# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Qing-Yan Liu' _publ_contact_author_address ; College of Chemistry and Chemical Engineering, Jiangxi Normal University, Nanchang, Jiangxi 330022, P. R. China ; _publ_contact_author_email qyliuchem@hotmail.com _publ_contact_author_fax +86-791-88120380 _publ_contact_author_phone +86-791-88120380 _publ_requested_coeditor_name ? _publ_author_name 'Qing-Yan Liu' data_La _database_code_depnum_ccdc_archive 'CCDC 879607' #TrackingRef '- revised Ln.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 La O11' _chemical_formula_weight 469.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.989(7) _cell_length_b 13.190(3) _cell_length_c 6.8105(14) _cell_angle_alpha 90.00 _cell_angle_beta 101.518(5) _cell_angle_gamma 90.00 _cell_volume 2639.7(10) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3085 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 28.90 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 3.304 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3666 _exptl_absorpt_correction_T_max 0.7553 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8106 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 28.97 _reflns_number_total 3220 _reflns_number_gt 2736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.0316P] 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 3220 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0692 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 La1 La 0.401199(6) 0.703229(14) 0.72791(3) 0.01177(7) Uani 1 1 d . . . O1 O 0.38145(8) 0.54134(19) 0.8799(4) 0.0243(6) Uani 1 1 d . . . O2 O 0.35630(8) 0.38685(18) 0.9267(4) 0.0190(6) Uani 1 1 d . . . O3 O 0.13894(8) 0.50730(19) 0.4001(4) 0.0235(6) Uani 1 1 d . . . O4 O 0.15362(8) 0.67121(19) 0.4617(4) 0.0226(6) Uani 1 1 d . . . O5 O 0.31799(8) 0.68407(18) 0.8105(4) 0.0179(6) Uani 1 1 d . . . H5 H 0.3043 0.7380 0.8093 0.027 Uiso 1 1 calc R . . O6 O 0.19775(8) 0.37129(18) 0.5525(4) 0.0209(6) Uani 1 1 d . . . H6 H 0.1728 0.3922 0.4947 0.031 Uiso 1 1 calc R . . O7 O 0.47756(8) 0.72255(18) 0.9407(4) 0.0204(6) Uani 1 1 d . . . O8 O 0.55187(8) 0.75053(18) 1.0279(4) 0.0166(5) Uani 1 1 d . . . O9 O 0.42562(7) 0.88752(18) 0.8158(4) 0.0165(5) Uani 1 1 d . . . H9 H 0.4066 0.9263 0.7533 0.025 Uiso 1 1 calc R . . O10 O 0.45174(9) 0.5514(2) 0.6547(5) 0.0312(7) Uani 1 1 d . . . H10A H 0.4369 0.5228 0.5561 0.047 Uiso 1 1 d R . . H10B H 0.4703 0.5772 0.5961 0.047 Uiso 1 1 d R . . O11 O 0.39143(9) 0.7403(2) 1.0933(4) 0.0299(7) Uani 1 1 d . . . H11A H 0.4119 0.7469 1.1919 0.045 Uiso 1 1 d R . . H11B H 0.3743 0.6992 1.1301 0.045 Uiso 1 1 d R . . C1 C 0.30232(11) 0.5065(3) 0.7667(5) 0.0123(7) Uani 1 1 d . . . C2 C 0.28755(11) 0.6079(3) 0.7410(5) 0.0140(7) Uani 1 1 d . . . C3 C 0.24326(11) 0.6295(3) 0.6512(5) 0.0140(7) Uani 1 1 d . . . H3 H 0.2339 0.6968 0.6361 0.017 Uiso 1 1 calc R . . C4 C 0.21196(11) 0.5524(3) 0.5821(5) 0.0137(7) Uani 1 1 d . . . C5 C 0.22629(11) 0.4519(3) 0.6101(5) 0.0136(7) Uani 1 1 d . . . C6 C 0.27103(11) 0.4300(3) 0.7005(5) 0.0141(7) Uani 1 1 d . . . H6A H 0.2802 0.3627 0.7171 0.017 Uiso 1 1 calc R . . C7 C 0.34998(11) 0.4767(3) 0.8641(5) 0.0136(7) Uani 1 1 d . . . C8 C 0.16488(11) 0.5795(3) 0.4750(6) 0.0160(7) Uani 1 1 d . . . C9 C 0.50370(11) 0.8933(3) 0.9968(5) 0.0114(7) Uani 1 1 d . . . C10 C 0.46238(11) 0.9416(3) 0.9102(5) 0.0122(7) Uani 1 1 d . . . C11 C 0.54027(11) 0.9532(3) 1.0846(5) 0.0143(7) Uani 1 1 d . . . H11 H 0.5675 0.9220 1.1421 0.017 Uiso 1 1 calc R . . C12 C 0.51092(11) 0.7820(3) 0.9879(5) 0.0133(7) 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 La1 0.00820(10) 0.00906(11) 0.01675(13) -0.00027(8) -0.00062(7) -0.00135(7) O1 0.0140(12) 0.0177(14) 0.0381(18) 0.0085(12) -0.0021(11) -0.0040(10) O2 0.0138(11) 0.0117(13) 0.0292(16) 0.0064(11) -0.0012(11) 0.0023(10) O3 0.0122(12) 0.0183(14) 0.0347(17) 0.0021(12) -0.0076(11) -0.0030(11) O4 0.0161(13) 0.0121(13) 0.0349(17) 0.0008(12) -0.0063(11) 0.0021(10) O5 0.0122(12) 0.0088(12) 0.0313(16) -0.0038(11) 0.0012(11) -0.0002(9) O6 0.0124(11) 0.0141(13) 0.0327(17) 0.0050(11) -0.0041(11) -0.0036(10) O7 0.0160(12) 0.0104(13) 0.0317(17) -0.0007(11) -0.0028(11) -0.0031(10) O8 0.0123(12) 0.0121(13) 0.0241(15) -0.0023(11) 0.0004(10) 0.0029(10) O9 0.0085(11) 0.0133(13) 0.0243(15) -0.0025(11) -0.0047(10) -0.0006(9) O10 0.0207(14) 0.0240(16) 0.045(2) -0.0110(14) -0.0025(13) 0.0032(12) O11 0.0226(14) 0.0460(19) 0.0192(16) -0.0001(14) -0.0003(12) -0.0136(14) C1 0.0117(15) 0.0117(17) 0.0130(18) 0.0023(13) 0.0008(13) 0.0010(13) C2 0.0135(16) 0.0136(17) 0.0149(19) 0.0007(14) 0.0030(13) 0.0009(13) C3 0.0145(16) 0.0103(17) 0.017(2) 0.0000(14) 0.0037(14) 0.0022(13) C4 0.0087(15) 0.0169(18) 0.0149(19) 0.0029(14) 0.0011(13) 0.0018(13) C5 0.0111(15) 0.0141(18) 0.0159(19) 0.0002(14) 0.0039(13) -0.0045(13) C6 0.0171(17) 0.0088(16) 0.0159(19) 0.0020(13) 0.0022(14) 0.0011(13) C7 0.0106(15) 0.0162(18) 0.0143(18) 0.0012(14) 0.0027(13) 0.0015(13) C8 0.0116(16) 0.0160(18) 0.020(2) 0.0041(15) 0.0020(14) 0.0017(13) C9 0.0107(15) 0.0117(16) 0.0120(17) -0.0003(13) 0.0027(13) -0.0010(13) C10 0.0073(14) 0.0147(18) 0.0131(18) -0.0023(14) -0.0013(13) -0.0016(12) C11 0.0092(15) 0.0155(18) 0.0172(19) 0.0000(14) 0.0000(13) 0.0019(13) C12 0.0100(16) 0.0142(18) 0.0139(18) 0.0006(14) -0.0016(13) -0.0009(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O7 2.467(3) . ? La1 O1 2.495(3) . ? La1 O4 2.503(3) 7_566 ? La1 O2 2.516(3) 6_565 ? La1 O8 2.527(2) 2_656 ? La1 O9 2.575(2) . ? La1 O11 2.609(3) . ? La1 O10 2.619(3) . ? La1 O5 2.677(2) . ? O1 C7 1.261(4) . ? O2 C7 1.260(4) . ? O2 La1 2.516(2) 6_566 ? O3 C8 1.271(4) . ? O4 C8 1.254(4) . ? O4 La1 2.503(3) 7_566 ? O5 C2 1.376(4) . ? O5 H5 0.8200 . ? O6 C5 1.372(4) . ? O6 H6 0.8200 . ? O7 C12 1.261(4) . ? O8 C12 1.273(4) . ? O8 La1 2.527(2) 2_656 ? O9 C10 1.362(4) . ? O9 H9 0.8200 . ? O10 H10A 0.8200 . ? O10 H10B 0.8200 . ? O11 H11A 0.8200 . ? O11 H11B 0.8200 . ? C1 C6 1.390(5) . ? C1 C2 1.409(5) . ? C1 C7 1.503(4) . ? C2 C3 1.376(5) . ? C3 C4 1.400(5) . ? C3 H3 0.9300 . ? C4 C5 1.395(5) . ? C4 C8 1.498(5) . ? C5 C6 1.390(5) . ? C6 H6A 0.9300 . ? C9 C11 1.387(5) . ? C9 C10 1.413(5) . ? C9 C12 1.487(5) . ? C10 C11 1.390(5) 5_677 ? C11 C10 1.390(5) 5_677 ? C11 H11 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 O7 La1 O1 96.55(8) . . ? O7 La1 O4 132.21(8) . 7_566 ? O1 La1 O4 126.47(8) . 7_566 ? O7 La1 O2 144.17(8) . 6_565 ? O1 La1 O2 78.55(9) . 6_565 ? O4 La1 O2 72.69(8) 7_566 6_565 ? O7 La1 O8 78.46(9) . 2_656 ? O1 La1 O8 135.11(8) . 2_656 ? O4 La1 O8 83.09(9) 7_566 2_656 ? O2 La1 O8 80.53(8) 6_565 2_656 ? O7 La1 O9 65.05(8) . . ? O1 La1 O9 142.33(9) . . ? O4 La1 O9 67.81(8) 7_566 . ? O2 La1 O9 135.77(8) 6_565 . ? O8 La1 O9 75.84(8) 2_656 . ? O7 La1 O11 71.83(9) . . ? O1 La1 O11 71.54(10) . . ? O4 La1 O11 100.42(10) 7_566 . ? O2 La1 O11 136.25(8) 6_565 . ? O8 La1 O11 142.69(9) 2_656 . ? O9 La1 O11 71.48(9) . . ? O7 La1 O10 71.71(9) . . ? O1 La1 O10 67.61(9) . . ? O4 La1 O10 138.86(10) 7_566 . ? O2 La1 O10 73.71(8) 6_565 . ? O8 La1 O10 68.54(9) 2_656 . ? O9 La1 O10 128.14(8) . . ? O11 La1 O10 120.29(10) . . ? O7 La1 O5 132.95(9) . . ? O1 La1 O5 61.55(8) . . ? O4 La1 O5 68.10(8) 7_566 . ? O2 La1 O5 75.95(8) 6_565 . ? O8 La1 O5 147.03(8) 2_656 . ? O9 La1 O5 105.91(7) . . ? O11 La1 O5 62.00(8) . . ? O10 La1 O5 124.54(8) . . ? C7 O1 La1 141.2(2) . . ? C7 O2 La1 137.7(2) . 6_566 ? C8 O4 La1 144.6(2) . 7_566 ? C2 O5 La1 125.37(19) . . ? C2 O5 H5 109.5 . . ? La1 O5 H5 113.7 . . ? C5 O6 H6 109.5 . . ? C12 O7 La1 144.1(2) . . ? C12 O8 La1 125.4(2) . 2_656 ? C10 O9 La1 140.4(2) . . ? C10 O9 H9 109.5 . . ? La1 O9 H9 109.4 . . ? La1 O10 H10A 105.4 . . ? La1 O10 H10B 104.5 . . ? H10A O10 H10B 96.0 . . ? La1 O11 H11A 126.3 . . ? La1 O11 H11B 111.4 . . ? H11A O11 H11B 103.6 . . ? C6 C1 C2 118.3(3) . . ? C6 C1 C7 118.3(3) . . ? C2 C1 C7 123.5(3) . . ? O5 C2 C3 121.1(3) . . ? O5 C2 C1 118.7(3) . . ? C3 C2 C1 120.2(3) . . ? C2 C3 C4 121.5(3) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 118.5(3) . . ? C5 C4 C8 121.9(3) . . ? C3 C4 C8 119.5(3) . . ? O6 C5 C6 117.3(3) . . ? O6 C5 C4 122.7(3) . . ? C6 C5 C4 120.1(3) . . ? C5 C6 C1 121.5(3) . . ? C5 C6 H6A 119.2 . . ? C1 C6 H6A 119.2 . . ? O2 C7 O1 123.2(3) . . ? O2 C7 C1 117.5(3) . . ? O1 C7 C1 119.3(3) . . ? O4 C8 O3 124.0(3) . . ? O4 C8 C4 118.7(3) . . ? O3 C8 C4 117.3(3) . . ? C11 C9 C10 118.4(3) . . ? C11 C9 C12 118.1(3) . . ? C10 C9 C12 123.4(3) . . ? O9 C10 C11 119.3(3) . 5_677 ? O9 C10 C9 121.4(3) . . ? C11 C10 C9 119.3(3) 5_677 . ? C9 C11 C10 122.4(3) . 5_677 ? C9 C11 H11 118.8 . . ? C10 C11 H11 118.8 5_677 . ? O7 C12 O8 122.2(3) . . ? O7 C12 C9 120.7(3) . . ? O8 C12 C9 117.1(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O6 0.82 2.00 2.714(3) 145.1 4_556 O6 H6 O3 0.82 1.87 2.584(3) 145.1 . O9 H9 O3 0.82 1.78 2.588(3) 170.9 7_566 O10 H10A O1 0.82 2.03 2.805(4) 157.4 6_565 O10 H10B O8 0.82 2.48 2.898(4) 112.7 2_656 O11 H11A O8 0.82 2.00 2.795(4) 163.8 2_657 O11 H11B O2 0.82 2.47 3.167(4) 143.7 6_566 _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 28.97 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.832 _refine_diff_density_min -0.813 _refine_diff_density_rms 0.147 #===END OF 1 ## Crystallographic Data for compound 2 data_Pr _database_code_depnum_ccdc_archive 'CCDC 879608' #TrackingRef '- revised Ln.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 O11 Pr' _chemical_formula_weight 471.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.844(7) _cell_length_b 13.113(3) _cell_length_c 6.7951(16) _cell_angle_alpha 90.00 _cell_angle_beta 101.574(3) _cell_angle_gamma 90.00 _cell_volume 2605.1(11) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3215 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 29.07 _exptl_crystal_description block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 3.808 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3255 _exptl_absorpt_correction_T_max 0.8037 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 7853 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 29.07 _reflns_number_total 3160 _reflns_number_gt 2738 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The final Fourier map had a maximum and a minimum electron density of 5.479 and -2.235 \%A^-3^, respectively, and are within 0.88 \%A of praseodymium ion, which resulted from the smear effect of the praseodymium ion. ; _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^)+(0.0667P)^2^+64.0989P] 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 3160 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.1282 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.401728(12) 0.70269(2) 0.72795(5) 0.01131(14) Uani 1 1 d . . . O1 O 0.38270(18) 0.5422(4) 0.8823(9) 0.0239(12) Uani 1 1 d . . . O2 O 0.35714(17) 0.3872(4) 0.9327(8) 0.0192(10) Uani 1 1 d . . . O3 O 0.13873(17) 0.5085(4) 0.4020(9) 0.0231(11) Uani 1 1 d . . . O4 O 0.15324(18) 0.6733(4) 0.4631(9) 0.0218(11) Uani 1 1 d . . . O5 O 0.31924(18) 0.6855(4) 0.8097(8) 0.0194(11) Uani 1 1 d . . . H5 H 0.3058 0.7401 0.8092 0.029 Uiso 1 1 calc R . . O6 O 0.19783(17) 0.3721(4) 0.5534(8) 0.0199(11) Uani 1 1 d . . . H6 H 0.1729 0.3936 0.4955 0.030 Uiso 1 1 calc R . . O7 O 0.47757(18) 0.7209(4) 0.9387(8) 0.0210(11) Uani 1 1 d . . . O8 O 0.55221(16) 0.7488(4) 1.0268(7) 0.0158(10) Uani 1 1 d . . . O9 O 0.42542(16) 0.8862(3) 0.8131(7) 0.0147(9) Uani 1 1 d . . . H9 H 0.4062 0.9251 0.7502 0.022 Uiso 1 1 calc R . . O10 O 0.4516(2) 0.5517(4) 0.6580(9) 0.0290(13) Uani 1 1 d . . . H10A H 0.4360 0.5208 0.5635 0.044 Uiso 1 1 d R . . H10B H 0.4692 0.5769 0.5931 0.044 Uiso 1 1 d R . . O11 O 0.3918(2) 0.7411(5) 1.0892(8) 0.0275(12) Uani 1 1 d . . . H11A H 0.4124 0.7479 1.1882 0.041 Uiso 1 1 d R . . H11B H 0.3746 0.6999 1.1263 0.041 Uiso 1 1 d R . . C1 C 0.3031(2) 0.5070(5) 0.7672(9) 0.0114(12) Uani 1 1 d . . . C2 C 0.2881(2) 0.6097(5) 0.7408(10) 0.0135(12) Uani 1 1 d . . . C3 C 0.2436(2) 0.6322(5) 0.6520(10) 0.0131(12) Uani 1 1 d . . . H3 H 0.2341 0.6998 0.6377 0.016 Uiso 1 1 calc R . . C4 C 0.2122(2) 0.5535(5) 0.5826(10) 0.0136(13) Uani 1 1 d . . . C5 C 0.2266(2) 0.4519(5) 0.6110(10) 0.0136(12) Uani 1 1 d . . . C6 C 0.2716(2) 0.4300(5) 0.7022(10) 0.0146(13) Uani 1 1 d . . . H6A H 0.2808 0.3623 0.7201 0.018 Uiso 1 1 calc R . . C7 C 0.3510(2) 0.4775(5) 0.8672(10) 0.0123(12) Uani 1 1 d . . . C8 C 0.1651(2) 0.5810(5) 0.4772(11) 0.0161(13) Uani 1 1 d . . . C9 C 0.5037(2) 0.8928(5) 0.9976(10) 0.0110(11) Uani 1 1 d . . . C10 C 0.4621(2) 0.9406(5) 0.9089(10) 0.0127(12) Uani 1 1 d . . . C11 C 0.5407(2) 0.9538(5) 1.0853(10) 0.0128(12) Uani 1 1 d . . . H11 H 0.5683 0.9225 1.1418 0.015 Uiso 1 1 calc R . . C12 C 0.5108(2) 0.7807(5) 0.9871(10) 0.0121(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 Pr1 0.0079(2) 0.00845(19) 0.0161(2) -0.00022(12) -0.00108(13) -0.00124(12) O1 0.015(3) 0.016(2) 0.038(3) 0.009(2) -0.003(2) -0.003(2) O2 0.015(2) 0.011(2) 0.028(3) 0.006(2) -0.004(2) 0.0014(19) O3 0.012(2) 0.015(2) 0.038(3) 0.002(2) -0.007(2) -0.0017(19) O4 0.016(3) 0.012(2) 0.033(3) 0.000(2) -0.004(2) 0.0008(19) O5 0.015(3) 0.008(2) 0.033(3) -0.0052(19) -0.001(2) -0.0017(18) O6 0.012(2) 0.010(2) 0.034(3) 0.005(2) -0.004(2) -0.0003(18) O7 0.015(3) 0.016(2) 0.028(3) -0.003(2) -0.004(2) -0.004(2) O8 0.011(2) 0.014(2) 0.021(3) -0.0021(19) 0.0015(19) 0.0043(18) O9 0.007(2) 0.011(2) 0.023(2) -0.0012(18) -0.0053(18) -0.0004(17) O10 0.019(3) 0.022(3) 0.043(4) -0.008(2) -0.001(2) 0.002(2) O11 0.025(3) 0.041(3) 0.014(3) -0.001(2) -0.001(2) -0.007(3) C1 0.012(3) 0.011(3) 0.011(3) 0.002(2) 0.003(2) -0.001(2) C2 0.016(3) 0.009(3) 0.015(3) 0.001(2) 0.002(2) -0.002(2) C3 0.015(3) 0.010(3) 0.016(3) -0.002(2) 0.004(2) 0.002(2) C4 0.010(3) 0.015(3) 0.015(3) 0.001(2) 0.000(2) -0.001(2) C5 0.013(3) 0.010(3) 0.017(3) 0.000(2) 0.000(2) 0.001(2) C6 0.016(3) 0.008(3) 0.020(3) 0.000(2) 0.003(3) 0.002(2) C7 0.008(3) 0.013(3) 0.015(3) -0.001(2) 0.002(2) 0.001(2) C8 0.013(3) 0.014(3) 0.020(3) 0.004(3) 0.000(3) 0.000(2) C9 0.010(3) 0.010(3) 0.012(3) -0.003(2) -0.001(2) -0.003(2) C10 0.014(3) 0.013(3) 0.010(3) -0.001(2) 0.000(2) -0.001(2) C11 0.010(3) 0.014(3) 0.012(3) -0.003(2) -0.003(2) 0.001(2) C12 0.007(3) 0.009(3) 0.018(3) 0.003(2) -0.001(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O7 2.435(5) . ? Pr1 O1 2.467(5) . ? Pr1 O2 2.473(5) 6_565 ? Pr1 O4 2.483(5) 7_566 ? Pr1 O8 2.491(5) 2_656 ? Pr1 O9 2.542(5) . ? Pr1 O10 2.579(6) . ? Pr1 O11 2.581(5) . ? Pr1 O5 2.640(5) . ? O1 C7 1.260(8) . ? O2 C7 1.265(8) . ? O2 Pr1 2.473(5) 6_566 ? O3 C8 1.274(9) . ? O4 C8 1.259(8) . ? O4 Pr1 2.483(5) 7_566 ? O5 C2 1.377(8) . ? O5 H5 0.8200 . ? O6 C5 1.361(8) . ? O6 H6 0.8200 . ? O7 C12 1.255(8) . ? O8 C12 1.282(8) . ? O8 Pr1 2.491(5) 2_656 ? O9 C10 1.358(8) . ? O9 H9 0.8200 . ? O10 H10A 0.8201 . ? O10 H10B 0.8199 . ? O11 H11A 0.8202 . ? O11 H11B 0.8201 . ? C1 C6 1.390(9) . ? C1 C2 1.419(9) . ? C1 C7 1.505(9) . ? C2 C3 1.377(9) . ? C3 C4 1.409(9) . ? C3 H3 0.9300 . ? C4 C5 1.402(9) . ? C4 C8 1.488(9) . ? C5 C6 1.390(9) . ? C6 H6A 0.9300 . ? C9 C11 1.397(9) . ? C9 C10 1.414(9) . ? C9 C12 1.489(8) . ? C10 C11 1.389(9) 5_677 ? C11 C10 1.389(9) 5_677 ? C11 H11 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 O7 Pr1 O1 95.72(18) . . ? O7 Pr1 O2 144.01(17) . 6_565 ? O1 Pr1 O2 78.82(18) . 6_565 ? O7 Pr1 O4 133.00(17) . 7_566 ? O1 Pr1 O4 126.60(18) . 7_566 ? O2 Pr1 O4 72.33(17) 6_565 7_566 ? O7 Pr1 O8 78.90(18) . 2_656 ? O1 Pr1 O8 135.11(18) . 2_656 ? O2 Pr1 O8 80.44(17) 6_565 2_656 ? O4 Pr1 O8 82.91(18) 7_566 2_656 ? O7 Pr1 O9 65.81(16) . . ? O1 Pr1 O9 141.97(18) . . ? O2 Pr1 O9 135.71(16) 6_565 . ? O4 Pr1 O9 67.89(16) 7_566 . ? O8 Pr1 O9 76.19(16) 2_656 . ? O7 Pr1 O10 71.37(18) . . ? O1 Pr1 O10 67.3(2) . . ? O2 Pr1 O10 73.80(18) 6_565 . ? O4 Pr1 O10 138.76(19) 7_566 . ? O8 Pr1 O10 68.82(18) 2_656 . ? O9 Pr1 O10 128.64(17) . . ? O7 Pr1 O11 72.08(19) . . ? O1 Pr1 O11 71.5(2) . . ? O2 Pr1 O11 135.97(18) 6_565 . ? O4 Pr1 O11 100.33(19) 7_566 . ? O8 Pr1 O11 142.97(18) 2_656 . ? O9 Pr1 O11 71.24(18) . . ? O10 Pr1 O11 120.4(2) . . ? O7 Pr1 O5 132.89(18) . . ? O1 Pr1 O5 62.20(17) . . ? O2 Pr1 O5 75.95(17) 6_565 . ? O4 Pr1 O5 67.66(17) 7_566 . ? O8 Pr1 O5 146.60(17) 2_656 . ? O9 Pr1 O5 105.17(15) . . ? O10 Pr1 O5 124.79(17) . . ? O11 Pr1 O5 61.73(18) . . ? C7 O1 Pr1 140.6(5) . . ? C7 O2 Pr1 138.4(4) . 6_566 ? C8 O4 Pr1 144.6(5) . 7_566 ? C2 O5 Pr1 125.8(4) . . ? C2 O5 H5 109.5 . . ? Pr1 O5 H5 113.5 . . ? C5 O6 H6 109.5 . . ? C12 O7 Pr1 143.8(5) . . ? C12 O8 Pr1 125.2(4) . 2_656 ? C10 O9 Pr1 140.1(4) . . ? C10 O9 H9 109.5 . . ? Pr1 O9 H9 109.8 . . ? Pr1 O10 H10A 105.4 . . ? Pr1 O10 H10B 104.2 . . ? H10A O10 H10B 95.8 . . ? Pr1 O11 H11A 126.2 . . ? Pr1 O11 H11B 111.2 . . ? H11A O11 H11B 103.5 . . ? C6 C1 C2 118.2(6) . . ? C6 C1 C7 118.5(6) . . ? C2 C1 C7 123.3(6) . . ? C3 C2 O5 121.4(6) . . ? C3 C2 C1 120.8(6) . . ? O5 C2 C1 117.8(6) . . ? C2 C3 C4 120.6(6) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 118.9(6) . . ? C5 C4 C8 122.1(6) . . ? C3 C4 C8 119.0(6) . . ? O6 C5 C6 117.8(6) . . ? O6 C5 C4 122.2(6) . . ? C6 C5 C4 120.0(6) . . ? C5 C6 C1 121.5(6) . . ? C5 C6 H6A 119.3 . . ? C1 C6 H6A 119.3 . . ? O1 C7 O2 123.3(6) . . ? O1 C7 C1 119.6(6) . . ? O2 C7 C1 117.2(6) . . ? O4 C8 O3 123.1(7) . . ? O4 C8 C4 119.5(6) . . ? O3 C8 C4 117.3(6) . . ? C11 C9 C10 118.7(6) . . ? C11 C9 C12 118.6(6) . . ? C10 C9 C12 122.5(6) . . ? O9 C10 C11 119.4(6) . 5_677 ? O9 C10 C9 121.7(6) . . ? C11 C10 C9 118.9(6) 5_677 . ? C10 C11 C9 122.4(6) 5_677 . ? C10 C11 H11 118.8 5_677 . ? C9 C11 H11 118.8 . . ? O7 C12 O8 121.9(6) . . ? O7 C12 C9 121.2(6) . . ? O8 C12 C9 116.9(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O6 0.82 1.98 2.702(7) 146.6 4_556 O6 H6 O3 0.82 1.86 2.577(7) 145.8 . O9 H9 O3 0.82 1.75 2.566(7) 171.2 7_566 O10 H10A O1 0.82 1.99 2.777(8) 161.6 6_565 O10 H10B O8 0.82 2.44 2.866(8) 113.5 2_656 O11 H11A O8 0.82 2.01 2.804(7) 162.4 2_657 O11 H11B O2 0.82 2.52 3.212(8) 143.0 6_566 _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 29.07 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 5.479 _refine_diff_density_min -2.235 _refine_diff_density_rms 0.254 #===END OF 2 ## Crystallographic Data for compound 3 data_Nd _database_code_depnum_ccdc_archive 'CCDC 879609' #TrackingRef '- revised Ln.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Nd O13' _chemical_formula_weight 510.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1061(15) _cell_length_b 9.9258(18) _cell_length_c 10.6687(19) _cell_angle_alpha 76.061(2) _cell_angle_beta 74.789(2) _cell_angle_gamma 74.686(2) _cell_volume 785.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5149 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description bolck _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 3.380 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3842 _exptl_absorpt_correction_T_max 0.6872 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7283 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 28.26 _reflns_number_total 3750 _reflns_number_gt 3454 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The final Fourier map had a maximum and a minimum electron density of 2.335 and -1.838 \%A^-3^, respectively, and are within 0.78 \%A of neodymium ion, which resulted from the smear effect of the neodymium ion. ; _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^)+(0.0592P)^2^+0.0917P] 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 3750 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.54325(2) 0.303462(18) 0.144966(16) 0.01975(8) Uani 1 1 d . . . O1 O 0.7301(4) 0.2218(3) -0.0598(3) 0.0346(7) Uani 1 1 d . . . O1W O 0.1624(4) 0.0774(3) 0.0130(3) 0.0417(7) Uani 1 1 d . . . H1WA H 0.0689 0.1156 0.0552 0.062 Uiso 1 1 d R . . H1WB H 0.1978 -0.0091 0.0284 0.062 Uiso 1 1 d R . . O2 O 0.6095(3) 0.4459(3) -0.1070(3) 0.0278(6) Uani 1 1 d . . . O3 O 1.2819(3) 0.2925(3) -0.6880(3) 0.0264(6) Uani 1 1 d . . . O4 O 1.0429(3) 0.3810(3) -0.7687(3) 0.0293(6) Uani 1 1 d . . . O5 O 0.5607(4) 0.4656(4) -0.3756(4) 0.0518(10) Uani 1 1 d . . . H5 H 0.5208 0.4793 -0.2996 0.078 Uiso 1 1 calc R . . O6 O 1.2647(3) 0.2149(3) -0.4369(3) 0.0339(7) Uani 1 1 d . . . H6 H 1.3135 0.2202 -0.5151 0.051 Uiso 1 1 calc R . . O7 O 0.6180(3) 0.2022(3) 0.3636(3) 0.0303(6) Uani 1 1 d . . . O8 O 0.8314(3) 0.1517(3) 0.1960(3) 0.0278(6) Uani 1 1 d . . . O9 O 0.6494(3) 0.0900(3) 0.6021(3) 0.0305(6) Uani 1 1 d . . . H9 H 0.5955 0.1235 0.5426 0.046 Uiso 1 1 calc R . . O10 O 0.5314(4) 0.0495(3) 0.1717(3) 0.0355(7) Uani 1 1 d . . . H10A H 0.6180 -0.0152 0.1617 0.053 Uiso 1 1 d R . . H10B H 0.4818 0.0104 0.2432 0.053 Uiso 1 1 d R . . O11 O 0.2993(3) 0.3010(3) 0.0336(3) 0.0275(6) Uani 1 1 d . . . H11A H 0.2114 0.3157 0.0920 0.041 Uiso 1 1 d R . . H11B H 0.2893 0.2275 0.0167 0.041 Uiso 1 1 d R . . O12 O 0.7354(4) 0.4553(4) 0.1503(4) 0.0506(10) Uani 1 1 d . . . H12A H 0.7132 0.5364 0.1085 0.076 Uiso 1 1 d R . . H12B H 0.8252 0.4258 0.1793 0.076 Uiso 1 1 d R . . C1 C 0.8124(5) 0.3377(4) -0.2815(4) 0.0216(7) Uani 1 1 d . . . C2 C 0.7362(4) 0.4026(4) -0.3900(4) 0.0252(7) Uani 1 1 d . . . C3 C 0.8361(4) 0.3999(4) -0.5147(4) 0.0234(7) Uani 1 1 d . . . H3A H 0.7839 0.4405 -0.5868 0.028 Uiso 1 1 calc R . . C4 C 1.0145(4) 0.3380(4) -0.5366(3) 0.0201(6) Uani 1 1 d . . . C5 C 1.0916(4) 0.2760(4) -0.4266(4) 0.0218(7) Uani 1 1 d . . . C6 C 0.9887(5) 0.2733(4) -0.3005(4) 0.0238(7) Uani 1 1 d . . . H6A H 1.0382 0.2278 -0.2278 0.029 Uiso 1 1 calc R . . C7 C 0.7116(4) 0.3343(4) -0.1428(3) 0.0209(7) Uani 1 1 d . . . C8 C 1.1180(4) 0.3384(4) -0.6739(4) 0.0209(7) Uani 1 1 d . . . C9 C 0.8216(4) 0.0468(4) 0.5493(4) 0.0211(7) Uani 1 1 d . . . C10 C 0.8900(5) 0.0683(4) 0.4125(4) 0.0211(7) Uani 1 1 d . . . C11 C 1.0673(4) 0.0212(4) 0.3659(4) 0.0220(7) Uani 1 1 d . . . H11 H 1.1125 0.0358 0.2753 0.026 Uiso 1 1 calc R . . C12 C 0.7761(4) 0.1431(4) 0.3178(4) 0.0219(7) 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 Nd1 0.01595(11) 0.02534(12) 0.01209(11) -0.00161(8) 0.00031(7) 0.00055(7) O1 0.0418(16) 0.0309(14) 0.0172(13) -0.0014(11) 0.0031(12) 0.0033(12) O1W 0.0412(17) 0.0367(16) 0.0407(19) -0.0126(14) 0.0041(15) -0.0052(13) O2 0.0251(13) 0.0262(13) 0.0241(14) -0.0103(11) 0.0062(11) 0.0023(10) O3 0.0184(12) 0.0395(15) 0.0161(12) -0.0071(11) 0.0022(10) -0.0013(10) O4 0.0243(13) 0.0445(16) 0.0157(13) -0.0066(12) -0.0022(11) -0.0028(11) O5 0.0209(14) 0.068(2) 0.041(2) 0.0046(17) 0.0035(14) 0.0108(14) O6 0.0170(12) 0.0539(18) 0.0204(14) -0.0075(13) 0.0015(11) 0.0051(12) O7 0.0198(12) 0.0435(16) 0.0176(13) -0.0022(12) -0.0024(10) 0.0055(11) O8 0.0219(12) 0.0369(15) 0.0169(13) -0.0030(11) -0.0034(10) 0.0043(10) O9 0.0188(12) 0.0421(16) 0.0182(13) 0.0036(12) -0.0008(11) 0.0032(11) O10 0.0356(15) 0.0293(14) 0.0302(16) -0.0019(12) 0.0085(13) -0.0062(12) O11 0.0257(13) 0.0370(15) 0.0198(13) -0.0096(11) -0.0009(11) -0.0068(11) O12 0.0438(19) 0.0407(18) 0.074(3) 0.0164(18) -0.0411(19) -0.0161(15) C1 0.0239(17) 0.0209(16) 0.0165(17) -0.0054(13) 0.0008(14) -0.0022(13) C2 0.0166(15) 0.0318(18) 0.0205(18) -0.0043(15) 0.0009(14) 0.0010(13) C3 0.0195(16) 0.0302(18) 0.0170(17) -0.0032(14) -0.0018(14) -0.0023(13) C4 0.0200(15) 0.0231(16) 0.0150(16) -0.0065(13) 0.0005(13) -0.0021(12) C5 0.0181(15) 0.0257(17) 0.0186(17) -0.0065(14) -0.0019(13) 0.0005(12) C6 0.0245(17) 0.0265(17) 0.0155(17) -0.0050(14) -0.0020(14) 0.0017(13) C7 0.0184(15) 0.0265(17) 0.0149(16) -0.0068(13) 0.0015(13) -0.0021(12) C8 0.0198(16) 0.0232(16) 0.0170(16) -0.0048(13) 0.0012(13) -0.0043(12) C9 0.0207(16) 0.0214(16) 0.0177(17) -0.0036(13) -0.0010(14) -0.0017(12) C10 0.0193(16) 0.0229(16) 0.0183(17) -0.0035(14) -0.0042(14) 0.0001(12) C11 0.0221(16) 0.0236(16) 0.0152(16) -0.0016(13) -0.0003(13) -0.0019(12) C12 0.0210(16) 0.0209(15) 0.0209(17) -0.0018(13) -0.0048(14) -0.0013(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O3 2.392(3) 1_456 ? Nd1 O12 2.455(3) . ? Nd1 O2 2.457(3) 2_665 ? Nd1 O7 2.472(3) . ? Nd1 O1 2.488(3) . ? Nd1 O10 2.492(3) . ? Nd1 O8 2.537(2) . ? Nd1 O11 2.568(3) . ? Nd1 O2 2.706(3) . ? Nd1 C12 2.885(3) . ? O1 C7 1.248(4) . ? O1W H1WA 0.8200 . ? O1W H1WB 0.8200 . ? O2 C7 1.269(4) . ? O2 Nd1 2.457(3) 2_665 ? O3 C8 1.267(4) . ? O3 Nd1 2.392(3) 1_654 ? O4 C8 1.246(4) . ? O5 C2 1.379(4) . ? O5 H5 0.8200 . ? O6 C5 1.360(4) . ? O6 H6 0.8200 . ? O7 C12 1.280(4) . ? O8 C12 1.247(4) . ? O9 C9 1.356(4) . ? O9 H9 0.8200 . ? O10 H10A 0.8200 . ? O10 H10B 0.8200 . ? O11 H11A 0.8200 . ? O11 H11B 0.8200 . ? O12 H12A 0.8200 . ? O12 H12B 0.8200 . ? C1 C6 1.386(5) . ? C1 C2 1.393(5) . ? C1 C7 1.489(5) . ? C2 C3 1.366(5) . ? C3 C4 1.395(5) . ? C3 H3A 0.9300 . ? C4 C5 1.407(5) . ? C4 C8 1.485(5) . ? C5 C6 1.383(5) . ? C6 H6A 0.9300 . ? C9 C11 1.377(5) 2_756 ? C9 C10 1.404(5) . ? C10 C11 1.383(5) . ? C10 C12 1.480(5) . ? C11 C9 1.377(5) 2_756 ? C11 H11 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 O3 Nd1 O12 119.67(12) 1_456 . ? O3 Nd1 O2 80.22(9) 1_456 2_665 ? O12 Nd1 O2 70.33(10) . 2_665 ? O3 Nd1 O7 70.00(9) 1_456 . ? O12 Nd1 O7 78.72(11) . . ? O2 Nd1 O7 117.40(9) 2_665 . ? O3 Nd1 O1 146.63(11) 1_456 . ? O12 Nd1 O1 93.68(13) . . ? O2 Nd1 O1 113.39(9) 2_665 . ? O7 Nd1 O1 121.82(9) . . ? O3 Nd1 O10 79.30(10) 1_456 . ? O12 Nd1 O10 142.01(10) . . ? O2 Nd1 O10 147.63(10) 2_665 . ? O7 Nd1 O10 78.16(10) . . ? O1 Nd1 O10 73.85(10) . . ? O3 Nd1 O8 118.64(9) 1_456 . ? O12 Nd1 O8 69.87(10) . . ? O2 Nd1 O8 140.15(9) 2_665 . ? O7 Nd1 O8 51.81(8) . . ? O1 Nd1 O8 71.25(9) . . ? O10 Nd1 O8 72.14(10) . . ? O3 Nd1 O11 71.97(9) 1_456 . ? O12 Nd1 O11 141.43(10) . . ? O2 Nd1 O11 76.59(9) 2_665 . ? O7 Nd1 O11 135.78(9) . . ? O1 Nd1 O11 81.54(10) . . ? O10 Nd1 O11 73.37(10) . . ? O8 Nd1 O11 140.68(9) . . ? O3 Nd1 O2 133.61(8) 1_456 . ? O12 Nd1 O2 76.41(11) . . ? O2 Nd1 O2 64.16(9) 2_665 . ? O7 Nd1 O2 152.53(9) . . ? O1 Nd1 O2 49.25(8) . . ? O10 Nd1 O2 115.82(9) . . ? O8 Nd1 O2 107.73(8) . . ? O11 Nd1 O2 71.61(9) . . ? O3 Nd1 C12 94.80(10) 1_456 . ? O12 Nd1 C12 72.14(10) . . ? O2 Nd1 C12 132.88(10) 2_665 . ? O7 Nd1 C12 26.23(9) . . ? O1 Nd1 C12 96.33(10) . . ? O10 Nd1 C12 73.79(10) . . ? O8 Nd1 C12 25.58(9) . . ? O11 Nd1 C12 146.32(10) . . ? O2 Nd1 C12 131.04(9) . . ? C7 O1 Nd1 101.1(2) . . ? H1WA O1W H1WB 120.9 . . ? C7 O2 Nd1 154.0(2) . 2_665 ? C7 O2 Nd1 90.1(2) . . ? Nd1 O2 Nd1 115.84(9) 2_665 . ? C8 O3 Nd1 139.5(2) . 1_654 ? C2 O5 H5 109.5 . . ? C5 O6 H6 109.5 . . ? C12 O7 Nd1 95.2(2) . . ? C12 O8 Nd1 93.0(2) . . ? C9 O9 H9 109.5 . . ? Nd1 O10 H10A 124.1 . . ? Nd1 O10 H10B 118.4 . . ? H10A O10 H10B 96.4 . . ? Nd1 O11 H11A 102.2 . . ? Nd1 O11 H11B 121.5 . . ? H11A O11 H11B 100.5 . . ? Nd1 O12 H12A 114.4 . . ? Nd1 O12 H12B 123.9 . . ? H12A O12 H12B 120.8 . . ? C6 C1 C2 120.1(3) . . ? C6 C1 C7 117.4(3) . . ? C2 C1 C7 122.6(3) . . ? C3 C2 O5 118.6(3) . . ? C3 C2 C1 119.4(3) . . ? O5 C2 C1 121.9(3) . . ? C2 C3 C4 121.7(3) . . ? C2 C3 H3A 119.2 . . ? C4 C3 H3A 119.2 . . ? C3 C4 C5 118.6(3) . . ? C3 C4 C8 119.8(3) . . ? C5 C4 C8 121.6(3) . . ? O6 C5 C6 117.0(3) . . ? O6 C5 C4 123.4(3) . . ? C6 C5 C4 119.6(3) . . ? C5 C6 C1 120.5(3) . . ? C5 C6 H6A 119.7 . . ? C1 C6 H6A 119.7 . . ? O1 C7 O2 119.5(3) . . ? O1 C7 C1 119.9(3) . . ? O2 C7 C1 120.6(3) . . ? O4 C8 O3 123.0(3) . . ? O4 C8 C4 120.0(3) . . ? O3 C8 C4 116.9(3) . . ? O9 C9 C11 118.2(3) . 2_756 ? O9 C9 C10 122.6(3) . . ? C11 C9 C10 119.2(3) 2_756 . ? C11 C10 C9 119.3(3) . . ? C11 C10 C12 119.6(3) . . ? C9 C10 C12 121.1(3) . . ? C9 C11 C10 121.5(3) 2_756 . ? C9 C11 H11 119.2 2_756 . ? C10 C11 H11 119.2 . . ? O8 C12 O7 120.0(3) . . ? O8 C12 C10 121.8(3) . . ? O7 C12 C10 118.2(3) . . ? O8 C12 Nd1 61.44(17) . . ? O7 C12 Nd1 58.58(17) . . ? C10 C12 Nd1 176.0(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O8 0.82 2.11 2.908(4) 162.9 1_455 O1W H1WB O1 0.82 2.01 2.824(4) 175.6 2_655 O5 H5 O2 0.82 2.27 2.948(5) 139.7 . O6 H6 O3 0.82 1.87 2.580(4) 144.3 . O9 H9 O7 0.82 1.86 2.570(4) 144.0 . O10 H10A O1W 0.82 2.29 2.934(4) 135.5 2_655 O10 H10B O9 0.82 1.92 2.738(4) 172.6 2_656 O11 H11A O4 0.82 1.85 2.652(4) 165.2 1_456 O11 H11B O1W 0.82 2.04 2.805(4) 156.3 . O12 H12A O11 0.82 1.93 2.725(4) 162.7 2_665 O12 H12B O4 0.82 1.90 2.712(4) 171.9 1_556 _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 2.335 _refine_diff_density_min -1.838 _refine_diff_density_rms 0.180 #===END OF 3 ## Crystallographic Data for compound 4 data_Eu _database_code_depnum_ccdc_archive 'CCDC 879610' #TrackingRef '- revised Ln.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H16 Eu N O15' _chemical_formula_weight 518.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 15.5221(1) _cell_length_b 15.5219(6) _cell_length_c 6.4783(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1560.81(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8373 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 28.30 _exptl_crystal_description bolck _exptl_crystal_colour brown _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 4.103 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2541 _exptl_absorpt_correction_T_max 0.7622 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13964 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0132 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 28.30 _reflns_number_total 2012 _reflns_number_gt 1883 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+0.9990P] 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 2012 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0182 _refine_ls_R_factor_gt 0.0164 _refine_ls_wR_factor_ref 0.0415 _refine_ls_wR_factor_gt 0.0407 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Eu1 Eu 0.282072(8) 0.7500 0.099551(19) 0.01525(5) Uani 1 2 d S . . O1 O 0.32245(10) 0.65341(11) 0.3963(2) 0.0277(3) Uani 1 1 d . . . O1W O 0.30112(11) 0.44586(12) 0.1006(2) 0.0311(4) Uani 1 1 d . . . H1WB H 0.2648 0.4172 0.0394 0.047 Uiso 1 1 d R . . H1WA H 0.3473 0.4381 0.0423 0.047 Uiso 1 1 d R . . O2 O 0.41187(10) 0.65771(11) 0.1366(2) 0.0318(4) Uani 1 1 d . . . O3 O 0.54842(10) 0.56774(12) 0.1235(2) 0.0328(4) Uani 1 1 d . . . H3 H 0.5130 0.6033 0.0842 0.049 Uiso 1 1 calc R . . O4 O 0.23662(11) 0.60691(10) 0.0031(3) 0.0325(3) Uani 1 1 d . . . H4A H 0.2176 0.6077 -0.1150 0.049 Uiso 1 1 d R . . H4B H 0.2681 0.5713 0.0585 0.049 Uiso 1 1 d R . . O5 O 0.15704(15) 0.7500 0.3127(4) 0.0385(5) Uani 1 2 d S . . H5B H 0.1078 0.7331 0.2902 0.058 Uiso 0.50 1 d PR . . H5A H 0.1500 0.7665 0.4319 0.058 Uiso 0.50 1 d PR . . O6 O 0.35688(13) 0.7500 -0.2221(3) 0.0277(4) Uani 1 2 d S . . H6B H 0.3274 0.7274 -0.3121 0.042 Uiso 0.50 1 d PR . . H6A H 0.4042 0.7728 -0.2095 0.042 Uiso 0.50 1 d PR . . O7 O 0.16322(14) 0.7500 -0.1722(4) 0.0332(5) Uani 1 2 d S . . O8 O 0.04123(17) 0.7500 -0.0048(4) 0.0512(7) Uani 1 2 d S . . O9 O 0.04260(17) 0.7500 -0.3340(4) 0.0636(10) Uani 1 2 d S . . C1 C 0.52300(12) 0.53455(13) 0.3088(3) 0.0218(4) Uani 1 1 d . . . C2 C 0.44821(13) 0.56310(13) 0.4103(3) 0.0204(4) Uani 1 1 d . . . C3 C 0.42689(13) 0.52858(14) 0.6015(3) 0.0236(4) Uani 1 1 d . . . H3A H 0.3781 0.5483 0.6701 0.028 Uiso 1 1 calc R . . C4 C 0.39145(12) 0.62818(12) 0.3118(3) 0.0210(4) Uani 1 1 d . . . N1 N 0.08179(17) 0.7500 -0.1680(4) 0.0305(6) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.01612(8) 0.01481(8) 0.01483(8) 0.000 -0.00154(4) 0.000 O1 0.0257(8) 0.0312(8) 0.0263(7) 0.0073(6) 0.0012(6) 0.0115(6) O1W 0.0290(8) 0.0304(9) 0.0340(9) -0.0012(7) 0.0043(6) 0.0006(7) O2 0.0273(8) 0.0384(9) 0.0298(7) 0.0168(7) 0.0030(6) 0.0119(7) O3 0.0258(8) 0.0431(10) 0.0293(8) 0.0179(7) 0.0066(6) 0.0112(7) O4 0.0429(9) 0.0194(7) 0.0350(9) -0.0016(7) -0.0129(8) -0.0021(6) O5 0.0285(11) 0.0543(16) 0.0327(12) 0.000 0.0105(10) 0.000 O6 0.0240(10) 0.0418(13) 0.0175(9) 0.000 -0.0010(8) 0.000 O7 0.0232(10) 0.0370(12) 0.0393(12) 0.000 -0.0077(10) 0.000 O8 0.0384(14) 0.085(2) 0.0306(13) 0.000 0.0037(11) 0.000 O9 0.0305(13) 0.132(3) 0.0279(13) 0.000 -0.0089(11) 0.000 C1 0.0198(9) 0.0246(10) 0.0209(9) 0.0045(8) -0.0001(7) 0.0013(7) C2 0.0190(9) 0.0193(9) 0.0230(9) 0.0026(7) -0.0037(7) 0.0020(7) C3 0.0192(9) 0.0273(11) 0.0244(10) 0.0034(8) 0.0013(7) 0.0047(8) C4 0.0202(8) 0.0197(9) 0.0230(9) 0.0013(7) -0.0053(7) 0.0008(7) N1 0.0280(13) 0.0352(14) 0.0283(13) 0.000 -0.0064(11) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O5 2.382(2) . ? Eu1 O6 2.385(2) . ? Eu1 O4 2.4127(15) 7_575 ? Eu1 O4 2.4127(15) . ? Eu1 O2 2.4836(15) 7_575 ? Eu1 O2 2.4836(15) . ? Eu1 O1 2.5172(14) 7_575 ? Eu1 O1 2.5172(14) . ? Eu1 O7 2.550(2) . ? Eu1 C4 2.8892(19) 7_575 ? Eu1 C4 2.8892(19) . ? Eu1 H4A 2.7951 . ? Eu1 H4B 2.7948 . ? Eu1 H6B 2.7804 . ? Eu1 H6A 2.7804 . ? O1 C4 1.265(2) . ? O1W H1WB 0.8200 . ? O1W H1WA 0.8200 . ? O2 C4 1.264(2) . ? O3 C1 1.365(2) . ? O3 H3 0.8200 . ? O4 H4A 0.8200 . ? O4 H4B 0.8200 . ? O5 H5B 0.8200 . ? O5 H5A 0.8200 . ? O6 H6B 0.8200 . ? O6 H6A 0.8200 . ? O7 N1 1.264(3) . ? O8 N1 1.231(4) . ? O9 N1 1.236(4) . ? C1 C3 1.379(3) 5_666 ? C1 C2 1.406(3) . ? C2 C3 1.390(3) . ? C2 C4 1.485(3) . ? C3 C1 1.379(3) 5_666 ? C3 H3A 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 Eu1 O6 154.56(8) . . ? O5 Eu1 O4 84.94(5) . 7_575 ? O6 Eu1 O4 85.19(5) . 7_575 ? O5 Eu1 O4 84.94(5) . . ? O6 Eu1 O4 85.19(5) . . ? O4 Eu1 O4 134.02(8) 7_575 . ? O5 Eu1 O2 127.23(5) . 7_575 ? O6 Eu1 O2 71.91(5) . 7_575 ? O4 Eu1 O2 74.41(6) 7_575 7_575 ? O4 Eu1 O2 142.48(6) . 7_575 ? O5 Eu1 O2 127.23(5) . . ? O6 Eu1 O2 71.91(5) . . ? O4 Eu1 O2 142.48(6) 7_575 . ? O4 Eu1 O2 74.41(6) . . ? O2 Eu1 O2 70.45(8) 7_575 . ? O5 Eu1 O1 76.12(6) . 7_575 ? O6 Eu1 O1 123.09(5) . 7_575 ? O4 Eu1 O1 73.87(6) 7_575 7_575 ? O4 Eu1 O1 144.97(6) . 7_575 ? O2 Eu1 O1 51.74(5) 7_575 7_575 ? O2 Eu1 O1 93.89(6) . 7_575 ? O5 Eu1 O1 76.12(6) . . ? O6 Eu1 O1 123.09(5) . . ? O4 Eu1 O1 144.97(6) 7_575 . ? O4 Eu1 O1 73.87(6) . . ? O2 Eu1 O1 93.89(6) 7_575 . ? O2 Eu1 O1 51.74(5) . . ? O1 Eu1 O1 73.11(8) 7_575 . ? O5 Eu1 O7 79.08(8) . . ? O6 Eu1 O7 75.47(7) . . ? O4 Eu1 O7 67.03(4) 7_575 . ? O4 Eu1 O7 67.03(4) . . ? O2 Eu1 O7 130.81(5) 7_575 . ? O2 Eu1 O7 130.81(5) . . ? O1 Eu1 O7 135.02(5) 7_575 . ? O1 Eu1 O7 135.02(5) . . ? O5 Eu1 C4 101.71(6) . 7_575 ? O6 Eu1 C4 97.45(5) . 7_575 ? O4 Eu1 C4 72.10(5) 7_575 7_575 ? O4 Eu1 C4 153.83(5) . 7_575 ? O2 Eu1 C4 25.83(5) 7_575 7_575 ? O2 Eu1 C4 81.65(6) . 7_575 ? O1 Eu1 C4 25.91(5) 7_575 7_575 ? O1 Eu1 C4 83.11(6) . 7_575 ? O7 Eu1 C4 138.91(4) . 7_575 ? O5 Eu1 C4 101.71(6) . . ? O6 Eu1 C4 97.45(5) . . ? O4 Eu1 C4 153.83(5) 7_575 . ? O4 Eu1 C4 72.10(5) . . ? O2 Eu1 C4 81.65(6) 7_575 . ? O2 Eu1 C4 25.83(5) . . ? O1 Eu1 C4 83.11(6) 7_575 . ? O1 Eu1 C4 25.91(5) . . ? O7 Eu1 C4 138.91(4) . . ? C4 Eu1 C4 81.75(8) 7_575 . ? O5 Eu1 H4A 89.8 . . ? O6 Eu1 H4A 74.9 . . ? O4 Eu1 H4A 119.6 7_575 . ? O4 Eu1 H4A 16.1 . . ? O2 Eu1 H4A 142.6 7_575 . ? O2 Eu1 H4A 83.3 . . ? O1 Eu1 H4A 160.0 7_575 . ? O1 Eu1 H4A 89.9 . . ? O7 Eu1 H4A 53.0 . . ? C4 Eu1 H4A 164.6 7_575 . ? C4 Eu1 H4A 86.0 . . ? O5 Eu1 H4B 89.5 . . ? O6 Eu1 H4B 87.4 . . ? O4 Eu1 H4B 150.0 7_575 . ? O4 Eu1 H4B 16.1 . . ? O2 Eu1 H4B 130.1 7_575 . ? O2 Eu1 H4B 60.0 . . ? O1 Eu1 H4B 133.1 7_575 . ? O1 Eu1 H4B 60.1 . . ? O7 Eu1 H4B 83.0 . . ? C4 Eu1 H4B 137.8 7_575 . ? C4 Eu1 H4B 56.0 . . ? H4A Eu1 H4B 30.7 . . ? O5 Eu1 H6B 139.7 . . ? O6 Eu1 H6B 16.0 . . ? O4 Eu1 H6B 86.7 7_575 . ? O4 Eu1 H6B 73.1 . . ? O2 Eu1 H6B 87.7 7_575 . ? O2 Eu1 H6B 79.3 . . ? O1 Eu1 H6B 138.1 7_575 . ? O1 Eu1 H6B 126.5 . . ? O7 Eu1 H6B 61.4 . . ? C4 Eu1 H6B 113.0 7_575 . ? C4 Eu1 H6B 103.0 . . ? H4A Eu1 H6B 60.9 . . ? H4B Eu1 H6B 78.7 . . ? O5 Eu1 H6A 166.7 . . ? O6 Eu1 H6A 16.0 . . ? O4 Eu1 H6A 84.0 7_575 . ? O4 Eu1 H6A 97.5 . . ? O2 Eu1 H6A 56.1 7_575 . ? O2 Eu1 H6A 65.8 . . ? O1 Eu1 H6A 107.7 7_575 . ? O1 Eu1 H6A 117.1 . . ? O7 Eu1 H6A 89.8 . . ? C4 Eu1 H6A 81.9 7_575 . ? C4 Eu1 H6A 91.4 . . ? H4A Eu1 H6A 89.2 . . ? H4B Eu1 H6A 96.4 . . ? H6B Eu1 H6A 32.1 . . ? C4 O1 Eu1 93.70(12) . . ? H1WB O1W H1WA 107.3 . . ? C4 O2 Eu1 95.31(12) . . ? C1 O3 H3 109.5 . . ? Eu1 O4 H4A 109.5 . . ? Eu1 O4 H4B 109.4 . . ? H4A O4 H4B 129.2 . . ? Eu1 O5 H5B 131.0 . . ? Eu1 O5 H5A 130.8 . . ? H5B O5 H5A 98.2 . . ? Eu1 O6 H6B 110.5 . . ? Eu1 O6 H6A 110.5 . . ? H6B O6 H6A 139.1 . . ? N1 O7 Eu1 135.1(2) . . ? O3 C1 C3 118.40(18) . 5_666 ? O3 C1 C2 122.09(17) . . ? C3 C1 C2 119.52(18) 5_666 . ? C3 C2 C1 119.47(18) . . ? C3 C2 C4 120.28(18) . . ? C1 C2 C4 120.23(17) . . ? C1 C3 C2 121.00(19) 5_666 . ? C1 C3 H3A 119.5 5_666 . ? C2 C3 H3A 119.5 . . ? O2 C4 O1 119.25(18) . . ? O2 C4 C2 118.94(18) . . ? O1 C4 C2 121.80(18) . . ? O2 C4 Eu1 58.86(10) . . ? O1 C4 Eu1 60.39(10) . . ? C2 C4 Eu1 176.96(14) . . ? O8 N1 O9 119.7(3) . . ? O8 N1 O7 122.0(3) . . ? O9 N1 O7 118.3(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 1.81 2.540(2) 146.7 . O4 H4B O1W 0.82 2.03 2.766(2) 148.7 . O4 H4A O1W 0.82 2.04 2.795(2) 152.5 2_564 O5 H5A O9 0.82 2.27 2.897(4) 133.7 1_556 O5 H5B O8 0.82 2.19 2.732(4) 123.8 . O6 H6A O9 0.82 2.19 2.906(3) 145.1 6_655 O6 H6B O1 0.82 2.21 2.940(2) 148.1 1_554 O1W H1WA O3 0.82 1.94 2.758(2) 171.8 5_665 O1W H1WB O1 0.82 1.97 2.794(2) 178.9 2_564 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.895 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.078 #===END OF 4 ## Crystallographic Data for compound 5 data_Gd _database_code_depnum_ccdc_archive 'CCDC 879611' #TrackingRef '- revised Ln.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H23 Gd2 O22' _chemical_formula_weight 929.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3991(9) _cell_length_b 11.4730(14) _cell_length_c 16.2335(19) _cell_angle_alpha 79.038(2) _cell_angle_beta 82.588(2) _cell_angle_gamma 79.972(2) _cell_volume 1325.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2096 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 26.63 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 894 _exptl_absorpt_coefficient_mu 5.063 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3527 _exptl_absorpt_correction_T_max 0.7182 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8325 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 29.04 _reflns_number_total 6123 _reflns_number_gt 4608 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+2.6918P] 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 6123 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.94417(4) 0.06378(3) -0.227338(19) 0.01345(9) Uani 1 1 d . . . Gd2 Gd 0.44670(4) 0.26273(3) -0.236454(19) 0.01528(9) Uani 1 1 d . . . O1 O 0.9287(6) 0.2187(4) -0.1456(3) 0.0240(11) Uani 1 1 d . . . O1W O 0.5159(10) 0.8254(7) -0.2224(4) 0.065(2) Uani 1 1 d . . . O2 O 0.7046(6) 0.3415(4) -0.2101(3) 0.0240(11) Uani 1 1 d . . . O2W O 0.9948(11) 0.3701(8) 0.2572(5) 0.088(3) Uani 1 1 d . . . H2WA H 1.0536 0.4140 0.2736 0.132 Uiso 1 1 d R . . H2WB H 0.9597 0.4287 0.2224 0.132 Uiso 1 1 d R . . O3 O 0.7374(7) 0.5615(5) 0.1812(3) 0.0337(13) Uani 1 1 d . . . O3W O 1.2172(13) -0.2413(7) -0.3725(5) 0.092(3) Uani 1 1 d . . . H3WA H 1.2153 -0.2360 -0.4235 0.138 Uiso 1 1 d R . . H3WB H 1.2030 -0.3062 -0.3431 0.138 Uiso 1 1 d R . . O4 O 0.6208(7) 0.7154(4) 0.0905(3) 0.0271(12) Uani 1 1 d . . . O4W O 0.6494(14) 0.6337(7) -0.3363(6) 0.110(4) Uani 1 1 d . . . H4WA H 0.7058 0.6601 -0.3808 0.166 Uiso 1 1 d R . . H4WB H 0.5552 0.6686 -0.3137 0.166 Uiso 1 1 d R . . O5 O 0.9845(8) 0.2436(5) 0.0065(3) 0.0390(14) Uani 1 1 d . . . H5A H 0.9977 0.2086 -0.0339 0.058 Uiso 1 1 calc R . . O6 O 0.5760(9) 0.6945(5) -0.0606(4) 0.0471(16) Uani 1 1 d . . . H6B H 0.5659 0.7288 -0.0199 0.071 Uiso 1 1 calc R . . O7 O 0.9813(6) 0.2202(4) -0.3455(3) 0.0222(11) Uani 1 1 d . . . O8 O 1.1972(7) 0.3134(5) -0.3164(3) 0.0349(13) Uani 1 1 d . . . O9 O 0.7946(7) 0.3155(4) -0.4725(3) 0.0298(12) Uani 1 1 d . . . H9 H 0.8419 0.2576 -0.4402 0.045 Uiso 1 1 calc R . . O10 O 0.6017(7) 0.1614(4) -0.3421(3) 0.0230(11) Uani 1 1 d . . . O11 O 0.8080(7) -0.0027(4) -0.3376(3) 0.0279(12) Uani 1 1 d . . . O12 O 0.2059(7) 0.1587(5) -0.5644(3) 0.0382(14) Uani 1 1 d . . . H12 H 0.1532 0.1277 -0.5940 0.057 Uiso 1 1 calc R . . O13 O 0.2716(6) 0.1042(4) -0.1990(3) 0.0173(10) Uani 1 1 d . . . O14 O 0.1160(6) -0.0211(4) -0.1113(3) 0.0225(11) Uani 1 1 d . . . O15 O 0.6342(6) 0.0895(4) -0.1648(3) 0.0158(9) Uani 1 1 d . . . O16 O 1.1927(7) -0.0492(5) -0.3005(3) 0.0355(13) Uani 1 1 d . . . H16A H 1.2924 -0.0698 -0.2809 0.053 Uiso 1 1 d R . . H16B H 1.2044 -0.1072 -0.3244 0.053 Uiso 1 1 d R . . O17 O 0.8887(7) -0.1426(4) -0.1727(3) 0.0347(13) Uani 1 1 d . . . H17A H 0.7989 -0.1740 -0.1756 0.052 Uiso 1 1 d R . . H17B H 0.9290 -0.1926 -0.1335 0.052 Uiso 1 1 d R . . O18 O 0.5219(7) 0.4240(5) -0.3525(3) 0.0326(13) Uani 1 1 d . . . H18A H 0.5619 0.4823 -0.3436 0.049 Uiso 1 1 d R . . H18B H 0.5686 0.3970 -0.3950 0.049 Uiso 1 1 d R . . C1 C 0.7960(9) 0.3923(6) -0.0877(4) 0.0191(14) Uani 1 1 d . . . C2 C 0.8712(10) 0.3502(6) -0.0109(4) 0.0218(15) Uani 1 1 d . . . C3 C 0.8354(10) 0.4191(6) 0.0525(4) 0.0239(16) Uani 1 1 d . . . H3A H 0.8771 0.3879 0.1050 0.029 Uiso 1 1 calc R . . C4 C 0.7381(9) 0.5337(6) 0.0378(4) 0.0218(15) Uani 1 1 d . . . C5 C 0.6735(10) 0.5803(6) -0.0411(4) 0.0212(15) Uani 1 1 d . . . C6 C 0.6980(9) 0.5090(6) -0.1024(4) 0.0235(15) Uani 1 1 d . . . H6A H 0.6492 0.5385 -0.1537 0.028 Uiso 1 1 calc R . . C7 C 0.8110(9) 0.3133(6) -0.1519(4) 0.0215(15) Uani 1 1 d . . . C8 C 0.7009(9) 0.6064(6) 0.1069(4) 0.0227(15) Uani 1 1 d . . . C9 C 0.9005(10) 0.4054(6) -0.4853(4) 0.0211(15) Uani 1 1 d . . . C10 C 1.0342(9) 0.4060(6) -0.4335(4) 0.0173(14) Uani 1 1 d . . . C11 C 1.1343(9) 0.5010(6) -0.4477(4) 0.0220(15) Uani 1 1 d . . . H11 H 1.2238 0.5021 -0.4126 0.026 Uiso 1 1 calc R . . C12 C 1.0741(9) 0.3053(6) -0.3596(4) 0.0184(14) Uani 1 1 d . . . C13 C 0.3502(9) 0.0782(6) -0.5334(4) 0.0222(15) Uani 1 1 d . . . C14 C 0.4359(10) 0.1068(6) -0.4710(4) 0.0232(16) Uani 1 1 d . . . H14A H 0.3934 0.1789 -0.4518 0.028 Uiso 1 1 calc R . . C15 C 0.5852(10) 0.0299(6) -0.4361(4) 0.0225(15) Uani 1 1 d . . . C16 C 0.6693(10) 0.0652(6) -0.3670(4) 0.0201(15) Uani 1 1 d . . . C17 C 0.6760(9) 0.0267(5) -0.0178(4) 0.0161(13) Uani 1 1 d . . . H17 H 0.7961 0.0436 -0.0289 0.019 Uiso 1 1 calc R . . C18 C 0.5676(9) 0.0453(5) -0.0854(4) 0.0151(13) Uani 1 1 d . . . C19 C 0.3881(8) 0.0159(6) -0.0649(4) 0.0153(13) Uani 1 1 d . . . C20 C 0.2546(9) 0.0329(6) -0.1275(4) 0.0166(14) 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 0.01392(17) 0.01588(17) 0.01160(16) -0.00104(12) -0.00501(12) -0.00385(12) Gd2 0.01621(18) 0.01730(17) 0.01317(17) -0.00171(13) -0.00514(13) -0.00313(13) O1 0.020(3) 0.027(3) 0.028(3) -0.014(2) -0.006(2) -0.001(2) O1W 0.060(5) 0.083(5) 0.052(4) -0.009(4) -0.016(4) -0.002(4) O2 0.024(3) 0.032(3) 0.021(3) -0.004(2) -0.009(2) -0.012(2) O2W 0.080(6) 0.107(7) 0.062(5) 0.010(5) -0.010(4) 0.003(5) O3 0.041(3) 0.036(3) 0.023(3) -0.011(2) -0.012(2) 0.008(3) O3W 0.162(9) 0.066(5) 0.065(5) -0.030(4) -0.026(5) -0.032(5) O4 0.041(3) 0.021(3) 0.019(3) -0.009(2) -0.002(2) -0.001(2) O4W 0.158(9) 0.062(5) 0.104(7) -0.019(5) 0.045(7) -0.034(6) O5 0.048(4) 0.034(3) 0.035(3) -0.009(3) -0.014(3) 0.004(3) O6 0.072(5) 0.032(3) 0.035(3) -0.011(3) -0.012(3) 0.008(3) O7 0.026(3) 0.022(3) 0.019(2) 0.002(2) -0.005(2) -0.011(2) O8 0.030(3) 0.036(3) 0.038(3) 0.017(2) -0.022(2) -0.016(2) O9 0.038(3) 0.026(3) 0.029(3) 0.009(2) -0.019(2) -0.019(2) O10 0.032(3) 0.025(3) 0.014(2) -0.006(2) 0.001(2) -0.012(2) O11 0.029(3) 0.032(3) 0.027(3) -0.008(2) -0.016(2) -0.006(2) O12 0.039(3) 0.035(3) 0.047(3) -0.019(3) -0.029(3) 0.007(3) O13 0.015(2) 0.024(2) 0.014(2) 0.0006(19) -0.0076(18) -0.0052(19) O14 0.020(3) 0.030(3) 0.020(2) 0.009(2) -0.014(2) -0.016(2) O15 0.015(2) 0.020(2) 0.011(2) 0.0015(18) -0.0021(17) -0.0025(18) O16 0.027(3) 0.046(3) 0.038(3) -0.024(3) -0.004(2) 0.002(3) O17 0.043(4) 0.027(3) 0.036(3) -0.002(2) -0.009(3) -0.012(3) O18 0.034(3) 0.032(3) 0.030(3) 0.006(2) -0.007(2) -0.012(3) C1 0.019(4) 0.018(3) 0.022(4) -0.005(3) 0.001(3) -0.007(3) C2 0.024(4) 0.015(3) 0.025(4) -0.004(3) -0.005(3) 0.002(3) C3 0.023(4) 0.036(4) 0.014(3) -0.006(3) -0.005(3) -0.005(3) C4 0.014(3) 0.023(4) 0.029(4) -0.003(3) -0.003(3) -0.006(3) C5 0.025(4) 0.017(3) 0.023(4) -0.003(3) -0.006(3) -0.005(3) C6 0.019(4) 0.033(4) 0.021(4) -0.008(3) -0.004(3) -0.007(3) C7 0.020(4) 0.026(4) 0.024(4) -0.008(3) -0.001(3) -0.015(3) C8 0.015(4) 0.029(4) 0.027(4) -0.007(3) 0.001(3) -0.011(3) C9 0.026(4) 0.016(3) 0.019(3) 0.007(3) -0.004(3) -0.007(3) C10 0.020(4) 0.018(3) 0.015(3) 0.000(3) -0.004(3) -0.007(3) C11 0.020(4) 0.026(4) 0.021(4) 0.002(3) -0.013(3) -0.009(3) C12 0.016(3) 0.024(4) 0.016(3) 0.001(3) -0.007(3) -0.008(3) C13 0.020(4) 0.025(4) 0.022(4) -0.002(3) -0.011(3) -0.003(3) C14 0.030(4) 0.017(3) 0.026(4) -0.007(3) -0.010(3) -0.001(3) C15 0.028(4) 0.028(4) 0.013(3) -0.005(3) -0.005(3) -0.006(3) C16 0.025(4) 0.025(4) 0.012(3) -0.004(3) 0.002(3) -0.012(3) C17 0.015(3) 0.014(3) 0.021(3) 0.001(3) -0.009(3) -0.005(3) C18 0.017(3) 0.017(3) 0.013(3) -0.002(2) -0.002(3) -0.007(3) C19 0.010(3) 0.021(3) 0.014(3) 0.001(3) -0.002(2) -0.003(3) C20 0.012(3) 0.021(3) 0.018(3) -0.003(3) -0.010(3) 0.001(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 O14 2.367(4) 1_655 ? Gd1 O15 2.378(4) . ? Gd1 O16 2.380(5) . ? Gd1 O7 2.387(4) . ? Gd1 O1 2.391(5) . ? Gd1 O17 2.451(5) . ? Gd1 O11 2.460(5) . ? Gd1 O13 2.656(4) 1_655 ? Gd1 Gd2 3.9833(6) . ? Gd2 O8 2.321(5) 1_455 ? Gd2 O10 2.323(4) . ? Gd2 O13 2.357(4) . ? Gd2 O2 2.366(5) . ? Gd2 O4 2.409(4) 2_665 ? Gd2 O15 2.409(4) . ? Gd2 O18 2.458(5) . ? Gd2 O3 2.479(5) 2_665 ? O1 C7 1.265(8) . ? O2 C7 1.267(8) . ? O2W H2WA 0.8200 . ? O2W H2WB 0.8200 . ? O3 C8 1.262(8) . ? O3 Gd2 2.479(5) 2_665 ? O3W H3WA 0.8200 . ? O3W H3WB 0.8200 . ? O4 C8 1.281(8) . ? O4 Gd2 2.409(4) 2_665 ? O4W H4WA 0.8200 . ? O4W H4WB 0.8200 . ? O5 C2 1.360(8) . ? O5 H5A 0.8200 . ? O6 C5 1.381(8) . ? O6 H6B 0.8200 . ? O7 C12 1.259(8) . ? O8 C12 1.245(8) . ? O8 Gd2 2.321(5) 1_655 ? O9 C9 1.370(8) . ? O9 H9 0.8200 . ? O10 C16 1.248(8) . ? O11 C16 1.263(8) . ? O12 C13 1.365(8) . ? O12 H12 0.8200 . ? O13 C20 1.292(7) . ? O13 Gd1 2.656(4) 1_455 ? O14 C20 1.263(8) . ? O14 Gd1 2.367(4) 1_455 ? O15 C18 1.355(7) . ? O16 H16A 0.8200 . ? O16 H16B 0.8200 . ? O17 H17A 0.8200 . ? O17 H17B 0.8200 . ? O18 H18A 0.8200 . ? O18 H18B 0.8200 . ? C1 C2 1.397(9) . ? C1 C6 1.401(9) . ? C1 C7 1.488(9) . ? C2 C3 1.386(9) . ? C3 C4 1.378(9) . ? C3 H3A 0.9300 . ? C4 C5 1.401(9) . ? C4 C8 1.492(9) . ? C5 C6 1.380(9) . ? C6 H6A 0.9300 . ? C9 C10 1.380(9) . ? C9 C11 1.391(8) 2_764 ? C10 C11 1.390(9) . ? C10 C12 1.518(8) . ? C11 C9 1.391(8) 2_764 ? C11 H11 0.9300 . ? C13 C14 1.379(9) . ? C13 C15 1.406(9) 2_654 ? C14 C15 1.397(9) . ? C14 H14A 0.9300 . ? C15 C13 1.406(9) 2_654 ? C15 C16 1.500(9) . ? C17 C19 1.390(8) 2_655 ? C17 C18 1.403(8) . ? C17 H17 0.9300 . ? C18 C19 1.410(8) . ? C19 C17 1.390(8) 2_655 ? C19 C20 1.471(8) . ? 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 O14 Gd1 O15 103.45(15) 1_655 . ? O14 Gd1 O16 82.13(17) 1_655 . ? O15 Gd1 O16 150.34(18) . . ? O14 Gd1 O7 133.77(16) 1_655 . ? O15 Gd1 O7 109.63(15) . . ? O16 Gd1 O7 84.55(17) . . ? O14 Gd1 O1 73.39(16) 1_655 . ? O15 Gd1 O1 75.45(16) . . ? O16 Gd1 O1 133.14(18) . . ? O7 Gd1 O1 84.56(16) . . ? O14 Gd1 O17 69.47(17) 1_655 . ? O15 Gd1 O17 76.66(16) . . ? O16 Gd1 O17 78.29(18) . . ? O7 Gd1 O17 148.81(17) . . ? O1 Gd1 O17 125.97(17) . . ? O14 Gd1 O11 138.90(16) 1_655 . ? O15 Gd1 O11 83.40(16) . . ? O16 Gd1 O11 74.27(17) . . ? O7 Gd1 O11 77.34(16) . . ? O1 Gd1 O11 145.61(16) . . ? O17 Gd1 O11 73.05(17) . . ? O14 Gd1 O13 51.29(14) 1_655 1_655 ? O15 Gd1 O13 138.32(14) . 1_655 ? O16 Gd1 O13 67.39(16) . 1_655 ? O7 Gd1 O13 82.75(15) . 1_655 ? O1 Gd1 O13 66.08(14) . 1_655 ? O17 Gd1 O13 113.45(16) . 1_655 ? O11 Gd1 O13 138.11(15) . 1_655 ? O14 Gd1 C20 25.04(16) 1_655 1_655 ? O15 Gd1 C20 121.53(16) . 1_655 ? O16 Gd1 C20 74.62(18) . 1_655 ? O7 Gd1 C20 108.79(17) . 1_655 ? O1 Gd1 C20 66.26(17) . 1_655 ? O17 Gd1 C20 91.60(18) . 1_655 ? O11 Gd1 C20 147.49(17) . 1_655 ? O13 Gd1 C20 26.31(15) 1_655 1_655 ? O14 Gd1 Gd2 130.51(12) 1_655 . ? O15 Gd1 Gd2 33.94(10) . . ? O16 Gd1 Gd2 146.89(13) . . ? O7 Gd1 Gd2 75.69(11) . . ? O1 Gd1 Gd2 71.67(11) . . ? O17 Gd1 Gd2 105.65(13) . . ? O11 Gd1 Gd2 75.61(11) . . ? O13 Gd1 Gd2 133.93(9) 1_655 . ? C20 Gd1 Gd2 136.82(12) 1_655 . ? O8 Gd2 O10 87.47(19) 1_455 . ? O8 Gd2 O13 73.13(16) 1_455 . ? O10 Gd2 O13 86.64(15) . . ? O8 Gd2 O2 140.64(17) 1_455 . ? O10 Gd2 O2 95.75(17) . . ? O13 Gd2 O2 146.14(15) . . ? O8 Gd2 O4 115.63(19) 1_455 2_665 ? O10 Gd2 O4 151.61(16) . 2_665 ? O13 Gd2 O4 84.89(16) . 2_665 ? O2 Gd2 O4 77.07(17) . 2_665 ? O8 Gd2 O15 140.85(17) 1_455 . ? O10 Gd2 O15 74.61(15) . . ? O13 Gd2 O15 71.35(15) . . ? O2 Gd2 O15 76.75(16) . . ? O4 Gd2 O15 77.01(15) 2_665 . ? O8 Gd2 O18 73.23(17) 1_455 . ? O10 Gd2 O18 75.94(17) . . ? O13 Gd2 O18 142.56(16) . . ? O2 Gd2 O18 69.64(17) . . ? O4 Gd2 O18 124.78(17) 2_665 . ? O15 Gd2 O18 132.14(15) . . ? O8 Gd2 O3 76.42(19) 1_455 2_665 ? O10 Gd2 O3 154.33(16) . 2_665 ? O13 Gd2 O3 107.08(17) . 2_665 ? O2 Gd2 O3 84.84(18) . 2_665 ? O4 Gd2 O3 53.45(16) 2_665 2_665 ? O15 Gd2 O3 129.93(15) . 2_665 ? O18 Gd2 O3 80.29(18) . 2_665 ? O8 Gd2 C8 97.8(2) 1_455 2_665 ? O10 Gd2 C8 173.25(18) . 2_665 ? O13 Gd2 C8 98.86(17) . 2_665 ? O2 Gd2 C8 77.50(18) . 2_665 ? O4 Gd2 C8 27.01(18) 2_665 2_665 ? O15 Gd2 C8 103.34(18) . 2_665 ? O18 Gd2 C8 101.53(19) . 2_665 ? O3 Gd2 C8 26.65(17) 2_665 2_665 ? O8 Gd2 Gd1 141.93(15) 1_455 . ? O10 Gd2 Gd1 54.76(12) . . ? O13 Gd2 Gd1 97.52(10) . . ? O2 Gd2 Gd1 58.51(12) . . ? O4 Gd2 Gd1 99.65(12) 2_665 . ? O15 Gd2 Gd1 33.44(10) . . ? O18 Gd2 Gd1 98.83(12) . . ? O3 Gd2 Gd1 140.18(13) 2_665 . ? C8 Gd2 Gd1 120.19(15) 2_665 . ? C7 O1 Gd1 124.1(4) . . ? C7 O2 Gd2 133.0(4) . . ? H2WA O2W H2WB 86.3 . . ? C8 O3 Gd2 91.6(4) . 2_665 ? H3WA O3W H3WB 116.9 . . ? C8 O4 Gd2 94.3(4) . 2_665 ? H4WA O4W H4WB 125.7 . . ? C2 O5 H5A 109.5 . . ? C5 O6 H6B 109.5 . . ? C12 O7 Gd1 132.5(4) . . ? C12 O8 Gd2 161.6(5) . 1_655 ? C9 O9 H9 109.5 . . ? C16 O10 Gd2 149.9(4) . . ? C16 O11 Gd1 116.7(4) . . ? C13 O12 H12 109.5 . . ? C20 O13 Gd2 128.1(4) . . ? C20 O13 Gd1 88.0(4) . 1_455 ? Gd2 O13 Gd1 136.85(18) . 1_455 ? C20 O14 Gd1 102.5(4) . 1_455 ? C18 O15 Gd1 128.2(4) . . ? C18 O15 Gd2 115.9(3) . . ? Gd1 O15 Gd2 112.62(16) . . ? Gd1 O16 H16A 120.1 . . ? Gd1 O16 H16B 135.5 . . ? H16A O16 H16B 94.1 . . ? Gd1 O17 H17A 129.2 . . ? Gd1 O17 H17B 131.7 . . ? H17A O17 H17B 95.8 . . ? Gd2 O18 H18A 121.0 . . ? Gd2 O18 H18B 111.4 . . ? H18A O18 H18B 116.1 . . ? C2 C1 C6 119.1(6) . . ? C2 C1 C7 121.1(6) . . ? C6 C1 C7 119.8(6) . . ? O5 C2 C3 115.8(6) . . ? O5 C2 C1 123.9(6) . . ? C3 C2 C1 120.3(6) . . ? C4 C3 C2 120.2(7) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 120.0(6) . . ? C3 C4 C8 119.3(6) . . ? C5 C4 C8 120.7(6) . . ? C6 C5 O6 116.7(6) . . ? C6 C5 C4 119.9(6) . . ? O6 C5 C4 123.2(6) . . ? C5 C6 C1 120.2(7) . . ? C5 C6 H6A 119.9 . . ? C1 C6 H6A 119.9 . . ? O1 C7 O2 122.1(6) . . ? O1 C7 C1 118.5(6) . . ? O2 C7 C1 119.4(6) . . ? O3 C8 O4 119.7(6) . . ? O3 C8 C4 121.7(6) . . ? O4 C8 C4 118.4(6) . . ? O3 C8 Gd2 61.8(4) . 2_665 ? O4 C8 Gd2 58.7(3) . 2_665 ? C4 C8 Gd2 167.9(5) . 2_665 ? O9 C9 C10 122.3(6) . . ? O9 C9 C11 117.2(6) . 2_764 ? C10 C9 C11 120.5(6) . 2_764 ? C9 C10 C11 120.0(6) . . ? C9 C10 C12 121.5(6) . . ? C11 C10 C12 118.4(6) . . ? C10 C11 C9 119.5(6) . 2_764 ? C10 C11 H11 120.3 . . ? C9 C11 H11 120.3 2_764 . ? O8 C12 O7 124.3(6) . . ? O8 C12 C10 117.0(6) . . ? O7 C12 C10 118.7(6) . . ? O12 C13 C14 117.7(6) . . ? O12 C13 C15 122.5(6) . 2_654 ? C14 C13 C15 119.8(6) . 2_654 ? C13 C14 C15 121.6(6) . . ? C13 C14 H14A 119.2 . . ? C15 C14 H14A 119.2 . . ? C14 C15 C13 118.7(6) . 2_654 ? C14 C15 C16 118.8(6) . . ? C13 C15 C16 122.5(6) 2_654 . ? O10 C16 O11 122.8(6) . . ? O10 C16 C15 118.7(6) . . ? O11 C16 C15 118.5(6) . . ? C19 C17 C18 123.0(6) 2_655 . ? C19 C17 H17 118.5 2_655 . ? C18 C17 H17 118.5 . . ? O15 C18 C17 121.0(6) . . ? O15 C18 C19 123.1(6) . . ? C17 C18 C19 115.8(6) . . ? C17 C19 C18 121.2(6) 2_655 . ? C17 C19 C20 115.8(6) 2_655 . ? C18 C19 C20 123.0(6) . . ? O14 C20 O13 117.9(6) . . ? O14 C20 C19 119.9(6) . . ? O13 C20 C19 122.1(6) . . ? O14 C20 Gd1 52.5(3) . 1_455 ? O13 C20 Gd1 65.6(3) . 1_455 ? C19 C20 Gd1 170.5(4) . 1_455 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O1 0.82 1.92 2.631(7) 144.0 . O6 H6B O4 0.82 1.86 2.578(7) 145.2 . O9 H9 O7 0.82 1.90 2.590(7) 140.9 . O12 H12 O11 0.82 1.94 2.634(7) 142.3 2_654 O16 H16A O1W 0.82 2.09 2.879(8) 161.7 1_645 O16 H16B O3W 0.82 1.84 2.654(8) 175.8 . O17 H17A O1W 0.82 2.32 3.072(9) 152.9 1_545 O17 H17B O5 0.82 2.18 2.930(7) 151.9 2_755 O18 H18A O4W 0.82 1.99 2.801(10) 172.7 . O18 H18B O9 0.82 2.15 2.906(7) 153.7 . O2W H2WA O4W 0.82 2.47 3.065(13) 130.1 2_765 O2W H2WB O3 0.82 2.12 2.845(9) 147.2 . O3W H3WA O9 0.82 2.08 2.822(9) 150.1 2_754 O3W H3WB O2W 0.82 2.02 2.672(11) 136.1 2_755 O4W H4WA O12 0.82 2.27 2.898(10) 133.6 2_664 O4W H4WB O1W 0.82 2.50 3.090(11) 130.1 . _diffrn_measured_fraction_theta_max 0.866 _diffrn_reflns_theta_full 29.04 _diffrn_measured_fraction_theta_full 0.866 _refine_diff_density_max 1.578 _refine_diff_density_min -1.260 _refine_diff_density_rms 0.213 #===END OF 5 ## Crystallographic Data for compound 6 data_Dy _database_code_depnum_ccdc_archive 'CCDC 879612' #TrackingRef '- revised Ln.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H23 Dy2 O22' _chemical_formula_weight 940.38 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3494(4) _cell_length_b 11.4750(6) _cell_length_c 16.1852(8) _cell_angle_alpha 78.7990(10) _cell_angle_beta 82.4830(10) _cell_angle_gamma 79.9550(10) _cell_volume 1311.79(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6535 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 28.28 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 902 _exptl_absorpt_coefficient_mu 5.757 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2450 _exptl_absorpt_correction_T_max 0.5450 _exptl_absorpt_process_details '(SADABS; Bruker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12411 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6347 _reflns_number_gt 5404 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+2.6918P] 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 6347 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0648 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.94154(2) 0.065975(16) -0.226370(11) 0.01322(5) Uani 1 1 d . . . Dy2 Dy 0.44429(2) 0.264555(16) -0.236029(11) 0.01513(6) Uani 1 1 d . . . O1 O 0.9258(4) 0.2197(3) -0.1455(2) 0.0239(7) Uani 1 1 d . . . O1W O 0.5140(7) 0.8269(5) -0.2225(3) 0.0673(14) Uani 1 1 d . . . O2 O 0.6979(4) 0.3437(3) -0.20938(19) 0.0232(7) Uani 1 1 d . . . O2W O 0.9968(8) 0.3707(6) 0.2590(4) 0.095(2) Uani 1 1 d . . . H2WA H 1.0558 0.4148 0.2754 0.142 Uiso 1 1 d R . . H2WB H 0.9616 0.4296 0.2241 0.142 Uiso 1 1 d R . . O3 O 0.7329(5) 0.5575(3) 0.1825(2) 0.0337(8) Uani 1 1 d . . . O3W O 1.2166(9) -0.2395(5) -0.3714(3) 0.0796(17) Uani 1 1 d . . . H3WA H 1.2146 -0.2342 -0.4225 0.119 Uiso 1 1 d R . . H3WB H 1.2023 -0.3046 -0.3419 0.119 Uiso 1 1 d R . . O4 O 0.6277(5) 0.7144(3) 0.0914(2) 0.0296(7) Uani 1 1 d . . . O4W O 0.6336(10) 0.6365(5) -0.3395(4) 0.106(2) Uani 1 1 d . . . H4WA H 0.6904 0.6631 -0.3843 0.159 Uiso 1 1 d R . . H4WB H 0.5390 0.6716 -0.3168 0.159 Uiso 1 1 d R . . O5 O 0.9819(6) 0.2418(3) 0.0076(2) 0.0426(9) Uani 1 1 d . . . H5A H 0.9947 0.2071 -0.0330 0.064 Uiso 1 1 calc R . . O6 O 0.5812(6) 0.6962(3) -0.0608(2) 0.0492(11) Uani 1 1 d . . . H6B H 0.5710 0.7306 -0.0201 0.074 Uiso 1 1 calc R . . O7 O 0.9787(4) 0.2213(3) -0.34341(19) 0.0222(6) Uani 1 1 d . . . O8 O 1.1911(5) 0.3175(3) -0.3126(2) 0.0329(8) Uani 1 1 d . . . O9 O 0.7977(5) 0.3132(3) -0.4731(2) 0.0292(8) Uani 1 1 d . . . H9 H 0.8463 0.2556 -0.4406 0.044 Uiso 1 1 calc R . . O10 O 0.5890(5) 0.1664(3) -0.34210(19) 0.0251(7) Uani 1 1 d . . . O11 O 0.8029(4) 0.0042(3) -0.3360(2) 0.0269(7) Uani 1 1 d . . . O12 O 0.2031(5) 0.1553(3) -0.5673(2) 0.0408(10) Uani 1 1 d . . . H12 H 0.1512 0.1234 -0.5968 0.061 Uiso 1 1 calc R . . O13 O 0.2712(4) 0.1065(3) -0.19893(17) 0.0180(6) Uani 1 1 d . . . O14 O 0.1132(4) -0.0188(3) -0.11176(19) 0.0243(7) Uani 1 1 d . . . O15 O 0.6335(4) 0.0939(3) -0.16515(16) 0.0152(5) Uani 1 1 d . . . O16 O 1.1873(4) -0.0446(3) -0.3005(2) 0.0345(8) Uani 1 1 d . . . H16A H 1.2859 -0.0682 -0.2796 0.052 Uiso 1 1 d R . . H16B H 1.1981 -0.1004 -0.3266 0.052 Uiso 1 1 d R . . O17 O 0.8841(5) -0.1382(3) -0.1732(2) 0.0317(8) Uani 1 1 d . . . H17A H 0.7910 -0.1685 -0.1731 0.048 Uiso 1 1 d R . . H17B H 0.9300 -0.1902 -0.1361 0.048 Uiso 1 1 d R . . O18 O 0.5214(5) 0.4222(3) -0.3533(2) 0.0309(7) Uani 1 1 d . . . H18A H 0.5512 0.4837 -0.3440 0.046 Uiso 1 1 d R . . H18B H 0.5779 0.3948 -0.3942 0.046 Uiso 1 1 d R . . C1 C 0.7940(6) 0.3926(4) -0.0873(3) 0.0179(8) Uani 1 1 d . . . C2 C 0.8703(6) 0.3489(4) -0.0100(3) 0.0244(9) Uani 1 1 d . . . C3 C 0.8347(6) 0.4174(4) 0.0537(3) 0.0267(10) Uani 1 1 d . . . H3A H 0.8746 0.3853 0.1068 0.032 Uiso 1 1 calc R . . C4 C 0.7396(6) 0.5338(4) 0.0383(3) 0.0214(9) Uani 1 1 d . . . C5 C 0.6769(6) 0.5815(4) -0.0405(3) 0.0238(9) Uani 1 1 d . . . C6 C 0.6989(6) 0.5106(4) -0.1019(3) 0.0223(9) Uani 1 1 d . . . H6A H 0.6502 0.5412 -0.1533 0.027 Uiso 1 1 calc R . . C7 C 0.8079(6) 0.3142(4) -0.1520(3) 0.0187(8) Uani 1 1 d . . . C8 C 0.7014(6) 0.6048(4) 0.1079(3) 0.0225(9) Uani 1 1 d . . . C9 C 0.9013(6) 0.4041(4) -0.4858(3) 0.0198(9) Uani 1 1 d . . . C10 C 1.0329(6) 0.4062(4) -0.4310(3) 0.0186(8) Uani 1 1 d . . . C11 C 1.1306(6) 0.5030(4) -0.4464(3) 0.0207(9) Uani 1 1 d . . . H11 H 1.2187 0.5054 -0.4107 0.025 Uiso 1 1 calc R . . C12 C 1.0715(6) 0.3084(4) -0.3570(3) 0.0189(8) Uani 1 1 d . . . C13 C 0.3502(6) 0.0759(4) -0.5360(3) 0.0223(9) Uani 1 1 d . . . C14 C 0.4315(6) 0.1073(4) -0.4720(3) 0.0243(9) Uani 1 1 d . . . H14A H 0.3851 0.1793 -0.4530 0.029 Uiso 1 1 calc R . . C15 C 0.5821(6) 0.0319(4) -0.4361(3) 0.0190(8) Uani 1 1 d . . . C16 C 0.6626(6) 0.0694(4) -0.3663(3) 0.0195(8) Uani 1 1 d . . . C17 C 0.6769(5) 0.0279(4) -0.0184(2) 0.0165(8) Uani 1 1 d . . . H17 H 0.7973 0.0459 -0.0297 0.020 Uiso 1 1 calc R . . C18 C 0.5671(5) 0.0472(3) -0.0854(2) 0.0141(7) Uani 1 1 d . . . C19 C 0.3868(5) 0.0171(4) -0.0647(2) 0.0137(7) Uani 1 1 d . . . C20 C 0.2521(5) 0.0349(4) -0.1285(2) 0.0153(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01395(9) 0.01479(10) 0.01152(9) -0.00075(7) -0.00461(7) -0.00305(7) Dy2 0.01636(10) 0.01647(10) 0.01304(10) -0.00108(7) -0.00508(7) -0.00283(7) O1 0.0226(15) 0.0234(16) 0.0279(17) -0.0116(13) -0.0046(13) -0.0003(12) O1W 0.059(3) 0.072(3) 0.067(3) -0.009(3) -0.020(3) 0.006(2) O2 0.0255(16) 0.0243(16) 0.0236(16) -0.0060(13) -0.0068(13) -0.0085(13) O2W 0.083(4) 0.111(5) 0.068(4) 0.025(3) -0.012(3) 0.005(4) O3 0.039(2) 0.038(2) 0.0238(17) -0.0123(15) -0.0117(15) 0.0101(16) O3W 0.138(5) 0.056(3) 0.056(3) -0.021(3) -0.026(3) -0.022(3) O4 0.045(2) 0.0201(16) 0.0235(17) -0.0077(13) 0.0004(14) -0.0017(14) O4W 0.171(7) 0.048(3) 0.096(5) -0.006(3) 0.028(5) -0.043(4) O5 0.057(2) 0.033(2) 0.037(2) -0.0099(17) -0.0134(19) 0.0065(18) O6 0.074(3) 0.034(2) 0.036(2) -0.0102(18) -0.013(2) 0.010(2) O7 0.0262(16) 0.0203(15) 0.0200(15) 0.0040(12) -0.0073(12) -0.0081(12) O8 0.0343(18) 0.0321(19) 0.0336(19) 0.0141(15) -0.0221(15) -0.0167(15) O9 0.0370(18) 0.0276(17) 0.0254(17) 0.0087(14) -0.0150(14) -0.0177(14) O10 0.0371(18) 0.0252(17) 0.0163(15) -0.0076(13) -0.0023(13) -0.0096(14) O11 0.0304(17) 0.0312(18) 0.0235(16) -0.0062(14) -0.0116(14) -0.0088(14) O12 0.046(2) 0.036(2) 0.046(2) -0.0165(17) -0.0304(18) 0.0102(17) O13 0.0193(14) 0.0206(15) 0.0140(14) 0.0025(11) -0.0075(11) -0.0050(11) O14 0.0194(15) 0.0308(17) 0.0233(16) 0.0069(13) -0.0120(12) -0.0114(13) O15 0.0152(13) 0.0215(15) 0.0075(12) -0.0001(11) -0.0007(10) -0.0022(11) O16 0.0247(17) 0.042(2) 0.041(2) -0.0227(17) -0.0058(15) 0.0017(15) O17 0.0343(19) 0.0255(18) 0.037(2) -0.0006(15) -0.0082(15) -0.0117(15) O18 0.0319(18) 0.0301(19) 0.0288(18) 0.0032(14) -0.0034(15) -0.0087(15) C1 0.019(2) 0.019(2) 0.0170(19) -0.0032(16) -0.0010(15) -0.0064(16) C2 0.024(2) 0.022(2) 0.026(2) -0.0059(18) -0.0038(18) 0.0043(17) C3 0.027(2) 0.031(3) 0.022(2) -0.0074(19) -0.0079(18) 0.0044(19) C4 0.022(2) 0.023(2) 0.021(2) -0.0081(17) -0.0006(17) -0.0038(17) C5 0.025(2) 0.017(2) 0.028(2) -0.0023(18) -0.0031(18) -0.0021(17) C6 0.023(2) 0.023(2) 0.022(2) -0.0039(17) -0.0068(17) -0.0036(17) C7 0.0179(19) 0.020(2) 0.021(2) -0.0054(17) 0.0005(16) -0.0096(16) C8 0.018(2) 0.026(2) 0.025(2) -0.0114(18) 0.0002(17) -0.0037(17) C9 0.021(2) 0.020(2) 0.020(2) 0.0022(17) -0.0064(16) -0.0079(16) C10 0.021(2) 0.021(2) 0.0138(19) 0.0021(16) -0.0053(16) -0.0057(16) C11 0.023(2) 0.022(2) 0.019(2) 0.0023(17) -0.0105(17) -0.0076(17) C12 0.0174(19) 0.020(2) 0.017(2) 0.0028(16) -0.0040(16) -0.0026(16) C13 0.023(2) 0.022(2) 0.023(2) -0.0074(18) -0.0076(17) 0.0014(17) C14 0.027(2) 0.021(2) 0.028(2) -0.0118(18) -0.0109(19) 0.0011(17) C15 0.020(2) 0.023(2) 0.0155(19) -0.0036(16) -0.0041(16) -0.0080(16) C16 0.022(2) 0.028(2) 0.0116(18) -0.0024(17) -0.0027(15) -0.0121(17) C17 0.0150(18) 0.021(2) 0.0132(18) 0.0030(15) -0.0046(15) -0.0062(15) C18 0.0146(18) 0.0147(19) 0.0123(18) -0.0002(15) -0.0030(14) -0.0015(14) C19 0.0121(17) 0.020(2) 0.0098(17) -0.0005(15) -0.0041(14) -0.0033(14) C20 0.0151(18) 0.0158(19) 0.0160(19) -0.0027(15) -0.0057(15) -0.0020(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 Dy1 O14 2.337(3) 1_655 ? Dy1 O15 2.344(3) . ? Dy1 O16 2.353(3) . ? Dy1 O7 2.359(3) . ? Dy1 O1 2.371(3) . ? Dy1 O17 2.424(3) . ? Dy1 O11 2.430(3) . ? Dy1 O13 2.652(3) 1_655 ? Dy1 Dy2 3.9596(3) . ? Dy2 O10 2.281(3) . ? Dy2 O8 2.299(3) 1_455 ? Dy2 O2 2.332(3) . ? Dy2 O13 2.335(3) . ? Dy2 O4 2.382(3) 2_665 ? Dy2 O15 2.383(3) . ? Dy2 O18 2.437(3) . ? Dy2 O3 2.466(3) 2_665 ? O1 C7 1.261(5) . ? O2 C7 1.269(5) . ? O2W H2WA 0.8200 . ? O2W H2WB 0.8200 . ? O3 C8 1.256(5) . ? O3 Dy2 2.466(3) 2_665 ? O3W H3WA 0.8200 . ? O3W H3WB 0.8200 . ? O4 C8 1.272(5) . ? O4 Dy2 2.382(3) 2_665 ? O4W H4WA 0.8200 . ? O4W H4WB 0.8200 . ? O5 C2 1.355(5) . ? O5 H5A 0.8200 . ? O6 C5 1.379(5) . ? O6 H6B 0.8200 . ? O7 C12 1.274(5) . ? O8 C12 1.235(5) . ? O8 Dy2 2.299(3) 1_655 ? O9 C9 1.365(5) . ? O9 H9 0.8200 . ? O10 C16 1.261(5) . ? O11 C16 1.258(5) . ? O12 C13 1.370(5) . ? O12 H12 0.8200 . ? O13 C20 1.276(5) . ? O13 Dy1 2.652(3) 1_455 ? O14 C20 1.256(5) . ? O14 Dy1 2.337(3) 1_455 ? O15 C18 1.360(4) . ? O16 H16A 0.8200 . ? O16 H16B 0.8200 . ? O17 H17A 0.8200 . ? O17 H17B 0.8200 . ? O18 H18A 0.8200 . ? O18 H18B 0.8200 . ? C1 C6 1.402(6) . ? C1 C2 1.405(6) . ? C1 C7 1.491(6) . ? C2 C3 1.385(6) . ? C3 C4 1.388(6) . ? C3 H3A 0.9300 . ? C4 C5 1.391(6) . ? C4 C8 1.486(6) . ? C5 C6 1.378(6) . ? C6 H6A 0.9300 . ? C9 C11 1.386(6) 2_764 ? C9 C10 1.401(5) . ? C10 C11 1.392(6) . ? C10 C12 1.494(5) . ? C11 C9 1.386(6) 2_764 ? C11 H11 0.9300 . ? C13 C15 1.388(6) 2_654 ? C13 C14 1.394(6) . ? C14 C15 1.396(6) . ? C14 H14A 0.9300 . ? C15 C13 1.388(6) 2_654 ? C15 C16 1.505(5) . ? C17 C19 1.395(5) 2_655 ? C17 C18 1.396(5) . ? C17 H17 0.9300 . ? C18 C19 1.409(5) . ? C19 C17 1.395(5) 2_655 ? C19 C20 1.485(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O14 Dy1 O15 104.08(10) 1_655 . ? O14 Dy1 O16 82.58(12) 1_655 . ? O15 Dy1 O16 150.76(11) . . ? O14 Dy1 O7 133.63(10) 1_655 . ? O15 Dy1 O7 108.91(10) . . ? O16 Dy1 O7 84.12(12) . . ? O14 Dy1 O1 73.77(11) 1_655 . ? O15 Dy1 O1 75.00(10) . . ? O16 Dy1 O1 133.51(11) . . ? O7 Dy1 O1 84.23(11) . . ? O14 Dy1 O17 70.04(11) 1_655 . ? O15 Dy1 O17 77.27(11) . . ? O16 Dy1 O17 78.52(12) . . ? O7 Dy1 O17 148.42(11) . . ? O1 Dy1 O17 126.60(11) . . ? O14 Dy1 O11 139.69(11) 1_655 . ? O15 Dy1 O11 83.02(10) . . ? O16 Dy1 O11 74.44(11) . . ? O7 Dy1 O11 76.87(10) . . ? O1 Dy1 O11 144.49(11) . . ? O17 Dy1 O11 73.17(11) . . ? O14 Dy1 O13 51.45(9) 1_655 1_655 ? O15 Dy1 O13 138.33(9) . 1_655 ? O16 Dy1 O13 67.68(10) . 1_655 ? O7 Dy1 O13 82.44(9) . 1_655 ? O1 Dy1 O13 66.23(10) . 1_655 ? O17 Dy1 O13 114.13(10) . 1_655 ? O11 Dy1 O13 138.30(10) . 1_655 ? O14 Dy1 C20 25.23(11) 1_655 1_655 ? O15 Dy1 C20 122.12(10) . 1_655 ? O16 Dy1 C20 74.89(11) . 1_655 ? O7 Dy1 C20 108.45(11) . 1_655 ? O1 Dy1 C20 66.64(10) . 1_655 ? O17 Dy1 C20 92.30(11) . 1_655 ? O11 Dy1 C20 148.10(11) . 1_655 ? O13 Dy1 C20 26.27(10) 1_655 1_655 ? O14 Dy1 Dy2 130.89(8) 1_655 . ? O15 Dy1 Dy2 33.41(6) . . ? O16 Dy1 Dy2 146.09(8) . . ? O7 Dy1 Dy2 75.50(7) . . ? O1 Dy1 Dy2 71.56(7) . . ? O17 Dy1 Dy2 105.45(8) . . ? O11 Dy1 Dy2 74.70(8) . . ? O13 Dy1 Dy2 133.85(6) 1_655 . ? C20 Dy1 Dy2 137.17(8) 1_655 . ? O10 Dy2 O8 87.17(13) . 1_455 ? O10 Dy2 O2 97.94(11) . . ? O8 Dy2 O2 140.28(11) 1_455 . ? O10 Dy2 O13 85.52(11) . . ? O8 Dy2 O13 73.29(10) 1_455 . ? O2 Dy2 O13 146.17(10) . . ? O10 Dy2 O4 153.32(11) . 2_665 ? O8 Dy2 O4 113.39(13) 1_455 2_665 ? O2 Dy2 O4 77.39(11) . 2_665 ? O13 Dy2 O4 84.57(11) . 2_665 ? O10 Dy2 O15 75.87(10) . . ? O8 Dy2 O15 141.94(11) 1_455 . ? O2 Dy2 O15 76.60(10) . . ? O13 Dy2 O15 71.64(9) . . ? O4 Dy2 O15 77.51(10) 2_665 . ? O10 Dy2 O18 74.68(12) . . ? O8 Dy2 O18 73.61(11) 1_455 . ? O2 Dy2 O18 69.98(11) . . ? O13 Dy2 O18 141.99(10) . . ? O4 Dy2 O18 126.00(12) 2_665 . ? O15 Dy2 O18 131.16(10) . . ? O10 Dy2 O3 152.65(11) . 2_665 ? O8 Dy2 O3 75.72(12) 1_455 2_665 ? O2 Dy2 O3 82.80(11) . 2_665 ? O13 Dy2 O3 109.07(12) . 2_665 ? O4 Dy2 O3 53.67(11) 2_665 2_665 ? O15 Dy2 O3 130.12(10) . 2_665 ? O18 Dy2 O3 80.03(12) . 2_665 ? O10 Dy2 C8 174.36(12) . 2_665 ? O8 Dy2 C8 96.41(13) 1_455 2_665 ? O2 Dy2 C8 76.52(12) . 2_665 ? O13 Dy2 C8 99.66(12) . 2_665 ? O4 Dy2 C8 27.07(12) 2_665 2_665 ? O15 Dy2 C8 103.54(11) . 2_665 ? O18 Dy2 C8 102.11(13) . 2_665 ? O3 Dy2 C8 26.80(12) 2_665 2_665 ? O10 Dy2 Dy1 56.61(8) . . ? O8 Dy2 Dy1 143.47(10) 1_455 . ? O2 Dy2 Dy1 59.20(8) . . ? O13 Dy2 Dy1 97.04(7) . . ? O4 Dy2 Dy1 100.22(8) 2_665 . ? O15 Dy2 Dy1 32.80(6) . . ? O18 Dy2 Dy1 98.47(8) . . ? O3 Dy2 Dy1 139.20(8) 2_665 . ? C8 Dy2 Dy1 120.07(9) 2_665 . ? C7 O1 Dy1 124.2(3) . . ? C7 O2 Dy2 133.2(3) . . ? H2WA O2W H2WB 86.1 . . ? C8 O3 Dy2 90.9(3) . 2_665 ? H3WA O3W H3WB 116.7 . . ? C8 O4 Dy2 94.5(3) . 2_665 ? H4WA O4W H4WB 125.5 . . ? C2 O5 H5A 109.5 . . ? C5 O6 H6B 109.5 . . ? C12 O7 Dy1 132.3(2) . . ? C12 O8 Dy2 159.6(3) . 1_655 ? C9 O9 H9 109.5 . . ? C16 O10 Dy2 149.2(3) . . ? C16 O11 Dy1 119.3(3) . . ? C13 O12 H12 109.5 . . ? C20 O13 Dy2 129.2(2) . . ? C20 O13 Dy1 86.8(2) . 1_455 ? Dy2 O13 Dy1 136.79(11) . 1_455 ? C20 O14 Dy1 102.3(2) . 1_455 ? C18 O15 Dy1 127.2(2) . . ? C18 O15 Dy2 116.4(2) . . ? Dy1 O15 Dy2 113.79(11) . . ? Dy1 O16 H16A 119.4 . . ? Dy1 O16 H16B 135.8 . . ? H16A O16 H16B 94.4 . . ? Dy1 O17 H17A 129.8 . . ? Dy1 O17 H17B 131.2 . . ? H17A O17 H17B 95.7 . . ? Dy2 O18 H18A 120.1 . . ? Dy2 O18 H18B 112.1 . . ? H18A O18 H18B 116.8 . . ? C6 C1 C2 118.9(4) . . ? C6 C1 C7 120.1(4) . . ? C2 C1 C7 120.9(4) . . ? O5 C2 C3 115.9(4) . . ? O5 C2 C1 124.2(4) . . ? C3 C2 C1 119.9(4) . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C4 C5 120.2(4) . . ? C3 C4 C8 118.9(4) . . ? C5 C4 C8 120.8(4) . . ? C6 C5 O6 116.2(4) . . ? C6 C5 C4 119.9(4) . . ? O6 C5 C4 123.7(4) . . ? C5 C6 C1 120.5(4) . . ? C5 C6 H6A 119.8 . . ? C1 C6 H6A 119.8 . . ? O1 C7 O2 123.1(4) . . ? O1 C7 C1 118.1(4) . . ? O2 C7 C1 118.8(4) . . ? O3 C8 O4 120.0(4) . . ? O3 C8 C4 121.5(4) . . ? O4 C8 C4 118.4(4) . . ? O3 C8 Dy2 62.3(2) . 2_665 ? O4 C8 Dy2 58.5(2) . 2_665 ? C4 C8 Dy2 168.5(3) . 2_665 ? O9 C9 C11 118.1(3) . 2_764 ? O9 C9 C10 121.5(4) . . ? C11 C9 C10 120.4(4) 2_764 . ? C11 C10 C9 118.6(4) . . ? C11 C10 C12 119.1(3) . . ? C9 C10 C12 122.3(4) . . ? C9 C11 C10 121.0(4) 2_764 . ? C9 C11 H11 119.5 2_764 . ? C10 C11 H11 119.5 . . ? O8 C12 O7 124.2(4) . . ? O8 C12 C10 117.7(4) . . ? O7 C12 C10 118.1(3) . . ? O12 C13 C15 123.6(4) . 2_654 ? O12 C13 C14 116.5(4) . . ? C15 C13 C14 119.9(4) 2_654 . ? C13 C14 C15 120.7(4) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C13 C15 C14 119.5(4) 2_654 . ? C13 C15 C16 122.1(4) 2_654 . ? C14 C15 C16 118.4(4) . . ? O11 C16 O10 122.9(4) . . ? O11 C16 C15 118.7(4) . . ? O10 C16 C15 118.4(4) . . ? C19 C17 C18 122.6(4) 2_655 . ? C19 C17 H17 118.7 2_655 . ? C18 C17 H17 118.7 . . ? O15 C18 C17 120.6(3) . . ? O15 C18 C19 123.3(3) . . ? C17 C18 C19 116.1(3) . . ? C17 C19 C18 121.3(3) 2_655 . ? C17 C19 C20 116.1(3) 2_655 . ? C18 C19 C20 122.5(3) . . ? O14 C20 O13 119.2(3) . . ? O14 C20 C19 119.3(3) . . ? O13 C20 C19 121.4(3) . . ? O14 C20 Dy1 52.50(18) . 1_455 ? O13 C20 Dy1 66.93(19) . 1_455 ? C19 C20 Dy1 169.7(3) . 1_455 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O1 0.82 1.93 2.632(5) 143.7 . O6 H6B O4 0.82 1.87 2.582(5) 144.3 . O9 H9 O7 0.82 1.90 2.582(4) 140.2 . O12 H12 O11 0.82 1.95 2.638(5) 141.5 2_654 O16 H16A O1W 0.82 2.09 2.893(6) 164.7 1_645 O16 H16B O3W 0.82 1.86 2.670(6) 172.3 . O17 H17A O1W 0.82 2.29 3.045(6) 152.3 1_545 O17 H17B O5 0.82 2.20 2.933(5) 149.3 2_755 O18 H18A O4W 0.82 1.97 2.783(6) 171.6 . O18 H18B O9 0.82 2.13 2.911(5) 160.5 . O2W H2WA O4W 0.82 2.56 3.144(10) 129.5 2_765 O2W H2WB O3 0.82 2.12 2.835(6) 146.1 . O3W H3WA O9 0.82 2.09 2.827(6) 150.3 2_754 O3W H3WB O2W 0.82 2.00 2.654(8) 136.5 2_755 O4W H4WA O12 0.82 2.31 2.924(7) 131.9 2_664 O4W H4WB O1W 0.82 2.53 3.104(8) 127.9 . _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.910 _refine_diff_density_min -0.830 _refine_diff_density_rms 0.141 #===END OF 6