# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_publication_text _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Catalina Ruiz Perez' _publ_contact_author_address ;Laboratorio de Rayos X y Materiales Moleculares Dpto. F\'isica Fundamental II. Facultad de F\'isica Universidad de La Laguna E-38204. La Laguna. Tenerife Spain ; _publ_contact_author_email caruiz@ull.es _publ_contact_author_phone +34922318236 _publ_contact_author_fax +34922318320 loop_ _publ_author_name _publ_author_address 'B. Gil-Hernandez' ;Laboratorio de Rayos X y Materiales Moleculares Dpto. F\'isica Fundamental II. Facultad de F\'isica Universidad de La Laguna E-38204. La Laguna. Tenerife Spain ; 'P. Gili' '' J.Pasan '' 'J. Sanchiz' '' 'C. Ruiz-Perez' '' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 828986' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Cu3, La, 3(C3 H3 O6), 16(H2 O)' _chemical_formula_sum 'C9 H35 Cu3 La O34' _chemical_formula_weight 1016.76 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.3238(5) _cell_length_b 20.5408(11) _cell_length_c 9.6118(5) _cell_angle_alpha 90.0 _cell_angle_beta 102.496(5) _cell_angle_gamma 90.0 _cell_volume 1604.47(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.104 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 975 _exptl_absorpt_coefficient_mu 3.385 _exptl_absorpt_correction_type cylinder _exptl_absorpt_correction_T_min 0.31 _exptl_absorpt_correction_T_max 0.33 _exptl_absorpt_process_details ; Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3 for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959) p.302; Table 5.3.6 B for muR in the range 2.6-10.0. The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975) A31,146-148) is used with some modification. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19052 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8365 _reflns_number_gt 7100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics CRYSTALMAKER _computing_publication_material 'PARST97 (Nardelli, 1997)' _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^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0025(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.022(17) _refine_ls_number_reflns 8365 _refine_ls_number_parameters 426 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1014 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7054(8) -0.0558(3) 0.2871(7) 0.0257(14) Uani 1 1 d . . . C2 C 0.6140(7) -0.0817(3) 0.4020(6) 0.0188(11) Uani 1 1 d . . . C3 C 0.7268(7) -0.1238(3) 0.5173(6) 0.0230(12) Uani 1 1 d . . . C4 C 0.3114(8) -0.3037(3) 0.2142(7) 0.0275(14) Uani 1 1 d . . . C5 C 0.1320(8) -0.3292(3) 0.1815(8) 0.0282(14) Uani 1 1 d . . . C6 C -0.0975(7) -0.1080(3) -0.0088(7) 0.0221(12) Uani 1 1 d . . . C7 C 0.0616(7) -0.0698(3) 0.0528(6) 0.0183(11) Uani 1 1 d . . . C8 C 0.1399(7) -0.0403(3) -0.0651(6) 0.0213(12) Uani 1 1 d . . . C9 C 0.4272(8) -0.3374(3) 0.3415(7) 0.0242(13) Uani 1 1 d . . . Cu3 Cu 0.10516(9) -0.19852(4) 0.14652(10) 0.0343(2) Uani 1 1 d . . . Cu2 Cu 0.50681(10) -0.20959(4) 0.36949(9) 0.0314(2) Uani 1 1 d . . . Cu1 Cu 0.39474(9) -0.08085(4) 0.14500(8) 0.02554(18) Uani 1 1 d . . . La1 La 0.74987(4) 0.007539(16) 0.73244(3) 0.01791(9) Uani 1 1 d . . . O1 O 0.4784(5) -0.1162(2) 0.3339(4) 0.0227(9) Uani 1 1 d . . . O2 O 0.3115(5) -0.2371(2) 0.2353(5) 0.0272(10) Uani 1 1 d . . . O1W O 0.8961(7) 0.0489(3) 0.5425(6) 0.0451(14) Uani 1 1 d . . . O3 O 0.1734(5) -0.1097(2) 0.1389(5) 0.0272(10) Uani 1 1 d . . . O2W O 0.4583(6) -0.0364(3) 0.7349(6) 0.0446(14) Uani 1 1 d . . . O4 O 0.7126(7) -0.1849(2) 0.4984(6) 0.0461(15) Uani 1 1 d . . . O3W O 0.6566(7) 0.0447(2) 0.9565(5) 0.0405(13) Uani 1 1 d . . . O5 O 0.8211(5) -0.0972(2) 0.6178(5) 0.0295(10) Uani 1 1 d . . . O4W O 0.6748(9) -0.2436(4) 0.1820(9) 0.080(2) Uani 1 1 d . . . O6 O 0.5728(5) -0.0267(2) 0.4773(4) 0.0221(9) Uani 1 1 d . . . O5W O 0.198(2) -0.2190(10) -0.119(2) 0.248(10) Uani 1 1 d . . . O7 O 0.6146(6) -0.0434(3) 0.1688(5) 0.0345(11) Uani 1 1 d . . . O6W O 0.0295(12) -0.1867(5) 0.3708(11) 0.114(3) Uani 1 1 d . . . O8 O 0.5297(7) -0.3014(2) 0.4196(6) 0.0434(14) Uani 1 1 d . . . O7W O 0.5050(10) -0.1566(4) -0.0090(9) 0.078(2) Uani 1 1 d . . . O9 O 0.0242(6) -0.2867(2) 0.1412(7) 0.0519(16) Uani 1 1 d . . . O8W O 0.2675(10) 0.1145(5) -0.1401(15) 0.121(4) Uani 1 1 d . . . O10 O 0.3759(6) -0.3207(2) 0.0913(5) 0.0372(12) Uani 1 1 d . . . O9W O 0.3367(10) 0.0344(4) 0.3001(9) 0.087(3) Uani 1 1 d . . . O11 O 0.1020(5) -0.3882(2) 0.1851(6) 0.0334(11) Uani 1 1 d . . . O10W O 0.1853(13) -0.0695(7) 0.5179(14) 0.146(5) Uani 1 1 d . . . O12 O -0.0998(6) -0.1664(2) 0.0305(7) 0.0464(15) Uani 1 1 d . . . O11W O 0.376(2) -0.1973(7) 0.5865(17) 0.193(7) Uani 1 1 d . . . O13 O 0.0208(6) -0.0138(2) 0.1242(5) 0.0291(10) Uani 1 1 d . . . O12W O -0.016(3) 0.1323(8) 0.1728(17) 0.228(9) Uani 1 1 d . . . O14 O 0.2953(5) -0.0388(2) -0.0364(5) 0.0309(11) Uani 1 1 d . . . O13W O 0.406(2) 0.1385(7) 0.1550(19) 0.212(8) Uani 1 1 d . . . O15 O 0.8568(6) -0.0479(3) 0.3178(6) 0.0495(16) Uani 1 1 d . . . O14W O 1.163(2) 0.1216(12) 0.526(2) 0.298(14) Uani 1 1 d . . . O16 O 0.0525(5) -0.0168(2) -0.1752(5) 0.0261(10) Uani 1 1 d . . . O15W O -0.229(3) -0.2527(7) -0.2170(15) 0.279(15) Uani 1 1 d . . . O17 O -0.2163(5) -0.0821(2) -0.0861(5) 0.0264(10) Uani 1 1 d . . . O16W O -0.260(2) 0.1279(15) 0.304(2) 0.293(15) Uani 1 1 d . . . O18 O 0.4263(6) -0.3975(2) 0.3556(6) 0.0348(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.021(3) 0.038(4) 0.019(3) -0.014(3) 0.007(2) -0.008(3) C2 0.021(3) 0.018(3) 0.016(3) -0.001(2) 0.001(2) 0.000(2) C3 0.019(3) 0.023(3) 0.024(3) -0.005(2) -0.002(2) -0.001(2) C4 0.033(3) 0.016(3) 0.033(4) 0.000(3) 0.006(3) 0.003(3) C5 0.023(3) 0.017(3) 0.039(4) 0.008(3) -0.003(3) 0.002(3) C6 0.022(3) 0.019(3) 0.027(3) -0.002(2) 0.009(2) 0.000(2) C7 0.017(3) 0.016(3) 0.020(3) 0.004(2) 0.001(2) -0.002(2) C8 0.023(3) 0.021(3) 0.020(3) 0.001(2) 0.005(2) 0.008(2) C9 0.020(3) 0.018(3) 0.033(3) -0.002(2) 0.001(2) -0.001(2) Cu3 0.0212(4) 0.0177(4) 0.0582(6) 0.0127(4) -0.0044(4) -0.0004(3) Cu2 0.0337(4) 0.0159(4) 0.0367(5) 0.0002(3) -0.0098(4) -0.0041(3) Cu1 0.0215(4) 0.0288(4) 0.0231(4) 0.0060(3) -0.0024(3) -0.0041(3) La1 0.02008(15) 0.01388(13) 0.01840(15) 0.00028(17) 0.00117(11) 0.00035(15) O1 0.023(2) 0.019(2) 0.024(2) 0.0047(17) -0.0009(17) -0.0044(18) O2 0.020(2) 0.013(2) 0.041(3) 0.0016(18) -0.0070(19) -0.0056(17) O1W 0.049(3) 0.055(4) 0.032(3) 0.000(2) 0.011(2) -0.022(3) O3 0.021(2) 0.021(2) 0.036(3) 0.0104(19) -0.0019(19) -0.0027(18) O2W 0.034(3) 0.070(4) 0.029(3) 0.007(3) 0.006(2) -0.013(3) O4 0.049(3) 0.019(2) 0.053(3) -0.002(2) -0.026(3) 0.005(2) O3W 0.070(4) 0.024(2) 0.031(3) -0.001(2) 0.018(3) 0.004(2) O5 0.032(2) 0.027(2) 0.023(2) -0.0073(18) -0.0086(19) 0.0074(19) O4W 0.056(4) 0.094(6) 0.095(6) 0.027(5) 0.028(4) -0.009(4) O6 0.029(2) 0.017(2) 0.019(2) -0.0007(16) 0.0013(17) 0.0020(17) O5W 0.206(15) 0.26(2) 0.32(2) -0.157(19) 0.151(16) -0.097(16) O7 0.025(2) 0.052(3) 0.024(2) 0.012(2) 0.0020(19) -0.005(2) O6W 0.104(6) 0.132(9) 0.119(8) 0.038(7) 0.057(6) 0.039(6) O8 0.047(3) 0.017(2) 0.050(3) 0.002(2) -0.024(2) -0.005(2) O7W 0.080(5) 0.060(4) 0.097(6) 0.004(4) 0.028(4) 0.005(4) O9 0.025(3) 0.017(2) 0.101(5) 0.015(3) -0.015(3) -0.002(2) O8W 0.067(5) 0.088(7) 0.213(12) 0.000(8) 0.041(6) -0.005(5) O10 0.040(3) 0.035(3) 0.037(3) 0.000(2) 0.008(2) -0.001(2) O9W 0.086(5) 0.066(5) 0.088(6) 0.016(4) -0.027(4) 0.006(4) O11 0.026(2) 0.017(2) 0.051(3) 0.008(2) -0.006(2) 0.0008(19) O10W 0.079(6) 0.188(12) 0.145(10) -0.015(9) -0.032(6) 0.001(7) O12 0.029(3) 0.021(3) 0.078(4) 0.020(3) -0.012(3) -0.006(2) O11W 0.267(18) 0.137(12) 0.211(15) -0.043(12) 0.129(14) -0.026(13) O13 0.030(2) 0.025(2) 0.035(3) -0.0034(18) 0.0144(19) 0.0009(18) O12W 0.33(2) 0.166(15) 0.157(14) 0.010(12) -0.015(15) 0.045(15) O14 0.018(2) 0.050(3) 0.025(2) 0.015(2) 0.0041(17) 0.001(2) O13W 0.30(2) 0.134(12) 0.230(18) 0.079(13) 0.125(16) 0.013(12) O15 0.026(3) 0.093(5) 0.030(3) 0.004(3) 0.007(2) -0.016(3) O14W 0.162(14) 0.43(4) 0.31(3) -0.13(3) 0.075(16) -0.194(19) O16 0.020(2) 0.033(2) 0.024(2) 0.0082(18) 0.0021(17) 0.0033(18) O15W 0.52(4) 0.099(11) 0.129(11) 0.027(8) -0.119(18) -0.087(14) O17 0.022(2) 0.023(2) 0.031(2) 0.0124(19) 0.0004(18) 0.0046(19) O16W 0.182(17) 0.43(4) 0.26(2) 0.21(2) 0.026(15) -0.021(18) O18 0.033(3) 0.015(2) 0.049(3) 0.002(2) -0.007(2) -0.003(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 C1 O15 1.240(8) . ? C1 O7 1.248(8) . ? C1 C2 1.564(9) . ? C2 O1 1.374(7) . ? C2 O6 1.424(7) . ? C2 C3 1.552(8) . ? C3 O5 1.232(7) . ? C3 O4 1.270(8) . ? C4 O2 1.384(8) . ? C4 O10 1.442(8) . ? C4 C9 1.547(9) . ? C4 C5 1.549(9) . ? C5 O11 1.239(8) . ? C5 O9 1.252(8) . ? C6 O17 1.223(7) . ? C6 O12 1.259(8) . ? C6 C7 1.543(8) . ? C7 O3 1.375(7) . ? C7 O13 1.418(7) . ? C7 C8 1.547(8) . ? C8 O16 1.245(7) . ? C8 O14 1.263(7) . ? C9 O18 1.243(8) . ? C9 O8 1.249(8) . ? Cu3 O2 1.916(4) . ? Cu3 O3 1.916(4) . ? Cu3 O9 1.929(5) . ? Cu3 O12 1.941(5) . ? Cu3 O6W 2.385(9) . ? Cu2 O2 1.928(4) . ? Cu2 O8 1.946(5) . ? Cu2 O4 1.951(5) . ? Cu2 O1 1.954(4) . ? Cu1 O3 1.925(4) . ? Cu1 O1 1.939(4) . ? Cu1 O7 1.953(5) . ? Cu1 O14 1.961(4) . ? La1 O18 2.476(4) 2_656 ? La1 O17 2.509(4) 1_656 ? La1 O11 2.513(4) 2_656 ? La1 O16 2.533(4) 1_656 ? La1 O5 2.545(4) . ? La1 O1W 2.549(5) . ? La1 O3W 2.558(5) . ? La1 O2W 2.594(5) . ? La1 O6 2.668(4) . ? O11 La1 2.513(4) 2_646 ? O16 La1 2.533(4) 1_454 ? O17 La1 2.509(4) 1_454 ? O18 La1 2.476(4) 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 O15 C1 O7 125.1(6) . . ? O15 C1 C2 120.0(6) . . ? O7 C1 C2 114.9(5) . . ? O1 C2 O6 112.9(5) . . ? O1 C2 C3 111.2(5) . . ? O6 C2 C3 104.8(4) . . ? O1 C2 C1 108.3(5) . . ? O6 C2 C1 107.2(5) . . ? C3 C2 C1 112.5(5) . . ? O5 C3 O4 125.0(6) . . ? O5 C3 C2 119.8(5) . . ? O4 C3 C2 115.2(5) . . ? O2 C4 O10 111.8(5) . . ? O2 C4 C9 110.2(5) . . ? O10 C4 C9 105.1(5) . . ? O2 C4 C5 109.5(5) . . ? O10 C4 C5 105.4(5) . . ? C9 C4 C5 114.7(5) . . ? O11 C5 O9 123.7(6) . . ? O11 C5 C4 121.1(5) . . ? O9 C5 C4 115.0(6) . . ? O17 C6 O12 122.3(6) . . ? O17 C6 C7 121.7(5) . . ? O12 C6 C7 115.9(5) . . ? O3 C7 O13 113.2(5) . . ? O3 C7 C6 109.9(5) . . ? O13 C7 C6 108.8(5) . . ? O3 C7 C8 109.7(5) . . ? O13 C7 C8 102.7(4) . . ? C6 C7 C8 112.4(5) . . ? O16 C8 O14 124.0(6) . . ? O16 C8 C7 120.9(5) . . ? O14 C8 C7 115.0(5) . . ? O18 C9 O8 122.8(6) . . ? O18 C9 C4 120.8(6) . . ? O8 C9 C4 116.0(5) . . ? O2 Cu3 O3 99.55(18) . . ? O2 Cu3 O9 84.14(19) . . ? O3 Cu3 O9 175.7(2) . . ? O2 Cu3 O12 171.3(3) . . ? O3 Cu3 O12 83.43(19) . . ? O9 Cu3 O12 92.6(2) . . ? O2 Cu3 O6W 91.5(3) . . ? O3 Cu3 O6W 94.3(3) . . ? O9 Cu3 O6W 87.8(4) . . ? O12 Cu3 O6W 96.5(3) . . ? O2 Cu2 O8 84.57(19) . . ? O2 Cu2 O4 176.4(2) . . ? O8 Cu2 O4 94.0(2) . . ? O2 Cu2 O1 96.75(18) . . ? O8 Cu2 O1 175.3(2) . . ? O4 Cu2 O1 84.98(19) . . ? O3 Cu1 O1 93.46(18) . . ? O3 Cu1 O7 172.7(2) . . ? O1 Cu1 O7 84.28(18) . . ? O3 Cu1 O14 83.79(18) . . ? O1 Cu1 O14 173.8(2) . . ? O7 Cu1 O14 97.75(19) . . ? O18 La1 O17 141.65(17) 2_656 1_656 ? O18 La1 O11 69.53(15) 2_656 2_656 ? O17 La1 O11 115.61(16) 1_656 2_656 ? O18 La1 O16 138.23(15) 2_656 1_656 ? O17 La1 O16 69.99(14) 1_656 1_656 ? O11 La1 O16 71.04(15) 2_656 1_656 ? O18 La1 O5 133.96(15) 2_656 . ? O17 La1 O5 71.28(15) 1_656 . ? O11 La1 O5 135.47(16) 2_656 . ? O16 La1 O5 71.18(14) 1_656 . ? O18 La1 O1W 80.34(19) 2_656 . ? O17 La1 O1W 137.98(17) 1_656 . ? O11 La1 O1W 70.39(17) 2_656 . ? O16 La1 O1W 73.98(16) 1_656 . ? O5 La1 O1W 77.26(17) . . ? O18 La1 O3W 77.74(17) 2_656 . ? O17 La1 O3W 69.05(15) 1_656 . ? O11 La1 O3W 72.42(18) 2_656 . ? O16 La1 O3W 102.94(17) 1_656 . ? O5 La1 O3W 139.28(16) . . ? O1W La1 O3W 141.50(18) . . ? O18 La1 O2W 77.93(18) 2_656 . ? O17 La1 O2W 72.74(16) 1_656 . ? O11 La1 O2W 133.61(18) 2_656 . ? O16 La1 O2W 142.15(17) 1_656 . ? O5 La1 O2W 90.91(18) . . ? O1W La1 O2W 135.63(17) . . ? O3W La1 O2W 68.97(18) . . ? O18 La1 O6 74.02(14) 2_656 . ? O17 La1 O6 113.74(14) 1_656 . ? O11 La1 O6 130.57(15) 2_656 . ? O16 La1 O6 125.44(14) 1_656 . ? O5 La1 O6 60.90(13) . . ? O1W La1 O6 71.56(15) . . ? O3W La1 O6 130.11(16) . . ? O2W La1 O6 65.46(15) . . ? C2 O1 Cu1 110.2(3) . . ? C2 O1 Cu2 111.6(3) . . ? Cu1 O1 Cu2 122.5(2) . . ? C4 O2 Cu3 111.8(4) . . ? C4 O2 Cu2 111.2(4) . . ? Cu3 O2 Cu2 136.2(2) . . ? C7 O3 Cu3 115.0(4) . . ? C7 O3 Cu1 110.7(3) . . ? Cu3 O3 Cu1 125.6(2) . . ? C3 O4 Cu2 112.9(4) . . ? C3 O5 La1 123.0(4) . . ? C2 O6 La1 122.0(3) . . ? C1 O7 Cu1 113.2(4) . . ? C9 O8 Cu2 114.0(4) . . ? C5 O9 Cu3 115.1(4) . . ? C5 O11 La1 138.9(4) . 2_646 ? C6 O12 Cu3 115.3(4) . . ? C8 O14 Cu1 113.5(4) . . ? C8 O16 La1 136.7(4) . 1_454 ? C6 O17 La1 134.2(4) . 1_454 ? C9 O18 La1 139.7(4) . 2_646 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.941 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.189 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 828987' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3Cu, La, 3(C3 H O6), 13(H2 O)' _chemical_formula_sum 'C9 H29 Cu3 La O31' _chemical_formula_weight 962.62 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.796(3) _cell_length_b 12.218(3) _cell_length_c 18.964(11) _cell_angle_alpha 90.00 _cell_angle_beta 93.794(16) _cell_angle_gamma 90.00 _cell_volume 2727.1(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Blue _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 3.968 _exptl_absorpt_correction_type cylinder _exptl_absorpt_process_details ; Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3 for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959) p.302; Table 5.3.6 B for muR in the range 2.6-10.0. The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975) A31,146-148) is used with some modification. ; _exptl_absorpt_correction_T_min 0.2688 _exptl_absorpt_correction_T_max 0.2909 _exptl_crystal_size_rad 0.2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8713 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 31.10 _reflns_number_total 8713 _reflns_number_gt 7362 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0781P)^2^+5.3697P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens notdet _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0053(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8713 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1448 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3884(4) 0.0986(3) 0.1915(2) 0.0171(8) Uani 1 1 d . . . C2 C 0.4577(3) 0.1868(4) 0.1555(2) 0.0168(7) Uani 1 1 d . . . C3 C 0.4755(4) 0.1492(4) 0.0792(2) 0.0179(8) Uani 1 1 d . . . C4 C 0.5847(4) 0.1471(4) 0.4274(2) 0.0180(8) Uani 1 1 d . . . C5 C 0.6889(4) 0.2100(3) 0.4035(2) 0.0151(7) Uani 1 1 d . . . C6 C 0.7970(4) 0.1532(4) 0.4361(2) 0.0169(8) Uani 1 1 d . . . C7 C 1.0176(4) 0.2055(4) 0.2166(2) 0.0215(9) Uani 1 1 d . . . C8 C 0.9126(3) 0.2368(3) 0.1677(2) 0.0162(7) Uani 1 1 d . . . C9 C 0.9079(4) 0.1658(4) 0.0994(2) 0.0177(8) Uani 1 1 d . . . Cu1 Cu 0.56393(5) 0.13034(4) 0.28547(3) 0.01877(13) Uani 1 1 d . . . Cu2 Cu 0.68972(4) 0.17603(5) 0.13626(3) 0.02250(14) Uani 1 1 d . . . Cu3 Cu 0.84210(5) 0.19297(5) 0.30149(3) 0.02208(14) Uani 1 1 d . . . La1 La 0.195623(18) 0.217572(19) 0.074526(11) 0.01414(9) Uani 1 1 d . . . O1 O 0.2894(3) 0.0809(3) 0.16565(16) 0.0219(6) Uani 1 1 d . . . O2 O 0.4345(3) 0.0492(3) 0.24451(17) 0.0258(7) Uani 1 1 d . . . O1W O 0.8949(4) 0.3706(4) 0.3619(2) 0.0407(9) Uani 1 1 d . . . O3 O 0.5599(2) 0.2070(2) 0.19302(16) 0.0172(6) Uani 1 1 d . . . O2W O 0.6868(6) 0.3547(5) 0.0841(3) 0.079(2) Uani 1 1 d . . . O4 O 0.3908(3) 0.1459(3) 0.03684(16) 0.0226(6) Uani 1 1 d . . . O3W O 0.6847(5) -0.0003(5) 0.2469(4) 0.080(2) Uani 1 1 d . . . O5 O 0.5756(3) 0.1241(3) 0.06567(18) 0.0292(8) Uani 1 1 d . . . O4W O 0.1694(3) 0.4125(3) 0.12387(19) 0.0310(8) Uani 1 1 d . . . O6 O 0.3844(3) 0.2798(2) 0.15095(16) 0.0185(6) Uani 1 1 d . . . O5W O 0.1812(3) 0.0073(3) 0.04329(18) 0.0257(7) Uani 1 1 d . . . O7 O 0.5306(3) 0.0890(3) 0.38115(16) 0.0251(7) Uani 1 1 d . . . O6W O 0.5076(4) 0.4143(4) 0.3826(3) 0.0522(12) Uani 1 1 d . . . O8 O 0.6885(3) 0.2146(2) 0.33080(15) 0.0168(6) Uani 1 1 d . . . O7W O 1.1157(4) 0.3863(4) 0.4217(2) 0.0502(12) Uani 1 1 d . . . O9 O 0.8698(3) 0.1234(3) 0.39408(17) 0.0287(8) Uani 1 1 d . . . O8W O 0.9075(5) -0.0623(4) 0.2593(3) 0.0614(14) Uani 1 1 d . . . O10 O 0.9977(3) 0.1767(4) 0.27952(18) 0.0326(8) Uani 1 1 d . . . O9W O 0.8279(4) 0.4136(4) -0.0171(3) 0.0620(14) Uani 1 1 d . . . O11 O 0.8132(3) 0.2244(3) 0.20216(16) 0.0208(6) Uani 1 1 d . . . O10W O 0.4720(6) 0.4559(5) 0.0870(3) 0.089(2) Uani 1 1 d . . . O12 O 0.5610(3) 0.1575(3) 0.48985(16) 0.0254(7) Uani 1 1 d . . . O11W O 1.2104(7) 0.1993(6) 0.3743(4) 0.091(2) Uani 1 1 d . . . O13 O 0.8062(3) 0.1411(3) 0.50160(16) 0.0226(6) Uani 1 1 d . . . O12W O 0.3825(7) 0.2767(5) 0.3057(4) 0.082(2) Uani 1 1 d . . . O14 O 0.6905(3) 0.3158(2) 0.43571(15) 0.0175(6) Uani 1 1 d . . . O13W O 0.3259(5) 0.4804(5) 0.2284(3) 0.0761(19) Uani 1 1 d . . . O15 O 1.1132(3) 0.2099(3) 0.19504(19) 0.0320(8) Uani 1 1 d . . . O16 O 0.9301(3) 0.3461(3) 0.1464(2) 0.0292(7) Uani 1 1 d . . . O17 O 0.8115(3) 0.1246(3) 0.08086(19) 0.0289(8) Uani 1 1 d . . . O18 O 0.9934(3) 0.1524(3) 0.06652(17) 0.0248(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0143(18) 0.0229(19) 0.0138(17) -0.0026(14) -0.0021(14) 0.0012(15) C2 0.0086(17) 0.0262(19) 0.0153(17) 0.0011(15) -0.0017(13) 0.0020(15) C3 0.0144(19) 0.0245(19) 0.0148(17) -0.0024(15) 0.0012(14) 0.0017(15) C4 0.0149(18) 0.026(2) 0.0133(17) 0.0024(15) 0.0013(14) 0.0000(15) C5 0.0149(18) 0.0204(18) 0.0100(16) -0.0012(13) 0.0007(13) -0.0001(14) C6 0.0171(19) 0.0220(19) 0.0121(16) -0.0006(14) 0.0049(14) -0.0003(15) C7 0.0134(19) 0.036(2) 0.0157(19) 0.0001(16) 0.0019(15) 0.0010(16) C8 0.0112(17) 0.0233(19) 0.0144(17) 0.0015(15) 0.0023(14) -0.0017(14) C9 0.0134(18) 0.025(2) 0.0150(17) -0.0013(15) 0.0046(14) 0.0010(15) Cu1 0.0174(3) 0.0277(3) 0.0108(2) 0.00026(18) -0.00178(18) -0.0055(2) Cu2 0.0092(2) 0.0382(3) 0.0202(3) -0.0071(2) 0.00168(19) -0.0006(2) Cu3 0.0161(3) 0.0375(3) 0.0133(2) 0.0043(2) 0.0054(2) 0.0035(2) La1 0.00966(13) 0.02309(14) 0.00966(12) 0.00106(7) 0.00055(8) -0.00106(8) O1 0.0120(14) 0.0344(17) 0.0190(14) 0.0038(12) -0.0007(11) -0.0038(12) O2 0.0224(16) 0.0298(16) 0.0236(15) 0.0060(13) -0.0096(13) -0.0075(13) O1W 0.038(2) 0.046(2) 0.039(2) 0.0000(18) 0.0076(18) -0.0062(18) O3 0.0082(13) 0.0283(15) 0.0149(13) 0.0019(11) -0.0003(10) -0.0024(11) O2W 0.099(5) 0.068(4) 0.072(4) 0.031(3) 0.021(4) 0.026(3) O4 0.0135(14) 0.0381(18) 0.0159(14) -0.0036(12) -0.0019(11) 0.0011(13) O3W 0.045(3) 0.062(3) 0.131(6) -0.060(4) -0.016(3) 0.023(2) O5 0.0123(15) 0.052(2) 0.0231(16) -0.0145(15) 0.0004(12) 0.0033(14) O4W 0.0300(19) 0.0336(18) 0.0300(18) -0.0086(15) 0.0064(15) 0.0039(15) O6 0.0132(14) 0.0227(14) 0.0192(14) -0.0007(11) -0.0003(11) 0.0036(11) O5W 0.0254(17) 0.0272(16) 0.0242(16) -0.0049(13) -0.0015(13) 0.0010(13) O7 0.0267(17) 0.0361(18) 0.0127(13) 0.0005(12) 0.0019(12) -0.0141(14) O6W 0.039(2) 0.066(3) 0.051(3) -0.008(2) -0.002(2) 0.024(2) O8 0.0135(14) 0.0295(15) 0.0075(12) -0.0005(10) 0.0011(10) -0.0007(11) O7W 0.057(3) 0.062(3) 0.032(2) 0.003(2) 0.005(2) -0.018(2) O9 0.0261(18) 0.0433(19) 0.0178(15) 0.0077(14) 0.0089(13) 0.0177(15) O8W 0.064(3) 0.048(3) 0.069(3) -0.004(2) -0.011(3) 0.006(2) O10 0.0178(16) 0.064(2) 0.0161(15) 0.0079(16) 0.0047(12) 0.0063(16) O9W 0.039(3) 0.064(3) 0.085(4) 0.025(3) 0.018(3) 0.009(2) O11 0.0143(14) 0.0331(17) 0.0154(14) -0.0008(12) 0.0040(11) 0.0012(12) O10W 0.096(5) 0.085(4) 0.080(4) 0.026(3) -0.043(4) -0.053(4) O12 0.0203(16) 0.0431(19) 0.0131(13) -0.0033(13) 0.0034(12) -0.0077(14) O11W 0.079(5) 0.097(5) 0.095(5) -0.025(4) -0.015(4) 0.008(4) O13 0.0217(16) 0.0329(17) 0.0132(13) 0.0011(12) 0.0009(12) 0.0075(13) O12W 0.107(6) 0.070(4) 0.067(4) -0.016(3) -0.002(4) -0.002(4) O14 0.0201(15) 0.0205(13) 0.0117(12) -0.0017(11) -0.0007(11) 0.0008(11) O13W 0.044(3) 0.103(5) 0.081(4) -0.059(4) 0.000(3) 0.010(3) O15 0.0162(16) 0.062(2) 0.0179(16) 0.0015(15) 0.0031(13) 0.0012(15) O16 0.0292(19) 0.0233(16) 0.0359(19) 0.0012(14) 0.0087(15) -0.0033(13) O17 0.0128(15) 0.046(2) 0.0285(17) -0.0189(15) 0.0050(13) -0.0047(14) O18 0.0135(15) 0.0395(18) 0.0222(15) -0.0075(13) 0.0071(12) -0.0036(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.254(5) . ? C1 O2 1.265(5) . ? C1 C2 1.539(6) . ? C2 O3 1.382(5) . ? C2 O6 1.427(5) . ? C2 C3 1.545(6) . ? C3 O4 1.241(5) . ? C3 O5 1.263(5) . ? C4 O12 1.241(5) . ? C4 O7 1.267(5) . ? C4 C5 1.543(6) . ? C5 O8 1.380(5) . ? C5 O14 1.429(5) . ? C5 C6 1.544(6) . ? C6 O13 1.249(5) . ? C6 O9 1.262(5) . ? C7 O15 1.227(6) . ? C7 O10 1.280(5) . ? C7 C8 1.545(6) . ? C8 O11 1.387(5) . ? C8 O16 1.414(5) . ? C8 C9 1.558(6) . ? C9 O18 1.232(5) . ? C9 O17 1.271(5) . ? Cu1 O2 1.939(3) . ? Cu1 O8 1.948(3) . ? Cu1 O7 1.949(3) . ? Cu1 O3 1.986(3) . ? Cu1 O3W 2.291(5) . ? Cu2 O17 1.940(3) . ? Cu2 O5 1.941(3) . ? Cu2 O11 1.947(3) . ? Cu2 O3 1.966(3) . ? Cu2 O2W 2.396(6) . ? Cu3 O10 1.920(4) . ? Cu3 O11 1.930(3) . ? Cu3 O8 1.948(3) . ? Cu3 O9 1.959(3) . ? La1 O18 2.509(3) 1_455 ? La1 O15 2.544(4) 1_455 ? La1 O4W 2.585(4) . ? La1 O1 2.597(3) . ? La1 O4 2.607(3) . ? La1 O13 2.615(3) 4_565 ? La1 O5W 2.639(3) . ? La1 O14 2.661(3) 4_565 ? La1 O12 2.663(3) 4_565 ? La1 O6 2.685(3) . ? O12 La1 2.663(3) 4_666 ? O13 La1 2.615(3) 4_666 ? O14 La1 2.661(3) 4_666 ? O15 La1 2.544(4) 1_655 ? O18 La1 2.509(3) 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 O1 C1 O2 124.7(4) . . ? O1 C1 C2 117.1(3) . . ? O2 C1 C2 118.2(4) . . ? O3 C2 O6 113.1(3) . . ? O3 C2 C1 111.6(3) . . ? O6 C2 C1 104.3(3) . . ? O3 C2 C3 111.5(3) . . ? O6 C2 C3 107.5(3) . . ? C1 C2 C3 108.4(3) . . ? O4 C3 O5 125.7(4) . . ? O4 C3 C2 117.5(4) . . ? O5 C3 C2 116.7(3) . . ? O12 C4 O7 125.6(4) . . ? O12 C4 C5 117.6(4) . . ? O7 C4 C5 116.7(4) . . ? O8 C5 O14 112.9(3) . . ? O8 C5 C4 111.4(3) . . ? O14 C5 C4 108.2(3) . . ? O8 C5 C6 111.5(3) . . ? O14 C5 C6 104.4(3) . . ? C4 C5 C6 108.2(3) . . ? O13 C6 O9 125.1(4) . . ? O13 C6 C5 117.8(4) . . ? O9 C6 C5 117.1(4) . . ? O15 C7 O10 123.5(4) . . ? O15 C7 C8 120.5(4) . . ? O10 C7 C8 116.0(4) . . ? O11 C8 O16 112.4(4) . . ? O11 C8 C7 111.0(3) . . ? O16 C8 C7 106.2(3) . . ? O11 C8 C9 110.2(3) . . ? O16 C8 C9 106.7(3) . . ? C7 C8 C9 110.1(3) . . ? O18 C9 O17 123.7(4) . . ? O18 C9 C8 120.6(4) . . ? O17 C9 C8 115.7(4) . . ? O2 Cu1 O8 176.74(15) . . ? O2 Cu1 O7 92.21(14) . . ? O8 Cu1 O7 85.35(13) . . ? O2 Cu1 O3 85.15(13) . . ? O8 Cu1 O3 96.51(12) . . ? O7 Cu1 O3 161.82(15) . . ? O2 Cu1 O3W 90.33(17) . . ? O8 Cu1 O3W 92.42(16) . . ? O7 Cu1 O3W 106.5(2) . . ? O3 Cu1 O3W 91.5(2) . . ? O17 Cu2 O5 91.44(14) . . ? O17 Cu2 O11 84.07(14) . . ? O5 Cu2 O11 175.50(14) . . ? O17 Cu2 O3 172.15(14) . . ? O5 Cu2 O3 84.89(14) . . ? O11 Cu2 O3 99.60(13) . . ? O17 Cu2 O2W 93.6(2) . . ? O5 Cu2 O2W 91.3(2) . . ? O11 Cu2 O2W 88.7(2) . . ? O3 Cu2 O2W 93.44(18) . . ? O10 Cu3 O11 85.33(14) . . ? O10 Cu3 O8 175.49(14) . . ? O11 Cu3 O8 98.28(13) . . ? O10 Cu3 O9 92.55(15) . . ? O11 Cu3 O9 165.76(15) . . ? O8 Cu3 O9 84.60(13) . . ? O18 La1 O15 67.95(11) 1_455 1_455 ? O18 La1 O4W 100.26(12) 1_455 . ? O15 La1 O4W 69.30(12) 1_455 . ? O18 La1 O1 101.41(11) 1_455 . ? O15 La1 O1 63.25(11) 1_455 . ? O4W La1 O1 114.04(11) . . ? O18 La1 O4 136.87(11) 1_455 . ? O15 La1 O4 129.11(11) 1_455 . ? O4W La1 O4 122.54(11) . . ? O1 La1 O4 67.74(10) . . ? O18 La1 O13 133.09(11) 1_455 4_565 ? O15 La1 O13 137.15(11) 1_455 4_565 ? O4W La1 O13 70.04(12) . 4_565 ? O1 La1 O13 124.82(10) . 4_565 ? O4 La1 O13 66.20(11) . 4_565 ? O18 La1 O5W 68.35(11) 1_455 . ? O15 La1 O5W 98.24(12) 1_455 . ? O4W La1 O5W 166.07(12) . . ? O1 La1 O5W 62.73(10) . . ? O4 La1 O5W 69.88(11) . . ? O13 La1 O5W 123.45(11) 4_565 . ? O18 La1 O14 86.12(10) 1_455 4_565 ? O15 La1 O14 153.95(11) 1_455 4_565 ? O4W La1 O14 120.25(11) . 4_565 ? O1 La1 O14 122.73(10) . 4_565 ? O4 La1 O14 68.89(9) . 4_565 ? O13 La1 O14 63.72(9) 4_565 4_565 ? O5W La1 O14 68.41(10) . 4_565 ? O18 La1 O12 67.60(11) 1_455 4_565 ? O15 La1 O12 108.34(11) 1_455 4_565 ? O4W La1 O12 67.00(12) . 4_565 ? O1 La1 O12 168.65(10) . 4_565 ? O4 La1 O12 121.97(10) . 4_565 ? O13 La1 O12 66.49(11) 4_565 4_565 ? O5W La1 O12 113.31(11) . 4_565 ? O14 La1 O12 61.16(10) 4_565 4_565 ? O18 La1 O6 150.85(10) 1_455 . ? O15 La1 O6 82.98(11) 1_455 . ? O4W La1 O6 70.03(10) . . ? O1 La1 O6 61.39(10) . . ? O4 La1 O6 61.79(10) . . ? O13 La1 O6 70.94(10) 4_565 . ? O5W La1 O6 115.81(9) . . ? O14 La1 O6 122.76(10) 4_565 . ? O12 La1 O6 127.11(10) 4_565 . ? C1 O1 La1 119.6(3) . . ? C1 O2 Cu1 111.2(3) . . ? C2 O3 Cu2 111.6(3) . . ? C2 O3 Cu1 109.8(3) . . ? Cu2 O3 Cu1 114.73(15) . . ? C3 O4 La1 120.0(3) . . ? C3 O5 Cu2 113.3(3) . . ? C2 O6 La1 106.5(2) . . ? C4 O7 Cu1 112.1(3) . . ? C5 O8 Cu3 109.8(2) . . ? C5 O8 Cu1 111.8(2) . . ? Cu3 O8 Cu1 119.41(15) . . ? C6 O9 Cu3 111.1(3) . . ? C7 O10 Cu3 114.2(3) . . ? C8 O11 Cu3 112.4(2) . . ? C8 O11 Cu2 110.5(2) . . ? Cu3 O11 Cu2 129.95(18) . . ? C4 O12 La1 118.1(3) . 4_666 ? C6 O13 La1 115.7(3) . 4_666 ? C5 O14 La1 106.4(2) . 4_666 ? C7 O15 La1 135.7(3) . 1_655 ? C9 O17 Cu2 113.7(3) . . ? C9 O18 La1 137.3(3) . 1_655 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 31.10 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.730 _refine_diff_density_min -1.234 _refine_diff_density_rms 0.362