# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'William J. Gee' _publ_contact_author_email will.gee@sci.monash.edu.au loop_ _publ_author_name 'Philip C. Andrews' 'William J. Gee' 'Peter C. Junk' 'Jonathan G. MacLellan' data_erpensq _database_code_depnum_ccdc_archive 'CCDC 801771' #TrackingRef 'erpensq.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C192 H184 Er9 O42, C6 H16 N' _chemical_formula_sum 'C198 H200 Er9 N O42' _chemical_formula_weight 4770.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Er Er -0.2586 4.9576 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 4' _symmetry_space_group_name_Hall 'I 4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' _cell_length_a 21.708(3) _cell_length_b 21.708(3) _cell_length_c 25.682(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12103(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22589 _cell_measurement_theta_min 1.23 _cell_measurement_theta_max 27.00 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4568 _exptl_absorpt_coefficient_mu 3.140 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22589 _diffrn_reflns_av_R_equivalents 0.1029 _diffrn_reflns_av_sigmaI/netI 0.1255 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 24.99 _reflns_number_total 10010 _reflns_number_gt 6500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The counter ion and the solvent molecules within the void could not be adequately modelled therefore the residual electron density was removed using platon. The total solvent accesible void was calculated to be 4155.8 A^3 and the electron count per cell was 3089. All phenyl rings are constrained as perfect hexagons, the 5 membered ring on ligand one had its bond lengths fixed to ideal values and all other rings were constrained to be the same as ligand one. The structure was refined as a racemic twin. ; _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^)+(0.0900P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.13(2) _refine_ls_number_reflns 10010 _refine_ls_number_parameters 434 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.1712 _refine_ls_wR_factor_gt 0.1572 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.994 _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 Er1 Er 0.96960(3) 0.11164(3) 0.52592(3) 0.03862(19) Uani 1 1 d . . . Er2 Er 1.0000 0.0000 0.42174(5) 0.0365(4) Uani 1 4 d S . . Er3 Er 1.10062(3) -0.05684(3) 0.31678(3) 0.0444(2) Uani 1 1 d . . . O1 O 1.0460(5) 0.0827(4) 0.4705(4) 0.036(3) Uani 1 1 d . . . H1 H 1.0651 0.1164 0.4495 0.044 Uiso 1 1 calc R . . O2 O 1.0000 0.0000 0.5365(6) 0.031(5) Uani 1 4 d S . . O3 O 1.0909(5) 0.0277(4) 0.3718(4) 0.040(3) Uani 1 1 d . . . H3A H 1.1283 0.0385 0.3926 0.047 Uiso 1 1 calc R . . O4 O 1.0000 0.0000 0.3083(8) 0.048(6) Uani 1 4 d S . . O5 O 0.8884(5) 0.1740(5) 0.5489(4) 0.049(3) Uani 1 1 d . . . O6 O 0.9493(5) 0.1719(5) 0.4531(4) 0.046(3) Uani 1 1 d . . . O7 O 1.0137(5) 0.2053(5) 0.5495(4) 0.049(3) Uani 1 1 d . . . O8 O 1.0497(5) 0.0907(5) 0.5841(4) 0.043(3) Uani 1 1 d . . . O9 O 1.2019(5) -0.0468(5) 0.2949(3) 0.040(3) Uani 1 1 d . . . O10 O 1.1583(5) -0.0858(5) 0.3896(4) 0.050(3) Uani 1 1 d . . . O11 O 1.1559(5) 0.1324(6) 0.2938(4) 0.061(3) Uani 1 1 d . . . O12 O 1.1007(6) 0.0284(5) 0.2575(4) 0.051(3) Uani 1 1 d . . . C1 C 0.8633(8) 0.2206(7) 0.5315(6) 0.053(5) Uani 1 1 d . . . C2 C 0.8184(4) 0.2510(4) 0.5691(3) 0.064(5) Uani 1 1 d G . . C3 C 0.8374(5) 0.2582(4) 0.6205(3) 0.114(9) Uani 1 1 d G . . H3 H 0.8779 0.2465 0.6304 0.136 Uiso 1 1 calc R . . C4 C 0.7972(6) 0.2824(5) 0.6572(3) 0.20(2) Uani 1 1 d G . . H4 H 0.8102 0.2872 0.6923 0.245 Uiso 1 1 calc R . . C5 C 0.7379(5) 0.2994(6) 0.6427(4) 0.148(14) Uani 1 1 d G . . H5 H 0.7104 0.3159 0.6679 0.177 Uiso 1 1 calc R . . C6 C 0.7189(4) 0.2922(6) 0.5914(4) 0.23(2) Uani 1 1 d G . . H6 H 0.6783 0.3039 0.5815 0.276 Uiso 1 1 calc R . . C7 C 0.7591(4) 0.2681(5) 0.5546(4) 0.157(13) Uani 1 1 d G . . H7 H 0.7461 0.2632 0.5195 0.188 Uiso 1 1 calc R . . C8 C 0.8756(3) 0.2446(3) 0.4829(2) 0.044(4) Uani 1 1 d GD . . C9 C 0.9169(4) 0.2202(4) 0.4476(3) 0.048(4) Uani 1 1 d GD . . C10 C 0.9164(4) 0.2533(5) 0.3963(2) 0.046(4) Uani 1 1 d GD . . H10A H 0.8964 0.2283 0.3689 0.055 Uiso 1 1 calc R . . H10B H 0.9585 0.2645 0.3851 0.055 Uiso 1 1 calc R . . C11 C 0.8789(4) 0.3094(5) 0.4096(3) 0.140(11) Uani 1 1 d GD . . H11A H 0.9065 0.3454 0.4135 0.168 Uiso 1 1 calc R . . H11B H 0.8496 0.3181 0.3810 0.168 Uiso 1 1 calc R . . C12 C 0.8439(4) 0.2994(4) 0.4593(3) 0.095(8) Uani 1 1 d GD . . H12A H 0.7999 0.2905 0.4523 0.114 Uiso 1 1 calc R . . H12B H 0.8468 0.3359 0.4824 0.114 Uiso 1 1 calc R . . C13 C 1.0439(4) 0.2250(8) 0.5876(4) 0.060(5) Uani 1 1 d G . . C14 C 1.0483(4) 0.2912(3) 0.5885(3) 0.058(5) Uani 1 1 d G . . C15 C 1.0031(5) 0.3259(4) 0.5637(3) 0.110(9) Uani 1 1 d G . . H15 H 0.9695 0.3059 0.5472 0.132 Uiso 1 1 calc R . . C16 C 1.0071(6) 0.3898(4) 0.5633(4) 0.120(10) Uani 1 1 d G . . H16 H 0.9763 0.4135 0.5464 0.144 Uiso 1 1 calc R . . C17 C 1.0564(7) 0.4190(3) 0.5875(4) 0.147(13) Uani 1 1 d G . . H17 H 1.0591 0.4627 0.5872 0.176 Uiso 1 1 calc R . . C18 C 1.1016(6) 0.3843(3) 0.6122(4) 0.174(16) Uani 1 1 d G . . H18 H 1.1352 0.4043 0.6288 0.208 Uiso 1 1 calc R . . C19 C 1.0975(4) 0.3204(3) 0.6127(3) 0.150(14) Uani 1 1 d G . . H19 H 1.1284 0.2968 0.6296 0.180 Uiso 1 1 calc R . . C20 C 1.0669(3) 0.1878(3) 0.6261(2) 0.053(5) Uani 1 1 d GD . . C21 C 1.0701(4) 0.1246(3) 0.6234(3) 0.050(5) Uani 1 1 d GD . . C22 C 1.0998(5) 0.0949(4) 0.6695(3) 0.059(5) Uani 1 1 d GD . . H22A H 1.1427 0.0822 0.6621 0.070 Uiso 1 1 calc R . . H22B H 1.0759 0.0591 0.6822 0.070 Uiso 1 1 calc R . . C23 C 1.0970(5) 0.1498(4) 0.7078(2) 0.187(17) Uani 1 1 d GD . . H23A H 1.0597 0.1467 0.7297 0.225 Uiso 1 1 calc R . . H23B H 1.1336 0.1494 0.7308 0.225 Uiso 1 1 calc R . . C24 C 1.0955(4) 0.2084(4) 0.6766(2) 0.117(10) Uani 1 1 d GD . . H24A H 1.1375 0.2249 0.6710 0.140 Uiso 1 1 calc R . . H24B H 1.0701 0.2402 0.6939 0.140 Uiso 1 1 calc R . . C25 C 1.2541(8) -0.0567(6) 0.3156(5) 0.066(5) Uani 1 1 d G . . C26 C 1.3098(4) -0.0421(3) 0.2787(3) 0.076(6) Uani 1 1 d G . . C27 C 1.3610(3) -0.0092(4) 0.2955(4) 0.108(9) Uani 1 1 d G . . H27 H 1.3631 0.0049 0.3305 0.130 Uiso 1 1 calc R . . C28 C 1.4089(4) 0.0031(6) 0.2612(5) 0.119(10) Uani 1 1 d G . . H28 H 1.4439 0.0257 0.2727 0.143 Uiso 1 1 calc R . . C29 C 1.4058(5) -0.0175(6) 0.2101(5) 0.145(13) Uani 1 1 d G . . H29 H 1.4385 -0.0091 0.1866 0.173 Uiso 1 1 calc R . . C30 C 1.3546(6) -0.0505(6) 0.1932(4) 0.130(12) Uani 1 1 d G . . H30 H 1.3524 -0.0646 0.1583 0.156 Uiso 1 1 calc R . . C31 C 1.3066(5) -0.0628(5) 0.2275(3) 0.109(9) Uani 1 1 d G . . H31 H 1.2717 -0.0853 0.2160 0.131 Uiso 1 1 calc R . . C32 C 1.2622(3) -0.0833(3) 0.3630(3) 0.047(4) Uani 1 1 d GD . . C33 C 1.2151(4) -0.0960(4) 0.3975(3) 0.064(5) Uani 1 1 d GD . . C34 C 1.2374(5) -0.1195(5) 0.4494(3) 0.085(7) Uani 1 1 d GD . . H34A H 1.2128 -0.1551 0.4616 0.103 Uiso 1 1 calc R . . H34B H 1.2371 -0.0868 0.4763 0.103 Uiso 1 1 calc R . . C35 C 1.3038(5) -0.1387(5) 0.4344(3) 0.108(9) Uani 1 1 d GD . . H35A H 1.3319 -0.1338 0.4645 0.130 Uiso 1 1 calc R . . H35B H 1.3048 -0.1822 0.4229 0.130 Uiso 1 1 calc R . . C36 C 1.3224(4) -0.0964(4) 0.3905(3) 0.070(6) Uani 1 1 d GD . . H36A H 1.3521 -0.1168 0.3669 0.084 Uiso 1 1 calc R . . H36B H 1.3411 -0.0580 0.4040 0.084 Uiso 1 1 calc R . . C37 C 1.1992(6) 0.1208(6) 0.2590(6) 0.074(6) Uani 1 1 d G . . C38 C 1.2503(4) 0.1625(4) 0.2680(3) 0.071(6) Uani 1 1 d G . . C39 C 1.2460(6) 0.2179(5) 0.2950(4) 0.096(8) Uani 1 1 d G . . H39 H 1.2067 0.2336 0.3045 0.116 Uiso 1 1 calc R . . C40 C 1.2990(6) 0.2502(5) 0.3080(4) 0.128(11) Uani 1 1 d G . . H40 H 1.2960 0.2880 0.3264 0.153 Uiso 1 1 calc R . . C41 C 1.3565(6) 0.2272(6) 0.2941(4) 0.124(11) Uani 1 1 d G . . H41 H 1.3927 0.2493 0.3030 0.149 Uiso 1 1 calc R . . C42 C 1.3609(4) 0.1719(6) 0.2672(5) 0.131(11) Uani 1 1 d G . . H42 H 1.4001 0.1561 0.2577 0.157 Uiso 1 1 calc R . . C43 C 1.3078(4) 0.1395(5) 0.2541(4) 0.090(7) Uani 1 1 d G . . H43 H 1.3108 0.1017 0.2357 0.108 Uiso 1 1 calc R . . C44 C 1.1902(4) 0.0814(4) 0.2217(3) 0.065(6) Uani 1 1 d GD . . C45 C 1.1422(4) 0.0398(5) 0.2193(4) 0.076(7) Uani 1 1 d GD . . C46 C 1.1410(5) -0.0021(5) 0.1728(4) 0.082(6) Uani 1 1 d GD . . H46A H 1.0994 -0.0051 0.1571 0.099 Uiso 1 1 calc R . . H46B H 1.1567 -0.0438 0.1809 0.099 Uiso 1 1 calc R . . C47 C 1.1864(6) 0.0352(5) 0.1381(3) 0.117(10) Uani 1 1 d GD . . H47A H 1.2113 0.0067 0.1165 0.141 Uiso 1 1 calc R . . H47B H 1.1632 0.0627 0.1145 0.141 Uiso 1 1 calc R . . C48 C 1.2280(5) 0.0726(5) 0.1726(3) 0.100(8) Uani 1 1 d GD . . H48A H 1.2380 0.1127 0.1563 0.120 Uiso 1 1 calc R . . H48B H 1.2667 0.0502 0.1801 0.120 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.0436(4) 0.0401(4) 0.0321(3) -0.0035(4) -0.0018(4) 0.0015(3) Er2 0.0398(6) 0.0398(6) 0.0299(7) 0.000 0.000 0.000 Er3 0.0478(5) 0.0493(5) 0.0361(4) -0.0016(4) 0.0046(4) 0.0019(4) O1 0.053(7) 0.031(6) 0.025(5) -0.002(4) -0.002(4) -0.004(5) O2 0.037(7) 0.037(7) 0.020(11) 0.000 0.000 0.000 O3 0.046(7) 0.043(7) 0.030(6) -0.009(4) 0.006(5) 0.000(5) O4 0.052(8) 0.052(8) 0.039(13) 0.000 0.000 0.000 O5 0.042(7) 0.059(8) 0.046(6) -0.014(6) 0.012(5) -0.002(6) O6 0.061(8) 0.040(7) 0.036(6) 0.012(5) -0.023(5) 0.005(6) O7 0.061(8) 0.046(7) 0.040(6) -0.007(5) -0.009(5) -0.003(6) O8 0.052(8) 0.046(7) 0.030(6) -0.001(5) -0.003(5) 0.002(5) O9 0.049(7) 0.047(7) 0.026(5) 0.001(5) 0.006(5) -0.002(6) O10 0.058(8) 0.042(7) 0.050(7) 0.017(5) -0.004(6) -0.004(6) O11 0.046(8) 0.071(9) 0.066(8) 0.007(6) 0.009(6) -0.009(6) O12 0.064(8) 0.050(8) 0.038(7) 0.009(5) 0.003(6) 0.004(6) C1 0.074(12) 0.043(10) 0.042(10) 0.003(9) -0.022(9) 0.037(9) C2 0.043(12) 0.093(17) 0.055(11) 0.011(11) -0.004(9) 0.015(11) C3 0.069(18) 0.13(2) 0.14(2) 0.001(19) 0.025(16) 0.041(16) C4 0.10(3) 0.31(5) 0.20(4) 0.14(4) 0.03(3) 0.02(3) C5 0.18(3) 0.15(3) 0.11(2) -0.07(2) 0.08(2) -0.07(2) C6 0.22(4) 0.31(6) 0.16(3) 0.07(3) 0.14(3) 0.08(4) C7 0.16(3) 0.22(4) 0.10(2) -0.02(2) -0.02(2) -0.01(3) C8 0.046(11) 0.046(11) 0.040(9) -0.010(8) -0.001(8) 0.009(8) C9 0.050(11) 0.034(10) 0.059(10) 0.007(8) -0.009(9) -0.005(9) C10 0.051(11) 0.054(11) 0.034(8) 0.018(8) -0.006(8) 0.002(9) C11 0.11(2) 0.15(3) 0.16(3) 0.01(2) 0.02(2) 0.00(2) C12 0.100(19) 0.081(17) 0.104(18) -0.001(13) 0.048(15) 0.002(14) C13 0.058(13) 0.062(14) 0.061(12) -0.018(10) -0.002(10) -0.008(10) C14 0.082(15) 0.053(13) 0.039(10) -0.018(8) -0.006(9) -0.007(10) C15 0.11(2) 0.069(18) 0.15(2) -0.027(16) -0.046(18) 0.001(16) C16 0.15(3) 0.10(2) 0.10(2) 0.004(16) -0.053(19) -0.02(2) C17 0.20(4) 0.061(18) 0.18(3) 0.043(18) -0.06(3) -0.04(2) C18 0.16(3) 0.09(2) 0.27(4) 0.02(3) -0.08(3) 0.00(2) C19 0.22(4) 0.08(2) 0.15(3) 0.028(18) -0.11(3) -0.01(2) C20 0.067(13) 0.053(12) 0.039(9) -0.016(8) -0.022(8) -0.003(9) C21 0.041(10) 0.081(14) 0.029(9) 0.020(9) 0.016(8) 0.003(9) C22 0.093(16) 0.037(11) 0.046(10) -0.004(8) -0.030(10) 0.007(10) C23 0.18(4) 0.18(4) 0.20(4) -0.03(3) -0.05(3) 0.08(3) C24 0.19(3) 0.070(18) 0.092(18) 0.012(13) -0.048(18) 0.023(17) C25 0.049(12) 0.069(13) 0.079(13) -0.006(12) 0.000(12) -0.008(9) C26 0.048(13) 0.104(19) 0.076(14) 0.023(13) 0.012(10) 0.021(12) C27 0.073(17) 0.11(2) 0.15(2) 0.069(17) 0.011(16) 0.003(14) C28 0.056(17) 0.11(2) 0.19(3) 0.05(2) 0.022(18) -0.013(14) C29 0.16(3) 0.18(4) 0.09(2) 0.02(2) 0.03(2) 0.03(3) C30 0.071(18) 0.21(4) 0.11(2) 0.08(2) 0.031(16) 0.010(19) C31 0.10(2) 0.15(3) 0.079(18) 0.025(16) 0.014(14) 0.007(16) C32 0.031(10) 0.064(12) 0.045(10) 0.008(9) 0.011(8) 0.013(8) C33 0.048(13) 0.056(13) 0.090(14) -0.002(10) -0.010(11) 0.022(10) C34 0.062(15) 0.13(2) 0.062(12) 0.034(13) 0.001(11) 0.013(14) C35 0.10(2) 0.12(2) 0.11(2) 0.024(16) -0.032(15) 0.017(16) C36 0.087(16) 0.068(14) 0.054(11) -0.004(10) -0.002(11) 0.015(11) C37 0.038(12) 0.098(18) 0.085(15) 0.049(13) 0.010(11) 0.006(12) C38 0.077(16) 0.099(18) 0.037(10) 0.027(10) 0.009(10) 0.011(14) C39 0.10(2) 0.12(2) 0.077(15) 0.026(14) 0.007(13) -0.009(16) C40 0.080(18) 0.15(2) 0.16(2) -0.02(2) 0.046(18) -0.076(17) C41 0.073(19) 0.15(3) 0.15(3) 0.07(2) 0.008(17) -0.053(19) C42 0.12(3) 0.14(3) 0.13(2) 0.05(2) -0.01(2) 0.00(2) C43 0.081(18) 0.092(19) 0.096(17) 0.032(13) 0.006(14) 0.018(14) C44 0.086(16) 0.069(14) 0.041(11) -0.011(9) 0.026(10) -0.001(11) C45 0.095(17) 0.088(17) 0.046(12) 0.021(11) 0.003(12) 0.051(13) C46 0.090(17) 0.084(17) 0.073(14) -0.007(12) 0.002(12) 0.006(13) C47 0.16(3) 0.12(2) 0.075(16) 0.035(15) 0.062(17) 0.021(19) C48 0.10(2) 0.10(2) 0.101(19) 0.034(15) 0.028(14) -0.005(15) _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 Er1 O1 2.275(10) . ? Er1 O5 2.299(11) . ? Er1 O1 2.311(10) 2_645 ? Er1 O6 2.324(9) . ? Er1 O7 2.328(11) . ? Er1 O8 2.338(10) . ? Er1 O8 2.400(10) 2_645 ? Er1 O2 2.5265(18) . ? Er1 Er1 3.5523(11) 4_665 ? Er1 Er1 3.5523(11) 2_645 ? Er1 Er2 3.6699(13) . ? Er2 O1 2.406(10) 4_665 ? Er2 O1 2.406(10) 3_755 ? Er2 O1 2.406(10) . ? Er2 O1 2.406(10) 2_645 ? Er2 O3 2.429(10) 4_665 ? Er2 O3 2.429(10) . ? Er2 O3 2.429(10) 3_755 ? Er2 O3 2.429(10) 2_645 ? Er2 Er1 3.6699(13) 4_665 ? Er2 Er1 3.6699(13) 3_755 ? Er2 Er1 3.6699(13) 2_645 ? Er3 O3 2.248(10) 4_665 ? Er3 O9 2.280(11) . ? Er3 O3 2.325(9) . ? Er3 O11 2.334(11) 4_665 ? Er3 O10 2.337(11) . ? Er3 O12 2.385(11) 4_665 ? Er3 O12 2.397(11) . ? Er3 O4 2.5182(19) . ? Er3 Er3 3.5478(11) 4_665 ? Er3 Er3 3.5478(11) 2_645 ? O1 Er1 2.311(10) 4_665 ? O1 H1 1.0000 . ? O2 Er1 2.5265(18) 3_755 ? O2 Er1 2.5265(18) 4_665 ? O2 Er1 2.5265(18) 2_645 ? O3 Er3 2.248(10) 2_645 ? O3 H3A 1.0000 . ? O4 Er3 2.5182(19) 4_665 ? O4 Er3 2.5182(19) 2_645 ? O4 Er3 2.5182(19) 3_755 ? O5 C1 1.234(17) . ? O6 C9 1.272(13) . ? O7 C13 1.253(13) . ? O8 C21 1.324(13) . ? O8 Er1 2.400(10) 4_665 ? O9 C25 1.271(19) . ? O10 C33 1.269(14) . ? O11 C37 1.322(15) . ? O11 Er3 2.334(11) 2_645 ? O12 C45 1.353(14) . ? O12 Er3 2.385(11) 2_645 ? C1 C8 1.378(18) . ? C1 C2 1.524(17) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C6 C7 1.3900 . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.3804 . ? C8 C12 1.5023 . ? C9 C10 1.4982 . ? C10 C11 1.5040 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.5006 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C20 1.370(12) . ? C13 C14 1.442(18) . ? C14 C15 1.3900 . ? C14 C19 1.3900 . ? C15 C16 1.3900 . ? C15 H15 0.9500 . ? C16 C17 1.3900 . ? C16 H16 0.9500 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 C19 1.3900 . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.3763 . ? C20 C24 1.5060 . ? C21 C22 1.4935 . ? C22 C23 1.5455 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.5041 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C32 1.357(17) . ? C25 C26 1.569(14) . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C27 C28 1.3900 . ? C27 H27 0.9500 . ? C28 C29 1.3900 . ? C28 H28 0.9500 . ? C29 C30 1.3900 . ? C29 H29 0.9500 . ? C30 C31 1.3900 . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.3826 . ? C32 C36 1.5126 . ? C33 C34 1.5060 . ? C34 C35 1.5487 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.5103 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C44 1.298(19) . ? C37 C38 1.451(19) . ? C38 C39 1.3900 . ? C38 C43 1.3900 . ? C39 C40 1.3900 . ? C39 H39 0.9500 . ? C40 C41 1.3900 . ? C40 H40 0.9500 . ? C41 C42 1.3900 . ? C41 H41 0.9500 . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.3825 . ? C44 C48 1.5170 . ? C45 C46 1.5023 . ? C46 C47 1.5567 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.5025 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? 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 O1 Er1 O5 151.9(4) . . ? O1 Er1 O1 78.6(5) . 2_645 ? O5 Er1 O1 98.3(4) . 2_645 ? O1 Er1 O6 77.9(4) . . ? O5 Er1 O6 74.3(4) . . ? O1 Er1 O6 76.0(4) 2_645 . ? O1 Er1 O7 95.9(4) . . ? O5 Er1 O7 74.6(4) . . ? O1 Er1 O7 154.2(4) 2_645 . ? O6 Er1 O7 78.2(4) . . ? O1 Er1 O8 78.7(3) . . ? O5 Er1 O8 121.4(4) . . ? O1 Er1 O8 129.7(4) 2_645 . ? O6 Er1 O8 139.9(4) . . ? O7 Er1 O8 72.4(4) . . ? O1 Er1 O8 129.3(3) . 2_645 ? O5 Er1 O8 75.6(4) . 2_645 ? O1 Er1 O8 76.7(3) 2_645 2_645 ? O6 Er1 O8 135.5(4) . 2_645 ? O7 Er1 O8 123.5(3) . 2_645 ? O8 Er1 O8 84.2(5) . 2_645 ? O1 Er1 O2 67.1(4) . . ? O5 Er1 O2 137.5(3) . . ? O1 Er1 O2 66.6(4) 2_645 . ? O6 Er1 O2 132.6(4) . . ? O7 Er1 O2 134.6(3) . . ? O8 Er1 O2 63.3(4) . . ? O8 Er1 O2 62.5(4) 2_645 . ? O1 Er1 Er1 39.6(3) . 4_665 ? O5 Er1 Er1 163.3(3) . 4_665 ? O1 Er1 Er1 96.9(2) 2_645 4_665 ? O6 Er1 Er1 116.4(3) . 4_665 ? O7 Er1 Er1 94.4(3) . 4_665 ? O8 Er1 Er1 42.1(3) . 4_665 ? O8 Er1 Er1 101.3(3) 2_645 4_665 ? O2 Er1 Er1 45.33(4) . 4_665 ? O1 Er1 Er1 97.0(2) . 2_645 ? O5 Er1 Er1 97.5(3) . 2_645 ? O1 Er1 Er1 38.9(3) 2_645 2_645 ? O6 Er1 Er1 113.3(3) . 2_645 ? O7 Er1 Er1 164.3(3) . 2_645 ? O8 Er1 Er1 101.6(3) . 2_645 ? O8 Er1 Er1 40.8(2) 2_645 2_645 ? O2 Er1 Er1 45.33(4) . 2_645 ? Er1 Er1 Er1 90.0 4_665 2_645 ? O1 Er1 Er2 39.7(2) . . ? O5 Er1 Er2 135.5(3) . . ? O1 Er1 Er2 39.9(2) 2_645 . ? O6 Er1 Er2 79.6(3) . . ? O7 Er1 Er2 133.8(3) . . ? O8 Er1 Er2 101.8(3) . . ? O8 Er1 Er2 100.5(3) 2_645 . ? O2 Er1 Er2 53.0(4) . . ? Er1 Er1 Er2 61.055(11) 4_665 . ? Er1 Er1 Er2 61.055(11) 2_645 . ? O1 Er2 O1 74.3(2) 4_665 3_755 ? O1 Er2 O1 74.3(2) 4_665 . ? O1 Er2 O1 117.3(5) 3_755 . ? O1 Er2 O1 117.3(5) 4_665 2_645 ? O1 Er2 O1 74.3(2) 3_755 2_645 ? O1 Er2 O1 74.3(2) . 2_645 ? O1 Er2 O3 75.7(3) 4_665 4_665 ? O1 Er2 O3 76.8(3) 3_755 4_665 ? O1 Er2 O3 141.1(3) . 4_665 ? O1 Er2 O3 142.8(3) 2_645 4_665 ? O1 Er2 O3 76.8(3) 4_665 . ? O1 Er2 O3 142.8(3) 3_755 . ? O1 Er2 O3 75.7(3) . . ? O1 Er2 O3 141.1(3) 2_645 . ? O3 Er2 O3 73.8(2) 4_665 . ? O1 Er2 O3 141.1(3) 4_665 3_755 ? O1 Er2 O3 75.7(3) 3_755 3_755 ? O1 Er2 O3 142.8(3) . 3_755 ? O1 Er2 O3 76.8(3) 2_645 3_755 ? O3 Er2 O3 73.8(2) 4_665 3_755 ? O3 Er2 O3 116.3(5) . 3_755 ? O1 Er2 O3 142.8(3) 4_665 2_645 ? O1 Er2 O3 141.1(3) 3_755 2_645 ? O1 Er2 O3 76.8(3) . 2_645 ? O1 Er2 O3 75.7(3) 2_645 2_645 ? O3 Er2 O3 116.3(5) 4_665 2_645 ? O3 Er2 O3 73.8(2) . 2_645 ? O3 Er2 O3 73.8(2) 3_755 2_645 ? O1 Er2 Er1 37.1(2) 4_665 4_665 ? O1 Er2 Er1 91.7(2) 3_755 4_665 ? O1 Er2 Er1 38.0(2) . 4_665 ? O1 Er2 Er1 92.2(2) 2_645 4_665 ? O3 Er2 Er1 111.6(2) 4_665 4_665 ? O3 Er2 Er1 78.7(3) . 4_665 ? O3 Er2 Er1 165.0(3) 3_755 4_665 ? O3 Er2 Er1 113.7(2) 2_645 4_665 ? O1 Er2 Er1 38.0(2) 4_665 3_755 ? O1 Er2 Er1 37.1(2) 3_755 3_755 ? O1 Er2 Er1 92.2(2) . 3_755 ? O1 Er2 Er1 91.7(2) 2_645 3_755 ? O3 Er2 Er1 78.7(3) 4_665 3_755 ? O3 Er2 Er1 113.7(2) . 3_755 ? O3 Er2 Er1 111.6(2) 3_755 3_755 ? O3 Er2 Er1 165.0(3) 2_645 3_755 ? Er1 Er2 Er1 57.89(2) 4_665 3_755 ? O1 Er2 Er1 91.7(2) 4_665 . ? O1 Er2 Er1 92.2(2) 3_755 . ? O1 Er2 Er1 37.1(2) . . ? O1 Er2 Er1 38.0(2) 2_645 . ? O3 Er2 Er1 165.0(3) 4_665 . ? O3 Er2 Er1 111.6(2) . . ? O3 Er2 Er1 113.7(2) 3_755 . ? O3 Er2 Er1 78.7(3) 2_645 . ? Er1 Er2 Er1 57.89(2) 4_665 . ? Er1 Er2 Er1 86.38(4) 3_755 . ? O1 Er2 Er1 92.2(2) 4_665 2_645 ? O1 Er2 Er1 38.0(2) 3_755 2_645 ? O1 Er2 Er1 91.7(2) . 2_645 ? O1 Er2 Er1 37.1(2) 2_645 2_645 ? O3 Er2 Er1 113.7(2) 4_665 2_645 ? O3 Er2 Er1 165.0(3) . 2_645 ? O3 Er2 Er1 78.7(3) 3_755 2_645 ? O3 Er2 Er1 111.6(2) 2_645 2_645 ? Er1 Er2 Er1 86.38(4) 4_665 2_645 ? Er1 Er2 Er1 57.89(2) 3_755 2_645 ? Er1 Er2 Er1 57.89(2) . 2_645 ? O3 Er3 O9 150.0(3) 4_665 . ? O3 Er3 O3 79.3(5) 4_665 . ? O9 Er3 O3 99.3(4) . . ? O3 Er3 O11 93.7(4) 4_665 4_665 ? O9 Er3 O11 75.0(4) . 4_665 ? O3 Er3 O11 155.1(4) . 4_665 ? O3 Er3 O10 77.6(4) 4_665 . ? O9 Er3 O10 72.9(4) . . ? O3 Er3 O10 76.9(4) . . ? O11 Er3 O10 78.3(4) 4_665 . ? O3 Er3 O12 78.9(3) 4_665 4_665 ? O9 Er3 O12 121.0(3) . 4_665 ? O3 Er3 O12 130.1(4) . 4_665 ? O11 Er3 O12 70.4(4) 4_665 4_665 ? O10 Er3 O12 139.1(4) . 4_665 ? O3 Er3 O12 130.9(4) 4_665 . ? O9 Er3 O12 76.6(4) . . ? O3 Er3 O12 77.1(3) . . ? O11 Er3 O12 123.4(4) 4_665 . ? O10 Er3 O12 135.7(4) . . ? O12 Er3 O12 84.4(6) 4_665 . ? O3 Er3 O4 66.7(4) 4_665 . ? O9 Er3 O4 140.2(3) . . ? O3 Er3 O4 65.7(4) . . ? O11 Er3 O4 133.3(4) 4_665 . ? O10 Er3 O4 131.8(5) . . ? O12 Er3 O4 64.5(4) 4_665 . ? O12 Er3 O4 64.4(4) . . ? O3 Er3 Er3 39.9(2) 4_665 4_665 ? O9 Er3 Er3 162.7(2) . 4_665 ? O3 Er3 Er3 97.1(3) . 4_665 ? O11 Er3 Er3 92.2(3) 4_665 4_665 ? O10 Er3 Er3 116.4(3) . 4_665 ? O12 Er3 Er3 42.2(3) 4_665 4_665 ? O12 Er3 Er3 102.0(3) . 4_665 ? O4 Er3 Er3 45.22(4) . 4_665 ? O3 Er3 Er3 97.4(3) 4_665 2_645 ? O9 Er3 Er3 99.6(3) . 2_645 ? O3 Er3 Er3 38.3(3) . 2_645 ? O11 Er3 Er3 165.2(3) 4_665 2_645 ? O10 Er3 Er3 113.7(3) . 2_645 ? O12 Er3 Er3 102.0(3) 4_665 2_645 ? O12 Er3 Er3 42.0(3) . 2_645 ? O4 Er3 Er3 45.22(4) . 2_645 ? Er3 Er3 Er3 90.0 4_665 2_645 ? O3 Er3 Er2 39.8(3) 4_665 . ? O9 Er3 Er2 136.1(2) . . ? O3 Er3 Er2 40.3(3) . . ? O11 Er3 Er2 132.0(3) 4_665 . ? O10 Er3 Er2 79.7(3) . . ? O12 Er3 Er2 102.2(3) 4_665 . ? O12 Er3 Er2 102.0(3) . . ? O4 Er3 Er2 52.0(4) . . ? Er3 Er3 Er2 61.202(12) 4_665 . ? Er3 Er3 Er2 61.202(12) 2_645 . ? Er1 O1 Er1 101.5(4) . 4_665 ? Er1 O1 Er2 103.2(4) . . ? Er1 O1 Er2 102.1(4) 4_665 . ? Er1 O1 H1 115.9 . . ? Er1 O1 H1 115.9 4_665 . ? Er2 O1 H1 115.9 . . ? Er1 O2 Er1 89.34(8) 3_755 4_665 ? Er1 O2 Er1 167.7(7) 3_755 . ? Er1 O2 Er1 89.34(8) 4_665 . ? Er1 O2 Er1 89.34(8) 3_755 2_645 ? Er1 O2 Er1 167.7(7) 4_665 2_645 ? Er1 O2 Er1 89.34(8) . 2_645 ? Er3 O3 Er3 101.7(4) 2_645 . ? Er3 O3 Er2 103.8(4) 2_645 . ? Er3 O3 Er2 101.5(4) . . ? Er3 O3 H3A 115.9 2_645 . ? Er3 O3 H3A 115.9 . . ? Er2 O3 H3A 115.9 . . ? Er3 O4 Er3 170.0(9) 4_665 2_645 ? Er3 O4 Er3 89.57(8) 4_665 . ? Er3 O4 Er3 89.57(8) 2_645 . ? Er3 O4 Er3 89.57(8) 4_665 3_755 ? Er3 O4 Er3 89.57(8) 2_645 3_755 ? Er3 O4 Er3 170.0(9) . 3_755 ? C1 O5 Er1 136.7(11) . . ? C9 O6 Er1 131.3(8) . . ? C13 O7 Er1 135.7(10) . . ? C21 O8 Er1 128.9(7) . . ? C21 O8 Er1 126.1(7) . 4_665 ? Er1 O8 Er1 97.1(4) . 4_665 ? C25 O9 Er3 137.7(9) . . ? C33 O10 Er3 134.1(8) . . ? C37 O11 Er3 140.4(12) . 2_645 ? C45 O12 Er3 127.5(8) . 2_645 ? C45 O12 Er3 127.0(8) . . ? Er3 O12 Er3 95.8(4) 2_645 . ? O5 C1 C8 123.6(14) . . ? O5 C1 C2 114.1(13) . . ? C8 C1 C2 122.3(11) . . ? C3 C2 C7 120.0 . . ? C3 C2 C1 117.4(6) . . ? C7 C2 C1 122.5(6) . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 120.0 . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 120.0 . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C1 C8 C9 125.1(7) . . ? C1 C8 C12 125.2(7) . . ? C9 C8 C12 109.6 . . ? O6 C9 C8 127.0(6) . . ? O6 C9 C10 119.8(6) . . ? C8 C9 C10 112.9 . . ? C9 C10 C11 101.1 . . ? C9 C10 H10A 111.6 . . ? C11 C10 H10A 111.6 . . ? C9 C10 H10B 111.6 . . ? C11 C10 H10B 111.6 . . ? H10A C10 H10B 109.4 . . ? C12 C11 C10 110.5 . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C11 C12 C8 103.0 . . ? C11 C12 H12A 111.2 . . ? C8 C12 H12A 111.2 . . ? C11 C12 H12B 111.2 . . ? C8 C12 H12B 111.2 . . ? H12A C12 H12B 109.1 . . ? O7 C13 C20 123.6(15) . . ? O7 C13 C14 112.8(10) . . ? C20 C13 C14 123.5(9) . . ? C15 C14 C19 120.0 . . ? C15 C14 C13 119.1(4) . . ? C19 C14 C13 120.9(4) . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C14 120.0 . . ? C18 C19 H19 120.0 . . ? C14 C19 H19 120.0 . . ? C13 C20 C21 124.7(7) . . ? C13 C20 C24 126.7(7) . . ? C21 C20 C24 108.6 . . ? O8 C21 C20 125.2(6) . . ? O8 C21 C22 120.5(6) . . ? C20 C21 C22 114.3 . . ? C21 C22 C23 98.9 . . ? C21 C22 H22A 112.0 . . ? C23 C22 H22A 112.0 . . ? C21 C22 H22B 112.0 . . ? C23 C22 H22B 112.0 . . ? H22A C22 H22B 109.7 . . ? C24 C23 C22 108.3 . . ? C24 C23 H23A 110.0 . . ? C22 C23 H23A 110.0 . . ? C24 C23 H23B 110.0 . . ? C22 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? C23 C24 C20 102.5 . . ? C23 C24 H24A 111.3 . . ? C20 C24 H24A 111.3 . . ? C23 C24 H24B 111.3 . . ? C20 C24 H24B 111.3 . . ? H24A C24 H24B 109.2 . . ? O9 C25 C32 124.3(12) . . ? O9 C25 C26 113.5(12) . . ? C32 C25 C26 121.9(13) . . ? C27 C26 C31 120.0 . . ? C27 C26 C25 122.0(6) . . ? C31 C26 C25 117.9(6) . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C26 120.0 . . ? C30 C31 H31 120.0 . . ? C26 C31 H31 120.0 . . ? C25 C32 C33 124.3(7) . . ? C25 C32 C36 127.6(7) . . ? C33 C32 C36 107.6 . . ? O10 C33 C32 125.5(6) . . ? O10 C33 C34 120.9(6) . . ? C32 C33 C34 113.4 . . ? C33 C34 C35 99.8 . . ? C33 C34 H34A 111.8 . . ? C35 C34 H34A 111.8 . . ? C33 C34 H34B 111.8 . . ? C35 C34 H34B 111.8 . . ? H34A C34 H34B 109.5 . . ? C36 C35 C34 105.8 . . ? C36 C35 H35A 110.6 . . ? C34 C35 H35A 110.6 . . ? C36 C35 H35B 110.6 . . ? C34 C35 H35B 110.6 . . ? H35A C35 H35B 108.7 . . ? C35 C36 C32 103.4 . . ? C35 C36 H36A 111.1 . . ? C32 C36 H36A 111.1 . . ? C35 C36 H36B 111.1 . . ? C32 C36 H36B 111.1 . . ? H36A C36 H36B 109.1 . . ? C44 C37 O11 121.1(14) . . ? C44 C37 C38 130.0(10) . . ? O11 C37 C38 108.6(13) . . ? C39 C38 C43 120.0 . . ? C39 C38 C37 124.5(5) . . ? C43 C38 C37 114.9(5) . . ? C38 C39 C40 120.0 . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C41 C40 C39 120.0 . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.0 . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C42 C43 C38 120.0 . . ? C42 C43 H43 120.0 . . ? C38 C43 H43 120.0 . . ? C37 C44 C45 125.3(6) . . ? C37 C44 C48 128.0(6) . . ? C45 C44 C48 106.7 . . ? O12 C45 C44 126.1(7) . . ? O12 C45 C46 117.0(7) . . ? C44 C45 C46 116.4 . . ? C45 C46 C47 97.4 . . ? C45 C46 H46A 112.3 . . ? C47 C46 H46A 112.3 . . ? C45 C46 H46B 112.3 . . ? C47 C46 H46B 112.3 . . ? H46A C46 H46B 109.9 . . ? C48 C47 C46 108.9 . . ? C48 C47 H47A 109.9 . . ? C46 C47 H47A 109.9 . . ? C48 C47 H47B 109.9 . . ? C46 C47 H47B 109.9 . . ? H47A C47 H47B 108.3 . . ? C47 C48 C44 103.6 . . ? C47 C48 H48A 111.0 . . ? C44 C48 H48A 111.0 . . ? C47 C48 H48B 111.0 . . ? C44 C48 H48B 111.0 . . ? H48A C48 H48B 109.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3A O6 1.00 1.84 2.776(16) 154.5 4_665 O1 H1 O10 1.00 1.84 2.785(16) 156.0 2_645 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.167 _refine_diff_density_min -2.353 _refine_diff_density_rms 0.248 # 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 -0.003 -0.001 -0.093 2129 1594 ' ' 2 0.000 0.000 0.199 7 1 ' ' 3 -0.032 0.495 0.407 2129 1594 ' ' 4 0.500 0.500 0.699 7 1 ' ' _platon_squeeze_details ; ; data_jon151ab _database_code_depnum_ccdc_archive 'CCDC 801772' #TrackingRef 'JON151AB.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H84 N8 O36 Tb4' _chemical_formula_sum 'C96 H84 N8 O36 Tb4' _chemical_formula_weight 2561.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' _symmetry_space_group_name_Hall 'P -4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 17.123(2) _cell_length_b 17.123(2) _cell_length_c 15.959(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4679.1(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 32048 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 3.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6723 _exptl_absorpt_correction_T_max 0.7906 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25666 _diffrn_reflns_av_R_equivalents 0.0853 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4126 _reflns_number_gt 3490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0820P)^2^+0.9458P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 4126 _refine_ls_number_parameters 328 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1276 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.385781(18) 0.49695(2) 0.575200(19) 0.02111(15) Uani 1 1 d . . . O1 O 0.4994(4) 0.4223(3) 0.5683(3) 0.0230(10) Uani 1 1 d D . . O2 O 0.3465(3) 0.3956(3) 0.6595(3) 0.0327(13) Uani 1 1 d . . . O3 O 0.3933(3) 0.5458(3) 0.7098(3) 0.0298(13) Uani 1 1 d . . . O4 O 0.4875(4) 0.3119(4) 0.7563(4) 0.0507(16) Uani 1 1 d . . . O5 O 0.4907(5) 0.2519(4) 0.8734(4) 0.069(2) Uani 1 1 d . . . O6 O 0.2590(3) 0.4926(4) 0.5349(3) 0.0297(12) Uani 1 1 d . . . O7 O 0.3544(3) 0.6252(3) 0.5350(3) 0.0312(13) Uani 1 1 d . . . O8 O 0.1097(3) 0.4989(5) 0.6256(4) 0.0503(16) Uani 1 1 d . . . O9 O 0.1070(4) 0.3727(4) 0.6230(5) 0.0586(19) Uani 1 1 d . . . N1 N 0.4561(4) 0.2723(4) 0.8086(5) 0.0417(18) Uani 1 1 d . . . N2 N 0.1076(4) 0.4366(5) 0.5877(5) 0.0421(19) Uani 1 1 d . . . C1 C 0.3432(5) 0.3830(5) 0.7383(5) 0.0279(18) Uani 1 1 d . . . C2 C 0.3571(5) 0.4391(5) 0.7977(5) 0.0306(18) Uani 1 1 d . . . C3 C 0.3822(4) 0.5147(4) 0.7803(5) 0.0232(16) Uani 1 1 d . . . C4 C 0.3967(7) 0.5585(5) 0.8602(5) 0.044(2) Uani 1 1 d . . . H4A H 0.3738 0.6115 0.8575 0.053 Uiso 1 1 calc R . . H4B H 0.4533 0.5630 0.8716 0.053 Uiso 1 1 calc R . . C5 C 0.3564(7) 0.5096(6) 0.9277(6) 0.055(3) Uani 1 1 d . . . H5A H 0.3874 0.5098 0.9801 0.065 Uiso 1 1 calc R . . H5B H 0.3037 0.5305 0.9399 0.065 Uiso 1 1 calc R . . C6 C 0.3509(6) 0.4280(5) 0.8926(6) 0.043(2) Uani 1 1 d . . . H6A H 0.3005 0.4034 0.9078 0.051 Uiso 1 1 calc R . . H6B H 0.3941 0.3949 0.9137 0.051 Uiso 1 1 calc R . . C7 C 0.3226(5) 0.3019(4) 0.7631(4) 0.0255(18) Uani 1 1 d . . . C8 C 0.3740(5) 0.2497(5) 0.7967(5) 0.034(2) Uani 1 1 d . . . C9 C 0.3554(6) 0.1748(5) 0.8205(5) 0.042(2) Uani 1 1 d . . . H9 H 0.3939 0.1413 0.8438 0.050 Uiso 1 1 calc R . . C10 C 0.2805(6) 0.1499(5) 0.8099(6) 0.043(2) Uani 1 1 d . . . H10 H 0.2666 0.0979 0.8241 0.052 Uiso 1 1 calc R . . C11 C 0.2242(6) 0.2008(5) 0.7780(6) 0.042(2) Uani 1 1 d . . . H11 H 0.1718 0.1838 0.7716 0.050 Uiso 1 1 calc R . . C12 C 0.2447(5) 0.2756(5) 0.7560(5) 0.034(2) Uani 1 1 d . . . H12 H 0.2058 0.3103 0.7356 0.041 Uiso 1 1 calc R . . C13 C 0.2139(4) 0.5346(5) 0.4893(5) 0.0276(18) Uani 1 1 d . . . C14 C 0.2262(4) 0.6132(5) 0.4763(5) 0.0268(18) Uani 1 1 d . . . C15 C 0.2918(5) 0.6524(5) 0.5011(5) 0.0303(19) Uani 1 1 d . . . C16 C 0.2850(5) 0.7405(4) 0.4858(6) 0.033(2) Uani 1 1 d . . . H16A H 0.2999 0.7706 0.5364 0.040 Uiso 1 1 calc R . . H16B H 0.3182 0.7572 0.4383 0.040 Uiso 1 1 calc R . . C17 C 0.1988(5) 0.7507(5) 0.4657(6) 0.039(2) Uani 1 1 d . . . H17A H 0.1914 0.7914 0.4224 0.047 Uiso 1 1 calc R . . H17B H 0.1693 0.7659 0.5166 0.047 Uiso 1 1 calc R . . C18 C 0.1705(5) 0.6702(5) 0.4331(6) 0.0368(19) Uani 1 1 d . . . H18A H 0.1156 0.6602 0.4495 0.044 Uiso 1 1 calc R . . H18B H 0.1750 0.6668 0.3714 0.044 Uiso 1 1 calc R . . C19 C 0.1473(4) 0.4901(6) 0.4534(5) 0.0312(18) Uani 1 1 d . . . C20 C 0.1020(5) 0.4377(5) 0.4958(5) 0.032(2) Uani 1 1 d . . . C21 C 0.0508(5) 0.3856(5) 0.4590(6) 0.040(2) Uani 1 1 d . . . H21 H 0.0213 0.3498 0.4917 0.049 Uiso 1 1 calc R . . C22 C 0.0441(6) 0.3877(7) 0.3741(7) 0.057(3) Uani 1 1 d . . . H22 H 0.0099 0.3520 0.3471 0.068 Uiso 1 1 calc R . . C23 C 0.0855(6) 0.4398(7) 0.3266(7) 0.058(3) Uani 1 1 d . . . H23 H 0.0789 0.4415 0.2675 0.069 Uiso 1 1 calc R . . C24 C 0.1373(5) 0.4902(7) 0.3663(5) 0.046(2) Uani 1 1 d . . . H24 H 0.1667 0.5259 0.3333 0.055 Uiso 1 1 calc R . . H1 H 0.512(6) 0.390(4) 0.610(4) 0.055 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0222(2) 0.0257(2) 0.0154(2) 0.0028(2) 0.00238(12) -0.0005(2) O1 0.036(3) 0.022(2) 0.011(2) -0.0030(18) -0.008(4) 0.002(2) O2 0.043(3) 0.032(3) 0.024(3) 0.000(3) 0.003(3) -0.004(3) O3 0.047(3) 0.023(3) 0.019(3) -0.002(2) 0.006(3) -0.006(3) O4 0.054(4) 0.048(4) 0.049(4) 0.008(3) -0.009(4) -0.014(4) O5 0.076(5) 0.073(5) 0.059(4) 0.014(4) -0.026(5) 0.011(4) O6 0.026(2) 0.040(3) 0.023(3) 0.004(3) 0.000(2) 0.005(3) O7 0.033(3) 0.030(3) 0.030(3) 0.006(2) -0.005(3) 0.002(3) O8 0.064(4) 0.053(4) 0.033(3) -0.004(4) 0.008(3) -0.022(5) O9 0.083(5) 0.054(4) 0.039(4) 0.007(4) 0.007(4) -0.017(4) N1 0.051(5) 0.041(4) 0.033(5) -0.010(4) -0.004(4) 0.003(4) N2 0.050(5) 0.042(4) 0.035(5) -0.008(4) 0.004(4) -0.008(4) C1 0.035(4) 0.033(4) 0.015(4) 0.006(3) 0.001(3) 0.000(4) C2 0.039(5) 0.034(5) 0.018(4) 0.001(4) 0.000(4) -0.004(4) C3 0.031(4) 0.028(4) 0.011(3) -0.001(3) 0.001(3) 0.003(3) C4 0.081(7) 0.029(4) 0.023(5) -0.010(4) -0.001(5) -0.002(5) C5 0.086(7) 0.055(6) 0.023(5) -0.002(7) 0.007(5) 0.000(6) C6 0.065(6) 0.043(5) 0.019(5) 0.002(4) -0.009(5) 0.006(5) C7 0.037(4) 0.026(4) 0.013(4) 0.001(3) -0.003(3) -0.004(4) C8 0.040(5) 0.041(5) 0.021(5) -0.012(4) 0.012(4) -0.007(4) C9 0.073(7) 0.032(5) 0.021(5) 0.006(4) 0.000(5) 0.001(5) C10 0.078(7) 0.029(5) 0.022(5) 0.003(4) 0.010(5) -0.011(5) C11 0.057(6) 0.042(5) 0.027(5) -0.012(4) 0.013(5) -0.026(5) C12 0.039(5) 0.044(5) 0.019(4) 0.008(4) 0.004(4) -0.008(4) C13 0.024(4) 0.038(4) 0.021(4) -0.001(4) 0.003(3) -0.006(4) C14 0.025(4) 0.042(5) 0.013(4) -0.003(4) 0.012(3) 0.001(4) C15 0.039(5) 0.044(5) 0.008(4) -0.001(4) 0.010(4) 0.010(4) C16 0.039(5) 0.028(4) 0.033(5) -0.003(4) -0.004(4) 0.004(4) C17 0.042(5) 0.043(5) 0.033(5) 0.014(4) 0.001(4) 0.009(4) C18 0.032(4) 0.050(5) 0.029(5) 0.010(4) 0.000(4) 0.003(4) C19 0.029(4) 0.041(5) 0.024(4) -0.005(4) 0.005(3) -0.004(4) C20 0.034(5) 0.038(5) 0.025(5) -0.009(4) -0.002(4) -0.005(4) C21 0.034(5) 0.049(5) 0.039(6) -0.012(4) -0.005(4) -0.008(4) C22 0.055(6) 0.064(7) 0.052(7) -0.022(6) -0.020(5) -0.013(6) C23 0.045(6) 0.100(9) 0.028(5) -0.018(6) -0.010(5) -0.008(6) C24 0.039(4) 0.065(7) 0.033(4) -0.005(6) -0.006(4) 0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O6 2.265(5) . ? Tb1 O2 2.296(5) . ? Tb1 O3 2.308(6) . ? Tb1 O1 2.329(6) . ? Tb1 O7 2.350(5) . ? Tb1 O1 2.375(4) 2_566 ? Tb1 O1 2.407(6) 3_665 ? Tb1 Tb1 3.6629(7) 4_656 ? Tb1 Tb1 3.6629(7) 2_566 ? Tb1 Tb1 3.9129(8) 3_665 ? O1 Tb1 2.375(4) 4_656 ? O1 Tb1 2.407(6) 3_665 ? O1 H1 0.898(10) . ? O2 C1 1.277(9) . ? O3 C3 1.260(9) . ? O4 N1 1.202(9) . ? O5 N1 1.242(10) . ? O6 C13 1.282(9) . ? O7 C15 1.289(10) . ? O8 N2 1.228(10) . ? O9 N2 1.231(10) . ? N1 C8 1.470(11) . ? N2 C20 1.469(11) . ? C1 C2 1.371(11) . ? C1 C7 1.486(11) . ? C2 C3 1.391(11) . ? C2 C6 1.531(12) . ? C3 C4 1.501(11) . ? C4 C5 1.528(13) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.508(14) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.364(12) . ? C7 C12 1.412(12) . ? C8 C9 1.374(12) . ? C9 C10 1.362(13) . ? C9 H9 0.9500 . ? C10 C11 1.395(14) . ? C10 H10 0.9500 . ? C11 C12 1.374(12) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.379(11) . ? C13 C19 1.487(11) . ? C14 C15 1.367(12) . ? C14 C18 1.529(11) . ? C15 C16 1.533(11) . ? C16 C17 1.521(12) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.550(13) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.366(12) . ? C19 C24 1.401(11) . ? C20 C21 1.382(11) . ? C21 C22 1.360(14) . ? C21 H21 0.9500 . ? C22 C23 1.368(15) . ? C22 H22 0.9500 . ? C23 C24 1.390(14) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Tb1 O2 82.01(19) . . ? O6 Tb1 O3 109.25(19) . . ? O2 Tb1 O3 75.23(19) . . ? O6 Tb1 O1 140.24(18) . . ? O2 Tb1 O1 81.81(18) . . ? O3 Tb1 O1 101.29(17) . . ? O6 Tb1 O7 74.6(2) . . ? O2 Tb1 O7 143.06(19) . . ? O3 Tb1 O7 85.89(19) . . ? O1 Tb1 O7 133.65(18) . . ? O6 Tb1 O1 88.84(16) . 2_566 ? O2 Tb1 O1 131.5(2) . 2_566 ? O3 Tb1 O1 150.77(19) . 2_566 ? O1 Tb1 O1 75.5(2) . 2_566 ? O7 Tb1 O1 76.8(2) . 2_566 ? O6 Tb1 O1 142.10(19) . 3_665 ? O2 Tb1 O1 134.43(18) . 3_665 ? O3 Tb1 O1 77.78(17) . 3_665 ? O1 Tb1 O1 68.32(18) . 3_665 ? O7 Tb1 O1 68.74(18) . 3_665 ? O1 Tb1 O1 74.06(18) 2_566 3_665 ? O6 Tb1 Tb1 108.81(13) . 4_656 ? O2 Tb1 Tb1 98.74(13) . 4_656 ? O3 Tb1 Tb1 140.11(14) . 4_656 ? O1 Tb1 Tb1 39.32(10) . 4_656 ? O7 Tb1 Tb1 115.58(14) . 4_656 ? O1 Tb1 Tb1 40.32(14) 2_566 4_656 ? O1 Tb1 Tb1 79.66(11) 3_665 4_656 ? O6 Tb1 Tb1 109.27(13) . 2_566 ? O2 Tb1 Tb1 161.87(13) . 2_566 ? O3 Tb1 Tb1 112.45(13) . 2_566 ? O1 Tb1 Tb1 80.56(12) . 2_566 ? O7 Tb1 Tb1 55.06(14) . 2_566 ? O1 Tb1 Tb1 38.42(14) 2_566 2_566 ? O1 Tb1 Tb1 39.69(10) 3_665 2_566 ? Tb1 Tb1 Tb1 64.569(12) 4_656 2_566 ? O6 Tb1 Tb1 163.51(11) . 3_665 ? O2 Tb1 Tb1 108.23(14) . 3_665 ? O3 Tb1 Tb1 86.23(14) . 3_665 ? O1 Tb1 Tb1 34.93(12) . 3_665 ? O7 Tb1 Tb1 101.73(13) . 3_665 ? O1 Tb1 Tb1 74.69(11) 2_566 3_665 ? O1 Tb1 Tb1 33.66(12) 3_665 3_665 ? Tb1 Tb1 Tb1 57.715(6) 4_656 3_665 ? Tb1 Tb1 Tb1 57.715(6) 2_566 3_665 ? Tb1 O1 Tb1 102.25(18) . 4_656 ? Tb1 O1 Tb1 111.41(18) . 3_665 ? Tb1 O1 Tb1 100.0(2) 4_656 3_665 ? Tb1 O1 H1 121(7) . . ? Tb1 O1 H1 123(6) 4_656 . ? Tb1 O1 H1 97(6) 3_665 . ? C1 O2 Tb1 135.9(5) . . ? C3 O3 Tb1 132.0(5) . . ? C13 O6 Tb1 136.1(5) . . ? C15 O7 Tb1 130.0(5) . . ? O4 N1 O5 121.6(8) . . ? O4 N1 C8 119.1(8) . . ? O5 N1 C8 119.2(8) . . ? O8 N2 O9 123.2(8) . . ? O8 N2 C20 118.8(8) . . ? O9 N2 C20 117.9(8) . . ? O2 C1 C2 123.6(7) . . ? O2 C1 C7 115.6(7) . . ? C2 C1 C7 120.8(7) . . ? C1 C2 C3 124.6(7) . . ? C1 C2 C6 125.8(8) . . ? C3 C2 C6 109.5(7) . . ? O3 C3 C2 128.2(7) . . ? O3 C3 C4 121.6(7) . . ? C2 C3 C4 110.3(7) . . ? C3 C4 C5 104.5(7) . . ? C3 C4 H4A 110.8 . . ? C5 C4 H4A 110.8 . . ? C3 C4 H4B 110.8 . . ? C5 C4 H4B 110.8 . . ? H4A C4 H4B 108.9 . . ? C6 C5 C4 105.9(8) . . ? C6 C5 H5A 110.6 . . ? C4 C5 H5A 110.6 . . ? C6 C5 H5B 110.6 . . ? C4 C5 H5B 110.6 . . ? H5A C5 H5B 108.7 . . ? C5 C6 C2 104.4(8) . . ? C5 C6 H6A 110.9 . . ? C2 C6 H6A 110.9 . . ? C5 C6 H6B 110.9 . . ? C2 C6 H6B 110.9 . . ? H6A C6 H6B 108.9 . . ? C8 C7 C12 115.6(7) . . ? C8 C7 C1 124.3(7) . . ? C12 C7 C1 120.0(7) . . ? C7 C8 C9 124.7(8) . . ? C7 C8 N1 119.7(8) . . ? C9 C8 N1 115.6(8) . . ? C10 C9 C8 118.4(9) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? C9 C10 C11 120.0(8) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 119.9(9) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C7 121.2(9) . . ? C11 C12 H12 119.4 . . ? C7 C12 H12 119.4 . . ? O6 C13 C14 122.7(7) . . ? O6 C13 C19 113.2(7) . . ? C14 C13 C19 124.1(8) . . ? C15 C14 C13 124.2(7) . . ? C15 C14 C18 109.3(7) . . ? C13 C14 C18 126.5(7) . . ? O7 C15 C14 128.9(7) . . ? O7 C15 C16 119.1(7) . . ? C14 C15 C16 112.1(7) . . ? C17 C16 C15 102.6(7) . . ? C17 C16 H16A 111.2 . . ? C15 C16 H16A 111.2 . . ? C17 C16 H16B 111.2 . . ? C15 C16 H16B 111.2 . . ? H16A C16 H16B 109.2 . . ? C16 C17 C18 105.9(7) . . ? C16 C17 H17A 110.6 . . ? C18 C17 H17A 110.6 . . ? C16 C17 H17B 110.6 . . ? C18 C17 H17B 110.6 . . ? H17A C17 H17B 108.7 . . ? C14 C18 C17 102.7(7) . . ? C14 C18 H18A 111.2 . . ? C17 C18 H18A 111.2 . . ? C14 C18 H18B 111.2 . . ? C17 C18 H18B 111.2 . . ? H18A C18 H18B 109.1 . . ? C20 C19 C24 115.1(9) . . ? C20 C19 C13 125.5(7) . . ? C24 C19 C13 118.4(8) . . ? C19 C20 C21 124.9(8) . . ? C19 C20 N2 117.8(7) . . ? C21 C20 N2 117.3(8) . . ? C22 C21 C20 117.4(9) . . ? C22 C21 H21 121.3 . . ? C20 C21 H21 121.3 . . ? C21 C22 C23 121.7(10) . . ? C21 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? C22 C23 C24 118.9(10) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C23 C24 C19 121.9(10) . . ? C23 C24 H24 119.0 . . ? C19 C24 H24 119.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O4 0.898(10) 2.72(5) 3.551(8) 155(9) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.398 _refine_diff_density_min -3.840 _refine_diff_density_rms 0.203 # Attachment 'jon153ab.cif' data_c:\folders\jon153\jon153ab _database_code_depnum_ccdc_archive 'CCDC 801773' #TrackingRef 'jon153ab.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H84 Er4 N8 O36' _chemical_formula_sum 'C96 H84 Er4 N8 O36' _chemical_formula_weight 2594.75 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 tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' _symmetry_space_group_name_Hall 'P -4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 17.0831(3) _cell_length_b 17.0831(3) _cell_length_c 15.9784(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4663.01(15) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 35542 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 3.658 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6099 _exptl_absorpt_correction_T_max 0.6891 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28596 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4114 _reflns_number_gt 3251 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0241P)^2^+2.5413P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(12) _refine_ls_number_reflns 4114 _refine_ls_number_parameters 328 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0564 _refine_ls_wR_factor_gt 0.0511 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Er1 Er 0.388204(10) 0.50060(2) 0.923580(11) 0.01675(7) Uani 1 1 d . . . O1 O 0.4970(3) 0.42161(16) 0.93503(17) 0.0166(6) Uani 1 1 d D . . O2 O 0.3488(2) 0.3979(2) 0.8441(2) 0.0235(9) Uani 1 1 d . . . O3 O 0.3958(2) 0.5480(2) 0.7921(2) 0.0222(9) Uani 1 1 d . . . O4 O 0.4897(3) 0.3123(2) 0.7483(3) 0.0442(12) Uani 1 1 d D . . O5 O 0.4900(3) 0.2526(3) 0.6293(3) 0.0607(14) Uani 1 1 d . . . O6 O 0.26270(18) 0.4919(3) 0.9623(2) 0.0225(8) Uani 1 1 d . . . O7 O 0.3546(2) 0.6274(2) 0.9574(2) 0.0262(10) Uani 1 1 d . . . O8 O 0.1120(2) 0.4995(4) 0.8713(2) 0.0416(9) Uani 1 1 d . . . O9 O 0.1079(3) 0.3733(3) 0.8741(3) 0.0539(13) Uani 1 1 d . . . N2 N 0.1091(3) 0.4375(3) 0.9085(3) 0.0333(13) Uani 1 1 d . . . N35 N 0.4573(3) 0.2740(3) 0.6938(4) 0.0356(13) Uani 1 1 d . . . C1 C 0.3448(3) 0.3851(3) 0.7656(4) 0.0223(13) Uani 1 1 d . . . C2 C 0.3572(3) 0.4400(3) 0.7031(4) 0.0219(14) Uani 1 1 d . . . C3 C 0.3827(3) 0.5169(3) 0.7202(3) 0.0200(16) Uani 1 1 d . . . C4 C 0.3972(4) 0.5587(4) 0.6398(4) 0.0336(16) Uani 1 1 d . . . H4A H 0.4540 0.5619 0.6278 0.040 Uiso 1 1 calc R . . H4B H 0.3752 0.6123 0.6414 0.040 Uiso 1 1 calc R . . C5 C 0.3560(4) 0.5093(5) 0.5756(4) 0.0435(17) Uani 1 1 d . . . H5A H 0.3028 0.5301 0.5648 0.052 Uiso 1 1 calc R . . H5B H 0.3856 0.5093 0.5223 0.052 Uiso 1 1 calc R . . C6 C 0.3512(4) 0.4281(4) 0.6103(4) 0.0313(15) Uani 1 1 d . . . H6A H 0.3948 0.3953 0.5893 0.038 Uiso 1 1 calc R . . H6B H 0.3009 0.4030 0.5952 0.038 Uiso 1 1 calc R . . C7 C 0.3224(3) 0.3026(3) 0.7405(3) 0.0195(13) Uani 1 1 d . . . C8 C 0.3748(3) 0.2505(3) 0.7057(4) 0.0281(14) Uani 1 1 d . . . C9 C 0.3545(4) 0.1750(3) 0.6826(4) 0.0334(15) Uani 1 1 d . . . H9 H 0.3923 0.1404 0.6594 0.040 Uiso 1 1 calc R . . C10 C 0.2791(4) 0.1516(3) 0.6939(4) 0.0330(15) Uani 1 1 d . . . H10 H 0.2642 0.0995 0.6806 0.040 Uiso 1 1 calc R . . C11 C 0.2248(4) 0.2029(4) 0.7245(4) 0.0371(17) Uani 1 1 d . . . H11 H 0.1717 0.1867 0.7292 0.044 Uiso 1 1 calc R . . C12 C 0.2455(4) 0.2778(3) 0.7488(4) 0.0272(16) Uani 1 1 d . . . H12 H 0.2071 0.3122 0.7712 0.033 Uiso 1 1 calc R . . C13 C 0.2163(3) 0.5354(3) 1.0072(3) 0.0233(13) Uani 1 1 d . . . C14 C 0.2279(3) 0.6138(3) 1.0210(3) 0.0214(13) Uani 1 1 d . . . C15 C 0.2943(3) 0.6549(3) 0.9926(3) 0.0209(13) Uani 1 1 d . . . C16 C 0.2850(3) 0.7410(3) 1.0096(4) 0.0300(17) Uani 1 1 d . . . H16A H 0.2988 0.7722 0.9595 0.036 Uiso 1 1 calc R . . H16B H 0.3188 0.7576 1.0567 0.036 Uiso 1 1 calc R . . C17 C 0.1994(3) 0.7509(3) 1.0314(4) 0.0305(14) Uani 1 1 d . . . H17A H 0.1689 0.7662 0.9813 0.037 Uiso 1 1 calc R . . H17B H 0.1927 0.7916 1.0749 0.037 Uiso 1 1 calc R . . C18 C 0.1725(3) 0.6711(3) 1.0640(4) 0.0279(14) Uani 1 1 d . . . H18A H 0.1776 0.6680 1.1257 0.033 Uiso 1 1 calc R . . H18B H 0.1175 0.6606 1.0483 0.033 Uiso 1 1 calc R . . C19 C 0.1500(3) 0.4906(4) 1.0447(3) 0.0251(14) Uani 1 1 d . . . C20 C 0.1039(3) 0.4387(3) 0.9993(4) 0.0264(14) Uani 1 1 d . . . C21 C 0.0511(3) 0.3881(4) 1.0365(4) 0.0373(16) Uani 1 1 d . . . H21 H 0.0203 0.3536 1.0034 0.045 Uiso 1 1 calc R . . C22 C 0.0440(4) 0.3886(4) 1.1220(5) 0.053(2) Uani 1 1 d . . . H22 H 0.0095 0.3529 1.1489 0.064 Uiso 1 1 calc R . . C23 C 0.0873(4) 0.4412(4) 1.1692(5) 0.054(2) Uani 1 1 d . . . H23 H 0.0810 0.4429 1.2282 0.065 Uiso 1 1 calc R . . C24 C 0.1394(3) 0.4909(6) 1.1308(3) 0.0416(18) Uani 1 1 d . . . H24 H 0.1689 0.5264 1.1640 0.050 Uiso 1 1 calc R . . H1 H 0.505(3) 0.389(2) 0.8915(17) 0.050 Uiso 1 1 d 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 Er1 0.01507(12) 0.01727(12) 0.01791(11) -0.0023(2) -0.00243(9) -0.0005(2) O1 0.0197(16) 0.0158(15) 0.0145(16) -0.0036(12) -0.005(3) 0.001(2) O2 0.030(2) 0.020(2) 0.020(2) -0.0017(17) 0.0000(18) -0.0057(18) O3 0.030(2) 0.014(2) 0.023(2) 0.0006(17) -0.0032(18) -0.0021(17) O4 0.041(3) 0.036(2) 0.056(3) -0.006(2) 0.005(3) -0.015(3) O5 0.054(3) 0.064(3) 0.064(3) -0.017(2) 0.019(3) 0.013(3) O6 0.0176(17) 0.022(2) 0.0280(18) -0.002(2) -0.0008(15) 0.002(2) O7 0.026(2) 0.020(2) 0.033(2) -0.0033(18) 0.0061(19) 0.0004(17) O8 0.056(3) 0.035(2) 0.034(2) 0.006(4) -0.0124(18) -0.016(4) O9 0.065(4) 0.044(3) 0.053(3) -0.006(3) -0.004(3) -0.011(3) N2 0.035(3) 0.029(3) 0.036(4) -0.001(3) -0.010(3) -0.010(2) N35 0.041(3) 0.021(3) 0.045(4) -0.003(3) 0.004(3) 0.004(3) C1 0.018(3) 0.024(3) 0.025(3) -0.003(3) -0.002(3) 0.001(3) C2 0.027(3) 0.022(3) 0.017(3) -0.001(3) -0.005(3) -0.002(3) C3 0.015(3) 0.031(5) 0.014(3) 0.002(3) 0.000(2) 0.005(3) C4 0.049(5) 0.025(4) 0.027(4) 0.007(3) -0.002(3) 0.006(3) C5 0.072(4) 0.040(5) 0.019(3) 0.012(5) -0.002(3) 0.004(4) C6 0.041(4) 0.032(4) 0.021(3) -0.002(3) 0.003(3) -0.003(3) C7 0.030(3) 0.019(3) 0.010(3) -0.001(2) -0.002(3) -0.004(3) C8 0.036(4) 0.027(3) 0.020(3) 0.000(3) -0.006(3) -0.005(3) C9 0.051(4) 0.025(4) 0.025(3) -0.003(3) -0.007(3) -0.001(3) C10 0.052(4) 0.020(3) 0.027(3) -0.001(3) -0.005(3) -0.014(3) C11 0.045(5) 0.042(4) 0.025(4) -0.001(3) -0.005(4) -0.023(4) C12 0.036(4) 0.025(3) 0.020(4) -0.001(3) -0.006(3) -0.010(3) C13 0.022(3) 0.033(3) 0.015(3) 0.004(3) -0.005(3) 0.001(3) C14 0.017(3) 0.027(3) 0.020(3) -0.001(3) -0.006(3) 0.007(2) C15 0.019(3) 0.025(3) 0.019(3) 0.002(3) -0.007(3) 0.000(2) C16 0.034(4) 0.026(4) 0.030(4) -0.004(3) -0.001(3) 0.001(3) C17 0.034(4) 0.028(3) 0.029(4) -0.005(3) -0.002(3) 0.013(3) C18 0.020(3) 0.036(4) 0.027(3) -0.007(3) -0.002(3) 0.007(3) C19 0.017(3) 0.029(4) 0.030(3) 0.007(4) -0.003(2) 0.004(3) C20 0.021(3) 0.027(3) 0.030(4) 0.009(3) -0.007(3) 0.000(3) C21 0.027(4) 0.037(4) 0.048(4) -0.002(3) 0.003(3) -0.010(3) C22 0.047(5) 0.062(5) 0.052(5) 0.007(4) 0.012(4) -0.020(4) C23 0.052(5) 0.075(6) 0.035(4) 0.014(4) 0.010(4) -0.013(4) C24 0.038(3) 0.061(5) 0.025(3) 0.003(5) -0.001(2) -0.015(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 Er1 O6 2.236(3) . ? Er1 O3 2.255(4) . ? Er1 O2 2.269(4) . ? Er1 O1 2.305(4) . ? Er1 O7 2.306(4) . ? Er1 O1 2.330(3) 2_567 ? Er1 O1 2.375(5) 3_665 ? Er1 Er1 3.6413(3) 2_567 ? Er1 Er1 3.6413(3) 4_657 ? Er1 Er1 3.8197(4) 3_665 ? O1 Er1 2.330(3) 4_657 ? O1 Er1 2.375(5) 3_665 ? O1 H1 0.898(10) . ? O2 C1 1.275(6) . ? O3 C3 1.285(6) . ? O4 N35 1.221(6) . ? O5 N35 1.229(6) . ? O6 C13 1.302(6) . ? O7 C15 1.263(6) . ? O8 N2 1.215(7) . ? O9 N2 1.227(6) . ? N2 C20 1.453(7) . ? N35 C8 1.478(7) . ? C1 C2 1.385(8) . ? C1 C7 1.514(7) . ? C2 C3 1.411(8) . ? C2 C6 1.501(8) . ? C3 C4 1.491(8) . ? C4 C5 1.504(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.496(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.379(7) . ? C7 C12 1.388(8) . ? C8 C9 1.387(8) . ? C9 C10 1.361(8) . ? C9 H9 0.9500 . ? C10 C11 1.366(9) . ? C10 H10 0.9500 . ? C11 C12 1.384(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.372(7) . ? C13 C19 1.494(8) . ? C14 C15 1.410(8) . ? C14 C18 1.524(7) . ? C15 C16 1.504(7) . ? C16 C17 1.513(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.530(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.387(7) . ? C19 C20 1.390(8) . ? C20 C21 1.383(8) . ? C21 C22 1.372(9) . ? C21 H21 0.9500 . ? C22 C23 1.387(10) . ? C22 H22 0.9500 . ? C23 C24 1.374(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Er1 O3 109.68(13) . . ? O6 Er1 O2 79.57(14) . . ? O3 Er1 O2 76.89(13) . . ? O6 Er1 O1 135.45(15) . . ? O3 Er1 O1 103.74(12) . . ? O2 Er1 O1 80.28(12) . . ? O6 Er1 O7 76.03(15) . . ? O3 Er1 O7 84.01(13) . . ? O2 Er1 O7 141.64(13) . . ? O1 Er1 O7 137.10(13) . . ? O6 Er1 O1 88.15(10) . 2_567 ? O3 Er1 O1 151.97(14) . 2_567 ? O2 Er1 O1 128.97(15) . 2_567 ? O1 Er1 O1 74.67(13) . 2_567 ? O7 Er1 O1 79.47(16) . 2_567 ? O6 Er1 O1 143.80(14) . 3_665 ? O3 Er1 O1 79.82(11) . 3_665 ? O2 Er1 O1 136.13(12) . 3_665 ? O1 Er1 O1 69.86(11) . 3_665 ? O7 Er1 O1 70.23(12) . 3_665 ? O1 Er1 O1 73.35(13) 2_567 3_665 ? O6 Er1 Er1 110.77(9) . 2_567 ? O3 Er1 Er1 114.02(9) . 2_567 ? O2 Er1 Er1 159.33(9) . 2_567 ? O1 Er1 Er1 80.03(8) . 2_567 ? O7 Er1 Er1 58.92(9) . 2_567 ? O1 Er1 Er1 37.97(11) 2_567 2_567 ? O1 Er1 Er1 38.86(7) 3_665 2_567 ? O6 Er1 Er1 106.24(10) . 4_657 ? O3 Er1 Er1 141.62(9) . 4_657 ? O2 Er1 Er1 97.04(9) . 4_657 ? O1 Er1 Er1 38.48(7) . 4_657 ? O7 Er1 Er1 117.91(9) . 4_657 ? O1 Er1 Er1 39.76(11) 2_567 4_657 ? O1 Er1 Er1 79.21(8) 3_665 4_657 ? Er1 Er1 Er1 63.269(6) 2_567 4_657 ? O6 Er1 Er1 163.40(8) . 3_665 ? O3 Er1 Er1 86.80(9) . 3_665 ? O2 Er1 Er1 107.02(9) . 3_665 ? O1 Er1 Er1 35.92(10) . 3_665 ? O7 Er1 Er1 104.72(9) . 3_665 ? O1 Er1 Er1 75.83(7) 2_567 3_665 ? O1 Er1 Er1 34.69(9) 3_665 3_665 ? Er1 Er1 Er1 58.366(3) 2_567 3_665 ? Er1 Er1 Er1 58.366(3) 4_657 3_665 ? Er1 O1 Er1 103.55(15) . 4_657 ? Er1 O1 Er1 109.40(11) . 3_665 ? Er1 O1 Er1 101.38(15) 4_657 3_665 ? Er1 O1 H1 115(3) . . ? Er1 O1 H1 127(3) 4_657 . ? Er1 O1 H1 99(4) 3_665 . ? C1 O2 Er1 134.4(3) . . ? C3 O3 Er1 132.4(3) . . ? C13 O6 Er1 134.3(4) . . ? C15 O7 Er1 131.0(3) . . ? O8 N2 O9 124.0(5) . . ? O8 N2 C20 118.6(5) . . ? O9 N2 C20 117.3(5) . . ? O4 N35 O5 123.5(6) . . ? O4 N35 C8 119.1(5) . . ? O5 N35 C8 117.4(6) . . ? O2 C1 C2 125.8(5) . . ? O2 C1 C7 115.7(5) . . ? C2 C1 C7 118.5(5) . . ? C1 C2 C3 122.5(5) . . ? C1 C2 C6 127.6(5) . . ? C3 C2 C6 109.8(5) . . ? O3 C3 C2 127.7(5) . . ? O3 C3 C4 122.9(5) . . ? C2 C3 C4 109.3(5) . . ? C3 C4 C5 103.9(5) . . ? C3 C4 H4A 111.0 . . ? C5 C4 H4A 111.0 . . ? C3 C4 H4B 111.0 . . ? C5 C4 H4B 111.0 . . ? H4A C4 H4B 109.0 . . ? C6 C5 C4 107.1(5) . . ? C6 C5 H5A 110.3 . . ? C4 C5 H5A 110.3 . . ? C6 C5 H5B 110.3 . . ? C4 C5 H5B 110.3 . . ? H5A C5 H5B 108.6 . . ? C5 C6 C2 103.7(5) . . ? C5 C6 H6A 111.0 . . ? C2 C6 H6A 111.0 . . ? C5 C6 H6B 111.0 . . ? C2 C6 H6B 111.0 . . ? H6A C6 H6B 109.0 . . ? C8 C7 C12 117.2(5) . . ? C8 C7 C1 122.9(5) . . ? C12 C7 C1 119.8(5) . . ? C7 C8 C9 123.1(6) . . ? C7 C8 N35 119.7(5) . . ? C9 C8 N35 117.2(5) . . ? C10 C9 C8 118.3(6) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C9 C10 C11 120.2(6) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 121.3(6) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 119.8(6) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? O6 C13 C14 123.9(5) . . ? O6 C13 C19 113.0(5) . . ? C14 C13 C19 123.0(5) . . ? C13 C14 C15 123.4(5) . . ? C13 C14 C18 127.6(5) . . ? C15 C14 C18 109.0(5) . . ? O7 C15 C14 127.9(5) . . ? O7 C15 C16 122.0(5) . . ? C14 C15 C16 110.1(5) . . ? C15 C16 C17 104.6(4) . . ? C15 C16 H16A 110.8 . . ? C17 C16 H16A 110.8 . . ? C15 C16 H16B 110.8 . . ? C17 C16 H16B 110.8 . . ? H16A C16 H16B 108.9 . . ? C16 C17 C18 105.6(5) . . ? C16 C17 H17A 110.6 . . ? C18 C17 H17A 110.6 . . ? C16 C17 H17B 110.6 . . ? C18 C17 H17B 110.6 . . ? H17A C17 H17B 108.7 . . ? C14 C18 C17 103.4(5) . . ? C14 C18 H18A 111.1 . . ? C17 C18 H18A 111.1 . . ? C14 C18 H18B 111.1 . . ? C17 C18 H18B 111.1 . . ? H18A C18 H18B 109.0 . . ? C24 C19 C20 116.5(6) . . ? C24 C19 C13 119.6(6) . . ? C20 C19 C13 123.2(5) . . ? C21 C20 C19 122.9(6) . . ? C21 C20 N2 117.4(5) . . ? C19 C20 N2 119.7(5) . . ? C22 C21 C20 118.8(6) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C23 119.9(7) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 120.2(7) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C19 121.6(7) . . ? C23 C24 H24 119.2 . . ? C19 C24 H24 119.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O4 0.898(10) 2.653(10) 3.522(5) 163(4) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.676 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.091 # Attachment '- wg3.cif' data_wg3 _database_code_depnum_ccdc_archive 'CCDC 801774' #TrackingRef '- wg3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C104 H104 Er4 O28, 0.25(C7 H8), 0.375(C7 H8)' _chemical_formula_sum 'C108.38 H111 Er4 O28' _chemical_formula_weight 2530.51 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' 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 15.585(5) _cell_length_b 17.398(4) _cell_length_c 23.610(5) _cell_angle_alpha 82.956(5) _cell_angle_beta 76.190(16) _cell_angle_gamma 86.901(24) _cell_volume 6168(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 59802 _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 25.0 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2515 _exptl_absorpt_coefficient_mu 2.757 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9469 _exptl_absorpt_correction_T_max 0.9730 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.77487 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Australian synchrotron MX1' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59802 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15564 _reflns_number_gt 12629 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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. These crystals were very poorly diffracting and this combined with the high concentration of electron density at the cluster core has meant that the ligands and the solvent molecules are poorly defined. There is clearly a large amount of thermal motion and disorder. Therefore the ligands have been modelled as best as possible to represent the structure present. The cyclopentyl ring in ligand two has been modelled as the same as in ligand one. The disordered phenyl groups in ligands two and eight have been restrained as perfect hexagons as have the toluene solvent molecules. The thermal parameters for each of these fragments have been restrained as one. The methyl group in the disordered toluene molecules could not be located and the rings were refined without hydrogen atoms. The two components of this disorder were refined as 25% and 12.5% occupancies. The second toluene molecule was refined as having an occupancy of 25%. Due to the problems mentioned previously only the Er and oxide cluster core atoms were refined anisotropically. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1303P)^2^+136.3708P] 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 15564 _refine_ls_number_parameters 498 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.1014 _refine_ls_R_factor_gt 0.0860 _refine_ls_wR_factor_ref 0.2486 _refine_ls_wR_factor_gt 0.2360 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.98664(5) 0.62210(4) 0.26260(3) 0.041 Uani 1 1 d . . . Er2 Er 0.77083(5) 0.66821(4) 0.34260(3) 0.036 Uani 1 1 d . . . Er3 Er 0.89092(7) 0.80621(5) 0.20986(4) 0.057 Uani 1 1 d . . . Er4 Er 0.93878(5) 0.80026(4) 0.34935(3) 0.033 Uani 1 1 d . . . O1 O 0.8526(8) 0.6799(6) 0.2455(5) 0.046 Uani 1 1 d . . . O2 O 0.9153(7) 0.6675(5) 0.3506(4) 0.035 Uani 1 1 d . . . O3 O 0.9980(8) 0.7558(6) 0.2580(5) 0.048 Uani 1 1 d . . . O4 O 0.8147(8) 0.7953(6) 0.3089(5) 0.042 Uani 1 1 d . . . O5 O 1.1336(8) 0.6406(7) 0.2444(5) 0.051 Uiso 1 1 d . . . C1 C 1.1952(12) 0.5962(11) 0.2575(8) 0.058 Uiso 1 1 d D . . C2 C 1.2915(14) 0.6114(14) 0.2308(11) 0.089 Uiso 1 1 d D . . H2A H 1.3063 0.6642 0.2363 0.106 Uiso 1 1 calc R . . H2B H 1.3065 0.6058 0.1883 0.106 Uiso 1 1 calc R . . C3 C 1.3404(16) 0.5501(14) 0.2640(12) 0.091 Uiso 1 1 d D . . H3A H 1.3632 0.5734 0.2936 0.110 Uiso 1 1 calc R . . H3B H 1.3909 0.5276 0.2365 0.110 Uiso 1 1 calc R . . C4 C 1.2735(16) 0.4866(15) 0.2946(13) 0.098 Uiso 1 1 d D . . H4A H 1.2810 0.4415 0.2718 0.118 Uiso 1 1 calc R . . H4B H 1.2803 0.4689 0.3348 0.118 Uiso 1 1 calc R . . C5 C 1.1857(12) 0.5267(11) 0.2958(8) 0.057 Uiso 1 1 d D . . C6 C 1.1033(10) 0.4968(10) 0.3297(7) 0.045 Uiso 1 1 d D . . O6 O 1.0300(8) 0.5342(7) 0.3321(5) 0.049 Uiso 1 1 d . . . C7 C 1.1017(10) 0.4165(9) 0.3610(7) 0.039 Uiso 1 1 d . . . C8 C 1.1024(13) 0.3538(12) 0.3292(9) 0.060 Uiso 1 1 d . . . H8 H 1.1074 0.3631 0.2881 0.072 Uiso 1 1 calc R . . C9 C 1.0960(13) 0.2779(12) 0.3564(9) 0.060 Uiso 1 1 d . . . H9 H 1.0938 0.2361 0.3344 0.072 Uiso 1 1 calc R . . C10 C 1.0927(11) 0.2639(11) 0.4155(8) 0.047 Uiso 1 1 d . . . H10 H 1.0896 0.2123 0.4342 0.056 Uiso 1 1 calc R . . C11 C 1.0940(10) 0.3259(9) 0.4485(7) 0.041 Uiso 1 1 d . . . H11 H 1.0906 0.3160 0.4894 0.049 Uiso 1 1 calc R . . C12 C 1.1001(10) 0.4024(9) 0.4207(7) 0.037 Uiso 1 1 d . . . O7 O 1.1038(7) 0.4651(7) 0.4500(5) 0.046 Uiso 1 1 d . . . C13 C 1.1013(13) 0.4533(11) 0.5103(8) 0.054 Uiso 1 1 d . . . H13A H 1.0488 0.4241 0.5310 0.081 Uiso 1 1 calc R . . H13B H 1.0990 0.5036 0.5255 0.081 Uiso 1 1 calc R . . H13C H 1.1545 0.4241 0.5164 0.081 Uiso 1 1 calc R . . O8 O 1.0094(8) 0.6734(7) 0.1626(5) 0.049 Uiso 1 1 d . . . C14 C 1.0206(15) 0.6371(12) 0.1195(9) 0.073 Uiso 1 1 d D . . C15 C 1.027(2) 0.6810(14) 0.0592(11) 0.103 Uiso 1 1 d D . . H15A H 1.0757 0.7178 0.0489 0.123 Uiso 1 1 calc R . . H15B H 0.9708 0.7096 0.0570 0.123 Uiso 1 1 calc R . . C16 C 1.044(2) 0.6161(18) 0.0191(12) 0.129 Uiso 1 1 d D . . H16A H 1.0818 0.6344 -0.0198 0.155 Uiso 1 1 calc R . . H16B H 0.9882 0.5974 0.0138 0.155 Uiso 1 1 calc R . . C17 C 1.093(3) 0.551(2) 0.0516(14) 0.188 Uiso 1 1 d D . . H17A H 1.0816 0.4992 0.0420 0.225 Uiso 1 1 calc R . . H17B H 1.1576 0.5589 0.0417 0.225 Uiso 1 1 calc R . . C18 C 1.053(2) 0.5600(14) 0.1157(11) 0.111 Uiso 1 1 d D A . C19 C 1.0583(18) 0.4972(9) 0.1613(11) 0.104 Uiso 1 1 d D . . O9 O 1.0177(8) 0.5194(7) 0.2135(5) 0.050 Uiso 1 1 d . A . C20 C 1.0726(18) 0.4312(18) 0.1547(19) 0.116 Uiso 0.50 1 d PG A 1 C21 C 1.0186(17) 0.370(2) 0.1550(18) 0.116 Uiso 0.50 1 d PG A 1 H21 H 0.9591 0.3800 0.1523 0.139 Uiso 0.50 1 calc PR A 1 C22 C 1.052(2) 0.294(2) 0.1594(16) 0.116 Uiso 0.50 1 d PG A 1 H22 H 1.0147 0.2525 0.1596 0.139 Uiso 0.50 1 calc PR A 1 C23 C 1.139(2) 0.2796(15) 0.1634(19) 0.116 Uiso 0.50 1 d PG A 1 H23 H 1.1612 0.2279 0.1664 0.139 Uiso 0.50 1 calc PR A 1 C24 C 1.1927(19) 0.3408(14) 0.1630(14) 0.116 Uiso 0.50 1 d PG A 1 H24 H 1.2522 0.3308 0.1658 0.139 Uiso 0.50 1 calc PR A 1 C25 C 1.1597(17) 0.4166(14) 0.1587(13) 0.116 Uiso 0.50 1 d PGD A 1 C26 C 1.328(2) 0.463(2) 0.122(2) 0.116 Uiso 0.50 1 d PGD A 1 H26A H 1.3448 0.4845 0.0804 0.173 Uiso 0.50 1 calc PR A 1 H26B H 1.3529 0.4099 0.1259 0.173 Uiso 0.50 1 calc PR A 1 H26C H 1.3511 0.4948 0.1457 0.173 Uiso 0.50 1 calc PR A 1 C20A C 1.1014(3) 0.4158(2) 0.1614(2) 0.074 Uiso 0.50 1 d PGD A 2 C21A C 1.0481(4) 0.3520(2) 0.1689(3) 0.074 Uiso 0.50 1 d PGD A 2 C22A C 1.0848(4) 0.2776(2) 0.1729(3) 0.074 Uiso 0.50 1 d PG A 2 H22A H 1.0484 0.2340 0.1781 0.089 Uiso 0.50 1 calc PR A 2 C23A C 1.1749(4) 0.2668(3) 0.1695(3) 0.074 Uiso 0.50 1 d PG A 2 H23A H 1.2000 0.2159 0.1723 0.089 Uiso 0.50 1 calc PR A 2 C24A C 1.2282(4) 0.3305(3) 0.1621(3) 0.074 Uiso 0.50 1 d PG A 2 H24A H 1.2897 0.3232 0.1597 0.089 Uiso 0.50 1 calc PR A 2 C25A C 1.1914(3) 0.4050(3) 0.1580(3) 0.074 Uiso 0.50 1 d PG A 2 H25A H 1.2278 0.4486 0.1529 0.089 Uiso 0.50 1 calc PR A 2 O11 O 0.8441(2) 0.54896(17) 0.31421(16) 0.044 Uiso 1 1 d G . . C27 C 0.8284(3) 0.47831(16) 0.34136(18) 0.047 Uiso 1 1 d G . . C28 C 0.8817(3) 0.40966(17) 0.3136(2) 0.058 Uiso 1 1 d G . . H28A H 0.8583 0.3949 0.2811 0.070 Uiso 1 1 calc R . . H28B H 0.9450 0.4216 0.2989 0.070 Uiso 1 1 calc R . . C29 C 0.8673(14) 0.3459(13) 0.3659(9) 0.069 Uiso 1 1 d . . . H29A H 0.9123 0.3477 0.3890 0.082 Uiso 1 1 calc R . . H29B H 0.8694 0.2939 0.3526 0.082 Uiso 1 1 calc R . . C30 C 0.7739(14) 0.3659(12) 0.4022(10) 0.065 Uiso 1 1 d . . . H30A H 0.7277 0.3416 0.3885 0.078 Uiso 1 1 calc R . . H30B H 0.7681 0.3484 0.4445 0.078 Uiso 1 1 calc R . . C31 C 0.7672(11) 0.4541(10) 0.3914(7) 0.044 Uiso 1 1 d . . . C32 C 0.7139(10) 0.5050(9) 0.4269(7) 0.035 Uiso 1 1 d . . . O12 O 0.7216(7) 0.5787(6) 0.4181(5) 0.038 Uiso 1 1 d . . . C33 C 0.6499(3) 0.4755(2) 0.48456(18) 0.042 Uiso 1 1 d G . . C34 C 0.6498(3) 0.5086(2) 0.53366(17) 0.051 Uiso 1 1 d G . . H34 H 0.6913 0.5476 0.5312 0.062 Uiso 1 1 calc R . . C35 C 0.5919(13) 0.4881(12) 0.5875(9) 0.064 Uiso 1 1 d . . . H35 H 0.5945 0.5100 0.6219 0.077 Uiso 1 1 calc R . . C36 C 0.5295(15) 0.4328(13) 0.5877(10) 0.073 Uiso 1 1 d . . . H36 H 0.4885 0.4172 0.6236 0.088 Uiso 1 1 calc R . . C37 C 0.5253(14) 0.4008(12) 0.5389(9) 0.062 Uiso 1 1 d . . . H37 H 0.4813 0.3640 0.5414 0.074 Uiso 1 1 calc R . . C38 C 0.5855(3) 0.4212(2) 0.4840(2) 0.053 Uiso 1 1 d G . . O13 O 0.5828(3) 0.3946(2) 0.4339(2) 0.062 Uiso 1 1 d G . . C39 C 0.5214(4) 0.3324(2) 0.4347(3) 0.082 Uiso 1 1 d G . . H39A H 0.5460 0.2825 0.4485 0.123 Uiso 1 1 calc R . . H39B H 0.5133 0.3308 0.3950 0.123 Uiso 1 1 calc R . . H39C H 0.4643 0.3428 0.4612 0.123 Uiso 1 1 calc R . . O14 O 0.6695(8) 0.6400(8) 0.2906(6) 0.058 Uiso 1 1 d . . . C40 C 0.6018(12) 0.6817(11) 0.2813(8) 0.054 Uiso 1 1 d . . . C41 C 0.5635(3) 0.6710(3) 0.2288(2) 0.090 Uiso 1 1 d G . . H41A H 0.5463 0.6170 0.2291 0.108 Uiso 1 1 calc R . . H41B H 0.6040 0.6884 0.1908 0.108 Uiso 1 1 calc R . . C42 C 0.482(2) 0.7271(17) 0.2442(14) 0.104 Uiso 1 1 d . . . H42A H 0.4707 0.7547 0.2072 0.125 Uiso 1 1 calc R . . H42B H 0.4291 0.6959 0.2634 0.125 Uiso 1 1 calc R . . C43 C 0.4905(16) 0.7837(15) 0.2820(11) 0.081 Uiso 1 1 d . . . H43A H 0.4347 0.7914 0.3115 0.098 Uiso 1 1 calc R . . H43B H 0.5093 0.8342 0.2593 0.098 Uiso 1 1 calc R . . C44 C 0.5625(12) 0.7455(11) 0.3107(8) 0.053 Uiso 1 1 d . . . C45 C 0.5833(11) 0.7674(10) 0.3596(8) 0.047 Uiso 1 1 d . . . O15 O 0.64624(18) 0.7381(2) 0.37992(15) 0.047 Uiso 1 1 d G . . C46 C 0.53224(19) 0.8313(2) 0.38874(19) 0.056 Uiso 1 1 d G . . C47 C 0.44802(19) 0.8172(3) 0.4263(2) 0.077 Uiso 1 1 d G . . H47 H 0.4214 0.7684 0.4298 0.092 Uiso 1 1 calc R . . C48 C 0.403(2) 0.8787(18) 0.4595(13) 0.105 Uiso 1 1 d . . . H48 H 0.3460 0.8724 0.4850 0.125 Uiso 1 1 calc R . . C49 C 0.448(2) 0.946(2) 0.4516(15) 0.118 Uiso 1 1 d . . . H49 H 0.4161 0.9875 0.4707 0.142 Uiso 1 1 calc R . . C50 C 0.5326(2) 0.9615(2) 0.4194(2) 0.095 Uiso 1 1 d G . . H50 H 0.5620 1.0074 0.4210 0.114 Uiso 1 1 calc R . . C51 C 0.5734(16) 0.9010(14) 0.3826(11) 0.078 Uiso 1 1 d . . . O16 O 0.6565(10) 0.9071(9) 0.3490(7) 0.077 Uiso 1 1 d . . . C52 C 0.702(2) 0.9802(19) 0.3386(15) 0.116 Uiso 1 1 d . . . H52A H 0.7021 1.0050 0.2990 0.175 Uiso 1 1 calc R . . H52B H 0.7631 0.9705 0.3424 0.175 Uiso 1 1 calc R . . H52C H 0.6716 1.0145 0.3676 0.175 Uiso 1 1 calc R . . O17 O 0.7739(10) 0.8921(9) 0.2026(7) 0.075 Uiso 1 1 d . . . C53 C 0.7117(3) 0.8933(2) 0.17560(16) 0.071 Uiso 1 1 d G . . C54 C 0.6410(3) 0.9512(2) 0.18678(19) 0.091 Uiso 1 1 d G . . H54A H 0.6635 1.0044 0.1801 0.109 Uiso 1 1 calc R . . H54B H 0.6028 0.9417 0.2269 0.109 Uiso 1 1 calc R . . C55 C 0.594(3) 0.935(2) 0.1401(17) 0.135 Uiso 1 1 d . . . H55A H 0.5298 0.9355 0.1572 0.162 Uiso 1 1 calc R . . H55B H 0.6063 0.9780 0.1077 0.162 Uiso 1 1 calc R . . C56 C 0.619(2) 0.8659(18) 0.1171(14) 0.108 Uiso 1 1 d . . . H56A H 0.6284 0.8724 0.0738 0.130 Uiso 1 1 calc R . . H56B H 0.5740 0.8260 0.1340 0.130 Uiso 1 1 calc R . . C57 C 0.7049(16) 0.8453(15) 0.1358(11) 0.080 Uiso 1 1 d . . . C58 C 0.7616(3) 0.7891(3) 0.11948(14) 0.082 Uiso 1 1 d G . . O18 O 0.8366(3) 0.7696(2) 0.13796(13) 0.078 Uiso 1 1 d G . . C59 C 0.7497(3) 0.7280(3) 0.08077(15) 0.093 Uiso 1 1 d G . . C60 C 0.7403(4) 0.7562(3) 0.02189(16) 0.128 Uiso 1 1 d G . . H60 H 0.7375 0.8099 0.0087 0.154 Uiso 1 1 calc R . . C61 C 0.735(3) 0.698(2) -0.0152(18) 0.144 Uiso 1 1 d . . . H61 H 0.7183 0.7147 -0.0508 0.173 Uiso 1 1 calc R . . C62 C 0.7512(4) 0.6273(4) -0.00576(18) 0.162 Uiso 1 1 d G . . H62 H 0.7557 0.5965 -0.0370 0.194 Uiso 1 1 calc R . . C63 C 0.764(3) 0.587(3) 0.053(2) 0.165 Uiso 1 1 d . . . H63 H 0.7694 0.5324 0.0623 0.199 Uiso 1 1 calc R . . C64 C 0.767(2) 0.644(2) 0.0929(15) 0.114 Uiso 1 1 d . . . O19 O 0.7832(16) 0.6196(15) 0.1500(11) 0.139 Uiso 1 1 d . . . C65 C 0.800(3) 0.530(2) 0.1688(18) 0.156 Uiso 1 1 d . . . H65A H 0.7574 0.4999 0.1567 0.234 Uiso 1 1 calc R . . H65B H 0.7915 0.5213 0.2115 0.234 Uiso 1 1 calc R . . H65C H 0.8600 0.5150 0.1497 0.234 Uiso 1 1 calc R . . O20 O 0.9334(2) 0.90628(17) 0.25646(14) 0.051 Uiso 1 1 d G . . C66 C 0.9886(2) 0.96067(18) 0.23644(15) 0.046 Uiso 1 1 d G . . C67 C 1.0078(3) 1.01766(19) 0.27338(17) 0.062 Uiso 1 1 d G . . H67A H 1.0145 0.9921 0.3120 0.075 Uiso 1 1 calc R . . H67B H 0.9607 1.0584 0.2796 0.075 Uiso 1 1 calc R . . C68 C 1.0970(14) 1.0517(13) 0.2358(9) 0.069 Uiso 1 1 d . . . H68A H 1.1017 1.1063 0.2423 0.083 Uiso 1 1 calc R . . H68B H 1.1478 1.0214 0.2461 0.083 Uiso 1 1 calc R . . C69 C 1.0949(16) 1.0461(14) 0.1716(10) 0.078 Uiso 1 1 d . . . H69A H 1.0672 1.0931 0.1546 0.093 Uiso 1 1 calc R . . H69B H 1.1550 1.0381 0.1471 0.093 Uiso 1 1 calc R . . C70 C 1.0399(3) 0.9768(2) 0.17725(16) 0.054 Uiso 1 1 d G . . C71 C 1.0342(3) 0.9300(2) 0.13118(14) 0.053 Uiso 1 1 d G . . O21 O 0.9909(3) 0.8698(2) 0.13894(13) 0.061 Uiso 1 1 d G . . C72 C 1.0915(3) 0.9503(3) 0.07013(15) 0.072 Uiso 1 1 d G . . C73 C 1.1436(3) 0.8909(3) 0.04901(15) 0.104 Uiso 1 1 d G . . H73 H 1.1470 0.8427 0.0721 0.125 Uiso 1 1 calc R . . C74 C 1.1957(4) 0.9057(3) -0.01298(16) 0.147 Uiso 1 1 d G . . H74 H 1.2324 0.8663 -0.0316 0.176 Uiso 1 1 calc R . . C75 C 1.189(3) 0.976(3) -0.041(2) 0.169 Uiso 1 1 d . . . H75 H 1.2288 0.9853 -0.0786 0.203 Uiso 1 1 calc R . . C76 C 1.132(2) 1.040(2) -0.0247(16) 0.130 Uiso 1 1 d . . . H76 H 1.1247 1.0856 -0.0502 0.155 Uiso 1 1 calc R . . C77 C 1.0846(17) 1.0261(15) 0.0384(11) 0.083 Uiso 1 1 d . . . O22 O 1.0309(11) 1.0764(10) 0.0604(8) 0.089 Uiso 1 1 d . . . C78 C 1.0225(4) 1.1553(3) 0.0298(2) 0.129 Uiso 1 1 d G . . H78A H 1.0574 1.1912 0.0435 0.194 Uiso 1 1 calc R . . H78B H 0.9603 1.1725 0.0383 0.194 Uiso 1 1 calc R . . H78C H 1.0444 1.1543 -0.0126 0.194 Uiso 1 1 calc R . . O23 O 0.8133(7) 0.7544(6) 0.4244(4) 0.035 Uiso 1 1 d . . . C79 C 0.7693(10) 0.7893(9) 0.4684(7) 0.036 Uiso 1 1 d . . . C80 C 0.6888(11) 0.7502(10) 0.5106(7) 0.043 Uiso 1 1 d . . . H80A H 0.7068 0.7098 0.5391 0.052 Uiso 1 1 calc R . . H80B H 0.6513 0.7270 0.4890 0.052 Uiso 1 1 calc R . . C81 C 0.6412(13) 0.8191(11) 0.5409(9) 0.056 Uiso 1 1 d . . . H81A H 0.5986 0.8448 0.5191 0.067 Uiso 1 1 calc R . . H81B H 0.6090 0.8018 0.5816 0.067 Uiso 1 1 calc R . . C82 C 0.7149(11) 0.8743(10) 0.5407(8) 0.047 Uiso 1 1 d . . . H82A H 0.7403 0.8607 0.5754 0.056 Uiso 1 1 calc R . . H82B H 0.6928 0.9287 0.5401 0.056 Uiso 1 1 calc R . . C83 C 0.7836(3) 0.8616(2) 0.48348(13) 0.036 Uiso 1 1 d G . . C84 C 0.8438(3) 0.9152(2) 0.44861(14) 0.037 Uiso 1 1 d G . . O24 O 0.8934(2) 0.90090(18) 0.40027(14) 0.041 Uiso 1 1 d G . . C85 C 0.8516(3) 0.9947(2) 0.46697(16) 0.041 Uiso 1 1 d G . . C86 C 0.8490(3) 1.05682(19) 0.42315(18) 0.052 Uiso 1 1 d G . . H86 H 0.8380 1.0486 0.3865 0.063 Uiso 1 1 calc R . . C87 C 0.8635(3) 1.1331(2) 0.4358(2) 0.064 Uiso 1 1 d G . . H87 H 0.8570 1.1768 0.4086 0.076 Uiso 1 1 calc R . . C88 C 0.8865(14) 1.1437(13) 0.4867(9) 0.068 Uiso 1 1 d . . . H88 H 0.9010 1.1937 0.4933 0.081 Uiso 1 1 calc R . . C89 C 0.8887(13) 1.0805(11) 0.5288(9) 0.059 Uiso 1 1 d . . . H89 H 0.9010 1.0881 0.5652 0.071 Uiso 1 1 calc R . . C90 C 0.8729(12) 1.0069(10) 0.5179(8) 0.048 Uiso 1 1 d . . . O25 O 0.8808(8) 0.9419(7) 0.5561(5) 0.052 Uiso 1 1 d . . . C91 C 0.9110(4) 0.9525(3) 0.60763(17) 0.064 Uiso 1 1 d G . . H91A H 0.9651 0.9825 0.5961 0.096 Uiso 1 1 calc R . . H91B H 0.9232 0.9019 0.6277 0.096 Uiso 1 1 calc R . . H91C H 0.8652 0.9804 0.6341 0.096 Uiso 1 1 calc R . . O26 O 1.0149(7) 0.7361(6) 0.4135(5) 0.044 Uiso 1 1 d . . . C92 C 1.0976(10) 0.7238(9) 0.4089(7) 0.039 Uiso 1 1 d . . . C93 C 1.1339(12) 0.6613(11) 0.4455(8) 0.051 Uiso 1 1 d . . . H93A H 1.1242 0.6096 0.4351 0.062 Uiso 1 1 calc R . . H93B H 1.1076 0.6637 0.4878 0.062 Uiso 1 1 calc R . . C94 C 1.2330(16) 0.6803(15) 0.4294(11) 0.086 Uiso 1 1 d . . . H94A H 1.2477 0.7053 0.4613 0.103 Uiso 1 1 calc R . . H94B H 1.2692 0.6319 0.4247 0.103 Uiso 1 1 calc R . . C95 C 1.2531(16) 0.7322(14) 0.3746(11) 0.079 Uiso 1 1 d . . . H95A H 1.2810 0.7031 0.3412 0.094 Uiso 1 1 calc R . . H95B H 1.2936 0.7730 0.3770 0.094 Uiso 1 1 calc R . . C96 C 1.1643(2) 0.7674(2) 0.3677(2) 0.051 Uiso 1 1 d G B . C97 C 1.15386(19) 0.8278(2) 0.32568(19) 0.056 Uiso 1 1 d GD . . O27 O 1.0750(2) 0.8538(2) 0.32221(16) 0.057 Uiso 1 1 d G B . C98 C 1.2231(13) 0.8585(14) 0.2724(7) 0.035 Uiso 0.48 1 d PGD B 1 C99 C 1.2851(16) 0.9078(15) 0.2808(8) 0.059 Uiso 0.48 1 d PG B 1 C100 C 1.3481(16) 0.9403(17) 0.2330(12) 0.066 Uiso 0.48 1 d PG B 1 H100 H 1.3905 0.9740 0.2388 0.079 Uiso 0.48 1 calc PR B 1 C101 C 1.3492(19) 0.924(2) 0.1768(9) 0.104 Uiso 0.48 1 d PG B 1 H101 H 1.3922 0.9458 0.1441 0.125 Uiso 0.48 1 calc PR B 1 C102 C 1.287(2) 0.874(2) 0.1683(6) 0.097 Uiso 0.48 1 d PG B 1 H102 H 1.2878 0.8628 0.1299 0.117 Uiso 0.48 1 calc PR B 1 C103 C 1.2241(17) 0.8417(16) 0.2161(9) 0.069 Uiso 0.48 1 d PG B 1 H103 H 1.1818 0.8080 0.2103 0.082 Uiso 0.48 1 calc PR B 1 O28 O 1.274(3) 0.922(3) 0.3396(17) 0.093 Uiso 0.48 1 d P B 1 C104 C 1.343(3) 0.980(3) 0.342(2) 0.076 Uiso 0.48 1 d P B 1 H10A H 1.4000 0.9654 0.3175 0.113 Uiso 0.48 1 calc PR B 1 H10B H 1.3481 0.9785 0.3829 0.113 Uiso 0.48 1 calc PR B 1 H10C H 1.3247 1.0317 0.3280 0.113 Uiso 0.48 1 calc PR B 1 C98A C 1.2327(10) 0.8759(11) 0.3009(6) 0.043 Uiso 0.52 1 d PGD B 2 C99A C 1.2783(12) 0.9229(12) 0.3266(7) 0.030 Uiso 0.52 1 d PG B 2 H99A H 1.2621 0.9250 0.3679 0.035 Uiso 0.52 1 calc PR B 2 C10A C 1.3476(13) 0.9668(13) 0.2920(9) 0.073 Uiso 0.52 1 d PG B 2 H10D H 1.3788 0.9989 0.3096 0.088 Uiso 0.52 1 calc PR B 2 C11A C 1.3713(16) 0.9637(16) 0.2317(8) 0.094 Uiso 0.52 1 d PG B 2 H11A H 1.4187 0.9937 0.2081 0.112 Uiso 0.52 1 calc PR B 2 C12A C 1.3257(14) 0.9167(13) 0.2060(6) 0.077 Uiso 0.52 1 d PG B 2 H12A H 1.3419 0.9146 0.1648 0.092 Uiso 0.52 1 calc PR B 2 C13A C 1.2564(8) 0.8729(8) 0.2406(6) 0.053 Uiso 0.52 1 d PG B 2 O28A O 1.2121(12) 0.8221(11) 0.2145(8) 0.063 Uiso 0.52 1 d PG B 2 C14A C 1.2240(18) 0.8056(16) 0.1589(9) 0.093 Uiso 0.52 1 d PG B 2 H14A H 1.2305 0.8539 0.1322 0.139 Uiso 0.52 1 calc PR B 2 H14B H 1.1728 0.7781 0.1551 0.139 Uiso 0.52 1 calc PR B 2 H14C H 1.2774 0.7730 0.1488 0.139 Uiso 0.52 1 calc PR B 2 C300 C 0.748(3) 1.154(3) 0.2333(17) 0.106 Uiso 0.25 1 d PGD . . C301 C 0.766(3) 1.169(3) 0.2857(19) 0.054 Uiso 0.25 1 d PGD . . H301 H 0.8257 1.1711 0.2887 0.065 Uiso 0.25 1 calc PR . . C302 C 0.697(4) 1.181(3) 0.3337(18) 0.065 Uiso 0.25 1 d PG . . H302 H 0.7097 1.1911 0.3695 0.078 Uiso 0.25 1 calc PR . . C303 C 0.610(3) 1.178(4) 0.329(2) 0.115 Uiso 0.25 1 d PG . . H303 H 0.5631 1.1860 0.3620 0.138 Uiso 0.25 1 calc PR . . C304 C 0.592(3) 1.163(4) 0.277(3) 0.099 Uiso 0.25 1 d PG . . H304 H 0.5325 1.1609 0.2738 0.119 Uiso 0.25 1 calc PR . . C305 C 0.661(3) 1.151(4) 0.229(2) 0.098 Uiso 0.25 1 d PGD . . H305 H 0.6486 1.1409 0.1931 0.118 Uiso 0.25 1 calc PR . . C306 C 0.825(4) 1.120(4) 0.193(2) 0.064 Uiso 0.25 1 d PGD . . H1 H 0.8748 1.1130 0.2118 0.096 Uiso 0.25 1 calc PR . . H2 H 0.8411 1.1547 0.1565 0.096 Uiso 0.25 1 calc PR . . H30C H 0.8089 1.0696 0.1845 0.096 Uiso 0.25 1 calc PR . . C307 C 1.331(11) 0.208(13) 0.305(9) 0.137 Uiso 0.13 1 d PG C 1 C308 C 1.365(14) 0.273(13) 0.320(7) 0.137 Uiso 0.13 1 d PG C 1 C309 C 1.438(14) 0.308(10) 0.282(10) 0.137 Uiso 0.13 1 d PG C 1 C310 C 1.477(11) 0.279(12) 0.230(9) 0.137 Uiso 0.13 1 d PG C 1 C311 C 1.442(14) 0.215(13) 0.215(7) 0.137 Uiso 0.13 1 d PG C 1 C312 C 1.369(14) 0.179(10) 0.253(10) 0.137 Uiso 0.13 1 d PG C 1 O10A O 0.9661(10) 0.3702(16) 0.1554(13) 0.074 Uiso 0.50 1 d PD A 2 C26A C 0.880(2) 0.322(2) 0.160(2) 0.074 Uiso 0.50 1 d PD A 2 H26D H 0.8504 0.3103 0.2017 0.111 Uiso 0.50 1 calc PR A 2 H26E H 0.8976 0.2737 0.1427 0.111 Uiso 0.50 1 calc PR A 2 H26F H 0.8405 0.3526 0.1394 0.111 Uiso 0.50 1 calc PR A 2 O10 O 1.236(2) 0.4609(16) 0.1403(18) 0.116 Uiso 0.50 1 d PD A 1 C407 C 1.311(4) 0.191(4) 0.274(3) 0.086 Uiso 0.25 1 d PG D 2 C408 C 1.349(4) 0.254(4) 0.289(2) 0.086 Uiso 0.25 1 d PG D 2 C409 C 1.418(4) 0.293(3) 0.248(3) 0.086 Uiso 0.25 1 d PG D 2 C410 C 1.447(4) 0.269(4) 0.193(3) 0.086 Uiso 0.25 1 d PG D 2 C411 C 1.409(4) 0.206(4) 0.178(2) 0.086 Uiso 0.25 1 d PG D 2 C412 C 1.341(4) 0.168(3) 0.218(3) 0.086 Uiso 0.25 1 d PG D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.058 0.020 0.038 0.005 0.002 -0.003 Er2 0.045 0.022 0.039 0.008 -0.008 -0.005 Er3 0.098 0.037 0.035 0.019 -0.022 -0.024 Er4 0.041 0.019 0.037 0.006 -0.007 -0.006 O1 0.060 0.034 0.039 0.005 -0.002 -0.011 O2 0.043 0.016 0.038 0.009 -0.003 -0.003 O3 0.071 0.026 0.038 0.008 0.004 -0.005 O4 0.059 0.029 0.040 0.014 -0.020 -0.012 _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 Er1 O9 2.218(12) . ? Er1 O5 2.260(12) . ? Er1 O6 2.300(12) . ? Er1 O2 2.319(10) . ? Er1 O3 2.330(10) . ? Er1 O1 2.369(12) . ? Er1 O8 2.370(12) . ? Er1 O11 2.583(4) . ? Er1 Er2 3.5455(15) . ? Er1 Er3 3.6644(16) . ? Er1 Er4 3.8648(18) . ? Er2 O12 2.234(11) . ? Er2 O15 2.283(3) . ? Er2 O2 2.302(11) . ? Er2 O14 2.324(13) . ? Er2 O1 2.333(11) . ? Er2 O4 2.337(10) . ? Er2 O11 2.403(3) . ? Er2 O23 2.801(10) . ? Er2 Er4 3.6186(14) . ? Er2 Er3 3.864(2) . ? Er3 O21 2.223(3) . ? Er3 O18 2.239(3) . ? Er3 O1 2.311(11) . ? Er3 O3 2.313(13) . ? Er3 O17 2.319(15) . ? Er3 O4 2.346(11) . ? Er3 O20 2.371(3) . ? Er3 Er4 3.5347(13) . ? Er4 O24 2.233(3) . ? Er4 O27 2.281(3) . ? Er4 O26 2.291(11) . ? Er4 O3 2.341(11) . ? Er4 O2 2.353(9) . ? Er4 O4 2.362(11) . ? Er4 O23 2.402(10) . ? Er4 O20 2.702(3) . ? O5 C1 1.27(2) . ? C1 C5 1.41(2) . ? C1 C2 1.51(2) . ? C2 C3 1.53(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.55(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.50(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.43(2) . ? C6 O6 1.276(19) . ? C6 C7 1.50(2) . ? C7 C8 1.40(3) . ? C7 C12 1.40(2) . ? C8 C9 1.39(3) . ? C8 H8 0.9500 . ? C9 C10 1.38(3) . ? C9 H9 0.9500 . ? C10 C11 1.41(2) . ? C10 H10 0.9500 . ? C11 C12 1.41(2) . ? C11 H11 0.9500 . ? C12 O7 1.373(19) . ? O7 C13 1.40(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? O8 C14 1.23(2) . ? C14 C18 1.41(2) . ? C14 C15 1.52(3) . ? C15 C16 1.53(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.56(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.52(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.45(2) . ? C19 C20 1.18(3) . ? C19 O9 1.34(3) . ? C19 C20A 1.534(10) . ? C20 C21 1.3900 . ? C20 C25 1.3900 . ? C21 C22 1.3900 . ? C21 H21 0.9500 . ? C22 C23 1.3900 . ? C22 H22 0.9500 . ? C23 C24 1.3900 . ? C23 H23 0.9500 . ? C24 C25 1.3900 . ? C24 H24 0.9500 . ? C25 O10 1.401(5) . ? C26 O10 1.400(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C20A C21A 1.3900 . ? C20A C25A 1.3900 . ? C21A C22A 1.3900 . ? C21A O10A 1.400(5) . ? C22A C23A 1.3900 . ? C22A H22A 0.9500 . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? O11 C27 1.3213 . ? C27 C31 1.366(17) . ? C27 C28 1.5394 . ? C28 C29 1.54(2) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.55(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.53(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.40(2) . ? C32 O12 1.280(18) . ? C32 C33 1.533(16) . ? C33 C34 1.3561 . ? C33 C38 1.4180 . ? C34 C35 1.39(2) . ? C34 H34 0.9500 . ? C35 C36 1.40(3) . ? C35 H35 0.9500 . ? C36 C37 1.36(3) . ? C36 H36 0.9500 . ? C37 C38 1.42(2) . ? C37 H37 0.9500 . ? C38 O13 1.3309 . ? O13 C39 1.4787 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? O14 C40 1.29(2) . ? C40 C44 1.42(3) . ? C40 C41 1.53(2) . ? C41 C42 1.56(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.44(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.53(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.37(3) . ? C45 O15 1.251(17) . ? C45 C46 1.475(17) . ? C46 C51 1.38(3) . ? C46 C47 1.4126 . ? C47 C48 1.45(3) . ? C47 H47 0.9500 . ? C48 C49 1.36(4) . ? C48 H48 0.9500 . ? C49 C50 1.38(3) . ? C49 H49 0.9500 . ? C50 C51 1.47(2) . ? C50 H50 0.9500 . ? C51 O16 1.35(3) . ? O16 C52 1.46(3) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? O17 C53 1.279(15) . ? C53 C57 1.36(3) . ? C53 C54 1.4518 . ? C54 C55 1.52(4) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.38(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.52(4) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.31(2) . ? C58 O18 1.3552 . ? C58 C59 1.5295 . ? C59 C60 1.4547 . ? C59 C64 1.48(3) . ? C60 C61 1.44(4) . ? C60 H60 0.9500 . ? C61 C62 1.24(4) . ? C61 H61 0.9500 . ? C62 C63 1.53(5) . ? C62 H62 0.9500 . ? C63 C64 1.45(5) . ? C63 H63 0.9500 . ? C64 O19 1.44(4) . ? O19 C65 1.58(4) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? O20 C66 1.2823 . ? C66 C70 1.4370 . ? C66 C67 1.4839 . ? C67 C68 1.56(2) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.54(3) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.49(2) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.4573 . ? C71 O21 1.2488 . ? C71 C72 1.5144 . ? C72 C73 1.3475 . ? C72 C77 1.45(3) . ? C73 C74 1.4934 . ? C73 H73 0.9500 . ? C74 C75 1.34(5) . ? C74 H74 0.9500 . ? C75 C76 1.42(5) . ? C75 H75 0.9500 . ? C76 C77 1.49(4) . ? C76 H76 0.9500 . ? C77 O22 1.25(3) . ? O22 C78 1.486(18) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? O23 C79 1.299(18) . ? C79 C83 1.391(16) . ? C79 C80 1.54(2) . ? C80 C81 1.54(2) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 C82 1.53(3) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.541(17) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.4025 . ? C84 O24 1.2603 . ? C84 C85 1.5198 . ? C85 C90 1.364(18) . ? C85 C86 1.4071 . ? C86 C87 1.4375 . ? C86 H86 0.9500 . ? C87 C88 1.37(2) . ? C87 H87 0.9500 . ? C88 C89 1.39(3) . ? C88 H88 0.9500 . ? C89 C90 1.38(3) . ? C89 H89 0.9500 . ? C90 O25 1.38(2) . ? O25 C91 1.440(13) . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? O26 C92 1.276(19) . ? C92 C96 1.423(17) . ? C92 C93 1.48(2) . ? C93 C94 1.54(3) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 C95 1.46(3) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.52(2) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 C97 1.3847 . ? C97 O27 1.3042 . ? C97 C98A 1.484(9) . ? C97 C98 1.511(9) . ? C98 C99 1.3900 . ? C98 C103 1.3900 . ? C99 C100 1.3900 . ? C99 O28 1.41(4) . ? C100 C101 1.3900 . ? C100 H100 0.9500 . ? C101 C102 1.3900 . ? C101 H101 0.9500 . ? C102 C103 1.3900 . ? C102 H102 0.9500 . ? C103 H103 0.9500 . ? O28 C104 1.53(6) . ? C104 H10A 0.9800 . ? C104 H10B 0.9800 . ? C104 H10C 0.9800 . ? C98A C99A 1.3900 . ? C98A C13A 1.3900 . ? C99A C10A 1.3900 . ? C99A H99A 0.9500 . ? C10A C11A 1.3900 . ? C10A H10D 0.9500 . ? C11A C12A 1.3900 . ? C11A H11A 0.9500 . ? C12A C13A 1.3900 . ? C12A H12A 0.9500 . ? C13A O28A 1.4280 . ? O28A C14A 1.3455 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C300 C301 1.3900 . ? C300 C305 1.3900 . ? C300 C306 1.4840 . ? C301 C302 1.3900 . ? C301 H301 0.9500 . ? C302 C303 1.3900 . ? C302 H302 0.9500 . ? C303 C304 1.3900 . ? C303 H303 0.9500 . ? C304 C305 1.3900 . ? C304 H304 0.9500 . ? C305 H305 0.9500 . ? C306 H1 0.9800 . ? C306 H2 0.9800 . ? C306 H30C 0.9800 . ? C307 C308 1.3900 . ? C307 C312 1.3900 . ? C308 C309 1.3900 . ? C309 C310 1.3900 . ? C310 C311 1.3900 . ? C311 C312 1.3900 . ? O10A C26A 1.587(5) . ? C26A H26D 0.9800 . ? C26A H26E 0.9800 . ? C26A H26F 0.9800 . ? C407 C408 1.3900 . ? C407 C412 1.3900 . ? C408 C409 1.3900 . ? C409 C410 1.3900 . ? C410 C411 1.3900 . ? C411 C412 1.3900 . ? 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 Er1 O5 87.9(4) . . ? O9 Er1 O6 79.7(4) . . ? O5 Er1 O6 77.2(4) . . ? O9 Er1 O2 145.7(4) . . ? O5 Er1 O2 110.3(4) . . ? O6 Er1 O2 76.6(4) . . ? O9 Er1 O3 145.8(4) . . ? O5 Er1 O3 75.9(4) . . ? O6 Er1 O3 124.1(4) . . ? O2 Er1 O3 68.5(3) . . ? O9 Er1 O1 108.1(4) . . ? O5 Er1 O1 142.9(4) . . ? O6 Er1 O1 137.4(4) . . ? O2 Er1 O1 75.0(4) . . ? O3 Er1 O1 72.4(4) . . ? O9 Er1 O8 75.4(4) . . ? O5 Er1 O8 81.8(4) . . ? O6 Er1 O8 147.8(4) . . ? O2 Er1 O8 134.2(4) . . ? O3 Er1 O8 72.6(4) . . ? O1 Er1 O8 70.9(4) . . ? O9 Er1 O11 83.6(3) . . ? O5 Er1 O11 153.1(3) . . ? O6 Er1 O11 76.2(3) . . ? O2 Er1 O11 66.9(3) . . ? O3 Er1 O11 123.3(3) . . ? O1 Er1 O11 63.7(3) . . ? O8 Er1 O11 120.1(3) . . ? O9 Er1 Er2 123.0(3) . . ? O5 Er1 Er2 148.1(3) . . ? O6 Er1 Er2 99.2(3) . . ? O2 Er1 Er2 39.7(3) . . ? O3 Er1 Er2 80.6(3) . . ? O1 Er1 Er2 40.7(3) . . ? O8 Er1 Er2 111.3(3) . . ? O11 Er1 Er2 42.68(7) . . ? O9 Er1 Er3 125.2(3) . . ? O5 Er1 Er3 105.6(3) . . ? O6 Er1 Er3 154.7(3) . . ? O2 Er1 Er3 78.9(2) . . ? O3 Er1 Er3 37.7(3) . . ? O1 Er1 Er3 37.9(3) . . ? O8 Er1 Er3 55.4(3) . . ? O11 Er1 Er3 100.11(8) . . ? Er2 Er1 Er3 64.79(4) . . ? O9 Er1 Er4 178.4(3) . . ? O5 Er1 Er4 90.7(3) . . ? O6 Er1 Er4 99.3(3) . . ? O2 Er1 Er4 34.5(2) . . ? O3 Er1 Er4 34.2(3) . . ? O1 Er1 Er4 73.5(3) . . ? O8 Er1 Er4 105.2(3) . . ? O11 Er1 Er4 97.32(7) . . ? Er2 Er1 Er4 58.27(3) . . ? Er3 Er1 Er4 55.92(2) . . ? O12 Er2 O15 85.6(3) . . ? O12 Er2 O2 97.6(3) . . ? O15 Er2 O2 134.1(3) . . ? O12 Er2 O14 94.2(4) . . ? O15 Er2 O14 75.4(3) . . ? O2 Er2 O14 148.8(4) . . ? O12 Er2 O1 141.1(4) . . ? O15 Er2 O1 126.6(3) . . ? O2 Er2 O1 76.1(4) . . ? O14 Er2 O1 76.7(4) . . ? O12 Er2 O4 148.8(4) . . ? O15 Er2 O4 78.1(3) . . ? O2 Er2 O4 76.2(4) . . ? O14 Er2 O4 106.9(4) . . ? O1 Er2 O4 67.9(4) . . ? O12 Er2 O11 74.5(3) . . ? O15 Er2 O11 151.19(14) . . ? O2 Er2 O11 70.4(3) . . ? O14 Er2 O11 85.3(3) . . ? O1 Er2 O11 67.2(3) . . ? O4 Er2 O11 128.8(3) . . ? O12 Er2 O23 86.6(3) . . ? O15 Er2 O23 73.5(2) . . ? O2 Er2 O23 61.1(3) . . ? O14 Er2 O23 148.7(4) . . ? O1 Er2 O23 120.5(4) . . ? O4 Er2 O23 63.4(3) . . ? O11 Er2 O23 124.6(2) . . ? O12 Er2 Er1 112.2(3) . . ? O15 Er2 Er1 160.89(9) . . ? O2 Er2 Er1 40.1(3) . . ? O14 Er2 Er1 108.8(3) . . ? O1 Er2 Er1 41.4(3) . . ? O4 Er2 Er1 82.9(3) . . ? O11 Er2 Er1 46.77(9) . . ? O23 Er2 Er1 99.7(2) . . ? O12 Er2 Er4 120.2(3) . . ? O15 Er2 Er4 100.25(9) . . ? O2 Er2 Er4 39.5(2) . . ? O14 Er2 Er4 145.2(3) . . ? O1 Er2 Er4 79.1(3) . . ? O4 Er2 Er4 39.9(3) . . ? O11 Er2 Er4 107.69(9) . . ? O23 Er2 Er4 41.5(2) . . ? Er1 Er2 Er4 65.29(3) . . ? O12 Er2 Er3 171.1(3) . . ? O15 Er2 Er3 102.89(9) . . ? O2 Er2 Er3 74.7(2) . . ? O14 Er2 Er3 90.5(3) . . ? O1 Er2 Er3 33.5(3) . . ? O4 Er2 Er3 34.5(3) . . ? O11 Er2 Er3 98.42(9) . . ? O23 Er2 Er3 93.3(2) . . ? Er1 Er2 Er3 59.10(3) . . ? Er4 Er2 Er3 56.27(3) . . ? O21 Er3 O18 86.29(10) . . ? O21 Er3 O1 138.9(3) . . ? O18 Er3 O1 78.2(3) . . ? O21 Er3 O3 91.8(3) . . ? O18 Er3 O3 134.2(3) . . ? O1 Er3 O3 73.8(4) . . ? O21 Er3 O17 96.1(4) . . ? O18 Er3 O17 74.9(4) . . ? O1 Er3 O17 115.5(5) . . ? O3 Er3 O17 150.4(5) . . ? O21 Er3 O4 146.8(3) . . ? O18 Er3 O4 123.9(3) . . ? O1 Er3 O4 68.1(4) . . ? O3 Er3 O4 77.1(4) . . ? O17 Er3 O4 80.8(5) . . ? O21 Er3 O20 76.43(11) . . ? O18 Er3 O20 149.59(16) . . ? O1 Er3 O20 130.7(3) . . ? O3 Er3 O20 72.0(3) . . ? O17 Er3 O20 82.2(4) . . ? O4 Er3 O20 70.4(3) . . ? O21 Er3 Er4 112.74(11) . . ? O18 Er3 Er4 158.82(10) . . ? O1 Er3 Er4 81.2(3) . . ? O3 Er3 Er4 40.9(3) . . ? O17 Er3 Er4 110.5(4) . . ? O4 Er3 Er4 41.5(3) . . ? O20 Er3 Er4 49.81(8) . . ? O21 Er3 Er1 110.04(12) . . ? O18 Er3 Er1 100.72(11) . . ? O1 Er3 Er1 39.0(3) . . ? O3 Er3 Er1 38.0(3) . . ? O17 Er3 Er1 153.3(4) . . ? O4 Er3 Er1 80.2(3) . . ? O20 Er3 Er1 108.61(8) . . ? Er4 Er3 Er1 64.91(4) . . ? O21 Er3 Er2 165.15(12) . . ? O18 Er3 Er2 101.00(10) . . ? O1 Er3 Er2 33.9(3) . . ? O3 Er3 Er2 73.8(3) . . ? O17 Er3 Er2 98.3(4) . . ? O4 Er3 Er2 34.3(3) . . ? O20 Er3 Er2 101.86(8) . . ? Er4 Er3 Er2 58.36(3) . . ? Er1 Er3 Er2 56.12(4) . . ? O24 Er4 O27 87.29(11) . . ? O24 Er4 O26 96.5(3) . . ? O27 Er4 O26 75.7(3) . . ? O24 Er4 O3 147.9(3) . . ? O27 Er4 O3 77.5(3) . . ? O26 Er4 O3 106.6(4) . . ? O24 Er4 O2 142.0(3) . . ? O27 Er4 O2 123.7(3) . . ? O26 Er4 O2 73.8(4) . . ? O3 Er4 O2 67.7(3) . . ? O24 Er4 O4 97.9(3) . . ? O27 Er4 O4 137.5(3) . . ? O26 Er4 O4 144.2(4) . . ? O3 Er4 O4 76.2(4) . . ? O2 Er4 O4 74.7(4) . . ? O24 Er4 O23 75.3(3) . . ? O27 Er4 O23 150.3(3) . . ? O26 Er4 O23 82.4(4) . . ? O3 Er4 O23 128.8(4) . . ? O2 Er4 O23 67.1(3) . . ? O4 Er4 O23 69.9(4) . . ? O24 Er4 O20 83.13(10) . . ? O27 Er4 O20 74.40(9) . . ? O26 Er4 O20 150.1(3) . . ? O3 Er4 O20 65.7(3) . . ? O2 Er4 O20 123.4(3) . . ? O4 Er4 O20 64.5(2) . . ? O23 Er4 O20 125.6(2) . . ? O24 Er4 Er3 117.74(10) . . ? O27 Er4 Er3 99.58(10) . . ? O26 Er4 Er3 145.4(3) . . ? O3 Er4 Er3 40.3(3) . . ? O2 Er4 Er3 81.4(3) . . ? O4 Er4 Er3 41.2(3) . . ? O23 Er4 Er3 109.8(2) . . ? O20 Er4 Er3 42.10(7) . . ? O24 Er4 Er2 116.60(9) . . ? O27 Er4 Er2 155.46(10) . . ? O26 Er4 Er2 105.2(3) . . ? O3 Er4 Er2 78.9(3) . . ? O2 Er4 Er2 38.5(3) . . ? O4 Er4 Er2 39.4(2) . . ? O23 Er4 Er2 50.7(2) . . ? O20 Er4 Er2 101.58(8) . . ? Er3 Er4 Er2 65.38(4) . . ? O24 Er4 Er1 172.88(9) . . ? O27 Er4 Er1 99.48(10) . . ? O26 Er4 Er1 87.4(3) . . ? O3 Er4 Er1 34.1(2) . . ? O2 Er4 Er1 33.9(2) . . ? O4 Er4 Er1 75.7(3) . . ? O23 Er4 Er1 99.4(2) . . ? O20 Er4 Er1 96.48(7) . . ? Er3 Er4 Er1 59.17(4) . . ? Er2 Er4 Er1 56.44(3) . . ? Er3 O1 Er2 112.6(5) . . ? Er3 O1 Er1 103.1(5) . . ? Er2 O1 Er1 97.9(4) . . ? Er2 O2 Er1 100.2(4) . . ? Er2 O2 Er4 102.0(4) . . ? Er1 O2 Er4 111.6(4) . . ? Er3 O3 Er1 104.2(5) . . ? Er3 O3 Er4 98.8(4) . . ? Er1 O3 Er4 111.7(4) . . ? Er2 O4 Er3 111.2(5) . . ? Er2 O4 Er4 100.7(4) . . ? Er3 O4 Er4 97.3(4) . . ? C1 O5 Er1 130.4(11) . . ? O5 C1 C5 127.0(17) . . ? O5 C1 C2 122.5(17) . . ? C5 C1 C2 110.5(15) . . ? C1 C2 C3 104.3(17) . . ? C1 C2 H2A 110.9 . . ? C3 C2 H2A 110.9 . . ? C1 C2 H2B 110.9 . . ? C3 C2 H2B 110.9 . . ? H2A C2 H2B 108.9 . . ? C2 C3 C4 107.2(19) . . ? C2 C3 H3A 110.3 . . ? C4 C3 H3A 110.3 . . ? C2 C3 H3B 110.3 . . ? C4 C3 H3B 110.3 . . ? H3A C3 H3B 108.5 . . ? C5 C4 C3 103.3(19) . . ? C5 C4 H4A 111.1 . . ? C3 C4 H4A 111.1 . . ? C5 C4 H4B 111.1 . . ? C3 C4 H4B 111.1 . . ? H4A C4 H4B 109.1 . . ? C1 C5 C6 124.8(16) . . ? C1 C5 C4 110.9(17) . . ? C6 C5 C4 124.2(17) . . ? O6 C6 C5 122.7(15) . . ? O6 C6 C7 118.3(14) . . ? C5 C6 C7 118.9(14) . . ? C6 O6 Er1 129.7(10) . . ? C8 C7 C12 119.1(16) . . ? C8 C7 C6 118.8(16) . . ? C12 C7 C6 122.1(15) . . ? C9 C8 C7 121.5(19) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C8 119(2) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 120.4(17) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 119.9(16) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? O7 C12 C7 117.6(14) . . ? O7 C12 C11 122.8(14) . . ? C7 C12 C11 119.6(15) . . ? C12 O7 C13 119.2(13) . . ? O7 C13 H13A 109.5 . . ? O7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C14 O8 Er1 127.6(12) . . ? O8 C14 C18 127(2) . . ? O8 C14 C15 119.4(18) . . ? C18 C14 C15 111.4(17) . . ? C14 C15 C16 102.7(19) . . ? C14 C15 H15A 111.2 . . ? C16 C15 H15A 111.2 . . ? C14 C15 H15B 111.2 . . ? C16 C15 H15B 111.2 . . ? H15A C15 H15B 109.1 . . ? C15 C16 C17 105(2) . . ? C15 C16 H16A 110.8 . . ? C17 C16 H16A 110.8 . . ? C15 C16 H16B 110.8 . . ? C17 C16 H16B 110.8 . . ? H16A C16 H16B 108.9 . . ? C18 C17 C16 103(2) . . ? C18 C17 H17A 111.3 . . ? C16 C17 H17A 111.3 . . ? C18 C17 H17B 111.3 . . ? C16 C17 H17B 111.3 . . ? H17A C17 H17B 109.2 . . ? C14 C18 C19 131(2) . . ? C14 C18 C17 108(2) . . ? C19 C18 C17 121(2) . . ? C20 C19 O9 121(3) . . ? C20 C19 C18 126(3) . . ? O9 C19 C18 109.1(13) . . ? C20 C19 C20A 18.3(17) . . ? O9 C19 C20A 116.7(16) . . ? C18 C19 C20A 134(2) . . ? C19 O9 Er1 142.8(12) . . ? C19 C20 C21 133(2) . . ? C19 C20 C25 105(3) . . ? C21 C20 C25 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C20 120.0 . . ? C24 C25 O10 103.6(6) . . ? C20 C25 O10 132.7(13) . . ? C21A C20A C25A 120.0 . . ? C21A C20A C19 119.0(12) . . ? C25A C20A C19 120.9(12) . . ? C20A C21A C22A 120.0 . . ? C20A C21A O10A 113.6(12) . . ? C22A C21A O10A 124.1(12) . . ? C23A C22A C21A 120.0 . . ? C23A C22A H22A 120.0 . . ? C21A C22A H22A 120.0 . . ? C22A C23A C24A 120.0 . . ? C22A C23A H23A 120.0 . . ? C24A C23A H23A 120.0 . . ? C23A C24A C25A 120.0 . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C24A C25A C20A 120.0 . . ? C24A C25A H25A 120.0 . . ? C20A C25A H25A 120.0 . . ? C27 O11 Er2 127.76(7) . . ? C27 O11 Er1 133.69(7) . . ? Er2 O11 Er1 90.56(10) . . ? O11 C27 C31 129.6(7) . . ? O11 C27 C28 118.7 . . ? C31 C27 C28 111.6(7) . . ? C29 C28 C27 101.7(8) . . ? C29 C28 H28A 111.4 . . ? C27 C28 H28A 111.4 . . ? C29 C28 H28B 111.4 . . ? C27 C28 H28B 111.4 . . ? H28A C28 H28B 109.3 . . ? C28 C29 C30 103.2(15) . . ? C28 C29 H29A 111.1 . . ? C30 C29 H29A 111.1 . . ? C28 C29 H29B 111.1 . . ? C30 C29 H29B 111.1 . . ? H29A C29 H29B 109.1 . . ? C31 C30 C29 103.7(17) . . ? C31 C30 H30A 111.0 . . ? C29 C30 H30A 111.0 . . ? C31 C30 H30B 111.0 . . ? C29 C30 H30B 111.0 . . ? H30A C30 H30B 109.0 . . ? C27 C31 C32 123.1(14) . . ? C27 C31 C30 108.5(13) . . ? C32 C31 C30 128.2(16) . . ? O12 C32 C31 123.5(14) . . ? O12 C32 C33 114.6(11) . . ? C31 C32 C33 121.4(13) . . ? C32 O12 Er2 137.6(10) . . ? C34 C33 C38 121.4 . . ? C34 C33 C32 118.7(6) . . ? C38 C33 C32 119.4(6) . . ? C33 C34 C35 123.1(9) . . ? C33 C34 H34 118.5 . . ? C35 C34 H34 118.5 . . ? C34 C35 C36 115.8(19) . . ? C34 C35 H35 122.1 . . ? C36 C35 H35 122.1 . . ? C37 C36 C35 123(2) . . ? C37 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? C36 C37 C38 121.3(19) . . ? C36 C37 H37 119.3 . . ? C38 C37 H37 119.3 . . ? O13 C38 C33 119.9 . . ? O13 C38 C37 124.6(9) . . ? C33 C38 C37 115.5(9) . . ? C38 O13 C39 119.5 . . ? O13 C39 H39A 109.5 . . ? O13 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O13 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C40 O14 Er2 127.8(12) . . ? O14 C40 C44 126.9(18) . . ? O14 C40 C41 120.1(15) . . ? C44 C40 C41 112.6(15) . . ? C40 C41 C42 96.7(13) . . ? C40 C41 H41A 112.4 . . ? C42 C41 H41A 112.4 . . ? C40 C41 H41B 112.4 . . ? C42 C41 H41B 112.4 . . ? H41A C41 H41B 110.0 . . ? C43 C42 C41 115(2) . . ? C43 C42 H42A 108.6 . . ? C41 C42 H42A 108.6 . . ? C43 C42 H42B 108.6 . . ? C41 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C42 C43 C44 101(2) . . ? C42 C43 H43A 111.5 . . ? C44 C43 H43A 111.5 . . ? C42 C43 H43B 111.5 . . ? C44 C43 H43B 111.5 . . ? H43A C43 H43B 109.3 . . ? C45 C44 C40 124.7(17) . . ? C45 C44 C43 125.0(18) . . ? C40 C44 C43 110.2(18) . . ? O15 C45 C44 123.5(15) . . ? O15 C45 C46 117.2(13) . . ? C44 C45 C46 119.2(14) . . ? C45 O15 Er2 134.0(8) . . ? C51 C46 C47 122.6(10) . . ? C51 C46 C45 117.5(12) . . ? C47 C46 C45 119.6(7) . . ? C46 C47 C48 118.7(13) . . ? C46 C47 H47 120.7 . . ? C48 C47 H47 120.7 . . ? C49 C48 C47 116(3) . . ? C49 C48 H48 122.1 . . ? C47 C48 H48 122.1 . . ? C48 C49 C50 129(3) . . ? C48 C49 H49 115.7 . . ? C50 C49 H49 115.7 . . ? C49 C50 C51 114.1(18) . . ? C49 C50 H50 123.0 . . ? C51 C50 H50 123.0 . . ? O16 C51 C46 118.2(19) . . ? O16 C51 C50 121(2) . . ? C46 C51 C50 119.7(17) . . ? C51 O16 C52 121(2) . . ? O16 C52 H52A 109.5 . . ? O16 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O16 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C53 O17 Er3 133.1(10) . . ? O17 C53 C57 126.3(13) . . ? O17 C53 C54 118.8(7) . . ? C57 C53 C54 114.9(10) . . ? C53 C54 C55 98.1(14) . . ? C53 C54 H54A 112.2 . . ? C55 C54 H54A 112.2 . . ? C53 C54 H54B 112.2 . . ? C55 C54 H54B 112.2 . . ? H54A C54 H54B 109.8 . . ? C56 C55 C54 115(3) . . ? C56 C55 H55A 108.6 . . ? C54 C55 H55A 108.6 . . ? C56 C55 H55B 108.6 . . ? C54 C55 H55B 108.6 . . ? H55A C55 H55B 107.6 . . ? C55 C56 C57 102(3) . . ? C55 C56 H56A 111.4 . . ? C57 C56 H56A 111.4 . . ? C55 C56 H56B 111.4 . . ? C57 C56 H56B 111.4 . . ? H56A C56 H56B 109.3 . . ? C58 C57 C53 124.7(19) . . ? C58 C57 C56 127(2) . . ? C53 C57 C56 108(2) . . ? C57 C58 O18 126.9(11) . . ? C57 C58 C59 125.7(11) . . ? O18 C58 C59 107.2 . . ? C58 O18 Er3 132.85(9) . . ? C60 C59 C64 116.7(14) . . ? C60 C59 C58 116.7 . . ? C64 C59 C58 125.1(14) . . ? C61 C60 C59 115.8(17) . . ? C61 C60 H60 122.1 . . ? C59 C60 H60 122.1 . . ? C62 C61 C60 127(3) . . ? C62 C61 H61 116.5 . . ? C60 C61 H61 116.5 . . ? C61 C62 C63 124(3) . . ? C61 C62 H62 118.0 . . ? C63 C62 H62 118.0 . . ? C64 C63 C62 110(3) . . ? C64 C63 H63 124.8 . . ? C62 C63 H63 124.8 . . ? O19 C64 C63 120(3) . . ? O19 C64 C59 115(3) . . ? C63 C64 C59 125(3) . . ? C64 O19 C65 119(3) . . ? O19 C65 H65A 109.5 . . ? O19 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? O19 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C66 O20 Er3 130.89(7) . . ? C66 O20 Er4 125.02(7) . . ? Er3 O20 Er4 88.10(10) . . ? O20 C66 C70 127.1 . . ? O20 C66 C67 122.9 . . ? C70 C66 C67 109.9 . . ? C66 C67 C68 102.3(8) . . ? C66 C67 H67A 111.3 . . ? C68 C67 H67A 111.3 . . ? C66 C67 H67B 111.3 . . ? C68 C67 H67B 111.3 . . ? H67A C67 H67B 109.2 . . ? C69 C68 C67 105.4(16) . . ? C69 C68 H68A 110.7 . . ? C67 C68 H68A 110.7 . . ? C69 C68 H68B 110.7 . . ? C67 C68 H68B 110.7 . . ? H68A C68 H68B 108.8 . . ? C70 C69 C68 102.1(17) . . ? C70 C69 H69A 111.3 . . ? C68 C69 H69A 111.3 . . ? C70 C69 H69B 111.3 . . ? C68 C69 H69B 111.3 . . ? H69A C69 H69B 109.2 . . ? C66 C70 C71 122.0 . . ? C66 C70 C69 110.6(9) . . ? C71 C70 C69 127.5(9) . . ? O21 C71 C70 124.9 . . ? O21 C71 C72 116.2 . . ? C70 C71 C72 118.6 . . ? C71 O21 Er3 138.21(9) . . ? C73 C72 C77 125.4(10) . . ? C73 C72 C71 113.7 . . ? C77 C72 C71 120.8(10) . . ? C72 C73 C74 115.9 . . ? C72 C73 H73 122.1 . . ? C74 C73 H73 122.1 . . ? C75 C74 C73 118(2) . . ? C75 C74 H74 121.2 . . ? C73 C74 H74 121.2 . . ? C74 C75 C76 131(4) . . ? C74 C75 H75 114.7 . . ? C76 C75 H75 114.7 . . ? C75 C76 C77 110(3) . . ? C75 C76 H76 124.8 . . ? C77 C76 H76 124.8 . . ? O22 C77 C72 121(2) . . ? O22 C77 C76 119(3) . . ? C72 C77 C76 119(2) . . ? C77 O22 C78 122.8(18) . . ? O22 C78 H78A 109.5 . . ? O22 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? O22 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C79 O23 Er4 127.9(10) . . ? C79 O23 Er2 135.8(9) . . ? Er4 O23 Er2 87.8(3) . . ? O23 C79 C83 128.5(13) . . ? O23 C79 C80 119.4(14) . . ? C83 C79 C80 112.1(12) . . ? C79 C80 C81 101.5(14) . . ? C79 C80 H80A 111.5 . . ? C81 C80 H80A 111.5 . . ? C79 C80 H80B 111.5 . . ? C81 C80 H80B 111.5 . . ? H80A C80 H80B 109.3 . . ? C82 C81 C80 105.0(15) . . ? C82 C81 H81A 110.7 . . ? C80 C81 H81A 110.7 . . ? C82 C81 H81B 110.7 . . ? C80 C81 H81B 110.7 . . ? H81A C81 H81B 108.8 . . ? C81 C82 C83 103.1(13) . . ? C81 C82 H82A 111.1 . . ? C83 C82 H82A 111.1 . . ? C81 C82 H82B 111.1 . . ? C83 C82 H82B 111.1 . . ? H82A C82 H82B 109.1 . . ? C79 C83 C84 124.8(6) . . ? C79 C83 C82 107.6(9) . . ? C84 C83 C82 127.2(7) . . ? O24 C84 C83 122.4 . . ? O24 C84 C85 116.3 . . ? C83 C84 C85 121.3 . . ? C84 O24 Er4 139.41(8) . . ? C90 C85 C86 120.4(8) . . ? C90 C85 C84 124.2(8) . . ? C86 C85 C84 114.7 . . ? C85 C86 C87 117.6 . . ? C85 C86 H86 121.2 . . ? C87 C86 H86 121.2 . . ? C88 C87 C86 120.7(10) . . ? C88 C87 H87 119.6 . . ? C86 C87 H87 119.6 . . ? C87 C88 C89 119.5(19) . . ? C87 C88 H88 120.2 . . ? C89 C88 H88 120.2 . . ? C90 C89 C88 120.3(19) . . ? C90 C89 H89 119.8 . . ? C88 C89 H89 119.8 . . ? C85 C90 O25 116.2(14) . . ? C85 C90 C89 121.1(16) . . ? O25 C90 C89 122.6(16) . . ? C90 O25 C91 117.2(12) . . ? O25 C91 H91A 109.5 . . ? O25 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? O25 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C92 O26 Er4 131.2(10) . . ? O26 C92 C96 123.9(13) . . ? O26 C92 C93 123.1(15) . . ? C96 C92 C93 113.1(13) . . ? C92 C93 C94 101.6(16) . . ? C92 C93 H93A 111.4 . . ? C94 C93 H93A 111.4 . . ? C92 C93 H93B 111.4 . . ? C94 C93 H93B 111.4 . . ? H93A C93 H93B 109.3 . . ? C95 C94 C93 110(2) . . ? C95 C94 H94A 109.8 . . ? C93 C94 H94A 109.8 . . ? C95 C94 H94B 109.8 . . ? C93 C94 H94B 109.8 . . ? H94A C94 H94B 108.2 . . ? C94 C95 C96 105.0(18) . . ? C94 C95 H95A 110.7 . . ? C96 C95 H95A 110.7 . . ? C94 C95 H95B 110.7 . . ? C96 C95 H95B 110.7 . . ? H95A C95 H95B 108.8 . . ? C97 C96 C92 128.3(6) . . ? C97 C96 C95 124.3(10) . . ? C92 C96 C95 107.3(11) . . ? O27 C97 C96 120.3 . . ? O27 C97 C98A 121.2(9) . . ? C96 C97 C98A 115.3(9) . . ? O27 C97 C98 111.4(10) . . ? C96 C97 C98 126.9(10) . . ? C98A C97 C98 31.8(10) . . ? C97 O27 Er4 133.39(8) . . ? C99 C98 C103 120.0 . . ? C99 C98 C97 117.5(16) . . ? C103 C98 C97 122.5(16) . . ? C100 C99 C98 120.0 . . ? C100 C99 O28 126(2) . . ? C98 C99 O28 113(2) . . ? C99 C100 C101 120.0 . . ? C99 C100 H100 120.0 . . ? C101 C100 H100 120.0 . . ? C100 C101 C102 120.0 . . ? C100 C101 H101 120.0 . . ? C102 C101 H101 120.0 . . ? C103 C102 C101 120.0 . . ? C103 C102 H102 120.0 . . ? C101 C102 H102 120.0 . . ? C102 C103 C98 120.0 . . ? C102 C103 H103 120.0 . . ? C98 C103 H103 120.0 . . ? C99 O28 C104 108(3) . . ? C99A C98A C13A 120.0 . . ? C99A C98A C97 131.7(8) . . ? C13A C98A C97 108.1(8) . . ? C98A C99A C10A 120.0 . . ? C98A C99A H99A 120.0 . . ? C10A C99A H99A 120.0 . . ? C11A C10A C99A 120.0 . . ? C11A C10A H10D 120.0 . . ? C99A C10A H10D 120.0 . . ? C12A C11A C10A 120.0 . . ? C12A C11A H11A 120.0 . . ? C10A C11A H11A 120.0 . . ? C11A C12A C13A 120.0 . . ? C11A C12A H12A 120.0 . . ? C13A C12A H12A 120.0 . . ? C12A C13A C98A 120.0 . . ? C12A C13A O28A 119.9 . . ? C98A C13A O28A 120.0 . . ? C14A O28A C13A 132.1 . . ? O28A C14A H14A 109.5 . . ? O28A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? O28A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C301 C300 C305 120.0 . . ? C301 C300 C306 113.2 . . ? C305 C300 C306 124.2 . . ? C300 C301 C302 120.0 . . ? C300 C301 H301 120.0 . . ? C302 C301 H301 120.0 . . ? C301 C302 C303 120.0 . . ? C301 C302 H302 120.0 . . ? C303 C302 H302 120.0 . . ? C304 C303 C302 120.0 . . ? C304 C303 H303 120.0 . . ? C302 C303 H303 120.0 . . ? C303 C304 C305 120.0 . . ? C303 C304 H304 120.0 . . ? C305 C304 H304 120.0 . . ? C304 C305 C300 120.0 . . ? C304 C305 H305 120.0 . . ? C300 C305 H305 120.0 . . ? C300 C306 H1 109.5 . . ? C300 C306 H2 109.5 . . ? H1 C306 H2 109.5 . . ? C300 C306 H30C 109.5 . . ? H1 C306 H30C 109.5 . . ? H2 C306 H30C 109.5 . . ? C308 C307 C312 120.0 . . ? C309 C308 C307 120.0 . . ? C308 C309 C310 120.0 . . ? C311 C310 C309 120.0 . . ? C310 C311 C312 120.0 . . ? C311 C312 C307 120.0 . . ? C21A O10A C26A 134(3) . . ? O10A C26A H26D 109.5 . . ? O10A C26A H26E 109.5 . . ? H26D C26A H26E 109.5 . . ? O10A C26A H26F 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? C26 O10 C25 148.1(11) . . ? C408 C407 C412 120.0 . . ? C407 C408 C409 120.0 . . ? C410 C409 C408 120.0 . . ? C409 C410 C411 120.0 . . ? C412 C411 C410 120.0 . . ? C411 C412 C407 120.0 . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 2.398 _refine_diff_density_min -2.433 _refine_diff_density_rms 0.239 # Attachment 'WGE036.CIF' data_wge036 _database_code_depnum_ccdc_archive 'CCDC 801775' #TrackingRef 'WGE036.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H84 Dy4 N8 O36' _chemical_formula_sum 'C96 H84 Dy4 N8 O36' _chemical_formula_weight 2575.71 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 tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' _symmetry_space_group_name_Hall 'P -4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 17.125(2) _cell_length_b 17.125(2) _cell_length_c 15.993(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4690.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 44403 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 24.99 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 3.244 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9089 _exptl_absorpt_correction_T_max 0.9683 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.773747856 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Australian synchrotron MX1' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44403 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0139 _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 -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3208 _reflns_number_gt 3152 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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^)+(0.0232P)^2^+12.1202P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.052(13) _refine_ls_number_reflns 3208 _refine_ls_number_parameters 325 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0211 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0517 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.159 _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 Dy1 Dy 0.386400(11) 0.502516(14) 0.575412(11) 0.01318(9) Uani 1 1 d . . . O1 O 0.4975(2) 0.57767(15) 0.56680(16) 0.0132(6) Uani 1 1 d D . . O2 O 0.3465(2) 0.60431(19) 0.6581(2) 0.0186(8) Uani 1 1 d . . . O3 O 0.3933(2) 0.45355(18) 0.7091(2) 0.0170(7) Uani 1 1 d . . . O4 O 0.4890(3) 0.6875(2) 0.7521(2) 0.0359(10) Uani 1 1 d D . . O5 O 0.4904(3) 0.7466(3) 0.8734(3) 0.0520(12) Uani 1 1 d . . . O6 O 0.25964(17) 0.5086(2) 0.53665(18) 0.0184(7) Uani 1 1 d . . . O7 O 0.35375(19) 0.37358(18) 0.5372(2) 0.0184(8) Uani 1 1 d . . . O8 O 0.1083(3) 0.6278(3) 0.6246(3) 0.0441(11) Uani 1 1 d . . . O9 O 0.1096(2) 0.5010(3) 0.6267(2) 0.0334(8) Uani 1 1 d . . . N1 N 0.4575(3) 0.7264(3) 0.8077(3) 0.0291(11) Uani 1 1 d . . . N2 N 0.1077(3) 0.5640(3) 0.5895(3) 0.0269(11) Uani 1 1 d . . . C1 C 0.3437(3) 0.6162(3) 0.7368(3) 0.0156(11) Uani 1 1 d . . . C2 C 0.3571(3) 0.5604(3) 0.7982(3) 0.0168(11) Uani 1 1 d . . . C3 C 0.3818(3) 0.4837(3) 0.7801(3) 0.0166(11) Uani 1 1 d . . . C4 C 0.3974(4) 0.4404(3) 0.8604(3) 0.0275(13) Uani 1 1 d . . . H4A H 0.4541 0.4380 0.8723 0.033 Uiso 1 1 calc R . . H4B H 0.3764 0.3866 0.8578 0.033 Uiso 1 1 calc R . . C5 C 0.3548(4) 0.4886(3) 0.9262(3) 0.0325(14) Uani 1 1 d . . . H5A H 0.3837 0.4879 0.9798 0.039 Uiso 1 1 calc R . . H5B H 0.3016 0.4677 0.9358 0.039 Uiso 1 1 calc R . . C6 C 0.3506(4) 0.5725(3) 0.8908(3) 0.0236(12) Uani 1 1 d . . . H6A H 0.3005 0.5978 0.9055 0.028 Uiso 1 1 calc R . . H6B H 0.3942 0.6049 0.9121 0.028 Uiso 1 1 calc R . . C7 C 0.3220(3) 0.6986(3) 0.7624(3) 0.0169(11) Uani 1 1 d . . . C8 C 0.3754(3) 0.7512(3) 0.7968(3) 0.0210(12) Uani 1 1 d . . . C9 C 0.3555(3) 0.8255(3) 0.8206(3) 0.0261(13) Uani 1 1 d . . . H9 H 0.3933 0.8593 0.8446 0.031 Uiso 1 1 calc R . . C10 C 0.2795(4) 0.8502(3) 0.8090(4) 0.0298(14) Uani 1 1 d . . . H10 H 0.2654 0.9024 0.8225 0.036 Uiso 1 1 calc R . . C11 C 0.2237(3) 0.7992(3) 0.7780(3) 0.0246(12) Uani 1 1 d . . . H11 H 0.1708 0.8154 0.7733 0.030 Uiso 1 1 calc R . . C12 C 0.2454(3) 0.7241(3) 0.7535(3) 0.0187(11) Uani 1 1 d . . . H12 H 0.2074 0.6899 0.7304 0.022 Uiso 1 1 calc R . . C13 C 0.2144(3) 0.4650(3) 0.4911(3) 0.0158(11) Uani 1 1 d . . . C14 C 0.2269(3) 0.3860(3) 0.4758(3) 0.0175(11) Uani 1 1 d . . . C15 C 0.2932(3) 0.3462(3) 0.5038(3) 0.0167(11) Uani 1 1 d . . . C16 C 0.2851(3) 0.2596(3) 0.4871(3) 0.0210(12) Uani 1 1 d . . . H16A H 0.2999 0.2286 0.5369 0.025 Uiso 1 1 calc R . . H16B H 0.3179 0.2434 0.4393 0.025 Uiso 1 1 calc R . . C17 C 0.1982(3) 0.2495(3) 0.4670(4) 0.0271(13) Uani 1 1 d . . . H17A H 0.1687 0.2351 0.5180 0.032 Uiso 1 1 calc R . . H17B H 0.1906 0.2083 0.4244 0.032 Uiso 1 1 calc R . . C18 C 0.1708(3) 0.3289(3) 0.4336(3) 0.0236(12) Uani 1 1 d . . . H18A H 0.1755 0.3314 0.3720 0.028 Uiso 1 1 calc R . . H18B H 0.1161 0.3395 0.4498 0.028 Uiso 1 1 calc R . . C19 C 0.1483(3) 0.5095(4) 0.4529(3) 0.0210(11) Uani 1 1 d . . . C20 C 0.1025(3) 0.5623(3) 0.4980(3) 0.0209(12) Uani 1 1 d . . . C21 C 0.0516(3) 0.6147(4) 0.4618(4) 0.0327(14) Uani 1 1 d . . . H21 H 0.0227 0.6506 0.4949 0.039 Uiso 1 1 calc R . . C22 C 0.0439(3) 0.6130(4) 0.3752(4) 0.0408(16) Uani 1 1 d . . . H22 H 0.0096 0.6486 0.3483 0.049 Uiso 1 1 calc R . . C23 C 0.0858(4) 0.5601(4) 0.3280(4) 0.0458(18) Uani 1 1 d . . . H23 H 0.0788 0.5560 0.2692 0.055 Uiso 1 1 calc R . . C24 C 0.1377(3) 0.5138(3) 0.3698(3) 0.0304(15) Uani 1 1 d . . . H24 H 0.1699 0.4811 0.3364 0.037 Uiso 1 1 calc R . . H1 H 0.4971 0.6152 0.5941 0.037 Uiso 1 1 d RD . . 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 Dy1 0.01069(12) 0.01419(12) 0.01464(13) -0.00267(15) 0.00191(8) 0.00032(13) O1 0.0154(15) 0.0091(14) 0.0149(14) -0.0013(11) 0.001(2) 0.0029(15) O2 0.028(2) 0.0201(19) 0.0080(17) 0.0020(15) 0.0043(15) 0.0091(16) O3 0.0222(19) 0.0116(17) 0.0172(19) 0.0015(15) 0.0042(16) -0.0011(15) O4 0.033(3) 0.033(2) 0.041(2) -0.0034(18) 0.004(2) 0.007(2) O5 0.044(3) 0.051(3) 0.061(3) -0.015(2) -0.022(3) -0.008(3) O6 0.0157(15) 0.0139(18) 0.0258(16) -0.0013(17) 0.0010(14) -0.0024(16) O7 0.0161(18) 0.0110(17) 0.0281(18) -0.0033(14) -0.0044(15) -0.0029(14) O8 0.055(3) 0.037(3) 0.041(2) -0.007(2) 0.003(2) 0.010(2) O9 0.042(2) 0.028(2) 0.0297(18) 0.006(3) 0.0106(15) 0.008(3) N1 0.032(3) 0.020(2) 0.034(3) 0.007(2) -0.011(2) -0.009(2) N2 0.024(2) 0.028(3) 0.029(3) 0.001(2) 0.004(2) 0.009(2) C1 0.011(2) 0.015(2) 0.021(3) 0.000(2) 0.002(2) 0.004(2) C2 0.022(3) 0.015(3) 0.014(3) -0.002(2) 0.003(2) 0.001(2) C3 0.013(2) 0.022(3) 0.015(2) 0.000(2) -0.0002(19) -0.005(2) C4 0.041(4) 0.019(3) 0.022(3) 0.002(2) -0.001(3) -0.001(3) C5 0.063(4) 0.011(3) 0.023(3) 0.007(3) 0.001(3) 0.007(3) C6 0.041(3) 0.018(3) 0.012(3) 0.006(2) 0.002(2) -0.002(2) C7 0.028(3) 0.016(3) 0.007(2) 0.000(2) 0.005(2) 0.003(2) C8 0.028(3) 0.020(3) 0.015(3) 0.003(2) 0.001(2) 0.004(2) C9 0.042(4) 0.020(3) 0.017(3) 0.000(2) 0.005(2) 0.000(3) C10 0.046(4) 0.021(3) 0.022(3) -0.002(2) 0.007(3) 0.006(3) C11 0.032(3) 0.027(3) 0.014(3) 0.000(2) 0.011(3) 0.017(3) C12 0.025(3) 0.018(3) 0.012(2) -0.002(2) 0.008(2) 0.005(3) C13 0.010(2) 0.025(3) 0.012(2) 0.004(2) 0.004(2) -0.002(2) C14 0.016(3) 0.025(3) 0.012(2) -0.002(2) 0.004(2) -0.005(2) C15 0.016(3) 0.017(3) 0.017(3) -0.001(2) 0.009(2) -0.007(2) C16 0.026(3) 0.018(3) 0.019(3) -0.003(2) 0.004(2) -0.005(2) C17 0.022(3) 0.025(3) 0.034(3) -0.009(3) 0.004(2) -0.014(2) C18 0.013(3) 0.034(3) 0.024(3) -0.009(3) -0.001(2) -0.006(2) C19 0.013(2) 0.029(3) 0.020(2) 0.002(3) 0.0034(18) 0.003(3) C20 0.016(3) 0.025(3) 0.022(3) 0.006(2) 0.000(2) -0.002(2) C21 0.021(3) 0.037(3) 0.040(4) 0.009(3) 0.002(3) 0.010(3) C22 0.027(3) 0.053(4) 0.042(4) 0.014(3) -0.008(3) 0.012(3) C23 0.042(4) 0.067(5) 0.029(4) 0.011(3) -0.006(3) 0.011(4) C24 0.028(3) 0.038(4) 0.025(3) 0.010(3) 0.004(2) 0.009(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 Dy1 O6 2.260(3) . ? Dy1 O2 2.292(3) . ? Dy1 O3 2.300(3) . ? Dy1 O1 2.302(4) . ? Dy1 O1 2.358(3) 4_656 ? Dy1 O7 2.358(3) . ? Dy1 O1 2.420(4) 3_665 ? Dy1 Dy1 3.6595(5) 4_656 ? Dy1 Dy1 3.6595(5) 2_566 ? Dy1 Dy1 3.8919(7) 3_665 ? O1 Dy1 2.358(3) 2_566 ? O1 Dy1 2.420(4) 3_665 ? O1 H1 0.7765 . ? O2 C1 1.275(6) . ? O3 C3 1.263(6) . ? O4 N1 1.235(6) . ? O5 N1 1.242(6) . ? O6 C13 1.300(6) . ? O7 C15 1.258(6) . ? O8 N2 1.229(6) . ? O9 N2 1.231(6) . ? N1 C8 1.480(7) . ? N2 C20 1.467(7) . ? C1 C2 1.389(7) . ? C1 C7 1.516(7) . ? C2 C3 1.410(7) . ? C2 C6 1.500(7) . ? C3 C4 1.506(7) . ? C4 C5 1.524(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.546(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C12 1.389(8) . ? C7 C8 1.396(7) . ? C8 C9 1.370(7) . ? C9 C10 1.382(8) . ? C9 H9 0.9500 . ? C10 C11 1.387(8) . ? C10 H10 0.9500 . ? C11 C12 1.396(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.391(7) . ? C13 C19 1.495(7) . ? C14 C15 1.397(8) . ? C14 C18 1.528(7) . ? C15 C16 1.514(7) . ? C16 C17 1.531(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.533(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.343(7) . ? C19 C20 1.398(8) . ? C20 C21 1.378(8) . ? C21 C22 1.392(9) . ? C21 H21 0.9500 . ? C22 C23 1.381(9) . ? C22 H22 0.9500 . ? C23 C24 1.365(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Dy1 O2 80.64(12) . . ? O6 Dy1 O3 108.74(12) . . ? O2 Dy1 O3 75.88(11) . . ? O6 Dy1 O1 138.78(12) . . ? O2 Dy1 O1 81.70(11) . . ? O3 Dy1 O1 102.53(11) . . ? O6 Dy1 O1 89.30(10) . 4_656 ? O2 Dy1 O1 131.45(12) . 4_656 ? O3 Dy1 O1 150.48(12) . 4_656 ? O1 Dy1 O1 75.33(11) . 4_656 ? O6 Dy1 O7 75.18(12) . . ? O2 Dy1 O7 142.28(12) . . ? O3 Dy1 O7 84.94(12) . . ? O1 Dy1 O7 134.75(11) . . ? O1 Dy1 O7 77.17(13) 4_656 . ? O6 Dy1 O1 143.08(11) . 3_665 ? O2 Dy1 O1 135.15(11) . 3_665 ? O3 Dy1 O1 78.68(10) . 3_665 ? O1 Dy1 O1 68.57(10) . 3_665 ? O1 Dy1 O1 73.15(11) 4_656 3_665 ? O7 Dy1 O1 69.43(11) . 3_665 ? O6 Dy1 Dy1 110.09(8) . 4_656 ? O2 Dy1 Dy1 161.52(9) . 4_656 ? O3 Dy1 Dy1 112.83(8) . 4_656 ? O1 Dy1 Dy1 80.48(7) . 4_656 ? O1 Dy1 Dy1 37.70(9) 4_656 4_656 ? O7 Dy1 Dy1 56.19(8) . 4_656 ? O1 Dy1 Dy1 39.39(6) 3_665 4_656 ? O6 Dy1 Dy1 108.50(8) . 2_566 ? O2 Dy1 Dy1 98.45(8) . 2_566 ? O3 Dy1 Dy1 140.75(8) . 2_566 ? O1 Dy1 Dy1 38.79(7) . 2_566 ? O1 Dy1 Dy1 40.64(9) 4_656 2_566 ? O7 Dy1 Dy1 116.40(9) . 2_566 ? O1 Dy1 Dy1 79.11(7) 3_665 2_566 ? Dy1 Dy1 Dy1 64.248(10) 4_656 2_566 ? O6 Dy1 Dy1 164.01(7) . 3_665 ? O2 Dy1 Dy1 108.34(9) . 3_665 ? O3 Dy1 Dy1 86.59(8) . 3_665 ? O1 Dy1 Dy1 35.48(8) . 3_665 ? O1 Dy1 Dy1 74.83(6) 4_656 3_665 ? O7 Dy1 Dy1 102.49(8) . 3_665 ? O1 Dy1 Dy1 33.51(7) 3_665 3_665 ? Dy1 Dy1 Dy1 57.876(5) 4_656 3_665 ? Dy1 Dy1 Dy1 57.876(5) 2_566 3_665 ? Dy1 O1 Dy1 103.51(12) . 2_566 ? Dy1 O1 Dy1 111.01(10) . 3_665 ? Dy1 O1 Dy1 99.97(12) 2_566 3_665 ? Dy1 O1 H1 114.9 . . ? Dy1 O1 H1 109.0 2_566 . ? Dy1 O1 H1 116.4 3_665 . ? C1 O2 Dy1 134.6(3) . . ? C3 O3 Dy1 132.8(3) . . ? C13 O6 Dy1 134.5(3) . . ? C15 O7 Dy1 130.9(3) . . ? O4 N1 O5 124.2(5) . . ? O4 N1 C8 119.0(5) . . ? O5 N1 C8 116.8(5) . . ? O8 N2 O9 123.9(5) . . ? O8 N2 C20 118.3(5) . . ? O9 N2 C20 117.8(5) . . ? O2 C1 C2 125.5(4) . . ? O2 C1 C7 115.2(4) . . ? C2 C1 C7 119.3(4) . . ? C1 C2 C3 123.1(4) . . ? C1 C2 C6 126.2(5) . . ? C3 C2 C6 110.7(5) . . ? O3 C3 C2 127.7(5) . . ? O3 C3 C4 122.5(4) . . ? C2 C3 C4 109.7(4) . . ? C3 C4 C5 103.7(4) . . ? C3 C4 H4A 111.0 . . ? C5 C4 H4A 111.0 . . ? C3 C4 H4B 111.0 . . ? C5 C4 H4B 111.0 . . ? H4A C4 H4B 109.0 . . ? C4 C5 C6 105.9(4) . . ? C4 C5 H5A 110.6 . . ? C6 C5 H5A 110.6 . . ? C4 C5 H5B 110.6 . . ? C6 C5 H5B 110.6 . . ? H5A C5 H5B 108.7 . . ? C2 C6 C5 103.3(5) . . ? C2 C6 H6A 111.1 . . ? C5 C6 H6A 111.1 . . ? C2 C6 H6B 111.1 . . ? C5 C6 H6B 111.1 . . ? H6A C6 H6B 109.1 . . ? C12 C7 C8 117.2(5) . . ? C12 C7 C1 119.7(4) . . ? C8 C7 C1 123.1(5) . . ? C9 C8 C7 123.0(5) . . ? C9 C8 N1 118.1(5) . . ? C7 C8 N1 118.9(5) . . ? C8 C9 C10 118.8(5) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? C9 C10 C11 120.3(5) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 119.8(5) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 120.8(5) . . ? C7 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? O6 C13 C14 124.4(4) . . ? O6 C13 C19 112.8(4) . . ? C14 C13 C19 122.7(5) . . ? C13 C14 C15 122.9(5) . . ? C13 C14 C18 127.1(5) . . ? C15 C14 C18 109.9(4) . . ? O7 C15 C14 128.6(4) . . ? O7 C15 C16 121.1(5) . . ? C14 C15 C16 110.3(4) . . ? C15 C16 C17 103.6(4) . . ? C15 C16 H16A 111.0 . . ? C17 C16 H16A 111.0 . . ? C15 C16 H16B 111.0 . . ? C17 C16 H16B 111.0 . . ? H16A C16 H16B 109.0 . . ? C16 C17 C18 105.7(4) . . ? C16 C17 H17A 110.6 . . ? C18 C17 H17A 110.6 . . ? C16 C17 H17B 110.6 . . ? C18 C17 H17B 110.6 . . ? H17A C17 H17B 108.7 . . ? C14 C18 C17 102.8(4) . . ? C14 C18 H18A 111.2 . . ? C17 C18 H18A 111.2 . . ? C14 C18 H18B 111.2 . . ? C17 C18 H18B 111.2 . . ? H18A C18 H18B 109.1 . . ? C24 C19 C20 113.5(5) . . ? C24 C19 C13 122.4(5) . . ? C20 C19 C13 122.9(4) . . ? C21 C20 C19 124.0(5) . . ? C21 C20 N2 116.4(5) . . ? C19 C20 N2 119.6(4) . . ? C20 C21 C22 117.6(6) . . ? C20 C21 H21 121.2 . . ? C22 C21 H21 121.2 . . ? C23 C22 C21 120.6(6) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 116.8(6) . . ? C24 C23 H23 121.6 . . ? C22 C23 H23 121.6 . . ? C19 C24 C23 127.2(6) . . ? C19 C24 H24 116.4 . . ? C23 C24 H24 116.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O4 0.78 2.82 3.512(5) 150.2 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.615 _refine_diff_density_min -0.827 _refine_diff_density_rms 0.083 # Attachment 'WGE037.CIF' data_wge037 _database_code_depnum_ccdc_archive 'CCDC 801776' #TrackingRef 'WGE037.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H84 Gd4 N8 O36' _chemical_formula_sum 'C96 H84 Gd4 N8 O36' _chemical_formula_weight 2554.71 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 tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' _symmetry_space_group_name_Hall 'P -4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 17.209(2) _cell_length_b 17.209(2) _cell_length_c 16.019(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4744.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 46069 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 25.00 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 2.853 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9193 _exptl_absorpt_correction_T_max 0.9451 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77369 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Australian synchrotron MX1' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% ? _diffrn_reflns_number 46069 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0112 _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 -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3228 _reflns_number_gt 3211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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^)+(0.0253P)^2^+8.0581P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.036(11) _refine_ls_number_reflns 3228 _refine_ls_number_parameters 328 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0189 _refine_ls_wR_factor_ref 0.0477 _refine_ls_wR_factor_gt 0.0476 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.385105(9) 0.494600(10) 1.074708(10) 0.01399(7) Uani 1 1 d . . . O1 O 0.50025(16) 0.42207(13) 1.06866(14) 0.0141(5) Uani 1 1 d D . . O2 O 0.34435(16) 0.39416(15) 1.16043(16) 0.0209(6) Uani 1 1 d . . . O3 O 0.38987(16) 0.54530(15) 1.20967(17) 0.0195(6) Uani 1 1 d . . . O4 O 0.48712(19) 0.31282(18) 1.25480(19) 0.0373(8) Uani 1 1 d D . . O5 O 0.4901(2) 0.2535(2) 1.3743(2) 0.0520(9) Uani 1 1 d . . . O6 O 0.25744(14) 0.49147(16) 1.03496(15) 0.0201(6) Uani 1 1 d . . . O7 O 0.35437(15) 0.62454(15) 1.03056(16) 0.0202(6) Uani 1 1 d . . . O8 O 0.10774(17) 0.4992(2) 1.12402(17) 0.0345(7) Uani 1 1 d . . . O9 O 0.1089(2) 0.3725(2) 1.1227(2) 0.0459(9) Uani 1 1 d . . . N1 N 0.4566(2) 0.2738(2) 1.3098(2) 0.0298(9) Uani 1 1 d . . . N2 N 0.1072(2) 0.4366(2) 1.0872(2) 0.0279(8) Uani 1 1 d . . . C1 C 0.3425(2) 0.3825(2) 1.2392(2) 0.0162(8) Uani 1 1 d . . . C2 C 0.3558(2) 0.4390(2) 1.2995(2) 0.0176(9) Uani 1 1 d . . . C3 C 0.3793(2) 0.5152(2) 1.2808(2) 0.0181(8) Uani 1 1 d . . . C4 C 0.3957(3) 0.5589(2) 1.3605(3) 0.0322(11) Uani 1 1 d . . . H4A H 0.3739 0.6121 1.3582 0.039 Uiso 1 1 calc R . . H4B H 0.4523 0.5623 1.3710 0.039 Uiso 1 1 calc R . . C5 C 0.3553(3) 0.5102(2) 1.4279(3) 0.0365(11) Uani 1 1 d . . . H5A H 0.3026 0.5309 1.4395 0.044 Uiso 1 1 calc R . . H5B H 0.3857 0.5109 1.4804 0.044 Uiso 1 1 calc R . . C6 C 0.3503(3) 0.4270(3) 1.3926(3) 0.0286(11) Uani 1 1 d . . . H6A H 0.3938 0.3946 1.4132 0.034 Uiso 1 1 calc R . . H6B H 0.3005 0.4020 1.4079 0.034 Uiso 1 1 calc R . . C7 C 0.3218(2) 0.3009(2) 1.2653(2) 0.0186(9) Uani 1 1 d . . . C8 C 0.3753(3) 0.2493(2) 1.2995(3) 0.0235(10) Uani 1 1 d . . . C9 C 0.3559(3) 0.1744(2) 1.3233(2) 0.0288(11) Uani 1 1 d . . . H9 H 0.3938 0.1408 1.3469 0.035 Uiso 1 1 calc R . . C10 C 0.2792(3) 0.1493(3) 1.3117(3) 0.0313(11) Uani 1 1 d . . . H10 H 0.2652 0.0974 1.3251 0.038 Uiso 1 1 calc R . . C11 C 0.2242(3) 0.2000(3) 1.2809(3) 0.0281(10) Uani 1 1 d . . . H11 H 0.1716 0.1838 1.2764 0.034 Uiso 1 1 calc R . . C12 C 0.2452(2) 0.2750(2) 1.2563(2) 0.0214(9) Uani 1 1 d . . . H12 H 0.2072 0.3088 1.2333 0.026 Uiso 1 1 calc R . . C13 C 0.2128(2) 0.5347(2) 0.9889(2) 0.0184(9) Uani 1 1 d . . . C14 C 0.2261(2) 0.6132(2) 0.9733(2) 0.0186(9) Uani 1 1 d . . . C15 C 0.2926(2) 0.6523(2) 0.9998(2) 0.0175(9) Uani 1 1 d . . . C16 C 0.2846(2) 0.7389(2) 0.9839(2) 0.0212(9) Uani 1 1 d . . . H16A H 0.3170 0.7552 0.9359 0.025 Uiso 1 1 calc R . . H16B H 0.3000 0.7692 1.0337 0.025 Uiso 1 1 calc R . . C17 C 0.1986(3) 0.7496(3) 0.9649(3) 0.0291(11) Uani 1 1 d . . . H17A H 0.1910 0.7904 0.9221 0.035 Uiso 1 1 calc R . . H17B H 0.1698 0.7645 1.0160 0.035 Uiso 1 1 calc R . . C18 C 0.1702(2) 0.6704(2) 0.9323(3) 0.0269(9) Uani 1 1 d . . . H18A H 0.1159 0.6602 0.9495 0.032 Uiso 1 1 calc R . . H18B H 0.1737 0.6677 0.8706 0.032 Uiso 1 1 calc R . . C19 C 0.1470(2) 0.4901(3) 0.9511(2) 0.0209(8) Uani 1 1 d . . . C20 C 0.1021(2) 0.4378(2) 0.9957(3) 0.0225(10) Uani 1 1 d . . . C21 C 0.0515(3) 0.3852(3) 0.9599(3) 0.0366(12) Uani 1 1 d . . . H21 H 0.0232 0.3494 0.9931 0.044 Uiso 1 1 calc R . . C22 C 0.0435(3) 0.3864(4) 0.8735(3) 0.0451(13) Uani 1 1 d . . . H22 H 0.0094 0.3506 0.8470 0.054 Uiso 1 1 calc R . . C23 C 0.0850(3) 0.4394(3) 0.8257(3) 0.0479(15) Uani 1 1 d . . . H23 H 0.0784 0.4406 0.7669 0.057 Uiso 1 1 calc R . . C24 C 0.1366(2) 0.4911(3) 0.8643(2) 0.0344(11) Uani 1 1 d . . . H24 H 0.1649 0.5271 0.8313 0.041 Uiso 1 1 calc R . . H1 H 0.501(3) 0.3865(18) 1.1106(15) 0.041 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01151(10) 0.01483(10) 0.01564(11) 0.00274(10) 0.00215(7) -0.00032(8) O1 0.0119(12) 0.0148(13) 0.0155(12) 0.0021(10) -0.0021(17) -0.0030(11) O2 0.0304(16) 0.0195(15) 0.0129(14) -0.0009(12) 0.0024(12) -0.0072(13) O3 0.0233(15) 0.0142(13) 0.0209(15) 0.0001(12) 0.0042(13) 0.0015(12) O4 0.034(2) 0.0345(18) 0.0437(18) 0.0054(15) 0.0008(16) -0.0102(16) O5 0.045(2) 0.051(2) 0.060(2) 0.0152(18) -0.022(2) 0.0087(19) O6 0.0169(13) 0.0177(14) 0.0258(13) 0.0030(13) 0.0013(11) -0.0008(12) O7 0.0208(15) 0.0157(14) 0.0242(15) 0.0039(11) -0.0031(12) 0.0011(12) O8 0.0432(18) 0.0290(17) 0.0313(15) -0.0070(18) 0.0106(13) -0.0111(19) O9 0.060(2) 0.036(2) 0.0412(19) 0.0043(17) 0.0071(18) -0.0077(18) N1 0.034(2) 0.0208(19) 0.035(2) -0.0065(18) -0.0090(19) 0.0049(17) N2 0.0251(19) 0.029(2) 0.030(2) -0.0010(18) 0.0070(17) -0.0086(15) C1 0.0167(19) 0.0152(19) 0.017(2) -0.0004(17) 0.0042(15) -0.0032(16) C2 0.024(2) 0.016(2) 0.013(2) 0.0002(17) -0.0005(17) 0.0038(17) C3 0.0169(19) 0.019(2) 0.0180(19) 0.0003(17) -0.0019(16) 0.0051(18) C4 0.052(3) 0.018(2) 0.027(3) -0.0045(18) 0.001(2) 0.002(2) C5 0.069(3) 0.014(2) 0.026(2) -0.002(3) 0.000(2) -0.005(2) C6 0.051(3) 0.018(2) 0.017(2) -0.0066(18) -0.001(2) 0.000(2) C7 0.032(2) 0.015(2) 0.0079(19) -0.0014(16) 0.0066(17) -0.0052(18) C8 0.032(2) 0.021(2) 0.017(2) -0.0023(17) 0.0001(18) -0.0029(19) C9 0.047(3) 0.022(2) 0.018(2) 0.0011(19) 0.000(2) -0.002(2) C10 0.052(3) 0.019(2) 0.023(2) 0.0023(19) 0.012(2) -0.006(2) C11 0.032(3) 0.031(2) 0.021(2) -0.003(2) 0.011(2) -0.013(2) C12 0.025(2) 0.023(2) 0.016(2) -0.0015(17) 0.0047(17) -0.0064(19) C13 0.013(2) 0.027(2) 0.015(2) -0.0042(17) 0.0026(16) 0.0009(17) C14 0.019(2) 0.023(2) 0.0136(19) 0.0047(17) 0.0064(16) 0.0056(18) C15 0.017(2) 0.021(2) 0.0149(19) 0.0013(17) 0.0067(17) 0.0084(17) C16 0.028(2) 0.016(2) 0.019(2) 0.0012(17) 0.0076(18) 0.0046(18) C17 0.028(2) 0.026(2) 0.033(2) 0.011(2) 0.0086(19) 0.0184(19) C18 0.015(2) 0.039(2) 0.027(2) 0.010(2) 0.0016(19) 0.0063(17) C19 0.0148(18) 0.028(2) 0.0200(18) -0.0057(19) 0.0024(15) 0.0002(18) C20 0.016(2) 0.030(2) 0.021(2) -0.0045(18) 0.0015(17) 0.0014(19) C21 0.021(2) 0.043(3) 0.046(3) -0.010(2) 0.001(2) -0.009(2) C22 0.029(3) 0.063(4) 0.044(3) -0.016(3) -0.007(2) -0.014(3) C23 0.041(3) 0.075(4) 0.028(3) -0.016(3) -0.009(3) -0.004(3) C24 0.029(2) 0.051(3) 0.023(2) 0.001(3) -0.0014(18) -0.006(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 Gd1 O6 2.288(2) . ? Gd1 O2 2.316(3) . ? Gd1 O3 2.333(3) . ? Gd1 O1 2.344(3) . ? Gd1 O1 2.385(2) 2_567 ? Gd1 O7 2.404(3) . ? Gd1 O1 2.441(3) 3_665 ? Gd1 O7 2.949(3) 4_657 ? Gd1 Gd1 3.6830(5) 2_567 ? Gd1 Gd1 3.6830(5) 4_657 ? Gd1 Gd1 3.9588(7) 3_665 ? O1 Gd1 2.385(2) 4_657 ? O1 Gd1 2.441(3) 3_665 ? O1 H1 0.909(9) . ? O2 C1 1.278(5) . ? O3 C3 1.264(5) . ? O4 N1 1.227(5) . ? O5 N1 1.234(5) . ? O6 C13 1.299(5) . ? O7 C15 1.265(5) . ? O7 Gd1 2.949(3) 2_567 ? O8 N2 1.227(5) . ? O9 N2 1.241(5) . ? N1 C8 1.470(6) . ? N2 C20 1.469(6) . ? C1 C2 1.390(5) . ? C1 C7 1.509(5) . ? C2 C3 1.406(6) . ? C2 C6 1.507(6) . ? C3 C4 1.508(6) . ? C4 C5 1.534(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.543(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.391(6) . ? C7 C12 1.398(6) . ? C8 C9 1.385(6) . ? C9 C10 1.401(7) . ? C9 H9 0.9500 . ? C10 C11 1.379(7) . ? C10 H10 0.9500 . ? C11 C12 1.399(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.392(6) . ? C13 C19 1.496(6) . ? C14 C15 1.394(6) . ? C14 C18 1.526(5) . ? C15 C16 1.518(5) . ? C16 C17 1.523(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.538(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.384(6) . ? C19 C24 1.402(5) . ? C20 C21 1.380(6) . ? C21 C22 1.390(7) . ? C21 H21 0.9500 . ? C22 C23 1.389(8) . ? C22 H22 0.9500 . ? C23 C24 1.401(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Gd1 O2 81.76(10) . . ? O6 Gd1 O3 107.48(9) . . ? O2 Gd1 O3 74.95(9) . . ? O6 Gd1 O1 141.98(9) . . ? O2 Gd1 O1 83.28(9) . . ? O3 Gd1 O1 101.99(9) . . ? O6 Gd1 O1 89.37(8) . 2_567 ? O2 Gd1 O1 132.80(9) . 2_567 ? O3 Gd1 O1 150.37(9) . 2_567 ? O1 Gd1 O1 75.79(9) . 2_567 ? O6 Gd1 O7 74.26(9) . . ? O2 Gd1 O7 143.31(9) . . ? O3 Gd1 O7 86.13(9) . . ? O1 Gd1 O7 132.00(9) . . ? O1 Gd1 O7 74.98(9) 2_567 . ? O6 Gd1 O1 141.16(9) . 3_665 ? O2 Gd1 O1 134.96(9) . 3_665 ? O3 Gd1 O1 77.80(8) . 3_665 ? O1 Gd1 O1 68.15(9) . 3_665 ? O1 Gd1 O1 74.00(9) 2_567 3_665 ? O7 Gd1 O1 67.65(9) . 3_665 ? O6 Gd1 O7 76.56(9) . 4_657 ? O2 Gd1 O7 73.22(8) . 4_657 ? O3 Gd1 O7 146.94(8) . 4_657 ? O1 Gd1 O7 65.68(8) . 4_657 ? O1 Gd1 O7 59.65(8) 2_567 4_657 ? O7 Gd1 O7 125.49(3) . 4_657 ? O1 Gd1 O7 120.24(7) 3_665 4_657 ? O6 Gd1 Gd1 108.88(6) . 2_567 ? O2 Gd1 Gd1 163.66(7) . 2_567 ? O3 Gd1 Gd1 111.97(7) . 2_567 ? O1 Gd1 Gd1 80.79(6) . 2_567 ? O1 Gd1 Gd1 38.45(6) 2_567 2_567 ? O7 Gd1 Gd1 53.03(6) . 2_567 ? O1 Gd1 Gd1 39.69(5) 3_665 2_567 ? O7 Gd1 Gd1 96.73(5) 4_657 2_567 ? O6 Gd1 Gd1 110.29(6) . 4_657 ? O2 Gd1 Gd1 100.00(7) . 4_657 ? O3 Gd1 Gd1 140.70(7) . 4_657 ? O1 Gd1 Gd1 39.24(5) . 4_657 ? O1 Gd1 Gd1 40.82(6) 2_567 4_657 ? O7 Gd1 Gd1 114.10(6) . 4_657 ? O1 Gd1 Gd1 79.66(5) 3_665 4_657 ? O7 Gd1 Gd1 40.65(5) 4_657 4_657 ? Gd1 Gd1 Gd1 65.019(9) 2_567 4_657 ? O6 Gd1 Gd1 163.79(6) . 3_665 ? O2 Gd1 Gd1 109.72(7) . 3_665 ? O3 Gd1 Gd1 86.98(7) . 3_665 ? O1 Gd1 Gd1 34.97(6) . 3_665 ? O1 Gd1 Gd1 74.44(5) 2_567 3_665 ? O7 Gd1 Gd1 100.14(6) . 3_665 ? O1 Gd1 Gd1 33.39(6) 3_665 3_665 ? O7 Gd1 Gd1 95.43(5) 4_657 3_665 ? Gd1 Gd1 Gd1 57.491(5) 2_567 3_665 ? Gd1 Gd1 Gd1 57.491(4) 4_657 3_665 ? Gd1 O1 Gd1 102.31(9) . 4_657 ? Gd1 O1 Gd1 111.64(9) . 3_665 ? Gd1 O1 Gd1 99.49(9) 4_657 3_665 ? Gd1 O1 H1 110(3) . . ? Gd1 O1 H1 122(2) 4_657 . ? Gd1 O1 H1 111(4) 3_665 . ? C1 O2 Gd1 135.3(2) . . ? C3 O3 Gd1 132.6(2) . . ? C13 O6 Gd1 135.4(2) . . ? C15 O7 Gd1 130.6(2) . . ? C15 O7 Gd1 119.1(2) . 2_567 ? Gd1 O7 Gd1 86.32(8) . 2_567 ? O4 N1 O5 123.7(4) . . ? O4 N1 C8 118.9(4) . . ? O5 N1 C8 117.3(4) . . ? O8 N2 O9 124.0(4) . . ? O8 N2 C20 117.9(4) . . ? O9 N2 C20 118.1(4) . . ? O2 C1 C2 124.9(4) . . ? O2 C1 C7 115.3(3) . . ? C2 C1 C7 119.8(3) . . ? C1 C2 C3 123.5(4) . . ? C1 C2 C6 125.6(4) . . ? C3 C2 C6 110.9(4) . . ? O3 C3 C2 128.1(4) . . ? O3 C3 C4 122.1(3) . . ? C2 C3 C4 109.8(3) . . ? C3 C4 C5 103.8(3) . . ? C3 C4 H4A 111.0 . . ? C5 C4 H4A 111.0 . . ? C3 C4 H4B 111.0 . . ? C5 C4 H4B 111.0 . . ? H4A C4 H4B 109.0 . . ? C4 C5 C6 105.9(4) . . ? C4 C5 H5A 110.6 . . ? C6 C5 H5A 110.6 . . ? C4 C5 H5B 110.6 . . ? C6 C5 H5B 110.6 . . ? H5A C5 H5B 108.7 . . ? C2 C6 C5 103.5(4) . . ? C2 C6 H6A 111.1 . . ? C5 C6 H6A 111.1 . . ? C2 C6 H6B 111.1 . . ? C5 C6 H6B 111.1 . . ? H6A C6 H6B 109.0 . . ? C8 C7 C12 117.5(4) . . ? C8 C7 C1 123.2(4) . . ? C12 C7 C1 119.3(4) . . ? C9 C8 C7 122.8(4) . . ? C9 C8 N1 117.7(4) . . ? C7 C8 N1 119.4(4) . . ? C8 C9 C10 118.5(4) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 119.9(4) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.5(4) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C7 C12 C11 120.6(4) . . ? C7 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? O6 C13 C14 124.1(4) . . ? O6 C13 C19 112.6(3) . . ? C14 C13 C19 123.3(4) . . ? C13 C14 C15 123.3(4) . . ? C13 C14 C18 126.8(4) . . ? C15 C14 C18 109.7(4) . . ? O7 C15 C14 128.7(4) . . ? O7 C15 C16 120.9(4) . . ? C14 C15 C16 110.4(3) . . ? C15 C16 C17 103.9(3) . . ? C15 C16 H16A 111.0 . . ? C17 C16 H16A 111.0 . . ? C15 C16 H16B 111.0 . . ? C17 C16 H16B 111.0 . . ? H16A C16 H16B 109.0 . . ? C16 C17 C18 105.6(3) . . ? C16 C17 H17A 110.6 . . ? C18 C17 H17A 110.6 . . ? C16 C17 H17B 110.6 . . ? C18 C17 H17B 110.6 . . ? H17A C17 H17B 108.7 . . ? C14 C18 C17 103.0(3) . . ? C14 C18 H18A 111.2 . . ? C17 C18 H18A 111.2 . . ? C14 C18 H18B 111.2 . . ? C17 C18 H18B 111.2 . . ? H18A C18 H18B 109.1 . . ? C20 C19 C24 116.6(4) . . ? C20 C19 C13 123.2(3) . . ? C24 C19 C13 119.4(4) . . ? C21 C20 C19 124.3(4) . . ? C21 C20 N2 116.4(4) . . ? C19 C20 N2 119.4(3) . . ? C20 C21 C22 117.9(5) . . ? C20 C21 H21 121.1 . . ? C22 C21 H21 121.1 . . ? C23 C22 C21 120.4(5) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.0(5) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.7(5) . . ? C23 C24 H24 119.6 . . ? C19 C24 H24 119.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O4 0.909(9) 2.646(9) 3.532(4) 165(3) . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.393 _refine_diff_density_min -0.881 _refine_diff_density_rms 0.074 # Attachment 'wge049d.cif' data_wge049d _database_code_depnum_ccdc_archive 'CCDC 801777' #TrackingRef 'wge049d.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C120 H87 Er4 N8 038, 2(C7 H8)' _chemical_formula_sum 'C134 H99 Er4 N8 O38' _chemical_formula_weight 3098.25 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 17.260(4) _cell_length_b 19.361(4) _cell_length_c 22.261(5) _cell_angle_alpha 87.89(3) _cell_angle_beta 71.93(3) _cell_angle_gamma 67.01(3) _cell_volume 6480(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 63355 _cell_measurement_theta_min 1.25 _cell_measurement_theta_max 47.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3070 _exptl_absorpt_coefficient_mu 2.648 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.773747856 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Australian synchrotron MX1' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63355 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16615 _reflns_number_gt 12987 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _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. Ligand 7 was constrained to be the same as ligand 2. Ligand 6 is disordered with the nitro group residing on one phenyl ring with 76.5% occupancy and on the other with 24.5% occupancy. There are three isolated toluene solvent molecules; two have 50% occupancies each and the third is disordered over two positions 70: 30 % occupancies. All three molecules were refined isotropically as perfect hexagons. Additionally the methyl group in the first molecules was fixed at an idealised distance to the ring. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0866P)^2^+76.5495P] 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 0.00273(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 16615 _refine_ls_number_parameters 1624 _refine_ls_number_restraints 53 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1770 _refine_ls_wR_factor_gt 0.1640 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.82112(4) 0.63895(2) 0.27443(2) 0.040 Uani 1 1 d . . . Er2 Er 0.65769(4) 0.82566(3) 0.24310(2) 0.053 Uani 1 1 d . . . Er3 Er 0.82666(5) 0.80564(3) 0.32973(3) 0.058 Uani 1 1 d . . . Er4 Er 0.88513(5) 0.77151(3) 0.15108(3) 0.065 Uani 1 1 d . . . O1 O 0.7221(6) 0.7634(4) 0.3179(3) 0.049 Uani 1 1 d . . . H1 H 0.6768 0.7649 0.3593 0.059 Uiso 1 1 calc R . . O2 O 0.7843(5) 0.7153(4) 0.1942(3) 0.044 Uani 1 1 d . . . H2 H 0.7758 0.6882 0.1610 0.052 Uiso 1 1 calc R . . O3 O 0.7850(7) 0.8524(4) 0.2398(4) 0.067 Uani 1 1 d . . . H3 H 0.7755 0.9064 0.2352 0.081 Uiso 1 1 calc R . . O4 O 0.9055(6) 0.7133(4) 0.2455(4) 0.056 Uani 1 1 d . . . H4 H 0.9694 0.6853 0.2423 0.067 Uiso 1 1 calc R . . O5 O 0.7974(5) 0.5657(4) 0.2096(3) 0.045 Uani 1 1 d . . . O6 O 0.6895(6) 0.6332(4) 0.3311(3) 0.050 Uani 1 1 d . . . O7 O 0.7837(6) 0.6239(4) 0.0941(3) 0.059 Uani 1 1 d . . . O8 O 0.9172(7) 0.5387(5) 0.0666(4) 0.075 Uani 1 1 d . . . O9 O 0.9661(5) 0.5605(4) 0.2128(4) 0.055 Uani 1 1 d D . . C16 C 1.0107(8) 0.4877(6) 0.2071(5) 0.053 Uani 1 1 d D . . C17 C 1.0941(8) 0.4532(6) 0.1510(5) 0.052 Uani 1 1 d D . . C18 C 1.1768(8) 0.4568(6) 0.1441(6) 0.065 Uani 1 1 d D . . C19 C 1.2516(9) 0.4215(7) 0.0903(7) 0.077 Uani 1 1 d D . . H19 H 1.3062 0.4259 0.0852 0.092 Uiso 1 1 calc R . . C20 C 1.2430(10) 0.3794(7) 0.0442(6) 0.069 Uani 1 1 d D . . H20 H 1.2929 0.3541 0.0079 0.083 Uiso 1 1 calc R . . C21 C 1.1644(10) 0.3745(8) 0.0508(6) 0.071 Uani 1 1 d D . . H21 H 1.1601 0.3455 0.0194 0.085 Uiso 1 1 calc R . . C22 C 1.0902(9) 0.4117(7) 0.1031(6) 0.065 Uani 1 1 d D . . H22 H 1.0354 0.4087 0.1063 0.078 Uiso 1 1 calc R . . C23 C 0.9850(8) 0.4381(6) 0.2472(5) 0.055 Uani 1 1 d D . . H23 H 1.0205 0.3858 0.2365 0.066 Uiso 1 1 calc R . . C24 C 0.9111(7) 0.4595(5) 0.3018(5) 0.042 Uani 1 1 d D . . C25 C 0.8955(8) 0.3995(6) 0.3421(5) 0.055 Uani 1 1 d D . . C26 C 0.9652(9) 0.3325(5) 0.3448(5) 0.051 Uani 1 1 d D . . H26 H 1.0243 0.3227 0.3188 0.061 Uiso 1 1 calc R . . C27 C 0.9482(10) 0.2801(7) 0.3854(6) 0.068 Uani 1 1 d D . . H27 H 0.9961 0.2353 0.3878 0.082 Uiso 1 1 calc R . . C28 C 0.8645(12) 0.2923(10) 0.4215(10) 0.125 Uani 1 1 d D . . H28 H 0.8537 0.2559 0.4488 0.150 Uiso 1 1 calc R . . C29 C 0.7935(13) 0.3581(11) 0.4189(12) 0.168 Uani 1 1 d D . . H29 H 0.7343 0.3660 0.4434 0.202 Uiso 1 1 calc R . . C30 C 0.8103(10) 0.4127(10) 0.3797(9) 0.117 Uani 1 1 d D . . H30 H 0.7627 0.4587 0.3791 0.140 Uiso 1 1 calc R . . O10 O 0.8567(5) 0.5266(4) 0.3203(3) 0.046 Uani 1 1 d D . . N2 N 1.1878(9) 0.4928(7) 0.1971(7) 0.091 Uani 1 1 d D . . O11 O 1.1305(6) 0.5135(5) 0.2466(5) 0.080 Uani 1 1 d D . . O12 O 1.2605(9) 0.4951(10) 0.1886(7) 0.146 Uani 1 1 d D . . O13 O 0.5390(6) 0.8421(4) 0.3340(4) 0.057 Uani 1 1 d . . . O14 O 0.6040(6) 0.7397(4) 0.2283(4) 0.052 Uani 1 1 d . . . O15 O 0.5302(9) 0.9355(6) 0.4550(5) 0.106 Uani 1 1 d . . . O16 O 0.5809(7) 0.8134(5) 0.4445(4) 0.080 Uani 1 1 d . . . O17 O 0.6035(7) 0.9538(4) 0.2799(4) 0.067 Uani 1 1 d . . . O18 O 0.5370(8) 0.8888(4) 0.2090(4) 0.084 Uani 1 1 d . . . O19 O 0.6339(10) 1.0817(6) 0.2120(5) 0.115 Uani 1 1 d . . . O20 O 0.7162(11) 1.0664(8) 0.2731(7) 0.135 Uani 1 1 d . . . O21 O 0.8429(6) 0.6803(4) 0.3716(4) 0.048 Uani 1 1 d . . . O22 O 0.7922(7) 0.8257(4) 0.4361(4) 0.064 Uani 1 1 d . . . O23 O 0.7020(6) 0.6483(5) 0.4852(5) 0.072 Uani 1 1 d . . . O24 O 0.6919(10) 0.5602(7) 0.5415(8) 0.159 Uani 1 1 d . . . O25 O 0.9696(7) 0.7468(5) 0.3398(4) 0.064 Uani 1 1 d . . . O26 O 0.8857(8) 0.8930(5) 0.3149(5) 0.086 Uani 1 1 d . . . O27 O 1.0262(14) 0.8065(11) 0.4867(9) 0.108 Uani 0.65 1 d P A 1 O27A O 0.967(3) 0.968(2) 0.457(2) 0.114 Uani 0.35 1 d P A 2 O28 O 1.1434(13) 0.8333(11) 0.4455(13) 0.134 Uani 0.65 1 d P A 1 O28A O 1.097(3) 0.9467(19) 0.4051(18) 0.101 Uani 0.35 1 d P A 2 O29 O 1.0049(10) 0.7818(8) 0.1609(6) 0.125 Uani 1 1 d D . . C91 C 1.0380(12) 0.8344(10) 0.1546(10) 0.109 Uani 1 1 d D . . C92 C 1.1143(12) 0.8169(11) 0.1797(10) 0.121 Uani 1 1 d D . . C93 C 1.1750(13) 0.7394(11) 0.1780(8) 0.124 Uani 1 1 d D . . C94 C 1.2429(15) 0.7165(14) 0.2049(10) 0.155 Uani 1 1 d D . . H94 H 1.2805 0.6653 0.2049 0.186 Uiso 1 1 calc R . . C95 C 1.2505(15) 0.7787(14) 0.2330(11) 0.148 Uani 1 1 d D . . H95 H 1.2968 0.7673 0.2510 0.177 Uiso 1 1 calc R . . C96 C 1.1956(16) 0.8527(15) 0.2354(14) 0.177 Uani 1 1 d D . . H96 H 1.2045 0.8909 0.2544 0.212 Uiso 1 1 calc R . . C97 C 1.1261(15) 0.8720(13) 0.2097(13) 0.157 Uani 1 1 d D . . H97 H 1.0866 0.9233 0.2129 0.188 Uiso 1 1 calc R . . C98 C 1.0031(13) 0.9026(10) 0.1301(10) 0.129 Uani 1 1 d D . . H98 H 1.0347 0.9343 0.1240 0.155 Uiso 1 1 calc R . . C99 C 0.9266(13) 0.9279(9) 0.1142(8) 0.113 Uani 1 1 d D . . C100 C 0.8978(14) 1.0017(8) 0.0870(9) 0.125 Uani 1 1 d D . . C101 C 0.8438(18) 1.0132(11) 0.0487(10) 0.176 Uani 1 1 d D . . H101 H 0.8252 0.9746 0.0423 0.212 Uiso 1 1 calc R . . C102 C 0.8164(19) 1.0795(10) 0.0197(12) 0.200 Uani 1 1 d D . . H102 H 0.7747 1.0881 -0.0022 0.240 Uiso 1 1 calc R . . C103 C 0.850(2) 1.1318(14) 0.0229(14) 0.279 Uani 1 1 d D . . H103 H 0.8401 1.1728 -0.0026 0.335 Uiso 1 1 calc R . . C104 C 0.8991(19) 1.1243(11) 0.0647(14) 0.190 Uani 1 1 d D . . H104 H 0.9116 1.1652 0.0750 0.228 Uiso 1 1 calc R . . C105 C 0.930(2) 1.0552(14) 0.0910(14) 0.242 Uani 1 1 d D . . H105 H 0.9728 1.0457 0.1116 0.290 Uiso 1 1 calc R . . O30 O 0.8843(8) 0.8872(6) 0.1177(4) 0.094 Uani 1 1 d D . . N7 N 1.172(2) 0.6781(18) 0.1404(12) 0.526 Uani 1 1 d D . . O31 O 1.1725(12) 0.6885(12) 0.0886(8) 0.183 Uani 1 1 d D . . O32 O 1.131(3) 0.6482(19) 0.1813(13) 0.352 Uani 1 1 d D . . O33 O 0.7406(7) 0.8390(4) 0.1330(4) 0.072 Uani 1 1 d . . . O34 O 0.9131(7) 0.7500(5) 0.0435(4) 0.070 Uani 1 1 d . . . O35 O 0.6391(8) 0.7850(6) 0.0664(5) 0.097 Uani 1 1 d . . . O36 O 0.5446(12) 0.8338(12) 0.0157(9) 0.204 Uani 1 1 d . . . O37 O 0.6941(7) 0.9216(4) 0.3692(4) 0.070 Uani 1 1 d . . . O38 O 0.9853(6) 0.6429(5) 0.1130(4) 0.068 Uani 1 1 d . . . N1 N 0.8367(8) 0.5573(6) 0.0867(4) 0.063 Uani 1 1 d . . . N3 N 0.5218(9) 0.8757(7) 0.4517(5) 0.081 Uani 1 1 d . . . N4 N 0.6467(12) 1.0839(6) 0.2637(7) 0.096 Uani 1 1 d . . . N5 N 0.7368(9) 0.5882(6) 0.5036(6) 0.087 Uani 1 1 d . . . N6 N 1.1028(16) 0.7938(14) 0.4475(11) 0.095 Uani 0.65 1 d P A 1 N6A N 1.015(3) 0.975(2) 0.407(2) 0.089 Uani 0.35 1 d P A 2 N8 N 0.5889(11) 0.8403(10) 0.0474(8) 0.131 Uani 1 1 d . . . C1 C 0.7411(9) 0.5371(6) 0.2164(6) 0.053 Uani 1 1 d . . . C2 C 0.7490(11) 0.4925(8) 0.1589(7) 0.072 Uani 1 1 d . . . C3 C 0.7997(11) 0.4993(7) 0.0985(6) 0.073 Uani 1 1 d . . . C4 C 0.8153(15) 0.4563(9) 0.0425(8) 0.106 Uani 1 1 d . . . H9 H 0.8511 0.4621 0.0022 0.128 Uiso 1 1 calc R . . C5 C 0.776(2) 0.4056(11) 0.0495(11) 0.146 Uani 1 1 d . . . H5 H 0.7857 0.3745 0.0135 0.175 Uiso 1 1 calc R . . C6 C 0.722(2) 0.3992(14) 0.1084(11) 0.165 Uani 1 1 d . . . H6 H 0.6927 0.3656 0.1124 0.198 Uiso 1 1 calc R . . C7 C 0.7096(16) 0.4434(11) 0.1624(9) 0.118 Uani 1 1 d . . . H7 H 0.6727 0.4384 0.2026 0.141 Uiso 1 1 calc R . . C8 C 0.6711(10) 0.5443(8) 0.2727(6) 0.065 Uani 1 1 d . . . H8 H 0.6375 0.5150 0.2740 0.078 Uiso 1 1 calc R . . C9 C 0.6479(9) 0.5929(7) 0.3277(6) 0.054 Uani 1 1 d . . . C10 C 0.5713(10) 0.5968(10) 0.3851(7) 0.076 Uani 1 1 d . . . C11 C 0.5431(12) 0.6517(13) 0.4327(8) 0.114 Uani 1 1 d . . . H11 H 0.5723 0.6852 0.4279 0.137 Uiso 1 1 calc R . . C12 C 0.4726(17) 0.661(2) 0.4884(11) 0.212 Uani 1 1 d . . . H12 H 0.4576 0.6964 0.5228 0.255 Uiso 1 1 calc R . . C13 C 0.429(2) 0.619(3) 0.4911(11) 0.235 Uani 1 1 d . . . H13 H 0.3749 0.6317 0.5252 0.281 Uiso 1 1 calc R . . C14 C 0.4551(17) 0.557(2) 0.4470(11) 0.173 Uani 1 1 d . . . H14 H 0.4267 0.5223 0.4543 0.208 Uiso 1 1 calc R . . C15 C 0.5288(14) 0.5488(14) 0.3903(9) 0.121 Uani 1 1 d . . . H15 H 0.5475 0.5108 0.3569 0.145 Uiso 1 1 calc R . . C31 C 0.4803(9) 0.8171(7) 0.3498(6) 0.062 Uani 1 1 d . . . C32 C 0.4112(11) 0.8492(8) 0.4155(7) 0.079 Uani 1 1 d . . . C33 C 0.4319(11) 0.8793(7) 0.4623(6) 0.077 Uani 1 1 d . . . C34 C 0.3716(12) 0.9133(8) 0.5205(7) 0.087 Uani 1 1 d . . . H34 H 0.3881 0.9355 0.5492 0.105 Uiso 1 1 calc R . . C35 C 0.2879(14) 0.9149(9) 0.5369(7) 0.103 Uani 1 1 d . . . H35 H 0.2468 0.9366 0.5778 0.124 Uiso 1 1 calc R . . C36 C 0.2620(11) 0.8846(10) 0.4935(8) 0.098 Uani 1 1 d . . . H36 H 0.2034 0.8863 0.5049 0.117 Uiso 1 1 calc R . . C37 C 0.3244(12) 0.8515(9) 0.4326(7) 0.093 Uani 1 1 d . . . H37 H 0.3074 0.8307 0.4033 0.112 Uiso 1 1 calc R . . C38 C 0.4719(9) 0.7648(8) 0.3145(6) 0.068 Uani 1 1 d . . . H38 H 0.4218 0.7522 0.3314 0.081 Uiso 1 1 calc R . . C39 C 0.5340(9) 0.7285(6) 0.2545(6) 0.056 Uani 1 1 d . . . C40 C 0.5166(10) 0.6743(9) 0.2198(7) 0.074 Uani 1 1 d . . . C41 C 0.5568(11) 0.6638(11) 0.1523(8) 0.101 Uani 1 1 d . . . H41 H 0.5925 0.6896 0.1305 0.121 Uiso 1 1 calc R . . C42 C 0.5396(16) 0.6126(15) 0.1204(10) 0.149 Uani 1 1 d . . . H42 H 0.5635 0.6048 0.0754 0.178 Uiso 1 1 calc R . . C43 C 0.4909(16) 0.5741(15) 0.1509(10) 0.161 Uani 1 1 d . . . H43 H 0.4800 0.5415 0.1268 0.194 Uiso 1 1 calc R . . C44 C 0.4561(14) 0.5811(15) 0.2171(10) 0.147 Uani 1 1 d . . . H44 H 0.4272 0.5501 0.2385 0.176 Uiso 1 1 calc R . . C45 C 0.4653(11) 0.6348(10) 0.2502(8) 0.094 Uani 1 1 d . . . H45 H 0.4360 0.6450 0.2947 0.113 Uiso 1 1 calc R . . C46 C 0.5239(10) 1.0045(6) 0.2939(6) 0.065 Uani 1 1 d . . . C47 C 0.5058(9) 1.0746(6) 0.3333(6) 0.057 Uani 1 1 d . . . C48 C 0.5644(10) 1.1104(6) 0.3208(6) 0.070 Uani 1 1 d . . . C49 C 0.5491(10) 1.1749(6) 0.3563(6) 0.067 Uani 1 1 d . . . H49 H 0.5910 1.1975 0.3463 0.080 Uiso 1 1 calc R . . C50 C 0.4710(9) 1.2051(7) 0.4065(6) 0.060 Uani 1 1 d . . . H50 H 0.4586 1.2492 0.4314 0.072 Uiso 1 1 calc R . . C51 C 0.4113(10) 1.1721(7) 0.4208(6) 0.060 Uani 1 1 d . . . H51 H 0.3579 1.1935 0.4555 0.072 Uiso 1 1 calc R . . C52 C 0.4281(10) 1.1069(6) 0.3848(5) 0.058 Uani 1 1 d . . . H52 H 0.3861 1.0845 0.3955 0.070 Uiso 1 1 calc R . . C53 C 0.4560(11) 1.0039(7) 0.2748(6) 0.075 Uani 1 1 d . . . H53 H 0.3996 1.0444 0.2916 0.090 Uiso 1 1 calc R . . C54 C 0.4632(13) 0.9473(7) 0.2319(7) 0.097 Uani 1 1 d . . . C55 C 0.3940(15) 0.9556(9) 0.2056(9) 0.125 Uani 1 1 d . . . C56 C 0.4071(15) 0.8905(10) 0.1696(10) 0.117 Uani 1 1 d . . . H56 H 0.4563 0.8440 0.1656 0.140 Uiso 1 1 calc R . . C57 C 0.3429(17) 0.8988(11) 0.1400(12) 0.152 Uani 1 1 d . . . H57 H 0.3468 0.8556 0.1183 0.182 Uiso 1 1 calc R . . C58 C 0.2726(19) 0.9695(13) 0.1415(14) 0.167 Uani 1 1 d . . . H58 H 0.2332 0.9747 0.1182 0.201 Uiso 1 1 calc R . . C59 C 0.263(2) 1.0314(12) 0.1785(13) 0.189 Uani 1 1 d . . . H59 H 0.2144 1.0783 0.1828 0.226 Uiso 1 1 calc R . . C60 C 0.3237(14) 1.0243(9) 0.2081(9) 0.118 Uani 1 1 d . . . H60 H 0.3179 1.0674 0.2311 0.142 Uiso 1 1 calc R . . C61 C 0.8538(9) 0.6608(6) 0.4250(5) 0.051 Uani 1 1 d . . . C62 C 0.8871(9) 0.5768(6) 0.4350(5) 0.052 Uani 1 1 d . . . C63 C 0.8343(9) 0.5450(6) 0.4773(6) 0.063 Uani 1 1 d . . . C64 C 0.8687(11) 0.4726(6) 0.4930(6) 0.072 Uani 1 1 d . . . H64 H 0.8311 0.4527 0.5218 0.086 Uiso 1 1 calc R . . C65 C 0.9576(11) 0.4293(7) 0.4669(7) 0.073 Uani 1 1 d . . . H65 H 0.9820 0.3794 0.4780 0.088 Uiso 1 1 calc R . . C66 C 1.0127(9) 0.4587(7) 0.4236(6) 0.062 Uani 1 1 d . . . H66 H 1.0745 0.4290 0.4051 0.074 Uiso 1 1 calc R . . C67 C 0.9750(10) 0.5329(7) 0.4082(6) 0.062 Uani 1 1 d . . . H67 H 1.0117 0.5528 0.3784 0.074 Uiso 1 1 calc R . . C68 C 0.8494(9) 0.7069(6) 0.4741(6) 0.053 Uani 1 1 d . . . H68 H 0.8687 0.6828 0.5079 0.064 Uiso 1 1 calc R . . C69 C 0.8193(10) 0.7851(6) 0.4775(6) 0.056 Uani 1 1 d . . . C70 C 0.8163(8) 0.8277(6) 0.5346(6) 0.054 Uani 1 1 d . . . C71 C 0.8127(11) 0.7988(7) 0.5925(7) 0.071 Uani 1 1 d . . . H71 H 0.8112 0.7504 0.5978 0.085 Uiso 1 1 calc R . . C72 C 0.8112(11) 0.8397(7) 0.6432(7) 0.083 Uani 1 1 d . . . H72 H 0.8091 0.8190 0.6827 0.100 Uiso 1 1 calc R . . C73 C 0.8128(11) 0.9111(8) 0.6359(8) 0.086 Uani 1 1 d . . . H73 H 0.8123 0.9392 0.6702 0.103 Uiso 1 1 calc R . . C74 C 0.8152(12) 0.9398(9) 0.5791(9) 0.093 Uani 1 1 d . . . H74 H 0.8172 0.9880 0.5737 0.112 Uiso 1 1 calc R . . C75 C 0.8148(11) 0.8994(7) 0.5283(8) 0.075 Uani 1 1 d . . . H75 H 0.8135 0.9214 0.4895 0.090 Uiso 1 1 calc R . . C76 C 1.0201(10) 0.7720(7) 0.3524(6) 0.063 Uani 1 1 d . . . C77 C 1.1041(10) 0.7124(7) 0.3621(6) 0.059 Uani 1 1 d . A . C78 C 1.1496(13) 0.7279(9) 0.3980(8) 0.089 Uani 1 1 d . . . C79 C 1.2303(13) 0.6733(10) 0.4023(8) 0.092 Uani 1 1 d . A . H79 H 1.2596 0.6849 0.4278 0.110 Uiso 1 1 calc R . . C80 C 1.2661(10) 0.6040(8) 0.3698(7) 0.071 Uani 1 1 d . . . H80 H 1.3217 0.5675 0.3707 0.086 Uiso 1 1 calc R A . C81 C 1.2203(11) 0.5878(9) 0.3355(7) 0.075 Uani 1 1 d . A . H81 H 1.2437 0.5390 0.3138 0.090 Uiso 1 1 calc R . . C82 C 1.1400(10) 0.6420(8) 0.3323(6) 0.067 Uani 1 1 d . . . H82 H 1.1097 0.6291 0.3084 0.081 Uiso 1 1 calc R A . C83 C 1.0111(12) 0.8454(8) 0.3501(8) 0.080 Uani 1 1 d . . . H83 H 1.0531 0.8584 0.3609 0.096 Uiso 1 1 calc R . . C84 C 0.9431(12) 0.9034(8) 0.3325(8) 0.081 Uani 1 1 d . . . C85 C 0.9438(13) 0.9811(9) 0.3297(9) 0.090 Uani 1 1 d . A . C86 C 0.9738(13) 1.0114(8) 0.3685(9) 0.092 Uani 1 1 d . . . C87 C 0.9754(14) 1.0811(9) 0.3604(11) 0.113 Uani 1 1 d . A . H87 H 0.9985 1.1007 0.3861 0.135 Uiso 1 1 calc R . . C88 C 0.9441(17) 1.1232(10) 0.3157(12) 0.133 Uani 1 1 d . . . H88 H 0.9438 1.1723 0.3115 0.160 Uiso 1 1 calc R A . C89 C 0.9139(17) 1.0956(10) 0.2781(12) 0.133 Uani 1 1 d . A . H89 H 0.8944 1.1243 0.2461 0.159 Uiso 1 1 calc R . . C90 C 0.9109(15) 1.0238(9) 0.2856(10) 0.116 Uani 1 1 d . . . H90 H 0.8863 1.0053 0.2604 0.139 Uiso 1 1 calc R A . C106 C 0.7276(12) 0.8630(6) 0.0814(6) 0.086 Uani 1 1 d . . . C107 C 0.6398(14) 0.9253(8) 0.0858(7) 0.111 Uani 1 1 d . . . C108 C 0.5772(16) 0.9137(10) 0.0673(8) 0.141 Uani 1 1 d . . . C109 C 0.4989(17) 0.9752(13) 0.0652(9) 0.183 Uani 1 1 d . . . H109 H 0.4578 0.9667 0.0494 0.220 Uiso 1 1 calc R . . C110 C 0.484(2) 1.0430(15) 0.0852(10) 0.215 Uani 1 1 d . . . H110 H 0.4281 1.0831 0.0890 0.259 Uiso 1 1 calc R . . C111 C 0.547(2) 1.0574(10) 0.1009(9) 0.192 Uani 1 1 d . . . H111 H 0.5385 1.1079 0.1100 0.230 Uiso 1 1 calc R . . C112 C 0.625(2) 0.9971(8) 0.1034(7) 0.176 Uani 1 1 d . . . H112 H 0.6676 1.0065 0.1172 0.211 Uiso 1 1 calc R . . C113 C 0.7911(12) 0.8448(7) 0.0207(6) 0.081 Uani 1 1 d . . . H113 H 0.7740 0.8736 -0.0120 0.097 Uiso 1 1 calc R . . C114 C 0.8773(11) 0.7881(7) 0.0034(6) 0.067 Uani 1 1 d . . . C115 C 0.9351(12) 0.7702(8) -0.0645(7) 0.078 Uani 1 1 d . . . C116 C 1.0196(16) 0.7192(8) -0.0817(8) 0.121 Uani 1 1 d . . . H116 H 1.0437 0.6943 -0.0500 0.145 Uiso 1 1 calc R . . C117 C 1.0730(17) 0.7020(9) -0.1458(9) 0.143 Uani 1 1 d . . . H117 H 1.1322 0.6651 -0.1574 0.171 Uiso 1 1 calc R . . C118 C 1.0393(16) 0.7383(12) -0.1905(8) 0.113 Uani 1 1 d . . . H118 H 1.0743 0.7268 -0.2341 0.135 Uiso 1 1 calc R . . C119 C 0.9608(17) 0.788(2) -0.1742(11) 0.243 Uani 1 1 d . . . H119 H 0.9385 0.8153 -0.2057 0.291 Uiso 1 1 calc R . . C120 C 0.9060(15) 0.803(2) -0.1113(10) 0.221 Uani 1 1 d . . . H120 H 0.8461 0.8386 -0.1014 0.265 Uiso 1 1 calc R . . C121 C 0.6307(13) 0.2711(11) 0.2105(8) 0.078 Uiso 0.50 1 d PGD . . C122 C 0.5497(11) 0.3273(12) 0.2449(10) 0.089 Uiso 0.50 1 d PGD . . H122 H 0.4999 0.3408 0.2303 0.107 Uiso 0.50 1 calc PR . . C123 C 0.5414(10) 0.3637(10) 0.3006(9) 0.096 Uiso 0.50 1 d PG . . H123 H 0.4861 0.4021 0.3241 0.115 Uiso 0.50 1 calc PR . . C124 C 0.6142(13) 0.3439(11) 0.3220(8) 0.071 Uiso 0.50 1 d PG . . H124 H 0.6086 0.3687 0.3601 0.085 Uiso 0.50 1 calc PR . . C125 C 0.6952(11) 0.2877(11) 0.2877(9) 0.073 Uiso 0.50 1 d PG . . H125 H 0.7449 0.2742 0.3023 0.087 Uiso 0.50 1 calc PR . . C126 C 0.7034(10) 0.2513(10) 0.2319(8) 0.078 Uiso 0.50 1 d PGD . . H126 H 0.7588 0.2130 0.2084 0.094 Uiso 0.50 1 calc PR . . C127 C 0.641(2) 0.235(3) 0.1489(17) 0.198 Uiso 0.50 1 d PD . . H12A H 0.7019 0.1968 0.1311 0.297 Uiso 0.50 1 calc PR . . H12B H 0.6289 0.2730 0.1192 0.297 Uiso 0.50 1 calc PR . . H12C H 0.5991 0.2104 0.1560 0.297 Uiso 0.50 1 calc PR . . C128 C 0.7184(11) 0.6870(8) 0.7035(7) 0.083 Uiso 0.70 1 d PG B 1 C129 C 0.6401(9) 0.7512(10) 0.7256(9) 0.097 Uiso 0.70 1 d PG B 1 H129 H 0.5952 0.7624 0.7063 0.117 Uiso 0.70 1 calc PR B 1 C130 C 0.6276(10) 0.7990(9) 0.7760(9) 0.118 Uiso 0.70 1 d PG B 1 H130 H 0.5742 0.8428 0.7912 0.142 Uiso 0.70 1 calc PR B 1 C131 C 0.6934(13) 0.7825(9) 0.8043(8) 0.123 Uiso 0.70 1 d PG B 1 H131 H 0.6849 0.8152 0.8388 0.148 Uiso 0.70 1 calc PR B 1 C132 C 0.7716(11) 0.7184(10) 0.7822(8) 0.095 Uiso 0.70 1 d PG B 1 H132 H 0.8166 0.7071 0.8015 0.113 Uiso 0.70 1 calc PR B 1 C133 C 0.7841(9) 0.6706(7) 0.7318(7) 0.066 Uiso 0.70 1 d PG B 1 H133 H 0.8376 0.6267 0.7166 0.079 Uiso 0.70 1 calc PR B 1 C134 C 0.7270(18) 0.6371(15) 0.6495(12) 0.098 Uiso 0.70 1 d P B 1 H13A H 0.7849 0.5943 0.6381 0.147 Uiso 0.70 1 calc PR B 1 H13B H 0.7223 0.6659 0.6128 0.147 Uiso 0.70 1 calc PR B 1 H13C H 0.6795 0.6185 0.6625 0.147 Uiso 0.70 1 calc PR B 1 C135 C 0.5047(17) 0.3107(15) 0.0651(12) 0.113 Uiso 0.50 1 d PG . . C136 C 0.5757(19) 0.2622(12) 0.0157(14) 0.104 Uiso 0.50 1 d PG . . H136 H 0.5851 0.2106 0.0112 0.125 Uiso 0.50 1 calc PR . . C137 C 0.6328(16) 0.2891(15) -0.0270(12) 0.148 Uiso 0.50 1 d PG . . H137 H 0.6813 0.2560 -0.0607 0.178 Uiso 0.50 1 calc PR . . C138 C 0.6190(17) 0.3645(16) -0.0204(12) 0.117 Uiso 0.50 1 d PG . . H138 H 0.6580 0.3829 -0.0496 0.141 Uiso 0.50 1 calc PR . . C139 C 0.5480(18) 0.4130(12) 0.0290(13) 0.107 Uiso 0.50 1 d PG . . H139 H 0.5385 0.4645 0.0335 0.129 Uiso 0.50 1 calc PR . . C140 C 0.4908(15) 0.3861(14) 0.0717(11) 0.110 Uiso 0.50 1 d PG . . H140 H 0.4423 0.4192 0.1055 0.132 Uiso 0.50 1 calc PR . . C141 C 0.464(4) 0.290(3) 0.098(3) 0.183 Uiso 0.50 1 d P . . H14A H 0.4172 0.3306 0.1289 0.275 Uiso 0.50 1 calc PR . . H14B H 0.4998 0.2513 0.1195 0.275 Uiso 0.50 1 calc PR . . H14C H 0.4377 0.2667 0.0758 0.275 Uiso 0.50 1 calc PR . . C228 C 0.723(2) 0.7299(17) 0.7815(14) 0.058 Uiso 0.30 1 d PG C 2 C229 C 0.7704(16) 0.6619(15) 0.7434(15) 0.057 Uiso 0.30 1 d PG C 2 H229 H 0.8270 0.6291 0.7455 0.068 Uiso 0.30 1 calc PR C 2 C230 C 0.7347(19) 0.6418(14) 0.7023(14) 0.075 Uiso 0.30 1 d PG C 2 H230 H 0.7670 0.5954 0.6762 0.090 Uiso 0.30 1 calc PR C 2 C231 C 0.6518(19) 0.6898(17) 0.6992(14) 0.067 Uiso 0.30 1 d PG C 2 H231 H 0.6275 0.6761 0.6710 0.080 Uiso 0.30 1 calc PR C 2 C232 C 0.6046(16) 0.7578(16) 0.7373(16) 0.064 Uiso 0.30 1 d PG C 2 H232 H 0.5480 0.7906 0.7352 0.076 Uiso 0.30 1 calc PR C 2 C233 C 0.640(2) 0.7778(15) 0.7785(16) 0.102 Uiso 0.30 1 d PG C 2 H233 H 0.6080 0.8243 0.8045 0.123 Uiso 0.30 1 calc PR C 2 C234 C 0.767(3) 0.752(3) 0.825(2) 0.065 Uiso 0.30 1 d P C 2 H23A H 0.7260 0.8002 0.8498 0.097 Uiso 0.30 1 calc PR C 2 H23B H 0.8220 0.7561 0.7989 0.097 Uiso 0.30 1 calc PR C 2 H23C H 0.7810 0.7128 0.8541 0.097 Uiso 0.30 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.057 0.019 0.032 0.003 -0.011 -0.006 Er2 0.088 0.018 0.041 0.000 -0.028 -0.001 Er3 0.100 0.029 0.055 0.013 -0.038 -0.028 Er4 0.102 0.053 0.052 0.026 -0.030 -0.042 O1 0.077 0.022 0.037 0.002 -0.018 -0.008 O2 0.062 0.028 0.033 0.004 -0.015 -0.010 O3 0.117 0.027 0.056 0.012 -0.028 -0.028 O4 0.083 0.039 0.053 0.015 -0.026 -0.029 O5 0.062 0.028 0.032 0.004 -0.009 -0.009 O6 0.078 0.025 0.032 0.001 -0.010 -0.011 O7 0.082 0.034 0.034 -0.002 -0.017 0.004 O8 0.066 0.073 0.046 -0.012 -0.007 0.005 O9 0.063 0.027 0.042 0.004 -0.001 0.005 C16 0.049 0.048 0.043 0.009 -0.007 -0.006 C17 0.046 0.040 0.052 0.012 -0.014 -0.001 C18 0.066 0.032 0.064 -0.013 -0.001 0.000 C19 0.065 0.053 0.079 -0.011 0.006 -0.010 C20 0.091 0.046 0.035 -0.010 0.005 -0.008 C21 0.082 0.079 0.037 -0.002 -0.002 -0.030 C22 0.072 0.055 0.051 0.007 -0.011 -0.014 C23 0.065 0.025 0.048 0.006 -0.003 -0.002 C24 0.052 0.026 0.042 0.005 -0.018 -0.008 C25 0.078 0.033 0.034 0.008 -0.009 -0.009 C26 0.079 0.023 0.045 0.002 -0.025 -0.011 C27 0.101 0.032 0.052 0.008 -0.013 -0.016 C28 0.106 0.076 0.134 0.064 0.007 -0.016 C29 0.099 0.105 0.195 0.104 0.030 0.000 C30 0.072 0.089 0.119 0.071 0.009 0.004 O10 0.057 0.028 0.034 0.004 -0.013 0.001 N2 0.066 0.073 0.109 -0.034 0.001 -0.021 O11 0.068 0.053 0.077 -0.031 0.003 0.000 O12 0.103 0.181 0.124 -0.065 0.011 -0.055 O13 0.078 0.030 0.045 -0.004 -0.032 0.005 O14 0.071 0.035 0.038 -0.007 -0.020 -0.007 O15 0.136 0.058 0.093 -0.050 -0.035 -0.005 O16 0.098 0.058 0.047 -0.015 -0.033 0.019 O17 0.110 0.022 0.055 0.001 -0.038 -0.004 O18 0.147 0.029 0.066 -0.005 -0.064 0.000 O19 0.183 0.052 0.054 -0.014 -0.002 -0.016 O20 0.124 0.091 0.121 -0.008 0.008 -0.006 O21 0.073 0.028 0.046 0.011 -0.029 -0.018 O22 0.104 0.030 0.065 0.013 -0.041 -0.023 O23 0.073 0.037 0.076 -0.010 -0.007 -0.004 O24 0.119 0.084 0.184 0.041 0.045 -0.021 O25 0.106 0.049 0.053 0.012 -0.032 -0.042 O26 0.146 0.049 0.103 0.038 -0.065 -0.065 O27 0.106 0.112 0.085 -0.017 -0.056 0.000 O27A 0.133 0.080 0.124 -0.007 -0.039 -0.040 O28 0.078 0.090 0.236 -0.058 -0.081 -0.007 O28A 0.115 0.083 0.139 0.003 -0.060 -0.058 O29 0.158 0.165 0.111 0.068 -0.058 -0.119 C91 0.105 0.127 0.119 0.021 -0.035 -0.074 C92 0.104 0.127 0.134 0.013 -0.014 -0.066 C93 0.156 0.182 0.070 0.032 -0.031 -0.109 C94 0.179 0.243 0.110 0.092 -0.063 -0.145 C95 0.132 0.202 0.135 0.040 -0.039 -0.098 C96 0.125 0.196 0.190 -0.043 -0.056 -0.034 C97 0.128 0.175 0.189 -0.020 -0.060 -0.072 C98 0.143 0.093 0.151 0.070 -0.025 -0.069 C99 0.164 0.112 0.067 0.029 -0.015 -0.079 C100 0.226 0.058 0.096 0.019 -0.010 -0.094 C101 0.323 0.082 0.096 0.015 -0.044 -0.070 C102 0.334 0.052 0.143 0.043 -0.022 -0.049 C103 0.451 0.108 0.144 0.070 0.024 -0.072 C104 0.263 0.067 0.206 0.052 -0.007 -0.087 C105 0.402 0.184 0.180 0.043 -0.035 -0.205 O30 0.171 0.090 0.054 0.025 -0.025 -0.094 N7 0.207 1.058 0.183 -0.046 -0.147 -0.045 O31 0.149 0.215 0.151 -0.052 -0.038 -0.040 O32 0.555 0.300 0.285 -0.027 -0.223 -0.184 O33 0.138 0.031 0.042 0.010 -0.038 -0.022 O34 0.113 0.043 0.053 0.023 -0.028 -0.031 O35 0.089 0.085 0.065 -0.030 -0.014 0.013 O36 0.152 0.230 0.177 -0.083 -0.108 0.029 O37 0.120 0.020 0.068 0.004 -0.048 -0.011 O38 0.057 0.076 0.059 0.030 -0.016 -0.018 N1 0.096 0.048 0.024 -0.009 -0.014 -0.010 N3 0.107 0.056 0.048 -0.025 -0.024 0.001 N4 0.141 0.030 0.080 -0.002 -0.011 -0.014 N5 0.094 0.043 0.084 0.008 0.007 -0.013 N6 0.102 0.112 0.089 -0.002 -0.050 -0.044 N6A 0.099 0.076 0.087 -0.026 0.006 -0.054 N8 0.107 0.121 0.102 -0.054 -0.055 0.042 C1 0.080 0.033 0.047 0.001 -0.025 -0.021 C2 0.108 0.052 0.068 -0.002 -0.035 -0.037 C3 0.124 0.040 0.054 -0.002 -0.038 -0.025 C4 0.183 0.062 0.062 -0.004 -0.052 -0.026 C5 0.286 0.077 0.108 -0.008 -0.092 -0.083 C6 0.309 0.153 0.100 0.003 -0.071 -0.155 C7 0.201 0.100 0.086 -0.007 -0.053 -0.089 C8 0.092 0.065 0.055 0.011 -0.022 -0.051 C9 0.063 0.053 0.044 0.010 -0.010 -0.028 C10 0.076 0.114 0.052 0.021 -0.017 -0.057 C11 0.089 0.178 0.052 -0.017 0.011 -0.052 C12 0.129 0.451 0.073 -0.028 0.018 -0.166 C13 0.177 0.503 0.081 -0.070 0.006 -0.223 C14 0.167 0.352 0.105 0.087 -0.064 -0.201 C15 0.132 0.201 0.072 0.051 -0.035 -0.110 C31 0.069 0.044 0.044 -0.023 -0.022 0.012 C32 0.081 0.058 0.063 -0.016 -0.023 0.009 C33 0.102 0.047 0.039 -0.024 -0.021 0.015 C34 0.101 0.057 0.051 -0.022 -0.009 0.014 C35 0.142 0.067 0.034 -0.024 -0.011 0.014 C36 0.063 0.103 0.074 -0.003 -0.003 0.007 C37 0.096 0.081 0.048 -0.017 -0.013 0.015 C38 0.060 0.075 0.049 -0.024 -0.009 -0.012 C39 0.070 0.030 0.051 -0.016 -0.033 0.009 C40 0.061 0.083 0.061 -0.038 -0.010 -0.015 C41 0.078 0.138 0.067 -0.062 0.008 -0.040 C42 0.153 0.215 0.083 -0.070 0.010 -0.108 C43 0.170 0.220 0.116 -0.096 0.023 -0.144 C44 0.130 0.203 0.116 -0.086 0.023 -0.116 C45 0.092 0.114 0.078 -0.038 -0.004 -0.057 C46 0.107 0.020 0.040 -0.004 -0.030 0.008 C47 0.092 0.020 0.045 0.007 -0.029 -0.005 C48 0.099 0.022 0.041 0.001 0.001 0.006 C49 0.092 0.027 0.061 -0.001 -0.017 -0.008 C50 0.090 0.037 0.039 -0.008 -0.023 -0.008 C51 0.073 0.045 0.053 -0.003 -0.028 -0.008 C52 0.089 0.035 0.037 -0.001 -0.022 -0.009 C53 0.110 0.030 0.060 -0.009 -0.049 0.016 C54 0.154 0.027 0.081 -0.008 -0.077 0.025 C55 0.165 0.050 0.126 -0.036 -0.109 0.042 C56 0.149 0.065 0.129 -0.021 -0.090 0.003 C57 0.194 0.069 0.199 -0.037 -0.146 0.010 C58 0.214 0.094 0.208 0.001 -0.152 -0.010 C59 0.234 0.086 0.213 -0.054 -0.177 0.056 C60 0.161 0.062 0.106 -0.026 -0.100 0.028 C61 0.072 0.023 0.047 0.006 -0.016 -0.012 C62 0.072 0.032 0.034 0.002 -0.021 -0.001 C63 0.084 0.024 0.048 0.001 -0.001 -0.002 C64 0.106 0.029 0.043 0.001 -0.008 -0.001 C65 0.111 0.034 0.064 -0.001 -0.045 -0.003 C66 0.054 0.039 0.071 -0.026 -0.026 0.010 C67 0.088 0.039 0.040 -0.008 -0.017 -0.008 C68 0.080 0.035 0.047 0.004 -0.030 -0.018 C69 0.096 0.034 0.047 0.003 -0.038 -0.022 C70 0.058 0.033 0.061 -0.006 -0.022 -0.007 C71 0.112 0.032 0.073 -0.005 -0.053 -0.015 C72 0.114 0.042 0.071 -0.015 -0.048 0.007 C73 0.096 0.063 0.080 -0.031 -0.037 -0.004 C74 0.111 0.050 0.116 -0.018 -0.043 -0.024 C75 0.097 0.045 0.084 0.000 -0.041 -0.018 C76 0.097 0.055 0.049 0.011 -0.025 -0.042 C77 0.086 0.061 0.049 0.013 -0.031 -0.043 C78 0.118 0.064 0.090 0.003 -0.050 -0.029 C79 0.118 0.100 0.076 0.012 -0.042 -0.055 C80 0.079 0.064 0.059 0.010 -0.011 -0.026 C81 0.082 0.071 0.079 0.008 -0.033 -0.034 C82 0.093 0.073 0.045 0.002 -0.020 -0.045 C83 0.114 0.054 0.108 0.022 -0.065 -0.050 C84 0.120 0.054 0.100 0.016 -0.047 -0.057 C85 0.127 0.058 0.106 0.035 -0.050 -0.052 C86 0.123 0.050 0.117 0.011 -0.058 -0.037 C87 0.159 0.062 0.161 0.022 -0.081 -0.068 C88 0.201 0.068 0.187 0.052 -0.101 -0.087 C89 0.226 0.062 0.175 0.042 -0.109 -0.091 C90 0.191 0.067 0.136 0.041 -0.076 -0.084 C106 0.144 0.022 0.049 0.002 -0.035 0.012 C107 0.169 0.048 0.042 -0.006 -0.032 0.030 C108 0.181 0.085 0.061 -0.040 -0.060 0.064 C109 0.193 0.136 0.083 -0.052 -0.081 0.109 C110 0.226 0.156 0.079 -0.042 -0.068 0.132 C111 0.313 0.047 0.053 -0.001 -0.001 0.050 C112 0.338 0.025 0.032 -0.002 -0.010 0.027 C113 0.142 0.038 0.052 0.019 -0.039 -0.020 C114 0.121 0.045 0.039 0.018 -0.030 -0.036 C115 0.129 0.063 0.059 0.024 -0.037 -0.054 C116 0.204 0.036 0.061 0.004 -0.007 -0.013 C117 0.209 0.043 0.085 -0.005 0.023 -0.011 C118 0.180 0.126 0.043 0.010 -0.015 -0.088 C119 0.099 0.389 0.085 0.112 0.006 0.026 C120 0.091 0.371 0.080 0.116 -0.003 0.004 _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 Er1 O6 2.276(8) . ? Er1 O5 2.288(8) . ? Er1 O10 2.309(7) . ? Er1 O9 2.346(7) . ? Er1 O2 2.357(7) . ? Er1 O1 2.365(7) . ? Er1 O4 2.366(8) . ? Er1 O21 2.516(7) . ? Er1 Er3 3.5420(11) . ? Er1 Er2 3.8185(16) . ? Er1 Er4 3.8939(14) . ? Er2 O14 2.275(8) . ? Er2 O18 2.308(10) . ? Er2 O13 2.315(9) . ? Er2 O1 2.326(7) . ? Er2 O17 2.358(7) . ? Er2 O2 2.361(7) . ? Er2 O3 2.426(10) . ? Er2 O33 2.488(9) . ? Er2 Er4 3.5581(18) . ? Er2 Er3 3.8633(13) . ? Er3 O26 2.259(9) . ? Er3 O22 2.263(9) . ? Er3 O4 2.307(8) . ? Er3 O1 2.337(8) . ? Er3 O25 2.358(10) . ? Er3 O3 2.365(8) . ? Er3 O37 2.435(9) . ? Er3 O21 2.511(7) . ? Er3 Er4 3.8017(13) . ? Er4 O29 2.229(12) . ? Er4 O3 2.310(9) . ? Er4 O34 2.310(9) . ? Er4 O30 2.330(9) . ? Er4 O2 2.345(8) . ? Er4 O38 2.406(10) . ? Er4 O4 2.406(8) . ? Er4 O33 2.475(10) . ? O1 H1 1.0000 . ? O2 H2 1.0000 . ? O3 H3 1.0000 . ? O4 H4 1.0000 . ? O5 C1 1.264(14) . ? O6 C9 1.266(14) . ? O7 N1 1.236(12) . ? O8 N1 1.222(14) . ? O9 C16 1.304(12) . ? C16 C23 1.393(14) . ? C16 C17 1.507(15) . ? C17 C22 1.392(16) . ? C17 C18 1.416(16) . ? C18 C19 1.407(16) . ? C18 N2 1.488(18) . ? C19 C20 1.411(18) . ? C19 H19 0.9500 . ? C20 C21 1.359(18) . ? C20 H20 0.9500 . ? C21 C22 1.389(17) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.393(14) . ? C23 H23 0.9500 . ? C24 O10 1.260(11) . ? C24 C25 1.497(14) . ? C25 C30 1.373(17) . ? C25 C26 1.398(15) . ? C26 C27 1.391(15) . ? C26 H26 0.9500 . ? C27 C28 1.35(2) . ? C27 H27 0.9500 . ? C28 C29 1.40(2) . ? C28 H28 0.9500 . ? C29 C30 1.407(19) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? N2 O11 1.184(14) . ? N2 O12 1.228(16) . ? O13 C31 1.239(16) . ? O14 C39 1.266(16) . ? O15 N3 1.228(16) . ? O16 N3 1.214(13) . ? O17 C46 1.285(15) . ? O18 C54 1.295(17) . ? O19 N4 1.244(18) . ? O20 N4 1.20(2) . ? O21 C61 1.280(13) . ? O22 C69 1.271(14) . ? O23 N5 1.208(14) . ? O24 N5 1.222(16) . ? O25 C76 1.254(15) . ? O26 C84 1.257(17) . ? O27 N6 1.27(3) . ? O27A N6A 1.19(5) . ? O28 N6 1.21(3) . ? O28A N6A 1.28(5) . ? O29 C91 1.333(15) . ? C91 C98 1.390(18) . ? C91 C92 1.503(18) . ? C92 C97 1.39(2) . ? C92 C93 1.45(2) . ? C93 C94 1.39(2) . ? C93 N7 1.50(2) . ? C94 C95 1.44(2) . ? C94 H94 0.9500 . ? C95 C96 1.37(2) . ? C95 H95 0.9500 . ? C96 C97 1.40(2) . ? C96 H96 0.9500 . ? C97 H97 0.9500 . ? C98 C99 1.373(18) . ? C98 H98 0.9500 . ? C99 O30 1.252(15) . ? C99 C100 1.490(17) . ? C100 C105 1.36(2) . ? C100 C101 1.40(2) . ? C101 C102 1.395(19) . ? C101 H101 0.9500 . ? C102 C103 1.36(2) . ? C102 H102 0.9500 . ? C103 C104 1.41(3) . ? C103 H103 0.9500 . ? C104 C105 1.41(2) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? N7 O31 1.162(19) . ? N7 O32 1.24(2) . ? O33 C106 1.276(15) . ? O34 C114 1.288(15) . ? O35 N8 1.244(17) . ? O36 N8 1.23(2) . ? N1 C3 1.474(18) . ? N3 C33 1.47(2) . ? N4 C48 1.502(19) . ? N5 C63 1.483(18) . ? N6 C78 1.50(3) . ? N6A C86 1.31(5) . ? N8 C108 1.42(3) . ? C1 C8 1.411(18) . ? C1 C2 1.511(17) . ? C2 C7 1.36(2) . ? C2 C3 1.39(2) . ? C3 C4 1.420(19) . ? C4 C5 1.38(3) . ? C4 H9 0.9500 . ? C5 C6 1.39(3) . ? C5 H5 0.9500 . ? C6 C7 1.42(2) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.425(18) . ? C8 H8 0.9500 . ? C9 C10 1.506(18) . ? C10 C11 1.36(2) . ? C10 C15 1.37(2) . ? C11 C12 1.40(2) . ? C11 H11 0.9500 . ? C12 C13 1.29(4) . ? C12 H12 0.9500 . ? C13 C14 1.43(4) . ? C13 H13 0.9500 . ? C14 C15 1.45(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C31 C38 1.382(19) . ? C31 C32 1.533(19) . ? C32 C33 1.41(2) . ? C32 C37 1.41(2) . ? C33 C34 1.374(19) . ? C34 C35 1.36(3) . ? C34 H34 0.9500 . ? C35 C36 1.41(3) . ? C35 H35 0.9500 . ? C36 C37 1.42(2) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.421(17) . ? C38 H38 0.9500 . ? C39 C40 1.496(18) . ? C40 C45 1.40(2) . ? C40 C41 1.43(2) . ? C41 C42 1.41(2) . ? C41 H41 0.9500 . ? C42 C43 1.35(3) . ? C42 H42 0.9500 . ? C43 C44 1.40(3) . ? C43 H43 0.9500 . ? C44 C45 1.38(2) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C53 1.37(2) . ? C46 C47 1.516(16) . ? C47 C48 1.39(2) . ? C47 C52 1.396(18) . ? C48 C49 1.393(18) . ? C49 C50 1.381(19) . ? C49 H49 0.9500 . ? C50 C51 1.366(19) . ? C50 H50 0.9500 . ? C51 C52 1.401(17) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.423(19) . ? C53 H53 0.9500 . ? C54 C55 1.44(2) . ? C55 C60 1.40(2) . ? C55 C56 1.42(2) . ? C56 C57 1.41(2) . ? C56 H56 0.9500 . ? C57 C58 1.42(3) . ? C57 H57 0.9500 . ? C58 C59 1.41(3) . ? C58 H58 0.9500 . ? C59 C60 1.36(3) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C68 1.403(16) . ? C61 C62 1.533(15) . ? C62 C67 1.360(18) . ? C62 C63 1.399(18) . ? C63 C64 1.372(16) . ? C64 C65 1.37(2) . ? C64 H64 0.9500 . ? C65 C66 1.40(2) . ? C65 H65 0.9500 . ? C66 C67 1.405(18) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 C69 1.390(16) . ? C68 H68 0.9500 . ? C69 C70 1.519(16) . ? C70 C71 1.378(18) . ? C70 C75 1.381(18) . ? C71 C72 1.390(18) . ? C71 H71 0.9500 . ? C72 C73 1.40(2) . ? C72 H72 0.9500 . ? C73 C74 1.36(2) . ? C73 H73 0.9500 . ? C74 C75 1.40(2) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C83 1.368(18) . ? C76 C77 1.53(2) . ? C77 C82 1.354(18) . ? C77 C78 1.39(2) . ? C78 C79 1.41(2) . ? C79 C80 1.36(2) . ? C79 H79 0.9500 . ? C80 C81 1.37(2) . ? C80 H80 0.9500 . ? C81 C82 1.40(2) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C84 1.42(2) . ? C83 H83 0.9500 . ? C84 C85 1.507(19) . ? C85 C90 1.38(2) . ? C85 C86 1.38(2) . ? C86 C87 1.37(2) . ? C87 C88 1.37(3) . ? C87 H87 0.9500 . ? C88 C89 1.33(3) . ? C88 H88 0.9500 . ? C89 C90 1.41(2) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C106 C113 1.40(2) . ? C106 C107 1.50(2) . ? C107 C112 1.36(3) . ? C107 C108 1.36(3) . ? C108 C109 1.42(2) . ? C109 C110 1.30(4) . ? C109 H109 0.9500 . ? C110 C111 1.37(5) . ? C110 H110 0.9500 . ? C111 C112 1.42(3) . ? C111 H111 0.9500 . ? C112 H112 0.9500 . ? C113 C114 1.40(2) . ? C113 H113 0.9500 . ? C114 C115 1.49(2) . ? C115 C120 1.33(2) . ? C115 C116 1.34(2) . ? C116 C117 1.41(2) . ? C116 H116 0.9500 . ? C117 C118 1.35(3) . ? C117 H117 0.9500 . ? C118 C119 1.26(3) . ? C118 H118 0.9500 . ? C119 C120 1.39(3) . ? C119 H119 0.9500 . ? C120 H120 0.9500 . ? C121 C122 1.3900 . ? C121 C126 1.3900 . ? C121 C127 1.494(7) . ? C122 C123 1.3900 . ? C122 H122 0.9500 . ? C123 C124 1.3900 . ? C123 H123 0.9500 . ? C124 C125 1.3900 . ? C124 H124 0.9500 . ? C125 C126 1.3900 . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C127 H12A 0.9800 . ? C127 H12B 0.9800 . ? C127 H12C 0.9800 . ? C128 C129 1.3900 . ? C128 C133 1.3900 . ? C128 C134 1.50(3) . ? C129 C130 1.3900 . ? C129 H129 0.9500 . ? C130 C131 1.3900 . ? C130 H130 0.9500 . ? C131 C132 1.3900 . ? C131 H131 0.9500 . ? C132 C133 1.3900 . ? C132 H132 0.9500 . ? C133 H133 0.9500 . ? C134 H13A 0.9800 . ? C134 H13B 0.9800 . ? C134 H13C 0.9800 . ? C135 C141 1.03(6) . ? C135 C136 1.3900 . ? C135 C140 1.3900 . ? C136 C137 1.3900 . ? C136 H136 0.9500 . ? C137 C138 1.3900 . ? C137 H137 0.9500 . ? C138 C139 1.3900 . ? C138 H138 0.9500 . ? C139 C140 1.3900 . ? C139 H139 0.9500 . ? C140 H140 0.9500 . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? C228 C229 1.3900 . ? C228 C233 1.3900 . ? C228 C234 1.56(5) . ? C229 C230 1.3900 . ? C229 H229 0.9500 . ? C230 C231 1.3900 . ? C230 H230 0.9500 . ? C231 C232 1.3900 . ? C231 H231 0.9500 . ? C232 C233 1.3900 . ? C232 H232 0.9500 . ? C233 H233 0.9500 . ? C234 H23A 0.9800 . ? C234 H23B 0.9800 . ? C234 H23C 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 O6 Er1 O5 75.1(3) . . ? O6 Er1 O10 73.9(3) . . ? O5 Er1 O10 78.8(3) . . ? O6 Er1 O9 140.6(3) . . ? O5 Er1 O9 77.4(3) . . ? O10 Er1 O9 73.6(2) . . ? O6 Er1 O2 102.6(3) . . ? O5 Er1 O2 75.1(2) . . ? O10 Er1 O2 153.6(3) . . ? O9 Er1 O2 96.8(3) . . ? O6 Er1 O1 73.5(3) . . ? O5 Er1 O1 124.8(3) . . ? O10 Er1 O1 131.5(2) . . ? O9 Er1 O1 145.9(3) . . ? O2 Er1 O1 69.1(2) . . ? O6 Er1 O4 147.3(3) . . ? O5 Er1 O4 128.4(3) . . ? O10 Er1 O4 127.7(3) . . ? O9 Er1 O4 71.9(3) . . ? O2 Er1 O4 68.7(3) . . ? O1 Er1 O4 74.0(3) . . ? O6 Er1 O21 92.9(3) . . ? O5 Er1 O21 158.3(2) . . ? O10 Er1 O21 80.5(2) . . ? O9 Er1 O21 103.0(3) . . ? O2 Er1 O21 125.8(2) . . ? O1 Er1 O21 66.4(2) . . ? O4 Er1 O21 70.6(3) . . ? O6 Er1 Er3 108.67(18) . . ? O5 Er1 Er3 155.88(17) . . ? O10 Er1 Er3 125.29(19) . . ? O9 Er1 Er3 108.0(2) . . ? O2 Er1 Er3 80.87(18) . . ? O1 Er1 Er3 40.8(2) . . ? O4 Er1 Er3 40.1(2) . . ? O21 Er1 Er3 45.14(15) . . ? O6 Er1 Er2 79.41(18) . . ? O5 Er1 Er2 95.13(18) . . ? O10 Er1 Er2 153.3(2) . . ? O9 Er1 Er2 130.94(17) . . ? O2 Er1 Er2 36.00(17) . . ? O1 Er1 Er2 35.18(18) . . ? O4 Er1 Er2 76.3(2) . . ? O21 Er1 Er2 100.40(16) . . ? Er3 Er1 Er2 63.19(2) . . ? O6 Er1 Er4 133.43(18) . . ? O5 Er1 Er4 98.31(17) . . ? O10 Er1 Er4 151.31(19) . . ? O9 Er1 Er4 77.94(18) . . ? O2 Er1 Er4 34.00(19) . . ? O1 Er1 Er4 73.59(19) . . ? O4 Er1 Er4 35.67(19) . . ? O21 Er1 Er4 103.01(16) . . ? Er3 Er1 Er4 61.28(2) . . ? Er2 Er1 Er4 54.94(3) . . ? O14 Er2 O18 73.2(3) . . ? O14 Er2 O13 74.4(3) . . ? O18 Er2 O13 77.7(3) . . ? O14 Er2 O1 95.8(3) . . ? O18 Er2 O1 152.6(4) . . ? O13 Er2 O1 75.1(3) . . ? O14 Er2 O17 138.9(3) . . ? O18 Er2 O17 73.4(3) . . ? O13 Er2 O17 75.7(3) . . ? O1 Er2 O17 103.0(3) . . ? O14 Er2 O2 74.6(3) . . ? O18 Er2 O2 128.0(3) . . ? O13 Er2 O2 129.7(2) . . ? O1 Er2 O2 69.7(2) . . ? O17 Er2 O2 146.3(3) . . ? O14 Er2 O3 148.3(3) . . ? O18 Er2 O3 132.0(3) . . ? O13 Er2 O3 124.3(3) . . ? O1 Er2 O3 68.9(3) . . ? O17 Er2 O3 72.7(3) . . ? O2 Er2 O3 74.0(3) . . ? O14 Er2 O33 103.0(3) . . ? O18 Er2 O33 82.0(4) . . ? O13 Er2 O33 159.4(3) . . ? O1 Er2 O33 125.3(3) . . ? O17 Er2 O33 95.4(3) . . ? O2 Er2 O33 66.8(3) . . ? O3 Er2 O33 68.4(3) . . ? O14 Er2 Er4 112.3(2) . . ? O18 Er2 Er4 126.1(3) . . ? O13 Er2 Er4 156.1(2) . . ? O1 Er2 Er4 81.2(2) . . ? O17 Er2 Er4 106.5(3) . . ? O2 Er2 Er4 40.72(18) . . ? O3 Er2 Er4 40.1(2) . . ? O33 Er2 Er4 44.1(2) . . ? O14 Er2 Er1 75.6(2) . . ? O18 Er2 Er1 148.5(2) . . ? O13 Er2 Er1 97.86(18) . . ? O1 Er2 Er1 35.86(17) . . ? O17 Er2 Er1 136.3(2) . . ? O2 Er2 Er1 35.94(16) . . ? O3 Er2 Er1 76.39(18) . . ? O33 Er2 Er1 101.2(2) . . ? Er4 Er2 Er1 63.61(3) . . ? O14 Er2 Er3 128.0(2) . . ? O18 Er2 Er3 155.8(2) . . ? O13 Er2 Er3 95.9(2) . . ? O1 Er2 Er3 34.1(2) . . ? O17 Er2 Er3 82.4(2) . . ? O2 Er2 Er3 73.94(19) . . ? O3 Er2 Er3 35.72(19) . . ? O33 Er2 Er3 101.3(2) . . ? Er4 Er2 Er3 61.47(3) . . ? Er1 Er2 Er3 54.91(2) . . ? O26 Er3 O22 90.2(4) . . ? O26 Er3 O4 108.5(4) . . ? O22 Er3 O4 142.7(3) . . ? O26 Er3 O1 149.7(3) . . ? O22 Er3 O1 104.3(3) . . ? O4 Er3 O1 75.7(3) . . ? O26 Er3 O25 73.3(3) . . ? O22 Er3 O25 79.9(3) . . ? O4 Er3 O25 75.4(3) . . ? O1 Er3 O25 134.9(3) . . ? O26 Er3 O3 83.0(3) . . ? O22 Er3 O3 145.0(3) . . ? O4 Er3 O3 71.0(3) . . ? O1 Er3 O3 69.8(3) . . ? O25 Er3 O3 129.6(3) . . ? O26 Er3 O37 78.5(4) . . ? O22 Er3 O37 70.8(3) . . ? O4 Er3 O37 143.1(3) . . ? O1 Er3 O37 81.3(3) . . ? O25 Er3 O37 138.9(3) . . ? O3 Er3 O37 74.2(3) . . ? O26 Er3 O21 143.4(3) . . ? O22 Er3 O21 74.3(3) . . ? O4 Er3 O21 71.7(2) . . ? O1 Er3 O21 66.9(2) . . ? O25 Er3 O21 71.5(3) . . ? O3 Er3 O21 128.0(3) . . ? O37 Er3 O21 124.3(3) . . ? O26 Er3 Er1 149.8(3) . . ? O22 Er3 Er1 116.0(2) . . ? O4 Er3 Er1 41.3(2) . . ? O1 Er3 Er1 41.43(17) . . ? O25 Er3 Er1 95.7(2) . . ? O3 Er3 Er1 83.03(19) . . ? O37 Er3 Er1 122.7(2) . . ? O21 Er3 Er1 45.26(17) . . ? O26 Er3 Er4 89.8(3) . . ? O22 Er3 Er4 179.8(3) . . ? O4 Er3 Er4 37.14(19) . . ? O1 Er3 Er4 75.79(18) . . ? O25 Er3 Er4 99.9(2) . . ? O3 Er3 Er4 35.1(2) . . ? O37 Er3 Er4 109.3(2) . . ? O21 Er3 Er4 105.65(17) . . ? Er1 Er3 Er4 63.93(3) . . ? O26 Er3 Er2 116.4(3) . . ? O22 Er3 Er2 124.8(3) . . ? O4 Er3 Er2 75.9(2) . . ? O1 Er3 Er2 33.97(17) . . ? O25 Er3 Er2 151.3(2) . . ? O3 Er3 Er2 36.8(2) . . ? O37 Er3 Er2 69.0(2) . . ? O21 Er3 Er2 99.35(18) . . ? Er1 Er3 Er2 61.90(3) . . ? Er4 Er3 Er2 55.31(3) . . ? O29 Er4 O3 95.8(5) . . ? O29 Er4 O34 106.1(4) . . ? O3 Er4 O34 142.4(3) . . ? O29 Er4 O30 72.1(4) . . ? O3 Er4 O30 78.7(3) . . ? O34 Er4 O30 79.5(3) . . ? O29 Er4 O2 142.1(3) . . ? O3 Er4 O2 76.5(3) . . ? O34 Er4 O2 101.6(3) . . ? O30 Er4 O2 139.2(4) . . ? O29 Er4 O38 83.9(5) . . ? O3 Er4 O38 144.7(3) . . ? O34 Er4 O38 69.2(3) . . ? O30 Er4 O38 133.2(4) . . ? O2 Er4 O38 82.2(3) . . ? O29 Er4 O4 74.2(4) . . ? O3 Er4 O4 70.2(3) . . ? O34 Er4 O4 144.8(3) . . ? O30 Er4 O4 130.8(3) . . ? O2 Er4 O4 68.2(3) . . ? O38 Er4 O4 75.9(3) . . ? O29 Er4 O33 145.4(4) . . ? O3 Er4 O33 70.5(3) . . ? O34 Er4 O33 74.3(3) . . ? O30 Er4 O33 74.1(4) . . ? O2 Er4 O33 67.3(3) . . ? O38 Er4 O33 125.8(3) . . ? O4 Er4 O33 125.7(3) . . ? O29 Er4 Er2 137.5(4) . . ? O3 Er4 Er2 42.5(2) . . ? O34 Er4 Er2 113.7(3) . . ? O30 Er4 Er2 100.6(3) . . ? O2 Er4 Er2 41.05(17) . . ? O38 Er4 Er2 123.3(2) . . ? O4 Er4 Er2 81.4(2) . . ? O33 Er4 Er2 44.3(2) . . ? O29 Er4 Er3 77.1(4) . . ? O3 Er4 Er3 36.1(2) . . ? O34 Er4 Er3 176.7(3) . . ? O30 Er4 Er3 101.9(2) . . ? O2 Er4 Er3 75.38(17) . . ? O38 Er4 Er3 111.3(2) . . ? O4 Er4 Er3 35.37(19) . . ? O33 Er4 Er3 103.2(2) . . ? Er2 Er4 Er3 63.22(4) . . ? O29 Er4 Er1 107.9(3) . . ? O3 Er4 Er1 75.87(19) . . ? O34 Er4 Er1 123.2(2) . . ? O30 Er4 Er1 154.5(3) . . ? O2 Er4 Er1 34.20(17) . . ? O38 Er4 Er1 70.8(2) . . ? O4 Er4 Er1 35.0(2) . . ? O33 Er4 Er1 99.4(2) . . ? Er2 Er4 Er1 61.45(3) . . ? Er3 Er4 Er1 54.79(2) . . ? Er2 O1 Er3 111.9(3) . . ? Er2 O1 Er1 109.0(3) . . ? Er3 O1 Er1 97.8(3) . . ? Er2 O1 H1 112.4 . . ? Er3 O1 H1 112.4 . . ? Er1 O1 H1 112.4 . . ? Er4 O2 Er1 111.8(3) . . ? Er4 O2 Er2 98.2(3) . . ? Er1 O2 Er2 108.1(3) . . ? Er4 O2 H2 112.6 . . ? Er1 O2 H2 112.6 . . ? Er2 O2 H2 112.6 . . ? Er4 O3 Er3 108.8(4) . . ? Er4 O3 Er2 97.4(3) . . ? Er3 O3 Er2 107.5(3) . . ? Er4 O3 H3 113.9 . . ? Er3 O3 H3 113.9 . . ? Er2 O3 H3 113.9 . . ? Er3 O4 Er1 98.6(3) . . ? Er3 O4 Er4 107.5(3) . . ? Er1 O4 Er4 109.3(3) . . ? Er3 O4 H4 113.4 . . ? Er1 O4 H4 113.4 . . ? Er4 O4 H4 113.4 . . ? C1 O5 Er1 134.5(7) . . ? C9 O6 Er1 136.2(7) . . ? C16 O9 Er1 132.3(7) . . ? O9 C16 C23 125.0(10) . . ? O9 C16 C17 118.2(9) . . ? C23 C16 C17 116.7(9) . . ? C22 C17 C18 117.3(11) . . ? C22 C17 C16 116.9(12) . . ? C18 C17 C16 125.7(11) . . ? C19 C18 C17 121.6(12) . . ? C19 C18 N2 118.5(13) . . ? C17 C18 N2 119.7(10) . . ? C18 C19 C20 117.8(14) . . ? C18 C19 H19 121.1 . . ? C20 C19 H19 121.1 . . ? C21 C20 C19 121.1(12) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 120.5(13) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C17 121.6(14) . . ? C21 C22 H22 119.2 . . ? C17 C22 H22 119.2 . . ? C16 C23 C24 125.0(9) . . ? C16 C23 H23 117.5 . . ? C24 C23 H23 117.5 . . ? O10 C24 C23 124.1(9) . . ? O10 C24 C25 117.5(9) . . ? C23 C24 C25 118.5(9) . . ? C30 C25 C26 119.3(11) . . ? C30 C25 C24 118.5(10) . . ? C26 C25 C24 122.0(10) . . ? C27 C26 C25 120.1(12) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 120.6(13) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 120.4(13) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C30 119.3(15) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C25 C30 C29 120.1(13) . . ? C25 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C24 O10 Er1 135.6(6) . . ? O11 N2 O12 121.7(15) . . ? O11 N2 C18 120.9(13) . . ? O12 N2 C18 117.2(12) . . ? C31 O13 Er2 134.3(7) . . ? C39 O14 Er2 136.1(7) . . ? C46 O17 Er2 128.9(9) . . ? C54 O18 Er2 134.1(8) . . ? C61 O21 Er3 126.1(7) . . ? C61 O21 Er1 144.2(7) . . ? Er3 O21 Er1 89.6(2) . . ? C69 O22 Er3 133.3(8) . . ? C76 O25 Er3 132.8(9) . . ? C84 O26 Er3 134.8(9) . . ? C91 O29 Er4 137.0(11) . . ? O29 C91 C98 124.0(15) . . ? O29 C91 C92 114.8(14) . . ? C98 C91 C92 121.1(15) . . ? C97 C92 C93 117.2(16) . . ? C97 C92 C91 122.6(17) . . ? C93 C92 C91 120.0(15) . . ? C94 C93 C92 124.6(17) . . ? C94 C93 N7 115.3(19) . . ? C92 C93 N7 119.9(17) . . ? C93 C94 C95 113.2(19) . . ? C93 C94 H94 123.4 . . ? C95 C94 H94 123.4 . . ? C96 C95 C94 124(2) . . ? C96 C95 H95 117.8 . . ? C94 C95 H95 117.8 . . ? C95 C96 C97 120(2) . . ? C95 C96 H96 120.1 . . ? C97 C96 H96 120.1 . . ? C92 C97 C96 121(2) . . ? C92 C97 H97 119.6 . . ? C96 C97 H97 119.6 . . ? C99 C98 C91 125.2(15) . . ? C99 C98 H98 117.4 . . ? C91 C98 H98 117.4 . . ? O30 C99 C98 120.8(15) . . ? O30 C99 C100 119.5(15) . . ? C98 C99 C100 119.5(14) . . ? C105 C100 C101 117.6(16) . . ? C105 C100 C99 123.6(17) . . ? C101 C100 C99 118.2(13) . . ? C102 C101 C100 121.9(19) . . ? C102 C101 H101 119.0 . . ? C100 C101 H101 119.0 . . ? C103 C102 C101 120(2) . . ? C103 C102 H102 120.2 . . ? C101 C102 H102 120.2 . . ? C102 C103 C104 119.1(18) . . ? C102 C103 H103 120.5 . . ? C104 C103 H103 120.5 . . ? C105 C104 C103 119(2) . . ? C105 C104 H104 120.5 . . ? C103 C104 H104 120.5 . . ? C100 C105 C104 121(2) . . ? C100 C105 H105 119.5 . . ? C104 C105 H105 119.5 . . ? C99 O30 Er4 140.4(11) . . ? O31 N7 O32 131(3) . . ? O31 N7 C93 116(2) . . ? O32 N7 C93 104(2) . . ? C106 O33 Er4 127.4(11) . . ? C106 O33 Er2 140.8(11) . . ? Er4 O33 Er2 91.6(3) . . ? C114 O34 Er4 133.4(9) . . ? O8 N1 O7 122.3(12) . . ? O8 N1 C3 120.0(11) . . ? O7 N1 C3 117.5(12) . . ? O16 N3 O15 125.3(15) . . ? O16 N3 C33 116.8(13) . . ? O15 N3 C33 117.7(12) . . ? O20 N4 O19 127.9(17) . . ? O20 N4 C48 117.0(15) . . ? O19 N4 C48 115.2(17) . . ? O23 N5 O24 120.6(14) . . ? O23 N5 C63 120.2(12) . . ? O24 N5 C63 119.1(12) . . ? O28 N6 O27 124(2) . . ? O28 N6 C78 114(2) . . ? O27 N6 C78 121(2) . . ? O27A N6A O28A 113(5) . . ? O27A N6A C86 114(4) . . ? O28A N6A C86 134(4) . . ? O36 N8 O35 122(2) . . ? O36 N8 C108 119.1(18) . . ? O35 N8 C108 118.6(16) . . ? O5 C1 C8 125.5(11) . . ? O5 C1 C2 116.8(12) . . ? C8 C1 C2 117.6(12) . . ? C7 C2 C3 116.2(14) . . ? C7 C2 C1 123.2(15) . . ? C3 C2 C1 120.6(12) . . ? C2 C3 C4 124.3(15) . . ? C2 C3 N1 121.9(11) . . ? C4 C3 N1 113.6(14) . . ? C5 C4 C3 116.6(18) . . ? C5 C4 H9 121.7 . . ? C3 C4 H9 121.7 . . ? C4 C5 C6 121.0(17) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 119(2) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C2 C7 C6 122(2) . . ? C2 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? C1 C8 C9 123.8(12) . . ? C1 C8 H8 118.1 . . ? C9 C8 H8 118.1 . . ? O6 C9 C8 123.0(11) . . ? O6 C9 C10 117.6(11) . . ? C8 C9 C10 119.4(12) . . ? C11 C10 C15 119.7(16) . . ? C11 C10 C9 117.3(14) . . ? C15 C10 C9 122.9(16) . . ? C10 C11 C12 123(2) . . ? C10 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C13 C12 C11 117(3) . . ? C13 C12 H12 121.3 . . ? C11 C12 H12 121.3 . . ? C12 C13 C14 125(3) . . ? C12 C13 H13 117.4 . . ? C14 C13 H13 117.4 . . ? C13 C14 C15 115(2) . . ? C13 C14 H14 122.7 . . ? C15 C14 H14 122.7 . . ? C10 C15 C14 120(2) . . ? C10 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? O13 C31 C38 126.6(12) . . ? O13 C31 C32 114.7(12) . . ? C38 C31 C32 118.7(15) . . ? C33 C32 C37 116.2(14) . . ? C33 C32 C31 120.8(16) . . ? C37 C32 C31 123.0(14) . . ? C34 C33 C32 123.8(18) . . ? C34 C33 N3 114.9(14) . . ? C32 C33 N3 121.3(12) . . ? C35 C34 C33 119.6(17) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 120.4(14) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C37 119.4(18) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C32 C37 C36 120.4(17) . . ? C32 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C31 C38 C39 123.7(14) . . ? C31 C38 H38 118.1 . . ? C39 C38 H38 118.1 . . ? O14 C39 C38 123.4(12) . . ? O14 C39 C40 117.6(11) . . ? C38 C39 C40 118.9(14) . . ? C45 C40 C41 120.6(14) . . ? C45 C40 C39 123.3(13) . . ? C41 C40 C39 116.1(15) . . ? C42 C41 C40 115.3(18) . . ? C42 C41 H41 122.4 . . ? C40 C41 H41 122.4 . . ? C43 C42 C41 123.0(19) . . ? C43 C42 H42 118.5 . . ? C41 C42 H42 118.5 . . ? C42 C43 C44 121.5(17) . . ? C42 C43 H43 119.2 . . ? C44 C43 H43 119.2 . . ? C45 C44 C43 118(2) . . ? C45 C44 H44 121.2 . . ? C43 C44 H44 121.2 . . ? C44 C45 C40 121.6(16) . . ? C44 C45 H45 119.2 . . ? C40 C45 H45 119.2 . . ? O17 C46 C53 127.7(11) . . ? O17 C46 C47 115.2(13) . . ? C53 C46 C47 117.0(11) . . ? C48 C47 C52 116.3(11) . . ? C48 C47 C46 122.8(12) . . ? C52 C47 C46 120.9(13) . . ? C47 C48 C49 123.7(12) . . ? C47 C48 N4 120.7(12) . . ? C49 C48 N4 115.4(14) . . ? C50 C49 C48 117.8(14) . . ? C50 C49 H49 121.1 . . ? C48 C49 H49 121.1 . . ? C51 C50 C49 120.7(12) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C50 C51 C52 120.7(13) . . ? C50 C51 H51 119.6 . . ? C52 C51 H51 119.6 . . ? C47 C52 C51 120.7(14) . . ? C47 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C46 C53 C54 125.2(13) . . ? C46 C53 H53 117.4 . . ? C54 C53 H53 117.4 . . ? O18 C54 C53 121.0(15) . . ? O18 C54 C55 116.0(12) . . ? C53 C54 C55 122.6(13) . . ? C60 C55 C56 120.8(16) . . ? C60 C55 C54 123.4(15) . . ? C56 C55 C54 115.4(13) . . ? C57 C56 C55 116.3(16) . . ? C57 C56 H56 121.8 . . ? C55 C56 H56 121.8 . . ? C56 C57 C58 122.4(18) . . ? C56 C57 H57 118.8 . . ? C58 C57 H57 118.8 . . ? C59 C58 C57 118(2) . . ? C59 C58 H58 121.0 . . ? C57 C58 H58 121.0 . . ? C60 C59 C58 120.3(18) . . ? C60 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C59 C60 C55 121.9(17) . . ? C59 C60 H60 119.1 . . ? C55 C60 H60 119.1 . . ? O21 C61 C68 127.2(10) . . ? O21 C61 C62 118.4(10) . . ? C68 C61 C62 113.9(10) . . ? C67 C62 C63 117.8(11) . . ? C67 C62 C61 118.5(12) . . ? C63 C62 C61 123.1(11) . . ? C64 C63 C62 122.2(13) . . ? C64 C63 N5 117.7(13) . . ? C62 C63 N5 120.0(10) . . ? C65 C64 C63 119.6(14) . . ? C65 C64 H64 120.2 . . ? C63 C64 H64 120.2 . . ? C64 C65 C66 120.0(12) . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C65 C66 C67 118.8(13) . . ? C65 C66 H66 120.6 . . ? C67 C66 H66 120.6 . . ? C62 C67 C66 121.5(14) . . ? C62 C67 H67 119.2 . . ? C66 C67 H67 119.2 . . ? C69 C68 C61 125.4(11) . . ? C69 C68 H68 117.3 . . ? C61 C68 H68 117.3 . . ? O22 C69 C68 125.1(11) . . ? O22 C69 C70 115.4(10) . . ? C68 C69 C70 119.5(10) . . ? C71 C70 C75 119.1(12) . . ? C71 C70 C69 122.9(11) . . ? C75 C70 C69 118.0(12) . . ? C70 C71 C72 120.8(13) . . ? C70 C71 H71 119.6 . . ? C72 C71 H71 119.6 . . ? C71 C72 C73 119.9(15) . . ? C71 C72 H72 120.0 . . ? C73 C72 H72 120.0 . . ? C74 C73 C72 119.1(14) . . ? C74 C73 H73 120.4 . . ? C72 C73 H73 120.4 . . ? C73 C74 C75 121.1(15) . . ? C73 C74 H74 119.4 . . ? C75 C74 H74 119.4 . . ? C70 C75 C74 119.8(15) . . ? C70 C75 H75 120.1 . . ? C74 C75 H75 120.1 . . ? O25 C76 C83 125.0(14) . . ? O25 C76 C77 115.2(11) . . ? C83 C76 C77 119.2(13) . . ? C82 C77 C78 116.9(14) . . ? C82 C77 C76 120.1(12) . . ? C78 C77 C76 122.9(12) . . ? C77 C78 C79 121.7(15) . . ? C77 C78 N6 120.1(16) . . ? C79 C78 N6 116.0(16) . . ? C80 C79 C78 119.7(16) . . ? C80 C79 H79 120.2 . . ? C78 C79 H79 120.2 . . ? C79 C80 C81 118.8(16) . . ? C79 C80 H80 120.6 . . ? C81 C80 H80 120.6 . . ? C80 C81 C82 120.9(14) . . ? C80 C81 H81 119.6 . . ? C82 C81 H81 119.6 . . ? C77 C82 C81 121.9(14) . . ? C77 C82 H82 119.0 . . ? C81 C82 H82 119.0 . . ? C76 C83 C84 124.3(14) . . ? C76 C83 H83 117.9 . . ? C84 C83 H83 117.9 . . ? O26 C84 C83 124.0(12) . . ? O26 C84 C85 117.6(14) . . ? C83 C84 C85 118.2(14) . . ? C90 C85 C86 119.2(15) . . ? C90 C85 C84 116.3(16) . . ? C86 C85 C84 124.5(15) . . ? N6A C86 C87 113(2) . . ? N6A C86 C85 126(2) . . ? C87 C86 C85 120.2(17) . . ? C86 C87 C88 120.6(18) . . ? C86 C87 H87 119.7 . . ? C88 C87 H87 119.7 . . ? C89 C88 C87 120.3(16) . . ? C89 C88 H88 119.9 . . ? C87 C88 H88 119.9 . . ? C88 C89 C90 120(2) . . ? C88 C89 H89 119.8 . . ? C90 C89 H89 119.8 . . ? C85 C90 C89 119.2(18) . . ? C85 C90 H90 120.4 . . ? C89 C90 H90 120.4 . . ? O33 C106 C113 126.6(15) . . ? O33 C106 C107 117.8(13) . . ? C113 C106 C107 115.0(12) . . ? C112 C107 C108 118.8(19) . . ? C112 C107 C106 119(2) . . ? C108 C107 C106 122.3(15) . . ? C107 C108 N8 121.5(15) . . ? C107 C108 C109 121(2) . . ? N8 C108 C109 117(2) . . ? C110 C109 C108 120(3) . . ? C110 C109 H109 120.2 . . ? C108 C109 H109 120.2 . . ? C109 C110 C111 121(2) . . ? C109 C110 H110 119.6 . . ? C111 C110 H110 119.6 . . ? C110 C111 C112 120(2) . . ? C110 C111 H111 119.9 . . ? C112 C111 H111 119.9 . . ? C107 C112 C111 119(3) . . ? C107 C112 H112 120.4 . . ? C111 C112 H112 120.4 . . ? C106 C113 C114 126.4(12) . . ? C106 C113 H113 116.8 . . ? C114 C113 H113 116.8 . . ? O34 C114 C113 123.8(12) . . ? O34 C114 C115 115.6(14) . . ? C113 C114 C115 120.6(12) . . ? C120 C115 C116 116.2(17) . . ? C120 C115 C114 122.2(18) . . ? C116 C115 C114 121.6(14) . . ? C115 C116 C117 121.1(19) . . ? C115 C116 H116 119.4 . . ? C117 C116 H116 119.4 . . ? C118 C117 C116 119(2) . . ? C118 C117 H117 120.3 . . ? C116 C117 H117 120.3 . . ? C119 C118 C117 119.5(19) . . ? C119 C118 H118 120.3 . . ? C117 C118 H118 120.3 . . ? C118 C119 C120 122(2) . . ? C118 C119 H119 119.1 . . ? C120 C119 H119 119.1 . . ? C115 C120 C119 122(2) . . ? C115 C120 H120 119.1 . . ? C119 C120 H120 119.1 . . ? C122 C121 C126 120.0 . . ? C122 C121 C127 120.1(6) . . ? C126 C121 C127 119.8(6) . . ? C123 C122 C121 120.0 . . ? C123 C122 H122 120.0 . . ? C121 C122 H122 120.0 . . ? C124 C123 C122 120.0 . . ? C124 C123 H123 120.0 . . ? C122 C123 H123 120.0 . . ? C123 C124 C125 120.0 . . ? C123 C124 H124 120.0 . . ? C125 C124 H124 120.0 . . ? C126 C125 C124 120.0 . . ? C126 C125 H125 120.0 . . ? C124 C125 H125 120.0 . . ? C125 C126 C121 120.0 . . ? C125 C126 H126 120.0 . . ? C121 C126 H126 120.0 . . ? C121 C127 H12A 109.5 . . ? C121 C127 H12B 109.5 . . ? H12A C127 H12B 109.5 . . ? C121 C127 H12C 109.5 . . ? H12A C127 H12C 109.5 . . ? H12B C127 H12C 109.5 . . ? C129 C128 C133 120.0 . . ? C129 C128 C134 117.3(15) . . ? C133 C128 C134 122.7(15) . . ? C130 C129 C128 120.0 . . ? C130 C129 H129 120.0 . . ? C128 C129 H129 120.0 . . ? C131 C130 C129 120.0 . . ? C131 C130 H130 120.0 . . ? C129 C130 H130 120.0 . . ? C130 C131 C132 120.0 . . ? C130 C131 H131 120.0 . . ? C132 C131 H131 120.0 . . ? C131 C132 C133 120.0 . . ? C131 C132 H132 120.0 . . ? C133 C132 H132 120.0 . . ? C132 C133 C128 120.0 . . ? C132 C133 H133 120.0 . . ? C128 C133 H133 120.0 . . ? C128 C134 H13A 109.5 . . ? C128 C134 H13B 109.5 . . ? H13A C134 H13B 109.5 . . ? C128 C134 H13C 109.5 . . ? H13A C134 H13C 109.5 . . ? H13B C134 H13C 109.5 . . ? C141 C135 C136 119(4) . . ? C141 C135 C140 121(4) . . ? C136 C135 C140 120.0 . . ? C137 C136 C135 120.0 . . ? C137 C136 H136 120.0 . . ? C135 C136 H136 120.0 . . ? C136 C137 C138 120.0 . . ? C136 C137 H137 120.0 . . ? C138 C137 H137 120.0 . . ? C137 C138 C139 120.0 . . ? C137 C138 H138 120.0 . . ? C139 C138 H138 120.0 . . ? C138 C139 C140 120.0 . . ? C138 C139 H139 120.0 . . ? C140 C139 H139 120.0 . . ? C139 C140 C135 120.0 . . ? C139 C140 H140 120.0 . . ? C135 C140 H140 120.0 . . ? C135 C141 H14A 109.5 . . ? C135 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C135 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C229 C228 C233 120.0 . . ? C229 C228 C234 118(3) . . ? C233 C228 C234 122(3) . . ? C230 C229 C228 120.0 . . ? C230 C229 H229 120.0 . . ? C228 C229 H229 120.0 . . ? C229 C230 C231 120.0 . . ? C229 C230 H230 120.0 . . ? C231 C230 H230 120.0 . . ? C230 C231 C232 120.0 . . ? C230 C231 H231 120.0 . . ? C232 C231 H231 120.0 . . ? C233 C232 C231 120.0 . . ? C233 C232 H232 120.0 . . ? C231 C232 H232 120.0 . . ? C232 C233 C228 120.0 . . ? C232 C233 H233 120.0 . . ? C228 C233 H233 120.0 . . ? C228 C234 H23A 109.5 . . ? C228 C234 H23B 109.5 . . ? H23A C234 H23B 109.5 . . ? C228 C234 H23C 109.5 . . ? H23A C234 H23C 109.5 . . ? H23B C234 H23C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O16 1.00 2.05 2.986(12) 155.8 . O2 H2 O7 1.00 1.91 2.902(11) 168.7 . _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 3.052 _refine_diff_density_min -1.932 _refine_diff_density_rms 0.151 # Attachment 'wge2.cif' data_wge2 _database_code_depnum_ccdc_archive 'CCDC 801778' #TrackingRef 'wge2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C120 H112 Nd4 O22' _chemical_formula_sum 'C120 H112 Nd4 O22' _chemical_formula_weight 2483.06 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' 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 12.378(3) _cell_length_b 15.353(3) _cell_length_c 15.713(3) _cell_angle_alpha 66.73(3) _cell_angle_beta 69.06(3) _cell_angle_gamma 74.93(3) _cell_volume 2537.3(9) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25247 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 25.0 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 2.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9400 _exptl_absorpt_correction_T_max 0.9594 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.773747856 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Australian synchrotron MX1' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25247 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6477 _reflns_number_gt 5442 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The phenyl ring of ligand 5 is disordered over 2 positions with refined occupancy of 76% for the major component. There is also disorder in the C-3 position of the 5-membered ring in ligand 4. Due to this disorder the Phenyl rings were constrained as perfect hexagons and the minor component of disorder was refined as one. ; _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^)+(0.0726P)^2^+7.6985P] 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 0.0084(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6477 _refine_ls_number_parameters 668 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Nd1 Nd 0.14287(3) 0.85547(2) 0.36343(2) 0.03791(17) Uani 1 1 d . . . Nd2 Nd -0.10816(3) 1.07293(2) 0.42061(2) 0.03514(16) Uani 1 1 d . . . O1 O -0.0068(4) 0.9141(3) 0.4902(3) 0.0383(11) Uani 1 1 d . . . H1 H -0.0634 0.8674 0.5325 0.046 Uiso 1 1 calc R . . O2 O 0.0173(4) 1.1898(3) 0.2914(3) 0.0455(12) Uani 1 1 d . . . O3 O 0.0165(4) 1.0056(3) 0.2911(3) 0.0397(11) Uani 1 1 d . . . O4 O 0.0161(4) 0.7354(3) 0.4656(3) 0.0446(12) Uani 1 1 d . . . O5 O 0.0954(5) 0.7923(4) 0.2663(4) 0.0576(14) Uani 1 1 d . . . O6 O 0.2627(4) 0.9203(3) 0.1970(3) 0.0493(13) Uani 1 1 d . . . O7 O 0.3203(4) 0.7488(3) 0.3371(3) 0.0526(13) Uani 1 1 d . . . O8 O -0.2320(4) 1.1775(3) 0.3219(3) 0.0432(11) Uani 1 1 d . . . O9 O -0.1965(4) 1.2144(3) 0.4758(3) 0.0380(11) Uani 1 1 d . . . O10 O -0.2461(4) 0.9763(3) 0.4505(3) 0.0491(13) Uani 1 1 d . C . O11 O -0.2138(4) 1.0226(3) 0.6004(3) 0.0383(11) Uani 1 1 d . . . C1 C 0.0435(6) 1.2128(5) 0.1998(5) 0.0406(16) Uani 1 1 d . . . C2 C 0.0678(7) 1.3153(5) 0.1430(5) 0.0487(18) Uani 1 1 d . . . C3 C -0.0069(8) 1.3880(5) 0.1800(6) 0.059(2) Uani 1 1 d . . . H3 H -0.0686 1.3714 0.2382 0.071 Uiso 1 1 calc R . . C4 C 0.0104(9) 1.4825(6) 0.1310(7) 0.076(3) Uani 1 1 d . . . H4 H -0.0406 1.5307 0.1555 0.091 Uiso 1 1 calc R . . C5 C 0.0998(9) 1.5079(7) 0.0481(7) 0.081(3) Uani 1 1 d . . . H5 H 0.1089 1.5735 0.0144 0.097 Uiso 1 1 calc R . . C6 C 0.1766(9) 1.4386(7) 0.0132(6) 0.074(3) Uani 1 1 d . . . H6 H 0.2413 1.4564 -0.0423 0.088 Uiso 1 1 calc R . . C7 C 0.1597(7) 1.3404(6) 0.0599(6) 0.060(2) Uani 1 1 d . . . H7 H 0.2108 1.2930 0.0343 0.072 Uiso 1 1 calc R . . C8 C 0.0429(6) 1.1514(5) 0.1531(5) 0.0421(17) Uani 1 1 d . . . C9 C 0.0253(6) 1.0550(5) 0.2006(5) 0.0407(17) Uani 1 1 d . . . C10 C 0.0194(7) 1.0114(5) 0.1329(5) 0.0424(17) Uani 1 1 d . . . H10A H -0.0504 0.9783 0.1604 0.051 Uiso 1 1 calc R . . H10B H 0.0900 0.9648 0.1200 0.051 Uiso 1 1 calc R . . C11 C 0.0122(7) 1.0952(5) 0.0401(5) 0.0470(18) Uani 1 1 d . . . H11A H -0.0694 1.1143 0.0367 0.056 Uiso 1 1 calc R . . H11B H 0.0615 1.0774 -0.0175 0.056 Uiso 1 1 calc R . . C12 C 0.0571(7) 1.1783(5) 0.0447(5) 0.052(2) Uani 1 1 d . . . H12A H 0.1399 1.1821 0.0061 0.063 Uiso 1 1 calc R . . H12B H 0.0097 1.2404 0.0205 0.063 Uiso 1 1 calc R . . C13 C -0.0438(7) 0.6823(5) 0.4604(5) 0.0437(17) Uani 1 1 d . . . C14 C -0.1077(7) 0.6168(5) 0.5566(5) 0.0490(18) Uani 1 1 d . . . C15 C -0.1403(7) 0.5320(5) 0.5670(6) 0.055(2) Uani 1 1 d . . . H15 H -0.1215 0.5141 0.5114 0.066 Uiso 1 1 calc R . . C16 C -0.1998(7) 0.4724(6) 0.6568(6) 0.062(2) Uani 1 1 d . . . H16 H -0.2221 0.4156 0.6614 0.074 Uiso 1 1 calc R . . C17 C -0.2263(8) 0.4966(6) 0.7396(7) 0.068(2) Uani 1 1 d . . . H17 H -0.2667 0.4564 0.8008 0.081 Uiso 1 1 calc R . . C18 C -0.1931(8) 0.5801(6) 0.7316(6) 0.068(2) Uani 1 1 d . . . H18 H -0.2115 0.5970 0.7877 0.082 Uiso 1 1 calc R . . C19 C -0.1323(7) 0.6402(6) 0.6409(6) 0.059(2) Uani 1 1 d . . . H19 H -0.1081 0.6960 0.6366 0.071 Uiso 1 1 calc R . . C20 C -0.0509(7) 0.6859(5) 0.3723(5) 0.0459(18) Uani 1 1 d . . . C21 C 0.0181(8) 0.7427(5) 0.2822(6) 0.054(2) Uani 1 1 d . . . C22 C -0.0073(11) 0.7314(6) 0.2001(6) 0.081(3) Uani 1 1 d . . . H22A H 0.0508 0.6820 0.1763 0.098 Uiso 1 1 calc R . . H22B H -0.0073 0.7926 0.1457 0.098 Uiso 1 1 calc R . . C23 C -0.1286(10) 0.7006(6) 0.2465(7) 0.078(3) Uani 1 1 d . . . H23A H -0.1417 0.6633 0.2129 0.094 Uiso 1 1 calc R . . H23B H -0.1904 0.7565 0.2463 0.094 Uiso 1 1 calc R . . C24 C -0.1249(8) 0.6368(6) 0.3520(6) 0.063(2) Uani 1 1 d . . . H24A H -0.2042 0.6358 0.3981 0.076 Uiso 1 1 calc R . . H24B H -0.0887 0.5704 0.3555 0.076 Uiso 1 1 calc R . . C25 C 0.3304(7) 0.8799(5) 0.1360(5) 0.0480(18) Uani 1 1 d . . . C26 C 0.3371(6) 0.9349(5) 0.0310(5) 0.052(2) Uani 1 1 d . . . C27 C 0.3501(8) 1.0318(6) -0.0085(6) 0.069(2) Uani 1 1 d . . . H27 H 0.3579 1.0632 0.0300 0.083 Uiso 1 1 calc R . . C28 C 0.3516(9) 1.0825(7) -0.1048(7) 0.081(3) Uani 1 1 d . . . H28 H 0.3640 1.1477 -0.1323 0.097 Uiso 1 1 calc R . . C29 C 0.3351(8) 1.0389(8) -0.1606(7) 0.075(3) Uani 1 1 d . . . H29 H 0.3324 1.0750 -0.2249 0.090 Uiso 1 1 calc R . . C30 C 0.3230(9) 0.9449(8) -0.1233(6) 0.079(3) Uani 1 1 d . . . H30 H 0.3132 0.9147 -0.1619 0.095 Uiso 1 1 calc R . . C31 C 0.3249(8) 0.8918(7) -0.0269(6) 0.072(3) Uani 1 1 d . . . H31 H 0.3178 0.8255 -0.0016 0.086 Uiso 1 1 calc R . . C32 C 0.3958(7) 0.7883(5) 0.1634(5) 0.0499(19) Uani 1 1 d . . . C33 C 0.3906(6) 0.7339(5) 0.2595(5) 0.0499(19) Uani 1 1 d . . . C34 C 0.4804(7) 0.6459(6) 0.2654(5) 0.056(2) Uani 1 1 d . . . H34A H 0.4423 0.5875 0.2934 0.067 Uiso 1 1 calc R . . H34B H 0.5286 0.6409 0.3061 0.067 Uiso 1 1 calc R . . C35 C 0.5548(9) 0.6581(6) 0.1626(6) 0.084(3) Uani 1 1 d . . . H35A H 0.5666 0.5982 0.1488 0.101 Uiso 1 1 calc R . . H35B H 0.6321 0.6737 0.1525 0.101 Uiso 1 1 calc R . . C36 C 0.4906(8) 0.7403(6) 0.0950(6) 0.065(2) Uani 1 1 d . . . H36A H 0.5442 0.7857 0.0448 0.077 Uiso 1 1 calc R . . H36B H 0.4556 0.7154 0.0630 0.077 Uiso 1 1 calc R . . C37 C -0.2793(6) 1.2646(5) 0.3014(5) 0.0428(17) Uani 1 1 d . . . C38 C -0.3265(6) 1.3028(5) 0.2152(5) 0.0424(17) Uani 1 1 d . . . C39 C -0.4352(7) 1.3589(5) 0.2161(6) 0.0526(19) Uani 1 1 d . . . H39 H -0.4832 1.3747 0.2719 0.063 Uiso 1 1 calc R . . C40 C -0.4724(7) 1.3918(5) 0.1316(6) 0.056(2) Uani 1 1 d . . . H40 H -0.5480 1.4271 0.1323 0.067 Uiso 1 1 calc R . . C41 C -0.4037(7) 1.3743(6) 0.0522(6) 0.060(2) Uani 1 1 d . . . H41 H -0.4286 1.4013 -0.0046 0.072 Uiso 1 1 calc R . . C42 C -0.2966(8) 1.3177(7) 0.0496(6) 0.069(2) Uani 1 1 d . . . H42 H -0.2490 1.3039 -0.0075 0.083 Uiso 1 1 calc R . . C43 C -0.2601(7) 1.2813(5) 0.1326(5) 0.054(2) Uani 1 1 d . . . H43 H -0.1876 1.2407 0.1325 0.065 Uiso 1 1 calc R . . C44 C -0.2826(6) 1.3269(5) 0.3495(5) 0.0416(17) Uani 1 1 d . B . C45 C -0.3265(8) 1.4331(5) 0.3210(5) 0.055(2) Uani 1 1 d D . . H45A H -0.4052 1.4463 0.3123 0.066 Uiso 1 1 calc R A 1 H45B H -0.2726 1.4691 0.2602 0.066 Uiso 1 1 calc R A 1 C46A C -0.2717(17) 1.4702(10) 0.3697(14) 0.061(6) Uani 0.63(3) 1 d P B 2 H46A H -0.2000 1.4973 0.3237 0.073 Uiso 0.63(3) 1 calc PR B 2 H46B H -0.3270 1.5209 0.3932 0.073 Uiso 0.63(3) 1 calc PR B 2 C47 C -0.2429(7) 1.3867(5) 0.4532(5) 0.0510(19) Uani 1 1 d D . . H47A H -0.2699 1.3731 0.5240 0.061 Uiso 1 1 calc R B 1 H47B H -0.1655 1.4090 0.4268 0.061 Uiso 1 1 calc R B 1 C48 C -0.2380(6) 1.2990(4) 0.4287(5) 0.0385(16) Uani 1 1 d . B . C49 C -0.3083(6) 0.9143(5) 0.5224(5) 0.0416(17) Uani 1 1 d . . . C50A C -0.3683(18) 0.8802(19) 0.4794(19) 0.028(9) Uiso 0.233(9) 1 d PG C 2 C51A C -0.3057(15) 0.8339(19) 0.4126(17) 0.073(7) Uani 0.233(9) 1 d PG C 2 H51A H -0.2234 0.8325 0.3871 0.088 Uiso 0.233(9) 1 calc PR C 2 C52A C -0.364(2) 0.7895(19) 0.3830(17) 0.073(7) Uani 0.233(9) 1 d PG C 2 H52A H -0.3208 0.7578 0.3373 0.088 Uiso 0.233(9) 1 calc PR C 2 C53A C -0.484(2) 0.792(2) 0.420(2) 0.073(7) Uani 0.233(9) 1 d PG C 2 H53A H -0.5235 0.7612 0.4002 0.088 Uiso 0.233(9) 1 calc PR C 2 C54A C -0.5465(15) 0.838(2) 0.4872(19) 0.073(7) Uani 0.233(9) 1 d PG C 2 H54A H -0.6288 0.8392 0.5127 0.088 Uiso 0.233(9) 1 calc PR C 2 C55A C -0.4887(18) 0.8822(19) 0.5168(17) 0.073(7) Uani 0.233(9) 1 d PG C 2 H55A H -0.5314 0.9139 0.5624 0.088 Uiso 0.233(9) 1 calc PR C 2 C50 C -0.3717(4) 0.8588(3) 0.4979(4) 0.043(4) Uani 0.767(9) 1 d PG C 1 C51 C -0.3657(5) 0.7597(3) 0.5328(4) 0.048(3) Uani 0.767(9) 1 d PG C 1 H51 H -0.3209 0.7219 0.5764 0.057 Uiso 0.767(9) 1 calc PR C 1 C52 C -0.4250(5) 0.7159(3) 0.5040(4) 0.049(3) Uani 0.767(9) 1 d PG C 1 H52 H -0.4209 0.6482 0.5279 0.059 Uiso 0.767(9) 1 calc PR C 1 C53 C -0.4905(5) 0.7713(4) 0.4402(4) 0.054(3) Uani 0.767(9) 1 d PG C 1 H53 H -0.5310 0.7413 0.4205 0.065 Uiso 0.767(9) 1 calc PR C 1 C54 C -0.4965(5) 0.8704(3) 0.4053(4) 0.049(3) Uani 0.767(9) 1 d PG C 1 H54 H -0.5413 0.9082 0.3617 0.058 Uiso 0.767(9) 1 calc PR C 1 C55 C -0.4372(4) 0.9142(3) 0.4341(3) 0.038(2) Uani 0.767(9) 1 d PG C 1 H55 H -0.4413 0.9819 0.4102 0.046 Uiso 0.767(9) 1 calc PR C 1 C46 C -0.3298(15) 1.4593(4) 0.4050(11) 0.057(10) Uani 0.37(3) 1 d PGD B 1 H46C H -0.3088 1.5244 0.3818 0.068 Uiso 0.37(3) 1 calc PR B 1 H46D H -0.4091 1.4579 0.4512 0.068 Uiso 0.37(3) 1 calc PR B 1 C56 C -0.3174(6) 0.8964(6) 0.6197(5) 0.0487(18) Uani 1 1 d . C . C57 C -0.2754(6) 0.9511(5) 0.6518(5) 0.0422(17) Uani 1 1 d . . . C58 C -0.3162(7) 0.9211(5) 0.7609(5) 0.0488(18) Uani 1 1 d . C . H58A H -0.3812 0.9679 0.7829 0.059 Uiso 1 1 calc R . . H58B H -0.2516 0.9145 0.7871 0.059 Uiso 1 1 calc R . . C59 C -0.3573(7) 0.8233(6) 0.7921(5) 0.056(2) Uani 1 1 d . . . H59A H -0.2930 0.7704 0.8041 0.067 Uiso 1 1 calc R C . H59B H -0.4238 0.8137 0.8517 0.067 Uiso 1 1 calc R . . C60 C -0.3944(7) 0.8276(6) 0.7071(5) 0.057(2) Uani 1 1 d . C . H60A H -0.3792 0.7636 0.7007 0.068 Uiso 1 1 calc R . . H60B H -0.4783 0.8527 0.7150 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0528(3) 0.0261(2) 0.0347(2) -0.01099(16) -0.01841(18) 0.00427(17) Nd2 0.0487(3) 0.0242(2) 0.0322(2) -0.00835(15) -0.01934(17) 0.00482(16) O1 0.051(3) 0.029(2) 0.031(2) -0.0092(19) -0.014(2) 0.003(2) O2 0.055(3) 0.037(3) 0.040(3) -0.012(2) -0.017(2) 0.004(2) O3 0.054(3) 0.032(2) 0.033(3) -0.009(2) -0.020(2) 0.004(2) O4 0.059(3) 0.037(3) 0.045(3) -0.018(2) -0.021(2) -0.004(2) O5 0.093(4) 0.038(3) 0.043(3) -0.012(2) -0.029(3) -0.001(3) O6 0.064(3) 0.035(3) 0.041(3) -0.013(2) -0.015(2) 0.007(2) O7 0.061(3) 0.047(3) 0.043(3) -0.014(2) -0.021(3) 0.010(2) O8 0.057(3) 0.024(2) 0.051(3) -0.009(2) -0.029(2) 0.005(2) O9 0.052(3) 0.024(2) 0.038(2) -0.0104(19) -0.018(2) 0.003(2) O10 0.067(3) 0.040(3) 0.044(3) -0.012(2) -0.031(3) 0.006(3) O11 0.047(3) 0.031(2) 0.039(3) -0.015(2) -0.015(2) 0.001(2) C1 0.045(4) 0.035(4) 0.042(4) -0.015(3) -0.015(3) -0.001(3) C2 0.054(4) 0.044(4) 0.044(4) -0.014(3) -0.013(4) -0.003(4) C3 0.076(6) 0.036(4) 0.058(5) -0.019(4) -0.005(4) -0.009(4) C4 0.097(7) 0.044(5) 0.071(6) -0.026(4) 0.002(5) -0.009(5) C5 0.101(7) 0.052(5) 0.074(6) -0.022(5) 0.000(6) -0.019(5) C6 0.085(6) 0.066(6) 0.054(5) -0.015(4) 0.002(5) -0.022(5) C7 0.072(6) 0.051(5) 0.052(5) -0.020(4) -0.010(4) -0.005(4) C8 0.051(4) 0.036(4) 0.037(4) -0.010(3) -0.020(3) 0.006(3) C9 0.045(4) 0.035(4) 0.038(4) -0.011(3) -0.018(3) 0.008(3) C10 0.056(4) 0.034(4) 0.041(4) -0.014(3) -0.018(3) -0.004(3) C11 0.068(5) 0.040(4) 0.036(4) -0.011(3) -0.028(4) 0.004(4) C12 0.070(5) 0.043(4) 0.038(4) -0.013(3) -0.021(4) 0.008(4) C13 0.056(4) 0.027(3) 0.055(5) -0.019(3) -0.025(4) 0.004(3) C14 0.057(5) 0.043(4) 0.048(4) -0.017(3) -0.017(4) -0.001(4) C15 0.068(5) 0.046(5) 0.058(5) -0.027(4) -0.021(4) 0.001(4) C16 0.071(5) 0.053(5) 0.064(5) -0.026(4) -0.016(4) -0.006(4) C17 0.074(6) 0.059(5) 0.064(6) -0.022(4) -0.011(4) -0.008(5) C18 0.084(6) 0.055(5) 0.060(5) -0.028(4) -0.005(5) -0.008(5) C19 0.071(5) 0.049(5) 0.056(5) -0.024(4) -0.011(4) -0.005(4) C20 0.062(5) 0.029(4) 0.054(5) -0.013(3) -0.030(4) -0.002(3) C21 0.087(6) 0.032(4) 0.054(5) -0.015(4) -0.040(4) 0.000(4) C22 0.163(11) 0.044(5) 0.054(5) -0.004(4) -0.066(6) -0.015(6) C23 0.123(9) 0.048(5) 0.090(7) -0.029(5) -0.068(7) 0.008(6) C24 0.083(6) 0.053(5) 0.071(6) -0.027(4) -0.041(5) 0.000(5) C25 0.060(5) 0.043(4) 0.039(4) -0.016(3) -0.014(4) -0.001(4) C26 0.050(4) 0.049(5) 0.039(4) -0.008(4) -0.010(3) 0.008(4) C27 0.085(6) 0.048(5) 0.057(5) -0.004(4) -0.023(5) 0.001(5) C28 0.093(7) 0.057(6) 0.060(6) 0.010(5) -0.022(5) -0.008(5) C29 0.070(6) 0.080(7) 0.046(5) -0.005(5) -0.009(4) 0.000(5) C30 0.089(7) 0.090(8) 0.048(5) -0.027(5) -0.019(5) 0.008(6) C31 0.091(7) 0.062(6) 0.051(5) -0.020(4) -0.024(5) 0.014(5) C32 0.061(5) 0.041(4) 0.040(4) -0.014(3) -0.015(3) 0.008(4) C33 0.052(4) 0.048(4) 0.045(4) -0.020(4) -0.016(4) 0.012(4) C34 0.062(5) 0.052(5) 0.049(5) -0.022(4) -0.020(4) 0.013(4) C35 0.091(7) 0.056(5) 0.067(6) -0.017(5) -0.009(5) 0.027(5) C36 0.070(5) 0.060(5) 0.055(5) -0.025(4) -0.017(4) 0.013(4) C37 0.050(4) 0.031(4) 0.040(4) -0.005(3) -0.017(3) 0.000(3) C38 0.054(4) 0.027(3) 0.042(4) -0.001(3) -0.021(3) -0.004(3) C39 0.052(4) 0.044(4) 0.057(5) -0.009(4) -0.022(4) -0.003(4) C40 0.054(5) 0.036(4) 0.066(6) 0.004(4) -0.034(4) 0.002(4) C41 0.065(5) 0.054(5) 0.048(5) 0.006(4) -0.031(4) -0.002(4) C42 0.086(6) 0.074(6) 0.038(4) -0.008(4) -0.023(4) -0.003(5) C43 0.059(5) 0.045(4) 0.052(5) -0.011(4) -0.024(4) 0.005(4) C44 0.050(4) 0.026(3) 0.044(4) -0.004(3) -0.020(3) 0.000(3) C45 0.073(5) 0.031(4) 0.054(5) -0.009(3) -0.025(4) 0.005(4) C46A 0.068(12) 0.019(7) 0.107(13) -0.010(7) -0.052(10) -0.003(7) C47 0.081(5) 0.024(4) 0.049(4) -0.010(3) -0.025(4) -0.004(4) C48 0.044(4) 0.025(3) 0.039(4) -0.008(3) -0.009(3) 0.000(3) C49 0.047(4) 0.028(4) 0.051(4) -0.013(3) -0.019(3) 0.001(3) C51A 0.075(13) 0.082(14) 0.069(14) -0.010(10) -0.046(11) -0.009(11) C52A 0.075(13) 0.082(14) 0.069(14) -0.010(10) -0.046(11) -0.009(11) C53A 0.075(13) 0.082(14) 0.069(14) -0.010(10) -0.046(11) -0.009(11) C54A 0.075(13) 0.082(14) 0.069(14) -0.010(10) -0.046(11) -0.009(11) C55A 0.075(13) 0.082(14) 0.069(14) -0.010(10) -0.046(11) -0.009(11) C50 0.061(7) 0.027(6) 0.030(5) 0.000(4) -0.014(5) 0.000(5) C51 0.052(6) 0.047(6) 0.040(5) -0.012(4) -0.019(4) 0.004(5) C52 0.046(5) 0.047(6) 0.054(6) -0.016(5) -0.018(5) 0.001(5) C53 0.053(6) 0.081(9) 0.043(6) -0.033(6) -0.013(5) -0.015(6) C54 0.049(6) 0.058(7) 0.045(6) -0.022(5) -0.025(5) 0.008(5) C55 0.039(5) 0.040(5) 0.035(5) -0.017(4) -0.015(4) 0.010(4) C46 0.049(17) 0.027(13) 0.12(3) -0.022(14) -0.054(17) -0.006(12) C56 0.053(4) 0.054(5) 0.046(4) -0.022(4) -0.017(4) -0.005(4) C57 0.050(4) 0.031(4) 0.043(4) -0.014(3) -0.017(3) 0.007(3) C58 0.050(4) 0.047(4) 0.043(4) -0.013(3) -0.015(3) 0.003(4) C59 0.063(5) 0.052(5) 0.048(5) -0.012(4) -0.017(4) -0.006(4) C60 0.064(5) 0.057(5) 0.047(5) -0.017(4) -0.003(4) -0.024(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 Nd1 O7 2.385(5) . ? Nd1 O5 2.392(6) . ? Nd1 O4 2.408(5) . ? Nd1 O6 2.443(5) . ? Nd1 O1 2.475(4) . ? Nd1 O3 2.525(4) . ? Nd1 O11 2.579(4) 2_576 ? Nd1 O9 2.581(4) 2_576 ? Nd1 Nd2 3.8167(10) 2_576 ? Nd2 O10 2.352(5) . ? Nd2 O8 2.405(4) . ? Nd2 O1 2.413(4) 2_576 ? Nd2 O1 2.449(4) . ? Nd2 O2 2.463(5) . ? Nd2 O3 2.486(4) . ? Nd2 O9 2.498(4) . ? Nd2 O11 2.539(4) . ? Nd2 Nd1 3.8167(9) 2_576 ? Nd2 Nd2 3.9563(16) 2_576 ? O1 Nd2 2.413(4) 2_576 ? O1 H1 1.0000 . ? O2 C1 1.276(8) . ? O3 C9 1.300(8) . ? O4 C13 1.277(9) . ? O5 C21 1.270(10) . ? O6 C25 1.276(8) . ? O7 C33 1.287(8) . ? O8 C37 1.273(8) . ? O9 C48 1.290(7) . ? O9 Nd1 2.581(4) 2_576 ? O10 C49 1.298(9) . ? O11 C57 1.317(8) . ? O11 Nd1 2.579(4) 2_576 ? C1 C8 1.407(10) . ? C1 C2 1.520(10) . ? C2 C7 1.385(11) . ? C2 C3 1.424(10) . ? C3 C4 1.380(11) . ? C3 H3 0.9500 . ? C4 C5 1.366(12) . ? C4 H4 0.9500 . ? C5 C6 1.378(13) . ? C5 H5 0.9500 . ? C6 C7 1.427(12) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.406(10) . ? C8 C12 1.540(9) . ? C9 C10 1.492(9) . ? C10 C11 1.530(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.552(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C20 1.398(10) . ? C13 C14 1.510(11) . ? C14 C15 1.393(11) . ? C14 C19 1.417(11) . ? C15 C16 1.400(11) . ? C15 H15 0.9500 . ? C16 C17 1.397(12) . ? C16 H16 0.9500 . ? C17 C18 1.393(12) . ? C17 H17 0.9500 . ? C18 C19 1.415(12) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.429(11) . ? C20 C24 1.504(11) . ? C21 C22 1.513(11) . ? C22 C23 1.525(14) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.568(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C32 1.413(10) . ? C25 C26 1.509(10) . ? C26 C31 1.384(12) . ? C26 C27 1.396(11) . ? C27 C28 1.397(12) . ? C27 H27 0.9500 . ? C28 C29 1.385(14) . ? C28 H28 0.9500 . ? C29 C30 1.353(14) . ? C29 H29 0.9500 . ? C30 C31 1.414(12) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.394(10) . ? C32 C36 1.533(10) . ? C33 C34 1.504(10) . ? C34 C35 1.511(11) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.541(11) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C44 1.421(10) . ? C37 C38 1.510(9) . ? C38 C43 1.379(10) . ? C38 C39 1.394(10) . ? C39 C40 1.419(11) . ? C39 H39 0.9500 . ? C40 C41 1.319(11) . ? C40 H40 0.9500 . ? C41 C42 1.381(12) . ? C41 H41 0.9500 . ? C42 C43 1.390(11) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C48 1.408(9) . ? C44 C45 1.513(9) . ? C45 C46A 1.512(18) . ? C45 C46 1.510(10) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46A C47 1.503(17) . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C47 C46 1.505(9) . ? C47 C48 1.522(9) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C49 C56 1.411(10) . ? C49 C50A 1.456(19) . ? C49 C50 1.521(8) . ? C50A C51A 1.3900 . ? C50A C55A 1.3900 . ? C51A C52A 1.3900 . ? C51A H51A 0.9500 . ? C52A C53A 1.3900 . ? C52A H52A 0.9500 . ? C53A C54A 1.3900 . ? C53A H53A 0.9500 . ? C54A C55A 1.3900 . ? C54A H54A 0.9500 . ? C55A H55A 0.9500 . ? C50 C51 1.3900 . ? C50 C55 1.3900 . ? C51 C52 1.3900 . ? C51 H51 0.9500 . ? C52 C53 1.3900 . ? C52 H52 0.9500 . ? C53 C54 1.3900 . ? C53 H53 0.9500 . ? C54 C55 1.3900 . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C46 H46C 0.9900 . ? C46 H46D 0.9900 . ? C56 C57 1.406(10) . ? C56 C60 1.534(11) . ? C57 C58 1.511(10) . ? C58 C59 1.545(11) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.533(11) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? 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 Nd1 O5 83.38(18) . . ? O7 Nd1 O4 97.22(17) . . ? O5 Nd1 O4 70.20(17) . . ? O7 Nd1 O6 70.93(16) . . ? O5 Nd1 O6 72.37(19) . . ? O4 Nd1 O6 141.79(16) . . ? O7 Nd1 O1 142.16(15) . . ? O5 Nd1 O1 122.82(18) . . ? O4 Nd1 O1 71.34(15) . . ? O6 Nd1 O1 138.88(15) . . ? O7 Nd1 O3 147.14(15) . . ? O5 Nd1 O3 84.31(16) . . ? O4 Nd1 O3 107.00(16) . . ? O6 Nd1 O3 76.32(15) . . ? O1 Nd1 O3 68.58(14) . . ? O7 Nd1 O11 99.67(16) . 2_576 ? O5 Nd1 O11 156.37(16) . 2_576 ? O4 Nd1 O11 131.81(15) . 2_576 ? O6 Nd1 O11 86.39(16) . 2_576 ? O1 Nd1 O11 67.72(15) . 2_576 ? O3 Nd1 O11 80.62(14) . 2_576 ? O7 Nd1 O9 73.96(15) . 2_576 ? O5 Nd1 O9 135.75(15) . 2_576 ? O4 Nd1 O9 75.50(15) . 2_576 ? O6 Nd1 O9 130.70(16) . 2_576 ? O1 Nd1 O9 68.28(13) . 2_576 ? O3 Nd1 O9 133.04(13) . 2_576 ? O11 Nd1 O9 66.59(14) 2_576 2_576 ? O7 Nd1 Nd2 109.12(12) . 2_576 ? O5 Nd1 Nd2 158.47(15) . 2_576 ? O4 Nd1 Nd2 90.43(11) . 2_576 ? O6 Nd1 Nd2 127.74(12) . 2_576 ? O1 Nd1 Nd2 38.07(10) . 2_576 ? O3 Nd1 Nd2 92.86(10) . 2_576 ? O11 Nd1 Nd2 41.38(10) 2_576 2_576 ? O9 Nd1 Nd2 40.47(9) 2_576 2_576 ? O10 Nd2 O8 76.91(16) . . ? O10 Nd2 O1 136.35(15) . 2_576 ? O8 Nd2 O1 137.96(14) . 2_576 ? O10 Nd2 O1 79.62(16) . . ? O8 Nd2 O1 150.88(15) . . ? O1 Nd2 O1 71.08(17) 2_576 . ? O10 Nd2 O2 143.21(16) . . ? O8 Nd2 O2 75.88(16) . . ? O1 Nd2 O2 79.86(16) 2_576 . ? O1 Nd2 O2 115.72(15) . . ? O10 Nd2 O3 86.95(16) . . ? O8 Nd2 O3 92.04(15) . . ? O1 Nd2 O3 111.09(15) 2_576 . ? O1 Nd2 O3 69.61(14) . . ? O2 Nd2 O3 69.84(15) . . ? O10 Nd2 O9 113.15(16) . . ? O8 Nd2 O9 72.09(14) . . ? O1 Nd2 O9 70.60(14) 2_576 . ? O1 Nd2 O9 134.04(14) . . ? O2 Nd2 O9 81.09(15) . . ? O3 Nd2 O9 149.67(14) . . ? O10 Nd2 O11 72.36(16) . . ? O8 Nd2 O11 113.26(15) . . ? O1 Nd2 O11 69.30(15) 2_576 . ? O1 Nd2 O11 75.00(14) . . ? O2 Nd2 O11 142.08(15) . . ? O3 Nd2 O11 141.63(14) . . ? O9 Nd2 O11 68.42(14) . . ? O10 Nd2 Nd1 113.34(12) . 2_576 ? O8 Nd2 Nd1 113.07(11) . 2_576 ? O1 Nd2 Nd1 39.24(10) 2_576 2_576 ? O1 Nd2 Nd1 91.94(10) . 2_576 ? O2 Nd2 Nd1 99.93(11) . 2_576 ? O3 Nd2 Nd1 150.21(10) . 2_576 ? O9 Nd2 Nd1 42.11(10) . 2_576 ? O11 Nd2 Nd1 42.17(10) . 2_576 ? O10 Nd2 Nd2 109.25(11) . 2_576 ? O8 Nd2 Nd2 173.56(11) . 2_576 ? O1 Nd2 Nd2 35.85(10) 2_576 2_576 ? O1 Nd2 Nd2 35.23(10) . 2_576 ? O2 Nd2 Nd2 99.28(11) . 2_576 ? O3 Nd2 Nd2 90.21(10) . 2_576 ? O9 Nd2 Nd2 103.17(10) . 2_576 ? O11 Nd2 Nd2 67.92(10) . 2_576 ? Nd1 Nd2 Nd2 63.17(3) 2_576 2_576 ? Nd2 O1 Nd2 108.92(17) 2_576 . ? Nd2 O1 Nd1 102.69(16) 2_576 . ? Nd2 O1 Nd1 111.62(16) . . ? Nd2 O1 H1 111.1 2_576 . ? Nd2 O1 H1 111.1 . . ? Nd1 O1 H1 111.1 . . ? C1 O2 Nd2 129.9(4) . . ? C9 O3 Nd2 120.9(4) . . ? C9 O3 Nd1 129.0(4) . . ? Nd2 O3 Nd1 108.76(15) . . ? C13 O4 Nd1 140.8(4) . . ? C21 O5 Nd1 133.9(5) . . ? C25 O6 Nd1 131.9(4) . . ? C33 O7 Nd1 131.4(4) . . ? C37 O8 Nd2 137.1(5) . . ? C48 O9 Nd2 128.9(4) . . ? C48 O9 Nd1 132.9(4) . 2_576 ? Nd2 O9 Nd1 97.42(14) . 2_576 ? C49 O10 Nd2 139.4(4) . . ? C57 O11 Nd2 127.5(4) . . ? C57 O11 Nd1 135.8(4) . 2_576 ? Nd2 O11 Nd1 96.45(16) . 2_576 ? O2 C1 C8 123.6(6) . . ? O2 C1 C2 115.1(6) . . ? C8 C1 C2 121.2(6) . . ? C7 C2 C3 119.2(7) . . ? C7 C2 C1 123.4(7) . . ? C3 C2 C1 117.3(6) . . ? C4 C3 C2 119.9(8) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 121.2(8) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 120.2(9) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 120.4(8) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C2 C7 C6 119.0(8) . . ? C2 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C1 C8 C9 124.2(6) . . ? C1 C8 C12 126.6(6) . . ? C9 C8 C12 109.2(6) . . ? O3 C9 C8 126.9(6) . . ? O3 C9 C10 121.7(6) . . ? C8 C9 C10 111.4(6) . . ? C9 C10 C11 105.4(6) . . ? C9 C10 H10A 110.7 . . ? C11 C10 H10A 110.7 . . ? C9 C10 H10B 110.7 . . ? C11 C10 H10B 110.7 . . ? H10A C10 H10B 108.8 . . ? C10 C11 C12 105.9(5) . . ? C10 C11 H11A 110.6 . . ? C12 C11 H11A 110.6 . . ? C10 C11 H11B 110.6 . . ? C12 C11 H11B 110.6 . . ? H11A C11 H11B 108.7 . . ? C8 C12 C11 103.6(6) . . ? C8 C12 H12A 111.0 . . ? C11 C12 H12A 111.0 . . ? C8 C12 H12B 111.0 . . ? C11 C12 H12B 111.0 . . ? H12A C12 H12B 109.0 . . ? O4 C13 C20 122.4(7) . . ? O4 C13 C14 115.0(6) . . ? C20 C13 C14 122.6(7) . . ? C15 C14 C19 118.1(7) . . ? C15 C14 C13 122.9(7) . . ? C19 C14 C13 119.0(7) . . ? C14 C15 C16 122.0(7) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C17 C16 C15 119.9(8) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C18 C17 C16 119.4(9) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 120.8(8) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C14 C19 C18 119.8(8) . . ? C14 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C13 C20 C21 121.3(7) . . ? C13 C20 C24 130.1(7) . . ? C21 C20 C24 108.7(7) . . ? O5 C21 C20 129.3(7) . . ? O5 C21 C22 121.3(8) . . ? C20 C21 C22 109.3(8) . . ? C21 C22 C23 103.1(8) . . ? C21 C22 H22A 111.1 . . ? C23 C22 H22A 111.1 . . ? C21 C22 H22B 111.1 . . ? C23 C22 H22B 111.1 . . ? H22A C22 H22B 109.1 . . ? C22 C23 C24 102.3(7) . . ? C22 C23 H23A 111.3 . . ? C24 C23 H23A 111.3 . . ? C22 C23 H23B 111.3 . . ? C24 C23 H23B 111.3 . . ? H23A C23 H23B 109.2 . . ? C20 C24 C23 102.9(7) . . ? C20 C24 H24A 111.2 . . ? C23 C24 H24A 111.2 . . ? C20 C24 H24B 111.2 . . ? C23 C24 H24B 111.2 . . ? H24A C24 H24B 109.1 . . ? O6 C25 C32 122.8(6) . . ? O6 C25 C26 116.5(6) . . ? C32 C25 C26 120.7(6) . . ? C31 C26 C27 118.5(7) . . ? C31 C26 C25 120.9(7) . . ? C27 C26 C25 120.5(8) . . ? C26 C27 C28 119.8(9) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 120.8(9) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C30 C29 C28 119.9(9) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.0(10) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C26 C31 C30 120.9(9) . . ? C26 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C33 C32 C25 122.8(6) . . ? C33 C32 C36 110.6(6) . . ? C25 C32 C36 126.2(6) . . ? O7 C33 C32 128.9(6) . . ? O7 C33 C34 120.4(6) . . ? C32 C33 C34 110.7(6) . . ? C33 C34 C35 105.5(6) . . ? C33 C34 H34A 110.6 . . ? C35 C34 H34A 110.6 . . ? C33 C34 H34B 110.6 . . ? C35 C34 H34B 110.6 . . ? H34A C34 H34B 108.8 . . ? C34 C35 C36 107.8(7) . . ? C34 C35 H35A 110.1 . . ? C36 C35 H35A 110.1 . . ? C34 C35 H35B 110.1 . . ? C36 C35 H35B 110.1 . . ? H35A C35 H35B 108.5 . . ? C32 C36 C35 103.5(6) . . ? C32 C36 H36A 111.1 . . ? C35 C36 H36A 111.1 . . ? C32 C36 H36B 111.1 . . ? C35 C36 H36B 111.1 . . ? H36A C36 H36B 109.0 . . ? O8 C37 C44 124.4(6) . . ? O8 C37 C38 115.6(6) . . ? C44 C37 C38 119.8(6) . . ? C43 C38 C39 118.7(7) . . ? C43 C38 C37 118.9(6) . . ? C39 C38 C37 122.3(7) . . ? C38 C39 C40 118.5(7) . . ? C38 C39 H39 120.8 . . ? C40 C39 H39 120.8 . . ? C41 C40 C39 121.1(7) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C40 C41 C42 121.7(7) . . ? C40 C41 H41 119.2 . . ? C42 C41 H41 119.2 . . ? C41 C42 C43 118.3(8) . . ? C41 C42 H42 120.9 . . ? C43 C42 H42 120.9 . . ? C38 C43 C42 121.6(7) . . ? C38 C43 H43 119.2 . . ? C42 C43 H43 119.2 . . ? C48 C44 C37 124.2(6) . . ? C48 C44 C45 109.6(6) . . ? C37 C44 C45 126.1(6) . . ? C46A C45 C44 104.1(7) . . ? C46A C45 C46 28.6(8) . . ? C44 C45 C46 103.7(6) . . ? C46A C45 H45A 133.3 . . ? C44 C45 H45A 111.0 . . ? C46 C45 H45A 111.0 . . ? C46A C45 H45B 84.8 . . ? C44 C45 H45B 111.0 . . ? C46 C45 H45B 111.0 . . ? H45A C45 H45B 109.0 . . ? C47 C46A C45 107.1(10) . . ? C47 C46A H46A 110.3 . . ? C45 C46A H46A 110.3 . . ? C47 C46A H46B 110.3 . . ? C45 C46A H46B 110.3 . . ? H46A C46A H46B 108.6 . . ? C46A C47 C46 28.7(8) . . ? C46A C47 C48 104.5(8) . . ? C46 C47 C48 103.0(6) . . ? C46A C47 H47A 132.9 . . ? C46 C47 H47A 111.2 . . ? C48 C47 H47A 111.2 . . ? C46A C47 H47B 84.4 . . ? C46 C47 H47B 111.2 . . ? C48 C47 H47B 111.2 . . ? H47A C47 H47B 109.1 . . ? O9 C48 C44 128.4(6) . . ? O9 C48 C47 122.1(6) . . ? C44 C48 C47 109.5(6) . . ? O10 C49 C56 122.9(7) . . ? O10 C49 C50A 105.4(12) . . ? C56 C49 C50A 131.4(12) . . ? O10 C49 C50 117.1(6) . . ? C56 C49 C50 120.0(6) . . ? C50A C49 C50 12.9(11) . . ? C51A C50A C55A 120.0 . . ? C51A C50A C49 120.8(14) . . ? C55A C50A C49 118.5(15) . . ? C50A C51A C52A 120.0 . . ? C50A C51A H51A 120.0 . . ? C52A C51A H51A 120.0 . . ? C53A C52A C51A 120.0 . . ? C53A C52A H52A 120.0 . . ? C51A C52A H52A 120.0 . . ? C54A C53A C52A 120.0 . . ? C54A C53A H53A 120.0 . . ? C52A C53A H53A 120.0 . . ? C53A C54A C55A 120.0 . . ? C53A C54A H54A 120.0 . . ? C55A C54A H54A 120.0 . . ? C54A C55A C50A 120.0 . . ? C54A C55A H55A 120.0 . . ? C50A C55A H55A 120.0 . . ? C51 C50 C55 120.0 . . ? C51 C50 C49 124.6(3) . . ? C55 C50 C49 115.4(3) . . ? C50 C51 C52 120.0 . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C53 C52 C51 120.0 . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C54 C53 C52 120.0 . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C55 120.0 . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C54 C55 C50 120.0 . . ? C54 C55 H55 120.0 . . ? C50 C55 H55 120.0 . . ? C47 C46 C45 107.1(9) . . ? C47 C46 H46C 110.3 . . ? C45 C46 H46C 110.3 . . ? C47 C46 H46D 110.3 . . ? C45 C46 H46D 110.3 . . ? H46C C46 H46D 108.5 . . ? C57 C56 C49 125.0(7) . . ? C57 C56 C60 109.3(6) . . ? C49 C56 C60 124.7(7) . . ? O11 C57 C56 128.9(6) . . ? O11 C57 C58 120.5(6) . . ? C56 C57 C58 110.6(6) . . ? C57 C58 C59 103.4(6) . . ? C57 C58 H58A 111.1 . . ? C59 C58 H58A 111.1 . . ? C57 C58 H58B 111.1 . . ? C59 C58 H58B 111.1 . . ? H58A C58 H58B 109.0 . . ? C60 C59 C58 105.1(6) . . ? C60 C59 H59A 110.7 . . ? C58 C59 H59A 110.7 . . ? C60 C59 H59B 110.7 . . ? C58 C59 H59B 110.7 . . ? H59A C59 H59B 108.8 . . ? C56 C60 C59 103.1(6) . . ? C56 C60 H60A 111.1 . . ? C59 C60 H60A 111.1 . . ? C56 C60 H60B 111.1 . . ? C59 C60 H60B 111.1 . . ? H60A C60 H60B 109.1 . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 1.268 _refine_diff_density_min -1.254 _refine_diff_density_rms 0.114 # Attachment 'wgex1.cif' data_wgex1 _database_code_depnum_ccdc_archive 'CCDC 819703' #TrackingRef 'wgex1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C251 H118 Er8 F80 O46' _chemical_formula_weight 6727.53 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 14.094(3) _cell_length_b 15.287(3) _cell_length_c 29.950(6) _cell_angle_alpha 95.26(3) _cell_angle_beta 100.82(3) _cell_angle_gamma 106.50(3) _cell_volume 6004(2) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 82925 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.861 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3256 _exptl_absorpt_coefficient_mu 2.901 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.710698 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Australian synchrotron MX1' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'scans in phi' _diffrn_detector_area_resol_mean none _diffrn_standards_number 0 _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 74072 _diffrn_reflns_av_R_equivalents 0.1496 _diffrn_reflns_av_sigmaI/netI 0.1066 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 19416 _reflns_number_gt 12354 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Blu-Ice (McPhillips et al, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEED _computing_publication_material 'XCIF V6.12 (BrukerAXS, 2001).' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The thermal parameters for O2, C123 and C96 were constrained using the ISOR command. The thermal parameters for the carbon atoms C40 to C45 in the phenyl ring of ligand 3 were refined as one parameter. The toluene solvent molecule was constrained as a perfect hexagon and with refined occupancies of 50%. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+150.0315P] 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 19416 _refine_ls_number_parameters 1688 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1291 _refine_ls_R_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.1957 _refine_ls_wR_factor_gt 0.1732 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.17770(5) 0.81449(5) 0.29515(2) 0.028 Uani 1 1 d . . . Er2 Er 0.45439(5) 0.83214(5) 0.29308(2) 0.031 Uani 1 1 d . . . Er3 Er 0.27740(5) 0.76093(5) 0.18751(2) 0.027 Uani 1 1 d . . . Er4 Er 0.23163(5) 0.60794(5) 0.27971(3) 0.031 Uani 1 1 d . . . F1 F 0.2826(8) 1.1470(7) 0.3410(4) 0.069 Uani 1 1 d . . . F2 F 0.4221(10) 1.3157(8) 0.3653(5) 0.088 Uani 1 1 d . . . F3 F 0.5898(10) 1.3419(8) 0.4314(5) 0.089 Uani 1 1 d . . . F4 F 0.6213(9) 1.1977(9) 0.4726(5) 0.092 Uani 1 1 d . . . F5 F 0.4829(9) 1.0312(7) 0.4491(4) 0.065 Uani 1 1 d . . . F6 F 0.2246(6) 0.6880(6) 0.4091(3) 0.040 Uani 1 1 d . . . F7 F 0.2388(7) 0.6125(7) 0.4859(3) 0.051 Uani 1 1 d . . . F8 F 0.0878(7) 0.4661(7) 0.4955(3) 0.051 Uani 1 1 d . . . F9 F -0.0822(7) 0.3957(7) 0.4271(3) 0.052 Uani 1 1 d . . . F10 F -0.1025(7) 0.4691(6) 0.3510(3) 0.045 Uani 1 1 d . . . F11 F 0.8230(9) 1.0234(9) 0.4002(5) 0.091 Uani 1 1 d . . . F12 F 0.9461(12) 0.9699(15) 0.4600(7) 0.153 Uani 1 1 d . . . F13 F 0.8707(14) 0.8655(14) 0.5229(6) 0.136 Uani 1 1 d . . . F14 F 0.6716(13) 0.8078(10) 0.5183(4) 0.100 Uani 1 1 d . . . F15 F 0.5447(11) 0.8535(10) 0.4551(4) 0.088 Uani 1 1 d . . . F16 F 0.3861(8) 1.0069(7) 0.1889(3) 0.051 Uani 1 1 d . . . F17 F 0.3473(8) 1.0907(8) 0.1166(4) 0.066 Uani 1 1 d . . . F18 F 0.4329(9) 1.0758(9) 0.0450(4) 0.076 Uani 1 1 d . . . F19 F 0.5672(9) 0.9780(9) 0.0471(4) 0.072 Uani 1 1 d . . . F20 F 0.6135(7) 0.8972(7) 0.1196(3) 0.049 Uani 1 1 d . . . F21 F -0.0516(8) 0.7884(7) 0.1495(4) 0.066 Uani 1 1 d . . . F22 F -0.1995(8) 0.8681(8) 0.1532(5) 0.074 Uani 1 1 d . . . F23 F -0.1692(8) 1.0434(8) 0.1377(5) 0.075 Uani 1 1 d . . . F24 F 0.0047(12) 1.1392(10) 0.1186(10) 0.197 Uani 1 1 d . . . F25 F 0.1514(12) 1.0605(10) 0.1134(8) 0.147 Uani 1 1 d . . . F26 F 0.2679(8) 0.4251(8) 0.0570(4) 0.073 Uani 1 1 d . . . F27 F 0.4096(10) 0.3706(9) 0.0277(5) 0.092 Uani 1 1 d . . . F28 F 0.6022(9) 0.4826(11) 0.0465(4) 0.091 Uani 1 1 d . . . F29 F 0.6510(8) 0.6534(9) 0.0937(4) 0.076 Uani 1 1 d . . . F30 F 0.5124(7) 0.7112(7) 0.1236(4) 0.054 Uani 1 1 d . . . F31 F -0.0691(8) 0.2645(7) 0.1868(4) 0.068 Uani 1 1 d . . . F32 F -0.2708(8) 0.1986(9) 0.1587(5) 0.086 Uani 1 1 d . . . F33 F -0.3783(8) 0.3161(11) 0.1401(5) 0.107 Uani 1 1 d . . . F34 F -0.2844(9) 0.5014(10) 0.1519(5) 0.096 Uani 1 1 d . . . F35 F -0.0843(8) 0.5689(7) 0.1816(4) 0.062 Uani 1 1 d . . . F36 F 0.5401(9) 0.5174(9) 0.3363(4) 0.073 Uani 1 1 d . . . F37 F 0.7235(10) 0.5518(10) 0.3935(6) 0.099 Uani 1 1 d . . . F38 F 0.7483(8) 0.5996(10) 0.4860(5) 0.096 Uani 1 1 d . . . F39 F 0.5877(9) 0.6135(9) 0.5201(4) 0.073 Uani 1 1 d . . . F40 F 0.4058(8) 0.5831(8) 0.4631(4) 0.067 Uani 1 1 d . . . O1 O 0.3153(8) 0.7613(7) 0.3227(3) 0.034 Uani 1 1 d . . . H1 H 0.3313 0.7632 0.3569 0.041 Uiso 1 1 calc R . . O2 O 0.3110(6) 0.8637(6) 0.2559(3) 0.019 Uani 1 1 d U . . H2 H 0.3247 0.9295 0.2510 0.022 Uiso 1 1 calc R . . O3 O 0.3564(7) 0.6966(7) 0.2457(3) 0.034 Uani 1 1 d . . . H3 H 0.3983 0.6603 0.2344 0.040 Uiso 1 1 calc R . . O4 O 0.1680(8) 0.7063(6) 0.2338(3) 0.032 Uani 1 1 d . . . H4 H 0.0967 0.6757 0.2159 0.038 Uiso 1 1 calc R . . O5 O 0.2767(9) 0.9570(8) 0.3365(4) 0.044 Uani 1 1 d . . . O6 O 0.1240(8) 0.8323(7) 0.3614(4) 0.039 Uani 1 1 d . . . O7 O 0.1290(7) 0.6636(7) 0.3193(3) 0.030 Uani 1 1 d . . . O8 O 0.0000(9) 0.7457(7) 0.2677(3) 0.040 Uani 1 1 d . . . O9 O 0.5256(9) 0.8858(9) 0.3675(4) 0.052 Uani 1 1 d . . . O10 O 0.5066(8) 0.9929(8) 0.2999(4) 0.047 Uani 1 1 d . . . O11 O 0.4593(7) 0.8540(7) 0.2137(4) 0.033 Uani 1 1 d . . . O12 O 0.6191(8) 0.8607(7) 0.2853(4) 0.036 Uani 1 1 d . . . O13 O 0.1703(7) 0.8526(7) 0.1682(3) 0.035 Uani 1 1 d . . . O14 O 0.2987(7) 0.8056(7) 0.1183(4) 0.033 Uani 1 1 d . . . O15 O 0.3406(7) 0.6537(7) 0.1536(3) 0.036 Uani 1 1 d . . . O16 O 0.1403(8) 0.6525(7) 0.1413(3) 0.038 Uani 1 1 d . . . O17 O 0.0767(8) 0.5251(7) 0.2338(4) 0.037 Uani 1 1 d . . . O18 O 0.2632(8) 0.5062(7) 0.2306(4) 0.041 Uani 1 1 d . . . O19 O 0.3622(9) 0.5878(8) 0.3347(4) 0.049 Uani 1 1 d . . . O20 O 0.1622(9) 0.4833(8) 0.3132(4) 0.050 Uani 1 1 d . . . O21 O 0.1231(8) 0.9096(7) 0.2450(3) 0.034 Uani 1 1 d . . . O22 O 0.5238(9) 0.7144(9) 0.3213(5) 0.058 Uani 1 1 d . . . O23 O 0.1631(15) 1.0946(11) 0.2362(8) 0.114 Uani 1 1 d . . . C1 C 0.2973(12) 0.9893(10) 0.3789(5) 0.032 Uani 1 1 d . . . C2 C 0.3781(13) 1.0824(11) 0.3935(6) 0.044 Uani 1 1 d . . . C3 C 0.3655(14) 1.1553(12) 0.3727(6) 0.047 Uani 1 1 d . . . C4 C 0.4355(16) 1.2437(12) 0.3859(7) 0.059 Uani 1 1 d . . . C5 C 0.5215(16) 1.2569(14) 0.4197(8) 0.070 Uani 1 1 d . . . C6 C 0.5356(14) 1.1859(14) 0.4404(7) 0.060 Uani 1 1 d . . . C7 C 0.4653(13) 1.0993(12) 0.4286(7) 0.050 Uani 1 1 d . . . C8 C 0.2523(12) 0.9498(11) 0.4121(6) 0.037 Uani 1 1 d . . . H8 H 0.2808 0.9768 0.4434 0.045 Uiso 1 1 calc R . . C9 C 0.1659(11) 0.8713(10) 0.4019(5) 0.028 Uani 1 1 d . . . C10 C 0.1146(13) 0.8353(11) 0.4388(5) 0.038 Uani 1 1 d . . . C11 C 0.1676(18) 0.8424(13) 0.4836(6) 0.062 Uani 1 1 d . . . H11 H 0.2376 0.8771 0.4919 0.074 Uiso 1 1 calc R . . C12 C 0.1230(18) 0.8012(14) 0.5165(7) 0.067 Uani 1 1 d . . . H12 H 0.1613 0.8083 0.5470 0.081 Uiso 1 1 calc R . . C13 C 0.0243(19) 0.7507(14) 0.5049(7) 0.070 Uani 1 1 d . . . H13 H -0.0073 0.7218 0.5274 0.085 Uiso 1 1 calc R . . C14 C -0.0316(17) 0.7406(15) 0.4602(7) 0.072 Uani 1 1 d . . . H14 H -0.1014 0.7053 0.4519 0.086 Uiso 1 1 calc R . . C15 C 0.0169(14) 0.7833(13) 0.4278(6) 0.050 Uani 1 1 d . . . H15 H -0.0205 0.7754 0.3970 0.060 Uiso 1 1 calc R . . C16 C 0.0475(12) 0.6309(10) 0.3353(5) 0.032 Uani 1 1 d . . . C17 C 0.0608(11) 0.5816(10) 0.3769(5) 0.032 Uani 1 1 d . . . C18 C 0.1473(13) 0.6161(11) 0.4120(6) 0.042 Uani 1 1 d . . . C19 C 0.1579(12) 0.5767(11) 0.4521(5) 0.036 Uani 1 1 d . . . C20 C 0.0794(16) 0.5030(13) 0.4575(6) 0.051 Uani 1 1 d . . . C21 C -0.0056(13) 0.4686(11) 0.4227(6) 0.041 Uani 1 1 d . . . C22 C -0.0156(12) 0.5076(11) 0.3839(5) 0.036 Uani 1 1 d . . . C23 C -0.0479(12) 0.6404(12) 0.3186(5) 0.039 Uani 1 1 d . . . H23 H -0.1021 0.6132 0.3326 0.047 Uiso 1 1 calc R . . C24 C -0.0668(11) 0.6889(10) 0.2817(5) 0.034 Uani 1 1 d . . . C25 C -0.1767(12) 0.6737(11) 0.2597(5) 0.037 Uani 1 1 d . . . C26 C -0.2002(12) 0.7314(11) 0.2290(5) 0.037 Uani 1 1 d . . . H26 H -0.1476 0.7791 0.2221 0.045 Uiso 1 1 calc R . . C27 C -0.2999(12) 0.7192(12) 0.2086(6) 0.041 Uani 1 1 d . . . H27 H -0.3159 0.7589 0.1878 0.050 Uiso 1 1 calc R . . C28 C -0.3758(13) 0.6508(12) 0.2181(6) 0.050 Uani 1 1 d . . . H28 H -0.4443 0.6423 0.2033 0.059 Uiso 1 1 calc R . . C29 C -0.3543(14) 0.5946(13) 0.2485(7) 0.055 Uani 1 1 d . . . H29 H -0.4080 0.5483 0.2555 0.066 Uiso 1 1 calc R . . C30 C -0.2543(13) 0.6044(14) 0.2693(7) 0.057 Uani 1 1 d . . . H30 H -0.2394 0.5639 0.2898 0.069 Uiso 1 1 calc R . . C31 C 0.6057(13) 0.9583(12) 0.3848(5) 0.043 Uani 1 1 d . . . C32 C 0.6782(14) 0.9403(13) 0.4252(6) 0.052 Uani 1 1 d . . . C33 C 0.7827(16) 0.9714(15) 0.4303(7) 0.061 Uani 1 1 d . . . C34 C 0.843(2) 0.9416(17) 0.4593(9) 0.085 Uani 1 1 d . . . C35 C 0.802(3) 0.890(2) 0.4919(8) 0.101 Uani 1 1 d . . . C36 C 0.707(2) 0.8623(17) 0.4887(8) 0.080 Uani 1 1 d . . . C37 C 0.6407(16) 0.8864(14) 0.4532(8) 0.061 Uani 1 1 d . . . C38 C 0.6301(14) 1.0391(12) 0.3686(7) 0.052 Uani 1 1 d . . . H38 H 0.6878 1.0875 0.3857 0.062 Uiso 1 1 calc R . . C39 C 0.5748(12) 1.0566(13) 0.3271(6) 0.048 Uani 1 1 d . . . C40 C 0.6060(19) 1.1490(16) 0.3152(11) 0.094 Uani 1 1 d . . . C41 C 0.5779(19) 1.1592(16) 0.2717(11) 0.094 Uani 1 1 d . . . H41 H 0.5436 1.1047 0.2500 0.113 Uiso 1 1 calc R . . C42 C 0.5956(18) 1.2486(15) 0.2539(11) 0.094 Uani 1 1 d . . . H42 H 0.5724 1.2531 0.2226 0.113 Uiso 1 1 calc R . . C43 C 0.6480(18) 1.3238(16) 0.2865(10) 0.094 Uani 1 1 d . . . H43 H 0.6614 1.3840 0.2783 0.113 Uiso 1 1 calc R . . C44 C 0.6816(19) 1.3125(16) 0.3315(11) 0.094 Uani 1 1 d . . . H44 H 0.7192 1.3659 0.3534 0.113 Uiso 1 1 calc R . . C45 C 0.6635(18) 1.2297(15) 0.3457(11) 0.094 Uani 1 1 d . . . H45 H 0.6900 1.2258 0.3768 0.113 Uiso 1 1 calc R . . C46 C 0.5298(10) 0.9097(10) 0.2002(5) 0.027 Uani 1 1 d . . . C47 C 0.5018(12) 0.9509(10) 0.1573(5) 0.033 Uani 1 1 d . . . C48 C 0.4352(12) 0.9993(12) 0.1551(6) 0.041 Uani 1 1 d . . . C49 C 0.4145(13) 1.0447(13) 0.1173(6) 0.046 Uani 1 1 d . . . C50 C 0.4600(15) 1.0370(13) 0.0819(7) 0.053 Uani 1 1 d . . . C51 C 0.5229(14) 0.9863(14) 0.0820(6) 0.049 Uani 1 1 d . . . C52 C 0.5479(12) 0.9449(12) 0.1198(6) 0.041 Uani 1 1 d . . . C53 C 0.6310(12) 0.9370(11) 0.2219(6) 0.040 Uani 1 1 d . . . H53 H 0.6768 0.9772 0.2077 0.048 Uiso 1 1 calc R . . C54 C 0.6734(11) 0.9109(10) 0.2632(6) 0.033 Uani 1 1 d . . . C55 C 0.7859(6) 0.9391(9) 0.2800(4) 0.045 Uani 1 1 d G . . C56 C 0.8524(9) 0.9976(9) 0.2589(4) 0.060 Uani 1 1 d G . . H56 H 0.8268 1.0215 0.2326 0.072 Uiso 1 1 calc R . . C57 C 0.9566(8) 1.0213(9) 0.2762(5) 0.062 Uani 1 1 d G . . H57 H 1.0021 1.0614 0.2617 0.075 Uiso 1 1 calc R . . C58 C 0.9942(6) 0.9865(10) 0.3146(5) 0.065 Uani 1 1 d G . . H58 H 1.0654 1.0027 0.3264 0.078 Uiso 1 1 calc R . . C59 C 0.9276(9) 0.9279(11) 0.3357(4) 0.090 Uani 1 1 d G . . H59 H 0.9533 0.9041 0.3620 0.108 Uiso 1 1 calc R . . C60 C 0.8235(8) 0.9042(10) 0.3184(5) 0.094 Uani 1 1 d G . . H60 H 0.7780 0.8642 0.3329 0.112 Uiso 1 1 calc R . . C61 C 0.1374(12) 0.8757(11) 0.1301(6) 0.038 Uani 1 1 d . . . C62 C 0.0515(13) 0.9184(11) 0.1308(6) 0.041 Uani 1 1 d . . . C63 C -0.0342(13) 0.8756(12) 0.1413(7) 0.049 Uani 1 1 d . . . C64 C -0.1119(13) 0.9157(13) 0.1432(7) 0.048 Uani 1 1 d . . . C65 C -0.0958(13) 1.0039(14) 0.1357(7) 0.056 Uani 1 1 d . . . C66 C -0.0117(18) 1.0514(15) 0.1276(11) 0.093 Uani 1 1 d . . . C67 C 0.0646(14) 1.0077(16) 0.1259(11) 0.089 Uani 1 1 d . . . C68 C 0.1673(14) 0.8642(13) 0.0896(6) 0.051 Uani 1 1 d . . . H68 H 0.1317 0.8813 0.0633 0.061 Uiso 1 1 calc R . . C69 C 0.2489(13) 0.8278(11) 0.0842(5) 0.038 Uani 1 1 d . . . C70 C 0.2782(14) 0.8193(12) 0.0395(5) 0.045 Uani 1 1 d . . . C71 C 0.3544(14) 0.7801(12) 0.0370(6) 0.048 Uani 1 1 d . . . H71 H 0.3848 0.7598 0.0635 0.058 Uiso 1 1 calc R . . C72 C 0.3876(16) 0.7698(13) -0.0037(7) 0.058 Uani 1 1 d . . . H72 H 0.4402 0.7430 -0.0053 0.070 Uiso 1 1 calc R . . C73 C 0.3403(17) 0.8005(14) -0.0424(6) 0.062 Uani 1 1 d . . . H73 H 0.3617 0.7951 -0.0705 0.075 Uiso 1 1 calc R . . C74 C 0.2633(16) 0.8381(15) -0.0396(6) 0.059 Uani 1 1 d . . . H74 H 0.2300 0.8567 -0.0660 0.070 Uiso 1 1 calc R . . C75 C 0.2352(16) 0.8485(14) 0.0009(6) 0.058 Uani 1 1 d . . . H75 H 0.1841 0.8771 0.0027 0.069 Uiso 1 1 calc R . . C76 C 0.3078(12) 0.6054(10) 0.1151(5) 0.034 Uani 1 1 d . . . C77 C 0.3848(11) 0.5717(12) 0.0937(5) 0.036 Uani 1 1 d . . . C78 C 0.3631(13) 0.4851(12) 0.0689(6) 0.049 Uani 1 1 d . . . C79 C 0.4360(15) 0.4576(14) 0.0527(6) 0.055 Uani 1 1 d . . . C80 C 0.5345(14) 0.5119(15) 0.0631(7) 0.062 Uani 1 1 d . . . C81 C 0.5554(13) 0.5962(14) 0.0867(6) 0.053 Uani 1 1 d . . . C82 C 0.4856(14) 0.6263(13) 0.1026(6) 0.045 Uani 1 1 d . . . C83 C 0.2061(13) 0.5742(11) 0.0900(6) 0.046 Uani 1 1 d . . . H83 H 0.1902 0.5356 0.0612 0.055 Uiso 1 1 calc R . . C84 C 0.1283(12) 0.5972(12) 0.1054(5) 0.039 Uani 1 1 d . . . C85 C 0.0194(12) 0.5492(11) 0.0813(5) 0.041 Uani 1 1 d . . . C86 C -0.0100(15) 0.4585(13) 0.0556(6) 0.057 Uani 1 1 d . . . H86 H 0.0394 0.4282 0.0529 0.068 Uiso 1 1 calc R . . C87 C -0.1118(14) 0.4151(14) 0.0344(7) 0.063 Uani 1 1 d . . . H87 H -0.1317 0.3550 0.0172 0.075 Uiso 1 1 calc R . . C88 C -0.1833(14) 0.4578(13) 0.0382(6) 0.052 Uani 1 1 d . . . H88 H -0.2529 0.4283 0.0241 0.062 Uiso 1 1 calc R . . C89 C -0.1515(15) 0.5445(14) 0.0630(8) 0.071 Uani 1 1 d . . . H89 H -0.2006 0.5753 0.0652 0.086 Uiso 1 1 calc R . . C90 C -0.0523(13) 0.5896(13) 0.0848(7) 0.059 Uani 1 1 d . . . H90 H -0.0346 0.6492 0.1024 0.071 Uiso 1 1 calc R . . C91 C 0.0476(11) 0.4567(11) 0.2023(6) 0.037 Uani 1 1 d . . . C92 C -0.0682(11) 0.4180(12) 0.1848(6) 0.038 Uani 1 1 d . . . C93 C -0.1185(12) 0.3249(13) 0.1784(7) 0.051 Uani 1 1 d . . . C94 C -0.2211(14) 0.2896(14) 0.1647(7) 0.061 Uani 1 1 d . . . C95 C -0.2789(13) 0.3512(17) 0.1551(7) 0.068 Uani 1 1 d . . . C96 C -0.2297(14) 0.4424(14) 0.1604(7) 0.056 Uani 1 1 d U . . C97 C -0.1255(13) 0.4781(13) 0.1754(6) 0.051 Uani 1 1 d . . . C98 C 0.1056(13) 0.4130(12) 0.1812(6) 0.048 Uani 1 1 d . . . H98 H 0.0734 0.3634 0.1565 0.058 Uiso 1 1 calc R . . C99 C 0.2122(11) 0.4424(11) 0.1964(6) 0.038 Uani 1 1 d . . . C100 C 0.2734(13) 0.3951(12) 0.1715(7) 0.051 Uani 1 1 d . . . C101 C 0.2315(15) 0.3168(13) 0.1397(8) 0.065 Uani 1 1 d . . . H101 H 0.1599 0.2895 0.1322 0.078 Uiso 1 1 calc R . . C102 C 0.2903(15) 0.2763(14) 0.1181(8) 0.072 Uani 1 1 d . . . H102 H 0.2598 0.2255 0.0939 0.086 Uiso 1 1 calc R . . C103 C 0.3937(14) 0.3112(14) 0.1325(8) 0.073 Uani 1 1 d . . . H103 H 0.4349 0.2810 0.1197 0.088 Uiso 1 1 calc R . . C104 C 0.4397(14) 0.3890(12) 0.1651(7) 0.057 Uani 1 1 d . . . H104 H 0.5116 0.4133 0.1737 0.069 Uiso 1 1 calc R . . C105 C 0.3798(11) 0.4312(12) 0.1851(7) 0.046 Uani 1 1 d . . . H105 H 0.4104 0.4844 0.2079 0.055 Uiso 1 1 calc R . . C106 C 0.3652(12) 0.5353(11) 0.3651(6) 0.039 Uani 1 1 d . . . C107 C 0.4677(13) 0.5512(13) 0.3980(7) 0.047 Uani 1 1 d . . . C108 C 0.5505(16) 0.5438(13) 0.3822(7) 0.059 Uani 1 1 d . . . C109 C 0.6487(15) 0.5602(14) 0.4129(8) 0.061 Uani 1 1 d . . . C110 C 0.6539(14) 0.5834(14) 0.4584(8) 0.064 Uani 1 1 d . . . C111 C 0.5765(16) 0.5921(13) 0.4746(7) 0.060 Uani 1 1 d . . . C112 C 0.4801(14) 0.5749(13) 0.4445(6) 0.049 Uani 1 1 d . . . C113 C 0.2870(14) 0.4597(12) 0.3708(7) 0.052 Uani 1 1 d . . . H113 H 0.3011 0.4227 0.3934 0.063 Uiso 1 1 calc R . . C114 C 0.1877(12) 0.4374(11) 0.3436(5) 0.033 Uani 1 1 d . . . C115 C 0.1031(13) 0.3529(10) 0.3472(5) 0.037 Uani 1 1 d . . . C116 C 0.1154(14) 0.2944(12) 0.3798(6) 0.047 Uani 1 1 d . . . H116 H 0.1792 0.3066 0.4006 0.056 Uiso 1 1 calc R . . C117 C 0.0348(15) 0.2192(13) 0.3818(7) 0.059 Uani 1 1 d . . . H117 H 0.0434 0.1806 0.4044 0.071 Uiso 1 1 calc R . . C118 C -0.0553(17) 0.1999(13) 0.3522(7) 0.065 Uani 1 1 d . . . H118 H -0.1088 0.1459 0.3526 0.078 Uiso 1 1 calc R . . C119 C -0.0700(14) 0.2601(12) 0.3207(7) 0.050 Uani 1 1 d . . . H119 H -0.1350 0.2490 0.3011 0.060 Uiso 1 1 calc R . . C120 C 0.0083(14) 0.3338(12) 0.3182(7) 0.048 Uani 1 1 d . . . H120 H -0.0019 0.3731 0.2962 0.058 Uiso 1 1 calc R . . C121 C 0.222(2) 1.1753(17) 0.2436(9) 0.094 Uani 1 1 d . . . C122 C 0.185(3) 1.251(2) 0.2573(11) 0.037 Uani 0.50 1 d P . . H12D H 0.1616 1.2761 0.2301 0.055 Uiso 0.50 1 calc PR . . H12E H 0.2404 1.2989 0.2788 0.055 Uiso 0.50 1 calc PR . . H12F H 0.1292 1.2276 0.2724 0.055 Uiso 0.50 1 calc PR . . C123 C 0.330(2) 1.196(2) 0.2382(11) 0.034 Uani 0.50 1 d PU . . H12A H 0.3752 1.2405 0.2646 0.052 Uiso 0.50 1 calc PR . . H12B H 0.3359 1.2224 0.2099 0.052 Uiso 0.50 1 calc PR . . H12C H 0.3485 1.1391 0.2366 0.052 Uiso 0.50 1 calc PR . . C124 C 0.059(3) 0.260(3) 0.0039(15) 0.069 Uiso 0.50 1 d P . . H12G H 0.1058 0.3184 0.0221 0.103 Uiso 0.50 1 calc PR . . H12H H 0.0104 0.2309 0.0214 0.103 Uiso 0.50 1 calc PR . . H12I H 0.0232 0.2732 -0.0248 0.103 Uiso 0.50 1 calc PR . . C125 C 0.111(2) 0.2053(19) -0.0056(10) 0.059 Uiso 0.50 1 d PG . . C126 C 0.088(2) 0.120(2) 0.0096(11) 0.103 Uiso 0.50 1 d PG . . H126 H 0.0332 0.1022 0.0245 0.123 Uiso 0.50 1 calc PR . . C127 C 0.145(3) 0.0614(17) 0.0032(12) 0.093 Uiso 0.50 1 d PG . . H127 H 0.1295 0.0032 0.0136 0.112 Uiso 0.50 1 calc PR . . C128 C 0.226(2) 0.0877(19) -0.0185(12) 0.101 Uiso 0.50 1 d PG . . H128 H 0.2648 0.0475 -0.0229 0.122 Uiso 0.50 1 calc PR . . C129 C 0.2489(19) 0.173(2) -0.0337(10) 0.064 Uiso 0.50 1 d PG . . H129 H 0.3038 0.1908 -0.0485 0.077 Uiso 0.50 1 calc PR . . C130 C 0.192(2) 0.2316(16) -0.0273(10) 0.069 Uiso 0.50 1 d PG . . H130 H 0.2076 0.2898 -0.0377 0.083 Uiso 0.50 1 calc PR . . 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 Er1 0.026 0.030 0.026 0.003 0.004 0.008 Er2 0.025 0.039 0.027 0.005 0.002 0.008 Er3 0.025 0.030 0.025 0.002 0.003 0.011 Er4 0.027 0.030 0.039 0.010 0.006 0.012 F1 0.059 0.052 0.076 0.019 -0.023 0.006 F2 0.075 0.054 0.126 0.027 0.014 0.007 F3 0.070 0.059 0.106 0.003 0.002 -0.017 F4 0.061 0.073 0.112 0.009 -0.024 0.002 F5 0.072 0.060 0.052 0.010 -0.008 0.017 F6 0.027 0.041 0.039 0.012 -0.004 -0.004 F7 0.040 0.063 0.043 0.013 -0.005 0.015 F8 0.052 0.070 0.042 0.027 0.013 0.027 F9 0.040 0.062 0.054 0.026 0.012 0.012 F10 0.038 0.038 0.050 0.008 -0.002 0.003 F11 0.062 0.089 0.108 0.016 0.001 0.011 F12 0.071 0.193 0.183 0.060 -0.010 0.038 F13 0.150 0.172 0.101 0.019 -0.015 0.099 F14 0.178 0.095 0.059 0.031 0.033 0.082 F15 0.107 0.110 0.040 0.009 0.020 0.022 F16 0.061 0.050 0.056 0.018 0.020 0.033 F17 0.046 0.068 0.104 0.038 0.027 0.031 F18 0.067 0.108 0.070 0.054 0.025 0.036 F19 0.082 0.098 0.056 0.029 0.042 0.034 F20 0.041 0.061 0.055 0.011 0.022 0.024 F21 0.056 0.058 0.109 0.036 0.043 0.035 F22 0.053 0.078 0.114 0.042 0.039 0.035 F23 0.045 0.073 0.131 0.032 0.027 0.045 F24 0.082 0.073 0.498 0.123 0.131 0.056 F25 0.089 0.082 0.319 0.087 0.086 0.060 F26 0.051 0.068 0.092 -0.020 0.014 0.015 F27 0.073 0.096 0.103 -0.031 0.003 0.045 F28 0.046 0.151 0.075 -0.024 0.008 0.044 F29 0.043 0.113 0.071 0.002 0.019 0.023 F30 0.038 0.048 0.067 -0.004 -0.003 0.012 F31 0.039 0.057 0.100 0.000 0.009 0.010 F32 0.030 0.089 0.112 -0.035 0.019 -0.007 F33 0.028 0.160 0.114 -0.064 -0.001 0.034 F34 0.056 0.139 0.091 -0.042 -0.013 0.062 F35 0.057 0.060 0.076 0.002 -0.003 0.043 F36 0.057 0.094 0.091 0.028 0.027 0.047 F37 0.061 0.119 0.139 0.035 0.035 0.050 F38 0.037 0.106 0.142 0.055 0.000 0.020 F39 0.061 0.088 0.065 0.030 0.004 0.014 F40 0.051 0.092 0.061 0.018 0.013 0.026 O1 0.035 0.044 0.023 0.004 0.000 0.015 O2 0.021 0.010 0.029 0.002 0.005 0.013 O3 0.021 0.047 0.039 0.017 0.012 0.014 O4 0.036 0.023 0.038 0.009 -0.001 0.016 O5 0.052 0.044 0.031 0.001 0.006 0.010 O6 0.033 0.046 0.032 -0.005 -0.001 0.012 O7 0.015 0.046 0.038 0.005 0.011 0.019 O8 0.056 0.040 0.023 0.006 -0.003 0.020 O9 0.048 0.066 0.045 0.016 0.016 0.016 O10 0.033 0.043 0.054 -0.004 -0.004 0.009 O11 0.019 0.031 0.049 0.003 0.006 0.010 O12 0.033 0.033 0.046 0.006 0.007 0.018 O13 0.028 0.049 0.032 -0.001 0.000 0.024 O14 0.024 0.040 0.043 0.015 0.014 0.014 O15 0.028 0.053 0.023 0.003 -0.008 0.020 O16 0.041 0.044 0.030 -0.003 -0.003 0.022 O17 0.031 0.035 0.053 0.014 0.015 0.015 O18 0.025 0.042 0.060 0.005 0.006 0.020 O19 0.040 0.055 0.055 0.017 -0.006 0.025 O20 0.056 0.039 0.057 0.018 0.008 0.017 O21 0.036 0.041 0.035 0.009 0.014 0.020 O22 0.045 0.064 0.068 0.028 0.002 0.020 O23 0.114 0.056 0.163 0.030 0.014 0.021 C1 0.035 0.032 0.029 0.000 0.001 0.015 C2 0.043 0.037 0.051 -0.006 0.023 0.004 C3 0.045 0.037 0.052 0.001 0.007 0.007 C4 0.067 0.034 0.079 0.016 0.021 0.015 C5 0.062 0.043 0.085 0.016 -0.006 -0.002 C6 0.043 0.061 0.066 0.010 -0.002 0.009 C7 0.044 0.036 0.058 0.003 -0.013 0.010 C8 0.034 0.041 0.037 0.008 0.000 0.016 C9 0.023 0.033 0.035 0.006 0.015 0.012 C10 0.041 0.043 0.035 0.004 0.016 0.019 C11 0.104 0.046 0.034 0.013 0.027 0.009 C12 0.099 0.059 0.047 0.016 0.016 0.025 C13 0.107 0.058 0.039 0.001 0.024 0.011 C14 0.060 0.071 0.068 -0.007 0.033 -0.010 C15 0.042 0.066 0.044 0.012 0.017 0.014 C16 0.033 0.031 0.034 0.011 0.004 0.012 C17 0.029 0.037 0.029 -0.003 0.006 0.013 C18 0.050 0.037 0.042 0.009 0.010 0.018 C19 0.042 0.038 0.026 0.004 0.000 0.014 C20 0.076 0.050 0.031 0.015 0.021 0.018 C21 0.038 0.043 0.037 0.014 0.010 0.000 C22 0.034 0.041 0.033 0.008 0.002 0.013 C23 0.029 0.057 0.030 0.003 0.002 0.016 C24 0.027 0.028 0.033 0.000 -0.003 -0.006 C25 0.033 0.036 0.035 -0.002 -0.003 0.008 C26 0.030 0.040 0.035 0.004 0.006 0.002 C27 0.030 0.045 0.053 0.003 0.002 0.024 C28 0.033 0.054 0.055 0.004 0.001 0.012 C29 0.042 0.060 0.063 0.027 0.011 0.012 C30 0.031 0.065 0.063 0.022 -0.012 0.005 C31 0.039 0.043 0.031 -0.017 -0.011 0.006 C32 0.046 0.057 0.046 0.002 0.013 0.006 C33 0.054 0.079 0.065 0.036 0.023 0.031 C34 0.095 0.072 0.085 0.003 -0.004 0.040 C35 0.146 0.122 0.042 0.022 -0.020 0.075 C36 0.091 0.092 0.064 -0.003 -0.001 0.055 C37 0.051 0.059 0.076 -0.002 0.031 0.015 C38 0.046 0.044 0.064 -0.006 0.009 0.020 C39 0.026 0.054 0.056 0.004 0.009 0.003 C40 0.074 0.051 0.140 0.020 0.004 0.003 C41 0.074 0.051 0.140 0.020 0.004 0.003 C42 0.074 0.051 0.140 0.020 0.004 0.003 C43 0.074 0.051 0.140 0.020 0.004 0.003 C44 0.074 0.051 0.140 0.020 0.004 0.003 C45 0.074 0.051 0.140 0.020 0.004 0.003 C46 0.018 0.032 0.031 0.007 0.010 0.005 C47 0.034 0.031 0.036 0.005 0.016 0.008 C48 0.028 0.050 0.052 0.012 0.016 0.015 C49 0.035 0.055 0.055 0.015 0.013 0.019 C50 0.051 0.063 0.055 0.030 0.026 0.016 C51 0.043 0.070 0.042 0.021 0.019 0.020 C52 0.035 0.045 0.041 0.008 0.010 0.011 C53 0.030 0.048 0.049 0.012 0.023 0.014 C54 0.023 0.030 0.047 0.005 0.009 0.012 C55 0.044 0.044 0.049 0.000 0.008 0.022 C56 0.038 0.077 0.056 -0.004 0.015 0.005 C57 0.034 0.066 0.077 0.012 0.008 0.002 C58 0.031 0.062 0.090 -0.017 0.014 0.006 C59 0.053 0.137 0.095 0.038 0.019 0.041 C60 0.037 0.149 0.099 0.065 -0.007 0.035 C61 0.028 0.047 0.042 0.016 -0.002 0.020 C62 0.041 0.029 0.054 0.013 0.008 0.015 C63 0.034 0.049 0.065 0.017 0.009 0.016 C64 0.032 0.056 0.063 0.019 0.010 0.024 C65 0.029 0.061 0.084 0.024 0.016 0.016 C66 0.071 0.046 0.173 0.021 0.029 0.031 C67 0.025 0.076 0.193 0.061 0.052 0.030 C68 0.055 0.065 0.036 0.012 0.011 0.024 C69 0.041 0.041 0.035 0.013 0.010 0.016 C70 0.054 0.058 0.027 0.009 0.018 0.018 C71 0.052 0.050 0.040 0.008 0.005 0.016 C72 0.063 0.055 0.059 0.009 0.022 0.016 C73 0.087 0.077 0.025 0.013 0.017 0.023 C74 0.069 0.083 0.034 0.015 0.015 0.037 C75 0.093 0.073 0.024 0.011 0.005 0.057 C76 0.040 0.030 0.041 0.002 0.008 0.025 C77 0.025 0.059 0.021 -0.007 -0.002 0.016 C78 0.029 0.053 0.056 -0.004 -0.002 0.008 C79 0.061 0.070 0.038 -0.012 -0.008 0.044 C80 0.044 0.093 0.049 -0.016 0.000 0.040 C81 0.032 0.076 0.044 0.002 -0.011 0.019 C82 0.049 0.059 0.033 0.000 0.001 0.030 C83 0.052 0.040 0.041 -0.003 0.006 0.016 C84 0.031 0.054 0.031 0.005 0.002 0.018 C85 0.040 0.044 0.028 -0.006 -0.013 0.014 C86 0.059 0.053 0.051 -0.010 0.003 0.016 C87 0.045 0.056 0.062 -0.022 0.000 -0.008 C88 0.036 0.054 0.056 -0.009 0.008 0.005 C89 0.044 0.063 0.096 -0.016 -0.015 0.029 C90 0.037 0.054 0.071 -0.020 -0.010 0.014 C91 0.020 0.034 0.051 0.000 -0.002 0.007 C92 0.017 0.053 0.041 -0.009 0.008 0.010 C93 0.026 0.063 0.062 -0.007 -0.007 0.028 C94 0.036 0.060 0.077 -0.028 0.026 0.001 C95 0.027 0.108 0.059 -0.032 0.000 0.025 C96 0.038 0.068 0.065 -0.007 0.008 0.032 C97 0.040 0.060 0.050 -0.019 0.007 0.020 C98 0.032 0.047 0.059 -0.003 0.005 0.009 C99 0.015 0.050 0.059 0.015 0.009 0.023 C100 0.034 0.036 0.078 0.005 0.013 0.005 C101 0.037 0.046 0.115 0.005 0.022 0.018 C102 0.045 0.056 0.098 -0.030 -0.001 0.014 C103 0.040 0.056 0.125 -0.022 0.024 0.026 C104 0.038 0.044 0.094 0.007 0.017 0.018 C105 0.018 0.048 0.069 -0.003 0.012 0.008 C106 0.036 0.036 0.053 0.016 0.009 0.024 C107 0.027 0.060 0.066 0.036 0.023 0.014 C108 0.073 0.055 0.059 0.027 0.023 0.026 C109 0.052 0.062 0.076 0.017 0.007 0.031 C110 0.041 0.070 0.089 0.033 0.002 0.031 C111 0.061 0.053 0.056 0.011 -0.002 0.012 C112 0.045 0.065 0.043 0.026 0.001 0.025 C113 0.064 0.039 0.064 0.025 0.012 0.028 C114 0.042 0.037 0.034 0.016 0.015 0.024 C115 0.056 0.027 0.032 0.007 0.016 0.017 C116 0.051 0.052 0.050 0.017 0.016 0.028 C117 0.064 0.051 0.059 0.019 0.016 0.007 C118 0.076 0.043 0.067 0.003 0.035 -0.009 C119 0.045 0.044 0.066 0.018 0.020 0.015 C120 0.051 0.040 0.057 0.011 0.018 0.013 C121 0.151 0.070 0.082 0.016 0.058 0.048 C122 0.051 0.037 0.049 0.021 0.045 0.029 C123 0.032 0.039 0.038 0.000 0.018 0.014 _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 Er1 O6 2.271(11) . ? Er1 O4 2.313(10) . ? Er1 O5 2.314(11) . ? Er1 O1 2.350(10) . ? Er1 O21 2.359(10) . ? Er1 O8 2.371(11) . ? Er1 O2 2.379(9) . ? Er1 O7 2.430(10) . ? Er1 Er4 3.4625(12) . ? Er1 Er2 3.8445(13) . ? Er1 Er3 3.8611(13) . ? Er2 O9 2.236(12) . ? Er2 O12 2.298(10) . ? Er2 O3 2.305(11) . ? Er2 O2 2.315(8) . ? Er2 O1 2.331(11) . ? Er2 O10 2.334(11) . ? Er2 O22 2.425(12) . ? Er2 O11 2.443(11) . ? Er2 Er3 3.5028(17) . ? Er2 Er4 3.8635(18) . ? Er3 O16 2.270(10) . ? Er3 O14 2.286(10) . ? Er3 O4 2.298(10) . ? Er3 O15 2.319(10) . ? Er3 O3 2.335(10) . ? Er3 O2 2.348(8) . ? Er3 O13 2.367(10) . ? Er3 O11 2.486(10) . ? Er3 Er4 3.8089(15) . ? Er4 O18 2.235(11) . ? Er4 O17 2.291(11) . ? Er4 O20 2.292(11) . ? Er4 O7 2.319(9) . ? Er4 O19 2.339(11) . ? Er4 O3 2.353(10) . ? Er4 O4 2.374(9) . ? Er4 O1 2.418(10) . ? F1 C3 1.33(2) . ? F2 C4 1.35(2) . ? F3 C5 1.35(2) . ? F4 C6 1.35(2) . ? F5 C7 1.316(19) . ? F6 C18 1.332(19) . ? F7 C19 1.318(17) . ? F8 C20 1.318(18) . ? F9 C21 1.350(18) . ? F10 C22 1.360(17) . ? F11 C33 1.35(2) . ? F12 C34 1.39(3) . ? F13 C35 1.37(3) . ? F14 C36 1.34(3) . ? F15 C37 1.32(2) . ? F16 C48 1.342(18) . ? F17 C49 1.330(19) . ? F18 C50 1.35(2) . ? F19 C51 1.328(19) . ? F20 C52 1.331(18) . ? F21 C63 1.34(2) . ? F22 C64 1.35(2) . ? F23 C65 1.34(2) . ? F24 C66 1.36(2) . ? F25 C67 1.40(2) . ? F26 C78 1.352(19) . ? F27 C79 1.38(2) . ? F28 C80 1.32(2) . ? F29 C81 1.35(2) . ? F30 C82 1.305(19) . ? F31 C93 1.321(19) . ? F32 C94 1.35(2) . ? F33 C95 1.32(2) . ? F34 C96 1.35(2) . ? F35 C97 1.32(2) . ? F36 C108 1.36(2) . ? F37 C109 1.33(2) . ? F38 C110 1.37(2) . ? F39 C111 1.34(2) . ? F40 C112 1.30(2) . ? O1 H1 1.0000 . ? O2 H2 1.0000 . ? O3 H3 1.0000 . ? O4 H4 1.0000 . ? O5 C1 1.266(17) . ? O6 C9 1.256(17) . ? O7 C16 1.312(18) . ? O8 C24 1.252(17) . ? O9 C31 1.317(19) . ? O10 C39 1.251(19) . ? O11 C46 1.269(16) . ? O12 C54 1.249(18) . ? O13 C61 1.269(18) . ? O14 C69 1.258(18) . ? O15 C76 1.242(17) . ? O16 C84 1.256(18) . ? O17 C91 1.257(18) . ? O18 C99 1.289(19) . ? O19 C106 1.270(19) . ? O20 C114 1.262(17) . ? O23 C121 1.25(3) . ? C1 C8 1.37(2) . ? C1 C2 1.51(2) . ? C2 C3 1.36(2) . ? C2 C7 1.40(2) . ? C3 C4 1.40(2) . ? C4 C5 1.38(3) . ? C5 C6 1.34(3) . ? C6 C7 1.38(2) . ? C8 C9 1.41(2) . ? C8 H8 0.9500 . ? C9 C10 1.49(2) . ? C10 C15 1.34(2) . ? C10 C11 1.39(2) . ? C11 C12 1.37(3) . ? C11 H11 0.9500 . ? C12 C13 1.34(3) . ? C12 H12 0.9500 . ? C13 C14 1.39(3) . ? C13 H13 0.9500 . ? C14 C15 1.40(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C23 1.40(2) . ? C16 C17 1.53(2) . ? C17 C22 1.38(2) . ? C17 C18 1.39(2) . ? C18 C19 1.39(2) . ? C19 C20 1.38(2) . ? C20 C21 1.37(2) . ? C21 C22 1.36(2) . ? C23 C24 1.41(2) . ? C23 H23 0.9500 . ? C24 C25 1.51(2) . ? C25 C30 1.38(2) . ? C25 C26 1.39(2) . ? C26 C27 1.37(2) . ? C26 H26 0.9500 . ? C27 C28 1.36(2) . ? C27 H27 0.9500 . ? C28 C29 1.36(2) . ? C28 H28 0.9500 . ? C29 C30 1.39(2) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C38 1.35(2) . ? C31 C32 1.53(2) . ? C32 C37 1.31(3) . ? C32 C33 1.39(3) . ? C33 C34 1.31(3) . ? C34 C35 1.41(4) . ? C35 C36 1.27(4) . ? C36 C37 1.43(3) . ? C38 C39 1.43(3) . ? C38 H38 0.9500 . ? C39 C40 1.45(3) . ? C40 C41 1.33(4) . ? C40 C45 1.40(3) . ? C41 C42 1.48(3) . ? C41 H41 0.9500 . ? C42 C43 1.36(3) . ? C42 H42 0.9500 . ? C43 C44 1.39(4) . ? C43 H43 0.9500 . ? C44 C45 1.34(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C53 1.38(2) . ? C46 C47 1.52(2) . ? C47 C48 1.35(2) . ? C47 C52 1.41(2) . ? C48 C49 1.41(2) . ? C49 C50 1.35(2) . ? C50 C51 1.33(3) . ? C51 C52 1.38(2) . ? C53 C54 1.41(2) . ? C53 H53 0.9500 . ? C54 C55 1.491(16) . ? C55 C56 1.3900 . ? C55 C60 1.3900 . ? C56 C57 1.3900 . ? C56 H56 0.9500 . ? C57 C58 1.3900 . ? C57 H57 0.9500 . ? C58 C59 1.3900 . ? C58 H58 0.9500 . ? C59 C60 1.3900 . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C68 1.37(2) . ? C61 C62 1.53(2) . ? C62 C63 1.31(2) . ? C62 C67 1.35(3) . ? C63 C64 1.41(2) . ? C64 C65 1.35(2) . ? C65 C66 1.28(3) . ? C66 C67 1.42(3) . ? C68 C69 1.44(2) . ? C68 H68 0.9500 . ? C69 C70 1.48(2) . ? C70 C75 1.38(2) . ? C70 C71 1.38(2) . ? C71 C72 1.40(2) . ? C71 H71 0.9500 . ? C72 C73 1.41(3) . ? C72 H72 0.9500 . ? C73 C74 1.38(3) . ? C73 H73 0.9500 . ? C74 C75 1.35(2) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C83 1.41(2) . ? C76 C77 1.54(2) . ? C77 C78 1.38(2) . ? C77 C82 1.39(2) . ? C78 C79 1.37(2) . ? C79 C80 1.36(3) . ? C80 C81 1.34(3) . ? C81 C82 1.34(2) . ? C83 C84 1.39(2) . ? C83 H83 0.9500 . ? C84 C85 1.51(2) . ? C85 C90 1.34(2) . ? C85 C86 1.43(2) . ? C86 C87 1.39(2) . ? C86 H86 0.9500 . ? C87 C88 1.36(3) . ? C87 H87 0.9500 . ? C88 C89 1.37(2) . ? C88 H88 0.9500 . ? C89 C90 1.37(2) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C91 C98 1.39(2) . ? C91 C92 1.54(2) . ? C92 C93 1.37(2) . ? C92 C97 1.40(2) . ? C93 C94 1.36(2) . ? C94 C95 1.42(3) . ? C95 C96 1.35(3) . ? C96 C97 1.38(2) . ? C98 C99 1.41(2) . ? C98 H98 0.9500 . ? C99 C100 1.52(2) . ? C100 C101 1.36(3) . ? C100 C105 1.41(2) . ? C101 C102 1.38(3) . ? C101 H101 0.9500 . ? C102 C103 1.37(3) . ? C102 H102 0.9500 . ? C103 C104 1.38(3) . ? C103 H103 0.9500 . ? C104 C105 1.38(2) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 C113 1.40(2) . ? C106 C107 1.53(2) . ? C107 C108 1.37(3) . ? C107 C112 1.37(3) . ? C108 C109 1.45(3) . ? C109 C110 1.36(3) . ? C110 C111 1.31(3) . ? C111 C112 1.42(3) . ? C113 C114 1.41(2) . ? C113 H113 0.9500 . ? C114 C115 1.52(2) . ? C115 C120 1.39(2) . ? C115 C116 1.40(2) . ? C116 C117 1.38(2) . ? C116 H116 0.9500 . ? C117 C118 1.34(3) . ? C117 H117 0.9500 . ? C118 C119 1.41(3) . ? C118 H118 0.9500 . ? C119 C120 1.35(2) . ? C119 H119 0.9500 . ? C120 H120 0.9500 . ? C121 C122 1.45(3) . ? C121 C123 1.50(4) . ? C122 H12D 0.9800 . ? C122 H12E 0.9800 . ? C122 H12F 0.9800 . ? C123 H12A 0.9800 . ? C123 H12B 0.9800 . ? C123 H12C 0.9800 . ? C124 C125 1.31(4) . ? C124 H12G 0.9800 . ? C124 H12H 0.9800 . ? C124 H12I 0.9800 . ? C125 C126 1.3900 . ? C125 C130 1.3900 . ? C126 C127 1.3900 . ? C126 H126 0.9500 . ? C127 C128 1.3900 . ? C127 H127 0.9500 . ? C128 C129 1.3900 . ? C128 H128 0.9500 . ? C129 C130 1.3900 . ? C129 H129 0.9500 . ? C130 H130 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Er1 O4 143.1(4) . . ? O6 Er1 O5 72.4(4) . . ? O4 Er1 O5 142.8(4) . . ? O6 Er1 O1 99.2(4) . . ? O4 Er1 O1 78.1(3) . . ? O5 Er1 O1 86.4(4) . . ? O6 Er1 O21 109.4(4) . . ? O4 Er1 O21 91.4(3) . . ? O5 Er1 O21 81.2(4) . . ? O1 Er1 O21 143.4(4) . . ? O6 Er1 O8 79.6(4) . . ? O4 Er1 O8 77.5(4) . . ? O5 Er1 O8 133.1(4) . . ? O1 Er1 O8 135.5(4) . . ? O21 Er1 O8 73.6(4) . . ? O6 Er1 O2 146.4(3) . . ? O4 Er1 O2 67.2(3) . . ? O5 Er1 O2 75.7(3) . . ? O1 Er1 O2 68.2(3) . . ? O21 Er1 O2 75.3(3) . . ? O8 Er1 O2 131.7(3) . . ? O6 Er1 O7 72.7(4) . . ? O4 Er1 O7 72.7(3) . . ? O5 Er1 O7 130.6(4) . . ? O1 Er1 O7 65.9(3) . . ? O21 Er1 O7 144.0(3) . . ? O8 Er1 O7 71.4(3) . . ? O2 Er1 O7 123.6(3) . . ? O6 Er1 Er4 111.3(3) . . ? O4 Er1 Er4 43.1(2) . . ? O5 Er1 Er4 130.6(3) . . ? O1 Er1 Er4 44.2(2) . . ? O21 Er1 Er4 134.3(2) . . ? O8 Er1 Er4 94.2(3) . . ? O2 Er1 Er4 82.02(19) . . ? O7 Er1 Er4 41.9(2) . . ? O6 Er1 Er2 123.0(3) . . ? O4 Er1 Er2 74.6(3) . . ? O5 Er1 Er2 73.5(3) . . ? O1 Er1 Er2 34.6(3) . . ? O21 Er1 Er2 108.8(2) . . ? O8 Er1 Er2 152.1(3) . . ? O2 Er1 Er2 34.5(2) . . ? O7 Er1 Er2 98.0(2) . . ? Er4 Er1 Er2 63.59(3) . . ? O6 Er1 Er3 173.6(3) . . ? O4 Er1 Er3 33.0(3) . . ? O5 Er1 Er3 110.4(3) . . ? O1 Er1 Er3 75.4(2) . . ? O21 Er1 Er3 76.9(2) . . ? O8 Er1 Er3 101.6(3) . . ? O2 Er1 Er3 35.0(2) . . ? O7 Er1 Er3 101.5(2) . . ? Er4 Er1 Er3 62.40(3) . . ? Er2 Er1 Er3 54.08(3) . . ? O9 Er2 O12 84.4(4) . . ? O9 Er2 O3 140.2(4) . . ? O12 Er2 O3 108.4(4) . . ? O9 Er2 O2 121.9(4) . . ? O12 Er2 O2 136.2(3) . . ? O3 Er2 O2 74.8(3) . . ? O9 Er2 O1 82.4(4) . . ? O12 Er2 O1 153.8(4) . . ? O3 Er2 O1 69.8(3) . . ? O2 Er2 O1 69.6(3) . . ? O9 Er2 O10 73.6(4) . . ? O12 Er2 O10 79.1(4) . . ? O3 Er2 O10 144.8(4) . . ? O2 Er2 O10 76.6(3) . . ? O1 Er2 O10 118.0(4) . . ? O9 Er2 O22 74.9(5) . . ? O12 Er2 O22 69.5(4) . . ? O3 Er2 O22 74.9(4) . . ? O2 Er2 O22 145.9(4) . . ? O1 Er2 O22 85.3(4) . . ? O10 Er2 O22 137.1(4) . . ? O9 Er2 O11 146.1(4) . . ? O12 Er2 O11 71.6(3) . . ? O3 Er2 O11 71.9(3) . . ? O2 Er2 O11 68.2(3) . . ? O1 Er2 O11 128.6(3) . . ? O10 Er2 O11 78.7(4) . . ? O22 Er2 O11 116.0(4) . . ? O9 Er2 Er3 162.0(3) . . ? O12 Er2 Er3 112.9(3) . . ? O3 Er2 Er3 41.3(2) . . ? O2 Er2 Er3 41.7(2) . . ? O1 Er2 Er3 83.6(2) . . ? O10 Er2 Er3 103.6(3) . . ? O22 Er2 Er3 115.0(3) . . ? O11 Er2 Er3 45.2(2) . . ? O9 Er2 Er1 99.0(3) . . ? O12 Er2 Er1 171.2(3) . . ? O3 Er2 Er1 74.2(2) . . ? O2 Er2 Er1 35.6(2) . . ? O1 Er2 Er1 34.9(2) . . ? O10 Er2 Er1 93.9(3) . . ? O22 Er2 Er1 119.2(3) . . ? O11 Er2 Er1 101.9(2) . . ? Er3 Er2 Er1 63.20(3) . . ? O9 Er2 Er4 110.5(3) . . ? O12 Er2 Er4 133.1(2) . . ? O3 Er2 Er4 34.4(2) . . ? O2 Er2 Er4 74.0(2) . . ? O1 Er2 Er4 36.3(2) . . ? O10 Er2 Er4 147.2(3) . . ? O22 Er2 Er4 72.1(3) . . ? O11 Er2 Er4 103.3(2) . . ? Er3 Er2 Er4 62.04(4) . . ? Er1 Er2 Er4 53.39(3) . . ? O16 Er3 O14 81.5(4) . . ? O16 Er3 O4 73.7(4) . . ? O14 Er3 O4 148.1(3) . . ? O16 Er3 O15 74.3(4) . . ? O14 Er3 O15 75.0(4) . . ? O4 Er3 O15 115.7(4) . . ? O16 Er3 O3 110.8(4) . . ? O14 Er3 O3 139.2(3) . . ? O4 Er3 O3 70.1(3) . . ? O15 Er3 O3 71.8(3) . . ? O16 Er3 O2 136.9(3) . . ? O14 Er3 O2 124.2(3) . . ? O4 Er3 O2 67.9(3) . . ? O15 Er3 O2 140.6(3) . . ? O3 Er3 O2 73.7(3) . . ? O16 Er3 O13 80.0(4) . . ? O14 Er3 O13 72.6(4) . . ? O4 Er3 O13 83.5(3) . . ? O15 Er3 O13 141.0(3) . . ? O3 Er3 O13 146.2(4) . . ? O2 Er3 O13 77.1(3) . . ? O16 Er3 O11 156.1(4) . . ? O14 Er3 O11 83.2(4) . . ? O4 Er3 O11 126.3(4) . . ? O15 Er3 O11 84.0(3) . . ? O3 Er3 O11 70.6(3) . . ? O2 Er3 O11 67.0(3) . . ? O13 Er3 O11 112.6(3) . . ? O16 Er3 Er2 149.0(3) . . ? O14 Er3 Er2 127.1(3) . . ? O4 Er3 Er2 82.4(2) . . ? O15 Er3 Er2 99.6(2) . . ? O3 Er3 Er2 40.7(3) . . ? O2 Er3 Er2 41.0(2) . . ? O13 Er3 Er2 117.1(2) . . ? O11 Er3 Er2 44.2(3) . . ? O16 Er3 Er4 85.5(3) . . ? O14 Er3 Er4 160.6(3) . . ? O4 Er3 Er4 36.1(2) . . ? O15 Er3 Er4 87.6(3) . . ? O3 Er3 Er4 35.8(2) . . ? O2 Er3 Er4 74.9(2) . . ? O13 Er3 Er4 119.3(3) . . ? O11 Er3 Er4 103.9(2) . . ? Er2 Er3 Er4 63.63(3) . . ? O16 Er3 Er1 102.7(3) . . ? O14 Er3 Er1 143.7(2) . . ? O4 Er3 Er1 33.3(2) . . ? O15 Er3 Er1 141.1(3) . . ? O3 Er3 Er1 73.6(3) . . ? O2 Er3 Er1 35.5(2) . . ? O13 Er3 Er1 72.8(2) . . ? O11 Er3 Er1 100.6(2) . . ? Er2 Er3 Er1 62.72(3) . . ? Er4 Er3 Er1 53.67(2) . . ? O18 Er4 O17 74.6(4) . . ? O18 Er4 O20 85.6(4) . . ? O17 Er4 O20 71.4(4) . . ? O18 Er4 O7 154.3(4) . . ? O17 Er4 O7 81.2(4) . . ? O20 Er4 O7 78.6(4) . . ? O18 Er4 O19 86.8(4) . . ? O17 Er4 O19 140.3(4) . . ? O20 Er4 O19 72.4(4) . . ? O7 Er4 O19 107.1(4) . . ? O18 Er4 O3 74.7(4) . . ? O17 Er4 O3 118.7(4) . . ? O20 Er4 O3 153.3(4) . . ? O7 Er4 O3 125.9(4) . . ? O19 Er4 O3 88.3(4) . . ? O18 Er4 O4 105.6(4) . . ? O17 Er4 O4 70.8(4) . . ? O20 Er4 O4 135.7(4) . . ? O7 Er4 O4 73.6(4) . . ? O19 Er4 O4 148.9(4) . . ? O3 Er4 O4 68.5(3) . . ? O18 Er4 O1 138.9(4) . . ? O17 Er4 O1 138.6(3) . . ? O20 Er4 O1 122.9(4) . . ? O7 Er4 O1 66.6(3) . . ? O19 Er4 O1 76.5(4) . . ? O3 Er4 O1 67.6(4) . . ? O4 Er4 O1 75.6(3) . . ? O18 Er4 Er1 146.0(3) . . ? O17 Er4 Er1 96.1(3) . . ? O20 Er4 Er1 123.0(3) . . ? O7 Er4 Er1 44.5(3) . . ? O19 Er4 Er1 117.3(3) . . ? O3 Er4 Er1 82.0(3) . . ? O4 Er4 Er1 41.7(2) . . ? O1 Er4 Er1 42.7(2) . . ? O18 Er4 Er3 83.1(3) . . ? O17 Er4 Er3 89.2(3) . . ? O20 Er4 Er3 159.6(3) . . ? O7 Er4 Er3 105.4(3) . . ? O19 Er4 Er3 123.6(3) . . ? O3 Er4 Er3 35.5(2) . . ? O4 Er4 Er3 34.7(3) . . ? O1 Er4 Er3 75.9(2) . . ? Er1 Er4 Er3 63.94(3) . . ? O18 Er4 Er2 104.9(3) . . ? O17 Er4 Er2 142.7(3) . . ? O20 Er4 Er2 145.7(3) . . ? O7 Er4 Er2 99.6(3) . . ? O19 Er4 Er2 75.6(3) . . ? O3 Er4 Er2 33.6(3) . . ? O4 Er4 Er2 73.7(2) . . ? O1 Er4 Er2 34.8(2) . . ? Er1 Er4 Er2 63.03(3) . . ? Er3 Er4 Er2 54.32(3) . . ? Er2 O1 Er1 110.5(4) . . ? Er2 O1 Er4 108.9(4) . . ? Er1 O1 Er4 93.1(3) . . ? Er2 O1 H1 114.2 . . ? Er1 O1 H1 114.2 . . ? Er4 O1 H1 114.2 . . ? Er2 O2 Er3 97.4(3) . . ? Er2 O2 Er1 109.9(4) . . ? Er3 O2 Er1 109.5(3) . . ? Er2 O2 H2 113.0 . . ? Er3 O2 H2 113.0 . . ? Er1 O2 H2 113.0 . . ? Er2 O3 Er3 98.0(4) . . ? Er2 O3 Er4 112.1(4) . . ? Er3 O3 Er4 108.7(4) . . ? Er2 O3 H3 112.4 . . ? Er3 O3 H3 112.4 . . ? Er4 O3 H3 112.4 . . ? Er3 O4 Er1 113.7(4) . . ? Er3 O4 Er4 109.2(4) . . ? Er1 O4 Er4 95.2(4) . . ? Er3 O4 H4 112.5 . . ? Er1 O4 H4 112.5 . . ? Er4 O4 H4 112.5 . . ? C1 O5 Er1 132.3(10) . . ? C9 O6 Er1 135.1(9) . . ? C16 O7 Er4 138.5(9) . . ? C16 O7 Er1 124.1(8) . . ? Er4 O7 Er1 93.6(3) . . ? C24 O8 Er1 133.9(10) . . ? C31 O9 Er2 127.3(11) . . ? C39 O10 Er2 134.4(12) . . ? C46 O11 Er2 126.6(9) . . ? C46 O11 Er3 141.3(9) . . ? Er2 O11 Er3 90.6(3) . . ? C54 O12 Er2 135.0(9) . . ? C61 O13 Er3 131.2(10) . . ? C69 O14 Er3 138.7(10) . . ? C76 O15 Er3 128.8(9) . . ? C84 O16 Er3 133.6(10) . . ? C91 O17 Er4 133.6(9) . . ? C99 O18 Er4 137.4(9) . . ? C106 O19 Er4 134.1(11) . . ? C114 O20 Er4 140.2(11) . . ? O5 C1 C8 126.7(15) . . ? O5 C1 C2 115.8(14) . . ? C8 C1 C2 117.5(14) . . ? C3 C2 C7 117.2(16) . . ? C3 C2 C1 119.1(16) . . ? C7 C2 C1 123.6(16) . . ? F1 C3 C2 121.5(15) . . ? F1 C3 C4 116.6(16) . . ? C2 C3 C4 121.8(17) . . ? F2 C4 C5 119.4(17) . . ? F2 C4 C3 121.5(19) . . ? C5 C4 C3 119.1(18) . . ? C6 C5 F3 121.4(19) . . ? C6 C5 C4 120.0(18) . . ? F3 C5 C4 118.6(18) . . ? C5 C6 F4 120.3(18) . . ? C5 C6 C7 121.2(18) . . ? F4 C6 C7 118.5(18) . . ? F5 C7 C6 119.3(16) . . ? F5 C7 C2 120.0(15) . . ? C6 C7 C2 120.7(17) . . ? C1 C8 C9 123.0(15) . . ? C1 C8 H8 118.5 . . ? C9 C8 H8 118.5 . . ? O6 C9 C8 121.9(14) . . ? O6 C9 C10 116.8(13) . . ? C8 C9 C10 121.1(14) . . ? C15 C10 C11 117.4(17) . . ? C15 C10 C9 119.8(15) . . ? C11 C10 C9 122.2(16) . . ? C12 C11 C10 123(2) . . ? C12 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? C13 C12 C11 119(2) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 120(2) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 118.7(19) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C10 C15 C14 121.9(18) . . ? C10 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? O7 C16 C23 125.9(14) . . ? O7 C16 C17 116.1(13) . . ? C23 C16 C17 117.9(15) . . ? C22 C17 C18 117.1(15) . . ? C22 C17 C16 122.3(14) . . ? C18 C17 C16 120.2(15) . . ? F6 C18 C17 121.9(15) . . ? F6 C18 C19 116.7(15) . . ? C17 C18 C19 121.4(16) . . ? F7 C19 C20 119.8(14) . . ? F7 C19 C18 120.7(15) . . ? C20 C19 C18 119.3(15) . . ? F8 C20 C21 120.9(17) . . ? F8 C20 C19 119.9(17) . . ? C21 C20 C19 119.2(15) . . ? F9 C21 C22 119.0(15) . . ? F9 C21 C20 119.9(15) . . ? C22 C21 C20 121.1(16) . . ? C21 C22 F10 117.4(15) . . ? C21 C22 C17 121.7(15) . . ? F10 C22 C17 120.8(14) . . ? C16 C23 C24 122.4(16) . . ? C16 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? O8 C24 C23 125.0(14) . . ? O8 C24 C25 118.7(14) . . ? C23 C24 C25 116.3(14) . . ? C30 C25 C26 119.3(15) . . ? C30 C25 C24 122.0(15) . . ? C26 C25 C24 118.6(14) . . ? C27 C26 C25 119.8(16) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 120.6(17) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C29 C28 C27 120.4(17) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C30 120.5(18) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C25 C30 C29 119.4(17) . . ? C25 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? O9 C31 C38 126.8(16) . . ? O9 C31 C32 112.7(15) . . ? C38 C31 C32 120.4(15) . . ? C37 C32 C33 118.7(19) . . ? C37 C32 C31 119.1(17) . . ? C33 C32 C31 121.9(17) . . ? C34 C33 F11 118(2) . . ? C34 C33 C32 122(2) . . ? F11 C33 C32 119.7(17) . . ? C33 C34 F12 119(2) . . ? C33 C34 C35 118(2) . . ? F12 C34 C35 123(2) . . ? C36 C35 F13 124(3) . . ? C36 C35 C34 120(2) . . ? F13 C35 C34 115(3) . . ? C35 C36 F14 118(2) . . ? C35 C36 C37 120(3) . . ? F14 C36 C37 122(2) . . ? C32 C37 F15 128(2) . . ? C32 C37 C36 120(2) . . ? F15 C37 C36 112(2) . . ? C31 C38 C39 124.0(17) . . ? C31 C38 H38 118.0 . . ? C39 C38 H38 118.0 . . ? O10 C39 C38 121.1(17) . . ? O10 C39 C40 120.6(19) . . ? C38 C39 C40 118.1(18) . . ? C41 C40 C45 116(2) . . ? C41 C40 C39 118(2) . . ? C45 C40 C39 126(3) . . ? C40 C41 C42 125(3) . . ? C40 C41 H41 117.3 . . ? C42 C41 H41 117.3 . . ? C43 C42 C41 114(3) . . ? C43 C42 H42 122.8 . . ? C41 C42 H42 122.8 . . ? C42 C43 C44 120(2) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 123(3) . . ? C45 C44 H44 118.4 . . ? C43 C44 H44 118.4 . . ? C44 C45 C40 121(3) . . ? C44 C45 H45 119.6 . . ? C40 C45 H45 119.6 . . ? O11 C46 C53 124.9(14) . . ? O11 C46 C47 118.3(13) . . ? C53 C46 C47 116.7(14) . . ? C48 C47 C52 117.6(15) . . ? C48 C47 C46 120.3(14) . . ? C52 C47 C46 121.9(14) . . ? F16 C48 C47 121.6(15) . . ? F16 C48 C49 117.1(14) . . ? C47 C48 C49 121.3(16) . . ? F17 C49 C50 121.8(17) . . ? F17 C49 C48 118.9(16) . . ? C50 C49 C48 119.3(17) . . ? C51 C50 F18 121.2(17) . . ? C51 C50 C49 121.0(18) . . ? F18 C50 C49 117.6(17) . . ? F19 C51 C50 121.2(17) . . ? F19 C51 C52 118.3(16) . . ? C50 C51 C52 120.5(17) . . ? F20 C52 C51 119.2(15) . . ? F20 C52 C47 120.6(15) . . ? C51 C52 C47 120.2(16) . . ? C46 C53 C54 126.3(15) . . ? C46 C53 H53 116.8 . . ? C54 C53 H53 116.8 . . ? O12 C54 C53 121.6(14) . . ? O12 C54 C55 118.4(13) . . ? C53 C54 C55 119.9(13) . . ? C56 C55 C60 120.0 . . ? C56 C55 C54 122.7(10) . . ? C60 C55 C54 117.3(10) . . ? C57 C56 C55 120.0 . . ? C57 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C58 C57 C56 120.0 . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C59 120.0 . . ? C57 C58 H58 120.0 . . ? C59 C58 H58 120.0 . . ? C60 C59 C58 120.0 . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 C55 120.0 . . ? C59 C60 H60 120.0 . . ? C55 C60 H60 120.0 . . ? O13 C61 C68 127.9(15) . . ? O13 C61 C62 113.7(14) . . ? C68 C61 C62 118.3(15) . . ? C63 C62 C67 115.2(17) . . ? C63 C62 C61 123.2(15) . . ? C67 C62 C61 121.2(16) . . ? C62 C63 F21 119.6(16) . . ? C62 C63 C64 123.2(17) . . ? F21 C63 C64 117.2(16) . . ? F22 C64 C65 120.6(15) . . ? F22 C64 C63 121.0(16) . . ? C65 C64 C63 118.4(17) . . ? C66 C65 F23 119.2(19) . . ? C66 C65 C64 121.7(19) . . ? F23 C65 C64 119.1(17) . . ? C65 C66 F24 123(2) . . ? C65 C66 C67 118(2) . . ? F24 C66 C67 120(2) . . ? C62 C67 F25 120.9(17) . . ? C62 C67 C66 123.5(19) . . ? F25 C67 C66 115.2(19) . . ? C61 C68 C69 124.4(16) . . ? C61 C68 H68 117.8 . . ? C69 C68 H68 117.8 . . ? O14 C69 C68 119.7(15) . . ? O14 C69 C70 118.9(15) . . ? C68 C69 C70 121.3(15) . . ? C75 C70 C71 118.5(16) . . ? C75 C70 C69 124.2(16) . . ? C71 C70 C69 117.3(16) . . ? C70 C71 C72 121.3(17) . . ? C70 C71 H71 119.4 . . ? C72 C71 H71 119.4 . . ? C71 C72 C73 117.8(19) . . ? C71 C72 H72 121.1 . . ? C73 C72 H72 121.1 . . ? C74 C73 C72 120.3(17) . . ? C74 C73 H73 119.9 . . ? C72 C73 H73 119.9 . . ? C75 C74 C73 119.8(18) . . ? C75 C74 H74 120.1 . . ? C73 C74 H74 120.1 . . ? C74 C75 C70 122.3(18) . . ? C74 C75 H75 118.8 . . ? C70 C75 H75 118.8 . . ? O15 C76 C83 126.5(14) . . ? O15 C76 C77 116.7(13) . . ? C83 C76 C77 116.7(13) . . ? C78 C77 C82 115.6(14) . . ? C78 C77 C76 124.1(14) . . ? C82 C77 C76 120.0(14) . . ? F26 C78 C79 116.4(16) . . ? F26 C78 C77 122.2(15) . . ? C79 C78 C77 121.4(16) . . ? C80 C79 C78 121.3(17) . . ? C80 C79 F27 119.8(16) . . ? C78 C79 F27 118.8(17) . . ? F28 C80 C81 123.4(19) . . ? F28 C80 C79 119.1(18) . . ? C81 C80 C79 117.2(16) . . ? C80 C81 C82 123.1(18) . . ? C80 C81 F29 117.5(17) . . ? C82 C81 F29 119.3(18) . . ? F30 C82 C81 118.5(17) . . ? F30 C82 C77 120.0(15) . . ? C81 C82 C77 121.2(16) . . ? C84 C83 C76 123.1(15) . . ? C84 C83 H83 118.5 . . ? C76 C83 H83 118.5 . . ? O16 C84 C83 124.6(15) . . ? O16 C84 C85 114.8(14) . . ? C83 C84 C85 120.4(15) . . ? C90 C85 C86 118.9(16) . . ? C90 C85 C84 120.4(15) . . ? C86 C85 C84 120.7(15) . . ? C87 C86 C85 119.3(18) . . ? C87 C86 H86 120.4 . . ? C85 C86 H86 120.4 . . ? C88 C87 C86 120.8(18) . . ? C88 C87 H87 119.6 . . ? C86 C87 H87 119.6 . . ? C87 C88 C89 117.7(17) . . ? C87 C88 H88 121.1 . . ? C89 C88 H88 121.1 . . ? C88 C89 C90 123.5(18) . . ? C88 C89 H89 118.2 . . ? C90 C89 H89 118.2 . . ? C85 C90 C89 119.7(17) . . ? C85 C90 H90 120.1 . . ? C89 C90 H90 120.1 . . ? O17 C91 C98 129.0(14) . . ? O17 C91 C92 114.4(13) . . ? C98 C91 C92 116.6(14) . . ? C93 C92 C97 118.2(15) . . ? C93 C92 C91 121.8(14) . . ? C97 C92 C91 120.0(15) . . ? F31 C93 C94 116.0(18) . . ? F31 C93 C92 121.3(14) . . ? C94 C93 C92 122.7(17) . . ? F32 C94 C93 123.0(19) . . ? F32 C94 C95 118.3(17) . . ? C93 C94 C95 118.7(19) . . ? F33 C95 C96 123(2) . . ? F33 C95 C94 118(2) . . ? C96 C95 C94 118.8(17) . . ? C95 C96 F34 119.0(17) . . ? C95 C96 C97 122.2(18) . . ? F34 C96 C97 118.7(18) . . ? F35 C97 C96 118.0(16) . . ? F35 C97 C92 122.6(15) . . ? C96 C97 C92 119.3(17) . . ? C91 C98 C99 120.0(16) . . ? C91 C98 H98 120.0 . . ? C99 C98 H98 120.0 . . ? O18 C99 C98 125.1(14) . . ? O18 C99 C100 116.4(13) . . ? C98 C99 C100 118.5(15) . . ? C101 C100 C105 118.8(17) . . ? C101 C100 C99 124.1(15) . . ? C105 C100 C99 116.9(15) . . ? C100 C101 C102 121.9(18) . . ? C100 C101 H101 119.0 . . ? C102 C101 H101 119.0 . . ? C103 C102 C101 118.2(18) . . ? C103 C102 H102 120.9 . . ? C101 C102 H102 120.9 . . ? C102 C103 C104 121.9(17) . . ? C102 C103 H103 119.1 . . ? C104 C103 H103 119.1 . . ? C103 C104 C105 119.2(17) . . ? C103 C104 H104 120.4 . . ? C105 C104 H104 120.4 . . ? C104 C105 C100 119.7(17) . . ? C104 C105 H105 120.1 . . ? C100 C105 H105 120.1 . . ? O19 C106 C113 128.0(16) . . ? O19 C106 C107 117.2(15) . . ? C113 C106 C107 114.7(15) . . ? C108 C107 C112 117.7(18) . . ? C108 C107 C106 121.5(18) . . ? C112 C107 C106 120.9(16) . . ? F36 C108 C107 119.2(19) . . ? F36 C108 C109 118.8(19) . . ? C107 C108 C109 122.0(19) . . ? F37 C109 C110 127.3(19) . . ? F37 C109 C108 116(2) . . ? C110 C109 C108 116.3(19) . . ? C111 C110 C109 123.3(19) . . ? C111 C110 F38 123(2) . . ? C109 C110 F38 114(2) . . ? C110 C111 F39 119.4(19) . . ? C110 C111 C112 120(2) . . ? F39 C111 C112 120.2(19) . . ? F40 C112 C107 122.5(16) . . ? F40 C112 C111 117.1(17) . . ? C107 C112 C111 120.3(19) . . ? C106 C113 C114 121.3(16) . . ? C106 C113 H113 119.3 . . ? C114 C113 H113 119.3 . . ? O20 C114 C113 123.4(16) . . ? O20 C114 C115 114.1(14) . . ? C113 C114 C115 122.4(14) . . ? C120 C115 C116 118.1(17) . . ? C120 C115 C114 119.1(14) . . ? C116 C115 C114 122.8(16) . . ? C117 C116 C115 120.0(18) . . ? C117 C116 H116 120.0 . . ? C115 C116 H116 120.0 . . ? C118 C117 C116 120.9(19) . . ? C118 C117 H117 119.5 . . ? C116 C117 H117 119.5 . . ? C117 C118 C119 119.6(18) . . ? C117 C118 H118 120.2 . . ? C119 C118 H118 120.2 . . ? C120 C119 C118 120.0(19) . . ? C120 C119 H119 120.0 . . ? C118 C119 H119 120.0 . . ? C119 C120 C115 121.2(18) . . ? C119 C120 H120 119.4 . . ? C115 C120 H120 119.4 . . ? O23 C121 C122 119(3) . . ? O23 C121 C123 122(2) . . ? C122 C121 C123 119(3) . . ? C121 C122 H12D 109.5 . . ? C121 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? C121 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? C121 C123 H12A 109.5 . . ? C121 C123 H12B 109.5 . . ? H12A C123 H12B 109.5 . . ? C121 C123 H12C 109.5 . . ? H12A C123 H12C 109.5 . . ? H12B C123 H12C 109.5 . . ? C125 C124 H12G 109.5 . . ? C125 C124 H12H 109.5 . . ? H12G C124 H12H 109.5 . . ? C125 C124 H12I 109.5 . . ? H12G C124 H12I 109.5 . . ? H12H C124 H12I 109.5 . . ? C124 C125 C126 118(3) . . ? C124 C125 C130 122(3) . . ? C126 C125 C130 120.0 . . ? C125 C126 C127 120.0 . . ? C125 C126 H126 120.0 . . ? C127 C126 H126 120.0 . . ? C128 C127 C126 120.0 . . ? C128 C127 H127 120.0 . . ? C126 C127 H127 120.0 . . ? C127 C128 C129 120.0 . . ? C127 C128 H128 120.0 . . ? C129 C128 H128 120.0 . . ? C128 C129 C130 120.0 . . ? C128 C129 H129 120.0 . . ? C130 C129 H129 120.0 . . ? C129 C130 C125 120.0 . . ? C129 C130 H130 120.0 . . ? C125 C130 H130 120.0 . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 2.451 _refine_diff_density_min -2.636 _refine_diff_density_rms 0.206