# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr M Ephritikhine' _publ_contact_author_email ephri@drecam.cea.fr _publ_section_title ; Towards high-valent uranium compounds from metallacyclic uranium(IV) precursors ; loop_ _publ_author_name M.Ephritikhine O.Benaud P.Thuery J.-C.Berthet # Attachment '- CIF.txt' data_2 _database_code_depnum_ccdc_archive 'CCDC 827395' #TrackingRef '- CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H52 I N3 Si6 U' _chemical_formula_weight 844.10 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8236(4) _cell_length_b 14.8539(3) _cell_length_c 19.3326(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.401(2) _cell_angle_gamma 90.00 _cell_volume 3389.34(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 105683 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 25.68 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light brown' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 5.923 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.382 _exptl_absorpt_correction_T_max 0.701 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and five \w scans with 2\% steps (426 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 105683 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.68 _reflns_number_total 6427 _reflns_number_gt 5912 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH~2~) or 1.5 (CH~3~) times that of the parent atom. 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^)+(0.0340P)^2^] 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 6427 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0553 _refine_ls_wR_factor_gt 0.0539 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.555 _refine_diff_density_min -1.435 _refine_diff_density_rms 0.164 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 U U 0.959879(8) 0.139540(7) 0.214629(5) 0.02856(5) Uani 1 1 d . . . I I 0.940397(17) -0.055266(13) 0.180371(10) 0.04019(6) Uani 1 1 d . . . Si1 Si 1.19763(7) 0.12606(6) 0.11481(5) 0.03535(19) Uani 1 1 d . . . Si2 Si 1.00940(6) 0.25475(5) 0.06845(4) 0.03326(17) Uani 1 1 d . . . Si3 Si 0.69181(6) 0.15999(6) 0.15930(4) 0.03314(17) Uani 1 1 d . . . Si4 Si 0.71931(7) 0.13723(6) 0.31588(5) 0.0373(2) Uani 1 1 d . . . Si5 Si 1.09625(7) 0.27982(6) 0.32039(4) 0.03785(19) Uani 1 1 d . . . Si6 Si 1.11211(7) 0.09474(6) 0.38196(4) 0.03479(18) Uani 1 1 d . . . N1 N 1.06988(18) 0.18002(16) 0.12935(12) 0.0312(5) Uani 1 1 d . . . N2 N 0.77684(19) 0.15319(16) 0.23569(12) 0.0315(5) Uani 1 1 d . . . N3 N 1.06141(18) 0.16596(16) 0.31544(12) 0.0299(5) Uani 1 1 d . . . C1 C 1.3054(3) 0.2068(2) 0.08503(18) 0.0503(8) Uani 1 1 d . . . H1A H 1.2787 0.2328 0.0416 0.075 Uiso 1 1 calc R . . H1B H 1.3752 0.1755 0.0792 0.075 Uiso 1 1 calc R . . H1C H 1.3176 0.2536 0.1189 0.075 Uiso 1 1 calc R . . C2 C 1.2560(3) 0.0741(2) 0.19748(17) 0.0436(7) Uani 1 1 d . . . H2A H 1.2704 0.1204 0.2316 0.065 Uiso 1 1 calc R . . H2B H 1.3254 0.0434 0.1894 0.065 Uiso 1 1 calc R . . H2C H 1.2022 0.0320 0.2139 0.065 Uiso 1 1 calc R . . C3 C 1.1797(3) 0.0344(2) 0.04902(18) 0.0505(8) Uani 1 1 d . . . H3A H 1.1258 -0.0087 0.0639 0.076 Uiso 1 1 calc R . . H3B H 1.2512 0.0052 0.0440 0.076 Uiso 1 1 calc R . . H3C H 1.1529 0.0596 0.0053 0.076 Uiso 1 1 calc R . . C4 C 1.0774(3) 0.3691(2) 0.0698(2) 0.0502(9) Uani 1 1 d . . . H4A H 1.0848 0.3909 0.1166 0.075 Uiso 1 1 calc R . . H4B H 1.0312 0.4099 0.0419 0.075 Uiso 1 1 calc R . . H4C H 1.1510 0.3649 0.0516 0.075 Uiso 1 1 calc R . . C5 C 1.0059(2) 0.2103(2) -0.02148(15) 0.0412(7) Uani 1 1 d . . . H5A H 1.0820 0.2020 -0.0351 0.062 Uiso 1 1 calc R . . H5B H 0.9671 0.2522 -0.0523 0.062 Uiso 1 1 calc R . . H5C H 0.9668 0.1536 -0.0235 0.062 Uiso 1 1 calc R . . C6 C 0.8578(2) 0.2658(2) 0.09191(15) 0.0343(6) Uani 1 1 d . . . H6A H 0.8563 0.2900 0.1384 0.041 Uiso 1 1 calc R . . H6B H 0.8191 0.3082 0.0605 0.041 Uiso 1 1 calc R . . C7 C 0.7929(2) 0.1744(2) 0.08846(15) 0.0347(6) Uani 1 1 d . . . H7A H 0.8476 0.1256 0.0914 0.042 Uiso 1 1 calc R . . H7B H 0.7509 0.1698 0.0440 0.042 Uiso 1 1 calc R . . C8 C 0.5998(3) 0.2626(2) 0.15615(17) 0.0448(8) Uani 1 1 d . . . H8A H 0.5379 0.2539 0.1854 0.067 Uiso 1 1 calc R . . H8B H 0.5708 0.2728 0.1094 0.067 Uiso 1 1 calc R . . H8C H 0.6436 0.3138 0.1721 0.067 Uiso 1 1 calc R . . C9 C 0.6075(3) 0.0561(2) 0.13897(18) 0.0475(8) Uani 1 1 d . . . H9A H 0.6558 0.0043 0.1442 0.071 Uiso 1 1 calc R . . H9B H 0.5758 0.0591 0.0922 0.071 Uiso 1 1 calc R . . H9C H 0.5475 0.0513 0.1701 0.071 Uiso 1 1 calc R . . C10 C 0.7557(3) 0.0218(3) 0.34888(19) 0.0571(9) Uani 1 1 d . . . H10A H 0.7213 -0.0224 0.3180 0.086 Uiso 1 1 calc R . . H10B H 0.7280 0.0143 0.3942 0.086 Uiso 1 1 calc R . . H10C H 0.8364 0.0141 0.3513 0.086 Uiso 1 1 calc R . . C11 C 0.7756(3) 0.2224(2) 0.37895(17) 0.0481(8) Uani 1 1 d . . . H11A H 0.8569 0.2223 0.3800 0.072 Uiso 1 1 calc R . . H11B H 0.7513 0.2081 0.4242 0.072 Uiso 1 1 calc R . . H11C H 0.7478 0.2808 0.3653 0.072 Uiso 1 1 calc R . . C12 C 0.5616(3) 0.1462(3) 0.3129(2) 0.0551(10) Uani 1 1 d . . . H12A H 0.5392 0.2063 0.3001 0.083 Uiso 1 1 calc R . . H12B H 0.5352 0.1322 0.3577 0.083 Uiso 1 1 calc R . . H12C H 0.5292 0.1045 0.2793 0.083 Uiso 1 1 calc R . . C13 C 1.0840(3) 0.3318(2) 0.40763(18) 0.0547(9) Uani 1 1 d . . . H13A H 1.0098 0.3203 0.4233 0.082 Uiso 1 1 calc R . . H13B H 1.0958 0.3956 0.4046 0.082 Uiso 1 1 calc R . . H13C H 1.1400 0.3062 0.4398 0.082 Uiso 1 1 calc R . . C14 C 1.2405(3) 0.3049(2) 0.2907(2) 0.0557(9) Uani 1 1 d . . . H14A H 1.2957 0.2689 0.3164 0.084 Uiso 1 1 calc R . . H14B H 1.2575 0.3675 0.2981 0.084 Uiso 1 1 calc R . . H14C H 1.2425 0.2913 0.2422 0.084 Uiso 1 1 calc R . . C15 C 0.9909(3) 0.3425(2) 0.26088(18) 0.0465(8) Uani 1 1 d . . . H15A H 1.0004 0.3249 0.2138 0.070 Uiso 1 1 calc R . . H15B H 1.0035 0.4061 0.2657 0.070 Uiso 1 1 calc R . . H15C H 0.9154 0.3283 0.2730 0.070 Uiso 1 1 calc R . . C16 C 1.2652(3) 0.1149(3) 0.40615(19) 0.0521(9) Uani 1 1 d . . . H16A H 1.3086 0.1061 0.3663 0.078 Uiso 1 1 calc R . . H16B H 1.2904 0.0735 0.4420 0.078 Uiso 1 1 calc R . . H16C H 1.2753 0.1755 0.4227 0.078 Uiso 1 1 calc R . . C17 C 1.0341(3) 0.1112(2) 0.46275(17) 0.0499(8) Uani 1 1 d . . . H17A H 1.0352 0.1738 0.4751 0.075 Uiso 1 1 calc R . . H17B H 1.0702 0.0767 0.4998 0.075 Uiso 1 1 calc R . . H17C H 0.9571 0.0915 0.4547 0.075 Uiso 1 1 calc R . . C18 C 1.1001(3) -0.0269(2) 0.35914(16) 0.0404(7) Uani 1 1 d . . . H18A H 1.0231 -0.0405 0.3443 0.061 Uiso 1 1 calc R . . H18B H 1.1223 -0.0627 0.3990 0.061 Uiso 1 1 calc R . . H18C H 1.1486 -0.0401 0.3224 0.061 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 U 0.02600(7) 0.03138(8) 0.02820(7) -0.00242(4) 0.00067(4) -0.00085(4) I 0.04582(12) 0.03236(11) 0.04243(12) -0.00465(8) 0.00284(9) -0.00064(8) Si1 0.0304(4) 0.0396(5) 0.0363(4) 0.0013(3) 0.0036(3) 0.0009(3) Si2 0.0333(4) 0.0334(4) 0.0331(4) 0.0040(3) 0.0024(3) -0.0025(3) Si3 0.0260(4) 0.0376(4) 0.0356(4) 0.0000(3) -0.0006(3) -0.0011(3) Si4 0.0326(4) 0.0454(5) 0.0346(5) -0.0005(3) 0.0066(3) 0.0036(3) Si5 0.0458(5) 0.0299(4) 0.0368(4) -0.0025(3) -0.0068(4) -0.0058(3) Si6 0.0372(4) 0.0343(5) 0.0322(4) 0.0014(3) -0.0037(3) -0.0018(3) N1 0.0299(11) 0.0317(13) 0.0318(12) 0.0012(10) 0.0015(9) -0.0027(10) N2 0.0269(12) 0.0354(13) 0.0322(13) -0.0023(10) 0.0022(9) 0.0015(9) N3 0.0324(12) 0.0274(12) 0.0291(12) -0.0026(10) -0.0053(9) -0.0038(10) C1 0.0349(16) 0.061(2) 0.055(2) 0.0086(17) 0.0048(14) -0.0017(15) C2 0.0411(17) 0.0420(18) 0.0474(19) 0.0049(15) 0.0005(14) 0.0053(14) C3 0.0493(19) 0.056(2) 0.0469(19) -0.0070(16) 0.0071(15) 0.0100(16) C4 0.051(2) 0.041(2) 0.059(2) 0.0080(15) 0.0035(17) -0.0088(14) C5 0.0371(16) 0.054(2) 0.0327(16) 0.0053(14) 0.0034(12) 0.0035(14) C6 0.0371(15) 0.0332(15) 0.0323(15) 0.0039(12) 0.0000(12) 0.0015(12) C7 0.0321(14) 0.0401(17) 0.0310(15) 0.0022(12) -0.0055(11) 0.0008(12) C8 0.0351(16) 0.0499(19) 0.0489(19) 0.0031(15) -0.0008(14) 0.0059(14) C9 0.0385(17) 0.050(2) 0.054(2) -0.0043(16) 0.0019(14) -0.0075(14) C10 0.062(2) 0.056(2) 0.056(2) 0.0136(18) 0.0172(18) 0.0054(18) C11 0.0454(18) 0.061(2) 0.0383(17) -0.0084(16) 0.0052(14) 0.0093(16) C12 0.0367(18) 0.078(3) 0.051(2) -0.0055(18) 0.0104(16) -0.0012(16) C13 0.077(3) 0.0407(19) 0.044(2) -0.0080(16) -0.0142(17) -0.0085(18) C14 0.054(2) 0.0430(19) 0.069(2) 0.0089(18) -0.0029(18) -0.0143(16) C15 0.064(2) 0.0318(16) 0.0431(19) -0.0036(14) -0.0028(16) 0.0053(15) C16 0.0468(19) 0.056(2) 0.051(2) 0.0074(17) -0.0171(16) -0.0069(16) C17 0.068(2) 0.0456(19) 0.0363(18) 0.0038(15) 0.0008(16) 0.0008(17) C18 0.0440(17) 0.0381(17) 0.0388(17) 0.0059(14) -0.0002(13) 0.0030(13) _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 U N2 2.235(2) . ? U N1 2.242(2) . ? U N3 2.262(2) . ? U I 2.9743(2) . ? Si1 N1 1.747(2) . ? Si1 C1 1.865(3) . ? Si1 C3 1.866(3) . ? Si1 C2 1.869(3) . ? Si2 N1 1.741(2) . ? Si2 C5 1.858(3) . ? Si2 C4 1.879(3) . ? Si2 C6 1.882(3) . ? Si3 N2 1.740(3) . ? Si3 C9 1.867(3) . ? Si3 C8 1.872(3) . ? Si3 C7 1.883(3) . ? Si4 N2 1.746(2) . ? Si4 C11 1.853(3) . ? Si4 C12 1.867(3) . ? Si4 C10 1.871(4) . ? Si5 N3 1.742(2) . ? Si5 C13 1.868(4) . ? Si5 C14 1.870(3) . ? Si5 C15 1.890(3) . ? Si6 N3 1.744(2) . ? Si6 C18 1.863(3) . ? Si6 C16 1.866(3) . ? Si6 C17 1.876(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? 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 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.559(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? 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 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? 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 N2 U N1 136.05(9) . . ? N2 U N3 107.30(8) . . ? N1 U N3 106.60(8) . . ? N2 U I 93.77(6) . . ? N1 U I 97.92(6) . . ? N3 U I 113.00(6) . . ? N1 Si1 C1 111.56(14) . . ? N1 Si1 C3 112.32(14) . . ? C1 Si1 C3 108.10(17) . . ? N1 Si1 C2 109.30(13) . . ? C1 Si1 C2 107.74(15) . . ? C3 Si1 C2 107.64(16) . . ? N1 Si2 C5 113.05(13) . . ? N1 Si2 C4 114.12(15) . . ? C5 Si2 C4 108.69(16) . . ? N1 Si2 C6 104.58(12) . . ? C5 Si2 C6 106.74(13) . . ? C4 Si2 C6 109.30(15) . . ? N2 Si3 C9 113.91(14) . . ? N2 Si3 C8 112.36(14) . . ? C9 Si3 C8 111.38(15) . . ? N2 Si3 C7 105.32(12) . . ? C9 Si3 C7 107.16(14) . . ? C8 Si3 C7 106.07(14) . . ? N2 Si4 C11 110.36(14) . . ? N2 Si4 C12 113.82(15) . . ? C11 Si4 C12 106.93(16) . . ? N2 Si4 C10 109.49(14) . . ? C11 Si4 C10 109.57(17) . . ? C12 Si4 C10 106.54(18) . . ? N3 Si5 C13 114.83(15) . . ? N3 Si5 C14 113.20(14) . . ? C13 Si5 C14 108.44(18) . . ? N3 Si5 C15 107.43(14) . . ? C13 Si5 C15 105.22(16) . . ? C14 Si5 C15 107.15(17) . . ? N3 Si6 C18 113.30(13) . . ? N3 Si6 C16 111.92(14) . . ? C18 Si6 C16 105.92(16) . . ? N3 Si6 C17 111.74(14) . . ? C18 Si6 C17 106.81(15) . . ? C16 Si6 C17 106.71(17) . . ? Si2 N1 Si1 120.53(13) . . ? Si2 N1 U 115.82(11) . . ? Si1 N1 U 122.69(12) . . ? Si3 N2 Si4 121.72(13) . . ? Si3 N2 U 111.57(12) . . ? Si4 N2 U 125.59(13) . . ? Si5 N3 Si6 118.59(13) . . ? Si5 N3 U 109.12(12) . . ? Si6 N3 U 132.21(12) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 Si2 112.75(19) . . ? C7 C6 H6A 109.0 . . ? Si2 C6 H6A 109.0 . . ? C7 C6 H6B 109.0 . . ? Si2 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C6 C7 Si3 113.6(2) . . ? C6 C7 H7A 108.9 . . ? Si3 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? Si3 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? Si3 C8 H8A 109.5 . . ? Si3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si3 C9 H9A 109.5 . . ? Si3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si4 C10 H10A 109.5 . . ? Si4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si4 C11 H11A 109.5 . . ? Si4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si4 C12 H12A 109.5 . . ? Si4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si5 C13 H13A 109.5 . . ? Si5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si5 C14 H14A 109.5 . . ? Si5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si5 C15 H15A 109.5 . . ? Si5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si6 C16 H16A 109.5 . . ? Si6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si6 C17 H17A 109.5 . . ? Si6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si6 C18 H18A 109.5 . . ? Si6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? #===END data_5b.0.5n-pentane _database_code_depnum_ccdc_archive 'CCDC 827396' #TrackingRef '- CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.50 H78 N6 Na O7 Si6 U' _chemical_formula_weight 1094.57 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.2539(3) _cell_length_b 18.7050(9) _cell_length_c 39.6518(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11313.6(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 168878 _cell_measurement_theta_min 3.43 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4464 _exptl_absorpt_coefficient_mu 3.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.563 _exptl_absorpt_correction_T_max 0.808 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 35 mm' _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and three \w scans with 2\% steps (332 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 168878 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 25.68 _reflns_number_total 21419 _reflns_number_gt 14631 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. The two pentane solvent molecules have been given 0.5 occupancy factors in order to retain acceptable displacement parameters. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for some badly behaving atoms, as well as restraints on bond lengths and angles for the solvent molecules. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH~2~) or 1.5 (CH~3~) times that of the parent atom. 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^)+(0.0647P)^2^+2.6856P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(6) _refine_ls_number_reflns 21419 _refine_ls_number_parameters 1042 _refine_ls_number_restraints 287 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.397 _refine_diff_density_min -1.079 _refine_diff_density_rms 0.091 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 0.62206(2) 0.997571(18) 0.502285(8) 0.05952(10) Uani 1 1 d . . . Na1 Na 0.7504(2) 1.13649(18) 0.36371(8) 0.0704(8) Uani 1 1 d . . . Si1A Si 0.5874(3) 0.8566(2) 0.45442(12) 0.1232(14) Uani 1 1 d . . . Si2A Si 0.6907(4) 0.8213(2) 0.51784(15) 0.1496(19) Uani 1 1 d U . . Si3A Si 0.5747(3) 1.0263(2) 0.58352(9) 0.1075(13) Uani 1 1 d . . . Si4A Si 0.4251(3) 0.9537(2) 0.54839(11) 0.1254(15) Uani 1 1 d U . . Si5A Si 0.7362(2) 1.16152(16) 0.50397(8) 0.0855(8) Uani 1 1 d . . . Si6A Si 0.5470(2) 1.16833(19) 0.48455(11) 0.1045(12) Uani 1 1 d . . . O1A O 0.5338(4) 0.9960(5) 0.46102(18) 0.091(2) Uani 1 1 d . . . O2A O 0.7114(4) 0.9958(5) 0.54121(18) 0.092(2) Uani 1 1 d . . . O3A O 0.8938(5) 1.0839(4) 0.3580(2) 0.097(2) Uani 1 1 d . . . O4A O 0.7469(8) 1.0498(4) 0.31884(18) 0.108(2) Uani 1 1 d . . . O5A O 0.6171(5) 1.1480(4) 0.33392(19) 0.091(2) Uani 1 1 d . . . O6A O 0.6892(5) 1.2570(5) 0.3697(3) 0.109(3) Uani 1 1 d . . . O7A O 0.8609(4) 1.2227(5) 0.3624(2) 0.105(3) Uani 1 1 d . . . N1A N 0.6281(6) 0.8784(5) 0.4948(2) 0.092(3) Uani 1 1 d . . . N2A N 0.5278(5) 0.9922(5) 0.5464(2) 0.080(2) Uani 1 1 d . . . N3A N 0.6363(5) 1.1182(4) 0.4995(2) 0.074(2) Uani 1 1 d . . . N4A N 0.7305(5) 0.9944(6) 0.4595(2) 0.078(2) Uani 1 1 d . . . N5A N 0.7312(6) 1.0294(5) 0.4341(3) 0.091(3) Uani 1 1 d . . . N6A N 0.7310(8) 1.0596(6) 0.4083(3) 0.128(4) Uani 1 1 d . . . C1A C 0.5511(8) 0.9431(8) 0.4359(3) 0.097(4) Uani 1 1 d . . . C2A C 0.5432(9) 0.9582(10) 0.4032(4) 0.146(7) Uani 1 1 d . . . H2A H 0.5262 1.0038 0.3965 0.175 Uiso 1 1 calc R . . H2B H 0.5547 0.9233 0.3872 0.175 Uiso 1 1 calc R . . C3A C 0.6723(12) 0.8186(10) 0.4253(5) 0.193(8) Uani 1 1 d U . . H3A H 0.7278 0.8411 0.4296 0.289 Uiso 1 1 calc R . . H3B H 0.6553 0.8272 0.4023 0.289 Uiso 1 1 calc R . . H3C H 0.6774 0.7680 0.4290 0.289 Uiso 1 1 calc R . . C4A C 0.4950(12) 0.7920(9) 0.4563(5) 0.176(7) Uani 1 1 d U . . H4A H 0.5107 0.7526 0.4706 0.263 Uiso 1 1 calc R . . H4B H 0.4826 0.7746 0.4340 0.263 Uiso 1 1 calc R . . H4C H 0.4440 0.8154 0.4652 0.263 Uiso 1 1 calc R . . C5A C 0.6583(16) 0.7267(12) 0.5093(7) 0.254(12) Uani 1 1 d U . . H5A H 0.5983 0.7197 0.5158 0.380 Uiso 1 1 calc R . . H5B H 0.6952 0.6951 0.5220 0.380 Uiso 1 1 calc R . . H5C H 0.6647 0.7168 0.4857 0.380 Uiso 1 1 calc R . . C6A C 0.8081(11) 0.8361(11) 0.5060(6) 0.188(8) Uani 1 1 d U . . H6A H 0.8193 0.8153 0.4843 0.282 Uiso 1 1 calc R . . H6B H 0.8455 0.8142 0.5225 0.282 Uiso 1 1 calc R . . H6C H 0.8199 0.8865 0.5051 0.282 Uiso 1 1 calc R . . C7A C 0.6777(13) 0.8391(10) 0.5634(5) 0.178(7) Uani 1 1 d U . . H7A H 0.6748 0.8898 0.5671 0.268 Uiso 1 1 calc R . . H7B H 0.7268 0.8197 0.5754 0.268 Uiso 1 1 calc R . . H7C H 0.6246 0.8172 0.5713 0.268 Uiso 1 1 calc R . . C8A C 0.6936(9) 1.0244(7) 0.5751(3) 0.106(4) Uani 1 1 d . . . C9A C 0.7546(13) 1.0375(7) 0.5954(3) 0.134(5) Uani 1 1 d . . . H9A H 0.8125 1.0290 0.5892 0.161 Uiso 1 1 calc R . . H9B H 0.7419 1.0556 0.6167 0.161 Uiso 1 1 calc R . . C10A C 0.5401(9) 1.1196(8) 0.5906(4) 0.139(5) Uani 1 1 d U . . H10A H 0.5472 1.1464 0.5701 0.209 Uiso 1 1 calc R . . H10B H 0.5754 1.1405 0.6080 0.209 Uiso 1 1 calc R . . H10C H 0.4796 1.1205 0.5973 0.209 Uiso 1 1 calc R . . C11A C 0.5545(12) 0.9767(9) 0.6237(4) 0.160(6) Uani 1 1 d U . . H11A H 0.4947 0.9833 0.6305 0.240 Uiso 1 1 calc R . . H11B H 0.5929 0.9944 0.6409 0.240 Uiso 1 1 calc R . . H11C H 0.5654 0.9267 0.6202 0.240 Uiso 1 1 calc R . . C12A C 0.3476(11) 1.0073(10) 0.5742(5) 0.177(7) Uani 1 1 d U . . H12A H 0.3729 1.0162 0.5960 0.266 Uiso 1 1 calc R . . H12B H 0.2936 0.9814 0.5769 0.266 Uiso 1 1 calc R . . H12C H 0.3361 1.0520 0.5632 0.266 Uiso 1 1 calc R . . C13A C 0.4313(11) 0.8607(9) 0.5680(4) 0.167(6) Uani 1 1 d U . . H13A H 0.3782 0.8351 0.5632 0.250 Uiso 1 1 calc R . . H13B H 0.4386 0.8649 0.5919 0.250 Uiso 1 1 calc R . . H13C H 0.4802 0.8353 0.5586 0.250 Uiso 1 1 calc R . . C14A C 0.3703(9) 0.9404(9) 0.5058(4) 0.143(6) Uani 1 1 d . . . H14A H 0.3456 0.9848 0.4983 0.215 Uiso 1 1 calc R . . H14B H 0.3246 0.9053 0.5078 0.215 Uiso 1 1 calc R . . H14C H 0.4129 0.9242 0.4897 0.215 Uiso 1 1 calc R . . C15A C 0.7649(10) 1.2194(7) 0.4670(3) 0.126(5) Uani 1 1 d . . . H15A H 0.7860 1.1900 0.4488 0.190 Uiso 1 1 calc R . . H15B H 0.8097 1.2528 0.4734 0.190 Uiso 1 1 calc R . . H15C H 0.7138 1.2451 0.4597 0.190 Uiso 1 1 calc R . . C16A C 0.8341(8) 1.1019(8) 0.5069(5) 0.146(7) Uani 1 1 d . . . H16A H 0.8277 1.0705 0.5259 0.219 Uiso 1 1 calc R . . H16B H 0.8859 1.1304 0.5097 0.219 Uiso 1 1 calc R . . H16C H 0.8390 1.0740 0.4867 0.219 Uiso 1 1 calc R . . C17A C 0.7393(8) 1.2160(6) 0.5428(3) 0.104(4) Uani 1 1 d . . . H17A H 0.6968 1.2537 0.5412 0.156 Uiso 1 1 calc R . . H17B H 0.7967 1.2363 0.5455 0.156 Uiso 1 1 calc R . . H17C H 0.7261 1.1863 0.5619 0.156 Uiso 1 1 calc R . . C18A C 0.5448(9) 1.2612(7) 0.5023(6) 0.166(7) Uani 1 1 d . . . H18A H 0.5394 1.2589 0.5264 0.249 Uiso 1 1 calc R . . H18B H 0.4957 1.2868 0.4931 0.249 Uiso 1 1 calc R . . H18C H 0.5981 1.2855 0.4964 0.249 Uiso 1 1 calc R . . C19A C 0.5462(10) 1.1772(8) 0.4387(4) 0.150(6) Uani 1 1 d . . . H19A H 0.5882 1.2127 0.4321 0.224 Uiso 1 1 calc R . . H19B H 0.4888 1.1913 0.4314 0.224 Uiso 1 1 calc R . . H19C H 0.5613 1.1321 0.4287 0.224 Uiso 1 1 calc R . . C20A C 0.4399(6) 1.1288(6) 0.4966(4) 0.111(4) Uani 1 1 d . . . H20A H 0.4328 1.0835 0.4856 0.167 Uiso 1 1 calc R . . H20B H 0.3934 1.1603 0.4898 0.167 Uiso 1 1 calc R . . H20C H 0.4379 1.1222 0.5206 0.167 Uiso 1 1 calc R . . C21A C 0.8893(10) 1.0274(8) 0.3320(4) 0.128(5) Uani 1 1 d U . . H21A H 0.9317 0.9905 0.3374 0.153 Uiso 1 1 calc R . . H21B H 0.9055 1.0478 0.3104 0.153 Uiso 1 1 calc R . . C22A C 0.8009(11) 0.9940(7) 0.3290(4) 0.129(5) Uani 1 1 d . . . H22A H 0.8012 0.9560 0.3123 0.155 Uiso 1 1 calc R . . H22B H 0.7818 0.9746 0.3504 0.155 Uiso 1 1 calc R . . C23A C 0.6554(11) 1.0298(7) 0.3148(4) 0.127(6) Uani 1 1 d . . . H23A H 0.6339 1.0061 0.3349 0.153 Uiso 1 1 calc R . . H23B H 0.6484 0.9978 0.2958 0.153 Uiso 1 1 calc R . . C24A C 0.6017(9) 1.1051(8) 0.3083(4) 0.122(5) Uani 1 1 d . . . H24A H 0.6212 1.1271 0.2875 0.146 Uiso 1 1 calc R . . H24B H 0.5393 1.0956 0.3065 0.146 Uiso 1 1 calc R . . C25A C 0.5946(8) 1.2187(6) 0.3250(3) 0.094(3) Uani 1 1 d D . . H25A H 0.5350 1.2206 0.3165 0.112 Uiso 1 1 calc R . . H25B H 0.6338 1.2365 0.3077 0.112 Uiso 1 1 calc R . . C26A C 0.6030(8) 1.2622(6) 0.3564(3) 0.107(4) Uani 1 1 d D . . H26A H 0.5897 1.3118 0.3514 0.129 Uiso 1 1 calc R . . H26B H 0.5611 1.2454 0.3730 0.129 Uiso 1 1 calc R . . C27A C 0.7481(8) 1.3056(6) 0.3586(3) 0.098(3) Uani 1 1 d . . . H27A H 0.7296 1.3533 0.3650 0.118 Uiso 1 1 calc R . . H27B H 0.7518 1.3037 0.3342 0.118 Uiso 1 1 calc R . . C28A C 0.8325(9) 1.2902(7) 0.3731(3) 0.099(4) Uani 1 1 d . . . H28A H 0.8745 1.3263 0.3662 0.119 Uiso 1 1 calc R . . H28B H 0.8284 1.2910 0.3975 0.119 Uiso 1 1 calc R . . C29A C 0.9391(7) 1.1972(8) 0.3778(4) 0.115(5) Uani 1 1 d . . . H29A H 0.9288 1.1850 0.4012 0.138 Uiso 1 1 calc R . . H29B H 0.9850 1.2331 0.3767 0.138 Uiso 1 1 calc R . . C30A C 0.9628(8) 1.1350(9) 0.3587(4) 0.128(5) Uani 1 1 d . . . H30A H 0.9771 1.1491 0.3358 0.154 Uiso 1 1 calc R . . H30B H 1.0146 1.1134 0.3686 0.154 Uiso 1 1 calc R . . U2 U 0.752945(19) 0.643958(14) 0.240210(7) 0.04318(8) Uani 1 1 d . . . Na2 Na 0.8786(3) 0.4435(2) 0.10878(9) 0.0790(10) Uani 1 1 d . . . Si1B Si 0.71193(18) 0.75952(17) 0.17910(9) 0.0822(10) Uani 1 1 d . . . Si2B Si 0.85114(18) 0.81311(14) 0.22623(9) 0.0795(9) Uani 1 1 d . . . Si3B Si 0.7505(3) 0.6628(2) 0.32329(7) 0.0978(10) Uani 1 1 d . . . Si4B Si 0.59552(18) 0.73738(17) 0.29290(9) 0.0839(9) Uani 1 1 d . . . Si5B Si 0.84497(18) 0.47413(15) 0.25721(9) 0.0694(8) Uani 1 1 d . . . Si6B Si 0.65033(18) 0.47936(16) 0.24921(7) 0.0656(8) Uani 1 1 d . . . O1B O 0.6446(3) 0.6372(3) 0.20759(14) 0.0558(14) Uani 1 1 d . . . O2B O 0.8653(3) 0.6550(3) 0.27033(14) 0.0607(14) Uani 1 1 d . . . O3B O 1.0246(7) 0.4125(7) 0.0992(3) 0.158(4) Uani 1 1 d U . . O4B O 0.9295(10) 0.5192(8) 0.0666(3) 0.176(5) Uani 1 1 d . . . O5B O 0.7555(9) 0.4789(7) 0.0750(3) 0.157(4) Uani 1 1 d U . . O6B O 0.7424(8) 0.3811(6) 0.1246(3) 0.145(4) Uani 1 1 d . . . O7B O 0.8965(8) 0.3176(5) 0.1160(3) 0.130(3) Uani 1 1 d . . . N1B N 0.7671(5) 0.7531(3) 0.21646(19) 0.0622(19) Uani 1 1 d . . . N2B N 0.6874(4) 0.6838(4) 0.28898(19) 0.065(2) Uani 1 1 d . . . N3B N 0.7486(5) 0.5253(3) 0.25187(14) 0.0522(16) Uani 1 1 d . . . N4B N 0.8387(5) 0.6112(4) 0.19304(19) 0.0578(19) Uani 1 1 d . . . N5B N 0.8434(5) 0.5661(5) 0.1726(2) 0.067(2) Uani 1 1 d . . . N6B N 0.8514(6) 0.5219(5) 0.1524(3) 0.107(3) Uani 1 1 d U . . C1B C 0.6496(6) 0.6732(5) 0.1769(2) 0.066(2) Uani 1 1 d . . . C2B C 0.6105(7) 0.6452(7) 0.1499(3) 0.092(3) Uani 1 1 d . . . H2C H 0.5805 0.6021 0.1516 0.111 Uiso 1 1 calc R . . H2D H 0.6134 0.6688 0.1292 0.111 Uiso 1 1 calc R . . C3B C 0.6317(8) 0.8362(6) 0.1771(4) 0.119(4) Uani 1 1 d U . . H3D H 0.6032 0.8414 0.1986 0.178 Uiso 1 1 calc R . . H3E H 0.5887 0.8267 0.1600 0.178 Uiso 1 1 calc R . . H3F H 0.6625 0.8795 0.1717 0.178 Uiso 1 1 calc R . . C4B C 0.7837(8) 0.7649(7) 0.1414(3) 0.115(4) Uani 1 1 d U . . H4D H 0.7824 0.8126 0.1325 0.173 Uiso 1 1 calc R . . H4E H 0.7632 0.7320 0.1246 0.173 Uiso 1 1 calc R . . H4F H 0.8427 0.7528 0.1477 0.173 Uiso 1 1 calc R . . C5B C 0.8287(9) 0.9029(7) 0.2064(4) 0.130(5) Uani 1 1 d U . . H5D H 0.8268 0.8979 0.1823 0.196 Uiso 1 1 calc R . . H5E H 0.8744 0.9358 0.2124 0.196 Uiso 1 1 calc R . . H5F H 0.7734 0.9208 0.2143 0.196 Uiso 1 1 calc R . . C6B C 0.9567(7) 0.7804(7) 0.2077(3) 0.103(4) Uani 1 1 d . . . H6D H 0.9686 0.7330 0.2159 0.155 Uiso 1 1 calc R . . H6E H 1.0034 0.8118 0.2142 0.155 Uiso 1 1 calc R . . H6F H 0.9520 0.7794 0.1836 0.155 Uiso 1 1 calc R . . C7B C 0.8704(7) 0.8258(6) 0.2723(4) 0.113(5) Uani 1 1 d . . . H7D H 0.8174 0.8424 0.2828 0.169 Uiso 1 1 calc R . . H7E H 0.9160 0.8604 0.2756 0.169 Uiso 1 1 calc R . . H7F H 0.8875 0.7811 0.2822 0.169 Uiso 1 1 calc R . . C8B C 0.8634(7) 0.6498(6) 0.3052(2) 0.080(3) Uani 1 1 d . . . C9B C 0.9360(7) 0.6452(7) 0.3225(3) 0.102(4) Uani 1 1 d . . . H9C H 0.9898 0.6454 0.3114 0.123 Uiso 1 1 calc R . . H9D H 0.9340 0.6418 0.3459 0.123 Uiso 1 1 calc R . . C10B C 0.7170(8) 0.5780(7) 0.3436(3) 0.120(4) Uani 1 1 d U . . H10D H 0.6648 0.5858 0.3566 0.180 Uiso 1 1 calc R . . H10E H 0.7631 0.5616 0.3581 0.180 Uiso 1 1 calc R . . H10F H 0.7057 0.5427 0.3266 0.180 Uiso 1 1 calc R . . C11B C 0.7642(10) 0.7376(8) 0.3553(4) 0.137(5) Uani 1 1 d U . . H11D H 0.7660 0.7827 0.3438 0.205 Uiso 1 1 calc R . . H11E H 0.8179 0.7307 0.3675 0.205 Uiso 1 1 calc R . . H11F H 0.7158 0.7370 0.3707 0.205 Uiso 1 1 calc R . . C12B C 0.5267(8) 0.7105(10) 0.3306(4) 0.145(6) Uani 1 1 d . . . H12D H 0.4847 0.6750 0.3239 0.218 Uiso 1 1 calc R . . H12E H 0.4964 0.7517 0.3392 0.218 Uiso 1 1 calc R . . H12F H 0.5639 0.6913 0.3479 0.218 Uiso 1 1 calc R . . C13B C 0.5215(7) 0.7338(6) 0.2566(3) 0.099(4) Uani 1 1 d . . . H13D H 0.5544 0.7231 0.2366 0.148 Uiso 1 1 calc R . . H13E H 0.4929 0.7792 0.2540 0.148 Uiso 1 1 calc R . . H13F H 0.4782 0.6973 0.2602 0.148 Uiso 1 1 calc R . . C14B C 0.6248(9) 0.8346(7) 0.2951(4) 0.132(5) Uani 1 1 d U . . H14D H 0.6607 0.8430 0.3146 0.197 Uiso 1 1 calc R . . H14E H 0.5722 0.8626 0.2968 0.197 Uiso 1 1 calc R . . H14F H 0.6564 0.8479 0.2752 0.197 Uiso 1 1 calc R . . C15B C 0.8423(8) 0.3939(6) 0.2280(3) 0.104(4) Uani 1 1 d . . . H15D H 0.7934 0.3640 0.2337 0.156 Uiso 1 1 calc R . . H15E H 0.8957 0.3672 0.2304 0.156 Uiso 1 1 calc R . . H15F H 0.8365 0.4099 0.2051 0.156 Uiso 1 1 calc R . . C16B C 0.8559(8) 0.4437(6) 0.3023(3) 0.102(4) Uani 1 1 d . . . H16D H 0.8546 0.4845 0.3170 0.152 Uiso 1 1 calc R . . H16E H 0.9105 0.4188 0.3051 0.152 Uiso 1 1 calc R . . H16F H 0.8083 0.4123 0.3078 0.152 Uiso 1 1 calc R . . C17B C 0.9518(6) 0.5166(6) 0.2459(3) 0.089(4) Uani 1 1 d . . . H17D H 0.9492 0.5340 0.2231 0.134 Uiso 1 1 calc R . . H17E H 0.9980 0.4819 0.2478 0.134 Uiso 1 1 calc R . . H17F H 0.9633 0.5557 0.2609 0.134 Uiso 1 1 calc R . . C18B C 0.6446(7) 0.4004(6) 0.2788(3) 0.102(4) Uani 1 1 d . . . H18D H 0.6929 0.3688 0.2745 0.154 Uiso 1 1 calc R . . H18E H 0.5904 0.3752 0.2753 0.154 Uiso 1 1 calc R . . H18F H 0.6475 0.4169 0.3017 0.154 Uiso 1 1 calc R . . C19B C 0.6287(8) 0.4511(6) 0.2055(3) 0.098(4) Uani 1 1 d . . . H19D H 0.6246 0.4925 0.1913 0.147 Uiso 1 1 calc R . . H19E H 0.5746 0.4250 0.2047 0.147 Uiso 1 1 calc R . . H19F H 0.6757 0.4211 0.1978 0.147 Uiso 1 1 calc R . . C20B C 0.5560(5) 0.5345(5) 0.2631(3) 0.075(3) Uani 1 1 d . . . H20D H 0.5656 0.5505 0.2858 0.113 Uiso 1 1 calc R . . H20E H 0.5034 0.5065 0.2622 0.113 Uiso 1 1 calc R . . H20F H 0.5502 0.5752 0.2485 0.113 Uiso 1 1 calc R . . C21B C 1.0681(11) 0.4503(10) 0.0761(5) 0.160(7) Uani 1 1 d DU . . H21C H 1.1086 0.4200 0.0638 0.191 Uiso 1 1 calc R . . H21D H 1.1006 0.4889 0.0866 0.191 Uiso 1 1 calc R . . C22B C 0.9989(13) 0.4791(11) 0.0531(5) 0.170(7) Uani 1 1 d DU . . H22C H 1.0280 0.5088 0.0364 0.204 Uiso 1 1 calc R . . H22D H 0.9736 0.4389 0.0411 0.204 Uiso 1 1 calc R . . C23B C 0.8658(12) 0.5365(10) 0.0449(5) 0.161(6) Uani 1 1 d DU . . H23C H 0.8586 0.4984 0.0285 0.194 Uiso 1 1 calc R . . H23D H 0.8817 0.5797 0.0329 0.194 Uiso 1 1 calc R . . C24B C 0.7806(12) 0.5480(10) 0.0635(5) 0.178(8) Uani 1 1 d DU . . H24C H 0.7889 0.5803 0.0824 0.214 Uiso 1 1 calc R . . H24D H 0.7364 0.5679 0.0486 0.214 Uiso 1 1 calc R . . C25B C 0.6841(14) 0.4757(13) 0.0939(6) 0.193(8) Uani 1 1 d U . . H25C H 0.6334 0.4888 0.0805 0.231 Uiso 1 1 calc R . . H25D H 0.6890 0.5094 0.1124 0.231 Uiso 1 1 calc R . . C26B C 0.6718(13) 0.3983(11) 0.1082(5) 0.162(7) Uani 1 1 d U . . H26C H 0.6215 0.3968 0.1232 0.194 Uiso 1 1 calc R . . H26D H 0.6620 0.3648 0.0899 0.194 Uiso 1 1 calc R . . C27B C 0.7494(13) 0.3128(9) 0.1283(4) 0.137(5) Uani 1 1 d U . . H27C H 0.7350 0.2890 0.1073 0.164 Uiso 1 1 calc R . . H27D H 0.7087 0.2965 0.1455 0.164 Uiso 1 1 calc R . . C28B C 0.8454(12) 0.2939(9) 0.1389(4) 0.138(5) Uani 1 1 d U . . H28C H 0.8592 0.3159 0.1604 0.166 Uiso 1 1 calc R . . H28D H 0.8519 0.2426 0.1411 0.166 Uiso 1 1 calc R . . C29B C 0.9895(11) 0.3077(9) 0.1224(5) 0.149(6) Uani 1 1 d U . . H29C H 1.0029 0.2571 0.1237 0.179 Uiso 1 1 calc R . . H29D H 1.0053 0.3296 0.1437 0.179 Uiso 1 1 calc R . . C30B C 1.0395(10) 0.3405(9) 0.0950(5) 0.147(6) Uani 1 1 d U . . H30C H 1.1014 0.3295 0.0969 0.176 Uiso 1 1 calc R . . H30D H 1.0184 0.3244 0.0732 0.176 Uiso 1 1 calc R . . C1 C 0.824(2) 0.2009(14) 0.2689(7) 0.216(12) Uani 0.50 1 d PDU . . H1A H 0.8189 0.1606 0.2838 0.324 Uiso 0.50 1 d PR . . H1B H 0.7709 0.2289 0.2702 0.324 Uiso 0.50 1 d PR . . H1C H 0.8728 0.2297 0.2754 0.324 Uiso 0.50 1 d PR . . C2 C 0.8353(17) 0.1728(16) 0.2339(8) 0.225(12) Uani 0.50 1 d PDU . . H2E H 0.8917 0.1491 0.2321 0.270 Uiso 0.50 1 d PR . . H2F H 0.8354 0.2133 0.2186 0.270 Uiso 0.50 1 d PR . . C3 C 0.7586(19) 0.1286(14) 0.2235(7) 0.223(12) Uani 0.50 1 d PDU . . H3G H 0.7774 0.0800 0.2281 0.268 Uiso 0.50 1 d PR . . H3H H 0.7066 0.1380 0.2369 0.268 Uiso 0.50 1 d PR . . C4 C 0.751(2) 0.1257(16) 0.1859(7) 0.229(12) Uani 0.50 1 d PDU . . H4G H 0.8036 0.1208 0.1725 0.275 Uiso 0.50 1 d PR . . H4H H 0.7260 0.1726 0.1816 0.275 Uiso 0.50 1 d PR . . C5 C 0.677(2) 0.0752(16) 0.1767(8) 0.223(13) Uani 0.50 1 d PDU . . H5G H 0.6286 0.0969 0.1654 0.335 Uiso 0.50 1 d PR . . H5H H 0.6572 0.0509 0.1965 0.335 Uiso 0.50 1 d PR . . H5I H 0.7052 0.0415 0.1618 0.335 Uiso 0.50 1 d PR . . C6 C 0.923(3) 0.8882(17) 0.5907(12) 0.291(19) Uani 0.50 1 d PDU . . H6G H 0.8838 0.9279 0.5888 0.436 Uiso 0.50 1 d PR . . H6H H 0.9334 0.8778 0.6141 0.436 Uiso 0.50 1 d PR . . H6I H 0.8985 0.8472 0.5798 0.436 Uiso 0.50 1 d PR . . C7 C 1.010(3) 0.9070(15) 0.5736(10) 0.290(19) Uani 0.50 1 d PDU . . H7G H 1.0547 0.8723 0.5796 0.347 Uiso 0.50 1 d PR . . H7H H 1.0035 0.9075 0.5493 0.347 Uiso 0.50 1 d PR . . C8 C 1.035(3) 0.9806(18) 0.5864(8) 0.288(19) Uani 0.50 1 d PDU . . H8A H 0.9841 1.0050 0.5951 0.346 Uiso 0.50 1 d PR . . H8B H 1.0782 0.9766 0.6044 0.346 Uiso 0.50 1 d PR . . C9 C 1.074(3) 1.0214(19) 0.5570(9) 0.289(19) Uani 0.50 1 d PDU . . H9E H 1.1227 0.9951 0.5471 0.347 Uiso 0.50 1 d PR . . H9F H 1.0301 1.0289 0.5398 0.347 Uiso 0.50 1 d PR . . C10 C 1.105(3) 1.0928(16) 0.5706(12) 0.289(19) Uani 0.50 1 d PDU . . H10G H 1.0732 1.1045 0.5906 0.433 Uiso 0.50 1 d PR . . H10H H 1.0967 1.1293 0.5540 0.433 Uiso 0.50 1 d PR . . H10I H 1.1668 1.0894 0.5759 0.433 Uiso 0.50 1 d 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 0.06253(19) 0.0690(2) 0.04701(17) 0.0000(2) 0.01019(14) 0.00084(17) Na1 0.0683(18) 0.078(2) 0.0649(19) 0.0074(16) -0.001(2) -0.010(2) Si1A 0.122(3) 0.112(3) 0.136(3) -0.059(3) 0.029(2) -0.021(3) Si2A 0.225(5) 0.072(2) 0.151(4) 0.011(3) 0.042(4) 0.030(3) Si3A 0.124(3) 0.124(3) 0.075(2) -0.029(2) 0.042(2) -0.027(2) Si4A 0.134(3) 0.131(3) 0.112(3) -0.032(2) 0.057(3) -0.056(3) Si5A 0.0866(19) 0.095(2) 0.0744(18) -0.0018(15) 0.0045(18) -0.0145(17) Si6A 0.098(2) 0.089(3) 0.126(3) 0.014(2) -0.008(2) 0.0290(18) O1A 0.086(5) 0.102(6) 0.087(5) 0.008(5) 0.006(4) -0.005(5) O2A 0.090(5) 0.106(6) 0.081(5) 0.004(5) -0.012(3) 0.021(5) O3A 0.107(6) 0.081(5) 0.104(6) 0.019(4) 0.040(5) 0.022(5) O4A 0.157(7) 0.076(5) 0.092(5) 0.001(4) 0.023(7) -0.031(7) O5A 0.087(5) 0.093(5) 0.092(5) -0.011(5) -0.011(4) -0.012(5) O6A 0.066(5) 0.119(7) 0.142(8) 0.025(6) -0.034(5) -0.010(5) O7A 0.062(5) 0.097(6) 0.156(8) 0.007(6) -0.005(5) -0.015(4) N1A 0.112(6) 0.084(6) 0.079(6) -0.018(5) 0.022(6) -0.007(5) N2A 0.099(6) 0.071(6) 0.070(5) -0.010(5) 0.027(4) -0.019(5) N3A 0.083(5) 0.065(5) 0.075(5) 0.005(5) 0.021(6) 0.001(4) N4A 0.079(6) 0.099(6) 0.058(5) -0.006(5) 0.018(4) 0.005(5) N5A 0.088(7) 0.100(7) 0.084(7) -0.004(5) 0.030(6) -0.007(5) N6A 0.146(11) 0.155(10) 0.082(7) 0.044(7) 0.050(7) 0.006(8) C1A 0.086(8) 0.123(11) 0.082(9) -0.023(8) 0.000(6) 0.012(7) C2A 0.136(12) 0.218(19) 0.083(10) 0.006(10) -0.011(9) -0.066(12) C3A 0.206(11) 0.199(11) 0.173(11) -0.047(9) 0.010(9) 0.012(9) C4A 0.178(10) 0.155(10) 0.194(11) -0.023(8) -0.010(9) -0.030(8) C5A 0.282(14) 0.224(14) 0.255(15) -0.008(10) 0.005(10) -0.014(9) C6A 0.177(10) 0.196(11) 0.190(12) 0.016(9) -0.030(9) 0.017(8) C7A 0.213(11) 0.156(10) 0.166(11) 0.030(8) -0.006(9) 0.027(8) C8A 0.129(10) 0.133(12) 0.056(7) 0.021(7) -0.003(7) 0.008(8) C9A 0.183(14) 0.148(12) 0.071(8) -0.008(7) -0.030(12) -0.018(13) C10A 0.130(8) 0.139(9) 0.149(9) -0.050(7) 0.001(7) 0.008(7) C11A 0.183(10) 0.167(10) 0.129(9) 0.000(8) 0.024(8) -0.023(8) C12A 0.155(9) 0.188(10) 0.187(10) -0.024(9) 0.045(8) -0.029(8) C13A 0.192(10) 0.165(10) 0.142(9) 0.014(8) 0.013(8) -0.056(8) C14A 0.142(12) 0.182(15) 0.106(11) 0.009(10) 0.006(10) -0.066(11) C15A 0.140(12) 0.145(12) 0.094(9) 0.020(8) -0.010(9) -0.053(11) C16A 0.101(9) 0.187(16) 0.150(16) -0.054(13) 0.008(10) -0.039(10) C17A 0.093(8) 0.118(9) 0.101(8) -0.017(7) -0.008(8) -0.005(8) C18A 0.136(12) 0.107(11) 0.25(2) 0.000(14) -0.001(15) 0.054(9) C19A 0.187(15) 0.126(12) 0.135(13) 0.025(10) -0.071(12) 0.032(11) C20A 0.072(6) 0.081(8) 0.181(14) -0.006(9) -0.007(8) 0.019(6) C21A 0.130(8) 0.126(8) 0.127(8) 0.016(7) 0.029(7) 0.042(7) C22A 0.210(17) 0.057(8) 0.120(10) 0.003(8) 0.032(10) 0.027(9) C23A 0.181(15) 0.081(9) 0.121(11) -0.033(8) 0.058(10) -0.071(10) C24A 0.104(10) 0.128(13) 0.135(13) -0.006(10) 0.007(9) -0.041(9) C25A 0.110(9) 0.066(8) 0.104(10) 0.006(7) -0.017(7) 0.000(6) C26A 0.106(9) 0.091(9) 0.125(11) 0.030(8) -0.019(8) 0.007(7) C27A 0.066(6) 0.101(8) 0.128(10) 0.026(7) -0.010(8) -0.011(8) C28A 0.126(10) 0.083(9) 0.088(9) 0.012(7) -0.010(8) -0.011(8) C29A 0.055(7) 0.149(13) 0.140(13) 0.026(10) -0.020(7) 0.003(8) C30A 0.073(8) 0.138(13) 0.174(15) 0.030(12) 0.027(9) 0.026(9) U2 0.04686(14) 0.04129(14) 0.04141(14) 0.00016(12) -0.00244(17) -0.00073(17) Na2 0.086(2) 0.090(3) 0.061(2) -0.0216(19) -0.003(2) 0.013(2) Si1B 0.0684(16) 0.086(2) 0.092(2) 0.0482(17) -0.0195(15) -0.0146(14) Si2B 0.0672(16) 0.0517(16) 0.120(3) 0.0096(15) -0.0092(16) -0.0140(13) Si3B 0.0864(18) 0.158(3) 0.0489(14) -0.0179(16) -0.0037(18) 0.003(3) Si4B 0.0605(16) 0.089(2) 0.102(2) -0.0372(18) 0.0160(15) 0.0047(14) Si5B 0.0642(16) 0.0494(16) 0.095(2) 0.0125(14) 0.0036(15) 0.0087(12) Si6B 0.0630(16) 0.0535(17) 0.080(2) 0.0122(11) -0.0008(12) -0.0122(13) O1B 0.057(3) 0.056(4) 0.054(3) 0.006(3) -0.005(3) -0.014(3) O2B 0.060(3) 0.065(4) 0.057(4) -0.002(3) -0.010(3) 0.007(3) O3B 0.143(7) 0.159(8) 0.172(8) -0.048(7) 0.001(6) -0.004(6) O4B 0.198(12) 0.194(13) 0.136(10) 0.037(9) -0.002(9) -0.003(10) O5B 0.144(7) 0.183(8) 0.143(7) -0.040(6) -0.005(7) 0.013(7) O6B 0.124(7) 0.152(9) 0.161(9) -0.058(7) 0.039(8) -0.025(8) O7B 0.168(9) 0.094(6) 0.128(8) -0.025(6) 0.016(7) -0.032(6) N1B 0.070(5) 0.037(3) 0.079(5) 0.005(3) -0.015(4) -0.005(3) N2B 0.056(4) 0.077(5) 0.061(5) -0.014(4) 0.000(4) 0.009(4) N3B 0.053(3) 0.041(4) 0.062(4) 0.008(2) 0.007(4) 0.015(4) N4B 0.068(5) 0.054(5) 0.051(5) 0.001(4) -0.001(4) -0.005(4) N5B 0.067(5) 0.079(6) 0.056(5) -0.019(5) 0.013(4) -0.023(4) N6B 0.107(6) 0.113(7) 0.101(6) -0.046(5) 0.023(5) -0.028(5) C1B 0.059(5) 0.092(7) 0.046(5) 0.005(5) -0.003(4) 0.009(5) C2B 0.106(8) 0.111(8) 0.061(6) 0.022(6) -0.018(6) -0.007(7) C3B 0.118(7) 0.092(7) 0.146(8) 0.046(6) -0.018(7) 0.017(6) C4B 0.095(7) 0.138(8) 0.113(8) 0.043(7) 0.005(6) -0.027(6) C5B 0.136(8) 0.085(7) 0.170(9) 0.021(7) -0.030(7) -0.019(6) C6B 0.080(7) 0.115(10) 0.115(10) -0.012(8) 0.012(7) -0.038(7) C7B 0.081(7) 0.106(9) 0.152(13) -0.063(9) 0.007(8) -0.009(7) C8B 0.078(6) 0.107(8) 0.055(6) -0.003(6) -0.010(5) 0.008(6) C9B 0.072(7) 0.152(11) 0.082(8) 0.006(8) -0.020(6) 0.015(8) C10B 0.116(8) 0.157(9) 0.087(7) 0.037(7) 0.008(6) 0.003(7) C11B 0.117(8) 0.179(9) 0.114(8) -0.051(7) 0.001(7) 0.013(7) C12B 0.083(8) 0.231(18) 0.122(12) -0.004(12) 0.044(8) 0.039(10) C13B 0.073(7) 0.086(8) 0.137(11) -0.022(7) -0.014(7) 0.014(6) C14B 0.120(8) 0.104(8) 0.171(9) -0.030(7) 0.007(7) 0.013(7) C15B 0.108(9) 0.076(8) 0.129(11) -0.014(7) 0.000(8) 0.034(6) C16B 0.100(8) 0.075(8) 0.129(11) 0.051(7) -0.032(7) -0.004(6) C17B 0.072(6) 0.066(7) 0.130(10) 0.024(6) 0.010(6) 0.021(5) C18B 0.085(8) 0.075(8) 0.147(12) 0.045(8) 0.009(8) -0.006(6) C19B 0.116(9) 0.075(7) 0.103(9) -0.015(6) -0.012(8) -0.031(7) C20B 0.048(5) 0.079(7) 0.099(8) 0.024(6) 0.004(5) -0.015(4) C21B 0.153(10) 0.172(10) 0.153(10) -0.008(8) 0.048(8) -0.028(8) C22B 0.164(10) 0.183(11) 0.163(10) -0.024(9) 0.030(9) -0.002(9) C23B 0.171(10) 0.143(9) 0.170(10) 0.021(8) -0.014(9) 0.007(8) C24B 0.185(11) 0.165(10) 0.185(11) 0.016(9) -0.013(9) 0.000(8) C25B 0.169(11) 0.209(12) 0.201(12) -0.026(9) 0.001(9) 0.004(9) C26B 0.142(9) 0.185(11) 0.158(10) -0.008(8) -0.010(8) 0.008(8) C27B 0.152(9) 0.126(8) 0.132(8) -0.028(7) 0.034(8) -0.007(9) C28B 0.162(9) 0.135(9) 0.116(9) -0.011(7) 0.019(8) -0.002(8) C29B 0.139(9) 0.153(10) 0.156(10) 0.006(8) -0.016(8) 0.017(8) C30B 0.139(9) 0.145(9) 0.157(10) -0.010(8) 0.005(8) 0.040(7) C1 0.23(2) 0.102(14) 0.32(3) 0.101(16) 0.19(2) 0.017(12) C2 0.24(2) 0.111(14) 0.32(3) 0.093(16) 0.19(2) 0.032(11) C3 0.24(2) 0.114(14) 0.32(3) 0.093(16) 0.19(2) 0.033(11) C4 0.24(2) 0.117(14) 0.33(3) 0.093(16) 0.18(2) 0.034(12) C5 0.23(2) 0.114(15) 0.32(3) 0.092(16) 0.18(2) 0.044(12) C6 0.31(3) 0.19(2) 0.37(4) -0.07(2) -0.21(3) 0.10(3) C7 0.31(3) 0.19(2) 0.37(4) -0.07(2) -0.21(3) 0.10(3) C8 0.31(3) 0.19(2) 0.37(4) -0.07(2) -0.22(3) 0.10(3) C9 0.31(3) 0.19(2) 0.37(4) -0.07(2) -0.21(3) 0.10(3) C10 0.31(3) 0.19(2) 0.37(4) -0.07(2) -0.22(3) 0.09(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 O2A 2.059(6) . ? U1 O1A 2.119(7) . ? U1 N1A 2.250(8) . ? U1 N2A 2.267(7) . ? U1 N3A 2.268(7) . ? U1 N4A 2.369(7) . ? Na1 N6A 2.299(11) . ? Na1 O7A 2.333(8) . ? Na1 O5A 2.361(8) . ? Na1 O4A 2.408(8) . ? Na1 O3A 2.409(8) . ? Na1 O6A 2.452(10) . ? Si1A N1A 1.765(10) . ? Si1A C4A 1.857(17) . ? Si1A C1A 1.862(15) . ? Si1A C3A 1.875(18) . ? Si2A N1A 1.700(11) . ? Si2A C7A 1.847(19) . ? Si2A C5A 1.87(2) . ? Si2A C6A 1.873(18) . ? Si3A N2A 1.756(9) . ? Si3A C8A 1.845(14) . ? Si3A C10A 1.845(14) . ? Si3A C11A 1.869(16) . ? Si4A N2A 1.726(9) . ? Si4A C12A 1.859(17) . ? Si4A C14A 1.902(15) . ? Si4A C13A 1.908(17) . ? Si5A N3A 1.736(8) . ? Si5A C17A 1.847(11) . ? Si5A C16A 1.868(15) . ? Si5A C15A 1.875(12) . ? Si6A N3A 1.757(9) . ? Si6A C19A 1.824(16) . ? Si6A C20A 1.856(11) . ? Si6A C18A 1.875(15) . ? O1A C1A 1.430(14) . ? O2A C8A 1.471(14) . ? O3A C30A 1.423(15) . ? O3A C21A 1.478(17) . ? O4A C22A 1.389(15) . ? O4A C23A 1.453(16) . ? O5A C24A 1.317(15) . ? O5A C25A 1.411(12) . ? O6A C27A 1.353(12) . ? O6A C26A 1.420(13) . ? O7A C28A 1.401(14) . ? O7A C29A 1.421(12) . ? N4A N5A 1.204(12) . ? N5A N6A 1.167(13) . ? C1A C2A 1.330(18) . ? C2A H2A 0.9300 . ? C2A H2B 0.9300 . ? C3A H3A 0.9600 . ? C3A H3B 0.9600 . ? C3A H3C 0.9600 . ? C4A H4A 0.9600 . ? C4A H4B 0.9600 . ? C4A H4C 0.9600 . ? C5A H5A 0.9600 . ? C5A H5B 0.9600 . ? C5A H5C 0.9600 . ? C6A H6A 0.9600 . ? C6A H6B 0.9600 . ? C6A H6C 0.9600 . ? C7A H7A 0.9600 . ? C7A H7B 0.9600 . ? C7A H7C 0.9600 . ? C8A C9A 1.255(18) . ? C9A H9A 0.9300 . ? C9A H9B 0.9300 . ? C10A H10A 0.9600 . ? C10A H10B 0.9600 . ? C10A H10C 0.9600 . ? C11A H11A 0.9600 . ? C11A H11B 0.9600 . ? C11A H11C 0.9600 . ? C12A H12A 0.9600 . ? C12A H12B 0.9600 . ? C12A H12C 0.9600 . ? C13A H13A 0.9600 . ? C13A H13B 0.9600 . ? C13A H13C 0.9600 . ? C14A H14A 0.9600 . ? C14A H14B 0.9600 . ? C14A H14C 0.9600 . ? C15A H15A 0.9600 . ? C15A H15B 0.9600 . ? C15A H15C 0.9600 . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C17A H17A 0.9600 . ? C17A H17B 0.9600 . ? C17A H17C 0.9600 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C19A H19A 0.9600 . ? C19A H19B 0.9600 . ? C19A H19C 0.9600 . ? C20A H20A 0.9600 . ? C20A H20B 0.9600 . ? C20A H20C 0.9600 . ? C21A C22A 1.491(19) . ? C21A H21A 0.9700 . ? C21A H21B 0.9700 . ? C22A H22A 0.9700 . ? C22A H22B 0.9700 . ? C23A C24A 1.649(19) . ? C23A H23A 0.9700 . ? C23A H23B 0.9700 . ? C24A H24A 0.9700 . ? C24A H24B 0.9700 . ? C25A C26A 1.494(9) . ? C25A H25A 0.9700 . ? C25A H25B 0.9700 . ? C26A H26A 0.9700 . ? C26A H26B 0.9700 . ? C27A C28A 1.440(15) . ? C27A H27A 0.9700 . ? C27A H27B 0.9700 . ? C28A H28A 0.9700 . ? C28A H28B 0.9700 . ? C29A C30A 1.434(19) . ? C29A H29A 0.9700 . ? C29A H29B 0.9700 . ? C30A H30A 0.9700 . ? C30A H30B 0.9700 . ? U2 O2B 2.099(5) . ? U2 O1B 2.102(5) . ? U2 N1B 2.258(6) . ? U2 N3B 2.269(6) . ? U2 N2B 2.301(7) . ? U2 N4B 2.363(8) . ? Na2 N6B 2.306(10) . ? Na2 O4B 2.324(13) . ? Na2 O3B 2.332(12) . ? Na2 O7B 2.388(10) . ? Na2 O5B 2.401(13) . ? Na2 O6B 2.464(11) . ? Si1B N1B 1.708(8) . ? Si1B C4B 1.855(13) . ? Si1B C1B 1.876(10) . ? Si1B C3B 1.887(11) . ? Si2B N1B 1.748(7) . ? Si2B C7B 1.865(14) . ? Si2B C6B 1.872(12) . ? Si2B C5B 1.887(13) . ? Si3B N2B 1.711(8) . ? Si3B C10B 1.851(13) . ? Si3B C8B 1.881(11) . ? Si3B C11B 1.900(13) . ? Si4B N2B 1.731(7) . ? Si4B C13B 1.830(12) . ? Si4B C14B 1.874(13) . ? Si4B C12B 1.895(13) . ? Si5B N3B 1.767(7) . ? Si5B C17B 1.868(10) . ? Si5B C16B 1.883(12) . ? Si5B C15B 1.896(12) . ? Si6B N3B 1.730(8) . ? Si6B C19B 1.841(11) . ? Si6B C20B 1.854(10) . ? Si6B C18B 1.889(10) . ? O1B C1B 1.391(10) . ? O2B C8B 1.387(11) . ? O3B C21B 1.335(18) . ? O3B C30B 1.375(17) . ? O4B C23B 1.338(19) . ? O4B C22B 1.404(19) . ? O5B C25B 1.32(2) . ? O5B C24B 1.423(18) . ? O6B C27B 1.290(16) . ? O6B C26B 1.297(18) . ? O7B C28B 1.277(17) . ? O7B C29B 1.453(17) . ? N4B N5B 1.174(10) . ? N5B N6B 1.155(11) . ? C1B C2B 1.335(13) . ? C2B H2C 0.9300 . ? C2B H2D 0.9300 . ? C3B H3D 0.9600 . ? C3B H3E 0.9600 . ? C3B H3F 0.9600 . ? C4B H4D 0.9600 . ? C4B H4E 0.9600 . ? C4B H4F 0.9600 . ? C5B H5D 0.9600 . ? C5B H5E 0.9600 . ? C5B H5F 0.9600 . ? C6B H6D 0.9600 . ? C6B H6E 0.9600 . ? C6B H6F 0.9600 . ? C7B H7D 0.9600 . ? C7B H7E 0.9600 . ? C7B H7F 0.9600 . ? C8B C9B 1.306(13) . ? C9B H9C 0.9300 . ? C9B H9D 0.9300 . ? C10B H10D 0.9600 . ? C10B H10E 0.9600 . ? C10B H10F 0.9600 . ? C11B H11D 0.9600 . ? C11B H11E 0.9600 . ? C11B H11F 0.9600 . ? C12B H12D 0.9600 . ? C12B H12E 0.9600 . ? C12B H12F 0.9600 . ? C13B H13D 0.9600 . ? C13B H13E 0.9600 . ? C13B H13F 0.9600 . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 0.9600 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C17B H17D 0.9600 . ? C17B H17E 0.9600 . ? C17B H17F 0.9600 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? C20B H20D 0.9600 . ? C20B H20E 0.9600 . ? C20B H20F 0.9600 . ? C21B C22B 1.50(3) . ? C21B H21C 0.9700 . ? C21B H21D 0.9700 . ? C22B H22C 0.9700 . ? C22B H22D 0.9700 . ? C23B C24B 1.51(3) . ? C23B H23C 0.9700 . ? C23B H23D 0.9700 . ? C24B H24C 0.9700 . ? C24B H24D 0.9700 . ? C25B C26B 1.57(3) . ? C25B H25C 0.9700 . ? C25B H25D 0.9700 . ? C26B H26C 0.9700 . ? C26B H26D 0.9700 . ? C27B C28B 1.56(2) . ? C27B H27C 0.9700 . ? C27B H27D 0.9700 . ? C28B H28C 0.9700 . ? C28B H28D 0.9700 . ? C29B C30B 1.46(2) . ? C29B H29C 0.9700 . ? C29B H29D 0.9700 . ? C30B H30C 0.9700 . ? C30B H30D 0.9700 . ? C1 C2 1.494(10) . ? C1 H1A 0.9597 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.492(10) . ? C2 H2E 0.9700 . ? C2 H2F 0.9701 . ? C3 C4 1.497(10) . ? C3 H3G 0.9700 . ? C3 H3H 0.9699 . ? C4 C5 1.508(10) . ? C4 H4G 0.9701 . ? C4 H4H 0.9700 . ? C5 H5G 0.9500 . ? C5 H5H 0.9600 . ? C5 H5I 0.9602 . ? C6 C7 1.523(10) . ? C6 H6G 0.9601 . ? C6 H6H 0.9597 . ? C6 H6I 0.9600 . ? C7 C8 1.518(10) . ? C7 H7G 0.9701 . ? C7 H7H 0.9698 . ? C8 C9 1.515(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9699 . ? C9 C10 1.516(10) . ? C9 H9E 0.9698 . ? C9 H9F 0.9699 . ? C10 H10G 0.9598 . ? C10 H10H 0.9600 . ? C10 H10I 0.9601 . ? 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 O2A U1 O1A 177.4(3) . . ? O2A U1 N1A 93.2(4) . . ? O1A U1 N1A 84.9(4) . . ? O2A U1 N2A 80.8(3) . . ? O1A U1 N2A 101.1(3) . . ? N1A U1 N2A 94.9(3) . . ? O2A U1 N3A 89.4(4) . . ? O1A U1 N3A 92.1(3) . . ? N1A U1 N3A 167.0(3) . . ? N2A U1 N3A 98.1(3) . . ? O2A U1 N4A 94.2(3) . . ? O1A U1 N4A 83.7(3) . . ? N1A U1 N4A 81.5(3) . . ? N2A U1 N4A 173.7(4) . . ? N3A U1 N4A 85.6(3) . . ? N6A Na1 O7A 122.9(4) . . ? N6A Na1 O5A 109.3(4) . . ? O7A Na1 O5A 123.2(3) . . ? N6A Na1 O4A 98.3(4) . . ? O7A Na1 O4A 117.7(4) . . ? O5A Na1 O4A 70.9(4) . . ? N6A Na1 O3A 86.2(4) . . ? O7A Na1 O3A 67.9(3) . . ? O5A Na1 O3A 140.6(3) . . ? O4A Na1 O3A 71.1(4) . . ? N6A Na1 O6A 116.8(4) . . ? O7A Na1 O6A 69.0(3) . . ? O5A Na1 O6A 68.7(3) . . ? O4A Na1 O6A 133.0(3) . . ? O3A Na1 O6A 136.9(3) . . ? N1A Si1A C4A 112.4(7) . . ? N1A Si1A C1A 105.2(5) . . ? C4A Si1A C1A 110.8(8) . . ? N1A Si1A C3A 113.8(7) . . ? C4A Si1A C3A 107.6(9) . . ? C1A Si1A C3A 106.9(8) . . ? N1A Si2A C7A 110.6(7) . . ? N1A Si2A C5A 110.5(10) . . ? C7A Si2A C5A 108.7(11) . . ? N1A Si2A C6A 108.0(7) . . ? C7A Si2A C6A 108.7(11) . . ? C5A Si2A C6A 110.4(10) . . ? N2A Si3A C8A 104.0(5) . . ? N2A Si3A C10A 110.7(7) . . ? C8A Si3A C10A 109.1(7) . . ? N2A Si3A C11A 117.8(6) . . ? C8A Si3A C11A 107.9(7) . . ? C10A Si3A C11A 107.1(8) . . ? N2A Si4A C12A 112.2(7) . . ? N2A Si4A C14A 114.4(5) . . ? C12A Si4A C14A 106.3(8) . . ? N2A Si4A C13A 110.7(7) . . ? C12A Si4A C13A 107.4(9) . . ? C14A Si4A C13A 105.3(7) . . ? N3A Si5A C17A 111.4(5) . . ? N3A Si5A C16A 115.4(5) . . ? C17A Si5A C16A 104.8(7) . . ? N3A Si5A C15A 113.3(6) . . ? C17A Si5A C15A 109.1(6) . . ? C16A Si5A C15A 102.0(8) . . ? N3A Si6A C19A 112.9(6) . . ? N3A Si6A C20A 112.5(5) . . ? C19A Si6A C20A 106.7(8) . . ? N3A Si6A C18A 112.5(6) . . ? C19A Si6A C18A 106.8(9) . . ? C20A Si6A C18A 104.9(7) . . ? C1A O1A U1 115.5(7) . . ? C8A O2A U1 123.8(7) . . ? C30A O3A C21A 121.9(11) . . ? C30A O3A Na1 113.3(7) . . ? C21A O3A Na1 108.4(8) . . ? C22A O4A C23A 114.1(11) . . ? C22A O4A Na1 106.2(8) . . ? C23A O4A Na1 106.0(7) . . ? C24A O5A C25A 109.5(10) . . ? C24A O5A Na1 119.0(8) . . ? C25A O5A Na1 114.9(6) . . ? C27A O6A C26A 116.6(9) . . ? C27A O6A Na1 109.5(7) . . ? C26A O6A Na1 112.3(7) . . ? C28A O7A C29A 115.5(11) . . ? C28A O7A Na1 113.1(7) . . ? C29A O7A Na1 111.4(7) . . ? Si2A N1A Si1A 122.6(5) . . ? Si2A N1A U1 125.1(5) . . ? Si1A N1A U1 109.6(5) . . ? Si4A N2A Si3A 118.9(5) . . ? Si4A N2A U1 129.0(5) . . ? Si3A N2A U1 111.9(4) . . ? Si5A N3A Si6A 117.7(4) . . ? Si5A N3A U1 122.9(4) . . ? Si6A N3A U1 118.3(4) . . ? N5A N4A U1 126.4(7) . . ? N6A N5A N4A 176.0(12) . . ? N5A N6A Na1 167.4(11) . . ? C2A C1A O1A 121.0(14) . . ? C2A C1A Si1A 126.6(13) . . ? O1A C1A Si1A 112.4(9) . . ? C1A C2A H2A 120.0 . . ? C1A C2A H2B 120.0 . . ? H2A C2A H2B 120.0 . . ? Si1A C3A H3A 109.5 . . ? Si1A C3A H3B 109.5 . . ? H3A C3A H3B 109.5 . . ? Si1A C3A H3C 109.5 . . ? H3A C3A H3C 109.5 . . ? H3B C3A H3C 109.5 . . ? Si1A C4A H4A 109.5 . . ? Si1A C4A H4B 109.5 . . ? H4A C4A H4B 109.5 . . ? Si1A C4A H4C 109.5 . . ? H4A C4A H4C 109.5 . . ? H4B C4A H4C 109.5 . . ? Si2A C5A H5A 109.5 . . ? Si2A C5A H5B 109.5 . . ? H5A C5A H5B 109.5 . . ? Si2A C5A H5C 109.5 . . ? H5A C5A H5C 109.5 . . ? H5B C5A H5C 109.5 . . ? Si2A C6A H6A 109.5 . . ? Si2A C6A H6B 109.5 . . ? H6A C6A H6B 109.5 . . ? Si2A C6A H6C 109.5 . . ? H6A C6A H6C 109.5 . . ? H6B C6A H6C 109.5 . . ? Si2A C7A H7A 109.5 . . ? Si2A C7A H7B 109.5 . . ? H7A C7A H7B 109.5 . . ? Si2A C7A H7C 109.5 . . ? H7A C7A H7C 109.5 . . ? H7B C7A H7C 109.5 . . ? C9A C8A O2A 121.4(13) . . ? C9A C8A Si3A 127.5(12) . . ? O2A C8A Si3A 110.8(9) . . ? C8A C9A H9A 120.0 . . ? C8A C9A H9B 120.0 . . ? H9A C9A H9B 120.0 . . ? Si3A C10A H10A 109.5 . . ? Si3A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? Si3A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? Si3A C11A H11A 109.5 . . ? Si3A C11A H11B 109.5 . . ? H11A C11A H11B 109.5 . . ? Si3A C11A H11C 109.5 . . ? H11A C11A H11C 109.5 . . ? H11B C11A H11C 109.5 . . ? Si4A C12A H12A 109.5 . . ? Si4A C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? Si4A C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? Si4A C13A H13A 109.5 . . ? Si4A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? Si4A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? Si4A C14A H14A 109.5 . . ? Si4A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? Si4A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? Si5A C15A H15A 109.5 . . ? Si5A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? Si5A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? Si5A C16A H16A 109.5 . . ? Si5A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? Si5A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? Si5A C17A H17A 109.5 . . ? Si5A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? Si5A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? Si6A C18A H18A 109.5 . . ? Si6A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? Si6A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? Si6A C19A H19A 109.5 . . ? Si6A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? Si6A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? Si6A C20A H20A 109.5 . . ? Si6A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? Si6A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? O3A C21A C22A 113.5(11) . . ? O3A C21A H21A 108.9 . . ? C22A C21A H21A 108.9 . . ? O3A C21A H21B 108.9 . . ? C22A C21A H21B 108.9 . . ? H21A C21A H21B 107.7 . . ? O4A C22A C21A 104.2(12) . . ? O4A C22A H22A 110.9 . . ? C21A C22A H22A 110.9 . . ? O4A C22A H22B 110.9 . . ? C21A C22A H22B 110.9 . . ? H22A C22A H22B 108.9 . . ? O4A C23A C24A 106.0(9) . . ? O4A C23A H23A 110.5 . . ? C24A C23A H23A 110.5 . . ? O4A C23A H23B 110.5 . . ? C24A C23A H23B 110.5 . . ? H23A C23A H23B 108.7 . . ? O5A C24A C23A 108.1(12) . . ? O5A C24A H24A 110.1 . . ? C23A C24A H24A 110.1 . . ? O5A C24A H24B 110.1 . . ? C23A C24A H24B 110.1 . . ? H24A C24A H24B 108.4 . . ? O5A C25A C26A 106.2(9) . . ? O5A C25A H25A 110.5 . . ? C26A C25A H25A 110.5 . . ? O5A C25A H25B 110.5 . . ? C26A C25A H25B 110.5 . . ? H25A C25A H25B 108.7 . . ? O6A C26A C25A 110.6(10) . . ? O6A C26A H26A 109.5 . . ? C25A C26A H26A 109.5 . . ? O6A C26A H26B 109.5 . . ? C25A C26A H26B 109.5 . . ? H26A C26A H26B 108.1 . . ? O6A C27A C28A 109.2(9) . . ? O6A C27A H27A 109.8 . . ? C28A C27A H27A 109.8 . . ? O6A C27A H27B 109.8 . . ? C28A C27A H27B 109.8 . . ? H27A C27A H27B 108.3 . . ? O7A C28A C27A 109.6(10) . . ? O7A C28A H28A 109.8 . . ? C27A C28A H28A 109.8 . . ? O7A C28A H28B 109.8 . . ? C27A C28A H28B 109.8 . . ? H28A C28A H28B 108.2 . . ? O7A C29A C30A 104.9(12) . . ? O7A C29A H29A 110.8 . . ? C30A C29A H29A 110.8 . . ? O7A C29A H29B 110.8 . . ? C30A C29A H29B 110.8 . . ? H29A C29A H29B 108.8 . . ? O3A C30A C29A 111.6(10) . . ? O3A C30A H30A 109.3 . . ? C29A C30A H30A 109.3 . . ? O3A C30A H30B 109.3 . . ? C29A C30A H30B 109.3 . . ? H30A C30A H30B 108.0 . . ? O2B U2 O1B 176.1(2) . . ? O2B U2 N1B 94.1(2) . . ? O1B U2 N1B 82.7(2) . . ? O2B U2 N3B 90.2(2) . . ? O1B U2 N3B 92.5(2) . . ? N1B U2 N3B 166.5(2) . . ? O2B U2 N2B 81.1(2) . . ? O1B U2 N2B 101.3(2) . . ? N1B U2 N2B 95.7(3) . . ? N3B U2 N2B 97.6(2) . . ? O2B U2 N4B 91.4(2) . . ? O1B U2 N4B 86.1(2) . . ? N1B U2 N4B 81.5(3) . . ? N3B U2 N4B 85.6(2) . . ? N2B U2 N4B 171.7(3) . . ? N6B Na2 O4B 102.3(5) . . ? N6B Na2 O3B 116.9(4) . . ? O4B Na2 O3B 73.5(5) . . ? N6B Na2 O7B 123.9(4) . . ? O4B Na2 O7B 130.4(5) . . ? O3B Na2 O7B 70.4(4) . . ? N6B Na2 O5B 95.9(4) . . ? O4B Na2 O5B 72.0(5) . . ? O3B Na2 O5B 136.5(5) . . ? O7B Na2 O5B 115.4(4) . . ? N6B Na2 O6B 87.6(3) . . ? O4B Na2 O6B 138.8(5) . . ? O3B Na2 O6B 136.8(5) . . ? O7B Na2 O6B 66.4(4) . . ? O5B Na2 O6B 67.2(5) . . ? N1B Si1B C4B 114.3(5) . . ? N1B Si1B C1B 103.2(4) . . ? C4B Si1B C1B 108.0(5) . . ? N1B Si1B C3B 114.2(6) . . ? C4B Si1B C3B 107.9(6) . . ? C1B Si1B C3B 108.9(5) . . ? N1B Si2B C7B 114.4(5) . . ? N1B Si2B C6B 109.5(4) . . ? C7B Si2B C6B 106.9(6) . . ? N1B Si2B C5B 110.3(5) . . ? C7B Si2B C5B 108.9(7) . . ? C6B Si2B C5B 106.5(6) . . ? N2B Si3B C10B 112.8(5) . . ? N2B Si3B C8B 103.9(4) . . ? C10B Si3B C8B 107.9(6) . . ? N2B Si3B C11B 115.1(6) . . ? C10B Si3B C11B 111.8(7) . . ? C8B Si3B C11B 104.4(6) . . ? N2B Si4B C13B 114.1(5) . . ? N2B Si4B C14B 111.9(5) . . ? C13B Si4B C14B 102.7(7) . . ? N2B Si4B C12B 111.5(6) . . ? C13B Si4B C12B 105.6(6) . . ? C14B Si4B C12B 110.6(7) . . ? N3B Si5B C17B 117.9(4) . . ? N3B Si5B C16B 110.5(5) . . ? C17B Si5B C16B 106.2(5) . . ? N3B Si5B C15B 109.7(4) . . ? C17B Si5B C15B 102.0(6) . . ? C16B Si5B C15B 110.0(6) . . ? N3B Si6B C19B 110.8(4) . . ? N3B Si6B C20B 112.2(4) . . ? C19B Si6B C20B 107.5(6) . . ? N3B Si6B C18B 113.0(4) . . ? C19B Si6B C18B 110.6(6) . . ? C20B Si6B C18B 102.4(5) . . ? C1B O1B U2 117.8(5) . . ? C8B O2B U2 122.9(5) . . ? C21B O3B C30B 110.6(15) . . ? C21B O3B Na2 117.0(12) . . ? C30B O3B Na2 114.9(10) . . ? C23B O4B C22B 115.6(16) . . ? C23B O4B Na2 111.6(11) . . ? C22B O4B Na2 101.6(11) . . ? C25B O5B C24B 116.3(15) . . ? C25B O5B Na2 108.4(13) . . ? C24B O5B Na2 102.6(11) . . ? C27B O6B C26B 111.7(16) . . ? C27B O6B Na2 115.4(12) . . ? C26B O6B Na2 117.1(12) . . ? C28B O7B C29B 115.4(15) . . ? C28B O7B Na2 110.9(10) . . ? C29B O7B Na2 105.0(9) . . ? Si1B N1B Si2B 120.5(4) . . ? Si1B N1B U2 112.2(3) . . ? Si2B N1B U2 123.9(4) . . ? Si3B N2B Si4B 121.1(5) . . ? Si3B N2B U2 110.5(3) . . ? Si4B N2B U2 127.9(4) . . ? Si6B N3B Si5B 117.4(3) . . ? Si6B N3B U2 119.9(3) . . ? Si5B N3B U2 122.0(4) . . ? N5B N4B U2 140.2(6) . . ? N6B N5B N4B 177.5(10) . . ? N5B N6B Na2 172.8(9) . . ? C2B C1B O1B 119.3(9) . . ? C2B C1B Si1B 126.9(8) . . ? O1B C1B Si1B 113.8(6) . . ? C1B C2B H2C 120.0 . . ? C1B C2B H2D 120.0 . . ? H2C C2B H2D 120.0 . . ? Si1B C3B H3D 109.5 . . ? Si1B C3B H3E 109.5 . . ? H3D C3B H3E 109.5 . . ? Si1B C3B H3F 109.5 . . ? H3D C3B H3F 109.5 . . ? H3E C3B H3F 109.5 . . ? Si1B C4B H4D 109.5 . . ? Si1B C4B H4E 109.5 . . ? H4D C4B H4E 109.5 . . ? Si1B C4B H4F 109.5 . . ? H4D C4B H4F 109.5 . . ? H4E C4B H4F 109.5 . . ? Si2B C5B H5D 109.5 . . ? Si2B C5B H5E 109.5 . . ? H5D C5B H5E 109.5 . . ? Si2B C5B H5F 109.5 . . ? H5D C5B H5F 109.5 . . ? H5E C5B H5F 109.5 . . ? Si2B C6B H6D 109.5 . . ? Si2B C6B H6E 109.5 . . ? H6D C6B H6E 109.5 . . ? Si2B C6B H6F 109.5 . . ? H6D C6B H6F 109.5 . . ? H6E C6B H6F 109.5 . . ? Si2B C7B H7D 109.5 . . ? Si2B C7B H7E 109.5 . . ? H7D C7B H7E 109.5 . . ? Si2B C7B H7F 109.5 . . ? H7D C7B H7F 109.5 . . ? H7E C7B H7F 109.5 . . ? C9B C8B O2B 120.7(9) . . ? C9B C8B Si3B 125.8(8) . . ? O2B C8B Si3B 113.0(6) . . ? C8B C9B H9C 120.0 . . ? C8B C9B H9D 120.0 . . ? H9C C9B H9D 120.0 . . ? Si3B C10B H10D 109.5 . . ? Si3B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? Si3B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? Si3B C11B H11D 109.5 . . ? Si3B C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? Si3B C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? Si4B C12B H12D 109.5 . . ? Si4B C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? Si4B C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? Si4B C13B H13D 109.5 . . ? Si4B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? Si4B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? Si4B C14B H14D 109.5 . . ? Si4B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? Si4B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? Si5B C15B H15D 109.5 . . ? Si5B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? Si5B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? Si5B C16B H16D 109.5 . . ? Si5B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? Si5B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? Si5B C17B H17D 109.5 . . ? Si5B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? Si5B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? Si6B C18B H18D 109.5 . . ? Si6B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? Si6B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? Si6B C19B H19D 109.5 . . ? Si6B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? Si6B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? Si6B C20B H20D 109.5 . . ? Si6B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? Si6B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? O3B C21B C22B 105.1(15) . . ? O3B C21B H21C 110.7 . . ? C22B C21B H21C 110.7 . . ? O3B C21B H21D 110.7 . . ? C22B C21B H21D 110.7 . . ? H21C C21B H21D 108.8 . . ? O4B C22B C21B 119.5(17) . . ? O4B C22B H22C 107.4 . . ? C21B C22B H22C 107.4 . . ? O4B C22B H22D 107.4 . . ? C21B C22B H22D 107.4 . . ? H22C C22B H22D 107.0 . . ? O4B C23B C24B 110.1(17) . . ? O4B C23B H23C 109.6 . . ? C24B C23B H23C 109.6 . . ? O4B C23B H23D 109.6 . . ? C24B C23B H23D 109.6 . . ? H23C C23B H23D 108.1 . . ? O5B C24B C23B 104.9(15) . . ? O5B C24B H24C 110.8 . . ? C23B C24B H24C 110.8 . . ? O5B C24B H24D 110.8 . . ? C23B C24B H24D 110.8 . . ? H24C C24B H24D 108.8 . . ? O5B C25B C26B 110.2(18) . . ? O5B C25B H25C 109.6 . . ? C26B C25B H25C 109.6 . . ? O5B C25B H25D 109.6 . . ? C26B C25B H25D 109.6 . . ? H25C C25B H25D 108.1 . . ? O6B C26B C25B 108.1(17) . . ? O6B C26B H26C 110.1 . . ? C25B C26B H26C 110.1 . . ? O6B C26B H26D 110.1 . . ? C25B C26B H26D 110.1 . . ? H26C C26B H26D 108.4 . . ? O6B C27B C28B 109.3(16) . . ? O6B C27B H27C 109.8 . . ? C28B C27B H27C 109.8 . . ? O6B C27B H27D 109.8 . . ? C28B C27B H27D 109.8 . . ? H27C C27B H27D 108.3 . . ? O7B C28B C27B 107.7(15) . . ? O7B C28B H28C 110.2 . . ? C27B C28B H28C 110.2 . . ? O7B C28B H28D 110.2 . . ? C27B C28B H28D 110.2 . . ? H28C C28B H28D 108.5 . . ? O7B C29B C30B 108.9(14) . . ? O7B C29B H29C 109.9 . . ? C30B C29B H29C 109.9 . . ? O7B C29B H29D 109.9 . . ? C30B C29B H29D 109.9 . . ? H29C C29B H29D 108.3 . . ? O3B C30B C29B 103.5(15) . . ? O3B C30B H30C 111.1 . . ? C29B C30B H30C 111.1 . . ? O3B C30B H30D 111.1 . . ? C29B C30B H30D 111.1 . . ? H30C C30B H30D 109.0 . . ? C2 C1 H1A 107.8 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 110.6 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C1 110.9(10) . . ? C3 C2 H2E 114.9 . . ? C1 C2 H2E 109.7 . . ? C3 C2 H2F 105.1 . . ? C1 C2 H2F 107.7 . . ? H2E C2 H2F 108.0 . . ? C2 C3 C4 111.0(10) . . ? C2 C3 H3G 103.7 . . ? C4 C3 H3G 100.1 . . ? C2 C3 H3H 112.9 . . ? C4 C3 H3H 119.1 . . ? H3G C3 H3H 108.0 . . ? C3 C4 C5 108.8(9) . . ? C3 C4 H4G 118.9 . . ? C5 C4 H4G 115.1 . . ? C3 C4 H4H 99.9 . . ? C5 C4 H4H 103.7 . . ? H4G C4 H4H 108.2 . . ? C4 C5 H5G 115.0 . . ? C4 C5 H5H 109.7 . . ? H5G C5 H5H 109.5 . . ? C4 C5 H5I 103.5 . . ? H5G C5 H5I 109.4 . . ? H5H C5 H5I 109.5 . . ? C7 C6 H6G 109.4 . . ? C7 C6 H6H 109.8 . . ? H6G C6 H6H 109.5 . . ? C7 C6 H6I 109.1 . . ? H6G C6 H6I 109.5 . . ? H6H C6 H6I 109.5 . . ? C8 C7 C6 106.4(10) . . ? C8 C7 H7G 110.2 . . ? C6 C7 H7G 110.4 . . ? C8 C7 H7H 110.4 . . ? C6 C7 H7H 110.9 . . ? H7G C7 H7H 108.7 . . ? C9 C8 C7 107.5(10) . . ? C9 C8 H8A 110.7 . . ? C7 C8 H8A 109.9 . . ? C9 C8 H8B 109.9 . . ? C7 C8 H8B 110.4 . . ? H8A C8 H8B 108.5 . . ? C8 C9 C10 107.0(10) . . ? C8 C9 H9E 110.7 . . ? C10 C9 H9E 110.7 . . ? C8 C9 H9F 109.9 . . ? C10 C9 H9F 109.9 . . ? H9E C9 H9F 108.6 . . ? C9 C10 H10G 109.6 . . ? C9 C10 H10H 109.8 . . ? H10G C10 H10H 109.5 . . ? C9 C10 H10I 109.0 . . ? H10G C10 H10I 109.5 . . ? H10H C10 H10I 109.5 . . ? #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 827397' #TrackingRef '- CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H40 I3 N2 O3 Si4 U' _chemical_formula_weight 1063.61 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.5673(4) _cell_length_b 18.2209(5) _cell_length_c 22.5867(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6818.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 182324 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 28.70 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent dark orange' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.072 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3944 _exptl_absorpt_coefficient_mu 7.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.265 _exptl_absorpt_correction_T_max 0.466 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 40 mm' _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and five \w scans with 1\% steps (1002 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 182324 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 28.70 _reflns_number_total 8795 _reflns_number_gt 5920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for some badly behaving C atoms. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH~2~) or 1.5 (CH~3~) times that of the parent atom. The highest residual electron density peak is located near atom I2, and is possibly due to imperfect absorption corrections. 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^)+(0.0675P)^2^+26.7147P] 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 8795 _refine_ls_number_parameters 290 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1425 _refine_ls_wR_factor_gt 0.1315 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.976 _refine_diff_density_min -2.054 _refine_diff_density_rms 0.164 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 U U 0.846093(17) 0.640215(15) 0.150745(13) 0.04353(10) Uani 1 1 d . . . I1 I 0.94951(4) 0.50621(3) 0.16293(3) 0.06283(17) Uani 1 1 d . . . I2 I 1.03751(5) 0.86352(4) 0.21651(4) 0.0857(2) Uani 1 1 d . . . I3 I 0.57811(6) 0.50733(5) 0.07263(5) 0.1072(3) Uani 1 1 d . . . Si1 Si 0.97584(17) 0.70497(14) 0.05004(12) 0.0645(7) Uani 1 1 d . . . Si2 Si 0.8354(2) 0.61743(16) -0.00261(12) 0.0705(8) Uani 1 1 d . . . Si3 Si 0.71663(16) 0.57767(15) 0.25318(13) 0.0662(7) Uani 1 1 d . . . Si4 Si 0.84461(17) 0.67989(18) 0.30221(13) 0.0720(7) Uani 1 1 d . . . O1 O 0.9374(3) 0.7169(3) 0.1689(2) 0.0531(13) Uani 1 1 d . . . O2 O 0.7400(4) 0.5833(3) 0.1299(3) 0.0623(15) Uani 1 1 d . . . O3 O 0.7635(3) 0.7477(3) 0.1391(3) 0.0573(14) Uani 1 1 d . . . N1 N 0.8848(4) 0.6562(4) 0.0591(3) 0.0505(15) Uani 1 1 d . . . N2 N 0.8026(4) 0.6315(4) 0.2410(3) 0.0522(16) Uani 1 1 d . . . C1 C 0.9855(5) 0.7489(5) 0.1254(4) 0.062(2) Uani 1 1 d . . . C2 C 1.0323(7) 0.8090(6) 0.1380(5) 0.081(3) Uani 1 1 d U . . H2 H 1.0648 0.8266 0.1076 0.097 Uiso 1 1 calc R . . C3 C 0.9757(8) 0.7805(7) -0.0052(5) 0.095(4) Uani 1 1 d . . . H3A H 0.9731 0.7601 -0.0444 0.143 Uiso 1 1 calc R . . H3B H 1.0242 0.8088 -0.0011 0.143 Uiso 1 1 calc R . . H3C H 0.9297 0.8114 0.0013 0.143 Uiso 1 1 calc R . . C4 C 1.0649(7) 0.6444(7) 0.0399(5) 0.089(4) Uani 1 1 d . . . H4A H 1.0612 0.6035 0.0666 0.134 Uiso 1 1 calc R . . H4B H 1.1133 0.6716 0.0481 0.134 Uiso 1 1 calc R . . H4C H 1.0663 0.6268 -0.0001 0.134 Uiso 1 1 calc R . . C5 C 0.7418(7) 0.6684(7) -0.0184(5) 0.093(4) Uani 1 1 d . . . H5A H 0.7028 0.6585 0.0120 0.139 Uiso 1 1 calc R . . H5B H 0.7206 0.6533 -0.0560 0.139 Uiso 1 1 calc R . . H5C H 0.7532 0.7201 -0.0194 0.139 Uiso 1 1 calc R . . C6 C 0.8999(9) 0.6227(8) -0.0701(5) 0.108(4) Uani 1 1 d . . . H6A H 0.9177 0.6723 -0.0758 0.162 Uiso 1 1 calc R . . H6B H 0.8693 0.6071 -0.1040 0.162 Uiso 1 1 calc R . . H6C H 0.9460 0.5913 -0.0653 0.162 Uiso 1 1 calc R . . C7 C 0.8161(9) 0.5186(5) 0.0103(5) 0.096(4) Uani 1 1 d . . . H7A H 0.8666 0.4933 0.0146 0.145 Uiso 1 1 calc R . . H7B H 0.7871 0.4986 -0.0228 0.145 Uiso 1 1 calc R . . H7C H 0.7847 0.5127 0.0456 0.145 Uiso 1 1 calc R . . C8 C 0.6846(6) 0.5578(5) 0.1726(5) 0.065(2) Uani 1 1 d . . . C9 C 0.6163(7) 0.5253(6) 0.1572(6) 0.086(3) Uani 1 1 d . . . H9 H 0.5828 0.5092 0.1876 0.104 Uiso 1 1 calc R . . C10 C 0.6338(7) 0.6281(7) 0.2877(6) 0.098(4) Uani 1 1 d . . . H10A H 0.6393 0.6260 0.3300 0.147 Uiso 1 1 calc R . . H10B H 0.5833 0.6066 0.2763 0.147 Uiso 1 1 calc R . . H10C H 0.6353 0.6784 0.2750 0.147 Uiso 1 1 calc R . . C11 C 0.7356(9) 0.4898(6) 0.2904(6) 0.107(4) Uani 1 1 d . . . H11A H 0.7739 0.4618 0.2679 0.161 Uiso 1 1 calc R . . H11B H 0.6860 0.4629 0.2935 0.161 Uiso 1 1 calc R . . H11C H 0.7568 0.4988 0.3293 0.161 Uiso 1 1 calc R . . C12 C 0.8116(8) 0.7765(7) 0.2976(6) 0.109(4) Uani 1 1 d U . . H12A H 0.8370 0.7996 0.2643 0.163 Uiso 1 1 calc R . . H12B H 0.8267 0.8018 0.3332 0.163 Uiso 1 1 calc R . . H12C H 0.7541 0.7783 0.2930 0.163 Uiso 1 1 calc R . . C13 C 0.8076(10) 0.6403(9) 0.3763(7) 0.126(5) Uani 1 1 d U . . H13A H 0.7520 0.6263 0.3727 0.189 Uiso 1 1 calc R . . H13B H 0.8130 0.6768 0.4067 0.189 Uiso 1 1 calc R . . H13C H 0.8394 0.5981 0.3864 0.189 Uiso 1 1 calc R . . C14 C 0.9555(7) 0.6695(8) 0.3035(6) 0.099(4) Uani 1 1 d . . . H14A H 0.9694 0.6197 0.2940 0.148 Uiso 1 1 calc R . . H14B H 0.9754 0.6813 0.3423 0.148 Uiso 1 1 calc R . . H14C H 0.9792 0.7020 0.2750 0.148 Uiso 1 1 calc R . . C15 C 0.7916(6) 0.8195(5) 0.1197(6) 0.091(4) Uani 1 1 d . . . H15A H 0.8101 0.8179 0.0790 0.109 Uiso 1 1 calc R . . H15B H 0.8351 0.8371 0.1447 0.109 Uiso 1 1 calc R . . C16 C 0.7192(10) 0.8664(8) 0.1256(8) 0.123(5) Uani 1 1 d U . . H16A H 0.7183 0.8897 0.1642 0.148 Uiso 1 1 calc R . . H16B H 0.7192 0.9043 0.0955 0.148 Uiso 1 1 calc R . . C17 C 0.6500(7) 0.8194(7) 0.1187(7) 0.099(4) Uani 1 1 d . . . H17A H 0.6374 0.8119 0.0772 0.119 Uiso 1 1 calc R . . H17B H 0.6031 0.8398 0.1385 0.119 Uiso 1 1 calc R . . C18 C 0.6763(6) 0.7502(6) 0.1471(5) 0.078(3) Uani 1 1 d . . . H18A H 0.6625 0.7501 0.1889 0.093 Uiso 1 1 calc R . . H18B H 0.6508 0.7083 0.1283 0.093 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 U 0.04697(16) 0.04055(15) 0.04308(16) -0.00255(12) 0.00162(12) 0.00419(11) I1 0.0614(3) 0.0430(3) 0.0841(4) 0.0062(3) 0.0027(3) 0.0087(2) I2 0.0832(5) 0.0713(4) 0.1026(6) -0.0078(4) -0.0228(4) -0.0101(3) I3 0.0938(6) 0.0871(5) 0.1406(8) -0.0108(5) -0.0505(6) -0.0150(4) Si1 0.0728(16) 0.0566(14) 0.0642(16) 0.0069(12) 0.0177(13) 0.0070(12) Si2 0.098(2) 0.0637(15) 0.0494(14) -0.0119(12) -0.0124(14) 0.0185(14) Si3 0.0612(15) 0.0643(15) 0.0731(16) 0.0071(13) 0.0116(13) -0.0036(12) Si4 0.0674(17) 0.092(2) 0.0571(15) -0.0154(14) -0.0081(13) 0.0029(14) O1 0.055(3) 0.052(3) 0.052(3) -0.006(3) -0.002(3) -0.002(3) O2 0.057(3) 0.051(3) 0.079(4) -0.008(3) -0.003(3) -0.004(3) O3 0.054(3) 0.050(3) 0.068(4) -0.002(3) 0.000(3) 0.009(3) N1 0.060(4) 0.051(4) 0.040(3) -0.003(3) 0.005(3) 0.012(3) N2 0.060(4) 0.055(4) 0.042(4) -0.006(3) 0.007(3) 0.001(3) C1 0.064(5) 0.051(5) 0.070(6) 0.001(4) 0.005(5) 0.002(4) C2 0.084(6) 0.072(5) 0.087(6) 0.004(5) 0.012(5) -0.008(5) C3 0.128(10) 0.089(8) 0.070(7) 0.016(6) -0.008(7) -0.013(7) C4 0.069(6) 0.123(10) 0.076(7) 0.011(6) 0.016(6) 0.019(6) C5 0.084(7) 0.096(8) 0.098(8) -0.024(7) -0.034(7) 0.015(6) C6 0.116(10) 0.147(12) 0.062(7) -0.030(7) 0.004(7) 0.006(9) C7 0.143(11) 0.060(6) 0.085(8) -0.036(6) -0.014(8) 0.002(7) C8 0.058(5) 0.046(4) 0.090(7) 0.000(5) -0.001(5) -0.006(4) C9 0.078(7) 0.074(7) 0.107(9) 0.008(6) 0.001(7) -0.010(6) C10 0.062(6) 0.137(11) 0.094(9) -0.008(8) 0.015(6) 0.006(6) C11 0.119(11) 0.085(8) 0.118(11) 0.040(7) -0.013(9) -0.014(7) C12 0.107(7) 0.101(7) 0.118(8) -0.036(6) -0.025(6) 0.007(6) C13 0.128(8) 0.152(9) 0.099(8) -0.002(7) 0.010(7) -0.017(7) C14 0.072(7) 0.144(11) 0.081(8) 0.004(8) -0.027(6) 0.017(7) C15 0.073(7) 0.045(5) 0.153(12) 0.014(6) 0.011(7) 0.013(5) C16 0.111(8) 0.097(7) 0.163(9) 0.018(7) -0.003(7) 0.020(7) C17 0.081(8) 0.078(8) 0.139(12) 0.007(8) -0.002(8) 0.026(6) C18 0.052(5) 0.072(6) 0.109(9) 0.005(6) 0.001(5) 0.020(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 U O2 2.094(6) . ? U O1 2.099(5) . ? U N2 2.168(6) . ? U N1 2.187(6) . ? U O3 2.405(5) . ? U I1 2.9955(6) . ? I2 C2 2.035(12) . ? I3 C9 2.038(12) . ? Si1 N1 1.763(8) . ? Si1 C3 1.857(11) . ? Si1 C4 1.857(11) . ? Si1 C1 1.888(10) . ? Si2 N1 1.764(7) . ? Si2 C5 1.843(11) . ? Si2 C7 1.851(11) . ? Si2 C6 1.864(13) . ? Si3 N2 1.751(7) . ? Si3 C10 1.827(11) . ? Si3 C11 1.835(11) . ? Si3 C8 1.930(11) . ? Si4 N2 1.781(7) . ? Si4 C14 1.847(11) . ? Si4 C12 1.846(13) . ? Si4 C13 1.922(15) . ? O1 C1 1.393(11) . ? O2 C8 1.411(11) . ? O3 C18 1.456(11) . ? O3 C15 1.456(11) . ? C1 C2 1.370(14) . ? C2 H2 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.324(15) . ? C9 H9 0.9300 . ? 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 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.478(16) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.439(19) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.481(15) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 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 O2 U O1 168.0(2) . . ? O2 U N2 84.1(3) . . ? O1 U N2 96.0(2) . . ? O2 U N1 95.7(3) . . ? O1 U N1 83.4(2) . . ? N2 U N1 175.9(2) . . ? O2 U O3 84.3(2) . . ? O1 U O3 83.7(2) . . ? N2 U O3 88.5(2) . . ? N1 U O3 87.4(2) . . ? O2 U I1 95.57(16) . . ? O1 U I1 96.45(15) . . ? N2 U I1 92.50(18) . . ? N1 U I1 91.61(16) . . ? O3 U I1 178.98(14) . . ? N1 Si1 C3 116.7(5) . . ? N1 Si1 C4 113.3(5) . . ? C3 Si1 C4 111.0(6) . . ? N1 Si1 C1 100.5(4) . . ? C3 Si1 C1 107.0(5) . . ? C4 Si1 C1 107.2(5) . . ? N1 Si2 C5 109.9(4) . . ? N1 Si2 C7 110.2(4) . . ? C5 Si2 C7 112.1(6) . . ? N1 Si2 C6 111.1(5) . . ? C5 Si2 C6 107.4(6) . . ? C7 Si2 C6 106.1(6) . . ? N2 Si3 C10 113.4(5) . . ? N2 Si3 C11 114.9(5) . . ? C10 Si3 C11 111.8(7) . . ? N2 Si3 C8 100.4(4) . . ? C10 Si3 C8 106.9(5) . . ? C11 Si3 C8 108.4(5) . . ? N2 Si4 C14 110.5(5) . . ? N2 Si4 C12 108.3(5) . . ? C14 Si4 C12 113.2(7) . . ? N2 Si4 C13 111.4(6) . . ? C14 Si4 C13 105.3(7) . . ? C12 Si4 C13 108.2(7) . . ? C1 O1 U 123.6(5) . . ? C8 O2 U 123.7(6) . . ? C18 O3 C15 109.1(7) . . ? C18 O3 U 125.2(6) . . ? C15 O3 U 125.6(5) . . ? Si2 N1 Si1 120.5(4) . . ? Si2 N1 U 124.0(4) . . ? Si1 N1 U 115.3(3) . . ? Si3 N2 Si4 118.2(4) . . ? Si3 N2 U 117.3(3) . . ? Si4 N2 U 124.3(4) . . ? O1 C1 C2 120.8(9) . . ? O1 C1 Si1 114.1(6) . . ? C2 C1 Si1 125.0(8) . . ? C1 C2 I2 126.5(8) . . ? C1 C2 H2 116.8 . . ? I2 C2 H2 116.8 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 O2 121.6(10) . . ? C9 C8 Si3 124.6(9) . . ? O2 C8 Si3 113.8(6) . . ? C8 C9 I3 125.7(9) . . ? C8 C9 H9 117.1 . . ? I3 C9 H9 117.1 . . ? Si3 C10 H10A 109.5 . . ? Si3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si3 C11 H11A 109.5 . . ? Si3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si4 C12 H12A 109.5 . . ? Si4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si4 C13 H13A 109.5 . . ? Si4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si4 C14 H14A 109.5 . . ? Si4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 C16 103.4(9) . . ? O3 C15 H15A 111.1 . . ? C16 C15 H15A 111.1 . . ? O3 C15 H15B 111.1 . . ? C16 C15 H15B 111.1 . . ? H15A C15 H15B 109.0 . . ? C17 C16 C15 107.1(11) . . ? C17 C16 H16A 110.3 . . ? C15 C16 H16A 110.3 . . ? C17 C16 H16B 110.3 . . ? C15 C16 H16B 110.3 . . ? H16A C16 H16B 108.6 . . ? C16 C17 C18 103.0(10) . . ? C16 C17 H17A 111.2 . . ? C18 C17 H17A 111.2 . . ? C16 C17 H17B 111.2 . . ? C18 C17 H17B 111.2 . . ? H17A C17 H17B 109.1 . . ? O3 C18 C17 105.3(9) . . ? O3 C18 H18A 110.7 . . ? C17 C18 H18A 110.7 . . ? O3 C18 H18B 110.7 . . ? C17 C18 H18B 110.7 . . ? H18A C18 H18B 108.8 . . ?