# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_exp_1338 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H17 Dy O10' _chemical_formula_weight 675.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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 P21/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 9.344(2) _cell_length_b 18.507(6) _cell_length_c 14.312(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.404(20) _cell_angle_gamma 90.00 _cell_volume 2467.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.5123 _cell_measurement_theta_max 28.3831 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.819 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 3.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8864 _exptl_absorpt_correction_T_max 0.9408 _exptl_absorpt_process_details multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8751 _diffrn_reflns_av_R_equivalents 0.1766 _diffrn_reflns_av_sigmaI/netI 0.2853 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4342 _reflns_number_gt 2044 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0777P)^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 4342 _refine_ls_number_parameters 364 _refine_ls_number_restraints 972 _refine_ls_R_factor_all 0.1954 _refine_ls_R_factor_gt 0.0905 _refine_ls_wR_factor_ref 0.2502 _refine_ls_wR_factor_gt 0.1753 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.78482(6) 0.97353(3) -0.01153(4) 0.03084(16) Uani 1 1 d U . . O1 O 0.6276(9) 0.8831(5) -0.0885(6) 0.048(2) Uani 1 1 d U A . O3 O 0.1352(10) 0.6779(5) -0.2733(6) 0.0535(18) Uani 1 1 d U A . O4 O 0.1334(8) 0.5628(5) -0.3989(5) 0.0453(19) Uani 1 1 d U . . O5 O -0.1004(8) 0.5370(5) -0.4259(5) 0.044(2) Uani 1 1 d U . . O6 O 0.8804(9) 1.0201(5) 0.1274(5) 0.052(2) Uani 1 1 d U . . O7 O 1.1053(8) 1.0556(5) 0.1447(5) 0.046(2) Uani 1 1 d U . . O8 O 1.1887(9) 1.1125(5) 0.3130(6) 0.0492(17) Uani 1 1 d U . . O9 O 1.6108(9) 1.3625(5) 0.4640(6) 0.045(2) Uani 1 1 d U . . O10 O 1.4118(9) 1.4216(5) 0.4550(6) 0.051(2) Uani 1 1 d U . . C1 C 0.6128(14) 0.8164(8) -0.0896(9) 0.045(2) Uani 1 1 d U . . C2 C 0.4899(14) 0.7803(8) -0.1398(9) 0.044(2) Uani 1 1 d U A . C3 C 0.4931(15) 0.7070(8) -0.1562(9) 0.054(2) Uani 1 1 d U . . H3 H 0.5745 0.6804 -0.1369 0.065 Uiso 1 1 calc R A . C4 C 0.3745(14) 0.6727(8) -0.2016(9) 0.051(2) Uani 1 1 d U A . H4 H 0.3789 0.6235 -0.2143 0.061 Uiso 1 1 calc R . . C5 C 0.2493(14) 0.7109(8) -0.2283(9) 0.049(2) Uani 1 1 d U . . C6 C 0.2524(14) 0.7824(8) -0.2101(9) 0.051(2) Uani 1 1 d U A . H6 H 0.1679 0.8081 -0.2242 0.061 Uiso 1 1 calc R . . C7 C 0.3711(14) 0.8216(8) -0.1717(9) 0.050(2) Uani 1 1 d U . . H7 H 0.3707 0.8718 -0.1678 0.060 Uiso 1 1 calc R A . C8 C 0.0598(13) 0.6270(8) -0.2229(9) 0.047(2) Uani 1 1 d U . . C9 C 0.0405(14) 0.6401(8) -0.1305(9) 0.052(2) Uani 1 1 d U A . H9 H 0.0828 0.6799 -0.0998 0.062 Uiso 1 1 calc R . . C10 C -0.0416(14) 0.5935(8) -0.0851(9) 0.054(3) Uani 1 1 d U . . H10 H -0.0479 0.5999 -0.0211 0.064 Uiso 1 1 calc R A . C11 C -0.1156(13) 0.5378(8) -0.1280(9) 0.049(3) Uani 1 1 d U A . H11 H -0.1734 0.5070 -0.0960 0.059 Uiso 1 1 calc R . . C12 C -0.0981(13) 0.5303(8) -0.2249(8) 0.044(2) Uani 1 1 d U . . H12 H -0.1477 0.4935 -0.2577 0.053 Uiso 1 1 calc R A . C13 C -0.0117(13) 0.5745(8) -0.2728(8) 0.046(2) Uani 1 1 d U A . C14 C 0.0084(13) 0.5557(8) -0.3754(9) 0.042(2) Uani 1 1 d U . . C15 C 0.9891(14) 1.0422(8) 0.1752(8) 0.045(2) Uani 1 1 d U . . C16 C 0.9601(13) 1.0567(8) 0.2774(8) 0.045(2) Uani 1 1 d U . . C17 C 0.8273(13) 1.0333(8) 0.3092(8) 0.046(2) Uani 1 1 d U . . H17 H 0.7578 1.0132 0.2670 0.056 Uiso 1 1 calc R . . C18 C 0.8026(14) 1.0397(8) 0.3959(9) 0.056(3) Uani 1 1 d U . . H18 H 0.7191 1.0197 0.4161 0.067 Uiso 1 1 calc R . . C19 C 0.8946(14) 1.0750(9) 0.4598(9) 0.056(3) Uani 1 1 d U . . H19 H 0.8701 1.0803 0.5212 0.067 Uiso 1 1 calc R . . C20 C 1.0202(14) 1.1022(8) 0.4349(9) 0.053(2) Uani 1 1 d U . . H20 H 1.0815 1.1274 0.4777 0.064 Uiso 1 1 calc R . . C21 C 1.0562(14) 1.0910(8) 0.3399(9) 0.048(2) Uani 1 1 d U . . C22 C 1.2513(14) 1.1746(8) 0.3508(9) 0.046(2) Uani 1 1 d U . . C23 C 1.4051(14) 1.1746(8) 0.3609(9) 0.046(2) Uani 1 1 d U . . H23 H 1.4575 1.1341 0.3459 0.055 Uiso 1 1 calc R . . C24 C 1.4694(14) 1.2341(8) 0.3924(9) 0.045(2) Uani 1 1 d U . . H24 H 1.5692 1.2340 0.4003 0.054 Uiso 1 1 calc R . . C25 C 1.3992(14) 1.2960(8) 0.4142(9) 0.042(2) Uani 1 1 d U . . C26 C 1.2555(14) 1.2940(8) 0.4010(9) 0.054(2) Uani 1 1 d U . . H26 H 1.2061 1.3361 0.4133 0.064 Uiso 1 1 calc R . . C27 C 1.1750(16) 1.2349(8) 0.3708(9) 0.055(2) Uani 1 1 d U . . H27 H 1.0752 1.2360 0.3644 0.066 Uiso 1 1 calc R . . C28 C 1.4780(14) 1.3640(8) 0.4431(9) 0.045(3) Uani 1 1 d U . . O2A O 0.6958(18) 0.7738(10) -0.0338(11) 0.056(4) Uani 0.577(17) 1 d PU A 1 H2A H 0.7619 0.7976 -0.0083 0.084 Uiso 0.577(17) 1 calc PR A 1 O2B O 0.728(2) 0.7698(12) -0.0771(16) 0.045(5) Uani 0.423(17) 1 d PU A 2 H2B H 0.7860 0.7856 -0.0360 0.068 Uiso 0.423(17) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0291(3) 0.0289(3) 0.0341(3) 0.0015(3) -0.0005(2) -0.0009(3) O1 0.041(4) 0.046(4) 0.057(4) -0.009(4) -0.005(4) -0.009(4) O3 0.052(3) 0.050(3) 0.058(3) -0.009(3) 0.002(3) -0.016(3) O4 0.039(3) 0.052(4) 0.046(3) -0.014(3) 0.007(3) -0.004(3) O5 0.034(4) 0.047(4) 0.048(4) -0.017(4) -0.007(3) 0.003(4) O6 0.046(4) 0.063(4) 0.047(4) -0.008(4) 0.004(3) -0.019(4) O7 0.040(4) 0.051(4) 0.049(4) -0.014(4) 0.011(3) -0.008(4) O8 0.047(3) 0.045(3) 0.056(3) -0.016(3) 0.006(3) -0.010(3) O9 0.043(4) 0.035(4) 0.057(4) -0.003(4) 0.005(4) -0.004(4) O10 0.041(4) 0.044(4) 0.066(4) -0.012(4) -0.007(4) 0.001(4) C1 0.037(4) 0.039(4) 0.060(4) -0.005(4) -0.002(4) -0.007(4) C2 0.041(4) 0.035(4) 0.056(4) -0.006(4) 0.000(4) -0.010(4) C3 0.053(4) 0.044(4) 0.064(4) -0.007(4) 0.003(4) -0.007(4) C4 0.053(4) 0.040(4) 0.060(4) -0.012(4) -0.003(4) -0.015(4) C5 0.047(4) 0.044(4) 0.055(4) -0.012(4) 0.003(4) -0.013(4) C6 0.049(4) 0.041(4) 0.063(4) -0.012(4) 0.000(4) -0.010(4) C7 0.046(4) 0.040(4) 0.062(4) -0.016(4) -0.001(4) -0.012(4) C8 0.041(3) 0.046(4) 0.053(3) -0.014(3) 0.006(3) -0.012(3) C9 0.051(4) 0.049(4) 0.054(4) -0.018(4) 0.002(4) -0.012(4) C10 0.056(5) 0.053(5) 0.051(4) -0.016(4) 0.002(4) -0.015(5) C11 0.048(5) 0.050(5) 0.051(5) -0.010(5) 0.011(4) -0.026(5) C12 0.040(4) 0.047(4) 0.046(4) -0.015(4) 0.000(4) -0.013(4) C13 0.043(4) 0.046(4) 0.047(4) -0.015(4) 0.003(4) -0.009(4) C14 0.035(4) 0.041(5) 0.051(4) -0.010(4) 0.007(4) -0.006(4) C15 0.039(4) 0.049(4) 0.048(4) -0.014(4) 0.002(4) -0.005(4) C16 0.040(4) 0.050(4) 0.046(4) -0.012(4) 0.009(3) -0.010(4) C17 0.043(4) 0.049(4) 0.048(4) -0.012(4) 0.009(4) -0.014(4) C18 0.050(5) 0.063(5) 0.057(5) -0.010(5) 0.013(4) -0.017(5) C19 0.052(5) 0.060(5) 0.058(5) -0.011(5) 0.012(4) -0.019(5) C20 0.048(4) 0.056(4) 0.056(4) -0.021(4) 0.006(4) -0.016(4) C21 0.042(3) 0.049(4) 0.053(3) -0.013(3) 0.006(3) -0.011(3) C22 0.042(4) 0.045(4) 0.049(4) -0.022(4) 0.002(4) -0.007(4) C23 0.044(4) 0.044(4) 0.050(4) -0.009(4) -0.001(4) 0.002(4) C24 0.041(4) 0.041(4) 0.053(4) -0.008(4) -0.003(4) -0.003(4) C25 0.042(4) 0.034(4) 0.049(4) -0.015(4) -0.009(4) -0.007(4) C26 0.052(4) 0.044(4) 0.063(4) -0.021(4) -0.008(4) 0.002(4) C27 0.048(4) 0.050(4) 0.067(4) -0.019(4) -0.002(4) -0.007(4) C28 0.045(5) 0.039(5) 0.049(4) -0.013(4) -0.006(4) 0.000(4) O2A 0.058(8) 0.059(8) 0.052(7) 0.002(7) 0.005(7) -0.003(7) O2B 0.037(8) 0.033(9) 0.067(9) -0.010(8) 0.008(8) -0.002(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 O5 2.216(8) 2_554 ? Dy1 O6 2.285(8) . ? Dy1 O7 2.297(8) 3_775 ? Dy1 O9 2.353(9) 2_745 ? Dy1 O10 2.343(10) 4_585 ? Dy1 O4 2.325(8) 4_676 ? Dy1 O1 2.434(9) . ? O1 C1 1.241(16) . ? O3 C5 1.348(15) . ? O3 C8 1.408(16) . ? O4 C14 1.247(14) . ? O4 Dy1 2.325(8) 4_575 ? O5 C14 1.250(14) . ? O5 Dy1 2.216(8) 2_544 ? O6 C15 1.249(14) . ? O7 C15 1.226(14) . ? O7 Dy1 2.297(8) 3_775 ? O8 C21 1.383(15) . ? O8 C22 1.381(16) . ? O9 C28 1.254(15) . ? O9 Dy1 2.353(9) 2_755 ? O10 C28 1.251(16) . ? O10 Dy1 2.343(10) 4_686 ? C1 O2A 1.33(2) . ? C1 O2B 1.38(2) . ? C1 C2 1.468(17) . ? C2 C7 1.396(18) . ? C2 C3 1.38(2) . ? C3 C4 1.395(18) . ? C3 H3 0.9300 . ? C4 C5 1.395(19) . ? C4 H4 0.9300 . ? C5 C6 1.349(19) . ? C6 C7 1.401(18) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.369(17) . ? C8 C13 1.352(18) . ? C9 C10 1.353(19) . ? C9 H9 0.9300 . ? C10 C11 1.361(18) . ? C10 H10 0.9300 . ? C11 C12 1.417(17) . ? C11 H11 0.9300 . ? C12 C13 1.369(18) . ? C12 H12 0.9300 . ? C13 C14 1.535(17) . ? C15 C16 1.531(17) . ? C16 C21 1.375(17) . ? C16 C17 1.422(17) . ? C17 C18 1.285(17) . ? C17 H17 0.9300 . ? C18 C19 1.372(18) . ? C18 H18 0.9300 . ? C19 C20 1.350(18) . ? C19 H19 0.9300 . ? C20 C21 1.440(18) . ? C20 H20 0.9300 . ? C22 C27 1.37(2) . ? C22 C23 1.433(17) . ? C23 C24 1.318(19) . ? C23 H23 0.9300 . ? C24 C25 1.367(19) . ? C24 H24 0.9300 . ? C25 C26 1.342(17) . ? C25 C28 1.501(19) . ? C26 C27 1.378(19) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? O2A H2A 0.8200 . ? O2B H2B 0.8200 . ? 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 O5 Dy1 O6 113.0(3) 2_554 . ? O5 Dy1 O7 99.9(3) 2_554 3_775 ? O6 Dy1 O7 129.8(3) . 3_775 ? O5 Dy1 O9 150.7(3) 2_554 2_745 ? O6 Dy1 O9 87.2(3) . 2_745 ? O7 Dy1 O9 80.4(3) 3_775 2_745 ? O5 Dy1 O10 82.5(3) 2_554 4_585 ? O6 Dy1 O10 72.3(3) . 4_585 ? O7 Dy1 O10 76.0(3) 3_775 4_585 ? O9 Dy1 O10 125.3(3) 2_745 4_585 ? O5 Dy1 O4 86.4(3) 2_554 4_676 ? O6 Dy1 O4 73.9(3) . 4_676 ? O7 Dy1 O4 147.4(3) 3_775 4_676 ? O9 Dy1 O4 78.9(3) 2_745 4_676 ? O10 Dy1 O4 136.6(3) 4_585 4_676 ? O5 Dy1 O1 76.0(3) 2_554 . ? O6 Dy1 O1 146.6(3) . . ? O7 Dy1 O1 75.9(3) 3_775 . ? O9 Dy1 O1 75.7(3) 2_745 . ? O10 Dy1 O1 140.8(3) 4_585 . ? O4 Dy1 O1 74.7(3) 4_676 . ? C1 O1 Dy1 138.8(8) . . ? C5 O3 C8 117.9(10) . . ? C14 O4 Dy1 142.1(8) . 4_575 ? C14 O5 Dy1 162.3(9) . 2_544 ? C15 O6 Dy1 147.9(8) . . ? C15 O7 Dy1 135.5(8) . 3_775 ? C21 O8 C22 119.4(10) . . ? C28 O9 Dy1 115.5(9) . 2_755 ? C28 O10 Dy1 175.7(9) . 4_686 ? O1 C1 O2A 121.5(13) . . ? O1 C1 O2B 122.2(14) . . ? O2A C1 O2B 30.5(11) . . ? O1 C1 C2 122.7(12) . . ? O2A C1 C2 115.0(14) . . ? O2B C1 C2 110.7(14) . . ? C7 C2 C3 120.7(12) . . ? C7 C2 C1 118.9(13) . . ? C3 C2 C1 120.4(12) . . ? C2 C3 C4 120.1(13) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 121.0(14) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C6 C5 O3 122.8(13) . . ? C6 C5 C4 116.1(12) . . ? O3 C5 C4 121.1(13) . . ? C5 C6 C7 126.0(13) . . ? C5 C6 H6 117.0 . . ? C7 C6 H6 117.0 . . ? C6 C7 C2 115.5(13) . . ? C6 C7 H7 122.3 . . ? C2 C7 H7 122.3 . . ? C9 C8 C13 122.7(13) . . ? C9 C8 O3 119.0(12) . . ? C13 C8 O3 117.1(11) . . ? C10 C9 C8 118.2(13) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C9 C10 C11 123.6(13) . . ? C9 C10 H10 118.2 . . ? C11 C10 H10 118.2 . . ? C10 C11 C12 115.1(12) . . ? C10 C11 H11 122.5 . . ? C12 C11 H11 122.5 . . ? C13 C12 C11 123.2(12) . . ? C13 C12 H12 118.4 . . ? C11 C12 H12 118.4 . . ? C12 C13 C8 116.8(12) . . ? C12 C13 C14 117.6(12) . . ? C8 C13 C14 125.3(12) . . ? O4 C14 O5 127.6(11) . . ? O4 C14 C13 114.8(11) . . ? O5 C14 C13 117.6(11) . . ? O7 C15 O6 125.2(11) . . ? O7 C15 C16 122.1(11) . . ? O6 C15 C16 112.6(11) . . ? C21 C16 C17 118.3(11) . . ? C21 C16 C15 123.2(11) . . ? C17 C16 C15 118.4(11) . . ? C18 C17 C16 120.5(12) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 122.5(13) . . ? C17 C18 H18 118.7 . . ? C19 C18 H18 118.7 . . ? C20 C19 C18 121.0(13) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 117.8(12) . . ? C19 C20 H20 121.1 . . ? C21 C20 H20 121.1 . . ? O8 C21 C16 120.4(11) . . ? O8 C21 C20 120.0(11) . . ? C16 C21 C20 119.5(12) . . ? C27 C22 O8 123.4(12) . . ? C27 C22 C23 121.0(13) . . ? O8 C22 C23 115.5(12) . . ? C24 C23 C22 117.5(14) . . ? C24 C23 H23 121.2 . . ? C22 C23 H23 121.2 . . ? C23 C24 C25 124.3(13) . . ? C23 C24 H24 117.9 . . ? C25 C24 H24 117.9 . . ? C26 C25 C24 116.0(13) . . ? C26 C25 C28 121.7(13) . . ? C24 C25 C28 122.1(12) . . ? C25 C26 C27 125.6(15) . . ? C25 C26 H26 117.2 . . ? C27 C26 H26 117.2 . . ? C22 C27 C26 115.6(13) . . ? C22 C27 H27 122.2 . . ? C26 C27 H27 122.2 . . ? O9 C28 O10 118.5(13) . . ? O9 C28 C25 120.2(13) . . ? O10 C28 C25 121.1(12) . . ? C1 O2A H2A 109.5 . . ? C1 O2B H2B 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Dy1 O1 C1 -166.1(13) 2_554 . . . ? O6 Dy1 O1 C1 -55.3(15) . . . . ? O7 Dy1 O1 C1 89.7(13) 3_775 . . . ? O9 Dy1 O1 C1 6.2(13) 2_745 . . . ? O10 Dy1 O1 C1 135.1(12) 4_585 . . . ? O4 Dy1 O1 C1 -76.0(13) 4_676 . . . ? O5 Dy1 O6 C15 -126.4(18) 2_554 . . . ? O7 Dy1 O6 C15 0(2) 3_775 . . . ? O9 Dy1 O6 C15 75.5(18) 2_745 . . . ? O10 Dy1 O6 C15 -53.0(18) 4_585 . . . ? O4 Dy1 O6 C15 154.7(18) 4_676 . . . ? O1 Dy1 O6 C15 133.9(17) . . . . ? Dy1 O1 C1 O2A 3(2) . . . . ? Dy1 O1 C1 O2B -33(2) . . . . ? Dy1 O1 C1 C2 172.8(8) . . . . ? O1 C1 C2 C7 -13(2) . . . . ? O2A C1 C2 C7 157.0(14) . . . . ? O2B C1 C2 C7 -170.2(15) . . . . ? O1 C1 C2 C3 165.8(13) . . . . ? O2A C1 C2 C3 -24(2) . . . . ? O2B C1 C2 C3 9(2) . . . . ? C7 C2 C3 C4 -3(2) . . . . ? C1 C2 C3 C4 178.2(12) . . . . ? C2 C3 C4 C5 -2(2) . . . . ? C8 O3 C5 C6 -114.5(15) . . . . ? C8 O3 C5 C4 68.4(17) . . . . ? C3 C4 C5 C6 2(2) . . . . ? C3 C4 C5 O3 179.2(12) . . . . ? O3 C5 C6 C7 -173.7(12) . . . . ? C4 C5 C6 C7 4(2) . . . . ? C5 C6 C7 C2 -8(2) . . . . ? C3 C2 C7 C6 7.4(19) . . . . ? C1 C2 C7 C6 -173.5(12) . . . . ? C5 O3 C8 C9 38.0(18) . . . . ? C5 O3 C8 C13 -153.6(13) . . . . ? C13 C8 C9 C10 7(2) . . . . ? O3 C8 C9 C10 175.0(12) . . . . ? C8 C9 C10 C11 -6(2) . . . . ? C9 C10 C11 C12 2(2) . . . . ? C10 C11 C12 C13 1(2) . . . . ? C11 C12 C13 C8 1(2) . . . . ? C11 C12 C13 C14 174.3(12) . . . . ? C9 C8 C13 C12 -5(2) . . . . ? O3 C8 C13 C12 -172.7(12) . . . . ? C9 C8 C13 C14 -178.0(13) . . . . ? O3 C8 C13 C14 14(2) . . . . ? Dy1 O4 C14 O5 -22(3) 4_575 . . . ? Dy1 O4 C14 C13 159.9(10) 4_575 . . . ? Dy1 O5 C14 O4 110(3) 2_544 . . . ? Dy1 O5 C14 C13 -72(3) 2_544 . . . ? C12 C13 C14 O4 -138.6(13) . . . . ? C8 C13 C14 O4 35(2) . . . . ? C12 C13 C14 O5 43.0(19) . . . . ? C8 C13 C14 O5 -143.8(14) . . . . ? Dy1 O7 C15 O6 -18(2) 3_775 . . . ? Dy1 O7 C15 C16 166.5(9) 3_775 . . . ? Dy1 O6 C15 O7 12(3) . . . . ? Dy1 O6 C15 C16 -171.8(12) . . . . ? O7 C15 C16 C21 6(2) . . . . ? O6 C15 C16 C21 -170.3(14) . . . . ? O7 C15 C16 C17 -174.1(13) . . . . ? O6 C15 C16 C17 10.0(19) . . . . ? C21 C16 C17 C18 -5(2) . . . . ? C15 C16 C17 C18 175.1(14) . . . . ? C16 C17 C18 C19 6(2) . . . . ? C17 C18 C19 C20 -3(3) . . . . ? C18 C19 C20 C21 -2(2) . . . . ? C22 O8 C21 C16 146.6(13) . . . . ? C22 O8 C21 C20 -35.7(19) . . . . ? C17 C16 C21 O8 177.7(12) . . . . ? C15 C16 C21 O8 -2(2) . . . . ? C17 C16 C21 C20 0(2) . . . . ? C15 C16 C21 C20 -179.8(13) . . . . ? C19 C20 C21 O8 -174.6(13) . . . . ? C19 C20 C21 C16 3(2) . . . . ? C21 O8 C22 C27 -36.3(18) . . . . ? C21 O8 C22 C23 148.8(12) . . . . ? C27 C22 C23 C24 2(2) . . . . ? O8 C22 C23 C24 176.8(12) . . . . ? C22 C23 C24 C25 -1(2) . . . . ? C23 C24 C25 C26 -1(2) . . . . ? C23 C24 C25 C28 -175.5(13) . . . . ? C24 C25 C26 C27 2(2) . . . . ? C28 C25 C26 C27 177.1(13) . . . . ? O8 C22 C27 C26 -174.9(12) . . . . ? C23 C22 C27 C26 0(2) . . . . ? C25 C26 C27 C22 -2(2) . . . . ? Dy1 O9 C28 O10 -4.7(15) 2_755 . . . ? Dy1 O9 C28 C25 -178.4(9) 2_755 . . . ? Dy1 O10 C28 O9 -91(12) 4_686 . . . ? Dy1 O10 C28 C25 82(12) 4_686 . . . ? C26 C25 C28 O9 172.8(13) . . . . ? C24 C25 C28 O9 -13(2) . . . . ? C26 C25 C28 O10 -1(2) . . . . ? C24 C25 C28 O10 173.8(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.990 _refine_diff_density_min -1.492 _refine_diff_density_rms 0.238 _database_code_depnum_ccdc_archive 'CCDC 916442' ####################################################################### # # 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_exp_1339 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H17 O10 Tb' _chemical_formula_weight 672.34 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' 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 P21/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 9.3363(4) _cell_length_b 18.4457(10) _cell_length_c 14.3315(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.174(5) _cell_angle_gamma 90.00 _cell_volume 2461.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1610 _cell_measurement_theta_min 2.5171 _cell_measurement_theta_max 28.4324 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 2.934 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.49044 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8722 _diffrn_reflns_av_R_equivalents 0.0844 _diffrn_reflns_av_sigmaI/netI 0.1254 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4338 _reflns_number_gt 2980 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0742P)^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 4338 _refine_ls_number_parameters 362 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1772 _refine_ls_wR_factor_gt 0.1468 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.006 _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 Tb1 Tb 0.21479(5) 0.47356(3) 0.01105(3) 0.0228(2) Uani 1 1 d . . . O1 O 0.3726(8) 0.3820(4) 0.0889(6) 0.0364(19) Uani 1 1 d . A . O3 O 0.8637(9) 0.1780(5) 0.2728(6) 0.050(2) Uani 1 1 d . A . O4 O 0.8697(7) 0.0598(5) 0.3993(5) 0.038(2) Uani 1 1 d . . . O5 O 1.1038(8) 0.0389(4) 0.4231(5) 0.036(2) Uani 1 1 d . . . O6 O 0.0878(9) 0.5778(4) 0.0450(6) 0.047(2) Uani 1 1 d . . . O7 O -0.1125(8) 0.6391(4) 0.0361(6) 0.038(2) Uani 1 1 d . . . O8 O 0.3133(9) 0.8875(5) 0.1869(6) 0.047(2) Uani 1 1 d . . . O9 O 0.3938(8) 0.9451(5) 0.3531(5) 0.0352(19) Uani 1 1 d . . . O10 O 0.6201(9) 0.9800(6) 0.3725(6) 0.057(3) Uani 1 1 d . . . C1 C 0.3855(13) 0.3156(7) 0.0912(9) 0.044(3) Uani 1 1 d . . . C2 C 0.5131(13) 0.2786(7) 0.1397(8) 0.037(3) Uani 1 1 d . A . C3 C 0.5063(15) 0.2055(7) 0.1581(11) 0.057(4) Uani 1 1 d . . . H3 H 0.4230 0.1795 0.1415 0.068 Uiso 1 1 calc R A . C4 C 0.6240(15) 0.1714(8) 0.2013(10) 0.056(4) Uani 1 1 d . A . H4 H 0.6222 0.1217 0.2114 0.067 Uiso 1 1 calc R . . C5 C 0.7457(13) 0.2113(8) 0.2298(9) 0.046(4) Uani 1 1 d . . . C6 C 0.7477(14) 0.2833(8) 0.2120(11) 0.058(4) Uani 1 1 d . A . H6 H 0.8297 0.3101 0.2293 0.069 Uiso 1 1 calc R . . C7 C 0.6297(14) 0.3173(7) 0.1687(9) 0.051(4) Uani 1 1 d . . . H7 H 0.6307 0.3672 0.1594 0.061 Uiso 1 1 calc R A . C8 C 0.9403(12) 0.1288(7) 0.2224(8) 0.037(3) Uani 1 1 d . . . C9 C 0.9578(14) 0.1390(8) 0.1282(8) 0.052(4) Uani 1 1 d . A . H9 H 0.9115 0.1773 0.0965 0.062 Uiso 1 1 calc R . . C10 C 1.0424(15) 0.0932(8) 0.0817(9) 0.059(4) Uani 1 1 d . . . H10 H 1.0514 0.0994 0.0179 0.071 Uiso 1 1 calc R A . C11 C 1.1149(14) 0.0376(8) 0.1297(9) 0.050(4) Uani 1 1 d . A . H11 H 1.1732 0.0064 0.0983 0.060 Uiso 1 1 calc R . . C12 C 1.1007(12) 0.0285(7) 0.2236(8) 0.036(3) Uani 1 1 d . . . H12 H 1.1517 -0.0082 0.2558 0.043 Uiso 1 1 calc R A . C13 C 1.0123(11) 0.0729(7) 0.2707(7) 0.032(3) Uani 1 1 d . A . C14 C 0.9901(11) 0.0571(6) 0.3720(8) 0.029(3) Uani 1 1 d . . . C15 C 0.0192(13) 0.6364(6) 0.0550(7) 0.031(3) Uani 1 1 d . . . C16 C 0.0996(11) 0.7036(6) 0.0861(8) 0.032(3) Uani 1 1 d . . . C17 C 0.2482(13) 0.7030(7) 0.0991(11) 0.058(4) Uani 1 1 d . . . H17 H 0.2984 0.6609 0.0873 0.069 Uiso 1 1 calc R . . C18 C 0.3225(13) 0.7645(7) 0.1294(11) 0.054(4) Uani 1 1 d . . . H18 H 0.4223 0.7647 0.1352 0.065 Uiso 1 1 calc R . . C19 C 0.2469(12) 0.8247(6) 0.1504(9) 0.037(3) Uani 1 1 d . . . C20 C 0.1006(13) 0.8257(7) 0.1381(9) 0.041(3) Uani 1 1 d . . . H20 H 0.0503 0.8677 0.1503 0.049 Uiso 1 1 calc R . . C21 C 0.0278(11) 0.7643(7) 0.1077(8) 0.035(3) Uani 1 1 d . . . H21 H -0.0721 0.7646 0.1018 0.042 Uiso 1 1 calc R . . C22 C 0.4428(12) 0.9091(7) 0.1585(8) 0.039(3) Uani 1 1 d . . . C23 C 0.4752(16) 0.9000(9) 0.0675(9) 0.065(5) Uani 1 1 d . . . H23 H 0.4108 0.8770 0.0246 0.078 Uiso 1 1 calc R . . C24 C 0.6038(19) 0.9254(10) 0.0405(11) 0.083(6) Uani 1 1 d . . . H24 H 0.6249 0.9202 -0.0216 0.099 Uiso 1 1 calc R . . C25 C 0.7008(17) 0.9577(9) 0.1014(11) 0.069(5) Uani 1 1 d . . . H25 H 0.7893 0.9722 0.0820 0.083 Uiso 1 1 calc R . . C26 C 0.6680(13) 0.9692(7) 0.1920(9) 0.041(3) Uani 1 1 d . . . H26 H 0.7317 0.9941 0.2333 0.049 Uiso 1 1 calc R . . C27 C 0.5395(12) 0.9434(6) 0.2217(8) 0.032(3) Uani 1 1 d . . . C28 C 0.5145(12) 0.9582(6) 0.3233(8) 0.032(3) Uani 1 1 d . . . O2A O 0.273(3) 0.2693(13) 0.068(3) 0.050(10) Uani 0.49(9) 1 d PU A 1 H2AA H 0.2113 0.2906 0.0349 0.075 Uiso 0.49(9) 1 calc PR A 1 O2B O 0.311(4) 0.2765(13) 0.033(3) 0.054(10) Uani 0.51(9) 1 d PU A 2 H2BB H 0.2202 0.2811 0.0327 0.064 Uiso 0.51(9) 1 d PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0225(3) 0.0253(3) 0.0211(3) -0.0004(3) 0.0045(2) 0.0001(2) O1 0.039(4) 0.028(5) 0.042(5) -0.002(4) 0.004(4) 0.005(4) O3 0.059(5) 0.057(6) 0.035(5) 0.002(5) 0.000(4) 0.035(5) O4 0.026(4) 0.061(6) 0.029(4) 0.017(5) 0.010(3) 0.002(4) O5 0.025(4) 0.047(5) 0.035(5) 0.011(4) -0.001(4) 0.006(4) O6 0.053(5) 0.028(5) 0.061(6) -0.011(5) 0.007(5) 0.010(4) O7 0.031(4) 0.040(5) 0.042(5) -0.004(4) -0.004(4) -0.013(4) O8 0.047(5) 0.045(5) 0.051(5) -0.025(5) 0.012(4) -0.012(4) O9 0.033(4) 0.046(5) 0.028(4) -0.008(4) 0.013(4) -0.005(4) O10 0.044(5) 0.095(8) 0.032(5) -0.023(6) 0.007(4) -0.029(5) C1 0.047(7) 0.041(8) 0.042(8) -0.013(7) -0.004(6) -0.010(6) C2 0.052(7) 0.035(7) 0.025(6) -0.003(6) 0.000(6) 0.019(6) C3 0.066(9) 0.025(7) 0.077(11) -0.002(8) -0.011(8) 0.009(7) C4 0.069(9) 0.042(8) 0.055(9) -0.007(8) -0.005(8) 0.023(8) C5 0.047(7) 0.055(9) 0.038(8) -0.007(7) 0.008(6) 0.020(7) C6 0.051(8) 0.050(9) 0.070(10) 0.015(9) -0.014(8) 0.011(7) C7 0.058(8) 0.033(7) 0.061(10) 0.014(8) 0.002(8) 0.002(7) C8 0.043(7) 0.031(7) 0.037(7) 0.005(6) -0.001(6) 0.007(6) C9 0.066(8) 0.071(10) 0.019(6) 0.021(7) 0.004(6) 0.029(8) C10 0.082(10) 0.072(11) 0.027(7) 0.028(8) 0.023(7) 0.033(9) C11 0.052(8) 0.077(11) 0.024(6) 0.002(7) 0.027(6) 0.025(7) C12 0.033(6) 0.045(8) 0.032(6) 0.001(6) 0.017(5) 0.010(6) C13 0.030(5) 0.046(8) 0.020(6) 0.007(6) 0.001(5) -0.005(6) C14 0.028(6) 0.027(6) 0.032(6) 0.001(6) 0.013(5) -0.003(5) C15 0.053(7) 0.026(6) 0.013(5) 0.000(5) -0.005(5) -0.002(6) C16 0.036(6) 0.029(6) 0.031(7) -0.001(6) 0.006(5) -0.001(5) C17 0.040(7) 0.041(8) 0.088(12) -0.023(9) -0.014(8) -0.007(6) C18 0.030(6) 0.042(8) 0.090(12) -0.021(9) -0.010(7) 0.002(6) C19 0.040(6) 0.031(7) 0.042(7) 0.000(6) 0.006(6) -0.006(6) C20 0.042(7) 0.043(8) 0.037(7) -0.002(7) -0.001(6) 0.001(6) C21 0.026(5) 0.043(8) 0.038(7) 0.001(7) 0.007(5) 0.000(5) C22 0.043(7) 0.040(8) 0.035(7) -0.019(7) 0.008(6) -0.002(6) C23 0.070(9) 0.091(13) 0.036(8) -0.024(9) 0.019(7) -0.033(9) C24 0.103(13) 0.097(14) 0.050(10) -0.038(11) 0.019(10) -0.039(12) C25 0.073(10) 0.082(12) 0.058(10) -0.029(10) 0.038(9) -0.019(9) C26 0.046(7) 0.043(8) 0.036(7) -0.020(7) 0.018(6) -0.018(6) C27 0.037(6) 0.029(6) 0.030(6) -0.002(6) 0.008(5) 0.001(5) C28 0.037(6) 0.040(7) 0.019(6) -0.006(6) 0.004(5) -0.005(5) O2A 0.048(11) 0.051(11) 0.050(12) 0.003(5) -0.002(5) 0.000(5) O2B 0.055(11) 0.052(11) 0.053(11) -0.002(5) 0.001(5) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O5 2.231(7) 2_655 ? Tb1 O10 2.280(8) 4_575 ? Tb1 O4 2.318(7) 4_565 ? Tb1 O9 2.320(7) 2_545 ? Tb1 O6 2.329(8) . ? Tb1 O7 2.365(8) 3_565 ? Tb1 O1 2.456(8) . ? O1 C1 1.230(15) . ? O3 C5 1.368(14) . ? O3 C8 1.391(14) . ? O4 C14 1.218(12) . ? O4 Tb1 2.318(7) 4_666 ? O5 C14 1.290(13) . ? O5 Tb1 2.231(7) 2_645 ? O6 C15 1.269(14) . ? O7 C15 1.241(13) . ? O7 Tb1 2.365(8) 3_565 ? O8 C22 1.363(13) . ? O8 C19 1.396(14) . ? O9 C28 1.257(13) . ? O9 Tb1 2.320(7) 2 ? O10 C28 1.237(13) . ? O10 Tb1 2.280(8) 4_676 ? C1 O2B 1.27(2) . ? C1 O2A 1.37(3) . ? C1 C2 1.499(17) . ? C2 C7 1.342(17) . ? C2 C3 1.376(17) . ? C3 C4 1.373(17) . ? C3 H3 0.9300 . ? C4 C5 1.390(18) . ? C4 H4 0.9300 . ? C5 C6 1.352(18) . ? C6 C7 1.376(17) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.384(16) . ? C8 C13 1.388(16) . ? C9 C10 1.363(18) . ? C9 H9 0.9300 . ? C10 C11 1.385(18) . ? C10 H10 0.9300 . ? C11 C12 1.372(17) . ? C11 H11 0.9300 . ? C12 C13 1.374(16) . ? C12 H12 0.9300 . ? C13 C14 1.509(15) . ? C15 C16 1.501(15) . ? C16 C21 1.352(16) . ? C16 C17 1.387(16) . ? C17 C18 1.382(17) . ? C17 H17 0.9300 . ? C18 C19 1.362(17) . ? C18 H18 0.9300 . ? C19 C20 1.364(16) . ? C20 C21 1.374(17) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.371(17) . ? C22 C27 1.384(16) . ? C23 C24 1.37(2) . ? C23 H23 0.9300 . ? C24 C25 1.35(2) . ? C24 H24 0.9300 . ? C25 C26 1.372(18) . ? C25 H25 0.9300 . ? C26 C27 1.385(16) . ? C26 H26 0.9300 . ? C27 C28 1.517(15) . ? O2A H2AA 0.8200 . ? O2A H2BB 0.7154 . ? O2B H2BB 0.8500 . ? 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 O5 Tb1 O10 113.6(3) 2_655 4_575 ? O5 Tb1 O4 86.7(3) 2_655 4_565 ? O10 Tb1 O4 73.7(3) 4_575 4_565 ? O5 Tb1 O9 97.6(3) 2_655 2_545 ? O10 Tb1 O9 130.6(3) 4_575 2_545 ? O4 Tb1 O9 148.5(3) 4_565 2_545 ? O5 Tb1 O6 81.3(3) 2_655 . ? O10 Tb1 O6 72.6(3) 4_575 . ? O4 Tb1 O6 135.8(3) 4_565 . ? O9 Tb1 O6 75.6(3) 2_545 . ? O5 Tb1 O7 150.9(3) 2_655 3_565 ? O10 Tb1 O7 87.6(3) 4_575 3_565 ? O4 Tb1 O7 80.1(3) 4_565 3_565 ? O9 Tb1 O7 81.3(3) 2_545 3_565 ? O6 Tb1 O7 125.7(3) . 3_565 ? O5 Tb1 O1 76.5(3) 2_655 . ? O10 Tb1 O1 146.7(3) 4_575 . ? O4 Tb1 O1 75.4(3) 4_565 . ? O9 Tb1 O1 75.4(3) 2_545 . ? O6 Tb1 O1 140.4(3) . . ? O7 Tb1 O1 75.0(3) 3_565 . ? C1 O1 Tb1 138.6(8) . . ? C5 O3 C8 119.1(9) . . ? C14 O4 Tb1 148.0(7) . 4_666 ? C14 O5 Tb1 161.7(8) . 2_645 ? C15 O6 Tb1 174.2(8) . . ? C15 O7 Tb1 113.6(7) . 3_565 ? C22 O8 C19 120.7(9) . . ? C28 O9 Tb1 134.3(7) . 2 ? C28 O10 Tb1 149.4(8) . 4_676 ? O1 C1 O2B 119.9(16) . . ? O1 C1 O2A 122.7(14) . . ? O2B C1 O2A 28.2(12) . . ? O1 C1 C2 122.5(11) . . ? O2B C1 C2 115.2(14) . . ? O2A C1 C2 113.3(15) . . ? C7 C2 C3 120.6(12) . . ? C7 C2 C1 120.1(12) . . ? C3 C2 C1 119.3(12) . . ? C4 C3 C2 119.2(14) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 120.1(13) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 O3 120.3(13) . . ? C6 C5 C4 119.0(12) . . ? O3 C5 C4 120.6(13) . . ? C5 C6 C7 120.7(14) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C2 C7 C6 120.2(13) . . ? C2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C9 C8 C13 120.0(12) . . ? C9 C8 O3 121.3(11) . . ? C13 C8 O3 118.3(10) . . ? C10 C9 C8 120.5(12) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 119.7(11) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 120.0(12) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.9(12) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 C8 118.9(10) . . ? C12 C13 C14 119.2(11) . . ? C8 C13 C14 121.8(11) . . ? O4 C14 O5 124.7(10) . . ? O4 C14 C13 119.7(10) . . ? O5 C14 C13 115.5(9) . . ? O7 C15 O6 120.7(11) . . ? O7 C15 C16 119.8(10) . . ? O6 C15 C16 119.5(10) . . ? C21 C16 C17 119.0(11) . . ? C21 C16 C15 120.5(10) . . ? C17 C16 C15 120.4(11) . . ? C18 C17 C16 120.6(12) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 118.9(11) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 120.7(12) . . ? C18 C19 O8 122.4(10) . . ? C20 C19 O8 116.8(11) . . ? C19 C20 C21 119.9(12) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C16 C21 C20 120.8(10) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? O8 C22 C23 120.7(12) . . ? O8 C22 C27 119.3(10) . . ? C23 C22 C27 119.9(12) . . ? C24 C23 C22 119.1(14) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C25 C24 C23 121.9(15) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 C26 119.6(14) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C27 119.7(13) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C26 C27 C22 119.6(11) . . ? C26 C27 C28 115.5(10) . . ? C22 C27 C28 124.8(10) . . ? O10 C28 O9 124.5(10) . . ? O10 C28 C27 115.7(10) . . ? O9 C28 C27 119.7(10) . . ? C1 O2A H2AA 109.5 . . ? C1 O2A H2BB 117.1 . . ? H2AA O2A H2BB 12.6 . . ? C1 O2B H2BB 116.1 . . ? 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 O5 Tb1 O1 C1 -169.2(13) 2_655 . . . ? O10 Tb1 O1 C1 -56.6(15) 4_575 . . . ? O4 Tb1 O1 C1 -79.1(13) 4_565 . . . ? O9 Tb1 O1 C1 89.1(13) 2_545 . . . ? O6 Tb1 O1 C1 133.1(12) . . . . ? O7 Tb1 O1 C1 4.4(13) 3_565 . . . ? O5 Tb1 O6 C15 100(8) 2_655 . . . ? O10 Tb1 O6 C15 -18(8) 4_575 . . . ? O4 Tb1 O6 C15 24(8) 4_565 . . . ? O9 Tb1 O6 C15 -160(8) 2_545 . . . ? O7 Tb1 O6 C15 -92(8) 3_565 . . . ? O1 Tb1 O6 C15 156(8) . . . . ? Tb1 O1 C1 O2B 10(3) . . . . ? Tb1 O1 C1 O2A -23(3) . . . . ? Tb1 O1 C1 C2 171.1(8) . . . . ? O1 C1 C2 C7 -11(2) . . . . ? O2B C1 C2 C7 151(3) . . . . ? O2A C1 C2 C7 -178(2) . . . . ? O1 C1 C2 C3 165.3(13) . . . . ? O2B C1 C2 C3 -32(3) . . . . ? O2A C1 C2 C3 -1(3) . . . . ? C7 C2 C3 C4 -4(2) . . . . ? C1 C2 C3 C4 179.1(12) . . . . ? C2 C3 C4 C5 3(2) . . . . ? C8 O3 C5 C6 -112.1(15) . . . . ? C8 O3 C5 C4 66.0(16) . . . . ? C3 C4 C5 C6 -2(2) . . . . ? C3 C4 C5 O3 -179.9(12) . . . . ? O3 C5 C6 C7 179.9(12) . . . . ? C4 C5 C6 C7 2(2) . . . . ? C3 C2 C7 C6 4(2) . . . . ? C1 C2 C7 C6 -179.1(13) . . . . ? C5 C6 C7 C2 -3(2) . . . . ? C5 O3 C8 C9 35.9(18) . . . . ? C5 O3 C8 C13 -150.9(12) . . . . ? C13 C8 C9 C10 2(2) . . . . ? O3 C8 C9 C10 174.9(13) . . . . ? C8 C9 C10 C11 -2(2) . . . . ? C9 C10 C11 C12 0(2) . . . . ? C10 C11 C12 C13 2(2) . . . . ? C11 C12 C13 C8 -1.9(19) . . . . ? C11 C12 C13 C14 174.9(12) . . . . ? C9 C8 C13 C12 0.2(19) . . . . ? O3 C8 C13 C12 -173.1(11) . . . . ? C9 C8 C13 C14 -176.5(12) . . . . ? O3 C8 C13 C14 10.2(17) . . . . ? Tb1 O4 C14 O5 -18(2) 4_666 . . . ? Tb1 O4 C14 C13 159.7(11) 4_666 . . . ? Tb1 O5 C14 O4 98(2) 2_645 . . . ? Tb1 O5 C14 C13 -79(2) 2_645 . . . ? C12 C13 C14 O4 -135.6(12) . . . . ? C8 C13 C14 O4 41.1(17) . . . . ? C12 C13 C14 O5 42.0(16) . . . . ? C8 C13 C14 O5 -141.4(11) . . . . ? Tb1 O7 C15 O6 2.6(14) 3_565 . . . ? Tb1 O7 C15 C16 -179.9(7) 3_565 . . . ? Tb1 O6 C15 O7 85(8) . . . . ? Tb1 O6 C15 C16 -93(8) . . . . ? O7 C15 C16 C21 10.2(17) . . . . ? O6 C15 C16 C21 -172.3(12) . . . . ? O7 C15 C16 C17 -174.0(12) . . . . ? O6 C15 C16 C17 3.5(18) . . . . ? C21 C16 C17 C18 -3(2) . . . . ? C15 C16 C17 C18 -178.8(13) . . . . ? C16 C17 C18 C19 3(2) . . . . ? C17 C18 C19 C20 -3(2) . . . . ? C17 C18 C19 O8 176.0(13) . . . . ? C22 O8 C19 C18 36.1(19) . . . . ? C22 O8 C19 C20 -145.0(12) . . . . ? C18 C19 C20 C21 3(2) . . . . ? O8 C19 C20 C21 -176.2(11) . . . . ? C17 C16 C21 C20 3(2) . . . . ? C15 C16 C21 C20 178.6(11) . . . . ? C19 C20 C21 C16 -2.6(19) . . . . ? C19 O8 C22 C23 36.5(19) . . . . ? C19 O8 C22 C27 -146.4(11) . . . . ? O8 C22 C23 C24 177.0(15) . . . . ? C27 C22 C23 C24 0(2) . . . . ? C22 C23 C24 C25 1(3) . . . . ? C23 C24 C25 C26 -3(3) . . . . ? C24 C25 C26 C27 4(2) . . . . ? C25 C26 C27 C22 -3(2) . . . . ? C25 C26 C27 C28 179.4(13) . . . . ? O8 C22 C27 C26 -176.4(12) . . . . ? C23 C22 C27 C26 1(2) . . . . ? O8 C22 C27 C28 1.3(19) . . . . ? C23 C22 C27 C28 178.4(14) . . . . ? Tb1 O10 C28 O9 -12(3) 4_676 . . . ? Tb1 O10 C28 C27 171.2(12) 4_676 . . . ? Tb1 O9 C28 O10 15.5(19) 2 . . . ? Tb1 O9 C28 C27 -167.9(8) 2 . . . ? C26 C27 C28 O10 -12.1(17) . . . . ? C22 C27 C28 O10 170.1(12) . . . . ? C26 C27 C28 O9 171.0(11) . . . . ? C22 C27 C28 O9 -6.8(19) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.715 _refine_diff_density_min -2.366 _refine_diff_density_rms 0.218 _database_code_depnum_ccdc_archive 'CCDC 916443' ####################################################################### # # 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_exp_1376 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H17 Gd O10' _chemical_formula_weight 670.67 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' Gd Gd -0.1653 3.9035 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 9.3657(5) _cell_length_b 18.4465(10) _cell_length_c 14.3860(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.004(6) _cell_angle_gamma 90.00 _cell_volume 2479.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1871 _cell_measurement_theta_min 2.4877 _cell_measurement_theta_max 28.3774 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 2.736 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8984 _exptl_absorpt_correction_T_max 0.9732 _exptl_absorpt_process_details multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8993 _diffrn_reflns_av_R_equivalents 0.0967 _diffrn_reflns_av_sigmaI/netI 0.1724 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4370 _reflns_number_gt 2575 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^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 4370 _refine_ls_number_parameters 352 _refine_ls_number_restraints 984 _refine_ls_R_factor_all 0.1365 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1583 _refine_ls_wR_factor_gt 0.1243 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.007 _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 Gd1 Gd 0.21356(6) 0.47341(3) 0.01083(4) 0.02248(19) Uani 1 1 d U . . O1 O 0.3958(8) 0.5397(4) 0.0782(6) 0.0330(18) Uani 1 1 d U . . O2 O 0.6291(9) 0.5602(4) 0.0986(6) 0.038(2) Uani 1 1 d U . . O3 O 0.6382(10) 0.6772(4) 0.2265(6) 0.047(2) Uani 1 1 d U . . O4 O 1.2056(13) 0.7713(5) 0.4500(8) 0.077(3) Uani 1 1 d U . . H4C H 1.2909 0.7775 0.4349 0.093 Uiso 1 1 d R . . O5 O 1.1273(9) 0.8815(4) 0.4105(6) 0.038(2) Uani 1 1 d U . . O6 O 0.0828(9) 0.5787(4) 0.0436(6) 0.045(2) Uani 1 1 d U . . O7 O -0.1160(9) 0.6420(4) 0.0364(6) 0.039(2) Uani 1 1 d U . . O8 O 0.3154(10) 0.8861(4) 0.1876(6) 0.0428(19) Uani 1 1 d U . . O9 O 0.3959(9) 0.9444(4) 0.3525(6) 0.040(2) Uani 1 1 d U . . O10 O 0.6219(9) 0.9797(5) 0.3718(6) 0.052(2) Uani 1 1 d U . . C1 C 0.5073(13) 0.5575(6) 0.1279(9) 0.028(2) Uani 1 1 d U . . C2 C 0.4891(13) 0.5725(6) 0.2275(9) 0.031(2) Uani 1 1 d U . . C3 C 0.4006(13) 0.5302(7) 0.2772(9) 0.040(2) Uani 1 1 d U . . H3 H 0.3477 0.4942 0.2452 0.048 Uiso 1 1 calc R . . C4 C 0.3855(14) 0.5376(7) 0.3708(9) 0.046(3) Uani 1 1 d U . . H4A H 0.3280 0.5059 0.4017 0.055 Uiso 1 1 calc R . . C5 C 0.4571(16) 0.5927(7) 0.4176(10) 0.050(3) Uani 1 1 d U . . H5 H 0.4476 0.5995 0.4810 0.061 Uiso 1 1 calc R . . C6 C 0.5457(15) 0.6394(7) 0.3687(10) 0.051(3) Uani 1 1 d U . . H6 H 0.5960 0.6767 0.3997 0.061 Uiso 1 1 calc R . . C7 C 0.5569(14) 0.6290(7) 0.2745(9) 0.038(2) Uani 1 1 d U . . C8 C 0.7561(15) 0.7092(7) 0.2736(10) 0.044(3) Uani 1 1 d U . . C9 C 0.8757(15) 0.6698(7) 0.2975(10) 0.046(3) Uani 1 1 d U . . H9 H 0.8793 0.6205 0.2846 0.056 Uiso 1 1 calc R . . C10 C 0.9936(15) 0.7056(7) 0.3422(10) 0.047(3) Uani 1 1 d U . . H10 H 1.0758 0.6794 0.3601 0.056 Uiso 1 1 calc R . . C11 C 0.9894(15) 0.7787(6) 0.3599(10) 0.042(3) Uani 1 1 d U . . C12 C 0.8697(15) 0.8173(7) 0.3320(10) 0.050(3) Uani 1 1 d U . . H12 H 0.8669 0.8670 0.3428 0.059 Uiso 1 1 calc R . . C13 C 0.7514(16) 0.7827(7) 0.2873(10) 0.050(3) Uani 1 1 d U . . H13 H 0.6705 0.8091 0.2671 0.060 Uiso 1 1 calc R . . C14 C 1.1137(15) 0.8165(7) 0.4082(10) 0.047(3) Uani 1 1 d U . . C15 C 0.0173(14) 0.6376(6) 0.0538(9) 0.034(3) Uani 1 1 d U . . C16 C 0.0991(13) 0.7025(6) 0.0874(9) 0.033(2) Uani 1 1 d U . . C17 C 0.0288(14) 0.7656(6) 0.1094(9) 0.040(3) Uani 1 1 d U . . H17 H -0.0706 0.7666 0.1030 0.048 Uiso 1 1 calc R . . C18 C 0.1013(14) 0.8270(6) 0.1404(9) 0.034(3) Uani 1 1 d U . . H18 H 0.0513 0.8686 0.1549 0.040 Uiso 1 1 calc R . . C19 C 0.2466(14) 0.8260(6) 0.1496(9) 0.039(3) Uani 1 1 d U . . C20 C 0.3233(15) 0.7629(6) 0.1300(10) 0.047(3) Uani 1 1 d U . . H20 H 0.4225 0.7610 0.1386 0.056 Uiso 1 1 calc R . . C21 C 0.2441(15) 0.7038(6) 0.0974(10) 0.043(2) Uani 1 1 d U . . H21 H 0.2934 0.6624 0.0812 0.052 Uiso 1 1 calc R . . C22 C 0.4429(14) 0.9091(6) 0.1575(9) 0.038(2) Uani 1 1 d U . . C23 C 0.4757(16) 0.8991(7) 0.0666(10) 0.052(3) Uani 1 1 d U . . H23 H 0.4114 0.8760 0.0242 0.062 Uiso 1 1 calc R . . C24 C 0.6031(17) 0.9233(8) 0.0399(11) 0.059(3) Uani 1 1 d U . . H24 H 0.6263 0.9148 -0.0210 0.071 Uiso 1 1 calc R . . C25 C 0.6998(16) 0.9602(7) 0.0994(10) 0.054(3) Uani 1 1 d U . . H25 H 0.7830 0.9796 0.0780 0.064 Uiso 1 1 calc R . . C26 C 0.6698(13) 0.9675(6) 0.1914(9) 0.040(2) Uani 1 1 d U . . H26 H 0.7359 0.9901 0.2330 0.048 Uiso 1 1 calc R . . C27 C 0.5434(14) 0.9417(6) 0.2227(9) 0.036(2) Uani 1 1 d U . . C28 C 0.5159(15) 0.9562(6) 0.3233(9) 0.037(3) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0130(3) 0.0257(3) 0.0281(3) -0.0004(3) -0.0029(2) 0.0012(3) O1 0.023(4) 0.033(4) 0.042(4) -0.007(3) -0.005(3) -0.003(3) O2 0.025(4) 0.050(4) 0.039(5) -0.009(4) 0.006(4) -0.012(4) O3 0.044(4) 0.052(4) 0.045(4) -0.008(4) -0.003(4) -0.022(4) O4 0.073(4) 0.070(4) 0.087(4) 0.005(3) -0.011(3) -0.003(3) O5 0.033(5) 0.033(4) 0.047(5) -0.001(4) -0.004(4) -0.005(4) O6 0.035(4) 0.034(4) 0.063(5) -0.013(4) -0.015(4) 0.003(4) O7 0.028(5) 0.035(4) 0.052(5) -0.011(4) -0.011(4) -0.003(4) O8 0.036(4) 0.040(4) 0.051(4) -0.021(4) 0.000(4) -0.010(3) O9 0.031(5) 0.050(4) 0.039(5) -0.011(4) 0.012(4) -0.007(4) O10 0.031(5) 0.075(5) 0.048(5) -0.011(5) 0.002(4) -0.013(5) C1 0.024(5) 0.031(5) 0.029(5) -0.004(4) -0.001(4) -0.003(4) C2 0.024(5) 0.038(5) 0.032(5) -0.013(4) 0.006(4) -0.010(4) C3 0.030(5) 0.047(5) 0.042(5) -0.013(5) -0.005(5) -0.011(5) C4 0.043(6) 0.055(6) 0.042(6) -0.009(6) 0.009(5) -0.014(5) C5 0.056(6) 0.056(6) 0.041(6) -0.020(5) 0.012(6) -0.020(6) C6 0.046(5) 0.059(5) 0.047(5) -0.015(5) -0.002(5) -0.016(5) C7 0.031(5) 0.046(5) 0.036(5) -0.010(4) 0.005(4) -0.011(4) C8 0.041(5) 0.043(5) 0.048(6) -0.015(5) -0.004(5) -0.017(5) C9 0.046(6) 0.038(5) 0.053(6) -0.004(5) -0.013(5) -0.010(5) C10 0.042(6) 0.039(5) 0.056(6) 0.000(5) -0.013(5) -0.004(5) C11 0.040(6) 0.032(5) 0.052(6) -0.007(5) -0.005(5) -0.010(5) C12 0.045(6) 0.044(5) 0.057(6) -0.012(5) -0.014(5) -0.007(5) C13 0.043(5) 0.048(5) 0.058(5) -0.009(5) -0.011(5) -0.007(5) C14 0.041(6) 0.041(6) 0.055(6) 0.007(6) -0.019(5) -0.006(5) C15 0.032(5) 0.028(5) 0.041(5) -0.010(5) -0.009(5) 0.004(5) C16 0.025(5) 0.027(5) 0.046(6) -0.007(5) -0.002(5) -0.002(4) C17 0.031(5) 0.036(5) 0.052(5) -0.012(5) -0.007(5) 0.000(5) C18 0.032(5) 0.025(5) 0.044(5) -0.011(5) 0.002(5) 0.002(5) C19 0.032(5) 0.035(5) 0.048(5) -0.013(5) -0.009(5) -0.011(5) C20 0.037(5) 0.044(5) 0.058(5) -0.018(5) -0.010(5) -0.005(5) C21 0.039(5) 0.035(4) 0.055(5) -0.014(4) -0.006(5) 0.000(4) C22 0.029(5) 0.044(5) 0.042(5) -0.013(4) 0.001(4) -0.011(4) C23 0.044(6) 0.064(6) 0.048(6) -0.018(5) 0.003(5) -0.028(5) C24 0.056(7) 0.078(6) 0.045(6) -0.018(6) 0.013(6) -0.024(6) C25 0.045(6) 0.069(6) 0.049(6) -0.007(6) 0.015(6) -0.020(6) C26 0.027(5) 0.051(5) 0.042(5) -0.015(5) 0.006(4) -0.020(5) C27 0.030(5) 0.039(5) 0.039(5) -0.007(4) 0.004(4) -0.011(4) C28 0.035(6) 0.039(5) 0.038(6) -0.005(5) 0.003(5) -0.008(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 Gd1 O1 2.262(8) . ? Gd1 O10 2.290(9) 4_575 ? Gd1 O2 2.314(8) 3_665 ? Gd1 O9 2.342(8) 2_545 ? Gd1 O6 2.361(8) . ? Gd1 O7 2.397(7) 3_565 ? Gd1 O5 2.478(8) 2_645 ? O1 C1 1.267(14) . ? O2 C1 1.245(13) . ? O2 Gd1 2.314(8) 3_665 ? O3 C7 1.385(13) . ? O3 C8 1.387(15) . ? O4 C14 1.313(16) . ? O4 H4C 0.8500 . ? O5 C14 1.206(13) . ? O5 Gd1 2.478(8) 2_655 ? O6 C15 1.261(13) . ? O7 C15 1.258(14) . ? O7 Gd1 2.397(7) 3_565 ? O8 C22 1.367(14) . ? O8 C19 1.376(13) . ? O9 C28 1.246(14) . ? O9 Gd1 2.342(8) 2 ? O10 C28 1.251(15) . ? O10 Gd1 2.290(9) 4_676 ? C1 C2 1.481(16) . ? C2 C7 1.374(16) . ? C2 C3 1.375(15) . ? C3 C4 1.370(16) . ? C3 H3 0.9300 . ? C4 C5 1.370(16) . ? C4 H4A 0.9300 . ? C5 C6 1.417(16) . ? C5 H5 0.9300 . ? C6 C7 1.380(17) . ? C6 H6 0.9300 . ? C8 C9 1.360(18) . ? C8 C13 1.370(15) . ? C9 C10 1.403(18) . ? C9 H9 0.9300 . ? C10 C11 1.374(15) . ? C10 H10 0.9300 . ? C11 C12 1.364(18) . ? C11 C14 1.487(18) . ? C12 C13 1.397(18) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.484(16) . ? C16 C21 1.356(17) . ? C16 C17 1.385(15) . ? C17 C18 1.378(15) . ? C17 H17 0.9300 . ? C18 C19 1.359(17) . ? C18 H18 0.9300 . ? C19 C20 1.406(16) . ? C20 C21 1.381(16) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.376(17) . ? C22 C27 1.415(17) . ? C23 C24 1.354(17) . ? C23 H23 0.9300 . ? C24 C25 1.382(19) . ? C24 H24 0.9300 . ? C25 C26 1.378(17) . ? C25 H25 0.9300 . ? C26 C27 1.381(15) . ? C26 H26 0.9300 . ? C27 C28 1.512(17) . ? 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 Gd1 O10 113.3(3) . 4_575 ? O1 Gd1 O2 86.5(3) . 3_665 ? O10 Gd1 O2 74.0(3) 4_575 3_665 ? O1 Gd1 O9 97.2(3) . 2_545 ? O10 Gd1 O9 131.3(3) 4_575 2_545 ? O2 Gd1 O9 147.8(3) 3_665 2_545 ? O1 Gd1 O6 81.7(3) . . ? O10 Gd1 O6 72.3(3) 4_575 . ? O2 Gd1 O6 136.0(3) 3_665 . ? O9 Gd1 O6 75.9(3) 2_545 . ? O1 Gd1 O7 149.7(3) . 3_565 ? O10 Gd1 O7 88.6(3) 4_575 3_565 ? O2 Gd1 O7 79.5(3) 3_665 3_565 ? O9 Gd1 O7 81.6(3) 2_545 3_565 ? O6 Gd1 O7 126.5(3) . 3_565 ? O1 Gd1 O5 76.2(3) . 2_645 ? O10 Gd1 O5 146.5(3) 4_575 2_645 ? O2 Gd1 O5 74.7(3) 3_665 2_645 ? O9 Gd1 O5 75.2(3) 2_545 2_645 ? O6 Gd1 O5 140.8(3) . 2_645 ? O7 Gd1 O5 74.2(3) 3_565 2_645 ? C1 O1 Gd1 161.7(8) . . ? C1 O2 Gd1 149.6(8) . 3_665 ? C7 O3 C8 118.5(11) . . ? C14 O4 H4C 113.3 . . ? C14 O5 Gd1 138.7(9) . 2_655 ? C15 O6 Gd1 174.3(9) . . ? C15 O7 Gd1 110.6(7) . 3_565 ? C22 O8 C19 121.3(10) . . ? C28 O9 Gd1 134.5(8) . 2 ? C28 O10 Gd1 148.5(9) . 4_676 ? O2 C1 O1 123.9(11) . . ? O2 C1 C2 119.4(11) . . ? O1 C1 C2 116.6(11) . . ? C7 C2 C3 116.8(11) . . ? C7 C2 C1 122.5(11) . . ? C3 C2 C1 120.7(10) . . ? C4 C3 C2 124.1(12) . . ? C4 C3 H3 117.9 . . ? C2 C3 H3 117.9 . . ? C3 C4 C5 118.6(13) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? C4 C5 C6 119.3(13) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C7 C6 C5 119.4(12) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C2 C7 C6 121.6(12) . . ? C2 C7 O3 119.5(11) . . ? C6 C7 O3 118.8(11) . . ? C9 C8 C13 121.8(13) . . ? C9 C8 O3 120.6(11) . . ? C13 C8 O3 117.4(13) . . ? C8 C9 C10 118.2(12) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? C11 C10 C9 121.0(13) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 119.5(13) . . ? C12 C11 C14 119.5(11) . . ? C10 C11 C14 121.0(13) . . ? C11 C12 C13 120.4(12) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C8 C13 C12 119.1(14) . . ? C8 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? O5 C14 O4 123.7(13) . . ? O5 C14 C11 123.8(13) . . ? O4 C14 C11 112.5(11) . . ? O7 C15 O6 121.1(11) . . ? O7 C15 C16 119.7(11) . . ? O6 C15 C16 119.2(11) . . ? C21 C16 C17 116.7(11) . . ? C21 C16 C15 122.7(11) . . ? C17 C16 C15 120.6(12) . . ? C18 C17 C16 122.2(12) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C19 C18 C17 119.2(11) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 O8 117.8(11) . . ? C18 C19 C20 120.9(11) . . ? O8 C19 C20 121.0(12) . . ? C21 C20 C19 116.9(13) . . ? C21 C20 H20 121.6 . . ? C19 C20 H20 121.6 . . ? C16 C21 C20 124.1(12) . . ? C16 C21 H21 118.0 . . ? C20 C21 H21 118.0 . . ? O8 C22 C23 121.2(12) . . ? O8 C22 C27 118.5(11) . . ? C23 C22 C27 120.3(13) . . ? C24 C23 C22 119.0(13) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C25 122.6(14) . . ? C23 C24 H24 118.7 . . ? C25 C24 H24 118.7 . . ? C26 C25 C24 118.3(13) . . ? C26 C25 H25 120.8 . . ? C24 C25 H25 120.8 . . ? C25 C26 C27 121.1(12) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C26 C27 C22 118.4(12) . . ? C26 C27 C28 117.3(11) . . ? C22 C27 C28 124.1(12) . . ? O9 C28 O10 124.9(12) . . ? O9 C28 C27 120.6(12) . . ? O10 C28 C27 114.4(12) . . ? 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 O10 Gd1 O1 C1 -156(3) 4_575 . . . ? O2 Gd1 O1 C1 -85(3) 3_665 . . . ? O9 Gd1 O1 C1 63(3) 2_545 . . . ? O6 Gd1 O1 C1 138(3) . . . . ? O7 Gd1 O1 C1 -23(3) 3_565 . . . ? O5 Gd1 O1 C1 -10(3) 2_645 . . . ? O1 Gd1 O6 C15 82(8) . . . . ? O10 Gd1 O6 C15 -36(8) 4_575 . . . ? O2 Gd1 O6 C15 6(9) 3_665 . . . ? O9 Gd1 O6 C15 -178(8) 2_545 . . . ? O7 Gd1 O6 C15 -110(8) 3_565 . . . ? O5 Gd1 O6 C15 138(8) 2_645 . . . ? Gd1 O2 C1 O1 -20(2) 3_665 . . . ? Gd1 O2 C1 C2 157.1(11) 3_665 . . . ? Gd1 O1 C1 O2 96(3) . . . . ? Gd1 O1 C1 C2 -81(3) . . . . ? O2 C1 C2 C7 43.8(18) . . . . ? O1 C1 C2 C7 -138.9(13) . . . . ? O2 C1 C2 C3 -137.0(12) . . . . ? O1 C1 C2 C3 40.3(17) . . . . ? C7 C2 C3 C4 -5(2) . . . . ? C1 C2 C3 C4 175.5(13) . . . . ? C2 C3 C4 C5 3(2) . . . . ? C3 C4 C5 C6 -1(2) . . . . ? C4 C5 C6 C7 1(2) . . . . ? C3 C2 C7 C6 5(2) . . . . ? C1 C2 C7 C6 -175.8(13) . . . . ? C3 C2 C7 O3 -174.8(11) . . . . ? C1 C2 C7 O3 4(2) . . . . ? C5 C6 C7 C2 -3(2) . . . . ? C5 C6 C7 O3 176.8(12) . . . . ? C8 O3 C7 C2 -148.8(12) . . . . ? C8 O3 C7 C6 31.5(18) . . . . ? C7 O3 C8 C9 71.5(18) . . . . ? C7 O3 C8 C13 -114.1(14) . . . . ? C13 C8 C9 C10 4(2) . . . . ? O3 C8 C9 C10 177.8(12) . . . . ? C8 C9 C10 C11 -1(2) . . . . ? C9 C10 C11 C12 -1(2) . . . . ? C9 C10 C11 C14 179.3(13) . . . . ? C10 C11 C12 C13 1(2) . . . . ? C14 C11 C12 C13 -179.4(14) . . . . ? C9 C8 C13 C12 -4(2) . . . . ? O3 C8 C13 C12 -178.1(13) . . . . ? C11 C12 C13 C8 1(2) . . . . ? Gd1 O5 C14 O4 -7(2) 2_655 . . . ? Gd1 O5 C14 C11 171.6(9) 2_655 . . . ? C12 C11 C14 O5 -14(2) . . . . ? C10 C11 C14 O5 165.8(13) . . . . ? C12 C11 C14 O4 164.9(14) . . . . ? C10 C11 C14 O4 -16(2) . . . . ? Gd1 O7 C15 O6 1.6(16) 3_565 . . . ? Gd1 O7 C15 C16 -178.0(9) 3_565 . . . ? Gd1 O6 C15 O7 104(8) . . . . ? Gd1 O6 C15 C16 -76(9) . . . . ? O7 C15 C16 C21 -172.3(13) . . . . ? O6 C15 C16 C21 8(2) . . . . ? O7 C15 C16 C17 7.0(19) . . . . ? O6 C15 C16 C17 -172.6(12) . . . . ? C21 C16 C17 C18 0(2) . . . . ? C15 C16 C17 C18 -179.7(12) . . . . ? C16 C17 C18 C19 0(2) . . . . ? C17 C18 C19 O8 -175.0(11) . . . . ? C17 C18 C19 C20 -2(2) . . . . ? C22 O8 C19 C18 -144.4(13) . . . . ? C22 O8 C19 C20 42.1(18) . . . . ? C18 C19 C20 C21 3(2) . . . . ? O8 C19 C20 C21 176.1(12) . . . . ? C17 C16 C21 C20 2(2) . . . . ? C15 C16 C21 C20 -178.8(13) . . . . ? C19 C20 C21 C16 -3(2) . . . . ? C19 O8 C22 C23 31.2(19) . . . . ? C19 O8 C22 C27 -146.8(12) . . . . ? O8 C22 C23 C24 179.5(12) . . . . ? C27 C22 C23 C24 -2(2) . . . . ? C22 C23 C24 C25 -2(2) . . . . ? C23 C24 C25 C26 5(2) . . . . ? C24 C25 C26 C27 -3(2) . . . . ? C25 C26 C27 C22 -2(2) . . . . ? C25 C26 C27 C28 -176.3(12) . . . . ? O8 C22 C27 C26 -177.5(11) . . . . ? C23 C22 C27 C26 4(2) . . . . ? O8 C22 C27 C28 -3.2(19) . . . . ? C23 C22 C27 C28 178.7(12) . . . . ? Gd1 O9 C28 O10 12(2) 2 . . . ? Gd1 O9 C28 C27 -168.3(8) 2 . . . ? Gd1 O10 C28 O9 -8(3) 4_676 . . . ? Gd1 O10 C28 C27 172.7(11) 4_676 . . . ? C26 C27 C28 O9 169.1(12) . . . . ? C22 C27 C28 O9 -5.2(19) . . . . ? C26 C27 C28 O10 -11.4(17) . . . . ? C22 C27 C28 O10 174.3(12) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.440 _refine_diff_density_min -1.574 _refine_diff_density_rms 0.214 _database_code_depnum_ccdc_archive 'CCDC 916444' ####################################################################### # # 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_exp_1344 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H17 Ho O10' _chemical_formula_weight 678.35 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' Ho Ho -0.2175 4.6783 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 9.3135(4) _cell_length_b 18.5484(11) _cell_length_c 14.2816(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.483(4) _cell_angle_gamma 90.00 _cell_volume 2459.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.5228 _cell_measurement_theta_max 28.3434 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.832 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 3.278 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.96773 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15685 _diffrn_reflns_av_R_equivalents 0.1061 _diffrn_reflns_av_sigmaI/netI 0.1155 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4340 _reflns_number_gt 2901 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 4340 _refine_ls_number_parameters 364 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0696 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.008 _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 Ho1 Ho 0.78409(4) 0.52643(2) 0.48836(3) 0.01976(12) Uani 1 1 d . . . O1 O 0.6294(6) 0.6170(3) 0.4114(4) 0.0348(16) Uani 1 1 d . A . O3 O 0.1360(6) 0.8231(4) 0.2258(4) 0.0454(18) Uani 1 1 d . A . O4 O 0.1340(5) 0.9390(3) 0.0996(4) 0.0318(16) Uani 1 1 d . . . O5 O -0.1013(5) 0.9622(3) 0.0758(4) 0.0291(15) Uani 1 1 d . . . O6 O 0.8895(5) 0.6360(3) 0.5356(4) 0.0322(15) Uani 1 1 d . . . O7 O 1.0949(6) 0.5778(4) 0.5445(4) 0.0457(18) Uani 1 1 d . . . O8 O 1.3107(6) 0.8866(3) 0.6869(4) 0.0387(17) Uani 1 1 d . . . O9 O 1.3918(6) 0.9453(3) 0.8542(4) 0.0339(16) Uani 1 1 d . . . O10 O 1.6192(6) 0.9813(4) 0.8741(4) 0.0466(18) Uani 1 1 d . . . C1 C 0.6159(10) 0.6821(6) 0.4101(7) 0.043(3) Uani 1 1 d . . . C2 C 0.4905(9) 0.7202(5) 0.3607(7) 0.036(2) Uani 1 1 d . A . C3 C 0.4945(10) 0.7932(6) 0.3442(7) 0.048(3) Uani 1 1 d . . . H3 H 0.5777 0.8191 0.3618 0.058 Uiso 1 1 calc R A . C4 C 0.3753(10) 0.8285(5) 0.3017(7) 0.053(3) Uani 1 1 d . A . H4 H 0.3773 0.8780 0.2918 0.063 Uiso 1 1 calc R . . C5 C 0.2553(10) 0.7895(6) 0.2745(6) 0.039(3) Uani 1 1 d . . . C6 C 0.2514(10) 0.7161(6) 0.2871(7) 0.051(3) Uani 1 1 d . A . H6 H 0.1702 0.6898 0.2660 0.061 Uiso 1 1 calc R . . C7 C 0.3699(10) 0.6819(5) 0.3317(7) 0.048(3) Uani 1 1 d . . . H7 H 0.3674 0.6324 0.3420 0.058 Uiso 1 1 calc R A . C8 C 0.0607(9) 0.8711(5) 0.2764(6) 0.030(2) Uani 1 1 d . . . C9 C 0.0449(9) 0.8605(6) 0.3714(7) 0.050(3) Uani 1 1 d . A . H9 H 0.0930 0.8230 0.4036 0.060 Uiso 1 1 calc R . . C10 C -0.0427(10) 0.9061(6) 0.4172(7) 0.057(3) Uani 1 1 d . . . H10 H -0.0537 0.8992 0.4807 0.068 Uiso 1 1 calc R A . C11 C -0.1142(9) 0.9617(6) 0.3702(6) 0.044(3) Uani 1 1 d . A . H11 H -0.1727 0.9926 0.4016 0.053 Uiso 1 1 calc R . . C12 C -0.0980(8) 0.9710(5) 0.2757(6) 0.032(2) Uani 1 1 d . . . H12 H -0.1478 1.0082 0.2438 0.039 Uiso 1 1 calc R A . C13 C -0.0095(8) 0.9266(5) 0.2269(6) 0.023(2) Uani 1 1 d . A . C14 C 0.0099(9) 0.9431(4) 0.1267(6) 0.024(2) Uani 1 1 d . . . C15 C 1.0258(9) 0.6350(5) 0.5545(6) 0.031(2) Uani 1 1 d . . . C16 C 1.1005(8) 0.7022(4) 0.5860(6) 0.022(2) Uani 1 1 d . . . C17 C 1.0268(8) 0.7634(5) 0.6056(6) 0.032(2) Uani 1 1 d . . . H17 H 0.9268 0.7638 0.5972 0.038 Uiso 1 1 calc R . . C18 C 1.0996(8) 0.8249(5) 0.6379(6) 0.027(2) Uani 1 1 d . . . H18 H 1.0487 0.8664 0.6506 0.032 Uiso 1 1 calc R . . C19 C 1.2466(9) 0.8241(5) 0.6509(6) 0.030(2) Uani 1 1 d . . . C20 C 1.3243(9) 0.7642(6) 0.6301(8) 0.054(3) Uani 1 1 d . . . H20 H 1.4244 0.7647 0.6367 0.065 Uiso 1 1 calc R . . C21 C 1.2501(9) 0.7022(5) 0.5987(7) 0.046(3) Uani 1 1 d . . . H21 H 1.3011 0.6607 0.5863 0.056 Uiso 1 1 calc R . . C22 C 1.4424(9) 0.9091(5) 0.6579(6) 0.029(2) Uani 1 1 d . . . C23 C 1.4761(11) 0.9004(6) 0.5667(7) 0.061(4) Uani 1 1 d . . . H23 H 1.4112 0.8776 0.5236 0.073 Uiso 1 1 calc R . . C24 C 1.6045(12) 0.9251(7) 0.5387(8) 0.082(5) Uani 1 1 d . . . H24 H 1.6264 0.9182 0.4769 0.098 Uiso 1 1 calc R . . C25 C 1.7015(10) 0.9600(6) 0.6005(7) 0.056(3) Uani 1 1 d . . . H25 H 1.7885 0.9769 0.5814 0.067 Uiso 1 1 calc R . . C26 C 1.6662(8) 0.9691(5) 0.6912(6) 0.033(2) Uani 1 1 d . . . H26 H 1.7315 0.9927 0.7333 0.040 Uiso 1 1 calc R . . C27 C 1.5367(8) 0.9446(5) 0.7237(6) 0.026(2) Uani 1 1 d . . . C28 C 1.5127(9) 0.9586(5) 0.8242(6) 0.030(2) Uani 1 1 d . . . O2A O 0.691(4) 0.7232(13) 0.470(3) 0.043(8) Uani 0.46(7) 1 d PU A 1 H2A H 0.6878 0.7067 0.5230 0.064 Uiso 0.46(7) 1 calc PR A 1 O2B O 0.729(3) 0.7271(10) 0.433(3) 0.050(7) Uani 0.54(7) 1 d PU A 2 H2B H 0.7936 0.7046 0.4626 0.075 Uiso 0.54(7) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.01477(19) 0.0220(2) 0.0222(2) -0.0003(2) -0.00074(15) 0.0000(2) O1 0.036(4) 0.019(4) 0.048(4) 0.006(3) -0.005(3) 0.011(3) O3 0.049(4) 0.048(5) 0.039(4) 0.002(4) 0.001(3) 0.029(4) O4 0.018(3) 0.049(5) 0.029(4) 0.019(3) 0.009(3) 0.005(3) O5 0.020(3) 0.038(4) 0.028(3) 0.010(3) -0.003(3) 0.006(3) O6 0.024(3) 0.025(4) 0.046(4) -0.007(3) -0.009(3) -0.002(3) O7 0.040(4) 0.036(5) 0.060(5) -0.006(4) -0.002(3) 0.005(3) O8 0.035(4) 0.036(4) 0.046(4) -0.021(3) 0.008(3) -0.018(3) O9 0.030(3) 0.034(4) 0.039(4) -0.004(3) 0.010(3) -0.007(3) O10 0.038(4) 0.071(6) 0.031(4) -0.019(4) 0.000(3) -0.012(4) C1 0.035(6) 0.045(8) 0.047(7) 0.003(6) -0.008(5) 0.008(5) C2 0.036(6) 0.034(7) 0.038(6) 0.007(5) 0.001(5) 0.013(5) C3 0.044(6) 0.031(7) 0.068(8) 0.001(6) -0.009(6) 0.001(5) C4 0.060(7) 0.017(6) 0.077(9) -0.002(6) -0.024(6) 0.011(5) C5 0.044(6) 0.043(8) 0.030(6) 0.005(5) -0.005(5) 0.017(5) C6 0.033(6) 0.044(8) 0.073(8) 0.017(6) -0.014(6) 0.005(5) C7 0.049(6) 0.027(7) 0.066(8) 0.017(6) -0.004(6) 0.009(5) C8 0.035(5) 0.032(6) 0.026(5) 0.009(5) 0.011(4) 0.015(5) C9 0.042(6) 0.062(8) 0.047(7) 0.017(6) 0.009(5) 0.026(6) C10 0.065(7) 0.073(10) 0.033(7) 0.024(6) 0.016(6) 0.029(7) C11 0.037(5) 0.059(8) 0.037(6) 0.006(6) 0.008(5) 0.016(5) C12 0.034(5) 0.029(6) 0.035(6) 0.007(5) 0.012(4) 0.017(5) C13 0.024(4) 0.026(6) 0.020(5) 0.005(4) 0.008(4) -0.001(4) C14 0.026(5) 0.019(5) 0.027(5) 0.000(4) 0.005(4) -0.003(4) C15 0.038(6) 0.028(6) 0.025(5) -0.010(5) -0.009(5) -0.002(5) C16 0.023(5) 0.013(5) 0.030(5) -0.004(4) -0.010(4) -0.002(4) C17 0.019(5) 0.027(6) 0.048(6) -0.005(5) 0.000(4) -0.010(4) C18 0.021(5) 0.029(6) 0.029(5) -0.006(4) -0.005(4) 0.012(4) C19 0.033(5) 0.022(6) 0.035(6) -0.006(5) -0.001(5) -0.006(4) C20 0.016(5) 0.048(8) 0.096(9) -0.025(7) -0.010(5) -0.002(5) C21 0.028(5) 0.036(7) 0.074(8) -0.012(6) -0.008(5) 0.004(5) C22 0.030(5) 0.028(6) 0.029(6) -0.005(5) 0.007(4) -0.010(4) C23 0.070(8) 0.074(9) 0.040(7) -0.032(6) 0.013(6) -0.041(7) C24 0.084(9) 0.116(12) 0.049(8) -0.044(8) 0.031(7) -0.050(8) C25 0.052(6) 0.084(10) 0.036(6) -0.018(6) 0.032(5) -0.032(6) C26 0.032(5) 0.035(6) 0.033(5) -0.001(5) 0.002(4) -0.012(5) C27 0.026(5) 0.028(6) 0.026(5) 0.004(4) 0.004(4) -0.002(4) C28 0.038(5) 0.025(6) 0.027(5) -0.005(4) 0.003(5) -0.009(4) O2A 0.044(11) 0.044(10) 0.040(11) 0.001(8) -0.009(8) 0.009(7) O2B 0.041(9) 0.048(8) 0.060(11) 0.005(7) -0.002(8) 0.004(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 Ho1 O5 2.216(5) 2_545 ? Ho1 O10 2.257(6) 2_746 ? Ho1 O4 2.288(5) 4_676 ? Ho1 O9 2.292(6) 4_575 ? Ho1 O7 2.304(6) 3_766 ? Ho1 O6 2.334(6) . ? Ho1 O1 2.420(6) . ? O1 C1 1.214(11) . ? O3 C8 1.373(9) . ? O3 C5 1.409(10) . ? O4 C14 1.249(8) . ? O4 Ho1 2.288(5) 4_575 ? O5 C14 1.269(9) . ? O5 Ho1 2.216(5) 2 ? O6 C15 1.277(9) . ? O7 C15 1.256(10) . ? O7 Ho1 2.304(6) 3_766 ? O8 C19 1.385(9) . ? O8 C22 1.389(9) . ? O9 C28 1.259(8) . ? O9 Ho1 2.292(6) 4_676 ? O10 C28 1.249(9) . ? O10 Ho1 2.257(6) 2_756 ? C1 O2A 1.31(2) . ? C1 O2B 1.36(2) . ? C1 C2 1.494(12) . ? C2 C7 1.365(12) . ? C2 C3 1.375(13) . ? C3 C4 1.387(11) . ? C3 H3 0.9300 . ? C4 C5 1.362(12) . ? C4 H4 0.9300 . ? C5 C6 1.374(13) . ? C6 C7 1.385(11) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.385(11) . ? C8 C9 1.389(11) . ? C9 C10 1.375(12) . ? C9 H9 0.9300 . ? C10 C11 1.375(12) . ? C10 H10 0.9300 . ? C11 C12 1.379(11) . ? C11 H11 0.9300 . ? C12 C13 1.391(10) . ? C12 H12 0.9300 . ? C13 C14 1.487(11) . ? C15 C16 1.480(11) . ? C16 C17 1.366(11) . ? C16 C21 1.391(10) . ? C17 C18 1.387(11) . ? C17 H17 0.9300 . ? C18 C19 1.367(10) . ? C18 H18 0.9300 . ? C19 C20 1.372(12) . ? C20 C21 1.395(12) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.372(11) . ? C22 C27 1.400(11) . ? C23 C24 1.370(12) . ? C23 H23 0.9300 . ? C24 C25 1.374(12) . ? C24 H24 0.9300 . ? C25 C26 1.372(11) . ? C25 H25 0.9300 . ? C26 C27 1.402(10) . ? C26 H26 0.9300 . ? C27 C28 1.492(11) . ? O2A H2A 0.8200 . ? O2B H2B 0.8200 . ? 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 O5 Ho1 O10 113.7(2) 2_545 2_746 ? O5 Ho1 O4 86.91(18) 2_545 4_676 ? O10 Ho1 O4 74.0(2) 2_746 4_676 ? O5 Ho1 O9 98.61(19) 2_545 4_575 ? O10 Ho1 O9 129.90(19) 2_746 4_575 ? O4 Ho1 O9 147.9(2) 4_676 4_575 ? O5 Ho1 O7 80.6(2) 2_545 3_766 ? O10 Ho1 O7 72.4(2) 2_746 3_766 ? O4 Ho1 O7 135.4(2) 4_676 3_766 ? O9 Ho1 O7 76.6(2) 4_575 3_766 ? O5 Ho1 O6 151.6(2) 2_545 . ? O10 Ho1 O6 86.7(2) 2_746 . ? O4 Ho1 O6 79.7(2) 4_676 . ? O9 Ho1 O6 80.8(2) 4_575 . ? O7 Ho1 O6 126.02(19) 3_766 . ? O5 Ho1 O1 77.0(2) 2_545 . ? O10 Ho1 O1 146.7(2) 2_746 . ? O4 Ho1 O1 75.3(2) 4_676 . ? O9 Ho1 O1 75.3(2) 4_575 . ? O7 Ho1 O1 140.6(2) 3_766 . ? O6 Ho1 O1 75.5(2) . . ? C1 O1 Ho1 139.0(6) . . ? C8 O3 C5 116.2(7) . . ? C14 O4 Ho1 145.9(5) . 4_575 ? C14 O5 Ho1 162.4(6) . 2 ? C15 O6 Ho1 115.9(5) . . ? C15 O7 Ho1 174.7(6) . 3_766 ? C19 O8 C22 120.3(7) . . ? C28 O9 Ho1 134.5(5) . 4_676 ? C28 O10 Ho1 150.1(6) . 2_756 ? O1 C1 O2A 121.5(14) . . ? O1 C1 O2B 121.9(12) . . ? O2A C1 O2B 28.5(12) . . ? O1 C1 C2 123.7(9) . . ? O2A C1 C2 112.9(13) . . ? O2B C1 C2 112.6(12) . . ? C7 C2 C3 119.5(9) . . ? C7 C2 C1 119.4(9) . . ? C3 C2 C1 121.1(9) . . ? C2 C3 C4 120.5(9) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 119.1(10) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 121.2(9) . . ? C4 C5 O3 120.3(9) . . ? C6 C5 O3 118.4(9) . . ? C5 C6 C7 119.1(9) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C2 C7 C6 120.6(10) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? O3 C8 C13 116.9(8) . . ? O3 C8 C9 121.3(8) . . ? C13 C8 C9 121.5(8) . . ? C10 C9 C8 119.3(9) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 120.8(9) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 119.0(9) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C11 C12 C13 122.1(9) . . ? C11 C12 H12 119.0 . . ? C13 C12 H12 119.0 . . ? C8 C13 C12 117.3(8) . . ? C8 C13 C14 123.8(8) . . ? C12 C13 C14 118.8(8) . . ? O4 C14 O5 124.9(8) . . ? O4 C14 C13 118.1(7) . . ? O5 C14 C13 116.9(7) . . ? O7 C15 O6 119.8(8) . . ? O7 C15 C16 120.9(8) . . ? O6 C15 C16 119.2(8) . . ? C17 C16 C21 119.2(8) . . ? C17 C16 C15 122.0(7) . . ? C21 C16 C15 118.8(8) . . ? C16 C17 C18 120.7(8) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C19 C18 C17 119.7(8) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 121.2(8) . . ? C18 C19 O8 116.1(8) . . ? C20 C19 O8 122.7(8) . . ? C19 C20 C21 118.7(8) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C16 C21 C20 120.5(9) . . ? C16 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C23 C22 O8 121.4(8) . . ? C23 C22 C27 120.9(8) . . ? O8 C22 C27 117.6(7) . . ? C24 C23 C22 120.5(10) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 121.0(10) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 118.1(9) . . ? C26 C25 H25 121.0 . . ? C24 C25 H25 121.0 . . ? C25 C26 C27 123.3(8) . . ? C25 C26 H26 118.3 . . ? C27 C26 H26 118.3 . . ? C22 C27 C26 116.2(8) . . ? C22 C27 C28 126.4(8) . . ? C26 C27 C28 117.4(8) . . ? O10 C28 O9 124.3(8) . . ? O10 C28 C27 115.8(8) . . ? O9 C28 C27 119.9(8) . . ? C1 O2A H2A 109.5 . . ? C1 O2B H2B 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Ho1 O1 C1 167.0(10) 2_545 . . . ? O10 Ho1 O1 C1 53.6(11) 2_746 . . . ? O4 Ho1 O1 C1 76.8(10) 4_676 . . . ? O9 Ho1 O1 C1 -90.3(10) 4_575 . . . ? O7 Ho1 O1 C1 -136.0(9) 3_766 . . . ? O6 Ho1 O1 C1 -6.1(10) . . . . ? O5 Ho1 O6 C15 -165.3(5) 2_545 . . . ? O10 Ho1 O6 C15 57.2(6) 2_746 . . . ? O4 Ho1 O6 C15 131.5(6) 4_676 . . . ? O9 Ho1 O6 C15 -74.2(6) 4_575 . . . ? O7 Ho1 O6 C15 -8.2(7) 3_766 . . . ? O1 Ho1 O6 C15 -151.2(6) . . . . ? Ho1 O1 C1 O2A -9(3) . . . . ? Ho1 O1 C1 O2B 25(3) . . . . ? Ho1 O1 C1 C2 -171.5(6) . . . . ? O1 C1 C2 C7 14.1(15) . . . . ? O2A C1 C2 C7 -150(3) . . . . ? O2B C1 C2 C7 179(2) . . . . ? O1 C1 C2 C3 -166.0(10) . . . . ? O2A C1 C2 C3 30(3) . . . . ? O2B C1 C2 C3 -1(2) . . . . ? C7 C2 C3 C4 2.4(16) . . . . ? C1 C2 C3 C4 -177.4(9) . . . . ? C2 C3 C4 C5 -1.5(16) . . . . ? C3 C4 C5 C6 -1.1(16) . . . . ? C3 C4 C5 O3 -176.0(8) . . . . ? C8 O3 C5 C4 -69.2(12) . . . . ? C8 O3 C5 C6 115.7(10) . . . . ? C4 C5 C6 C7 2.6(16) . . . . ? O3 C5 C6 C7 177.6(8) . . . . ? C3 C2 C7 C6 -0.9(15) . . . . ? C1 C2 C7 C6 179.0(9) . . . . ? C5 C6 C7 C2 -1.6(16) . . . . ? C5 O3 C8 C13 151.7(8) . . . . ? C5 O3 C8 C9 -34.1(13) . . . . ? O3 C8 C9 C10 -173.8(9) . . . . ? C13 C8 C9 C10 0.1(16) . . . . ? C8 C9 C10 C11 -0.1(17) . . . . ? C9 C10 C11 C12 0.6(16) . . . . ? C10 C11 C12 C13 -1.1(15) . . . . ? O3 C8 C13 C12 173.6(8) . . . . ? C9 C8 C13 C12 -0.7(14) . . . . ? O3 C8 C13 C14 -9.5(13) . . . . ? C9 C8 C13 C14 176.3(8) . . . . ? C11 C12 C13 C8 1.2(13) . . . . ? C11 C12 C13 C14 -176.0(8) . . . . ? Ho1 O4 C14 O5 18.8(15) 4_575 . . . ? Ho1 O4 C14 C13 -159.2(7) 4_575 . . . ? Ho1 O5 C14 O4 -103.5(18) 2 . . . ? Ho1 O5 C14 C13 74.6(19) 2 . . . ? C8 C13 C14 O4 -40.2(12) . . . . ? C12 C13 C14 O4 136.7(8) . . . . ? C8 C13 C14 O5 141.6(9) . . . . ? C12 C13 C14 O5 -41.4(11) . . . . ? Ho1 O7 C15 O6 66(7) 3_766 . . . ? Ho1 O7 C15 C16 -113(7) 3_766 . . . ? Ho1 O6 C15 O7 2.1(11) . . . . ? Ho1 O6 C15 C16 -179.3(6) . . . . ? O7 C15 C16 C17 -173.9(9) . . . . ? O6 C15 C16 C17 7.5(13) . . . . ? O7 C15 C16 C21 4.0(13) . . . . ? O6 C15 C16 C21 -174.5(8) . . . . ? C21 C16 C17 C18 0.0(14) . . . . ? C15 C16 C17 C18 177.9(8) . . . . ? C16 C17 C18 C19 -0.5(14) . . . . ? C17 C18 C19 C20 1.9(14) . . . . ? C17 C18 C19 O8 -177.4(8) . . . . ? C22 O8 C19 C18 -144.7(8) . . . . ? C22 O8 C19 C20 36.0(13) . . . . ? C18 C19 C20 C21 -2.6(16) . . . . ? O8 C19 C20 C21 176.6(9) . . . . ? C17 C16 C21 C20 -0.8(15) . . . . ? C15 C16 C21 C20 -178.8(9) . . . . ? C19 C20 C21 C16 2.1(16) . . . . ? C19 O8 C22 C23 36.9(13) . . . . ? C19 O8 C22 C27 -146.7(8) . . . . ? O8 C22 C23 C24 177.8(10) . . . . ? C27 C22 C23 C24 1.4(17) . . . . ? C22 C23 C24 C25 -1(2) . . . . ? C23 C24 C25 C26 0.3(19) . . . . ? C24 C25 C26 C27 0.1(17) . . . . ? C23 C22 C27 C26 -1.0(14) . . . . ? O8 C22 C27 C26 -177.5(7) . . . . ? C23 C22 C27 C28 179.0(9) . . . . ? O8 C22 C27 C28 2.5(13) . . . . ? C25 C26 C27 C22 0.3(14) . . . . ? C25 C26 C27 C28 -179.7(9) . . . . ? Ho1 O10 C28 O9 -10(2) 2_756 . . . ? Ho1 O10 C28 C27 172.2(9) 2_756 . . . ? Ho1 O9 C28 O10 15.2(14) 4_676 . . . ? Ho1 O9 C28 C27 -167.1(6) 4_676 . . . ? C22 C27 C28 O10 169.6(9) . . . . ? C26 C27 C28 O10 -10.4(12) . . . . ? C22 C27 C28 O9 -8.3(14) . . . . ? C26 C27 C28 O9 171.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.358 _refine_diff_density_min -0.902 _refine_diff_density_rms 0.177 _database_code_depnum_ccdc_archive 'CCDC 916445' ####################################################################### # # 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_exp_1353 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H17 Er O10' _chemical_formula_weight 680.68 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 9.2869(3) _cell_length_b 18.5404(9) _cell_length_c 14.2415(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.635(3) _cell_angle_gamma 90.00 _cell_volume 2444.11(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1662 _cell_measurement_theta_min 2.5123 _cell_measurement_theta_max 28.3831 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.850 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 3.495 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8864 _exptl_absorpt_correction_T_max 0.9408 _exptl_absorpt_process_details multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8782 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0907 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4313 _reflns_number_gt 3126 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 4313 _refine_ls_number_parameters 364 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0668 _refine_ls_wR_factor_gt 0.0572 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 0.78341(3) 0.526329(18) 0.98817(2) 0.01756(9) Uani 1 1 d . . . O1 O 0.6001(4) 0.4630(3) 0.9253(3) 0.0308(13) Uani 1 1 d . . . O2 O 0.3660(4) 0.4387(3) 0.9007(3) 0.0300(13) Uani 1 1 d . . . O3 O 0.3632(5) 0.3228(3) 0.7735(3) 0.0452(16) Uani 1 1 d . . . O5 O -0.1294(5) 0.1169(3) 0.5893(3) 0.0335(13) Uani 1 1 d . . . O6 O 0.9012(5) 0.4227(3) 0.9542(3) 0.0427(15) Uani 1 1 d . . . O7 O 1.1085(4) 0.3649(3) 0.9644(3) 0.0306(13) Uani 1 1 d . . . O8 O 0.6901(5) 0.1124(3) 0.8142(3) 0.0360(14) Uani 1 1 d . . . O9 O 0.6099(4) 0.0539(3) 0.6462(3) 0.0296(13) Uani 1 1 d . . . O10 O 0.3819(4) 0.0170(3) 0.6252(3) 0.0455(16) Uani 1 1 d . . . C1 C 0.4884(6) 0.4441(4) 0.8733(4) 0.0189(16) Uani 1 1 d . . . C2 C 0.5100(6) 0.4259(4) 0.7713(4) 0.0196(16) Uani 1 1 d . . . C3 C 0.5988(7) 0.4720(5) 0.7238(5) 0.037(2) Uani 1 1 d . . . H3 H 0.6484 0.5089 0.7566 0.045 Uiso 1 1 calc R . . C4 C 0.6135(8) 0.4631(5) 0.6297(5) 0.050(3) Uani 1 1 d . . . H4 H 0.6704 0.4948 0.5980 0.060 Uiso 1 1 calc R . . C5 C 0.5437(8) 0.4073(6) 0.5825(5) 0.057(3) Uani 1 1 d . . . H5 H 0.5543 0.4006 0.5187 0.068 Uiso 1 1 calc R . . C6 C 0.4567(8) 0.3602(5) 0.6296(5) 0.051(3) Uani 1 1 d . . . H6 H 0.4105 0.3219 0.5976 0.062 Uiso 1 1 calc R . . C7 C 0.4397(7) 0.3709(4) 0.7239(5) 0.0290(19) Uani 1 1 d . . . C8 C 0.2447(8) 0.2890(5) 0.7262(5) 0.037(2) Uani 1 1 d . . . C9 C 0.1231(8) 0.3296(5) 0.6996(5) 0.047(2) Uani 1 1 d . . . H9 H 0.1199 0.3789 0.7111 0.057 Uiso 1 1 calc R . . C10 C 0.0052(9) 0.2929(5) 0.6546(5) 0.048(2) Uani 1 1 d . . . H10 H -0.0779 0.3185 0.6350 0.057 Uiso 1 1 calc R . . C11 C 0.0091(8) 0.2202(4) 0.6386(5) 0.034(2) Uani 1 1 d . A . C12 C 0.1308(8) 0.1798(5) 0.6689(5) 0.046(2) Uani 1 1 d . . . H12 H 0.1331 0.1300 0.6605 0.056 Uiso 1 1 calc R . . C13 C 0.2487(9) 0.2167(5) 0.7125(6) 0.053(3) Uani 1 1 d . . . H13 H 0.3318 0.1913 0.7325 0.064 Uiso 1 1 calc R . . C14 C -0.1170(9) 0.1814(5) 0.5891(6) 0.039(2) Uani 1 1 d . . . C15 C 0.9709(7) 0.3659(4) 0.9455(4) 0.0220(17) Uani 1 1 d . . . C16 C 0.8979(6) 0.2981(4) 0.9141(4) 0.0200(16) Uani 1 1 d . . . C17 C 0.7487(8) 0.2975(5) 0.9015(5) 0.047(2) Uani 1 1 d . . . H17 H 0.6968 0.3387 0.9147 0.056 Uiso 1 1 calc R . . C18 C 0.6765(8) 0.2363(5) 0.8696(6) 0.049(3) Uani 1 1 d . . . H18 H 0.5761 0.2360 0.8618 0.059 Uiso 1 1 calc R . . C19 C 0.7532(7) 0.1759(4) 0.8495(5) 0.0283(19) Uani 1 1 d . . . C20 C 0.9020(7) 0.1763(4) 0.8608(4) 0.0276(19) Uani 1 1 d . . . H20 H 0.9541 0.1354 0.8465 0.033 Uiso 1 1 calc R . . C21 C 0.9735(7) 0.2381(4) 0.8936(4) 0.0256(18) Uani 1 1 d . . . H21 H 1.0739 0.2385 0.9017 0.031 Uiso 1 1 calc R . . C22 C 0.5585(7) 0.0906(4) 0.8410(5) 0.0308(19) Uani 1 1 d . . . C23 C 0.5251(9) 0.0993(5) 0.9322(5) 0.055(3) Uani 1 1 d . . . H23 H 0.5907 0.1221 0.9752 0.066 Uiso 1 1 calc R . . C24 C 0.3972(9) 0.0750(6) 0.9610(6) 0.072(3) Uani 1 1 d . . . H24 H 0.3758 0.0818 1.0231 0.086 Uiso 1 1 calc R . . C25 C 0.2990(8) 0.0401(5) 0.8979(5) 0.055(3) Uani 1 1 d . . . H25 H 0.2120 0.0229 0.9171 0.066 Uiso 1 1 calc R . . C26 C 0.3328(7) 0.0315(4) 0.8068(5) 0.0319(19) Uani 1 1 d . . . H26 H 0.2664 0.0092 0.7638 0.038 Uiso 1 1 calc R . . C27 C 0.4631(6) 0.0551(4) 0.7767(4) 0.0223(17) Uani 1 1 d . . . C28 C 0.4890(7) 0.0417(4) 0.6754(4) 0.0272(19) Uani 1 1 d . . . O4A O -0.226(2) 0.2258(8) 0.562(2) 0.043(7) Uani 0.60(7) 1 d PU A 1 H4A H -0.2906 0.2028 0.5328 0.065 Uiso 0.60(7) 1 calc PR A 1 O4B O -0.192(4) 0.2228(16) 0.522(4) 0.061(9) Uani 0.40(7) 1 d PU A 2 H4B H -0.2490 0.1974 0.4904 0.092 Uiso 0.40(7) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01252(14) 0.01895(18) 0.02090(17) 0.00005(18) -0.00054(10) 0.00028(17) O1 0.020(2) 0.038(4) 0.033(3) -0.008(3) -0.006(2) -0.006(3) O2 0.019(2) 0.047(4) 0.025(3) -0.018(3) 0.009(2) -0.004(2) O3 0.054(3) 0.049(4) 0.032(3) -0.009(3) 0.000(3) -0.035(3) O5 0.029(3) 0.020(3) 0.051(3) -0.005(3) -0.001(2) -0.005(3) O6 0.035(3) 0.024(3) 0.068(4) -0.012(3) 0.001(3) 0.009(3) O7 0.027(3) 0.021(3) 0.042(3) -0.007(3) -0.008(2) -0.004(2) O8 0.031(3) 0.032(4) 0.045(3) -0.018(3) 0.003(2) -0.017(3) O9 0.028(3) 0.035(4) 0.027(3) -0.009(3) 0.006(2) -0.009(2) O10 0.031(3) 0.075(5) 0.031(3) -0.022(3) 0.001(2) -0.018(3) C1 0.013(3) 0.016(4) 0.027(4) -0.002(3) 0.001(3) -0.001(3) C2 0.012(3) 0.027(5) 0.020(4) -0.007(4) 0.000(3) 0.000(3) C3 0.029(4) 0.053(6) 0.031(4) -0.008(5) 0.008(3) -0.023(5) C4 0.057(5) 0.064(8) 0.030(5) -0.008(5) 0.014(4) -0.027(5) C5 0.058(6) 0.085(9) 0.029(5) -0.022(5) 0.017(4) -0.021(6) C6 0.048(5) 0.063(7) 0.043(5) -0.027(5) 0.007(4) -0.023(5) C7 0.028(4) 0.026(5) 0.033(5) -0.005(4) 0.002(3) -0.008(4) C8 0.037(5) 0.033(6) 0.040(5) -0.005(4) -0.002(4) -0.023(4) C9 0.057(6) 0.028(6) 0.054(6) -0.006(5) -0.015(4) -0.010(5) C10 0.053(5) 0.026(6) 0.061(6) 0.009(5) -0.016(4) -0.002(5) C11 0.034(4) 0.025(5) 0.043(5) -0.003(4) -0.007(4) -0.014(4) C12 0.043(5) 0.029(6) 0.066(6) -0.008(5) -0.008(4) -0.013(4) C13 0.042(5) 0.046(7) 0.069(7) -0.016(6) -0.010(5) 0.001(5) C14 0.043(5) 0.030(6) 0.042(5) 0.003(5) -0.004(4) -0.011(5) C15 0.029(4) 0.022(5) 0.014(4) 0.000(3) -0.005(3) 0.003(4) C16 0.017(4) 0.014(4) 0.029(4) 0.000(3) 0.001(3) -0.002(3) C17 0.032(5) 0.028(6) 0.079(7) -0.019(5) -0.008(4) 0.008(4) C18 0.020(4) 0.045(6) 0.081(7) -0.022(5) -0.004(4) -0.007(4) C19 0.022(4) 0.029(5) 0.033(4) -0.013(4) -0.003(3) -0.005(4) C20 0.021(4) 0.025(5) 0.037(5) -0.008(4) 0.002(3) 0.008(3) C21 0.028(4) 0.019(5) 0.030(4) 0.002(4) 0.004(3) -0.003(4) C22 0.038(4) 0.025(5) 0.029(4) -0.007(4) 0.002(3) -0.010(4) C23 0.069(6) 0.077(8) 0.019(4) -0.019(5) 0.008(4) -0.034(6) C24 0.084(7) 0.100(10) 0.036(5) -0.033(6) 0.036(5) -0.046(7) C25 0.043(5) 0.063(8) 0.062(6) -0.019(6) 0.030(4) -0.025(5) C26 0.030(4) 0.036(5) 0.031(4) -0.021(4) 0.005(3) -0.011(4) C27 0.019(3) 0.021(4) 0.026(4) -0.001(3) -0.003(3) 0.003(3) C28 0.031(4) 0.027(5) 0.023(4) -0.007(4) -0.002(3) -0.004(4) O4A 0.043(9) 0.030(7) 0.052(10) -0.005(6) -0.024(6) -0.002(5) O4B 0.069(11) 0.049(11) 0.064(13) 0.004(9) -0.006(9) -0.011(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 Er1 O1 2.199(4) . ? Er1 O10 2.236(4) 4_666 ? Er1 O2 2.281(4) 3_667 ? Er1 O6 2.283(5) . ? Er1 O9 2.283(4) 2_656 ? Er1 O7 2.328(5) 3_767 ? Er1 O5 2.414(5) 2_556 ? O1 C1 1.274(6) . ? O2 C1 1.236(7) . ? O2 Er1 2.281(4) 3_667 ? O3 C7 1.371(8) . ? O3 C8 1.392(8) . ? O5 C14 1.202(9) . ? O5 Er1 2.414(5) 2_546 ? O6 C15 1.247(8) . ? O7 C15 1.284(7) . ? O7 Er1 2.328(5) 3_767 ? O8 C22 1.371(8) . ? O8 C19 1.391(8) . ? O9 C28 1.249(7) . ? O9 Er1 2.283(4) 2_646 ? O10 C28 1.263(7) . ? O10 Er1 2.236(4) 4_565 ? C1 C2 1.520(8) . ? C2 C7 1.360(9) . ? C2 C3 1.400(9) . ? C3 C4 1.368(8) . ? C3 H3 0.9300 . ? C4 C5 1.369(11) . ? C4 H4 0.9300 . ? C5 C6 1.397(11) . ? C5 H5 0.9300 . ? C6 C7 1.378(9) . ? C6 H6 0.9300 . ? C8 C13 1.355(12) . ? C8 C9 1.384(10) . ? C9 C10 1.400(9) . ? C9 H9 0.9300 . ? C10 C11 1.368(11) . ? C10 H10 0.9300 . ? C11 C12 1.395(10) . ? C11 C14 1.499(9) . ? C12 C13 1.394(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O4A 1.338(16) . ? C14 O4B 1.37(3) . ? C15 C16 1.480(9) . ? C16 C21 1.360(9) . ? C16 C17 1.383(8) . ? C17 C18 1.375(10) . ? C17 H17 0.9300 . ? C18 C19 1.370(10) . ? C18 H18 0.9300 . ? C19 C20 1.378(8) . ? C20 C21 1.386(9) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.370(9) . ? C22 C27 1.387(8) . ? C23 C24 1.364(10) . ? C23 H23 0.9300 . ? C24 C25 1.388(10) . ? C24 H24 0.9300 . ? C25 C26 1.369(9) . ? C25 H25 0.9300 . ? C26 C27 1.386(8) . ? C26 H26 0.9300 . ? C27 C28 1.502(8) . ? O4A H4A 0.8200 . ? O4B H4B 0.8200 . ? 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 O10 114.35(19) . 4_666 ? O1 Er1 O2 86.55(15) . 3_667 ? O10 Er1 O2 74.09(16) 4_666 3_667 ? O1 Er1 O6 80.36(17) . . ? O10 Er1 O6 73.33(19) 4_666 . ? O2 Er1 O6 135.65(19) 3_667 . ? O1 Er1 O9 98.77(16) . 2_656 ? O10 Er1 O9 129.59(15) 4_666 2_656 ? O2 Er1 O9 147.90(18) 3_667 2_656 ? O6 Er1 O9 76.31(18) . 2_656 ? O1 Er1 O7 151.94(17) . 3_767 ? O10 Er1 O7 85.49(19) 4_666 3_767 ? O2 Er1 O7 79.92(17) 3_667 3_767 ? O6 Er1 O7 126.00(16) . 3_767 ? O9 Er1 O7 80.96(17) 2_656 3_767 ? O1 Er1 O5 76.99(18) . 2_556 ? O10 Er1 O5 146.51(19) 4_666 2_556 ? O2 Er1 O5 75.40(17) 3_667 2_556 ? O6 Er1 O5 139.94(17) . 2_556 ? O9 Er1 O5 75.07(16) 2_656 2_556 ? O7 Er1 O5 75.86(16) 3_767 2_556 ? C1 O1 Er1 161.9(5) . . ? C1 O2 Er1 145.4(4) . 3_667 ? C7 O3 C8 117.8(5) . . ? C14 O5 Er1 138.2(5) . 2_546 ? C15 O6 Er1 173.3(5) . . ? C15 O7 Er1 116.6(5) . 3_767 ? C22 O8 C19 120.5(6) . . ? C28 O9 Er1 134.5(4) . 2_646 ? C28 O10 Er1 150.8(4) . 4_565 ? O2 C1 O1 124.4(6) . . ? O2 C1 C2 118.7(5) . . ? O1 C1 C2 116.9(5) . . ? C7 C2 C3 119.7(6) . . ? C7 C2 C1 123.2(6) . . ? C3 C2 C1 117.0(6) . . ? C4 C3 C2 120.7(7) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.4(8) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 120.4(7) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 119.6(7) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C2 C7 O3 118.6(6) . . ? C2 C7 C6 120.2(7) . . ? O3 C7 C6 120.9(7) . . ? C13 C8 C9 122.0(7) . . ? C13 C8 O3 119.0(7) . . ? C9 C8 O3 118.9(7) . . ? C8 C9 C10 116.8(8) . . ? C8 C9 H9 121.6 . . ? C10 C9 H9 121.6 . . ? C11 C10 C9 121.7(8) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 120.6(7) . . ? C10 C11 C14 121.3(7) . . ? C12 C11 C14 118.1(7) . . ? C13 C12 C11 117.5(8) . . ? C13 C12 H12 121.3 . . ? C11 C12 H12 121.3 . . ? C8 C13 C12 121.4(8) . . ? C8 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? O5 C14 O4A 122.8(10) . . ? O5 C14 O4B 121.1(15) . . ? O4A C14 O4B 28.7(14) . . ? O5 C14 C11 123.2(8) . . ? O4A C14 C11 112.7(9) . . ? O4B C14 C11 113.0(13) . . ? O6 C15 O7 120.4(7) . . ? O6 C15 C16 121.2(6) . . ? O7 C15 C16 118.4(7) . . ? C21 C16 C17 119.6(7) . . ? C21 C16 C15 121.9(6) . . ? C17 C16 C15 118.4(7) . . ? C18 C17 C16 120.4(8) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 119.7(7) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 120.3(7) . . ? C18 C19 O8 123.8(6) . . ? C20 C19 O8 115.8(7) . . ? C19 C20 C21 119.5(7) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C16 C21 C20 120.5(6) . . ? C16 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 O8 120.3(6) . . ? C23 C22 C27 120.0(7) . . ? O8 C22 C27 119.5(6) . . ? C24 C23 C22 121.0(7) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 120.1(7) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 118.6(7) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 C27 122.0(6) . . ? C25 C26 H26 119.0 . . ? C27 C26 H26 119.0 . . ? C26 C27 C22 118.2(6) . . ? C26 C27 C28 117.1(5) . . ? C22 C27 C28 124.7(6) . . ? O9 C28 O10 124.4(6) . . ? O9 C28 C27 120.5(5) . . ? O10 C28 C27 115.1(6) . . ? C14 O4A H4A 109.5 . . ? C14 O4B H4B 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O10 Er1 O1 C1 165.7(14) 4_666 . . . ? O2 Er1 O1 C1 94.9(14) 3_667 . . . ? O6 Er1 O1 C1 -127.7(14) . . . . ? O9 Er1 O1 C1 -53.3(14) 2_656 . . . ? O7 Er1 O1 C1 33.9(15) 3_767 . . . ? O5 Er1 O1 C1 19.1(14) 2_556 . . . ? O1 Er1 O6 C15 -125(4) . . . . ? O10 Er1 O6 C15 -6(4) 4_666 . . . ? O2 Er1 O6 C15 -50(5) 3_667 . . . ? O9 Er1 O6 C15 133(5) 2_656 . . . ? O7 Er1 O6 C15 66(5) 3_767 . . . ? O5 Er1 O6 C15 179(100) 2_556 . . . ? Er1 O2 C1 O1 22.2(13) 3_667 . . . ? Er1 O2 C1 C2 -159.1(6) 3_667 . . . ? Er1 O1 C1 O2 -108.1(14) . . . . ? Er1 O1 C1 C2 73.2(16) . . . . ? O2 C1 C2 C7 -37.5(10) . . . . ? O1 C1 C2 C7 141.3(7) . . . . ? O2 C1 C2 C3 137.7(7) . . . . ? O1 C1 C2 C3 -43.5(9) . . . . ? C7 C2 C3 C4 1.3(11) . . . . ? C1 C2 C3 C4 -174.1(7) . . . . ? C2 C3 C4 C5 -2.0(13) . . . . ? C3 C4 C5 C6 0.9(14) . . . . ? C4 C5 C6 C7 0.9(14) . . . . ? C3 C2 C7 O3 174.5(6) . . . . ? C1 C2 C7 O3 -10.4(10) . . . . ? C3 C2 C7 C6 0.5(11) . . . . ? C1 C2 C7 C6 175.6(7) . . . . ? C8 O3 C7 C2 151.6(7) . . . . ? C8 O3 C7 C6 -34.4(11) . . . . ? C5 C6 C7 C2 -1.6(12) . . . . ? C5 C6 C7 O3 -175.5(7) . . . . ? C7 O3 C8 C13 114.5(9) . . . . ? C7 O3 C8 C9 -69.2(10) . . . . ? C13 C8 C9 C10 -2.2(13) . . . . ? O3 C8 C9 C10 -178.3(7) . . . . ? C8 C9 C10 C11 0.8(13) . . . . ? C9 C10 C11 C12 1.5(14) . . . . ? C9 C10 C11 C14 -179.2(7) . . . . ? C10 C11 C12 C13 -2.4(13) . . . . ? C14 C11 C12 C13 178.3(7) . . . . ? C9 C8 C13 C12 1.3(14) . . . . ? O3 C8 C13 C12 177.4(7) . . . . ? C11 C12 C13 C8 1.1(13) . . . . ? Er1 O5 C14 O4A 23(2) 2_546 . . . ? Er1 O5 C14 O4B -11(3) 2_546 . . . ? Er1 O5 C14 C11 -170.9(5) 2_546 . . . ? C10 C11 C14 O5 -165.5(9) . . . . ? C12 C11 C14 O5 13.8(13) . . . . ? C10 C11 C14 O4A 2(2) . . . . ? C12 C11 C14 O4A -178.8(19) . . . . ? C10 C11 C14 O4B 33(3) . . . . ? C12 C11 C14 O4B -148(3) . . . . ? Er1 O6 C15 O7 -60(5) . . . . ? Er1 O6 C15 C16 119(4) . . . . ? Er1 O7 C15 O6 -1.1(8) 3_767 . . . ? Er1 O7 C15 C16 179.3(4) 3_767 . . . ? O6 C15 C16 C21 172.1(7) . . . . ? O7 C15 C16 C21 -8.3(10) . . . . ? O6 C15 C16 C17 -5.0(10) . . . . ? O7 C15 C16 C17 174.6(6) . . . . ? C21 C16 C17 C18 0.9(12) . . . . ? C15 C16 C17 C18 178.0(7) . . . . ? C16 C17 C18 C19 -0.6(13) . . . . ? C17 C18 C19 C20 -0.2(13) . . . . ? C17 C18 C19 O8 -177.9(7) . . . . ? C22 O8 C19 C18 -34.4(11) . . . . ? C22 O8 C19 C20 147.8(6) . . . . ? C18 C19 C20 C21 0.7(12) . . . . ? O8 C19 C20 C21 178.5(6) . . . . ? C17 C16 C21 C20 -0.4(11) . . . . ? C15 C16 C21 C20 -177.4(6) . . . . ? C19 C20 C21 C16 -0.4(11) . . . . ? C19 O8 C22 C23 -39.0(11) . . . . ? C19 O8 C22 C27 145.6(7) . . . . ? O8 C22 C23 C24 -177.0(9) . . . . ? C27 C22 C23 C24 -1.6(15) . . . . ? C22 C23 C24 C25 0.7(16) . . . . ? C23 C24 C25 C26 -0.7(16) . . . . ? C24 C25 C26 C27 1.6(14) . . . . ? C25 C26 C27 C22 -2.4(12) . . . . ? C25 C26 C27 C28 179.1(8) . . . . ? C23 C22 C27 C26 2.4(12) . . . . ? O8 C22 C27 C26 177.9(7) . . . . ? C23 C22 C27 C28 -179.3(8) . . . . ? O8 C22 C27 C28 -3.8(11) . . . . ? Er1 O9 C28 O10 -11.3(12) 2_646 . . . ? Er1 O9 C28 C27 167.6(5) 2_646 . . . ? Er1 O10 C28 O9 3.6(17) 4_565 . . . ? Er1 O10 C28 C27 -175.4(8) 4_565 . . . ? C26 C27 C28 O9 -171.8(7) . . . . ? C22 C27 C28 O9 9.9(11) . . . . ? C26 C27 C28 O10 7.2(10) . . . . ? C22 C27 C28 O10 -171.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.883 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.161 _database_code_depnum_ccdc_archive 'CCDC 916447' ####################################################################### # # 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_exp_1354 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H17 Eu O10' _chemical_formula_weight 665.38 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' Eu Eu -0.1578 3.6682 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 9.3601(7) _cell_length_b 18.4170(15) _cell_length_c 14.3938(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.847(7) _cell_angle_gamma 90.00 _cell_volume 2475.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1871 _cell_measurement_theta_min 2.4877 _cell_measurement_theta_max 28.3774 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 2.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8984 _exptl_absorpt_correction_T_max 0.9732 _exptl_absorpt_process_details multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9443 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0774 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4364 _reflns_number_gt 3230 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4364 _refine_ls_number_parameters 364 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0789 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.038 _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 Eu1 Eu 0.71323(3) 0.973391(16) 0.01069(2) 0.02121(10) Uani 1 1 d . . . O1 O 0.8724(4) 0.8807(2) 0.0890(3) 0.0363(11) Uani 1 1 d . A . O3 O 1.3623(5) 0.6769(2) 0.2734(3) 0.0477(13) Uani 1 1 d . A . O4 O 1.3710(4) 0.5605(2) 0.3997(3) 0.0383(11) Uani 1 1 d . . . O5 O 1.6055(4) 0.5393(2) 0.4220(3) 0.0331(10) Uani 1 1 d . . . O6 O 0.6047(4) 0.9444(2) 0.1482(3) 0.0357(11) Uani 1 1 d . . . O7 O 0.3768(4) 0.9777(3) 0.1285(3) 0.0528(14) Uani 1 1 d . . . O8 O 0.6855(5) 0.8862(2) 0.3121(3) 0.0434(12) Uani 1 1 d . . . O9 O 0.9203(5) 0.5781(2) 0.4557(3) 0.0462(12) Uani 1 1 d . . . O10 O 1.1176(4) 0.6426(2) 0.4634(3) 0.0362(11) Uani 1 1 d . . . C1 C 0.8873(8) 0.8155(4) 0.0930(5) 0.0454(19) Uani 1 1 d . . . C2 C 1.0099(7) 0.7775(4) 0.1418(4) 0.0356(16) Uani 1 1 d . A . C3 C 1.1287(7) 0.8174(4) 0.1693(5) 0.051(2) Uani 1 1 d . . . H3 H 1.1297 0.8673 0.1596 0.061 Uiso 1 1 calc R A . C4 C 1.2481(8) 0.7828(4) 0.2121(5) 0.054(2) Uani 1 1 d . A . H4 H 1.3300 0.8094 0.2298 0.064 Uiso 1 1 calc R . . C5 C 1.2446(7) 0.7104(4) 0.2278(5) 0.0406(18) Uani 1 1 d . . . C6 C 1.1260(8) 0.6705(4) 0.2026(5) 0.049(2) Uani 1 1 d . A . H6 H 1.1252 0.6209 0.2142 0.059 Uiso 1 1 calc R . . C7 C 1.0074(8) 0.7035(4) 0.1599(5) 0.053(2) Uani 1 1 d . . . H7 H 0.9259 0.6764 0.1432 0.064 Uiso 1 1 calc R A . C8 C 1.4410(7) 0.6286(4) 0.2240(4) 0.0361(16) Uani 1 1 d . . . C9 C 1.4560(8) 0.6389(4) 0.1309(5) 0.053(2) Uani 1 1 d . A . H9 H 1.4073 0.6766 0.0996 0.064 Uiso 1 1 calc R . . C10 C 1.5444(8) 0.5928(4) 0.0827(5) 0.057(2) Uani 1 1 d . . . H10 H 1.5544 0.5996 0.0195 0.069 Uiso 1 1 calc R A . C11 C 1.6159(8) 0.5376(4) 0.1295(5) 0.052(2) Uani 1 1 d . A . H11 H 1.6726 0.5059 0.0978 0.063 Uiso 1 1 calc R . . C12 C 1.6036(6) 0.5292(4) 0.2242(4) 0.0374(16) Uani 1 1 d . . . H12 H 1.6565 0.4933 0.2563 0.045 Uiso 1 1 calc R A . C13 C 1.5130(6) 0.5736(3) 0.2721(4) 0.0260(14) Uani 1 1 d . A . C14 C 1.4934(6) 0.5580(3) 0.3722(4) 0.0256(14) Uani 1 1 d . . . C15 C 0.4837(7) 0.9558(3) 0.1772(4) 0.0330(16) Uani 1 1 d . . . C16 C 0.4594(6) 0.9421(3) 0.2779(4) 0.0287(15) Uani 1 1 d . . . C17 C 0.3315(7) 0.9667(3) 0.3086(4) 0.0399(17) Uani 1 1 d . . . H17 H 0.2674 0.9904 0.2666 0.048 Uiso 1 1 calc R . . C18 C 0.2955(8) 0.9576(4) 0.3985(5) 0.061(2) Uani 1 1 d U . . H18 H 0.2082 0.9741 0.4175 0.073 Uiso 1 1 calc R . . C19 C 0.3924(9) 0.9231(5) 0.4604(6) 0.078(3) Uani 1 1 d U . . H19 H 0.3698 0.9162 0.5217 0.094 Uiso 1 1 calc R . . C20 C 0.5226(8) 0.8988(4) 0.4324(5) 0.062(2) Uani 1 1 d U . . H20 H 0.5875 0.8762 0.4749 0.074 Uiso 1 1 calc R . . C21 C 0.5553(7) 0.9081(3) 0.3417(5) 0.0379(17) Uani 1 1 d . . . C22 C 0.7525(7) 0.8249(3) 0.3504(5) 0.0350(16) Uani 1 1 d . . . C23 C 0.8987(7) 0.8269(3) 0.3612(4) 0.0341(16) Uani 1 1 d . . . H23 H 0.9480 0.8690 0.3474 0.041 Uiso 1 1 calc R . . C24 C 0.9720(6) 0.7660(3) 0.3926(4) 0.0324(16) Uani 1 1 d . . . H24 H 1.0715 0.7672 0.3993 0.039 Uiso 1 1 calc R . . C25 C 0.9022(6) 0.7040(3) 0.4142(4) 0.0285(15) Uani 1 1 d . . . C26 C 0.7542(7) 0.7028(4) 0.4014(6) 0.053(2) Uani 1 1 d . . . H26 H 0.7049 0.6605 0.4139 0.063 Uiso 1 1 calc R . . C27 C 0.6798(7) 0.7626(4) 0.3708(6) 0.056(2) Uani 1 1 d . . . H27 H 0.5804 0.7614 0.3637 0.067 Uiso 1 1 calc R . . C28 C 0.9818(7) 0.6382(3) 0.4459(4) 0.0316(16) Uani 1 1 d . . . O2A O 0.780(2) 0.7683(10) 0.066(3) 0.063(7) Uani 0.58(8) 1 d PU A 1 H2A H 0.7153 0.7903 0.0370 0.095 Uiso 0.58(8) 1 calc PR A 1 O2B O 0.817(5) 0.7710(13) 0.031(3) 0.058(9) Uani 0.42(8) 1 d PU A 2 H2B H 0.7629 0.7950 -0.0040 0.087 Uiso 0.42(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01657(15) 0.02465(17) 0.02214(16) -0.00080(15) -0.00074(11) 0.00057(16) O1 0.032(2) 0.029(3) 0.047(3) 0.005(2) -0.009(2) 0.008(2) O3 0.054(3) 0.054(3) 0.034(3) 0.001(2) -0.004(2) 0.034(3) O4 0.026(2) 0.062(3) 0.028(2) 0.011(2) 0.007(2) 0.006(2) O5 0.027(2) 0.040(3) 0.031(2) 0.010(2) -0.006(2) -0.001(2) O6 0.030(2) 0.048(3) 0.030(2) 0.009(2) 0.009(2) 0.011(2) O7 0.033(2) 0.090(4) 0.036(3) 0.022(3) 0.001(2) 0.021(3) O8 0.038(3) 0.044(3) 0.048(3) 0.024(2) 0.006(2) 0.020(3) O9 0.050(3) 0.027(3) 0.060(3) 0.008(2) -0.008(3) -0.005(3) O10 0.029(2) 0.029(3) 0.049(3) 0.002(2) -0.011(2) 0.007(2) C1 0.040(4) 0.044(5) 0.051(5) 0.000(4) -0.002(4) -0.004(4) C2 0.037(4) 0.032(4) 0.037(4) -0.001(3) -0.008(3) 0.004(4) C3 0.045(4) 0.032(4) 0.074(6) 0.016(4) 0.004(4) 0.011(4) C4 0.038(4) 0.043(5) 0.077(6) 0.009(4) -0.014(4) -0.003(4) C5 0.039(4) 0.044(5) 0.039(4) 0.005(3) 0.001(4) 0.020(4) C6 0.066(5) 0.021(4) 0.059(5) 0.003(4) -0.009(4) 0.018(4) C7 0.051(5) 0.040(5) 0.067(5) -0.006(4) -0.011(4) 0.003(4) C8 0.034(4) 0.046(4) 0.028(4) 0.004(3) -0.005(3) 0.015(4) C9 0.058(5) 0.065(5) 0.037(4) 0.016(4) 0.011(4) 0.027(5) C10 0.066(5) 0.078(6) 0.030(4) 0.024(4) 0.017(4) 0.027(5) C11 0.056(5) 0.061(5) 0.041(4) 0.004(4) 0.016(4) 0.025(4) C12 0.031(3) 0.046(4) 0.035(4) 0.012(3) 0.004(3) 0.018(4) C13 0.024(3) 0.028(3) 0.026(3) 0.001(3) 0.002(3) 0.003(3) C14 0.027(3) 0.023(3) 0.026(3) 0.005(3) -0.003(3) 0.004(3) C15 0.033(4) 0.034(4) 0.033(4) 0.007(3) 0.004(3) 0.006(3) C16 0.033(3) 0.025(3) 0.029(4) 0.008(3) 0.006(3) 0.005(3) C17 0.043(4) 0.040(4) 0.038(4) 0.007(3) 0.010(3) 0.014(4) C18 0.056(4) 0.070(4) 0.059(4) 0.014(3) 0.018(3) 0.012(3) C19 0.080(4) 0.095(5) 0.062(4) 0.019(4) 0.021(4) 0.022(4) C20 0.063(4) 0.074(4) 0.049(4) 0.019(3) 0.003(3) 0.020(4) C21 0.039(4) 0.036(4) 0.040(4) 0.012(3) 0.004(3) 0.011(4) C22 0.031(4) 0.034(4) 0.040(4) 0.009(3) -0.001(3) 0.005(3) C23 0.036(4) 0.029(4) 0.037(4) 0.006(3) -0.003(3) 0.000(3) C24 0.022(3) 0.040(4) 0.035(4) 0.007(3) -0.002(3) 0.008(3) C25 0.029(3) 0.023(3) 0.033(4) 0.006(3) -0.003(3) -0.005(3) C26 0.030(4) 0.034(4) 0.091(6) 0.016(4) -0.016(4) -0.001(4) C27 0.028(4) 0.041(5) 0.097(7) 0.019(4) -0.012(4) 0.001(4) C28 0.045(4) 0.024(4) 0.024(3) 0.004(3) -0.012(3) 0.000(4) O2A 0.051(8) 0.053(7) 0.083(11) -0.002(7) -0.013(7) 0.003(6) O2B 0.063(12) 0.054(9) 0.053(12) 0.002(7) -0.029(8) 0.003(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 O5 2.252(4) 2_755 ? Eu1 O7 2.303(4) 3_675 ? Eu1 O4 2.332(4) 4_575 ? Eu1 O6 2.347(4) . ? Eu1 O9 2.365(4) 2_655 ? Eu1 O10 2.397(4) 4_575 ? Eu1 O1 2.485(4) . ? Eu1 O9 2.958(4) 4_575 ? Eu1 C28 3.085(6) 4_575 ? Eu1 Eu1 4.1018(6) 3_675 ? O1 C1 1.211(7) . ? O3 C8 1.381(7) . ? O3 C5 1.389(7) . ? O4 C14 1.238(6) . ? O4 Eu1 2.332(4) 4_676 ? O5 C14 1.277(6) . ? O5 Eu1 2.252(4) 2_745 ? O6 C15 1.250(7) . ? O7 C15 1.250(7) . ? O7 Eu1 2.303(4) 3_675 ? O8 C21 1.379(7) . ? O8 C22 1.386(7) . ? O9 C28 1.260(7) . ? O9 Eu1 2.365(4) 2_645 ? O9 Eu1 2.958(4) 4_676 ? O10 C28 1.282(7) . ? O10 Eu1 2.397(4) 4_676 ? C1 O2B 1.35(2) . ? C1 O2A 1.365(17) . ? C1 C2 1.480(9) . ? C2 C3 1.369(9) . ? C2 C7 1.388(9) . ? C3 C4 1.393(9) . ? C3 H3 0.9300 . ? C4 C5 1.354(9) . ? C4 H4 0.9300 . ? C5 C6 1.360(9) . ? C6 C7 1.374(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.371(8) . ? C8 C13 1.377(8) . ? C9 C10 1.401(9) . ? C9 H9 0.9300 . ? C10 C11 1.369(9) . ? C10 H10 0.9300 . ? C11 C12 1.384(9) . ? C11 H11 0.9300 . ? C12 C13 1.394(8) . ? C12 H12 0.9300 . ? C13 C14 1.493(8) . ? C15 C16 1.504(8) . ? C16 C17 1.381(8) . ? C16 C21 1.390(8) . ? C17 C18 1.370(9) . ? C17 H17 0.9300 . ? C18 C19 1.382(10) . ? C18 H18 0.9300 . ? C19 C20 1.383(10) . ? C19 H19 0.9300 . ? C20 C21 1.371(9) . ? C20 H20 0.9300 . ? C22 C23 1.367(8) . ? C22 C27 1.376(8) . ? C23 C24 1.376(8) . ? C23 H23 0.9300 . ? C24 C25 1.363(8) . ? C24 H24 0.9300 . ? C25 C26 1.385(8) . ? C25 C28 1.478(8) . ? C26 C27 1.361(9) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 Eu1 3.085(6) 4_676 ? O2A H2A 0.8200 . ? O2B H2B 0.8200 . ? 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 O5 Eu1 O7 112.62(16) 2_755 3_675 ? O5 Eu1 O4 86.87(14) 2_755 4_575 ? O7 Eu1 O4 73.76(15) 3_675 4_575 ? O5 Eu1 O6 96.67(14) 2_755 . ? O7 Eu1 O6 131.97(14) 3_675 . ? O4 Eu1 O6 147.88(15) 4_575 . ? O5 Eu1 O9 82.29(14) 2_755 2_655 ? O7 Eu1 O9 72.06(16) 3_675 2_655 ? O4 Eu1 O9 136.53(16) 4_575 2_655 ? O6 Eu1 O9 75.42(15) . 2_655 ? O5 Eu1 O10 149.17(14) 2_755 4_575 ? O7 Eu1 O10 89.64(16) 3_675 4_575 ? O4 Eu1 O10 78.98(15) 4_575 4_575 ? O6 Eu1 O10 82.06(15) . 4_575 ? O9 Eu1 O10 126.31(15) 2_655 4_575 ? O5 Eu1 O1 76.32(14) 2_755 . ? O7 Eu1 O1 146.71(15) 3_675 . ? O4 Eu1 O1 74.88(15) 4_575 . ? O6 Eu1 O1 75.02(14) . . ? O9 Eu1 O1 140.87(15) 2_655 . ? O10 Eu1 O1 73.61(14) 4_575 . ? O5 Eu1 O9 161.07(13) 2_755 4_575 ? O7 Eu1 O9 67.30(14) 3_675 4_575 ? O4 Eu1 O9 110.44(13) 4_575 4_575 ? O6 Eu1 O9 72.95(14) . 4_575 ? O9 Eu1 O9 79.80(14) 2_655 4_575 ? O10 Eu1 O9 46.91(13) 4_575 4_575 ? O1 Eu1 O9 114.71(13) . 4_575 ? O5 Eu1 C28 169.38(15) 2_755 4_575 ? O7 Eu1 C28 77.81(17) 3_675 4_575 ? O4 Eu1 C28 94.53(16) 4_575 4_575 ? O6 Eu1 C28 76.61(15) . 4_575 ? O9 Eu1 C28 103.58(16) 2_655 4_575 ? O10 Eu1 C28 22.96(15) 4_575 4_575 ? O1 Eu1 C28 93.86(15) . 4_575 ? O9 Eu1 C28 23.95(13) 4_575 4_575 ? O5 Eu1 Eu1 127.22(10) 2_755 3_675 ? O7 Eu1 Eu1 62.87(10) 3_675 3_675 ? O4 Eu1 Eu1 132.09(10) 4_575 3_675 ? O6 Eu1 Eu1 69.11(10) . 3_675 ? O9 Eu1 Eu1 45.22(11) 2_655 3_675 ? O10 Eu1 Eu1 81.30(10) 4_575 3_675 ? O1 Eu1 Eu1 138.49(10) . 3_675 ? O9 Eu1 Eu1 34.58(8) 4_575 3_675 ? C28 Eu1 Eu1 58.42(12) 4_575 3_675 ? C1 O1 Eu1 140.0(5) . . ? C8 O3 C5 118.5(5) . . ? C14 O4 Eu1 148.4(4) . 4_676 ? C14 O5 Eu1 162.5(4) . 2_745 ? C15 O6 Eu1 134.1(4) . . ? C15 O7 Eu1 147.8(4) . 3_675 ? C21 O8 C22 120.0(5) . . ? C28 O9 Eu1 172.2(4) . 2_645 ? C28 O9 Eu1 83.7(4) . 4_676 ? Eu1 O9 Eu1 100.20(14) 2_645 4_676 ? C28 O10 Eu1 110.2(4) . 4_676 ? O1 C1 O2B 121.4(11) . . ? O1 C1 O2A 122.6(9) . . ? O2B C1 O2A 27.3(12) . . ? O1 C1 C2 125.0(7) . . ? O2B C1 C2 110.8(13) . . ? O2A C1 C2 111.5(9) . . ? C3 C2 C7 119.8(6) . . ? C3 C2 C1 118.2(6) . . ? C7 C2 C1 122.0(6) . . ? C2 C3 C4 119.6(6) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 119.8(7) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.1(6) . . ? C4 C5 O3 119.3(7) . . ? C6 C5 O3 119.6(6) . . ? C5 C6 C7 120.1(6) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 119.9 . . ? C6 C7 C2 119.6(7) . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.2 . . ? C9 C8 C13 120.9(6) . . ? C9 C8 O3 120.5(6) . . ? C13 C8 O3 118.4(5) . . ? C8 C9 C10 120.2(7) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 119.5(6) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 119.8(6) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 121.0(6) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C8 C13 C12 118.5(6) . . ? C8 C13 C14 122.6(5) . . ? C12 C13 C14 118.9(5) . . ? O4 C14 O5 125.0(5) . . ? O4 C14 C13 118.5(5) . . ? O5 C14 C13 116.4(5) . . ? O7 C15 O6 125.2(6) . . ? O7 C15 C16 115.3(5) . . ? O6 C15 C16 119.5(6) . . ? C17 C16 C21 118.2(6) . . ? C17 C16 C15 116.3(6) . . ? C21 C16 C15 125.5(6) . . ? C18 C17 C16 122.3(7) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C17 C18 C19 118.2(7) . . ? C17 C18 H18 120.9 . . ? C19 C18 H18 120.9 . . ? C18 C19 C20 121.0(8) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C21 C20 C19 119.6(7) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 O8 121.1(6) . . ? C20 C21 C16 120.7(6) . . ? O8 C21 C16 118.2(6) . . ? C23 C22 C27 120.2(6) . . ? C23 C22 O8 116.5(6) . . ? C27 C22 O8 123.1(6) . . ? C22 C23 C24 119.3(6) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 121.5(6) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 118.2(6) . . ? C24 C25 C28 121.2(6) . . ? C26 C25 C28 120.5(6) . . ? C27 C26 C25 121.1(7) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C22 119.7(7) . . ? C26 C27 H27 120.2 . . ? C22 C27 H27 120.2 . . ? O9 C28 O10 119.2(6) . . ? O9 C28 C25 122.0(6) . . ? O10 C28 C25 118.8(6) . . ? O9 C28 Eu1 72.4(3) . 4_676 ? O10 C28 Eu1 46.8(3) . 4_676 ? C25 C28 Eu1 165.6(4) . 4_676 ? C1 O2A H2A 109.5 . . ? C1 O2B H2B 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Eu1 O1 C1 -170.3(7) 2_755 . . . ? O7 Eu1 O1 C1 -59.8(8) 3_675 . . . ? O4 Eu1 O1 C1 -79.9(7) 4_575 . . . ? O6 Eu1 O1 C1 88.8(7) . . . . ? O9 Eu1 O1 C1 130.9(7) 2_655 . . . ? O10 Eu1 O1 C1 2.8(7) 4_575 . . . ? O9 Eu1 O1 C1 26.0(8) 4_575 . . . ? C28 Eu1 O1 C1 13.8(7) 4_575 . . . ? Eu1 Eu1 O1 C1 58.1(8) 3_675 . . . ? O5 Eu1 O6 C15 120.1(6) 2_755 . . . ? O7 Eu1 O6 C15 -8.7(7) 3_675 . . . ? O4 Eu1 O6 C15 -145.1(5) 4_575 . . . ? O9 Eu1 O6 C15 39.9(6) 2_655 . . . ? O10 Eu1 O6 C15 -91.0(6) 4_575 . . . ? O1 Eu1 O6 C15 -166.0(6) . . . . ? O9 Eu1 O6 C15 -43.7(6) 4_575 . . . ? C28 Eu1 O6 C15 -68.3(6) 4_575 . . . ? Eu1 Eu1 O6 C15 -7.3(5) 3_675 . . . ? Eu1 O1 C1 O2B 13(3) . . . . ? Eu1 O1 C1 O2A -19(3) . . . . ? Eu1 O1 C1 C2 172.6(4) . . . . ? O1 C1 C2 C3 -13.3(11) . . . . ? O2B C1 C2 C3 148(3) . . . . ? O2A C1 C2 C3 177(2) . . . . ? O1 C1 C2 C7 166.8(7) . . . . ? O2B C1 C2 C7 -32(3) . . . . ? O2A C1 C2 C7 -3(2) . . . . ? C7 C2 C3 C4 2.4(11) . . . . ? C1 C2 C3 C4 -177.4(7) . . . . ? C2 C3 C4 C5 -1.4(11) . . . . ? C3 C4 C5 C6 0.0(11) . . . . ? C3 C4 C5 O3 -177.8(6) . . . . ? C8 O3 C5 C4 -112.6(7) . . . . ? C8 O3 C5 C6 69.6(9) . . . . ? C4 C5 C6 C7 0.4(11) . . . . ? O3 C5 C6 C7 178.1(6) . . . . ? C5 C6 C7 C2 0.7(11) . . . . ? C3 C2 C7 C6 -2.1(11) . . . . ? C1 C2 C7 C6 177.8(7) . . . . ? C5 O3 C8 C9 32.9(10) . . . . ? C5 O3 C8 C13 -152.2(6) . . . . ? C13 C8 C9 C10 0.6(11) . . . . ? O3 C8 C9 C10 175.4(7) . . . . ? C8 C9 C10 C11 -0.2(12) . . . . ? C9 C10 C11 C12 -1.9(12) . . . . ? C10 C11 C12 C13 3.6(11) . . . . ? C9 C8 C13 C12 1.0(10) . . . . ? O3 C8 C13 C12 -173.9(6) . . . . ? C9 C8 C13 C14 -176.5(6) . . . . ? O3 C8 C13 C14 8.6(9) . . . . ? C11 C12 C13 C8 -3.1(10) . . . . ? C11 C12 C13 C14 174.5(6) . . . . ? Eu1 O4 C14 O5 -17.0(12) 4_676 . . . ? Eu1 O4 C14 C13 159.1(5) 4_676 . . . ? Eu1 O5 C14 O4 95.2(13) 2_745 . . . ? Eu1 O5 C14 C13 -81.1(13) 2_745 . . . ? C8 C13 C14 O4 41.2(9) . . . . ? C12 C13 C14 O4 -136.3(6) . . . . ? C8 C13 C14 O5 -142.2(6) . . . . ? C12 C13 C14 O5 40.3(8) . . . . ? Eu1 O7 C15 O6 -12.2(14) 3_675 . . . ? Eu1 O7 C15 C16 168.5(6) 3_675 . . . ? Eu1 O6 C15 O7 12.9(10) . . . . ? Eu1 O6 C15 C16 -167.9(4) . . . . ? O7 C15 C16 C17 -10.8(9) . . . . ? O6 C15 C16 C17 169.9(6) . . . . ? O7 C15 C16 C21 170.3(6) . . . . ? O6 C15 C16 C21 -9.0(10) . . . . ? C21 C16 C17 C18 -1.2(10) . . . . ? C15 C16 C17 C18 179.8(6) . . . . ? C16 C17 C18 C19 0.8(11) . . . . ? C17 C18 C19 C20 0.3(13) . . . . ? C18 C19 C20 C21 -0.8(13) . . . . ? C19 C20 C21 O8 178.3(7) . . . . ? C19 C20 C21 C16 0.4(12) . . . . ? C22 O8 C21 C20 34.0(10) . . . . ? C22 O8 C21 C16 -148.1(6) . . . . ? C17 C16 C21 C20 0.6(10) . . . . ? C15 C16 C21 C20 179.5(7) . . . . ? C17 C16 C21 O8 -177.3(6) . . . . ? C15 C16 C21 O8 1.6(10) . . . . ? C21 O8 C22 C23 -144.8(6) . . . . ? C21 O8 C22 C27 39.9(10) . . . . ? C27 C22 C23 C24 0.0(11) . . . . ? O8 C22 C23 C24 -175.5(5) . . . . ? C22 C23 C24 C25 -0.7(10) . . . . ? C23 C24 C25 C26 1.7(10) . . . . ? C23 C24 C25 C28 178.5(6) . . . . ? C24 C25 C26 C27 -2.0(12) . . . . ? C28 C25 C26 C27 -178.9(7) . . . . ? C25 C26 C27 C22 1.3(12) . . . . ? C23 C22 C27 C26 -0.3(12) . . . . ? O8 C22 C27 C26 174.8(7) . . . . ? Eu1 O9 C28 O10 120(3) 2_645 . . . ? Eu1 O9 C28 O10 -0.4(5) 4_676 . . . ? Eu1 O9 C28 C25 -61(3) 2_645 . . . ? Eu1 O9 C28 C25 179.3(6) 4_676 . . . ? Eu1 O9 C28 Eu1 120(3) 2_645 . . 4_676 ? Eu1 O10 C28 O9 0.5(7) 4_676 . . . ? Eu1 O10 C28 C25 -179.2(4) 4_676 . . . ? C24 C25 C28 O9 -171.5(6) . . . . ? C26 C25 C28 O9 5.2(10) . . . . ? C24 C25 C28 O10 8.2(9) . . . . ? C26 C25 C28 O10 -175.1(6) . . . . ? C24 C25 C28 Eu1 6(2) . . . 4_676 ? C26 C25 C28 Eu1 -177.4(13) . . . 4_676 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.118 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.130 _database_code_depnum_ccdc_archive 'CCDC 916448' ####################################################################### # # 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_exp_1244 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H42 Dy2 O24' _chemical_formula_weight 1423.90 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' Dy Dy -0.1892 4.4098 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7896(8) _cell_length_b 11.5519(8) _cell_length_c 12.6529(19) _cell_angle_alpha 74.677(9) _cell_angle_beta 72.626(10) _cell_angle_gamma 72.086(7) _cell_volume 1275.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1551 _cell_measurement_theta_min 2.5194 _cell_measurement_theta_max 28.4872 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 702 _exptl_absorpt_coefficient_mu 2.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8895 _exptl_absorpt_correction_T_max 0.9425 _exptl_absorpt_process_details multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7973 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_sigmaI/netI 0.1141 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4486 _reflns_number_gt 3478 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0094P)^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 4486 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.0898 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _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 C1 C 0.5551(8) -0.0666(7) 0.2480(7) 0.0253(19) Uani 1 1 d . . . C2 C 0.4521(8) -0.0687(7) 0.3603(7) 0.0258(19) Uani 1 1 d . . . C3 C 0.4921(10) -0.1584(7) 0.4490(8) 0.037(2) Uani 1 1 d . . . H3 H 0.5800 -0.2191 0.4358 0.045 Uiso 1 1 calc R . . C4 C 0.4041(11) -0.1606(8) 0.5586(9) 0.055(3) Uani 1 1 d . . . H4 H 0.4344 -0.2211 0.6177 0.065 Uiso 1 1 calc R . . C5 C 0.2748(11) -0.0747(8) 0.5784(9) 0.054(3) Uani 1 1 d . . . H5 H 0.2162 -0.0772 0.6515 0.065 Uiso 1 1 calc R . . C6 C 0.2275(10) 0.0172(8) 0.4925(9) 0.050(3) Uani 1 1 d . . . H6 H 0.1383 0.0760 0.5076 0.060 Uiso 1 1 calc R . . C7 C 0.3150(9) 0.0206(7) 0.3831(8) 0.036(2) Uani 1 1 d . . . C8 C 0.1758(8) 0.2172(7) 0.3030(8) 0.034(2) Uani 1 1 d . . . C9 C 0.2017(9) 0.2995(8) 0.3510(9) 0.050(3) Uani 1 1 d . . . H9 H 0.2819 0.2763 0.3836 0.060 Uiso 1 1 calc R . . C10 C 0.1099(9) 0.4152(8) 0.3508(9) 0.047(3) Uani 1 1 d . . . H10 H 0.1280 0.4704 0.3837 0.057 Uiso 1 1 calc R . . C11 C -0.0091(8) 0.4515(7) 0.3027(8) 0.032(2) Uani 1 1 d . . . C12 C -0.0356(9) 0.3674(7) 0.2572(8) 0.037(2) Uani 1 1 d . . . H12 H -0.1175 0.3896 0.2266 0.045 Uiso 1 1 calc R . . C13 C 0.0565(9) 0.2516(7) 0.2560(8) 0.039(2) Uani 1 1 d . . . H13 H 0.0384 0.1961 0.2234 0.046 Uiso 1 1 calc R . . C14 C -0.1056(9) 0.5795(8) 0.3027(8) 0.040(2) Uani 1 1 d . . . C15 C 0.7313(9) 0.1300(7) -0.1433(8) 0.028(2) Uani 1 1 d . . . C16 C 0.7101(8) 0.2320(6) -0.2439(7) 0.0243(19) Uani 1 1 d . . . C17 C 0.5969(8) 0.3400(6) -0.2373(7) 0.0252(19) Uani 1 1 d . . . C18 C 0.5760(9) 0.4283(7) -0.3340(8) 0.037(2) Uani 1 1 d . . . H18 H 0.4989 0.4994 -0.3292 0.045 Uiso 1 1 calc R . . C19 C 0.6703(10) 0.4096(8) -0.4365(8) 0.042(2) Uani 1 1 d . . . H19 H 0.6564 0.4683 -0.5012 0.051 Uiso 1 1 calc R . . C20 C 0.7857(9) 0.3043(8) -0.4443(8) 0.044(2) Uani 1 1 d . . . H20 H 0.8506 0.2923 -0.5134 0.053 Uiso 1 1 calc R . . C21 C 0.8020(8) 0.2176(7) -0.3474(8) 0.029(2) Uani 1 1 d . . . H21 H 0.8788 0.1464 -0.3526 0.035 Uiso 1 1 calc R . . C22 C 0.4068(8) 0.4620(6) -0.1060(7) 0.031(2) Uani 1 1 d . . . C23 C 0.2687(9) 0.4512(7) -0.0381(8) 0.037(2) Uani 1 1 d . . . H23 H 0.2463 0.3744 -0.0142 0.044 Uiso 1 1 calc R . . C24 C 0.9234(9) 0.2181(7) 0.0154(7) 0.0251(19) Uani 1 1 d . . . C25 C 0.8009(8) 0.3295(6) 0.0435(7) 0.025(2) Uani 1 1 d . . . C26 C 0.8343(8) 0.4443(6) 0.0067(7) 0.031(2) Uani 1 1 d . . . H26 H 0.9266 0.4506 -0.0393 0.037 Uiso 1 1 calc R . . C27 C 0.6600(8) 0.3229(7) 0.1052(7) 0.033(2) Uani 1 1 d . . . H27 H 0.6349 0.2473 0.1252 0.040 Uiso 1 1 calc R . . C28 C 0.5559(9) 0.4266(7) 0.1377(8) 0.040(2) Uani 1 1 d . . . H28 H 0.4619 0.4210 0.1805 0.048 Uiso 1 1 calc R . . O1 O 0.6560(5) -0.1361(4) -0.0260(5) 0.0298(14) Uani 1 1 d . . . H1A H 0.6704 -0.1096 -0.0968 0.036 Uiso 1 1 d R . . H1B H 0.5638 -0.1159 0.0030 0.036 Uiso 1 1 d R . . O2 O 0.8867(5) -0.0934(4) 0.2136(5) 0.0319(14) Uani 1 1 d . . . H2A H 0.8830 -0.1673 0.2481 0.048 Uiso 1 1 d R . . H2B H 0.9769 -0.0889 0.1923 0.048 Uiso 1 1 d R . . O3 O 0.5632(6) 0.0367(5) 0.1817(5) 0.0384(15) Uani 1 1 d . . . O4 O 0.6404(5) -0.1644(4) 0.2165(5) 0.0276(14) Uani 1 1 d . . . O5 O 0.8476(5) 0.0419(4) -0.1543(5) 0.0261(13) Uani 1 1 d . . . O6 O 0.6373(5) 0.1300(4) -0.0514(5) 0.0319(14) Uani 1 1 d . . . O7 O 0.8960(6) 0.1124(4) 0.0395(5) 0.0360(15) Uani 1 1 d . . . O8 O -0.2294(6) 0.5971(5) 0.2712(6) 0.0466(18) Uani 1 1 d . . . H8 H -0.2747 0.6701 0.2675 0.070 Uiso 1 1 calc R . . O9 O -0.0761(7) 0.6609(5) 0.3288(6) 0.063(2) Uani 1 1 d . . . O10 O 0.5020(6) 0.3506(4) -0.1334(5) 0.0444(17) Uani 1 1 d . . . O11 O 0.2714(6) 0.1012(6) 0.2910(6) 0.0530(18) Uani 1 1 d . . . O12 O 0.9492(6) -0.2324(4) 0.0272(6) 0.0406(17) Uani 1 1 d . . . Dy1 Dy 0.78435(4) -0.04220(3) 0.05158(4) 0.02625(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(5) 0.027(4) 0.019(5) 0.002(4) -0.005(4) -0.006(4) C2 0.026(4) 0.029(4) 0.021(5) 0.002(4) -0.005(4) -0.009(4) C3 0.048(6) 0.036(5) 0.022(6) -0.003(4) -0.005(5) -0.006(4) C4 0.067(7) 0.040(6) 0.042(8) 0.004(5) -0.016(6) 0.000(5) C5 0.067(7) 0.047(6) 0.037(8) -0.017(6) 0.003(6) -0.006(5) C6 0.039(6) 0.047(6) 0.047(8) -0.023(6) 0.009(5) 0.006(5) C7 0.034(5) 0.033(5) 0.039(7) -0.012(5) -0.008(5) -0.004(4) C8 0.023(5) 0.028(5) 0.030(6) -0.008(4) 0.010(4) 0.008(4) C9 0.022(5) 0.063(6) 0.064(9) -0.014(6) -0.014(5) -0.003(5) C10 0.036(5) 0.046(6) 0.065(8) -0.010(5) -0.021(5) -0.009(5) C11 0.033(5) 0.024(4) 0.032(6) 0.005(4) -0.010(4) -0.004(4) C12 0.035(5) 0.031(5) 0.039(7) -0.005(4) -0.013(5) 0.004(4) C13 0.035(5) 0.041(5) 0.030(6) -0.008(5) -0.007(5) 0.005(4) C14 0.037(6) 0.038(5) 0.043(7) 0.004(5) -0.013(5) -0.012(4) C15 0.031(5) 0.021(4) 0.032(6) -0.010(4) -0.003(4) -0.006(4) C16 0.021(4) 0.026(4) 0.027(6) -0.012(4) -0.008(4) -0.001(3) C17 0.016(4) 0.026(4) 0.022(5) -0.001(4) 0.002(4) 0.000(3) C18 0.034(5) 0.028(5) 0.035(7) 0.004(4) -0.005(5) 0.001(4) C19 0.053(6) 0.042(5) 0.029(6) 0.011(5) -0.015(5) -0.018(5) C20 0.033(5) 0.060(6) 0.031(7) -0.019(5) 0.010(5) -0.009(5) C21 0.016(4) 0.029(4) 0.035(6) -0.009(4) -0.002(4) 0.002(3) C22 0.030(5) 0.020(4) 0.026(6) -0.006(4) -0.004(4) 0.015(4) C23 0.041(5) 0.019(4) 0.039(7) -0.001(4) -0.001(5) -0.002(4) C24 0.033(5) 0.024(4) 0.022(5) -0.014(4) -0.016(4) 0.006(4) C25 0.020(4) 0.017(4) 0.036(6) -0.012(4) -0.007(4) 0.003(3) C26 0.028(5) 0.027(4) 0.030(6) -0.009(4) 0.003(4) -0.004(4) C27 0.036(5) 0.027(4) 0.036(6) -0.007(4) -0.003(4) -0.011(4) C28 0.029(5) 0.030(5) 0.053(7) -0.016(5) 0.010(5) -0.009(4) O1 0.019(3) 0.036(3) 0.031(4) -0.006(3) -0.003(3) -0.005(2) O2 0.026(3) 0.031(3) 0.038(4) 0.000(3) -0.008(3) -0.011(2) O3 0.035(3) 0.031(3) 0.029(4) -0.003(3) 0.008(3) 0.004(3) O4 0.019(3) 0.023(3) 0.035(4) -0.009(3) 0.000(3) 0.001(2) O5 0.019(3) 0.019(3) 0.030(4) -0.003(3) 0.000(3) 0.003(2) O6 0.027(3) 0.026(3) 0.027(4) 0.003(3) 0.003(3) -0.001(2) O7 0.050(4) 0.012(3) 0.045(5) -0.004(3) -0.020(3) 0.001(2) O8 0.044(4) 0.029(3) 0.062(5) -0.008(3) -0.015(4) 0.001(3) O9 0.088(5) 0.029(3) 0.092(7) -0.005(4) -0.060(5) -0.009(3) O10 0.045(4) 0.023(3) 0.029(4) 0.001(3) 0.012(3) 0.017(3) O11 0.042(4) 0.064(4) 0.030(5) -0.013(4) -0.005(3) 0.020(3) O12 0.022(3) 0.033(3) 0.064(5) -0.018(3) -0.008(3) 0.003(3) Dy1 0.0232(2) 0.0188(2) 0.0309(3) -0.00431(17) -0.00384(17) 0.00024(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O4 1.262(8) . ? C1 O3 1.274(9) . ? C1 C2 1.476(11) . ? C1 Dy1 2.825(8) . ? C2 C3 1.373(11) . ? C2 C7 1.422(10) . ? C3 C4 1.395(12) . ? C3 H3 0.9300 . ? C4 C5 1.349(11) . ? C4 H4 0.9300 . ? C5 C6 1.382(13) . ? C5 H5 0.9300 . ? C6 C7 1.391(12) . ? C6 H6 0.9300 . ? C7 O11 1.373(10) . ? C8 C9 1.372(11) . ? C8 C13 1.371(11) . ? C8 O11 1.395(8) . ? C9 C10 1.362(10) . ? C9 H9 0.9300 . ? C10 C11 1.375(11) . ? C10 H10 0.9300 . ? C11 C12 1.373(10) . ? C11 C14 1.490(10) . ? C12 C13 1.365(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O9 1.210(9) . ? C14 O8 1.327(9) . ? C15 O6 1.249(9) . ? C15 O5 1.272(8) . ? C15 C16 1.506(11) . ? C15 Dy1 2.801(9) . ? C16 C21 1.367(11) . ? C16 C17 1.393(9) . ? C17 O10 1.376(9) . ? C17 C18 1.392(11) . ? C18 C19 1.375(11) . ? C18 H18 0.9300 . ? C19 C20 1.385(11) . ? C19 H19 0.9300 . ? C20 C21 1.380(12) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C28 1.371(10) 2_665 ? C22 C23 1.391(10) . ? C22 O10 1.397(7) . ? C23 C26 1.378(9) 2_665 ? C23 H23 0.9300 . ? C24 O12 1.246(9) 2_755 ? C24 O7 1.270(8) . ? C24 C25 1.502(9) . ? C24 Dy1 2.987(7) 2_755 ? C25 C27 1.382(10) . ? C25 C26 1.390(9) . ? C26 C23 1.378(9) 2_665 ? C26 H26 0.9300 . ? C27 C28 1.379(9) . ? C27 H27 0.9300 . ? C28 C22 1.371(10) 2_665 ? C28 H28 0.9300 . ? O1 Dy1 2.420(4) . ? O1 H1A 0.8500 . ? O1 H1B 0.8500 . ? O2 Dy1 2.403(5) . ? O2 H2A 0.8568 . ? O2 H2B 0.8568 . ? O3 Dy1 2.383(5) . ? O4 Dy1 2.499(5) . ? O5 Dy1 2.486(6) . ? O6 Dy1 2.391(5) . ? O7 Dy1 2.316(5) . ? O8 H8 0.8200 . ? O12 C24 1.246(9) 2_755 ? O12 Dy1 2.326(5) . ? Dy1 C24 2.987(7) 2_755 ? 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 C1 O3 118.3(7) . . ? O4 C1 C2 121.9(7) . . ? O3 C1 C2 119.7(7) . . ? O4 C1 Dy1 62.2(4) . . ? O3 C1 Dy1 57.0(4) . . ? C2 C1 Dy1 168.4(5) . . ? C3 C2 C7 117.7(8) . . ? C3 C2 C1 118.8(7) . . ? C7 C2 C1 123.5(8) . . ? C2 C3 C4 121.5(8) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 119.7(10) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.5(10) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C7 119.1(8) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? O11 C7 C6 123.3(8) . . ? O11 C7 C2 116.1(8) . . ? C6 C7 C2 120.3(9) . . ? C9 C8 C13 119.8(7) . . ? C9 C8 O11 123.4(8) . . ? C13 C8 O11 116.7(8) . . ? C10 C9 C8 120.0(8) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.9(8) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 118.5(7) . . ? C12 C11 C14 122.2(8) . . ? C10 C11 C14 119.3(8) . . ? C13 C12 C11 121.0(8) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C8 119.8(8) . . ? C12 C13 H13 120.1 . . ? C8 C13 H13 120.1 . . ? O9 C14 O8 122.3(8) . . ? O9 C14 C11 124.1(8) . . ? O8 C14 C11 113.6(7) . . ? O6 C15 O5 120.3(8) . . ? O6 C15 C16 121.5(7) . . ? O5 C15 C16 118.2(7) . . ? O6 C15 Dy1 58.2(4) . . ? O5 C15 Dy1 62.6(4) . . ? C16 C15 Dy1 173.4(5) . . ? C21 C16 C17 117.9(8) . . ? C21 C16 C15 119.3(7) . . ? C17 C16 C15 122.8(7) . . ? O10 C17 C18 122.1(7) . . ? O10 C17 C16 117.0(7) . . ? C18 C17 C16 120.7(8) . . ? C19 C18 C17 119.5(8) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 120.7(9) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 118.4(9) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? C16 C21 C20 122.8(7) . . ? C16 C21 H21 118.6 . . ? C20 C21 H21 118.6 . . ? C28 C22 C23 121.2(6) 2_665 . ? C28 C22 O10 124.5(7) 2_665 . ? C23 C22 O10 114.3(7) . . ? C26 C23 C22 119.1(7) 2_665 . ? C26 C23 H23 120.5 2_665 . ? C22 C23 H23 120.5 . . ? O12 C24 O7 122.0(7) 2_755 . ? O12 C24 C25 118.2(7) 2_755 . ? O7 C24 C25 119.7(7) . . ? O12 C24 Dy1 47.1(3) 2_755 2_755 ? O7 C24 Dy1 74.9(4) . 2_755 ? C25 C24 Dy1 165.1(5) . 2_755 ? C27 C25 C26 119.1(6) . . ? C27 C25 C24 123.6(7) . . ? C26 C25 C24 117.3(7) . . ? C23 C26 C25 120.3(7) 2_665 . ? C23 C26 H26 119.8 2_665 . ? C25 C26 H26 119.8 . . ? C25 C27 C28 121.1(7) . . ? C25 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C22 C28 C27 118.9(7) 2_665 . ? C22 C28 H28 120.5 2_665 . ? C27 C28 H28 120.5 . . ? Dy1 O1 H1A 109.2 . . ? Dy1 O1 H1B 109.8 . . ? H1A O1 H1B 108.4 . . ? Dy1 O2 H2A 109.4 . . ? Dy1 O2 H2B 109.6 . . ? H2A O2 H2B 109.2 . . ? C1 O3 Dy1 96.4(4) . . ? C1 O4 Dy1 91.3(4) . . ? C15 O5 Dy1 90.4(5) . . ? C15 O6 Dy1 95.4(5) . . ? C24 O7 Dy1 160.6(5) . . ? C14 O8 H8 109.5 . . ? C17 O10 C22 123.9(6) . . ? C7 O11 C8 120.0(7) . . ? C24 O12 Dy1 109.8(4) 2_755 . ? O7 Dy1 O12 114.08(18) . . ? O7 Dy1 O3 95.17(18) . . ? O12 Dy1 O3 138.1(2) . . ? O7 Dy1 O6 79.57(17) . . ? O12 Dy1 O6 139.6(2) . . ? O3 Dy1 O6 72.20(19) . . ? O7 Dy1 O2 72.32(18) . . ? O12 Dy1 O2 79.02(19) . . ? O3 Dy1 O2 82.52(19) . . ? O6 Dy1 O2 140.04(16) . . ? O7 Dy1 O1 150.90(19) . . ? O12 Dy1 O1 76.94(17) . . ? O3 Dy1 O1 92.04(18) . . ? O6 Dy1 O1 75.89(16) . . ? O2 Dy1 O1 136.69(17) . . ? O7 Dy1 O5 76.62(18) . . ? O12 Dy1 O5 91.46(19) . . ? O3 Dy1 O5 125.42(18) . . ? O6 Dy1 O5 53.22(16) . . ? O2 Dy1 O5 139.93(16) . . ? O1 Dy1 O5 76.24(17) . . ? O7 Dy1 O4 131.63(19) . . ? O12 Dy1 O4 85.31(18) . . ? O3 Dy1 O4 52.91(16) . . ? O6 Dy1 O4 114.75(16) . . ? O2 Dy1 O4 68.61(17) . . ? O1 Dy1 O4 73.97(17) . . ? O5 Dy1 O4 149.99(16) . . ? O7 Dy1 C15 74.6(2) . . ? O12 Dy1 C15 117.2(2) . . ? O3 Dy1 C15 98.5(2) . . ? O6 Dy1 C15 26.35(18) . . ? O2 Dy1 C15 146.85(18) . . ? O1 Dy1 C15 76.46(19) . . ? O5 Dy1 C15 27.02(17) . . ? O4 Dy1 C15 137.1(2) . . ? O7 Dy1 C1 113.1(2) . . ? O12 Dy1 C1 111.5(2) . . ? O3 Dy1 C1 26.62(18) . . ? O6 Dy1 C1 95.2(2) . . ? O2 Dy1 C1 71.4(2) . . ? O1 Dy1 C1 84.7(2) . . ? O5 Dy1 C1 146.03(19) . . ? O4 Dy1 C1 26.53(16) . . ? C15 Dy1 C1 121.2(2) . . ? O7 Dy1 C24 91.7(2) . 2_755 ? O12 Dy1 C24 23.11(19) . 2_755 ? O3 Dy1 C24 154.4(2) . 2_755 ? O6 Dy1 C24 133.3(2) . 2_755 ? O2 Dy1 C24 76.20(19) . 2_755 ? O1 Dy1 C24 93.78(17) . 2_755 ? O5 Dy1 C24 80.13(19) . 2_755 ? O4 Dy1 C24 105.2(2) . 2_755 ? C15 Dy1 C24 107.1(2) . 2_755 ? C1 Dy1 C24 129.6(2) . 2_755 ? 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 O4 C1 C2 C3 31.8(11) . . . . ? O3 C1 C2 C3 -145.6(8) . . . . ? Dy1 C1 C2 C3 -75(3) . . . . ? O4 C1 C2 C7 -150.8(7) . . . . ? O3 C1 C2 C7 31.7(11) . . . . ? Dy1 C1 C2 C7 102(3) . . . . ? C7 C2 C3 C4 -1.7(12) . . . . ? C1 C2 C3 C4 175.8(8) . . . . ? C2 C3 C4 C5 1.4(14) . . . . ? C3 C4 C5 C6 -0.7(14) . . . . ? C4 C5 C6 C7 0.3(14) . . . . ? C5 C6 C7 O11 174.0(8) . . . . ? C5 C6 C7 C2 -0.6(13) . . . . ? C3 C2 C7 O11 -173.7(7) . . . . ? C1 C2 C7 O11 8.9(11) . . . . ? C3 C2 C7 C6 1.3(11) . . . . ? C1 C2 C7 C6 -176.1(7) . . . . ? C13 C8 C9 C10 -0.6(14) . . . . ? O11 C8 C9 C10 174.3(9) . . . . ? C8 C9 C10 C11 -0.2(15) . . . . ? C9 C10 C11 C12 1.6(15) . . . . ? C9 C10 C11 C14 -179.1(9) . . . . ? C10 C11 C12 C13 -2.2(14) . . . . ? C14 C11 C12 C13 178.5(8) . . . . ? C11 C12 C13 C8 1.4(14) . . . . ? C9 C8 C13 C12 0.0(14) . . . . ? O11 C8 C13 C12 -175.2(8) . . . . ? C12 C11 C14 O9 -170.3(9) . . . . ? C10 C11 C14 O9 10.4(15) . . . . ? C12 C11 C14 O8 9.9(13) . . . . ? C10 C11 C14 O8 -169.5(9) . . . . ? O6 C15 C16 C21 -168.7(7) . . . . ? O5 C15 C16 C21 10.5(10) . . . . ? Dy1 C15 C16 C21 106(5) . . . . ? O6 C15 C16 C17 9.2(11) . . . . ? O5 C15 C16 C17 -171.6(7) . . . . ? Dy1 C15 C16 C17 -76(5) . . . . ? C21 C16 C17 O10 177.5(7) . . . . ? C15 C16 C17 O10 -0.4(11) . . . . ? C21 C16 C17 C18 2.0(11) . . . . ? C15 C16 C17 C18 -176.0(7) . . . . ? O10 C17 C18 C19 -176.7(7) . . . . ? C16 C17 C18 C19 -1.4(12) . . . . ? C17 C18 C19 C20 -0.2(13) . . . . ? C18 C19 C20 C21 1.2(12) . . . . ? C17 C16 C21 C20 -0.9(11) . . . . ? C15 C16 C21 C20 177.1(7) . . . . ? C19 C20 C21 C16 -0.6(12) . . . . ? C28 C22 C23 C26 3.0(14) 2_665 . . 2_665 ? O10 C22 C23 C26 -179.5(8) . . . 2_665 ? O12 C24 C25 C27 -170.4(8) 2_755 . . . ? O7 C24 C25 C27 6.9(12) . . . . ? Dy1 C24 C25 C27 -161.9(18) 2_755 . . . ? O12 C24 C25 C26 8.1(12) 2_755 . . . ? O7 C24 C25 C26 -174.6(7) . . . . ? Dy1 C24 C25 C26 17(3) 2_755 . . . ? C27 C25 C26 C23 4.4(13) . . . 2_665 ? C24 C25 C26 C23 -174.1(8) . . . 2_665 ? C26 C25 C27 C28 -4.8(13) . . . . ? C24 C25 C27 C28 173.7(8) . . . . ? C25 C27 C28 C22 1.2(14) . . . 2_665 ? O4 C1 O3 Dy1 -10.6(8) . . . . ? C2 C1 O3 Dy1 167.0(6) . . . . ? O3 C1 O4 Dy1 10.0(7) . . . . ? C2 C1 O4 Dy1 -167.5(7) . . . . ? O6 C15 O5 Dy1 -8.2(7) . . . . ? C16 C15 O5 Dy1 172.6(6) . . . . ? O5 C15 O6 Dy1 8.5(7) . . . . ? C16 C15 O6 Dy1 -172.3(6) . . . . ? O12 C24 O7 Dy1 -132.1(13) 2_755 . . . ? C25 C24 O7 Dy1 51(2) . . . . ? Dy1 C24 O7 Dy1 -132.3(16) 2_755 . . . ? C18 C17 O10 C22 -20.5(12) . . . . ? C16 C17 O10 C22 164.0(7) . . . . ? C28 C22 O10 C17 -41.2(13) 2_665 . . . ? C23 C22 O10 C17 141.4(8) . . . . ? C6 C7 O11 C8 30.2(12) . . . . ? C2 C7 O11 C8 -155.0(7) . . . . ? C9 C8 O11 C7 53.5(12) . . . . ? C13 C8 O11 C7 -131.5(9) . . . . ? C24 O7 Dy1 O12 140.5(16) . . . . ? C24 O7 Dy1 O3 -70.3(16) . . . . ? C24 O7 Dy1 O6 0.5(16) . . . . ? C24 O7 Dy1 O2 -150.7(16) . . . . ? C24 O7 Dy1 O1 33.4(18) . . . . ? C24 O7 Dy1 O5 54.9(16) . . . . ? C24 O7 Dy1 O4 -113.4(16) . . . . ? C24 O7 Dy1 C15 27.1(16) . . . . ? C24 O7 Dy1 C1 -90.7(16) . . . . ? C24 O7 Dy1 C24 134.4(15) . . . 2_755 ? C24 O12 Dy1 O7 -15.7(6) 2_755 . . . ? C24 O12 Dy1 O3 -146.0(5) 2_755 . . . ? C24 O12 Dy1 O6 86.9(6) 2_755 . . . ? C24 O12 Dy1 O2 -80.5(5) 2_755 . . . ? C24 O12 Dy1 O1 135.8(6) 2_755 . . . ? C24 O12 Dy1 O5 60.2(5) 2_755 . . . ? C24 O12 Dy1 O4 -149.6(6) 2_755 . . . ? C24 O12 Dy1 C15 68.7(6) 2_755 . . . ? C24 O12 Dy1 C1 -145.4(5) 2_755 . . . ? C1 O3 Dy1 O7 -134.3(5) . . . . ? C1 O3 Dy1 O12 1.3(6) . . . . ? C1 O3 Dy1 O6 148.4(5) . . . . ? C1 O3 Dy1 O2 -62.9(5) . . . . ? C1 O3 Dy1 O1 73.9(5) . . . . ? C1 O3 Dy1 O5 148.5(4) . . . . ? C1 O3 Dy1 O4 5.9(4) . . . . ? C1 O3 Dy1 C15 150.5(5) . . . . ? C1 O3 Dy1 C24 -29.2(7) . . . 2_755 ? C15 O6 Dy1 O7 76.3(4) . . . . ? C15 O6 Dy1 O12 -38.8(5) . . . . ? C15 O6 Dy1 O3 175.2(5) . . . . ? C15 O6 Dy1 O2 121.8(5) . . . . ? C15 O6 Dy1 O1 -87.9(4) . . . . ? C15 O6 Dy1 O5 -4.7(4) . . . . ? C15 O6 Dy1 O4 -152.5(4) . . . . ? C15 O6 Dy1 C1 -171.1(4) . . . . ? C15 O6 Dy1 C24 -6.2(5) . . . 2_755 ? C15 O5 Dy1 O7 -82.3(4) . . . . ? C15 O5 Dy1 O12 163.3(4) . . . . ? C15 O5 Dy1 O3 4.5(5) . . . . ? C15 O5 Dy1 O6 4.6(4) . . . . ? C15 O5 Dy1 O2 -122.1(4) . . . . ? C15 O5 Dy1 O1 87.1(4) . . . . ? C15 O5 Dy1 O4 80.1(5) . . . . ? C15 O5 Dy1 C1 29.3(5) . . . . ? C15 O5 Dy1 C24 -176.5(4) . . . 2_755 ? C1 O4 Dy1 O7 52.7(5) . . . . ? C1 O4 Dy1 O12 171.1(5) . . . . ? C1 O4 Dy1 O3 -5.9(4) . . . . ? C1 O4 Dy1 O6 -45.5(5) . . . . ? C1 O4 Dy1 O2 91.1(4) . . . . ? C1 O4 Dy1 O1 -111.2(5) . . . . ? C1 O4 Dy1 O5 -104.1(5) . . . . ? C1 O4 Dy1 C15 -63.0(5) . . . . ? C1 O4 Dy1 C24 159.2(4) . . . 2_755 ? O6 C15 Dy1 O7 -97.6(4) . . . . ? O5 C15 Dy1 O7 90.7(4) . . . . ? C16 C15 Dy1 O7 -8(5) . . . . ? O6 C15 Dy1 O12 152.8(4) . . . . ? O5 C15 Dy1 O12 -18.9(5) . . . . ? C16 C15 Dy1 O12 -118(5) . . . . ? O6 C15 Dy1 O3 -4.6(5) . . . . ? O5 C15 Dy1 O3 -176.3(4) . . . . ? C16 C15 Dy1 O3 85(5) . . . . ? O5 C15 Dy1 O6 -171.7(7) . . . . ? C16 C15 Dy1 O6 89(5) . . . . ? O6 C15 Dy1 O2 -93.8(5) . . . . ? O5 C15 Dy1 O2 94.5(5) . . . . ? C16 C15 Dy1 O2 -4(5) . . . . ? O6 C15 Dy1 O1 85.5(4) . . . . ? O5 C15 Dy1 O1 -86.2(4) . . . . ? C16 C15 Dy1 O1 175(5) . . . . ? O6 C15 Dy1 O5 171.7(7) . . . . ? C16 C15 Dy1 O5 -99(5) . . . . ? O6 C15 Dy1 O4 38.1(5) . . . . ? O5 C15 Dy1 O4 -133.6(4) . . . . ? C16 C15 Dy1 O4 128(5) . . . . ? O6 C15 Dy1 C1 10.3(5) . . . . ? O5 C15 Dy1 C1 -161.3(4) . . . . ? C16 C15 Dy1 C1 100(5) . . . . ? O6 C15 Dy1 C24 175.3(4) . . . 2_755 ? O5 C15 Dy1 C24 3.6(4) . . . 2_755 ? C16 C15 Dy1 C24 -95(5) . . . 2_755 ? O4 C1 Dy1 O7 -139.7(4) . . . . ? O3 C1 Dy1 O7 50.8(5) . . . . ? C2 C1 Dy1 O7 -26(3) . . . . ? O4 C1 Dy1 O12 -9.6(5) . . . . ? O3 C1 Dy1 O12 -179.0(4) . . . . ? C2 C1 Dy1 O12 104(3) . . . . ? O4 C1 Dy1 O3 169.5(8) . . . . ? C2 C1 Dy1 O3 -77(3) . . . . ? O4 C1 Dy1 O6 139.4(4) . . . . ? O3 C1 Dy1 O6 -30.1(5) . . . . ? C2 C1 Dy1 O6 -107(3) . . . . ? O4 C1 Dy1 O2 -79.2(4) . . . . ? O3 C1 Dy1 O2 111.4(5) . . . . ? C2 C1 Dy1 O2 34(3) . . . . ? O4 C1 Dy1 O1 64.2(4) . . . . ? O3 C1 Dy1 O1 -105.3(5) . . . . ? C2 C1 Dy1 O1 178(3) . . . . ? O4 C1 Dy1 O5 119.8(4) . . . . ? O3 C1 Dy1 O5 -49.7(6) . . . . ? C2 C1 Dy1 O5 -127(3) . . . . ? O3 C1 Dy1 O4 -169.5(8) . . . . ? C2 C1 Dy1 O4 114(3) . . . . ? O4 C1 Dy1 C15 134.8(4) . . . . ? O3 C1 Dy1 C15 -34.6(5) . . . . ? C2 C1 Dy1 C15 -112(3) . . . . ? O4 C1 Dy1 C24 -26.4(5) . . . 2_755 ? O3 C1 Dy1 C24 164.1(4) . . . 2_755 ? C2 C1 Dy1 C24 87(3) . . . 2_755 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.328 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.174 _database_code_depnum_ccdc_archive 'CCDC 916102' ####################################################################### # # 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_exp_1334 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H21 O12 Tb' _chemical_formula_weight 708.37 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8077(19) _cell_length_b 11.548(2) _cell_length_c 12.6506(16) _cell_angle_alpha 74.508(13) _cell_angle_beta 72.369(14) _cell_angle_gamma 71.967(17) _cell_volume 1274.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1551 _cell_measurement_theta_min 2.5194 _cell_measurement_theta_max 28.4872 _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 2.844 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9453 _exptl_absorpt_correction_T_max 0.9721 _exptl_absorpt_process_details SADABS _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, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7618 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4501 _reflns_number_gt 3610 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^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 4501 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1020 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 C1 C -0.4205(8) 0.7813(7) 0.9832(7) 0.0306(18) Uani 1 1 d . . . C2 C -0.3323(8) 0.5548(7) 0.9913(7) 0.036(2) Uani 1 1 d . . . H2 H -0.4251 0.5481 1.0362 0.043 Uiso 1 1 calc R . . C3 C -0.2318(8) 0.4520(7) 0.9609(7) 0.038(2) Uani 1 1 d . . . H3 H -0.2552 0.3755 0.9856 0.046 Uiso 1 1 calc R . . C4 C -0.0939(8) 0.4608(7) 0.8930(7) 0.035(2) Uani 1 1 d . . . C5 C -0.0558(8) 0.5739(7) 0.8636(7) 0.039(2) Uani 1 1 d . . . H5 H 0.0393 0.5793 0.8232 0.047 Uiso 1 1 calc R . . C6 C -0.1614(8) 0.6781(7) 0.8954(7) 0.037(2) Uani 1 1 d . . . H6 H -0.1377 0.7544 0.8746 0.045 Uiso 1 1 calc R . . C7 C -0.3011(7) 0.6699(6) 0.9575(6) 0.0265(17) Uani 1 1 d . . . C8 C 0.0975(7) 0.3402(7) 0.7615(6) 0.0304(18) Uani 1 1 d . . . C9 C 0.2105(7) 0.2324(6) 0.7550(6) 0.0254(17) Uani 1 1 d . . . C10 C 0.3040(8) 0.2177(7) 0.6527(7) 0.036(2) Uani 1 1 d . . . H10 H 0.3821 0.1473 0.6478 0.043 Uiso 1 1 calc R . . C11 C 0.2860(9) 0.3043(8) 0.5564(7) 0.046(2) Uani 1 1 d . . . H11 H 0.3500 0.2920 0.4869 0.055 Uiso 1 1 calc R . . C12 C 0.1720(9) 0.4093(8) 0.5641(7) 0.044(2) Uani 1 1 d . . . H12 H 0.1601 0.4688 0.4993 0.053 Uiso 1 1 calc R . . C13 C 0.0744(8) 0.4281(7) 0.6669(7) 0.041(2) Uani 1 1 d . . . H13 H -0.0044 0.4980 0.6716 0.049 Uiso 1 1 calc R . . C14 C 0.2305(8) 0.1314(6) 0.8554(7) 0.0293(18) Uani 1 1 d . . . C15 C -0.0541(7) 1.0646(7) 0.7522(7) 0.0292(18) Uani 1 1 d . . . C16 C 0.0483(8) 1.0684(7) 0.6380(7) 0.035(2) Uani 1 1 d . . . C17 C 0.0092(9) 1.1590(8) 0.5501(7) 0.043(2) Uani 1 1 d . . . H17 H -0.0778 1.2205 0.5641 0.052 Uiso 1 1 calc R . . C18 C 0.0957(10) 1.1615(9) 0.4408(8) 0.052(2) Uani 1 1 d . . . H18 H 0.0659 1.2227 0.3818 0.062 Uiso 1 1 calc R . . C19 C 0.2281(10) 1.0710(9) 0.4203(7) 0.054(3) Uani 1 1 d . . . H19 H 0.2868 1.0703 0.3472 0.065 Uiso 1 1 calc R . . C20 C 0.2711(9) 0.9828(8) 0.5091(8) 0.050(2) Uani 1 1 d . . . H20 H 0.3609 0.9241 0.4963 0.060 Uiso 1 1 calc R . . C21 C 0.1827(8) 0.9807(8) 0.6164(7) 0.038(2) Uani 1 1 d . . . C22 C 0.3246(8) 0.7838(8) 0.6967(7) 0.042(2) Uani 1 1 d . . . C23 C 0.4432(8) 0.7513(7) 0.7444(7) 0.040(2) Uani 1 1 d . . . H23 H 0.4608 0.8070 0.7768 0.048 Uiso 1 1 calc R . . C24 C 0.5366(8) 0.6321(8) 0.7429(7) 0.041(2) Uani 1 1 d . . . H24 H 0.6186 0.6094 0.7732 0.049 Uiso 1 1 calc R . . C25 C 0.5099(8) 0.5475(7) 0.6976(7) 0.037(2) Uani 1 1 d . . . C26 C 0.3890(9) 0.5830(8) 0.6504(8) 0.054(3) Uani 1 1 d . . . H26 H 0.3709 0.5271 0.6184 0.065 Uiso 1 1 calc R . . C27 C 0.2943(10) 0.7012(9) 0.6504(8) 0.055(3) Uani 1 1 d . . . H27 H 0.2125 0.7243 0.6199 0.066 Uiso 1 1 calc R . . C28 C 0.6082(9) 0.4191(8) 0.6970(8) 0.044(2) Uani 1 1 d . . . O1 O -0.1557(5) 1.1354(4) 1.0255(4) 0.0349(13) Uani 1 1 d . . . H1A H -0.2026 1.1425 1.0929 0.052 Uiso 1 1 d R . . H1B H -0.0692 1.0894 1.0253 0.052 Uiso 1 1 d R . . O2 O -0.3872(5) 1.0931(5) 0.7869(4) 0.0332(13) Uani 1 1 d . . . H2A H -0.4795 1.0983 0.8091 0.050 Uiso 1 1 d R . . H2B H -0.3728 1.1624 0.7475 0.050 Uiso 1 1 d R . . O3 O -0.3951(5) 0.8878(5) 0.9598(5) 0.0384(14) Uani 1 1 d . . . O4 O -0.5505(5) 0.7685(5) 1.0265(5) 0.0396(14) Uani 1 1 d . . . O5 O -0.1400(5) 1.1642(4) 0.7819(4) 0.0308(13) Uani 1 1 d . . . O6 O -0.0626(5) 0.9636(5) 0.8189(5) 0.0455(16) Uani 1 1 d . . . O7 O 0.1364(5) 0.1301(5) 0.9479(4) 0.0357(14) Uani 1 1 d . . . O8 O 0.3479(5) 0.0415(4) 0.8470(4) 0.0291(12) Uani 1 1 d . . . O9 O 0.7291(6) 0.4035(5) 0.7286(6) 0.0492(16) Uani 1 1 d . . . H9 H 0.7828 0.3344 0.7212 0.074 Uiso 1 1 calc R . . O10 O 0.5754(7) 0.3391(6) 0.6715(6) 0.069(2) Uani 1 1 d . . . O11 O 0.2294(6) 0.8988(6) 0.7090(5) 0.0551(17) Uani 1 1 d . . . O12 O 0.0021(6) 0.3506(5) 0.8677(5) 0.0519(17) Uani 1 1 d . . . Tb1 Tb -0.28432(4) 1.04228(3) 0.94842(3) 0.02771(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(5) 0.023(4) 0.033(5) -0.012(4) -0.015(4) 0.004(3) C2 0.036(5) 0.032(5) 0.033(5) -0.009(4) 0.000(4) -0.004(4) C3 0.041(5) 0.022(4) 0.040(6) -0.004(4) 0.000(4) -0.004(4) C4 0.037(5) 0.018(4) 0.039(5) -0.005(4) -0.009(4) 0.010(3) C5 0.025(4) 0.041(5) 0.043(6) -0.010(4) -0.001(4) 0.001(4) C6 0.046(5) 0.019(4) 0.047(6) -0.007(4) -0.009(4) -0.010(4) C7 0.026(4) 0.020(4) 0.031(5) -0.004(4) -0.007(3) -0.003(3) C8 0.025(4) 0.034(5) 0.023(5) -0.004(4) 0.002(3) -0.003(3) C9 0.022(4) 0.020(4) 0.030(5) -0.002(3) -0.008(3) 0.000(3) C10 0.036(5) 0.031(5) 0.031(5) -0.003(4) 0.001(4) -0.005(4) C11 0.056(6) 0.050(6) 0.026(5) -0.006(5) -0.002(4) -0.014(5) C12 0.052(6) 0.045(6) 0.028(5) 0.006(4) -0.012(4) -0.009(4) C13 0.038(5) 0.026(4) 0.052(6) -0.002(4) -0.014(4) 0.002(4) C14 0.033(4) 0.014(4) 0.032(5) -0.009(3) -0.001(4) 0.004(3) C15 0.025(4) 0.031(5) 0.028(5) -0.005(4) -0.006(3) -0.004(3) C16 0.035(5) 0.034(5) 0.032(5) -0.002(4) -0.008(4) -0.009(4) C17 0.048(5) 0.040(5) 0.032(5) -0.006(4) -0.006(4) 0.000(4) C18 0.073(7) 0.048(6) 0.031(6) -0.001(5) -0.013(5) -0.017(5) C19 0.068(6) 0.053(6) 0.025(6) -0.013(5) 0.017(4) -0.013(5) C20 0.040(5) 0.047(6) 0.042(6) -0.017(5) 0.010(4) 0.004(4) C21 0.037(5) 0.042(5) 0.030(5) -0.008(4) -0.009(4) 0.000(4) C22 0.033(5) 0.039(5) 0.035(5) 0.001(4) 0.000(4) 0.003(4) C23 0.043(5) 0.033(5) 0.037(5) -0.006(4) -0.010(4) 0.001(4) C24 0.036(5) 0.048(5) 0.033(5) -0.007(4) -0.013(4) 0.002(4) C25 0.039(5) 0.036(5) 0.031(5) 0.001(4) -0.006(4) -0.012(4) C26 0.050(6) 0.040(6) 0.071(8) -0.008(5) -0.020(5) -0.007(5) C27 0.052(6) 0.049(6) 0.070(7) -0.003(5) -0.036(5) -0.008(5) C28 0.047(6) 0.036(5) 0.044(6) 0.002(5) -0.014(4) -0.009(4) O1 0.023(3) 0.027(3) 0.050(4) -0.009(3) -0.005(2) -0.001(2) O2 0.026(3) 0.038(3) 0.034(3) -0.002(3) -0.004(2) -0.013(2) O3 0.046(3) 0.022(3) 0.050(4) -0.008(3) -0.021(3) -0.002(2) O4 0.025(3) 0.031(3) 0.054(4) -0.021(3) -0.004(3) 0.010(2) O5 0.024(3) 0.027(3) 0.035(3) -0.008(3) 0.000(2) -0.001(2) O6 0.052(4) 0.024(3) 0.034(4) 0.002(3) 0.008(3) 0.003(3) O7 0.030(3) 0.031(3) 0.030(3) 0.002(3) -0.001(2) 0.002(2) O8 0.026(3) 0.022(3) 0.034(3) -0.009(2) 0.000(2) -0.003(2) O9 0.043(4) 0.028(3) 0.071(5) -0.009(3) -0.020(3) 0.005(3) O10 0.091(5) 0.034(4) 0.098(6) -0.003(4) -0.057(5) -0.011(4) O11 0.041(3) 0.062(4) 0.039(4) -0.016(3) -0.009(3) 0.023(3) O12 0.062(4) 0.024(3) 0.035(4) 0.001(3) 0.006(3) 0.015(3) Tb1 0.0263(2) 0.0183(2) 0.0332(2) -0.00483(16) -0.00488(15) -0.00048(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O4 1.264(8) . ? C1 O3 1.269(8) . ? C1 C7 1.481(10) . ? C1 Tb1 3.009(7) 2_477 ? C2 C3 1.348(10) . ? C2 C7 1.383(10) . ? C2 H2 0.9300 . ? C3 C4 1.383(10) . ? C3 H3 0.9300 . ? C4 O12 1.379(8) . ? C4 C5 1.393(10) . ? C5 C6 1.385(10) . ? C5 H5 0.9300 . ? C6 C7 1.375(10) . ? C6 H6 0.9300 . ? C8 C13 1.374(10) . ? C8 C9 1.388(9) . ? C8 O12 1.397(9) . ? C9 C10 1.359(10) . ? C9 C14 1.494(9) . ? C10 C11 1.373(10) . ? C10 H10 0.9300 . ? C11 C12 1.374(11) . ? C11 H11 0.9300 . ? C12 C13 1.386(11) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O7 1.251(8) . ? C14 O8 1.289(8) . ? C14 Tb1 2.818(7) 2_567 ? C15 O6 1.254(8) . ? C15 O5 1.271(9) . ? C15 C16 1.487(10) . ? C16 C17 1.366(10) . ? C16 C21 1.393(10) . ? C17 C18 1.384(11) . ? C17 H17 0.9300 . ? C18 C19 1.396(12) . ? C18 H18 0.9300 . ? C19 C20 1.373(11) . ? C19 H19 0.9300 . ? C20 C21 1.371(11) . ? C20 H20 0.9300 . ? C21 O11 1.394(9) . ? C22 C23 1.375(10) . ? C22 O11 1.383(9) . ? C22 C27 1.386(12) . ? C23 C24 1.398(11) . ? C23 H23 0.9300 . ? C24 C25 1.380(11) . ? C24 H24 0.9300 . ? C25 C26 1.388(11) . ? C25 C28 1.498(11) . ? C26 C27 1.394(12) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 O10 1.211(10) . ? C28 O9 1.309(9) . ? O1 Tb1 2.418(5) . ? O1 H1A 0.8499 . ? O1 H1B 0.8500 . ? O2 Tb1 2.404(5) . ? O2 H2A 0.8500 . ? O2 H2B 0.8500 . ? O3 Tb1 2.313(5) . ? O4 Tb1 2.317(5) 2_477 ? O5 Tb1 2.503(5) . ? O6 Tb1 2.377(5) . ? O7 Tb1 2.399(5) 2_567 ? O8 Tb1 2.466(5) 2_567 ? O9 H9 0.8200 . ? Tb1 O4 2.317(5) 2_477 ? Tb1 O7 2.399(5) 2_567 ? Tb1 O8 2.466(5) 2_567 ? Tb1 C14 2.818(7) 2_567 ? Tb1 C1 3.009(7) 2_477 ? 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 C1 O3 120.4(7) . . ? O4 C1 C7 118.1(7) . . ? O3 C1 C7 121.5(7) . . ? O4 C1 Tb1 46.0(3) . 2_477 ? O3 C1 Tb1 74.4(4) . 2_477 ? C7 C1 Tb1 164.0(5) . 2_477 ? C3 C2 C7 121.8(7) . . ? C3 C2 H2 119.1 . . ? C7 C2 H2 119.1 . . ? C2 C3 C4 119.7(7) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? O12 C4 C3 115.6(7) . . ? O12 C4 C5 124.4(7) . . ? C3 C4 C5 119.8(7) . . ? C6 C5 C4 119.1(7) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C7 C6 C5 120.6(7) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C2 118.7(7) . . ? C6 C7 C1 121.8(7) . . ? C2 C7 C1 119.3(6) . . ? C13 C8 C9 121.6(7) . . ? C13 C8 O12 121.5(7) . . ? C9 C8 O12 116.7(6) . . ? C10 C9 C8 118.5(7) . . ? C10 C9 C14 119.1(7) . . ? C8 C9 C14 122.4(7) . . ? C9 C10 C11 121.6(8) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C12 119.1(8) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C11 C12 C13 121.1(8) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C8 C13 C12 118.0(7) . . ? C8 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? O7 C14 O8 118.4(6) . . ? O7 C14 C9 122.4(6) . . ? O8 C14 C9 119.2(7) . . ? O7 C14 Tb1 57.9(4) . 2_567 ? O8 C14 Tb1 61.0(4) . 2_567 ? C9 C14 Tb1 173.4(5) . 2_567 ? O6 C15 O5 118.6(7) . . ? O6 C15 C16 121.2(7) . . ? O5 C15 C16 120.2(7) . . ? C17 C16 C21 118.3(7) . . ? C17 C16 C15 119.5(7) . . ? C21 C16 C15 122.2(7) . . ? C16 C17 C18 121.7(8) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C19 119.2(8) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C20 C19 C18 119.3(8) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C21 C20 C19 120.6(8) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C16 120.8(8) . . ? C20 C21 O11 121.5(7) . . ? C16 C21 O11 117.4(7) . . ? C23 C22 O11 115.6(8) . . ? C23 C22 C27 121.8(8) . . ? O11 C22 C27 122.2(8) . . ? C22 C23 C24 118.3(8) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? C25 C24 C23 121.5(8) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 118.9(8) . . ? C24 C25 C28 121.9(7) . . ? C26 C25 C28 119.3(8) . . ? C25 C26 C27 120.8(9) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C22 C27 C26 118.7(8) . . ? C22 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? O10 C28 O9 124.7(8) . . ? O10 C28 C25 122.3(8) . . ? O9 C28 C25 113.0(8) . . ? Tb1 O1 H1A 109.1 . . ? Tb1 O1 H1B 109.4 . . ? H1A O1 H1B 109.5 . . ? Tb1 O2 H2A 109.3 . . ? Tb1 O2 H2B 109.2 . . ? H2A O2 H2B 109.5 . . ? C1 O3 Tb1 160.1(5) . . ? C1 O4 Tb1 110.9(5) . 2_477 ? C15 O5 Tb1 90.6(4) . . ? C15 O6 Tb1 97.0(4) . . ? C14 O7 Tb1 95.9(4) . 2_567 ? C14 O8 Tb1 91.8(4) . 2_567 ? C28 O9 H9 109.5 . . ? C22 O11 C21 120.3(7) . . ? C4 O12 C8 123.2(6) . . ? O3 Tb1 O4 113.95(17) . 2_477 ? O3 Tb1 O6 95.15(19) . . ? O4 Tb1 O6 138.44(18) 2_477 . ? O3 Tb1 O7 80.01(17) . 2_567 ? O4 Tb1 O7 139.25(19) 2_477 2_567 ? O6 Tb1 O7 71.99(17) . 2_567 ? O3 Tb1 O2 71.77(17) . . ? O4 Tb1 O2 79.08(19) 2_477 . ? O6 Tb1 O2 83.05(18) . . ? O7 Tb1 O2 140.23(18) 2_567 . ? O3 Tb1 O1 151.11(17) . . ? O4 Tb1 O1 77.29(17) 2_477 . ? O6 Tb1 O1 91.51(19) . . ? O7 Tb1 O1 75.41(17) 2_567 . ? O2 Tb1 O1 137.04(16) . . ? O3 Tb1 O8 76.87(18) . 2_567 ? O4 Tb1 O8 91.21(18) 2_477 2_567 ? O6 Tb1 O8 125.25(16) . 2_567 ? O7 Tb1 O8 53.25(16) 2_567 2_567 ? O2 Tb1 O8 139.51(15) . 2_567 ? O1 Tb1 O8 76.36(16) . 2_567 ? O3 Tb1 O5 130.95(19) . . ? O4 Tb1 O5 85.78(17) 2_477 . ? O6 Tb1 O5 52.73(16) . . ? O7 Tb1 O5 114.62(15) 2_567 . ? O2 Tb1 O5 68.68(15) . . ? O1 Tb1 O5 74.24(17) . . ? O8 Tb1 O5 150.39(16) 2_567 . ? O3 Tb1 C14 75.0(2) . 2_567 ? O4 Tb1 C14 117.1(2) 2_477 2_567 ? O6 Tb1 C14 98.11(19) . 2_567 ? O7 Tb1 C14 26.21(17) 2_567 2_567 ? O2 Tb1 C14 146.67(19) . 2_567 ? O1 Tb1 C14 76.28(19) . 2_567 ? O8 Tb1 C14 27.20(17) 2_567 2_567 ? O5 Tb1 C14 137.06(18) . 2_567 ? O3 Tb1 C1 91.61(19) . 2_477 ? O4 Tb1 C1 23.12(18) 2_477 2_477 ? O6 Tb1 C1 154.81(19) . 2_477 ? O7 Tb1 C1 133.16(19) 2_567 2_477 ? O2 Tb1 C1 76.08(19) . 2_477 ? O1 Tb1 C1 94.20(18) . 2_477 ? O8 Tb1 C1 79.93(18) 2_567 2_477 ? O5 Tb1 C1 105.58(18) . 2_477 ? C14 Tb1 C1 107.1(2) 2_567 2_477 ? 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 C7 C2 C3 C4 -0.8(13) . . . . ? C2 C3 C4 O12 179.1(8) . . . . ? C2 C3 C4 C5 4.9(13) . . . . ? O12 C4 C5 C6 -178.9(8) . . . . ? C3 C4 C5 C6 -5.3(12) . . . . ? C4 C5 C6 C7 1.6(13) . . . . ? C5 C6 C7 C2 2.5(12) . . . . ? C5 C6 C7 C1 -173.9(8) . . . . ? C3 C2 C7 C6 -2.9(12) . . . . ? C3 C2 C7 C1 173.6(8) . . . . ? O4 C1 C7 C6 170.1(7) . . . . ? O3 C1 C7 C6 -7.9(12) . . . . ? Tb1 C1 C7 C6 164.5(15) 2_477 . . . ? O4 C1 C7 C2 -6.3(11) . . . . ? O3 C1 C7 C2 175.8(7) . . . . ? Tb1 C1 C7 C2 -12(2) 2_477 . . . ? C13 C8 C9 C10 3.3(11) . . . . ? O12 C8 C9 C10 178.7(7) . . . . ? C13 C8 C9 C14 -175.2(7) . . . . ? O12 C8 C9 C14 0.2(11) . . . . ? C8 C9 C10 C11 -2.2(12) . . . . ? C14 C9 C10 C11 176.3(7) . . . . ? C9 C10 C11 C12 1.1(13) . . . . ? C10 C11 C12 C13 -0.9(13) . . . . ? C9 C8 C13 C12 -3.1(12) . . . . ? O12 C8 C13 C12 -178.3(7) . . . . ? C11 C12 C13 C8 1.9(13) . . . . ? C10 C9 C14 O7 -169.0(7) . . . . ? C8 C9 C14 O7 9.5(12) . . . . ? C10 C9 C14 O8 10.4(11) . . . . ? C8 C9 C14 O8 -171.1(7) . . . . ? C10 C9 C14 Tb1 101(4) . . . 2_567 ? C8 C9 C14 Tb1 -81(4) . . . 2_567 ? O6 C15 C16 C17 146.8(8) . . . . ? O5 C15 C16 C17 -29.9(11) . . . . ? O6 C15 C16 C21 -31.9(11) . . . . ? O5 C15 C16 C21 151.4(8) . . . . ? C21 C16 C17 C18 3.3(13) . . . . ? C15 C16 C17 C18 -175.4(8) . . . . ? C16 C17 C18 C19 -1.7(14) . . . . ? C17 C18 C19 C20 -1.2(14) . . . . ? C18 C19 C20 C21 2.3(14) . . . . ? C19 C20 C21 C16 -0.7(14) . . . . ? C19 C20 C21 O11 -174.6(8) . . . . ? C17 C16 C21 C20 -2.1(12) . . . . ? C15 C16 C21 C20 176.6(8) . . . . ? C17 C16 C21 O11 172.0(7) . . . . ? C15 C16 C21 O11 -9.3(11) . . . . ? O11 C22 C23 C24 174.8(7) . . . . ? C27 C22 C23 C24 1.5(13) . . . . ? C22 C23 C24 C25 -1.6(12) . . . . ? C23 C24 C25 C26 1.3(13) . . . . ? C23 C24 C25 C28 -179.2(8) . . . . ? C24 C25 C26 C27 -1.1(13) . . . . ? C28 C25 C26 C27 179.4(8) . . . . ? C23 C22 C27 C26 -1.3(14) . . . . ? O11 C22 C27 C26 -174.2(8) . . . . ? C25 C26 C27 C22 1.1(14) . . . . ? C24 C25 C28 O10 169.8(8) . . . . ? C26 C25 C28 O10 -10.7(13) . . . . ? C24 C25 C28 O9 -8.9(12) . . . . ? C26 C25 C28 O9 170.6(7) . . . . ? O4 C1 O3 Tb1 133.2(13) . . . . ? C7 C1 O3 Tb1 -49(2) . . . . ? Tb1 C1 O3 Tb1 133.3(15) 2_477 . . . ? O3 C1 O4 Tb1 0.1(9) . . . 2_477 ? C7 C1 O4 Tb1 -177.9(5) . . . 2_477 ? O6 C15 O5 Tb1 -10.0(7) . . . . ? C16 C15 O5 Tb1 166.8(6) . . . . ? O5 C15 O6 Tb1 10.6(8) . . . . ? C16 C15 O6 Tb1 -166.2(6) . . . . ? O8 C14 O7 Tb1 8.4(7) . . . 2_567 ? C9 C14 O7 Tb1 -172.2(6) . . . 2_567 ? O7 C14 O8 Tb1 -8.1(7) . . . 2_567 ? C9 C14 O8 Tb1 172.4(6) . . . 2_567 ? C23 C22 O11 C21 132.6(8) . . . . ? C27 C22 O11 C21 -54.1(11) . . . . ? C20 C21 O11 C22 -31.2(12) . . . . ? C16 C21 O11 C22 154.7(7) . . . . ? C3 C4 O12 C8 140.7(8) . . . . ? C5 C4 O12 C8 -45.4(12) . . . . ? C13 C8 O12 C4 -19.0(12) . . . . ? C9 C8 O12 C4 165.5(7) . . . . ? C1 O3 Tb1 O4 -141.6(15) . . . 2_477 ? C1 O3 Tb1 O6 68.8(16) . . . . ? C1 O3 Tb1 O7 -1.9(16) . . . 2_567 ? C1 O3 Tb1 O2 149.8(16) . . . . ? C1 O3 Tb1 O1 -33.8(17) . . . . ? C1 O3 Tb1 O8 -56.2(16) . . . 2_567 ? C1 O3 Tb1 O5 112.2(16) . . . . ? C1 O3 Tb1 C14 -28.2(16) . . . 2_567 ? C1 O3 Tb1 C1 -135.5(15) . . . 2_477 ? C15 O6 Tb1 O3 133.4(5) . . . . ? C15 O6 Tb1 O4 -2.3(6) . . . 2_477 ? C15 O6 Tb1 O7 -148.8(5) . . . 2_567 ? C15 O6 Tb1 O2 62.5(5) . . . . ? C15 O6 Tb1 O1 -74.7(5) . . . . ? C15 O6 Tb1 O8 -149.0(4) . . . 2_567 ? C15 O6 Tb1 O5 -5.9(4) . . . . ? C15 O6 Tb1 C14 -151.1(5) . . . 2_567 ? C15 O6 Tb1 C1 28.5(8) . . . 2_477 ? C15 O5 Tb1 O3 -53.5(5) . . . . ? C15 O5 Tb1 O4 -171.8(5) . . . 2_477 ? C15 O5 Tb1 O6 5.8(4) . . . . ? C15 O5 Tb1 O7 44.9(5) . . . 2_567 ? C15 O5 Tb1 O2 -91.9(5) . . . . ? C15 O5 Tb1 O1 110.2(4) . . . . ? C15 O5 Tb1 O8 103.2(5) . . . 2_567 ? C15 O5 Tb1 C14 61.9(5) . . . 2_567 ? C15 O5 Tb1 C1 -159.8(4) . . . 2_477 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.031 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.157 _database_code_depnum_ccdc_archive 'CCDC 916103' ####################################################################### # # 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_exp_1346 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H21 Gd O12' _chemical_formula_weight 706.70 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7629(11) _cell_length_b 11.5128(7) _cell_length_c 12.6274(10) _cell_angle_alpha 74.605(6) _cell_angle_beta 72.647(9) _cell_angle_gamma 72.200(8) _cell_volume 1265.90(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1871 _cell_measurement_theta_min 2.4877 _cell_measurement_theta_max 28.3774 _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 698 _exptl_absorpt_coefficient_mu 2.690 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9000 _exptl_absorpt_correction_T_max 0.9482 _exptl_absorpt_process_details SADABS _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, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7743 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0960 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4475 _reflns_number_gt 3601 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0134P)^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 4475 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Gd1 Gd 1.28617(4) -0.04212(3) 0.05086(3) 0.02439(11) Uani 1 1 d . . . O1 O 1.1391(5) -0.1647(4) 0.2176(4) 0.0303(11) Uani 1 1 d . . . O2 O 1.0633(5) 0.0377(4) 0.1814(4) 0.0385(13) Uani 1 1 d . . . O3 O 0.7730(6) 0.1027(4) 0.2904(4) 0.0513(15) Uani 1 1 d . . . O4 O 0.4219(7) 0.6618(4) 0.3293(5) 0.0636(19) Uani 1 1 d . . . O5 O 0.2688(6) 0.5964(4) 0.2723(5) 0.0444(14) Uani 1 1 d . . . H5 H 0.2320 0.6709 0.2546 0.067 Uiso 1 1 calc R . . O6 O 1.4008(6) 0.1131(4) 0.0383(4) 0.0384(13) Uani 1 1 d . . . O7 O 1.5527(5) 0.2368(4) -0.0294(4) 0.0400(13) Uani 1 1 d . . . O8 O 0.9961(6) 0.6473(4) 0.1329(4) 0.0502(16) Uani 1 1 d . . . O9 O 0.8624(5) 0.8675(4) 0.0525(4) 0.0335(12) Uani 1 1 d . . . O10 O 0.6529(5) 0.9571(4) 0.1556(3) 0.0276(11) Uani 1 1 d . . . O11 O 1.3875(5) -0.0921(4) 0.2151(4) 0.0339(12) Uani 1 1 d . . . H11A H 1.4799 -0.0970 0.1936 0.051 Uiso 1 1 d R . . H11C H 1.3729 -0.1615 0.2546 0.051 Uiso 1 1 d R . . O12 O 1.1529(5) -0.1352(3) -0.0253(4) 0.0327(12) Uani 1 1 d . . . H12A H 1.1988 -0.1424 -0.0928 0.049 Uiso 1 1 d R . . H12C H 1.0663 -0.0887 -0.0246 0.049 Uiso 1 1 d R . . C1 C 1.0547(7) -0.0652(6) 0.2476(6) 0.0263(16) Uani 1 1 d . . . C2 C 0.9519(8) -0.0676(5) 0.3600(5) 0.0276(16) Uani 1 1 d . . . C3 C 0.9905(9) -0.1577(6) 0.4498(6) 0.0401(19) Uani 1 1 d . . . H3 H 1.0786 -0.2184 0.4366 0.048 Uiso 1 1 calc R . . C4 C 0.9039(10) -0.1614(7) 0.5580(6) 0.053(2) Uani 1 1 d . . . H4 H 0.9331 -0.2230 0.6171 0.063 Uiso 1 1 calc R . . C5 C 0.7730(10) -0.0719(7) 0.5772(7) 0.060(3) Uani 1 1 d . . . H5A H 0.7145 -0.0725 0.6504 0.072 Uiso 1 1 calc R . . C6 C 0.7270(9) 0.0191(7) 0.4894(7) 0.051(2) Uani 1 1 d . . . H6 H 0.6367 0.0773 0.5027 0.061 Uiso 1 1 calc R . . C7 C 0.8175(8) 0.0215(6) 0.3820(6) 0.0330(17) Uani 1 1 d . . . C8 C 0.6768(8) 0.2183(7) 0.3024(6) 0.042(2) Uani 1 1 d . . . C9 C 0.7028(9) 0.3007(7) 0.3497(7) 0.050(2) Uani 1 1 d . . . H9 H 0.7840 0.2776 0.3815 0.060 Uiso 1 1 calc R . . C10 C 0.6105(8) 0.4169(7) 0.3507(7) 0.044(2) Uani 1 1 d . . . H10 H 0.6287 0.4722 0.3837 0.053 Uiso 1 1 calc R . . C11 C 0.4907(8) 0.4525(6) 0.3030(6) 0.0365(18) Uani 1 1 d . . . C12 C 0.4618(8) 0.3693(6) 0.2570(6) 0.0374(19) Uani 1 1 d . . . H12 H 0.3791 0.3920 0.2269 0.045 Uiso 1 1 calc R . . C13 C 0.5558(8) 0.2517(6) 0.2554(6) 0.0360(19) Uani 1 1 d . . . H13 H 0.5378 0.1958 0.2230 0.043 Uiso 1 1 calc R . . C14 C 0.3906(9) 0.5810(6) 0.3035(6) 0.040(2) Uani 1 1 d . . . C15 C 1.4262(8) 0.2205(6) 0.0134(5) 0.0254(16) Uani 1 1 d . . . C16 C 1.3008(7) 0.3311(5) 0.0419(5) 0.0228(15) Uani 1 1 d . . . C17 C 1.3331(8) 0.4478(5) 0.0057(6) 0.0338(18) Uani 1 1 d . . . H17 H 1.4248 0.4558 -0.0411 0.041 Uiso 1 1 calc R . . C18 C 1.2297(8) 0.5499(6) 0.0393(6) 0.0374(19) Uani 1 1 d . . . H18 H 1.2512 0.6274 0.0168 0.045 Uiso 1 1 calc R . . C19 C 1.0932(8) 0.5372(6) 0.1066(6) 0.0342(19) Uani 1 1 d . . . C20 C 1.0565(8) 0.4240(6) 0.1370(6) 0.0370(18) Uani 1 1 d . . . H20 H 0.9621 0.4173 0.1787 0.044 Uiso 1 1 calc R . . C21 C 1.1638(8) 0.3204(5) 0.1040(6) 0.0334(18) Uani 1 1 d . . . H21 H 1.1415 0.2433 0.1246 0.040 Uiso 1 1 calc R . . C22 C 0.9038(8) 0.6579(5) 0.2375(5) 0.0294(17) Uani 1 1 d . . . C23 C 0.9239(8) 0.5689(6) 0.3343(6) 0.0363(18) Uani 1 1 d . . . H23 H 0.9999 0.4968 0.3299 0.044 Uiso 1 1 calc R . . C24 C 0.8291(8) 0.5895(6) 0.4368(6) 0.0391(19) Uani 1 1 d . . . H24 H 0.8427 0.5310 0.5020 0.047 Uiso 1 1 calc R . . C25 C 0.7152(9) 0.6944(7) 0.4448(6) 0.045(2) Uani 1 1 d . . . H25 H 0.6504 0.7060 0.5142 0.054 Uiso 1 1 calc R . . C26 C 0.6988(8) 0.7812(6) 0.3493(6) 0.0354(18) Uani 1 1 d . . . H26 H 0.6230 0.8532 0.3550 0.042 Uiso 1 1 calc R . . C27 C 0.7901(7) 0.7662(5) 0.2450(5) 0.0217(15) Uani 1 1 d . . . C28 C 0.7682(8) 0.8675(5) 0.1460(6) 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 Gd1 0.02119(19) 0.01666(17) 0.0297(2) -0.00360(13) -0.00274(15) -0.00062(13) O1 0.025(3) 0.025(2) 0.036(3) -0.006(2) -0.001(2) -0.006(2) O2 0.033(3) 0.030(3) 0.033(3) 0.001(2) 0.003(2) 0.003(2) O3 0.039(4) 0.053(3) 0.041(3) -0.015(3) -0.010(3) 0.023(3) O4 0.091(5) 0.026(3) 0.089(5) -0.007(3) -0.049(4) -0.013(3) O5 0.035(3) 0.026(3) 0.069(4) -0.001(3) -0.022(3) 0.000(2) O6 0.054(4) 0.017(2) 0.045(3) -0.005(2) -0.018(3) -0.004(2) O7 0.024(3) 0.030(3) 0.062(4) -0.019(2) -0.005(3) 0.004(2) O8 0.060(4) 0.024(3) 0.033(3) -0.002(2) 0.007(3) 0.016(2) O9 0.025(3) 0.028(3) 0.032(3) 0.001(2) 0.000(2) 0.002(2) O10 0.019(3) 0.026(2) 0.029(3) -0.0054(19) 0.000(2) 0.002(2) O11 0.027(3) 0.036(3) 0.037(3) -0.003(2) -0.003(2) -0.012(2) O12 0.026(3) 0.030(3) 0.036(3) -0.010(2) -0.004(2) 0.001(2) C1 0.012(4) 0.027(4) 0.037(4) -0.008(3) -0.006(3) 0.000(3) C2 0.028(4) 0.025(4) 0.029(4) -0.005(3) -0.005(3) -0.006(3) C3 0.035(5) 0.039(4) 0.041(5) -0.010(4) -0.003(4) -0.005(4) C4 0.065(7) 0.047(5) 0.031(5) 0.000(4) 0.001(5) -0.012(5) C5 0.068(7) 0.061(6) 0.044(6) -0.026(5) 0.020(5) -0.023(5) C6 0.043(6) 0.045(5) 0.048(5) -0.016(4) 0.010(5) -0.001(4) C7 0.027(4) 0.034(4) 0.035(4) -0.010(3) -0.008(4) 0.000(3) C8 0.027(5) 0.042(5) 0.038(5) -0.011(4) 0.001(4) 0.010(4) C9 0.031(5) 0.050(5) 0.070(6) -0.010(4) -0.023(5) -0.002(4) C10 0.025(5) 0.047(5) 0.068(6) -0.011(4) -0.019(4) -0.009(4) C11 0.039(5) 0.033(4) 0.035(4) -0.006(3) -0.003(4) -0.011(4) C12 0.037(5) 0.040(4) 0.030(4) -0.003(3) -0.012(4) -0.001(4) C13 0.034(5) 0.031(4) 0.035(4) -0.010(3) -0.003(4) 0.001(3) C14 0.050(6) 0.029(4) 0.035(5) 0.003(3) -0.011(4) -0.008(4) C15 0.026(4) 0.022(4) 0.026(4) -0.005(3) -0.011(3) 0.003(3) C16 0.020(4) 0.019(3) 0.027(4) -0.009(3) -0.008(3) 0.005(3) C17 0.031(4) 0.019(4) 0.044(5) -0.013(3) 0.001(4) 0.001(3) C18 0.040(5) 0.016(3) 0.045(5) -0.005(3) -0.001(4) -0.002(3) C19 0.037(5) 0.019(4) 0.030(4) -0.003(3) -0.005(4) 0.013(3) C20 0.023(4) 0.033(4) 0.050(5) -0.009(3) -0.002(4) -0.005(3) C21 0.038(5) 0.016(3) 0.044(5) -0.011(3) -0.005(4) -0.003(3) C22 0.035(5) 0.022(4) 0.025(4) -0.001(3) -0.004(3) -0.004(3) C23 0.038(5) 0.028(4) 0.039(5) -0.002(3) -0.014(4) -0.001(3) C24 0.041(5) 0.048(5) 0.025(4) 0.000(3) -0.008(4) -0.013(4) C25 0.045(6) 0.053(5) 0.030(5) -0.007(4) 0.004(4) -0.013(4) C26 0.034(5) 0.037(4) 0.032(4) -0.004(3) -0.006(4) -0.008(3) C27 0.019(4) 0.022(3) 0.021(4) -0.005(3) 0.001(3) -0.007(3) C28 0.022(4) 0.025(4) 0.032(4) -0.006(3) -0.007(3) -0.005(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 Gd1 O6 2.332(4) . ? Gd1 O7 2.342(4) 2_855 ? Gd1 O2 2.396(4) . ? Gd1 O9 2.409(4) 2_765 ? Gd1 O11 2.419(4) . ? Gd1 O12 2.431(4) . ? Gd1 O10 2.487(4) 2_765 ? Gd1 O1 2.519(4) . ? Gd1 C28 2.825(6) 2_765 ? Gd1 C1 2.831(7) . ? Gd1 O6 2.860(5) 2_855 ? Gd1 C15 2.960(6) 2_855 ? O1 C1 1.265(7) . ? O2 C1 1.265(7) . ? O3 C7 1.371(8) . ? O3 C8 1.391(7) . ? O4 C14 1.208(8) . ? O5 C14 1.309(9) . ? O5 H5 0.8200 . ? O6 C15 1.274(7) . ? O6 Gd1 2.860(5) 2_855 ? O7 C15 1.242(8) . ? O7 Gd1 2.342(4) 2_855 ? O8 C22 1.372(7) . ? O8 C19 1.384(7) . ? O9 C28 1.262(7) . ? O9 Gd1 2.409(4) 2_765 ? O10 C28 1.272(7) . ? O10 Gd1 2.487(4) 2_765 ? O11 H11A 0.8500 . ? O11 H11C 0.8501 . ? O12 H12A 0.8500 . ? O12 H12C 0.8500 . ? C1 C2 1.472(9) . ? C2 C3 1.376(9) . ? C2 C7 1.401(9) . ? C3 C4 1.373(9) . ? C3 H3 0.9300 . ? C4 C5 1.377(11) . ? C4 H4 0.9300 . ? C5 C6 1.386(11) . ? C5 H5A 0.9300 . ? C6 C7 1.379(9) . ? C6 H6 0.9300 . ? C8 C9 1.364(9) . ? C8 C13 1.384(10) . ? C9 C10 1.367(9) . ? C9 H9 0.9300 . ? C10 C11 1.377(10) . ? C10 H10 0.9300 . ? C11 C12 1.376(9) . ? C11 C14 1.504(9) . ? C12 C13 1.385(8) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.510(8) . ? C15 Gd1 2.960(6) 2_855 ? C16 C21 1.358(9) . ? C16 C17 1.400(8) . ? C17 C18 1.365(8) . ? C17 H17 0.9300 . ? C18 C19 1.377(10) . ? C18 H18 0.9300 . ? C19 C20 1.382(9) . ? C20 C21 1.390(8) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.392(8) . ? C22 C27 1.396(8) . ? C23 C24 1.380(9) . ? C23 H23 0.9300 . ? C24 C25 1.371(9) . ? C24 H24 0.9300 . ? C25 C26 1.363(9) . ? C25 H25 0.9300 . ? C26 C27 1.373(8) . ? C26 H26 0.9300 . ? C27 C28 1.484(8) . ? C28 Gd1 2.825(6) 2_765 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Gd1 O7 115.00(17) . 2_855 ? O6 Gd1 O2 95.49(16) . . ? O7 Gd1 O2 136.86(16) 2_855 . ? O6 Gd1 O9 79.74(15) . 2_765 ? O7 Gd1 O9 140.25(16) 2_855 2_765 ? O2 Gd1 O9 71.80(15) . 2_765 ? O6 Gd1 O11 71.96(14) . . ? O7 Gd1 O11 79.53(15) 2_855 . ? O2 Gd1 O11 82.14(15) . . ? O9 Gd1 O11 139.20(14) 2_765 . ? O6 Gd1 O12 151.16(14) . . ? O7 Gd1 O12 76.86(15) 2_855 . ? O2 Gd1 O12 91.08(15) . . ? O9 Gd1 O12 75.72(14) 2_765 . ? O11 Gd1 O12 136.85(14) . . ? O6 Gd1 O10 76.92(14) . 2_765 ? O7 Gd1 O10 92.75(15) 2_855 2_765 ? O2 Gd1 O10 124.80(14) . 2_765 ? O9 Gd1 O10 53.01(14) 2_765 2_765 ? O11 Gd1 O10 140.68(15) . 2_765 ? O12 Gd1 O10 76.30(14) . 2_765 ? O6 Gd1 O1 131.62(15) . . ? O7 Gd1 O1 84.25(16) 2_855 . ? O2 Gd1 O1 52.67(13) . . ? O9 Gd1 O1 114.31(15) 2_765 . ? O11 Gd1 O1 68.64(15) . . ? O12 Gd1 O1 73.47(14) . . ? O10 Gd1 O1 149.51(14) 2_765 . ? O6 Gd1 C28 74.84(17) . 2_765 ? O7 Gd1 C28 118.19(17) 2_855 2_765 ? O2 Gd1 C28 98.13(17) . 2_765 ? O9 Gd1 C28 26.40(16) 2_765 2_765 ? O11 Gd1 C28 146.65(16) . 2_765 ? O12 Gd1 C28 76.44(16) . 2_765 ? O10 Gd1 C28 26.76(15) 2_765 2_765 ? O1 Gd1 C28 136.68(17) . 2_765 ? O6 Gd1 C1 113.19(17) . . ? O7 Gd1 C1 110.50(18) 2_855 . ? O2 Gd1 C1 26.37(15) . . ? O9 Gd1 C1 94.58(17) 2_765 . ? O11 Gd1 C1 71.32(17) . . ? O12 Gd1 C1 83.91(16) . . ? O10 Gd1 C1 145.13(16) 2_765 . ? O1 Gd1 C1 26.54(14) . . ? C28 Gd1 C1 120.60(19) 2_765 . ? O6 Gd1 O6 67.90(15) . 2_855 ? O7 Gd1 O6 48.82(15) 2_855 2_855 ? O2 Gd1 O6 155.85(14) . 2_855 ? O9 Gd1 O6 119.44(14) 2_765 2_855 ? O11 Gd1 O6 76.17(13) . 2_855 ? O12 Gd1 O6 112.00(13) . 2_855 ? O10 Gd1 O6 70.15(13) 2_765 2_855 ? O1 Gd1 O6 125.64(13) . 2_855 ? C28 Gd1 O6 94.28(16) 2_765 2_855 ? C1 Gd1 O6 144.65(15) . 2_855 ? O6 Gd1 C15 92.22(18) . 2_855 ? O7 Gd1 C15 23.61(17) 2_855 2_855 ? O2 Gd1 C15 153.92(16) . 2_855 ? O9 Gd1 C15 134.21(16) 2_765 2_855 ? O11 Gd1 C15 76.64(15) . 2_855 ? O12 Gd1 C15 94.09(16) . 2_855 ? O10 Gd1 C15 81.22(15) 2_765 2_855 ? O1 Gd1 C15 104.65(16) . 2_855 ? C28 Gd1 C15 107.93(18) 2_765 2_855 ? C1 Gd1 C15 129.18(18) . 2_855 ? O6 Gd1 C15 25.21(14) 2_855 2_855 ? C1 O1 Gd1 90.6(4) . . ? C1 O2 Gd1 96.4(4) . . ? C7 O3 C8 120.4(5) . . ? C14 O5 H5 109.5 . . ? C15 O6 Gd1 159.2(4) . . ? C15 O6 Gd1 81.8(4) . 2_855 ? Gd1 O6 Gd1 112.10(15) . 2_855 ? C15 O7 Gd1 107.3(4) . 2_855 ? C22 O8 C19 123.8(5) . . ? C28 O9 Gd1 95.5(4) . 2_765 ? C28 O10 Gd1 91.6(4) . 2_765 ? Gd1 O11 H11A 109.2 . . ? Gd1 O11 H11C 109.3 . . ? H11A O11 H11C 109.5 . . ? Gd1 O12 H12A 109.2 . . ? Gd1 O12 H12C 109.3 . . ? H12A O12 H12C 109.5 . . ? O1 C1 O2 119.3(6) . . ? O1 C1 C2 120.8(6) . . ? O2 C1 C2 119.9(5) . . ? O1 C1 Gd1 62.8(3) . . ? O2 C1 Gd1 57.2(3) . . ? C2 C1 Gd1 168.3(5) . . ? C3 C2 C7 117.4(6) . . ? C3 C2 C1 119.5(6) . . ? C7 C2 C1 123.1(6) . . ? C4 C3 C2 122.6(7) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 118.7(7) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C4 C5 C6 121.2(7) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C7 C6 C5 118.7(7) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? O3 C7 C6 121.5(6) . . ? O3 C7 C2 116.8(6) . . ? C6 C7 C2 121.4(7) . . ? C9 C8 C13 120.1(6) . . ? C9 C8 O3 123.2(7) . . ? C13 C8 O3 116.5(6) . . ? C8 C9 C10 120.5(7) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 C11 120.3(7) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 119.7(7) . . ? C12 C11 C14 120.4(7) . . ? C10 C11 C14 119.9(6) . . ? C11 C12 C13 120.0(7) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C8 C13 C12 119.4(7) . . ? C8 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? O4 C14 O5 123.9(7) . . ? O4 C14 C11 122.4(8) . . ? O5 C14 C11 113.6(6) . . ? O7 C15 O6 122.1(6) . . ? O7 C15 C16 118.4(6) . . ? O6 C15 C16 119.5(6) . . ? O7 C15 Gd1 49.1(3) . 2_855 ? O6 C15 Gd1 73.0(3) . 2_855 ? C16 C15 Gd1 167.2(5) . 2_855 ? C21 C16 C17 120.2(5) . . ? C21 C16 C15 122.9(6) . . ? C17 C16 C15 116.9(6) . . ? C18 C17 C16 119.9(7) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 119.4(6) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C20 121.3(6) . . ? C18 C19 O8 114.4(6) . . ? C20 C19 O8 124.2(7) . . ? C19 C20 C21 118.6(7) . . ? C19 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? C16 C21 C20 120.4(6) . . ? C16 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? O8 C22 C23 122.7(6) . . ? O8 C22 C27 117.0(5) . . ? C23 C22 C27 120.2(6) . . ? C24 C23 C22 118.8(6) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C25 C24 C23 121.5(7) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C26 C25 C24 118.8(7) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? C25 C26 C27 122.4(7) . . ? C25 C26 H26 118.8 . . ? C27 C26 H26 118.8 . . ? C26 C27 C22 118.3(6) . . ? C26 C27 C28 118.9(6) . . ? C22 C27 C28 122.7(6) . . ? O9 C28 O10 119.2(6) . . ? O9 C28 C27 121.3(5) . . ? O10 C28 C27 119.5(6) . . ? O9 C28 Gd1 58.1(3) . 2_765 ? O10 C28 Gd1 61.6(3) . 2_765 ? C27 C28 Gd1 173.4(4) . 2_765 ? 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 O6 Gd1 O1 C1 53.2(4) . . . . ? O7 Gd1 O1 C1 171.7(4) 2_855 . . . ? O2 Gd1 O1 C1 -5.7(4) . . . . ? O9 Gd1 O1 C1 -44.9(4) 2_765 . . . ? O11 Gd1 O1 C1 90.8(4) . . . . ? O12 Gd1 O1 C1 -110.3(4) . . . . ? O10 Gd1 O1 C1 -102.6(4) 2_765 . . . ? C28 Gd1 O1 C1 -62.4(4) 2_765 . . . ? O6 Gd1 O1 C1 144.2(3) 2_855 . . . ? C15 Gd1 O1 C1 159.7(4) 2_855 . . . ? O6 Gd1 O2 C1 -134.2(4) . . . . ? O7 Gd1 O2 C1 2.1(5) 2_855 . . . ? O9 Gd1 O2 C1 148.5(4) 2_765 . . . ? O11 Gd1 O2 C1 -63.3(4) . . . . ? O12 Gd1 O2 C1 73.9(4) . . . . ? O10 Gd1 O2 C1 147.9(4) 2_765 . . . ? O1 Gd1 O2 C1 5.8(4) . . . . ? C28 Gd1 O2 C1 150.4(4) 2_765 . . . ? O6 Gd1 O2 C1 -89.4(5) 2_855 . . . ? C15 Gd1 O2 C1 -27.7(6) 2_855 . . . ? O7 Gd1 O6 C15 142.4(12) 2_855 . . . ? O2 Gd1 O6 C15 -69.0(12) . . . . ? O9 Gd1 O6 C15 1.4(12) 2_765 . . . ? O11 Gd1 O6 C15 -148.8(12) . . . . ? O12 Gd1 O6 C15 33.4(14) . . . . ? O10 Gd1 O6 C15 55.5(12) 2_765 . . . ? O1 Gd1 O6 C15 -112.1(12) . . . . ? C28 Gd1 O6 C15 28.0(12) 2_765 . . . ? C1 Gd1 O6 C15 -89.2(12) . . . . ? O6 Gd1 O6 C15 129.2(13) 2_855 . . . ? C15 Gd1 O6 C15 136.0(12) 2_855 . . . ? O7 Gd1 O6 Gd1 13.3(2) 2_855 . . 2_855 ? O2 Gd1 O6 Gd1 161.88(16) . . . 2_855 ? O9 Gd1 O6 Gd1 -127.78(18) 2_765 . . 2_855 ? O11 Gd1 O6 Gd1 82.00(17) . . . 2_855 ? O12 Gd1 O6 Gd1 -95.8(3) . . . 2_855 ? O10 Gd1 O6 Gd1 -73.63(16) 2_765 . . 2_855 ? O1 Gd1 O6 Gd1 118.71(18) . . . 2_855 ? C28 Gd1 O6 Gd1 -101.2(2) 2_765 . . 2_855 ? C1 Gd1 O6 Gd1 141.60(17) . . . 2_855 ? O6 Gd1 O6 Gd1 0.0 2_855 . . 2_855 ? C15 Gd1 O6 Gd1 6.82(18) 2_855 . . 2_855 ? Gd1 O1 C1 O2 10.0(6) . . . . ? Gd1 O1 C1 C2 -167.2(6) . . . . ? Gd1 O2 C1 O1 -10.5(6) . . . . ? Gd1 O2 C1 C2 166.7(5) . . . . ? O6 Gd1 C1 O1 -139.4(3) . . . . ? O7 Gd1 C1 O1 -8.8(4) 2_855 . . . ? O2 Gd1 C1 O1 169.7(6) . . . . ? O9 Gd1 C1 O1 139.8(3) 2_765 . . . ? O11 Gd1 C1 O1 -79.4(3) . . . . ? O12 Gd1 C1 O1 64.7(3) . . . . ? O10 Gd1 C1 O1 120.0(4) 2_765 . . . ? C28 Gd1 C1 O1 135.0(3) 2_765 . . . ? O6 Gd1 C1 O1 -55.3(5) 2_855 . . . ? C15 Gd1 C1 O1 -25.6(4) 2_855 . . . ? O6 Gd1 C1 O2 50.9(4) . . . . ? O7 Gd1 C1 O2 -178.4(4) 2_855 . . . ? O9 Gd1 C1 O2 -29.9(4) 2_765 . . . ? O11 Gd1 C1 O2 110.9(4) . . . . ? O12 Gd1 C1 O2 -104.9(4) . . . . ? O10 Gd1 C1 O2 -49.7(5) 2_765 . . . ? O1 Gd1 C1 O2 -169.7(6) . . . . ? C28 Gd1 C1 O2 -34.6(5) 2_765 . . . ? O6 Gd1 C1 O2 135.0(4) 2_855 . . . ? C15 Gd1 C1 O2 164.7(4) 2_855 . . . ? O6 Gd1 C1 C2 -28(2) . . . . ? O7 Gd1 C1 C2 102(2) 2_855 . . . ? O2 Gd1 C1 C2 -79(2) . . . . ? O9 Gd1 C1 C2 -109(2) 2_765 . . . ? O11 Gd1 C1 C2 32(2) . . . . ? O12 Gd1 C1 C2 176(2) . . . . ? O10 Gd1 C1 C2 -129(2) 2_765 . . . ? O1 Gd1 C1 C2 111(2) . . . . ? C28 Gd1 C1 C2 -114(2) 2_765 . . . ? O6 Gd1 C1 C2 56(2) 2_855 . . . ? C15 Gd1 C1 C2 85(2) 2_855 . . . ? O1 C1 C2 C3 31.5(9) . . . . ? O2 C1 C2 C3 -145.7(7) . . . . ? Gd1 C1 C2 C3 -73(2) . . . . ? O1 C1 C2 C7 -151.4(6) . . . . ? O2 C1 C2 C7 31.4(10) . . . . ? Gd1 C1 C2 C7 104(2) . . . . ? C7 C2 C3 C4 -0.9(11) . . . . ? C1 C2 C3 C4 176.3(7) . . . . ? C2 C3 C4 C5 0.4(12) . . . . ? C3 C4 C5 C6 1.2(13) . . . . ? C4 C5 C6 C7 -2.3(13) . . . . ? C8 O3 C7 C6 30.9(10) . . . . ? C8 O3 C7 C2 -155.9(6) . . . . ? C5 C6 C7 O3 174.6(7) . . . . ? C5 C6 C7 C2 1.8(11) . . . . ? C3 C2 C7 O3 -173.4(6) . . . . ? C1 C2 C7 O3 9.5(10) . . . . ? C3 C2 C7 C6 -0.2(10) . . . . ? C1 C2 C7 C6 -177.3(7) . . . . ? C7 O3 C8 C9 53.9(11) . . . . ? C7 O3 C8 C13 -131.1(7) . . . . ? C13 C8 C9 C10 -0.3(12) . . . . ? O3 C8 C9 C10 174.5(7) . . . . ? C8 C9 C10 C11 -0.6(13) . . . . ? C9 C10 C11 C12 1.8(12) . . . . ? C9 C10 C11 C14 -179.4(7) . . . . ? C10 C11 C12 C13 -2.2(11) . . . . ? C14 C11 C12 C13 179.1(6) . . . . ? C9 C8 C13 C12 -0.1(11) . . . . ? O3 C8 C13 C12 -175.2(6) . . . . ? C11 C12 C13 C8 1.3(11) . . . . ? C12 C11 C14 O4 -170.2(7) . . . . ? C10 C11 C14 O4 11.1(12) . . . . ? C12 C11 C14 O5 9.1(10) . . . . ? C10 C11 C14 O5 -169.6(7) . . . . ? Gd1 O7 C15 O6 0.3(7) 2_855 . . . ? Gd1 O7 C15 C16 177.0(4) 2_855 . . . ? Gd1 O6 C15 O7 -133.7(10) . . . . ? Gd1 O6 C15 O7 -0.2(6) 2_855 . . . ? Gd1 O6 C15 C16 49.6(14) . . . . ? Gd1 O6 C15 C16 -176.9(5) 2_855 . . . ? Gd1 O6 C15 Gd1 -133.5(12) . . . 2_855 ? O7 C15 C16 C21 -169.7(6) . . . . ? O6 C15 C16 C21 7.1(9) . . . . ? Gd1 C15 C16 C21 -159.4(16) 2_855 . . . ? O7 C15 C16 C17 7.4(9) . . . . ? O6 C15 C16 C17 -175.8(5) . . . . ? Gd1 C15 C16 C17 18(2) 2_855 . . . ? C21 C16 C17 C18 4.4(10) . . . . ? C15 C16 C17 C18 -172.8(6) . . . . ? C16 C17 C18 C19 -1.4(10) . . . . ? C17 C18 C19 C20 -2.8(11) . . . . ? C17 C18 C19 O8 -178.4(6) . . . . ? C22 O8 C19 C18 -139.4(7) . . . . ? C22 O8 C19 C20 45.2(10) . . . . ? C18 C19 C20 C21 4.0(11) . . . . ? O8 C19 C20 C21 179.1(6) . . . . ? C17 C16 C21 C20 -3.2(10) . . . . ? C15 C16 C21 C20 173.8(6) . . . . ? C19 C20 C21 C16 -0.9(10) . . . . ? C19 O8 C22 C23 16.7(11) . . . . ? C19 O8 C22 C27 -166.1(6) . . . . ? O8 C22 C23 C24 177.5(6) . . . . ? C27 C22 C23 C24 0.4(10) . . . . ? C22 C23 C24 C25 0.9(11) . . . . ? C23 C24 C25 C26 -1.8(12) . . . . ? C24 C25 C26 C27 1.5(11) . . . . ? C25 C26 C27 C22 -0.2(10) . . . . ? C25 C26 C27 C28 -177.6(7) . . . . ? O8 C22 C27 C26 -178.0(6) . . . . ? C23 C22 C27 C26 -0.8(10) . . . . ? O8 C22 C27 C28 -0.7(10) . . . . ? C23 C22 C27 C28 176.6(6) . . . . ? Gd1 O9 C28 O10 -8.5(6) 2_765 . . . ? Gd1 O9 C28 C27 172.3(5) 2_765 . . . ? Gd1 O10 C28 O9 8.2(6) 2_765 . . . ? Gd1 O10 C28 C27 -172.6(5) 2_765 . . . ? C26 C27 C28 O9 168.5(6) . . . . ? C22 C27 C28 O9 -8.8(10) . . . . ? C26 C27 C28 O10 -10.6(9) . . . . ? C22 C27 C28 O10 172.0(6) . . . . ? C26 C27 C28 Gd1 -109(4) . . . 2_765 ? C22 C27 C28 Gd1 74(4) . . . 2_765 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.939 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.153 _database_code_depnum_ccdc_archive 'CCDC 916104' ####################################################################### # # 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_exp_1355 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H21 Ho O12' _chemical_formula_weight 714.38 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7886(7) _cell_length_b 11.5573(8) _cell_length_c 12.5972(12) _cell_angle_alpha 74.649(7) _cell_angle_beta 72.626(7) _cell_angle_gamma 71.873(6) _cell_volume 1269.20(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2903 _cell_measurement_theta_min 2.5256 _cell_measurement_theta_max 28.4486 _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 3.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9104 _exptl_absorpt_correction_T_max 0.9390 _exptl_absorpt_process_details SADABS _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, Gemini' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7764 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0679 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4476 _reflns_number_gt 3969 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0156P)^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 4476 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 Ho1 Ho 1.28094(2) 0.45773(2) 0.05271(2) 0.02314(9) Uani 1 1 d . . . O1 O 1.0612(4) 0.5359(3) 0.1821(3) 0.0376(10) Uani 1 1 d . . . O2 O 1.1405(3) 0.3341(3) 0.2174(3) 0.0288(9) Uani 1 1 d . . . O3 O 0.7701(4) 0.5993(4) 0.2925(4) 0.0501(12) Uani 1 1 d . . . O4 O 0.4265(5) 1.1609(4) 0.3273(4) 0.0644(15) Uani 1 1 d . . . O5 O 0.2715(4) 1.0964(3) 0.2717(4) 0.0458(11) Uani 1 1 d . . . H5 H 0.2285 1.1702 0.2630 0.069 Uiso 1 1 calc R . . O6 O 1.3851(4) 0.6112(3) 0.0443(3) 0.0380(10) Uani 1 1 d . . . O7 O 1.5460(4) 0.7248(3) -0.0217(3) 0.0389(10) Uani 1 1 d . . . O8 O 0.9997(4) 1.1515(3) 0.1319(3) 0.0437(11) Uani 1 1 d . . . O9 O 0.8653(4) 1.3726(3) 0.0508(3) 0.0322(9) Uani 1 1 d . . . O10 O 0.6511(3) 1.4604(3) 0.1504(3) 0.0261(8) Uani 1 1 d . . . O11 O 1.3863(3) 0.4062(3) 0.2119(3) 0.0316(9) Uani 1 1 d . . . H11A H 1.4784 0.4014 0.1891 0.047 Uiso 1 1 d R . . H11C H 1.3730 0.3366 0.2509 0.047 Uiso 1 1 d R . . O12 O 1.1568(3) 0.3631(3) -0.0240(3) 0.0303(9) Uani 1 1 d . . . H12A H 1.2038 0.3563 -0.0916 0.045 Uiso 1 1 d R . . H12C H 1.0695 0.4080 -0.0238 0.045 Uiso 1 1 d R . . C1 C 1.0544(5) 0.4335(5) 0.2476(4) 0.0246(12) Uani 1 1 d . . . C2 C 0.9519(5) 0.4304(5) 0.3620(5) 0.0270(12) Uani 1 1 d . . . C3 C 0.9925(6) 0.3387(5) 0.4511(5) 0.0399(15) Uani 1 1 d . . . H3 H 1.0794 0.2768 0.4371 0.048 Uiso 1 1 calc R . . C4 C 0.9067(7) 0.3371(6) 0.5599(5) 0.0505(17) Uani 1 1 d . . . H4 H 0.9373 0.2764 0.6192 0.061 Uiso 1 1 calc R . . C5 C 0.7757(7) 0.4258(6) 0.5804(5) 0.0508(18) Uani 1 1 d . . . H5A H 0.7179 0.4253 0.6540 0.061 Uiso 1 1 calc R . . C6 C 0.7299(6) 0.5145(6) 0.4938(5) 0.0463(17) Uani 1 1 d . . . H6 H 0.6395 0.5725 0.5083 0.056 Uiso 1 1 calc R . . C7 C 0.8166(6) 0.5190(5) 0.3849(5) 0.0362(14) Uani 1 1 d . . . C8 C 0.6748(6) 0.7154(5) 0.3036(5) 0.0404(15) Uani 1 1 d . . . C9 C 0.7054(6) 0.7968(6) 0.3514(6) 0.0533(19) Uani 1 1 d . . . H9 H 0.7864 0.7723 0.3836 0.064 Uiso 1 1 calc R . . C10 C 0.6132(6) 0.9150(5) 0.3503(6) 0.0496(17) Uani 1 1 d . . . H10 H 0.6331 0.9712 0.3810 0.060 Uiso 1 1 calc R . . C11 C 0.4911(6) 0.9505(5) 0.3036(5) 0.0329(14) Uani 1 1 d . . . C12 C 0.4623(6) 0.8676(5) 0.2569(5) 0.0351(14) Uani 1 1 d . . . H12 H 0.3802 0.8912 0.2260 0.042 Uiso 1 1 calc R . . C13 C 0.5555(6) 0.7491(5) 0.2559(5) 0.0377(14) Uani 1 1 d . . . H13 H 0.5373 0.6935 0.2235 0.045 Uiso 1 1 calc R . . C14 C 0.3951(7) 1.0801(5) 0.3031(5) 0.0400(15) Uani 1 1 d . . . C15 C 1.4150(6) 0.7142(5) 0.0198(4) 0.0265(12) Uani 1 1 d . . . C16 C 1.2983(5) 0.8283(4) 0.0442(4) 0.0234(12) Uani 1 1 d . . . C17 C 1.3332(5) 0.9419(4) 0.0091(5) 0.0292(13) Uani 1 1 d . . . H17 H 1.4266 0.9467 -0.0358 0.035 Uiso 1 1 calc R . . C18 C 1.2318(6) 1.0480(5) 0.0397(5) 0.0352(14) Uani 1 1 d . . . H18 H 1.2559 1.1240 0.0154 0.042 Uiso 1 1 calc R . . C19 C 1.0938(6) 1.0396(5) 0.1069(5) 0.0309(13) Uani 1 1 d . . . C20 C 1.0524(6) 0.9295(5) 0.1357(5) 0.0353(14) Uani 1 1 d . . . H20 H 0.9562 0.9264 0.1747 0.042 Uiso 1 1 calc R . . C21 C 1.1562(5) 0.8241(5) 0.1054(5) 0.0321(13) Uani 1 1 d . . . H21 H 1.1301 0.7489 0.1266 0.038 Uiso 1 1 calc R . . C22 C 0.9056(5) 1.1614(4) 0.2364(5) 0.0274(12) Uani 1 1 d . . . C23 C 0.9235(6) 1.0748(5) 0.3345(5) 0.0368(14) Uani 1 1 d . . . H23 H 1.0017 1.0042 0.3312 0.044 Uiso 1 1 calc R . . C24 C 0.8264(6) 1.0929(5) 0.4365(5) 0.0390(15) Uani 1 1 d . . . H24 H 0.8383 1.0336 0.5016 0.047 Uiso 1 1 calc R . . C25 C 0.7114(6) 1.1982(6) 0.4431(5) 0.0454(16) Uani 1 1 d . . . H25 H 0.6455 1.2098 0.5122 0.054 Uiso 1 1 calc R . . C26 C 0.6946(5) 1.2861(5) 0.3470(5) 0.0301(13) Uani 1 1 d . . . H26 H 0.6181 1.3578 0.3522 0.036 Uiso 1 1 calc R . . C27 C 0.7898(5) 1.2702(4) 0.2422(4) 0.0233(12) Uani 1 1 d . . . C28 C 0.7685(5) 1.3713(4) 0.1431(5) 0.0250(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.02128(14) 0.01535(13) 0.02826(16) -0.00471(11) -0.00400(11) 0.00035(10) O1 0.038(2) 0.023(2) 0.035(2) -0.0007(19) -0.0016(19) 0.0051(18) O2 0.0253(19) 0.0227(19) 0.034(2) -0.0091(17) -0.0031(18) -0.0002(16) O3 0.045(2) 0.046(3) 0.042(3) -0.018(2) -0.012(2) 0.023(2) O4 0.089(3) 0.026(2) 0.096(4) -0.005(3) -0.056(3) -0.012(2) O5 0.039(2) 0.027(2) 0.072(3) -0.009(2) -0.021(2) -0.0024(19) O6 0.053(2) 0.0139(19) 0.051(3) -0.0076(18) -0.025(2) -0.0010(18) O7 0.022(2) 0.033(2) 0.056(3) -0.019(2) -0.007(2) 0.0068(17) O8 0.047(2) 0.025(2) 0.032(2) -0.0021(18) 0.002(2) 0.0163(18) O9 0.0262(19) 0.028(2) 0.028(2) 0.0018(18) -0.0039(18) 0.0049(16) O10 0.0206(18) 0.0200(19) 0.033(2) -0.0084(17) -0.0009(17) -0.0015(15) O11 0.0263(19) 0.032(2) 0.035(2) -0.0037(18) -0.0046(18) -0.0100(16) O12 0.0189(18) 0.027(2) 0.041(2) -0.0115(18) -0.0033(17) 0.0002(15) C1 0.019(3) 0.023(3) 0.029(3) -0.008(3) -0.007(2) 0.002(2) C2 0.024(3) 0.028(3) 0.026(3) -0.004(3) -0.002(2) -0.008(2) C3 0.038(3) 0.032(3) 0.041(4) -0.003(3) -0.007(3) -0.001(3) C4 0.059(4) 0.051(4) 0.031(4) 0.000(3) -0.008(3) -0.009(4) C5 0.066(5) 0.057(4) 0.023(3) -0.010(3) 0.010(3) -0.024(4) C6 0.040(4) 0.045(4) 0.043(4) -0.018(3) 0.003(3) -0.001(3) C7 0.034(3) 0.037(3) 0.035(4) -0.012(3) -0.005(3) -0.002(3) C8 0.028(3) 0.040(4) 0.038(4) -0.007(3) -0.001(3) 0.005(3) C9 0.031(3) 0.051(4) 0.073(5) -0.009(4) -0.025(4) 0.005(3) C10 0.047(4) 0.041(4) 0.068(5) -0.009(4) -0.020(4) -0.015(3) C11 0.028(3) 0.034(3) 0.033(3) -0.002(3) -0.007(3) -0.007(3) C12 0.035(3) 0.033(3) 0.030(3) -0.002(3) -0.013(3) 0.002(3) C13 0.036(3) 0.039(3) 0.036(4) -0.009(3) -0.015(3) 0.002(3) C14 0.047(4) 0.029(3) 0.037(4) 0.004(3) -0.012(3) -0.006(3) C15 0.032(3) 0.022(3) 0.025(3) -0.010(2) -0.014(3) 0.006(2) C16 0.025(3) 0.016(3) 0.027(3) -0.003(2) -0.006(2) -0.003(2) C17 0.025(3) 0.022(3) 0.035(3) -0.009(3) -0.002(3) 0.000(2) C18 0.042(3) 0.018(3) 0.041(4) -0.009(3) -0.004(3) -0.003(3) C19 0.032(3) 0.017(3) 0.034(3) -0.009(3) -0.007(3) 0.011(2) C20 0.025(3) 0.031(3) 0.042(4) -0.012(3) 0.005(3) -0.004(3) C21 0.031(3) 0.023(3) 0.040(4) -0.007(3) -0.008(3) -0.004(2) C22 0.029(3) 0.019(3) 0.031(3) -0.009(2) -0.002(3) -0.002(2) C23 0.034(3) 0.030(3) 0.036(4) -0.001(3) -0.009(3) 0.002(3) C24 0.048(4) 0.036(3) 0.031(4) 0.005(3) -0.010(3) -0.016(3) C25 0.040(4) 0.055(4) 0.031(4) -0.006(3) 0.012(3) -0.018(3) C26 0.025(3) 0.031(3) 0.030(3) -0.009(3) -0.005(3) 0.000(2) C27 0.022(3) 0.024(3) 0.023(3) -0.002(2) -0.004(2) -0.007(2) C28 0.023(3) 0.021(3) 0.029(3) -0.009(2) 0.000(3) -0.005(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 Ho1 O6 2.271(4) . ? Ho1 O7 2.300(3) 2_865 ? Ho1 O1 2.361(3) . ? Ho1 O9 2.368(3) 2_775 ? Ho1 O11 2.379(3) . ? Ho1 O12 2.387(3) . ? Ho1 O10 2.445(4) 2_775 ? Ho1 O2 2.487(3) . ? Ho1 C28 2.785(5) 2_775 ? O1 C1 1.260(6) . ? O2 C1 1.269(5) . ? O3 C7 1.379(6) . ? O3 C8 1.390(6) . ? O4 C14 1.202(7) . ? O5 C14 1.327(6) . ? O5 H5 0.8200 . ? O6 C15 1.251(6) . ? O7 C15 1.264(6) . ? O7 Ho1 2.300(3) 2_865 ? O8 C22 1.372(6) . ? O8 C19 1.386(5) . ? O9 C28 1.261(6) . ? O9 Ho1 2.368(3) 2_775 ? O10 C28 1.280(5) . ? O10 Ho1 2.445(4) 2_775 ? O11 H11A 0.8499 . ? O11 H11C 0.8500 . ? O12 H12A 0.8500 . ? O12 H12C 0.8499 . ? C1 C2 1.488(7) . ? C2 C3 1.385(7) . ? C2 C7 1.403(7) . ? C3 C4 1.376(8) . ? C3 H3 0.9300 . ? C4 C5 1.373(8) . ? C4 H4 0.9300 . ? C5 C6 1.362(8) . ? C5 H5A 0.9300 . ? C6 C7 1.379(8) . ? C6 H6 0.9300 . ? C8 C13 1.374(7) . ? C8 C9 1.386(8) . ? C9 C10 1.383(8) . ? C9 H9 0.9300 . ? C10 C11 1.389(7) . ? C10 H10 0.9300 . ? C11 C12 1.381(7) . ? C11 C14 1.500(7) . ? C12 C13 1.391(7) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.486(6) . ? C16 C21 1.384(7) . ? C16 C17 1.385(7) . ? C17 C18 1.379(6) . ? C17 H17 0.9300 . ? C18 C19 1.380(7) . ? C18 H18 0.9300 . ? C19 C20 1.380(7) . ? C20 C21 1.381(7) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.387(7) . ? C22 C27 1.408(6) . ? C23 C24 1.374(8) . ? C23 H23 0.9300 . ? C24 C25 1.379(7) . ? C24 H24 0.9300 . ? C25 C26 1.374(8) . ? C25 H25 0.9300 . ? C26 C27 1.390(7) . ? C26 H26 0.9300 . ? C27 C28 1.484(7) . ? C28 Ho1 2.785(5) 2_775 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Ho1 O7 112.56(13) . 2_865 ? O6 Ho1 O1 93.84(14) . . ? O7 Ho1 O1 141.09(13) 2_865 . ? O6 Ho1 O9 79.61(12) . 2_775 ? O7 Ho1 O9 138.00(14) 2_865 2_775 ? O1 Ho1 O9 72.45(12) . 2_775 ? O6 Ho1 O11 71.67(12) . . ? O7 Ho1 O11 78.77(13) 2_865 . ? O1 Ho1 O11 83.48(12) . . ? O9 Ho1 O11 140.95(12) 2_775 . ? O6 Ho1 O12 151.74(13) . . ? O7 Ho1 O12 77.87(12) 2_865 . ? O1 Ho1 O12 92.36(13) . . ? O9 Ho1 O12 76.07(12) 2_775 . ? O11 Ho1 O12 136.49(12) . . ? O6 Ho1 O10 76.82(13) . 2_775 ? O7 Ho1 O10 88.48(12) 2_865 2_775 ? O1 Ho1 O10 126.42(11) . 2_775 ? O9 Ho1 O10 53.99(11) 2_775 2_775 ? O11 Ho1 O10 137.86(11) . 2_775 ? O12 Ho1 O10 77.33(11) . 2_775 ? O6 Ho1 O2 130.61(13) . . ? O7 Ho1 O2 87.75(12) 2_865 . ? O1 Ho1 O2 53.48(11) . . ? O9 Ho1 O2 115.37(11) 2_775 . ? O11 Ho1 O2 68.98(11) . . ? O12 Ho1 O2 73.91(12) . . ? O10 Ho1 O2 151.15(11) 2_775 . ? O6 Ho1 C28 74.58(14) . 2_775 ? O7 Ho1 C28 114.78(14) 2_865 2_775 ? O1 Ho1 C28 99.10(13) . 2_775 ? O9 Ho1 C28 26.80(12) 2_775 2_775 ? O11 Ho1 C28 146.25(13) . 2_775 ? O12 Ho1 C28 77.22(13) . 2_775 ? O10 Ho1 C28 27.35(12) 2_775 2_775 ? O2 Ho1 C28 138.34(12) . 2_775 ? C1 O1 Ho1 96.1(3) . . ? C1 O2 Ho1 90.0(3) . . ? C7 O3 C8 120.6(5) . . ? C14 O5 H5 109.5 . . ? C15 O6 Ho1 161.7(3) . . ? C15 O7 Ho1 114.5(3) . 2_865 ? C22 O8 C19 122.4(4) . . ? C28 O9 Ho1 95.4(3) . 2_775 ? C28 O10 Ho1 91.3(3) . 2_775 ? Ho1 O11 H11A 109.3 . . ? Ho1 O11 H11C 109.2 . . ? H11A O11 H11C 109.5 . . ? Ho1 O12 H12A 109.1 . . ? Ho1 O12 H12C 109.4 . . ? H12A O12 H12C 109.5 . . ? O1 C1 O2 119.5(5) . . ? O1 C1 C2 119.8(4) . . ? O2 C1 C2 120.6(5) . . ? C3 C2 C7 118.0(5) . . ? C3 C2 C1 119.1(5) . . ? C7 C2 C1 122.9(5) . . ? C4 C3 C2 121.3(5) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 119.6(6) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C6 C5 C4 120.5(6) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C7 120.5(5) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? O3 C7 C6 122.9(5) . . ? O3 C7 C2 116.6(5) . . ? C6 C7 C2 120.1(6) . . ? C13 C8 C9 121.8(5) . . ? C13 C8 O3 116.4(6) . . ? C9 C8 O3 121.7(5) . . ? C10 C9 C8 118.7(6) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C9 C10 C11 120.4(6) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 119.9(5) . . ? C12 C11 C14 121.5(5) . . ? C10 C11 C14 118.6(5) . . ? C11 C12 C13 120.3(5) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C8 C13 C12 119.0(6) . . ? C8 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? O4 C14 O5 123.5(5) . . ? O4 C14 C11 124.1(6) . . ? O5 C14 C11 112.4(5) . . ? O6 C15 O7 121.7(5) . . ? O6 C15 C16 121.1(5) . . ? O7 C15 C16 117.2(5) . . ? C21 C16 C17 118.6(5) . . ? C21 C16 C15 121.8(5) . . ? C17 C16 C15 119.5(5) . . ? C18 C17 C16 121.1(5) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 118.9(5) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C20 C19 C18 121.0(5) . . ? C20 C19 O8 124.2(5) . . ? C18 C19 O8 114.5(5) . . ? C19 C20 C21 118.9(5) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C20 C21 C16 121.1(5) . . ? C20 C21 H21 119.4 . . ? C16 C21 H21 119.4 . . ? O8 C22 C23 123.9(5) . . ? O8 C22 C27 116.4(5) . . ? C23 C22 C27 119.6(5) . . ? C24 C23 C22 120.4(5) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.4(5) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 119.7(6) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 121.3(5) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C26 C27 C22 118.4(5) . . ? C26 C27 C28 118.3(4) . . ? C22 C27 C28 123.2(5) . . ? O9 C28 O10 118.6(5) . . ? O9 C28 C27 121.2(4) . . ? O10 C28 C27 120.1(5) . . ? O9 C28 Ho1 57.8(3) . 2_775 ? O10 C28 Ho1 61.3(3) . 2_775 ? C27 C28 Ho1 173.4(4) . 2_775 ? 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 O6 Ho1 O1 C1 -134.0(3) . . . . ? O7 Ho1 O1 C1 0.1(4) 2_865 . . . ? O9 Ho1 O1 C1 148.2(3) 2_775 . . . ? O11 Ho1 O1 C1 -63.0(3) . . . . ? O12 Ho1 O1 C1 73.6(3) . . . . ? O10 Ho1 O1 C1 149.5(3) 2_775 . . . ? O2 Ho1 O1 C1 5.6(3) . . . . ? C28 Ho1 O1 C1 151.0(3) 2_775 . . . ? O6 Ho1 O2 C1 52.8(3) . . . . ? O7 Ho1 O2 C1 170.9(3) 2_865 . . . ? O1 Ho1 O2 C1 -5.6(3) . . . . ? O9 Ho1 O2 C1 -45.5(3) 2_775 . . . ? O11 Ho1 O2 C1 92.1(3) . . . . ? O12 Ho1 O2 C1 -111.0(3) . . . . ? O10 Ho1 O2 C1 -106.3(3) 2_775 . . . ? C28 Ho1 O2 C1 -63.1(4) 2_775 . . . ? O7 Ho1 O6 C15 131.5(12) 2_865 . . . ? O1 Ho1 O6 C15 -77.7(12) . . . . ? O9 Ho1 O6 C15 -6.4(12) 2_775 . . . ? O11 Ho1 O6 C15 -159.6(12) . . . . ? O12 Ho1 O6 C15 24.5(14) . . . . ? O10 Ho1 O6 C15 48.8(12) 2_775 . . . ? O2 Ho1 O6 C15 -121.0(12) . . . . ? C28 Ho1 O6 C15 20.7(12) 2_775 . . . ? Ho1 O1 C1 O2 -10.2(5) . . . . ? Ho1 O1 C1 C2 166.4(4) . . . . ? Ho1 O2 C1 O1 9.7(5) . . . . ? Ho1 O2 C1 C2 -166.9(4) . . . . ? O1 C1 C2 C3 -146.5(5) . . . . ? O2 C1 C2 C3 30.1(8) . . . . ? O1 C1 C2 C7 31.6(8) . . . . ? O2 C1 C2 C7 -151.8(5) . . . . ? C7 C2 C3 C4 -3.0(9) . . . . ? C1 C2 C3 C4 175.2(6) . . . . ? C2 C3 C4 C5 2.2(10) . . . . ? C3 C4 C5 C6 0.4(10) . . . . ? C4 C5 C6 C7 -2.1(11) . . . . ? C8 O3 C7 C6 32.2(9) . . . . ? C8 O3 C7 C2 -154.9(5) . . . . ? C5 C6 C7 O3 173.9(6) . . . . ? C5 C6 C7 C2 1.2(10) . . . . ? C3 C2 C7 O3 -171.9(5) . . . . ? C1 C2 C7 O3 10.0(8) . . . . ? C3 C2 C7 C6 1.3(9) . . . . ? C1 C2 C7 C6 -176.8(5) . . . . ? C7 O3 C8 C13 -132.6(6) . . . . ? C7 O3 C8 C9 52.7(8) . . . . ? C13 C8 C9 C10 -0.3(10) . . . . ? O3 C8 C9 C10 174.1(6) . . . . ? C8 C9 C10 C11 1.0(10) . . . . ? C9 C10 C11 C12 -0.7(10) . . . . ? C9 C10 C11 C14 -179.3(6) . . . . ? C10 C11 C12 C13 -0.3(9) . . . . ? C14 C11 C12 C13 178.3(5) . . . . ? C9 C8 C13 C12 -0.7(9) . . . . ? O3 C8 C13 C12 -175.3(5) . . . . ? C11 C12 C13 C8 1.0(9) . . . . ? C12 C11 C14 O4 -168.8(6) . . . . ? C10 C11 C14 O4 9.8(10) . . . . ? C12 C11 C14 O5 10.6(8) . . . . ? C10 C11 C14 O5 -170.8(5) . . . . ? Ho1 O6 C15 O7 -125.8(10) . . . . ? Ho1 O6 C15 C16 57.5(14) . . . . ? Ho1 O7 C15 O6 1.9(6) 2_865 . . . ? Ho1 O7 C15 C16 178.7(3) 2_865 . . . ? O6 C15 C16 C21 7.0(8) . . . . ? O7 C15 C16 C21 -169.8(5) . . . . ? O6 C15 C16 C17 -175.7(5) . . . . ? O7 C15 C16 C17 7.5(7) . . . . ? C21 C16 C17 C18 3.7(8) . . . . ? C15 C16 C17 C18 -173.6(5) . . . . ? C16 C17 C18 C19 0.4(9) . . . . ? C17 C18 C19 C20 -5.5(9) . . . . ? C17 C18 C19 O8 -179.4(5) . . . . ? C22 O8 C19 C20 45.1(8) . . . . ? C22 O8 C19 C18 -141.2(5) . . . . ? C18 C19 C20 C21 6.3(9) . . . . ? O8 C19 C20 C21 179.6(5) . . . . ? C19 C20 C21 C16 -2.1(9) . . . . ? C17 C16 C21 C20 -2.8(8) . . . . ? C15 C16 C21 C20 174.5(5) . . . . ? C19 O8 C22 C23 20.0(9) . . . . ? C19 O8 C22 C27 -163.5(5) . . . . ? O8 C22 C23 C24 178.4(5) . . . . ? C27 C22 C23 C24 2.0(9) . . . . ? C22 C23 C24 C25 -1.1(9) . . . . ? C23 C24 C25 C26 -0.5(9) . . . . ? C24 C25 C26 C27 1.3(9) . . . . ? C25 C26 C27 C22 -0.4(8) . . . . ? C25 C26 C27 C28 -177.6(5) . . . . ? O8 C22 C27 C26 -177.9(5) . . . . ? C23 C22 C27 C26 -1.2(8) . . . . ? O8 C22 C27 C28 -0.9(8) . . . . ? C23 C22 C27 C28 175.8(5) . . . . ? Ho1 O9 C28 O10 -8.6(5) 2_775 . . . ? Ho1 O9 C28 C27 172.3(4) 2_775 . . . ? Ho1 O10 C28 O9 8.3(5) 2_775 . . . ? Ho1 O10 C28 C27 -172.6(4) 2_775 . . . ? C26 C27 C28 O9 167.4(5) . . . . ? C22 C27 C28 O9 -9.6(8) . . . . ? C26 C27 C28 O10 -11.7(7) . . . . ? C22 C27 C28 O10 171.2(5) . . . . ? C26 C27 C28 Ho1 -113(3) . . . 2_775 ? C22 C27 C28 Ho1 70(3) . . . 2_775 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.841 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.126 _database_code_depnum_ccdc_archive 'CCDC 916105' ####################################################################### # # 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_exp_1343 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H42 Er2 O24' _chemical_formula_weight 1433.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8061(9) _cell_length_b 11.5898(8) _cell_length_c 12.6074(10) _cell_angle_alpha 74.575(6) _cell_angle_beta 72.548(8) _cell_angle_gamma 71.682(7) _cell_volume 1274.08(18) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.4868 _cell_measurement_theta_max 28.4184 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.868 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 706 _exptl_absorpt_coefficient_mu 3.363 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.96774 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7648 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.1115 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4489 _reflns_number_gt 3564 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^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 4489 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1000 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.003 _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 C1 C 1.4120(9) 0.7126(7) 0.0216(7) 0.027(2) Uani 1 1 d . . . C2 C 1.2960(8) 0.8277(6) 0.0451(7) 0.0196(18) Uani 1 1 d . . . C3 C 1.1544(9) 0.8246(7) 0.1047(7) 0.030(2) Uani 1 1 d . . . H21 H 1.1273 0.7503 0.1243 0.036 Uiso 1 1 calc R . . C4 C 1.0506(9) 0.9308(7) 0.1365(8) 0.033(2) Uani 1 1 d . . . H20 H 0.9550 0.9281 0.1771 0.040 Uiso 1 1 calc R . . C5 C 1.0935(9) 1.0403(7) 0.1062(7) 0.029(2) Uani 1 1 d . . . C6 C 1.2320(9) 1.0457(7) 0.0410(8) 0.031(2) Uani 1 1 d . . . H18 H 1.2575 1.1208 0.0187 0.038 Uiso 1 1 calc R . . C7 C 1.3339(9) 0.9408(7) 0.0083(7) 0.028(2) Uani 1 1 d . . . H17 H 1.4267 0.9453 -0.0378 0.034 Uiso 1 1 calc R . . C8 C 0.9053(9) 1.1617(7) 0.2371(8) 0.028(2) Uani 1 1 d . . . C9 C 0.9233(10) 1.0745(7) 0.3351(8) 0.036(2) Uani 1 1 d . . . H23 H 1.0012 1.0036 0.3322 0.043 Uiso 1 1 calc R . . C10 C 0.8258(10) 1.0940(8) 0.4352(8) 0.040(2) Uani 1 1 d . . . H24 H 0.8375 1.0345 0.5001 0.048 Uiso 1 1 calc R . . C11 C 0.7100(10) 1.1988(8) 0.4441(8) 0.043(3) Uani 1 1 d . . . H25 H 0.6441 1.2103 0.5133 0.052 Uiso 1 1 calc R . . C12 C 0.6957(9) 1.2855(8) 0.3470(8) 0.036(2) Uani 1 1 d . . . H26 H 0.6186 1.3569 0.3518 0.044 Uiso 1 1 calc R . . C13 C 0.7910(8) 1.2715(6) 0.2424(7) 0.0183(18) Uani 1 1 d . . . C14 C 0.7721(9) 1.3733(6) 0.1429(7) 0.029(2) Uani 1 1 d . . . C15 C 1.0550(9) 0.4338(7) 0.2485(7) 0.027(2) Uani 1 1 d . . . C16 C 0.9516(9) 0.4296(7) 0.3614(7) 0.026(2) Uani 1 1 d . . . C17 C 0.9930(10) 0.3384(7) 0.4516(8) 0.036(2) Uani 1 1 d . . . H3 H 1.0812 0.2777 0.4381 0.043 Uiso 1 1 calc R . . C18 C 0.9070(12) 0.3361(9) 0.5596(9) 0.056(3) Uani 1 1 d . . . H4 H 0.9367 0.2737 0.6181 0.067 Uiso 1 1 calc R . . C19 C 0.7766(11) 0.4257(9) 0.5823(9) 0.052(3) Uani 1 1 d . . . H5A H 0.7206 0.4261 0.6562 0.062 Uiso 1 1 calc R . . C20 C 0.7295(11) 0.5156(8) 0.4935(8) 0.046(3) Uani 1 1 d . . . H6 H 0.6393 0.5742 0.5073 0.055 Uiso 1 1 calc R . . C21 C 0.8170(10) 0.5172(7) 0.3857(8) 0.033(2) Uani 1 1 d . . . C22 C 0.6741(11) 0.7146(8) 0.3037(8) 0.039(2) Uani 1 1 d . . . C23 C 0.5556(10) 0.7496(8) 0.2569(8) 0.036(2) Uani 1 1 d . . . H13 H 0.5376 0.6939 0.2247 0.043 Uiso 1 1 calc R . . C24 C 0.4606(10) 0.8681(8) 0.2565(8) 0.039(2) Uani 1 1 d . . . H12 H 0.3790 0.8918 0.2252 0.046 Uiso 1 1 calc R . . C25 C 0.4911(10) 0.9502(7) 0.3043(7) 0.032(2) Uani 1 1 d . . . C26 C 0.6121(11) 0.9133(8) 0.3494(9) 0.050(3) Uani 1 1 d . . . H10 H 0.6325 0.9691 0.3799 0.060 Uiso 1 1 calc R . . C27 C 0.7055(11) 0.7944(9) 0.3508(10) 0.056(3) Uani 1 1 d . . . H9 H 0.7867 0.7698 0.3826 0.067 Uiso 1 1 calc R . . C28 C 0.3961(11) 1.0786(8) 0.3017(8) 0.037(2) Uani 1 1 d . . . O1 O 1.3847(6) 0.4053(5) 0.2124(5) 0.0318(15) Uani 1 1 d . . . H11A H 1.4034 0.3273 0.2356 0.048 Uiso 1 1 d R . . H11B H 1.4645 0.4283 0.1927 0.048 Uiso 1 1 d R . . O2 O 1.1598(6) 0.3630(5) -0.0259(5) 0.0320(15) Uani 1 1 d . . . H12A H 1.0640 0.3972 -0.0137 0.048 Uiso 1 1 d R . . H12B H 1.1955 0.3716 -0.0996 0.048 Uiso 1 1 d R . . O3 O 1.3794(7) 0.6114(5) 0.0463(5) 0.0407(17) Uani 1 1 d . . . O4 O 1.5428(6) 0.7200(5) -0.0187(5) 0.0370(17) Uani 1 1 d . . . O5 O 1.1410(6) 0.3337(4) 0.2167(5) 0.0295(15) Uani 1 1 d . . . O6 O 1.0616(6) 0.5356(5) 0.1814(5) 0.0389(17) Uani 1 1 d . . . O7 O 0.2716(7) 1.0963(5) 0.2713(6) 0.0481(19) Uani 1 1 d . . . H5 H 0.2292 1.1702 0.2629 0.072 Uiso 1 1 calc R . . O8 O 0.4273(8) 1.1593(6) 0.3281(7) 0.064(2) Uani 1 1 d . . . O9 O 0.6508(6) 1.4605(4) 0.1489(5) 0.0286(14) Uani 1 1 d . . . O10 O 0.8667(6) 1.3740(4) 0.0509(5) 0.0308(15) Uani 1 1 d . . . O11 O 0.7702(7) 0.5985(5) 0.2922(5) 0.0485(19) Uani 1 1 d . . . O12 O 0.9996(7) 1.1525(4) 0.1314(5) 0.0415(18) Uani 1 1 d . . . Er1 Er 1.27907(4) 0.45756(3) 0.05343(4) 0.02378(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(5) 0.026(5) 0.034(6) -0.010(4) -0.014(4) 0.000(4) C2 0.019(4) 0.021(4) 0.019(5) -0.012(4) -0.004(4) 0.000(3) C3 0.029(5) 0.020(4) 0.035(6) -0.007(4) -0.005(4) 0.000(4) C4 0.023(5) 0.032(5) 0.034(6) -0.008(4) 0.001(4) 0.001(4) C5 0.026(5) 0.017(4) 0.032(6) -0.004(4) -0.003(4) 0.006(4) C6 0.039(6) 0.018(4) 0.037(6) -0.004(4) -0.011(4) -0.006(4) C7 0.028(5) 0.024(5) 0.030(5) -0.005(4) -0.008(4) -0.003(4) C8 0.020(5) 0.024(4) 0.034(6) -0.009(4) 0.005(4) -0.007(4) C9 0.043(6) 0.025(5) 0.030(6) 0.007(4) -0.014(5) 0.000(4) C10 0.046(6) 0.039(5) 0.031(6) 0.003(4) -0.015(5) -0.008(5) C11 0.041(6) 0.045(6) 0.028(6) -0.003(5) 0.010(5) -0.011(5) C12 0.022(5) 0.036(5) 0.044(7) -0.014(5) 0.003(5) -0.002(4) C13 0.016(4) 0.013(4) 0.021(5) -0.001(3) -0.004(4) -0.001(3) C14 0.038(5) 0.008(4) 0.030(6) -0.005(4) 0.010(4) -0.007(4) C15 0.023(5) 0.033(5) 0.025(5) -0.006(4) -0.010(4) 0.000(4) C16 0.026(5) 0.024(4) 0.026(5) -0.007(4) -0.001(4) -0.005(4) C17 0.037(6) 0.030(5) 0.039(6) -0.008(4) -0.009(5) -0.005(4) C18 0.073(8) 0.058(7) 0.029(6) -0.005(5) -0.006(6) -0.015(6) C19 0.055(7) 0.056(7) 0.035(7) -0.021(5) 0.008(6) -0.008(6) C20 0.043(6) 0.047(6) 0.037(6) -0.020(5) 0.005(5) 0.001(5) C21 0.037(6) 0.032(5) 0.026(6) -0.010(4) -0.007(4) 0.002(4) C22 0.040(6) 0.040(6) 0.029(6) -0.008(5) -0.004(5) -0.001(5) C23 0.048(6) 0.033(5) 0.028(6) -0.012(4) -0.010(5) -0.007(4) C24 0.046(6) 0.043(6) 0.030(6) -0.005(4) -0.017(5) -0.008(5) C25 0.031(5) 0.029(5) 0.025(5) 0.004(4) -0.006(4) 0.000(4) C26 0.050(7) 0.038(6) 0.068(8) -0.005(5) -0.023(6) -0.014(5) C27 0.040(7) 0.056(7) 0.072(9) -0.015(6) -0.025(6) -0.001(5) C28 0.050(7) 0.024(5) 0.033(6) 0.004(4) -0.011(5) -0.009(4) O1 0.023(3) 0.034(3) 0.039(4) -0.003(3) -0.006(3) -0.014(3) O2 0.016(3) 0.042(3) 0.035(4) -0.012(3) -0.001(3) -0.005(3) O3 0.062(5) 0.018(3) 0.050(5) -0.009(3) -0.028(3) -0.004(3) O4 0.015(3) 0.029(3) 0.059(5) -0.009(3) -0.006(3) 0.003(2) O5 0.026(3) 0.024(3) 0.033(4) -0.004(3) -0.004(3) -0.003(3) O6 0.044(4) 0.020(3) 0.036(4) 0.001(3) 0.000(3) 0.000(3) O7 0.044(4) 0.025(3) 0.076(6) -0.001(4) -0.032(4) 0.001(3) O8 0.082(6) 0.031(4) 0.094(7) -0.010(4) -0.057(5) -0.002(4) O9 0.022(3) 0.026(3) 0.031(4) -0.005(3) -0.003(3) -0.001(3) O10 0.027(3) 0.021(3) 0.028(4) 0.006(3) 0.000(3) 0.001(2) O11 0.041(4) 0.049(4) 0.035(4) -0.017(3) -0.011(3) 0.027(3) O12 0.048(4) 0.015(3) 0.036(4) -0.005(3) 0.006(3) 0.010(3) Er1 0.0208(2) 0.0165(2) 0.0290(2) -0.00372(15) -0.00409(16) 0.00000(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O3 1.247(9) . ? C1 O4 1.251(9) . ? C1 C2 1.488(10) . ? C2 C3 1.372(10) . ? C2 C7 1.398(10) . ? C3 C4 1.394(10) . ? C3 H21 0.9300 . ? C4 C5 1.384(10) . ? C4 H20 0.9300 . ? C5 C6 1.371(11) . ? C5 O12 1.389(8) . ? C6 C7 1.379(10) . ? C6 H18 0.9300 . ? C7 H17 0.9300 . ? C8 O12 1.385(9) . ? C8 C9 1.390(11) . ? C8 C13 1.409(10) . ? C9 C10 1.360(11) . ? C9 H23 0.9300 . ? C10 C11 1.381(11) . ? C10 H24 0.9300 . ? C11 C12 1.374(12) . ? C11 H25 0.9300 . ? C12 C13 1.385(11) . ? C12 H26 0.9300 . ? C13 C14 1.489(11) . ? C14 O10 1.249(9) . ? C14 O9 1.294(9) . ? C14 Er1 2.787(9) 2_775 ? C15 O6 1.264(9) . ? C15 O5 1.283(8) . ? C15 C16 1.478(11) . ? C15 Er1 2.781(8) . ? C16 C17 1.394(12) . ? C16 C21 1.395(10) . ? C17 C18 1.368(12) . ? C17 H3 0.9300 . ? C18 C19 1.378(12) . ? C18 H4 0.9300 . ? C19 C20 1.392(14) . ? C19 H5A 0.9300 . ? C20 C21 1.372(12) . ? C20 H6 0.9300 . ? C21 O11 1.397(10) . ? C22 C23 1.361(13) . ? C22 C27 1.372(13) . ? C22 O11 1.395(9) . ? C23 C24 1.396(11) . ? C23 H13 0.9300 . ? C24 C25 1.396(12) . ? C24 H12 0.9300 . ? C25 C26 1.368(13) . ? C25 C28 1.485(11) . ? C26 C27 1.394(12) . ? C26 H10 0.9300 . ? C27 H9 0.9300 . ? C28 O8 1.220(11) . ? C28 O7 1.327(11) . ? O1 Er1 2.380(6) . ? O1 H11A 0.8510 . ? O1 H11B 0.8510 . ? O2 Er1 2.378(6) . ? O2 H12A 0.8802 . ? O2 H12B 0.8792 . ? O3 Er1 2.263(6) . ? O4 Er1 2.288(5) 2_865 ? O5 Er1 2.472(5) . ? O6 Er1 2.339(5) . ? O7 H5 0.8200 . ? O9 Er1 2.439(6) 2_775 ? O10 Er1 2.365(5) 2_775 ? Er1 O4 2.288(5) 2_865 ? Er1 O10 2.365(5) 2_775 ? Er1 O9 2.439(6) 2_775 ? Er1 C14 2.787(9) 2_775 ? 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 O3 C1 O4 121.5(7) . . ? O3 C1 C2 120.4(7) . . ? O4 C1 C2 118.0(7) . . ? C3 C2 C7 119.5(7) . . ? C3 C2 C1 121.6(7) . . ? C7 C2 C1 118.9(7) . . ? C2 C3 C4 121.2(7) . . ? C2 C3 H21 119.4 . . ? C4 C3 H21 119.4 . . ? C5 C4 C3 118.3(8) . . ? C5 C4 H20 120.8 . . ? C3 C4 H20 120.8 . . ? C6 C5 C4 120.8(7) . . ? C6 C5 O12 115.4(7) . . ? C4 C5 O12 123.7(7) . . ? C5 C6 C7 120.7(7) . . ? C5 C6 H18 119.6 . . ? C7 C6 H18 119.6 . . ? C6 C7 C2 119.2(8) . . ? C6 C7 H17 120.4 . . ? C2 C7 H17 120.4 . . ? O12 C8 C9 124.1(7) . . ? O12 C8 C13 115.5(7) . . ? C9 C8 C13 120.3(8) . . ? C10 C9 C8 119.3(8) . . ? C10 C9 H23 120.4 . . ? C8 C9 H23 120.4 . . ? C9 C10 C11 122.5(9) . . ? C9 C10 H24 118.7 . . ? C11 C10 H24 118.7 . . ? C12 C11 C10 117.5(8) . . ? C12 C11 H25 121.3 . . ? C10 C11 H25 121.3 . . ? C11 C12 C13 123.0(8) . . ? C11 C12 H26 118.5 . . ? C13 C12 H26 118.5 . . ? C12 C13 C8 117.4(8) . . ? C12 C13 C14 119.3(7) . . ? C8 C13 C14 123.3(7) . . ? O10 C14 O9 118.4(8) . . ? O10 C14 C13 122.0(7) . . ? O9 C14 C13 119.5(7) . . ? O10 C14 Er1 57.6(4) . 2_775 ? O9 C14 Er1 61.1(4) . 2_775 ? C13 C14 Er1 171.9(6) . 2_775 ? O6 C15 O5 118.4(7) . . ? O6 C15 C16 121.0(7) . . ? O5 C15 C16 120.6(7) . . ? O6 C15 Er1 56.7(4) . . ? O5 C15 Er1 62.7(4) . . ? C16 C15 Er1 169.5(6) . . ? C17 C16 C21 117.1(8) . . ? C17 C16 C15 119.1(8) . . ? C21 C16 C15 123.7(8) . . ? C18 C17 C16 121.5(9) . . ? C18 C17 H3 119.2 . . ? C16 C17 H3 119.2 . . ? C17 C18 C19 120.5(10) . . ? C17 C18 H4 119.8 . . ? C19 C18 H4 119.8 . . ? C18 C19 C20 119.5(9) . . ? C18 C19 H5A 120.3 . . ? C20 C19 H5A 120.3 . . ? C21 C20 C19 119.5(9) . . ? C21 C20 H6 120.3 . . ? C19 C20 H6 120.3 . . ? C20 C21 C16 121.9(9) . . ? C20 C21 O11 122.0(8) . . ? C16 C21 O11 115.8(7) . . ? C23 C22 C27 121.5(9) . . ? C23 C22 O11 117.1(9) . . ? C27 C22 O11 121.1(10) . . ? C22 C23 C24 120.7(9) . . ? C22 C23 H13 119.6 . . ? C24 C23 H13 119.6 . . ? C25 C24 C23 118.4(9) . . ? C25 C24 H12 120.8 . . ? C23 C24 H12 120.8 . . ? C26 C25 C24 119.7(9) . . ? C26 C25 C28 120.2(9) . . ? C24 C25 C28 120.1(9) . . ? C25 C26 C27 121.6(10) . . ? C25 C26 H10 119.2 . . ? C27 C26 H10 119.2 . . ? C22 C27 C26 118.0(10) . . ? C22 C27 H9 121.0 . . ? C26 C27 H9 121.0 . . ? O8 C28 O7 123.0(9) . . ? O8 C28 C25 123.3(10) . . ? O7 C28 C25 113.6(8) . . ? Er1 O1 H11A 109.2 . . ? Er1 O1 H11B 109.2 . . ? H11A O1 H11B 109.5 . . ? Er1 O2 H12A 111.5 . . ? Er1 O2 H12B 110.1 . . ? H12A O2 H12B 107.6 . . ? C1 O3 Er1 163.0(6) . . ? C1 O4 Er1 117.9(5) . 2_865 ? C15 O5 Er1 89.8(4) . . ? C15 O6 Er1 96.5(4) . . ? C28 O7 H5 109.5 . . ? C14 O9 Er1 91.3(5) . 2_775 ? C14 O10 Er1 96.0(5) . 2_775 ? C22 O11 C21 120.3(7) . . ? C8 O12 C5 121.9(6) . . ? O3 Er1 O4 111.5(2) . 2_865 ? O3 Er1 O6 92.9(2) . . ? O4 Er1 O6 143.10(19) 2_865 . ? O3 Er1 O10 79.5(2) . 2_775 ? O4 Er1 O10 136.9(2) 2_865 2_775 ? O6 Er1 O10 72.65(19) . 2_775 ? O3 Er1 O2 151.3(2) . . ? O4 Er1 O2 78.3(2) 2_865 . ? O6 Er1 O2 93.6(2) . . ? O10 Er1 O2 75.84(19) 2_775 . ? O3 Er1 O1 71.8(2) . . ? O4 Er1 O1 78.7(2) 2_865 . ? O6 Er1 O1 83.6(2) . . ? O10 Er1 O1 141.54(19) 2_775 . ? O2 Er1 O1 136.76(18) . . ? O3 Er1 O9 76.6(2) . 2_775 ? O4 Er1 O9 86.93(19) 2_865 2_775 ? O6 Er1 O9 126.66(18) . 2_775 ? O10 Er1 O9 54.06(17) 2_775 2_775 ? O2 Er1 O9 77.07(19) . 2_775 ? O1 Er1 O9 137.18(18) . 2_775 ? O3 Er1 O5 130.4(2) . . ? O4 Er1 O5 89.28(18) 2_865 . ? O6 Er1 O5 54.03(17) . . ? O10 Er1 O5 115.74(18) 2_775 . ? O2 Er1 O5 74.66(19) . . ? O1 Er1 O5 68.95(19) . . ? O9 Er1 O5 151.66(19) 2_775 . ? O3 Er1 C15 110.8(2) . . ? O4 Er1 C15 116.3(2) 2_865 . ? O6 Er1 C15 26.84(18) . . ? O10 Er1 C15 95.8(2) 2_775 . ? O2 Er1 C15 86.3(2) . . ? O1 Er1 C15 72.0(2) . . ? O9 Er1 C15 148.2(2) 2_775 . ? O5 Er1 C15 27.48(18) . . ? O3 Er1 C14 75.2(2) . 2_775 ? O4 Er1 C14 113.4(2) 2_865 2_775 ? O6 Er1 C14 99.0(2) . 2_775 ? O10 Er1 C14 26.48(19) 2_775 2_775 ? O2 Er1 C14 76.2(2) . 2_775 ? O1 Er1 C14 147.0(2) . 2_775 ? O9 Er1 C14 27.65(18) 2_775 2_775 ? O5 Er1 C14 138.1(2) . 2_775 ? C15 Er1 C14 122.0(2) . 2_775 ? 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 O3 C1 C2 C3 7.0(13) . . . . ? O4 C1 C2 C3 -170.0(8) . . . . ? O3 C1 C2 C7 -175.0(8) . . . . ? O4 C1 C2 C7 8.0(12) . . . . ? C7 C2 C3 C4 -4.8(13) . . . . ? C1 C2 C3 C4 173.3(8) . . . . ? C2 C3 C4 C5 0.2(14) . . . . ? C3 C4 C5 C6 3.6(14) . . . . ? C3 C4 C5 O12 179.0(8) . . . . ? C4 C5 C6 C7 -2.7(14) . . . . ? O12 C5 C6 C7 -178.5(8) . . . . ? C5 C6 C7 C2 -1.9(14) . . . . ? C3 C2 C7 C6 5.6(13) . . . . ? C1 C2 C7 C6 -172.5(8) . . . . ? O12 C8 C9 C10 178.6(9) . . . . ? C13 C8 C9 C10 2.7(14) . . . . ? C8 C9 C10 C11 -1.2(15) . . . . ? C9 C10 C11 C12 -0.3(15) . . . . ? C10 C11 C12 C13 0.4(15) . . . . ? C11 C12 C13 C8 1.1(14) . . . . ? C11 C12 C13 C14 -176.6(9) . . . . ? O12 C8 C13 C12 -178.8(8) . . . . ? C9 C8 C13 C12 -2.6(12) . . . . ? O12 C8 C13 C14 -1.2(12) . . . . ? C9 C8 C13 C14 175.0(8) . . . . ? C12 C13 C14 O10 169.3(9) . . . . ? C8 C13 C14 O10 -8.3(13) . . . . ? C12 C13 C14 O9 -14.9(12) . . . . ? C8 C13 C14 O9 167.5(8) . . . . ? C12 C13 C14 Er1 -106(4) . . . 2_775 ? C8 C13 C14 Er1 76(4) . . . 2_775 ? O6 C15 C16 C17 -146.4(9) . . . . ? O5 C15 C16 C17 33.1(13) . . . . ? Er1 C15 C16 C17 -72(3) . . . . ? O6 C15 C16 C21 29.3(13) . . . . ? O5 C15 C16 C21 -151.3(8) . . . . ? Er1 C15 C16 C21 103(3) . . . . ? C21 C16 C17 C18 -1.2(14) . . . . ? C15 C16 C17 C18 174.7(9) . . . . ? C16 C17 C18 C19 -0.7(16) . . . . ? C17 C18 C19 C20 2.9(17) . . . . ? C18 C19 C20 C21 -3.1(17) . . . . ? C19 C20 C21 C16 1.2(16) . . . . ? C19 C20 C21 O11 174.6(9) . . . . ? C17 C16 C21 C20 0.9(14) . . . . ? C15 C16 C21 C20 -174.8(9) . . . . ? C17 C16 C21 O11 -172.9(8) . . . . ? C15 C16 C21 O11 11.4(13) . . . . ? C27 C22 C23 C24 -0.8(15) . . . . ? O11 C22 C23 C24 -174.8(7) . . . . ? C22 C23 C24 C25 0.7(13) . . . . ? C23 C24 C25 C26 0.3(13) . . . . ? C23 C24 C25 C28 177.7(8) . . . . ? C24 C25 C26 C27 -1.1(15) . . . . ? C28 C25 C26 C27 -178.5(9) . . . . ? C23 C22 C27 C26 0.0(16) . . . . ? O11 C22 C27 C26 173.7(8) . . . . ? C25 C26 C27 C22 0.9(16) . . . . ? C26 C25 C28 O8 7.4(15) . . . . ? C24 C25 C28 O8 -170.0(9) . . . . ? C26 C25 C28 O7 -170.6(9) . . . . ? C24 C25 C28 O7 12.0(12) . . . . ? O4 C1 O3 Er1 -120.8(17) . . . . ? C2 C1 O3 Er1 62(2) . . . . ? O3 C1 O4 Er1 2.6(11) . . . 2_865 ? C2 C1 O4 Er1 179.5(6) . . . 2_865 ? O6 C15 O5 Er1 10.9(8) . . . . ? C16 C15 O5 Er1 -168.6(8) . . . . ? O5 C15 O6 Er1 -11.6(8) . . . . ? C16 C15 O6 Er1 167.9(7) . . . . ? O10 C14 O9 Er1 5.3(8) . . . 2_775 ? C13 C14 O9 Er1 -170.7(7) . . . 2_775 ? O9 C14 O10 Er1 -5.5(8) . . . 2_775 ? C13 C14 O10 Er1 170.4(7) . . . 2_775 ? C23 C22 O11 C21 -132.6(9) . . . . ? C27 C22 O11 C21 53.4(13) . . . . ? C20 C21 O11 C22 31.0(14) . . . . ? C16 C21 O11 C22 -155.2(8) . . . . ? C9 C8 O12 C5 20.0(14) . . . . ? C13 C8 O12 C5 -164.0(8) . . . . ? C6 C5 O12 C8 -140.1(9) . . . . ? C4 C5 O12 C8 44.3(13) . . . . ? C1 O3 Er1 O4 125.3(19) . . . 2_865 ? C1 O3 Er1 O6 -82.9(19) . . . . ? C1 O3 Er1 O10 -11.2(19) . . . 2_775 ? C1 O3 Er1 O2 20(2) . . . . ? C1 O3 Er1 O1 -165(2) . . . . ? C1 O3 Er1 O9 44.1(19) . . . 2_775 ? C1 O3 Er1 O5 -126.1(19) . . . . ? C1 O3 Er1 C15 -103.5(19) . . . . ? C1 O3 Er1 C14 15.6(19) . . . 2_775 ? C15 O6 Er1 O3 -133.4(5) . . . . ? C15 O6 Er1 O4 -0.6(7) . . . 2_865 ? C15 O6 Er1 O10 148.6(6) . . . 2_775 ? C15 O6 Er1 O2 74.6(5) . . . . ? C15 O6 Er1 O1 -62.1(5) . . . . ? C15 O6 Er1 O9 151.1(5) . . . 2_775 ? C15 O6 Er1 O5 6.5(5) . . . . ? C15 O6 Er1 C14 151.1(5) . . . 2_775 ? C15 O5 Er1 O3 51.3(6) . . . . ? C15 O5 Er1 O4 169.4(5) . . . 2_865 ? C15 O5 Er1 O6 -6.4(5) . . . . ? C15 O5 Er1 O10 -47.0(5) . . . 2_775 ? C15 O5 Er1 O2 -112.6(5) . . . . ? C15 O5 Er1 O1 91.2(5) . . . . ? C15 O5 Er1 O9 -108.4(5) . . . 2_775 ? C15 O5 Er1 C14 -65.2(6) . . . 2_775 ? O6 C15 Er1 O3 50.9(6) . . . . ? O5 C15 Er1 O3 -140.5(5) . . . . ? C16 C15 Er1 O3 -30(3) . . . . ? O6 C15 Er1 O4 179.6(5) . . . 2_865 ? O5 C15 Er1 O4 -11.8(6) . . . 2_865 ? C16 C15 Er1 O4 99(3) . . . 2_865 ? O5 C15 Er1 O6 168.6(8) . . . . ? C16 C15 Er1 O6 -81(3) . . . . ? O6 C15 Er1 O10 -30.0(5) . . . 2_775 ? O5 C15 Er1 O10 138.5(5) . . . 2_775 ? C16 C15 Er1 O10 -111(3) . . . 2_775 ? O6 C15 Er1 O2 -105.4(5) . . . . ? O5 C15 Er1 O2 63.2(5) . . . . ? C16 C15 Er1 O2 174(3) . . . . ? O6 C15 Er1 O1 112.6(5) . . . . ? O5 C15 Er1 O1 -78.9(5) . . . . ? C16 C15 Er1 O1 32(3) . . . . ? O6 C15 Er1 O9 -47.3(7) . . . 2_775 ? O5 C15 Er1 O9 121.2(5) . . . 2_775 ? C16 C15 Er1 O9 -128(3) . . . 2_775 ? O6 C15 Er1 O5 -168.6(8) . . . . ? C16 C15 Er1 O5 111(3) . . . . ? O6 C15 Er1 C14 -34.2(6) . . . 2_775 ? O5 C15 Er1 C14 134.3(5) . . . 2_775 ? C16 C15 Er1 C14 -115(3) . . . 2_775 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.250 _refine_diff_density_min -0.902 _refine_diff_density_rms 0.187 _database_code_depnum_ccdc_archive 'CCDC 916106'