# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 894562' #TrackingRef 'cec.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H32 Er2 N2 O17' _chemical_formula_weight 1207.25 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.0445(12) _cell_length_b 27.598(2) _cell_length_c 9.9439(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.898(9) _cell_angle_gamma 90.00 _cell_volume 4379.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6092 _cell_measurement_theta_min 2.4205 _cell_measurement_theta_max 25 _exptl_crystal_description sheet _exptl_crystal_colour pink _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 3.884 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.22446 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 20728 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7705 _reflns_number_gt 5732 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0679P)^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 0.00015(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7705 _refine_ls_number_parameters 551 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1020 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_restrained_S_all 0.888 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.944292(18) 0.470757(10) -0.22399(3) 0.02295(11) Uani 1 1 d . . . Er2 Er 0.639677(18) 0.485301(10) -0.35581(3) 0.02460(11) Uani 1 1 d . . . O4 O 0.7094(3) 0.41551(16) -0.3245(5) 0.0390(12) Uani 1 1 d . . . O12 O 0.5259(3) 0.44286(16) -0.2858(4) 0.0328(11) Uani 1 1 d . . . O14 O 0.4357(3) 0.05266(16) -0.1151(5) 0.0401(12) Uani 1 1 d . . . O1 O 0.9475(3) 0.01774(16) -0.3304(5) 0.0355(12) Uani 1 1 d . . . O6 O 0.9633(3) 0.90518(16) -0.3098(4) 0.0350(11) Uani 1 1 d . . . O3 O 0.8473(3) 0.42001(17) -0.3070(5) 0.0364(12) Uani 1 1 d . . . O7 O 0.9683(3) 0.93916(16) -0.1117(4) 0.0335(11) Uani 1 1 d . . . C14 C 0.7808(4) 0.3967(2) -0.2954(6) 0.0258(15) Uani 1 1 d . . . C21 C 0.9430(4) 0.9054(2) -0.1911(6) 0.0291(15) Uani 1 1 d . . . C28 C 0.7996(4) 0.5522(2) -0.1871(6) 0.0277(15) Uani 1 1 d . . . O8 O 0.7378(3) 0.52989(16) -0.2413(5) 0.0403(12) Uani 1 1 d . . . C42 C 0.5050(4) 0.0713(2) -0.0724(6) 0.0279(15) Uani 1 1 d . . . C11 C 0.7856(4) 0.3461(2) -0.2460(6) 0.0267(15) Uani 1 1 d . . . C7 C 0.9187(4) 0.0543(2) -0.3962(7) 0.0293(15) Uani 1 1 d . . . O13 O 0.5713(3) 0.04804(16) -0.0475(4) 0.0319(11) Uani 1 1 d . . . O9 O 0.8707(3) 0.53469(18) -0.1585(5) 0.0435(13) Uani 1 1 d . . . O16 O 0.7235(3) 0.50826(19) -0.5224(5) 0.0411(12) Uani 1 1 d . . . C25 C 0.7886(4) 0.6054(2) -0.1545(6) 0.0262(15) Uani 1 1 d . . . C39 C 0.5044(4) 0.1246(2) -0.0437(6) 0.0287(15) Uani 1 1 d . . . C40 C 0.5790(4) 0.1499(2) -0.0192(7) 0.0325(16) Uani 1 1 d . . . H40A H 0.6296 0.1348 -0.0303 0.039 Uiso 1 1 calc R . . O1W O 0.8966(3) 0.50944(18) -0.4283(5) 0.0386(12) Uani 1 1 d . . . H1WB H 0.9252 0.5362 -0.4572 0.046 Uiso 1 1 calc R . . H1WA H 0.8491 0.4980 -0.4801 0.046 Uiso 1 1 calc R . . O11 O 0.6202(3) 0.46524(17) -0.1227(5) 0.0441(13) Uani 1 1 d . . . O2 O 0.9164(3) 0.05740(18) -0.5215(5) 0.0447(13) Uani 1 1 d . . . O10 O 0.7569(4) 0.74683(17) -0.0336(5) 0.0500(14) Uani 1 1 d . . . N2 N 0.7774(4) 0.5121(3) -0.7251(6) 0.055(2) Uani 1 1 d . . . O5 O 0.7944(5) 0.20609(18) -0.1005(6) 0.074(2) Uani 1 1 d . . . C45 C 0.7163(4) 0.5178(3) -0.6464(7) 0.0340(16) Uani 1 1 d . . . C35 C 0.5629(4) 0.4365(2) -0.1674(7) 0.0301(16) Uani 1 1 d . . . N1 N 0.6502(4) 0.5371(3) -0.7151(6) 0.057(2) Uani 1 1 d . . . H1A H 0.6054 0.5453 -0.6800 0.068 Uiso 1 1 calc R . . C15 C 0.8924(5) 0.8647(2) -0.1478(7) 0.0339(17) Uani 1 1 d . . . C33 C 0.4868(5) 0.3119(2) -0.0973(7) 0.0395(19) Uani 1 1 d . . . H33A H 0.4579 0.2871 -0.1452 0.047 Uiso 1 1 calc R . . C1 C 0.8870(4) 0.0945(2) -0.3197(6) 0.0287(15) Uani 1 1 d . . . C2 C 0.8998(5) 0.0959(2) -0.1823(7) 0.0379(18) Uani 1 1 d . . . H2B H 0.9294 0.0710 -0.1360 0.046 Uiso 1 1 calc R . . C34 C 0.4991(4) 0.3556(2) -0.1587(7) 0.0335(16) Uani 1 1 d . . . H34A H 0.4769 0.3602 -0.2479 0.040 Uiso 1 1 calc R . . C22 C 0.7699(5) 0.7006(2) -0.0835(7) 0.0328(17) Uani 1 1 d . . . C27 C 0.8497(5) 0.6822(2) -0.0863(7) 0.0367(17) Uani 1 1 d . . . H27A H 0.8965 0.7017 -0.0659 0.044 Uiso 1 1 calc R . . C24 C 0.7103(4) 0.6247(2) -0.1557(7) 0.0355(17) Uani 1 1 d . . . H24A H 0.6633 0.6057 -0.1805 0.043 Uiso 1 1 calc R . . C29 C 0.5430(4) 0.3922(2) -0.0920(7) 0.0290(15) Uani 1 1 d . . . O15 O 0.5030(4) 0.26414(16) 0.1058(5) 0.0624(19) Uani 1 1 d . . . C26 C 0.8583(4) 0.6341(2) -0.1202(7) 0.0340(17) Uani 1 1 d . . . H26A H 0.9116 0.6208 -0.1199 0.041 Uiso 1 1 calc R . . C38 C 0.4295(5) 0.1480(3) -0.0311(7) 0.0402(18) Uani 1 1 d . . . H38A H 0.3790 0.1318 -0.0528 0.048 Uiso 1 1 calc R . . C20 C 0.8692(5) 0.8600(3) -0.0182(8) 0.050(2) Uani 1 1 d . . . H20A H 0.8832 0.8842 0.0452 0.060 Uiso 1 1 calc R . . C12 C 0.7146(5) 0.3230(2) -0.2132(7) 0.0374(18) Uani 1 1 d . . . H12A H 0.6637 0.3395 -0.2225 0.045 Uiso 1 1 calc R . . C3 C 0.8693(5) 0.1339(2) -0.1106(7) 0.045(2) Uani 1 1 d . . . H3A H 0.8778 0.1342 -0.0167 0.054 Uiso 1 1 calc R . . C41 C 0.5781(5) 0.1979(3) 0.0218(7) 0.042(2) Uani 1 1 d . . . H41A H 0.6277 0.2154 0.0356 0.050 Uiso 1 1 calc R . . C23 C 0.7009(5) 0.6733(2) -0.1196(8) 0.0408(19) Uani 1 1 d . . . H23A H 0.6477 0.6867 -0.1203 0.049 Uiso 1 1 calc R . . C10 C 0.8610(5) 0.3221(3) -0.2320(8) 0.044(2) Uani 1 1 d . . . H10A H 0.9092 0.3373 -0.2555 0.053 Uiso 1 1 calc R . . C36 C 0.5036(6) 0.2192(2) 0.0418(7) 0.046(2) Uani 1 1 d . . . C13 C 0.7176(5) 0.2761(3) -0.1668(8) 0.050(2) Uani 1 1 d . . . H13A H 0.6693 0.2606 -0.1449 0.061 Uiso 1 1 calc R . . C30 C 0.5749(6) 0.3854(3) 0.0416(8) 0.052(2) Uani 1 1 d . . . H30A H 0.6055 0.4098 0.0882 0.063 Uiso 1 1 calc R . . C18 C 0.8022(5) 0.7851(2) -0.0749(8) 0.043(2) Uani 1 1 d . . . C6 C 0.8433(6) 0.1319(3) -0.3867(7) 0.058(3) Uani 1 1 d . . . H6A H 0.8351 0.1317 -0.4806 0.069 Uiso 1 1 calc R . . C4 C 0.8269(6) 0.1708(2) -0.1778(8) 0.051(2) Uani 1 1 d . . . C32 C 0.5175(5) 0.3052(2) 0.0349(7) 0.0364(18) Uani 1 1 d . . . C19 C 0.8263(6) 0.8205(3) 0.0176(8) 0.055(2) Uani 1 1 d . . . H19A H 0.8132 0.8173 0.1061 0.066 Uiso 1 1 calc R . . C44 C 0.7496(5) 0.5257(3) -0.8637(9) 0.059(2) Uiso 1 1 d . . . H44A H 0.7509 0.4982 -0.9241 0.071 Uiso 1 1 calc R . . H44B H 0.7841 0.5515 -0.8948 0.071 Uiso 1 1 calc R . . C8 C 0.7929(5) 0.2528(3) -0.1534(8) 0.049(2) Uiso 1 1 d . . . C37 C 0.4296(5) 0.1955(3) 0.0140(8) 0.045(2) Uiso 1 1 d . . . H37A H 0.3793 0.2110 0.0251 0.054 Uiso 1 1 calc R . . C31 C 0.5611(5) 0.3423(3) 0.1050(9) 0.050(2) Uiso 1 1 d . . . H31A H 0.5811 0.3380 0.1954 0.060 Uiso 1 1 calc R . . C43 C 0.6614(5) 0.5428(3) -0.8551(9) 0.057(2) Uiso 1 1 d . . . H43A H 0.6548 0.5764 -0.8826 0.068 Uiso 1 1 calc R . . H43B H 0.6216 0.5231 -0.9114 0.068 Uiso 1 1 calc R . . C5 C 0.8114(6) 0.1696(3) -0.3159(9) 0.061(2) Uiso 1 1 d . . . H5A H 0.7798 0.1939 -0.3615 0.073 Uiso 1 1 calc R . . C9 C 0.8648(5) 0.2751(3) -0.1829(9) 0.056(2) Uiso 1 1 d . . . H9A H 0.9159 0.2589 -0.1700 0.067 Uiso 1 1 calc R . . C16 C 0.8680(6) 0.8292(3) -0.2382(10) 0.062(2) Uiso 1 1 d . . . H16A H 0.8827 0.8318 -0.3259 0.074 Uiso 1 1 calc R . . C17 C 0.8216(6) 0.7891(3) -0.2039(10) 0.066(3) Uiso 1 1 d . . . H17A H 0.8044 0.7657 -0.2681 0.079 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 0.02809(17) 0.02010(17) 0.02097(16) 0.00161(11) 0.00395(12) -0.00231(12) Er2 0.02947(18) 0.01814(17) 0.02598(17) 0.00347(12) 0.00188(12) -0.00088(13) O4 0.039(3) 0.020(2) 0.055(3) 0.005(2) -0.008(2) 0.003(2) O12 0.036(3) 0.035(3) 0.029(3) 0.007(2) 0.005(2) 0.000(2) O14 0.041(3) 0.023(3) 0.053(3) -0.005(2) -0.012(2) -0.002(2) O1 0.036(3) 0.023(3) 0.047(3) -0.001(2) 0.001(2) 0.014(2) O6 0.049(3) 0.033(3) 0.024(3) -0.006(2) 0.005(2) -0.010(2) O3 0.040(3) 0.031(3) 0.037(3) -0.003(2) -0.002(2) -0.013(2) O7 0.042(3) 0.032(3) 0.028(3) -0.010(2) 0.008(2) -0.008(2) C14 0.038(4) 0.021(3) 0.018(3) -0.006(3) 0.002(3) -0.002(3) C21 0.034(4) 0.033(4) 0.020(4) 0.002(3) 0.001(3) 0.002(3) C28 0.044(4) 0.026(4) 0.014(3) 0.004(3) 0.002(3) 0.006(3) O8 0.047(3) 0.028(3) 0.045(3) -0.009(2) -0.002(3) -0.013(2) C42 0.039(4) 0.024(4) 0.021(3) 0.002(3) 0.007(3) -0.008(3) C11 0.036(4) 0.020(3) 0.024(3) -0.001(3) 0.001(3) 0.000(3) C7 0.023(3) 0.027(4) 0.038(4) -0.006(3) 0.008(3) -0.006(3) O13 0.037(3) 0.029(3) 0.030(3) -0.006(2) 0.003(2) 0.010(2) O9 0.047(3) 0.033(3) 0.049(3) -0.008(2) -0.002(3) 0.010(3) O16 0.037(3) 0.055(3) 0.031(3) 0.012(2) 0.006(2) -0.003(3) C25 0.035(4) 0.019(3) 0.024(3) 0.001(3) 0.005(3) -0.001(3) C39 0.038(4) 0.020(3) 0.027(4) 0.003(3) -0.002(3) 0.003(3) C40 0.036(4) 0.023(4) 0.038(4) 0.001(3) 0.003(3) -0.003(3) O1W 0.035(3) 0.048(3) 0.032(3) 0.015(2) -0.001(2) -0.007(2) O11 0.064(3) 0.038(3) 0.030(3) 0.000(2) 0.004(3) -0.023(3) O2 0.064(3) 0.041(3) 0.032(3) -0.009(2) 0.018(3) -0.002(3) O10 0.077(4) 0.021(3) 0.058(4) -0.005(2) 0.033(3) -0.006(3) N2 0.046(4) 0.093(6) 0.029(4) 0.010(4) 0.008(3) 0.027(4) O5 0.166(7) 0.018(3) 0.050(4) 0.010(2) 0.060(4) 0.029(3) C45 0.034(4) 0.039(4) 0.028(4) 0.005(3) 0.002(3) 0.003(3) C35 0.044(4) 0.019(3) 0.028(4) 0.000(3) 0.011(3) 0.001(3) N1 0.036(4) 0.098(6) 0.036(4) 0.023(4) 0.007(3) 0.022(4) C15 0.054(4) 0.022(4) 0.027(4) -0.006(3) 0.008(3) -0.003(3) C33 0.065(5) 0.026(4) 0.028(4) 0.000(3) 0.004(4) -0.011(4) C1 0.044(4) 0.018(3) 0.026(4) -0.001(3) 0.012(3) 0.003(3) C2 0.062(5) 0.027(4) 0.023(4) 0.007(3) -0.002(4) 0.009(4) C34 0.043(4) 0.032(4) 0.024(4) -0.001(3) 0.001(3) 0.000(3) C22 0.055(5) 0.015(3) 0.031(4) -0.004(3) 0.019(4) -0.005(3) C27 0.043(4) 0.030(4) 0.037(4) -0.005(3) 0.004(3) -0.018(4) C24 0.038(4) 0.026(4) 0.043(4) 0.001(3) 0.005(3) -0.008(3) C29 0.043(4) 0.017(3) 0.027(4) 0.004(3) 0.007(3) -0.001(3) O15 0.144(6) 0.012(2) 0.034(3) 0.002(2) 0.021(3) -0.010(3) C26 0.041(4) 0.028(4) 0.033(4) -0.008(3) 0.003(3) -0.005(3) C38 0.044(4) 0.033(4) 0.042(5) -0.001(3) -0.002(4) -0.002(4) C20 0.081(6) 0.037(5) 0.033(4) -0.010(3) 0.019(4) -0.023(4) C12 0.044(4) 0.025(4) 0.043(4) 0.006(3) 0.007(4) 0.004(3) C3 0.090(6) 0.024(4) 0.022(4) 0.001(3) 0.010(4) 0.014(4) C41 0.064(5) 0.027(4) 0.032(4) 0.008(3) -0.004(4) -0.023(4) C23 0.036(4) 0.026(4) 0.063(5) -0.003(4) 0.013(4) 0.008(3) C10 0.047(5) 0.040(5) 0.047(5) 0.009(4) 0.011(4) 0.017(4) C36 0.091(7) 0.019(4) 0.028(4) 0.006(3) 0.001(4) 0.008(4) C13 0.072(6) 0.035(4) 0.048(5) 0.008(4) 0.022(4) -0.004(4) C30 0.094(7) 0.026(4) 0.035(5) 0.001(3) -0.001(4) -0.016(4) C18 0.071(6) 0.016(4) 0.044(5) 0.004(3) 0.020(4) -0.010(4) C6 0.108(7) 0.046(5) 0.019(4) 0.002(3) 0.011(4) 0.041(5) C4 0.102(7) 0.020(4) 0.035(4) 0.006(3) 0.033(5) 0.018(4) C32 0.066(5) 0.016(3) 0.030(4) -0.002(3) 0.016(4) 0.003(3) C19 0.094(7) 0.040(5) 0.036(5) -0.006(4) 0.027(5) -0.022(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 O1 2.189(4) 2_754 ? Er1 O3 2.191(4) . ? Er1 O2 2.246(5) 4_566 ? Er1 O9 2.256(5) . ? Er1 O6 2.342(4) 2_744 ? Er1 O1W 2.352(4) . ? Er1 O7 2.422(4) 2_744 ? Er1 C21 2.748(7) 2_744 ? Er2 O8 2.218(5) . ? Er2 O14 2.220(4) 2_654 ? Er2 O4 2.233(4) . ? Er2 O13 2.292(4) 4_565 ? Er2 O16 2.326(5) . ? Er2 O12 2.335(4) . ? Er2 O11 2.434(5) . ? Er2 C35 2.705(7) . ? O4 C14 1.264(7) . ? O12 C35 1.275(8) . ? O14 C42 1.260(8) . ? O14 Er2 2.220(4) 2_644 ? O1 C7 1.264(8) . ? O1 Er1 2.189(4) 2_744 ? O6 C21 1.256(8) . ? O6 Er1 2.342(4) 2_754 ? O3 C14 1.261(7) . ? O7 C21 1.261(7) . ? O7 Er1 2.422(4) 2_754 ? C14 C11 1.480(9) . ? C21 C15 1.474(9) . ? C21 Er1 2.748(7) 2_754 ? C28 O8 1.242(8) . ? C28 O9 1.244(8) . ? C28 C25 1.517(8) . ? C42 O13 1.245(8) . ? C42 C39 1.497(8) . ? C11 C12 1.373(9) . ? C11 C10 1.374(9) . ? C7 O2 1.245(8) . ? C7 C1 1.467(9) . ? O13 Er2 2.292(4) 4_566 ? O16 C45 1.255(8) . ? C25 C24 1.365(9) . ? C25 C26 1.384(9) . ? C39 C38 1.382(9) . ? C39 C40 1.386(9) . ? C40 C41 1.386(9) . ? O11 C35 1.260(8) . ? O2 Er1 2.246(5) 4_565 ? O10 C18 1.370(8) . ? O10 C22 1.392(8) . ? N2 C45 1.324(9) . ? N2 C44 1.454(11) . ? O5 C4 1.376(8) . ? O5 C8 1.390(9) . ? C45 N1 1.314(9) . ? C35 C29 1.485(9) . ? N1 C43 1.431(10) . ? C15 C16 1.360(10) . ? C15 C20 1.384(10) . ? C33 C32 1.367(10) . ? C33 C34 1.374(9) . ? C1 C2 1.361(9) . ? C1 C6 1.379(9) . ? C2 C3 1.386(9) . ? C34 C29 1.366(9) . ? C22 C23 1.357(9) . ? C22 C27 1.381(10) . ? C27 C26 1.380(9) . ? C24 C23 1.399(9) . ? C29 C30 1.387(10) . ? O15 C32 1.368(8) . ? O15 C36 1.396(8) . ? C38 C37 1.384(10) . ? C20 C19 1.357(10) . ? C12 C13 1.374(10) . ? C3 C4 1.361(10) . ? C41 C36 1.363(11) . ? C10 C9 1.384(10) . ? C36 C37 1.360(11) . ? C13 C8 1.365(11) . ? C30 C31 1.374(10) . ? C18 C17 1.355(11) . ? C18 C19 1.370(10) . ? C6 C5 1.384(11) . ? C4 C5 1.371(11) . ? C32 C31 1.387(10) . ? C44 C43 1.502(11) . ? C8 C9 1.367(11) . ? C16 C17 1.396(12) . ? 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 O3 170.38(18) 2_754 . ? O1 Er1 O2 102.10(19) 2_754 4_566 ? O3 Er1 O2 85.27(19) . 4_566 ? O1 Er1 O9 83.74(18) 2_754 . ? O3 Er1 O9 103.65(18) . . ? O2 Er1 O9 81.57(19) 4_566 . ? O1 Er1 O6 87.02(17) 2_754 2_744 ? O3 Er1 O6 88.56(17) . 2_744 ? O2 Er1 O6 77.63(17) 4_566 2_744 ? O9 Er1 O6 154.90(17) . 2_744 ? O1 Er1 O1W 97.11(17) 2_754 . ? O3 Er1 O1W 79.00(17) . . ? O2 Er1 O1W 148.67(18) 4_566 . ? O9 Er1 O1W 76.15(18) . . ? O6 Er1 O1W 128.29(16) 2_744 . ? O1 Er1 O7 83.14(17) 2_754 2_744 ? O3 Er1 O7 87.34(17) . 2_744 ? O2 Er1 O7 131.50(17) 4_566 2_744 ? O9 Er1 O7 146.38(17) . 2_744 ? O6 Er1 O7 54.30(15) 2_744 2_744 ? O1W Er1 O7 74.96(16) . 2_744 ? O1 Er1 C21 86.24(18) 2_754 2_744 ? O3 Er1 C21 85.94(18) . 2_744 ? O2 Er1 C21 104.27(19) 4_566 2_744 ? O9 Er1 C21 169.29(19) . 2_744 ? O6 Er1 C21 27.10(17) 2_744 2_744 ? O1W Er1 C21 101.45(18) . 2_744 ? O7 Er1 C21 27.31(16) 2_744 2_744 ? O8 Er2 O14 87.17(17) . 2_654 ? O8 Er2 O4 95.04(17) . . ? O14 Er2 O4 177.02(17) 2_654 . ? O8 Er2 O13 154.61(18) . 4_565 ? O14 Er2 O13 91.15(17) 2_654 4_565 ? O4 Er2 O13 87.70(17) . 4_565 ? O8 Er2 O16 77.44(19) . . ? O14 Er2 O16 91.50(19) 2_654 . ? O4 Er2 O16 90.92(18) . . ? O13 Er2 O16 77.28(17) 4_565 . ? O8 Er2 O12 131.36(18) . . ? O14 Er2 O12 91.53(17) 2_654 . ? O4 Er2 O12 85.51(16) . . ? O13 Er2 O12 73.99(15) 4_565 . ? O16 Er2 O12 151.16(17) . . ? O8 Er2 O11 77.94(18) . . ? O14 Er2 O11 101.13(19) 2_654 . ? O4 Er2 O11 77.44(18) . . ? O13 Er2 O11 127.10(16) 4_565 . ? O16 Er2 O11 151.64(17) . . ? O12 Er2 O11 54.65(16) . . ? O8 Er2 C35 105.7(2) . . ? O14 Er2 C35 103.07(19) 2_654 . ? O4 Er2 C35 74.43(19) . . ? O13 Er2 C35 99.37(18) 4_565 . ? O16 Er2 C35 165.17(18) . . ? O12 Er2 C35 28.11(17) . . ? O11 Er2 C35 27.76(17) . . ? C14 O4 Er2 144.7(4) . . ? C35 O12 Er2 92.3(4) . . ? C42 O14 Er2 146.8(4) . 2_644 ? C7 O1 Er1 147.0(4) . 2_744 ? C21 O6 Er1 94.8(4) . 2_754 ? C14 O3 Er1 150.0(4) . . ? C21 O7 Er1 90.9(4) . 2_754 ? O3 C14 O4 121.6(6) . . ? O3 C14 C11 119.8(6) . . ? O4 C14 C11 118.6(6) . . ? O6 C21 O7 119.5(6) . . ? O6 C21 C15 118.3(6) . . ? O7 C21 C15 122.1(6) . . ? O6 C21 Er1 58.1(3) . 2_754 ? O7 C21 Er1 61.8(3) . 2_754 ? C15 C21 Er1 171.2(5) . 2_754 ? O8 C28 O9 125.3(6) . . ? O8 C28 C25 117.9(6) . . ? O9 C28 C25 116.8(6) . . ? C28 O8 Er2 172.1(5) . . ? O13 C42 O14 124.2(6) . . ? O13 C42 C39 119.4(6) . . ? O14 C42 C39 116.3(6) . . ? C12 C11 C10 119.8(6) . . ? C12 C11 C14 120.0(6) . . ? C10 C11 C14 120.3(6) . . ? O2 C7 O1 123.0(6) . . ? O2 C7 C1 119.4(6) . . ? O1 C7 C1 117.6(6) . . ? C42 O13 Er2 134.3(4) . 4_566 ? C28 O9 Er1 137.1(4) . . ? C45 O16 Er2 139.1(5) . . ? C24 C25 C26 119.9(6) . . ? C24 C25 C28 120.2(6) . . ? C26 C25 C28 119.9(6) . . ? C38 C39 C40 119.5(6) . . ? C38 C39 C42 119.9(6) . . ? C40 C39 C42 120.4(6) . . ? C39 C40 C41 119.9(7) . . ? C35 O11 Er2 88.1(4) . . ? C7 O2 Er1 152.2(5) . 4_565 ? C18 O10 C22 119.7(6) . . ? C45 N2 C44 110.9(6) . . ? C4 O5 C8 115.9(6) . . ? O16 C45 N1 125.6(7) . . ? O16 C45 N2 123.9(6) . . ? N1 C45 N2 110.4(6) . . ? O11 C35 O12 119.5(6) . . ? O11 C35 C29 121.7(6) . . ? O12 C35 C29 118.4(6) . . ? O11 C35 Er2 64.1(3) . . ? O12 C35 Er2 59.6(3) . . ? C29 C35 Er2 153.6(5) . . ? C45 N1 C43 112.0(6) . . ? C16 C15 C20 117.4(7) . . ? C16 C15 C21 119.0(7) . . ? C20 C15 C21 123.5(6) . . ? C32 C33 C34 119.4(7) . . ? C2 C1 C6 118.8(6) . . ? C2 C1 C7 121.1(6) . . ? C6 C1 C7 120.1(6) . . ? C1 C2 C3 120.8(6) . . ? C29 C34 C33 121.7(7) . . ? C23 C22 C27 121.5(6) . . ? C23 C22 O10 117.2(7) . . ? C27 C22 O10 121.2(6) . . ? C22 C27 C26 118.4(6) . . ? C25 C24 C23 119.7(6) . . ? C34 C29 C30 119.0(6) . . ? C34 C29 C35 119.4(6) . . ? C30 C29 C35 121.3(6) . . ? C32 O15 C36 119.5(6) . . ? C27 C26 C25 120.8(7) . . ? C39 C38 C37 120.0(7) . . ? C19 C20 C15 120.8(7) . . ? C11 C12 C13 121.0(7) . . ? C4 C3 C2 119.9(7) . . ? C36 C41 C40 119.3(7) . . ? C22 C23 C24 119.7(7) . . ? C11 C10 C9 119.6(8) . . ? C37 C36 C41 121.6(7) . . ? C37 C36 O15 118.2(8) . . ? C41 C36 O15 119.8(8) . . ? C8 C13 C12 118.6(8) . . ? C31 C30 C29 119.8(7) . . ? C17 C18 C19 120.1(7) . . ? C17 C18 O10 121.9(7) . . ? C19 C18 O10 118.0(7) . . ? C1 C6 C5 120.9(7) . . ? C3 C4 C5 120.3(7) . . ? C3 C4 O5 117.0(7) . . ? C5 C4 O5 122.4(7) . . ? C33 C32 O15 122.9(6) . . ? C33 C32 C31 119.8(7) . . ? O15 C32 C31 117.1(7) . . ? C20 C19 C18 120.8(7) . . ? N2 C44 C43 103.1(7) . . ? C13 C8 C9 121.7(8) . . ? C13 C8 O5 117.1(7) . . ? C9 C8 O5 121.1(8) . . ? C36 C37 C38 119.5(7) . . ? C30 C31 C32 120.3(8) . . ? N1 C43 C44 103.5(7) . . ? C4 C5 C6 119.2(8) . . ? C8 C9 C10 119.3(8) . . ? C15 C16 C17 122.4(9) . . ? C18 C17 C16 118.4(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.255 _refine_diff_density_min -1.229 _refine_diff_density_rms 0.177 data_2 _database_code_depnum_ccdc_archive 'CCDC 894563' #TrackingRef 'cec.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H32 N2 O17 Yb2' _chemical_formula_weight 1218.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.0603(5) _cell_length_b 27.6878(11) _cell_length_c 9.9639(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.019(4) _cell_angle_gamma 90.00 _cell_volume 4406.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5247 _cell_measurement_theta_min 2.5229 _cell_measurement_theta_max 25 _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 4.297 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.50974 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 20610 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.1023 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7746 _reflns_number_gt 6544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0500P)^2^+6.5578P] 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 7746 _refine_ls_number_parameters 590 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1098 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.055536(17) 0.470769(11) 0.22406(3) 0.02054(10) Uani 1 1 d . . . Yb2 Yb 0.360232(17) 0.485363(11) 0.35548(3) 0.02201(11) Uani 1 1 d . . . C45 C 0.2497(5) 0.5276(4) 0.8654(8) 0.054(3) Uani 1 1 d . . . H45A H 0.2475 0.5008 0.9277 0.064 Uiso 1 1 calc R . . H45B H 0.2148 0.5537 0.8925 0.064 Uiso 1 1 calc R . . O1 O 0.1532(3) 0.41951(19) 0.3080(5) 0.0305(12) Uani 1 1 d . . . O14 O 0.5643(3) 0.05275(18) 0.1158(5) 0.0314(12) Uani 1 1 d . . . O3 O 0.0542(3) 0.01837(19) 0.3313(5) 0.0309(12) Uani 1 1 d . . . O2 O 0.2908(3) 0.41529(18) 0.3249(5) 0.0313(12) Uani 1 1 d . . . C43 C 0.2839(4) 0.5180(3) 0.6463(7) 0.0239(16) Uani 1 1 d . . . C28 C 0.0580(4) 0.9055(3) 0.1919(7) 0.0223(16) Uani 1 1 d . . . C7 C 0.2189(4) 0.3966(2) 0.2953(6) 0.0192(15) Uani 1 1 d . . . C14 C 0.0817(4) 0.0545(3) 0.3968(7) 0.0213(15) Uani 1 1 d . . . C12 C 0.1007(5) 0.0965(3) 0.1804(7) 0.0307(18) Uani 1 1 d . . . H12A H 0.0710 0.0717 0.1339 0.037 Uiso 1 1 calc R . . C21 C 0.1996(4) 0.5536(3) 0.1859(6) 0.0198(15) Uani 1 1 d . . . O7 O 0.2605(3) 0.53010(19) 0.2391(5) 0.0313(12) Uani 1 1 d . . . C18 C 0.2316(5) 0.7006(3) 0.0846(7) 0.0280(17) Uani 1 1 d . . . C15 C 0.2107(4) 0.6053(2) 0.1544(6) 0.0188(14) Uani 1 1 d . . . O1W O 0.1037(3) 0.5092(2) 0.4288(5) 0.0353(14) Uani 1 1 d . . . H1WB H 0.1462 0.4952 0.4866 0.042 Uiso 1 1 calc R . . H9C H 0.0803 0.5384 0.4518 0.042 Uiso 1 1 calc R . . O4 O 0.0847(3) 0.0579(2) 0.5216(5) 0.0391(14) Uani 1 1 d . . . C35 C 0.4376(4) 0.4360(3) 0.1670(7) 0.0251(16) Uani 1 1 d . . . C11 C 0.1145(4) 0.0951(3) 0.3200(6) 0.0211(15) Uani 1 1 d . . . C25 C 0.1093(4) 0.8650(3) 0.1480(7) 0.0262(16) Uani 1 1 d . . . C8 C 0.1743(6) 0.1713(3) 0.1776(7) 0.044(2) Uani 1 1 d . . . O5 O 0.2055(5) 0.2066(2) 0.1011(6) 0.073(2) Uani 1 1 d . . . O10 O 0.2444(3) 0.7467(2) 0.0356(5) 0.0440(15) Uani 1 1 d . . . C39 C 0.4958(4) 0.1246(3) 0.0437(6) 0.0227(15) Uani 1 1 d . . . C16 C 0.1414(4) 0.6341(3) 0.1200(7) 0.0270(17) Uani 1 1 d . . . H16A H 0.0880 0.6212 0.1199 0.032 Uiso 1 1 calc R . . C29 C 0.4575(4) 0.3919(3) 0.0919(6) 0.0215(15) Uani 1 1 d . . . C1 C 0.2148(4) 0.3458(3) 0.2468(6) 0.0215(15) Uani 1 1 d . . . C13 C 0.1306(5) 0.1340(3) 0.1109(7) 0.041(2) Uani 1 1 d . . . H13A H 0.1214 0.1344 0.0172 0.049 Uiso 1 1 calc R . . C20 C 0.2896(4) 0.6249(3) 0.1557(7) 0.0302(17) Uani 1 1 d . . . H20A H 0.3365 0.6060 0.1811 0.036 Uiso 1 1 calc R . . N1 N 0.3491(4) 0.5376(3) 0.7158(7) 0.049(2) Uani 1 1 d . . . H1A H 0.3938 0.5458 0.6812 0.059 Uiso 1 1 calc R . . C38 C 0.4211(4) 0.1505(3) 0.0187(7) 0.0297(17) Uani 1 1 d . . . H38A H 0.3707 0.1353 0.0302 0.036 Uiso 1 1 calc R . . C2 C 0.2844(4) 0.3229(3) 0.2125(7) 0.0293(17) Uani 1 1 d . . . H2A H 0.3355 0.3390 0.2216 0.035 Uiso 1 1 calc R . . C19 C 0.2993(4) 0.6722(3) 0.1195(8) 0.0321(18) Uani 1 1 d . . . H19A H 0.3529 0.6850 0.1189 0.039 Uiso 1 1 calc R . . O15 O 0.4957(4) 0.2640(2) -0.1068(5) 0.0553(18) Uani 1 1 d . . . C22 C 0.1981(5) 0.7854(3) 0.0749(8) 0.0328(18) Uani 1 1 d . . . C41 C 0.5711(5) 0.1949(3) -0.0137(8) 0.042(2) Uani 1 1 d . . . H41A H 0.6214 0.2104 -0.0239 0.050 Uiso 1 1 calc R . . C30 C 0.5007(4) 0.3555(3) 0.1584(7) 0.0290(17) Uani 1 1 d . . . H30A H 0.5232 0.3602 0.2473 0.035 Uiso 1 1 calc R . . C37 C 0.4208(5) 0.1978(3) -0.0227(7) 0.0350(19) Uani 1 1 d . . . H37A H 0.3710 0.2151 -0.0373 0.042 Uiso 1 1 calc R . . N2 N 0.2248(4) 0.5127(3) 0.7265(6) 0.052(2) Uani 1 1 d . . . H2B H 0.1760 0.5014 0.6998 0.062 Uiso 1 1 calc R . . C31 C 0.5121(5) 0.3117(3) 0.0979(7) 0.0330(18) Uani 1 1 d . . . H31A H 0.5397 0.2866 0.1464 0.040 Uiso 1 1 calc R . . C27 C 0.1788(7) 0.7900(3) 0.2047(8) 0.063(3) Uani 1 1 d . . . H27A H 0.1955 0.7665 0.2686 0.076 Uiso 1 1 calc R . . C17 C 0.1511(5) 0.6821(3) 0.0859(7) 0.0334(18) Uani 1 1 d . . . H17A H 0.1046 0.7016 0.0641 0.040 Uiso 1 1 calc R . . C3 C 0.2806(6) 0.2766(3) 0.1651(8) 0.042(2) Uani 1 1 d . . . H3A H 0.3287 0.2616 0.1412 0.050 Uiso 1 1 calc R . . C36 C 0.4964(6) 0.2189(3) -0.0419(7) 0.037(2) Uani 1 1 d . . . C24 C 0.1315(5) 0.8602(3) 0.0196(7) 0.041(2) Uani 1 1 d . . . H24A H 0.1160 0.8839 -0.0441 0.049 Uiso 1 1 calc R . . O12 O 0.3804(3) 0.4655(2) 0.1218(5) 0.0393(14) Uani 1 1 d . . . C26 C 0.1345(7) 0.8297(3) 0.2397(8) 0.061(3) Uani 1 1 d . . . H26A H 0.1212 0.8326 0.3279 0.073 Uiso 1 1 calc R . . C33 C 0.4391(6) 0.3423(3) -0.1047(8) 0.046(2) Uani 1 1 d . . . H33A H 0.4187 0.3380 -0.1948 0.055 Uiso 1 1 calc R . . C42 C 0.4956(4) 0.0717(3) 0.0712(6) 0.0223(15) Uani 1 1 d . . . C23 C 0.1756(5) 0.8213(3) -0.0165(8) 0.045(2) Uani 1 1 d . . . H23A H 0.1908 0.8191 -0.1039 0.053 Uiso 1 1 calc R . . C6 C 0.1398(5) 0.3214(3) 0.2318(8) 0.038(2) Uani 1 1 d . . . H6A H 0.0912 0.3365 0.2535 0.045 Uiso 1 1 calc R . . C5 C 0.1368(6) 0.2744(3) 0.1842(9) 0.052(3) Uani 1 1 d . . . H5A H 0.0862 0.2577 0.1740 0.062 Uiso 1 1 calc R . . C4 C 0.2076(6) 0.2528(3) 0.1528(8) 0.045(2) Uani 1 1 d . . . C10 C 0.1572(6) 0.1330(3) 0.3845(8) 0.053(3) Uani 1 1 d . . . H10A H 0.1648 0.1334 0.4783 0.063 Uiso 1 1 calc R . . C32 C 0.4822(5) 0.3055(3) -0.0352(7) 0.0339(19) Uani 1 1 d . . . O6 O 0.1285(3) 0.5357(2) 0.1595(5) 0.0369(13) Uani 1 1 d . . . C40 C 0.5708(5) 0.1480(3) 0.0294(7) 0.0322(18) Uani 1 1 d . . . H40A H 0.6212 0.1317 0.0493 0.039 Uiso 1 1 calc R . . C44 C 0.3378(5) 0.5440(4) 0.8567(8) 0.055(3) Uani 1 1 d . . . H44A H 0.3448 0.5776 0.8831 0.066 Uiso 1 1 calc R . . H44B H 0.3772 0.5245 0.9137 0.066 Uiso 1 1 calc R . . C34 C 0.4263(6) 0.3854(3) -0.0412(8) 0.046(2) Uani 1 1 d . . . H34A H 0.3967 0.4102 -0.0879 0.055 Uiso 1 1 calc R . . C9 C 0.1888(6) 0.1702(4) 0.3151(10) 0.059(3) Uiso 1 1 d . . . H1WA H 0.2199 0.1945 0.3611 0.071 Uiso 1 1 calc R . . O8 O 0.0327(3) 0.93847(18) 0.1123(4) 0.0262(11) Uani 1 1 d . . . O13 O 0.4291(3) 0.04815(19) 0.0473(5) 0.0268(11) Uani 1 1 d . . . O16 O 0.2758(3) 0.5086(2) 0.5226(5) 0.0328(13) Uani 1 1 d . . . O9 O 0.0376(3) 0.90518(19) 0.3101(4) 0.0293(12) Uani 1 1 d . . . O11 O 0.4741(3) 0.44271(18) 0.2847(4) 0.0257(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.02342(17) 0.01734(19) 0.02132(17) -0.00172(12) 0.00448(12) 0.00227(13) Yb2 0.02494(17) 0.01505(19) 0.02605(18) -0.00339(13) 0.00279(13) 0.00106(13) C45 0.041(5) 0.086(9) 0.036(5) 0.012(5) 0.007(4) -0.009(5) O1 0.030(3) 0.028(3) 0.032(3) 0.000(2) -0.002(2) 0.007(2) O14 0.032(3) 0.011(3) 0.049(3) 0.005(2) -0.005(2) 0.004(2) O3 0.026(2) 0.024(3) 0.043(3) 0.005(2) 0.005(2) -0.009(2) O2 0.031(3) 0.016(3) 0.046(3) -0.004(2) -0.002(2) -0.007(2) C43 0.021(3) 0.025(4) 0.026(4) -0.006(3) 0.004(3) 0.006(3) C28 0.020(3) 0.025(4) 0.021(4) 0.005(3) 0.000(3) -0.004(3) C7 0.028(4) 0.011(4) 0.018(3) 0.004(3) -0.001(3) 0.002(3) C14 0.014(3) 0.020(4) 0.031(4) 0.004(3) 0.008(3) 0.003(3) C12 0.054(5) 0.019(4) 0.019(4) -0.005(3) 0.002(3) -0.011(4) C21 0.030(4) 0.020(4) 0.010(3) -0.001(3) 0.007(3) 0.004(3) O7 0.034(3) 0.020(3) 0.038(3) 0.006(2) -0.003(2) 0.009(2) C18 0.050(5) 0.012(4) 0.023(4) 0.000(3) 0.011(3) 0.005(4) C15 0.029(3) 0.013(4) 0.014(3) 0.003(3) 0.000(3) -0.002(3) O1W 0.031(3) 0.046(4) 0.028(3) -0.019(3) 0.001(2) 0.009(3) O4 0.053(3) 0.039(4) 0.027(3) 0.016(2) 0.017(2) 0.001(3) C35 0.038(4) 0.015(4) 0.025(4) 0.001(3) 0.016(3) 0.002(3) C11 0.028(3) 0.015(4) 0.021(4) -0.001(3) 0.006(3) -0.004(3) C25 0.035(4) 0.015(4) 0.029(4) 0.002(3) 0.006(3) 0.006(3) C8 0.099(7) 0.018(5) 0.020(4) -0.003(3) 0.028(4) -0.017(5) O5 0.162(7) 0.020(4) 0.047(4) -0.011(3) 0.058(4) -0.035(4) O10 0.069(4) 0.017(3) 0.051(4) 0.005(3) 0.035(3) 0.011(3) C39 0.034(4) 0.012(4) 0.021(4) -0.004(3) -0.003(3) 0.002(3) C16 0.024(3) 0.031(5) 0.025(4) 0.005(3) -0.004(3) 0.006(3) C29 0.027(3) 0.017(4) 0.023(4) -0.004(3) 0.008(3) -0.002(3) C1 0.028(3) 0.018(4) 0.019(3) 0.004(3) 0.003(3) -0.003(3) C13 0.085(6) 0.022(5) 0.016(4) 0.000(3) 0.006(4) -0.012(4) C20 0.025(4) 0.024(5) 0.041(4) 0.003(4) 0.003(3) 0.003(3) N1 0.031(3) 0.082(6) 0.036(4) -0.024(4) 0.012(3) -0.021(4) C38 0.034(4) 0.030(5) 0.025(4) -0.007(3) 0.003(3) 0.002(4) C2 0.032(4) 0.019(4) 0.038(4) -0.003(3) 0.006(3) -0.001(3) C19 0.028(4) 0.019(4) 0.050(5) -0.002(4) 0.008(3) -0.002(3) O15 0.131(6) 0.010(3) 0.025(3) -0.002(2) 0.014(3) 0.009(3) C22 0.050(5) 0.011(4) 0.040(5) -0.001(3) 0.017(4) 0.005(4) C41 0.060(5) 0.016(5) 0.051(5) -0.005(4) 0.005(4) -0.014(4) C30 0.041(4) 0.028(5) 0.018(4) -0.005(3) -0.001(3) 0.005(4) C37 0.053(5) 0.024(5) 0.027(4) -0.008(3) 0.000(4) 0.016(4) N2 0.034(4) 0.096(7) 0.026(4) -0.013(4) 0.009(3) -0.035(4) C31 0.045(4) 0.020(4) 0.033(4) 0.000(3) 0.001(3) 0.009(4) C27 0.126(9) 0.035(6) 0.030(5) 0.015(4) 0.016(5) 0.044(6) C17 0.043(4) 0.027(5) 0.031(4) 0.004(3) 0.005(3) 0.012(4) C3 0.070(6) 0.016(5) 0.044(5) 0.000(4) 0.029(4) 0.002(4) C36 0.086(6) 0.010(4) 0.016(4) -0.005(3) 0.001(4) 0.005(4) C24 0.075(6) 0.022(5) 0.027(4) 0.014(3) 0.014(4) 0.021(4) O12 0.061(3) 0.031(3) 0.026(3) 0.000(2) 0.004(3) 0.023(3) C26 0.123(8) 0.039(6) 0.024(4) 0.008(4) 0.026(5) 0.045(6) C33 0.086(6) 0.028(5) 0.021(4) -0.006(4) -0.002(4) 0.016(5) C42 0.032(4) 0.016(4) 0.019(3) -0.005(3) 0.004(3) 0.002(3) C23 0.074(6) 0.035(5) 0.028(4) 0.012(4) 0.022(4) 0.019(5) C6 0.035(4) 0.036(5) 0.044(5) -0.004(4) 0.010(4) -0.013(4) C5 0.062(6) 0.044(6) 0.051(6) -0.009(5) 0.012(5) -0.036(5) C4 0.095(7) 0.018(5) 0.027(4) -0.003(3) 0.029(4) -0.014(5) C10 0.100(7) 0.042(6) 0.017(4) -0.006(4) 0.011(4) -0.036(6) C32 0.063(5) 0.015(4) 0.025(4) -0.004(3) 0.014(4) 0.000(4) O6 0.036(3) 0.028(3) 0.045(3) 0.014(3) -0.001(2) -0.012(3) C40 0.036(4) 0.017(4) 0.042(5) 0.002(3) -0.005(3) -0.005(3) C44 0.052(5) 0.082(8) 0.028(5) -0.009(5) -0.004(4) -0.017(6) C34 0.078(6) 0.030(5) 0.028(4) 0.008(4) 0.005(4) 0.016(5) O8 0.031(2) 0.025(3) 0.023(3) 0.010(2) 0.008(2) 0.006(2) O13 0.028(2) 0.025(3) 0.027(3) 0.000(2) 0.002(2) -0.004(2) O16 0.023(2) 0.052(4) 0.024(3) -0.015(2) 0.003(2) 0.004(2) O9 0.044(3) 0.029(3) 0.016(2) 0.008(2) 0.011(2) 0.019(3) O11 0.023(2) 0.030(3) 0.025(3) -0.008(2) 0.006(2) 0.000(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 Yb1 O1 2.214(5) . ? Yb1 O3 2.224(5) 2 ? Yb1 O4 2.261(5) 4_565 ? Yb1 O6 2.275(5) . ? Yb1 O9 2.355(5) 2_545 ? Yb1 O1W 2.358(5) . ? Yb1 O8 2.440(4) 2_545 ? Yb1 C28 2.759(7) 2_545 ? Yb2 O14 2.227(5) 2_655 ? Yb2 O2 2.243(5) . ? Yb2 O7 2.248(5) . ? Yb2 O13 2.301(5) 4_566 ? Yb2 O16 2.344(4) . ? Yb2 O11 2.347(4) . ? Yb2 O12 2.446(5) . ? Yb2 C35 2.725(7) . ? C45 N2 1.459(11) . ? C45 C44 1.498(11) . ? O1 C7 1.248(7) . ? O14 C42 1.260(8) . ? O14 Yb2 2.227(5) 2_645 ? O3 C14 1.250(8) . ? O3 Yb1 2.224(5) 2_545 ? O2 C7 1.272(7) . ? C43 O16 1.254(8) . ? C43 N1 1.311(9) . ? C43 N2 1.311(9) . ? C28 O8 1.249(8) . ? C28 O9 1.255(8) . ? C28 C25 1.484(10) . ? C28 Yb1 2.759(7) 2 ? C7 C1 1.487(10) . ? C14 O4 1.243(8) . ? C14 C11 1.486(9) . ? C12 C13 1.362(10) . ? C12 C11 1.386(9) . ? C21 O6 1.247(8) . ? C21 O7 1.246(8) . ? C21 C15 1.481(9) . ? C18 C19 1.357(10) . ? C18 O10 1.390(9) . ? C18 C17 1.392(10) . ? C15 C20 1.378(9) . ? C15 C16 1.382(9) . ? O4 Yb1 2.261(5) 4_566 ? C35 O11 1.269(8) . ? C35 O12 1.276(8) . ? C35 C29 1.484(9) . ? C11 C10 1.377(10) . ? C25 C26 1.371(11) . ? C25 C24 1.371(10) . ? C8 C9 1.366(11) . ? C8 O5 1.367(9) . ? C8 C13 1.381(11) . ? O5 C4 1.377(10) . ? O10 C22 1.382(9) . ? C39 C40 1.388(10) . ? C39 C38 1.396(10) . ? C39 C42 1.489(9) . ? C16 C17 1.384(10) . ? C29 C30 1.357(10) . ? C29 C34 1.379(10) . ? C1 C2 1.359(9) . ? C1 C6 1.375(9) . ? C20 C19 1.373(10) . ? N1 C44 1.445(10) . ? C38 C37 1.374(11) . ? C2 C3 1.366(11) . ? O15 C32 1.382(9) . ? O15 C36 1.403(9) . ? C22 C27 1.367(11) . ? C22 C23 1.372(11) . ? C41 C40 1.367(11) . ? C41 C36 1.375(11) . ? C30 C31 1.375(10) . ? C37 C36 1.380(11) . ? C31 C32 1.373(10) . ? C27 C26 1.374(11) . ? C3 C4 1.340(12) . ? C24 C23 1.357(11) . ? C33 C32 1.377(11) . ? C33 C34 1.378(11) . ? C42 O13 1.254(8) . ? C6 C5 1.386(12) . ? C5 C4 1.350(12) . ? C10 C9 1.366(12) . ? O8 Yb1 2.440(4) 2 ? O13 Yb2 2.301(5) 4_565 ? O9 Yb1 2.355(5) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Yb1 O3 170.31(18) . 2 ? O1 Yb1 O4 84.69(19) . 4_565 ? O3 Yb1 O4 102.67(19) 2 4_565 ? O1 Yb1 O6 104.36(18) . . ? O3 Yb1 O6 83.09(19) 2 . ? O4 Yb1 O6 82.2(2) 4_565 . ? O1 Yb1 O9 88.54(18) . 2_545 ? O3 Yb1 O9 86.91(18) 2 2_545 ? O4 Yb1 O9 77.81(17) 4_565 2_545 ? O6 Yb1 O9 155.05(17) . 2_545 ? O1 Yb1 O1W 78.87(18) . . ? O3 Yb1 O1W 97.30(18) 2 . ? O4 Yb1 O1W 148.18(18) 4_565 . ? O6 Yb1 O1W 75.88(19) . . ? O9 Yb1 O1W 128.23(17) 2_545 . ? O1 Yb1 O8 87.19(17) . 2_545 ? O3 Yb1 O8 83.22(18) 2 2_545 ? O4 Yb1 O8 131.06(18) 4_565 2_545 ? O6 Yb1 O8 146.20(19) . 2_545 ? O9 Yb1 O8 53.78(15) 2_545 2_545 ? O1W Yb1 O8 75.42(17) . 2_545 ? O1 Yb1 C28 85.98(19) . 2_545 ? O3 Yb1 C28 86.09(19) 2 2_545 ? O4 Yb1 C28 104.3(2) 4_565 2_545 ? O6 Yb1 C28 168.4(2) . 2_545 ? O9 Yb1 C28 26.95(17) 2_545 2_545 ? O1W Yb1 C28 101.56(19) . 2_545 ? O8 Yb1 C28 26.91(17) 2_545 2_545 ? O14 Yb2 O2 176.81(17) 2_655 . ? O14 Yb2 O7 87.33(18) 2_655 . ? O2 Yb2 O7 95.11(18) . . ? O14 Yb2 O13 91.35(18) 2_655 4_566 ? O2 Yb2 O13 87.30(18) . 4_566 ? O7 Yb2 O13 154.80(18) . 4_566 ? O14 Yb2 O16 91.54(19) 2_655 . ? O2 Yb2 O16 90.99(18) . . ? O7 Yb2 O16 77.38(18) . . ? O13 Yb2 O16 77.50(17) 4_566 . ? O14 Yb2 O11 91.66(17) 2_655 . ? O2 Yb2 O11 85.19(17) . . ? O7 Yb2 O11 131.15(17) . . ? O13 Yb2 O11 74.04(16) 4_566 . ? O16 Yb2 O11 151.42(17) . . ? O14 Yb2 O12 100.68(19) 2_655 . ? O2 Yb2 O12 77.89(19) . . ? O7 Yb2 O12 77.96(18) . . ? O13 Yb2 O12 126.87(17) 4_566 . ? O16 Yb2 O12 151.84(17) . . ? O11 Yb2 O12 54.26(16) . . ? O14 Yb2 C35 103.1(2) 2_655 . ? O2 Yb2 C35 74.3(2) . . ? O7 Yb2 C35 105.8(2) . . ? O13 Yb2 C35 98.99(19) 4_566 . ? O16 Yb2 C35 165.1(2) . . ? O11 Yb2 C35 27.70(18) . . ? O12 Yb2 C35 27.90(18) . . ? N2 C45 C44 101.4(6) . . ? C7 O1 Yb1 149.3(4) . . ? C42 O14 Yb2 147.1(5) . 2_645 ? C14 O3 Yb1 146.3(4) . 2_545 ? C7 O2 Yb2 144.1(5) . . ? O16 C43 N1 126.8(6) . . ? O16 C43 N2 124.8(6) . . ? N1 C43 N2 108.2(6) . . ? O8 C28 O9 120.2(7) . . ? O8 C28 C25 121.2(6) . . ? O9 C28 C25 118.6(6) . . ? O8 C28 Yb1 62.2(4) . 2 ? O9 C28 Yb1 58.3(3) . 2 ? C25 C28 Yb1 171.6(5) . 2 ? O1 C7 O2 121.7(6) . . ? O1 C7 C1 120.4(6) . . ? O2 C7 C1 117.9(6) . . ? O4 C14 O3 123.8(7) . . ? O4 C14 C11 118.7(7) . . ? O3 C14 C11 117.4(6) . . ? C13 C12 C11 120.3(7) . . ? O6 C21 O7 122.9(7) . . ? O6 C21 C15 117.8(6) . . ? O7 C21 C15 119.2(6) . . ? C21 O7 Yb2 172.9(5) . . ? C19 C18 O10 118.6(7) . . ? C19 C18 C17 120.3(7) . . ? O10 C18 C17 120.9(7) . . ? C20 C15 C16 119.4(7) . . ? C20 C15 C21 120.6(6) . . ? C16 C15 C21 120.0(6) . . ? C14 O4 Yb1 151.2(5) . 4_566 ? O11 C35 O12 118.6(6) . . ? O11 C35 C29 118.9(6) . . ? O12 C35 C29 122.3(6) . . ? O11 C35 Yb2 59.3(3) . . ? O12 C35 Yb2 63.8(3) . . ? C29 C35 Yb2 153.8(5) . . ? C10 C11 C12 117.8(7) . . ? C10 C11 C14 121.5(6) . . ? C12 C11 C14 120.7(6) . . ? C26 C25 C24 117.7(7) . . ? C26 C25 C28 118.5(6) . . ? C24 C25 C28 123.8(7) . . ? C9 C8 O5 122.8(8) . . ? C9 C8 C13 119.4(8) . . ? O5 C8 C13 117.7(7) . . ? C8 O5 C4 116.8(6) . . ? C22 O10 C18 120.5(6) . . ? C40 C39 C38 118.7(7) . . ? C40 C39 C42 119.8(6) . . ? C38 C39 C42 121.2(6) . . ? C15 C16 C17 120.4(7) . . ? C30 C29 C34 119.2(7) . . ? C30 C29 C35 119.5(6) . . ? C34 C29 C35 121.1(7) . . ? C2 C1 C6 118.7(7) . . ? C2 C1 C7 120.9(6) . . ? C6 C1 C7 120.4(6) . . ? C12 C13 C8 120.9(7) . . ? C19 C20 C15 120.2(7) . . ? C43 N1 C44 112.9(6) . . ? C37 C38 C39 121.3(7) . . ? C1 C2 C3 121.0(7) . . ? C18 C19 C20 120.7(7) . . ? C32 O15 C36 119.7(6) . . ? C27 C22 C23 119.4(7) . . ? C27 C22 O10 121.5(7) . . ? C23 C22 O10 119.0(7) . . ? C40 C41 C36 119.5(8) . . ? C29 C30 C31 121.8(7) . . ? C38 C37 C36 118.1(7) . . ? C43 N2 C45 113.8(6) . . ? C30 C31 C32 119.0(7) . . ? C22 C27 C26 119.3(8) . . ? C16 C17 C18 119.0(7) . . ? C4 C3 C2 120.0(8) . . ? C41 C36 C37 121.9(7) . . ? C41 C36 O15 119.3(8) . . ? C37 C36 O15 118.4(8) . . ? C23 C24 C25 121.3(7) . . ? C35 O12 Yb2 88.3(4) . . ? C25 C26 C27 121.8(8) . . ? C32 C33 C34 120.1(7) . . ? O13 C42 O14 123.1(7) . . ? O13 C42 C39 119.7(6) . . ? O14 C42 C39 117.2(6) . . ? C24 C23 C22 120.5(7) . . ? C1 C6 C5 119.7(8) . . ? C4 C5 C6 119.8(8) . . ? C3 C4 C5 120.8(8) . . ? C3 C4 O5 118.5(8) . . ? C5 C4 O5 120.7(9) . . ? C9 C10 C11 122.1(8) . . ? C33 C32 C31 120.0(7) . . ? C33 C32 O15 117.0(7) . . ? C31 C32 O15 123.0(7) . . ? C21 O6 Yb1 137.8(5) . . ? C41 C40 C39 120.5(7) . . ? N1 C44 C45 103.6(6) . . ? C29 C34 C33 119.9(8) . . ? C10 C9 C8 119.4(9) . . ? C28 O8 Yb1 90.9(4) . 2 ? C42 O13 Yb2 133.9(4) . 4_565 ? C43 O16 Yb2 138.4(4) . . ? C28 O9 Yb1 94.8(4) . 2 ? C35 O11 Yb2 93.0(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.425 _refine_diff_density_min -1.171 _refine_diff_density_rms 0.169 data_3 _database_code_depnum_ccdc_archive 'CCDC 894564' #TrackingRef 'cec.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H32 Ho2 N2 O17' _chemical_formula_weight 1202.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.0587(4) _cell_length_b 27.6658(6) _cell_length_c 9.9524(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.044(2) _cell_angle_gamma 90.00 _cell_volume 4397.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6202 _cell_measurement_theta_min 2.4139 _cell_measurement_theta_max 25 _exptl_crystal_description sheet _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 3.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.39257 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 19450 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0978 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.4139 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7700 _reflns_number_gt 6370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0557P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7700 _refine_ls_number_parameters 590 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho2 Ho 0.055572(18) 0.529236(10) -0.77593(3) 0.02026(11) Uani 1 1 d . . . Ho1 Ho 0.360211(19) 0.514606(11) -0.64442(3) 0.02176(11) Uani 1 1 d . . . O9 O 0.1531(3) 0.91967(18) -1.1918(5) 0.0371(13) Uani 1 1 d . . . O7 O 0.0537(3) 0.51789(17) -1.1695(5) 0.0343(12) Uani 1 1 d . . . O11 O -0.0375(3) 0.59469(17) -0.8095(5) 0.0351(13) Uani 1 1 d . . . O1W O 0.1036(3) 0.49045(18) -0.5714(5) 0.0376(13) Uani 1 1 d . . . H10B H 0.0750 0.4638 -0.5424 0.045 Uiso 1 1 calc R . . H10C H 0.1512 0.5018 -0.5196 0.045 Uiso 1 1 calc R . . O14 O -0.2612(3) 0.96974(16) -0.7392(5) 0.0376(13) Uani 1 1 d . . . O1 O 0.4357(3) 0.44693(16) -0.6160(5) 0.0371(13) Uani 1 1 d . . . O16 O 0.2760(3) 0.49153(18) -0.4780(5) 0.0355(13) Uani 1 1 d . . . O6 O 0.0846(3) 0.55746(19) -0.9782(5) 0.0447(14) Uani 1 1 d . . . O13 O -0.1281(3) 0.96453(18) -0.6590(5) 0.0398(13) Uani 1 1 d . . . C35 C -0.0582(4) 0.5951(2) -0.6925(7) 0.0279(16) Uani 1 1 d . . . O15 O -0.2452(3) 0.75326(17) -0.5358(6) 0.0483(15) Uani 1 1 d . . . C36 C -0.2307(5) 0.7992(2) -0.5836(7) 0.0340(18) Uani 1 1 d . . . C32 C -0.1981(5) 0.7146(3) -0.5765(8) 0.043(2) Uani 1 1 d . . . O8 O 0.2903(3) 0.91501(17) -1.1751(5) 0.0383(13) Uani 1 1 d . . . C15 C 0.1137(4) 0.5947(2) -1.1808(7) 0.0244(16) Uani 1 1 d . . . C17 C 0.1308(5) 0.6338(3) -1.3903(8) 0.044(2) Uani 1 1 d . . . H17A H 0.1221 0.6342 -1.4842 0.053 Uiso 1 1 calc R . . O10 O 0.2058(5) 0.70604(19) -1.3991(6) 0.077(2) Uani 1 1 d . . . C29 C -0.1091(4) 0.6352(2) -0.6480(7) 0.0296(17) Uani 1 1 d . . . C16 C 0.1010(5) 0.5966(3) -1.3181(7) 0.0370(19) Uani 1 1 d . . . H16A H 0.0711 0.5719 -1.3645 0.044 Uiso 1 1 calc R . . C25 C 0.2147(4) 0.8460(2) -1.2544(7) 0.0288(17) Uani 1 1 d . . . C42 C -0.1985(5) 0.9465(2) -0.6866(7) 0.0276(16) Uani 1 1 d . . . N1 N 0.2246(4) 0.4871(3) -0.2726(6) 0.057(2) Uani 1 1 d . . . H1A H 0.1755 0.4980 -0.2997 0.068 Uiso 1 1 calc R . . C18 C 0.1735(6) 0.6703(3) -1.3219(8) 0.052(3) Uani 1 1 d . . . N2 N 0.3495(4) 0.4623(3) -0.2846(7) 0.059(2) Uani 1 1 d . . . H2A H 0.3942 0.4538 -0.3190 0.071 Uiso 1 1 calc R . . C21 C 0.0818(4) 0.5539(3) -1.1026(7) 0.0276(16) Uani 1 1 d . . . C14 C 0.5623(4) 0.0633(2) -0.6676(7) 0.0276(16) Uani 1 1 d . . . C43 C 0.2843(4) 0.4819(3) -0.3540(7) 0.0309(17) Uani 1 1 d . . . C39 C -0.2111(4) 0.8943(2) -0.6537(7) 0.0256(16) Uani 1 1 d . . . O5 O 0.5047(4) 0.23566(18) -0.3939(5) 0.0647(19) Uani 1 1 d . . . O4 O 0.6200(3) 0.03485(19) -0.6216(5) 0.0437(14) Uani 1 1 d . . . C6 C 0.5789(4) 0.3496(3) -0.5194(7) 0.0299(17) Uani 1 1 d . . . H6A H 0.6294 0.3646 -0.5314 0.036 Uiso 1 1 calc R . . C4 C 0.5039(6) 0.2802(2) -0.4581(8) 0.042(2) Uani 1 1 d . . . C41 C -0.2995(5) 0.8268(3) -0.6192(8) 0.039(2) Uani 1 1 d . . . H41A H -0.3528 0.8137 -0.6192 0.047 Uiso 1 1 calc R . . C11 C 0.5422(4) 0.1081(2) -0.5919(7) 0.0276(17) Uani 1 1 d . . . C1 C 0.5046(4) 0.3753(2) -0.5434(7) 0.0248(16) Uani 1 1 d . . . C37 C -0.1505(5) 0.8176(3) -0.5849(8) 0.0371(19) Uani 1 1 d . . . H37A H -0.1039 0.7980 -0.5634 0.044 Uiso 1 1 calc R . . C40 C -0.2895(4) 0.8747(2) -0.6557(8) 0.0316(18) Uani 1 1 d . . . H40A H -0.3364 0.8936 -0.6816 0.038 Uiso 1 1 calc R . . C13 C 0.5608(6) 0.1576(3) -0.3934(8) 0.055(3) Uani 1 1 d . . . H13A H 0.5803 0.1617 -0.3028 0.066 Uiso 1 1 calc R . . C28 C 0.2187(4) 0.8967(2) -1.2043(6) 0.0250(16) Uani 1 1 d . . . C38 C -0.1414(4) 0.8656(3) -0.6189(7) 0.0299(17) Uani 1 1 d . . . H38A H -0.0881 0.8788 -0.6184 0.036 Uiso 1 1 calc R . . C3 C 0.4292(6) 0.3047(3) -0.4862(8) 0.049(2) Uani 1 1 d . . . H3A H 0.3786 0.2895 -0.4757 0.059 Uiso 1 1 calc R . . C12 C 0.5743(5) 0.1143(3) -0.4588(8) 0.048(2) Uani 1 1 d . . . H12A H 0.6048 0.0896 -0.4132 0.058 Uiso 1 1 calc R . . C9 C 0.4873(5) 0.1885(3) -0.5979(8) 0.0378(19) Uani 1 1 d . . . H9A H 0.4591 0.2135 -0.6457 0.045 Uiso 1 1 calc R . . C34 C -0.1310(5) 0.6400(3) -0.5210(8) 0.047(2) Uani 1 1 d . . . H34A H -0.1153 0.6161 -0.4576 0.057 Uiso 1 1 calc R . . C27 C 0.2821(5) 0.7762(3) -1.3346(8) 0.049(2) Uani 1 1 d . . . H27A H 0.3302 0.7610 -1.3578 0.059 Uiso 1 1 calc R . . C2 C 0.4304(5) 0.3520(3) -0.5302(8) 0.0367(19) Uani 1 1 d . . . H2B H 0.3801 0.3683 -0.5512 0.044 Uiso 1 1 calc R . . C10 C 0.4991(4) 0.1449(2) -0.6593(7) 0.0316(17) Uani 1 1 d . . . H10A H 0.4772 0.1403 -0.7486 0.038 Uiso 1 1 calc R . . C33 C -0.1757(6) 0.6792(3) -0.4829(9) 0.054(3) Uani 1 1 d . . . H33A H -0.1905 0.6817 -0.3953 0.065 Uiso 1 1 calc R . . C24 C 0.1385(5) 0.8215(3) -1.2697(8) 0.045(2) Uani 1 1 d . . . H24A H 0.0897 0.8368 -1.2495 0.054 Uiso 1 1 calc R . . C26 C 0.2847(4) 0.8230(3) -1.2872(7) 0.0360(19) Uani 1 1 d . . . H26A H 0.3356 0.8393 -1.2773 0.043 Uiso 1 1 calc R . . O2 O 0.5717(3) 0.45148(17) -0.5473(5) 0.0314(12) Uani 1 1 d . . . C45 C 0.3376(6) 0.4565(4) -0.1442(8) 0.063(3) Uani 1 1 d . . . H45A H 0.3771 0.4762 -0.0876 0.076 Uiso 1 1 calc R . . H45B H 0.3448 0.4230 -0.1168 0.076 Uiso 1 1 calc R . . O12 O -0.0318(3) 0.56133(16) -0.6119(5) 0.0283(11) Uani 1 1 d . . . O3 O 0.5256(3) 0.05709(16) -0.7853(5) 0.0279(11) Uani 1 1 d . . . C8 C 0.5179(5) 0.1945(2) -0.4650(8) 0.039(2) Uani 1 1 d . . . C5 C 0.5788(5) 0.3023(3) -0.4782(7) 0.041(2) Uani 1 1 d . . . H5A H 0.6288 0.2851 -0.4639 0.050 Uiso 1 1 calc R . . C20 C 0.1565(6) 0.6322(3) -1.1155(8) 0.057(3) Uani 1 1 d . . . H20A H 0.1645 0.6321 -1.0215 0.069 Uiso 1 1 calc R . . C22 C 0.2069(6) 0.7528(3) -1.3465(8) 0.053(3) Uani 1 1 d . . . C19 C 0.1884(6) 0.6703(3) -1.1845(8) 0.067(3) Uani 1 1 d . . . H19A H 0.2189 0.6949 -1.1389 0.081 Uiso 1 1 calc R . . C30 C -0.1339(6) 0.6704(3) -0.7400(8) 0.066(3) Uani 1 1 d . . . H30A H -0.1195 0.6678 -0.8278 0.080 Uiso 1 1 calc R . . C31 C -0.1804(6) 0.7100(3) -0.7049(10) 0.064(3) Uiso 1 1 d . . . H31A H -0.1989 0.7330 -0.7693 0.077 Uiso 1 1 calc R . . C23 C 0.1363(6) 0.7746(3) -1.3150(9) 0.062(3) Uani 1 1 d . . . H23A H 0.0859 0.7577 -1.3240 0.075 Uiso 1 1 calc R . . C44 C 0.2495(5) 0.4728(4) -0.1338(9) 0.068(3) Uani 1 1 d . . . H44A H 0.2149 0.4467 -0.1056 0.082 Uiso 1 1 calc R . . H44B H 0.2476 0.4998 -0.0720 0.082 Uiso 1 1 calc R . . C7 C 0.5058(4) 0.4283(2) -0.5709(7) 0.0261(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho2 0.02315(19) 0.01873(18) 0.01944(18) 0.00175(13) 0.00481(13) -0.00215(13) Ho1 0.02484(19) 0.01636(18) 0.02420(19) 0.00338(13) 0.00312(14) -0.00107(13) O9 0.029(3) 0.038(3) 0.042(3) 0.002(3) -0.005(2) 0.015(2) O7 0.031(3) 0.025(3) 0.047(3) 0.001(2) 0.005(2) -0.011(2) O11 0.048(3) 0.035(3) 0.025(3) 0.010(2) 0.014(2) 0.022(2) O1W 0.035(3) 0.042(3) 0.034(3) 0.015(3) -0.002(2) -0.010(2) O14 0.041(3) 0.022(3) 0.049(4) 0.003(2) -0.001(3) 0.008(2) O1 0.042(3) 0.021(3) 0.047(3) 0.004(2) -0.003(3) 0.006(2) O16 0.027(3) 0.052(3) 0.027(3) 0.019(3) 0.002(2) -0.004(2) O6 0.063(4) 0.043(3) 0.032(3) 0.008(3) 0.026(3) 0.001(3) O13 0.037(3) 0.034(3) 0.048(4) 0.011(3) -0.003(3) -0.014(2) C35 0.030(4) 0.027(4) 0.027(4) 0.003(3) 0.005(3) 0.004(3) O15 0.072(4) 0.017(3) 0.063(4) 0.008(3) 0.036(3) 0.011(3) C36 0.052(5) 0.021(4) 0.031(4) 0.002(3) 0.015(4) 0.003(4) C32 0.070(6) 0.020(4) 0.042(5) 0.005(4) 0.026(4) 0.014(4) O8 0.035(3) 0.028(3) 0.051(4) -0.003(3) 0.001(3) -0.005(2) C15 0.036(4) 0.013(3) 0.025(4) -0.002(3) 0.008(3) -0.008(3) C17 0.089(7) 0.023(4) 0.021(4) -0.003(3) 0.015(4) -0.012(4) O10 0.167(7) 0.024(3) 0.053(4) -0.013(3) 0.065(4) -0.033(4) C29 0.044(4) 0.015(3) 0.032(4) 0.008(3) 0.014(3) 0.004(3) C16 0.056(5) 0.028(4) 0.028(4) -0.005(3) 0.006(4) -0.015(4) C25 0.033(4) 0.026(4) 0.027(4) -0.002(3) 0.005(3) -0.005(3) C42 0.044(5) 0.025(4) 0.015(4) -0.004(3) 0.008(3) 0.004(4) N1 0.039(4) 0.110(7) 0.022(4) 0.008(4) 0.006(3) 0.032(4) C18 0.105(7) 0.021(4) 0.036(5) -0.006(4) 0.036(5) -0.020(5) N2 0.027(4) 0.110(7) 0.042(5) 0.026(4) 0.010(3) 0.022(4) C21 0.019(4) 0.032(4) 0.033(4) 0.003(4) 0.010(3) 0.002(3) C14 0.033(4) 0.025(4) 0.027(4) 0.005(3) 0.010(3) -0.002(3) C43 0.033(4) 0.035(4) 0.024(4) 0.001(3) 0.003(3) -0.003(3) C39 0.033(4) 0.023(4) 0.022(4) 0.004(3) 0.007(3) 0.006(3) O5 0.150(6) 0.017(3) 0.031(3) -0.005(2) 0.024(4) 0.010(3) O4 0.059(4) 0.042(3) 0.029(3) 0.000(3) 0.001(3) 0.022(3) C6 0.033(4) 0.029(4) 0.027(4) -0.006(3) 0.000(3) 0.007(3) C4 0.084(7) 0.014(4) 0.028(5) -0.005(3) 0.004(4) 0.001(4) C41 0.032(4) 0.026(4) 0.060(6) 0.001(4) 0.011(4) -0.004(3) C11 0.042(4) 0.016(3) 0.026(4) 0.002(3) 0.013(3) 0.006(3) C1 0.034(4) 0.016(3) 0.023(4) -0.002(3) -0.005(3) 0.001(3) C37 0.041(5) 0.032(4) 0.039(5) 0.013(4) 0.006(4) 0.019(4) C40 0.026(4) 0.018(4) 0.050(5) 0.004(3) 0.002(3) 0.008(3) C13 0.109(8) 0.034(5) 0.021(4) -0.003(4) -0.002(5) 0.017(5) C28 0.029(4) 0.028(4) 0.018(4) 0.009(3) -0.001(3) 0.000(3) C38 0.026(4) 0.035(4) 0.026(4) 0.009(3) -0.007(3) 0.002(3) C3 0.063(6) 0.031(5) 0.053(6) -0.001(4) 0.009(5) -0.012(4) C12 0.086(7) 0.025(4) 0.033(5) 0.003(4) 0.005(5) 0.014(4) C9 0.058(5) 0.022(4) 0.033(5) 0.004(4) 0.004(4) 0.009(4) C34 0.077(6) 0.034(5) 0.033(5) 0.013(4) 0.017(4) 0.021(4) C27 0.075(6) 0.025(4) 0.052(6) 0.000(4) 0.034(5) 0.001(4) C2 0.042(5) 0.026(4) 0.041(5) -0.001(4) -0.003(4) -0.004(4) C10 0.043(4) 0.025(4) 0.026(4) -0.005(3) -0.001(3) 0.000(3) C33 0.085(7) 0.037(5) 0.046(6) 0.011(4) 0.031(5) 0.022(5) C24 0.045(5) 0.043(5) 0.051(6) -0.007(4) 0.017(4) -0.013(4) C26 0.041(5) 0.022(4) 0.047(5) -0.004(4) 0.012(4) -0.003(3) O2 0.032(3) 0.032(3) 0.031(3) 0.003(2) 0.005(2) -0.010(2) C45 0.067(6) 0.094(8) 0.029(5) 0.011(5) 0.005(4) 0.028(6) O12 0.032(3) 0.028(3) 0.025(3) 0.007(2) 0.007(2) 0.009(2) O3 0.030(3) 0.027(3) 0.026(3) -0.005(2) 0.002(2) 0.002(2) C8 0.073(6) 0.013(4) 0.034(5) -0.003(3) 0.014(4) -0.002(4) C5 0.066(6) 0.029(4) 0.028(4) -0.003(4) 0.002(4) 0.025(4) C20 0.109(8) 0.047(5) 0.015(4) -0.006(4) 0.003(5) -0.027(5) C22 0.101(8) 0.024(4) 0.039(5) -0.006(4) 0.036(5) -0.026(5) C19 0.131(9) 0.040(5) 0.032(5) -0.011(4) 0.011(6) -0.052(6) C30 0.130(9) 0.045(5) 0.027(5) 0.012(4) 0.024(5) 0.054(6) C23 0.074(7) 0.051(6) 0.066(7) -0.016(5) 0.030(6) -0.040(5) C44 0.032(5) 0.139(10) 0.035(5) -0.024(6) 0.010(4) 0.015(5) C7 0.039(4) 0.021(4) 0.018(4) 0.000(3) 0.001(3) 0.008(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 Ho2 O7 2.208(5) 3_563 ? Ho2 O9 2.208(5) 4_576 ? Ho2 O6 2.254(5) . ? Ho2 O13 2.267(5) 2_543 ? Ho2 O11 2.350(4) . ? Ho2 O1W 2.358(5) . ? Ho2 O12 2.430(4) . ? Ho2 C35 2.769(7) . ? Ho1 O1 2.232(5) . ? Ho1 O14 2.241(5) 2_543 ? Ho1 O8 2.253(5) 4_576 ? Ho1 O2 2.297(5) 3_664 ? Ho1 O16 2.334(4) . ? Ho1 O3 2.346(4) 2_653 ? Ho1 O4 2.448(5) 2_653 ? Ho1 C14 2.712(7) 2_653 ? O9 C28 1.247(7) . ? O9 Ho2 2.208(5) 4_575 ? O7 C21 1.256(8) . ? O7 Ho2 2.208(5) 3_563 ? O11 C35 1.244(8) . ? O14 C42 1.261(8) . ? O14 Ho1 2.241(5) 2_553 ? O1 C7 1.275(8) . ? O16 C43 1.256(8) . ? O6 C21 1.238(8) . ? O13 C42 1.239(8) . ? O13 Ho2 2.267(5) 2_553 ? C35 O12 1.275(8) . ? C35 C29 1.473(9) . ? O15 C36 1.385(8) . ? O15 C32 1.394(8) . ? C36 C41 1.359(10) . ? C36 C37 1.386(10) . ? C32 C31 1.345(11) . ? C32 C33 1.372(11) . ? O8 C28 1.261(7) . ? O8 Ho1 2.253(5) 4_575 ? C15 C16 1.362(9) . ? C15 C20 1.371(10) . ? C15 C21 1.491(9) . ? C17 C18 1.360(10) . ? C17 C16 1.371(9) . ? O10 C18 1.387(9) . ? O10 C22 1.395(9) . ? C29 C34 1.354(9) . ? C29 C30 1.367(10) . ? C25 C26 1.360(9) . ? C25 C24 1.393(9) . ? C25 C28 1.489(9) . ? C42 C39 1.500(9) . ? N1 C43 1.327(9) . ? N1 C44 1.453(11) . ? C18 C19 1.363(11) . ? N2 C43 1.310(9) . ? N2 C45 1.440(10) . ? C14 O3 1.266(8) . ? C14 O4 1.265(8) . ? C14 C11 1.503(9) . ? C14 Ho1 2.712(7) 2_643 ? C39 C40 1.370(9) . ? C39 C38 1.385(9) . ? O5 C8 1.369(8) . ? O5 C4 1.387(8) . ? O4 Ho1 2.448(5) 2_643 ? C6 C5 1.372(10) . ? C6 C1 1.389(9) . ? C4 C3 1.380(11) . ? C4 C5 1.382(10) . ? C41 C40 1.388(9) . ? C11 C10 1.366(9) . ? C11 C12 1.380(10) . ? C1 C2 1.372(9) . ? C1 C7 1.493(9) . ? C37 C38 1.384(9) . ? C13 C8 1.387(10) . ? C13 C12 1.391(10) . ? C3 C2 1.382(10) . ? C9 C8 1.372(10) . ? C9 C10 1.375(9) . ? C34 C33 1.376(10) . ? C27 C22 1.365(11) . ? C27 C26 1.375(10) . ? C24 C23 1.373(11) . ? O2 C7 1.239(8) . ? O2 Ho1 2.297(5) 3_664 ? C45 C44 1.499(10) . ? O3 Ho1 2.346(4) 2_643 ? C20 C19 1.384(11) . ? C22 C23 1.349(12) . ? C30 C31 1.392(11) . ? 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 Ho2 O9 170.09(18) 3_563 4_576 ? O7 Ho2 O6 102.64(19) 3_563 . ? O9 Ho2 O6 84.9(2) 4_576 . ? O7 Ho2 O13 83.25(18) 3_563 2_543 ? O9 Ho2 O13 104.38(18) 4_576 2_543 ? O6 Ho2 O13 81.81(19) . 2_543 ? O7 Ho2 O11 86.72(17) 3_563 . ? O9 Ho2 O11 88.61(18) 4_576 . ? O6 Ho2 O11 78.14(17) . . ? O13 Ho2 O11 155.01(18) 2_543 . ? O7 Ho2 O1W 97.07(18) 3_563 . ? O9 Ho2 O1W 79.02(18) 4_576 . ? O6 Ho2 O1W 148.12(18) . . ? O13 Ho2 O1W 75.87(18) 2_543 . ? O11 Ho2 O1W 128.24(17) . . ? O7 Ho2 O12 83.16(17) 3_563 . ? O9 Ho2 O12 87.03(17) 4_576 . ? O6 Ho2 O12 131.46(17) . . ? O13 Ho2 O12 146.18(18) 2_543 . ? O11 Ho2 O12 53.85(15) . . ? O1W Ho2 O12 75.29(16) . . ? O7 Ho2 C35 86.00(19) 3_563 . ? O9 Ho2 C35 85.92(19) 4_576 . ? O6 Ho2 C35 104.18(19) . . ? O13 Ho2 C35 168.65(19) 2_543 . ? O11 Ho2 C35 26.53(17) . . ? O1W Ho2 C35 101.95(19) . . ? O12 Ho2 C35 27.41(17) . . ? O1 Ho1 O14 86.98(17) . 2_543 ? O1 Ho1 O8 176.96(17) . 4_576 ? O14 Ho1 O8 95.30(18) 2_543 4_576 ? O1 Ho1 O2 91.86(18) . 3_664 ? O14 Ho1 O2 154.87(18) 2_543 3_664 ? O8 Ho1 O2 86.93(18) 4_576 3_664 ? O1 Ho1 O16 91.61(18) . . ? O14 Ho1 O16 77.47(19) 2_543 . ? O8 Ho1 O16 90.86(18) 4_576 . ? O2 Ho1 O16 77.48(16) 3_664 . ? O1 Ho1 O3 91.54(16) . 2_653 ? O14 Ho1 O3 131.11(18) 2_543 2_653 ? O8 Ho1 O3 85.44(16) 4_576 2_653 ? O2 Ho1 O3 73.99(16) 3_664 2_653 ? O16 Ho1 O3 151.38(17) . 2_653 ? O1 Ho1 O4 100.92(18) . 2_653 ? O14 Ho1 O4 77.93(18) 2_543 2_653 ? O8 Ho1 O4 77.64(18) 4_576 2_653 ? O2 Ho1 O4 126.76(16) 3_664 2_653 ? O16 Ho1 O4 151.66(17) . 2_653 ? O3 Ho1 O4 54.41(16) 2_653 2_653 ? O1 Ho1 C14 102.80(19) . 2_653 ? O14 Ho1 C14 105.7(2) 2_543 2_653 ? O8 Ho1 C14 74.66(19) 4_576 2_653 ? O2 Ho1 C14 99.02(19) 3_664 2_653 ? O16 Ho1 C14 165.33(19) . 2_653 ? O3 Ho1 C14 27.79(18) 2_653 2_653 ? O4 Ho1 C14 27.79(18) 2_653 2_653 ? C28 O9 Ho2 149.4(5) . 4_575 ? C21 O7 Ho2 146.2(4) . 3_563 ? C35 O11 Ho2 95.9(4) . . ? C42 O14 Ho1 171.4(5) . 2_553 ? C7 O1 Ho1 146.2(5) . . ? C43 O16 Ho1 138.3(5) . . ? C21 O6 Ho2 151.2(5) . . ? C42 O13 Ho2 137.6(5) . 2_553 ? O11 C35 O12 118.5(6) . . ? O11 C35 C29 120.0(6) . . ? O12 C35 C29 121.4(6) . . ? O11 C35 Ho2 57.6(3) . . ? O12 C35 Ho2 61.3(3) . . ? C29 C35 Ho2 171.9(5) . . ? C36 O15 C32 119.3(6) . . ? C41 C36 C37 121.4(7) . . ? C41 C36 O15 116.4(7) . . ? C37 C36 O15 122.0(7) . . ? C31 C32 C33 120.7(8) . . ? C31 C32 O15 121.6(8) . . ? C33 C32 O15 117.5(7) . . ? C28 O8 Ho1 143.8(5) . 4_575 ? C16 C15 C20 117.5(6) . . ? C16 C15 C21 122.0(6) . . ? C20 C15 C21 120.5(7) . . ? C18 C17 C16 118.7(7) . . ? C18 O10 C22 116.4(6) . . ? C34 C29 C30 118.0(7) . . ? C34 C29 C35 124.2(6) . . ? C30 C29 C35 117.8(7) . . ? C15 C16 C17 122.1(7) . . ? C26 C25 C24 119.0(7) . . ? C26 C25 C28 120.9(6) . . ? C24 C25 C28 120.0(6) . . ? O13 C42 O14 123.9(7) . . ? O13 C42 C39 118.6(6) . . ? O14 C42 C39 117.4(6) . . ? C43 N1 C44 114.0(6) . . ? C19 C18 C17 121.9(7) . . ? C19 C18 O10 121.3(8) . . ? C17 C18 O10 116.7(7) . . ? C43 N2 C45 112.2(6) . . ? O6 C21 O7 124.5(7) . . ? O6 C21 C15 118.9(7) . . ? O7 C21 C15 116.6(6) . . ? O3 C14 O4 120.1(6) . . ? O3 C14 C11 118.2(6) . . ? O4 C14 C11 121.3(7) . . ? O3 C14 Ho1 59.8(3) . 2_643 ? O4 C14 Ho1 64.4(4) . 2_643 ? C11 C14 Ho1 153.3(4) . 2_643 ? O16 C43 N2 127.0(7) . . ? O16 C43 N1 124.6(7) . . ? N2 C43 N1 108.2(7) . . ? C40 C39 C38 119.7(6) . . ? C40 C39 C42 121.5(6) . . ? C38 C39 C42 118.8(6) . . ? C8 O5 C4 119.7(6) . . ? C14 O4 Ho1 87.8(4) . 2_643 ? C5 C6 C1 120.8(7) . . ? C3 C4 C5 120.4(7) . . ? C3 C4 O5 119.6(8) . . ? C5 C4 O5 119.5(8) . . ? C36 C41 C40 119.5(7) . . ? C10 C11 C12 119.8(6) . . ? C10 C11 C14 119.5(6) . . ? C12 C11 C14 120.3(6) . . ? C2 C1 C6 118.8(6) . . ? C2 C1 C7 120.5(6) . . ? C6 C1 C7 120.5(6) . . ? C38 C37 C36 118.5(6) . . ? C39 C40 C41 120.3(6) . . ? C8 C13 C12 119.2(8) . . ? O9 C28 O8 122.1(7) . . ? O9 C28 C25 120.4(6) . . ? O8 C28 C25 117.5(6) . . ? C37 C38 C39 120.6(7) . . ? C4 C3 C2 119.2(7) . . ? C11 C12 C13 119.7(7) . . ? C8 C9 C10 118.8(7) . . ? C29 C34 C33 121.9(7) . . ? C22 C27 C26 118.1(8) . . ? C1 C2 C3 121.1(7) . . ? C11 C10 C9 121.5(7) . . ? C32 C33 C34 118.9(8) . . ? C23 C24 C25 119.1(8) . . ? C25 C26 C27 121.7(7) . . ? C7 O2 Ho1 133.8(4) . 3_664 ? N2 C45 C44 104.8(7) . . ? C35 O12 Ho2 91.3(4) . . ? C14 O3 Ho1 92.4(4) . 2_643 ? C9 C8 O5 122.7(7) . . ? C9 C8 C13 121.0(7) . . ? O5 C8 C13 116.3(7) . . ? C6 C5 C4 119.6(7) . . ? C15 C20 C19 122.2(7) . . ? C23 C22 C27 121.7(8) . . ? C23 C22 O10 121.6(8) . . ? C27 C22 O10 116.7(8) . . ? C18 C19 C20 117.6(7) . . ? C29 C30 C31 121.3(8) . . ? C32 C31 C30 119.1(9) . . ? C22 C23 C24 120.4(8) . . ? N1 C44 C45 100.6(6) . . ? O2 C7 O1 124.2(6) . . ? O2 C7 C1 120.1(6) . . ? O1 C7 C1 115.7(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.405 _refine_diff_density_min -1.322 _refine_diff_density_rms 0.220 data_4 _database_code_depnum_ccdc_archive 'CCDC 894565' #TrackingRef 'cec.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H36 N2 O19 Tb2' _chemical_formula_weight 1226.60 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 monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8868(5) _cell_length_b 29.0154(14) _cell_length_c 16.6276(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.827(6) _cell_angle_gamma 90.00 _cell_volume 4285.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6225 _cell_measurement_theta_min 2.2883 _cell_measurement_theta_max 25 _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 3.360 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.75798 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 15797 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.2883 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7508 _reflns_number_gt 4936 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART(Bruker,1998) _computing_cell_refinement SMART _computing_data_reduction SAINT(Bruker,1998) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL (Bruker,1998)' _computing_publication_material SHELXL _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^)+(0.1000P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7508 _refine_ls_number_parameters 641 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 0.640 _refine_ls_restrained_S_all 0.640 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.44442(4) 0.011312(9) 0.357142(18) 0.02573(10) Uani 1 1 d . . . Tb2 Tb 0.19183(3) 0.014213(9) 0.068151(17) 0.01900(10) Uani 1 1 d . . . O4 O 0.5337(4) -0.45170(12) 0.5006(2) 0.0235(9) Uani 1 1 d . . . O3 O 0.7750(5) -0.45253(13) 0.4777(3) 0.0288(10) Uani 1 1 d . . . O7 O 0.2797(5) 0.05733(14) -0.0325(3) 0.0347(11) Uani 1 1 d . . . C42 C 0.2285(7) 0.4367(2) 0.2788(4) 0.0269(15) Uani 1 1 d . . . O14 O 0.1775(6) 0.45395(15) 0.2143(3) 0.0421(13) Uani 1 1 d . . . O2 O 0.5923(6) -0.07517(14) 0.5581(3) 0.0397(12) Uani 1 1 d . . . O12 O 0.3486(6) 0.05680(14) 0.2587(3) 0.0387(12) Uani 1 1 d . . . C35 C 0.2985(7) 0.0867(2) 0.2109(4) 0.0268(15) Uani 1 1 d . . . O11 O 0.2096(5) 0.07840(13) 0.1521(3) 0.0310(11) Uani 1 1 d . . . O6 O 0.2083(6) 0.07015(15) -0.1608(3) 0.0399(12) Uani 1 1 d . . . O13 O 0.2289(5) 0.45629(15) 0.3449(3) 0.0349(11) Uani 1 1 d . . . O1 O 0.5203(6) -0.04597(14) 0.4405(3) 0.0413(12) Uani 1 1 d . . . C14 C 0.6507(6) -0.43232(19) 0.4737(3) 0.0175(12) Uani 1 1 d . . . C11 C 0.6375(6) -0.38468(19) 0.4396(4) 0.0214(14) Uani 1 1 d . . . C7 C 0.5617(7) -0.07930(19) 0.4848(4) 0.0256(14) Uani 1 1 d . . . C32 C 0.3481(7) 0.1352(2) 0.2249(4) 0.0234(14) Uani 1 1 d . . . C12 C 0.7350(7) -0.3705(2) 0.3810(4) 0.0244(14) Uani 1 1 d . . . O15 O 0.5244(6) 0.26586(16) 0.2605(4) 0.077(2) Uani 1 1 d . . . O10 O 0.5348(6) 0.25937(14) -0.0709(4) 0.0561(17) Uani 1 1 d . . . C22 C 0.4644(8) 0.3002(2) -0.0977(5) 0.0401(19) Uani 1 1 d . . . O5 O 0.6042(7) -0.25480(13) 0.3390(3) 0.0506(16) Uani 1 1 d . . . C21 C 0.2699(7) 0.0823(2) -0.0958(4) 0.0258(14) Uani 1 1 d . . . C4 C 0.5747(7) -0.12632(19) 0.4476(4) 0.0258(14) Uani 1 1 d . . . C38 C 0.3526(10) 0.3751(3) 0.2022(5) 0.052(2) Uani 1 1 d . . . H38A H 0.3428 0.3936 0.1566 0.062 Uiso 1 1 calc R . . C17 C 0.2950(8) 0.1641(2) -0.1439(4) 0.0386(18) Uani 1 1 d . . . H17A H 0.2265 0.1574 -0.1858 0.046 Uiso 1 1 calc R . . C1 C 0.5906(8) -0.21340(19) 0.3802(4) 0.0307(16) Uani 1 1 d . . . C29 C 0.4523(8) 0.2237(2) 0.2499(5) 0.042(2) Uani 1 1 d . . . C15 C 0.4585(8) 0.2175(2) -0.0776(4) 0.0347(17) Uani 1 1 d . . . C3 C 0.5153(10) -0.1351(2) 0.3716(5) 0.044(2) Uani 1 1 d . . . C36 C 0.4341(8) 0.3057(2) 0.2621(5) 0.043(2) Uani 1 1 d . . . C33 C 0.4404(9) 0.1460(2) 0.2908(4) 0.0409(19) Uani 1 1 d . . . H33A H 0.4694 0.1229 0.3270 0.049 Uiso 1 1 calc R . . C6 C 0.6554(9) -0.2054(2) 0.4557(4) 0.0350(17) Uani 1 1 d . . . C8 C 0.6177(8) -0.29647(19) 0.3781(4) 0.0317(16) Uani 1 1 d . . . C5 C 0.6444(7) -0.1625(2) 0.4890(4) 0.0307(16) Uani 1 1 d . . . H5A H 0.6845 -0.1573 0.5406 0.037 Uiso 1 1 calc R . . C23 C 0.3387(9) 0.3162(2) -0.0605(5) 0.046(2) Uani 1 1 d . . . H23A H 0.2942 0.2989 -0.0206 0.055 Uiso 1 1 calc R . . C9 C 0.5233(9) -0.3098(2) 0.4382(5) 0.0336(17) Uani 1 1 d . . . C39 C 0.2959(8) 0.3896(2) 0.2726(4) 0.0302(16) Uani 1 1 d . . . C20 C 0.5020(9) 0.1842(2) -0.0234(5) 0.055(2) Uani 1 1 d . . . H20A H 0.5736 0.1909 0.0170 0.066 Uiso 1 1 calc R . . C34 C 0.4898(9) 0.1905(2) 0.3035(5) 0.0421(19) Uani 1 1 d . . . H34A H 0.5488 0.1976 0.3490 0.050 Uiso 1 1 calc R . . C26 C 0.4666(8) 0.3663(2) -0.1805(5) 0.0384(17) Uani 1 1 d . . . H26A H 0.5096 0.3830 -0.2215 0.046 Uiso 1 1 calc R . . C19 C 0.4396(9) 0.1408(2) -0.0286(5) 0.049(2) Uani 1 1 d . . . H19A H 0.4678 0.1186 0.0093 0.059 Uiso 1 1 calc R . . C13 C 0.7225(8) -0.3264(2) 0.3500(4) 0.0329(16) Uani 1 1 d . . . H13A H 0.7859 -0.3170 0.3097 0.039 Uiso 1 1 calc R . . C30 C 0.3577(10) 0.2147(2) 0.1848(6) 0.070(3) Uani 1 1 d . . . H30A H 0.3281 0.2381 0.1495 0.084 Uiso 1 1 calc R . . C18 C 0.3364(7) 0.12965(19) -0.0889(4) 0.0225(13) Uani 1 1 d . . . C16 C 0.3543(8) 0.2080(2) -0.1372(5) 0.0431(19) Uani 1 1 d . . . H16A H 0.3233 0.2309 -0.1731 0.052 Uiso 1 1 calc R . . C10 C 0.5307(7) -0.3542(2) 0.4679(4) 0.0292(15) Uani 1 1 d . . . H10A H 0.4643 -0.3637 0.5067 0.035 Uiso 1 1 calc R . . C27 C 0.5298(9) 0.3246(2) -0.1580(5) 0.045(2) Uani 1 1 d . . . H27A H 0.6144 0.3134 -0.1831 0.054 Uiso 1 1 calc R . . C2 C 0.5192(10) -0.1783(2) 0.3383(4) 0.047(2) Uani 1 1 d . . . H2A H 0.4740 -0.1839 0.2880 0.056 Uiso 1 1 calc R . . C24 C 0.2793(8) 0.3588(2) -0.0837(4) 0.0387(18) Uani 1 1 d . . . H24A H 0.1961 0.3705 -0.0581 0.046 Uiso 1 1 calc R . . C31 C 0.3077(9) 0.1700(2) 0.1730(5) 0.054(2) Uani 1 1 d . . . H31A H 0.2450 0.1635 0.1286 0.064 Uiso 1 1 calc R . . O16 O 0.2173(6) 0.00467(17) 0.4121(4) 0.0516(15) Uani 1 1 d . . . O8 O 0.3234(6) 0.44826(16) -0.2316(3) 0.0498(14) Uani 1 1 d . . . C25 C 0.3437(7) 0.3837(2) -0.1445(4) 0.0288(15) Uani 1 1 d . . . C28 C 0.2761(8) 0.4288(2) -0.1704(4) 0.0306(16) Uani 1 1 d . . . C45 C 0.1122(9) -0.0217(3) 0.4176(5) 0.0418(18) Uani 1 1 d . . . N1 N -0.0105(8) -0.0240(2) 0.3668(5) 0.063(2) Uani 1 1 d . . . H1A H -0.0224 -0.0073 0.3243 0.076 Uiso 1 1 calc R . . N2 N 0.0946(8) -0.0537(2) 0.4749(4) 0.0583(19) Uani 1 1 d . . . H2B H 0.1606 -0.0585 0.5130 0.070 Uiso 1 1 calc R . . C40 C 0.3006(11) 0.3604(2) 0.3364(5) 0.056(2) Uani 1 1 d . . . H40A H 0.2589 0.3693 0.3846 0.068 Uiso 1 1 calc R . . C41 C 0.3670(11) 0.3172(3) 0.3303(6) 0.066(3) Uani 1 1 d . . . H41A H 0.3650 0.2966 0.3730 0.079 Uiso 1 1 calc R . . C37 C 0.4251(11) 0.3329(3) 0.1977(6) 0.061(3) Uani 1 1 d . . . H37A H 0.4673 0.3237 0.1498 0.073 Uiso 1 1 calc R . . C44 C -0.0447(9) -0.0793(3) 0.4672(5) 0.058(2) Uani 1 1 d . . . H44A H -0.1060 -0.0751 0.5138 0.070 Uiso 1 1 calc R . . H44B H -0.0261 -0.1119 0.4596 0.070 Uiso 1 1 calc R . . C43 C -0.1186(10) -0.0578(4) 0.3922(7) 0.082(3) Uani 1 1 d . . . H43A H -0.1368 -0.0808 0.3507 0.099 Uiso 1 1 calc R . . H43B H -0.2133 -0.0433 0.4047 0.099 Uiso 1 1 calc R . . O9 O 0.1735(5) 0.44540(15) -0.1282(3) 0.0383(12) Uani 1 1 d . . . O3W O 0.4582(5) 0.02127(16) 0.0930(3) 0.0354(11) Uani 1 1 d D . . H3WB H 0.4881 -0.0002 0.1213 0.053 Uiso 1 1 calc RD . . O2W O -0.0149(6) 0.00372(16) 0.1560(3) 0.0376(12) Uani 1 1 d D . . H2WB H -0.0238 -0.0237 0.1665 0.056 Uiso 1 1 calc RD . . O1W O 0.6108(7) -0.0126(2) 0.2515(4) 0.0550(15) Uani 1 1 d D . . H1WB H 0.6676 0.0086 0.2408 0.083 Uiso 1 1 calc RD . . H3WA H 0.537(4) 0.0235(19) 0.069(3) 0.015(16) Uiso 1 1 d D . . H2WA H -0.101(7) -0.008(4) 0.142(8) 0.15(6) Uiso 1 1 d D . . H1WA H 0.670(7) -0.029(2) 0.281(4) 0.04(2) Uiso 1 1 d D . . H3A H 0.475(8) -0.115(2) 0.342(5) 0.05(2) Uiso 1 1 d . . . H12A H 0.800(6) -0.3890(17) 0.359(3) 0.003(13) Uiso 1 1 d . . . H6A H 0.708(7) -0.226(2) 0.484(4) 0.030(18) Uiso 1 1 d . . . H9A H 0.456(7) -0.293(2) 0.450(4) 0.021(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0386(2) 0.01378(16) 0.02458(19) -0.00076(12) -0.00336(14) -0.00376(14) Tb2 0.02460(17) 0.01225(15) 0.01999(17) -0.00023(12) -0.00176(12) -0.00255(12) O4 0.025(2) 0.0166(19) 0.029(2) 0.0067(18) 0.0003(19) -0.0024(19) O3 0.035(3) 0.021(2) 0.030(3) 0.0083(19) 0.001(2) 0.002(2) O7 0.037(3) 0.026(2) 0.041(3) 0.011(2) 0.001(2) -0.007(2) C42 0.039(4) 0.014(3) 0.027(4) -0.003(3) -0.006(3) -0.006(3) O14 0.062(3) 0.025(2) 0.039(3) -0.002(2) -0.009(3) 0.017(2) O2 0.068(4) 0.024(2) 0.027(3) -0.009(2) 0.001(2) 0.000(2) O12 0.060(3) 0.015(2) 0.040(3) 0.006(2) -0.010(2) -0.004(2) C35 0.034(4) 0.024(3) 0.022(3) -0.005(3) 0.002(3) 0.004(3) O11 0.038(3) 0.021(2) 0.033(3) -0.010(2) -0.007(2) -0.001(2) O6 0.058(3) 0.027(2) 0.035(3) -0.001(2) 0.001(2) -0.011(2) O13 0.043(3) 0.028(2) 0.034(3) -0.013(2) 0.001(2) -0.001(2) O1 0.054(3) 0.019(2) 0.050(3) 0.000(2) -0.009(2) 0.004(2) C14 0.020(3) 0.016(3) 0.016(3) -0.002(2) 0.003(2) 0.001(3) C11 0.022(3) 0.020(3) 0.022(3) 0.003(3) -0.005(3) -0.003(3) C7 0.030(4) 0.017(3) 0.030(4) 0.003(3) 0.003(3) -0.002(3) C32 0.028(4) 0.018(3) 0.024(4) -0.003(3) -0.001(3) 0.000(3) C12 0.027(3) 0.019(3) 0.027(4) -0.003(3) 0.009(3) 0.004(3) O15 0.049(4) 0.015(2) 0.163(7) -0.012(3) -0.045(4) 0.005(2) O10 0.046(3) 0.018(2) 0.102(5) 0.015(3) -0.037(3) -0.004(2) C22 0.036(4) 0.020(3) 0.063(5) 0.000(3) -0.019(4) -0.005(3) O5 0.120(5) 0.010(2) 0.021(3) 0.0028(19) -0.006(3) 0.005(3) C21 0.027(4) 0.023(3) 0.027(4) 0.003(3) 0.010(3) -0.001(3) C4 0.034(4) 0.015(3) 0.028(4) 0.002(3) -0.001(3) -0.001(3) C38 0.083(6) 0.033(4) 0.040(5) 0.016(4) 0.016(4) 0.018(4) C17 0.048(5) 0.029(4) 0.038(4) 0.008(3) -0.015(3) -0.009(3) C1 0.052(4) 0.011(3) 0.029(4) 0.001(3) -0.003(3) -0.005(3) C29 0.031(4) 0.012(3) 0.083(6) -0.008(3) -0.011(4) 0.004(3) C15 0.036(4) 0.018(3) 0.049(5) 0.005(3) -0.013(3) 0.000(3) C3 0.073(6) 0.019(3) 0.038(5) 0.005(3) -0.025(4) 0.007(4) C36 0.043(4) 0.015(3) 0.070(6) -0.007(4) -0.021(4) 0.006(3) C33 0.064(5) 0.030(4) 0.028(4) 0.001(3) -0.010(4) -0.008(4) C6 0.051(5) 0.017(3) 0.037(4) 0.007(3) -0.011(4) 0.008(3) C8 0.057(5) 0.011(3) 0.026(4) 0.002(3) -0.010(3) -0.003(3) C5 0.045(4) 0.025(3) 0.022(4) 0.002(3) -0.008(3) 0.000(3) C23 0.051(5) 0.033(4) 0.053(5) 0.021(4) 0.001(4) -0.010(4) C9 0.037(4) 0.018(3) 0.046(5) -0.008(3) -0.003(4) 0.013(3) C39 0.045(4) 0.015(3) 0.030(4) -0.002(3) -0.011(3) 0.003(3) C20 0.064(6) 0.031(4) 0.066(6) 0.018(4) -0.034(5) -0.016(4) C34 0.059(5) 0.027(4) 0.039(5) -0.011(3) -0.013(4) -0.006(4) C26 0.040(4) 0.033(4) 0.042(5) 0.008(3) 0.004(3) -0.007(3) C19 0.067(6) 0.030(4) 0.049(5) 0.019(3) -0.028(4) -0.009(4) C13 0.055(5) 0.023(3) 0.021(4) 0.003(3) 0.003(3) -0.008(3) C30 0.085(7) 0.018(4) 0.103(8) 0.018(4) -0.058(6) -0.004(4) C18 0.026(3) 0.018(3) 0.024(3) 0.003(3) 0.005(3) 0.000(3) C16 0.055(5) 0.024(4) 0.049(5) 0.013(3) -0.013(4) -0.005(3) C10 0.028(4) 0.022(3) 0.037(4) 0.007(3) 0.005(3) 0.000(3) C27 0.048(5) 0.030(4) 0.056(5) 0.003(4) -0.002(4) 0.011(4) C2 0.089(6) 0.025(4) 0.026(4) 0.003(3) -0.022(4) 0.002(4) C24 0.042(4) 0.030(4) 0.044(5) 0.009(3) 0.004(3) 0.004(3) C31 0.066(6) 0.024(4) 0.068(6) 0.008(4) -0.037(5) -0.005(4) O16 0.048(3) 0.041(3) 0.066(4) -0.016(3) 0.013(3) -0.013(3) O8 0.058(4) 0.035(3) 0.057(4) 0.015(3) 0.018(3) 0.011(3) C25 0.028(4) 0.024(3) 0.035(4) 0.001(3) 0.002(3) 0.004(3) C28 0.038(4) 0.020(3) 0.034(4) -0.001(3) 0.000(3) -0.002(3) C45 0.040(4) 0.040(4) 0.046(5) -0.001(4) 0.005(4) 0.001(4) N1 0.052(4) 0.064(5) 0.073(6) 0.028(4) -0.014(4) -0.006(4) N2 0.057(5) 0.061(4) 0.057(5) 0.030(4) -0.003(4) -0.008(4) C40 0.099(7) 0.029(4) 0.039(5) 0.005(4) -0.015(5) 0.005(4) C41 0.111(8) 0.027(4) 0.058(6) 0.017(4) -0.031(6) 0.008(5) C37 0.092(7) 0.033(4) 0.059(6) -0.009(4) 0.015(5) 0.017(5) C44 0.051(5) 0.050(5) 0.075(7) 0.014(4) 0.019(5) -0.011(4) C43 0.036(5) 0.085(7) 0.126(10) 0.035(7) 0.003(6) 0.002(5) O9 0.045(3) 0.033(3) 0.037(3) 0.008(2) 0.008(2) 0.012(2) O3W 0.024(3) 0.045(3) 0.037(3) 0.013(2) 0.004(2) 0.001(2) O2W 0.046(3) 0.028(2) 0.040(3) -0.001(2) 0.004(2) -0.012(2) O1W 0.051(4) 0.051(4) 0.062(4) -0.016(3) 0.004(3) -0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O12 2.248(4) . ? Tb1 O1 2.253(4) . ? Tb1 O16 2.251(6) . ? Tb1 O14 2.296(4) 2_545 ? Tb1 O2 2.357(4) 3_656 ? Tb1 O9 2.398(5) 4_666 ? Tb1 O1W 2.433(6) . ? Tb2 O7 2.250(4) . ? Tb2 O13 2.312(4) 2_545 ? Tb2 O11 2.330(4) . ? Tb2 O2W 2.403(5) . ? Tb2 O3W 2.399(4) . ? Tb2 O3 2.466(4) 4 ? Tb2 O4 2.481(4) 2 ? Tb2 O4 2.535(4) 4 ? Tb2 C14 2.865(6) 4 ? O4 C14 1.275(7) . ? O4 Tb2 2.481(4) 2_545 ? O4 Tb2 2.535(4) 4_656 ? O3 C14 1.250(7) . ? O3 Tb2 2.466(4) 4_656 ? O7 C21 1.278(7) . ? C42 O13 1.238(7) . ? C42 O14 1.255(7) . ? C42 C39 1.497(8) . ? O14 Tb1 2.296(4) 2 ? O2 C7 1.245(8) . ? O2 Tb1 2.357(4) 3_656 ? O12 C35 1.250(7) . ? C35 O11 1.261(7) . ? C35 C32 1.488(8) . ? O6 C21 1.246(8) . ? O13 Tb2 2.312(4) 2 ? O1 C7 1.264(7) . ? C14 C11 1.497(8) . ? C14 Tb2 2.865(6) 4_656 ? C11 C12 1.387(9) . ? C11 C10 1.390(9) . ? C7 C4 1.504(8) . ? C32 C31 1.370(9) . ? C32 C33 1.385(9) . ? C12 C13 1.383(8) . ? O15 C29 1.389(8) . ? O15 C36 1.408(8) . ? O10 C15 1.395(7) . ? O10 C22 1.406(8) . ? C22 C27 1.372(11) . ? C22 C23 1.375(10) . ? O5 C8 1.377(7) . ? O5 C1 1.390(7) . ? C21 C18 1.499(8) . ? C4 C3 1.378(9) . ? C4 C5 1.389(8) . ? C38 C39 1.356(10) . ? C38 C37 1.387(10) . ? C17 C16 1.381(9) . ? C17 C18 1.398(9) . ? C1 C2 1.376(9) . ? C1 C6 1.385(9) . ? C29 C34 1.347(10) . ? C29 C30 1.374(10) . ? C15 C16 1.362(9) . ? C15 C20 1.368(9) . ? C3 C2 1.371(9) . ? C36 C37 1.331(11) . ? C36 C41 1.340(12) . ? C33 C34 1.379(9) . ? C6 C5 1.369(9) . ? C8 C13 1.366(9) . ? C8 C9 1.379(10) . ? C23 C24 1.394(9) . ? C9 C10 1.381(8) . ? C39 C40 1.357(10) . ? C20 C19 1.378(9) . ? C26 C25 1.359(9) . ? C26 C27 1.379(9) . ? C19 C18 1.375(9) . ? C30 C31 1.382(10) . ? C24 C25 1.382(9) . ? O16 C45 1.213(9) . ? O8 C28 1.248(8) . ? C25 C28 1.497(8) . ? C28 O9 1.264(8) . ? C45 N2 1.343(10) . ? C45 N1 1.360(10) . ? N1 C43 1.445(11) . ? N2 C44 1.446(10) . ? C40 C41 1.390(10) . ? C44 C43 1.524(13) . ? O9 Tb1 2.398(5) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Tb1 O1 168.35(16) . . ? O12 Tb1 O16 91.3(2) . . ? O1 Tb1 O16 86.7(2) . . ? O12 Tb1 O14 83.54(16) . 2_545 ? O1 Tb1 O14 84.86(17) . 2_545 ? O16 Tb1 O14 74.55(18) . 2_545 ? O12 Tb1 O2 85.26(16) . 3_656 ? O1 Tb1 O2 104.87(17) . 3_656 ? O16 Tb1 O2 71.41(17) . 3_656 ? O14 Tb1 O2 143.81(18) 2_545 3_656 ? O12 Tb1 O9 93.83(17) . 4_666 ? O1 Tb1 O9 95.03(17) . 4_666 ? O16 Tb1 O9 140.64(17) . 4_666 ? O14 Tb1 O9 144.80(17) 2_545 4_666 ? O2 Tb1 O9 70.18(16) 3_656 4_666 ? O12 Tb1 O1W 82.3(2) . . ? O1 Tb1 O1W 93.2(2) . . ? O16 Tb1 O1W 147.38(18) . . ? O14 Tb1 O1W 72.95(18) 2_545 . ? O2 Tb1 O1W 139.05(17) 3_656 . ? O9 Tb1 O1W 71.91(17) 4_666 . ? O7 Tb2 O13 139.77(16) . 2_545 ? O7 Tb2 O11 89.01(16) . . ? O13 Tb2 O11 101.12(16) 2_545 . ? O7 Tb2 O2W 144.41(17) . . ? O13 Tb2 O2W 75.60(17) 2_545 . ? O11 Tb2 O2W 77.03(16) . . ? O7 Tb2 O3W 73.52(16) . . ? O13 Tb2 O3W 71.04(16) 2_545 . ? O11 Tb2 O3W 77.35(16) . . ? O2W Tb2 O3W 132.52(17) . . ? O7 Tb2 O3 80.32(15) . 4 ? O13 Tb2 O3 76.28(15) 2_545 4 ? O11 Tb2 O3 158.38(15) . 4 ? O2W Tb2 O3 121.91(15) . 4 ? O3W Tb2 O3 81.59(15) . 4 ? O7 Tb2 O4 74.36(15) . 2 ? O13 Tb2 O4 143.44(14) 2_545 2 ? O11 Tb2 O4 89.74(13) . 2 ? O2W Tb2 O4 73.03(16) . 2 ? O3W Tb2 O4 145.45(14) . 2 ? O3 Tb2 O4 105.18(13) 4 2 ? O7 Tb2 O4 105.59(15) . 4 ? O13 Tb2 O4 84.87(15) 2_545 4 ? O11 Tb2 O4 149.72(14) . 4 ? O2W Tb2 O4 75.82(15) . 4 ? O3W Tb2 O4 131.86(15) . 4 ? O3 Tb2 O4 51.90(13) 4 4 ? O4 Tb2 O4 69.69(13) 2 4 ? O7 Tb2 C14 95.42(16) . 4 ? O13 Tb2 C14 76.77(16) 2_545 4 ? O11 Tb2 C14 175.12(16) . 4 ? O2W Tb2 C14 98.14(16) . 4 ? O3W Tb2 C14 105.84(17) . 4 ? O3 Tb2 C14 25.75(14) 4 4 ? O4 Tb2 C14 89.49(14) 2 4 ? O4 Tb2 C14 26.42(14) 4 4 ? C14 O4 Tb2 132.1(4) . 2_545 ? C14 O4 Tb2 91.4(3) . 4_656 ? Tb2 O4 Tb2 110.31(13) 2_545 4_656 ? C14 O3 Tb2 95.3(3) . 4_656 ? C21 O7 Tb2 155.7(4) . . ? O13 C42 O14 124.4(6) . . ? O13 C42 C39 119.4(6) . . ? O14 C42 C39 116.2(6) . . ? C42 O14 Tb1 152.0(4) . 2 ? C7 O2 Tb1 129.1(4) . 3_656 ? C35 O12 Tb1 171.8(4) . . ? O12 C35 O11 124.2(6) . . ? O12 C35 C32 117.3(6) . . ? O11 C35 C32 118.5(5) . . ? C35 O11 Tb2 130.3(4) . . ? C42 O13 Tb2 151.9(4) . 2 ? C7 O1 Tb1 177.6(4) . . ? O3 C14 O4 120.2(5) . . ? O3 C14 C11 120.8(5) . . ? O4 C14 C11 119.0(5) . . ? O3 C14 Tb2 59.0(3) . 4_656 ? O4 C14 Tb2 62.2(3) . 4_656 ? C11 C14 Tb2 168.6(4) . 4_656 ? C12 C11 C10 119.8(6) . . ? C12 C11 C14 119.8(5) . . ? C10 C11 C14 120.4(5) . . ? O2 C7 O1 123.2(6) . . ? O2 C7 C4 118.2(5) . . ? O1 C7 C4 118.6(6) . . ? C31 C32 C33 117.9(6) . . ? C31 C32 C35 121.9(6) . . ? C33 C32 C35 120.1(6) . . ? C13 C12 C11 119.5(6) . . ? C29 O15 C36 117.7(6) . . ? C15 O10 C22 119.9(5) . . ? C27 C22 C23 121.7(6) . . ? C27 C22 O10 118.2(7) . . ? C23 C22 O10 120.0(7) . . ? C8 O5 C1 122.2(5) . . ? O6 C21 O7 124.7(6) . . ? O6 C21 C18 119.2(5) . . ? O7 C21 C18 116.1(6) . . ? C3 C4 C5 117.8(6) . . ? C3 C4 C7 120.9(6) . . ? C5 C4 C7 121.3(6) . . ? C39 C38 C37 120.4(7) . . ? C16 C17 C18 121.0(6) . . ? C2 C1 C6 120.5(6) . . ? C2 C1 O5 115.8(6) . . ? C6 C1 O5 123.5(6) . . ? C34 C29 C30 121.2(6) . . ? C34 C29 O15 116.3(7) . . ? C30 C29 O15 122.3(7) . . ? C16 C15 C20 120.6(6) . . ? C16 C15 O10 123.5(6) . . ? C20 C15 O10 115.8(6) . . ? C2 C3 C4 121.7(6) . . ? C37 C36 C41 121.1(7) . . ? C37 C36 O15 119.5(8) . . ? C41 C36 O15 119.3(8) . . ? C34 C33 C32 120.7(6) . . ? C5 C6 C1 119.1(6) . . ? C13 C8 O5 116.5(6) . . ? C13 C8 C9 120.5(6) . . ? O5 C8 C9 122.8(6) . . ? C6 C5 C4 121.6(6) . . ? C22 C23 C24 118.6(7) . . ? C8 C9 C10 119.8(6) . . ? C40 C39 C38 118.6(6) . . ? C40 C39 C42 121.2(7) . . ? C38 C39 C42 120.1(6) . . ? C15 C20 C19 119.9(7) . . ? C29 C34 C33 119.9(7) . . ? C25 C26 C27 122.1(7) . . ? C18 C19 C20 121.2(6) . . ? C8 C13 C12 120.5(6) . . ? C29 C30 C31 118.4(7) . . ? C19 C18 C17 117.7(6) . . ? C19 C18 C21 121.6(6) . . ? C17 C18 C21 120.8(6) . . ? C15 C16 C17 119.6(6) . . ? C9 C10 C11 119.9(6) . . ? C22 C27 C26 118.2(7) . . ? C3 C2 C1 119.3(7) . . ? C25 C24 C23 120.3(7) . . ? C32 C31 C30 121.8(7) . . ? C45 O16 Tb1 141.9(5) . . ? C26 C25 C24 119.1(6) . . ? C26 C25 C28 121.3(6) . . ? C24 C25 C28 119.7(6) . . ? O8 C28 O9 123.1(6) . . ? O8 C28 C25 119.2(6) . . ? O9 C28 C25 117.7(6) . . ? O16 C45 N2 126.6(8) . . ? O16 C45 N1 126.0(8) . . ? N2 C45 N1 107.4(7) . . ? C45 N1 C43 112.2(7) . . ? C45 N2 C44 114.2(7) . . ? C39 C40 C41 120.5(8) . . ? C36 C41 C40 119.2(8) . . ? C36 C37 C38 119.8(8) . . ? N2 C44 C43 102.0(6) . . ? N1 C43 C44 104.1(7) . . ? C28 O9 Tb1 140.3(4) . 4_565 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.207 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.125 data_5 _database_code_depnum_ccdc_archive 'CCDC 894566' #TrackingRef 'cec.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H36 Dy2 N2 O19' _chemical_formula_weight 1233.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8980(4) _cell_length_b 28.9894(12) _cell_length_c 16.6177(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.950(4) _cell_angle_gamma 90.00 _cell_volume 4284.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4012 _cell_measurement_theta_min 2.4336 _cell_measurement_theta_max 21 _exptl_crystal_description sheet _exptl_crystal_colour green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.913 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 3.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.53766 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 12793 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.1164 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.4336 _diffrn_reflns_theta_max 21.00 _reflns_number_total 4582 _reflns_number_gt 3771 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART(Bruker,1998) _computing_cell_refinement SMART _computing_data_reduction SAINT(Bruker,1998) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL (Bruker,1998)' _computing_publication_material SHELXL _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^)+(0.0670P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4582 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1688 _refine_ls_wR_factor_gt 0.1598 _refine_ls_goodness_of_fit_ref 1.477 _refine_ls_restrained_S_all 1.477 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 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 0.94470(7) 0.01133(2) 0.85835(3) 0.0248(3) Uani 1 1 d . . . Dy2 Dy 0.69268(7) 0.01434(2) 0.56843(3) 0.0189(3) Uani 1 1 d . . . O6 O 0.4640(9) 0.0489(3) 0.4993(4) 0.017(2) Uani 1 1 d . . . O1 O 0.8226(10) -0.0466(3) 0.7867(5) 0.030(2) Uani 1 1 d . . . O11 O 0.7804(9) 0.0581(3) 0.4661(5) 0.025(2) Uani 1 1 d . . . O7 O 0.2241(9) 0.0482(3) 0.5225(4) 0.023(2) Uiso 1 1 d . . . O1W O 0.4844(10) 0.0026(3) 0.6580(5) 0.025(2) Uani 1 1 d . . . H10B H 0.4071 0.0134 0.6373 0.030 Uiso 1 1 calc R . . H10C H 0.5009 -0.0127 0.7089 0.030 Uiso 1 1 d R . . O16 O 0.7136(11) 0.0050(3) 0.9150(6) 0.037(3) Uani 1 1 d . . . O3W O 1.1160(10) -0.0125(4) 0.7523(5) 0.048(3) Uani 1 1 d . . . H10F H 1.0766 -0.0331 0.7252 0.057 Uiso 1 1 calc R . . H10G H 1.2122 0.0021 0.7476 0.057 Uiso 1 1 d R . . O15 O 1.0345(10) 0.2585(3) 0.4290(6) 0.045(3) Uani 1 1 d . . . C14 C 0.7025(13) -0.4120(5) 0.7889(7) 0.018(3) Uani 1 1 d . . . C25 C 0.4265(13) 0.3733(4) 0.5502(6) 0.013(3) Uani 1 1 d . . . C36 C 0.9671(15) 0.2986(5) 0.4014(9) 0.035(4) Uani 1 1 d . . . C22 C 0.4121(16) 0.2860(5) 0.6206(7) 0.032(4) Uani 1 1 d . . . C39 C 0.8447(13) 0.3840(5) 0.3552(6) 0.018(3) Uiso 1 1 d . . . C19 C 0.3823(14) 0.2038(5) 0.6212(7) 0.024(3) Uiso 1 1 d . . . C1 C 0.7703(14) -0.0637(5) 0.7218(8) 0.022(3) Uani 1 1 d . . . C43 C 0.6070(17) -0.0224(6) 0.9186(8) 0.032(4) Uani 1 1 d . . . C33 C 0.9625(14) 0.2175(5) 0.4233(8) 0.031(4) Uani 1 1 d . . . C15 C 0.3488(13) 0.0690(4) 0.5273(6) 0.013(3) Uiso 1 1 d . . . C31 C 0.9374(16) 0.1408(5) 0.4714(8) 0.038(4) Uani 1 1 d . . . H31A H 0.9634 0.1187 0.5100 0.045 Uiso 1 1 calc R . . C11 C 0.6518(13) -0.3650(5) 0.7747(6) 0.022(3) Uiso 1 1 d . . . C35 C 0.7980(14) 0.1646(5) 0.3560(7) 0.031(4) Uani 1 1 d . . . H35A H 0.7293 0.1583 0.3140 0.037 Uiso 1 1 calc R . . C45 C 0.3779(17) -0.0578(6) 0.8952(11) 0.062(5) Uani 1 1 d . . . H45A H 0.3563 -0.0809 0.8543 0.074 Uiso 1 1 calc R . . H45B H 0.2851 -0.0428 0.9094 0.074 Uiso 1 1 calc R . . C40 C 0.9677(15) 0.3664(5) 0.3198(7) 0.033(4) Uani 1 1 d . . . H40A H 1.0120 0.3830 0.2790 0.040 Uiso 1 1 calc R . . C2 C 0.7065(13) -0.1102(5) 0.7264(7) 0.022(3) Uani 1 1 d . . . N2 N 0.4871(14) -0.0248(5) 0.8689(7) 0.049(4) Uani 1 1 d . . . H2A H 0.4759 -0.0086 0.8258 0.059 Uiso 1 1 calc R . . C24 C 0.3578(14) 0.3375(5) 0.5120(7) 0.025(3) Uani 1 1 d . . . H24A H 0.3164 0.3423 0.4606 0.030 Uiso 1 1 calc R . . C7 C 0.6485(16) -0.1260(5) 0.7963(7) 0.040(4) Uani 1 1 d . . . H7A H 0.6609 -0.1079 0.8423 0.048 Uiso 1 1 calc R . . C37 C 0.8433(16) 0.3158(6) 0.4386(8) 0.041(4) Uani 1 1 d . . . H37A H 0.8005 0.2989 0.4795 0.049 Uiso 1 1 calc R . . C28 C 0.4364(14) 0.4192(5) 0.5157(7) 0.022(3) Uiso 1 1 d . . . C34 C 0.8581(15) 0.2071(6) 0.3629(8) 0.040(4) Uiso 1 1 d . . . H34A H 0.8285 0.2299 0.3263 0.048 Uiso 1 1 calc R . . C21 C 0.2643(14) 0.1310(5) 0.6169(7) 0.024(3) Uiso 1 1 d . . . H21A H 0.1882 0.1115 0.6334 0.029 Uiso 1 1 calc R . . C23 C 0.3462(15) 0.2944(5) 0.5453(7) 0.031(4) Uani 1 1 d . . . H23A H 0.2946 0.2711 0.5176 0.037 Uiso 1 1 calc R . . C27 C 0.4794(16) 0.3215(5) 0.6603(7) 0.039(4) Uani 1 1 d . . . H27A H 0.5208 0.3166 0.7118 0.047 Uiso 1 1 calc R . . C18 C 0.4798(14) 0.1899(4) 0.5622(6) 0.024(3) Uani 1 1 d . . . H18A H 0.5521 0.2099 0.5433 0.029 Uiso 1 1 calc R . . C20 C 0.2784(15) 0.1734(5) 0.6487(6) 0.032(4) Uani 1 1 d . . . H20A H 0.2165 0.1823 0.6899 0.039 Uiso 1 1 calc R . . C26 C 0.4882(14) 0.3644(5) 0.6271(7) 0.034(4) Uiso 1 1 d . . . H26A H 0.5360 0.3880 0.6560 0.040 Uiso 1 1 calc R . . C29 C 0.7707(14) 0.0834(5) 0.4038(8) 0.023(3) Uani 1 1 d . . . C17 C 0.4667(13) 0.1461(5) 0.5328(7) 0.021(3) Uiso 1 1 d . . . H17A H 0.5310 0.1365 0.4931 0.025 Uiso 1 1 calc R . . N1 N 0.5946(13) -0.0534(5) 0.9749(7) 0.044(4) Uani 1 1 d . . . H1A H 0.6620 -0.0582 1.0122 0.053 Uiso 1 1 calc R . . C41 C 1.0277(14) 0.3247(5) 0.3430(8) 0.031(4) Uani 1 1 d . . . H41A H 1.1127 0.3139 0.3178 0.037 Uiso 1 1 calc R . . C44 C 0.4573(17) -0.0783(6) 0.9676(8) 0.056(5) Uani 1 1 d . . . H44A H 0.3986 -0.0744 1.0153 0.067 Uiso 1 1 calc R . . H44B H 0.4760 -0.1109 0.9597 0.067 Uiso 1 1 calc R . . C30 C 0.8374(12) 0.1299(5) 0.4107(6) 0.015(3) Uani 1 1 d . . . O5 O 0.4750(13) -0.2335(5) 0.7409(6) 0.071(3) Uiso 1 1 d . . . C8 C 0.5502(16) -0.2770(6) 0.7484(8) 0.043(4) Uiso 1 1 d . . . C9 C 0.5057(14) -0.3098(5) 0.6971(7) 0.030(4) Uani 1 1 d . . . H9A H 0.4413 -0.3030 0.6535 0.036 Uiso 1 1 calc R . . C13 C 0.6368(18) -0.2862(7) 0.8151(10) 0.066(5) Uiso 1 1 d . . . H13A H 0.6568 -0.2631 0.8527 0.079 Uiso 1 1 calc R . . C5 C 0.5660(16) -0.1941(6) 0.7361(8) 0.043(4) Uiso 1 1 d . . . O2 O 0.7727(9) -0.0446(3) 0.6550(5) 0.029(2) Uani 1 1 d . . . O9 O 0.4809(9) 0.4533(3) 0.5573(5) 0.033(2) Uiso 1 1 d . . . O13 O 0.6747(10) 0.4455(3) 0.3733(5) 0.027(2) Uani 1 1 d . . . O3 O 0.7908(9) -0.4210(3) 0.8473(5) 0.025(2) Uani 1 1 d . . . O8 O 0.4036(10) 0.4232(3) 0.4414(4) 0.032(2) Uani 1 1 d . . . O12 O 0.7100(10) 0.0701(3) 0.3389(5) 0.031(2) Uani 1 1 d . . . O2W O 0.9607(8) 0.0213(3) 0.5939(5) 0.029(2) Uani 1 1 d . . . H10D H 0.9923 0.0438 0.5696 0.035 Uiso 1 1 calc R . . H10E H 1.0120 -0.0009 0.6276 0.035 Uiso 1 1 d R . . O4 O 0.6500(10) -0.4424(3) 0.7420(5) 0.033(2) Uani 1 1 d . . . O10 O 0.3963(12) 0.2453(3) 0.6614(4) 0.045(3) Uani 1 1 d . . . O14 O 0.8248(9) 0.4475(3) 0.2693(5) 0.036(3) Uani 1 1 d . . . C16 C 0.3633(12) 0.1163(4) 0.5596(5) 0.010(3) Uani 1 1 d . . . C38 C 0.7802(15) 0.3587(5) 0.4157(7) 0.031(4) Uani 1 1 d . . . H38A H 0.6959 0.3699 0.4409 0.038 Uiso 1 1 calc R . . C42 C 0.7737(15) 0.4289(5) 0.3313(7) 0.023(3) Uani 1 1 d . . . C32 C 0.9997(16) 0.1835(6) 0.4767(8) 0.048(4) Uani 1 1 d . . . H32A H 1.0700 0.1897 0.5181 0.057 Uiso 1 1 calc R . . C3 C 0.7001(17) -0.1403(5) 0.6614(7) 0.041(4) Uani 1 1 d . . . H3A H 0.7421 -0.1322 0.6129 0.050 Uiso 1 1 calc R . . C10 C 0.5567(16) -0.3537(5) 0.7100(7) 0.037(4) Uani 1 1 d . . . H10A H 0.5265 -0.3767 0.6741 0.044 Uiso 1 1 calc R . . C12 C 0.6949(16) -0.3295(6) 0.8272(8) 0.044(4) Uiso 1 1 d . . . H12A H 0.7624 -0.3352 0.8700 0.053 Uiso 1 1 calc R . . C6 C 0.5727(18) -0.1673(7) 0.8023(9) 0.059(5) Uiso 1 1 d . . . H6A H 0.5283 -0.1762 0.8498 0.070 Uiso 1 1 calc R . . C4 C 0.6311(16) -0.1821(6) 0.6695(8) 0.052(4) Uiso 1 1 d . . . H4A H 0.6302 -0.2027 0.6266 0.063 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 Dy1 0.0320(5) 0.0186(5) 0.0237(4) -0.0002(3) -0.0015(3) -0.0037(4) Dy2 0.0212(5) 0.0172(5) 0.0181(4) 0.0001(3) -0.0002(3) -0.0029(3) O6 0.027(5) 0.006(5) 0.018(4) -0.001(4) 0.002(4) 0.002(4) O1 0.043(6) 0.020(6) 0.027(5) 0.001(5) -0.006(5) -0.022(5) O11 0.024(5) 0.024(6) 0.028(5) 0.007(5) 0.000(4) 0.000(5) O1W 0.028(6) 0.025(6) 0.021(4) 0.011(4) 0.008(4) -0.002(5) O16 0.024(6) 0.032(7) 0.054(6) -0.020(5) 0.005(5) -0.017(6) O3W 0.024(6) 0.059(8) 0.060(6) -0.028(6) 0.005(5) -0.028(6) O15 0.031(6) 0.012(6) 0.090(7) 0.013(6) -0.034(5) -0.003(5) C14 0.017(8) 0.018(9) 0.020(7) 0.002(7) 0.002(6) 0.013(7) C25 0.020(7) 0.009(8) 0.011(6) 0.000(6) 0.004(5) 0.003(7) C36 0.016(8) 0.015(10) 0.071(10) -0.017(9) -0.017(8) 0.005(8) C22 0.067(11) 0.015(9) 0.014(7) -0.002(7) -0.011(7) -0.006(8) C1 0.034(9) 0.006(8) 0.026(8) 0.004(7) -0.001(7) -0.003(7) C43 0.026(10) 0.042(12) 0.029(8) -0.008(9) 0.006(8) 0.006(9) C33 0.019(8) 0.025(10) 0.046(8) -0.001(8) -0.018(7) -0.002(8) C31 0.053(10) 0.017(10) 0.041(8) 0.019(7) -0.021(8) -0.008(8) C35 0.035(9) 0.024(10) 0.033(7) -0.001(7) -0.023(7) -0.010(8) C45 0.031(10) 0.034(12) 0.118(14) 0.023(11) -0.013(10) -0.023(9) C40 0.041(9) 0.024(10) 0.036(8) -0.001(7) 0.009(7) -0.002(8) C2 0.024(8) 0.017(9) 0.024(7) 0.006(7) -0.006(6) 0.010(7) N2 0.044(9) 0.046(10) 0.056(8) 0.020(7) -0.015(7) 0.007(8) C24 0.034(8) 0.021(10) 0.018(6) 0.001(7) -0.015(6) 0.004(8) C7 0.069(11) 0.023(10) 0.029(8) 0.000(7) 0.008(8) -0.019(9) C37 0.028(9) 0.038(11) 0.055(9) 0.014(8) -0.026(8) -0.005(9) C23 0.044(9) 0.014(9) 0.033(8) -0.007(7) -0.008(7) -0.002(8) C27 0.074(11) 0.023(10) 0.018(7) 0.000(7) -0.027(7) -0.001(9) C18 0.031(8) 0.012(8) 0.029(7) 0.006(6) -0.004(6) -0.011(7) C20 0.041(9) 0.039(11) 0.018(6) -0.001(7) 0.007(6) 0.014(8) C29 0.027(8) 0.022(9) 0.021(8) 0.006(7) 0.007(7) 0.012(7) N1 0.041(9) 0.054(10) 0.038(7) 0.028(7) 0.012(6) 0.020(8) C41 0.019(8) 0.027(10) 0.047(8) 0.000(8) -0.007(7) -0.002(8) C44 0.041(10) 0.078(15) 0.050(10) 0.013(10) 0.023(9) -0.013(11) C30 0.007(7) 0.026(9) 0.012(6) 0.003(6) -0.005(5) -0.004(7) C9 0.039(9) 0.022(10) 0.029(7) 0.002(7) -0.014(7) 0.001(8) O2 0.036(6) 0.030(7) 0.022(5) 0.005(5) 0.011(4) 0.002(5) O13 0.030(5) 0.020(6) 0.033(5) 0.007(5) 0.010(4) 0.008(5) O3 0.023(5) 0.016(6) 0.034(5) 0.011(4) -0.014(4) 0.002(4) O8 0.054(6) 0.018(6) 0.024(5) 0.003(4) 0.010(4) 0.000(5) O12 0.044(6) 0.027(7) 0.022(5) 0.004(4) -0.002(4) -0.013(5) O2W 0.010(5) 0.041(7) 0.035(5) 0.020(5) 0.002(4) -0.006(5) O4 0.054(7) 0.013(6) 0.031(5) -0.005(5) -0.010(5) 0.005(5) O10 0.103(9) 0.011(6) 0.021(5) 0.004(4) -0.008(5) -0.011(6) O14 0.036(6) 0.027(7) 0.044(6) 0.019(5) 0.020(5) 0.010(5) C16 0.019(7) 0.006(7) 0.005(5) -0.001(5) -0.002(5) 0.003(6) C38 0.031(9) 0.021(10) 0.043(8) -0.006(7) 0.003(7) 0.002(8) C42 0.028(9) 0.018(9) 0.023(7) 0.008(7) -0.003(7) 0.003(8) C32 0.047(11) 0.044(13) 0.048(8) 0.009(9) -0.038(8) -0.002(9) C3 0.063(11) 0.034(11) 0.027(8) 0.011(8) -0.006(7) -0.016(9) C10 0.067(11) 0.013(9) 0.028(7) -0.003(7) -0.012(7) 0.016(8) _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 O4 2.278(9) 2_656 ? Dy1 O9 2.273(9) 2_646 ? Dy1 O16 2.298(10) . ? Dy1 O1 2.308(9) . ? Dy1 O8 2.382(8) 4_666 ? Dy1 O13 2.404(9) 4_666 ? Dy1 O3W 2.467(9) . ? Dy2 O11 2.280(8) . ? Dy2 O2 2.330(9) . ? Dy2 O3 2.342(8) 2_656 ? Dy2 O2W 2.416(7) . ? Dy2 O1W 2.441(8) . ? Dy2 O7 2.489(8) 3_656 ? Dy2 O6 2.511(8) . ? Dy2 O6 2.542(8) 3_656 ? Dy2 C15 2.909(12) 3_656 ? O6 C15 1.280(13) . ? O6 Dy2 2.542(8) 3_656 ? O1 C1 1.262(14) . ? O11 C29 1.270(14) . ? O7 C15 1.262(13) . ? O7 Dy2 2.489(8) 3_656 ? O16 C43 1.240(17) . ? O15 C33 1.353(16) . ? O15 C36 1.380(16) . ? C14 O3 1.256(13) . ? C14 O4 1.258(15) . ? C14 C11 1.452(18) . ? C25 C24 1.352(17) . ? C25 C26 1.398(16) . ? C25 C28 1.451(17) . ? C36 C41 1.356(19) . ? C36 C37 1.374(19) . ? C22 C27 1.353(18) . ? C22 O10 1.368(15) . ? C22 C23 1.387(16) . ? C39 C40 1.359(17) . ? C39 C38 1.385(17) . ? C39 C42 1.493(18) . ? C19 C20 1.366(18) . ? C19 O10 1.381(16) . ? C19 C18 1.390(16) . ? C1 O2 1.240(14) . ? C1 C2 1.466(18) . ? C43 N1 1.305(18) . ? C43 N2 1.329(17) . ? C33 C32 1.360(19) . ? C33 C34 1.378(17) . ? C15 C16 1.476(16) . ? C15 Dy2 2.909(12) 3_656 ? C31 C32 1.36(2) . ? C31 C30 1.359(17) . ? C11 C10 1.384(17) . ? C11 C12 1.395(19) . ? C35 C34 1.348(19) . ? C35 C30 1.393(18) . ? C45 N2 1.441(18) . ? C45 C44 1.50(2) . ? C40 C41 1.373(19) . ? C2 C7 1.366(16) . ? C2 C3 1.390(18) . ? C24 C23 1.371(18) . ? C7 C6 1.38(2) . ? C37 C38 1.412(19) . ? C28 O9 1.263(14) . ? C28 O8 1.265(13) . ? C21 C20 1.343(18) . ? C21 C16 1.387(15) . ? C27 C26 1.362(19) . ? C18 C17 1.364(17) . ? C29 O12 1.251(14) . ? C29 C30 1.475(18) . ? C17 C16 1.349(16) . ? N1 C44 1.420(18) . ? O5 C5 1.403(18) . ? O5 C8 1.430(19) . ? C8 C9 1.328(19) . ? C8 C13 1.35(2) . ? C9 C10 1.365(18) . ? C13 C12 1.37(2) . ? C5 C4 1.313(17) . ? C5 C6 1.35(2) . ? O9 Dy1 2.273(9) 2_656 ? O13 C42 1.240(14) . ? O13 Dy1 2.404(9) 4_565 ? O3 Dy2 2.342(8) 2_646 ? O8 Dy1 2.382(8) 4_565 ? O4 Dy1 2.278(9) 2_646 ? O14 C42 1.263(14) . ? C3 C4 1.37(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Dy1 O9 168.3(3) 2_656 2_646 ? O4 Dy1 O16 91.9(3) 2_656 . ? O9 Dy1 O16 86.2(3) 2_646 . ? O4 Dy1 O1 84.0(3) 2_656 . ? O9 Dy1 O1 84.4(3) 2_646 . ? O16 Dy1 O1 75.0(3) . . ? O4 Dy1 O8 84.0(3) 2_656 4_666 ? O9 Dy1 O8 106.2(3) 2_646 4_666 ? O16 Dy1 O8 70.7(3) . 4_666 ? O1 Dy1 O8 143.1(3) . 4_666 ? O4 Dy1 O13 93.6(3) 2_656 4_666 ? O9 Dy1 O13 95.3(3) 2_646 4_666 ? O16 Dy1 O13 140.3(3) . 4_666 ? O1 Dy1 O13 144.7(3) . 4_666 ? O8 Dy1 O13 70.9(3) 4_666 4_666 ? O4 Dy1 O3W 82.2(3) 2_656 . ? O9 Dy1 O3W 93.4(3) 2_646 . ? O16 Dy1 O3W 148.6(3) . . ? O1 Dy1 O3W 73.7(3) . . ? O8 Dy1 O3W 138.4(3) 4_666 . ? O13 Dy1 O3W 71.1(3) 4_666 . ? O11 Dy2 O2 139.8(3) . . ? O11 Dy2 O3 89.1(3) . 2_656 ? O2 Dy2 O3 101.9(3) . 2_656 ? O11 Dy2 O2W 73.9(3) . . ? O2 Dy2 O2W 71.0(3) . . ? O3 Dy2 O2W 77.7(3) 2_656 . ? O11 Dy2 O1W 145.0(3) . . ? O2 Dy2 O1W 75.1(3) . . ? O3 Dy2 O1W 77.3(3) 2_656 . ? O2W Dy2 O1W 132.1(3) . . ? O11 Dy2 O7 80.5(3) . 3_656 ? O2 Dy2 O7 75.5(3) . 3_656 ? O3 Dy2 O7 158.8(3) 2_656 3_656 ? O2W Dy2 O7 81.7(3) . 3_656 ? O1W Dy2 O7 121.1(3) . 3_656 ? O11 Dy2 O6 74.3(3) . . ? O2 Dy2 O6 143.2(3) . . ? O3 Dy2 O6 89.3(3) 2_656 . ? O2W Dy2 O6 145.7(3) . . ? O1W Dy2 O6 73.4(3) . . ? O7 Dy2 O6 105.4(2) 3_656 . ? O11 Dy2 O6 105.5(3) . 3_656 ? O2 Dy2 O6 84.0(3) . 3_656 ? O3 Dy2 O6 149.8(3) 2_656 3_656 ? O2W Dy2 O6 131.4(3) . 3_656 ? O1W Dy2 O6 75.7(3) . 3_656 ? O7 Dy2 O6 51.4(2) 3_656 3_656 ? O6 Dy2 O6 70.2(3) . 3_656 ? O11 Dy2 C15 95.4(3) . 3_656 ? O2 Dy2 C15 76.1(3) . 3_656 ? O3 Dy2 C15 175.0(3) 2_656 3_656 ? O2W Dy2 C15 105.7(3) . 3_656 ? O1W Dy2 C15 97.6(3) . 3_656 ? O7 Dy2 C15 25.6(3) 3_656 3_656 ? O6 Dy2 C15 89.7(3) . 3_656 ? O6 Dy2 C15 26.1(3) 3_656 3_656 ? C15 O6 Dy2 131.4(6) . . ? C15 O6 Dy2 93.2(7) . 3_656 ? Dy2 O6 Dy2 109.8(3) . 3_656 ? C1 O1 Dy1 151.6(8) . . ? C29 O11 Dy2 156.1(8) . . ? C15 O7 Dy2 96.1(7) . 3_656 ? C43 O16 Dy1 140.1(9) . . ? C33 O15 C36 121.2(10) . . ? O3 C14 O4 122.9(12) . . ? O3 C14 C11 120.2(12) . . ? O4 C14 C11 116.8(11) . . ? C24 C25 C26 116.3(12) . . ? C24 C25 C28 123.4(10) . . ? C26 C25 C28 120.2(12) . . ? C41 C36 C37 117.7(14) . . ? C41 C36 O15 121.8(13) . . ? C37 C36 O15 120.2(14) . . ? C27 C22 O10 117.8(10) . . ? C27 C22 C23 118.2(13) . . ? O10 C22 C23 123.5(12) . . ? C40 C39 C38 118.4(13) . . ? C40 C39 C42 123.5(12) . . ? C38 C39 C42 118.2(11) . . ? C20 C19 O10 116.8(11) . . ? C20 C19 C18 119.6(13) . . ? O10 C19 C18 123.1(12) . . ? O2 C1 O1 125.0(12) . . ? O2 C1 C2 118.4(11) . . ? O1 C1 C2 116.6(11) . . ? O16 C43 N1 124.0(14) . . ? O16 C43 N2 127.1(15) . . ? N1 C43 N2 108.9(14) . . ? O15 C33 C32 119.2(12) . . ? O15 C33 C34 123.2(13) . . ? C32 C33 C34 117.5(14) . . ? O7 C15 O6 118.2(11) . . ? O7 C15 C16 122.1(11) . . ? O6 C15 C16 119.5(10) . . ? O7 C15 Dy2 58.3(6) . 3_656 ? O6 C15 Dy2 60.8(6) . 3_656 ? C16 C15 Dy2 167.9(7) . 3_656 ? C32 C31 C30 121.0(13) . . ? C10 C11 C12 117.3(13) . . ? C10 C11 C14 121.8(12) . . ? C12 C11 C14 120.9(12) . . ? C34 C35 C30 120.9(12) . . ? N2 C45 C44 101.7(12) . . ? C39 C40 C41 121.4(13) . . ? C7 C2 C3 116.3(13) . . ? C7 C2 C1 120.7(12) . . ? C3 C2 C1 122.9(11) . . ? C43 N2 C45 112.4(13) . . ? C25 C24 C23 123.4(11) . . ? C2 C7 C6 123.5(13) . . ? C36 C37 C38 121.0(14) . . ? O9 C28 O8 121.3(12) . . ? O9 C28 C25 121.6(10) . . ? O8 C28 C25 117.0(11) . . ? C35 C34 C33 121.1(14) . . ? C20 C21 C16 120.0(12) . . ? C24 C23 C22 119.3(13) . . ? C22 C27 C26 121.9(12) . . ? C17 C18 C19 118.4(12) . . ? C21 C20 C19 120.9(12) . . ? C27 C26 C25 120.9(13) . . ? O12 C29 O11 122.6(13) . . ? O12 C29 C30 120.7(11) . . ? O11 C29 C30 116.7(11) . . ? C16 C17 C18 121.9(12) . . ? C43 N1 C44 112.5(12) . . ? C36 C41 C40 122.1(13) . . ? N1 C44 C45 104.3(12) . . ? C31 C30 C35 117.5(12) . . ? C31 C30 C29 121.4(12) . . ? C35 C30 C29 121.1(10) . . ? C5 O5 C8 116.9(12) . . ? C9 C8 C13 122.2(17) . . ? C9 C8 O5 116.5(13) . . ? C13 C8 O5 119.8(15) . . ? C8 C9 C10 118.4(13) . . ? C8 C13 C12 120.2(17) . . ? C4 C5 C6 121.8(17) . . ? C4 C5 O5 122.3(14) . . ? C6 C5 O5 115.6(13) . . ? C1 O2 Dy2 149.9(9) . . ? C28 O9 Dy1 175.1(8) . 2_656 ? C42 O13 Dy1 139.7(7) . 4_565 ? C14 O3 Dy2 130.8(8) . 2_646 ? C28 O8 Dy1 127.2(9) . 4_565 ? C14 O4 Dy1 170.8(8) . 2_646 ? C22 O10 C19 121.4(9) . . ? C17 C16 C21 119.0(12) . . ? C17 C16 C15 121.8(10) . . ? C21 C16 C15 119.1(11) . . ? C39 C38 C37 119.5(12) . . ? O13 C42 O14 125.2(12) . . ? O13 C42 C39 119.5(11) . . ? O14 C42 C39 115.3(12) . . ? C31 C32 C33 121.9(13) . . ? C4 C3 C2 119.1(13) . . ? C9 C10 C11 122.3(13) . . ? C13 C12 C11 119.3(14) . . ? C5 C6 C7 116.7(15) . . ? C5 C4 C3 122.0(16) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.608 _refine_diff_density_min -1.606 _refine_diff_density_rms 0.207 data_6 _database_code_depnum_ccdc_archive 'CCDC 894567' #TrackingRef 'cec.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H36 Eu2 N2 O19' _chemical_formula_weight 1212.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9134(3) _cell_length_b 29.0448(10) _cell_length_c 16.6484(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.909(3) _cell_angle_gamma 90.00 _cell_volume 4307.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3973 _cell_measurement_theta_min 2.3865 _cell_measurement_theta_max 24.6261 _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.870 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 2.971 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.39426 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 12420 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0995 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 24.68 _reflns_number_total 5575 _reflns_number_gt 4570 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART(Bruker,1998) _computing_cell_refinement SMART _computing_data_reduction SAINT(Bruker,1998) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL (Bruker,1998)' _computing_publication_material SHELXL _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^)+(0.1000P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5575 _refine_ls_number_parameters 593 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1715 _refine_ls_wR_factor_gt 0.1560 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.078 _refine_ls_shift/su_mean 0.014 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 Eu1 Eu 0.44486(6) 0.011399(15) 0.85818(3) 0.0237(2) Uani 1 1 d . . . Eu2 Eu 0.19263(5) 0.014340(14) 0.56836(3) 0.0184(2) Uani 1 1 d . . . O8 O 0.7745(7) -0.4518(2) 0.9768(4) 0.0293(15) Uani 1 1 d . . . O11 O 0.2799(8) 0.0576(2) 0.4663(4) 0.0366(17) Uani 1 1 d . . . O4 O 0.1755(8) 0.4535(2) 0.7132(4) 0.0364(18) Uani 1 1 d . . . O3 O 0.2273(8) 0.4559(2) 0.8447(4) 0.0364(18) Uani 1 1 d . . . O1 O 0.3498(8) 0.0572(2) 0.7573(4) 0.0337(16) Uani 1 1 d . . . O9 O 0.5361(7) -0.4509(2) 0.9997(3) 0.0219(14) Uani 1 1 d . . . O16 O 0.2136(9) 0.0048(3) 0.9144(5) 0.050(2) Uani 1 1 d . . . O3W O -0.0163(8) 0.0027(2) 0.6570(4) 0.0366(18) Uani 1 1 d . . . H10F H 0.0155 0.0015 0.7037 0.044 Uiso 1 1 calc R . . H10G H -0.1171 0.0008 0.6350 0.044 Uiso 1 1 d R . . O6 O 0.5194(8) -0.0472(2) 0.9427(4) 0.0370(18) Uani 1 1 d . . . O15 O 0.5337(8) 0.2592(2) 0.4295(5) 0.056(2) Uani 1 1 d . . . C16 C 0.5736(10) -0.1267(3) 0.9479(5) 0.023(2) Uani 1 1 d . . . C36 C 0.4650(12) 0.2992(3) 0.4022(7) 0.039(3) Uani 1 1 d . . . C15 C 0.5613(10) -0.0811(3) 0.9843(5) 0.024(2) Uani 1 1 d . . . O1W O 0.6157(9) -0.0125(2) 0.7517(5) 0.051(2) Uani 1 1 d . . . H10B H 0.6630 -0.0354 0.7665 0.061 Uiso 1 1 calc R . . H10C H 0.6182 0.0047 0.7025 0.061 Uiso 1 1 d R . . C19 C 0.5912(13) -0.2139(3) 0.8801(5) 0.038(3) Uani 1 1 d . . . C1 C 0.2984(11) 0.0877(4) 0.7108(5) 0.032(3) Uani 1 1 d . . . C5 C 0.4494(11) 0.2233(4) 0.7492(6) 0.035(2) Uiso 1 1 d . . . C22 C 0.6187(12) -0.2961(3) 0.8782(5) 0.032(2) Uani 1 1 d . . . O5 O 0.5248(9) 0.2667(3) 0.7589(5) 0.066(2) Uiso 1 1 d . . . C43 C 0.1067(12) -0.0228(4) 0.9183(7) 0.042(3) Uani 1 1 d . . . O14 O 0.3264(9) 0.4480(2) 0.2688(5) 0.051(2) Uani 1 1 d . . . C29 C 0.2683(10) 0.0825(3) 0.4050(6) 0.029(2) Uani 1 1 d . . . C40 C 0.4691(11) 0.3659(3) 0.3185(6) 0.038(3) Uani 1 1 d . . . H40A H 0.5135 0.3826 0.2779 0.046 Uiso 1 1 calc R . . C39 C 0.3442(10) 0.3837(3) 0.3545(6) 0.028(2) Uani 1 1 d . . . C30 C 0.3360(9) 0.1301(3) 0.4109(5) 0.023(2) Uani 1 1 d . . . C34 C 0.3540(12) 0.2076(4) 0.3622(6) 0.046(3) Uani 1 1 d . . . H34A H 0.3225 0.2303 0.3261 0.056 Uiso 1 1 calc R . . C37 C 0.3440(13) 0.3158(4) 0.4395(7) 0.049(3) Uani 1 1 d . . . H37A H 0.3028 0.2989 0.4807 0.058 Uiso 1 1 calc R . . C27 C 0.5187(11) -0.3098(3) 0.9378(6) 0.032(2) Uani 1 1 d . . . H27A H 0.4473 -0.2897 0.9574 0.038 Uiso 1 1 calc R . . C24 C 0.7349(11) -0.3697(3) 0.8812(5) 0.030(2) Uani 1 1 d . . . H24A H 0.8091 -0.3894 0.8632 0.036 Uiso 1 1 calc R . . C33 C 0.4594(10) 0.2179(3) 0.4227(6) 0.034(2) Uani 1 1 d . . . C23 C 0.7212(12) -0.3262(3) 0.8507(5) 0.032(3) Uani 1 1 d . . . H23A H 0.7838 -0.3171 0.8101 0.039 Uiso 1 1 calc R . . C20 C 0.6548(11) -0.2065(3) 0.9545(6) 0.035(3) Uani 1 1 d . . . H20A H 0.7039 -0.2301 0.9825 0.041 Uiso 1 1 calc R . . C2 C 0.3478(10) 0.1358(3) 0.7239(5) 0.023(2) Uani 1 1 d . . . C18 C 0.5200(13) -0.1785(3) 0.8385(6) 0.046(3) Uani 1 1 d . . . H18A H 0.4779 -0.1838 0.7875 0.055 Uiso 1 1 calc R . . C21 C 0.6444(11) -0.1637(3) 0.9866(5) 0.037(3) Uani 1 1 d . . . H21A H 0.6873 -0.1588 1.0376 0.045 Uiso 1 1 calc R . . C6 C 0.4926(11) 0.1908(4) 0.8027(6) 0.042(3) Uani 1 1 d . . . H6A H 0.5545 0.1981 0.8469 0.050 Uiso 1 1 calc R . . C32 C 0.5003(13) 0.1845(3) 0.4777(7) 0.051(3) Uani 1 1 d . . . H32A H 0.5697 0.1910 0.5191 0.061 Uiso 1 1 calc R . . C14 C 0.2281(11) 0.4364(3) 0.7793(6) 0.029(2) Uani 1 1 d . . . C26 C 0.5326(11) -0.3543(3) 0.9652(6) 0.030(2) Uani 1 1 d . . . H26A H 0.4667 -0.3643 1.0037 0.036 Uiso 1 1 calc R . . C31 C 0.4376(14) 0.1411(4) 0.4710(7) 0.054(3) Uani 1 1 d . . . H31A H 0.4654 0.1187 0.5085 0.065 Uiso 1 1 calc R . . C41 C 0.5279(13) 0.3247(4) 0.3413(7) 0.048(3) Uani 1 1 d . . . H41A H 0.6116 0.3134 0.3158 0.057 Uiso 1 1 calc R . . C42 C 0.2779(10) 0.4285(3) 0.3302(6) 0.027(2) Uani 1 1 d . . . C13 C 0.3687(13) 0.3175(4) 0.8306(7) 0.060(3) Uiso 1 1 d . . . H13A H 0.3671 0.2969 0.8733 0.072 Uiso 1 1 calc R . . C7 C 0.4422(12) 0.1462(3) 0.7901(6) 0.040(3) Uani 1 1 d . . . H7A H 0.4713 0.1230 0.8259 0.048 Uiso 1 1 calc R . . C8 C 0.4342(11) 0.3060(4) 0.7633(6) 0.041(3) Uiso 1 1 d . . . N1 N -0.0135(10) -0.0251(3) 0.8674(6) 0.055(3) Uani 1 1 d . . . H1A H -0.0259 -0.0081 0.8254 0.065 Uiso 1 1 calc R . . N2 N 0.0945(11) -0.0550(3) 0.9752(5) 0.054(3) Uani 1 1 d . . . H2A H 0.1614 -0.0598 1.0127 0.065 Uiso 1 1 calc R . . C10 C 0.3518(13) 0.3749(4) 0.7014(6) 0.050(3) Uani 1 1 d . . . H10A H 0.3419 0.3937 0.6564 0.060 Uiso 1 1 calc R . . O2 O 0.2088(7) 0.0788(2) 0.6538(4) 0.0315(16) Uani 1 1 d . . . O2W O 0.4621(7) 0.0214(2) 0.5929(4) 0.0394(18) Uani 1 1 d . . . H10D H 0.4813 0.0197 0.6413 0.047 Uiso 1 1 calc R . . H10E H 0.5268 0.0253 0.5485 0.047 Uiso 1 1 d R . . O13 O 0.1769(7) 0.4453(2) 0.3722(4) 0.0353(17) Uani 1 1 d . . . O12 O 0.2082(8) 0.0699(2) 0.3387(4) 0.0365(17) Uani 1 1 d . . . O7 O 0.5950(8) -0.0770(2) 1.0580(4) 0.0381(18) Uani 1 1 d . . . O10 O 0.6028(9) -0.2547(2) 0.8389(4) 0.048(2) Uani 1 1 d . . . C25 C 0.6376(9) -0.3844(3) 0.9391(5) 0.017(2) Uani 1 1 d . . . C28 C 0.6513(10) -0.4317(3) 0.9720(5) 0.017(2) Uani 1 1 d . . . C11 C 0.2924(11) 0.3893(3) 0.7734(5) 0.025(2) Uani 1 1 d . . . C35 C 0.2961(12) 0.1640(3) 0.3555(6) 0.036(3) Uani 1 1 d . . . H35A H 0.2291 0.1570 0.3132 0.044 Uiso 1 1 calc R . . C38 C 0.2795(10) 0.3581(3) 0.4168(6) 0.031(2) Uani 1 1 d . . . H38A H 0.1955 0.3691 0.4424 0.037 Uiso 1 1 calc R . . C45 C -0.0430(12) -0.0805(4) 0.9667(7) 0.049(3) Uani 1 1 d . . . H45A H -0.1042 -0.0765 1.0133 0.059 Uiso 1 1 calc R . . H45B H -0.0237 -0.1130 0.9592 0.059 Uiso 1 1 calc R . . C12 C 0.3016(13) 0.3611(3) 0.8373(7) 0.050(3) Uani 1 1 d . . . H12A H 0.2635 0.3704 0.8860 0.060 Uiso 1 1 calc R . . C17 C 0.5113(13) -0.1358(4) 0.8721(6) 0.046(3) Uani 1 1 d . . . H17A H 0.4625 -0.1123 0.8437 0.055 Uiso 1 1 calc R . . C3 C 0.3060(13) 0.1705(4) 0.6710(7) 0.055(3) Uani 1 1 d . . . H3A H 0.2440 0.1642 0.6263 0.066 Uiso 1 1 calc R . . C9 C 0.4251(15) 0.3331(4) 0.6954(8) 0.063(4) Uani 1 1 d . . . H9A H 0.4666 0.3238 0.6476 0.076 Uiso 1 1 calc R . . C44 C -0.1185(14) -0.0595(5) 0.8920(9) 0.072(4) Uani 1 1 d . . . H44A H -0.1348 -0.0825 0.8505 0.087 Uiso 1 1 calc R . . H44B H -0.2141 -0.0457 0.9045 0.087 Uiso 1 1 calc R . . C4 C 0.3578(16) 0.2152(4) 0.6854(8) 0.075(4) Uani 1 1 d . . . H4A H 0.3291 0.2391 0.6510 0.090 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 Eu1 0.0313(4) 0.0156(3) 0.0239(3) -0.0007(2) -0.0026(3) -0.0031(2) Eu2 0.0221(3) 0.0135(3) 0.0192(3) -0.00058(19) -0.0019(2) -0.0029(2) O8 0.032(4) 0.022(4) 0.034(4) 0.011(3) 0.005(3) 0.002(3) O11 0.049(4) 0.026(4) 0.034(4) 0.021(4) -0.003(3) -0.006(3) O4 0.049(4) 0.022(4) 0.038(4) -0.001(3) -0.002(4) 0.014(4) O3 0.049(5) 0.033(4) 0.028(4) -0.012(3) 0.004(3) -0.003(4) O1 0.062(5) 0.014(3) 0.024(3) 0.005(3) -0.011(3) -0.008(3) O9 0.026(3) 0.024(3) 0.016(3) 0.005(3) 0.003(3) 0.001(3) O16 0.038(5) 0.039(4) 0.073(6) -0.014(4) 0.007(4) -0.004(4) O3W 0.039(4) 0.046(4) 0.025(4) -0.007(3) -0.003(3) -0.003(4) O6 0.042(4) 0.021(4) 0.047(4) -0.002(4) -0.009(4) 0.007(3) O15 0.054(5) 0.019(4) 0.093(6) 0.018(4) -0.038(5) -0.011(4) C16 0.034(5) 0.014(5) 0.022(5) 0.006(4) 0.011(4) 0.006(5) C36 0.041(7) 0.012(5) 0.063(7) -0.008(6) -0.021(6) -0.005(5) C15 0.025(5) 0.025(6) 0.020(5) -0.001(5) -0.003(4) -0.001(5) O1W 0.048(5) 0.052(5) 0.054(5) -0.006(4) 0.011(4) -0.013(4) C19 0.082(8) 0.017(5) 0.013(5) 0.003(4) -0.009(5) -0.002(5) C1 0.049(7) 0.032(6) 0.013(5) -0.002(5) 0.006(5) 0.001(5) C22 0.057(7) 0.010(5) 0.027(5) 0.002(5) -0.011(5) 0.000(5) C43 0.024(6) 0.044(7) 0.059(8) -0.020(7) 0.018(6) 0.006(6) O14 0.064(5) 0.037(4) 0.053(5) 0.021(4) 0.020(4) 0.012(4) C29 0.024(5) 0.021(6) 0.041(6) -0.001(5) 0.009(5) 0.003(4) C40 0.040(6) 0.028(6) 0.047(6) 0.007(5) 0.011(5) -0.004(5) C39 0.024(5) 0.022(5) 0.038(6) 0.000(5) 0.001(5) 0.004(5) C30 0.023(5) 0.029(6) 0.017(4) 0.004(4) -0.009(4) 0.004(4) C34 0.044(7) 0.033(7) 0.061(7) 0.019(6) -0.021(6) -0.005(6) C37 0.056(8) 0.025(6) 0.064(8) 0.009(6) -0.007(7) -0.021(6) C27 0.041(6) 0.017(5) 0.037(6) -0.008(5) -0.014(5) 0.003(5) C24 0.042(6) 0.018(5) 0.029(5) -0.003(5) 0.003(5) 0.002(5) C33 0.029(5) 0.021(6) 0.052(6) 0.009(5) -0.015(5) 0.001(5) C23 0.055(7) 0.026(6) 0.017(5) 0.003(5) 0.005(5) -0.014(6) C20 0.046(6) 0.020(6) 0.037(6) 0.003(5) -0.007(5) 0.021(5) C2 0.022(5) 0.020(5) 0.027(5) -0.010(4) -0.007(4) 0.002(4) C18 0.082(9) 0.023(6) 0.032(6) 0.003(5) -0.028(6) 0.006(6) C21 0.054(7) 0.029(6) 0.029(5) -0.005(5) -0.009(5) -0.003(6) C6 0.044(6) 0.041(7) 0.040(6) -0.007(6) -0.010(5) -0.015(6) C32 0.066(8) 0.029(6) 0.056(7) -0.008(6) -0.028(6) -0.008(6) C14 0.039(6) 0.016(6) 0.033(6) -0.011(5) 0.005(5) 0.000(5) C26 0.039(6) 0.018(5) 0.034(6) -0.003(5) 0.010(5) 0.005(5) C31 0.072(8) 0.025(6) 0.065(8) 0.012(6) -0.014(7) 0.008(6) C41 0.056(7) 0.029(6) 0.058(7) 0.005(6) 0.005(6) 0.006(6) C42 0.023(5) 0.019(5) 0.040(6) -0.003(5) 0.000(5) 0.002(5) C7 0.060(7) 0.031(6) 0.029(5) 0.003(5) -0.002(5) -0.024(6) N1 0.040(6) 0.058(7) 0.065(7) 0.031(6) -0.003(5) -0.007(5) N2 0.060(7) 0.062(7) 0.040(5) 0.036(5) 0.009(5) 0.003(6) C10 0.069(8) 0.043(7) 0.038(7) 0.016(6) 0.017(6) 0.009(7) O2 0.042(4) 0.025(4) 0.027(4) -0.007(3) -0.009(3) 0.005(3) O2W 0.027(4) 0.056(5) 0.035(4) 0.011(4) -0.004(3) -0.014(4) O13 0.035(4) 0.034(4) 0.038(4) 0.012(3) 0.013(3) 0.011(4) O12 0.047(4) 0.034(4) 0.027(4) 0.000(3) -0.003(3) -0.013(4) O7 0.048(4) 0.032(4) 0.035(4) -0.003(3) 0.008(4) 0.001(4) O10 0.104(6) 0.009(4) 0.031(4) 0.000(3) -0.008(4) 0.007(4) C25 0.012(4) 0.018(5) 0.021(5) -0.002(4) -0.008(4) -0.003(4) C28 0.020(5) 0.015(5) 0.018(4) -0.004(4) 0.004(4) -0.003(4) C11 0.039(6) 0.016(5) 0.019(5) 0.002(4) -0.009(5) 0.003(5) C35 0.051(7) 0.024(6) 0.033(6) 0.006(5) -0.019(5) 0.000(5) C38 0.028(5) 0.019(5) 0.046(6) -0.004(5) 0.002(5) 0.000(5) C45 0.035(6) 0.048(7) 0.065(8) -0.002(6) 0.018(6) -0.010(6) C12 0.082(9) 0.015(6) 0.052(7) -0.001(5) -0.010(7) 0.017(6) C17 0.074(8) 0.026(6) 0.037(6) 0.006(5) -0.019(6) 0.010(6) C3 0.071(8) 0.026(6) 0.065(8) 0.010(6) -0.044(7) 0.001(6) C9 0.088(10) 0.031(7) 0.072(9) -0.006(6) 0.024(8) 0.021(7) C44 0.038(7) 0.079(10) 0.100(11) 0.012(9) -0.002(8) -0.006(8) C4 0.110(11) 0.025(7) 0.086(9) 0.012(7) -0.056(9) 0.008(7) _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 Eu1 O1 2.282(6) . ? Eu1 O6 2.293(7) . ? Eu1 O16 2.300(8) . ? Eu1 O4 2.303(6) 2_546 ? Eu1 O7 2.394(7) 3_657 ? Eu1 O13 2.425(6) 4_666 ? Eu1 O1W 2.475(7) . ? Eu2 O11 2.271(6) . ? Eu2 O3 2.328(7) 2_546 ? Eu2 O2 2.354(6) . ? Eu2 O2W 2.431(6) . ? Eu2 O3W 2.438(7) . ? Eu2 O8 2.496(6) 4 ? Eu2 O9 2.511(6) 2_556 ? Eu2 O9 2.558(6) 4 ? Eu2 C28 2.904(9) 4 ? Eu2 Eu2 4.1407(9) 3_556 ? O8 C28 1.244(10) . ? O8 Eu2 2.496(6) 4_656 ? O11 C29 1.253(11) . ? O4 C14 1.281(11) . ? O4 Eu1 2.303(6) 2_556 ? O3 C14 1.228(11) . ? O3 Eu2 2.328(7) 2_556 ? O1 C1 1.255(11) . ? O9 C28 1.269(10) . ? O9 Eu2 2.511(6) 2_546 ? O9 Eu2 2.558(6) 4_656 ? O16 C43 1.250(12) . ? O6 C15 1.252(11) . ? O15 C33 1.372(11) . ? O15 C36 1.384(12) . ? C16 C17 1.387(13) . ? C16 C21 1.394(12) . ? C16 C15 1.463(12) . ? C36 C37 1.351(15) . ? C36 C41 1.389(15) . ? C15 O7 1.259(10) . ? C19 C20 1.362(12) . ? C19 O10 1.374(11) . ? C19 C18 1.383(13) . ? C1 O2 1.246(10) . ? C1 C2 1.478(14) . ? C5 C4 1.339(14) . ? C5 C6 1.345(14) . ? C5 O5 1.435(12) . ? C22 C23 1.355(13) . ? C22 O10 1.376(10) . ? C22 C27 1.413(14) . ? O5 C8 1.402(13) . ? C43 N2 1.338(14) . ? C43 N1 1.345(14) . ? O14 C42 1.258(11) . ? C29 O12 1.266(11) . ? C29 C30 1.509(13) . ? C40 C41 1.356(14) . ? C40 C39 1.381(13) . ? C39 C38 1.415(13) . ? C39 C42 1.479(13) . ? C30 C31 1.364(14) . ? C30 C35 1.388(12) . ? C34 C35 1.371(14) . ? C34 C33 1.387(13) . ? C37 C38 1.402(14) . ? C27 C26 1.374(13) . ? C24 C23 1.365(13) . ? C24 C25 1.386(12) . ? C33 C32 1.376(13) . ? C20 C21 1.358(13) . ? C2 C3 1.382(13) . ? C2 C7 1.398(12) . ? C18 C17 1.364(14) . ? C6 C7 1.387(13) . ? C32 C31 1.382(14) . ? C14 C11 1.488(13) . ? C26 C25 1.364(12) . ? C42 O13 1.257(11) . ? C13 C8 1.323(14) . ? C13 C12 1.405(15) . ? C8 C9 1.378(15) . ? N1 C44 1.439(15) . ? N2 C45 1.435(14) . ? C10 C9 1.382(15) . ? C10 C11 1.391(13) . ? O13 Eu1 2.425(6) 4_565 ? O7 Eu1 2.394(6) 3_657 ? C25 C28 1.481(12) . ? C28 Eu2 2.904(9) 4_656 ? C11 C12 1.343(13) . ? C45 C44 1.521(17) . ? C3 C4 1.396(15) . ? 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 Eu1 O6 167.6(2) . . ? O1 Eu1 O16 91.8(3) . . ? O6 Eu1 O16 86.2(3) . . ? O1 Eu1 O4 83.7(2) . 2_546 ? O6 Eu1 O4 84.0(2) . 2_546 ? O16 Eu1 O4 75.0(3) . 2_546 ? O1 Eu1 O7 84.7(2) . 3_657 ? O6 Eu1 O7 106.2(2) . 3_657 ? O16 Eu1 O7 71.1(2) . 3_657 ? O4 Eu1 O7 143.7(2) 2_546 3_657 ? O1 Eu1 O13 93.6(2) . 4_666 ? O6 Eu1 O13 95.6(2) . 4_666 ? O16 Eu1 O13 141.0(2) . 4_666 ? O4 Eu1 O13 144.0(2) 2_546 4_666 ? O7 Eu1 O13 71.0(2) 3_657 4_666 ? O1 Eu1 O1W 81.9(3) . . ? O6 Eu1 O1W 93.4(3) . . ? O16 Eu1 O1W 148.1(2) . . ? O4 Eu1 O1W 73.3(2) 2_546 . ? O7 Eu1 O1W 138.4(2) 3_657 . ? O13 Eu1 O1W 70.8(2) 4_666 . ? O11 Eu2 O3 139.8(2) . 2_546 ? O11 Eu2 O2 89.8(2) . . ? O3 Eu2 O2 101.1(2) 2_546 . ? O11 Eu2 O2W 73.6(2) . . ? O3 Eu2 O2W 71.1(2) 2_546 . ? O2 Eu2 O2W 78.0(2) . . ? O11 Eu2 O3W 144.8(2) . . ? O3 Eu2 O3W 75.3(2) 2_546 . ? O2 Eu2 O3W 77.1(2) . . ? O2W Eu2 O3W 132.9(2) . . ? O11 Eu2 O8 80.3(2) . 4 ? O3 Eu2 O8 76.1(2) 2_546 4 ? O2 Eu2 O8 159.2(2) . 4 ? O2W Eu2 O8 81.7(2) . 4 ? O3W Eu2 O8 120.9(2) . 4 ? O11 Eu2 O9 74.5(2) . 2_556 ? O3 Eu2 O9 143.2(2) 2_546 2_556 ? O2 Eu2 O9 89.2(2) . 2_556 ? O2W Eu2 O9 145.6(2) . 2_556 ? O3W Eu2 O9 72.7(2) . 2_556 ? O8 Eu2 O9 105.5(2) 4 2_556 ? O11 Eu2 O9 105.0(2) . 4 ? O3 Eu2 O9 84.5(2) 2_546 4 ? O2 Eu2 O9 149.9(2) . 4 ? O2W Eu2 O9 131.0(2) . 4 ? O3W Eu2 O9 75.8(2) . 4 ? O8 Eu2 O9 50.88(19) 4 4 ? O9 Eu2 O9 70.4(2) 2_556 4 ? O11 Eu2 C28 94.8(2) . 4 ? O3 Eu2 C28 76.8(2) 2_546 4 ? O2 Eu2 C28 174.8(2) . 4 ? O2W Eu2 C28 105.6(2) . 4 ? O3W Eu2 C28 97.7(2) . 4 ? O8 Eu2 C28 25.2(2) 4 4 ? O9 Eu2 C28 89.8(2) 2_556 4 ? O9 Eu2 C28 25.9(2) 4 4 ? O11 Eu2 Eu2 89.90(17) . 3_556 ? O3 Eu2 Eu2 115.26(18) 2_546 3_556 ? O2 Eu2 Eu2 121.70(16) . 3_556 ? O2W Eu2 Eu2 154.91(17) . 3_556 ? O3W Eu2 Eu2 70.63(16) . 3_556 ? O8 Eu2 Eu2 76.81(14) 4 3_556 ? O9 Eu2 Eu2 35.59(13) 2_556 3_556 ? O9 Eu2 Eu2 34.85(13) 4 3_556 ? C28 Eu2 Eu2 56.11(17) 4 3_556 ? C28 O8 Eu2 96.1(5) . 4_656 ? C29 O11 Eu2 155.3(6) . . ? C14 O4 Eu1 151.3(6) . 2_556 ? C14 O3 Eu2 151.4(7) . 2_556 ? C1 O1 Eu1 170.1(6) . . ? C28 O9 Eu2 131.9(5) . 2_546 ? C28 O9 Eu2 92.5(5) . 4_656 ? Eu2 O9 Eu2 109.6(2) 2_546 4_656 ? C43 O16 Eu1 140.3(7) . . ? C15 O6 Eu1 175.7(6) . . ? C33 O15 C36 120.0(7) . . ? C17 C16 C21 115.8(8) . . ? C17 C16 C15 121.1(8) . . ? C21 C16 C15 123.1(8) . . ? C37 C36 C41 119.6(10) . . ? C37 C36 O15 119.9(11) . . ? C41 C36 O15 120.2(10) . . ? O6 C15 O7 121.4(9) . . ? O6 C15 C16 120.5(8) . . ? O7 C15 C16 118.1(8) . . ? C20 C19 O10 123.7(8) . . ? C20 C19 C18 120.6(9) . . ? O10 C19 C18 115.6(8) . . ? O2 C1 O1 122.3(9) . . ? O2 C1 C2 119.3(9) . . ? O1 C1 C2 118.5(8) . . ? C4 C5 C6 123.8(10) . . ? C4 C5 O5 120.9(10) . . ? C6 C5 O5 114.8(9) . . ? C23 C22 O10 117.7(9) . . ? C23 C22 C27 120.2(8) . . ? O10 C22 C27 121.5(9) . . ? C8 O5 C5 116.9(8) . . ? O16 C43 N2 124.4(11) . . ? O16 C43 N1 126.2(11) . . ? N2 C43 N1 109.4(10) . . ? O11 C29 O12 124.2(9) . . ? O11 C29 C30 117.0(9) . . ? O12 C29 C30 118.7(8) . . ? C41 C40 C39 121.2(10) . . ? C40 C39 C38 118.4(9) . . ? C40 C39 C42 122.0(9) . . ? C38 C39 C42 119.6(8) . . ? C31 C30 C35 118.1(9) . . ? C31 C30 C29 121.0(8) . . ? C35 C30 C29 120.8(8) . . ? C35 C34 C33 120.3(9) . . ? C36 C37 C38 121.0(10) . . ? C26 C27 C22 116.5(9) . . ? C23 C24 C25 119.5(9) . . ? O15 C33 C32 116.5(8) . . ? O15 C33 C34 124.2(9) . . ? C32 C33 C34 119.2(9) . . ? C22 C23 C24 121.7(9) . . ? C21 C20 C19 118.1(9) . . ? C3 C2 C7 119.2(9) . . ? C3 C2 C1 121.5(8) . . ? C7 C2 C1 119.2(8) . . ? C17 C18 C19 120.1(9) . . ? C20 C21 C16 124.0(9) . . ? C5 C6 C7 118.2(10) . . ? C33 C32 C31 119.6(10) . . ? O3 C14 O4 124.6(9) . . ? O3 C14 C11 119.8(9) . . ? O4 C14 C11 115.6(8) . . ? C25 C26 C27 123.6(9) . . ? C30 C31 C32 121.9(10) . . ? C40 C41 C36 120.9(11) . . ? O13 C42 O14 123.2(9) . . ? O13 C42 C39 118.5(9) . . ? O14 C42 C39 118.3(9) . . ? C8 C13 C12 119.6(12) . . ? C6 C7 C2 120.2(10) . . ? C13 C8 C9 122.3(11) . . ? C13 C8 O5 121.4(10) . . ? C9 C8 O5 116.1(9) . . ? C43 N1 C44 111.4(10) . . ? C43 N2 C45 112.3(10) . . ? C9 C10 C11 121.4(10) . . ? C1 O2 Eu2 130.5(6) . . ? C42 O13 Eu1 140.6(6) . 4_565 ? C15 O7 Eu1 127.5(6) . 3_657 ? C19 O10 C22 121.7(7) . . ? C26 C25 C24 118.4(8) . . ? C26 C25 C28 121.8(8) . . ? C24 C25 C28 119.8(8) . . ? O8 C28 O9 119.5(8) . . ? O8 C28 C25 121.4(8) . . ? O9 C28 C25 119.0(8) . . ? O8 C28 Eu2 58.7(4) . 4_656 ? O9 C28 Eu2 61.6(4) . 4_656 ? C25 C28 Eu2 167.8(6) . 4_656 ? C12 C11 C10 118.9(9) . . ? C12 C11 C14 121.5(9) . . ? C10 C11 C14 119.5(8) . . ? C34 C35 C30 120.9(9) . . ? C37 C38 C39 118.9(9) . . ? N2 C45 C44 103.1(9) . . ? C11 C12 C13 120.1(11) . . ? C18 C17 C16 121.3(9) . . ? C2 C3 C4 119.3(10) . . ? C10 C9 C8 117.2(11) . . ? N1 C44 C45 103.7(10) . . ? C5 C4 C3 119.2(10) . . ? _diffrn_measured_fraction_theta_max 0.761 _diffrn_reflns_theta_full 24.68 _diffrn_measured_fraction_theta_full 0.761 _refine_diff_density_max 1.795 _refine_diff_density_min -1.253 _refine_diff_density_rms 0.189 data_7 _database_code_depnum_ccdc_archive 'CCDC 894568' #TrackingRef 'cec.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H32 La2 N2 O18' _chemical_formula_weight 1166.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.0550(4) _cell_length_b 16.3958(3) _cell_length_c 29.0934(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8612.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9193 _cell_measurement_theta_min 2.3792 _cell_measurement_theta_max 25 _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4592 _exptl_absorpt_coefficient_mu 2.040 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.64619 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 22269 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.3792 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7580 _reflns_number_gt 5303 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART(Bruker,1998) _computing_cell_refinement SMART _computing_data_reduction SAINT(Bruker,1998) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL (Bruker,1998)' _computing_publication_material SHELXL _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^)+(0.1000P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7580 _refine_ls_number_parameters 608 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 0.580 _refine_ls_restrained_S_all 0.580 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.002 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 La1 La 0.310382(12) 0.220531(12) 0.005816(7) 0.01649(8) Uani 1 1 d . . . La2 La 0.162905(12) 0.424859(11) 0.001015(7) 0.01495(8) Uani 1 1 d . . . O4 O 0.21083(15) 0.65257(15) 0.46073(8) 0.0246(6) Uani 1 1 d . . . O9 O 0.19284(15) 0.30379(15) 0.46105(9) 0.0288(7) Uani 1 1 d . . . O14 O 0.40160(14) 0.47010(14) 0.45452(8) 0.0209(6) Uani 1 1 d . . . O1 O 0.12124(17) 0.50165(15) 0.06934(9) 0.0310(7) Uani 1 1 d . . . O12 O 0.34661(16) 0.33163(15) 0.06167(9) 0.0283(7) Uani 1 1 d . . . O11 O 0.27692(16) 0.44107(15) 0.05064(10) 0.0322(7) Uani 1 1 d . . . O16 O 0.25612(17) 0.06883(14) 0.00317(8) 0.0258(6) Uani 1 1 d . . . O6 O 0.17960(16) 0.29864(15) 0.04834(9) 0.0270(7) Uani 1 1 d . . . O10 O 0.09582(19) 0.36808(17) 0.25475(9) 0.0441(9) Uani 1 1 d . . . O1W O 0.02791(16) 0.39007(18) 0.01209(11) 0.0338(7) Uani 1 1 d . . . H1WA H 0.0219 0.3409 0.0085 0.051 Uiso 1 1 calc R . . C20 C 0.3224(2) 0.3998(2) 0.07366(13) 0.0188(8) Uani 1 1 d . . . C21 C 0.4036(2) 0.4987(2) 0.28553(13) 0.0291(10) Uani 1 1 d . . . O13 O 0.34947(17) 0.35265(15) 0.43345(9) 0.0282(7) Uani 1 1 d . . . O8 O 0.12874(15) 0.19041(15) 0.44748(9) 0.0275(6) Uani 1 1 d . . . O15 O 0.4142(2) 0.53449(18) 0.24293(9) 0.0556(10) Uani 1 1 d . . . O7 O 0.23781(17) 0.19465(16) 0.07953(9) 0.0318(7) Uani 1 1 d . . . C26 C 0.4283(2) 0.5146(2) 0.36531(12) 0.0239(9) Uani 1 1 d . . . H26A H 0.4498 0.5440 0.3892 0.029 Uiso 1 1 calc R . . C27 C 0.1549(2) 0.2582(2) 0.43531(13) 0.0199(8) Uani 1 1 d . . . C28 C 0.0773(2) 0.3482(2) 0.17637(13) 0.0279(9) Uani 1 1 d . . . H28A H 0.0328 0.3763 0.1795 0.034 Uiso 1 1 calc R . . C29 C 0.3786(2) 0.4198(2) 0.42408(13) 0.0195(8) Uani 1 1 d . . . O2 O 0.10910(15) 0.63049(15) 0.04724(8) 0.0252(6) Uani 1 1 d . . . C32 C 0.1402(2) 0.2868(2) 0.38739(13) 0.0229(9) Uani 1 1 d . . . C33 C 0.1101(2) 0.6042(2) 0.12661(12) 0.0198(8) Uani 1 1 d . . . C34 C 0.3573(2) 0.4017(2) 0.33889(13) 0.0269(9) Uani 1 1 d . . . H34A H 0.3313 0.3539 0.3448 0.032 Uiso 1 1 calc R . . C35 C 0.1902(2) 0.6320(2) 0.38099(13) 0.0230(9) Uani 1 1 d . . . C36 C 0.3903(3) 0.4967(2) 0.20268(14) 0.0370(11) Uani 1 1 d . . . C37 C 0.3480(2) 0.4341(2) 0.11876(13) 0.0199(8) Uani 1 1 d . . . C38 C 0.1824(3) 0.2844(3) 0.21124(15) 0.0427(12) Uani 1 1 d . . . H38A H 0.2096 0.2714 0.2374 0.051 Uiso 1 1 calc R . . O3 O 0.26525(17) 0.54828(16) 0.42781(9) 0.0367(8) Uani 1 1 d . . . C40 C 0.1010(2) 0.6579(3) 0.21564(14) 0.0332(10) Uani 1 1 d . . . C41 C 0.1270(2) 0.6798(2) 0.37876(13) 0.0274(9) Uani 1 1 d . . . H41A H 0.1072 0.7015 0.4056 0.033 Uiso 1 1 calc R . . C42 C 0.1194(2) 0.5505(2) 0.16238(13) 0.0254(9) Uani 1 1 d . . . H42A H 0.1290 0.4959 0.1561 0.031 Uiso 1 1 calc R . . O5 O 0.0879(2) 0.6913(2) 0.25875(10) 0.0593(11) Uani 1 1 d . . . C45 C 0.0952(2) 0.6855(2) 0.13592(14) 0.0312(10) Uani 1 1 d . . . H45A H 0.0876 0.7221 0.1120 0.037 Uiso 1 1 calc R . . C46 C 0.1657(2) 0.2781(2) 0.12887(13) 0.0233(9) Uani 1 1 d . . . C47 C 0.1249(3) 0.6674(2) 0.29790(13) 0.0340(11) Uani 1 1 d . . . C48 C 0.1192(2) 0.3304(2) 0.21431(13) 0.0298(10) Uani 1 1 d . . . C104 C 0.1959(2) 0.2554(2) 0.08287(13) 0.0214(9) Uani 1 1 d . . . C50 C 0.2047(3) 0.2578(3) 0.16828(14) 0.0371(11) Uani 1 1 d . . . H50A H 0.2469 0.2256 0.1658 0.045 Uiso 1 1 calc R . . C51 C 0.3883(2) 0.4442(2) 0.37504(12) 0.0191(8) Uani 1 1 d . . . C52 C 0.1154(2) 0.3373(2) 0.29784(13) 0.0304(10) Uani 1 1 d . . . C53 C 0.1015(2) 0.3242(2) 0.13334(13) 0.0247(9) Uani 1 1 d . . . H53A H 0.0747 0.3390 0.1073 0.030 Uiso 1 1 calc R . . C54 C 0.2219(2) 0.6049(3) 0.34050(14) 0.0345(11) Uani 1 1 d . . . H54A H 0.2645 0.5731 0.3415 0.041 Uiso 1 1 calc R . . C103 C 0.2244(2) 0.6100(2) 0.42542(12) 0.0211(9) Uani 1 1 d . . . C58 C 0.4362(2) 0.5413(2) 0.32072(12) 0.0245(9) Uani 1 1 d . . . H58A H 0.4637 0.5880 0.3145 0.029 Uiso 1 1 calc R . . C60 C 0.0917(3) 0.7115(2) 0.18079(14) 0.0343(11) Uani 1 1 d . . . H60A H 0.0830 0.7663 0.1872 0.041 Uiso 1 1 calc R . . C62 C 0.0971(3) 0.2601(3) 0.31075(15) 0.0492(14) Uani 1 1 d . . . H62A H 0.0766 0.2240 0.2896 0.059 Uiso 1 1 calc R . . C63 C 0.1907(3) 0.6246(3) 0.29865(14) 0.0420(12) Uani 1 1 d . . . H63A H 0.2137 0.6093 0.2714 0.050 Uiso 1 1 calc R . . C65 C 0.4129(3) 0.4099(2) 0.13890(15) 0.0354(11) Uani 1 1 d . . . H65A H 0.4427 0.3717 0.1242 0.042 Uiso 1 1 calc R . . C68 C 0.3261(3) 0.5227(3) 0.18274(17) 0.0510(14) Uani 1 1 d . . . H68A H 0.2965 0.5610 0.1975 0.061 Uiso 1 1 calc R . . C69 C 0.4349(3) 0.4415(3) 0.18111(16) 0.0442(13) Uani 1 1 d . . . H69A H 0.4794 0.4253 0.1944 0.053 Uiso 1 1 calc R . . C70 C 0.3054(2) 0.4918(3) 0.14074(16) 0.0443(13) Uani 1 1 d . . . H70A H 0.2620 0.5102 0.1270 0.053 Uiso 1 1 calc R . . C71 C 0.1149(3) 0.5763(2) 0.20751(15) 0.0377(12) Uani 1 1 d . . . H71A H 0.1210 0.5398 0.2317 0.045 Uiso 1 1 calc R . . C72 C 0.1469(3) 0.3894(3) 0.32828(16) 0.0507(14) Uani 1 1 d . . . H72A H 0.1598 0.4418 0.3192 0.061 Uiso 1 1 calc R . . C73 C 0.0931(3) 0.6955(2) 0.33765(14) 0.0315(10) Uani 1 1 d . . . H73A H 0.0490 0.7249 0.3367 0.038 Uiso 1 1 calc R . . C75 C 0.1095(3) 0.2360(2) 0.35555(15) 0.0424(13) Uani 1 1 d . . . H75A H 0.0964 0.1834 0.3643 0.051 Uiso 1 1 calc R . . C76 C 0.1597(3) 0.3642(3) 0.37282(16) 0.0459(14) Uani 1 1 d . . . H76A H 0.1819 0.4000 0.3935 0.055 Uiso 1 1 calc R . . C79 C 0.3641(3) 0.4288(2) 0.29390(14) 0.0354(11) Uani 1 1 d . . . H79A H 0.3422 0.4001 0.2699 0.042 Uiso 1 1 calc R . . O17 O 0.44541(16) 0.26361(17) -0.00781(10) 0.0363(8) Uani 1 1 d . . . N2 N 0.4508(2) 0.3999(2) -0.02640(14) 0.0404(9) Uani 1 1 d . . . H2A H 0.4100 0.4167 -0.0144 0.049 Uiso 1 1 calc R . . C102 C 0.4788(2) 0.3241(2) -0.02158(15) 0.0322(10) Uani 1 1 d . . . N1 N 0.5497(2) 0.3251(2) -0.03510(16) 0.0547(12) Uani 1 1 d . . . H1A H 0.5778 0.2827 -0.0362 0.066 Uiso 1 1 calc R . . C101 C 0.4998(3) 0.4493(3) -0.0549(2) 0.0555(15) Uani 1 1 d . . . H10A H 0.5016 0.5054 -0.0443 0.067 Uiso 1 1 calc R . . H10B H 0.4849 0.4482 -0.0869 0.067 Uiso 1 1 calc R . . C100 C 0.5731(3) 0.4064(3) -0.0476(2) 0.0701(19) Uani 1 1 d . . . H10C H 0.6024 0.4060 -0.0756 0.084 Uiso 1 1 calc R . . H10D H 0.6014 0.4318 -0.0232 0.084 Uiso 1 1 calc R . . C31 C 0.1135(2) 0.5764(2) 0.07779(13) 0.0191(8) Uani 1 1 d . . . H1WB H 0.002(3) 0.427(2) 0.0208(15) 0.034(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.02148(14) 0.01557(12) 0.01243(12) -0.00048(8) -0.00056(9) 0.00353(9) La2 0.01850(13) 0.01496(13) 0.01139(12) -0.00035(8) -0.00023(9) 0.00158(9) O4 0.0306(16) 0.0285(14) 0.0148(13) -0.0033(11) -0.0040(12) 0.0042(13) O9 0.0336(17) 0.0270(14) 0.0258(15) 0.0012(12) -0.0101(14) -0.0061(14) O14 0.0228(14) 0.0265(13) 0.0134(13) -0.0018(11) 0.0003(11) 0.0035(12) O1 0.050(2) 0.0254(14) 0.0175(14) -0.0056(12) 0.0070(14) 0.0021(14) O12 0.0332(17) 0.0258(14) 0.0260(15) -0.0055(12) -0.0088(13) 0.0044(13) O11 0.0395(18) 0.0238(13) 0.0332(17) -0.0004(13) -0.0185(15) 0.0041(14) O16 0.0280(16) 0.0188(13) 0.0307(16) 0.0040(11) 0.0012(13) 0.0023(12) O6 0.0393(17) 0.0260(14) 0.0159(14) 0.0070(11) -0.0014(13) -0.0052(13) O10 0.072(2) 0.0475(17) 0.0130(15) 0.0055(13) 0.0049(15) 0.0270(18) O1W 0.0213(16) 0.0274(16) 0.053(2) -0.0088(15) 0.0104(15) -0.0026(14) C20 0.024(2) 0.0145(17) 0.017(2) 0.0012(15) -0.0033(16) -0.0011(17) C21 0.044(3) 0.026(2) 0.017(2) 0.0013(16) 0.0013(19) -0.001(2) O13 0.0445(19) 0.0208(14) 0.0191(14) 0.0016(11) 0.0065(13) -0.0019(13) O8 0.0287(16) 0.0284(14) 0.0253(15) 0.0112(12) -0.0052(13) -0.0083(13) O15 0.113(3) 0.0429(17) 0.0110(15) 0.0034(13) -0.0090(18) -0.035(2) O7 0.0410(18) 0.0295(14) 0.0248(15) 0.0020(12) 0.0089(14) 0.0063(15) C26 0.029(2) 0.030(2) 0.0122(19) -0.0031(16) -0.0018(17) -0.0042(19) C27 0.021(2) 0.0203(19) 0.019(2) 0.0038(16) -0.0012(17) 0.0009(18) C28 0.029(2) 0.033(2) 0.022(2) 0.0022(18) 0.0027(18) 0.008(2) C29 0.021(2) 0.0201(19) 0.018(2) 0.0036(15) 0.0056(16) 0.0059(17) O2 0.0335(16) 0.0293(14) 0.0128(13) 0.0007(11) 0.0038(12) -0.0073(13) C32 0.023(2) 0.0237(19) 0.022(2) 0.0022(16) 0.0003(17) 0.0018(18) C33 0.022(2) 0.0227(18) 0.0143(19) -0.0014(15) 0.0014(16) -0.0028(18) C34 0.039(3) 0.0221(19) 0.020(2) 0.0017(17) -0.0022(19) -0.009(2) C35 0.024(2) 0.025(2) 0.020(2) -0.0031(16) -0.0045(18) 0.0042(19) C36 0.065(3) 0.033(2) 0.014(2) 0.0015(18) -0.009(2) -0.016(2) C37 0.023(2) 0.0169(18) 0.019(2) -0.0017(15) -0.0033(17) -0.0034(17) C38 0.047(3) 0.061(3) 0.020(2) 0.008(2) -0.005(2) 0.022(3) O3 0.047(2) 0.0355(16) 0.0272(16) -0.0081(13) -0.0145(15) 0.0193(16) C40 0.036(3) 0.046(2) 0.018(2) -0.0081(19) -0.0031(19) 0.017(2) C41 0.035(3) 0.030(2) 0.018(2) -0.0044(17) 0.0036(18) 0.007(2) C42 0.031(2) 0.0234(19) 0.022(2) 0.0003(17) 0.0008(18) 0.007(2) O5 0.089(3) 0.076(2) 0.0122(16) -0.0141(15) -0.0154(17) 0.053(2) C45 0.051(3) 0.024(2) 0.019(2) 0.0021(17) 0.004(2) 0.006(2) C46 0.025(2) 0.0264(19) 0.019(2) 0.0072(17) 0.0041(16) 0.0042(19) C47 0.051(3) 0.036(2) 0.015(2) -0.0050(18) -0.009(2) 0.014(2) C48 0.041(3) 0.033(2) 0.016(2) 0.0042(17) 0.0074(19) 0.008(2) C104 0.025(2) 0.0206(19) 0.019(2) 0.0021(16) -0.0004(17) -0.0043(19) C50 0.037(3) 0.049(3) 0.026(2) 0.005(2) 0.003(2) 0.019(2) C51 0.021(2) 0.0226(18) 0.0138(19) 0.0004(15) 0.0031(16) 0.0019(17) C52 0.040(3) 0.036(2) 0.015(2) 0.0035(18) 0.0012(19) 0.012(2) C53 0.027(2) 0.030(2) 0.017(2) 0.0034(17) 0.0002(18) 0.0029(19) C54 0.031(2) 0.049(3) 0.024(2) -0.013(2) -0.0023(19) 0.014(2) C103 0.023(2) 0.0234(19) 0.017(2) -0.0031(16) -0.0022(17) 0.0007(18) C58 0.031(2) 0.024(2) 0.018(2) 0.0009(16) 0.0019(18) -0.0096(19) C60 0.054(3) 0.027(2) 0.022(2) -0.0069(17) 0.001(2) 0.007(2) C62 0.086(4) 0.044(3) 0.018(2) -0.001(2) -0.012(3) -0.014(3) C63 0.051(3) 0.061(3) 0.014(2) -0.010(2) -0.002(2) 0.018(3) C65 0.042(3) 0.025(2) 0.040(3) -0.0050(19) -0.013(2) 0.010(2) C68 0.050(3) 0.067(3) 0.036(3) -0.030(3) 0.010(2) 0.010(3) C69 0.062(4) 0.033(2) 0.037(3) -0.003(2) -0.031(3) 0.006(2) C70 0.030(3) 0.067(3) 0.036(3) -0.020(2) -0.005(2) 0.019(3) C71 0.051(3) 0.043(3) 0.019(2) 0.0040(19) -0.003(2) 0.020(2) C72 0.082(4) 0.035(2) 0.035(3) 0.018(2) -0.012(3) -0.021(3) C73 0.038(3) 0.031(2) 0.025(2) -0.0022(18) -0.007(2) 0.016(2) C75 0.070(4) 0.030(2) 0.026(2) 0.0066(19) -0.011(2) -0.016(2) C76 0.072(4) 0.035(2) 0.031(3) 0.009(2) -0.016(2) -0.025(3) C79 0.058(3) 0.028(2) 0.020(2) -0.0026(17) -0.006(2) -0.016(2) O17 0.0289(18) 0.0333(16) 0.0467(19) 0.0023(14) 0.0068(14) -0.0018(15) N2 0.031(2) 0.0290(18) 0.062(3) 0.0005(19) 0.006(2) 0.0008(18) C102 0.028(2) 0.031(2) 0.037(3) -0.001(2) 0.002(2) 0.001(2) N1 0.032(2) 0.039(2) 0.093(4) 0.022(2) 0.025(2) 0.008(2) C101 0.053(3) 0.036(3) 0.077(4) 0.011(3) 0.001(3) -0.007(3) C100 0.038(3) 0.051(3) 0.121(6) 0.021(3) 0.016(4) -0.009(3) C31 0.017(2) 0.023(2) 0.018(2) -0.0048(16) 0.0040(16) -0.0051(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O2 2.397(2) 8_655 ? La1 O4 2.489(2) 2_564 ? La1 O9 2.522(3) 7_565 ? La1 O13 2.524(2) 7_565 ? La1 O12 2.527(2) . ? La1 O7 2.549(3) . ? La1 O17 2.569(3) . ? La1 O16 2.674(2) . ? La1 O6 2.957(3) . ? La1 C104 3.102(4) . ? La2 O1 2.470(2) . ? La2 O14 2.480(2) 2_564 ? La2 O6 2.504(2) . ? La2 O1W 2.524(3) . ? La2 O8 2.525(2) 7_565 ? La2 O11 2.528(3) . ? La2 O3 2.532(3) 2_564 ? La2 O16 2.777(2) 8_665 ? La2 O4 2.861(3) 2_564 ? La2 C103 3.051(4) 2_564 ? O4 C103 1.266(4) . ? O4 La1 2.489(2) 2_565 ? O4 La2 2.861(3) 2_565 ? O9 C27 1.261(4) . ? O9 La1 2.522(3) 7_566 ? O14 C29 1.279(4) . ? O14 La2 2.480(2) 2_565 ? O1 C31 1.258(4) . ? O12 C20 1.250(4) . ? O11 C20 1.257(4) . ? O16 La2 2.777(2) 8_655 ? O6 C104 1.264(4) . ? O10 C48 1.394(5) . ? O10 C52 1.396(4) . ? C20 C37 1.500(5) . ? C21 C79 1.372(5) . ? C21 C58 1.372(5) . ? C21 O15 1.385(5) . ? O13 C29 1.251(4) . ? O13 La1 2.524(2) 7_566 ? O8 C27 1.258(4) . ? O8 La2 2.525(2) 7_566 ? O15 C36 1.394(5) . ? O7 C104 1.255(4) . ? C26 C58 1.376(5) . ? C26 C51 1.391(5) . ? C27 C32 1.495(5) . ? C28 C48 1.370(5) . ? C28 C53 1.383(5) . ? C29 C51 1.492(5) . ? O2 C31 1.258(4) . ? O2 La1 2.397(2) 8_665 ? C32 C75 1.364(5) . ? C32 C76 1.384(5) . ? C33 C42 1.374(5) . ? C33 C45 1.386(5) . ? C33 C31 1.493(5) . ? C34 C51 1.379(5) . ? C34 C79 1.388(5) . ? C35 C54 1.384(5) . ? C35 C41 1.386(5) . ? C35 C103 1.477(5) . ? C36 C69 1.364(6) . ? C36 C68 1.365(6) . ? C37 C65 1.370(5) . ? C37 C70 1.377(5) . ? C38 C48 1.371(6) . ? C38 C50 1.383(6) . ? O3 C103 1.255(4) . ? O3 La2 2.532(3) 2_565 ? C40 C60 1.353(6) . ? C40 C71 1.382(5) . ? C40 O5 1.389(4) . ? C41 C73 1.368(5) . ? C42 C71 1.382(6) . ? O5 C47 1.377(5) . ? C45 C60 1.375(5) . ? C46 C50 1.386(6) . ? C46 C53 1.390(5) . ? C46 C104 1.493(5) . ? C47 C73 1.371(6) . ? C47 C63 1.381(6) . ? C52 C72 1.355(6) . ? C52 C62 1.362(6) . ? C54 C63 1.380(6) . ? C103 La2 3.051(4) 2_565 ? C62 C75 1.380(6) . ? C65 C69 1.391(6) . ? C68 C70 1.374(6) . ? C72 C76 1.379(6) . ? O17 C102 1.228(5) . ? N2 C102 1.349(5) . ? N2 C101 1.458(6) . ? C102 N1 1.340(6) . ? N1 C100 1.446(6) . ? C101 C100 1.513(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La1 O4 150.82(9) 8_655 2_564 ? O2 La1 O9 132.28(8) 8_655 7_565 ? O4 La1 O9 74.37(8) 2_564 7_565 ? O2 La1 O13 87.54(8) 8_655 7_565 ? O4 La1 O13 90.05(8) 2_564 7_565 ? O9 La1 O13 74.29(9) 7_565 7_565 ? O2 La1 O12 87.92(8) 8_655 . ? O4 La1 O12 77.07(8) 2_564 . ? O9 La1 O12 131.60(8) 7_565 . ? O13 La1 O12 143.77(9) 7_565 . ? O2 La1 O7 77.66(9) 8_655 . ? O4 La1 O7 120.23(8) 2_564 . ? O9 La1 O7 88.60(9) 7_565 . ? O13 La1 O7 140.04(8) 7_565 . ? O12 La1 O7 73.26(9) . . ? O2 La1 O17 70.81(9) 8_655 . ? O4 La1 O17 80.50(9) 2_564 . ? O9 La1 O17 139.68(9) 7_565 . ? O13 La1 O17 74.73(9) 7_565 . ? O12 La1 O17 69.85(9) . . ? O7 La1 O17 131.57(9) . . ? O2 La1 O16 70.36(9) 8_655 . ? O4 La1 O16 134.90(8) 2_564 . ? O9 La1 O16 61.95(8) 7_565 . ? O13 La1 O16 68.67(8) 7_565 . ? O12 La1 O16 141.60(8) . . ? O7 La1 O16 71.40(8) . . ? O17 La1 O16 126.79(9) . . ? O2 La1 O6 122.73(8) 8_655 . ? O4 La1 O6 74.67(7) 2_564 . ? O9 La1 O6 67.21(8) 7_565 . ? O13 La1 O6 141.08(8) 7_565 . ? O12 La1 O6 68.01(8) . . ? O7 La1 O6 46.34(8) . . ? O17 La1 O6 134.69(8) . . ? O16 La1 O6 97.02(8) . . ? O2 La1 C104 98.88(9) 8_655 . ? O4 La1 C104 97.13(9) 2_564 . ? O9 La1 C104 80.90(9) 7_565 . ? O13 La1 C104 151.25(10) 7_565 . ? O12 La1 C104 64.83(9) . . ? O7 La1 C104 23.11(9) . . ? O17 La1 C104 133.87(9) . . ? O16 La1 C104 87.04(9) . . ? O6 La1 C104 23.93(8) . . ? O1 La2 O14 86.67(8) . 2_564 ? O1 La2 O6 90.89(8) . . ? O14 La2 O6 158.48(9) 2_564 . ? O1 La2 O1W 73.64(10) . . ? O14 La2 O1W 76.88(9) 2_564 . ? O6 La2 O1W 81.91(10) . . ? O1 La2 O8 143.44(9) . 7_565 ? O14 La2 O8 93.93(8) 2_564 7_565 ? O6 La2 O8 75.52(9) . 7_565 ? O1W La2 O8 70.96(9) . 7_565 ? O1 La2 O11 74.63(10) . . ? O14 La2 O11 128.37(8) 2_564 . ? O6 La2 O11 71.03(9) . . ? O1W La2 O11 137.49(10) . . ? O8 La2 O11 129.02(8) 7_565 . ? O1 La2 O3 138.08(9) . 2_564 ? O14 La2 O3 70.19(9) 2_564 2_564 ? O6 La2 O3 122.99(9) . 2_564 ? O1W La2 O3 129.89(10) . 2_564 ? O8 La2 O3 74.73(9) 7_565 2_564 ? O11 La2 O3 92.57(10) . 2_564 ? O1 La2 O16 73.08(8) . 8_665 ? O14 La2 O16 70.69(8) 2_564 8_665 ? O6 La2 O16 128.81(8) . 8_665 ? O1W La2 O16 134.23(9) . 8_665 ? O8 La2 O16 141.13(8) 7_565 8_665 ? O11 La2 O16 57.94(8) . 8_665 ? O3 La2 O16 66.52(8) 2_564 8_665 ? O1 La2 O4 143.00(9) . 2_564 ? O14 La2 O4 117.32(8) 2_564 2_564 ? O6 La2 O4 76.26(8) . 2_564 ? O1W La2 O4 136.19(9) . 2_564 ? O8 La2 O4 67.04(8) 7_565 2_564 ? O11 La2 O4 68.39(8) . 2_564 ? O3 La2 O4 47.50(8) 2_564 2_564 ? O16 La2 O4 88.10(8) 8_665 2_564 ? O1 La2 C103 151.50(10) . 2_564 ? O14 La2 C103 92.88(9) 2_564 2_564 ? O6 La2 C103 99.27(9) . 2_564 ? O1W La2 C103 133.95(10) . 2_564 ? O8 La2 C103 65.04(9) 7_565 2_564 ? O11 La2 C103 83.58(10) . 2_564 ? O3 La2 C103 23.73(9) 2_564 2_564 ? O16 La2 C103 79.89(9) 8_665 2_564 ? O4 La2 C103 24.45(8) 2_564 2_564 ? C103 O4 La1 156.7(2) . 2_565 ? C103 O4 La2 86.2(2) . 2_565 ? La1 O4 La2 106.12(9) 2_565 2_565 ? C27 O9 La1 132.1(2) . 7_566 ? C29 O14 La2 132.3(2) . 2_565 ? C31 O1 La2 133.4(2) . . ? C20 O12 La1 137.2(2) . . ? C20 O11 La2 141.2(2) . . ? La1 O16 La2 126.75(12) . 8_655 ? C104 O6 La2 158.2(2) . . ? C104 O6 La1 84.5(2) . . ? La2 O6 La1 102.95(9) . . ? C48 O10 C52 121.4(3) . . ? O12 C20 O11 124.1(3) . . ? O12 C20 C37 118.1(3) . . ? O11 C20 C37 117.7(3) . . ? C79 C21 C58 121.1(4) . . ? C79 C21 O15 125.8(4) . . ? C58 C21 O15 113.1(3) . . ? C29 O13 La1 135.9(2) . 7_566 ? C27 O8 La2 138.0(2) . 7_566 ? C21 O15 C36 121.4(3) . . ? C104 O7 La1 104.0(2) . . ? C58 C26 C51 120.6(3) . . ? O8 C27 O9 124.1(3) . . ? O8 C27 C32 118.3(3) . . ? O9 C27 C32 117.6(3) . . ? C48 C28 C53 119.6(4) . . ? O13 C29 O14 123.6(3) . . ? O13 C29 C51 119.5(3) . . ? O14 C29 C51 116.9(3) . . ? C31 O2 La1 138.6(3) . 8_665 ? C75 C32 C76 117.1(4) . . ? C75 C32 C27 120.9(3) . . ? C76 C32 C27 121.9(4) . . ? C42 C33 C45 119.5(4) . . ? C42 C33 C31 121.4(3) . . ? C45 C33 C31 119.2(3) . . ? C51 C34 C79 121.5(4) . . ? C54 C35 C41 118.9(4) . . ? C54 C35 C103 119.6(3) . . ? C41 C35 C103 121.6(3) . . ? C69 C36 C68 120.9(4) . . ? C69 C36 O15 119.9(4) . . ? C68 C36 O15 118.8(4) . . ? C65 C37 C70 118.6(4) . . ? C65 C37 C20 121.9(3) . . ? C70 C37 C20 119.5(4) . . ? C48 C38 C50 118.3(4) . . ? C103 O3 La2 102.0(2) . 2_565 ? C60 C40 C71 121.6(4) . . ? C60 C40 O5 113.6(4) . . ? C71 C40 O5 124.5(4) . . ? C73 C41 C35 121.1(4) . . ? C33 C42 C71 121.1(4) . . ? C47 O5 C40 123.6(3) . . ? C60 C45 C33 119.5(4) . . ? C50 C46 C53 118.5(4) . . ? C50 C46 C104 119.7(4) . . ? C53 C46 C104 121.6(3) . . ? C73 C47 O5 113.5(4) . . ? C73 C47 C63 121.2(4) . . ? O5 C47 C63 125.1(4) . . ? C28 C48 C38 121.6(4) . . ? C28 C48 O10 114.7(4) . . ? C38 C48 O10 123.4(4) . . ? O7 C104 O6 121.6(3) . . ? O7 C104 C46 119.2(3) . . ? O6 C104 C46 119.2(3) . . ? O7 C104 La1 52.85(19) . . ? O6 C104 La1 71.6(2) . . ? C46 C104 La1 159.7(3) . . ? C38 C50 C46 121.6(4) . . ? C34 C51 C26 118.3(3) . . ? C34 C51 C29 123.1(3) . . ? C26 C51 C29 118.5(3) . . ? C72 C52 C62 120.5(4) . . ? C72 C52 O10 117.7(4) . . ? C62 C52 O10 121.5(4) . . ? C28 C53 C46 120.2(4) . . ? C35 C54 C63 120.5(4) . . ? O3 C103 O4 120.9(3) . . ? O3 C103 C35 119.4(3) . . ? O4 C103 C35 119.7(3) . . ? O3 C103 La2 54.28(19) . 2_565 ? O4 C103 La2 69.3(2) . 2_565 ? C35 C103 La2 162.8(3) . 2_565 ? C21 C58 C26 119.8(4) . . ? C40 C60 C45 120.3(4) . . ? C52 C62 C75 119.2(4) . . ? C47 C63 C54 119.0(4) . . ? C37 C65 C69 120.9(4) . . ? C36 C68 C70 119.6(4) . . ? C36 C69 C65 119.0(4) . . ? C37 C70 C68 121.0(4) . . ? C40 C71 C42 118.0(4) . . ? C52 C72 C76 119.8(4) . . ? C41 C73 C47 119.1(4) . . ? C32 C75 C62 122.2(4) . . ? C72 C76 C32 121.3(4) . . ? C21 C79 C34 118.7(4) . . ? C102 O17 La1 137.6(3) . . ? C102 N2 C101 110.1(4) . . ? O17 C102 N1 125.0(4) . . ? O17 C102 N2 126.5(4) . . ? N1 C102 N2 108.5(4) . . ? C102 N1 C100 111.3(4) . . ? N2 C101 C100 101.1(4) . . ? N1 C100 C101 102.0(4) . . ? O1 C31 O2 123.7(3) . . ? O1 C31 C33 119.2(3) . . ? O2 C31 C33 117.1(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.463 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.082 data_8 _database_code_depnum_ccdc_archive 'CCDC 894569' #TrackingRef 'cec.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H36 O21 Sm2' _chemical_formula_weight 1177.43 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 23.4064(10) _cell_length_b 5.9565(2) _cell_length_c 33.4858(17) _cell_angle_alpha 90.00 _cell_angle_beta 121.375(3) _cell_angle_gamma 90.00 _cell_volume 3985.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6753 _cell_measurement_theta_min 2.4719 _cell_measurement_theta_max 23.5 _exptl_crystal_description sheet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.962 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 3.009 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.75285 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2083 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 14079 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.4719 _diffrn_reflns_theta_max 23.50 _reflns_number_total 5867 _reflns_number_gt 4479 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART(Bruker,1998) _computing_cell_refinement SMART _computing_data_reduction SAINT(Bruker,1998) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL (Bruker,1998)' _computing_publication_material SHELXL _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^)+(0.0380P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5867 _refine_ls_number_parameters 592 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.814 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.403461(16) -0.39995(5) 0.016108(10) 0.01232(10) Uani 1 1 d . . . Sm2 Sm -0.154122(16) -0.51630(5) -0.480550(11) 0.01332(10) Uani 1 1 d . . . O3 O -0.0962(2) -0.2025(7) -0.43491(14) 0.0256(11) Uani 1 1 d . . . O14 O 0.6445(2) 0.5249(7) 0.43444(13) 0.0214(11) Uani 1 1 d . . . O10 O 0.7646(3) -0.6626(9) 0.25501(14) 0.0491(16) Uani 1 1 d . . . O7 O 0.5765(2) -0.4469(7) 0.03940(14) 0.0259(12) Uani 1 1 d . . . O2 O 0.2042(2) -0.4661(7) -0.06670(13) 0.0201(10) Uani 1 1 d . . . O15 O 0.6062(2) -0.1027(8) 0.26756(14) 0.0360(13) Uani 1 1 d . . . O9 O 0.9394(2) -0.2020(8) 0.45108(15) 0.0265(11) Uani 1 1 d . . . O5 O 0.1085(2) 0.2170(7) -0.23596(13) 0.0320(12) Uani 1 1 d . . . O13 O 0.7410(2) 0.3388(7) 0.46705(13) 0.0189(10) Uani 1 1 d . . . O12 O 0.4602(2) 0.2657(7) 0.05910(14) 0.0245(11) Uani 1 1 d . . . O8 O 0.8623(2) -0.3512(8) 0.46190(15) 0.0283(12) Uani 1 1 d . . . O11 O 0.4010(2) -0.0430(6) 0.04930(13) 0.0160(10) Uani 1 1 d . . . O6 O 0.5181(2) -0.2955(7) 0.06696(13) 0.0177(10) Uani 1 1 d . . . O1 O 0.2960(2) -0.2595(7) -0.04132(13) 0.0198(10) Uani 1 1 d . . . C28 C 0.8858(3) -0.3069(11) 0.4364(2) 0.0220(16) Uani 1 1 d . . . C38 C 0.6631(3) 0.2684(10) 0.38708(19) 0.0142(14) Uani 1 1 d . . . C42 C 0.6828(3) 0.3870(10) 0.4319(2) 0.0164(15) Uani 1 1 d . . . C29 C 0.4874(3) 0.0566(9) 0.1268(2) 0.0130(14) Uani 1 1 d . . . C37 C 0.6956(3) 0.0731(10) 0.3876(2) 0.0194(16) Uani 1 1 d . . . H37A H 0.7312 0.0205 0.4158 0.023 Uiso 1 1 calc R . . C11 C 0.0113(3) -0.1015(11) -0.3458(2) 0.0235(16) Uani 1 1 d . . . H11A H 0.0129 -0.2348 -0.3597 0.028 Uiso 1 1 calc R . . C15 C 0.6263(3) -0.4387(10) 0.1220(2) 0.0155(15) Uani 1 1 d . . . C27 C 0.5696(3) -0.3903(10) 0.0727(2) 0.0153(14) Uani 1 1 d . . . O4 O -0.1420(2) 0.1325(7) -0.44217(13) 0.0183(10) Uani 1 1 d . . . C4 C 0.1381(3) 0.0704(10) -0.1983(2) 0.0188(16) Uani 1 1 d . . . C41 C 0.4469(3) 0.0951(11) 0.0754(2) 0.0181(15) Uani 1 1 d . . . C33 C 0.5758(3) 0.1619(11) 0.2039(2) 0.0241(17) Uani 1 1 d . . . H33A H 0.6090 0.2629 0.2236 0.029 Uiso 1 1 calc R . . C8 C 0.0055(3) 0.2905(11) -0.3048(2) 0.0248(17) Uani 1 1 d . . . H8A H 0.0037 0.4232 -0.2909 0.030 Uiso 1 1 calc R . . C5 C 0.1110(3) -0.1285(11) -0.1960(2) 0.0247(17) Uani 1 1 d . . . H5A H 0.0715 -0.1813 -0.2216 0.030 Uiso 1 1 calc R . . C10 C -0.0417(3) 0.0457(10) -0.3705(2) 0.0145(15) Uani 1 1 d . . . C9 C -0.0439(3) 0.2426(11) -0.3499(2) 0.0212(16) Uani 1 1 d . . . H9A H -0.0789 0.3432 -0.3666 0.025 Uiso 1 1 calc R . . C30 C 0.4765(3) -0.1350(11) 0.1456(2) 0.0243(17) Uani 1 1 d . . . H30A H 0.4424 -0.2336 0.1262 0.029 Uiso 1 1 calc R . . C35 C 0.6243(3) 0.0372(10) 0.3055(2) 0.0219(16) Uani 1 1 d . . . C13 C 0.2370(3) -0.3096(10) -0.07172(19) 0.0117(14) Uiso 1 1 d . . . C34 C 0.5364(3) 0.2047(11) 0.1564(2) 0.0213(16) Uani 1 1 d . . . H34A H 0.5432 0.3357 0.1443 0.026 Uiso 1 1 calc R . . C17 C 0.6834(3) -0.3779(12) 0.2051(2) 0.0284(18) Uani 1 1 d . . . H17A H 0.6899 -0.2928 0.2304 0.034 Uiso 1 1 calc R . . C1 C 0.2031(3) -0.1772(10) -0.11626(19) 0.0122(14) Uani 1 1 d . . . C25 C 0.8587(4) -0.2857(14) 0.3540(2) 0.042(2) Uani 1 1 d . . . H25A H 0.8878 -0.1644 0.3625 0.050 Uiso 1 1 calc R . . C16 C 0.6357(3) -0.3154(11) 0.1595(2) 0.0232(16) Uani 1 1 d . . . H16A H 0.6098 -0.1880 0.1544 0.028 Uiso 1 1 calc R . . C24 C 0.8475(3) -0.3808(11) 0.3862(2) 0.0199(15) Uani 1 1 d . . . C12 C 0.0619(3) -0.0508(11) -0.3006(2) 0.0262(18) Uani 1 1 d . . . H12A H 0.0983 -0.1465 -0.2843 0.031 Uiso 1 1 calc R . . C19 C 0.7138(3) -0.6895(12) 0.1748(2) 0.0317(18) Uani 1 1 d . . . H19A H 0.7401 -0.8159 0.1800 0.038 Uiso 1 1 calc R . . C36 C 0.6762(3) -0.0433(11) 0.3475(2) 0.0239(17) Uani 1 1 d . . . H36A H 0.6978 -0.1759 0.3484 0.029 Uiso 1 1 calc R . . C6 C 0.1435(3) -0.2506(11) -0.1546(2) 0.0218(16) Uani 1 1 d . . . H6A H 0.1249 -0.3849 -0.1526 0.026 Uiso 1 1 calc R . . C21 C 0.7870(4) -0.5506(13) 0.2970(2) 0.033(2) Uani 1 1 d . . . C22 C 0.7737(4) -0.6480(13) 0.3278(2) 0.043(2) Uani 1 1 d . . . H22A H 0.7452 -0.7713 0.3192 0.052 Uiso 1 1 calc R . . C3 C 0.1974(3) 0.1479(10) -0.1604(2) 0.0204(16) Uani 1 1 d . . . H3A H 0.2155 0.2836 -0.1624 0.024 Uiso 1 1 calc R . . C7 C 0.0574(3) 0.1441(11) -0.2802(2) 0.0229(17) Uani 1 1 d . . . C18 C 0.7204(3) -0.5667(11) 0.2118(2) 0.0252(17) Uani 1 1 d . . . C20 C 0.6671(3) -0.6208(11) 0.1297(2) 0.0234(16) Uani 1 1 d . . . H20A H 0.6633 -0.6985 0.1043 0.028 Uiso 1 1 calc R . . C39 C 0.6126(3) 0.3490(11) 0.3450(2) 0.0231(17) Uani 1 1 d . . . H39A H 0.5909 0.4813 0.3441 0.028 Uiso 1 1 calc R . . C26 C 0.8274(4) -0.3668(15) 0.3087(2) 0.048(2) Uani 1 1 d . . . H26A H 0.8338 -0.2968 0.2865 0.058 Uiso 1 1 calc R . . C23 C 0.8034(4) -0.5597(13) 0.3728(2) 0.036(2) Uani 1 1 d . . . H23A H 0.7936 -0.6215 0.3940 0.043 Uiso 1 1 calc R . . C31 C 0.5157(3) -0.1805(11) 0.1927(2) 0.0243(17) Uani 1 1 d . . . H31A H 0.5086 -0.3106 0.2049 0.029 Uiso 1 1 calc R . . C2 C 0.2296(3) 0.0239(10) -0.1200(2) 0.0182(15) Uani 1 1 d . . . H2A H 0.2697 0.0756 -0.0948 0.022 Uiso 1 1 calc R . . C40 C 0.5933(3) 0.2358(10) 0.3036(2) 0.0224(16) Uiso 1 1 d . . . H40A H 0.5599 0.2937 0.2750 0.027 Uiso 1 1 calc R . . C32 C 0.5654(3) -0.0320(11) 0.2218(2) 0.0228(16) Uani 1 1 d . . . O3W O -0.2305(3) -0.1867(9) -0.51317(16) 0.0232(12) Uani 1 1 d . . . H3WA H -0.2124 -0.0766 -0.4966 0.035 Uiso 1 1 calc R . . O2W O 0.3268(2) -0.7242(8) -0.02031(15) 0.0196(11) Uani 1 1 d . . . H2WA H 0.3426 -0.8345 -0.0033 0.029 Uiso 1 1 calc R . . O4W O -0.1281(2) -0.8226(8) -0.52018(15) 0.0312(12) Uani 1 1 d . . . H4WB H -0.1498 -0.8026 -0.5486 0.037 Uiso 1 1 calc R . . H4WA H -0.0968 -0.9387 -0.5020 0.037 Uiso 1 1 d R . . O1W O 0.4261(2) -0.0849(7) -0.02645(14) 0.0281(12) Uani 1 1 d . . . H10C H 0.4036 -0.1064 -0.0548 0.034 Uiso 1 1 calc R . . H10D H 0.4569 0.0338 -0.0091 0.034 Uiso 1 1 d R . . O5W O -0.0323(2) -0.5679(7) -0.43755(14) 0.0256(11) Uani 1 1 d . . . H10A H -0.0227 -0.6674 -0.4500 0.031 Uiso 1 1 calc R . . H10B H -0.0040 -0.4773 -0.4106 0.031 Uiso 1 1 d R . . C14 C -0.0970(3) -0.0131(11) -0.4197(2) 0.0161(15) Uani 1 1 d . . . O6W O 0.0308(3) 0.2368(10) 0.0454(2) 0.0355(15) Uani 1 1 d . . . H3WB H -0.265(3) -0.205(12) -0.524(2) 0.02(2) Uiso 1 1 d . . . H6WB H 0.009(4) 0.242(16) 0.023(3) 0.06(4) Uiso 1 1 d . . . H6WA H 0.042(3) 0.067(12) 0.054(2) 0.04(2) Uiso 1 1 d . . . H2WB H 0.292(3) -0.669(9) -0.0290(18) 0.000(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01385(18) 0.01264(19) 0.00703(16) 0.00075(14) 0.00303(13) 0.00066(15) Sm2 0.01524(18) 0.0132(2) 0.00922(17) -0.00076(14) 0.00477(14) 0.00072(15) O3 0.020(3) 0.016(3) 0.025(3) -0.009(2) 0.000(2) 0.003(2) O14 0.026(3) 0.027(3) 0.013(2) 0.004(2) 0.011(2) 0.012(2) O10 0.060(4) 0.054(4) 0.008(3) -0.004(2) 0.000(2) 0.021(3) O7 0.024(3) 0.039(3) 0.014(2) 0.005(2) 0.009(2) 0.009(2) O2 0.017(2) 0.022(3) 0.016(2) 0.002(2) 0.0045(19) -0.004(2) O15 0.053(3) 0.030(3) 0.007(2) -0.006(2) 0.004(2) 0.008(3) O9 0.024(3) 0.029(3) 0.025(3) -0.007(2) 0.012(2) -0.009(2) O5 0.042(3) 0.023(3) 0.007(2) 0.002(2) -0.004(2) -0.007(2) O13 0.022(3) 0.019(3) 0.008(2) -0.0058(19) 0.003(2) -0.001(2) O12 0.023(3) 0.016(3) 0.023(3) 0.012(2) 0.004(2) 0.003(2) O8 0.033(3) 0.039(3) 0.022(2) 0.002(2) 0.020(2) -0.001(2) O11 0.019(2) 0.014(2) 0.014(2) -0.0008(19) 0.0081(19) 0.000(2) O6 0.012(2) 0.023(3) 0.015(2) -0.002(2) 0.0054(19) 0.001(2) O1 0.017(2) 0.018(3) 0.016(2) 0.005(2) 0.002(2) -0.001(2) C28 0.026(4) 0.018(4) 0.026(4) 0.001(3) 0.016(3) 0.002(3) C38 0.018(4) 0.015(4) 0.004(3) -0.001(3) 0.002(3) 0.001(3) C42 0.010(3) 0.014(4) 0.015(3) 0.001(3) 0.000(3) 0.000(3) C29 0.020(4) 0.013(4) 0.009(3) -0.002(3) 0.010(3) 0.000(3) C37 0.022(4) 0.021(4) 0.009(3) 0.003(3) 0.004(3) 0.005(3) C11 0.026(4) 0.021(4) 0.014(3) -0.001(3) 0.004(3) 0.005(3) C15 0.014(3) 0.024(4) 0.010(3) -0.001(3) 0.007(3) -0.001(3) C27 0.022(4) 0.017(4) 0.012(3) -0.008(3) 0.012(3) -0.008(3) O4 0.021(3) 0.019(3) 0.010(2) 0.005(2) 0.0052(19) 0.003(2) C4 0.026(4) 0.014(4) 0.008(3) 0.000(3) 0.004(3) 0.002(3) C41 0.017(4) 0.018(4) 0.018(3) -0.004(3) 0.008(3) 0.001(3) C33 0.020(4) 0.028(4) 0.018(4) -0.011(3) 0.005(3) -0.007(3) C8 0.041(5) 0.017(4) 0.011(3) 0.001(3) 0.009(3) 0.003(4) C5 0.021(4) 0.029(4) 0.012(3) 0.000(3) 0.001(3) -0.010(3) C10 0.018(4) 0.012(4) 0.013(3) 0.001(3) 0.007(3) -0.001(3) C9 0.022(4) 0.022(4) 0.008(3) -0.002(3) -0.001(3) 0.005(3) C30 0.027(4) 0.028(4) 0.018(4) -0.004(3) 0.012(3) -0.010(3) C35 0.031(4) 0.022(4) 0.011(3) -0.007(3) 0.010(3) -0.005(3) C34 0.024(4) 0.021(4) 0.019(4) 0.000(3) 0.010(3) -0.007(3) C17 0.033(4) 0.035(4) 0.009(3) -0.011(3) 0.006(3) 0.003(4) C1 0.012(3) 0.018(4) 0.008(3) 0.002(3) 0.005(3) 0.001(3) C25 0.043(5) 0.061(6) 0.018(4) -0.003(4) 0.014(4) -0.025(4) C16 0.023(4) 0.027(4) 0.018(4) -0.006(3) 0.009(3) 0.002(3) C24 0.018(4) 0.022(4) 0.019(4) 0.002(3) 0.009(3) 0.000(3) C12 0.031(4) 0.021(4) 0.020(4) 0.006(3) 0.008(3) 0.010(3) C19 0.030(4) 0.041(5) 0.016(4) 0.000(3) 0.006(3) 0.014(4) C36 0.026(4) 0.027(4) 0.011(3) 0.000(3) 0.004(3) 0.012(3) C6 0.029(4) 0.019(4) 0.016(4) 0.002(3) 0.011(3) -0.005(3) C21 0.030(4) 0.049(5) 0.007(3) -0.002(3) 0.000(3) 0.011(4) C22 0.044(5) 0.048(6) 0.026(4) -0.002(4) 0.010(4) -0.018(4) C3 0.031(4) 0.013(4) 0.014(3) 0.002(3) 0.009(3) -0.004(3) C7 0.025(4) 0.023(4) 0.008(3) 0.005(3) 0.000(3) -0.002(3) C18 0.026(4) 0.035(5) 0.006(3) -0.001(3) 0.002(3) 0.004(3) C20 0.022(4) 0.030(4) 0.013(3) -0.007(3) 0.005(3) 0.004(3) C39 0.029(4) 0.018(4) 0.021(4) -0.006(3) 0.013(3) 0.006(3) C26 0.056(6) 0.074(7) 0.017(4) 0.000(4) 0.022(4) -0.018(5) C23 0.034(4) 0.056(6) 0.017(4) 0.001(4) 0.012(3) -0.014(4) C31 0.037(4) 0.017(4) 0.014(4) -0.001(3) 0.011(3) -0.006(3) C2 0.020(4) 0.020(4) 0.007(3) -0.001(3) 0.002(3) -0.002(3) C32 0.030(4) 0.024(4) 0.010(3) -0.003(3) 0.008(3) 0.006(3) O3W 0.016(3) 0.027(3) 0.022(3) 0.007(2) 0.007(2) 0.004(3) O2W 0.015(3) 0.018(3) 0.020(3) 0.000(2) 0.005(2) 0.003(2) O4W 0.037(3) 0.029(3) 0.027(3) -0.002(2) 0.017(2) 0.009(2) O1W 0.034(3) 0.033(3) 0.014(2) -0.001(2) 0.011(2) -0.013(2) O5W 0.025(3) 0.023(3) 0.026(3) -0.010(2) 0.011(2) 0.001(2) C14 0.016(4) 0.013(4) 0.018(3) 0.008(3) 0.009(3) -0.001(3) O6W 0.039(4) 0.028(4) 0.035(4) 0.000(3) 0.016(3) 0.007(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 Sm1 O7 2.328(4) 3_645 ? Sm1 O1 2.386(4) . ? Sm1 O6 2.394(4) . ? Sm1 O12 2.411(4) 1_545 ? Sm1 O11 2.414(4) . ? Sm1 O14 2.478(4) 2_645 ? Sm1 O2W 2.482(4) . ? Sm1 O1W 2.573(4) . ? Sm2 O13 2.316(4) 1_444 ? Sm2 O3 2.347(4) . ? Sm2 O8 2.366(4) 1_454 ? Sm2 O4 2.394(4) 1_545 ? Sm2 O2 2.429(4) 2_554 ? Sm2 O5W 2.455(4) . ? Sm2 O3W 2.492(5) . ? Sm2 O4W 2.510(4) . ? O3 C14 1.242(7) . ? O14 C42 1.250(7) . ? O14 Sm1 2.478(4) 2_665 ? O10 C21 1.388(7) . ? O10 C18 1.390(7) . ? O7 C27 1.254(7) . ? O7 Sm1 2.328(4) 3_645 ? O2 C13 1.272(7) . ? O2 Sm2 2.429(4) 2_554 ? O15 C32 1.385(7) . ? O15 C35 1.387(7) . ? O9 C28 1.250(7) . ? O5 C4 1.387(7) . ? O5 C7 1.403(7) . ? O13 C42 1.286(7) . ? O13 Sm2 2.316(4) 1_666 ? O12 C41 1.266(7) . ? O12 Sm1 2.411(4) 1_565 ? O8 C28 1.262(7) . ? O8 Sm2 2.366(4) 1_656 ? O11 C41 1.272(7) . ? O6 C27 1.251(7) . ? O1 C13 1.252(7) . ? C28 C24 1.501(8) . ? C38 C39 1.372(8) . ? C38 C37 1.384(8) . ? C38 C42 1.499(8) . ? C29 C34 1.376(8) . ? C29 C30 1.390(8) . ? C29 C41 1.488(8) . ? C37 C36 1.363(8) . ? C37 H37A 0.9300 . ? C11 C12 1.384(8) . ? C11 C10 1.387(8) . ? C11 H11A 0.9300 . ? C15 C16 1.368(8) . ? C15 C20 1.378(8) . ? C15 C27 1.513(8) . ? O4 C14 1.266(7) . ? O4 Sm2 2.394(4) 1_565 ? C4 C5 1.364(8) . ? C4 C3 1.384(8) . ? C33 C32 1.379(9) . ? C33 C34 1.386(8) . ? C33 H33A 0.9300 . ? C8 C7 1.369(9) . ? C8 C9 1.371(8) . ? C8 H8A 0.9300 . ? C5 C6 1.389(8) . ? C5 H5A 0.9300 . ? C10 C9 1.374(8) . ? C10 C14 1.515(8) . ? C9 H9A 0.9300 . ? C30 C31 1.378(8) . ? C30 H30A 0.9300 . ? C35 C40 1.372(9) . ? C35 C36 1.381(8) . ? C13 C1 1.498(7) . ? C34 H34A 0.9300 . ? C17 C18 1.365(9) . ? C17 C16 1.394(8) . ? C17 H17A 0.9300 . ? C1 C6 1.385(8) . ? C1 C2 1.384(8) . ? C25 C24 1.360(8) . ? C25 C26 1.383(9) . ? C25 H25A 0.9300 . ? C16 H16A 0.9300 . ? C24 C23 1.384(9) . ? C12 C7 1.379(9) . ? C12 H12A 0.9300 . ? C19 C18 1.375(8) . ? C19 C20 1.389(8) . ? C19 H19A 0.9300 . ? C36 H36A 0.9300 . ? C6 H6A 0.9300 . ? C21 C22 1.355(10) . ? C21 C26 1.364(10) . ? C22 C23 1.391(9) . ? C22 H22A 0.9300 . ? C3 C2 1.372(8) . ? C3 H3A 0.9300 . ? C20 H20A 0.9300 . ? C39 C40 1.389(8) . ? C39 H39A 0.9300 . ? C26 H26A 0.9300 . ? C23 H23A 0.9300 . ? C31 C32 1.380(9) . ? C31 H31A 0.9300 . ? C2 H2A 0.9300 . ? C40 H40A 0.9300 . ? O3W H3WA 0.8200 . ? O3W H3WB 0.69(6) . ? O2W H2WA 0.8200 . ? O2W H2WB 0.78(5) . ? O4W H4WB 0.8200 . ? O4W H4WA 0.9601 . ? O1W H10C 0.8200 . ? O1W H10D 0.9600 . ? O5W H10A 0.8200 . ? O5W H10B 0.9602 . ? O6W H6WB 0.66(8) . ? O6W H6WA 1.05(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Sm1 O1 93.47(14) 3_645 . ? O7 Sm1 O6 93.00(14) 3_645 . ? O1 Sm1 O6 143.48(14) . . ? O7 Sm1 O12 82.85(14) 3_645 1_545 ? O1 Sm1 O12 142.47(14) . 1_545 ? O6 Sm1 O12 74.03(14) . 1_545 ? O7 Sm1 O11 140.93(14) 3_645 . ? O1 Sm1 O11 78.11(13) . . ? O6 Sm1 O11 74.36(14) . . ? O12 Sm1 O11 126.19(13) 1_545 . ? O7 Sm1 O14 144.40(15) 3_645 2_645 ? O1 Sm1 O14 86.96(14) . 2_645 ? O6 Sm1 O14 107.58(13) . 2_645 ? O12 Sm1 O14 75.66(14) 1_545 2_645 ? O11 Sm1 O14 73.93(14) . 2_645 ? O7 Sm1 O2W 72.38(15) 3_645 . ? O1 Sm1 O2W 71.80(15) . . ? O6 Sm1 O2W 143.88(16) . . ? O12 Sm1 O2W 71.52(15) 1_545 . ? O11 Sm1 O2W 136.65(15) . . ? O14 Sm1 O2W 74.02(14) 2_645 . ? O7 Sm1 O1W 70.00(14) 3_645 . ? O1 Sm1 O1W 74.51(13) . . ? O6 Sm1 O1W 74.11(14) . . ? O12 Sm1 O1W 136.45(14) 1_545 . ? O11 Sm1 O1W 70.98(13) . . ? O14 Sm1 O1W 142.91(14) 2_645 . ? O2W Sm1 O1W 126.89(14) . . ? O13 Sm2 O3 144.57(14) 1_444 . ? O13 Sm2 O8 95.46(15) 1_444 1_454 ? O3 Sm2 O8 85.18(16) . 1_454 ? O13 Sm2 O4 82.16(14) 1_444 1_545 ? O3 Sm2 O4 118.66(14) . 1_545 ? O8 Sm2 O4 140.95(15) 1_454 1_545 ? O13 Sm2 O2 81.88(14) 1_444 2_554 ? O3 Sm2 O2 77.80(14) . 2_554 ? O8 Sm2 O2 144.83(15) 1_454 2_554 ? O4 Sm2 O2 73.73(14) 1_545 2_554 ? O13 Sm2 O5W 147.90(14) 1_444 . ? O3 Sm2 O5W 67.51(14) . . ? O8 Sm2 O5W 84.15(15) 1_454 . ? O4 Sm2 O5W 78.41(14) 1_545 . ? O2 Sm2 O5W 116.16(13) 2_554 . ? O13 Sm2 O3W 74.10(16) 1_444 . ? O3 Sm2 O3W 72.37(16) . . ? O8 Sm2 O3W 72.49(16) 1_454 . ? O4 Sm2 O3W 141.36(16) 1_545 . ? O2 Sm2 O3W 73.09(14) 2_554 . ? O5W Sm2 O3W 134.84(16) . . ? O13 Sm2 O4W 77.39(14) 1_444 . ? O3 Sm2 O4W 134.94(15) . . ? O8 Sm2 O4W 71.62(15) 1_454 . ? O4 Sm2 O4W 69.83(14) 1_545 . ? O2 Sm2 O4W 139.99(15) 2_554 . ? O5W Sm2 O4W 72.03(14) . . ? O3W Sm2 O4W 131.07(15) . . ? C14 O3 Sm2 149.8(4) . . ? C42 O14 Sm1 138.9(4) . 2_665 ? C21 O10 C18 122.7(5) . . ? C27 O7 Sm1 171.5(4) . 3_645 ? C13 O2 Sm2 134.8(4) . 2_554 ? C32 O15 C35 122.5(5) . . ? C4 O5 C7 120.9(5) . . ? C42 O13 Sm2 144.1(4) . 1_666 ? C41 O12 Sm1 137.5(4) . 1_565 ? C28 O8 Sm2 162.0(4) . 1_656 ? C41 O11 Sm1 132.2(4) . . ? C27 O6 Sm1 128.7(4) . . ? C13 O1 Sm1 145.6(4) . . ? O9 C28 O8 122.8(6) . . ? O9 C28 C24 118.7(6) . . ? O8 C28 C24 118.6(6) . . ? C39 C38 C37 118.8(5) . . ? C39 C38 C42 121.0(5) . . ? C37 C38 C42 120.2(5) . . ? O14 C42 O13 122.7(5) . . ? O14 C42 C38 121.3(5) . . ? O13 C42 C38 115.9(5) . . ? C34 C29 C30 118.7(6) . . ? C34 C29 C41 121.6(6) . . ? C30 C29 C41 119.7(6) . . ? C36 C37 C38 121.1(5) . . ? C36 C37 H37A 119.5 . . ? C38 C37 H37A 119.5 . . ? C12 C11 C10 120.2(6) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C16 C15 C20 119.2(6) . . ? C16 C15 C27 121.9(6) . . ? C20 C15 C27 118.8(5) . . ? O6 C27 O7 122.9(6) . . ? O6 C27 C15 118.9(5) . . ? O7 C27 C15 118.2(6) . . ? C14 O4 Sm2 138.3(4) . 1_565 ? C5 C4 C3 120.8(6) . . ? C5 C4 O5 124.8(5) . . ? C3 C4 O5 114.3(5) . . ? O12 C41 O11 122.3(6) . . ? O12 C41 C29 118.1(6) . . ? O11 C41 C29 119.7(6) . . ? C32 C33 C34 119.3(6) . . ? C32 C33 H33A 120.4 . . ? C34 C33 H33A 120.4 . . ? C7 C8 C9 120.4(6) . . ? C7 C8 H8A 119.8 . . ? C9 C8 H8A 119.8 . . ? C4 C5 C6 118.8(6) . . ? C4 C5 H5A 120.6 . . ? C6 C5 H5A 120.6 . . ? C9 C10 C11 119.8(6) . . ? C9 C10 C14 120.5(6) . . ? C11 C10 C14 119.7(5) . . ? C8 C9 C10 119.9(6) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? C31 C30 C29 120.8(6) . . ? C31 C30 H30A 119.6 . . ? C29 C30 H30A 119.6 . . ? C40 C35 C36 120.7(6) . . ? C40 C35 O15 125.0(6) . . ? C36 C35 O15 114.3(5) . . ? O1 C13 O2 123.5(5) . . ? O1 C13 C1 118.2(5) . . ? O2 C13 C1 118.3(5) . . ? C29 C34 C33 121.1(6) . . ? C29 C34 H34A 119.5 . . ? C33 C34 H34A 119.5 . . ? C18 C17 C16 118.6(6) . . ? C18 C17 H17A 120.7 . . ? C16 C17 H17A 120.7 . . ? C6 C1 C2 118.1(5) . . ? C6 C1 C13 120.8(5) . . ? C2 C1 C13 121.0(5) . . ? C24 C25 C26 120.9(7) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C15 C16 C17 121.0(6) . . ? C15 C16 H16A 119.5 . . ? C17 C16 H16A 119.5 . . ? C25 C24 C23 118.7(6) . . ? C25 C24 C28 121.0(6) . . ? C23 C24 C28 120.1(6) . . ? C7 C12 C11 118.9(6) . . ? C7 C12 H12A 120.6 . . ? C11 C12 H12A 120.6 . . ? C18 C19 C20 118.6(6) . . ? C18 C19 H19A 120.7 . . ? C20 C19 H19A 120.7 . . ? C37 C36 C35 119.5(6) . . ? C37 C36 H36A 120.2 . . ? C35 C36 H36A 120.2 . . ? C1 C6 C5 121.6(6) . . ? C1 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? C22 C21 C26 121.6(6) . . ? C22 C21 O10 116.7(7) . . ? C26 C21 O10 121.1(7) . . ? C21 C22 C23 118.6(7) . . ? C21 C22 H22A 120.7 . . ? C23 C22 H22A 120.7 . . ? C2 C3 C4 119.8(6) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C8 C7 C12 120.7(6) . . ? C8 C7 O5 116.1(6) . . ? C12 C7 O5 122.8(6) . . ? C17 C18 C19 121.7(6) . . ? C17 C18 O10 125.1(6) . . ? C19 C18 O10 113.1(6) . . ? C15 C20 C19 120.7(6) . . ? C15 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C38 C39 C40 121.0(6) . . ? C38 C39 H39A 119.5 . . ? C40 C39 H39A 119.5 . . ? C21 C26 C25 119.2(7) . . ? C21 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? C24 C23 C22 120.8(7) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C30 C31 C32 119.6(6) . . ? C30 C31 H31A 120.2 . . ? C32 C31 H31A 120.2 . . ? C3 C2 C1 120.9(6) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C35 C40 C39 118.9(6) . . ? C35 C40 H40A 120.6 . . ? C39 C40 H40A 120.6 . . ? C33 C32 C31 120.4(6) . . ? C33 C32 O15 124.0(6) . . ? C31 C32 O15 115.3(6) . . ? Sm2 O3W H3WA 109.5 . . ? Sm2 O3W H3WB 118(6) . . ? H3WA O3W H3WB 121.4 . . ? Sm1 O2W H2WA 109.5 . . ? Sm1 O2W H2WB 102(4) . . ? H2WA O2W H2WB 127.2 . . ? Sm2 O4W H4WB 109.5 . . ? Sm2 O4W H4WA 120.2 . . ? H4WB O4W H4WA 130.3 . . ? Sm1 O1W H10C 109.5 . . ? Sm1 O1W H10D 120.5 . . ? H10C O1W H10D 130.0 . . ? Sm2 O5W H10A 109.5 . . ? Sm2 O5W H10B 120.1 . . ? H10A O5W H10B 130.4 . . ? O3 C14 O4 124.3(6) . . ? O3 C14 C10 118.0(6) . . ? O4 C14 C10 117.7(6) . . ? H6WB O6W H6WA 107(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O13 Sm2 O3 C14 5.7(10) 1_444 . . . ? O8 Sm2 O3 C14 98.3(8) 1_454 . . . ? O4 Sm2 O3 C14 -114.3(8) 1_545 . . . ? O2 Sm2 O3 C14 -50.7(8) 2_554 . . . ? O5W Sm2 O3 C14 -176.0(9) . . . . ? O3W Sm2 O3 C14 25.2(8) . . . . ? O4W Sm2 O3 C14 156.2(8) . . . . ? O7 Sm1 O11 C41 -68.7(6) 3_645 . . . ? O1 Sm1 O11 C41 -149.4(5) . . . . ? O6 Sm1 O11 C41 6.3(5) . . . . ? O12 Sm1 O11 C41 62.3(5) 1_545 . . . ? O14 Sm1 O11 C41 120.3(5) 2_645 . . . ? O2W Sm1 O11 C41 164.0(5) . . . . ? O1W Sm1 O11 C41 -71.9(5) . . . . ? O7 Sm1 O6 C27 -31.5(5) 3_645 . . . ? O1 Sm1 O6 C27 -131.4(5) . . . . ? O12 Sm1 O6 C27 50.2(5) 1_545 . . . ? O11 Sm1 O6 C27 -173.9(5) . . . . ? O14 Sm1 O6 C27 119.1(5) 2_645 . . . ? O2W Sm1 O6 C27 32.3(6) . . . . ? O1W Sm1 O6 C27 -99.7(5) . . . . ? O7 Sm1 O1 C13 69.5(7) 3_645 . . . ? O6 Sm1 O1 C13 169.3(6) . . . . ? O12 Sm1 O1 C13 -13.3(8) 1_545 . . . ? O11 Sm1 O1 C13 -149.0(7) . . . . ? O14 Sm1 O1 C13 -74.8(7) 2_645 . . . ? O2W Sm1 O1 C13 -0.7(7) . . . . ? O1W Sm1 O1 C13 137.7(7) . . . . ? Sm2 O8 C28 O9 -73.9(16) 1_656 . . . ? Sm2 O8 C28 C24 106.9(14) 1_656 . . . ? Sm1 O14 C42 O13 -51.5(9) 2_665 . . . ? Sm1 O14 C42 C38 129.0(5) 2_665 . . . ? Sm2 O13 C42 O14 -63.4(10) 1_666 . . . ? Sm2 O13 C42 C38 116.1(6) 1_666 . . . ? C39 C38 C42 O14 18.4(10) . . . . ? C37 C38 C42 O14 -160.9(6) . . . . ? C39 C38 C42 O13 -161.1(6) . . . . ? C37 C38 C42 O13 19.6(9) . . . . ? C39 C38 C37 C36 -2.7(10) . . . . ? C42 C38 C37 C36 176.6(6) . . . . ? Sm1 O6 C27 O7 49.4(8) . . . . ? Sm1 O6 C27 C15 -130.9(5) . . . . ? Sm1 O7 C27 O6 -140(3) 3_645 . . . ? Sm1 O7 C27 C15 41(3) 3_645 . . . ? C16 C15 C27 O6 -25.1(9) . . . . ? C20 C15 C27 O6 150.8(6) . . . . ? C16 C15 C27 O7 154.7(6) . . . . ? C20 C15 C27 O7 -29.4(9) . . . . ? C7 O5 C4 C5 -18.6(10) . . . . ? C7 O5 C4 C3 165.1(6) . . . . ? Sm1 O12 C41 O11 61.2(9) 1_565 . . . ? Sm1 O12 C41 C29 -119.4(6) 1_565 . . . ? Sm1 O11 C41 O12 97.4(7) . . . . ? Sm1 O11 C41 C29 -82.0(7) . . . . ? C34 C29 C41 O12 2.2(9) . . . . ? C30 C29 C41 O12 -176.7(6) . . . . ? C34 C29 C41 O11 -178.3(6) . . . . ? C30 C29 C41 O11 2.7(9) . . . . ? C3 C4 C5 C6 1.1(10) . . . . ? O5 C4 C5 C6 -174.9(6) . . . . ? C12 C11 C10 C9 0.0(10) . . . . ? C12 C11 C10 C14 -179.4(6) . . . . ? C7 C8 C9 C10 0.5(10) . . . . ? C11 C10 C9 C8 -1.3(10) . . . . ? C14 C10 C9 C8 178.1(6) . . . . ? C34 C29 C30 C31 -2.4(10) . . . . ? C41 C29 C30 C31 176.5(6) . . . . ? C32 O15 C35 C40 15.9(10) . . . . ? C32 O15 C35 C36 -166.4(6) . . . . ? Sm1 O1 C13 O2 39.3(10) . . . . ? Sm1 O1 C13 C1 -141.1(5) . . . . ? Sm2 O2 C13 O1 71.6(8) 2_554 . . . ? Sm2 O2 C13 C1 -108.1(5) 2_554 . . . ? C30 C29 C34 C33 1.9(10) . . . . ? C41 C29 C34 C33 -177.0(6) . . . . ? C32 C33 C34 C29 -0.3(10) . . . . ? O1 C13 C1 C6 167.2(6) . . . . ? O2 C13 C1 C6 -13.1(9) . . . . ? O1 C13 C1 C2 -14.1(8) . . . . ? O2 C13 C1 C2 165.6(6) . . . . ? C20 C15 C16 C17 -3.2(10) . . . . ? C27 C15 C16 C17 172.7(6) . . . . ? C18 C17 C16 C15 -0.7(11) . . . . ? C26 C25 C24 C23 -0.7(12) . . . . ? C26 C25 C24 C28 174.5(7) . . . . ? O9 C28 C24 C25 -18.6(10) . . . . ? O8 C28 C24 C25 160.7(7) . . . . ? O9 C28 C24 C23 156.5(7) . . . . ? O8 C28 C24 C23 -24.2(10) . . . . ? C10 C11 C12 C7 2.2(11) . . . . ? C38 C37 C36 C35 1.4(10) . . . . ? C40 C35 C36 C37 1.7(10) . . . . ? O15 C35 C36 C37 -176.0(6) . . . . ? C2 C1 C6 C5 0.4(10) . . . . ? C13 C1 C6 C5 179.2(6) . . . . ? C4 C5 C6 C1 -1.3(10) . . . . ? C18 O10 C21 C22 120.9(8) . . . . ? C18 O10 C21 C26 -67.0(10) . . . . ? C26 C21 C22 C23 -1.4(12) . . . . ? O10 C21 C22 C23 170.7(6) . . . . ? C5 C4 C3 C2 -0.1(10) . . . . ? O5 C4 C3 C2 176.3(6) . . . . ? C9 C8 C7 C12 1.7(11) . . . . ? C9 C8 C7 O5 174.5(6) . . . . ? C11 C12 C7 C8 -3.0(11) . . . . ? C11 C12 C7 O5 -175.4(6) . . . . ? C4 O5 C7 C8 139.9(6) . . . . ? C4 O5 C7 C12 -47.5(9) . . . . ? C16 C17 C18 C19 3.0(11) . . . . ? C16 C17 C18 O10 -172.8(6) . . . . ? C20 C19 C18 C17 -1.4(11) . . . . ? C20 C19 C18 O10 174.9(6) . . . . ? C21 O10 C18 C17 -14.5(11) . . . . ? C21 O10 C18 C19 169.4(7) . . . . ? C16 C15 C20 C19 4.8(10) . . . . ? C27 C15 C20 C19 -171.2(6) . . . . ? C18 C19 C20 C15 -2.6(11) . . . . ? C37 C38 C39 C40 1.0(10) . . . . ? C42 C38 C39 C40 -178.3(6) . . . . ? C22 C21 C26 C25 3.9(13) . . . . ? O10 C21 C26 C25 -167.9(7) . . . . ? C24 C25 C26 C21 -2.8(13) . . . . ? C25 C24 C23 C22 3.1(11) . . . . ? C28 C24 C23 C22 -172.1(7) . . . . ? C21 C22 C23 C24 -2.1(12) . . . . ? C29 C30 C31 C32 1.3(10) . . . . ? C4 C3 C2 C1 -0.8(10) . . . . ? C6 C1 C2 C3 0.6(9) . . . . ? C13 C1 C2 C3 -178.2(6) . . . . ? C36 C35 C40 C39 -3.4(10) . . . . ? O15 C35 C40 C39 174.1(6) . . . . ? C38 C39 C40 C35 2.0(10) . . . . ? C34 C33 C32 C31 -0.9(10) . . . . ? C34 C33 C32 O15 172.9(6) . . . . ? C30 C31 C32 C33 0.4(10) . . . . ? C30 C31 C32 O15 -173.9(6) . . . . ? C35 O15 C32 C33 50.5(9) . . . . ? C35 O15 C32 C31 -135.4(6) . . . . ? Sm2 O3 C14 O4 -33.2(12) . . . . ? Sm2 O3 C14 C10 144.8(6) . . . . ? Sm2 O4 C14 O3 -108.7(7) 1_565 . . . ? Sm2 O4 C14 C10 73.3(8) 1_565 . . . ? C9 C10 C14 O3 -172.8(6) . . . . ? C11 C10 C14 O3 6.6(9) . . . . ? C9 C10 C14 O4 5.4(9) . . . . ? C11 C10 C14 O4 -175.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.966 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.130