# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_apx1549 _database_code_depnum_ccdc_archive 'CCDC 904329' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H37 F12 N2 O18 P3 S4 U' _chemical_formula_weight 1268.69 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 8.3319(7) _cell_length_b 21.0439(19) _cell_length_c 24.947(2) _cell_angle_alpha 100.891(1) _cell_angle_beta 90.379(1) _cell_angle_gamma 96.996(1) _cell_volume 4261.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.977 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2472 _exptl_absorpt_coefficient_mu 4.237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3833 _exptl_absorpt_correction_T_max 0.7851 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 47416 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.45 _reflns_number_total 18927 _reflns_number_gt 14944 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _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. Hydrogen atom positions on the bound water molecules were found on the difference map and refined with isotropic temperature factors set to 0.08 \%A^2^. Two O-H distances were restrained to prevent unreasonably short O-H water bond distances. ; _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^)+(0.0255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18927 _refine_ls_number_parameters 1105 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0651 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.003 _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 0.244334(17) 0.897154(7) 0.148363(6) 0.01106(4) Uani 1 1 d . . . U2 U 0.813052(17) 0.081649(7) 0.342406(6) 0.01164(4) Uani 1 1 d . . . P1 P -0.16454(12) 1.12057(5) 0.13515(4) 0.0153(2) Uani 1 1 d . . . P2 P 0.09961(13) 0.63463(5) -0.01471(4) 0.0155(2) Uani 1 1 d . . . P3 P 0.68300(12) 0.75171(5) 0.16795(4) 0.0130(2) Uani 1 1 d . . . P4 P 1.34490(12) 0.22339(5) 0.32567(4) 0.0134(2) Uani 1 1 d . . . P5 P 0.85115(13) 0.34973(5) 0.50104(4) 0.0167(2) Uani 1 1 d . . . P6 P 0.25112(12) -0.13565(5) 0.35756(4) 0.0157(2) Uani 1 1 d . . . S1 S 0.36357(12) 0.22691(5) 0.14228(4) 0.0165(2) Uani 1 1 d . . . S2 S 0.42358(12) 0.19478(6) 0.03145(4) 0.0202(2) Uani 1 1 d . . . S3 S 0.14918(12) 0.54479(5) 0.13780(4) 0.0175(2) Uani 1 1 d . . . S4 S 0.47160(12) 0.53577(5) 0.10714(4) 0.0177(2) Uani 1 1 d . . . S5 S 0.71666(12) 0.75742(5) 0.35621(4) 0.0180(2) Uani 1 1 d . . . S6 S 0.78616(13) 0.80823(6) 0.46654(4) 0.0214(2) Uani 1 1 d . . . S7 S 0.29060(13) 0.43916(5) 0.38747(4) 0.0205(2) Uani 1 1 d . . . S8 S -0.01633(14) 0.44321(6) 0.34481(5) 0.0254(3) Uani 1 1 d . . . F1 F 0.3221(3) 0.34049(13) 0.19728(11) 0.0421(8) Uani 1 1 d . . . F2 F 0.3826(4) 0.34061(13) 0.11364(12) 0.0437(8) Uani 1 1 d . . . F3 F 0.5660(3) 0.33275(13) 0.17194(12) 0.0435(8) Uani 1 1 d . . . F4 F 0.2498(3) 0.08639(14) 0.04139(14) 0.0611(10) Uani 1 1 d . . . F5 F 0.4953(3) 0.07517(12) 0.02035(10) 0.0332(6) Uani 1 1 d . . . F6 F 0.3287(3) 0.09169(16) -0.04048(12) 0.0583(10) Uani 1 1 d . . . F7 F 0.2287(3) 0.55882(14) 0.24147(10) 0.0356(7) Uani 1 1 d . . . F8 F -0.0237(3) 0.56121(13) 0.22404(10) 0.0319(6) Uani 1 1 d . . . F9 F 0.1509(3) 0.64393(12) 0.21882(10) 0.0333(7) Uani 1 1 d . . . F10 F 0.4499(3) 0.47239(12) 0.18823(10) 0.0276(6) Uani 1 1 d . . . F11 F 0.6076(3) 0.56278(12) 0.20467(10) 0.0314(6) Uani 1 1 d . . . F12 F 0.6833(3) 0.47890(13) 0.15152(10) 0.0315(6) Uani 1 1 d . . . F13 F 0.6764(4) 0.65281(14) 0.39859(12) 0.0585(10) Uani 1 1 d . . . F14 F 0.8694(4) 0.65475(14) 0.34209(13) 0.0567(9) Uani 1 1 d . . . F15 F 0.6217(4) 0.63690(13) 0.31240(12) 0.0493(8) Uani 1 1 d . . . F16 F 0.7409(4) 0.91927(16) 0.52554(13) 0.0608(10) Uani 1 1 d . . . F17 F 0.9374(3) 0.92568(13) 0.47048(11) 0.0366(7) Uani 1 1 d . . . F18 F 0.6935(3) 0.91188(14) 0.43895(13) 0.0502(8) Uani 1 1 d . . . F19 F 0.5670(4) 0.50350(17) 0.37483(16) 0.0670(11) Uani 1 1 d . . . F20 F 0.4631(5) 0.4395(3) 0.30223(15) 0.1074(17) Uani 1 1 d . . . F21 F 0.3688(4) 0.5296(2) 0.33213(19) 0.0995(16) Uani 1 1 d . . . F22 F -0.1017(4) 0.34354(14) 0.26638(13) 0.0516(9) Uani 1 1 d . . . F23 F -0.2052(4) 0.43082(15) 0.26048(12) 0.0539(9) Uani 1 1 d . . . F24 F 0.0420(4) 0.42288(15) 0.24087(12) 0.0546(9) Uani 1 1 d . . . O1 O 0.3323(3) 0.92439(13) 0.09175(10) 0.0171(6) Uani 1 1 d . . . O2 O 0.1564(3) 0.87037(13) 0.20582(10) 0.0148(6) Uani 1 1 d . . . O4 O 0.0976(3) 0.98694(13) 0.16689(11) 0.0167(6) Uani 1 1 d . . . O6 O 0.0519(3) 0.76833(14) 0.03079(11) 0.0226(7) Uani 1 1 d . . . O7 O 0.2213(3) 0.78717(13) 0.10400(11) 0.0166(6) Uani 1 1 d . . . O8 O 0.4918(3) 0.86059(13) 0.17214(11) 0.0165(6) Uani 1 1 d . . . O9 O 0.6868(3) 0.94246(12) 0.19935(11) 0.0151(6) Uani 1 1 d . . . O10 O 0.4018(3) 0.98674(14) 0.20967(12) 0.0163(6) Uani 1 1 d . . . O11 O -0.0153(3) 0.87070(13) 0.09810(11) 0.0167(6) Uani 1 1 d D . . O12 O 0.7375(3) 0.10982(13) 0.28567(10) 0.0150(6) Uani 1 1 d . . . O13 O 0.8904(3) 0.05313(13) 0.39768(11) 0.0188(6) Uani 1 1 d . . . O14 O 1.0801(3) 0.11633(13) 0.31800(11) 0.0168(6) Uani 1 1 d . . . O15 O 1.2213(3) 0.03314(13) 0.29014(11) 0.0159(6) Uani 1 1 d . . . O16 O 0.6044(3) -0.00615(13) 0.32532(11) 0.0182(6) Uani 1 1 d . . . O17 O 0.4346(3) -0.00683(13) 0.39475(11) 0.0200(6) Uani 1 1 d . . . O18 O 0.8661(3) 0.19145(13) 0.38744(11) 0.0169(6) Uani 1 1 d . . . O19 O 0.7021(3) 0.21801(14) 0.45633(12) 0.0255(7) Uani 1 1 d . . . O20 O 0.5771(3) 0.11083(14) 0.39402(12) 0.0171(6) Uani 1 1 d . . . O21 O 0.9035(3) -0.00779(14) 0.27813(12) 0.0168(7) Uani 1 1 d . . . O22 O 0.1933(3) 0.21599(14) 0.13169(12) 0.0244(7) Uani 1 1 d . . . O23 O 0.4229(4) 0.20752(15) 0.19007(11) 0.0272(7) Uani 1 1 d . . . O24 O 0.2794(4) 0.22114(17) 0.02034(12) 0.0375(9) Uani 1 1 d . . . O25 O 0.5652(3) 0.20813(15) 0.00184(12) 0.0285(7) Uani 1 1 d . . . O26 O 0.1206(3) 0.47559(13) 0.13254(12) 0.0228(7) Uani 1 1 d . . . O27 O 0.0388(3) 0.57590(14) 0.11028(12) 0.0247(7) Uani 1 1 d . . . O28 O 0.4246(3) 0.47640(14) 0.06943(11) 0.0225(7) Uani 1 1 d . . . O29 O 0.5978(3) 0.58179(14) 0.09331(11) 0.0236(7) Uani 1 1 d . . . O30 O 0.5506(3) 0.76671(15) 0.36317(12) 0.0285(8) Uani 1 1 d . . . O31 O 0.7885(3) 0.76972(15) 0.30677(11) 0.0274(7) Uani 1 1 d . . . O32 O 0.6246(4) 0.78470(16) 0.47791(12) 0.0329(8) Uani 1 1 d . . . O33 O 0.9169(4) 0.79964(16) 0.50059(11) 0.0296(8) Uani 1 1 d . . . O34 O 0.2583(4) 0.48787(15) 0.43229(12) 0.0342(8) Uani 1 1 d . . . O35 O 0.3733(4) 0.38735(15) 0.39806(13) 0.0344(8) Uani 1 1 d . . . O36 O -0.1426(4) 0.41563(19) 0.37474(15) 0.0508(10) Uani 1 1 d . . . O37 O 0.0057(4) 0.51205(15) 0.34876(13) 0.0339(8) Uani 1 1 d . . . N1 N 0.4752(4) 0.20430(16) 0.09396(13) 0.0161(7) Uani 1 1 d . . . N2 N 0.3291(4) 0.57506(16) 0.13015(14) 0.0185(8) Uani 1 1 d . . . N4 N 0.1423(5) 0.40969(18) 0.34857(17) 0.0375(11) Uani 1 1 d . . . O5 O -0.0588(3) 0.99211(13) 0.09488(11) 0.0208(7) Uani 1 1 d . . . N3 N 0.8378(4) 0.78951(16) 0.40505(13) 0.0166(7) Uani 1 1 d . . . C1 C 0.0101(5) 1.01585(19) 0.13933(16) 0.0156(9) Uani 1 1 d . . . C2 C -0.0088(5) 1.08598(19) 0.16565(16) 0.0157(9) Uani 1 1 d . . . H2A H 0.0934 1.1129 0.1639 0.019 Uiso 1 1 calc R . . H2B H -0.0318 1.0875 0.2039 0.019 Uiso 1 1 calc R . . C3 C -0.1707(5) 1.19963(19) 0.17564(17) 0.0203(9) Uani 1 1 d . . . H3A H -0.0668 1.2250 0.1759 0.030 Uiso 1 1 calc R . . H3B H -0.1978 1.1956 0.2123 0.030 Uiso 1 1 calc R . . H3C H -0.2510 1.2208 0.1605 0.030 Uiso 1 1 calc R . . C4 C -0.1250(5) 1.1276(2) 0.06637(16) 0.0216(10) Uani 1 1 d . . . H4A H -0.2066 1.1495 0.0528 0.032 Uiso 1 1 calc R . . H4B H -0.1263 1.0848 0.0443 0.032 Uiso 1 1 calc R . . H4C H -0.0208 1.1521 0.0649 0.032 Uiso 1 1 calc R . . C5 C -0.3537(5) 1.0731(2) 0.14030(18) 0.0221(10) Uani 1 1 d . . . H5A H -0.4388 1.0930 0.1265 0.033 Uiso 1 1 calc R . . H5B H -0.3717 1.0706 0.1779 0.033 Uiso 1 1 calc R . . H5C H -0.3525 1.0299 0.1193 0.033 Uiso 1 1 calc R . . C6 C 0.1563(5) 0.7524(2) 0.05921(16) 0.0174(9) Uani 1 1 d . . . C7 C 0.2128(5) 0.68600(19) 0.04272(16) 0.0165(9) Uani 1 1 d . . . H7A H 0.2042 0.6641 0.0737 0.020 Uiso 1 1 calc R . . H7B H 0.3260 0.6918 0.0337 0.020 Uiso 1 1 calc R . . C8 C 0.1244(5) 0.6687(2) -0.07492(17) 0.0274(11) Uani 1 1 d . . . H8A H 0.2375 0.6802 -0.0801 0.041 Uiso 1 1 calc R . . H8B H 0.0702 0.7070 -0.0711 0.041 Uiso 1 1 calc R . . H8C H 0.0787 0.6372 -0.1059 0.041 Uiso 1 1 calc R . . C9 C -0.1102(4) 0.6217(2) -0.00139(17) 0.0200(9) Uani 1 1 d . . . H9A H -0.1652 0.5913 -0.0314 0.030 Uiso 1 1 calc R . . H9B H -0.1544 0.6623 0.0029 0.030 Uiso 1 1 calc R . . H9C H -0.1243 0.6044 0.0315 0.030 Uiso 1 1 calc R . . C10 C 0.1832(5) 0.5598(2) -0.02500(17) 0.0234(10) Uani 1 1 d . . . H10A H 0.1687 0.5407 0.0070 0.035 Uiso 1 1 calc R . . H10B H 0.2966 0.5676 -0.0317 0.035 Uiso 1 1 calc R . . H10C H 0.1296 0.5305 -0.0559 0.035 Uiso 1 1 calc R . . C11 C 0.6349(5) 0.88370(19) 0.18873(15) 0.0127(8) Uani 1 1 d . . . C12 C 0.7493(4) 0.83557(18) 0.19805(16) 0.0137(8) Uani 1 1 d . . . H12A H 0.7651 0.8388 0.2371 0.016 Uiso 1 1 calc R . . H12B H 0.8534 0.8483 0.1835 0.016 Uiso 1 1 calc R . . C13 C 0.8460(5) 0.70722(19) 0.17692(17) 0.0191(9) Uani 1 1 d . . . H13A H 0.8182 0.6624 0.1595 0.029 Uiso 1 1 calc R . . H13B H 0.8668 0.7098 0.2152 0.029 Uiso 1 1 calc R . . H13C H 0.9409 0.7254 0.1609 0.029 Uiso 1 1 calc R . . C14 C 0.5080(5) 0.72181(19) 0.20012(16) 0.0184(9) Uani 1 1 d . . . H14A H 0.4206 0.7457 0.1941 0.028 Uiso 1 1 calc R . . H14B H 0.5304 0.7271 0.2386 0.028 Uiso 1 1 calc R . . H14C H 0.4784 0.6764 0.1850 0.028 Uiso 1 1 calc R . . C15 C 0.6417(5) 0.7441(2) 0.09717(15) 0.0189(9) Uani 1 1 d . . . H15A H 0.6161 0.6988 0.0809 0.028 Uiso 1 1 calc R . . H15B H 0.7351 0.7625 0.0804 0.028 Uiso 1 1 calc R . . H15C H 0.5516 0.7669 0.0919 0.028 Uiso 1 1 calc R . . C16 C 1.2083(4) 0.09237(19) 0.30160(15) 0.0130(8) Uani 1 1 d . . . C17 C 1.3536(4) 0.14009(18) 0.29408(16) 0.0137(8) Uani 1 1 d . . . H17A H 1.3675 0.1381 0.2552 0.016 Uiso 1 1 calc R . . H17B H 1.4489 0.1260 0.3085 0.016 Uiso 1 1 calc R . . C18 C 1.5373(4) 0.26718(19) 0.31651(16) 0.0180(9) Uani 1 1 d . . . H18A H 1.5416 0.3114 0.3357 0.027 Uiso 1 1 calc R . . H18B H 1.5522 0.2667 0.2783 0.027 Uiso 1 1 calc R . . H18C H 1.6213 0.2469 0.3305 0.027 Uiso 1 1 calc R . . C19 C 1.3129(5) 0.22981(19) 0.39689(15) 0.0166(9) Uani 1 1 d . . . H19A H 1.3141 0.2749 0.4136 0.025 Uiso 1 1 calc R . . H19B H 1.3973 0.2119 0.4132 0.025 Uiso 1 1 calc R . . H19C H 1.2101 0.2062 0.4022 0.025 Uiso 1 1 calc R . . C20 C 1.1862(5) 0.2556(2) 0.29549(16) 0.0182(9) Uani 1 1 d . . . H20A H 1.0837 0.2370 0.3066 0.027 Uiso 1 1 calc R . . H20B H 1.1915 0.2450 0.2564 0.027 Uiso 1 1 calc R . . H20C H 1.1979 0.3021 0.3072 0.027 Uiso 1 1 calc R . . C21 C 0.8206(5) 0.2298(2) 0.42892(16) 0.0169(9) Uani 1 1 d . . . C22 C 0.9230(5) 0.29582(19) 0.44392(16) 0.0169(9) Uani 1 1 d . . . H22A H 0.9264 0.3168 0.4124 0.020 Uiso 1 1 calc R . . H22B H 1.0328 0.2891 0.4524 0.020 Uiso 1 1 calc R . . C23 C 0.8250(5) 0.3142(2) 0.56048(17) 0.0255(10) Uani 1 1 d . . . H23A H 0.9153 0.2913 0.5652 0.038 Uiso 1 1 calc R . . H23B H 0.7271 0.2843 0.5563 0.038 Uiso 1 1 calc R . . H23C H 0.8186 0.3480 0.5919 0.038 Uiso 1 1 calc R . . C24 C 1.0057(5) 0.4173(2) 0.51646(18) 0.0263(10) Uani 1 1 d . . . H24A H 0.9735 0.4487 0.5463 0.039 Uiso 1 1 calc R . . H24B H 1.0226 0.4371 0.4850 0.039 Uiso 1 1 calc R . . H24C H 1.1042 0.4025 0.5264 0.039 Uiso 1 1 calc R . . C25 C 0.6648(5) 0.3746(2) 0.48299(18) 0.0262(10) Uani 1 1 d . . . H25A H 0.6324 0.4063 0.5126 0.039 Uiso 1 1 calc R . . H25B H 0.5833 0.3375 0.4757 0.039 Uiso 1 1 calc R . . H25C H 0.6783 0.3936 0.4510 0.039 Uiso 1 1 calc R . . C26 C 0.4926(5) -0.0324(2) 0.35176(16) 0.0167(9) Uani 1 1 d . . . C27 C 0.4273(4) -0.10265(19) 0.32581(16) 0.0156(9) Uani 1 1 d . . . H27A H 0.5121 -0.1301 0.3275 0.019 Uiso 1 1 calc R . . H27B H 0.4009 -0.1044 0.2876 0.019 Uiso 1 1 calc R . . C28 C 0.2885(5) -0.1376(2) 0.42772(16) 0.0191(9) Uani 1 1 d . . . H28A H 0.3229 -0.0942 0.4473 0.029 Uiso 1 1 calc R . . H28B H 0.3716 -0.1647 0.4306 0.029 Uiso 1 1 calc R . . H28C H 0.1911 -0.1550 0.4430 0.029 Uiso 1 1 calc R . . C29 C 0.0903(5) -0.0895(2) 0.35037(17) 0.0199(9) Uani 1 1 d . . . H29A H -0.0053 -0.1080 0.3659 0.030 Uiso 1 1 calc R . . H29B H 0.0696 -0.0902 0.3123 0.030 Uiso 1 1 calc R . . H29C H 0.1195 -0.0452 0.3690 0.030 Uiso 1 1 calc R . . C30 C 0.1966(5) -0.21633(19) 0.31962(18) 0.0216(10) Uani 1 1 d . . . H30A H 0.0990 -0.2355 0.3335 0.032 Uiso 1 1 calc R . . H30B H 0.2820 -0.2422 0.3231 0.032 Uiso 1 1 calc R . . H30C H 0.1794 -0.2147 0.2818 0.032 Uiso 1 1 calc R . . C31 C 0.4106(5) 0.3153(2) 0.15664(19) 0.0260(10) Uani 1 1 d . . . C32 C 0.3717(5) 0.1067(2) 0.0122(2) 0.0336(12) Uani 1 1 d . . . C33 C 0.1257(5) 0.5790(2) 0.21017(17) 0.0223(10) Uani 1 1 d . . . C34 C 0.5569(5) 0.5110(2) 0.16667(17) 0.0209(10) Uani 1 1 d . . . C35 C 0.7226(6) 0.6700(2) 0.3520(2) 0.0328(12) Uani 1 1 d . . . C36 C 0.7900(6) 0.8966(2) 0.47594(19) 0.0316(12) Uani 1 1 d . . . C37 C 0.4310(7) 0.4812(3) 0.3468(3) 0.0489(15) Uani 1 1 d . . . C38 C -0.0716(6) 0.4079(2) 0.27382(19) 0.0302(11) Uani 1 1 d . . . H10E H 0.363(7) 1.004(3) 0.238(2) 0.080 Uiso 1 1 d . . . H20D H 0.614(7) 0.147(3) 0.423(2) 0.080 Uiso 1 1 d . . . H10D H 0.499(7) 0.980(3) 0.217(2) 0.080 Uiso 1 1 d . . . H21B H 0.850(7) -0.025(3) 0.250(2) 0.080 Uiso 1 1 d . . . H21A H 0.993(7) -0.003(3) 0.272(3) 0.080 Uiso 1 1 d . . . H11A H -0.049(7) 0.9060(18) 0.090(2) 0.080 Uiso 1 1 d D . . H20E H 0.524(7) 0.081(3) 0.404(2) 0.080 Uiso 1 1 d . . . H11B H -0.017(7) 0.837(2) 0.0704(17) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.00904(7) 0.01185(8) 0.01253(8) 0.00236(6) -0.00033(6) 0.00223(6) U2 0.00913(7) 0.01280(8) 0.01308(8) 0.00251(6) 0.00023(6) 0.00172(6) P1 0.0126(5) 0.0150(6) 0.0201(6) 0.0067(5) -0.0003(4) 0.0037(4) P2 0.0163(5) 0.0138(6) 0.0148(5) -0.0001(4) -0.0012(4) -0.0003(4) P3 0.0127(5) 0.0130(5) 0.0135(5) 0.0025(4) -0.0010(4) 0.0033(4) P4 0.0124(5) 0.0136(6) 0.0137(5) 0.0014(4) 0.0010(4) 0.0021(4) P5 0.0187(6) 0.0146(6) 0.0165(6) 0.0001(4) -0.0001(4) 0.0051(4) P6 0.0125(5) 0.0164(6) 0.0190(6) 0.0067(5) 0.0019(4) 0.0003(4) S1 0.0169(5) 0.0164(6) 0.0165(5) 0.0036(4) 0.0031(4) 0.0017(4) S2 0.0180(5) 0.0304(6) 0.0140(5) 0.0068(5) -0.0003(4) 0.0058(5) S3 0.0169(5) 0.0173(6) 0.0172(5) 0.0020(4) -0.0017(4) -0.0004(4) S4 0.0185(5) 0.0162(6) 0.0180(5) 0.0032(4) -0.0007(4) 0.0006(4) S5 0.0167(5) 0.0206(6) 0.0172(5) 0.0044(4) -0.0024(4) 0.0027(4) S6 0.0191(6) 0.0324(7) 0.0147(5) 0.0077(5) 0.0025(4) 0.0060(5) S7 0.0243(6) 0.0148(6) 0.0220(6) 0.0011(4) -0.0032(5) 0.0050(4) S8 0.0272(6) 0.0277(7) 0.0232(6) 0.0038(5) -0.0011(5) 0.0124(5) F1 0.0518(19) 0.0222(15) 0.0488(19) -0.0042(13) 0.0253(15) 0.0066(13) F2 0.070(2) 0.0223(16) 0.0443(18) 0.0168(14) 0.0050(16) 0.0089(15) F3 0.0310(16) 0.0349(17) 0.0539(19) -0.0090(14) 0.0014(14) -0.0113(13) F4 0.0375(18) 0.0365(19) 0.093(3) -0.0156(18) 0.0322(18) -0.0175(15) F5 0.0374(16) 0.0234(15) 0.0344(16) -0.0052(12) 0.0018(13) 0.0035(12) F6 0.0357(17) 0.080(2) 0.0422(19) -0.0338(17) -0.0216(15) 0.0125(17) F7 0.0348(16) 0.0555(19) 0.0177(14) 0.0036(13) -0.0028(12) 0.0157(14) F8 0.0231(14) 0.0415(17) 0.0292(15) 0.0046(13) 0.0074(11) -0.0011(12) F9 0.0342(15) 0.0233(15) 0.0371(16) -0.0076(12) 0.0005(12) 0.0036(12) F10 0.0315(15) 0.0254(15) 0.0298(15) 0.0128(12) 0.0046(12) 0.0063(12) F11 0.0401(16) 0.0270(15) 0.0238(14) -0.0030(12) -0.0105(12) 0.0036(12) F12 0.0301(15) 0.0354(16) 0.0328(15) 0.0078(13) 0.0000(12) 0.0170(12) F13 0.105(3) 0.0272(17) 0.0434(19) 0.0181(15) -0.0049(19) -0.0079(18) F14 0.057(2) 0.0382(19) 0.072(2) -0.0100(17) -0.0153(18) 0.0271(16) F15 0.065(2) 0.0285(17) 0.0455(19) -0.0043(14) -0.0158(16) -0.0094(15) F16 0.054(2) 0.067(2) 0.050(2) -0.0241(17) 0.0208(17) 0.0196(18) F17 0.0337(16) 0.0306(16) 0.0406(17) -0.0037(13) -0.0005(13) 0.0015(13) F18 0.0466(19) 0.0352(18) 0.071(2) 0.0068(16) -0.0183(17) 0.0188(15) F19 0.0302(18) 0.069(2) 0.115(3) 0.057(2) -0.0031(19) -0.0024(17) F20 0.080(3) 0.212(5) 0.042(2) 0.033(3) 0.034(2) 0.049(3) F21 0.047(2) 0.129(4) 0.161(4) 0.129(3) 0.000(2) 0.008(2) F22 0.056(2) 0.0283(18) 0.064(2) -0.0034(15) -0.0262(17) 0.0008(15) F23 0.059(2) 0.054(2) 0.049(2) 0.0003(16) -0.0281(16) 0.0248(17) F24 0.083(2) 0.052(2) 0.0347(18) 0.0137(16) 0.0250(17) 0.0190(18) O1 0.0192(15) 0.0176(16) 0.0146(15) 0.0027(12) 0.0039(12) 0.0038(12) O2 0.0103(13) 0.0152(15) 0.0197(15) 0.0059(12) -0.0014(11) 0.0007(11) O4 0.0154(14) 0.0170(16) 0.0183(15) 0.0025(12) -0.0034(12) 0.0068(12) O6 0.0219(16) 0.0206(17) 0.0240(17) -0.0009(13) -0.0090(13) 0.0063(13) O7 0.0155(14) 0.0152(15) 0.0183(15) 0.0007(12) -0.0041(12) 0.0022(12) O8 0.0093(14) 0.0147(15) 0.0246(16) 0.0006(12) -0.0036(12) 0.0025(11) O9 0.0134(14) 0.0103(15) 0.0201(15) 0.0001(12) -0.0021(12) 0.0003(11) O10 0.0118(14) 0.0174(16) 0.0187(16) 0.0000(12) -0.0004(12) 0.0033(12) O11 0.0140(14) 0.0147(16) 0.0220(16) 0.0024(12) -0.0039(12) 0.0060(12) O12 0.0134(14) 0.0175(15) 0.0149(14) 0.0040(12) 0.0015(11) 0.0036(12) O13 0.0225(16) 0.0177(16) 0.0170(15) 0.0047(12) -0.0023(12) 0.0042(12) O14 0.0111(14) 0.0154(15) 0.0225(16) -0.0014(12) 0.0021(12) 0.0042(11) O15 0.0134(14) 0.0120(15) 0.0223(16) 0.0018(12) 0.0014(12) 0.0034(11) O16 0.0129(14) 0.0238(17) 0.0168(15) 0.0039(13) 0.0046(12) -0.0026(12) O17 0.0196(15) 0.0213(17) 0.0190(16) 0.0038(13) 0.0071(12) 0.0016(13) O18 0.0163(15) 0.0149(15) 0.0184(15) -0.0004(12) 0.0045(12) 0.0030(12) O19 0.0194(16) 0.0243(18) 0.0276(18) -0.0061(14) 0.0089(13) -0.0014(13) O20 0.0154(15) 0.0171(17) 0.0188(16) 0.0040(13) 0.0028(12) 0.0003(12) O21 0.0095(14) 0.0179(16) 0.0212(16) -0.0001(13) -0.0010(12) 0.0003(12) O22 0.0147(15) 0.0291(18) 0.0273(17) 0.0015(14) 0.0060(13) -0.0002(13) O23 0.0381(19) 0.0320(19) 0.0139(16) 0.0056(14) 0.0036(14) 0.0117(15) O24 0.0310(19) 0.065(3) 0.0223(18) 0.0112(17) -0.0025(14) 0.0267(18) O25 0.0266(17) 0.041(2) 0.0202(17) 0.0117(15) 0.0074(13) 0.0037(15) O26 0.0193(16) 0.0171(16) 0.0293(17) 0.0008(13) 0.0020(13) -0.0029(13) O27 0.0177(15) 0.0321(19) 0.0259(17) 0.0107(14) -0.0067(13) 0.0025(13) O28 0.0219(16) 0.0219(17) 0.0200(16) -0.0044(13) 0.0000(13) 0.0014(13) O29 0.0198(16) 0.0246(17) 0.0256(17) 0.0062(14) 0.0014(13) -0.0022(13) O30 0.0161(16) 0.041(2) 0.0283(18) 0.0037(15) -0.0055(13) 0.0068(14) O31 0.0290(18) 0.036(2) 0.0159(16) 0.0055(14) -0.0015(13) -0.0014(15) O32 0.0243(17) 0.050(2) 0.0229(18) 0.0078(16) 0.0077(14) -0.0030(16) O33 0.0286(18) 0.045(2) 0.0187(16) 0.0115(15) -0.0050(14) 0.0116(15) O34 0.0359(19) 0.036(2) 0.0267(18) -0.0110(15) -0.0052(15) 0.0153(16) O35 0.0306(18) 0.0212(18) 0.052(2) 0.0051(16) -0.0145(16) 0.0085(15) O36 0.048(2) 0.067(3) 0.052(2) 0.036(2) 0.0243(19) 0.029(2) O37 0.039(2) 0.0217(18) 0.040(2) -0.0026(15) -0.0069(16) 0.0135(15) N1 0.0140(17) 0.023(2) 0.0119(17) 0.0032(15) -0.0007(13) 0.0053(15) N2 0.0148(18) 0.0152(19) 0.025(2) 0.0027(15) 0.0002(15) 0.0010(14) N4 0.030(2) 0.026(2) 0.050(3) -0.017(2) -0.019(2) 0.0172(18) O5 0.0254(16) 0.0174(16) 0.0202(16) 0.0022(13) -0.0095(13) 0.0074(13) N3 0.0121(17) 0.023(2) 0.0147(18) 0.0024(15) 0.0018(14) 0.0038(14) C1 0.011(2) 0.018(2) 0.020(2) 0.0082(18) 0.0055(17) 0.0035(16) C2 0.019(2) 0.015(2) 0.013(2) 0.0002(17) -0.0021(16) 0.0030(17) C3 0.020(2) 0.016(2) 0.026(2) 0.0065(19) -0.0015(18) 0.0053(18) C4 0.024(2) 0.022(2) 0.021(2) 0.0073(19) -0.0009(18) 0.0055(19) C5 0.019(2) 0.018(2) 0.030(3) 0.0067(19) 0.0013(19) 0.0014(18) C6 0.014(2) 0.018(2) 0.019(2) 0.0035(18) 0.0017(17) -0.0023(17) C7 0.014(2) 0.015(2) 0.019(2) -0.0017(17) -0.0041(17) 0.0017(17) C8 0.031(3) 0.030(3) 0.019(2) 0.005(2) -0.002(2) -0.002(2) C9 0.013(2) 0.022(2) 0.023(2) 0.0011(19) -0.0010(17) 0.0006(18) C10 0.019(2) 0.025(3) 0.023(2) -0.0041(19) -0.0025(18) 0.0033(19) C11 0.014(2) 0.015(2) 0.0088(19) 0.0009(16) 0.0019(15) 0.0053(16) C12 0.0092(19) 0.014(2) 0.017(2) 0.0004(17) -0.0035(16) 0.0007(16) C13 0.021(2) 0.016(2) 0.022(2) 0.0036(18) 0.0001(18) 0.0077(18) C14 0.020(2) 0.015(2) 0.021(2) 0.0034(18) 0.0026(18) 0.0021(17) C15 0.017(2) 0.021(2) 0.017(2) 0.0001(18) -0.0007(17) 0.0052(18) C16 0.012(2) 0.019(2) 0.0088(19) 0.0041(16) -0.0019(15) -0.0003(16) C17 0.0108(19) 0.014(2) 0.017(2) 0.0025(17) -0.0009(16) 0.0025(16) C18 0.015(2) 0.018(2) 0.019(2) 0.0010(18) 0.0046(17) 0.0001(17) C19 0.017(2) 0.017(2) 0.016(2) 0.0030(17) -0.0011(17) 0.0042(17) C20 0.016(2) 0.020(2) 0.019(2) 0.0023(18) -0.0014(17) 0.0034(17) C21 0.017(2) 0.016(2) 0.017(2) -0.0001(18) -0.0027(17) 0.0042(17) C22 0.015(2) 0.017(2) 0.018(2) 0.0019(18) 0.0050(17) 0.0024(17) C23 0.033(3) 0.023(3) 0.021(2) 0.005(2) 0.006(2) 0.006(2) C24 0.026(2) 0.020(2) 0.030(3) -0.001(2) 0.002(2) 0.001(2) C25 0.019(2) 0.025(3) 0.034(3) 0.000(2) 0.001(2) 0.0101(19) C26 0.011(2) 0.020(2) 0.020(2) 0.0079(18) -0.0046(17) 0.0002(17) C27 0.013(2) 0.018(2) 0.014(2) 0.0039(17) 0.0022(16) -0.0021(17) C28 0.015(2) 0.025(2) 0.019(2) 0.0079(19) 0.0020(17) 0.0015(18) C29 0.016(2) 0.022(2) 0.025(2) 0.0114(19) 0.0042(18) 0.0057(18) C30 0.015(2) 0.016(2) 0.034(3) 0.005(2) -0.0024(19) 0.0009(17) C31 0.026(3) 0.018(2) 0.031(3) 0.001(2) 0.008(2) 0.0001(19) C32 0.019(2) 0.037(3) 0.036(3) -0.009(2) 0.007(2) -0.006(2) C33 0.017(2) 0.025(3) 0.024(2) 0.003(2) 0.0004(18) 0.0029(19) C34 0.021(2) 0.019(2) 0.022(2) 0.0005(19) 0.0003(18) 0.0064(18) C35 0.041(3) 0.027(3) 0.029(3) 0.004(2) -0.008(2) 0.001(2) C36 0.028(3) 0.035(3) 0.030(3) -0.003(2) -0.001(2) 0.011(2) C37 0.032(3) 0.070(4) 0.057(4) 0.035(3) 0.004(3) 0.014(3) C38 0.041(3) 0.021(3) 0.028(3) 0.002(2) -0.006(2) 0.006(2) _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 O1 1.754(3) . ? U1 O2 1.769(3) . ? U1 O4 2.349(3) . ? U1 O7 2.354(3) . ? U1 O8 2.395(3) . ? U1 O10 2.428(3) . ? U1 O11 2.443(3) . ? U2 O13 1.753(3) . ? U2 O12 1.774(3) . ? U2 O16 2.351(3) . ? U2 O18 2.358(3) . ? U2 O14 2.376(3) . ? U2 O21 2.430(3) . ? U2 O20 2.435(3) . ? P1 C4 1.779(4) . ? P1 C5 1.780(4) . ? P1 C3 1.783(4) . ? P1 C2 1.794(4) . ? P2 C10 1.775(4) . ? P2 C9 1.780(4) . ? P2 C8 1.785(4) . ? P2 C7 1.805(4) . ? P3 C15 1.770(4) . ? P3 C14 1.775(4) . ? P3 C13 1.776(4) . ? P3 C12 1.800(4) . ? P4 C19 1.780(4) . ? P4 C20 1.781(4) . ? P4 C18 1.787(4) . ? P4 C17 1.791(4) . ? P5 C25 1.779(4) . ? P5 C24 1.780(4) . ? P5 C23 1.785(4) . ? P5 C22 1.801(4) . ? P6 C29 1.776(4) . ? P6 C30 1.784(4) . ? P6 C28 1.785(4) . ? P6 C27 1.800(4) . ? S1 O22 1.424(3) . ? S1 O23 1.434(3) . ? S1 N1 1.565(3) . ? S1 C31 1.820(4) . ? S2 O25 1.423(3) . ? S2 O24 1.430(3) . ? S2 N1 1.584(3) . ? S2 C32 1.822(5) . ? S3 O26 1.427(3) . ? S3 O27 1.433(3) . ? S3 N2 1.583(3) . ? S3 C33 1.834(4) . ? S4 O28 1.425(3) . ? S4 O29 1.430(3) . ? S4 N2 1.579(3) . ? S4 C34 1.830(4) . ? S5 O31 1.428(3) . ? S5 O30 1.428(3) . ? S5 N3 1.571(3) . ? S5 C35 1.830(5) . ? S6 O33 1.426(3) . ? S6 O32 1.426(3) . ? S6 N3 1.586(3) . ? S6 C36 1.826(5) . ? S7 O34 1.418(3) . ? S7 O35 1.422(3) . ? S7 N4 1.557(4) . ? S7 C37 1.812(6) . ? S8 O37 1.422(3) . ? S8 O36 1.423(3) . ? S8 N4 1.582(4) . ? S8 C38 1.819(5) . ? F1 C31 1.324(5) . ? F2 C31 1.315(5) . ? F3 C31 1.334(5) . ? F4 C32 1.329(5) . ? F5 C32 1.325(5) . ? F6 C32 1.329(5) . ? F7 C33 1.315(5) . ? F8 C33 1.323(5) . ? F9 C33 1.333(5) . ? F10 C34 1.319(5) . ? F11 C34 1.326(5) . ? F12 C34 1.339(4) . ? F13 C35 1.326(5) . ? F14 C35 1.315(6) . ? F15 C35 1.325(5) . ? F16 C36 1.326(5) . ? F17 C36 1.323(5) . ? F18 C36 1.329(5) . ? F19 C37 1.314(6) . ? F20 C37 1.332(7) . ? F21 C37 1.306(6) . ? F22 C38 1.325(5) . ? F23 C38 1.330(5) . ? F24 C38 1.306(5) . ? O4 C1 1.278(4) . ? O6 C6 1.235(5) . ? O7 C6 1.290(4) . ? O8 C11 1.267(4) . ? O9 C11 1.237(4) . ? O14 C16 1.274(4) . ? O15 C16 1.243(4) . ? O16 C26 1.276(4) . ? O17 C26 1.235(5) . ? O18 C21 1.277(4) . ? O19 C21 1.232(5) . ? O5 C1 1.233(4) . ? C1 C2 1.525(5) . ? C6 C7 1.512(5) . ? C11 C12 1.520(5) . ? C16 C17 1.512(5) . ? C21 C22 1.520(5) . ? C26 C27 1.528(5) . ? 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 O1 U1 O2 179.49(13) . . ? O1 U1 O4 91.51(11) . . ? O2 U1 O4 88.22(11) . . ? O1 U1 O7 92.47(11) . . ? O2 U1 O7 88.01(11) . . ? O4 U1 O7 142.08(9) . . ? O1 U1 O8 91.31(11) . . ? O2 U1 O8 88.64(10) . . ? O4 U1 O8 142.02(9) . . ? O7 U1 O8 75.55(9) . . ? O1 U1 O10 90.48(11) . . ? O2 U1 O10 89.02(11) . . ? O4 U1 O10 70.10(9) . . ? O7 U1 O10 147.49(9) . . ? O8 U1 O10 72.01(9) . . ? O1 U1 O11 89.46(11) . . ? O2 U1 O11 90.85(11) . . ? O4 U1 O11 70.45(9) . . ? O7 U1 O11 71.90(9) . . ? O8 U1 O11 147.45(9) . . ? O10 U1 O11 140.53(9) . . ? O13 U2 O12 178.92(12) . . ? O13 U2 O16 91.81(11) . . ? O12 U2 O16 88.33(11) . . ? O13 U2 O18 92.57(11) . . ? O12 U2 O18 87.98(11) . . ? O16 U2 O18 141.44(9) . . ? O13 U2 O14 90.21(11) . . ? O12 U2 O14 89.03(10) . . ? O16 U2 O14 142.92(9) . . ? O18 U2 O14 75.35(9) . . ? O13 U2 O21 91.14(11) . . ? O12 U2 O21 87.90(11) . . ? O16 U2 O21 70.63(9) . . ? O18 U2 O21 147.46(9) . . ? O14 U2 O21 72.31(9) . . ? O13 U2 O20 90.71(11) . . ? O12 U2 O20 90.34(10) . . ? O16 U2 O20 70.30(9) . . ? O18 U2 O20 71.36(9) . . ? O14 U2 O20 146.71(9) . . ? O21 U2 O20 140.92(10) . . ? C4 P1 C5 111.6(2) . . ? C4 P1 C3 109.6(2) . . ? C5 P1 C3 108.0(2) . . ? C4 P1 C2 112.54(19) . . ? C5 P1 C2 108.86(19) . . ? C3 P1 C2 106.08(19) . . ? C10 P2 C9 110.5(2) . . ? C10 P2 C8 108.9(2) . . ? C9 P2 C8 109.0(2) . . ? C10 P2 C7 105.39(19) . . ? C9 P2 C7 111.65(19) . . ? C8 P2 C7 111.3(2) . . ? C15 P3 C14 109.93(19) . . ? C15 P3 C13 108.82(19) . . ? C14 P3 C13 110.61(19) . . ? C15 P3 C12 110.08(19) . . ? C14 P3 C12 110.75(19) . . ? C13 P3 C12 106.58(18) . . ? C19 P4 C20 109.22(19) . . ? C19 P4 C18 108.85(19) . . ? C20 P4 C18 110.97(19) . . ? C19 P4 C17 110.33(19) . . ? C20 P4 C17 110.82(19) . . ? C18 P4 C17 106.60(18) . . ? C25 P5 C24 111.3(2) . . ? C25 P5 C23 109.2(2) . . ? C24 P5 C23 107.8(2) . . ? C25 P5 C22 110.1(2) . . ? C24 P5 C22 105.20(19) . . ? C23 P5 C22 113.1(2) . . ? C29 P6 C30 108.2(2) . . ? C29 P6 C28 110.73(19) . . ? C30 P6 C28 110.3(2) . . ? C29 P6 C27 109.12(19) . . ? C30 P6 C27 105.86(19) . . ? C28 P6 C27 112.47(18) . . ? O22 S1 O23 117.27(18) . . ? O22 S1 N1 117.63(17) . . ? O23 S1 N1 108.09(17) . . ? O22 S1 C31 104.1(2) . . ? O23 S1 C31 103.9(2) . . ? N1 S1 C31 103.88(19) . . ? O25 S2 O24 119.67(19) . . ? O25 S2 N1 107.99(17) . . ? O24 S2 N1 115.57(18) . . ? O25 S2 C32 104.0(2) . . ? O24 S2 C32 104.9(2) . . ? N1 S2 C32 102.6(2) . . ? O26 S3 O27 118.08(18) . . ? O26 S3 N2 116.57(18) . . ? O27 S3 N2 109.74(18) . . ? O26 S3 C33 106.28(19) . . ? O27 S3 C33 103.49(19) . . ? N2 S3 C33 100.02(19) . . ? O28 S4 O29 119.22(18) . . ? O28 S4 N2 115.60(17) . . ? O29 S4 N2 107.26(18) . . ? O28 S4 C34 104.99(19) . . ? O29 S4 C34 103.29(19) . . ? N2 S4 C34 104.75(19) . . ? O31 S5 O30 117.38(18) . . ? O31 S5 N3 108.28(18) . . ? O30 S5 N3 117.07(18) . . ? O31 S5 C35 103.4(2) . . ? O30 S5 C35 105.4(2) . . ? N3 S5 C35 103.3(2) . . ? O33 S6 O32 119.61(19) . . ? O33 S6 N3 107.54(18) . . ? O32 S6 N3 116.10(18) . . ? O33 S6 C36 104.2(2) . . ? O32 S6 C36 104.8(2) . . ? N3 S6 C36 102.3(2) . . ? O34 S7 O35 118.3(2) . . ? O34 S7 N4 114.9(2) . . ? O35 S7 N4 108.6(2) . . ? O34 S7 C37 104.9(3) . . ? O35 S7 C37 103.4(2) . . ? N4 S7 C37 105.3(3) . . ? O37 S8 O36 118.2(2) . . ? O37 S8 N4 116.4(2) . . ? O36 S8 N4 110.9(2) . . ? O37 S8 C38 106.5(2) . . ? O36 S8 C38 104.2(2) . . ? N4 S8 C38 97.5(2) . . ? C1 O4 U1 136.3(2) . . ? C6 O7 U1 137.0(3) . . ? C11 O8 U1 139.7(2) . . ? C16 O14 U2 139.7(2) . . ? C26 O16 U2 137.8(3) . . ? C21 O18 U2 139.8(3) . . ? S1 N1 S2 124.2(2) . . ? S4 N2 S3 126.0(2) . . ? S7 N4 S8 124.7(2) . . ? S5 N3 S6 124.0(2) . . ? O5 C1 O4 126.1(4) . . ? O5 C1 C2 118.9(3) . . ? O4 C1 C2 115.0(3) . . ? C1 C2 P1 114.9(3) . . ? O6 C6 O7 125.5(4) . . ? O6 C6 C7 119.3(4) . . ? O7 C6 C7 115.1(3) . . ? C6 C7 P2 113.7(3) . . ? O9 C11 O8 124.9(4) . . ? O9 C11 C12 117.7(3) . . ? O8 C11 C12 117.3(3) . . ? C11 C12 P3 115.1(3) . . ? O15 C16 O14 125.0(4) . . ? O15 C16 C17 118.1(3) . . ? O14 C16 C17 116.9(3) . . ? C16 C17 P4 115.8(3) . . ? O19 C21 O18 125.8(4) . . ? O19 C21 C22 118.8(4) . . ? O18 C21 C22 115.4(3) . . ? C21 C22 P5 114.2(3) . . ? O17 C26 O16 126.7(4) . . ? O17 C26 C27 118.9(3) . . ? O16 C26 C27 114.4(3) . . ? C26 C27 P6 114.4(3) . . ? F2 C31 F1 109.1(4) . . ? F2 C31 F3 108.1(4) . . ? F1 C31 F3 107.8(4) . . ? F2 C31 S1 111.7(3) . . ? F1 C31 S1 109.6(3) . . ? F3 C31 S1 110.5(3) . . ? F5 C32 F6 108.5(4) . . ? F5 C32 F4 107.8(4) . . ? F6 C32 F4 109.4(4) . . ? F5 C32 S2 111.9(3) . . ? F6 C32 S2 108.8(4) . . ? F4 C32 S2 110.4(3) . . ? F7 C33 F8 109.4(4) . . ? F7 C33 F9 108.3(3) . . ? F8 C33 F9 108.3(3) . . ? F7 C33 S3 111.4(3) . . ? F8 C33 S3 109.1(3) . . ? F9 C33 S3 110.3(3) . . ? F10 C34 F11 108.5(3) . . ? F10 C34 F12 108.4(3) . . ? F11 C34 F12 108.4(3) . . ? F10 C34 S4 111.6(3) . . ? F11 C34 S4 110.6(3) . . ? F12 C34 S4 109.3(3) . . ? F14 C35 F15 109.3(4) . . ? F14 C35 F13 108.8(4) . . ? F15 C35 F13 108.3(4) . . ? F14 C35 S5 111.0(3) . . ? F15 C35 S5 109.3(3) . . ? F13 C35 S5 110.1(3) . . ? F17 C36 F16 108.7(4) . . ? F17 C36 F18 107.6(4) . . ? F16 C36 F18 109.4(4) . . ? F17 C36 S6 111.4(3) . . ? F16 C36 S6 109.3(4) . . ? F18 C36 S6 110.5(3) . . ? F21 C37 F19 109.5(5) . . ? F21 C37 F20 108.9(5) . . ? F19 C37 F20 108.6(5) . . ? F21 C37 S7 110.6(4) . . ? F19 C37 S7 110.1(4) . . ? F20 C37 S7 109.0(4) . . ? F24 C38 F22 108.4(4) . . ? F24 C38 F23 108.5(4) . . ? F22 C38 F23 108.3(4) . . ? F24 C38 S8 111.9(3) . . ? F22 C38 S8 111.1(3) . . ? F23 C38 S8 108.6(3) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.122 _refine_diff_density_min -1.115 _refine_diff_density_rms 0.129 data_apx1524 _database_code_depnum_ccdc_archive 'CCDC 904330' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H66 F24 N4 O32 P6 S8 U2' _chemical_formula_weight 2465.31 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _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 14.9671(7) _cell_length_b 17.1019(8) _cell_length_c 17.3543(8) _cell_angle_alpha 87.020(1) _cell_angle_beta 77.318(1) _cell_angle_gamma 74.0413(4) _cell_volume 4166.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.965 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 4.327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4782 _exptl_absorpt_correction_T_max 0.7234 _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 47312 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.44 _reflns_number_total 19106 _reflns_number_gt 16379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL, v. 6.14, (Bruker AXS, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19106 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0535 _refine_ls_wR_factor_gt 0.0509 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.005 _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 0.365327(7) 0.966514(6) 0.126149(5) 0.01239(3) Uani 1 1 d . . . U2 U 0.388987(7) 0.444916(6) 0.131598(5) 0.01321(3) Uani 1 1 d . . . P1 P 0.20745(5) 0.97101(4) 0.41522(4) 0.01413(14) Uani 1 1 d . . . P2 P 0.18631(5) 0.75284(4) 0.06137(4) 0.01528(14) Uani 1 1 d . . . P3 P 0.43769(5) 0.87350(4) -0.21313(4) 0.01494(14) Uani 1 1 d . . . P4 P 0.21667(5) 0.39873(4) 0.43026(4) 0.01594(15) Uani 1 1 d . . . P5 P 0.15546(5) 0.27752(4) 0.12847(4) 0.01486(14) Uani 1 1 d . . . P6 P 0.45507(5) 0.34509(4) -0.20637(4) 0.01336(14) Uani 1 1 d . . . S1 S 0.15318(5) 0.68493(5) 0.38992(5) 0.02795(18) Uani 1 1 d . . . S2 S 0.02170(5) 0.76726(5) 0.51837(5) 0.02835(18) Uani 1 1 d . . . S3 S 0.48913(5) 0.28966(5) 0.52815(4) 0.02009(15) Uani 1 1 d . . . S4 S 0.46269(5) 0.13926(5) 0.49620(4) 0.02321(16) Uani 1 1 d . . . S5 S 0.14160(5) 0.07356(5) 0.90070(4) 0.02161(16) Uani 1 1 d . . . S6 S 0.09018(5) 0.04257(4) 0.76266(4) 0.02085(15) Uani 1 1 d . . . S7 S 0.88445(5) 0.50318(4) 0.24960(4) 0.01717(14) Uani 1 1 d . . . S8 S 0.82659(5) 0.40782(4) 0.15491(4) 0.02201(16) Uani 1 1 d . . . F1 F 0.14022(16) 0.66784(12) 0.59382(12) 0.0504(6) Uani 1 1 d . . . F2 F 0.14305(14) 0.79166(12) 0.59588(11) 0.0411(5) Uani 1 1 d . . . F3 F 0.02640(15) 0.75445(14) 0.66694(11) 0.0505(6) Uani 1 1 d . . . F4 F 0.04477(14) 0.73836(11) 0.28707(11) 0.0398(5) Uani 1 1 d . . . F5 F 0.12213(14) 0.61190(11) 0.27594(11) 0.0407(5) Uani 1 1 d . . . F6 F -0.00144(13) 0.65183(12) 0.36863(10) 0.0348(5) Uani 1 1 d . . . F7 F 0.36579(17) 0.15854(13) 0.64204(10) 0.0527(6) Uani 1 1 d . . . F8 F 0.35890(14) 0.05455(11) 0.58244(11) 0.0373(5) Uani 1 1 d . . . F9 F 0.27934(14) 0.17321(13) 0.55554(12) 0.0479(6) Uani 1 1 d . . . F10 F 0.24639(13) 0.14704(11) 0.79590(11) 0.0357(5) Uani 1 1 d . . . F11 F 0.14611(15) 0.22615(11) 0.88614(13) 0.0475(6) Uani 1 1 d . . . F12 F 0.27205(14) 0.14355(13) 0.91329(12) 0.0459(5) Uani 1 1 d . . . F13 F 0.04883(15) -0.08775(11) 0.72924(12) 0.0428(5) Uani 1 1 d . . . F14 F -0.05140(13) -0.01786(12) 0.82602(13) 0.0432(5) Uani 1 1 d . . . F15 F 0.08459(14) -0.09114(11) 0.84278(11) 0.0377(5) Uani 1 1 d . . . F16 F 0.57684(16) 0.32292(14) 0.38846(11) 0.0510(6) Uani 1 1 d . . . F17 F 0.64317(15) 0.33630(15) 0.48339(13) 0.0566(6) Uani 1 1 d . . . F18 F 0.65512(13) 0.21697(13) 0.44074(12) 0.0461(5) Uani 1 1 d . . . F19 F 1.03836(14) 0.52605(12) 0.15697(12) 0.0459(5) Uani 1 1 d . . . F20 F 0.93800(14) 0.63457(11) 0.21269(12) 0.0391(5) Uani 1 1 d . . . F21 F 0.90994(18) 0.57927(14) 0.11530(12) 0.0574(7) Uani 1 1 d . . . F22 F 0.72129(13) 0.39965(12) 0.29630(11) 0.0395(5) Uani 1 1 d . . . F23 F 0.68032(15) 0.35064(13) 0.20160(14) 0.0561(6) Uani 1 1 d . . . F24 F 0.80415(15) 0.28350(11) 0.24472(13) 0.0456(5) Uani 1 1 d . . . N1 N 0.09928(18) 0.76457(14) 0.44009(14) 0.0241(6) Uani 1 1 d . . . N2 N 0.44532(17) 0.23477(15) 0.48582(13) 0.0227(5) Uani 1 1 d . . . N3 N 0.06941(16) 0.08993(14) 0.84387(14) 0.0214(5) Uani 1 1 d . . . N4 N 0.90095(16) 0.42344(14) 0.19957(13) 0.0190(5) Uani 1 1 d . . . O1 O 0.46122(13) 0.88757(11) 0.14704(12) 0.0215(4) Uani 1 1 d . . . O2 O 0.26904(13) 1.04414(11) 0.10499(11) 0.0187(4) Uani 1 1 d . . . O3 O 0.33231(13) 1.00937(11) 0.25624(10) 0.0177(4) Uani 1 1 d . . . O4 O 0.24432(15) 1.13840(12) 0.27192(11) 0.0258(5) Uani 1 1 d . . . O5 O 0.25154(13) 0.89565(11) 0.20058(10) 0.0169(4) Uani 1 1 d . . . O6 O 0.30224(13) 0.86362(11) 0.07463(11) 0.0188(4) Uani 1 1 d . . . O7 O 0.43338(15) 0.95419(13) -0.00676(11) 0.0285(5) Uani 1 1 d . . . O8 O 0.54190(13) 0.93841(11) -0.11834(10) 0.0156(4) Uani 1 1 d . . . O9 O 0.49381(13) 0.36581(12) 0.13115(11) 0.0223(4) Uani 1 1 d . . . O10 O 0.28416(14) 0.52472(11) 0.13387(11) 0.0192(4) Uani 1 1 d . . . O11 O 0.39177(14) 0.48554(12) 0.26516(11) 0.0211(4) Uani 1 1 d . . . O12 O 0.31106(13) 0.39750(11) 0.25913(10) 0.0168(4) Uani 1 1 d . . . O13 O 0.31433(13) 0.35203(11) 0.10137(10) 0.0159(4) Uani 1 1 d . . . O14 O 0.42748(13) 0.24802(11) 0.03624(11) 0.0195(4) Uani 1 1 d . . . O15 O 0.42357(14) 0.45875(12) -0.00469(11) 0.0240(5) Uani 1 1 d . . . O16 O 0.52253(14) 0.45596(12) -0.12055(10) 0.0207(4) Uani 1 1 d . . . O17 O 0.16873(16) 0.61151(13) 0.43399(14) 0.0385(6) Uani 1 1 d . . . O18 O 0.23055(17) 0.70197(17) 0.33386(15) 0.0537(8) Uani 1 1 d . . . O19 O -0.02866(17) 0.70732(17) 0.52477(13) 0.0467(7) Uani 1 1 d . . . O20 O -0.02961(18) 0.85057(15) 0.53368(14) 0.0550(8) Uani 1 1 d . . . O21 O 0.43091(15) 0.37114(12) 0.52997(12) 0.0290(5) Uani 1 1 d . . . O22 O 0.52071(14) 0.25754(12) 0.59821(11) 0.0235(5) Uani 1 1 d . . . O23 O 0.54428(16) 0.09672(13) 0.52557(13) 0.0349(6) Uani 1 1 d . . . O24 O 0.44488(15) 0.10825(13) 0.42767(11) 0.0301(5) Uani 1 1 d . . . O25 O 0.08947(15) 0.09709(14) 0.97896(12) 0.0349(6) Uani 1 1 d . . . O26 O 0.21534(14) -0.00129(12) 0.88882(12) 0.0250(5) Uani 1 1 d . . . O27 O 0.18754(15) 0.00678(13) 0.72785(12) 0.0280(5) Uani 1 1 d . . . O28 O 0.02917(16) 0.08990(12) 0.71492(12) 0.0307(5) Uani 1 1 d . . . O30 O 0.78922(14) 0.55292(12) 0.27075(13) 0.0282(5) Uani 1 1 d . . . O31 O 0.75939(14) 0.47774(12) 0.13337(12) 0.0266(5) Uani 1 1 d . . . O32 O 0.87571(16) 0.34586(14) 0.09673(13) 0.0376(6) Uani 1 1 d . . . O29 O 0.94011(14) 0.48362(12) 0.30804(11) 0.0246(5) Uani 1 1 d . . . C10 C 0.1461(2) 0.82660(18) -0.00827(16) 0.0232(6) Uani 1 1 d . . . H10A H 0.1423 0.7997 -0.0541 0.035 Uiso 1 1 calc R . . H10B H 0.1898 0.8593 -0.0233 0.035 Uiso 1 1 calc R . . H10C H 0.0843 0.8607 0.0150 0.035 Uiso 1 1 calc R . . C1 C 0.27678(19) 1.07144(17) 0.29735(15) 0.0171(6) Uani 1 1 d . . . C2 C 0.2562(2) 1.05577(16) 0.38621(15) 0.0173(6) Uani 1 1 d . . . H2A H 0.2120 1.1043 0.4126 0.021 Uiso 1 1 calc R . . H2B H 0.3149 1.0466 0.4046 0.021 Uiso 1 1 calc R . . C3 C 0.1079(2) 0.97813(18) 0.37291(17) 0.0228(6) Uani 1 1 d . . . H3A H 0.1278 0.9754 0.3164 0.034 Uiso 1 1 calc R . . H3B H 0.0611 1.0289 0.3883 0.034 Uiso 1 1 calc R . . H3C H 0.0808 0.9340 0.3911 0.034 Uiso 1 1 calc R . . C4 C 0.2926(2) 0.87721(16) 0.38474(17) 0.0217(6) Uani 1 1 d . . . H4A H 0.2659 0.8331 0.4041 0.033 Uiso 1 1 calc R . . H4B H 0.3481 0.8730 0.4055 0.033 Uiso 1 1 calc R . . H4C H 0.3098 0.8747 0.3281 0.033 Uiso 1 1 calc R . . C5 C 0.1729(2) 0.97516(19) 0.52043(16) 0.0264(7) Uani 1 1 d . . . H5A H 0.1452 0.9314 0.5389 0.040 Uiso 1 1 calc R . . H5B H 0.1271 1.0262 0.5367 0.040 Uiso 1 1 calc R . . H5C H 0.2277 0.9701 0.5424 0.040 Uiso 1 1 calc R . . C6 C 0.25031(18) 0.85662(16) 0.14115(16) 0.0153(6) Uani 1 1 d . . . C7 C 0.18626(19) 0.80114(16) 0.15092(15) 0.0159(6) Uani 1 1 d . . . H7A H 0.1218 0.8323 0.1733 0.019 Uiso 1 1 calc R . . H7B H 0.2054 0.7593 0.1885 0.019 Uiso 1 1 calc R . . C8 C 0.1057(2) 0.69179(18) 0.08861(17) 0.0239(7) Uani 1 1 d . . . H8A H 0.0447 0.7251 0.1147 0.036 Uiso 1 1 calc R . . H8B H 0.1295 0.6498 0.1237 0.036 Uiso 1 1 calc R . . H8C H 0.0995 0.6675 0.0421 0.036 Uiso 1 1 calc R . . C9 C 0.3016(2) 0.68931(17) 0.02012(17) 0.0224(6) Uani 1 1 d . . . H9A H 0.3218 0.6492 0.0581 0.034 Uiso 1 1 calc R . . H9B H 0.3457 0.7218 0.0065 0.034 Uiso 1 1 calc R . . H9C H 0.2993 0.6626 -0.0264 0.034 Uiso 1 1 calc R . . C11 C 0.46790(18) 0.92649(15) -0.07431(15) 0.0136(5) Uani 1 1 d . . . C12 C 0.41617(19) 0.87572(16) -0.10741(14) 0.0136(5) Uani 1 1 d . . . H12A H 0.3484 0.8969 -0.0868 0.016 Uiso 1 1 calc R . . H12B H 0.4352 0.8204 -0.0887 0.016 Uiso 1 1 calc R . . C13 C 0.5508(2) 0.80616(17) -0.25188(16) 0.0231(6) Uani 1 1 d . . . H13A H 0.5544 0.7535 -0.2286 0.035 Uiso 1 1 calc R . . H13B H 0.5997 0.8269 -0.2399 0.035 Uiso 1 1 calc R . . H13C H 0.5595 0.8016 -0.3081 0.035 Uiso 1 1 calc R . . C14 C 0.3485(2) 0.83484(19) -0.23783(18) 0.0280(7) Uani 1 1 d . . . H14A H 0.3571 0.8328 -0.2942 0.042 Uiso 1 1 calc R . . H14B H 0.2868 0.8698 -0.2157 0.042 Uiso 1 1 calc R . . H14C H 0.3535 0.7811 -0.2169 0.042 Uiso 1 1 calc R . . C15 C 0.4280(2) 0.97228(16) -0.25468(16) 0.0204(6) Uani 1 1 d . . . H15A H 0.4729 0.9956 -0.2390 0.031 Uiso 1 1 calc R . . H15B H 0.3647 1.0063 -0.2362 0.031 Uiso 1 1 calc R . . H15C H 0.4413 0.9681 -0.3112 0.031 Uiso 1 1 calc R . . C16 C 0.34017(19) 0.44155(16) 0.29922(15) 0.0152(6) Uani 1 1 d . . . C17 C 0.31391(19) 0.44146(17) 0.38807(15) 0.0163(6) Uani 1 1 d . . . H17A H 0.2976 0.4971 0.4069 0.020 Uiso 1 1 calc R . . H17B H 0.3694 0.4113 0.4075 0.020 Uiso 1 1 calc R . . C18 C 0.11133(19) 0.44963(17) 0.39728(17) 0.0217(6) Uani 1 1 d . . . H18A H 0.1251 0.4513 0.3406 0.033 Uiso 1 1 calc R . . H18B H 0.0882 0.5041 0.4182 0.033 Uiso 1 1 calc R . . H18C H 0.0638 0.4209 0.4152 0.033 Uiso 1 1 calc R . . C19 C 0.1949(2) 0.4117(2) 0.53431(16) 0.0308(8) Uani 1 1 d . . . H19A H 0.1754 0.4687 0.5471 0.046 Uiso 1 1 calc R . . H19B H 0.2520 0.3863 0.5526 0.046 Uiso 1 1 calc R . . H19C H 0.1455 0.3872 0.5594 0.046 Uiso 1 1 calc R . . C20 C 0.2484(2) 0.29347(16) 0.40651(17) 0.0209(6) Uani 1 1 d . . . H20A H 0.1988 0.2701 0.4337 0.031 Uiso 1 1 calc R . . H20B H 0.3067 0.2666 0.4225 0.031 Uiso 1 1 calc R . . H20C H 0.2568 0.2868 0.3506 0.031 Uiso 1 1 calc R . . C21 C 0.34795(19) 0.27755(16) 0.07530(15) 0.0150(6) Uani 1 1 d . . . C22 C 0.27905(18) 0.22494(15) 0.09637(15) 0.0140(5) Uani 1 1 d . . . H22A H 0.2980 0.1881 0.1379 0.017 Uiso 1 1 calc R . . H22B H 0.2858 0.1920 0.0505 0.017 Uiso 1 1 calc R . . C23 C 0.1198(2) 0.34982(18) 0.05552(16) 0.0231(6) Uani 1 1 d . . . H23A H 0.1361 0.3231 0.0051 0.035 Uiso 1 1 calc R . . H23B H 0.1518 0.3918 0.0528 0.035 Uiso 1 1 calc R . . H23C H 0.0522 0.3735 0.0695 0.035 Uiso 1 1 calc R . . C24 C 0.13429(19) 0.32515(16) 0.22163(15) 0.0171(6) Uani 1 1 d . . . H24A H 0.0679 0.3524 0.2379 0.026 Uiso 1 1 calc R . . H24B H 0.1708 0.3640 0.2175 0.026 Uiso 1 1 calc R . . H24C H 0.1528 0.2848 0.2599 0.026 Uiso 1 1 calc R . . C25 C 0.0884(2) 0.20477(17) 0.13944(17) 0.0219(6) Uani 1 1 d . . . H25A H 0.1073 0.1659 0.1787 0.033 Uiso 1 1 calc R . . H25B H 0.0997 0.1772 0.0900 0.033 Uiso 1 1 calc R . . H25C H 0.0219 0.2319 0.1555 0.033 Uiso 1 1 calc R . . C26 C 0.45706(19) 0.43434(16) -0.07418(15) 0.0145(6) Uani 1 1 d . . . C27 C 0.41245(19) 0.37568(16) -0.10421(14) 0.0143(5) Uani 1 1 d . . . H27A H 0.3444 0.4004 -0.0956 0.017 Uiso 1 1 calc R . . H27B H 0.4221 0.3271 -0.0722 0.017 Uiso 1 1 calc R . . C28 C 0.43608(19) 0.42844(16) -0.27204(15) 0.0178(6) Uani 1 1 d . . . H28A H 0.4695 0.4662 -0.2622 0.027 Uiso 1 1 calc R . . H28B H 0.3693 0.4552 -0.2638 0.027 Uiso 1 1 calc R . . H28C H 0.4593 0.4090 -0.3256 0.027 Uiso 1 1 calc R . . C29 C 0.57787(19) 0.29251(17) -0.22350(17) 0.0224(6) Uani 1 1 d . . . H29A H 0.5983 0.2703 -0.2761 0.034 Uiso 1 1 calc R . . H29B H 0.5878 0.2492 -0.1862 0.034 Uiso 1 1 calc R . . H29C H 0.6138 0.3296 -0.2175 0.034 Uiso 1 1 calc R . . C30 C 0.3883(2) 0.27707(17) -0.22056(16) 0.0217(6) Uani 1 1 d . . . H30A H 0.3223 0.3062 -0.2135 0.033 Uiso 1 1 calc R . . H30B H 0.3956 0.2340 -0.1828 0.033 Uiso 1 1 calc R . . H30C H 0.4110 0.2545 -0.2730 0.033 Uiso 1 1 calc R . . C31 C 0.0741(2) 0.67204(19) 0.32746(18) 0.0286(7) Uani 1 1 d . . . C32 C 0.0873(2) 0.7434(2) 0.59793(19) 0.0305(7) Uani 1 1 d . . . C33 C 0.5972(2) 0.2917(2) 0.45611(19) 0.0335(8) Uani 1 1 d . . . C34 C 0.3606(2) 0.13154(19) 0.57426(17) 0.0285(7) Uani 1 1 d . . . C35 C 0.2048(2) 0.15182(19) 0.87179(19) 0.0284(7) Uani 1 1 d . . . C36 C 0.0398(2) -0.04336(18) 0.79229(19) 0.0276(7) Uani 1 1 d . . . C37 C 0.9462(2) 0.5641(2) 0.17889(19) 0.0304(7) Uani 1 1 d . . . C38 C 0.7542(2) 0.35763(19) 0.2297(2) 0.0331(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01320(5) 0.01233(5) 0.01167(5) -0.00173(4) 0.00014(4) -0.00536(4) U2 0.01591(6) 0.01415(5) 0.01025(5) -0.00038(4) 0.00031(4) -0.00751(4) P1 0.0148(4) 0.0153(4) 0.0126(3) 0.0019(3) -0.0033(3) -0.0047(3) P2 0.0167(4) 0.0149(4) 0.0158(3) 0.0008(3) -0.0030(3) -0.0072(3) P3 0.0169(4) 0.0149(4) 0.0130(3) -0.0014(3) -0.0042(3) -0.0031(3) P4 0.0129(4) 0.0216(4) 0.0119(3) 0.0020(3) -0.0003(3) -0.0045(3) P5 0.0157(4) 0.0144(4) 0.0150(3) -0.0007(3) -0.0032(3) -0.0048(3) P6 0.0136(3) 0.0141(3) 0.0126(3) -0.0014(3) -0.0019(3) -0.0046(3) S1 0.0210(4) 0.0247(4) 0.0343(4) -0.0115(3) 0.0058(3) -0.0071(3) S2 0.0193(4) 0.0328(4) 0.0256(4) -0.0029(3) 0.0031(3) -0.0007(3) S3 0.0169(4) 0.0260(4) 0.0169(3) 0.0004(3) -0.0050(3) -0.0041(3) S4 0.0238(4) 0.0292(4) 0.0182(4) -0.0030(3) -0.0074(3) -0.0068(3) S5 0.0173(4) 0.0260(4) 0.0209(4) -0.0044(3) -0.0043(3) -0.0037(3) S6 0.0229(4) 0.0179(4) 0.0238(4) 0.0010(3) -0.0106(3) -0.0047(3) S7 0.0157(3) 0.0169(3) 0.0192(3) -0.0010(3) -0.0033(3) -0.0050(3) S8 0.0236(4) 0.0214(4) 0.0234(4) -0.0020(3) -0.0107(3) -0.0052(3) F1 0.0754(16) 0.0280(11) 0.0497(13) 0.0073(10) -0.0291(12) -0.0061(11) F2 0.0434(12) 0.0458(12) 0.0439(12) 0.0068(10) -0.0095(10) -0.0293(10) F3 0.0508(14) 0.0831(17) 0.0241(11) -0.0003(10) 0.0022(10) -0.0369(13) F4 0.0542(13) 0.0275(11) 0.0355(11) 0.0107(9) -0.0056(10) -0.0126(10) F5 0.0518(13) 0.0330(11) 0.0325(11) -0.0119(9) -0.0041(10) -0.0051(10) F6 0.0367(11) 0.0472(12) 0.0282(10) 0.0071(9) -0.0037(8) -0.0275(10) F7 0.0885(18) 0.0633(15) 0.0172(10) -0.0082(9) 0.0025(10) -0.0478(14) F8 0.0514(13) 0.0305(11) 0.0359(11) 0.0065(9) -0.0134(9) -0.0185(10) F9 0.0279(11) 0.0523(13) 0.0511(13) 0.0225(11) 0.0056(10) -0.0053(10) F10 0.0403(12) 0.0356(11) 0.0341(11) -0.0011(9) -0.0020(9) -0.0195(9) F11 0.0480(13) 0.0227(10) 0.0697(15) -0.0159(10) -0.0115(11) -0.0037(9) F12 0.0434(13) 0.0585(14) 0.0521(13) 0.0001(11) -0.0273(11) -0.0271(11) F13 0.0638(14) 0.0251(10) 0.0501(13) -0.0033(9) -0.0317(11) -0.0132(10) F14 0.0263(11) 0.0402(12) 0.0663(14) 0.0105(10) -0.0109(10) -0.0154(9) F15 0.0470(12) 0.0286(10) 0.0486(12) 0.0184(9) -0.0307(10) -0.0155(9) F16 0.0557(14) 0.0726(16) 0.0287(11) 0.0125(10) 0.0011(10) -0.0342(13) F17 0.0444(13) 0.0825(17) 0.0547(14) -0.0158(12) 0.0004(11) -0.0424(13) F18 0.0248(11) 0.0637(15) 0.0424(12) -0.0161(11) 0.0049(9) -0.0061(10) F19 0.0390(12) 0.0417(12) 0.0531(13) -0.0067(10) 0.0159(10) -0.0237(10) F20 0.0464(12) 0.0216(10) 0.0541(13) 0.0027(9) -0.0095(10) -0.0186(9) F21 0.0983(19) 0.0596(15) 0.0356(12) 0.0279(11) -0.0305(12) -0.0483(14) F22 0.0354(11) 0.0388(12) 0.0417(12) 0.0120(9) -0.0003(9) -0.0142(10) F23 0.0497(14) 0.0511(14) 0.0925(18) 0.0245(12) -0.0436(13) -0.0368(12) F24 0.0531(13) 0.0187(10) 0.0742(15) 0.0156(10) -0.0317(12) -0.0134(10) N1 0.0306(15) 0.0125(12) 0.0229(13) -0.0033(10) 0.0088(11) -0.0065(11) N2 0.0231(13) 0.0318(15) 0.0178(12) 0.0048(11) -0.0115(10) -0.0102(11) N3 0.0180(13) 0.0207(13) 0.0247(13) -0.0044(10) -0.0066(10) -0.0011(10) N4 0.0180(13) 0.0194(13) 0.0204(13) -0.0043(10) -0.0047(10) -0.0051(10) O1 0.0151(10) 0.0178(10) 0.0314(12) -0.0031(9) -0.0045(9) -0.0037(8) O2 0.0175(10) 0.0158(10) 0.0241(11) 0.0008(8) -0.0051(8) -0.0062(8) O3 0.0198(10) 0.0188(10) 0.0147(10) -0.0019(8) 0.0002(8) -0.0083(8) O4 0.0376(13) 0.0167(11) 0.0195(11) 0.0029(8) -0.0016(9) -0.0052(10) O5 0.0216(10) 0.0186(10) 0.0125(9) -0.0033(8) -0.0004(8) -0.0109(8) O6 0.0208(10) 0.0214(11) 0.0151(10) -0.0037(8) 0.0030(8) -0.0119(9) O7 0.0364(13) 0.0388(13) 0.0160(10) -0.0121(9) 0.0076(9) -0.0278(11) O8 0.0171(10) 0.0180(10) 0.0127(9) -0.0014(8) 0.0006(8) -0.0093(8) O9 0.0169(10) 0.0252(11) 0.0241(11) -0.0038(9) -0.0020(8) -0.0056(9) O10 0.0246(11) 0.0150(10) 0.0174(10) 0.0010(8) -0.0039(8) -0.0050(8) O11 0.0258(11) 0.0278(11) 0.0144(10) 0.0011(8) -0.0014(8) -0.0175(9) O12 0.0220(11) 0.0182(10) 0.0124(9) -0.0009(8) -0.0004(8) -0.0115(8) O13 0.0199(10) 0.0122(9) 0.0156(10) -0.0023(7) -0.0008(8) -0.0061(8) O14 0.0167(10) 0.0165(10) 0.0215(10) 0.0019(8) 0.0013(8) -0.0027(8) O15 0.0333(12) 0.0316(12) 0.0129(10) -0.0023(9) -0.0004(9) -0.0216(10) O16 0.0269(11) 0.0270(11) 0.0119(10) -0.0009(8) 0.0023(8) -0.0182(9) O17 0.0407(14) 0.0196(12) 0.0550(16) -0.0102(11) -0.0229(12) 0.0041(10) O18 0.0342(15) 0.077(2) 0.0482(16) -0.0297(14) 0.0244(12) -0.0330(14) O19 0.0353(14) 0.083(2) 0.0301(13) -0.0034(13) 0.0037(11) -0.0369(14) O20 0.0529(17) 0.0494(17) 0.0395(15) -0.0200(13) -0.0096(13) 0.0279(13) O21 0.0284(12) 0.0246(12) 0.0319(12) 0.0049(9) -0.0108(10) -0.0008(10) O22 0.0248(11) 0.0269(11) 0.0181(10) -0.0028(9) -0.0083(9) -0.0023(9) O23 0.0309(13) 0.0297(13) 0.0469(14) -0.0093(11) -0.0213(11) -0.0010(10) O24 0.0355(13) 0.0429(14) 0.0165(11) -0.0046(9) -0.0055(9) -0.0176(11) O25 0.0272(12) 0.0527(15) 0.0225(12) -0.0119(11) -0.0001(10) -0.0089(11) O26 0.0199(11) 0.0273(12) 0.0288(12) 0.0004(9) -0.0108(9) -0.0033(9) O27 0.0261(12) 0.0328(12) 0.0232(11) -0.0052(9) -0.0038(9) -0.0052(10) O28 0.0406(14) 0.0225(12) 0.0365(13) 0.0081(10) -0.0244(11) -0.0097(10) O30 0.0169(11) 0.0236(12) 0.0413(13) -0.0102(10) -0.0060(10) 0.0008(9) O31 0.0245(12) 0.0291(12) 0.0280(12) 0.0056(9) -0.0130(9) -0.0053(10) O32 0.0388(14) 0.0379(14) 0.0362(13) -0.0187(11) -0.0171(11) 0.0001(11) O29 0.0255(11) 0.0277(12) 0.0219(11) -0.0031(9) -0.0093(9) -0.0054(9) C10 0.0215(16) 0.0288(17) 0.0215(15) 0.0036(13) -0.0062(12) -0.0096(13) C1 0.0194(15) 0.0206(15) 0.0137(13) -0.0019(11) -0.0004(11) -0.0115(12) C2 0.0227(15) 0.0163(14) 0.0134(13) -0.0015(11) -0.0009(11) -0.0080(12) C3 0.0165(15) 0.0271(17) 0.0257(16) -0.0004(13) -0.0086(12) -0.0038(13) C4 0.0259(16) 0.0162(15) 0.0237(15) 0.0030(12) -0.0104(13) -0.0034(12) C5 0.0360(19) 0.0304(17) 0.0144(14) 0.0044(12) -0.0037(13) -0.0140(15) C6 0.0123(13) 0.0131(13) 0.0189(14) 0.0034(11) -0.0025(11) -0.0023(11) C7 0.0169(14) 0.0169(14) 0.0150(14) -0.0006(11) -0.0013(11) -0.0081(12) C8 0.0294(17) 0.0290(17) 0.0195(15) 0.0018(13) -0.0047(13) -0.0185(14) C9 0.0235(16) 0.0150(14) 0.0255(16) -0.0006(12) -0.0009(13) -0.0031(12) C11 0.0153(14) 0.0116(13) 0.0140(13) 0.0020(10) -0.0031(11) -0.0041(11) C12 0.0139(13) 0.0145(13) 0.0135(13) 0.0007(10) -0.0022(10) -0.0062(11) C13 0.0224(16) 0.0200(15) 0.0201(15) -0.0043(12) -0.0019(12) 0.0040(12) C14 0.0286(17) 0.0322(18) 0.0290(17) -0.0066(14) -0.0151(14) -0.0095(14) C15 0.0251(16) 0.0180(15) 0.0147(14) 0.0012(11) -0.0056(12) 0.0005(12) C16 0.0136(14) 0.0161(14) 0.0138(13) 0.0003(11) -0.0004(11) -0.0025(11) C17 0.0168(14) 0.0207(15) 0.0126(13) 0.0013(11) -0.0036(11) -0.0069(12) C18 0.0171(15) 0.0190(15) 0.0270(16) 0.0001(12) -0.0047(12) -0.0013(12) C19 0.0288(18) 0.052(2) 0.0128(15) 0.0025(14) 0.0002(13) -0.0176(16) C20 0.0161(15) 0.0207(15) 0.0249(15) 0.0065(12) -0.0035(12) -0.0054(12) C21 0.0185(15) 0.0157(14) 0.0122(13) 0.0053(11) -0.0060(11) -0.0058(12) C22 0.0185(14) 0.0098(13) 0.0131(13) -0.0023(10) -0.0018(11) -0.0036(11) C23 0.0231(16) 0.0268(16) 0.0183(15) 0.0012(12) -0.0077(12) -0.0022(13) C24 0.0175(14) 0.0172(14) 0.0170(14) -0.0016(11) -0.0021(11) -0.0060(12) C25 0.0200(15) 0.0210(15) 0.0264(16) -0.0035(12) -0.0026(12) -0.0094(13) C26 0.0206(15) 0.0139(13) 0.0110(13) 0.0017(10) -0.0046(11) -0.0072(11) C27 0.0168(14) 0.0147(13) 0.0121(13) 0.0001(10) -0.0016(11) -0.0066(11) C28 0.0180(15) 0.0200(15) 0.0161(14) 0.0014(11) -0.0039(11) -0.0063(12) C29 0.0167(15) 0.0200(15) 0.0275(16) -0.0034(12) -0.0031(12) -0.0005(12) C30 0.0245(16) 0.0250(16) 0.0204(15) -0.0005(12) -0.0070(12) -0.0124(13) C31 0.0335(19) 0.0221(17) 0.0262(17) 0.0025(13) 0.0031(14) -0.0088(14) C32 0.0304(18) 0.0340(19) 0.0294(18) 0.0032(14) -0.0027(14) -0.0157(16) C33 0.0318(19) 0.047(2) 0.0238(17) -0.0032(15) -0.0015(14) -0.0174(17) C34 0.040(2) 0.0284(18) 0.0179(16) 0.0056(13) -0.0069(14) -0.0110(15) C35 0.0264(17) 0.0240(17) 0.0359(19) -0.0072(14) -0.0080(14) -0.0065(14) C36 0.0338(19) 0.0184(16) 0.0354(18) 0.0037(13) -0.0197(15) -0.0059(14) C37 0.036(2) 0.0268(18) 0.0339(19) 0.0050(14) -0.0104(15) -0.0162(15) C38 0.0329(19) 0.0193(17) 0.057(2) 0.0119(16) -0.0257(17) -0.0124(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 1.7617(19) . ? U1 O1 1.7681(19) . ? U1 O7 2.3028(19) . ? U1 O3 2.3155(17) . ? U1 O8 2.3930(17) 2_675 ? U1 O5 2.4584(17) . ? U1 O6 2.4971(18) . ? U1 C6 2.845(3) . ? U2 O9 1.7664(19) . ? U2 O10 1.7683(19) . ? U2 O13 2.3167(17) . ? U2 O15 2.3215(18) . ? U2 O16 2.3987(18) 2_665 ? U2 O11 2.4663(18) . ? U2 O12 2.4732(17) . ? U2 C16 2.841(3) . ? P1 C4 1.773(3) . ? P1 C3 1.774(3) . ? P1 C5 1.785(3) . ? P1 C2 1.798(3) . ? P2 C10 1.777(3) . ? P2 C8 1.777(3) . ? P2 C9 1.782(3) . ? P2 C7 1.797(3) . ? P3 C13 1.776(3) . ? P3 C14 1.780(3) . ? P3 C15 1.783(3) . ? P3 C12 1.792(3) . ? P4 C20 1.777(3) . ? P4 C19 1.778(3) . ? P4 C18 1.778(3) . ? P4 C17 1.803(3) . ? P5 C24 1.774(3) . ? P5 C25 1.781(3) . ? P5 C23 1.785(3) . ? P5 C22 1.796(3) . ? P6 C29 1.776(3) . ? P6 C28 1.778(3) . ? P6 C30 1.786(3) . ? P6 C27 1.800(3) . ? S1 O17 1.426(2) . ? S1 O18 1.426(2) . ? S1 N1 1.573(2) . ? S1 C31 1.833(3) . ? S2 O19 1.417(2) . ? S2 O20 1.428(2) . ? S2 N1 1.575(2) . ? S2 C32 1.831(3) . ? S3 O21 1.424(2) . ? S3 O22 1.4295(19) . ? S3 N2 1.573(2) . ? S3 C33 1.822(3) . ? S4 O23 1.424(2) . ? S4 O24 1.432(2) . ? S4 N2 1.589(3) . ? S4 C34 1.836(3) . ? S5 O25 1.426(2) . ? S5 O26 1.432(2) . ? S5 N3 1.578(2) . ? S5 C35 1.832(3) . ? S6 O27 1.423(2) . ? S6 O28 1.425(2) . ? S6 N3 1.590(2) . ? S6 C36 1.831(3) . ? S7 O29 1.420(2) . ? S7 O30 1.423(2) . ? S7 N4 1.587(2) . ? S7 C37 1.829(3) . ? S8 O31 1.428(2) . ? S8 O32 1.428(2) . ? S8 N4 1.573(2) . ? S8 C38 1.837(3) . ? F1 C32 1.313(4) . ? F2 C32 1.320(3) . ? F3 C32 1.323(3) . ? F4 C31 1.322(3) . ? F5 C31 1.335(3) . ? F6 C31 1.319(3) . ? F7 C34 1.311(3) . ? F8 C34 1.324(3) . ? F9 C34 1.328(4) . ? F10 C35 1.324(3) . ? F11 C35 1.331(3) . ? F12 C35 1.335(3) . ? F13 C36 1.326(3) . ? F14 C36 1.321(4) . ? F15 C36 1.329(3) . ? F16 C33 1.327(4) . ? F17 C33 1.322(4) . ? F18 C33 1.334(4) . ? F19 C37 1.332(4) . ? F20 C37 1.331(3) . ? F21 C37 1.317(4) . ? F22 C38 1.317(4) . ? F23 C38 1.339(4) . ? F24 C38 1.328(3) . ? O3 C1 1.288(3) . ? O4 C1 1.216(3) . ? O5 C6 1.263(3) . ? O6 C6 1.262(3) . ? O7 C11 1.234(3) . ? O8 C11 1.260(3) . ? O8 U1 2.3930(17) 2_675 ? O11 C16 1.259(3) . ? O12 C16 1.269(3) . ? O13 C21 1.299(3) . ? O14 C21 1.217(3) . ? O15 C26 1.246(3) . ? O16 C26 1.252(3) . ? O16 U2 2.3987(18) 2_665 ? C1 C2 1.529(3) . ? C6 C7 1.503(3) . ? C11 C12 1.517(3) . ? C16 C17 1.505(3) . ? C21 C22 1.522(3) . ? C26 C27 1.516(3) . ? 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 179.19(8) . . ? O2 U1 O7 89.33(8) . . ? O1 U1 O7 90.55(9) . . ? O2 U1 O3 92.07(8) . . ? O1 U1 O3 88.33(8) . . ? O7 U1 O3 159.33(7) . . ? O2 U1 O8 90.54(7) . 2_675 ? O1 U1 O8 90.23(7) . 2_675 ? O7 U1 O8 81.31(6) . 2_675 ? O3 U1 O8 78.05(6) . 2_675 ? O2 U1 O5 89.06(7) . . ? O1 U1 O5 90.37(8) . . ? O7 U1 O5 127.12(6) . . ? O3 U1 O5 73.53(6) . . ? O8 U1 O5 151.55(6) 2_675 . ? O2 U1 O6 89.52(7) . . ? O1 U1 O6 89.67(7) . . ? O7 U1 O6 74.55(6) . . ? O3 U1 O6 126.07(6) . . ? O8 U1 O6 155.86(6) 2_675 . ? O5 U1 O6 52.59(6) . . ? O2 U1 C6 88.66(8) . . ? O1 U1 C6 90.57(8) . . ? O7 U1 C6 100.84(7) . . ? O3 U1 C6 99.81(7) . . ? O8 U1 C6 177.69(7) 2_675 . ? O5 U1 C6 26.29(6) . . ? O6 U1 C6 26.32(6) . . ? O9 U2 O10 178.89(8) . . ? O9 U2 O13 90.15(8) . . ? O10 U2 O13 90.54(7) . . ? O9 U2 O15 93.20(8) . . ? O10 U2 O15 87.74(8) . . ? O13 U2 O15 82.55(6) . . ? O9 U2 O16 90.42(8) . 2_665 ? O10 U2 O16 89.17(8) . 2_665 ? O13 U2 O16 162.75(6) . 2_665 ? O15 U2 O16 80.21(6) . 2_665 ? O9 U2 O11 89.65(8) . . ? O10 U2 O11 89.24(7) . . ? O13 U2 O11 126.29(6) . . ? O15 U2 O11 151.04(6) . . ? O16 U2 O11 70.96(6) 2_665 . ? O9 U2 O12 90.75(8) . . ? O10 U2 O12 88.62(7) . . ? O13 U2 O12 73.58(6) . . ? O15 U2 O12 155.81(6) . . ? O16 U2 O12 123.65(6) 2_665 . ? O11 U2 O12 52.72(6) . . ? O9 U2 C16 90.52(8) . . ? O10 U2 C16 88.51(8) . . ? O13 U2 C16 100.06(7) . . ? O15 U2 C16 175.46(7) . . ? O16 U2 C16 97.18(7) 2_665 . ? O11 U2 C16 26.24(7) . . ? O12 U2 C16 26.48(6) . . ? C4 P1 C3 108.16(14) . . ? C4 P1 C5 109.75(14) . . ? C3 P1 C5 110.58(14) . . ? C4 P1 C2 111.47(13) . . ? C3 P1 C2 110.60(14) . . ? C5 P1 C2 106.30(13) . . ? C10 P2 C8 109.48(14) . . ? C10 P2 C9 110.48(14) . . ? C8 P2 C9 109.14(14) . . ? C10 P2 C7 110.68(13) . . ? C8 P2 C7 105.92(13) . . ? C9 P2 C7 111.02(13) . . ? C13 P3 C14 108.62(14) . . ? C13 P3 C15 111.01(14) . . ? C14 P3 C15 108.30(14) . . ? C13 P3 C12 109.93(13) . . ? C14 P3 C12 106.54(13) . . ? C15 P3 C12 112.27(12) . . ? C20 P4 C19 109.70(15) . . ? C20 P4 C18 109.76(13) . . ? C19 P4 C18 108.62(14) . . ? C20 P4 C17 110.14(13) . . ? C19 P4 C17 106.71(13) . . ? C18 P4 C17 111.84(13) . . ? C24 P5 C25 107.88(13) . . ? C24 P5 C23 111.27(13) . . ? C25 P5 C23 109.30(14) . . ? C24 P5 C22 110.78(12) . . ? C25 P5 C22 108.26(12) . . ? C23 P5 C22 109.29(13) . . ? C29 P6 C28 110.09(13) . . ? C29 P6 C30 109.59(14) . . ? C28 P6 C30 109.84(13) . . ? C29 P6 C27 109.78(13) . . ? C28 P6 C27 112.69(13) . . ? C30 P6 C27 104.70(13) . . ? O17 S1 O18 119.51(17) . . ? O17 S1 N1 115.34(13) . . ? O18 S1 N1 107.58(14) . . ? O17 S1 C31 103.85(14) . . ? O18 S1 C31 102.69(15) . . ? N1 S1 C31 106.20(15) . . ? O19 S2 O20 119.61(17) . . ? O19 S2 N1 115.81(14) . . ? O20 S2 N1 107.01(15) . . ? O19 S2 C32 104.30(15) . . ? O20 S2 C32 102.76(15) . . ? N1 S2 C32 105.58(15) . . ? O21 S3 O22 118.41(12) . . ? O21 S3 N2 108.36(13) . . ? O22 S3 N2 116.41(13) . . ? O21 S3 C33 104.06(15) . . ? O22 S3 C33 104.99(14) . . ? N2 S3 C33 102.49(14) . . ? O23 S4 O24 119.01(14) . . ? O23 S4 N2 116.93(13) . . ? O24 S4 N2 107.46(13) . . ? O23 S4 C34 105.09(14) . . ? O24 S4 C34 103.44(13) . . ? N2 S4 C34 102.67(14) . . ? O25 S5 O26 118.99(14) . . ? O25 S5 N3 108.59(13) . . ? O26 S5 N3 116.55(12) . . ? O25 S5 C35 103.52(14) . . ? O26 S5 C35 104.09(13) . . ? N3 S5 C35 102.76(14) . . ? O27 S6 O28 119.24(13) . . ? O27 S6 N3 116.28(12) . . ? O28 S6 N3 108.06(13) . . ? O27 S6 C36 105.06(14) . . ? O28 S6 C36 103.47(13) . . ? N3 S6 C36 102.46(14) . . ? O29 S7 O30 119.18(13) . . ? O29 S7 N4 108.48(12) . . ? O30 S7 N4 116.60(12) . . ? O29 S7 C37 103.65(14) . . ? O30 S7 C37 104.42(14) . . ? N4 S7 C37 102.06(14) . . ? O31 S8 O32 118.53(13) . . ? O31 S8 N4 116.93(13) . . ? O32 S8 N4 108.05(13) . . ? O31 S8 C38 104.15(14) . . ? O32 S8 C38 103.95(16) . . ? N4 S8 C38 103.09(14) . . ? S1 N1 S2 123.65(15) . . ? S3 N2 S4 125.30(15) . . ? S5 N3 S6 123.36(15) . . ? S8 N4 S7 124.08(15) . . ? C1 O3 U1 136.12(17) . . ? C6 O5 U1 94.20(15) . . ? C6 O6 U1 92.41(15) . . ? C11 O7 U1 162.71(19) . . ? C11 O8 U1 137.23(16) . 2_675 ? C16 O11 U2 93.73(16) . . ? C16 O12 U2 93.16(15) . . ? C21 O13 U2 131.52(17) . . ? C26 O15 U2 155.21(19) . . ? C26 O16 U2 140.61(17) . 2_665 ? O4 C1 O3 126.1(2) . . ? O4 C1 C2 120.2(2) . . ? O3 C1 C2 113.6(2) . . ? C1 C2 P1 115.00(18) . . ? O6 C6 O5 120.8(2) . . ? O6 C6 C7 120.3(2) . . ? O5 C6 C7 118.9(2) . . ? O6 C6 U1 61.27(13) . . ? O5 C6 U1 59.52(13) . . ? C7 C6 U1 177.70(19) . . ? C6 C7 P2 114.80(18) . . ? O7 C11 O8 124.9(2) . . ? O7 C11 C12 117.5(2) . . ? O8 C11 C12 117.6(2) . . ? C11 C12 P3 114.42(18) . . ? O11 C16 O12 120.4(2) . . ? O11 C16 C17 119.2(2) . . ? O12 C16 C17 120.4(2) . . ? O11 C16 U2 60.02(13) . . ? O12 C16 U2 60.36(13) . . ? C17 C16 U2 178.93(18) . . ? C16 C17 P4 115.47(19) . . ? O14 C21 O13 125.8(2) . . ? O14 C21 C22 119.1(2) . . ? O13 C21 C22 115.1(2) . . ? C21 C22 P5 116.53(18) . . ? O15 C26 O16 124.9(2) . . ? O15 C26 C27 116.6(2) . . ? O16 C26 C27 118.5(2) . . ? C26 C27 P6 116.94(18) . . ? F6 C31 F4 108.3(3) . . ? F6 C31 F5 107.6(2) . . ? F4 C31 F5 108.0(2) . . ? F6 C31 S1 112.2(2) . . ? F4 C31 S1 112.2(2) . . ? F5 C31 S1 108.2(2) . . ? F1 C32 F2 108.2(3) . . ? F1 C32 F3 108.3(3) . . ? F2 C32 F3 107.8(3) . . ? F1 C32 S2 112.1(2) . . ? F2 C32 S2 111.0(2) . . ? F3 C32 S2 109.4(2) . . ? F17 C33 F16 108.7(3) . . ? F17 C33 F18 108.4(3) . . ? F16 C33 F18 107.6(3) . . ? F17 C33 S3 110.0(2) . . ? F16 C33 S3 110.8(2) . . ? F18 C33 S3 111.3(2) . . ? F7 C34 F8 108.7(2) . . ? F7 C34 F9 109.1(3) . . ? F8 C34 F9 107.4(3) . . ? F7 C34 S4 111.2(2) . . ? F8 C34 S4 109.5(2) . . ? F9 C34 S4 110.9(2) . . ? F10 C35 F11 107.9(3) . . ? F10 C35 F12 107.9(3) . . ? F11 C35 F12 107.6(2) . . ? F10 C35 S5 112.2(2) . . ? F11 C35 S5 111.3(2) . . ? F12 C35 S5 109.8(2) . . ? F14 C36 F13 108.5(3) . . ? F14 C36 F15 108.3(3) . . ? F13 C36 F15 107.9(2) . . ? F14 C36 S6 111.0(2) . . ? F13 C36 S6 109.6(2) . . ? F15 C36 S6 111.4(2) . . ? F21 C37 F20 108.6(3) . . ? F21 C37 F19 108.6(3) . . ? F20 C37 F19 108.2(3) . . ? F21 C37 S7 111.4(2) . . ? F20 C37 S7 109.2(2) . . ? F19 C37 S7 110.8(2) . . ? F22 C38 F24 108.8(3) . . ? F22 C38 F23 108.5(3) . . ? F24 C38 F23 108.1(2) . . ? F22 C38 S8 111.9(2) . . ? F24 C38 S8 110.9(2) . . ? F23 C38 S8 108.4(2) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.968 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.096