# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Andrew Gaunt' _publ_contact_author_email gaunt@lanl.gov loop_ _publ_author_name 'Andrew Gaunt' 'Sean Reilly' 'Brian Scott' 'Giuseppe Modolo' 'Mark Sarsfield' W.Verboom 'Mudassir Iqbal' data_xpl210_005 _database_code_depnum_ccdc_archive 'CCDC 891841' #TrackingRef '- TMDGA Pu complex MeCN solvate CCDC 891841.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H51 N11 O21 Pu' _chemical_formula_weight 1092.75 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' Pu Pu -9.4100 4.3056 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2980(16) _cell_length_b 37.077(6) _cell_length_c 10.7859(17) _cell_angle_alpha 90.00 _cell_angle_beta 95.598(2) _cell_angle_gamma 90.00 _cell_volume 4098.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.776 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 1.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7725 _exptl_absorpt_correction_T_max 0.8483 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 SMART 1k CCD' _diffrn_measurement_method '\f 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 40321 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7780 _reflns_number_gt 7713 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 4.210 (Bruker, 1996)' _computing_cell_refinement 'SAINT 4.05 (Bruker, 1996)' _computing_data_reduction 'SAINT 4.05 (Bruker, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker, 2001)' _computing_publication_material 'SHELXTL 6.10 (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The ligand atomic positions O3 O4 O9 N3 and N6 were refined with restrained anisotropic temperature factors to force convergence. ; _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^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7780 _refine_ls_number_parameters 544 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0886 _refine_ls_wR_factor_ref 0.1623 _refine_ls_wR_factor_gt 0.1622 _refine_ls_goodness_of_fit_ref 4.433 _refine_ls_restrained_S_all 4.431 _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 Pu1 Pu 0.53445(3) 0.116538(8) 0.29480(3) 0.01974(13) Uani 1 1 d . . . N1 N 0.3002(8) 0.0314(2) 0.4694(7) 0.0257(18) Uani 1 1 d . . . N2 N 0.7887(8) 0.0553(2) 0.0574(7) 0.0231(17) Uani 1 1 d . . . N3 N 0.3020(8) 0.1081(2) -0.0772(7) 0.0249(18) Uani 1 1 d U . . N4 N 0.7851(9) 0.2142(2) 0.2684(8) 0.033(2) Uani 1 1 d . . . N5 N 0.2682(8) 0.2092(2) 0.3567(7) 0.0262(19) Uani 1 1 d . . . N6 N 0.8157(7) 0.1151(2) 0.6329(7) 0.0214(16) Uani 1 1 d U . . N7 N 0.5491(8) 0.0683(2) 0.8043(7) 0.0266(19) Uani 1 1 d . . . N8 N 0.5252(10) 0.2674(2) 0.3022(8) 0.034(2) Uani 1 1 d . . . N9 N 0.0075(10) 0.1773(3) 0.9858(10) 0.043(3) Uani 1 1 d . . . N10 N 0.0049(9) 0.0161(2) 0.2652(8) 0.032(2) Uani 1 1 d . . . N11 N 0.1155(12) 0.1493(3) 0.5093(10) 0.060(3) Uani 1 1 d . . . O1 O 0.3876(7) 0.08231(17) 0.3940(6) 0.0241(15) Uani 1 1 d . . . O2 O 0.5417(6) 0.04972(16) 0.2648(5) 0.0200(14) Uani 1 1 d . . . O3 O 0.7007(6) 0.09369(17) 0.1872(6) 0.0228(14) Uani 1 1 d U . . O4 O 0.4036(7) 0.10045(17) 0.1169(6) 0.0234(14) Uani 1 1 d U . . O5 O 0.5459(8) 0.15631(19) 0.1139(6) 0.0343(18) Uani 1 1 d . . . O6 O 0.6833(7) 0.16342(17) 0.3166(6) 0.0281(16) Uani 1 1 d . . . O7 O 0.3701(7) 0.15899(17) 0.2955(6) 0.0280(16) Uani 1 1 d . . . O8 O 0.5113(6) 0.14889(16) 0.4947(5) 0.0199(13) Uani 1 1 d . . . O9 O 0.6802(6) 0.10091(17) 0.4630(6) 0.0219(14) Uani 1 1 d U . . O11 O 0.5011(8) 0.0433(2) 0.8659(7) 0.0386(19) Uani 1 1 d . . . O12 O 0.5950(8) 0.09561(19) 0.8550(7) 0.0395(19) Uani 1 1 d . . . O13 O 0.5429(10) 0.0651(2) 0.6898(7) 0.058(3) Uani 1 1 d . . . O14 O 0.5567(9) 0.2511(2) 0.3997(8) 0.051(2) Uani 1 1 d . . . O15 O 0.5603(13) 0.2989(2) 0.2933(8) 0.086(4) Uani 1 1 d . . . O16 O 0.4705(10) 0.2506(3) 0.2125(8) 0.066(3) Uani 1 1 d . . . O17 O -0.0742(11) 0.1730(4) 1.0663(13) 0.098(4) Uani 1 1 d . . . O18 O 0.0019(15) 0.2020(3) 0.9133(13) 0.116(6) Uani 1 1 d . . . O19 O 0.0903(11) 0.1540(3) 0.9881(10) 0.081(3) Uani 1 1 d . . . O20 O 0.1035(8) 0.0305(2) 0.2268(8) 0.046(2) Uani 1 1 d . . . O21 O -0.0222(10) -0.0154(2) 0.2331(8) 0.056(2) Uani 1 1 d . . . O22 O -0.0661(10) 0.0332(3) 0.3315(8) 0.063(3) Uani 1 1 d . . . C1 C 0.2282(12) 0.0519(3) 0.5548(11) 0.044(3) Uani 1 1 d . . . H1A H 0.2525 0.0768 0.5521 0.066 Uiso 1 1 calc R . . H1B H 0.2481 0.0428 0.6379 0.066 Uiso 1 1 calc R . . H1C H 0.1363 0.0495 0.5309 0.066 Uiso 1 1 calc R . . C2 C 0.2750(11) -0.0073(3) 0.4652(10) 0.034(2) Uani 1 1 d . . . H2A H 0.1836 -0.0115 0.4438 0.051 Uiso 1 1 calc R . . H2B H 0.3011 -0.0177 0.5453 0.051 Uiso 1 1 calc R . . H2C H 0.3239 -0.0182 0.4037 0.051 Uiso 1 1 calc R . . C3 C 0.3733(9) 0.0483(2) 0.3937(8) 0.0192(19) Uani 1 1 d . . . C4 C 0.4377(10) 0.0267(3) 0.2990(9) 0.027(2) Uani 1 1 d . . . H4A H 0.4722 0.0042 0.3347 0.032 Uiso 1 1 calc R . . H4B H 0.3765 0.0213 0.2272 0.032 Uiso 1 1 calc R . . C5 C 0.6102(10) 0.0347(3) 0.1681(8) 0.027(2) Uani 1 1 d . . . H5A H 0.5501 0.0288 0.0961 0.033 Uiso 1 1 calc R . . H5B H 0.6561 0.0130 0.1968 0.033 Uiso 1 1 calc R . . C6 C 0.7052(10) 0.0632(2) 0.1354(8) 0.023(2) Uani 1 1 d . . . C7 C 0.7938(10) 0.0199(3) -0.0027(9) 0.033(2) Uani 1 1 d . . . H7A H 0.8642 0.0060 0.0382 0.049 Uiso 1 1 calc R . . H7B H 0.8076 0.0230 -0.0888 0.049 Uiso 1 1 calc R . . H7C H 0.7129 0.0074 0.0032 0.049 Uiso 1 1 calc R . . C8 C 0.8831(11) 0.0815(3) 0.0248(10) 0.039(3) Uani 1 1 d . . . H8A H 0.8586 0.1050 0.0518 0.058 Uiso 1 1 calc R . . H8B H 0.8860 0.0816 -0.0639 0.058 Uiso 1 1 calc R . . H8C H 0.9675 0.0753 0.0647 0.058 Uiso 1 1 calc R . . C9 C 0.2241(11) 0.0763(3) -0.0678(10) 0.039(3) Uani 1 1 d . . . H9A H 0.2592 0.0570 -0.1138 0.059 Uiso 1 1 calc R . . H9B H 0.1360 0.0811 -0.1014 0.059 Uiso 1 1 calc R . . H9C H 0.2250 0.0694 0.0181 0.059 Uiso 1 1 calc R . . C10 C 0.2826(10) 0.1285(3) -0.1952(9) 0.033(2) Uani 1 1 d . . . H10A H 0.2609 0.1531 -0.1781 0.050 Uiso 1 1 calc R . . H10B H 0.2129 0.1178 -0.2484 0.050 Uiso 1 1 calc R . . H10C H 0.3614 0.1279 -0.2360 0.050 Uiso 1 1 calc R . . C11 C 0.3835(10) 0.1197(3) 0.0183(9) 0.027(2) Uani 1 1 d . . . C12 C 0.4566(11) 0.1541(3) 0.0055(9) 0.032(2) Uani 1 1 d . . . H12A H 0.5025 0.1537 -0.0688 0.038 Uiso 1 1 calc R . . H12B H 0.3975 0.1745 0.0006 0.038 Uiso 1 1 calc R . . C13 C 0.6344(11) 0.1866(3) 0.1114(9) 0.032(3) Uani 1 1 d . . . H13A H 0.5867 0.2088 0.0918 0.039 Uiso 1 1 calc R . . H13B H 0.6960 0.1828 0.0502 0.039 Uiso 1 1 calc R . . C14 C 0.7014(10) 0.1880(2) 0.2374(9) 0.026(2) Uani 1 1 d . . . C15 C 0.8064(12) 0.2439(3) 0.1813(11) 0.039(3) Uani 1 1 d . . . H15A H 0.8842 0.2393 0.1415 0.059 Uiso 1 1 calc R . . H15B H 0.8157 0.2662 0.2263 0.059 Uiso 1 1 calc R . . H15C H 0.7331 0.2455 0.1192 0.059 Uiso 1 1 calc R . . C16 C 0.8491(12) 0.2169(3) 0.3943(10) 0.042(3) Uani 1 1 d . . . H16A H 0.7861 0.2131 0.4531 0.063 Uiso 1 1 calc R . . H16B H 0.8871 0.2404 0.4068 0.063 Uiso 1 1 calc R . . H16C H 0.9162 0.1989 0.4063 0.063 Uiso 1 1 calc R . . C17 C 0.1933(11) 0.2127(3) 0.2355(10) 0.035(3) Uani 1 1 d . . . H17A H 0.2380 0.2005 0.1737 0.052 Uiso 1 1 calc R . . H17B H 0.1840 0.2378 0.2143 0.052 Uiso 1 1 calc R . . H17C H 0.1086 0.2022 0.2388 0.052 Uiso 1 1 calc R . . C18 C 0.2460(11) 0.2357(3) 0.4504(10) 0.036(3) Uani 1 1 d . . . H18A H 0.1693 0.2294 0.4894 0.053 Uiso 1 1 calc R . . H18B H 0.2342 0.2590 0.4120 0.053 Uiso 1 1 calc R . . H18C H 0.3199 0.2364 0.5120 0.053 Uiso 1 1 calc R . . C19 C 0.3497(9) 0.1824(3) 0.3762(9) 0.024(2) Uani 1 1 d . . . C20 C 0.4303(10) 0.1798(2) 0.5020(8) 0.024(2) Uani 1 1 d . . . H20A H 0.4828 0.2013 0.5179 0.028 Uiso 1 1 calc R . . H20B H 0.3739 0.1770 0.5684 0.028 Uiso 1 1 calc R . . C21 C 0.6141(9) 0.1476(3) 0.5929(8) 0.025(2) Uani 1 1 d . . . H21A H 0.5795 0.1420 0.6712 0.029 Uiso 1 1 calc R . . H21B H 0.6584 0.1706 0.6011 0.029 Uiso 1 1 calc R . . C22 C 0.7074(9) 0.1186(2) 0.5610(8) 0.0210(19) Uani 1 1 d . . . C23 C 0.8486(12) 0.1381(3) 0.7399(10) 0.040(3) Uani 1 1 d . . . H23A H 0.8639 0.1622 0.7123 0.060 Uiso 1 1 calc R . . H23B H 0.9258 0.1291 0.7868 0.060 Uiso 1 1 calc R . . H23C H 0.7777 0.1382 0.7915 0.060 Uiso 1 1 calc R . . C24 C 0.9075(10) 0.0858(3) 0.6097(10) 0.035(2) Uani 1 1 d . . . H24A H 0.8873 0.0767 0.5268 0.052 Uiso 1 1 calc R . . H24B H 0.8996 0.0667 0.6687 0.052 Uiso 1 1 calc R . . H24C H 0.9951 0.0950 0.6186 0.052 Uiso 1 1 calc R . . C25 C 0.0876(13) 0.1355(3) 0.4157(12) 0.046(3) Uani 1 1 d . . . C26 C 0.0521(16) 0.1183(3) 0.2988(11) 0.069(5) Uani 1 1 d . . . H26A H 0.1051 0.0972 0.2919 0.104 Uiso 1 1 calc R . . H26B H 0.0654 0.1347 0.2322 0.104 Uiso 1 1 calc R . . H26C H -0.0381 0.1114 0.2936 0.104 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pu1 0.0290(2) 0.01662(19) 0.01365(18) -0.00042(15) 0.00253(13) -0.00371(17) N1 0.029(5) 0.022(4) 0.027(4) 0.003(3) 0.008(4) -0.005(4) N2 0.021(4) 0.026(4) 0.023(4) 0.001(3) 0.006(3) 0.002(3) N3 0.025(2) 0.025(2) 0.025(2) -0.0005(10) 0.0027(10) 0.0009(10) N4 0.045(6) 0.027(5) 0.030(5) 0.002(4) 0.012(4) -0.010(4) N5 0.029(5) 0.022(4) 0.026(4) 0.003(3) -0.002(4) 0.006(4) N6 0.0213(18) 0.0214(18) 0.0214(18) 0.0002(10) 0.0017(10) -0.0007(10) N7 0.020(5) 0.030(5) 0.030(5) 0.001(4) 0.005(4) 0.010(4) N8 0.049(6) 0.029(5) 0.027(5) -0.002(4) 0.017(4) 0.003(5) N9 0.037(6) 0.039(6) 0.050(6) -0.023(5) -0.010(5) 0.006(5) N10 0.039(6) 0.029(5) 0.026(5) 0.004(4) -0.002(4) 0.000(4) N11 0.079(9) 0.053(7) 0.046(6) 0.007(6) 0.000(6) -0.021(6) O1 0.031(4) 0.020(3) 0.022(3) 0.001(3) 0.004(3) -0.003(3) O2 0.026(4) 0.018(3) 0.018(3) -0.005(2) 0.009(3) -0.007(3) O3 0.0230(16) 0.0227(16) 0.0228(16) 0.0000(10) 0.0030(10) -0.0010(10) O4 0.0253(16) 0.0203(16) 0.0245(16) 0.0003(10) 0.0019(10) 0.0015(10) O5 0.053(5) 0.030(4) 0.019(3) 0.002(3) 0.000(3) -0.007(4) O6 0.042(4) 0.026(4) 0.017(3) 0.001(3) 0.004(3) -0.012(3) O7 0.038(4) 0.025(4) 0.020(3) -0.007(3) 0.000(3) 0.002(3) O8 0.021(3) 0.018(3) 0.020(3) -0.001(3) -0.002(3) 0.007(3) O9 0.0213(16) 0.0236(16) 0.0209(16) 0.0009(10) 0.0021(10) 0.0003(10) O11 0.045(5) 0.030(4) 0.043(4) 0.007(3) 0.015(4) -0.006(4) O12 0.048(5) 0.029(4) 0.040(4) -0.005(3) -0.004(4) -0.011(4) O13 0.104(8) 0.043(5) 0.028(5) -0.007(4) 0.017(5) -0.010(5) O14 0.064(6) 0.044(5) 0.043(5) 0.014(4) -0.004(4) -0.003(4) O15 0.183(14) 0.028(5) 0.054(6) -0.003(4) 0.041(7) -0.005(6) O16 0.069(7) 0.084(7) 0.041(5) -0.001(5) -0.008(5) -0.033(6) O17 0.060(7) 0.109(10) 0.130(11) -0.038(8) 0.040(8) -0.014(7) O18 0.166(14) 0.033(6) 0.135(11) 0.018(7) -0.060(10) 0.000(7) O19 0.083(8) 0.089(8) 0.069(7) -0.009(6) 0.002(6) 0.051(7) O20 0.039(5) 0.046(5) 0.053(5) -0.005(4) 0.013(4) -0.009(4) O21 0.085(7) 0.038(5) 0.044(5) 0.005(4) 0.002(5) -0.017(5) O22 0.075(7) 0.062(6) 0.056(6) 0.000(5) 0.030(5) 0.006(5) C1 0.045(7) 0.039(7) 0.054(7) 0.003(5) 0.041(6) 0.000(5) C2 0.039(7) 0.023(5) 0.041(6) 0.007(4) 0.005(5) -0.005(5) C3 0.014(5) 0.028(5) 0.015(4) 0.005(4) -0.001(4) -0.002(4) C4 0.032(6) 0.027(5) 0.024(5) -0.003(4) 0.013(4) -0.016(4) C5 0.039(6) 0.026(5) 0.019(5) -0.008(4) 0.013(4) -0.010(4) C6 0.031(6) 0.022(5) 0.016(5) 0.006(4) 0.001(4) 0.003(4) C7 0.033(6) 0.035(6) 0.030(6) -0.010(5) 0.006(5) 0.005(5) C8 0.032(6) 0.056(8) 0.029(6) -0.003(5) 0.012(5) -0.009(5) C9 0.027(6) 0.058(8) 0.033(6) -0.003(5) 0.002(5) -0.007(5) C10 0.023(6) 0.051(7) 0.024(5) 0.006(5) -0.005(4) 0.000(5) C11 0.028(5) 0.027(5) 0.024(5) -0.001(4) -0.002(4) 0.010(4) C12 0.047(7) 0.028(5) 0.020(5) 0.001(4) 0.002(5) 0.003(5) C13 0.049(7) 0.023(5) 0.026(5) -0.001(4) 0.014(5) -0.011(5) C14 0.032(6) 0.013(5) 0.036(6) -0.005(4) 0.017(5) -0.001(4) C15 0.047(7) 0.020(5) 0.053(7) 0.006(5) 0.017(6) -0.007(5) C16 0.043(7) 0.042(7) 0.040(7) -0.011(5) 0.000(5) -0.014(6) C17 0.029(6) 0.038(6) 0.036(6) 0.011(5) -0.006(5) -0.001(5) C18 0.033(6) 0.031(6) 0.042(6) -0.009(5) 0.001(5) 0.010(5) C19 0.018(5) 0.026(5) 0.027(5) 0.006(4) -0.002(4) -0.006(4) C20 0.033(6) 0.015(4) 0.022(5) 0.000(4) -0.002(4) 0.009(4) C21 0.027(5) 0.027(5) 0.019(5) 0.000(4) -0.004(4) 0.005(4) C22 0.022(5) 0.024(5) 0.017(4) 0.006(4) 0.002(4) 0.000(4) C23 0.043(7) 0.041(7) 0.032(6) -0.006(5) -0.012(5) 0.000(5) C24 0.023(6) 0.033(6) 0.046(6) 0.001(5) -0.006(5) 0.007(5) C25 0.045(8) 0.044(7) 0.048(8) 0.013(6) -0.001(6) -0.008(6) C26 0.109(14) 0.051(8) 0.044(8) 0.004(7) -0.009(8) -0.025(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 Pu1 O7 2.312(7) . ? Pu1 O9 2.313(6) . ? Pu1 O4 2.313(6) . ? Pu1 O6 2.314(6) . ? Pu1 O1 2.315(6) . ? Pu1 O3 2.320(6) . ? Pu1 O5 2.458(6) . ? Pu1 O8 2.499(6) . ? Pu1 O2 2.501(6) . ? N1 C3 1.322(11) . ? N1 C1 1.451(12) . ? N1 C2 1.459(12) . ? N2 C6 1.294(12) . ? N2 C8 1.441(13) . ? N2 C7 1.468(12) . ? N3 C11 1.335(12) . ? N3 C9 1.436(13) . ? N3 C10 1.477(12) . ? N4 C14 1.321(13) . ? N4 C16 1.454(14) . ? N4 C15 1.477(12) . ? N5 C19 1.304(12) . ? N5 C18 1.445(12) . ? N5 C17 1.457(12) . ? N6 C22 1.302(12) . ? N6 C23 1.447(12) . ? N6 C24 1.477(12) . ? N7 O12 1.225(10) . ? N7 O13 1.236(10) . ? N7 O11 1.266(10) . ? N8 O15 1.226(12) . ? N8 O14 1.230(11) . ? N8 O16 1.239(11) . ? N9 O18 1.201(14) . ? N9 O19 1.212(13) . ? N9 O17 1.276(14) . ? N10 O21 1.242(11) . ? N10 O22 1.243(12) . ? N10 O20 1.253(11) . ? N11 C25 1.142(15) . ? O1 C3 1.268(11) . ? O2 C5 1.428(10) . ? O2 C4 1.446(10) . ? O3 C6 1.263(11) . ? O4 C11 1.280(11) . ? O5 C12 1.417(12) . ? O5 C13 1.447(12) . ? O6 C14 1.274(11) . ? O7 C19 1.261(11) . ? O8 C21 1.423(10) . ? O8 C20 1.424(10) . ? O9 C22 1.252(11) . ? C3 C4 1.504(13) . ? C5 C6 1.505(13) . ? C11 C12 1.494(14) . ? C13 C14 1.464(14) . ? C19 C20 1.523(13) . ? C21 C22 1.503(13) . ? C25 C26 1.430(17) . ? 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 O7 Pu1 O9 126.0(2) . . ? O7 Pu1 O4 79.1(2) . . ? O9 Pu1 O4 150.1(2) . . ? O7 Pu1 O6 88.1(2) . . ? O9 Pu1 O6 74.7(2) . . ? O4 Pu1 O6 127.2(2) . . ? O7 Pu1 O1 81.9(2) . . ? O9 Pu1 O1 84.5(2) . . ? O4 Pu1 O1 83.6(2) . . ? O6 Pu1 O1 145.2(2) . . ? O7 Pu1 O3 145.7(2) . . ? O9 Pu1 O3 81.2(2) . . ? O4 Pu1 O3 83.7(2) . . ? O6 Pu1 O3 79.1(2) . . ? O1 Pu1 O3 125.3(2) . . ? O7 Pu1 O5 71.7(2) . . ? O9 Pu1 O5 134.0(2) . . ? O4 Pu1 O5 64.2(2) . . ? O6 Pu1 O5 63.1(2) . . ? O1 Pu1 O5 141.3(2) . . ? O3 Pu1 O5 74.2(2) . . ? O7 Pu1 O8 62.5(2) . . ? O9 Pu1 O8 63.4(2) . . ? O4 Pu1 O8 138.0(2) . . ? O6 Pu1 O8 70.7(2) . . ? O1 Pu1 O8 75.1(2) . . ? O3 Pu1 O8 138.1(2) . . ? O5 Pu1 O8 114.4(2) . . ? O7 Pu1 O2 134.9(2) . . ? O9 Pu1 O2 80.1(2) . . ? O4 Pu1 O2 70.1(2) . . ? O6 Pu1 O2 136.9(2) . . ? O1 Pu1 O2 63.0(2) . . ? O3 Pu1 O2 62.7(2) . . ? O5 Pu1 O2 119.2(2) . . ? O8 Pu1 O2 126.43(19) . . ? C3 N1 C1 120.1(8) . . ? C3 N1 C2 123.9(8) . . ? C1 N1 C2 115.7(8) . . ? C6 N2 C8 120.9(8) . . ? C6 N2 C7 123.0(8) . . ? C8 N2 C7 116.1(8) . . ? C11 N3 C9 121.5(8) . . ? C11 N3 C10 121.5(8) . . ? C9 N3 C10 116.9(8) . . ? C14 N4 C16 120.7(9) . . ? C14 N4 C15 121.4(9) . . ? C16 N4 C15 117.5(9) . . ? C19 N5 C18 123.3(8) . . ? C19 N5 C17 119.3(8) . . ? C18 N5 C17 117.4(8) . . ? C22 N6 C23 122.5(8) . . ? C22 N6 C24 119.8(8) . . ? C23 N6 C24 117.6(8) . . ? O12 N7 O13 120.3(9) . . ? O12 N7 O11 121.6(8) . . ? O13 N7 O11 118.0(9) . . ? O15 N8 O14 118.7(10) . . ? O15 N8 O16 122.2(10) . . ? O14 N8 O16 118.7(10) . . ? O18 N9 O19 123.0(14) . . ? O18 N9 O17 123.0(13) . . ? O19 N9 O17 114.0(13) . . ? O21 N10 O22 120.7(10) . . ? O21 N10 O20 118.3(10) . . ? O22 N10 O20 121.0(9) . . ? C3 O1 Pu1 128.6(6) . . ? C5 O2 C4 112.8(7) . . ? C5 O2 Pu1 120.2(5) . . ? C4 O2 Pu1 121.4(5) . . ? C6 O3 Pu1 127.5(6) . . ? C11 O4 Pu1 125.4(6) . . ? C12 O5 C13 112.9(7) . . ? C12 O5 Pu1 122.8(6) . . ? C13 O5 Pu1 124.0(6) . . ? C14 O6 Pu1 127.4(6) . . ? C19 O7 Pu1 130.0(6) . . ? C21 O8 C20 112.6(6) . . ? C21 O8 Pu1 119.9(5) . . ? C20 O8 Pu1 122.7(5) . . ? C22 O9 Pu1 127.3(6) . . ? O1 C3 N1 122.9(8) . . ? O1 C3 C4 118.3(8) . . ? N1 C3 C4 118.8(8) . . ? O2 C4 C3 104.1(7) . . ? O2 C5 C6 106.0(7) . . ? O3 C6 N2 123.1(9) . . ? O3 C6 C5 118.2(8) . . ? N2 C6 C5 118.8(8) . . ? O4 C11 N3 120.0(9) . . ? O4 C11 C12 120.7(9) . . ? N3 C11 C12 119.2(8) . . ? O5 C12 C11 105.4(8) . . ? O5 C13 C14 104.6(7) . . ? O6 C14 N4 119.4(9) . . ? O6 C14 C13 120.7(8) . . ? N4 C14 C13 119.9(9) . . ? O7 C19 N5 124.1(9) . . ? O7 C19 C20 117.3(8) . . ? N5 C19 C20 118.6(9) . . ? O8 C20 C19 105.9(7) . . ? O8 C21 C22 107.5(7) . . ? O9 C22 N6 124.0(9) . . ? O9 C22 C21 118.2(8) . . ? N6 C22 C21 117.6(8) . . ? N11 C25 C26 179.7(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.203 _refine_diff_density_min -4.890 _refine_diff_density_rms 0.202 # Attachment '- xpl201s EtOH solvate squeezed CCDC 891842.cif' data_xpl201s _database_code_depnum_ccdc_archive 'CCDC 891842' #TrackingRef '- xpl201s EtOH solvate squeezed CCDC 891842.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H54 N10 O22 Pu' _chemical_formula_weight 1097.77 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' Pu Pu -9.4100 4.3056 '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 21.121(5) _cell_length_b 12.830(3) _cell_length_c 19.842(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.811(3) _cell_angle_gamma 90.00 _cell_volume 5198(2) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 1.342 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8139 _exptl_absorpt_correction_T_max 0.8343 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 SMART 1k CCD' _diffrn_measurement_method '\f 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 23624 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4926 _reflns_number_gt 4193 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 4.210 (Bruker, 1996)' _computing_cell_refinement 'SAINT 4.05 (Bruker, 1996)' _computing_data_reduction 'SAINT 4.05 (Bruker, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker, 2001)' _computing_publication_material 'SHELXTL 6.10 (Bruker, 2001)' _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. ; # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.320 -0.250 0.070 735 360 ethanol 2 0.331 0.250 0.581 735 360 ethanol _platon_squeeze_details ; Two disordered independent ethanol solvent molecules ; _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^)+(0.1015P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4926 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1773 _refine_ls_wR_factor_gt 0.1735 _refine_ls_goodness_of_fit_ref 1.265 _refine_ls_restrained_S_all 1.265 _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 Pu1 Pu 0.0000 0.10322(3) 0.2500 0.0438(2) Uani 1 2 d S . . N1 N 0.0067(5) 0.3767(7) 0.1118(5) 0.074(3) Uani 1 1 d . . . N2 N 0.2074(4) 0.0526(8) 0.3719(4) 0.066(2) Uani 1 1 d . . . N3 N 0.0600(5) -0.1095(8) 0.0971(6) 0.086(3) Uani 1 1 d . . . N4 N 0.1144(8) 0.2829(16) 0.9829(8) 0.124(5) Uani 1 1 d . . . N5 N 0.2109(8) 0.8793(15) 0.2422(8) 0.118(6) Uani 1 1 d . . . O1 O -0.0155(3) 0.2374(5) 0.1692(3) 0.0557(15) Uani 1 1 d . . . O2 O 0.0992(3) 0.2026(5) 0.2397(3) 0.0567(15) Uani 1 1 d . . . O3 O 0.0983(3) 0.0564(5) 0.3242(3) 0.0576(15) Uani 1 1 d . . . O4 O 0.0347(3) 0.0230(5) 0.1631(4) 0.0612(16) Uani 1 1 d . . . O5 O 0.0000 -0.0867(6) 0.2500 0.074(3) Uani 1 2 d S . . O6 O 0.1041(10) 0.253(2) 0.9290(11) 0.269(15) Uani 1 1 d . . . O7 O 0.0894(8) 0.2360(15) 1.0243(9) 0.171(6) Uani 1 1 d . . . O8 O 0.1510(11) 0.352(2) 1.0003(10) 0.221(10) Uani 1 1 d . . . O9 O 0.2630(8) 0.8737(18) 0.2798(10) 0.210(10) Uani 1 1 d . . . O10 O 0.1828(13) 0.7933(19) 0.2343(12) 0.253(13) Uani 1 1 d . . . O11 O 0.1839(7) 0.9558(13) 0.2173(7) 0.141(5) Uani 1 1 d . . . C1 C 0.0249(5) 0.3010(7) 0.1566(5) 0.054(2) Uani 1 1 d . . . C2 C -0.0612(8) 0.3913(11) 0.0742(7) 0.094(4) Uani 1 1 d . . . H2A H -0.0847 0.3272 0.0740 0.141 Uiso 1 1 calc R . . H2B H -0.0635 0.4118 0.0271 0.141 Uiso 1 1 calc R . . H2C H -0.0804 0.4446 0.0966 0.141 Uiso 1 1 calc R . . C3 C 0.0545(9) 0.4558(14) 0.0999(9) 0.119(6) Uani 1 1 d . . . H3A H 0.0957 0.4465 0.1337 0.179 Uiso 1 1 calc R . . H3B H 0.0381 0.5245 0.1045 0.179 Uiso 1 1 calc R . . H3C H 0.0606 0.4474 0.0539 0.179 Uiso 1 1 calc R . . C4 C 0.0954(5) 0.2889(8) 0.1964(6) 0.068(3) Uani 1 1 d . . . H4A H 0.1228 0.2787 0.1645 0.082 Uiso 1 1 calc R . . H4B H 0.1103 0.3509 0.2240 0.082 Uiso 1 1 calc R . . C5 C 0.1614(4) 0.1836(9) 0.2852(6) 0.069(3) Uani 1 1 d . . . H5A H 0.1763 0.2445 0.3138 0.083 Uiso 1 1 calc R . . H5B H 0.1930 0.1682 0.2587 0.083 Uiso 1 1 calc R . . C6 C 0.1552(5) 0.0940(7) 0.3296(5) 0.052(2) Uani 1 1 d . . . C7 C 0.2733(6) 0.0910(11) 0.3780(8) 0.090(4) Uani 1 1 d . . . H7A H 0.2960 0.0442 0.3545 0.136 Uiso 1 1 calc R . . H7B H 0.2964 0.0954 0.4264 0.136 Uiso 1 1 calc R . . H7C H 0.2712 0.1589 0.3572 0.136 Uiso 1 1 calc R . . C8 C 0.1998(7) -0.0354(13) 0.4167(8) 0.110(5) Uani 1 1 d . . . H8A H 0.2110 -0.0134 0.4645 0.165 Uiso 1 1 calc R . . H8B H 0.2282 -0.0913 0.4109 0.165 Uiso 1 1 calc R . . H8C H 0.1552 -0.0591 0.4038 0.165 Uiso 1 1 calc R . . C9 C 0.0370(5) -0.0743(9) 0.1500(6) 0.067(3) Uani 1 1 d . . . C10 C 0.0648(9) -0.2212(12) 0.0849(9) 0.116(6) Uani 1 1 d . . . H10A H 0.0714 -0.2580 0.1283 0.174 Uiso 1 1 calc R . . H10B H 0.1010 -0.2342 0.0651 0.174 Uiso 1 1 calc R . . H10C H 0.0250 -0.2449 0.0532 0.174 Uiso 1 1 calc R . . C11 C 0.0833(7) -0.0356(16) 0.0528(7) 0.106(5) Uani 1 1 d . . . H11A H 0.0781 0.0342 0.0680 0.159 Uiso 1 1 calc R . . H11B H 0.0584 -0.0439 0.0054 0.159 Uiso 1 1 calc R . . H11C H 0.1287 -0.0484 0.0560 0.159 Uiso 1 1 calc R . . C12 C 0.0182(7) -0.1476(9) 0.1972(7) 0.080(3) Uani 1 1 d . . . H12A H -0.0183 -0.1900 0.1724 0.096 Uiso 1 1 calc R . . H12B H 0.0546 -0.1931 0.2181 0.096 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pu1 0.0320(2) 0.0249(2) 0.0753(4) 0.000 0.01486(19) 0.000 N1 0.088(7) 0.059(6) 0.077(6) 0.027(4) 0.027(5) -0.001(5) N2 0.036(4) 0.083(6) 0.072(5) 0.003(5) -0.001(4) 0.020(4) N3 0.065(6) 0.085(8) 0.107(8) -0.049(6) 0.022(6) 0.003(5) N4 0.117(11) 0.173(16) 0.092(9) -0.032(10) 0.046(8) -0.034(10) N5 0.092(10) 0.131(13) 0.111(10) -0.044(9) -0.013(8) 0.050(9) O1 0.044(3) 0.040(3) 0.083(4) 0.013(3) 0.014(3) 0.002(3) O2 0.042(3) 0.052(4) 0.073(4) 0.011(3) 0.010(3) -0.002(3) O3 0.042(3) 0.053(4) 0.081(4) 0.004(3) 0.021(3) 0.003(3) O4 0.055(4) 0.043(4) 0.087(5) -0.003(3) 0.020(3) -0.002(3) O5 0.058(6) 0.021(4) 0.144(10) 0.000 0.030(6) 0.000 O6 0.21(2) 0.44(4) 0.185(16) -0.12(2) 0.103(15) -0.12(2) O7 0.156(13) 0.173(15) 0.193(14) 0.036(12) 0.063(11) -0.016(11) O8 0.21(2) 0.27(2) 0.188(16) -0.083(16) 0.056(13) -0.141(19) O9 0.110(11) 0.29(2) 0.201(15) -0.076(15) -0.017(11) 0.099(13) O10 0.29(3) 0.17(2) 0.227(19) -0.026(16) -0.078(18) 0.027(18) O11 0.125(10) 0.148(13) 0.138(10) -0.001(9) 0.010(8) 0.053(10) C1 0.057(5) 0.041(5) 0.066(6) 0.002(4) 0.022(4) -0.001(4) C2 0.097(10) 0.099(11) 0.077(8) 0.015(7) 0.006(7) 0.039(8) C3 0.126(13) 0.111(13) 0.123(12) 0.055(10) 0.034(10) -0.032(10) C4 0.057(6) 0.061(6) 0.091(7) 0.017(5) 0.027(5) -0.003(5) C5 0.038(5) 0.068(7) 0.097(7) 0.005(6) 0.011(5) -0.010(5) C6 0.046(5) 0.051(5) 0.058(5) -0.011(4) 0.012(4) 0.010(4) C7 0.047(6) 0.112(12) 0.101(9) -0.013(7) -0.003(6) 0.007(6) C8 0.104(11) 0.109(12) 0.107(10) 0.025(9) 0.008(8) 0.041(9) C9 0.047(5) 0.061(6) 0.084(7) -0.016(5) 0.001(5) 0.001(5) C10 0.136(13) 0.087(11) 0.136(12) -0.059(9) 0.054(11) 0.004(9) C11 0.087(9) 0.142(16) 0.093(9) -0.021(10) 0.033(8) 0.014(10) C12 0.091(9) 0.046(6) 0.104(9) -0.017(6) 0.027(7) 0.016(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 Pu1 O4 2.284(7) . ? Pu1 O4 2.284(7) 2 ? Pu1 O3 2.297(6) . ? Pu1 O3 2.297(6) 2 ? Pu1 O1 2.317(6) . ? Pu1 O1 2.317(6) 2 ? Pu1 O5 2.437(8) . ? Pu1 O2 2.504(6) . ? Pu1 O2 2.504(6) 2 ? N1 C1 1.306(12) . ? N1 C2 1.450(19) . ? N1 C3 1.494(17) . ? N2 C6 1.314(12) . ? N2 C7 1.453(15) . ? N2 C8 1.471(18) . ? N3 C9 1.344(16) . ? N3 C11 1.46(2) . ? N3 C10 1.462(16) . ? N4 O6 1.101(18) . ? N4 O8 1.17(2) . ? N4 O7 1.240(19) . ? N5 O9 1.163(19) . ? N5 O11 1.18(2) . ? N5 O10 1.24(3) . ? O1 C1 1.253(11) . ? O2 C4 1.391(11) . ? O2 C5 1.414(11) . ? O3 C6 1.273(11) . ? O4 C9 1.278(13) . ? O5 C12 1.435(12) . ? O5 C12 1.435(12) 2 ? C1 C4 1.505(14) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.474(14) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C12 1.451(19) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? 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 O4 Pu1 O4 126.4(3) . 2 ? O4 Pu1 O3 87.4(2) . . ? O4 Pu1 O3 79.1(2) 2 . ? O4 Pu1 O3 79.1(2) . 2 ? O4 Pu1 O3 87.4(2) 2 2 ? O3 Pu1 O3 149.7(3) . 2 ? O4 Pu1 O1 80.1(2) . . ? O4 Pu1 O1 147.3(2) 2 . ? O3 Pu1 O1 125.6(2) . . ? O3 Pu1 O1 78.8(2) 2 . ? O4 Pu1 O1 147.3(2) . 2 ? O4 Pu1 O1 80.1(2) 2 2 ? O3 Pu1 O1 78.8(2) . 2 ? O3 Pu1 O1 125.6(2) 2 2 ? O1 Pu1 O1 84.1(3) . 2 ? O4 Pu1 O5 63.21(17) . . ? O4 Pu1 O5 63.21(17) 2 . ? O3 Pu1 O5 74.84(17) . . ? O3 Pu1 O5 74.85(17) 2 . ? O1 Pu1 O5 137.96(16) . . ? O1 Pu1 O5 137.96(16) 2 . ? O4 Pu1 O2 74.4(2) . . ? O4 Pu1 O2 136.7(2) 2 . ? O3 Pu1 O2 63.1(2) . . ? O3 Pu1 O2 135.9(2) 2 . ? O1 Pu1 O2 62.5(2) . . ? O1 Pu1 O2 72.9(2) 2 . ? O5 Pu1 O2 120.59(15) . . ? O4 Pu1 O2 136.7(2) . 2 ? O4 Pu1 O2 74.4(2) 2 2 ? O3 Pu1 O2 135.9(2) . 2 ? O3 Pu1 O2 63.1(2) 2 2 ? O1 Pu1 O2 72.9(2) . 2 ? O1 Pu1 O2 62.5(2) 2 2 ? O5 Pu1 O2 120.59(15) . 2 ? O2 Pu1 O2 118.8(3) . 2 ? C1 N1 C2 121.8(10) . . ? C1 N1 C3 121.2(11) . . ? C2 N1 C3 116.8(11) . . ? C6 N2 C7 123.1(10) . . ? C6 N2 C8 119.5(10) . . ? C7 N2 C8 117.4(9) . . ? C9 N3 C11 119.8(11) . . ? C9 N3 C10 120.9(13) . . ? C11 N3 C10 119.3(11) . . ? O6 N4 O8 120(2) . . ? O6 N4 O7 118(2) . . ? O8 N4 O7 122.2(19) . . ? O9 N5 O11 127(2) . . ? O9 N5 O10 112(2) . . ? O11 N5 O10 121.5(19) . . ? C1 O1 Pu1 129.7(6) . . ? C4 O2 C5 115.4(7) . . ? C4 O2 Pu1 122.6(5) . . ? C5 O2 Pu1 121.4(5) . . ? C6 O3 Pu1 129.4(6) . . ? C9 O4 Pu1 129.0(7) . . ? C12 O5 C12 114.1(12) . 2 ? C12 O5 Pu1 123.0(6) . . ? C12 O5 Pu1 123.0(6) 2 . ? O1 C1 N1 121.5(9) . . ? O1 C1 C4 117.5(8) . . ? N1 C1 C4 121.0(9) . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O2 C4 C1 107.3(8) . . ? O2 C4 H4A 110.2 . . ? C1 C4 H4A 110.2 . . ? O2 C4 H4B 110.2 . . ? C1 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? O2 C5 C6 107.9(7) . . ? O2 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? O2 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? O3 C6 N2 121.4(9) . . ? O3 C6 C5 118.0(8) . . ? N2 C6 C5 120.5(9) . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4 C9 N3 121.8(12) . . ? O4 C9 C12 118.1(10) . . ? N3 C9 C12 120.0(11) . . ? N3 C10 H10A 109.5 . . ? N3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O5 C12 C9 106.6(9) . . ? O5 C12 H12A 110.4 . . ? C9 C12 H12A 110.4 . . ? O5 C12 H12B 110.4 . . ? C9 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.284 _refine_diff_density_min -4.637 _refine_diff_density_rms 0.182