# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Mark Sarsfield' 'Madeleine Helliwell' 'Gordon H. John' 'Iain May' 'Clint A. Sharrad' 'A. Sutton' _publ_contact_author_name 'Dr Mark Sarsfield' _publ_contact_author_address ; Department of Chemistry University of Manchester Oxford Road Manchester UK M13 9PL ; _publ_contact_author_email MARK.J.SARSFIELD@MAN.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Coordination of pertechnetate [TcO4]- to actinides ; data_s1879-29ba _database_code_depnum_ccdc_archive 'CCDC 235211' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _publ_section_exptl_refinement ; The solution at 130K was used as a starting point. The crystal was twinned such that the twin matrix was 0 -1 0 -1 0 0 0 0 -1 and the twin fraction refined to a value of 0.073. Restraints were applied to the bond lengths and angles of the Bu groups. The non-H atoms, were refined anisotropically, using restraints. H atoms were included in calculated positions. ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H108 O20 P4 Tc4 Th' _chemical_formula_weight 1753.26 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' 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' Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbc2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, z' 'x, -y+1/2, z+1/2' _cell_length_a 21.386(4) _cell_length_b 21.732(4) _cell_length_c 14.820(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6888(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5577 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.42 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3512 _exptl_absorpt_coefficient_mu 3.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7476 _exptl_absorpt_correction_T_max 0.7476 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 35481 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.1003 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.56 _reflns_number_total 13901 _reflns_number_gt 12000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+22.3563P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.020(8) _refine_ls_number_reflns 13901 _refine_ls_number_parameters 707 _refine_ls_number_restraints 544 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1618 _refine_ls_wR_factor_gt 0.1507 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Th1 Th 0.251706(17) 0.005698(17) 0.15905(5) 0.01568(10) Uani 1 1 d U . . Tc1 Tc 0.39783(5) -0.00506(5) -0.01417(8) 0.0229(2) Uani 1 1 d U . . Tc2 Tc 0.26246(5) 0.16645(5) 0.29379(7) 0.0210(2) Uani 1 1 d U . . Tc3 Tc 0.25072(5) -0.13664(5) 0.34311(8) 0.0250(2) Uani 1 1 d U . . Tc1A Tc 0.09097(5) -0.01163(5) 0.01687(7) 0.0215(2) Uani 1 1 d U . . P1 P 0.41131(16) 0.00321(15) 0.2737(2) 0.0239(7) Uani 1 1 d U . . P2 P 0.22620(16) 0.13474(14) -0.0086(2) 0.0215(6) Uani 1 1 d DU . . P3 P 0.25975(17) -0.15146(17) 0.0481(3) 0.0318(8) Uani 1 1 d DU . . P1A P 0.11870(14) 0.03808(14) 0.32415(18) 0.0209(6) Uani 1 1 d DU . . O1 O 0.3276(4) 0.0198(4) 0.0357(6) 0.0321(17) Uani 1 1 d U . . O2 O 0.4587(5) 0.0374(5) 0.0243(8) 0.045(2) Uani 1 1 d U . . O3 O 0.3919(5) 0.0061(5) -0.1275(6) 0.045(3) Uani 1 1 d U . . O4 O 0.4111(5) -0.0805(5) 0.0071(6) 0.041(2) Uani 1 1 d U . . O5 O 0.3524(4) -0.0110(4) 0.2214(6) 0.0299(16) Uani 1 1 d U . . O6 O 0.2848(4) 0.1000(4) 0.2355(5) 0.0268(15) Uani 1 1 d U . . O7 O 0.2384(5) 0.1484(5) 0.4015(6) 0.043(3) Uani 1 1 d U . . O8 O 0.3258(4) 0.2142(4) 0.2984(6) 0.038(2) Uani 1 1 d U . . O9 O 0.2201(4) 0.0878(4) 0.0669(5) 0.0244(14) Uani 1 1 d U . . O10 O 0.2384(4) -0.0693(5) 0.2800(6) 0.0343(18) Uani 1 1 d U . . O11 O 0.3263(5) -0.1594(5) 0.3342(7) 0.044(2) Uani 1 1 d U . . O12 O 0.2350(5) -0.1217(5) 0.4538(6) 0.038(2) Uani 1 1 d U . . O13 O 0.2694(5) -0.0893(4) 0.0898(7) 0.0338(17) Uani 1 1 d U . . O1A O 0.1546(4) -0.0283(4) 0.0871(6) 0.0288(16) Uani 1 1 d U . . O2A O 0.0465(5) 0.0446(5) 0.0643(6) 0.039(2) Uani 1 1 d U . . O3A O 0.1160(5) 0.0111(5) -0.0859(7) 0.041(2) Uani 1 1 d U . . O4A O 0.0481(5) -0.0757(5) 0.0053(6) 0.044(2) Uani 1 1 d U . . O5A O 0.1689(4) 0.0405(4) 0.2520(5) 0.0255(15) Uani 1 1 d U . . O8A O 0.2036(5) 0.2018(5) 0.2390(6) 0.036(2) Uani 1 1 d U . . O11A O 0.2027(5) -0.1925(5) 0.3074(7) 0.044(2) Uani 1 1 d U . . C1 C 0.3994(6) -0.0098(6) 0.3905(8) 0.028(2) Uani 1 1 d DU . . H1A H 0.3898 -0.0539 0.3996 0.034 Uiso 1 1 calc R . . H1B H 0.4389 -0.0008 0.4227 0.034 Uiso 1 1 calc R . . C2 C 0.3468(6) 0.0286(6) 0.4338(7) 0.030(3) Uani 1 1 d DU . . H2A H 0.3602 0.0721 0.4375 0.036 Uiso 1 1 calc R . . H2B H 0.3092 0.0267 0.3949 0.036 Uiso 1 1 calc R . . C3 C 0.3299(6) 0.0055(7) 0.5288(8) 0.038(3) Uani 1 1 d DU . . H3A H 0.2923 0.0276 0.5505 0.046 Uiso 1 1 calc R . . H3B H 0.3197 -0.0389 0.5258 0.046 Uiso 1 1 calc R . . C4 C 0.3837(7) 0.0153(8) 0.5963(9) 0.051(4) Uani 1 1 d DU . . H4A H 0.4217 -0.0042 0.5731 0.076 Uiso 1 1 calc R . . H4B H 0.3725 -0.0031 0.6544 0.076 Uiso 1 1 calc R . . H4C H 0.3910 0.0595 0.6042 0.076 Uiso 1 1 calc R . . C5 C 0.4338(6) 0.0820(6) 0.2561(8) 0.027(2) Uani 1 1 d DU . . H5A H 0.4424 0.0877 0.1909 0.032 Uiso 1 1 calc R . . H5B H 0.3977 0.1085 0.2716 0.032 Uiso 1 1 calc R . . C6 C 0.4910(5) 0.1051(5) 0.3092(8) 0.030(2) Uani 1 1 d DU . . H6A H 0.4837 0.0996 0.3746 0.036 Uiso 1 1 calc R . . H6B H 0.5283 0.0806 0.2922 0.036 Uiso 1 1 calc R . . C7 C 0.5032(5) 0.1731(5) 0.2893(9) 0.029(2) Uani 1 1 d DU . . H7A H 0.5103 0.1787 0.2238 0.034 Uiso 1 1 calc R . . H7B H 0.4661 0.1976 0.3066 0.034 Uiso 1 1 calc R . . C8 C 0.5600(6) 0.1955(7) 0.3415(9) 0.042(4) Uani 1 1 d DU . . H8A H 0.5504 0.1961 0.4061 0.063 Uiso 1 1 calc R . . H8B H 0.5709 0.2371 0.3215 0.063 Uiso 1 1 calc R . . H8C H 0.5953 0.1678 0.3303 0.063 Uiso 1 1 calc R . . C9 C 0.4751(6) -0.0462(5) 0.2392(8) 0.028(2) Uani 1 1 d DU . . H9A H 0.4897 -0.0333 0.1787 0.033 Uiso 1 1 calc R . . H9B H 0.5104 -0.0409 0.2818 0.033 Uiso 1 1 calc R . . C10 C 0.4572(6) -0.1139(5) 0.2360(9) 0.034(2) Uani 1 1 d DU . . H10A H 0.4411 -0.1266 0.2958 0.041 Uiso 1 1 calc R . . H10B H 0.4232 -0.1197 0.1914 0.041 Uiso 1 1 calc R . . C11 C 0.5118(6) -0.1547(6) 0.2107(8) 0.036(3) Uani 1 1 d DU . . H11A H 0.4962 -0.1970 0.2008 0.043 Uiso 1 1 calc R . . H11B H 0.5296 -0.1399 0.1529 0.043 Uiso 1 1 calc R . . C12 C 0.5632(7) -0.1566(8) 0.2803(11) 0.052(4) Uani 1 1 d DU . . H12A H 0.5449 -0.1536 0.3408 0.078 Uiso 1 1 calc R . . H12B H 0.5918 -0.1221 0.2705 0.078 Uiso 1 1 calc R . . H12C H 0.5862 -0.1954 0.2748 0.078 Uiso 1 1 calc R . . C13 C 0.1515(5) 0.1734(5) -0.0265(9) 0.028(2) Uani 1 1 d DU . . H13C H 0.1484 0.1854 -0.0909 0.033 Uiso 1 1 calc R . . H13D H 0.1173 0.1438 -0.0141 0.033 Uiso 1 1 calc R . . C14 C 0.1414(5) 0.2305(6) 0.0314(8) 0.031(3) Uani 1 1 d DU . . H14C H 0.1744 0.2609 0.0172 0.037 Uiso 1 1 calc R . . H14D H 0.1458 0.2190 0.0957 0.037 Uiso 1 1 calc R . . C15 C 0.0774(5) 0.2605(6) 0.0175(9) 0.031(2) Uani 1 1 d DU . . H15A H 0.0719 0.2701 -0.0474 0.037 Uiso 1 1 calc R . . H15B H 0.0443 0.2309 0.0349 0.037 Uiso 1 1 calc R . . C16 C 0.0696(7) 0.3185(6) 0.0714(9) 0.040(3) Uani 1 1 d DU . . H16A H 0.0739 0.3091 0.1358 0.060 Uiso 1 1 calc R . . H16B H 0.0281 0.3359 0.0600 0.060 Uiso 1 1 calc R . . H16C H 0.1018 0.3483 0.0536 0.060 Uiso 1 1 calc R . . C17 C 0.2449(6) 0.0986(6) -0.1134(8) 0.027(2) Uani 1 1 d DU . . H17A H 0.2837 0.0744 -0.1054 0.032 Uiso 1 1 calc R . . H17B H 0.2110 0.0695 -0.1287 0.032 Uiso 1 1 calc R . . C18 C 0.2541(6) 0.1433(6) -0.1936(7) 0.032(3) Uani 1 1 d DU . . H18A H 0.2169 0.1701 -0.1990 0.038 Uiso 1 1 calc R . . H18B H 0.2907 0.1699 -0.1816 0.038 Uiso 1 1 calc R . . C19 C 0.2640(9) 0.1091(7) -0.2822(8) 0.044(4) Uani 1 1 d DU . . H19A H 0.2279 0.0817 -0.2940 0.052 Uiso 1 1 calc R . . H19B H 0.3021 0.0832 -0.2779 0.052 Uiso 1 1 calc R . . C20 C 0.2712(12) 0.1553(7) -0.3601(8) 0.065(5) Uani 1 1 d DU . . H20A H 0.2354 0.1834 -0.3604 0.097 Uiso 1 1 calc R . . H20B H 0.2729 0.1330 -0.4175 0.097 Uiso 1 1 calc R . . H20C H 0.3099 0.1788 -0.3520 0.097 Uiso 1 1 calc R . . C21 C 0.1835(6) -0.1813(5) 0.0760(8) 0.029(2) Uani 1 1 d DU . . H21A H 0.1803 -0.1834 0.1426 0.035 Uiso 1 1 calc R . . H21B H 0.1519 -0.1513 0.0550 0.035 Uiso 1 1 calc R . . C22 C 0.1664(5) -0.2441(6) 0.0380(9) 0.033(3) Uani 1 1 d DU . . H22A H 0.1992 -0.2742 0.0546 0.040 Uiso 1 1 calc R . . H22B H 0.1647 -0.2417 -0.0286 0.040 Uiso 1 1 calc R . . C23 C 0.1035(6) -0.2660(6) 0.0740(10) 0.037(3) Uani 1 1 d DU . . H23A H 0.0705 -0.2364 0.0560 0.044 Uiso 1 1 calc R . . H23B H 0.1049 -0.2673 0.1407 0.044 Uiso 1 1 calc R . . C24 C 0.0872(7) -0.3299(6) 0.0376(12) 0.042(4) Uani 1 1 d DU . . H24A H 0.1043 -0.3345 -0.0234 0.064 Uiso 1 1 calc R . . H24B H 0.0416 -0.3347 0.0357 0.064 Uiso 1 1 calc R . . H24C H 0.1052 -0.3614 0.0771 0.064 Uiso 1 1 calc R . . C25 C 0.2695(8) -0.1486(7) -0.0718(8) 0.044(3) Uani 1 1 d DU . . H25A H 0.3138 -0.1395 -0.0856 0.053 Uiso 1 1 calc R . . H25B H 0.2597 -0.1896 -0.0973 0.053 Uiso 1 1 calc R . . C26 C 0.2290(10) -0.1012(9) -0.1174(11) 0.071(4) Uani 1 1 d DU . . H26A H 0.2292 -0.0629 -0.0813 0.085 Uiso 1 1 calc R . . H26B H 0.1854 -0.1165 -0.1201 0.085 Uiso 1 1 calc R . . C27 C 0.2521(7) -0.0870(8) -0.2143(11) 0.061(4) Uani 1 1 d DU . . H27A H 0.2299 -0.0503 -0.2375 0.073 Uiso 1 1 calc R . . H27B H 0.2973 -0.0774 -0.2126 0.073 Uiso 1 1 calc R . . C28 C 0.2411(10) -0.1407(9) -0.2779(12) 0.073(6) Uani 1 1 d DU . . H28A H 0.2743 -0.1713 -0.2698 0.109 Uiso 1 1 calc R . . H28B H 0.2414 -0.1259 -0.3403 0.109 Uiso 1 1 calc R . . H28C H 0.2005 -0.1596 -0.2645 0.109 Uiso 1 1 calc R . . C1A C 0.1525(5) 0.0193(6) 0.4308(6) 0.020(2) Uani 1 1 d DU . . H1C H 0.1794 -0.0174 0.4226 0.024 Uiso 1 1 calc R . . H1D H 0.1801 0.0537 0.4491 0.024 Uiso 1 1 calc R . . C2A C 0.1071(5) 0.0063(5) 0.5085(6) 0.023(2) Uani 1 1 d DU . . H2C H 0.0829 -0.0315 0.4951 0.027 Uiso 1 1 calc R . . H2D H 0.0773 0.0409 0.5142 0.027 Uiso 1 1 calc R . . C3A C 0.1424(7) -0.0021(7) 0.5982(7) 0.037(3) Uani 1 1 d DU . . H3C H 0.1699 0.0339 0.6085 0.045 Uiso 1 1 calc R . . H3D H 0.1691 -0.0392 0.5946 0.045 Uiso 1 1 calc R . . C4A C 0.0966(7) -0.0087(8) 0.6783(8) 0.044(4) Uani 1 1 d DU . . H4D H 0.0638 0.0226 0.6735 0.066 Uiso 1 1 calc R . . H4E H 0.1194 -0.0032 0.7351 0.066 Uiso 1 1 calc R . . H4F H 0.0776 -0.0497 0.6771 0.066 Uiso 1 1 calc R . . C5A C 0.0802(5) 0.1108(5) 0.3367(7) 0.024(2) Uani 1 1 d DU . . H5C H 0.0464 0.1064 0.3820 0.029 Uiso 1 1 calc R . . H5D H 0.1106 0.1411 0.3604 0.029 Uiso 1 1 calc R . . C6A C 0.0516(5) 0.1362(5) 0.2478(7) 0.025(2) Uani 1 1 d DU . . H6C H 0.0855 0.1442 0.2039 0.030 Uiso 1 1 calc R . . H6D H 0.0233 0.1049 0.2215 0.030 Uiso 1 1 calc R . . C7A C 0.0150(6) 0.1958(6) 0.2645(8) 0.033(3) Uani 1 1 d DU . . H7C H 0.0430 0.2255 0.2951 0.040 Uiso 1 1 calc R . . H7D H 0.0035 0.2137 0.2053 0.040 Uiso 1 1 calc R . . C8A C -0.0443(7) 0.1889(7) 0.3206(10) 0.047(4) Uani 1 1 d DU . . H8D H -0.0725 0.2233 0.3081 0.071 Uiso 1 1 calc R . . H8E H -0.0334 0.1887 0.3849 0.071 Uiso 1 1 calc R . . H8F H -0.0651 0.1501 0.3050 0.071 Uiso 1 1 calc R . . C9A C 0.0590(6) -0.0162(5) 0.2960(8) 0.023(2) Uani 1 1 d DU . . H9C H 0.0259 -0.0139 0.3425 0.028 Uiso 1 1 calc R . . H9D H 0.0401 -0.0039 0.2378 0.028 Uiso 1 1 calc R . . C10A C 0.0810(5) -0.0832(5) 0.2884(8) 0.024(2) Uani 1 1 d DU . . H10C H 0.1168 -0.0850 0.2462 0.029 Uiso 1 1 calc R . . H10D H 0.0960 -0.0970 0.3482 0.029 Uiso 1 1 calc R . . C11A C 0.0307(6) -0.1273(6) 0.2558(8) 0.031(3) Uani 1 1 d DU . . H11C H 0.0493 -0.1688 0.2495 0.037 Uiso 1 1 calc R . . H11D H 0.0166 -0.1140 0.1953 0.037 Uiso 1 1 calc R . . C12A C -0.0263(6) -0.1318(6) 0.3178(8) 0.034(3) Uani 1 1 d DU . . H12D H -0.0127 -0.1422 0.3791 0.051 Uiso 1 1 calc R . . H12E H -0.0546 -0.1638 0.2954 0.051 Uiso 1 1 calc R . . H12F H -0.0482 -0.0922 0.3187 0.051 Uiso 1 1 calc R . . C13A C 0.2840(5) 0.1923(5) 0.0182(8) 0.025(2) Uani 1 1 d DU . . H13A H 0.2833 0.2243 -0.0293 0.030 Uiso 1 1 calc R . . H13B H 0.2723 0.2122 0.0759 0.030 Uiso 1 1 calc R . . C14A C 0.3510(5) 0.1672(5) 0.0266(9) 0.031(2) Uani 1 1 d DU . . H14A H 0.3652 0.1522 -0.0331 0.037 Uiso 1 1 calc R . . H14B H 0.3512 0.1318 0.0687 0.037 Uiso 1 1 calc R . . C15A C 0.3971(6) 0.2164(5) 0.0610(8) 0.032(3) Uani 1 1 d DU . . H15C H 0.3827 0.2307 0.1209 0.039 Uiso 1 1 calc R . . H15D H 0.4385 0.1968 0.0694 0.039 Uiso 1 1 calc R . . C16A C 0.4052(8) 0.2722(7) 0.0000(7) 0.041(4) Uani 1 1 d DU . . H16D H 0.4201 0.2588 -0.0594 0.062 Uiso 1 1 calc R . . H16E H 0.4357 0.3004 0.0268 0.062 Uiso 1 1 calc R . . H16F H 0.3649 0.2933 -0.0067 0.062 Uiso 1 1 calc R . . C21A C 0.3220(7) -0.2010(6) 0.0945(9) 0.037(3) Uani 1 1 d DU . . H21C H 0.3599 -0.1754 0.1024 0.045 Uiso 1 1 calc R . . H21D H 0.3087 -0.2146 0.1553 0.045 Uiso 1 1 calc R . . C22A C 0.3405(6) -0.2578(6) 0.0413(9) 0.037(3) Uani 1 1 d DU . . H22C H 0.3485 -0.2462 -0.0223 0.044 Uiso 1 1 calc R . . H22D H 0.3057 -0.2879 0.0422 0.044 Uiso 1 1 calc R . . C23A C 0.3993(7) -0.2871(7) 0.0818(9) 0.042(3) Uani 1 1 d DU . . H23C H 0.4341 -0.2572 0.0790 0.050 Uiso 1 1 calc R . . H23D H 0.3915 -0.2970 0.1460 0.050 Uiso 1 1 calc R . . C24A C 0.4179(8) -0.3451(7) 0.0325(11) 0.048(4) Uani 1 1 d DU . . H24D H 0.3832 -0.3745 0.0338 0.072 Uiso 1 1 calc R . . H24E H 0.4546 -0.3633 0.0619 0.072 Uiso 1 1 calc R . . H24F H 0.4282 -0.3351 -0.0303 0.072 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 Th1 0.0137(2) 0.0225(2) 0.01082(15) 0.0008(2) -0.00024(14) 0.00010(14) Tc1 0.0198(5) 0.0302(6) 0.0185(5) 0.0007(4) 0.0049(4) 0.0026(4) Tc2 0.0237(5) 0.0251(5) 0.0142(4) -0.0025(4) -0.0011(4) 0.0006(4) Tc3 0.0240(6) 0.0324(6) 0.0185(5) 0.0095(4) 0.0016(4) 0.0034(4) Tc1A 0.0170(5) 0.0321(6) 0.0154(4) -0.0025(5) -0.0026(4) 0.0000(4) P1 0.0220(16) 0.0293(17) 0.0204(15) 0.0017(11) -0.0042(12) -0.0012(12) P2 0.0283(17) 0.0233(16) 0.0128(13) -0.0002(11) 0.0004(12) 0.0011(12) P3 0.0345(19) 0.0276(17) 0.0332(18) -0.0080(14) 0.0086(15) -0.0056(14) P1A 0.0192(16) 0.0300(16) 0.0135(12) -0.0023(11) 0.0027(10) -0.0001(11) O1 0.032(3) 0.039(4) 0.026(3) 0.003(3) 0.014(3) 0.007(3) O2 0.035(4) 0.052(5) 0.049(5) -0.003(5) 0.000(4) -0.012(4) O3 0.050(7) 0.063(7) 0.021(3) 0.004(4) 0.009(3) 0.000(5) O4 0.045(6) 0.036(4) 0.041(6) -0.001(4) 0.012(5) 0.011(4) O5 0.023(3) 0.034(4) 0.033(4) -0.002(3) -0.010(3) 0.001(2) O6 0.025(4) 0.037(3) 0.018(3) -0.007(3) 0.002(3) 0.001(2) O7 0.065(7) 0.058(7) 0.005(3) -0.001(3) 0.008(3) -0.011(5) O8 0.041(4) 0.045(5) 0.026(4) -0.009(4) 0.005(4) -0.010(4) O9 0.026(4) 0.032(3) 0.015(3) 0.003(2) 0.002(3) 0.002(3) O10 0.029(4) 0.046(4) 0.028(3) 0.018(3) 0.003(3) 0.008(3) O11 0.037(4) 0.060(6) 0.034(5) 0.011(5) 0.003(4) 0.022(4) O12 0.053(6) 0.043(6) 0.017(3) 0.006(3) 0.005(4) 0.003(5) O13 0.027(4) 0.032(3) 0.043(4) -0.012(3) 0.002(4) 0.001(3) O1A 0.026(3) 0.036(4) 0.024(3) -0.004(3) -0.009(3) 0.000(3) O2A 0.033(5) 0.056(5) 0.029(4) -0.014(4) -0.001(4) 0.014(4) O3A 0.038(6) 0.060(6) 0.025(4) 0.013(4) 0.005(3) 0.008(4) O4A 0.049(6) 0.045(5) 0.037(6) 0.001(4) -0.020(4) -0.014(4) O5A 0.027(3) 0.034(4) 0.016(3) -0.002(3) 0.007(3) 0.002(3) O8A 0.042(5) 0.045(6) 0.023(4) -0.003(4) -0.003(4) 0.009(4) O11A 0.061(5) 0.044(5) 0.027(5) -0.002(4) -0.007(5) -0.006(4) C1 0.019(6) 0.040(7) 0.026(3) 0.001(4) 0.000(3) -0.001(5) C2 0.018(6) 0.047(7) 0.026(4) 0.000(5) -0.005(4) 0.004(5) C3 0.035(7) 0.052(8) 0.027(5) -0.007(6) 0.002(4) 0.000(6) C4 0.053(10) 0.082(12) 0.018(5) -0.016(7) -0.006(6) 0.011(9) C5 0.025(6) 0.034(4) 0.021(5) 0.001(4) -0.003(4) -0.003(3) C6 0.030(6) 0.034(5) 0.024(6) 0.007(5) -0.009(5) -0.004(4) C7 0.025(6) 0.033(5) 0.027(6) -0.001(5) -0.004(5) -0.004(4) C8 0.045(8) 0.050(8) 0.030(7) 0.015(6) -0.010(6) -0.024(6) C9 0.024(5) 0.039(4) 0.021(5) 0.002(5) -0.002(4) 0.006(4) C10 0.038(6) 0.039(5) 0.024(6) -0.001(5) -0.006(5) 0.002(4) C11 0.047(7) 0.031(6) 0.028(6) -0.004(5) 0.003(5) -0.002(5) C12 0.042(8) 0.056(10) 0.057(10) -0.006(8) -0.007(7) 0.016(7) C13 0.026(4) 0.031(6) 0.026(6) 0.003(4) -0.002(4) 0.003(4) C14 0.029(6) 0.046(6) 0.018(5) -0.002(5) 0.002(5) 0.009(4) C15 0.022(6) 0.044(6) 0.028(5) 0.006(5) 0.006(5) 0.003(4) C16 0.045(9) 0.039(7) 0.037(7) 0.008(5) 0.006(6) 0.011(5) C17 0.033(7) 0.034(6) 0.013(3) -0.003(3) -0.003(4) 0.001(5) C18 0.043(8) 0.040(7) 0.013(3) 0.000(4) 0.006(5) 0.006(5) C19 0.079(10) 0.037(7) 0.014(4) -0.001(4) 0.000(6) -0.001(7) C20 0.139(17) 0.047(9) 0.009(5) -0.002(5) 0.005(8) -0.012(11) C21 0.028(5) 0.035(6) 0.023(5) 0.002(5) 0.003(4) -0.002(4) C22 0.026(6) 0.042(6) 0.032(6) -0.005(5) 0.007(5) -0.005(4) C23 0.022(6) 0.039(7) 0.049(8) -0.014(6) 0.006(5) -0.004(4) C24 0.033(8) 0.027(6) 0.068(10) -0.008(7) 0.009(7) 0.002(5) C25 0.059(9) 0.048(8) 0.027(4) 0.002(4) 0.011(5) -0.007(7) C26 0.089(11) 0.080(11) 0.044(5) -0.007(6) -0.019(7) 0.020(9) C27 0.075(12) 0.057(9) 0.051(7) 0.007(6) -0.026(8) 0.007(8) C28 0.098(16) 0.081(13) 0.040(8) -0.005(8) -0.038(9) 0.015(11) C1A 0.019(6) 0.023(6) 0.018(3) -0.001(4) -0.002(3) -0.002(4) C2A 0.027(6) 0.024(6) 0.017(4) 0.000(4) -0.001(4) -0.001(4) C3A 0.039(8) 0.056(8) 0.017(4) 0.000(5) -0.006(4) -0.004(6) C4A 0.034(8) 0.081(11) 0.016(5) 0.004(6) -0.008(5) -0.002(7) C5A 0.022(6) 0.028(4) 0.021(5) 0.002(4) 0.000(4) 0.003(3) C6A 0.019(6) 0.039(6) 0.018(5) 0.010(4) 0.007(4) 0.001(4) C7A 0.042(7) 0.037(6) 0.020(5) 0.006(5) -0.008(5) 0.006(5) C8A 0.047(8) 0.048(9) 0.048(9) -0.005(7) 0.009(6) 0.024(6) C9A 0.029(5) 0.027(4) 0.012(5) 0.000(4) -0.010(4) 0.001(4) C10A 0.032(5) 0.027(4) 0.014(5) 0.003(4) 0.004(5) 0.000(4) C11A 0.038(7) 0.029(5) 0.027(6) -0.006(5) 0.007(5) -0.004(5) C12A 0.036(6) 0.045(8) 0.021(6) 0.001(6) 0.003(5) -0.009(6) C13A 0.027(4) 0.035(6) 0.013(4) 0.002(4) -0.003(4) -0.004(4) C14A 0.031(4) 0.033(6) 0.028(6) -0.003(5) -0.005(5) 0.002(4) C15A 0.035(6) 0.040(6) 0.021(5) -0.002(4) -0.008(5) -0.007(5) C16A 0.058(10) 0.049(8) 0.017(7) 0.002(5) 0.005(6) -0.014(7) C21A 0.034(6) 0.038(6) 0.039(6) -0.010(5) -0.003(5) 0.002(4) C22A 0.037(7) 0.048(6) 0.024(6) -0.006(5) -0.005(5) 0.006(5) C23A 0.042(8) 0.059(8) 0.024(6) 0.003(5) -0.001(5) 0.017(6) C24A 0.046(9) 0.059(9) 0.039(8) -0.011(7) -0.007(7) 0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Th1 O13 2.336(9) . ? Th1 O9 2.347(8) . ? Th1 O5A 2.367(8) . ? Th1 O5 2.372(8) . ? Th1 O10 2.440(9) . ? Th1 O6 2.447(9) . ? Th1 O1A 2.449(8) . ? Th1 O1 2.465(8) . ? Tc1 O4 1.693(10) . ? Tc1 O2 1.694(10) . ? Tc1 O3 1.702(9) . ? Tc1 O1 1.758(8) . ? Tc2 O8A 1.684(9) . ? Tc2 O8 1.707(9) . ? Tc2 O7 1.723(9) . ? Tc2 O6 1.749(8) . ? Tc3 O11A 1.676(10) . ? Tc3 O11 1.695(10) . ? Tc3 O12 1.706(9) . ? Tc3 O10 1.756(9) . ? Tc1A O4A 1.676(10) . ? Tc1A O3A 1.688(10) . ? Tc1A O2A 1.701(9) . ? Tc1A O1A 1.751(9) . ? P1 O5 1.510(9) . ? P1 C1 1.772(13) . ? P1 C5 1.798(12) . ? P1 C9 1.810(12) . ? P2 O9 1.519(8) . ? P2 C17 1.785(12) . ? P2 C13A 1.803(10) . ? P2 C13 1.826(10) . ? P3 O13 1.500(9) . ? P3 C25 1.791(12) . ? P3 C21 1.802(13) . ? P3 C21A 1.845(14) . ? P1A O5A 1.516(8) . ? P1A C1A 1.785(10) . ? P1A C9A 1.787(12) . ? P1A C5A 1.791(10) . ? C1 C2 1.540(13) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.538(13) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.538(14) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.539(12) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.527(13) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.521(13) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.522(14) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.513(13) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.508(14) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.524(13) . ? C13 H13C 0.9900 . ? C13 H13D 0.9900 . ? C14 C15 1.530(13) . ? C14 H14C 0.9900 . ? C14 H14D 0.9900 . ? C15 C16 1.501(14) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.546(13) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.523(13) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.538(14) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.521(13) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.524(13) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.531(13) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.506(16) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.550(16) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.518(16) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C1A C2A 1.534(12) . ? C1A H1C 0.9900 . ? C1A H1D 0.9900 . ? C2A C3A 1.539(13) . ? C2A H2C 0.9900 . ? C2A H2D 0.9900 . ? C3A C4A 1.544(14) . ? C3A H3C 0.9900 . ? C3A H3D 0.9900 . ? C4A H4D 0.9800 . ? C4A H4E 0.9800 . ? C4A H4F 0.9800 . ? C5A C6A 1.554(12) . ? C5A H5C 0.9900 . ? C5A H5D 0.9900 . ? C6A C7A 1.533(13) . ? C6A H6C 0.9900 . ? C6A H6D 0.9900 . ? C7A C8A 1.525(14) . ? C7A H7C 0.9900 . ? C7A H7D 0.9900 . ? C8A H8D 0.9800 . ? C8A H8E 0.9800 . ? C8A H8F 0.9800 . ? C9A C10A 1.535(12) . ? C9A H9C 0.9900 . ? C9A H9D 0.9900 . ? C10A C11A 1.519(13) . ? C10A H10C 0.9900 . ? C10A H10D 0.9900 . ? C11A C12A 1.530(13) . ? C11A H11C 0.9900 . ? C11A H11D 0.9900 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13A C14A 1.539(13) . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C14A C15A 1.541(13) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A C16A 1.523(13) . ? C15A H15C 0.9900 . ? C15A H15D 0.9900 . ? C16A H16D 0.9800 . ? C16A H16E 0.9800 . ? C16A H16F 0.9800 . ? C21A C22A 1.515(13) . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? C22A C23A 1.533(14) . ? C22A H22C 0.9900 . ? C22A H22D 0.9900 . ? C23A C24A 1.510(14) . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? 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 O13 Th1 O9 117.6(3) . . ? O13 Th1 O5A 131.2(3) . . ? O9 Th1 O5A 83.1(3) . . ? O13 Th1 O5 83.6(3) . . ? O9 Th1 O5 127.2(3) . . ? O5A Th1 O5 120.1(3) . . ? O13 Th1 O10 75.6(4) . . ? O9 Th1 O10 154.5(3) . . ? O5A Th1 O10 72.5(3) . . ? O5 Th1 O10 73.6(3) . . ? O13 Th1 O6 153.8(3) . . ? O9 Th1 O6 73.5(3) . . ? O5A Th1 O6 71.3(3) . . ? O5 Th1 O6 71.7(3) . . ? O10 Th1 O6 104.7(3) . . ? O13 Th1 O1A 71.3(3) . . ? O9 Th1 O1A 74.4(3) . . ? O5A Th1 O1A 73.5(3) . . ? O5 Th1 O1A 153.3(3) . . ? O10 Th1 O1A 91.1(3) . . ? O6 Th1 O1A 134.4(3) . . ? O13 Th1 O1 71.2(3) . . ? O9 Th1 O1 70.4(3) . . ? O5A Th1 O1 152.2(3) . . ? O5 Th1 O1 73.1(3) . . ? O10 Th1 O1 134.8(3) . . ? O6 Th1 O1 92.8(3) . . ? O1A Th1 O1 105.9(3) . . ? O4 Tc1 O2 109.6(5) . . ? O4 Tc1 O3 109.5(5) . . ? O2 Tc1 O3 108.2(5) . . ? O4 Tc1 O1 111.2(4) . . ? O2 Tc1 O1 110.3(5) . . ? O3 Tc1 O1 107.9(5) . . ? O8A Tc2 O8 109.6(5) . . ? O8A Tc2 O7 109.1(5) . . ? O8 Tc2 O7 109.8(5) . . ? O8A Tc2 O6 110.0(4) . . ? O8 Tc2 O6 107.7(4) . . ? O7 Tc2 O6 110.6(5) . . ? O11A Tc3 O11 110.4(5) . . ? O11A Tc3 O12 108.7(5) . . ? O11 Tc3 O12 108.6(5) . . ? O11A Tc3 O10 110.1(5) . . ? O11 Tc3 O10 110.2(5) . . ? O12 Tc3 O10 108.9(5) . . ? O4A Tc1A O3A 109.0(5) . . ? O4A Tc1A O2A 109.5(5) . . ? O3A Tc1A O2A 109.9(5) . . ? O4A Tc1A O1A 108.3(5) . . ? O3A Tc1A O1A 110.5(5) . . ? O2A Tc1A O1A 109.7(4) . . ? O5 P1 C1 110.4(6) . . ? O5 P1 C5 110.1(5) . . ? C1 P1 C5 109.4(6) . . ? O5 P1 C9 111.2(5) . . ? C1 P1 C9 106.9(6) . . ? C5 P1 C9 108.8(6) . . ? O9 P2 C17 111.4(5) . . ? O9 P2 C13A 111.3(5) . . ? C17 P2 C13A 110.1(6) . . ? O9 P2 C13 109.9(6) . . ? C17 P2 C13 105.7(6) . . ? C13A P2 C13 108.2(6) . . ? O13 P3 C25 111.2(7) . . ? O13 P3 C21 110.7(6) . . ? C25 P3 C21 110.2(7) . . ? O13 P3 C21A 105.9(6) . . ? C25 P3 C21A 107.8(7) . . ? C21 P3 C21A 110.9(7) . . ? O5A P1A C1A 110.2(5) . . ? O5A P1A C9A 111.4(5) . . ? C1A P1A C9A 110.2(5) . . ? O5A P1A C5A 111.7(5) . . ? C1A P1A C5A 107.2(5) . . ? C9A P1A C5A 106.1(5) . . ? Tc1 O1 Th1 146.8(5) . . ? P1 O5 Th1 157.8(6) . . ? Tc2 O6 Th1 147.3(5) . . ? P2 O9 Th1 156.1(5) . . ? Tc3 O10 Th1 158.5(5) . . ? P3 O13 Th1 162.7(6) . . ? Tc1A O1A Th1 148.8(5) . . ? P1A O5A Th1 158.3(5) . . ? C2 C1 P1 115.2(9) . . ? C2 C1 H1A 108.5 . . ? P1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? P1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C3 C2 C1 112.1(10) . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C4 C3 C2 112.0(11) . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 P1 116.7(8) . . ? C6 C5 H5A 108.1 . . ? P1 C5 H5A 108.1 . . ? C6 C5 H5B 108.1 . . ? P1 C5 H5B 108.1 . . ? H5A C5 H5B 107.3 . . ? C7 C6 C5 110.6(9) . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C6 110.3(10) . . ? C8 C7 H7A 109.6 . . ? C6 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P1 113.1(9) . . ? C10 C9 H9A 109.0 . . ? P1 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? P1 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C11 C10 C9 112.3(11) . . ? C11 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? C11 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C10 114.2(11) . . ? C12 C11 H11A 108.7 . . ? C10 C11 H11A 108.7 . . ? C12 C11 H11B 108.7 . . ? C10 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 P2 114.6(8) . . ? C14 C13 H13C 108.6 . . ? P2 C13 H13C 108.6 . . ? C14 C13 H13D 108.6 . . ? P2 C13 H13D 108.6 . . ? H13C C13 H13D 107.6 . . ? C13 C14 C15 113.4(10) . . ? C13 C14 H14C 108.9 . . ? C15 C14 H14C 108.9 . . ? C13 C14 H14D 108.9 . . ? C15 C14 H14D 108.9 . . ? H14C C14 H14D 107.7 . . ? C16 C15 C14 112.6(11) . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 P2 115.0(9) . . ? C18 C17 H17A 108.5 . . ? P2 C17 H17A 108.5 . . ? C18 C17 H17B 108.5 . . ? P2 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C19 C18 C17 112.0(10) . . ? C19 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? C19 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C18 C19 C20 110.0(11) . . ? C18 C19 H19A 109.7 . . ? C20 C19 H19A 109.7 . . ? C18 C19 H19B 109.7 . . ? C20 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 P3 117.1(9) . . ? C22 C21 H21A 108.0 . . ? P3 C21 H21A 108.0 . . ? C22 C21 H21B 108.0 . . ? P3 C21 H21B 108.0 . . ? H21A C21 H21B 107.3 . . ? C21 C22 C23 111.3(10) . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C24 111.2(11) . . ? C22 C23 H23A 109.4 . . ? C24 C23 H23A 109.4 . . ? C22 C23 H23B 109.4 . . ? C24 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 P3 113.7(11) . . ? C26 C25 H25A 108.8 . . ? P3 C25 H25A 108.8 . . ? C26 C25 H25B 108.8 . . ? P3 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C25 C26 C27 111.6(14) . . ? C25 C26 H26A 109.3 . . ? C27 C26 H26A 109.3 . . ? C25 C26 H26B 109.3 . . ? C27 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C26 111.8(15) . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27B 109.3 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C2A C1A P1A 116.8(8) . . ? C2A C1A H1C 108.1 . . ? P1A C1A H1C 108.1 . . ? C2A C1A H1D 108.1 . . ? P1A C1A H1D 108.1 . . ? H1C C1A H1D 107.3 . . ? C1A C2A C3A 111.1(9) . . ? C1A C2A H2C 109.4 . . ? C3A C2A H2C 109.4 . . ? C1A C2A H2D 109.4 . . ? C3A C2A H2D 109.4 . . ? H2C C2A H2D 108.0 . . ? C2A C3A C4A 111.4(10) . . ? C2A C3A H3C 109.3 . . ? C4A C3A H3C 109.3 . . ? C2A C3A H3D 109.3 . . ? C4A C3A H3D 109.3 . . ? H3C C3A H3D 108.0 . . ? C3A C4A H4D 109.5 . . ? C3A C4A H4E 109.5 . . ? H4D C4A H4E 109.5 . . ? C3A C4A H4F 109.5 . . ? H4D C4A H4F 109.5 . . ? H4E C4A H4F 109.5 . . ? C6A C5A P1A 114.0(8) . . ? C6A C5A H5C 108.8 . . ? P1A C5A H5C 108.8 . . ? C6A C5A H5D 108.8 . . ? P1A C5A H5D 108.8 . . ? H5C C5A H5D 107.7 . . ? C7A C6A C5A 111.4(9) . . ? C7A C6A H6C 109.3 . . ? C5A C6A H6C 109.3 . . ? C7A C6A H6D 109.3 . . ? C5A C6A H6D 109.3 . . ? H6C C6A H6D 108.0 . . ? C8A C7A C6A 115.4(10) . . ? C8A C7A H7C 108.4 . . ? C6A C7A H7C 108.4 . . ? C8A C7A H7D 108.4 . . ? C6A C7A H7D 108.4 . . ? H7C C7A H7D 107.5 . . ? C7A C8A H8D 109.5 . . ? C7A C8A H8E 109.5 . . ? H8D C8A H8E 109.5 . . ? C7A C8A H8F 109.5 . . ? H8D C8A H8F 109.5 . . ? H8E C8A H8F 109.5 . . ? C10A C9A P1A 115.1(8) . . ? C10A C9A H9C 108.5 . . ? P1A C9A H9C 108.5 . . ? C10A C9A H9D 108.5 . . ? P1A C9A H9D 108.5 . . ? H9C C9A H9D 107.5 . . ? C11A C10A C9A 113.9(9) . . ? C11A C10A H10C 108.8 . . ? C9A C10A H10C 108.8 . . ? C11A C10A H10D 108.8 . . ? C9A C10A H10D 108.8 . . ? H10C C10A H10D 107.7 . . ? C10A C11A C12A 114.5(9) . . ? C10A C11A H11C 108.6 . . ? C12A C11A H11C 108.6 . . ? C10A C11A H11D 108.6 . . ? C12A C11A H11D 108.6 . . ? H11C C11A H11D 107.6 . . ? C11A C12A H12D 109.5 . . ? C11A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C11A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C14A C13A P2 114.2(8) . . ? C14A C13A H13A 108.7 . . ? P2 C13A H13A 108.7 . . ? C14A C13A H13B 108.7 . . ? P2 C13A H13B 108.7 . . ? H13A C13A H13B 107.6 . . ? C13A C14A C15A 112.1(10) . . ? C13A C14A H14A 109.2 . . ? C15A C14A H14A 109.2 . . ? C13A C14A H14B 109.2 . . ? C15A C14A H14B 109.2 . . ? H14A C14A H14B 107.9 . . ? C16A C15A C14A 115.4(11) . . ? C16A C15A H15C 108.4 . . ? C14A C15A H15C 108.4 . . ? C16A C15A H15D 108.4 . . ? C14A C15A H15D 108.4 . . ? H15C C15A H15D 107.5 . . ? C15A C16A H16D 109.5 . . ? C15A C16A H16E 109.5 . . ? H16D C16A H16E 109.5 . . ? C15A C16A H16F 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? C22A C21A P3 118.0(9) . . ? C22A C21A H21C 107.8 . . ? P3 C21A H21C 107.8 . . ? C22A C21A H21D 107.8 . . ? P3 C21A H21D 107.8 . . ? H21C C21A H21D 107.1 . . ? C21A C22A C23A 110.4(10) . . ? C21A C22A H22C 109.6 . . ? C23A C22A H22C 109.6 . . ? C21A C22A H22D 109.6 . . ? C23A C22A H22D 109.6 . . ? H22C C22A H22D 108.1 . . ? C24A C23A C22A 112.0(11) . . ? C24A C23A H23C 109.2 . . ? C22A C23A H23C 109.2 . . ? C24A C23A H23D 109.2 . . ? C22A C23A H23D 109.2 . . ? H23C C23A H23D 107.9 . . ? C23A C24A H24D 109.5 . . ? C23A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C23A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Tc1 O1 Th1 28.1(11) . . . . ? O2 Tc1 O1 Th1 -93.8(10) . . . . ? O3 Tc1 O1 Th1 148.3(9) . . . . ? O13 Th1 O1 Tc1 -51.4(9) . . . . ? O9 Th1 O1 Tc1 178.8(10) . . . . ? O5A Th1 O1 Tc1 160.8(7) . . . . ? O5 Th1 O1 Tc1 37.6(9) . . . . ? O10 Th1 O1 Tc1 -6.5(12) . . . . ? O6 Th1 O1 Tc1 107.4(10) . . . . ? O1A Th1 O1 Tc1 -114.7(9) . . . . ? C1 P1 O5 Th1 82.1(16) . . . . ? C5 P1 O5 Th1 -38.8(17) . . . . ? C9 P1 O5 Th1 -159.4(14) . . . . ? O13 Th1 O5 P1 174.1(16) . . . . ? O9 Th1 O5 P1 54.1(17) . . . . ? O5A Th1 O5 P1 -51.3(16) . . . . ? O10 Th1 O5 P1 -109.1(16) . . . . ? O6 Th1 O5 P1 3.0(15) . . . . ? O1A Th1 O5 P1 -166.2(12) . . . . ? O1 Th1 O5 P1 101.9(16) . . . . ? O8A Tc2 O6 Th1 -47.2(10) . . . . ? O8 Tc2 O6 Th1 -166.6(8) . . . . ? O7 Tc2 O6 Th1 73.4(9) . . . . ? O13 Th1 O6 Tc2 -170.9(7) . . . . ? O9 Th1 O6 Tc2 69.7(8) . . . . ? O5A Th1 O6 Tc2 -18.5(8) . . . . ? O5 Th1 O6 Tc2 -150.5(9) . . . . ? O10 Th1 O6 Tc2 -83.8(9) . . . . ? O1A Th1 O6 Tc2 22.8(11) . . . . ? O1 Th1 O6 Tc2 138.3(9) . . . . ? C17 P2 O9 Th1 53.4(14) . . . . ? C13A P2 O9 Th1 -69.8(14) . . . . ? C13 P2 O9 Th1 170.3(12) . . . . ? O13 Th1 O9 P2 -62.4(13) . . . . ? O5A Th1 O9 P2 164.3(13) . . . . ? O5 Th1 O9 P2 41.5(14) . . . . ? O10 Th1 O9 P2 -178.5(10) . . . . ? O6 Th1 O9 P2 91.9(13) . . . . ? O1A Th1 O9 P2 -121.0(13) . . . . ? O1 Th1 O9 P2 -7.3(12) . . . . ? O11A Tc3 O10 Th1 -90.7(16) . . . . ? O11 Tc3 O10 Th1 31.3(17) . . . . ? O12 Tc3 O10 Th1 150.3(15) . . . . ? O13 Th1 O10 Tc3 33.8(15) . . . . ? O9 Th1 O10 Tc3 158.5(12) . . . . ? O5A Th1 O10 Tc3 176.4(16) . . . . ? O5 Th1 O10 Tc3 -53.7(15) . . . . ? O6 Th1 O10 Tc3 -119.1(15) . . . . ? O1A Th1 O10 Tc3 104.1(16) . . . . ? O1 Th1 O10 Tc3 -9.8(18) . . . . ? C25 P3 O13 Th1 107(2) . . . . ? C21 P3 O13 Th1 -16(2) . . . . ? C21A P3 O13 Th1 -137(2) . . . . ? O9 Th1 O13 P3 -82(2) . . . . ? O5A Th1 O13 P3 24(2) . . . . ? O5 Th1 O13 P3 149(2) . . . . ? O10 Th1 O13 P3 74(2) . . . . ? O6 Th1 O13 P3 168.3(18) . . . . ? O1A Th1 O13 P3 -22(2) . . . . ? O1 Th1 O13 P3 -137(2) . . . . ? O4A Tc1A O1A Th1 176.2(9) . . . . ? O3A Tc1A O1A Th1 56.9(10) . . . . ? O2A Tc1A O1A Th1 -64.4(10) . . . . ? O13 Th1 O1A Tc1A -130.9(10) . . . . ? O9 Th1 O1A Tc1A -4.0(9) . . . . ? O5A Th1 O1A Tc1A 83.3(9) . . . . ? O5 Th1 O1A Tc1A -151.6(7) . . . . ? O10 Th1 O1A Tc1A 154.7(9) . . . . ? O6 Th1 O1A Tc1A 42.7(11) . . . . ? O1 Th1 O1A Tc1A -67.7(10) . . . . ? C1A P1A O5A Th1 58.5(15) . . . . ? C9A P1A O5A Th1 -64.0(15) . . . . ? C5A P1A O5A Th1 177.5(13) . . . . ? O13 Th1 O5A P1A 38.3(16) . . . . ? O9 Th1 O5A P1A 159.3(14) . . . . ? O5 Th1 O5A P1A -71.4(15) . . . . ? O10 Th1 O5A P1A -13.1(14) . . . . ? O6 Th1 O5A P1A -125.9(14) . . . . ? O1A Th1 O5A P1A 83.5(14) . . . . ? O1 Th1 O5A P1A 176.3(11) . . . . ? O5 P1 C1 C2 -59.3(11) . . . . ? C5 P1 C1 C2 62.0(11) . . . . ? C9 P1 C1 C2 179.6(10) . . . . ? P1 C1 C2 C3 167.9(9) . . . . ? C1 C2 C3 C4 66.6(16) . . . . ? O5 P1 C5 C6 176.6(9) . . . . ? C1 P1 C5 C6 55.1(11) . . . . ? C9 P1 C5 C6 -61.3(11) . . . . ? P1 C5 C6 C7 -178.3(9) . . . . ? C5 C6 C7 C8 -179.6(11) . . . . ? O5 P1 C9 C10 -48.7(10) . . . . ? C1 P1 C9 C10 71.9(10) . . . . ? C5 P1 C9 C10 -170.1(8) . . . . ? P1 C9 C10 C11 -177.7(8) . . . . ? C9 C10 C11 C12 66.8(16) . . . . ? O9 P2 C13 C14 88.5(10) . . . . ? C17 P2 C13 C14 -151.2(10) . . . . ? C13A P2 C13 C14 -33.3(11) . . . . ? P2 C13 C14 C15 -177.8(9) . . . . ? C13 C14 C15 C16 -177.0(11) . . . . ? O9 P2 C17 C18 -178.2(8) . . . . ? C13A P2 C17 C18 -54.2(10) . . . . ? C13 P2 C17 C18 62.5(10) . . . . ? P2 C17 C18 C19 -174.9(11) . . . . ? C17 C18 C19 C20 178.5(14) . . . . ? O13 P3 C21 C22 179.6(10) . . . . ? C25 P3 C21 C22 56.1(12) . . . . ? C21A P3 C21 C22 -63.2(11) . . . . ? P3 C21 C22 C23 174.8(10) . . . . ? C21 C22 C23 C24 -178.5(12) . . . . ? O13 P3 C25 C26 -54.3(17) . . . . ? C21 P3 C25 C26 68.8(16) . . . . ? C21A P3 C25 C26 -170.0(14) . . . . ? P3 C25 C26 C27 163.3(13) . . . . ? C25 C26 C27 C28 70(2) . . . . ? O5A P1A C1A C2A -171.8(8) . . . . ? C9A P1A C1A C2A -48.6(11) . . . . ? C5A P1A C1A C2A 66.5(10) . . . . ? P1A C1A C2A C3A -173.7(9) . . . . ? C1A C2A C3A C4A 174.3(12) . . . . ? O5A P1A C5A C6A 55.5(10) . . . . ? C1A P1A C5A C6A 176.2(8) . . . . ? C9A P1A C5A C6A -66.0(10) . . . . ? P1A C5A C6A C7A 175.6(9) . . . . ? C5A C6A C7A C8A -67.1(14) . . . . ? O5A P1A C9A C10A 62.4(10) . . . . ? C1A P1A C9A C10A -60.2(10) . . . . ? C5A P1A C9A C10A -175.9(8) . . . . ? P1A C9A C10A C11A -174.5(8) . . . . ? C9A C10A C11A C12A -61.6(14) . . . . ? O9 P2 C13A C14A 64.5(10) . . . . ? C17 P2 C13A C14A -59.5(11) . . . . ? C13 P2 C13A C14A -174.6(9) . . . . ? P2 C13A C14A C15A -172.9(9) . . . . ? C13A C14A C15A C16A -62.5(16) . . . . ? O13 P3 C21A C22A -157.2(11) . . . . ? C25 P3 C21A C22A -38.0(14) . . . . ? C21 P3 C21A C22A 82.7(13) . . . . ? P3 C21A C22A C23A 170.9(11) . . . . ? C21A C22A C23A C24A 178.1(13) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.56 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 4.887 _refine_diff_density_min -3.482 _refine_diff_density_rms 0.286 data_im1ba _database_code_depnum_ccdc_archive 'CCDC 235212' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H45 O13 P3 Tc2 U' _chemical_formula_weight 1428.84 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' 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' Tc Tc -1.4390 0.7593 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8713(13) _cell_length_b 15.6591(15) _cell_length_c 12.9940(12) _cell_angle_alpha 95.128(2) _cell_angle_beta 111.6520(10) _cell_angle_gamma 82.660(2) _cell_volume 2599.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9652 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 26.37 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 3.789 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.706534 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; The structure was solved by direct methods. All non-hydrogen atoms were refined anisotropically. All hydrogen atoms were found by difference Fourier techniques and refined isotropically. ; _diffrn_ambient_temperature 100(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 20707 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10411 _reflns_number_gt 9409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+1.6591P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10411 _refine_ls_number_parameters 658 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0622 _refine_ls_wR_factor_gt 0.0566 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.357395(10) 0.232821(8) 0.414648(11) 0.01150(4) Uani 1 1 d . . . Tc1 Tc 0.34230(3) 0.31781(2) 0.69159(3) 0.02230(8) Uani 1 1 d . . . Tc2 Tc 0.62767(2) 0.18692(2) 0.65947(3) 0.02389(8) Uani 1 1 d . . . P1 P 0.07421(7) 0.24077(6) 0.39473(8) 0.01475(19) Uani 1 1 d . . . P2 P 0.21870(7) 0.26471(6) 0.11408(7) 0.01272(18) Uani 1 1 d . . . P3 P 0.56660(7) 0.22389(6) 0.30543(7) 0.01223(18) Uani 1 1 d . . . O1 O 0.35089(18) 0.12019(15) 0.3968(2) 0.0149(5) Uani 1 1 d . . . O2 O 0.36347(19) 0.34534(15) 0.4307(2) 0.0162(5) Uani 1 1 d . . . O3 O 0.18941(18) 0.24376(16) 0.4273(2) 0.0177(5) Uani 1 1 d . . . O4 O 0.23207(18) 0.25177(15) 0.23247(19) 0.0139(5) Uani 1 1 d . . . O5 O 0.45333(18) 0.22516(15) 0.29333(19) 0.0137(5) Uani 1 1 d . . . O6 O 0.3798(2) 0.23819(17) 0.6058(2) 0.0208(6) Uani 1 1 d . . . O7 O 0.2492(2) 0.39049(18) 0.6123(3) 0.0339(7) Uani 1 1 d . . . O8 O 0.2927(3) 0.2721(2) 0.7725(3) 0.0458(9) Uani 1 1 d . . . O9 O 0.4456(3) 0.3692(3) 0.7731(3) 0.0623(11) Uani 1 1 d . . . O10 O 0.53672(18) 0.20010(16) 0.5246(2) 0.0186(6) Uani 1 1 d . . . O11 O 0.5874(2) 0.1245(2) 0.7328(3) 0.0414(9) Uani 1 1 d . . . O12 O 0.7432(2) 0.1415(3) 0.6533(3) 0.0514(10) Uani 1 1 d . . . O13 O 0.6445(3) 0.2854(2) 0.7286(3) 0.0497(9) Uani 1 1 d . . . C1 C 0.0278(3) 0.1565(2) 0.2909(3) 0.0170(8) Uani 1 1 d . . . C2 C 0.0956(3) 0.0833(2) 0.2863(3) 0.0210(8) Uani 1 1 d . . . H2 H 0.1661 0.0791 0.3361 0.025 Uiso 1 1 calc R . . C3 C 0.0595(3) 0.0170(3) 0.2087(3) 0.0277(9) Uani 1 1 d . . . H3 H 0.1058 -0.0321 0.2039 0.033 Uiso 1 1 calc R . . C4 C -0.0438(3) 0.0221(3) 0.1382(4) 0.0308(10) Uani 1 1 d . . . H4 H -0.0684 -0.0245 0.0868 0.037 Uiso 1 1 calc R . . C5 C -0.1113(3) 0.0938(3) 0.1418(3) 0.0281(10) Uani 1 1 d . . . H5 H -0.1818 0.0972 0.0923 0.034 Uiso 1 1 calc R . . C6 C -0.0756(3) 0.1610(3) 0.2181(3) 0.0229(9) Uani 1 1 d . . . H6 H -0.1220 0.2106 0.2207 0.028 Uiso 1 1 calc R . . C7 C 0.0393(3) 0.2215(2) 0.5111(3) 0.0171(8) Uani 1 1 d . . . C8 C -0.0042(3) 0.1475(3) 0.5141(3) 0.0204(8) Uani 1 1 d . . . H8 H -0.0164 0.1057 0.4541 0.024 Uiso 1 1 calc R . . C9 C -0.0302(3) 0.1341(3) 0.6045(3) 0.0267(9) Uani 1 1 d . . . H9 H -0.0600 0.0832 0.6065 0.032 Uiso 1 1 calc R . . C10 C -0.0126(3) 0.1951(3) 0.6919(3) 0.0298(10) Uani 1 1 d . . . H10 H -0.0304 0.1860 0.7537 0.036 Uiso 1 1 calc R . . C11 C 0.0310(3) 0.2693(3) 0.6891(3) 0.0291(10) Uani 1 1 d . . . H11 H 0.0435 0.3109 0.7492 0.035 Uiso 1 1 calc R . . C12 C 0.0565(3) 0.2829(3) 0.5981(3) 0.0232(9) Uani 1 1 d . . . H12 H 0.0856 0.3340 0.5957 0.028 Uiso 1 1 calc R . . C13 C 0.0011(3) 0.3402(2) 0.3404(3) 0.0190(8) Uani 1 1 d . . . C14 C -0.0932(3) 0.3690(3) 0.3536(4) 0.0259(9) Uani 1 1 d . . . H14 H -0.1187 0.3364 0.3946 0.031 Uiso 1 1 calc R . . C15 C -0.1500(3) 0.4441(3) 0.3077(4) 0.0300(10) Uani 1 1 d . . . H15 H -0.2144 0.4630 0.3166 0.036 Uiso 1 1 calc R . . C16 C -0.1130(4) 0.4909(3) 0.2495(4) 0.0378(11) Uani 1 1 d . . . H16 H -0.1523 0.5425 0.2174 0.045 Uiso 1 1 calc R . . C17 C -0.0186(5) 0.4644(3) 0.2362(5) 0.0622(19) Uani 1 1 d . . . H17 H 0.0064 0.4976 0.1955 0.075 Uiso 1 1 calc R . . C18 C 0.0390(4) 0.3890(3) 0.2828(4) 0.0441(14) Uani 1 1 d . . . H18 H 0.1042 0.3710 0.2752 0.053 Uiso 1 1 calc R . . C19 C 0.0826(3) 0.2887(2) 0.0326(3) 0.0162(8) Uani 1 1 d . . . C20 C 0.0155(3) 0.2257(3) 0.0206(3) 0.0212(8) Uani 1 1 d . . . H20 H 0.0426 0.1718 0.0538 0.025 Uiso 1 1 calc R . . C21 C -0.0901(3) 0.2416(3) -0.0393(3) 0.0280(9) Uani 1 1 d . . . H21 H -0.1347 0.1979 -0.0488 0.034 Uiso 1 1 calc R . . C22 C -0.1312(3) 0.3202(3) -0.0855(4) 0.0304(10) Uani 1 1 d . . . H22 H -0.2040 0.3312 -0.1251 0.036 Uiso 1 1 calc R . . C23 C -0.0655(3) 0.3828(3) -0.0737(4) 0.0299(10) Uani 1 1 d . . . H23 H -0.0935 0.4368 -0.1061 0.036 Uiso 1 1 calc R . . C24 C 0.0411(3) 0.3675(3) -0.0150(3) 0.0230(9) Uani 1 1 d . . . H24 H 0.0855 0.4110 -0.0075 0.028 Uiso 1 1 calc R . . C25 C 0.2837(3) 0.3555(2) 0.1059(3) 0.0151(7) Uani 1 1 d . . . C26 C 0.2862(3) 0.4236(2) 0.1838(3) 0.0189(8) Uani 1 1 d . . . H26 H 0.2553 0.4208 0.2374 0.023 Uiso 1 1 calc R . . C27 C 0.3343(3) 0.4954(2) 0.1817(3) 0.0235(9) Uani 1 1 d . . . H27 H 0.3371 0.5415 0.2351 0.028 Uiso 1 1 calc R . . C28 C 0.3784(3) 0.5009(3) 0.1031(3) 0.0269(9) Uani 1 1 d . . . H28 H 0.4105 0.5506 0.1018 0.032 Uiso 1 1 calc R . . C29 C 0.3750(3) 0.4335(3) 0.0271(4) 0.0289(10) Uani 1 1 d . . . H29 H 0.4055 0.4371 -0.0267 0.035 Uiso 1 1 calc R . . C30 C 0.3284(3) 0.3604(3) 0.0268(3) 0.0213(8) Uani 1 1 d . . . H30 H 0.3269 0.3143 -0.0264 0.026 Uiso 1 1 calc R . . C31 C 0.2606(3) 0.1688(2) 0.0509(3) 0.0145(7) Uani 1 1 d . . . C32 C 0.2487(3) 0.1652(2) -0.0598(3) 0.0202(8) Uani 1 1 d . . . H32 H 0.2135 0.2129 -0.1039 0.024 Uiso 1 1 calc R . . C33 C 0.2878(3) 0.0921(3) -0.1075(3) 0.0277(9) Uani 1 1 d . . . H33 H 0.2821 0.0909 -0.1827 0.033 Uiso 1 1 calc R . . C34 C 0.3351(3) 0.0213(3) -0.0436(4) 0.0264(9) Uani 1 1 d . . . H34 H 0.3621 -0.0286 -0.0754 0.032 Uiso 1 1 calc R . . C35 C 0.3434(3) 0.0224(3) 0.0660(3) 0.0258(9) Uani 1 1 d . . . H35 H 0.3743 -0.0269 0.1085 0.031 Uiso 1 1 calc R . . C36 C 0.3062(3) 0.0961(2) 0.1139(3) 0.0172(8) Uani 1 1 d . . . H36 H 0.3118 0.0971 0.1891 0.021 Uiso 1 1 calc R . . C37 C 0.6285(3) 0.3085(2) 0.3994(3) 0.0157(7) Uani 1 1 d . . . C38 C 0.5750(3) 0.3912(2) 0.3807(3) 0.0239(9) Uani 1 1 d . . . H38 H 0.5095 0.3993 0.3217 0.029 Uiso 1 1 calc R . . C39 C 0.6168(3) 0.4604(3) 0.4471(4) 0.0290(10) Uani 1 1 d . . . H39 H 0.5798 0.5162 0.4344 0.035 Uiso 1 1 calc R . . C40 C 0.7127(3) 0.4494(3) 0.5328(4) 0.0280(9) Uani 1 1 d . . . H40 H 0.7422 0.4978 0.5773 0.034 Uiso 1 1 calc R . . C41 C 0.7649(3) 0.3683(3) 0.5531(3) 0.0256(9) Uani 1 1 d . . . H41 H 0.8296 0.3608 0.6132 0.031 Uiso 1 1 calc R . . C42 C 0.7241(3) 0.2972(2) 0.4866(3) 0.0186(8) Uani 1 1 d . . . H42 H 0.7610 0.2414 0.5006 0.022 Uiso 1 1 calc R . . C43 C 0.5790(3) 0.2413(2) 0.1760(3) 0.0155(7) Uani 1 1 d . . . C44 C 0.6473(3) 0.2974(3) 0.1701(3) 0.0231(9) Uani 1 1 d . . . H44 H 0.6844 0.3305 0.2342 0.028 Uiso 1 1 calc R . . C45 C 0.6613(3) 0.3050(3) 0.0708(4) 0.0297(10) Uani 1 1 d . . . H45 H 0.7081 0.3430 0.0675 0.036 Uiso 1 1 calc R . . C46 C 0.6072(3) 0.2573(3) -0.0234(3) 0.0276(10) Uani 1 1 d . . . H46 H 0.6169 0.2622 -0.0912 0.033 Uiso 1 1 calc R . . C47 C 0.5385(3) 0.2024(3) -0.0176(3) 0.0244(9) Uani 1 1 d . . . H47 H 0.5001 0.1705 -0.0822 0.029 Uiso 1 1 calc R . . C48 C 0.5254(3) 0.1935(2) 0.0816(3) 0.0207(8) Uani 1 1 d . . . H48 H 0.4796 0.1545 0.0849 0.025 Uiso 1 1 calc R . . C49 C 0.6355(3) 0.1197(2) 0.3435(3) 0.0138(7) Uani 1 1 d . . . C50 C 0.7376(3) 0.1004(2) 0.3496(3) 0.0198(8) Uani 1 1 d . . . H50 H 0.7736 0.1437 0.3371 0.024 Uiso 1 1 calc R . . C51 C 0.7874(3) 0.0180(2) 0.3738(3) 0.0222(8) Uani 1 1 d . . . H51 H 0.8577 0.0052 0.3785 0.027 Uiso 1 1 calc R . . C52 C 0.7349(3) -0.0457(2) 0.3912(3) 0.0228(9) Uani 1 1 d . . . H52 H 0.7697 -0.1016 0.4096 0.027 Uiso 1 1 calc R . . C53 C 0.6323(3) -0.0277(2) 0.3816(3) 0.0210(8) Uani 1 1 d . . . H53 H 0.5956 -0.0719 0.3908 0.025 Uiso 1 1 calc R . . C54 C 0.5821(3) 0.0553(2) 0.3586(3) 0.0178(8) Uani 1 1 d . . . H54 H 0.5116 0.0678 0.3532 0.021 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 U1 0.01138(7) 0.01317(7) 0.01080(7) 0.00187(5) 0.00492(5) -0.00059(5) Tc1 0.02857(18) 0.02437(18) 0.01658(17) -0.00400(14) 0.01135(14) -0.00580(14) Tc2 0.01350(16) 0.0418(2) 0.01573(17) 0.01049(15) 0.00201(13) -0.00413(14) P1 0.0132(4) 0.0168(5) 0.0165(5) 0.0011(4) 0.0080(4) -0.0012(4) P2 0.0127(4) 0.0141(5) 0.0113(4) 0.0021(4) 0.0043(4) -0.0001(4) P3 0.0121(4) 0.0123(4) 0.0136(5) 0.0029(4) 0.0059(4) -0.0002(3) O1 0.0155(12) 0.0152(13) 0.0163(13) 0.0045(10) 0.0081(10) 0.0006(10) O2 0.0179(13) 0.0160(13) 0.0148(13) 0.0018(10) 0.0062(11) -0.0009(10) O3 0.0145(13) 0.0260(14) 0.0149(13) -0.0021(11) 0.0080(11) -0.0040(11) O4 0.0130(12) 0.0183(13) 0.0117(12) 0.0023(10) 0.0058(10) -0.0011(10) O5 0.0123(12) 0.0169(13) 0.0132(13) 0.0032(10) 0.0056(10) -0.0021(10) O6 0.0274(15) 0.0230(14) 0.0148(13) 0.0063(11) 0.0118(12) 0.0047(12) O7 0.0392(18) 0.0214(15) 0.0458(19) -0.0003(14) 0.0241(16) 0.0053(13) O8 0.058(2) 0.060(2) 0.0343(19) 0.0119(17) 0.0353(18) 0.0034(18) O9 0.049(2) 0.059(3) 0.059(3) -0.016(2) -0.0053(19) -0.0207(19) O10 0.0137(13) 0.0256(14) 0.0140(13) 0.0034(11) 0.0027(10) 0.0010(11) O11 0.0297(17) 0.066(2) 0.0320(18) 0.0292(17) 0.0094(14) -0.0026(16) O12 0.0207(16) 0.087(3) 0.049(2) 0.040(2) 0.0151(15) 0.0182(17) O13 0.053(2) 0.065(2) 0.0296(19) -0.0092(17) 0.0074(17) -0.0296(19) C1 0.0199(19) 0.0185(19) 0.0175(19) 0.0020(15) 0.0112(16) -0.0048(15) C2 0.023(2) 0.020(2) 0.022(2) 0.0029(16) 0.0104(17) -0.0017(16) C3 0.037(2) 0.018(2) 0.031(2) -0.0006(18) 0.017(2) -0.0012(18) C4 0.041(3) 0.029(2) 0.026(2) -0.0055(19) 0.013(2) -0.017(2) C5 0.024(2) 0.035(2) 0.026(2) 0.0011(19) 0.0057(18) -0.0134(19) C6 0.020(2) 0.026(2) 0.024(2) 0.0024(17) 0.0089(17) -0.0018(17) C7 0.0121(17) 0.023(2) 0.0155(19) 0.0040(16) 0.0054(15) 0.0030(15) C8 0.0167(18) 0.025(2) 0.020(2) 0.0033(16) 0.0070(16) 0.0001(16) C9 0.028(2) 0.029(2) 0.030(2) 0.0131(19) 0.0176(19) 0.0016(18) C10 0.026(2) 0.046(3) 0.020(2) 0.013(2) 0.0118(18) 0.003(2) C11 0.028(2) 0.043(3) 0.018(2) -0.0001(19) 0.0120(18) 0.000(2) C12 0.021(2) 0.030(2) 0.021(2) 0.0017(17) 0.0105(17) -0.0041(17) C13 0.0215(19) 0.0176(19) 0.020(2) 0.0008(16) 0.0100(16) -0.0002(16) C14 0.023(2) 0.023(2) 0.035(2) 0.0019(18) 0.0155(19) -0.0020(17) C15 0.021(2) 0.022(2) 0.045(3) -0.001(2) 0.012(2) 0.0032(17) C16 0.046(3) 0.025(2) 0.046(3) 0.013(2) 0.024(2) 0.015(2) C17 0.081(4) 0.045(3) 0.095(5) 0.045(3) 0.075(4) 0.032(3) C18 0.049(3) 0.038(3) 0.066(4) 0.026(3) 0.047(3) 0.020(2) C19 0.0171(18) 0.0203(19) 0.0093(17) 0.0016(15) 0.0030(14) 0.0007(15) C20 0.0205(19) 0.022(2) 0.022(2) 0.0071(17) 0.0078(16) -0.0026(16) C21 0.018(2) 0.036(2) 0.031(2) 0.0035(19) 0.0084(18) -0.0070(18) C22 0.0146(19) 0.041(3) 0.033(2) 0.011(2) 0.0050(18) 0.0017(18) C23 0.022(2) 0.028(2) 0.035(3) 0.017(2) 0.0045(19) 0.0087(18) C24 0.0190(19) 0.024(2) 0.026(2) 0.0074(17) 0.0060(17) -0.0019(16) C25 0.0116(17) 0.0149(18) 0.0166(19) 0.0070(15) 0.0017(14) 0.0011(14) C26 0.0186(19) 0.0191(19) 0.0167(19) 0.0045(15) 0.0037(15) 0.0014(15) C27 0.027(2) 0.0142(19) 0.023(2) -0.0006(16) 0.0017(17) -0.0023(16) C28 0.022(2) 0.024(2) 0.033(2) 0.0107(19) 0.0040(18) -0.0083(17) C29 0.030(2) 0.032(2) 0.032(2) 0.010(2) 0.0157(19) -0.0079(19) C30 0.022(2) 0.022(2) 0.019(2) 0.0013(16) 0.0070(16) -0.0022(16) C31 0.0131(17) 0.0137(18) 0.0153(18) -0.0018(14) 0.0034(14) -0.0031(14) C32 0.024(2) 0.021(2) 0.018(2) -0.0008(16) 0.0098(16) -0.0060(16) C33 0.035(2) 0.027(2) 0.023(2) -0.0076(18) 0.0134(19) -0.0098(19) C34 0.030(2) 0.020(2) 0.034(2) -0.0096(18) 0.0188(19) -0.0047(18) C35 0.028(2) 0.0155(19) 0.031(2) 0.0002(17) 0.0086(19) -0.0021(17) C36 0.0189(18) 0.0179(19) 0.0176(19) 0.0029(15) 0.0094(16) -0.0019(15) C37 0.0170(18) 0.0130(18) 0.0200(19) 0.0008(15) 0.0106(15) -0.0001(14) C38 0.0169(19) 0.018(2) 0.033(2) 0.0069(17) 0.0038(17) 0.0012(16) C39 0.030(2) 0.014(2) 0.042(3) 0.0004(18) 0.012(2) 0.0008(17) C40 0.029(2) 0.021(2) 0.036(2) -0.0088(18) 0.015(2) -0.0072(18) C41 0.0161(19) 0.032(2) 0.023(2) -0.0048(18) 0.0024(17) -0.0031(17) C42 0.0140(18) 0.0182(19) 0.021(2) 0.0028(16) 0.0045(15) 0.0015(15) C43 0.0134(17) 0.0184(19) 0.0176(19) 0.0062(15) 0.0094(15) 0.0037(14) C44 0.0183(19) 0.027(2) 0.025(2) 0.0040(17) 0.0069(17) -0.0066(17) C45 0.030(2) 0.033(2) 0.031(2) 0.012(2) 0.014(2) -0.0057(19) C46 0.028(2) 0.038(3) 0.022(2) 0.0090(19) 0.0162(18) 0.0054(19) C47 0.026(2) 0.032(2) 0.017(2) 0.0017(17) 0.0123(17) 0.0028(18) C48 0.0201(19) 0.023(2) 0.023(2) 0.0067(17) 0.0123(17) 0.0030(16) C49 0.0152(17) 0.0110(17) 0.0143(18) 0.0012(14) 0.0046(14) 0.0001(14) C50 0.0188(19) 0.0169(19) 0.026(2) -0.0012(16) 0.0104(17) -0.0039(15) C51 0.0151(19) 0.023(2) 0.028(2) -0.0021(17) 0.0092(17) 0.0027(16) C52 0.026(2) 0.0150(19) 0.020(2) 0.0028(16) 0.0028(17) 0.0060(16) C53 0.030(2) 0.0140(19) 0.023(2) 0.0069(16) 0.0117(17) -0.0036(16) C54 0.0201(19) 0.0170(19) 0.0188(19) 0.0041(15) 0.0104(16) 0.0014(15) _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 1.765(2) . ? U1 O1 1.768(2) . ? U1 O3 2.379(2) . ? U1 O6 2.381(2) . ? U1 O4 2.381(2) . ? U1 O10 2.382(2) . ? U1 O5 2.397(2) . ? Tc1 O9 1.687(3) . ? Tc1 O7 1.696(3) . ? Tc1 O8 1.698(3) . ? Tc1 O6 1.755(3) . ? Tc2 O12 1.695(3) . ? Tc2 O11 1.695(3) . ? Tc2 O13 1.711(4) . ? Tc2 O10 1.753(2) . ? P1 O3 1.501(2) . ? P1 C13 1.793(4) . ? P1 C1 1.798(4) . ? P1 C7 1.809(4) . ? P2 O4 1.509(2) . ? P2 C31 1.782(4) . ? P2 C19 1.801(4) . ? P2 C25 1.808(4) . ? P3 O5 1.518(2) . ? P3 C37 1.793(4) . ? P3 C49 1.794(3) . ? P3 C43 1.800(4) . ? C1 C6 1.393(5) . ? C1 C2 1.399(5) . ? C2 C3 1.385(5) . ? C2 H2 0.9500 . ? C3 C4 1.383(6) . ? C3 H3 0.9500 . ? C4 C5 1.376(6) . ? C4 H4 0.9500 . ? C5 C6 1.385(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.382(5) . ? C7 C12 1.387(5) . ? C8 C9 1.390(5) . ? C8 H8 0.9500 . ? C9 C10 1.386(6) . ? C9 H9 0.9500 . ? C10 C11 1.386(6) . ? C10 H10 0.9500 . ? C11 C12 1.393(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.385(5) . ? C13 C14 1.394(5) . ? C14 C15 1.379(6) . ? C14 H14 0.9500 . ? C15 C16 1.362(6) . ? C15 H15 0.9500 . ? C16 C17 1.389(6) . ? C16 H16 0.9500 . ? C17 C18 1.388(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.389(5) . ? C19 C20 1.402(5) . ? C20 C21 1.383(5) . ? C20 H20 0.9500 . ? C21 C22 1.378(6) . ? C21 H21 0.9500 . ? C22 C23 1.384(6) . ? C22 H22 0.9500 . ? C23 C24 1.391(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.395(5) . ? C25 C26 1.397(5) . ? C26 C27 1.386(5) . ? C26 H26 0.9500 . ? C27 C28 1.383(6) . ? C27 H27 0.9500 . ? C28 C29 1.373(6) . ? C28 H28 0.9500 . ? C29 C30 1.383(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.382(5) . ? C31 C36 1.403(5) . ? C32 C33 1.396(5) . ? C32 H32 0.9500 . ? C33 C34 1.388(6) . ? C33 H33 0.9500 . ? C34 C35 1.384(6) . ? C34 H34 0.9500 . ? C35 C36 1.393(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.393(5) . ? C37 C38 1.401(5) . ? C38 C39 1.371(6) . ? C38 H38 0.9500 . ? C39 C40 1.386(6) . ? C39 H39 0.9500 . ? C40 C41 1.375(6) . ? C40 H40 0.9500 . ? C41 C42 1.392(5) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.387(5) . ? C43 C44 1.396(5) . ? C44 C45 1.391(5) . ? C44 H44 0.9500 . ? C45 C46 1.386(6) . ? C45 H45 0.9500 . ? C46 C47 1.388(6) . ? C46 H46 0.9500 . ? C47 C48 1.388(5) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.384(5) . ? C49 C54 1.391(5) . ? C50 C51 1.387(5) . ? C50 H50 0.9500 . ? C51 C52 1.387(5) . ? C51 H51 0.9500 . ? C52 C53 1.376(5) . ? C52 H52 0.9500 . ? C53 C54 1.396(5) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? 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 179.32(11) . . ? O2 U1 O3 93.25(10) . . ? O1 U1 O3 86.87(10) . . ? O2 U1 O6 86.33(10) . . ? O1 U1 O6 94.35(10) . . ? O3 U1 O6 71.93(9) . . ? O2 U1 O4 89.05(10) . . ? O1 U1 O4 90.34(10) . . ? O3 U1 O4 72.65(8) . . ? O6 U1 O4 143.93(8) . . ? O2 U1 O10 93.99(10) . . ? O1 U1 O10 86.34(10) . . ? O3 U1 O10 140.61(8) . . ? O6 U1 O10 69.98(9) . . ? O4 U1 O10 146.08(8) . . ? O2 U1 O5 89.08(10) . . ? O1 U1 O5 90.44(9) . . ? O3 U1 O5 145.96(8) . . ? O6 U1 O5 142.09(8) . . ? O4 U1 O5 73.43(8) . . ? O10 U1 O5 72.85(8) . . ? O9 Tc1 O7 109.06(18) . . ? O9 Tc1 O8 109.25(19) . . ? O7 Tc1 O8 108.71(15) . . ? O9 Tc1 O6 110.37(17) . . ? O7 Tc1 O6 109.54(13) . . ? O8 Tc1 O6 109.88(14) . . ? O12 Tc2 O11 109.37(16) . . ? O12 Tc2 O13 109.25(19) . . ? O11 Tc2 O13 107.45(17) . . ? O12 Tc2 O10 109.29(14) . . ? O11 Tc2 O10 111.98(13) . . ? O13 Tc2 O10 109.46(15) . . ? O3 P1 C13 112.18(16) . . ? O3 P1 C1 111.36(16) . . ? C13 P1 C1 107.59(18) . . ? O3 P1 C7 112.18(15) . . ? C13 P1 C7 105.99(17) . . ? C1 P1 C7 107.21(17) . . ? O4 P2 C31 111.46(15) . . ? O4 P2 C19 109.87(15) . . ? C31 P2 C19 105.58(17) . . ? O4 P2 C25 110.95(16) . . ? C31 P2 C25 111.95(17) . . ? C19 P2 C25 106.77(16) . . ? O5 P3 C37 111.67(15) . . ? O5 P3 C49 110.71(15) . . ? C37 P3 C49 112.35(17) . . ? O5 P3 C43 111.77(15) . . ? C37 P3 C43 105.46(17) . . ? C49 P3 C43 104.56(16) . . ? P1 O3 U1 160.52(15) . . ? P2 O4 U1 143.98(14) . . ? P3 O5 U1 136.84(14) . . ? Tc1 O6 U1 132.43(13) . . ? Tc2 O10 U1 145.29(13) . . ? C6 C1 C2 119.3(4) . . ? C6 C1 P1 121.3(3) . . ? C2 C1 P1 119.3(3) . . ? C3 C2 C1 119.6(4) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 120.2(4) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 120.7(4) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 119.5(4) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C1 120.6(4) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C8 C7 C12 120.1(3) . . ? C8 C7 P1 121.2(3) . . ? C12 C7 P1 118.7(3) . . ? C7 C8 C9 120.1(4) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 120.0(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.0(4) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 119.9(4) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C7 C12 C11 119.9(4) . . ? C7 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C18 C13 C14 119.3(4) . . ? C18 C13 P1 118.9(3) . . ? C14 C13 P1 121.8(3) . . ? C15 C14 C13 120.8(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 119.5(4) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 120.9(4) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C18 C17 C16 119.7(4) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C13 C18 C17 119.7(4) . . ? C13 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C24 C19 C20 119.0(3) . . ? C24 C19 P2 123.0(3) . . ? C20 C19 P2 118.0(3) . . ? C21 C20 C19 120.2(4) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 120.7(4) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 119.4(4) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C22 C23 C24 120.7(4) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C19 C24 C23 119.9(4) . . ? C19 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C30 C25 C26 120.2(3) . . ? C30 C25 P2 123.6(3) . . ? C26 C25 P2 116.2(3) . . ? C27 C26 C25 119.1(4) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C28 C27 C26 121.0(4) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C29 C28 C27 119.1(4) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C28 C29 C30 121.8(4) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C29 C30 C25 118.9(4) . . ? C29 C30 H30 120.6 . . ? C25 C30 H30 120.6 . . ? C32 C31 C36 119.5(3) . . ? C32 C31 P2 120.7(3) . . ? C36 C31 P2 119.8(3) . . ? C31 C32 C33 120.8(4) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 119.2(4) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C35 C34 C33 120.8(4) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 119.9(4) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C35 C36 C31 119.9(3) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C42 C37 C38 119.5(3) . . ? C42 C37 P3 124.7(3) . . ? C38 C37 P3 115.9(3) . . ? C39 C38 C37 120.3(4) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 120.3(4) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C41 C40 C39 119.8(4) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 120.8(4) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C41 C42 C37 119.3(3) . . ? C41 C42 H42 120.4 . . ? C37 C42 H42 120.4 . . ? C48 C43 C44 119.1(3) . . ? C48 C43 P3 119.3(3) . . ? C44 C43 P3 121.4(3) . . ? C45 C44 C43 120.4(4) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C46 C45 C44 120.3(4) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 119.2(4) . . ? C45 C46 H46 120.4 . . ? C47 C46 H46 120.4 . . ? C48 C47 C46 120.8(4) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C43 C48 C47 120.2(4) . . ? C43 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C50 C49 C54 119.6(3) . . ? C50 C49 P3 121.4(3) . . ? C54 C49 P3 118.9(3) . . ? C49 C50 C51 120.2(3) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C52 C51 C50 120.1(3) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C53 C52 C51 119.9(3) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 120.2(3) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C49 C54 C53 119.9(3) . . ? C49 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 P1 O3 U1 -87.9(5) . . . . ? C1 P1 O3 U1 32.7(5) . . . . ? C7 P1 O3 U1 152.9(4) . . . . ? O2 U1 O3 P1 111.3(5) . . . . ? O1 U1 O3 P1 -68.0(5) . . . . ? O6 U1 O3 P1 -163.6(5) . . . . ? O4 U1 O3 P1 23.3(5) . . . . ? O10 U1 O3 P1 -148.4(4) . . . . ? O5 U1 O3 P1 18.1(6) . . . . ? C31 P2 O4 U1 71.7(3) . . . . ? C19 P2 O4 U1 -171.6(2) . . . . ? C25 P2 O4 U1 -53.8(3) . . . . ? O2 U1 O4 P2 81.0(3) . . . . ? O1 U1 O4 P2 -98.7(3) . . . . ? O3 U1 O4 P2 174.7(3) . . . . ? O6 U1 O4 P2 163.4(2) . . . . ? O10 U1 O4 P2 -14.8(3) . . . . ? O5 U1 O4 P2 -8.4(2) . . . . ? C37 P3 O5 U1 -49.1(2) . . . . ? C49 P3 O5 U1 76.9(2) . . . . ? C43 P3 O5 U1 -167.02(19) . . . . ? O2 U1 O5 P3 80.5(2) . . . . ? O1 U1 O5 P3 -100.0(2) . . . . ? O3 U1 O5 P3 174.95(16) . . . . ? O6 U1 O5 P3 -2.3(3) . . . . ? O4 U1 O5 P3 169.8(2) . . . . ? O10 U1 O5 P3 -13.95(19) . . . . ? O9 Tc1 O6 U1 -103.0(2) . . . . ? O7 Tc1 O6 U1 17.1(2) . . . . ? O8 Tc1 O6 U1 136.44(19) . . . . ? O2 U1 O6 Tc1 31.07(19) . . . . ? O1 U1 O6 Tc1 -148.83(19) . . . . ? O3 U1 O6 Tc1 -63.55(18) . . . . ? O4 U1 O6 Tc1 -52.3(3) . . . . ? O10 U1 O6 Tc1 126.7(2) . . . . ? O5 U1 O6 Tc1 114.85(18) . . . . ? O12 Tc2 O10 U1 168.2(2) . . . . ? O11 Tc2 O10 U1 46.9(3) . . . . ? O13 Tc2 O10 U1 -72.1(3) . . . . ? O2 U1 O10 Tc2 85.3(2) . . . . ? O1 U1 O10 Tc2 -95.3(2) . . . . ? O3 U1 O10 Tc2 -14.7(3) . . . . ? O6 U1 O10 Tc2 0.7(2) . . . . ? O4 U1 O10 Tc2 179.58(18) . . . . ? O5 U1 O10 Tc2 173.1(3) . . . . ? O3 P1 C1 C6 -154.7(3) . . . . ? C13 P1 C1 C6 -31.3(3) . . . . ? C7 P1 C1 C6 82.3(3) . . . . ? O3 P1 C1 C2 28.1(3) . . . . ? C13 P1 C1 C2 151.5(3) . . . . ? C7 P1 C1 C2 -94.9(3) . . . . ? C6 C1 C2 C3 0.8(5) . . . . ? P1 C1 C2 C3 178.1(3) . . . . ? C1 C2 C3 C4 -1.8(6) . . . . ? C2 C3 C4 C5 1.9(6) . . . . ? C3 C4 C5 C6 -1.0(6) . . . . ? C4 C5 C6 C1 0.0(6) . . . . ? C2 C1 C6 C5 0.1(6) . . . . ? P1 C1 C6 C5 -177.1(3) . . . . ? O3 P1 C7 C8 -116.1(3) . . . . ? C13 P1 C7 C8 121.2(3) . . . . ? C1 P1 C7 C8 6.5(3) . . . . ? O3 P1 C7 C12 64.3(3) . . . . ? C13 P1 C7 C12 -58.5(3) . . . . ? C1 P1 C7 C12 -173.2(3) . . . . ? C12 C7 C8 C9 -0.4(5) . . . . ? P1 C7 C8 C9 179.9(3) . . . . ? C7 C8 C9 C10 0.1(6) . . . . ? C8 C9 C10 C11 -0.1(6) . . . . ? C9 C10 C11 C12 0.4(6) . . . . ? C8 C7 C12 C11 0.8(6) . . . . ? P1 C7 C12 C11 -179.5(3) . . . . ? C10 C11 C12 C7 -0.8(6) . . . . ? O3 P1 C13 C18 31.8(4) . . . . ? C1 P1 C13 C18 -91.0(4) . . . . ? C7 P1 C13 C18 154.5(4) . . . . ? O3 P1 C13 C14 -149.0(3) . . . . ? C1 P1 C13 C14 88.2(4) . . . . ? C7 P1 C13 C14 -26.3(4) . . . . ? C18 C13 C14 C15 1.6(7) . . . . ? P1 C13 C14 C15 -177.6(3) . . . . ? C13 C14 C15 C16 -0.4(7) . . . . ? C14 C15 C16 C17 -0.4(8) . . . . ? C15 C16 C17 C18 0.0(9) . . . . ? C14 C13 C18 C17 -1.9(8) . . . . ? P1 C13 C18 C17 177.3(5) . . . . ? C16 C17 C18 C13 1.1(9) . . . . ? O4 P2 C19 C24 114.6(3) . . . . ? C31 P2 C19 C24 -125.1(3) . . . . ? C25 P2 C19 C24 -5.8(4) . . . . ? O4 P2 C19 C20 -63.0(3) . . . . ? C31 P2 C19 C20 57.3(3) . . . . ? C25 P2 C19 C20 176.6(3) . . . . ? C24 C19 C20 C21 1.1(6) . . . . ? P2 C19 C20 C21 178.7(3) . . . . ? C19 C20 C21 C22 -1.8(6) . . . . ? C20 C21 C22 C23 1.5(7) . . . . ? C21 C22 C23 C24 -0.6(7) . . . . ? C20 C19 C24 C23 -0.2(6) . . . . ? P2 C19 C24 C23 -177.7(3) . . . . ? C22 C23 C24 C19 0.0(7) . . . . ? O4 P2 C25 C30 148.2(3) . . . . ? C31 P2 C25 C30 23.0(4) . . . . ? C19 P2 C25 C30 -92.1(3) . . . . ? O4 P2 C25 C26 -32.7(3) . . . . ? C31 P2 C25 C26 -157.9(3) . . . . ? C19 P2 C25 C26 87.0(3) . . . . ? C30 C25 C26 C27 -0.5(5) . . . . ? P2 C25 C26 C27 -179.7(3) . . . . ? C25 C26 C27 C28 0.9(6) . . . . ? C26 C27 C28 C29 -0.7(6) . . . . ? C27 C28 C29 C30 0.2(6) . . . . ? C28 C29 C30 C25 0.1(6) . . . . ? C26 C25 C30 C29 0.1(5) . . . . ? P2 C25 C30 C29 179.1(3) . . . . ? O4 P2 C31 C32 175.8(3) . . . . ? C19 P2 C31 C32 56.5(3) . . . . ? C25 P2 C31 C32 -59.3(3) . . . . ? O4 P2 C31 C36 -4.2(3) . . . . ? C19 P2 C31 C36 -123.5(3) . . . . ? C25 P2 C31 C36 120.7(3) . . . . ? C36 C31 C32 C33 -4.3(6) . . . . ? P2 C31 C32 C33 175.7(3) . . . . ? C31 C32 C33 C34 2.8(6) . . . . ? C32 C33 C34 C35 0.2(6) . . . . ? C33 C34 C35 C36 -1.6(6) . . . . ? C34 C35 C36 C31 0.0(6) . . . . ? C32 C31 C36 C35 3.0(5) . . . . ? P2 C31 C36 C35 -177.1(3) . . . . ? O5 P3 C37 C42 130.6(3) . . . . ? C49 P3 C37 C42 5.5(4) . . . . ? C43 P3 C37 C42 -107.8(3) . . . . ? O5 P3 C37 C38 -49.9(3) . . . . ? C49 P3 C37 C38 -175.0(3) . . . . ? C43 P3 C37 C38 71.7(3) . . . . ? C42 C37 C38 C39 0.5(6) . . . . ? P3 C37 C38 C39 -179.0(3) . . . . ? C37 C38 C39 C40 0.6(6) . . . . ? C38 C39 C40 C41 -1.8(6) . . . . ? C39 C40 C41 C42 1.9(6) . . . . ? C40 C41 C42 C37 -0.8(6) . . . . ? C38 C37 C42 C41 -0.4(5) . . . . ? P3 C37 C42 C41 179.1(3) . . . . ? O5 P3 C43 C48 -49.2(3) . . . . ? C37 P3 C43 C48 -170.7(3) . . . . ? C49 P3 C43 C48 70.6(3) . . . . ? O5 P3 C43 C44 135.5(3) . . . . ? C37 P3 C43 C44 14.0(3) . . . . ? C49 P3 C43 C44 -104.6(3) . . . . ? C48 C43 C44 C45 0.0(6) . . . . ? P3 C43 C44 C45 175.2(3) . . . . ? C43 C44 C45 C46 0.3(6) . . . . ? C44 C45 C46 C47 0.4(6) . . . . ? C45 C46 C47 C48 -1.4(6) . . . . ? C44 C43 C48 C47 -1.0(5) . . . . ? P3 C43 C48 C47 -176.3(3) . . . . ? C46 C47 C48 C43 1.7(6) . . . . ? O5 P3 C49 C50 174.1(3) . . . . ? C37 P3 C49 C50 -60.3(4) . . . . ? C43 P3 C49 C50 53.5(3) . . . . ? O5 P3 C49 C54 -0.8(3) . . . . ? C37 P3 C49 C54 124.8(3) . . . . ? C43 P3 C49 C54 -121.4(3) . . . . ? C54 C49 C50 C51 -1.9(6) . . . . ? P3 C49 C50 C51 -176.8(3) . . . . ? C49 C50 C51 C52 0.6(6) . . . . ? C50 C51 C52 C53 1.6(6) . . . . ? C51 C52 C53 C54 -2.4(6) . . . . ? C50 C49 C54 C53 1.2(6) . . . . ? P3 C49 C54 C53 176.1(3) . . . . ? C52 C53 C54 C49 1.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.388 _refine_diff_density_min -1.132 _refine_diff_density_rms 0.106