Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _publ_contact_author 'Prof Bryan Eichhorn' _publ_contact_author_address ; Bryan W. Eichhorn Department of Chemistry and Biochemistry University of Maryland College Park MD 20742 USA ; _publ_contact_author_email 'b._eichhorn@umail.umd.edu' _publ_contact_author_fax '(301) 314 9121' _publ_contact_author_phone '(301) 405 1864' _publ_requested_journal 'J. Chem. Soc. Chem. Commun.' _publ_requested_coeditor_name ? _publ_contact_letter ; ; # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_Cambridge 182 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Danis, Janet' ; Environmental and Chemical Science and Technology Division Los Alamos National Laboratory Los Alamos NM 87545 USA ; 'Runde, Wolfgang' ; Environmental and Chemical Science and Technology Division Los Alamos National Laboratory Los Alamos NM 87545 USA ; 'Fettinger, James C.' ; Department of Chemistry and Biochemistry University of Maryland College Park MD 20742 USA ; 'Eichhorn, Bryan' ; Department of Chemistry and Biochemistry University of Maryland College Park MD 20742 USA ; data_649all _database_code_CSD 171758 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H40 N4 O52 P8 U10' _chemical_formula_weight 3748.58 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' '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 I2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.4442(17) _cell_length_b 15.449(3) _cell_length_c 9.5719(17) _cell_angle_alpha 90.00 _cell_angle_beta 93.268(3) _cell_angle_gamma 90.00 _cell_volume 1394.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.085 _exptl_crystal_size_mid 0.048 _exptl_crystal_size_min 0.008 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 29.280 _exptl_absorpt_correction_type 'Analytical, SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8638 _diffrn_reflns_av_R_equivalents 0.0916 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 24.97 _reflns_number_total 1243 _reflns_number_gt 948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0684P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00017(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1243 _refine_ls_number_parameters 99 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 U1 U 0.45078(6) 0.22963(4) 0.19832(6) 0.0205(3) Uani 1 1 d . . . U2 U 0.0000 0.0000 0.0000 0.0425(5) Uani 1 4 d S . . P1 P 0.2030(4) 0.2014(4) -0.0317(4) 0.0317(12) Uani 1 1 d . . . O1 O 0.4633(14) 0.3391(9) 0.1515(11) 0.039(3) Uani 1 1 d . . . O2 O 0.4325(12) 0.1204(9) 0.2355(12) 0.033(3) Uani 1 1 d . . . O3 O 0.3645(10) 0.2011(7) -0.0507(10) 0.021(2) Uani 1 1 d . . . O4 O 0.1961(12) 0.2311(10) 0.1176(12) 0.044(4) Uani 1 1 d . . . O5 O 0.1248(12) 0.2647(10) -0.1352(12) 0.041(4) Uani 1 1 d . . . O6 O -0.058(3) 0.0000 -0.173(2) 0.059(6) Uani 1 2 d S . . O7 O 0.1476(14) 0.1092(10) -0.0536(15) 0.051(4) Uani 1 1 d . . . N21 N 0.337(5) 0.0000 0.499(4) 0.140(17) Uiso 1 2 d SD . . C21 C 0.239(5) 0.0000 0.597(4) 0.108(16) Uiso 1 2 d SD . . H21A H 0.1780 0.0518 0.5845 0.130 Uiso 0.50 1 calc PR . . H21B H 0.1780 -0.0518 0.5845 0.130 Uiso 0.50 1 calc PR . . C22 C 0.299(6) 0.0000 0.727(4) 0.121(18) Uiso 1 2 d SD . . H22A H 0.3733 -0.0446 0.7345 0.181 Uiso 0.50 1 calc PR . . H22B H 0.2274 -0.0122 0.7940 0.181 Uiso 0.50 1 calc PR . . H22C H 0.3419 0.0568 0.7473 0.181 Uiso 0.50 1 calc PR . . C23 C 0.242(7) 0.0000 0.385(6) 0.25(5) Uiso 1 2 d SD . . H23A H 0.2559 -0.0520 0.3271 0.305 Uiso 0.50 1 calc PR . . H23B H 0.2559 0.0520 0.3271 0.305 Uiso 0.50 1 calc PR . . C24 C 0.102(6) 0.0000 0.434(10) 0.31(6) Uiso 1 2 d SD . . H24A H 0.0859 -0.0539 0.4847 0.471 Uiso 0.50 1 calc PR . . H24B H 0.0326 0.0045 0.3540 0.471 Uiso 0.50 1 calc PR . . H24C H 0.0907 0.0494 0.4967 0.471 Uiso 0.50 1 calc PR . . 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 0.0071(3) 0.0417(5) 0.0125(4) -0.0005(3) -0.0004(2) 0.0010(3) U2 0.0566(11) 0.0317(9) 0.0392(9) 0.000 0.0016(7) 0.000 P1 0.007(2) 0.075(4) 0.014(2) 0.000(2) -0.0003(16) -0.002(2) O1 0.048(8) 0.054(9) 0.011(5) -0.011(6) -0.018(5) 0.007(7) O2 0.024(6) 0.046(8) 0.028(6) 0.012(6) -0.002(5) -0.007(6) O3 0.009(5) 0.037(7) 0.018(5) -0.003(5) 0.003(4) 0.007(5) O4 0.009(6) 0.108(12) 0.014(6) -0.007(6) 0.003(5) 0.004(6) O5 0.007(6) 0.095(12) 0.018(6) -0.016(6) -0.007(5) 0.004(6) O6 0.079(16) 0.056(15) 0.039(12) 0.000 -0.017(11) 0.000 O7 0.032(8) 0.066(11) 0.054(9) 0.013(8) -0.005(6) -0.021(7) _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 O2 1.736(13) . ? U1 O1 1.756(14) . ? U1 O5 2.225(12) 8 ? U1 O3 2.348(10) 2_655 ? U1 O4 2.382(11) 7 ? U1 O4 2.484(12) . ? U1 O3 2.513(10) . ? U1 P1 3.151(4) . ? U1 U1 3.9599(12) 2_655 ? U1 U1 4.0230(12) 7 ? U2 O6 1.72(2) 5 ? U2 O6 1.72(2) . ? U2 O7 2.266(13) . ? U2 O7 2.266(13) 6 ? U2 O7 2.266(13) 5 ? U2 O7 2.266(13) 2 ? P1 O4 1.506(12) . ? P1 O7 1.528(16) . ? P1 O3 1.547(10) . ? P1 O5 1.548(15) . ? O3 U1 2.348(10) 2_655 ? O4 U1 2.382(11) 7 ? O5 U1 2.225(12) 8_454 ? N21 C21 1.36(3) . ? N21 C23 1.37(4) . ? C21 C22 1.34(3) . ? C23 C24 1.43(4) . ? 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 U1 O1 176.6(5) . . ? O2 U1 O5 88.3(5) . 8 ? O1 U1 O5 95.0(5) . 8 ? O2 U1 O3 91.5(5) . 2_655 ? O1 U1 O3 87.9(5) . 2_655 ? O5 U1 O3 84.0(4) 8 2_655 ? O2 U1 O4 91.6(6) . 7 ? O1 U1 O4 89.7(6) . 7 ? O5 U1 O4 84.1(4) 8 7 ? O3 U1 O4 167.6(4) 2_655 7 ? O2 U1 O4 88.1(5) . . ? O1 U1 O4 89.4(6) . . ? O5 U1 O4 152.3(4) 8 . ? O3 U1 O4 123.6(4) 2_655 . ? O4 U1 O4 68.5(5) 7 . ? O2 U1 O3 89.6(5) . . ? O1 U1 O3 87.1(4) . . ? O5 U1 O3 150.7(4) 8 . ? O3 U1 O3 66.9(4) 2_655 . ? O4 U1 O3 125.1(4) 7 . ? O4 U1 O3 56.7(3) . . ? O2 U1 P1 86.0(4) . . ? O1 U1 P1 90.8(4) . . ? O5 U1 P1 174.3(4) 8 . ? O3 U1 P1 95.8(3) 2_655 . ? O4 U1 P1 96.4(3) 7 . ? O4 U1 P1 27.9(3) . . ? O3 U1 P1 29.0(2) . . ? O2 U1 U1 103.2(4) . 2_655 ? O1 U1 U1 74.5(4) . 2_655 ? O5 U1 U1 118.8(3) 8 2_655 ? O3 U1 U1 36.9(3) 2_655 2_655 ? O4 U1 U1 152.6(3) 7 2_655 ? O4 U1 U1 88.7(2) . 2_655 ? O3 U1 U1 34.1(2) . 2_655 ? P1 U1 U1 62.32(7) . 2_655 ? O2 U1 U1 89.8(4) . 7 ? O1 U1 U1 89.4(5) . 7 ? O5 U1 U1 119.1(3) 8 7 ? O3 U1 U1 157.0(3) 2_655 7 ? O4 U1 U1 35.1(3) 7 7 ? O4 U1 U1 33.4(3) . 7 ? O3 U1 U1 90.1(2) . 7 ? P1 U1 U1 61.35(7) . 7 ? U1 U1 U1 120.79(3) 2_655 7 ? O6 U2 O6 180.0(4) 5 . ? O6 U2 O7 93.0(6) 5 . ? O6 U2 O7 87.0(6) . . ? O6 U2 O7 93.0(6) 5 6 ? O6 U2 O7 87.0(6) . 6 ? O7 U2 O7 96.2(8) . 6 ? O6 U2 O7 87.0(6) 5 5 ? O6 U2 O7 93.0(6) . 5 ? O7 U2 O7 180.0(9) . 5 ? O7 U2 O7 83.8(8) 6 5 ? O6 U2 O7 87.0(6) 5 2 ? O6 U2 O7 93.0(6) . 2 ? O7 U2 O7 83.8(8) . 2 ? O7 U2 O7 180.0(8) 6 2 ? O7 U2 O7 96.2(8) 5 2 ? O4 P1 O7 112.4(8) . . ? O4 P1 O3 102.0(6) . . ? O7 P1 O3 108.3(8) . . ? O4 P1 O5 111.7(8) . . ? O7 P1 O5 110.7(8) . . ? O3 P1 O5 111.4(7) . . ? O4 P1 U1 50.6(5) . . ? O7 P1 U1 117.4(6) . . ? O3 P1 U1 52.0(4) . . ? O5 P1 U1 131.9(6) . . ? P1 O3 U1 147.3(6) . 2_655 ? P1 O3 U1 99.0(5) . . ? U1 O3 U1 109.0(4) 2_655 . ? P1 O4 U1 146.9(7) . 7 ? P1 O4 U1 101.5(5) . . ? U1 O4 U1 111.5(5) 7 . ? P1 O5 U1 142.1(9) . 8_454 ? P1 O7 U2 150.9(9) . . ? C21 N21 C23 96(4) . . ? C22 C21 N21 112(4) . . ? N21 C23 C24 109(4) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 2.259 _refine_diff_density_min -2.397 _refine_diff_density_rms 0.408