# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1518 data_shelxl #------------------------------------------------------------------------------ _audit_creation_date '1999-09-22' _audit_creation_method SHELXL-97 _audit_update_record ; ? ; #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author ; Paul H Walton Department of Chemistry University of York Heslington York UK YO10 5DD ; _publ_contact_author_email phw2@york.ac.uk _publ_contact_author_fax '+44 (1904) 43 25 16' _publ_contact_author_phone '+44 (1904) 42 25 80' # TITLE AND AUTHOR LIST _publ_section_title ; A Selective Uranium Extraction Agent Prepared by Polymer Imprinting ; loop_ _publ_author_name _publ_author_address 'Gregory D Saunders' ; Department of Chemistry University of York Heslington YORK UK YO10 5DD ; 'Simon P Foxon' ; Department of Chemistry University of York Heslington YORK UK YO10 5DD ; 'Paul H Walton' ; Department of Chemistry University of York Heslington YORK UK YO10 5DD ; 'Malcolm J Joyce' ; BNFL Research and Technology Salwick PRESTON Lancashire UK PR4 0XJ ; 'Simon N Port' ; BNFL Research and Technology Salwick PRESTON Lancashire UK PR4 0XJ ; _publ_requested_journal 'Chem. Commun.' _publ_section_references ; Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garc\'ia-Granda, S., Gould, R.O., Smits, J.M.M. & Smykalla, C. (1992) The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Johnson, C.K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany, 1997. ; #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H34 Cl2 O8 P2 U' _chemical_formula_weight 1037.56 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' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.927(3) _cell_length_b 8.8708(12) _cell_length_c 15.795(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.735(15) _cell_angle_gamma 90.00 _cell_volume 2072.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 4.5 _cell_measurement_theta_max 5.6 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 4.173 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.633 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; The scan width was (1.31+0.34tan\q)\% with an \w scan speed of 8\% per minute (up to 4 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.25 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 2 1 0 1 -3 3 1 -2 _diffrn_reflns_number 8443 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3920 _reflns_number_gt 3038 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.06086 _diffrn_orient_matrix_UB_12 0.01652 _diffrn_orient_matrix_UB_13 -0.01822 _diffrn_orient_matrix_UB_21 -0.02453 _diffrn_orient_matrix_UB_22 -0.03010 _diffrn_orient_matrix_UB_23 -0.05962 _diffrn_orient_matrix_UB_31 -0.01627 _diffrn_orient_matrix_UB_32 0.10737 _diffrn_orient_matrix_UB_33 -0.01399 _computing_data_collection 'MSC/AFC (Diffractometer Control)' _computing_cell_refinement 'MSC/AFC (Diffractometer Control)' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; DIRDIF94 (Beurskens, P.T.,et al, 1992) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL-97 _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^)+(0.0421P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.011(11) _refine_ls_number_reflns 3914 _refine_ls_number_parameters 505 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.23959(2) 0.50685(5) 0.23379(2) 0.01976(11) Uani 1 1 d . . . Cl1 Cl -0.098(2) 0.556(2) 0.300(2) 0.102(12) Uani 0.50 1 d P A 1 Cl2 Cl -0.0927(17) 0.642(3) 0.3068(18) 0.086(7) Uani 0.50 1 d P A 2 Cl3 Cl 0.6404(2) 0.3845(7) 0.2824(3) 0.0743(16) Uani 1 1 d . . . P1 P 0.2676(2) 0.3479(4) 0.4624(2) 0.0260(7) Uani 1 1 d . . . P2 P 0.2479(2) 0.6290(4) 0.00528(19) 0.0216(7) Uani 1 1 d . . . O1 O 0.1900(5) 0.3323(9) 0.1988(5) 0.0257(19) Uani 1 1 d . . . O2 O 0.2872(5) 0.6835(11) 0.2684(5) 0.032(2) Uani 1 1 d . . . O3 O 0.2625(5) 0.4214(10) 0.3767(5) 0.030(2) Uani 1 1 d . . . O4 O 0.2596(5) 0.5593(9) 0.0936(5) 0.022(2) Uani 1 1 d . . . O5 O 0.0998(6) 0.6372(11) 0.1663(5) 0.037(2) Uani 1 1 d . . . O6 O 0.0970(5) 0.5534(10) 0.2963(5) 0.034(3) Uani 1 1 d . . . O7 O 0.3788(5) 0.3933(10) 0.2335(5) 0.032(2) Uani 1 1 d . . . O8 O 0.4843(7) 0.5465(12) 0.1928(7) 0.046(3) Uani 1 1 d . . . C1 C 0.2277(9) 0.1561(16) 0.4504(9) 0.026(3) Uani 1 1 d . . . C2 C 0.2070(16) 0.096(2) 0.3698(16) 0.042(6) Uani 1 1 d . . . H2 H 0.2097 0.1563 0.3219 0.050 Uiso 1 1 calc R . . C3 C 0.1827(18) -0.050(3) 0.3606(19) 0.056(8) Uani 1 1 d . . . H3 H 0.1722 -0.0891 0.3056 0.068 Uiso 1 1 calc R . . C4 C 0.1722(10) -0.1456(18) 0.4286(11) 0.042(4) Uani 1 1 d . . . H4 H 0.1520 -0.2444 0.4206 0.050 Uiso 1 1 calc R . . C5 C 0.1942(13) -0.082(2) 0.5094(14) 0.049(6) Uani 1 1 d . . . H5 H 0.1909 -0.1421 0.5572 0.059 Uiso 1 1 calc R . . C6 C 0.2201(12) 0.063(2) 0.5213(12) 0.047(6) Uani 1 1 d . . . H6 H 0.2329 0.1018 0.5763 0.056 Uiso 1 1 calc R . . C7 C 0.1986(8) 0.4422(15) 0.5294(7) 0.023(3) Uani 1 1 d . . . C8 C 0.1051(10) 0.448(2) 0.5009(10) 0.057(5) Uani 1 1 d . . . H8 H 0.0835 0.4057 0.4482 0.068 Uiso 1 1 calc R . . C9 C 0.0454(8) 0.512(5) 0.5474(8) 0.063(4) Uani 1 1 d . . . H9 H -0.0165 0.5040 0.5300 0.076 Uiso 1 1 calc R . . C10 C 0.0795(9) 0.5937(18) 0.6250(9) 0.044(4) Uani 1 1 d . . . H10 H 0.0405 0.6486 0.6545 0.053 Uiso 1 1 calc R . . C11 C 0.1717(9) 0.5880(17) 0.6543(9) 0.041(4) Uani 1 1 d . . . H11 H 0.1943 0.6311 0.7065 0.049 Uiso 1 1 calc R . . C12 C 0.2293(8) 0.518(3) 0.6052(7) 0.040(3) Uani 1 1 d . . . H12 H 0.2912 0.5210 0.6235 0.047 Uiso 1 1 calc R . . C13 C 0.3839(8) 0.3498(14) 0.5157(7) 0.022(3) Uani 1 1 d . . . C14 C 0.4107(8) 0.2775(16) 0.5915(7) 0.031(3) Uani 1 1 d . . . H14 H 0.3684 0.2285 0.6199 0.038 Uiso 1 1 calc R . . C15 C 0.5029(8) 0.2778(16) 0.6261(8) 0.031(3) Uani 1 1 d . . . H15 H 0.5214 0.2304 0.6780 0.037 Uiso 1 1 calc R . . C16 C 0.5650(9) 0.348(2) 0.5832(9) 0.048(4) Uani 1 1 d . . . H16 H 0.6260 0.3445 0.6051 0.057 Uiso 1 1 calc R . . C17 C 0.5375(10) 0.423(2) 0.5077(11) 0.067(6) Uani 1 1 d . . . H17 H 0.5797 0.4737 0.4798 0.081 Uiso 1 1 calc R . . C18 C 0.4473(9) 0.424(2) 0.4736(10) 0.054(5) Uani 1 1 d . . . H18 H 0.4289 0.4732 0.4223 0.065 Uiso 1 1 calc R . . C19 C 0.2810(7) 0.8215(15) 0.0098(7) 0.021(3) Uani 1 1 d . . . C20 C 0.2680(12) 0.911(2) 0.0799(14) 0.039(5) Uani 1 1 d . . . H20 H 0.2435 0.8686 0.1254 0.047 Uiso 1 1 calc R . . C21 C 0.2918(13) 1.065(2) 0.0823(16) 0.050(6) Uani 1 1 d . . . H21 H 0.2832 1.1237 0.1293 0.060 Uiso 1 1 calc R . . C22 C 0.3276(10) 1.126(2) 0.0150(13) 0.055(5) Uani 1 1 d . . . H22 H 0.3432 1.2279 0.0165 0.065 Uiso 1 1 calc R . . C23 C 0.3412(10) 1.040(3) -0.0558(11) 0.053(6) Uani 1 1 d . . . H23 H 0.3658 1.0821 -0.1015 0.063 Uiso 1 1 calc R . . C24 C 0.3174(9) 0.893(2) -0.0557(11) 0.042(4) Uani 1 1 d . . . H24 H 0.3260 0.8358 -0.1032 0.051 Uiso 1 1 calc R . . C25 C 0.3150(7) 0.533(2) -0.0623(7) 0.024(4) Uani 1 1 d . . . C26 C 0.4088(7) 0.509(3) -0.0368(8) 0.039(3) Uani 1 1 d . . . H26 H 0.4343 0.5467 0.0160 0.047 Uiso 1 1 calc R . . C27 C 0.4636(10) 0.4344(19) -0.0849(10) 0.045(4) Uani 1 1 d . . . H27 H 0.5257 0.4293 -0.0684 0.054 Uiso 1 1 calc R . . C28 C 0.4233(10) 0.3667(16) -0.1591(8) 0.041(4) Uani 1 1 d . . . H28 H 0.4587 0.3094 -0.1911 0.050 Uiso 1 1 calc R . . C29 C 0.3310(10) 0.3817(18) -0.1876(9) 0.044(4) Uani 1 1 d . . . H29 H 0.3058 0.3376 -0.2387 0.053 Uiso 1 1 calc R . . C30 C 0.2773(9) 0.4635(14) -0.1386(7) 0.033(4) Uani 1 1 d . . . H30 H 0.2156 0.4723 -0.1567 0.040 Uiso 1 1 calc R . . C31 C 0.1316(7) 0.6163(13) -0.0440(7) 0.020(2) Uani 1 1 d . . . C32 C 0.0983(7) 0.7189(15) -0.1079(8) 0.028(3) Uani 1 1 d . . . H32 H 0.1352 0.7953 -0.1241 0.033 Uiso 1 1 calc R . . C33 C 0.0095(8) 0.7054(16) -0.1469(9) 0.036(3) Uani 1 1 d . . . H33 H -0.0146 0.7763 -0.1870 0.044 Uiso 1 1 calc R . . C34 C -0.0433(8) 0.5853(16) -0.1257(8) 0.034(3) Uani 1 1 d . . . H34 H -0.1017 0.5713 -0.1535 0.041 Uiso 1 1 calc R . . C35 C -0.0076(9) 0.490(4) -0.0639(9) 0.053(7) Uani 1 1 d . . . H35 H -0.0447 0.4129 -0.0485 0.064 Uiso 1 1 calc R . . C36 C 0.0793(8) 0.496(3) -0.0216(7) 0.031(4) Uani 1 1 d . . . H36 H 0.1016 0.4255 0.0192 0.037 Uiso 1 1 calc R . . C37 C 0.0574(8) 0.6064(16) 0.2262(8) 0.033(3) Uani 1 1 d . A . C38 C -0.0433(9) 0.6268(18) 0.2142(10) 0.046(4) Uani 1 1 d . . . C39 C -0.0912(10) 0.6505(18) 0.1387(11) 0.053(4) Uani 1 1 d . A . H39A H -0.0625 0.6552 0.0900 0.064 Uiso 1 1 calc R . . H39B H -0.1535 0.6625 0.1343 0.064 Uiso 1 1 calc R . . C40 C 0.4613(10) 0.434(2) 0.2280(9) 0.033(4) Uani 1 1 d . . . C41 C 0.5274(10) 0.322(2) 0.2699(10) 0.045(4) Uani 1 1 d . . . C42 C 0.5098(14) 0.192(3) 0.2928(15) 0.104(9) Uani 1 1 d . . . H42A H 0.4506 0.1570 0.2842 0.124 Uiso 1 1 calc R . . H42B H 0.5559 0.1303 0.3186 0.124 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 0.01822(17) 0.02266(18) 0.01774(17) 0.0009(5) -0.00005(11) 0.0009(5) Cl1 0.059(7) 0.16(3) 0.099(12) 0.05(2) 0.051(8) 0.038(18) Cl2 0.042(6) 0.150(19) 0.069(8) 0.006(14) 0.027(5) 0.047(13) Cl3 0.0249(18) 0.139(5) 0.057(3) -0.024(3) -0.0016(18) 0.012(3) P1 0.0249(16) 0.0324(19) 0.0194(16) 0.0033(14) -0.0018(13) -0.0035(15) P2 0.0200(15) 0.0220(16) 0.0230(16) 0.0059(13) 0.0033(13) -0.0001(13) O1 0.030(5) 0.023(5) 0.024(4) -0.003(4) 0.003(4) -0.005(4) O2 0.033(5) 0.033(5) 0.030(5) -0.003(4) 0.007(4) 0.000(4) O3 0.028(5) 0.041(5) 0.020(5) 0.005(4) -0.004(4) -0.003(4) O4 0.018(4) 0.026(5) 0.023(4) 0.006(3) 0.001(3) 0.000(3) O5 0.032(5) 0.046(6) 0.033(5) 0.004(5) 0.008(4) 0.013(5) O6 0.033(4) 0.047(8) 0.021(4) -0.004(4) 0.003(3) 0.011(4) O7 0.016(4) 0.034(5) 0.043(5) 0.016(4) -0.003(4) 0.003(4) O8 0.042(6) 0.037(10) 0.061(7) 0.003(6) 0.015(5) -0.010(5) C1 0.017(6) 0.029(8) 0.035(8) -0.005(6) 0.012(6) -0.010(6) C2 0.071(14) 0.012(10) 0.046(12) -0.010(7) 0.023(10) -0.004(9) C3 0.076(17) 0.046(14) 0.049(14) -0.018(10) 0.015(12) 0.017(10) C4 0.019(7) 0.034(9) 0.073(12) -0.003(9) 0.007(8) 0.005(7) C5 0.049(12) 0.030(12) 0.065(15) 0.028(11) -0.005(11) -0.012(9) C6 0.049(10) 0.058(16) 0.030(8) 0.019(9) -0.003(7) -0.006(9) C7 0.017(6) 0.035(7) 0.017(6) 0.002(5) -0.001(5) -0.003(5) C8 0.039(8) 0.091(15) 0.042(9) -0.023(8) 0.011(7) -0.027(8) C9 0.028(6) 0.121(14) 0.041(7) -0.01(3) 0.008(6) -0.01(2) C10 0.045(8) 0.049(10) 0.040(8) 0.001(7) 0.012(7) -0.003(8) C11 0.046(8) 0.045(9) 0.035(8) -0.007(7) 0.012(7) -0.001(7) C12 0.034(6) 0.032(7) 0.050(7) 0.010(16) -0.006(6) -0.019(13) C13 0.030(6) 0.021(6) 0.014(6) 0.003(5) -0.002(5) 0.006(5) C14 0.024(6) 0.049(9) 0.023(7) 0.007(6) 0.009(5) 0.000(6) C15 0.018(6) 0.050(9) 0.021(6) -0.002(6) -0.012(5) 0.013(6) C16 0.018(7) 0.078(12) 0.045(9) 0.014(9) -0.007(6) 0.003(7) C17 0.036(9) 0.114(16) 0.051(10) 0.025(10) 0.003(8) -0.020(10) C18 0.026(8) 0.084(12) 0.046(9) 0.033(9) -0.019(7) -0.019(8) C19 0.010(6) 0.028(7) 0.026(7) 0.001(6) 0.001(5) 0.010(6) C20 0.023(9) 0.044(14) 0.053(11) -0.013(10) 0.016(8) -0.002(8) C21 0.033(10) 0.031(12) 0.086(14) -0.013(10) 0.011(10) 0.003(8) C22 0.031(9) 0.024(9) 0.105(16) 0.016(11) -0.004(10) -0.003(8) C23 0.034(7) 0.05(2) 0.075(11) 0.027(12) 0.011(7) 0.001(9) C24 0.025(8) 0.051(11) 0.047(10) 0.025(9) -0.008(7) -0.007(8) C25 0.026(5) 0.018(12) 0.031(6) 0.009(7) 0.014(5) 0.005(7) C26 0.030(6) 0.050(8) 0.039(7) 0.034(14) 0.010(5) 0.006(15) C27 0.029(7) 0.057(10) 0.051(10) 0.005(8) 0.017(7) 0.006(7) C28 0.073(11) 0.030(8) 0.027(7) 0.009(6) 0.028(7) 0.026(8) C29 0.052(9) 0.051(10) 0.028(8) 0.005(7) 0.003(7) 0.025(8) C30 0.034(7) 0.054(12) 0.011(6) 0.004(5) 0.002(5) 0.010(6) C31 0.027(6) 0.017(6) 0.015(6) 0.004(5) 0.003(5) 0.001(5) C32 0.019(6) 0.029(7) 0.034(7) -0.002(6) 0.000(5) 0.003(5) C33 0.025(7) 0.042(9) 0.038(8) 0.013(7) -0.011(6) 0.010(6) C34 0.013(6) 0.042(8) 0.043(8) -0.006(7) -0.010(5) -0.002(6) C35 0.029(6) 0.09(2) 0.041(7) 0.005(11) 0.010(6) -0.028(12) C36 0.035(6) 0.035(11) 0.020(5) -0.006(9) -0.003(4) -0.001(9) C37 0.030(7) 0.035(8) 0.034(7) -0.013(6) 0.006(6) 0.011(6) C38 0.040(8) 0.042(9) 0.059(10) 0.000(8) 0.015(7) 0.013(7) C39 0.035(8) 0.041(10) 0.081(12) 0.011(9) -0.003(8) -0.004(7) C40 0.030(8) 0.039(10) 0.030(9) -0.003(7) 0.008(7) 0.016(8) C41 0.033(8) 0.050(10) 0.048(9) -0.016(8) -0.007(7) 0.020(8) C42 0.062(13) 0.10(2) 0.14(2) 0.024(18) -0.008(14) 0.050(14) _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 1.772(8) . ? U1 O2 1.776(9) . ? U1 O7 2.309(8) . ? U1 O4 2.320(7) . ? U1 O3 2.361(8) . ? U1 O5 2.496(8) . ? U1 O6 2.499(8) . ? Cl1 C38 1.78(3) . ? Cl2 C38 1.73(3) . ? Cl3 C41 1.761(16) . ? P1 O3 1.495(8) . ? P1 C7 1.782(13) . ? P1 C1 1.805(13) . ? P1 C13 1.824(11) . ? P2 O4 1.515(8) . ? P2 C19 1.776(14) . ? P2 C25 1.777(14) . ? P2 C31 1.808(11) . ? O5 C37 1.238(15) . ? O6 C37 1.273(14) . ? O7 C40 1.299(17) . ? O8 C40 1.213(18) . ? C1 C2 1.38(3) . ? C1 C6 1.41(2) . ? C2 C3 1.35(2) . ? C3 C4 1.39(3) . ? C4 C5 1.39(3) . ? C5 C6 1.35(2) . ? C7 C12 1.40(2) . ? C7 C8 1.409(18) . ? C8 C9 1.35(3) . ? C9 C10 1.46(3) . ? C10 C11 1.392(18) . ? C11 C12 1.38(2) . ? C13 C14 1.369(16) . ? C13 C18 1.392(18) . ? C14 C15 1.410(15) . ? C15 C16 1.368(19) . ? C16 C17 1.38(2) . ? C17 C18 1.381(17) . ? C19 C24 1.39(2) . ? C19 C20 1.40(2) . ? C20 C21 1.41(3) . ? C21 C22 1.37(3) . ? C22 C23 1.39(3) . ? C23 C24 1.35(3) . ? C25 C30 1.402(18) . ? C25 C26 1.419(15) . ? C26 C27 1.36(2) . ? C27 C28 1.38(2) . ? C28 C29 1.397(19) . ? C29 C30 1.391(18) . ? C31 C36 1.39(2) . ? C31 C32 1.399(16) . ? C32 C33 1.390(15) . ? C33 C34 1.392(18) . ? C34 C35 1.35(2) . ? C35 C36 1.379(16) . ? C37 C38 1.500(18) . ? C38 C39 1.322(19) . ? C40 C41 1.49(2) . ? C41 C42 1.25(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 O1 U1 O2 178.9(4) . . ? O1 U1 O7 87.5(3) . . ? O2 U1 O7 93.6(4) . . ? O1 U1 O4 88.8(3) . . ? O2 U1 O4 91.1(3) . . ? O7 U1 O4 81.6(3) . . ? O1 U1 O3 91.0(3) . . ? O2 U1 O3 89.3(3) . . ? O7 U1 O3 81.2(3) . . ? O4 U1 O3 162.8(3) . . ? O1 U1 O5 89.0(4) . . ? O2 U1 O5 90.0(4) . . ? O7 U1 O5 154.4(3) . . ? O4 U1 O5 73.0(3) . . ? O3 U1 O5 124.2(3) . . ? O1 U1 O6 85.7(3) . . ? O2 U1 O6 93.4(3) . . ? O7 U1 O6 152.6(3) . . ? O4 U1 O6 124.7(2) . . ? O3 U1 O6 72.4(3) . . ? O5 U1 O6 52.0(3) . . ? O3 P1 C7 111.7(6) . . ? O3 P1 C1 109.9(6) . . ? C7 P1 C1 107.2(6) . . ? O3 P1 C13 110.1(5) . . ? C7 P1 C13 108.1(5) . . ? C1 P1 C13 109.7(6) . . ? O4 P2 C19 111.0(5) . . ? O4 P2 C25 110.7(6) . . ? C19 P2 C25 108.1(7) . . ? O4 P2 C31 110.8(5) . . ? C19 P2 C31 108.8(5) . . ? C25 P2 C31 107.3(5) . . ? P1 O3 U1 171.3(6) . . ? P2 O4 U1 161.3(5) . . ? C37 O5 U1 93.2(7) . . ? C37 O6 U1 92.2(7) . . ? C40 O7 U1 137.8(10) . . ? C2 C1 C6 118.6(16) . . ? C2 C1 P1 119.4(13) . . ? C6 C1 P1 122.0(13) . . ? C3 C2 C1 120(3) . . ? C2 C3 C4 124(3) . . ? C5 C4 C3 114.9(19) . . ? C6 C5 C4 123(2) . . ? C5 C6 C1 120(2) . . ? C12 C7 C8 117.0(13) . . ? C12 C7 P1 125.9(10) . . ? C8 C7 P1 117.0(10) . . ? C9 C8 C7 122.6(13) . . ? C8 C9 C10 119.0(12) . . ? C11 C10 C9 118.7(14) . . ? C12 C11 C10 119.5(13) . . ? C11 C12 C7 122.7(11) . . ? C14 C13 C18 120.0(11) . . ? C14 C13 P1 123.2(10) . . ? C18 C13 P1 116.7(9) . . ? C13 C14 C15 119.6(12) . . ? C16 C15 C14 120.0(12) . . ? C15 C16 C17 120.4(12) . . ? C18 C17 C16 119.9(15) . . ? C17 C18 C13 120.2(13) . . ? C24 C19 C20 116.1(16) . . ? C24 C19 P2 123.1(12) . . ? C20 C19 P2 120.8(12) . . ? C19 C20 C21 121(2) . . ? C22 C21 C20 119(2) . . ? C21 C22 C23 121.4(18) . . ? C24 C23 C22 117.5(17) . . ? C23 C24 C19 125.0(19) . . ? C30 C25 C26 116.5(15) . . ? C30 C25 P2 122.2(9) . . ? C26 C25 P2 120.9(12) . . ? C27 C26 C25 123.8(16) . . ? C26 C27 C28 117.4(14) . . ? C27 C28 C29 122.0(13) . . ? C30 C29 C28 119.3(13) . . ? C29 C30 C25 120.7(12) . . ? C36 C31 C32 121.6(11) . . ? C36 C31 P2 118.5(9) . . ? C32 C31 P2 119.8(9) . . ? C33 C32 C31 119.2(12) . . ? C32 C33 C34 119.7(12) . . ? C35 C34 C33 118.4(12) . . ? C34 C35 C36 125(2) . . ? C35 C36 C31 116(2) . . ? O5 C37 O6 121.4(11) . . ? O5 C37 C38 118.9(12) . . ? O6 C37 C38 119.6(12) . . ? C39 C38 C37 123.0(14) . . ? C39 C38 Cl2 120.6(14) . . ? C37 C38 Cl2 115.9(13) . . ? C39 C38 Cl1 119.5(16) . . ? C37 C38 Cl1 114.4(14) . . ? Cl2 C38 Cl1 25.5(10) . . ? O8 C40 O7 126.1(15) . . ? O8 C40 C41 122.7(15) . . ? O7 C40 C41 111.2(14) . . ? C42 C41 C40 126.4(17) . . ? C42 C41 Cl3 119.6(14) . . ? C40 C41 Cl3 114.0(13) . . ? 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 C7 P1 O3 U1 -102(4) . . . . ? C1 P1 O3 U1 17(4) . . . . ? C13 P1 O3 U1 138(4) . . . . ? O1 U1 O3 P1 -13(4) . . . . ? O2 U1 O3 P1 166(4) . . . . ? O7 U1 O3 P1 -100(4) . . . . ? O4 U1 O3 P1 -102(4) . . . . ? O5 U1 O3 P1 77(4) . . . . ? O6 U1 O3 P1 72(4) . . . . ? C19 P2 O4 U1 67.5(15) . . . . ? C25 P2 O4 U1 -172.4(14) . . . . ? C31 P2 O4 U1 -53.5(16) . . . . ? O1 U1 O4 P2 107.6(15) . . . . ? O2 U1 O4 P2 -71.3(15) . . . . ? O7 U1 O4 P2 -164.8(15) . . . . ? O3 U1 O4 P2 -162.6(12) . . . . ? O5 U1 O4 P2 18.4(14) . . . . ? O6 U1 O4 P2 23.6(16) . . . . ? O1 U1 O5 C37 79.1(8) . . . . ? O2 U1 O5 C37 -100.6(8) . . . . ? O7 U1 O5 C37 161.1(8) . . . . ? O4 U1 O5 C37 168.2(9) . . . . ? O3 U1 O5 C37 -11.5(9) . . . . ? O6 U1 O5 C37 -6.3(7) . . . . ? O1 U1 O6 C37 -85.9(8) . . . . ? O2 U1 O6 C37 93.4(8) . . . . ? O7 U1 O6 C37 -162.0(8) . . . . ? O4 U1 O6 C37 -0.3(9) . . . . ? O3 U1 O6 C37 -178.3(8) . . . . ? O5 U1 O6 C37 6.1(7) . . . . ? O1 U1 O7 C40 156.5(13) . . . . ? O2 U1 O7 C40 -23.3(13) . . . . ? O4 U1 O7 C40 67.3(13) . . . . ? O3 U1 O7 C40 -112.0(13) . . . . ? O5 U1 O7 C40 74.2(15) . . . . ? O6 U1 O7 C40 -127.7(12) . . . . ? O3 P1 C1 C2 6.1(16) . . . . ? C7 P1 C1 C2 127.7(15) . . . . ? C13 P1 C1 C2 -115.1(15) . . . . ? O3 P1 C1 C6 -176.2(12) . . . . ? C7 P1 C1 C6 -54.5(14) . . . . ? C13 P1 C1 C6 62.7(14) . . . . ? C6 C1 C2 C3 -2(3) . . . . ? P1 C1 C2 C3 176(2) . . . . ? C1 C2 C3 C4 4(4) . . . . ? C2 C3 C4 C5 -4(4) . . . . ? C3 C4 C5 C6 3(3) . . . . ? C4 C5 C6 C1 -1(3) . . . . ? C2 C1 C6 C5 1(3) . . . . ? P1 C1 C6 C5 -176.7(16) . . . . ? O3 P1 C7 C12 -115.3(16) . . . . ? C1 P1 C7 C12 124.2(16) . . . . ? C13 P1 C7 C12 6.0(17) . . . . ? O3 P1 C7 C8 61.1(13) . . . . ? C1 P1 C7 C8 -59.4(13) . . . . ? C13 P1 C7 C8 -177.6(11) . . . . ? C12 C7 C8 C9 -5(3) . . . . ? P1 C7 C8 C9 178(2) . . . . ? C7 C8 C9 C10 7(4) . . . . ? C8 C9 C10 C11 -8(4) . . . . ? C9 C10 C11 C12 6(3) . . . . ? C10 C11 C12 C7 -5(3) . . . . ? C8 C7 C12 C11 4(3) . . . . ? P1 C7 C12 C11 -179.7(14) . . . . ? O3 P1 C13 C14 -173.4(11) . . . . ? C7 P1 C13 C14 64.3(12) . . . . ? C1 P1 C13 C14 -52.4(13) . . . . ? O3 P1 C13 C18 3.6(13) . . . . ? C7 P1 C13 C18 -118.8(12) . . . . ? C1 P1 C13 C18 124.6(12) . . . . ? C18 C13 C14 C15 0(2) . . . . ? P1 C13 C14 C15 176.6(10) . . . . ? C13 C14 C15 C16 -1(2) . . . . ? C14 C15 C16 C17 2(3) . . . . ? C15 C16 C17 C18 -2(3) . . . . ? C16 C17 C18 C13 1(3) . . . . ? C14 C13 C18 C17 0(2) . . . . ? P1 C13 C18 C17 -176.6(14) . . . . ? O4 P2 C19 C24 149.1(10) . . . . ? C25 P2 C19 C24 27.5(12) . . . . ? C31 P2 C19 C24 -88.7(11) . . . . ? O4 P2 C19 C20 -33.3(13) . . . . ? C25 P2 C19 C20 -154.9(12) . . . . ? C31 P2 C19 C20 88.9(13) . . . . ? C24 C19 C20 C21 0(3) . . . . ? P2 C19 C20 C21 -178.1(16) . . . . ? C19 C20 C21 C22 0(3) . . . . ? C20 C21 C22 C23 0(3) . . . . ? C21 C22 C23 C24 0(3) . . . . ? C22 C23 C24 C19 0(3) . . . . ? C20 C19 C24 C23 1(2) . . . . ? P2 C19 C24 C23 178.2(12) . . . . ? O4 P2 C25 C30 121.0(14) . . . . ? C19 P2 C25 C30 -117.2(15) . . . . ? C31 P2 C25 C30 0.0(17) . . . . ? O4 P2 C25 C26 -52.3(19) . . . . ? C19 P2 C25 C26 69.4(18) . . . . ? C31 P2 C25 C26 -173.4(17) . . . . ? C30 C25 C26 C27 5(3) . . . . ? P2 C25 C26 C27 179.0(16) . . . . ? C25 C26 C27 C28 -6(3) . . . . ? C26 C27 C28 C29 4(2) . . . . ? C27 C28 C29 C30 -2(2) . . . . ? C28 C29 C30 C25 1(2) . . . . ? C26 C25 C30 C29 -3(2) . . . . ? P2 C25 C30 C29 -176.3(12) . . . . ? O4 P2 C31 C36 -29.4(12) . . . . ? C19 P2 C31 C36 -151.7(11) . . . . ? C25 P2 C31 C36 91.6(12) . . . . ? O4 P2 C31 C32 155.6(9) . . . . ? C19 P2 C31 C32 33.3(11) . . . . ? C25 P2 C31 C32 -83.4(12) . . . . ? C36 C31 C32 C33 3(2) . . . . ? P2 C31 C32 C33 178.2(10) . . . . ? C31 C32 C33 C34 -4(2) . . . . ? C32 C33 C34 C35 4(2) . . . . ? C33 C34 C35 C36 -3(3) . . . . ? C34 C35 C36 C31 2(3) . . . . ? C32 C31 C36 C35 -3(2) . . . . ? P2 C31 C36 C35 -177.5(14) . . . . ? U1 O5 C37 O6 11.5(13) . . . . ? U1 O5 C37 C38 -166.2(11) . . . . ? U1 O6 C37 O5 -11.5(13) . . . . ? U1 O6 C37 C38 166.2(11) . . . . ? O5 C37 C38 C39 12(2) . . . . ? O6 C37 C38 C39 -165.5(14) . . . . ? O5 C37 C38 Cl2 -159.6(14) . . . . ? O6 C37 C38 Cl2 23(2) . . . . ? O5 C37 C38 Cl1 172.3(14) . . . . ? O6 C37 C38 Cl1 -5(2) . . . . ? U1 O7 C40 O8 -27(2) . . . . ? U1 O7 C40 C41 154.1(10) . . . . ? O8 C40 C41 C42 -165(2) . . . . ? O7 C40 C41 C42 13(3) . . . . ? O8 C40 C41 Cl3 12(2) . . . . ? O7 C40 C41 Cl3 -169.2(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.009 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.151