# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name I.Goldberg A.Karmakar _publ_contact_author_name 'Goldberg, I.' _publ_contact_author_email GOLDBERG@POST.TAU.AC.IL data_1 _database_code_depnum_ccdc_archive 'CCDC 772531' #TrackingRef '- ka3-26-Ln.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H12 O10, 3(C12 H12 N2), 3(H2 O)' _chemical_formula_sum 'C53 H54 N6 O13' _chemical_formula_weight 983.02 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.3767(3) _cell_length_b 23.1849(7) _cell_length_c 13.7787(3) _cell_angle_alpha 90.00 _cell_angle_beta 126.7422(13) _cell_angle_gamma 90.00 _cell_volume 4960.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5214 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 26.01 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18609 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4872 _reflns_number_gt 3000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The central bond C37-C37' in one of the bipyridyl moieties is partly disordered. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+2.0290P] 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 4872 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1289 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.1599 _refine_ls_wR_factor_gt 0.1400 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 C1 C 0.5000 -0.03724(18) 0.7500 0.0313(10) Uani 1 2 d S . . H1A H 0.4494 -0.0624 0.6962 0.038 Uiso 0.50 1 calc PR . . H1B H 0.5506 -0.0624 0.8038 0.038 Uiso 0.50 1 calc PR . . O2 O 0.48538(12) -0.00302(9) 0.82123(16) 0.0333(5) Uani 1 1 d . . . C3 C 0.40651(18) 0.02353(12) 0.7639(2) 0.0290(7) Uani 1 1 d . . . C4 C 0.34642(18) 0.02842(12) 0.6385(2) 0.0291(7) Uani 1 1 d . . . H4 H 0.3579 0.0122 0.5863 0.035 Uiso 1 1 calc R . . C5 C 0.26988(18) 0.05715(13) 0.5913(2) 0.0310(7) Uani 1 1 d . . . C6 C 0.2527(2) 0.08088(13) 0.6677(3) 0.0333(7) Uani 1 1 d . . . H6 H 0.2000 0.1006 0.6347 0.040 Uiso 1 1 calc R . . C7 C 0.3129(2) 0.07552(13) 0.7927(3) 0.0329(7) Uani 1 1 d . . . C8 C 0.38967(19) 0.04689(13) 0.8407(3) 0.0315(7) Uani 1 1 d . . . H8 H 0.4308 0.0432 0.9260 0.038 Uiso 1 1 calc R . . C9 C 0.2048(2) 0.06397(13) 0.4576(3) 0.0358(7) Uani 1 1 d . . . O10 O 0.13259(14) 0.08248(10) 0.41150(19) 0.0466(6) Uani 1 1 d . . . O11 O 0.23212(14) 0.04751(12) 0.39590(18) 0.0578(7) Uani 1 1 d . . . H11 H 0.1908 0.0537 0.3165 0.069 Uiso 1 1 d R . . C12 C 0.2969(2) 0.10208(14) 0.8781(3) 0.0418(8) Uani 1 1 d . . . O13 O 0.35339(16) 0.10159(11) 0.9877(2) 0.0505(6) Uani 1 1 d . . . O14 O 0.22285(16) 0.12484(11) 0.8272(2) 0.0543(7) Uani 1 1 d . . . H14 H 0.2206 0.1411 0.8797 0.081 Uiso 1 1 calc R . . N15 N 0.2800(2) 0.32394(13) 1.0085(3) 0.0502(8) Uani 1 1 d . . . C16 C 0.3482(3) 0.29252(16) 1.0504(4) 0.0612(10) Uani 1 1 d . . . H16 H 0.3901 0.2885 1.1355 0.073 Uiso 1 1 calc R . . C17 C 0.3605(3) 0.26539(16) 0.9745(3) 0.0536(10) Uani 1 1 d . . . H17 H 0.4109 0.2428 1.0076 0.064 Uiso 1 1 calc R . . C18 C 0.3014(2) 0.26995(15) 0.8502(3) 0.0445(9) Uani 1 1 d . . . C19 C 0.2293(2) 0.30333(17) 0.8051(3) 0.0550(10) Uani 1 1 d . . . H19 H 0.1872 0.3083 0.7204 0.066 Uiso 1 1 calc R . . C20 C 0.2199(3) 0.33025(16) 0.8898(4) 0.0512(10) Uani 1 1 d . . . H20 H 0.1703 0.3529 0.8612 0.061 Uiso 1 1 calc R . . C21 C 0.3174(3) 0.23844(16) 0.7692(3) 0.0519(10) Uani 1 1 d . . . H21A H 0.3626 0.2090 0.8176 0.062 Uiso 1 1 calc R . . H21B H 0.2640 0.2181 0.7048 0.062 Uiso 1 1 calc R . . C22 C 0.3448(3) 0.27776(16) 0.7115(3) 0.0541(10) Uani 1 1 d . . . H22A H 0.3923 0.3024 0.7755 0.065 Uiso 1 1 calc R . . H22B H 0.2959 0.3034 0.6541 0.065 Uiso 1 1 calc R . . C23 C 0.3743(2) 0.24831(15) 0.6446(3) 0.0441(8) Uani 1 1 d . . . C24 C 0.3801(3) 0.18919(16) 0.6392(3) 0.0565(10) Uani 1 1 d . . . H24 H 0.3645 0.1646 0.6783 0.068 Uiso 1 1 calc R . . C25 C 0.4088(3) 0.16582(17) 0.5764(4) 0.0619(11) Uani 1 1 d . . . H25 H 0.4122 0.1250 0.5741 0.074 Uiso 1 1 calc R . . N26 N 0.4317(2) 0.19708(14) 0.5197(3) 0.0592(9) Uani 1 1 d . . . C27 C 0.4263(3) 0.25404(18) 0.5259(3) 0.0597(11) Uani 1 1 d . . . H27 H 0.4427 0.2776 0.4864 0.072 Uiso 1 1 calc R . . C28 C 0.3987(3) 0.28080(16) 0.5854(3) 0.0547(10) Uani 1 1 d . . . H28 H 0.3961 0.3217 0.5861 0.066 Uiso 1 1 calc R . . O29 O 0.52312(19) 0.14269(13) 0.1173(2) 0.0749(9) Uani 1 1 d . . . H29A H 0.4733 0.1246 0.0724 0.112 Uiso 1 1 d R . . H29B H 0.5305 0.1565 0.0618 0.112 Uiso 1 1 d R . . O30 O 0.5000 0.2196(2) 0.2500 0.0835(13) Uani 1 2 d S . . H30 H 0.5098 0.1977 0.2053 0.125 Uiso 1 1 d R . . N31 N 0.12804(17) -0.06413(11) 0.6651(2) 0.0404(7) Uani 1 1 d . . . C32 C 0.1670(2) -0.05635(14) 0.6126(3) 0.0398(8) Uani 1 1 d . . . H32 H 0.2271 -0.0487 0.6626 0.048 Uiso 1 1 calc R . . C33 C 0.1240(2) -0.05882(14) 0.4891(3) 0.0423(8) Uani 1 1 d . . . H33 H 0.1544 -0.0537 0.4554 0.051 Uiso 1 1 calc R . . C34 C 0.0368(2) -0.06875(18) 0.4152(3) 0.0564(10) Uani 1 1 d . . . C35 C -0.0033(2) -0.07787(19) 0.4707(3) 0.0613(11) Uani 1 1 d . . . H35 H -0.0631 -0.0862 0.4231 0.074 Uiso 1 1 calc R . . C36 C 0.0437(2) -0.07479(16) 0.5936(3) 0.0486(9) Uani 1 1 d . . . H36 H 0.0151 -0.0805 0.6297 0.058 Uiso 1 1 calc R . . C37 C -0.0202(2) -0.0690(3) 0.2801(3) 0.134(3) Uani 1 1 d D . . H37A H -0.0577 -0.1035 0.2526 0.160 Uiso 1 1 calc R . . H37B H -0.0581 -0.0348 0.2520 0.160 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.034(2) 0.037(2) 0.030(2) 0.000 0.023(2) 0.000 O2 0.0298(12) 0.0472(13) 0.0237(10) -0.0017(9) 0.0165(10) 0.0034(10) C3 0.0299(17) 0.0337(17) 0.0270(15) -0.0020(13) 0.0190(14) -0.0020(14) C4 0.0326(17) 0.0356(17) 0.0249(14) -0.0031(13) 0.0203(14) -0.0023(14) C5 0.0316(17) 0.0345(17) 0.0293(15) -0.0022(13) 0.0196(14) 0.0006(14) C6 0.0354(18) 0.0351(17) 0.0355(17) -0.0020(14) 0.0246(16) 0.0006(14) C7 0.0385(18) 0.0351(17) 0.0334(16) -0.0052(13) 0.0259(16) -0.0046(14) C8 0.0349(18) 0.0381(18) 0.0240(15) -0.0025(13) 0.0190(14) -0.0030(14) C9 0.0384(19) 0.0378(19) 0.0305(17) -0.0019(14) 0.0202(16) 0.0011(15) O10 0.0383(14) 0.0559(15) 0.0364(12) 0.0028(11) 0.0173(11) 0.0111(12) O11 0.0450(14) 0.102(2) 0.0217(11) 0.0056(12) 0.0175(11) 0.0237(14) C12 0.055(2) 0.041(2) 0.048(2) -0.0024(16) 0.041(2) 0.0000(17) O13 0.0592(16) 0.0693(17) 0.0329(13) -0.0096(12) 0.0328(13) -0.0023(13) O14 0.0588(17) 0.0691(18) 0.0491(14) -0.0105(13) 0.0398(14) 0.0104(14) N15 0.063(2) 0.0539(19) 0.0526(19) -0.0100(15) 0.0443(18) -0.0120(17) C16 0.068(3) 0.056(2) 0.056(2) -0.0050(19) 0.035(2) -0.001(2) C17 0.067(3) 0.058(2) 0.057(2) -0.0087(19) 0.048(2) -0.004(2) C18 0.056(2) 0.047(2) 0.053(2) -0.0146(17) 0.045(2) -0.0114(18) C19 0.056(2) 0.065(3) 0.057(2) -0.0149(19) 0.040(2) -0.004(2) C20 0.053(2) 0.047(2) 0.054(3) -0.004(2) 0.033(3) 0.0016(19) C21 0.066(3) 0.055(2) 0.055(2) -0.0116(18) 0.048(2) -0.0020(19) C22 0.082(3) 0.049(2) 0.067(2) -0.0082(18) 0.063(2) -0.002(2) C23 0.058(2) 0.043(2) 0.048(2) -0.0072(16) 0.0401(19) -0.0014(17) C24 0.089(3) 0.049(2) 0.071(3) -0.0110(19) 0.069(3) -0.009(2) C25 0.097(3) 0.047(2) 0.082(3) -0.010(2) 0.075(3) -0.005(2) N26 0.087(3) 0.058(2) 0.066(2) -0.0036(16) 0.064(2) 0.0054(18) C27 0.087(3) 0.058(3) 0.065(3) 0.006(2) 0.062(3) 0.005(2) C28 0.082(3) 0.045(2) 0.065(2) 0.0027(18) 0.059(2) 0.008(2) O29 0.089(2) 0.100(2) 0.0610(17) -0.0081(15) 0.0587(18) -0.0327(18) O30 0.085(3) 0.103(4) 0.056(2) 0.000 0.039(2) 0.000 N31 0.0435(17) 0.0468(17) 0.0275(13) 0.0004(12) 0.0194(14) -0.0039(14) C32 0.0384(19) 0.042(2) 0.0317(17) -0.0024(14) 0.0173(16) -0.0087(16) C33 0.043(2) 0.055(2) 0.0300(17) -0.0013(15) 0.0218(16) -0.0066(17) C34 0.044(2) 0.092(3) 0.0253(17) -0.0043(18) 0.0164(17) -0.009(2) C35 0.034(2) 0.108(3) 0.0343(19) -0.002(2) 0.0157(17) -0.007(2) C36 0.045(2) 0.066(2) 0.0385(19) 0.0040(17) 0.0271(18) -0.0005(19) C37 0.067(3) 0.292(9) 0.027(2) -0.018(3) 0.019(2) -0.046(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.416(3) . ? C1 O2 1.416(3) 2_656 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? O2 C3 1.376(3) . ? C3 C4 1.395(4) . ? C3 C8 1.390(4) . ? C4 C5 1.383(4) . ? C4 H4 0.9500 . ? C5 C6 1.394(4) . ? C5 C9 1.494(4) . ? C6 C7 1.392(4) . ? C6 H6 0.9500 . ? C7 C8 1.383(4) . ? C7 C12 1.515(4) . ? C8 H8 0.9500 . ? C9 O10 1.217(4) . ? C9 O11 1.299(3) . ? O11 H11 0.9008 . ? C12 O13 1.226(4) . ? C12 O14 1.275(4) . ? O14 H14 0.8400 . ? N15 C16 1.304(5) . ? N15 C20 1.332(5) . ? C16 C17 1.359(5) . ? C16 H16 0.9500 . ? C17 C18 1.382(5) . ? C17 H17 0.9500 . ? C18 C19 1.377(5) . ? C18 C21 1.514(4) . ? C19 C20 1.428(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.500(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.509(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.381(5) . ? C23 C28 1.384(5) . ? C24 C25 1.388(5) . ? C24 H24 0.9500 . ? C25 N26 1.322(4) . ? C25 H25 0.9500 . ? N26 C27 1.331(5) . ? C27 C28 1.367(5) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? O29 H29A 0.8805 . ? O29 H29B 0.9155 . ? O30 H30 0.9014 . ? N31 C36 1.333(4) . ? N31 C32 1.334(4) . ? C32 C33 1.377(4) . ? C32 H32 0.9500 . ? C33 C34 1.373(5) . ? C33 H33 0.9500 . ? C34 C35 1.395(5) . ? C34 C37 1.492(5) . ? C35 C36 1.362(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C37 1.441(6) 2 ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O2 111.9(3) . 2_656 ? O2 C1 H1A 109.2 . . ? O2 C1 H1A 109.2 2_656 . ? O2 C1 H1B 109.2 . . ? O2 C1 H1B 109.2 2_656 . ? H1A C1 H1B 107.9 . . ? C3 O2 C1 117.82(18) . . ? O2 C3 C4 124.4(2) . . ? O2 C3 C8 115.0(2) . . ? C4 C3 C8 120.6(3) . . ? C5 C4 C3 119.2(2) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 120.6(3) . . ? C4 C5 C9 120.6(2) . . ? C6 C5 C9 118.9(3) . . ? C5 C6 C7 119.8(3) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 120.0(3) . . ? C8 C7 C12 119.0(3) . . ? C6 C7 C12 121.0(3) . . ? C7 C8 C3 119.9(3) . . ? C7 C8 H8 120.1 . . ? C3 C8 H8 120.1 . . ? O10 C9 O11 123.6(3) . . ? O10 C9 C5 122.7(3) . . ? O11 C9 C5 113.7(3) . . ? C9 O11 H11 109.5 . . ? O13 C12 O14 124.3(3) . . ? O13 C12 C7 120.5(3) . . ? O14 C12 C7 115.3(3) . . ? C12 O14 H14 109.5 . . ? C16 N15 C20 121.0(3) . . ? N15 C16 C17 121.1(4) . . ? N15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C16 C17 C18 121.4(4) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C19 C18 C17 117.9(3) . . ? C19 C18 C21 122.6(3) . . ? C17 C18 C21 119.5(3) . . ? C18 C19 C20 117.8(3) . . ? C18 C19 H19 121.1 . . ? C20 C19 H19 121.1 . . ? N15 C20 C19 120.7(3) . . ? N15 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C18 113.0(3) . . ? C22 C21 H21A 109.0 . . ? C18 C21 H21A 109.0 . . ? C22 C21 H21B 109.0 . . ? C18 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C21 C22 C23 115.7(3) . . ? C21 C22 H22A 108.4 . . ? C23 C22 H22A 108.4 . . ? C21 C22 H22B 108.4 . . ? C23 C22 H22B 108.4 . . ? H22A C22 H22B 107.4 . . ? C24 C23 C28 116.2(3) . . ? C24 C23 C22 123.7(3) . . ? C28 C23 C22 120.1(3) . . ? C23 C24 C25 119.8(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? N26 C25 C24 123.7(3) . . ? N26 C25 H25 118.1 . . ? C24 C25 H25 118.1 . . ? C25 N26 C27 116.1(3) . . ? N26 C27 C28 124.2(3) . . ? N26 C27 H27 117.9 . . ? C28 C27 H27 117.9 . . ? C27 C28 C23 120.0(3) . . ? C27 C28 H28 120.0 . . ? C23 C28 H28 120.0 . . ? H29A O29 H29B 103.5 . . ? C36 N31 C32 117.7(3) . . ? N31 C32 C33 123.0(3) . . ? N31 C32 H32 118.5 . . ? C33 C32 H32 118.5 . . ? C34 C33 C32 119.3(3) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 117.4(3) . . ? C33 C34 C37 126.2(3) . . ? C35 C34 C37 116.4(3) . . ? C36 C35 C34 119.8(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? N31 C36 C35 122.8(3) . . ? N31 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? C37 C37 C34 117.8(4) 2 . ? C37 C37 H37A 107.9 2 . ? C34 C37 H37A 107.9 . . ? C37 C37 H37B 107.9 2 . ? C34 C37 H37B 107.9 . . ? H37A C37 H37B 107.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H11 N31 0.90 1.69 2.579(3) 170 6 O14 H14 N15 0.84 1.75 2.586(3) 178 7_557 O29 H29A O13 0.88 1.95 2.808(4) 165 1_554 O29 H29B N26 0.92 1.92 2.810(3) 165 2_655 O30 H30 O29 0.90 1.88 2.776(4) 171 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.343 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.045 #================END===================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 772532' #TrackingRef '- ka3-26-Ln.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H14 O10, H2 O' _chemical_formula_sum 'C18 H16 O11' _chemical_formula_weight 408.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9466(2) _cell_length_b 8.6064(2) _cell_length_c 14.9515(4) _cell_angle_alpha 79.1115(11) _cell_angle_beta 76.3526(10) _cell_angle_gamma 62.5022(10) _cell_volume 877.63(4) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3116 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 27.91 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 0.131 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f & \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9750 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 27.91 _reflns_number_total 4145 _reflns_number_gt 2855 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4145 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1418 _refine_ls_wR_factor_gt 0.1250 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 O1 O 0.8056(2) 1.00113(16) -0.26761(9) 0.0253(3) Uani 1 1 d . . . H1 H 0.7895 0.9688 -0.3186 0.030 Uiso 1 1 d R . . O2 O 0.7198(2) 0.79774(15) -0.18479(9) 0.0255(3) Uani 1 1 d . . . C3 C 0.7599(3) 0.9198(2) -0.18847(13) 0.0204(4) Uani 1 1 d . . . C4 C 0.7580(3) 0.9956(2) -0.10629(12) 0.0201(4) Uani 1 1 d . . . C5 C 0.7569(3) 1.1609(2) -0.11838(13) 0.0205(4) Uani 1 1 d . . . H5 H 0.7587 1.2232 -0.1780 0.025 Uiso 1 1 calc R . . C6 C 0.7531(3) 1.2325(2) -0.04195(13) 0.0213(4) Uani 1 1 d . . . C7 C 0.7507(3) 1.4094(2) -0.05317(13) 0.0249(4) Uani 1 1 d . . . O8 O 0.7423(3) 1.48350(18) -0.13827(10) 0.0427(4) Uani 1 1 d . . . H8 H 0.7205 1.6004 -0.1399 0.051 Uiso 1 1 d R . . O9 O 0.7548(2) 1.47933(17) 0.00874(10) 0.0373(4) Uani 1 1 d . . . C10 C 0.7508(3) 1.1417(2) 0.04598(13) 0.0214(4) Uani 1 1 d . . . H10 H 0.7513 1.1907 0.0977 0.026 Uiso 1 1 calc R . . C11 C 0.7478(3) 0.9791(2) 0.05691(12) 0.0199(4) Uani 1 1 d . . . C12 C 0.7509(3) 0.9054(2) -0.01951(12) 0.0202(4) Uani 1 1 d . . . H12 H 0.7481 0.7945 -0.0119 0.024 Uiso 1 1 calc R . . O13 O 0.7406(2) 0.88085(15) 0.14023(8) 0.0237(3) Uani 1 1 d . . . C14 C 0.7264(3) 0.9575(2) 0.22116(12) 0.0212(4) Uani 1 1 d . . . H14A H 0.6283 1.0816 0.2196 0.025 Uiso 1 1 calc R . . H14B H 0.8516 0.9544 0.2230 0.025 Uiso 1 1 calc R . . C15 C 0.6709(3) 0.8538(2) 0.30453(12) 0.0203(4) Uani 1 1 d . . . H15A H 0.6382 0.9153 0.3603 0.024 Uiso 1 1 calc R . . H15B H 0.5563 0.8420 0.2980 0.024 Uiso 1 1 calc R . . O16 O 0.82889(18) 0.68280(15) 0.31397(9) 0.0216(3) Uani 1 1 d . . . C17 C 0.8125(3) 0.5813(2) 0.39481(12) 0.0177(4) Uani 1 1 d . . . C18 C 0.9634(3) 0.4122(2) 0.40094(12) 0.0181(4) Uani 1 1 d . . . H18 H 1.0666 0.3737 0.3505 0.022 Uiso 1 1 calc R . . C19 C 0.9616(3) 0.3006(2) 0.48123(12) 0.0176(4) Uani 1 1 d . . . C20 C 1.1246(3) 0.1218(2) 0.48804(12) 0.0182(4) Uani 1 1 d . . . O21 O 1.11332(18) 0.03767(15) 0.57063(9) 0.0235(3) Uani 1 1 d . . . H21 H 1.2139 -0.0796 0.5743 0.028 Uiso 1 1 d R . . O22 O 1.25514(18) 0.05895(15) 0.42382(9) 0.0232(3) Uani 1 1 d . . . C23 C 0.8103(3) 0.3551(2) 0.55593(12) 0.0181(4) Uani 1 1 d . . . H23 H 0.8099 0.2786 0.6108 0.022 Uiso 1 1 calc R . . C24 C 0.6606(2) 0.5230(2) 0.54860(12) 0.0170(4) Uani 1 1 d . . . C25 C 0.4972(3) 0.5843(2) 0.62668(12) 0.0186(4) Uani 1 1 d . . . O26 O 0.50406(19) 0.46336(15) 0.69605(8) 0.0234(3) Uani 1 1 d . . . H26 H 0.3808 0.5065 0.7376 0.057(8) Uiso 1 1 d R . . O27 O 0.36741(19) 0.73411(15) 0.62642(9) 0.0254(3) Uani 1 1 d . . . C28 C 0.6605(3) 0.6361(2) 0.46843(12) 0.0189(4) Uani 1 1 d . . . H28 H 0.5569 0.7503 0.4641 0.023 Uiso 1 1 calc R . . O29 O 0.8110(2) 0.46336(18) 0.18421(9) 0.0327(4) Uani 1 1 d . . . H29A H 0.8207 0.5618 0.1844 0.049 Uiso 1 1 d R . . H29B H 0.7999 0.4745 0.1269 0.049 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0392(9) 0.0240(6) 0.0169(7) 0.0001(5) -0.0041(6) -0.0183(6) O2 0.0365(8) 0.0181(6) 0.0267(7) 0.0010(5) -0.0090(6) -0.0154(6) C3 0.0217(10) 0.0151(8) 0.0222(10) 0.0011(7) -0.0055(8) -0.0065(7) C4 0.0212(10) 0.0171(8) 0.0212(10) -0.0019(7) -0.0042(8) -0.0074(7) C5 0.0233(10) 0.0182(8) 0.0194(9) 0.0031(7) -0.0053(8) -0.0097(7) C6 0.0252(10) 0.0161(8) 0.0227(10) 0.0010(7) -0.0048(8) -0.0098(7) C7 0.0357(12) 0.0199(8) 0.0212(10) 0.0014(7) -0.0062(8) -0.0144(8) O8 0.0916(14) 0.0264(7) 0.0239(8) 0.0070(6) -0.0173(8) -0.0373(8) O9 0.0705(12) 0.0257(7) 0.0260(8) -0.0016(6) -0.0120(8) -0.0281(8) C10 0.0263(10) 0.0180(8) 0.0218(10) -0.0020(7) -0.0067(8) -0.0099(7) C11 0.0222(10) 0.0161(8) 0.0190(9) 0.0019(7) -0.0044(8) -0.0073(7) C12 0.0238(10) 0.0142(8) 0.0225(10) 0.0009(7) -0.0040(8) -0.0091(7) O13 0.0375(8) 0.0175(6) 0.0169(7) 0.0017(5) -0.0065(6) -0.0130(6) C14 0.0270(10) 0.0188(8) 0.0188(9) -0.0002(7) -0.0068(8) -0.0102(7) C15 0.0204(10) 0.0153(8) 0.0211(9) 0.0007(7) -0.0060(8) -0.0042(7) O16 0.0235(7) 0.0175(6) 0.0185(7) 0.0036(5) -0.0040(5) -0.0062(5) C17 0.0215(9) 0.0165(8) 0.0166(9) 0.0015(7) -0.0060(7) -0.0094(7) C18 0.0189(9) 0.0181(8) 0.0184(9) -0.0018(7) -0.0048(7) -0.0081(7) C19 0.0198(9) 0.0151(8) 0.0194(9) -0.0014(7) -0.0062(7) -0.0077(7) C20 0.0219(10) 0.0166(8) 0.0191(9) -0.0016(7) -0.0071(8) -0.0091(7) O21 0.0243(7) 0.0152(6) 0.0216(7) 0.0016(5) -0.0052(6) -0.0015(5) O22 0.0230(7) 0.0202(6) 0.0214(7) -0.0034(5) -0.0034(6) -0.0050(5) C23 0.0213(9) 0.0162(8) 0.0174(9) -0.0006(7) -0.0048(7) -0.0083(7) C24 0.0199(9) 0.0176(8) 0.0158(9) -0.0018(7) -0.0047(7) -0.0092(7) C25 0.0215(9) 0.0159(8) 0.0180(9) 0.0003(7) -0.0068(7) -0.0070(7) O26 0.0247(7) 0.0192(6) 0.0189(7) 0.0027(5) -0.0022(6) -0.0059(5) O27 0.0248(7) 0.0166(6) 0.0249(7) 0.0006(5) -0.0037(6) -0.0019(5) C28 0.0197(9) 0.0146(7) 0.0223(9) -0.0015(7) -0.0070(8) -0.0059(7) O29 0.0346(9) 0.0394(8) 0.0225(7) -0.0051(6) -0.0016(6) -0.0156(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C3 1.319(2) . ? O1 H1 0.9131 . ? O2 C3 1.220(2) . ? C3 C4 1.490(2) . ? C4 C12 1.384(2) . ? C4 C5 1.396(2) . ? C5 C6 1.386(2) . ? C5 H5 0.9500 . ? C6 C10 1.398(2) . ? C6 C7 1.491(2) . ? C7 O9 1.210(2) . ? C7 O8 1.313(2) . ? O8 H8 0.9350 . ? C10 C11 1.388(2) . ? C10 H10 0.9500 . ? C11 O13 1.372(2) . ? C11 C12 1.398(2) . ? C12 H12 0.9500 . ? O13 C14 1.442(2) . ? C14 C15 1.493(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O16 1.4357(19) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O16 C17 1.368(2) . ? C17 C28 1.391(3) . ? C17 C18 1.398(2) . ? C18 C19 1.390(2) . ? C18 H18 0.9500 . ? C19 C23 1.399(3) . ? C19 C20 1.489(2) . ? C20 O22 1.224(2) . ? C20 O21 1.314(2) . ? O21 H21 0.9570 . ? C23 C24 1.389(2) . ? C23 H23 0.9500 . ? C24 C28 1.394(2) . ? C24 C25 1.487(3) . ? C25 O27 1.224(2) . ? C25 O26 1.315(2) . ? O26 H26 0.9733 . ? C28 H28 0.9500 . ? O29 H29A 0.8857 . ? O29 H29B 0.8650 . ? 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 C3 O1 H1 114.8 . . ? O2 C3 O1 122.27(16) . . ? O2 C3 C4 124.57(17) . . ? O1 C3 C4 113.14(14) . . ? C12 C4 C5 121.08(15) . . ? C12 C4 C3 120.17(14) . . ? C5 C4 C3 118.71(16) . . ? C6 C5 C4 118.86(16) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? C5 C6 C10 120.98(15) . . ? C5 C6 C7 119.77(16) . . ? C10 C6 C7 119.25(15) . . ? O9 C7 O8 122.90(16) . . ? O9 C7 C6 124.42(17) . . ? O8 C7 C6 112.68(15) . . ? C7 O8 H8 109.5 . . ? C11 C10 C6 119.29(15) . . ? C11 C10 H10 120.4 . . ? C6 C10 H10 120.4 . . ? O13 C11 C10 124.17(15) . . ? O13 C11 C12 115.47(14) . . ? C10 C11 C12 120.36(16) . . ? C4 C12 C11 119.39(15) . . ? C4 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C11 O13 C14 116.88(12) . . ? O13 C14 C15 108.24(13) . . ? O13 C14 H14A 110.0 . . ? C15 C14 H14A 110.0 . . ? O13 C14 H14B 110.0 . . ? C15 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? O16 C15 C14 109.11(15) . . ? O16 C15 H15A 109.9 . . ? C14 C15 H15A 109.9 . . ? O16 C15 H15B 109.9 . . ? C14 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? C17 O16 C15 116.25(14) . . ? O16 C17 C28 124.66(15) . . ? O16 C17 C18 115.43(16) . . ? C28 C17 C18 119.91(16) . . ? C19 C18 C17 119.64(16) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C23 120.85(15) . . ? C18 C19 C20 119.39(16) . . ? C23 C19 C20 119.76(16) . . ? O22 C20 O21 123.29(15) . . ? O22 C20 C19 123.95(16) . . ? O21 C20 C19 112.76(15) . . ? C20 O21 H21 113.0 . . ? C24 C23 C19 118.89(16) . . ? C24 C23 H23 120.6 . . ? C19 C23 H23 120.6 . . ? C23 C24 C28 120.84(16) . . ? C23 C24 C25 120.13(15) . . ? C28 C24 C25 119.03(14) . . ? O27 C25 O26 122.87(17) . . ? O27 C25 C24 123.03(16) . . ? O26 C25 C24 114.11(14) . . ? C25 O26 H26 108.3 . . ? C17 C28 C24 119.87(15) . . ? C17 C28 H28 120.1 . . ? C24 C28 H28 120.1 . . ? H29A O29 H29B 98.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O22 0.91 1.77 2.678(2) 171 2_765 O8 H8 O2 0.93 1.70 2.595(2) 158 1_565 O21 H21 O27 0.96 1.68 2.588(2) 156 1_645 O26 H26 O29 0.97 1.63 2.593(2) 168 2_666 O29 H29A O16 0.89 2.39 3.019(2) 128 . O29 H29A O13 0.89 2.51 3.328(2) 155 . O29 H29B O9 0.86 1.87 2.732(2) 172 1_545 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.295 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.067 #=============================END================================ data_3 _database_code_depnum_ccdc_archive 'CCDC 772533' #TrackingRef '- ka3-26-Ln.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 La O11' _chemical_formula_sum 'C17 H11 La O11' _chemical_formula_weight 530.17 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8934(2) _cell_length_b 8.9328(2) _cell_length_c 12.6735(3) _cell_angle_alpha 81.2596(11) _cell_angle_beta 69.6581(11) _cell_angle_gamma 60.9613(10) _cell_volume 825.19(3) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3018 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 26.39 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 2.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5564 _exptl_absorpt_correction_T_max 0.7771 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8617 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 26.39 _reflns_number_total 3362 _reflns_number_gt 2976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.4795P] 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 3362 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 La La 1.08300(3) -0.23046(3) 0.586207(19) 0.01162(10) Uani 1 1 d . . . O1 O 0.8571(4) -0.2615(4) 0.5073(3) 0.0169(7) Uani 1 1 d . . . O2 O 0.9208(4) -0.0526(4) 0.4344(2) 0.0138(6) Uani 1 1 d . . . C3 C 0.8463(5) -0.1447(5) 0.4372(3) 0.0119(8) Uani 1 1 d . . . C4 C 0.7498(6) -0.1108(5) 0.3533(4) 0.0131(9) Uani 1 1 d . . . C5 C 0.5967(6) -0.1360(5) 0.3815(3) 0.0127(9) Uani 1 1 d . . . H5 H 0.5568 -0.1814 0.4523 0.015 Uiso 1 1 calc R . . C6 C 0.5052(5) -0.0936(5) 0.3044(3) 0.0123(9) Uani 1 1 d . . . C7 C 0.3297(6) -0.1026(5) 0.3387(3) 0.0139(9) Uani 1 1 d . . . O8 O 0.3129(4) -0.2154(4) 0.4071(2) 0.0142(6) Uani 1 1 d . . . O9 O 0.2076(4) 0.0108(4) 0.2982(2) 0.0139(6) Uani 1 1 d . . . C10 C 0.5652(6) -0.0331(5) 0.1993(3) 0.0121(8) Uani 1 1 d . . . H10 H 0.4984 -0.0013 0.1481 0.014 Uiso 1 1 calc R . . C11 C 0.7240(6) -0.0192(5) 0.1691(3) 0.0138(9) Uani 1 1 d . . . C12 C 0.8126(5) -0.0523(5) 0.2486(3) 0.0114(8) Uani 1 1 d . . . H12 H 0.9158 -0.0345 0.2305 0.014 Uiso 1 1 calc R . . O13 O 0.8032(4) 0.0286(4) 0.0647(2) 0.0157(6) Uani 1 1 d . . . C14 C 0.7448(6) 0.0192(6) -0.0233(4) 0.0165(9) Uani 1 1 d . . . H14A H 0.7291 -0.0848 -0.0146 0.020 Uiso 1 1 calc R . . H14B H 0.8393 0.0090 -0.0962 0.020 Uiso 1 1 calc R . . O15 O 0.5786(4) 0.1656(4) -0.0243(3) 0.0163(6) Uani 1 1 d . . . C16 C 0.5908(6) 0.3031(5) -0.0870(4) 0.0141(9) Uani 1 1 d . . . C17 C 0.7296(6) 0.3437(5) -0.1026(3) 0.0141(9) Uani 1 1 d . . . H17 H 0.8177 0.2827 -0.0650 0.017 Uiso 1 1 calc R . . C18 C 0.7358(6) 0.4767(5) -0.1751(3) 0.0135(9) Uani 1 1 d . . . C19 C 0.8830(6) 0.5256(5) -0.2029(4) 0.0156(9) Uani 1 1 d . . . O20 O 0.9653(5) 0.4881(4) -0.1259(3) 0.0226(7) Uani 1 1 d . . . H20 H 1.0569 0.5155 -0.1521 0.027 Uiso 1 1 d R . . O21 O 0.9222(4) 0.5970(4) -0.2900(3) 0.0203(7) Uani 1 1 d . . . C22 C 0.6060(6) 0.5673(5) -0.2289(4) 0.0137(9) Uani 1 1 d . . . H22 H 0.6150 0.6538 -0.2806 0.016 Uiso 1 1 calc R . . C23 C 0.4622(6) 0.5309(5) -0.2066(3) 0.0131(9) Uani 1 1 d . . . C24 C 0.3266(6) 0.6256(5) -0.2688(4) 0.0123(9) Uani 1 1 d . . . O25 O 0.1645(4) 0.6499(4) -0.2243(3) 0.0184(7) Uani 1 1 d . . . O26 O 0.3785(4) 0.6774(4) -0.3662(3) 0.0156(6) Uani 1 1 d . . . C27 C 0.4536(6) 0.4001(5) -0.1338(4) 0.0153(9) Uani 1 1 d . . . H27 H 0.3538 0.3774 -0.1163 0.018 Uiso 1 1 calc R . . O28 O 1.2588(4) -0.5130(4) 0.4965(3) 0.0181(7) Uani 1 1 d . . . H28A H 1.2202 -0.5974 0.4986 0.022 Uiso 1 1 d R . . H28B H 1.3755 -0.5567 0.4552 0.022 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La 0.01107(15) 0.01302(15) 0.01334(15) 0.00203(10) -0.00553(10) -0.00693(11) O1 0.0236(17) 0.0171(15) 0.0184(16) 0.0074(13) -0.0140(13) -0.0129(13) O2 0.0160(15) 0.0154(15) 0.0181(15) 0.0044(12) -0.0101(13) -0.0114(13) C3 0.0075(19) 0.015(2) 0.0097(19) -0.0005(17) -0.0009(15) -0.0039(16) C4 0.016(2) 0.0086(19) 0.015(2) -0.0008(17) -0.0076(17) -0.0034(17) C5 0.017(2) 0.013(2) 0.010(2) 0.0016(17) -0.0048(17) -0.0087(17) C6 0.009(2) 0.0100(19) 0.014(2) -0.0015(16) -0.0029(16) -0.0015(16) C7 0.015(2) 0.015(2) 0.012(2) -0.0059(18) -0.0013(17) -0.0071(18) O8 0.0141(15) 0.0156(15) 0.0144(15) 0.0038(13) -0.0052(12) -0.0085(13) O9 0.0084(14) 0.0178(15) 0.0152(15) 0.0011(13) -0.0056(12) -0.0048(12) C10 0.013(2) 0.014(2) 0.013(2) -0.0008(17) -0.0080(17) -0.0060(17) C11 0.016(2) 0.013(2) 0.011(2) 0.0012(17) -0.0037(17) -0.0062(18) C12 0.0084(19) 0.014(2) 0.014(2) 0.0007(17) -0.0049(16) -0.0061(16) O13 0.0126(15) 0.0231(16) 0.0135(15) 0.0060(13) -0.0041(12) -0.0114(13) C14 0.019(2) 0.018(2) 0.015(2) 0.0006(18) -0.0068(18) -0.0096(19) O15 0.0149(15) 0.0210(16) 0.0167(15) 0.0082(13) -0.0069(13) -0.0120(13) C16 0.016(2) 0.015(2) 0.014(2) 0.0005(17) -0.0040(17) -0.0090(18) C17 0.015(2) 0.016(2) 0.013(2) 0.0033(17) -0.0087(17) -0.0069(18) C18 0.017(2) 0.014(2) 0.013(2) -0.0004(17) -0.0047(17) -0.0098(18) C19 0.015(2) 0.011(2) 0.020(2) 0.0015(18) -0.0079(18) -0.0045(18) O20 0.0228(17) 0.041(2) 0.0206(17) 0.0161(15) -0.0159(14) -0.0261(16) O21 0.0244(17) 0.0265(17) 0.0210(17) 0.0119(14) -0.0137(14) -0.0189(15) C22 0.017(2) 0.011(2) 0.013(2) 0.0001(17) -0.0029(17) -0.0083(17) C23 0.017(2) 0.012(2) 0.014(2) 0.0024(17) -0.0086(17) -0.0073(18) C24 0.013(2) 0.013(2) 0.015(2) 0.0016(17) -0.0073(17) -0.0075(17) O25 0.0154(16) 0.0253(17) 0.0201(16) 0.0060(14) -0.0092(13) -0.0129(14) O26 0.0147(15) 0.0160(15) 0.0175(16) 0.0049(13) -0.0080(13) -0.0074(13) C27 0.016(2) 0.018(2) 0.016(2) -0.0003(18) -0.0070(17) -0.0094(18) O28 0.0143(15) 0.0141(15) 0.0257(17) -0.0007(13) -0.0039(13) -0.0075(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La O28 2.431(3) . ? La O9 2.448(3) 2_656 ? La O2 2.487(3) 2_756 ? La O8 2.510(3) 1_655 ? La O21 2.594(3) 1_546 ? La O26 2.607(3) 1_646 ? La O2 2.662(3) . ? La O25 2.667(3) 1_646 ? La O1 2.671(3) . ? La C24 3.012(4) 1_646 ? La C3 3.056(4) . ? La La 4.1850(5) 2_756 ? O1 C3 1.252(5) . ? O2 C3 1.273(5) . ? O2 La 2.487(3) 2_756 ? C3 C4 1.498(6) . ? C4 C12 1.380(6) . ? C4 C5 1.403(6) . ? C5 C6 1.379(6) . ? C5 H5 0.9500 . ? C6 C10 1.385(6) . ? C6 C7 1.507(6) . ? C7 O8 1.257(5) . ? C7 O9 1.277(5) . ? O8 La 2.510(3) 1_455 ? O9 La 2.448(3) 2_656 ? C10 C11 1.391(6) . ? C10 H10 0.9500 . ? C11 O13 1.379(5) . ? C11 C12 1.399(6) . ? C12 H12 0.9500 . ? O13 C14 1.412(5) . ? C14 O15 1.424(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O15 C16 1.388(5) . ? C16 C27 1.383(6) . ? C16 C17 1.392(6) . ? C17 C18 1.399(6) . ? C17 H17 0.9500 . ? C18 C22 1.387(6) . ? C18 C19 1.489(6) . ? C19 O21 1.216(6) . ? C19 O20 1.327(5) . ? O20 H20 0.9018 . ? O21 La 2.594(3) 1_564 ? C22 C23 1.395(6) . ? C22 H22 0.9500 . ? C23 C27 1.390(6) . ? C23 C24 1.503(6) . ? C24 O26 1.261(5) . ? C24 O25 1.270(5) . ? C24 La 3.012(4) 1_464 ? O25 La 2.667(3) 1_464 ? O26 La 2.607(3) 1_464 ? C27 H27 0.9500 . ? O28 H28A 0.9619 . ? O28 H28B 0.8918 . ? 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 O28 La O9 148.69(10) . 2_656 ? O28 La O2 140.16(10) . 2_756 ? O9 La O2 69.17(10) 2_656 2_756 ? O28 La O8 72.46(10) . 1_655 ? O9 La O8 132.26(10) 2_656 1_655 ? O2 La O8 68.04(9) 2_756 1_655 ? O28 La O21 75.90(10) . 1_546 ? O9 La O21 76.08(10) 2_656 1_546 ? O2 La O21 143.91(10) 2_756 1_546 ? O8 La O21 147.81(10) 1_655 1_546 ? O28 La O26 82.24(10) . 1_646 ? O9 La O26 120.04(9) 2_656 1_646 ? O2 La O26 81.74(9) 2_756 1_646 ? O8 La O26 73.12(9) 1_655 1_646 ? O21 La O26 108.47(10) 1_546 1_646 ? O28 La O2 99.94(10) . . ? O9 La O2 77.28(9) 2_656 . ? O2 La O2 71.30(10) 2_756 . ? O8 La O2 69.87(9) 1_655 . ? O21 La O2 110.61(9) 1_546 . ? O26 La O2 140.17(9) 1_646 . ? O28 La O25 92.79(10) . 1_646 ? O9 La O25 87.65(10) 2_656 1_646 ? O2 La O25 103.74(9) 2_756 1_646 ? O8 La O25 122.29(9) 1_655 1_646 ? O21 La O25 64.63(10) 1_546 1_646 ? O26 La O25 49.40(9) 1_646 1_646 ? O2 La O25 164.93(9) . 1_646 ? O28 La O1 75.48(10) . . ? O9 La O1 80.02(9) 2_656 . ? O2 La O1 116.97(10) 2_756 . ? O8 La O1 101.45(9) 1_655 . ? O21 La O1 64.38(10) 1_546 . ? O26 La O1 157.64(9) 1_646 . ? O2 La O1 48.49(9) . . ? O25 La O1 129.01(10) 1_646 . ? O28 La C24 85.51(11) . 1_646 ? O9 La C24 106.07(10) 2_656 1_646 ? O2 La C24 94.46(10) 2_756 1_646 ? O8 La C24 97.39(11) 1_655 1_646 ? O21 La C24 85.82(11) 1_546 1_646 ? O26 La C24 24.60(11) 1_646 1_646 ? O2 La C24 163.46(11) . 1_646 ? O25 La C24 24.91(10) 1_646 1_646 ? O1 La C24 147.58(11) . 1_646 ? O28 La C3 86.30(10) . . ? O9 La C3 78.87(10) 2_656 . ? O2 La C3 94.82(10) 2_756 . ? O8 La C3 84.58(10) 1_655 . ? O21 La C3 87.66(11) 1_546 . ? O26 La C3 157.12(10) 1_646 . ? O2 La C3 24.50(10) . . ? O25 La C3 151.50(10) 1_646 . ? O1 La C3 24.06(11) . . ? C24 La C3 170.57(11) 1_646 . ? O28 La La 124.48(8) . 2_756 ? O9 La La 69.43(7) 2_656 2_756 ? O2 La La 37.05(7) 2_756 2_756 ? O8 La La 63.82(7) 1_655 2_756 ? O21 La La 134.76(7) 1_546 2_756 ? O26 La La 113.77(7) 1_646 2_756 ? O2 La La 34.26(6) . 2_756 ? O25 La La 139.05(7) 1_646 2_756 ? O1 La La 81.26(7) . 2_756 ? C24 La La 130.99(8) 1_646 2_756 ? C3 La La 58.07(8) . 2_756 ? C3 O1 La 95.5(3) . . ? C3 O2 La 150.7(3) . 2_756 ? C3 O2 La 95.4(2) . . ? La O2 La 108.70(10) 2_756 . ? O1 C3 O2 120.3(4) . . ? O1 C3 C4 121.7(4) . . ? O2 C3 C4 118.0(4) . . ? O1 C3 La 60.5(2) . . ? O2 C3 La 60.1(2) . . ? C4 C3 La 173.5(3) . . ? C12 C4 C5 120.7(4) . . ? C12 C4 C3 118.9(4) . . ? C5 C4 C3 120.4(4) . . ? C6 C5 C4 118.6(4) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C5 C6 C10 121.4(4) . . ? C5 C6 C7 118.8(4) . . ? C10 C6 C7 119.6(4) . . ? O8 C7 O9 125.6(4) . . ? O8 C7 C6 118.1(4) . . ? O9 C7 C6 116.3(4) . . ? C7 O8 La 137.3(3) . 1_455 ? C7 O9 La 123.3(3) . 2_656 ? C6 C10 C11 119.6(4) . . ? C6 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? O13 C11 C10 124.8(4) . . ? O13 C11 C12 115.6(4) . . ? C10 C11 C12 119.6(4) . . ? C4 C12 C11 119.8(4) . . ? C4 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C11 O13 C14 115.8(3) . . ? O13 C14 O15 112.2(3) . . ? O13 C14 H14A 109.2 . . ? O15 C14 H14A 109.2 . . ? O13 C14 H14B 109.2 . . ? O15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 O15 C14 116.8(3) . . ? C27 C16 O15 115.3(4) . . ? C27 C16 C17 121.3(4) . . ? O15 C16 C17 123.4(4) . . ? C16 C17 C18 118.1(4) . . ? C16 C17 H17 121.0 . . ? C18 C17 H17 121.0 . . ? C22 C18 C17 121.0(4) . . ? C22 C18 C19 116.0(4) . . ? C17 C18 C19 123.0(4) . . ? O21 C19 O20 122.9(4) . . ? O21 C19 C18 121.7(4) . . ? O20 C19 C18 115.4(4) . . ? C19 O20 H20 109.0 . . ? C19 O21 La 151.3(3) . 1_564 ? C18 C22 C23 119.7(4) . . ? C18 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C27 C23 C22 119.8(4) . . ? C27 C23 C24 121.1(4) . . ? C22 C23 C24 119.0(4) . . ? O26 C24 O25 121.1(4) . . ? O26 C24 C23 118.5(4) . . ? O25 C24 C23 120.3(4) . . ? O26 C24 La 59.4(2) . 1_464 ? O25 C24 La 62.2(2) . 1_464 ? C23 C24 La 171.8(3) . 1_464 ? C24 O25 La 92.9(3) . 1_464 ? C24 O26 La 96.0(2) . 1_464 ? C16 C27 C23 119.8(4) . . ? C16 C27 H27 120.1 . . ? C23 C27 H27 120.1 . . ? La O28 H28A 128.5 . . ? La O28 H28B 123.9 . . ? H28A O28 H28B 107.7 . . ? 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 O20 H20 O25 0.90 1.83 2.680(4) 155 1_655 O28 H28A O1 0.96 1.72 2.684(4) 175 2_746 O28 H28B O26 0.89 1.89 2.779(4) 172 2_755 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.567 _refine_diff_density_min -1.258 _refine_diff_density_rms 0.160 #=================END=================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 772534' #TrackingRef '- ka3-26-Ln.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 Nd O11' _chemical_formula_sum 'C17 H11 Nd O11' _chemical_formula_weight 535.50 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' 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.82770(10) _cell_length_b 8.8751(2) _cell_length_c 12.6582(3) _cell_angle_alpha 81.0037(8) _cell_angle_beta 69.8251(9) _cell_angle_gamma 61.2379(18) _cell_volume 815.98(3) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3022 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 27.91 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 522 _exptl_absorpt_coefficient_mu 3.250 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4422 _exptl_absorpt_correction_T_max 0.7370 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9148 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.91 _reflns_number_total 3846 _reflns_number_gt 3435 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution DIRDIF-96 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+1.7366P] 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 3846 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Nd Nd 1.08292(3) -0.22930(3) 0.582378(17) 0.01027(9) Uani 1 1 d . . . O1 O 0.8653(4) -0.2663(4) 0.5026(3) 0.0148(6) Uani 1 1 d . . . O2 O 0.9184(4) -0.0476(4) 0.4356(2) 0.0128(6) Uani 1 1 d . . . C3 C 0.8482(5) -0.1427(5) 0.4353(3) 0.0093(7) Uani 1 1 d . . . C4 C 0.7483(5) -0.1084(5) 0.3526(3) 0.0113(8) Uani 1 1 d . . . C5 C 0.5957(5) -0.1338(5) 0.3811(4) 0.0121(8) Uani 1 1 d . . . H5 H 0.5569 -0.1805 0.4520 0.015 Uiso 1 1 calc R . . C6 C 0.5006(5) -0.0898(5) 0.3041(3) 0.0106(8) Uani 1 1 d . . . C7 C 0.3233(5) -0.0985(5) 0.3397(3) 0.0113(8) Uani 1 1 d . . . O8 O 0.3073(4) -0.2141(4) 0.4061(2) 0.0128(6) Uani 1 1 d . . . O9 O 0.2008(4) 0.0190(4) 0.3016(2) 0.0122(6) Uani 1 1 d . . . C10 C 0.5617(5) -0.0289(5) 0.1985(3) 0.0120(8) Uani 1 1 d . . . H10 H 0.4947 0.0030 0.1470 0.014 Uiso 1 1 calc R . . C11 C 0.7207(5) -0.0149(5) 0.1687(3) 0.0121(8) Uani 1 1 d . . . C12 C 0.8121(5) -0.0493(5) 0.2471(3) 0.0108(8) Uani 1 1 d . . . H12 H 0.9167 -0.0324 0.2284 0.013 Uiso 1 1 calc R . . O13 O 0.7994(4) 0.0329(4) 0.0640(2) 0.0149(6) Uani 1 1 d . . . C14 C 0.7395(6) 0.0240(5) -0.0239(4) 0.0146(8) Uani 1 1 d . . . H14A H 0.7228 -0.0804 -0.0147 0.018 Uiso 1 1 calc R . . H14B H 0.8343 0.0137 -0.0968 0.018 Uiso 1 1 calc R . . O15 O 0.5733(4) 0.1707(4) -0.0260(3) 0.0159(6) Uani 1 1 d . . . C16 C 0.5863(5) 0.3081(5) -0.0899(3) 0.0129(8) Uani 1 1 d . . . C17 C 0.7273(5) 0.3487(5) -0.1065(4) 0.0135(8) Uani 1 1 d . . . H17 H 0.8153 0.2881 -0.0682 0.016 Uiso 1 1 calc R . . C18 C 0.7358(5) 0.4807(5) -0.1808(3) 0.0121(8) Uani 1 1 d . . . C19 C 0.8843(5) 0.5294(5) -0.2080(4) 0.0132(8) Uani 1 1 d . . . O20 O 0.9635(4) 0.4974(5) -0.1299(3) 0.0232(7) Uani 1 1 d . . . H20 H 1.0550 0.5248 -0.1562 0.028 Uiso 1 1 d R . . O21 O 0.9258(4) 0.5980(4) -0.2966(3) 0.0175(6) Uani 1 1 d . . . C22 C 0.6054(5) 0.5721(5) -0.2354(4) 0.0120(8) Uani 1 1 d . . . H22 H 0.6153 0.6584 -0.2881 0.014 Uiso 1 1 calc R . . C23 C 0.4597(5) 0.5357(5) -0.2119(3) 0.0113(8) Uani 1 1 d . . . C24 C 0.3252(5) 0.6307(5) -0.2754(4) 0.0117(8) Uani 1 1 d . . . O25 O 0.1600(4) 0.6611(4) -0.2304(3) 0.0166(6) Uani 1 1 d . . . O26 O 0.3780(4) 0.6783(4) -0.3746(2) 0.0135(6) Uani 1 1 d . . . C27 C 0.4486(5) 0.4057(5) -0.1381(3) 0.0127(8) Uani 1 1 d . . . H27 H 0.3476 0.3835 -0.1205 0.015 Uiso 1 1 calc R . . O28 O 1.2570(4) -0.5101(4) 0.5021(3) 0.0164(6) Uani 1 1 d . . . H28A H 1.2185 -0.5945 0.5041 0.020 Uiso 1 1 d R . . H28B H 1.3738 -0.5538 0.4607 0.020 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd 0.00829(12) 0.01243(13) 0.01293(13) 0.00325(8) -0.00556(8) -0.00633(9) O1 0.0202(15) 0.0157(15) 0.0183(16) 0.0081(12) -0.0133(13) -0.0132(12) O2 0.0124(13) 0.0166(15) 0.0147(15) 0.0020(12) -0.0068(11) -0.0094(12) C3 0.0059(17) 0.016(2) 0.0076(18) -0.0007(15) -0.0022(14) -0.0056(15) C4 0.0101(18) 0.0097(19) 0.014(2) -0.0017(16) -0.0061(15) -0.0021(15) C5 0.0127(19) 0.0094(19) 0.014(2) 0.0013(16) -0.0026(15) -0.0058(15) C6 0.0085(17) 0.0103(19) 0.013(2) 0.0003(15) -0.0034(15) -0.0045(15) C7 0.0100(18) 0.013(2) 0.0111(19) -0.0037(16) -0.0015(15) -0.0056(15) O8 0.0096(13) 0.0165(15) 0.0133(14) 0.0027(12) -0.0028(11) -0.0080(11) O9 0.0078(13) 0.0152(15) 0.0133(14) 0.0028(12) -0.0051(11) -0.0046(11) C10 0.0122(19) 0.015(2) 0.012(2) 0.0012(16) -0.0056(15) -0.0082(16) C11 0.0132(19) 0.013(2) 0.011(2) 0.0040(16) -0.0044(16) -0.0078(16) C12 0.0066(17) 0.0130(19) 0.017(2) 0.0017(16) -0.0069(15) -0.0057(15) O13 0.0121(14) 0.0234(16) 0.0127(15) 0.0062(12) -0.0060(12) -0.0111(12) C14 0.017(2) 0.013(2) 0.016(2) 0.0064(16) -0.0095(17) -0.0063(17) O15 0.0145(14) 0.0207(16) 0.0175(16) 0.0091(13) -0.0083(12) -0.0121(13) C16 0.0129(19) 0.015(2) 0.012(2) 0.0025(16) -0.0047(16) -0.0081(16) C17 0.0111(18) 0.016(2) 0.017(2) 0.0038(17) -0.0076(16) -0.0074(16) C18 0.0135(19) 0.015(2) 0.011(2) 0.0003(16) -0.0044(15) -0.0085(16) C19 0.0108(18) 0.012(2) 0.020(2) 0.0021(17) -0.0072(16) -0.0062(16) O20 0.0222(16) 0.042(2) 0.0216(17) 0.0146(15) -0.0164(14) -0.0247(16) O21 0.0183(15) 0.0245(17) 0.0186(16) 0.0096(13) -0.0101(13) -0.0163(13) C22 0.0116(18) 0.0118(19) 0.015(2) 0.0008(16) -0.0047(16) -0.0072(16) C23 0.0092(17) 0.013(2) 0.013(2) -0.0005(16) -0.0033(15) -0.0061(15) C24 0.0107(18) 0.013(2) 0.016(2) 0.0022(16) -0.0072(16) -0.0074(15) O25 0.0102(14) 0.0239(17) 0.0201(16) 0.0051(13) -0.0079(12) -0.0104(12) O26 0.0121(14) 0.0174(15) 0.0127(15) 0.0025(12) -0.0055(11) -0.0077(12) C27 0.0117(19) 0.020(2) 0.0081(19) -0.0005(16) -0.0016(15) -0.0098(17) O28 0.0112(14) 0.0132(15) 0.0244(17) -0.0028(13) -0.0022(12) -0.0067(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 Nd O28 2.374(3) . ? Nd O9 2.395(3) 2_656 ? Nd O2 2.428(3) 2_756 ? Nd O8 2.457(3) 1_655 ? Nd O21 2.543(3) 1_546 ? Nd O26 2.557(3) 1_646 ? Nd O25 2.604(3) 1_646 ? Nd O2 2.614(3) . ? Nd O1 2.620(3) . ? Nd C24 2.959(4) 1_646 ? Nd C3 3.006(4) . ? Nd Nd 4.0958(4) 2_756 ? O1 C3 1.260(5) . ? O2 C3 1.266(5) . ? O2 Nd 2.428(3) 2_756 ? C3 C4 1.498(5) . ? C4 C12 1.386(6) . ? C4 C5 1.388(5) . ? C5 C6 1.393(5) . ? C5 H5 0.9500 . ? C6 C10 1.388(6) . ? C6 C7 1.509(5) . ? C7 O8 1.251(5) . ? C7 O9 1.268(5) . ? O8 Nd 2.457(3) 1_455 ? O9 Nd 2.395(3) 2_656 ? C10 C11 1.384(5) . ? C10 H10 0.9500 . ? C11 O13 1.375(5) . ? C11 C12 1.397(5) . ? C12 H12 0.9500 . ? O13 C14 1.414(5) . ? C14 O15 1.423(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O15 C16 1.385(5) . ? C16 C27 1.390(5) . ? C16 C17 1.396(5) . ? C17 C18 1.398(6) . ? C17 H17 0.9500 . ? C18 C22 1.392(5) . ? C18 C19 1.488(5) . ? C19 O21 1.217(5) . ? C19 O20 1.320(5) . ? O20 H20 0.8948 . ? O21 Nd 2.543(3) 1_564 ? C22 C23 1.398(5) . ? C22 H22 0.9500 . ? C23 C27 1.386(6) . ? C23 C24 1.499(5) . ? C24 O26 1.262(5) . ? C24 O25 1.273(5) . ? C24 Nd 2.959(4) 1_464 ? O25 Nd 2.604(3) 1_464 ? O26 Nd 2.557(3) 1_464 ? C27 H27 0.9500 . ? O28 H28A 0.9542 . ? O28 H28B 0.8906 . ? 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 O28 Nd O9 148.02(10) . 2_656 ? O28 Nd O2 141.33(10) . 2_756 ? O9 Nd O2 69.91(10) 2_656 2_756 ? O28 Nd O8 73.35(10) . 1_655 ? O9 Nd O8 133.63(10) 2_656 1_655 ? O2 Nd O8 68.87(10) 2_756 1_655 ? O28 Nd O21 74.55(10) . 1_546 ? O9 Nd O21 75.42(10) 2_656 1_546 ? O2 Nd O21 143.90(10) 2_756 1_546 ? O8 Nd O21 147.04(10) 1_655 1_546 ? O28 Nd O26 79.97(10) . 1_646 ? O9 Nd O26 120.51(9) 2_656 1_646 ? O2 Nd O26 81.22(9) 2_756 1_646 ? O8 Nd O26 72.52(9) 1_655 1_646 ? O21 Nd O26 108.91(9) 1_546 1_646 ? O28 Nd O25 92.09(10) . 1_646 ? O9 Nd O25 85.32(9) 2_656 1_646 ? O2 Nd O25 101.36(9) 2_756 1_646 ? O8 Nd O25 122.85(9) 1_655 1_646 ? O21 Nd O25 65.48(9) 1_546 1_646 ? O26 Nd O25 50.40(9) 1_646 1_646 ? O28 Nd O2 103.39(10) . . ? O9 Nd O2 77.35(9) 2_656 . ? O2 Nd O2 71.38(10) 2_756 . ? O8 Nd O2 70.21(9) 1_655 . ? O21 Nd O2 110.74(9) 1_546 . ? O26 Nd O2 139.61(9) 1_646 . ? O25 Nd O2 162.60(10) 1_646 . ? O28 Nd O1 75.70(10) . . ? O9 Nd O1 81.60(10) 2_656 . ? O2 Nd O1 118.61(9) 2_756 . ? O8 Nd O1 100.30(9) 1_655 . ? O21 Nd O1 64.31(9) 1_546 . ? O26 Nd O1 155.67(10) 1_646 . ? O25 Nd O1 129.78(9) 1_646 . ? O2 Nd O1 49.43(9) . . ? O28 Nd C24 83.70(11) . 1_646 ? O9 Nd C24 105.11(10) 2_656 1_646 ? O2 Nd C24 93.11(10) 2_756 1_646 ? O8 Nd C24 97.41(10) 1_655 1_646 ? O21 Nd C24 86.30(10) 1_546 1_646 ? O26 Nd C24 25.10(10) 1_646 1_646 ? O25 Nd C24 25.44(10) 1_646 1_646 ? O2 Nd C24 162.67(10) . 1_646 ? O1 Nd C24 147.53(10) . 1_646 ? O28 Nd C3 88.49(10) . . ? O9 Nd C3 79.63(10) 2_656 . ? O2 Nd C3 95.44(10) 2_756 . ? O8 Nd C3 84.04(10) 1_655 . ? O21 Nd C3 87.84(10) 1_546 . ? O26 Nd C3 155.98(10) 1_646 . ? O25 Nd C3 152.02(10) 1_646 . ? O2 Nd C3 24.80(10) . . ? O1 Nd C3 24.69(10) . . ? C24 Nd C3 171.26(11) 1_646 . ? O28 Nd Nd 127.63(7) . 2_756 ? O9 Nd Nd 69.92(7) 2_656 2_756 ? O2 Nd Nd 37.21(6) 2_756 2_756 ? O8 Nd Nd 64.55(7) 1_655 2_756 ? O21 Nd Nd 134.81(7) 1_546 2_756 ? O26 Nd Nd 113.30(7) 1_646 2_756 ? O25 Nd Nd 136.53(7) 1_646 2_756 ? O2 Nd Nd 34.17(6) . 2_756 ? O1 Nd Nd 82.46(6) . 2_756 ? C24 Nd Nd 129.89(8) 1_646 2_756 ? C3 Nd Nd 58.46(8) . 2_756 ? C3 O1 Nd 95.0(2) . . ? C3 O2 Nd 152.2(3) . 2_756 ? C3 O2 Nd 95.2(2) . . ? Nd O2 Nd 108.62(10) 2_756 . ? O1 C3 O2 120.0(3) . . ? O1 C3 C4 120.8(3) . . ? O2 C3 C4 119.2(4) . . ? O1 C3 Nd 60.28(19) . . ? O2 C3 Nd 59.98(19) . . ? C4 C3 Nd 174.3(3) . . ? C12 C4 C5 121.1(4) . . ? C12 C4 C3 118.0(3) . . ? C5 C4 C3 121.0(4) . . ? C4 C5 C6 118.9(4) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C10 C6 C5 120.7(4) . . ? C10 C6 C7 120.3(3) . . ? C5 C6 C7 118.9(4) . . ? O8 C7 O9 126.1(4) . . ? O8 C7 C6 118.4(3) . . ? O9 C7 C6 115.4(4) . . ? C7 O8 Nd 136.3(3) . 1_455 ? C7 O9 Nd 123.8(3) . 2_656 ? C11 C10 C6 119.7(4) . . ? C11 C10 H10 120.1 . . ? C6 C10 H10 120.1 . . ? O13 C11 C10 124.4(3) . . ? O13 C11 C12 115.4(3) . . ? C10 C11 C12 120.3(4) . . ? C4 C12 C11 119.2(4) . . ? C4 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C11 O13 C14 116.1(3) . . ? O13 C14 O15 112.4(3) . . ? O13 C14 H14A 109.1 . . ? O15 C14 H14A 109.1 . . ? O13 C14 H14B 109.1 . . ? O15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C16 O15 C14 116.9(3) . . ? O15 C16 C27 115.7(3) . . ? O15 C16 C17 123.3(3) . . ? C27 C16 C17 121.1(4) . . ? C16 C17 C18 118.3(4) . . ? C16 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? C22 C18 C17 121.1(4) . . ? C22 C18 C19 116.2(4) . . ? C17 C18 C19 122.7(4) . . ? O21 C19 O20 122.9(4) . . ? O21 C19 C18 120.9(4) . . ? O20 C19 C18 116.1(4) . . ? C19 O20 H20 109.1 . . ? C19 O21 Nd 150.4(3) . 1_564 ? C18 C22 C23 119.2(4) . . ? C18 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C27 C23 C22 120.4(4) . . ? C27 C23 C24 121.2(3) . . ? C22 C23 C24 118.2(4) . . ? O26 C24 O25 120.2(4) . . ? O26 C24 C23 119.3(3) . . ? O25 C24 C23 120.4(4) . . ? O26 C24 Nd 59.29(19) . 1_464 ? O25 C24 Nd 61.5(2) . 1_464 ? C23 C24 Nd 171.7(3) . 1_464 ? C24 O25 Nd 93.1(2) . 1_464 ? C24 O26 Nd 95.6(2) . 1_464 ? C23 C27 C16 119.6(4) . . ? C23 C27 H27 120.2 . . ? C16 C27 H27 120.2 . . ? Nd O28 H28A 128.6 . . ? Nd O28 H28B 124.1 . . ? H28A O28 H28B 107.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O20 H20 O25 0.89 1.82 2.657(4) 154 1_655 O28 H28A O1 0.95 1.74 2.693(4) 174 2_746 O28 H28B O26 0.89 1.90 2.784(4) 172 2_755 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.096 _refine_diff_density_min -1.440 _refine_diff_density_rms 0.179 #============================END======================= data_5 _database_code_depnum_ccdc_archive 'CCDC 772535' #TrackingRef '- ka3-26-Ln.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H13 O12 Sm, 5(H2 O)' _chemical_formula_sum 'C17 H23 O17 Sm' _chemical_formula_weight 649.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9205(2) _cell_length_b 10.6776(3) _cell_length_c 11.7567(4) _cell_angle_alpha 96.6635(12) _cell_angle_beta 108.3377(13) _cell_angle_gamma 106.8366(15) _cell_volume 1101.63(5) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4148 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 26.35 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.959 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 646 _exptl_absorpt_coefficient_mu 2.753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6829 _exptl_absorpt_correction_T_max 0.7704 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13401 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 26.35 _reflns_number_total 4445 _reflns_number_gt 4174 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+3.3076P] 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 4445 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm Sm 1.095963(18) 0.860672(16) 0.481659(15) 0.00746(7) Uani 1 1 d . . . O1 O 0.8427(3) 0.7166(2) 0.3303(2) 0.0121(5) Uani 1 1 d . . . O2 O 0.8424(3) 0.9124(2) 0.4109(2) 0.0104(5) Uani 1 1 d . . . C3 C 0.7711(4) 0.7950(3) 0.3429(3) 0.0097(7) Uani 1 1 d . . . C4 C 0.6033(4) 0.7471(3) 0.2815(3) 0.0092(7) Uani 1 1 d . . . C5 C 0.5180(4) 0.8003(3) 0.3331(3) 0.0093(7) Uani 1 1 d . . . H5 H 0.5667 0.8723 0.4041 0.011 Uiso 1 1 calc R . . C6 C 0.3610(4) 0.7477(3) 0.2805(3) 0.0099(7) Uani 1 1 d . . . C7 C 0.2654(4) 0.7912(3) 0.3423(3) 0.0088(7) Uani 1 1 d . . . O8 O 0.3313(3) 0.8814(2) 0.4431(2) 0.0109(5) Uani 1 1 d . . . O9 O 0.1243(3) 0.7375(2) 0.2978(2) 0.0123(5) Uani 1 1 d . . . C10 C 0.2881(4) 0.6482(3) 0.1722(3) 0.0088(7) Uani 1 1 d . . . H10 H 0.1808 0.6147 0.1353 0.011 Uiso 1 1 calc R . . C11 C 0.3743(4) 0.5982(3) 0.1185(3) 0.0083(7) Uani 1 1 d . . . C12 C 0.5315(4) 0.6443(3) 0.1741(3) 0.0092(7) Uani 1 1 d . . . H12 H 0.5895 0.6065 0.1396 0.011 Uiso 1 1 calc R . . O13 O 0.3148(3) 0.5008(2) 0.0107(2) 0.0096(5) Uani 1 1 d . . . C14 C 0.1557(4) 0.4552(3) -0.0531(3) 0.0091(7) Uani 1 1 d . . . H14A H 0.1245 0.5331 -0.0709 0.011 Uiso 1 1 calc R . . H14B H 0.1292 0.3935 -0.1326 0.011 Uiso 1 1 calc R . . O15 O 0.0753(3) 0.3879(2) 0.0154(2) 0.0099(5) Uani 1 1 d . . . C16 C 0.1085(4) 0.2788(3) 0.0520(3) 0.0111(7) Uani 1 1 d . . . C17 C 0.0759(4) 0.2471(3) 0.1543(3) 0.0111(7) Uani 1 1 d . . . H17 H 0.0346 0.3001 0.1942 0.013 Uiso 1 1 calc R . . C18 C 0.1038(4) 0.1380(3) 0.1979(3) 0.0100(7) Uani 1 1 d . . . C19 C 0.0747(4) 0.1033(3) 0.3104(3) 0.0108(7) Uani 1 1 d . . . O20 O 0.0261(3) 0.1774(2) 0.3677(2) 0.0126(5) Uani 1 1 d . . . O21 O 0.1049(3) 0.0024(2) 0.3427(2) 0.0139(5) Uani 1 1 d . . . C22 C 0.1624(4) 0.0592(3) 0.1374(3) 0.0107(7) Uani 1 1 d . . . H22 H 0.1787 -0.0172 0.1650 0.013 Uiso 1 1 calc R . . C23 C 0.1964(4) 0.0933(3) 0.0369(3) 0.0105(7) Uani 1 1 d . . . C24 C 0.2609(4) 0.0122(3) -0.0290(3) 0.0132(7) Uani 1 1 d . . . O25 O 0.2861(3) 0.0387(3) -0.1202(2) 0.0168(6) Uani 1 1 d . . . O26 O 0.2859(3) -0.0871(3) 0.0199(2) 0.0191(6) Uani 1 1 d . . . H26 H 0.3266 -0.1383 -0.0293 0.023 Uiso 1 1 d R . . C27 C 0.1692(4) 0.2025(3) -0.0074(3) 0.0118(7) Uani 1 1 d . . . H27 H 0.1918 0.2243 -0.0770 0.014 Uiso 1 1 d R . . O28 O 1.2957(3) 0.8897(2) 0.6801(2) 0.0133(5) Uani 1 1 d . . . H28A H 1.3058 0.9320 0.7556 0.016 Uiso 1 1 d R . . H28B H 1.3913 0.8819 0.6932 0.016 Uiso 1 1 d R . . O29 O 1.1045(3) 0.6403(2) 0.5116(2) 0.0166(5) Uani 1 1 d . . . H29A H 1.1580 0.6344 0.5883 0.020 Uiso 1 1 d R . . H29B H 1.1116 0.5821 0.4527 0.020 Uiso 1 1 d R . . O30 O 0.5855(3) 0.2223(3) 0.0835(2) 0.0194(6) Uani 1 1 d . . . H30A H 0.6449 0.2986 0.1435 0.029 Uiso 1 1 d R . . H30B H 0.5144 0.2401 0.0229 0.029 Uiso 1 1 d R . . O31 O 0.4528(3) 0.1439(3) 0.3669(2) 0.0192(6) Uani 1 1 d . . . H31A H 0.3588 0.0841 0.3499 0.029 Uiso 1 1 d R . . H31B H 0.5210 0.1354 0.4357 0.029 Uiso 1 1 d R . . O32 O 0.7223(4) 0.4342(3) 0.2860(3) 0.0314(7) Uani 1 1 d . . . H32A H 0.6418 0.4249 0.3099 0.047 Uiso 1 1 d R . . H32B H 0.7811 0.5221 0.3033 0.047 Uiso 1 1 d R . . O33 O 0.2305(5) 0.4640(4) 0.4154(3) 0.0500(10) Uani 1 1 d . . . H33A H 0.1719 0.3730 0.4130 0.075 Uiso 1 1 d R . . H33B H 0.3024 0.4924 0.4997 0.075 Uiso 1 1 d R . . O34 O 0.4866(4) 0.4059(3) 0.3667(4) 0.0479(10) Uani 1 1 d . . . H34A H 0.4465 0.4426 0.4167 0.072 Uiso 1 1 d R . . H34B H 0.4469 0.3126 0.3532 0.072 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm 0.00773(10) 0.00871(10) 0.00699(10) 0.00047(6) 0.00354(7) 0.00394(7) O1 0.0087(12) 0.0120(12) 0.0148(13) -0.0015(10) 0.0036(10) 0.0052(10) O2 0.0080(12) 0.0079(12) 0.0112(12) -0.0025(9) 0.0016(10) 0.0010(9) C3 0.0118(17) 0.0121(17) 0.0072(16) 0.0025(13) 0.0056(13) 0.0043(13) C4 0.0118(17) 0.0089(16) 0.0084(16) 0.0027(13) 0.0048(14) 0.0041(13) C5 0.0123(17) 0.0099(16) 0.0055(16) 0.0022(13) 0.0026(13) 0.0043(13) C6 0.0118(17) 0.0107(17) 0.0106(17) 0.0040(13) 0.0062(14) 0.0059(13) C7 0.0100(17) 0.0102(16) 0.0092(16) 0.0042(13) 0.0046(13) 0.0059(13) O8 0.0077(12) 0.0141(12) 0.0102(12) -0.0030(10) 0.0048(10) 0.0036(10) O9 0.0058(12) 0.0161(13) 0.0129(12) -0.0021(10) 0.0027(10) 0.0036(10) C10 0.0066(16) 0.0095(16) 0.0111(17) 0.0014(13) 0.0048(13) 0.0026(13) C11 0.0100(16) 0.0054(15) 0.0078(16) 0.0005(12) 0.0029(13) 0.0009(13) C12 0.0095(16) 0.0105(16) 0.0095(16) 0.0024(13) 0.0048(13) 0.0049(13) O13 0.0078(11) 0.0106(12) 0.0085(12) -0.0026(9) 0.0027(9) 0.0024(9) C14 0.0071(16) 0.0109(16) 0.0071(16) 0.0022(13) 0.0016(13) 0.0012(13) O15 0.0099(12) 0.0104(12) 0.0117(12) 0.0038(9) 0.0057(10) 0.0044(10) C16 0.0094(16) 0.0107(17) 0.0121(17) 0.0013(13) 0.0033(14) 0.0030(13) C17 0.0085(16) 0.0132(17) 0.0127(17) 0.0014(14) 0.0059(14) 0.0038(13) C18 0.0092(16) 0.0118(17) 0.0081(16) 0.0006(13) 0.0030(13) 0.0032(13) C19 0.0101(17) 0.0110(17) 0.0107(17) 0.0010(13) 0.0034(14) 0.0039(13) O20 0.0170(13) 0.0159(13) 0.0127(13) 0.0054(10) 0.0110(10) 0.0099(10) O21 0.0202(14) 0.0129(13) 0.0169(13) 0.0047(10) 0.0116(11) 0.0117(11) C22 0.0101(17) 0.0111(17) 0.0109(17) 0.0044(13) 0.0038(13) 0.0029(13) C23 0.0097(16) 0.0119(17) 0.0077(16) -0.0007(13) 0.0026(13) 0.0026(13) C24 0.0148(18) 0.0111(17) 0.0129(18) 0.0010(14) 0.0061(15) 0.0029(14) O25 0.0241(14) 0.0195(14) 0.0140(13) 0.0054(11) 0.0124(11) 0.0113(11) O26 0.0316(16) 0.0173(14) 0.0196(14) 0.0085(11) 0.0158(12) 0.0159(12) C27 0.0129(17) 0.0144(17) 0.0088(17) 0.0028(14) 0.0059(14) 0.0036(14) O28 0.0136(13) 0.0181(13) 0.0076(12) 0.0002(10) 0.0016(10) 0.0079(10) O29 0.0209(14) 0.0117(13) 0.0161(13) 0.0003(10) 0.0046(11) 0.0075(11) O30 0.0222(14) 0.0193(14) 0.0188(14) 0.0046(11) 0.0067(12) 0.0111(11) O31 0.0136(13) 0.0253(15) 0.0171(14) 0.0049(11) 0.0039(11) 0.0064(11) O32 0.0398(19) 0.0118(14) 0.0318(17) 0.0038(12) 0.0009(14) 0.0071(13) O33 0.081(3) 0.0279(19) 0.042(2) 0.0042(16) 0.031(2) 0.0104(19) O34 0.050(2) 0.0260(18) 0.054(2) 0.0111(16) 0.0089(19) 0.0033(16) _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 Sm O21 2.356(2) 1_665 ? Sm O2 2.405(2) 2_776 ? Sm O29 2.440(2) . ? Sm O20 2.449(2) 2_666 ? Sm O28 2.457(2) . ? Sm O8 2.469(2) 1_655 ? Sm O1 2.482(2) . ? Sm O9 2.533(2) 1_655 ? Sm O2 2.631(2) . ? Sm C7 2.869(3) 1_655 ? Sm C3 2.942(3) . ? Sm Sm 4.0205(3) 2_776 ? O1 C3 1.268(4) . ? O2 C3 1.269(4) . ? O2 Sm 2.405(2) 2_776 ? C3 C4 1.490(5) . ? C4 C5 1.390(5) . ? C4 C12 1.401(5) . ? C5 C6 1.389(5) . ? C5 H5 0.9500 . ? C6 C10 1.390(5) . ? C6 C7 1.502(4) . ? C7 O9 1.252(4) . ? C7 O8 1.281(4) . ? C7 Sm 2.869(3) 1_455 ? O8 Sm 2.469(2) 1_455 ? O9 Sm 2.533(2) 1_455 ? C10 C11 1.394(5) . ? C10 H10 0.9500 . ? C11 O13 1.380(4) . ? C11 C12 1.393(5) . ? C12 H12 0.9500 . ? O13 C14 1.420(4) . ? C14 O15 1.417(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O15 C16 1.378(4) . ? C16 C27 1.390(5) . ? C16 C17 1.393(5) . ? C17 C18 1.390(5) . ? C17 H17 0.9500 . ? C18 C22 1.398(5) . ? C18 C19 1.504(5) . ? C19 O21 1.268(4) . ? C19 O20 1.271(4) . ? O20 Sm 2.449(2) 2_666 ? O21 Sm 2.356(2) 1_445 ? C22 C23 1.387(5) . ? C22 H22 0.9500 . ? C23 C27 1.392(5) . ? C23 C24 1.495(5) . ? C24 O25 1.221(4) . ? C24 O26 1.312(4) . ? O26 H26 0.9990 . ? C27 H27 0.9500 . ? O28 H28A 0.9092 . ? O28 H28B 0.9413 . ? O29 H29A 0.9108 . ? O29 H29B 0.9097 . ? O30 H30A 0.9136 . ? O30 H30B 0.9134 . ? O31 H31A 0.9092 . ? O31 H31B 0.9099 . ? O32 H32A 0.9094 . ? O32 H32B 0.9093 . ? O33 H33A 0.9695 . ? O33 H33B 0.9715 . ? O34 H34A 0.9173 . ? O34 H34B 0.9325 . ? 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 O21 Sm O2 71.03(8) 1_665 2_776 ? O21 Sm O29 142.76(8) 1_665 . ? O2 Sm O29 143.23(8) 2_776 . ? O21 Sm O20 135.76(8) 1_665 2_666 ? O2 Sm O20 78.88(8) 2_776 2_666 ? O29 Sm O20 77.93(8) . 2_666 ? O21 Sm O28 126.47(9) 1_665 . ? O2 Sm O28 75.03(8) 2_776 . ? O29 Sm O28 71.05(8) . . ? O20 Sm O28 72.79(8) 2_666 . ? O21 Sm O8 74.15(8) 1_665 1_655 ? O2 Sm O8 100.01(8) 2_776 1_655 ? O29 Sm O8 83.11(8) . 1_655 ? O20 Sm O8 144.25(8) 2_666 1_655 ? O28 Sm O8 72.47(8) . 1_655 ? O21 Sm O1 87.30(9) 1_665 . ? O2 Sm O1 124.84(8) 2_776 . ? O29 Sm O1 80.40(8) . . ? O20 Sm O1 84.01(8) 2_666 . ? O28 Sm O1 146.18(9) . . ? O8 Sm O1 122.42(8) 1_655 . ? O21 Sm O9 72.35(8) 1_665 1_655 ? O2 Sm O9 139.11(8) 2_776 1_655 ? O29 Sm O9 70.42(8) . 1_655 ? O20 Sm O9 141.75(8) 2_666 1_655 ? O28 Sm O9 114.57(8) . 1_655 ? O8 Sm O9 52.24(7) 1_655 1_655 ? O1 Sm O9 70.26(8) . 1_655 ? O21 Sm O2 70.78(8) 1_665 . ? O2 Sm O2 74.15(8) 2_776 . ? O29 Sm O2 122.85(8) . . ? O20 Sm O2 70.26(8) 2_666 . ? O28 Sm O2 135.41(8) . . ? O8 Sm O2 144.43(8) 1_655 . ? O1 Sm O2 50.74(7) . . ? O9 Sm O2 109.86(7) 1_655 . ? O21 Sm C7 72.42(9) 1_665 1_655 ? O2 Sm C7 122.13(9) 2_776 1_655 ? O29 Sm C7 74.13(9) . 1_655 ? O20 Sm C7 151.61(9) 2_666 1_655 ? O28 Sm C7 93.24(9) . 1_655 ? O8 Sm C7 26.44(9) 1_655 1_655 ? O1 Sm C7 96.10(9) . 1_655 ? O9 Sm C7 25.84(9) 1_655 1_655 ? O2 Sm C7 130.55(8) . 1_655 ? O21 Sm C3 79.27(9) 1_665 . ? O2 Sm C3 99.68(8) 2_776 . ? O29 Sm C3 101.17(9) . . ? O20 Sm C3 74.61(9) 2_666 . ? O28 Sm C3 147.39(9) . . ? O8 Sm C3 139.39(8) 1_655 . ? O1 Sm C3 25.26(8) . . ? O9 Sm C3 90.76(8) 1_655 . ? O2 Sm C3 25.54(8) . . ? C7 Sm C3 115.59(9) 1_655 . ? O21 Sm Sm 65.80(6) 1_665 2_776 ? O2 Sm Sm 39.01(6) 2_776 2_776 ? O29 Sm Sm 146.52(6) . 2_776 ? O20 Sm Sm 70.34(6) 2_666 2_776 ? O28 Sm Sm 108.14(6) . 2_776 ? O8 Sm Sm 129.51(6) 1_655 2_776 ? O1 Sm Sm 85.85(5) . 2_776 ? O9 Sm Sm 132.42(6) 1_655 2_776 ? O2 Sm Sm 35.14(5) . 2_776 ? C7 Sm Sm 138.04(7) 1_655 2_776 ? C3 Sm Sm 60.67(6) . 2_776 ? C3 O1 Sm 98.1(2) . . ? C3 O2 Sm 163.1(2) . 2_776 ? C3 O2 Sm 91.07(19) . . ? Sm O2 Sm 105.85(8) 2_776 . ? O2 C3 O1 119.8(3) . . ? O2 C3 C4 120.3(3) . . ? O1 C3 C4 119.8(3) . . ? O2 C3 Sm 63.39(17) . . ? O1 C3 Sm 56.64(17) . . ? C4 C3 Sm 172.4(2) . . ? C5 C4 C12 120.1(3) . . ? C5 C4 C3 120.1(3) . . ? C12 C4 C3 119.7(3) . . ? C6 C5 C4 119.6(3) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C10 120.9(3) . . ? C5 C6 C7 121.0(3) . . ? C10 C6 C7 118.1(3) . . ? O9 C7 O8 120.8(3) . . ? O9 C7 C6 120.4(3) . . ? O8 C7 C6 118.7(3) . . ? O9 C7 Sm 61.90(17) . 1_455 ? O8 C7 Sm 59.07(16) . 1_455 ? C6 C7 Sm 173.7(2) . 1_455 ? C7 O8 Sm 94.49(19) . 1_455 ? C7 O9 Sm 92.25(19) . 1_455 ? C6 C10 C11 119.2(3) . . ? C6 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? O13 C11 C12 115.0(3) . . ? O13 C11 C10 124.4(3) . . ? C12 C11 C10 120.6(3) . . ? C11 C12 C4 119.4(3) . . ? C11 C12 H12 120.3 . . ? C4 C12 H12 120.3 . . ? C11 O13 C14 117.3(2) . . ? O15 C14 O13 112.1(3) . . ? O15 C14 H14A 109.2 . . ? O13 C14 H14A 109.2 . . ? O15 C14 H14B 109.2 . . ? O13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 O15 C14 117.1(3) . . ? O15 C16 C27 123.8(3) . . ? O15 C16 C17 115.5(3) . . ? C27 C16 C17 120.7(3) . . ? C18 C17 C16 120.0(3) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C22 119.7(3) . . ? C17 C18 C19 121.6(3) . . ? C22 C18 C19 118.8(3) . . ? O21 C19 O20 124.7(3) . . ? O21 C19 C18 116.5(3) . . ? O20 C19 C18 118.8(3) . . ? C19 O20 Sm 131.7(2) . 2_666 ? C19 O21 Sm 145.3(2) . 1_445 ? C23 C22 C18 119.6(3) . . ? C23 C22 H22 120.2 . . ? C18 C22 H22 120.2 . . ? C22 C23 C27 121.2(3) . . ? C22 C23 C24 121.0(3) . . ? C27 C23 C24 117.8(3) . . ? O25 C24 O26 124.6(3) . . ? O25 C24 C23 121.3(3) . . ? O26 C24 C23 114.0(3) . . ? C24 O26 H26 110.0 . . ? C23 C27 C16 118.7(3) . . ? C23 C27 H27 120.6 . . ? C16 C27 H27 120.7 . . ? Sm O28 H28A 127.5 . . ? Sm O28 H28B 127.2 . . ? H28A O28 H28B 103.4 . . ? Sm O29 H29A 117.9 . . ? Sm O29 H29B 120.8 . . ? H29A O29 H29B 110.8 . . ? H30A O30 H30B 110.3 . . ? H31A O31 H31B 111.0 . . ? H32A O32 H32B 111.1 . . ? H33A O33 H33B 101.3 . . ? H34A O34 H34B 108.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O26 H26 O30 1.00 1.62 2.612(4) 169 2_655 O28 H28A O25 0.91 1.84 2.723(3) 163 1_666 O28 H28B O31 0.94 1.96 2.828(4) 152 2_766 O29 H29A O32 0.91 1.94 2.812(4) 158 2_766 O29 H29B O33 0.91 2.06 2.855(4) 146 1_655 O30 H30A O32 0.91 1.86 2.751(4) 163 . O30 H30B O25 0.91 2.55 3.076(4) 117 . O31 H31A O21 0.91 2.38 3.246(4) 158 . O31 H31B O8 0.91 1.76 2.667(4) 172 2_666 O32 H32A O34 0.91 1.83 2.740(5) 177 . O32 H32B O1 0.91 1.94 2.819(4) 161 . O33 H33A O20 0.97 2.06 3.014(4) 168 . O33 H33B O34 0.97 2.06 2.960(6) 153 2_666 O34 H34A O33 0.92 2.21 2.985(6) 141 . O34 H34B O31 0.93 1.84 2.720(4) 156 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.168 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.128 #========================END================================ data_6 _database_code_depnum_ccdc_archive 'CCDC 772536' #TrackingRef '- ka3-26-Ln.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H13 Dy O12, 3(H2 O)' _chemical_formula_sum 'C17 H19 Dy O15' _chemical_formula_weight 625.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.8023(6) _cell_length_b 20.1819(6) _cell_length_c 7.1981(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.2972(14) _cell_angle_gamma 90.00 _cell_volume 2092.70(12) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4473 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 27.86 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.986 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 3.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5289 _exptl_absorpt_correction_T_max 0.8386 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f & \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17040 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.86 _reflns_number_total 4962 _reflns_number_gt 4170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+1.8780P] 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 4962 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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 Dy Dy 0.864478(18) 0.141934(12) 0.19290(4) 0.00971(9) Uani 1 1 d . . . O1 O 0.7097(3) 0.12573(19) 0.2515(6) 0.0162(9) Uani 1 1 d . . . O2 O 0.7472(3) 0.22684(19) 0.1830(6) 0.0129(8) Uani 1 1 d . . . C3 C 0.6892(4) 0.1870(3) 0.2244(8) 0.0139(12) Uani 1 1 d . . . C4 C 0.5964(4) 0.2117(3) 0.2425(8) 0.0142(12) Uani 1 1 d . . . C5 C 0.5802(4) 0.2797(3) 0.2385(8) 0.0141(12) Uani 1 1 d . . . H5 H 0.6270 0.3097 0.2208 0.017 Uiso 1 1 calc R . . C6 C 0.4956(4) 0.3034(3) 0.2606(8) 0.0148(12) Uani 1 1 d . . . C7 C 0.4815(5) 0.3765(3) 0.2671(9) 0.0214(14) Uani 1 1 d . . . O8 O 0.4009(3) 0.3932(2) 0.3000(8) 0.0302(12) Uani 1 1 d . . . H8 H 0.3999 0.4342 0.3196 0.045 Uiso 1 1 calc R . . O9 O 0.5403(3) 0.4170(2) 0.2489(7) 0.0280(11) Uani 1 1 d . . . C10 C 0.4251(4) 0.2602(3) 0.2802(9) 0.0180(13) Uani 1 1 d . . . H10 H 0.3671 0.2769 0.2949 0.022 Uiso 1 1 calc R . . C11 C 0.4406(4) 0.1924(3) 0.2779(9) 0.0179(13) Uani 1 1 d . . . C12 C 0.5263(4) 0.1680(3) 0.2618(9) 0.0154(12) Uani 1 1 d . . . H12 H 0.5370 0.1216 0.2639 0.018 Uiso 1 1 calc R . . O13 O 0.3741(3) 0.1457(2) 0.2922(7) 0.0226(10) Uani 1 1 d . . . C14 C 0.2874(5) 0.1689(4) 0.3177(10) 0.0262(15) Uani 1 1 d . . . H14A H 0.2981 0.1980 0.4301 0.031 Uiso 1 1 calc R . . H14B H 0.2498 0.1308 0.3395 0.031 Uiso 1 1 calc R . . O15 O 0.2371(3) 0.2053(2) 0.1541(6) 0.0187(9) Uani 1 1 d . . . C16 C 0.1830(4) 0.1688(3) 0.0056(9) 0.0158(12) Uani 1 1 d . . . C17 C 0.1978(4) 0.1026(3) -0.0242(8) 0.0141(12) Uani 1 1 d . . . H17 H 0.2483 0.0798 0.0556 0.017 Uiso 1 1 calc R . . C18 C 0.1373(4) 0.0693(3) -0.1742(8) 0.0135(11) Uani 1 1 d . . . C19 C 0.1473(4) -0.0037(3) -0.1901(8) 0.0139(12) Uani 1 1 d . . . O20 O 0.1152(3) -0.0334(2) -0.3473(5) 0.0137(9) Uani 1 1 d . . . O21 O 0.1842(3) -0.0364(2) -0.0416(6) 0.0180(9) Uani 1 1 d . . . C22 C 0.0634(4) 0.1028(3) -0.2922(8) 0.0149(12) Uani 1 1 d . . . H22 H 0.0232 0.0802 -0.3943 0.018 Uiso 1 1 calc R . . C23 C 0.0488(4) 0.1697(3) -0.2598(8) 0.0119(11) Uani 1 1 d . . . C24 C -0.0352(4) 0.2047(3) -0.3729(8) 0.0123(11) Uani 1 1 d . . . O25 O -0.0486(3) 0.2638(2) -0.3325(6) 0.0165(9) Uani 1 1 d . . . O26 O -0.0895(3) 0.1720(2) -0.5012(6) 0.0173(9) Uani 1 1 d . . . C27 C 0.1099(4) 0.2031(3) -0.1118(9) 0.0158(12) Uani 1 1 d . . . H27 H 0.1015 0.2490 -0.0917 0.019 Uiso 1 1 calc R . . O28 O 0.8164(3) 0.1584(2) -0.1328(6) 0.0178(9) Uani 1 1 d . . . H28A H 0.7910 0.1320 -0.2260 0.027 Uiso 1 1 d R . . H28B H 0.8037 0.2065 -0.1910 0.027 Uiso 1 1 d R . . O29 O 1.0075(4) 0.1047(3) 0.1516(8) 0.0394(14) Uani 1 1 d . . . H29A H 1.0482 0.0761 0.2041 0.059 Uiso 1 1 d R . . H29B H 0.9548 0.0857 0.1218 0.059 Uiso 1 1 d R . . O30 O 0.3964(3) -0.0140(2) 0.9034(8) 0.0320(12) Uani 1 1 d . . . H30A H 0.3622 -0.0497 0.8526 0.048 Uiso 1 1 d R . . H30B H 0.4164 -0.0359 1.0131 0.048 Uiso 1 1 d R . . O31 O 0.2880(3) -0.0728(2) 1.3786(6) 0.0245(10) Uani 1 1 d . . . H31A H 0.2880 -0.0888 1.4881 0.037 Uiso 1 1 d R . . H31B H 0.3377 -0.0758 1.3392 0.037 Uiso 1 1 d R . . O32 O 0.1279(5) 0.0192(4) 1.3052(9) 0.074(3) Uani 1 1 d . . . H32A H 0.1441 0.0028 1.2050 0.111 Uiso 1 1 d R . . H32B H 0.1252 0.0031 1.4164 0.111 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy 0.01156(14) 0.00530(13) 0.01230(14) 0.00068(11) 0.00280(9) 0.00066(11) O1 0.016(2) 0.006(2) 0.026(2) 0.0014(16) 0.0057(18) 0.0011(16) O2 0.0115(19) 0.008(2) 0.020(2) -0.0013(16) 0.0054(17) 0.0004(16) C3 0.019(3) 0.010(3) 0.012(3) -0.003(2) 0.003(2) 0.000(2) C4 0.016(3) 0.015(3) 0.011(3) -0.001(2) 0.002(2) 0.000(2) C5 0.017(3) 0.015(3) 0.011(3) -0.002(2) 0.004(2) 0.002(2) C6 0.014(3) 0.012(3) 0.017(3) -0.005(2) 0.001(2) 0.001(2) C7 0.021(3) 0.014(3) 0.027(3) -0.004(2) 0.001(3) 0.004(3) O8 0.020(2) 0.015(2) 0.059(3) -0.006(2) 0.016(2) 0.002(2) O9 0.023(2) 0.016(2) 0.048(3) -0.006(2) 0.013(2) -0.001(2) C10 0.016(3) 0.020(3) 0.019(3) -0.006(2) 0.004(2) 0.001(3) C11 0.013(3) 0.022(3) 0.018(3) -0.004(2) 0.003(2) -0.002(3) C12 0.015(3) 0.009(3) 0.022(3) 0.001(2) 0.005(3) 0.003(2) O13 0.017(2) 0.019(2) 0.034(3) 0.000(2) 0.0088(19) 0.0009(19) C14 0.016(3) 0.038(4) 0.026(4) 0.001(3) 0.006(3) 0.005(3) O15 0.015(2) 0.013(2) 0.024(2) -0.0051(17) -0.0029(18) -0.0006(17) C16 0.014(3) 0.015(3) 0.019(3) -0.004(2) 0.004(2) -0.003(2) C17 0.009(3) 0.013(3) 0.020(3) 0.000(2) 0.003(2) -0.002(2) C18 0.018(3) 0.007(3) 0.017(3) 0.000(2) 0.006(2) 0.002(2) C19 0.011(3) 0.010(3) 0.021(3) 0.002(2) 0.004(2) -0.002(2) O20 0.018(2) 0.013(2) 0.0107(19) 0.0016(15) 0.0045(17) 0.0045(17) O21 0.026(2) 0.008(2) 0.016(2) 0.0021(16) -0.0030(18) 0.0001(18) C22 0.016(3) 0.012(3) 0.017(3) 0.000(2) 0.006(2) 0.002(2) C23 0.015(3) 0.007(3) 0.015(3) 0.002(2) 0.007(2) -0.003(2) C24 0.019(3) 0.008(3) 0.013(3) 0.001(2) 0.011(2) 0.000(2) O25 0.018(2) 0.011(2) 0.022(2) 0.0000(17) 0.0067(18) 0.0029(17) O26 0.024(2) 0.014(2) 0.013(2) 0.0004(17) 0.0037(18) 0.0019(18) C27 0.020(3) 0.005(3) 0.026(3) 0.001(2) 0.014(3) -0.002(2) O28 0.030(2) 0.010(2) 0.011(2) 0.0008(15) 0.0001(18) 0.0011(18) O29 0.024(3) 0.032(3) 0.071(4) 0.031(3) 0.030(3) 0.016(2) O30 0.030(3) 0.022(3) 0.042(3) 0.003(2) 0.003(2) -0.005(2) O31 0.024(2) 0.031(3) 0.018(2) 0.006(2) 0.0048(19) 0.000(2) O32 0.090(5) 0.098(6) 0.053(4) 0.057(4) 0.055(4) 0.079(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy O26 2.234(4) 1_656 ? Dy O28 2.312(4) . ? Dy O25 2.327(4) 4_666 ? Dy O29 2.330(5) . ? Dy O21 2.425(4) 3_655 ? Dy O2 2.429(4) . ? Dy O20 2.443(4) 3_655 ? Dy O1 2.445(4) . ? Dy C19 2.795(6) 3_655 ? Dy C3 2.808(6) . ? Dy H29B 1.9117 . ? O1 C3 1.278(7) . ? O2 C3 1.261(7) . ? C3 C4 1.494(8) . ? C4 C5 1.391(8) . ? C4 C12 1.393(9) . ? C5 C6 1.383(8) . ? C5 H5 0.9500 . ? C6 C10 1.392(9) . ? C6 C7 1.493(8) . ? C7 O9 1.222(8) . ? C7 O8 1.313(8) . ? O8 H8 0.8400 . ? C10 C11 1.388(9) . ? C10 H10 0.9500 . ? C11 O13 1.384(8) . ? C11 C12 1.389(9) . ? C12 H12 0.9500 . ? O13 C14 1.418(8) . ? C14 O15 1.441(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O15 C16 1.391(7) . ? C16 C17 1.379(8) . ? C16 C27 1.395(9) . ? C17 C18 1.405(8) . ? C17 H17 0.9500 . ? C18 C22 1.396(8) . ? C18 C19 1.487(8) . ? C19 O21 1.268(7) . ? C19 O20 1.272(7) . ? C19 Dy 2.795(6) 3_655 ? O20 Dy 2.443(4) 3_655 ? O21 Dy 2.425(4) 3_655 ? C22 C23 1.394(8) . ? C22 H22 0.9500 . ? C23 C27 1.402(8) . ? C23 C24 1.497(8) . ? C24 O25 1.255(7) . ? C24 O26 1.262(7) . ? O25 Dy 2.327(4) 4_465 ? O26 Dy 2.234(4) 1_454 ? C27 H27 0.9500 . ? O28 H28A 0.8710 . ? O28 H28B 1.0563 . ? O29 H29A 0.8560 . ? O29 H29B 0.8515 . ? O30 H30A 0.9076 . ? O30 H30B 0.8934 . ? O31 H31A 0.8514 . ? O31 H31B 0.8491 . ? O32 H32A 0.8753 . ? O32 H32B 0.8734 . ? 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 O26 Dy O28 155.97(15) 1_656 . ? O26 Dy O25 78.85(15) 1_656 4_666 ? O28 Dy O25 81.35(15) . 4_666 ? O26 Dy O29 97.67(19) 1_656 . ? O28 Dy O29 89.65(18) . . ? O25 Dy O29 73.65(17) 4_666 . ? O26 Dy O21 132.30(15) 1_656 3_655 ? O28 Dy O21 71.37(14) . 3_655 ? O25 Dy O21 142.66(15) 4_666 3_655 ? O29 Dy O21 81.02(19) . 3_655 ? O26 Dy O2 83.76(14) 1_656 . ? O28 Dy O2 79.47(14) . . ? O25 Dy O2 79.95(14) 4_666 . ? O29 Dy O2 152.69(16) . . ? O21 Dy O2 118.03(14) 3_655 . ? O26 Dy O20 79.47(14) 1_656 3_655 ? O28 Dy O20 124.56(14) . 3_655 ? O25 Dy O20 139.12(14) 4_666 3_655 ? O29 Dy O20 75.42(15) . 3_655 ? O21 Dy O20 53.83(13) 3_655 3_655 ? O2 Dy O20 131.17(14) . 3_655 ? O26 Dy O1 87.23(15) 1_656 . ? O28 Dy O1 96.43(15) . . ? O25 Dy O1 132.84(14) 4_666 . ? O29 Dy O1 153.39(16) . . ? O21 Dy O1 76.51(15) 3_655 . ? O2 Dy O1 53.68(13) . . ? O20 Dy O1 79.85(13) 3_655 . ? O26 Dy C19 106.41(16) 1_656 3_655 ? O28 Dy C19 97.60(16) . 3_655 ? O25 Dy C19 148.22(16) 4_666 3_655 ? O29 Dy C19 74.57(18) . 3_655 ? O21 Dy C19 26.94(15) 3_655 3_655 ? O2 Dy C19 131.37(15) . 3_655 ? O20 Dy C19 27.05(15) 3_655 3_655 ? O1 Dy C19 78.94(15) . 3_655 ? O26 Dy C3 84.86(16) 1_656 . ? O28 Dy C3 87.74(16) . . ? O25 Dy C3 106.23(16) 4_666 . ? O29 Dy C3 177.37(18) . . ? O21 Dy C3 97.83(16) 3_655 . ? O2 Dy C3 26.63(15) . . ? O20 Dy C3 105.85(15) 3_655 . ? O1 Dy C3 27.04(15) . . ? C19 Dy C3 105.46(17) 3_655 . ? O26 Dy H29B 110.6 1_656 . ? O28 Dy H29B 83.4 . . ? O25 Dy H29B 91.8 4_666 . ? O29 Dy H29B 20.2 . . ? O21 Dy H29B 60.8 3_655 . ? O2 Dy H29B 161.9 . . ? O20 Dy H29B 64.5 3_655 . ? O1 Dy H29B 135.0 . . ? C19 Dy H29B 56.7 3_655 . ? C3 Dy H29B 158.5 . . ? C3 O1 Dy 92.5(4) . . ? C3 O2 Dy 93.7(3) . . ? O2 C3 O1 120.1(5) . . ? O2 C3 C4 119.8(5) . . ? O1 C3 C4 120.1(5) . . ? O2 C3 Dy 59.7(3) . . ? O1 C3 Dy 60.4(3) . . ? C4 C3 Dy 179.3(4) . . ? C5 C4 C12 119.8(6) . . ? C5 C4 C3 119.0(5) . . ? C12 C4 C3 121.2(5) . . ? C6 C5 C4 119.6(6) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C10 121.0(6) . . ? C5 C6 C7 118.8(6) . . ? C10 C6 C7 120.1(6) . . ? O9 C7 O8 123.2(6) . . ? O9 C7 C6 123.3(6) . . ? O8 C7 C6 113.5(6) . . ? C7 O8 H8 109.5 . . ? C11 C10 C6 119.0(6) . . ? C11 C10 H10 120.5 . . ? C6 C10 H10 120.5 . . ? O13 C11 C10 123.2(6) . . ? O13 C11 C12 116.3(6) . . ? C10 C11 C12 120.5(6) . . ? C11 C12 C4 120.0(6) . . ? C11 C12 H12 120.0 . . ? C4 C12 H12 120.0 . . ? C11 O13 C14 117.7(5) . . ? O13 C14 O15 112.1(5) . . ? O13 C14 H14A 109.0 . . ? O15 C14 H14A 109.0 . . ? O13 C14 H14B 109.0 . . ? O15 C14 H14B 109.0 . . ? H14A C14 H14B 109.0 . . ? C16 O15 C14 117.1(5) . . ? C17 C16 O15 123.3(5) . . ? C17 C16 C27 121.1(5) . . ? O15 C16 C27 115.6(5) . . ? C16 C17 C18 119.1(5) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C22 C18 C17 120.5(5) . . ? C22 C18 C19 120.8(5) . . ? C17 C18 C19 118.4(5) . . ? O21 C19 O20 120.3(5) . . ? O21 C19 C18 118.8(5) . . ? O20 C19 C18 120.8(5) . . ? O21 C19 Dy 60.1(3) . 3_655 ? O20 C19 Dy 60.9(3) . 3_655 ? C18 C19 Dy 169.1(4) . 3_655 ? C19 O20 Dy 92.1(3) . 3_655 ? C19 O21 Dy 93.0(3) . 3_655 ? C23 C22 C18 119.9(5) . . ? C23 C22 H22 120.1 . . ? C18 C22 H22 120.1 . . ? C22 C23 C27 119.7(5) . . ? C22 C23 C24 120.5(5) . . ? C27 C23 C24 119.7(5) . . ? O25 C24 O26 124.0(5) . . ? O25 C24 C23 118.6(5) . . ? O26 C24 C23 117.4(5) . . ? C24 O25 Dy 156.2(4) . 4_465 ? C24 O26 Dy 149.5(4) . 1_454 ? C16 C27 C23 119.7(5) . . ? C16 C27 H27 120.1 . . ? C23 C27 H27 120.1 . . ? Dy O28 H28A 132.1 . . ? Dy O28 H28B 121.3 . . ? H28A O28 H28B 104.6 . . ? Dy O29 H29A 136.7 . . ? Dy O29 H29B 51.0 . . ? H29A O29 H29B 108.6 . . ? H30A O30 H30B 90.3 . . ? H31A O31 H31B 117.9 . . ? H32A O32 H32B 133.9 . . ? 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 O8 H8 O30 0.84 1.73 2.556(7) 169 4_565 O28 H28A O31 0.87 1.85 2.691(6) 163 3_656 O28 H28B O2 1.06 1.73 2.747(6) 161 4_565 O29 H29A O32 0.86 1.69 2.543(7) 179 1_654 O29 H29B O21 0.85 2.24 3.090(7) 179 3_655 O30 H30A O1 0.91 1.92 2.826(6) 179 3_656 O30 H30B O9 0.89 1.93 2.828(7) 180 2_646 O31 H31A O1 0.85 2.01 2.861(6) 179 3_657 O31 H31B O9 0.85 2.05 2.901(7) 178 2_646 O32 H32A O21 0.88 2.15 3.023(8) 179 1_556 O32 H32B O20 0.87 1.89 2.764(7) 178 1_557 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.456 _refine_diff_density_min -1.293 _refine_diff_density_rms 0.194 #===============END=============================== data_7 _database_code_depnum_ccdc_archive 'CCDC 772537' #TrackingRef '- ka3-26-Ln.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H13 Eu O12, 3(H2 O)' _chemical_formula_sum 'C17 H19 Eu O15' _chemical_formula_weight 615.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.8422(3) _cell_length_b 20.2605(3) _cell_length_c 7.22730(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.6300(5) _cell_angle_gamma 90.00 _cell_volume 2112.12(6) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4826 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 27.87 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 3.048 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5808 _exptl_absorpt_correction_T_max 0.8625 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18767 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.87 _reflns_number_total 4992 _reflns_number_gt 4076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The water solvent species are partly disordered. ; _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^)+(0.0831P)^2^+2.4905P] 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 4992 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu Eu 0.864849(12) 0.141278(8) 0.19196(2) 0.01043(8) Uani 1 1 d . . . O1 O 0.70856(19) 0.12725(13) 0.2539(4) 0.0159(5) Uani 1 1 d . . . O2 O 0.74590(18) 0.22706(12) 0.1787(3) 0.0143(5) Uani 1 1 d . . . C3 C 0.6879(2) 0.18816(17) 0.2233(5) 0.0123(7) Uani 1 1 d . . . C4 C 0.5958(3) 0.21324(18) 0.2400(5) 0.0142(7) Uani 1 1 d . . . C5 C 0.5803(3) 0.28117(18) 0.2359(5) 0.0142(7) Uani 1 1 d . . . H5 H 0.6271 0.3109 0.2181 0.017 Uiso 1 1 calc R . . C6 C 0.4948(3) 0.30501(19) 0.2584(5) 0.0155(7) Uani 1 1 d . . . C7 C 0.4819(3) 0.3776(2) 0.2651(5) 0.0181(8) Uani 1 1 d . . . O8 O 0.4016(2) 0.39465(15) 0.2972(5) 0.0272(7) Uani 1 1 d . . . H8 H 0.4007 0.4356 0.3143 0.041 Uiso 1 1 calc R . . O9 O 0.5414(2) 0.41759(14) 0.2479(4) 0.0245(6) Uani 1 1 d . . . C10 C 0.4251(3) 0.26199(19) 0.2775(5) 0.0154(7) Uani 1 1 d . . . H10 H 0.3673 0.2786 0.2916 0.018 Uiso 1 1 calc R . . C11 C 0.4404(3) 0.19408(19) 0.2760(5) 0.0158(7) Uani 1 1 d . . . C12 C 0.5257(3) 0.16962(19) 0.2601(5) 0.0161(7) Uani 1 1 d . . . H12 H 0.5364 0.1234 0.2629 0.019 Uiso 1 1 calc R . . O13 O 0.37549(19) 0.14758(12) 0.2940(4) 0.0174(6) Uani 1 1 d . . . C14 C 0.2886(3) 0.1711(2) 0.3195(5) 0.0191(8) Uani 1 1 d . . . H14A H 0.2996 0.2005 0.4320 0.023 Uiso 1 1 calc R . . H14B H 0.2513 0.1331 0.3449 0.023 Uiso 1 1 calc R . . O15 O 0.23791(18) 0.20595(13) 0.1586(4) 0.0174(6) Uani 1 1 d . . . C16 C 0.1853(3) 0.16997(19) 0.0092(5) 0.0152(7) Uani 1 1 d . . . C17 C 0.2006(3) 0.10375(18) -0.0211(5) 0.0136(7) Uani 1 1 d . . . H17 H 0.2507 0.0809 0.0596 0.016 Uiso 1 1 calc R . . C18 C 0.1410(2) 0.07112(19) -0.1726(5) 0.0131(7) Uani 1 1 d . . . C19 C 0.1506(3) -0.00243(18) -0.1907(5) 0.0129(7) Uani 1 1 d . . . O20 O 0.11676(19) -0.03153(13) -0.3471(4) 0.0165(6) Uani 1 1 d . . . O21 O 0.1905(2) -0.03476(13) -0.0445(4) 0.0203(6) Uani 1 1 d . . . C22 C 0.0678(3) 0.10404(18) -0.2916(5) 0.0143(7) Uani 1 1 d . . . H22 H 0.0287 0.0816 -0.3956 0.017 Uiso 1 1 calc R . . C23 C 0.0521(2) 0.17055(18) -0.2571(5) 0.0123(7) Uani 1 1 d . . . C24 C -0.0324(3) 0.20547(17) -0.3709(5) 0.0128(7) Uani 1 1 d . . . O25 O -0.04515(19) 0.26470(13) -0.3320(4) 0.0178(6) Uani 1 1 d . . . O26 O -0.08694(19) 0.17245(13) -0.4968(4) 0.0165(5) Uani 1 1 d . . . C27 C 0.1113(3) 0.20345(19) -0.1072(5) 0.0156(7) Uani 1 1 d . . . H27 H 0.1013 0.2487 -0.0845 0.019 Uiso 1 1 calc R . . O28 O 0.8151(2) 0.15779(14) -0.1403(4) 0.0191(6) Uani 1 1 d . . . H28A H 0.7898 0.1314 -0.2334 0.029 Uiso 1 1 d R . . H28B H 0.8025 0.2059 -0.1984 0.029 Uiso 1 1 d R . . O29 O 1.0046(3) 0.0984(2) 0.1348(7) 0.0421(15) Uani 1 1 d . . . H29A H 1.0452 0.0699 0.1874 0.050 Uiso 1 1 d R . . H29B H 0.9518 0.0794 0.1050 0.050 Uiso 1 1 d R . . O30 O 0.3985(2) -0.01551(15) 0.9009(4) 0.0275(7) Uani 1 1 d . . . H30A H 0.3642 -0.0512 0.8501 0.041 Uiso 1 1 d R . . H30B H 0.4184 -0.0374 1.0106 0.041 Uiso 1 1 d R . . O31 O 0.29002(19) -0.07023(14) 1.3827(4) 0.0227(6) Uani 1 1 d . . . H31A H 0.2900 -0.0862 1.4922 0.034 Uiso 1 1 d R . . H31B H 0.3397 -0.0732 1.3433 0.034 Uiso 1 1 d R . . O32 O 0.1030(5) -0.0050(5) 1.2645(10) 0.0284(19) Uani 0.50 1 d P A 1 O32A O 0.1382(4) 0.0285(3) 1.3202(8) 0.0216(14) Uani 0.50 1 d P A 1 H32A H 0.1039 -0.0076 1.3775 0.042 Uiso 1 1 d R A 1 H32B H 0.1534 -0.0034 1.2463 0.042 Uiso 1 1 d R A 1 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 Eu 0.01260(12) 0.00795(12) 0.01025(12) 0.00011(6) 0.00172(7) 0.00023(6) O1 0.0161(14) 0.0118(12) 0.0214(14) 0.0007(10) 0.0076(11) 0.0019(10) O2 0.0155(13) 0.0115(13) 0.0160(12) -0.0011(10) 0.0041(10) -0.0007(10) C3 0.0145(18) 0.0124(17) 0.0078(15) -0.0007(13) -0.0020(13) -0.0017(14) C4 0.0168(18) 0.0165(18) 0.0082(16) -0.0016(13) 0.0006(13) 0.0009(15) C5 0.0157(18) 0.0165(18) 0.0091(16) -0.0005(13) 0.0006(13) -0.0030(15) C6 0.0164(18) 0.0172(18) 0.0122(17) -0.0022(13) 0.0020(13) 0.0049(15) C7 0.0162(19) 0.0187(18) 0.0194(19) -0.0005(15) 0.0045(15) 0.0034(16) O8 0.0239(16) 0.0156(15) 0.0448(18) -0.0039(13) 0.0138(13) 0.0046(12) O9 0.0221(15) 0.0167(15) 0.0373(17) -0.0025(12) 0.0121(12) 0.0035(12) C10 0.0135(18) 0.0182(19) 0.0136(17) -0.0017(14) 0.0013(13) 0.0016(15) C11 0.0154(18) 0.0189(19) 0.0120(17) -0.0002(13) 0.0009(13) -0.0019(15) C12 0.0179(19) 0.0148(18) 0.0145(17) 0.0017(14) 0.0018(14) 0.0026(15) O13 0.0132(14) 0.0167(14) 0.0220(15) 0.0028(10) 0.0033(11) -0.0013(10) C14 0.0132(18) 0.026(2) 0.0177(18) 0.0001(15) 0.0029(14) -0.0001(16) O15 0.0162(14) 0.0115(13) 0.0212(14) -0.0038(10) -0.0019(10) -0.0017(10) C16 0.0123(18) 0.0159(19) 0.0183(18) -0.0052(14) 0.0056(14) -0.0050(15) C17 0.0143(18) 0.0114(17) 0.0150(17) 0.0022(13) 0.0033(13) 0.0012(14) C18 0.0161(18) 0.0103(18) 0.0148(17) -0.0016(13) 0.0074(14) -0.0012(14) C19 0.0163(18) 0.0091(17) 0.0135(17) 0.0022(12) 0.0040(13) 0.0009(14) O20 0.0242(15) 0.0125(13) 0.0124(12) 0.0010(10) 0.0035(10) 0.0002(11) O21 0.0281(16) 0.0107(13) 0.0182(13) 0.0003(10) -0.0020(11) 0.0006(11) C22 0.0186(19) 0.0143(18) 0.0094(16) -0.0012(13) 0.0023(13) 0.0013(15) C23 0.0155(18) 0.0101(17) 0.0120(16) 0.0003(13) 0.0044(13) 0.0018(14) C24 0.0177(18) 0.0106(17) 0.0114(16) 0.0007(13) 0.0059(13) -0.0002(14) O25 0.0217(14) 0.0139(13) 0.0177(13) -0.0004(10) 0.0044(10) 0.0042(11) O26 0.0208(14) 0.0148(14) 0.0122(12) 0.0007(10) 0.0002(10) 0.0019(11) C27 0.0169(19) 0.0141(18) 0.0165(18) -0.0034(14) 0.0053(14) -0.0022(15) O28 0.0286(16) 0.0132(13) 0.0141(13) 0.0004(10) 0.0021(11) 0.0005(12) O29 0.045(2) 0.036(3) 0.042(4) 0.013(3) 0.014(3) 0.016(2) O30 0.0310(18) 0.0172(15) 0.0315(17) 0.0028(12) 0.0020(13) -0.0085(13) O31 0.0225(15) 0.0298(16) 0.0161(13) 0.0010(11) 0.0048(11) 0.0008(13) O32 0.026(4) 0.029(6) 0.030(4) 0.020(4) 0.022(3) 0.016(4) O32A 0.028(4) 0.013(3) 0.025(3) 0.006(2) 0.009(3) 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 Eu O26 2.283(2) 1_656 ? Eu O25 2.356(3) 4_666 ? Eu O28 2.364(3) . ? Eu O29 2.372(3) . ? Eu O21 2.461(3) 3_655 ? Eu O2 2.463(3) . ? Eu O1 2.480(3) . ? Eu O20 2.476(3) 3_655 ? Eu C19 2.822(4) 3_655 ? Eu C3 2.852(4) . ? Eu H29B 2.0035 . ? O1 C3 1.278(4) . ? O2 C3 1.264(4) . ? C3 C4 1.490(5) . ? C4 C5 1.394(5) . ? C4 C12 1.398(5) . ? C5 C6 1.403(5) . ? C5 H5 0.9500 . ? C6 C10 1.384(6) . ? C6 C7 1.486(5) . ? C7 O9 1.226(5) . ? C7 O8 1.312(5) . ? O8 H8 0.8400 . ? C10 C11 1.395(5) . ? C10 H10 0.9500 . ? C11 O13 1.376(5) . ? C11 C12 1.389(5) . ? C12 H12 0.9500 . ? O13 C14 1.427(5) . ? C14 O15 1.416(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O15 C16 1.382(4) . ? C16 C17 1.387(5) . ? C16 C27 1.391(5) . ? C17 C18 1.401(5) . ? C17 H17 0.9500 . ? C18 C22 1.387(5) . ? C18 C19 1.506(5) . ? C19 O20 1.269(4) . ? C19 O21 1.265(4) . ? C19 Eu 2.822(4) 3_655 ? O20 Eu 2.476(3) 3_655 ? O21 Eu 2.461(3) 3_655 ? C22 C23 1.400(5) . ? C22 H22 0.9500 . ? C23 C27 1.394(5) . ? C23 C24 1.504(5) . ? C24 O25 1.257(4) . ? C24 O26 1.258(4) . ? O25 Eu 2.356(3) 4_465 ? O26 Eu 2.283(2) 1_454 ? C27 H27 0.9500 . ? O28 H28A 0.8727 . ? O28 H28B 1.0600 . ? O29 H29A 0.8574 . ? O29 H29B 0.8529 . ? O30 H30A 0.9097 . ? O30 H30B 0.8954 . ? O31 H31A 0.8549 . ? O31 H31B 0.8530 . ? O32 O32A 0.893(10) . ? O32 H32A 0.8149 . ? O32 H32B 0.7902 . ? O32A H32A 1.0331 . ? O32A H32B 0.9013 . ? 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 O26 Eu O25 78.30(9) 1_656 4_666 ? O26 Eu O28 155.80(10) 1_656 . ? O25 Eu O28 81.82(9) 4_666 . ? O26 Eu O29 100.89(15) 1_656 . ? O25 Eu O29 75.47(12) 4_666 . ? O28 Eu O29 87.22(14) . . ? O26 Eu O21 131.64(9) 1_656 3_655 ? O25 Eu O21 144.52(9) 4_666 3_655 ? O28 Eu O21 72.04(9) . 3_655 ? O29 Eu O21 79.61(14) . 3_655 ? O26 Eu O2 84.17(9) 1_656 . ? O25 Eu O2 80.81(9) 4_666 . ? O28 Eu O2 79.12(9) . . ? O29 Eu O2 154.08(11) . . ? O21 Eu O2 116.04(9) 3_655 . ? O26 Eu O1 86.74(9) 1_656 . ? O25 Eu O1 132.56(9) 4_666 . ? O28 Eu O1 96.79(10) . . ? O29 Eu O1 151.95(12) . . ? O21 Eu O1 75.34(9) 3_655 . ? O2 Eu O1 52.81(8) . . ? O26 Eu O20 80.03(9) 1_656 3_655 ? O25 Eu O20 139.05(9) 4_666 3_655 ? O28 Eu O20 124.18(9) . 3_655 ? O29 Eu O20 75.08(11) . 3_655 ? O21 Eu O20 53.02(9) 3_655 3_655 ? O2 Eu O20 130.75(9) . 3_655 ? O1 Eu O20 79.83(9) . 3_655 ? O26 Eu C19 106.58(9) 1_656 3_655 ? O25 Eu C19 148.50(10) 4_666 3_655 ? O28 Eu C19 97.59(10) . 3_655 ? O29 Eu C19 73.04(13) . 3_655 ? O21 Eu C19 26.60(9) 3_655 3_655 ? O2 Eu C19 130.26(9) . 3_655 ? O1 Eu C19 78.91(10) . 3_655 ? O20 Eu C19 26.70(9) 3_655 3_655 ? O26 Eu C3 84.85(9) 1_656 . ? O25 Eu C3 106.57(10) 4_666 . ? O28 Eu C3 87.75(10) . . ? O29 Eu C3 174.23(15) . . ? O21 Eu C3 96.15(10) 3_655 . ? O2 Eu C3 26.22(9) . . ? O1 Eu C3 26.59(9) . . ? O20 Eu C3 105.57(10) 3_655 . ? C19 Eu C3 104.87(10) 3_655 . ? O26 Eu H29B 114.0 1_656 . ? O25 Eu H29B 93.7 4_666 . ? O28 Eu H29B 80.8 . . ? O29 Eu H29B 20.3 . . ? O21 Eu H29B 59.3 3_655 . ? O2 Eu H29B 159.7 . . ? O1 Eu H29B 133.2 . . ? O20 Eu H29B 64.5 3_655 . ? C19 Eu H29B 55.5 3_655 . ? C3 Eu H29B 155.1 . . ? C3 O1 Eu 93.1(2) . . ? C3 O2 Eu 94.3(2) . . ? O2 C3 O1 119.7(3) . . ? O2 C3 C4 120.1(3) . . ? O1 C3 C4 120.2(3) . . ? O2 C3 Eu 59.46(19) . . ? O1 C3 Eu 60.28(19) . . ? C4 C3 Eu 179.5(3) . . ? C5 C4 C12 120.2(3) . . ? C5 C4 C3 119.0(3) . . ? C12 C4 C3 120.8(3) . . ? C4 C5 C6 119.1(4) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C10 C6 C5 120.8(4) . . ? C10 C6 C7 121.0(3) . . ? C5 C6 C7 118.1(3) . . ? O9 C7 O8 123.4(4) . . ? O9 C7 C6 123.3(4) . . ? O8 C7 C6 113.3(4) . . ? C7 O8 H8 109.5 . . ? C6 C10 C11 119.6(4) . . ? C6 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? O13 C11 C12 115.8(3) . . ? O13 C11 C10 123.8(3) . . ? C12 C11 C10 120.4(4) . . ? C11 C12 C4 119.8(4) . . ? C11 C12 H12 120.1 . . ? C4 C12 H12 120.1 . . ? C11 O13 C14 117.3(3) . . ? O13 C14 O15 112.4(3) . . ? O13 C14 H14A 109.1 . . ? O15 C14 H14A 109.1 . . ? O13 C14 H14B 109.1 . . ? O15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C16 O15 C14 118.1(3) . . ? O15 C16 C17 123.3(3) . . ? O15 C16 C27 115.8(3) . . ? C17 C16 C27 120.8(3) . . ? C16 C17 C18 118.9(3) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C22 C18 C17 121.1(3) . . ? C22 C18 C19 119.9(3) . . ? C17 C18 C19 118.7(3) . . ? O20 C19 O21 120.8(3) . . ? O20 C19 C18 120.8(3) . . ? O21 C19 C18 118.4(3) . . ? O20 C19 Eu 61.26(19) . 3_655 ? O21 C19 Eu 60.55(19) . 3_655 ? C18 C19 Eu 167.8(2) . 3_655 ? C19 O20 Eu 92.0(2) . 3_655 ? C19 O21 Eu 92.9(2) . 3_655 ? C18 C22 C23 119.5(3) . . ? C18 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C27 C23 C22 119.8(3) . . ? C27 C23 C24 119.5(3) . . ? C22 C23 C24 120.6(3) . . ? O25 C24 O26 124.4(3) . . ? O25 C24 C23 118.5(3) . . ? O26 C24 C23 117.1(3) . . ? C24 O25 Eu 154.9(3) . 4_465 ? C24 O26 Eu 149.1(2) . 1_454 ? C23 C27 C16 120.0(3) . . ? C23 C27 H27 120.0 . . ? C16 C27 H27 120.0 . . ? Eu O28 H28A 132.2 . . ? Eu O28 H28B 121.1 . . ? H28A O28 H28B 104.7 . . ? Eu O29 H29A 136.2 . . ? Eu O29 H29B 54.7 . . ? H29A O29 H29B 108.4 . . ? H30A O30 H30B 90.1 . . ? H31A O31 H31B 118.1 . . ? H32A O32 H32B 112.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 O13 O15 C16 123.3(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 O8 H8 O30 0.84 1.74 2.564(4) 167 4_565 O28 H28A O31 0.87 1.87 2.713(4) 162 3_656 O28 H28B O2 1.06 1.73 2.753(4) 161 4_565 O29 H29A O32A 0.86 1.70 2.546(7) 167 1_654 O29 H29B O21 0.85 2.24 3.095(5) 175 3_655 O30 H30A O1 0.91 1.93 2.840(4) 179 3_656 O30 H30B O9 0.90 1.94 2.830(4) 178 2_646 O31 H31A O1 0.85 2.01 2.865(4) 178 3_657 O31 H31B O9 0.85 2.03 2.885(4) 179 2_646 O32 H32B O21 0.79 2.38 2.899(7) 124 1_556 O32 H32A O20 0.81 2.01 2.817(7) 169 1_557 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.448 _refine_diff_density_min -1.449 _refine_diff_density_rms 0.150 #=================END============================== data_8 _database_code_depnum_ccdc_archive 'CCDC 772538' #TrackingRef '- ka3-26-Ln.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H17 La O13, H2 O' _chemical_formula_sum 'C18 H19 La O14' _chemical_formula_weight 598.24 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5147(2) _cell_length_b 10.2584(2) _cell_length_c 12.4540(5) _cell_angle_alpha 68.4154(10) _cell_angle_beta 89.3378(11) _cell_angle_gamma 72.780(2) _cell_volume 960.37(5) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4226 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.99 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 2.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5963 _exptl_absorpt_correction_T_max 0.8022 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f anf \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16654 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.99 _reflns_number_total 4565 _reflns_number_gt 3924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo and Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two of the O-atoms are disordered. ; _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^)+(0.0531P)^2^+2.6625P] 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 4565 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.009 _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 La La 0.84466(3) 1.17822(2) 0.263756(18) 0.01304(8) Uani 1 1 d . . . O1 O 0.6548(4) 1.0446(3) 0.2267(2) 0.0183(6) Uani 1 1 d . . . O2 O 0.8755(4) 1.0299(3) 0.1320(2) 0.0180(6) Uani 1 1 d . . . C3 C 0.7444(5) 0.9991(4) 0.1572(3) 0.0130(7) Uani 1 1 d . . . C4 C 0.6935(5) 0.9040(4) 0.1064(3) 0.0128(7) Uani 1 1 d . . . C5 C 0.7834(5) 0.8606(4) 0.0252(3) 0.0139(7) Uani 1 1 d . . . H5 H 0.8752 0.8937 -0.0010 0.017 Uiso 1 1 calc R . . C6 C 0.7371(5) 0.7671(4) -0.0177(3) 0.0149(8) Uani 1 1 d . . . C7 C 0.8331(6) 0.7168(5) -0.1041(4) 0.0198(9) Uani 1 1 d . . . O8 O 0.8996(3) 0.8014(3) -0.1754(2) 0.0181(6) Uani 1 1 d . . . O9A O 0.8033(10) 0.6086(8) -0.1189(6) 0.0171(14) Uani 0.50 1 d P . . O9B O 0.8815(10) 0.5753(8) -0.0852(7) 0.0201(15) Uani 0.50 1 d P . . C10 C 0.6026(5) 0.7192(4) 0.0206(3) 0.0154(8) Uani 1 1 d . . . H10 H 0.5741 0.6532 -0.0067 0.018 Uiso 1 1 calc R . . C11 C 0.5100(5) 0.7679(4) 0.0987(3) 0.0140(7) Uani 1 1 d . . . C12 C 0.5544(5) 0.8589(4) 0.1428(3) 0.0140(7) Uani 1 1 d . . . H12 H 0.4917 0.8907 0.1972 0.017 Uiso 1 1 calc R . . O13 O 0.3759(4) 0.7173(3) 0.1269(2) 0.0171(6) Uani 1 1 d . . . C14 C 0.2674(5) 0.7667(5) 0.2039(3) 0.0176(8) Uani 1 1 d . . . H14A H 0.1592 0.7531 0.1931 0.021 Uiso 1 1 calc R . . H14B H 0.2487 0.8734 0.1830 0.021 Uiso 1 1 calc R . . C15 C 0.3364(5) 0.6848(4) 0.3292(3) 0.0176(8) Uani 1 1 d . . . H15A H 0.4414 0.7028 0.3419 0.021 Uiso 1 1 calc R . . H15B H 0.2574 0.7210 0.3786 0.021 Uiso 1 1 calc R . . O16 O 0.3659(4) 0.5279(3) 0.3612(2) 0.0185(6) Uani 1 1 d . . . C17 C 0.2886(5) 0.4584(4) 0.4531(3) 0.0144(8) Uani 1 1 d . . . C18 C 0.2592(5) 0.4993(4) 0.5484(3) 0.0151(8) Uani 1 1 d . . . H18 H 0.2989 0.5735 0.5552 0.018 Uiso 1 1 calc R . . C19 C 0.1709(5) 0.4297(4) 0.6335(3) 0.0146(8) Uani 1 1 d . . . C20 C 0.1231(5) 0.4872(4) 0.7266(3) 0.0165(8) Uani 1 1 d . . . O21 O 0.1930(4) 0.5655(3) 0.7488(2) 0.0211(6) Uani 1 1 d . . . O22 O -0.0018(4) 0.4535(3) 0.7788(2) 0.0204(6) Uani 1 1 d . . . H22 H -0.0582 0.5181 0.8210 0.025 Uiso 1 1 d R . . C23 C 0.1149(5) 0.3183(4) 0.6253(3) 0.0143(8) Uani 1 1 d . . . H23 H 0.0539 0.2719 0.6832 0.017 Uiso 1 1 calc R . . C24 C 0.1494(5) 0.2764(4) 0.5314(3) 0.0149(8) Uani 1 1 d . . . C25 C 0.0709(5) 0.1708(4) 0.5138(3) 0.0176(8) Uani 1 1 d . . . O26 O 0.0208(4) 0.0879(3) 0.6018(2) 0.0172(6) Uani 1 1 d . . . O27 O 0.0522(4) 0.1760(3) 0.4126(2) 0.0215(6) Uani 1 1 d . . . C28 C 0.2373(5) 0.3454(4) 0.4458(3) 0.0173(8) Uani 1 1 d . . . H28 H 0.2620 0.3150 0.3825 0.021 Uiso 1 1 calc R . . O29 O 0.7602(4) 1.3514(3) 0.0481(2) 0.0191(6) Uani 1 1 d . . . H29A H 0.7690 1.4426 0.0036 0.023 Uiso 1 1 d R . . H29B H 0.7353 1.3091 -0.0109 0.023 Uiso 1 1 d R . . O30 O 0.5313(4) 1.3318(3) 0.2401(3) 0.0229(6) Uani 1 1 d . . . H30A H 0.4868 1.4322 0.2245 0.028 Uiso 1 1 d R . . H30B H 0.4463 1.3007 0.2227 0.028 Uiso 1 1 d R . . O31 O 0.7302(4) 1.1434(4) 0.4614(3) 0.0275(7) Uani 1 1 d . . . H31A H 0.8104 1.1129 0.5219 0.033 Uiso 1 1 d R . . H31B H 0.6418 1.1120 0.4892 0.033 Uiso 1 1 d R . . O32A O 0.3999(12) 1.0601(10) 0.3563(9) 0.034(2) Uani 0.56 1 d P . . O32B O 0.402(2) 0.9958(13) 0.3639(14) 0.049(4) Uani 0.44 1 d P . . H32A H 0.4784 1.0405 0.3151 0.074 Uiso 1 1 d R . . H32B H 0.2919 1.1368 0.3242 0.074 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La 0.01875(13) 0.01231(12) 0.01114(12) -0.00584(9) 0.00210(8) -0.00749(9) O1 0.0203(15) 0.0229(15) 0.0191(14) -0.0144(12) 0.0044(11) -0.0091(12) O2 0.0216(15) 0.0228(15) 0.0180(14) -0.0125(12) 0.0052(11) -0.0131(13) C3 0.0190(19) 0.0103(17) 0.0099(17) -0.0039(14) 0.0000(14) -0.0047(15) C4 0.0175(19) 0.0087(17) 0.0104(17) -0.0031(14) -0.0037(14) -0.0019(15) C5 0.021(2) 0.0086(17) 0.0137(18) -0.0044(14) 0.0013(15) -0.0066(15) C6 0.023(2) 0.0104(18) 0.0113(18) -0.0041(14) 0.0019(15) -0.0051(16) C7 0.033(2) 0.017(2) 0.017(2) -0.0123(16) 0.0065(17) -0.0115(18) O8 0.0161(14) 0.0189(14) 0.0231(15) -0.0109(12) 0.0049(11) -0.0074(12) O9A 0.023(4) 0.018(4) 0.017(4) -0.013(3) 0.010(3) -0.010(3) O9B 0.026(4) 0.018(4) 0.021(4) -0.012(3) 0.011(3) -0.009(3) C10 0.022(2) 0.0112(18) 0.0143(18) -0.0056(15) -0.0024(15) -0.0061(16) C11 0.0166(19) 0.0104(17) 0.0130(18) -0.0024(14) -0.0026(14) -0.0036(15) C12 0.0187(19) 0.0121(18) 0.0106(17) -0.0050(14) -0.0024(14) -0.0029(15) O13 0.0206(15) 0.0194(14) 0.0182(14) -0.0105(12) 0.0046(11) -0.0118(12) C14 0.0148(19) 0.022(2) 0.019(2) -0.0103(17) 0.0014(15) -0.0058(16) C15 0.021(2) 0.0133(19) 0.021(2) -0.0083(16) 0.0043(16) -0.0068(16) O16 0.0260(16) 0.0125(13) 0.0218(15) -0.0092(12) 0.0099(12) -0.0101(12) C17 0.0160(19) 0.0103(17) 0.0146(18) -0.0035(15) -0.0005(14) -0.0024(15) C18 0.0173(19) 0.0113(18) 0.0171(19) -0.0065(15) -0.0027(15) -0.0035(15) C19 0.0174(19) 0.0089(17) 0.0142(18) -0.0034(14) -0.0057(14) -0.0004(15) C20 0.024(2) 0.0114(18) 0.0104(18) -0.0019(14) -0.0035(15) -0.0038(16) O21 0.0339(17) 0.0165(14) 0.0163(14) -0.0078(12) -0.0032(12) -0.0102(13) O22 0.0331(17) 0.0168(14) 0.0145(14) -0.0082(11) 0.0057(12) -0.0096(13) C23 0.0182(19) 0.0112(18) 0.0144(18) -0.0048(15) -0.0038(14) -0.0059(15) C24 0.0183(19) 0.0104(17) 0.0148(18) -0.0049(15) -0.0040(15) -0.0025(15) C25 0.024(2) 0.0092(18) 0.0173(19) -0.0037(15) -0.0036(16) -0.0036(16) O26 0.0269(16) 0.0113(13) 0.0139(13) -0.0041(11) 0.0012(11) -0.0078(12) O27 0.0370(18) 0.0213(15) 0.0115(13) -0.0074(12) -0.0010(12) -0.0152(14) C28 0.024(2) 0.0125(18) 0.0140(19) -0.0047(15) -0.0029(15) -0.0044(16) O29 0.0292(16) 0.0152(14) 0.0150(14) -0.0058(11) -0.0004(12) -0.0098(13) O30 0.0187(15) 0.0257(16) 0.0300(16) -0.0171(14) 0.0028(12) -0.0066(13) O31 0.0289(17) 0.0343(18) 0.0194(15) -0.0135(14) 0.0046(13) -0.0063(15) O32A 0.018(3) 0.056(6) 0.042(5) -0.030(5) 0.016(3) -0.016(5) O32B 0.036(6) 0.034(7) 0.062(7) -0.002(6) 0.016(5) -0.012(6) _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 La O8 2.457(3) 2_775 ? La O21 2.498(3) 2_676 ? La O26 2.530(3) 2_666 ? La O1 2.549(3) . ? La O27 2.566(3) 1_665 ? La O31 2.577(3) . ? La O29 2.582(3) . ? La O2 2.582(3) . ? La O30 2.622(3) . ? La C3 2.935(4) . ? O1 C3 1.273(5) . ? O2 C3 1.254(5) . ? C3 C4 1.501(5) . ? C4 C5 1.384(5) . ? C4 C12 1.407(5) . ? C5 C6 1.402(5) . ? C5 H5 0.9500 . ? C6 C10 1.388(6) . ? C6 C7 1.494(5) . ? C7 O8 1.255(5) . ? C7 O9A 1.284(8) . ? C7 O9B 1.315(8) . ? O8 La 2.457(3) 2_775 ? O9A O9B 0.708(7) . ? C10 C11 1.387(6) . ? C10 H10 0.9500 . ? C11 O13 1.380(5) . ? C11 C12 1.382(5) . ? C12 H12 0.9500 . ? O13 C14 1.446(5) . ? C14 C15 1.500(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O16 1.450(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O16 C17 1.382(5) . ? C17 C28 1.386(5) . ? C17 C18 1.395(5) . ? C18 C19 1.393(6) . ? C18 H18 0.9500 . ? C19 C23 1.397(5) . ? C19 C20 1.486(5) . ? C20 O21 1.236(5) . ? C20 O22 1.307(5) . ? O21 La 2.498(3) 2_676 ? O22 H22 1.0042 . ? C23 C24 1.387(5) . ? C23 H23 0.9500 . ? C24 C28 1.392(6) . ? C24 C25 1.508(5) . ? C25 O27 1.252(5) . ? C25 O26 1.274(5) . ? O26 La 2.530(3) 2_666 ? O27 La 2.566(3) 1_445 ? C28 H28 0.9500 . ? O29 H29A 0.9202 . ? O29 H29B 1.0325 . ? O30 H30A 0.9307 . ? O30 H30B 0.9296 . ? O31 H31A 0.9193 . ? O31 H31B 0.9191 . ? O32A O32B 0.625(11) . ? O32A H32A 0.8595 . ? O32A H32B 0.9862 . ? 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 O8 La O21 84.20(10) 2_775 2_676 ? O8 La O26 93.20(9) 2_775 2_666 ? O21 La O26 140.68(9) 2_676 2_666 ? O8 La O1 126.80(9) 2_775 . ? O21 La O1 135.01(10) 2_676 . ? O26 La O1 76.17(9) 2_666 . ? O8 La O27 70.81(9) 2_775 1_665 ? O21 La O27 69.49(9) 2_676 1_665 ? O26 La O27 72.63(9) 2_666 1_665 ? O1 La O27 145.07(9) . 1_665 ? O8 La O31 139.13(10) 2_775 . ? O21 La O31 84.13(10) 2_676 . ? O26 La O31 72.41(10) 2_666 . ? O1 La O31 87.59(10) . . ? O27 La O31 68.41(10) 1_665 . ? O8 La O29 72.79(9) 2_775 . ? O21 La O29 72.83(9) 2_676 . ? O26 La O29 143.44(9) 2_666 . ? O1 La O29 85.51(9) . . ? O27 La O29 129.28(9) 1_665 . ? O31 La O29 138.85(10) . . ? O8 La O2 75.94(9) 2_775 . ? O21 La O2 140.45(9) 2_676 . ? O26 La O2 75.17(9) 2_666 . ? O1 La O2 50.87(9) . . ? O27 La O2 131.55(10) 1_665 . ? O31 La O2 132.28(10) . . ? O29 La O2 68.76(9) . . ? O8 La O30 140.05(10) 2_775 . ? O21 La O30 68.05(10) 2_676 . ? O26 La O30 126.53(9) 2_666 . ? O1 La O30 67.86(9) . . ? O27 La O30 120.76(10) 1_665 . ? O31 La O30 67.97(10) . . ? O29 La O30 71.87(9) . . ? O2 La O30 107.42(9) . . ? O8 La C3 101.19(10) 2_775 . ? O21 La C3 145.07(10) 2_676 . ? O26 La C3 73.97(9) 2_666 . ? O1 La C3 25.62(10) . . ? O27 La C3 145.03(10) 1_665 . ? O31 La C3 110.55(10) . . ? O29 La C3 75.93(9) . . ? O2 La C3 25.25(10) . . ? O30 La C3 87.76(10) . . ? C3 O1 La 94.4(2) . . ? C3 O2 La 93.3(2) . . ? O2 C3 O1 121.4(3) . . ? O2 C3 C4 119.4(3) . . ? O1 C3 C4 119.1(3) . . ? O2 C3 La 61.42(19) . . ? O1 C3 La 60.00(19) . . ? C4 C3 La 178.2(2) . . ? C5 C4 C12 120.6(3) . . ? C5 C4 C3 120.2(3) . . ? C12 C4 C3 119.2(3) . . ? C4 C5 C6 119.1(4) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C10 C6 C5 120.4(4) . . ? C10 C6 C7 119.3(3) . . ? C5 C6 C7 120.3(4) . . ? O8 C7 O9A 123.5(5) . . ? O8 C7 O9B 120.1(5) . . ? O8 C7 C6 118.8(3) . . ? O9A C7 C6 115.0(5) . . ? O9B C7 C6 118.8(4) . . ? C7 O8 La 145.3(3) . 2_775 ? O9B O9A C7 76.6(10) . . ? O9A O9B C7 71.8(10) . . ? C11 C10 C6 119.9(3) . . ? C11 C10 H10 120.0 . . ? C6 C10 H10 120.0 . . ? O13 C11 C12 124.8(4) . . ? O13 C11 C10 114.7(3) . . ? C12 C11 C10 120.6(4) . . ? C11 C12 C4 119.3(4) . . ? C11 C12 H12 120.3 . . ? C4 C12 H12 120.3 . . ? C11 O13 C14 119.0(3) . . ? O13 C14 C15 112.5(3) . . ? O13 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? O13 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? O16 C15 C14 109.8(3) . . ? O16 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? O16 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C17 O16 C15 117.2(3) . . ? O16 C17 C28 116.7(3) . . ? O16 C17 C18 122.9(3) . . ? C28 C17 C18 120.4(4) . . ? C19 C18 C17 119.1(4) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C23 C19 C18 120.8(4) . . ? C23 C19 C20 120.7(4) . . ? C18 C19 C20 118.2(3) . . ? O21 C20 O22 123.3(4) . . ? O21 C20 C19 121.8(4) . . ? O22 C20 C19 114.8(3) . . ? C20 O21 La 143.6(3) . 2_676 ? C20 O22 H22 114.6 . . ? C24 C23 C19 119.2(4) . . ? C24 C23 H23 120.4 . . ? C19 C23 H23 120.4 . . ? C23 C24 C28 120.4(4) . . ? C23 C24 C25 119.3(4) . . ? C28 C24 C25 119.7(3) . . ? O27 C25 O26 124.6(4) . . ? O27 C25 C24 117.6(4) . . ? O26 C25 C24 117.8(3) . . ? C25 O26 La 130.8(3) . 2_666 ? C25 O27 La 143.2(3) . 1_445 ? C17 C28 C24 120.0(4) . . ? C17 C28 H28 120.0 . . ? C24 C28 H28 120.0 . . ? La O29 H29A 134.1 . . ? La O29 H29B 119.1 . . ? H29A O29 H29B 105.1 . . ? La O30 H30A 127.4 . . ? La O30 H30B 122.9 . . ? H30A O30 H30B 107.1 . . ? La O31 H31A 113.6 . . ? La O31 H31B 129.6 . . ? H31A O31 H31B 109.4 . . ? H32A O32A H32B 124.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O22 H22 O9B 1.00 1.51 2.491(8) 163 1_456 O22 H22 O9A 1.00 1.63 2.606(8) 163 1_456 O29 H29A O9B 0.92 1.91 2.767(8) 155 1_565 O29 H29A O9A 0.92 1.92 2.818(8) 165 1_565 O29 H29B O13 1.03 1.88 2.874(4) 161 2_675 O30 H30A O16 0.93 2.35 2.968(4) 124 1_565 O30 H30B O9A 0.93 2.25 3.026(8) 141 2_675 O31 H31A O26 0.92 1.96 2.836(4) 158 1_665 O31 H31B O32B 0.92 1.86 2.580(15) 134 2_676 O31 H31B O32A 0.92 2.19 2.927(10) 136 2_676 O32A H32A O1 0.86 1.85 2.691(10) 164 . O32A H32B O8 0.99 2.26 3.038(11) 135 2_675 O32A H32B O27 0.99 2.31 3.025(10) 129 1_565 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.932 _refine_diff_density_min -1.781 _refine_diff_density_rms 0.158 #======================END============================== data_9 _database_code_depnum_ccdc_archive 'CCDC 772539' #TrackingRef '- ka3-26-Ln.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H15 Nd O12), 4(H2 O), 3(O)' _chemical_formula_sum 'C36 H38 Nd2 O31' _chemical_formula_weight 1255.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5679(3) _cell_length_b 9.9939(3) _cell_length_c 12.5472(5) _cell_angle_alpha 91.5960(15) _cell_angle_beta 94.8827(14) _cell_angle_gamma 93.4052(16) _cell_volume 1068.00(7) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3561 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.90 _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.952 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 622 _exptl_absorpt_coefficient_mu 2.514 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5193 _exptl_absorpt_correction_T_max 0.7043 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10107 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.90 _reflns_number_total 4997 _reflns_number_gt 4113 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Atoms O33a and O33b represent possible positions of two severely disordered water molecules trapped in the interstitial voids. ; _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^)+(0.0815P)^2^+1.1382P] 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 4997 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1294 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Nd Nd 0.40284(3) 0.60355(3) -0.32267(2) 0.01608(12) Uani 1 1 d . . . O1 O 0.3606(5) 0.7364(4) -0.1512(3) 0.0249(9) Uani 1 1 d . . . O2 O 0.4736(5) 0.8404(4) -0.2797(3) 0.0220(9) Uani 1 1 d . . . C3 C 0.4074(6) 0.8437(5) -0.1938(4) 0.0165(11) Uani 1 1 d . . . C4 C 0.3791(6) 0.9766(5) -0.1429(4) 0.0166(11) Uani 1 1 d . . . C5 C 0.4200(6) 1.0912(5) -0.1985(4) 0.0166(11) Uani 1 1 d . . . H5 H 0.4685 1.0844 -0.2636 0.020 Uiso 1 1 calc R . . C6 C 0.3872(6) 1.2166(5) -0.1551(4) 0.0169(11) Uani 1 1 d . . . C7 C 0.4155(7) 1.3422(5) -0.2153(4) 0.0173(11) Uani 1 1 d . . . O8 O 0.5051(5) 1.3488(4) -0.2905(3) 0.0177(8) Uani 1 1 d . . . O9 O 0.3420(5) 1.4428(4) -0.1876(3) 0.0208(8) Uani 1 1 d . . . C10 C 0.3183(6) 1.2250(5) -0.0598(5) 0.0174(11) Uani 1 1 d . . . H10 H 0.2970 1.3101 -0.0309 0.021 Uiso 1 1 calc R . . C11 C 0.2795(6) 1.1085(6) -0.0056(4) 0.0181(11) Uani 1 1 d . . . C12 C 0.3100(6) 0.9834(5) -0.0473(4) 0.0174(11) Uani 1 1 d . . . H12 H 0.2839 0.9041 -0.0109 0.021 Uiso 1 1 calc R . . O13 O 0.2120(5) 1.1297(4) 0.0893(3) 0.0228(9) Uani 1 1 d . . . C14 C 0.1574(7) 1.0121(6) 0.1407(5) 0.0210(12) Uani 1 1 d . . . H14A H 0.2475 0.9627 0.1697 0.025 Uiso 1 1 calc R . . H14B H 0.0912 0.9522 0.0888 0.025 Uiso 1 1 calc R . . C15 C 0.0636(7) 1.0563(5) 0.2296(5) 0.0194(11) Uani 1 1 d . . . H15A H 0.1295 1.1134 0.2837 0.023 Uiso 1 1 calc R . . H15B H -0.0266 1.1064 0.2018 0.023 Uiso 1 1 calc R . . O16 O 0.0117(5) 0.9316(4) 0.2739(3) 0.0218(8) Uani 1 1 d . . . C17 C -0.0865(6) 0.9348(5) 0.3542(4) 0.0167(11) Uani 1 1 d . . . C18 C -0.1359(6) 0.8085(5) 0.3881(4) 0.0170(11) Uani 1 1 d . . . H18 H -0.0991 0.7300 0.3568 0.020 Uiso 1 1 calc R . . C19 C -0.2385(6) 0.7974(5) 0.4677(4) 0.0143(10) Uani 1 1 d . . . C20 C -0.2988(6) 0.6578(5) 0.4958(4) 0.0147(10) Uani 1 1 d . . . O21 O -0.2564(5) 0.5590(4) 0.4439(3) 0.0178(8) Uani 1 1 d . . . O22 O -0.3889(5) 0.6474(4) 0.5694(3) 0.0213(8) Uani 1 1 d . . . C23 C -0.2918(6) 0.9122(5) 0.5161(4) 0.0160(10) Uani 1 1 d . . . H23 H -0.3600 0.9050 0.5718 0.019 Uiso 1 1 calc R . . C24 C -0.2419(6) 1.0374(5) 0.4802(4) 0.0146(10) Uani 1 1 d . . . C25 C -0.2959(6) 1.1641(5) 0.5273(4) 0.0165(11) Uani 1 1 d . . . O26 O -0.2879(5) 1.2708(4) 0.4820(3) 0.0200(8) Uani 1 1 d . . . O27 O -0.3528(5) 1.1500(4) 0.6208(3) 0.0209(8) Uani 1 1 d . . . H27 H -0.3986 1.2189 0.6366 0.031 Uiso 1 1 calc R . . C28 C -0.1398(6) 1.0490(5) 0.3993(4) 0.0166(11) Uani 1 1 d . . . H28 H -0.1074 1.1349 0.3756 0.020 Uiso 1 1 calc R . . O29 O 0.1188(5) 0.6319(4) -0.2962(3) 0.0219(9) Uani 1 1 d . . . H29A H 0.1037 0.6455 -0.2266 0.033 Uiso 1 1 d R . . H29B H 0.0372 0.5855 -0.3329 0.033 Uiso 1 1 d R . . O30 O 0.6592(5) 0.6015(4) -0.2027(3) 0.0226(9) Uani 1 1 d . . . H30A H 0.7077 0.6820 -0.1841 0.034 Uiso 1 1 d R . . H30B H 0.6497 0.5482 -0.1468 0.034 Uiso 1 1 d R . . O31 O 0.3264(7) 0.5686(5) 0.0385(4) 0.0450(13) Uani 1 1 d . . . H31A H 0.4086 0.6153 0.0157 0.068 Uiso 1 1 d R . . H31B H 0.2430 0.5515 -0.0096 0.068 Uiso 1 1 d R . . O32 O 0.1382(5) 0.5459(4) 0.3399(4) 0.0281(10) Uani 1 1 d . . . H32A H 0.1823 0.4780 0.3075 0.042 Uiso 1 1 d R . . H32B H 0.0646 0.5832 0.2968 0.042 Uiso 1 1 d R . . O33A O 0.0516(13) 0.5723(11) 0.9185(9) 0.046(3) Uiso 0.75 1 d P A 1 O33B O -0.0698(17) 0.3143(15) 0.8487(12) 0.050(3) Uiso 0.75 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd 0.02020(17) 0.01153(16) 0.01752(17) 0.00167(10) 0.00644(11) 0.00180(11) O1 0.038(2) 0.0131(19) 0.025(2) 0.0031(16) 0.0116(19) -0.0024(17) O2 0.032(2) 0.0116(18) 0.025(2) 0.0019(16) 0.0124(18) 0.0059(16) C3 0.019(3) 0.013(2) 0.018(3) 0.002(2) 0.002(2) 0.004(2) C4 0.017(3) 0.014(3) 0.019(3) -0.001(2) 0.003(2) -0.001(2) C5 0.018(3) 0.016(3) 0.016(3) -0.001(2) 0.001(2) 0.002(2) C6 0.017(3) 0.017(3) 0.017(3) 0.003(2) 0.005(2) 0.001(2) C7 0.024(3) 0.011(2) 0.016(3) 0.000(2) 0.002(2) 0.000(2) O8 0.024(2) 0.0143(18) 0.0157(19) 0.0013(15) 0.0081(16) 0.0031(15) O9 0.030(2) 0.0122(18) 0.022(2) 0.0006(15) 0.0121(17) 0.0071(16) C10 0.019(3) 0.013(2) 0.020(3) 0.000(2) 0.003(2) 0.000(2) C11 0.019(3) 0.019(3) 0.017(3) 0.001(2) 0.006(2) 0.003(2) C12 0.016(3) 0.016(3) 0.020(3) 0.006(2) 0.002(2) 0.001(2) O13 0.031(2) 0.017(2) 0.023(2) 0.0029(16) 0.0158(18) 0.0022(16) C14 0.026(3) 0.018(3) 0.021(3) 0.010(2) 0.007(2) 0.004(2) C15 0.024(3) 0.013(3) 0.022(3) 0.005(2) 0.004(2) 0.000(2) O16 0.026(2) 0.0148(19) 0.026(2) 0.0036(16) 0.0110(17) 0.0020(16) C17 0.015(3) 0.022(3) 0.013(2) 0.001(2) 0.002(2) 0.000(2) C18 0.016(3) 0.015(2) 0.021(3) -0.001(2) 0.002(2) 0.002(2) C19 0.015(2) 0.013(2) 0.015(2) 0.0018(19) 0.002(2) 0.0018(19) C20 0.013(2) 0.016(3) 0.014(3) 0.002(2) 0.002(2) -0.0030(19) O21 0.025(2) 0.0115(18) 0.0181(19) -0.0006(14) 0.0052(16) 0.0032(15) O22 0.023(2) 0.0178(19) 0.025(2) 0.0024(16) 0.0139(17) 0.0011(16) C23 0.014(3) 0.016(3) 0.017(3) 0.000(2) 0.003(2) 0.000(2) C24 0.020(3) 0.009(2) 0.015(3) 0.0042(19) 0.000(2) 0.0022(19) C25 0.013(2) 0.017(3) 0.020(3) -0.002(2) 0.000(2) 0.001(2) O26 0.024(2) 0.0132(19) 0.024(2) 0.0023(16) 0.0051(17) 0.0034(15) O27 0.026(2) 0.0176(19) 0.021(2) 0.0023(16) 0.0091(17) 0.0044(16) C28 0.018(3) 0.014(2) 0.018(3) 0.001(2) 0.004(2) -0.004(2) O29 0.020(2) 0.0175(19) 0.029(2) 0.0028(16) 0.0095(17) 0.0011(15) O30 0.026(2) 0.022(2) 0.020(2) 0.0018(16) 0.0045(17) 0.0018(17) O31 0.055(3) 0.033(3) 0.043(3) 0.012(2) -0.011(3) -0.011(2) O32 0.024(2) 0.032(2) 0.029(2) -0.0003(19) 0.0051(18) 0.0047(18) _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 Nd O22 2.359(4) 1_654 ? Nd O21 2.413(4) 2_565 ? Nd O9 2.434(4) 1_545 ? Nd O2 2.442(4) . ? Nd O29 2.515(4) . ? Nd O26 2.549(4) 2_575 ? Nd O30 2.556(4) . ? Nd O1 2.560(4) . ? Nd O8 2.770(4) 1_545 ? Nd C3 2.852(5) . ? Nd C7 2.975(5) 1_545 ? O1 C3 1.270(6) . ? O2 C3 1.260(7) . ? C3 C4 1.499(7) . ? C4 C12 1.385(8) . ? C4 C5 1.399(7) . ? C5 C6 1.406(7) . ? C5 H5 0.9500 . ? C6 C10 1.381(8) . ? C6 C7 1.501(7) . ? C7 O8 1.266(7) . ? C7 O9 1.273(6) . ? C7 Nd 2.975(5) 1_565 ? O8 Nd 2.770(4) 1_565 ? O9 Nd 2.434(4) 1_565 ? C10 C11 1.402(7) . ? C10 H10 0.9500 . ? C11 O13 1.384(7) . ? C11 C12 1.390(8) . ? C12 H12 0.9500 . ? O13 C14 1.429(6) . ? C14 C15 1.501(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O16 1.441(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O16 C17 1.367(7) . ? C17 C28 1.379(7) . ? C17 C18 1.397(7) . ? C18 C19 1.388(8) . ? C18 H18 0.9500 . ? C19 C23 1.401(7) . ? C19 C20 1.520(7) . ? C20 O22 1.256(6) . ? C20 O21 1.256(6) . ? O21 Nd 2.413(4) 2_565 ? O22 Nd 2.359(4) 1_456 ? C23 C24 1.397(7) . ? C23 H23 0.9500 . ? C24 C28 1.398(8) . ? C24 C25 1.497(7) . ? C25 O26 1.224(6) . ? C25 O27 1.316(7) . ? O26 Nd 2.549(4) 2_575 ? O27 H27 0.8400 . ? C28 H28 0.9500 . ? O29 H29A 0.9011 . ? O29 H29B 0.9008 . ? O30 H30A 0.8989 . ? O30 H30B 0.8991 . ? O31 H31A 0.8934 . ? O31 H31B 0.8999 . ? O32 H32A 0.8998 . ? O32 H32B 0.8998 . ? 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 O22 Nd O21 96.48(14) 1_654 2_565 ? O22 Nd O9 136.20(13) 1_654 1_545 ? O21 Nd O9 83.75(13) 2_565 1_545 ? O22 Nd O2 78.05(13) 1_654 . ? O21 Nd O2 146.81(13) 2_565 . ? O9 Nd O2 122.85(13) 1_545 . ? O22 Nd O29 146.71(13) 1_654 . ? O21 Nd O29 74.50(13) 2_565 . ? O9 Nd O29 75.63(13) 1_545 . ? O2 Nd O29 92.10(13) . . ? O22 Nd O26 74.01(13) 1_654 2_575 ? O21 Nd O26 72.42(12) 2_565 2_575 ? O9 Nd O26 144.35(14) 1_545 2_575 ? O2 Nd O26 74.63(13) . 2_575 ? O29 Nd O26 72.72(13) . 2_575 ? O22 Nd O30 72.42(14) 1_654 . ? O21 Nd O30 134.06(13) 2_565 . ? O9 Nd O30 76.38(14) 1_545 . ? O2 Nd O30 75.99(13) . . ? O29 Nd O30 136.35(13) . . ? O26 Nd O30 139.01(13) 2_575 . ? O22 Nd O1 124.90(14) 1_654 . ? O21 Nd O1 137.77(13) 2_565 . ? O9 Nd O1 72.35(12) 1_545 . ? O2 Nd O1 52.21(12) . . ? O29 Nd O1 66.22(14) . . ? O26 Nd O1 108.37(13) 2_575 . ? O30 Nd O1 73.73(14) . . ? O22 Nd O8 89.25(12) 1_654 1_545 ? O21 Nd O8 69.10(12) 2_565 1_545 ? O9 Nd O8 49.80(11) 1_545 1_545 ? O2 Nd O8 142.37(13) . 1_545 ? O29 Nd O8 115.71(12) . 1_545 ? O26 Nd O8 135.71(12) 2_575 1_545 ? O30 Nd O8 66.39(12) . 1_545 ? O1 Nd O8 114.69(12) . 1_545 ? O22 Nd C3 102.84(15) 1_654 . ? O21 Nd C3 148.54(14) 2_565 . ? O9 Nd C3 98.56(14) 1_545 . ? O2 Nd C3 26.09(14) . . ? O29 Nd C3 75.74(15) . . ? O26 Nd C3 89.22(14) 2_575 . ? O30 Nd C3 76.11(14) . . ? O1 Nd C3 26.44(13) . . ? O8 Nd C3 134.88(13) 1_545 . ? O22 Nd C7 113.59(14) 1_654 1_545 ? O21 Nd C7 73.97(14) 2_565 1_545 ? O9 Nd C7 24.72(13) 1_545 1_545 ? O2 Nd C7 138.41(14) . 1_545 ? O29 Nd C7 94.96(14) . 1_545 ? O26 Nd C7 146.20(14) 2_575 1_545 ? O30 Nd C7 70.78(14) . 1_545 ? O1 Nd C7 94.10(13) . 1_545 ? O8 Nd C7 25.14(13) 1_545 1_545 ? C3 Nd C7 118.79(15) . 1_545 ? C3 O1 Nd 89.7(3) . . ? C3 O2 Nd 95.5(3) . . ? O2 C3 O1 121.1(5) . . ? O2 C3 C4 119.4(5) . . ? O1 C3 C4 119.5(5) . . ? O2 C3 Nd 58.5(3) . . ? O1 C3 Nd 63.8(3) . . ? C4 C3 Nd 167.2(4) . . ? C12 C4 C5 122.3(5) . . ? C12 C4 C3 120.7(5) . . ? C5 C4 C3 117.0(5) . . ? C4 C5 C6 118.1(5) . . ? C4 C5 H5 121.0 . . ? C6 C5 H5 121.0 . . ? C10 C6 C5 120.3(5) . . ? C10 C6 C7 118.9(5) . . ? C5 C6 C7 120.6(5) . . ? O8 C7 O9 121.2(5) . . ? O8 C7 C6 122.7(5) . . ? O9 C7 C6 116.1(5) . . ? O8 C7 Nd 68.3(3) . 1_565 ? O9 C7 Nd 53.1(3) . 1_565 ? C6 C7 Nd 167.7(4) . 1_565 ? C7 O8 Nd 86.5(3) . 1_565 ? C7 O9 Nd 102.2(3) . 1_565 ? C6 C10 C11 120.4(5) . . ? C6 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? O13 C11 C12 124.7(5) . . ? O13 C11 C10 115.1(5) . . ? C12 C11 C10 120.2(5) . . ? C4 C12 C11 118.7(5) . . ? C4 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C11 O13 C14 116.0(4) . . ? O13 C14 C15 107.6(4) . . ? O13 C14 H14A 110.2 . . ? C15 C14 H14A 110.2 . . ? O13 C14 H14B 110.2 . . ? C15 C14 H14B 110.2 . . ? H14A C14 H14B 108.5 . . ? O16 C15 C14 103.1(4) . . ? O16 C15 H15A 111.1 . . ? C14 C15 H15A 111.1 . . ? O16 C15 H15B 111.1 . . ? C14 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? C17 O16 C15 118.7(4) . . ? O16 C17 C28 125.6(5) . . ? O16 C17 C18 114.2(5) . . ? C28 C17 C18 120.2(5) . . ? C19 C18 C17 120.1(5) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C23 120.7(5) . . ? C18 C19 C20 118.1(5) . . ? C23 C19 C20 121.1(5) . . ? O22 C20 O21 123.5(5) . . ? O22 C20 C19 118.2(5) . . ? O21 C20 C19 118.3(5) . . ? C20 O21 Nd 131.4(3) . 2_565 ? C20 O22 Nd 167.1(4) . 1_456 ? C24 C23 C19 118.2(5) . . ? C24 C23 H23 120.9 . . ? C19 C23 H23 120.9 . . ? C23 C24 C28 121.3(5) . . ? C23 C24 C25 121.1(5) . . ? C28 C24 C25 117.6(4) . . ? O26 C25 O27 123.4(5) . . ? O26 C25 C24 122.5(5) . . ? O27 C25 C24 114.1(4) . . ? C25 O26 Nd 143.5(4) . 2_575 ? C25 O27 H27 109.5 . . ? C17 C28 C24 119.5(5) . . ? C17 C28 H28 120.2 . . ? C24 C28 H28 120.2 . . ? Nd O29 H29A 111.8 . . ? Nd O29 H29B 124.8 . . ? H29A O29 H29B 112.6 . . ? Nd O30 H30A 116.2 . . ? Nd O30 H30B 112.0 . . ? H30A O30 H30B 113.1 . . ? H31A O31 H31B 116.4 . . ? H32A O32 H32B 113.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O27 H27 O8 0.84 1.84 2.658(5) 163 1_456 O29 H29A O33A 0.90 2.05 2.873(12) 150 1_554 O29 H29B O32 0.90 1.93 2.754(6) 151 2_565 O30 H30A O13 0.90 2.24 3.103(6) 161 2_675 O30 H30B O31 0.90 1.82 2.707(6) 168 2_665 O31 H31A O1 0.89 2.46 2.974(6) 117 . O31 H31B O33A 0.90 1.83 2.688(6) 159 1_554 O32 H32A O30 0.90 2.14 2.970(6) 153 2_665 O32 H32B O33B 0.90 2.12 2.817(7) 134 2_566 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.068 _refine_diff_density_min -2.017 _refine_diff_density_rms 0.203 #=====================END========================== data_10 _database_code_depnum_ccdc_archive 'CCDC 772540' #TrackingRef '- ka3-26-Ln.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H15 O12 Sm), 4(H2 O), 3(O)' _chemical_formula_sum 'C36 H38 O31 Sm2' _chemical_formula_weight 1267.36 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5589(2) _cell_length_b 9.9686(3) _cell_length_c 12.5240(4) _cell_angle_alpha 91.3986(13) _cell_angle_beta 94.9577(12) _cell_angle_gamma 93.4852(11) _cell_volume 1062.11(5) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3640 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 27.83 _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.981 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 626 _exptl_absorpt_coefficient_mu 2.848 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3955 _exptl_absorpt_correction_T_max 0.5997 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10883 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.83 _reflns_number_total 4966 _reflns_number_gt 4221 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Atoms O33a and O33b represent disordered water solvent trapped within the layered coordination polymers. ; _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^)+(0.0815P)^2^+1.1382P] 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 4966 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1097 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.904 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm Sm 0.40285(3) 0.60437(2) -0.322458(18) 0.01258(10) Uani 1 1 d . . . O1 O 0.3603(4) 0.7348(3) -0.1518(3) 0.0194(7) Uani 1 1 d . . . O2 O 0.4726(4) 0.8397(3) -0.2810(3) 0.0167(7) Uani 1 1 d . . . C3 C 0.4076(6) 0.8419(5) -0.1944(4) 0.0142(9) Uani 1 1 d . . . C4 C 0.3795(5) 0.9756(5) -0.1444(4) 0.0137(9) Uani 1 1 d . . . C5 C 0.4212(5) 1.0912(4) -0.1984(4) 0.0135(9) Uani 1 1 d . . . H5 H 0.4709 1.0851 -0.2632 0.016 Uiso 1 1 calc R . . C6 C 0.3890(5) 1.2155(5) -0.1558(4) 0.0131(9) Uani 1 1 d . . . C7 C 0.4180(6) 1.3417(4) -0.2164(4) 0.0137(9) Uani 1 1 d . . . O8 O 0.5084(4) 1.3488(3) -0.2911(3) 0.0147(7) Uani 1 1 d . . . O9 O 0.3434(4) 1.4426(3) -0.1906(3) 0.0169(7) Uani 1 1 d . . . C10 C 0.3194(6) 1.2245(5) -0.0601(4) 0.0153(9) Uani 1 1 d . . . H10 H 0.2975 1.3099 -0.0316 0.018 Uiso 1 1 calc R . . C11 C 0.2814(6) 1.1080(5) -0.0057(4) 0.0161(10) Uani 1 1 d . . . C12 C 0.3111(5) 0.9821(5) -0.0476(4) 0.0137(9) Uani 1 1 d . . . H12 H 0.2853 0.9026 -0.0109 0.016 Uiso 1 1 calc R . . O13 O 0.2136(4) 1.1288(3) 0.0896(3) 0.0193(7) Uani 1 1 d . . . C14 C 0.1574(6) 1.0108(5) 0.1396(4) 0.0166(10) Uani 1 1 d . . . H14A H 0.2466 0.9599 0.1685 0.020 Uiso 1 1 calc R . . H14B H 0.0903 0.9521 0.0870 0.020 Uiso 1 1 calc R . . C15 C 0.0637(6) 1.0553(5) 0.2290(4) 0.0155(9) Uani 1 1 d . . . H15A H 0.1301 1.1121 0.2832 0.019 Uiso 1 1 calc R . . H15B H -0.0263 1.1061 0.2012 0.019 Uiso 1 1 calc R . . O16 O 0.0108(4) 0.9304(3) 0.2736(3) 0.0176(7) Uani 1 1 d . . . C17 C -0.0882(5) 0.9327(5) 0.3541(4) 0.0135(9) Uani 1 1 d . . . C18 C -0.1372(5) 0.8065(4) 0.3883(4) 0.0135(9) Uani 1 1 d . . . H18 H -0.0992 0.7279 0.3580 0.016 Uiso 1 1 calc R . . C19 C -0.2425(5) 0.7957(4) 0.4672(4) 0.0129(9) Uani 1 1 d . . . C20 C -0.3032(5) 0.6563(4) 0.4960(4) 0.0116(9) Uani 1 1 d . . . O21 O -0.2616(4) 0.5573(3) 0.4425(3) 0.0155(7) Uani 1 1 d . . . O22 O -0.3928(4) 0.6459(3) 0.5696(3) 0.0180(7) Uani 1 1 d . . . C23 C -0.2936(5) 0.9107(4) 0.5154(4) 0.0124(9) Uani 1 1 d . . . H23 H -0.3618 0.9037 0.5712 0.015 Uiso 1 1 calc R . . C24 C -0.2427(5) 1.0365(4) 0.4799(4) 0.0114(9) Uani 1 1 d . . . C25 C -0.2964(5) 1.1633(4) 0.5261(4) 0.0123(9) Uani 1 1 d . . . O26 O -0.2874(4) 1.2712(3) 0.4810(3) 0.0186(7) Uani 1 1 d . . . O27 O -0.3501(4) 1.1494(3) 0.6209(3) 0.0169(7) Uani 1 1 d . . . H27 H -0.3985 1.2172 0.6361 0.025 Uiso 1 1 calc R . . C28 C -0.1411(5) 1.0482(5) 0.3981(4) 0.0139(9) Uani 1 1 d . . . H28 H -0.1091 1.1341 0.3734 0.017 Uiso 1 1 calc R . . O29 O 0.1221(4) 0.6312(3) -0.2965(3) 0.0187(7) Uani 1 1 d . . . H29A H 0.1070 0.6448 -0.2269 0.028 Uiso 1 1 d R . . H29B H 0.0405 0.5847 -0.3332 0.028 Uiso 1 1 d R . . O30 O 0.6572(4) 0.6023(3) -0.2034(3) 0.0190(7) Uani 1 1 d . . . H30A H 0.7058 0.6828 -0.1848 0.028 Uiso 1 1 d R . . H30B H 0.6477 0.5490 -0.1474 0.028 Uiso 1 1 d R . . O31 O 0.3270(6) 0.5673(4) 0.0386(4) 0.0398(11) Uani 1 1 d . . . H31A H 0.4092 0.6140 0.0157 0.060 Uiso 1 1 d R . . H31B H 0.2436 0.5503 -0.0096 0.060 Uiso 1 1 d R . . O32 O 0.1386(4) 0.5453(4) 0.3403(3) 0.0230(8) Uani 1 1 d . . . H32A H 0.1828 0.4774 0.3080 0.035 Uiso 1 1 d R . . H32B H 0.0651 0.5826 0.2972 0.035 Uiso 1 1 d R . . O33A O 0.0474(11) 0.5748(9) 0.9180(7) 0.037(2) Uiso 0.75 1 d P A 1 O33B O -0.0760(14) 0.3142(12) 0.8461(10) 0.040(3) Uiso 0.75 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm 0.01660(15) 0.00887(13) 0.01290(14) -0.00011(9) 0.00486(9) 0.00091(8) O1 0.035(2) 0.0100(15) 0.0149(17) 0.0015(13) 0.0116(15) 0.0001(14) O2 0.0236(18) 0.0111(15) 0.0169(17) 0.0021(13) 0.0081(14) 0.0038(13) C3 0.018(2) 0.012(2) 0.012(2) -0.0026(18) 0.0006(18) -0.0006(17) C4 0.013(2) 0.013(2) 0.015(2) -0.0011(18) 0.0024(18) -0.0010(16) C5 0.014(2) 0.013(2) 0.013(2) -0.0026(18) 0.0031(17) 0.0008(17) C6 0.014(2) 0.014(2) 0.011(2) 0.0005(18) 0.0036(17) -0.0004(17) C7 0.018(2) 0.011(2) 0.012(2) 0.0005(17) 0.0014(18) 0.0004(17) O8 0.0180(17) 0.0127(15) 0.0136(16) 0.0007(13) 0.0032(13) 0.0003(12) O9 0.0236(19) 0.0108(15) 0.0176(17) -0.0004(13) 0.0077(14) 0.0032(13) C10 0.020(2) 0.011(2) 0.016(2) 0.0015(18) 0.0046(19) 0.0044(17) C11 0.017(2) 0.016(2) 0.016(2) 0.0015(19) 0.0074(19) 0.0026(18) C12 0.015(2) 0.012(2) 0.014(2) 0.0038(18) 0.0022(18) -0.0027(16) O13 0.028(2) 0.0159(17) 0.0158(17) 0.0025(14) 0.0132(15) 0.0019(14) C14 0.020(2) 0.018(2) 0.013(2) 0.0043(19) 0.0085(19) 0.0026(18) C15 0.020(2) 0.013(2) 0.014(2) 0.0008(18) 0.0080(19) -0.0022(17) O16 0.0246(19) 0.0100(15) 0.0196(18) -0.0010(13) 0.0124(14) -0.0009(13) C17 0.013(2) 0.019(2) 0.010(2) 0.0007(18) 0.0055(17) 0.0008(17) C18 0.018(2) 0.011(2) 0.011(2) -0.0012(17) 0.0000(18) 0.0036(17) C19 0.016(2) 0.009(2) 0.013(2) -0.0023(17) 0.0017(17) 0.0006(16) C20 0.013(2) 0.012(2) 0.010(2) 0.0002(17) -0.0005(17) 0.0014(16) O21 0.0212(18) 0.0090(15) 0.0169(17) -0.0015(13) 0.0052(14) 0.0010(12) O22 0.0202(18) 0.0142(16) 0.0206(18) 0.0002(14) 0.0092(14) -0.0007(13) C23 0.014(2) 0.013(2) 0.011(2) -0.0009(17) 0.0026(17) -0.0009(16) C24 0.013(2) 0.0081(19) 0.012(2) -0.0014(17) -0.0016(17) 0.0001(16) C25 0.010(2) 0.010(2) 0.017(2) -0.0009(17) 0.0015(17) -0.0011(15) O26 0.029(2) 0.0093(15) 0.0183(18) 0.0002(13) 0.0024(15) 0.0030(13) O27 0.0225(18) 0.0146(16) 0.0159(17) 0.0015(14) 0.0098(14) 0.0065(13) C28 0.015(2) 0.012(2) 0.014(2) 0.0029(18) -0.0005(17) -0.0010(16) O29 0.0172(17) 0.0186(17) 0.0218(18) 0.0006(14) 0.0090(14) 0.0016(13) O30 0.0203(18) 0.0194(17) 0.0169(17) -0.0004(14) 0.0019(14) -0.0016(14) O31 0.055(3) 0.029(2) 0.031(2) 0.0083(19) -0.012(2) -0.011(2) O32 0.0228(19) 0.0248(19) 0.0212(19) -0.0010(15) -0.0016(15) 0.0041(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm O22 2.325(3) 1_654 ? Sm O21 2.377(3) 2_565 ? Sm O9 2.400(3) 1_545 ? Sm O2 2.418(3) . ? Sm O29 2.482(3) . ? Sm O26 2.527(4) 2_575 ? Sm O30 2.532(3) . ? Sm O1 2.539(3) . ? Sm O8 2.780(3) 1_545 ? Sm C3 2.824(4) . ? Sm C7 2.970(5) 1_545 ? O1 C3 1.265(6) . ? O2 C3 1.262(6) . ? C3 C4 1.500(6) . ? C4 C12 1.393(6) . ? C4 C5 1.393(7) . ? C5 C6 1.389(6) . ? C5 H5 0.9500 . ? C6 C10 1.388(7) . ? C6 C7 1.504(6) . ? C7 O8 1.265(6) . ? C7 O9 1.273(5) . ? C7 Sm 2.969(5) 1_565 ? O8 Sm 2.780(3) 1_565 ? O9 Sm 2.400(3) 1_565 ? C10 C11 1.396(7) . ? C10 H10 0.9500 . ? C11 O13 1.388(6) . ? C11 C12 1.394(6) . ? C12 H12 0.9500 . ? O13 C14 1.423(6) . ? C14 C15 1.506(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O16 1.441(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O16 C17 1.373(5) . ? C17 C28 1.382(6) . ? C17 C18 1.391(6) . ? C18 C19 1.396(7) . ? C18 H18 0.9500 . ? C19 C23 1.393(6) . ? C19 C20 1.517(6) . ? C20 O22 1.251(6) . ? C20 O21 1.266(5) . ? O21 Sm 2.377(3) 2_565 ? O22 Sm 2.325(3) 1_456 ? C23 C24 1.398(6) . ? C23 H23 0.9500 . ? C24 C28 1.402(7) . ? C24 C25 1.492(6) . ? C25 O26 1.229(6) . ? C25 O27 1.317(6) . ? O26 Sm 2.527(4) 2_575 ? O27 H27 0.8400 . ? C28 H28 0.9500 . ? O29 H29A 0.9001 . ? O29 H29B 0.8993 . ? O30 H30A 0.8969 . ? O30 H30B 0.8958 . ? O31 H31A 0.8913 . ? O31 H31B 0.8982 . ? O32 H32A 0.8996 . ? O32 H32B 0.8975 . ? 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 O22 Sm O21 95.19(12) 1_654 2_565 ? O22 Sm O9 135.55(12) 1_654 1_545 ? O21 Sm O9 83.21(12) 2_565 1_545 ? O22 Sm O2 78.59(11) 1_654 . ? O21 Sm O2 146.90(12) 2_565 . ? O9 Sm O2 123.86(11) 1_545 . ? O22 Sm O29 146.73(13) 1_654 . ? O21 Sm O29 75.13(11) 2_565 . ? O9 Sm O29 75.79(12) 1_545 . ? O2 Sm O29 92.28(11) . . ? O22 Sm O26 74.14(12) 1_654 2_575 ? O21 Sm O26 72.50(11) 2_565 2_575 ? O9 Sm O26 144.01(12) 1_545 2_575 ? O2 Sm O26 74.54(11) . 2_575 ? O29 Sm O26 72.60(12) . 2_575 ? O22 Sm O30 72.77(12) 1_654 . ? O21 Sm O30 133.37(11) 2_565 . ? O9 Sm O30 76.52(12) 1_545 . ? O2 Sm O30 76.22(11) . . ? O29 Sm O30 136.39(12) . . ? O26 Sm O30 139.28(12) 2_575 . ? O22 Sm O1 125.90(11) 1_654 . ? O21 Sm O1 138.22(12) 2_565 . ? O9 Sm O1 72.81(11) 1_545 . ? O2 Sm O1 52.77(11) . . ? O29 Sm O1 66.19(12) . . ? O26 Sm O1 108.59(11) 2_575 . ? O30 Sm O1 73.79(12) . . ? O22 Sm O8 88.22(11) 1_654 1_545 ? O21 Sm O8 68.66(10) 2_565 1_545 ? O9 Sm O8 49.73(10) 1_545 1_545 ? O2 Sm O8 142.32(11) . 1_545 ? O29 Sm O8 116.11(11) . 1_545 ? O26 Sm O8 135.39(10) 2_575 1_545 ? O30 Sm O8 66.15(10) . 1_545 ? O1 Sm O8 114.82(10) . 1_545 ? O22 Sm C3 103.63(13) 1_654 . ? O21 Sm C3 149.38(12) 2_565 . ? O9 Sm C3 99.16(13) 1_545 . ? O2 Sm C3 26.43(13) . . ? O29 Sm C3 75.92(12) . . ? O26 Sm C3 89.50(12) 2_575 . ? O30 Sm C3 76.02(12) . . ? O1 Sm C3 26.62(12) . . ? O8 Sm C3 134.87(12) 1_545 . ? O22 Sm C7 112.69(12) 1_654 1_545 ? O21 Sm C7 73.56(12) 2_565 1_545 ? O9 Sm C7 24.63(12) 1_545 1_545 ? O2 Sm C7 138.95(12) . 1_545 ? O29 Sm C7 95.28(12) . 1_545 ? O26 Sm C7 145.87(12) 2_575 1_545 ? O30 Sm C7 70.63(12) . 1_545 ? O1 Sm C7 94.31(12) . 1_545 ? O8 Sm C7 25.15(11) 1_545 1_545 ? C3 Sm C7 119.05(13) . 1_545 ? C3 O1 Sm 89.3(3) . . ? C3 O2 Sm 95.0(3) . . ? O2 C3 O1 121.6(4) . . ? O2 C3 C4 118.6(4) . . ? O1 C3 C4 119.8(4) . . ? O2 C3 Sm 58.5(2) . . ? O1 C3 Sm 64.0(2) . . ? C4 C3 Sm 166.8(3) . . ? C12 C4 C5 121.7(4) . . ? C12 C4 C3 120.2(4) . . ? C5 C4 C3 118.1(4) . . ? C4 C5 C6 118.8(4) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C10 C6 C5 120.6(4) . . ? C10 C6 C7 118.6(4) . . ? C5 C6 C7 120.7(4) . . ? O8 C7 O9 120.6(4) . . ? O8 C7 C6 122.8(4) . . ? O9 C7 C6 116.6(4) . . ? O8 C7 Sm 69.0(2) . 1_565 ? O9 C7 Sm 51.8(2) . 1_565 ? C6 C7 Sm 166.9(3) . 1_565 ? C7 O8 Sm 85.8(3) . 1_565 ? C7 O9 Sm 103.6(3) . 1_565 ? C6 C10 C11 119.9(4) . . ? C6 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? O13 C11 C12 124.5(4) . . ? O13 C11 C10 115.1(4) . . ? C12 C11 C10 120.5(4) . . ? C4 C12 C11 118.5(4) . . ? C4 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C11 O13 C14 115.8(4) . . ? O13 C14 C15 107.3(4) . . ? O13 C14 H14A 110.3 . . ? C15 C14 H14A 110.3 . . ? O13 C14 H14B 110.3 . . ? C15 C14 H14B 110.3 . . ? H14A C14 H14B 108.5 . . ? O16 C15 C14 103.3(4) . . ? O16 C15 H15A 111.1 . . ? C14 C15 H15A 111.1 . . ? O16 C15 H15B 111.1 . . ? C14 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? C17 O16 C15 119.2(3) . . ? O16 C17 C28 124.6(4) . . ? O16 C17 C18 114.6(4) . . ? C28 C17 C18 120.9(4) . . ? C19 C18 C17 119.8(4) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C23 120.4(4) . . ? C18 C19 C20 118.3(4) . . ? C23 C19 C20 121.3(4) . . ? O22 C20 O21 123.9(4) . . ? O22 C20 C19 118.5(4) . . ? O21 C20 C19 117.6(4) . . ? C20 O21 Sm 132.8(3) . 2_565 ? C20 O22 Sm 167.6(3) . 1_456 ? C24 C23 C19 118.7(4) . . ? C24 C23 H23 120.6 . . ? C19 C23 H23 120.6 . . ? C23 C24 C28 121.2(4) . . ? C23 C24 C25 121.4(4) . . ? C28 C24 C25 117.4(4) . . ? O26 C25 O27 123.3(4) . . ? O26 C25 C24 122.9(4) . . ? O27 C25 C24 113.7(4) . . ? C25 O26 Sm 142.8(3) . 2_575 ? C25 O27 H27 109.5 . . ? C17 C28 C24 118.9(4) . . ? C17 C28 H28 120.6 . . ? C24 C28 H28 120.6 . . ? Sm O29 H29A 111.8 . . ? Sm O29 H29B 125.0 . . ? H29A O29 H29B 112.7 . . ? Sm O30 H30A 116.2 . . ? Sm O30 H30B 112.0 . . ? H30A O30 H30B 113.0 . . ? H31A O31 H31B 116.4 . . ? H32A O32 H32B 113.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O27 H27 O8 0.84 1.84 2.655(4) 163 1_456 O29 H29A O33A 0.90 2.05 2.876(10) 151 1_554 O29 H29B O32 0.90 1.94 2.764(5) 151 2_565 O30 H30A O13 0.90 2.24 3.102(5) 161 2_675 O30 H30B O31 0.90 1.82 2.700(6) 167 2_665 O31 H31A O1 0.89 2.46 2.968(6) 116 . O31 H31B O33A 0.90 1.87 2.722(8) 157 1_554 O32 H32A O30 0.90 2.15 2.978(5) 153 2_665 O32 H32B O33B 0.90 2.10 2.781(13) 132 2_566 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.83 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.825 _refine_diff_density_min -1.564 _refine_diff_density_rms 0.184 #===================END========================== data_11 _database_code_depnum_ccdc_archive 'CCDC 772541' #TrackingRef '- ka3-26-Ln.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H15 Ce O12, H2 O' _chemical_formula_sum 'C18 H17 Ce O13' _chemical_formula_weight 581.44 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0901(3) _cell_length_b 10.1509(4) _cell_length_c 14.6134(7) _cell_angle_alpha 82.8401(18) _cell_angle_beta 88.141(2) _cell_angle_gamma 66.521(3) _cell_volume 1091.94(8) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4203 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.50 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 574 _exptl_absorpt_coefficient_mu 2.150 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6155 _exptl_absorpt_correction_T_max 0.8137 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13557 _diffrn_reflns_av_R_equivalents 0.0790 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 26.50 _reflns_number_total 4472 _reflns_number_gt 3728 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains also additional molecules of the water solvent in intermolecular voids, which could not be reliably modeled by discrete atoms. The contribution of these molecules to the diffraction pattern was thus subtracted by the Squeeze procedure, using the PLATON software (Spek, 2003). ; _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^)+(0.0484P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4472 _refine_ls_number_parameters 289 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce Ce -0.37853(4) 0.56670(3) 0.675511(19) 0.01385(10) Uani 1 1 d . . . O1 O -0.2484(4) 0.4065(3) 0.5468(2) 0.0145(7) Uani 1 1 d . . . O2 O -0.3896(4) 0.3416(4) 0.4435(2) 0.0189(8) Uani 1 1 d . . . C3 C -0.2877(6) 0.3145(5) 0.5137(3) 0.0166(10) Uani 1 1 d . . . C4 C -0.2093(6) 0.1595(5) 0.5590(3) 0.0133(10) Uani 1 1 d . . . C5 C -0.2483(6) 0.0544(5) 0.5226(3) 0.0152(10) Uani 1 1 d . . . H5 H -0.3197 0.0782 0.4679 0.018 Uiso 1 1 calc R . . C6 C -0.1805(6) -0.0864(5) 0.5682(3) 0.0161(10) Uani 1 1 d . . . C7 C -0.2194(6) -0.2011(5) 0.5325(3) 0.0151(10) Uani 1 1 d . . . O8 O -0.2013(4) -0.3158(4) 0.5796(2) 0.0175(7) Uani 1 1 d . . . O9 O -0.2718(5) -0.1732(4) 0.4457(2) 0.0236(8) Uani 1 1 d D . . H9 H -0.2671 -0.2571 0.4293 0.035 Uiso 1 1 d RD . . C10 C -0.0721(6) -0.1234(5) 0.6468(3) 0.0148(10) Uani 1 1 d . . . H10 H -0.0272 -0.2194 0.6774 0.018 Uiso 1 1 calc R . . C11 C -0.0300(6) -0.0170(5) 0.6801(3) 0.0141(10) Uani 1 1 d . . . C12 C -0.0965(6) 0.1241(5) 0.6367(3) 0.0150(10) Uani 1 1 d . . . H12 H -0.0659 0.1954 0.6594 0.018 Uiso 1 1 calc R . . O13 O 0.0783(4) -0.0654(4) 0.7589(2) 0.0171(7) Uani 1 1 d . . . C14 C 0.1174(7) 0.0384(5) 0.8026(3) 0.0181(11) Uani 1 1 d . . . H14A H 0.0068 0.1263 0.8080 0.022 Uiso 1 1 calc R . . H14B H 0.2075 0.0664 0.7674 0.022 Uiso 1 1 calc R . . C15 C 0.1920(6) -0.0403(5) 0.8972(3) 0.0141(10) Uani 1 1 d . . . H15A H 0.1033 -0.0721 0.9306 0.017 Uiso 1 1 calc R . . H15B H 0.3043 -0.1265 0.8912 0.017 Uiso 1 1 calc R . . O16 O 0.2271(5) 0.0595(4) 0.9455(2) 0.0184(8) Uani 1 1 d . . . C17 C 0.2900(6) 0.0123(5) 1.0354(3) 0.0173(10) Uani 1 1 d . . . C18 C 0.3247(6) -0.1268(5) 1.0784(3) 0.0171(10) Uani 1 1 d . . . H18 H 0.3063 -0.1955 1.0460 0.021 Uiso 1 1 calc R . . C19 C 0.3876(6) -0.1636(5) 1.1708(3) 0.0167(10) Uani 1 1 d . . . C20 C 0.4020(6) -0.3084(5) 1.2176(3) 0.0145(10) Uani 1 1 d . . . O21 O 0.4732(5) -0.3527(4) 1.2978(2) 0.0179(7) Uani 1 1 d . . . O22 O 0.3372(5) -0.3815(4) 1.1785(2) 0.0183(7) Uani 1 1 d . . . C23 C 0.4151(6) -0.0631(5) 1.2186(3) 0.0131(10) Uani 1 1 d . . . H23 H 0.4601 -0.0895 1.2804 0.016 Uiso 1 1 calc R . . C24 C 0.3760(6) 0.0759(5) 1.1750(3) 0.0151(10) Uani 1 1 d . . . C25 C 0.3901(6) 0.1917(5) 1.2258(3) 0.0146(10) Uani 1 1 d . . . O26 O 0.4879(5) 0.1583(4) 1.2969(2) 0.0192(8) Uani 1 1 d . . . O27 O 0.2971(5) 0.3239(4) 1.1957(2) 0.0215(8) Uani 1 1 d . . . C28 C 0.3102(6) 0.1153(5) 1.0840(3) 0.0144(10) Uani 1 1 d . . . H28 H 0.2794 0.2115 1.0554 0.017 Uiso 1 1 calc R . . O29 O -0.0489(4) 0.4179(4) 0.7146(2) 0.0203(8) Uani 1 1 d D . . H29A H -0.1137 0.5087 0.7271 0.030 Uiso 1 1 d RD . . H29B H 0.0355 0.4128 0.6719 0.030 Uiso 1 1 d RD . . O30 O -0.6675(5) 0.6474(4) 0.7640(3) 0.0233(8) Uani 1 1 d D . . H30A H -0.6868 0.5859 0.8109 0.035 Uiso 1 1 d RD . . H30B H -0.7520 0.7385 0.7556 0.035 Uiso 1 1 d RD . . O31 O 0.2323(4) 0.4117(4) 0.6057(2) 0.0179(7) Uani 1 1 d . . . H31A H 0.2375 0.4711 0.5557 0.027 Uiso 1 1 d R . . H31B H 0.3334 0.3911 0.6390 0.027 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce 0.02002(16) 0.00953(15) 0.01292(15) -0.00086(9) -0.00272(10) -0.00676(11) O1 0.0227(17) 0.0072(17) 0.0147(17) -0.0022(13) -0.0032(14) -0.0068(14) O2 0.0239(18) 0.0127(18) 0.0188(18) 0.0010(14) -0.0071(15) -0.0061(15) C3 0.015(2) 0.012(3) 0.018(3) 0.000(2) -0.002(2) -0.001(2) C4 0.008(2) 0.014(3) 0.014(2) -0.0031(19) 0.0024(18) 0.0003(18) C5 0.016(2) 0.014(3) 0.015(2) -0.0042(19) 0.0013(19) -0.0039(19) C6 0.015(2) 0.014(3) 0.019(3) -0.002(2) 0.001(2) -0.006(2) C7 0.012(2) 0.015(3) 0.017(3) -0.005(2) 0.0000(19) -0.0025(19) O8 0.0239(18) 0.0119(18) 0.0176(18) -0.0014(14) 0.0008(14) -0.0083(14) O9 0.041(2) 0.018(2) 0.0183(19) 0.0002(15) -0.0081(16) -0.0183(17) C10 0.018(2) 0.011(2) 0.016(2) -0.0002(19) 0.0015(19) -0.0058(19) C11 0.014(2) 0.017(3) 0.012(2) 0.0009(19) -0.0005(18) -0.0077(19) C12 0.018(2) 0.014(3) 0.013(2) -0.0031(19) -0.0004(19) -0.007(2) O13 0.0232(18) 0.0108(18) 0.0173(18) -0.0028(14) -0.0043(14) -0.0060(14) C14 0.025(3) 0.011(3) 0.020(3) 0.000(2) -0.003(2) -0.009(2) C15 0.018(2) 0.014(3) 0.013(2) -0.0035(19) -0.0040(19) -0.008(2) O16 0.0324(19) 0.0134(18) 0.0119(17) 0.0027(14) -0.0078(14) -0.0123(15) C17 0.018(2) 0.017(3) 0.017(3) -0.003(2) -0.001(2) -0.008(2) C18 0.022(3) 0.014(3) 0.017(3) 0.001(2) -0.002(2) -0.010(2) C19 0.016(2) 0.014(3) 0.020(3) -0.004(2) 0.000(2) -0.005(2) C20 0.014(2) 0.012(2) 0.016(2) -0.0072(19) 0.0025(19) -0.0021(19) O21 0.0292(19) 0.0128(18) 0.0156(18) 0.0047(14) -0.0083(15) -0.0138(15) O22 0.0269(19) 0.0126(18) 0.0179(18) 0.0007(14) -0.0045(15) -0.0107(15) C23 0.012(2) 0.012(2) 0.013(2) -0.0020(19) 0.0010(18) -0.0023(19) C24 0.015(2) 0.014(3) 0.019(3) -0.007(2) 0.0005(19) -0.008(2) C25 0.016(2) 0.016(3) 0.014(2) -0.0015(19) 0.0039(19) -0.008(2) O26 0.0286(19) 0.0135(18) 0.0158(18) 0.0015(14) -0.0076(15) -0.0092(15) O27 0.034(2) 0.0116(18) 0.0193(19) 0.0013(14) -0.0101(16) -0.0103(16) C28 0.016(2) 0.012(3) 0.015(2) 0.0022(19) -0.0018(19) -0.0053(19) O29 0.0226(18) 0.0162(19) 0.0180(18) -0.0024(14) 0.0022(14) -0.0035(15) O30 0.0215(18) 0.0101(18) 0.033(2) -0.0025(15) 0.0027(16) -0.0010(14) O31 0.0235(18) 0.0171(19) 0.0165(18) -0.0017(14) -0.0033(14) -0.0114(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce O2 2.414(3) 2_466 ? Ce O8 2.502(3) 1_565 ? Ce O27 2.528(3) 2_567 ? Ce O29 2.528(3) . ? Ce O30 2.520(4) . ? Ce O21 2.560(3) 2_557 ? Ce O1 2.562(3) . ? Ce O22 2.596(3) 2_557 ? Ce O26 2.651(3) 2_567 ? Ce C20 2.951(5) 2_557 ? Ce C25 2.966(5) 2_567 ? Ce H29A 2.1196 . ? O1 C3 1.252(6) . ? O2 C3 1.269(6) . ? O2 Ce 2.414(3) 2_466 ? C3 C4 1.513(6) . ? C4 C5 1.393(7) . ? C4 C12 1.398(6) . ? C5 C6 1.396(7) . ? C5 H5 0.9500 . ? C6 C10 1.387(7) . ? C6 C7 1.477(7) . ? C7 O8 1.233(6) . ? C7 O9 1.311(6) . ? O8 Ce 2.502(3) 1_545 ? O9 H9 0.8997 . ? C10 C11 1.397(7) . ? C10 H10 0.9500 . ? C11 O13 1.385(5) . ? C11 C12 1.387(7) . ? C12 H12 0.9500 . ? O13 C14 1.436(6) . ? C14 C15 1.519(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O16 1.423(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O16 C17 1.381(6) . ? C17 C18 1.393(7) . ? C17 C28 1.398(7) . ? C18 C19 1.411(7) . ? C18 H18 0.9500 . ? C19 C23 1.395(7) . ? C19 C20 1.503(7) . ? C20 O22 1.259(6) . ? C20 O21 1.271(5) . ? C20 Ce 2.951(5) 2_557 ? O21 Ce 2.560(3) 2_557 ? O22 Ce 2.596(3) 2_557 ? C23 C24 1.390(7) . ? C23 H23 0.9500 . ? C24 C28 1.398(6) . ? C24 C25 1.508(7) . ? C25 O26 1.254(6) . ? C25 O27 1.277(6) . ? C25 Ce 2.966(5) 2_567 ? O26 Ce 2.651(3) 2_567 ? O27 Ce 2.528(3) 2_567 ? C28 H28 0.9500 . ? O29 H29A 0.8992 . ? O29 H29B 0.8998 . ? O30 H30A 0.9214 . ? O30 H30B 0.9008 . ? O31 H31A 0.8981 . ? O31 H31B 0.9019 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ce O8 89.22(11) 2_466 1_565 ? O2 Ce O27 133.93(11) 2_466 2_567 ? O8 Ce O27 83.44(11) 1_565 2_567 ? O2 Ce O29 146.24(12) 2_466 . ? O8 Ce O29 72.70(11) 1_565 . ? O27 Ce O29 73.31(11) 2_567 . ? O2 Ce O30 76.25(12) 2_466 . ? O8 Ce O30 137.05(11) 1_565 . ? O27 Ce O30 78.79(12) 2_567 . ? O29 Ce O30 135.88(11) . . ? O2 Ce O21 84.33(11) 2_466 2_557 ? O8 Ce O21 146.68(11) 1_565 2_557 ? O27 Ce O21 123.63(11) 2_567 2_557 ? O29 Ce O21 95.27(11) . 2_557 ? O30 Ce O21 72.70(11) . 2_557 ? O2 Ce O1 75.21(11) 2_466 . ? O8 Ce O1 75.11(11) 1_565 . ? O27 Ce O1 143.88(11) 2_567 . ? O29 Ce O1 72.71(11) . . ? O30 Ce O1 135.88(11) . . ? O21 Ce O1 71.62(11) 2_557 . ? O2 Ce O22 130.28(11) 2_466 2_557 ? O8 Ce O22 139.49(10) 1_565 2_557 ? O27 Ce O22 74.80(11) 2_567 2_557 ? O29 Ce O22 68.51(11) . 2_557 ? O30 Ce O22 71.62(11) . 2_557 ? O21 Ce O22 50.50(10) 2_557 2_557 ? O1 Ce O22 103.45(10) . 2_557 ? O2 Ce O26 84.54(11) 2_466 2_567 ? O8 Ce O26 69.68(11) 1_565 2_567 ? O27 Ce O26 50.29(10) 2_567 2_567 ? O29 Ce O26 113.80(11) . 2_567 ? O30 Ce O26 68.86(11) . 2_567 ? O21 Ce O26 141.49(11) 2_557 2_567 ? O1 Ce O26 139.37(10) . 2_567 ? O22 Ce O26 116.39(11) 2_557 2_567 ? O2 Ce C20 108.40(12) 2_466 2_557 ? O8 Ce C20 150.20(12) 1_565 2_557 ? O27 Ce C20 99.60(12) 2_567 2_557 ? O29 Ce C20 79.77(12) . 2_557 ? O30 Ce C20 71.92(12) . 2_557 ? O21 Ce C20 25.41(11) 2_557 2_557 ? O1 Ce C20 86.13(12) . 2_557 ? O22 Ce C20 25.21(12) 2_557 2_557 ? O26 Ce C20 134.10(12) 2_567 2_557 ? O2 Ce C25 109.29(12) 2_466 2_567 ? O8 Ce C25 74.49(12) 1_565 2_567 ? O27 Ce C25 25.30(12) 2_567 2_567 ? O29 Ce C25 93.38(12) . 2_567 ? O30 Ce C25 72.83(12) . 2_567 ? O21 Ce C25 138.30(12) 2_557 2_567 ? O1 Ce C25 149.18(11) . 2_567 ? O22 Ce C25 96.31(12) 2_557 2_567 ? O26 Ce C25 25.00(11) 2_567 2_567 ? C20 Ce C25 119.08(13) 2_557 2_567 ? O2 Ce H29A 153.9 2_466 . ? O8 Ce H29A 66.1 1_565 . ? O27 Ce H29A 54.9 2_567 . ? O29 Ce H29A 19.9 . . ? O30 Ce H29A 127.5 . . ? O21 Ce H29A 111.3 2_557 . ? O1 Ce H29A 89.6 . . ? O22 Ce H29A 73.4 2_557 . ? O26 Ce H29A 94.1 2_567 . ? C20 Ce H29A 91.2 2_557 . ? C25 Ce H29A 73.5 2_567 . ? C3 O1 Ce 134.0(3) . . ? C3 O2 Ce 168.8(3) . 2_466 ? O1 C3 O2 124.5(4) . . ? O1 C3 C4 118.8(4) . . ? O2 C3 C4 116.8(4) . . ? C5 C4 C12 121.1(4) . . ? C5 C4 C3 119.9(4) . . ? C12 C4 C3 118.9(4) . . ? C4 C5 C6 118.7(4) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C10 C6 C5 121.3(5) . . ? C10 C6 C7 118.1(4) . . ? C5 C6 C7 120.6(4) . . ? O8 C7 O9 122.1(4) . . ? O8 C7 C6 123.1(4) . . ? O9 C7 C6 114.7(4) . . ? C7 O8 Ce 141.3(3) . 1_545 ? C7 O9 H9 105.9 . . ? C6 C10 C11 118.9(4) . . ? C6 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? O13 C11 C12 124.7(4) . . ? O13 C11 C10 114.1(4) . . ? C12 C11 C10 121.2(4) . . ? C11 C12 C4 118.8(4) . . ? C11 C12 H12 120.6 . . ? C4 C12 H12 120.6 . . ? C11 O13 C14 118.3(4) . . ? O13 C14 C15 104.0(4) . . ? O13 C14 H14A 111.0 . . ? C15 C14 H14A 111.0 . . ? O13 C14 H14B 111.0 . . ? C15 C14 H14B 111.0 . . ? H14A C14 H14B 109.0 . . ? O16 C15 C14 106.7(4) . . ? O16 C15 H15A 110.4 . . ? C14 C15 H15A 110.4 . . ? O16 C15 H15B 110.4 . . ? C14 C15 H15B 110.4 . . ? H15A C15 H15B 108.6 . . ? C17 O16 C15 116.8(4) . . ? O16 C17 C18 123.4(4) . . ? O16 C17 C28 115.9(4) . . ? C18 C17 C28 120.6(4) . . ? C17 C18 C19 118.8(5) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C23 C19 C18 120.9(4) . . ? C23 C19 C20 122.0(4) . . ? C18 C19 C20 116.7(4) . . ? O22 C20 O21 120.9(4) . . ? O22 C20 C19 119.8(4) . . ? O21 C20 C19 119.3(4) . . ? O22 C20 Ce 61.4(2) . 2_557 ? O21 C20 Ce 59.8(2) . 2_557 ? C19 C20 Ce 171.0(3) . 2_557 ? C20 O21 Ce 94.8(3) . 2_557 ? C20 O22 Ce 93.3(3) . 2_557 ? C24 C23 C19 119.3(4) . . ? C24 C23 H23 120.3 . . ? C19 C23 H23 120.3 . . ? C23 C24 C28 120.6(4) . . ? C23 C24 C25 121.4(4) . . ? C28 C24 C25 117.8(4) . . ? O26 C25 O27 121.1(4) . . ? O26 C25 C24 120.6(4) . . ? O27 C25 C24 118.4(4) . . ? O26 C25 Ce 63.3(3) . 2_567 ? O27 C25 Ce 57.8(2) . 2_567 ? C24 C25 Ce 174.3(3) . 2_567 ? C25 O26 Ce 91.7(3) . 2_567 ? C25 O27 Ce 96.9(3) . 2_567 ? C24 C28 C17 119.6(4) . . ? C24 C28 H28 120.2 . . ? C17 C28 H28 120.2 . . ? Ce O29 H29A 53.4 . . ? Ce O29 H29B 120.4 . . ? H29A O29 H29B 113.0 . . ? Ce O30 H30A 120.6 . . ? Ce O30 H30B 122.8 . . ? H30A O30 H30B 116.4 . . ? H31A O31 H31B 105.6 . . ? 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 O9 H9 O31 0.90 1.63 2.520(5) 172 2_556 O29 H29A O27 0.90 2.17 3.019(5) 156 2_567 O29 H29B O31 0.90 1.83 2.718(5) 167 . O30 H30B O13 0.90 1.92 2.813(5) 170 1_465 O31 H31A O1 0.90 1.85 2.745(5) 180 2_566 O31 H31B O21 0.90 1.72 2.626(4) 180 2_657 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.050 0.500 1.000 179 54 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.235 _refine_diff_density_min -1.071 _refine_diff_density_rms 0.153 #===============================END================================