# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Rico Del Sesto' _publ_contact_author_email RICOD@LANL.GOV _publ_section_title ; Luminescence in CeIV Polyoxometalate [Ce(W5O18)2]8-: A Combined Experimental and Theoretical Study ; loop_ _publ_author_name 'Rico Del Sesto' 'Enrique Batista' 'Michael W. Blair' 'Richard L. Martin' 'Iain May' 'Denisse Ortiz-Acosta' ; L.E.Roy ; 'Brian L. Scott' # Attachment 'Article_B926660G_CIF_file.cif' data_apx683 _database_code_depnum_ccdc_archive 'CCDC 758779' #TrackingRef 'Article_B926660G_CIF_file.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H62 Ce Na8 O67 W10' _chemical_formula_weight 3297.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.041(5) _cell_length_b 18.497(5) _cell_length_c 18.324(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.941(3) _cell_angle_gamma 90.00 _cell_volume 6082(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used 8198 _cell_measurement_theta_min 4.47 _cell_measurement_theta_max 55.92 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5936 _exptl_absorpt_coefficient_mu 19.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1101 _exptl_absorpt_correction_T_max 0.2428 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _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 'Bruker D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 32637 _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.19 _reflns_number_total 7032 _reflns_number_gt 5595 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 1.08 (Bruker AXS, 2003)' _computing_cell_refinement 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_data_reduction 'SAINT+, v. 7.06 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.10, (Bruker AXS, 2000)' _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^)+(0.0593P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7032 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.5000 0.74534(4) 0.2500 0.01292(16) Uani 1 2 d S . . W1 W 0.64456(2) 0.86009(2) 0.16795(2) 0.01399(11) Uani 1 1 d . . . W2 W 0.67491(2) 0.63057(2) 0.26371(2) 0.01348(10) Uani 1 1 d . . . W3 W 0.69565(2) 0.79458(2) 0.33002(2) 0.01392(10) Uani 1 1 d . . . W4 W 0.62219(2) 0.694613(19) 0.10050(2) 0.01347(10) Uani 1 1 d . . . W5 W 0.78547(2) 0.74545(2) 0.18799(2) 0.01468(11) Uani 1 1 d . . . Na1 Na 0.5542(2) 0.5527(2) -0.0598(2) 0.0234(9) Uani 1 1 d . . . Na2 Na 0.5000 0.5689(3) -0.2500 0.0208(12) Uani 1 2 d S . . Na3 Na 0.7001(3) 0.9934(2) 0.0128(2) 0.0317(11) Uani 1 1 d . . . Na4 Na 0.5718(3) 1.1447(3) 0.0885(3) 0.0534(16) Uani 1 1 d . . . Na5 Na 0.5000 1.0648(4) 0.2500 0.053(2) Uani 1 2 d S . . O1 O 0.5523(4) 0.8470(3) 0.1939(4) 0.0170(15) Uani 1 1 d . . . O2 O 0.5329(4) 0.7014(3) 0.1351(4) 0.0161(15) Uani 1 1 d . . . O3 O 0.5787(4) 0.6432(3) 0.2794(4) 0.0159(14) Uani 1 1 d . . . O4 O 0.5973(4) 0.7885(3) 0.3384(4) 0.0165(14) Uani 1 1 d . . . O5 O 0.7076(4) 0.6908(4) 0.3479(4) 0.0181(15) Uani 1 1 d . . . O6 O 0.6827(4) 0.8802(4) 0.2681(4) 0.0183(15) Uani 1 1 d . . . O7 O 0.6220(4) 0.7978(3) 0.0822(4) 0.0175(15) Uani 1 1 d . . . O8 O 0.6478(4) 0.6105(4) 0.1609(4) 0.0188(15) Uani 1 1 d . . . O9 O 0.6648(4) 0.7451(3) 0.2160(3) 0.0144(14) Uani 1 1 d . . . O10 O 0.6431(4) 0.9448(3) 0.1284(4) 0.0180(15) Uani 1 1 d . . . O11 O 0.6021(4) 0.6563(4) 0.0159(4) 0.0221(16) Uani 1 1 d . . . O12 O 0.6960(4) 0.5446(4) 0.2974(4) 0.0226(16) Uani 1 1 d . . . O13 O 0.7327(4) 0.8302(4) 0.4125(4) 0.0253(17) Uani 1 1 d . . . O14 O 0.7502(4) 0.8375(3) 0.1548(4) 0.0158(14) Uani 1 1 d . . . O15 O 0.7325(4) 0.7060(3) 0.1024(4) 0.0158(14) Uani 1 1 d . . . O16 O 0.7751(4) 0.6534(3) 0.2318(4) 0.0156(14) Uani 1 1 d . . . O17 O 0.7930(4) 0.7854(3) 0.2853(4) 0.0161(14) Uani 1 1 d . . . O18 O 0.8777(4) 0.7463(4) 0.1681(4) 0.0224(16) Uani 1 1 d . . . O19 O 0.5755(4) 0.4584(4) 0.0296(4) 0.0277(18) Uani 1 1 d . . . O20 O 0.6836(4) 0.5460(4) -0.0845(4) 0.0232(16) Uani 1 1 d . . . O21 O 0.5194(4) 0.6459(4) -0.1476(4) 0.0204(16) Uani 1 1 d . . . O22 O 0.5062(4) 0.4711(3) -0.1583(4) 0.0169(14) Uani 1 1 d . . . O23 O 0.3707(4) 0.5758(4) -0.2194(5) 0.037(2) Uani 1 1 d . . . O24 O 0.6760(4) 0.8763(4) -0.0276(4) 0.0246(17) Uani 1 1 d . . . O25 O 0.7631(6) 1.0041(4) -0.0987(5) 0.054(3) Uani 1 1 d . . . O26 O 0.5679(7) 1.0209(6) -0.0243(9) 0.097(5) Uani 1 1 d . . . O27 O 0.6966(4) 1.1181(4) 0.0473(4) 0.0267(17) Uani 1 1 d . . . O28 O 0.5308(4) 1.1666(4) -0.0348(4) 0.0271(17) Uani 1 1 d . . . O29 O 0.5951(4) 1.2702(4) 0.0998(4) 0.0288(18) Uani 1 1 d . . . O30 O 0.5125(15) 1.1938(15) 0.2194(11) 0.093(9) Uani 0.50 1 d P . . O31 O 0.4541(7) 1.1128(8) 0.1201(8) 0.110(6) Uani 1 1 d . . . O32 O 0.6127(4) 1.0754(4) 0.1943(4) 0.0264(17) Uani 1 1 d . . . O33 O 0.4461(5) 0.9617(5) 0.1801(5) 0.050(3) Uani 1 1 d . . . O34 O 0.4019(4) 0.6678(4) 0.0432(4) 0.0214(16) 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 Ce1 0.0150(4) 0.0111(4) 0.0127(4) 0.000 0.0018(3) 0.000 W1 0.0171(2) 0.01094(19) 0.0144(2) 0.00003(14) 0.00377(16) -0.00038(14) W2 0.0145(2) 0.01105(19) 0.0152(2) 0.00104(14) 0.00285(16) 0.00028(14) W3 0.0146(2) 0.0142(2) 0.0131(2) -0.00124(14) 0.00209(16) -0.00137(14) W4 0.0161(2) 0.01187(19) 0.0127(2) -0.00169(14) 0.00299(16) -0.00048(14) W5 0.0150(2) 0.0130(2) 0.0166(2) -0.00055(14) 0.00389(16) -0.00056(14) Na1 0.031(3) 0.017(2) 0.023(2) 0.0001(16) 0.0057(19) -0.0016(17) Na2 0.032(3) 0.019(3) 0.012(3) 0.000 0.004(2) 0.000 Na3 0.045(3) 0.023(2) 0.028(2) -0.0007(18) 0.010(2) -0.002(2) Na4 0.043(3) 0.054(3) 0.058(4) 0.030(3) -0.016(3) -0.016(3) Na5 0.034(4) 0.042(4) 0.088(6) 0.000 0.035(4) 0.000 O1 0.017(4) 0.015(3) 0.018(4) -0.006(3) 0.002(3) 0.006(3) O2 0.014(4) 0.013(3) 0.021(4) 0.002(3) -0.001(3) -0.002(3) O3 0.013(4) 0.016(3) 0.019(4) -0.001(3) 0.005(3) -0.004(3) O4 0.013(4) 0.018(3) 0.020(4) 0.001(3) 0.007(3) 0.001(3) O5 0.017(4) 0.020(4) 0.016(4) -0.003(3) -0.003(3) -0.004(3) O6 0.025(4) 0.015(3) 0.015(3) -0.004(3) 0.003(3) 0.003(3) O7 0.020(4) 0.018(3) 0.015(4) -0.003(3) 0.001(3) -0.005(3) O8 0.024(4) 0.019(4) 0.014(3) -0.004(3) 0.005(3) 0.000(3) O9 0.017(4) 0.010(3) 0.016(4) -0.004(3) 0.000(3) 0.002(3) O10 0.029(4) 0.010(3) 0.016(4) 0.003(3) 0.004(3) -0.001(3) O11 0.025(4) 0.016(4) 0.026(4) -0.004(3) 0.006(3) 0.002(3) O12 0.030(4) 0.012(3) 0.027(4) 0.006(3) 0.009(3) -0.001(3) O13 0.029(4) 0.023(4) 0.022(4) 0.000(3) -0.003(3) 0.003(3) O14 0.013(4) 0.013(3) 0.023(4) -0.004(3) 0.012(3) -0.004(3) O15 0.016(4) 0.011(3) 0.022(4) -0.004(3) 0.006(3) -0.004(3) O16 0.015(4) 0.018(3) 0.013(3) 0.005(3) 0.002(3) 0.000(3) O17 0.016(4) 0.019(3) 0.014(3) 0.000(3) 0.003(3) 0.000(3) O18 0.014(4) 0.023(4) 0.033(4) 0.004(3) 0.011(3) -0.001(3) O19 0.032(5) 0.021(4) 0.031(4) -0.002(3) 0.004(4) 0.001(3) O20 0.029(4) 0.022(4) 0.021(4) -0.004(3) 0.009(3) -0.003(3) O21 0.024(4) 0.020(4) 0.018(4) -0.004(3) 0.002(3) -0.002(3) O22 0.024(4) 0.012(3) 0.016(3) -0.004(3) 0.006(3) 0.001(3) O23 0.020(4) 0.023(4) 0.064(6) -0.003(4) -0.007(4) 0.006(3) O24 0.031(4) 0.021(4) 0.024(4) -0.004(3) 0.011(3) 0.000(3) O25 0.097(9) 0.027(5) 0.045(6) 0.008(4) 0.037(6) 0.014(5) O26 0.078(9) 0.036(6) 0.165(14) 0.006(7) -0.052(9) 0.001(6) O27 0.031(5) 0.023(4) 0.025(4) 0.005(3) 0.001(3) -0.004(3) O28 0.027(4) 0.029(4) 0.024(4) 0.007(3) -0.003(3) 0.000(3) O29 0.028(5) 0.034(4) 0.025(4) -0.003(3) 0.001(3) 0.000(4) O30 0.09(2) 0.16(3) 0.030(13) -0.010(13) -0.018(14) 0.000(18) O31 0.040(7) 0.171(14) 0.120(12) 0.091(11) 0.014(7) 0.015(8) O32 0.021(4) 0.029(4) 0.029(4) -0.006(3) 0.001(3) -0.002(3) O33 0.053(6) 0.041(5) 0.058(6) 0.016(5) 0.015(5) 0.004(5) O34 0.023(4) 0.018(4) 0.023(4) -0.003(3) 0.003(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O1 2.384(7) . ? Ce1 O1 2.384(7) 2_655 ? Ce1 O2 2.389(7) . ? Ce1 O2 2.389(7) 2_655 ? Ce1 O3 2.391(7) . ? Ce1 O3 2.391(7) 2_655 ? Ce1 O4 2.399(7) . ? Ce1 O4 2.399(7) 2_655 ? W1 O10 1.726(6) . ? W1 O1 1.793(7) . ? W1 O6 1.929(7) . ? W1 O7 1.956(7) . ? W1 O14 1.989(6) . ? W1 O9 2.316(6) . ? W2 O12 1.733(7) . ? W2 O3 1.803(7) . ? W2 O8 1.933(7) . ? W2 O5 1.943(7) . ? W2 O16 2.001(7) . ? W2 O9 2.292(6) . ? W3 O13 1.719(7) . ? W3 O4 1.800(7) . ? W3 O6 1.948(7) . ? W3 O5 1.956(7) . ? W3 O17 2.021(7) . ? W3 O9 2.297(6) . ? W4 O11 1.709(7) . ? W4 O2 1.796(7) . ? W4 O8 1.938(7) . ? W4 O7 1.939(6) . ? W4 O15 1.998(7) . ? W4 O9 2.367(6) . ? W5 O18 1.741(7) . ? W5 O14 1.895(7) . ? W5 O15 1.896(7) . ? W5 O16 1.900(6) . ? W5 O17 1.921(6) . ? W5 O9 2.287(7) . ? Na1 O19 2.396(8) . ? Na1 O21 2.397(8) . ? Na1 O20 2.427(9) . ? Na1 O22 2.440(7) . ? Na1 O19 2.469(9) 5_665 ? Na1 O11 2.470(8) . ? Na1 Na2 3.533(4) . ? Na1 Na1 3.649(8) 5_665 ? Na2 O21 2.352(7) . ? Na2 O21 2.352(7) 2_654 ? Na2 O23 2.458(8) . ? Na2 O23 2.458(8) 2_654 ? Na2 O22 2.464(8) . ? Na2 O22 2.464(8) 2_654 ? Na2 Na1 3.533(4) 2_654 ? Na3 O24 2.316(8) . ? Na3 O27 2.394(9) . ? Na3 O25 2.445(10) . ? Na3 O26 2.465(13) . ? Na3 O20 2.468(9) 7_665 ? Na3 O10 2.609(8) . ? Na3 Na4 3.973(8) . ? Na4 O31 2.334(13) . ? Na4 O28 2.339(9) . ? Na4 O29 2.364(10) . ? Na4 O32 2.378(9) . ? Na4 O27 2.497(10) . ? Na4 O30 2.87(2) . ? Na4 Na5 3.663(6) . ? Na5 O32 2.375(7) 2_655 ? Na5 O32 2.375(7) . ? Na5 O33 2.441(12) . ? Na5 O33 2.441(12) 2_655 ? Na5 O30 2.47(3) . ? Na5 O30 2.47(3) 2_655 ? Na5 O31 2.595(13) . ? Na5 O31 2.595(13) 2_655 ? Na5 Na4 3.663(6) 2_655 ? O19 Na1 2.469(9) 5_665 ? O20 Na3 2.468(9) 7_665 ? O30 O30 1.25(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 O1 Ce1 O1 75.9(3) . 2_655 ? O1 Ce1 O2 75.1(2) . . ? O1 Ce1 O2 142.6(2) 2_655 . ? O1 Ce1 O2 142.6(2) . 2_655 ? O1 Ce1 O2 75.1(2) 2_655 2_655 ? O2 Ce1 O2 140.2(3) . 2_655 ? O1 Ce1 O3 117.9(2) . . ? O1 Ce1 O3 141.1(2) 2_655 . ? O2 Ce1 O3 74.6(2) . . ? O2 Ce1 O3 74.2(2) 2_655 . ? O1 Ce1 O3 141.1(2) . 2_655 ? O1 Ce1 O3 117.9(2) 2_655 2_655 ? O2 Ce1 O3 74.2(2) . 2_655 ? O2 Ce1 O3 74.6(2) 2_655 2_655 ? O3 Ce1 O3 75.7(3) . 2_655 ? O1 Ce1 O4 74.6(2) . . ? O1 Ce1 O4 75.0(2) 2_655 . ? O2 Ce1 O4 118.5(2) . . ? O2 Ce1 O4 75.5(2) 2_655 . ? O3 Ce1 O4 74.6(2) . . ? O3 Ce1 O4 142.3(2) 2_655 . ? O1 Ce1 O4 75.0(2) . 2_655 ? O1 Ce1 O4 74.6(2) 2_655 2_655 ? O2 Ce1 O4 75.5(2) . 2_655 ? O2 Ce1 O4 118.5(2) 2_655 2_655 ? O3 Ce1 O4 142.3(2) . 2_655 ? O3 Ce1 O4 74.6(2) 2_655 2_655 ? O4 Ce1 O4 141.1(3) . 2_655 ? O10 W1 O1 105.0(3) . . ? O10 W1 O6 102.3(3) . . ? O1 W1 O6 91.3(3) . . ? O10 W1 O7 101.8(3) . . ? O1 W1 O7 90.7(3) . . ? O6 W1 O7 154.4(3) . . ? O10 W1 O14 96.5(3) . . ? O1 W1 O14 158.4(3) . . ? O6 W1 O14 84.5(3) . . ? O7 W1 O14 84.3(3) . . ? O10 W1 O9 171.3(3) . . ? O1 W1 O9 83.7(3) . . ? O6 W1 O9 77.8(2) . . ? O7 W1 O9 77.1(3) . . ? O14 W1 O9 74.8(2) . . ? O12 W2 O3 104.0(3) . . ? O12 W2 O8 101.2(3) . . ? O3 W2 O8 91.7(3) . . ? O12 W2 O5 101.9(3) . . ? O3 W2 O5 91.0(3) . . ? O8 W2 O5 155.4(3) . . ? O12 W2 O16 97.2(3) . . ? O3 W2 O16 158.8(3) . . ? O8 W2 O16 84.3(3) . . ? O5 W2 O16 84.4(3) . . ? O12 W2 O9 171.7(3) . . ? O3 W2 O9 84.3(3) . . ? O8 W2 O9 78.7(3) . . ? O5 W2 O9 77.2(3) . . ? O16 W2 O9 74.4(2) . . ? O13 W3 O4 104.2(3) . . ? O13 W3 O6 102.3(3) . . ? O4 W3 O6 92.3(3) . . ? O13 W3 O5 101.7(3) . . ? O4 W3 O5 91.0(3) . . ? O6 W3 O5 154.2(3) . . ? O13 W3 O17 96.6(3) . . ? O4 W3 O17 159.2(3) . . ? O6 W3 O17 83.7(3) . . ? O5 W3 O17 84.3(3) . . ? O13 W3 O9 171.2(3) . . ? O4 W3 O9 84.5(3) . . ? O6 W3 O9 77.9(2) . . ? O5 W3 O9 76.9(2) . . ? O17 W3 O9 74.7(2) . . ? O11 W4 O2 103.6(3) . . ? O11 W4 O8 101.6(3) . . ? O2 W4 O8 91.4(3) . . ? O11 W4 O7 104.8(3) . . ? O2 W4 O7 90.4(3) . . ? O8 W4 O7 152.4(3) . . ? O11 W4 O15 100.2(3) . . ? O2 W4 O15 156.2(3) . . ? O8 W4 O15 84.0(3) . . ? O7 W4 O15 83.3(3) . . ? O11 W4 O9 173.3(3) . . ? O2 W4 O9 83.0(3) . . ? O8 W4 O9 76.7(2) . . ? O7 W4 O9 76.1(2) . . ? O15 W4 O9 73.3(2) . . ? O18 W5 O14 102.8(3) . . ? O18 W5 O15 104.0(3) . . ? O14 W5 O15 87.5(3) . . ? O18 W5 O16 103.6(3) . . ? O14 W5 O16 153.6(3) . . ? O15 W5 O16 86.6(3) . . ? O18 W5 O17 102.3(3) . . ? O14 W5 O17 86.6(3) . . ? O15 W5 O17 153.7(3) . . ? O16 W5 O17 87.3(3) . . ? O18 W5 O9 179.1(3) . . ? O14 W5 O9 77.2(2) . . ? O15 W5 O9 77.0(3) . . ? O16 W5 O9 76.4(2) . . ? O17 W5 O9 76.7(3) . . ? O19 Na1 O21 174.1(3) . . ? O19 Na1 O20 90.1(3) . . ? O21 Na1 O20 95.8(3) . . ? O19 Na1 O22 94.3(3) . . ? O21 Na1 O22 84.3(3) . . ? O20 Na1 O22 96.0(3) . . ? O19 Na1 O19 82.8(3) . 5_665 ? O21 Na1 O19 91.3(3) . 5_665 ? O20 Na1 O19 172.0(3) . 5_665 ? O22 Na1 O19 81.0(3) . 5_665 ? O19 Na1 O11 99.1(3) . . ? O21 Na1 O11 82.6(3) . . ? O20 Na1 O11 81.8(3) . . ? O22 Na1 O11 166.4(3) . . ? O19 Na1 O11 102.9(3) 5_665 . ? O19 Na1 Na2 138.1(3) . . ? O21 Na1 Na2 41.45(19) . . ? O20 Na1 Na2 89.6(2) . . ? O22 Na1 Na2 44.19(19) . . ? O19 Na1 Na2 93.3(2) 5_665 . ? O11 Na1 Na2 122.2(2) . . ? O19 Na1 Na1 42.2(2) . 5_665 ? O21 Na1 Na1 131.9(3) . 5_665 ? O20 Na1 Na1 132.1(3) . 5_665 ? O22 Na1 Na1 86.7(2) . 5_665 ? O19 Na1 Na1 40.65(19) 5_665 5_665 ? O11 Na1 Na1 104.8(2) . 5_665 ? Na2 Na1 Na1 121.84(19) . 5_665 ? O21 Na2 O21 105.5(4) . 2_654 ? O21 Na2 O23 81.6(3) . . ? O21 Na2 O23 94.8(3) 2_654 . ? O21 Na2 O23 94.8(3) . 2_654 ? O21 Na2 O23 81.6(3) 2_654 2_654 ? O23 Na2 O23 174.1(4) . 2_654 ? O21 Na2 O22 84.7(2) . . ? O21 Na2 O22 168.8(3) 2_654 . ? O23 Na2 O22 81.9(3) . . ? O23 Na2 O22 102.5(3) 2_654 . ? O21 Na2 O22 168.8(3) . 2_654 ? O21 Na2 O22 84.7(2) 2_654 2_654 ? O23 Na2 O22 102.5(3) . 2_654 ? O23 Na2 O22 81.9(3) 2_654 2_654 ? O22 Na2 O22 85.5(3) . 2_654 ? O21 Na2 Na1 147.3(3) . 2_654 ? O21 Na2 Na1 42.43(18) 2_654 2_654 ? O23 Na2 Na1 93.3(2) . 2_654 ? O23 Na2 Na1 87.2(2) 2_654 2_654 ? O22 Na2 Na1 126.8(2) . 2_654 ? O22 Na2 Na1 43.63(16) 2_654 2_654 ? O21 Na2 Na1 42.43(18) . . ? O21 Na2 Na1 147.3(3) 2_654 . ? O23 Na2 Na1 87.2(2) . . ? O23 Na2 Na1 93.3(2) 2_654 . ? O22 Na2 Na1 43.63(16) . . ? O22 Na2 Na1 126.8(2) 2_654 . ? Na1 Na2 Na1 170.2(2) 2_654 . ? O24 Na3 O27 167.5(4) . . ? O24 Na3 O25 84.1(3) . . ? O27 Na3 O25 99.8(3) . . ? O24 Na3 O26 87.7(4) . . ? O27 Na3 O26 79.8(3) . . ? O25 Na3 O26 105.9(5) . . ? O24 Na3 O20 90.9(3) . 7_665 ? O27 Na3 O20 100.9(3) . 7_665 ? O25 Na3 O20 91.5(4) . 7_665 ? O26 Na3 O20 162.3(5) . 7_665 ? O24 Na3 O10 81.9(3) . . ? O27 Na3 O10 95.4(3) . . ? O25 Na3 O10 164.2(3) . . ? O26 Na3 O10 81.0(4) . . ? O20 Na3 O10 81.4(3) 7_665 . ? O24 Na3 Na4 132.3(3) . . ? O27 Na3 Na4 36.6(2) . . ? O25 Na3 Na4 124.9(3) . . ? O26 Na3 Na4 50.8(3) . . ? O20 Na3 Na4 121.1(2) 7_665 . ? O10 Na3 Na4 70.50(19) . . ? O31 Na4 O28 94.5(4) . . ? O31 Na4 O29 112.6(5) . . ? O28 Na4 O29 87.2(3) . . ? O31 Na4 O32 82.8(4) . . ? O28 Na4 O32 157.1(4) . . ? O29 Na4 O32 114.9(4) . . ? O31 Na4 O27 153.8(5) . . ? O28 Na4 O27 87.0(3) . . ? O29 Na4 O27 93.6(3) . . ? O32 Na4 O27 85.8(3) . . ? O31 Na4 O30 56.3(7) . . ? O28 Na4 O30 130.1(6) . . ? O29 Na4 O30 72.2(6) . . ? O32 Na4 O30 66.4(6) . . ? O27 Na4 O30 137.7(6) . . ? O31 Na4 Na5 44.8(3) . . ? O28 Na4 Na5 138.4(3) . . ? O29 Na4 Na5 113.6(3) . . ? O32 Na4 Na5 39.5(2) . . ? O27 Na4 Na5 124.7(2) . . ? O30 Na4 Na5 42.2(6) . . ? O31 Na4 Na3 119.1(5) . . ? O28 Na4 Na3 85.5(3) . . ? O29 Na4 Na3 128.1(3) . . ? O32 Na4 Na3 76.2(2) . . ? O27 Na4 Na3 34.8(2) . . ? O30 Na4 Na3 142.7(6) . . ? Na5 Na4 Na3 105.38(17) . . ? O32 Na5 O32 170.5(5) 2_655 . ? O32 Na5 O33 88.7(3) 2_655 . ? O32 Na5 O33 98.7(3) . . ? O32 Na5 O33 98.7(3) 2_655 2_655 ? O32 Na5 O33 88.7(3) . 2_655 ? O33 Na5 O33 77.4(5) . 2_655 ? O32 Na5 O30 96.9(7) 2_655 . ? O32 Na5 O30 73.7(7) . . ? O33 Na5 O30 132.6(5) . . ? O33 Na5 O30 146.5(6) 2_655 . ? O32 Na5 O30 73.7(7) 2_655 2_655 ? O32 Na5 O30 96.9(7) . 2_655 ? O33 Na5 O30 146.5(6) . 2_655 ? O33 Na5 O30 132.6(5) 2_655 2_655 ? O30 Na5 O30 29.4(10) . 2_655 ? O32 Na5 O31 99.2(3) 2_655 . ? O32 Na5 O31 77.5(3) . . ? O33 Na5 O31 73.4(4) . . ? O33 Na5 O31 145.1(5) 2_655 . ? O30 Na5 O31 59.2(6) . . ? O30 Na5 O31 81.3(6) 2_655 . ? O32 Na5 O31 77.5(3) 2_655 2_655 ? O32 Na5 O31 99.2(3) . 2_655 ? O33 Na5 O31 145.1(5) . 2_655 ? O33 Na5 O31 73.4(4) 2_655 2_655 ? O30 Na5 O31 81.3(6) . 2_655 ? O30 Na5 O31 59.2(6) 2_655 2_655 ? O31 Na5 O31 139.9(8) . 2_655 ? O32 Na5 Na4 39.6(2) 2_655 2_655 ? O32 Na5 Na4 134.7(3) . 2_655 ? O33 Na5 Na4 125.7(3) . 2_655 ? O33 Na5 Na4 92.7(2) 2_655 2_655 ? O30 Na5 Na4 80.9(6) . 2_655 ? O30 Na5 Na4 51.5(5) 2_655 2_655 ? O31 Na5 Na4 119.8(4) . 2_655 ? O31 Na5 Na4 39.3(3) 2_655 2_655 ? O32 Na5 Na4 134.7(3) 2_655 . ? O32 Na5 Na4 39.6(2) . . ? O33 Na5 Na4 92.7(2) . . ? O33 Na5 Na4 125.7(3) 2_655 . ? O30 Na5 Na4 51.5(5) . . ? O30 Na5 Na4 80.9(6) 2_655 . ? O31 Na5 Na4 39.3(3) . . ? O31 Na5 Na4 119.8(4) 2_655 . ? Na4 Na5 Na4 132.4(3) 2_655 . ? W1 O1 Ce1 129.8(3) . . ? W4 O2 Ce1 130.4(3) . . ? W2 O3 Ce1 128.7(3) . . ? W3 O4 Ce1 128.5(3) . . ? W2 O5 W3 114.3(3) . . ? W1 O6 W3 114.0(3) . . ? W4 O7 W1 116.4(3) . . ? W2 O8 W4 115.1(3) . . ? W5 O9 W2 92.8(2) . . ? W5 O9 W3 93.2(2) . . ? W2 O9 W3 91.1(2) . . ? W5 O9 W1 91.7(2) . . ? W2 O9 W1 175.5(3) . . ? W3 O9 W1 89.6(2) . . ? W5 O9 W4 91.7(2) . . ? W2 O9 W4 89.0(2) . . ? W3 O9 W4 175.1(3) . . ? W1 O9 W4 89.9(2) . . ? W1 O10 Na3 131.6(3) . . ? W4 O11 Na1 149.4(4) . . ? W5 O14 W1 116.4(3) . . ? W5 O15 W4 118.1(3) . . ? W5 O16 W2 116.4(3) . . ? W5 O17 W3 115.3(3) . . ? Na1 O19 Na1 97.2(3) . 5_665 ? Na1 O20 Na3 134.2(3) . 7_665 ? Na2 O21 Na1 96.1(3) . . ? Na1 O22 Na2 92.2(2) . . ? Na3 O27 Na4 108.6(3) . . ? O30 O30 Na5 75.3(5) 2_655 . ? O30 O30 Na4 161.5(6) 2_655 . ? Na5 O30 Na4 86.3(8) . . ? Na4 O31 Na5 95.9(5) . . ? Na5 O32 Na4 100.8(3) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.259 _refine_diff_density_min -3.344 _refine_diff_density_rms 0.397