Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_xl _database_code_CSD 174541 _journal_coden_Cambridge 186 loop_ _publ_author_name 'J.H. Matonic' 'M.P. Neu' 'R.T. Paine' 'B.L. Scott' _publ_contact_author_name 'Prof R T Paine' _publ_contact_author_address ; Clark 103 Department of Chemistry University of New Mexico Albuquerque NM 87131 USA ; _publ_contact_author_phone '505 277 1661' _publ_contact_author_fax '505 277 2609' _publ_contact_author_email 'rtpaine@unm.edu' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and Crystal Structure of a Ten Coordinate Plutonium (IV) Ion Complexed by 2- [(Diphenylphosphino)methyl]pyridine N,P - Dioxide: [Pu)NO3)3{2-[C6H5)xP(O)CH2]C5H4No}2][Oy(NO3)6}0.5- ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H32 N8 O22 P2 Pu1.50' _chemical_formula_weight 1353.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0407(6) _cell_length_b 14.2228(7) _cell_length_c 15.6363(7) _cell_angle_alpha 65.1950(10) _cell_angle_beta 80.5710(10) _cell_angle_gamma 72.3810(10) _cell_volume 2314.58(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 23.28 _exptl_crystal_description yellow _exptl_crystal_colour needle _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1302 _exptl_absorpt_coefficient_mu 2.283 _exptl_absorpt_correction_type 'empirical (SADABS, Sheldrick 1996)' _exptl_absorpt_correction_T_min 0.565 _exptl_absorpt_correction_T_max 0.726 _exptl_absorpt_process_details ? _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 graphite _diffrn_measurement_device_type 'Bruker P4/PC ccd' _diffrn_measurement_method '/w and /f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '<2' _diffrn_reflns_number 11151 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 23.28 _reflns_number_total 6115 _reflns_number_gt 5439 _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, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 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^)+(0.0267P)^2^+4.7376P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6115 _refine_ls_number_parameters 628 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0632 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.428432(16) -0.109187(15) -0.167022(14) 0.03408(8) Uani 1 1 d . . . P1 P 0.70549(12) -0.04722(11) -0.18238(10) 0.0378(3) Uani 1 1 d . . . P2 P 0.30355(12) -0.33393(11) -0.10787(10) 0.0356(3) Uani 1 1 d . . . O1 O 0.4202(3) 0.0421(3) -0.1399(3) 0.0474(10) Uani 1 1 d . . . O2 O 0.6170(3) -0.0919(3) -0.1999(3) 0.0433(9) Uani 1 1 d . . . O3 O 0.5345(3) -0.2386(3) -0.2262(3) 0.0431(9) Uani 1 1 d . . . O4 O 0.3080(3) -0.2211(3) -0.1334(3) 0.0393(9) Uani 1 1 d . . . O5 O 0.5119(4) -0.1539(4) -0.0084(3) 0.0620(12) Uani 1 1 d . . . O6 O 0.5189(4) -0.2861(3) -0.0413(3) 0.0518(10) Uani 1 1 d . . . O7 O 0.5864(4) -0.3157(4) 0.0914(3) 0.0722(13) Uani 1 1 d . . . O8 O 0.2254(4) 0.0016(3) -0.1898(3) 0.0578(11) Uani 1 1 d . . . O9 O 0.2750(4) -0.0836(4) -0.0456(3) 0.0576(11) Uani 1 1 d . . . O10 O 0.0942(4) 0.0029(5) -0.0774(5) 0.099(2) Uani 1 1 d . . . O11 O 0.4340(4) 0.0339(4) -0.3235(3) 0.0617(12) Uani 1 1 d . . . O12 O 0.3445(4) -0.0779(3) -0.3160(3) 0.0579(11) Uani 1 1 d . . . O13 O 0.3647(6) 0.0504(5) -0.4507(4) 0.106(2) Uani 1 1 d . . . N1 N 0.4439(4) 0.1340(4) -0.2001(3) 0.0434(11) Uani 1 1 d . . . N2 N 0.5092(4) -0.2764(4) -0.2837(3) 0.0421(11) Uani 1 1 d . . . N3 N 0.5404(4) -0.2546(4) 0.0174(4) 0.0479(12) Uani 1 1 d . . . N4 N 0.1945(5) -0.0247(5) -0.1033(5) 0.0580(15) Uani 1 1 d . . . N5 N 0.3797(5) 0.0054(4) -0.3675(4) 0.0596(14) Uani 1 1 d . . . C1 C 0.3588(5) 0.2119(5) -0.2541(5) 0.0610(18) Uani 1 1 d . . . H1A H 0.2851 0.2011 -0.2485 0.073 Uiso 1 1 calc R . . C2 C 0.3794(6) 0.3062(5) -0.3168(5) 0.0662(19) Uani 1 1 d . . . H2A H 0.3205 0.3598 -0.3544 0.079 Uiso 1 1 calc R . . C3 C 0.4887(6) 0.3214(5) -0.3240(5) 0.0599(18) Uani 1 1 d . . . H3A H 0.5045 0.3853 -0.3671 0.072 Uiso 1 1 calc R . . C4 C 0.5742(5) 0.2416(5) -0.2671(4) 0.0516(16) Uani 1 1 d . . . H4A H 0.6483 0.2515 -0.2721 0.062 Uiso 1 1 calc R . . C5 C 0.5514(5) 0.1466(4) -0.2025(4) 0.0400(13) Uani 1 1 d . . . C6 C 0.6378(5) 0.0559(4) -0.1371(4) 0.0426(14) Uani 1 1 d . . . H6A H 0.5989 0.0249 -0.0765 0.051 Uiso 1 1 calc R . . H6B H 0.6976 0.0830 -0.1275 0.051 Uiso 1 1 calc R . . C7 C 0.5363(6) -0.2301(5) -0.3767(4) 0.0571(17) Uani 1 1 d . . . H7A H 0.5711 -0.1736 -0.3989 0.069 Uiso 1 1 calc R . . C8 C 0.5125(7) -0.2662(7) -0.4379(5) 0.075(2) Uani 1 1 d . . . H8A H 0.5313 -0.2345 -0.5019 0.090 Uiso 1 1 calc R . . C9 C 0.4609(7) -0.3495(7) -0.4052(5) 0.083(2) Uani 1 1 d . . . H9A H 0.4417 -0.3729 -0.4468 0.099 Uiso 1 1 calc R . . C10 C 0.4381(6) -0.3973(6) -0.3105(5) 0.0618(18) Uani 1 1 d . . . H10A H 0.4051 -0.4550 -0.2879 0.074 Uiso 1 1 calc R . . C11 C 0.4626(5) -0.3624(5) -0.2473(4) 0.0436(14) Uani 1 1 d . . . C12 C 0.4383(5) -0.4104(4) -0.1440(4) 0.0399(13) Uani 1 1 d . . . H12A H 0.5022 -0.4136 -0.1115 0.048 Uiso 1 1 calc R . . H12B H 0.4334 -0.4832 -0.1259 0.048 Uiso 1 1 calc R . . C20 C 0.8073(5) -0.1492(4) -0.0998(4) 0.0407(13) Uani 1 1 d . . . C21 C 0.8771(5) -0.1274(5) -0.0509(5) 0.0593(17) Uani 1 1 d . . . H21A H 0.8691 -0.0571 -0.0589 0.071 Uiso 1 1 calc R . . C22 C 0.9579(6) -0.2105(6) 0.0093(5) 0.070(2) Uani 1 1 d . . . H22A H 1.0044 -0.1959 0.0417 0.084 Uiso 1 1 calc R . . C23 C 0.9703(5) -0.3147(6) 0.0219(5) 0.0631(19) Uani 1 1 d . . . H23A H 1.0244 -0.3703 0.0633 0.076 Uiso 1 1 calc R . . C24 C 0.9040(5) -0.3361(5) -0.0259(5) 0.0626(19) Uani 1 1 d . . . H24A H 0.9130 -0.4066 -0.0177 0.075 Uiso 1 1 calc R . . C25 C 0.8226(5) -0.2538(5) -0.0870(5) 0.0558(16) Uani 1 1 d . . . H25A H 0.7778 -0.2696 -0.1198 0.067 Uiso 1 1 calc R . . C30 C 0.7809(5) 0.0156(5) -0.2910(4) 0.0477(15) Uani 1 1 d . . . C31 C 0.8709(7) 0.0583(6) -0.2918(5) 0.077(2) Uani 1 1 d . . . H31A H 0.8945 0.0517 -0.2354 0.093 Uiso 1 1 calc R . . C32 C 0.9255(9) 0.1104(8) -0.3760(8) 0.108(3) Uani 1 1 d . . . H32A H 0.9838 0.1413 -0.3768 0.130 Uiso 1 1 calc R . . C33 C 0.8932(10) 0.1161(9) -0.4573(8) 0.122(4) Uani 1 1 d . . . H33A H 0.9314 0.1497 -0.5138 0.146 Uiso 1 1 calc R . . C34 C 0.8071(9) 0.0744(9) -0.4583(6) 0.116(4) Uani 1 1 d . . . H34A H 0.7854 0.0804 -0.5152 0.139 Uiso 1 1 calc R . . C35 C 0.7503(7) 0.0219(7) -0.3736(5) 0.079(2) Uani 1 1 d . . . H35A H 0.6919 -0.0083 -0.3738 0.094 Uiso 1 1 calc R . . C40 C 0.1905(5) -0.3336(5) -0.1698(4) 0.0455(14) Uani 1 1 d . . . C41 C 0.1192(5) -0.2347(6) -0.2227(4) 0.0558(16) Uani 1 1 d . . . H41A H 0.1290 -0.1719 -0.2235 0.067 Uiso 1 1 calc R . . C42 C 0.0333(6) -0.2304(7) -0.2745(5) 0.077(2) Uani 1 1 d . . . H42A H -0.0149 -0.1649 -0.3109 0.093 Uiso 1 1 calc R . . C43 C 0.0204(7) -0.3263(9) -0.2710(6) 0.085(3) Uani 1 1 d . . . H43A H -0.0381 -0.3236 -0.3048 0.102 Uiso 1 1 calc R . . C44 C 0.0915(7) -0.4249(8) -0.2192(6) 0.083(3) Uani 1 1 d . . . H44A H 0.0821 -0.4879 -0.2183 0.100 Uiso 1 1 calc R . . C45 C 0.1770(6) -0.4274(6) -0.1688(5) 0.0632(19) Uani 1 1 d . . . H45A H 0.2262 -0.4930 -0.1336 0.076 Uiso 1 1 calc R . . C50 C 0.2818(4) -0.3996(4) 0.0171(4) 0.0379(13) Uani 1 1 d . . . C51 C 0.2691(5) -0.3404(5) 0.0720(4) 0.0532(16) Uani 1 1 d . . . H51A H 0.2730 -0.2694 0.0434 0.064 Uiso 1 1 calc R . . C52 C 0.2508(6) -0.3872(6) 0.1687(5) 0.0624(18) Uani 1 1 d . . . H52A H 0.2428 -0.3478 0.2051 0.075 Uiso 1 1 calc R . . C53 C 0.2445(5) -0.4922(6) 0.2111(5) 0.0588(17) Uani 1 1 d . . . H53A H 0.2329 -0.5239 0.2761 0.071 Uiso 1 1 calc R . . C54 C 0.2552(5) -0.5497(5) 0.1579(4) 0.0529(16) Uani 1 1 d . . . H54A H 0.2499 -0.6203 0.1870 0.064 Uiso 1 1 calc R . . C55 C 0.2739(5) -0.5046(5) 0.0614(4) 0.0460(14) Uani 1 1 d . . . H55A H 0.2812 -0.5449 0.0259 0.055 Uiso 1 1 calc R . . Pu2 Pu 0.0000 0.5000 0.5000 0.03984(9) Uani 1 2 d S . . O14 O 0.1799(4) 0.5135(4) 0.5484(3) 0.0679(13) Uani 1 1 d . . . O15 O 0.1462(4) 0.6041(4) 0.4027(3) 0.0744(14) Uani 1 1 d . . . O16 O 0.3079(5) 0.5901(6) 0.4588(5) 0.122(2) Uani 1 1 d . . . O17 O 0.0078(4) 0.5327(4) 0.3320(3) 0.0657(13) Uani 1 1 d . . . O18 O -0.0915(4) 0.6654(4) 0.3675(3) 0.0677(13) Uani 1 1 d . . . O19 O -0.0780(6) 0.6815(6) 0.2226(4) 0.127(3) Uani 1 1 d . . . O20 O 0.1822(4) 0.3883(4) 0.4529(3) 0.0670(13) Uani 1 1 d . . . O21 O 0.0292(4) 0.3326(4) 0.4753(3) 0.0686(13) Uani 1 1 d . . . O22 O 0.1917(5) 0.2456(5) 0.4289(5) 0.102(2) Uani 1 1 d . . . N6 N 0.2155(5) 0.5700(5) 0.4696(5) 0.0706(17) Uani 1 1 d . . . N7 N -0.0541(5) 0.6294(5) 0.3042(4) 0.0694(17) Uani 1 1 d . . . N8 N 0.1371(5) 0.3175(5) 0.4521(4) 0.0649(15) 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 0.03587(12) 0.02898(12) 0.03921(13) -0.01462(9) 0.00398(8) -0.01214(8) P1 0.0368(7) 0.0348(8) 0.0448(9) -0.0180(7) 0.0011(6) -0.0115(6) P2 0.0372(7) 0.0352(8) 0.0380(8) -0.0151(7) 0.0019(6) -0.0150(6) O1 0.045(2) 0.035(2) 0.064(3) -0.022(2) 0.0089(19) -0.0160(18) O2 0.037(2) 0.047(2) 0.057(3) -0.031(2) 0.0027(17) -0.0128(17) O3 0.046(2) 0.045(2) 0.048(2) -0.028(2) 0.0054(18) -0.0157(18) O4 0.042(2) 0.033(2) 0.045(2) -0.0164(17) 0.0046(16) -0.0152(16) O5 0.091(3) 0.045(3) 0.055(3) -0.029(2) 0.000(2) -0.013(2) O6 0.066(3) 0.046(2) 0.052(3) -0.026(2) -0.010(2) -0.014(2) O7 0.096(4) 0.061(3) 0.051(3) -0.018(3) -0.017(3) -0.008(3) O8 0.048(2) 0.052(3) 0.075(3) -0.030(2) 0.008(2) -0.014(2) O9 0.066(3) 0.058(3) 0.062(3) -0.035(2) 0.020(2) -0.030(2) O10 0.048(3) 0.124(5) 0.152(6) -0.092(5) 0.038(3) -0.027(3) O11 0.065(3) 0.057(3) 0.058(3) -0.010(2) -0.008(2) -0.024(2) O12 0.064(3) 0.053(3) 0.054(3) -0.015(2) -0.003(2) -0.019(2) O13 0.138(5) 0.110(5) 0.048(3) 0.012(3) -0.030(3) -0.052(4) N1 0.042(3) 0.029(3) 0.060(3) -0.021(2) 0.005(2) -0.009(2) N2 0.045(3) 0.042(3) 0.045(3) -0.024(2) 0.007(2) -0.014(2) N3 0.054(3) 0.044(3) 0.044(3) -0.018(3) 0.004(2) -0.013(2) N4 0.047(3) 0.057(4) 0.089(5) -0.046(4) 0.019(3) -0.025(3) N5 0.059(3) 0.056(4) 0.051(4) -0.008(3) -0.002(3) -0.017(3) C1 0.045(3) 0.046(4) 0.092(5) -0.025(4) -0.005(3) -0.012(3) C2 0.060(4) 0.040(4) 0.078(5) -0.011(4) -0.012(4) 0.001(3) C3 0.070(4) 0.038(4) 0.063(4) -0.015(3) 0.009(4) -0.016(3) C4 0.051(4) 0.048(4) 0.062(4) -0.027(3) 0.010(3) -0.020(3) C5 0.040(3) 0.036(3) 0.055(4) -0.027(3) 0.006(3) -0.015(3) C6 0.043(3) 0.040(3) 0.054(4) -0.027(3) -0.002(3) -0.012(3) C7 0.064(4) 0.062(4) 0.050(4) -0.027(3) 0.016(3) -0.024(3) C8 0.097(6) 0.088(6) 0.050(4) -0.033(4) 0.012(4) -0.037(5) C9 0.110(6) 0.109(7) 0.062(5) -0.057(5) 0.018(4) -0.051(6) C10 0.073(4) 0.071(5) 0.063(5) -0.043(4) 0.014(4) -0.035(4) C11 0.046(3) 0.040(3) 0.048(4) -0.024(3) 0.009(3) -0.012(3) C12 0.043(3) 0.031(3) 0.047(4) -0.017(3) 0.003(3) -0.012(2) C20 0.038(3) 0.037(3) 0.047(3) -0.017(3) 0.002(3) -0.010(2) C21 0.059(4) 0.051(4) 0.067(5) -0.021(4) -0.016(3) -0.009(3) C22 0.063(4) 0.079(6) 0.063(5) -0.021(4) -0.016(4) -0.016(4) C23 0.047(4) 0.057(5) 0.056(4) -0.001(4) -0.004(3) -0.003(3) C24 0.048(4) 0.042(4) 0.080(5) -0.010(4) -0.002(4) -0.009(3) C25 0.049(3) 0.048(4) 0.069(4) -0.020(3) -0.002(3) -0.015(3) C30 0.048(3) 0.038(3) 0.051(4) -0.015(3) 0.006(3) -0.011(3) C31 0.093(6) 0.081(6) 0.069(5) -0.026(4) 0.019(4) -0.055(5) C32 0.119(8) 0.118(8) 0.102(8) -0.039(7) 0.045(6) -0.081(7) C33 0.126(9) 0.139(10) 0.078(7) -0.023(7) 0.044(6) -0.058(8) C34 0.115(8) 0.165(11) 0.056(6) -0.025(6) 0.010(5) -0.053(8) C35 0.076(5) 0.105(7) 0.051(5) -0.024(4) 0.004(4) -0.032(5) C40 0.049(3) 0.051(4) 0.039(3) -0.018(3) -0.001(3) -0.017(3) C41 0.053(4) 0.065(4) 0.047(4) -0.023(3) 0.001(3) -0.012(3) C42 0.058(4) 0.111(7) 0.054(5) -0.028(5) -0.014(4) -0.012(4) C43 0.071(5) 0.145(9) 0.064(5) -0.052(6) -0.005(4) -0.045(6) C44 0.094(6) 0.115(7) 0.074(5) -0.047(5) -0.008(5) -0.057(6) C45 0.071(4) 0.062(4) 0.067(5) -0.022(4) -0.007(4) -0.035(4) C50 0.032(3) 0.041(3) 0.039(3) -0.012(3) 0.001(2) -0.014(2) C51 0.070(4) 0.052(4) 0.047(4) -0.024(3) 0.009(3) -0.028(3) C52 0.080(5) 0.071(5) 0.047(4) -0.027(4) 0.008(3) -0.037(4) C53 0.057(4) 0.065(5) 0.041(4) -0.009(3) 0.008(3) -0.020(3) C54 0.049(4) 0.045(4) 0.046(4) -0.002(3) 0.005(3) -0.013(3) C55 0.044(3) 0.041(3) 0.051(4) -0.015(3) -0.001(3) -0.012(3) Pu2 0.03443(16) 0.05023(19) 0.03228(17) -0.01048(14) -0.00040(12) -0.01640(13) O14 0.059(3) 0.082(3) 0.059(3) -0.016(3) -0.012(2) -0.025(3) O15 0.073(3) 0.079(4) 0.059(3) -0.008(3) 0.003(3) -0.034(3) O16 0.071(4) 0.171(7) 0.147(6) -0.058(5) 0.014(4) -0.081(4) O17 0.065(3) 0.083(4) 0.044(3) -0.022(3) -0.003(2) -0.016(3) O18 0.070(3) 0.074(3) 0.048(3) -0.017(3) -0.002(2) -0.014(3) O19 0.144(6) 0.138(6) 0.036(3) -0.012(3) -0.013(3) 0.025(5) O20 0.053(3) 0.081(3) 0.061(3) -0.025(3) 0.002(2) -0.016(3) O21 0.069(3) 0.071(3) 0.067(3) -0.026(3) 0.000(2) -0.022(3) O22 0.086(4) 0.091(4) 0.140(6) -0.077(4) -0.021(4) 0.016(3) N6 0.051(3) 0.091(5) 0.072(4) -0.023(4) 0.001(3) -0.038(3) N7 0.070(4) 0.079(5) 0.036(4) -0.016(3) -0.006(3) 0.002(3) N8 0.054(4) 0.070(4) 0.074(4) -0.034(3) -0.006(3) -0.011(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 Pu1 O2 2.309(3) . ? Pu1 O4 2.315(3) . ? Pu1 O1 2.334(4) . ? Pu1 O3 2.344(4) . ? Pu1 O11 2.446(4) . ? Pu1 O8 2.463(4) . ? Pu1 O9 2.484(4) . ? Pu1 O12 2.505(4) . ? Pu1 O6 2.505(4) . ? Pu1 O5 2.582(4) . ? Pu1 N4 2.899(5) . ? Pu1 N5 2.927(6) . ? P1 O2 1.505(4) . ? P1 C20 1.773(6) . ? P1 C30 1.795(6) . ? P1 C6 1.809(6) . ? P2 O4 1.498(4) . ? P2 C50 1.791(5) . ? P2 C40 1.793(6) . ? P2 C12 1.811(5) . ? O1 N1 1.334(6) . ? O3 N2 1.336(5) . ? O5 N3 1.263(6) . ? O6 N3 1.267(6) . ? O7 N3 1.214(6) . ? O8 N4 1.266(7) . ? O9 N4 1.271(7) . ? O10 N4 1.210(7) . ? O11 N5 1.268(7) . ? O12 N5 1.275(6) . ? O13 N5 1.201(7) . ? N1 C1 1.342(8) . ? N1 C5 1.351(6) . ? N2 C7 1.352(7) . ? N2 C11 1.365(7) . ? C1 C2 1.357(9) . ? C2 C3 1.376(9) . ? C3 C4 1.374(9) . ? C4 C5 1.382(8) . ? C5 C6 1.490(8) . ? C7 C8 1.360(9) . ? C8 C9 1.372(10) . ? C9 C10 1.365(10) . ? C10 C11 1.380(8) . ? C11 C12 1.484(8) . ? C20 C25 1.373(8) . ? C20 C21 1.398(8) . ? C21 C22 1.378(9) . ? C22 C23 1.374(10) . ? C23 C24 1.350(9) . ? C24 C25 1.384(9) . ? C30 C35 1.360(9) . ? C30 C31 1.389(9) . ? C31 C32 1.382(11) . ? C32 C33 1.352(13) . ? C33 C34 1.347(13) . ? C34 C35 1.401(11) . ? C40 C45 1.386(8) . ? C40 C41 1.387(9) . ? C41 C42 1.388(9) . ? C42 C43 1.397(12) . ? C43 C44 1.380(12) . ? C44 C45 1.379(9) . ? C50 C55 1.385(8) . ? C50 C51 1.397(8) . ? C51 C52 1.383(8) . ? C52 C53 1.378(9) . ? C53 C54 1.358(9) . ? C54 C55 1.380(8) . ? Pu2 O17 2.460(4) . ? Pu2 O17 2.460(4) 2_566 ? Pu2 O18 2.476(5) 2_566 ? Pu2 O18 2.476(5) . ? Pu2 O21 2.482(5) . ? Pu2 O21 2.482(5) 2_566 ? Pu2 O14 2.492(4) 2_566 ? Pu2 O14 2.492(4) . ? Pu2 O20 2.495(5) . ? Pu2 O20 2.495(5) 2_566 ? Pu2 O15 2.533(4) . ? Pu2 O15 2.533(4) 2_566 ? O14 N6 1.245(7) . ? O15 N6 1.282(7) . ? O16 N6 1.200(7) . ? O17 N7 1.272(7) . ? O18 N7 1.259(7) . ? O19 N7 1.207(7) . ? O20 N8 1.286(7) . ? O21 N8 1.269(7) . ? O22 N8 1.198(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Pu1 O4 146.19(13) . . ? O2 Pu1 O1 76.01(13) . . ? O4 Pu1 O1 135.82(13) . . ? O2 Pu1 O3 72.76(12) . . ? O4 Pu1 O3 75.85(12) . . ? O1 Pu1 O3 148.29(12) . . ? O2 Pu1 O11 72.43(14) . . ? O4 Pu1 O11 120.55(14) . . ? O1 Pu1 O11 74.62(15) . . ? O3 Pu1 O11 90.70(15) . . ? O2 Pu1 O8 140.42(14) . . ? O4 Pu1 O8 71.65(13) . . ? O1 Pu1 O8 73.45(13) . . ? O3 Pu1 O8 130.65(14) . . ? O11 Pu1 O8 75.62(15) . . ? O2 Pu1 O9 134.05(14) . . ? O4 Pu1 O9 69.35(13) . . ? O1 Pu1 O9 67.92(13) . . ? O3 Pu1 O9 141.33(13) . . ? O11 Pu1 O9 121.22(16) . . ? O8 Pu1 O9 51.51(16) . . ? O2 Pu1 O12 108.93(13) . . ? O4 Pu1 O12 70.39(13) . . ? O1 Pu1 O12 117.07(14) . . ? O3 Pu1 O12 69.32(14) . . ? O11 Pu1 O12 50.99(14) . . ? O8 Pu1 O12 65.33(15) . . ? O9 Pu1 O12 112.34(15) . . ? O2 Pu1 O6 84.23(13) . . ? O4 Pu1 O6 71.92(13) . . ? O1 Pu1 O6 115.69(13) . . ? O3 Pu1 O6 66.63(13) . . ? O11 Pu1 O6 151.64(15) . . ? O8 Pu1 O6 131.91(14) . . ? O9 Pu1 O6 86.58(15) . . ? O12 Pu1 O6 127.23(13) . . ? O2 Pu1 O5 73.24(14) . . ? O4 Pu1 O5 105.97(14) . . ? O1 Pu1 O5 66.40(14) . . ? O3 Pu1 O5 108.77(14) . . ? O11 Pu1 O5 132.83(14) . . ? O8 Pu1 O5 115.22(15) . . ? O9 Pu1 O5 66.86(16) . . ? O12 Pu1 O5 176.12(13) . . ? O6 Pu1 O5 49.30(13) . . ? O2 Pu1 N4 145.94(13) . . ? O4 Pu1 N4 66.79(13) . . ? O1 Pu1 N4 69.95(13) . . ? O3 Pu1 N4 141.22(13) . . ? O11 Pu1 N4 99.21(17) . . ? O8 Pu1 N4 25.71(16) . . ? O9 Pu1 N4 25.87(15) . . ? O12 Pu1 N4 88.15(17) . . ? O6 Pu1 N4 109.13(16) . . ? O5 Pu1 N4 91.62(17) . . ? O2 Pu1 N5 90.31(14) . . ? O4 Pu1 N5 95.73(14) . . ? O1 Pu1 N5 96.10(15) . . ? O3 Pu1 N5 78.83(15) . . ? O11 Pu1 N5 25.32(14) . . ? O8 Pu1 N5 68.78(16) . . ? O9 Pu1 N5 120.26(16) . . ? O12 Pu1 N5 25.67(14) . . ? O6 Pu1 N5 145.12(15) . . ? O5 Pu1 N5 158.13(15) . . ? N4 Pu1 N5 94.48(18) . . ? O2 P1 C20 111.2(2) . . ? O2 P1 C30 110.1(3) . . ? C20 P1 C30 109.7(3) . . ? O2 P1 C6 111.9(2) . . ? C20 P1 C6 107.7(3) . . ? C30 P1 C6 106.0(3) . . ? O4 P2 C50 110.2(2) . . ? O4 P2 C40 109.8(3) . . ? C50 P2 C40 111.3(2) . . ? O4 P2 C12 111.0(2) . . ? C50 P2 C12 108.2(3) . . ? C40 P2 C12 106.2(3) . . ? N1 O1 Pu1 128.7(3) . . ? P1 O2 Pu1 145.2(2) . . ? N2 O3 Pu1 133.5(3) . . ? P2 O4 Pu1 145.3(2) . . ? N3 O5 Pu1 96.5(3) . . ? N3 O6 Pu1 100.1(3) . . ? N4 O8 Pu1 96.7(4) . . ? N4 O9 Pu1 95.6(3) . . ? N5 O11 Pu1 99.1(3) . . ? N5 O12 Pu1 96.0(4) . . ? O1 N1 C1 118.6(5) . . ? O1 N1 C5 119.0(4) . . ? C1 N1 C5 122.4(5) . . ? O3 N2 C7 117.9(4) . . ? O3 N2 C11 119.9(4) . . ? C7 N2 C11 122.1(5) . . ? O7 N3 O5 122.9(5) . . ? O7 N3 O6 123.0(5) . . ? O5 N3 O6 114.1(5) . . ? O7 N3 Pu1 178.3(4) . . ? O5 N3 Pu1 58.8(3) . . ? O6 N3 Pu1 55.3(3) . . ? O10 N4 O8 121.9(7) . . ? O10 N4 O9 122.3(7) . . ? O8 N4 O9 115.8(5) . . ? O10 N4 Pu1 174.0(4) . . ? O8 N4 Pu1 57.5(3) . . ? O9 N4 Pu1 58.5(3) . . ? O13 N5 O11 123.8(6) . . ? O13 N5 O12 122.3(6) . . ? O11 N5 O12 113.9(5) . . ? O13 N5 Pu1 177.1(5) . . ? O11 N5 Pu1 55.6(3) . . ? O12 N5 Pu1 58.3(3) . . ? N1 C1 C2 120.5(6) . . ? C1 C2 C3 119.2(6) . . ? C4 C3 C2 119.5(6) . . ? C3 C4 C5 120.7(6) . . ? N1 C5 C4 117.7(5) . . ? N1 C5 C6 117.7(5) . . ? C4 C5 C6 124.6(5) . . ? C5 C6 P1 111.9(4) . . ? N2 C7 C8 120.0(6) . . ? C7 C8 C9 120.0(7) . . ? C10 C9 C8 118.9(7) . . ? C9 C10 C11 121.9(6) . . ? N2 C11 C10 117.1(5) . . ? N2 C11 C12 118.8(5) . . ? C10 C11 C12 124.1(5) . . ? C11 C12 P2 111.9(4) . . ? C25 C20 C21 118.5(5) . . ? C25 C20 P1 118.5(4) . . ? C21 C20 P1 123.0(5) . . ? C22 C21 C20 119.8(6) . . ? C23 C22 C21 120.6(7) . . ? C24 C23 C22 119.9(6) . . ? C23 C24 C25 120.5(6) . . ? C20 C25 C24 120.8(6) . . ? C35 C30 C31 119.3(6) . . ? C35 C30 P1 120.1(5) . . ? C31 C30 P1 120.5(5) . . ? C32 C31 C30 120.3(8) . . ? C33 C32 C31 119.3(9) . . ? C34 C33 C32 121.5(9) . . ? C33 C34 C35 119.9(9) . . ? C30 C35 C34 119.6(8) . . ? C45 C40 C41 120.7(6) . . ? C45 C40 P2 121.9(5) . . ? C41 C40 P2 117.3(5) . . ? C40 C41 C42 119.3(7) . . ? C41 C42 C43 118.8(8) . . ? C44 C43 C42 122.3(7) . . ? C45 C44 C43 118.0(8) . . ? C44 C45 C40 120.9(7) . . ? C55 C50 C51 118.7(5) . . ? C55 C50 P2 123.3(5) . . ? C51 C50 P2 118.0(4) . . ? C52 C51 C50 120.1(6) . . ? C53 C52 C51 120.0(6) . . ? C54 C53 C52 120.1(6) . . ? C53 C54 C55 120.8(6) . . ? C54 C55 C50 120.3(6) . . ? O17 Pu2 O17 180.000(1) . 2_566 ? O17 Pu2 O18 128.52(16) . 2_566 ? O17 Pu2 O18 51.48(16) 2_566 2_566 ? O17 Pu2 O18 51.48(16) . . ? O17 Pu2 O18 128.52(16) 2_566 . ? O18 Pu2 O18 180.0(2) 2_566 . ? O17 Pu2 O21 67.72(16) . . ? O17 Pu2 O21 112.28(16) 2_566 . ? O18 Pu2 O21 65.96(16) 2_566 . ? O18 Pu2 O21 114.04(16) . . ? O17 Pu2 O21 112.28(16) . 2_566 ? O17 Pu2 O21 67.72(16) 2_566 2_566 ? O18 Pu2 O21 114.04(16) 2_566 2_566 ? O18 Pu2 O21 65.96(16) . 2_566 ? O21 Pu2 O21 180.0(2) . 2_566 ? O17 Pu2 O14 67.26(15) . 2_566 ? O17 Pu2 O14 112.74(15) 2_566 2_566 ? O18 Pu2 O14 112.04(16) 2_566 2_566 ? O18 Pu2 O14 67.96(16) . 2_566 ? O21 Pu2 O14 67.10(16) . 2_566 ? O21 Pu2 O14 112.90(16) 2_566 2_566 ? O17 Pu2 O14 112.75(15) . . ? O17 Pu2 O14 67.25(15) 2_566 . ? O18 Pu2 O14 67.96(16) 2_566 . ? O18 Pu2 O14 112.04(16) . . ? O21 Pu2 O14 112.90(16) . . ? O21 Pu2 O14 67.10(16) 2_566 . ? O14 Pu2 O14 180.0(3) 2_566 . ? O17 Pu2 O20 67.82(16) . . ? O17 Pu2 O20 112.18(16) 2_566 . ? O18 Pu2 O20 66.18(16) 2_566 . ? O18 Pu2 O20 113.82(16) . . ? O21 Pu2 O20 50.96(16) . . ? O21 Pu2 O20 129.04(16) 2_566 . ? O14 Pu2 O20 112.95(16) 2_566 . ? O14 Pu2 O20 67.05(16) . . ? O17 Pu2 O20 112.18(16) . 2_566 ? O17 Pu2 O20 67.82(16) 2_566 2_566 ? O18 Pu2 O20 113.82(16) 2_566 2_566 ? O18 Pu2 O20 66.18(16) . 2_566 ? O21 Pu2 O20 129.04(16) . 2_566 ? O21 Pu2 O20 50.96(16) 2_566 2_566 ? O14 Pu2 O20 67.05(16) 2_566 2_566 ? O14 Pu2 O20 112.95(16) . 2_566 ? O20 Pu2 O20 180.000(1) . 2_566 ? O17 Pu2 O15 67.03(16) . . ? O17 Pu2 O15 112.97(16) 2_566 . ? O18 Pu2 O15 111.95(16) 2_566 . ? O18 Pu2 O15 68.05(16) . . ? O21 Pu2 O15 111.92(17) . . ? O21 Pu2 O15 68.08(17) 2_566 . ? O14 Pu2 O15 129.85(16) 2_566 . ? O14 Pu2 O15 50.15(16) . . ? O20 Pu2 O15 66.05(17) . . ? O20 Pu2 O15 113.95(17) 2_566 . ? O17 Pu2 O15 112.97(16) . 2_566 ? O17 Pu2 O15 67.03(16) 2_566 2_566 ? O18 Pu2 O15 68.05(16) 2_566 2_566 ? O18 Pu2 O15 111.95(16) . 2_566 ? O21 Pu2 O15 68.08(17) . 2_566 ? O21 Pu2 O15 111.92(17) 2_566 2_566 ? O14 Pu2 O15 50.15(16) 2_566 2_566 ? O14 Pu2 O15 129.85(16) . 2_566 ? O20 Pu2 O15 113.95(17) . 2_566 ? O20 Pu2 O15 66.05(17) 2_566 2_566 ? O15 Pu2 O15 180.0 . 2_566 ? N6 O14 Pu2 98.8(4) . . ? N6 O15 Pu2 95.8(4) . . ? N7 O17 Pu2 96.6(4) . . ? N7 O18 Pu2 96.2(4) . . ? N8 O20 Pu2 97.0(4) . . ? N8 O21 Pu2 98.2(4) . . ? O16 N6 O14 121.6(6) . . ? O16 N6 O15 123.5(7) . . ? O14 N6 O15 114.9(5) . . ? O16 N6 Pu2 174.8(6) . . ? O14 N6 Pu2 56.5(3) . . ? O15 N6 Pu2 58.6(3) . . ? O19 N7 O18 122.6(7) . . ? O19 N7 O17 121.7(7) . . ? O18 N7 O17 115.7(5) . . ? O19 N7 Pu2 178.4(6) . . ? O18 N7 Pu2 58.2(3) . . ? O17 N7 Pu2 57.5(3) . . ? O22 N8 O21 123.3(6) . . ? O22 N8 O20 122.8(6) . . ? O21 N8 O20 113.9(6) . . ? O22 N8 Pu2 177.4(5) . . ? O21 N8 Pu2 56.6(4) . . ? O20 N8 Pu2 57.3(3) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.877 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.085