H12B H -0.2483 1.6179 0.8680 0.033 Uiso 1 1 calc R . . C13 C -0.3714(3) 1.6017(3) 1.1392(2) 0.0252(9) Uani 1 1 d . . . C14 C -0.3022(3) 1.6597(3) 1.0351(2) 0.0241(9) Uani 1 1 d . . . C15 C -0.4040(3) 1.7431(3) 1.0375(2) 0.0262(9) Uani 1 1 d . . . C16 C -0.3990(3) 1.7039(3) 0.9212(2) 0.0239(9) Uani 1 1 d . . . C17 C -0.5201(3) 1.7477(3) 1.1373(2) 0.0283(9) Uani 1 1 d . . . H17A H -0.5241 1.8110 1.1370 0.034 Uiso 1 1 calc R . . H17B H -0.5118 1.7096 1.1911 0.034 Uiso 1 1 calc R . . C18 C -0.5477(3) 1.8406(3) 0.9319(2) 0.0266(9) Uani 1 1 d . . . H18A H -0.5509 1.8992 0.9421 0.032 Uiso 1 1 calc R . . H18B H -0.5545 1.8530 0.8760 0.032 Uiso 1 1 calc R . . C19 C -0.3180(3) 1.0539(3) 0.9621(3) 0.0381(11) Uani 1 1 d . . . H19A H -0.2819 1.0035 1.0100 0.046 Uiso 1 1 calc R . . H19B H -0.3790 1.0537 0.9553 0.046 Uiso 1 1 calc R . . C20 C -0.2631(4) 1.0301(4) 0.8946(3) 0.0559(15) Uani 1 1 d . . . H20A H -0.2437 0.9616 0.8975 0.067 Uiso 1 1 calc R . . H20B H -0.3054 1.0713 0.8466 0.067 Uiso 1 1 calc R . . C21 C -0.1758(4) 1.0458(4) 0.8924(3) 0.0504(13) Uani 1 1 d . . . H21A H -0.1849 1.0996 0.8467 0.060 Uiso 1 1 calc R . . H21B H -0.1209 0.9863 0.8882 0.060 Uiso 1 1 calc R . . C22 C -0.1549(3) 1.0705(3) 0.9650(2) 0.0340(10) Uani 1 1 d . . . H22A H -0.1410 1.0151 1.0107 0.041 Uiso 1 1 calc R . . H22B H -0.0994 1.0824 0.9606 0.041 Uiso 1 1 calc R . . C23 C -0.0199(3) 1.2486(3) 0.9965(2) 0.0310(10) Uani 1 1 d . . . H23A H -0.0122 1.1857 0.9919 0.037 Uiso 1 1 calc R . . H23B H 0.0008 1.2796 0.9510 0.037 Uiso 1 1 calc R . . C24 C 0.0415(3) 1.2309(3) 1.0685(3) 0.0392(11) Uani 1 1 d . . . H24A H 0.1083 1.2002 1.0602 0.047 Uiso 1 1 calc R . . H24B H 0.0325 1.1847 1.1115 0.047 Uiso 1 1 calc R . . C25 C 0.0189(3) 1.3244(3) 1.0902(3) 0.0361(10) Uani 1 1 d . . . H25A H -0.0093 1.3220 1.1384 0.043 Uiso 1 1 calc R . . H25B H 0.0780 1.3276 1.0988 0.043 Uiso 1 1 calc R . . C26 C -0.0488(3) 1.4163(3) 1.0284(2) 0.0289(9) Uani 1 1 d . . . H26A H -0.0196 1.4210 0.9808 0.035 Uiso 1 1 calc R . . H26B H -0.0616 1.4744 1.0447 0.035 Uiso 1 1 calc R . . C27 C -0.2251(3) 1.6879(3) 1.0462(2) 0.0326(10) Uani 1 1 d . . . H27A H -0.2284 1.7384 1.0001 0.039 Uiso 1 1 calc R . . H27B H -0.1629 1.6305 1.0532 0.039 Uiso 1 1 calc R . . C28 C -0.2348(3) 1.7267(3) 1.1156(3) 0.0406(11) Uani 1 1 d . . . H28A H -0.1870 1.7491 1.1179 0.049 Uiso 1 1 calc R . . H28B H -0.2215 1.6728 1.1623 0.049 Uiso 1 1 calc R . . C29 C -0.3330(3) 1.8112(4) 1.1143(3) 0.0440(12) Uani 1 1 d . . . H29A H -0.3264 1.8696 1.1137 0.053 Uiso 1 1 calc R . . H29B H -0.3596 1.7934 1.1612 0.053 Uiso 1 1 calc R . . C30 C -0.4015(3) 1.8354(3) 1.0441(2) 0.0333(10) Uani 1 1 d . . . H30A H -0.4653 1.8836 1.0489 0.040 Uiso 1 1 calc R . . H30B H -0.3811 1.8645 0.9975 0.040 Uiso 1 1 calc R . . C31 C -0.1727(3) 0.8688(3) 1.4885(2) 0.0228(8) Uani 1 1 d . . . C32 C -0.1196(3) 0.7575(3) 1.6116(2) 0.0212(8) Uani 1 1 d . . . C33 C -0.2064(3) 0.8557(3) 1.6161(2) 0.0219(8) Uani 1 1 d . . . C34 C -0.0719(3) 0.8284(3) 1.6898(2) 0.0206(8) Uani 1 1 d . . . C35 C -0.3111(3) 1.0097(3) 1.5059(2) 0.0235(8) Uani 1 1 d . . . H35A H -0.3649 1.0034 1.5288 0.028 Uiso 1 1 calc R . . H35B H -0.3226 1.0213 1.4504 0.028 Uiso 1 1 calc R . . C36 C -0.2205(3) 0.9668(3) 1.7007(2) 0.0243(9) Uani 1 1 d . . . H36A H -0.1834 0.9568 1.7477 0.029 Uiso 1 1 calc R . . H36B H -0.2783 0.9626 1.7153 0.029 Uiso 1 1 calc R . . C37 C -0.3101(3) 1.1678(3) 1.4601(2) 0.0210(8) Uani 1 1 d . . . C38 C -0.3284(3) 1.1227(3) 1.59064(19) 0.0206(8) Uani 1 1 d . . . C39 C -0.3327(3) 1.2267(3) 1.56720(19) 0.0212(8) Uani 1 1 d . . . C40 C -0.2026(3) 1.1174(3) 1.6610(2) 0.0237(9) Uani 1 1 d . . . C41 C -0.3364(3) 1.3368(3) 1.4348(2) 0.0209(8) Uani 1 1 d . . . H41A H -0.3817 1.3909 1.4531 0.025 Uiso 1 1 calc R . . H41B H -0.3629 1.3457 1.3833 0.025 Uiso 1 1 calc R . . C42 C -0.2245(3) 1.2869(3) 1.6154(2) 0.0265(9) Uani 1 1 d . . . H42A H -0.2831 1.3470 1.6122 0.032 Uiso 1 1 calc R . . H42B H -0.1880 1.2669 1.6655 0.032 Uiso 1 1 calc R . . C43 C -0.1918(3) 1.3154(3) 1.3751(2) 0.0204(8) Uani 1 1 d . . . C44 C -0.2095(3) 1.3786(3) 1.4799(2) 0.0239(9) Uani 1 1 d . . . C45 C -0.1196(3) 1.3771(3) 1.4432(2) 0.0216(8) Uani 1 1 d . . . C46 C -0.0754(3) 1.2784(3) 1.5707(2) 0.0257(9) Uani 1 1 d . . . C47 C -0.0532(3) 0.7017(3) 1.4946(2) 0.0262(9) Uani 1 1 d . . . H47A H -0.0821 0.7213 1.4416 0.031 Uiso 1 1 calc R . . H47B H -0.0533 0.6397 1.5217 0.031 Uiso 1 1 calc R . . C48 C 0.0536(3) 0.6729(3) 1.6781(2) 0.0226(8) Uani 1 1 d . . . H48A H 0.0832 0.6768 1.7232 0.027 Uiso 1 1 calc R . . H48B H 0.0483 0.6119 1.6931 0.027 Uiso 1 1 calc R . . C49 C -0.1361(3) 0.6690(3) 1.6459(2) 0.0282(9) Uani 1 1 d . . . H49A H -0.1832 0.6700 1.6109 0.034 Uiso 1 1 calc R . . H49B H -0.0767 0.6090 1.6507 0.034 Uiso 1 1 calc R . . C50 C -0.1701(3) 0.6673(3) 1.7233(2) 0.0326(10) Uani 1 1 d . . . H50A H -0.1212 0.6620 1.7592 0.039 Uiso 1 1 calc R . . H50B H -0.1799 0.6093 1.7428 0.039 Uiso 1 1 calc R . . C51 C -0.2621(3) 0.7588(3) 1.7203(3) 0.0391(11) Uani 1 1 d . . . H51A H -0.3134 0.7406 1.7295 0.047 Uiso 1 1 calc R . . H51B H -0.2556 0.7851 1.7617 0.047 Uiso 1 1 calc R . . C52 C -0.2893(3) 0.8386(3) 1.6442(2) 0.0308(9) Uani 1 1 d . . . H52A H -0.3143 0.8203 1.6055 0.037 Uiso 1 1 calc R . . H52B H -0.3398 0.8999 1.6500 0.037 Uiso 1 1 calc R . . C53 C -0.4209(3) 1.1264(3) 1.6171(2) 0.0289(9) Uani 1 1 d . . . H53A H -0.4711 1.1632 1.5734 0.035 Uiso 1 1 calc R . . H53B H -0.4134 1.0595 1.6349 0.035 Uiso 1 1 calc R . . C54 C -0.4506(3) 1.1737(3) 1.6808(2) 0.0364(10) Uani 1 1 d . . . H54A H -0.4125 1.1263 1.7292 0.044 Uiso 1 1 calc R . . H54B H -0.5171 1.1900 1.6861 0.044 Uiso 1 1 calc R . . C55 C -0.4394(3) 1.2679(3) 1.6679(2) 0.0346(10) Uani 1 1 d . . . H55A H -0.4965 1.3191 1.6797 0.042 Uiso 1 1 calc R . . H55B H -0.3853 1.2543 1.7027 0.042 Uiso 1 1 calc R . . C56 C -0.4237(3) 1.3045(3) 1.5844(2) 0.0276(9) Uani 1 1 d . . . H56A H -0.4775 1.3181 1.5493 0.033 Uiso 1 1 calc R . . H56B H -0.4191 1.3655 1.5768 0.033 Uiso 1 1 calc R . . C57 C -0.2804(3) 1.4813(3) 1.4824(2) 0.0286(9) Uani 1 1 d . . . H57A H -0.3371 1.4795 1.5028 0.034 Uiso 1 1 calc R . . H57B H -0.2521 1.5019 1.5172 0.034 Uiso 1 1 calc R . . C58 C -0.3089(3) 1.5551(3) 1.4037(3) 0.0372(10) Uani 1 1 d . . . H58A H -0.3439 1.6213 1.4092 0.045 Uiso 1 1 calc R . . H58B H -0.3515 1.5444 1.3731 0.045 Uiso 1 1 calc R . . C59 C -0.2236(3) 1.5487(3) 1.3606(2) 0.0371(10) Uani 1 1 d . . . H59A H -0.2250 1.5247 1.3165 0.044 Uiso 1 1 calc R . . H59B H -0.2286 1.6145 1.3409 0.044 Uiso 1 1 calc R . . C60 C -0.1297(3) 1.4810(3) 1.4115(2) 0.0311(10) Uani 1 1 d . . . H60A H -0.1264 1.5066 1.4542 0.037 Uiso 1 1 calc R . . H60B H -0.0773 1.4788 1.3818 0.037 Uiso 1 1 calc R . . N1 N -0.3731(2) 1.1737(2) 1.03858(16) 0.0221(7) Uani 1 1 d . . . N2 N -0.2346(2) 1.1740(2) 1.04882(16) 0.0217(7) Uani 1 1 d . . . N3 N -0.3904(2) 1.2344(2) 0.89974(17) 0.0251(7) Uani 1 1 d . . . N4 N -0.2595(2) 1.2487(2) 0.91102(17) 0.0267(7) Uani 1 1 d . . . N5 N -0.1596(2) 1.2713(2) 1.06616(17) 0.0236(7) Uani 1 1 d . . . N6 N -0.1935(2) 1.4163(2) 1.08192(16) 0.0216(7) Uani 1 1 d . . . N7 N -0.1839(2) 1.3468(2) 0.92842(17) 0.0241(7) Uani 1 1 d . . . N8 N -0.2004(2) 1.4861(2) 0.94450(17) 0.0245(7) Uani 1 1 d . . . N9 N -0.2955(2) 1.5770(2) 1.09874(17) 0.0231(7) Uani 1 1 d . . . N10 N -0.4365(2) 1.6964(2) 1.10297(17) 0.0238(7) Uani 1 1 d . . . N11 N -0.3101(2) 1.6451(2) 0.96075(17) 0.0249(7) Uani 1 1 d . . . N12 N -0.4550(2) 1.7588(2) 0.96391(17) 0.0245(7) Uani 1 1 d . . . N13 N -0.1111(2) 0.7757(2) 1.53075(17) 0.0247(7) Uani 1 1 d . . . N14 N -0.2262(2) 0.9186(2) 1.53680(17) 0.0218(7) Uani 1 1 d . . . N15 N -0.0420(2) 0.7561(2) 1.65576(17) 0.0213(7) Uani 1 1 d . . . N16 N -0.1660(2) 0.8879(2) 1.66792(17) 0.0236(7) Uani 1 1 d . . . N17 N -0.3078(2) 1.0946(2) 1.51925(16) 0.0208(7) Uani 1 1 d . . . N18 N -0.3275(2) 1.2465(2) 1.48477(16) 0.0229(7) Uani 1 1 d . . . N19 N -0.2475(2) 1.0654(2) 1.65063(16) 0.0216(7) Uani 1 1 d . . . N20 N -0.2489(2) 1.2106(2) 1.61139(17) 0.0231(7) Uani 1 1 d . . . N21 N -0.2474(2) 1.3431(2) 1.42930(17) 0.0226(7) Uani 1 1 d . . . N22 N -0.1153(2) 1.3311(2) 1.38249(17) 0.0211(7) Uani 1 1 d . . . N23 N -0.1702(2) 1.3082(2) 1.55574(17) 0.0236(7) Uani 1 1 d . . . N24 N -0.0442(2) 1.3148(2) 1.50628(17) 0.0224(7) Uani 1 1 d . . . O1 O -0.32535(18) 1.1970(2) 1.14741(14) 0.0255(6) Uani 1 1 d . . . O2 O -0.23484(19) 1.3121(2) 1.16929(14) 0.0262(6) Uani 1 1 d . . . O3 O -0.3788(2) 1.5488(2) 1.19902(15) 0.0307(6) Uani 1 1 d . . . O4 O -0.3766(2) 1.3597(2) 0.81095(16) 0.0378(7) Uani 1 1 d . . . O5 O -0.2651(2) 1.4908(2) 0.82997(14) 0.0326(7) Uani 1 1 d . . . O6 O -0.4219(2) 1.7058(2) 0.85620(15) 0.0339(7) Uani 1 1 d . . . O7 O -0.1780(2) 0.9013(2) 1.41866(14) 0.0341(7) Uani 1 1 d . . . O8 O -0.30071(18) 1.16487(19) 1.39356(13) 0.0242(6) Uani 1 1 d . . . O9 O -0.20749(18) 1.2829(2) 1.32561(14) 0.0264(6) Uani 1 1 d . . . O10 O -0.02267(18) 0.8386(2) 1.73544(14) 0.0274(6) Uani 1 1 d . . . O11 O -0.1345(2) 1.0870(2) 1.70918(16) 0.0376(7) Uani 1 1 d . . . O12 O -0.0274(2) 1.2269(2) 1.63269(15) 0.0355(7) Uani 1 1 d . . . N25 N -0.5658(4) 1.2811(4) 1.4148(3) 0.0614(12) Uani 1 1 d . . . N26 N -0.4063(5) 0.9388(5) 1.8320(3) 0.0761(18) Uani 1 1 d . . . N27 N 0.0111(3) 1.4403(3) 0.8042(2) 0.0401(9) Uani 1 1 d . . . O13 O -0.5467(5) 1.3298(4) 1.3584(3) 0.124(2) Uani 1 1 d . . . O14 O -0.6225(4) 1.3227(4) 1.4562(3) 0.1090(19) Uani 1 1 d . . . O15 O -0.5270(3) 1.1935(4) 1.4297(3) 0.0850(14) Uani 1 1 d . . . O16 O -0.4652(3) 0.9998(3) 1.8664(2) 0.0763(12) Uani 1 1 d . . . O17 O -0.4218(4) 0.9450(4) 1.7695(3) 0.1100(18) Uani 1 1 d . . . O18 O -0.3253(4) 0.8714(4) 1.8692(3) 0.1045(17) Uani 1 1 d . . . O19 O -0.0298(3) 1.3905(3) 0.8195(2) 0.0798(13) Uani 1 1 d . . . O20 O 0.0472(3) 1.4470(3) 0.7442(2) 0.0659(11) Uani 1 1 d . . . O21 O 0.0142(3) 1.4860(3) 0.8475(2) 0.0747(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.0417(18) 0.0252(16) 0.0269(15) -0.0039(12) -0.0021(13) -0.0116(14) O2W 0.0288(16) 0.0443(19) 0.0305(15) -0.0057(14) -0.0022(12) -0.0179(15) O3W 0.0310(17) 0.0398(19) 0.0445(18) -0.0115(15) 0.0039(14) -0.0180(15) O4W 0.0357(17) 0.0271(16) 0.0316(15) -0.0041(13) 0.0023(13) -0.0138(14) Y1 0.0305(2) 0.0308(3) 0.0200(2) -0.00567(17) 0.00225(16) -0.0167(2) C1 0.023(2) 0.017(2) 0.0167(18) -0.0024(15) -0.0007(15) -0.0086(17) C2 0.028(2) 0.021(2) 0.0202(19) -0.0039(16) -0.0012(16) -0.0101(18) C3 0.033(2) 0.025(2) 0.0181(19) -0.0077(17) 0.0012(16) -0.0128(19) C4 0.034(2) 0.031(3) 0.019(2) -0.0114(19) 0.0038(18) -0.012(2) C5 0.024(2) 0.021(2) 0.0217(19) -0.0039(16) 0.0011(16) -0.0094(18) C6 0.038(2) 0.038(3) 0.0161(19) -0.0068(18) 0.0051(17) -0.018(2) C7 0.0187(19) 0.024(2) 0.0194(19) -0.0031(16) -0.0008(15) -0.0116(18) C8 0.027(2) 0.030(2) 0.0190(19) -0.0035(17) 0.0072(16) -0.0162(19) C9 0.024(2) 0.025(2) 0.0175(18) -0.0002(16) 0.0035(16) -0.0131(18) C10 0.029(2) 0.035(3) 0.023(2) -0.0077(19) 0.0106(18) -0.018(2) C11 0.027(2) 0.023(2) 0.0202(19) -0.0008(17) -0.0039(16) -0.0119(19) C12 0.033(2) 0.029(2) 0.021(2) -0.0001(17) 0.0066(17) -0.018(2) C13 0.028(2) 0.028(2) 0.025(2) -0.0105(19) 0.0022(17) -0.016(2) C14 0.022(2) 0.025(2) 0.0222(19) -0.0009(17) 0.0002(16) -0.0116(18) C15 0.031(2) 0.029(2) 0.0187(19) -0.0008(17) -0.0051(16) -0.018(2) C16 0.033(2) 0.024(2) 0.0177(19) -0.0020(17) 0.0014(17) -0.017(2) C17 0.033(2) 0.029(2) 0.0188(19) -0.0062(17) -0.0026(17) -0.011(2) C18 0.030(2) 0.030(2) 0.0204(19) 0.0009(17) -0.0017(17) -0.019(2) C19 0.039(3) 0.024(2) 0.043(3) -0.010(2) -0.012(2) -0.006(2) C20 0.056(3) 0.044(3) 0.056(3) -0.034(3) -0.005(3) -0.002(3) C21 0.068(4) 0.036(3) 0.040(3) -0.022(2) 0.008(2) -0.011(3) C22 0.036(2) 0.028(2) 0.030(2) -0.0084(19) 0.0076(19) -0.008(2) C23 0.025(2) 0.035(3) 0.030(2) -0.0054(19) 0.0087(18) -0.014(2) C24 0.024(2) 0.040(3) 0.044(3) -0.002(2) 0.003(2) -0.013(2) C25 0.028(2) 0.041(3) 0.040(2) -0.005(2) -0.0033(19) -0.020(2) C26 0.029(2) 0.033(2) 0.029(2) -0.0073(19) 0.0053(18) -0.019(2) C27 0.030(2) 0.033(3) 0.038(2) -0.005(2) -0.0029(19) -0.020(2) C28 0.042(3) 0.032(3) 0.045(3) -0.006(2) -0.018(2) -0.016(2) C29 0.049(3) 0.046(3) 0.045(3) -0.014(2) -0.007(2) -0.028(3) C30 0.039(3) 0.024(2) 0.039(2) -0.0064(19) -0.007(2) -0.018(2) C31 0.022(2) 0.024(2) 0.022(2) -0.0057(18) 0.0002(16) -0.0113(19) C32 0.021(2) 0.026(2) 0.0174(18) -0.0046(16) 0.0015(15) -0.0120(18) C33 0.022(2) 0.021(2) 0.0192(18) -0.0009(16) 0.0003(15) -0.0091(18) C34 0.021(2) 0.021(2) 0.0175(18) -0.0007(16) 0.0013(16) -0.0103(18) C35 0.025(2) 0.024(2) 0.0228(19) -0.0059(17) 0.0021(16) -0.0120(19) C36 0.026(2) 0.025(2) 0.0150(18) -0.0035(16) 0.0012(16) -0.0072(19) C37 0.0174(19) 0.023(2) 0.021(2) -0.0036(17) 0.0006(15) -0.0101(17) C38 0.022(2) 0.023(2) 0.0152(18) -0.0048(16) 0.0021(15) -0.0087(18) C39 0.024(2) 0.023(2) 0.0130(17) -0.0034(16) 0.0062(15) -0.0097(18) C40 0.021(2) 0.027(2) 0.0214(19) -0.0103(17) 0.0073(17) -0.0073(18) C41 0.020(2) 0.020(2) 0.0176(18) -0.0020(16) 0.0009(15) -0.0073(17) C42 0.031(2) 0.034(2) 0.0188(19) -0.0116(18) 0.0070(17) -0.016(2) C43 0.021(2) 0.017(2) 0.0170(18) -0.0015(16) -0.0027(15) -0.0052(17) C44 0.025(2) 0.026(2) 0.0204(19) -0.0069(17) 0.0015(16) -0.0123(19) C45 0.022(2) 0.020(2) 0.0212(19) -0.0050(16) 0.0035(16) -0.0083(18) C46 0.031(2) 0.024(2) 0.024(2) -0.0088(18) -0.0017(18) -0.0130(19) C47 0.027(2) 0.028(2) 0.023(2) -0.0076(18) -0.0016(17) -0.0129(19) C48 0.021(2) 0.026(2) 0.0163(18) -0.0045(16) 0.0016(15) -0.0073(18) C49 0.031(2) 0.023(2) 0.034(2) -0.0068(18) 0.0018(18) -0.015(2) C50 0.035(2) 0.027(2) 0.030(2) 0.0003(18) 0.0059(18) -0.014(2) C51 0.039(3) 0.036(3) 0.038(2) -0.002(2) 0.014(2) -0.017(2) C52 0.024(2) 0.030(2) 0.035(2) -0.0045(19) 0.0046(18) -0.012(2) C53 0.023(2) 0.033(2) 0.025(2) -0.0038(18) 0.0047(17) -0.012(2) C54 0.028(2) 0.041(3) 0.031(2) -0.006(2) 0.0128(19) -0.011(2) C55 0.029(2) 0.042(3) 0.023(2) -0.014(2) 0.0088(18) -0.005(2) C56 0.028(2) 0.025(2) 0.022(2) -0.0061(17) 0.0054(17) -0.0072(19) C57 0.027(2) 0.026(2) 0.035(2) -0.0144(19) 0.0093(18) -0.0098(19) C58 0.031(2) 0.019(2) 0.047(3) -0.007(2) 0.000(2) -0.001(2) C59 0.037(3) 0.023(2) 0.036(2) 0.001(2) 0.001(2) -0.007(2) C60 0.035(2) 0.026(2) 0.035(2) -0.0064(19) 0.0094(19) -0.018(2) N1 0.0275(18) 0.0265(19) 0.0171(15) -0.0076(14) 0.0042(13) -0.0158(16) N2 0.0225(17) 0.0255(19) 0.0159(15) -0.0052(14) 0.0033(13) -0.0105(15) N3 0.0291(18) 0.0254(19) 0.0182(16) -0.0043(14) -0.0004(14) -0.0114(16) N4 0.0326(19) 0.032(2) 0.0154(15) -0.0032(14) 0.0001(14) -0.0163(17) N5 0.0279(18) 0.0252(19) 0.0194(16) -0.0029(14) 0.0058(14) -0.0157(16) N6 0.0262(18) 0.0230(18) 0.0180(15) -0.0034(14) 0.0035(13) -0.0147(15) N7 0.0273(18) 0.0242(19) 0.0202(16) -0.0048(14) 0.0039(14) -0.0123(16) N8 0.0268(18) 0.0275(19) 0.0184(16) -0.0038(14) 0.0025(13) -0.0134(16) N9 0.0253(18) 0.0206(18) 0.0197(16) -0.0001(14) -0.0003(14) -0.0105(15) N10 0.0245(18) 0.0258(19) 0.0176(16) -0.0046(14) 0.0006(13) -0.0096(16) N11 0.0261(18) 0.0252(19) 0.0204(16) -0.0020(14) -0.0009(14) -0.0118(16) N12 0.0246(18) 0.0257(19) 0.0210(16) 0.0003(14) -0.0063(14) -0.0133(16) N13 0.0241(18) 0.026(2) 0.0194(16) -0.0035(14) 0.0012(14) -0.0097(16) N14 0.0206(17) 0.0209(18) 0.0178(15) -0.0008(13) 0.0002(13) -0.0071(15) N15 0.0170(16) 0.0236(18) 0.0218(16) -0.0064(14) 0.0002(13) -0.0083(15) N16 0.0236(18) 0.0260(19) 0.0200(16) -0.0063(14) 0.0014(13) -0.0107(16) N17 0.0237(17) 0.0220(18) 0.0170(15) -0.0048(13) 0.0031(13) -0.0114(15) N18 0.0286(18) 0.0251(19) 0.0153(15) -0.0046(14) 0.0046(13) -0.0135(16) N19 0.0235(17) 0.0228(18) 0.0157(15) -0.0029(13) 0.0019(13) -0.0098(15) N20 0.0262(18) 0.0251(19) 0.0175(15) -0.0041(14) 0.0007(13) -0.0125(16) N21 0.0241(17) 0.0273(19) 0.0189(16) -0.0078(14) 0.0021(13) -0.0133(15) N22 0.0201(17) 0.0249(18) 0.0202(16) -0.0087(14) 0.0047(13) -0.0107(15) N23 0.0280(18) 0.0291(19) 0.0166(15) -0.0053(14) 0.0036(13) -0.0163(16) N24 0.0206(17) 0.0266(19) 0.0192(16) -0.0075(14) 0.0022(13) -0.0097(15) O1 0.0305(15) 0.0337(16) 0.0160(13) -0.0071(12) 0.0050(11) -0.0182(14) O2 0.0344(16) 0.0312(16) 0.0186(13) -0.0068(12) 0.0087(12) -0.0202(14) O3 0.0407(17) 0.0255(16) 0.0210(14) 0.0009(12) 0.0057(12) -0.0152(14) O4 0.0447(19) 0.0351(18) 0.0244(15) 0.0048(14) -0.0053(13) -0.0177(16) O5 0.0382(17) 0.0342(17) 0.0191(14) -0.0007(13) -0.0014(13) -0.0153(15) O6 0.0317(16) 0.0423(19) 0.0239(15) -0.0076(13) -0.0027(12) -0.0149(15) O7 0.0379(17) 0.0320(17) 0.0179(14) -0.0019(12) 0.0000(12) -0.0066(14) O8 0.0300(15) 0.0305(16) 0.0127(13) -0.0052(11) 0.0035(11) -0.0150(13) O9 0.0276(15) 0.0328(16) 0.0214(13) -0.0109(12) 0.0031(11) -0.0146(14) O10 0.0237(15) 0.0337(17) 0.0256(14) -0.0116(12) -0.0002(12) -0.0121(13) O11 0.0376(18) 0.0412(19) 0.0304(16) -0.0052(14) -0.0100(14) -0.0176(15) O12 0.0366(17) 0.0421(19) 0.0238(15) -0.0050(14) -0.0041(13) -0.0171(15) N25 0.063(3) 0.060(4) 0.062(3) -0.025(3) 0.021(3) -0.026(3) N26 0.147(6) 0.090(4) 0.043(3) -0.032(3) 0.036(4) -0.093(5) N27 0.037(2) 0.044(2) 0.030(2) -0.0035(18) -0.0017(17) -0.015(2) O13 0.190(6) 0.086(4) 0.119(4) -0.041(3) 0.094(5) -0.080(4) O14 0.133(5) 0.090(4) 0.105(4) -0.061(3) 0.070(4) -0.037(3) O15 0.088(3) 0.058(3) 0.091(3) -0.022(3) -0.010(3) -0.017(3) O16 0.097(3) 0.077(3) 0.064(3) -0.032(2) 0.028(2) -0.042(3) O17 0.147(5) 0.098(4) 0.063(3) -0.024(3) 0.019(3) -0.037(4) O18 0.097(4) 0.097(4) 0.100(4) -0.019(3) -0.008(3) -0.034(3) O19 0.093(3) 0.090(3) 0.077(3) -0.006(2) 0.020(2) -0.070(3) O20 0.064(3) 0.074(3) 0.040(2) -0.0008(19) 0.0197(19) -0.025(2) O21 0.065(3) 0.091(3) 0.064(3) -0.039(2) -0.009(2) -0.023(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 O1W Y1 2.388(3) . ? O2W Y1 2.401(3) . ? O3W Y1 2.323(3) . ? O4W Y1 2.341(3) . ? Y1 O8 2.325(2) . ? Y1 O1 2.353(2) . ? Y1 O2 2.381(2) . ? Y1 O9 2.407(2) . ? C1 O1 1.243(4) . ? C1 N2 1.338(5) . ? C1 N1 1.360(4) . ? C2 N3 1.446(5) . ? C2 N1 1.473(5) . ? C2 C19 1.532(6) . ? C2 C3 1.567(5) . ? C3 N4 1.457(5) . ? C3 N2 1.469(5) . ? C3 C22 1.497(6) . ? C4 O4 1.229(5) . ? C4 N4 1.362(5) . ? C4 N3 1.366(5) . ? C5 N2 1.439(5) . ? C5 N5 1.448(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.450(5) . ? C6 N4 1.458(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.232(4) . ? C7 N6 1.356(5) . ? C7 N5 1.357(5) . ? C8 N7 1.450(5) . ? C8 N5 1.454(5) . ? C8 C23 1.537(6) . ? C8 C9 1.556(6) . ? C9 N8 1.448(5) . ? C9 N6 1.477(5) . ? C9 C26 1.523(5) . ? C10 O5 1.233(5) . ? C10 N7 1.362(5) . ? C10 N8 1.363(5) . ? C11 N9 1.443(5) . ? C11 N6 1.452(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.450(5) . ? C12 N8 1.451(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.228(5) . ? C13 N9 1.364(5) . ? C13 N10 1.367(5) . ? C14 N11 1.448(5) . ? C14 N9 1.470(5) . ? C14 C27 1.515(5) . ? C14 C15 1.577(6) . ? C15 N10 1.449(5) . ? C15 N12 1.475(4) . ? C15 C30 1.527(5) . ? C16 O6 1.231(4) . ? C16 N12 1.344(5) . ? C16 N11 1.367(5) . ? C17 N10 1.450(5) . ? C17 N3 1.454(5) 2_487 ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.449(5) 2_487 ? C18 N12 1.451(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.529(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.516(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.553(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.527(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.529(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.519(6) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.522(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.532(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.536(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O7 1.226(4) . ? C31 N13 1.364(5) . ? C31 N14 1.368(5) . ? C32 N13 1.439(5) . ? C32 N15 1.469(4) . ? C32 C49 1.519(5) . ? C32 C33 1.576(5) . ? C33 N16 1.460(5) . ? C33 N14 1.466(5) . ? C33 C52 1.518(5) . ? C34 O10 1.237(4) . ? C34 N15 1.346(5) . ? C34 N16 1.356(5) . ? C35 N14 1.440(5) . ? C35 N17 1.462(5) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N16 1.447(5) . ? C36 N19 1.459(5) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O8 1.229(4) . ? C37 N17 1.348(5) . ? C37 N18 1.354(5) . ? C38 N19 1.459(5) . ? C38 N17 1.470(4) . ? C38 C53 1.522(5) . ? C38 C39 1.569(5) . ? C39 N20 1.448(5) . ? C39 N18 1.458(4) . ? C39 C56 1.521(5) . ? C40 O11 1.226(4) . ? C40 N19 1.361(5) . ? C40 N20 1.374(5) . ? C41 N18 1.431(5) . ? C41 N21 1.462(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N23 1.446(5) . ? C42 N20 1.450(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 O9 1.229(4) . ? C43 N21 1.345(5) . ? C43 N22 1.362(5) . ? C44 N23 1.457(5) . ? C44 N21 1.458(4) . ? C44 C57 1.528(6) . ? C44 C45 1.564(5) . ? C45 N24 1.449(5) . ? C45 N22 1.464(5) . ? C45 C60 1.537(5) . ? C46 O12 1.223(5) . ? C46 N24 1.357(5) . ? C46 N23 1.366(5) . ? C47 N13 1.447(5) . ? C47 N24 1.451(5) 2_578 ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 N22 1.463(5) 2_578 ? C48 N15 1.467(5) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.502(6) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.522(6) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.519(6) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.506(6) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.546(6) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.537(5) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C58 1.512(6) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 C59 1.536(6) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 C60 1.519(6) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? N1 C18 1.449(5) 2_487 ? N3 C17 1.454(5) 2_487 ? N22 C48 1.463(5) 2_578 ? N24 C47 1.451(5) 2_578 ? N25 O15 1.198(6) . ? N25 O14 1.237(6) . ? N25 O13 1.237(6) . ? N26 O17 1.135(6) . ? N26 O18 1.289(8) . ? N26 O16 1.306(7) . ? N27 O19 1.214(5) . ? N27 O21 1.221(5) . ? N27 O20 1.229(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3W Y1 O8 96.56(10) . . ? O3W Y1 O4W 140.72(10) . . ? O8 Y1 O4W 94.73(9) . . ? O3W Y1 O1 97.01(10) . . ? O8 Y1 O1 138.31(9) . . ? O4W Y1 O1 99.12(9) . . ? O3W Y1 O2 76.92(10) . . ? O8 Y1 O2 146.31(9) . . ? O4W Y1 O2 72.99(9) . . ? O1 Y1 O2 75.31(8) . . ? O3W Y1 O1W 71.94(10) . . ? O8 Y1 O1W 75.50(9) . . ? O4W Y1 O1W 147.31(10) . . ? O1 Y1 O1W 71.69(9) . . ? O2 Y1 O1W 130.64(10) . . ? O3W Y1 O2W 146.93(11) . . ? O8 Y1 O2W 74.53(9) . . ? O4W Y1 O2W 72.32(10) . . ? O1 Y1 O2W 72.69(9) . . ? O2 Y1 O2W 127.46(9) . . ? O1W Y1 O2W 75.00(10) . . ? O3W Y1 O9 72.46(10) . . ? O8 Y1 O9 76.01(9) . . ? O4W Y1 O9 74.07(9) . . ? O1 Y1 O9 145.65(9) . . ? O2 Y1 O9 70.49(8) . . ? O1W Y1 O9 130.77(9) . . ? O2W Y1 O9 132.61(9) . . ? O1 C1 N2 125.1(3) . . ? O1 C1 N1 124.5(3) . . ? N2 C1 N1 110.4(3) . . ? N3 C2 N1 112.3(3) . . ? N3 C2 C19 113.7(3) . . ? N1 C2 C19 112.3(3) . . ? N3 C2 C3 103.6(3) . . ? N1 C2 C3 103.1(3) . . ? C19 C2 C3 111.1(3) . . ? N4 C3 N2 111.9(3) . . ? N4 C3 C22 113.7(3) . . ? N2 C3 C22 112.2(3) . . ? N4 C3 C2 102.0(3) . . ? N2 C3 C2 102.3(3) . . ? C22 C3 C2 113.8(3) . . ? O4 C4 N4 125.9(4) . . ? O4 C4 N3 125.6(4) . . ? N4 C4 N3 108.4(3) . . ? N2 C5 N5 113.9(3) . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? N5 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N4 114.0(3) . . ? N7 C6 H6A 108.8 . . ? N4 C6 H6A 108.8 . . ? N7 C6 H6B 108.8 . . ? N4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 125.1(3) . . ? O2 C7 N5 124.8(3) . . ? N6 C7 N5 110.1(3) . . ? N7 C8 N5 113.3(3) . . ? N7 C8 C23 112.4(3) . . ? N5 C8 C23 111.7(3) . . ? N7 C8 C9 103.2(3) . . ? N5 C8 C9 103.1(3) . . ? C23 C8 C9 112.5(3) . . ? N8 C9 N6 112.6(3) . . ? N8 C9 C26 113.3(3) . . ? N6 C9 C26 112.0(3) . . ? N8 C9 C8 103.0(3) . . ? N6 C9 C8 103.1(3) . . ? C26 C9 C8 112.1(3) . . ? O5 C10 N7 126.3(4) . . ? O5 C10 N8 124.9(4) . . ? N7 C10 N8 108.8(3) . . ? N9 C11 N6 114.9(3) . . ? N9 C11 H11A 108.5 . . ? N6 C11 H11A 108.5 . . ? N9 C11 H11B 108.5 . . ? N6 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N11 C12 N8 114.7(3) . . ? N11 C12 H12A 108.6 . . ? N8 C12 H12A 108.6 . . ? N11 C12 H12B 108.6 . . ? N8 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N9 125.7(4) . . ? O3 C13 N10 126.0(4) . . ? N9 C13 N10 108.2(3) . . ? N11 C14 N9 112.4(3) . . ? N11 C14 C27 113.6(3) . . ? N9 C14 C27 112.4(3) . . ? N11 C14 C15 103.3(3) . . ? N9 C14 C15 102.0(3) . . ? C27 C14 C15 112.2(3) . . ? N10 C15 N12 112.3(3) . . ? N10 C15 C30 113.6(3) . . ? N12 C15 C30 112.8(3) . . ? N10 C15 C14 103.1(3) . . ? N12 C15 C14 101.9(3) . . ? C30 C15 C14 112.1(3) . . ? O6 C16 N12 126.4(4) . . ? O6 C16 N11 124.2(4) . . ? N12 C16 N11 109.4(3) . . ? N10 C17 N3 115.7(3) . 2_487 ? N10 C17 H17A 108.4 . . ? N3 C17 H17A 108.4 2_487 . ? N10 C17 H17B 108.4 . . ? N3 C17 H17B 108.4 2_487 . ? H17A C17 H17B 107.4 . . ? N1 C18 N12 114.8(3) 2_487 . ? N1 C18 H18A 108.6 2_487 . ? N12 C18 H18A 108.6 . . ? N1 C18 H18B 108.6 2_487 . ? N12 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C20 C19 C2 110.2(4) . . ? C20 C19 H19A 109.6 . . ? C2 C19 H19A 109.6 . . ? C20 C19 H19B 109.6 . . ? C2 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? C21 C20 C19 113.7(4) . . ? C21 C20 H20A 108.8 . . ? C19 C20 H20A 108.8 . . ? C21 C20 H20B 108.8 . . ? C19 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C20 C21 C22 112.3(4) . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.9 . . ? C3 C22 C21 109.2(4) . . ? C3 C22 H22A 109.8 . . ? C21 C22 H22A 109.8 . . ? C3 C22 H22B 109.8 . . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.3 . . ? C24 C23 C8 110.5(3) . . ? C24 C23 H23A 109.6 . . ? C8 C23 H23A 109.6 . . ? C24 C23 H23B 109.6 . . ? C8 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C23 C24 C25 113.5(4) . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C24 112.2(3) . . ? C26 C25 H25A 109.2 . . ? C24 C25 H25A 109.2 . . ? C26 C25 H25B 109.2 . . ? C24 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C25 C26 C9 110.3(3) . . ? C25 C26 H26A 109.6 . . ? C9 C26 H26A 109.6 . . ? C25 C26 H26B 109.6 . . ? C9 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C14 C27 C28 111.7(4) . . ? C14 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C14 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C29 113.8(3) . . ? C27 C28 H28A 108.8 . . ? C29 C28 H28A 108.8 . . ? C27 C28 H28B 108.8 . . ? C29 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C28 C29 C30 112.1(4) . . ? C28 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? C28 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C15 C30 C29 110.7(3) . . ? C15 C30 H30A 109.5 . . ? C29 C30 H30A 109.5 . . ? C15 C30 H30B 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? O7 C31 N13 124.8(4) . . ? O7 C31 N14 126.4(4) . . ? N13 C31 N14 108.8(3) . . ? N13 C32 N15 112.6(3) . . ? N13 C32 C49 113.6(3) . . ? N15 C32 C49 112.9(3) . . ? N13 C32 C33 103.2(3) . . ? N15 C32 C33 101.7(3) . . ? C49 C32 C33 111.7(3) . . ? N16 C33 N14 111.7(3) . . ? N16 C33 C52 113.9(3) . . ? N14 C33 C52 113.6(3) . . ? N16 C33 C32 102.9(3) . . ? N14 C33 C32 102.2(3) . . ? C52 C33 C32 111.4(3) . . ? O10 C34 N15 126.0(3) . . ? O10 C34 N16 124.4(4) . . ? N15 C34 N16 109.5(3) . . ? N14 C35 N17 114.1(3) . . ? N14 C35 H35A 108.7 . . ? N17 C35 H35A 108.7 . . ? N14 C35 H35B 108.7 . . ? N17 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? N16 C36 N19 115.4(3) . . ? N16 C36 H36A 108.4 . . ? N19 C36 H36A 108.4 . . ? N16 C36 H36B 108.4 . . ? N19 C36 H36B 108.4 . . ? H36A C36 H36B 107.5 . . ? O8 C37 N17 125.4(3) . . ? O8 C37 N18 125.1(3) . . ? N17 C37 N18 109.5(3) . . ? N19 C38 N17 112.2(3) . . ? N19 C38 C53 113.7(3) . . ? N17 C38 C53 113.3(3) . . ? N19 C38 C39 102.8(3) . . ? N17 C38 C39 101.8(3) . . ? C53 C38 C39 111.9(3) . . ? N20 C39 N18 113.7(3) . . ? N20 C39 C56 112.7(3) . . ? N18 C39 C56 111.1(3) . . ? N20 C39 C38 103.1(3) . . ? N18 C39 C38 103.0(3) . . ? C56 C39 C38 112.5(3) . . ? O11 C40 N19 125.3(4) . . ? O11 C40 N20 125.8(4) . . ? N19 C40 N20 108.9(3) . . ? N18 C41 N21 114.4(3) . . ? N18 C41 H41A 108.6 . . ? N21 C41 H41A 108.6 . . ? N18 C41 H41B 108.6 . . ? N21 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? N23 C42 N20 114.0(3) . . ? N23 C42 H42A 108.8 . . ? N20 C42 H42A 108.8 . . ? N23 C42 H42B 108.8 . . ? N20 C42 H42B 108.8 . . ? H42A C42 H42B 107.6 . . ? O9 C43 N21 126.1(3) . . ? O9 C43 N22 124.8(3) . . ? N21 C43 N22 109.1(3) . . ? N23 C44 N21 112.6(3) . . ? N23 C44 C57 113.4(3) . . ? N21 C44 C57 112.1(3) . . ? N23 C44 C45 103.2(3) . . ? N21 C44 C45 102.6(3) . . ? C57 C44 C45 112.1(3) . . ? N24 C45 N22 113.0(3) . . ? N24 C45 C60 113.6(3) . . ? N22 C45 C60 112.3(3) . . ? N24 C45 C44 102.7(3) . . ? N22 C45 C44 102.6(3) . . ? C60 C45 C44 111.6(3) . . ? O12 C46 N24 126.1(4) . . ? O12 C46 N23 124.6(4) . . ? N24 C46 N23 109.2(3) . . ? N13 C47 N24 114.0(3) . 2_578 ? N13 C47 H47A 108.7 . . ? N24 C47 H47A 108.7 2_578 . ? N13 C47 H47B 108.7 . . ? N24 C47 H47B 108.7 2_578 . ? H47A C47 H47B 107.6 . . ? N22 C48 N15 113.8(3) 2_578 . ? N22 C48 H48A 108.8 2_578 . ? N15 C48 H48A 108.8 . . ? N22 C48 H48B 108.8 2_578 . ? N15 C48 H48B 108.8 . . ? H48A C48 H48B 107.7 . . ? C50 C49 C32 112.3(3) . . ? C50 C49 H49A 109.1 . . ? C32 C49 H49A 109.1 . . ? C50 C49 H49B 109.1 . . ? C32 C49 H49B 109.1 . . ? H49A C49 H49B 107.9 . . ? C49 C50 C51 112.1(3) . . ? C49 C50 H50A 109.2 . . ? C51 C50 H50A 109.2 . . ? C49 C50 H50B 109.2 . . ? C51 C50 H50B 109.2 . . ? H50A C50 H50B 107.9 . . ? C52 C51 C50 113.3(3) . . ? C52 C51 H51A 108.9 . . ? C50 C51 H51A 108.9 . . ? C52 C51 H51B 108.9 . . ? C50 C51 H51B 108.9 . . ? H51A C51 H51B 107.7 . . ? C33 C52 C51 112.8(3) . . ? C33 C52 H52A 109.0 . . ? C51 C52 H52A 109.0 . . ? C33 C52 H52B 109.0 . . ? C51 C52 H52B 109.0 . . ? H52A C52 H52B 107.8 . . ? C54 C53 C38 112.5(3) . . ? C54 C53 H53A 109.1 . . ? C38 C53 H53A 109.1 . . ? C54 C53 H53B 109.1 . . ? C38 C53 H53B 109.1 . . ? H53A C53 H53B 107.8 . . ? C53 C54 C55 113.7(3) . . ? C53 C54 H54A 108.8 . . ? C55 C54 H54A 108.8 . . ? C53 C54 H54B 108.8 . . ? C55 C54 H54B 108.8 . . ? H54A C54 H54B 107.7 . . ? C56 C55 C54 111.0(3) . . ? C56 C55 H55A 109.4 . . ? C54 C55 H55A 109.4 . . ? C56 C55 H55B 109.4 . . ? C54 C55 H55B 109.4 . . ? H55A C55 H55B 108.0 . . ? C39 C56 C55 109.4(3) . . ? C39 C56 H56A 109.8 . . ? C55 C56 H56A 109.8 . . ? C39 C56 H56B 109.8 . . ? C55 C56 H56B 109.8 . . ? H56A C56 H56B 108.2 . . ? C58 C57 C44 111.7(3) . . ? C58 C57 H57A 109.3 . . ? C44 C57 H57A 109.3 . . ? C58 C57 H57B 109.3 . . ? C44 C57 H57B 109.3 . . ? H57A C57 H57B 107.9 . . ? C57 C58 C59 112.9(3) . . ? C57 C58 H58A 109.0 . . ? C59 C58 H58A 109.0 . . ? C57 C58 H58B 109.0 . . ? C59 C58 H58B 109.0 . . ? H58A C58 H58B 107.8 . . ? C60 C59 C58 112.2(3) . . ? C60 C59 H59A 109.2 . . ? C58 C59 H59A 109.2 . . ? C60 C59 H59B 109.2 . . ? C58 C59 H59B 109.2 . . ? H59A C59 H59B 107.9 . . ? C59 C60 C45 110.4(3) . . ? C59 C60 H60A 109.6 . . ? C45 C60 H60A 109.6 . . ? C59 C60 H60B 109.6 . . ? C45 C60 H60B 109.6 . . ? H60A C60 H60B 108.1 . . ? C1 N1 C18 122.0(3) . 2_487 ? C1 N1 C2 111.4(3) . . ? C18 N1 C2 124.9(3) 2_487 . ? C1 N2 C5 123.0(3) . . ? C1 N2 C3 112.7(3) . . ? C5 N2 C3 124.2(3) . . ? C4 N3 C2 112.5(3) . . ? C4 N3 C17 121.7(3) . 2_487 ? C2 N3 C17 125.6(3) . 2_487 ? C4 N4 C3 113.2(3) . . ? C4 N4 C6 121.4(3) . . ? C3 N4 C6 124.6(3) . . ? C7 N5 C5 121.9(3) . . ? C7 N5 C8 112.3(3) . . ? C5 N5 C8 125.8(3) . . ? C7 N6 C11 121.3(3) . . ? C7 N6 C9 111.1(3) . . ? C11 N6 C9 125.3(3) . . ? C10 N7 C6 120.8(3) . . ? C10 N7 C8 112.0(3) . . ? C6 N7 C8 126.1(3) . . ? C10 N8 C9 112.4(3) . . ? C10 N8 C12 121.0(3) . . ? C9 N8 C12 126.4(3) . . ? C13 N9 C11 121.0(3) . . ? C13 N9 C14 113.1(3) . . ? C11 N9 C14 124.8(3) . . ? C13 N10 C15 113.3(3) . . ? C13 N10 C17 121.2(3) . . ? C15 N10 C17 124.4(3) . . ? C16 N11 C14 112.5(3) . . ? C16 N11 C12 121.3(3) . . ? C14 N11 C12 125.0(3) . . ? C16 N12 C18 121.8(3) . . ? C16 N12 C15 112.8(3) . . ? C18 N12 C15 123.7(3) . . ? C31 N13 C32 113.1(3) . . ? C31 N13 C47 121.6(3) . . ? C32 N13 C47 124.9(3) . . ? C31 N14 C35 119.9(3) . . ? C31 N14 C33 112.2(3) . . ? C35 N14 C33 124.6(3) . . ? C34 N15 C48 120.9(3) . . ? C34 N15 C32 113.0(3) . . ? C48 N15 C32 124.4(3) . . ? C34 N16 C36 122.4(3) . . ? C34 N16 C33 112.4(3) . . ? C36 N16 C33 124.7(3) . . ? C37 N17 C35 120.9(3) . . ? C37 N17 C38 112.8(3) . . ? C35 N17 C38 124.2(3) . . ? C37 N18 C41 122.8(3) . . ? C37 N18 C39 112.3(3) . . ? C41 N18 C39 124.8(3) . . ? C40 N19 C38 112.5(3) . . ? C40 N19 C36 121.5(3) . . ? C38 N19 C36 125.7(3) . . ? C40 N20 C39 112.4(3) . . ? C40 N20 C42 121.6(3) . . ? C39 N20 C42 125.0(3) . . ? C43 N21 C44 113.1(3) . . ? C43 N21 C41 121.8(3) . . ? C44 N21 C41 125.1(3) . . ? C43 N22 C48 120.6(3) . 2_578 ? C43 N22 C45 112.3(3) . . ? C48 N22 C45 125.0(3) 2_578 . ? C46 N23 C42 121.6(3) . . ? C46 N23 C44 111.5(3) . . ? C42 N23 C44 125.6(3) . . ? C46 N24 C45 112.7(3) . . ? C46 N24 C47 121.8(3) . 2_578 ? C45 N24 C47 125.2(3) . 2_578 ? C1 O1 Y1 155.4(2) . . ? C7 O2 Y1 155.8(3) . . ? C37 O8 Y1 158.6(2) . . ? C43 O9 Y1 156.1(2) . . ? O15 N25 O14 120.8(6) . . ? O15 N25 O13 119.1(6) . . ? O14 N25 O13 120.1(6) . . ? O17 N26 O18 118.3(7) . . ? O17 N26 O16 122.6(8) . . ? O18 N26 O16 119.0(5) . . ? O19 N27 O21 119.9(4) . . ? O19 N27 O20 120.2(4) . . ? O21 N27 O20 119.8(4) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.045 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.082 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 108 22 ' ' 2 0.225 0.126 0.720 206 71 ' ' 3 -0.224 0.873 0.280 204 71 ' ' 4 0.161 0.542 0.347 58 20 ' ' 5 0.500 0.500 0.000 116 29 ' ' 6 0.469 0.515 0.343 17 9 ' ' 7 0.541 0.484 0.659 18 9 ' ' 8 0.846 0.457 0.652 57 19 ' ' _platon_squeeze_details ; ; data_a2 _database_code_depnum_ccdc_archive 'CCDC 881898' #TrackingRef '110104qx-submit-cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H106 N27 O38 Sm' _chemical_formula_weight 1964.07 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.8719(8) _cell_length_b 15.9679(8) _cell_length_c 18.3263(9) _cell_angle_alpha 74.450(2) _cell_angle_beta 88.987(2) _cell_angle_gamma 63.323(2) _cell_volume 3969.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2042 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7901 _exptl_absorpt_correction_T_max 0.8413 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42684 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 25.10 _reflns_number_total 13919 _reflns_number_gt 12237 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+5.5485P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13919 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1W O 0.60099(19) 0.38115(19) 0.74789(16) 0.0284(6) Uani 1 1 d . . . O2W O 0.7426(2) 0.04521(19) 0.78771(15) 0.0280(6) Uani 1 1 d . . . O3W O 0.55581(19) 0.2236(2) 0.76543(15) 0.0283(6) Uani 1 1 d . . . O4W O 0.8810(2) 0.1118(2) 0.77472(18) 0.0349(7) Uani 1 1 d . . . Sm1 Sm 0.714256(13) 0.213179(14) 0.764771(10) 0.02116(8) Uani 1 1 d . . . C1 C 0.7998(2) 0.3324(3) 0.61019(19) 0.0175(7) Uani 1 1 d . . . C2 C 0.8760(3) 0.3162(3) 0.5006(2) 0.0208(8) Uani 1 1 d . . . C3 C 0.8590(3) 0.4151(3) 0.5150(2) 0.0210(8) Uani 1 1 d . . . C4 C 0.7798(3) 0.4481(3) 0.3953(2) 0.0220(8) Uani 1 1 d . . . C5 C 0.7888(3) 0.4841(3) 0.6275(2) 0.0206(8) Uani 1 1 d . . . H5A H 0.7836 0.4519 0.6798 0.025 Uiso 1 1 calc R . . H5B H 0.8437 0.4966 0.6292 0.025 Uiso 1 1 calc R . . C6 C 0.7692(3) 0.5923(3) 0.4260(2) 0.0236(8) Uani 1 1 d . . . H6A H 0.7520 0.6201 0.3706 0.028 Uiso 1 1 calc R . . H6B H 0.8229 0.6021 0.4393 0.028 Uiso 1 1 calc R . . C7 C 0.6276(3) 0.6012(3) 0.6399(2) 0.0220(8) Uani 1 1 d . . . C8 C 0.6964(3) 0.6602(3) 0.5372(2) 0.0206(8) Uani 1 1 d . . . C9 C 0.5946(3) 0.7434(3) 0.5391(2) 0.0212(8) Uani 1 1 d . . . C10 C 0.6006(3) 0.7048(3) 0.4236(2) 0.0226(8) Uani 1 1 d . . . C11 C 0.4775(3) 0.7451(3) 0.6391(2) 0.0245(8) Uani 1 1 d . . . H11A H 0.4728 0.8081 0.6403 0.029 Uiso 1 1 calc R . . H11B H 0.4852 0.7056 0.6921 0.029 Uiso 1 1 calc R . . C12 C 0.4516(3) 0.8415(3) 0.4349(2) 0.0197(7) Uani 1 1 d . . . H12A H 0.4456 0.8544 0.3793 0.024 Uiso 1 1 calc R . . H12B H 0.4486 0.8996 0.4456 0.024 Uiso 1 1 calc R . . C13 C 0.3437(3) 0.7090(3) 0.6313(2) 0.0236(8) Uani 1 1 d . . . C14 C 0.3334(3) 0.8447(3) 0.5342(2) 0.0193(7) Uani 1 1 d . . . C15 C 0.2381(3) 0.8373(3) 0.5286(2) 0.0203(8) Uani 1 1 d . . . C16 C 0.3114(2) 0.8175(2) 0.41794(19) 0.0158(7) Uani 1 1 d . . . C17 C 0.1881(3) 0.7134(3) 0.6141(2) 0.0234(8) Uani 1 1 d . . . H17A H 0.2046 0.6768 0.6685 0.028 Uiso 1 1 calc R . . H17B H 0.1252 0.7696 0.6079 0.028 Uiso 1 1 calc R . . C18 C 0.1546(3) 0.8235(3) 0.4164(2) 0.0187(7) Uani 1 1 d . . . H18A H 0.1516 0.8489 0.3610 0.022 Uiso 1 1 calc R . . H18B H 0.0958 0.8677 0.4321 0.022 Uiso 1 1 calc R . . C19 C 0.9805(3) 0.2507(3) 0.4968(2) 0.0280(9) Uani 1 1 d . . . H19A H 1.0015 0.2820 0.4518 0.034 Uiso 1 1 calc R . . H19B H 0.9884 0.1880 0.4919 0.034 Uiso 1 1 calc R . . C20 C 1.0418(3) 0.2322(3) 0.5685(3) 0.0342(10) Uani 1 1 d . . . H20A H 1.0326 0.1858 0.6111 0.041 Uiso 1 1 calc R . . H20B H 1.1088 0.2016 0.5601 0.041 Uiso 1 1 calc R . . C21 C 1.0193(3) 0.3251(3) 0.5906(2) 0.0329(10) Uani 1 1 d . . . H21A H 1.0785 0.3281 0.5993 0.040 Uiso 1 1 calc R . . H21B H 0.9907 0.3223 0.6385 0.040 Uiso 1 1 calc R . . C22 C 0.9515(3) 0.4180(3) 0.5291(2) 0.0264(8) Uani 1 1 d . . . H22A H 0.9387 0.4757 0.5455 0.032 Uiso 1 1 calc R . . H22B H 0.9809 0.4230 0.4817 0.032 Uiso 1 1 calc R . . C23 C 0.7735(3) 0.6901(3) 0.5477(2) 0.0282(9) Uani 1 1 d . . . H23A H 0.8362 0.6339 0.5527 0.034 Uiso 1 1 calc R . . H23B H 0.7683 0.7424 0.5025 0.034 Uiso 1 1 calc R . . C24 C 0.7648(3) 0.7255(3) 0.6179(3) 0.0380(11) Uani 1 1 d . . . H24A H 0.8127 0.7476 0.6210 0.046 Uiso 1 1 calc R . . H24B H 0.7775 0.6707 0.6635 0.046 Uiso 1 1 calc R . . C25 C 0.6654(3) 0.8100(3) 0.6162(3) 0.0385(11) Uani 1 1 d . . . H25A H 0.6385 0.7920 0.6629 0.046 Uiso 1 1 calc R . . H25B H 0.6717 0.8685 0.6158 0.046 Uiso 1 1 calc R . . C26 C 0.5972(3) 0.8346(3) 0.5473(2) 0.0284(9) Uani 1 1 d . . . H26A H 0.5333 0.8820 0.5528 0.034 Uiso 1 1 calc R . . H26B H 0.6172 0.8648 0.5010 0.034 Uiso 1 1 calc R . . C27 C 0.3153(3) 0.9435(3) 0.5421(2) 0.0293(9) Uani 1 1 d . . . H27A H 0.2799 0.9950 0.4949 0.035 Uiso 1 1 calc R . . H27B H 0.3760 0.9437 0.5504 0.035 Uiso 1 1 calc R . . C28 C 0.2583(4) 0.9649(4) 0.6095(3) 0.0471(13) Uani 1 1 d . . . H28A H 0.2994 0.9214 0.6573 0.057 Uiso 1 1 calc R . . H28B H 0.2401 1.0325 0.6090 0.057 Uiso 1 1 calc R . . C29 C 0.1691(4) 0.9517(4) 0.6084(3) 0.0438(12) Uani 1 1 d . . . H29A H 0.1142 1.0119 0.6115 0.053 Uiso 1 1 calc R . . H29B H 0.1753 0.8985 0.6533 0.053 Uiso 1 1 calc R . . C30 C 0.1516(3) 0.9281(3) 0.5363(2) 0.0297(9) Uani 1 1 d . . . H30A H 0.0957 0.9167 0.5389 0.036 Uiso 1 1 calc R . . H30B H 0.1391 0.9838 0.4914 0.036 Uiso 1 1 calc R . . C31 C 0.6874(2) 0.1667(3) 0.96225(19) 0.0165(7) Uani 1 1 d . . . C32 C 0.6698(2) 0.1219(2) 1.09172(19) 0.0162(7) Uani 1 1 d . . . C33 C 0.6655(2) 0.2262(2) 1.06801(19) 0.0165(7) Uani 1 1 d . . . C34 C 0.7960(3) 0.1163(3) 1.1618(2) 0.0204(8) Uani 1 1 d . . . C35 C 0.6631(2) 0.3355(3) 0.9360(2) 0.0180(7) Uani 1 1 d . . . H35A H 0.6178 0.3899 0.9538 0.022 Uiso 1 1 calc R . . H35B H 0.6370 0.3441 0.8849 0.022 Uiso 1 1 calc R . . C36 C 0.7759(3) 0.2847(3) 1.11570(19) 0.0209(8) Uani 1 1 d . . . H36A H 0.7175 0.3447 1.1132 0.025 Uiso 1 1 calc R . . H36B H 0.8131 0.2641 1.1651 0.025 Uiso 1 1 calc R . . C37 C 0.8087(2) 0.3136(2) 0.87659(19) 0.0168(7) Uani 1 1 d . . . C38 C 0.7900(2) 0.3761(3) 0.9813(2) 0.0187(7) Uani 1 1 d . . . C39 C 0.8802(2) 0.3757(2) 0.9435(2) 0.0176(7) Uani 1 1 d . . . C40 C 0.9254(3) 0.2754(3) 1.0705(2) 0.0214(8) Uani 1 1 d . . . C41 C 0.9471(2) 0.3250(3) 0.8233(2) 0.0191(7) Uani 1 1 d . . . H41A H 0.9176 0.3206 0.7789 0.023 Uiso 1 1 calc R . . H41B H 0.9516 0.3864 0.8080 0.023 Uiso 1 1 calc R . . C42 C 1.0531(2) 0.2975(3) 1.0048(2) 0.0201(7) Uani 1 1 d . . . H42A H 1.0819 0.2774 1.0574 0.024 Uiso 1 1 calc R . . H42B H 1.0527 0.3597 0.9782 0.024 Uiso 1 1 calc R . . C43 C 1.0727(2) 0.1719(3) 0.81002(19) 0.0178(7) Uani 1 1 d . . . C44 C 1.1201(2) 0.2427(3) 0.8879(2) 0.0170(7) Uani 1 1 d . . . C45 C 1.2075(2) 0.1451(3) 0.8830(2) 0.0183(7) Uani 1 1 d . . . C46 C 1.1737(3) 0.1312(3) 1.0098(2) 0.0215(8) Uani 1 1 d . . . C47 C 1.2229(3) 0.0340(3) 0.7989(2) 0.0212(8) Uani 1 1 d . . . H47A H 1.2809 0.0381 0.7843 0.025 Uiso 1 1 calc R . . H47B H 1.1862 0.0438 0.7521 0.025 Uiso 1 1 calc R . . C48 C 0.6862(2) 0.0087(2) 1.0090(2) 0.0184(7) Uani 1 1 d . . . H48A H 0.6334 0.0017 1.0335 0.022 Uiso 1 1 calc R . . H48B H 0.6730 0.0205 0.9542 0.022 Uiso 1 1 calc R . . C49 C 0.5771(3) 0.1257(3) 1.1187(2) 0.0233(8) Uani 1 1 d . . . H49A H 0.5268 0.1624 1.0755 0.028 Uiso 1 1 calc R . . H49B H 0.5845 0.0589 1.1366 0.028 Uiso 1 1 calc R . . C50 C 0.5473(3) 0.1736(3) 1.1825(2) 0.0312(9) Uani 1 1 d . . . H50A H 0.5850 0.1262 1.2306 0.037 Uiso 1 1 calc R . . H50B H 0.4804 0.1906 1.1878 0.037 Uiso 1 1 calc R . . C51 C 0.5597(3) 0.2658(3) 1.1693(2) 0.0277(9) Uani 1 1 d . . . H51A H 0.5031 0.3170 1.1818 0.033 Uiso 1 1 calc R . . H51B H 0.6143 0.2514 1.2035 0.033 Uiso 1 1 calc R . . C52 C 0.5749(3) 0.3035(3) 1.0869(2) 0.0229(8) Uani 1 1 d . . . H52A H 0.5205 0.3182 1.0523 0.027 Uiso 1 1 calc R . . H52B H 0.5800 0.3640 1.0800 0.027 Uiso 1 1 calc R . . C53 C 0.7187(3) 0.4786(3) 0.9839(2) 0.0259(8) Uani 1 1 d . . . H53A H 0.6619 0.4766 1.0044 0.031 Uiso 1 1 calc R . . H53B H 0.7469 0.4993 1.0184 0.031 Uiso 1 1 calc R . . C54 C 0.6901(3) 0.5533(3) 0.9049(3) 0.0352(10) Uani 1 1 d . . . H54A H 0.6558 0.6194 0.9104 0.042 Uiso 1 1 calc R . . H54B H 0.6468 0.5432 0.8750 0.042 Uiso 1 1 calc R . . C55 C 0.7756(3) 0.5458(3) 0.8616(3) 0.0358(10) Uani 1 1 d . . . H55A H 0.7743 0.5206 0.8186 0.043 Uiso 1 1 calc R . . H55B H 0.7707 0.6113 0.8409 0.043 Uiso 1 1 calc R . . C56 C 0.8700(3) 0.4787(3) 0.9125(2) 0.0264(8) Uani 1 1 d . . . H56A H 0.9226 0.4768 0.8830 0.032 Uiso 1 1 calc R . . H56B H 0.8726 0.5042 0.9550 0.032 Uiso 1 1 calc R . . C57 C 1.1351(3) 0.3328(3) 0.8540(2) 0.0250(8) Uani 1 1 d . . . H57A H 1.0751 0.3921 0.8493 0.030 Uiso 1 1 calc R . . H57B H 1.1817 0.3326 0.8884 0.030 Uiso 1 1 calc R . . C58 C 1.1696(3) 0.3344(3) 0.7763(2) 0.0298(9) Uani 1 1 d . . . H58A H 1.1787 0.3928 0.7564 0.036 Uiso 1 1 calc R . . H58B H 1.1210 0.3388 0.7411 0.036 Uiso 1 1 calc R . . C59 C 1.2634(3) 0.2427(3) 0.7791(2) 0.0356(10) Uani 1 1 d . . . H59A H 1.2576 0.2165 0.7379 0.043 Uiso 1 1 calc R . . H59B H 1.3143 0.2617 0.7700 0.043 Uiso 1 1 calc R . . C60 C 1.2911(3) 0.1624(3) 0.8548(2) 0.0246(8) Uani 1 1 d . . . H60A H 1.3161 0.1805 0.8933 0.029 Uiso 1 1 calc R . . H60B H 1.3417 0.1013 0.8487 0.029 Uiso 1 1 calc R . . N1 N 0.8403(2) 0.2731(2) 0.56569(17) 0.0197(6) Uani 1 1 d . . . N2 N 0.8062(2) 0.4175(2) 0.58185(16) 0.0187(6) Uani 1 1 d . . . N3 N 0.8166(2) 0.3495(2) 0.42851(17) 0.0218(7) Uani 1 1 d . . . N4 N 0.7996(2) 0.4883(2) 0.44553(17) 0.0213(7) Uani 1 1 d . . . N5 N 0.7039(2) 0.5773(2) 0.59993(17) 0.0213(7) Uani 1 1 d . . . N6 N 0.5617(2) 0.6957(2) 0.60465(17) 0.0219(7) Uani 1 1 d . . . N7 N 0.6897(2) 0.6457(2) 0.46289(17) 0.0216(7) Uani 1 1 d . . . N8 N 0.5437(2) 0.7594(2) 0.46686(17) 0.0199(6) Uani 1 1 d . . . N9 N 0.3886(2) 0.7633(2) 0.60092(17) 0.0215(7) Uani 1 1 d . . . N10 N 0.2571(2) 0.7492(2) 0.59031(17) 0.0224(7) Uani 1 1 d . . . N11 N 0.3713(2) 0.8279(2) 0.46325(16) 0.0187(6) Uani 1 1 d . . . N12 N 0.2344(2) 0.8243(2) 0.45297(16) 0.0184(6) Uani 1 1 d . . . N13 N 0.6898(2) 0.0934(2) 1.02117(16) 0.0169(6) Uani 1 1 d . . . N14 N 0.6717(2) 0.2448(2) 0.98648(16) 0.0174(6) Uani 1 1 d . . . N15 N 0.7505(2) 0.0643(2) 1.15117(16) 0.0186(6) Uani 1 1 d . . . N16 N 0.7508(2) 0.2086(2) 1.11172(17) 0.0186(6) Uani 1 1 d . . . N17 N 0.7521(2) 0.3412(2) 0.93047(16) 0.0165(6) Uani 1 1 d . . . N18 N 0.8851(2) 0.3291(2) 0.88361(16) 0.0161(6) Uani 1 1 d . . . N19 N 0.8294(2) 0.3063(2) 1.05589(16) 0.0202(6) Uani 1 1 d . . . N20 N 0.9559(2) 0.3131(2) 1.00592(17) 0.0195(6) Uani 1 1 d . . . N21 N 1.0421(2) 0.2442(2) 0.84404(16) 0.0169(6) Uani 1 1 d . . . N22 N 1.1678(2) 0.1129(2) 0.83120(17) 0.0191(6) Uani 1 1 d . . . N23 N 1.1114(2) 0.2244(2) 0.96809(17) 0.0190(6) Uani 1 1 d . . . N24 N 1.2273(2) 0.0825(2) 0.96162(16) 0.0168(6) Uani 1 1 d . . . O1 O 0.76470(19) 0.31277(19) 0.66891(14) 0.0229(6) Uani 1 1 d . . . O2 O 0.6203(2) 0.5485(2) 0.69954(15) 0.0289(6) Uani 1 1 d . . . O3 O 0.3742(2) 0.6382(2) 0.68835(15) 0.0323(7) Uani 1 1 d . . . O4 O 0.7364(2) 0.4933(2) 0.33152(15) 0.0305(6) Uani 1 1 d . . . O5 O 0.5777(2) 0.7070(2) 0.35895(15) 0.0288(6) Uani 1 1 d . . . O6 O 0.32510(18) 0.80592(19) 0.35416(13) 0.0205(5) Uani 1 1 d . . . O7 O 0.69642(18) 0.16377(19) 0.89558(13) 0.0213(5) Uani 1 1 d . . . O8 O 0.79263(18) 0.2811(2) 0.82724(14) 0.0227(6) Uani 1 1 d . . . O9 O 1.02373(18) 0.16190(19) 0.76482(15) 0.0247(6) Uani 1 1 d . . . O10 O 0.8640(2) 0.0857(2) 1.20862(16) 0.0320(7) Uani 1 1 d . . . O11 O 0.9731(2) 0.2251(2) 1.13158(15) 0.0303(6) Uani 1 1 d . . . O12 O 1.1794(2) 0.0983(2) 1.07909(15) 0.0308(6) Uani 1 1 d . . . N25 N 0.0111(3) 0.4401(3) 0.3043(2) 0.0377(9) Uani 1 1 d . . . N26 N 0.5984(4) 0.9353(3) 0.3369(3) 0.0506(11) Uani 1 1 d . . . N27 N 0.5652(3) 0.7180(3) 0.0849(2) 0.0468(10) Uani 1 1 d . . . O13 O 0.0484(3) 0.4491(3) 0.2448(2) 0.0606(10) Uani 1 1 d . . . O14 O -0.0262(3) 0.3864(4) 0.3180(3) 0.0782(13) Uani 1 1 d . . . O15 O 0.0127(3) 0.4851(3) 0.3490(2) 0.0729(13) Uani 1 1 d . . . O16 O 0.5383(3) 0.9958(3) 0.3684(2) 0.0665(11) Uani 1 1 d . . . O17 O 0.6772(3) 0.8721(3) 0.3705(3) 0.0709(12) Uani 1 1 d . . . O18 O 0.5759(4) 0.9422(4) 0.2714(3) 0.0855(15) Uani 1 1 d . . . O19 O 0.5472(5) 0.6710(4) 0.1419(3) 0.0982(19) Uani 1 1 d . . . O20 O 0.5272(3) 0.8079(3) 0.0686(2) 0.0659(11) Uani 1 1 d . . . O21 O 0.6203(4) 0.6762(4) 0.0432(3) 0.0943(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.0285(14) 0.0228(14) 0.0298(15) -0.0018(12) 0.0019(12) -0.0117(12) O2W 0.0389(16) 0.0211(14) 0.0229(14) -0.0015(11) -0.0027(12) -0.0154(12) O3W 0.0258(14) 0.0384(16) 0.0234(14) -0.0076(12) 0.0020(11) -0.0179(13) O4W 0.0245(15) 0.0350(16) 0.0473(19) -0.0131(14) 0.0025(13) -0.0149(13) Sm1 0.02580(12) 0.02529(12) 0.01523(11) -0.00447(8) 0.00235(8) -0.01496(9) C1 0.0163(17) 0.0221(18) 0.0151(17) -0.0025(15) -0.0004(14) -0.0113(15) C2 0.0206(18) 0.0234(19) 0.0171(18) -0.0018(15) 0.0024(15) -0.0113(16) C3 0.0218(19) 0.0227(19) 0.0168(18) 0.0016(15) 0.0027(15) -0.0127(16) C4 0.0207(18) 0.030(2) 0.0156(18) -0.0057(16) 0.0097(15) -0.0132(17) C5 0.0257(19) 0.0205(18) 0.0155(17) -0.0038(15) 0.0000(15) -0.0112(16) C6 0.027(2) 0.0224(19) 0.0204(19) -0.0003(16) 0.0043(16) -0.0137(17) C7 0.027(2) 0.0220(19) 0.0210(19) -0.0080(16) -0.0022(16) -0.0134(16) C8 0.0249(19) 0.0227(19) 0.0157(18) -0.0008(15) 0.0000(15) -0.0147(16) C9 0.0263(19) 0.0221(19) 0.0170(18) -0.0018(15) -0.0034(15) -0.0146(16) C10 0.0240(19) 0.0206(19) 0.023(2) 0.0006(16) -0.0009(16) -0.0135(16) C11 0.027(2) 0.031(2) 0.0159(18) -0.0103(16) 0.0017(15) -0.0114(17) C12 0.0228(19) 0.0198(18) 0.0159(17) -0.0006(15) -0.0014(14) -0.0117(15) C13 0.034(2) 0.022(2) 0.0161(19) -0.0097(17) 0.0058(16) -0.0115(17) C14 0.0251(19) 0.0179(18) 0.0139(17) -0.0064(15) 0.0036(15) -0.0082(15) C15 0.0258(19) 0.0192(18) 0.0145(17) -0.0056(15) 0.0010(15) -0.0087(16) C16 0.0208(18) 0.0120(16) 0.0130(17) -0.0004(14) 0.0009(14) -0.0079(14) C17 0.028(2) 0.030(2) 0.0122(17) -0.0066(16) 0.0093(15) -0.0138(17) C18 0.0200(18) 0.0177(18) 0.0161(17) -0.0002(14) -0.0002(14) -0.0094(15) C19 0.0207(19) 0.032(2) 0.030(2) -0.0061(18) 0.0100(17) -0.0129(17) C20 0.019(2) 0.035(2) 0.039(2) 0.000(2) -0.0003(18) -0.0098(18) C21 0.022(2) 0.044(3) 0.032(2) -0.002(2) -0.0018(17) -0.0203(19) C22 0.023(2) 0.032(2) 0.028(2) -0.0042(18) 0.0040(16) -0.0188(17) C23 0.025(2) 0.026(2) 0.034(2) -0.0028(18) -0.0025(17) -0.0159(17) C24 0.044(3) 0.038(2) 0.038(3) -0.011(2) -0.012(2) -0.024(2) C25 0.043(3) 0.040(3) 0.040(3) -0.014(2) -0.008(2) -0.024(2) C26 0.033(2) 0.024(2) 0.031(2) -0.0075(17) -0.0035(18) -0.0155(18) C27 0.036(2) 0.021(2) 0.031(2) -0.0105(17) -0.0015(18) -0.0119(18) C28 0.053(3) 0.040(3) 0.042(3) -0.028(2) -0.003(2) -0.007(2) C29 0.060(3) 0.036(3) 0.036(3) -0.025(2) 0.019(2) -0.014(2) C30 0.030(2) 0.024(2) 0.029(2) -0.0088(18) 0.0080(18) -0.0070(17) C31 0.0154(17) 0.0200(18) 0.0143(17) -0.0033(14) 0.0009(13) -0.0093(14) C32 0.0162(17) 0.0161(17) 0.0117(16) -0.0015(14) 0.0034(14) -0.0049(14) C33 0.0172(17) 0.0167(17) 0.0149(17) -0.0060(14) 0.0043(14) -0.0064(14) C34 0.0211(19) 0.0224(19) 0.0155(18) -0.0076(15) 0.0048(15) -0.0069(16) C35 0.0177(17) 0.0185(18) 0.0148(17) 0.0000(14) -0.0011(14) -0.0085(15) C36 0.031(2) 0.0248(19) 0.0112(17) -0.0059(15) 0.0015(15) -0.0165(17) C37 0.0196(17) 0.0154(17) 0.0129(17) 0.0000(14) -0.0001(14) -0.0081(14) C38 0.0186(18) 0.0205(18) 0.0192(18) -0.0074(15) 0.0036(15) -0.0101(15) C39 0.0207(18) 0.0150(17) 0.0168(17) -0.0043(14) 0.0010(14) -0.0081(15) C40 0.0242(19) 0.0228(19) 0.0196(19) -0.0109(16) 0.0020(16) -0.0102(16) C41 0.0186(18) 0.0208(18) 0.0147(17) -0.0033(15) 0.0020(14) -0.0074(15) C42 0.0192(18) 0.0225(19) 0.0205(18) -0.0102(16) 0.0018(15) -0.0091(15) C43 0.0180(17) 0.0190(18) 0.0144(17) 0.0006(14) 0.0030(14) -0.0098(15) C44 0.0163(17) 0.0176(18) 0.0171(17) -0.0041(15) 0.0015(14) -0.0083(15) C45 0.0184(18) 0.0170(18) 0.0175(18) -0.0008(15) -0.0010(14) -0.0088(15) C46 0.0192(18) 0.0243(19) 0.020(2) -0.0043(16) 0.0003(15) -0.0105(16) C47 0.0263(19) 0.0189(18) 0.0123(17) -0.0025(15) 0.0039(15) -0.0067(16) C48 0.0169(17) 0.0164(17) 0.0190(18) -0.0039(15) -0.0032(14) -0.0058(14) C49 0.0200(19) 0.028(2) 0.0195(19) -0.0040(16) 0.0052(15) -0.0108(16) C50 0.032(2) 0.037(2) 0.022(2) -0.0078(18) 0.0134(17) -0.0143(19) C51 0.024(2) 0.033(2) 0.0199(19) -0.0125(17) 0.0084(16) -0.0059(17) C52 0.0202(19) 0.0212(19) 0.0207(19) -0.0064(16) 0.0038(15) -0.0039(15) C53 0.024(2) 0.024(2) 0.031(2) -0.0136(17) 0.0071(17) -0.0088(17) C54 0.030(2) 0.021(2) 0.044(3) -0.0065(19) 0.000(2) -0.0046(17) C55 0.039(2) 0.021(2) 0.034(2) 0.0015(18) 0.002(2) -0.0079(19) C56 0.030(2) 0.0179(19) 0.034(2) -0.0077(17) 0.0060(17) -0.0130(17) C57 0.025(2) 0.0193(19) 0.032(2) -0.0035(17) 0.0033(17) -0.0127(16) C58 0.032(2) 0.027(2) 0.028(2) -0.0004(17) 0.0055(17) -0.0159(18) C59 0.037(2) 0.034(2) 0.028(2) 0.0011(19) 0.0106(19) -0.015(2) C60 0.0185(18) 0.027(2) 0.026(2) -0.0023(17) 0.0040(16) -0.0115(16) N1 0.0217(16) 0.0221(16) 0.0163(15) -0.0024(13) 0.0033(12) -0.0127(13) N2 0.0245(16) 0.0217(16) 0.0148(15) -0.0054(13) 0.0060(12) -0.0149(13) N3 0.0240(16) 0.0246(17) 0.0166(15) -0.0043(13) 0.0040(13) -0.0121(14) N4 0.0230(16) 0.0232(16) 0.0150(15) -0.0008(13) 0.0004(13) -0.0110(14) N5 0.0242(16) 0.0187(16) 0.0188(16) -0.0009(13) 0.0011(13) -0.0104(13) N6 0.0275(17) 0.0224(16) 0.0148(15) -0.0037(13) 0.0018(13) -0.0116(14) N7 0.0230(16) 0.0242(16) 0.0152(15) -0.0006(13) -0.0028(13) -0.0116(14) N8 0.0217(16) 0.0237(16) 0.0147(15) -0.0033(13) -0.0008(12) -0.0118(13) N9 0.0246(16) 0.0247(17) 0.0128(15) -0.0035(13) -0.0013(12) -0.0103(14) N10 0.0326(18) 0.0256(17) 0.0123(15) -0.0048(13) 0.0022(13) -0.0166(15) N11 0.0246(16) 0.0254(16) 0.0118(14) -0.0067(13) 0.0038(12) -0.0157(14) N12 0.0202(15) 0.0235(16) 0.0115(14) -0.0048(12) 0.0009(12) -0.0102(13) N13 0.0201(15) 0.0189(15) 0.0125(14) -0.0055(12) 0.0032(12) -0.0092(13) N14 0.0225(15) 0.0170(15) 0.0112(14) -0.0035(12) 0.0041(12) -0.0082(13) N15 0.0201(15) 0.0211(16) 0.0122(14) -0.0026(12) -0.0003(12) -0.0087(13) N16 0.0210(15) 0.0196(15) 0.0163(15) -0.0061(13) 0.0010(12) -0.0098(13) N17 0.0174(15) 0.0210(15) 0.0136(14) -0.0068(12) 0.0025(12) -0.0100(13) N18 0.0160(14) 0.0192(15) 0.0137(14) -0.0051(12) 0.0015(12) -0.0085(12) N19 0.0224(16) 0.0262(17) 0.0128(14) -0.0035(13) 0.0017(12) -0.0130(14) N20 0.0191(15) 0.0230(16) 0.0162(15) -0.0083(13) 0.0017(12) -0.0082(13) N21 0.0157(14) 0.0182(15) 0.0161(15) -0.0048(12) -0.0006(12) -0.0071(12) N22 0.0176(15) 0.0205(16) 0.0164(15) -0.0081(13) 0.0001(12) -0.0047(13) N23 0.0181(15) 0.0205(16) 0.0154(15) -0.0048(13) 0.0013(12) -0.0065(13) N24 0.0169(15) 0.0150(14) 0.0148(15) -0.0029(12) 0.0028(12) -0.0051(12) O1 0.0317(14) 0.0262(14) 0.0156(13) -0.0050(11) 0.0078(11) -0.0181(12) O2 0.0382(16) 0.0262(15) 0.0206(14) -0.0014(12) 0.0074(12) -0.0165(13) O3 0.0422(17) 0.0294(15) 0.0179(14) 0.0044(12) -0.0044(12) -0.0163(14) O4 0.0348(16) 0.0304(15) 0.0203(14) -0.0017(12) -0.0002(12) -0.0129(13) O5 0.0307(15) 0.0378(16) 0.0156(13) -0.0071(12) -0.0025(11) -0.0141(13) O6 0.0252(13) 0.0289(14) 0.0120(12) -0.0071(11) 0.0039(10) -0.0158(12) O7 0.0286(14) 0.0262(14) 0.0123(12) -0.0063(11) 0.0051(10) -0.0152(12) O8 0.0251(14) 0.0340(15) 0.0166(13) -0.0119(12) 0.0050(11) -0.0178(12) O9 0.0216(13) 0.0282(14) 0.0248(14) -0.0099(12) -0.0007(11) -0.0106(11) O10 0.0343(16) 0.0286(15) 0.0278(15) -0.0032(12) -0.0105(13) -0.0123(13) O11 0.0293(15) 0.0381(16) 0.0181(14) -0.0023(13) -0.0044(12) -0.0141(13) O12 0.0342(16) 0.0288(15) 0.0173(14) -0.0025(12) 0.0033(12) -0.0066(13) N25 0.032(2) 0.045(2) 0.028(2) -0.0002(17) -0.0045(16) -0.0158(18) N26 0.084(4) 0.047(3) 0.043(3) -0.018(2) 0.024(3) -0.047(3) N27 0.052(3) 0.052(3) 0.040(2) -0.020(2) 0.011(2) -0.023(2) O13 0.056(2) 0.064(3) 0.045(2) 0.0038(19) 0.0151(18) -0.023(2) O14 0.088(3) 0.103(4) 0.065(3) -0.006(3) 0.018(2) -0.072(3) O15 0.061(3) 0.089(3) 0.062(3) -0.039(2) -0.015(2) -0.019(2) O16 0.082(3) 0.062(3) 0.056(2) -0.030(2) 0.023(2) -0.027(2) O17 0.071(3) 0.066(3) 0.068(3) -0.016(2) 0.003(2) -0.027(2) O18 0.102(4) 0.083(3) 0.048(3) -0.023(2) 0.000(2) -0.021(3) O19 0.153(5) 0.064(3) 0.089(4) -0.031(3) 0.076(4) -0.057(3) O20 0.071(3) 0.051(3) 0.066(3) -0.017(2) 0.002(2) -0.021(2) O21 0.122(4) 0.074(3) 0.084(3) -0.041(3) 0.061(3) -0.034(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 O1W Sm1 2.401(3) . ? O2W Sm1 2.427(3) . ? O3W Sm1 2.444(3) . ? O4W Sm1 2.381(3) . ? Sm1 O7 2.369(2) . ? Sm1 O6 2.410(2) 2_666 ? Sm1 O1 2.419(2) . ? Sm1 O8 2.441(2) . ? C1 O1 1.233(4) . ? C1 N1 1.350(5) . ? C1 N2 1.368(4) . ? C2 N1 1.450(5) . ? C2 N3 1.462(5) . ? C2 C19 1.525(5) . ? C2 C3 1.572(5) . ? C3 N4 1.460(5) . ? C3 N2 1.471(5) . ? C3 C22 1.518(5) . ? C4 O4 1.220(5) . ? C4 N3 1.365(5) . ? C4 N4 1.366(5) . ? C5 N5 1.451(5) . ? C5 N2 1.454(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.444(5) . ? C6 N7 1.446(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.227(5) . ? C7 N5 1.361(5) . ? C7 N6 1.369(5) . ? C8 N7 1.455(5) . ? C8 N5 1.461(5) . ? C8 C23 1.531(5) . ? C8 C9 1.571(5) . ? C9 N8 1.463(4) . ? C9 N6 1.463(5) . ? C9 C26 1.522(5) . ? C10 O5 1.232(5) . ? C10 N8 1.357(5) . ? C10 N7 1.371(5) . ? C11 N6 1.449(5) . ? C11 N9 1.457(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.448(5) . ? C12 N11 1.451(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.224(5) . ? C13 N9 1.360(5) . ? C13 N10 1.360(5) . ? C14 N9 1.454(5) . ? C14 N11 1.464(4) . ? C14 C27 1.518(5) . ? C14 C15 1.577(5) . ? C15 N10 1.458(5) . ? C15 N12 1.461(4) . ? C15 C30 1.524(5) . ? C16 O6 1.233(4) . ? C16 N12 1.344(5) . ? C16 N11 1.365(4) . ? C17 N3 1.455(5) 2_666 ? C17 N10 1.460(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.450(4) . ? C18 N1 1.454(4) 2_666 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.529(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.529(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.530(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.518(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.543(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.524(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.539(7) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.524(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.530(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O7 1.238(4) . ? C31 N13 1.350(4) . ? C31 N14 1.353(5) . ? C32 N15 1.459(4) . ? C32 N13 1.467(4) . ? C32 C49 1.524(5) . ? C32 C33 1.575(5) . ? C33 N14 1.454(4) . ? C33 N16 1.460(4) . ? C33 C52 1.525(5) . ? C34 O10 1.214(4) . ? C34 N15 1.370(5) . ? C34 N16 1.371(5) . ? C35 N14 1.443(4) . ? C35 N17 1.454(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N19 1.439(5) . ? C36 N16 1.457(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O8 1.238(4) . ? C37 N17 1.350(5) . ? C37 N18 1.356(4) . ? C38 N19 1.446(5) . ? C38 N17 1.463(4) . ? C38 C53 1.530(5) . ? C38 C39 1.578(5) . ? C39 N20 1.452(4) . ? C39 N18 1.465(4) . ? C39 C56 1.522(5) . ? C40 O11 1.213(5) . ? C40 N20 1.363(5) . ? C40 N19 1.380(5) . ? C41 N21 1.447(4) . ? C41 N18 1.462(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N20 1.449(5) . ? C42 N23 1.450(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 O9 1.233(4) . ? C43 N21 1.352(5) . ? C43 N22 1.365(5) . ? C44 N23 1.436(5) . ? C44 N21 1.476(4) . ? C44 C57 1.528(5) . ? C44 C45 1.578(5) . ? C45 N22 1.461(4) . ? C45 N24 1.462(4) . ? C45 C60 1.526(5) . ? C46 O12 1.226(5) . ? C46 N24 1.361(5) . ? C46 N23 1.368(5) . ? C47 N22 1.448(5) . ? C47 N15 1.459(5) 2_757 ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 N24 1.451(4) 2_757 ? C48 N13 1.453(4) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.521(6) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.528(6) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.527(5) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.529(6) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.534(6) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.528(6) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C58 1.515(6) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 C59 1.539(6) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 C60 1.524(5) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? N1 C18 1.454(4) 2_666 ? N3 C17 1.455(5) 2_666 ? N15 C47 1.459(5) 2_757 ? N24 C48 1.451(4) 2_757 ? O6 Sm1 2.410(2) 2_666 ? N25 O14 1.219(5) . ? N25 O15 1.233(5) . ? N25 O13 1.236(5) . ? N26 O18 1.221(6) . ? N26 O17 1.234(6) . ? N26 O16 1.276(6) . ? N27 O19 1.223(6) . ? N27 O20 1.230(6) . ? N27 O21 1.234(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Sm1 O4W 97.48(10) . . ? O7 Sm1 O1W 93.41(9) . . ? O4W Sm1 O1W 140.60(9) . . ? O7 Sm1 O6 138.83(8) . 2_666 ? O4W Sm1 O6 96.38(10) . 2_666 ? O1W Sm1 O6 99.91(9) . 2_666 ? O7 Sm1 O1 145.84(8) . . ? O4W Sm1 O1 77.04(10) . . ? O1W Sm1 O1 72.92(9) . . ? O6 Sm1 O1 75.18(8) 2_666 . ? O7 Sm1 O2W 76.09(9) . . ? O4W Sm1 O2W 71.80(10) . . ? O1W Sm1 O2W 147.53(9) . . ? O6 Sm1 O2W 71.85(9) 2_666 . ? O1 Sm1 O2W 131.00(9) . . ? O7 Sm1 O8 75.38(8) . . ? O4W Sm1 O8 72.56(9) . . ? O1W Sm1 O8 73.85(9) . . ? O6 Sm1 O8 145.77(8) 2_666 . ? O1 Sm1 O8 70.80(8) . . ? O2W Sm1 O8 130.24(9) . . ? O7 Sm1 O3W 75.22(9) . . ? O4W Sm1 O3W 147.36(10) . . ? O1W Sm1 O3W 72.03(9) . . ? O6 Sm1 O3W 72.32(9) 2_666 . ? O1 Sm1 O3W 126.29(9) . . ? O2W Sm1 O3W 75.57(10) . . ? O8 Sm1 O3W 132.87(9) . . ? O1 C1 N1 125.9(3) . . ? O1 C1 N2 124.4(3) . . ? N1 C1 N2 109.6(3) . . ? N1 C2 N3 113.5(3) . . ? N1 C2 C19 112.2(3) . . ? N3 C2 C19 112.9(3) . . ? N1 C2 C3 102.4(3) . . ? N3 C2 C3 102.7(3) . . ? C19 C2 C3 112.3(3) . . ? N4 C3 N2 112.2(3) . . ? N4 C3 C22 113.4(3) . . ? N2 C3 C22 112.6(3) . . ? N4 C3 C2 102.6(3) . . ? N2 C3 C2 103.1(3) . . ? C22 C3 C2 112.1(3) . . ? O4 C4 N3 126.1(3) . . ? O4 C4 N4 125.5(4) . . ? N3 C4 N4 108.4(3) . . ? N5 C5 N2 114.6(3) . . ? N5 C5 H5A 108.6 . . ? N2 C5 H5A 108.6 . . ? N5 C5 H5B 108.6 . . ? N2 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N4 C6 N7 114.9(3) . . ? N4 C6 H6A 108.5 . . ? N7 C6 H6A 108.5 . . ? N4 C6 H6B 108.5 . . ? N7 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? O2 C7 N5 125.9(4) . . ? O2 C7 N6 125.2(4) . . ? N5 C7 N6 108.8(3) . . ? N7 C8 N5 112.5(3) . . ? N7 C8 C23 112.9(3) . . ? N5 C8 C23 112.7(3) . . ? N7 C8 C9 103.3(3) . . ? N5 C8 C9 103.0(3) . . ? C23 C8 C9 111.6(3) . . ? N8 C9 N6 112.0(3) . . ? N8 C9 C26 113.6(3) . . ? N6 C9 C26 112.9(3) . . ? N8 C9 C8 102.6(3) . . ? N6 C9 C8 102.6(3) . . ? C26 C9 C8 112.2(3) . . ? O5 C10 N8 126.4(3) . . ? O5 C10 N7 124.2(4) . . ? N8 C10 N7 109.3(3) . . ? N6 C11 N9 115.2(3) . . ? N6 C11 H11A 108.5 . . ? N9 C11 H11A 108.5 . . ? N6 C11 H11B 108.5 . . ? N9 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N8 C12 N11 114.9(3) . . ? N8 C12 H12A 108.5 . . ? N11 C12 H12A 108.5 . . ? N8 C12 H12B 108.5 . . ? N11 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? O3 C13 N9 125.7(4) . . ? O3 C13 N10 125.4(4) . . ? N9 C13 N10 108.9(3) . . ? N9 C14 N11 112.4(3) . . ? N9 C14 C27 113.4(3) . . ? N11 C14 C27 113.3(3) . . ? N9 C14 C15 102.5(3) . . ? N11 C14 C15 102.8(3) . . ? C27 C14 C15 111.4(3) . . ? N10 C15 N12 113.1(3) . . ? N10 C15 C30 113.1(3) . . ? N12 C15 C30 112.1(3) . . ? N10 C15 C14 102.6(3) . . ? N12 C15 C14 102.2(3) . . ? C30 C15 C14 112.8(3) . . ? O6 C16 N12 125.5(3) . . ? O6 C16 N11 125.1(3) . . ? N12 C16 N11 109.4(3) . . ? N3 C17 N10 113.5(3) 2_666 . ? N3 C17 H17A 108.9 2_666 . ? N10 C17 H17A 108.9 . . ? N3 C17 H17B 108.9 2_666 . ? N10 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N12 C18 N1 113.6(3) . 2_666 ? N12 C18 H18A 108.9 . . ? N1 C18 H18A 108.9 2_666 . ? N12 C18 H18B 108.9 . . ? N1 C18 H18B 108.9 2_666 . ? H18A C18 H18B 107.7 . . ? C2 C19 C20 110.8(3) . . ? C2 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? C2 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C21 C20 C19 113.5(3) . . ? C21 C20 H20A 108.9 . . ? C19 C20 H20A 108.9 . . ? C21 C20 H20B 108.9 . . ? C19 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C20 C21 C22 112.2(3) . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C3 C22 C21 110.0(3) . . ? C3 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? C3 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? C24 C23 C8 111.4(3) . . ? C24 C23 H23A 109.3 . . ? C8 C23 H23A 109.3 . . ? C24 C23 H23B 109.3 . . ? C8 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? C23 C24 C25 112.2(3) . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C24 112.9(4) . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25B 109.0 . . ? C24 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C9 C26 C25 111.4(3) . . ? C9 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C9 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C14 C27 C28 110.6(4) . . ? C14 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? C14 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C29 C28 C27 113.9(4) . . ? C29 C28 H28A 108.8 . . ? C27 C28 H28A 108.8 . . ? C29 C28 H28B 108.8 . . ? C27 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C28 C29 C30 112.1(4) . . ? C28 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? C28 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C15 C30 C29 109.9(3) . . ? C15 C30 H30A 109.7 . . ? C29 C30 H30A 109.7 . . ? C15 C30 H30B 109.7 . . ? C29 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? O7 C31 N13 125.2(3) . . ? O7 C31 N14 124.9(3) . . ? N13 C31 N14 109.9(3) . . ? N15 C32 N13 112.4(3) . . ? N15 C32 C49 113.4(3) . . ? N13 C32 C49 112.9(3) . . ? N15 C32 C33 103.2(3) . . ? N13 C32 C33 102.3(3) . . ? C49 C32 C33 111.8(3) . . ? N14 C33 N16 113.2(3) . . ? N14 C33 C52 112.8(3) . . ? N16 C33 C52 112.7(3) . . ? N14 C33 C32 102.6(3) . . ? N16 C33 C32 102.3(3) . . ? C52 C33 C32 112.3(3) . . ? O10 C34 N15 125.5(3) . . ? O10 C34 N16 126.0(3) . . ? N15 C34 N16 108.5(3) . . ? N14 C35 N17 114.2(3) . . ? N14 C35 H35A 108.7 . . ? N17 C35 H35A 108.7 . . ? N14 C35 H35B 108.7 . . ? N17 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? N19 C36 N16 113.8(3) . . ? N19 C36 H36A 108.8 . . ? N16 C36 H36A 108.8 . . ? N19 C36 H36B 108.8 . . ? N16 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? O8 C37 N17 125.4(3) . . ? O8 C37 N18 125.0(3) . . ? N17 C37 N18 109.6(3) . . ? N19 C38 N17 113.2(3) . . ? N19 C38 C53 113.5(3) . . ? N17 C38 C53 111.9(3) . . ? N19 C38 C39 103.4(3) . . ? N17 C38 C39 102.0(3) . . ? C53 C38 C39 111.8(3) . . ? N20 C39 N18 112.4(3) . . ? N20 C39 C56 113.6(3) . . ? N18 C39 C56 112.9(3) . . ? N20 C39 C38 102.3(3) . . ? N18 C39 C38 102.7(3) . . ? C56 C39 C38 111.8(3) . . ? O11 C40 N20 126.4(3) . . ? O11 C40 N19 125.0(3) . . ? N20 C40 N19 108.5(3) . . ? N21 C41 N18 114.8(3) . . ? N21 C41 H41A 108.6 . . ? N18 C41 H41A 108.6 . . ? N21 C41 H41B 108.6 . . ? N18 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? N20 C42 N23 114.0(3) . . ? N20 C42 H42A 108.8 . . ? N23 C42 H42A 108.8 . . ? N20 C42 H42B 108.8 . . ? N23 C42 H42B 108.8 . . ? H42A C42 H42B 107.6 . . ? O9 C43 N21 125.8(3) . . ? O9 C43 N22 124.7(3) . . ? N21 C43 N22 109.4(3) . . ? N23 C44 N21 112.6(3) . . ? N23 C44 C57 113.2(3) . . ? N21 C44 C57 112.4(3) . . ? N23 C44 C45 103.4(3) . . ? N21 C44 C45 102.0(3) . . ? C57 C44 C45 112.4(3) . . ? N22 C45 N24 112.2(3) . . ? N22 C45 C60 113.5(3) . . ? N24 C45 C60 113.4(3) . . ? N22 C45 C44 103.0(3) . . ? N24 C45 C44 101.9(3) . . ? C60 C45 C44 111.8(3) . . ? O12 C46 N24 126.5(3) . . ? O12 C46 N23 124.7(4) . . ? N24 C46 N23 108.8(3) . . ? N22 C47 N15 115.2(3) . 2_757 ? N22 C47 H47A 108.5 . . ? N15 C47 H47A 108.5 2_757 . ? N22 C47 H47B 108.5 . . ? N15 C47 H47B 108.5 2_757 . ? H47A C47 H47B 107.5 . . ? N24 C48 N13 114.1(3) 2_757 . ? N24 C48 H48A 108.7 2_757 . ? N13 C48 H48A 108.7 . . ? N24 C48 H48B 108.7 2_757 . ? N13 C48 H48B 108.7 . . ? H48A C48 H48B 107.6 . . ? C50 C49 C32 112.5(3) . . ? C50 C49 H49A 109.1 . . ? C32 C49 H49A 109.1 . . ? C50 C49 H49B 109.1 . . ? C32 C49 H49B 109.1 . . ? H49A C49 H49B 107.8 . . ? C49 C50 C51 113.4(3) . . ? C49 C50 H50A 108.9 . . ? C51 C50 H50A 108.9 . . ? C49 C50 H50B 108.9 . . ? C51 C50 H50B 108.9 . . ? H50A C50 H50B 107.7 . . ? C52 C51 C50 111.9(3) . . ? C52 C51 H51A 109.2 . . ? C50 C51 H51A 109.2 . . ? C52 C51 H51B 109.2 . . ? C50 C51 H51B 109.2 . . ? H51A C51 H51B 107.9 . . ? C33 C52 C51 109.7(3) . . ? C33 C52 H52A 109.7 . . ? C51 C52 H52A 109.7 . . ? C33 C52 H52B 109.7 . . ? C51 C52 H52B 109.7 . . ? H52A C52 H52B 108.2 . . ? C54 C53 C38 111.7(3) . . ? C54 C53 H53A 109.3 . . ? C38 C53 H53A 109.3 . . ? C54 C53 H53B 109.3 . . ? C38 C53 H53B 109.3 . . ? H53A C53 H53B 107.9 . . ? C53 C54 C55 112.7(3) . . ? C53 C54 H54A 109.0 . . ? C55 C54 H54A 109.0 . . ? C53 C54 H54B 109.0 . . ? C55 C54 H54B 109.0 . . ? H54A C54 H54B 107.8 . . ? C56 C55 C54 112.2(4) . . ? C56 C55 H55A 109.2 . . ? C54 C55 H55A 109.2 . . ? C56 C55 H55B 109.2 . . ? C54 C55 H55B 109.2 . . ? H55A C55 H55B 107.9 . . ? C39 C56 C55 109.9(3) . . ? C39 C56 H56A 109.7 . . ? C55 C56 H56A 109.7 . . ? C39 C56 H56B 109.7 . . ? C55 C56 H56B 109.7 . . ? H56A C56 H56B 108.2 . . ? C58 C57 C44 111.4(3) . . ? C58 C57 H57A 109.4 . . ? C44 C57 H57A 109.4 . . ? C58 C57 H57B 109.4 . . ? C44 C57 H57B 109.4 . . ? H57A C57 H57B 108.0 . . ? C57 C58 C59 112.3(3) . . ? C57 C58 H58A 109.2 . . ? C59 C58 H58A 109.2 . . ? C57 C58 H58B 109.2 . . ? C59 C58 H58B 109.2 . . ? H58A C58 H58B 107.9 . . ? C60 C59 C58 113.5(3) . . ? C60 C59 H59A 108.9 . . ? C58 C59 H59A 108.9 . . ? C60 C59 H59B 108.9 . . ? C58 C59 H59B 108.9 . . ? H59A C59 H59B 107.7 . . ? C59 C60 C45 112.4(3) . . ? C59 C60 H60A 109.1 . . ? C45 C60 H60A 109.1 . . ? C59 C60 H60B 109.1 . . ? C45 C60 H60B 109.1 . . ? H60A C60 H60B 107.8 . . ? C1 N1 C2 113.3(3) . . ? C1 N1 C18 121.4(3) . 2_666 ? C2 N1 C18 125.4(3) . 2_666 ? C1 N2 C5 121.0(3) . . ? C1 N2 C3 111.2(3) . . ? C5 N2 C3 125.2(3) . . ? C4 N3 C17 120.5(3) . 2_666 ? C4 N3 C2 112.6(3) . . ? C17 N3 C2 125.5(3) 2_666 . ? C4 N4 C6 121.0(3) . . ? C4 N4 C3 113.0(3) . . ? C6 N4 C3 125.8(3) . . ? C7 N5 C5 121.2(3) . . ? C7 N5 C8 112.7(3) . . ? C5 N5 C8 125.2(3) . . ? C7 N6 C11 121.2(3) . . ? C7 N6 C9 112.7(3) . . ? C11 N6 C9 125.1(3) . . ? C10 N7 C6 121.4(3) . . ? C10 N7 C8 112.1(3) . . ? C6 N7 C8 125.4(3) . . ? C10 N8 C12 121.4(3) . . ? C10 N8 C9 112.6(3) . . ? C12 N8 C9 124.1(3) . . ? C13 N9 C14 113.0(3) . . ? C13 N9 C11 121.0(3) . . ? C14 N9 C11 125.6(3) . . ? C13 N10 C15 112.8(3) . . ? C13 N10 C17 121.6(3) . . ? C15 N10 C17 125.1(3) . . ? C16 N11 C12 121.6(3) . . ? C16 N11 C14 112.1(3) . . ? C12 N11 C14 125.0(3) . . ? C16 N12 C18 122.2(3) . . ? C16 N12 C15 113.3(3) . . ? C18 N12 C15 124.4(3) . . ? C31 N13 C48 121.5(3) . . ? C31 N13 C32 112.2(3) . . ? C48 N13 C32 124.3(3) . . ? C31 N14 C35 122.8(3) . . ? C31 N14 C33 112.5(3) . . ? C35 N14 C33 124.7(3) . . ? C34 N15 C47 121.2(3) . 2_757 ? C34 N15 C32 112.6(3) . . ? C47 N15 C32 126.0(3) 2_757 . ? C34 N16 C36 121.2(3) . . ? C34 N16 C33 113.0(3) . . ? C36 N16 C33 124.6(3) . . ? C37 N17 C35 122.3(3) . . ? C37 N17 C38 113.0(3) . . ? C35 N17 C38 124.7(3) . . ? C37 N18 C41 120.7(3) . . ? C37 N18 C39 112.1(3) . . ? C41 N18 C39 124.9(3) . . ? C40 N19 C36 121.0(3) . . ? C40 N19 C38 112.0(3) . . ? C36 N19 C38 125.8(3) . . ? C40 N20 C42 121.4(3) . . ? C40 N20 C39 113.2(3) . . ? C42 N20 C39 125.2(3) . . ? C43 N21 C41 121.0(3) . . ? C43 N21 C44 112.7(3) . . ? C41 N21 C44 124.8(3) . . ? C43 N22 C47 122.5(3) . . ? C43 N22 C45 112.4(3) . . ? C47 N22 C45 124.8(3) . . ? C46 N23 C44 112.8(3) . . ? C46 N23 C42 121.4(3) . . ? C44 N23 C42 125.4(3) . . ? C46 N24 C48 120.7(3) . 2_757 ? C46 N24 C45 112.7(3) . . ? C48 N24 C45 123.5(3) 2_757 . ? C1 O1 Sm1 155.1(2) . . ? C16 O6 Sm1 155.3(2) . 2_666 ? C31 O7 Sm1 158.9(2) . . ? C37 O8 Sm1 156.8(2) . . ? O14 N25 O15 121.0(5) . . ? O14 N25 O13 119.4(5) . . ? O15 N25 O13 119.6(4) . . ? O18 N26 O17 120.2(5) . . ? O18 N26 O16 117.8(5) . . ? O17 N26 O16 122.0(5) . . ? O19 N27 O20 119.8(5) . . ? O19 N27 O21 120.6(5) . . ? O20 N27 O21 119.6(5) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.714 _refine_diff_density_min -1.014 _refine_diff_density_rms 0.098 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 108 23 ' ' 2 0.225 0.129 0.220 208 73 ' ' 3 -0.163 0.458 0.153 62 20 ' ' 4 0.158 0.545 0.846 63 20 ' ' 5 -0.226 0.873 0.780 205 72 ' ' 6 0.500 0.500 0.500 116 32 ' ' 7 0.472 0.514 0.846 18 9 ' ' 8 0.528 0.486 0.154 17 8 ' ' _platon_squeeze_details ; ; data_a3 _database_code_depnum_ccdc_archive 'CCDC 881899' #TrackingRef '110105qx-submit-cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H106 Dy N27 O38' _chemical_formula_weight 1976.22 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.9117(7) _cell_length_b 15.9777(6) _cell_length_c 18.2073(7) _cell_angle_alpha 74.7500(10) _cell_angle_beta 89.332(2) _cell_angle_gamma 63.3840(10) _cell_volume 3962.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2050 _exptl_absorpt_coefficient_mu 1.056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7636 _exptl_absorpt_correction_T_max 0.8246 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42146 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13781 _reflns_number_gt 12194 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+5.0068P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13781 _refine_ls_number_parameters 1008 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1349 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1W O 0.2584(2) 0.9497(2) 0.71365(18) 0.0279(7) Uani 1 1 d . . . O2W O 0.3955(2) 0.6204(2) 0.75410(18) 0.0276(7) Uani 1 1 d . . . O3W O 0.4410(2) 0.7749(2) 0.73405(18) 0.0290(7) Uani 1 1 d . . . O4W O 0.1232(2) 0.8833(2) 0.72716(19) 0.0306(7) Uani 1 1 d . . . Dy1 Dy 0.285464(14) 0.784683(14) 0.736370(11) 0.02223(9) Uani 1 1 d . . . O4 O 0.2644(2) 0.5097(2) 1.16988(18) 0.0288(7) Uiso 1 1 d . . . C4 C 0.2207(3) 0.5551(3) 1.1058(2) 0.0212(9) Uani 1 1 d . . . C17 C 0.7708(3) 0.5889(3) 0.9240(2) 0.0207(9) Uani 1 1 d . . . H17A H 0.7534 0.6162 0.8683 0.025 Uiso 1 1 calc R . . H17B H 0.8249 0.5983 0.9371 0.025 Uiso 1 1 calc R . . C18 C 0.2096(3) 0.5179(3) 0.8729(2) 0.0202(8) Uiso 1 1 d . . . H18A H 0.1546 0.5057 0.8710 0.024 Uiso 1 1 calc R . . H18B H 0.2149 0.5494 0.8203 0.024 Uiso 1 1 calc R . . C45 C 0.3286(3) 0.8768(3) 0.4098(2) 0.0180(8) Uani 1 1 d . . . C57 C 0.4249(3) 0.6958(3) 0.4147(2) 0.0233(9) Uani 1 1 d . . . H57A H 0.4789 0.6816 0.4498 0.028 Uiso 1 1 calc R . . H57B H 0.4203 0.6351 0.4215 0.028 Uiso 1 1 calc R . . C58 C 0.4402(3) 0.7334(3) 0.3321(3) 0.0275(10) Uani 1 1 d . . . H58A H 0.4972 0.6825 0.3200 0.033 Uiso 1 1 calc R . . H58B H 0.3862 0.7467 0.2974 0.033 Uiso 1 1 calc R . . C59 C 0.4510(3) 0.8262(4) 0.3186(3) 0.0326(11) Uani 1 1 d . . . H59A H 0.4127 0.8731 0.2704 0.039 Uiso 1 1 calc R . . H59B H 0.5174 0.8102 0.3130 0.039 Uiso 1 1 calc R . . C60 C 0.4209(3) 0.8743(3) 0.3835(3) 0.0249(9) Uani 1 1 d . . . H60A H 0.4710 0.8381 0.4270 0.030 Uiso 1 1 calc R . . H60B H 0.4128 0.9413 0.3657 0.030 Uiso 1 1 calc R . . N3 N 0.2001(2) 0.5147(2) 1.05564(19) 0.0195(7) Uani 1 1 d . . . N22 N 0.3081(2) 0.9054(2) 0.48101(19) 0.0163(7) Uani 1 1 d . . . N24 N 0.2479(2) 0.9337(2) 0.35001(19) 0.0177(7) Uani 1 1 d . . . C1 C 0.1998(3) 0.6685(3) 0.8902(2) 0.0172(8) Uani 1 1 d . . . C2 C 0.1410(3) 0.5875(3) 0.9863(2) 0.0175(8) Uani 1 1 d . . . C3 C 0.1247(3) 0.6864(3) 1.0005(2) 0.0190(8) Uani 1 1 d . . . C5 C 0.1559(3) 0.8248(3) 0.9169(2) 0.0201(8) Uani 1 1 d . . . H5A H 0.1519 0.8501 0.8611 0.024 Uiso 1 1 calc R . . H5B H 0.0979 0.8692 0.9333 0.024 Uiso 1 1 calc R . . C6 C 0.1919(3) 0.7159(3) 1.1148(2) 0.0249(9) Uani 1 1 d . . . H6A H 0.1297 0.7726 1.1090 0.030 Uiso 1 1 calc R . . H6B H 0.2090 0.6797 1.1694 0.030 Uiso 1 1 calc R . . C7 C 0.3136(3) 0.8158(3) 0.9174(2) 0.0159(8) Uani 1 1 d . . . C8 C 0.2420(3) 0.8382(3) 1.0285(2) 0.0198(9) Uani 1 1 d . . . C9 C 0.3375(3) 0.8438(3) 1.0335(2) 0.0189(8) Uani 1 1 d . . . C10 C 0.3471(3) 0.7099(3) 1.1323(2) 0.0230(9) Uani 1 1 d . . . C11 C 0.4540(3) 0.8382(3) 0.9331(2) 0.0200(8) Uani 1 1 d . . . H11A H 0.4476 0.8499 0.8774 0.024 Uiso 1 1 calc R . . H11B H 0.4512 0.8968 0.9429 0.024 Uiso 1 1 calc R . . C12 C 0.4816(3) 0.7446(3) 1.1390(2) 0.0240(9) Uani 1 1 d . . . H12A H 0.4900 0.7055 1.1924 0.029 Uiso 1 1 calc R . . H12B H 0.4777 0.8073 1.1400 0.029 Uiso 1 1 calc R . . C13 C 0.6026(3) 0.7021(3) 0.9211(2) 0.0215(9) Uani 1 1 d . . . C14 C 0.5978(3) 0.7413(3) 1.0377(2) 0.0196(8) Uani 1 1 d . . . C15 C 0.6992(3) 0.6576(3) 1.0357(2) 0.0194(8) Uani 1 1 d . . . C16 C 0.6295(3) 0.5998(3) 1.1393(2) 0.0209(9) Uani 1 1 d . . . C19 C 0.0473(3) 0.5862(3) 0.9720(3) 0.0242(9) Uani 1 1 d . . . H19A H 0.0591 0.5288 0.9552 0.029 Uiso 1 1 calc R . . H19B H 0.0186 0.5813 1.0198 0.029 Uiso 1 1 calc R . . C20 C -0.0202(3) 0.6783(4) 0.9112(3) 0.0318(10) Uani 1 1 d . . . H20A H -0.0794 0.6755 0.9026 0.038 Uiso 1 1 calc R . . H20B H 0.0078 0.6811 0.8629 0.038 Uiso 1 1 calc R . . C21 C -0.0421(3) 0.7706(3) 0.9332(3) 0.0331(11) Uani 1 1 d . . . H21A H -0.1086 0.8007 0.9424 0.040 Uiso 1 1 calc R . . H21B H -0.0339 0.8171 0.8902 0.040 Uiso 1 1 calc R . . C22 C 0.0202(3) 0.7525(3) 1.0045(3) 0.0257(9) Uani 1 1 d . . . H22A H -0.0002 0.7218 1.0501 0.031 Uiso 1 1 calc R . . H22B H 0.0128 0.8151 1.0090 0.031 Uiso 1 1 calc R . . C23 C 0.1564(3) 0.9296(3) 1.0368(3) 0.0289(10) Uani 1 1 d . . . H23A H 0.1003 0.9188 1.0405 0.035 Uiso 1 1 calc R . . H23B H 0.1434 0.9852 0.9918 0.035 Uiso 1 1 calc R . . C24 C 0.1777(4) 0.9518(4) 1.1093(3) 0.0456(14) Uani 1 1 d . . . H24A H 0.1232 1.0106 1.1147 0.055 Uiso 1 1 calc R . . H24B H 0.1873 0.8973 1.1543 0.055 Uiso 1 1 calc R . . C25 C 0.2658(4) 0.9677(4) 1.1070(3) 0.0473(15) Uani 1 1 d . . . H25A H 0.2464 1.0361 1.1038 0.057 Uiso 1 1 calc R . . H25B H 0.3078 0.9270 1.1551 0.057 Uiso 1 1 calc R . . C26 C 0.3210(3) 0.9435(3) 1.0402(3) 0.0288(10) Uani 1 1 d . . . H26A H 0.3822 0.9429 1.0477 0.035 Uiso 1 1 calc R . . H26B H 0.2858 0.9941 0.9924 0.035 Uiso 1 1 calc R . . C27 C 0.6009(3) 0.8319(3) 1.0461(3) 0.0279(10) Uani 1 1 d . . . H27A H 0.5374 0.8793 1.0519 0.033 Uiso 1 1 calc R . . H27B H 0.6204 0.8621 0.9995 0.033 Uiso 1 1 calc R . . C28 C 0.6695(4) 0.8078(4) 1.1151(3) 0.0375(12) Uani 1 1 d . . . H28A H 0.6429 0.7909 1.1621 0.045 Uiso 1 1 calc R . . H28B H 0.6767 0.8659 1.1140 0.045 Uiso 1 1 calc R . . C29 C 0.7673(4) 0.7229(4) 1.1167(3) 0.0364(12) Uani 1 1 d . . . H29A H 0.8157 0.7443 1.1203 0.044 Uiso 1 1 calc R . . H29B H 0.7795 0.6688 1.1628 0.044 Uiso 1 1 calc R . . C30 C 0.7768(3) 0.6863(3) 1.0470(3) 0.0273(10) Uani 1 1 d . . . H30A H 0.8390 0.6294 1.0530 0.033 Uiso 1 1 calc R . . H30B H 0.7728 0.7375 1.0014 0.033 Uiso 1 1 calc R . . C31 C -0.0715(3) 0.8294(3) 0.6904(2) 0.0175(8) Uani 1 1 d . . . C32 C -0.2065(3) 0.8569(3) 0.6158(2) 0.0173(8) Uani 1 1 d . . . C33 C -0.1197(3) 0.7582(3) 0.6115(2) 0.0168(8) Uani 1 1 d . . . C34 C -0.1723(3) 0.8695(3) 0.4880(2) 0.0199(9) Uani 1 1 d . . . C35 C 0.0526(3) 0.6747(3) 0.6777(2) 0.0179(8) Uani 1 1 d . . . H35A H 0.0473 0.6138 0.6924 0.021 Uiso 1 1 calc R . . H35B H 0.0818 0.6787 0.7228 0.021 Uiso 1 1 calc R . . C36 C -0.0522(3) 0.7021(3) 0.4942(2) 0.0215(9) Uani 1 1 d . . . H36A H -0.0523 0.6403 0.5209 0.026 Uiso 1 1 calc R . . H36B H -0.0806 0.7218 0.4411 0.026 Uiso 1 1 calc R . . C37 C 0.1913(3) 0.6853(3) 0.6250(2) 0.0163(8) Uani 1 1 d . . . C38 C 0.1198(3) 0.6233(3) 0.5569(2) 0.0161(8) Uani 1 1 d . . . C39 C 0.2106(3) 0.6214(3) 0.5203(2) 0.0167(8) Uani 1 1 d . . . C40 C 0.0759(3) 0.7217(3) 0.4290(2) 0.0209(9) Uani 1 1 d . . . C41 C 0.3363(3) 0.6631(3) 0.5657(2) 0.0158(8) Uani 1 1 d . . . H41A H 0.3625 0.6546 0.6171 0.019 Uiso 1 1 calc R . . H41B H 0.3815 0.6089 0.5477 0.019 Uiso 1 1 calc R . . C42 C 0.2251(3) 0.7127(3) 0.3849(2) 0.0216(9) Uani 1 1 d . . . H42A H 0.1886 0.7326 0.3350 0.026 Uiso 1 1 calc R . . H42B H 0.2837 0.6529 0.3879 0.026 Uiso 1 1 calc R . . C43 C 0.3104(3) 0.8325(3) 0.5399(2) 0.0167(8) Uani 1 1 d . . . C44 C 0.3338(3) 0.7730(3) 0.4333(2) 0.0169(8) Uani 1 1 d . . . C46 C 0.2028(3) 0.8818(3) 0.3395(2) 0.0196(9) Uani 1 1 d . . . C47 C -0.2209(3) 0.9683(3) 0.7003(2) 0.0201(8) Uani 1 1 d . . . H47A H -0.1838 0.9586 0.7471 0.024 Uiso 1 1 calc R . . H47B H -0.2787 0.9642 0.7152 0.024 Uiso 1 1 calc R . . C48 C -0.3111(3) 1.0102(3) 0.5060(2) 0.0190(8) Uani 1 1 d . . . H48A H -0.3230 1.0219 0.4507 0.023 Uiso 1 1 calc R . . H48B H -0.3645 1.0037 0.5293 0.023 Uiso 1 1 calc R . . C49 C -0.2902(3) 0.8404(3) 0.6436(3) 0.0236(9) Uani 1 1 d . . . H49A H -0.3150 0.8218 0.6049 0.028 Uiso 1 1 calc R . . H49B H -0.3407 0.9018 0.6491 0.028 Uiso 1 1 calc R . . C50 C -0.2631(4) 0.7611(3) 0.7201(3) 0.0352(11) Uani 1 1 d . . . H50A H -0.3146 0.7433 0.7296 0.042 Uiso 1 1 calc R . . H50B H -0.2562 0.7874 0.7612 0.042 Uiso 1 1 calc R . . C51 C -0.1711(3) 0.6689(3) 0.7230(3) 0.0298(10) Uani 1 1 d . . . H51A H -0.1221 0.6634 0.7587 0.036 Uiso 1 1 calc R . . H51B H -0.1814 0.6114 0.7425 0.036 Uiso 1 1 calc R . . C52 C -0.1364(3) 0.6700(3) 0.6444(3) 0.0253(9) Uani 1 1 d . . . H52A H -0.0772 0.6101 0.6492 0.030 Uiso 1 1 calc R . . H52B H -0.1835 0.6712 0.6094 0.030 Uiso 1 1 calc R . . C53 C 0.1293(3) 0.5207(3) 0.5888(3) 0.0244(9) Uani 1 1 d . . . H53A H 0.0769 0.5235 0.6186 0.029 Uiso 1 1 calc R . . H53B H 0.1258 0.4949 0.5463 0.029 Uiso 1 1 calc R . . C54 C 0.2227(3) 0.4535(3) 0.6395(3) 0.0349(11) Uani 1 1 d . . . H54A H 0.2271 0.3882 0.6594 0.042 Uiso 1 1 calc R . . H54B H 0.2240 0.4778 0.6833 0.042 Uiso 1 1 calc R . . C55 C 0.3085(3) 0.4454(3) 0.5975(3) 0.0337(11) Uani 1 1 d . . . H55A H 0.3431 0.3792 0.5923 0.040 Uiso 1 1 calc R . . H55B H 0.3512 0.4558 0.6282 0.040 Uiso 1 1 calc R . . C56 C 0.2808(3) 0.5196(3) 0.5176(3) 0.0246(9) Uani 1 1 d . . . H56A H 0.3377 0.5210 0.4976 0.030 Uiso 1 1 calc R . . H56B H 0.2526 0.4991 0.4827 0.030 Uiso 1 1 calc R . . N1 N 0.1923(2) 0.5851(2) 0.91851(19) 0.0180(7) Uani 1 1 d . . . N2 N 0.1601(2) 0.7289(2) 0.93492(19) 0.0179(7) Uani 1 1 d . . . N4 N 0.1843(3) 0.6531(3) 1.0725(2) 0.0218(7) Uani 1 1 d . . . N5 N 0.2359(2) 0.8251(2) 0.95252(19) 0.0180(7) Uani 1 1 d . . . N6 N 0.3744(2) 0.8249(2) 0.96259(18) 0.0177(7) Uani 1 1 d . . . N7 N 0.2608(3) 0.7503(3) 1.0904(2) 0.0216(7) Uani 1 1 d . . . N8 N 0.3926(2) 0.7630(2) 1.10158(19) 0.0201(7) Uani 1 1 d . . . N9 N 0.5459(2) 0.7567(2) 0.96556(19) 0.0197(7) Uani 1 1 d . . . N10 N 0.6915(2) 0.6436(2) 0.9612(2) 0.0208(7) Uani 1 1 d . . . N11 N 0.5650(2) 0.6946(2) 1.1038(2) 0.0206(7) Uani 1 1 d . . . N12 N 0.7060(2) 0.5753(2) 1.09870(19) 0.0199(7) Uani 1 1 d . . . N13 N -0.1665(2) 0.8893(2) 0.66750(19) 0.0167(7) Uani 1 1 d . . . N14 N -0.0418(2) 0.7564(2) 0.65569(19) 0.0166(7) Uani 1 1 d . . . N15 N -0.2256(2) 0.9189(2) 0.53645(19) 0.0175(7) Uani 1 1 d . . . N16 N -0.1109(2) 0.7762(2) 0.5307(2) 0.0194(7) Uani 1 1 d . . . N17 N 0.1146(2) 0.6705(2) 0.61755(18) 0.0159(7) Uani 1 1 d . . . N18 N 0.2476(2) 0.6576(2) 0.57090(19) 0.0162(7) Uani 1 1 d . . . N19 N 0.0449(2) 0.6859(2) 0.49388(19) 0.0185(7) Uani 1 1 d . . . N20 N 0.1712(2) 0.6909(3) 0.44444(19) 0.0197(7) Uani 1 1 d . . . N21 N 0.3276(2) 0.7538(2) 0.51506(19) 0.0169(7) Uani 1 1 d . . . N23 N 0.2495(2) 0.7889(2) 0.38892(19) 0.0186(7) Uani 1 1 d . . . N25 N 0.5659(4) 0.7182(4) 0.5863(3) 0.0520(13) Uani 1 1 d . . . N26 N 0.0096(3) 0.4439(3) 0.8035(2) 0.0356(10) Uani 1 1 d . . . N27 N 0.5943(5) 0.9375(4) 0.8335(3) 0.0587(15) Uani 1 1 d . . . O1 O 0.2350(2) 0.6879(2) 0.83142(16) 0.0228(6) Uani 1 1 d . . . O2 O 0.3265(2) 0.8027(2) 0.85373(16) 0.0218(6) Uani 1 1 d . . . O3 O 0.5793(2) 0.7044(2) 0.85715(17) 0.0271(7) Uani 1 1 d . . . O5 O 0.3777(2) 0.6391(2) 1.18925(18) 0.0317(7) Uani 1 1 d . . . O6 O 0.6227(2) 0.5476(2) 1.19872(17) 0.0269(7) Uani 1 1 d . . . O7 O -0.0227(2) 0.8385(2) 0.73548(17) 0.0227(6) Uani 1 1 d . . . O8 O 0.2075(2) 0.7173(2) 0.67470(16) 0.0215(6) Uani 1 1 d . . . O9 O 0.3007(2) 0.8352(2) 0.60673(16) 0.0204(6) Uani 1 1 d . . . O10 O -0.1775(2) 0.9017(2) 0.41896(17) 0.0281(7) Uani 1 1 d . . . O11 O 0.0280(2) 0.7721(2) 0.36718(17) 0.0288(7) Uani 1 1 d . . . O12 O 0.1344(2) 0.9115(2) 0.29263(18) 0.0310(7) Uani 1 1 d . . . O13 O 0.5271(4) 0.8074(3) 0.5700(3) 0.0685(13) Uani 1 1 d . . . O14 O 0.6227(5) 0.6762(4) 0.5452(3) 0.096(2) Uani 1 1 d . . . O15 O 0.5445(5) 0.6712(4) 0.6407(4) 0.096(2) Uani 1 1 d . . . O16 O 0.0117(3) 0.4900(3) 0.8478(3) 0.0641(13) Uani 1 1 d . . . O17 O -0.0287(4) 0.3907(4) 0.8199(3) 0.0713(14) Uani 1 1 d . . . O18 O 0.0456(3) 0.4507(3) 0.7441(2) 0.0567(11) Uani 1 1 d . . . O19 O 0.5350(4) 0.9969(4) 0.8677(3) 0.0646(12) Uani 1 1 d . . . O20 O 0.5768(5) 0.9461(4) 0.7681(3) 0.098(2) Uani 1 1 d . . . O21 O 0.6736(4) 0.8731(4) 0.8682(3) 0.0808(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.0346(17) 0.0211(15) 0.0229(16) -0.0027(13) -0.0007(14) -0.0105(13) O2W 0.0269(16) 0.0251(16) 0.0259(17) -0.0011(13) 0.0004(13) -0.0111(13) O3W 0.0237(16) 0.0360(17) 0.0258(17) -0.0051(14) -0.0004(13) -0.0146(14) O4W 0.0235(16) 0.0314(17) 0.0370(19) -0.0093(15) 0.0028(14) -0.0130(14) Dy1 0.02602(13) 0.02528(13) 0.01627(13) -0.00481(9) 0.00241(8) -0.01320(9) C4 0.019(2) 0.029(2) 0.014(2) -0.0033(17) 0.0045(17) -0.0115(18) C17 0.024(2) 0.022(2) 0.017(2) 0.0005(17) 0.0048(17) -0.0145(18) C45 0.018(2) 0.0187(19) 0.012(2) -0.0028(16) 0.0025(16) -0.0048(16) C57 0.020(2) 0.022(2) 0.021(2) -0.0093(18) 0.0047(17) -0.0029(17) C58 0.021(2) 0.033(2) 0.020(2) -0.0119(19) 0.0076(18) -0.0031(19) C59 0.029(2) 0.039(3) 0.024(2) -0.010(2) 0.014(2) -0.011(2) C60 0.020(2) 0.027(2) 0.022(2) -0.0039(18) 0.0044(18) -0.0080(18) N3 0.0217(18) 0.0205(17) 0.0128(17) 0.0004(14) 0.0008(14) -0.0095(15) N22 0.0193(17) 0.0172(16) 0.0121(16) -0.0050(13) 0.0033(13) -0.0078(14) N24 0.0176(17) 0.0193(16) 0.0125(17) -0.0018(13) -0.0020(14) -0.0068(14) C1 0.0168(19) 0.021(2) 0.014(2) -0.0015(16) -0.0016(16) -0.0105(16) C2 0.0174(19) 0.0187(19) 0.015(2) 0.0008(16) 0.0044(16) -0.0101(16) C3 0.017(2) 0.024(2) 0.016(2) -0.0044(17) 0.0059(16) -0.0102(17) C5 0.022(2) 0.021(2) 0.016(2) -0.0035(16) 0.0019(17) -0.0104(17) C6 0.035(2) 0.032(2) 0.014(2) -0.0092(18) 0.0090(18) -0.019(2) C7 0.021(2) 0.0131(18) 0.012(2) -0.0007(15) 0.0011(16) -0.0086(16) C8 0.025(2) 0.020(2) 0.013(2) -0.0077(16) 0.0019(17) -0.0078(17) C9 0.022(2) 0.0167(19) 0.016(2) -0.0074(16) 0.0020(17) -0.0061(16) C10 0.032(2) 0.020(2) 0.017(2) -0.0087(18) 0.0061(19) -0.0094(18) C11 0.019(2) 0.020(2) 0.018(2) -0.0006(16) -0.0006(17) -0.0094(17) C12 0.024(2) 0.028(2) 0.017(2) -0.0104(18) -0.0016(17) -0.0067(18) C13 0.024(2) 0.022(2) 0.023(2) -0.0034(17) 0.0024(18) -0.0166(18) C14 0.021(2) 0.022(2) 0.017(2) -0.0022(17) -0.0010(17) -0.0117(17) C15 0.023(2) 0.0174(19) 0.019(2) -0.0014(16) -0.0004(17) -0.0122(17) C16 0.025(2) 0.023(2) 0.020(2) -0.0098(18) 0.0008(18) -0.0134(18) C19 0.019(2) 0.032(2) 0.025(2) -0.0057(19) 0.0061(18) -0.0162(19) C20 0.023(2) 0.040(3) 0.032(3) -0.004(2) 0.000(2) -0.018(2) C21 0.018(2) 0.032(2) 0.038(3) -0.001(2) 0.002(2) -0.0073(19) C22 0.016(2) 0.030(2) 0.027(2) -0.0052(19) 0.0089(18) -0.0086(18) C23 0.029(2) 0.023(2) 0.031(3) -0.0119(19) 0.009(2) -0.0061(19) C24 0.064(4) 0.039(3) 0.040(3) -0.030(3) 0.020(3) -0.019(3) C25 0.048(3) 0.040(3) 0.050(3) -0.034(3) -0.002(3) -0.006(3) C26 0.033(2) 0.017(2) 0.034(3) -0.0099(19) -0.004(2) -0.0087(19) C27 0.030(2) 0.023(2) 0.032(3) -0.0081(19) -0.004(2) -0.0127(19) C28 0.038(3) 0.040(3) 0.041(3) -0.015(2) -0.006(2) -0.021(2) C29 0.035(3) 0.034(3) 0.041(3) -0.009(2) -0.012(2) -0.017(2) C30 0.025(2) 0.027(2) 0.032(3) -0.0017(19) -0.0046(19) -0.0164(19) C31 0.018(2) 0.021(2) 0.015(2) -0.0042(16) 0.0061(16) -0.0114(17) C32 0.0161(19) 0.0181(19) 0.014(2) -0.0014(16) 0.0007(16) -0.0062(16) C33 0.0154(19) 0.0157(19) 0.018(2) -0.0033(16) 0.0003(16) -0.0068(16) C34 0.018(2) 0.022(2) 0.018(2) -0.0033(17) -0.0004(17) -0.0098(17) C35 0.0152(19) 0.0197(19) 0.013(2) -0.0031(16) 0.0022(16) -0.0042(16) C36 0.018(2) 0.028(2) 0.023(2) -0.0125(18) 0.0011(17) -0.0108(17) C37 0.0157(19) 0.0147(18) 0.015(2) -0.0016(15) -0.0005(16) -0.0051(15) C38 0.0145(19) 0.0172(19) 0.015(2) -0.0054(16) 0.0015(16) -0.0054(16) C39 0.0169(19) 0.0191(19) 0.016(2) -0.0067(16) 0.0036(16) -0.0089(16) C40 0.024(2) 0.022(2) 0.018(2) -0.0099(18) 0.0024(18) -0.0090(18) C41 0.0136(18) 0.0164(19) 0.0136(19) -0.0022(15) 0.0008(15) -0.0048(15) C42 0.030(2) 0.026(2) 0.013(2) -0.0078(17) 0.0049(17) -0.0150(19) C43 0.0137(18) 0.0200(19) 0.017(2) -0.0053(16) 0.0009(16) -0.0084(16) C44 0.0168(19) 0.0187(19) 0.0121(19) -0.0041(16) 0.0045(16) -0.0058(16) C46 0.021(2) 0.022(2) 0.012(2) -0.0053(16) 0.0044(17) -0.0064(17) C47 0.023(2) 0.0186(19) 0.0105(19) -0.0027(16) 0.0037(16) -0.0040(17) C48 0.0139(19) 0.0194(19) 0.021(2) -0.0063(17) 0.0004(16) -0.0054(16) C49 0.016(2) 0.021(2) 0.028(2) 0.0001(18) 0.0040(18) -0.0081(17) C50 0.034(3) 0.033(3) 0.031(3) -0.002(2) 0.013(2) -0.013(2) C51 0.031(2) 0.027(2) 0.026(2) 0.0024(19) 0.005(2) -0.014(2) C52 0.025(2) 0.023(2) 0.026(2) -0.0041(18) 0.0023(19) -0.0108(18) C53 0.028(2) 0.019(2) 0.028(2) -0.0066(18) 0.0060(19) -0.0118(18) C54 0.036(3) 0.020(2) 0.035(3) -0.001(2) 0.004(2) -0.006(2) C55 0.028(2) 0.021(2) 0.041(3) -0.005(2) -0.001(2) -0.0033(19) C56 0.022(2) 0.021(2) 0.031(2) -0.0147(19) 0.0084(19) -0.0075(18) N1 0.0224(17) 0.0229(17) 0.0124(17) -0.0061(14) 0.0054(14) -0.0130(15) N2 0.0222(17) 0.0194(17) 0.0138(17) -0.0025(14) 0.0055(14) -0.0124(14) N4 0.0268(19) 0.0274(19) 0.0129(17) -0.0048(15) 0.0029(15) -0.0145(16) N5 0.0189(17) 0.0229(17) 0.0119(17) -0.0055(14) 0.0004(14) -0.0091(14) N6 0.0227(18) 0.0238(17) 0.0096(16) -0.0037(14) 0.0024(14) -0.0137(15) N7 0.0272(19) 0.0222(18) 0.0150(18) -0.0029(14) 0.0008(15) -0.0124(15) N8 0.0223(18) 0.0211(17) 0.0132(17) -0.0040(14) 0.0002(14) -0.0073(15) N9 0.0213(18) 0.0211(17) 0.0148(17) -0.0007(14) -0.0030(14) -0.0104(15) N10 0.0203(18) 0.0216(17) 0.0159(18) -0.0013(14) -0.0027(14) -0.0078(15) N11 0.0216(18) 0.0201(17) 0.0164(18) -0.0028(14) 0.0011(14) -0.0076(15) N12 0.0248(18) 0.0183(17) 0.0140(17) 0.0009(14) 0.0018(14) -0.0108(15) N13 0.0158(16) 0.0176(16) 0.0136(17) -0.0043(13) 0.0000(13) -0.0053(14) N14 0.0121(16) 0.0195(16) 0.0138(17) -0.0037(13) -0.0009(13) -0.0040(13) N15 0.0169(16) 0.0161(16) 0.0141(17) -0.0001(13) 0.0003(14) -0.0054(14) N16 0.0176(17) 0.0199(17) 0.0176(18) -0.0063(14) 0.0001(14) -0.0055(14) N17 0.0174(16) 0.0178(16) 0.0117(16) -0.0037(13) 0.0030(13) -0.0078(14) N18 0.0174(16) 0.0186(16) 0.0134(17) -0.0052(13) 0.0025(13) -0.0087(14) N19 0.0163(16) 0.0229(17) 0.0145(17) -0.0066(14) 0.0015(14) -0.0070(14) N20 0.0207(17) 0.0260(18) 0.0130(17) -0.0059(14) 0.0021(14) -0.0111(15) N21 0.0208(17) 0.0168(16) 0.0127(17) -0.0051(13) 0.0051(14) -0.0080(14) N23 0.0207(17) 0.0205(17) 0.0141(17) -0.0041(14) 0.0007(14) -0.0096(14) N25 0.054(3) 0.050(3) 0.050(3) -0.020(3) 0.010(3) -0.019(3) N26 0.032(2) 0.040(2) 0.027(2) -0.0003(19) -0.0023(18) -0.0138(19) N27 0.096(5) 0.057(3) 0.042(3) -0.012(3) 0.016(3) -0.053(4) O1 0.0319(16) 0.0248(15) 0.0150(15) -0.0046(12) 0.0080(13) -0.0167(13) O2 0.0257(15) 0.0301(16) 0.0147(15) -0.0066(12) 0.0051(12) -0.0172(13) O3 0.0283(16) 0.0315(16) 0.0169(16) -0.0051(13) -0.0040(13) -0.0107(14) O5 0.0397(19) 0.0282(17) 0.0192(17) 0.0038(14) -0.0055(14) -0.0144(15) O6 0.0341(17) 0.0239(15) 0.0189(16) -0.0012(13) 0.0074(13) -0.0130(14) O7 0.0195(14) 0.0275(15) 0.0204(15) -0.0089(13) 0.0009(12) -0.0089(12) O8 0.0242(15) 0.0310(16) 0.0140(14) -0.0091(12) 0.0054(12) -0.0153(13) O9 0.0276(15) 0.0245(15) 0.0113(14) -0.0057(12) 0.0042(12) -0.0135(13) O10 0.0292(17) 0.0275(16) 0.0161(16) -0.0020(13) 0.0019(13) -0.0057(13) O11 0.0292(17) 0.0345(17) 0.0165(16) -0.0021(14) -0.0040(13) -0.0122(14) O12 0.0311(17) 0.0319(17) 0.0243(17) -0.0036(14) -0.0082(14) -0.0120(14) O13 0.073(3) 0.054(3) 0.065(3) -0.017(2) 0.001(3) -0.017(2) O14 0.112(5) 0.072(3) 0.086(4) -0.038(3) 0.062(4) -0.021(3) O15 0.148(6) 0.065(3) 0.088(4) -0.031(3) 0.076(4) -0.057(4) O16 0.058(3) 0.070(3) 0.059(3) -0.028(2) -0.015(2) -0.019(2) O17 0.084(3) 0.082(3) 0.067(3) -0.007(3) 0.019(3) -0.063(3) O18 0.056(3) 0.060(3) 0.039(2) 0.000(2) 0.018(2) -0.023(2) O19 0.079(3) 0.070(3) 0.050(3) -0.027(2) 0.026(2) -0.034(3) O20 0.125(5) 0.084(4) 0.053(3) -0.021(3) 0.009(3) -0.019(4) O21 0.077(4) 0.077(4) 0.082(4) -0.028(3) 0.013(3) -0.027(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 O1W Dy1 2.391(3) . ? O2W Dy1 2.348(3) . ? O3W Dy1 2.409(3) . ? O4W Dy1 2.325(3) . ? Dy1 O9 2.333(3) . ? Dy1 O2 2.366(3) . ? Dy1 O1 2.388(3) . ? Dy1 O8 2.414(3) . ? O4 C4 1.221(5) . ? C4 N4 1.361(6) . ? C4 N3 1.366(5) . ? C17 N3 1.445(5) 2_667 ? C17 N10 1.455(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.452(5) 2_667 ? C18 N1 1.455(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C45 N24 1.458(5) . ? C45 N22 1.472(5) . ? C45 C60 1.525(6) . ? C45 C44 1.564(6) . ? C57 C58 1.526(6) . ? C57 C44 1.530(5) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 C59 1.525(7) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 C60 1.534(6) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? N3 C17 1.445(5) 2_667 ? N3 C2 1.452(5) . ? N22 C43 1.347(5) . ? N22 C48 1.450(5) 2_576 ? N24 C46 1.364(5) . ? N24 C47 1.459(5) 2_576 ? C1 O1 1.234(5) . ? C1 N1 1.354(5) . ? C1 N2 1.361(5) . ? C2 N1 1.470(5) . ? C2 C19 1.527(6) . ? C2 C3 1.573(5) . ? C3 N2 1.452(5) . ? C3 N4 1.454(5) . ? C3 C22 1.532(6) . ? C5 N5 1.439(5) . ? C5 N2 1.449(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.451(6) . ? C6 N4 1.459(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.230(5) . ? C7 N5 1.352(5) . ? C7 N6 1.356(5) . ? C8 N7 1.458(5) . ? C8 N5 1.463(5) . ? C8 C23 1.530(6) . ? C8 C9 1.568(6) . ? C9 N6 1.460(5) . ? C9 N8 1.463(5) . ? C9 C26 1.532(5) . ? C10 O5 1.222(5) . ? C10 N8 1.361(6) . ? C10 N7 1.361(6) . ? C11 N9 1.447(5) . ? C11 N6 1.450(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.450(5) . ? C12 N11 1.452(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.213(5) . ? C13 N9 1.371(6) . ? C13 N10 1.373(5) . ? C14 N9 1.463(5) . ? C14 N11 1.464(5) . ? C14 C27 1.517(6) . ? C14 C15 1.577(6) . ? C15 N10 1.448(5) . ? C15 N12 1.462(5) . ? C15 C30 1.529(6) . ? C16 O6 1.217(5) . ? C16 N11 1.368(5) . ? C16 N12 1.374(6) . ? C19 C20 1.517(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.518(7) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.525(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.532(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.530(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.523(7) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.522(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.534(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.512(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O7 1.215(5) . ? C31 N14 1.368(5) . ? C31 N13 1.372(5) . ? C32 N13 1.457(5) . ? C32 N15 1.466(5) . ? C32 C49 1.525(6) . ? C32 C33 1.585(5) . ? C33 N16 1.440(5) . ? C33 N14 1.471(5) . ? C33 C52 1.518(6) . ? C34 O10 1.215(5) . ? C34 N15 1.366(5) . ? C34 N16 1.373(5) . ? C35 N14 1.450(5) . ? C35 N17 1.460(5) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N19 1.448(5) . ? C36 N16 1.458(5) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O8 1.230(5) . ? C37 N18 1.349(5) . ? C37 N17 1.357(5) . ? C38 N19 1.449(5) . ? C38 N17 1.475(5) . ? C38 C53 1.526(6) . ? C38 C39 1.575(6) . ? C39 N20 1.458(5) . ? C39 N18 1.459(5) . ? C39 C56 1.519(5) . ? C40 O11 1.220(5) . ? C40 N19 1.361(6) . ? C40 N20 1.373(5) . ? C41 N21 1.445(5) . ? C41 N18 1.454(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N20 1.443(5) . ? C42 N23 1.451(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 O9 1.234(5) . ? C43 N21 1.359(5) . ? C44 N21 1.451(5) . ? C44 N23 1.459(5) . ? C46 O12 1.217(5) . ? C46 N23 1.375(5) . ? C47 N13 1.451(5) . ? C47 N24 1.459(5) 2_576 ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 N22 1.450(5) 2_576 ? C48 N15 1.449(5) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.526(6) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.531(6) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.525(6) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.515(7) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.529(7) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.534(7) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? N12 C18 1.452(5) 2_667 ? N25 O15 1.220(7) . ? N25 O13 1.222(7) . ? N25 O14 1.238(7) . ? N26 O18 1.222(6) . ? N26 O17 1.229(6) . ? N26 O16 1.236(6) . ? N27 O20 1.184(7) . ? N27 O21 1.250(8) . ? N27 O19 1.293(7) . ? 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 O4W Dy1 O9 97.04(11) . . ? O4W Dy1 O2W 140.39(11) . . ? O9 Dy1 O2W 94.80(10) . . ? O4W Dy1 O2 96.82(11) . . ? O9 Dy1 O2 138.30(10) . . ? O2W Dy1 O2 99.02(10) . . ? O4W Dy1 O1 76.42(11) . . ? O9 Dy1 O1 146.26(10) . . ? O2W Dy1 O1 72.91(10) . . ? O2 Dy1 O1 75.37(10) . . ? O4W Dy1 O1W 72.10(11) . . ? O9 Dy1 O1W 75.27(10) . . ? O2W Dy1 O1W 147.48(11) . . ? O2 Dy1 O1W 72.03(10) . . ? O1 Dy1 O1W 130.81(10) . . ? O4W Dy1 O3W 147.33(11) . . ? O9 Dy1 O3W 74.80(10) . . ? O2W Dy1 O3W 72.28(11) . . ? O2 Dy1 O3W 72.41(10) . . ? O1 Dy1 O3W 127.24(11) . . ? O1W Dy1 O3W 75.24(11) . . ? O4W Dy1 O8 72.56(10) . . ? O9 Dy1 O8 75.88(10) . . ? O2W Dy1 O8 73.99(10) . . ? O2 Dy1 O8 145.80(10) . . ? O1 Dy1 O8 70.57(10) . . ? O1W Dy1 O8 130.48(10) . . ? O3W Dy1 O8 132.59(10) . . ? O4 C4 N4 126.4(4) . . ? O4 C4 N3 125.0(4) . . ? N4 C4 N3 108.6(3) . . ? N3 C17 N10 114.6(3) 2_667 . ? N3 C17 H17A 108.6 2_667 . ? N10 C17 H17A 108.6 . . ? N3 C17 H17B 108.6 2_667 . ? N10 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? N12 C18 N1 114.5(3) 2_667 . ? N12 C18 H18A 108.6 2_667 . ? N1 C18 H18A 108.6 . . ? N12 C18 H18B 108.6 2_667 . ? N1 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? N24 C45 N22 112.1(3) . . ? N24 C45 C60 113.7(3) . . ? N22 C45 C60 112.6(3) . . ? N24 C45 C44 103.2(3) . . ? N22 C45 C44 102.2(3) . . ? C60 C45 C44 112.1(3) . . ? C58 C57 C44 109.6(3) . . ? C58 C57 H57A 109.8 . . ? C44 C57 H57A 109.8 . . ? C58 C57 H57B 109.8 . . ? C44 C57 H57B 109.8 . . ? H57A C57 H57B 108.2 . . ? C59 C58 C57 112.3(4) . . ? C59 C58 H58A 109.2 . . ? C57 C58 H58A 109.2 . . ? C59 C58 H58B 109.2 . . ? C57 C58 H58B 109.2 . . ? H58A C58 H58B 107.9 . . ? C58 C59 C60 113.2(4) . . ? C58 C59 H59A 108.9 . . ? C60 C59 H59A 108.9 . . ? C58 C59 H59B 108.9 . . ? C60 C59 H59B 108.9 . . ? H59A C59 H59B 107.7 . . ? C45 C60 C59 111.9(4) . . ? C45 C60 H60A 109.2 . . ? C59 C60 H60A 109.2 . . ? C45 C60 H60B 109.2 . . ? C59 C60 H60B 109.2 . . ? H60A C60 H60B 107.9 . . ? C4 N3 C17 120.9(3) . 2_667 ? C4 N3 C2 112.6(3) . . ? C17 N3 C2 126.2(3) 2_667 . ? C43 N22 C48 121.2(3) . 2_576 ? C43 N22 C45 112.3(3) . . ? C48 N22 C45 124.4(3) 2_576 . ? C46 N24 C45 112.7(3) . . ? C46 N24 C47 121.2(3) . 2_576 ? C45 N24 C47 125.9(3) . 2_576 ? O1 C1 N1 125.1(4) . . ? O1 C1 N2 125.0(4) . . ? N1 C1 N2 109.9(3) . . ? N3 C2 N1 112.7(3) . . ? N3 C2 C19 113.6(3) . . ? N1 C2 C19 112.2(3) . . ? N3 C2 C3 102.9(3) . . ? N1 C2 C3 103.0(3) . . ? C19 C2 C3 111.5(3) . . ? N2 C3 N4 113.5(3) . . ? N2 C3 C22 112.2(3) . . ? N4 C3 C22 113.0(3) . . ? N2 C3 C2 102.5(3) . . ? N4 C3 C2 102.5(3) . . ? C22 C3 C2 112.4(3) . . ? N5 C5 N2 113.7(3) . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5B 108.8 . . ? N2 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N4 114.3(3) . . ? N7 C6 H6A 108.7 . . ? N4 C6 H6A 108.7 . . ? N7 C6 H6B 108.7 . . ? N4 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N5 125.1(4) . . ? O2 C7 N6 125.3(4) . . ? N5 C7 N6 109.6(3) . . ? N7 C8 N5 112.6(3) . . ? N7 C8 C23 113.1(4) . . ? N5 C8 C23 112.0(3) . . ? N7 C8 C9 102.5(3) . . ? N5 C8 C9 102.6(3) . . ? C23 C8 C9 113.2(3) . . ? N6 C9 N8 112.6(3) . . ? N6 C9 C26 113.2(4) . . ? N8 C9 C26 113.2(3) . . ? N6 C9 C8 102.7(3) . . ? N8 C9 C8 102.8(3) . . ? C26 C9 C8 111.3(3) . . ? O5 C10 N8 125.5(4) . . ? O5 C10 N7 125.8(4) . . ? N8 C10 N7 108.7(4) . . ? N9 C11 N6 114.7(3) . . ? N9 C11 H11A 108.6 . . ? N6 C11 H11A 108.6 . . ? N9 C11 H11B 108.6 . . ? N6 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? N8 C12 N11 115.3(3) . . ? N8 C12 H12A 108.4 . . ? N11 C12 H12A 108.4 . . ? N8 C12 H12B 108.4 . . ? N11 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? O3 C13 N9 126.4(4) . . ? O3 C13 N10 125.1(4) . . ? N9 C13 N10 108.5(4) . . ? N9 C14 N11 111.4(3) . . ? N9 C14 C27 114.2(3) . . ? N11 C14 C27 112.5(3) . . ? N9 C14 C15 102.7(3) . . ? N11 C14 C15 102.7(3) . . ? C27 C14 C15 112.3(3) . . ? N10 C15 N12 112.7(3) . . ? N10 C15 C30 113.3(4) . . ? N12 C15 C30 112.5(3) . . ? N10 C15 C14 103.0(3) . . ? N12 C15 C14 102.7(3) . . ? C30 C15 C14 111.7(3) . . ? O6 C16 N11 126.1(4) . . ? O6 C16 N12 125.6(4) . . ? N11 C16 N12 108.2(4) . . ? C20 C19 C2 110.5(4) . . ? C20 C19 H19A 109.5 . . ? C2 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? C2 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C19 C20 C21 112.7(4) . . ? C19 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C20 C21 C22 113.4(4) . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C21 C22 C3 111.2(4) . . ? C21 C22 H22A 109.4 . . ? C3 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C3 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C8 C23 C24 109.0(4) . . ? C8 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? C8 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? C25 C24 C23 111.9(4) . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C24 113.9(4) . . ? C26 C25 H25A 108.8 . . ? C24 C25 H25A 108.8 . . ? C26 C25 H25B 108.8 . . ? C24 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C25 C26 C9 111.1(4) . . ? C25 C26 H26A 109.4 . . ? C9 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? C9 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C14 C27 C28 111.7(4) . . ? C14 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C14 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C29 112.6(4) . . ? C27 C28 H28A 109.1 . . ? C29 C28 H28A 109.1 . . ? C27 C28 H28B 109.1 . . ? C29 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? C30 C29 C28 113.3(4) . . ? C30 C29 H29A 108.9 . . ? C28 C29 H29A 108.9 . . ? C30 C29 H29B 108.9 . . ? C28 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C29 C30 C15 111.2(4) . . ? C29 C30 H30A 109.4 . . ? C15 C30 H30A 109.4 . . ? C29 C30 H30B 109.4 . . ? C15 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? O7 C31 N14 125.9(4) . . ? O7 C31 N13 125.6(4) . . ? N14 C31 N13 108.5(3) . . ? N13 C32 N15 111.9(3) . . ? N13 C32 C49 113.9(3) . . ? N15 C32 C49 113.4(3) . . ? N13 C32 C33 103.2(3) . . ? N15 C32 C33 102.0(3) . . ? C49 C32 C33 111.4(3) . . ? N16 C33 N14 112.4(3) . . ? N16 C33 C52 112.9(3) . . ? N14 C33 C52 113.2(3) . . ? N16 C33 C32 103.1(3) . . ? N14 C33 C32 101.8(3) . . ? C52 C33 C32 112.4(3) . . ? O10 C34 N15 126.5(4) . . ? O10 C34 N16 125.1(4) . . ? N15 C34 N16 108.3(3) . . ? N14 C35 N17 114.1(3) . . ? N14 C35 H35A 108.7 . . ? N17 C35 H35A 108.7 . . ? N14 C35 H35B 108.7 . . ? N17 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? N19 C36 N16 114.0(3) . . ? N19 C36 H36A 108.7 . . ? N16 C36 H36A 108.7 . . ? N19 C36 H36B 108.7 . . ? N16 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? O8 C37 N18 125.5(4) . . ? O8 C37 N17 124.7(4) . . ? N18 C37 N17 109.8(3) . . ? N19 C38 N17 112.1(3) . . ? N19 C38 C53 114.1(3) . . ? N17 C38 C53 112.4(3) . . ? N19 C38 C39 102.7(3) . . ? N17 C38 C39 102.7(3) . . ? C53 C38 C39 111.7(3) . . ? N20 C39 N18 112.9(3) . . ? N20 C39 C56 113.1(3) . . ? N18 C39 C56 112.8(3) . . ? N20 C39 C38 102.7(3) . . ? N18 C39 C38 102.2(3) . . ? C56 C39 C38 112.2(3) . . ? O11 C40 N19 126.2(4) . . ? O11 C40 N20 125.4(4) . . ? N19 C40 N20 108.4(3) . . ? N21 C41 N18 114.1(3) . . ? N21 C41 H41A 108.7 . . ? N18 C41 H41A 108.7 . . ? N21 C41 H41B 108.7 . . ? N18 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? N20 C42 N23 114.3(3) . . ? N20 C42 H42A 108.7 . . ? N23 C42 H42A 108.7 . . ? N20 C42 H42B 108.7 . . ? N23 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? O9 C43 N22 125.5(4) . . ? O9 C43 N21 124.9(4) . . ? N22 C43 N21 109.6(3) . . ? N21 C44 N23 113.1(3) . . ? N21 C44 C57 112.3(3) . . ? N23 C44 C57 112.3(3) . . ? N21 C44 C45 103.1(3) . . ? N23 C44 C45 102.7(3) . . ? C57 C44 C45 112.5(3) . . ? O12 C46 N24 125.9(4) . . ? O12 C46 N23 125.5(4) . . ? N24 C46 N23 108.5(3) . . ? N13 C47 N24 115.2(3) . 2_576 ? N13 C47 H47A 108.5 . . ? N24 C47 H47A 108.5 2_576 . ? N13 C47 H47B 108.5 . . ? N24 C47 H47B 108.5 2_576 . ? H47A C47 H47B 107.5 . . ? N22 C48 N15 114.5(3) 2_576 . ? N22 C48 H48A 108.6 2_576 . ? N15 C48 H48A 108.6 . . ? N22 C48 H48B 108.6 2_576 . ? N15 C48 H48B 108.6 . . ? H48A C48 H48B 107.6 . . ? C32 C49 C50 112.4(4) . . ? C32 C49 H49A 109.1 . . ? C50 C49 H49A 109.1 . . ? C32 C49 H49B 109.1 . . ? C50 C49 H49B 109.1 . . ? H49A C49 H49B 107.9 . . ? C49 C50 C51 113.2(4) . . ? C49 C50 H50A 108.9 . . ? C51 C50 H50A 108.9 . . ? C49 C50 H50B 108.9 . . ? C51 C50 H50B 108.9 . . ? H50A C50 H50B 107.7 . . ? C52 C51 C50 112.3(4) . . ? C52 C51 H51A 109.1 . . ? C50 C51 H51A 109.1 . . ? C52 C51 H51B 109.1 . . ? C50 C51 H51B 109.1 . . ? H51A C51 H51B 107.9 . . ? C33 C52 C51 111.2(4) . . ? C33 C52 H52A 109.4 . . ? C51 C52 H52A 109.4 . . ? C33 C52 H52B 109.4 . . ? C51 C52 H52B 109.4 . . ? H52A C52 H52B 108.0 . . ? C54 C53 C38 110.4(4) . . ? C54 C53 H53A 109.6 . . ? C38 C53 H53A 109.6 . . ? C54 C53 H53B 109.6 . . ? C38 C53 H53B 109.6 . . ? H53A C53 H53B 108.1 . . ? C53 C54 C55 113.0(4) . . ? C53 C54 H54A 109.0 . . ? C55 C54 H54A 109.0 . . ? C53 C54 H54B 109.0 . . ? C55 C54 H54B 109.0 . . ? H54A C54 H54B 107.8 . . ? C54 C55 C56 112.5(4) . . ? C54 C55 H55A 109.1 . . ? C56 C55 H55A 109.1 . . ? C54 C55 H55B 109.1 . . ? C56 C55 H55B 109.1 . . ? H55A C55 H55B 107.8 . . ? C39 C56 C55 111.3(4) . . ? C39 C56 H56A 109.4 . . ? C55 C56 H56A 109.4 . . ? C39 C56 H56B 109.4 . . ? C55 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? C1 N1 C18 120.9(3) . . ? C1 N1 C2 111.6(3) . . ? C18 N1 C2 125.3(3) . . ? C1 N2 C5 121.8(3) . . ? C1 N2 C3 112.7(3) . . ? C5 N2 C3 125.5(3) . . ? C4 N4 C3 112.7(3) . . ? C4 N4 C6 120.5(3) . . ? C3 N4 C6 125.7(3) . . ? C7 N5 C5 122.7(3) . . ? C7 N5 C8 112.5(3) . . ? C5 N5 C8 124.8(3) . . ? C7 N6 C11 121.2(3) . . ? C7 N6 C9 112.4(3) . . ? C11 N6 C9 124.7(3) . . ? C10 N7 C6 121.1(4) . . ? C10 N7 C8 113.0(4) . . ? C6 N7 C8 125.2(4) . . ? C10 N8 C12 121.5(4) . . ? C10 N8 C9 112.7(3) . . ? C12 N8 C9 125.5(4) . . ? C13 N9 C11 120.7(3) . . ? C13 N9 C14 112.5(3) . . ? C11 N9 C14 124.6(3) . . ? C13 N10 C15 113.1(3) . . ? C13 N10 C17 120.8(3) . . ? C15 N10 C17 125.2(3) . . ? C16 N11 C12 120.6(4) . . ? C16 N11 C14 113.2(3) . . ? C12 N11 C14 125.3(3) . . ? C16 N12 C18 120.8(3) . 2_667 ? C16 N12 C15 113.0(3) . . ? C18 N12 C15 125.2(3) 2_667 . ? C31 N13 C47 121.7(3) . . ? C31 N13 C32 112.9(3) . . ? C47 N13 C32 125.0(3) . . ? C31 N14 C35 120.4(3) . . ? C31 N14 C33 113.2(3) . . ? C35 N14 C33 124.8(3) . . ? C34 N15 C48 120.2(3) . . ? C34 N15 C32 112.9(3) . . ? C48 N15 C32 123.9(3) . . ? C34 N16 C33 113.3(3) . . ? C34 N16 C36 121.3(3) . . ? C33 N16 C36 125.0(3) . . ? C37 N17 C35 121.2(3) . . ? C37 N17 C38 111.7(3) . . ? C35 N17 C38 124.8(3) . . ? C37 N18 C41 122.2(3) . . ? C37 N18 C39 113.2(3) . . ? C41 N18 C39 124.6(3) . . ? C40 N19 C36 121.1(3) . . ? C40 N19 C38 113.3(3) . . ? C36 N19 C38 125.2(3) . . ? C40 N20 C42 121.1(3) . . ? C40 N20 C39 112.3(3) . . ? C42 N20 C39 125.6(3) . . ? C43 N21 C41 122.5(3) . . ? C43 N21 C44 112.3(3) . . ? C41 N21 C44 125.2(3) . . ? C46 N23 C42 121.5(3) . . ? C46 N23 C44 112.5(3) . . ? C42 N23 C44 125.0(3) . . ? O15 N25 O13 119.8(5) . . ? O15 N25 O14 120.2(6) . . ? O13 N25 O14 119.9(6) . . ? O18 N26 O17 120.0(5) . . ? O18 N26 O16 120.5(5) . . ? O17 N26 O16 119.5(5) . . ? O20 N27 O21 118.8(7) . . ? O20 N27 O19 120.9(7) . . ? O21 N27 O19 120.2(6) . . ? C1 O1 Dy1 155.6(3) . . ? C7 O2 Dy1 155.5(3) . . ? C37 O8 Dy1 156.3(3) . . ? C43 O9 Dy1 158.8(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.214 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.118 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 108 24 ' ' 2 0.225 0.127 0.721 211 70 ' ' 3 -0.162 0.459 0.652 60 21 ' ' 4 0.159 0.543 0.348 61 20 ' ' 5 -0.225 0.874 0.279 208 69 ' ' 6 0.500 0.500 0.000 116 32 ' ' 7 0.474 0.513 0.344 18 9 ' ' 8 0.526 0.487 0.656 17 8 ' ' _platon_squeeze_details ; ; data_p3 _database_code_depnum_ccdc_archive 'CCDC 881900' #TrackingRef '110320qx-submit-cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H106 N27 O38 Yb' _chemical_formula_weight 1986.76 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.8602(7) _cell_length_b 15.9685(6) _cell_length_c 18.0548(8) _cell_angle_alpha 74.9100(10) _cell_angle_beta 89.449(2) _cell_angle_gamma 63.4040(10) _cell_volume 3917.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2058 _exptl_absorpt_coefficient_mu 1.308 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7029 _exptl_absorpt_correction_T_max 0.7618 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41677 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13625 _reflns_number_gt 12566 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+4.0003P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13625 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 O1W O 0.75720(17) 0.44501(16) 0.21610(13) 0.0262(5) Uani 1 1 d . . . O2W O 0.93693(16) 0.27425(17) 0.23565(13) 0.0258(5) Uani 1 1 d . . . O3W O 0.89198(16) 0.12394(16) 0.25526(13) 0.0250(5) Uani 1 1 d . . . O4W O 0.62573(16) 0.37932(17) 0.22657(14) 0.0286(5) Uani 1 1 d . . . Yb1 Yb 0.785111(9) 0.283816(9) 0.237285(7) 0.01659(6) Uani 1 1 d . . . C1 C 0.6926(2) 0.1847(2) 0.12532(17) 0.0179(6) Uani 1 1 d . . . C2 C 0.6207(2) 0.1239(2) 0.05536(17) 0.0178(6) Uani 1 1 d . . . C3 C 0.7120(2) 0.1216(2) 0.01938(18) 0.0183(6) Uani 1 1 d . . . C4 C 0.5789(2) 0.2223(2) -0.07347(18) 0.0205(7) Uani 1 1 d . . . C5 C 0.8387(2) 0.1618(2) 0.06682(17) 0.0177(6) Uani 1 1 d . . . H5A H 0.8646 0.1527 0.1190 0.021 Uiso 1 1 calc R . . H5B H 0.8841 0.1078 0.0485 0.021 Uiso 1 1 calc R . . C6 C 0.7292(2) 0.2121(2) -0.11607(18) 0.0216(7) Uani 1 1 d . . . H6A H 0.6935 0.2317 -0.1668 0.026 Uiso 1 1 calc R . . H6B H 0.7883 0.1524 -0.1125 0.026 Uiso 1 1 calc R . . C7 C 0.8114(2) 0.3315(2) 0.04222(18) 0.0173(6) Uani 1 1 d . . . C8 C 0.8368(2) 0.2727(2) -0.06570(17) 0.0193(6) Uani 1 1 d . . . C9 C 0.8311(2) 0.3770(2) -0.08824(17) 0.0181(6) Uani 1 1 d . . . C10 C 0.7056(2) 0.3813(2) -0.15978(18) 0.0201(7) Uani 1 1 d . . . C11 C 0.8116(2) 0.4889(2) -0.00210(18) 0.0192(6) Uani 1 1 d . . . H11A H 0.8228 0.4772 0.0538 0.023 Uiso 1 1 calc R . . H11B H 0.8653 0.4956 -0.0249 0.023 Uiso 1 1 calc R . . C12 C 0.7229(2) 0.5316(2) -0.19888(18) 0.0210(7) Uani 1 1 d . . . H12A H 0.7808 0.5361 -0.2133 0.025 Uiso 1 1 calc R . . H12B H 0.6861 0.5414 -0.2464 0.025 Uiso 1 1 calc R . . C13 C 0.6711(2) 0.6290(2) 0.01532(18) 0.0197(6) Uani 1 1 d . . . C14 C 0.7072(2) 0.6424(2) -0.11238(18) 0.0187(6) Uani 1 1 d . . . C15 C 0.6203(2) 0.7405(2) -0.10866(18) 0.0178(6) Uani 1 1 d . . . C16 C 0.5726(2) 0.6697(2) -0.18835(17) 0.0182(6) Uani 1 1 d . . . C17 C 0.5519(2) 0.7957(2) 0.00960(19) 0.0212(7) Uani 1 1 d . . . H17A H 0.5528 0.8572 -0.0168 0.025 Uiso 1 1 calc R . . H17B H 0.5798 0.7757 0.0634 0.025 Uiso 1 1 calc R . . C18 C 0.5524(2) 0.1755(2) 0.17639(18) 0.0192(6) Uani 1 1 d . . . H18A H 0.5813 0.1798 0.2221 0.023 Uiso 1 1 calc R . . H18B H 0.5471 0.1147 0.1911 0.023 Uiso 1 1 calc R . . C19 C 0.6280(2) 0.0223(2) 0.0862(2) 0.0252(7) Uani 1 1 d . . . H19A H 0.6253 -0.0032 0.0429 0.030 Uiso 1 1 calc R . . H19B H 0.5744 0.0259 0.1150 0.030 Uiso 1 1 calc R . . C20 C 0.7217(3) -0.0463(2) 0.1393(2) 0.0318(8) Uani 1 1 d . . . H20A H 0.7225 -0.0219 0.1837 0.038 Uiso 1 1 calc R . . H20B H 0.7256 -0.1114 0.1589 0.038 Uiso 1 1 calc R . . C21 C 0.8083(3) -0.0544(2) 0.0974(2) 0.0308(8) Uani 1 1 d . . . H21A H 0.8508 -0.0443 0.1291 0.037 Uiso 1 1 calc R . . H21B H 0.8429 -0.1207 0.0923 0.037 Uiso 1 1 calc R . . C22 C 0.7827(2) 0.0190(2) 0.0171(2) 0.0248(7) Uani 1 1 d . . . H22A H 0.8405 0.0198 -0.0018 0.030 Uiso 1 1 calc R . . H22B H 0.7551 -0.0013 -0.0188 0.030 Uiso 1 1 calc R . . C23 C 0.9284(2) 0.1968(2) -0.08449(19) 0.0231(7) Uani 1 1 d . . . H23A H 0.9822 0.1829 -0.0488 0.028 Uiso 1 1 calc R . . H23B H 0.9245 0.1358 -0.0783 0.028 Uiso 1 1 calc R . . C24 C 0.9436(2) 0.2353(2) -0.16735(19) 0.0270(7) Uani 1 1 d . . . H24A H 0.8894 0.2490 -0.2026 0.032 Uiso 1 1 calc R . . H24B H 1.0008 0.1848 -0.1800 0.032 Uiso 1 1 calc R . . C25 C 0.9545(3) 0.3285(3) -0.1800(2) 0.0322(8) Uani 1 1 d . . . H25A H 1.0214 0.3125 -0.1842 0.039 Uiso 1 1 calc R . . H25B H 0.9171 0.3754 -0.2289 0.039 Uiso 1 1 calc R . . C26 C 0.9222(2) 0.3763(2) -0.11449(19) 0.0233(7) Uani 1 1 d . . . H26A H 0.9724 0.3409 -0.0705 0.028 Uiso 1 1 calc R . . H26B H 0.9128 0.4437 -0.1321 0.028 Uiso 1 1 calc R . . C27 C 0.7911(2) 0.6588(2) -0.1395(2) 0.0250(7) Uani 1 1 d . . . H27A H 0.8418 0.5975 -0.1450 0.030 Uiso 1 1 calc R . . H27B H 0.8157 0.6770 -0.1000 0.030 Uiso 1 1 calc R . . C28 C 0.7652(3) 0.7383(3) -0.2162(2) 0.0327(8) Uani 1 1 d . . . H28A H 0.7594 0.7121 -0.2582 0.039 Uiso 1 1 calc R . . H28B H 0.8168 0.7563 -0.2245 0.039 Uiso 1 1 calc R . . C29 C 0.6723(3) 0.8302(3) -0.2196(2) 0.0293(8) Uani 1 1 d . . . H29A H 0.6823 0.8879 -0.2389 0.035 Uiso 1 1 calc R . . H29B H 0.6237 0.8353 -0.2560 0.035 Uiso 1 1 calc R . . C30 C 0.6366(2) 0.8290(2) -0.14073(19) 0.0237(7) Uani 1 1 d . . . H30A H 0.6834 0.8278 -0.1048 0.028 Uiso 1 1 calc R . . H30B H 0.5771 0.8887 -0.1456 0.028 Uiso 1 1 calc R . . C31 C 0.8684(2) -0.0966(2) 0.35977(18) 0.0204(7) Uani 1 1 d . . . C32 C 0.9006(2) -0.2383(2) 0.46134(18) 0.0192(6) Uani 1 1 d . . . C33 C 0.7988(2) -0.1547(2) 0.46326(18) 0.0200(6) Uani 1 1 d . . . C34 C 0.8954(2) -0.1988(2) 0.57866(18) 0.0212(7) Uani 1 1 d . . . C35 C 0.7079(2) 0.0203(2) 0.37212(18) 0.0196(6) Uani 1 1 d . . . H35A H 0.6528 0.0079 0.3701 0.024 Uiso 1 1 calc R . . H35B H 0.7132 0.0518 0.3192 0.024 Uiso 1 1 calc R . . C36 C 0.7266(2) -0.0861(2) 0.57595(18) 0.0227(7) Uani 1 1 d . . . H36A H 0.6724 -0.0952 0.5620 0.027 Uiso 1 1 calc R . . H36B H 0.7434 -0.1133 0.6321 0.027 Uiso 1 1 calc R . . C37 C 0.6975(2) 0.1711(2) 0.38970(18) 0.0184(6) Uani 1 1 d . . . C38 C 0.6386(2) 0.0897(2) 0.48604(18) 0.0200(6) Uani 1 1 d . . . C39 C 0.6217(2) 0.1887(2) 0.50043(18) 0.0206(7) Uani 1 1 d . . . C40 C 0.7190(2) 0.0569(2) 0.60687(18) 0.0215(7) Uani 1 1 d . . . C41 C 0.6538(2) 0.3267(2) 0.41672(17) 0.0183(6) Uani 1 1 d . . . H41A H 0.6492 0.3525 0.3606 0.022 Uiso 1 1 calc R . . H41B H 0.5962 0.3710 0.4339 0.022 Uiso 1 1 calc R . . C42 C 0.6892(3) 0.2179(2) 0.61559(18) 0.0249(7) Uani 1 1 d . . . H42A H 0.7055 0.1824 0.6708 0.030 Uiso 1 1 calc R . . H42B H 0.6269 0.2750 0.6090 0.030 Uiso 1 1 calc R . . C43 C 0.8132(2) 0.3149(2) 0.41748(17) 0.0180(6) Uani 1 1 d . . . C44 C 0.7416(2) 0.3386(2) 0.52926(17) 0.0190(6) Uani 1 1 d . . . C45 C 0.8385(2) 0.3429(2) 0.53409(18) 0.0202(6) Uani 1 1 d . . . C46 C 0.8464(2) 0.2099(2) 0.63330(18) 0.0224(7) Uani 1 1 d . . . C47 C 0.9560(2) 0.3355(2) 0.43298(18) 0.0202(6) Uani 1 1 d . . . H47A H 0.9494 0.3471 0.3768 0.024 Uiso 1 1 calc R . . H47B H 0.9539 0.3939 0.4429 0.024 Uiso 1 1 calc R . . C48 C 0.9836(2) 0.2417(2) 0.64041(18) 0.0227(7) Uani 1 1 d . . . H48A H 0.9807 0.3038 0.6421 0.027 Uiso 1 1 calc R . . H48B H 0.9917 0.2021 0.6939 0.027 Uiso 1 1 calc R . . C49 C 0.8972(2) -0.3286(2) 0.4533(2) 0.0264(7) Uani 1 1 d . . . H49A H 0.8773 -0.3581 0.5003 0.032 Uiso 1 1 calc R . . H49B H 0.9610 -0.3763 0.4478 0.032 Uiso 1 1 calc R . . C50 C 0.8286(3) -0.3048(3) 0.3836(2) 0.0324(8) Uani 1 1 d . . . H50A H 0.8216 -0.3630 0.3847 0.039 Uiso 1 1 calc R . . H50B H 0.8557 -0.2882 0.3363 0.039 Uiso 1 1 calc R . . C51 C 0.7305(3) -0.2200(3) 0.3811(2) 0.0345(9) Uani 1 1 d . . . H51A H 0.7187 -0.1660 0.3348 0.041 Uiso 1 1 calc R . . H51B H 0.6820 -0.2414 0.3771 0.041 Uiso 1 1 calc R . . C52 C 0.7212(2) -0.1836(2) 0.4525(2) 0.0263(7) Uani 1 1 d . . . H52A H 0.6588 -0.1270 0.4469 0.032 Uiso 1 1 calc R . . H52B H 0.7259 -0.2351 0.4984 0.032 Uiso 1 1 calc R . . C53 C 0.5450(2) 0.0880(2) 0.47183(19) 0.0240(7) Uani 1 1 d . . . H53A H 0.5161 0.0835 0.5200 0.029 Uiso 1 1 calc R . . H53B H 0.5568 0.0304 0.4551 0.029 Uiso 1 1 calc R . . C54 C 0.4770(2) 0.1806(3) 0.4098(2) 0.0290(8) Uani 1 1 d . . . H54A H 0.4178 0.1776 0.4007 0.035 Uiso 1 1 calc R . . H54B H 0.5054 0.1833 0.3614 0.035 Uiso 1 1 calc R . . C55 C 0.4543(2) 0.2739(3) 0.4325(2) 0.0313(8) Uani 1 1 d . . . H55A H 0.3876 0.3038 0.4418 0.038 Uiso 1 1 calc R . . H55B H 0.4625 0.3205 0.3894 0.038 Uiso 1 1 calc R . . C56 C 0.5179(2) 0.2542(2) 0.5051(2) 0.0269(7) Uani 1 1 d . . . H56A H 0.5108 0.3164 0.5107 0.032 Uiso 1 1 calc R . . H56B H 0.4977 0.2228 0.5509 0.032 Uiso 1 1 calc R . . C57 C 0.6573(2) 0.4302(2) 0.5381(2) 0.0268(7) Uani 1 1 d . . . H57A H 0.6006 0.4203 0.5419 0.032 Uiso 1 1 calc R . . H57B H 0.6447 0.4855 0.4926 0.032 Uiso 1 1 calc R . . C58 C 0.6794(3) 0.4524(3) 0.6107(2) 0.0384(9) Uani 1 1 d . . . H58A H 0.6881 0.3985 0.6561 0.046 Uiso 1 1 calc R . . H58B H 0.6253 0.5118 0.6158 0.046 Uiso 1 1 calc R . . C59 C 0.7691(3) 0.4663(3) 0.6084(3) 0.0434(10) Uani 1 1 d . . . H59A H 0.7509 0.5345 0.6057 0.052 Uiso 1 1 calc R . . H59B H 0.8113 0.4249 0.6567 0.052 Uiso 1 1 calc R . . C60 C 0.8236(3) 0.4419(2) 0.5408(2) 0.0293(8) Uani 1 1 d . . . H60A H 0.8854 0.4404 0.5482 0.035 Uiso 1 1 calc R . . H60B H 0.7882 0.4928 0.4929 0.035 Uiso 1 1 calc R . . N1 N 0.61525(18) 0.17057(18) 0.11689(15) 0.0179(5) Uani 1 1 d . . . N2 N 0.74989(18) 0.15680(19) 0.07088(14) 0.0186(5) Uani 1 1 d . . . N3 N 0.54593(18) 0.18728(19) -0.00863(15) 0.0196(5) Uani 1 1 d . . . N4 N 0.67394(19) 0.19041(19) -0.05681(15) 0.0208(6) Uani 1 1 d . . . N5 N 0.83051(19) 0.25245(19) 0.01681(14) 0.0188(5) Uani 1 1 d . . . N6 N 0.80908(18) 0.40468(18) -0.01595(15) 0.0182(5) Uani 1 1 d . . . N7 N 0.75257(19) 0.28843(19) -0.11092(15) 0.0197(5) Uani 1 1 d . . . N8 N 0.74998(19) 0.43376(18) -0.14908(14) 0.0192(5) Uani 1 1 d . . . N9 N 0.72595(18) 0.57976(18) -0.03305(15) 0.0188(5) Uani 1 1 d . . . N10 N 0.61014(18) 0.72202(19) -0.02689(15) 0.0201(6) Uani 1 1 d . . . N11 N 0.66760(18) 0.61024(18) -0.16561(15) 0.0189(5) Uani 1 1 d . . . N12 N 0.54276(18) 0.74252(18) -0.15383(15) 0.0187(5) Uani 1 1 d . . . N13 N 0.93379(19) -0.19160(19) 0.39518(15) 0.0213(6) Uani 1 1 d . . . N14 N 0.79190(19) -0.07210(18) 0.40029(15) 0.0206(6) Uani 1 1 d . . . N15 N 0.95209(19) -0.25377(19) 0.53454(15) 0.0204(6) Uani 1 1 d . . . N16 N 0.80650(19) -0.14086(19) 0.53901(15) 0.0208(6) Uani 1 1 d . . . N17 N 0.69014(19) 0.08776(19) 0.41801(14) 0.0187(5) Uani 1 1 d . . . N18 N 0.65755(19) 0.23137(19) 0.43436(15) 0.0194(5) Uani 1 1 d . . . N19 N 0.69771(19) 0.01751(19) 0.55580(15) 0.0204(6) Uani 1 1 d . . . N20 N 0.68213(19) 0.15553(19) 0.57375(15) 0.0207(6) Uani 1 1 d . . . N21 N 0.73529(19) 0.32594(19) 0.45256(15) 0.0193(5) Uani 1 1 d . . . N22 N 0.87549(18) 0.32319(18) 0.46280(14) 0.0183(5) Uani 1 1 d . . . N23 N 0.75946(19) 0.25152(19) 0.59134(15) 0.0214(6) Uani 1 1 d . . . N24 N 0.89313(19) 0.26209(19) 0.60211(15) 0.0205(6) Uani 1 1 d . . . O1 O 0.70886(16) 0.21654(16) 0.17579(12) 0.0220(5) Uani 1 1 d . . . O2 O 0.80040(16) 0.33388(15) 0.10948(12) 0.0205(5) Uani 1 1 d . . . O3 O 0.67539(17) 0.59603(17) 0.08522(13) 0.0264(5) Uani 1 1 d . . . O4 O 0.53185(17) 0.27299(17) -0.13600(13) 0.0278(5) Uani 1 1 d . . . O5 O 0.63617(18) 0.41128(17) -0.20658(14) 0.0301(5) Uani 1 1 d . . . O6 O 0.52371(16) 0.66069(16) -0.23466(13) 0.0241(5) Uani 1 1 d . . . O7 O 0.87610(17) -0.04435(16) 0.29980(13) 0.0273(5) Uani 1 1 d . . . O8 O 0.73308(16) 0.18977(16) 0.33047(12) 0.0223(5) Uani 1 1 d . . . O9 O 0.82647(15) 0.30111(16) 0.35320(12) 0.0216(5) Uani 1 1 d . . . O10 O 0.91927(17) -0.20116(17) 0.64353(13) 0.0267(5) Uani 1 1 d . . . O11 O 0.76261(17) 0.01221(17) 0.67124(13) 0.0282(5) Uani 1 1 d . . . O12 O 0.87664(18) 0.13909(17) 0.69097(13) 0.0312(6) Uani 1 1 d . . . N25 N 1.0673(2) 0.2185(3) 0.0869(2) 0.0395(8) Uani 1 1 d . . . N26 N 1.0924(3) 0.4357(3) 0.3338(2) 0.0440(9) Uani 1 1 d . . . N27 N 0.4919(2) 0.0528(2) 0.69642(17) 0.0309(7) Uani 1 1 d . . . O13 O 1.0454(3) 0.1700(3) 0.1423(2) 0.0694(11) Uani 1 1 d . . . O14 O 1.1263(3) 0.1772(3) 0.0474(2) 0.0715(11) Uani 1 1 d . . . O15 O 1.0261(2) 0.3085(2) 0.07122(19) 0.0541(8) Uani 1 1 d . . . O16 O 1.0341(2) 0.4932(2) 0.36816(19) 0.0573(8) Uani 1 1 d . . . O17 O 1.0724(3) 0.4453(3) 0.2665(2) 0.0879(14) Uani 1 1 d . . . O18 O 1.1716(3) 0.3710(3) 0.3678(2) 0.0640(9) Uani 1 1 d . . . O19 O 0.4916(2) 0.0059(2) 0.65205(18) 0.0528(8) Uani 1 1 d . . . O20 O 0.4552(2) 0.0445(2) 0.75713(16) 0.0476(7) Uani 1 1 d . . . O21 O 0.5285(3) 0.1083(3) 0.6812(2) 0.0589(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.0303(13) 0.0213(11) 0.0259(12) -0.0071(10) 0.0005(10) -0.0108(10) O2W 0.0232(12) 0.0308(12) 0.0218(12) -0.0066(10) -0.0005(10) -0.0116(10) O3W 0.0237(12) 0.0209(11) 0.0271(12) -0.0047(10) 0.0006(10) -0.0087(10) O4W 0.0229(12) 0.0288(12) 0.0314(13) -0.0086(11) -0.0011(10) -0.0096(10) Yb1 0.01909(8) 0.01853(8) 0.01293(8) -0.00450(5) 0.00091(5) -0.00932(6) C1 0.0184(15) 0.0162(14) 0.0160(15) -0.0033(12) -0.0008(12) -0.0060(12) C2 0.0175(15) 0.0188(15) 0.0158(15) -0.0071(12) 0.0006(12) -0.0061(13) C3 0.0197(15) 0.0167(14) 0.0189(15) -0.0060(12) 0.0032(13) -0.0081(13) C4 0.0225(16) 0.0200(15) 0.0216(17) -0.0123(14) 0.0031(14) -0.0086(13) C5 0.0162(15) 0.0183(15) 0.0151(15) -0.0041(12) 0.0005(12) -0.0054(12) C6 0.0277(17) 0.0245(16) 0.0145(15) -0.0081(13) 0.0024(13) -0.0123(14) C7 0.0159(15) 0.0201(15) 0.0192(16) -0.0079(13) 0.0032(12) -0.0099(13) C8 0.0201(16) 0.0208(15) 0.0147(15) -0.0059(13) 0.0023(13) -0.0072(13) C9 0.0195(15) 0.0186(15) 0.0135(14) -0.0032(12) 0.0015(13) -0.0071(13) C10 0.0199(16) 0.0230(16) 0.0145(15) -0.0057(13) 0.0027(13) -0.0070(13) C11 0.0182(15) 0.0194(15) 0.0191(15) -0.0068(13) 0.0007(13) -0.0072(13) C12 0.0242(16) 0.0216(16) 0.0151(15) -0.0053(13) 0.0038(13) -0.0088(14) C13 0.0178(15) 0.0227(16) 0.0202(16) -0.0063(13) -0.0013(13) -0.0104(13) C14 0.0189(15) 0.0195(15) 0.0172(15) -0.0057(13) 0.0012(13) -0.0082(13) C15 0.0171(15) 0.0201(15) 0.0176(15) -0.0067(13) 0.0029(12) -0.0091(13) C16 0.0206(16) 0.0201(15) 0.0155(15) -0.0037(12) 0.0039(13) -0.0115(13) C17 0.0203(16) 0.0245(16) 0.0216(16) -0.0109(13) 0.0006(13) -0.0104(14) C18 0.0190(15) 0.0182(15) 0.0162(15) -0.0022(12) 0.0011(13) -0.0065(13) C19 0.0270(17) 0.0235(17) 0.0283(18) -0.0093(14) 0.0056(15) -0.0135(15) C20 0.036(2) 0.0204(17) 0.0279(18) -0.0006(14) -0.0003(16) -0.0067(15) C21 0.0281(18) 0.0187(16) 0.035(2) -0.0051(15) -0.0015(16) -0.0035(14) C22 0.0217(16) 0.0227(16) 0.0292(18) -0.0124(14) 0.0033(14) -0.0068(14) C23 0.0203(16) 0.0209(16) 0.0225(17) -0.0087(13) 0.0025(13) -0.0034(13) C24 0.0228(17) 0.0301(18) 0.0201(17) -0.0098(14) 0.0060(14) -0.0041(15) C25 0.0295(19) 0.039(2) 0.0276(19) -0.0126(16) 0.0132(16) -0.0134(17) C26 0.0206(16) 0.0255(16) 0.0220(16) -0.0050(14) 0.0041(14) -0.0101(14) C27 0.0202(16) 0.0246(16) 0.0286(18) -0.0058(14) 0.0038(14) -0.0100(14) C28 0.033(2) 0.0308(19) 0.0289(19) -0.0025(16) 0.0090(16) -0.0131(16) C29 0.0297(19) 0.0263(17) 0.0289(18) -0.0016(15) 0.0032(15) -0.0137(15) C30 0.0247(17) 0.0191(15) 0.0260(17) -0.0043(14) -0.0012(14) -0.0099(14) C31 0.0237(16) 0.0201(15) 0.0175(16) -0.0068(13) -0.0019(13) -0.0094(13) C32 0.0197(15) 0.0195(15) 0.0176(15) -0.0028(13) -0.0024(13) -0.0095(13) C33 0.0238(16) 0.0211(15) 0.0162(15) -0.0054(13) -0.0005(13) -0.0111(14) C34 0.0242(16) 0.0206(15) 0.0222(17) -0.0050(13) 0.0013(14) -0.0137(14) C35 0.0229(16) 0.0184(15) 0.0153(15) -0.0046(12) -0.0013(13) -0.0077(13) C36 0.0268(17) 0.0228(16) 0.0174(15) -0.0023(13) 0.0035(14) -0.0122(14) C37 0.0155(15) 0.0206(15) 0.0172(15) -0.0048(13) -0.0013(12) -0.0070(13) C38 0.0216(16) 0.0215(15) 0.0160(15) -0.0033(13) 0.0029(13) -0.0103(13) C39 0.0202(16) 0.0242(16) 0.0198(16) -0.0077(13) 0.0053(13) -0.0116(14) C40 0.0204(16) 0.0277(17) 0.0162(16) -0.0056(14) 0.0046(13) -0.0114(14) C41 0.0189(15) 0.0200(15) 0.0145(14) -0.0050(12) -0.0006(12) -0.0076(13) C42 0.0334(19) 0.0282(17) 0.0162(16) -0.0101(14) 0.0077(14) -0.0148(15) C43 0.0221(16) 0.0137(14) 0.0164(15) -0.0034(12) 0.0001(13) -0.0073(13) C44 0.0225(16) 0.0197(15) 0.0127(14) -0.0059(12) -0.0016(13) -0.0072(13) C45 0.0214(16) 0.0195(15) 0.0172(15) -0.0062(13) -0.0003(13) -0.0067(13) C46 0.0277(17) 0.0222(16) 0.0185(16) -0.0112(14) 0.0039(14) -0.0096(14) C47 0.0228(16) 0.0209(15) 0.0154(15) -0.0013(12) -0.0035(13) -0.0107(13) C48 0.0230(16) 0.0257(16) 0.0179(16) -0.0100(13) 0.0003(13) -0.0079(14) C49 0.0261(17) 0.0220(16) 0.0317(19) -0.0099(14) -0.0016(15) -0.0105(14) C50 0.034(2) 0.0345(19) 0.035(2) -0.0159(16) -0.0040(16) -0.0177(17) C51 0.036(2) 0.035(2) 0.035(2) -0.0127(17) -0.0098(17) -0.0177(17) C52 0.0261(17) 0.0240(16) 0.0272(18) -0.0017(14) -0.0047(15) -0.0130(14) C53 0.0248(17) 0.0278(17) 0.0246(17) -0.0067(14) 0.0039(14) -0.0170(15) C54 0.0227(17) 0.0343(19) 0.0302(19) -0.0054(16) 0.0001(15) -0.0152(15) C55 0.0206(17) 0.0304(18) 0.036(2) -0.0076(16) 0.0001(15) -0.0070(15) C56 0.0241(17) 0.0265(17) 0.0299(18) -0.0109(15) 0.0098(15) -0.0101(15) C57 0.0265(18) 0.0221(16) 0.0279(18) -0.0100(14) 0.0063(15) -0.0064(14) C58 0.049(2) 0.0299(19) 0.035(2) -0.0209(17) 0.0088(18) -0.0102(18) C59 0.046(2) 0.038(2) 0.044(2) -0.0289(19) 0.0002(19) -0.0071(19) C60 0.0323(19) 0.0209(16) 0.0339(19) -0.0120(15) -0.0038(16) -0.0092(15) N1 0.0182(13) 0.0202(13) 0.0165(13) -0.0073(11) 0.0020(11) -0.0090(11) N2 0.0181(13) 0.0233(13) 0.0150(13) -0.0076(11) 0.0017(11) -0.0090(11) N3 0.0187(13) 0.0214(13) 0.0163(13) -0.0063(11) -0.0009(11) -0.0067(11) N4 0.0214(14) 0.0229(13) 0.0166(13) -0.0048(11) 0.0011(11) -0.0095(12) N5 0.0234(14) 0.0190(13) 0.0134(12) -0.0040(10) 0.0008(11) -0.0094(11) N6 0.0215(13) 0.0193(13) 0.0168(13) -0.0071(11) 0.0052(11) -0.0108(11) N7 0.0221(14) 0.0222(13) 0.0172(13) -0.0062(11) 0.0011(11) -0.0120(11) N8 0.0214(13) 0.0187(13) 0.0141(12) -0.0033(11) -0.0015(11) -0.0070(11) N9 0.0193(13) 0.0168(12) 0.0161(13) -0.0031(10) -0.0001(11) -0.0055(11) N10 0.0183(13) 0.0200(13) 0.0166(13) -0.0053(11) -0.0003(11) -0.0042(11) N11 0.0186(13) 0.0186(13) 0.0178(13) -0.0063(11) -0.0004(11) -0.0066(11) N12 0.0150(13) 0.0197(13) 0.0182(13) -0.0055(11) -0.0015(11) -0.0052(11) N13 0.0219(14) 0.0201(13) 0.0171(13) -0.0039(11) 0.0008(11) -0.0063(11) N14 0.0248(14) 0.0165(13) 0.0184(13) -0.0017(11) 0.0015(11) -0.0095(11) N15 0.0211(14) 0.0236(13) 0.0171(13) -0.0066(11) -0.0012(11) -0.0102(12) N16 0.0221(14) 0.0216(13) 0.0153(13) -0.0033(11) -0.0009(11) -0.0081(11) N17 0.0230(14) 0.0220(13) 0.0147(13) -0.0064(11) 0.0053(11) -0.0129(11) N18 0.0237(14) 0.0203(13) 0.0154(13) -0.0055(11) 0.0017(11) -0.0108(11) N19 0.0228(14) 0.0196(13) 0.0182(13) -0.0042(11) 0.0025(11) -0.0099(11) N20 0.0245(14) 0.0203(13) 0.0134(13) -0.0016(11) -0.0011(11) -0.0088(11) N21 0.0202(13) 0.0244(13) 0.0145(13) -0.0079(11) 0.0008(11) -0.0099(11) N22 0.0214(13) 0.0220(13) 0.0132(12) -0.0048(11) 0.0004(11) -0.0114(11) N23 0.0245(14) 0.0236(14) 0.0171(13) -0.0044(11) 0.0004(11) -0.0127(12) N24 0.0218(14) 0.0226(13) 0.0151(13) -0.0054(11) -0.0003(11) -0.0084(11) O1 0.0236(12) 0.0301(12) 0.0165(11) -0.0108(10) 0.0023(9) -0.0136(10) O2 0.0280(12) 0.0193(11) 0.0121(11) -0.0033(9) -0.0004(9) -0.0096(9) O3 0.0301(13) 0.0263(12) 0.0159(11) -0.0029(10) 0.0025(10) -0.0088(10) O4 0.0270(12) 0.0312(13) 0.0203(12) -0.0036(10) -0.0041(10) -0.0112(11) O5 0.0327(13) 0.0273(12) 0.0239(12) -0.0023(10) -0.0103(11) -0.0107(11) O6 0.0220(11) 0.0281(12) 0.0247(12) -0.0098(10) 0.0008(10) -0.0124(10) O7 0.0325(13) 0.0226(12) 0.0231(12) -0.0033(10) 0.0054(10) -0.0113(10) O8 0.0298(12) 0.0237(11) 0.0168(11) -0.0062(9) 0.0077(10) -0.0152(10) O9 0.0235(12) 0.0299(12) 0.0162(11) -0.0091(9) 0.0039(9) -0.0150(10) O10 0.0283(12) 0.0321(13) 0.0183(12) -0.0082(10) -0.0017(10) -0.0121(11) O11 0.0318(13) 0.0313(13) 0.0198(12) -0.0059(10) 0.0003(10) -0.0137(11) O12 0.0380(14) 0.0276(13) 0.0204(12) 0.0027(11) -0.0045(11) -0.0137(11) N25 0.0415(19) 0.045(2) 0.0377(19) -0.0182(16) 0.0087(16) -0.0211(17) N26 0.066(3) 0.041(2) 0.0351(19) -0.0077(16) 0.0071(19) -0.035(2) N27 0.0286(16) 0.0343(16) 0.0236(16) -0.0004(13) -0.0039(13) -0.0134(14) O13 0.105(3) 0.054(2) 0.063(2) -0.0250(18) 0.049(2) -0.045(2) O14 0.081(3) 0.062(2) 0.071(2) -0.035(2) 0.050(2) -0.023(2) O15 0.059(2) 0.0436(18) 0.0531(19) -0.0169(15) 0.0028(16) -0.0158(16) O16 0.064(2) 0.057(2) 0.0525(19) -0.0255(17) 0.0222(17) -0.0233(17) O17 0.104(3) 0.086(3) 0.044(2) -0.024(2) -0.008(2) -0.016(3) O18 0.063(2) 0.061(2) 0.061(2) -0.0163(18) 0.0008(19) -0.0225(19) O19 0.0546(19) 0.0578(19) 0.0442(17) -0.0239(16) -0.0088(15) -0.0192(16) O20 0.0506(18) 0.0475(17) 0.0331(15) -0.0008(13) 0.0119(14) -0.0187(15) O21 0.071(2) 0.064(2) 0.058(2) -0.0094(17) 0.0149(18) -0.0489(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1W Yb1 2.332(2) . ? O2W Yb1 2.344(2) . ? O3W Yb1 2.280(2) . ? O4W Yb1 2.271(2) . ? Yb1 O2 2.286(2) . ? Yb1 O9 2.319(2) . ? Yb1 O8 2.353(2) . ? Yb1 O1 2.379(2) . ? C1 O1 1.231(4) . ? C1 N2 1.356(4) . ? C1 N1 1.361(4) . ? C2 N3 1.452(4) . ? C2 N1 1.473(4) . ? C2 C19 1.522(4) . ? C2 C3 1.571(4) . ? C3 N4 1.449(4) . ? C3 N2 1.458(4) . ? C3 C22 1.526(4) . ? C4 O4 1.219(4) . ? C4 N3 1.366(4) . ? C4 N4 1.366(4) . ? C5 N5 1.443(4) . ? C5 N2 1.446(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.447(4) . ? C6 N7 1.449(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.233(4) . ? C7 N6 1.340(4) . ? C7 N5 1.360(4) . ? C8 N5 1.452(4) . ? C8 N7 1.459(4) . ? C8 C23 1.524(4) . ? C8 C9 1.568(4) . ? C9 N8 1.466(4) . ? C9 N6 1.475(4) . ? C9 C26 1.513(4) . ? C10 O5 1.221(4) . ? C10 N8 1.360(4) . ? C10 N7 1.369(4) . ? C11 N9 1.446(4) . ? C11 N6 1.447(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.450(4) . ? C12 N8 1.453(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.224(4) . ? C13 N10 1.364(4) . ? C13 N9 1.367(4) . ? C14 N9 1.461(4) . ? C14 N11 1.462(4) . ? C14 C27 1.521(4) . ? C14 C15 1.574(4) . ? C15 N10 1.450(4) . ? C15 N12 1.465(4) . ? C15 C30 1.518(4) . ? C16 O6 1.223(4) . ? C16 N12 1.358(4) . ? C16 N11 1.367(4) . ? C17 N10 1.446(4) . ? C17 N3 1.450(4) 2_665 ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.452(4) . ? C18 N12 1.457(4) 2_665 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.534(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.531(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.530(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.524(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.534(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.533(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.525(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.533(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.525(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O7 1.226(4) . ? C31 N14 1.366(4) . ? C31 N13 1.373(4) . ? C32 N13 1.462(4) . ? C32 N15 1.465(4) . ? C32 C49 1.509(4) . ? C32 C33 1.576(4) . ? C33 N16 1.456(4) . ? C33 N14 1.462(4) . ? C33 C52 1.524(4) . ? C34 O10 1.221(4) . ? C34 N15 1.363(4) . ? C34 N16 1.365(4) . ? C35 N14 1.440(4) . ? C35 N17 1.454(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N19 1.445(4) . ? C36 N16 1.453(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O8 1.235(4) . ? C37 N18 1.351(4) . ? C37 N17 1.352(4) . ? C38 N19 1.447(4) . ? C38 N17 1.468(4) . ? C38 C53 1.523(4) . ? C38 C39 1.572(4) . ? C39 N18 1.456(4) . ? C39 N20 1.468(4) . ? C39 C56 1.521(5) . ? C40 O11 1.217(4) . ? C40 N19 1.363(4) . ? C40 N20 1.368(4) . ? C41 N21 1.445(4) . ? C41 N18 1.446(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N20 1.438(4) . ? C42 N23 1.458(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 O9 1.236(4) . ? C43 N21 1.344(4) . ? C43 N22 1.361(4) . ? C44 N23 1.453(4) . ? C44 N21 1.461(4) . ? C44 C57 1.522(4) . ? C44 C45 1.573(4) . ? C45 N24 1.455(4) . ? C45 N22 1.460(4) . ? C45 C60 1.528(4) . ? C46 O12 1.226(4) . ? C46 N23 1.361(4) . ? C46 N24 1.365(4) . ? C47 N15 1.444(4) 2_756 ? C47 N22 1.455(4) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 N13 1.443(4) 2_756 ? C48 N24 1.458(4) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.523(5) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.529(5) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.529(5) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.528(5) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.533(5) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.538(5) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C58 1.526(5) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 C59 1.535(6) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 C60 1.521(6) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? N3 C17 1.450(4) 2_665 ? N12 C18 1.457(4) 2_665 ? N13 C48 1.443(4) 2_756 ? N15 C47 1.444(4) 2_756 ? N25 O14 1.224(5) . ? N25 O15 1.235(4) . ? N25 O13 1.247(5) . ? N26 O17 1.212(5) . ? N26 O18 1.243(5) . ? N26 O16 1.269(5) . ? N27 O19 1.232(4) . ? N27 O21 1.237(4) . ? N27 O20 1.240(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 O4W Yb1 O3W 139.67(8) . . ? O4W Yb1 O2 96.50(8) . . ? O3W Yb1 O2 95.34(8) . . ? O4W Yb1 O9 98.10(8) . . ? O3W Yb1 O9 98.54(8) . . ? O2 Yb1 O9 137.78(8) . . ? O4W Yb1 O1W 72.05(8) . . ? O3W Yb1 O1W 148.26(8) . . ? O2 Yb1 O1W 75.47(8) . . ? O9 Yb1 O1W 71.85(8) . . ? O4W Yb1 O2W 147.82(8) . . ? O3W Yb1 O2W 72.50(8) . . ? O2 Yb1 O2W 74.77(8) . . ? O9 Yb1 O2W 71.87(8) . . ? O1W Yb1 O2W 75.77(8) . . ? O4W Yb1 O8 75.80(8) . . ? O3W Yb1 O8 73.04(8) . . ? O2 Yb1 O8 146.17(7) . . ? O9 Yb1 O8 76.01(8) . . ? O1W Yb1 O8 129.97(8) . . ? O2W Yb1 O8 127.88(8) . . ? O4W Yb1 O1 72.04(8) . . ? O3W Yb1 O1 73.68(8) . . ? O2 Yb1 O1 76.18(8) . . ? O9 Yb1 O1 146.04(8) . . ? O1W Yb1 O1 130.65(8) . . ? O2W Yb1 O1 132.45(8) . . ? O8 Yb1 O1 70.09(7) . . ? O1 C1 N2 125.3(3) . . ? O1 C1 N1 124.9(3) . . ? N2 C1 N1 109.8(3) . . ? N3 C2 N1 112.1(2) . . ? N3 C2 C19 113.5(3) . . ? N1 C2 C19 112.6(3) . . ? N3 C2 C3 102.6(2) . . ? N1 C2 C3 102.7(2) . . ? C19 C2 C3 112.4(3) . . ? N4 C3 N2 113.1(2) . . ? N4 C3 C22 113.1(3) . . ? N2 C3 C22 112.0(3) . . ? N4 C3 C2 103.0(2) . . ? N2 C3 C2 102.7(2) . . ? C22 C3 C2 112.1(3) . . ? O4 C4 N3 126.0(3) . . ? O4 C4 N4 125.4(3) . . ? N3 C4 N4 108.5(3) . . ? N5 C5 N2 114.0(2) . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5B 108.8 . . ? N2 C5 H5B 108.8 . . ? H5A C5 H5B 107.6 . . ? N4 C6 N7 113.9(3) . . ? N4 C6 H6A 108.8 . . ? N7 C6 H6A 108.8 . . ? N4 C6 H6B 108.8 . . ? N7 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 125.3(3) . . ? O2 C7 N5 124.7(3) . . ? N6 C7 N5 110.0(3) . . ? N5 C8 N7 113.2(3) . . ? N5 C8 C23 112.2(3) . . ? N7 C8 C23 112.5(2) . . ? N5 C8 C9 103.1(2) . . ? N7 C8 C9 102.9(2) . . ? C23 C8 C9 112.2(3) . . ? N8 C9 N6 112.0(2) . . ? N8 C9 C26 113.2(3) . . ? N6 C9 C26 113.2(3) . . ? N8 C9 C8 102.8(2) . . ? N6 C9 C8 101.9(2) . . ? C26 C9 C8 112.6(3) . . ? O5 C10 N8 125.6(3) . . ? O5 C10 N7 125.2(3) . . ? N8 C10 N7 109.1(3) . . ? N9 C11 N6 114.3(2) . . ? N9 C11 H11A 108.7 . . ? N6 C11 H11A 108.7 . . ? N9 C11 H11B 108.7 . . ? N6 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N11 C12 N8 115.3(3) . . ? N11 C12 H12A 108.5 . . ? N8 C12 H12A 108.5 . . ? N11 C12 H12B 108.5 . . ? N8 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? O3 C13 N10 124.9(3) . . ? O3 C13 N9 126.1(3) . . ? N10 C13 N9 108.9(3) . . ? N9 C14 N11 111.7(2) . . ? N9 C14 C27 113.5(3) . . ? N11 C14 C27 113.6(3) . . ? N9 C14 C15 102.7(2) . . ? N11 C14 C15 102.9(2) . . ? C27 C14 C15 111.4(2) . . ? N10 C15 N12 112.0(2) . . ? N10 C15 C30 112.9(2) . . ? N12 C15 C30 113.2(3) . . ? N10 C15 C14 102.8(2) . . ? N12 C15 C14 102.2(2) . . ? C30 C15 C14 112.8(3) . . ? O6 C16 N12 125.8(3) . . ? O6 C16 N11 125.4(3) . . ? N12 C16 N11 108.8(3) . . ? N10 C17 N3 113.7(2) . 2_665 ? N10 C17 H17A 108.8 . . ? N3 C17 H17A 108.8 2_665 . ? N10 C17 H17B 108.8 . . ? N3 C17 H17B 108.8 2_665 . ? H17A C17 H17B 107.7 . . ? N1 C18 N12 114.5(2) . 2_665 ? N1 C18 H18A 108.6 . . ? N12 C18 H18A 108.6 2_665 . ? N1 C18 H18B 108.6 . . ? N12 C18 H18B 108.6 2_665 . ? H18A C18 H18B 107.6 . . ? C2 C19 C20 109.9(3) . . ? C2 C19 H19A 109.7 . . ? C20 C19 H19A 109.7 . . ? C2 C19 H19B 109.7 . . ? C20 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? C21 C20 C19 112.1(3) . . ? C21 C20 H20A 109.2 . . ? C19 C20 H20A 109.2 . . ? C21 C20 H20B 109.2 . . ? C19 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C22 C21 C20 113.5(3) . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21B 108.9 . . ? C20 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C3 C22 C21 111.1(3) . . ? C3 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C3 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C8 109.6(3) . . ? C24 C23 H23A 109.8 . . ? C8 C23 H23A 109.8 . . ? C24 C23 H23B 109.8 . . ? C8 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? C23 C24 C25 112.3(3) . . ? C23 C24 H24A 109.1 . . ? C25 C24 H24A 109.1 . . ? C23 C24 H24B 109.1 . . ? C25 C24 H24B 109.1 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C24 112.8(3) . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25B 109.0 . . ? C24 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C9 C26 C25 112.6(3) . . ? C9 C26 H26A 109.1 . . ? C25 C26 H26A 109.1 . . ? C9 C26 H26B 109.1 . . ? C25 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? C14 C27 C28 112.9(3) . . ? C14 C27 H27A 109.0 . . ? C28 C27 H27A 109.0 . . ? C14 C27 H27B 109.0 . . ? C28 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C28 C29 113.0(3) . . ? C27 C28 H28A 109.0 . . ? C29 C28 H28A 109.0 . . ? C27 C28 H28B 109.0 . . ? C29 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C30 C29 C28 112.2(3) . . ? C30 C29 H29A 109.2 . . ? C28 C29 H29A 109.2 . . ? C30 C29 H29B 109.2 . . ? C28 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C15 C30 C29 110.8(3) . . ? C15 C30 H30A 109.5 . . ? C29 C30 H30A 109.5 . . ? C15 C30 H30B 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? O7 C31 N14 126.0(3) . . ? O7 C31 N13 125.2(3) . . ? N14 C31 N13 108.7(3) . . ? N13 C32 N15 111.6(2) . . ? N13 C32 C49 113.2(3) . . ? N15 C32 C49 113.7(3) . . ? N13 C32 C33 102.8(2) . . ? N15 C32 C33 102.5(2) . . ? C49 C32 C33 112.1(3) . . ? N16 C33 N14 112.5(2) . . ? N16 C33 C52 112.7(3) . . ? N14 C33 C52 113.1(3) . . ? N16 C33 C32 103.0(2) . . ? N14 C33 C32 102.9(2) . . ? C52 C33 C32 111.8(3) . . ? O10 C34 N15 125.9(3) . . ? O10 C34 N16 125.0(3) . . ? N15 C34 N16 109.1(3) . . ? N14 C35 N17 114.9(2) . . ? N14 C35 H35A 108.6 . . ? N17 C35 H35A 108.6 . . ? N14 C35 H35B 108.6 . . ? N17 C35 H35B 108.6 . . ? H35A C35 H35B 107.5 . . ? N19 C36 N16 114.6(3) . . ? N19 C36 H36A 108.6 . . ? N16 C36 H36A 108.6 . . ? N19 C36 H36B 108.6 . . ? N16 C36 H36B 108.6 . . ? H36A C36 H36B 107.6 . . ? O8 C37 N18 125.5(3) . . ? O8 C37 N17 124.5(3) . . ? N18 C37 N17 109.9(3) . . ? N19 C38 N17 112.8(3) . . ? N19 C38 C53 113.5(3) . . ? N17 C38 C53 112.6(3) . . ? N19 C38 C39 102.9(2) . . ? N17 C38 C39 102.7(2) . . ? C53 C38 C39 111.3(3) . . ? N18 C39 N20 113.3(3) . . ? N18 C39 C56 112.6(3) . . ? N20 C39 C56 112.4(3) . . ? N18 C39 C38 102.5(2) . . ? N20 C39 C38 102.5(2) . . ? C56 C39 C38 112.8(3) . . ? O11 C40 N19 125.9(3) . . ? O11 C40 N20 125.7(3) . . ? N19 C40 N20 108.4(3) . . ? N21 C41 N18 113.5(2) . . ? N21 C41 H41A 108.9 . . ? N18 C41 H41A 108.9 . . ? N21 C41 H41B 108.9 . . ? N18 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? N20 C42 N23 114.0(3) . . ? N20 C42 H42A 108.8 . . ? N23 C42 H42A 108.8 . . ? N20 C42 H42B 108.8 . . ? N23 C42 H42B 108.8 . . ? H42A C42 H42B 107.6 . . ? O9 C43 N21 125.8(3) . . ? O9 C43 N22 124.4(3) . . ? N21 C43 N22 109.8(3) . . ? N23 C44 N21 112.9(2) . . ? N23 C44 C57 112.9(3) . . ? N21 C44 C57 112.3(3) . . ? N23 C44 C45 102.7(2) . . ? N21 C44 C45 102.0(2) . . ? C57 C44 C45 113.0(3) . . ? N24 C45 N22 112.1(2) . . ? N24 C45 C60 113.3(3) . . ? N22 C45 C60 113.2(3) . . ? N24 C45 C44 102.7(2) . . ? N22 C45 C44 103.1(2) . . ? C60 C45 C44 111.4(3) . . ? O12 C46 N23 125.8(3) . . ? O12 C46 N24 125.5(3) . . ? N23 C46 N24 108.7(3) . . ? N15 C47 N22 114.9(3) 2_756 . ? N15 C47 H47A 108.6 2_756 . ? N22 C47 H47A 108.6 . . ? N15 C47 H47B 108.6 2_756 . ? N22 C47 H47B 108.6 . . ? H47A C47 H47B 107.5 . . ? N13 C48 N24 115.4(2) 2_756 . ? N13 C48 H48A 108.4 2_756 . ? N24 C48 H48A 108.4 . . ? N13 C48 H48B 108.4 2_756 . ? N24 C48 H48B 108.4 . . ? H48A C48 H48B 107.5 . . ? C32 C49 C50 111.6(3) . . ? C32 C49 H49A 109.3 . . ? C50 C49 H49A 109.3 . . ? C32 C49 H49B 109.3 . . ? C50 C49 H49B 109.3 . . ? H49A C49 H49B 108.0 . . ? C49 C50 C51 113.1(3) . . ? C49 C50 H50A 109.0 . . ? C51 C50 H50A 109.0 . . ? C49 C50 H50B 109.0 . . ? C51 C50 H50B 109.0 . . ? H50A C50 H50B 107.8 . . ? C52 C51 C50 112.4(3) . . ? C52 C51 H51A 109.1 . . ? C50 C51 H51A 109.1 . . ? C52 C51 H51B 109.1 . . ? C50 C51 H51B 109.1 . . ? H51A C51 H51B 107.9 . . ? C33 C52 C51 110.8(3) . . ? C33 C52 H52A 109.5 . . ? C51 C52 H52A 109.5 . . ? C33 C52 H52B 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 108.1 . . ? C38 C53 C54 110.3(3) . . ? C38 C53 H53A 109.6 . . ? C54 C53 H53A 109.6 . . ? C38 C53 H53B 109.6 . . ? C54 C53 H53B 109.6 . . ? H53A C53 H53B 108.1 . . ? C53 C54 C55 112.5(3) . . ? C53 C54 H54A 109.1 . . ? C55 C54 H54A 109.1 . . ? C53 C54 H54B 109.1 . . ? C55 C54 H54B 109.1 . . ? H54A C54 H54B 107.8 . . ? C54 C55 C56 112.5(3) . . ? C54 C55 H55A 109.1 . . ? C56 C55 H55A 109.1 . . ? C54 C55 H55B 109.1 . . ? C56 C55 H55B 109.1 . . ? H55A C55 H55B 107.8 . . ? C39 C56 C55 111.2(3) . . ? C39 C56 H56A 109.4 . . ? C55 C56 H56A 109.4 . . ? C39 C56 H56B 109.4 . . ? C55 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? C44 C57 C58 109.5(3) . . ? C44 C57 H57A 109.8 . . ? C58 C57 H57A 109.8 . . ? C44 C57 H57B 109.8 . . ? C58 C57 H57B 109.8 . . ? H57A C57 H57B 108.2 . . ? C57 C58 C59 111.9(3) . . ? C57 C58 H58A 109.2 . . ? C59 C58 H58A 109.2 . . ? C57 C58 H58B 109.2 . . ? C59 C58 H58B 109.2 . . ? H58A C58 H58B 107.9 . . ? C60 C59 C58 113.9(3) . . ? C60 C59 H59A 108.8 . . ? C58 C59 H59A 108.8 . . ? C60 C59 H59B 108.8 . . ? C58 C59 H59B 108.8 . . ? H59A C59 H59B 107.7 . . ? C59 C60 C45 110.9(3) . . ? C59 C60 H60A 109.5 . . ? C45 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? C45 C60 H60B 109.5 . . ? H60A C60 H60B 108.0 . . ? C1 N1 C18 121.2(2) . . ? C1 N1 C2 111.7(2) . . ? C18 N1 C2 124.9(2) . . ? C1 N2 C5 122.1(2) . . ? C1 N2 C3 112.6(2) . . ? C5 N2 C3 125.3(2) . . ? C4 N3 C17 121.4(3) . 2_665 ? C4 N3 C2 112.9(3) . . ? C17 N3 C2 125.4(3) 2_665 . ? C4 N4 C6 120.8(3) . . ? C4 N4 C3 112.5(3) . . ? C6 N4 C3 125.8(3) . . ? C7 N5 C5 122.7(3) . . ? C7 N5 C8 112.0(2) . . ? C5 N5 C8 125.3(2) . . ? C7 N6 C11 121.6(3) . . ? C7 N6 C9 112.3(2) . . ? C11 N6 C9 123.9(2) . . ? C10 N7 C6 121.7(3) . . ? C10 N7 C8 112.4(2) . . ? C6 N7 C8 124.9(3) . . ? C10 N8 C12 121.8(3) . . ? C10 N8 C9 112.4(2) . . ? C12 N8 C9 125.6(2) . . ? C13 N9 C11 120.4(3) . . ? C13 N9 C14 112.2(2) . . ? C11 N9 C14 124.2(3) . . ? C13 N10 C17 121.7(3) . . ? C13 N10 C15 112.9(2) . . ? C17 N10 C15 124.9(3) . . ? C16 N11 C12 122.2(3) . . ? C16 N11 C14 112.6(2) . . ? C12 N11 C14 124.9(3) . . ? C16 N12 C18 120.4(2) . 2_665 ? C16 N12 C15 113.1(2) . . ? C18 N12 C15 125.0(2) 2_665 . ? C31 N13 C48 121.1(3) . 2_756 ? C31 N13 C32 112.7(3) . . ? C48 N13 C32 125.2(3) 2_756 . ? C31 N14 C35 121.0(3) . . ? C31 N14 C33 112.7(3) . . ? C35 N14 C33 125.2(3) . . ? C34 N15 C47 121.3(3) . 2_756 ? C34 N15 C32 112.6(3) . . ? C47 N15 C32 124.1(3) 2_756 . ? C34 N16 C36 121.6(3) . . ? C34 N16 C33 112.7(3) . . ? C36 N16 C33 124.8(3) . . ? C37 N17 C35 121.0(3) . . ? C37 N17 C38 111.9(2) . . ? C35 N17 C38 125.0(2) . . ? C37 N18 C41 121.8(3) . . ? C37 N18 C39 112.7(2) . . ? C41 N18 C39 125.5(2) . . ? C40 N19 C36 120.6(3) . . ? C40 N19 C38 113.4(3) . . ? C36 N19 C38 125.8(3) . . ? C40 N20 C42 121.2(3) . . ? C40 N20 C39 112.2(2) . . ? C42 N20 C39 125.5(3) . . ? C43 N21 C41 122.8(3) . . ? C43 N21 C44 113.0(2) . . ? C41 N21 C44 124.2(3) . . ? C43 N22 C47 121.7(3) . . ? C43 N22 C45 111.8(3) . . ? C47 N22 C45 124.8(2) . . ? C46 N23 C44 112.9(3) . . ? C46 N23 C42 121.3(3) . . ? C44 N23 C42 125.2(3) . . ? C46 N24 C45 112.8(3) . . ? C46 N24 C48 121.0(3) . . ? C45 N24 C48 125.9(3) . . ? C1 O1 Yb1 156.3(2) . . ? C7 O2 Yb1 159.2(2) . . ? C37 O8 Yb1 155.2(2) . . ? C43 O9 Yb1 155.0(2) . . ? O14 N25 O15 121.0(4) . . ? O14 N25 O13 120.2(4) . . ? O15 N25 O13 118.8(4) . . ? O17 N26 O18 119.2(4) . . ? O17 N26 O16 120.1(4) . . ? O18 N26 O16 120.6(4) . . ? O19 N27 O21 120.7(3) . . ? O19 N27 O20 119.9(3) . . ? O21 N27 O20 119.4(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.086 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.090 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 113 27 ' ' 2 -0.031 0.015 0.842 19 10 ' ' 3 0.031 0.985 0.158 18 9 ' ' 4 0.275 0.373 0.778 201 71 ' ' 5 0.347 0.956 0.152 57 20 ' ' 6 0.500 0.500 0.000 106 24 ' ' 7 0.725 0.626 0.222 201 71 ' ' 8 0.654 0.043 0.848 56 19 ' ' _platon_squeeze_details ; ; data_a4 _database_code_depnum_ccdc_archive 'CCDC 881901' #TrackingRef '110321qx-submit-cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H124 Cl2 N25 O41 Pr' _chemical_formula_weight 2063.65 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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7042(6) _cell_length_b 14.7774(8) _cell_length_c 29.5216(16) _cell_angle_alpha 77.486(2) _cell_angle_beta 81.423(2) _cell_angle_gamma 69.116(2) _cell_volume 4246.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8590 _exptl_absorpt_correction_T_max 0.9027 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45518 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0730 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 0.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14804 _reflns_number_gt 11417 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1522P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14804 _refine_ls_number_parameters 1027 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.2293 _refine_ls_wR_factor_gt 0.2161 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 N25 N 0.7040(8) 0.3215(6) 0.2508(3) 0.0354(19) Uani 0.50 1 d P . . N25A N 0.7752(8) 0.1767(6) 0.2508(3) 0.0342(18) Uani 0.50 1 d P . . O1W O 1.1070(5) 0.4313(3) 0.2989(2) 0.0888(17) Uani 1 1 d . . . O2W O 1.3031(5) 0.0326(4) 0.3033(3) 0.126(3) Uani 1 1 d . . . O3W O 1.1417(5) -0.5354(4) 0.2010(2) 0.0968(19) Uani 1 1 d . . . O4W O 1.3304(6) 0.0691(4) 0.2084(3) 0.113(2) Uani 1 1 d . . . O5W O 0.9351(7) 0.3008(4) 0.2543(2) 0.0378(15) Uani 0.50 1 d P . . O6W O 0.9879(7) 0.1960(5) 0.2547(3) 0.0411(16) Uani 0.50 1 d P . . O13 O 0.7669(6) 0.3818(5) 0.2495(3) 0.0406(16) Uani 0.50 1 d P . . O13A O 0.8946(7) 0.1208(5) 0.2498(3) 0.0467(18) Uani 0.50 1 d P . . O14 O 0.6842(11) 0.3074(9) 0.2127(3) 0.070(3) Uani 0.50 1 d P . . O14A O 0.7074(9) 0.1876(10) 0.2868(3) 0.079(3) Uani 0.50 1 d P . . O15 O 0.6647(11) 0.2821(9) 0.2863(3) 0.072(3) Uani 0.50 1 d P . . O15A O 0.7241(10) 0.2266(9) 0.2142(3) 0.074(3) Uani 0.50 1 d P . . Pr1 Pr 1.00829(4) 0.36018(3) 0.253895(16) 0.02214(16) Uani 0.50 1 d P . . Pr2 Pr 1.11788(5) 0.13952(3) 0.252885(18) 0.02748(17) Uani 0.50 1 d P . . Cl1 Cl 1.2064(3) 0.2671(2) 0.20456(12) 0.1320(10) Uani 1 1 d . . . Cl2 Cl 1.1839(4) 0.2325(2) 0.30178(12) 0.1362(10) Uani 1 1 d . . . C1 C 0.7359(4) 0.5705(3) 0.25006(15) 0.0259(9) Uani 1 1 d . . . C2 C 0.5235(4) 0.6418(3) 0.22104(16) 0.0286(10) Uani 1 1 d . . . C3 C 0.5067(4) 0.6215(3) 0.27520(15) 0.0278(9) Uani 1 1 d . . . C4 C 0.4110(4) 0.5281(3) 0.24612(17) 0.0326(10) Uani 1 1 d . . . C5 C 0.6883(5) 0.5442(3) 0.33439(15) 0.0296(10) Uani 1 1 d . . . H5A H 0.6346 0.5930 0.3537 0.036 Uiso 1 1 calc R . . H5B H 0.7819 0.5406 0.3332 0.036 Uiso 1 1 calc R . . C6 C 0.3744(5) 0.5199(4) 0.33008(17) 0.0370(11) Uani 1 1 d . . . H6A H 0.2942 0.5068 0.3253 0.044 Uiso 1 1 calc R . . H6B H 0.3455 0.5742 0.3475 0.044 Uiso 1 1 calc R . . C7 C 0.7851(4) 0.3636(3) 0.35681(15) 0.0283(9) Uani 1 1 d . . . C8 C 0.5617(4) 0.4345(3) 0.38579(15) 0.0293(10) Uani 1 1 d . . . C9 C 0.6183(5) 0.3250(3) 0.41017(15) 0.0332(10) Uani 1 1 d . . . C10 C 0.4391(5) 0.3458(4) 0.36673(17) 0.0366(11) Uani 1 1 d . . . C11 C 0.8509(5) 0.1963(3) 0.40043(16) 0.0323(10) Uani 1 1 d . . . H11A H 0.8504 0.1843 0.4344 0.039 Uiso 1 1 calc R . . H11B H 0.9388 0.2006 0.3875 0.039 Uiso 1 1 calc R . . C12 C 0.5147(5) 0.1876(3) 0.42112(17) 0.0382(11) Uani 1 1 d . . . H12A H 0.4239 0.1887 0.4185 0.046 Uiso 1 1 calc R . . H12B H 0.5267 0.1778 0.4543 0.046 Uiso 1 1 calc R . . C13 C 0.9330(5) 0.0591(3) 0.35794(16) 0.0317(10) Uani 1 1 d . . . C14 C 0.7499(5) 0.0574(3) 0.41260(16) 0.0360(11) Uani 1 1 d . . . C15 C 0.7942(5) -0.0367(3) 0.38853(16) 0.0365(11) Uani 1 1 d . . . C16 C 0.5766(5) 0.0640(4) 0.37065(19) 0.0418(12) Uani 1 1 d . . . C17 C 1.0096(5) -0.1067(3) 0.33787(16) 0.0371(11) Uani 1 1 d . . . H17A H 1.0128 -0.1705 0.3569 0.045 Uiso 1 1 calc R . . H17B H 1.0987 -0.1011 0.3364 0.045 Uiso 1 1 calc R . . C18 C 0.6718(6) -0.0834(4) 0.33414(18) 0.0414(12) Uani 1 1 d . . . H18A H 0.7049 -0.1505 0.3518 0.050 Uiso 1 1 calc R . . H18B H 0.5769 -0.0684 0.3300 0.050 Uiso 1 1 calc R . . C19 C 1.0496(4) -0.0701(3) 0.25345(15) 0.0260(9) Uani 1 1 d . . . C20 C 0.8817(5) -0.1408(3) 0.27821(16) 0.0306(10) Uani 1 1 d . . . C21 C 0.8970(4) -0.1193(3) 0.22418(16) 0.0285(10) Uani 1 1 d . . . C22 C 0.6811(5) -0.0268(3) 0.25012(17) 0.0324(10) Uani 1 1 d . . . C23 C 1.0599(5) -0.0444(3) 0.16848(16) 0.0322(10) Uani 1 1 d . . . H23A H 1.1489 -0.0424 0.1712 0.039 Uiso 1 1 calc R . . H23B H 1.0714 -0.0933 0.1490 0.039 Uiso 1 1 calc R . . C24 C 0.7196(5) -0.0169(3) 0.16537(17) 0.0351(11) Uani 1 1 d . . . H24A H 0.7606 -0.0714 0.1481 0.042 Uiso 1 1 calc R . . H24B H 0.6222 -0.0022 0.1680 0.042 Uiso 1 1 calc R . . C25 C 1.0011(5) 0.1352(3) 0.14679(15) 0.0289(10) Uani 1 1 d . . . C26 C 0.8778(5) 0.0662(3) 0.11426(15) 0.0312(10) Uani 1 1 d . . . C27 C 0.8519(5) 0.1752(3) 0.08977(15) 0.0298(10) Uani 1 1 d . . . C28 C 0.6509(5) 0.1569(3) 0.12789(17) 0.0346(11) Uani 1 1 d . . . C29 C 0.9447(5) 0.3043(3) 0.10346(16) 0.0312(10) Uani 1 1 d . . . H29A H 1.0234 0.3001 0.1181 0.037 Uiso 1 1 calc R . . H29B H 0.9653 0.3166 0.0697 0.037 Uiso 1 1 calc R . . C30 C 0.6258(5) 0.3137(3) 0.07464(16) 0.0340(11) Uani 1 1 d . . . H30A H 0.5344 0.3131 0.0750 0.041 Uiso 1 1 calc R . . H30B H 0.6611 0.3233 0.0420 0.041 Uiso 1 1 calc R . . C31 C 0.8483(5) 0.4413(3) 0.14586(15) 0.0309(10) Uani 1 1 d . . . C32 C 0.7208(5) 0.4435(3) 0.08745(15) 0.0306(10) Uani 1 1 d . . . C33 C 0.6487(5) 0.5377(3) 0.11078(16) 0.0328(10) Uani 1 1 d . . . C34 C 0.5136(5) 0.4377(3) 0.12428(16) 0.0337(10) Uani 1 1 d . . . C35 C 0.7424(5) 0.6071(3) 0.16543(15) 0.0315(10) Uani 1 1 d . . . H35A H 0.8348 0.6015 0.1687 0.038 Uiso 1 1 calc R . . H35B H 0.7007 0.6708 0.1459 0.038 Uiso 1 1 calc R . . C36 C 0.4278(5) 0.5828(3) 0.16224(17) 0.0364(11) Uani 1 1 d . . . H36A H 0.4100 0.6502 0.1450 0.044 Uiso 1 1 calc R . . H36B H 0.3450 0.5673 0.1648 0.044 Uiso 1 1 calc R . . C37 C 0.4623(5) 0.7490(3) 0.20041(18) 0.0391(11) Uani 1 1 d . . . H37A H 0.3643 0.7682 0.2049 0.047 Uiso 1 1 calc R . . H37B H 0.4875 0.7588 0.1669 0.047 Uiso 1 1 calc R . . C38 C 0.5083(6) 0.8139(4) 0.2227(2) 0.0481(14) Uani 1 1 d . . . H38A H 0.4571 0.8829 0.2113 0.058 Uiso 1 1 calc R . . H38B H 0.6030 0.8039 0.2125 0.058 Uiso 1 1 calc R . . C39 C 0.4925(6) 0.7952(4) 0.2758(2) 0.0475(14) Uani 1 1 d . . . H39A H 0.4352 0.8562 0.2866 0.057 Uiso 1 1 calc R . . H39B H 0.5806 0.7759 0.2879 0.057 Uiso 1 1 calc R . . C40 C 0.4309(5) 0.7143(3) 0.29505(19) 0.0417(12) Uani 1 1 d . . . H40A H 0.4317 0.6991 0.3290 0.050 Uiso 1 1 calc R . . H40B H 0.3373 0.7382 0.2874 0.050 Uiso 1 1 calc R . . C41 C 0.5053(6) 0.5051(4) 0.42020(16) 0.0413(12) Uani 1 1 d . . . H41A H 0.4553 0.5708 0.4041 0.050 Uiso 1 1 calc R . . H41B H 0.5785 0.5102 0.4348 0.050 Uiso 1 1 calc R . . C42 C 0.4109(7) 0.4648(5) 0.4579(2) 0.0677(18) Uani 1 1 d . . . H42A H 0.3700 0.5115 0.4793 0.081 Uiso 1 1 calc R . . H42B H 0.3386 0.4601 0.4427 0.081 Uiso 1 1 calc R . . C43 C 0.4836(8) 0.3638(5) 0.4857(2) 0.0681(19) Uani 1 1 d . . . H43A H 0.4927 0.3710 0.5172 0.082 Uiso 1 1 calc R . . H43B H 0.4301 0.3209 0.4884 0.082 Uiso 1 1 calc R . . C44 C 0.6215(5) 0.3166(4) 0.46268(16) 0.0406(12) Uani 1 1 d . . . H44A H 0.6562 0.2470 0.4769 0.049 Uiso 1 1 calc R . . H44B H 0.6826 0.3485 0.4681 0.049 Uiso 1 1 calc R . . C45 C 0.7682(7) 0.0288(4) 0.46418(17) 0.0522(14) Uani 1 1 d . . . H45A H 0.7405 0.0881 0.4782 0.063 Uiso 1 1 calc R . . H45B H 0.8630 -0.0075 0.4691 0.063 Uiso 1 1 calc R . . C46 C 0.6808(13) -0.0376(6) 0.4879(3) 0.108(4) Uani 1 1 d . . . H46A H 0.7101 -0.0698 0.5191 0.129 Uiso 1 1 calc R . . H46B H 0.5868 0.0044 0.4915 0.129 Uiso 1 1 calc R . . C47 C 0.6910(11) -0.1172(6) 0.4596(2) 0.094(3) Uani 1 1 d . . . H47A H 0.6103 -0.0970 0.4429 0.112 Uiso 1 1 calc R . . H47B H 0.6977 -0.1795 0.4808 0.112 Uiso 1 1 calc R . . C48 C 0.8168(8) -0.1312(4) 0.4245(2) 0.0648(19) Uani 1 1 d . . . H48A H 0.8967 -0.1447 0.4408 0.078 Uiso 1 1 calc R . . H48B H 0.8304 -0.1869 0.4092 0.078 Uiso 1 1 calc R . . C49 C 0.9088(6) -0.2488(3) 0.29773(18) 0.0405(12) Uani 1 1 d . . . H49A H 0.8369 -0.2685 0.2905 0.049 Uiso 1 1 calc R . . H49B H 0.9086 -0.2593 0.3317 0.049 Uiso 1 1 calc R . . C50 C 1.0433(6) -0.3128(4) 0.2779(2) 0.0509(14) Uani 1 1 d . . . H50A H 1.0531 -0.3823 0.2892 0.061 Uiso 1 1 calc R . . H50B H 1.1159 -0.3000 0.2892 0.061 Uiso 1 1 calc R . . C51 C 1.0564(6) -0.2932(4) 0.2241(2) 0.0497(14) Uani 1 1 d . . . H51A H 1.1364 -0.2746 0.2131 0.060 Uiso 1 1 calc R . . H51B H 1.0686 -0.3540 0.2131 0.060 Uiso 1 1 calc R . . C52 C 0.9346(5) -0.2122(3) 0.20339(18) 0.0384(11) Uani 1 1 d . . . H52A H 0.8583 -0.2362 0.2089 0.046 Uiso 1 1 calc R . . H52B H 0.9535 -0.1963 0.1697 0.046 Uiso 1 1 calc R . . C53 C 0.9261(6) -0.0051(4) 0.07965(17) 0.0423(12) Uani 1 1 d . . . H53A H 0.9261 -0.0708 0.0954 0.051 Uiso 1 1 calc R . . H53B H 1.0176 -0.0101 0.0668 0.051 Uiso 1 1 calc R . . C54 C 0.8300(9) 0.0343(5) 0.0402(3) 0.084(2) Uani 1 1 d . . . H54A H 0.8554 -0.0131 0.0190 0.101 Uiso 1 1 calc R . . H54B H 0.7384 0.0411 0.0536 0.101 Uiso 1 1 calc R . . C55 C 0.8333(9) 0.1339(5) 0.0127(2) 0.080(2) Uani 1 1 d . . . H55A H 0.7413 0.1776 0.0074 0.096 Uiso 1 1 calc R . . H55B H 0.8821 0.1247 -0.0177 0.096 Uiso 1 1 calc R . . C56 C 0.9006(6) 0.1827(4) 0.03803(16) 0.0392(11) Uani 1 1 d . . . H56A H 0.9981 0.1506 0.0348 0.047 Uiso 1 1 calc R . . H56B H 0.8801 0.2521 0.0236 0.047 Uiso 1 1 calc R . . C57 C 0.7658(6) 0.4709(4) 0.03663(17) 0.0424(12) Uani 1 1 d . . . H57A H 0.8053 0.4111 0.0229 0.051 Uiso 1 1 calc R . . H57B H 0.8351 0.5010 0.0345 0.051 Uiso 1 1 calc R . . C58 C 0.6469(7) 0.5438(4) 0.00865(19) 0.0584(16) Uani 1 1 d . . . H58A H 0.6826 0.5768 -0.0201 0.070 Uiso 1 1 calc R . . H58B H 0.5975 0.5065 -0.0001 0.070 Uiso 1 1 calc R . . C59 C 0.5508(7) 0.6208(4) 0.03527(19) 0.0584(16) Uani 1 1 d . . . H59A H 0.4714 0.6022 0.0475 0.070 Uiso 1 1 calc R . . H59B H 0.5214 0.6840 0.0141 0.070 Uiso 1 1 calc R . . C60 C 0.6156(6) 0.6323(3) 0.07586(17) 0.0433(12) Uani 1 1 d . . . H60A H 0.6976 0.6478 0.0641 0.052 Uiso 1 1 calc R . . H60B H 0.5537 0.6865 0.0908 0.052 Uiso 1 1 calc R . . N1 N 0.6703(4) 0.6055(3) 0.21100(13) 0.0300(8) Uani 1 1 d . . . N2 N 0.6448(4) 0.5779(3) 0.28814(12) 0.0267(8) Uani 1 1 d . . . N3 N 0.4606(4) 0.5790(3) 0.20785(13) 0.0315(9) Uani 1 1 d . . . N4 N 0.4364(4) 0.5497(3) 0.28558(13) 0.0318(8) Uani 1 1 d . . . N5 N 0.6783(4) 0.4500(3) 0.35638(12) 0.0276(8) Uani 1 1 d . . . N6 N 0.7500(4) 0.2894(3) 0.38597(13) 0.0310(8) Uani 1 1 d . . . N7 N 0.4614(4) 0.4329(3) 0.35778(14) 0.0340(9) Uani 1 1 d . . . N8 N 0.5254(4) 0.2824(3) 0.39878(14) 0.0365(9) Uani 1 1 d . . . N9 N 0.8352(4) 0.1123(3) 0.38673(13) 0.0330(9) Uani 1 1 d . . . N10 N 0.9140(4) -0.0300(3) 0.36029(13) 0.0358(9) Uani 1 1 d . . . N11 N 0.6108(4) 0.1044(3) 0.40199(14) 0.0384(10) Uani 1 1 d . . . N12 N 0.6828(4) -0.0158(3) 0.36091(14) 0.0375(9) Uani 1 1 d . . . N13 N 0.9800(4) -0.1045(3) 0.29095(13) 0.0311(8) Uani 1 1 d . . . N14 N 1.0047(4) -0.0765(3) 0.21416(13) 0.0282(8) Uani 1 1 d . . . N15 N 0.7450(4) -0.0799(3) 0.28897(13) 0.0328(9) Uani 1 1 d . . . N16 N 0.7668(4) -0.0477(3) 0.21165(13) 0.0299(8) Uani 1 1 d . . . N17 N 0.9800(4) 0.0504(3) 0.14530(13) 0.0306(8) Uani 1 1 d . . . N18 N 0.9238(4) 0.2102(3) 0.11654(13) 0.0309(8) Uani 1 1 d . . . N19 N 0.7500(4) 0.0689(3) 0.13925(14) 0.0331(9) Uani 1 1 d . . . N20 N 0.7062(4) 0.2194(3) 0.09756(13) 0.0308(8) Uani 1 1 d . . . N21 N 0.8335(4) 0.3871(3) 0.11586(12) 0.0291(8) Uani 1 1 d . . . N22 N 0.7458(4) 0.5294(3) 0.14187(13) 0.0308(8) Uani 1 1 d . . . N23 N 0.6186(4) 0.3977(3) 0.09433(13) 0.0324(9) Uani 1 1 d . . . N24 N 0.5308(4) 0.5164(3) 0.13578(13) 0.0314(8) Uani 1 1 d . . . O1 O 0.8589(3) 0.5400(2) 0.25182(11) 0.0356(8) Uani 1 1 d . . . O2 O 0.8929(3) 0.3555(2) 0.33507(11) 0.0369(8) Uani 1 1 d . . . O3 O 1.0242(3) 0.0839(3) 0.33553(12) 0.0432(8) Uani 1 1 d . . . O4 O 1.1436(3) -0.0406(2) 0.25458(12) 0.0387(8) Uani 1 1 d . . . O5 O 1.0797(3) 0.1440(2) 0.17055(11) 0.0369(8) Uani 1 1 d . . . O6 O 0.9418(3) 0.4150(2) 0.17075(11) 0.0366(8) Uani 1 1 d . . . O7 O 0.3488(3) 0.4727(2) 0.24504(13) 0.0403(8) Uani 1 1 d . . . O8 O 0.3559(4) 0.3266(3) 0.35031(15) 0.0555(10) Uani 1 1 d . . . O9 O 0.4673(4) 0.0926(3) 0.35412(16) 0.0600(11) Uani 1 1 d . . . O10 O 0.5652(3) 0.0282(2) 0.24951(13) 0.0430(9) Uani 1 1 d . . . O11 O 0.5327(4) 0.1763(3) 0.14106(14) 0.0505(9) Uani 1 1 d . . . O12 O 0.4189(4) 0.4087(3) 0.13821(14) 0.0522(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N25 0.035(5) 0.034(4) 0.047(5) -0.015(4) -0.011(4) -0.016(4) N25A 0.022(4) 0.036(4) 0.047(5) -0.010(4) -0.011(4) -0.007(4) O1W 0.049(3) 0.044(3) 0.180(6) -0.028(3) -0.007(3) -0.020(2) O2W 0.052(3) 0.074(4) 0.270(9) -0.089(5) 0.000(4) -0.013(3) O3W 0.056(3) 0.068(3) 0.182(6) -0.048(4) -0.015(3) -0.021(3) O4W 0.063(4) 0.065(3) 0.207(7) -0.032(4) -0.037(4) -0.003(3) O5W 0.030(4) 0.023(3) 0.059(4) -0.015(3) -0.006(3) -0.001(3) O6W 0.034(4) 0.026(3) 0.066(5) -0.013(3) 0.002(3) -0.012(3) O13 0.023(3) 0.029(3) 0.073(5) -0.010(3) -0.005(3) -0.012(3) O13A 0.024(4) 0.032(4) 0.086(5) -0.018(4) -0.005(3) -0.006(3) O14 0.093(8) 0.092(8) 0.049(5) -0.010(5) -0.023(5) -0.054(7) O14A 0.036(5) 0.130(10) 0.055(5) -0.013(6) 0.017(4) -0.021(6) O15 0.096(8) 0.103(8) 0.048(5) -0.010(5) 0.019(5) -0.082(7) O15A 0.059(6) 0.084(7) 0.055(6) 0.002(5) -0.022(4) 0.001(6) Pr1 0.0159(3) 0.0187(3) 0.0322(3) -0.00453(19) -0.00188(18) -0.00634(19) Pr2 0.0178(3) 0.0190(3) 0.0468(3) -0.0068(2) -0.0048(2) -0.0060(2) Cl1 0.132(2) 0.119(2) 0.149(2) -0.0361(18) 0.006(2) -0.0467(19) Cl2 0.130(2) 0.121(2) 0.156(3) -0.0333(19) -0.021(2) -0.0308(19) C1 0.027(2) 0.018(2) 0.033(2) -0.0065(17) -0.0030(18) -0.0058(18) C2 0.024(2) 0.020(2) 0.044(3) -0.0078(19) -0.0074(19) -0.0071(18) C3 0.020(2) 0.020(2) 0.043(3) -0.0069(19) 0.0003(18) -0.0064(18) C4 0.021(2) 0.022(2) 0.051(3) -0.007(2) -0.006(2) -0.0012(19) C5 0.034(3) 0.024(2) 0.034(2) -0.0096(18) 0.0010(19) -0.013(2) C6 0.022(2) 0.042(3) 0.045(3) -0.007(2) -0.001(2) -0.009(2) C7 0.027(2) 0.026(2) 0.032(2) -0.0076(18) -0.0023(19) -0.0075(19) C8 0.023(2) 0.028(2) 0.034(2) -0.0045(19) 0.0053(18) -0.0088(19) C9 0.036(3) 0.030(2) 0.034(2) -0.009(2) 0.008(2) -0.014(2) C10 0.030(3) 0.035(3) 0.048(3) -0.009(2) 0.000(2) -0.015(2) C11 0.033(3) 0.026(2) 0.035(2) -0.0023(19) -0.0018(19) -0.008(2) C12 0.041(3) 0.027(2) 0.046(3) -0.007(2) 0.011(2) -0.017(2) C13 0.028(3) 0.032(2) 0.036(2) -0.011(2) -0.008(2) -0.006(2) C14 0.042(3) 0.027(2) 0.039(3) -0.007(2) 0.002(2) -0.014(2) C15 0.049(3) 0.023(2) 0.035(2) -0.0046(19) 0.002(2) -0.012(2) C16 0.038(3) 0.038(3) 0.055(3) -0.017(2) 0.016(2) -0.023(2) C17 0.041(3) 0.022(2) 0.041(3) -0.004(2) -0.010(2) 0.000(2) C18 0.045(3) 0.038(3) 0.050(3) -0.016(2) 0.011(2) -0.025(2) C19 0.020(2) 0.015(2) 0.038(2) -0.0031(17) -0.0025(18) -0.0003(17) C20 0.027(2) 0.018(2) 0.045(3) -0.0045(19) -0.0011(19) -0.0065(18) C21 0.019(2) 0.022(2) 0.046(3) -0.0061(19) -0.0050(18) -0.0072(18) C22 0.028(3) 0.019(2) 0.053(3) -0.004(2) -0.002(2) -0.013(2) C23 0.023(2) 0.027(2) 0.041(3) -0.008(2) 0.0028(19) -0.0024(19) C24 0.028(3) 0.030(3) 0.051(3) -0.003(2) -0.010(2) -0.015(2) C25 0.028(2) 0.023(2) 0.034(2) -0.0046(18) 0.0010(19) -0.0078(19) C26 0.032(3) 0.030(2) 0.032(2) -0.0078(19) -0.0028(19) -0.009(2) C27 0.035(3) 0.026(2) 0.031(2) -0.0082(18) -0.0047(19) -0.011(2) C28 0.032(3) 0.031(3) 0.042(3) 0.000(2) -0.011(2) -0.013(2) C29 0.033(3) 0.026(2) 0.038(2) -0.0026(19) -0.0025(19) -0.016(2) C30 0.040(3) 0.028(2) 0.040(3) -0.010(2) -0.012(2) -0.012(2) C31 0.036(3) 0.031(2) 0.031(2) -0.0046(19) 0.001(2) -0.020(2) C32 0.034(3) 0.025(2) 0.033(2) -0.0058(18) -0.0062(19) -0.008(2) C33 0.042(3) 0.024(2) 0.035(2) -0.0036(19) -0.007(2) -0.013(2) C34 0.034(3) 0.027(2) 0.042(3) -0.007(2) -0.008(2) -0.010(2) C35 0.042(3) 0.026(2) 0.033(2) -0.0044(19) -0.003(2) -0.019(2) C36 0.029(3) 0.028(2) 0.053(3) -0.015(2) -0.014(2) -0.001(2) C37 0.039(3) 0.022(2) 0.052(3) -0.003(2) -0.009(2) -0.006(2) C38 0.058(4) 0.021(2) 0.065(4) -0.010(2) -0.001(3) -0.012(2) C39 0.046(3) 0.026(3) 0.071(4) -0.016(2) -0.017(3) -0.001(2) C40 0.036(3) 0.027(3) 0.058(3) -0.017(2) 0.001(2) -0.002(2) C41 0.056(3) 0.033(3) 0.033(2) -0.013(2) 0.007(2) -0.012(2) C42 0.067(4) 0.070(4) 0.066(4) -0.028(3) 0.017(3) -0.023(4) C43 0.091(5) 0.064(4) 0.053(4) -0.023(3) 0.023(3) -0.036(4) C44 0.050(3) 0.038(3) 0.036(3) -0.010(2) 0.004(2) -0.019(2) C45 0.078(4) 0.042(3) 0.033(3) -0.005(2) -0.003(3) -0.017(3) C46 0.199(11) 0.082(6) 0.051(4) -0.012(4) 0.024(5) -0.072(7) C47 0.160(9) 0.073(5) 0.055(4) -0.003(4) 0.006(5) -0.059(6) C48 0.110(6) 0.033(3) 0.043(3) -0.001(2) 0.006(3) -0.021(3) C49 0.052(3) 0.022(2) 0.045(3) 0.001(2) -0.003(2) -0.014(2) C50 0.059(4) 0.023(3) 0.066(4) -0.008(2) -0.018(3) -0.003(2) C51 0.042(3) 0.022(3) 0.077(4) -0.009(2) 0.003(3) -0.005(2) C52 0.039(3) 0.023(2) 0.055(3) -0.011(2) -0.001(2) -0.010(2) C53 0.062(4) 0.030(3) 0.035(3) -0.010(2) -0.002(2) -0.014(2) C54 0.104(6) 0.066(5) 0.090(5) -0.030(4) -0.020(5) -0.023(4) C55 0.107(6) 0.074(5) 0.047(4) -0.014(3) -0.002(4) -0.016(4) C56 0.052(3) 0.037(3) 0.030(2) -0.006(2) 0.004(2) -0.018(2) C57 0.050(3) 0.037(3) 0.038(3) -0.004(2) -0.003(2) -0.013(2) C58 0.085(5) 0.052(4) 0.038(3) 0.003(3) -0.023(3) -0.021(3) C59 0.080(5) 0.043(3) 0.044(3) 0.000(3) -0.024(3) -0.008(3) C60 0.062(4) 0.028(3) 0.040(3) -0.002(2) -0.013(2) -0.014(2) N1 0.027(2) 0.026(2) 0.038(2) -0.0090(16) -0.0055(16) -0.0076(16) N2 0.0239(19) 0.0239(19) 0.033(2) -0.0076(15) -0.0018(15) -0.0075(15) N3 0.029(2) 0.0246(19) 0.046(2) -0.0080(17) -0.0080(17) -0.0124(17) N4 0.028(2) 0.031(2) 0.041(2) -0.0052(17) -0.0031(16) -0.0157(17) N5 0.027(2) 0.028(2) 0.0290(19) -0.0020(15) 0.0032(15) -0.0145(16) N6 0.027(2) 0.029(2) 0.036(2) -0.0054(16) 0.0006(16) -0.0102(17) N7 0.025(2) 0.033(2) 0.044(2) -0.0058(17) -0.0004(17) -0.0121(17) N8 0.036(2) 0.027(2) 0.049(2) -0.0090(18) 0.0068(18) -0.0175(18) N9 0.039(2) 0.028(2) 0.032(2) -0.0068(16) 0.0004(17) -0.0107(18) N10 0.033(2) 0.032(2) 0.040(2) -0.0093(17) -0.0014(17) -0.0076(18) N11 0.036(2) 0.031(2) 0.049(2) -0.0139(18) 0.0126(19) -0.0145(19) N12 0.033(2) 0.037(2) 0.049(2) -0.0161(19) 0.0077(18) -0.0188(19) N13 0.029(2) 0.026(2) 0.039(2) -0.0066(16) -0.0072(16) -0.0091(17) N14 0.0224(19) 0.0221(19) 0.041(2) -0.0048(16) -0.0014(16) -0.0096(15) N15 0.029(2) 0.029(2) 0.040(2) -0.0107(17) 0.0033(17) -0.0092(17) N16 0.0220(19) 0.0224(19) 0.041(2) -0.0020(16) -0.0019(16) -0.0049(15) N17 0.026(2) 0.026(2) 0.037(2) -0.0071(16) -0.0057(16) -0.0039(16) N18 0.031(2) 0.028(2) 0.036(2) -0.0066(16) -0.0045(16) -0.0109(17) N19 0.027(2) 0.0213(19) 0.051(2) -0.0038(17) -0.0064(17) -0.0075(16) N20 0.028(2) 0.026(2) 0.038(2) -0.0061(16) -0.0061(16) -0.0062(16) N21 0.036(2) 0.0253(19) 0.0295(19) -0.0059(15) -0.0029(16) -0.0137(17) N22 0.028(2) 0.031(2) 0.039(2) -0.0110(17) -0.0021(16) -0.0140(17) N23 0.038(2) 0.0234(19) 0.039(2) -0.0073(16) -0.0055(17) -0.0114(17) N24 0.029(2) 0.0244(19) 0.043(2) -0.0095(16) -0.0054(17) -0.0084(16) O1 0.0223(18) 0.046(2) 0.0425(18) -0.0094(15) -0.0023(14) -0.0155(15) O2 0.0260(18) 0.042(2) 0.0418(18) -0.0054(15) 0.0035(15) -0.0144(15) O3 0.0292(19) 0.051(2) 0.055(2) -0.0203(17) 0.0013(16) -0.0155(17) O4 0.0259(18) 0.044(2) 0.051(2) -0.0099(16) -0.0058(15) -0.0159(16) O5 0.0285(18) 0.0390(19) 0.0454(19) -0.0061(15) -0.0083(15) -0.0128(15) O6 0.0309(18) 0.043(2) 0.0414(18) -0.0094(15) -0.0048(15) -0.0170(15) O7 0.0329(19) 0.0337(18) 0.065(2) -0.0114(16) -0.0053(16) -0.0218(16) O8 0.047(2) 0.055(2) 0.076(3) -0.007(2) -0.008(2) -0.033(2) O9 0.032(2) 0.060(3) 0.098(3) -0.040(2) 0.004(2) -0.016(2) O10 0.0181(18) 0.0311(18) 0.078(3) -0.0174(17) -0.0029(16) -0.0020(15) O11 0.029(2) 0.041(2) 0.073(3) 0.0036(18) -0.0052(18) -0.0089(17) O12 0.039(2) 0.054(2) 0.080(3) -0.034(2) 0.0063(19) -0.0252(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N25 O15 1.181(11) . ? N25 O14 1.247(11) . ? N25 O13 1.285(10) . ? N25A O14A 1.201(11) . ? N25A O15A 1.248(11) . ? N25A O13A 1.250(10) . ? O1W Pr1 2.408(5) . ? O2W Pr2 2.505(7) . ? O3W Pr1 2.592(6) 1_545 ? O4W Pr2 2.449(7) . ? O5W Pr1 1.366(6) . ? O5W O6W 1.445(9) . ? O5W O13 1.777(9) . ? O5W Pr2 2.491(6) . ? O6W Pr2 1.343(7) . ? O6W O13A 1.777(9) . ? O6W Pr1 2.507(6) . ? O13 Pr1 2.508(6) . ? O13A Pr2 2.518(7) . ? O14 O15A 1.109(12) . ? O14A O15 1.302(14) . ? Pr1 Cl2 2.490(3) . ? Pr1 Cl1 2.525(3) . ? Pr1 O2 2.526(3) . ? Pr1 O6 2.537(3) . ? Pr1 O1 2.560(3) . ? Pr1 O3W 2.592(6) 1_565 ? Pr1 Pr2 3.0520(6) . ? Pr2 Cl1 2.489(3) . ? Pr2 O5 2.508(3) . ? Pr2 Cl2 2.516(3) . ? Pr2 O4 2.567(3) . ? Pr2 O3 2.573(4) . ? C1 O1 1.235(5) . ? C1 N1 1.347(6) . ? C1 N2 1.370(6) . ? C2 N3 1.465(5) . ? C2 N1 1.474(6) . ? C2 C37 1.507(6) . ? C2 C3 1.557(6) . ? C3 N2 1.459(6) . ? C3 N4 1.466(5) . ? C3 C40 1.515(6) . ? C4 O7 1.234(5) . ? C4 N4 1.360(6) . ? C4 N3 1.364(6) . ? C5 N2 1.434(6) . ? C5 N5 1.437(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.435(6) . ? C6 N7 1.451(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.213(5) . ? C7 N6 1.369(6) . ? C7 N5 1.377(6) . ? C8 N7 1.459(6) . ? C8 N5 1.469(5) . ? C8 C41 1.521(6) . ? C8 C9 1.559(6) . ? C9 N6 1.451(6) . ? C9 N8 1.461(6) . ? C9 C44 1.533(6) . ? C10 O8 1.214(6) . ? C10 N7 1.356(6) . ? C10 N8 1.374(6) . ? C11 N6 1.437(6) . ? C11 N9 1.455(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.449(6) . ? C12 N11 1.455(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.218(6) . ? C13 N9 1.369(6) . ? C13 N10 1.387(6) . ? C14 N11 1.450(7) . ? C14 N9 1.459(6) . ? C14 C45 1.512(7) . ? C14 C15 1.588(6) . ? C15 N10 1.444(6) . ? C15 N12 1.449(7) . ? C15 C48 1.526(7) . ? C16 O9 1.231(7) . ? C16 N11 1.358(6) . ? C16 N12 1.364(6) . ? C17 N10 1.438(6) . ? C17 N13 1.458(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.443(6) . ? C18 N12 1.446(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.238(5) . ? C19 N13 1.349(6) . ? C19 N14 1.353(6) . ? C20 N15 1.448(6) . ? C20 N13 1.465(6) . ? C20 C49 1.511(6) . ? C20 C21 1.553(7) . ? C21 N16 1.460(6) . ? C21 N14 1.468(5) . ? C21 C52 1.524(6) . ? C22 O10 1.217(6) . ? C22 N15 1.364(6) . ? C22 N16 1.366(6) . ? C23 N17 1.437(6) . ? C23 N14 1.441(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.450(6) . ? C24 N16 1.450(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.228(5) . ? C25 N18 1.360(6) . ? C25 N17 1.361(6) . ? C26 N19 1.445(6) . ? C26 N17 1.455(6) . ? C26 C53 1.531(6) . ? C26 C27 1.560(6) . ? C27 N18 1.458(5) . ? C27 N20 1.464(6) . ? C27 C56 1.532(6) . ? C28 O11 1.215(6) . ? C28 N19 1.365(6) . ? C28 N20 1.371(6) . ? C29 N21 1.440(6) . ? C29 N18 1.448(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.432(6) . ? C30 N23 1.454(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O6 1.229(6) . ? C31 N22 1.365(6) . ? C31 N21 1.376(5) . ? C32 N23 1.450(6) . ? C32 N21 1.461(6) . ? C32 C57 1.519(7) . ? C32 C33 1.581(6) . ? C33 N22 1.443(6) . ? C33 N24 1.464(6) . ? C33 C60 1.508(7) . ? C34 O12 1.220(6) . ? C34 N24 1.358(5) . ? C34 N23 1.361(6) . ? C35 N1 1.448(6) . ? C35 N22 1.453(5) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N3 1.426(6) . ? C36 N24 1.447(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C38 1.517(7) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 C39 1.528(8) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C39 C40 1.531(7) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 C42 1.556(8) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 C43 1.530(10) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 C44 1.516(8) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.578(10) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C46 C47 1.549(10) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C47 C48 1.552(11) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.526(8) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.545(8) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.521(7) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.546(9) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.527(10) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.537(9) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C58 1.554(8) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 C59 1.511(8) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 C60 1.539(7) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 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 O15 N25 O14 121.0(9) . . ? O15 N25 O13 121.8(8) . . ? O14 N25 O13 117.1(9) . . ? O14A N25A O15A 117.5(9) . . ? O14A N25A O13A 121.8(9) . . ? O15A N25A O13A 120.6(9) . . ? Pr1 O5W O6W 126.2(5) . . ? Pr1 O5W O13 105.1(4) . . ? O6W O5W O13 128.6(5) . . ? Pr1 O5W Pr2 100.5(3) . . ? O6W O5W Pr2 25.7(3) . . ? O13 O5W Pr2 153.8(4) . . ? Pr2 O6W O5W 126.6(5) . . ? Pr2 O6W O13A 106.8(4) . . ? O5W O6W O13A 126.1(6) . . ? Pr2 O6W Pr1 100.5(3) . . ? O5W O6W Pr1 26.1(3) . . ? O13A O6W Pr1 152.0(4) . . ? N25 O13 O5W 101.8(6) . . ? N25 O13 Pr1 133.5(5) . . ? O5W O13 Pr1 31.7(2) . . ? N25A O13A O6W 104.6(6) . . ? N25A O13A Pr2 135.3(5) . . ? O6W O13A Pr2 30.7(2) . . ? O15A O14 N25 106.1(11) . . ? N25A O14A O15 105.0(10) . . ? N25 O15 O14A 109.1(10) . . ? O14 O15A N25A 115.8(11) . . ? O5W Pr1 O1W 147.1(3) . . ? O5W Pr1 Cl2 95.0(3) . . ? O1W Pr1 Cl2 67.97(14) . . ? O5W Pr1 O6W 27.7(3) . . ? O1W Pr1 O6W 137.8(2) . . ? Cl2 Pr1 O6W 71.99(18) . . ? O5W Pr1 O13 43.2(3) . . ? O1W Pr1 O13 130.04(19) . . ? Cl2 Pr1 O13 131.30(18) . . ? O6W Pr1 O13 70.9(2) . . ? O5W Pr1 Cl1 95.0(3) . . ? O1W Pr1 Cl1 103.31(14) . . ? Cl2 Pr1 Cl1 67.69(12) . . ? O6W Pr1 Cl1 72.29(17) . . ? O13 Pr1 Cl1 126.44(18) . . ? O5W Pr1 O2 77.9(3) . . ? O1W Pr1 O2 71.04(16) . . ? Cl2 Pr1 O2 77.21(11) . . ? O6W Pr1 O2 87.96(18) . . ? O13 Pr1 O2 71.13(19) . . ? Cl1 Pr1 O2 143.50(11) . . ? O5W Pr1 O6 80.5(3) . . ? O1W Pr1 O6 130.61(16) . . ? Cl2 Pr1 O6 140.89(11) . . ? O6W Pr1 O6 89.50(18) . . ? O13 Pr1 O6 68.25(19) . . ? Cl1 Pr1 O6 73.99(11) . . ? O2 Pr1 O6 137.75(11) . . ? O5W Pr1 O1 111.8(3) . . ? O1W Pr1 O1 72.56(13) . . ? Cl2 Pr1 O1 138.39(10) . . ? O6W Pr1 O1 139.53(17) . . ? O13 Pr1 O1 68.69(16) . . ? Cl1 Pr1 O1 136.09(11) . . ? O2 Pr1 O1 78.09(10) . . ? O6 Pr1 O1 76.89(10) . . ? O5W Pr1 O3W 144.4(3) . 1_565 ? O1W Pr1 O3W 68.44(19) . 1_565 ? Cl2 Pr1 O3W 102.42(15) . 1_565 ? O6W Pr1 O3W 134.6(2) . 1_565 ? O13 Pr1 O3W 126.1(2) . 1_565 ? Cl1 Pr1 O3W 64.46(13) . 1_565 ? O2 Pr1 O3W 135.96(15) . 1_565 ? O6 Pr1 O3W 66.35(15) . 1_565 ? O1 Pr1 O3W 74.04(13) . 1_565 ? O5W Pr1 Pr2 53.4(3) . . ? O1W Pr1 Pr2 120.52(11) . . ? Cl2 Pr1 Pr2 52.81(7) . . ? O6W Pr1 Pr2 25.64(16) . . ? O13 Pr1 Pr2 96.38(14) . . ? Cl1 Pr1 Pr2 51.96(8) . . ? O2 Pr1 Pr2 98.62(8) . . ? O6 Pr1 Pr2 96.92(7) . . ? O1 Pr1 Pr2 165.03(7) . . ? O3W Pr1 Pr2 116.33(11) 1_565 . ? O6W Pr2 O4W 150.7(4) . . ? O6W Pr2 Cl1 97.0(3) . . ? O4W Pr2 Cl1 67.19(16) . . ? O6W Pr2 O5W 27.8(3) . . ? O4W Pr2 O5W 139.2(2) . . ? Cl1 Pr2 O5W 73.37(18) . . ? O6W Pr2 O2W 142.4(4) . . ? O4W Pr2 O2W 66.9(2) . . ? Cl1 Pr2 O2W 104.32(17) . . ? O5W Pr2 O2W 135.7(2) . . ? O6W Pr2 O5 83.2(3) . . ? O4W Pr2 O5 69.16(18) . . ? Cl1 Pr2 O5 74.35(11) . . ? O5W Pr2 O5 90.76(17) . . ? O2W Pr2 O5 132.15(17) . . ? O6W Pr2 Cl2 94.2(3) . . ? O4W Pr2 Cl2 101.53(16) . . ? Cl1 Pr2 Cl2 67.86(12) . . ? O5W Pr2 Cl2 72.01(16) . . ? O2W Pr2 Cl2 66.77(14) . . ? O5 Pr2 Cl2 141.52(11) . . ? O6W Pr2 O13A 42.5(3) . . ? O4W Pr2 O13A 128.4(2) . . ? Cl1 Pr2 O13A 127.5(2) . . ? O5W Pr2 O13A 70.1(2) . . ? O2W Pr2 O13A 128.2(2) . . ? O5 Pr2 O13A 69.8(2) . . ? Cl2 Pr2 O13A 130.06(18) . . ? O6W Pr2 O4 110.9(3) . . ? O4W Pr2 O4 73.57(15) . . ? Cl1 Pr2 O4 138.06(11) . . ? O5W Pr2 O4 138.68(17) . . ? O2W Pr2 O4 71.97(14) . . ? O5 Pr2 O4 78.49(11) . . ? Cl2 Pr2 O4 136.46(11) . . ? O13A Pr2 O4 68.76(17) . . ? O6W Pr2 O3 75.5(3) . . ? O4W Pr2 O3 132.02(18) . . ? Cl1 Pr2 O3 143.12(10) . . ? O5W Pr2 O3 86.80(18) . . ? O2W Pr2 O3 68.83(19) . . ? O5 Pr2 O3 138.02(11) . . ? Cl2 Pr2 O3 76.63(11) . . ? O13A Pr2 O3 70.0(2) . . ? O4 Pr2 O3 76.15(11) . . ? O6W Pr2 Pr1 53.9(3) . . ? O4W Pr2 Pr1 119.80(14) . . ? Cl1 Pr2 Pr1 53.06(7) . . ? O5W Pr2 Pr1 26.11(15) . . ? O2W Pr2 Pr1 118.77(12) . . ? O5 Pr2 Pr1 98.82(8) . . ? Cl2 Pr2 Pr1 52.04(8) . . ? O13A Pr2 Pr1 96.15(15) . . ? O4 Pr2 Pr1 164.75(8) . . ? O3 Pr2 Pr1 97.06(8) . . ? Pr2 Cl1 Pr1 74.99(9) . . ? Pr1 Cl2 Pr2 75.14(10) . . ? O1 C1 N1 125.9(4) . . ? O1 C1 N2 124.6(4) . . ? N1 C1 N2 109.4(4) . . ? N3 C2 N1 111.5(3) . . ? N3 C2 C37 113.1(4) . . ? N1 C2 C37 111.9(4) . . ? N3 C2 C3 103.7(3) . . ? N1 C2 C3 102.9(3) . . ? C37 C2 C3 112.9(4) . . ? N2 C3 N4 112.1(3) . . ? N2 C3 C40 112.3(4) . . ? N4 C3 C40 113.1(4) . . ? N2 C3 C2 103.1(3) . . ? N4 C3 C2 103.1(3) . . ? C40 C3 C2 112.4(4) . . ? O7 C4 N4 124.9(5) . . ? O7 C4 N3 124.8(4) . . ? N4 C4 N3 110.2(4) . . ? N2 C5 N5 114.6(3) . . ? N2 C5 H5A 108.6 . . ? N5 C5 H5A 108.6 . . ? N2 C5 H5B 108.6 . . ? N5 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N4 C6 N7 113.7(4) . . ? N4 C6 H6A 108.8 . . ? N7 C6 H6A 108.8 . . ? N4 C6 H6B 108.8 . . ? N7 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 126.0(4) . . ? O2 C7 N5 125.1(4) . . ? N6 C7 N5 108.9(4) . . ? N7 C8 N5 111.2(3) . . ? N7 C8 C41 113.7(4) . . ? N5 C8 C41 112.6(4) . . ? N7 C8 C9 102.6(3) . . ? N5 C8 C9 103.0(3) . . ? C41 C8 C9 112.7(4) . . ? N6 C9 N8 111.8(3) . . ? N6 C9 C44 113.8(4) . . ? N8 C9 C44 113.0(4) . . ? N6 C9 C8 103.3(3) . . ? N8 C9 C8 102.6(4) . . ? C44 C9 C8 111.4(4) . . ? O8 C10 N7 126.7(5) . . ? O8 C10 N8 125.3(5) . . ? N7 C10 N8 108.0(4) . . ? N6 C11 N9 115.1(4) . . ? N6 C11 H11A 108.5 . . ? N9 C11 H11A 108.5 . . ? N6 C11 H11B 108.5 . . ? N9 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N8 C12 N11 114.5(4) . . ? N8 C12 H12A 108.6 . . ? N11 C12 H12A 108.6 . . ? N8 C12 H12B 108.6 . . ? N11 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N9 125.8(4) . . ? O3 C13 N10 125.8(4) . . ? N9 C13 N10 108.3(4) . . ? N11 C14 N9 112.4(4) . . ? N11 C14 C45 113.6(4) . . ? N9 C14 C45 113.6(4) . . ? N11 C14 C15 101.8(4) . . ? N9 C14 C15 102.8(4) . . ? C45 C14 C15 111.4(4) . . ? N10 C15 N12 112.5(4) . . ? N10 C15 C48 114.0(5) . . ? N12 C15 C48 113.1(5) . . ? N10 C15 C14 102.2(4) . . ? N12 C15 C14 102.4(4) . . ? C48 C15 C14 111.6(4) . . ? O9 C16 N11 126.2(5) . . ? O9 C16 N12 124.9(5) . . ? N11 C16 N12 108.8(5) . . ? N10 C17 N13 114.0(4) . . ? N10 C17 H17A 108.8 . . ? N13 C17 H17A 108.8 . . ? N10 C17 H17B 108.8 . . ? N13 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N15 C18 N12 113.7(4) . . ? N15 C18 H18A 108.8 . . ? N12 C18 H18A 108.8 . . ? N15 C18 H18B 108.8 . . ? N12 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? O4 C19 N13 125.5(4) . . ? O4 C19 N14 124.9(4) . . ? N13 C19 N14 109.6(4) . . ? N15 C20 N13 112.2(3) . . ? N15 C20 C49 113.2(4) . . ? N13 C20 C49 112.1(4) . . ? N15 C20 C21 103.0(4) . . ? N13 C20 C21 102.9(3) . . ? C49 C20 C21 112.6(4) . . ? N16 C21 N14 112.7(3) . . ? N16 C21 C52 113.3(4) . . ? N14 C21 C52 111.4(4) . . ? N16 C21 C20 103.6(3) . . ? N14 C21 C20 102.9(3) . . ? C52 C21 C20 112.3(4) . . ? O10 C22 N15 125.8(5) . . ? O10 C22 N16 125.2(5) . . ? N15 C22 N16 109.0(4) . . ? N17 C23 N14 114.7(3) . . ? N17 C23 H23A 108.6 . . ? N14 C23 H23A 108.6 . . ? N17 C23 H23B 108.6 . . ? N14 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? N19 C24 N16 113.3(4) . . ? N19 C24 H24A 108.9 . . ? N16 C24 H24A 108.9 . . ? N19 C24 H24B 108.9 . . ? N16 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? O5 C25 N18 124.2(4) . . ? O5 C25 N17 126.3(4) . . ? N18 C25 N17 109.4(4) . . ? N19 C26 N17 112.3(4) . . ? N19 C26 C53 113.8(4) . . ? N17 C26 C53 111.9(4) . . ? N19 C26 C27 103.1(4) . . ? N17 C26 C27 102.5(3) . . ? C53 C26 C27 112.3(4) . . ? N18 C27 N20 112.3(3) . . ? N18 C27 C56 113.4(4) . . ? N20 C27 C56 112.8(4) . . ? N18 C27 C26 103.2(3) . . ? N20 C27 C26 102.5(4) . . ? C56 C27 C26 111.7(3) . . ? O11 C28 N19 126.2(5) . . ? O11 C28 N20 125.3(4) . . ? N19 C28 N20 108.4(4) . . ? N21 C29 N18 115.2(4) . . ? N21 C29 H29A 108.5 . . ? N18 C29 H29A 108.5 . . ? N21 C29 H29B 108.5 . . ? N18 C29 H29B 108.5 . . ? H29A C29 H29B 107.5 . . ? N20 C30 N23 115.9(4) . . ? N20 C30 H30A 108.3 . . ? N23 C30 H30A 108.3 . . ? N20 C30 H30B 108.3 . . ? N23 C30 H30B 108.3 . . ? H30A C30 H30B 107.4 . . ? O6 C31 N22 126.4(4) . . ? O6 C31 N21 124.7(4) . . ? N22 C31 N21 108.8(4) . . ? N23 C32 N21 112.5(4) . . ? N23 C32 C57 113.6(4) . . ? N21 C32 C57 112.5(4) . . ? N23 C32 C33 102.4(4) . . ? N21 C32 C33 103.3(3) . . ? C57 C32 C33 111.6(4) . . ? N22 C33 N24 112.2(4) . . ? N22 C33 C60 113.2(4) . . ? N24 C33 C60 113.9(4) . . ? N22 C33 C32 101.8(4) . . ? N24 C33 C32 101.6(3) . . ? C60 C33 C32 112.9(4) . . ? O12 C34 N24 125.5(4) . . ? O12 C34 N23 125.9(4) . . ? N24 C34 N23 108.5(4) . . ? N1 C35 N22 114.3(4) . . ? N1 C35 H35A 108.7 . . ? N22 C35 H35A 108.7 . . ? N1 C35 H35B 108.7 . . ? N22 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? N3 C36 N24 114.3(4) . . ? N3 C36 H36A 108.7 . . ? N24 C36 H36A 108.7 . . ? N3 C36 H36B 108.7 . . ? N24 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C2 C37 C38 111.6(4) . . ? C2 C37 H37A 109.3 . . ? C38 C37 H37A 109.3 . . ? C2 C37 H37B 109.3 . . ? C38 C37 H37B 109.3 . . ? H37A C37 H37B 108.0 . . ? C37 C38 C39 114.5(4) . . ? C37 C38 H38A 108.6 . . ? C39 C38 H38A 108.6 . . ? C37 C38 H38B 108.6 . . ? C39 C38 H38B 108.6 . . ? H38A C38 H38B 107.6 . . ? C38 C39 C40 111.5(4) . . ? C38 C39 H39A 109.3 . . ? C40 C39 H39A 109.3 . . ? C38 C39 H39B 109.3 . . ? C40 C39 H39B 109.3 . . ? H39A C39 H39B 108.0 . . ? C3 C40 C39 111.7(4) . . ? C3 C40 H40A 109.3 . . ? C39 C40 H40A 109.3 . . ? C3 C40 H40B 109.3 . . ? C39 C40 H40B 109.3 . . ? H40A C40 H40B 107.9 . . ? C8 C41 C42 108.1(4) . . ? C8 C41 H41A 110.1 . . ? C42 C41 H41A 110.1 . . ? C8 C41 H41B 110.1 . . ? C42 C41 H41B 110.1 . . ? H41A C41 H41B 108.4 . . ? C43 C42 C41 112.9(5) . . ? C43 C42 H42A 109.0 . . ? C41 C42 H42A 109.0 . . ? C43 C42 H42B 109.0 . . ? C41 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? C44 C43 C42 111.5(5) . . ? C44 C43 H43A 109.3 . . ? C42 C43 H43A 109.3 . . ? C44 C43 H43B 109.3 . . ? C42 C43 H43B 109.3 . . ? H43A C43 H43B 108.0 . . ? C43 C44 C9 112.0(5) . . ? C43 C44 H44A 109.2 . . ? C9 C44 H44A 109.2 . . ? C43 C44 H44B 109.2 . . ? C9 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? C14 C45 C46 109.4(5) . . ? C14 C45 H45A 109.8 . . ? C46 C45 H45A 109.8 . . ? C14 C45 H45B 109.8 . . ? C46 C45 H45B 109.8 . . ? H45A C45 H45B 108.3 . . ? C47 C46 C45 112.8(6) . . ? C47 C46 H46A 109.0 . . ? C45 C46 H46A 109.0 . . ? C47 C46 H46B 109.0 . . ? C45 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? C46 C47 C48 109.5(7) . . ? C46 C47 H47A 109.8 . . ? C48 C47 H47A 109.8 . . ? C46 C47 H47B 109.8 . . ? C48 C47 H47B 109.8 . . ? H47A C47 H47B 108.2 . . ? C15 C48 C47 108.0(6) . . ? C15 C48 H48A 110.1 . . ? C47 C48 H48A 110.1 . . ? C15 C48 H48B 110.1 . . ? C47 C48 H48B 110.1 . . ? H48A C48 H48B 108.4 . . ? C20 C49 C50 111.8(4) . . ? C20 C49 H49A 109.3 . . ? C50 C49 H49A 109.3 . . ? C20 C49 H49B 109.3 . . ? C50 C49 H49B 109.3 . . ? H49A C49 H49B 107.9 . . ? C49 C50 C51 112.3(4) . . ? C49 C50 H50A 109.1 . . ? C51 C50 H50A 109.1 . . ? C49 C50 H50B 109.1 . . ? C51 C50 H50B 109.1 . . ? H50A C50 H50B 107.9 . . ? C52 C51 C50 112.6(4) . . ? C52 C51 H51A 109.1 . . ? C50 C51 H51A 109.1 . . ? C52 C51 H51B 109.1 . . ? C50 C51 H51B 109.1 . . ? H51A C51 H51B 107.8 . . ? C51 C52 C21 112.2(4) . . ? C51 C52 H52A 109.2 . . ? C21 C52 H52A 109.2 . . ? C51 C52 H52B 109.2 . . ? C21 C52 H52B 109.2 . . ? H52A C52 H52B 107.9 . . ? C26 C53 C54 108.3(5) . . ? C26 C53 H53A 110.0 . . ? C54 C53 H53A 110.0 . . ? C26 C53 H53B 110.0 . . ? C54 C53 H53B 110.0 . . ? H53A C53 H53B 108.4 . . ? C55 C54 C53 111.8(6) . . ? C55 C54 H54A 109.2 . . ? C53 C54 H54A 109.2 . . ? C55 C54 H54B 109.2 . . ? C53 C54 H54B 109.2 . . ? H54A C54 H54B 107.9 . . ? C54 C55 C56 112.5(5) . . ? C54 C55 H55A 109.1 . . ? C56 C55 H55A 109.1 . . ? C54 C55 H55B 109.1 . . ? C56 C55 H55B 109.1 . . ? H55A C55 H55B 107.8 . . ? C27 C56 C55 111.1(4) . . ? C27 C56 H56A 109.4 . . ? C55 C56 H56A 109.4 . . ? C27 C56 H56B 109.4 . . ? C55 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? C32 C57 C58 111.5(5) . . ? C32 C57 H57A 109.3 . . ? C58 C57 H57A 109.3 . . ? C32 C57 H57B 109.3 . . ? C58 C57 H57B 109.3 . . ? H57A C57 H57B 108.0 . . ? C59 C58 C57 113.4(4) . . ? C59 C58 H58A 108.9 . . ? C57 C58 H58A 108.9 . . ? C59 C58 H58B 108.9 . . ? C57 C58 H58B 108.9 . . ? H58A C58 H58B 107.7 . . ? C58 C59 C60 111.8(5) . . ? C58 C59 H59A 109.3 . . ? C60 C59 H59A 109.3 . . ? C58 C59 H59B 109.3 . . ? C60 C59 H59B 109.3 . . ? H59A C59 H59B 107.9 . . ? C33 C60 C59 109.2(4) . . ? C33 C60 H60A 109.8 . . ? C59 C60 H60A 109.8 . . ? C33 C60 H60B 109.8 . . ? C59 C60 H60B 109.8 . . ? H60A C60 H60B 108.3 . . ? C1 N1 C35 121.1(4) . . ? C1 N1 C2 112.3(4) . . ? C35 N1 C2 126.5(4) . . ? C1 N2 C5 120.9(4) . . ? C1 N2 C3 112.2(3) . . ? C5 N2 C3 126.9(4) . . ? C4 N3 C36 121.4(4) . . ? C4 N3 C2 111.3(4) . . ? C36 N3 C2 126.1(4) . . ? C4 N4 C6 121.2(4) . . ? C4 N4 C3 111.8(4) . . ? C6 N4 C3 125.8(4) . . ? C7 N5 C5 122.8(4) . . ? C7 N5 C8 111.6(3) . . ? C5 N5 C8 125.1(4) . . ? C7 N6 C11 120.2(4) . . ? C7 N6 C9 112.3(4) . . ? C11 N6 C9 124.7(4) . . ? C10 N7 C6 121.7(4) . . ? C10 N7 C8 113.2(4) . . ? C6 N7 C8 124.0(4) . . ? C10 N8 C12 122.2(4) . . ? C10 N8 C9 112.6(4) . . ? C12 N8 C9 125.1(4) . . ? C13 N9 C11 119.6(4) . . ? C13 N9 C14 112.3(4) . . ? C11 N9 C14 124.6(4) . . ? C13 N10 C17 121.5(4) . . ? C13 N10 C15 113.0(4) . . ? C17 N10 C15 125.5(4) . . ? C16 N11 C14 113.0(4) . . ? C16 N11 C12 121.4(4) . . ? C14 N11 C12 125.5(4) . . ? C16 N12 C18 122.2(4) . . ? C16 N12 C15 112.5(4) . . ? C18 N12 C15 123.9(4) . . ? C19 N13 C17 120.7(4) . . ? C19 N13 C20 112.4(4) . . ? C17 N13 C20 126.8(4) . . ? C19 N14 C23 122.2(4) . . ? C19 N14 C21 112.1(4) . . ? C23 N14 C21 125.7(4) . . ? C22 N15 C18 120.6(4) . . ? C22 N15 C20 112.7(4) . . ? C18 N15 C20 126.0(4) . . ? C22 N16 C24 121.3(4) . . ? C22 N16 C21 111.6(4) . . ? C24 N16 C21 125.8(4) . . ? C25 N17 C23 122.9(4) . . ? C25 N17 C26 112.2(4) . . ? C23 N17 C26 124.6(4) . . ? C25 N18 C29 121.7(4) . . ? C25 N18 C27 111.6(3) . . ? C29 N18 C27 124.2(4) . . ? C28 N19 C26 112.7(4) . . ? C28 N19 C24 121.4(4) . . ? C26 N19 C24 124.5(4) . . ? C28 N20 C30 122.1(4) . . ? C28 N20 C27 112.1(4) . . ? C30 N20 C27 125.7(4) . . ? C31 N21 C29 120.1(4) . . ? C31 N21 C32 111.2(4) . . ? C29 N21 C32 124.6(3) . . ? C31 N22 C33 113.5(3) . . ? C31 N22 C35 121.6(4) . . ? C33 N22 C35 124.9(4) . . ? C34 N23 C32 112.9(3) . . ? C34 N23 C30 121.2(4) . . ? C32 N23 C30 125.8(4) . . ? C34 N24 C36 122.1(4) . . ? C34 N24 C33 112.9(4) . . ? C36 N24 C33 123.7(4) . . ? C1 O1 Pr1 124.5(3) . . ? C7 O2 Pr1 143.2(3) . . ? C13 O3 Pr2 144.3(3) . . ? C19 O4 Pr2 124.5(3) . . ? C25 O5 Pr2 142.5(3) . . ? C31 O6 Pr1 144.9(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.997 _refine_diff_density_min -1.557 _refine_diff_density_rms 0.123 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.161 0.713 0.000 614 209 ' ' 2 -0.048 0.480 0.500 609 201 ' ' 3 0.450 0.246 0.252 11 9 ' ' 4 0.549 0.754 0.748 11 9 ' ' _platon_squeeze_details ; ; data_p4 _database_code_depnum_ccdc_archive 'CCDC 881902' #TrackingRef '110329qx-submit-cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H106 Eu N27 O38' _chemical_formula_weight 1965.68 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.8602(6) _cell_length_b 15.9876(6) _cell_length_c 18.2197(6) _cell_angle_alpha 74.9540(10) _cell_angle_beta 89.0860(10) _cell_angle_gamma 63.2820(10) _cell_volume 3957.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7856 _exptl_absorpt_correction_T_max 0.8326 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42437 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13757 _reflns_number_gt 11924 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+0.7089P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13757 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1W O -0.24289(17) 0.95246(17) -0.28549(13) 0.0264(5) Uani 1 1 d . . . O2W O -0.10270(16) 0.61888(17) -0.24599(14) 0.0254(5) Uani 1 1 d . . . O3W O -0.05606(16) 0.77435(18) -0.26413(14) 0.0260(5) Uani 1 1 d . . . O4W O -0.38047(17) 0.88514(18) -0.27091(15) 0.0300(6) Uani 1 1 d . . . Eu1 Eu -0.214573(11) 0.785640(11) -0.263239(9) 0.01742(7) Uani 1 1 d . . . C1 C -0.1324(2) 0.4026(2) -0.14061(19) 0.0207(7) Uani 1 1 d . . . C2 C -0.0999(2) 0.2611(2) -0.03941(18) 0.0180(7) Uani 1 1 d . . . C3 C -0.2015(2) 0.3449(2) -0.03740(18) 0.0180(7) Uani 1 1 d . . . C4 C -0.1051(2) 0.3004(2) 0.07680(18) 0.0185(7) Uani 1 1 d . . . C5 C -0.2930(2) 0.5200(2) -0.12680(18) 0.0184(7) Uani 1 1 d . . . H5A H -0.3482 0.5081 -0.1286 0.022 Uiso 1 1 calc R . . H5B H -0.2877 0.5517 -0.1792 0.022 Uiso 1 1 calc R . . C6 C -0.2736(2) 0.4131(2) 0.07491(19) 0.0202(7) Uani 1 1 d . . . H6A H -0.3277 0.4039 0.0610 0.024 Uiso 1 1 calc R . . H6B H -0.2570 0.3856 0.1305 0.024 Uiso 1 1 calc R . . C7 C -0.3019(2) 0.6703(2) -0.10880(18) 0.0174(7) Uani 1 1 d . . . C8 C -0.3619(2) 0.5892(2) -0.01300(19) 0.0192(7) Uani 1 1 d . . . C9 C -0.3776(2) 0.6879(2) 0.00185(18) 0.0183(7) Uani 1 1 d . . . C10 C -0.2816(2) 0.5567(2) 0.10669(19) 0.0202(7) Uani 1 1 d . . . C11 C -0.3446(2) 0.8250(2) -0.08083(19) 0.0172(7) Uani 1 1 d . . . H11A H -0.3480 0.8502 -0.1364 0.021 Uiso 1 1 calc R . . H11B H -0.4027 0.8697 -0.0644 0.021 Uiso 1 1 calc R . . C12 C -0.3101(2) 0.7164(3) 0.11662(19) 0.0228(8) Uani 1 1 d . . . H12A H -0.3724 0.7733 0.1111 0.027 Uiso 1 1 calc R . . H12B H -0.2931 0.6803 0.1710 0.027 Uiso 1 1 calc R . . C13 C -0.1863(2) 0.8162(2) -0.08026(18) 0.0157(7) Uani 1 1 d . . . C14 C -0.2577(2) 0.8372(2) 0.03096(18) 0.0185(7) Uani 1 1 d . . . C15 C -0.1618(2) 0.8421(2) 0.03638(18) 0.0185(7) Uani 1 1 d . . . C16 C -0.1524(2) 0.7083(2) 0.13371(19) 0.0196(7) Uani 1 1 d . . . C17 C 0.0438(2) 0.1632(2) 0.06478(18) 0.0190(7) Uani 1 1 d . . . H17A H 0.0458 0.1051 0.0547 0.023 Uiso 1 1 calc R . . H17B H 0.0501 0.1515 0.1204 0.023 Uiso 1 1 calc R . . C18 C -0.0169(2) 0.7418(2) 0.14058(19) 0.0211(7) Uani 1 1 d . . . H18A H -0.0206 0.8041 0.1423 0.025 Uiso 1 1 calc R . . H18B H -0.0088 0.7023 0.1935 0.025 Uiso 1 1 calc R . . C19 C -0.1030(2) 0.1708(2) -0.0477(2) 0.0252(8) Uani 1 1 d . . . H19A H -0.1231 0.1412 -0.0013 0.030 Uiso 1 1 calc R . . H19B H -0.0391 0.1231 -0.0533 0.030 Uiso 1 1 calc R . . C20 C -0.1716(3) 0.1950(3) -0.1172(2) 0.0317(9) Uani 1 1 d . . . H20A H -0.1787 0.1371 -0.1166 0.038 Uiso 1 1 calc R . . H20B H -0.1445 0.2120 -0.1641 0.038 Uiso 1 1 calc R . . C21 C -0.2700(3) 0.2799(3) -0.1184(2) 0.0327(9) Uani 1 1 d . . . H21A H -0.2821 0.3341 -0.1641 0.039 Uiso 1 1 calc R . . H21B H -0.3186 0.2587 -0.1219 0.039 Uiso 1 1 calc R . . C22 C -0.2786(2) 0.3159(3) -0.0478(2) 0.0248(8) Uani 1 1 d . . . H22A H -0.3411 0.3722 -0.0527 0.030 Uiso 1 1 calc R . . H22B H -0.2737 0.2642 -0.0025 0.030 Uiso 1 1 calc R . . C23 C -0.4554(2) 0.5880(2) -0.02714(19) 0.0214(7) Uani 1 1 d . . . H23A H -0.4849 0.5841 0.0204 0.026 Uiso 1 1 calc R . . H23B H -0.4436 0.5305 -0.0436 0.026 Uiso 1 1 calc R . . C24 C -0.5226(2) 0.6808(3) -0.0889(2) 0.0297(8) Uani 1 1 d . . . H24A H -0.5823 0.6786 -0.0979 0.036 Uiso 1 1 calc R . . H24B H -0.4937 0.6830 -0.1368 0.036 Uiso 1 1 calc R . . C25 C -0.5442(3) 0.7735(3) -0.0658(2) 0.0309(9) Uani 1 1 d . . . H25A H -0.5348 0.8195 -0.1082 0.037 Uiso 1 1 calc R . . H25B H -0.6110 0.8044 -0.0568 0.037 Uiso 1 1 calc R . . C26 C -0.4818(2) 0.7536(2) 0.0060(2) 0.0229(7) Uani 1 1 d . . . H26A H -0.4890 0.8157 0.0119 0.027 Uiso 1 1 calc R . . H26B H -0.5028 0.7225 0.0510 0.027 Uiso 1 1 calc R . . C27 C -0.3433(2) 0.9291(3) 0.0398(2) 0.0260(8) Uani 1 1 d . . . H27A H -0.3554 0.9847 -0.0047 0.031 Uiso 1 1 calc R . . H27B H -0.4000 0.9192 0.0429 0.031 Uiso 1 1 calc R . . C28 C -0.3222(3) 0.9503(3) 0.1128(2) 0.0351(9) Uani 1 1 d . . . H28A H -0.3139 0.8960 0.1572 0.042 Uiso 1 1 calc R . . H28B H -0.3766 1.0094 0.1183 0.042 Uiso 1 1 calc R . . C29 C -0.2328(3) 0.9645(3) 0.1118(2) 0.0370(10) Uani 1 1 d . . . H29A H -0.1912 0.9227 0.1596 0.044 Uiso 1 1 calc R . . H29B H -0.2513 1.0324 0.1099 0.044 Uiso 1 1 calc R . . C30 C -0.1771(3) 0.9408(3) 0.0442(2) 0.0264(8) Uani 1 1 d . . . H30A H -0.2121 0.9920 -0.0030 0.032 Uiso 1 1 calc R . . H30B H -0.1154 0.9393 0.0520 0.032 Uiso 1 1 calc R . . C31 C -0.5737(2) 0.8291(2) -0.31061(18) 0.0167(7) Uani 1 1 d . . . C32 C -0.7076(2) 0.8564(2) -0.38587(18) 0.0178(7) Uani 1 1 d . . . C33 C -0.6205(2) 0.7592(2) -0.39035(18) 0.0175(7) Uani 1 1 d . . . C34 C -0.6722(2) 0.8701(2) -0.51323(19) 0.0187(7) Uani 1 1 d . . . C35 C -0.4476(2) 0.6760(2) -0.32435(18) 0.0171(7) Uani 1 1 d . . . H35A H -0.4522 0.6149 -0.3093 0.021 Uiso 1 1 calc R . . H35B H -0.4186 0.6808 -0.2795 0.021 Uiso 1 1 calc R . . C36 C -0.5527(2) 0.7041(2) -0.5082(2) 0.0194(7) Uani 1 1 d . . . H36A H -0.5809 0.7239 -0.5612 0.023 Uiso 1 1 calc R . . H36B H -0.5532 0.6426 -0.4818 0.023 Uiso 1 1 calc R . . C37 C -0.3082(2) 0.6861(2) -0.37640(17) 0.0162(7) Uani 1 1 d . . . C38 C -0.3800(2) 0.6253(2) -0.44590(18) 0.0168(7) Uani 1 1 d . . . C39 C -0.2883(2) 0.6230(2) -0.48198(18) 0.0166(7) Uani 1 1 d . . . C40 C -0.4220(2) 0.7228(2) -0.57282(19) 0.0196(7) Uani 1 1 d . . . C41 C -0.1625(2) 0.6641(2) -0.43540(18) 0.0164(7) Uani 1 1 d . . . H41A H -0.1167 0.6097 -0.4533 0.020 Uiso 1 1 calc R . . H41B H -0.1372 0.6556 -0.3838 0.020 Uiso 1 1 calc R . . C42 C -0.2725(2) 0.7143(2) -0.61639(19) 0.0205(7) Uani 1 1 d . . . H42A H -0.2136 0.6547 -0.6138 0.025 Uiso 1 1 calc R . . H42B H -0.3088 0.7344 -0.6663 0.025 Uiso 1 1 calc R . . C43 C -0.1875(2) 0.8330(2) -0.46086(18) 0.0171(7) Uani 1 1 d . . . C44 C -0.1632(2) 0.7733(2) -0.56754(18) 0.0163(7) Uani 1 1 d . . . C45 C -0.1683(2) 0.8780(2) -0.59057(18) 0.0162(7) Uani 1 1 d . . . C46 C -0.2949(2) 0.8818(2) -0.65984(18) 0.0197(7) Uani 1 1 d . . . C47 C -0.1871(2) 0.9905(2) -0.50543(19) 0.0181(7) Uani 1 1 d . . . H47A H -0.1755 0.9792 -0.4502 0.022 Uiso 1 1 calc R . . H47B H -0.1335 0.9972 -0.5288 0.022 Uiso 1 1 calc R . . C48 C -0.7242(2) 0.9683(2) -0.30058(18) 0.0187(7) Uani 1 1 d . . . H48A H -0.7822 0.9642 -0.2859 0.022 Uiso 1 1 calc R . . H48B H -0.6875 0.9590 -0.2538 0.022 Uiso 1 1 calc R . . C49 C -0.7919(2) 0.8397(2) -0.3586(2) 0.0222(7) Uani 1 1 d . . . H49A H -0.8428 0.9009 -0.3528 0.027 Uiso 1 1 calc R . . H49B H -0.8162 0.8211 -0.3975 0.027 Uiso 1 1 calc R . . C50 C -0.7655(3) 0.7607(3) -0.2829(2) 0.0309(9) Uani 1 1 d . . . H50A H -0.8169 0.7424 -0.2742 0.037 Uiso 1 1 calc R . . H50B H -0.7599 0.7873 -0.2415 0.037 Uiso 1 1 calc R . . C51 C -0.6720(3) 0.6688(3) -0.2798(2) 0.0287(8) Uani 1 1 d . . . H51A H -0.6235 0.6641 -0.2440 0.034 Uiso 1 1 calc R . . H51B H -0.6817 0.6109 -0.2605 0.034 Uiso 1 1 calc R . . C52 C -0.6367(2) 0.6702(2) -0.3582(2) 0.0217(7) Uani 1 1 d . . . H52A H -0.6836 0.6714 -0.3934 0.026 Uiso 1 1 calc R . . H52B H -0.5771 0.6107 -0.3538 0.026 Uiso 1 1 calc R . . C53 C -0.3713(2) 0.5229(2) -0.4144(2) 0.0239(8) Uani 1 1 d . . . H53A H -0.4243 0.5261 -0.3850 0.029 Uiso 1 1 calc R . . H53B H -0.3742 0.4969 -0.4569 0.029 Uiso 1 1 calc R . . C54 C -0.2776(3) 0.4553(3) -0.3632(2) 0.0302(8) Uani 1 1 d . . . H54A H -0.2732 0.3901 -0.3437 0.036 Uiso 1 1 calc R . . H54B H -0.2768 0.4797 -0.3193 0.036 Uiso 1 1 calc R . . C55 C -0.1914(3) 0.4477(3) -0.4053(2) 0.0307(9) Uani 1 1 d . . . H55A H -0.1491 0.4583 -0.3743 0.037 Uiso 1 1 calc R . . H55B H -0.1564 0.3815 -0.4105 0.037 Uiso 1 1 calc R . . C56 C -0.2175(2) 0.5206(2) -0.4843(2) 0.0232(8) Uani 1 1 d . . . H56A H -0.2451 0.5000 -0.5194 0.028 Uiso 1 1 calc R . . H56B H -0.1599 0.5215 -0.5037 0.028 Uiso 1 1 calc R . . C57 C -0.0718(2) 0.6970(2) -0.58669(19) 0.0207(7) Uani 1 1 d . . . H57A H -0.0178 0.6832 -0.5518 0.025 Uiso 1 1 calc R . . H57B H -0.0760 0.6363 -0.5802 0.025 Uiso 1 1 calc R . . C58 C -0.0567(2) 0.7346(3) -0.66871(19) 0.0247(8) Uani 1 1 d . . . H58A H -0.1114 0.7493 -0.7031 0.030 Uiso 1 1 calc R . . H58B H -0.0002 0.6836 -0.6817 0.030 Uiso 1 1 calc R . . C59 C -0.0439(3) 0.8268(3) -0.6813(2) 0.0305(9) Uani 1 1 d . . . H59A H -0.0805 0.8737 -0.7297 0.037 Uiso 1 1 calc R . . H59B H 0.0233 0.8096 -0.6854 0.037 Uiso 1 1 calc R . . C60 C -0.0761(2) 0.8752(3) -0.61643(19) 0.0215(7) Uani 1 1 d . . . H60A H -0.0264 0.8393 -0.5728 0.026 Uiso 1 1 calc R . . H60B H -0.0843 0.9420 -0.6339 0.026 Uiso 1 1 calc R . . N1 N -0.06651(19) 0.3078(2) -0.10516(15) 0.0201(6) Uani 1 1 d . . . N2 N -0.20856(19) 0.42703(19) -0.09935(15) 0.0190(6) Uani 1 1 d . . . N3 N -0.04801(19) 0.2452(2) 0.03292(15) 0.0197(6) Uani 1 1 d . . . N4 N -0.19376(19) 0.3587(2) 0.03811(15) 0.0199(6) Uani 1 1 d . . . N5 N -0.30973(19) 0.58658(19) -0.08059(15) 0.0174(6) Uani 1 1 d . . . N6 N -0.34159(18) 0.72999(19) -0.06361(15) 0.0177(6) Uani 1 1 d . . . N7 N -0.30297(19) 0.51649(19) 0.05577(15) 0.0198(6) Uani 1 1 d . . . N8 N -0.31751(19) 0.6542(2) 0.07403(15) 0.0201(6) Uani 1 1 d . . . N9 N -0.26409(18) 0.82491(19) -0.04492(15) 0.0168(6) Uani 1 1 d . . . N10 N -0.12478(19) 0.8249(2) -0.03537(15) 0.0186(6) Uani 1 1 d . . . N11 N -0.2404(2) 0.7502(2) 0.09191(16) 0.0202(6) Uani 1 1 d . . . N12 N -0.10647(19) 0.7611(2) 0.10292(15) 0.0190(6) Uani 1 1 d . . . N13 N -0.66856(18) 0.88844(19) -0.33338(15) 0.0170(6) Uani 1 1 d . . . N14 N -0.54271(18) 0.75686(19) -0.34574(15) 0.0171(6) Uani 1 1 d . . . N15 N -0.72713(18) 0.91907(18) -0.46445(15) 0.0167(6) Uani 1 1 d . . . N16 N -0.61052(18) 0.77739(19) -0.47179(15) 0.0190(6) Uani 1 1 d . . . N17 N -0.38508(18) 0.67126(19) -0.38410(15) 0.0159(6) Uani 1 1 d . . . N18 N -0.25084(18) 0.65870(19) -0.43111(15) 0.0167(6) Uani 1 1 d . . . N19 N -0.45427(18) 0.68740(19) -0.50826(15) 0.0173(6) Uani 1 1 d . . . N20 N -0.32710(18) 0.6919(2) -0.55729(15) 0.0180(6) Uani 1 1 d . . . N21 N -0.16996(18) 0.75422(19) -0.48525(15) 0.0163(6) Uani 1 1 d . . . N22 N -0.19001(18) 0.90584(18) -0.51881(15) 0.0158(6) Uani 1 1 d . . . N23 N -0.24835(18) 0.78979(19) -0.61155(15) 0.0174(6) Uani 1 1 d . . . N24 N -0.24907(18) 0.93461(19) -0.64986(15) 0.0171(6) Uani 1 1 d . . . O1 O -0.12443(17) 0.45423(17) -0.20016(14) 0.0258(5) Uani 1 1 d . . . O2 O -0.26682(17) 0.68909(17) -0.16745(13) 0.0227(5) Uani 1 1 d . . . O3 O -0.17326(15) 0.80398(17) -0.14461(12) 0.0203(5) Uani 1 1 d . . . O4 O -0.08118(16) 0.29787(17) 0.14128(13) 0.0247(5) Uani 1 1 d . . . O5 O -0.23761(17) 0.51073(17) 0.17046(13) 0.0260(5) Uani 1 1 d . . . O6 O -0.12293(18) 0.63773(18) 0.18993(14) 0.0292(6) Uani 1 1 d . . . O7 O -0.52501(16) 0.83810(17) -0.26430(13) 0.0231(5) Uani 1 1 d . . . O8 O -0.29199(15) 0.71725(17) -0.32592(12) 0.0213(5) Uani 1 1 d . . . O9 O -0.19712(16) 0.83564(16) -0.39382(12) 0.0205(5) Uani 1 1 d . . . O10 O -0.67632(17) 0.90300(17) -0.58213(13) 0.0255(5) Uani 1 1 d . . . O11 O -0.46949(17) 0.77355(17) -0.63485(13) 0.0263(6) Uani 1 1 d . . . O12 O -0.36453(17) 0.91271(18) -0.70596(14) 0.0292(6) Uani 1 1 d . . . N25 N 0.0671(2) 0.7195(3) -0.41519(19) 0.0365(8) Uani 1 1 d . . . N26 N -0.5088(2) 0.5534(2) 0.19643(18) 0.0313(7) Uani 1 1 d . . . N27 N -0.9064(3) 0.9353(3) -0.1648(2) 0.0408(9) Uani 1 1 d . . . O13 O 0.0481(3) 0.6705(2) -0.3581(2) 0.0707(11) Uani 1 1 d . . . O14 O 0.0271(2) 0.8091(2) -0.43111(19) 0.0518(8) Uani 1 1 d . . . O15 O 0.1229(3) 0.6786(3) -0.4562(2) 0.0727(12) Uani 1 1 d . . . O16 O -0.5089(2) 0.5067(2) 0.15181(17) 0.0502(8) Uani 1 1 d . . . O17 O -0.4722(2) 0.6089(3) 0.18201(19) 0.0555(9) Uani 1 1 d . . . O18 O -0.5464(2) 0.5447(2) 0.25673(16) 0.0453(7) Uani 1 1 d . . . O19 O -0.8269(2) 0.8702(3) -0.1313(2) 0.0581(9) Uani 1 1 d . . . O20 O -0.9265(3) 0.9444(3) -0.2321(2) 0.0780(12) Uani 1 1 d . . . O21 O -0.9654(2) 0.9928(2) -0.13146(19) 0.0545(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.0324(13) 0.0250(13) 0.0219(13) -0.0048(10) -0.0019(11) -0.0142(11) O2W 0.0258(13) 0.0241(12) 0.0275(14) -0.0053(11) 0.0037(11) -0.0137(10) O3W 0.0230(12) 0.0347(14) 0.0248(13) -0.0097(11) 0.0019(10) -0.0163(11) O4W 0.0235(13) 0.0323(14) 0.0364(15) -0.0103(12) 0.0021(11) -0.0144(11) Eu1 0.02044(10) 0.02207(10) 0.01283(10) -0.00554(7) 0.00141(7) -0.01206(7) C1 0.0270(18) 0.0233(17) 0.0166(18) -0.0075(15) 0.0012(14) -0.0148(15) C2 0.0203(16) 0.0215(17) 0.0134(16) -0.0027(13) -0.0024(13) -0.0116(14) C3 0.0189(16) 0.0216(17) 0.0158(17) -0.0051(14) 0.0008(13) -0.0113(14) C4 0.0236(17) 0.0202(16) 0.0150(17) -0.0014(13) -0.0005(14) -0.0147(14) C5 0.0229(17) 0.0184(16) 0.0147(16) -0.0018(13) 0.0003(13) -0.0117(14) C6 0.0256(17) 0.0223(17) 0.0150(17) -0.0044(14) 0.0039(14) -0.0136(14) C7 0.0149(15) 0.0221(17) 0.0155(17) -0.0034(13) -0.0012(13) -0.0098(13) C8 0.0192(16) 0.0203(16) 0.0183(17) -0.0045(14) 0.0035(14) -0.0098(14) C9 0.0191(16) 0.0238(17) 0.0154(17) -0.0051(14) 0.0022(13) -0.0130(14) C10 0.0191(16) 0.0253(18) 0.0185(18) -0.0083(15) 0.0060(14) -0.0112(14) C11 0.0165(15) 0.0177(16) 0.0159(17) -0.0024(13) 0.0005(13) -0.0077(13) C12 0.0283(18) 0.0299(19) 0.0178(18) -0.0127(15) 0.0070(15) -0.0168(16) C13 0.0193(16) 0.0128(15) 0.0134(16) -0.0020(13) -0.0028(13) -0.0068(13) C14 0.0220(17) 0.0221(17) 0.0131(16) -0.0074(14) 0.0032(13) -0.0102(14) C15 0.0218(16) 0.0214(17) 0.0110(16) -0.0058(13) 0.0018(13) -0.0081(14) C16 0.0235(17) 0.0207(17) 0.0176(18) -0.0106(15) 0.0017(14) -0.0098(14) C17 0.0220(17) 0.0221(17) 0.0137(16) -0.0029(14) -0.0007(13) -0.0120(14) C18 0.0227(17) 0.0261(18) 0.0152(17) -0.0100(14) 0.0013(14) -0.0096(14) C19 0.0266(18) 0.0208(17) 0.030(2) -0.0089(15) -0.0017(15) -0.0116(15) C20 0.033(2) 0.036(2) 0.033(2) -0.0150(18) -0.0039(17) -0.0175(17) C21 0.033(2) 0.032(2) 0.036(2) -0.0100(18) -0.0105(17) -0.0173(17) C22 0.0215(17) 0.0263(18) 0.029(2) -0.0050(16) -0.0018(15) -0.0145(15) C23 0.0211(17) 0.0275(18) 0.0179(17) -0.0035(14) 0.0024(14) -0.0148(15) C24 0.0218(18) 0.037(2) 0.030(2) -0.0027(17) -0.0019(16) -0.0165(16) C25 0.0212(18) 0.0288(19) 0.039(2) -0.0042(17) -0.0005(16) -0.0109(16) C26 0.0181(16) 0.0252(18) 0.0262(19) -0.0067(15) 0.0070(14) -0.0111(14) C27 0.0231(18) 0.0246(18) 0.0264(19) -0.0090(16) 0.0050(15) -0.0068(15) C28 0.046(2) 0.030(2) 0.031(2) -0.0193(18) 0.0104(18) -0.0136(18) C29 0.041(2) 0.034(2) 0.033(2) -0.0232(19) -0.0007(18) -0.0070(18) C30 0.0317(19) 0.0238(18) 0.029(2) -0.0129(16) -0.0004(16) -0.0140(16) C31 0.0180(16) 0.0187(16) 0.0135(16) -0.0014(13) 0.0022(13) -0.0104(13) C32 0.0170(16) 0.0207(16) 0.0157(17) -0.0039(14) -0.0009(13) -0.0092(14) C33 0.0147(15) 0.0209(16) 0.0164(17) -0.0036(14) 0.0000(13) -0.0086(13) C34 0.0180(16) 0.0224(17) 0.0185(18) -0.0078(14) 0.0006(13) -0.0107(14) C35 0.0154(15) 0.0205(16) 0.0130(16) -0.0037(13) 0.0002(13) -0.0067(13) C36 0.0146(15) 0.0232(17) 0.0251(18) -0.0123(15) 0.0000(14) -0.0096(13) C37 0.0166(15) 0.0175(16) 0.0125(16) -0.0027(13) -0.0004(13) -0.0070(13) C38 0.0164(16) 0.0195(16) 0.0158(16) -0.0077(14) 0.0017(13) -0.0079(13) C39 0.0176(16) 0.0192(16) 0.0148(16) -0.0066(13) 0.0025(13) -0.0090(13) C40 0.0220(17) 0.0195(16) 0.0215(18) -0.0140(15) 0.0026(15) -0.0087(14) C41 0.0153(15) 0.0189(16) 0.0143(16) -0.0038(13) 0.0018(13) -0.0078(13) C42 0.0271(18) 0.0250(17) 0.0148(17) -0.0089(14) 0.0022(14) -0.0148(15) C43 0.0143(15) 0.0186(16) 0.0172(17) -0.0053(14) 0.0000(13) -0.0063(13) C44 0.0156(15) 0.0181(16) 0.0147(16) -0.0057(13) 0.0031(13) -0.0068(13) C45 0.0174(16) 0.0185(16) 0.0117(16) -0.0060(13) 0.0021(13) -0.0065(13) C46 0.0199(17) 0.0255(18) 0.0123(16) -0.0063(14) 0.0010(14) -0.0088(14) C47 0.0181(16) 0.0193(16) 0.0179(17) -0.0071(14) -0.0010(13) -0.0084(13) C48 0.0226(17) 0.0154(16) 0.0141(16) -0.0037(13) 0.0019(13) -0.0057(13) C49 0.0181(16) 0.0254(18) 0.0241(19) -0.0059(15) 0.0045(14) -0.0116(14) C50 0.033(2) 0.030(2) 0.028(2) -0.0017(16) 0.0095(17) -0.0157(17) C51 0.031(2) 0.0242(18) 0.029(2) -0.0029(16) 0.0049(16) -0.0134(16) C52 0.0227(17) 0.0206(17) 0.0244(19) -0.0060(15) 0.0018(14) -0.0124(14) C53 0.0273(18) 0.0259(18) 0.0254(19) -0.0109(15) 0.0065(15) -0.0163(15) C54 0.032(2) 0.0208(18) 0.028(2) -0.0015(16) 0.0005(16) -0.0067(16) C55 0.0294(19) 0.0215(18) 0.035(2) -0.0089(16) -0.0010(17) -0.0061(15) C56 0.0229(17) 0.0223(17) 0.0280(19) -0.0128(15) 0.0061(15) -0.0105(15) C57 0.0177(16) 0.0213(17) 0.0176(17) -0.0074(14) 0.0029(13) -0.0035(14) C58 0.0208(17) 0.0327(19) 0.0187(18) -0.0119(16) 0.0059(14) -0.0082(15) C59 0.030(2) 0.036(2) 0.025(2) -0.0102(17) 0.0132(16) -0.0143(17) C60 0.0182(16) 0.0277(18) 0.0198(18) -0.0056(15) 0.0047(14) -0.0122(14) N1 0.0217(14) 0.0226(14) 0.0151(14) -0.0049(12) 0.0012(11) -0.0097(12) N2 0.0197(14) 0.0194(14) 0.0163(14) -0.0021(12) 0.0008(11) -0.0093(12) N3 0.0228(14) 0.0225(14) 0.0142(14) -0.0046(12) -0.0010(11) -0.0109(12) N4 0.0221(14) 0.0234(14) 0.0159(14) -0.0065(12) 0.0020(12) -0.0114(12) N5 0.0221(14) 0.0220(14) 0.0131(14) -0.0058(11) 0.0060(11) -0.0141(12) N6 0.0193(14) 0.0191(14) 0.0171(14) -0.0046(11) 0.0042(11) -0.0112(11) N7 0.0227(14) 0.0212(14) 0.0158(14) -0.0036(12) -0.0002(12) -0.0114(12) N8 0.0243(15) 0.0247(15) 0.0142(14) -0.0058(12) 0.0020(12) -0.0137(12) N9 0.0184(14) 0.0229(14) 0.0130(14) -0.0071(11) 0.0023(11) -0.0118(11) N10 0.0235(14) 0.0260(15) 0.0128(14) -0.0076(12) 0.0018(11) -0.0159(12) N11 0.0265(15) 0.0218(14) 0.0166(14) -0.0060(12) 0.0027(12) -0.0144(12) N12 0.0213(14) 0.0254(15) 0.0113(14) -0.0058(12) 0.0005(11) -0.0112(12) N13 0.0163(13) 0.0201(14) 0.0151(14) -0.0059(11) 0.0007(11) -0.0082(11) N14 0.0146(13) 0.0206(14) 0.0172(14) -0.0049(11) -0.0010(11) -0.0093(11) N15 0.0170(13) 0.0152(13) 0.0175(14) -0.0045(11) 0.0026(11) -0.0072(11) N16 0.0188(14) 0.0196(14) 0.0148(14) -0.0059(12) -0.0012(11) -0.0049(11) N17 0.0185(13) 0.0196(14) 0.0139(14) -0.0065(11) 0.0024(11) -0.0113(11) N18 0.0158(13) 0.0219(14) 0.0149(14) -0.0064(12) 0.0014(11) -0.0104(11) N19 0.0158(13) 0.0228(14) 0.0133(14) -0.0054(11) 0.0013(11) -0.0086(11) N20 0.0185(14) 0.0238(14) 0.0130(14) -0.0036(12) 0.0009(11) -0.0116(12) N21 0.0202(14) 0.0168(13) 0.0116(13) -0.0028(11) 0.0010(11) -0.0089(11) N22 0.0200(14) 0.0171(13) 0.0121(13) -0.0058(11) 0.0020(11) -0.0092(11) N23 0.0182(13) 0.0188(14) 0.0160(14) -0.0046(11) 0.0012(11) -0.0092(11) N24 0.0178(13) 0.0200(14) 0.0114(13) -0.0025(11) -0.0030(11) -0.0080(11) O1 0.0322(13) 0.0238(12) 0.0210(13) -0.0059(11) 0.0062(11) -0.0129(11) O2 0.0314(13) 0.0290(13) 0.0159(12) -0.0076(10) 0.0093(10) -0.0203(11) O3 0.0230(12) 0.0302(13) 0.0121(12) -0.0073(10) 0.0026(9) -0.0153(10) O4 0.0279(13) 0.0287(13) 0.0156(12) -0.0074(10) -0.0033(10) -0.0106(11) O5 0.0305(13) 0.0299(13) 0.0143(13) -0.0029(11) -0.0021(11) -0.0127(11) O6 0.0347(14) 0.0273(13) 0.0200(13) 0.0026(11) -0.0049(11) -0.0141(11) O7 0.0202(12) 0.0269(13) 0.0232(13) -0.0086(11) -0.0005(10) -0.0110(10) O8 0.0225(12) 0.0340(13) 0.0146(12) -0.0119(10) 0.0019(10) -0.0163(11) O9 0.0282(12) 0.0265(12) 0.0098(11) -0.0064(10) 0.0040(9) -0.0146(10) O10 0.0276(13) 0.0250(13) 0.0172(13) -0.0044(10) 0.0025(10) -0.0072(10) O11 0.0255(13) 0.0315(13) 0.0167(13) -0.0030(11) -0.0057(10) -0.0104(11) O12 0.0307(14) 0.0300(13) 0.0252(14) -0.0042(11) -0.0097(11) -0.0140(11) N25 0.0381(19) 0.042(2) 0.0305(19) -0.0131(16) 0.0051(15) -0.0180(17) N26 0.0271(16) 0.0310(17) 0.0261(18) 0.0008(14) -0.0059(14) -0.0098(14) N27 0.058(2) 0.041(2) 0.037(2) -0.0129(17) 0.0147(19) -0.034(2) O13 0.113(3) 0.050(2) 0.061(2) -0.0243(19) 0.050(2) -0.045(2) O14 0.0542(19) 0.0437(19) 0.050(2) -0.0136(16) 0.0034(16) -0.0164(15) O15 0.089(3) 0.062(2) 0.071(3) -0.037(2) 0.055(2) -0.029(2) O16 0.0519(19) 0.058(2) 0.0410(18) -0.0241(16) -0.0090(15) -0.0203(16) O17 0.065(2) 0.063(2) 0.057(2) -0.0091(17) 0.0142(17) -0.0487(19) O18 0.0493(18) 0.0481(18) 0.0293(16) -0.0017(14) 0.0132(14) -0.0199(15) O19 0.055(2) 0.056(2) 0.056(2) -0.0161(18) 0.0002(17) -0.0191(18) O20 0.094(3) 0.078(3) 0.040(2) -0.024(2) -0.001(2) -0.017(2) O21 0.062(2) 0.055(2) 0.049(2) -0.0245(17) 0.0233(17) -0.0248(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1W Eu1 2.418(2) . ? O2W Eu1 2.384(2) . ? O3W Eu1 2.438(2) . ? O4W Eu1 2.368(2) . ? Eu1 O9 2.359(2) . ? Eu1 O3 2.394(2) . ? Eu1 O2 2.413(2) . ? Eu1 O8 2.431(2) . ? C1 O1 1.224(4) . ? C1 N2 1.369(4) . ? C1 N1 1.377(4) . ? C2 N1 1.464(4) . ? C2 N3 1.467(4) . ? C2 C19 1.513(5) . ? C2 C3 1.573(4) . ? C3 N2 1.454(4) . ? C3 N4 1.464(4) . ? C3 C22 1.520(5) . ? C4 O4 1.225(4) . ? C4 N4 1.362(4) . ? C4 N3 1.365(4) . ? C5 N2 1.449(4) . ? C5 N5 1.454(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.444(4) . ? C6 N4 1.447(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.227(4) . ? C7 N6 1.355(4) . ? C7 N5 1.365(4) . ? C8 N7 1.449(4) . ? C8 N5 1.472(4) . ? C8 C23 1.517(5) . ? C8 C9 1.579(4) . ? C9 N6 1.452(4) . ? C9 N8 1.463(4) . ? C9 C26 1.521(4) . ? C10 O5 1.224(4) . ? C10 N8 1.356(4) . ? C10 N7 1.379(4) . ? C11 N9 1.443(4) . ? C11 N6 1.448(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.454(4) . ? C12 N8 1.454(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.237(4) . ? C13 N9 1.350(4) . ? C13 N10 1.359(4) . ? C14 N11 1.452(4) . ? C14 N9 1.458(4) . ? C14 C27 1.533(4) . ? C14 C15 1.564(5) . ? C15 N12 1.454(4) . ? C15 N10 1.465(4) . ? C15 C30 1.529(4) . ? C16 O6 1.217(4) . ? C16 N12 1.361(5) . ? C16 N11 1.380(4) . ? C17 N3 1.446(4) . ? C17 N10 1.455(4) 2_565 ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.445(4) 2_565 ? C18 N12 1.454(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.533(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.535(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.521(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.534(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.535(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.528(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.531(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.532(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.532(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O7 1.230(4) . ? C31 N14 1.360(4) . ? C31 N13 1.366(4) . ? C32 N13 1.455(4) . ? C32 N15 1.463(4) . ? C32 C49 1.528(5) . ? C32 C33 1.570(4) . ? C33 N16 1.456(4) . ? C33 N14 1.469(4) . ? C33 C52 1.524(5) . ? C34 O10 1.219(4) . ? C34 N16 1.364(4) . ? C34 N15 1.373(4) . ? C35 N14 1.450(4) . ? C35 N17 1.454(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N16 1.439(4) . ? C36 N19 1.460(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O8 1.234(4) . ? C37 N17 1.358(4) . ? C37 N18 1.361(4) . ? C38 N19 1.438(4) . ? C38 N17 1.479(4) . ? C38 C53 1.530(5) . ? C38 C39 1.576(4) . ? C39 N20 1.452(4) . ? C39 N18 1.461(4) . ? C39 C56 1.525(4) . ? C40 O11 1.227(4) . ? C40 N20 1.364(4) . ? C40 N19 1.365(4) . ? C41 N18 1.441(4) . ? C41 N21 1.445(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N23 1.444(4) . ? C42 N20 1.444(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 O9 1.238(4) . ? C43 N22 1.339(4) . ? C43 N21 1.354(4) . ? C44 N21 1.463(4) . ? C44 N23 1.463(4) . ? C44 C57 1.524(4) . ? C44 C45 1.582(4) . ? C45 N24 1.457(4) . ? C45 N22 1.475(4) . ? C45 C60 1.513(5) . ? C46 O12 1.222(4) . ? C46 N23 1.362(4) . ? C46 N24 1.382(4) . ? C47 N15 1.444(4) 2_474 ? C47 N22 1.457(4) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 N24 1.449(4) 2_474 ? C48 N13 1.460(4) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.519(5) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.537(5) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.524(5) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.523(5) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.529(5) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.522(5) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C58 1.518(5) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 C59 1.535(5) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 C60 1.535(5) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? N1 C18 1.445(4) 2_565 ? N10 C17 1.455(4) 2_565 ? N15 C47 1.444(4) 2_474 ? N24 C48 1.449(4) 2_474 ? N25 O15 1.218(4) . ? N25 O14 1.229(4) . ? N25 O13 1.250(5) . ? N26 O17 1.237(4) . ? N26 O16 1.238(4) . ? N26 O18 1.247(4) . ? N27 O20 1.227(5) . ? N27 O19 1.249(5) . ? N27 O21 1.259(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 O9 Eu1 O4W 98.07(8) . . ? O9 Eu1 O2W 94.44(8) . . ? O4W Eu1 O2W 139.95(8) . . ? O9 Eu1 O3 138.06(8) . . ? O4W Eu1 O3 96.57(8) . . ? O2W Eu1 O3 99.06(8) . . ? O9 Eu1 O2 146.57(8) . . ? O4W Eu1 O2 75.61(9) . . ? O2W Eu1 O2 73.15(8) . . ? O3 Eu1 O2 75.27(8) . . ? O9 Eu1 O1W 75.52(8) . . ? O4W Eu1 O1W 72.11(8) . . ? O2W Eu1 O1W 147.92(8) . . ? O3 Eu1 O1W 72.05(8) . . ? O2 Eu1 O1W 130.27(8) . . ? O9 Eu1 O8 75.81(8) . . ? O4W Eu1 O8 72.97(8) . . ? O2W Eu1 O8 73.56(8) . . ? O3 Eu1 O8 146.12(8) . . ? O2 Eu1 O8 70.94(8) . . ? O1W Eu1 O8 130.45(8) . . ? O9 Eu1 O3W 75.05(8) . . ? O4W Eu1 O3W 147.95(8) . . ? O2W Eu1 O3W 72.09(8) . . ? O3 Eu1 O3W 71.82(7) . . ? O2 Eu1 O3W 126.70(8) . . ? O1W Eu1 O3W 75.87(8) . . ? O8 Eu1 O3W 132.38(7) . . ? O1 C1 N2 126.6(3) . . ? O1 C1 N1 125.1(3) . . ? N2 C1 N1 108.3(3) . . ? N1 C2 N3 111.5(3) . . ? N1 C2 C19 112.9(3) . . ? N3 C2 C19 113.6(3) . . ? N1 C2 C3 102.5(2) . . ? N3 C2 C3 102.9(2) . . ? C19 C2 C3 112.4(3) . . ? N2 C3 N4 112.5(3) . . ? N2 C3 C22 113.0(3) . . ? N4 C3 C22 112.8(3) . . ? N2 C3 C2 103.3(2) . . ? N4 C3 C2 102.7(2) . . ? C22 C3 C2 111.5(3) . . ? O4 C4 N4 124.8(3) . . ? O4 C4 N3 125.7(3) . . ? N4 C4 N3 109.5(3) . . ? N2 C5 N5 114.4(3) . . ? N2 C5 H5A 108.7 . . ? N5 C5 H5A 108.7 . . ? N2 C5 H5B 108.7 . . ? N5 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N7 C6 N4 114.9(3) . . ? N7 C6 H6A 108.5 . . ? N4 C6 H6A 108.5 . . ? N7 C6 H6B 108.5 . . ? N4 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? O2 C7 N6 125.8(3) . . ? O2 C7 N5 124.7(3) . . ? N6 C7 N5 109.5(3) . . ? N7 C8 N5 112.4(3) . . ? N7 C8 C23 113.7(3) . . ? N5 C8 C23 112.5(3) . . ? N7 C8 C9 102.7(2) . . ? N5 C8 C9 102.7(3) . . ? C23 C8 C9 111.9(3) . . ? N6 C9 N8 113.5(3) . . ? N6 C9 C26 112.3(3) . . ? N8 C9 C26 113.2(3) . . ? N6 C9 C8 102.4(2) . . ? N8 C9 C8 102.6(3) . . ? C26 C9 C8 111.9(3) . . ? O5 C10 N8 126.6(3) . . ? O5 C10 N7 124.9(3) . . ? N8 C10 N7 108.5(3) . . ? N9 C11 N6 114.2(3) . . ? N9 C11 H11A 108.7 . . ? N6 C11 H11A 108.7 . . ? N9 C11 H11B 108.7 . . ? N6 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N11 C12 N8 113.6(3) . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12B 108.8 . . ? N8 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 125.3(3) . . ? O3 C13 N10 124.7(3) . . ? N9 C13 N10 110.0(3) . . ? N11 C14 N9 112.7(3) . . ? N11 C14 C27 112.9(3) . . ? N9 C14 C27 111.7(3) . . ? N11 C14 C15 103.0(3) . . ? N9 C14 C15 103.0(2) . . ? C27 C14 C15 112.9(3) . . ? N12 C15 N10 112.6(2) . . ? N12 C15 C30 113.2(3) . . ? N10 C15 C30 112.5(3) . . ? N12 C15 C14 103.2(3) . . ? N10 C15 C14 102.8(2) . . ? C30 C15 C14 111.7(3) . . ? O6 C16 N12 126.3(3) . . ? O6 C16 N11 125.2(3) . . ? N12 C16 N11 108.4(3) . . ? N3 C17 N10 115.0(3) . 2_565 ? N3 C17 H17A 108.5 . . ? N10 C17 H17A 108.5 2_565 . ? N3 C17 H17B 108.5 . . ? N10 C17 H17B 108.5 2_565 . ? H17A C17 H17B 107.5 . . ? N1 C18 N12 115.4(2) 2_565 . ? N1 C18 H18A 108.4 2_565 . ? N12 C18 H18A 108.4 . . ? N1 C18 H18B 108.4 2_565 . ? N12 C18 H18B 108.4 . . ? H18A C18 H18B 107.5 . . ? C2 C19 C20 111.4(3) . . ? C2 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? C2 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C19 C20 C21 112.5(3) . . ? C19 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C20 112.6(3) . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21B 109.1 . . ? C20 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C3 C22 C21 111.2(3) . . ? C3 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C3 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C8 C23 C24 110.1(3) . . ? C8 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? C8 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C23 C24 C25 111.9(3) . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C24 113.1(3) . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25B 109.0 . . ? C24 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C9 C26 C25 111.4(3) . . ? C9 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C9 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C14 109.0(3) . . ? C28 C27 H27A 109.9 . . ? C14 C27 H27A 109.9 . . ? C28 C27 H27B 109.9 . . ? C14 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? C27 C28 C29 112.1(3) . . ? C27 C28 H28A 109.2 . . ? C29 C28 H28A 109.2 . . ? C27 C28 H28B 109.2 . . ? C29 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C28 C29 C30 113.6(3) . . ? C28 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? C28 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C15 C30 C29 110.8(3) . . ? C15 C30 H30A 109.5 . . ? C29 C30 H30A 109.5 . . ? C15 C30 H30B 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? O7 C31 N14 125.6(3) . . ? O7 C31 N13 125.6(3) . . ? N14 C31 N13 108.8(3) . . ? N13 C32 N15 112.1(3) . . ? N13 C32 C49 113.5(3) . . ? N15 C32 C49 113.0(3) . . ? N13 C32 C33 102.9(2) . . ? N15 C32 C33 102.7(2) . . ? C49 C32 C33 111.7(3) . . ? N16 C33 N14 112.4(3) . . ? N16 C33 C52 112.8(3) . . ? N14 C33 C52 112.9(3) . . ? N16 C33 C32 103.1(2) . . ? N14 C33 C32 102.5(2) . . ? C52 C33 C32 112.4(3) . . ? O10 C34 N16 124.9(3) . . ? O10 C34 N15 126.4(3) . . ? N16 C34 N15 108.8(3) . . ? N14 C35 N17 114.6(3) . . ? N14 C35 H35A 108.6 . . ? N17 C35 H35A 108.6 . . ? N14 C35 H35B 108.6 . . ? N17 C35 H35B 108.6 . . ? H35A C35 H35B 107.6 . . ? N16 C36 N19 113.7(3) . . ? N16 C36 H36A 108.8 . . ? N19 C36 H36A 108.8 . . ? N16 C36 H36B 108.8 . . ? N19 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? O8 C37 N17 124.8(3) . . ? O8 C37 N18 125.3(3) . . ? N17 C37 N18 109.9(3) . . ? N19 C38 N17 112.9(2) . . ? N19 C38 C53 114.0(3) . . ? N17 C38 C53 111.5(3) . . ? N19 C38 C39 102.9(2) . . ? N17 C38 C39 102.6(2) . . ? C53 C38 C39 112.0(2) . . ? N20 C39 N18 113.1(3) . . ? N20 C39 C56 113.4(3) . . ? N18 C39 C56 112.1(3) . . ? N20 C39 C38 102.6(2) . . ? N18 C39 C38 102.7(2) . . ? C56 C39 C38 112.0(3) . . ? O11 C40 N20 125.2(3) . . ? O11 C40 N19 126.2(3) . . ? N20 C40 N19 108.6(3) . . ? N18 C41 N21 114.5(3) . . ? N18 C41 H41A 108.6 . . ? N21 C41 H41A 108.6 . . ? N18 C41 H41B 108.6 . . ? N21 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? N23 C42 N20 114.5(2) . . ? N23 C42 H42A 108.6 . . ? N20 C42 H42A 108.6 . . ? N23 C42 H42B 108.6 . . ? N20 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? O9 C43 N22 125.2(3) . . ? O9 C43 N21 124.3(3) . . ? N22 C43 N21 110.5(3) . . ? N21 C44 N23 112.8(3) . . ? N21 C44 C57 112.6(3) . . ? N23 C44 C57 112.9(2) . . ? N21 C44 C45 102.9(2) . . ? N23 C44 C45 102.6(2) . . ? C57 C44 C45 112.0(3) . . ? N24 C45 N22 112.0(2) . . ? N24 C45 C60 114.0(3) . . ? N22 C45 C60 113.2(3) . . ? N24 C45 C44 102.9(2) . . ? N22 C45 C44 101.6(2) . . ? C60 C45 C44 112.0(2) . . ? O12 C46 N23 126.0(3) . . ? O12 C46 N24 125.0(3) . . ? N23 C46 N24 108.9(3) . . ? N15 C47 N22 114.0(3) 2_474 . ? N15 C47 H47A 108.8 2_474 . ? N22 C47 H47A 108.8 . . ? N15 C47 H47B 108.8 2_474 . ? N22 C47 H47B 108.8 . . ? H47A C47 H47B 107.7 . . ? N24 C48 N13 115.4(3) 2_474 . ? N24 C48 H48A 108.4 2_474 . ? N13 C48 H48A 108.4 . . ? N24 C48 H48B 108.4 2_474 . ? N13 C48 H48B 108.4 . . ? H48A C48 H48B 107.5 . . ? C50 C49 C32 112.5(3) . . ? C50 C49 H49A 109.1 . . ? C32 C49 H49A 109.1 . . ? C50 C49 H49B 109.1 . . ? C32 C49 H49B 109.1 . . ? H49A C49 H49B 107.8 . . ? C49 C50 C51 113.3(3) . . ? C49 C50 H50A 108.9 . . ? C51 C50 H50A 108.9 . . ? C49 C50 H50B 108.9 . . ? C51 C50 H50B 108.9 . . ? H50A C50 H50B 107.7 . . ? C52 C51 C50 111.9(3) . . ? C52 C51 H51A 109.2 . . ? C50 C51 H51A 109.2 . . ? C52 C51 H51B 109.2 . . ? C50 C51 H51B 109.2 . . ? H51A C51 H51B 107.9 . . ? C51 C52 C33 111.0(3) . . ? C51 C52 H52A 109.4 . . ? C33 C52 H52A 109.4 . . ? C51 C52 H52B 109.4 . . ? C33 C52 H52B 109.4 . . ? H52A C52 H52B 108.0 . . ? C54 C53 C38 110.3(3) . . ? C54 C53 H53A 109.6 . . ? C38 C53 H53A 109.6 . . ? C54 C53 H53B 109.6 . . ? C38 C53 H53B 109.6 . . ? H53A C53 H53B 108.1 . . ? C53 C54 C55 112.5(3) . . ? C53 C54 H54A 109.1 . . ? C55 C54 H54A 109.1 . . ? C53 C54 H54B 109.1 . . ? C55 C54 H54B 109.1 . . ? H54A C54 H54B 107.8 . . ? C56 C55 C54 113.3(3) . . ? C56 C55 H55A 108.9 . . ? C54 C55 H55A 108.9 . . ? C56 C55 H55B 108.9 . . ? C54 C55 H55B 108.9 . . ? H55A C55 H55B 107.7 . . ? C55 C56 C39 111.4(3) . . ? C55 C56 H56A 109.4 . . ? C39 C56 H56A 109.4 . . ? C55 C56 H56B 109.4 . . ? C39 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? C58 C57 C44 109.7(3) . . ? C58 C57 H57A 109.7 . . ? C44 C57 H57A 109.7 . . ? C58 C57 H57B 109.7 . . ? C44 C57 H57B 109.7 . . ? H57A C57 H57B 108.2 . . ? C57 C58 C59 112.1(3) . . ? C57 C58 H58A 109.2 . . ? C59 C58 H58A 109.2 . . ? C57 C58 H58B 109.2 . . ? C59 C58 H58B 109.2 . . ? H58A C58 H58B 107.9 . . ? C58 C59 C60 112.7(3) . . ? C58 C59 H59A 109.1 . . ? C60 C59 H59A 109.1 . . ? C58 C59 H59B 109.1 . . ? C60 C59 H59B 109.1 . . ? H59A C59 H59B 107.8 . . ? C45 C60 C59 112.7(3) . . ? C45 C60 H60A 109.0 . . ? C59 C60 H60A 109.0 . . ? C45 C60 H60B 109.0 . . ? C59 C60 H60B 109.0 . . ? H60A C60 H60B 107.8 . . ? C1 N1 C18 120.8(3) . 2_565 ? C1 N1 C2 112.7(3) . . ? C18 N1 C2 125.5(3) 2_565 . ? C1 N2 C5 120.7(3) . . ? C1 N2 C3 112.8(3) . . ? C5 N2 C3 125.4(3) . . ? C4 N3 C17 121.4(3) . . ? C4 N3 C2 112.2(3) . . ? C17 N3 C2 124.4(2) . . ? C4 N4 C6 121.9(3) . . ? C4 N4 C3 112.5(2) . . ? C6 N4 C3 124.6(3) . . ? C7 N5 C5 120.7(3) . . ? C7 N5 C8 111.7(2) . . ? C5 N5 C8 125.2(3) . . ? C7 N6 C11 121.3(3) . . ? C7 N6 C9 113.3(3) . . ? C11 N6 C9 125.4(2) . . ? C10 N7 C6 121.1(3) . . ? C10 N7 C8 112.8(3) . . ? C6 N7 C8 125.9(3) . . ? C10 N8 C12 120.6(3) . . ? C10 N8 C9 112.7(3) . . ? C12 N8 C9 125.6(3) . . ? C13 N9 C11 122.6(3) . . ? C13 N9 C14 112.3(3) . . ? C11 N9 C14 125.1(3) . . ? C13 N10 C17 121.5(3) . 2_565 ? C13 N10 C15 111.7(3) . . ? C17 N10 C15 125.4(3) 2_565 . ? C16 N11 C14 112.5(3) . . ? C16 N11 C12 121.0(3) . . ? C14 N11 C12 125.9(3) . . ? C16 N12 C18 121.0(3) . . ? C16 N12 C15 112.8(3) . . ? C18 N12 C15 125.8(3) . . ? C31 N13 C32 112.9(2) . . ? C31 N13 C48 121.8(3) . . ? C32 N13 C48 125.0(3) . . ? C31 N14 C35 120.5(3) . . ? C31 N14 C33 112.5(2) . . ? C35 N14 C33 125.4(2) . . ? C34 N15 C47 120.1(3) . 2_474 ? C34 N15 C32 112.3(2) . . ? C47 N15 C32 124.4(3) 2_474 . ? C34 N16 C36 121.7(3) . . ? C34 N16 C33 112.7(2) . . ? C36 N16 C33 125.0(3) . . ? C37 N17 C35 120.8(2) . . ? C37 N17 C38 111.8(2) . . ? C35 N17 C38 125.2(3) . . ? C37 N18 C41 122.0(3) . . ? C37 N18 C39 112.6(3) . . ? C41 N18 C39 125.4(2) . . ? C40 N19 C38 113.0(3) . . ? C40 N19 C36 121.4(3) . . ? C38 N19 C36 125.2(3) . . ? C40 N20 C42 121.0(3) . . ? C40 N20 C39 112.4(3) . . ? C42 N20 C39 125.8(3) . . ? C43 N21 C41 123.2(3) . . ? C43 N21 C44 111.9(3) . . ? C41 N21 C44 124.9(2) . . ? C43 N22 C47 121.5(3) . . ? C43 N22 C45 112.6(2) . . ? C47 N22 C45 123.7(3) . . ? C46 N23 C42 121.2(3) . . ? C46 N23 C44 112.8(3) . . ? C42 N23 C44 124.9(3) . . ? C46 N24 C48 121.6(3) . 2_474 ? C46 N24 C45 112.3(3) . . ? C48 N24 C45 125.8(3) 2_474 . ? C7 O2 Eu1 155.4(2) . . ? C13 O3 Eu1 155.2(2) . . ? C37 O8 Eu1 156.3(2) . . ? C43 O9 Eu1 159.0(2) . . ? O15 N25 O14 120.0(4) . . ? O15 N25 O13 120.0(4) . . ? O14 N25 O13 119.9(3) . . ? O17 N26 O16 121.0(4) . . ? O17 N26 O18 119.4(3) . . ? O16 N26 O18 119.7(4) . . ? O20 N27 O19 119.0(4) . . ? O20 N27 O21 119.5(4) . . ? O19 N27 O21 121.5(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.113 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.090 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 114 31 ' ' 2 0.037 0.486 0.656 19 9 ' ' 3 -0.037 0.515 0.344 20 9 ' ' 4 0.276 -0.128 0.278 203 72 ' ' 5 0.350 0.456 0.652 58 21 ' ' 6 0.500 0.000 0.500 107 24 ' ' 7 0.725 0.126 0.722 203 72 ' ' 8 0.654 0.541 0.348 56 21 ' ' _platon_squeeze_details ; ; data_p5 _database_code_depnum_ccdc_archive 'CCDC 881903' #TrackingRef '110419qx-submit-cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H128 Cl2 N25 O43 Pr' _chemical_formula_weight 2099.68 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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m' _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 10.6667(8) _cell_length_b 28.785(2) _cell_length_c 14.6296(11) _cell_angle_alpha 90.00 _cell_angle_beta 110.470(2) _cell_angle_gamma 90.00 _cell_volume 4208.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8822 _exptl_absorpt_correction_T_max 0.9214 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35332 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.10 _reflns_number_total 7611 _reflns_number_gt 4534 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0004(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7611 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1504 _refine_ls_R_factor_gt 0.1109 _refine_ls_wR_factor_ref 0.3602 _refine_ls_wR_factor_gt 0.3278 _refine_ls_goodness_of_fit_ref 1.264 _refine_ls_restrained_S_all 1.264 _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 O3W O 0.0940(7) 0.2500 -0.3050(5) 0.219(7) Uani 1 2 d S . . O1W O 0.9156(4) 0.2500 -0.1740(3) 0.0752(19) Uani 1 2 d S . . O2W O 1.3048(3) 0.3006(2) 0.0734(3) 0.0951(17) Uani 1 1 d . . . Cl1 Cl 1.1769(3) 0.29603(18) -0.1306(2) 0.2140(18) Uani 1 1 d . . . N13 N 0.7630(6) 0.2500 -0.0496(5) 0.0908(12) Uani 1 2 d S . . O9 O 0.8770(5) 0.2500 0.0090(4) 0.0908(12) Uani 1 2 d S . . O10 O 0.7008(4) 0.21344(19) -0.0771(3) 0.0908(12) Uani 1 1 d . . . Pr1 Pr 1.10336(3) 0.2500 -0.01213(3) 0.0912(2) Uani 1 2 d S . . C1 C 1.0336(6) 0.2500 0.1930(4) 0.0587(16) Uani 1 2 d S . . C2 C 0.8772(4) 0.22266(18) 0.2593(3) 0.0475(13) Uani 1 1 d . . . C3 C 0.6690(6) 0.2500 0.1553(4) 0.0587(16) Uani 1 2 d S . . C4 C 1.0222(5) 0.1664(2) 0.1984(3) 0.0726(18) Uani 1 1 d . . . H4A H 1.0312 0.1463 0.2546 0.087 Uiso 1 1 calc R . . H4B H 1.1107 0.1686 0.1925 0.087 Uiso 1 1 calc R . . C5 C 0.6830(4) 0.16569(16) 0.1794(3) 0.0452(13) Uani 1 1 d . . . H5A H 0.7203 0.1482 0.2404 0.054 Uiso 1 1 calc R . . H5B H 0.5868 0.1693 0.1659 0.054 Uiso 1 1 calc R . . C6 C 0.9529(5) 0.1446(2) 0.0271(3) 0.0706(18) Uani 1 1 d . . . C7 C 0.8248(5) 0.1125(2) 0.1111(3) 0.0643(16) Uani 1 1 d . . . C8 C 0.7806(5) 0.0864(2) 0.0075(3) 0.0644(16) Uani 1 1 d . . . C9 C 0.5976(4) 0.12868(17) 0.0185(3) 0.0465(12) Uani 1 1 d . . . C10 C 0.8801(5) 0.1013(3) -0.1296(3) 0.076(2) Uani 1 1 d . . . H10A H 0.9629 0.1149 -0.1323 0.091 Uiso 1 1 calc R . . H10B H 0.8895 0.0674 -0.1303 0.091 Uiso 1 1 calc R . . C11 C 0.5545(5) 0.0750(2) -0.1216(3) 0.0578(15) Uani 1 1 d . . . H11A H 0.4637 0.0747 -0.1195 0.069 Uiso 1 1 calc R . . H11B H 0.5837 0.0426 -0.1202 0.069 Uiso 1 1 calc R . . C12 C 0.7948(4) 0.1435(2) -0.2826(3) 0.0574(15) Uani 1 1 d . . . C13 C 0.6480(4) 0.08730(17) -0.2611(3) 0.0475(13) Uani 1 1 d . . . C14 C 0.5853(4) 0.11179(16) -0.3605(3) 0.0394(12) Uani 1 1 d . . . C15 C 0.4520(4) 0.12707(16) -0.2662(3) 0.0430(12) Uani 1 1 d . . . C16 C 0.6923(4) 0.16517(16) -0.4551(3) 0.0449(12) Uani 1 1 d . . . H16A H 0.6428 0.1466 -0.5126 0.054 Uiso 1 1 calc R . . H16B H 0.7851 0.1673 -0.4526 0.054 Uiso 1 1 calc R . . C17 C 0.3763(4) 0.16575(17) -0.4244(3) 0.0487(14) Uani 1 1 d . . . H17A H 0.2954 0.1691 -0.4079 0.058 Uiso 1 1 calc R . . H17B H 0.3521 0.1485 -0.4859 0.058 Uiso 1 1 calc R . . C18 C 0.7163(5) 0.2500 -0.4492(4) 0.0378(17) Uani 1 2 d S . . C19 C 0.4908(4) 0.22296(17) -0.5075(3) 0.0419(12) Uani 1 1 d . . . C20 C 0.3857(5) 0.2500 -0.4028(4) 0.0385(17) Uani 1 2 d S . . C21 C 1.0395(5) 0.2231(2) 0.4337(4) 0.092(3) Uani 1 1 d . . . H21A H 1.0512 0.2122 0.4996 0.111 Uiso 1 1 calc R . . H21B H 1.1162 0.2122 0.4175 0.111 Uiso 1 1 calc R . . C22 C 0.9100(5) 0.2015(2) 0.3609(3) 0.0669(17) Uani 1 1 d . . . H22A H 0.9216 0.1679 0.3575 0.080 Uiso 1 1 calc R . . H22B H 0.8355 0.2071 0.3840 0.080 Uiso 1 1 calc R . . C23 C 0.8588(6) 0.0771(2) 0.1955(4) 0.0851(19) Uani 1 1 d . . . C24A C 0.7358(9) 0.0325(3) 0.1715(6) 0.047(2) Uani 0.50 1 d P . . H24A H 0.7567 0.0118 0.2279 0.056 Uiso 0.50 1 calc PR . . H24B H 0.6477 0.0463 0.1601 0.056 Uiso 0.50 1 calc PR . . C24 C 1.0006(11) 0.0562(3) 0.1912(7) 0.059(2) Uani 0.50 1 d P . . H24C H 1.0680 0.0809 0.2052 0.070 Uiso 0.50 1 calc PR . . H24D H 1.0343 0.0316 0.2400 0.070 Uiso 0.50 1 calc PR . . C25A C 0.7334(9) 0.0067(3) 0.0875(7) 0.052(3) Uani 0.50 1 d P . . H25A H 0.6402 0.0009 0.0464 0.062 Uiso 0.50 1 calc PR . . H25B H 0.7767 -0.0234 0.1085 0.062 Uiso 0.50 1 calc PR . . C25 C 0.9738(11) 0.0368(3) 0.0896(7) 0.059(2) Uani 0.50 1 d P . . H25C H 1.0101 0.0053 0.0957 0.070 Uiso 0.50 1 calc PR . . H25D H 1.0223 0.0558 0.0573 0.070 Uiso 0.50 1 calc PR . . C26 C 0.8136(5) 0.03521(19) 0.0190(4) 0.0704(17) Uani 1 1 d . . . C27 C 0.6729(5) 0.0377(2) -0.2713(4) 0.0636(17) Uani 1 1 d . . . H27A H 0.7108 0.0237 -0.2064 0.076 Uiso 1 1 calc R . . H27B H 0.7386 0.0344 -0.3038 0.076 Uiso 1 1 calc R . . C28 C 0.5454(6) 0.01196(14) -0.3299(4) 0.0591(15) Uani 1 1 d . . . H28A H 0.5698 -0.0174 -0.3533 0.071 Uiso 1 1 calc R . . H28B H 0.4959 0.0044 -0.2866 0.071 Uiso 1 1 calc R . . C29 C 0.4551(5) 0.03884(18) -0.4159(4) 0.0607(16) Uani 1 1 d . . . H29A H 0.3820 0.0527 -0.3992 0.073 Uiso 1 1 calc R . . H29B H 0.4159 0.0177 -0.4711 0.073 Uiso 1 1 calc R . . C30 C 0.5328(5) 0.07684(17) -0.4448(3) 0.0495(13) Uani 1 1 d . . . H30A H 0.4745 0.0927 -0.5035 0.059 Uiso 1 1 calc R . . H30B H 0.6080 0.0632 -0.4593 0.059 Uiso 1 1 calc R . . C31 C 0.4250(4) 0.2031(2) -0.6077(3) 0.0531(15) Uani 1 1 d . . . H31A H 0.3284 0.2086 -0.6290 0.064 Uiso 1 1 calc R . . H31B H 0.4394 0.1694 -0.6053 0.064 Uiso 1 1 calc R . . C32 C 0.4794(5) 0.22428(19) -0.6817(3) 0.0635(16) Uani 1 1 d . . . H32A H 0.5712 0.2133 -0.6677 0.076 Uiso 1 1 calc R . . H32B H 0.4253 0.2133 -0.7470 0.076 Uiso 1 1 calc R . . N1 N 0.9839(3) 0.21143(17) 0.2187(3) 0.0572(13) Uani 1 1 d . . . N2 N 0.7442(3) 0.21155(13) 0.1933(2) 0.0421(10) Uani 1 1 d . . . N3 N 0.9331(4) 0.14397(18) 0.1121(3) 0.0686(14) Uani 1 1 d . . . N4 N 0.8657(4) 0.11481(16) -0.0373(3) 0.0580(12) Uani 1 1 d . . . N5 N 0.7012(3) 0.13867(14) 0.1016(3) 0.0486(11) Uani 1 1 d . . . N6 N 0.6420(4) 0.09835(15) -0.0355(3) 0.0582(12) Uani 1 1 d . . . N7 N 0.7720(3) 0.11486(14) -0.2150(3) 0.0473(11) Uani 1 1 d . . . N8 N 0.6906(4) 0.14099(14) -0.3691(2) 0.0466(11) Uani 1 1 d . . . N9 N 0.5505(3) 0.09640(14) -0.2146(2) 0.0470(11) Uani 1 1 d . . . N10 N 0.4750(3) 0.13881(12) -0.3478(2) 0.0368(10) Uani 1 1 d . . . N11 N 0.6355(3) 0.21158(13) -0.4676(2) 0.0396(10) Uani 1 1 d . . . N12 N 0.4235(3) 0.21211(14) -0.4390(2) 0.0437(10) Uani 1 1 d . . . O1 O 1.1272(4) 0.2500 0.1588(3) 0.0681(7) Uani 1 2 d S . . O2 O 1.0361(3) 0.17044(15) 0.0056(2) 0.0681(7) Uani 1 1 d . . . O3 O 0.8972(3) 0.16677(15) -0.2690(2) 0.0678(12) Uani 1 1 d . . . O4 O 0.8359(4) 0.2500 -0.4269(3) 0.0565(15) Uani 1 2 d S . . O5 O 0.5521(4) 0.2500 0.1000(3) 0.0681(7) Uani 1 2 d S . . O6 O 0.4833(3) 0.14405(15) -0.0048(2) 0.0681(7) Uani 1 1 d . . . O7 O 0.3609(3) 0.14205(12) -0.2398(2) 0.0546(9) Uani 1 1 d . . . O8 O 0.3217(4) 0.2500 -0.3449(3) 0.0497(13) Uani 1 2 d S . . 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 O3W 0.044(3) 0.57(2) 0.045(3) 0.000 0.021(3) 0.000 O1W 0.021(2) 0.180(5) 0.021(2) 0.000 0.0020(17) 0.000 O2W 0.0177(15) 0.231(5) 0.0361(17) 0.015(2) 0.0093(12) 0.006(2) Cl1 0.137(2) 0.389(5) 0.131(2) 0.016(3) 0.0661(16) -0.022(3) N13 0.0256(14) 0.183(3) 0.0594(17) 0.000 0.0090(12) 0.000 O9 0.0256(14) 0.183(3) 0.0594(17) 0.000 0.0090(12) 0.000 O10 0.0256(14) 0.183(3) 0.0594(17) 0.000 0.0090(12) 0.000 Pr1 0.01511(17) 0.2371(7) 0.02371(17) 0.000 0.00983(13) 0.000 C1 0.0188(19) 0.140(4) 0.0173(18) 0.000 0.0070(15) 0.000 C2 0.0136(16) 0.111(3) 0.0182(17) 0.0072(19) 0.0062(13) 0.017(2) C3 0.0188(19) 0.140(4) 0.0173(18) 0.000 0.0070(15) 0.000 C4 0.021(2) 0.167(5) 0.022(2) -0.024(3) -0.0030(17) 0.027(3) C5 0.0274(18) 0.084(3) 0.0280(19) 0.006(2) 0.0144(14) 0.015(2) C6 0.031(2) 0.150(5) 0.026(2) -0.015(3) 0.0051(18) 0.017(3) C7 0.039(2) 0.130(4) 0.021(2) 0.000(2) 0.0076(17) 0.041(3) C8 0.047(2) 0.121(4) 0.025(2) -0.002(2) 0.0131(18) 0.031(3) C9 0.0317(19) 0.086(3) 0.0273(18) -0.001(2) 0.0175(14) 0.010(2) C10 0.032(2) 0.171(5) 0.024(2) -0.013(3) 0.0094(17) 0.025(3) C11 0.045(2) 0.104(4) 0.026(2) -0.001(2) 0.0151(17) 0.013(3) C12 0.0159(18) 0.121(4) 0.036(2) -0.025(2) 0.0105(15) 0.010(2) C13 0.042(2) 0.077(3) 0.0257(19) -0.0017(19) 0.0150(16) 0.024(2) C14 0.0304(19) 0.065(3) 0.0234(18) 0.0012(18) 0.0105(15) 0.008(2) C15 0.035(2) 0.067(3) 0.0300(19) 0.0026(19) 0.0145(16) 0.003(2) C16 0.0262(18) 0.076(3) 0.038(2) -0.009(2) 0.0176(15) 0.002(2) C17 0.0227(19) 0.097(3) 0.0261(19) 0.002(2) 0.0077(15) 0.008(2) C18 0.007(2) 0.088(4) 0.013(2) 0.000 -0.0036(18) 0.000 C19 0.0174(18) 0.080(3) 0.0268(19) -0.0025(19) 0.0059(14) -0.002(2) C20 0.008(2) 0.087(4) 0.019(2) 0.000 0.0029(18) 0.000 C21 0.017(2) 0.227(7) 0.025(2) 0.000(3) -0.0011(18) 0.023(3) C22 0.042(2) 0.139(4) 0.0206(19) 0.015(2) 0.0124(17) 0.037(3) C23 0.103(4) 0.114(4) 0.031(3) 0.008(3) 0.014(3) 0.071(3) C24A 0.075(4) 0.025(4) 0.062(4) 0.015(3) 0.051(3) 0.001(4) C24 0.071(4) 0.056(4) 0.051(4) 0.013(3) 0.025(3) 0.021(3) C25A 0.052(5) 0.065(6) 0.048(4) 0.010(4) 0.030(3) -0.005(4) C25 0.071(4) 0.056(4) 0.051(4) 0.013(3) 0.025(3) 0.021(3) C26 0.076(3) 0.088(3) 0.051(3) 0.007(2) 0.027(2) 0.049(3) C27 0.049(3) 0.110(4) 0.032(2) 0.008(2) 0.0155(19) 0.016(3) C28 0.108(3) 0.023(2) 0.060(3) 0.0113(18) 0.046(2) 0.015(2) C29 0.056(3) 0.087(4) 0.038(2) -0.005(2) 0.016(2) 0.011(3) C30 0.048(2) 0.079(3) 0.0221(18) -0.002(2) 0.0133(17) 0.011(2) C31 0.018(2) 0.110(4) 0.024(2) -0.011(2) -0.0010(16) 0.002(2) C32 0.047(3) 0.129(4) 0.0140(18) -0.012(2) 0.0098(17) 0.000(3) N1 0.0166(16) 0.133(3) 0.0189(16) -0.006(2) 0.0022(13) 0.017(2) N2 0.0187(15) 0.076(2) 0.0311(17) 0.0102(17) 0.0079(13) 0.0117(17) N3 0.0262(18) 0.150(4) 0.0289(18) -0.016(2) 0.0094(14) 0.021(2) N4 0.0420(19) 0.111(3) 0.0212(16) -0.0071(19) 0.0114(14) 0.026(2) N5 0.0272(16) 0.084(3) 0.0376(18) 0.0037(18) 0.0147(13) 0.0216(18) N6 0.0366(18) 0.110(3) 0.0251(17) -0.0068(19) 0.0077(14) 0.032(2) N7 0.0237(16) 0.089(3) 0.0285(16) -0.0007(18) 0.0082(13) 0.0179(18) N8 0.0321(18) 0.086(3) 0.0214(16) -0.0078(17) 0.0090(13) 0.0019(19) N9 0.0245(15) 0.090(3) 0.0286(16) 0.0059(17) 0.0121(13) 0.0240(17) N10 0.0231(16) 0.056(2) 0.0290(16) -0.0060(15) 0.0059(13) 0.0104(15) N11 0.0180(15) 0.070(2) 0.0295(16) -0.0102(16) 0.0063(12) -0.0008(16) N12 0.0249(15) 0.080(3) 0.0318(16) 0.0011(17) 0.0170(12) -0.0044(17) O1 0.0144(8) 0.1543(19) 0.0341(9) 0.000 0.0067(7) 0.000 O2 0.0144(8) 0.1543(19) 0.0341(9) 0.000 0.0067(7) 0.000 O3 0.0249(14) 0.149(3) 0.0329(15) -0.0196(18) 0.0140(11) -0.0036(19) O4 0.0141(19) 0.124(4) 0.028(2) 0.000 0.0021(16) 0.000 O5 0.0144(8) 0.1543(19) 0.0341(9) 0.000 0.0067(7) 0.000 O6 0.0144(8) 0.1543(19) 0.0341(9) 0.000 0.0067(7) 0.000 O7 0.0359(14) 0.086(2) 0.0490(16) 0.0106(15) 0.0240(12) 0.0199(15) O8 0.0267(19) 0.097(3) 0.0272(19) 0.000 0.0113(15) 0.000 _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 O1W Pr1 2.510(4) . ? O2W Pr1 2.535(4) . ? Cl1 Pr1 2.515(4) . ? N13 O9 1.218(8) . ? N13 O10 1.234(6) . ? N13 O10 1.234(6) 4_565 ? O9 Pr1 2.539(6) . ? Pr1 O1 2.423(5) . ? Pr1 O2 2.441(4) . ? Pr1 O2 2.441(4) 4_565 ? Pr1 Cl1 2.515(4) 4_565 ? Pr1 O2W 2.535(4) 4_565 ? C1 O1 1.263(8) . ? C1 N1 1.340(6) . ? C1 N1 1.340(6) 4_565 ? C2 N2 1.445(5) . ? C2 N1 1.492(6) . ? C2 C22 1.529(6) . ? C2 C2 1.574(10) 4_565 ? C3 O5 1.226(7) . ? C3 N2 1.365(5) 4_565 ? C3 N2 1.365(5) . ? C4 N1 1.422(7) . ? C4 N3 1.441(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 N5 1.446(6) . ? C5 N2 1.455(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 O2 1.279(7) . ? C6 N3 1.332(7) . ? C6 N4 1.369(7) . ? C7 N3 1.465(7) . ? C7 N5 1.482(6) . ? C7 C23 1.543(8) . ? C7 C8 1.608(7) . ? C8 N6 1.432(6) . ? C8 C26 1.509(8) . ? C8 N4 1.529(7) . ? C9 O6 1.228(5) . ? C9 N5 1.358(5) . ? C9 N6 1.369(6) . ? C10 N7 1.427(5) . ? C10 N4 1.464(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 N6 1.445(6) . ? C11 N9 1.481(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 O3 1.237(6) . ? C12 N8 1.363(5) . ? C12 N7 1.372(7) . ? C13 N9 1.452(6) . ? C13 C27 1.470(7) . ? C13 N7 1.486(6) . ? C13 C14 1.542(6) . ? C14 N8 1.443(6) . ? C14 N10 1.475(6) . ? C14 C30 1.537(6) . ? C15 O7 1.242(6) . ? C15 N10 1.344(6) . ? C15 N9 1.378(5) . ? C16 N8 1.444(6) . ? C16 N11 1.452(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 N10 1.463(5) . ? C17 N12 1.467(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 O4 1.202(7) . ? C18 N11 1.369(5) . ? C18 N11 1.369(5) 4_565 ? C19 N12 1.456(6) . ? C19 N11 1.483(5) . ? C19 C31 1.500(6) . ? C19 C19 1.556(10) 4_565 ? C20 O8 1.258(7) . ? C20 N12 1.335(5) . ? C20 N12 1.335(5) 4_565 ? C21 C21 1.546(14) 4_565 ? C21 C22 1.549(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.649(13) . ? C23 C24A 1.780(11) . ? C24A C25A 1.428(13) . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24 C25 1.518(14) . ? C24 H24C 0.9800 . ? C24 H24D 0.9800 . ? C25A C26 1.735(12) . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25 C26 1.659(11) . ? C25 H25C 0.9800 . ? C25 H25D 0.9800 . ? C27 C28 1.522(7) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.504(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.519(8) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 C32 1.524(7) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C32 C32 1.481(11) 4_565 ? C32 H32A 0.9800 . ? C32 H32B 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 O9 N13 O10 121.3(3) . . ? O9 N13 O10 121.3(3) . 4_565 ? O10 N13 O10 117.0(6) . 4_565 ? N13 O9 Pr1 132.2(5) . . ? O1 Pr1 O2 79.56(8) . . ? O1 Pr1 O2 79.56(8) . 4_565 ? O2 Pr1 O2 139.54(17) . 4_565 ? O1 Pr1 O1W 137.27(16) . . ? O2 Pr1 O1W 86.17(8) . . ? O2 Pr1 O1W 86.17(8) 4_565 . ? O1 Pr1 Cl1 139.95(11) . 4_565 ? O2 Pr1 Cl1 75.71(14) . 4_565 ? O2 Pr1 Cl1 137.89(14) 4_565 4_565 ? O1W Pr1 Cl1 71.84(12) . 4_565 ? O1 Pr1 Cl1 139.95(11) . . ? O2 Pr1 Cl1 137.89(14) . . ? O2 Pr1 Cl1 75.71(14) 4_565 . ? O1W Pr1 Cl1 71.84(12) . . ? Cl1 Pr1 Cl1 63.6(2) 4_565 . ? O1 Pr1 O2W 74.07(12) . . ? O2 Pr1 O2W 135.79(13) . . ? O2 Pr1 O2W 68.77(13) 4_565 . ? O1W Pr1 O2W 136.44(12) . . ? Cl1 Pr1 O2W 103.19(13) 4_565 . ? Cl1 Pr1 O2W 67.82(12) . . ? O1 Pr1 O2W 74.07(12) . 4_565 ? O2 Pr1 O2W 68.77(13) . 4_565 ? O2 Pr1 O2W 135.79(13) 4_565 4_565 ? O1W Pr1 O2W 136.44(12) . 4_565 ? Cl1 Pr1 O2W 67.82(12) 4_565 4_565 ? Cl1 Pr1 O2W 103.19(13) . 4_565 ? O2W Pr1 O2W 70.2(2) . 4_565 ? O1 Pr1 O9 68.63(16) . . ? O2 Pr1 O9 70.10(8) . . ? O2 Pr1 O9 70.10(8) 4_565 . ? O1W Pr1 O9 68.64(17) . . ? Cl1 Pr1 O9 128.53(12) 4_565 . ? Cl1 Pr1 O9 128.53(12) . . ? O2W Pr1 O9 128.16(13) . . ? O2W Pr1 O9 128.16(13) 4_565 . ? O1 C1 N1 123.8(3) . . ? O1 C1 N1 123.8(3) . 4_565 ? N1 C1 N1 112.0(6) . 4_565 ? N2 C2 N1 113.2(3) . . ? N2 C2 C22 113.5(4) . . ? N1 C2 C22 110.7(4) . . ? N2 C2 C2 102.8(2) . 4_565 ? N1 C2 C2 102.5(3) . 4_565 ? C22 C2 C2 113.4(3) . 4_565 ? O5 C3 N2 125.8(2) . 4_565 ? O5 C3 N2 125.8(2) . . ? N2 C3 N2 108.3(5) 4_565 . ? N1 C4 N3 116.2(4) . . ? N1 C4 H4A 108.2 . . ? N3 C4 H4A 108.2 . . ? N1 C4 H4B 108.2 . . ? N3 C4 H4B 108.2 . . ? H4A C4 H4B 107.4 . . ? N5 C5 N2 114.9(4) . . ? N5 C5 H5A 108.5 . . ? N2 C5 H5A 108.5 . . ? N5 C5 H5B 108.5 . . ? N2 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? O2 C6 N3 125.9(5) . . ? O2 C6 N4 124.0(5) . . ? N3 C6 N4 110.1(5) . . ? N3 C7 N5 111.0(5) . . ? N3 C7 C23 115.9(4) . . ? N5 C7 C23 111.3(4) . . ? N3 C7 C8 105.6(4) . . ? N5 C7 C8 101.1(3) . . ? C23 C7 C8 110.8(5) . . ? N6 C8 C26 116.7(5) . . ? N6 C8 N4 111.0(4) . . ? C26 C8 N4 114.8(4) . . ? N6 C8 C7 102.6(4) . . ? C26 C8 C7 111.8(4) . . ? N4 C8 C7 97.6(4) . . ? O6 C9 N5 126.2(4) . . ? O6 C9 N6 125.4(4) . . ? N5 C9 N6 108.3(4) . . ? N7 C10 N4 114.9(4) . . ? N7 C10 H10A 108.5 . . ? N4 C10 H10A 108.5 . . ? N7 C10 H10B 108.5 . . ? N4 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? N6 C11 N9 114.2(4) . . ? N6 C11 H11A 108.7 . . ? N9 C11 H11A 108.7 . . ? N6 C11 H11B 108.7 . . ? N9 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? O3 C12 N8 124.4(5) . . ? O3 C12 N7 125.4(4) . . ? N8 C12 N7 110.2(4) . . ? N9 C13 C27 114.0(4) . . ? N9 C13 N7 111.2(4) . . ? C27 C13 N7 113.6(4) . . ? N9 C13 C14 102.4(3) . . ? C27 C13 C14 112.5(4) . . ? N7 C13 C14 102.0(4) . . ? N8 C14 N10 112.5(4) . . ? N8 C14 C30 112.8(4) . . ? N10 C14 C30 111.3(3) . . ? N8 C14 C13 104.7(3) . . ? N10 C14 C13 102.9(3) . . ? C30 C14 C13 111.9(4) . . ? O7 C15 N10 126.5(4) . . ? O7 C15 N9 125.6(4) . . ? N10 C15 N9 107.9(4) . . ? N8 C16 N11 114.9(4) . . ? N8 C16 H16A 108.5 . . ? N11 C16 H16A 108.5 . . ? N8 C16 H16B 108.5 . . ? N11 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? N10 C17 N12 113.7(3) . . ? N10 C17 H17A 108.8 . . ? N12 C17 H17A 108.8 . . ? N10 C17 H17B 108.8 . . ? N12 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? O4 C18 N11 126.1(2) . . ? O4 C18 N11 126.1(2) . 4_565 ? N11 C18 N11 107.7(4) . 4_565 ? N12 C19 N11 112.2(3) . . ? N12 C19 C31 114.6(4) . . ? N11 C19 C31 111.5(4) . . ? N12 C19 C19 102.4(2) . 4_565 ? N11 C19 C19 102.8(2) . 4_565 ? C31 C19 C19 112.4(3) . 4_565 ? O8 C20 N12 125.2(3) . . ? O8 C20 N12 125.2(3) . 4_565 ? N12 C20 N12 109.5(5) . 4_565 ? C21 C21 C22 113.7(3) 4_565 . ? C21 C21 H21A 108.8 4_565 . ? C22 C21 H21A 108.8 . . ? C21 C21 H21B 108.8 4_565 . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C2 C22 C21 110.8(5) . . ? C2 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? C2 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C7 C23 C24 99.9(6) . . ? C7 C23 C24A 111.5(4) . . ? C24 C23 C24A 110.6(6) . . ? C25A C24A C23 109.5(7) . . ? C25A C24A H24A 109.8 . . ? C23 C24A H24A 109.8 . . ? C25A C24A H24B 109.8 . . ? C23 C24A H24B 109.8 . . ? H24A C24A H24B 108.2 . . ? C25 C24 C23 108.0(7) . . ? C25 C24 H24C 110.1 . . ? C23 C24 H24C 110.1 . . ? C25 C24 H24D 110.1 . . ? C23 C24 H24D 110.1 . . ? H24C C24 H24D 108.4 . . ? C24A C25A C26 112.8(7) . . ? C24A C25A H25A 109.0 . . ? C26 C25A H25A 109.0 . . ? C24A C25A H25B 109.0 . . ? C26 C25A H25B 109.0 . . ? H25A C25A H25B 107.8 . . ? C24 C25 C26 114.9(8) . . ? C24 C25 H25C 108.5 . . ? C26 C25 H25C 108.5 . . ? C24 C25 H25D 108.5 . . ? C26 C25 H25D 108.5 . . ? H25C C25 H25D 107.5 . . ? C8 C26 C25 101.0(5) . . ? C8 C26 C25A 112.4(5) . . ? C25 C26 C25A 105.2(6) . . ? C13 C27 C28 111.9(4) . . ? C13 C27 H27A 109.2 . . ? C28 C27 H27A 109.2 . . ? C13 C27 H27B 109.2 . . ? C28 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C29 C28 C27 113.9(4) . . ? C29 C28 H28A 108.8 . . ? C27 C28 H28A 108.8 . . ? C29 C28 H28B 108.8 . . ? C27 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C28 C29 C30 110.6(4) . . ? C28 C29 H29A 109.5 . . ? C30 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? C29 C30 C14 109.2(4) . . ? C29 C30 H30A 109.8 . . ? C14 C30 H30A 109.8 . . ? C29 C30 H30B 109.8 . . ? C14 C30 H30B 109.8 . . ? H30A C30 H30B 108.3 . . ? C19 C31 C32 112.2(4) . . ? C19 C31 H31A 109.2 . . ? C32 C31 H31A 109.2 . . ? C19 C31 H31B 109.2 . . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C32 C32 C31 113.6(3) 4_565 . ? C32 C32 H32A 108.8 4_565 . ? C31 C32 H32A 108.8 . . ? C32 C32 H32B 108.8 4_565 . ? C31 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? C1 N1 C4 121.8(4) . . ? C1 N1 C2 111.3(4) . . ? C4 N1 C2 126.5(4) . . ? C3 N2 C2 113.1(4) . . ? C3 N2 C5 120.5(3) . . ? C2 N2 C5 125.6(3) . . ? C6 N3 C4 122.8(5) . . ? C6 N3 C7 112.4(4) . . ? C4 N3 C7 124.2(4) . . ? C6 N4 C10 122.4(5) . . ? C6 N4 C8 113.7(4) . . ? C10 N4 C8 121.4(4) . . ? C9 N5 C5 121.8(4) . . ? C9 N5 C7 113.2(4) . . ? C5 N5 C7 124.0(3) . . ? C9 N6 C8 114.4(4) . . ? C9 N6 C11 123.5(4) . . ? C8 N6 C11 121.6(4) . . ? C12 N7 C10 120.2(4) . . ? C12 N7 C13 110.3(3) . . ? C10 N7 C13 124.7(4) . . ? C12 N8 C14 110.9(4) . . ? C12 N8 C16 121.9(4) . . ? C14 N8 C16 127.2(3) . . ? C15 N9 C13 113.1(4) . . ? C15 N9 C11 122.8(4) . . ? C13 N9 C11 124.1(4) . . ? C15 N10 C17 120.5(4) . . ? C15 N10 C14 112.4(3) . . ? C17 N10 C14 125.0(4) . . ? C18 N11 C16 120.8(3) . . ? C18 N11 C19 113.3(4) . . ? C16 N11 C19 125.7(3) . . ? C20 N12 C19 112.8(4) . . ? C20 N12 C17 121.2(4) . . ? C19 N12 C17 124.8(4) . . ? C1 O1 Pr1 126.6(4) . . ? C6 O2 Pr1 145.8(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.123 _refine_diff_density_min -2.984 _refine_diff_density_rms 0.163 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.027 0.000 0.500 528 234 ' ' 2 -0.040 0.500 0.500 528 235 ' ' 3 0.437 0.250 0.869 12 9 ' ' 4 0.562 0.750 0.131 12 9 ' ' _platon_squeeze_details ; ; data_p6 _database_code_depnum_ccdc_archive 'CCDC 881904' #TrackingRef '110510qx-submit-cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H104 Ho N27 O37' _chemical_formula_weight 1960.63 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.8450(7) _cell_length_b 15.9385(7) _cell_length_c 18.1401(8) _cell_angle_alpha 74.731(2) _cell_angle_beta 89.311(2) _cell_angle_gamma 63.456(2) _cell_volume 3923.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 1.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7593 _exptl_absorpt_correction_T_max 0.8237 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40293 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13635 _reflns_number_gt 11861 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+4.2238P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13635 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 O1W O 0.2581(2) 0.9484(2) -0.28531(16) 0.0254(6) Uani 1 1 d . . . O2W O 0.3949(2) 0.6206(2) -0.24588(17) 0.0250(6) Uani 1 1 d . . . O3W O 0.4400(2) 0.7748(2) -0.26600(17) 0.0266(7) Uani 1 1 d . . . O4W O 0.1233(2) 0.8826(2) -0.27385(18) 0.0292(7) Uani 1 1 d . . . Ho1 Ho 0.285241(13) 0.784303(13) -0.263644(10) 0.01968(8) Uani 1 1 d . . . C1 C 0.1985(3) 0.6696(3) -0.1104(2) 0.0157(8) Uani 1 1 d . . . C2 C 0.1394(3) 0.5884(3) -0.0136(2) 0.0187(8) Uani 1 1 d . . . C3 C 0.1232(3) 0.6871(3) 0.0004(2) 0.0185(8) Uani 1 1 d . . . C4 C 0.2202(3) 0.5558(3) 0.1064(2) 0.0216(9) Uani 1 1 d . . . C5 C 0.1543(3) 0.8257(3) -0.0834(2) 0.0179(8) Uani 1 1 d . . . H5A H 0.0966 0.8697 -0.0662 0.021 Uiso 1 1 calc R . . H5B H 0.1494 0.8518 -0.1393 0.021 Uiso 1 1 calc R . . C6 C 0.1905(3) 0.7164(3) 0.1150(2) 0.0220(9) Uani 1 1 d . . . H6A H 0.2077 0.6801 0.1698 0.026 Uiso 1 1 calc R . . H6B H 0.1280 0.7731 0.1092 0.026 Uiso 1 1 calc R . . C7 C 0.3125(3) 0.8164(3) -0.0831(2) 0.0157(8) Uani 1 1 d . . . C8 C 0.2416(3) 0.8388(3) 0.0286(2) 0.0185(8) Uani 1 1 d . . . C9 C 0.3376(3) 0.8439(3) 0.0336(2) 0.0194(8) Uani 1 1 d . . . C10 C 0.3468(3) 0.7103(3) 0.1324(2) 0.0209(9) Uani 1 1 d . . . C11 C 0.4544(3) 0.8378(3) -0.0675(2) 0.0191(8) Uani 1 1 d . . . H11A H 0.4477 0.8492 -0.1234 0.023 Uiso 1 1 calc R . . H11B H 0.4515 0.8967 -0.0580 0.023 Uiso 1 1 calc R . . C12 C 0.4822(3) 0.7448(3) 0.1390(2) 0.0228(9) Uani 1 1 d . . . H12A H 0.4787 0.8075 0.1397 0.027 Uiso 1 1 calc R . . H12B H 0.4902 0.7059 0.1925 0.027 Uiso 1 1 calc R . . C13 C 0.6037(3) 0.7011(3) -0.0785(2) 0.0199(9) Uani 1 1 d . . . C14 C 0.5987(3) 0.7409(3) 0.0375(2) 0.0193(8) Uani 1 1 d . . . C15 C 0.7002(3) 0.6577(3) 0.0359(2) 0.0194(8) Uani 1 1 d . . . C16 C 0.6306(3) 0.5999(3) 0.1394(2) 0.0188(8) Uani 1 1 d . . . C17 C 0.7720(3) 0.5881(3) -0.0757(2) 0.0211(9) Uani 1 1 d . . . H17A H 0.7553 0.6155 -0.1317 0.025 Uiso 1 1 calc R . . H17B H 0.8263 0.5972 -0.0620 0.025 Uiso 1 1 calc R . . C18 C 0.7917(3) 0.4812(3) 0.1273(2) 0.0181(8) Uani 1 1 d . . . H18A H 0.8469 0.4934 0.1290 0.022 Uiso 1 1 calc R . . H18B H 0.7864 0.4497 0.1802 0.022 Uiso 1 1 calc R . . C19 C 0.0466(3) 0.5859(3) -0.0281(2) 0.0226(9) Uani 1 1 d . . . H19A H 0.0173 0.5811 0.0196 0.027 Uiso 1 1 calc R . . H19B H 0.0590 0.5283 -0.0449 0.027 Uiso 1 1 calc R . . C20 C -0.0211(3) 0.6789(3) -0.0901(3) 0.0284(10) Uani 1 1 d . . . H20A H -0.0804 0.6759 -0.0993 0.034 Uiso 1 1 calc R . . H20B H 0.0076 0.6816 -0.1383 0.034 Uiso 1 1 calc R . . C21 C -0.0440(3) 0.7726(3) -0.0676(3) 0.0309(10) Uani 1 1 d . . . H21A H -0.0357 0.8194 -0.1106 0.037 Uiso 1 1 calc R . . H21B H -0.1107 0.8024 -0.0583 0.037 Uiso 1 1 calc R . . C22 C 0.0192(3) 0.7530(3) 0.0044(3) 0.0254(9) Uani 1 1 d . . . H22A H 0.0122 0.8154 0.0096 0.030 Uiso 1 1 calc R . . H22B H -0.0015 0.7220 0.0500 0.030 Uiso 1 1 calc R . . C23 C 0.1562(3) 0.9307(3) 0.0367(3) 0.0266(9) Uani 1 1 d . . . H23A H 0.0998 0.9200 0.0406 0.032 Uiso 1 1 calc R . . H23B H 0.1433 0.9860 -0.0088 0.032 Uiso 1 1 calc R . . C24 C 0.1771(4) 0.9540(4) 0.1089(3) 0.0413(12) Uani 1 1 d . . . H24A H 0.1227 1.0137 0.1133 0.050 Uiso 1 1 calc R . . H24B H 0.1855 0.9004 0.1544 0.050 Uiso 1 1 calc R . . C25 C 0.2658(4) 0.9684(4) 0.1070(3) 0.0473(14) Uani 1 1 d . . . H25A H 0.3077 0.9269 0.1553 0.057 Uiso 1 1 calc R . . H25B H 0.2472 1.0367 0.1044 0.057 Uiso 1 1 calc R . . C26 C 0.3213(3) 0.9442(3) 0.0396(3) 0.0291(10) Uani 1 1 d . . . H26A H 0.3828 0.9436 0.0471 0.035 Uiso 1 1 calc R . . H26B H 0.2859 0.9948 -0.0083 0.035 Uiso 1 1 calc R . . C27 C 0.6018(3) 0.8318(3) 0.0451(3) 0.0273(10) Uani 1 1 d . . . H27A H 0.5380 0.8797 0.0504 0.033 Uiso 1 1 calc R . . H27B H 0.6220 0.8614 -0.0016 0.033 Uiso 1 1 calc R . . C28 C 0.6702(3) 0.8074(3) 0.1146(3) 0.0351(11) Uani 1 1 d . . . H28A H 0.6429 0.7905 0.1616 0.042 Uiso 1 1 calc R . . H28B H 0.6773 0.8656 0.1139 0.042 Uiso 1 1 calc R . . C29 C 0.7683(3) 0.7227(4) 0.1172(3) 0.0359(11) Uani 1 1 d . . . H29A H 0.8167 0.7443 0.1209 0.043 Uiso 1 1 calc R . . H29B H 0.7801 0.6686 0.1635 0.043 Uiso 1 1 calc R . . C30 C 0.7778(3) 0.6859(3) 0.0465(3) 0.0261(10) Uani 1 1 d . . . H30A H 0.7738 0.7372 0.0007 0.031 Uiso 1 1 calc R . . H30B H 0.8401 0.6289 0.0525 0.031 Uiso 1 1 calc R . . C31 C -0.0723(3) 0.8290(3) -0.3107(2) 0.0155(8) Uani 1 1 d . . . C32 C -0.2073(3) 0.8564(3) -0.3856(2) 0.0163(8) Uani 1 1 d . . . C33 C -0.1201(3) 0.7581(3) -0.3900(2) 0.0155(8) Uani 1 1 d . . . C34 C -0.1722(3) 0.8699(3) -0.5129(2) 0.0180(8) Uani 1 1 d . . . C35 C 0.0523(3) 0.6743(3) -0.3235(2) 0.0185(8) Uani 1 1 d . . . H35A H 0.0470 0.6133 -0.3088 0.022 Uiso 1 1 calc R . . H35B H 0.0818 0.6781 -0.2781 0.022 Uiso 1 1 calc R . . C36 C -0.0527(3) 0.7033(3) -0.5077(2) 0.0195(8) Uani 1 1 d . . . H36A H -0.0534 0.6415 -0.4814 0.023 Uiso 1 1 calc R . . H36B H -0.0810 0.7235 -0.5611 0.023 Uiso 1 1 calc R . . C37 C 0.1916(3) 0.6851(3) -0.3757(2) 0.0161(8) Uani 1 1 d . . . C38 C 0.1199(3) 0.6232(3) -0.4444(2) 0.0149(8) Uani 1 1 d . . . C39 C 0.2109(3) 0.6216(3) -0.4809(2) 0.0160(8) Uani 1 1 d . . . C40 C 0.0764(3) 0.7226(3) -0.5727(2) 0.0206(9) Uani 1 1 d . . . C41 C 0.3369(3) 0.6627(3) -0.4346(2) 0.0152(8) Uani 1 1 d . . . H41A H 0.3821 0.6087 -0.4530 0.018 Uiso 1 1 calc R . . H41B H 0.3633 0.6535 -0.3828 0.018 Uiso 1 1 calc R . . C42 C 0.2257(3) 0.7135(3) -0.6168(2) 0.0204(9) Uani 1 1 d . . . H42A H 0.1887 0.7342 -0.6668 0.025 Uiso 1 1 calc R . . H42B H 0.2844 0.6538 -0.6144 0.025 Uiso 1 1 calc R . . C43 C 0.3110(3) 0.8321(3) -0.4599(2) 0.0160(8) Uani 1 1 d . . . C44 C 0.3349(3) 0.7730(3) -0.5671(2) 0.0164(8) Uani 1 1 d . . . C45 C 0.3301(3) 0.8769(3) -0.5901(2) 0.0167(8) Uani 1 1 d . . . C46 C 0.2037(3) 0.8824(3) -0.6610(2) 0.0182(8) Uani 1 1 d . . . C47 C 0.3124(3) 0.9892(3) -0.5049(2) 0.0177(8) Uani 1 1 d . . . H47A H 0.3661 0.9958 -0.5282 0.021 Uiso 1 1 calc R . . H47B H 0.3243 0.9773 -0.4493 0.021 Uiso 1 1 calc R . . C48 C -0.2224(3) 0.9676(3) -0.3000(2) 0.0190(8) Uani 1 1 d . . . H48A H -0.1854 0.9575 -0.2527 0.023 Uiso 1 1 calc R . . H48B H -0.2805 0.9634 -0.2856 0.023 Uiso 1 1 calc R . . C49 C -0.2909(3) 0.8395(3) -0.3582(2) 0.0230(9) Uani 1 1 d . . . H49A H -0.3156 0.8211 -0.3972 0.028 Uiso 1 1 calc R . . H49B H -0.3416 0.9009 -0.3526 0.028 Uiso 1 1 calc R . . C50 C -0.2645(3) 0.7600(3) -0.2818(3) 0.0328(11) Uani 1 1 d . . . H50A H -0.3161 0.7419 -0.2728 0.039 Uiso 1 1 calc R . . H50B H -0.2581 0.7862 -0.2402 0.039 Uiso 1 1 calc R . . C51 C -0.1715(3) 0.6678(3) -0.2789(3) 0.0280(10) Uani 1 1 d . . . H51A H -0.1225 0.6625 -0.2430 0.034 Uiso 1 1 calc R . . H51B H -0.1815 0.6099 -0.2595 0.034 Uiso 1 1 calc R . . C52 C -0.1373(3) 0.6700(3) -0.3576(2) 0.0216(9) Uani 1 1 d . . . H52A H -0.0782 0.6100 -0.3533 0.026 Uiso 1 1 calc R . . H52B H -0.1849 0.6720 -0.3929 0.026 Uiso 1 1 calc R . . C53 C 0.1281(3) 0.5213(3) -0.4134(2) 0.0232(9) Uani 1 1 d . . . H53A H 0.1247 0.4959 -0.4564 0.028 Uiso 1 1 calc R . . H53B H 0.0751 0.5243 -0.3840 0.028 Uiso 1 1 calc R . . C54 C 0.2221(3) 0.4528(3) -0.3617(3) 0.0312(10) Uani 1 1 d . . . H54A H 0.2262 0.3874 -0.3422 0.037 Uiso 1 1 calc R . . H54B H 0.2232 0.4767 -0.3173 0.037 Uiso 1 1 calc R . . C55 C 0.3088(3) 0.4449(3) -0.4034(3) 0.0300(10) Uani 1 1 d . . . H55A H 0.3437 0.3785 -0.4086 0.036 Uiso 1 1 calc R . . H55B H 0.3513 0.4554 -0.3722 0.036 Uiso 1 1 calc R . . C56 C 0.2815(3) 0.5196(3) -0.4839(2) 0.0238(9) Uani 1 1 d . . . H56A H 0.3388 0.5211 -0.5037 0.029 Uiso 1 1 calc R . . H56B H 0.2534 0.4992 -0.5192 0.029 Uiso 1 1 calc R . . C57 C 0.4258(3) 0.6964(3) -0.5859(2) 0.0224(9) Uani 1 1 d . . . H57A H 0.4799 0.6819 -0.5504 0.027 Uiso 1 1 calc R . . H57B H 0.4210 0.6357 -0.5794 0.027 Uiso 1 1 calc R . . C58 C 0.4419(3) 0.7336(3) -0.6681(2) 0.0267(10) Uani 1 1 d . . . H58A H 0.3883 0.7466 -0.7033 0.032 Uiso 1 1 calc R . . H58B H 0.4995 0.6827 -0.6799 0.032 Uiso 1 1 calc R . . C59 C 0.4525(3) 0.8275(3) -0.6815(3) 0.0298(10) Uani 1 1 d . . . H59A H 0.5190 0.8118 -0.6872 0.036 Uiso 1 1 calc R . . H59B H 0.4139 0.8745 -0.7298 0.036 Uiso 1 1 calc R . . C60 C 0.4225(3) 0.8754(3) -0.6167(2) 0.0221(9) Uani 1 1 d . . . H60A H 0.4138 0.9427 -0.6347 0.026 Uiso 1 1 calc R . . H60B H 0.4730 0.8394 -0.5731 0.026 Uiso 1 1 calc R . . N1 N 0.1915(2) 0.5858(2) -0.08166(18) 0.0176(7) Uani 1 1 d . . . N2 N 0.1585(2) 0.7304(2) -0.06584(18) 0.0167(7) Uani 1 1 d . . . N3 N 0.1989(2) 0.5152(2) 0.05593(18) 0.0188(7) Uani 1 1 d . . . N4 N 0.1835(2) 0.6540(2) 0.07274(18) 0.0198(7) Uani 1 1 d . . . N5 N 0.2354(2) 0.8259(2) -0.04811(18) 0.0164(7) Uani 1 1 d . . . N6 N 0.3746(2) 0.8246(2) -0.03750(18) 0.0175(7) Uani 1 1 d . . . N7 N 0.2598(2) 0.7511(2) 0.09016(19) 0.0209(7) Uani 1 1 d . . . N8 N 0.3925(2) 0.7637(2) 0.10126(18) 0.0191(7) Uani 1 1 d . . . N9 N 0.5470(2) 0.7564(2) -0.03505(18) 0.0180(7) Uani 1 1 d . . . N10 N 0.6926(2) 0.6433(2) -0.03936(19) 0.0214(7) Uani 1 1 d . . . N11 N 0.5657(2) 0.6940(2) 0.10391(18) 0.0197(7) Uani 1 1 d . . . N12 N 0.7069(2) 0.5747(2) 0.09896(18) 0.0189(7) Uani 1 1 d . . . N13 N -0.1676(2) 0.8888(2) -0.33305(18) 0.0164(7) Uani 1 1 d . . . N14 N -0.0425(2) 0.7563(2) -0.34532(18) 0.0157(7) Uani 1 1 d . . . N15 N -0.2261(2) 0.9186(2) -0.46437(18) 0.0167(7) Uani 1 1 d . . . N16 N -0.1112(2) 0.7767(2) -0.47114(18) 0.0179(7) Uani 1 1 d . . . N17 N 0.1147(2) 0.6702(2) -0.38376(18) 0.0156(7) Uani 1 1 d . . . N18 N 0.2489(2) 0.6571(2) -0.42960(17) 0.0152(7) Uani 1 1 d . . . N19 N 0.0446(2) 0.6861(2) -0.50770(18) 0.0178(7) Uani 1 1 d . . . N20 N 0.1719(2) 0.6908(2) -0.55671(18) 0.0189(7) Uani 1 1 d . . . N21 N 0.3284(2) 0.7539(2) -0.48474(18) 0.0162(7) Uani 1 1 d . . . N22 N 0.3091(2) 0.9055(2) -0.51834(17) 0.0155(7) Uani 1 1 d . . . N23 N 0.2502(2) 0.7894(2) -0.61180(18) 0.0183(7) Uani 1 1 d . . . N24 N 0.2489(2) 0.9344(2) -0.65028(18) 0.0174(7) Uani 1 1 d . . . O1 O 0.2339(2) 0.6885(2) -0.16919(15) 0.0216(6) Uani 1 1 d . . . O2 O 0.32668(19) 0.8020(2) -0.14665(15) 0.0201(6) Uani 1 1 d . . . O3 O 0.5801(2) 0.7030(2) -0.14337(16) 0.0252(6) Uani 1 1 d . . . O4 O 0.2638(2) 0.5108(2) 0.17036(16) 0.0268(7) Uani 1 1 d . . . O5 O 0.3771(2) 0.6399(2) 0.18969(16) 0.0298(7) Uani 1 1 d . . . O6 O 0.6232(2) 0.5476(2) 0.19940(16) 0.0245(6) Uani 1 1 d . . . O7 O -0.02315(19) 0.8376(2) -0.26446(16) 0.0216(6) Uani 1 1 d . . . O8 O 0.20781(19) 0.7165(2) -0.32521(15) 0.0207(6) Uani 1 1 d . . . O9 O 0.30100(19) 0.83459(19) -0.39275(15) 0.0187(6) Uani 1 1 d . . . O10 O -0.1773(2) 0.9025(2) -0.58272(16) 0.0265(7) Uani 1 1 d . . . O11 O 0.0289(2) 0.7733(2) -0.63457(16) 0.0263(7) Uani 1 1 d . . . O12 O 0.1352(2) 0.9127(2) -0.70818(17) 0.0292(7) Uani 1 1 d . . . N25 N 0.0094(3) 0.4443(3) -0.1967(2) 0.0318(9) Uani 1 1 d . . . N26 N 0.5662(3) 0.7193(3) -0.4145(3) 0.0419(10) Uani 1 1 d . . . N27 N 0.5933(5) 0.9369(4) -0.1666(3) 0.0568(14) Uani 1 1 d . . . O13 O 0.0462(3) 0.4516(3) -0.2563(2) 0.0494(10) Uani 1 1 d . . . O14 O 0.0106(3) 0.4904(3) -0.1518(2) 0.0548(10) Uani 1 1 d . . . O15 O -0.0286(3) 0.3903(3) -0.1810(2) 0.0622(12) Uani 1 1 d . . . O16 O 0.5265(3) 0.8080(3) -0.4301(2) 0.0568(10) Uani 1 1 d . . . O17 O 0.6245(4) 0.6770(3) -0.4547(3) 0.0792(15) Uani 1 1 d . . . O18 O 0.5458(4) 0.6704(3) -0.3588(3) 0.0846(17) Uani 1 1 d . . . O19 O 0.5340(3) 0.9974(3) -0.1325(2) 0.0600(11) Uani 1 1 d . . . O20 O 0.6739(4) 0.8713(4) -0.1321(3) 0.0775(14) Uani 1 1 d . . . O21 O 0.5748(4) 0.9451(4) -0.2316(3) 0.0901(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.0309(16) 0.0173(14) 0.0225(15) -0.0021(12) -0.0010(13) -0.0082(13) O2W 0.0238(15) 0.0194(15) 0.0258(16) -0.0012(12) 0.0001(13) -0.0078(13) O3W 0.0230(16) 0.0336(17) 0.0222(15) -0.0033(13) -0.0014(12) -0.0148(14) O4W 0.0224(16) 0.0310(17) 0.0353(18) -0.0101(14) 0.0044(13) -0.0129(14) Ho1 0.02301(12) 0.02232(12) 0.01452(11) -0.00374(8) 0.00202(8) -0.01197(9) C1 0.0154(19) 0.0167(19) 0.0122(19) -0.0003(16) -0.0008(15) -0.0068(16) C2 0.017(2) 0.020(2) 0.016(2) 0.0002(16) 0.0026(16) -0.0093(17) C3 0.017(2) 0.023(2) 0.016(2) -0.0050(17) 0.0051(16) -0.0103(17) C4 0.022(2) 0.026(2) 0.019(2) -0.0066(18) 0.0083(18) -0.0124(18) C5 0.019(2) 0.017(2) 0.0154(19) -0.0028(16) 0.0020(16) -0.0072(17) C6 0.031(2) 0.025(2) 0.014(2) -0.0084(17) 0.0072(17) -0.0143(19) C7 0.018(2) 0.0088(18) 0.017(2) -0.0006(15) -0.0002(16) -0.0046(16) C8 0.024(2) 0.018(2) 0.0113(19) -0.0057(16) 0.0007(16) -0.0077(17) C9 0.023(2) 0.017(2) 0.016(2) -0.0051(16) 0.0011(17) -0.0069(17) C10 0.026(2) 0.021(2) 0.015(2) -0.0111(18) 0.0043(17) -0.0073(18) C11 0.020(2) 0.020(2) 0.0158(19) 0.0009(16) -0.0003(16) -0.0122(17) C12 0.026(2) 0.028(2) 0.013(2) -0.0082(17) -0.0017(17) -0.0103(19) C13 0.026(2) 0.018(2) 0.019(2) -0.0010(17) 0.0001(18) -0.0151(18) C14 0.023(2) 0.019(2) 0.017(2) -0.0013(16) -0.0032(17) -0.0114(17) C15 0.020(2) 0.017(2) 0.021(2) -0.0011(17) -0.0002(17) -0.0104(17) C16 0.022(2) 0.018(2) 0.018(2) -0.0071(17) 0.0012(17) -0.0101(17) C17 0.026(2) 0.021(2) 0.015(2) 0.0014(17) 0.0036(17) -0.0138(18) C18 0.021(2) 0.0158(19) 0.0148(19) -0.0004(16) -0.0007(16) -0.0081(17) C19 0.021(2) 0.030(2) 0.020(2) -0.0040(18) 0.0037(17) -0.0162(19) C20 0.019(2) 0.033(2) 0.029(2) 0.000(2) -0.0022(19) -0.014(2) C21 0.020(2) 0.030(2) 0.033(3) -0.003(2) -0.0001(19) -0.0068(19) C22 0.018(2) 0.025(2) 0.029(2) -0.0057(19) 0.0088(18) -0.0074(18) C23 0.024(2) 0.022(2) 0.027(2) -0.0097(19) 0.0062(19) -0.0032(18) C24 0.052(3) 0.029(3) 0.034(3) -0.019(2) 0.010(2) -0.006(2) C25 0.049(3) 0.038(3) 0.047(3) -0.033(3) -0.008(3) -0.002(3) C26 0.035(3) 0.017(2) 0.036(3) -0.0123(19) -0.003(2) -0.0092(19) C27 0.028(2) 0.019(2) 0.036(3) -0.0090(19) -0.004(2) -0.0110(19) C28 0.037(3) 0.033(3) 0.037(3) -0.015(2) -0.007(2) -0.015(2) C29 0.039(3) 0.034(3) 0.038(3) -0.008(2) -0.010(2) -0.020(2) C30 0.026(2) 0.024(2) 0.028(2) -0.0023(19) -0.0045(19) -0.0146(19) C31 0.0130(19) 0.0170(19) 0.0131(19) 0.0012(16) 0.0038(15) -0.0071(16) C32 0.017(2) 0.0166(19) 0.0145(19) -0.0034(16) 0.0014(16) -0.0079(17) C33 0.0137(19) 0.0170(19) 0.0158(19) -0.0059(16) 0.0025(15) -0.0063(16) C34 0.016(2) 0.021(2) 0.018(2) -0.0051(17) 0.0004(16) -0.0095(17) C35 0.017(2) 0.021(2) 0.016(2) -0.0037(17) 0.0047(16) -0.0076(17) C36 0.019(2) 0.024(2) 0.018(2) -0.0097(17) 0.0010(16) -0.0097(18) C37 0.0159(19) 0.0109(18) 0.016(2) -0.0003(15) -0.0007(16) -0.0038(16) C38 0.0147(19) 0.0147(19) 0.0128(18) -0.0036(15) 0.0018(15) -0.0048(16) C39 0.0164(19) 0.0163(19) 0.0154(19) -0.0049(16) 0.0029(16) -0.0075(16) C40 0.024(2) 0.021(2) 0.019(2) -0.0099(18) 0.0033(18) -0.0106(18) C41 0.0152(19) 0.0135(19) 0.0131(18) -0.0020(15) 0.0014(15) -0.0045(16) C42 0.027(2) 0.024(2) 0.0130(19) -0.0090(17) 0.0061(17) -0.0116(18) C43 0.0107(18) 0.018(2) 0.017(2) -0.0030(16) -0.0004(15) -0.0051(16) C44 0.0152(19) 0.019(2) 0.0115(18) -0.0037(16) 0.0032(15) -0.0056(16) C45 0.0159(19) 0.016(2) 0.0119(19) -0.0019(16) 0.0027(16) -0.0038(16) C46 0.019(2) 0.022(2) 0.0124(19) -0.0054(16) 0.0052(17) -0.0077(17) C47 0.0170(19) 0.0157(19) 0.019(2) -0.0023(16) -0.0008(16) -0.0074(16) C48 0.021(2) 0.016(2) 0.0137(19) 0.0000(16) 0.0005(16) -0.0055(17) C49 0.016(2) 0.023(2) 0.025(2) -0.0030(18) 0.0045(17) -0.0076(18) C50 0.028(2) 0.031(3) 0.031(3) 0.001(2) 0.012(2) -0.012(2) C51 0.030(2) 0.027(2) 0.024(2) 0.0021(19) 0.0021(19) -0.016(2) C52 0.018(2) 0.016(2) 0.026(2) -0.0014(17) 0.0016(17) -0.0073(17) C53 0.025(2) 0.020(2) 0.027(2) -0.0085(18) 0.0073(18) -0.0122(18) C54 0.035(3) 0.022(2) 0.028(2) -0.0023(19) 0.004(2) -0.008(2) C55 0.026(2) 0.018(2) 0.038(3) -0.005(2) 0.001(2) -0.0042(19) C56 0.022(2) 0.023(2) 0.028(2) -0.0128(19) 0.0076(18) -0.0086(18) C57 0.018(2) 0.021(2) 0.022(2) -0.0067(17) 0.0042(17) -0.0026(17) C58 0.020(2) 0.032(2) 0.022(2) -0.0127(19) 0.0087(18) -0.0037(19) C59 0.027(2) 0.033(3) 0.022(2) -0.006(2) 0.0134(19) -0.008(2) C60 0.017(2) 0.023(2) 0.022(2) -0.0049(18) 0.0054(17) -0.0067(17) N1 0.0203(17) 0.0207(17) 0.0140(16) -0.0054(14) 0.0061(14) -0.0111(15) N2 0.0191(17) 0.0160(16) 0.0134(16) 0.0000(13) 0.0037(13) -0.0090(14) N3 0.0207(18) 0.0190(17) 0.0136(16) 0.0000(14) 0.0007(14) -0.0089(15) N4 0.0236(18) 0.0225(18) 0.0121(16) -0.0035(14) 0.0026(14) -0.0105(15) N5 0.0185(17) 0.0196(17) 0.0107(16) -0.0059(13) 0.0020(13) -0.0075(14) N6 0.0230(18) 0.0212(17) 0.0122(16) -0.0049(14) 0.0027(14) -0.0135(15) N7 0.0262(19) 0.0224(18) 0.0151(17) -0.0054(14) 0.0029(14) -0.0121(16) N8 0.0186(17) 0.0214(18) 0.0129(16) -0.0036(14) -0.0014(14) -0.0062(15) N9 0.0196(17) 0.0185(17) 0.0146(16) -0.0026(14) -0.0006(14) -0.0089(14) N10 0.0224(18) 0.0239(18) 0.0151(17) -0.0007(14) -0.0008(14) -0.0108(15) N11 0.0228(18) 0.0187(17) 0.0149(17) -0.0014(14) 0.0013(14) -0.0092(15) N12 0.0236(18) 0.0153(17) 0.0139(16) 0.0019(14) -0.0007(14) -0.0088(15) N13 0.0162(16) 0.0177(17) 0.0136(16) -0.0067(13) 0.0022(13) -0.0053(14) N14 0.0126(16) 0.0175(17) 0.0145(16) -0.0044(13) 0.0006(13) -0.0051(14) N15 0.0173(17) 0.0124(16) 0.0144(16) -0.0020(13) -0.0001(13) -0.0028(14) N16 0.0152(16) 0.0175(17) 0.0173(17) -0.0055(14) 0.0008(14) -0.0040(14) N17 0.0160(16) 0.0179(16) 0.0136(16) -0.0071(13) 0.0046(13) -0.0071(14) N18 0.0161(16) 0.0189(17) 0.0121(16) -0.0057(13) 0.0027(13) -0.0087(14) N19 0.0159(17) 0.0223(18) 0.0145(16) -0.0052(14) 0.0012(13) -0.0081(14) N20 0.0185(17) 0.0246(18) 0.0126(16) -0.0033(14) 0.0019(14) -0.0102(15) N21 0.0196(17) 0.0165(16) 0.0122(16) -0.0042(13) 0.0054(13) -0.0083(14) N22 0.0178(16) 0.0168(16) 0.0104(15) -0.0033(13) 0.0028(13) -0.0071(14) N23 0.0203(17) 0.0200(17) 0.0141(16) -0.0062(14) 0.0016(14) -0.0081(15) N24 0.0183(17) 0.0158(16) 0.0124(16) -0.0003(13) -0.0006(13) -0.0050(14) O1 0.0291(16) 0.0240(15) 0.0166(14) -0.0061(12) 0.0082(12) -0.0162(13) O2 0.0239(15) 0.0276(15) 0.0117(14) -0.0059(12) 0.0039(11) -0.0143(13) O3 0.0265(16) 0.0301(16) 0.0163(15) -0.0067(13) -0.0015(12) -0.0106(13) O4 0.0314(17) 0.0267(16) 0.0166(15) -0.0017(13) -0.0016(13) -0.0107(14) O5 0.0356(18) 0.0259(16) 0.0172(15) 0.0044(13) -0.0055(13) -0.0106(14) O6 0.0301(16) 0.0200(15) 0.0203(15) -0.0033(13) 0.0075(13) -0.0103(13) O7 0.0195(14) 0.0253(15) 0.0198(15) -0.0074(12) 0.0009(12) -0.0096(12) O8 0.0213(15) 0.0294(16) 0.0148(14) -0.0094(12) 0.0039(12) -0.0131(13) O9 0.0259(15) 0.0212(14) 0.0116(14) -0.0070(11) 0.0047(11) -0.0118(12) O10 0.0278(16) 0.0247(16) 0.0167(15) -0.0033(13) 0.0037(13) -0.0048(13) O11 0.0264(16) 0.0304(17) 0.0154(15) -0.0016(13) -0.0043(13) -0.0101(14) O12 0.0307(17) 0.0287(17) 0.0229(16) -0.0032(13) -0.0072(14) -0.0114(14) N25 0.026(2) 0.034(2) 0.025(2) 0.0020(18) -0.0022(17) -0.0103(18) N26 0.044(3) 0.045(3) 0.039(3) -0.017(2) 0.009(2) -0.020(2) N27 0.090(4) 0.054(3) 0.045(3) -0.011(3) 0.014(3) -0.051(3) O13 0.048(2) 0.053(2) 0.034(2) 0.0007(18) 0.0143(18) -0.0194(19) O14 0.052(2) 0.062(3) 0.046(2) -0.024(2) -0.0077(19) -0.018(2) O15 0.074(3) 0.071(3) 0.059(3) -0.009(2) 0.019(2) -0.053(3) O16 0.062(3) 0.044(2) 0.057(3) -0.016(2) 0.000(2) -0.016(2) O17 0.094(4) 0.061(3) 0.075(3) -0.032(3) 0.054(3) -0.023(3) O18 0.131(5) 0.059(3) 0.077(3) -0.026(3) 0.062(3) -0.052(3) O19 0.072(3) 0.064(3) 0.050(2) -0.027(2) 0.026(2) -0.031(2) O20 0.075(3) 0.076(3) 0.072(3) -0.022(3) 0.006(3) -0.027(3) O21 0.109(4) 0.087(4) 0.052(3) -0.028(3) 0.012(3) -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 O1W Ho1 2.375(3) . ? O2W Ho1 2.334(3) . ? O3W Ho1 2.389(3) . ? O4W Ho1 2.310(3) . ? Ho1 O9 2.316(3) . ? Ho1 O2 2.351(3) . ? Ho1 O1 2.373(3) . ? Ho1 O8 2.403(3) . ? C1 O1 1.229(5) . ? C1 N1 1.353(5) . ? C1 N2 1.358(5) . ? C2 N3 1.453(5) . ? C2 N1 1.476(5) . ? C2 C19 1.516(5) . ? C2 C3 1.567(5) . ? C3 N2 1.458(5) . ? C3 N4 1.459(5) . ? C3 C22 1.522(5) . ? C4 O4 1.215(5) . ? C4 N4 1.361(5) . ? C4 N3 1.372(5) . ? C5 N2 1.439(5) . ? C5 N5 1.444(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.447(5) . ? C6 N7 1.454(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.233(5) . ? C7 N5 1.336(5) . ? C7 N6 1.363(5) . ? C8 N7 1.452(5) . ? C8 N5 1.469(5) . ? C8 C23 1.529(6) . ? C8 C9 1.564(6) . ? C9 N8 1.451(5) . ? C9 N6 1.459(5) . ? C9 C26 1.535(5) . ? C10 O5 1.219(5) . ? C10 N8 1.362(5) . ? C10 N7 1.369(5) . ? C11 N9 1.449(5) . ? C11 N6 1.450(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.450(5) . ? C12 N8 1.453(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.228(5) . ? C13 N9 1.359(5) . ? C13 N10 1.362(5) . ? C14 N9 1.463(5) . ? C14 N11 1.464(5) . ? C14 C27 1.513(5) . ? C14 C15 1.568(6) . ? C15 N10 1.457(5) . ? C15 N12 1.465(5) . ? C15 C30 1.516(5) . ? C16 O6 1.225(5) . ? C16 N11 1.360(5) . ? C16 N12 1.365(5) . ? C17 N3 1.438(5) 2_665 ? C17 N10 1.445(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.451(5) 2_665 ? C18 N12 1.454(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.530(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.537(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.531(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.530(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.519(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.529(7) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.521(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.527(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.525(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O7 1.224(5) . ? C31 N14 1.360(5) . ? C31 N13 1.371(5) . ? C32 N15 1.454(5) . ? C32 N13 1.462(5) . ? C32 C49 1.518(5) . ? C32 C33 1.580(5) . ? C33 N16 1.441(5) . ? C33 N14 1.467(5) . ? C33 C52 1.514(5) . ? C34 O10 1.224(5) . ? C34 N16 1.363(5) . ? C34 N15 1.363(5) . ? C35 N14 1.452(5) . ? C35 N17 1.459(5) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N19 1.441(5) . ? C36 N16 1.447(5) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O8 1.232(5) . ? C37 N18 1.351(5) . ? C37 N17 1.358(5) . ? C38 N19 1.450(5) . ? C38 N17 1.468(5) . ? C38 C53 1.518(5) . ? C38 C39 1.572(5) . ? C39 N20 1.449(5) . ? C39 N18 1.465(5) . ? C39 C56 1.523(5) . ? C40 O11 1.217(5) . ? C40 N19 1.366(5) . ? C40 N20 1.370(5) . ? C41 N18 1.437(5) . ? C41 N21 1.446(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N20 1.446(5) . ? C42 N23 1.450(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 O9 1.235(5) . ? C43 N22 1.345(5) . ? C43 N21 1.349(5) . ? C44 N21 1.456(5) . ? C44 N23 1.458(5) . ? C44 C57 1.523(5) . ? C44 C45 1.564(5) . ? C45 N24 1.463(5) . ? C45 N22 1.477(5) . ? C45 C60 1.528(5) . ? C46 O12 1.216(5) . ? C46 N24 1.363(5) . ? C46 N23 1.371(5) . ? C47 N22 1.441(5) . ? C47 N15 1.460(5) 2_574 ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 N13 1.448(5) . ? C48 N24 1.453(5) 2_574 ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.522(6) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.536(6) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.518(6) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.528(6) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.532(6) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.542(6) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C58 1.516(6) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 C59 1.535(6) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 C60 1.525(6) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? N1 C18 1.451(5) 2_665 ? N3 C17 1.438(5) 2_665 ? N15 C47 1.460(5) 2_574 ? N24 C48 1.453(5) 2_574 ? N25 O13 1.226(5) . ? N25 O15 1.230(5) . ? N25 O14 1.238(5) . ? N26 O16 1.213(6) . ? N26 O17 1.235(6) . ? N26 O18 1.240(6) . ? N27 O21 1.179(7) . ? N27 O20 1.263(7) . ? N27 O19 1.298(7) . ? 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 O4W Ho1 O9 96.75(10) . . ? O4W Ho1 O2W 140.29(10) . . ? O9 Ho1 O2W 94.80(10) . . ? O4W Ho1 O2 97.46(10) . . ? O9 Ho1 O2 138.06(9) . . ? O2W Ho1 O2 98.87(10) . . ? O4W Ho1 O1 76.38(10) . . ? O9 Ho1 O1 146.25(9) . . ? O2W Ho1 O1 73.06(10) . . ? O2 Ho1 O1 75.62(9) . . ? O4W Ho1 O1W 71.99(10) . . ? O9 Ho1 O1W 75.66(9) . . ? O2W Ho1 O1W 147.69(10) . . ? O2 Ho1 O1W 71.70(10) . . ? O1 Ho1 O1W 130.29(10) . . ? O4W Ho1 O3W 147.30(10) . . ? O9 Ho1 O3W 74.62(10) . . ? O2W Ho1 O3W 72.39(10) . . ? O2 Ho1 O3W 72.21(10) . . ? O1 Ho1 O3W 127.58(10) . . ? O1W Ho1 O3W 75.31(10) . . ? O4W Ho1 O8 72.48(10) . . ? O9 Ho1 O8 76.02(9) . . ? O2W Ho1 O8 73.76(10) . . ? O2 Ho1 O8 145.91(9) . . ? O1 Ho1 O8 70.38(9) . . ? O1W Ho1 O8 130.86(10) . . ? O3W Ho1 O8 132.45(10) . . ? O1 C1 N1 124.8(4) . . ? O1 C1 N2 125.2(3) . . ? N1 C1 N2 110.0(3) . . ? N3 C2 N1 112.3(3) . . ? N3 C2 C19 113.6(3) . . ? N1 C2 C19 112.1(3) . . ? N3 C2 C3 103.0(3) . . ? N1 C2 C3 102.8(3) . . ? C19 C2 C3 112.2(3) . . ? N2 C3 N4 113.3(3) . . ? N2 C3 C22 111.8(3) . . ? N4 C3 C22 113.1(3) . . ? N2 C3 C2 102.7(3) . . ? N4 C3 C2 102.6(3) . . ? C22 C3 C2 112.4(3) . . ? O4 C4 N4 126.4(4) . . ? O4 C4 N3 125.1(4) . . ? N4 C4 N3 108.5(3) . . ? N2 C5 N5 113.8(3) . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? N5 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N4 C6 N7 113.7(3) . . ? N4 C6 H6A 108.8 . . ? N7 C6 H6A 108.8 . . ? N4 C6 H6B 108.8 . . ? N7 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N5 125.9(3) . . ? O2 C7 N6 124.5(3) . . ? N5 C7 N6 109.6(3) . . ? N7 C8 N5 112.5(3) . . ? N7 C8 C23 113.3(3) . . ? N5 C8 C23 111.8(3) . . ? N7 C8 C9 102.8(3) . . ? N5 C8 C9 102.5(3) . . ? C23 C8 C9 113.1(3) . . ? N8 C9 N6 112.3(3) . . ? N8 C9 C26 113.5(3) . . ? N6 C9 C26 113.1(3) . . ? N8 C9 C8 103.0(3) . . ? N6 C9 C8 102.7(3) . . ? C26 C9 C8 111.2(3) . . ? O5 C10 N8 125.8(4) . . ? O5 C10 N7 125.7(4) . . ? N8 C10 N7 108.4(3) . . ? N9 C11 N6 114.9(3) . . ? N9 C11 H11A 108.5 . . ? N6 C11 H11A 108.5 . . ? N9 C11 H11B 108.5 . . ? N6 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N11 C12 N8 115.4(3) . . ? N11 C12 H12A 108.4 . . ? N8 C12 H12A 108.4 . . ? N11 C12 H12B 108.4 . . ? N8 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? O3 C13 N9 126.0(4) . . ? O3 C13 N10 124.6(4) . . ? N9 C13 N10 109.4(3) . . ? N9 C14 N11 111.7(3) . . ? N9 C14 C27 113.5(3) . . ? N11 C14 C27 113.0(3) . . ? N9 C14 C15 102.8(3) . . ? N11 C14 C15 102.7(3) . . ? C27 C14 C15 112.1(3) . . ? N10 C15 N12 112.3(3) . . ? N10 C15 C30 112.9(3) . . ? N12 C15 C30 112.8(3) . . ? N10 C15 C14 102.9(3) . . ? N12 C15 C14 102.9(3) . . ? C30 C15 C14 112.2(3) . . ? O6 C16 N11 125.5(4) . . ? O6 C16 N12 125.6(4) . . ? N11 C16 N12 108.8(3) . . ? N3 C17 N10 115.3(3) 2_665 . ? N3 C17 H17A 108.4 2_665 . ? N10 C17 H17A 108.4 . . ? N3 C17 H17B 108.4 2_665 . ? N10 C17 H17B 108.4 . . ? H17A C17 H17B 107.5 . . ? N1 C18 N12 114.5(3) 2_665 . ? N1 C18 H18A 108.6 2_665 . ? N12 C18 H18A 108.6 . . ? N1 C18 H18B 108.6 2_665 . ? N12 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C2 C19 C20 110.0(3) . . ? C2 C19 H19A 109.7 . . ? C20 C19 H19A 109.7 . . ? C2 C19 H19B 109.7 . . ? C20 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? C19 C20 C21 112.6(4) . . ? C19 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C20 112.6(4) . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21B 109.1 . . ? C20 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C3 C22 C21 111.5(4) . . ? C3 C22 H22A 109.3 . . ? C21 C22 H22A 109.3 . . ? C3 C22 H22B 109.3 . . ? C21 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C8 C23 C24 109.5(4) . . ? C8 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? C8 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? C25 C24 C23 112.0(4) . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C24 C25 C26 114.1(4) . . ? C24 C25 H25A 108.7 . . ? C26 C25 H25A 108.7 . . ? C24 C25 H25B 108.7 . . ? C26 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? C25 C26 C9 110.6(4) . . ? C25 C26 H26A 109.5 . . ? C9 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C9 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C14 C27 C28 111.0(4) . . ? C14 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? C14 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C27 C28 C29 113.2(4) . . ? C27 C28 H28A 108.9 . . ? C29 C28 H28A 108.9 . . ? C27 C28 H28B 108.9 . . ? C29 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? C30 C29 C28 112.6(4) . . ? C30 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? C30 C29 H29B 109.1 . . ? C28 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C15 C30 C29 110.7(4) . . ? C15 C30 H30A 109.5 . . ? C29 C30 H30A 109.5 . . ? C15 C30 H30B 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? O7 C31 N14 125.7(3) . . ? O7 C31 N13 125.3(4) . . ? N14 C31 N13 108.9(3) . . ? N15 C32 N13 111.6(3) . . ? N15 C32 C49 113.6(3) . . ? N13 C32 C49 113.6(3) . . ? N15 C32 C33 102.2(3) . . ? N13 C32 C33 103.2(3) . . ? C49 C32 C33 111.5(3) . . ? N16 C33 N14 112.5(3) . . ? N16 C33 C52 113.0(3) . . ? N14 C33 C52 113.4(3) . . ? N16 C33 C32 102.9(3) . . ? N14 C33 C32 101.9(3) . . ? C52 C33 C32 112.0(3) . . ? O10 C34 N16 124.6(4) . . ? O10 C34 N15 126.6(4) . . ? N16 C34 N15 108.7(3) . . ? N14 C35 N17 114.3(3) . . ? N14 C35 H35A 108.7 . . ? N17 C35 H35A 108.7 . . ? N14 C35 H35B 108.7 . . ? N17 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? N19 C36 N16 114.5(3) . . ? N19 C36 H36A 108.6 . . ? N16 C36 H36A 108.6 . . ? N19 C36 H36B 108.6 . . ? N16 C36 H36B 108.6 . . ? H36A C36 H36B 107.6 . . ? O8 C37 N18 125.4(3) . . ? O8 C37 N17 124.8(4) . . ? N18 C37 N17 109.7(3) . . ? N19 C38 N17 112.1(3) . . ? N19 C38 C53 113.5(3) . . ? N17 C38 C53 112.8(3) . . ? N19 C38 C39 102.8(3) . . ? N17 C38 C39 102.5(3) . . ? C53 C38 C39 112.2(3) . . ? N20 C39 N18 113.3(3) . . ? N20 C39 C56 112.8(3) . . ? N18 C39 C56 112.3(3) . . ? N20 C39 C38 102.8(3) . . ? N18 C39 C38 102.6(3) . . ? C56 C39 C38 112.2(3) . . ? O11 C40 N19 126.1(4) . . ? O11 C40 N20 125.6(4) . . ? N19 C40 N20 108.3(3) . . ? N18 C41 N21 114.3(3) . . ? N18 C41 H41A 108.7 . . ? N21 C41 H41A 108.7 . . ? N18 C41 H41B 108.7 . . ? N21 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? N20 C42 N23 113.9(3) . . ? N20 C42 H42A 108.8 . . ? N23 C42 H42A 108.8 . . ? N20 C42 H42B 108.8 . . ? N23 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? O9 C43 N22 125.2(3) . . ? O9 C43 N21 124.7(3) . . ? N22 C43 N21 110.0(3) . . ? N21 C44 N23 113.3(3) . . ? N21 C44 C57 112.6(3) . . ? N23 C44 C57 112.4(3) . . ? N21 C44 C45 102.7(3) . . ? N23 C44 C45 102.8(3) . . ? C57 C44 C45 112.2(3) . . ? N24 C45 N22 111.9(3) . . ? N24 C45 C60 113.4(3) . . ? N22 C45 C60 112.6(3) . . ? N24 C45 C44 103.1(3) . . ? N22 C45 C44 102.3(3) . . ? C60 C45 C44 112.7(3) . . ? O12 C46 N24 125.6(4) . . ? O12 C46 N23 125.7(4) . . ? N24 C46 N23 108.7(3) . . ? N22 C47 N15 114.3(3) . 2_574 ? N22 C47 H47A 108.7 . . ? N15 C47 H47A 108.7 2_574 . ? N22 C47 H47B 108.7 . . ? N15 C47 H47B 108.7 2_574 . ? H47A C47 H47B 107.6 . . ? N13 C48 N24 115.3(3) . 2_574 ? N13 C48 H48A 108.4 . . ? N24 C48 H48A 108.4 2_574 . ? N13 C48 H48B 108.4 . . ? N24 C48 H48B 108.4 2_574 . ? H48A C48 H48B 107.5 . . ? C32 C49 C50 112.7(3) . . ? C32 C49 H49A 109.1 . . ? C50 C49 H49A 109.1 . . ? C32 C49 H49B 109.1 . . ? C50 C49 H49B 109.1 . . ? H49A C49 H49B 107.8 . . ? C49 C50 C51 113.0(4) . . ? C49 C50 H50A 109.0 . . ? C51 C50 H50A 109.0 . . ? C49 C50 H50B 109.0 . . ? C51 C50 H50B 109.0 . . ? H50A C50 H50B 107.8 . . ? C52 C51 C50 111.9(3) . . ? C52 C51 H51A 109.2 . . ? C50 C51 H51A 109.2 . . ? C52 C51 H51B 109.2 . . ? C50 C51 H51B 109.2 . . ? H51A C51 H51B 107.9 . . ? C33 C52 C51 111.4(3) . . ? C33 C52 H52A 109.3 . . ? C51 C52 H52A 109.3 . . ? C33 C52 H52B 109.3 . . ? C51 C52 H52B 109.3 . . ? H52A C52 H52B 108.0 . . ? C38 C53 C54 110.2(3) . . ? C38 C53 H53A 109.6 . . ? C54 C53 H53A 109.6 . . ? C38 C53 H53B 109.6 . . ? C54 C53 H53B 109.6 . . ? H53A C53 H53B 108.1 . . ? C53 C54 C55 112.8(4) . . ? C53 C54 H54A 109.0 . . ? C55 C54 H54A 109.0 . . ? C53 C54 H54B 109.0 . . ? C55 C54 H54B 109.0 . . ? H54A C54 H54B 107.8 . . ? C54 C55 C56 112.6(4) . . ? C54 C55 H55A 109.1 . . ? C56 C55 H55A 109.1 . . ? C54 C55 H55B 109.1 . . ? C56 C55 H55B 109.1 . . ? H55A C55 H55B 107.8 . . ? C39 C56 C55 111.0(3) . . ? C39 C56 H56A 109.4 . . ? C55 C56 H56A 109.4 . . ? C39 C56 H56B 109.4 . . ? C55 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? C58 C57 C44 110.1(3) . . ? C58 C57 H57A 109.6 . . ? C44 C57 H57A 109.6 . . ? C58 C57 H57B 109.6 . . ? C44 C57 H57B 109.6 . . ? H57A C57 H57B 108.2 . . ? C57 C58 C59 112.2(3) . . ? C57 C58 H58A 109.2 . . ? C59 C58 H58A 109.2 . . ? C57 C58 H58B 109.2 . . ? C59 C58 H58B 109.2 . . ? H58A C58 H58B 107.9 . . ? C60 C59 C58 113.6(3) . . ? C60 C59 H59A 108.9 . . ? C58 C59 H59A 108.9 . . ? C60 C59 H59B 108.9 . . ? C58 C59 H59B 108.9 . . ? H59A C59 H59B 107.7 . . ? C59 C60 C45 111.5(3) . . ? C59 C60 H60A 109.3 . . ? C45 C60 H60A 109.3 . . ? C59 C60 H60B 109.3 . . ? C45 C60 H60B 109.3 . . ? H60A C60 H60B 108.0 . . ? C1 N1 C18 120.9(3) . 2_665 ? C1 N1 C2 111.6(3) . . ? C18 N1 C2 125.1(3) 2_665 . ? C1 N2 C5 122.3(3) . . ? C1 N2 C3 112.4(3) . . ? C5 N2 C3 125.3(3) . . ? C4 N3 C17 121.3(3) . 2_665 ? C4 N3 C2 112.5(3) . . ? C17 N3 C2 126.0(3) 2_665 . ? C4 N4 C6 120.3(3) . . ? C4 N4 C3 112.7(3) . . ? C6 N4 C3 125.8(3) . . ? C7 N5 C5 123.1(3) . . ? C7 N5 C8 112.7(3) . . ? C5 N5 C8 124.2(3) . . ? C7 N6 C11 121.1(3) . . ? C7 N6 C9 112.3(3) . . ? C11 N6 C9 124.8(3) . . ? C10 N7 C8 112.7(3) . . ? C10 N7 C6 120.9(3) . . ? C8 N7 C6 125.7(3) . . ? C10 N8 C9 112.8(3) . . ? C10 N8 C12 121.1(3) . . ? C9 N8 C12 125.7(3) . . ? C13 N9 C11 121.4(3) . . ? C13 N9 C14 112.3(3) . . ? C11 N9 C14 124.5(3) . . ? C13 N10 C17 121.8(3) . . ? C13 N10 C15 112.4(3) . . ? C17 N10 C15 124.9(3) . . ? C16 N11 C12 121.2(3) . . ? C16 N11 C14 112.9(3) . . ? C12 N11 C14 124.9(3) . . ? C16 N12 C18 121.2(3) . . ? C16 N12 C15 112.4(3) . . ? C18 N12 C15 125.2(3) . . ? C31 N13 C48 122.2(3) . . ? C31 N13 C32 112.3(3) . . ? C48 N13 C32 125.1(3) . . ? C31 N14 C35 120.7(3) . . ? C31 N14 C33 113.2(3) . . ? C35 N14 C33 124.6(3) . . ? C34 N15 C32 112.7(3) . . ? C34 N15 C47 120.2(3) . 2_574 ? C32 N15 C47 123.9(3) . 2_574 ? C34 N16 C33 113.0(3) . . ? C34 N16 C36 121.7(3) . . ? C33 N16 C36 124.9(3) . . ? C37 N17 C35 120.7(3) . . ? C37 N17 C38 112.1(3) . . ? C35 N17 C38 124.7(3) . . ? C37 N18 C41 122.5(3) . . ? C37 N18 C39 112.6(3) . . ? C41 N18 C39 125.0(3) . . ? C40 N19 C36 121.2(3) . . ? C40 N19 C38 113.0(3) . . ? C36 N19 C38 125.6(3) . . ? C40 N20 C42 120.3(3) . . ? C40 N20 C39 112.7(3) . . ? C42 N20 C39 126.1(3) . . ? C43 N21 C41 122.9(3) . . ? C43 N21 C44 112.5(3) . . ? C41 N21 C44 124.5(3) . . ? C43 N22 C47 121.5(3) . . ? C43 N22 C45 111.9(3) . . ? C47 N22 C45 124.5(3) . . ? C46 N23 C42 121.2(3) . . ? C46 N23 C44 112.7(3) . . ? C42 N23 C44 125.1(3) . . ? C46 N24 C48 121.6(3) . 2_574 ? C46 N24 C45 112.5(3) . . ? C48 N24 C45 125.7(3) 2_574 . ? C1 O1 Ho1 155.3(3) . . ? C7 O2 Ho1 154.7(3) . . ? C37 O8 Ho1 155.9(3) . . ? C43 O9 Ho1 159.1(2) . . ? O13 N25 O15 120.0(4) . . ? O13 N25 O14 120.5(4) . . ? O15 N25 O14 119.5(4) . . ? O16 N26 O17 121.1(5) . . ? O16 N26 O18 119.5(5) . . ? O17 N26 O18 119.4(5) . . ? O21 N27 O20 118.5(6) . . ? O21 N27 O19 120.5(6) . . ? O20 N27 O19 120.9(5) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.424 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.107 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 107 21 ' ' 2 0.226 0.127 0.720 203 68 ' ' 3 -0.162 0.456 0.655 57 20 ' ' 4 0.159 0.546 0.345 58 19 ' ' 5 -0.227 0.874 0.279 201 68 ' ' 6 0.500 0.500 0.000 115 28 ' ' 7 0.475 0.515 0.343 18 9 ' ' 8 0.525 0.485 0.657 17 8 ' ' _platon_squeeze_details ; ; data_p7 _database_code_depnum_ccdc_archive 'CCDC 881905' #TrackingRef '110519qx-submit-cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H106 N27 O38 Tb' _chemical_formula_weight 1972.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.8446(6) _cell_length_b 15.9631(7) _cell_length_c 18.1699(7) _cell_angle_alpha 74.8650(10) _cell_angle_beta 89.2060(10) _cell_angle_gamma 63.3360(10) _cell_volume 3936.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8080 _exptl_absorpt_correction_T_max 0.8713 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42259 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13706 _reflns_number_gt 11652 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0714P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13706 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 O1W O 1.2575(2) 0.4504(2) 0.71470(17) 0.0240(7) Uani 1 1 d . . . O2W O 1.3959(2) 0.1198(2) 0.75379(17) 0.0247(7) Uani 1 1 d . . . O3W O 1.1214(2) 0.3837(2) 0.72767(19) 0.0290(7) Uani 1 1 d . . . O4W O 1.44136(19) 0.2753(2) 0.73536(17) 0.0244(7) Uani 1 1 d . . . Tb1 Tb 1.285534(13) 0.284863(14) 0.736676(11) 0.01773(8) Uani 1 1 d . . . C1 C 1.1915(3) 0.1862(3) 0.6242(2) 0.0152(8) Uani 1 1 d . . . C2 C 1.1198(3) 0.1242(3) 0.5555(2) 0.0152(8) Uani 1 1 d . . . C3 C 1.2114(3) 0.1217(3) 0.5191(2) 0.0142(8) Uani 1 1 d . . . C4 C 1.0773(3) 0.2226(3) 0.4273(2) 0.0184(9) Uani 1 1 d . . . C5 C 1.3372(3) 0.1629(3) 0.5655(2) 0.0143(8) Uani 1 1 d . . . H5A H 1.3825 0.1086 0.5473 0.017 Uiso 1 1 calc R . . H5B H 1.3631 0.1540 0.6172 0.017 Uiso 1 1 calc R . . C6 C 1.2275(3) 0.2133(3) 0.3840(2) 0.0204(9) Uani 1 1 d . . . H6A H 1.2863 0.1535 0.3867 0.025 Uiso 1 1 calc R . . H6B H 1.1911 0.2336 0.3339 0.025 Uiso 1 1 calc R . . C7 C 1.3119(3) 0.3321(3) 0.5397(2) 0.0157(8) Uani 1 1 d . . . C8 C 1.3360(3) 0.2732(3) 0.4338(2) 0.0162(8) Uani 1 1 d . . . C9 C 1.3313(3) 0.3770(3) 0.4100(2) 0.0166(8) Uani 1 1 d . . . C10 C 1.2049(3) 0.3820(3) 0.3395(2) 0.0186(9) Uani 1 1 d . . . C11 C 1.3128(3) 0.4894(3) 0.4949(2) 0.0167(8) Uani 1 1 d . . . H11A H 1.3665 0.4960 0.4715 0.020 Uiso 1 1 calc R . . H11B H 1.3248 0.4776 0.5503 0.020 Uiso 1 1 calc R . . C12 C 1.2231(3) 0.5320(3) 0.3007(2) 0.0178(9) Uani 1 1 d . . . H12A H 1.2810 0.5362 0.2856 0.021 Uiso 1 1 calc R . . H12B H 1.1858 0.5418 0.2538 0.021 Uiso 1 1 calc R . . C13 C 1.1724(3) 0.6297(3) 0.5135(2) 0.0167(8) Uani 1 1 d . . . C14 C 1.2076(3) 0.6430(3) 0.3852(2) 0.0158(8) Uani 1 1 d . . . C15 C 1.1205(3) 0.7413(3) 0.3899(2) 0.0161(8) Uani 1 1 d . . . C16 C 1.0730(3) 0.6708(3) 0.3110(2) 0.0161(8) Uani 1 1 d . . . C17 C 1.0527(3) 0.7962(3) 0.5078(2) 0.0187(9) Uani 1 1 d . . . H17A H 1.0533 0.8579 0.4817 0.022 Uiso 1 1 calc R . . H17B H 1.0808 0.7759 0.5611 0.022 Uiso 1 1 calc R . . C18 C 1.0526(3) 0.1755(3) 0.6761(2) 0.0152(8) Uani 1 1 d . . . H18A H 1.0819 0.1798 0.7212 0.018 Uiso 1 1 calc R . . H18B H 1.0477 0.1143 0.6911 0.018 Uiso 1 1 calc R . . C19 C 1.1287(3) 0.0219(3) 0.5870(3) 0.0227(9) Uani 1 1 d . . . H19A H 1.0756 0.0250 0.6165 0.027 Uiso 1 1 calc R . . H19B H 1.1254 -0.0039 0.5443 0.027 Uiso 1 1 calc R . . C20 C 1.2216(3) -0.0458(3) 0.6379(3) 0.0280(10) Uani 1 1 d . . . H20A H 1.2258 -0.1111 0.6571 0.034 Uiso 1 1 calc R . . H20B H 1.2225 -0.0220 0.6823 0.034 Uiso 1 1 calc R . . C21 C 1.3090(3) -0.0537(3) 0.5963(3) 0.0306(11) Uani 1 1 d . . . H21A H 1.3510 -0.0427 0.6273 0.037 Uiso 1 1 calc R . . H21B H 1.3443 -0.1200 0.5911 0.037 Uiso 1 1 calc R . . C22 C 1.2814(3) 0.0201(3) 0.5166(2) 0.0219(9) Uani 1 1 d . . . H22A H 1.3387 0.0213 0.4965 0.026 Uiso 1 1 calc R . . H22B H 1.2532 -0.0005 0.4817 0.026 Uiso 1 1 calc R . . C23 C 1.4274(3) 0.1959(3) 0.4137(2) 0.0209(9) Uani 1 1 d . . . H23A H 1.4820 0.1806 0.4489 0.025 Uiso 1 1 calc R . . H23B H 1.4222 0.1356 0.4196 0.025 Uiso 1 1 calc R . . C24 C 1.4427(3) 0.2341(3) 0.3316(2) 0.0244(10) Uani 1 1 d . . . H24A H 1.3883 0.2481 0.2968 0.029 Uiso 1 1 calc R . . H24B H 1.4997 0.1835 0.3189 0.029 Uiso 1 1 calc R . . C25 C 1.4540(3) 0.3267(3) 0.3191(3) 0.0289(11) Uani 1 1 d . . . H25A H 1.5209 0.3102 0.3143 0.035 Uiso 1 1 calc R . . H25B H 1.4165 0.3736 0.2706 0.035 Uiso 1 1 calc R . . C26 C 1.4229(3) 0.3752(3) 0.3834(2) 0.0223(9) Uani 1 1 d . . . H26A H 1.4731 0.3397 0.4270 0.027 Uiso 1 1 calc R . . H26B H 1.4141 0.4424 0.3654 0.027 Uiso 1 1 calc R . . C27 C 1.2918(3) 0.6603(3) 0.3583(2) 0.0221(9) Uani 1 1 d . . . H27A H 1.3155 0.6794 0.3974 0.026 Uiso 1 1 calc R . . H27B H 1.3432 0.5991 0.3530 0.026 Uiso 1 1 calc R . . C28 C 1.2652(3) 0.7392(3) 0.2822(3) 0.0296(11) Uani 1 1 d . . . H28A H 1.2593 0.7125 0.2408 0.036 Uiso 1 1 calc R . . H28B H 1.3166 0.7575 0.2731 0.036 Uiso 1 1 calc R . . C29 C 1.1718(3) 0.8311(3) 0.2790(3) 0.0270(10) Uani 1 1 d . . . H29A H 1.1814 0.8892 0.2593 0.032 Uiso 1 1 calc R . . H29B H 1.1230 0.8358 0.2434 0.032 Uiso 1 1 calc R . . C30 C 1.1377(3) 0.8294(3) 0.3574(2) 0.0206(9) Uani 1 1 d . . . H30A H 1.0786 0.8894 0.3533 0.025 Uiso 1 1 calc R . . H30B H 1.1855 0.8274 0.3925 0.025 Uiso 1 1 calc R . . C31 C 1.1990(3) 0.1693(3) 0.8908(2) 0.0162(8) Uani 1 1 d . . . C32 C 1.1387(3) 0.0888(3) 0.9867(2) 0.0188(9) Uani 1 1 d . . . C33 C 1.1226(3) 0.1871(3) 1.0011(2) 0.0191(9) Uani 1 1 d . . . C34 C 1.2195(3) 0.0555(3) 1.1064(2) 0.0203(9) Uani 1 1 d . . . C35 C 1.1543(3) 0.3250(3) 0.9178(2) 0.0178(9) Uani 1 1 d . . . H35A H 1.0962 0.3690 0.9348 0.021 Uiso 1 1 calc R . . H35B H 1.1500 0.3508 0.8620 0.021 Uiso 1 1 calc R . . C36 C 1.1901(3) 0.2162(3) 1.1157(2) 0.0225(9) Uani 1 1 d . . . H36A H 1.1276 0.2730 1.1099 0.027 Uiso 1 1 calc R . . H36B H 1.2071 0.1800 1.1704 0.027 Uiso 1 1 calc R . . C37 C 1.3133(3) 0.3156(3) 0.9183(2) 0.0146(8) Uani 1 1 d . . . C38 C 1.2418(3) 0.3379(3) 1.0294(2) 0.0175(9) Uani 1 1 d . . . C39 C 1.3376(3) 0.3425(3) 1.0346(2) 0.0192(9) Uani 1 1 d . . . C40 C 1.3465(3) 0.2090(3) 1.1331(2) 0.0210(9) Uani 1 1 d . . . C41 C 1.4550(3) 0.3369(3) 0.9342(2) 0.0199(9) Uani 1 1 d . . . H41A H 1.4525 0.3957 0.9436 0.024 Uiso 1 1 calc R . . H41B H 1.4484 0.3481 0.8785 0.024 Uiso 1 1 calc R . . C42 C 1.4820(3) 0.2431(3) 1.1400(2) 0.0210(9) Uani 1 1 d . . . H42A H 1.4781 0.3057 1.1413 0.025 Uiso 1 1 calc R . . H42B H 1.4901 0.2038 1.1933 0.025 Uiso 1 1 calc R . . C43 C 1.6036(3) 0.2010(3) 0.9221(2) 0.0194(9) Uani 1 1 d . . . C44 C 1.5992(3) 0.2398(3) 1.0391(2) 0.0187(9) Uani 1 1 d . . . C45 C 1.7011(3) 0.1562(3) 1.0368(2) 0.0188(9) Uani 1 1 d . . . C46 C 1.6311(3) 0.0981(3) 1.1402(2) 0.0197(9) Uani 1 1 d . . . C47 C 1.2081(3) 0.0191(3) 0.8727(2) 0.0189(9) Uani 1 1 d . . . H47A H 1.1530 0.0068 0.8710 0.023 Uiso 1 1 calc R . . H47B H 1.2134 0.0507 0.8201 0.023 Uiso 1 1 calc R . . C48 C 1.2271(3) -0.0873(3) 1.0751(2) 0.0188(9) Uani 1 1 d . . . H48A H 1.1727 -0.0964 1.0615 0.023 Uiso 1 1 calc R . . H48B H 1.2439 -0.1148 1.1309 0.023 Uiso 1 1 calc R . . C49 C 1.0453(3) 0.0869(3) 0.9718(2) 0.0216(9) Uani 1 1 d . . . H49A H 1.0158 0.0821 1.0194 0.026 Uiso 1 1 calc R . . H49B H 1.0577 0.0294 0.9549 0.026 Uiso 1 1 calc R . . C50 C 0.9773(3) 0.1803(3) 0.9099(3) 0.0285(10) Uani 1 1 d . . . H50A H 1.0058 0.1828 0.8616 0.034 Uiso 1 1 calc R . . H50B H 0.9176 0.1781 0.9010 0.034 Uiso 1 1 calc R . . C51 C 0.9561(3) 0.2729(3) 0.9331(3) 0.0311(11) Uani 1 1 d . . . H51A H 0.9653 0.3191 0.8904 0.037 Uiso 1 1 calc R . . H51B H 0.8893 0.3037 0.9420 0.037 Uiso 1 1 calc R . . C52 C 1.0186(3) 0.2534(3) 1.0050(2) 0.0236(10) Uani 1 1 d . . . H52A H 1.0117 0.3156 1.0103 0.028 Uiso 1 1 calc R . . H52B H 0.9974 0.2226 1.0503 0.028 Uiso 1 1 calc R . . C53 C 1.1565(3) 0.4291(3) 1.0385(3) 0.0258(10) Uani 1 1 d . . . H53A H 1.1433 0.4845 0.9932 0.031 Uiso 1 1 calc R . . H53B H 1.1003 0.4182 1.0425 0.031 Uiso 1 1 calc R . . C54 C 1.1770(4) 0.4526(4) 1.1101(3) 0.0389(13) Uani 1 1 d . . . H54A H 1.1227 0.5129 1.1140 0.047 Uiso 1 1 calc R . . H54B H 1.1838 0.3997 1.1555 0.047 Uiso 1 1 calc R . . C55 C 1.2661(4) 0.4652(4) 1.1101(3) 0.0398(13) Uani 1 1 d . . . H55A H 1.3075 0.4224 1.1581 0.048 Uiso 1 1 calc R . . H55B H 1.2484 0.5328 1.1088 0.048 Uiso 1 1 calc R . . C56 C 1.3223(3) 0.4418(3) 1.0423(3) 0.0266(10) Uani 1 1 d . . . H56A H 1.3840 0.4403 1.0504 0.032 Uiso 1 1 calc R . . H56B H 1.2873 0.4932 0.9948 0.032 Uiso 1 1 calc R . . C57 C 1.6024(3) 0.3299(3) 1.0467(3) 0.0243(10) Uani 1 1 d . . . H57A H 1.5385 0.3780 1.0519 0.029 Uiso 1 1 calc R . . H57B H 1.6229 0.3591 1.0002 0.029 Uiso 1 1 calc R . . C58 C 1.6705(3) 0.3060(3) 1.1162(3) 0.0327(11) Uani 1 1 d . . . H58A H 1.6434 0.2886 1.1631 0.039 Uiso 1 1 calc R . . H58B H 1.6771 0.3642 1.1157 0.039 Uiso 1 1 calc R . . C59 C 1.7692(3) 0.2214(3) 1.1178(3) 0.0328(11) Uani 1 1 d . . . H59A H 1.8174 0.2433 1.1209 0.039 Uiso 1 1 calc R . . H59B H 1.7818 0.1673 1.1639 0.039 Uiso 1 1 calc R . . C60 C 1.7777(3) 0.1853(3) 1.0477(3) 0.0251(10) Uani 1 1 d . . . H60A H 1.7729 0.2369 1.0021 0.030 Uiso 1 1 calc R . . H60B H 1.8402 0.1288 1.0530 0.030 Uiso 1 1 calc R . . N1 N 1.1148(2) 0.1709(2) 0.61641(19) 0.0159(7) Uani 1 1 d . . . N2 N 1.2494(2) 0.1580(2) 0.57011(18) 0.0147(7) Uani 1 1 d . . . N3 N 1.0455(2) 0.1869(2) 0.49254(19) 0.0167(7) Uani 1 1 d . . . N4 N 1.1726(2) 0.1910(2) 0.44353(19) 0.0183(7) Uani 1 1 d . . . N5 N 1.3299(2) 0.2539(2) 0.51515(18) 0.0163(7) Uani 1 1 d . . . N6 N 1.3100(2) 0.4058(2) 0.48172(18) 0.0135(7) Uani 1 1 d . . . N7 N 1.2519(2) 0.2887(2) 0.38891(19) 0.0161(7) Uani 1 1 d . . . N8 N 1.2504(2) 0.4340(2) 0.35013(19) 0.0167(7) Uani 1 1 d . . . N9 N 1.2268(2) 0.5810(2) 0.46477(18) 0.0154(7) Uani 1 1 d . . . N10 N 1.1109(2) 0.7229(2) 0.47098(19) 0.0171(7) Uani 1 1 d . . . N11 N 1.1688(2) 0.6108(2) 0.33334(18) 0.0158(7) Uani 1 1 d . . . N12 N 1.0431(2) 0.7429(2) 0.34524(18) 0.0149(7) Uani 1 1 d . . . N13 N 1.1910(2) 0.0860(2) 0.91867(18) 0.0165(7) Uani 1 1 d . . . N14 N 1.1588(2) 0.2299(2) 0.93511(19) 0.0169(7) Uani 1 1 d . . . N15 N 1.1977(2) 0.0156(2) 1.05594(19) 0.0190(7) Uani 1 1 d . . . N16 N 1.1828(2) 0.1535(2) 1.07333(19) 0.0195(7) Uani 1 1 d . . . N17 N 1.2356(2) 0.3252(2) 0.95382(19) 0.0171(7) Uani 1 1 d . . . N18 N 1.3747(2) 0.3248(2) 0.96397(18) 0.0168(7) Uani 1 1 d . . . N19 N 1.2591(2) 0.2501(2) 1.09127(19) 0.0191(7) Uani 1 1 d . . . N20 N 1.3925(2) 0.2618(2) 1.10218(19) 0.0187(7) Uani 1 1 d . . . N21 N 1.5473(2) 0.2554(2) 0.96654(19) 0.0170(7) Uani 1 1 d . . . N22 N 1.6931(2) 0.1427(2) 0.96166(19) 0.0189(7) Uani 1 1 d . . . N23 N 1.5651(2) 0.1933(2) 1.10468(19) 0.0184(7) Uani 1 1 d . . . N24 N 1.7073(2) 0.0736(2) 1.09922(18) 0.0172(7) Uani 1 1 d . . . O1 O 1.20787(19) 0.2172(2) 0.67461(15) 0.0197(6) Uani 1 1 d . . . O2 O 1.30196(19) 0.3351(2) 0.60668(15) 0.0185(6) Uani 1 1 d . . . O3 O 1.1768(2) 0.5977(2) 0.58215(16) 0.0246(7) Uani 1 1 d . . . O4 O 1.0299(2) 0.2729(2) 0.36534(16) 0.0254(7) Uani 1 1 d . . . O5 O 1.1361(2) 0.4122(2) 0.29329(18) 0.0295(7) Uani 1 1 d . . . O6 O 1.02450(19) 0.6614(2) 0.26475(16) 0.0211(6) Uani 1 1 d . . . O7 O 1.2343(2) 0.1880(2) 0.83200(16) 0.0214(6) Uani 1 1 d . . . O8 O 1.32638(19) 0.3032(2) 0.85469(15) 0.0201(6) Uani 1 1 d . . . O9 O 1.5808(2) 0.2031(2) 0.85804(16) 0.0234(7) Uani 1 1 d . . . O10 O 1.2621(2) 0.0107(2) 1.17007(17) 0.0258(7) Uani 1 1 d . . . O11 O 1.3764(2) 0.1389(2) 1.18972(17) 0.0297(7) Uani 1 1 d . . . O12 O 1.6233(2) 0.0463(2) 1.19967(16) 0.0231(7) Uani 1 1 d . . . N25 N 0.9906(3) 1.0549(3) 0.1961(2) 0.0317(9) Uani 1 1 d . . . N26 N 0.5940(3) 0.4356(3) 0.8347(3) 0.0413(11) Uani 1 1 d . . . N27 N 1.5670(3) 0.2185(3) 0.5851(3) 0.0385(10) Uani 1 1 d . . . O13 O 0.9543(3) 1.0459(3) 0.2568(2) 0.0478(10) Uani 1 1 d . . . O14 O 0.9903(3) 1.0093(3) 0.1510(2) 0.0509(10) Uani 1 1 d . . . O15 O 1.0277(3) 1.1099(3) 0.1815(2) 0.0557(11) Uani 1 1 d . . . O16 O 0.5351(3) 0.4941(3) 0.8678(2) 0.0557(11) Uani 1 1 d . . . O17 O 0.6733(3) 0.3705(3) 0.8685(3) 0.0620(12) Uani 1 1 d . . . O18 O 0.5752(4) 0.4444(4) 0.7678(3) 0.0778(15) Uani 1 1 d . . . O19 O 1.5476(4) 0.1700(3) 0.6419(3) 0.0730(15) Uani 1 1 d . . . O20 O 1.5269(3) 0.3090(3) 0.5699(2) 0.0514(10) Uani 1 1 d . . . O21 O 1.6240(3) 0.1774(3) 0.5450(3) 0.0679(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.0296(16) 0.0180(14) 0.0216(16) -0.0007(12) -0.0065(13) -0.0109(13) O2W 0.0271(16) 0.0200(15) 0.0255(17) -0.0032(13) -0.0006(13) -0.0113(13) O3W 0.0223(15) 0.0300(17) 0.0377(19) -0.0128(15) 0.0011(14) -0.0127(14) O4W 0.0204(15) 0.0332(17) 0.0219(16) -0.0073(13) -0.0026(12) -0.0145(13) Tb1 0.02108(12) 0.02158(12) 0.01250(12) -0.00480(8) -0.00102(8) -0.01146(9) C1 0.021(2) 0.0142(19) 0.010(2) -0.0026(16) -0.0018(16) -0.0079(16) C2 0.0167(19) 0.0152(19) 0.014(2) -0.0061(16) -0.0041(16) -0.0063(16) C3 0.0174(19) 0.0150(19) 0.011(2) -0.0053(16) -0.0015(16) -0.0068(16) C4 0.022(2) 0.019(2) 0.019(2) -0.0117(18) 0.0024(18) -0.0106(17) C5 0.0153(19) 0.0160(19) 0.0081(19) -0.0033(15) -0.0031(15) -0.0042(16) C6 0.028(2) 0.025(2) 0.015(2) -0.0114(18) 0.0036(18) -0.0150(19) C7 0.0115(18) 0.019(2) 0.016(2) -0.0044(16) -0.0028(16) -0.0067(16) C8 0.0131(19) 0.018(2) 0.014(2) -0.0043(16) 0.0003(16) -0.0044(16) C9 0.019(2) 0.017(2) 0.009(2) -0.0030(16) -0.0023(16) -0.0051(16) C10 0.020(2) 0.022(2) 0.012(2) -0.0066(17) 0.0024(17) -0.0063(17) C11 0.0168(19) 0.0156(19) 0.015(2) -0.0033(16) -0.0048(16) -0.0055(16) C12 0.020(2) 0.016(2) 0.009(2) 0.0007(16) -0.0033(16) -0.0031(16) C13 0.019(2) 0.019(2) 0.014(2) -0.0049(17) -0.0025(16) -0.0103(17) C14 0.0138(19) 0.017(2) 0.013(2) -0.0042(16) -0.0051(16) -0.0039(16) C15 0.0161(19) 0.018(2) 0.013(2) -0.0035(16) -0.0049(16) -0.0071(17) C16 0.017(2) 0.019(2) 0.011(2) 0.0004(16) -0.0014(16) -0.0098(17) C17 0.0161(19) 0.025(2) 0.017(2) -0.0073(17) -0.0042(16) -0.0104(17) C18 0.0138(18) 0.017(2) 0.010(2) -0.0025(16) -0.0015(15) -0.0037(16) C19 0.030(2) 0.021(2) 0.023(2) -0.0093(18) 0.0052(19) -0.0148(19) C20 0.033(2) 0.017(2) 0.027(3) -0.0029(19) 0.001(2) -0.0067(19) C21 0.028(2) 0.018(2) 0.036(3) -0.006(2) -0.003(2) -0.0033(19) C22 0.021(2) 0.024(2) 0.023(2) -0.0117(18) 0.0006(18) -0.0097(18) C23 0.018(2) 0.019(2) 0.021(2) -0.0097(18) 0.0000(17) -0.0021(17) C24 0.019(2) 0.030(2) 0.020(2) -0.0125(19) 0.0033(18) -0.0045(18) C25 0.027(2) 0.035(3) 0.020(2) -0.009(2) 0.0089(19) -0.009(2) C26 0.018(2) 0.025(2) 0.020(2) -0.0025(18) -0.0003(17) -0.0088(18) C27 0.019(2) 0.022(2) 0.023(2) -0.0028(18) 0.0022(18) -0.0089(18) C28 0.031(2) 0.026(2) 0.025(3) 0.000(2) 0.005(2) -0.011(2) C29 0.028(2) 0.022(2) 0.025(2) 0.0007(19) 0.0000(19) -0.0099(19) C30 0.017(2) 0.017(2) 0.026(2) -0.0035(18) -0.0038(17) -0.0087(17) C31 0.0150(19) 0.022(2) 0.010(2) -0.0012(16) -0.0043(16) -0.0081(17) C32 0.021(2) 0.023(2) 0.015(2) -0.0068(17) 0.0028(17) -0.0117(18) C33 0.021(2) 0.024(2) 0.014(2) -0.0041(17) 0.0014(17) -0.0124(18) C34 0.023(2) 0.027(2) 0.015(2) -0.0069(18) 0.0042(18) -0.0136(18) C35 0.017(2) 0.021(2) 0.016(2) -0.0040(17) -0.0012(16) -0.0096(17) C36 0.030(2) 0.030(2) 0.012(2) -0.0115(18) 0.0051(18) -0.014(2) C37 0.019(2) 0.0139(19) 0.010(2) -0.0002(15) -0.0060(16) -0.0089(16) C38 0.025(2) 0.017(2) 0.010(2) -0.0071(16) -0.0011(16) -0.0073(17) C39 0.022(2) 0.018(2) 0.014(2) -0.0044(17) -0.0022(17) -0.0064(17) C40 0.027(2) 0.022(2) 0.016(2) -0.0101(18) 0.0019(18) -0.0103(19) C41 0.023(2) 0.022(2) 0.015(2) -0.0019(17) -0.0028(17) -0.0130(18) C42 0.024(2) 0.026(2) 0.012(2) -0.0079(17) -0.0034(17) -0.0089(18) C43 0.022(2) 0.018(2) 0.019(2) 0.0010(17) -0.0034(18) -0.0135(18) C44 0.023(2) 0.017(2) 0.015(2) -0.0033(17) -0.0036(17) -0.0094(17) C45 0.024(2) 0.020(2) 0.015(2) -0.0045(17) -0.0020(17) -0.0122(18) C46 0.023(2) 0.021(2) 0.017(2) -0.0089(18) -0.0031(17) -0.0098(18) C47 0.025(2) 0.022(2) 0.011(2) -0.0026(16) -0.0023(17) -0.0119(18) C48 0.025(2) 0.020(2) 0.015(2) -0.0030(17) 0.0025(17) -0.0136(18) C49 0.022(2) 0.023(2) 0.021(2) -0.0019(18) 0.0014(18) -0.0133(18) C50 0.023(2) 0.037(3) 0.026(3) -0.004(2) -0.0018(19) -0.017(2) C51 0.021(2) 0.030(2) 0.036(3) -0.004(2) -0.002(2) -0.008(2) C52 0.015(2) 0.027(2) 0.022(2) -0.0055(19) 0.0012(17) -0.0058(18) C53 0.024(2) 0.021(2) 0.028(3) -0.0103(19) 0.0062(19) -0.0053(18) C54 0.057(3) 0.029(3) 0.032(3) -0.021(2) 0.011(2) -0.014(2) C55 0.048(3) 0.032(3) 0.034(3) -0.023(2) -0.006(2) -0.006(2) C56 0.035(2) 0.016(2) 0.029(3) -0.0115(19) -0.007(2) -0.0092(19) C57 0.026(2) 0.022(2) 0.027(3) -0.0099(19) -0.0045(19) -0.0111(19) C58 0.035(3) 0.034(3) 0.037(3) -0.019(2) -0.008(2) -0.017(2) C59 0.036(3) 0.033(3) 0.034(3) -0.011(2) -0.009(2) -0.018(2) C60 0.023(2) 0.025(2) 0.026(2) -0.0020(19) -0.0083(19) -0.0131(19) N1 0.0158(16) 0.0186(17) 0.0156(18) -0.0071(14) 0.0005(14) -0.0086(14) N2 0.0169(16) 0.0211(17) 0.0107(17) -0.0087(14) -0.0014(13) -0.0104(14) N3 0.0138(16) 0.0193(17) 0.0180(18) -0.0093(14) -0.0009(14) -0.0063(14) N4 0.0209(17) 0.0238(18) 0.0105(17) -0.0051(14) -0.0002(14) -0.0105(15) N5 0.0223(17) 0.0162(17) 0.0104(17) -0.0054(14) 0.0007(14) -0.0079(14) N6 0.0163(16) 0.0138(16) 0.0085(16) -0.0037(13) -0.0019(13) -0.0049(13) N7 0.0195(17) 0.0188(17) 0.0123(17) -0.0055(14) -0.0031(14) -0.0102(14) N8 0.0161(16) 0.0184(17) 0.0128(18) -0.0044(14) -0.0034(13) -0.0056(14) N9 0.0136(16) 0.0154(16) 0.0124(17) -0.0004(13) -0.0040(13) -0.0043(13) N10 0.0166(16) 0.0177(17) 0.0131(18) -0.0061(14) -0.0040(13) -0.0036(14) N11 0.0157(16) 0.0186(17) 0.0114(17) -0.0073(14) -0.0021(13) -0.0048(14) N12 0.0127(16) 0.0185(17) 0.0122(17) -0.0045(14) -0.0042(13) -0.0059(14) N13 0.0225(17) 0.0193(17) 0.0118(17) -0.0044(14) 0.0028(14) -0.0130(15) N14 0.0183(17) 0.0180(17) 0.0121(17) -0.0012(14) 0.0000(14) -0.0081(14) N15 0.0232(18) 0.0197(18) 0.0105(17) -0.0010(14) -0.0016(14) -0.0084(15) N16 0.0245(18) 0.0208(18) 0.0133(18) -0.0045(14) -0.0001(14) -0.0107(15) N17 0.0164(17) 0.0199(17) 0.0136(18) -0.0041(14) -0.0022(14) -0.0074(14) N18 0.0217(17) 0.0214(17) 0.0114(18) -0.0064(14) -0.0008(14) -0.0125(15) N19 0.0289(19) 0.0180(17) 0.0101(17) -0.0044(14) -0.0042(14) -0.0104(15) N20 0.0217(18) 0.0203(17) 0.0123(18) -0.0067(14) -0.0011(14) -0.0068(15) N21 0.0195(17) 0.0181(17) 0.0132(18) -0.0057(14) -0.0046(14) -0.0078(14) N22 0.0185(17) 0.0203(17) 0.0149(18) -0.0036(14) -0.0029(14) -0.0070(15) N23 0.0196(17) 0.0189(17) 0.0125(18) -0.0021(14) -0.0022(14) -0.0065(14) N24 0.0219(17) 0.0146(16) 0.0119(17) -0.0019(13) -0.0015(14) -0.0067(14) O1 0.0228(15) 0.0292(16) 0.0120(15) -0.0116(12) 0.0003(12) -0.0130(13) O2 0.0280(15) 0.0231(15) 0.0082(15) -0.0064(11) 0.0008(12) -0.0138(13) O3 0.0280(16) 0.0238(15) 0.0150(16) -0.0032(13) -0.0008(12) -0.0071(13) O4 0.0250(15) 0.0316(17) 0.0137(16) -0.0012(13) -0.0071(13) -0.0107(14) O5 0.0283(17) 0.0288(17) 0.0268(18) -0.0056(14) -0.0144(14) -0.0100(14) O6 0.0194(14) 0.0248(15) 0.0207(16) -0.0099(13) -0.0012(12) -0.0095(12) O7 0.0319(16) 0.0242(15) 0.0152(15) -0.0077(12) 0.0044(13) -0.0177(13) O8 0.0229(15) 0.0284(16) 0.0110(15) -0.0048(12) 0.0003(12) -0.0141(13) O9 0.0252(15) 0.0305(17) 0.0128(16) -0.0063(13) -0.0052(12) -0.0110(13) O10 0.0292(16) 0.0264(16) 0.0167(17) -0.0016(13) -0.0059(13) -0.0108(14) O11 0.0379(18) 0.0260(16) 0.0197(17) 0.0024(14) -0.0059(14) -0.0145(14) O12 0.0300(16) 0.0203(15) 0.0153(15) -0.0017(12) 0.0018(12) -0.0103(13) N25 0.030(2) 0.035(2) 0.020(2) 0.0010(18) -0.0032(17) -0.0115(19) N26 0.056(3) 0.040(3) 0.035(3) -0.007(2) 0.007(2) -0.030(2) N27 0.040(2) 0.043(3) 0.037(3) -0.014(2) 0.006(2) -0.022(2) O13 0.050(2) 0.049(2) 0.035(2) 0.0009(17) 0.0113(18) -0.0217(19) O14 0.050(2) 0.060(3) 0.040(2) -0.023(2) -0.0097(18) -0.018(2) O15 0.058(3) 0.064(3) 0.059(3) -0.009(2) 0.010(2) -0.044(2) O16 0.063(3) 0.051(2) 0.052(3) -0.024(2) 0.020(2) -0.021(2) O17 0.059(3) 0.061(3) 0.059(3) -0.015(2) -0.001(2) -0.023(2) O18 0.092(4) 0.080(3) 0.041(3) -0.028(2) -0.003(2) -0.016(3) O19 0.109(4) 0.054(3) 0.067(3) -0.027(2) 0.047(3) -0.043(3) O20 0.056(2) 0.037(2) 0.051(3) -0.0131(18) -0.0013(19) -0.0119(19) O21 0.079(3) 0.057(3) 0.065(3) -0.034(2) 0.044(3) -0.021(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 O1W Tb1 2.396(3) . ? O2W Tb1 2.355(3) . ? O3W Tb1 2.339(3) . ? O4W Tb1 2.405(3) . ? Tb1 O2 2.339(3) . ? Tb1 O8 2.374(3) . ? Tb1 O7 2.396(3) . ? Tb1 O1 2.412(3) . ? C1 O1 1.229(5) . ? C1 N1 1.358(5) . ? C1 N2 1.360(5) . ? C2 N3 1.441(5) . ? C2 N1 1.470(5) . ? C2 C19 1.524(5) . ? C2 C3 1.575(5) . ? C3 N4 1.452(5) . ? C3 N2 1.472(5) . ? C3 C22 1.511(5) . ? C4 O4 1.219(5) . ? C4 N3 1.368(5) . ? C4 N4 1.369(5) . ? C5 N2 1.427(5) . ? C5 N5 1.455(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.442(5) . ? C6 N4 1.450(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.235(5) . ? C7 N5 1.344(5) . ? C7 N6 1.347(5) . ? C8 N5 1.440(5) . ? C8 N7 1.460(5) . ? C8 C23 1.541(5) . ? C8 C9 1.566(5) . ? C9 N8 1.459(5) . ? C9 N6 1.478(5) . ? C9 C26 1.513(5) . ? C10 O5 1.211(5) . ? C10 N8 1.367(5) . ? C10 N7 1.380(5) . ? C11 N6 1.436(5) . ? C11 N9 1.452(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.442(5) . ? C12 N8 1.454(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.208(5) . ? C13 N9 1.367(5) . ? C13 N10 1.370(5) . ? C14 N11 1.443(5) . ? C14 N9 1.469(5) . ? C14 C27 1.528(5) . ? C14 C15 1.581(5) . ? C15 N10 1.444(5) . ? C15 N12 1.467(5) . ? C15 C30 1.519(5) . ? C16 O6 1.227(5) . ? C16 N12 1.347(5) . ? C16 N11 1.376(5) . ? C17 N10 1.446(5) . ? C17 N3 1.455(5) 2_766 ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.449(5) . ? C18 N12 1.459(5) 2_766 ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.510(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.539(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.529(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.518(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.525(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.524(6) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.520(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.535(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.515(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O7 1.229(5) . ? C31 N14 1.352(5) . ? C31 N13 1.356(5) . ? C32 N15 1.452(5) . ? C32 N13 1.477(5) . ? C32 C49 1.523(6) . ? C32 C33 1.564(6) . ? C33 N16 1.458(5) . ? C33 N14 1.463(5) . ? C33 C52 1.520(5) . ? C34 O10 1.209(5) . ? C34 N16 1.359(5) . ? C34 N15 1.370(5) . ? C35 N14 1.436(5) . ? C35 N17 1.454(5) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N19 1.442(5) . ? C36 N16 1.455(5) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O8 1.223(5) . ? C37 N17 1.348(5) . ? C37 N18 1.367(5) . ? C38 N17 1.451(5) . ? C38 N19 1.464(5) . ? C38 C53 1.525(5) . ? C38 C39 1.557(6) . ? C39 N18 1.445(5) . ? C39 N20 1.457(5) . ? C39 C56 1.538(6) . ? C40 O11 1.214(5) . ? C40 N20 1.360(5) . ? C40 N19 1.371(6) . ? C41 N18 1.447(5) . ? C41 N21 1.448(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N23 1.444(5) . ? C42 N20 1.453(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 O9 1.212(5) . ? C43 N21 1.361(5) . ? C43 N22 1.374(5) . ? C44 N23 1.464(5) . ? C44 N21 1.466(5) . ? C44 C57 1.504(6) . ? C44 C45 1.576(6) . ? C45 N22 1.452(5) . ? C45 N24 1.463(5) . ? C45 C60 1.511(6) . ? C46 O12 1.219(5) . ? C46 N24 1.368(5) . ? C46 N23 1.378(5) . ? C47 N24 1.446(5) 2_857 ? C47 N13 1.452(5) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 N15 1.434(5) . ? C48 N22 1.453(5) 2_857 ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.538(6) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.533(7) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.527(6) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.522(7) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.513(8) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.536(7) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C58 1.522(6) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 C59 1.534(6) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 C60 1.512(7) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? N3 C17 1.455(5) 2_766 ? N12 C18 1.459(5) 2_766 ? N22 C48 1.453(5) 2_857 ? N24 C47 1.446(5) 2_857 ? N25 O14 1.231(5) . ? N25 O15 1.234(5) . ? N25 O13 1.242(5) . ? N26 O18 1.212(6) . ? N26 O17 1.247(6) . ? N26 O16 1.265(6) . ? N27 O21 1.215(5) . ? N27 O20 1.241(5) . ? N27 O19 1.243(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3W Tb1 O2 97.35(10) . . ? O3W Tb1 O2W 139.92(10) . . ? O2 Tb1 O2W 94.54(10) . . ? O3W Tb1 O8 96.86(10) . . ? O2 Tb1 O8 138.21(9) . . ? O2W Tb1 O8 99.30(10) . . ? O3W Tb1 O1W 72.04(10) . . ? O2 Tb1 O1W 75.60(10) . . ? O2W Tb1 O1W 148.00(10) . . ? O8 Tb1 O1W 71.87(10) . . ? O3W Tb1 O7 76.20(10) . . ? O2 Tb1 O7 146.35(10) . . ? O2W Tb1 O7 72.87(9) . . ? O8 Tb1 O7 75.35(9) . . ? O1W Tb1 O7 130.44(10) . . ? O3W Tb1 O4W 147.39(10) . . ? O2 Tb1 O4W 75.01(10) . . ? O2W Tb1 O4W 72.69(10) . . ? O8 Tb1 O4W 71.96(9) . . ? O1W Tb1 O4W 75.35(10) . . ? O7 Tb1 O4W 127.02(10) . . ? O3W Tb1 O1 72.52(10) . . ? O2 Tb1 O1 75.88(9) . . ? O2W Tb1 O1 73.58(10) . . ? O8 Tb1 O1 145.89(9) . . ? O1W Tb1 O1 130.49(10) . . ? O7 Tb1 O1 70.66(9) . . ? O4W Tb1 O1 132.87(10) . . ? O1 C1 N1 125.1(3) . . ? O1 C1 N2 125.0(4) . . ? N1 C1 N2 109.8(3) . . ? N3 C2 N1 112.3(3) . . ? N3 C2 C19 114.3(3) . . ? N1 C2 C19 112.2(3) . . ? N3 C2 C3 102.5(3) . . ? N1 C2 C3 102.7(3) . . ? C19 C2 C3 111.7(3) . . ? N4 C3 N2 112.6(3) . . ? N4 C3 C22 113.3(3) . . ? N2 C3 C22 112.4(3) . . ? N4 C3 C2 102.7(3) . . ? N2 C3 C2 102.7(3) . . ? C22 C3 C2 112.2(3) . . ? O4 C4 N3 126.5(4) . . ? O4 C4 N4 125.7(4) . . ? N3 C4 N4 107.8(3) . . ? N2 C5 N5 114.6(3) . . ? N2 C5 H5A 108.6 . . ? N5 C5 H5A 108.6 . . ? N2 C5 H5B 108.6 . . ? N5 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? N7 C6 N4 114.4(3) . . ? N7 C6 H6A 108.6 . . ? N4 C6 H6A 108.6 . . ? N7 C6 H6B 108.6 . . ? N4 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N5 124.9(4) . . ? O2 C7 N6 124.6(4) . . ? N5 C7 N6 110.5(3) . . ? N5 C8 N7 113.7(3) . . ? N5 C8 C23 112.9(3) . . ? N7 C8 C23 111.0(3) . . ? N5 C8 C9 103.7(3) . . ? N7 C8 C9 102.9(3) . . ? C23 C8 C9 112.0(3) . . ? N8 C9 N6 112.0(3) . . ? N8 C9 C26 113.3(3) . . ? N6 C9 C26 112.8(3) . . ? N8 C9 C8 103.3(3) . . ? N6 C9 C8 101.6(3) . . ? C26 C9 C8 112.8(3) . . ? O5 C10 N8 125.7(4) . . ? O5 C10 N7 125.7(4) . . ? N8 C10 N7 108.5(3) . . ? N6 C11 N9 114.6(3) . . ? N6 C11 H11A 108.6 . . ? N9 C11 H11A 108.6 . . ? N6 C11 H11B 108.6 . . ? N9 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? N11 C12 N8 115.9(3) . . ? N11 C12 H12A 108.3 . . ? N8 C12 H12A 108.3 . . ? N11 C12 H12B 108.3 . . ? N8 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? O3 C13 N9 126.8(4) . . ? O3 C13 N10 125.1(4) . . ? N9 C13 N10 108.1(3) . . ? N11 C14 N9 112.3(3) . . ? N11 C14 C27 114.1(3) . . ? N9 C14 C27 112.9(3) . . ? N11 C14 C15 103.5(3) . . ? N9 C14 C15 101.9(3) . . ? C27 C14 C15 111.0(3) . . ? N10 C15 N12 112.4(3) . . ? N10 C15 C30 113.2(3) . . ? N12 C15 C30 113.4(3) . . ? N10 C15 C14 103.1(3) . . ? N12 C15 C14 101.6(3) . . ? C30 C15 C14 112.1(3) . . ? O6 C16 N12 126.2(3) . . ? O6 C16 N11 124.8(4) . . ? N12 C16 N11 109.0(3) . . ? N10 C17 N3 113.9(3) . 2_766 ? N10 C17 H17A 108.8 . . ? N3 C17 H17A 108.8 2_766 . ? N10 C17 H17B 108.8 . . ? N3 C17 H17B 108.8 2_766 . ? H17A C17 H17B 107.7 . . ? N1 C18 N12 114.8(3) . 2_766 ? N1 C18 H18A 108.6 . . ? N12 C18 H18A 108.6 2_766 . ? N1 C18 H18B 108.6 . . ? N12 C18 H18B 108.6 2_766 . ? H18A C18 H18B 107.5 . . ? C20 C19 C2 110.6(3) . . ? C20 C19 H19A 109.5 . . ? C2 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? C2 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C19 C20 C21 112.9(4) . . ? C19 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? C19 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C20 112.3(4) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C3 C22 C21 111.5(3) . . ? C3 C22 H22A 109.3 . . ? C21 C22 H22A 109.3 . . ? C3 C22 H22B 109.3 . . ? C21 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C8 109.9(3) . . ? C24 C23 H23A 109.7 . . ? C8 C23 H23A 109.7 . . ? C24 C23 H23B 109.7 . . ? C8 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? C23 C24 C25 112.3(4) . . ? C23 C24 H24A 109.1 . . ? C25 C24 H24A 109.1 . . ? C23 C24 H24B 109.1 . . ? C25 C24 H24B 109.1 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C24 113.7(3) . . ? C26 C25 H25A 108.8 . . ? C24 C25 H25A 108.8 . . ? C26 C25 H25B 108.8 . . ? C24 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C9 C26 C25 112.2(4) . . ? C9 C26 H26A 109.2 . . ? C25 C26 H26A 109.2 . . ? C9 C26 H26B 109.2 . . ? C25 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C28 C27 C14 112.3(3) . . ? C28 C27 H27A 109.2 . . ? C14 C27 H27A 109.2 . . ? C28 C27 H27B 109.2 . . ? C14 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C29 113.2(3) . . ? C27 C28 H28A 108.9 . . ? C29 C28 H28A 108.9 . . ? C27 C28 H28B 108.9 . . ? C29 C28 H28B 108.9 . . ? H28A C28 H28B 107.8 . . ? C30 C29 C28 111.6(4) . . ? C30 C29 H29A 109.3 . . ? C28 C29 H29A 109.3 . . ? C30 C29 H29B 109.3 . . ? C28 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? C29 C30 C15 111.3(4) . . ? C29 C30 H30A 109.4 . . ? C15 C30 H30A 109.4 . . ? C29 C30 H30B 109.4 . . ? C15 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? O7 C31 N14 125.3(4) . . ? O7 C31 N13 124.4(4) . . ? N14 C31 N13 110.2(3) . . ? N15 C32 N13 112.5(3) . . ? N15 C32 C49 113.5(3) . . ? N13 C32 C49 111.8(3) . . ? N15 C32 C33 103.1(3) . . ? N13 C32 C33 103.1(3) . . ? C49 C32 C33 112.1(3) . . ? N16 C33 N14 113.3(3) . . ? N16 C33 C52 113.2(3) . . ? N14 C33 C52 111.9(3) . . ? N16 C33 C32 102.5(3) . . ? N14 C33 C32 102.6(3) . . ? C52 C33 C32 112.6(3) . . ? O10 C34 N16 126.5(4) . . ? O10 C34 N15 125.2(4) . . ? N16 C34 N15 108.3(4) . . ? N14 C35 N17 113.6(3) . . ? N14 C35 H35A 108.8 . . ? N17 C35 H35A 108.8 . . ? N14 C35 H35B 108.8 . . ? N17 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? N19 C36 N16 113.9(3) . . ? N19 C36 H36A 108.8 . . ? N16 C36 H36A 108.8 . . ? N19 C36 H36B 108.8 . . ? N16 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? O8 C37 N17 125.8(4) . . ? O8 C37 N18 125.1(3) . . ? N17 C37 N18 109.1(3) . . ? N17 C38 N19 112.5(3) . . ? N17 C38 C53 112.2(3) . . ? N19 C38 C53 112.4(3) . . ? N17 C38 C39 102.6(3) . . ? N19 C38 C39 103.1(3) . . ? C53 C38 C39 113.3(3) . . ? N18 C39 N20 112.8(3) . . ? N18 C39 C56 112.7(3) . . ? N20 C39 C56 112.6(4) . . ? N18 C39 C38 103.4(3) . . ? N20 C39 C38 103.0(3) . . ? C56 C39 C38 111.5(3) . . ? O11 C40 N20 125.8(4) . . ? O11 C40 N19 125.4(4) . . ? N20 C40 N19 108.8(3) . . ? N18 C41 N21 115.1(3) . . ? N18 C41 H41A 108.5 . . ? N21 C41 H41A 108.5 . . ? N18 C41 H41B 108.5 . . ? N21 C41 H41B 108.5 . . ? H41A C41 H41B 107.5 . . ? N23 C42 N20 115.1(3) . . ? N23 C42 H42A 108.5 . . ? N20 C42 H42A 108.5 . . ? N23 C42 H42B 108.5 . . ? N20 C42 H42B 108.5 . . ? H42A C42 H42B 107.5 . . ? O9 C43 N21 126.8(4) . . ? O9 C43 N22 124.6(4) . . ? N21 C43 N22 108.5(4) . . ? N23 C44 N21 111.0(3) . . ? N23 C44 C57 113.4(3) . . ? N21 C44 C57 113.6(3) . . ? N23 C44 C45 103.2(3) . . ? N21 C44 C45 102.6(3) . . ? C57 C44 C45 112.1(3) . . ? N22 C45 N24 112.4(3) . . ? N22 C45 C60 113.3(3) . . ? N24 C45 C60 113.3(3) . . ? N22 C45 C44 102.8(3) . . ? N24 C45 C44 102.5(3) . . ? C60 C45 C44 111.4(3) . . ? O12 C46 N24 126.3(4) . . ? O12 C46 N23 125.2(4) . . ? N24 C46 N23 108.4(3) . . ? N24 C47 N13 114.3(3) 2_857 . ? N24 C47 H47A 108.7 2_857 . ? N13 C47 H47A 108.7 . . ? N24 C47 H47B 108.7 2_857 . ? N13 C47 H47B 108.7 . . ? H47A C47 H47B 107.6 . . ? N15 C48 N22 115.6(3) . 2_857 ? N15 C48 H48A 108.4 . . ? N22 C48 H48A 108.4 2_857 . ? N15 C48 H48B 108.4 . . ? N22 C48 H48B 108.4 2_857 . ? H48A C48 H48B 107.4 . . ? C32 C49 C50 110.2(3) . . ? C32 C49 H49A 109.6 . . ? C50 C49 H49A 109.6 . . ? C32 C49 H49B 109.6 . . ? C50 C49 H49B 109.6 . . ? H49A C49 H49B 108.1 . . ? C51 C50 C49 111.9(4) . . ? C51 C50 H50A 109.2 . . ? C49 C50 H50A 109.2 . . ? C51 C50 H50B 109.2 . . ? C49 C50 H50B 109.2 . . ? H50A C50 H50B 107.9 . . ? C52 C51 C50 113.4(4) . . ? C52 C51 H51A 108.9 . . ? C50 C51 H51A 108.9 . . ? C52 C51 H51B 108.9 . . ? C50 C51 H51B 108.9 . . ? H51A C51 H51B 107.7 . . ? C33 C52 C51 111.3(4) . . ? C33 C52 H52A 109.4 . . ? C51 C52 H52A 109.4 . . ? C33 C52 H52B 109.4 . . ? C51 C52 H52B 109.4 . . ? H52A C52 H52B 108.0 . . ? C54 C53 C38 110.0(4) . . ? C54 C53 H53A 109.7 . . ? C38 C53 H53A 109.7 . . ? C54 C53 H53B 109.7 . . ? C38 C53 H53B 109.7 . . ? H53A C53 H53B 108.2 . . ? C55 C54 C53 112.8(4) . . ? C55 C54 H54A 109.0 . . ? C53 C54 H54A 109.0 . . ? C55 C54 H54B 109.0 . . ? C53 C54 H54B 109.0 . . ? H54A C54 H54B 107.8 . . ? C54 C55 C56 113.8(4) . . ? C54 C55 H55A 108.8 . . ? C56 C55 H55A 108.8 . . ? C54 C55 H55B 108.8 . . ? C56 C55 H55B 108.8 . . ? H55A C55 H55B 107.7 . . ? C55 C56 C39 110.4(4) . . ? C55 C56 H56A 109.6 . . ? C39 C56 H56A 109.6 . . ? C55 C56 H56B 109.6 . . ? C39 C56 H56B 109.6 . . ? H56A C56 H56B 108.1 . . ? C44 C57 C58 111.3(4) . . ? C44 C57 H57A 109.4 . . ? C58 C57 H57A 109.4 . . ? C44 C57 H57B 109.4 . . ? C58 C57 H57B 109.4 . . ? H57A C57 H57B 108.0 . . ? C57 C58 C59 112.6(4) . . ? C57 C58 H58A 109.1 . . ? C59 C58 H58A 109.1 . . ? C57 C58 H58B 109.1 . . ? C59 C58 H58B 109.1 . . ? H58A C58 H58B 107.8 . . ? C60 C59 C58 112.4(4) . . ? C60 C59 H59A 109.1 . . ? C58 C59 H59A 109.1 . . ? C60 C59 H59B 109.1 . . ? C58 C59 H59B 109.1 . . ? H59A C59 H59B 107.9 . . ? C45 C60 C59 111.8(4) . . ? C45 C60 H60A 109.3 . . ? C59 C60 H60A 109.3 . . ? C45 C60 H60B 109.3 . . ? C59 C60 H60B 109.3 . . ? H60A C60 H60B 107.9 . . ? C1 N1 C18 120.7(3) . . ? C1 N1 C2 112.3(3) . . ? C18 N1 C2 124.9(3) . . ? C1 N2 C5 122.6(3) . . ? C1 N2 C3 112.2(3) . . ? C5 N2 C3 125.2(3) . . ? C4 N3 C2 113.7(3) . . ? C4 N3 C17 120.7(3) . 2_766 ? C2 N3 C17 125.2(3) . 2_766 ? C4 N4 C6 120.6(3) . . ? C4 N4 C3 112.8(3) . . ? C6 N4 C3 125.7(3) . . ? C7 N5 C8 112.1(3) . . ? C7 N5 C5 122.9(3) . . ? C8 N5 C5 125.0(3) . . ? C7 N6 C11 122.1(3) . . ? C7 N6 C9 111.5(3) . . ? C11 N6 C9 124.4(3) . . ? C10 N7 C6 121.1(3) . . ? C10 N7 C8 112.4(3) . . ? C6 N7 C8 125.6(3) . . ? C10 N8 C12 121.3(3) . . ? C10 N8 C9 112.6(3) . . ? C12 N8 C9 125.9(3) . . ? C13 N9 C11 120.4(3) . . ? C13 N9 C14 113.1(3) . . ? C11 N9 C14 123.7(3) . . ? C13 N10 C15 113.4(3) . . ? C13 N10 C17 121.0(3) . . ? C15 N10 C17 125.1(3) . . ? C16 N11 C12 121.9(3) . . ? C16 N11 C14 112.3(3) . . ? C12 N11 C14 125.5(3) . . ? C16 N12 C18 120.6(3) . 2_766 ? C16 N12 C15 113.3(3) . . ? C18 N12 C15 124.7(3) 2_766 . ? C31 N13 C47 121.0(3) . . ? C31 N13 C32 111.4(3) . . ? C47 N13 C32 125.4(3) . . ? C31 N14 C35 122.4(3) . . ? C31 N14 C33 112.5(3) . . ? C35 N14 C33 125.2(3) . . ? C34 N15 C48 121.1(3) . . ? C34 N15 C32 112.6(3) . . ? C48 N15 C32 126.1(3) . . ? C34 N16 C36 120.5(4) . . ? C34 N16 C33 112.9(3) . . ? C36 N16 C33 125.5(3) . . ? C37 N17 C38 112.8(3) . . ? C37 N17 C35 122.4(3) . . ? C38 N17 C35 124.8(3) . . ? C37 N18 C39 111.9(3) . . ? C37 N18 C41 120.8(3) . . ? C39 N18 C41 125.9(3) . . ? C40 N19 C36 121.2(3) . . ? C40 N19 C38 112.1(3) . . ? C36 N19 C38 126.1(3) . . ? C40 N20 C42 121.2(3) . . ? C40 N20 C39 112.8(3) . . ? C42 N20 C39 125.6(3) . . ? C43 N21 C41 120.6(3) . . ? C43 N21 C44 112.8(3) . . ? C41 N21 C44 124.5(3) . . ? C43 N22 C45 113.0(3) . . ? C43 N22 C48 121.4(3) . 2_857 ? C45 N22 C48 124.7(3) . 2_857 ? C46 N23 C42 120.9(3) . . ? C46 N23 C44 112.4(3) . . ? C42 N23 C44 125.6(3) . . ? C46 N24 C47 120.7(3) . 2_857 ? C46 N24 C45 113.1(3) . . ? C47 N24 C45 124.9(3) 2_857 . ? C1 O1 Tb1 156.1(3) . . ? C7 O2 Tb1 158.8(3) . . ? C31 O7 Tb1 155.1(3) . . ? C37 O8 Tb1 155.3(3) . . ? O14 N25 O15 120.1(4) . . ? O14 N25 O13 120.8(4) . . ? O15 N25 O13 119.1(5) . . ? O18 N26 O17 118.5(5) . . ? O18 N26 O16 120.1(5) . . ? O17 N26 O16 121.4(5) . . ? O21 N27 O20 120.8(4) . . ? O21 N27 O19 120.2(5) . . ? O20 N27 O19 119.0(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.276 _refine_diff_density_min -1.212 _refine_diff_density_rms 0.109 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.157 0.045 0.347 60 22 ' ' 2 -0.226 0.373 0.279 201 75 ' ' 3 0.000 0.500 0.500 107 25 ' ' 4 0.225 0.628 0.721 203 75 ' ' 5 -0.162 0.957 0.653 59 22 ' ' 6 0.500 0.000 0.000 115 29 ' ' 7 0.477 0.015 0.342 17 9 ' ' 8 0.523 0.985 0.658 16 8 ' ' _platon_squeeze_details ; ; data_a5 _database_code_depnum_ccdc_archive 'CCDC 881906' #TrackingRef '110621qx-submit-cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H136 Cl2 Lu2 N28 O56' _chemical_formula_weight 2566.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.7064(13) _cell_length_b 26.467(2) _cell_length_c 21.9800(16) _cell_angle_alpha 90.00 _cell_angle_beta 111.594(2) _cell_angle_gamma 90.00 _cell_volume 9577.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5264 _exptl_absorpt_coefficient_mu 2.226 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5745 _exptl_absorpt_correction_T_max 0.6061 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42116 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9283 _reflns_number_gt 7527 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+4.4089P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9283 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.007 _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 Cl1 Cl 0.1003(2) -0.09488(16) 0.12135(18) 0.2193(17) Uani 1 1 d . . . O1W O 0.44855(13) -0.13465(8) 0.30327(10) 0.0325(6) Uani 1 1 d . . . O2W O 0.46799(14) -0.04000(10) 0.35332(11) 0.0394(7) Uani 1 1 d . . . O3W O 0.40596(13) -0.00129(9) 0.22691(10) 0.0318(6) Uani 1 1 d . . . O4W O 0.24303(14) -0.04443(10) 0.18039(12) 0.0405(7) Uani 1 1 d . . . O5W O 0.27069(15) -0.13767(10) 0.23112(11) 0.0438(7) Uani 1 1 d . . . O6W O 0.38470(13) -0.09873(9) 0.17838(10) 0.0345(6) Uani 1 1 d . . . Lu1 Lu 0.355192(7) -0.067992(5) 0.266853(5) 0.02130(4) Uani 1 1 d . . . C1 C 0.29543(17) -0.10074(11) 0.39561(13) 0.0221(7) Uani 1 1 d . . . C2 C 0.27182(16) -0.12486(11) 0.48995(13) 0.0221(7) Uani 1 1 d . . . C3 C 0.21134(17) -0.08141(12) 0.45310(14) 0.0233(7) Uani 1 1 d . . . C4 C 0.29920(19) -0.05177(13) 0.55530(14) 0.0288(8) Uani 1 1 d . . . C5 C 0.18861(17) -0.03852(12) 0.34280(14) 0.0251(8) Uani 1 1 d . . . H5A H 0.1311 -0.0384 0.3372 0.030 Uiso 1 1 calc R . . H5B H 0.1923 -0.0510 0.3020 0.030 Uiso 1 1 calc R . . C6 C 0.1940(2) 0.00811(13) 0.49271(15) 0.0325(8) Uani 1 1 d . . . H6A H 0.2020 0.0211 0.5364 0.039 Uiso 1 1 calc R . . H6B H 0.1357 0.0024 0.4698 0.039 Uiso 1 1 calc R . . C7 C 0.27507(17) 0.02969(11) 0.33074(13) 0.0210(7) Uani 1 1 d . . . C8 C 0.18956(17) 0.05193(12) 0.38643(14) 0.0243(7) Uani 1 1 d . . . C9 C 0.23586(16) 0.10039(11) 0.37695(14) 0.0222(7) Uani 1 1 d . . . C10 C 0.27051(18) 0.08520(13) 0.48873(15) 0.0299(8) Uani 1 1 d . . . C11 C 0.33174(17) 0.10969(12) 0.31192(14) 0.0246(7) Uani 1 1 d . . . H11A H 0.3383 0.0897 0.2767 0.030 Uiso 1 1 calc R . . H11B H 0.2991 0.1394 0.2919 0.030 Uiso 1 1 calc R . . C12 C 0.32871(18) 0.16189(13) 0.46153(16) 0.0346(9) Uani 1 1 d . . . H12A H 0.3351 0.1705 0.5065 0.041 Uiso 1 1 calc R . . H12B H 0.2981 0.1893 0.4331 0.041 Uiso 1 1 calc R . . C13 C 0.48070(17) 0.10732(11) 0.35142(13) 0.0226(7) Uani 1 1 d . . . C14 C 0.42524(17) 0.17010(11) 0.39885(14) 0.0233(7) Uani 1 1 d . . . C15 C 0.52099(16) 0.17509(11) 0.42554(13) 0.0208(7) Uani 1 1 d . . . C16 C 0.54772(19) 0.22738(12) 0.41288(15) 0.0295(8) Uani 1 1 d . . . H16A H 0.6071 0.2281 0.4271 0.035 Uiso 1 1 calc R . . H16B H 0.5317 0.2523 0.4389 0.035 Uiso 1 1 calc R . . C16' C 0.47675(18) 0.15611(13) 0.51229(14) 0.0293(8) Uani 1 1 d . . . C17 C 0.62572(17) 0.12754(12) 0.39128(13) 0.0238(7) Uani 1 1 d . . . H17A H 0.6220 0.1086 0.3520 0.029 Uiso 1 1 calc R . . H17B H 0.6493 0.1606 0.3888 0.029 Uiso 1 1 calc R . . C18 C 0.62269(17) 0.17189(12) 0.54458(14) 0.0240(7) Uani 1 1 d . . . H18A H 0.6449 0.2031 0.5340 0.029 Uiso 1 1 calc R . . H18B H 0.6167 0.1770 0.5867 0.029 Uiso 1 1 calc R . . C19 C 0.22735(18) -0.17219(12) 0.49697(14) 0.0263(8) Uani 1 1 d . . . H19A H 0.2667 -0.1970 0.5238 0.032 Uiso 1 1 calc R . . H19B H 0.1991 -0.1871 0.4537 0.032 Uiso 1 1 calc R . . C20 C 0.16567(18) -0.15997(13) 0.52880(15) 0.0321(8) Uani 1 1 d . . . H20A H 0.1349 -0.1906 0.5295 0.039 Uiso 1 1 calc R . . H20B H 0.1949 -0.1495 0.5742 0.039 Uiso 1 1 calc R . . C21 C 0.1064(2) -0.11821(16) 0.49305(19) 0.0478(10) Uani 1 1 d . . . H21A H 0.1097 -0.0908 0.5239 0.057 Uiso 1 1 calc R . . H21B H 0.0510 -0.1317 0.4777 0.057 Uiso 1 1 calc R . . C22 C 0.12311(18) -0.09672(14) 0.43469(17) 0.0349(9) Uani 1 1 d . . . H22A H 0.1092 -0.1222 0.3999 0.042 Uiso 1 1 calc R . . H22B H 0.0883 -0.0672 0.4176 0.042 Uiso 1 1 calc R . . C24 C 0.09780(19) 0.05815(13) 0.35728(18) 0.0341(9) Uani 1 1 d . . . H24A H 0.0795 0.0584 0.3094 0.041 Uiso 1 1 calc R . . H24B H 0.0721 0.0294 0.3701 0.041 Uiso 1 1 calc R . . C25 C 0.0720(2) 0.10677(15) 0.3804(2) 0.0513(11) Uani 1 1 d . . . H25A H 0.0856 0.1049 0.4278 0.062 Uiso 1 1 calc R . . H25B H 0.0129 0.1104 0.3595 0.062 Uiso 1 1 calc R . . C26 C 0.1130(2) 0.15365(15) 0.3648(2) 0.0469(11) Uani 1 1 d . . . H26A H 0.0714 0.1751 0.3338 0.056 Uiso 1 1 calc R . . H26B H 0.1389 0.1731 0.4051 0.056 Uiso 1 1 calc R . . C27 C 0.17685(18) 0.14059(13) 0.33583(17) 0.0329(9) Uani 1 1 d . . . H27A H 0.2072 0.1711 0.3339 0.039 Uiso 1 1 calc R . . H27B H 0.1498 0.1281 0.2911 0.039 Uiso 1 1 calc R . . C28 C 0.3835(2) 0.21753(13) 0.36330(18) 0.0367(9) Uani 1 1 d . . . H28A H 0.3905 0.2448 0.3951 0.044 Uiso 1 1 calc R . . H28B H 0.3252 0.2111 0.3417 0.044 Uiso 1 1 calc R . . C29 C 0.4185(2) 0.23424(15) 0.31191(19) 0.0483(11) Uani 1 1 d . . . H29A H 0.4054 0.2087 0.2773 0.058 Uiso 1 1 calc R . . H29B H 0.3925 0.2660 0.2919 0.058 Uiso 1 1 calc R . . C30 C 0.5105(2) 0.24183(15) 0.34084(17) 0.0420(10) Uani 1 1 d . . . H30A H 0.5354 0.2214 0.3161 0.050 Uiso 1 1 calc R . . H30B H 0.5227 0.2774 0.3360 0.050 Uiso 1 1 calc R . . N1 N 0.31989(14) -0.13186(9) 0.44837(11) 0.0220(6) Uani 1 1 d . . . N2 N 0.23148(15) -0.07270(9) 0.39486(12) 0.0229(6) Uani 1 1 d . . . N3 N 0.31946(14) -0.10096(10) 0.55193(11) 0.0236(6) Uani 1 1 d . . . N4 N 0.23596(15) -0.04000(10) 0.49965(12) 0.0287(7) Uani 1 1 d . . . N5 N 0.21879(14) 0.01290(9) 0.35356(11) 0.0231(6) Uani 1 1 d . . . N6 N 0.28720(14) 0.07977(10) 0.34280(12) 0.0231(6) Uani 1 1 d . . . N7 N 0.22090(16) 0.04651(11) 0.45727(12) 0.0295(7) Uani 1 1 d . . . N8 N 0.28171(14) 0.11583(10) 0.44310(12) 0.0285(7) Uani 1 1 d . . . N9 N 0.41107(14) 0.12652(10) 0.35517(11) 0.0246(6) Uani 1 1 d . . . N10 N 0.54411(14) 0.13526(9) 0.39033(11) 0.0221(6) Uani 1 1 d . . . N11 N 0.40863(14) 0.15935(10) 0.45759(12) 0.0268(6) Uani 1 1 d . . . N12 N 0.54336(14) 0.16345(10) 0.49527(11) 0.0244(6) Uani 1 1 d . . . O1 O 0.32597(12) -0.09970(8) 0.35272(10) 0.0276(5) Uani 1 1 d . . . O2 O 0.30873(12) 0.00381(8) 0.30181(10) 0.0281(5) Uani 1 1 d . . . O3 O 0.48496(14) 0.07215(9) 0.31620(11) 0.0354(6) Uani 1 1 d . . . O4 O 0.33130(17) -0.02317(10) 0.60095(11) 0.0498(8) Uani 1 1 d . . . O5 O 0.47913(14) 0.14906(12) 0.56789(10) 0.0485(8) Uani 1 1 d . . . O6 O 0.29860(15) 0.09209(11) 0.54773(11) 0.0452(7) Uani 1 1 d . . . N13 N 0.28282(18) 0.27853(12) 0.16580(13) 0.0408(8) Uani 1 1 d . . . N14 N 0.1636(3) 0.07368(14) 0.17038(19) 0.0618(12) Uani 1 1 d . . . O7 O 0.23515(16) 0.28134(11) 0.19556(14) 0.0556(8) Uani 1 1 d . . . O8 O 0.33067(17) 0.31354(11) 0.16995(13) 0.0522(8) Uani 1 1 d . . . O9 O 0.28085(18) 0.24079(12) 0.13188(15) 0.0639(9) Uani 1 1 d . . . O10 O 0.1837(4) 0.11636(18) 0.1831(2) 0.138(2) Uani 1 1 d . . . O11 O 0.1199(3) 0.0520(2) 0.1920(3) 0.135(2) Uani 1 1 d . . . O12 O 0.1938(4) 0.0500(2) 0.1393(3) 0.234(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.159(2) 0.256(3) 0.199(3) 0.026(3) 0.014(2) -0.021(3) O1W 0.0425(11) 0.0327(13) 0.0293(10) 0.0055(9) 0.0215(9) 0.0098(10) O2W 0.0374(12) 0.0456(15) 0.0286(12) -0.0070(11) 0.0045(10) -0.0023(11) O3W 0.0371(10) 0.0351(13) 0.0256(10) 0.0011(9) 0.0144(9) -0.0083(10) O4W 0.0357(12) 0.0365(14) 0.0377(13) -0.0052(11) -0.0001(10) 0.0025(11) O5W 0.0536(13) 0.0419(14) 0.0323(12) -0.0025(11) 0.0117(11) -0.0206(11) O6W 0.0387(11) 0.0469(14) 0.0209(10) -0.0055(10) 0.0144(9) 0.0019(10) Lu1 0.02602(6) 0.02579(8) 0.01395(6) -0.00084(5) 0.00953(5) -0.00174(5) C1 0.0245(13) 0.0255(16) 0.0150(13) 0.0004(11) 0.0058(11) -0.0075(12) C2 0.0264(13) 0.0250(15) 0.0177(13) -0.0016(11) 0.0115(10) -0.0015(12) C3 0.0245(13) 0.0291(16) 0.0196(13) 0.0029(12) 0.0121(11) 0.0008(12) C4 0.0383(15) 0.0354(18) 0.0130(13) -0.0026(13) 0.0096(12) 0.0046(14) C5 0.0263(13) 0.0351(18) 0.0126(13) 0.0031(12) 0.0057(11) -0.0021(13) C6 0.0477(16) 0.0331(18) 0.0257(14) 0.0036(13) 0.0239(12) 0.0074(14) C7 0.0230(13) 0.0251(15) 0.0113(12) 0.0028(11) 0.0023(10) 0.0032(12) C8 0.0237(13) 0.0294(16) 0.0205(14) -0.0001(12) 0.0091(11) 0.0012(12) C9 0.0221(12) 0.0246(16) 0.0198(14) -0.0016(12) 0.0075(11) 0.0033(12) C10 0.0286(14) 0.0363(18) 0.0260(15) -0.0021(14) 0.0115(12) 0.0028(14) C11 0.0274(13) 0.0316(17) 0.0135(13) -0.0003(12) 0.0059(11) -0.0059(13) C12 0.0297(14) 0.0430(19) 0.0341(16) -0.0197(14) 0.0153(12) -0.0019(14) C13 0.0306(13) 0.0258(16) 0.0142(13) 0.0005(11) 0.0115(11) -0.0020(12) C14 0.0248(13) 0.0211(15) 0.0233(14) -0.0005(12) 0.0081(11) 0.0001(12) C15 0.0235(12) 0.0232(15) 0.0161(13) 0.0011(11) 0.0077(10) 0.0007(11) C16 0.0288(14) 0.0239(16) 0.0304(16) 0.0003(13) 0.0047(13) -0.0036(13) C16' 0.0289(14) 0.0385(18) 0.0230(14) -0.0105(13) 0.0124(11) -0.0074(13) C17 0.0292(13) 0.0296(16) 0.0165(13) 0.0033(12) 0.0130(10) -0.0025(12) C18 0.0289(13) 0.0284(16) 0.0151(13) -0.0038(12) 0.0084(11) -0.0021(12) C19 0.0307(14) 0.0319(17) 0.0164(13) 0.0015(12) 0.0088(11) -0.0065(13) C20 0.0311(14) 0.0404(19) 0.0295(15) 0.0086(14) 0.0166(12) -0.0042(14) C21 0.0394(16) 0.058(2) 0.058(2) 0.0228(18) 0.0316(15) 0.0078(17) C22 0.0232(14) 0.045(2) 0.0369(17) 0.0129(15) 0.0115(13) 0.0029(14) C24 0.0231(14) 0.0394(19) 0.0408(18) 0.0074(15) 0.0129(13) 0.0023(13) C25 0.0434(17) 0.049(2) 0.071(2) 0.0116(19) 0.0330(17) 0.0117(17) C26 0.0374(17) 0.044(2) 0.062(2) 0.0005(18) 0.0220(16) 0.0092(16) C27 0.0280(14) 0.0291(18) 0.0397(18) 0.0046(14) 0.0102(13) 0.0041(13) C28 0.0284(15) 0.0316(19) 0.0438(19) 0.0016(15) 0.0059(14) 0.0007(14) C29 0.052(2) 0.036(2) 0.043(2) 0.0211(17) 0.0020(17) -0.0028(17) C30 0.0435(18) 0.041(2) 0.0388(18) 0.0178(16) 0.0115(15) 0.0036(16) N1 0.0257(11) 0.0262(13) 0.0183(11) 0.0044(10) 0.0131(9) 0.0002(10) N2 0.0272(11) 0.0281(14) 0.0179(11) 0.0015(10) 0.0135(9) -0.0008(10) N3 0.0243(11) 0.0320(14) 0.0106(11) -0.0013(10) 0.0019(9) -0.0011(11) N4 0.0350(13) 0.0294(15) 0.0222(12) 0.0014(11) 0.0109(10) 0.0060(11) N5 0.0269(11) 0.0244(13) 0.0199(11) 0.0025(10) 0.0110(9) 0.0008(10) N6 0.0275(11) 0.0245(13) 0.0210(12) 0.0010(10) 0.0133(9) -0.0011(10) N7 0.0380(13) 0.0310(15) 0.0226(12) 0.0003(11) 0.0147(10) -0.0011(12) N8 0.0254(11) 0.0376(15) 0.0235(12) -0.0073(11) 0.0101(10) -0.0015(11) N9 0.0225(11) 0.0328(14) 0.0165(11) -0.0014(10) 0.0047(9) -0.0019(10) N10 0.0235(11) 0.0244(13) 0.0190(11) -0.0036(10) 0.0085(9) -0.0019(10) N11 0.0247(11) 0.0375(15) 0.0205(12) -0.0088(11) 0.0109(9) -0.0030(11) N12 0.0279(11) 0.0317(14) 0.0133(11) -0.0012(10) 0.0073(9) -0.0005(11) O1 0.0388(10) 0.0268(12) 0.0251(10) 0.0030(9) 0.0210(8) 0.0025(9) O2 0.0376(10) 0.0248(11) 0.0288(10) -0.0013(9) 0.0204(8) 0.0006(9) O3 0.0343(11) 0.0449(14) 0.0270(11) -0.0158(10) 0.0113(9) -0.0064(10) O4 0.0693(16) 0.0440(15) 0.0245(12) -0.0075(11) 0.0036(12) 0.0174(13) O5 0.0353(11) 0.096(2) 0.0165(11) -0.0071(12) 0.0119(9) -0.0155(13) O6 0.0533(14) 0.0642(17) 0.0178(11) -0.0074(11) 0.0128(10) -0.0039(13) N13 0.0464(16) 0.0445(18) 0.0233(14) -0.0022(13) 0.0030(12) 0.0127(14) N14 0.074(2) 0.065(2) 0.044(2) -0.0060(17) 0.0197(18) 0.0217(19) O7 0.0623(14) 0.0562(17) 0.0607(15) -0.0141(13) 0.0374(12) 0.0027(13) O8 0.0618(15) 0.0484(16) 0.0448(14) 0.0017(12) 0.0179(12) -0.0059(14) O9 0.0719(17) 0.0601(18) 0.0599(16) -0.0283(15) 0.0246(14) 0.0051(15) O10 0.212(5) 0.089(3) 0.067(3) 0.006(2) -0.003(3) -0.024(3) O11 0.087(3) 0.177(5) 0.137(4) -0.003(4) 0.038(3) -0.017(3) O12 0.498(5) 0.126(3) 0.209(3) 0.093(3) 0.284(3) 0.165(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1W Lu1 2.348(2) . ? O2W Lu1 2.314(2) . ? O3W Lu1 2.297(2) . ? O4W Lu1 2.273(2) . ? O5W Lu1 2.322(2) . ? O6W Lu1 2.337(2) . ? Lu1 O1 2.292(2) . ? Lu1 O2 2.312(2) . ? C1 O1 1.248(4) . ? C1 N2 1.349(4) . ? C1 N1 1.357(4) . ? C2 N3 1.457(3) . ? C2 N1 1.472(4) . ? C2 C19 1.517(4) . ? C2 C3 1.577(4) . ? C3 N4 1.453(4) . ? C3 N2 1.468(4) . ? C3 C22 1.518(4) . ? C4 O4 1.218(4) . ? C4 N4 1.356(4) . ? C4 N3 1.360(4) . ? C5 N2 1.437(4) . ? C5 N5 1.449(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.454(4) . ? C6 N7 1.463(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.228(4) . ? C7 N5 1.345(4) . ? C7 N6 1.353(4) . ? C8 N7 1.455(4) . ? C8 N5 1.460(4) . ? C8 C24 1.520(4) . ? C8 C9 1.577(4) . ? C9 N8 1.439(4) . ? C9 N6 1.480(4) . ? C9 C27 1.532(4) . ? C10 O6 1.220(4) . ? C10 N8 1.360(4) . ? C10 N7 1.361(4) . ? C11 N9 1.447(3) . ? C11 N6 1.450(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.447(4) . ? C12 N11 1.451(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.231(4) . ? C13 N10 1.354(4) . ? C13 N9 1.364(4) . ? C14 N11 1.454(4) . ? C14 N9 1.462(4) . ? C14 C28 1.519(4) . ? C14 C15 1.582(4) . ? C15 N10 1.453(4) . ? C15 N12 1.468(4) . ? C15 C16 1.521(4) . ? C16 C30 1.523(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16' O5 1.222(4) . ? C16' N11 1.357(4) . ? C16' N12 1.376(4) . ? C17 N3 1.450(3) 5_656 ? C17 N10 1.452(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N1 1.437(4) 5_656 ? C18 N12 1.441(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.533(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.528(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.528(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C24 C25 1.515(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.540(6) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 C27 1.527(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.540(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 C30 1.528(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? N1 C18 1.437(4) 5_656 ? N3 C17 1.450(3) 5_656 ? N13 O8 1.236(4) . ? N13 O9 1.239(4) . ? N13 O7 1.246(4) . ? N14 O10 1.186(6) . ? N14 O12 1.189(7) . ? N14 O11 1.194(7) . ? 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 O4W Lu1 O1 113.35(9) . . ? O4W Lu1 O3W 79.28(8) . . ? O1 Lu1 O3W 146.60(8) . . ? O4W Lu1 O2 75.17(8) . . ? O1 Lu1 O2 79.13(8) . . ? O3W Lu1 O2 74.48(8) . . ? O4W Lu1 O2W 145.41(9) . . ? O1 Lu1 O2W 80.16(8) . . ? O3W Lu1 O2W 74.16(8) . . ? O2 Lu1 O2W 76.64(8) . . ? O4W Lu1 O5W 71.28(9) . . ? O1 Lu1 O5W 71.04(8) . . ? O3W Lu1 O5W 140.83(8) . . ? O2 Lu1 O5W 120.10(9) . . ? O2W Lu1 O5W 141.81(9) . . ? O4W Lu1 O6W 78.11(9) . . ? O1 Lu1 O6W 138.16(8) . . ? O3W Lu1 O6W 73.19(8) . . ? O2 Lu1 O6W 141.12(8) . . ? O2W Lu1 O6W 113.89(8) . . ? O5W Lu1 O6W 75.86(9) . . ? O4W Lu1 O1W 141.27(8) . . ? O1 Lu1 O1W 77.77(8) . . ? O3W Lu1 O1W 112.48(8) . . ? O2 Lu1 O1W 142.80(7) . . ? O2W Lu1 O1W 70.97(8) . . ? O5W Lu1 O1W 78.68(8) . . ? O6W Lu1 O1W 71.17(8) . . ? O1 C1 N2 125.0(3) . . ? O1 C1 N1 124.6(3) . . ? N2 C1 N1 110.3(3) . . ? N3 C2 N1 111.5(2) . . ? N3 C2 C19 114.0(2) . . ? N1 C2 C19 113.6(2) . . ? N3 C2 C3 102.3(2) . . ? N1 C2 C3 102.2(2) . . ? C19 C2 C3 112.0(2) . . ? N4 C3 N2 112.9(3) . . ? N4 C3 C22 113.7(3) . . ? N2 C3 C22 111.5(2) . . ? N4 C3 C2 102.6(2) . . ? N2 C3 C2 103.0(2) . . ? C22 C3 C2 112.3(3) . . ? O4 C4 N4 125.5(3) . . ? O4 C4 N3 126.0(3) . . ? N4 C4 N3 108.5(3) . . ? N2 C5 N5 114.0(2) . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? N5 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N4 C6 N7 114.2(3) . . ? N4 C6 H6A 108.7 . . ? N7 C6 H6A 108.7 . . ? N4 C6 H6B 108.7 . . ? N7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N5 125.2(3) . . ? O2 C7 N6 125.1(3) . . ? N5 C7 N6 109.6(3) . . ? N7 C8 N5 113.2(2) . . ? N7 C8 C24 112.9(3) . . ? N5 C8 C24 112.7(2) . . ? N7 C8 C9 102.1(2) . . ? N5 C8 C9 102.3(2) . . ? C24 C8 C9 112.5(3) . . ? N8 C9 N6 113.2(2) . . ? N8 C9 C27 114.0(3) . . ? N6 C9 C27 111.7(3) . . ? N8 C9 C8 103.0(2) . . ? N6 C9 C8 102.3(2) . . ? C27 C9 C8 111.6(2) . . ? O6 C10 N8 125.6(3) . . ? O6 C10 N7 126.0(3) . . ? N8 C10 N7 108.4(3) . . ? N9 C11 N6 115.1(2) . . ? N9 C11 H11A 108.5 . . ? N6 C11 H11A 108.5 . . ? N9 C11 H11B 108.5 . . ? N6 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N8 C12 N11 114.7(3) . . ? N8 C12 H12A 108.6 . . ? N11 C12 H12A 108.6 . . ? N8 C12 H12B 108.6 . . ? N11 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N10 125.6(3) . . ? O3 C13 N9 125.9(3) . . ? N10 C13 N9 108.4(3) . . ? N11 C14 N9 112.8(2) . . ? N11 C14 C28 113.5(3) . . ? N9 C14 C28 112.4(2) . . ? N11 C14 C15 103.1(2) . . ? N9 C14 C15 102.2(2) . . ? C28 C14 C15 112.0(2) . . ? N10 C15 N12 112.5(2) . . ? N10 C15 C16 113.3(3) . . ? N12 C15 C16 113.6(2) . . ? N10 C15 C14 102.4(2) . . ? N12 C15 C14 102.1(2) . . ? C16 C15 C14 111.8(2) . . ? C15 C16 C30 112.0(3) . . ? C15 C16 H16A 109.2 . . ? C30 C16 H16A 109.2 . . ? C15 C16 H16B 109.2 . . ? C30 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? O5 C16' N11 126.0(3) . . ? O5 C16' N12 125.2(3) . . ? N11 C16' N12 108.8(3) . . ? N3 C17 N10 115.3(2) 5_656 . ? N3 C17 H17A 108.4 5_656 . ? N10 C17 H17A 108.4 . . ? N3 C17 H17B 108.4 5_656 . ? N10 C17 H17B 108.4 . . ? H17A C17 H17B 107.5 . . ? N1 C18 N12 115.0(2) 5_656 . ? N1 C18 H18A 108.5 5_656 . ? N12 C18 H18A 108.5 . . ? N1 C18 H18B 108.5 5_656 . ? N12 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? C2 C19 C20 110.8(3) . . ? C2 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? C2 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C21 C20 C19 112.8(3) . . ? C21 C20 H20A 109.0 . . ? C19 C20 H20A 109.0 . . ? C21 C20 H20B 109.0 . . ? C19 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C20 C21 C22 113.1(3) . . ? C20 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? C20 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C3 C22 C21 112.0(3) . . ? C3 C22 H22A 109.2 . . ? C21 C22 H22A 109.2 . . ? C3 C22 H22B 109.2 . . ? C21 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C25 C24 C8 111.0(3) . . ? C25 C24 H24A 109.4 . . ? C8 C24 H24A 109.4 . . ? C25 C24 H24B 109.4 . . ? C8 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C24 C25 C26 112.6(3) . . ? C24 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? C24 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C27 C26 C25 113.2(3) . . ? C27 C26 H26A 108.9 . . ? C25 C26 H26A 108.9 . . ? C27 C26 H26B 108.9 . . ? C25 C26 H26B 108.9 . . ? H26A C26 H26B 107.8 . . ? C26 C27 C9 111.1(3) . . ? C26 C27 H27A 109.4 . . ? C9 C27 H27A 109.4 . . ? C26 C27 H27B 109.4 . . ? C9 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C14 C28 C29 111.3(3) . . ? C14 C28 H28A 109.4 . . ? C29 C28 H28A 109.4 . . ? C14 C28 H28B 109.4 . . ? C29 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C28 112.8(3) . . ? C30 C29 H29A 109.0 . . ? C28 C29 H29A 109.0 . . ? C30 C29 H29B 109.0 . . ? C28 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C16 C30 C29 112.8(3) . . ? C16 C30 H30A 109.0 . . ? C29 C30 H30A 109.0 . . ? C16 C30 H30B 109.0 . . ? C29 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? C1 N1 C18 122.0(3) . 5_656 ? C1 N1 C2 112.3(2) . . ? C18 N1 C2 125.0(2) 5_656 . ? C1 N2 C5 123.5(3) . . ? C1 N2 C3 112.0(2) . . ? C5 N2 C3 124.5(2) . . ? C4 N3 C17 121.6(2) . 5_656 ? C4 N3 C2 113.2(2) . . ? C17 N3 C2 124.6(2) 5_656 . ? C4 N4 C3 113.3(3) . . ? C4 N4 C6 121.1(3) . . ? C3 N4 C6 125.3(2) . . ? C7 N5 C5 121.9(3) . . ? C7 N5 C8 113.4(2) . . ? C5 N5 C8 124.6(3) . . ? C7 N6 C11 121.2(3) . . ? C7 N6 C9 112.2(2) . . ? C11 N6 C9 125.3(3) . . ? C10 N7 C8 113.0(3) . . ? C10 N7 C6 121.9(3) . . ? C8 N7 C6 124.6(3) . . ? C10 N8 C9 113.2(3) . . ? C10 N8 C12 121.4(3) . . ? C9 N8 C12 125.1(3) . . ? C13 N9 C11 121.8(3) . . ? C13 N9 C14 113.2(2) . . ? C11 N9 C14 124.4(2) . . ? C13 N10 C17 121.5(3) . . ? C13 N10 C15 113.7(2) . . ? C17 N10 C15 124.6(2) . . ? C16' N11 C12 121.2(3) . . ? C16' N11 C14 113.3(2) . . ? C12 N11 C14 124.4(2) . . ? C16' N12 C18 120.9(2) . . ? C16' N12 C15 112.6(2) . . ? C18 N12 C15 124.5(3) . . ? C1 O1 Lu1 157.2(2) . . ? C7 O2 Lu1 158.5(2) . . ? O8 N13 O9 121.0(3) . . ? O8 N13 O7 119.7(3) . . ? O9 N13 O7 119.3(3) . . ? O10 N14 O12 118.6(6) . . ? O10 N14 O11 123.0(6) . . ? O12 N14 O11 118.0(6) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.472 _refine_diff_density_min -1.424 _refine_diff_density_rms 0.117 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 44 22 ' ' 2 0.000 0.000 0.500 44 22 ' ' 3 0.000 0.087 0.750 67 26 ' ' 4 -0.163 0.250 0.087 649 236 ' ' 5 0.000 0.500 0.500 84 31 ' ' 6 0.000 0.500 1.000 84 31 ' ' 7 -0.014 0.750 0.736 649 236 ' ' 8 0.000 0.913 0.250 67 26 ' ' 9 0.500 0.000 1.000 84 31 ' ' 10 0.500 1.000 0.500 84 31 ' ' 11 0.500 0.413 0.250 67 26 ' ' 12 0.500 0.587 0.750 67 26 ' ' 13 0.500 0.500 1.000 44 22 ' ' 14 0.500 0.500 0.500 44 22 ' ' _platon_squeeze_details ; ; data_p8 _database_code_depnum_ccdc_archive 'CCDC 881907' #TrackingRef '110706qx-submit-cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C120 H218 N60 Nd4 O97' _chemical_formula_weight 4630.50 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.558(2) _cell_length_b 15.609(2) _cell_length_c 20.746(2) _cell_angle_alpha 104.250(4) _cell_angle_beta 95.811(4) _cell_angle_gamma 119.308(4) _cell_volume 4108.7(9) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2374 _exptl_absorpt_coefficient_mu 1.379 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7994 _exptl_absorpt_correction_T_max 0.8631 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39166 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14141 _reflns_number_gt 12176 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0836P)^2^+95.4895P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14141 _refine_ls_number_parameters 1153 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0927 _refine_ls_wR_factor_ref 0.2380 _refine_ls_wR_factor_gt 0.2341 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 3.741 _refine_ls_shift/su_max 0.129 _refine_ls_shift/su_mean 0.003 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 N25 N 0.2943(16) 0.1306(14) -0.0907(10) 0.036(6) Uani 1 1 d . . . N26 N 0.3499(15) 0.3683(15) 0.2127(10) 0.034(6) Uani 1 1 d . . . O1W O 0.6027(13) 0.5318(13) 0.6231(9) 0.043(6) Uani 1 1 d . . . O2W O 0.4378(12) 0.4762(12) 0.1147(9) 0.035(5) Uani 1 1 d . . . O3W O 0.6360(12) 0.4269(11) 0.5113(8) 0.033(5) Uani 1 1 d . . . O4W O 0.4736(14) 0.3894(13) -0.0082(9) 0.044(6) Uani 1 1 d . . . O5W O 0.2832(14) 0.3807(13) -0.0324(9) 0.044(5) Uani 1 1 d . . . O6W O 0.8786(15) 0.7739(15) 0.5599(9) 0.052(6) Uani 1 1 d . . . O7W O 0.6169(12) 0.6671(14) 0.5349(8) 0.042(5) Uani 1 1 d . . . O8W O 0.8493(13) 0.5696(16) 0.5174(10) 0.054(6) Uani 1 1 d . . . O13 O 0.2372(13) 0.1661(15) -0.0851(9) 0.047(6) Uani 1 1 d . . . O14 O 0.3675(13) 0.1672(13) -0.0379(9) 0.041(5) Uani 1 1 d . . . O15 O 0.2822(19) 0.0647(16) -0.1436(12) 0.071(9) Uani 1 1 d . . . O16 O 0.3132(14) 0.2960(12) 0.1547(8) 0.039(5) Uani 1 1 d . . . O17 O 0.4240(16) 0.3854(18) 0.2527(12) 0.069(7) Uani 1 1 d . . . O18 O 0.3092(18) 0.414(2) 0.2285(13) 0.084(9) Uani 1 1 d . . . Nd1 Nd 0.32948(9) 0.29496(8) 0.03876(6) 0.0245(3) Uani 1 1 d . . . Nd2 Nd 0.73202(8) 0.61527(9) 0.56509(6) 0.0244(3) Uani 1 1 d . . . N27 N 1.1113(17) 1.0100(17) 0.3713(12) 0.046(7) Uani 1 1 d . . . N28 N -0.1139(15) -0.4335(16) 0.0994(11) 0.040(6) Uani 1 1 d . . . N29 N 0.563(3) 0.145(2) 0.4181(17) 0.085(11) Uani 1 1 d . . . N30 N 0.9141(3) 0.3195(3) 0.3599(2) 0.105(14) Uani 1 1 d D . . O19 O 1.0364(17) 1.0076(17) 0.3402(14) 0.074(7) Uani 1 1 d . . . O20 O 1.140(2) 0.959(2) 0.3423(17) 0.104(10) Uani 1 1 d . . . O21 O 1.152(3) 1.063(2) 0.4311(16) 0.113(12) Uani 1 1 d . . . O22 O -0.1217(19) -0.379(2) 0.1484(12) 0.086(9) Uani 1 1 d . . . O23 O -0.102(2) -0.5034(19) 0.1011(18) 0.120(11) Uani 1 1 d . . . O24 O -0.1211(19) -0.4152(18) 0.0456(11) 0.074(8) Uani 1 1 d . . . O25 O 0.626(2) 0.189(2) 0.3912(16) 0.105(10) Uani 1 1 d . . . O26 O 0.479(3) 0.064(3) 0.393(2) 0.128(17) Uani 1 1 d . . . O27 O 0.592(6) 0.185(5) 0.482(2) 0.26(5) Uani 1 1 d . . . O28 O 0.9136(6) 0.2551(5) 0.3074(4) 0.125(16) Uani 1 1 d D . . O29 O 0.9159(11) 0.3038(6) 0.4178(3) 0.70(7) Uani 1 1 d D . . O30 O 0.9129(7) 0.3989(4) 0.3545(6) 0.24(4) Uani 1 1 d D . . C1 C 0.4902(14) 0.2528(14) 0.1451(10) 0.022(5) Uani 1 1 d . . . C2 C 0.5945(14) 0.2647(14) 0.2417(10) 0.018(5) Uani 1 1 d . . . C3 C 0.4838(14) 0.1663(14) 0.2239(9) 0.018(5) Uani 1 1 d . . . C4 C 0.5197(14) 0.2852(14) 0.3314(9) 0.018(5) Uani 1 1 d . . . C5 C 0.3373(14) 0.0746(14) 0.1145(10) 0.019(4) Uani 1 1 d . . . H5A H 0.3378 0.0758 0.0676 0.023 Uiso 1 1 calc R . . H5B H 0.3340 0.0108 0.1162 0.023 Uiso 1 1 calc R . . C6 C 0.3495(14) 0.1268(14) 0.2937(10) 0.019(4) Uani 1 1 d . . . H6A H 0.3377 0.0566 0.2836 0.023 Uiso 1 1 calc R . . H6B H 0.3526 0.1529 0.3425 0.023 Uiso 1 1 calc R . . C7 C 0.1925(15) 0.0935(14) 0.0903(10) 0.022(5) Uani 1 1 d . . . C8 C 0.2014(13) 0.0389(13) 0.1847(9) 0.015(4) Uani 1 1 d . . . C9 C 0.1057(14) 0.0489(13) 0.1731(10) 0.018(5) Uani 1 1 d . . . C10 C 0.2183(14) 0.1681(13) 0.2793(10) 0.019(5) Uani 1 1 d . . . C11 C 0.0434(15) 0.1069(14) 0.0817(10) 0.022(5) Uani 1 1 d . . . H11A H 0.0486 0.1014 0.0344 0.027 Uiso 1 1 calc R . . H11B H -0.0269 0.0544 0.0792 0.027 Uiso 1 1 calc R . . C12 C 0.0555(14) 0.1558(14) 0.2551(10) 0.020(5) Uani 1 1 d . . . H12A H 0.0673 0.1752 0.3053 0.024 Uiso 1 1 calc R . . H12B H -0.0135 0.0936 0.2344 0.024 Uiso 1 1 calc R . . C13 C 0.1180(14) 0.2935(15) 0.0982(10) 0.022(5) Uani 1 1 d . . . C14 C 0.0105(14) 0.2261(14) 0.1663(9) 0.019(5) Uani 1 1 d . . . C15 C 0.0360(14) 0.3400(14) 0.1765(11) 0.022(5) Uani 1 1 d . . . C16 C 0.1050(13) 0.3366(14) 0.2802(10) 0.017(5) Uani 1 1 d . . . C17 C 0.1429(16) 0.4678(15) 0.1173(12) 0.028(6) Uani 1 1 d . . . H17A H 0.0859 0.4780 0.1090 0.033 Uiso 1 1 calc R . . H17B H 0.1649 0.4607 0.0747 0.033 Uiso 1 1 calc R . . C18 C 0.1081(15) 0.4974(14) 0.2867(11) 0.025(5) Uani 1 1 d . . . H18A H 0.0500 0.5014 0.2685 0.030 Uiso 1 1 calc R . . H18B H 0.1100 0.5016 0.3348 0.030 Uiso 1 1 calc R . . C19 C 0.3180(15) 0.6155(15) 0.1567(11) 0.024(5) Uani 1 1 d . . . C20 C 0.2141(15) 0.6248(14) 0.2278(10) 0.021(5) Uani 1 1 d . . . C21 C 0.3247(14) 0.7268(14) 0.2591(10) 0.020(5) Uani 1 1 d . . . C22 C 0.2867(15) 0.6359(15) 0.3365(10) 0.023(5) Uani 1 1 d . . . C23 C 0.4712(15) 0.7911(15) 0.2008(11) 0.024(5) Uani 1 1 d . . . H23A H 0.4762 0.8583 0.2170 0.029 Uiso 1 1 calc R . . H23B H 0.4716 0.7761 0.1521 0.029 Uiso 1 1 calc R . . C24 C 0.4566(14) 0.7921(16) 0.3721(11) 0.024(5) Uani 1 1 d . . . H24A H 0.4524 0.7787 0.4158 0.029 Uiso 1 1 calc R . . H24B H 0.4673 0.8615 0.3797 0.029 Uiso 1 1 calc R . . C25 C 0.6102(15) 0.7607(14) 0.2082(10) 0.022(5) Uani 1 1 d . . . C26 C 0.6052(15) 0.8515(14) 0.3132(10) 0.022(5) Uani 1 1 d . . . C27 C 0.7007(15) 0.8418(14) 0.3245(10) 0.021(5) Uani 1 1 d . . . C28 C 0.5891(15) 0.7502(15) 0.3839(10) 0.022(5) Uani 1 1 d . . . C29 C 0.7641(15) 0.7569(15) 0.2366(11) 0.025(6) Uani 1 1 d . . . H29A H 0.7599 0.7464 0.1876 0.030 Uiso 1 1 calc R . . H29B H 0.8334 0.8147 0.2628 0.030 Uiso 1 1 calc R . . C30 C 0.7536(15) 0.7637(15) 0.4050(11) 0.024(6) Uani 1 1 d . . . H30A H 0.8222 0.8252 0.4143 0.029 Uiso 1 1 calc R . . H30B H 0.7397 0.7589 0.4494 0.029 Uiso 1 1 calc R . . C31 C 0.6925(14) 0.5677(15) 0.2002(11) 0.024(5) Uani 1 1 d . . . C32 C 0.7992(14) 0.6644(15) 0.3109(10) 0.021(5) Uani 1 1 d . . . C33 C 0.7748(14) 0.5500(15) 0.2924(10) 0.022(5) Uani 1 1 d . . . C34 C 0.7182(14) 0.5880(15) 0.3882(11) 0.021(5) Uani 1 1 d . . . C35 C 0.6680(15) 0.3965(15) 0.1786(10) 0.022(5) Uani 1 1 d . . . H35A H 0.6486 0.3940 0.1314 0.026 Uiso 1 1 calc R . . H35B H 0.7259 0.3871 0.1822 0.026 Uiso 1 1 calc R . . C36 C 0.7013(14) 0.4181(14) 0.3549(10) 0.019(5) Uani 1 1 d . . . H36A H 0.6987 0.4241 0.4027 0.023 Uiso 1 1 calc R . . H36B H 0.7561 0.4059 0.3471 0.023 Uiso 1 1 calc R . . C37 C 0.6750(15) 0.2379(15) 0.2398(11) 0.024(5) Uani 1 1 d . . . H37A H 0.6847 0.2176 0.2798 0.028 Uiso 1 1 calc R . . H37B H 0.7400 0.2996 0.2426 0.028 Uiso 1 1 calc R . . C38 C 0.6452(16) 0.1490(17) 0.1742(11) 0.030(6) Uani 1 1 d . . . H38A H 0.6973 0.1310 0.1759 0.036 Uiso 1 1 calc R . . H38B H 0.6440 0.1728 0.1348 0.036 Uiso 1 1 calc R . . C39 C 0.5409(16) 0.0510(16) 0.1630(13) 0.031(6) Uani 1 1 d . . . H39A H 0.4981 0.0304 0.1172 0.038 Uiso 1 1 calc R . . H39B H 0.5502 -0.0063 0.1643 0.038 Uiso 1 1 calc R . . C40 C 0.4866(15) 0.0687(14) 0.2175(10) 0.024(5) Uani 1 1 d . . . H40A H 0.4167 0.0080 0.2048 0.028 Uiso 1 1 calc R . . H40B H 0.5224 0.0759 0.2620 0.028 Uiso 1 1 calc R . . C41 C 0.1753(17) -0.0693(14) 0.1813(11) 0.027(6) Uani 1 1 d . . . H41A H 0.1524 -0.0832 0.2219 0.033 Uiso 1 1 calc R . . H41B H 0.2365 -0.0730 0.1817 0.033 Uiso 1 1 calc R . . C42 C 0.0909(19) -0.1527(16) 0.1158(14) 0.038(7) Uani 1 1 d . . . H42A H 0.1191 -0.1471 0.0758 0.045 Uiso 1 1 calc R . . H42B H 0.0691 -0.2220 0.1183 0.045 Uiso 1 1 calc R . . C43 C 0.001(2) -0.1436(17) 0.1053(15) 0.048(8) Uani 1 1 d . . . H43A H -0.0597 -0.2097 0.1024 0.058 Uiso 1 1 calc R . . H43B H -0.0090 -0.1334 0.0610 0.058 Uiso 1 1 calc R . . C44 C 0.0074(15) -0.0550(15) 0.1614(12) 0.026(6) Uani 1 1 d . . . H44A H 0.0053 -0.0705 0.2044 0.031 Uiso 1 1 calc R . . H44B H -0.0515 -0.0497 0.1480 0.031 Uiso 1 1 calc R . . C45 C -0.1033(15) 0.1459(15) 0.1467(13) 0.028(6) Uani 1 1 d . . . H45A H -0.1322 0.1610 0.1847 0.034 Uiso 1 1 calc R . . H45B H -0.1148 0.0761 0.1387 0.034 Uiso 1 1 calc R . . C46 C -0.1565(16) 0.1480(17) 0.0819(12) 0.030(6) Uani 1 1 d . . . H46A H -0.1399 0.1164 0.0421 0.036 Uiso 1 1 calc R . . H46B H -0.2306 0.1055 0.0750 0.036 Uiso 1 1 calc R . . C47 C -0.1262(17) 0.2578(19) 0.0850(14) 0.041(7) Uani 1 1 d . . . H47A H -0.1882 0.2590 0.0737 0.049 Uiso 1 1 calc R . . H47B H -0.0892 0.2754 0.0500 0.049 Uiso 1 1 calc R . . C48 C -0.0592(15) 0.3405(16) 0.1554(12) 0.029(6) Uani 1 1 d . . . H48A H -0.0401 0.4096 0.1537 0.035 Uiso 1 1 calc R . . H48B H -0.0981 0.3271 0.1899 0.035 Uiso 1 1 calc R . . C49 C 0.1360(15) 0.6516(15) 0.2069(11) 0.026(5) Uani 1 1 d . . . H49A H 0.1505 0.6786 0.1688 0.031 Uiso 1 1 calc R . . H49B H 0.0677 0.5879 0.1904 0.031 Uiso 1 1 calc R . . C50 C 0.1370(16) 0.7312(16) 0.2653(12) 0.030(6) Uani 1 1 d . . . H50A H 0.0986 0.6961 0.2951 0.037 Uiso 1 1 calc R . . H50B H 0.1017 0.7608 0.2465 0.037 Uiso 1 1 calc R . . C51 C 0.2446(17) 0.8211(17) 0.3094(12) 0.033(6) Uani 1 1 d . . . H51A H 0.2476 0.8874 0.3205 0.040 Uiso 1 1 calc R . . H51B H 0.2593 0.8103 0.3528 0.040 Uiso 1 1 calc R . . C52 C 0.3240(15) 0.8260(15) 0.2709(11) 0.025(6) Uani 1 1 d . . . H52A H 0.3078 0.8337 0.2266 0.030 Uiso 1 1 calc R . . H52B H 0.3916 0.8866 0.2979 0.030 Uiso 1 1 calc R . . C53 C 0.6343(16) 0.9648(15) 0.3381(12) 0.028(6) Uani 1 1 d . . . H53A H 0.5734 0.9675 0.3260 0.034 Uiso 1 1 calc R . . H53B H 0.6602 0.9938 0.3884 0.034 Uiso 1 1 calc R . . C54 C 0.7142(19) 1.0304(18) 0.3069(15) 0.042(7) Uani 1 1 d . . . H54A H 0.7385 1.1040 0.3300 0.050 Uiso 1 1 calc R . . H54B H 0.6827 1.0118 0.2582 0.050 Uiso 1 1 calc R . . C55 C 0.8052(19) 1.0178(18) 0.3119(15) 0.043(8) Uani 1 1 d . . . H55A H 0.8681 1.0869 0.3328 0.051 Uiso 1 1 calc R . . H55B H 0.8073 0.9864 0.2654 0.051 Uiso 1 1 calc R . . C56 C 0.8008(16) 0.9486(16) 0.3551(14) 0.034(7) Uani 1 1 d . . . H56A H 0.8589 0.9397 0.3552 0.041 Uiso 1 1 calc R . . H56B H 0.8050 0.9826 0.4028 0.041 Uiso 1 1 calc R . . C57 C 0.9139(16) 0.7441(17) 0.3338(13) 0.031(6) Uani 1 1 d . . . H57A H 0.9416 0.7420 0.2935 0.038 Uiso 1 1 calc R . . H57B H 0.9263 0.8142 0.3535 0.038 Uiso 1 1 calc R . . C58 C 0.9683(17) 0.7243(19) 0.3856(15) 0.041(8) Uani 1 1 d . . . H58A H 0.9487 0.7380 0.4287 0.049 Uiso 1 1 calc R . . H58B H 1.0420 0.7736 0.3951 0.049 Uiso 1 1 calc R . . C59 C 0.9468(17) 0.6135(18) 0.3637(13) 0.036(7) Uani 1 1 d . . . H59A H 0.9197 0.5814 0.3979 0.043 Uiso 1 1 calc R . . H59B H 1.0108 0.6162 0.3621 0.043 Uiso 1 1 calc R . . C60 C 0.8701(15) 0.5461(15) 0.2928(10) 0.023(5) Uani 1 1 d . . . H60A H 0.9009 0.5720 0.2574 0.027 Uiso 1 1 calc R . . H60B H 0.8523 0.4737 0.2822 0.027 Uiso 1 1 calc R . . N1 N 0.5843(12) 0.3105(12) 0.1894(8) 0.019(4) Uani 1 1 d . . . N2 N 0.4320(11) 0.1647(11) 0.1619(8) 0.018(4) Uani 1 1 d . . . N3 N 0.6054(11) 0.3282(12) 0.3096(8) 0.018(4) Uani 1 1 d . . . N4 N 0.4470(12) 0.1943(12) 0.2824(8) 0.020(4) Uani 1 1 d . . . N5 N 0.2468(12) 0.0704(12) 0.1295(8) 0.019(4) Uani 1 1 d . . . N6 N 0.1112(12) 0.0805(11) 0.1131(8) 0.019(4) Uani 1 1 d . . . N7 N 0.2646(11) 0.1196(11) 0.2526(8) 0.015(4) Uani 1 1 d . . . N8 N 0.1273(12) 0.1293(11) 0.2355(9) 0.020(4) Uani 1 1 d . . . N9 N 0.0614(12) 0.2083(12) 0.1158(8) 0.020(4) Uani 1 1 d . . . N10 N 0.1064(12) 0.3721(12) 0.1314(8) 0.021(4) Uani 1 1 d . . . N11 N 0.0599(12) 0.2393(12) 0.2354(8) 0.019(4) Uani 1 1 d . . . N12 N 0.0904(12) 0.3964(12) 0.2480(8) 0.020(4) Uani 1 1 d . . . N13 N 0.2260(12) 0.5599(12) 0.1707(8) 0.021(4) Uani 1 1 d . . . N14 N 0.3748(13) 0.7105(12) 0.2061(9) 0.023(5) Uani 1 1 d . . . N15 N 0.1993(12) 0.5852(12) 0.2852(8) 0.021(4) Uani 1 1 d . . . N16 N 0.3616(12) 0.7160(12) 0.3218(9) 0.022(4) Uani 1 1 d . . . N17 N 0.5605(11) 0.8008(11) 0.2397(8) 0.017(3) Uani 1 1 d . . . N18 N 0.6929(12) 0.7859(12) 0.2553(9) 0.024(5) Uani 1 1 d . . . N19 N 0.5475(11) 0.7929(11) 0.3526(8) 0.017(3) Uani 1 1 d . . . N20 N 0.6796(12) 0.7786(12) 0.3683(8) 0.019(4) Uani 1 1 d . . . N21 N 0.7469(12) 0.6639(12) 0.2489(9) 0.022(4) Uani 1 1 d . . . N22 N 0.7018(13) 0.4987(12) 0.2249(8) 0.022(5) Uani 1 1 d . . . N23 N 0.7522(13) 0.6731(12) 0.3683(9) 0.024(5) Uani 1 1 d . . . N24 N 0.7266(12) 0.5154(12) 0.3461(8) 0.018(4) Uani 1 1 d . . . O1 O 0.4625(10) 0.2735(11) 0.0961(7) 0.024(3) Uani 1 1 d . . . O2 O 0.2123(11) 0.1190(11) 0.0389(7) 0.024(3) Uani 1 1 d . . . O3 O 0.1707(11) 0.2993(10) 0.0571(7) 0.024(4) Uani 1 1 d . . . O4 O 0.3428(11) 0.5828(11) 0.1078(8) 0.030(4) Uani 1 1 d . . . O5 O 0.5857(12) 0.7115(11) 0.1466(8) 0.031(4) Uani 1 1 d . . . O6 O 0.6431(11) 0.5467(11) 0.1437(8) 0.030(4) Uani 1 1 d . . . O7 O 0.5097(10) 0.3221(11) 0.3869(7) 0.023(4) Uani 1 1 d . . . O8 O 0.2531(10) 0.2360(10) 0.3364(7) 0.023(4) Uani 1 1 d . . . O9 O 0.1510(11) 0.3674(10) 0.3398(7) 0.025(4) Uani 1 1 d . . . O10 O 0.2960(13) 0.6154(13) 0.3886(8) 0.038(5) Uani 1 1 d . . . O11 O 0.5523(11) 0.6963(11) 0.4188(7) 0.030(4) Uani 1 1 d . . . O12 O 0.6860(10) 0.5815(11) 0.4404(7) 0.024(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N25 0.046(10) 0.028(8) 0.019(8) 0.011(7) 0.015(8) 0.006(8) N26 0.042(9) 0.039(8) 0.019(9) 0.010(7) 0.006(8) 0.020(7) O1W 0.046(8) 0.034(8) 0.036(9) 0.010(7) 0.019(7) 0.011(7) O2W 0.035(7) 0.030(7) 0.028(8) 0.010(6) 0.001(7) 0.010(6) O3W 0.044(8) 0.032(6) 0.016(7) 0.009(5) 0.002(6) 0.016(6) O4W 0.047(9) 0.039(8) 0.027(8) 0.010(7) 0.015(7) 0.011(7) O5W 0.055(9) 0.052(7) 0.030(8) 0.029(6) 0.005(7) 0.026(6) O6W 0.057(10) 0.046(9) 0.033(9) 0.012(7) 0.025(8) 0.012(8) O7W 0.043(7) 0.080(9) 0.019(7) 0.019(6) 0.013(6) 0.043(6) O8W 0.045(7) 0.085(10) 0.031(10) -0.001(8) 0.004(7) 0.043(7) O13 0.035(8) 0.064(10) 0.027(8) 0.019(7) 0.002(7) 0.016(7) O14 0.034(7) 0.046(8) 0.037(9) 0.014(7) 0.003(7) 0.017(6) O15 0.088(14) 0.037(10) 0.050(12) 0.004(9) 0.029(11) 0.010(10) O16 0.055(9) 0.035(7) 0.007(6) 0.005(5) -0.005(7) 0.014(6) O17 0.065(10) 0.079(11) 0.052(13) 0.004(10) -0.017(10) 0.045(8) O18 0.087(11) 0.107(13) 0.054(14) -0.012(11) 0.003(11) 0.071(9) Nd1 0.0273(5) 0.0259(4) 0.0151(5) 0.0117(4) 0.0035(4) 0.0088(4) Nd2 0.0232(4) 0.0316(5) 0.0124(5) 0.0041(4) 0.0029(4) 0.0122(4) N27 0.054(11) 0.049(10) 0.040(11) 0.025(8) 0.025(9) 0.025(8) N28 0.036(9) 0.050(9) 0.034(10) 0.023(8) 0.001(8) 0.021(7) N29 0.13(2) 0.083(14) 0.054(17) 0.019(13) 0.023(16) 0.073(13) N30 0.054(12) 0.08(2) 0.084(16) -0.035(15) 0.056(11) -0.009(14) O19 0.076(11) 0.082(10) 0.102(15) 0.063(10) 0.046(11) 0.050(8) O20 0.130(12) 0.122(14) 0.12(2) 0.045(14) 0.072(14) 0.102(10) O21 0.16(2) 0.106(17) 0.054(17) -0.004(14) -0.016(17) 0.080(15) O22 0.094(12) 0.150(15) 0.063(11) 0.072(10) 0.050(10) 0.078(11) O23 0.130(15) 0.079(11) 0.13(2) 0.030(12) -0.057(16) 0.060(11) O24 0.117(14) 0.095(12) 0.028(10) 0.020(9) 0.016(10) 0.072(10) O25 0.132(17) 0.137(16) 0.109(18) 0.079(14) 0.069(15) 0.093(13) O26 0.10(2) 0.10(2) 0.11(3) 0.00(2) 0.00(2) 0.027(19) O27 0.33(8) 0.23(6) 0.05(2) 0.00(3) 0.03(3) 0.05(6) O28 0.083(19) 0.14(3) 0.12(2) 0.07(2) 0.040(17) 0.030(19) O29 0.37(7) 0.56(10) 0.22(4) -0.29(5) 0.21(4) -0.26(7) O30 0.05(2) 0.25(6) 0.34(8) 0.09(6) 0.04(3) 0.04(3) C1 0.025(8) 0.023(7) 0.020(9) 0.011(7) 0.012(7) 0.012(6) C2 0.018(7) 0.020(7) 0.015(8) 0.010(6) 0.007(7) 0.007(6) C3 0.020(7) 0.025(7) 0.008(8) 0.009(6) 0.008(6) 0.009(6) C4 0.019(7) 0.025(7) 0.010(8) 0.013(6) 0.002(7) 0.008(6) C5 0.022(5) 0.024(5) 0.009(5) 0.010(4) 0.005(5) 0.009(4) C6 0.022(5) 0.024(5) 0.009(5) 0.010(4) 0.005(5) 0.009(4) C7 0.028(8) 0.015(7) 0.016(9) 0.004(7) 0.003(8) 0.007(6) C8 0.019(7) 0.019(6) 0.011(8) 0.012(6) 0.003(6) 0.009(5) C9 0.017(7) 0.018(7) 0.022(8) 0.018(6) 0.007(7) 0.005(6) C10 0.018(8) 0.019(7) 0.016(8) 0.015(6) 0.004(7) 0.004(6) C11 0.031(8) 0.022(7) 0.014(9) 0.009(6) 0.002(7) 0.014(6) C12 0.026(7) 0.025(7) 0.021(8) 0.017(6) 0.016(7) 0.016(6) C13 0.020(8) 0.030(8) 0.013(8) 0.011(7) -0.002(7) 0.012(6) C14 0.022(8) 0.025(7) 0.007(8) 0.009(6) -0.001(7) 0.010(6) C15 0.017(7) 0.019(7) 0.026(10) 0.007(7) -0.002(8) 0.007(6) C16 0.016(7) 0.026(7) 0.018(8) 0.015(6) 0.013(6) 0.012(5) C17 0.024(9) 0.019(8) 0.024(10) 0.006(7) -0.005(8) 0.003(7) C18 0.031(8) 0.021(7) 0.028(10) 0.011(7) 0.011(8) 0.016(6) C19 0.026(8) 0.025(8) 0.018(9) 0.011(7) -0.001(8) 0.011(6) C20 0.028(8) 0.019(7) 0.016(9) 0.008(6) 0.001(7) 0.012(6) C21 0.025(8) 0.018(7) 0.015(8) 0.008(6) 0.002(7) 0.010(6) C22 0.033(9) 0.027(8) 0.012(8) 0.010(6) 0.009(7) 0.015(6) C23 0.026(8) 0.028(8) 0.021(9) 0.016(7) 0.008(7) 0.013(6) C24 0.020(8) 0.032(8) 0.015(9) 0.003(7) 0.000(7) 0.013(6) C25 0.025(9) 0.013(7) 0.017(9) 0.009(6) 0.003(7) 0.000(6) C26 0.028(8) 0.020(7) 0.016(9) 0.008(7) 0.009(7) 0.010(6) C27 0.028(8) 0.017(7) 0.021(9) 0.010(6) 0.011(7) 0.011(6) C28 0.025(8) 0.027(8) 0.012(8) 0.011(6) 0.003(7) 0.012(6) C29 0.026(8) 0.024(8) 0.027(10) 0.011(7) 0.011(8) 0.012(6) C30 0.021(8) 0.023(8) 0.017(9) 0.004(7) 0.001(8) 0.005(7) C31 0.019(8) 0.029(8) 0.027(9) 0.018(7) 0.015(7) 0.009(6) C32 0.023(8) 0.028(8) 0.015(8) 0.012(6) 0.009(7) 0.013(6) C33 0.018(8) 0.023(8) 0.016(9) 0.003(7) 0.006(7) 0.006(6) C34 0.015(7) 0.026(7) 0.022(9) 0.009(7) 0.002(7) 0.010(6) C35 0.027(8) 0.026(8) 0.010(8) 0.008(6) 0.012(7) 0.011(6) C36 0.020(7) 0.025(7) 0.013(8) 0.010(6) -0.002(7) 0.011(6) C37 0.026(8) 0.028(8) 0.020(9) 0.010(7) 0.009(7) 0.016(6) C38 0.033(9) 0.035(9) 0.023(10) 0.012(8) 0.015(8) 0.017(7) C39 0.030(8) 0.030(9) 0.037(11) 0.011(8) 0.020(8) 0.017(7) C40 0.031(9) 0.020(7) 0.012(9) 0.000(7) -0.004(8) 0.012(6) C41 0.036(9) 0.017(7) 0.033(10) 0.020(7) 0.015(8) 0.011(7) C42 0.045(12) 0.019(8) 0.042(13) 0.015(8) 0.012(10) 0.010(8) C43 0.064(14) 0.016(8) 0.041(14) -0.002(9) -0.024(12) 0.017(8) C44 0.018(8) 0.019(8) 0.030(10) 0.014(7) 0.000(8) 0.001(6) C45 0.019(8) 0.022(8) 0.039(12) 0.015(8) 0.000(8) 0.007(6) C46 0.023(9) 0.034(9) 0.023(10) 0.008(8) -0.002(8) 0.010(7) C47 0.025(9) 0.045(11) 0.041(13) 0.012(10) -0.013(10) 0.015(8) C48 0.027(8) 0.029(8) 0.034(11) 0.012(8) -0.002(9) 0.018(6) C49 0.025(8) 0.025(7) 0.029(10) 0.017(7) -0.001(8) 0.012(6) C50 0.033(9) 0.026(8) 0.035(11) 0.013(8) 0.014(9) 0.016(7) C51 0.046(10) 0.032(8) 0.029(11) 0.012(8) 0.011(9) 0.025(7) C52 0.024(9) 0.018(7) 0.026(10) 0.011(7) -0.001(8) 0.006(6) C53 0.039(9) 0.020(7) 0.026(10) 0.007(7) 0.008(8) 0.018(6) C54 0.037(11) 0.029(9) 0.056(15) 0.021(9) 0.010(11) 0.013(8) C55 0.037(11) 0.033(10) 0.057(15) 0.021(10) 0.019(11) 0.015(8) C56 0.022(9) 0.024(8) 0.050(14) 0.015(9) 0.005(9) 0.007(7) C57 0.021(8) 0.025(9) 0.039(12) 0.008(8) 0.014(9) 0.006(7) C58 0.023(9) 0.037(11) 0.047(15) -0.002(11) 0.006(10) 0.012(8) C59 0.024(9) 0.045(10) 0.040(12) 0.022(9) 0.010(9) 0.015(8) C60 0.029(8) 0.030(8) 0.012(8) 0.011(7) 0.008(7) 0.016(6) N1 0.020(6) 0.024(6) 0.014(7) 0.012(5) 0.002(6) 0.010(5) N2 0.015(6) 0.019(6) 0.015(7) 0.012(5) 0.005(6) 0.003(5) N3 0.017(6) 0.023(6) 0.009(7) 0.004(5) 0.006(6) 0.007(5) N4 0.021(6) 0.024(6) 0.016(7) 0.012(5) 0.007(6) 0.010(5) N5 0.017(6) 0.020(6) 0.018(7) 0.011(5) 0.004(6) 0.006(5) N6 0.028(7) 0.020(6) 0.014(7) 0.010(5) 0.008(6) 0.014(5) N7 0.018(6) 0.021(6) 0.005(6) 0.006(5) 0.003(5) 0.008(5) N8 0.019(6) 0.018(6) 0.020(8) 0.012(5) 0.003(6) 0.007(5) N9 0.022(7) 0.020(6) 0.010(7) 0.005(5) -0.002(6) 0.007(5) N10 0.028(7) 0.023(6) 0.013(7) 0.007(5) 0.008(6) 0.014(5) N11 0.024(6) 0.023(6) 0.012(7) 0.009(5) 0.005(6) 0.013(5) N12 0.024(6) 0.020(6) 0.016(7) 0.008(5) 0.009(6) 0.011(5) N13 0.023(7) 0.022(6) 0.014(7) 0.009(6) 0.003(6) 0.008(5) N14 0.026(7) 0.021(6) 0.022(8) 0.012(6) 0.007(6) 0.009(5) N15 0.026(7) 0.022(6) 0.009(7) 0.006(5) -0.002(6) 0.009(5) N16 0.019(6) 0.023(6) 0.022(8) 0.012(6) 0.002(6) 0.009(5) N17 0.020(4) 0.023(4) 0.009(5) 0.007(4) -0.001(4) 0.012(3) N18 0.028(7) 0.024(6) 0.030(8) 0.015(6) 0.016(6) 0.016(5) N19 0.020(4) 0.023(4) 0.009(5) 0.007(4) -0.001(4) 0.012(3) N20 0.015(6) 0.023(6) 0.013(7) 0.008(6) -0.001(6) 0.005(5) N21 0.027(7) 0.023(6) 0.020(8) 0.010(6) 0.006(6) 0.015(5) N22 0.026(7) 0.022(6) 0.015(7) 0.011(6) 0.010(6) 0.008(5) N23 0.033(7) 0.025(6) 0.020(8) 0.013(6) 0.015(6) 0.016(5) N24 0.020(6) 0.023(6) 0.008(7) 0.008(5) 0.008(5) 0.008(5) O1 0.028(4) 0.033(4) 0.011(4) 0.013(3) 0.007(4) 0.012(3) O2 0.028(4) 0.033(4) 0.011(4) 0.013(3) 0.007(4) 0.012(3) O3 0.034(6) 0.022(5) 0.015(6) 0.012(5) 0.008(5) 0.012(5) O4 0.034(6) 0.034(6) 0.025(7) 0.014(5) 0.011(6) 0.017(5) O5 0.034(7) 0.030(6) 0.021(7) 0.014(5) 0.008(6) 0.009(5) O6 0.032(6) 0.030(6) 0.027(7) 0.015(5) 0.014(6) 0.014(5) O7 0.023(6) 0.036(6) 0.006(6) 0.005(5) 0.009(5) 0.012(5) O8 0.025(6) 0.029(6) 0.010(6) 0.001(5) 0.002(5) 0.013(5) O9 0.032(6) 0.024(5) 0.019(7) 0.010(5) 0.007(5) 0.013(5) O10 0.036(8) 0.048(7) 0.020(7) 0.021(6) 0.000(6) 0.012(6) O11 0.036(7) 0.038(6) 0.021(6) 0.022(5) 0.010(6) 0.016(5) O12 0.025(6) 0.036(6) 0.013(6) 0.013(5) 0.009(5) 0.014(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N25 O15 1.23(3) . ? N25 O13 1.26(4) . ? N25 O14 1.27(3) . ? N25 Nd1 3.00(2) . ? N26 O18 1.18(4) . ? N26 O17 1.22(3) . ? N26 O16 1.27(2) . ? O1W Nd2 2.427(19) . ? O2W Nd1 2.434(14) . ? O3W Nd2 2.423(15) . ? O4W Nd1 2.462(19) . ? O5W Nd1 2.49(2) . ? O6W Nd2 2.448(18) . ? O7W Nd2 2.39(2) . ? O8W Nd2 2.47(2) . ? O13 Nd1 2.567(16) . ? O14 Nd1 2.58(2) . ? O16 Nd1 2.440(16) . ? Nd1 O2 2.444(14) . ? Nd1 O1 2.488(17) . ? Nd1 O3 2.567(17) . ? Nd2 O9 2.410(16) 2_666 ? Nd2 O12 2.464(14) . ? Nd2 O8 2.581(14) 2_666 ? N27 O20 1.17(4) . ? N27 O21 1.20(3) . ? N27 O19 1.25(4) . ? N28 O23 1.20(4) . ? N28 O22 1.21(4) . ? N28 O24 1.23(3) . ? N29 O25 1.17(5) . ? N29 O26 1.22(4) . ? N29 O27 1.24(5) . ? N30 O30 1.282(6) . ? N30 O28 1.283(6) . ? N30 O29 1.284(5) . ? C1 O1 1.24(3) . ? C1 N1 1.35(2) . ? C1 N2 1.38(3) . ? C2 N3 1.45(2) . ? C2 N1 1.47(3) . ? C2 C37 1.50(3) . ? C2 C3 1.57(2) . ? C3 N2 1.43(3) . ? C3 N4 1.46(3) . ? C3 C40 1.52(3) . ? C4 O7 1.22(2) . ? C4 N4 1.35(2) . ? C4 N3 1.35(3) . ? C5 N5 1.45(3) . ? C5 N2 1.45(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.44(3) . ? C6 N4 1.45(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.24(3) . ? C7 N6 1.33(3) . ? C7 N5 1.34(3) . ? C8 N5 1.47(3) . ? C8 N7 1.47(2) . ? C8 C41 1.51(3) . ? C8 C9 1.57(3) . ? C9 N8 1.44(3) . ? C9 N6 1.44(3) . ? C9 C44 1.53(2) . ? C10 O8 1.23(2) . ? C10 N7 1.34(3) . ? C10 N8 1.35(3) . ? C11 N9 1.43(3) . ? C11 N6 1.46(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.43(3) . ? C12 N11 1.43(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.23(3) . ? C13 N9 1.35(3) . ? C13 N10 1.36(3) . ? C14 N9 1.43(3) . ? C14 N11 1.47(3) . ? C14 C45 1.52(3) . ? C14 C15 1.57(3) . ? C15 N12 1.44(3) . ? C15 N10 1.49(3) . ? C15 C48 1.51(3) . ? C16 O9 1.21(2) . ? C16 N11 1.34(2) . ? C16 N12 1.36(3) . ? C17 N10 1.44(3) . ? C17 N13 1.44(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.42(2) . ? C18 N12 1.45(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.21(3) . ? C19 N14 1.35(2) . ? C19 N13 1.37(3) . ? C20 N13 1.45(3) . ? C20 N15 1.46(3) . ? C20 C49 1.52(3) . ? C20 C21 1.58(2) . ? C21 N16 1.45(3) . ? C21 N14 1.45(3) . ? C21 C52 1.51(3) . ? C22 O10 1.22(3) . ? C22 N15 1.36(2) . ? C22 N16 1.36(3) . ? C23 N14 1.45(3) . ? C23 N17 1.45(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.43(2) . ? C24 N19 1.51(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.23(2) . ? C25 N17 1.34(3) . ? C25 N18 1.35(3) . ? C26 N19 1.42(3) . ? C26 N17 1.44(2) . ? C26 C53 1.52(3) . ? C26 C27 1.57(3) . ? C27 N18 1.44(3) . ? C27 N20 1.45(3) . ? C27 C56 1.53(2) . ? C28 O11 1.21(3) . ? C28 N20 1.35(3) . ? C28 N19 1.35(3) . ? C29 N21 1.43(3) . ? C29 N18 1.44(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N23 1.42(3) . ? C30 N20 1.46(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O6 1.21(3) . ? C31 N21 1.35(2) . ? C31 N22 1.36(3) . ? C32 N21 1.45(3) . ? C32 N23 1.47(3) . ? C32 C57 1.52(3) . ? C32 C33 1.57(3) . ? C33 N22 1.46(2) . ? C33 N24 1.47(3) . ? C33 C60 1.51(3) . ? C34 O12 1.24(3) . ? C34 N24 1.32(3) . ? C34 N23 1.36(3) . ? C35 N1 1.43(2) . ? C35 N22 1.44(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N24 1.44(3) . ? C36 N3 1.45(2) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C38 1.52(3) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 C39 1.53(3) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C39 C40 1.53(3) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 C42 1.54(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 C43 1.48(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 C44 1.52(4) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.52(3) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C46 C47 1.52(4) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C47 C48 1.53(3) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.50(3) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.54(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.52(4) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.50(4) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.52(4) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.55(4) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C58 1.48(4) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 C59 1.52(4) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 C60 1.53(3) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? O8 Nd2 2.581(14) 2_666 ? O9 Nd2 2.410(16) 2_666 ? 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 O15 N25 O13 123(2) . . ? O15 N25 O14 121(3) . . ? O13 N25 O14 116.3(19) . . ? O15 N25 Nd1 178.5(18) . . ? O13 N25 Nd1 57.9(10) . . ? O14 N25 Nd1 58.4(12) . . ? O18 N26 O17 121(2) . . ? O18 N26 O16 120(2) . . ? O17 N26 O16 119(3) . . ? N25 O13 Nd1 97.6(12) . . ? N25 O14 Nd1 96.7(16) . . ? N26 O16 Nd1 133.3(14) . . ? O2W Nd1 O16 73.4(6) . . ? O2W Nd1 O2 142.1(5) . . ? O16 Nd1 O2 68.7(5) . . ? O2W Nd1 O4W 70.4(6) . . ? O16 Nd1 O4W 133.8(5) . . ? O2 Nd1 O4W 140.6(6) . . ? O2W Nd1 O5W 80.4(6) . . ? O16 Nd1 O5W 129.0(7) . . ? O2 Nd1 O5W 124.2(5) . . ? O4W Nd1 O5W 71.3(7) . . ? O2W Nd1 O1 84.4(6) . . ? O16 Nd1 O1 70.8(6) . . ? O2 Nd1 O1 83.8(5) . . ? O4W Nd1 O1 77.9(6) . . ? O5W Nd1 O1 148.7(5) . . ? O2W Nd1 O13 147.6(6) . . ? O16 Nd1 O13 137.3(5) . . ? O2 Nd1 O13 69.5(5) . . ? O4W Nd1 O13 85.9(6) . . ? O5W Nd1 O13 71.0(7) . . ? O1 Nd1 O13 112.7(6) . . ? O2W Nd1 O3 89.7(5) . . ? O16 Nd1 O3 70.0(6) . . ? O2 Nd1 O3 77.2(5) . . ? O4W Nd1 O3 136.1(7) . . ? O5W Nd1 O3 66.9(6) . . ? O1 Nd1 O3 140.4(5) . . ? O13 Nd1 O3 92.7(6) . . ? O2W Nd1 O14 132.8(6) . . ? O16 Nd1 O14 121.2(7) . . ? O2 Nd1 O14 71.1(6) . . ? O4W Nd1 O14 69.5(6) . . ? O5W Nd1 O14 108.8(6) . . ? O1 Nd1 O14 63.8(5) . . ? O13 Nd1 O14 49.4(7) . . ? O3 Nd1 O14 137.0(4) . . ? O2W Nd1 N25 146.9(6) . . ? O16 Nd1 N25 133.9(6) . . ? O2 Nd1 N25 68.4(5) . . ? O4W Nd1 N25 76.5(5) . . ? O5W Nd1 N25 89.6(6) . . ? O1 Nd1 N25 88.5(6) . . ? O13 Nd1 N25 24.5(7) . . ? O3 Nd1 N25 115.3(5) . . ? O14 Nd1 N25 24.9(6) . . ? O7W Nd2 O9 143.8(5) . 2_666 ? O7W Nd2 O3W 105.2(6) . . ? O9 Nd2 O3W 98.8(5) 2_666 . ? O7W Nd2 O1W 79.0(7) . . ? O9 Nd2 O1W 84.9(6) 2_666 . ? O3W Nd2 O1W 69.0(6) . . ? O7W Nd2 O6W 92.1(7) . . ? O9 Nd2 O6W 85.4(6) 2_666 . ? O3W Nd2 O6W 141.3(7) . . ? O1W Nd2 O6W 149.4(6) . . ? O7W Nd2 O12 67.8(6) . . ? O9 Nd2 O12 146.3(6) 2_666 . ? O3W Nd2 O12 74.4(5) . . ? O1W Nd2 O12 121.0(5) . . ? O6W Nd2 O12 81.0(5) . . ? O7W Nd2 O8W 140.5(7) . . ? O9 Nd2 O8W 72.4(6) 2_666 . ? O3W Nd2 O8W 73.3(6) . . ? O1W Nd2 O8W 131.9(8) . . ? O6W Nd2 O8W 71.5(8) . . ? O12 Nd2 O8W 74.1(6) . . ? O7W Nd2 O8 66.4(5) . 2_666 ? O9 Nd2 O8 78.0(5) 2_666 2_666 ? O3W Nd2 O8 142.6(5) . 2_666 ? O1W Nd2 O8 73.7(5) . 2_666 ? O6W Nd2 O8 76.0(6) . 2_666 ? O12 Nd2 O8 127.2(5) . 2_666 ? O8W Nd2 O8 137.2(5) . 2_666 ? O20 N27 O21 120(3) . . ? O20 N27 O19 120(3) . . ? O21 N27 O19 120(3) . . ? O23 N28 O22 123(3) . . ? O23 N28 O24 120(3) . . ? O22 N28 O24 116(3) . . ? O25 N29 O26 130(4) . . ? O25 N29 O27 113(4) . . ? O26 N29 O27 117(5) . . ? O30 N30 O28 120.1(7) . . ? O30 N30 O29 120.3(7) . . ? O28 N30 O29 119.6(7) . . ? O1 C1 N1 125.5(18) . . ? O1 C1 N2 125.9(16) . . ? N1 C1 N2 108.5(19) . . ? N3 C2 N1 111.2(17) . . ? N3 C2 C37 113.1(16) . . ? N1 C2 C37 113.8(18) . . ? N3 C2 C3 102.7(15) . . ? N1 C2 C3 102.0(15) . . ? C37 C2 C3 113.0(17) . . ? N2 C3 N4 111.8(19) . . ? N2 C3 C40 114.8(15) . . ? N4 C3 C40 112.1(17) . . ? N2 C3 C2 103.6(16) . . ? N4 C3 C2 102.4(13) . . ? C40 C3 C2 110.9(18) . . ? O7 C4 N4 125.0(18) . . ? O7 C4 N3 125.5(15) . . ? N4 C4 N3 109.5(17) . . ? N5 C5 N2 113.7(16) . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5B 108.8 . . ? N2 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N4 113.9(17) . . ? N7 C6 H6A 108.8 . . ? N4 C6 H6A 108.8 . . ? N7 C6 H6B 108.8 . . ? N4 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 125(2) . . ? O2 C7 N5 125(2) . . ? N6 C7 N5 109.7(19) . . ? N5 C8 N7 111.0(13) . . ? N5 C8 C41 113.0(17) . . ? N7 C8 C41 113.5(17) . . ? N5 C8 C9 102.0(16) . . ? N7 C8 C9 102.6(16) . . ? C41 C8 C9 113.7(15) . . ? N8 C9 N6 113.8(16) . . ? N8 C9 C44 113.1(17) . . ? N6 C9 C44 112.7(15) . . ? N8 C9 C8 102.8(14) . . ? N6 C9 C8 102.5(16) . . ? C44 C9 C8 110.9(17) . . ? O8 C10 N7 124.3(19) . . ? O8 C10 N8 125(2) . . ? N7 C10 N8 110.4(16) . . ? N9 C11 N6 116.5(15) . . ? N9 C11 H11A 108.2 . . ? N6 C11 H11A 108.2 . . ? N9 C11 H11B 108.2 . . ? N6 C11 H11B 108.2 . . ? H11A C11 H11B 107.3 . . ? N8 C12 N11 114.7(17) . . ? N8 C12 H12A 108.6 . . ? N11 C12 H12A 108.6 . . ? N8 C12 H12B 108.6 . . ? N11 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N9 126(2) . . ? O3 C13 N10 124.3(19) . . ? N9 C13 N10 110.0(19) . . ? N9 C14 N11 112.6(18) . . ? N9 C14 C45 114.2(15) . . ? N11 C14 C45 111.0(17) . . ? N9 C14 C15 103.9(16) . . ? N11 C14 C15 101.1(14) . . ? C45 C14 C15 113.0(19) . . ? N12 C15 N10 110.9(14) . . ? N12 C15 C48 115(2) . . ? N10 C15 C48 113(2) . . ? N12 C15 C14 103.7(17) . . ? N10 C15 C14 101.7(17) . . ? C48 C15 C14 111.4(15) . . ? O9 C16 N11 126(2) . . ? O9 C16 N12 124.9(17) . . ? N11 C16 N12 108.9(16) . . ? N10 C17 N13 115.3(19) . . ? N10 C17 H17A 108.5 . . ? N13 C17 H17A 108.5 . . ? N10 C17 H17B 108.5 . . ? N13 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? N15 C18 N12 115.0(19) . . ? N15 C18 H18A 108.5 . . ? N12 C18 H18A 108.5 . . ? N15 C18 H18B 108.5 . . ? N12 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? O4 C19 N14 126.4(19) . . ? O4 C19 N13 124.4(16) . . ? N14 C19 N13 109.1(19) . . ? N13 C20 N15 112.8(18) . . ? N13 C20 C49 114.1(17) . . ? N15 C20 C49 112.9(19) . . ? N13 C20 C21 103.5(17) . . ? N15 C20 C21 101.7(15) . . ? C49 C20 C21 110.7(17) . . ? N16 C21 N14 112.5(19) . . ? N16 C21 C52 113.7(16) . . ? N14 C21 C52 112.8(18) . . ? N16 C21 C20 102.9(15) . . ? N14 C21 C20 101.1(14) . . ? C52 C21 C20 112.8(18) . . ? O10 C22 N15 125.6(19) . . ? O10 C22 N16 124.9(18) . . ? N15 C22 N16 109.5(19) . . ? N14 C23 N17 114.3(19) . . ? N14 C23 H23A 108.7 . . ? N17 C23 H23A 108.7 . . ? N14 C23 H23B 108.7 . . ? N17 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? N16 C24 N19 114.0(17) . . ? N16 C24 H24A 108.7 . . ? N19 C24 H24A 108.7 . . ? N16 C24 H24B 108.7 . . ? N19 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? O5 C25 N17 126(2) . . ? O5 C25 N18 126(2) . . ? N17 C25 N18 108.7(17) . . ? N19 C26 N17 113.6(14) . . ? N19 C26 C53 113.2(19) . . ? N17 C26 C53 112.9(19) . . ? N19 C26 C27 100.9(18) . . ? N17 C26 C27 103.1(17) . . ? C53 C26 C27 112.1(15) . . ? N18 C27 N20 112.3(17) . . ? N18 C27 C56 112.1(19) . . ? N20 C27 C56 114.0(18) . . ? N18 C27 C26 101.6(16) . . ? N20 C27 C26 103.6(17) . . ? C56 C27 C26 112.2(18) . . ? O11 C28 N20 126(2) . . ? O11 C28 N19 127(2) . . ? N20 C28 N19 106.8(18) . . ? N21 C29 N18 114.0(18) . . ? N21 C29 H29A 108.8 . . ? N18 C29 H29A 108.8 . . ? N21 C29 H29B 108.8 . . ? N18 C29 H29B 108.8 . . ? H29A C29 H29B 107.6 . . ? N23 C30 N20 113.6(16) . . ? N23 C30 H30A 108.8 . . ? N20 C30 H30A 108.8 . . ? N23 C30 H30B 108.8 . . ? N20 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? O6 C31 N21 125(2) . . ? O6 C31 N22 125.5(18) . . ? N21 C31 N22 109.7(18) . . ? N21 C32 N23 113.2(19) . . ? N21 C32 C57 114.2(18) . . ? N23 C32 C57 111.1(16) . . ? N21 C32 C33 103.9(14) . . ? N23 C32 C33 102.1(16) . . ? C57 C32 C33 112(2) . . ? N22 C33 N24 112.4(15) . . ? N22 C33 C60 114.2(18) . . ? N24 C33 C60 112.4(19) . . ? N22 C33 C32 101.9(18) . . ? N24 C33 C32 103.0(17) . . ? C60 C33 C32 111.9(15) . . ? O12 C34 N24 125(2) . . ? O12 C34 N23 124(2) . . ? N24 C34 N23 111.1(19) . . ? N1 C35 N22 116.2(18) . . ? N1 C35 H35A 108.2 . . ? N22 C35 H35A 108.2 . . ? N1 C35 H35B 108.2 . . ? N22 C35 H35B 108.2 . . ? H35A C35 H35B 107.4 . . ? N24 C36 N3 114.7(17) . . ? N24 C36 H36A 108.6 . . ? N3 C36 H36A 108.6 . . ? N24 C36 H36B 108.6 . . ? N3 C36 H36B 108.6 . . ? H36A C36 H36B 107.6 . . ? C2 C37 C38 111.2(17) . . ? C2 C37 H37A 109.4 . . ? C38 C37 H37A 109.4 . . ? C2 C37 H37B 109.4 . . ? C38 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? C37 C38 C39 113.2(19) . . ? C37 C38 H38A 108.9 . . ? C39 C38 H38A 108.9 . . ? C37 C38 H38B 108.9 . . ? C39 C38 H38B 108.9 . . ? H38A C38 H38B 107.8 . . ? C40 C39 C38 112.1(17) . . ? C40 C39 H39A 109.2 . . ? C38 C39 H39A 109.2 . . ? C40 C39 H39B 109.2 . . ? C38 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C3 C40 C39 110.8(19) . . ? C3 C40 H40A 109.5 . . ? C39 C40 H40A 109.5 . . ? C3 C40 H40B 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? C8 C41 C42 111(2) . . ? C8 C41 H41A 109.5 . . ? C42 C41 H41A 109.5 . . ? C8 C41 H41B 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 108.0 . . ? C43 C42 C41 114(2) . . ? C43 C42 H42A 108.9 . . ? C41 C42 H42A 108.9 . . ? C43 C42 H42B 108.9 . . ? C41 C42 H42B 108.9 . . ? H42A C42 H42B 107.7 . . ? C42 C43 C44 114.7(19) . . ? C42 C43 H43A 108.6 . . ? C44 C43 H43A 108.6 . . ? C42 C43 H43B 108.6 . . ? C44 C43 H43B 108.6 . . ? H43A C43 H43B 107.6 . . ? C43 C44 C9 111(2) . . ? C43 C44 H44A 109.4 . . ? C9 C44 H44A 109.4 . . ? C43 C44 H44B 109.4 . . ? C9 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? C14 C45 C46 110.4(19) . . ? C14 C45 H45A 109.6 . . ? C46 C45 H45A 109.6 . . ? C14 C45 H45B 109.6 . . ? C46 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? C47 C46 C45 113.0(17) . . ? C47 C46 H46A 109.0 . . ? C45 C46 H46A 109.0 . . ? C47 C46 H46B 109.0 . . ? C45 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? C46 C47 C48 113(2) . . ? C46 C47 H47A 109.0 . . ? C48 C47 H47A 109.0 . . ? C46 C47 H47B 109.0 . . ? C48 C47 H47B 109.0 . . ? H47A C47 H47B 107.8 . . ? C15 C48 C47 111(2) . . ? C15 C48 H48A 109.4 . . ? C47 C48 H48A 109.4 . . ? C15 C48 H48B 109.4 . . ? C47 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? C50 C49 C20 112.4(18) . . ? C50 C49 H49A 109.1 . . ? C20 C49 H49A 109.1 . . ? C50 C49 H49B 109.1 . . ? C20 C49 H49B 109.1 . . ? H49A C49 H49B 107.9 . . ? C49 C50 C51 114(2) . . ? C49 C50 H50A 108.7 . . ? C51 C50 H50A 108.7 . . ? C49 C50 H50B 108.7 . . ? C51 C50 H50B 108.7 . . ? H50A C50 H50B 107.6 . . ? C52 C51 C50 110.4(18) . . ? C52 C51 H51A 109.6 . . ? C50 C51 H51A 109.6 . . ? C52 C51 H51B 109.6 . . ? C50 C51 H51B 109.6 . . ? H51A C51 H51B 108.1 . . ? C21 C52 C51 109.3(18) . . ? C21 C52 H52A 109.8 . . ? C51 C52 H52A 109.8 . . ? C21 C52 H52B 109.8 . . ? C51 C52 H52B 109.8 . . ? H52A C52 H52B 108.3 . . ? C54 C53 C26 112(2) . . ? C54 C53 H53A 109.2 . . ? C26 C53 H53A 109.2 . . ? C54 C53 H53B 109.2 . . ? C26 C53 H53B 109.2 . . ? H53A C53 H53B 107.9 . . ? C53 C54 C55 114(2) . . ? C53 C54 H54A 108.8 . . ? C55 C54 H54A 108.8 . . ? C53 C54 H54B 108.8 . . ? C55 C54 H54B 108.8 . . ? H54A C54 H54B 107.7 . . ? C54 C55 C56 112(2) . . ? C54 C55 H55A 109.1 . . ? C56 C55 H55A 109.1 . . ? C54 C55 H55B 109.1 . . ? C56 C55 H55B 109.1 . . ? H55A C55 H55B 107.9 . . ? C27 C56 C55 109.7(19) . . ? C27 C56 H56A 109.7 . . ? C55 C56 H56A 109.7 . . ? C27 C56 H56B 109.7 . . ? C55 C56 H56B 109.7 . . ? H56A C56 H56B 108.2 . . ? C58 C57 C32 112(2) . . ? C58 C57 H57A 109.1 . . ? C32 C57 H57A 109.1 . . ? C58 C57 H57B 109.1 . . ? C32 C57 H57B 109.1 . . ? H57A C57 H57B 107.8 . . ? C57 C58 C59 114(2) . . ? C57 C58 H58A 108.7 . . ? C59 C58 H58A 108.7 . . ? C57 C58 H58B 108.7 . . ? C59 C58 H58B 108.7 . . ? H58A C58 H58B 107.6 . . ? C58 C59 C60 111(2) . . ? C58 C59 H59A 109.3 . . ? C60 C59 H59A 109.3 . . ? C58 C59 H59B 109.3 . . ? C60 C59 H59B 109.3 . . ? H59A C59 H59B 108.0 . . ? C33 C60 C59 109.9(19) . . ? C33 C60 H60A 109.7 . . ? C59 C60 H60A 109.7 . . ? C33 C60 H60B 109.7 . . ? C59 C60 H60B 109.7 . . ? H60A C60 H60B 108.2 . . ? C1 N1 C35 122.3(18) . . ? C1 N1 C2 112.8(15) . . ? C35 N1 C2 124.1(16) . . ? C1 N2 C3 112.6(14) . . ? C1 N2 C5 121.9(17) . . ? C3 N2 C5 124.8(16) . . ? C4 N3 C36 122.3(16) . . ? C4 N3 C2 112.6(13) . . ? C36 N3 C2 124.3(16) . . ? C4 N4 C6 121.7(17) . . ? C4 N4 C3 112.5(15) . . ? C6 N4 C3 125.1(14) . . ? C7 N5 C5 121.2(18) . . ? C7 N5 C8 112.3(18) . . ? C5 N5 C8 126.5(18) . . ? C7 N6 C9 113.4(19) . . ? C7 N6 C11 120.3(18) . . ? C9 N6 C11 126.0(18) . . ? C10 N7 C6 122.2(15) . . ? C10 N7 C8 111.3(16) . . ? C6 N7 C8 124.4(17) . . ? C10 N8 C12 122.0(17) . . ? C10 N8 C9 112.9(19) . . ? C12 N8 C9 124.5(15) . . ? C13 N9 C14 112.9(18) . . ? C13 N9 C11 124.1(19) . . ? C14 N9 C11 122.6(16) . . ? C13 N10 C17 124.8(19) . . ? C13 N10 C15 111.3(17) . . ? C17 N10 C15 123.2(19) . . ? C16 N11 C12 122.4(17) . . ? C16 N11 C14 113.5(18) . . ? C12 N11 C14 124.0(14) . . ? C16 N12 C15 112.7(16) . . ? C16 N12 C18 121.5(17) . . ? C15 N12 C18 124.5(19) . . ? C19 N13 C17 119.3(18) . . ? C19 N13 C20 111.2(15) . . ? C17 N13 C20 124.7(18) . . ? C19 N14 C23 121.6(19) . . ? C19 N14 C21 113.7(16) . . ? C23 N14 C21 124.3(15) . . ? C22 N15 C18 121.8(19) . . ? C22 N15 C20 112.4(16) . . ? C18 N15 C20 125.5(16) . . ? C22 N16 C24 120.9(18) . . ? C22 N16 C21 112.1(15) . . ? C24 N16 C21 125.5(17) . . ? C25 N17 C26 112.9(18) . . ? C25 N17 C23 120.9(16) . . ? C26 N17 C23 126.2(19) . . ? C25 N18 C29 121.9(18) . . ? C25 N18 C27 113.6(19) . . ? C29 N18 C27 124.5(18) . . ? C28 N19 C26 115.9(18) . . ? C28 N19 C24 118.2(18) . . ? C26 N19 C24 124.8(19) . . ? C28 N20 C27 112.8(19) . . ? C28 N20 C30 120.8(18) . . ? C27 N20 C30 125.2(17) . . ? C31 N21 C29 123.8(19) . . ? C31 N21 C32 111.8(18) . . ? C29 N21 C32 123.7(15) . . ? C31 N22 C35 119.9(17) . . ? C31 N22 C33 112.2(16) . . ? C35 N22 C33 125(2) . . ? C34 N23 C30 123.0(19) . . ? C34 N23 C32 111.3(19) . . ? C30 N23 C32 125.1(18) . . ? C34 N24 C36 124.6(18) . . ? C34 N24 C33 112.0(18) . . ? C36 N24 C33 123.1(18) . . ? C1 O1 Nd1 145.0(15) . . ? C7 O2 Nd1 126.5(11) . . ? C13 O3 Nd1 142.3(15) . . ? C10 O8 Nd2 157.1(16) . 2_666 ? C16 O9 Nd2 156.0(16) . 2_666 ? C34 O12 Nd2 145.6(13) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 4.867 _refine_diff_density_min -3.494 _refine_diff_density_rms 0.215 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 33 11 ' ' 2 -0.020 0.480 0.000 236 112 ' ' 3 0.244 0.854 0.480 95 43 ' ' 4 0.756 0.146 0.520 95 46 ' ' _platon_squeeze_details ; ; data_a6 _database_code_depnum_ccdc_archive 'CCDC 881908' #TrackingRef '110707qx-submit-cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C120 H208 Ce4 N60 O92' _chemical_formula_weight 4523.94 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.5784(9) _cell_length_b 15.6145(9) _cell_length_c 20.8875(17) _cell_angle_alpha 104.115(3) _cell_angle_beta 95.999(3) _cell_angle_gamma 119.254(2) _cell_volume 4146.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2316 _exptl_absorpt_coefficient_mu 1.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7363 _exptl_absorpt_correction_T_max 0.8119 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44618 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15766 _reflns_number_gt 14077 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+12.0928P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15766 _refine_ls_number_parameters 1172 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0483 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1173 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.012 _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 N27 N -0.6069(4) -0.5079(4) 0.6314(3) 0.0484(12) Uani 1 1 d . . . N28 N 0.6147(3) -0.0635(3) 0.9025(2) 0.0383(10) Uani 1 1 d . . . N29 N -0.0644(6) -0.6467(5) 0.5812(3) 0.0770(19) Uani 1 1 d . . . N30 N -0.4130(4) -0.8208(4) 0.6425(3) 0.077(2) Uani 1 1 d D . . O19 O -0.5331(4) -0.5071(4) 0.6606(3) 0.0710(13) Uani 1 1 d . . . O20 O -0.6383(5) -0.4586(5) 0.6623(3) 0.0932(19) Uani 1 1 d . . . O21 O -0.6495(6) -0.5617(5) 0.5701(3) 0.111(2) Uani 1 1 d . . . O22 O 0.6167(4) -0.0862(3) 0.95508(19) 0.0564(11) Uani 1 1 d . . . O23 O 0.6248(4) -0.1138(4) 0.8524(2) 0.0624(12) Uani 1 1 d . . . O24 O 0.6013(5) 0.0069(4) 0.9008(3) 0.094(2) Uani 1 1 d . . . O25 O -0.1247(5) -0.6910(5) 0.6109(3) 0.0810(15) Uani 1 1 d . . . O26 O 0.0228(5) -0.5656(5) 0.6083(4) 0.113(2) Uani 1 1 d . . . O27 O -0.0939(8) -0.6851(7) 0.5182(3) 0.162(4) Uani 1 1 d . . . O28 O -0.4045(4) -0.7535(3) 0.6933(3) 0.0777(15) Uani 1 1 d D . . O29 O -0.4283(8) -0.8027(8) 0.5886(4) 0.53(2) Uani 1 1 d D . . O30 O -0.4177(6) -0.9001(6) 0.6489(6) 0.180(5) Uani 1 1 d D . . N25 N 0.1531(3) 0.1340(3) 0.78753(18) 0.0292(8) Uani 1 1 d . . . N26 N 0.2004(3) 0.3697(3) 1.08989(18) 0.0307(8) Uani 1 1 d . . . O1W O -0.0993(3) -0.0301(2) 0.37798(16) 0.0373(8) Uani 1 1 d . . . O2W O 0.0634(2) 0.0234(2) 0.88464(15) 0.0296(7) Uani 1 1 d . . . O3W O 0.0261(2) 0.1072(2) 1.01137(15) 0.0330(7) Uani 1 1 d . . . O4W O -0.1365(3) 0.0744(2) 0.48975(15) 0.0344(7) Uani 1 1 d . . . O5W O 0.2214(3) 0.1222(3) 1.03415(16) 0.0360(7) Uani 1 1 d . . . O6W O -0.1166(3) -0.1698(3) 0.46614(16) 0.0421(9) Uani 1 1 d . . . O7W O -0.3821(3) -0.2757(3) 0.4405(2) 0.0571(11) Uani 1 1 d . . . O8W O -0.3529(3) -0.0709(4) 0.48342(18) 0.0579(12) Uani 1 1 d . . . O13 O 0.1892(2) 0.2053(2) 0.84531(14) 0.0312(7) Uani 1 1 d . . . O14 O 0.0793(3) 0.1164(3) 0.7478(2) 0.0561(11) Uani 1 1 d . . . O15 O 0.1958(4) 0.0879(4) 0.7724(2) 0.0722(14) Uani 1 1 d . . . O16 O 0.2611(2) 0.3382(3) 1.08742(16) 0.0373(8) Uani 1 1 d . . . O17 O 0.1293(2) 0.3307(2) 1.03713(16) 0.0334(7) Uani 1 1 d . . . O18 O 0.2094(3) 0.4340(3) 1.14173(19) 0.0511(10) Uani 1 1 d . . . Ce1 Ce 0.172197(16) 0.205910(16) 0.961778(10) 0.01898(7) Uani 1 1 d . . . Ce2 Ce -0.232642(17) -0.115474(17) 0.434949(10) 0.02225(7) Uani 1 1 d . . . C1 C 0.3839(3) 0.2075(3) 0.90139(18) 0.0164(7) Uani 1 1 d . . . C2 C 0.4671(3) 0.1628(3) 0.82412(18) 0.0166(7) Uani 1 1 d . . . C3 C 0.4918(3) 0.2754(3) 0.83262(18) 0.0171(7) Uani 1 1 d . . . C4 C 0.3978(3) 0.1650(3) 0.72099(19) 0.0172(7) Uani 1 1 d . . . C5 C 0.4580(3) 0.3953(3) 0.91899(18) 0.0173(7) Uani 1 1 d . . . H5A H 0.4512 0.3989 0.9655 0.021 Uiso 1 1 calc R . . H5B H 0.5284 0.4488 0.9229 0.021 Uiso 1 1 calc R . . C6 C 0.4460(3) 0.3460(3) 0.74523(19) 0.0168(7) Uani 1 1 d . . . H6A H 0.4337 0.3265 0.6954 0.020 Uiso 1 1 calc R . . H6B H 0.5149 0.4083 0.7657 0.020 Uiso 1 1 calc R . . C7 C 0.3085(3) 0.4081(3) 0.90964(18) 0.0162(7) Uani 1 1 d . . . C8 C 0.3955(3) 0.4536(3) 0.82717(18) 0.0147(7) Uani 1 1 d . . . C9 C 0.2981(3) 0.4613(3) 0.81587(17) 0.0135(7) Uani 1 1 d . . . C10 C 0.2827(3) 0.3326(3) 0.72136(18) 0.0154(7) Uani 1 1 d . . . C11 C 0.1622(3) 0.4255(3) 0.88534(18) 0.0174(7) Uani 1 1 d . . . H11A H 0.1619 0.4244 0.9320 0.021 Uiso 1 1 calc R . . H11B H 0.1649 0.4889 0.8836 0.021 Uiso 1 1 calc R . . C12 C 0.1505(3) 0.3752(3) 0.70773(19) 0.0174(7) Uani 1 1 d . . . H12A H 0.1620 0.4452 0.7183 0.021 Uiso 1 1 calc R . . H12B H 0.1477 0.3501 0.6593 0.021 Uiso 1 1 calc R . . C13 C 0.0096(3) 0.2483(3) 0.85443(18) 0.0175(7) Uani 1 1 d . . . C14 C 0.0159(3) 0.3347(3) 0.77625(18) 0.0150(7) Uani 1 1 d . . . C15 C -0.0946(3) 0.2353(3) 0.75852(18) 0.0157(7) Uani 1 1 d . . . C16 C -0.0189(3) 0.2159(3) 0.66949(18) 0.0164(7) Uani 1 1 d . . . C17 C -0.1688(3) 0.1036(3) 0.82188(19) 0.0187(7) Uani 1 1 d . . . H17A H -0.1494 0.1062 0.8688 0.022 Uiso 1 1 calc R . . H17B H -0.2271 0.1122 0.8179 0.022 Uiso 1 1 calc R . . C18 C -0.2007(3) 0.0829(3) 0.64549(18) 0.0163(7) Uani 1 1 d . . . H18A H -0.1972 0.0763 0.5981 0.020 Uiso 1 1 calc R . . H18B H -0.2553 0.0957 0.6522 0.020 Uiso 1 1 calc R . . C19 C -0.1918(3) -0.0675(3) 0.8003(2) 0.0198(8) Uani 1 1 d . . . C20 C -0.2738(3) -0.0492(3) 0.70860(19) 0.0178(7) Uani 1 1 d . . . C21 C -0.2988(3) -0.1643(3) 0.6895(2) 0.0205(8) Uani 1 1 d . . . C22 C -0.2175(3) -0.0876(3) 0.61231(18) 0.0176(7) Uani 1 1 d . . . C23 C -0.2619(3) -0.2559(3) 0.7654(2) 0.0231(8) Uani 1 1 d . . . H23A H -0.2555 -0.2437 0.8144 0.028 Uiso 1 1 calc R . . H23B H -0.3313 -0.3146 0.7406 0.028 Uiso 1 1 calc R . . C24 C -0.2521(3) -0.2639(3) 0.5967(2) 0.0221(8) Uani 1 1 d . . . H24A H -0.2391 -0.2596 0.5523 0.026 Uiso 1 1 calc R . . H24B H -0.3202 -0.3256 0.5878 0.026 Uiso 1 1 calc R . . C25 C -0.1078(3) -0.2592(3) 0.7927(2) 0.0196(8) Uani 1 1 d . . . C26 C -0.1983(3) -0.3404(3) 0.6767(2) 0.0207(8) Uani 1 1 d . . . C27 C -0.1023(3) -0.3501(3) 0.68732(19) 0.0192(8) Uani 1 1 d . . . C28 C -0.0867(3) -0.2489(3) 0.61765(19) 0.0199(8) Uani 1 1 d . . . C29 C 0.0318(3) -0.2895(3) 0.7988(2) 0.0203(8) Uani 1 1 d . . . H29A H 0.0269 -0.3565 0.7825 0.024 Uiso 1 1 calc R . . H29B H 0.0313 -0.2752 0.8471 0.024 Uiso 1 1 calc R . . C30 C 0.0451(3) -0.2904(3) 0.6296(2) 0.0212(8) Uani 1 1 d . . . H30A H 0.0336 -0.3599 0.6232 0.025 Uiso 1 1 calc R . . H30B H 0.0487 -0.2787 0.5857 0.025 Uiso 1 1 calc R . . C31 C 0.1858(3) -0.1130(3) 0.84305(19) 0.0193(8) Uani 1 1 d . . . C32 C 0.1787(3) -0.2245(3) 0.74202(19) 0.0183(7) Uani 1 1 d . . . C33 C 0.2899(3) -0.1233(3) 0.77143(18) 0.0178(7) Uani 1 1 d . . . C34 C 0.2165(3) -0.1336(3) 0.6643(2) 0.0210(8) Uani 1 1 d . . . C35 C 0.3614(3) 0.0341(3) 0.88243(18) 0.0189(8) Uani 1 1 d . . . H35A H 0.4181 0.0237 0.8907 0.023 Uiso 1 1 calc R . . H35B H 0.3396 0.0415 0.9247 0.023 Uiso 1 1 calc R . . C36 C 0.3954(3) 0.0048(3) 0.71370(19) 0.0190(8) Uani 1 1 d . . . H36A H 0.3934 0.0006 0.6659 0.023 Uiso 1 1 calc R . . H36B H 0.4534 0.0006 0.7318 0.023 Uiso 1 1 calc R . . C37 C 0.5639(3) 0.1627(3) 0.8451(2) 0.0229(8) Uani 1 1 d . . . H37A H 0.5454 0.0935 0.8464 0.027 Uiso 1 1 calc R . . H37B H 0.6029 0.1772 0.8111 0.027 Uiso 1 1 calc R . . C38 C 0.6298(3) 0.2445(3) 0.9153(2) 0.0300(9) Uani 1 1 d . . . H38A H 0.6921 0.2439 0.9268 0.036 Uiso 1 1 calc R . . H38B H 0.5926 0.2261 0.9497 0.036 Uiso 1 1 calc R . . C39 C 0.6592(3) 0.3552(3) 0.9183(2) 0.0265(9) Uani 1 1 d . . . H39A H 0.6417 0.3861 0.9575 0.032 Uiso 1 1 calc R . . H39B H 0.7331 0.3985 0.9254 0.032 Uiso 1 1 calc R . . C40 C 0.6057(3) 0.3563(3) 0.8534(2) 0.0210(8) Uani 1 1 d . . . H40A H 0.6166 0.4258 0.8611 0.025 Uiso 1 1 calc R . . H40B H 0.6353 0.3419 0.8161 0.025 Uiso 1 1 calc R . . C41 C 0.4940(3) 0.5561(3) 0.8379(2) 0.0216(8) Uani 1 1 d . . . H41A H 0.5524 0.5497 0.8507 0.026 Uiso 1 1 calc R . . H41B H 0.4955 0.5709 0.7949 0.026 Uiso 1 1 calc R . . C42 C 0.5034(4) 0.6463(3) 0.8935(2) 0.0317(10) Uani 1 1 d . . . H42A H 0.5617 0.7119 0.8937 0.038 Uiso 1 1 calc R . . H42B H 0.5174 0.6390 0.9380 0.038 Uiso 1 1 calc R . . C43 C 0.4082(3) 0.6522(3) 0.8842(2) 0.0284(9) Uani 1 1 d . . . H43A H 0.3808 0.6438 0.9239 0.034 Uiso 1 1 calc R . . H43B H 0.4277 0.7216 0.8831 0.034 Uiso 1 1 calc R . . C44 C 0.3251(3) 0.5707(3) 0.8198(2) 0.0200(8) Uani 1 1 d . . . H44A H 0.3482 0.5851 0.7796 0.024 Uiso 1 1 calc R . . H44B H 0.2642 0.5747 0.8194 0.024 Uiso 1 1 calc R . . C45 C 0.0138(3) 0.4326(3) 0.7834(2) 0.0210(8) Uani 1 1 d . . . H45A H -0.0209 0.4268 0.7392 0.025 Uiso 1 1 calc R . . H45B H 0.0838 0.4932 0.7970 0.025 Uiso 1 1 calc R . . C46 C -0.0414(3) 0.4485(3) 0.8367(2) 0.0276(9) Uani 1 1 d . . . H46A H -0.0508 0.5058 0.8354 0.033 Uiso 1 1 calc R . . H46B H 0.0013 0.4691 0.8823 0.033 Uiso 1 1 calc R . . C47 C -0.1462(3) 0.3505(3) 0.8258(2) 0.0267(9) Uani 1 1 d . . . H47A H -0.1448 0.3262 0.8647 0.032 Uiso 1 1 calc R . . H47B H -0.1982 0.3687 0.8243 0.032 Uiso 1 1 calc R . . C48 C -0.1753(3) 0.2630(3) 0.7602(2) 0.0209(8) Uani 1 1 d . . . H48A H -0.1839 0.2844 0.7209 0.025 Uiso 1 1 calc R . . H48B H -0.2407 0.2012 0.7566 0.025 Uiso 1 1 calc R . . C49 C -0.3703(3) -0.0456(3) 0.7070(2) 0.0218(8) Uani 1 1 d . . . H49A H -0.4012 -0.0706 0.7423 0.026 Uiso 1 1 calc R . . H49B H -0.3527 0.0265 0.7168 0.026 Uiso 1 1 calc R . . C50 C -0.4465(3) -0.1135(3) 0.6370(2) 0.0260(9) Uani 1 1 d . . . H50A H -0.4195 -0.0816 0.6030 0.031 Uiso 1 1 calc R . . H50B H -0.5104 -0.1162 0.6383 0.031 Uiso 1 1 calc R . . C51 C -0.4684(3) -0.2249(3) 0.6150(3) 0.0351(10) Uani 1 1 d . . . H51A H -0.5420 -0.2742 0.6053 0.042 Uiso 1 1 calc R . . H51B H -0.4484 -0.2386 0.5725 0.042 Uiso 1 1 calc R . . C52 C -0.4133(3) -0.2445(3) 0.6680(2) 0.0276(9) Uani 1 1 d . . . H52A H -0.4255 -0.3147 0.6493 0.033 Uiso 1 1 calc R . . H52B H -0.4403 -0.2412 0.7083 0.033 Uiso 1 1 calc R . . C53 C -0.2984(3) -0.4469(3) 0.6469(2) 0.0287(9) Uani 1 1 d . . . H53A H -0.3562 -0.4375 0.6474 0.034 Uiso 1 1 calc R . . H53B H -0.3036 -0.4808 0.5993 0.034 Uiso 1 1 calc R . . C54 C -0.3027(4) -0.5157(3) 0.6888(3) 0.0374(11) Uani 1 1 d . . . H54A H -0.3050 -0.4848 0.7350 0.045 Uiso 1 1 calc R . . H54B H -0.3658 -0.5845 0.6678 0.045 Uiso 1 1 calc R . . C55 C -0.2125(3) -0.5297(3) 0.6944(3) 0.0346(10) Uani 1 1 d . . . H55A H -0.2374 -0.6034 0.6716 0.042 Uiso 1 1 calc R . . H55B H -0.1812 -0.5111 0.7428 0.042 Uiso 1 1 calc R . . C56 C -0.1313(3) -0.4638(3) 0.6628(2) 0.0252(8) Uani 1 1 d . . . H56A H -0.1571 -0.4930 0.6128 0.030 Uiso 1 1 calc R . . H56B H -0.0704 -0.4665 0.6752 0.030 Uiso 1 1 calc R . . C57 C 0.1789(3) -0.3248(3) 0.7289(2) 0.0227(8) Uani 1 1 d . . . H57A H 0.1940 -0.3341 0.7725 0.027 Uiso 1 1 calc R . . H57B H 0.1114 -0.3847 0.7014 0.027 Uiso 1 1 calc R . . C58 C 0.2587(3) -0.3198(3) 0.6911(2) 0.0282(9) Uani 1 1 d . . . H58A H 0.2436 -0.3099 0.6477 0.034 Uiso 1 1 calc R . . H58B H 0.2556 -0.3861 0.6805 0.034 Uiso 1 1 calc R . . C59 C 0.3665(3) -0.2305(3) 0.7336(2) 0.0289(9) Uani 1 1 d . . . H59A H 0.4025 -0.2597 0.7520 0.035 Uiso 1 1 calc R . . H59B H 0.4038 -0.1955 0.7036 0.035 Uiso 1 1 calc R . . C60 C 0.3674(3) -0.1503(3) 0.7925(2) 0.0242(8) Uani 1 1 d . . . H60A H 0.3524 -0.1777 0.8301 0.029 Uiso 1 1 calc R . . H60B H 0.4356 -0.0866 0.8093 0.029 Uiso 1 1 calc R . . N1 N 0.3988(2) 0.1309(2) 0.86828(16) 0.0175(6) Uani 1 1 d . . . N2 N 0.4412(2) 0.2941(2) 0.88395(15) 0.0164(6) Uani 1 1 d . . . N3 N 0.4134(2) 0.1055(2) 0.75214(16) 0.0172(6) Uani 1 1 d . . . N4 N 0.4413(2) 0.2623(2) 0.76532(15) 0.0169(6) Uani 1 1 d . . . N5 N 0.3910(2) 0.4214(2) 0.88765(15) 0.0153(6) Uani 1 1 d . . . N6 N 0.2541(2) 0.4313(2) 0.87115(15) 0.0154(6) Uani 1 1 d . . . N7 N 0.3732(2) 0.3713(2) 0.76547(15) 0.0152(6) Uani 1 1 d . . . N8 N 0.2367(2) 0.3825(2) 0.74868(15) 0.0154(6) Uani 1 1 d . . . N9 N 0.0677(2) 0.3358(2) 0.83888(15) 0.0161(6) Uani 1 1 d . . . N10 N -0.0843(2) 0.1906(2) 0.81081(15) 0.0165(6) Uani 1 1 d . . . N11 N 0.0536(2) 0.3072(2) 0.71822(15) 0.0161(6) Uani 1 1 d . . . N12 N -0.1054(2) 0.1717(2) 0.69069(15) 0.0155(6) Uani 1 1 d . . . N13 N -0.2008(2) 0.0021(2) 0.77569(16) 0.0190(6) Uani 1 1 d . . . N14 N -0.2466(2) -0.1630(2) 0.75134(16) 0.0201(7) Uani 1 1 d . . . N15 N -0.2269(2) -0.0150(2) 0.65538(15) 0.0172(6) Uani 1 1 d . . . N16 N -0.2515(2) -0.1724(2) 0.63313(16) 0.0202(7) Uani 1 1 d . . . N17 N -0.1906(3) -0.2838(3) 0.74597(17) 0.0226(7) Uani 1 1 d . . . N18 N -0.0571(2) -0.2995(2) 0.76088(16) 0.0203(7) Uani 1 1 d . . . N19 N -0.1778(2) -0.2779(2) 0.63250(16) 0.0203(7) Uani 1 1 d . . . N20 N -0.0411(3) -0.2889(3) 0.64842(17) 0.0220(7) Uani 1 1 d . . . N21 N 0.1282(2) -0.2091(2) 0.79425(16) 0.0195(7) Uani 1 1 d . . . N22 N 0.2778(2) -0.0582(2) 0.82945(16) 0.0187(6) Uani 1 1 d . . . N23 N 0.1413(2) -0.2138(2) 0.67910(16) 0.0197(7) Uani 1 1 d . . . N24 N 0.3037(2) -0.0835(2) 0.71508(16) 0.0183(6) Uani 1 1 d . . . O1 O 0.3332(2) 0.2027(2) 0.94310(13) 0.0213(6) Uani 1 1 d . . . O2 O 0.2894(2) 0.3831(2) 0.96108(13) 0.0200(5) Uani 1 1 d . . . O3 O 0.0377(2) 0.2269(2) 0.90278(14) 0.0240(6) Uani 1 1 d . . . O4 O -0.1423(2) -0.0466(2) 0.85725(14) 0.0245(6) Uani 1 1 d . . . O5 O -0.0831(2) -0.2104(2) 0.85360(14) 0.0256(6) Uani 1 1 d . . . O6 O 0.1600(2) -0.0815(2) 0.89187(14) 0.0252(6) Uani 1 1 d . . . O7 O 0.3529(2) 0.1352(2) 0.66023(13) 0.0224(6) Uani 1 1 d . . . O8 O 0.2483(2) 0.2646(2) 0.66505(13) 0.0217(6) Uani 1 1 d . . . O9 O -0.0088(2) 0.1798(2) 0.61366(13) 0.0237(6) Uani 1 1 d . . . O10 O -0.1848(2) -0.0803(2) 0.56094(13) 0.0220(6) Uani 1 1 d . . . O11 O -0.0508(2) -0.1955(2) 0.58163(15) 0.0274(6) Uani 1 1 d . . . O12 O 0.2085(2) -0.1115(3) 0.61265(16) 0.0363(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N27 0.053(3) 0.047(3) 0.060(3) 0.034(2) 0.033(3) 0.027(2) N28 0.031(2) 0.037(2) 0.040(2) 0.0157(18) -0.0024(18) 0.0140(18) N29 0.127(6) 0.076(4) 0.049(3) 0.024(3) 0.027(4) 0.067(4) N30 0.050(3) 0.059(3) 0.048(3) -0.014(3) 0.034(3) -0.013(3) O19 0.064(3) 0.083(3) 0.097(4) 0.060(3) 0.033(3) 0.045(3) O20 0.121(5) 0.130(5) 0.099(4) 0.055(4) 0.070(4) 0.102(5) O21 0.146(6) 0.112(5) 0.061(3) 0.009(3) -0.004(4) 0.075(5) O22 0.090(3) 0.058(2) 0.0313(19) 0.0194(18) 0.014(2) 0.045(2) O23 0.067(3) 0.099(3) 0.041(2) 0.037(2) 0.027(2) 0.050(3) O24 0.108(4) 0.061(3) 0.099(4) 0.014(3) -0.042(3) 0.054(3) O25 0.097(4) 0.109(4) 0.075(3) 0.058(3) 0.040(3) 0.067(4) O26 0.076(4) 0.084(4) 0.117(5) -0.019(4) -0.012(4) 0.029(3) O27 0.215(10) 0.160(7) 0.044(3) 0.016(4) 0.037(5) 0.059(7) O28 0.071(3) 0.064(3) 0.084(4) 0.019(3) 0.041(3) 0.025(3) O29 0.217(14) 0.46(3) 0.216(13) -0.258(16) 0.152(12) -0.163(15) O30 0.080(5) 0.075(5) 0.369(17) 0.051(7) 0.081(7) 0.038(4) N25 0.033(2) 0.0344(19) 0.0192(17) 0.0091(15) 0.0058(15) 0.0178(17) N26 0.033(2) 0.0241(17) 0.0253(19) 0.0097(15) 0.0145(16) 0.0064(16) O1W 0.0395(19) 0.0322(16) 0.0275(16) 0.0071(13) 0.0157(14) 0.0103(14) O2W 0.0294(16) 0.0252(14) 0.0298(16) 0.0103(12) 0.0072(13) 0.0111(13) O3W 0.0314(17) 0.0300(15) 0.0245(15) 0.0123(12) 0.0126(13) 0.0048(13) O4W 0.051(2) 0.0306(16) 0.0201(14) 0.0071(12) 0.0025(14) 0.0223(15) O5W 0.0388(18) 0.0442(18) 0.0327(17) 0.0269(15) 0.0094(14) 0.0215(15) O6W 0.044(2) 0.079(3) 0.0226(16) 0.0151(16) 0.0122(14) 0.047(2) O7W 0.052(2) 0.045(2) 0.042(2) 0.0061(17) 0.0241(18) 0.0041(18) O8W 0.051(2) 0.099(3) 0.0275(18) -0.0046(19) 0.0040(16) 0.056(2) O13 0.0375(18) 0.0269(15) 0.0182(14) 0.0068(12) 0.0066(13) 0.0099(13) O14 0.054(2) 0.064(3) 0.041(2) -0.0005(18) -0.0144(18) 0.039(2) O15 0.079(3) 0.099(4) 0.052(3) -0.001(2) 0.011(2) 0.070(3) O16 0.0295(17) 0.050(2) 0.0247(16) 0.0148(14) 0.0047(13) 0.0153(15) O17 0.0310(17) 0.0385(17) 0.0283(16) 0.0104(13) 0.0072(14) 0.0174(14) O18 0.065(3) 0.0298(17) 0.0367(19) 0.0040(15) 0.0228(18) 0.0119(17) Ce1 0.01903(12) 0.02078(12) 0.01466(11) 0.00941(8) 0.00399(8) 0.00744(9) Ce2 0.02105(13) 0.02913(13) 0.01392(11) 0.00227(9) 0.00262(9) 0.01416(10) C1 0.0168(18) 0.0185(17) 0.0145(17) 0.0075(14) 0.0012(14) 0.0097(14) C2 0.0159(18) 0.0170(17) 0.0174(17) 0.0068(14) 0.0046(14) 0.0086(14) C3 0.0165(18) 0.0207(18) 0.0167(17) 0.0084(14) 0.0028(14) 0.0112(15) C4 0.0150(18) 0.0210(18) 0.0205(18) 0.0108(15) 0.0081(15) 0.0108(15) C5 0.0185(18) 0.0170(17) 0.0130(16) 0.0051(13) -0.0034(14) 0.0085(14) C6 0.0201(19) 0.0212(18) 0.0172(17) 0.0117(14) 0.0104(15) 0.0133(15) C7 0.0173(18) 0.0107(15) 0.0147(17) 0.0025(13) 0.0024(14) 0.0044(14) C8 0.0162(18) 0.0130(16) 0.0150(17) 0.0063(13) 0.0043(14) 0.0070(14) C9 0.0152(17) 0.0136(16) 0.0128(16) 0.0062(13) 0.0044(13) 0.0076(14) C10 0.0172(18) 0.0160(16) 0.0151(17) 0.0088(14) 0.0056(14) 0.0085(14) C11 0.0150(18) 0.0206(18) 0.0136(16) 0.0036(14) 0.0049(14) 0.0083(15) C12 0.0152(18) 0.0252(18) 0.0157(17) 0.0112(14) 0.0058(14) 0.0113(15) C13 0.0196(19) 0.0200(17) 0.0138(17) 0.0038(14) 0.0051(14) 0.0118(15) C14 0.0143(17) 0.0206(17) 0.0118(16) 0.0066(13) 0.0045(13) 0.0100(14) C15 0.0171(18) 0.0185(17) 0.0124(16) 0.0072(14) 0.0043(14) 0.0093(14) C16 0.0159(18) 0.0227(18) 0.0152(17) 0.0088(14) 0.0043(14) 0.0125(15) C17 0.0189(19) 0.0208(18) 0.0160(17) 0.0079(14) 0.0084(15) 0.0088(15) C18 0.0179(18) 0.0192(17) 0.0145(17) 0.0083(14) 0.0035(14) 0.0107(15) C19 0.0145(18) 0.0247(19) 0.025(2) 0.0130(16) 0.0104(15) 0.0112(15) C20 0.0184(18) 0.0176(17) 0.0173(17) 0.0079(14) 0.0065(15) 0.0084(15) C21 0.021(2) 0.0208(18) 0.0231(19) 0.0104(15) 0.0082(16) 0.0116(16) C22 0.0132(17) 0.0203(18) 0.0158(17) 0.0034(14) 0.0010(14) 0.0082(14) C23 0.024(2) 0.0199(18) 0.031(2) 0.0149(16) 0.0130(17) 0.0113(16) C24 0.023(2) 0.0216(18) 0.0198(18) 0.0033(15) 0.0015(15) 0.0131(16) C25 0.0187(19) 0.0148(17) 0.023(2) 0.0114(15) 0.0075(15) 0.0051(14) C26 0.0161(19) 0.0185(18) 0.0242(19) 0.0068(15) 0.0031(15) 0.0076(15) C27 0.0161(18) 0.0181(17) 0.0216(19) 0.0075(15) 0.0036(15) 0.0077(15) C28 0.024(2) 0.0187(17) 0.0157(17) 0.0058(14) 0.0030(15) 0.0113(15) C29 0.0195(19) 0.0199(18) 0.0216(19) 0.0115(15) 0.0046(15) 0.0087(15) C30 0.0199(19) 0.0236(19) 0.0196(18) 0.0071(15) 0.0044(15) 0.0115(16) C31 0.0201(19) 0.0194(18) 0.0202(19) 0.0098(15) 0.0023(15) 0.0109(15) C32 0.0180(19) 0.0189(18) 0.0192(18) 0.0082(14) 0.0029(15) 0.0103(15) C33 0.023(2) 0.0157(17) 0.0163(17) 0.0084(14) 0.0043(15) 0.0103(15) C34 0.023(2) 0.0201(18) 0.0220(19) 0.0109(15) 0.0053(16) 0.0113(16) C35 0.0219(19) 0.0174(17) 0.0156(17) 0.0084(14) 0.0019(15) 0.0085(15) C36 0.0203(19) 0.0165(17) 0.0208(18) 0.0068(14) 0.0085(15) 0.0095(15) C37 0.021(2) 0.0221(19) 0.029(2) 0.0107(16) 0.0038(16) 0.0133(16) C38 0.021(2) 0.034(2) 0.031(2) 0.0137(18) -0.0033(17) 0.0126(18) C39 0.019(2) 0.027(2) 0.028(2) 0.0073(17) -0.0003(16) 0.0100(16) C40 0.0138(18) 0.0221(18) 0.026(2) 0.0105(15) 0.0028(15) 0.0080(15) C41 0.0168(19) 0.0169(18) 0.028(2) 0.0110(15) 0.0035(15) 0.0055(15) C42 0.035(2) 0.0174(19) 0.028(2) 0.0022(16) -0.0064(18) 0.0088(18) C43 0.030(2) 0.0150(18) 0.029(2) 0.0018(16) 0.0094(18) 0.0066(16) C44 0.025(2) 0.0171(17) 0.0240(19) 0.0115(15) 0.0087(16) 0.0128(15) C45 0.0211(19) 0.0174(17) 0.0259(19) 0.0074(15) 0.0064(16) 0.0111(15) C46 0.030(2) 0.026(2) 0.028(2) 0.0030(17) 0.0091(18) 0.0175(18) C47 0.028(2) 0.030(2) 0.028(2) 0.0101(17) 0.0139(18) 0.0190(18) C48 0.0192(19) 0.0230(19) 0.0222(19) 0.0079(15) 0.0065(15) 0.0123(16) C49 0.020(2) 0.0264(19) 0.0238(19) 0.0114(16) 0.0088(16) 0.0142(16) C50 0.018(2) 0.032(2) 0.026(2) 0.0106(17) 0.0026(16) 0.0121(17) C51 0.021(2) 0.030(2) 0.040(3) 0.0009(19) -0.0001(19) 0.0095(18) C52 0.018(2) 0.0207(19) 0.041(2) 0.0100(17) 0.0085(18) 0.0085(16) C53 0.019(2) 0.0190(19) 0.043(3) 0.0087(18) 0.0025(18) 0.0076(16) C54 0.030(2) 0.021(2) 0.060(3) 0.019(2) 0.017(2) 0.0095(18) C55 0.028(2) 0.024(2) 0.048(3) 0.017(2) 0.008(2) 0.0091(18) C56 0.025(2) 0.0200(19) 0.029(2) 0.0061(16) 0.0038(17) 0.0124(16) C57 0.025(2) 0.0188(18) 0.025(2) 0.0097(15) 0.0039(16) 0.0118(16) C58 0.035(2) 0.025(2) 0.030(2) 0.0086(17) 0.0090(19) 0.0207(19) C59 0.028(2) 0.027(2) 0.043(3) 0.0175(19) 0.0153(19) 0.0188(18) C60 0.021(2) 0.0220(19) 0.030(2) 0.0122(16) 0.0018(16) 0.0113(16) N1 0.0234(17) 0.0157(14) 0.0176(15) 0.0098(12) 0.0058(13) 0.0115(13) N2 0.0161(15) 0.0166(14) 0.0169(15) 0.0065(12) 0.0050(12) 0.0086(12) N3 0.0203(16) 0.0171(15) 0.0168(15) 0.0071(12) 0.0047(12) 0.0113(13) N4 0.0200(16) 0.0178(15) 0.0163(15) 0.0092(12) 0.0030(12) 0.0113(13) N5 0.0196(16) 0.0178(14) 0.0143(14) 0.0096(12) 0.0055(12) 0.0119(13) N6 0.0149(15) 0.0183(14) 0.0130(14) 0.0072(12) 0.0053(12) 0.0078(12) N7 0.0153(15) 0.0177(14) 0.0138(14) 0.0052(12) 0.0052(12) 0.0095(12) N8 0.0137(15) 0.0180(14) 0.0140(14) 0.0047(12) 0.0040(12) 0.0084(12) N9 0.0152(15) 0.0175(14) 0.0131(14) 0.0059(12) 0.0029(12) 0.0068(12) N10 0.0172(16) 0.0175(15) 0.0158(15) 0.0092(12) 0.0044(12) 0.0084(12) N11 0.0168(16) 0.0204(15) 0.0135(14) 0.0063(12) 0.0052(12) 0.0111(13) N12 0.0157(15) 0.0168(14) 0.0126(14) 0.0051(12) 0.0041(12) 0.0076(12) N13 0.0188(16) 0.0201(15) 0.0165(15) 0.0084(12) 0.0047(13) 0.0081(13) N14 0.0230(17) 0.0210(16) 0.0212(16) 0.0113(13) 0.0066(13) 0.0131(14) N15 0.0193(16) 0.0186(15) 0.0138(14) 0.0066(12) 0.0073(12) 0.0090(13) N16 0.0220(17) 0.0207(16) 0.0183(15) 0.0056(13) 0.0071(13) 0.0119(13) N17 0.0224(17) 0.0234(16) 0.0243(17) 0.0092(13) 0.0090(14) 0.0129(14) N18 0.0179(16) 0.0226(16) 0.0197(16) 0.0082(13) 0.0044(13) 0.0100(13) N19 0.0209(17) 0.0215(16) 0.0198(16) 0.0075(13) 0.0030(13) 0.0125(13) N20 0.0200(17) 0.0263(17) 0.0209(16) 0.0101(13) 0.0067(13) 0.0121(14) N21 0.0160(16) 0.0200(15) 0.0204(16) 0.0079(13) 0.0061(13) 0.0073(13) N22 0.0188(16) 0.0183(15) 0.0185(15) 0.0079(12) 0.0046(13) 0.0089(13) N23 0.0178(16) 0.0210(15) 0.0185(15) 0.0088(13) 0.0016(13) 0.0087(13) N24 0.0202(16) 0.0172(15) 0.0166(15) 0.0075(12) 0.0041(13) 0.0087(13) O1 0.0262(15) 0.0224(13) 0.0176(13) 0.0093(11) 0.0089(11) 0.0129(11) O2 0.0226(14) 0.0217(13) 0.0134(12) 0.0081(10) 0.0062(10) 0.0090(11) O3 0.0205(14) 0.0313(15) 0.0182(13) 0.0148(11) 0.0023(11) 0.0101(12) O4 0.0260(15) 0.0284(14) 0.0218(14) 0.0128(12) 0.0057(12) 0.0147(12) O5 0.0284(15) 0.0265(14) 0.0214(14) 0.0091(12) 0.0080(12) 0.0135(12) O6 0.0254(15) 0.0261(14) 0.0224(14) 0.0078(11) 0.0086(12) 0.0122(12) O7 0.0276(15) 0.0237(13) 0.0176(13) 0.0081(11) 0.0030(11) 0.0150(12) O8 0.0202(14) 0.0255(14) 0.0160(13) 0.0012(11) 0.0021(11) 0.0128(11) O9 0.0224(14) 0.0320(15) 0.0129(13) 0.0027(11) 0.0064(11) 0.0135(12) O10 0.0243(14) 0.0264(14) 0.0173(13) 0.0074(11) 0.0072(11) 0.0147(12) O11 0.0296(16) 0.0338(16) 0.0252(15) 0.0182(13) 0.0078(12) 0.0175(13) O12 0.0302(17) 0.0388(17) 0.0289(16) 0.0217(14) -0.0007(13) 0.0077(14) _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 N27 O20 1.200(7) . ? N27 O19 1.235(7) . ? N27 O21 1.240(7) . ? N28 O23 1.221(6) . ? N28 O24 1.223(6) . ? N28 O22 1.235(5) . ? N29 O25 1.201(8) . ? N29 O27 1.233(8) . ? N29 O26 1.257(9) . ? N30 O28 1.242(2) . ? N30 O30 1.245(2) . ? N30 O29 1.253(2) . ? N25 O15 1.210(6) . ? N25 O14 1.211(5) . ? N25 O13 1.266(5) . ? N26 O18 1.225(5) . ? N26 O17 1.253(5) . ? N26 O16 1.261(5) . ? O1W Ce2 2.469(3) . ? O2W Ce1 2.462(3) . ? O3W Ce1 2.544(3) . ? O4W Ce2 2.448(3) . ? O5W Ce1 2.507(3) . ? O6W Ce2 2.436(3) . ? O7W Ce2 2.489(4) . ? O8W Ce2 2.519(3) . ? O13 Ce1 2.473(3) . ? O16 Ce1 2.621(3) . ? O17 Ce1 2.592(3) . ? Ce1 O2 2.465(3) . ? Ce1 O3 2.519(3) . ? Ce1 O1 2.600(3) . ? Ce2 O7 2.432(3) 2_556 ? Ce2 O10 2.503(3) . ? Ce2 O8 2.610(3) 2_556 ? C1 O1 1.228(5) . ? C1 N1 1.366(5) . ? C1 N2 1.373(5) . ? C2 N3 1.453(5) . ? C2 N1 1.464(5) . ? C2 C37 1.526(5) . ? C2 C3 1.564(5) . ? C3 N2 1.451(5) . ? C3 N4 1.452(5) . ? C3 C40 1.521(5) . ? C4 O7 1.235(5) . ? C4 N4 1.342(5) . ? C4 N3 1.352(5) . ? C5 N5 1.445(5) . ? C5 N2 1.447(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.440(5) . ? C6 N7 1.441(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.246(4) . ? C7 N6 1.341(5) . ? C7 N5 1.347(5) . ? C8 N7 1.447(5) . ? C8 N5 1.465(4) . ? C8 C41 1.523(5) . ? C8 C9 1.577(5) . ? C9 N8 1.458(4) . ? C9 N6 1.462(4) . ? C9 C44 1.526(5) . ? C10 O8 1.225(4) . ? C10 N7 1.351(5) . ? C10 N8 1.365(5) . ? C11 N9 1.447(5) . ? C11 N6 1.456(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.439(5) . ? C12 N8 1.451(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.240(5) . ? C13 N10 1.348(5) . ? C13 N9 1.363(5) . ? C14 N9 1.456(4) . ? C14 N11 1.463(5) . ? C14 C45 1.517(5) . ? C14 C15 1.575(5) . ? C15 N12 1.457(5) . ? C15 N10 1.467(4) . ? C15 C48 1.518(5) . ? C16 O9 1.227(5) . ? C16 N11 1.350(5) . ? C16 N12 1.361(5) . ? C17 N13 1.439(5) . ? C17 N10 1.449(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.440(5) . ? C18 N15 1.452(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.221(5) . ? C19 N14 1.352(5) . ? C19 N13 1.367(5) . ? C20 N13 1.458(5) . ? C20 N15 1.460(5) . ? C20 C49 1.529(5) . ? C20 C21 1.573(5) . ? C21 N14 1.444(5) . ? C21 N16 1.464(5) . ? C21 C52 1.525(5) . ? C22 O10 1.242(5) . ? C22 N15 1.344(5) . ? C22 N16 1.366(5) . ? C23 N17 1.437(5) . ? C23 N14 1.460(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.442(5) . ? C24 N19 1.446(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.218(5) . ? C25 N17 1.355(5) . ? C25 N18 1.361(5) . ? C26 N19 1.450(5) . ? C26 N17 1.459(5) . ? C26 C53 1.531(5) . ? C26 C27 1.573(5) . ? C27 N18 1.456(5) . ? C27 N20 1.460(5) . ? C27 C56 1.531(5) . ? C28 O11 1.230(5) . ? C28 N20 1.357(5) . ? C28 N19 1.360(5) . ? C29 N18 1.439(5) . ? C29 N21 1.444(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N23 1.438(5) . ? C30 N20 1.447(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O6 1.216(5) . ? C31 N21 1.358(5) . ? C31 N22 1.368(5) . ? C32 N21 1.450(5) . ? C32 N23 1.461(5) . ? C32 C57 1.524(5) . ? C32 C33 1.582(5) . ? C33 N24 1.448(5) . ? C33 N22 1.473(5) . ? C33 C60 1.518(5) . ? C34 O12 1.222(5) . ? C34 N24 1.356(5) . ? C34 N23 1.367(5) . ? C35 N22 1.444(5) . ? C35 N1 1.450(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N24 1.430(5) . ? C36 N3 1.450(5) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C38 1.525(6) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 C39 1.539(6) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C39 C40 1.524(5) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 C42 1.522(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 C43 1.525(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 C44 1.516(6) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.521(6) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C46 C47 1.539(6) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C47 C48 1.517(5) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.523(5) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.534(6) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.511(7) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.526(6) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.521(7) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.525(6) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C58 1.522(6) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 C59 1.532(6) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 C60 1.520(6) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? O7 Ce2 2.432(3) 2_556 ? O8 Ce2 2.610(3) 2_556 ? 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 O20 N27 O19 120.4(6) . . ? O20 N27 O21 120.1(7) . . ? O19 N27 O21 119.5(6) . . ? O23 N28 O24 121.1(5) . . ? O23 N28 O22 118.7(4) . . ? O24 N28 O22 120.2(5) . . ? O25 N29 O27 115.2(8) . . ? O25 N29 O26 126.1(7) . . ? O27 N29 O26 118.6(8) . . ? O28 N30 O30 119.4(8) . . ? O28 N30 O29 111.4(7) . . ? O30 N30 O29 128.6(8) . . ? O15 N25 O14 121.6(4) . . ? O15 N25 O13 118.9(4) . . ? O14 N25 O13 119.5(4) . . ? O18 N26 O17 121.5(4) . . ? O18 N26 O16 121.6(4) . . ? O17 N26 O16 116.8(4) . . ? N25 O13 Ce1 133.8(3) . . ? N26 O16 Ce1 96.5(2) . . ? N26 O17 Ce1 98.2(3) . . ? O2W Ce1 O2 141.37(9) . . ? O2W Ce1 O13 73.02(10) . . ? O2 Ce1 O13 68.35(9) . . ? O2W Ce1 O5W 81.52(11) . . ? O2 Ce1 O5W 123.63(10) . . ? O13 Ce1 O5W 129.09(11) . . ? O2W Ce1 O3 83.93(10) . . ? O2 Ce1 O3 83.48(9) . . ? O13 Ce1 O3 70.50(10) . . ? O5W Ce1 O3 149.54(10) . . ? O2W Ce1 O3W 70.90(10) . . ? O2 Ce1 O3W 141.20(10) . . ? O13 Ce1 O3W 134.88(10) . . ? O5W Ce1 O3W 70.44(11) . . ? O3 Ce1 O3W 79.55(10) . . ? O2W Ce1 O17 131.75(10) . . ? O2 Ce1 O17 72.15(10) . . ? O13 Ce1 O17 121.34(10) . . ? O5W Ce1 O17 108.63(11) . . ? O3 Ce1 O17 63.43(10) . . ? O3W Ce1 O17 69.05(10) . . ? O2W Ce1 O1 89.67(9) . . ? O2 Ce1 O1 77.02(9) . . ? O13 Ce1 O1 69.51(10) . . ? O5W Ce1 O1 66.98(10) . . ? O3 Ce1 O1 139.63(8) . . ? O3W Ce1 O1 135.27(10) . . ? O17 Ce1 O1 138.24(9) . . ? O2W Ce1 O16 148.27(10) . . ? O2 Ce1 O16 69.84(9) . . ? O13 Ce1 O16 137.61(10) . . ? O5W Ce1 O16 71.49(11) . . ? O3 Ce1 O16 111.32(10) . . ? O3W Ce1 O16 84.29(10) . . ? O17 Ce1 O16 48.51(11) . . ? O1 Ce1 O16 94.68(10) . . ? O7 Ce2 O6W 143.85(10) 2_556 . ? O7 Ce2 O4W 99.63(10) 2_556 . ? O6W Ce2 O4W 105.70(12) . . ? O7 Ce2 O1W 86.66(11) 2_556 . ? O6W Ce2 O1W 78.87(12) . . ? O4W Ce2 O1W 69.25(11) . . ? O7 Ce2 O7W 84.32(13) 2_556 . ? O6W Ce2 O7W 91.99(15) . . ? O4W Ce2 O7W 140.36(12) . . ? O1W Ce2 O7W 150.16(12) . . ? O7 Ce2 O10 145.98(9) 2_556 . ? O6W Ce2 O10 67.57(10) . . ? O4W Ce2 O10 73.71(9) . . ? O1W Ce2 O10 119.77(10) . . ? O7W Ce2 O10 81.23(11) . . ? O7 Ce2 O8W 72.32(11) 2_556 . ? O6W Ce2 O8W 139.61(12) . . ? O4W Ce2 O8W 73.39(14) . . ? O1W Ce2 O8W 132.94(15) . . ? O7W Ce2 O8W 70.37(16) . . ? O10 Ce2 O8W 73.84(11) . . ? O7 Ce2 O8 77.13(9) 2_556 2_556 ? O6W Ce2 O8 67.07(10) . 2_556 ? O4W Ce2 O8 142.79(10) . 2_556 ? O1W Ce2 O8 73.55(10) . 2_556 ? O7W Ce2 O8 76.72(11) . 2_556 ? O10 Ce2 O8 128.22(9) . 2_556 ? O8W Ce2 O8 136.64(11) . 2_556 ? O1 C1 N1 126.0(3) . . ? O1 C1 N2 125.3(3) . . ? N1 C1 N2 108.5(3) . . ? N3 C2 N1 111.7(3) . . ? N3 C2 C37 113.7(3) . . ? N1 C2 C37 113.1(3) . . ? N3 C2 C3 103.1(3) . . ? N1 C2 C3 102.7(3) . . ? C37 C2 C3 111.5(3) . . ? N2 C3 N4 111.9(3) . . ? N2 C3 C40 112.8(3) . . ? N4 C3 C40 112.6(3) . . ? N2 C3 C2 103.3(3) . . ? N4 C3 C2 102.3(3) . . ? C40 C3 C2 113.0(3) . . ? O7 C4 N4 124.9(3) . . ? O7 C4 N3 125.1(3) . . ? N4 C4 N3 109.9(3) . . ? N5 C5 N2 116.2(3) . . ? N5 C5 H5A 108.2 . . ? N2 C5 H5A 108.2 . . ? N5 C5 H5B 108.2 . . ? N2 C5 H5B 108.2 . . ? H5A C5 H5B 107.4 . . ? N4 C6 N7 113.2(3) . . ? N4 C6 H6A 108.9 . . ? N7 C6 H6A 108.9 . . ? N4 C6 H6B 108.9 . . ? N7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 125.2(3) . . ? O2 C7 N5 124.0(3) . . ? N6 C7 N5 110.6(3) . . ? N7 C8 N5 112.6(3) . . ? N7 C8 C41 112.8(3) . . ? N5 C8 C41 112.8(3) . . ? N7 C8 C9 102.8(3) . . ? N5 C8 C9 102.1(3) . . ? C41 C8 C9 112.8(3) . . ? N8 C9 N6 112.6(3) . . ? N8 C9 C44 113.5(3) . . ? N6 C9 C44 112.1(3) . . ? N8 C9 C8 102.7(3) . . ? N6 C9 C8 102.8(3) . . ? C44 C9 C8 112.2(3) . . ? O8 C10 N7 125.2(3) . . ? O8 C10 N8 125.4(3) . . ? N7 C10 N8 109.4(3) . . ? N9 C11 N6 114.7(3) . . ? N9 C11 H11A 108.6 . . ? N6 C11 H11A 108.6 . . ? N9 C11 H11B 108.6 . . ? N6 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? N11 C12 N8 114.4(3) . . ? N11 C12 H12A 108.7 . . ? N8 C12 H12A 108.7 . . ? N11 C12 H12B 108.7 . . ? N8 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N10 125.1(3) . . ? O3 C13 N9 125.3(3) . . ? N10 C13 N9 109.6(3) . . ? N9 C14 N11 111.8(3) . . ? N9 C14 C45 114.2(3) . . ? N11 C14 C45 112.5(3) . . ? N9 C14 C15 102.9(3) . . ? N11 C14 C15 102.6(3) . . ? C45 C14 C15 111.9(3) . . ? N12 C15 N10 111.9(3) . . ? N12 C15 C48 113.2(3) . . ? N10 C15 C48 113.6(3) . . ? N12 C15 C14 102.7(3) . . ? N10 C15 C14 102.3(3) . . ? C48 C15 C14 112.1(3) . . ? O9 C16 N11 124.8(3) . . ? O9 C16 N12 125.3(3) . . ? N11 C16 N12 109.9(3) . . ? N13 C17 N10 115.1(3) . . ? N13 C17 H17A 108.5 . . ? N10 C17 H17A 108.5 . . ? N13 C17 H17B 108.5 . . ? N10 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? N12 C18 N15 114.1(3) . . ? N12 C18 H18A 108.7 . . ? N15 C18 H18A 108.7 . . ? N12 C18 H18B 108.7 . . ? N15 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? O4 C19 N14 125.6(4) . . ? O4 C19 N13 125.4(4) . . ? N14 C19 N13 109.0(3) . . ? N13 C20 N15 112.7(3) . . ? N13 C20 C49 115.0(3) . . ? N15 C20 C49 111.3(3) . . ? N13 C20 C21 102.5(3) . . ? N15 C20 C21 102.8(3) . . ? C49 C20 C21 111.6(3) . . ? N14 C21 N16 113.3(3) . . ? N14 C21 C52 113.0(3) . . ? N16 C21 C52 112.3(3) . . ? N14 C21 C20 102.8(3) . . ? N16 C21 C20 102.2(3) . . ? C52 C21 C20 112.3(3) . . ? O10 C22 N15 125.8(3) . . ? O10 C22 N16 124.9(3) . . ? N15 C22 N16 109.3(3) . . ? N17 C23 N14 113.3(3) . . ? N17 C23 H23A 108.9 . . ? N14 C23 H23A 108.9 . . ? N17 C23 H23B 108.9 . . ? N14 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? N16 C24 N19 114.1(3) . . ? N16 C24 H24A 108.7 . . ? N19 C24 H24A 108.7 . . ? N16 C24 H24B 108.7 . . ? N19 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? O5 C25 N17 125.9(4) . . ? O5 C25 N18 125.2(4) . . ? N17 C25 N18 108.9(3) . . ? N19 C26 N17 112.5(3) . . ? N19 C26 C53 113.9(3) . . ? N17 C26 C53 111.6(3) . . ? N19 C26 C27 103.1(3) . . ? N17 C26 C27 102.5(3) . . ? C53 C26 C27 112.5(3) . . ? N18 C27 N20 112.5(3) . . ? N18 C27 C56 112.4(3) . . ? N20 C27 C56 113.5(3) . . ? N18 C27 C26 102.8(3) . . ? N20 C27 C26 102.5(3) . . ? C56 C27 C26 112.2(3) . . ? O11 C28 N20 124.9(4) . . ? O11 C28 N19 125.8(4) . . ? N20 C28 N19 109.3(3) . . ? N18 C29 N21 115.3(3) . . ? N18 C29 H29A 108.5 . . ? N21 C29 H29A 108.5 . . ? N18 C29 H29B 108.5 . . ? N21 C29 H29B 108.5 . . ? H29A C29 H29B 107.5 . . ? N23 C30 N20 114.1(3) . . ? N23 C30 H30A 108.7 . . ? N20 C30 H30A 108.7 . . ? N23 C30 H30B 108.7 . . ? N20 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? O6 C31 N21 125.1(4) . . ? O6 C31 N22 125.5(4) . . ? N21 C31 N22 109.5(3) . . ? N21 C32 N23 112.6(3) . . ? N21 C32 C57 113.2(3) . . ? N23 C32 C57 112.5(3) . . ? N21 C32 C33 102.9(3) . . ? N23 C32 C33 102.1(3) . . ? C57 C32 C33 112.5(3) . . ? N24 C33 N22 112.8(3) . . ? N24 C33 C60 113.9(3) . . ? N22 C33 C60 113.4(3) . . ? N24 C33 C32 102.6(3) . . ? N22 C33 C32 102.0(3) . . ? C60 C33 C32 110.9(3) . . ? O12 C34 N24 124.7(4) . . ? O12 C34 N23 126.0(4) . . ? N24 C34 N23 109.2(3) . . ? N22 C35 N1 115.7(3) . . ? N22 C35 H35A 108.4 . . ? N1 C35 H35A 108.4 . . ? N22 C35 H35B 108.4 . . ? N1 C35 H35B 108.4 . . ? H35A C35 H35B 107.4 . . ? N24 C36 N3 115.1(3) . . ? N24 C36 H36A 108.5 . . ? N3 C36 H36A 108.5 . . ? N24 C36 H36B 108.5 . . ? N3 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? C38 C37 C2 111.0(3) . . ? C38 C37 H37A 109.4 . . ? C2 C37 H37A 109.4 . . ? C38 C37 H37B 109.4 . . ? C2 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? C37 C38 C39 112.6(3) . . ? C37 C38 H38A 109.1 . . ? C39 C38 H38A 109.1 . . ? C37 C38 H38B 109.1 . . ? C39 C38 H38B 109.1 . . ? H38A C38 H38B 107.8 . . ? C40 C39 C38 112.7(3) . . ? C40 C39 H39A 109.0 . . ? C38 C39 H39A 109.0 . . ? C40 C39 H39B 109.0 . . ? C38 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C3 C40 C39 111.2(3) . . ? C3 C40 H40A 109.4 . . ? C39 C40 H40A 109.4 . . ? C3 C40 H40B 109.4 . . ? C39 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C42 C41 C8 111.5(3) . . ? C42 C41 H41A 109.3 . . ? C8 C41 H41A 109.3 . . ? C42 C41 H41B 109.3 . . ? C8 C41 H41B 109.3 . . ? H41A C41 H41B 108.0 . . ? C41 C42 C43 113.5(3) . . ? C41 C42 H42A 108.9 . . ? C43 C42 H42A 108.9 . . ? C41 C42 H42B 108.9 . . ? C43 C42 H42B 108.9 . . ? H42A C42 H42B 107.7 . . ? C44 C43 C42 113.9(3) . . ? C44 C43 H43A 108.8 . . ? C42 C43 H43A 108.8 . . ? C44 C43 H43B 108.8 . . ? C42 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? C43 C44 C9 111.0(3) . . ? C43 C44 H44A 109.4 . . ? C9 C44 H44A 109.4 . . ? C43 C44 H44B 109.4 . . ? C9 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? C14 C45 C46 110.7(3) . . ? C14 C45 H45A 109.5 . . ? C46 C45 H45A 109.5 . . ? C14 C45 H45B 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? C45 C46 C47 113.2(3) . . ? C45 C46 H46A 108.9 . . ? C47 C46 H46A 108.9 . . ? C45 C46 H46B 108.9 . . ? C47 C46 H46B 108.9 . . ? H46A C46 H46B 107.7 . . ? C48 C47 C46 112.2(3) . . ? C48 C47 H47A 109.2 . . ? C46 C47 H47A 109.2 . . ? C48 C47 H47B 109.2 . . ? C46 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? C47 C48 C15 111.3(3) . . ? C47 C48 H48A 109.4 . . ? C15 C48 H48A 109.4 . . ? C47 C48 H48B 109.4 . . ? C15 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? C50 C49 C20 110.2(3) . . ? C50 C49 H49A 109.6 . . ? C20 C49 H49A 109.6 . . ? C50 C49 H49B 109.6 . . ? C20 C49 H49B 109.6 . . ? H49A C49 H49B 108.1 . . ? C49 C50 C51 112.3(3) . . ? C49 C50 H50A 109.1 . . ? C51 C50 H50A 109.1 . . ? C49 C50 H50B 109.1 . . ? C51 C50 H50B 109.1 . . ? H50A C50 H50B 107.9 . . ? C52 C51 C50 113.6(4) . . ? C52 C51 H51A 108.9 . . ? C50 C51 H51A 108.9 . . ? C52 C51 H51B 108.9 . . ? C50 C51 H51B 108.9 . . ? H51A C51 H51B 107.7 . . ? C51 C52 C21 111.2(3) . . ? C51 C52 H52A 109.4 . . ? C21 C52 H52A 109.4 . . ? C51 C52 H52B 109.4 . . ? C21 C52 H52B 109.4 . . ? H52A C52 H52B 108.0 . . ? C54 C53 C26 110.1(4) . . ? C54 C53 H53A 109.6 . . ? C26 C53 H53A 109.6 . . ? C54 C53 H53B 109.6 . . ? C26 C53 H53B 109.6 . . ? H53A C53 H53B 108.2 . . ? C55 C54 C53 113.4(4) . . ? C55 C54 H54A 108.9 . . ? C53 C54 H54A 108.9 . . ? C55 C54 H54B 108.9 . . ? C53 C54 H54B 108.9 . . ? H54A C54 H54B 107.7 . . ? C54 C55 C56 113.4(4) . . ? C54 C55 H55A 108.9 . . ? C56 C55 H55A 108.9 . . ? C54 C55 H55B 108.9 . . ? C56 C55 H55B 108.9 . . ? H55A C55 H55B 107.7 . . ? C55 C56 C27 111.5(4) . . ? C55 C56 H56A 109.3 . . ? C27 C56 H56A 109.3 . . ? C55 C56 H56B 109.3 . . ? C27 C56 H56B 109.3 . . ? H56A C56 H56B 108.0 . . ? C58 C57 C32 109.9(3) . . ? C58 C57 H57A 109.7 . . ? C32 C57 H57A 109.7 . . ? C58 C57 H57B 109.7 . . ? C32 C57 H57B 109.7 . . ? H57A C57 H57B 108.2 . . ? C57 C58 C59 111.6(3) . . ? C57 C58 H58A 109.3 . . ? C59 C58 H58A 109.3 . . ? C57 C58 H58B 109.3 . . ? C59 C58 H58B 109.3 . . ? H58A C58 H58B 108.0 . . ? C60 C59 C58 113.2(3) . . ? C60 C59 H59A 108.9 . . ? C58 C59 H59A 108.9 . . ? C60 C59 H59B 108.9 . . ? C58 C59 H59B 108.9 . . ? H59A C59 H59B 107.7 . . ? C33 C60 C59 112.1(3) . . ? C33 C60 H60A 109.2 . . ? C59 C60 H60A 109.2 . . ? C33 C60 H60B 109.2 . . ? C59 C60 H60B 109.2 . . ? H60A C60 H60B 107.9 . . ? C1 N1 C35 123.1(3) . . ? C1 N1 C2 112.6(3) . . ? C35 N1 C2 123.8(3) . . ? C1 N2 C5 123.0(3) . . ? C1 N2 C3 112.5(3) . . ? C5 N2 C3 124.1(3) . . ? C4 N3 C36 121.9(3) . . ? C4 N3 C2 111.7(3) . . ? C36 N3 C2 125.3(3) . . ? C4 N4 C6 122.7(3) . . ? C4 N4 C3 112.7(3) . . ? C6 N4 C3 124.3(3) . . ? C7 N5 C5 120.5(3) . . ? C7 N5 C8 112.3(3) . . ? C5 N5 C8 127.0(3) . . ? C7 N6 C11 121.5(3) . . ? C7 N6 C9 112.1(3) . . ? C11 N6 C9 126.4(3) . . ? C10 N7 C6 121.3(3) . . ? C10 N7 C8 113.0(3) . . ? C6 N7 C8 124.6(3) . . ? C10 N8 C12 122.0(3) . . ? C10 N8 C9 112.1(3) . . ? C12 N8 C9 124.2(3) . . ? C13 N9 C11 123.0(3) . . ? C13 N9 C14 112.1(3) . . ? C11 N9 C14 124.2(3) . . ? C13 N10 C17 122.4(3) . . ? C13 N10 C15 112.6(3) . . ? C17 N10 C15 124.3(3) . . ? C16 N11 C12 122.2(3) . . ? C16 N11 C14 112.2(3) . . ? C12 N11 C14 124.9(3) . . ? C16 N12 C18 122.4(3) . . ? C16 N12 C15 112.2(3) . . ? C18 N12 C15 124.4(3) . . ? C19 N13 C17 120.0(3) . . ? C19 N13 C20 112.0(3) . . ? C17 N13 C20 124.7(3) . . ? C19 N14 C21 113.1(3) . . ? C19 N14 C23 121.6(3) . . ? C21 N14 C23 124.6(3) . . ? C22 N15 C18 122.6(3) . . ? C22 N15 C20 112.9(3) . . ? C18 N15 C20 124.4(3) . . ? C22 N16 C24 122.4(3) . . ? C22 N16 C21 112.2(3) . . ? C24 N16 C21 124.9(3) . . ? C25 N17 C23 121.6(3) . . ? C25 N17 C26 113.0(3) . . ? C23 N17 C26 125.5(3) . . ? C25 N18 C29 121.1(3) . . ? C25 N18 C27 112.7(3) . . ? C29 N18 C27 126.1(3) . . ? C28 N19 C24 121.7(3) . . ? C28 N19 C26 112.6(3) . . ? C24 N19 C26 124.7(3) . . ? C28 N20 C30 121.2(3) . . ? C28 N20 C27 112.6(3) . . ? C30 N20 C27 124.6(3) . . ? C31 N21 C29 122.5(3) . . ? C31 N21 C32 112.7(3) . . ? C29 N21 C32 124.5(3) . . ? C31 N22 C35 119.5(3) . . ? C31 N22 C33 111.8(3) . . ? C35 N22 C33 124.5(3) . . ? C34 N23 C30 121.6(3) . . ? C34 N23 C32 112.1(3) . . ? C30 N23 C32 124.9(3) . . ? C34 N24 C36 121.8(3) . . ? C34 N24 C33 112.7(3) . . ? C36 N24 C33 125.3(3) . . ? C1 O1 Ce1 141.6(2) . . ? C7 O2 Ce1 126.3(2) . . ? C13 O3 Ce1 145.9(3) . . ? C4 O7 Ce2 155.4(3) . 2_556 ? C10 O8 Ce2 158.2(3) . 2_556 ? C22 O10 Ce2 145.0(2) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 3.183 _refine_diff_density_min -1.102 _refine_diff_density_rms 0.117 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.004 0.496 1.000 237 81 ' ' 2 0.495 0.995 0.500 215 67 ' ' 3 0.500 0.500 0.500 33 7 ' ' _platon_squeeze_details ; ; data_p9 _database_code_depnum_ccdc_archive 'CCDC 881909' #TrackingRef '110708qx-submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C120 H212 La4 N60 O94' _chemical_formula_weight 4555.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.5568(18) _cell_length_b 15.6496(19) _cell_length_c 21.030(2) _cell_angle_alpha 104.420(4) _cell_angle_beta 95.910(4) _cell_angle_gamma 119.074(4) _cell_volume 4179.4(8) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.810 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2332 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7969 _exptl_absorpt_correction_T_max 0.8667 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44452 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15836 _reflns_number_gt 13639 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+55.9995P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15836 _refine_ls_number_parameters 1171 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.1907 _refine_ls_wR_factor_gt 0.1871 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N27 N -0.6065(7) -0.0076(7) 0.1321(5) 0.051(2) Uani 1 1 d . . . N28 N -0.0637(13) 0.8529(11) 0.0816(6) 0.084(4) Uani 1 1 d . . . N29 N 0.6150(6) 0.4353(5) 0.4010(3) 0.0427(19) Uani 1 1 d D . . N30 N 0.5818(5) 0.6846(7) 0.1400(5) 0.095(5) Uani 1 1 d D . . O19 O -0.5334(7) -0.0045(8) 0.1636(5) 0.079(3) Uani 1 1 d . . . O20 O -0.6429(10) 0.0362(10) 0.1588(6) 0.106(4) Uani 1 1 d . . . O21 O -0.6439(12) -0.0588(11) 0.0708(6) 0.128(5) Uani 1 1 d . . . O22 O -0.1258(8) 0.8087(8) 0.1100(5) 0.076(3) Uani 1 1 d . . . O23 O 0.0232(8) 0.9379(9) 0.1066(7) 0.121(5) Uani 1 1 d . . . O24 O -0.0892(17) 0.8161(14) 0.0166(6) 0.198(9) Uani 1 1 d . . . O25 O 0.6200(7) 0.4151(6) 0.4546(3) 0.067(2) Uani 1 1 d D . . O26 O 0.6217(7) 0.3803(7) 0.3497(3) 0.078(3) Uani 1 1 d D . . O27 O 0.6005(9) 0.5068(6) 0.3999(6) 0.113(5) Uani 1 1 d D . . O28 O 0.5988(7) 0.7502(7) 0.1953(5) 0.081(3) Uani 1 1 d D . . O29 O 0.5662(13) 0.7094(11) 0.0899(6) 0.222(12) Uani 1 1 d D . . O30 O 0.5821(9) 0.6054(10) 0.1411(10) 0.154(7) Uani 1 1 d D . . N25 N 0.1513(5) 0.6340(6) 0.2877(3) 0.0305(15) Uani 1 1 d . . . N26 N 0.1988(6) 0.8725(5) 0.5920(4) 0.0323(16) Uani 1 1 d . . . O1W O 0.0978(5) 0.5282(5) 0.1228(3) 0.0423(15) Uani 1 1 d . . . O2W O 0.0604(4) 0.5226(4) 0.3852(3) 0.0315(12) Uani 1 1 d . . . O3W O 0.1352(5) 0.4215(5) 0.0101(3) 0.0368(14) Uani 1 1 d . . . O4W O 0.0220(5) 0.6079(5) 0.5117(3) 0.0404(15) Uani 1 1 d . . . O5W O 0.2198(5) 0.6228(5) 0.5366(3) 0.0399(15) Uani 1 1 d . . . O6W O 0.1178(5) 0.6730(6) 0.0352(3) 0.0510(19) Uani 1 1 d . . . O7W O 0.3879(6) 0.7758(6) 0.0623(4) 0.062(2) Uani 1 1 d . . . O8W O 0.3521(6) 0.5649(7) 0.0176(3) 0.065(2) Uani 1 1 d . . . O13 O 0.1874(5) 0.7065(4) 0.3461(3) 0.0333(13) Uani 1 1 d . . . O14 O 0.0772(6) 0.6158(6) 0.2473(4) 0.060(2) Uani 1 1 d . . . O15 O 0.1970(7) 0.5908(8) 0.2731(4) 0.077(3) Uani 1 1 d . . . O16 O 0.2612(4) 0.8423(5) 0.5884(3) 0.0367(14) Uani 1 1 d . . . O17 O 0.1282(4) 0.8331(5) 0.5392(3) 0.0358(13) Uani 1 1 d . . . O18 O 0.2078(6) 0.9369(5) 0.6440(4) 0.0530(19) Uani 1 1 d . . . La1 La 0.17061(3) 0.70718(3) 0.46295(2) 0.02140(12) Uani 1 1 d . . . La2 La 0.23286(3) 0.61458(4) 0.06596(2) 0.02595(13) Uani 1 1 d . . . C1 C 0.3842(5) 0.7081(5) 0.4024(3) 0.0187(14) Uani 1 1 d . . . C2 C 0.4676(5) 0.6634(5) 0.3262(4) 0.0184(14) Uani 1 1 d . . . C3 C 0.4920(5) 0.7764(6) 0.3346(4) 0.0198(14) Uani 1 1 d . . . C4 C 0.3994(5) 0.6663(5) 0.2223(4) 0.0187(14) Uani 1 1 d . . . C5 C 0.4575(5) 0.8961(5) 0.4203(4) 0.0207(15) Uani 1 1 d . . . H5A H 0.5280 0.9488 0.4240 0.025 Uiso 1 1 calc R . . H5B H 0.4510 0.9004 0.4667 0.025 Uiso 1 1 calc R . . C6 C 0.4475(5) 0.8472(5) 0.2470(4) 0.0188(14) Uani 1 1 d . . . H6A H 0.4356 0.8272 0.1974 0.023 Uiso 1 1 calc R . . H6B H 0.5163 0.9093 0.2675 0.023 Uiso 1 1 calc R . . C7 C 0.3076(5) 0.9097(5) 0.4104(3) 0.0173(14) Uani 1 1 d . . . C8 C 0.3952(5) 0.9552(5) 0.3292(3) 0.0156(13) Uani 1 1 d . . . C9 C 0.2981(5) 0.9622(5) 0.3166(3) 0.0151(13) Uani 1 1 d . . . C10 C 0.2832(5) 0.8333(5) 0.2225(3) 0.0157(13) Uani 1 1 d . . . C11 C 0.1615(5) 0.9272(5) 0.3850(3) 0.0176(13) Uani 1 1 d . . . H11A H 0.1605 0.9264 0.4313 0.021 Uiso 1 1 calc R . . H11B H 0.1641 0.9903 0.3830 0.021 Uiso 1 1 calc R . . C12 C 0.1497(5) 0.8736(6) 0.2080(3) 0.0172(14) Uani 1 1 d . . . H12A H 0.1609 0.9434 0.2174 0.021 Uiso 1 1 calc R . . H12B H 0.1474 0.8473 0.1600 0.021 Uiso 1 1 calc R . . C13 C 0.0090(5) 0.7501(5) 0.3550(3) 0.0181(14) Uani 1 1 d . . . C14 C 0.0157(5) 0.8355(5) 0.2762(3) 0.0163(13) Uani 1 1 d . . . C15 C -0.0949(5) 0.7362(5) 0.2577(3) 0.0148(13) Uani 1 1 d . . . C16 C -0.0200(5) 0.7154(5) 0.1695(3) 0.0170(14) Uani 1 1 d . . . C17 C -0.1701(5) 0.6046(5) 0.3208(4) 0.0205(14) Uani 1 1 d . . . H17A H -0.1503 0.6071 0.3673 0.025 Uiso 1 1 calc R . . H17B H -0.2284 0.6135 0.3174 0.025 Uiso 1 1 calc R . . C18 C -0.2016(5) 0.5829(5) 0.1452(3) 0.0184(14) Uani 1 1 d . . . H18A H -0.2562 0.5958 0.1520 0.022 Uiso 1 1 calc R . . H18B H -0.1982 0.5762 0.0980 0.022 Uiso 1 1 calc R . . C19 C -0.1933(5) 0.4338(6) 0.2995(4) 0.0240(16) Uani 1 1 d . . . C20 C -0.2758(5) 0.4516(6) 0.2077(4) 0.0209(15) Uani 1 1 d . . . C21 C -0.3002(5) 0.3367(6) 0.1883(4) 0.0218(15) Uani 1 1 d . . . C22 C -0.2191(5) 0.4121(6) 0.1116(4) 0.0210(15) Uani 1 1 d . . . C23 C -0.2634(6) 0.2449(6) 0.2638(4) 0.0261(16) Uani 1 1 d . . . H23A H -0.2573 0.2574 0.3125 0.031 Uiso 1 1 calc R . . H23B H -0.3328 0.1864 0.2391 0.031 Uiso 1 1 calc R . . C24 C -0.2539(6) 0.2350(6) 0.0956(4) 0.0253(16) Uani 1 1 d . . . H24A H -0.3220 0.1736 0.0866 0.030 Uiso 1 1 calc R . . H24B H -0.2405 0.2391 0.0516 0.030 Uiso 1 1 calc R . . C25 C -0.1098(6) 0.2411(5) 0.2920(4) 0.0227(15) Uani 1 1 d . . . C26 C -0.2003(6) 0.1589(5) 0.1756(4) 0.0212(15) Uani 1 1 d . . . C27 C -0.1028(5) 0.1500(6) 0.1872(4) 0.0213(15) Uani 1 1 d . . . C28 C -0.0889(6) 0.2499(6) 0.1178(3) 0.0211(15) Uani 1 1 d . . . C29 C 0.0309(5) 0.2110(6) 0.2986(4) 0.0214(15) Uani 1 1 d . . . H29A H 0.0303 0.2251 0.3466 0.026 Uiso 1 1 calc R . . H29B H 0.0267 0.1443 0.2822 0.026 Uiso 1 1 calc R . . C30 C 0.0448(5) 0.2109(6) 0.1293(4) 0.0219(15) Uani 1 1 d . . . H30A H 0.0346 0.1417 0.1205 0.026 Uiso 1 1 calc R . . H30B H 0.0490 0.2259 0.0867 0.026 Uiso 1 1 calc R . . C31 C 0.1845(6) 0.3869(6) 0.3433(4) 0.0224(15) Uani 1 1 d . . . C32 C 0.1774(5) 0.2761(5) 0.2425(3) 0.0191(14) Uani 1 1 d . . . C33 C 0.2890(5) 0.3773(5) 0.2726(3) 0.0184(14) Uani 1 1 d . . . C34 C 0.2159(6) 0.3673(6) 0.1653(4) 0.0247(16) Uani 1 1 d . . . C35 C 0.3604(5) 0.5342(5) 0.3837(4) 0.0231(15) Uani 1 1 d . . . H35A H 0.4171 0.5235 0.3917 0.028 Uiso 1 1 calc R . . H35B H 0.3385 0.5414 0.4258 0.028 Uiso 1 1 calc R . . C36 C 0.3957(5) 0.5053(5) 0.2163(4) 0.0212(15) Uani 1 1 d . . . H36A H 0.3941 0.5010 0.1688 0.025 Uiso 1 1 calc R . . H36B H 0.4532 0.5006 0.2345 0.025 Uiso 1 1 calc R . . C37 C 0.5631(6) 0.6628(6) 0.3476(4) 0.0252(16) Uani 1 1 d . . . H37A H 0.6023 0.6762 0.3138 0.030 Uiso 1 1 calc R . . H37B H 0.5441 0.5939 0.3491 0.030 Uiso 1 1 calc R . . C38 C 0.6292(6) 0.7447(6) 0.4171(4) 0.0333(19) Uani 1 1 d . . . H38A H 0.6916 0.7440 0.4282 0.040 Uiso 1 1 calc R . . H38B H 0.5924 0.7267 0.4514 0.040 Uiso 1 1 calc R . . C39 C 0.6587(6) 0.8556(6) 0.4204(4) 0.0289(17) Uani 1 1 d . . . H39A H 0.6411 0.8864 0.4595 0.035 Uiso 1 1 calc R . . H39B H 0.7327 0.8986 0.4278 0.035 Uiso 1 1 calc R . . C40 C 0.6058(5) 0.8574(6) 0.3563(4) 0.0240(15) Uani 1 1 d . . . H40A H 0.6163 0.9267 0.3645 0.029 Uiso 1 1 calc R . . H40B H 0.6361 0.8438 0.3194 0.029 Uiso 1 1 calc R . . C41 C 0.4934(5) 1.0582(5) 0.3407(4) 0.0261(16) Uani 1 1 d . . . H41A H 0.4956 1.0733 0.2982 0.031 Uiso 1 1 calc R . . H41B H 0.5522 1.0526 0.3541 0.031 Uiso 1 1 calc R . . C42 C 0.4998(7) 1.1478(6) 0.3967(5) 0.040(2) Uani 1 1 d . . . H42A H 0.5089 1.1379 0.4406 0.048 Uiso 1 1 calc R . . H42B H 0.5598 1.2138 0.3998 0.048 Uiso 1 1 calc R . . C43 C 0.4070(6) 1.1542(6) 0.3839(4) 0.0317(18) Uani 1 1 d . . . H43A H 0.4279 1.2228 0.3809 0.038 Uiso 1 1 calc R . . H43B H 0.3782 1.1490 0.4230 0.038 Uiso 1 1 calc R . . C44 C 0.3245(6) 1.0718(5) 0.3201(4) 0.0211(15) Uani 1 1 d . . . H44A H 0.3475 1.0855 0.2801 0.025 Uiso 1 1 calc R . . H44B H 0.2632 1.0753 0.3194 0.025 Uiso 1 1 calc R . . C45 C 0.0131(6) 0.9342(6) 0.2832(4) 0.0210(15) Uani 1 1 d . . . H45A H 0.0830 0.9947 0.2968 0.025 Uiso 1 1 calc R . . H45B H -0.0216 0.9280 0.2391 0.025 Uiso 1 1 calc R . . C46 C -0.0422(6) 0.9502(6) 0.3358(4) 0.0283(17) Uani 1 1 d . . . H46A H -0.0518 1.0071 0.3343 0.034 Uiso 1 1 calc R . . H46B H 0.0005 0.9712 0.3811 0.034 Uiso 1 1 calc R . . C47 C -0.1469(6) 0.8524(6) 0.3250(4) 0.0274(16) Uani 1 1 d . . . H47A H -0.1451 0.8286 0.3637 0.033 Uiso 1 1 calc R . . H47B H -0.1989 0.8706 0.3237 0.033 Uiso 1 1 calc R . . C48 C -0.1766(6) 0.7644(6) 0.2599(4) 0.0223(15) Uani 1 1 d . . . H48A H -0.1858 0.7851 0.2207 0.027 Uiso 1 1 calc R . . H48B H -0.2417 0.7030 0.2567 0.027 Uiso 1 1 calc R . . C49 C -0.3720(5) 0.4552(6) 0.2065(4) 0.0232(15) Uani 1 1 d . . . H49A H -0.3544 0.5272 0.2167 0.028 Uiso 1 1 calc R . . H49B H -0.4028 0.4299 0.2414 0.028 Uiso 1 1 calc R . . C50 C -0.4487(6) 0.3872(7) 0.1360(4) 0.0297(17) Uani 1 1 d . . . H50A H -0.4216 0.4188 0.1022 0.036 Uiso 1 1 calc R . . H50B H -0.5127 0.3847 0.1373 0.036 Uiso 1 1 calc R . . C51 C -0.4703(6) 0.2754(7) 0.1143(5) 0.039(2) Uani 1 1 d . . . H51A H -0.5438 0.2263 0.1047 0.047 Uiso 1 1 calc R . . H51B H -0.4503 0.2613 0.0721 0.047 Uiso 1 1 calc R . . C52 C -0.4153(6) 0.2564(6) 0.1669(5) 0.0309(18) Uani 1 1 d . . . H52A H -0.4276 0.1864 0.1482 0.037 Uiso 1 1 calc R . . H52B H -0.4423 0.2602 0.2069 0.037 Uiso 1 1 calc R . . C53 C -0.2989(6) 0.0528(6) 0.1457(5) 0.0309(18) Uani 1 1 d . . . H53A H -0.3573 0.0613 0.1452 0.037 Uiso 1 1 calc R . . H53B H -0.3028 0.0187 0.0986 0.037 Uiso 1 1 calc R . . C54 C -0.3033(7) -0.0148(7) 0.1877(6) 0.042(2) Uani 1 1 d . . . H54A H -0.3667 -0.0832 0.1674 0.051 Uiso 1 1 calc R . . H54B H -0.3045 0.0173 0.2338 0.051 Uiso 1 1 calc R . . C55 C -0.2117(7) -0.0295(7) 0.1923(5) 0.041(2) Uani 1 1 d . . . H55A H -0.1801 -0.0117 0.2402 0.050 Uiso 1 1 calc R . . H55B H -0.2366 -0.1030 0.1688 0.050 Uiso 1 1 calc R . . C56 C -0.1321(6) 0.0365(6) 0.1614(4) 0.0276(16) Uani 1 1 d . . . H56A H -0.1585 0.0082 0.1117 0.033 Uiso 1 1 calc R . . H56B H -0.0712 0.0334 0.1726 0.033 Uiso 1 1 calc R . . C57 C 0.1777(6) 0.1757(6) 0.2292(4) 0.0248(16) Uani 1 1 d . . . H57A H 0.1925 0.1664 0.2725 0.030 Uiso 1 1 calc R . . H57B H 0.1103 0.1160 0.2017 0.030 Uiso 1 1 calc R . . C58 C 0.2579(6) 0.1807(6) 0.1919(4) 0.0301(17) Uani 1 1 d . . . H58A H 0.2428 0.1905 0.1488 0.036 Uiso 1 1 calc R . . H58B H 0.2548 0.1145 0.1813 0.036 Uiso 1 1 calc R . . C59 C 0.3654(6) 0.2693(6) 0.2340(4) 0.0300(17) Uani 1 1 d . . . H59A H 0.4025 0.3042 0.2043 0.036 Uiso 1 1 calc R . . H59B H 0.4015 0.2401 0.2520 0.036 Uiso 1 1 calc R . . C60 C 0.3663(6) 0.3505(6) 0.2937(4) 0.0238(16) Uani 1 1 d . . . H60A H 0.3510 0.3230 0.3309 0.029 Uiso 1 1 calc R . . H60B H 0.4345 0.4139 0.3107 0.029 Uiso 1 1 calc R . . N1 N 0.3981(5) 0.6316(4) 0.3701(3) 0.0203(12) Uani 1 1 d . . . N2 N 0.4399(4) 0.7941(4) 0.3854(3) 0.0175(12) Uani 1 1 d . . . N3 N 0.4140(5) 0.6062(5) 0.2545(3) 0.0214(13) Uani 1 1 d . . . N4 N 0.4424(4) 0.7634(4) 0.2675(3) 0.0177(12) Uani 1 1 d . . . N5 N 0.3898(4) 0.9221(4) 0.3885(3) 0.0158(11) Uani 1 1 d . . . N6 N 0.2536(4) 0.9335(5) 0.3720(3) 0.0188(12) Uani 1 1 d . . . N7 N 0.3739(4) 0.8728(4) 0.2667(3) 0.0154(11) Uani 1 1 d . . . N8 N 0.2359(4) 0.8823(4) 0.2499(3) 0.0157(11) Uani 1 1 d . . . N9 N 0.0673(4) 0.8378(4) 0.3386(3) 0.0177(12) Uani 1 1 d . . . N10 N -0.0859(4) 0.6919(5) 0.3101(3) 0.0191(12) Uani 1 1 d . . . N11 N 0.0529(4) 0.8073(5) 0.2180(3) 0.0185(12) Uani 1 1 d . . . N12 N -0.1062(4) 0.6720(4) 0.1901(3) 0.0161(11) Uani 1 1 d . . . N13 N -0.2029(5) 0.5031(4) 0.2746(3) 0.0191(12) Uani 1 1 d . . . N14 N -0.2485(5) 0.3369(5) 0.2500(3) 0.0231(13) Uani 1 1 d . . . N15 N -0.2279(4) 0.4857(4) 0.1544(3) 0.0174(12) Uani 1 1 d . . . N16 N -0.2530(5) 0.3280(5) 0.1326(3) 0.0214(13) Uani 1 1 d . . . N17 N -0.1924(5) 0.2164(5) 0.2449(3) 0.0240(13) Uani 1 1 d . . . N18 N -0.0586(4) 0.2006(5) 0.2607(3) 0.0217(13) Uani 1 1 d . . . N19 N -0.1792(5) 0.2218(5) 0.1320(3) 0.0214(12) Uani 1 1 d . . . N20 N -0.0443(4) 0.2087(5) 0.1484(3) 0.0153(11) Uani 1 1 d . . . N21 N 0.1269(5) 0.2916(5) 0.2943(3) 0.0217(13) Uani 1 1 d . . . N22 N 0.2768(4) 0.4423(4) 0.3305(3) 0.0191(12) Uani 1 1 d . . . N23 N 0.1412(5) 0.2872(5) 0.1803(3) 0.0214(13) Uani 1 1 d . . . N24 N 0.3031(5) 0.4175(5) 0.2173(3) 0.0216(13) Uani 1 1 d . . . O1 O 0.3318(4) 0.7029(4) 0.4439(2) 0.0224(11) Uani 1 1 d . . . O2 O 0.2886(4) 0.8859(4) 0.4620(2) 0.0202(10) Uani 1 1 d . . . O3 O 0.0355(4) 0.7299(4) 0.4038(3) 0.0262(12) Uani 1 1 d . . . O4 O -0.1443(4) 0.4546(4) 0.3557(3) 0.0266(11) Uani 1 1 d . . . O5 O -0.0860(4) 0.2898(4) 0.3525(3) 0.0292(12) Uani 1 1 d . . . O6 O 0.1587(4) 0.4190(4) 0.3928(3) 0.0284(12) Uani 1 1 d . . . O7 O 0.3552(4) 0.6365(4) 0.1623(3) 0.0239(11) Uani 1 1 d . . . O8 O 0.2489(4) 0.7646(4) 0.1661(2) 0.0229(11) Uani 1 1 d . . . O9 O -0.0098(4) 0.6788(4) 0.1139(2) 0.0234(11) Uani 1 1 d . . . O10 O -0.1861(4) 0.4189(4) 0.0605(3) 0.0241(11) Uani 1 1 d . . . O11 O -0.0529(4) 0.3040(4) 0.0810(3) 0.0298(12) Uani 1 1 d . . . O12 O 0.2079(5) 0.3894(5) 0.1149(3) 0.0403(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N27 0.058(5) 0.052(5) 0.061(6) 0.035(5) 0.030(5) 0.032(5) N28 0.149(13) 0.094(9) 0.051(7) 0.023(7) 0.045(8) 0.092(10) N29 0.036(4) 0.048(5) 0.043(5) 0.023(4) -0.002(4) 0.020(4) N30 0.051(6) 0.073(8) 0.073(8) -0.012(7) 0.044(6) -0.017(6) O19 0.073(6) 0.089(7) 0.109(8) 0.068(6) 0.041(6) 0.048(5) O20 0.134(10) 0.149(11) 0.122(9) 0.062(8) 0.075(8) 0.121(9) O21 0.186(14) 0.149(12) 0.060(7) 0.019(7) 0.010(8) 0.108(11) O22 0.089(7) 0.107(8) 0.059(5) 0.041(5) 0.035(5) 0.063(6) O23 0.064(7) 0.079(8) 0.141(11) -0.018(7) -0.009(7) 0.014(6) O24 0.28(2) 0.173(15) 0.049(7) 0.005(8) 0.054(10) 0.067(15) O25 0.103(7) 0.067(5) 0.035(4) 0.009(4) 0.003(4) 0.055(5) O26 0.073(6) 0.140(9) 0.050(5) 0.056(6) 0.034(4) 0.063(6) O27 0.120(9) 0.062(6) 0.129(9) 0.018(6) -0.059(7) 0.053(6) O28 0.062(5) 0.082(7) 0.081(7) 0.016(6) 0.026(5) 0.029(5) O29 0.30(2) 0.107(11) 0.079(9) 0.014(8) 0.094(13) -0.018(13) O30 0.071(8) 0.085(9) 0.26(2) 0.005(11) 0.021(10) 0.040(7) N25 0.036(4) 0.039(4) 0.017(3) 0.009(3) 0.006(3) 0.021(3) N26 0.038(4) 0.018(3) 0.031(4) 0.007(3) 0.017(3) 0.008(3) O1W 0.050(4) 0.032(3) 0.034(3) 0.006(3) 0.016(3) 0.015(3) O2W 0.030(3) 0.021(3) 0.037(3) 0.009(2) 0.005(3) 0.011(2) O3W 0.052(4) 0.029(3) 0.026(3) 0.007(3) 0.003(3) 0.021(3) O4W 0.040(3) 0.035(3) 0.029(3) 0.013(3) 0.009(3) 0.006(3) O5W 0.046(4) 0.042(4) 0.036(3) 0.021(3) 0.004(3) 0.025(3) O6W 0.054(4) 0.096(6) 0.030(3) 0.021(4) 0.018(3) 0.058(4) O7W 0.059(5) 0.051(4) 0.041(4) 0.002(3) 0.027(4) 0.007(4) O8W 0.051(4) 0.103(6) 0.028(4) -0.015(4) -0.001(3) 0.051(5) O13 0.047(3) 0.028(3) 0.014(3) 0.005(2) 0.005(2) 0.014(3) O14 0.062(5) 0.070(5) 0.041(4) -0.003(4) -0.013(4) 0.046(4) O15 0.080(6) 0.103(7) 0.056(5) -0.006(5) 0.009(4) 0.071(6) O16 0.031(3) 0.049(4) 0.026(3) 0.013(3) 0.006(2) 0.018(3) O17 0.030(3) 0.041(4) 0.035(3) 0.010(3) 0.007(3) 0.019(3) O18 0.065(5) 0.027(3) 0.049(4) 0.004(3) 0.024(4) 0.014(3) La1 0.0235(2) 0.0202(2) 0.0165(2) 0.00915(17) 0.00246(16) 0.00808(18) La2 0.0243(2) 0.0317(3) 0.0161(2) -0.00024(18) 0.00239(17) 0.0153(2) C1 0.015(3) 0.020(4) 0.017(3) 0.007(3) -0.002(3) 0.007(3) C2 0.020(3) 0.017(3) 0.019(3) 0.005(3) 0.001(3) 0.011(3) C3 0.019(3) 0.020(4) 0.021(4) 0.006(3) 0.002(3) 0.012(3) C4 0.017(3) 0.018(4) 0.022(4) 0.010(3) 0.005(3) 0.009(3) C5 0.023(4) 0.018(4) 0.019(4) 0.006(3) -0.004(3) 0.011(3) C6 0.018(3) 0.019(4) 0.032(4) 0.016(3) 0.011(3) 0.015(3) C7 0.021(3) 0.006(3) 0.014(3) -0.003(3) -0.003(3) 0.004(3) C8 0.017(3) 0.013(3) 0.019(3) 0.006(3) 0.005(3) 0.009(3) C9 0.016(3) 0.014(3) 0.016(3) 0.007(3) 0.002(3) 0.007(3) C10 0.017(3) 0.017(3) 0.015(3) 0.008(3) 0.007(3) 0.009(3) C11 0.017(3) 0.019(4) 0.013(3) 0.003(3) 0.005(3) 0.008(3) C12 0.022(3) 0.026(4) 0.010(3) 0.010(3) 0.004(3) 0.015(3) C13 0.019(3) 0.019(3) 0.016(3) 0.005(3) 0.007(3) 0.009(3) C14 0.019(3) 0.018(3) 0.012(3) 0.004(3) 0.008(3) 0.010(3) C15 0.017(3) 0.014(3) 0.016(3) 0.007(3) 0.006(3) 0.009(3) C16 0.021(3) 0.021(4) 0.015(3) 0.009(3) 0.003(3) 0.015(3) C17 0.025(4) 0.021(4) 0.016(3) 0.006(3) 0.009(3) 0.012(3) C18 0.019(3) 0.022(4) 0.014(3) 0.007(3) 0.003(3) 0.011(3) C19 0.017(3) 0.023(4) 0.037(5) 0.018(3) 0.012(3) 0.009(3) C20 0.018(3) 0.019(4) 0.019(4) 0.004(3) 0.005(3) 0.006(3) C21 0.020(3) 0.020(4) 0.026(4) 0.006(3) 0.007(3) 0.011(3) C22 0.019(3) 0.021(4) 0.021(4) 0.004(3) 0.003(3) 0.011(3) C23 0.023(4) 0.021(4) 0.038(4) 0.015(3) 0.012(3) 0.011(3) C24 0.031(4) 0.017(4) 0.020(4) 0.000(3) 0.000(3) 0.011(3) C25 0.027(4) 0.013(3) 0.022(4) 0.009(3) 0.004(3) 0.005(3) C26 0.027(4) 0.016(3) 0.024(4) 0.005(3) 0.006(3) 0.015(3) C27 0.024(4) 0.020(4) 0.022(4) 0.010(3) 0.007(3) 0.012(3) C28 0.029(4) 0.020(4) 0.010(3) 0.002(3) -0.003(3) 0.013(3) C29 0.025(4) 0.021(4) 0.017(3) 0.008(3) 0.004(3) 0.011(3) C30 0.019(3) 0.029(4) 0.014(3) 0.003(3) 0.006(3) 0.012(3) C31 0.027(4) 0.018(4) 0.024(4) 0.010(3) 0.003(3) 0.013(3) C32 0.022(3) 0.019(4) 0.015(3) 0.006(3) 0.002(3) 0.012(3) C33 0.025(4) 0.014(3) 0.016(3) 0.002(3) 0.001(3) 0.013(3) C34 0.028(4) 0.023(4) 0.022(4) 0.007(3) 0.002(3) 0.013(3) C35 0.022(4) 0.015(4) 0.028(4) 0.007(3) -0.002(3) 0.008(3) C36 0.021(3) 0.019(4) 0.025(4) 0.009(3) 0.006(3) 0.011(3) C37 0.022(4) 0.019(4) 0.036(4) 0.009(3) -0.001(3) 0.014(3) C38 0.029(4) 0.032(5) 0.029(4) 0.004(4) -0.010(3) 0.015(4) C39 0.019(4) 0.026(4) 0.034(4) 0.003(3) -0.004(3) 0.012(3) C40 0.021(4) 0.018(4) 0.033(4) 0.010(3) 0.005(3) 0.010(3) C41 0.018(3) 0.014(4) 0.035(4) 0.006(3) -0.003(3) 0.003(3) C42 0.052(5) 0.013(4) 0.038(5) -0.006(4) -0.022(4) 0.017(4) C43 0.036(4) 0.017(4) 0.028(4) 0.000(3) 0.006(4) 0.008(4) C44 0.027(4) 0.018(4) 0.025(4) 0.012(3) 0.009(3) 0.015(3) C45 0.026(4) 0.018(4) 0.014(3) 0.000(3) 0.003(3) 0.011(3) C46 0.030(4) 0.020(4) 0.033(4) 0.002(3) 0.012(3) 0.014(3) C47 0.027(4) 0.028(4) 0.030(4) 0.008(3) 0.014(3) 0.017(4) C48 0.025(4) 0.023(4) 0.023(4) 0.008(3) 0.007(3) 0.015(3) C49 0.021(3) 0.028(4) 0.025(4) 0.011(3) 0.009(3) 0.015(3) C50 0.021(4) 0.037(5) 0.027(4) 0.010(4) 0.002(3) 0.014(4) C51 0.019(4) 0.035(5) 0.051(6) 0.004(4) 0.001(4) 0.012(4) C52 0.020(4) 0.019(4) 0.043(5) 0.007(4) 0.007(3) 0.005(3) C53 0.021(4) 0.023(4) 0.044(5) 0.008(4) 0.001(3) 0.011(3) C54 0.032(5) 0.030(5) 0.062(6) 0.014(5) 0.013(4) 0.016(4) C55 0.031(4) 0.027(5) 0.059(6) 0.016(4) 0.005(4) 0.012(4) C56 0.028(4) 0.020(4) 0.030(4) 0.002(3) 0.002(3) 0.013(3) C57 0.023(4) 0.013(4) 0.028(4) 0.002(3) -0.004(3) 0.006(3) C58 0.039(4) 0.024(4) 0.024(4) 0.001(3) 0.002(3) 0.018(4) C59 0.030(4) 0.026(4) 0.040(5) 0.013(4) 0.012(4) 0.017(4) C60 0.023(4) 0.021(4) 0.031(4) 0.015(3) 0.003(3) 0.013(3) N1 0.024(3) 0.015(3) 0.023(3) 0.006(3) 0.004(3) 0.011(3) N2 0.020(3) 0.017(3) 0.017(3) 0.006(2) 0.004(2) 0.011(3) N3 0.023(3) 0.020(3) 0.023(3) 0.008(3) 0.006(3) 0.013(3) N4 0.020(3) 0.016(3) 0.021(3) 0.008(2) 0.004(2) 0.011(3) N5 0.021(3) 0.015(3) 0.013(3) 0.004(2) 0.002(2) 0.012(2) N6 0.017(3) 0.020(3) 0.016(3) 0.008(2) 0.003(2) 0.007(3) N7 0.018(3) 0.017(3) 0.011(3) 0.003(2) 0.005(2) 0.010(2) N8 0.020(3) 0.017(3) 0.009(3) 0.002(2) 0.003(2) 0.010(2) N9 0.018(3) 0.017(3) 0.013(3) 0.004(2) 0.003(2) 0.007(3) N10 0.020(3) 0.020(3) 0.016(3) 0.008(2) 0.004(2) 0.009(3) N11 0.019(3) 0.019(3) 0.017(3) 0.004(2) 0.004(2) 0.010(3) N12 0.018(3) 0.018(3) 0.007(3) -0.002(2) 0.001(2) 0.009(2) N13 0.026(3) 0.016(3) 0.014(3) 0.004(2) 0.004(2) 0.011(3) N14 0.024(3) 0.020(3) 0.027(3) 0.011(3) 0.008(3) 0.011(3) N15 0.021(3) 0.017(3) 0.013(3) 0.004(2) 0.004(2) 0.010(3) N16 0.024(3) 0.017(3) 0.024(3) 0.005(3) 0.007(3) 0.012(3) N17 0.027(3) 0.019(3) 0.025(3) 0.005(3) 0.010(3) 0.013(3) N18 0.020(3) 0.019(3) 0.019(3) 0.004(3) 0.002(2) 0.007(3) N19 0.021(3) 0.016(3) 0.023(3) 0.005(3) 0.004(3) 0.009(3) N20 0.027(3) 0.027(3) 0.009(3) 0.011(2) 0.009(2) 0.023(3) N21 0.022(3) 0.020(3) 0.018(3) 0.004(3) 0.002(2) 0.008(3) N22 0.023(3) 0.012(3) 0.020(3) 0.003(2) 0.003(2) 0.009(3) N23 0.022(3) 0.020(3) 0.019(3) 0.007(3) 0.001(2) 0.010(3) N24 0.026(3) 0.018(3) 0.019(3) 0.006(3) 0.001(2) 0.011(3) O1 0.027(3) 0.021(3) 0.018(3) 0.007(2) 0.007(2) 0.011(2) O2 0.027(3) 0.021(3) 0.010(2) 0.006(2) 0.005(2) 0.011(2) O3 0.021(3) 0.030(3) 0.024(3) 0.014(2) 0.001(2) 0.010(2) O4 0.026(3) 0.027(3) 0.027(3) 0.013(2) 0.006(2) 0.013(2) O5 0.032(3) 0.024(3) 0.025(3) 0.007(2) 0.005(2) 0.012(3) O6 0.032(3) 0.027(3) 0.022(3) 0.005(2) 0.009(2) 0.014(3) O7 0.032(3) 0.019(3) 0.024(3) 0.007(2) 0.004(2) 0.016(2) O8 0.025(3) 0.024(3) 0.015(3) 0.000(2) 0.002(2) 0.014(2) O9 0.025(3) 0.031(3) 0.012(2) 0.002(2) 0.006(2) 0.015(2) O10 0.028(3) 0.027(3) 0.019(3) 0.006(2) 0.008(2) 0.016(2) O11 0.034(3) 0.035(3) 0.026(3) 0.015(3) 0.009(2) 0.020(3) O12 0.035(3) 0.046(4) 0.031(3) 0.023(3) -0.001(3) 0.012(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 N27 O20 1.165(12) . ? N27 O19 1.229(12) . ? N27 O21 1.233(14) . ? N28 O22 1.201(15) . ? N28 O23 1.277(17) . ? N28 O24 1.278(16) . ? N29 O26 1.249(2) . ? N29 O25 1.249(2) . ? N29 O27 1.249(2) . ? N30 O28 1.247(2) . ? N30 O30 1.248(2) . ? N30 O29 1.251(2) . ? N25 O15 1.210(10) . ? N25 O14 1.222(9) . ? N25 O13 1.287(9) . ? N26 O18 1.229(9) . ? N26 O17 1.253(9) . ? N26 O16 1.271(9) . ? N26 La1 3.067(7) . ? O1W La2 2.496(6) . ? O2W La1 2.493(6) . ? O3W La2 2.494(6) . ? O4W La1 2.569(6) . ? O5W La1 2.547(5) . ? O6W La2 2.470(6) . ? O7W La2 2.532(7) . ? O8W La2 2.544(7) . ? O13 La1 2.495(5) . ? O16 La1 2.642(6) . ? O17 La1 2.607(6) . ? La1 O2 2.498(5) . ? La1 O3 2.548(5) . ? La1 O1 2.609(5) . ? La2 O7 2.464(5) . ? La2 O10 2.533(5) 2_565 ? La2 O8 2.620(5) . ? C1 O1 1.246(9) . ? C1 N1 1.348(9) . ? C1 N2 1.364(9) . ? C2 N3 1.454(9) . ? C2 N1 1.475(9) . ? C2 C37 1.513(9) . ? C2 C3 1.575(9) . ? C3 N4 1.453(9) . ? C3 N2 1.458(9) . ? C3 C40 1.520(10) . ? C4 O7 1.225(9) . ? C4 N4 1.350(9) . ? C4 N3 1.373(9) . ? C5 N2 1.452(9) . ? C5 N5 1.460(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.448(8) . ? C6 N7 1.451(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.251(8) . ? C7 N6 1.344(9) . ? C7 N5 1.344(9) . ? C8 N5 1.462(8) . ? C8 N7 1.466(9) . ? C8 C41 1.525(9) . ? C8 C9 1.567(9) . ? C9 N8 1.463(9) . ? C9 N6 1.471(8) . ? C9 C44 1.537(9) . ? C10 O8 1.234(8) . ? C10 N7 1.355(8) . ? C10 N8 1.370(9) . ? C11 N9 1.445(9) . ? C11 N6 1.447(9) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.430(9) . ? C12 N8 1.454(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.236(8) . ? C13 N10 1.371(9) . ? C13 N9 1.384(9) . ? C14 N9 1.449(8) . ? C14 N11 1.467(8) . ? C14 C45 1.536(9) . ? C14 C15 1.577(9) . ? C15 N12 1.458(8) . ? C15 N10 1.469(8) . ? C15 C48 1.536(9) . ? C16 O9 1.229(8) . ? C16 N12 1.353(9) . ? C16 N11 1.357(9) . ? C17 N13 1.439(9) . ? C17 N10 1.451(9) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.441(9) . ? C18 N12 1.444(9) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.211(9) . ? C19 N14 1.373(10) . ? C19 N13 1.376(9) . ? C20 N13 1.460(9) . ? C20 N15 1.477(9) . ? C20 C49 1.523(10) . ? C20 C21 1.574(10) . ? C21 N14 1.452(9) . ? C21 N16 1.458(9) . ? C21 C52 1.534(10) . ? C22 O10 1.243(9) . ? C22 N15 1.349(9) . ? C22 N16 1.368(9) . ? C23 N17 1.434(10) . ? C23 N14 1.452(9) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.452(9) . ? C24 N16 1.462(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.216(9) . ? C25 N17 1.359(10) . ? C25 N18 1.365(10) . ? C26 N19 1.453(9) . ? C26 N17 1.467(9) . ? C26 C53 1.521(10) . ? C26 C27 1.588(10) . ? C27 N20 1.432(9) . ? C27 N18 1.460(9) . ? C27 C56 1.531(10) . ? C28 O11 1.260(9) . ? C28 N19 1.344(10) . ? C28 N20 1.363(8) . ? C29 N21 1.443(9) . ? C29 N18 1.444(9) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N23 1.454(9) . ? C30 N20 1.470(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O6 1.233(9) . ? C31 N21 1.354(10) . ? C31 N22 1.368(9) . ? C32 N21 1.447(9) . ? C32 N23 1.455(8) . ? C32 C57 1.528(10) . ? C32 C33 1.590(10) . ? C33 N24 1.441(9) . ? C33 N22 1.474(9) . ? C33 C60 1.514(9) . ? C34 O12 1.208(9) . ? C34 N23 1.371(10) . ? C34 N24 1.372(9) . ? C35 N22 1.446(9) . ? C35 N1 1.461(9) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N24 1.435(9) . ? C36 N3 1.451(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C38 1.520(11) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 C39 1.545(11) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C39 C40 1.521(10) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 C42 1.543(11) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 C43 1.497(12) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 C44 1.511(11) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.514(10) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C46 C47 1.541(11) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C47 C48 1.516(10) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 C50 1.539(11) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C50 C51 1.544(12) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 C52 1.502(12) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.521(12) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.548(12) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 C56 1.510(12) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 C58 1.521(11) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 C59 1.528(11) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 C60 1.541(11) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? O10 La2 2.533(5) 2_565 ? 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 O20 N27 O19 121.7(12) . . ? O20 N27 O21 118.1(13) . . ? O19 N27 O21 120.1(12) . . ? O22 N28 O23 129.3(13) . . ? O22 N28 O24 117.1(17) . . ? O23 N28 O24 113.3(15) . . ? O26 N29 O25 118.0(7) . . ? O26 N29 O27 122.7(9) . . ? O25 N29 O27 119.3(8) . . ? O28 N30 O30 118.2(13) . . ? O28 N30 O29 112.9(12) . . ? O30 N30 O29 128.9(14) . . ? O15 N25 O14 122.1(8) . . ? O15 N25 O13 118.0(7) . . ? O14 N25 O13 119.6(7) . . ? O18 N26 O17 122.3(8) . . ? O18 N26 O16 121.9(8) . . ? O17 N26 O16 115.8(6) . . ? O18 N26 La1 178.3(6) . . ? O17 N26 La1 57.0(4) . . ? O16 N26 La1 58.8(4) . . ? N25 O13 La1 133.7(5) . . ? N26 O16 La1 97.0(4) . . ? N26 O17 La1 99.2(5) . . ? O2W La1 O13 73.18(19) . . ? O2W La1 O2 141.24(17) . . ? O13 La1 O2 68.07(17) . . ? O2W La1 O5W 81.7(2) . . ? O13 La1 O5W 129.8(2) . . ? O2 La1 O5W 124.01(18) . . ? O2W La1 O3 84.27(18) . . ? O13 La1 O3 70.13(19) . . ? O2 La1 O3 82.80(16) . . ? O5W La1 O3 149.57(19) . . ? O2W La1 O4W 70.6(2) . . ? O13 La1 O4W 134.36(19) . . ? O2 La1 O4W 141.21(19) . . ? O5W La1 O4W 70.4(2) . . ? O3 La1 O4W 79.46(19) . . ? O2W La1 O17 131.92(19) . . ? O13 La1 O17 121.37(19) . . ? O2 La1 O17 72.13(17) . . ? O5W La1 O17 107.8(2) . . ? O3 La1 O17 63.65(18) . . ? O4W La1 O17 69.1(2) . . ? O2W La1 O1 89.55(17) . . ? O13 La1 O1 69.64(18) . . ? O2 La1 O1 77.28(16) . . ? O5W La1 O1 67.47(18) . . ? O3 La1 O1 139.37(16) . . ? O4W La1 O1 135.52(19) . . ? O17 La1 O1 138.16(17) . . ? O2W La1 O16 148.89(19) . . ? O13 La1 O16 136.89(19) . . ? O2 La1 O16 69.37(17) . . ? O5W La1 O16 71.7(2) . . ? O3 La1 O16 110.90(19) . . ? O4W La1 O16 85.24(19) . . ? O17 La1 O16 48.04(18) . . ? O1 La1 O16 94.70(17) . . ? O2W La1 N26 145.95(18) . . ? O13 La1 N26 133.62(18) . . ? O2 La1 N26 69.41(16) . . ? O5W La1 N26 89.6(2) . . ? O3 La1 N26 87.11(19) . . ? O4W La1 N26 75.46(19) . . ? O17 La1 N26 23.78(19) . . ? O1 La1 N26 117.36(18) . . ? O16 La1 N26 24.28(19) . . ? O7 La2 O6W 142.9(2) . . ? O7 La2 O3W 100.19(18) . . ? O6W La2 O3W 106.7(2) . . ? O7 La2 O1W 86.8(2) . . ? O6W La2 O1W 79.7(2) . . ? O3W La2 O1W 69.0(2) . . ? O7 La2 O7W 82.6(2) . . ? O6W La2 O7W 92.4(3) . . ? O3W La2 O7W 139.9(2) . . ? O1W La2 O7W 150.5(2) . . ? O7 La2 O10 146.17(17) . 2_565 ? O6W La2 O10 67.49(18) . 2_565 ? O3W La2 O10 74.42(17) . 2_565 ? O1W La2 O10 120.19(19) . 2_565 ? O7W La2 O10 81.5(2) . 2_565 ? O7 La2 O8W 72.3(2) . . ? O6W La2 O8W 140.2(2) . . ? O3W La2 O8W 72.1(3) . . ? O1W La2 O8W 131.3(3) . . ? O7W La2 O8W 70.8(3) . . ? O10 La2 O8W 74.3(2) 2_565 . ? O7 La2 O8 76.52(16) . . ? O6W La2 O8 66.61(19) . . ? O3W La2 O8 142.94(18) . . ? O1W La2 O8 73.91(18) . . ? O7W La2 O8 76.9(2) . . ? O10 La2 O8 127.73(16) 2_565 . ? O8W La2 O8 137.3(2) . . ? O1 C1 N1 125.2(6) . . ? O1 C1 N2 124.7(7) . . ? N1 C1 N2 110.0(6) . . ? N3 C2 N1 111.5(6) . . ? N3 C2 C37 114.1(6) . . ? N1 C2 C37 112.8(6) . . ? N3 C2 C3 102.8(5) . . ? N1 C2 C3 102.7(5) . . ? C37 C2 C3 111.9(6) . . ? N4 C3 N2 112.1(5) . . ? N4 C3 C40 112.7(6) . . ? N2 C3 C40 112.9(6) . . ? N4 C3 C2 102.6(5) . . ? N2 C3 C2 102.7(5) . . ? C40 C3 C2 113.0(5) . . ? O7 C4 N4 125.7(6) . . ? O7 C4 N3 125.4(7) . . ? N4 C4 N3 108.9(6) . . ? N2 C5 N5 115.7(6) . . ? N2 C5 H5A 108.3 . . ? N5 C5 H5A 108.3 . . ? N2 C5 H5B 108.3 . . ? N5 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? N4 C6 N7 113.0(5) . . ? N4 C6 H6A 109.0 . . ? N7 C6 H6A 109.0 . . ? N4 C6 H6B 109.0 . . ? N7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O2 C7 N6 125.2(7) . . ? O2 C7 N5 124.0(6) . . ? N6 C7 N5 110.6(6) . . ? N5 C8 N7 112.4(5) . . ? N5 C8 C41 113.1(6) . . ? N7 C8 C41 112.8(6) . . ? N5 C8 C9 102.9(5) . . ? N7 C8 C9 102.2(5) . . ? C41 C8 C9 112.5(5) . . ? N8 C9 N6 112.3(5) . . ? N8 C9 C44 113.6(5) . . ? N6 C9 C44 111.7(6) . . ? N8 C9 C8 103.6(5) . . ? N6 C9 C8 102.5(5) . . ? C44 C9 C8 112.4(5) . . ? O8 C10 N7 125.4(6) . . ? O8 C10 N8 125.4(6) . . ? N7 C10 N8 109.3(6) . . ? N9 C11 N6 115.4(6) . . ? N9 C11 H11A 108.4 . . ? N6 C11 H11A 108.4 . . ? N9 C11 H11B 108.4 . . ? N6 C11 H11B 108.4 . . ? H11A C11 H11B 107.5 . . ? N11 C12 N8 114.7(5) . . ? N11 C12 H12A 108.6 . . ? N8 C12 H12A 108.6 . . ? N11 C12 H12B 108.6 . . ? N8 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N10 125.4(6) . . ? O3 C13 N9 126.1(6) . . ? N10 C13 N9 108.4(6) . . ? N9 C14 N11 112.6(5) . . ? N9 C14 C45 113.8(6) . . ? N11 C14 C45 112.3(5) . . ? N9 C14 C15 103.6(5) . . ? N11 C14 C15 101.9(5) . . ? C45 C14 C15 111.7(5) . . ? N12 C15 N10 112.3(5) . . ? N12 C15 C48 113.3(5) . . ? N10 C15 C48 112.4(5) . . ? N12 C15 C14 103.5(5) . . ? N10 C15 C14 102.3(5) . . ? C48 C15 C14 112.1(5) . . ? O9 C16 N12 125.1(6) . . ? O9 C16 N11 124.7(6) . . ? N12 C16 N11 110.2(6) . . ? N13 C17 N10 115.8(6) . . ? N13 C17 H17A 108.3 . . ? N10 C17 H17A 108.3 . . ? N13 C17 H17B 108.3 . . ? N10 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? N15 C18 N12 114.7(5) . . ? N15 C18 H18A 108.6 . . ? N12 C18 H18A 108.6 . . ? N15 C18 H18B 108.6 . . ? N12 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? O4 C19 N14 125.4(7) . . ? O4 C19 N13 125.8(7) . . ? N14 C19 N13 108.7(6) . . ? N13 C20 N15 112.6(5) . . ? N13 C20 C49 114.6(6) . . ? N15 C20 C49 111.8(6) . . ? N13 C20 C21 102.6(5) . . ? N15 C20 C21 102.4(5) . . ? C49 C20 C21 111.7(6) . . ? N14 C21 N16 113.1(6) . . ? N14 C21 C52 112.5(6) . . ? N16 C21 C52 112.3(6) . . ? N14 C21 C20 103.3(6) . . ? N16 C21 C20 102.8(5) . . ? C52 C21 C20 112.0(6) . . ? O10 C22 N15 125.5(7) . . ? O10 C22 N16 125.0(7) . . ? N15 C22 N16 109.5(6) . . ? N17 C23 N14 113.8(6) . . ? N17 C23 H23A 108.8 . . ? N14 C23 H23A 108.8 . . ? N17 C23 H23B 108.8 . . ? N14 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? N19 C24 N16 113.3(6) . . ? N19 C24 H24A 108.9 . . ? N16 C24 H24A 108.9 . . ? N19 C24 H24B 108.9 . . ? N16 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? O5 C25 N17 125.9(7) . . ? O5 C25 N18 125.2(7) . . ? N17 C25 N18 108.8(6) . . ? N19 C26 N17 112.1(6) . . ? N19 C26 C53 114.3(6) . . ? N17 C26 C53 112.3(6) . . ? N19 C26 C27 103.1(6) . . ? N17 C26 C27 101.7(6) . . ? C53 C26 C27 112.2(6) . . ? N20 C27 N18 113.8(6) . . ? N20 C27 C56 112.5(6) . . ? N18 C27 C56 113.4(6) . . ? N20 C27 C26 101.6(5) . . ? N18 C27 C26 103.0(6) . . ? C56 C27 C26 111.4(6) . . ? O11 C28 N19 124.9(6) . . ? O11 C28 N20 125.9(7) . . ? N19 C28 N20 109.1(6) . . ? N21 C29 N18 115.1(6) . . ? N21 C29 H29A 108.5 . . ? N18 C29 H29A 108.5 . . ? N21 C29 H29B 108.5 . . ? N18 C29 H29B 108.5 . . ? H29A C29 H29B 107.5 . . ? N23 C30 N20 114.2(6) . . ? N23 C30 H30A 108.7 . . ? N20 C30 H30A 108.7 . . ? N23 C30 H30B 108.7 . . ? N20 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? O6 C31 N21 125.3(7) . . ? O6 C31 N22 124.7(7) . . ? N21 C31 N22 110.1(6) . . ? N21 C32 N23 112.9(6) . . ? N21 C32 C57 113.2(6) . . ? N23 C32 C57 112.6(6) . . ? N21 C32 C33 102.6(5) . . ? N23 C32 C33 102.1(5) . . ? C57 C32 C33 112.5(6) . . ? N24 C33 N22 112.6(5) . . ? N24 C33 C60 114.3(6) . . ? N22 C33 C60 113.0(6) . . ? N24 C33 C32 102.5(5) . . ? N22 C33 C32 102.2(5) . . ? C60 C33 C32 111.1(5) . . ? O12 C34 N23 126.5(7) . . ? O12 C34 N24 125.5(7) . . ? N23 C34 N24 108.0(6) . . ? N22 C35 N1 115.5(6) . . ? N22 C35 H35A 108.4 . . ? N1 C35 H35A 108.4 . . ? N22 C35 H35B 108.4 . . ? N1 C35 H35B 108.4 . . ? H35A C35 H35B 107.5 . . ? N24 C36 N3 115.0(6) . . ? N24 C36 H36A 108.5 . . ? N3 C36 H36A 108.5 . . ? N24 C36 H36B 108.5 . . ? N3 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? C2 C37 C38 111.4(6) . . ? C2 C37 H37A 109.3 . . ? C38 C37 H37A 109.3 . . ? C2 C37 H37B 109.3 . . ? C38 C37 H37B 109.3 . . ? H37A C37 H37B 108.0 . . ? C37 C38 C39 113.0(6) . . ? C37 C38 H38A 109.0 . . ? C39 C38 H38A 109.0 . . ? C37 C38 H38B 109.0 . . ? C39 C38 H38B 109.0 . . ? H38A C38 H38B 107.8 . . ? C40 C39 C38 113.0(6) . . ? C40 C39 H39A 109.0 . . ? C38 C39 H39A 109.0 . . ? C40 C39 H39B 109.0 . . ? C38 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C3 C40 C39 111.4(6) . . ? C3 C40 H40A 109.3 . . ? C39 C40 H40A 109.3 . . ? C3 C40 H40B 109.3 . . ? C39 C40 H40B 109.3 . . ? H40A C40 H40B 108.0 . . ? C8 C41 C42 110.7(7) . . ? C8 C41 H41A 109.5 . . ? C42 C41 H41A 109.5 . . ? C8 C41 H41B 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C43 C42 C41 113.0(7) . . ? C43 C42 H42A 109.0 . . ? C41 C42 H42A 109.0 . . ? C43 C42 H42B 109.0 . . ? C41 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? C42 C43 C44 115.0(7) . . ? C42 C43 H43A 108.5 . . ? C44 C43 H43A 108.5 . . ? C42 C43 H43B 108.5 . . ? C44 C43 H43B 108.5 . . ? H43A C43 H43B 107.5 . . ? C43 C44 C9 111.4(6) . . ? C43 C44 H44A 109.3 . . ? C9 C44 H44A 109.3 . . ? C43 C44 H44B 109.3 . . ? C9 C44 H44B 109.3 . . ? H44A C44 H44B 108.0 . . ? C46 C45 C14 110.6(6) . . ? C46 C45 H45A 109.5 . . ? C14 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? C14 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? C45 C46 C47 113.4(6) . . ? C45 C46 H46A 108.9 . . ? C47 C46 H46A 108.9 . . ? C45 C46 H46B 108.9 . . ? C47 C46 H46B 108.9 . . ? H46A C46 H46B 107.7 . . ? C48 C47 C46 112.6(6) . . ? C48 C47 H47A 109.1 . . ? C46 C47 H47A 109.1 . . ? C48 C47 H47B 109.1 . . ? C46 C47 H47B 109.1 . . ? H47A C47 H47B 107.8 . . ? C47 C48 C15 111.3(6) . . ? C47 C48 H48A 109.4 . . ? C15 C48 H48A 109.4 . . ? C47 C48 H48B 109.4 . . ? C15 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? C20 C49 C50 110.2(6) . . ? C20 C49 H49A 109.6 . . ? C50 C49 H49A 109.6 . . ? C20 C49 H49B 109.6 . . ? C50 C49 H49B 109.6 . . ? H49A C49 H49B 108.1 . . ? C49 C50 C51 111.6(7) . . ? C49 C50 H50A 109.3 . . ? C51 C50 H50A 109.3 . . ? C49 C50 H50B 109.3 . . ? C51 C50 H50B 109.3 . . ? H50A C50 H50B 108.0 . . ? C52 C51 C50 113.8(7) . . ? C52 C51 H51A 108.8 . . ? C50 C51 H51A 108.8 . . ? C52 C51 H51B 108.8 . . ? C50 C51 H51B 108.8 . . ? H51A C51 H51B 107.7 . . ? C51 C52 C21 111.3(7) . . ? C51 C52 H52A 109.4 . . ? C21 C52 H52A 109.4 . . ? C51 C52 H52B 109.4 . . ? C21 C52 H52B 109.4 . . ? H52A C52 H52B 108.0 . . ? C54 C53 C26 110.2(7) . . ? C54 C53 H53A 109.6 . . ? C26 C53 H53A 109.6 . . ? C54 C53 H53B 109.6 . . ? C26 C53 H53B 109.6 . . ? H53A C53 H53B 108.1 . . ? C53 C54 C55 112.5(8) . . ? C53 C54 H54A 109.1 . . ? C55 C54 H54A 109.1 . . ? C53 C54 H54B 109.1 . . ? C55 C54 H54B 109.1 . . ? H54A C54 H54B 107.8 . . ? C56 C55 C54 112.9(7) . . ? C56 C55 H55A 109.0 . . ? C54 C55 H55A 109.0 . . ? C56 C55 H55B 109.0 . . ? C54 C55 H55B 109.0 . . ? H55A C55 H55B 107.8 . . ? C55 C56 C27 111.8(7) . . ? C55 C56 H56A 109.3 . . ? C27 C56 H56A 109.3 . . ? C55 C56 H56B 109.3 . . ? C27 C56 H56B 109.3 . . ? H56A C56 H56B 107.9 . . ? C58 C57 C32 109.9(6) . . ? C58 C57 H57A 109.7 . . ? C32 C57 H57A 109.7 . . ? C58 C57 H57B 109.7 . . ? C32 C57 H57B 109.7 . . ? H57A C57 H57B 108.2 . . ? C57 C58 C59 112.1(6) . . ? C57 C58 H58A 109.2 . . ? C59 C58 H58A 109.2 . . ? C57 C58 H58B 109.2 . . ? C59 C58 H58B 109.2 . . ? H58A C58 H58B 107.9 . . ? C58 C59 C60 113.0(6) . . ? C58 C59 H59A 109.0 . . ? C60 C59 H59A 109.0 . . ? C58 C59 H59B 109.0 . . ? C60 C59 H59B 109.0 . . ? H59A C59 H59B 107.8 . . ? C33 C60 C59 111.7(6) . . ? C33 C60 H60A 109.3 . . ? C59 C60 H60A 109.3 . . ? C33 C60 H60B 109.3 . . ? C59 C60 H60B 109.3 . . ? H60A C60 H60B 107.9 . . ? C1 N1 C35 124.0(6) . . ? C1 N1 C2 112.0(5) . . ? C35 N1 C2 123.5(6) . . ? C1 N2 C5 124.2(6) . . ? C1 N2 C3 112.3(6) . . ? C5 N2 C3 123.0(6) . . ? C4 N3 C36 121.3(6) . . ? C4 N3 C2 112.3(6) . . ? C36 N3 C2 125.2(6) . . ? C4 N4 C6 121.7(6) . . ? C4 N4 C3 113.2(5) . . ? C6 N4 C3 124.7(6) . . ? C7 N5 C5 120.6(6) . . ? C7 N5 C8 112.1(5) . . ? C5 N5 C8 127.2(6) . . ? C7 N6 C11 121.8(6) . . ? C7 N6 C9 111.9(6) . . ? C11 N6 C9 126.2(5) . . ? C10 N7 C6 121.3(6) . . ? C10 N7 C8 113.1(5) . . ? C6 N7 C8 124.8(6) . . ? C10 N8 C12 121.0(5) . . ? C10 N8 C9 111.8(5) . . ? C12 N8 C9 125.1(5) . . ? C13 N9 C11 122.3(6) . . ? C13 N9 C14 112.4(5) . . ? C11 N9 C14 124.6(6) . . ? C13 N10 C17 121.6(6) . . ? C13 N10 C15 112.8(5) . . ? C17 N10 C15 125.0(6) . . ? C16 N11 C12 122.3(6) . . ? C16 N11 C14 112.3(5) . . ? C12 N11 C14 124.9(6) . . ? C16 N12 C18 122.7(6) . . ? C16 N12 C15 111.8(5) . . ? C18 N12 C15 124.7(5) . . ? C19 N13 C17 119.4(6) . . ? C19 N13 C20 112.3(6) . . ? C17 N13 C20 125.3(6) . . ? C19 N14 C21 112.4(6) . . ? C19 N14 C23 121.6(6) . . ? C21 N14 C23 125.4(6) . . ? C22 N15 C18 123.3(6) . . ? C22 N15 C20 112.4(6) . . ? C18 N15 C20 124.1(6) . . ? C22 N16 C21 112.3(6) . . ? C22 N16 C24 122.0(6) . . ? C21 N16 C24 125.1(6) . . ? C25 N17 C23 121.3(7) . . ? C25 N17 C26 113.6(6) . . ? C23 N17 C26 125.2(6) . . ? C25 N18 C29 121.5(6) . . ? C25 N18 C27 112.8(6) . . ? C29 N18 C27 125.7(6) . . ? C28 N19 C24 121.9(6) . . ? C28 N19 C26 112.3(6) . . ? C24 N19 C26 124.6(6) . . ? C28 N20 C27 113.9(6) . . ? C28 N20 C30 118.9(6) . . ? C27 N20 C30 126.2(5) . . ? C31 N21 C29 122.7(6) . . ? C31 N21 C32 112.8(6) . . ? C29 N21 C32 124.1(6) . . ? C31 N22 C35 119.9(6) . . ? C31 N22 C33 111.2(6) . . ? C35 N22 C33 124.5(6) . . ? C34 N23 C30 119.9(6) . . ? C34 N23 C32 113.0(6) . . ? C30 N23 C32 125.7(6) . . ? C34 N24 C36 121.3(6) . . ? C34 N24 C33 113.3(6) . . ? C36 N24 C33 125.2(6) . . ? C1 O1 La1 142.3(4) . . ? C7 O2 La1 126.0(4) . . ? C13 O3 La1 144.6(5) . . ? C4 O7 La2 155.6(5) . . ? C10 O8 La2 158.6(5) . . ? C22 O10 La2 145.2(5) . 2_565 ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 4.390 _refine_diff_density_min -2.989 _refine_diff_density_rms 0.166 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.005 -0.005 0.500 241 96 ' ' 2 0.499 1.499 1.000 221 75 ' ' 3 0.500 0.000 0.000 34 10 ' ' _platon_squeeze_details ; ;