# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 loop_ _publ_author_name 'Andreas Danopoulos' 'Jamie Old' 'Scott Winston' _publ_contact_author_name 'Dr Andreas Danopoulos' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ UNITED KINGDOM ; _publ_contact_author_email AD1@SOTON.AC.UK _publ_section_title ; Uranium complexes with dianionic O-methylated calix[4]arene ligands ; _publ_section_references ; ENTER OTHER REFERENCES WinGX - L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838 ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. PLATON/PLUTON - (a) A. L. Spek, Acta Crystallogr., Sect A 1990, 46, C34. (b) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands, A. L. Spek, 1998. ; data_compopund1 _database_code_CSD 192743 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 01sw015 _chemical_melting_point ? _chemical_formula_moiety 'C138 H170 Cl6 O12 U3' _chemical_formula_sum 'C138 H170 Cl6 O12 U3' _chemical_formula_weight 2947.53 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.796(4) _cell_length_b 36.322(7) _cell_length_c 23.030(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.92(3) _cell_angle_gamma 90.00 _cell_volume 17021(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 101600 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Shard _exptl_crystal_colour Green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5888 _exptl_absorpt_coefficient_mu 2.986 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4678 _exptl_absorpt_correction_T_max 0.7749 _exptl_absorpt_process_details Sortav _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source "Nonius FR591 Rotating anode'" _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD area detector' _diffrn_measurement_method 'Phi and Omega scans to fill ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52642 _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.49 _reflns_number_total 19213 _reflns_number_gt 13050 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.1068P)^2^+196.9425P] 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 19213 _refine_ls_number_parameters 738 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.2183 _refine_ls_wR_factor_gt 0.1787 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 2.093 _refine_ls_shift/su_max 4.499 _refine_ls_shift/su_mean 0.030 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 C1 C 0.0539(11) 1.0929(6) 0.5494(8) 0.052(5) Uani 1 1 d . . . C2 C 0.0528(11) 1.0551(6) 0.5485(7) 0.050(5) Uani 1 1 d . . . C3 C 0.0911(11) 1.0371(6) 0.5140(8) 0.055(5) Uani 1 1 d . . . H3 H 0.0926 1.0110 0.5143 0.066 Uiso 1 1 calc R . . C4 C 0.1270(12) 1.0561(7) 0.4793(8) 0.060(6) Uani 1 1 d . . . C5 C 0.1261(13) 1.0941(7) 0.4817(9) 0.066(6) Uani 1 1 d . . . H5 H 0.1505 1.1077 0.4583 0.079 Uiso 1 1 calc R . . C6 C 0.0906(13) 1.1134(6) 0.5175(9) 0.062(6) Uani 1 1 d . . . C7 C 0.1654(14) 1.0367(7) 0.4378(10) 0.070(7) Uani 1 1 d . . . C8 C 0.228(2) 1.0552(11) 0.439(2) 0.16(2) Uani 1 1 d . . . H8A H 0.2475 1.0460 0.4069 0.233 Uiso 1 1 calc R . . H8B H 0.2577 1.0502 0.4774 0.233 Uiso 1 1 calc R . . H8C H 0.2206 1.0818 0.4349 0.233 Uiso 1 1 calc R . . C9 C 0.1223(18) 1.0396(10) 0.3741(15) 0.105(10) Uani 1 1 d U . . H9A H 0.0790 1.0288 0.3736 0.158 Uiso 1 1 calc R . . H9B H 0.1436 1.0262 0.3463 0.158 Uiso 1 1 calc R . . H9C H 0.1172 1.0655 0.3623 0.158 Uiso 1 1 calc R . . C10 C 0.1767(16) 0.9961(7) 0.4533(13) 0.084(8) Uani 1 1 d . . . H10A H 0.1343 0.9833 0.4473 0.126 Uiso 1 1 calc R . . H10B H 0.1993 0.9938 0.4949 0.126 Uiso 1 1 calc R . . H10C H 0.2038 0.9851 0.4278 0.126 Uiso 1 1 calc R . . C11 C 0.0136(10) 1.0329(6) 0.5851(8) 0.051(5) Uani 1 1 d . . . H11A H -0.0134 1.0499 0.6038 0.061 Uiso 1 1 calc R . . H11B H -0.0164 1.0160 0.5588 0.061 Uiso 1 1 calc R . . C12 C 0.0575(10) 1.0112(5) 0.6322(8) 0.047(4) Uani 1 1 d . . . C13 C 0.0981(9) 1.0289(5) 0.6794(8) 0.042(4) Uani 1 1 d . . . C14 C 0.1416(10) 1.0094(5) 0.7221(8) 0.047(5) Uani 1 1 d . . . C15 C 0.1445(11) 0.9714(6) 0.7177(9) 0.054(5) Uani 1 1 d . . . H15 H 0.1748 0.9581 0.7466 0.065 Uiso 1 1 calc R . . C16 C 0.1036(13) 0.9523(6) 0.6715(10) 0.062(6) Uani 1 1 d . . . C17 C 0.0601(12) 0.9730(6) 0.6294(9) 0.059(5) Uani 1 1 d . . . H17 H 0.0315 0.9605 0.5980 0.071 Uiso 1 1 calc R . . C18 C 0.1037(14) 0.9103(7) 0.6683(12) 0.071(7) Uani 1 1 d . . . C19 C 0.095(3) 0.8965(10) 0.6086(18) 0.164(12) Uani 1 1 d U . . H19A H 0.1317 0.9041 0.5912 0.246 Uiso 1 1 calc R . . H19B H 0.0538 0.9065 0.5848 0.246 Uiso 1 1 calc R . . H19C H 0.0920 0.8696 0.6091 0.246 Uiso 1 1 calc R . . C20 C 0.061(3) 0.8949(15) 0.711(2) 0.160(17) Uani 1 1 d U . . H20A H 0.0727 0.9078 0.7490 0.240 Uiso 1 1 calc R . . H20B H 0.0701 0.8685 0.7169 0.240 Uiso 1 1 calc R . . H20C H 0.0148 0.8987 0.6933 0.240 Uiso 1 1 calc R . . C21 C 0.172(2) 0.8937(14) 0.701(2) 0.149(16) Uani 1 1 d U . . H21A H 0.1809 0.9010 0.7425 0.224 Uiso 1 1 calc R . . H21B H 0.2067 0.9031 0.6818 0.224 Uiso 1 1 calc R . . H21C H 0.1702 0.8668 0.6977 0.224 Uiso 1 1 calc R . . C22 C 0.1888(9) 1.0309(6) 0.7707(9) 0.050(5) Uani 1 1 d . . . H22A H 0.1633 1.0477 0.7912 0.060 Uiso 1 1 calc R . . H22B H 0.2131 1.0135 0.8004 0.060 Uiso 1 1 calc R . . C23 C 0.2368(9) 1.0528(6) 0.7435(9) 0.050(5) Uani 1 1 d . . . C24 C 0.2813(12) 1.0345(6) 0.7153(12) 0.066(6) Uani 1 1 d . . . H24 H 0.2834 1.0084 0.7170 0.080 Uiso 1 1 calc R . . C25 C 0.3220(12) 1.0531(7) 0.6855(13) 0.072(7) Uani 1 1 d . . . C26 C 0.3210(11) 1.0910(6) 0.6863(12) 0.069(7) Uani 1 1 d . . . H26 H 0.3504 1.1042 0.6675 0.083 Uiso 1 1 calc R . . C27 C 0.2782(10) 1.1105(6) 0.7140(12) 0.060(6) Uani 1 1 d . . . C28 C 0.2354(9) 1.0907(6) 0.7417(9) 0.050(5) Uani 1 1 d . . . C29 C 0.3674(16) 1.0320(7) 0.6510(18) 0.100(11) Uani 1 1 d . . . C30 C 0.391(2) 1.0564(13) 0.605(2) 0.147(16) Uani 1 1 d U . . H30A H 0.3534 1.0639 0.5739 0.221 Uiso 1 1 calc R . . H30B H 0.4220 1.0424 0.5863 0.221 Uiso 1 1 calc R . . H30C H 0.4131 1.0783 0.6241 0.221 Uiso 1 1 calc R . . C31 C 0.336(3) 0.9972(15) 0.621(2) 0.177(19) Uani 1 1 d U . . H31A H 0.2915 1.0030 0.5985 0.265 Uiso 1 1 calc R . . H31B H 0.3324 0.9788 0.6516 0.265 Uiso 1 1 calc R . . H31C H 0.3625 0.9875 0.5944 0.265 Uiso 1 1 calc R . . C32 C 0.415(3) 1.0114(18) 0.690(3) 0.219(17) Uani 1 1 d U . . H32A H 0.4317 1.0258 0.7262 0.328 Uiso 1 1 calc R . . H32B H 0.4518 1.0057 0.6707 0.328 Uiso 1 1 calc R . . H32C H 0.3957 0.9885 0.7007 0.328 Uiso 1 1 calc R . . C33 C 0.2748(10) 1.1523(6) 0.7083(12) 0.063(6) Uani 1 1 d . . . H33A H 0.2438 1.1622 0.7317 0.075 Uiso 1 1 calc R . . H33B H 0.3187 1.1630 0.7240 0.075 Uiso 1 1 calc R . . C34 C 0.2526(11) 1.1624(5) 0.6451(13) 0.065(7) Uani 1 1 d . . . C35 C 0.2984(13) 1.1750(6) 0.6125(15) 0.078(8) Uani 1 1 d . . . H35 H 0.3424 1.1797 0.6324 0.094 Uiso 1 1 calc R . . C36 C 0.2800(14) 1.1808(6) 0.5502(16) 0.085(10) Uani 1 1 d . . . C37 C 0.2147(16) 1.1762(6) 0.5230(13) 0.083(9) Uani 1 1 d . . . H37 H 0.2011 1.1815 0.4819 0.099 Uiso 1 1 calc R . . C38 C 0.1674(12) 1.1636(6) 0.5554(11) 0.063(6) Uani 1 1 d . . . C39 C 0.1879(10) 1.1569(5) 0.6158(10) 0.054(5) Uani 1 1 d . . . C40 C 0.3315(19) 1.1897(8) 0.513(2) 0.119(15) Uani 1 1 d . . . C41 C 0.359(2) 1.2264(12) 0.530(2) 0.136(14) Uani 1 1 d U . . H41A H 0.3828 1.2261 0.5715 0.204 Uiso 1 1 calc R . . H41B H 0.3240 1.2446 0.5248 0.204 Uiso 1 1 calc R . . H41C H 0.3902 1.2328 0.5045 0.204 Uiso 1 1 calc R . . C42 C 0.378(2) 1.1588(11) 0.517(3) 0.18(3) Uani 1 1 d . . . H42A H 0.3908 1.1556 0.4790 0.267 Uiso 1 1 calc R . . H42B H 0.3572 1.1363 0.5277 0.267 Uiso 1 1 calc R . . H42C H 0.4173 1.1641 0.5480 0.267 Uiso 1 1 calc R . . C43 C 0.303(2) 1.1899(13) 0.447(2) 0.147(18) Uani 1 1 d . . . H43A H 0.2874 1.1652 0.4343 0.220 Uiso 1 1 calc R . . H43B H 0.3371 1.1975 0.4258 0.220 Uiso 1 1 calc R . . H43C H 0.2662 1.2073 0.4385 0.220 Uiso 1 1 calc R . . C44 C 0.0996(14) 1.1549(6) 0.5242(9) 0.067(7) Uani 1 1 d . . . H44A H 0.0907 1.1666 0.4845 0.081 Uiso 1 1 calc R . . H44B H 0.0680 1.1650 0.5469 0.081 Uiso 1 1 calc R . . C45 C 0.2152(10) 1.1179(7) 0.8290(9) 0.059(6) Uani 1 1 d . . . H45A H 0.1813 1.1304 0.8456 0.088 Uiso 1 1 calc R . . H45B H 0.2536 1.1340 0.8325 0.088 Uiso 1 1 calc R . . H45C H 0.2281 1.0950 0.8509 0.088 Uiso 1 1 calc R . . C46 C -0.0485(11) 1.1199(7) 0.5534(9) 0.061(6) Uani 1 1 d . . . H46A H -0.0738 1.1309 0.5805 0.091 Uiso 1 1 calc R . . H46B H -0.0701 1.0972 0.5366 0.091 Uiso 1 1 calc R . . H46C H -0.0462 1.1373 0.5214 0.091 Uiso 1 1 calc R . . C47 C -0.0909(14) 1.2934(6) 0.6561(11) 0.069(7) Uani 1 1 d . . . C48 C -0.1502(14) 1.3074(7) 0.6676(11) 0.073(7) Uani 1 1 d . . . C49 C -0.1882(17) 1.3337(7) 0.6280(12) 0.085(8) Uani 1 1 d . . . H49 H -0.2283 1.3427 0.6361 0.102 Uiso 1 1 calc R . . C50 C -0.1672(18) 1.3459(8) 0.5785(13) 0.090(9) Uani 1 1 d . . . C51 C -0.1075(15) 1.3306(8) 0.5686(14) 0.086(8) Uani 1 1 d U . . H51 H -0.0929 1.3380 0.5339 0.104 Uiso 1 1 calc R . . C52 C -0.0688(16) 1.3053(7) 0.6065(12) 0.081(8) Uani 1 1 d . . . C53 C -0.1707(13) 1.2965(7) 0.7271(13) 0.074(8) Uani 1 1 d . . . C54 C 0.1298(15) 1.3152(7) 0.7215(12) 0.074(8) Uani 1 1 d . . . C55 C 0.1343(13) 1.3547(7) 0.7144(12) 0.070(7) Uani 1 1 d . . . H55 H 0.1642 1.3688 0.7426 0.084 Uiso 1 1 calc R . . C56 C -0.0035(16) 1.2926(7) 0.5965(13) 0.079(8) Uani 1 1 d . . . H56A H 0.0022 1.2660 0.6051 0.095 Uiso 1 1 calc R . . H56B H -0.0004 1.2968 0.5546 0.095 Uiso 1 1 calc R . . C57 C 0.0444(15) 1.3125(8) 0.6341(13) 0.077(8) Uani 1 1 d . . . C58 C 0.0850(13) 1.2956(7) 0.6801(12) 0.072(8) Uani 1 1 d . . . C59 C 0.0529(14) 1.3517(8) 0.6322(13) 0.077(7) Uani 1 1 d U . . H59 H 0.0238 1.3646 0.6018 0.092 Uiso 1 1 calc R . . C60 C 0.0957(15) 1.3710(8) 0.6674(13) 0.079(7) Uani 1 1 d U . . C61 C 0.1044(17) 1.4140(9) 0.6606(15) 0.096(9) Uani 1 1 d U . . C62 C 0.107(2) 1.4207(11) 0.5924(17) 0.121(12) Uani 1 1 d U . . H62A H 0.1057 1.4472 0.5840 0.181 Uiso 1 1 calc R . . H62B H 0.0700 1.4085 0.5668 0.181 Uiso 1 1 calc R . . H62C H 0.1485 1.4105 0.5846 0.181 Uiso 1 1 calc R . . C63 C 0.161(2) 1.4292(14) 0.696(2) 0.151(16) Uani 1 1 d U . . H63A H 0.1997 1.4200 0.6832 0.227 Uiso 1 1 calc R . . H63B H 0.1628 1.4223 0.7376 0.227 Uiso 1 1 calc R . . H63C H 0.1589 1.4561 0.6926 0.227 Uiso 1 1 calc R . . C64 C 0.043(3) 1.4315(14) 0.675(2) 0.159(17) Uani 1 1 d U . . H64A H 0.0051 1.4254 0.6442 0.239 Uiso 1 1 calc R . . H64B H 0.0489 1.4583 0.6775 0.239 Uiso 1 1 calc R . . H64C H 0.0368 1.4222 0.7135 0.239 Uiso 1 1 calc R . . C65 C -0.2104(18) 1.3740(9) 0.5373(16) 0.096(9) Uani 1 1 d U . . C66 C -0.202(3) 1.4084(13) 0.571(2) 0.162(17) Uani 1 1 d U . . H66A H -0.2301 1.4274 0.5481 0.243 Uiso 1 1 calc R . . H66B H -0.1561 1.4161 0.5772 0.243 Uiso 1 1 calc R . . H66C H -0.2147 1.4047 0.6089 0.243 Uiso 1 1 calc R . . C67 C -0.184(3) 1.3794(15) 0.482(3) 0.18(2) Uani 1 1 d U . . H67A H -0.1439 1.3942 0.4915 0.266 Uiso 1 1 calc R . . H67B H -0.2170 1.3921 0.4524 0.266 Uiso 1 1 calc R . . H67C H -0.1741 1.3554 0.4669 0.266 Uiso 1 1 calc R . . C68 C -0.274(3) 1.3628(15) 0.521(2) 0.161(18) Uani 1 1 d U . . H68A H -0.2767 1.3402 0.4978 0.242 Uiso 1 1 calc R . . H68B H -0.3004 1.3821 0.4977 0.242 Uiso 1 1 calc R . . H68C H -0.2918 1.3581 0.5571 0.242 Uiso 1 1 calc R . . C69 C 0.1291(11) 1.2380(6) 0.6556(10) 0.056(5) Uani 1 1 d U . . H69A H 0.1295 1.2114 0.6627 0.084 Uiso 1 1 calc R . . H69B H 0.1736 1.2479 0.6691 0.084 Uiso 1 1 calc R . . H69C H 0.1141 1.2429 0.6131 0.084 Uiso 1 1 calc R . . O5 O -0.0556(7) 1.2684(4) 0.6928(7) 0.059(4) Uani 1 1 d . . . O6 O 0.0842(7) 1.2559(4) 0.6888(6) 0.057(4) Uani 1 1 d . . . Cl1 Cl -0.0001(2) 1.18516(13) 0.64980(19) 0.0454(10) Uani 1 1 d . . . Cl2 Cl 0.1141(2) 1.18471(13) 0.7693(2) 0.0464(10) Uani 1 1 d . . . O1 O 0.0942(6) 1.0664(3) 0.6834(5) 0.040(3) Uani 1 1 d . . . O2 O 0.1896(6) 1.1095(4) 0.7669(6) 0.046(3) Uani 1 1 d . . . O3 O 0.1439(6) 1.1431(4) 0.6468(6) 0.047(3) Uani 1 1 d . . . O4 O 0.0167(7) 1.1116(4) 0.5854(5) 0.048(3) Uani 1 1 d . . . U1 U 0.07664(3) 1.122162(18) 0.69522(3) 0.0366(2) Uani 1 1 d . . . U2 U 0.0000 1.23004(3) 0.7500 0.0443(3) Uani 1 2 d S . . Cl3 Cl -0.0556(2) 1.10009(13) 0.69157(17) 0.0406(9) 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 C1 0.066(13) 0.067(13) 0.029(8) -0.008(8) 0.025(9) 0.002(10) C2 0.069(13) 0.059(12) 0.024(8) -0.015(8) 0.015(8) -0.009(10) C3 0.067(13) 0.063(13) 0.038(10) -0.012(9) 0.022(10) -0.008(10) C4 0.075(15) 0.077(15) 0.033(9) -0.009(10) 0.022(10) -0.008(12) C5 0.100(18) 0.071(15) 0.040(10) 0.003(10) 0.046(12) -0.009(13) C6 0.088(17) 0.062(13) 0.044(11) -0.004(10) 0.034(12) -0.006(12) C7 0.098(19) 0.066(14) 0.059(13) -0.014(11) 0.050(14) -0.003(13) C8 0.14(3) 0.11(3) 0.26(6) -0.07(3) 0.15(4) -0.03(2) C9 0.106(10) 0.106(10) 0.105(10) 0.000(2) 0.022(3) 0.000(2) C10 0.11(2) 0.073(17) 0.086(18) -0.009(14) 0.054(17) 0.014(15) C11 0.061(12) 0.060(12) 0.034(9) -0.009(8) 0.018(9) -0.013(10) C12 0.056(11) 0.054(11) 0.038(9) -0.007(8) 0.023(9) -0.009(9) C13 0.050(10) 0.047(10) 0.035(9) -0.011(8) 0.023(8) -0.005(8) C14 0.064(12) 0.054(11) 0.033(9) -0.001(8) 0.031(9) -0.004(9) C15 0.072(14) 0.055(12) 0.043(10) 0.000(9) 0.030(10) -0.001(10) C16 0.095(17) 0.047(11) 0.056(12) -0.001(10) 0.045(13) -0.007(11) C17 0.083(15) 0.055(12) 0.045(11) -0.005(10) 0.028(11) -0.012(11) C18 0.094(19) 0.055(13) 0.071(15) -0.005(11) 0.033(14) -0.005(12) C19 0.310(12) 0.067(12) 0.111(12) 0.000(2) 0.035(3) 0.000(2) C20 0.160(17) 0.160(17) 0.160(17) 0.000(2) 0.033(4) 0.000(2) C21 0.149(16) 0.149(16) 0.149(16) 0.000(2) 0.031(4) 0.000(2) C22 0.043(10) 0.065(13) 0.045(10) 0.008(9) 0.018(8) 0.006(9) C23 0.038(10) 0.058(12) 0.058(12) 0.001(10) 0.017(9) 0.004(8) C24 0.064(14) 0.049(12) 0.096(18) -0.005(12) 0.041(13) -0.002(10) C25 0.056(13) 0.065(14) 0.11(2) -0.009(14) 0.047(14) 0.008(11) C26 0.058(13) 0.057(13) 0.109(19) -0.012(13) 0.056(14) -0.003(10) C27 0.044(11) 0.050(11) 0.093(17) -0.004(11) 0.029(11) 0.003(9) C28 0.038(9) 0.061(12) 0.055(11) -0.008(9) 0.022(9) 0.000(9) C29 0.10(2) 0.049(14) 0.18(3) 0.007(17) 0.09(2) 0.012(13) C30 0.147(16) 0.147(16) 0.147(16) 0.000(2) 0.031(4) 0.000(2) C31 0.181(19) 0.180(19) 0.180(19) -0.005(2) 0.062(4) 0.000(2) C32 0.219(17) 0.219(17) 0.219(17) 0.000(2) 0.045(4) 0.143(2) C33 0.039(10) 0.059(13) 0.101(18) -0.020(12) 0.041(12) -0.011(9) C34 0.060(13) 0.039(10) 0.11(2) -0.018(12) 0.062(14) -0.010(9) C35 0.075(16) 0.047(12) 0.14(3) -0.002(14) 0.074(18) -0.003(11) C36 0.084(19) 0.049(13) 0.15(3) 0.017(15) 0.09(2) 0.007(12) C37 0.13(3) 0.048(13) 0.100(19) 0.009(13) 0.08(2) 0.010(14) C38 0.080(16) 0.052(12) 0.077(15) -0.003(11) 0.062(14) -0.002(11) C39 0.063(13) 0.045(10) 0.069(13) -0.010(9) 0.052(11) -0.001(9) C40 0.14(3) 0.069(17) 0.20(4) 0.04(2) 0.14(3) 0.010(17) C41 0.136(14) 0.136(14) 0.137(14) 0.000(2) 0.030(4) 0.000(2) C42 0.18(4) 0.13(3) 0.30(6) 0.05(4) 0.21(5) 0.05(3) C43 0.15(4) 0.18(4) 0.15(4) 0.05(3) 0.11(3) 0.01(3) C44 0.10(2) 0.066(14) 0.044(11) 0.009(10) 0.046(13) 0.017(13) C45 0.041(11) 0.086(16) 0.049(11) -0.017(11) 0.008(9) 0.000(10) C46 0.061(13) 0.090(17) 0.033(9) 0.007(10) 0.012(9) 0.011(11) C47 0.098(18) 0.056(13) 0.063(14) 0.009(11) 0.042(13) 0.021(13) C48 0.10(2) 0.060(14) 0.071(15) 0.010(12) 0.047(15) 0.006(13) C49 0.12(2) 0.067(16) 0.077(17) -0.004(14) 0.046(18) 0.011(16) C50 0.13(3) 0.068(16) 0.079(18) -0.009(14) 0.039(18) 0.006(17) C51 0.087(8) 0.086(8) 0.086(8) 0.000(2) 0.018(3) 0.000(2) C52 0.13(2) 0.059(14) 0.077(16) 0.018(12) 0.062(17) 0.016(15) C53 0.084(17) 0.062(14) 0.100(19) 0.027(14) 0.071(16) 0.025(12) C54 0.10(2) 0.062(14) 0.080(17) 0.011(13) 0.067(16) 0.013(14) C55 0.085(17) 0.060(14) 0.082(16) -0.013(12) 0.053(15) -0.015(12) C56 0.12(2) 0.059(14) 0.082(17) 0.019(13) 0.068(18) 0.008(15) C57 0.087(19) 0.076(17) 0.085(18) 0.035(15) 0.059(16) 0.026(15) C58 0.086(17) 0.063(14) 0.092(18) -0.035(14) 0.074(16) -0.023(13) C59 0.077(7) 0.077(7) 0.077(7) 0.001(2) 0.017(3) 0.001(2) C60 0.079(7) 0.079(7) 0.079(7) 0.000(2) 0.017(3) 0.000(2) C61 0.096(9) 0.095(9) 0.096(9) 0.000(2) 0.020(3) 0.000(2) C62 0.121(12) 0.121(12) 0.121(12) 0.001(2) 0.025(3) 0.000(2) C63 0.151(16) 0.151(16) 0.151(16) 0.000(2) 0.031(4) 0.000(2) C64 0.160(17) 0.159(17) 0.160(17) 0.000(2) 0.033(4) 0.000(2) C65 0.096(9) 0.096(9) 0.096(9) 0.000(2) 0.020(3) 0.000(2) C66 0.190(17) 0.136(17) 0.159(17) 0.000(2) 0.035(4) 0.000(2) C67 0.18(2) 0.18(2) 0.18(2) 0.000(2) 0.037(5) 0.000(2) C68 0.161(18) 0.161(18) 0.161(18) 0.000(2) 0.033(4) 0.000(2) C69 0.056(5) 0.056(5) 0.056(5) 0.000(2) 0.013(2) -0.001(2) O5 0.068(9) 0.058(9) 0.066(9) 0.016(7) 0.045(8) 0.009(7) O6 0.072(9) 0.045(7) 0.071(9) -0.006(7) 0.055(8) -0.008(7) Cl1 0.051(2) 0.053(3) 0.039(2) 0.0035(19) 0.0250(19) 0.001(2) Cl2 0.040(2) 0.058(3) 0.046(2) -0.013(2) 0.0209(19) -0.0048(19) O1 0.040(6) 0.054(7) 0.027(5) -0.004(5) 0.013(5) -0.003(5) O2 0.029(6) 0.065(8) 0.046(7) -0.014(6) 0.013(5) 0.000(6) O3 0.048(7) 0.051(7) 0.053(7) -0.006(6) 0.034(6) -0.005(6) O4 0.051(8) 0.068(8) 0.026(6) -0.002(6) 0.015(5) 0.001(6) U1 0.0346(4) 0.0490(4) 0.0313(3) -0.0042(3) 0.0188(3) -0.0024(3) U2 0.0499(6) 0.0459(6) 0.0472(5) 0.000 0.0337(5) 0.000 Cl3 0.035(2) 0.060(3) 0.0297(18) 0.0006(18) 0.0125(16) -0.0047(18) _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 C1 C2 1.37(3) . ? C1 C6 1.38(3) . ? C1 O4 1.42(2) . ? C2 C3 1.40(3) . ? C2 C11 1.52(3) . ? C3 C4 1.38(3) . ? C4 C5 1.38(3) . ? C4 C7 1.54(3) . ? C5 C6 1.40(3) . ? C6 C44 1.52(3) . ? C7 C8 1.46(4) . ? C7 C10 1.53(4) . ? C7 C9 1.56(4) . ? C11 C12 1.49(3) . ? C12 C13 1.39(3) . ? C12 C17 1.39(3) . ? C13 O1 1.37(2) . ? C13 C14 1.39(3) . ? C14 C15 1.38(3) . ? C14 C22 1.54(3) . ? C15 C16 1.40(3) . ? C16 C17 1.40(3) . ? C16 C18 1.53(3) . ? C18 C19 1.44(4) . ? C18 C20 1.55(6) . ? C18 C21 1.58(5) . ? C22 C23 1.51(3) . ? C23 C28 1.38(3) . ? C23 C24 1.40(3) . ? C24 C25 1.37(3) . ? C25 C26 1.38(3) . ? C25 C29 1.56(3) . ? C26 C27 1.39(3) . ? C27 C28 1.40(3) . ? C27 C33 1.52(3) . ? C28 O2 1.39(2) . ? C29 C32 1.41(6) . ? C29 C31 1.52(6) . ? C29 C30 1.55(5) . ? C33 C34 1.48(4) . ? C34 C39 1.39(3) . ? C34 C35 1.41(3) . ? C35 C36 1.42(4) . ? C36 C37 1.38(4) . ? C36 C40 1.53(3) . ? C37 C38 1.43(3) . ? C38 C39 1.39(3) . ? C38 C44 1.48(4) . ? C39 O3 1.37(2) . ? C40 C41 1.47(5) . ? C40 C42 1.47(5) . ? C40 C43 1.52(6) . ? C45 O2 1.45(2) . ? C46 O4 1.44(3) . ? C47 O5 1.35(3) . ? C47 C52 1.39(3) . ? C47 C48 1.41(3) . ? C48 C49 1.44(4) . ? C48 C53 1.57(3) . ? C49 C50 1.38(4) . ? C50 C51 1.42(4) . ? C50 C65 1.55(4) . ? C51 C52 1.40(4) . ? C52 C56 1.50(4) . ? C53 C54 1.47(4) 2_556 ? C54 C58 1.38(4) . ? C54 C55 1.45(3) . ? C54 C53 1.47(4) 2_556 ? C55 C60 1.35(4) . ? C56 C57 1.38(4) . ? C57 C58 1.36(4) . ? C57 C59 1.43(4) . ? C58 O6 1.45(3) . ? C59 C60 1.28(4) . ? C60 C61 1.59(4) . ? C61 C63 1.40(5) . ? C61 C64 1.52(6) . ? C61 C62 1.60(5) . ? C65 C68 1.37(6) . ? C65 C66 1.46(5) . ? C65 C67 1.49(6) . ? C69 O6 1.47(2) . ? O5 U2 2.093(15) . ? O6 U2 2.637(12) . ? Cl1 U2 2.825(4) . ? Cl1 U1 2.861(5) . ? Cl2 U2 2.847(5) . ? Cl2 U1 2.852(5) . ? O1 U1 2.087(12) . ? O2 U1 2.617(12) . ? O3 U1 2.103(11) . ? O4 U1 2.606(12) . ? U1 Cl3 2.847(4) 2_556 ? U1 Cl3 2.849(4) . ? U2 O5 2.093(15) 2_556 ? U2 O6 2.637(12) 2_556 ? U2 Cl1 2.825(4) 2_556 ? U2 Cl2 2.847(5) 2_556 ? Cl3 U1 2.847(4) 2_556 ? 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 C2 C1 C6 122.7(18) . . ? C2 C1 O4 118.7(17) . . ? C6 C1 O4 118.7(19) . . ? C1 C2 C3 117.8(19) . . ? C1 C2 C11 121.9(17) . . ? C3 C2 C11 120.3(19) . . ? C4 C3 C2 122(2) . . ? C5 C4 C3 117(2) . . ? C5 C4 C7 119.7(19) . . ? C3 C4 C7 123(2) . . ? C4 C5 C6 122.4(19) . . ? C1 C6 C5 117(2) . . ? C1 C6 C44 123.4(19) . . ? C5 C6 C44 119.0(19) . . ? C8 C7 C10 110(3) . . ? C8 C7 C4 110(2) . . ? C10 C7 C4 111.8(19) . . ? C8 C7 C9 109(3) . . ? C10 C7 C9 108(2) . . ? C4 C7 C9 106(2) . . ? C12 C11 C2 111.4(18) . . ? C13 C12 C17 118(2) . . ? C13 C12 C11 120.5(18) . . ? C17 C12 C11 121.2(18) . . ? O1 C13 C12 118.6(17) . . ? O1 C13 C14 119.9(16) . . ? C12 C13 C14 121.5(18) . . ? C15 C14 C13 119.2(19) . . ? C15 C14 C22 121.9(19) . . ? C13 C14 C22 118.8(17) . . ? C14 C15 C16 121(2) . . ? C17 C16 C15 118(2) . . ? C17 C16 C18 121(2) . . ? C15 C16 C18 122(2) . . ? C12 C17 C16 122(2) . . ? C19 C18 C16 113(2) . . ? C19 C18 C20 120(4) . . ? C16 C18 C20 109(3) . . ? C19 C18 C21 104(3) . . ? C16 C18 C21 112(3) . . ? C20 C18 C21 98(3) . . ? C23 C22 C14 110.0(15) . . ? C28 C23 C24 118.1(19) . . ? C28 C23 C22 122.0(17) . . ? C24 C23 C22 119.8(19) . . ? C25 C24 C23 122(2) . . ? C24 C25 C26 118(2) . . ? C24 C25 C29 121(2) . . ? C26 C25 C29 121(2) . . ? C25 C26 C27 122(2) . . ? C26 C27 C28 118(2) . . ? C26 C27 C33 119.3(19) . . ? C28 C27 C33 122.0(18) . . ? C23 C28 O2 119.2(17) . . ? C23 C28 C27 121.1(18) . . ? O2 C28 C27 119.6(18) . . ? C32 C29 C31 92(4) . . ? C32 C29 C30 117(4) . . ? C31 C29 C30 110(4) . . ? C32 C29 C25 111(4) . . ? C31 C29 C25 113(3) . . ? C30 C29 C25 113(3) . . ? C34 C33 C27 109.4(19) . . ? C39 C34 C35 119(3) . . ? C39 C34 C33 121.2(17) . . ? C35 C34 C33 120(2) . . ? C34 C35 C36 121(3) . . ? C37 C36 C35 118(2) . . ? C37 C36 C40 120(3) . . ? C35 C36 C40 121(3) . . ? C36 C37 C38 121(3) . . ? C39 C38 C37 119(3) . . ? C39 C38 C44 120.9(17) . . ? C37 C38 C44 120(2) . . ? O3 C39 C38 119(2) . . ? O3 C39 C34 119(2) . . ? C38 C39 C34 121.8(19) . . ? C41 C40 C42 117(4) . . ? C41 C40 C36 109(3) . . ? C42 C40 C36 109(2) . . ? C41 C40 C43 108(3) . . ? C42 C40 C43 100(4) . . ? C36 C40 C43 113(3) . . ? C38 C44 C6 110(2) . . ? O5 C47 C52 120(2) . . ? O5 C47 C48 121(2) . . ? C52 C47 C48 120(2) . . ? C47 C48 C49 121(2) . . ? C47 C48 C53 119(2) . . ? C49 C48 C53 120(2) . . ? C50 C49 C48 121(3) . . ? C49 C50 C51 116(3) . . ? C49 C50 C65 118(3) . . ? C51 C50 C65 125(3) . . ? C52 C51 C50 124(3) . . ? C47 C52 C51 118(3) . . ? C47 C52 C56 120(2) . . ? C51 C52 C56 122(2) . . ? C54 C53 C48 112(2) 2_556 . ? C58 C54 C55 119(3) . . ? C58 C54 C53 121(2) . 2_556 ? C55 C54 C53 120(3) . 2_556 ? C60 C55 C54 119(3) . . ? C57 C56 C52 107(2) . . ? C58 C57 C56 120(3) . . ? C58 C57 C59 114(3) . . ? C56 C57 C59 125(3) . . ? C57 C58 C54 122(3) . . ? C57 C58 O6 122(2) . . ? C54 C58 O6 116(3) . . ? C60 C59 C57 127(3) . . ? C59 C60 C55 119(3) . . ? C59 C60 C61 124(3) . . ? C55 C60 C61 117(3) . . ? C63 C61 C64 110(4) . . ? C63 C61 C60 116(3) . . ? C64 C61 C60 106(3) . . ? C63 C61 C62 108(3) . . ? C64 C61 C62 111(3) . . ? C60 C61 C62 106(3) . . ? C68 C65 C66 114(4) . . ? C68 C65 C67 108(4) . . ? C66 C65 C67 108(4) . . ? C68 C65 C50 112(4) . . ? C66 C65 C50 105(3) . . ? C67 C65 C50 110(3) . . ? C47 O5 U2 179.3(19) . . ? C58 O6 C69 109.8(14) . . ? C58 O6 U2 117.0(10) . . ? C69 O6 U2 132.9(11) . . ? U2 Cl1 U1 104.87(15) . . ? U2 Cl2 U1 104.54(15) . . ? C13 O1 U1 171.7(10) . . ? C28 O2 C45 111.7(15) . . ? C28 O2 U1 115.1(11) . . ? C45 O2 U1 133.2(11) . . ? C39 O3 U1 179.4(14) . . ? C1 O4 C46 111.8(14) . . ? C1 O4 U1 115.4(11) . . ? C46 O4 U1 132.7(11) . . ? O1 U1 O3 97.4(5) . . ? O1 U1 O4 78.0(4) . . ? O3 U1 O4 77.0(5) . . ? O1 U1 O2 75.7(4) . . ? O3 U1 O2 77.9(5) . . ? O4 U1 O2 140.6(4) . . ? O1 U1 Cl3 84.8(3) . 2_556 ? O3 U1 Cl3 146.4(4) . 2_556 ? O4 U1 Cl3 135.6(3) . 2_556 ? O2 U1 Cl3 70.1(3) . 2_556 ? O1 U1 Cl3 85.2(3) . . ? O3 U1 Cl3 146.1(4) . . ? O4 U1 Cl3 70.4(3) . . ? O2 U1 Cl3 134.7(3) . . ? Cl3 U1 Cl3 67.52(15) 2_556 . ? O1 U1 Cl2 144.9(3) . . ? O3 U1 Cl2 84.3(4) . . ? O4 U1 Cl2 135.6(3) . . ? O2 U1 Cl2 70.3(3) . . ? Cl3 U1 Cl2 75.58(13) 2_556 . ? Cl3 U1 Cl2 112.63(12) . . ? O1 U1 Cl1 145.9(3) . . ? O3 U1 Cl1 84.2(4) . . ? O4 U1 Cl1 69.2(3) . . ? O2 U1 Cl1 137.0(3) . . ? Cl3 U1 Cl1 112.36(12) 2_556 . ? Cl3 U1 Cl1 75.66(13) . . ? Cl2 U1 Cl1 69.18(14) . . ? O5 U2 O5 96.6(9) . 2_556 ? O5 U2 O6 76.6(5) . . ? O5 U2 O6 76.0(5) 2_556 . ? O5 U2 O6 76.0(5) . 2_556 ? O5 U2 O6 76.6(5) 2_556 2_556 ? O6 U2 O6 138.2(6) . 2_556 ? O5 U2 Cl1 87.9(4) . . ? O5 U2 Cl1 143.6(4) 2_556 . ? O6 U2 Cl1 70.0(3) . . ? O6 U2 Cl1 138.9(4) 2_556 . ? O5 U2 Cl1 143.6(4) . 2_556 ? O5 U2 Cl1 87.9(4) 2_556 2_556 ? O6 U2 Cl1 138.9(4) . 2_556 ? O6 U2 Cl1 70.0(3) 2_556 2_556 ? Cl1 U2 Cl1 109.51(18) . 2_556 ? O5 U2 Cl2 87.2(4) . 2_556 ? O5 U2 Cl2 144.8(4) 2_556 2_556 ? O6 U2 Cl2 138.3(3) . 2_556 ? O6 U2 Cl2 70.5(3) 2_556 2_556 ? Cl1 U2 Cl2 71.26(13) . 2_556 ? Cl1 U2 Cl2 69.75(14) 2_556 2_556 ? O5 U2 Cl2 144.8(4) . . ? O5 U2 Cl2 87.2(4) 2_556 . ? O6 U2 Cl2 70.5(3) . . ? O6 U2 Cl2 138.3(3) 2_556 . ? Cl1 U2 Cl2 69.75(14) . . ? Cl1 U2 Cl2 71.26(13) 2_556 . ? Cl2 U2 Cl2 109.34(19) 2_556 . ? U1 Cl3 U1 102.94(13) 2_556 . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 3.465 _refine_diff_density_min -2.656 _refine_diff_density_rms 0.187