# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email zhzhou@xmu.edu.cn _publ_contact_author_name 'Zhao-Hui Zhou' _publ_author_name 'Zhao-Hui Zhou' data_sad1 _database_code_depnum_ccdc_archive 'CCDC 837348' #TrackingRef 'cif1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Ammonium ethylenediaminietetraacetato lanthanum citrate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H84 La2 N12 O39' _chemical_formula_weight 1538.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4854(2) _cell_length_b 10.7110(2) _cell_length_c 14.5757(3) _cell_angle_alpha 102.744(2) _cell_angle_beta 90.147(2) _cell_angle_gamma 91.855(2) _cell_volume 1443.55(5) _cell_formula_units_Z 1 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 786 _exptl_absorpt_coefficient_mu 1.574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6088 _exptl_absorpt_correction_T_max 0.7437 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(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 'Oxford CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20662 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5055 _reflns_number_gt 4764 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+0.6940P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5055 _refine_ls_number_parameters 466 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0201 _refine_ls_R_factor_gt 0.0183 _refine_ls_wR_factor_ref 0.0465 _refine_ls_wR_factor_gt 0.0460 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.035 _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 La1 La 0.955254(11) 0.654947(10) 0.728752(7) 0.01244(5) Uani 1 1 d . . . N1 N 1.13104(18) 0.75241(16) 0.88820(12) 0.0166(4) Uani 1 1 d . . . N2 N 0.82737(18) 0.68499(16) 0.90379(12) 0.0164(4) Uani 1 1 d . . . N3 N 0.87815(19) 0.73269(17) 0.26617(12) 0.0195(4) Uani 1 1 d D . . N4 N 0.4523(2) 1.10264(19) 0.79051(14) 0.0268(4) Uani 1 1 d D . . N5 N 1.3052(2) 0.43595(19) 0.56085(13) 0.0251(4) Uani 1 1 d D . . N6 N 0.6608(2) -0.08130(19) 0.59802(14) 0.0248(4) Uani 1 1 d D . . O1 O 1.14131(14) 0.70690(13) 0.60888(10) 0.0155(3) Uani 1 1 d D . . O2 O 0.87454(14) 0.72601(14) 0.58524(10) 0.0178(3) Uani 1 1 d . . . O3 O 0.89602(15) 0.80785(13) 0.45894(9) 0.0177(3) Uani 1 1 d . . . O5 O 1.01965(15) 0.55033(14) 0.39891(10) 0.0191(3) Uani 1 1 d . . . O4 O 1.23931(15) 0.52012(14) 0.35179(11) 0.0220(3) Uani 1 1 d . . . O7 O 1.35834(16) 0.86383(15) 0.64688(11) 0.0243(3) Uani 1 1 d . . . O6 O 1.37074(19) 1.03604(19) 0.58741(14) 0.0415(5) Uani 1 1 d . . . O8 O 1.20184(15) 0.56820(14) 0.73955(10) 0.0189(3) Uani 1 1 d . . . O9 O 1.34056(16) 0.46910(15) 0.82196(11) 0.0254(4) Uani 1 1 d . . . O10 O 0.99497(15) 0.89943(14) 0.78704(10) 0.0190(3) Uani 1 1 d . . . O11 O 1.15955(16) 1.05708(14) 0.82094(11) 0.0230(3) Uani 1 1 d . . . O12 O 0.94464(15) 0.46593(14) 0.81252(10) 0.0191(3) Uani 1 1 d . . . O13 O 0.78406(16) 0.34007(14) 0.86252(11) 0.0232(3) Uani 1 1 d . . . O14 O 0.71330(15) 0.74745(16) 0.75094(10) 0.0239(3) Uani 1 1 d . . . O15 O 0.5673(2) 0.8857(2) 0.83444(13) 0.0517(6) Uani 1 1 d . . . O1W O 1.50642(19) 0.33880(18) 0.67772(13) 0.0351(4) Uani 1 1 d D . . O2W O 1.51274(17) 0.64125(17) 0.60233(12) 0.0321(4) Uani 1 1 d D . . O3W O 0.50656(17) 0.33232(16) 0.92394(12) 0.0264(4) Uani 1 1 d D . . O4W O 0.8241(2) 0.09634(17) 0.73603(13) 0.0378(4) Uani 1 1 d D . . O5W O 0.5445(7) 1.0624(6) 0.9816(4) 0.0815(17) Uani 0.50 1 d PD . . C1 C 1.1080(2) 0.77710(19) 0.53868(13) 0.0142(4) Uani 1 1 d . . . C2 C 0.9474(2) 0.76721(18) 0.52476(14) 0.0141(4) Uani 1 1 d . . . C3 C 1.1867(2) 0.7244(2) 0.44780(14) 0.0171(4) Uani 1 1 d . . . H3A H 1.1716 0.7803 0.4048 0.020 Uiso 1 1 calc R . . H3B H 1.2869 0.7283 0.4622 0.020 Uiso 1 1 calc R . . C4 C 1.1458(2) 0.58875(19) 0.39769(13) 0.0153(4) Uani 1 1 d . . . C5 C 1.1500(2) 0.91916(19) 0.57474(14) 0.0164(4) Uani 1 1 d . . . H5A H 1.1306 0.9647 0.5257 0.020 Uiso 1 1 calc R . . H5B H 1.0918 0.9544 0.6283 0.020 Uiso 1 1 calc R . . C6 C 1.3043(2) 0.9422(2) 0.60385(15) 0.0203(5) Uani 1 1 d . . . C7 C 1.2309(2) 0.6562(2) 0.90382(14) 0.0188(4) Uani 1 1 d . . . H7A H 1.1922 0.6125 0.9502 0.023 Uiso 1 1 calc R . . H7B H 1.3187 0.6994 0.9290 0.023 Uiso 1 1 calc R . . C8 C 1.2614(2) 0.5578(2) 0.81451(14) 0.0171(4) Uani 1 1 d . . . C9 C 1.2080(2) 0.8613(2) 0.86373(15) 0.0195(4) Uani 1 1 d . . . H9A H 1.2810 0.8294 0.8190 0.023 Uiso 1 1 calc R . . H9B H 1.2537 0.9123 0.9199 0.023 Uiso 1 1 calc R . . C10 C 1.1131(2) 0.9465(2) 0.82151(14) 0.0177(4) Uani 1 1 d . . . C11 C 0.7455(2) 0.5636(2) 0.89538(15) 0.0197(4) Uani 1 1 d . . . H11A H 0.6634 0.5642 0.8556 0.024 Uiso 1 1 calc R . . H11B H 0.7125 0.5571 0.9571 0.024 Uiso 1 1 calc R . . C12 C 0.8315(2) 0.4467(2) 0.85400(14) 0.0172(4) Uani 1 1 d . . . C13 C 0.7303(2) 0.7919(2) 0.91841(15) 0.0205(5) Uani 1 1 d . . . H13A H 0.7814 0.8702 0.9484 0.025 Uiso 1 1 calc R . . H13B H 0.6561 0.7765 0.9606 0.025 Uiso 1 1 calc R . . C14 C 0.6640(2) 0.8097(2) 0.82701(16) 0.0241(5) Uani 1 1 d . . . C15 C 1.0469(2) 0.7977(2) 0.97405(14) 0.0190(4) Uani 1 1 d . . . H15A H 1.0070 0.8792 0.9718 0.023 Uiso 1 1 calc R . . H15B H 1.1081 0.8108 1.0290 0.023 Uiso 1 1 calc R . . C16 C 0.9292(2) 0.7025(2) 0.98293(14) 0.0193(4) Uani 1 1 d . . . H16A H 0.9691 0.6208 0.9845 0.023 Uiso 1 1 calc R . . H16B H 0.8803 0.7324 1.0416 0.023 Uiso 1 1 calc R . . H1 H 1.2196(15) 0.741(2) 0.6297(16) 0.023 Uiso 1 1 d D . . H2 H 0.883(2) 0.7976(12) 0.2427(12) 0.023 Uiso 1 1 d D . . H3 H 0.9431(15) 0.6810(15) 0.2452(12) 0.023 Uiso 1 1 d D . . H4 H 0.7980(12) 0.6932(16) 0.2532(13) 0.023 Uiso 1 1 d D . . H5 H 0.8868(19) 0.7548(17) 0.3262(6) 0.023 Uiso 1 1 d D . . H6 H 0.3657(10) 1.0842(18) 0.8006(13) 0.023 Uiso 1 1 d D . . H7 H 0.5039(17) 1.0421(13) 0.7965(13) 0.023 Uiso 1 1 d D . . H8 H 0.4762(19) 1.1706(12) 0.8314(10) 0.023 Uiso 1 1 d D . . H9 H 0.4599(19) 1.1171(18) 0.7358(7) 0.023 Uiso 1 1 d D . . H10 H 1.3503(18) 0.3806(14) 0.5829(12) 0.023 Uiso 1 1 d D . . H11 H 1.2662(18) 0.4014(17) 0.5090(8) 0.023 Uiso 1 1 d D . . H12 H 1.3623(16) 0.4962(13) 0.5554(13) 0.023 Uiso 1 1 d D . . H13 H 1.2413(15) 0.4648(17) 0.6007(10) 0.023 Uiso 1 1 d D . . H14 H 0.5750(10) -0.0852(18) 0.6155(12) 0.023 Uiso 1 1 d D . . H15 H 0.7035(17) -0.0179(13) 0.6344(11) 0.023 Uiso 1 1 d D . . H16 H 0.7008(18) -0.1500(12) 0.6017(13) 0.023 Uiso 1 1 d D . . H17 H 0.6620(19) -0.0719(18) 0.5417(7) 0.023 Uiso 1 1 d D . . H1W1 H 1.4581(19) 0.3857(19) 0.7208(13) 0.023 Uiso 1 1 d D . . H1W2 H 1.5788(17) 0.3831(19) 0.6675(16) 0.023 Uiso 1 1 d D . . H2W1 H 1.575(2) 0.637(2) 0.6431(13) 0.023 Uiso 1 1 d D . . H2W2 H 1.469(2) 0.7103(15) 0.6196(15) 0.023 Uiso 1 1 d D . . H3W1 H 0.5917(11) 0.341(2) 0.9096(17) 0.023 Uiso 1 1 d D . . H3W2 H 0.4586(18) 0.3907(18) 0.9099(17) 0.023 Uiso 1 1 d D . . H4W1 H 0.870(2) 0.0435(16) 0.7570(15) 0.023 Uiso 1 1 d D . . H4W2 H 0.814(2) 0.1648(13) 0.7760(13) 0.023 Uiso 1 1 d D . . H5W1 H 0.555(3) 0.9871(15) 0.9451(15) 0.023 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01530(7) 0.01126(7) 0.01137(7) 0.00362(4) 0.00010(4) 0.00197(4) N1 0.0221(9) 0.0142(9) 0.0146(8) 0.0048(7) -0.0006(7) 0.0044(7) N2 0.0208(9) 0.0143(9) 0.0148(8) 0.0041(7) 0.0005(7) 0.0039(7) N3 0.0252(10) 0.0163(9) 0.0180(9) 0.0055(7) -0.0003(7) 0.0039(8) N4 0.0293(11) 0.0231(11) 0.0274(11) 0.0035(8) -0.0049(8) 0.0043(8) N5 0.0221(10) 0.0260(11) 0.0240(10) -0.0008(8) 0.0029(8) -0.0023(8) N6 0.0212(10) 0.0227(10) 0.0312(11) 0.0075(8) 0.0009(8) 0.0018(8) O1 0.0158(7) 0.0161(7) 0.0166(7) 0.0082(6) -0.0019(6) -0.0001(6) O2 0.0168(7) 0.0210(8) 0.0175(7) 0.0084(6) -0.0008(6) -0.0002(6) O3 0.0213(7) 0.0177(8) 0.0157(7) 0.0070(6) -0.0025(6) 0.0025(6) O5 0.0188(7) 0.0174(8) 0.0198(8) 0.0014(6) 0.0025(6) -0.0022(6) O4 0.0209(8) 0.0179(8) 0.0257(8) 0.0014(6) 0.0020(6) 0.0035(6) O7 0.0235(8) 0.0216(8) 0.0281(8) 0.0064(7) -0.0086(6) 0.0006(6) O6 0.0333(10) 0.0453(11) 0.0542(12) 0.0323(10) -0.0211(9) -0.0214(9) O8 0.0189(7) 0.0239(8) 0.0146(7) 0.0053(6) -0.0017(6) 0.0046(6) O9 0.0289(8) 0.0246(9) 0.0231(8) 0.0044(7) -0.0026(7) 0.0127(7) O10 0.0219(7) 0.0160(7) 0.0199(7) 0.0054(6) -0.0033(6) 0.0024(6) O11 0.0281(8) 0.0129(8) 0.0289(8) 0.0068(6) -0.0024(7) -0.0004(6) O12 0.0223(8) 0.0179(8) 0.0189(7) 0.0073(6) 0.0052(6) 0.0050(6) O13 0.0284(8) 0.0169(8) 0.0263(8) 0.0087(6) 0.0031(6) 0.0017(6) O14 0.0207(8) 0.0326(9) 0.0190(8) 0.0061(7) 0.0008(6) 0.0081(7) O15 0.0545(12) 0.0731(15) 0.0354(10) 0.0224(10) 0.0134(9) 0.0487(12) O1W 0.0310(9) 0.0334(10) 0.0367(10) -0.0015(8) 0.0073(8) 0.0016(8) O2W 0.0219(8) 0.0340(10) 0.0376(10) 0.0017(8) -0.0040(7) 0.0025(7) O3W 0.0254(8) 0.0263(9) 0.0305(9) 0.0131(7) -0.0016(7) -0.0006(7) O4W 0.0539(12) 0.0236(9) 0.0343(10) 0.0017(8) -0.0165(9) 0.0106(8) O5W 0.102(4) 0.066(4) 0.067(3) -0.008(3) -0.003(3) 0.012(3) C1 0.0195(10) 0.0126(10) 0.0117(10) 0.0054(8) -0.0010(8) 0.0001(8) C2 0.0193(10) 0.0092(9) 0.0131(10) 0.0011(8) 0.0004(8) 0.0014(8) C3 0.0187(10) 0.0163(10) 0.0164(10) 0.0042(8) 0.0009(8) -0.0010(8) C4 0.0210(10) 0.0148(10) 0.0117(10) 0.0060(8) -0.0001(8) 0.0015(8) C5 0.0205(10) 0.0124(10) 0.0167(10) 0.0038(8) -0.0021(8) 0.0000(8) C6 0.0225(11) 0.0196(11) 0.0175(11) 0.0016(9) -0.0019(8) -0.0009(9) C7 0.0241(11) 0.0180(11) 0.0156(10) 0.0056(8) -0.0040(8) 0.0056(9) C8 0.0159(10) 0.0181(11) 0.0182(10) 0.0060(8) -0.0007(8) 0.0012(8) C9 0.0223(11) 0.0163(11) 0.0201(11) 0.0043(8) -0.0034(9) 0.0001(8) C10 0.0233(11) 0.0163(11) 0.0126(10) 0.0010(8) 0.0030(8) 0.0030(9) C11 0.0221(11) 0.0179(11) 0.0206(11) 0.0073(9) 0.0059(9) 0.0021(9) C12 0.0216(11) 0.0197(11) 0.0118(10) 0.0062(8) -0.0024(8) 0.0016(9) C13 0.0260(11) 0.0177(11) 0.0184(11) 0.0044(9) 0.0036(9) 0.0069(9) C14 0.0233(11) 0.0279(12) 0.0234(12) 0.0094(10) 0.0035(9) 0.0084(10) C15 0.0272(11) 0.0166(11) 0.0130(10) 0.0019(8) -0.0017(8) 0.0065(9) C16 0.0275(11) 0.0189(11) 0.0125(10) 0.0049(8) 0.0021(8) 0.0066(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O2 2.5045(14) . ? La1 O14 2.5225(14) . ? La1 O8 2.5617(14) . ? La1 O5 2.5660(14) 2_766 ? La1 O10 2.5834(14) . ? La1 O12 2.5841(15) . ? La1 O1 2.6188(14) . ? La1 O4 2.6634(15) 2_766 ? La1 N2 2.7862(17) . ? La1 N1 2.8404(17) . ? La1 C4 2.972(2) 2_766 ? N1 C9 1.467(3) . ? N1 C7 1.475(3) . ? N1 C15 1.483(3) . ? N2 C13 1.471(3) . ? N2 C11 1.474(3) . ? N2 C16 1.479(3) . ? O1 C1 1.437(2) . ? O2 C2 1.267(3) . ? O3 C2 1.242(2) . ? O5 C4 1.254(3) . ? O5 La1 2.5660(14) 2_766 ? O4 C4 1.266(2) . ? O4 La1 2.6634(15) 2_766 ? O7 C6 1.272(3) . ? O6 C6 1.237(3) . ? O8 C8 1.257(2) . ? O9 C8 1.253(3) . ? O10 C10 1.270(3) . ? O11 C10 1.252(3) . ? O12 C12 1.266(3) . ? O13 C12 1.246(3) . ? O14 C14 1.261(3) . ? O15 C14 1.235(3) . ? O5W O5W 1.741(13) 2_677 ? C1 C3 1.528(3) . ? C1 C2 1.533(3) . ? C1 C5 1.535(3) . ? C3 C4 1.513(3) . ? C4 La1 2.972(2) 2_766 ? C5 C6 1.520(3) . ? C7 C8 1.518(3) . ? C9 C10 1.523(3) . ? C11 C12 1.528(3) . ? C13 C14 1.524(3) . ? C15 C16 1.512(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La1 O14 68.58(5) . . ? O2 La1 O8 121.48(5) . . ? O14 La1 O8 169.36(5) . . ? O2 La1 O5 78.59(5) . 2_766 ? O14 La1 O5 117.07(5) . 2_766 ? O8 La1 O5 70.57(4) . 2_766 ? O2 La1 O10 80.64(5) . . ? O14 La1 O10 73.79(5) . . ? O8 La1 O10 103.34(5) . . ? O5 La1 O10 150.23(5) 2_766 . ? O2 La1 O12 143.50(5) . . ? O14 La1 O12 104.59(5) . . ? O8 La1 O12 69.65(5) . . ? O5 La1 O12 73.13(5) 2_766 . ? O10 La1 O12 133.51(5) . . ? O2 La1 O1 60.26(4) . . ? O14 La1 O1 124.57(5) . . ? O8 La1 O1 63.64(4) . . ? O5 La1 O1 73.05(5) 2_766 . ? O10 La1 O1 78.19(5) . . ? O12 La1 O1 128.97(4) . . ? O2 La1 O4 74.70(5) . 2_766 ? O14 La1 O4 69.95(5) . 2_766 ? O8 La1 O4 114.60(5) . 2_766 ? O5 La1 O4 49.88(4) 2_766 2_766 ? O10 La1 O4 141.55(4) . 2_766 ? O12 La1 O4 69.52(5) . 2_766 ? O1 La1 O4 112.69(4) . 2_766 ? O2 La1 N2 129.16(5) . . ? O14 La1 N2 60.82(5) . . ? O8 La1 N2 108.79(5) . . ? O5 La1 N2 128.70(5) 2_766 . ? O10 La1 N2 81.06(5) . . ? O12 La1 N2 60.33(5) . . ? O1 La1 N2 155.17(5) . . ? O4 La1 N2 92.06(5) 2_766 . ? O2 La1 N1 137.60(5) . . ? O14 La1 N1 111.16(5) . . ? O8 La1 N1 59.51(5) . . ? O5 La1 N1 128.63(5) 2_766 . ? O10 La1 N1 60.28(5) . . ? O12 La1 N1 78.84(5) . . ? O1 La1 N1 93.95(5) . . ? O4 La1 N1 147.09(5) 2_766 . ? N2 La1 N1 63.67(5) . . ? O2 La1 C4 77.14(5) . 2_766 ? O14 La1 C4 94.34(5) . 2_766 ? O8 La1 C4 91.60(5) . 2_766 ? O5 La1 C4 24.80(5) 2_766 2_766 ? O10 La1 C4 157.44(5) . 2_766 ? O12 La1 C4 67.48(5) . 2_766 ? O1 La1 C4 93.93(5) . 2_766 ? O4 La1 C4 25.21(5) 2_766 2_766 ? N2 La1 C4 110.29(5) . 2_766 ? N1 La1 C4 142.04(5) . 2_766 ? C9 N1 C7 110.07(16) . . ? C9 N1 C15 109.64(16) . . ? C7 N1 C15 110.17(16) . . ? C9 N1 La1 103.89(11) . . ? C7 N1 La1 111.35(12) . . ? C15 N1 La1 111.55(12) . . ? C13 N2 C11 109.32(16) . . ? C13 N2 C16 110.35(16) . . ? C11 N2 C16 110.18(16) . . ? C13 N2 La1 110.42(12) . . ? C11 N2 La1 102.85(11) . . ? C16 N2 La1 113.44(12) . . ? C1 O1 La1 122.63(11) . . ? C2 O2 La1 129.03(12) . . ? C4 O5 La1 96.05(12) . 2_766 ? C4 O4 La1 91.17(12) . 2_766 ? C8 O8 La1 124.92(13) . . ? C10 O10 La1 120.83(12) . . ? C12 O12 La1 117.72(12) . . ? C14 O14 La1 126.11(13) . . ? O1 C1 C3 110.37(16) . . ? O1 C1 C2 107.19(16) . . ? C3 C1 C2 112.48(16) . . ? O1 C1 C5 109.70(15) . . ? C3 C1 C5 109.32(17) . . ? C2 C1 C5 107.70(16) . . ? O3 C2 O2 123.84(18) . . ? O3 C2 C1 118.34(18) . . ? O2 C2 C1 117.63(17) . . ? C4 C3 C1 115.90(17) . . ? O5 C4 O4 122.26(18) . . ? O5 C4 C3 119.19(17) . . ? O4 C4 C3 118.45(18) . . ? O5 C4 La1 59.15(10) . 2_766 ? O4 C4 La1 63.62(10) . 2_766 ? C3 C4 La1 169.23(14) . 2_766 ? C6 C5 C1 113.57(17) . . ? O6 C6 O7 122.9(2) . . ? O6 C6 C5 119.8(2) . . ? O7 C6 C5 117.27(19) . . ? N1 C7 C8 112.73(16) . . ? O9 C8 O8 124.77(19) . . ? O9 C8 C7 117.10(18) . . ? O8 C8 C7 118.08(17) . . ? N1 C9 C10 112.92(17) . . ? O11 C10 O10 124.73(19) . . ? O11 C10 C9 117.29(18) . . ? O10 C10 C9 117.94(19) . . ? N2 C11 C12 112.56(17) . . ? O13 C12 O12 125.24(19) . . ? O13 C12 C11 117.58(18) . . ? O12 C12 C11 117.17(19) . . ? N2 C13 C14 112.75(17) . . ? O15 C14 O14 125.8(2) . . ? O15 C14 C13 116.58(19) . . ? O14 C14 C13 117.59(18) . . ? N1 C15 C16 111.47(17) . . ? N2 C16 C15 111.64(17) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.619 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.064 # Attachment 'cif2.cif' data_sad3 _database_code_depnum_ccdc_archive 'CCDC 837349' #TrackingRef 'cif2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Ammonium ethylenediaminietetraacetato cerium citrate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H84 Ce2 N12 O39' _chemical_formula_weight 1541.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ce Ce -0.2486 2.6331 '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 9.4887(3) _cell_length_b 10.6793(4) _cell_length_c 14.5334(6) _cell_angle_alpha 102.722(4) _cell_angle_beta 90.144(3) _cell_angle_gamma 91.800(3) _cell_volume 1435.78(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 1.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5909 _exptl_absorpt_correction_T_max 0.7867 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Oxford CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13326 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6582 _reflns_number_gt 5902 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+0.2297P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6582 _refine_ls_number_parameters 466 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 2.042 _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 Ce1 Ce 0.04471(3) 0.34523(3) 0.27084(2) 0.01020(10) Uani 1 1 d . . . C1 C 0.1077(5) 0.7762(5) 0.5392(4) 0.0110(11) Uani 1 1 d . . . C2 C -0.0534(6) 0.7659(5) 0.5252(4) 0.0123(11) Uani 1 1 d . . . C3 C 0.1862(6) 0.7230(6) 0.4480(4) 0.0147(12) Uani 1 1 d . . . H04A H 0.1712 0.7806 0.4042 0.018 Uiso 1 1 calc R . . H04B H 0.2883 0.7266 0.4628 0.018 Uiso 1 1 calc R . . C4 C 0.1458(6) 0.5878(6) 0.3971(4) 0.0143(12) Uani 1 1 d . . . C5 C 0.1491(5) 0.9178(5) 0.5749(4) 0.0141(12) Uani 1 1 d . . . H03K H 0.0901 0.9538 0.6299 0.017 Uiso 1 1 calc R . . H03L H 0.1286 0.9644 0.5248 0.017 Uiso 1 1 calc R . . C6 C 0.3043(6) 0.9416(6) 0.6037(4) 0.0176(12) Uani 1 1 d . . . C7 C -0.2073(6) 0.1402(6) 0.1365(4) 0.0163(12) Uani 1 1 d . . . H03E H -0.2540 0.0881 0.0791 0.020 Uiso 1 1 calc R . . H03F H -0.2817 0.1731 0.1823 0.020 Uiso 1 1 calc R . . C8 C -0.1119(6) 0.0551(6) 0.1788(4) 0.0157(12) Uani 1 1 d . . . C9 C -0.2293(6) 0.3460(6) 0.0961(4) 0.0166(12) Uani 1 1 d . . . H02A H -0.3190 0.3020 0.0703 0.020 Uiso 1 1 calc R . . H02B H -0.1897 0.3907 0.0487 0.020 Uiso 1 1 calc R . . C10 C -0.2592(6) 0.4437(6) 0.1852(4) 0.0156(12) Uani 1 1 d . . . C11 C 0.2698(6) 0.2076(6) 0.0825(4) 0.0181(13) Uani 1 1 d . . . H03A H 0.3461 0.2233 0.0397 0.022 Uiso 1 1 calc R . . H03B H 0.2178 0.1274 0.0517 0.022 Uiso 1 1 calc R . . C12 C 0.3344(6) 0.1901(6) 0.1739(4) 0.0213(14) Uani 1 1 d . . . C13 C 0.2551(6) 0.4362(6) 0.1057(4) 0.0182(13) Uani 1 1 d . . . H03I H 0.2894 0.4432 0.0427 0.022 Uiso 1 1 calc R . . H03J H 0.3384 0.4353 0.1467 0.022 Uiso 1 1 calc R . . C14 C 0.1687(6) 0.5532(6) 0.1471(4) 0.0150(12) Uani 1 1 d . . . C15 C -0.0459(6) 0.2033(6) 0.0255(4) 0.0166(12) Uani 1 1 d . . . H03C H -0.1084 0.1905 -0.0307 0.020 Uiso 1 1 calc R . . H03D H -0.0057 0.1196 0.0276 0.020 Uiso 1 1 calc R . . C16 C 0.0722(6) 0.2984(6) 0.0168(4) 0.0178(12) Uani 1 1 d . . . H03G H 0.1226 0.2677 -0.0431 0.021 Uiso 1 1 calc R . . H03H H 0.0321 0.3823 0.0152 0.021 Uiso 1 1 calc R . . N1 N -0.1298(5) 0.2492(5) 0.1119(3) 0.0142(10) Uani 1 1 d . . . N2 N 0.1730(5) 0.3148(5) 0.0968(3) 0.0144(10) Uani 1 1 d . . . O1 O 0.1407(4) 0.7051(4) 0.6094(3) 0.0130(8) Uani 1 1 d . . . H1A H 0.215(6) 0.741(6) 0.631(4) 0.016 Uiso 1 1 d . . . O2 O -0.1049(4) 0.8073(4) 0.4597(3) 0.0157(9) Uani 1 1 d . . . O3 O -0.1250(4) 0.7243(4) 0.5863(3) 0.0162(9) Uani 1 1 d . . . O5 O 0.0193(4) 0.5485(4) 0.3977(3) 0.0172(9) Uani 1 1 d . . . O4 O 0.2394(4) 0.5186(4) 0.3509(3) 0.0188(9) Uani 1 1 d . . . O6 O 0.3693(5) 1.0358(5) 0.5876(4) 0.0394(14) Uani 1 1 d . . . O7 O 0.3573(4) 0.8628(4) 0.6473(3) 0.0223(10) Uani 1 1 d . . . O8 O -0.1580(4) -0.0559(4) 0.1792(3) 0.0216(9) Uani 1 1 d . . . O9 O 0.0055(4) 0.1026(4) 0.2132(3) 0.0162(9) Uani 1 1 d . . . O10 O -0.3392(4) 0.5331(4) 0.1790(3) 0.0229(10) Uani 1 1 d . . . O11 O -0.1997(4) 0.4336(4) 0.2608(3) 0.0161(9) Uani 1 1 d . . . O12 O 0.4332(5) 0.1146(6) 0.1670(4) 0.0497(17) Uani 1 1 d . . . O13 O 0.2844(4) 0.2516(4) 0.2499(3) 0.0208(9) Uani 1 1 d . . . O14 O 0.2159(4) 0.6604(4) 0.1384(3) 0.0211(9) Uani 1 1 d . . . O15 O 0.0557(4) 0.5337(4) 0.1880(3) 0.0168(9) Uani 1 1 d . . . N3 N -0.1210(6) 0.7338(5) 0.2670(4) 0.0176(11) Uani 1 1 d . . . H1 H -0.043(6) 0.681(6) 0.244(4) 0.021 Uiso 1 1 d . . . H2 H -0.116(6) 0.798(7) 0.236(5) 0.021 Uiso 1 1 d . . . H3 H -0.196(7) 0.690(7) 0.251(5) 0.021 Uiso 1 1 d . . . H4 H -0.107(6) 0.758(6) 0.334(5) 0.021 Uiso 1 1 d . . . N4 N 0.5494(6) -0.1025(6) 0.2095(5) 0.0265(13) Uani 1 1 d . . . H5 H 0.540(7) -0.124(7) 0.264(5) 0.032 Uiso 1 1 d . . . H6 H 0.648(7) -0.085(7) 0.193(5) 0.032 Uiso 1 1 d . . . H7 H 0.517(7) -0.180(7) 0.163(5) 0.032 Uiso 1 1 d . . . H8 H 0.499(7) -0.037(7) 0.203(5) 0.032 Uiso 1 1 d . . . N5 N 0.3384(6) 1.0819(6) 0.4022(4) 0.0226(12) Uani 1 1 d . . . H9 H 0.291(7) 1.012(7) 0.353(5) 0.027 Uiso 1 1 d . . . H10 H 0.328(6) 1.076(6) 0.477(5) 0.027 Uiso 1 1 d . . . H11 H 0.296(7) 1.160(7) 0.397(5) 0.027 Uiso 1 1 d . . . H12 H 0.415(7) 1.078(7) 0.388(5) 0.027 Uiso 1 1 d . . . N6 N -0.3053(6) 0.5637(6) 0.4392(4) 0.0230(12) Uani 1 1 d . . . H13 H -0.367(7) 0.624(7) 0.414(5) 0.028 Uiso 1 1 d . . . H14 H -0.381(7) 0.515(7) 0.451(5) 0.028 Uiso 1 1 d . . . H15 H -0.259(7) 0.605(7) 0.489(5) 0.028 Uiso 1 1 d . . . H16 H -0.239(7) 0.539(7) 0.402(5) 0.028 Uiso 1 1 d . . . O1W O 0.5125(5) 0.6407(5) 0.6027(4) 0.0310(11) Uani 1 1 d D . . H1W2 H 0.571(6) 0.630(7) 0.644(4) 0.037 Uiso 1 1 d D . . O2W O -0.5073(5) 0.6628(5) 0.3227(4) 0.0325(11) Uani 1 1 d D . . H2W1 H -0.465(7) 0.617(6) 0.277(4) 0.039 Uiso 1 1 d D . . H2W2 H -0.577(5) 0.619(6) 0.336(5) 0.039 Uiso 1 1 d D . . O3W O 0.4935(4) 0.6677(4) 0.0761(3) 0.0246(10) Uani 1 1 d D . . H3W1 H 0.542(5) 0.613(5) 0.095(5) 0.030 Uiso 1 1 d D . . H3W2 H 0.408(3) 0.661(6) 0.092(5) 0.030 Uiso 1 1 d D . . O4W O 0.1749(6) 0.9045(5) 0.2648(4) 0.0359(12) Uani 1 1 d D . . H4W1 H 0.128(7) 0.953(5) 0.238(4) 0.043 Uiso 1 1 d D . . H4W2 H 0.187(7) 0.834(4) 0.225(4) 0.043 Uiso 1 1 d D . . O5W O 0.4528(18) -0.058(2) 0.0204(13) 0.093(5) Uani 0.50 1 d PD . . H5W1 H 0.495(12) -0.084(13) -0.033(5) 0.112 Uiso 1 1 d D . . H1W1 H 0.468(9) 0.709(6) 0.624(6) 0.112 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.01133(17) 0.01037(18) 0.00905(17) 0.00227(12) 0.00020(11) 0.00178(11) C1 0.015(3) 0.011(3) 0.008(3) 0.002(2) 0.000(2) 0.001(2) C2 0.018(3) 0.007(3) 0.011(3) 0.000(2) 0.000(2) 0.002(2) C3 0.015(3) 0.018(3) 0.011(3) 0.002(2) 0.000(2) -0.003(2) C4 0.020(3) 0.015(3) 0.009(3) 0.004(2) 0.000(2) 0.000(2) C5 0.014(3) 0.011(3) 0.016(3) 0.001(2) -0.002(2) 0.000(2) C6 0.018(3) 0.018(3) 0.015(3) 0.000(2) 0.000(2) -0.001(2) C7 0.017(3) 0.015(3) 0.016(3) 0.003(2) -0.003(2) 0.001(2) C8 0.022(3) 0.014(3) 0.010(3) 0.000(2) 0.002(2) 0.003(2) C9 0.019(3) 0.018(3) 0.014(3) 0.003(2) -0.003(2) 0.006(2) C10 0.012(3) 0.016(3) 0.019(3) 0.005(2) 0.001(2) 0.002(2) C11 0.022(3) 0.016(3) 0.016(3) 0.004(2) 0.005(2) 0.007(2) C12 0.018(3) 0.025(4) 0.023(3) 0.010(3) 0.005(2) 0.006(3) C13 0.017(3) 0.019(3) 0.019(3) 0.006(3) 0.004(2) 0.004(2) C14 0.021(3) 0.015(3) 0.010(3) 0.003(2) -0.001(2) 0.003(2) C15 0.021(3) 0.017(3) 0.010(3) -0.001(2) -0.001(2) 0.004(2) C16 0.026(3) 0.017(3) 0.012(3) 0.005(2) 0.002(2) 0.006(2) N1 0.018(2) 0.013(3) 0.012(2) 0.0024(19) 0.0009(19) 0.0039(19) N2 0.017(2) 0.014(3) 0.013(2) 0.0027(19) 0.0013(19) 0.0043(19) O1 0.0119(19) 0.016(2) 0.012(2) 0.0067(16) -0.0030(16) 0.0000(16) O2 0.018(2) 0.016(2) 0.013(2) 0.0051(17) -0.0022(16) 0.0022(17) O3 0.0129(19) 0.023(2) 0.015(2) 0.0079(17) 0.0000(16) 0.0001(16) O5 0.015(2) 0.016(2) 0.018(2) 0.0002(17) 0.0021(16) -0.0021(16) O4 0.016(2) 0.017(2) 0.021(2) 0.0006(18) 0.0033(17) 0.0019(17) O6 0.031(3) 0.045(3) 0.049(3) 0.029(3) -0.020(2) -0.024(2) O7 0.017(2) 0.020(2) 0.029(3) 0.0054(19) -0.0096(18) 0.0001(17) O8 0.023(2) 0.016(2) 0.027(3) 0.0060(19) -0.0036(18) -0.0021(18) O9 0.018(2) 0.014(2) 0.016(2) 0.0013(17) -0.0050(16) 0.0011(16) O10 0.026(2) 0.022(3) 0.021(2) 0.0037(19) -0.0017(18) 0.0121(19) O11 0.017(2) 0.020(2) 0.012(2) 0.0023(17) -0.0012(16) 0.0049(17) O12 0.049(3) 0.075(4) 0.032(3) 0.020(3) 0.011(2) 0.051(3) O13 0.016(2) 0.031(3) 0.016(2) 0.0034(19) 0.0004(17) 0.0078(18) O14 0.025(2) 0.014(2) 0.026(2) 0.0067(18) 0.0020(18) 0.0016(18) O15 0.018(2) 0.016(2) 0.017(2) 0.0055(17) 0.0064(17) 0.0040(17) N3 0.021(3) 0.016(3) 0.016(3) 0.004(2) -0.002(2) 0.002(2) N4 0.027(3) 0.023(3) 0.030(3) 0.004(3) -0.006(3) 0.004(2) N5 0.014(3) 0.024(3) 0.030(3) 0.006(3) 0.002(2) 0.003(2) N6 0.015(3) 0.028(3) 0.022(3) -0.002(2) 0.003(2) -0.003(2) O1W 0.017(2) 0.034(3) 0.040(3) 0.004(2) -0.004(2) 0.000(2) O2W 0.029(3) 0.031(3) 0.032(3) -0.003(2) 0.008(2) 0.000(2) O3W 0.023(2) 0.026(3) 0.029(3) 0.012(2) -0.002(2) 0.0005(19) O4W 0.048(3) 0.022(3) 0.035(3) 0.001(2) -0.018(2) 0.009(2) O5W 0.105(13) 0.092(14) 0.079(13) 0.010(10) 0.018(10) 0.012(10) _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 Ce1 O3 2.480(4) 2_566 ? Ce1 O13 2.506(4) . ? Ce1 O5 2.538(4) . ? Ce1 O11 2.547(4) . ? Ce1 O9 2.557(4) . ? Ce1 O15 2.562(4) . ? Ce1 O1 2.604(4) 2_566 ? Ce1 O4 2.649(4) . ? Ce1 N2 2.768(5) . ? Ce1 N1 2.821(5) . ? Ce1 C4 2.956(6) . ? C1 O1 1.438(6) . ? C1 C5 1.526(8) . ? C1 C3 1.528(7) . ? C1 C2 1.538(7) . ? C2 O2 1.239(6) . ? C2 O3 1.267(6) . ? C3 C4 1.507(8) . ? C4 O5 1.259(7) . ? C4 O4 1.270(7) . ? C5 C6 1.528(7) . ? C6 O6 1.229(7) . ? C6 O7 1.275(7) . ? C7 N1 1.468(7) . ? C7 C8 1.522(8) . ? C8 O8 1.253(7) . ? C8 O9 1.264(7) . ? C9 N1 1.476(7) . ? C9 C10 1.507(8) . ? C10 O10 1.257(7) . ? C10 O11 1.261(6) . ? C11 N2 1.470(7) . ? C11 C12 1.512(8) . ? C12 O12 1.245(7) . ? C12 O13 1.257(7) . ? C13 N2 1.472(7) . ? C13 C14 1.527(8) . ? C14 O14 1.249(7) . ? C14 O15 1.260(7) . ? C15 N1 1.487(7) . ? C15 C16 1.512(8) . ? C16 N2 1.480(7) . ? O1 Ce1 2.604(4) 2_566 ? O3 Ce1 2.480(4) 2_566 ? O5W O5W 1.71(4) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ce1 O13 68.10(13) 2_566 . ? O3 Ce1 O5 78.24(13) 2_566 . ? O13 Ce1 O5 117.14(13) . . ? O3 Ce1 O11 121.38(12) 2_566 . ? O13 Ce1 O11 170.00(13) . . ? O5 Ce1 O11 70.10(12) . . ? O3 Ce1 O9 80.86(13) 2_566 . ? O13 Ce1 O9 73.48(13) . . ? O5 Ce1 O9 150.01(13) . . ? O11 Ce1 O9 103.80(12) . . ? O3 Ce1 O15 143.02(13) 2_566 . ? O13 Ce1 O15 105.11(13) . . ? O5 Ce1 O15 73.12(13) . . ? O11 Ce1 O15 69.53(12) . . ? O9 Ce1 O15 133.75(13) . . ? O3 Ce1 O1 60.48(12) 2_566 2_566 ? O13 Ce1 O1 124.25(13) . 2_566 ? O5 Ce1 O1 72.60(13) . 2_566 ? O11 Ce1 O1 63.46(12) . 2_566 ? O9 Ce1 O1 78.46(13) . 2_566 ? O15 Ce1 O1 128.66(12) . 2_566 ? O3 Ce1 O4 74.28(13) 2_566 . ? O13 Ce1 O4 69.75(13) . . ? O5 Ce1 O4 50.34(12) . . ? O11 Ce1 O4 114.54(13) . . ? O9 Ce1 O4 141.15(12) . . ? O15 Ce1 O4 69.53(13) . . ? O1 Ce1 O4 112.68(12) 2_566 . ? O3 Ce1 N2 128.93(13) 2_566 . ? O13 Ce1 N2 61.02(13) . . ? O5 Ce1 N2 128.92(14) . . ? O11 Ce1 N2 109.22(13) . . ? O9 Ce1 N2 81.05(13) . . ? O15 Ce1 N2 60.60(13) . . ? O1 Ce1 N2 155.46(14) 2_566 . ? O4 Ce1 N2 91.77(13) . . ? O3 Ce1 N1 138.08(13) 2_566 . ? O13 Ce1 N1 111.42(13) . . ? O5 Ce1 N1 128.47(13) . . ? O11 Ce1 N1 59.79(13) . . ? O9 Ce1 N1 60.54(13) . . ? O15 Ce1 N1 78.83(13) . . ? O1 Ce1 N1 94.10(13) 2_566 . ? O4 Ce1 N1 147.01(13) . . ? N2 Ce1 N1 63.84(13) . . ? O3 Ce1 C4 76.72(14) 2_566 . ? O13 Ce1 C4 94.29(15) . . ? O5 Ce1 C4 25.05(13) . . ? O11 Ce1 C4 91.33(14) . . ? O9 Ce1 C4 157.24(14) . . ? O15 Ce1 C4 67.39(14) . . ? O1 Ce1 C4 93.72(14) 2_566 . ? O4 Ce1 C4 25.43(13) . . ? N2 Ce1 C4 110.24(15) . . ? N1 Ce1 C4 141.99(14) . . ? O1 C1 C5 110.1(4) . . ? O1 C1 C3 110.2(4) . . ? C5 C1 C3 109.4(4) . . ? O1 C1 C2 106.9(4) . . ? C5 C1 C2 107.7(4) . . ? C3 C1 C2 112.3(4) . . ? O2 C2 O3 124.4(5) . . ? O2 C2 C1 118.3(5) . . ? O3 C2 C1 117.1(5) . . ? C4 C3 C1 116.5(5) . . ? O5 C4 O4 121.7(5) . . ? O5 C4 C3 119.4(5) . . ? O4 C4 C3 118.8(5) . . ? O5 C4 Ce1 58.6(3) . . ? O4 C4 Ce1 63.7(3) . . ? C3 C4 Ce1 169.5(4) . . ? C1 C5 C6 113.7(5) . . ? O6 C6 O7 123.7(5) . . ? O6 C6 C5 119.9(5) . . ? O7 C6 C5 116.4(5) . . ? N1 C7 C8 112.4(4) . . ? O8 C8 O9 124.9(5) . . ? O8 C8 C7 117.1(5) . . ? O9 C8 C7 117.9(5) . . ? N1 C9 C10 112.4(4) . . ? O10 C10 O11 123.8(5) . . ? O10 C10 C9 117.6(5) . . ? O11 C10 C9 118.6(5) . . ? N2 C11 C12 112.6(5) . . ? O12 C12 O13 125.4(6) . . ? O12 C12 C11 116.6(6) . . ? O13 C12 C11 117.9(5) . . ? N2 C13 C14 112.3(5) . . ? O14 C14 O15 125.3(5) . . ? O14 C14 C13 117.5(5) . . ? O15 C14 C13 117.2(5) . . ? N1 C15 C16 111.2(5) . . ? N2 C16 C15 111.2(5) . . ? C7 N1 C9 110.0(4) . . ? C7 N1 C15 109.6(4) . . ? C9 N1 C15 110.1(4) . . ? C7 N1 Ce1 103.8(3) . . ? C9 N1 Ce1 111.5(3) . . ? C15 N1 Ce1 111.7(3) . . ? C11 N2 C13 109.2(4) . . ? C11 N2 C16 110.6(4) . . ? C13 N2 C16 109.9(4) . . ? C11 N2 Ce1 110.5(3) . . ? C13 N2 Ce1 102.7(3) . . ? C16 N2 Ce1 113.7(3) . . ? C1 O1 Ce1 122.5(3) . 2_566 ? C2 O3 Ce1 129.6(3) . 2_566 ? C4 O5 Ce1 96.4(3) . . ? C4 O4 Ce1 90.9(3) . . ? C8 O9 Ce1 121.1(4) . . ? C10 O11 Ce1 124.5(3) . . ? C12 O13 Ce1 126.1(4) . . ? C14 O15 Ce1 117.7(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.766 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.117 # Attachment 'cif3.cif' data_sad2 _database_code_depnum_ccdc_archive 'CCDC 837350' #TrackingRef 'cif3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Potassium ethylenediaminietetraacetato lanthanum citrate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H66 K8 La2 N4 O46' _chemical_formula_weight 1833.51 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.234(3) _cell_length_b 11.305(3) _cell_length_c 14.592(4) _cell_angle_alpha 84.066(4) _cell_angle_beta 72.720(4) _cell_angle_gamma 65.178(4) _cell_volume 1605.6(7) _cell_formula_units_Z 1 _cell_measurement_temperature 566(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.942 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6974 _exptl_absorpt_correction_T_max 0.8295 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 566(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 'Oxford CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8064 _diffrn_reflns_av_R_equivalents 0.0803 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5608 _reflns_number_gt 5245 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+2.5241P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5608 _refine_ls_number_parameters 466 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 2.326 _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 La1 La 0.33052(5) 0.03635(5) 0.23405(4) 0.0193(2) Uani 1 1 d . . . O1 O 0.3491(7) -0.1291(7) 0.1064(5) 0.0243(15) Uani 1 1 d D . . O2 O 0.2249(7) 0.1200(7) 0.0996(5) 0.0275(15) Uani 1 1 d . . . O3 O 0.1319(7) 0.1154(7) -0.0127(5) 0.0311(16) Uani 1 1 d . . . O5 O 0.4422(7) -0.0011(7) -0.1018(5) 0.0292(16) Uani 1 1 d . . . O4 O 0.5664(7) -0.2056(7) -0.1460(5) 0.0300(16) Uani 1 1 d . . . O7 O 0.2881(9) -0.3279(8) 0.1385(8) 0.047(2) Uani 1 1 d . . . O6 O 0.0936(11) -0.3157(9) 0.1221(8) 0.058(3) Uani 1 1 d . . . O9 O 0.0114(8) -0.1307(9) 0.3348(6) 0.0383(19) Uani 1 1 d . . . O10 O 0.5145(8) -0.2009(7) 0.2298(5) 0.0301(16) Uani 1 1 d . . . O11 O 0.6267(8) -0.3814(8) 0.2972(7) 0.044(2) Uani 1 1 d . . . O12 O 0.5092(7) 0.0359(7) 0.3113(5) 0.0306(16) Uani 1 1 d . . . O13 O 0.5669(8) 0.1694(8) 0.3719(6) 0.0383(19) Uani 1 1 d . . . O14 O 0.1475(8) 0.2704(7) 0.2688(5) 0.0319(17) Uani 1 1 d . . . O15 O -0.0507(9) 0.4038(10) 0.3600(7) 0.061(3) Uani 1 1 d . . . O8 O 0.1108(7) 0.0084(8) 0.2977(6) 0.0320(17) Uani 1 1 d . . . N1 N 0.2992(8) -0.1254(9) 0.3901(6) 0.0263(18) Uani 1 1 d . . . N2 N 0.2448(8) 0.1498(9) 0.4144(6) 0.0261(18) Uani 1 1 d . . . C1 C 0.2571(10) -0.0876(9) 0.0476(7) 0.022(2) Uani 1 1 d . . . C2 C 0.2008(9) 0.0612(9) 0.0437(7) 0.023(2) Uani 1 1 d . . . C3 C 0.3344(10) -0.1498(10) -0.0527(7) 0.025(2) Uani 1 1 d . . . H3A H 0.3672 -0.2438 -0.0476 0.030 Uiso 1 1 calc R . . H3B H 0.2716 -0.1219 -0.0919 0.030 Uiso 1 1 calc R . . C4 C 0.4548(10) -0.1160(10) -0.1028(7) 0.023(2) Uani 1 1 d . . . C5 C 0.1373(10) -0.1255(10) 0.0919(7) 0.024(2) Uani 1 1 d . . . H5A H 0.0796 -0.0719 0.1493 0.028 Uiso 1 1 calc R . . H5B H 0.0833 -0.1060 0.0470 0.028 Uiso 1 1 calc R . . C6 C 0.1781(11) -0.2681(11) 0.1182(8) 0.031(2) Uani 1 1 d . . . C7 C 0.2235(11) -0.1913(11) 0.3671(8) 0.033(2) Uani 1 1 d . . . H7A H 0.1891 -0.2330 0.4240 0.040 Uiso 1 1 calc R . . H7B H 0.2846 -0.2585 0.3183 0.040 Uiso 1 1 calc R . . C8 C 0.1055(11) -0.0967(11) 0.3315(7) 0.029(2) Uani 1 1 d . . . C9 C 0.4312(11) -0.2219(11) 0.3981(8) 0.031(2) Uani 1 1 d . . . H9A H 0.4187 -0.2940 0.4355 0.037 Uiso 1 1 calc R . . H9B H 0.4688 -0.1829 0.4319 0.037 Uiso 1 1 calc R . . C10 C 0.5313(10) -0.2731(10) 0.3007(8) 0.028(2) Uani 1 1 d . . . C11 C 0.3311(11) 0.2187(10) 0.4067(8) 0.030(2) Uani 1 1 d . . . H11A H 0.3209 0.2466 0.4703 0.036 Uiso 1 1 calc R . . H11B H 0.3012 0.2960 0.3691 0.036 Uiso 1 1 calc R . . C12 C 0.4806(11) 0.1350(10) 0.3601(7) 0.028(2) Uani 1 1 d . . . C13 C 0.1003(11) 0.2435(11) 0.4364(8) 0.033(2) Uani 1 1 d . . . H13A H 0.0831 0.3074 0.4836 0.039 Uiso 1 1 calc R . . H13B H 0.0424 0.1975 0.4642 0.039 Uiso 1 1 calc R . . C14 C 0.0635(11) 0.3123(11) 0.3490(8) 0.032(2) Uani 1 1 d . . . C15 C 0.2194(11) -0.0500(11) 0.4818(8) 0.032(2) Uani 1 1 d . . . H15A H 0.2299 -0.1087 0.5351 0.038 Uiso 1 1 calc R . . H15B H 0.1233 -0.0095 0.4845 0.038 Uiso 1 1 calc R . . C16 C 0.2661(11) 0.0529(11) 0.4913(7) 0.029(2) Uani 1 1 d . . . H16A H 0.2160 0.0970 0.5533 0.035 Uiso 1 1 calc R . . H16B H 0.3623 0.0123 0.4882 0.035 Uiso 1 1 calc R . . H1 H 0.359(13) -0.206(5) 0.123(9) 0.035 Uiso 1 1 d D . . K2 K 0.6535(2) -0.2579(2) 0.03117(17) 0.0312(5) Uani 1 1 d . . . K3 K 0.7779(3) -0.1454(3) 0.20197(19) 0.0409(6) Uani 1 1 d . . . O3W O 0.8797(9) -0.4339(8) -0.1143(6) 0.0399(19) Uani 1 1 d D . . K1 K 0.9427(3) -0.6468(3) 0.0493(2) 0.0540(8) Uani 1 1 d . . . O1W O 0.6385(15) -0.5002(13) 0.0512(10) 0.080(4) Uani 1 1 d D . . O4W O 0.8353(8) -0.3995(9) 0.1384(6) 0.0401(19) Uani 1 1 d D . . K4 K 0.5549(4) -0.5907(3) 0.3457(3) 0.0607(9) Uani 1 1 d . . . H3W1 H 0.864(18) -0.379(11) -0.158(8) 0.073 Uiso 1 1 d D . . H3W2 H 0.866(17) -0.499(9) -0.124(10) 0.073 Uiso 1 1 d D . . H1W1 H 0.595(16) -0.514(16) 0.107(4) 0.073 Uiso 1 1 d D . . H1W2 H 0.637(17) -0.547(15) 0.010(7) 0.073 Uiso 1 1 d D . . H4W1 H 0.911(7) -0.440(14) 0.152(9) 0.073 Uiso 1 1 d D . . H4W2 H 0.850(13) -0.373(15) 0.081(5) 0.073 Uiso 1 1 d D . . O2W O 0.8363(16) -0.6991(14) 0.2387(11) 0.083(4) Uani 1 1 d D . . O7W O 0.3309(11) -0.4954(11) 0.5242(8) 0.061(3) Uani 1 1 d D . . O8W O 0.4336(11) -0.5636(9) 0.2038(8) 0.056(3) Uani 1 1 d D . . H2W1 H 0.896(13) -0.689(17) 0.258(12) 0.067 Uiso 1 1 d D . . H2W2 H 0.868(17) -0.782(3) 0.233(13) 0.067 Uiso 1 1 d D . . H7W1 H 0.292(14) -0.453(12) 0.578(5) 0.067 Uiso 1 1 d D . . H7W2 H 0.290(14) -0.453(12) 0.483(7) 0.067 Uiso 1 1 d D . . H8W1 H 0.417(14) -0.631(8) 0.206(12) 0.067 Uiso 1 1 d D . . H8W2 H 0.374(12) -0.499(8) 0.184(12) 0.067 Uiso 1 1 d D . . O5W O 0.8229(9) 0.0581(10) 0.2518(7) 0.046(2) Uani 1 1 d D . . O6W O 0.8852(13) -0.3183(12) 0.3337(9) 0.072(3) Uani 1 1 d D . . H5W1 H 0.878(13) -0.001(13) 0.279(10) 0.087 Uiso 1 1 d D . . H5W2 H 0.751(10) 0.104(14) 0.294(8) 0.087 Uiso 1 1 d D . . H6W1 H 0.916(15) -0.347(17) 0.276(5) 0.087 Uiso 1 1 d D . . H6W2 H 0.947(12) -0.357(16) 0.362(10) 0.087 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0171(3) 0.0212(3) 0.0172(3) -0.0028(2) -0.0023(2) -0.0065(2) O1 0.024(3) 0.024(4) 0.028(4) -0.001(3) -0.011(3) -0.009(3) O2 0.033(4) 0.024(4) 0.028(4) -0.003(3) -0.009(3) -0.012(3) O3 0.031(4) 0.029(4) 0.031(4) 0.000(3) -0.014(3) -0.006(3) O5 0.029(4) 0.025(4) 0.030(4) -0.007(3) 0.003(3) -0.012(3) O4 0.025(4) 0.027(4) 0.031(4) -0.002(3) 0.000(3) -0.010(3) O7 0.039(5) 0.032(4) 0.076(7) 0.015(4) -0.024(5) -0.018(4) O6 0.068(7) 0.048(6) 0.084(8) 0.020(5) -0.040(6) -0.041(5) O9 0.032(4) 0.055(5) 0.032(4) 0.002(4) -0.004(3) -0.026(4) O10 0.032(4) 0.028(4) 0.024(4) 0.001(3) -0.007(3) -0.007(3) O11 0.033(4) 0.030(4) 0.049(5) 0.004(4) -0.007(4) 0.001(4) O12 0.025(4) 0.035(4) 0.029(4) -0.007(3) -0.006(3) -0.009(3) O13 0.031(4) 0.039(4) 0.052(5) -0.004(4) -0.016(4) -0.016(4) O14 0.032(4) 0.029(4) 0.024(4) -0.002(3) -0.003(3) -0.005(3) O15 0.032(5) 0.063(6) 0.045(5) -0.004(5) -0.003(4) 0.017(4) O8 0.026(4) 0.037(4) 0.032(4) 0.005(3) -0.008(3) -0.012(3) N1 0.022(4) 0.031(5) 0.021(4) -0.002(3) -0.004(3) -0.007(4) N2 0.019(4) 0.032(5) 0.023(4) -0.004(4) -0.004(3) -0.007(4) C1 0.020(5) 0.023(5) 0.023(5) -0.001(4) -0.007(4) -0.008(4) C2 0.019(5) 0.023(5) 0.024(5) -0.004(4) -0.002(4) -0.009(4) C3 0.024(5) 0.023(5) 0.029(5) -0.007(4) -0.003(4) -0.012(4) C4 0.020(5) 0.029(5) 0.018(5) -0.004(4) -0.001(4) -0.009(4) C5 0.021(5) 0.028(5) 0.022(5) -0.004(4) -0.004(4) -0.010(4) C6 0.032(6) 0.032(6) 0.030(6) -0.004(5) -0.005(5) -0.016(5) C7 0.033(6) 0.034(6) 0.031(6) 0.001(5) -0.006(5) -0.013(5) C8 0.025(5) 0.040(6) 0.021(5) -0.006(4) 0.003(4) -0.016(5) C9 0.032(6) 0.031(6) 0.025(5) 0.005(4) -0.013(5) -0.007(5) C10 0.024(5) 0.026(5) 0.035(6) 0.001(4) -0.010(5) -0.011(4) C11 0.029(5) 0.027(5) 0.032(6) -0.008(4) -0.007(5) -0.007(4) C12 0.030(5) 0.031(6) 0.023(5) 0.002(4) -0.008(4) -0.013(5) C13 0.025(5) 0.036(6) 0.025(5) -0.008(5) 0.003(4) -0.006(5) C14 0.027(5) 0.034(6) 0.031(6) -0.006(5) -0.006(5) -0.007(5) C15 0.028(5) 0.036(6) 0.021(5) -0.001(4) -0.002(4) -0.008(5) C16 0.028(5) 0.036(6) 0.019(5) -0.003(4) -0.006(4) -0.009(5) K2 0.0287(12) 0.0321(12) 0.0301(12) -0.0015(10) -0.0062(10) -0.0108(10) K3 0.0495(16) 0.0367(14) 0.0339(14) -0.0031(11) -0.0098(12) -0.0155(12) O3W 0.051(5) 0.034(4) 0.039(5) 0.003(4) -0.017(4) -0.018(4) K1 0.0538(17) 0.0398(16) 0.0594(19) -0.0200(14) -0.0091(15) -0.0104(13) O1W 0.089(9) 0.080(8) 0.076(8) -0.015(7) 0.010(7) -0.058(8) O4W 0.037(4) 0.040(5) 0.041(5) -0.002(4) -0.016(4) -0.010(4) K4 0.082(2) 0.0485(18) 0.065(2) 0.0068(15) -0.0302(19) -0.0341(17) O2W 0.101(11) 0.087(9) 0.088(9) 0.011(8) -0.038(8) -0.059(9) O7W 0.048(6) 0.073(7) 0.050(6) 0.002(5) -0.009(5) -0.016(5) O8W 0.072(7) 0.038(5) 0.065(7) 0.002(5) -0.036(6) -0.018(5) O5W 0.037(5) 0.053(6) 0.042(5) -0.008(4) -0.009(4) -0.012(4) O6W 0.077(8) 0.073(8) 0.064(7) 0.004(6) -0.033(6) -0.020(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 La1 O2 2.492(7) . ? La1 O8 2.507(7) . ? La1 O14 2.565(7) . ? La1 O12 2.576(7) . ? La1 O10 2.603(7) . ? La1 O5 2.603(7) 2_655 ? La1 O4 2.669(7) 2_655 ? La1 O1 2.679(7) . ? La1 N2 2.767(8) . ? La1 N1 2.803(9) . ? O1 C1 1.436(11) . ? O1 K2 2.990(7) . ? O2 C2 1.255(12) . ? O2 K2 2.750(8) 2_655 ? O2 K1 3.392(8) 1_465 ? O3 C2 1.236(13) . ? O3 K1 2.670(8) 1_465 ? O3 K3 2.684(8) 2_655 ? O3 K2 3.357(8) 2_655 ? O5 C4 1.247(12) . ? O5 La1 2.603(7) 2_655 ? O5 K2 2.848(7) 2_655 ? O5 K3 3.033(8) 2_655 ? O4 C4 1.261(12) . ? O4 La1 2.669(7) 2_655 ? O4 K2 2.948(8) . ? O7 C6 1.244(14) . ? O6 C6 1.258(14) . ? O6 K1 2.752(11) 2_645 ? O6 K3 3.150(11) 1_455 ? O9 C8 1.255(13) . ? O10 C10 1.259(13) . ? O10 K2 2.847(8) . ? O10 K3 3.179(8) . ? O11 C10 1.237(13) . ? O11 K4 2.769(9) . ? O12 C12 1.262(13) . ? O12 K3 2.912(8) . ? O13 C12 1.245(13) . ? O13 K4 2.650(9) 1_565 ? O14 C14 1.251(13) . ? O15 C14 1.241(14) . ? O8 C8 1.257(14) . ? N1 C9 1.457(13) . ? N1 C7 1.463(14) . ? N1 C15 1.485(13) . ? N2 C11 1.452(14) . ? N2 C13 1.476(13) . ? N2 C16 1.483(14) . ? C1 C5 1.524(13) . ? C1 C3 1.528(13) . ? C1 C2 1.529(13) . ? C3 C4 1.517(13) . ? C5 C6 1.521(15) . ? C7 C8 1.508(16) . ? C9 C10 1.514(15) . ? C11 C12 1.516(15) . ? C13 C14 1.497(16) . ? C15 C16 1.495(16) . ? K2 O2 2.750(8) 2_655 ? K2 O1W 2.795(12) . ? K2 O4W 2.796(9) . ? K2 O5 2.848(7) 2_655 ? K2 O3W 2.889(9) . ? K2 O3 3.357(8) 2_655 ? K3 O3 2.683(8) 2_655 ? K3 O6W 2.755(12) . ? K3 O5W 2.760(10) . ? K3 O4W 2.858(9) . ? K3 O5 3.033(8) 2_655 ? K3 O6 3.150(11) 1_655 ? O3W K1 2.923(9) 2_745 ? O3W K1 3.221(9) . ? K1 O3 2.670(8) 1_645 ? K1 O6 2.752(11) 2_645 ? K1 O2W 2.777(15) . ? K1 O4W 2.820(9) . ? K1 O3W 2.923(9) 2_745 ? K1 O1W 3.103(16) . ? K1 O4W 3.277(10) 2_745 ? K1 O2 3.392(8) 1_645 ? O4W K1 3.277(10) 2_745 ? K4 O13 2.650(9) 1_545 ? K4 O8W 2.727(10) . ? K4 O2W 2.854(16) . ? K4 O7W 2.947(11) . ? K4 O7W 3.012(12) 2_646 ? O7W K4 3.012(12) 2_646 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La1 O8 78.4(2) . . ? O2 La1 O14 68.5(2) . . ? O8 La1 O14 76.1(3) . . ? O2 La1 O12 145.0(2) . . ? O8 La1 O12 133.9(2) . . ? O14 La1 O12 102.3(2) . . ? O2 La1 O10 121.1(2) . . ? O8 La1 O10 102.8(2) . . ? O14 La1 O10 170.1(2) . . ? O12 La1 O10 71.1(2) . . ? O2 La1 O5 84.0(2) . 2_655 ? O8 La1 O5 151.7(2) . 2_655 ? O14 La1 O5 117.6(2) . 2_655 ? O12 La1 O5 70.2(2) . 2_655 ? O10 La1 O5 67.9(2) . 2_655 ? O2 La1 O4 75.0(2) . 2_655 ? O8 La1 O4 142.5(2) . 2_655 ? O14 La1 O4 69.7(2) . 2_655 ? O12 La1 O4 70.3(2) . 2_655 ? O10 La1 O4 113.5(2) . 2_655 ? O5 La1 O4 49.0(2) 2_655 2_655 ? O2 La1 O1 59.5(2) . . ? O8 La1 O1 76.6(2) . . ? O14 La1 O1 124.8(2) . . ? O12 La1 O1 130.8(2) . . ? O10 La1 O1 63.7(2) . . ? O5 La1 O1 75.5(2) 2_655 . ? O4 La1 O1 110.7(2) 2_655 . ? O2 La1 N2 127.5(2) . . ? O8 La1 N2 81.2(2) . . ? O14 La1 N2 59.8(2) . . ? O12 La1 N2 60.5(2) . . ? O10 La1 N2 110.3(2) . . ? O5 La1 N2 126.9(2) 2_655 . ? O4 La1 N2 94.4(2) 2_655 . ? O1 La1 N2 154.6(2) . . ? O2 La1 N1 135.8(2) . . ? O8 La1 N1 60.2(2) . . ? O14 La1 N1 112.0(2) . . ? O12 La1 N1 79.2(2) . . ? O10 La1 N1 60.2(2) . . ? O5 La1 N1 125.8(2) 2_655 . ? O4 La1 N1 148.7(2) 2_655 . ? O1 La1 N1 94.0(2) . . ? N2 La1 N1 63.9(3) . . ? O2 La1 C4 81.1(3) . 2_655 ? O8 La1 C4 159.4(3) . 2_655 ? O14 La1 C4 94.4(3) . 2_655 ? O12 La1 C4 65.6(3) . 2_655 ? O10 La1 C4 89.6(3) . 2_655 ? O5 La1 C4 24.4(2) 2_655 2_655 ? O4 La1 C4 24.8(2) 2_655 2_655 ? O1 La1 C4 94.9(2) . 2_655 ? N2 La1 C4 110.1(3) . 2_655 ? N1 La1 C4 139.9(3) . 2_655 ? O2 La1 K2 85.89(17) . . ? O8 La1 K2 116.07(18) . . ? O14 La1 K2 149.34(17) . . ? O12 La1 K2 88.89(16) . . ? O10 La1 K2 39.90(16) . . ? O5 La1 K2 39.93(15) 2_655 . ? O4 La1 K2 88.05(16) 2_655 . ? O1 La1 K2 43.39(15) . . ? N2 La1 K2 145.98(18) . . ? N1 La1 K2 98.05(18) . . ? C4 La1 K2 64.18(19) 2_655 . ? C1 O1 La1 120.5(5) . . ? C1 O1 K2 124.5(5) . . ? La1 O1 K2 98.6(2) . . ? C2 O2 La1 130.2(6) . . ? C2 O2 K2 99.7(6) . 2_655 ? La1 O2 K2 113.5(3) . 2_655 ? C2 O2 K1 77.2(6) . 1_465 ? La1 O2 K1 141.6(3) . 1_465 ? K2 O2 K1 80.87(19) 2_655 1_465 ? C2 O3 K1 112.6(6) . 1_465 ? C2 O3 K3 127.7(6) . 2_655 ? K1 O3 K3 103.0(3) 1_465 2_655 ? C2 O3 K2 72.6(6) . 2_655 ? K1 O3 K2 82.7(2) 1_465 2_655 ? K3 O3 K2 75.6(2) 2_655 2_655 ? C4 O5 La1 96.0(6) . 2_655 ? C4 O5 K2 158.5(6) . 2_655 ? La1 O5 K2 104.2(2) 2_655 2_655 ? C4 O5 K3 103.6(6) . 2_655 ? La1 O5 K3 104.1(3) 2_655 2_655 ? K2 O5 K3 78.9(2) 2_655 2_655 ? C4 O4 La1 92.6(6) . 2_655 ? C4 O4 K2 90.2(6) . . ? La1 O4 K2 102.6(2) 2_655 . ? C6 O6 K1 116.9(8) . 2_645 ? C6 O6 K3 120.1(8) . 1_455 ? K1 O6 K3 90.2(3) 2_645 1_455 ? C10 O10 La1 126.4(7) . . ? C10 O10 K2 129.3(7) . . ? La1 O10 K2 104.2(2) . . ? C10 O10 K3 95.0(6) . . ? La1 O10 K3 100.3(2) . . ? K2 O10 K3 76.53(19) . . ? C10 O11 K4 116.1(7) . . ? C12 O12 La1 118.4(6) . . ? C12 O12 K3 127.8(6) . . ? La1 O12 K3 108.3(2) . . ? C12 O13 K4 124.2(7) . 1_565 ? C14 O14 La1 124.5(7) . . ? C8 O8 La1 122.9(7) . . ? C9 N1 C7 109.5(8) . . ? C9 N1 C15 110.1(8) . . ? C7 N1 C15 109.6(8) . . ? C9 N1 La1 111.1(6) . . ? C7 N1 La1 104.2(6) . . ? C15 N1 La1 112.1(6) . . ? C11 N2 C13 109.8(8) . . ? C11 N2 C16 108.9(8) . . ? C13 N2 C16 110.5(8) . . ? C11 N2 La1 103.9(6) . . ? C13 N2 La1 110.6(6) . . ? C16 N2 La1 113.0(6) . . ? O1 C1 C5 110.6(8) . . ? O1 C1 C3 109.2(8) . . ? C5 C1 C3 110.2(8) . . ? O1 C1 C2 107.6(7) . . ? C5 C1 C2 108.2(8) . . ? C3 C1 C2 111.1(8) . . ? O3 C2 O2 124.5(9) . . ? O3 C2 C1 117.7(8) . . ? O2 C2 C1 117.8(9) . . ? O3 C2 K2 85.9(6) . 2_655 ? O2 C2 K2 57.6(5) . 2_655 ? C1 C2 K2 132.3(6) . 2_655 ? O3 C2 K1 47.5(5) . 1_465 ? O2 C2 K1 81.4(6) . 1_465 ? C1 C2 K1 151.2(6) . 1_465 ? K2 C2 K1 75.5(2) 2_655 1_465 ? C4 C3 C1 113.8(8) . . ? O5 C4 O4 121.2(9) . . ? O5 C4 C3 120.1(8) . . ? O4 C4 C3 118.7(9) . . ? O5 C4 La1 59.6(5) . 2_655 ? O4 C4 La1 62.6(5) . 2_655 ? C3 C4 La1 168.9(7) . 2_655 ? O5 C4 K2 102.6(6) . . ? O4 C4 K2 66.6(5) . . ? C3 C4 K2 100.9(6) . . ? La1 C4 K2 89.7(3) 2_655 . ? C6 C5 C1 114.5(8) . . ? O7 C6 O6 124.4(11) . . ? O7 C6 C5 118.7(9) . . ? O6 C6 C5 116.8(10) . . ? O7 C6 K1 128.9(8) . 2_645 ? O6 C6 K1 44.4(7) . 2_645 ? C5 C6 K1 96.5(6) . 2_645 ? N1 C7 C8 111.4(9) . . ? O9 C8 O8 124.8(10) . . ? O9 C8 C7 117.5(10) . . ? O8 C8 C7 117.6(9) . . ? N1 C9 C10 111.9(8) . . ? O11 C10 O10 124.6(10) . . ? O11 C10 C9 117.4(10) . . ? O10 C10 C9 117.9(9) . . ? O11 C10 K4 45.4(6) . . ? O10 C10 K4 132.4(7) . . ? C9 C10 K4 93.0(6) . . ? O11 C10 K3 87.7(7) . . ? O10 C10 K3 64.1(6) . . ? C9 C10 K3 118.7(7) . . ? K4 C10 K3 132.7(3) . . ? N2 C11 C12 112.4(8) . . ? O13 C12 O12 124.4(10) . . ? O13 C12 C11 117.7(9) . . ? O12 C12 C11 117.8(9) . . ? O13 C12 K4 38.7(5) . 1_565 ? O12 C12 K4 140.9(7) . 1_565 ? C11 C12 K4 90.0(6) . 1_565 ? N2 C13 C14 112.1(9) . . ? O15 C14 O14 123.9(11) . . ? O15 C14 C13 118.1(10) . . ? O14 C14 C13 118.0(10) . . ? N1 C15 C16 111.1(9) . . ? N2 C16 C15 111.6(9) . . ? O2 K2 O1W 140.6(3) 2_655 . ? O2 K2 O4W 106.8(2) 2_655 . ? O1W K2 O4W 76.1(4) . . ? O2 K2 O10 128.8(2) 2_655 . ? O1W K2 O10 89.9(3) . . ? O4W K2 O10 71.1(2) . . ? O2 K2 O5 69.7(2) 2_655 2_655 ? O1W K2 O5 149.5(3) . 2_655 ? O4W K2 O5 101.7(3) . 2_655 ? O10 K2 O5 61.4(2) . 2_655 ? O2 K2 O3W 70.2(2) 2_655 . ? O1W K2 O3W 72.0(3) . . ? O4W K2 O3W 78.9(2) . . ? O10 K2 O3W 148.0(2) . . ? O5 K2 O3W 138.1(2) 2_655 . ? O2 K2 O4 66.8(2) 2_655 . ? O1W K2 O4 92.3(4) . . ? O4W K2 O4 152.7(2) . . ? O10 K2 O4 134.4(2) . . ? O5 K2 O4 100.6(2) 2_655 . ? O3W K2 O4 74.0(2) . . ? O2 K2 O1 116.2(2) 2_655 . ? O1W K2 O1 89.2(3) . . ? O4W K2 O1 126.1(2) . . ? O10 K2 O1 57.0(2) . . ? O5 K2 O1 67.2(2) 2_655 . ? O3W K2 O1 144.9(2) . . ? O4 K2 O1 77.5(2) . . ? O2 K2 C2 22.7(2) 2_655 2_655 ? O1W K2 C2 155.3(3) . 2_655 ? O4W K2 C2 93.1(3) . 2_655 ? O10 K2 C2 107.8(2) . 2_655 ? O5 K2 C2 53.9(2) 2_655 2_655 ? O3W K2 C2 84.2(2) . 2_655 ? O4 K2 C2 87.4(2) . 2_655 ? O1 K2 C2 114.8(2) . 2_655 ? O2 K2 C4 73.7(2) 2_655 . ? O1W K2 C4 100.5(4) . . ? O4W K2 C4 175.4(3) . . ? O10 K2 C4 112.3(2) . . ? O5 K2 C4 82.9(2) 2_655 . ? O3W K2 C4 97.2(2) . . ? O4 K2 C4 23.1(2) . . ? O1 K2 C4 56.5(2) . . ? C2 K2 C4 88.8(3) 2_655 . ? O2 K2 O3 40.8(2) 2_655 2_655 ? O1W K2 O3 142.5(3) . 2_655 ? O4W K2 O3 71.7(2) . 2_655 ? O10 K2 O3 97.5(2) . 2_655 ? O5 K2 O3 58.49(19) 2_655 2_655 ? O3W K2 O3 83.0(2) . 2_655 ? O4 K2 O3 107.6(2) . 2_655 ? O1 K2 O3 125.54(19) . 2_655 ? C2 K2 O3 21.5(2) 2_655 2_655 ? C4 K2 O3 110.3(2) . 2_655 ? O2 K2 K3 83.58(16) 2_655 . ? O1W K2 K3 120.8(3) . . ? O4W K2 K3 49.28(19) . . ? O10 K2 K3 55.72(16) . . ? O5 K2 K3 52.72(17) 2_655 . ? O3W K2 K3 111.00(19) . . ? O4 K2 K3 146.72(17) . . ? O1 K2 K3 104.08(15) . . ? C2 K2 K3 61.35(19) 2_655 . ? C4 K2 K3 135.08(19) . . ? O3 K2 K3 44.01(14) 2_655 . ? O3 K3 O6W 134.7(3) 2_655 . ? O3 K3 O5W 93.8(3) 2_655 . ? O6W K3 O5W 96.6(3) . . ? O3 K3 O4W 81.9(2) 2_655 . ? O6W K3 O4W 73.2(3) . . ? O5W K3 O4W 159.3(3) . . ? O3 K3 O12 119.9(2) 2_655 . ? O6W K3 O12 105.4(3) . . ? O5W K3 O12 75.6(2) . . ? O4W K3 O12 124.0(2) . . ? O3 K3 O5 64.5(2) 2_655 2_655 ? O6W K3 O5 153.4(3) . 2_655 ? O5W K3 O5 100.4(2) . 2_655 ? O4W K3 O5 95.9(2) . 2_655 ? O12 K3 O5 60.1(2) . 2_655 ? O3 K3 O6 68.5(3) 2_655 1_655 ? O6W K3 O6 67.1(3) . 1_655 ? O5W K3 O6 92.0(3) . 1_655 ? O4W K3 O6 67.6(2) . 1_655 ? O12 K3 O6 165.0(2) . 1_655 ? O5 K3 O6 131.9(3) 2_655 1_655 ? O3 K3 O10 105.5(2) 2_655 . ? O6W K3 O10 97.9(3) . . ? O5W K3 O10 134.6(2) . . ? O4W K3 O10 65.6(2) . . ? O12 K3 O10 59.1(2) . . ? O5 K3 O10 55.73(19) 2_655 . ? O6 K3 O10 133.2(2) 1_655 . ? O3 K3 C10 122.8(3) 2_655 . ? O6W K3 C10 77.2(3) . . ? O5W K3 C10 134.4(3) . . ? O4W K3 C10 62.0(2) . . ? O12 K3 C10 63.3(2) . . ? O5 K3 C10 76.3(2) 2_655 . ? O6 K3 C10 124.5(2) 1_655 . ? O10 K3 C10 20.9(2) . . ? O3 K3 K2 60.36(17) 2_655 . ? O6W K3 K2 118.6(3) . . ? O5W K3 K2 144.7(2) . . ? O4W K3 K2 47.87(18) . . ? O12 K3 K2 95.92(16) . . ? O5 K3 K2 48.34(14) 2_655 . ? O6 K3 K2 99.1(2) 1_655 . ? O10 K3 K2 47.74(14) . . ? C10 K3 K2 62.52(19) . . ? O3 K3 K1 38.36(16) 2_655 2_745 ? O6W K3 K1 98.4(3) . 2_745 ? O5W K3 K1 114.9(2) . 2_745 ? O4W K3 K1 51.25(19) . 2_745 ? O12 K3 K1 152.77(17) . 2_745 ? O5 K3 K1 92.77(15) 2_655 2_745 ? O6 K3 K1 41.0(2) 1_655 2_745 ? O10 K3 K1 105.10(15) . 2_745 ? C10 K3 K1 110.63(19) . 2_745 ? K2 K3 K1 60.48(7) . 2_745 ? O3 K3 La1 98.84(17) 2_655 . ? O6W K3 La1 121.4(3) . . ? O5W K3 La1 102.39(19) . . ? O4W K3 La1 98.24(18) . . ? O12 K3 La1 33.31(14) . . ? O5 K3 La1 34.54(14) 2_655 . ? O6 K3 La1 161.7(2) 1_655 . ? O10 K3 La1 35.10(13) . . ? C10 K3 La1 50.42(17) . . ? K2 K3 La1 62.64(6) . . ? K1 K3 La1 121.09(8) 2_745 . ? K2 O3W K1 87.3(2) . 2_745 ? K2 O3W K1 88.5(2) . . ? K1 O3W K1 81.8(2) 2_745 . ? O3 K1 O6 75.2(3) 1_645 2_645 ? O3 K1 O2W 99.9(4) 1_645 . ? O6 K1 O2W 133.7(3) 2_645 . ? O3 K1 O4W 156.0(3) 1_645 . ? O6 K1 O4W 123.2(3) 2_645 . ? O2W K1 O4W 78.6(4) . . ? O3 K1 O3W 95.9(3) 1_645 2_745 ? O6 K1 O3W 137.8(3) 2_645 2_745 ? O2W K1 O3W 88.2(3) . 2_745 ? O4W K1 O3W 60.3(2) . 2_745 ? O3 K1 O1W 132.9(3) 1_645 . ? O6 K1 O1W 69.1(4) 2_645 . ? O2W K1 O1W 84.3(4) . . ? O4W K1 O1W 71.0(3) . . ? O3W K1 O1W 131.3(3) 2_745 . ? O3 K1 O3W 115.8(2) 1_645 . ? O6 K1 O3W 53.7(2) 2_645 . ? O2W K1 O3W 142.6(4) . . ? O4W K1 O3W 73.1(2) . . ? O3W K1 O3W 98.2(2) 2_745 . ? O1W K1 O3W 63.8(3) . . ? O3 K1 O4W 74.5(2) 1_645 2_745 ? O6 K1 O4W 66.9(3) 2_645 2_745 ? O2W K1 O4W 157.5(3) . 2_745 ? O4W K1 O4W 97.6(2) . 2_745 ? O3W K1 O4W 71.0(2) 2_745 2_745 ? O1W K1 O4W 115.7(3) . 2_745 ? O3W K1 O4W 52.7(2) . 2_745 ? O3 K1 C2 19.9(2) 1_645 1_645 ? O6 K1 C2 95.1(3) 2_645 1_645 ? O2W K1 C2 85.9(4) . 1_645 ? O4W K1 C2 138.6(3) . 1_645 ? O3W K1 C2 81.3(2) 2_745 1_645 ? O1W K1 C2 145.4(3) . 1_645 ? O3W K1 C2 131.5(3) . 1_645 ? O4W K1 C2 82.6(2) 2_745 1_645 ? O3 K1 O2 40.5(2) 1_645 1_645 ? O6 K1 O2 114.8(3) 2_645 1_645 ? O2W K1 O2 78.5(4) . 1_645 ? O4W K1 O2 117.2(2) . 1_645 ? O3W K1 O2 61.3(2) 2_745 1_645 ? O1W K1 O2 158.6(3) . 1_645 ? O3W K1 O2 136.5(2) . 1_645 ? O4W K1 O2 83.8(2) 2_745 1_645 ? C2 K1 O2 21.5(2) 1_645 1_645 ? O3 K1 C6 76.5(2) 1_645 2_645 ? O6 K1 C6 18.7(3) 2_645 2_645 ? O2W K1 C6 115.0(3) . 2_645 ? O4W K1 C6 126.1(3) . 2_645 ? O3W K1 C6 156.3(3) 2_745 2_645 ? O1W K1 C6 59.9(3) . 2_645 ? O3W K1 C6 66.5(2) . 2_645 ? O4W K1 C6 85.3(2) 2_745 2_645 ? C2 K1 C6 95.3(3) 1_645 2_645 ? O2 K1 C6 116.7(2) 1_645 2_645 ? O3 K1 K2 56.04(18) 1_645 2_745 ? O6 K1 K2 100.3(2) 2_645 2_745 ? O2W K1 K2 115.0(3) . 2_745 ? O4W K1 K2 102.53(19) . 2_745 ? O3W K1 K2 45.98(19) 2_745 2_745 ? O1W K1 K2 158.6(3) . 2_745 ? O3W K1 K2 94.87(19) . 2_745 ? O4W K1 K2 43.67(16) 2_745 2_745 ? C2 K1 K2 50.75(17) 1_645 2_745 ? O2 K1 K2 42.58(13) 1_645 2_745 ? C6 K1 K2 114.78(19) 2_645 2_745 ? K2 O1W K1 92.6(4) . . ? K2 O4W K1 99.0(3) . . ? K2 O4W K3 82.9(2) . . ? K1 O4W K3 167.8(4) . . ? K2 O4W K1 82.3(2) . 2_745 ? K1 O4W K1 82.4(2) . 2_745 ? K3 O4W K1 85.9(2) . 2_745 ? O13 K4 O8W 89.1(3) 1_545 . ? O13 K4 O11 162.7(3) 1_545 . ? O8W K4 O11 96.8(3) . . ? O13 K4 O2W 88.7(3) 1_545 . ? O8W K4 O2W 100.7(4) . . ? O11 K4 O2W 74.2(3) . . ? O13 K4 O7W 91.5(3) 1_545 . ? O8W K4 O7W 106.1(4) . . ? O11 K4 O7W 102.4(3) . . ? O2W K4 O7W 153.3(4) . . ? O13 K4 O7W 115.4(3) 1_545 2_646 ? O8W K4 O7W 155.6(3) . 2_646 ? O11 K4 O7W 59.9(3) . 2_646 ? O2W K4 O7W 81.2(3) . 2_646 ? O7W K4 O7W 74.6(3) . 2_646 ? O13 K4 C10 176.8(3) 1_545 . ? O8W K4 C10 87.7(3) . . ? O11 K4 C10 18.5(2) . . ? O2W K4 C10 91.7(3) . . ? O7W K4 C10 89.5(3) . . ? O7W K4 C10 67.8(3) 2_646 . ? O13 K4 C12 17.1(2) 1_545 1_545 ? O8W K4 C12 74.7(3) . 1_545 ? O11 K4 C12 169.1(3) . 1_545 ? O2W K4 C12 100.3(3) . 1_545 ? O7W K4 C12 86.7(3) . 1_545 ? O7W K4 C12 129.3(3) 2_646 1_545 ? C10 K4 C12 160.2(3) . 1_545 ? O13 K4 K4 106.8(2) 1_545 2_646 ? O8W K4 K4 138.6(3) . 2_646 ? O11 K4 K4 79.3(2) . 2_646 ? O2W K4 K4 117.2(3) . 2_646 ? O7W K4 K4 37.8(2) . 2_646 ? O7W K4 K4 36.8(2) 2_646 2_646 ? C10 K4 K4 75.8(2) . 2_646 ? C12 K4 K4 111.5(2) 1_545 2_646 ? O13 K4 K1 102.3(2) 1_545 . ? O8W K4 K1 78.1(3) . . ? O11 K4 K1 63.36(19) . . ? O2W K4 K1 26.6(3) . . ? O7W K4 K1 165.7(3) . . ? O7W K4 K1 95.9(2) 2_646 . ? C10 K4 K1 76.88(19) . . ? C12 K4 K1 107.58(19) 1_545 . ? K4 K4 K1 131.88(12) 2_646 . ? K1 O2W K4 125.9(6) . . ? K4 O7W K4 105.4(3) . 2_646 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.355 _refine_diff_density_min -0.804 _refine_diff_density_rms 0.161 # Attachment 'cif4.cif' data_sad4 _database_code_depnum_ccdc_archive 'CCDC 837351' #TrackingRef 'cif4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Potassium ethylenediaminietetraacetato lanthanum malate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H60 K6 La2 N4 O40' _chemical_formula_weight 1605.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8421(3) _cell_length_b 11.2798(5) _cell_length_c 13.7733(5) _cell_angle_alpha 72.370(4) _cell_angle_beta 72.257(3) _cell_angle_gamma 88.654(3) _cell_volume 1383.94(9) _cell_formula_units_Z 1 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.926 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 2.084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6807 _exptl_absorpt_correction_T_max 0.8187 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(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 'Oxford CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13227 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4858 _reflns_number_gt 4064 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0185P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4858 _refine_ls_number_parameters 406 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0469 _refine_ls_wR_factor_gt 0.0459 _refine_ls_goodness_of_fit_ref 0.922 _refine_ls_restrained_S_all 0.922 _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 La1 La 0.859313(19) 0.248944(18) 0.218574(14) 0.01098(6) Uani 1 1 d . . . K1 K 0.24975(7) 0.37990(7) 0.24015(5) 0.02010(16) Uani 1 1 d . . . K2 K 0.97735(7) 0.37818(7) -0.14345(5) 0.02337(17) Uani 1 1 d . . . K3 K 0.61371(8) 0.17756(7) -0.01558(6) 0.02841(18) Uani 1 1 d . . . O10 O 0.9349(2) 0.3967(2) 0.30492(16) 0.0171(5) Uani 1 1 d . . . O11 O 1.0255(2) 0.4093(2) 0.43174(17) 0.0276(6) Uani 1 1 d . . . O8 O 0.5903(2) 0.2182(2) 0.30076(15) 0.0168(5) Uani 1 1 d . . . O9 O 0.4074(2) 0.3126(2) 0.37940(17) 0.0284(6) Uani 1 1 d . . . O12 O 1.0661(2) 0.1624(2) 0.28698(16) 0.0193(5) Uani 1 1 d . . . O13 O 1.2169(2) 0.0129(2) 0.27997(17) 0.0241(5) Uani 1 1 d . . . O14 O 0.7854(2) 0.0662(2) 0.16076(16) 0.0210(5) Uani 1 1 d . . . O15 O 0.6640(2) -0.1163(2) 0.20029(17) 0.0215(5) Uani 1 1 d . . . O1 O 0.7563(2) 0.4686(2) 0.17086(16) 0.0176(5) Uani 1 1 d D . . O2 O 0.7783(2) 0.32227(19) 0.05705(15) 0.0154(5) Uani 1 1 d . . . O3 O 0.6537(2) 0.4344(2) -0.04545(16) 0.0220(5) Uani 1 1 d . . . O4 O 0.9155(2) 0.7784(2) -0.05569(16) 0.0222(5) Uani 1 1 d . . . O5 O 0.9195(2) 0.6004(2) -0.09054(16) 0.0177(5) Uani 1 1 d . . . N1 N 0.7328(2) 0.2146(2) 0.43867(18) 0.0133(5) Uani 1 1 d . . . N2 N 0.8312(2) 0.0036(2) 0.35352(18) 0.0138(6) Uani 1 1 d . . . C9 C 0.8315(3) 0.2613(3) 0.4833(2) 0.0176(7) Uani 1 1 d . . . H9A H 0.8828 0.1927 0.5135 0.021 Uiso 1 1 calc R . . H9B H 0.7760 0.2918 0.5411 0.021 Uiso 1 1 calc R . . C10 C 0.9379(3) 0.3643(3) 0.4012(2) 0.0159(7) Uani 1 1 d . . . C7 C 0.6101(3) 0.2909(3) 0.4420(2) 0.0178(7) Uani 1 1 d . . . H7A H 0.6434 0.3782 0.4197 0.021 Uiso 1 1 calc R . . H7B H 0.5464 0.2693 0.5151 0.021 Uiso 1 1 calc R . . C8 C 0.5276(3) 0.2726(3) 0.3695(2) 0.0160(7) Uani 1 1 d . . . C11 C 0.9727(3) -0.0424(3) 0.3147(2) 0.0177(7) Uani 1 1 d . . . H11A H 0.9801 -0.0613 0.2492 0.021 Uiso 1 1 calc R . . H11B H 0.9812 -0.1191 0.3678 0.021 Uiso 1 1 calc R . . C12 C 1.0954(3) 0.0514(3) 0.2931(2) 0.0155(7) Uani 1 1 d . . . C13 C 0.7221(3) -0.0705(3) 0.3402(2) 0.0173(7) Uani 1 1 d . . . H13A H 0.6284 -0.0570 0.3834 0.021 Uiso 1 1 calc R . . H13B H 0.7371 -0.1583 0.3660 0.021 Uiso 1 1 calc R . . C14 C 0.7254(3) -0.0373(3) 0.2241(2) 0.0167(7) Uani 1 1 d . . . C15 C 0.6848(3) 0.0824(3) 0.4985(2) 0.0169(7) Uani 1 1 d . . . H15A H 0.5994 0.0612 0.4842 0.020 Uiso 1 1 calc R . . H15B H 0.6602 0.0705 0.5748 0.020 Uiso 1 1 calc R . . C16 C 0.7989(3) -0.0040(3) 0.4678(2) 0.0177(7) Uani 1 1 d . . . H16A H 0.8854 0.0185 0.4801 0.021 Uiso 1 1 calc R . . H16B H 0.7663 -0.0891 0.5127 0.021 Uiso 1 1 calc R . . C1 C 0.6737(3) 0.5017(3) 0.0974(2) 0.0162(7) Uani 1 1 d . . . H1A H 0.5721 0.4875 0.1398 0.019 Uiso 1 1 calc R . . C2 C 0.7047(3) 0.4138(3) 0.0304(2) 0.0172(7) Uani 1 1 d . . . C3 C 0.7032(3) 0.6381(3) 0.0317(2) 0.0152(7) Uani 1 1 d . . . H3A H 0.6816 0.6880 0.0801 0.018 Uiso 1 1 calc R . . H3B H 0.6391 0.6586 -0.0114 0.018 Uiso 1 1 calc R . . C4 C 0.8563(3) 0.6738(3) -0.0421(2) 0.0142(7) Uani 1 1 d . . . O1W O 0.2418(3) 0.4192(3) 0.52828(19) 0.0366(7) Uani 1 1 d D . . O2W O 0.9380(3) 0.1236(2) -0.07428(19) 0.0414(7) Uani 1 1 d D . . O3W O 0.1837(3) 0.6161(3) 0.2723(2) 0.0418(7) Uani 1 1 d D . . O4W O 0.4316(2) 0.2028(2) 0.16912(17) 0.0234(5) Uani 1 1 d D . . O5W O 0.6285(2) 0.1791(2) -0.22601(19) 0.0277(6) Uani 1 1 d D . . O6W O 0.6784(4) -0.0604(3) -0.0102(2) 0.0617(10) Uani 1 1 d D . . O7W O 1.2601(3) 0.3620(2) -0.27179(18) 0.0293(6) Uani 1 1 d D . . H1W1 H 0.1601(17) 0.416(3) 0.513(2) 0.035 Uiso 1 1 d D . . H1W2 H 0.298(2) 0.378(3) 0.487(2) 0.035 Uiso 1 1 d D . . H2W1 H 0.935(3) 0.119(3) -0.0083(13) 0.035 Uiso 1 1 d D . . H2W2 H 0.893(3) 0.0510(19) -0.064(2) 0.035 Uiso 1 1 d D . . H3W1 H 0.137(3) 0.579(3) 0.3413(11) 0.035 Uiso 1 1 d D . . H3W2 H 0.240(3) 0.676(2) 0.274(2) 0.035 Uiso 1 1 d D . . H4W1 H 0.481(3) 0.207(3) 0.212(2) 0.035 Uiso 1 1 d D . . H4W2 H 0.368(3) 0.138(2) 0.210(2) 0.035 Uiso 1 1 d D . . H5W1 H 0.680(3) 0.118(2) -0.243(3) 0.035 Uiso 1 1 d D . . H5W2 H 0.5430(15) 0.159(3) -0.228(3) 0.035 Uiso 1 1 d D . . H6W1 H 0.675(3) -0.077(3) 0.0582(10) 0.035 Uiso 1 1 d D . . H6W2 H 0.763(2) -0.084(3) -0.040(2) 0.035 Uiso 1 1 d D . . H7W1 H 1.253(4) 0.381(3) -0.3373(13) 0.035 Uiso 1 1 d D . . H7W2 H 1.296(3) 0.2884(17) -0.261(2) 0.035 Uiso 1 1 d D . . H1 H 0.743(4) 0.516(3) 0.214(2) 0.035 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01056(9) 0.01147(9) 0.01072(9) -0.00334(7) -0.00305(6) -0.00083(7) K1 0.0172(4) 0.0222(4) 0.0212(4) -0.0049(3) -0.0081(3) 0.0009(3) K2 0.0232(4) 0.0215(4) 0.0228(4) -0.0077(3) -0.0026(3) -0.0014(3) K3 0.0314(4) 0.0238(4) 0.0338(5) -0.0157(4) -0.0089(3) 0.0026(3) O10 0.0175(11) 0.0178(12) 0.0152(12) -0.0052(9) -0.0036(9) -0.0038(9) O11 0.0255(13) 0.0356(15) 0.0273(13) -0.0119(11) -0.0133(10) -0.0082(11) O8 0.0124(11) 0.0256(13) 0.0160(11) -0.0092(10) -0.0065(9) 0.0002(9) O9 0.0165(12) 0.0467(16) 0.0312(14) -0.0220(12) -0.0115(10) 0.0128(11) O12 0.0167(11) 0.0168(13) 0.0239(12) -0.0036(10) -0.0084(9) -0.0005(10) O13 0.0139(12) 0.0236(13) 0.0362(14) -0.0105(11) -0.0090(10) 0.0047(10) O14 0.0307(13) 0.0146(12) 0.0176(12) -0.0049(10) -0.0070(10) -0.0051(10) O15 0.0253(12) 0.0168(12) 0.0279(13) -0.0079(10) -0.0147(10) -0.0014(10) O1 0.0235(12) 0.0187(12) 0.0142(11) -0.0065(9) -0.0097(9) 0.0027(10) O2 0.0178(11) 0.0155(12) 0.0143(11) -0.0046(9) -0.0073(9) 0.0043(9) O3 0.0244(12) 0.0250(13) 0.0195(12) -0.0027(10) -0.0147(10) -0.0007(10) O4 0.0220(12) 0.0182(13) 0.0243(13) -0.0099(10) -0.0001(10) -0.0061(10) O5 0.0142(11) 0.0173(12) 0.0186(11) -0.0068(10) 0.0006(9) -0.0001(9) N1 0.0108(13) 0.0171(14) 0.0130(13) -0.0049(11) -0.0052(10) 0.0007(11) N2 0.0106(13) 0.0179(14) 0.0122(13) -0.0045(11) -0.0024(10) -0.0018(11) C9 0.0180(17) 0.0211(18) 0.0173(17) -0.0067(14) -0.0098(13) 0.0002(14) C10 0.0159(16) 0.0166(17) 0.0193(18) -0.0095(14) -0.0078(13) 0.0052(13) C7 0.0163(16) 0.0195(18) 0.0182(17) -0.0090(14) -0.0032(13) 0.0014(14) C8 0.0161(17) 0.0159(17) 0.0152(16) -0.0028(14) -0.0055(13) -0.0015(14) C11 0.0178(17) 0.0144(17) 0.0222(17) -0.0056(14) -0.0081(13) 0.0033(13) C12 0.0167(17) 0.0187(18) 0.0107(16) -0.0025(13) -0.0058(13) -0.0003(14) C13 0.0159(16) 0.0150(17) 0.0194(17) -0.0034(14) -0.0052(13) -0.0011(13) C14 0.0117(16) 0.0179(18) 0.0215(17) -0.0082(15) -0.0050(13) 0.0037(14) C15 0.0160(16) 0.0202(18) 0.0105(16) -0.0002(14) -0.0024(12) -0.0047(14) C16 0.0192(17) 0.0173(18) 0.0155(16) -0.0008(14) -0.0078(13) -0.0031(14) C1 0.0099(15) 0.0196(18) 0.0174(16) -0.0036(14) -0.0038(12) 0.0015(13) C2 0.0118(16) 0.0155(18) 0.0184(17) -0.0013(14) 0.0003(13) -0.0062(13) C3 0.0133(16) 0.0165(17) 0.0157(16) -0.0054(13) -0.0041(12) 0.0032(13) C4 0.0168(16) 0.0141(17) 0.0141(16) -0.0033(14) -0.0094(13) 0.0032(14) O1W 0.0308(15) 0.0614(19) 0.0333(15) -0.0302(14) -0.0179(12) 0.0219(14) O2W 0.072(2) 0.0285(16) 0.0289(15) -0.0141(12) -0.0174(14) 0.0051(14) O3W 0.0545(18) 0.0370(17) 0.0310(15) -0.0053(13) -0.0126(13) -0.0234(14) O4W 0.0210(13) 0.0298(14) 0.0212(13) -0.0069(11) -0.0098(10) -0.0020(10) O5W 0.0210(13) 0.0248(14) 0.0389(14) -0.0150(12) -0.0068(11) 0.0026(11) O6W 0.128(3) 0.0289(17) 0.0233(15) -0.0126(13) -0.0145(17) 0.0299(19) O7W 0.0487(16) 0.0227(14) 0.0256(14) -0.0147(11) -0.0181(12) 0.0131(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O2 2.4908(19) . ? La1 O8 2.5279(19) . ? La1 O12 2.549(2) . ? La1 O10 2.558(2) . ? La1 O5 2.599(2) 2_765 ? La1 O14 2.614(2) . ? La1 O1 2.627(2) . ? La1 O4 2.720(2) 2_765 ? La1 N2 2.792(2) . ? La1 N1 2.811(2) . ? K1 O9 2.745(2) . ? K1 O3 2.760(2) 2_665 ? K1 O4W 2.846(2) . ? K1 O3W 2.860(3) . ? K1 O12 2.871(2) 1_455 ? K1 O10 2.971(2) 1_455 ? K1 O5 2.978(2) 2_665 ? K1 O11 2.982(2) 1_455 ? K2 O3W 2.703(3) 2_665 ? K2 O2W 2.733(3) . ? K2 O2 2.751(2) . ? K2 O10 2.766(2) 2_765 ? K2 O5 2.815(2) . ? K2 O7W 2.842(3) . ? K2 O1 3.035(2) 2_765 ? K2 O3 3.190(2) . ? K2 O4 3.240(2) 2_765 ? K3 O4W 2.721(2) . ? K3 O6W 2.728(3) . ? K3 O3 2.820(2) . ? K3 O5W 2.852(2) . ? K3 O2 2.897(2) . ? K3 O6W 3.068(4) 2_655 ? K3 O2W 3.138(3) . ? K3 O14 3.299(2) . ? O10 C10 1.275(3) . ? O10 K2 2.766(2) 2_765 ? O10 K1 2.971(2) 1_655 ? O11 C10 1.243(4) . ? O11 K1 2.982(2) 1_655 ? O8 C8 1.277(4) . ? O9 C8 1.239(3) . ? O12 C12 1.262(4) . ? O12 K1 2.871(2) 1_655 ? O13 C12 1.242(3) . ? O14 C14 1.254(4) . ? O15 C14 1.261(4) . ? O1 C1 1.443(3) . ? O1 K2 3.035(2) 2_765 ? O2 C2 1.274(4) . ? O3 C2 1.251(4) . ? O3 K1 2.760(2) 2_665 ? O4 C4 1.264(4) . ? O4 La1 2.720(2) 2_765 ? O4 K2 3.240(2) 2_765 ? O5 C4 1.255(3) . ? O5 La1 2.5994(19) 2_765 ? O5 K1 2.978(2) 2_665 ? N1 C7 1.464(4) . ? N1 C15 1.475(4) . ? N1 C9 1.478(4) . ? N2 C13 1.464(4) . ? N2 C11 1.475(4) . ? N2 C16 1.483(4) . ? C9 C10 1.505(4) . ? C7 C8 1.525(4) . ? C11 C12 1.521(4) . ? C13 C14 1.518(4) . ? C15 C16 1.516(4) . ? C1 C3 1.513(4) . ? C1 C2 1.515(4) . ? C3 C4 1.521(4) . ? O3W K2 2.703(3) 2_665 ? O6W K3 3.068(4) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La1 O8 78.10(6) . . ? O2 La1 O12 144.70(7) . . ? O8 La1 O12 133.43(7) . . ? O2 La1 O10 123.26(7) . . ? O8 La1 O10 104.03(6) . . ? O12 La1 O10 70.80(7) . . ? O2 La1 O5 81.39(6) . 2_765 ? O8 La1 O5 147.33(7) . 2_765 ? O12 La1 O5 75.33(7) . 2_765 ? O10 La1 O5 67.15(6) . 2_765 ? O2 La1 O14 66.97(7) . . ? O8 La1 O14 75.60(7) . . ? O12 La1 O14 101.74(7) . . ? O10 La1 O14 169.67(6) . . ? O5 La1 O14 118.72(6) 2_765 . ? O2 La1 O1 60.06(6) . . ? O8 La1 O1 72.17(7) . . ? O12 La1 O1 135.25(7) . . ? O10 La1 O1 66.84(6) . . ? O5 La1 O1 75.61(6) 2_765 . ? O14 La1 O1 121.98(7) . . ? O2 La1 O4 75.42(6) . 2_765 ? O8 La1 O4 144.47(6) . 2_765 ? O12 La1 O4 69.28(7) . 2_765 ? O10 La1 O4 110.18(6) . 2_765 ? O5 La1 O4 48.76(6) 2_765 2_765 ? O14 La1 O4 72.47(6) . 2_765 ? O1 La1 O4 112.84(6) . 2_765 ? O2 La1 N2 126.03(7) . . ? O8 La1 N2 79.95(7) . . ? O12 La1 N2 60.57(7) . . ? O10 La1 N2 109.67(7) . . ? O5 La1 N2 132.67(7) 2_765 . ? O14 La1 N2 60.00(7) . . ? O1 La1 N2 149.52(6) . . ? O4 La1 N2 96.96(7) 2_765 . ? O2 La1 N1 135.12(7) . . ? O8 La1 N1 59.85(6) . . ? O12 La1 N1 80.14(7) . . ? O10 La1 N1 59.91(7) . . ? O5 La1 N1 126.40(7) 2_765 . ? O14 La1 N1 112.51(7) . . ? O1 La1 N1 90.68(7) . . ? O4 La1 N1 149.29(7) 2_765 . ? N2 La1 N1 64.21(7) . . ? O2 La1 C4 79.08(7) . 2_765 ? O8 La1 C4 157.16(7) . 2_765 ? O12 La1 C4 68.78(7) . 2_765 ? O10 La1 C4 87.63(7) . 2_765 ? O5 La1 C4 24.24(7) 2_765 2_765 ? O14 La1 C4 96.39(7) . 2_765 ? O1 La1 C4 95.37(7) . 2_765 ? O4 La1 C4 24.64(7) 2_765 2_765 ? N2 La1 C4 114.97(7) . 2_765 ? N1 La1 C4 141.28(7) . 2_765 ? O2 La1 K2 87.18(5) . 2_765 ? O8 La1 K2 113.17(5) . 2_765 ? O12 La1 K2 91.69(5) . 2_765 ? O10 La1 K2 38.87(5) . 2_765 ? O5 La1 K2 40.22(5) 2_765 2_765 ? O14 La1 K2 150.93(5) . 2_765 ? O1 La1 K2 45.24(5) . 2_765 ? O4 La1 K2 88.83(5) 2_765 2_765 ? N2 La1 K2 146.71(5) . 2_765 ? N1 La1 K2 95.02(5) . 2_765 ? C4 La1 K2 64.45(6) 2_765 2_765 ? O9 K1 O3 122.57(7) . 2_665 ? O9 K1 O4W 75.47(7) . . ? O3 K1 O4W 94.09(7) 2_665 . ? O9 K1 O3W 95.84(7) . . ? O3 K1 O3W 70.92(7) 2_665 . ? O4W K1 O3W 155.40(7) . . ? O9 K1 O12 105.35(7) . 1_455 ? O3 K1 O12 126.05(6) 2_665 1_455 ? O4W K1 O12 74.06(6) . 1_455 ? O3W K1 O12 130.50(7) . 1_455 ? O9 K1 O10 124.87(6) . 1_455 ? O3 K1 O10 103.29(6) 2_665 1_455 ? O4W K1 O10 133.60(7) . 1_455 ? O3W K1 O10 70.26(7) . 1_455 ? O12 K1 O10 60.84(6) 1_455 1_455 ? O9 K1 O5 168.53(7) . 2_665 ? O3 K1 O5 63.96(6) 2_665 2_665 ? O4W K1 O5 95.20(6) . 2_665 ? O3W K1 O5 95.35(7) . 2_665 ? O12 K1 O5 65.06(6) 1_455 2_665 ? O10 K1 O5 57.31(5) 1_455 2_665 ? O9 K1 O11 83.13(6) . 1_455 ? O3 K1 O11 124.05(7) 2_665 1_455 ? O4W K1 O11 141.86(7) . 1_455 ? O3W K1 O11 56.58(7) . 1_455 ? O12 K1 O11 81.88(6) 1_455 1_455 ? O10 K1 O11 43.99(6) 1_455 1_455 ? O5 K1 O11 101.00(6) 2_665 1_455 ? O9 K1 C10 101.15(7) . 1_455 ? O3 K1 C10 122.47(7) 2_665 1_455 ? O4W K1 C10 134.76(8) . 1_455 ? O3W K1 C10 69.06(8) . 1_455 ? O12 K1 C10 63.26(7) 1_455 1_455 ? O10 K1 C10 23.71(6) 1_455 1_455 ? O5 K1 C10 80.52(7) 2_665 1_455 ? O11 K1 C10 23.10(6) 1_455 1_455 ? O9 K1 C4 148.78(7) . 2_665 ? O3 K1 C4 66.13(7) 2_665 2_665 ? O4W K1 C4 73.94(7) . 2_665 ? O3W K1 C4 114.71(7) . 2_665 ? O12 K1 C4 59.98(6) 1_455 2_665 ? O10 K1 C4 74.59(6) 1_455 2_665 ? O5 K1 C4 21.27(6) 2_665 2_665 ? O11 K1 C4 118.34(7) 1_455 2_665 ? C10 K1 C4 95.90(7) 1_455 2_665 ? O9 K1 K2 142.35(6) . 2_665 ? O3 K1 K2 57.26(5) 2_665 2_665 ? O4W K1 K2 139.73(5) . 2_665 ? O3W K1 K2 46.78(5) . 2_665 ? O12 K1 K2 99.17(5) 1_455 2_665 ? O10 K1 K2 47.69(4) 1_455 2_665 ? O5 K1 K2 48.62(4) 2_665 2_665 ? O11 K1 K2 72.44(5) 1_455 2_665 ? C10 K1 K2 65.24(6) 1_455 2_665 ? C4 K1 K2 68.78(5) 2_665 2_665 ? O9 K1 La1 136.92(5) . 1_455 ? O3 K1 La1 100.28(5) 2_665 1_455 ? O4W K1 La1 99.06(5) . 1_455 ? O3W K1 La1 102.69(6) . 1_455 ? O12 K1 La1 35.38(4) 1_455 1_455 ? O10 K1 La1 35.99(4) 1_455 1_455 ? O5 K1 La1 36.82(4) 2_665 1_455 ? O11 K1 La1 75.67(4) 1_455 1_455 ? C10 K1 La1 52.57(6) 1_455 1_455 ? C4 K1 La1 44.72(5) 2_665 1_455 ? K2 K1 La1 63.989(16) 2_665 1_455 ? O3W K2 O2W 88.79(9) 2_665 . ? O3W K2 O2 103.20(7) 2_665 . ? O2W K2 O2 75.68(7) . . ? O3W K2 O10 75.70(7) 2_665 2_765 ? O2W K2 O10 151.51(7) . 2_765 ? O2 K2 O10 130.70(7) . 2_765 ? O3W K2 O5 102.92(8) 2_665 . ? O2W K2 O5 146.65(7) . . ? O2 K2 O5 71.29(6) . . ? O10 K2 O5 61.48(6) 2_765 . ? O3W K2 O7W 104.03(8) 2_665 . ? O2W K2 O7W 89.43(8) . . ? O2 K2 O7W 148.54(7) . . ? O10 K2 O7W 71.87(6) 2_765 . ? O5 K2 O7W 116.92(7) . . ? O3W K2 O1 133.09(7) 2_665 2_765 ? O2W K2 O1 126.17(8) . 2_765 ? O2 K2 O1 114.30(6) . 2_765 ? O10 K2 O1 58.77(6) 2_765 2_765 ? O5 K2 O1 66.28(6) . 2_765 ? O7W K2 O1 53.66(6) . 2_765 ? O3W K2 C2 89.09(8) 2_665 . ? O2W K2 C2 94.61(8) . . ? O2 K2 C2 24.06(7) . . ? O10 K2 C2 108.64(7) 2_765 . ? O5 K2 C2 55.15(7) . . ? O7W K2 C2 166.37(8) . . ? O1 K2 C2 114.33(7) 2_765 . ? O3W K2 O3 66.62(7) 2_665 . ? O2W K2 O3 97.69(8) . . ? O2 K2 O3 43.44(6) . . ? O10 K2 O3 97.78(6) 2_765 . ? O5 K2 O3 60.55(6) . . ? O7W K2 O3 167.96(6) . . ? O1 K2 O3 126.61(6) 2_765 . ? C2 K2 O3 22.85(7) . . ? O3W K2 O4 148.64(7) 2_665 2_765 ? O2W K2 O4 60.90(7) . 2_765 ? O2 K2 O4 63.79(6) . 2_765 ? O10 K2 O4 135.03(6) 2_765 2_765 ? O5 K2 O4 99.41(6) . 2_765 ? O7W K2 O4 84.75(6) . 2_765 ? O1 K2 O4 76.36(5) 2_765 2_765 ? C2 K2 O4 85.86(7) . 2_765 ? O3 K2 O4 107.19(5) . 2_765 ? O3W K2 C4 170.33(8) 2_665 2_765 ? O2W K2 C4 82.70(8) . 2_765 ? O2 K2 C4 70.30(7) . 2_765 ? O10 K2 C4 113.94(7) 2_765 2_765 ? O5 K2 C4 82.08(7) . 2_765 ? O7W K2 C4 80.54(7) . 2_765 ? O1 K2 C4 56.46(6) 2_765 2_765 ? C2 K2 C4 87.05(8) . 2_765 ? O3 K2 C4 109.90(7) . 2_765 ? O4 K2 C4 22.09(6) 2_765 2_765 ? O3W K2 K1 50.44(6) 2_665 2_665 ? O2W K2 K1 131.45(7) . 2_665 ? O2 K2 K1 88.09(5) . 2_665 ? O10 K2 K1 52.59(4) 2_765 2_665 ? O5 K2 K1 52.54(5) . 2_665 ? O7W K2 K1 121.66(5) . 2_665 ? O1 K2 K1 102.29(5) 2_765 2_665 ? C2 K2 K1 64.23(6) . 2_665 ? O3 K2 K1 46.71(4) . 2_665 ? O4 K2 K1 146.89(4) 2_765 2_665 ? C4 K2 K1 134.30(6) 2_765 2_665 ? O4W K3 O6W 115.62(8) . . ? O4W K3 O3 77.35(7) . . ? O6W K3 O3 159.57(10) . . ? O4W K3 O5W 142.67(7) . . ? O6W K3 O5W 77.98(7) . . ? O3 K3 O5W 101.47(7) . . ? O4W K3 O2 74.54(6) . . ? O6W K3 O2 119.57(9) . . ? O3 K3 O2 46.02(6) . . ? O5W K3 O2 131.20(6) . . ? O4W K3 O6W 73.95(7) . 2_655 ? O6W K3 O6W 79.05(10) . 2_655 ? O3 K3 O6W 120.85(7) . 2_655 ? O5W K3 O6W 75.18(7) . 2_655 ? O2 K3 O6W 148.12(7) . 2_655 ? O4W K3 C2 68.53(7) . . ? O6W K3 C2 143.54(10) . . ? O3 K3 C2 23.56(7) . . ? O5W K3 C2 122.15(8) . . ? O2 K3 C2 24.02(7) . . ? O6W K3 C2 132.68(8) 2_655 . ? O4W K3 O2W 130.35(7) . . ? O6W K3 O2W 62.49(9) . . ? O3 K3 O2W 97.09(7) . . ? O5W K3 O2W 86.97(7) . . ? O2 K3 O2W 67.64(6) . . ? O6W K3 O2W 140.30(7) 2_655 . ? C2 K3 O2W 86.85(8) . . ? O4W K3 O14 76.60(6) . . ? O6W K3 O14 70.47(8) . . ? O3 K3 O14 99.31(6) . . ? O5W K3 O14 138.87(6) . . ? O2 K3 O14 53.63(5) . . ? O6W K3 O14 121.94(7) 2_655 . ? C2 K3 O14 76.03(7) . . ? O2W K3 O14 55.38(6) . . ? O4W K3 K2 118.14(5) . . ? O6W K3 K2 105.82(8) . . ? O3 K3 K2 53.91(5) . . ? O5W K3 K2 87.72(5) . . ? O2 K3 K2 44.89(4) . . ? O6W K3 K2 160.99(6) 2_655 . ? C2 K3 K2 51.29(5) . . ? O2W K3 K2 44.15(5) . . ? O14 K3 K2 76.55(4) . . ? O4W K3 K3 94.25(6) . 2_655 ? O6W K3 K3 42.29(8) . 2_655 ? O3 K3 K3 157.31(5) . 2_655 ? O5W K3 K3 72.41(5) . 2_655 ? O2 K3 K3 151.98(5) . 2_655 ? O6W K3 K3 36.76(5) 2_655 2_655 ? C2 K3 K3 162.71(6) . 2_655 ? O2W K3 K3 104.23(5) . 2_655 ? O14 K3 K3 99.14(4) . 2_655 ? K2 K3 K3 144.50(3) . 2_655 ? O4W K3 K1 101.71(5) . 2_665 ? O6W K3 K1 142.24(7) . 2_665 ? O3 K3 K1 26.69(4) . 2_665 ? O5W K3 K1 75.52(5) . 2_665 ? O2 K3 K1 63.89(4) . 2_665 ? O6W K3 K1 118.63(5) 2_655 2_665 ? C2 K3 K1 46.97(6) . 2_665 ? O2W K3 K1 89.57(5) . 2_665 ? O14 K3 K1 115.67(4) . 2_665 ? K2 K3 K1 47.138(16) . 2_665 ? K3 K3 K1 144.13(3) 2_655 2_665 ? C10 O10 La1 124.23(19) . . ? C10 O10 K2 129.95(19) . 2_765 ? La1 O10 K2 105.65(7) . 2_765 ? C10 O10 K1 86.68(16) . 1_655 ? La1 O10 K1 100.98(7) . 1_655 ? K2 O10 K1 79.72(5) 2_765 1_655 ? C10 O11 K1 86.70(17) . 1_655 ? C8 O8 La1 119.58(18) . . ? C8 O9 K1 131.97(19) . . ? C12 O12 La1 119.31(19) . . ? C12 O12 K1 130.33(18) . 1_655 ? La1 O12 K1 103.93(7) . 1_655 ? C14 O14 La1 124.89(19) . . ? C14 O14 K3 109.50(18) . . ? La1 O14 K3 108.91(7) . . ? C1 O1 La1 121.82(17) . . ? C1 O1 K2 123.26(17) . 2_765 ? La1 O1 K2 96.84(6) . 2_765 ? C2 O2 La1 129.23(18) . . ? C2 O2 K2 94.26(16) . . ? La1 O2 K2 119.33(8) . . ? C2 O2 K3 88.23(17) . . ? La1 O2 K3 127.14(8) . . ? K2 O2 K3 87.11(6) . . ? C2 O3 K1 126.37(19) . 2_665 ? C2 O3 K3 92.19(18) . . ? K1 O3 K3 126.00(8) 2_665 . ? C2 O3 K2 75.28(17) . . ? K1 O3 K2 76.03(5) 2_665 . ? K3 O3 K2 80.50(6) . . ? C4 O4 La1 91.59(18) . 2_765 ? C4 O4 K2 83.42(17) . 2_765 ? La1 O4 K2 98.45(7) 2_765 2_765 ? C4 O5 La1 97.53(18) . 2_765 ? C4 O5 K2 159.24(19) . . ? La1 O5 K2 103.17(7) 2_765 . ? C4 O5 K1 99.37(17) . 2_665 ? La1 O5 K1 99.83(6) 2_765 2_665 ? K2 O5 K1 78.83(6) . 2_665 ? C7 N1 C15 110.5(2) . . ? C7 N1 C9 109.8(2) . . ? C15 N1 C9 110.6(2) . . ? C7 N1 La1 103.29(16) . . ? C15 N1 La1 111.15(17) . . ? C9 N1 La1 111.22(16) . . ? C13 N2 C11 109.4(2) . . ? C13 N2 C16 110.5(2) . . ? C11 N2 C16 110.1(2) . . ? C13 N2 La1 110.56(17) . . ? C11 N2 La1 103.48(16) . . ? C16 N2 La1 112.61(18) . . ? N1 C9 C10 113.1(2) . . ? O11 C10 O10 124.6(3) . . ? O11 C10 C9 117.5(3) . . ? O10 C10 C9 117.9(3) . . ? O11 C10 K1 70.20(16) . 1_655 ? O10 C10 K1 69.61(15) . 1_655 ? C9 C10 K1 135.7(2) . 1_655 ? N1 C7 C8 112.1(2) . . ? O9 C8 O8 124.7(3) . . ? O9 C8 C7 118.8(3) . . ? O8 C8 C7 116.6(3) . . ? N2 C11 C12 112.7(3) . . ? O13 C12 O12 125.4(3) . . ? O13 C12 C11 117.2(3) . . ? O12 C12 C11 117.5(3) . . ? N2 C13 C14 112.2(2) . . ? O14 C14 O15 125.5(3) . . ? O14 C14 C13 118.1(3) . . ? O15 C14 C13 116.3(3) . . ? N1 C15 C16 112.0(2) . . ? N2 C16 C15 111.0(2) . . ? O1 C1 C3 111.2(2) . . ? O1 C1 C2 107.9(2) . . ? C3 C1 C2 113.7(2) . . ? O3 C2 O2 124.6(3) . . ? O3 C2 C1 117.9(3) . . ? O2 C2 C1 117.5(3) . . ? O3 C2 K2 81.87(17) . . ? O2 C2 K2 61.68(14) . . ? C1 C2 K2 132.95(19) . . ? O3 C2 K3 64.25(17) . . ? O2 C2 K3 67.75(16) . . ? C1 C2 K3 149.45(19) . . ? K2 C2 K3 77.13(7) . . ? C1 C3 C4 114.2(2) . . ? O5 C4 O4 121.5(3) . . ? O5 C4 C3 119.3(3) . . ? O4 C4 C3 119.2(3) . . ? O5 C4 La1 58.23(15) . 2_765 ? O4 C4 La1 63.76(15) . 2_765 ? C3 C4 La1 170.7(2) . 2_765 ? O5 C4 K2 98.38(18) . 2_765 ? O4 C4 K2 74.49(16) . 2_765 ? C3 C4 K2 98.91(17) . 2_765 ? La1 C4 K2 90.40(7) 2_765 2_765 ? O5 C4 K1 59.36(15) . 2_665 ? O4 C4 K1 120.87(19) . 2_665 ? C3 C4 K1 88.33(17) . 2_665 ? La1 C4 K1 82.84(7) 2_765 2_665 ? K2 C4 K1 156.92(10) 2_765 2_665 ? K2 O2W K3 82.77(8) . . ? K2 O3W K1 82.79(7) 2_665 . ? K3 O4W K1 139.32(9) . . ? K3 O6W K3 100.95(10) . 2_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.674 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.085 # Attachment 'cif5.cif' data_sad5 _database_code_depnum_ccdc_archive 'CCDC 837352' #TrackingRef 'cif5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Potassium ethylenediaminietetraacetato cerium malate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H60 Ce2 K6 N4 O40' _chemical_formula_weight 1607.64 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' K K 0.2009 0.2494 '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' _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 9.8381(3) _cell_length_b 11.2618(4) _cell_length_c 13.7843(5) _cell_angle_alpha 72.303(3) _cell_angle_beta 72.095(3) _cell_angle_gamma 88.588(2) _cell_volume 1380.49(8) _cell_formula_units_Z 1 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.934 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 806 _exptl_absorpt_coefficient_mu 2.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5144 _exptl_absorpt_correction_T_max 0.7347 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(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 'Oxford CCD diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24860 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5401 _reflns_number_gt 4964 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1184P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5401 _refine_ls_number_parameters 406 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1459 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.093 _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 Ce1 Ce 0.63978(2) 0.75111(2) -0.21952(2) 0.01156(14) Uani 1 1 d . . . C1 C 0.8254(6) 0.4982(5) -0.0988(4) 0.0200(11) Uani 1 1 d . . . H1A H 0.9270 0.5127 -0.1417 0.024 Uiso 1 1 calc R . . C2 C 0.7944(5) 0.5858(5) -0.0313(4) 0.0180(10) Uani 1 1 d . . . C3 C 0.7967(5) 0.3608(5) -0.0317(4) 0.0162(10) Uani 1 1 d . . . H3A H 0.8607 0.3415 0.0114 0.019 Uiso 1 1 calc R . . H3B H 0.8192 0.3103 -0.0796 0.019 Uiso 1 1 calc R . . C4 C 0.6421(5) 0.3239(5) 0.0430(4) 0.0146(10) Uani 1 1 d . . . C7 C 0.8896(5) 0.7085(5) -0.4412(4) 0.0153(10) Uani 1 1 d . . . H7A H 0.9543 0.7307 -0.5142 0.018 Uiso 1 1 calc R . . H7B H 0.8568 0.6210 -0.4193 0.018 Uiso 1 1 calc R . . C8 C 0.9703(5) 0.7273(5) -0.3675(4) 0.0170(10) Uani 1 1 d . . . C9 C 0.6679(5) 0.7383(5) -0.4829(4) 0.0184(11) Uani 1 1 d . . . H9A H 0.7237 0.7074 -0.5404 0.022 Uiso 1 1 calc R . . H9B H 0.6164 0.8067 -0.5133 0.022 Uiso 1 1 calc R . . C10 C 0.5611(5) 0.6346(5) -0.3992(4) 0.0155(10) Uani 1 1 d . . . C11 C 0.7780(5) 1.0702(5) -0.3401(4) 0.0169(10) Uani 1 1 d . . . H11A H 0.7622 1.1581 -0.3653 0.020 Uiso 1 1 calc R . . H11B H 0.8720 1.0575 -0.3837 0.020 Uiso 1 1 calc R . . C12 C 0.7744(5) 1.0357(5) -0.2241(4) 0.0161(10) Uani 1 1 d . . . C13 C 0.5279(5) 1.0418(5) -0.3147(5) 0.0187(11) Uani 1 1 d . . . H13A H 0.5193 1.1186 -0.3678 0.022 Uiso 1 1 calc R . . H13B H 0.5205 1.0607 -0.2492 0.022 Uiso 1 1 calc R . . C14 C 0.4065(5) 0.9471(5) -0.2929(4) 0.0165(10) Uani 1 1 d . . . C15 C 0.8150(5) 0.9173(5) -0.4991(4) 0.0166(10) Uani 1 1 d . . . H15A H 0.8390 0.9290 -0.5753 0.020 Uiso 1 1 calc R . . H15B H 0.9009 0.9383 -0.4854 0.020 Uiso 1 1 calc R . . C16 C 0.7010(5) 1.0038(5) -0.4677(4) 0.0166(10) Uani 1 1 d . . . H16A H 0.7338 1.0892 -0.5124 0.020 Uiso 1 1 calc R . . H16B H 0.6144 0.9816 -0.4799 0.020 Uiso 1 1 calc R . . O1 O 0.7415(4) 0.5311(4) -0.1717(3) 0.0193(8) Uani 1 1 d D . . H1 H 0.772(6) 0.477(5) -0.209(4) 0.023 Uiso 1 1 d D . . O2 O 0.7194(4) 0.6776(3) -0.0593(3) 0.0152(7) Uani 1 1 d . . . O3 O 0.8449(4) 0.5662(4) 0.0432(3) 0.0247(9) Uani 1 1 d . . . O4 O 0.5842(4) 0.2197(4) 0.0576(3) 0.0232(8) Uani 1 1 d . . . O5 O 0.5797(4) 0.3987(3) 0.0909(3) 0.0181(8) Uani 1 1 d . . . O8 O 0.9067(4) 0.7816(3) -0.2994(3) 0.0163(7) Uani 1 1 d . . . O9 O 1.0909(4) 0.6877(4) -0.3775(3) 0.0308(10) Uani 1 1 d . . . O10 O 0.5631(4) 0.6036(4) -0.3041(3) 0.0188(8) Uani 1 1 d . . . O11 O 0.4732(4) 0.5900(4) -0.4303(3) 0.0289(10) Uani 1 1 d . . . O12 O 0.7135(4) 0.9322(3) -0.1615(3) 0.0209(8) Uani 1 1 d . . . O13 O 0.8349(4) 1.1139(4) -0.1998(3) 0.0230(8) Uani 1 1 d . . . O14 O 0.4349(4) 0.8366(3) -0.2876(3) 0.0187(8) Uani 1 1 d . . . O15 O 0.2826(4) 0.9862(4) -0.2801(3) 0.0257(9) Uani 1 1 d . . . N1 N 0.7655(4) 0.7851(4) -0.4382(3) 0.0143(8) Uani 1 1 d . . . N2 N 0.6688(4) 0.9953(4) -0.3536(3) 0.0144(8) Uani 1 1 d . . . K1 K 0.88397(15) 0.82142(12) 0.01648(11) 0.0302(3) Uani 1 1 d . . . K2 K 0.52187(13) 0.62172(12) 0.14259(10) 0.0250(3) Uani 1 1 d . . . K3 K 0.24905(12) 0.61990(11) -0.23894(9) 0.0205(3) Uani 1 1 d . . . O1W O 0.8228(9) 1.0617(5) 0.0100(4) 0.067(2) Uani 1 1 d D . . O2W O 0.5628(6) 0.8764(4) 0.0727(4) 0.0445(13) Uani 1 1 d D . . O3W O 0.3149(6) 0.3830(5) -0.2699(4) 0.0445(13) Uani 1 1 d D . . O4W O 1.0664(4) 0.7972(4) -0.1688(3) 0.0222(8) Uani 1 1 d D . . O5W O 0.8719(4) 0.8215(4) 0.2265(4) 0.0291(9) Uani 1 1 d D . . O6W O 0.7423(5) 0.4190(5) 0.5271(4) 0.0371(11) Uani 1 1 d D . . O7W O 0.2385(5) 0.6391(4) 0.2731(4) 0.0315(10) Uani 1 1 d D . . H3W1 H 0.356(7) 0.429(5) -0.3389(17) 0.038 Uiso 1 1 d D . . H3W2 H 0.265(6) 0.322(4) -0.277(4) 0.038 Uiso 1 1 d D . . H6W1 H 0.800(5) 0.383(6) 0.482(5) 0.038 Uiso 1 1 d D . . H7W1 H 0.207(8) 0.716(3) 0.260(5) 0.038 Uiso 1 1 d D . . H6W2 H 0.658(3) 0.412(7) 0.516(5) 0.038 Uiso 1 1 d D . . H7W2 H 0.249(8) 0.627(5) 0.338(3) 0.038 Uiso 1 1 d D . . H4W1 H 1.121(6) 0.868(4) -0.211(4) 0.038 Uiso 1 1 d D . . H4W2 H 1.009(6) 0.792(6) -0.207(4) 0.038 Uiso 1 1 d D . . H5W1 H 0.815(5) 0.881(4) 0.243(6) 0.038 Uiso 1 1 d D . . H1W1 H 0.876(5) 1.087(7) -0.0595(17) 0.038 Uiso 1 1 d D . . H2W1 H 0.555(8) 0.9590(16) 0.061(4) 0.038 Uiso 1 1 d D . . H5W2 H 0.958(3) 0.854(5) 0.220(6) 0.038 Uiso 1 1 d D . . H2W2 H 0.583(8) 0.872(5) 0.006(2) 0.038 Uiso 1 1 d D . . H1W2 H 0.736(3) 1.049(8) 0.005(5) 0.038 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.01088(18) 0.01258(19) 0.01162(19) -0.00375(12) -0.00404(12) -0.00007(11) C1 0.016(2) 0.018(3) 0.021(3) -0.005(2) -0.001(2) 0.001(2) C2 0.015(2) 0.017(3) 0.019(3) -0.001(2) -0.006(2) -0.0003(19) C3 0.013(2) 0.017(3) 0.016(2) -0.003(2) -0.0031(19) 0.0041(19) C4 0.014(2) 0.016(2) 0.013(2) -0.002(2) -0.0064(19) 0.0026(19) C7 0.014(2) 0.020(3) 0.016(2) -0.010(2) -0.007(2) 0.0042(19) C8 0.014(2) 0.023(3) 0.014(2) -0.004(2) -0.005(2) 0.001(2) C9 0.016(2) 0.025(3) 0.019(3) -0.007(2) -0.012(2) 0.001(2) C10 0.013(2) 0.019(3) 0.020(3) -0.012(2) -0.007(2) 0.0033(19) C11 0.013(2) 0.017(3) 0.021(3) -0.005(2) -0.008(2) -0.0026(19) C12 0.011(2) 0.017(3) 0.024(3) -0.008(2) -0.010(2) 0.0062(18) C13 0.015(2) 0.018(3) 0.024(3) -0.007(2) -0.008(2) 0.004(2) C14 0.017(2) 0.021(3) 0.013(2) -0.004(2) -0.007(2) 0.002(2) C15 0.016(2) 0.021(3) 0.010(2) -0.002(2) -0.0029(19) -0.003(2) C16 0.016(2) 0.018(3) 0.015(2) -0.001(2) -0.009(2) 0.0007(19) O1 0.0234(19) 0.020(2) 0.0178(19) -0.0041(15) -0.0132(16) 0.0052(15) O2 0.0168(17) 0.0138(17) 0.0169(18) -0.0052(14) -0.0081(14) 0.0062(13) O3 0.025(2) 0.027(2) 0.023(2) -0.0023(17) -0.0148(17) -0.0013(16) O4 0.0204(19) 0.022(2) 0.025(2) -0.0112(17) -0.0005(16) -0.0031(15) O5 0.0155(17) 0.0177(19) 0.0184(19) -0.0053(15) -0.0020(15) 0.0007(14) O8 0.0108(16) 0.025(2) 0.0167(18) -0.0079(15) -0.0081(14) 0.0018(14) O9 0.0180(19) 0.052(3) 0.031(2) -0.022(2) -0.0119(17) 0.0120(18) O10 0.0195(18) 0.0197(19) 0.0191(19) -0.0076(16) -0.0069(15) -0.0029(15) O11 0.025(2) 0.039(3) 0.029(2) -0.013(2) -0.0144(18) -0.0086(18) O12 0.030(2) 0.0166(19) 0.0167(19) -0.0032(15) -0.0099(16) -0.0031(16) O13 0.026(2) 0.020(2) 0.029(2) -0.0075(17) -0.0154(17) -0.0013(15) O14 0.0136(17) 0.0164(19) 0.027(2) -0.0055(16) -0.0087(15) 0.0015(14) O15 0.0150(18) 0.029(2) 0.034(2) -0.0088(18) -0.0105(17) 0.0054(16) N1 0.0115(19) 0.022(2) 0.013(2) -0.0059(17) -0.0082(16) 0.0014(16) N2 0.0134(19) 0.015(2) 0.016(2) -0.0049(17) -0.0064(16) 0.0001(16) K1 0.0348(7) 0.0255(7) 0.0352(7) -0.0161(6) -0.0114(6) 0.0058(5) K2 0.0261(6) 0.0231(6) 0.0242(6) -0.0078(5) -0.0051(5) 0.0008(5) K3 0.0171(5) 0.0241(6) 0.0219(6) -0.0058(5) -0.0097(5) 0.0029(4) O1W 0.140(6) 0.032(3) 0.027(3) -0.013(2) -0.022(3) 0.032(4) O2W 0.077(4) 0.032(3) 0.034(3) -0.019(2) -0.022(3) 0.014(2) O3W 0.058(3) 0.041(3) 0.035(3) -0.008(2) -0.017(2) -0.019(2) O4W 0.0166(18) 0.030(2) 0.023(2) -0.0051(17) -0.0142(16) 0.0018(15) O5W 0.021(2) 0.028(2) 0.039(2) -0.014(2) -0.0078(19) 0.0002(16) O6W 0.036(2) 0.058(3) 0.033(2) -0.028(2) -0.021(2) 0.024(2) O7W 0.054(3) 0.023(2) 0.025(2) -0.0127(18) -0.020(2) 0.013(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 Ce1 O2 2.469(3) . ? Ce1 O8 2.502(3) . ? Ce1 O14 2.528(4) . ? Ce1 O10 2.543(4) . ? Ce1 O5 2.580(3) 2_665 ? Ce1 O12 2.597(4) . ? Ce1 O1 2.620(4) . ? Ce1 O4 2.707(4) 2_665 ? Ce1 N2 2.772(4) . ? Ce1 N1 2.792(4) . ? C1 O1 1.448(7) . ? C1 C2 1.517(8) . ? C1 C3 1.523(7) . ? C2 O3 1.233(7) . ? C2 O2 1.288(6) . ? C3 C4 1.534(7) . ? C4 O4 1.250(6) . ? C4 O5 1.259(6) . ? C7 N1 1.475(6) . ? C7 C8 1.530(7) . ? C8 O9 1.240(6) . ? C8 O8 1.272(6) . ? C9 N1 1.472(6) . ? C9 C10 1.514(7) . ? C10 O11 1.251(6) . ? C10 O10 1.257(6) . ? C11 N2 1.470(6) . ? C11 C12 1.516(7) . ? C12 O12 1.252(6) . ? C12 O13 1.253(6) . ? C13 N2 1.470(6) . ? C13 C14 1.517(7) . ? C14 O14 1.254(6) . ? C14 O15 1.264(6) . ? C15 N1 1.478(7) . ? C15 C16 1.516(7) . ? C16 N2 1.479(7) . ? O1 K2 2.999(4) 2_665 ? O2 K2 2.754(4) . ? O2 K1 2.921(4) . ? O3 K3 2.766(4) 2_665 ? O3 K1 2.805(4) . ? O3 K2 3.180(4) . ? O4 Ce1 2.707(4) 2_665 ? O4 K2 3.252(4) 2_665 ? O5 Ce1 2.580(3) 2_665 ? O5 K2 2.812(4) . ? O5 K3 2.981(4) 2_665 ? O9 K3 2.745(4) 1_655 ? O10 K2 2.760(4) 2_665 ? O10 K3 2.959(4) . ? O11 K3 2.977(4) . ? O12 K1 3.309(4) . ? O14 K3 2.867(4) . ? K1 O4W 2.720(4) . ? K1 O1W 2.738(6) . ? K1 O5W 2.861(5) . ? K1 O1W 3.072(9) 2_775 ? K1 O2W 3.108(6) . ? K2 O3W 2.708(5) 2_665 ? K2 O2W 2.731(5) . ? K2 O10 2.760(4) 2_665 ? K2 O7W 2.855(5) . ? K2 O1 2.999(4) 2_665 ? K2 O4 3.252(4) 2_665 ? K2 C4 3.325(5) 2_665 ? K3 O9 2.745(4) 1_455 ? K3 O3 2.766(4) 2_665 ? K3 O4W 2.843(4) 1_455 ? K3 O3W 2.856(6) . ? K3 O5 2.981(4) 2_665 ? O1W K1 3.072(9) 2_775 ? O3W K2 2.708(5) 2_665 ? O4W K3 2.843(4) 1_655 ? 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 Ce1 O8 77.67(11) . . ? O2 Ce1 O14 144.81(12) . . ? O8 Ce1 O14 133.82(12) . . ? O2 Ce1 O10 123.02(12) . . ? O8 Ce1 O10 104.86(12) . . ? O14 Ce1 O10 70.46(12) . . ? O2 Ce1 O5 80.83(12) . 2_665 ? O8 Ce1 O5 147.01(12) . 2_665 ? O14 Ce1 O5 75.62(12) . 2_665 ? O10 Ce1 O5 67.15(12) . 2_665 ? O2 Ce1 O12 66.81(12) . . ? O8 Ce1 O12 75.17(12) . . ? O14 Ce1 O12 102.19(12) . . ? O10 Ce1 O12 170.12(12) . . ? O5 Ce1 O12 118.26(12) 2_665 . ? O2 Ce1 O1 60.04(11) . . ? O8 Ce1 O1 72.33(12) . . ? O14 Ce1 O1 134.87(12) . . ? O10 Ce1 O1 66.73(12) . . ? O5 Ce1 O1 75.32(11) 2_665 . ? O12 Ce1 O1 121.88(12) . . ? O2 Ce1 O4 75.41(12) . 2_665 ? O8 Ce1 O4 143.64(12) . 2_665 ? O14 Ce1 O4 69.41(13) . 2_665 ? O10 Ce1 O4 110.18(12) . 2_665 ? O5 Ce1 O4 49.00(11) 2_665 2_665 ? O12 Ce1 O4 72.01(12) . 2_665 ? O1 Ce1 O4 113.08(12) . 2_665 ? O2 Ce1 N2 126.03(12) . . ? O8 Ce1 N2 79.98(12) . . ? O14 Ce1 N2 60.84(12) . . ? O10 Ce1 N2 109.98(12) . . ? O5 Ce1 N2 133.01(12) 2_665 . ? O12 Ce1 N2 60.16(12) . . ? O1 Ce1 N2 149.59(12) . . ? O4 Ce1 N2 96.63(12) 2_665 . ? O2 Ce1 N1 135.25(11) . . ? O8 Ce1 N1 60.53(11) . . ? O14 Ce1 N1 79.92(12) . . ? O10 Ce1 N1 60.18(12) . . ? O5 Ce1 N1 126.71(12) 2_665 . ? O12 Ce1 N1 112.79(12) . . ? O1 Ce1 N1 90.74(12) . . ? O4 Ce1 N1 149.14(13) 2_665 . ? N2 Ce1 N1 64.26(13) . . ? O2 Ce1 C4 78.62(12) . 2_665 ? O8 Ce1 C4 156.28(12) . 2_665 ? O14 Ce1 C4 69.08(13) . 2_665 ? O10 Ce1 C4 87.85(13) . 2_665 ? O5 Ce1 C4 24.56(13) 2_665 2_665 ? O12 Ce1 C4 95.72(13) . 2_665 ? O1 Ce1 C4 95.42(13) . 2_665 ? O4 Ce1 C4 24.55(13) 2_665 2_665 ? N2 Ce1 C4 114.89(13) . 2_665 ? N1 Ce1 C4 141.70(12) . 2_665 ? O2 Ce1 K2 86.64(8) . 2_665 ? O8 Ce1 K2 113.16(9) . 2_665 ? O14 Ce1 K2 91.89(8) . 2_665 ? O10 Ce1 K2 38.96(9) . 2_665 ? O5 Ce1 K2 40.38(8) 2_665 2_665 ? O12 Ce1 K2 150.34(8) . 2_665 ? O1 Ce1 K2 44.73(8) . 2_665 ? O4 Ce1 K2 89.24(8) 2_665 2_665 ? N2 Ce1 K2 147.27(9) . 2_665 ? N1 Ce1 K2 95.18(9) . 2_665 ? C4 Ce1 K2 64.93(10) 2_665 2_665 ? O1 C1 C2 108.0(4) . . ? O1 C1 C3 111.6(4) . . ? C2 C1 C3 113.0(4) . . ? O3 C2 O2 125.3(5) . . ? O3 C2 C1 118.4(5) . . ? O2 C2 C1 116.2(5) . . ? O3 C2 K2 81.9(3) . . ? O2 C2 K2 62.1(3) . . ? C1 C2 K2 133.0(3) . . ? O3 C2 K1 63.6(3) . . ? O2 C2 K1 68.8(3) . . ? C1 C2 K1 149.8(3) . . ? K2 C2 K1 76.68(13) . . ? C1 C3 C4 114.3(4) . . ? O4 C4 O5 122.1(4) . . ? O4 C4 C3 119.5(5) . . ? O5 C4 C3 118.3(4) . . ? O4 C4 Ce1 64.2(3) . 2_665 ? O5 C4 Ce1 58.4(2) . 2_665 ? C3 C4 Ce1 170.2(3) . 2_665 ? O4 C4 K2 75.8(3) . 2_665 ? O5 C4 K2 98.2(3) . 2_665 ? C3 C4 K2 98.6(3) . 2_665 ? Ce1 C4 K2 91.10(13) 2_665 2_665 ? O4 C4 K3 120.7(3) . 2_665 ? O5 C4 K3 59.3(3) . 2_665 ? C3 C4 K3 87.7(3) . 2_665 ? Ce1 C4 K3 82.87(12) 2_665 2_665 ? K2 C4 K3 156.51(17) 2_665 2_665 ? N1 C7 C8 111.7(4) . . ? O9 C8 O8 124.9(5) . . ? O9 C8 C7 118.2(5) . . ? O8 C8 C7 116.9(4) . . ? N1 C9 C10 112.3(4) . . ? O11 C10 O10 125.0(5) . . ? O11 C10 C9 116.5(5) . . ? O10 C10 C9 118.4(4) . . ? O11 C10 K3 70.2(3) . . ? O10 C10 K3 69.4(3) . . ? C9 C10 K3 135.6(3) . . ? N2 C11 C12 112.0(4) . . ? O12 C12 O13 125.7(5) . . ? O12 C12 C11 117.9(4) . . ? O13 C12 C11 116.4(5) . . ? N2 C13 C14 111.8(4) . . ? O14 C14 O15 124.7(5) . . ? O14 C14 C13 118.4(4) . . ? O15 C14 C13 116.8(5) . . ? N1 C15 C16 111.3(4) . . ? N2 C16 C15 111.1(4) . . ? C1 O1 Ce1 121.7(3) . . ? C1 O1 K2 123.2(3) . 2_665 ? Ce1 O1 K2 97.34(11) . 2_665 ? C2 O2 Ce1 130.2(3) . . ? C2 O2 K2 93.5(3) . . ? Ce1 O2 K2 120.00(13) . . ? C2 O2 K1 86.9(3) . . ? Ce1 O2 K1 127.68(14) . . ? K2 O2 K1 85.95(10) . . ? C2 O3 K3 126.7(3) . 2_665 ? C2 O3 K1 93.3(3) . . ? K3 O3 K1 124.94(15) 2_665 . ? C2 O3 K2 75.6(3) . . ? K3 O3 K2 76.27(10) 2_665 . ? K1 O3 K2 80.31(11) . . ? C4 O4 Ce1 91.3(3) . 2_665 ? C4 O4 K2 82.4(3) . 2_665 ? Ce1 O4 K2 98.42(12) 2_665 2_665 ? C4 O5 Ce1 97.1(3) . 2_665 ? C4 O5 K2 159.7(3) . . ? Ce1 O5 K2 103.15(12) 2_665 . ? C4 O5 K3 99.4(3) . 2_665 ? Ce1 O5 K3 99.88(12) 2_665 2_665 ? K2 O5 K3 78.97(10) . 2_665 ? C8 O8 Ce1 119.5(3) . . ? C8 O9 K3 132.3(4) . 1_655 ? C10 O10 Ce1 124.4(3) . . ? C10 O10 K2 129.9(3) . 2_665 ? Ce1 O10 K2 105.62(13) . 2_665 ? C10 O10 K3 87.2(3) . . ? Ce1 O10 K3 101.35(12) . . ? K2 O10 K3 80.18(10) 2_665 . ? C10 O11 K3 86.5(3) . . ? C12 O12 Ce1 125.2(3) . . ? C12 O12 K1 108.8(3) . . ? Ce1 O12 K1 109.54(13) . . ? C14 O14 Ce1 118.5(3) . . ? C14 O14 K3 130.3(3) . . ? Ce1 O14 K3 104.28(13) . . ? C9 N1 C7 109.9(4) . . ? C9 N1 C15 110.6(4) . . ? C7 N1 C15 109.8(4) . . ? C9 N1 Ce1 111.6(3) . . ? C7 N1 Ce1 103.0(3) . . ? C15 N1 Ce1 111.6(3) . . ? C13 N2 C11 108.9(4) . . ? C13 N2 C16 110.0(4) . . ? C11 N2 C16 110.5(4) . . ? C13 N2 Ce1 103.5(3) . . ? C11 N2 Ce1 110.8(3) . . ? C16 N2 Ce1 112.9(3) . . ? O4W K1 O1W 114.91(16) . . ? O4W K1 O3 76.85(12) . . ? O1W K1 O3 160.5(2) . . ? O4W K1 O5W 142.29(12) . . ? O1W K1 O5W 77.79(15) . . ? O3 K1 O5W 102.71(13) . . ? O4W K1 O2 74.07(11) . . ? O1W K1 O2 119.81(18) . . ? O3 K1 O2 45.99(10) . . ? O5W K1 O2 132.59(12) . . ? O4W K1 O1W 73.80(13) . 2_775 ? O1W K1 O1W 78.4(2) . 2_775 ? O3 K1 O1W 120.76(14) . 2_775 ? O5W K1 O1W 74.59(13) . 2_775 ? O2 K1 O1W 147.55(13) . 2_775 ? O4W K1 O2W 129.75(13) . . ? O1W K1 O2W 63.1(2) . . ? O3 K1 O2W 97.38(13) . . ? O5W K1 O2W 87.93(13) . . ? O2 K1 O2W 67.61(11) . . ? O1W K1 O2W 140.43(14) 2_775 . ? O4W K1 C2 68.22(13) . . ? O1W K1 C2 144.1(2) . . ? O3 K1 C2 23.18(13) . . ? O5W K1 C2 123.13(14) . . ? O2 K1 C2 24.27(12) . . ? O1W K1 C2 132.29(15) 2_775 . ? O2W K1 C2 87.02(13) . . ? O4W K1 O12 75.99(11) . . ? O1W K1 O12 71.20(16) . . ? O3 K1 O12 98.40(11) . . ? O5W K1 O12 139.61(12) . . ? O2 K1 O12 52.79(10) . . ? O1W K1 O12 121.90(13) 2_775 . ? O2W K1 O12 55.23(12) . . ? C2 K1 O12 75.46(12) . . ? O4W K1 K2 117.96(9) . . ? O1W K1 K2 106.64(19) . . ? O3 K1 K2 54.10(9) . . ? O5W K1 K2 88.72(9) . . ? O2 K1 K2 45.22(7) . . ? O1W K1 K2 161.30(11) 2_775 . ? O2W K1 K2 44.42(9) . . ? C2 K1 K2 51.47(10) . . ? O12 K1 K2 76.39(7) . . ? O4W K1 K1 93.77(10) . 2_775 ? O1W K1 K1 41.91(19) . 2_775 ? O3 K1 K1 157.13(10) . 2_775 ? O5W K1 K1 71.96(9) . 2_775 ? O2 K1 K1 151.33(9) . 2_775 ? O1W K1 K1 36.54(10) 2_775 2_775 ? O2W K1 K1 104.50(10) . 2_775 ? C2 K1 K1 161.94(11) . 2_775 ? O12 K1 K1 99.46(8) . 2_775 ? K2 K1 K1 145.06(5) . 2_775 ? O4W K1 K3 101.64(9) . 2_665 ? O1W K1 K3 143.13(15) . 2_665 ? O3 K1 K3 27.32(8) . 2_665 ? O5W K1 K3 76.11(9) . 2_665 ? O2 K1 K3 64.65(7) . 2_665 ? O1W K1 K3 118.28(11) 2_775 2_665 ? O2W K1 K3 90.32(10) . 2_665 ? C2 K1 K3 47.34(10) . 2_665 ? O12 K1 K3 115.69(7) . 2_665 ? K2 K1 K3 47.58(3) . 2_665 ? K1 K1 K3 144.01(5) 2_775 2_665 ? O3W K2 O2W 88.44(16) 2_665 . ? O3W K2 O2 103.32(14) 2_665 . ? O2W K2 O2 75.50(14) . . ? O3W K2 O10 75.60(13) 2_665 2_665 ? O2W K2 O10 151.70(14) . 2_665 ? O2 K2 O10 130.48(12) . 2_665 ? O3W K2 O5 102.73(15) 2_665 . ? O2W K2 O5 146.66(14) . . ? O2 K2 O5 71.40(10) . . ? O10 K2 O5 61.13(11) 2_665 . ? O3W K2 O7W 103.91(15) 2_665 . ? O2W K2 O7W 89.48(15) . . ? O2 K2 O7W 148.38(12) . . ? O10 K2 O7W 72.39(12) 2_665 . ? O5 K2 O7W 117.24(12) . . ? O3W K2 O1 133.14(14) 2_665 2_665 ? O2W K2 O1 126.70(15) . 2_665 ? O2 K2 O1 114.06(11) . 2_665 ? O10 K2 O1 58.93(11) 2_665 2_665 ? O5 K2 O1 66.19(10) . 2_665 ? O7W K2 O1 54.12(12) . 2_665 ? O3W K2 C2 88.72(16) 2_665 . ? O2W K2 C2 94.37(16) . . ? O2 K2 C2 24.39(12) . . ? O10 K2 C2 108.22(13) 2_665 . ? O5 K2 C2 55.25(12) . . ? O7W K2 C2 166.90(14) . . ? O1 K2 C2 114.40(13) 2_665 . ? O3W K2 O3 66.52(14) 2_665 . ? O2W K2 O3 97.27(15) . . ? O2 K2 O3 43.61(10) . . ? O10 K2 O3 97.50(11) 2_665 . ? O5 K2 O3 60.58(10) . . ? O7W K2 O3 167.98(12) . . ? O1 K2 O3 126.54(11) 2_665 . ? C2 K2 O3 22.57(12) . . ? O3W K2 O4 148.01(13) 2_665 2_665 ? O2W K2 O4 60.70(13) . 2_665 ? O2 K2 O4 63.11(10) . 2_665 ? O10 K2 O4 135.87(11) 2_665 2_665 ? O5 K2 O4 99.80(11) . 2_665 ? O7W K2 O4 85.26(11) . 2_665 ? O1 K2 O4 77.07(10) 2_665 2_665 ? C2 K2 O4 85.72(12) . 2_665 ? O3 K2 O4 106.71(10) . 2_665 ? O3W K2 C4 169.41(14) 2_665 2_665 ? O2W K2 C4 82.30(14) . 2_665 ? O2 K2 C4 69.44(11) . 2_665 ? O10 K2 C4 114.94(12) 2_665 2_665 ? O5 K2 C4 82.61(12) . 2_665 ? O7W K2 C4 81.22(13) . 2_665 ? O1 K2 C4 57.35(11) 2_665 2_665 ? C2 K2 C4 86.89(13) . 2_665 ? O3 K2 C4 109.46(12) . 2_665 ? O4 K2 C4 21.87(11) 2_665 2_665 ? O3W K2 K3 50.25(12) 2_665 2_665 ? O2W K2 K3 130.93(13) . 2_665 ? O2 K2 K3 88.33(8) . 2_665 ? O10 K2 K3 52.27(8) 2_665 2_665 ? O5 K2 K3 52.54(8) . 2_665 ? O7W K2 K3 121.70(10) . 2_665 ? O1 K2 K3 102.28(8) 2_665 2_665 ? C2 K2 K3 64.09(10) . 2_665 ? O3 K2 K3 46.79(7) . 2_665 ? O4 K2 K3 146.89(8) 2_665 2_665 ? C4 K2 K3 134.72(10) 2_665 2_665 ? O9 K3 O3 123.19(13) 1_455 2_665 ? O9 K3 O4W 74.99(12) 1_455 1_455 ? O3 K3 O4W 94.45(12) 2_665 1_455 ? O9 K3 O3W 96.15(14) 1_455 . ? O3 K3 O3W 70.71(14) 2_665 . ? O4W K3 O3W 155.19(14) 1_455 . ? O9 K3 O14 105.37(13) 1_455 . ? O3 K3 O14 125.72(12) 2_665 . ? O4W K3 O14 74.74(11) 1_455 . ? O3W K3 O14 130.04(14) . . ? O9 K3 O10 124.97(12) 1_455 . ? O3 K3 O10 102.78(12) 2_665 . ? O4W K3 O10 133.72(11) 1_455 . ? O3W K3 O10 70.38(13) . . ? O14 K3 O10 60.25(10) . . ? O9 K3 O11 83.28(12) 1_455 . ? O3 K3 O11 123.75(13) 2_665 . ? O4W K3 O11 141.80(13) 1_455 . ? O3W K3 O11 56.68(13) . . ? O14 K3 O11 81.43(11) . . ? O10 K3 O11 44.02(10) . . ? O9 K3 O5 168.25(13) 1_455 2_665 ? O3 K3 O5 63.73(10) 2_665 2_665 ? O4W K3 O5 95.62(11) 1_455 2_665 ? O3W K3 O5 95.25(13) . 2_665 ? O14 K3 O5 64.72(11) . 2_665 ? O10 K3 O5 56.99(10) . 2_665 ? O11 K3 O5 100.70(10) . 2_665 ? O9 K3 C10 101.54(13) 1_455 . ? O3 K3 C10 121.72(13) 2_665 . ? O4W K3 C10 134.94(13) 1_455 . ? O3W K3 C10 69.08(14) . . ? O14 K3 C10 62.76(12) . . ? O10 K3 C10 23.43(12) . . ? O11 K3 C10 23.29(12) . . ? O5 K3 C10 79.93(12) 2_665 . ? O9 K3 C4 148.55(13) 1_455 2_665 ? O3 K3 C4 66.18(12) 2_665 2_665 ? O4W K3 C4 74.31(11) 1_455 2_665 ? O3W K3 C4 114.72(14) . 2_665 ? O14 K3 C4 59.64(11) . 2_665 ? O10 K3 C4 74.19(11) . 2_665 ? O11 K3 C4 117.96(11) . 2_665 ? O5 K3 C4 21.30(11) 2_665 2_665 ? C10 K3 C4 95.26(12) . 2_665 ? O9 K3 K2 142.66(10) 1_455 2_665 ? O3 K3 K2 56.94(9) 2_665 2_665 ? O4W K3 K2 139.98(9) 1_455 2_665 ? O3W K3 K2 46.82(11) . 2_665 ? O14 K3 K2 98.58(8) . 2_665 ? O10 K3 K2 47.54(8) . 2_665 ? O11 K3 K2 72.32(9) . 2_665 ? O5 K3 K2 48.49(7) 2_665 2_665 ? C10 K3 K2 64.80(10) . 2_665 ? C4 K3 K2 68.73(9) 2_665 2_665 ? O9 K3 Ce1 136.78(10) 1_455 . ? O3 K3 Ce1 99.80(8) 2_665 . ? O4W K3 Ce1 99.42(8) 1_455 . ? O3W K3 Ce1 102.60(11) . . ? O14 K3 Ce1 35.06(7) . . ? O10 K3 Ce1 35.79(7) . . ? O11 K3 Ce1 75.52(7) . . ? O5 K3 Ce1 36.59(7) 2_665 . ? C10 K3 Ce1 52.23(9) . . ? C4 K3 Ce1 44.40(8) 2_665 . ? K2 K3 Ce1 63.75(3) 2_665 . ? K1 O1W K1 101.6(2) . 2_775 ? K2 O2W K1 82.77(14) . . ? K2 O3W K3 82.93(13) 2_665 . ? K1 O4W K3 138.89(15) . 1_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.553 _refine_diff_density_min -2.309 _refine_diff_density_rms 0.279