Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Kwang-Hwa Lii' _publ_contact_author_address ; Department of Chemistry National Central University Chungli 320 TAIWAN ; _publ_contact_author_email liikh@cc.ncu.edu.tw _publ_section_title ; Organically Templated Uranium(IV) Fluorooxalates with Layer Structures: (H4TREN)[U2F6(C2O4)3],4H2O (TREN = tris(2-aminoethyl)amine) and (H4APPIP)[U2F6(C2O4)3],4H2O (APPIP = 1,4-bis(3-amino-propyl)piperazine) ; loop_ _publ_author_name 'Chih-Min Wang.' 'Yi-Ying Wu.' 'Pei-Lin Chen.' 'Kwang-Hwa Lii.' data_ufox-1 _database_code_depnum_ccdc_archive 'CCDC 629037' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety (C6H22N3)[U2F6(C2O4)3],4H2O _chemical_formula_sum 'C12 H30 F6 N4 O16 U2' _chemical_formula_weight 1076.46 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 19.1563(5) _cell_length_b 8.9531(2) _cell_length_c 16.6221(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.6330(10) _cell_angle_gamma 90.00 _cell_volume 2591.39(11) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.091 _exptl_crystal_size_mid 0.065 _exptl_crystal_size_min 0.052 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 12.605 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.592 _exptl_absorpt_correction_T_max 0.953 _exptl_absorpt_process_details 'SADABS program' _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 CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24082 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5932 _reflns_number_gt 4208 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _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^)+(0.0162P)^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 SHELXL _refine_ls_extinction_coef 0.000185(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5932 _refine_ls_number_parameters 365 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0532 _refine_ls_wR_factor_gt 0.0514 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.002 _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 U1 U 0.127811(15) 0.47478(3) 0.354695(14) 0.01720(7) Uani 1 1 d . . . U2 U 0.388277(15) 0.91309(3) 0.618978(14) 0.01667(7) Uani 1 1 d . . . F1 F 0.2020(2) 0.4736(4) 0.2856(2) 0.0271(9) Uani 1 1 d . . . F2 F 0.1793(2) 0.2510(4) 0.3864(2) 0.0294(10) Uani 1 1 d . . . F3 F 0.1236(2) 0.4727(4) 0.4830(2) 0.0358(11) Uani 1 1 d . . . F4 F 0.4227(2) 0.9155(4) 0.5092(2) 0.0270(9) Uani 1 1 d . . . F5 F 0.2860(2) 0.9134(4) 0.6488(2) 0.0252(9) Uani 1 1 d . . . F6 F 0.3434(2) 1.1338(4) 0.5686(2) 0.0284(9) Uani 1 1 d . . . O1 O -0.0163(3) 0.1296(5) 0.1538(3) 0.0400(14) Uani 1 1 d . . . O2 O -0.0641(3) 0.1327(5) 0.2814(3) 0.0300(12) Uani 1 1 d . . . O3 O 0.0646(3) 0.3157(5) 0.2193(3) 0.0370(14) Uani 1 1 d . . . O4 O 0.0191(3) 0.3142(6) 0.3489(3) 0.0448(15) Uani 1 1 d . . . O5 O 0.1770(3) 0.7350(5) 0.3839(3) 0.0289(12) Uani 1 1 d . . . O6 O 0.2597(3) 0.5032(5) 0.4762(3) 0.0283(12) Uani 1 1 d . . . O7 O 0.2658(3) 0.8907(5) 0.4753(3) 0.0264(11) Uani 1 1 d . . . O8 O 0.3449(3) 0.6596(5) 0.5683(3) 0.0270(11) Uani 1 1 d . . . O9 O 0.5073(3) 1.0702(5) 0.6595(3) 0.0268(11) Uani 1 1 d . . . O10 O 0.4223(3) 1.0708(5) 0.7525(2) 0.0228(11) Uani 1 1 d . . . O11 O 0.5832(3) 1.2453(5) 0.7501(2) 0.0224(11) Uani 1 1 d . . . O12 O 0.4975(3) 1.2495(5) 0.8400(2) 0.0243(11) Uani 1 1 d . . . C1 C 0.0145(4) 0.2227(7) 0.2131(4) 0.0224(16) Uani 1 1 d . . . C2 C -0.0135(4) 0.2229(8) 0.2871(4) 0.0243(16) Uani 1 1 d . . . C3 C 0.2383(4) 0.7650(7) 0.4495(4) 0.0209(16) Uani 1 1 d . . . C4 C 0.2847(4) 0.6293(7) 0.5019(4) 0.0202(16) Uani 1 1 d . . . C5 C 0.5267(4) 1.1579(7) 0.7230(4) 0.0176(15) Uani 1 1 d . . . C6 C 0.4772(4) 1.1587(7) 0.7758(4) 0.0194(16) Uani 1 1 d . . . C7 C 0.2456(4) 0.2593(7) 0.6815(4) 0.0301(18) Uani 1 1 d . . . H7A H 0.2678 0.3288 0.6539 0.036 Uiso 1 1 calc R . . H7B H 0.2799 0.1743 0.7022 0.036 Uiso 1 1 calc R . . C8 C 0.1702(4) 0.2076(8) 0.6144(4) 0.0323(19) Uani 1 1 d . . . H8A H 0.1473 0.1391 0.6416 0.039 Uiso 1 1 calc R . . H8B H 0.1361 0.2924 0.5918 0.039 Uiso 1 1 calc R . . C9 C 0.3183(4) 0.3651(8) 0.8338(4) 0.0375(19) Uani 1 1 d . . . H9A H 0.3535 0.3946 0.8083 0.045 Uiso 1 1 calc R . . H9B H 0.3142 0.4476 0.8695 0.045 Uiso 1 1 calc R . . C10 C 0.3501(4) 0.2320(8) 0.8918(4) 0.037(2) Uani 1 1 d . . . H10A H 0.3171 0.2042 0.9205 0.044 Uiso 1 1 calc R . . H10B H 0.3539 0.1478 0.8571 0.044 Uiso 1 1 calc R . . C11 C 0.1908(4) 0.4752(7) 0.7339(4) 0.0304(18) Uani 1 1 d . . . H11A H 0.1869 0.5164 0.7859 0.036 Uiso 1 1 calc R . . H11B H 0.1394 0.4495 0.6914 0.036 Uiso 1 1 calc R . . C12 C 0.2248(5) 0.5941(7) 0.6934(4) 0.0355(19) Uani 1 1 d . . . H12A H 0.2803 0.5866 0.7205 0.043 Uiso 1 1 calc R . . H12B H 0.2072 0.5751 0.6305 0.043 Uiso 1 1 calc R . . N1 N 0.2400(3) 0.3345(6) 0.7599(3) 0.0279(14) Uani 1 1 d . . . HN1 H 0.2158 0.2687 0.7817 0.050 Uiso 1 1 d . . . N2 N 0.1798(4) 0.1318(6) 0.5403(3) 0.0365(16) Uani 1 1 d . . . HN2A H 0.1321 0.0638 0.4954 0.050 Uiso 1 1 d . . . HN2B H 0.2112 0.0525 0.5612 0.050 Uiso 1 1 d . . . HN2C H 0.2008 0.1942 0.5149 0.050 Uiso 1 1 d . . . N3 N 0.4274(4) 0.2742(7) 0.9589(3) 0.0377(16) Uani 1 1 d . . . HN3A H 0.4483 0.1962 0.9947 0.050 Uiso 1 1 d . . . HN3B H 0.4232 0.3503 0.9908 0.050 Uiso 1 1 d . . . HN3C H 0.4572 0.2995 0.9321 0.050 Uiso 1 1 d . . . N4 N 0.2027(4) 0.7419(6) 0.7061(4) 0.0394(17) Uani 1 1 d . . . HN4A H 0.2236 0.8082 0.6823 0.050 Uiso 1 1 d . . . HN4B H 0.2198 0.7606 0.7640 0.050 Uiso 1 1 d . . . HN4C H 0.1522 0.7500 0.6806 0.050 Uiso 1 1 d . . . OW1 O 0.0605(4) 0.6955(7) 0.5462(3) 0.072(2) Uani 1 1 d . . . HO1A H 0.0968 0.7353 0.5231 0.050 Uiso 1 1 d . . . HO1B H 0.0481 0.7859 0.5711 0.050 Uiso 1 1 d . . . OW2 O 0.3519(4) 0.7196(7) 0.3722(3) 0.078(2) Uani 1 1 d . . . HO2A H 0.3388 0.6786 0.3137 0.050 Uiso 1 1 d . . . HO2B H 0.3155 0.6723 0.3917 0.050 Uiso 1 1 d . . . OW3 O 0.0514(5) -0.0354(8) 0.4545(4) 0.110(3) Uani 1 1 d . . . OW4 O 0.4068(11) 0.3921(19) 0.6509(8) 0.052(4) Uani 0.50 1 d P . . OW4' O 0.4222(11) 0.3882(19) 0.6142(8) 0.052(4) Uani 0.50 1 d P . . 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 U1 0.01695(16) 0.01582(14) 0.01740(11) -0.00112(10) 0.00574(11) 0.00030(12) U2 0.01625(16) 0.01569(14) 0.01654(11) -0.00031(9) 0.00531(11) -0.00054(12) F1 0.023(3) 0.030(2) 0.0307(19) -0.0014(16) 0.0138(19) -0.0010(19) F2 0.028(3) 0.017(2) 0.040(2) 0.0032(16) 0.011(2) 0.0036(18) F3 0.043(3) 0.043(3) 0.0226(18) 0.0037(17) 0.015(2) 0.005(2) F4 0.029(3) 0.033(2) 0.0215(17) -0.0041(16) 0.0129(18) -0.005(2) F5 0.023(2) 0.022(2) 0.0334(19) 0.0020(16) 0.0144(19) 0.0009(19) F6 0.026(3) 0.018(2) 0.031(2) 0.0026(16) 0.0010(19) 0.0021(18) O1 0.047(4) 0.049(4) 0.033(3) -0.024(2) 0.026(3) -0.031(3) O2 0.029(3) 0.038(3) 0.028(2) -0.011(2) 0.016(2) -0.018(3) O3 0.041(4) 0.046(3) 0.029(2) -0.012(2) 0.019(3) -0.028(3) O4 0.048(4) 0.055(4) 0.046(3) -0.033(3) 0.034(3) -0.034(3) O5 0.021(3) 0.018(3) 0.032(3) -0.001(2) -0.005(2) -0.002(2) O6 0.026(3) 0.010(3) 0.033(2) -0.004(2) -0.002(2) 0.000(2) O7 0.026(3) 0.018(3) 0.025(2) 0.000(2) 0.001(2) -0.002(2) O8 0.022(3) 0.021(3) 0.024(2) -0.0030(19) -0.005(2) -0.001(2) O9 0.027(3) 0.030(3) 0.026(2) -0.012(2) 0.014(2) -0.009(2) O10 0.021(3) 0.025(3) 0.024(2) -0.0060(19) 0.011(2) -0.008(2) O11 0.019(3) 0.029(3) 0.021(2) -0.0057(19) 0.010(2) -0.008(2) O12 0.023(3) 0.030(3) 0.021(2) -0.009(2) 0.009(2) -0.004(2) C1 0.020(5) 0.025(4) 0.020(3) -0.002(3) 0.006(3) -0.001(3) C2 0.016(4) 0.025(4) 0.030(4) -0.003(3) 0.007(3) 0.000(3) C3 0.018(4) 0.022(4) 0.021(3) -0.002(3) 0.006(3) 0.001(3) C4 0.018(4) 0.020(4) 0.021(3) -0.004(3) 0.007(3) 0.003(3) C5 0.015(4) 0.019(4) 0.020(3) 0.004(3) 0.008(3) 0.004(3) C6 0.020(4) 0.018(4) 0.017(3) 0.007(3) 0.005(3) 0.004(3) C7 0.035(5) 0.018(4) 0.043(4) 0.002(3) 0.022(4) 0.004(4) C8 0.037(5) 0.030(5) 0.032(4) 0.002(3) 0.016(4) 0.001(4) C9 0.035(6) 0.028(5) 0.041(4) 0.002(3) 0.008(4) -0.004(4) C10 0.024(5) 0.050(6) 0.037(4) 0.002(4) 0.014(4) -0.003(4) C11 0.031(5) 0.024(4) 0.045(4) -0.002(3) 0.025(4) -0.006(4) C12 0.042(6) 0.027(4) 0.050(4) 0.004(3) 0.032(4) 0.006(4) N1 0.027(4) 0.019(3) 0.043(3) 0.010(3) 0.020(3) 0.003(3) N2 0.039(5) 0.042(4) 0.030(3) 0.008(3) 0.015(3) 0.009(3) N3 0.028(4) 0.050(4) 0.037(3) -0.007(3) 0.015(3) 0.000(3) N4 0.046(5) 0.030(4) 0.056(4) 0.009(3) 0.035(4) 0.010(3) OW1 0.091(6) 0.082(5) 0.067(4) -0.020(3) 0.055(4) 0.000(4) OW2 0.086(6) 0.118(6) 0.057(4) -0.032(3) 0.055(4) -0.044(4) OW3 0.105(7) 0.098(6) 0.097(5) -0.029(4) 0.013(5) -0.040(5) OW4 0.051(8) 0.036(4) 0.034(8) 0.007(6) -0.016(6) -0.009(5) OW4' 0.051(8) 0.036(4) 0.034(8) 0.007(6) -0.016(6) -0.009(5) _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 U1 F1 2.167(3) . ? U1 F3 2.168(3) . ? U1 F2 2.198(3) . ? U1 O5 2.484(4) . ? U1 O4 2.500(5) . ? U1 O1 2.501(5) 2 ? U1 O6 2.505(4) . ? U1 O3 2.508(4) . ? U1 O2 2.511(4) 2 ? U2 F6 2.179(3) . ? U2 F4 2.184(3) . ? U2 F5 2.212(3) . ? U2 O8 2.443(4) . ? U2 O10 2.477(4) . ? U2 O12 2.480(4) 2_646 ? U2 O11 2.510(4) 2_646 ? U2 O9 2.520(4) . ? U2 O7 2.565(4) . ? O1 C1 1.237(7) . ? O1 U1 2.501(5) 2_545 ? O2 C2 1.235(7) . ? O2 U1 2.511(4) 2_545 ? O3 C1 1.242(7) . ? O4 C2 1.256(7) . ? O5 C3 1.254(7) . ? O6 C4 1.231(7) . ? O7 C3 1.240(7) . ? O8 C4 1.250(7) . ? O9 C5 1.241(7) . ? O10 C6 1.239(7) . ? O11 C5 1.257(7) . ? O11 U2 2.510(4) 2_656 ? O12 C6 1.266(7) . ? O12 U2 2.480(4) 2_656 ? C1 C2 1.532(8) . ? C3 C4 1.543(9) . ? C5 C6 1.539(8) . ? C7 C8 1.484(9) . ? C7 N1 1.510(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N2 1.483(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.494(9) . ? C9 N1 1.516(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N3 1.484(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N1 1.524(8) . ? C11 C12 1.542(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N4 1.431(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? N1 HN1 0.9120 . ? N2 HN2A 1.0932 . ? N2 HN2B 0.9002 . ? N2 HN2C 0.8902 . ? N3 HN3A 0.8950 . ? N3 HN3B 0.8873 . ? N3 HN3C 0.8877 . ? N4 HN4A 0.8943 . ? N4 HN4B 0.8941 . ? N4 HN4C 0.8838 . ? OW1 HO1A 0.9892 . ? OW1 HO1B 0.9828 . ? OW2 HO2A 0.9697 . ? OW2 HO2B 0.9798 . ? OW4 OW4' 0.780(18) . ? 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 F1 U1 F3 145.36(14) . . ? F1 U1 F2 78.18(13) . . ? F3 U1 F2 87.31(13) . . ? F1 U1 O5 80.15(14) . . ? F3 U1 O5 88.98(14) . . ? F2 U1 O5 135.41(15) . . ? F1 U1 O4 134.16(13) . . ? F3 U1 O4 70.17(14) . . ? F2 U1 O4 76.61(16) . . ? O5 U1 O4 142.11(15) . . ? F1 U1 O1 134.91(13) . 2 ? F3 U1 O1 71.27(14) . 2 ? F2 U1 O1 143.71(14) . 2 ? O5 U1 O1 74.74(16) . 2 ? O4 U1 O1 68.78(17) . 2 ? F1 U1 O6 76.34(14) . . ? F3 U1 O6 69.30(15) . . ? F2 U1 O6 72.43(14) . . ? O5 U1 O6 64.78(14) . . ? O4 U1 O6 129.34(16) . . ? O1 U1 O6 122.70(15) 2 . ? F1 U1 O3 72.53(14) . . ? F3 U1 O3 132.53(14) . . ? F2 U1 O3 72.44(15) . . ? O5 U1 O3 135.25(13) . . ? O4 U1 O3 63.62(13) . . ? O1 U1 O3 100.51(17) 2 . ? O6 U1 O3 136.79(15) . . ? F1 U1 O2 72.85(13) . 2 ? F3 U1 O2 133.45(14) . 2 ? F2 U1 O2 136.92(13) . 2 ? O5 U1 O2 69.54(14) . 2 ? O4 U1 O2 101.82(17) . 2 ? O1 U1 O2 63.52(13) 2 2 ? O6 U1 O2 128.12(15) . 2 ? O3 U1 O2 68.88(15) . 2 ? F6 U2 F4 83.00(13) . . ? F6 U2 F5 80.83(13) . . ? F4 U2 F5 142.31(13) . . ? F6 U2 O8 133.40(14) . . ? F4 U2 O8 84.18(13) . . ? F5 U2 O8 82.69(14) . . ? F6 U2 O10 75.03(13) . . ? F4 U2 O10 133.21(13) . . ? F5 U2 O10 74.07(13) . . ? O8 U2 O10 139.74(13) . . ? F6 U2 O12 143.42(14) . 2_646 ? F4 U2 O12 72.34(12) . 2_646 ? F5 U2 O12 134.51(12) . 2_646 ? O8 U2 O12 71.36(15) . 2_646 ? O10 U2 O12 102.57(14) . 2_646 ? F6 U2 O11 141.69(12) . 2_646 ? F4 U2 O11 134.26(13) . 2_646 ? F5 U2 O11 72.51(13) . 2_646 ? O8 U2 O11 70.30(13) . 2_646 ? O10 U2 O11 71.55(13) . 2_646 ? O12 U2 O11 63.88(12) 2_646 2_646 ? F6 U2 O9 76.38(14) . . ? F4 U2 O9 70.30(12) . . ? F5 U2 O9 136.61(12) . . ? O8 U2 O9 138.63(14) . . ? O10 U2 O9 64.64(13) . . ? O12 U2 O9 70.13(14) 2_646 . ? O11 U2 O9 104.88(14) 2_646 . ? F6 U2 O7 69.59(13) . . ? F4 U2 O7 72.57(13) . . ? F5 U2 O7 69.92(13) . . ? O8 U2 O7 63.82(14) . . ? O10 U2 O7 132.49(14) . . ? O12 U2 O7 124.74(13) 2_646 . ? O11 U2 O7 123.01(14) 2_646 . ? O9 U2 O7 131.83(13) . . ? C1 O1 U1 122.0(4) . 2_545 ? C2 O2 U1 120.6(4) . 2_545 ? C1 O3 U1 121.5(4) . . ? C2 O4 U1 121.8(4) . . ? C3 O5 U1 120.9(4) . . ? C4 O6 U1 119.3(4) . . ? C3 O7 U2 118.9(4) . . ? C4 O8 U2 124.2(4) . . ? C5 O9 U2 119.8(4) . . ? C6 O10 U2 121.0(3) . . ? C5 O11 U2 121.8(3) . 2_656 ? C6 O12 U2 122.5(4) . 2_656 ? O1 C1 O3 127.8(6) . . ? O1 C1 C2 115.5(6) . . ? O3 C1 C2 116.7(5) . . ? O2 C2 O4 126.4(6) . . ? O2 C2 C1 117.6(6) . . ? O4 C2 C1 115.9(6) . . ? O7 C3 O5 127.1(6) . . ? O7 C3 C4 117.3(6) . . ? O5 C3 C4 115.6(6) . . ? O6 C4 O8 126.0(6) . . ? O6 C4 C3 118.5(6) . . ? O8 C4 C3 115.5(6) . . ? O9 C5 O11 127.4(5) . . ? O9 C5 C6 116.8(6) . . ? O11 C5 C6 115.8(5) . . ? O10 C6 O12 126.5(6) . . ? O10 C6 C5 117.6(5) . . ? O12 C6 C5 115.9(6) . . ? C8 C7 N1 113.0(6) . . ? C8 C7 H7A 109.0 . . ? N1 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? N1 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N2 C8 C7 110.4(6) . . ? N2 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? N2 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 N1 112.3(6) . . ? C10 C9 H9A 109.2 . . ? N1 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? N1 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? N3 C10 C9 107.1(6) . . ? N3 C10 H10A 110.3 . . ? C9 C10 H10A 110.3 . . ? N3 C10 H10B 110.3 . . ? C9 C10 H10B 110.3 . . ? H10A C10 H10B 108.6 . . ? N1 C11 C12 111.8(5) . . ? N1 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? N1 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? N4 C12 C11 111.7(5) . . ? N4 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? N4 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C7 N1 C9 112.1(5) . . ? C7 N1 C11 112.5(5) . . ? C9 N1 C11 111.5(5) . . ? C7 N1 HN1 106.6 . . ? C9 N1 HN1 106.8 . . ? C11 N1 HN1 106.9 . . ? C8 N2 HN2A 117.6 . . ? C8 N2 HN2B 109.5 . . ? HN2A N2 HN2B 93.3 . . ? C8 N2 HN2C 110.0 . . ? HN2A N2 HN2C 116.1 . . ? HN2B N2 HN2C 108.5 . . ? C10 N3 HN3A 109.3 . . ? C10 N3 HN3B 109.5 . . ? HN3A N3 HN3B 109.2 . . ? C10 N3 HN3C 109.6 . . ? HN3A N3 HN3C 109.2 . . ? HN3B N3 HN3C 109.9 . . ? C12 N4 HN4A 109.5 . . ? C12 N4 HN4B 109.5 . . ? HN4A N4 HN4B 108.7 . . ? C12 N4 HN4C 109.7 . . ? HN4A N4 HN4C 109.6 . . ? HN4B N4 HN4C 109.7 . . ? HO1A OW1 HO1B 101.5 . . ? HO2A OW2 HO2B 104.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.338 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.168 #===End # # (H4APPIP)[U2F6(C2O4)3],4H2O (APPIP = 1,4-bis(3-amino-propyl)piperazine) # (compound 2) # data_ufox-2 _database_code_depnum_ccdc_archive 'CCDC 629038' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety (C10H28N4)[U2F6(C2O4)3].4H2O _chemical_formula_sum 'C16 H36 F6 N4 O16 U2' _chemical_formula_weight 1130.55 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.3309(8) _cell_length_b 15.5639(11) _cell_length_c 17.5369(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.430(4) _cell_angle_gamma 90.00 _cell_volume 2807.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.078 _exptl_crystal_size_mid 0.078 _exptl_crystal_size_min 0.052 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 11.644 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.385 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_process_details 'SADABS program' _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 CCD _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23468 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6305 _reflns_number_gt 5121 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material ? _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^)+(0.0253P)^2^+8.2404P] 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 SHELXL _refine_ls_extinction_coef 0.00017(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6305 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.002 _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 U1 U 0.041313(15) 0.230248(10) 0.066618(9) 0.01481(6) Uani 1 1 d . . . U2 U 0.572948(15) 0.232295(11) 0.298758(9) 0.01641(6) Uani 1 1 d . . . F1 F 0.0866(3) 0.09461(17) 0.06500(16) 0.0280(6) Uani 1 1 d . . . F2 F 0.1148(3) 0.35850(17) 0.08028(16) 0.0279(6) Uani 1 1 d . . . F3 F 0.1285(3) 0.24554(18) -0.04240(16) 0.0251(6) Uani 1 1 d . . . F4 F 0.5211(3) 0.09714(18) 0.29883(16) 0.0299(7) Uani 1 1 d . . . F5 F 0.4965(3) 0.2441(2) 0.41177(17) 0.0316(7) Uani 1 1 d . . . F6 F 0.4961(3) 0.36037(18) 0.27734(16) 0.0291(7) Uani 1 1 d . . . O1 O -0.1099(3) 0.3278(2) -0.0140(2) 0.0280(8) Uani 1 1 d . . . O2 O -0.1170(3) 0.1585(2) -0.0290(2) 0.0260(8) Uani 1 1 d . . . O3 O -0.1086(3) 0.3156(2) 0.14523(19) 0.0222(7) Uani 1 1 d . . . O4 O -0.1095(3) 0.1476(2) 0.14807(18) 0.0205(7) Uani 1 1 d . . . O5 O 0.2913(3) 0.2186(2) 0.08478(19) 0.0224(7) Uani 1 1 d . . . O6 O 0.1450(3) 0.2227(2) 0.20015(19) 0.0253(8) Uani 1 1 d . . . O7 O -0.2678(3) 0.3407(2) -0.10922(19) 0.0267(8) Uani 1 1 d . . . O8 O -0.2758(3) 0.1697(2) -0.12350(19) 0.0245(7) Uani 1 1 d . . . O9 O -0.2809(3) 0.3188(2) 0.21373(19) 0.0243(7) Uani 1 1 d . . . O10 O -0.2734(3) 0.1480(2) 0.22263(19) 0.0230(7) Uani 1 1 d . . . O11 O 0.4710(3) 0.2177(2) 0.16531(19) 0.0233(7) Uani 1 1 d . . . O12 O 0.3231(3) 0.2218(2) 0.28290(19) 0.0287(8) Uani 1 1 d . . . N1 N -0.2891(5) 0.0014(3) -0.0229(3) 0.0378(12) Uani 1 1 d . . . HN1A H -0.3097 0.0588 -0.0078 0.050 Uiso 1 1 d . . . HN1B H -0.3309 -0.0019 -0.0708 0.050 Uiso 1 1 d . . . HN1C H -0.2053 -0.0105 -0.0253 0.050 Uiso 1 1 d . . . N2 N -0.0785(4) -0.0183(3) 0.1951(2) 0.0251(9) Uani 1 1 d . . . HN2 H -0.0891 0.0418 0.1853 0.050 Uiso 1 1 d . . . N3 N 0.0596(4) -0.0118(3) 0.3460(3) 0.0305(10) Uani 1 1 d . . . HN3 H 0.0686 -0.0726 0.3559 0.050 Uiso 1 1 d . . . N4 N 0.3460(4) 0.1400(3) 0.4891(3) 0.0358(11) Uani 1 1 d . . . HN4A H 0.2715 0.1591 0.4871 0.050 Uiso 1 1 d . . . HN4B H 0.3833 0.1290 0.5366 0.050 Uiso 1 1 d . . . HN4C H 0.4103 0.1801 0.4639 0.050 Uiso 1 1 d . . . C1 C -0.1906(4) 0.2987(3) -0.0649(3) 0.0202(9) Uani 1 1 d . . . C2 C -0.1946(4) 0.2005(3) -0.0730(3) 0.0204(9) Uani 1 1 d . . . C3 C -0.1961(4) 0.2815(3) 0.1807(3) 0.0175(9) Uani 1 1 d . . . C4 C -0.1935(4) 0.1837(3) 0.1839(2) 0.0157(9) Uani 1 1 d . . . C5 C 0.3493(4) 0.2188(3) 0.1492(3) 0.0178(9) Uani 1 1 d . . . C6 C 0.2660(4) 0.2216(3) 0.2174(3) 0.0194(10) Uani 1 1 d . . . C7 C -0.3367(6) -0.0614(4) 0.0315(3) 0.0364(13) Uani 1 1 d . . . H7A H -0.3117 -0.1188 0.0173 0.044 Uiso 1 1 calc R . . H7B H -0.4310 -0.0592 0.0280 0.044 Uiso 1 1 calc R . . C8 C -0.2837(6) -0.0438(4) 0.1121(3) 0.0362(13) Uani 1 1 d . . . H8A H -0.3306 -0.0783 0.1465 0.043 Uiso 1 1 calc R . . H8B H -0.2977 0.0162 0.1239 0.043 Uiso 1 1 calc R . . C9 C -0.1399(6) -0.0639(4) 0.1256(3) 0.0384(14) Uani 1 1 d . . . H9A H -0.1281 -0.1254 0.1322 0.046 Uiso 1 1 calc R . . H9B H -0.0971 -0.0465 0.0812 0.046 Uiso 1 1 calc R . . C10 C -0.1443(5) -0.0366(3) 0.2656(3) 0.0256(11) Uani 1 1 d . . . H10A H -0.1399 -0.0976 0.2768 0.031 Uiso 1 1 calc R . . H10B H -0.2351 -0.0203 0.2574 0.031 Uiso 1 1 calc R . . C11 C 0.0633(5) -0.0378(4) 0.2084(3) 0.0321(12) Uani 1 1 d . . . H11A H 0.1056 -0.0209 0.1636 0.038 Uiso 1 1 calc R . . H11B H 0.0751 -0.0992 0.2154 0.038 Uiso 1 1 calc R . . C12 C -0.0794(5) 0.0127(3) 0.3317(3) 0.0282(11) Uani 1 1 d . . . H12A H -0.0860 0.0738 0.3209 0.034 Uiso 1 1 calc R . . H12B H -0.1233 0.0013 0.3772 0.034 Uiso 1 1 calc R . . C13 C 0.1259(5) 0.0086(3) 0.2776(3) 0.0351(13) Uani 1 1 d . . . H13A H 0.2166 -0.0080 0.2862 0.042 Uiso 1 1 calc R . . H13B H 0.1223 0.0701 0.2685 0.042 Uiso 1 1 calc R . . C14 C 0.1183(6) 0.0283(4) 0.4197(4) 0.0539(19) Uani 1 1 d . . . H14A H 0.1161 0.0902 0.4138 0.065 Uiso 1 1 calc R . . H14B H 0.0639 0.0138 0.4601 0.065 Uiso 1 1 calc R . . C15 C 0.2542(7) 0.0021(4) 0.4449(4) 0.0538(18) Uani 1 1 d . . . H15A H 0.2588 -0.0141 0.4985 0.065 Uiso 1 1 calc R . . H15B H 0.2750 -0.0485 0.4162 0.065 Uiso 1 1 calc R . . C16 C 0.3522(7) 0.0669(4) 0.4359(4) 0.0534(18) Uani 1 1 d . . . H16A H 0.3417 0.0882 0.3837 0.064 Uiso 1 1 calc R . . H16B H 0.4375 0.0406 0.4442 0.064 Uiso 1 1 calc R . . OW1 O -0.0091(4) 0.2691(3) -0.1806(2) 0.0382(10) Uani 1 1 d . . . HO1A H 0.0533 0.2671 -0.2138 0.050 Uiso 1 1 d . . . HO1B H 0.0411 0.2632 -0.1309 0.050 Uiso 1 1 d . . . OW2 O 0.6098(4) 0.3329(3) 0.5375(2) 0.0505(12) Uani 1 1 d . . . HO2A H 0.5704 0.3329 0.4708 0.050 Uiso 1 1 d . . . HO2B H 0.5216 0.3142 0.5543 0.050 Uiso 1 1 d . . . OW3 O 0.6057(5) 0.5121(3) 0.3268(2) 0.0547(13) Uani 1 1 d . . . HO3A H 0.5520 0.5487 0.3005 0.050 Uiso 1 1 d . . . HO3B H 0.5861 0.4570 0.3072 0.050 Uiso 1 1 d . . . OW4 O 0.5717(6) -0.0645(3) 0.3657(3) 0.0630(14) Uani 1 1 d . . . HO4A H 0.5619 -0.0028 0.3497 0.050 Uiso 1 1 d . . . HO4B H 0.5649 -0.0792 0.3167 0.050 Uiso 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 U1 0.01222(9) 0.01752(9) 0.01423(9) 0.00042(6) -0.00120(6) -0.00043(6) U2 0.01320(9) 0.02038(10) 0.01521(10) -0.00104(6) -0.00099(6) -0.00072(6) F1 0.0277(16) 0.0227(15) 0.0339(16) 0.0006(12) 0.0040(13) 0.0066(12) F2 0.0286(16) 0.0220(15) 0.0327(16) -0.0032(12) 0.0019(13) -0.0067(12) F3 0.0237(15) 0.0353(16) 0.0164(14) 0.0005(11) 0.0023(12) -0.0023(12) F4 0.0322(17) 0.0264(15) 0.0307(16) 0.0003(12) 0.0012(13) -0.0103(13) F5 0.0292(17) 0.0476(19) 0.0186(15) -0.0051(12) 0.0049(13) -0.0084(13) F6 0.0260(16) 0.0275(16) 0.0336(17) -0.0019(12) 0.0019(13) 0.0060(12) O1 0.0258(19) 0.0260(19) 0.030(2) -0.0020(14) -0.0076(15) 0.0007(14) O2 0.0250(19) 0.0213(17) 0.0295(19) 0.0044(14) -0.0088(15) 0.0013(14) O3 0.0227(17) 0.0153(16) 0.0294(18) 0.0021(13) 0.0079(14) 0.0014(13) O4 0.0191(17) 0.0166(16) 0.0272(18) 0.0017(13) 0.0092(14) 0.0025(13) O5 0.0132(16) 0.034(2) 0.0195(18) 0.0026(14) -0.0018(13) 0.0018(13) O6 0.0131(17) 0.044(2) 0.0181(17) 0.0015(14) -0.0008(13) 0.0000(14) O7 0.0261(19) 0.0248(18) 0.0272(19) 0.0053(14) -0.0083(15) -0.0001(15) O8 0.0227(18) 0.0215(17) 0.0277(19) -0.0039(14) -0.0060(14) 0.0000(13) O9 0.0217(18) 0.0194(17) 0.0329(19) -0.0009(14) 0.0082(15) 0.0015(13) O10 0.0215(17) 0.0200(17) 0.0289(19) 0.0019(14) 0.0092(14) -0.0004(13) O11 0.0157(17) 0.037(2) 0.0171(17) -0.0017(14) 0.0003(13) 0.0004(14) O12 0.0150(17) 0.056(3) 0.0147(18) 0.0006(15) -0.0014(13) -0.0028(15) N1 0.031(3) 0.051(3) 0.032(3) 0.007(2) 0.006(2) 0.011(2) N2 0.030(2) 0.022(2) 0.025(2) 0.0058(16) 0.0078(18) 0.0053(17) N3 0.034(3) 0.016(2) 0.041(3) -0.0028(18) -0.002(2) 0.0024(18) N4 0.026(2) 0.034(3) 0.048(3) -0.015(2) 0.010(2) -0.002(2) C1 0.019(2) 0.023(2) 0.019(2) 0.0008(18) 0.0016(19) 0.0003(19) C2 0.021(2) 0.024(2) 0.016(2) 0.0025(18) 0.0000(18) -0.0006(19) C3 0.013(2) 0.020(2) 0.020(2) 0.0018(17) 0.0016(17) -0.0016(17) C4 0.013(2) 0.017(2) 0.016(2) 0.0013(17) -0.0015(16) 0.0003(17) C5 0.015(2) 0.023(2) 0.016(2) -0.0004(17) 0.0012(17) -0.0001(17) C6 0.017(2) 0.026(3) 0.015(2) 0.0005(17) -0.0004(18) -0.0012(18) C7 0.036(3) 0.034(3) 0.040(3) -0.004(2) 0.002(3) -0.001(2) C8 0.039(3) 0.033(3) 0.037(3) -0.003(2) 0.009(3) -0.004(2) C9 0.048(4) 0.038(3) 0.028(3) -0.006(2) -0.001(3) 0.013(3) C10 0.027(3) 0.026(3) 0.024(3) 0.006(2) 0.005(2) 0.000(2) C11 0.034(3) 0.032(3) 0.032(3) 0.009(2) 0.012(2) 0.014(2) C12 0.031(3) 0.025(3) 0.029(3) 0.004(2) 0.008(2) 0.003(2) C13 0.028(3) 0.024(3) 0.054(4) 0.002(3) 0.009(3) 0.001(2) C14 0.047(4) 0.049(4) 0.062(5) -0.028(3) -0.016(3) 0.003(3) C15 0.064(5) 0.035(4) 0.059(4) -0.011(3) -0.008(4) 0.002(3) C16 0.041(4) 0.050(4) 0.072(5) -0.019(3) 0.019(3) 0.001(3) OW1 0.024(2) 0.066(3) 0.026(2) 0.0059(18) 0.0065(16) 0.0072(18) OW2 0.044(3) 0.076(3) 0.032(2) -0.006(2) 0.0088(19) -0.025(2) OW3 0.080(4) 0.032(2) 0.046(3) 0.0000(19) -0.028(2) 0.000(2) OW4 0.109(4) 0.037(3) 0.041(3) -0.003(2) -0.002(3) 0.018(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 U1 F2 2.141(3) . ? U1 F1 2.163(3) . ? U1 F3 2.202(3) . ? U1 O6 2.484(3) . ? U1 O2 2.493(3) . ? U1 O1 2.516(3) . ? U1 O3 2.544(3) . ? U1 O4 2.558(3) . ? U1 O5 2.579(3) . ? U2 F6 2.165(3) . ? U2 F4 2.171(3) . ? U2 F5 2.209(3) . ? U2 O7 2.470(3) 4_666 ? U2 O11 2.484(3) . ? U2 O8 2.494(3) 4_666 ? U2 O10 2.535(3) 1_655 ? U2 O12 2.575(3) . ? U2 O9 2.597(3) 1_655 ? O1 C1 1.247(5) . ? O2 C2 1.244(5) . ? O3 C3 1.261(5) . ? O4 C4 1.252(5) . ? O5 C5 1.227(6) . ? O6 C6 1.258(6) . ? O7 C1 1.244(5) . ? O7 U2 2.470(3) 4_465 ? O8 C2 1.256(5) . ? O8 U2 2.494(3) 4_465 ? O9 C3 1.239(5) . ? O9 U2 2.597(3) 1_455 ? O10 C4 1.248(5) . ? O10 U2 2.535(3) 1_455 ? O11 C5 1.262(6) . ? O12 C6 1.241(6) . ? N1 C7 1.481(7) . ? N1 HN1A 0.9620 . ? N1 HN1B 0.9090 . ? N1 HN1C 0.8901 . ? N2 C11 1.492(6) . ? N2 C10 1.494(6) . ? N2 C9 1.498(7) . ? N2 HN2 0.9558 . ? N3 C13 1.471(7) . ? N3 C12 1.484(7) . ? N3 C14 1.510(7) . ? N3 HN3 0.9650 . ? N4 C16 1.476(7) . ? N4 HN4A 0.8224 . ? N4 HN4B 0.9013 . ? N4 HN4C 1.0399 . ? C1 C2 1.535(7) . ? C3 C4 1.524(6) . ? C5 C6 1.538(6) . ? C7 C8 1.492(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.515(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C12 1.495(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C13 1.505(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.489(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.448(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? OW1 HO1A 0.9090 . ? OW1 HO1B 0.9758 . ? OW2 HO2A 1.2012 . ? OW2 HO2B 1.0264 . ? OW3 HO3A 0.8923 . ? OW3 HO3B 0.9385 . ? OW4 HO4A 1.0032 . ? OW4 HO4B 0.8854 . ? 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 F2 U1 F1 146.79(11) . . ? F2 U1 F3 80.01(11) . . ? F1 U1 F3 89.28(11) . . ? F2 U1 O6 79.74(11) . . ? F1 U1 O6 83.79(11) . . ? F3 U1 O6 130.41(11) . . ? F2 U1 O2 134.10(11) . . ? F1 U1 O2 71.51(11) . . ? F3 U1 O2 76.15(11) . . ? O6 U1 O2 144.09(11) . . ? F2 U1 O1 72.24(11) . . ? F1 U1 O1 134.84(11) . . ? F3 U1 O1 74.34(11) . . ? O6 U1 O1 138.42(11) . . ? O2 U1 O1 63.84(11) . . ? F2 U1 O3 71.33(10) . . ? F1 U1 O3 131.34(10) . . ? F3 U1 O3 137.24(10) . . ? O6 U1 O3 75.18(11) . . ? O2 U1 O3 101.79(11) . . ? O1 U1 O3 67.15(11) . . ? F2 U1 O4 129.38(10) . . ? F1 U1 O4 70.16(10) . . ? F3 U1 O4 149.32(10) . . ? O6 U1 O4 71.38(11) . . ? O2 U1 O4 75.82(11) . . ? O1 U1 O4 103.80(11) . . ? O3 U1 O4 61.68(10) . . ? F2 U1 O5 73.24(11) . . ? F1 U1 O5 73.59(11) . . ? F3 U1 O5 68.13(10) . . ? O6 U1 O5 62.79(11) . . ? O2 U1 O5 129.57(11) . . ? O1 U1 O5 132.34(11) . . ? O3 U1 O5 128.62(11) . . ? O4 U1 O5 123.47(10) . . ? F6 U2 F4 143.68(11) . . ? F6 U2 F5 85.55(11) . . ? F4 U2 F5 88.35(11) . . ? F6 U2 O7 138.36(11) . 4_666 ? F4 U2 O7 72.74(11) . 4_666 ? F5 U2 O7 74.03(12) . 4_666 ? F6 U2 O11 78.75(11) . . ? F4 U2 O11 80.16(11) . . ? F5 U2 O11 134.18(11) . . ? O7 U2 O11 140.39(11) 4_666 . ? F6 U2 O8 74.50(11) . 4_666 ? F4 U2 O8 137.21(11) . 4_666 ? F5 U2 O8 73.58(11) . 4_666 ? O7 U2 O8 65.14(11) 4_666 4_666 ? O11 U2 O8 139.35(11) . 4_666 ? F6 U2 O10 128.52(11) . 1_655 ? F4 U2 O10 70.46(11) . 1_655 ? F5 U2 O10 144.14(11) . 1_655 ? O7 U2 O10 72.20(11) 4_666 1_655 ? O11 U2 O10 71.78(11) . 1_655 ? O8 U2 O10 102.30(11) 4_666 1_655 ? F6 U2 O12 72.07(11) . . ? F4 U2 O12 72.17(12) . . ? F5 U2 O12 70.27(11) . . ? O7 U2 O12 129.83(11) 4_666 . ? O11 U2 O12 63.96(11) . . ? O8 U2 O12 131.88(11) 4_666 . ? O10 U2 O12 125.56(11) 1_655 . ? F6 U2 O9 69.31(10) . 1_655 ? F4 U2 O9 131.28(11) . 1_655 ? F5 U2 O9 138.46(11) . 1_655 ? O7 U2 O9 103.05(11) 4_666 1_655 ? O11 U2 O9 74.00(11) . 1_655 ? O8 U2 O9 68.20(11) 4_666 1_655 ? O10 U2 O9 62.53(10) 1_655 1_655 ? O12 U2 O9 127.04(11) . 1_655 ? C1 O1 U1 121.4(3) . . ? C2 O2 U1 121.6(3) . . ? C3 O3 U1 123.3(3) . . ? C4 O4 U1 122.9(3) . . ? C5 O5 U1 120.6(3) . . ? C6 O6 U1 123.8(3) . . ? C1 O7 U2 121.0(3) . 4_465 ? C2 O8 U2 119.6(3) . 4_465 ? C3 O9 U2 120.1(3) . 1_455 ? C4 O10 U2 122.4(3) . 1_455 ? C5 O11 U2 122.3(3) . . ? C6 O12 U2 118.9(3) . . ? C7 N1 HN1A 109.9 . . ? C7 N1 HN1B 113.6 . . ? HN1A N1 HN1B 102.0 . . ? C7 N1 HN1C 106.1 . . ? HN1A N1 HN1C 116.6 . . ? HN1B N1 HN1C 108.9 . . ? C11 N2 C10 110.4(4) . . ? C11 N2 C9 111.4(4) . . ? C10 N2 C9 113.1(4) . . ? C11 N2 HN2 108.7 . . ? C10 N2 HN2 106.4 . . ? C9 N2 HN2 106.5 . . ? C13 N3 C12 109.0(4) . . ? C13 N3 C14 115.4(5) . . ? C12 N3 C14 110.0(4) . . ? C13 N3 HN3 108.3 . . ? C12 N3 HN3 111.0 . . ? C14 N3 HN3 103.1 . . ? C16 N4 HN4A 110.4 . . ? C16 N4 HN4B 113.4 . . ? HN4A N4 HN4B 115.1 . . ? C16 N4 HN4C 97.3 . . ? HN4A N4 HN4C 113.5 . . ? HN4B N4 HN4C 105.8 . . ? O7 C1 O1 127.0(5) . . ? O7 C1 C2 117.1(4) . . ? O1 C1 C2 116.0(4) . . ? O2 C2 O8 125.8(5) . . ? O2 C2 C1 117.1(4) . . ? O8 C2 C1 117.1(4) . . ? O9 C3 O3 127.2(4) . . ? O9 C3 C4 117.5(4) . . ? O3 C3 C4 115.3(4) . . ? O10 C4 O4 126.8(4) . . ? O10 C4 C3 117.1(4) . . ? O4 C4 C3 116.1(4) . . ? O5 C5 O11 126.5(4) . . ? O5 C5 C6 117.1(4) . . ? O11 C5 C6 116.4(4) . . ? O12 C6 O6 126.6(4) . . ? O12 C6 C5 117.9(4) . . ? O6 C6 C5 115.4(4) . . ? N1 C7 C8 112.0(5) . . ? N1 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N1 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C9 112.1(5) . . ? C7 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? C7 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N2 C9 C8 111.3(4) . . ? N2 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? N2 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N2 C10 C12 109.8(4) . . ? N2 C10 H10A 109.7 . . ? C12 C10 H10A 109.7 . . ? N2 C10 H10B 109.7 . . ? C12 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N2 C11 C13 111.7(4) . . ? N2 C11 H11A 109.3 . . ? C13 C11 H11A 109.3 . . ? N2 C11 H11B 109.3 . . ? C13 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? N3 C12 C10 110.7(4) . . ? N3 C12 H12A 109.5 . . ? C10 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? N3 C13 C11 110.9(4) . . ? N3 C13 H13A 109.5 . . ? C11 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C15 C14 N3 115.6(5) . . ? C15 C14 H14A 108.4 . . ? N3 C14 H14A 108.4 . . ? C15 C14 H14B 108.4 . . ? N3 C14 H14B 108.4 . . ? H14A C14 H14B 107.4 . . ? C16 C15 C14 115.3(6) . . ? C16 C15 H15A 108.5 . . ? C14 C15 H15A 108.5 . . ? C16 C15 H15B 108.5 . . ? C14 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? C15 C16 N4 113.3(5) . . ? C15 C16 H16A 108.9 . . ? N4 C16 H16A 108.9 . . ? C15 C16 H16B 108.9 . . ? N4 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? HO1A OW1 HO1B 102.7 . . ? HO2A OW2 HO2B 92.9 . . ? HO3A OW3 HO3B 107.0 . . ? HO4A OW4 HO4B 88.8 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.759 _refine_diff_density_min -1.202 _refine_diff_density_rms 0.148