# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_erhex10a _database_code_depnum_ccdc_archive 'CCDC 898151' #TrackingRef 'compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H16 Er O11' _chemical_formula_weight 467.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.247(2) _cell_length_b 9.437(2) _cell_length_c 9.862(3) _cell_angle_alpha 74.36(2) _cell_angle_beta 63.38(2) _cell_angle_gamma 87.67(2) _cell_volume 737.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 80 _cell_measurement_theta_min 8.4 _cell_measurement_theta_max 12.1 _exptl_crystal_description prismatic _exptl_crystal_colour pink _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 5.740 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.0056 _exptl_absorpt_correction_T_max 0.4129 _exptl_absorpt_process_details ? _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 P4 _diffrn_measurement_method scintillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3062 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2557 _reflns_number_gt 2506 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Due to the presence of pairs of cations (high electron density) near the water molecules, refinement of these protons resulted to deformation of the water geometry. For this reason, we restrained the water geometry near theoretical values by using DFIX and DANG. DFIX 0.83 O2W H2a O2W H2b DANG 1.32 0.08 H2a H2b DFIX 0.83 O3W H3a O3W H3b DANG 1.32 0.08 H3a H3b DFIX 0.83 O4W H4a O4W H4b DANG 1.32 0.08 H4a H4b 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+7.1625P] 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 2557 _refine_ls_number_parameters 208 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.054 _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 Er1 Er 0.56149(4) 0.61995(3) 0.14494(4) 0.01531(19) Uani 1 1 d . . . O1 O 0.5859(7) 0.3556(6) 0.2181(7) 0.0192(12) Uani 1 1 d . . . O2 O 0.4263(7) 0.4472(7) 0.4096(7) 0.0212(13) Uani 1 1 d . . . O3 O 0.3496(7) 0.5042(8) 0.1423(8) 0.0275(14) Uani 1 1 d . . . O4 O 0.1999(8) 0.4055(8) 0.0662(8) 0.0284(15) Uani 1 1 d . . . O5 O 0.3790(8) 0.7553(7) 0.2914(8) 0.0259(14) Uani 1 1 d . . . O6 O 0.2604(8) 0.8906(7) 0.1539(8) 0.0268(14) Uani 1 1 d . . . O1W O 0.5122(8) 0.7869(7) -0.0536(7) 0.0232(13) Uani 1 1 d . . . O2W O 0.7149(9) 0.8490(7) 0.0619(9) 0.0320(15) Uani 1 1 d D . . O3W O 0.7293(8) 0.5961(9) 0.2716(8) 0.0294(15) Uani 1 1 d D . . O4W O 0.8983(11) 0.2505(12) 0.1512(13) 0.057(2) Uani 1 1 d D . . O5W O 1.0193(11) 0.1894(11) -0.1298(12) 0.051(2) Uani 1 1 d . . . C1 C 0.4879(11) 0.3363(10) 0.3651(11) 0.0233(19) Uani 1 1 d . . . C2 C 0.4495(14) 0.1894(10) 0.4798(12) 0.031(2) Uani 1 1 d . . . H2 H 0.3735 0.1806 0.5837 0.037 Uiso 1 1 calc R . . C3 C 0.5152(12) 0.0699(10) 0.4453(11) 0.026(2) Uani 1 1 d . . . H3 H 0.5876 0.0784 0.3403 0.032 Uiso 1 1 calc R . . C4 C 0.2153(11) 0.4597(10) 0.1647(11) 0.0228(18) Uani 1 1 d . . . C5 C 0.0683(11) 0.4597(10) 0.3109(10) 0.0230(18) Uani 1 1 d . . . H5 H -0.0319 0.4298 0.3220 0.028 Uiso 1 1 calc R . . C6 C 0.0733(11) 0.5005(10) 0.4270(11) 0.0213(18) Uani 1 1 d . . . H6 H 0.1734 0.5310 0.4157 0.026 Uiso 1 1 calc R . . C7 C 0.2769(11) 0.8431(10) 0.2793(11) 0.0227(18) Uani 1 1 d . . . C8 C 0.1706(12) 0.8908(10) 0.4211(11) 0.0263(19) Uani 1 1 d . . . H8 H 0.1880 0.8572 0.5098 0.032 Uiso 1 1 calc R . . C9 C 0.0532(12) 0.9774(11) 0.4305(12) 0.028(2) Uani 1 1 d . . . H9 H 0.0374 1.0123 0.3410 0.034 Uiso 1 1 calc R . . H1A H 0.4529 0.8559 -0.0233 0.080 Uiso 1 1 d . . . H1B H 0.5857 0.8030 -0.1630 0.080 Uiso 1 1 d . . . H2A H 0.72(2) 0.918(12) -0.011(14) 0.080 Uiso 1 1 d D . . H2B H 0.778(17) 0.870(17) 0.094(19) 0.080 Uiso 1 1 d D . . H3A H 0.687(17) 0.572(18) 0.370(3) 0.080 Uiso 1 1 d D . . H3B H 0.818(10) 0.639(17) 0.247(17) 0.080 Uiso 1 1 d D . . H4A H 0.807(9) 0.282(17) 0.186(19) 0.080 Uiso 1 1 d D . . H4B H 0.961(15) 0.318(13) 0.074(14) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.0151(3) 0.0159(3) 0.0159(3) -0.00557(17) -0.00733(19) 0.00270(16) O1 0.025(3) 0.015(3) 0.012(3) 0.000(2) -0.004(2) -0.002(2) O2 0.026(3) 0.018(3) 0.021(3) -0.008(2) -0.010(3) 0.002(2) O3 0.012(3) 0.044(4) 0.023(3) -0.008(3) -0.005(2) -0.004(3) O4 0.030(4) 0.038(4) 0.019(3) -0.015(3) -0.009(3) 0.004(3) O5 0.025(3) 0.030(4) 0.033(4) -0.019(3) -0.017(3) 0.018(3) O6 0.030(4) 0.026(3) 0.027(3) -0.011(3) -0.014(3) 0.008(3) O1W 0.027(3) 0.025(3) 0.018(3) -0.006(2) -0.011(3) 0.003(3) O2W 0.038(4) 0.020(3) 0.040(4) 0.002(3) -0.025(3) -0.004(3) O3W 0.027(3) 0.046(4) 0.026(3) -0.015(3) -0.020(3) 0.005(3) O4W 0.035(5) 0.068(7) 0.063(7) -0.024(5) -0.017(5) 0.003(4) O5W 0.047(5) 0.057(6) 0.063(6) -0.015(5) -0.037(5) -0.006(4) C1 0.026(5) 0.027(5) 0.027(5) -0.012(4) -0.019(4) 0.006(4) C2 0.052(6) 0.017(5) 0.024(5) -0.003(4) -0.019(5) 0.003(4) C3 0.036(5) 0.020(5) 0.024(5) -0.005(4) -0.014(4) -0.001(4) C4 0.023(5) 0.026(5) 0.025(5) -0.013(4) -0.013(4) 0.006(4) C5 0.016(4) 0.028(5) 0.017(4) -0.006(4) -0.001(3) -0.007(3) C6 0.016(4) 0.024(5) 0.023(5) -0.009(3) -0.006(4) 0.000(3) C7 0.025(4) 0.022(4) 0.025(5) -0.011(4) -0.012(4) -0.001(4) C8 0.028(5) 0.025(5) 0.024(5) -0.007(4) -0.010(4) 0.005(4) C9 0.030(5) 0.027(5) 0.026(5) -0.009(4) -0.011(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O5 2.281(6) . ? Er1 O3 2.295(7) . ? Er1 O4 2.318(7) 2_665 ? Er1 O1W 2.367(7) . ? Er1 O3W 2.361(7) . ? Er1 O2W 2.369(7) . ? Er1 O1 2.434(6) . ? Er1 O2 2.445(7) . ? Er1 C1 2.834(10) . ? O1 C1 1.285(12) . ? O2 C1 1.260(12) . ? O3 C4 1.230(12) . ? O4 C4 1.274(12) . ? O4 Er1 2.318(7) 2_665 ? O5 C7 1.255(12) . ? O6 C7 1.272(12) . ? O1W H1A 0.86 . ? O1W H1B 0.95 . ? O2W H2A 0.82(2) . ? O2W H2B 0.83(2) . ? O3W H3A 0.83(2) . ? O3W H3B 0.83(2) . ? O4W H4A 0.83(2) . ? O4W H4B 0.83(2) . ? C1 C2 1.470(14) . ? C2 C3 1.313(15) . ? C2 H2 0.9300 . ? C3 C3 1.40(2) 2_656 ? C3 H3 0.9300 . ? C4 C5 1.474(13) . ? C5 C6 1.321(14) . ? C5 H5 0.9300 . ? C6 C6 1.469(18) 2_566 ? C6 H6 0.9300 . ? C7 C8 1.483(14) . ? C8 C9 1.316(15) . ? C8 H8 0.9300 . ? C9 C9 1.45(2) 2_576 ? C9 H9 0.9300 . ? 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 Er1 O3 88.2(3) . . ? O5 Er1 O4 153.1(3) . 2_665 ? O3 Er1 O4 108.3(3) . 2_665 ? O5 Er1 O1W 79.9(2) . . ? O3 Er1 O1W 75.0(3) . . ? O4 Er1 O1W 84.0(2) 2_665 . ? O5 Er1 O3W 96.4(2) . . ? O3 Er1 O3W 143.5(3) . . ? O4 Er1 O3W 82.9(3) 2_665 . ? O1W Er1 O3W 141.5(3) . . ? O5 Er1 O2W 77.1(3) . . ? O3 Er1 O2W 144.5(3) . . ? O4 Er1 O2W 77.3(3) 2_665 . ? O1W Er1 O2W 70.8(2) . . ? O3W Er1 O2W 71.0(3) . . ? O5 Er1 O1 128.6(2) . . ? O3 Er1 O1 73.1(3) . . ? O4 Er1 O1 77.5(2) 2_665 . ? O1W Er1 O1 135.5(2) . . ? O3W Er1 O1 75.9(3) . . ? O2W Er1 O1 140.4(2) . . ? O5 Er1 O2 76.3(2) . . ? O3 Er1 O2 76.5(2) . . ? O4 Er1 O2 127.4(2) 2_665 . ? O1W Er1 O2 143.1(2) . . ? O3W Er1 O2 69.7(2) . . ? O2W Er1 O2 128.9(2) . . ? O1 Er1 O2 53.2(2) . . ? O5 Er1 C1 102.2(3) . . ? O3 Er1 C1 72.8(3) . . ? O4 Er1 C1 102.9(3) 2_665 . ? O1W Er1 C1 147.6(3) . . ? O3W Er1 C1 70.9(3) . . ? O2W Er1 C1 141.5(3) . . ? O1 Er1 C1 26.9(3) . . ? O2 Er1 C1 26.3(3) . . ? C1 O1 Er1 94.2(6) . . ? C1 O2 Er1 94.3(6) . . ? C4 O3 Er1 165.5(7) . . ? C4 O4 Er1 116.3(6) . 2_665 ? C7 O5 Er1 138.1(6) . . ? Er1 O1W H1B 121.00 . . ? H1A O1W H1B 119.00 . . ? Er1 O2W H2A 123(10) . . ? Er1 O2W H2B 127(10) . . ? H2A O2W H2B 110(9) . . ? Er1 O3W H3A 120(10) . . ? Er1 O3W H3B 133(10) . . ? H3A O3W H3B 102(9) . . ? H4A O4W H4B 107(9) . . ? O2 C1 O1 118.3(9) . . ? O2 C1 C2 120.5(9) . . ? O1 C1 C2 121.2(9) . . ? O2 C1 Er1 59.4(5) . . ? O1 C1 Er1 58.9(5) . . ? C2 C1 Er1 179.8(9) . . ? C3 C2 C1 124.4(10) . . ? C3 C2 H2 117.8 . . ? C1 C2 H2 117.8 . . ? C2 C3 C3 125.1(13) . 2_656 ? C2 C3 H3 117.5 . . ? C3 C3 H3 117.5 2_656 . ? O3 C4 O4 121.2(9) . . ? O3 C4 C5 120.8(9) . . ? O4 C4 C5 117.9(9) . . ? C6 C5 C4 122.6(9) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C6 122.5(11) . 2_566 ? C5 C6 H6 118.7 . . ? C6 C6 H6 118.7 2_566 . ? O5 C7 O6 123.6(9) . . ? O5 C7 C8 116.9(9) . . ? O6 C7 C8 119.5(9) . . ? C9 C8 C7 124.7(10) . . ? C9 C8 H8 117.6 . . ? C7 C8 H8 117.6 . . ? C8 C9 C9 125.1(13) . 2_576 ? C8 C9 H9 117.4 . . ? C9 C9 H9 117.4 2_576 . ? 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 Er1 O1 C1 -11.6(6) . . . . ? O3 Er1 O1 C1 -85.1(5) . . . . ? O4 Er1 O1 C1 161.1(6) 2_665 . . . ? O1W Er1 O1 C1 -131.1(5) . . . . ? O3W Er1 O1 C1 75.4(5) . . . . ? O2W Er1 O1 C1 109.5(6) . . . . ? O2 Er1 O1 C1 0.4(5) . . . . ? O5 Er1 O2 C1 170.0(6) . . . . ? O3 Er1 O2 C1 78.5(5) . . . . ? O4 Er1 O2 C1 -24.4(6) 2_665 . . . ? O1W Er1 O2 C1 118.7(6) . . . . ? O3W Er1 O2 C1 -87.7(5) . . . . ? O2W Er1 O2 C1 -129.6(5) . . . . ? O1 Er1 O2 C1 -0.4(5) . . . . ? O5 Er1 O3 C4 -8(3) . . . . ? O4 Er1 O3 C4 -166(3) 2_665 . . . ? O1W Er1 O3 C4 -88(3) . . . . ? O3W Er1 O3 C4 91(3) . . . . ? O2W Er1 O3 C4 -72(3) . . . . ? O1 Er1 O3 C4 124(3) . . . . ? O2 Er1 O3 C4 69(3) . . . . ? C1 Er1 O3 C4 96(3) . . . . ? O3 Er1 O5 C7 -58.5(10) . . . . ? O4 Er1 O5 C7 70.8(12) 2_665 . . . ? O1W Er1 O5 C7 16.6(10) . . . . ? O3W Er1 O5 C7 157.8(10) . . . . ? O2W Er1 O5 C7 89.0(10) . . . . ? O1 Er1 O5 C7 -125.1(10) . . . . ? O2 Er1 O5 C7 -135.0(10) . . . . ? C1 Er1 O5 C7 -130.5(10) . . . . ? Er1 O2 C1 O1 0.7(9) . . . . ? Er1 O2 C1 C2 179.9(8) . . . . ? Er1 O1 C1 O2 -0.7(9) . . . . ? Er1 O1 C1 C2 -179.9(8) . . . . ? O5 Er1 C1 O2 -10.0(6) . . . . ? O3 Er1 C1 O2 -94.2(5) . . . . ? O4 Er1 C1 O2 160.3(5) 2_665 . . . ? O1W Er1 C1 O2 -100.3(6) . . . . ? O3W Er1 C1 O2 82.7(5) . . . . ? O2W Er1 C1 O2 74.5(7) . . . . ? O1 Er1 C1 O2 179.3(9) . . . . ? O5 Er1 C1 O1 170.7(5) . . . . ? O3 Er1 C1 O1 86.5(5) . . . . ? O4 Er1 C1 O1 -18.9(6) 2_665 . . . ? O1W Er1 C1 O1 80.4(7) . . . . ? O3W Er1 C1 O1 -96.6(6) . . . . ? O2W Er1 C1 O1 -104.8(6) . . . . ? O2 Er1 C1 O1 -179.3(9) . . . . ? O2 C1 C2 C3 -175.9(10) . . . . ? O1 C1 C2 C3 3.3(17) . . . . ? C1 C2 C3 C3 177.3(12) . . . 2_656 ? Er1 O3 C4 O4 160(2) . . . . ? Er1 O3 C4 C5 -24(3) . . . . ? Er1 O4 C4 O3 4.4(13) 2_665 . . . ? Er1 O4 C4 C5 -172.2(7) 2_665 . . . ? O3 C4 C5 C6 -3.1(16) . . . . ? O4 C4 C5 C6 173.6(10) . . . . ? C4 C5 C6 C6 -179.6(11) . . . 2_566 ? Er1 O5 C7 O6 -6.3(16) . . . . ? Er1 O5 C7 C8 173.1(7) . . . . ? O5 C7 C8 C9 -177.2(10) . . . . ? O6 C7 C8 C9 2.3(16) . . . . ? C7 C8 C9 C9 178.8(13) . . . 2_576 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.079 _refine_diff_density_min -2.611 _refine_diff_density_rms 0.360 data_yhex10 _database_code_depnum_ccdc_archive 'CCDC 898152' #TrackingRef 'compound 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H16 O11 Y' _chemical_formula_weight 389.13 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2850(10) _cell_length_b 9.4680(10) _cell_length_c 9.8860(10) _cell_angle_alpha 74.440(10) _cell_angle_beta 63.350(10) _cell_angle_gamma 87.800(10) _cell_volume 744.89(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 64 _cell_measurement_theta_min 9.3 _cell_measurement_theta_max 12.2 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 394 _exptl_absorpt_coefficient_mu 3.966 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 P4 _diffrn_measurement_method scintillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3076 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2566 _reflns_number_gt 2301 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Due to the presence of pairs of cations (high electron density) near the water molecules, refinement of these protons resulted to deformation of the water geometry. For this reason, we restrained the water geometry near theoretical values by using DFIX and DANG. DFIX 0.83 O1W H1a O1W H1b DANG 1.32 0.08 H1a H1b DFIX 0.83 O2W H2a O2W H2b DANG 1.32 0.08 H2a H2b DFIX 0.83 O3W H3a O3W H3b DANG 1.32 0.08 H3a H3b DFIX 0.83 O4W H4a O4W H4b DANG 1.32 0.08 H4a H4b DFIX 0.83 O5W H5a O5W H5b DANG 1.32 0.08 H5a H5b 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0944P)^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 2566 _refine_ls_number_parameters 220 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1150 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.030 _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 Y1 Y 0.56128(4) 0.61941(4) 0.14431(4) 0.01784(17) Uani 1 1 d . . . O1 O 0.5860(4) 0.3546(3) 0.2184(3) 0.0249(7) Uani 1 1 d . . . O2 O 0.4263(4) 0.4467(3) 0.4096(3) 0.0231(6) Uani 1 1 d . . . O3 O 0.3487(3) 0.5052(4) 0.1409(4) 0.0293(7) Uani 1 1 d . . . O4 O 0.1962(4) 0.4044(4) 0.0680(4) 0.0306(7) Uani 1 1 d . . . O5 O 0.3773(4) 0.7544(4) 0.2909(4) 0.0291(7) Uani 1 1 d . . . O6 O 0.2582(4) 0.8899(4) 0.1559(4) 0.0305(7) Uani 1 1 d . . . O1W O 0.5114(4) 0.7868(3) -0.0537(4) 0.0276(7) Uani 1 1 d D . . O2W O 0.7161(4) 0.8505(4) 0.0611(4) 0.0356(8) Uani 1 1 d D . . O3W O 0.7291(4) 0.5957(4) 0.2717(4) 0.0289(7) Uani 1 1 d D . . O4W O 0.8989(5) 0.2517(6) 0.1502(6) 0.0612(12) Uani 1 1 d D . . O5W O 1.0216(5) 0.1876(5) -0.1298(5) 0.0557(11) Uani 1 1 d D . . C1 C 0.4890(5) 0.3367(5) 0.3630(5) 0.0228(9) Uani 1 1 d . . . C2 C 0.4510(6) 0.1906(5) 0.4786(5) 0.0315(11) Uani 1 1 d . . . H2 H 0.3760 0.1815 0.5826 0.038 Uiso 1 1 calc R . . C3 C 0.5180(6) 0.0715(5) 0.4419(5) 0.0302(10) Uani 1 1 d . . . H3 H 0.5912 0.0796 0.3376 0.036 Uiso 1 1 calc R . . C4 C 0.2132(5) 0.4574(4) 0.1659(5) 0.0223(9) Uani 1 1 d . . . C5 C 0.0664(5) 0.4596(5) 0.3112(5) 0.0281(10) Uani 1 1 d . . . H5 H -0.0336 0.4317 0.3211 0.034 Uiso 1 1 calc R . . C6 C 0.0705(5) 0.4995(5) 0.4289(5) 0.0246(9) Uani 1 1 d . . . H6 H 0.1707 0.5285 0.4179 0.030 Uiso 1 1 calc R . . C7 C 0.2767(5) 0.8442(5) 0.2788(5) 0.0243(9) Uani 1 1 d . . . C8 C 0.1714(6) 0.8920(5) 0.4212(6) 0.0314(10) Uani 1 1 d . . . H8 H 0.1895 0.8600 0.5093 0.038 Uiso 1 1 calc R . . C9 C 0.0526(6) 0.9781(6) 0.4290(6) 0.0337(11) Uani 1 1 d . . . H9 H 0.0356 1.0120 0.3403 0.040 Uiso 1 1 calc R . . H1A H 0.435(6) 0.829(7) -0.002(7) 0.080 Uiso 1 1 d D . . H1B H 0.503(9) 0.770(8) -0.127(6) 0.080 Uiso 1 1 d D . . H2A H 0.728(9) 0.916(6) -0.019(6) 0.080 Uiso 1 1 d D . . H2B H 0.792(6) 0.872(8) 0.078(8) 0.080 Uiso 1 1 d D . . H3A H 0.681(8) 0.561(8) 0.369(3) 0.080 Uiso 1 1 d D . . H3B H 0.816(5) 0.639(8) 0.247(8) 0.080 Uiso 1 1 d D . . H4A H 0.829(7) 0.307(7) 0.140(10) 0.080 Uiso 1 1 d D . . H4B H 0.975(6) 0.316(6) 0.119(9) 0.080 Uiso 1 1 d D . . H5A H 0.949(6) 0.158(8) -0.145(8) 0.080 Uiso 1 1 d D . . H5B H 0.966(8) 0.206(9) -0.043(5) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0207(2) 0.0170(2) 0.0172(2) -0.00564(15) -0.00938(17) 0.00289(15) O1 0.0344(16) 0.0203(15) 0.0207(15) -0.0067(12) -0.0127(13) 0.0034(12) O2 0.0302(16) 0.0183(15) 0.0205(15) -0.0072(12) -0.0104(13) 0.0036(12) O3 0.0181(15) 0.0412(19) 0.0251(16) -0.0083(14) -0.0071(13) -0.0015(13) O4 0.0325(17) 0.0391(19) 0.0249(16) -0.0190(14) -0.0114(14) 0.0028(14) O5 0.0288(17) 0.0347(18) 0.0289(17) -0.0175(14) -0.0136(14) 0.0140(14) O6 0.0391(18) 0.0306(17) 0.0285(17) -0.0131(13) -0.0190(15) 0.0127(14) O1W 0.0395(18) 0.0260(17) 0.0264(17) -0.0115(13) -0.0207(15) 0.0063(13) O2W 0.045(2) 0.0246(17) 0.042(2) 0.0003(14) -0.0292(17) -0.0030(15) O3W 0.0304(17) 0.0368(19) 0.0230(15) -0.0060(14) -0.0159(14) -0.0016(14) O4W 0.040(2) 0.074(3) 0.079(3) -0.033(3) -0.028(2) 0.009(2) O5W 0.047(2) 0.068(3) 0.058(3) -0.011(2) -0.032(2) -0.015(2) C1 0.026(2) 0.025(2) 0.022(2) -0.0091(17) -0.0143(18) 0.0018(17) C2 0.049(3) 0.017(2) 0.021(2) -0.0004(17) -0.013(2) 0.004(2) C3 0.044(3) 0.019(2) 0.024(2) -0.0027(19) -0.015(2) -0.0017(19) C4 0.026(2) 0.021(2) 0.018(2) -0.0055(16) -0.0088(17) 0.0046(17) C5 0.022(2) 0.039(3) 0.026(2) -0.016(2) -0.0103(19) 0.0041(19) C6 0.022(2) 0.029(2) 0.024(2) -0.0102(17) -0.0105(18) 0.0015(17) C7 0.025(2) 0.024(2) 0.027(2) -0.0116(18) -0.0127(18) 0.0040(17) C8 0.039(3) 0.032(3) 0.031(2) -0.017(2) -0.019(2) 0.012(2) C9 0.037(3) 0.038(3) 0.032(3) -0.020(2) -0.015(2) 0.014(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 Y1 O5 2.293(3) . ? Y1 O3 2.304(3) . ? Y1 O4 2.345(3) 2_665 ? Y1 O3W 2.376(3) . ? Y1 O1W 2.377(3) . ? Y1 O2W 2.396(4) . ? Y1 O1 2.449(3) . ? Y1 O2 2.456(3) . ? Y1 C1 2.832(5) . ? O1 C1 1.269(6) . ? O2 C1 1.267(6) . ? O3 C4 1.246(6) . ? O4 C4 1.272(6) . ? O4 Y1 2.345(3) 2_665 ? O5 C7 1.263(6) . ? O6 C7 1.261(6) . ? O1W H1A 0.83(2) . ? O1W H1B 0.82(2) . ? O2W H2A 0.83(2) . ? O2W H2B 0.83(2) . ? O3W H3A 0.83(2) . ? O3W H3B 0.82(2) . ? O4W H4A 0.84(2) . ? O4W H4B 0.84(2) . ? O5W H5A 0.83(2) . ? O5W H5B 0.84(2) . ? C1 C2 1.474(7) . ? C2 C3 1.324(7) . ? C2 H2 0.9300 . ? C3 C3 1.456(10) 2_656 ? C3 H3 0.9300 . ? C4 C5 1.476(7) . ? C5 C6 1.333(7) . ? C5 H5 0.9300 . ? C6 C6 1.431(10) 2_566 ? C6 H6 0.9300 . ? C7 C8 1.488(7) . ? C8 C9 1.333(8) . ? C8 H8 0.9300 . ? C9 C9 1.465(10) 2_576 ? C9 H9 0.9300 . ? 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 Y1 O3 87.54(13) . . ? O5 Y1 O4 152.88(14) . 2_665 ? O3 Y1 O4 109.13(12) . 2_665 ? O5 Y1 O3W 96.75(13) . . ? O3 Y1 O3W 143.91(13) . . ? O4 Y1 O3W 82.40(12) 2_665 . ? O5 Y1 O1W 79.46(12) . . ? O3 Y1 O1W 74.56(12) . . ? O4 Y1 O1W 84.49(13) 2_665 . ? O3W Y1 O1W 141.50(12) . . ? O5 Y1 O2W 77.31(14) . . ? O3 Y1 O2W 144.13(13) . . ? O4 Y1 O2W 76.82(13) 2_665 . ? O3W Y1 O2W 70.98(12) . . ? O1W Y1 O2W 70.82(12) . . ? O5 Y1 O1 128.49(12) . . ? O3 Y1 O1 73.81(13) . . ? O4 Y1 O1 77.77(12) 2_665 . ? O3W Y1 O1 75.67(12) . . ? O1W Y1 O1 135.90(11) . . ? O2W Y1 O1 140.16(13) . . ? O5 Y1 O2 76.27(12) . . ? O3 Y1 O2 76.91(12) . . ? O4 Y1 O2 127.39(12) 2_665 . ? O3W Y1 O2 69.49(12) . . ? O1W Y1 O2 143.02(12) . . ? O2W Y1 O2 128.70(12) . . ? O1 Y1 O2 53.08(11) . . ? O5 Y1 C1 102.36(13) . . ? O3 Y1 C1 73.35(13) . . ? O4 Y1 C1 102.87(13) 2_665 . ? O3W Y1 C1 70.73(13) . . ? O1W Y1 C1 147.73(13) . . ? O2W Y1 C1 141.37(13) . . ? O1 Y1 C1 26.56(13) . . ? O2 Y1 C1 26.52(12) . . ? C1 O1 Y1 93.8(3) . . ? C1 O2 Y1 93.5(3) . . ? C4 O3 Y1 165.7(3) . . ? C4 O4 Y1 115.0(3) . 2_665 ? C7 O5 Y1 138.9(3) . . ? Y1 O1W H1A 103(5) . . ? Y1 O1W H1B 128(5) . . ? H1A O1W H1B 113(6) . . ? Y1 O2W H2A 122(5) . . ? Y1 O2W H2B 130(5) . . ? H2A O2W H2B 104(6) . . ? Y1 O3W H3A 115(5) . . ? Y1 O3W H3B 132(5) . . ? H3A O3W H3B 109(6) . . ? H4A O4W H4B 99(6) . . ? H5A O5W H5B 100(6) . . ? O2 C1 O1 119.6(4) . . ? O2 C1 C2 119.3(4) . . ? O1 C1 C2 121.1(4) . . ? O2 C1 Y1 59.9(2) . . ? O1 C1 Y1 59.6(2) . . ? C2 C1 Y1 179.2(3) . . ? C3 C2 C1 123.4(5) . . ? C3 C2 H2 118.3 . . ? C1 C2 H2 118.3 . . ? C2 C3 C3 122.8(6) . 2_656 ? C2 C3 H3 118.6 . . ? C3 C3 H3 118.6 2_656 . ? O3 C4 O4 121.4(4) . . ? O3 C4 C5 121.1(4) . . ? O4 C4 C5 117.5(4) . . ? C6 C5 C4 123.0(5) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C5 C6 C6 123.6(6) . 2_566 ? C5 C6 H6 118.2 . . ? C6 C6 H6 118.2 2_566 . ? O5 C7 O6 123.5(4) . . ? O5 C7 C8 116.9(4) . . ? O6 C7 C8 119.6(4) . . ? C9 C8 C7 123.4(5) . . ? C9 C8 H8 118.3 . . ? C7 C8 H8 118.3 . . ? C8 C9 C9 123.0(7) . 2_576 ? C8 C9 H9 118.5 . . ? C9 C9 H9 118.5 2_576 . ? 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 Y1 O1 C1 -11.8(3) . . . . ? O3 Y1 O1 C1 -85.0(3) . . . . ? O4 Y1 O1 C1 160.6(3) 2_665 . . . ? O3W Y1 O1 C1 75.5(3) . . . . ? O1W Y1 O1 C1 -130.8(3) . . . . ? O2W Y1 O1 C1 109.2(3) . . . . ? O2 Y1 O1 C1 0.6(3) . . . . ? O5 Y1 O2 C1 169.5(3) . . . . ? O3 Y1 O2 C1 78.9(3) . . . . ? O4 Y1 O2 C1 -25.4(3) 2_665 . . . ? O3W Y1 O2 C1 -87.7(3) . . . . ? O1W Y1 O2 C1 119.1(3) . . . . ? O2W Y1 O2 C1 -129.5(3) . . . . ? O1 Y1 O2 C1 -0.6(3) . . . . ? O5 Y1 O3 C4 -14.7(13) . . . . ? O4 Y1 O3 C4 -172.9(13) 2_665 . . . ? O3W Y1 O3 C4 83.4(14) . . . . ? O1W Y1 O3 C4 -94.5(13) . . . . ? O2W Y1 O3 C4 -79.0(14) . . . . ? O1 Y1 O3 C4 116.7(14) . . . . ? O2 Y1 O3 C4 61.7(13) . . . . ? C1 Y1 O3 C4 89.0(13) . . . . ? O3 Y1 O5 C7 -60.0(5) . . . . ? O4 Y1 O5 C7 69.4(6) 2_665 . . . ? O3W Y1 O5 C7 155.9(5) . . . . ? O1W Y1 O5 C7 14.7(5) . . . . ? O2W Y1 O5 C7 87.2(5) . . . . ? O1 Y1 O5 C7 -127.0(5) . . . . ? O2 Y1 O5 C7 -137.2(5) . . . . ? C1 Y1 O5 C7 -132.4(5) . . . . ? Y1 O2 C1 O1 1.0(4) . . . . ? Y1 O2 C1 C2 179.6(4) . . . . ? Y1 O1 C1 O2 -1.0(5) . . . . ? Y1 O1 C1 C2 -179.6(4) . . . . ? O5 Y1 C1 O2 -10.4(3) . . . . ? O3 Y1 C1 O2 -94.0(3) . . . . ? O4 Y1 C1 O2 159.6(3) 2_665 . . . ? O3W Y1 C1 O2 82.5(3) . . . . ? O1W Y1 C1 O2 -100.2(3) . . . . ? O2W Y1 C1 O2 74.7(3) . . . . ? O1 Y1 C1 O2 179.0(5) . . . . ? O5 Y1 C1 O1 170.6(3) . . . . ? O3 Y1 C1 O1 87.0(3) . . . . ? O4 Y1 C1 O1 -19.4(3) 2_665 . . . ? O3W Y1 C1 O1 -96.5(3) . . . . ? O1W Y1 C1 O1 80.8(4) . . . . ? O2W Y1 C1 O1 -104.3(3) . . . . ? O2 Y1 C1 O1 -179.0(5) . . . . ? O2 C1 C2 C3 -176.0(5) . . . . ? O1 C1 C2 C3 2.5(9) . . . . ? C1 C2 C3 C3 178.6(6) . . . 2_656 ? Y1 O3 C4 O4 165.0(11) . . . . ? Y1 O3 C4 C5 -15.4(16) . . . . ? Y1 O4 C4 O3 6.3(6) 2_665 . . . ? Y1 O4 C4 C5 -173.3(3) 2_665 . . . ? O3 C4 C5 C6 -6.0(8) . . . . ? O4 C4 C5 C6 173.6(5) . . . . ? C4 C5 C6 C6 -179.2(6) . . . 2_566 ? Y1 O5 C7 O6 -3.0(8) . . . . ? Y1 O5 C7 C8 174.5(3) . . . . ? O5 C7 C8 C9 -175.2(5) . . . . ? O6 C7 C8 C9 2.3(8) . . . . ? C7 C8 C9 C9 178.6(6) . . . 2_576 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.272 _refine_diff_density_min -2.026 _refine_diff_density_rms 0.139 data_erhex4 _database_code_depnum_ccdc_archive 'CCDC 898153' #TrackingRef 'compound 5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H28 Er2 O20' _chemical_formula_weight 898.92 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6770(10) _cell_length_b 8.0180(10) _cell_length_c 22.389(2) _cell_angle_alpha 94.550(10) _cell_angle_beta 93.330(10) _cell_angle_gamma 101.860(10) _cell_volume 1340.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 66 _cell_measurement_theta_min 9.3 _cell_measurement_theta_max 12.3 _exptl_crystal_description prismatic _exptl_crystal_colour pink _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 6.307 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 P4 _diffrn_measurement_method scintillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5883 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4730 _reflns_number_gt 4339 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Due to the presence of pairs of cations (high electron density) near the water molecules, refinement of these protons resulted to deformation of the water geometry. For this reason, we restrained the water geometry near theoretical values by using DFIX and DANG. DFIX 0.83 O1W H1a O1W H1b DANG 1.32 0.08 H1a H1b DFIX 0.83 O2W H2a O2W H2b DANG 1.32 0.08 H2a H2b DFIX 0.83 O3W H3a O3W H3b DANG 1.32 0.08 H3a H3b DFIX 0.83 O4W H4a O4W H4b DANG 1.32 0.08 H4a H4b DFIX 0.83 O5W H5a O5W H5b DANG 1.32 0.08 H5a H5b DFIX 0.83 O6W H6a O6W H6b DANG 1.32 0.08 H6a H6b DFIX 0.83 O7W H7a O7W H7b DANG 1.32 0.08 H7a H7b DFIX 0.83 O8W H8a O8W H8b DANG 1.32 0.08 H8a H8b 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+2.4673P] 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 4730 _refine_ls_number_parameters 409 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.1000 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.77890(3) 0.23681(3) 0.052493(10) 0.01666(11) Uani 1 1 d . . . Er2 Er 1.09224(3) 0.18393(3) 0.445775(10) 0.01612(11) Uani 1 1 d . . . O1 O 0.9516(6) 0.1812(6) -0.03145(19) 0.0244(10) Uani 1 1 d . . . O2 O 0.6643(6) 0.1506(6) -0.05132(19) 0.0275(10) Uani 1 1 d . . . O3 O 0.7828(6) -0.0786(5) -0.36191(18) 0.0236(9) Uani 1 1 d . . . O4 O 0.4901(6) -0.1074(8) -0.3800(2) 0.0475(15) Uani 1 1 d . . . O5 O 1.0607(6) 0.2870(6) 0.08894(19) 0.0279(10) Uani 1 1 d . . . O6 O 1.3141(6) 0.4783(6) 0.10327(19) 0.0293(10) Uani 1 1 d . . . O7 O 1.1963(6) 0.4366(5) 0.41499(19) 0.0302(10) Uani 1 1 d . . . O8 O 1.3521(7) 0.7024(6) 0.4356(2) 0.0353(11) Uani 1 1 d . . . O9 O 0.7762(6) 0.4474(5) 0.13466(18) 0.0273(10) Uani 1 1 d . . . O10 O 0.7158(6) 0.1796(5) 0.15351(18) 0.0276(10) Uani 1 1 d . . . O11 O 0.8201(6) 0.6362(5) 0.45540(19) 0.0257(10) Uani 1 1 d . . . O12 O 0.9734(6) 0.8953(5) 0.45169(18) 0.0239(9) Uani 1 1 d . . . O1W O 0.7555(6) -0.0597(5) 0.0500(2) 0.0233(9) Uani 1 1 d D . . O2W O 0.4789(6) 0.2403(6) 0.0478(2) 0.0299(10) Uani 1 1 d D . . O3W O 0.7976(7) 0.4933(5) 0.0110(2) 0.0274(10) Uani 1 1 d D . . O4W O 1.3643(7) 0.1388(7) 0.4825(2) 0.0372(12) Uani 1 1 d D . . O5W O 0.8707(6) 0.1312(7) 0.3630(2) 0.0309(10) Uani 1 1 d D . . O6W O 0.8461(6) 0.3017(6) 0.46868(19) 0.0248(9) Uani 1 1 d D . . O7W O 0.6324(6) -0.2658(6) 0.1345(2) 0.0328(10) Uani 1 1 d D . . O8W O 0.8112(8) -0.0325(7) 0.2394(2) 0.0403(12) Uani 1 1 d D . . C1 C 0.8142(8) 0.1461(7) -0.0697(3) 0.0190(12) Uani 1 1 d . . . C2 C 0.8427(9) 0.1032(9) -0.1332(3) 0.0290(14) Uani 1 1 d . . . H2 H 0.9584 0.1026 -0.1432 0.035 Uiso 1 1 calc R . . C3 C 0.7121(8) 0.0652(8) -0.1770(3) 0.0235(13) Uani 1 1 d . . . H3 H 0.5966 0.0677 -0.1671 0.028 Uiso 1 1 calc R . . C4 C 0.7391(8) 0.0205(8) -0.2392(3) 0.0252(13) Uani 1 1 d . . . H4 H 0.8540 0.0158 -0.2492 0.030 Uiso 1 1 calc R . . C5 C 0.6096(8) -0.0138(8) -0.2821(3) 0.0239(13) Uani 1 1 d . . . H5 H 0.4968 -0.0022 -0.2718 0.029 Uiso 1 1 calc R . . C6 C 0.6290(8) -0.0701(8) -0.3462(3) 0.0223(12) Uani 1 1 d . . . C7 C 1.1872(8) 0.3787(8) 0.1239(3) 0.0234(13) Uani 1 1 d . . . C8 C 1.1793(8) 0.3647(8) 0.1886(3) 0.0266(13) Uani 1 1 d . . . H8 H 1.0957 0.2751 0.2008 0.032 Uiso 1 1 calc R . . C9 C 1.2826(9) 0.4704(8) 0.2308(3) 0.0278(13) Uani 1 1 d . . . H9 H 1.3739 0.5541 0.2192 0.033 Uiso 1 1 calc R . . C10 C 1.2599(9) 0.4614(8) 0.2941(3) 0.0286(14) Uani 1 1 d . . . H10 H 1.1813 0.3663 0.3051 0.034 Uiso 1 1 calc R . . C11 C 1.3416(9) 0.5773(8) 0.3379(3) 0.0273(13) Uani 1 1 d . . . H11 H 1.4309 0.6664 0.3284 0.033 Uiso 1 1 calc R . . C12 C 1.2967(8) 0.5709(7) 0.4010(3) 0.0220(12) Uani 1 1 d . . . C13 C 0.7413(8) 0.3375(8) 0.1717(3) 0.0221(12) Uani 1 1 d . . . C14 C 0.7286(9) 0.3860(8) 0.2362(3) 0.0275(14) Uani 1 1 d . . . H14 H 0.6543 0.3097 0.2576 0.033 Uiso 1 1 calc R . . C15 C 0.8173(9) 0.5324(7) 0.2652(3) 0.0238(13) Uani 1 1 d . . . H15 H 0.8853 0.6125 0.2434 0.029 Uiso 1 1 calc R . . C16 C 0.8130(9) 0.5731(8) 0.3293(3) 0.0252(13) Uani 1 1 d . . . H16 H 0.7406 0.4948 0.3506 0.030 Uiso 1 1 calc R . . C17 C 0.9080(9) 0.7179(8) 0.3597(3) 0.0260(13) Uani 1 1 d . . . H17 H 0.9797 0.7991 0.3392 0.031 Uiso 1 1 calc R . . C18 C 0.8991(8) 0.7487(7) 0.4254(2) 0.0192(12) Uani 1 1 d . . . H8A H 0.788(14) 0.029(10) 0.213(3) 0.080 Uiso 1 1 d D . . H8B H 0.762(14) -0.126(6) 0.221(4) 0.080 Uiso 1 1 d D . . H7A H 0.671(12) -0.349(8) 0.144(4) 0.080 Uiso 1 1 d D . . H7B H 0.533(7) -0.314(11) 0.118(4) 0.080 Uiso 1 1 d D . . H6A H 0.798(13) 0.278(12) 0.500(3) 0.080 Uiso 1 1 d D . . H6B H 0.855(15) 0.405(4) 0.465(4) 0.080 Uiso 1 1 d D . . H5A H 0.852(13) 0.083(12) 0.3282(19) 0.080 Uiso 1 1 d D . . H5B H 0.768(6) 0.129(14) 0.373(4) 0.080 Uiso 1 1 d D . . H4A H 1.424(11) 0.162(13) 0.516(2) 0.080 Uiso 1 1 d D . . H4B H 1.429(12) 0.197(12) 0.459(4) 0.080 Uiso 1 1 d D . . H3A H 0.764(14) 0.509(12) -0.0240(19) 0.080 Uiso 1 1 d D . . H3B H 0.843(14) 0.588(6) 0.028(4) 0.080 Uiso 1 1 d D . . H2A H 0.411(12) 0.192(11) 0.019(3) 0.080 Uiso 1 1 d D . . H2B H 0.471(14) 0.174(10) 0.074(3) 0.080 Uiso 1 1 d D . . H1A H 0.696(12) -0.116(11) 0.075(4) 0.080 Uiso 1 1 d D . . H1B H 0.852(7) -0.089(13) 0.047(5) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01802(17) 0.01865(16) 0.01362(16) -0.00198(10) 0.00178(11) 0.00572(11) Er2 0.01714(16) 0.01790(16) 0.01328(16) -0.00125(10) 0.00294(11) 0.00412(11) O1 0.020(2) 0.032(2) 0.022(2) -0.0052(18) 0.0001(17) 0.0114(18) O2 0.020(2) 0.041(3) 0.023(2) -0.0029(18) 0.0032(17) 0.0107(19) O3 0.019(2) 0.033(2) 0.019(2) -0.0029(17) 0.0032(17) 0.0085(18) O4 0.019(2) 0.094(4) 0.025(2) -0.017(3) 0.001(2) 0.009(3) O5 0.021(2) 0.039(2) 0.021(2) -0.0024(19) -0.0005(18) 0.0023(19) O6 0.027(2) 0.034(2) 0.023(2) 0.0011(18) 0.0057(18) -0.0024(19) O7 0.040(3) 0.023(2) 0.025(2) 0.0019(17) 0.011(2) -0.002(2) O8 0.040(3) 0.035(3) 0.026(2) -0.006(2) 0.007(2) -0.002(2) O9 0.039(3) 0.023(2) 0.020(2) -0.0009(17) 0.0029(19) 0.0080(19) O10 0.039(3) 0.022(2) 0.019(2) -0.0044(17) 0.0043(19) 0.0031(19) O11 0.036(3) 0.020(2) 0.020(2) -0.0016(17) 0.0029(19) 0.0048(19) O12 0.034(2) 0.020(2) 0.016(2) -0.0012(16) 0.0034(18) 0.0010(18) O1W 0.022(2) 0.022(2) 0.028(2) -0.0003(17) 0.0070(18) 0.0093(18) O2W 0.015(2) 0.037(3) 0.033(3) -0.012(2) -0.0005(19) 0.0025(19) O3W 0.035(3) 0.024(2) 0.022(2) 0.0029(17) 0.0002(19) 0.0043(19) O4W 0.028(3) 0.065(4) 0.019(2) -0.010(2) -0.0052(19) 0.018(2) O5W 0.023(2) 0.050(3) 0.021(2) -0.006(2) -0.0014(19) 0.017(2) O6W 0.023(2) 0.030(2) 0.025(2) -0.0009(18) 0.0082(18) 0.0145(19) O7W 0.029(2) 0.025(2) 0.044(3) 0.003(2) 0.004(2) 0.0052(19) O8W 0.044(3) 0.046(3) 0.034(3) 0.003(2) 0.000(2) 0.018(3) C1 0.019(3) 0.024(3) 0.015(3) -0.003(2) 0.002(2) 0.009(2) C2 0.020(3) 0.045(4) 0.023(3) -0.007(3) 0.005(3) 0.009(3) C3 0.019(3) 0.029(3) 0.023(3) -0.002(2) 0.004(2) 0.009(2) C4 0.022(3) 0.031(3) 0.025(3) 0.001(3) 0.005(3) 0.010(3) C5 0.014(3) 0.033(3) 0.025(3) -0.003(2) 0.006(2) 0.005(2) C6 0.020(3) 0.029(3) 0.018(3) -0.001(2) 0.002(2) 0.006(2) C7 0.020(3) 0.028(3) 0.023(3) -0.005(2) -0.002(2) 0.011(2) C8 0.024(3) 0.032(3) 0.023(3) 0.004(3) 0.004(3) 0.005(3) C9 0.024(3) 0.034(3) 0.022(3) 0.000(3) 0.003(3) 0.001(3) C10 0.026(3) 0.033(3) 0.027(3) 0.005(3) 0.007(3) 0.005(3) C11 0.026(3) 0.025(3) 0.031(3) 0.007(3) 0.008(3) 0.004(3) C12 0.025(3) 0.022(3) 0.019(3) 0.000(2) 0.001(2) 0.006(2) C13 0.022(3) 0.024(3) 0.019(3) -0.003(2) 0.003(2) 0.004(2) C14 0.034(4) 0.026(3) 0.022(3) 0.000(2) 0.006(3) 0.006(3) C15 0.033(3) 0.020(3) 0.018(3) -0.001(2) 0.002(2) 0.006(3) C16 0.032(3) 0.025(3) 0.019(3) -0.002(2) 0.004(3) 0.007(3) C17 0.034(4) 0.021(3) 0.022(3) -0.001(2) 0.005(3) 0.004(3) C18 0.023(3) 0.020(3) 0.014(3) -0.003(2) -0.002(2) 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 Er1 O5 2.212(5) . ? Er1 O3W 2.304(5) . ? Er1 O2W 2.306(5) . ? Er1 O1W 2.343(4) . ? Er1 O10 2.400(5) . ? Er1 O9 2.400(5) . ? Er1 O1 2.426(5) . ? Er1 O2 2.431(5) . ? Er1 C13 2.775(6) . ? Er1 C1 2.817(6) . ? Er1 H2B 2.40(11) . ? Er2 O7 2.200(5) . ? Er2 O4W 2.308(5) . ? Er2 O12 2.324(4) 1_545 ? Er2 O3 2.335(4) 2_755 ? Er2 O6W 2.345(4) . ? Er2 O5W 2.392(5) . ? Er2 O12 2.482(4) 2_766 ? Er2 O11 2.520(4) 2_766 ? Er2 C18 2.886(6) 2_766 ? O1 C1 1.288(8) . ? O2 C1 1.250(8) . ? O3 C6 1.265(8) . ? O3 Er2 2.334(4) 2_755 ? O4 C6 1.240(9) . ? O5 C7 1.274(8) . ? O6 C7 1.262(8) . ? O7 C12 1.261(8) . ? O8 C12 1.241(8) . ? O9 C13 1.258(8) . ? O10 C13 1.270(8) . ? O11 C18 1.246(8) . ? O11 Er2 2.520(4) 2_766 ? O12 C18 1.276(8) . ? O12 Er2 2.324(4) 1_565 ? O12 Er2 2.483(4) 2_766 ? O1W H1A 0.84(2) . ? O1W H1B 0.83(2) . ? O2W H2A 0.83(2) . ? O2W H2B 0.82(2) . ? O3W H3A 0.84(2) . ? O3W H3B 0.82(2) . ? O4W H4A 0.83(2) . ? O4W H4B 0.84(2) . ? O5W H5A 0.83(2) . ? O5W H5B 0.83(2) . ? O6W H6A 0.82(2) . ? O6W H6B 0.83(2) . ? O7W H7A 0.82(2) . ? O7W H7B 0.83(2) . ? O8W H8A 0.83(2) . ? O8W H8B 0.83(2) . ? C1 C2 1.475(9) . ? C2 C3 1.332(10) . ? C2 H2 0.9300 . ? C3 C4 1.448(9) . ? C3 H3 0.9300 . ? C4 C5 1.313(9) . ? C4 H4 0.9300 . ? C5 C6 1.496(9) . ? C5 H5 0.9300 . ? C7 C8 1.465(9) . ? C8 C9 1.323(10) . ? C8 H8 0.9300 . ? C9 C10 1.442(9) . ? C9 H9 0.9300 . ? C10 C11 1.328(10) . ? C10 H10 0.9300 . ? C11 C12 1.476(9) . ? C11 H11 0.9300 . ? C13 C14 1.480(9) . ? C14 C15 1.328(10) . ? C14 H14 0.9300 . ? C15 C16 1.449(9) . ? C15 H15 0.9300 . ? C16 C17 1.346(9) . ? C16 H16 0.9300 . ? C17 C18 1.481(9) . ? C17 H17 0.9300 . ? C18 Er2 2.887(6) 2_766 ? 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 Er1 O3W 96.07(18) . . ? O5 Er1 O2W 158.81(17) . . ? O3W Er1 O2W 82.51(18) . . ? O5 Er1 O1W 91.62(17) . . ? O3W Er1 O1W 155.01(16) . . ? O2W Er1 O1W 98.51(17) . . ? O5 Er1 O10 84.02(18) . . ? O3W Er1 O10 127.16(16) . . ? O2W Er1 O10 80.19(18) . . ? O1W Er1 O10 77.21(16) . . ? O5 Er1 O9 79.27(18) . . ? O3W Er1 O9 73.95(16) . . ? O2W Er1 O9 80.04(17) . . ? O1W Er1 O9 130.96(16) . . ? O10 Er1 O9 54.06(16) . . ? O5 Er1 O1 73.71(16) . . ? O3W Er1 O1 81.45(17) . . ? O2W Er1 O1 126.54(16) . . ? O1W Er1 O1 77.97(16) . . ? O10 Er1 O1 145.92(16) . . ? O9 Er1 O1 141.00(16) . . ? O5 Er1 O2 127.10(16) . . ? O3W Er1 O2 76.56(17) . . ? O2W Er1 O2 73.30(16) . . ? O1W Er1 O2 79.84(17) . . ? O10 Er1 O2 141.65(16) . . ? O9 Er1 O2 142.32(16) . . ? O1 Er1 O2 53.42(15) . . ? O5 Er1 C13 79.84(18) . . ? O3W Er1 C13 100.58(18) . . ? O2W Er1 C13 79.66(18) . . ? O1W Er1 C13 104.17(18) . . ? O10 Er1 C13 27.19(17) . . ? O9 Er1 C13 26.90(18) . . ? O1 Er1 C13 153.52(17) . . ? O2 Er1 C13 152.96(18) . . ? O5 Er1 C1 100.84(18) . . ? O3W Er1 C1 77.37(18) . . ? O2W Er1 C1 99.46(18) . . ? O1W Er1 C1 77.84(17) . . ? O10 Er1 C1 154.70(17) . . ? O9 Er1 C1 151.15(17) . . ? O1 Er1 C1 27.15(17) . . ? O2 Er1 C1 26.27(17) . . ? C13 Er1 C1 177.89(18) . . ? O5 Er1 H2B 146.5(15) . . ? O3W Er1 H2B 101.1(13) . . ? O2W Er1 H2B 20.1(9) . . ? O1W Er1 H2B 85(2) . . ? O10 Er1 H2B 62.7(14) . . ? O9 Er1 H2B 78(2) . . ? O1 Er1 H2B 137(2) . . ? O2 Er1 H2B 85(2) . . ? C13 Er1 H2B 69(2) . . ? C1 Er1 H2B 111(2) . . ? O7 Er2 O4W 96.2(2) . . ? O7 Er2 O12 165.09(17) . 1_545 ? O4W Er2 O12 88.4(2) . 1_545 ? O7 Er2 O3 84.74(17) . 2_755 ? O4W Er2 O3 75.15(17) . 2_755 ? O12 Er2 O3 82.75(16) 1_545 2_755 ? O7 Er2 O6W 83.85(18) . . ? O4W Er2 O6W 144.97(17) . . ? O12 Er2 O6W 100.46(17) 1_545 . ? O3 Er2 O6W 139.27(16) 2_755 . ? O7 Er2 O5W 88.54(19) . . ? O4W Er2 O5W 146.21(17) . . ? O12 Er2 O5W 79.90(18) 1_545 . ? O3 Er2 O5W 72.00(16) 2_755 . ? O6W Er2 O5W 68.75(16) . . ? O7 Er2 O12 129.71(16) . 2_766 ? O4W Er2 O12 78.36(18) . 2_766 ? O12 Er2 O12 65.09(17) 1_545 2_766 ? O3 Er2 O12 138.54(16) 2_755 2_766 ? O6W Er2 O12 75.06(16) . 2_766 ? O5W Er2 O12 123.09(17) . 2_766 ? O7 Er2 O11 78.92(16) . 2_766 ? O4W Er2 O11 71.92(17) . 2_766 ? O12 Er2 O11 115.98(15) 1_545 2_766 ? O3 Er2 O11 141.14(16) 2_755 2_766 ? O6W Er2 O11 73.76(17) . 2_766 ? O5W Er2 O11 141.49(17) . 2_766 ? O12 Er2 O11 51.61(15) 2_766 2_766 ? O7 Er2 C18 103.87(18) . 2_766 ? O4W Er2 C18 74.46(18) . 2_766 ? O12 Er2 C18 91.02(16) 1_545 2_766 ? O3 Er2 C18 149.12(17) 2_755 2_766 ? O6W Er2 C18 71.59(17) . 2_766 ? O5W Er2 C18 136.72(18) . 2_766 ? O12 Er2 C18 26.14(16) 2_766 2_766 ? O11 Er2 C18 25.51(16) 2_766 2_766 ? C1 O1 Er1 93.6(4) . . ? C1 O2 Er1 94.4(4) . . ? C6 O3 Er2 137.7(4) . 2_755 ? C7 O5 Er1 148.8(4) . . ? C12 O7 Er2 164.2(5) . . ? C13 O9 Er1 93.4(4) . . ? C13 O10 Er1 93.1(4) . . ? C18 O11 Er2 93.9(4) . 2_766 ? C18 O12 Er2 149.2(4) . 1_565 ? C18 O12 Er2 94.9(4) . 2_766 ? Er2 O12 Er2 114.91(17) 1_565 2_766 ? Er1 O1W H1A 120(7) . . ? Er1 O1W H1B 113(7) . . ? H1A O1W H1B 111(8) . . ? Er1 O2W H2A 121(8) . . ? Er1 O2W H2B 86(8) . . ? H2A O2W H2B 108(7) . . ? Er1 O3W H3A 128(7) . . ? Er1 O3W H3B 125(7) . . ? H3A O3W H3B 107(7) . . ? Er2 O4W H4A 135(7) . . ? Er2 O4W H4B 98(7) . . ? H4A O4W H4B 103(7) . . ? Er2 O5W H5A 140(7) . . ? Er2 O5W H5B 114(7) . . ? H5A O5W H5B 101(7) . . ? Er2 O6W H6A 119(7) . . ? Er2 O6W H6B 117(8) . . ? H6A O6W H6B 109(7) . . ? H7A O7W H7B 100(7) . . ? H8A O8W H8B 98(7) . . ? O2 C1 O1 118.6(6) . . ? O2 C1 C2 123.4(6) . . ? O1 C1 C2 117.9(6) . . ? O2 C1 Er1 59.4(3) . . ? O1 C1 Er1 59.3(3) . . ? C2 C1 Er1 177.0(5) . . ? C3 C2 C1 123.7(6) . . ? C3 C2 H2 118.1 . . ? C1 C2 H2 118.1 . . ? C2 C3 C4 123.9(6) . . ? C2 C3 H3 118.1 . . ? C4 C3 H3 118.1 . . ? C5 C4 C3 123.2(6) . . ? C5 C4 H4 118.4 . . ? C3 C4 H4 118.4 . . ? C4 C5 C6 125.2(6) . . ? C4 C5 H5 117.4 . . ? C6 C5 H5 117.4 . . ? O4 C6 O3 124.9(6) . . ? O4 C6 C5 116.5(6) . . ? O3 C6 C5 118.5(6) . . ? O6 C7 O5 120.8(6) . . ? O6 C7 C8 121.5(6) . . ? O5 C7 C8 117.7(6) . . ? C9 C8 C7 124.7(7) . . ? C9 C8 H8 117.7 . . ? C7 C8 H8 117.7 . . ? C8 C9 C10 122.9(7) . . ? C8 C9 H9 118.5 . . ? C10 C9 H9 118.5 . . ? C11 C10 C9 125.6(7) . . ? C11 C10 H10 117.2 . . ? C9 C10 H10 117.2 . . ? C10 C11 C12 122.9(6) . . ? C10 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? O8 C12 O7 124.8(6) . . ? O8 C12 C11 117.2(6) . . ? O7 C12 C11 117.8(6) . . ? O9 C13 O10 119.4(6) . . ? O9 C13 C14 122.0(6) . . ? O10 C13 C14 118.6(6) . . ? O9 C13 Er1 59.7(3) . . ? O10 C13 Er1 59.7(3) . . ? C14 C13 Er1 176.9(5) . . ? C15 C14 C13 123.7(7) . . ? C15 C14 H14 118.1 . . ? C13 C14 H14 118.1 . . ? C14 C15 C16 123.0(7) . . ? C14 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C17 C16 C15 123.6(7) . . ? C17 C16 H16 118.2 . . ? C15 C16 H16 118.2 . . ? C16 C17 C18 120.4(6) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? O11 C18 O12 119.4(6) . . ? O11 C18 C17 121.8(6) . . ? O12 C18 C17 118.8(6) . . ? O11 C18 Er2 60.6(3) . 2_766 ? O12 C18 Er2 59.0(3) . 2_766 ? C17 C18 Er2 176.1(5) . 2_766 ? 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 Er1 O1 C1 -177.9(4) . . . . ? O3W Er1 O1 C1 -79.0(4) . . . . ? O2W Er1 O1 C1 -5.0(4) . . . . ? O1W Er1 O1 C1 86.8(4) . . . . ? O10 Er1 O1 C1 130.8(4) . . . . ? O9 Er1 O1 C1 -129.9(4) . . . . ? O2 Er1 O1 C1 0.6(4) . . . . ? C13 Er1 O1 C1 -175.6(4) . . . . ? O5 Er1 O2 C1 1.2(5) . . . . ? O3W Er1 O2 C1 88.7(4) . . . . ? O2W Er1 O2 C1 174.7(4) . . . . ? O1W Er1 O2 C1 -83.1(4) . . . . ? O10 Er1 O2 C1 -137.0(4) . . . . ? O9 Er1 O2 C1 127.9(4) . . . . ? O1 Er1 O2 C1 -0.6(4) . . . . ? C13 Er1 O2 C1 175.6(4) . . . . ? O3W Er1 O5 C7 61.1(9) . . . . ? O2W Er1 O5 C7 -23.8(12) . . . . ? O1W Er1 O5 C7 -142.7(9) . . . . ? O10 Er1 O5 C7 -65.7(9) . . . . ? O9 Er1 O5 C7 -11.2(9) . . . . ? O1 Er1 O5 C7 140.4(9) . . . . ? O2 Er1 O5 C7 138.9(8) . . . . ? C13 Er1 O5 C7 -38.6(9) . . . . ? C1 Er1 O5 C7 139.4(9) . . . . ? O4W Er2 O7 C12 7.9(17) . . . . ? O12 Er2 O7 C12 -99.6(17) 1_545 . . . ? O3 Er2 O7 C12 -66.5(16) 2_755 . . . ? O6W Er2 O7 C12 152.7(17) . . . . ? O5W Er2 O7 C12 -138.5(16) . . . . ? O12 Er2 O7 C12 87.9(17) 2_766 . . . ? O11 Er2 O7 C12 78.1(16) 2_766 . . . ? C18 Er2 O7 C12 83.4(16) 2_766 . . . ? O5 Er1 O9 C13 -88.7(4) . . . . ? O3W Er1 O9 C13 171.8(4) . . . . ? O2W Er1 O9 C13 86.8(4) . . . . ? O1W Er1 O9 C13 -5.9(5) . . . . ? O10 Er1 O9 C13 1.7(4) . . . . ? O1 Er1 O9 C13 -135.2(4) . . . . ? O2 Er1 O9 C13 131.9(4) . . . . ? C1 Er1 O9 C13 178.3(4) . . . . ? O5 Er1 O10 C13 79.4(4) . . . . ? O3W Er1 O10 C13 -13.7(5) . . . . ? O2W Er1 O10 C13 -86.4(4) . . . . ? O1W Er1 O10 C13 172.4(4) . . . . ? O9 Er1 O10 C13 -1.7(4) . . . . ? O1 Er1 O10 C13 128.2(4) . . . . ? O2 Er1 O10 C13 -132.9(4) . . . . ? C1 Er1 O10 C13 -177.9(4) . . . . ? Er1 O2 C1 O1 1.0(6) . . . . ? Er1 O2 C1 C2 -178.7(6) . . . . ? Er1 O1 C1 O2 -1.0(6) . . . . ? Er1 O1 C1 C2 178.7(5) . . . . ? O5 Er1 C1 O2 -179.0(4) . . . . ? O3W Er1 C1 O2 -85.2(4) . . . . ? O2W Er1 C1 O2 -5.1(4) . . . . ? O1W Er1 C1 O2 91.6(4) . . . . ? O10 Er1 C1 O2 81.9(6) . . . . ? O9 Er1 C1 O2 -91.6(5) . . . . ? O1 Er1 C1 O2 178.9(7) . . . . ? O5 Er1 C1 O1 2.0(4) . . . . ? O3W Er1 C1 O1 95.9(4) . . . . ? O2W Er1 C1 O1 176.0(4) . . . . ? O1W Er1 C1 O1 -87.3(4) . . . . ? O10 Er1 C1 O1 -97.0(5) . . . . ? O9 Er1 C1 O1 89.4(5) . . . . ? O2 Er1 C1 O1 -178.9(7) . . . . ? O2 C1 C2 C3 0.0(12) . . . . ? O1 C1 C2 C3 -179.7(7) . . . . ? C1 C2 C3 C4 -179.0(7) . . . . ? C2 C3 C4 C5 -178.8(7) . . . . ? C3 C4 C5 C6 -176.4(7) . . . . ? Er2 O3 C6 O4 -8.8(12) 2_755 . . . ? Er2 O3 C6 C5 170.0(4) 2_755 . . . ? C4 C5 C6 O4 175.6(7) . . . . ? C4 C5 C6 O3 -3.4(11) . . . . ? Er1 O5 C7 O6 -107.2(9) . . . . ? Er1 O5 C7 C8 72.5(11) . . . . ? O6 C7 C8 C9 11.5(11) . . . . ? O5 C7 C8 C9 -168.2(7) . . . . ? C7 C8 C9 C10 174.3(7) . . . . ? C8 C9 C10 C11 -169.9(8) . . . . ? C9 C10 C11 C12 172.5(7) . . . . ? Er2 O7 C12 O8 -90.7(18) . . . . ? Er2 O7 C12 C11 93.8(17) . . . . ? C10 C11 C12 O8 -164.9(7) . . . . ? C10 C11 C12 O7 10.9(11) . . . . ? Er1 O9 C13 O10 -3.0(7) . . . . ? Er1 O9 C13 C14 177.0(6) . . . . ? Er1 O10 C13 O9 3.0(7) . . . . ? Er1 O10 C13 C14 -177.0(6) . . . . ? O5 Er1 C13 O9 86.3(4) . . . . ? O3W Er1 C13 O9 -8.1(4) . . . . ? O2W Er1 C13 O9 -88.3(4) . . . . ? O1W Er1 C13 O9 175.4(4) . . . . ? O10 Er1 C13 O9 -177.0(7) . . . . ? O1 Er1 C13 O9 84.0(6) . . . . ? O2 Er1 C13 O9 -89.2(5) . . . . ? O5 Er1 C13 O10 -96.7(4) . . . . ? O3W Er1 C13 O10 168.9(4) . . . . ? O2W Er1 C13 O10 88.6(4) . . . . ? O1W Er1 C13 O10 -7.6(4) . . . . ? O9 Er1 C13 O10 177.0(7) . . . . ? O1 Er1 C13 O10 -99.0(5) . . . . ? O2 Er1 C13 O10 87.8(6) . . . . ? O9 C13 C14 C15 -28.3(11) . . . . ? O10 C13 C14 C15 151.7(7) . . . . ? C13 C14 C15 C16 -175.6(6) . . . . ? C14 C15 C16 C17 177.2(8) . . . . ? C15 C16 C17 C18 -178.8(6) . . . . ? Er2 O11 C18 O12 -4.2(6) 2_766 . . . ? Er2 O11 C18 C17 176.4(6) 2_766 . . . ? Er2 O12 C18 O11 -161.6(6) 1_565 . . . ? Er2 O12 C18 O11 4.3(7) 2_766 . . . ? Er2 O12 C18 C17 17.7(12) 1_565 . . . ? Er2 O12 C18 C17 -176.4(5) 2_766 . . . ? Er2 O12 C18 Er2 -165.9(9) 1_565 . . 2_766 ? C16 C17 C18 O11 7.7(11) . . . . ? C16 C17 C18 O12 -171.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.150 _refine_diff_density_min -3.497 _refine_diff_density_rms 0.256 data_yhexaa _database_code_depnum_ccdc_archive 'CCDC 898154' #TrackingRef 'compound 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H28 O20 Y2' _chemical_formula_weight 742.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6940(10) _cell_length_b 8.0330(10) _cell_length_c 22.392(3) _cell_angle_alpha 94.750(10) _cell_angle_beta 93.000(10) _cell_angle_gamma 101.840(10) _cell_volume 1346.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 9.6 _cell_measurement_theta_max 12.2 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 4.378 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 P4 _diffrn_measurement_method scintillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5832 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4705 _reflns_number_gt 3471 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Due to the presence of pairs of cations (high electron density) near the water molecules, refinement of these protons resulted to deformation of the water geometry. For this reason, we restrained the water geometry near theoretical values by using DFIX and DANG. DFIX 0.83 O1W H1a O1W H1b DANG 1.32 0.08 H1a H1b DFIX 0.83 O2W H2a O2W H2b DANG 1.32 0.08 H2a H2b DFIX 0.83 O3W H3a O3W H3b DANG 1.32 0.08 H3a H3b DFIX 0.83 O4W H4a O4W H4b DANG 1.32 0.08 H4a H4b DFIX 0.83 O5W H5a O5W H5b DANG 1.32 0.08 H5a H5b DFIX 0.83 O6W H6a O6W H6b DANG 1.32 0.08 H6a H6b DFIX 0.83 O7W H7a O7W H7b DANG 1.32 0.08 H7a H7b DFIX 0.83 O8W H8a O8W H8b DANG 1.32 0.08 H8a H8b 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+1.4188P] 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 4705 _refine_ls_number_parameters 409 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.995 _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 Y1 Y 0.77698(6) 0.23701(6) 0.052734(19) 0.02238(14) Uani 1 1 d . . . Y2 Y 1.09200(6) 0.18440(6) 0.445608(19) 0.02210(13) Uani 1 1 d . . . O1 O 0.9517(4) 0.1815(4) -0.03157(14) 0.0287(8) Uani 1 1 d . . . O2 O 0.6639(4) 0.1479(4) -0.05129(14) 0.0300(8) Uani 1 1 d . . . O3 O 0.7819(4) -0.0811(4) -0.36154(14) 0.0291(8) Uani 1 1 d . . . O4 O 0.4888(5) -0.1067(6) -0.37936(17) 0.0543(12) Uani 1 1 d . . . O5 O 1.0584(5) 0.2891(5) 0.08947(15) 0.0364(9) Uani 1 1 d . . . O6 O 1.3115(5) 0.4802(5) 0.10390(15) 0.0380(9) Uani 1 1 d . . . O7 O 1.1979(5) 0.4373(4) 0.41559(15) 0.0364(9) Uani 1 1 d . . . O8 O 1.3538(5) 0.7023(5) 0.43615(16) 0.0453(10) Uani 1 1 d . . . O9 O 0.7720(5) 0.4485(4) 0.13488(14) 0.0337(8) Uani 1 1 d . . . O10 O 0.7127(5) 0.1811(4) 0.15411(14) 0.0339(8) Uani 1 1 d . . . O11 O 0.8230(5) 0.6365(4) 0.45518(15) 0.0341(8) Uani 1 1 d . . . O12 O 0.9764(5) 0.8953(4) 0.45162(14) 0.0309(8) Uani 1 1 d . . . O1W O 0.7558(5) -0.0589(4) 0.05043(16) 0.0291(8) Uani 1 1 d D . . O2W O 0.4778(5) 0.2404(5) 0.04744(17) 0.0398(9) Uani 1 1 d D . . O3W O 0.7983(5) 0.4929(4) 0.01090(15) 0.0331(8) Uani 1 1 d D . . O4W O 1.3632(5) 0.1411(6) 0.48243(17) 0.0482(11) Uani 1 1 d D . . O5W O 0.8699(5) 0.1285(5) 0.36270(16) 0.0369(9) Uani 1 1 d D . . O6W O 0.8443(5) 0.3001(4) 0.46784(16) 0.0328(8) Uani 1 1 d D . . O7W O 0.6297(5) -0.2653(5) 0.13458(19) 0.0391(9) Uani 1 1 d D . . O8W O 0.8113(6) -0.0319(5) 0.23837(19) 0.0458(10) Uani 1 1 d D . . C1 C 0.8145(7) 0.1458(6) -0.0700(2) 0.0267(11) Uani 1 1 d . . . C2 C 0.8429(7) 0.1014(7) -0.1332(2) 0.0316(12) Uani 1 1 d . . . H2 H 0.9582 0.0998 -0.1434 0.038 Uiso 1 1 calc R . . C3 C 0.7136(7) 0.0636(6) -0.1763(2) 0.0316(12) Uani 1 1 d . . . H3 H 0.5987 0.0666 -0.1660 0.038 Uiso 1 1 calc R . . C4 C 0.7388(7) 0.0179(6) -0.2387(2) 0.0288(11) Uani 1 1 d . . . H4 H 0.8531 0.0122 -0.2490 0.035 Uiso 1 1 calc R . . C5 C 0.6088(7) -0.0163(6) -0.2819(2) 0.0300(11) Uani 1 1 d . . . H5 H 0.4962 -0.0041 -0.2716 0.036 Uiso 1 1 calc R . . C6 C 0.6288(7) -0.0722(6) -0.3451(2) 0.0299(11) Uani 1 1 d . . . C7 C 1.1849(6) 0.3825(6) 0.1237(2) 0.0287(11) Uani 1 1 d . . . C8 C 1.1769(7) 0.3675(7) 0.1889(2) 0.0334(12) Uani 1 1 d . . . H8 H 1.0950 0.2770 0.2012 0.040 Uiso 1 1 calc R . . C9 C 1.2786(7) 0.4745(7) 0.2306(2) 0.0377(13) Uani 1 1 d . . . H9 H 1.3668 0.5604 0.2188 0.045 Uiso 1 1 calc R . . C10 C 1.2582(8) 0.4633(7) 0.2937(2) 0.0388(13) Uani 1 1 d . . . H10 H 1.1806 0.3678 0.3047 0.047 Uiso 1 1 calc R . . C11 C 1.3419(7) 0.5791(7) 0.3378(2) 0.0361(13) Uani 1 1 d . . . H11 H 1.4332 0.6661 0.3284 0.043 Uiso 1 1 calc R . . C12 C 1.2946(7) 0.5740(7) 0.4012(2) 0.0311(12) Uani 1 1 d . . . C13 C 0.7365(7) 0.3375(6) 0.1724(2) 0.0274(11) Uani 1 1 d . . . C14 C 0.7284(7) 0.3871(6) 0.2363(2) 0.0314(12) Uani 1 1 d . . . H14 H 0.6562 0.3108 0.2583 0.038 Uiso 1 1 calc R . . C15 C 0.8168(7) 0.5332(6) 0.2651(2) 0.0309(12) Uani 1 1 d . . . H15 H 0.8841 0.6127 0.2430 0.037 Uiso 1 1 calc R . . C16 C 0.8141(7) 0.5753(7) 0.3289(2) 0.0358(13) Uani 1 1 d . . . H16 H 0.7405 0.4979 0.3502 0.043 Uiso 1 1 calc R . . C17 C 0.9092(7) 0.7170(6) 0.3599(2) 0.0337(12) Uani 1 1 d . . . H17 H 0.9827 0.7973 0.3397 0.040 Uiso 1 1 calc R . . C18 C 0.9003(7) 0.7485(6) 0.4250(2) 0.0286(11) Uani 1 1 d . . . H5A H 0.863(9) 0.087(9) 0.3276(13) 0.080 Uiso 1 1 d D . . H5B H 0.765(4) 0.122(9) 0.371(3) 0.080 Uiso 1 1 d D . . H6A H 0.844(10) 0.398(4) 0.460(3) 0.080 Uiso 1 1 d D . . H7A H 0.524(4) -0.306(8) 0.124(3) 0.080 Uiso 1 1 d D . . H8A H 0.745(8) -0.126(5) 0.230(3) 0.080 Uiso 1 1 d D . . H3A H 0.860(8) 0.587(5) 0.023(3) 0.080 Uiso 1 1 d D . . H2A H 0.418(8) 0.184(8) 0.018(2) 0.080 Uiso 1 1 d D . . H3B H 0.756(9) 0.497(8) -0.0235(14) 0.080 Uiso 1 1 d D . . H1A H 0.712(8) -0.120(7) 0.077(2) 0.080 Uiso 1 1 d D . . H2B H 0.422(8) 0.295(8) 0.068(3) 0.080 Uiso 1 1 d D . . H4A H 1.428(7) 0.130(9) 0.455(2) 0.080 Uiso 1 1 d D . . H4B H 1.425(8) 0.171(9) 0.5136(17) 0.080 Uiso 1 1 d D . . H1B H 0.855(5) -0.079(9) 0.044(3) 0.080 Uiso 1 1 d D . . H7B H 0.679(8) -0.346(6) 0.139(3) 0.080 Uiso 1 1 d D . . H8B H 0.783(9) 0.041(6) 0.218(3) 0.080 Uiso 1 1 d D . . H6B H 0.787(8) 0.286(9) 0.498(2) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0264(3) 0.0225(3) 0.0173(2) -0.00157(18) -0.00281(19) 0.0053(2) Y2 0.0262(3) 0.0223(3) 0.0166(2) -0.00158(18) -0.00069(19) 0.0044(2) O1 0.0215(18) 0.041(2) 0.0223(17) -0.0047(15) -0.0038(14) 0.0070(15) O2 0.0241(19) 0.042(2) 0.0233(17) -0.0075(15) -0.0005(14) 0.0103(16) O3 0.0234(19) 0.043(2) 0.0208(17) -0.0041(15) -0.0014(14) 0.0105(16) O4 0.026(2) 0.097(3) 0.034(2) -0.017(2) -0.0033(18) 0.011(2) O5 0.031(2) 0.046(2) 0.0268(19) -0.0007(16) -0.0082(16) -0.0003(17) O6 0.035(2) 0.044(2) 0.0282(19) 0.0021(17) -0.0015(16) -0.0038(18) O7 0.050(2) 0.0264(19) 0.0297(19) 0.0041(15) 0.0071(17) -0.0010(17) O8 0.056(3) 0.039(2) 0.032(2) -0.0120(18) 0.0053(19) -0.0055(19) O9 0.054(2) 0.0214(18) 0.0245(18) 0.0004(15) -0.0005(16) 0.0061(16) O10 0.050(2) 0.0252(19) 0.0231(18) -0.0016(15) 0.0015(16) 0.0023(17) O11 0.047(2) 0.0253(19) 0.0269(18) 0.0007(15) -0.0024(16) 0.0023(17) O12 0.047(2) 0.0222(18) 0.0199(17) -0.0035(14) -0.0007(15) 0.0007(16) O1W 0.026(2) 0.0284(19) 0.033(2) 0.0014(15) -0.0001(16) 0.0079(16) O2W 0.028(2) 0.047(2) 0.039(2) -0.0167(18) -0.0007(17) 0.0041(18) O3W 0.041(2) 0.0282(19) 0.0265(19) 0.0050(16) -0.0060(16) 0.0008(17) O4W 0.038(2) 0.079(3) 0.028(2) -0.017(2) -0.0114(17) 0.023(2) O5W 0.030(2) 0.054(2) 0.0252(19) -0.0086(17) -0.0027(16) 0.0124(19) O6W 0.036(2) 0.031(2) 0.033(2) -0.0002(16) 0.0054(16) 0.0112(17) O7W 0.033(2) 0.033(2) 0.050(2) 0.0028(18) 0.0002(19) 0.0049(17) O8W 0.044(3) 0.052(3) 0.042(2) -0.001(2) -0.0041(19) 0.014(2) C1 0.031(3) 0.024(3) 0.023(3) -0.003(2) -0.006(2) 0.006(2) C2 0.028(3) 0.045(3) 0.023(3) -0.003(2) 0.000(2) 0.012(2) C3 0.034(3) 0.037(3) 0.024(3) -0.002(2) 0.003(2) 0.009(2) C4 0.023(3) 0.036(3) 0.027(3) -0.002(2) 0.000(2) 0.007(2) C5 0.025(3) 0.041(3) 0.024(3) -0.001(2) 0.000(2) 0.009(2) C6 0.029(3) 0.032(3) 0.026(3) -0.005(2) -0.004(2) 0.003(2) C7 0.025(3) 0.034(3) 0.027(3) 0.001(2) -0.006(2) 0.009(2) C8 0.032(3) 0.042(3) 0.024(3) 0.007(2) -0.004(2) 0.001(2) C9 0.040(3) 0.045(3) 0.026(3) 0.005(2) -0.001(2) 0.006(3) C10 0.046(3) 0.038(3) 0.029(3) 0.003(2) -0.003(2) 0.002(3) C11 0.039(3) 0.036(3) 0.030(3) 0.005(2) 0.004(2) 0.000(2) C12 0.027(3) 0.034(3) 0.032(3) 0.002(2) -0.004(2) 0.007(2) C13 0.029(3) 0.030(3) 0.021(2) -0.005(2) -0.005(2) 0.006(2) C14 0.035(3) 0.031(3) 0.026(3) -0.002(2) 0.001(2) 0.005(2) C15 0.034(3) 0.029(3) 0.028(3) -0.005(2) -0.002(2) 0.005(2) C16 0.048(3) 0.035(3) 0.024(3) 0.002(2) 0.001(2) 0.008(3) C17 0.047(3) 0.028(3) 0.025(3) 0.003(2) 0.002(2) 0.006(2) C18 0.039(3) 0.026(3) 0.021(2) -0.002(2) -0.009(2) 0.011(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 Y1 O5 2.219(4) . ? Y1 O2W 2.305(4) . ? Y1 O3W 2.308(4) . ? Y1 O1W 2.345(4) . ? Y1 O9 2.406(4) . ? Y1 O10 2.407(4) . ? Y1 O1 2.438(3) . ? Y1 O2 2.440(3) . ? Y1 C13 2.785(5) . ? Y1 C1 2.831(5) . ? Y2 O7 2.201(4) . ? Y2 O4W 2.306(4) . ? Y2 O12 2.328(4) 1_545 ? Y2 O3 2.332(3) 2_755 ? Y2 O6W 2.344(4) . ? Y2 O5W 2.405(4) . ? Y2 O12 2.493(4) 2_766 ? Y2 O11 2.523(4) 2_766 ? Y2 C18 2.898(5) 2_766 ? O1 C1 1.296(6) . ? O2 C1 1.255(6) . ? O3 C6 1.266(6) . ? O3 Y2 2.332(3) 2_755 ? O4 C6 1.258(6) . ? O5 C7 1.275(6) . ? O6 C7 1.245(6) . ? O7 C12 1.270(6) . ? O8 C12 1.232(6) . ? O9 C13 1.273(6) . ? O10 C13 1.262(6) . ? O11 C18 1.242(6) . ? O11 Y2 2.523(4) 2_766 ? O12 C18 1.285(6) . ? O12 Y2 2.328(4) 1_565 ? O12 Y2 2.493(4) 2_766 ? O1W H1A 0.84(2) . ? O1W H1B 0.83(2) . ? O2W H2A 0.82(2) . ? O2W H2B 0.82(2) . ? O3W H3A 0.82(2) . ? O3W H3B 0.83(2) . ? O4W H4A 0.82(2) . ? O4W H4B 0.81(2) . ? O5W H5A 0.82(2) . ? O5W H5B 0.83(2) . ? O6W H6A 0.82(2) . ? O6W H6B 0.82(2) . ? O7W H7A 0.82(2) . ? O7W H7B 0.83(2) . ? O8W H8A 0.83(2) . ? O8W H8B 0.83(2) . ? C1 C2 1.469(7) . ? C2 C3 1.319(7) . ? C2 H2 0.9300 . ? C3 C4 1.447(7) . ? C3 H3 0.9300 . ? C4 C5 1.324(7) . ? C4 H4 0.9300 . ? C5 C6 1.475(7) . ? C5 H5 0.9300 . ? C7 C8 1.478(7) . ? C8 C9 1.319(8) . ? C8 H8 0.9300 . ? C9 C10 1.436(8) . ? C9 H9 0.9300 . ? C10 C11 1.339(8) . ? C10 H10 0.9300 . ? C11 C12 1.486(8) . ? C11 H11 0.9300 . ? C13 C14 1.463(7) . ? C14 C15 1.325(7) . ? C14 H14 0.9300 . ? C15 C16 1.443(7) . ? C15 H15 0.9300 . ? C16 C17 1.337(8) . ? C16 H16 0.9300 . ? C17 C18 1.467(7) . ? C17 H17 0.9300 . ? C18 Y2 2.897(5) 2_766 ? 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 Y1 O2W 158.86(14) . . ? O5 Y1 O3W 95.52(14) . . ? O2W Y1 O3W 82.77(15) . . ? O5 Y1 O1W 91.57(14) . . ? O2W Y1 O1W 98.89(14) . . ? O3W Y1 O1W 154.85(13) . . ? O5 Y1 O9 79.18(14) . . ? O2W Y1 O9 80.10(14) . . ? O3W Y1 O9 74.08(13) . . ? O1W Y1 O9 131.04(13) . . ? O5 Y1 O10 83.92(14) . . ? O2W Y1 O10 80.57(15) . . ? O3W Y1 O10 127.37(13) . . ? O1W Y1 O10 77.33(13) . . ? O9 Y1 O10 54.03(12) . . ? O5 Y1 O1 73.83(13) . . ? O2W Y1 O1 126.23(13) . . ? O3W Y1 O1 80.92(13) . . ? O1W Y1 O1 77.95(13) . . ? O9 Y1 O1 140.94(13) . . ? O10 Y1 O1 146.02(13) . . ? O5 Y1 O2 127.23(13) . . ? O2W Y1 O2 73.07(13) . . ? O3W Y1 O2 76.89(13) . . ? O1W Y1 O2 79.60(13) . . ? O9 Y1 O2 142.47(13) . . ? O10 Y1 O2 141.52(13) . . ? O1 Y1 O2 53.41(11) . . ? O5 Y1 C13 79.78(15) . . ? O2W Y1 C13 79.89(15) . . ? O3W Y1 C13 101.02(15) . . ? O1W Y1 C13 103.99(15) . . ? O9 Y1 C13 27.16(14) . . ? O10 Y1 C13 26.89(14) . . ? O1 Y1 C13 153.59(14) . . ? O2 Y1 C13 152.93(14) . . ? O5 Y1 C1 100.99(15) . . ? O2W Y1 C1 99.14(15) . . ? O3W Y1 C1 77.01(14) . . ? O1W Y1 C1 77.96(14) . . ? O9 Y1 C1 150.95(14) . . ? O10 Y1 C1 154.92(14) . . ? O1 Y1 C1 27.18(13) . . ? O2 Y1 C1 26.23(13) . . ? C13 Y1 C1 177.92(16) . . ? O7 Y2 O4W 95.55(17) . . ? O7 Y2 O12 165.55(13) . 1_545 ? O4W Y2 O12 88.08(16) . 1_545 ? O7 Y2 O3 84.52(14) . 2_755 ? O4W Y2 O3 75.44(13) . 2_755 ? O12 Y2 O3 82.87(13) 1_545 2_755 ? O7 Y2 O6W 84.24(14) . . ? O4W Y2 O6W 145.30(14) . . ? O12 Y2 O6W 100.69(14) 1_545 . ? O3 Y2 O6W 138.63(13) 2_755 . ? O7 Y2 O5W 89.61(15) . . ? O4W Y2 O5W 146.32(14) . . ? O12 Y2 O5W 79.81(14) 1_545 . ? O3 Y2 O5W 71.96(12) 2_755 . ? O6W Y2 O5W 68.28(13) . . ? O7 Y2 O12 129.48(13) . 2_766 ? O4W Y2 O12 78.56(15) . 2_766 ? O12 Y2 O12 64.94(13) 1_545 2_766 ? O3 Y2 O12 138.95(13) 2_755 2_766 ? O6W Y2 O12 75.16(13) . 2_766 ? O5W Y2 O12 122.45(13) . 2_766 ? O7 Y2 O11 78.74(13) . 2_766 ? O4W Y2 O11 71.75(14) . 2_766 ? O12 Y2 O11 115.62(12) 1_545 2_766 ? O3 Y2 O11 141.24(13) 2_755 2_766 ? O6W Y2 O11 74.22(14) . 2_766 ? O5W Y2 O11 141.65(13) . 2_766 ? O12 Y2 O11 51.52(12) 2_766 2_766 ? O7 Y2 C18 103.58(15) . 2_766 ? O4W Y2 C18 74.14(15) . 2_766 ? O12 Y2 C18 90.87(14) 1_545 2_766 ? O3 Y2 C18 149.12(14) 2_755 2_766 ? O6W Y2 C18 72.24(14) . 2_766 ? O5W Y2 C18 136.71(15) . 2_766 ? O12 Y2 C18 26.24(13) 2_766 2_766 ? O11 Y2 C18 25.30(13) 2_766 2_766 ? C1 O1 Y1 93.5(3) . . ? C1 O2 Y1 94.5(3) . . ? C6 O3 Y2 138.4(3) . 2_755 ? C7 O5 Y1 149.2(4) . . ? C12 O7 Y2 166.3(4) . . ? C13 O9 Y1 93.2(3) . . ? C13 O10 Y1 93.5(3) . . ? C18 O11 Y2 94.5(3) . 2_766 ? C18 O12 Y2 148.8(3) . 1_565 ? C18 O12 Y2 94.7(3) . 2_766 ? Y2 O12 Y2 115.06(13) 1_565 2_766 ? Y1 O1W H1A 125(5) . . ? Y1 O1W H1B 108(5) . . ? H1A O1W H1B 108(6) . . ? Y1 O2W H2A 116(5) . . ? Y1 O2W H2B 130(5) . . ? H2A O2W H2B 113(6) . . ? Y1 O3W H3A 129(5) . . ? Y1 O3W H3B 122(5) . . ? H3A O3W H3B 108(6) . . ? Y2 O4W H4A 110(5) . . ? Y2 O4W H4B 135(5) . . ? H4A O4W H4B 109(6) . . ? Y2 O5W H5A 136(5) . . ? Y2 O5W H5B 117(5) . . ? H5A O5W H5B 105(6) . . ? Y2 O6W H6A 119(5) . . ? Y2 O6W H6B 127(5) . . ? H6A O6W H6B 105(6) . . ? H7A O7W H7B 107(6) . . ? H8A O8W H8B 111(6) . . ? O2 C1 O1 118.5(5) . . ? O2 C1 C2 123.4(5) . . ? O1 C1 C2 118.2(5) . . ? O2 C1 Y1 59.2(3) . . ? O1 C1 Y1 59.3(3) . . ? C2 C1 Y1 177.4(4) . . ? C3 C2 C1 123.6(5) . . ? C3 C2 H2 118.2 . . ? C1 C2 H2 118.2 . . ? C2 C3 C4 124.3(5) . . ? C2 C3 H3 117.8 . . ? C4 C3 H3 117.8 . . ? C5 C4 C3 123.9(5) . . ? C5 C4 H4 118.0 . . ? C3 C4 H4 118.0 . . ? C4 C5 C6 125.0(5) . . ? C4 C5 H5 117.5 . . ? C6 C5 H5 117.5 . . ? O4 C6 O3 124.5(5) . . ? O4 C6 C5 116.2(5) . . ? O3 C6 C5 119.3(5) . . ? O6 C7 O5 122.5(5) . . ? O6 C7 C8 120.8(5) . . ? O5 C7 C8 116.7(5) . . ? C9 C8 C7 124.1(5) . . ? C9 C8 H8 118.0 . . ? C7 C8 H8 118.0 . . ? C8 C9 C10 122.5(6) . . ? C8 C9 H9 118.7 . . ? C10 C9 H9 118.7 . . ? C11 C10 C9 125.3(6) . . ? C11 C10 H10 117.3 . . ? C9 C10 H10 117.3 . . ? C10 C11 C12 122.6(5) . . ? C10 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? O8 C12 O7 124.8(5) . . ? O8 C12 C11 117.5(5) . . ? O7 C12 C11 117.6(5) . . ? O10 C13 O9 119.1(5) . . ? O10 C13 C14 119.2(5) . . ? O9 C13 C14 121.6(5) . . ? O10 C13 Y1 59.6(3) . . ? O9 C13 Y1 59.6(3) . . ? C14 C13 Y1 175.6(4) . . ? C15 C14 C13 124.5(5) . . ? C15 C14 H14 117.7 . . ? C13 C14 H14 117.7 . . ? C14 C15 C16 123.5(5) . . ? C14 C15 H15 118.3 . . ? C16 C15 H15 118.3 . . ? C17 C16 C15 125.0(6) . . ? C17 C16 H16 117.5 . . ? C15 C16 H16 117.5 . . ? C16 C17 C18 121.4(5) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? O11 C18 O12 119.2(5) . . ? O11 C18 C17 121.7(5) . . ? O12 C18 C17 119.0(5) . . ? O11 C18 Y2 60.2(3) . 2_766 ? O12 C18 Y2 59.0(3) . 2_766 ? C17 C18 Y2 176.2(4) . 2_766 ? 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 Y1 O1 C1 -177.7(3) . . . . ? O2W Y1 O1 C1 -5.2(4) . . . . ? O3W Y1 O1 C1 -79.2(3) . . . . ? O1W Y1 O1 C1 87.1(3) . . . . ? O9 Y1 O1 C1 -129.6(3) . . . . ? O10 Y1 O1 C1 131.2(3) . . . . ? O2 Y1 O1 C1 1.2(3) . . . . ? C13 Y1 O1 C1 -175.7(3) . . . . ? O5 Y1 O2 C1 0.2(4) . . . . ? O2W Y1 O2 C1 173.5(3) . . . . ? O3W Y1 O2 C1 87.2(3) . . . . ? O1W Y1 O2 C1 -83.8(3) . . . . ? O9 Y1 O2 C1 127.2(3) . . . . ? O10 Y1 O2 C1 -137.7(3) . . . . ? O1 Y1 O2 C1 -1.2(3) . . . . ? C13 Y1 O2 C1 175.7(3) . . . . ? O2W Y1 O5 C7 -24.6(10) . . . . ? O3W Y1 O5 C7 59.6(7) . . . . ? O1W Y1 O5 C7 -144.6(7) . . . . ? O9 Y1 O5 C7 -13.0(7) . . . . ? O10 Y1 O5 C7 -67.5(7) . . . . ? O1 Y1 O5 C7 138.5(7) . . . . ? O2 Y1 O5 C7 137.3(7) . . . . ? C13 Y1 O5 C7 -40.6(7) . . . . ? C1 Y1 O5 C7 137.4(7) . . . . ? O4W Y2 O7 C12 9.1(15) . . . . ? O12 Y2 O7 C12 -94.9(16) 1_545 . . . ? O3 Y2 O7 C12 -65.7(15) 2_755 . . . ? O6W Y2 O7 C12 154.2(15) . . . . ? O5W Y2 O7 C12 -137.6(15) . . . . ? O12 Y2 O7 C12 88.8(15) 2_766 . . . ? O11 Y2 O7 C12 79.2(15) 2_766 . . . ? C18 Y2 O7 C12 84.1(15) 2_766 . . . ? O5 Y1 O9 C13 -88.7(3) . . . . ? O2W Y1 O9 C13 87.1(3) . . . . ? O3W Y1 O9 C13 172.3(3) . . . . ? O1W Y1 O9 C13 -6.1(4) . . . . ? O10 Y1 O9 C13 1.6(3) . . . . ? O1 Y1 O9 C13 -135.4(3) . . . . ? O2 Y1 O9 C13 131.7(3) . . . . ? C1 Y1 O9 C13 178.1(3) . . . . ? O5 Y1 O10 C13 79.4(3) . . . . ? O2W Y1 O10 C13 -86.2(3) . . . . ? O3W Y1 O10 C13 -12.9(4) . . . . ? O1W Y1 O10 C13 172.4(3) . . . . ? O9 Y1 O10 C13 -1.7(3) . . . . ? O1 Y1 O10 C13 128.1(3) . . . . ? O2 Y1 O10 C13 -133.1(3) . . . . ? C1 Y1 O10 C13 -177.6(4) . . . . ? Y1 O2 C1 O1 2.0(5) . . . . ? Y1 O2 C1 C2 -179.4(5) . . . . ? Y1 O1 C1 O2 -2.0(5) . . . . ? Y1 O1 C1 C2 179.3(4) . . . . ? O5 Y1 C1 O2 -179.8(3) . . . . ? O2W Y1 C1 O2 -6.3(3) . . . . ? O3W Y1 C1 O2 -86.7(3) . . . . ? O1W Y1 C1 O2 90.9(3) . . . . ? O9 Y1 C1 O2 -92.4(4) . . . . ? O10 Y1 C1 O2 80.9(5) . . . . ? O1 Y1 C1 O2 177.9(5) . . . . ? O5 Y1 C1 O1 2.2(3) . . . . ? O2W Y1 C1 O1 175.8(3) . . . . ? O3W Y1 C1 O1 95.4(3) . . . . ? O1W Y1 C1 O1 -87.0(3) . . . . ? O9 Y1 C1 O1 89.7(4) . . . . ? O10 Y1 C1 O1 -97.0(4) . . . . ? O2 Y1 C1 O1 -177.9(5) . . . . ? O2 C1 C2 C3 1.7(9) . . . . ? O1 C1 C2 C3 -179.7(5) . . . . ? C1 C2 C3 C4 -179.3(5) . . . . ? C2 C3 C4 C5 -178.5(6) . . . . ? C3 C4 C5 C6 -176.5(5) . . . . ? Y2 O3 C6 O4 -10.1(10) 2_755 . . . ? Y2 O3 C6 C5 170.6(4) 2_755 . . . ? C4 C5 C6 O4 176.7(6) . . . . ? C4 C5 C6 O3 -3.9(9) . . . . ? Y1 O5 C7 O6 -106.4(7) . . . . ? Y1 O5 C7 C8 74.7(9) . . . . ? O6 C7 C8 C9 13.3(9) . . . . ? O5 C7 C8 C9 -167.8(6) . . . . ? C7 C8 C9 C10 175.3(6) . . . . ? C8 C9 C10 C11 -171.5(6) . . . . ? C9 C10 C11 C12 170.2(6) . . . . ? Y2 O7 C12 O8 -87.9(16) . . . . ? Y2 O7 C12 C11 91.3(16) . . . . ? C10 C11 C12 O8 -166.2(6) . . . . ? C10 C11 C12 O7 14.6(9) . . . . ? Y1 O10 C13 O9 2.9(5) . . . . ? Y1 O10 C13 C14 -175.2(4) . . . . ? Y1 O9 C13 O10 -2.9(5) . . . . ? Y1 O9 C13 C14 175.1(5) . . . . ? O5 Y1 C13 O10 -96.8(3) . . . . ? O2W Y1 C13 O10 89.1(3) . . . . ? O3W Y1 C13 O10 169.6(3) . . . . ? O1W Y1 C13 O10 -7.7(3) . . . . ? O9 Y1 C13 O10 177.1(5) . . . . ? O1 Y1 C13 O10 -98.7(4) . . . . ? O2 Y1 C13 O10 86.8(4) . . . . ? O10 C13 C14 C15 151.1(6) . . . . ? O9 C13 C14 C15 -26.9(9) . . . . ? C13 C14 C15 C16 -176.5(6) . . . . ? C14 C15 C16 C17 176.1(6) . . . . ? C15 C16 C17 C18 -179.1(6) . . . . ? Y2 O11 C18 O12 -2.9(5) 2_766 . . . ? Y2 O11 C18 C17 176.3(5) 2_766 . . . ? Y2 O12 C18 O11 -160.4(5) 1_565 . . . ? Y2 O12 C18 O11 2.9(6) 2_766 . . . ? Y2 O12 C18 C17 20.5(10) 1_565 . . . ? Y2 O12 C18 C17 -176.2(5) 2_766 . . . ? Y2 O12 C18 Y2 -163.3(7) 1_565 . . 2_766 ? C16 C17 C18 O11 9.5(9) . . . . ? C16 C17 C18 O12 -171.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.751 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.094 data_erhex2 _database_code_depnum_ccdc_archive 'CCDC 898155' #TrackingRef 'compound 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H20 Er2 O16' _chemical_formula_weight 826.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.2522(9) _cell_length_b 7.7825(5) _cell_length_c 20.2169(16) _cell_angle_alpha 90.00 _cell_angle_beta 110.634(2) _cell_angle_gamma 90.00 _cell_volume 2245.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 9.8 _cell_measurement_theta_max 12.3 _exptl_crystal_description prismatic _exptl_crystal_colour pink _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 7.505 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 9139 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1980 _reflns_number_gt 1944 _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 ; DANG 1.312545 0.020000 H1b H1a H2a H2b DFIX 0.830000 0.010000 O1W H1a O1W H1b O2W H2a O2W H2b 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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0088P)^2^+6.1417P] 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 1980 _refine_ls_number_parameters 175 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0158 _refine_ls_R_factor_gt 0.0152 _refine_ls_wR_factor_ref 0.0357 _refine_ls_wR_factor_gt 0.0356 _refine_ls_goodness_of_fit_ref 1.240 _refine_ls_restrained_S_all 1.238 _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 0.636621(8) 0.543368(16) 0.518041(6) 0.00727(6) Uani 1 1 d . . . O1 O 0.18451(14) 0.1783(3) 0.09349(11) 0.0125(4) Uani 1 1 d . . . O2 O 0.09193(14) 0.4030(3) 0.09191(11) 0.0140(5) Uani 1 1 d . . . O3 O 0.48112(14) 0.4849(3) 0.42783(11) 0.0096(4) Uani 1 1 d . . . O4 O 0.59898(14) 0.3207(3) 0.42943(10) 0.0116(4) Uani 1 1 d . . . O5 O 0.84354(14) 0.8171(3) 0.57289(10) 0.0127(5) Uani 1 1 d . . . O6 O 0.73038(13) 0.7088(3) 0.60646(11) 0.0123(4) Uani 1 1 d . . . O1W O 0.56488(15) 0.8138(3) 0.50871(11) 0.0130(5) Uani 1 1 d D . . H1A H 0.5138(14) 0.837(4) 0.4782(12) 0.019 Uiso 1 1 d D . . H1B H 0.573(2) 0.881(4) 0.5418(12) 0.019 Uiso 1 1 d D . . O2W O 0.78695(15) 0.4639(3) 0.52025(12) 0.0138(5) Uani 1 1 d D . . H2A H 0.8265(17) 0.534(3) 0.518(2) 0.021 Uiso 1 1 d D . . H2B H 0.8177(19) 0.377(2) 0.5378(18) 0.021 Uiso 1 1 d D . . C1 C 0.1662(2) 0.3164(4) 0.11835(15) 0.0107(6) Uani 1 1 d . . . C2 C 0.2357(2) 0.3819(4) 0.18567(15) 0.0112(6) Uani 1 1 d . . . H2 H 0.2219 0.4868 0.2040 0.013 Uiso 1 1 calc R . . C3 C 0.3157(2) 0.3034(4) 0.22192(15) 0.0109(6) Uani 1 1 d . . . H3 H 0.3332 0.2036 0.2025 0.013 Uiso 1 1 calc R . . C4 C 0.3770(2) 0.3657(4) 0.29024(15) 0.0121(6) Uani 1 1 d . . . H4 H 0.3579 0.4663 0.3081 0.015 Uiso 1 1 calc R . . C5 C 0.4579(2) 0.2941(4) 0.33012(15) 0.0122(6) Uani 1 1 d . . . H5 H 0.4789 0.1933 0.3138 0.015 Uiso 1 1 calc R . . C6 C 0.5154(2) 0.3680(4) 0.39900(15) 0.0098(6) Uani 1 1 d . . . C7 C 0.8130(2) 0.7651(4) 0.61934(15) 0.0098(6) Uani 1 1 d . . . C8 C 0.8759(2) 0.7654(4) 0.69401(16) 0.0109(6) Uani 1 1 d . . . H8 H 0.8490 0.7612 0.7298 0.013 Uiso 1 1 calc R . . C9 C 0.9690(2) 0.7714(4) 0.71345(15) 0.0121(6) Uani 1 1 d . . . H9 H 0.9958 0.7758 0.6776 0.014 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.00478(8) 0.00792(8) 0.00786(8) 0.00014(5) 0.00068(6) 0.00029(5) O1 0.0112(10) 0.0115(11) 0.0135(10) -0.0034(9) 0.0028(9) -0.0032(9) O2 0.0103(11) 0.0105(11) 0.0163(11) 0.0014(9) -0.0013(9) -0.0011(9) O3 0.0085(10) 0.0098(10) 0.0102(10) -0.0009(8) 0.0029(9) 0.0007(8) O4 0.0072(10) 0.0126(11) 0.0125(10) -0.0002(8) 0.0003(8) 0.0009(9) O5 0.0122(11) 0.0135(11) 0.0116(10) 0.0021(9) 0.0032(9) -0.0005(9) O6 0.0056(10) 0.0142(11) 0.0160(11) -0.0029(9) 0.0024(8) 0.0008(9) O1W 0.0103(10) 0.0118(11) 0.0130(11) -0.0026(9) -0.0008(9) 0.0022(9) O2W 0.0084(11) 0.0104(11) 0.0233(12) 0.0033(9) 0.0064(10) 0.0023(9) C1 0.0104(15) 0.0105(15) 0.0119(14) 0.0020(12) 0.0050(12) -0.0034(13) C2 0.0136(15) 0.0111(15) 0.0105(14) -0.0019(12) 0.0063(12) -0.0030(13) C3 0.0095(14) 0.0128(15) 0.0119(15) -0.0010(12) 0.0057(12) -0.0018(13) C4 0.0127(15) 0.0129(15) 0.0119(15) -0.0013(12) 0.0059(12) -0.0041(13) C5 0.0100(15) 0.0135(15) 0.0138(15) -0.0039(12) 0.0051(12) 0.0009(13) C6 0.0087(14) 0.0097(14) 0.0116(14) 0.0028(12) 0.0044(12) -0.0019(12) C7 0.0097(14) 0.0067(14) 0.0121(14) -0.0014(11) 0.0028(12) 0.0023(12) C8 0.0104(14) 0.0104(15) 0.0118(15) -0.0006(12) 0.0039(12) 0.0001(12) C9 0.0117(15) 0.0122(15) 0.0112(15) 0.0000(12) 0.0026(12) -0.0016(13) _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 O5 2.245(2) 7_666 ? Er1 O1 2.247(2) 8_556 ? Er1 O6 2.258(2) . ? Er1 O1W 2.349(2) . ? Er1 O2W 2.360(2) . ? Er1 O4 2.412(2) . ? Er1 O3 2.420(2) 5_666 ? Er1 O3 2.472(2) . ? Er1 C6 2.817(3) . ? O1 C1 1.259(4) . ? O1 Er1 2.247(2) 8_455 ? O2 C1 1.263(4) . ? O3 C6 1.287(4) . ? O3 Er1 2.420(2) 5_666 ? O4 C6 1.259(4) . ? O5 C7 1.253(4) . ? O5 Er1 2.245(2) 7_666 ? O6 C7 1.272(4) . ? O1W H1A 0.825(10) . ? O1W H1B 0.825(10) . ? O2W H2A 0.829(10) . ? O2W H2B 0.826(10) . ? C1 C2 1.489(4) . ? C2 C3 1.331(4) . ? C2 H2 0.9500 . ? C3 C4 1.452(4) . ? C3 H3 0.9500 . ? C4 C5 1.334(4) . ? C4 H4 0.9500 . ? C5 C6 1.476(4) . ? C5 H5 0.9500 . ? C7 C8 1.476(4) . ? C8 C9 1.333(4) . ? C8 H8 0.9500 . ? C9 C9 1.447(6) 2_756 ? C9 H9 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Er1 O1 145.23(7) 7_666 8_556 ? O5 Er1 O6 98.16(8) 7_666 . ? O1 Er1 O6 86.36(8) 8_556 . ? O5 Er1 O1W 72.21(8) 7_666 . ? O1 Er1 O1W 140.62(7) 8_556 . ? O6 Er1 O1W 72.52(7) . . ? O5 Er1 O2W 74.45(8) 7_666 . ? O1 Er1 O2W 72.82(8) 8_556 . ? O6 Er1 O2W 78.13(7) . . ? O1W Er1 O2W 131.18(8) . . ? O5 Er1 O4 78.74(7) 7_666 . ? O1 Er1 O4 83.58(7) 8_556 . ? O6 Er1 O4 156.42(7) . . ? O1W Er1 O4 127.01(7) . . ? O2W Er1 O4 78.53(7) . . ? O5 Er1 O3 138.57(7) 7_666 5_666 ? O1 Er1 O3 74.86(7) 8_556 5_666 ? O6 Er1 O3 93.31(7) . 5_666 ? O1W Er1 O3 73.67(7) . 5_666 ? O2W Er1 O3 146.98(7) . 5_666 ? O4 Er1 O3 104.49(7) . 5_666 ? O5 Er1 O3 81.72(7) 7_666 . ? O1 Er1 O3 110.94(7) 8_556 . ? O6 Er1 O3 149.84(7) . . ? O1W Er1 O3 78.87(7) . . ? O2W Er1 O3 129.71(7) . . ? O4 Er1 O3 53.44(7) . . ? O3 Er1 O3 69.20(8) 5_666 . ? O5 Er1 C6 76.83(8) 7_666 . ? O1 Er1 C6 99.58(8) 8_556 . ? O6 Er1 C6 174.05(8) . . ? O1W Er1 C6 102.63(8) . . ? O2W Er1 C6 103.29(8) . . ? O4 Er1 C6 26.44(8) . . ? O3 Er1 C6 88.51(8) 5_666 . ? O3 Er1 C6 27.17(8) . . ? C1 O1 Er1 149.50(19) . 8_455 ? C6 O3 Er1 128.70(18) . 5_666 ? C6 O3 Er1 91.55(16) . . ? Er1 O3 Er1 110.80(8) 5_666 . ? C6 O4 Er1 95.06(18) . . ? C7 O5 Er1 164.3(2) . 7_666 ? C7 O6 Er1 131.61(19) . . ? Er1 O1W H1A 123(2) . . ? Er1 O1W H1B 125(2) . . ? H1A O1W H1B 107(2) . . ? Er1 O2W H2A 123(2) . . ? Er1 O2W H2B 128(2) . . ? H2A O2W H2B 104(2) . . ? O1 C1 O2 125.3(3) . . ? O1 C1 C2 118.1(3) . . ? O2 C1 C2 116.6(3) . . ? C3 C2 C1 124.4(3) . . ? C3 C2 H2 117.8 . . ? C1 C2 H2 117.8 . . ? C2 C3 C4 122.0(3) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C5 C4 C3 125.7(3) . . ? C5 C4 H4 117.1 . . ? C3 C4 H4 117.1 . . ? C4 C5 C6 121.5(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? O4 C6 O3 119.2(3) . . ? O4 C6 C5 120.7(3) . . ? O3 C6 C5 120.1(3) . . ? O4 C6 Er1 58.50(15) . . ? O3 C6 Er1 61.28(15) . . ? C5 C6 Er1 171.0(2) . . ? O5 C7 O6 124.1(3) . . ? O5 C7 C8 119.1(3) . . ? O6 C7 C8 116.7(3) . . ? C9 C8 C7 122.8(3) . . ? C9 C8 H8 118.6 . . ? C7 C8 H8 118.6 . . ? C8 C9 C9 123.1(4) . 2_756 ? C8 C9 H9 118.4 . . ? C9 C9 H9 118.4 2_756 . ? 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 Er1 O3 C6 77.24(17) 7_666 . . . ? O1 Er1 O3 C6 -69.19(17) 8_556 . . . ? O6 Er1 O3 C6 169.25(17) . . . . ? O1W Er1 O3 C6 150.61(17) . . . . ? O2W Er1 O3 C6 15.46(19) . . . . ? O4 Er1 O3 C6 -4.84(15) . . . . ? O3 Er1 O3 C6 -132.8(2) 5_666 . . . ? O5 Er1 O3 Er1 -149.97(9) 7_666 . . 5_666 ? O1 Er1 O3 Er1 63.60(10) 8_556 . . 5_666 ? O6 Er1 O3 Er1 -57.95(17) . . . 5_666 ? O1W Er1 O3 Er1 -76.59(9) . . . 5_666 ? O2W Er1 O3 Er1 148.26(8) . . . 5_666 ? O4 Er1 O3 Er1 127.96(11) . . . 5_666 ? O3 Er1 O3 Er1 0.0 5_666 . . 5_666 ? C6 Er1 O3 Er1 132.8(2) . . . 5_666 ? O5 Er1 O4 C6 -83.03(17) 7_666 . . . ? O1 Er1 O4 C6 127.05(17) 8_556 . . . ? O6 Er1 O4 C6 -167.61(19) . . . . ? O1W Er1 O4 C6 -25.7(2) . . . . ? O2W Er1 O4 C6 -159.24(18) . . . . ? O3 Er1 O4 C6 54.54(18) 5_666 . . . ? O3 Er1 O4 C6 4.96(16) . . . . ? O5 Er1 O6 C7 -47.2(3) 7_666 . . . ? O1 Er1 O6 C7 98.1(3) 8_556 . . . ? O1W Er1 O6 C7 -115.5(3) . . . . ? O2W Er1 O6 C7 24.9(2) . . . . ? O4 Er1 O6 C7 33.3(4) . . . . ? O3 Er1 O6 C7 172.7(3) 5_666 . . . ? O3 Er1 O6 C7 -134.7(2) . . . . ? C6 Er1 O6 C7 -79.6(8) . . . . ? Er1 O1 C1 O2 -12.2(6) 8_455 . . . ? Er1 O1 C1 C2 165.6(3) 8_455 . . . ? O1 C1 C2 C3 -0.6(4) . . . . ? O2 C1 C2 C3 177.4(3) . . . . ? C1 C2 C3 C4 -174.8(3) . . . . ? C2 C3 C4 C5 179.5(3) . . . . ? C3 C4 C5 C6 179.9(3) . . . . ? Er1 O4 C6 O3 -8.8(3) . . . . ? Er1 O4 C6 C5 169.5(2) . . . . ? Er1 O3 C6 O4 -109.9(3) 5_666 . . . ? Er1 O3 C6 O4 8.5(3) . . . . ? Er1 O3 C6 C5 71.8(3) 5_666 . . . ? Er1 O3 C6 C5 -169.8(2) . . . . ? Er1 O3 C6 Er1 -118.48(19) 5_666 . . . ? C4 C5 C6 O4 -165.9(3) . . . . ? C4 C5 C6 O3 12.4(4) . . . . ? C4 C5 C6 Er1 -83.9(14) . . . . ? O5 Er1 C6 O4 91.15(17) 7_666 . . . ? O1 Er1 C6 O4 -53.55(17) 8_556 . . . ? O6 Er1 C6 O4 124.1(7) . . . . ? O1W Er1 C6 O4 159.18(16) . . . . ? O2W Er1 C6 O4 20.91(18) . . . . ? O3 Er1 C6 O4 -127.92(17) 5_666 . . . ? O3 Er1 C6 O4 -171.2(3) . . . . ? O5 Er1 C6 O3 -97.60(17) 7_666 . . . ? O1 Er1 C6 O3 117.70(16) 8_556 . . . ? O6 Er1 C6 O3 -64.6(8) . . . . ? O1W Er1 C6 O3 -29.57(17) . . . . ? O2W Er1 C6 O3 -167.84(15) . . . . ? O4 Er1 C6 O3 171.2(3) . . . . ? O3 Er1 C6 O3 43.33(18) 5_666 . . . ? O5 Er1 C6 C5 3.7(13) 7_666 . . . ? O1 Er1 C6 C5 -141.0(14) 8_556 . . . ? O6 Er1 C6 C5 36.7(18) . . . . ? O1W Er1 C6 C5 71.7(14) . . . . ? O2W Er1 C6 C5 -66.6(14) . . . . ? O4 Er1 C6 C5 -87.5(14) . . . . ? O3 Er1 C6 C5 144.6(14) 5_666 . . . ? O3 Er1 C6 C5 101.3(14) . . . . ? Er1 O5 C7 O6 54.2(9) 7_666 . . . ? Er1 O5 C7 C8 -126.7(6) 7_666 . . . ? Er1 O6 C7 O5 38.8(4) . . . . ? Er1 O6 C7 C8 -140.3(2) . . . . ? O5 C7 C8 C9 -19.5(4) . . . . ? O6 C7 C8 C9 159.7(3) . . . . ? C7 C8 C9 C9 -179.87(19) . . . 2_756 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.643 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.086