# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Wolfgang Runde' _publ_contact_author_address ; Los Alamos National Laboratory PO Box 1663 Los Alamos NM 87545 UNITED STATES OF AMERICA ; _publ_contact_author_email RUNDE@LANL.GOV _publ_section_title ; Synthesis and structural characterization of a molecular plutonium (IV) compound constructed from dimeric building blocks ; loop_ _publ_author_name 'Wolfgang Runde' 'Lia F. Brodnax' 'George Goff' 'Shane Peper' 'Brian L. Scott' 'Felicia L. Taw' # Attachment 'apx115rev.cif' data_apx115 _database_code_depnum_ccdc_archive 'CCDC 630066' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H24 Na8 O34 Pu2' _chemical_formula_weight 1308.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pu Pu -9.4100 4.3056 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.861(8) _cell_length_b 8.889(8) _cell_length_c 11.511(10) _cell_angle_alpha 69.451(12) _cell_angle_beta 67.990(11) _cell_angle_gamma 64.692(11) _cell_volume 739.9(11) _cell_formula_units_Z 1 _cell_measurement_temperature 141(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular plate' _exptl_crystal_colour green _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.936 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 4.665 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7672 _exptl_absorpt_correction_T_max 0.9548 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 141(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 '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 8192 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.70 _reflns_number_total 3522 _reflns_number_gt 3247 _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^)+(0.0600P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3522 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Pu1 Pu 0.86237(2) 0.43412(2) 0.149061(18) 0.00904(9) Uani 1 1 d . . . Na1 Na 0.0166(3) 0.7379(3) 0.4728(2) 0.0185(5) Uani 1 1 d . . . Na2 Na 0.3073(3) 0.8484(3) 0.4876(2) 0.0167(5) Uani 1 1 d . . . Na3 Na 1.2851(3) 0.0520(3) 0.0099(2) 0.0188(5) Uani 1 1 d . . . Na4 Na 0.7029(4) 0.4304(4) -0.1035(3) 0.0299(7) Uani 1 1 d . . . O1 O 0.9695(5) 0.2426(5) 0.3335(4) 0.0144(8) Uani 1 1 d . . . O2 O 1.0205(5) 0.1364(5) 0.1715(4) 0.0137(8) Uani 1 1 d . . . O3 O 1.1147(5) -0.0369(5) 0.3457(4) 0.0182(9) Uani 1 1 d . . . O4 O 0.7784(5) 0.5817(5) 0.3153(4) 0.0140(8) Uani 1 1 d . . . O5 O 0.6506(5) 0.7156(5) 0.1599(4) 0.0131(8) Uani 1 1 d . . . O6 O 0.5669(5) 0.8359(5) 0.3255(4) 0.0158(8) Uani 1 1 d . . . O7 O 0.6257(5) 0.3381(6) 0.3154(4) 0.0198(9) Uani 1 1 d . . . O8 O 0.6278(6) 0.3974(7) 0.1140(5) 0.0277(11) Uani 1 1 d . . . O9 O 0.4091(5) 0.3251(5) 0.2641(4) 0.0179(9) Uani 1 1 d . . . O10 O 1.1482(5) 0.4291(5) 0.0661(4) 0.0162(9) Uani 1 1 d . . . O11 O 1.0339(5) 0.6120(5) 0.0589(4) 0.0169(9) Uani 1 1 d . . . O12 O 0.3271(5) 0.5954(5) 0.4485(4) 0.0174(9) Uani 1 1 d . . . O13 O 0.0669(10) 0.5367(17) 0.3706(15) 0.145(6) Uani 1 1 d . . . O14 O -0.2894(5) 0.8782(6) 0.4979(5) 0.0219(10) Uani 1 1 d . . . O15 O 0.6772(6) 0.2202(6) -0.1540(5) 0.0199(9) Uani 1 1 d . . . O16 O 1.1304(8) 0.0477(9) -0.1183(7) 0.0507(18) Uani 1 1 d . . . O17 O 1.5642(6) -0.0925(6) -0.1268(4) 0.0189(9) Uani 1 1 d . . . C1 C 1.0382(7) 0.1080(7) 0.2868(6) 0.0137(11) Uani 1 1 d . . . C2 C 0.6608(7) 0.7169(7) 0.2686(6) 0.0112(10) Uani 1 1 d . . . C3 C 0.5517(7) 0.3510(7) 0.2315(6) 0.0127(11) 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 Pu1 0.00941(12) 0.00835(12) 0.00754(12) -0.00049(8) -0.00204(8) -0.00262(8) Na1 0.0148(11) 0.0209(12) 0.0188(13) -0.0045(10) -0.0043(9) -0.0054(9) Na2 0.0150(10) 0.0193(12) 0.0146(12) -0.0035(10) -0.0041(9) -0.0047(9) Na3 0.0159(11) 0.0172(12) 0.0154(13) 0.0015(10) -0.0017(9) -0.0047(9) Na4 0.0411(16) 0.0204(13) 0.0384(18) 0.0030(12) -0.0275(14) -0.0127(12) O1 0.0173(19) 0.0107(18) 0.010(2) 0.0004(15) -0.0061(16) -0.0006(15) O2 0.0185(19) 0.0122(19) 0.007(2) -0.0022(16) -0.0020(16) -0.0036(16) O3 0.020(2) 0.0108(19) 0.015(2) 0.0018(16) -0.0055(17) 0.0002(16) O4 0.0153(18) 0.0119(19) 0.013(2) -0.0011(16) -0.0068(16) -0.0013(15) O5 0.0158(19) 0.0123(19) 0.008(2) -0.0008(16) -0.0031(16) -0.0036(15) O6 0.0154(19) 0.0123(19) 0.016(2) -0.0051(17) -0.0040(16) -0.0006(15) O7 0.020(2) 0.027(2) 0.014(2) 0.0049(18) -0.0084(18) -0.0132(18) O8 0.037(3) 0.043(3) 0.014(2) -0.004(2) -0.003(2) -0.029(2) O9 0.0151(19) 0.019(2) 0.020(2) 0.0008(18) -0.0052(17) -0.0100(16) O10 0.0161(19) 0.014(2) 0.016(2) -0.0009(17) -0.0039(17) -0.0055(16) O11 0.0190(19) 0.015(2) 0.014(2) -0.0014(17) -0.0040(17) -0.0057(16) O12 0.018(2) 0.015(2) 0.016(2) -0.0019(17) -0.0053(17) -0.0029(16) O13 0.040(4) 0.188(11) 0.289(16) -0.204(13) -0.039(6) 0.001(5) O14 0.0159(19) 0.029(2) 0.023(3) -0.007(2) -0.0017(18) -0.0111(18) O15 0.022(2) 0.017(2) 0.020(2) -0.0048(18) -0.0069(18) -0.0039(17) O16 0.058(4) 0.077(5) 0.046(4) -0.020(3) -0.006(3) -0.051(4) O17 0.019(2) 0.017(2) 0.017(2) -0.0047(18) -0.0014(17) -0.0055(17) C1 0.010(2) 0.014(3) 0.015(3) -0.002(2) -0.002(2) -0.004(2) C2 0.012(2) 0.012(2) 0.011(3) -0.002(2) 0.000(2) -0.007(2) C3 0.014(2) 0.009(2) 0.013(3) -0.001(2) -0.005(2) -0.002(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 Pu1 O10 2.334(4) . ? Pu1 O11 2.337(5) 2_765 ? Pu1 O10 2.363(5) 2_765 ? Pu1 O11 2.368(5) . ? Pu1 O2 2.378(4) . ? Pu1 O4 2.407(5) . ? Pu1 O5 2.414(4) . ? Pu1 O8 2.427(5) . ? Pu1 O1 2.429(4) . ? Pu1 O7 2.483(4) . ? Pu1 C1 2.847(6) . ? Pu1 C2 2.855(6) . ? Na1 O13 2.277(8) . ? Na1 O3 2.320(5) 1_465 ? Na1 O1 2.348(5) 2_666 ? Na1 O14 2.401(5) . ? Na1 O12 2.438(5) . ? Na1 O13 2.685(16) 2_566 ? Na1 Na2 3.201(4) . ? Na1 Na2 3.625(4) 2_576 ? Na1 Na1 4.176(6) 2_566 ? Na2 O6 2.344(5) . ? Na2 O12 2.368(5) . ? Na2 O7 2.402(5) 2_666 ? Na2 O14 2.427(6) 2_576 ? Na2 O3 2.461(5) 1_465 ? Na2 O1 2.766(5) 2_666 ? Na2 Na1 3.625(4) 2_576 ? Na2 Pu1 4.147(4) 2_666 ? Na3 O15 2.372(5) 2_755 ? Na3 O16 2.379(7) . ? Na3 O2 2.393(5) . ? Na3 O5 2.397(5) 2_765 ? Na3 O17 2.413(6) 2_855 ? Na3 O17 2.455(5) . ? Na3 Na3 3.449(6) 2_855 ? Na3 Na4 4.002(5) 2_755 ? Na3 Pu1 4.091(4) 2_765 ? Na4 O15 2.259(6) . ? Na4 O8 2.280(6) . ? Na4 O10 2.387(5) 2_765 ? Na4 O11 2.420(5) 2_765 ? Na4 O9 2.416(5) 2_665 ? Na4 O8 2.692(6) 2_665 ? Na4 C3 2.788(6) 2_665 ? Na4 O13 2.980(15) 2_665 ? Na4 Na4 3.461(7) 2_665 ? Na4 Na3 4.002(5) 2_755 ? O1 C1 1.294(7) . ? O1 Na1 2.348(5) 2_666 ? O1 Na2 2.766(5) 2_666 ? O2 C1 1.318(7) . ? O3 C1 1.251(7) . ? O3 Na1 2.320(5) 1_645 ? O3 Na2 2.461(5) 1_645 ? O4 C2 1.310(7) . ? O5 C2 1.292(7) . ? O5 Na3 2.397(5) 2_765 ? O6 C2 1.251(7) . ? O7 C3 1.307(7) . ? O7 Na2 2.402(5) 2_666 ? O8 C3 1.272(8) . ? O8 Na4 2.692(6) 2_665 ? O9 C3 1.274(7) . ? O9 Na4 2.416(5) 2_665 ? O10 O11 1.495(6) . ? O10 Pu1 2.363(5) 2_765 ? O10 Na4 2.387(5) 2_765 ? O11 Pu1 2.337(5) 2_765 ? O11 Na4 2.420(5) 2_765 ? O13 Na1 2.685(16) 2_566 ? O13 Na4 2.980(15) 2_665 ? O14 Na2 2.427(6) 2_576 ? O15 Na3 2.372(5) 2_755 ? O17 Na3 2.413(6) 2_855 ? C3 Na4 2.788(6) 2_665 ? 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 O10 Pu1 O11 71.35(15) . 2_765 ? O10 Pu1 O10 82.65(15) . 2_765 ? O11 Pu1 O10 37.10(15) 2_765 2_765 ? O10 Pu1 O11 37.08(14) . . ? O11 Pu1 O11 82.86(16) 2_765 . ? O10 Pu1 O11 70.31(15) 2_765 . ? O10 Pu1 O2 77.98(15) . . ? O11 Pu1 O2 74.47(14) 2_765 . ? O10 Pu1 O2 111.42(14) 2_765 . ? O11 Pu1 O2 115.06(15) . . ? O10 Pu1 O4 97.40(15) . . ? O11 Pu1 O4 157.75(15) 2_765 . ? O10 Pu1 O4 124.39(15) 2_765 . ? O11 Pu1 O4 77.13(15) . . ? O2 Pu1 O4 123.02(14) . . ? O10 Pu1 O5 113.97(15) . . ? O11 Pu1 O5 112.18(14) 2_765 . ? O10 Pu1 O5 75.27(14) 2_765 . ? O11 Pu1 O5 76.95(16) . . ? O2 Pu1 O5 167.44(14) . . ? O4 Pu1 O5 53.87(14) . . ? O10 Pu1 O8 146.09(17) . . ? O11 Pu1 O8 74.84(16) 2_765 . ? O10 Pu1 O8 71.87(16) 2_765 . ? O11 Pu1 O8 139.96(16) . . ? O2 Pu1 O8 90.64(17) . . ? O4 Pu1 O8 115.30(16) . . ? O5 Pu1 O8 81.26(17) . . ? O10 Pu1 O1 81.83(15) . . ? O11 Pu1 O1 126.09(15) 2_765 . ? O10 Pu1 O1 160.96(15) 2_765 . ? O11 Pu1 O1 102.83(15) . . ? O2 Pu1 O1 54.31(14) . . ? O4 Pu1 O1 68.75(15) . . ? O5 Pu1 O1 121.40(14) . . ? O8 Pu1 O1 117.20(16) . . ? O10 Pu1 O7 152.94(15) . . ? O11 Pu1 O7 122.84(15) 2_765 . ? O10 Pu1 O7 123.06(14) 2_765 . ? O11 Pu1 O7 152.51(16) . . ? O2 Pu1 O7 83.96(15) . . ? O4 Pu1 O7 75.76(16) . . ? O5 Pu1 O7 83.49(16) . . ? O8 Pu1 O7 52.80(16) . . ? O1 Pu1 O7 71.25(15) . . ? O10 Pu1 C1 78.84(16) . . ? O11 Pu1 C1 100.67(16) 2_765 . ? O10 Pu1 C1 137.70(16) 2_765 . ? O11 Pu1 C1 111.38(16) . . ? O2 Pu1 C1 27.38(15) . . ? O4 Pu1 C1 95.65(17) . . ? O5 Pu1 C1 147.00(16) . . ? O8 Pu1 C1 105.22(18) . . ? O1 Pu1 C1 26.93(15) . . ? O7 Pu1 C1 75.91(16) . . ? O10 Pu1 C2 108.50(15) . . ? O11 Pu1 C2 137.24(15) 2_765 . ? O10 Pu1 C2 100.26(16) 2_765 . ? O11 Pu1 C2 76.45(16) . . ? O2 Pu1 C2 148.29(15) . . ? O4 Pu1 C2 27.15(15) . . ? O5 Pu1 C2 26.76(15) . . ? O8 Pu1 C2 97.97(17) . . ? O1 Pu1 C2 95.09(16) . . ? O7 Pu1 C2 77.39(16) . . ? C1 Pu1 C2 121.61(18) . . ? O13 Na1 O3 115.7(4) . 1_465 ? O13 Na1 O1 139.9(4) . 2_666 ? O3 Na1 O1 95.28(18) 1_465 2_666 ? O13 Na1 O14 99.7(2) . . ? O3 Na1 O14 100.33(18) 1_465 . ? O1 Na1 O14 98.84(18) 2_666 . ? O13 Na1 O12 80.5(2) . . ? O3 Na1 O12 79.78(17) 1_465 . ? O1 Na1 O12 80.84(16) 2_666 . ? O14 Na1 O12 179.7(2) . . ? O13 Na1 O13 65.7(6) . 2_566 ? O3 Na1 O13 173.9(2) 1_465 2_566 ? O1 Na1 O13 81.0(3) 2_666 2_566 ? O14 Na1 O13 85.1(2) . 2_566 ? O12 Na1 O13 94.7(2) . 2_566 ? O13 Na1 Na2 125.3(2) . . ? O3 Na1 Na2 49.88(13) 1_465 . ? O1 Na1 Na2 57.37(12) 2_666 . ? O14 Na1 Na2 132.55(16) . . ? O12 Na1 Na2 47.32(13) . . ? O13 Na1 Na2 124.2(2) 2_566 . ? O13 Na1 Na2 136.2(3) . 2_576 ? O3 Na1 Na2 67.18(14) 1_465 2_576 ? O1 Na1 Na2 77.73(13) 2_666 2_576 ? O14 Na1 Na2 41.62(12) . 2_576 ? O12 Na1 Na2 138.28(15) . 2_576 ? O13 Na1 Na2 116.4(2) 2_566 2_576 ? Na2 Na1 Na2 91.12(11) . 2_576 ? O13 Na1 Na1 35.9(4) . 2_566 ? O3 Na1 Na1 151.16(17) 1_465 2_566 ? O1 Na1 Na1 108.46(15) 2_666 2_566 ? O14 Na1 Na1 92.15(15) . 2_566 ? O12 Na1 Na1 87.89(14) . 2_566 ? O13 Na1 Na1 29.8(2) 2_566 2_566 ? Na2 Na1 Na1 132.54(11) . 2_566 ? Na2 Na1 Na1 132.83(11) 2_576 2_566 ? O6 Na2 O12 87.37(17) . . ? O6 Na2 O7 108.70(17) . 2_666 ? O12 Na2 O7 83.57(18) . 2_666 ? O6 Na2 O14 88.94(17) . 2_576 ? O12 Na2 O14 173.5(2) . 2_576 ? O7 Na2 O14 102.67(19) 2_666 2_576 ? O6 Na2 O3 97.20(18) . 1_465 ? O12 Na2 O3 78.40(16) . 1_465 ? O7 Na2 O3 147.60(18) 2_666 1_465 ? O14 Na2 O3 96.81(17) 2_576 1_465 ? O6 Na2 O1 161.04(17) . 2_666 ? O12 Na2 O1 73.94(15) . 2_666 ? O7 Na2 O1 66.80(15) 2_666 2_666 ? O14 Na2 O1 109.97(16) 2_576 2_666 ? O3 Na2 O1 82.35(16) 1_465 2_666 ? O6 Na2 Na1 122.52(16) . . ? O12 Na2 Na1 49.19(12) . . ? O7 Na2 Na1 102.17(14) 2_666 . ? O14 Na2 Na1 129.75(14) 2_576 . ? O3 Na2 Na1 46.12(12) 1_465 . ? O1 Na2 Na1 45.62(12) 2_666 . ? O6 Na2 Na1 119.13(14) . 2_576 ? O12 Na2 Na1 137.90(14) . 2_576 ? O7 Na2 Na1 113.53(15) 2_666 2_576 ? O14 Na2 Na1 41.06(12) 2_576 2_576 ? O3 Na2 Na1 66.97(12) 1_465 2_576 ? O1 Na2 Na1 78.28(12) 2_666 2_576 ? Na1 Na2 Na1 88.88(11) . 2_576 ? O6 Na2 Pu1 138.17(13) . 2_666 ? O12 Na2 Pu1 75.96(14) . 2_666 ? O7 Na2 Pu1 32.50(11) 2_666 2_666 ? O14 Na2 Pu1 110.24(14) 2_576 2_666 ? O3 Na2 Pu1 115.96(14) 1_465 2_666 ? O1 Na2 Pu1 34.32(9) 2_666 2_666 ? Na1 Na2 Pu1 73.41(8) . 2_666 ? Na1 Na2 Pu1 97.85(8) 2_576 2_666 ? O15 Na3 O16 102.3(2) 2_755 . ? O15 Na3 O2 83.40(17) 2_755 . ? O16 Na3 O2 90.3(2) . . ? O15 Na3 O5 160.87(18) 2_755 2_765 ? O16 Na3 O5 85.5(2) . 2_765 ? O2 Na3 O5 114.29(18) . 2_765 ? O15 Na3 O17 84.56(18) 2_755 2_855 ? O16 Na3 O17 173.0(2) . 2_855 ? O2 Na3 O17 89.53(18) . 2_855 ? O5 Na3 O17 88.23(18) 2_765 2_855 ? O15 Na3 O17 84.94(18) 2_755 . ? O16 Na3 O17 91.8(2) . . ? O2 Na3 O17 168.34(18) . . ? O5 Na3 O17 77.32(17) 2_765 . ? O17 Na3 O17 89.78(19) 2_855 . ? O15 Na3 Na3 82.58(14) 2_755 2_855 ? O16 Na3 Na3 135.8(2) . 2_855 ? O2 Na3 Na3 133.75(18) . 2_855 ? O5 Na3 Na3 79.76(13) 2_765 2_855 ? O17 Na3 Na3 45.39(12) 2_855 2_855 ? O17 Na3 Na3 44.39(13) . 2_855 ? O15 Na3 Na4 29.43(13) 2_755 2_755 ? O16 Na3 Na4 74.55(19) . 2_755 ? O2 Na3 Na4 93.09(13) . 2_755 ? O5 Na3 Na4 146.27(15) 2_765 2_755 ? O17 Na3 Na4 112.40(14) 2_855 2_755 ? O17 Na3 Na4 76.43(14) . 2_755 ? Na3 Na3 Na4 95.72(10) 2_855 2_755 ? O15 Na3 Pu1 114.23(14) 2_755 . ? O16 Na3 Pu1 88.94(19) . . ? O2 Na3 Pu1 31.30(10) . . ? O5 Na3 Pu1 83.01(13) 2_765 . ? O17 Na3 Pu1 87.32(14) 2_855 . ? O17 Na3 Pu1 160.19(14) . . ? Na3 Na3 Pu1 129.58(12) 2_855 . ? Na4 Na3 Pu1 122.65(9) 2_755 . ? O15 Na3 Pu1 164.44(15) 2_755 2_765 ? O16 Na3 Pu1 84.22(19) . 2_765 ? O2 Na3 Pu1 82.45(12) . 2_765 ? O5 Na3 Pu1 31.86(10) 2_765 2_765 ? O17 Na3 Pu1 88.87(13) 2_855 2_765 ? O17 Na3 Pu1 109.18(13) . 2_765 ? Na3 Na3 Pu1 102.71(10) 2_855 2_765 ? Na4 Na3 Pu1 158.30(8) 2_755 2_765 ? Pu1 Na3 Pu1 51.21(5) . 2_765 ? O15 Na4 O8 111.0(2) . . ? O15 Na4 O10 155.8(2) . 2_765 ? O8 Na4 O10 74.04(18) . 2_765 ? O15 Na4 O11 120.4(2) . 2_765 ? O8 Na4 O11 76.00(18) . 2_765 ? O10 Na4 O11 36.24(15) 2_765 2_765 ? O15 Na4 O9 100.9(2) . 2_665 ? O8 Na4 O9 129.0(2) . 2_665 ? O10 Na4 O9 92.47(18) 2_765 2_665 ? O11 Na4 O9 120.02(19) 2_765 2_665 ? O15 Na4 O8 85.42(18) . 2_665 ? O8 Na4 O8 92.2(2) . 2_665 ? O10 Na4 O8 118.46(19) 2_765 2_665 ? O11 Na4 O8 154.0(2) 2_765 2_665 ? O9 Na4 O8 51.18(15) 2_665 2_665 ? O15 Na4 C3 85.09(19) . 2_665 ? O8 Na4 C3 117.3(2) . 2_665 ? O10 Na4 C3 114.3(2) 2_765 2_665 ? O11 Na4 C3 146.5(2) 2_765 2_665 ? O9 Na4 C3 27.15(15) 2_665 2_665 ? O8 Na4 C3 26.77(16) 2_665 2_665 ? O15 Na4 O13 82.4(2) . 2_665 ? O8 Na4 O13 156.4(2) . 2_665 ? O10 Na4 O13 86.0(2) 2_765 2_665 ? O11 Na4 O13 80.4(2) 2_765 2_665 ? O9 Na4 O13 63.1(3) 2_665 2_665 ? O8 Na4 O13 108.7(2) 2_665 2_665 ? C3 Na4 O13 82.1(3) 2_665 2_665 ? O15 Na4 Na4 100.03(18) . 2_665 ? O8 Na4 Na4 50.99(15) . 2_665 ? O10 Na4 Na4 100.92(18) 2_765 2_665 ? O11 Na4 Na4 122.64(19) 2_765 2_665 ? O9 Na4 Na4 85.82(16) 2_665 2_665 ? O8 Na4 Na4 41.17(13) 2_665 2_665 ? C3 Na4 Na4 66.93(16) 2_665 2_665 ? O13 Na4 Na4 148.5(3) 2_665 2_665 ? O15 Na4 Pu1 132.86(16) . . ? O8 Na4 Pu1 39.76(13) . . ? O10 Na4 Pu1 38.75(11) 2_765 . ? O11 Na4 Pu1 38.27(11) 2_765 . ? O9 Na4 Pu1 126.19(15) 2_665 . ? O8 Na4 Pu1 121.92(15) 2_665 . ? C3 Na4 Pu1 137.07(16) 2_665 . ? O13 Na4 Pu1 116.93(19) 2_665 . ? Na4 Na4 Pu1 84.53(13) 2_665 . ? O15 Na4 Na3 31.05(14) . 2_755 ? O8 Na4 Na3 83.45(16) . 2_755 ? O10 Na4 Na3 134.88(15) 2_765 2_755 ? O11 Na4 Na3 100.90(13) 2_765 2_755 ? O9 Na4 Na3 131.22(15) 2_665 2_755 ? O8 Na4 Na3 100.65(14) 2_665 2_755 ? C3 Na4 Na3 110.76(15) 2_665 2_755 ? O13 Na4 Na3 102.8(2) 2_665 2_755 ? Na4 Na4 Na3 93.94(12) 2_665 2_755 ? Pu1 Na4 Na3 102.21(8) . 2_755 ? C1 O1 Na1 127.2(4) . 2_666 ? C1 O1 Pu1 94.9(3) . . ? Na1 O1 Pu1 137.8(2) 2_666 . ? C1 O1 Na2 95.4(3) . 2_666 ? Na1 O1 Na2 77.00(15) 2_666 2_666 ? Pu1 O1 Na2 105.73(16) . 2_666 ? C1 O2 Pu1 96.6(3) . . ? C1 O2 Na3 115.2(3) . . ? Pu1 O2 Na3 117.17(18) . . ? C1 O3 Na1 130.7(4) . 1_645 ? C1 O3 Na2 135.9(4) . 1_645 ? Na1 O3 Na2 84.01(16) 1_645 1_645 ? C2 O4 Pu1 95.8(3) . . ? C2 O5 Na3 112.5(3) . 2_765 ? C2 O5 Pu1 96.0(3) . . ? Na3 O5 Pu1 116.53(18) 2_765 . ? C2 O6 Na2 126.6(4) . . ? C3 O7 Na2 139.6(4) . 2_666 ? C3 O7 Pu1 93.9(3) . . ? Na2 O7 Pu1 116.18(18) 2_666 . ? C3 O8 Na4 157.9(4) . . ? C3 O8 Pu1 97.5(4) . . ? Na4 O8 Pu1 103.30(19) . . ? C3 O8 Na4 80.8(3) . 2_665 ? Na4 O8 Na4 87.8(2) . 2_665 ? Pu1 O8 Na4 140.3(2) . 2_665 ? C3 O9 Na4 92.9(4) . 2_665 ? O11 O10 Pu1 72.7(2) . . ? O11 O10 Pu1 70.5(2) . 2_765 ? Pu1 O10 Pu1 97.35(15) . 2_765 ? O11 O10 Na4 73.0(2) . 2_765 ? Pu1 O10 Na4 131.8(2) . 2_765 ? Pu1 O10 Na4 102.03(17) 2_765 2_765 ? O10 O11 Pu1 72.4(2) . 2_765 ? O10 O11 Pu1 70.2(2) . . ? Pu1 O11 Pu1 97.14(16) 2_765 . ? O10 O11 Na4 70.7(2) . 2_765 ? Pu1 O11 Na4 101.84(18) 2_765 2_765 ? Pu1 O11 Na4 128.4(2) . 2_765 ? Na2 O12 Na1 83.49(16) . . ? Na1 O13 Na1 114.3(6) . 2_566 ? Na1 O13 Na4 115.3(5) . 2_665 ? Na1 O13 Na4 128.1(3) 2_566 2_665 ? Na1 O14 Na2 97.32(18) . 2_576 ? Na4 O15 Na3 119.5(2) . 2_755 ? Na3 O17 Na3 90.22(19) 2_855 . ? O3 C1 O1 123.1(6) . . ? O3 C1 O2 122.7(5) . . ? O1 C1 O2 114.3(5) . . ? O3 C1 Pu1 178.6(5) . . ? O1 C1 Pu1 58.2(3) . . ? O2 C1 Pu1 56.1(3) . . ? O6 C2 O5 123.5(5) . . ? O6 C2 O4 122.3(5) . . ? O5 C2 O4 114.1(5) . . ? O6 C2 Pu1 176.6(4) . . ? O5 C2 Pu1 57.2(3) . . ? O4 C2 Pu1 57.0(3) . . ? O9 C3 O8 121.4(6) . . ? O9 C3 O7 122.8(5) . . ? O8 C3 O7 115.7(5) . . ? O9 C3 Na4 59.9(3) . 2_665 ? O8 C3 Na4 72.4(3) . 2_665 ? O7 C3 Na4 143.5(4) . 2_665 ? O9 C3 Pu1 175.9(4) . . ? O8 C3 Pu1 56.6(3) . . ? O7 C3 Pu1 59.2(3) . . ? Na4 C3 Pu1 116.2(2) 2_665 . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.721 _refine_diff_density_min -2.284 _refine_diff_density_rms 0.274