Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address D.Collinson ; FIRST AUTHORS ADDRESS ; M.Helliwell '' G.H.John '' I.May '' M.Sarsfield '' _publ_contact_author_name 'David Collison' _publ_contact_author_address ; Department of Chemistry University of Manchester Manchester M13 9PL UNITED KINGDOM ; _publ_contact_author_email DAVID.COLLISON@MANCHESTER.AC.UK _publ_section_title ; Dimeric uranyl complexes with bridging perrhenates ; _publ_contact_author ; Madeleine Helliwell ; _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? # Attachment 'Uranylbridge2.cif' data_s945abs _database_code_depnum_ccdc_archive 'CCDC 623014' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _publ_section_exptl_refinement ; The structure was solved by direct methods, and there are 2 half molecules in the asymmetric unit. The non-H atoms were refined anisotropically, and H atoms were included in calculated positions. ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H108 O36 P4 Re4 U2' _chemical_formula_weight 2606.08 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' Re Re -1.0185 7.2310 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 26.129(5) _cell_length_b 10.1329(18) _cell_length_c 30.099(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.113(5) _cell_angle_gamma 90.00 _cell_volume 7957(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6518 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 26.08 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4912 _exptl_absorpt_coefficient_mu 10.276 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2108 _exptl_absorpt_correction_T_max 0.6840 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57489 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.39 _reflns_number_total 16241 _reflns_number_gt 12479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^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 16241 _refine_ls_number_parameters 871 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.446719(9) 0.45633(2) 0.399508(8) 0.01449(6) Uani 1 1 d . . . Re1 Re 0.554863(12) 0.33325(3) 0.486054(10) 0.02166(7) Uani 1 1 d . . . Re2 Re 0.383055(11) 0.25606(3) 0.293231(10) 0.02371(7) Uani 1 1 d . . . P1 P 0.53511(7) 0.21984(18) 0.34613(6) 0.0175(4) Uani 1 1 d . . . P2 P 0.32166(7) 0.6477(2) 0.38548(7) 0.0234(4) Uani 1 1 d . . . O1 O 0.41571(18) 0.3412(5) 0.43243(16) 0.0237(12) Uani 1 1 d . . . O2 O 0.47894(18) 0.5751(5) 0.36860(15) 0.0213(11) Uani 1 1 d . . . O3 O 0.51917(18) 0.4507(5) 0.45539(15) 0.0209(11) Uani 1 1 d . . . O4 O 0.5646(2) 0.3829(5) 0.54126(16) 0.0267(12) Uani 1 1 d . . . O5 O 0.5225(3) 0.1868(5) 0.48383(19) 0.0490(17) Uani 1 1 d . . . O6 O 0.6124(2) 0.3129(6) 0.46385(19) 0.0455(16) Uani 1 1 d . . . O7 O 0.41169(18) 0.3550(5) 0.33547(17) 0.0295(13) Uani 1 1 d . . . O8 O 0.3189(2) 0.2469(6) 0.2991(2) 0.0458(17) Uani 1 1 d . . . O9 O 0.3945(3) 0.3213(7) 0.2429(2) 0.066(2) Uani 1 1 d . . . O10 O 0.4069(2) 0.0992(6) 0.2958(2) 0.0500(18) Uani 1 1 d . . . O11 O 0.50732(17) 0.2947(5) 0.37975(15) 0.0199(11) Uani 1 1 d . . . O12 O 0.53409(18) 0.0679(5) 0.35168(15) 0.0213(11) Uani 1 1 d . . . O13 O 0.59337(17) 0.2550(5) 0.34777(17) 0.0234(12) Uani 1 1 d . . . O14 O 0.51084(18) 0.2473(5) 0.29914(15) 0.0204(11) Uani 1 1 d . . . O15 O 0.36844(18) 0.5671(5) 0.38226(16) 0.0244(12) Uani 1 1 d . . . O16 O 0.2830(2) 0.5870(6) 0.41752(19) 0.0448(17) Uani 1 1 d . . . O17 O 0.33167(19) 0.7916(5) 0.40248(18) 0.0310(13) Uani 1 1 d . . . O18 O 0.29097(18) 0.6644(5) 0.34061(17) 0.0264(12) Uani 1 1 d . . . C1 C 0.5568(3) 0.0022(7) 0.3917(2) 0.0288(18) Uani 1 1 d . . . H1A H 0.5411 0.0351 0.4179 0.035 Uiso 1 1 calc R . . H1B H 0.5933 0.0204 0.3947 0.035 Uiso 1 1 calc R . . C2 C 0.5479(3) -0.1437(7) 0.3872(2) 0.0244(17) Uani 1 1 d . . . H2 H 0.5110 -0.1590 0.3828 0.029 Uiso 1 1 calc R . . C3 C 0.5669(3) -0.2125(7) 0.4302(3) 0.037(2) Uani 1 1 d . . . H3A H 0.6034 -0.2022 0.4342 0.055 Uiso 1 1 calc R . . H3B H 0.5586 -0.3046 0.4283 0.055 Uiso 1 1 calc R . . H3C H 0.5507 -0.1737 0.4549 0.055 Uiso 1 1 calc R . . C4 C 0.5741(3) -0.2010(7) 0.3474(3) 0.0307(19) Uani 1 1 d . . . H4A H 0.5649 -0.1499 0.3213 0.046 Uiso 1 1 calc R . . H4B H 0.5633 -0.2907 0.3428 0.046 Uiso 1 1 calc R . . H4C H 0.6106 -0.1984 0.3531 0.046 Uiso 1 1 calc R . . C5 C 0.6098(3) 0.3928(7) 0.3522(2) 0.0202(16) Uani 1 1 d . . . H5A H 0.6036 0.4252 0.3818 0.024 Uiso 1 1 calc R . . H5B H 0.5907 0.4472 0.3306 0.024 Uiso 1 1 calc R . . C6 C 0.6671(3) 0.4000(8) 0.3442(3) 0.0299(19) Uani 1 1 d . . . H6 H 0.6720 0.3738 0.3134 0.036 Uiso 1 1 calc R . . C7 C 0.6975(3) 0.3094(9) 0.3740(3) 0.044(2) Uani 1 1 d . . . H7A H 0.6956 0.3379 0.4043 0.066 Uiso 1 1 calc R . . H7B H 0.7326 0.3100 0.3661 0.066 Uiso 1 1 calc R . . H7C H 0.6840 0.2216 0.3709 0.066 Uiso 1 1 calc R . . C8 C 0.6833(3) 0.5448(8) 0.3498(3) 0.040(2) Uani 1 1 d . . . H8A H 0.6653 0.5974 0.3275 0.061 Uiso 1 1 calc R . . H8B H 0.7195 0.5524 0.3465 0.061 Uiso 1 1 calc R . . H8C H 0.6753 0.5752 0.3788 0.061 Uiso 1 1 calc R . . C9 C 0.5221(3) 0.1667(7) 0.2606(2) 0.0259(17) Uani 1 1 d . . . H9A H 0.4941 0.1056 0.2540 0.031 Uiso 1 1 calc R . . H9B H 0.5530 0.1159 0.2671 0.031 Uiso 1 1 calc R . . C10 C 0.5292(3) 0.2550(7) 0.2207(2) 0.0235(17) Uani 1 1 d . . . H10 H 0.5007 0.3179 0.2185 0.028 Uiso 1 1 calc R . . C11 C 0.5786(3) 0.3323(9) 0.2253(3) 0.037(2) Uani 1 1 d . . . H11A H 0.6071 0.2724 0.2266 0.056 Uiso 1 1 calc R . . H11B H 0.5792 0.3840 0.2521 0.056 Uiso 1 1 calc R . . H11C H 0.5810 0.3897 0.2001 0.056 Uiso 1 1 calc R . . C12 C 0.5266(4) 0.1705(8) 0.1790(3) 0.040(2) Uani 1 1 d . . . H12A H 0.5347 0.2235 0.1539 0.060 Uiso 1 1 calc R . . H12B H 0.4927 0.1350 0.1743 0.060 Uiso 1 1 calc R . . H12C H 0.5508 0.0995 0.1825 0.060 Uiso 1 1 calc R . . C13 C 0.3008(3) 0.5155(9) 0.4571(3) 0.042(2) Uani 1 1 d . . . H13A H 0.3164 0.5763 0.4787 0.051 Uiso 1 1 calc R . . H13B H 0.3264 0.4512 0.4495 0.051 Uiso 1 1 calc R . . C14 C 0.2562(3) 0.4470(8) 0.4764(3) 0.0311(19) Uani 1 1 d . . . H14 H 0.2313 0.5138 0.4847 0.037 Uiso 1 1 calc R . . C15 C 0.2293(4) 0.3491(10) 0.4454(4) 0.063(3) Uani 1 1 d . . . H15A H 0.2181 0.3928 0.4183 0.095 Uiso 1 1 calc R . . H15B H 0.2002 0.3131 0.4593 0.095 Uiso 1 1 calc R . . H15C H 0.2526 0.2792 0.4389 0.095 Uiso 1 1 calc R . . C16 C 0.2774(4) 0.3768(9) 0.5190(3) 0.052(3) Uani 1 1 d . . . H16A H 0.2984 0.3036 0.5111 0.078 Uiso 1 1 calc R . . H16B H 0.2495 0.3452 0.5355 0.078 Uiso 1 1 calc R . . H16C H 0.2976 0.4377 0.5370 0.078 Uiso 1 1 calc R . . C17 C 0.3688(3) 0.8762(9) 0.3816(4) 0.063(3) Uani 1 1 d . . . H17A H 0.3554 0.9032 0.3523 0.076 Uiso 1 1 calc R . . H17B H 0.4005 0.8284 0.3783 0.076 Uiso 1 1 calc R . . C18 C 0.3786(4) 0.9948(12) 0.4103(5) 0.097(6) Uani 1 1 d . . . H18 H 0.3984 1.0485 0.3903 0.116 Uiso 1 1 calc R . . C19 C 0.4109(6) 0.9895(13) 0.4449(5) 0.152(9) Uani 1 1 d . . . H19A H 0.3996 0.9246 0.4654 0.227 Uiso 1 1 calc R . . H19B H 0.4127 1.0742 0.4591 0.227 Uiso 1 1 calc R . . H19C H 0.4442 0.9658 0.4355 0.227 Uiso 1 1 calc R . . C20 C 0.3313(3) 1.0812(8) 0.4131(4) 0.055(3) Uani 1 1 d . . . H20A H 0.3401 1.1596 0.4297 0.083 Uiso 1 1 calc R . . H20B H 0.3053 1.0335 0.4277 0.083 Uiso 1 1 calc R . . H20C H 0.3187 1.1050 0.3836 0.083 Uiso 1 1 calc R . . C21 C 0.2803(3) 0.5483(8) 0.3115(3) 0.0295(19) Uani 1 1 d . . . H21A H 0.2809 0.4687 0.3294 0.035 Uiso 1 1 calc R . . H21B H 0.3067 0.5408 0.2902 0.035 Uiso 1 1 calc R . . C22 C 0.2291(3) 0.5623(9) 0.2873(3) 0.036(2) Uani 1 1 d . . . H22 H 0.2280 0.6474 0.2717 0.043 Uiso 1 1 calc R . . C23 C 0.1861(3) 0.5594(8) 0.3190(3) 0.034(2) Uani 1 1 d . . . H23A H 0.1827 0.4718 0.3306 0.051 Uiso 1 1 calc R . . H23B H 0.1546 0.5850 0.3035 0.051 Uiso 1 1 calc R . . H23C H 0.1937 0.6197 0.3431 0.051 Uiso 1 1 calc R . . C24 C 0.2232(3) 0.4521(9) 0.2525(3) 0.043(2) Uani 1 1 d . . . H24A H 0.2514 0.4555 0.2333 0.065 Uiso 1 1 calc R . . H24B H 0.1916 0.4636 0.2351 0.065 Uiso 1 1 calc R . . H24C H 0.2231 0.3680 0.2672 0.065 Uiso 1 1 calc R . . U2 U 0.545059(9) 0.59369(2) 0.101202(8) 0.01387(6) Uani 1 1 d . . . Re3 Re 0.619363(11) 0.76920(3) 0.206645(10) 0.02131(7) Uani 1 1 d . . . Re4 Re 0.576455(10) 0.38358(3) -0.006794(9) 0.01592(7) Uani 1 1 d . . . P3 P 0.66458(7) 0.39631(19) 0.11664(7) 0.0219(4) Uani 1 1 d . . . P4 P 0.43135(7) 0.78586(18) 0.13090(6) 0.0188(4) Uani 1 1 d . . . O19 O 0.51110(18) 0.4797(5) 0.13238(16) 0.0213(11) Uani 1 1 d . . . O20 O 0.57781(18) 0.7046(5) 0.06782(16) 0.0236(11) Uani 1 1 d . . . O21 O 0.57569(18) 0.7063(5) 0.16550(17) 0.0298(13) Uani 1 1 d . . . O22 O 0.6771(2) 0.8050(7) 0.1847(2) 0.0522(18) Uani 1 1 d . . . O23 O 0.6293(2) 0.6563(6) 0.24818(19) 0.0414(15) Uani 1 1 d . . . O24 O 0.5945(2) 0.9099(6) 0.2281(2) 0.0523(19) Uani 1 1 d . . . O25 O 0.56325(17) 0.4208(4) 0.04828(15) 0.0199(11) Uani 1 1 d . . . O26 O 0.52286(18) 0.4145(5) -0.04199(16) 0.0230(11) Uani 1 1 d . . . O27 O 0.6264(2) 0.4796(6) -0.02253(18) 0.0382(14) Uani 1 1 d . . . O28 O 0.5929(2) 0.2219(5) -0.00981(16) 0.0305(13) Uani 1 1 d . . . O29 O 0.62490(17) 0.4952(5) 0.12546(15) 0.0205(11) Uani 1 1 d . . . O30 O 0.6873(2) 0.4125(5) 0.0697(2) 0.0461(17) Uani 1 1 d . . . O31 O 0.64083(18) 0.2576(5) 0.11542(18) 0.0276(12) Uani 1 1 d . . . O32 O 0.7124(2) 0.4034(7) 0.1475(2) 0.058(2) Uani 1 1 d . . . O33 O 0.48407(18) 0.7557(5) 0.11711(17) 0.0237(12) Uani 1 1 d . . . O34 O 0.42344(19) 0.7722(5) 0.18126(16) 0.0249(12) Uani 1 1 d . . . O35 O 0.38915(19) 0.6949(5) 0.10950(16) 0.0264(12) Uani 1 1 d . . . O36 O 0.41578(18) 0.9287(4) 0.11691(16) 0.0227(11) Uani 1 1 d . . . C25 C 0.7050(3) 0.5450(7) 0.0570(3) 0.0298(19) Uani 1 1 d . . . H25A H 0.7183 0.5925 0.0831 0.036 Uiso 1 1 calc R . . H25B H 0.6768 0.5952 0.0432 0.036 Uiso 1 1 calc R . . C26 C 0.7468(3) 0.5261(8) 0.0244(3) 0.0276(18) Uani 1 1 d . . . H26 H 0.7352 0.4606 0.0022 0.033 Uiso 1 1 calc R . . C27 C 0.7964(3) 0.4777(9) 0.0476(3) 0.037(2) Uani 1 1 d . . . H27A H 0.8121 0.5484 0.0646 0.055 Uiso 1 1 calc R . . H27B H 0.8193 0.4484 0.0257 0.055 Uiso 1 1 calc R . . H27C H 0.7892 0.4057 0.0670 0.055 Uiso 1 1 calc R . . C28 C 0.7547(3) 0.6592(8) 0.0007(3) 0.037(2) Uani 1 1 d . . . H28A H 0.7227 0.6884 -0.0131 0.055 Uiso 1 1 calc R . . H28B H 0.7792 0.6481 -0.0217 0.055 Uiso 1 1 calc R . . H28C H 0.7671 0.7237 0.0220 0.055 Uiso 1 1 calc R . . C29 C 0.6694(3) 0.1329(7) 0.1126(3) 0.0276(18) Uani 1 1 d . . . H29A H 0.6676 0.0845 0.1403 0.033 Uiso 1 1 calc R . . H29B H 0.7052 0.1516 0.1081 0.033 Uiso 1 1 calc R . . C30 C 0.6475(3) 0.0509(7) 0.0749(2) 0.0234(17) Uani 1 1 d . . . H30 H 0.6523 0.0989 0.0472 0.028 Uiso 1 1 calc R . . C31 C 0.5905(3) 0.0272(7) 0.0784(3) 0.0302(19) Uani 1 1 d . . . H31A H 0.5847 -0.0166 0.1059 0.045 Uiso 1 1 calc R . . H31B H 0.5780 -0.0269 0.0540 0.045 Uiso 1 1 calc R . . H31C H 0.5728 0.1102 0.0774 0.045 Uiso 1 1 calc R . . C32 C 0.6775(3) -0.0785(7) 0.0733(3) 0.0305(19) Uani 1 1 d . . . H32A H 0.6729 -0.1280 0.1000 0.046 Uiso 1 1 calc R . . H32B H 0.7132 -0.0596 0.0709 0.046 Uiso 1 1 calc R . . H32C H 0.6652 -0.1292 0.0480 0.046 Uiso 1 1 calc R . . C33 C 0.7154(3) 0.4407(9) 0.1949(3) 0.039(2) Uani 1 1 d . . . H33A H 0.6848 0.4885 0.2020 0.047 Uiso 1 1 calc R . . H33B H 0.7179 0.3621 0.2133 0.047 Uiso 1 1 calc R . . C34 C 0.7603(3) 0.5232(11) 0.2036(3) 0.052(3) Uani 1 1 d . . . H34 H 0.7543 0.6036 0.1860 0.063 Uiso 1 1 calc R . . C35 C 0.7658(3) 0.5668(10) 0.2512(3) 0.053(3) Uani 1 1 d . . . H35A H 0.7363 0.6175 0.2582 0.080 Uiso 1 1 calc R . . H35B H 0.7961 0.6200 0.2556 0.080 Uiso 1 1 calc R . . H35C H 0.7686 0.4908 0.2702 0.080 Uiso 1 1 calc R . . C36 C 0.8094(3) 0.4628(10) 0.1876(3) 0.050(3) Uani 1 1 d . . . H36A H 0.8380 0.5184 0.1963 0.075 Uiso 1 1 calc R . . H36B H 0.8068 0.4551 0.1558 0.075 Uiso 1 1 calc R . . H36C H 0.8144 0.3770 0.2006 0.075 Uiso 1 1 calc R . . C37 C 0.4568(3) 0.8333(7) 0.2159(2) 0.0261(17) Uani 1 1 d . . . H37A H 0.4442 0.9204 0.2229 0.031 Uiso 1 1 calc R . . H37B H 0.4913 0.8423 0.2057 0.031 Uiso 1 1 calc R . . C38 C 0.4574(3) 0.7464(7) 0.2566(2) 0.0242(17) Uani 1 1 d . . . H38 H 0.4786 0.7909 0.2800 0.029 Uiso 1 1 calc R . . C39 C 0.4820(3) 0.6122(8) 0.2487(3) 0.038(2) Uani 1 1 d . . . H39A H 0.4862 0.5654 0.2764 0.057 Uiso 1 1 calc R . . H39B H 0.5149 0.6248 0.2366 0.057 Uiso 1 1 calc R . . H39C H 0.4604 0.5621 0.2282 0.057 Uiso 1 1 calc R . . C40 C 0.4044(3) 0.7308(9) 0.2739(3) 0.043(2) Uani 1 1 d . . . H40A H 0.3898 0.8163 0.2784 0.064 Uiso 1 1 calc R . . H40B H 0.4068 0.6836 0.3016 0.064 Uiso 1 1 calc R . . H40C H 0.3831 0.6826 0.2526 0.064 Uiso 1 1 calc R . . C41 C 0.3776(3) 0.5622(7) 0.1264(3) 0.0294(19) Uani 1 1 d . . . H41A H 0.3942 0.5499 0.1558 0.035 Uiso 1 1 calc R . . H41B H 0.3903 0.4954 0.1068 0.035 Uiso 1 1 calc R . . C42 C 0.3205(3) 0.5498(8) 0.1288(3) 0.0310(19) Uani 1 1 d . . . H42 H 0.3045 0.5711 0.0995 0.037 Uiso 1 1 calc R . . C43 C 0.3081(3) 0.4053(8) 0.1396(3) 0.045(2) Uani 1 1 d . . . H43A H 0.3203 0.3490 0.1168 0.068 Uiso 1 1 calc R . . H43B H 0.2717 0.3950 0.1408 0.068 Uiso 1 1 calc R . . H43C H 0.3245 0.3818 0.1678 0.068 Uiso 1 1 calc R . . C44 C 0.2993(3) 0.6419(8) 0.1626(3) 0.044(2) Uani 1 1 d . . . H44A H 0.3146 0.6222 0.1916 0.067 Uiso 1 1 calc R . . H44B H 0.2628 0.6308 0.1628 0.067 Uiso 1 1 calc R . . H44C H 0.3070 0.7315 0.1549 0.067 Uiso 1 1 calc R . . C45 C 0.4460(3) 1.0053(7) 0.0864(3) 0.0266(18) Uani 1 1 d . . . H45A H 0.4475 0.9594 0.0582 0.032 Uiso 1 1 calc R . . H45B H 0.4807 1.0164 0.0989 0.032 Uiso 1 1 calc R . . C46 C 0.4209(3) 1.1382(8) 0.0793(3) 0.0296(18) Uani 1 1 d . . . H46 H 0.4178 1.1815 0.1081 0.035 Uiso 1 1 calc R . . C47 C 0.3678(3) 1.1225(9) 0.0564(3) 0.049(2) Uani 1 1 d . . . H47A H 0.3707 1.0813 0.0279 0.073 Uiso 1 1 calc R . . H47B H 0.3522 1.2077 0.0524 0.073 Uiso 1 1 calc R . . H47C H 0.3470 1.0686 0.0744 0.073 Uiso 1 1 calc R . . C48 C 0.4560(3) 1.2202(8) 0.0511(3) 0.045(2) Uani 1 1 d . . . H48A H 0.4896 1.2249 0.0657 0.068 Uiso 1 1 calc R . . H48B H 0.4423 1.3076 0.0474 0.068 Uiso 1 1 calc R . . H48C H 0.4583 1.1795 0.0224 0.068 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 0.01593(13) 0.01707(14) 0.01050(13) -0.00107(10) 0.00104(10) 0.00062(10) Re1 0.03242(17) 0.02068(16) 0.01184(15) -0.00311(12) 0.00070(12) 0.00957(13) Re2 0.02176(15) 0.02646(17) 0.02257(17) -0.00866(13) -0.00194(12) -0.00349(12) P1 0.0183(9) 0.0171(10) 0.0177(10) -0.0041(8) 0.0044(8) -0.0002(7) P2 0.0222(10) 0.0302(11) 0.0180(10) 0.0024(8) 0.0024(8) 0.0074(8) O1 0.024(3) 0.023(3) 0.025(3) 0.004(2) 0.007(2) -0.001(2) O2 0.023(3) 0.027(3) 0.013(3) 0.003(2) -0.001(2) -0.005(2) O3 0.026(3) 0.022(3) 0.014(3) -0.005(2) -0.003(2) 0.003(2) O4 0.042(3) 0.020(3) 0.018(3) -0.005(2) -0.001(2) 0.014(2) O5 0.096(5) 0.024(3) 0.028(3) 0.003(3) 0.007(3) -0.007(3) O6 0.039(3) 0.070(4) 0.028(3) 0.007(3) 0.009(3) 0.024(3) O7 0.023(3) 0.036(3) 0.029(3) -0.014(3) -0.005(2) 0.002(2) O8 0.028(3) 0.043(4) 0.066(5) -0.023(3) 0.003(3) 0.003(3) O9 0.090(6) 0.077(5) 0.029(4) 0.004(4) -0.012(4) -0.032(4) O10 0.029(3) 0.035(4) 0.087(5) -0.020(3) 0.005(3) -0.002(3) O11 0.017(2) 0.027(3) 0.016(3) -0.008(2) 0.001(2) 0.004(2) O12 0.026(3) 0.024(3) 0.014(3) -0.004(2) -0.001(2) 0.000(2) O13 0.020(3) 0.018(3) 0.033(3) 0.000(2) 0.005(2) 0.000(2) O14 0.027(3) 0.021(3) 0.013(3) -0.006(2) 0.003(2) 0.001(2) O15 0.021(3) 0.031(3) 0.021(3) -0.001(2) 0.002(2) 0.007(2) O16 0.033(3) 0.066(4) 0.036(4) 0.027(3) 0.014(3) 0.022(3) O17 0.030(3) 0.035(3) 0.029(3) -0.009(3) 0.006(3) 0.005(2) O18 0.026(3) 0.027(3) 0.026(3) 0.001(2) -0.004(2) 0.002(2) C1 0.042(5) 0.027(4) 0.017(4) 0.001(3) -0.002(4) -0.002(4) C2 0.025(4) 0.020(4) 0.028(4) 0.003(3) 0.004(3) 0.001(3) C3 0.049(5) 0.018(4) 0.041(5) 0.007(4) -0.010(4) -0.011(4) C4 0.031(4) 0.016(4) 0.046(5) -0.010(4) 0.007(4) -0.001(3) C5 0.021(4) 0.018(4) 0.022(4) -0.003(3) 0.000(3) -0.006(3) C6 0.019(4) 0.039(5) 0.031(5) 0.004(4) -0.002(3) -0.006(3) C7 0.023(4) 0.045(6) 0.063(7) -0.011(5) -0.004(4) 0.001(4) C8 0.037(5) 0.037(5) 0.046(6) 0.019(4) -0.013(4) -0.016(4) C9 0.043(5) 0.022(4) 0.013(4) -0.003(3) 0.004(3) -0.001(3) C10 0.030(4) 0.022(4) 0.019(4) 0.005(3) 0.008(3) 0.001(3) C11 0.035(5) 0.058(6) 0.018(4) 0.014(4) -0.006(4) -0.007(4) C12 0.067(6) 0.031(5) 0.021(5) 0.007(4) 0.000(4) -0.003(4) C13 0.035(5) 0.057(6) 0.035(5) 0.016(5) 0.007(4) 0.015(4) C14 0.030(4) 0.035(5) 0.028(5) 0.002(4) 0.005(4) 0.007(4) C15 0.052(6) 0.056(7) 0.082(9) -0.011(6) 0.000(6) 0.009(5) C16 0.057(6) 0.061(7) 0.041(6) 0.022(5) 0.016(5) 0.018(5) C17 0.032(5) 0.055(7) 0.103(10) -0.040(6) 0.020(6) -0.015(5) C18 0.028(6) 0.089(9) 0.173(15) -0.102(10) -0.007(7) 0.007(6) C19 0.180(15) 0.111(12) 0.148(14) -0.094(11) -0.137(13) 0.124(11) C20 0.032(5) 0.035(6) 0.100(9) -0.026(6) 0.005(5) -0.002(4) C21 0.020(4) 0.046(5) 0.022(4) 0.002(4) -0.003(3) 0.005(4) C22 0.032(5) 0.043(5) 0.032(5) 0.005(4) 0.000(4) -0.003(4) C23 0.024(4) 0.028(5) 0.051(6) -0.001(4) 0.001(4) -0.002(3) C24 0.047(6) 0.053(6) 0.031(5) -0.004(4) 0.002(4) -0.010(5) U2 0.01529(13) 0.01545(13) 0.01070(13) -0.00059(10) -0.00088(10) 0.00002(10) Re3 0.02222(15) 0.02370(17) 0.01733(16) -0.00536(12) -0.00517(12) 0.00423(12) Re4 0.01693(14) 0.01858(15) 0.01195(14) -0.00137(11) -0.00211(11) 0.00257(11) P3 0.0169(9) 0.0238(11) 0.0248(11) -0.0063(8) -0.0004(8) 0.0011(8) P4 0.0217(10) 0.0188(10) 0.0163(10) 0.0021(8) 0.0031(8) 0.0010(7) O19 0.025(3) 0.021(3) 0.018(3) 0.004(2) 0.002(2) 0.002(2) O20 0.028(3) 0.020(3) 0.023(3) 0.001(2) 0.003(2) -0.005(2) O21 0.024(3) 0.041(3) 0.024(3) -0.015(3) -0.005(2) 0.002(2) O22 0.038(4) 0.075(5) 0.044(4) 0.006(4) -0.001(3) -0.008(3) O23 0.049(4) 0.045(4) 0.030(3) 0.005(3) -0.007(3) 0.001(3) O24 0.058(4) 0.039(4) 0.056(4) -0.024(3) -0.026(3) 0.026(3) O25 0.023(3) 0.021(3) 0.015(3) -0.002(2) -0.003(2) 0.005(2) O26 0.022(3) 0.029(3) 0.017(3) -0.002(2) -0.005(2) 0.008(2) O27 0.036(3) 0.051(4) 0.029(3) -0.003(3) 0.005(3) -0.015(3) O28 0.050(4) 0.027(3) 0.015(3) 0.000(2) -0.002(3) 0.013(3) O29 0.020(3) 0.024(3) 0.017(3) 0.001(2) -0.002(2) 0.006(2) O30 0.057(4) 0.025(3) 0.059(4) 0.004(3) 0.032(3) 0.002(3) O31 0.025(3) 0.019(3) 0.038(3) 0.001(2) 0.003(2) 0.003(2) O32 0.043(4) 0.075(5) 0.052(4) -0.032(4) -0.026(3) 0.027(3) O33 0.022(3) 0.020(3) 0.029(3) -0.004(2) 0.000(2) 0.006(2) O34 0.033(3) 0.026(3) 0.016(3) 0.006(2) 0.002(2) -0.007(2) O35 0.035(3) 0.025(3) 0.019(3) 0.005(2) -0.004(2) -0.008(2) O36 0.026(3) 0.016(3) 0.027(3) 0.006(2) 0.007(2) 0.005(2) C25 0.026(4) 0.021(4) 0.043(5) -0.003(4) 0.007(4) -0.003(3) C26 0.018(4) 0.034(5) 0.031(5) 0.001(4) 0.005(3) 0.003(3) C27 0.031(5) 0.046(5) 0.034(5) 0.006(4) 0.015(4) 0.013(4) C28 0.037(5) 0.040(5) 0.034(5) 0.010(4) 0.013(4) 0.002(4) C29 0.025(4) 0.027(4) 0.030(5) 0.000(4) 0.000(3) 0.009(3) C30 0.025(4) 0.021(4) 0.024(4) 0.009(3) 0.005(3) 0.004(3) C31 0.028(4) 0.024(4) 0.038(5) -0.002(4) 0.002(4) -0.002(3) C32 0.033(5) 0.031(5) 0.028(5) 0.002(4) 0.005(4) 0.001(4) C33 0.032(5) 0.053(6) 0.032(5) -0.002(4) -0.006(4) -0.002(4) C34 0.027(5) 0.082(8) 0.050(6) -0.017(6) 0.010(4) 0.002(5) C35 0.040(6) 0.058(7) 0.059(7) -0.024(5) -0.015(5) 0.015(5) C36 0.031(5) 0.073(7) 0.045(6) 0.004(5) 0.011(4) 0.025(5) C37 0.030(4) 0.026(4) 0.022(4) -0.005(3) -0.002(3) -0.007(3) C38 0.034(4) 0.028(4) 0.011(4) -0.003(3) -0.002(3) 0.001(3) C39 0.044(5) 0.038(5) 0.032(5) 0.010(4) 0.007(4) 0.004(4) C40 0.042(5) 0.064(7) 0.023(5) 0.008(4) 0.007(4) 0.018(5) C41 0.039(5) 0.029(5) 0.020(4) -0.003(3) 0.008(4) -0.005(4) C42 0.026(4) 0.045(5) 0.023(4) -0.001(4) 0.002(3) -0.004(4) C43 0.049(6) 0.042(6) 0.045(6) -0.004(5) 0.002(5) -0.018(4) C44 0.043(5) 0.036(5) 0.057(6) -0.006(5) 0.023(5) 0.000(4) C45 0.033(4) 0.024(4) 0.023(4) 0.005(3) 0.005(3) -0.005(3) C46 0.036(5) 0.030(5) 0.022(4) 0.005(4) -0.002(4) -0.004(4) C47 0.050(6) 0.046(6) 0.050(6) 0.008(5) -0.003(5) 0.001(5) C48 0.044(5) 0.030(5) 0.060(7) 0.023(5) -0.004(5) -0.004(4) _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 1.757(5) . ? U1 O2 1.763(5) . ? U1 O7 2.327(5) . ? U1 O15 2.366(5) . ? U1 O11 2.376(4) . ? U1 O4 2.444(5) 3_666 ? U1 O3 2.464(5) . ? Re1 O6 1.691(5) . ? Re1 O5 1.707(6) . ? Re1 O4 1.741(5) . ? Re1 O3 1.745(5) . ? Re2 O9 1.695(6) . ? Re2 O8 1.698(5) . ? Re2 O10 1.707(6) . ? Re2 O7 1.754(5) . ? P1 O11 1.485(5) . ? P1 O14 1.544(5) . ? P1 O12 1.549(5) . ? P1 O13 1.562(5) . ? P2 O15 1.477(5) . ? P2 O18 1.542(5) . ? P2 O16 1.560(6) . ? P2 O17 1.562(6) . ? O4 U1 2.444(5) 3_666 ? O12 C1 1.472(8) . ? O13 C5 1.465(8) . ? O14 C9 1.463(8) . ? O16 C13 1.448(9) . ? O17 C17 1.461(10) . ? O18 C21 1.484(9) . ? C1 C2 1.502(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.526(10) . ? C2 C3 1.529(10) . ? C2 H2 0.9800 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.531(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.482(11) . ? C6 C8 1.534(10) . ? C6 H6 0.9800 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.516(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.511(10) . ? C10 C12 1.518(10) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.501(11) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.508(12) . ? C14 C16 1.545(11) . ? C14 H14 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.493(12) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.304(15) . ? C18 C20 1.520(12) . ? C18 H18 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.497(10) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.514(10) . ? C22 C24 1.533(11) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? U2 O19 1.758(5) . ? U2 O20 1.760(5) . ? U2 O21 2.349(5) . ? U2 O33 2.355(4) . ? U2 O29 2.391(4) . ? U2 O25 2.432(4) . ? U2 O26 2.447(5) 3_665 ? Re3 O23 1.704(6) . ? Re3 O24 1.709(5) . ? Re3 O22 1.718(6) . ? Re3 O21 1.758(5) . ? Re4 O28 1.697(5) . ? Re4 O27 1.715(5) . ? Re4 O26 1.738(5) . ? Re4 O25 1.752(5) . ? P3 O29 1.476(5) . ? P3 O32 1.518(6) . ? P3 O31 1.536(5) . ? P3 O30 1.571(6) . ? P4 O33 1.492(5) . ? P4 O34 1.547(5) . ? P4 O35 1.550(5) . ? P4 O36 1.556(5) . ? O26 U2 2.447(5) 3_665 ? O30 C25 1.477(9) . ? O31 C29 1.473(8) . ? O32 C33 1.472(10) . ? O34 C37 1.460(8) . ? O35 C41 1.475(8) . ? O36 C45 1.465(8) . ? C25 C26 1.519(10) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.519(10) . ? C26 C28 1.545(10) . ? C26 H26 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.496(10) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.516(10) . ? C30 C32 1.530(10) . ? C30 H30 0.9800 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.453(12) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.497(12) . ? C34 C36 1.524(11) . ? C34 H34 0.9800 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.509(10) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C40 1.514(10) . ? C38 C39 1.529(10) . ? C38 H38 0.9800 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.503(10) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C44 1.509(11) . ? C42 C43 1.538(11) . ? C42 H42 0.9800 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.508(10) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.525(11) . ? C46 C48 1.529(10) . ? C46 H46 0.9800 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 O2 177.5(2) . . ? O1 U1 O7 90.1(2) . . ? O2 U1 O7 92.4(2) . . ? O1 U1 O15 91.10(19) . . ? O2 U1 O15 89.55(19) . . ? O7 U1 O15 74.41(17) . . ? O1 U1 O11 91.00(19) . . ? O2 U1 O11 89.70(19) . . ? O7 U1 O11 74.09(16) . . ? O15 U1 O11 148.43(16) . . ? O1 U1 O4 87.3(2) . 3_666 ? O2 U1 O4 90.6(2) . 3_666 ? O7 U1 O4 147.20(17) . 3_666 ? O15 U1 O4 72.95(17) . 3_666 ? O11 U1 O4 138.61(16) . 3_666 ? O1 U1 O3 87.7(2) . . ? O2 U1 O3 90.28(19) . . ? O7 U1 O3 143.92(16) . . ? O15 U1 O3 141.62(16) . . ? O11 U1 O3 69.94(15) . . ? O4 U1 O3 68.67(16) 3_666 . ? O6 Re1 O5 109.1(3) . . ? O6 Re1 O4 109.0(3) . . ? O5 Re1 O4 109.6(3) . . ? O6 Re1 O3 109.6(2) . . ? O5 Re1 O3 108.8(3) . . ? O4 Re1 O3 110.7(2) . . ? O9 Re2 O8 109.7(3) . . ? O9 Re2 O10 108.7(4) . . ? O8 Re2 O10 107.7(3) . . ? O9 Re2 O7 109.7(3) . . ? O8 Re2 O7 109.9(3) . . ? O10 Re2 O7 111.1(3) . . ? O11 P1 O14 109.9(3) . . ? O11 P1 O12 115.0(3) . . ? O14 P1 O12 105.6(3) . . ? O11 P1 O13 111.9(3) . . ? O14 P1 O13 109.8(3) . . ? O12 P1 O13 104.2(3) . . ? O15 P2 O18 113.3(3) . . ? O15 P2 O16 112.9(3) . . ? O18 P2 O16 105.1(3) . . ? O15 P2 O17 114.4(3) . . ? O18 P2 O17 104.7(3) . . ? O16 P2 O17 105.5(3) . . ? Re1 O3 U1 138.2(2) . . ? Re1 O4 U1 150.6(3) . 3_666 ? Re2 O7 U1 170.2(3) . . ? P1 O11 U1 151.6(3) . . ? C1 O12 P1 121.9(4) . . ? C5 O13 P1 120.1(4) . . ? C9 O14 P1 122.4(4) . . ? P2 O15 U1 163.0(3) . . ? C13 O16 P2 121.0(5) . . ? C17 O17 P2 120.7(5) . . ? C21 O18 P2 120.1(4) . . ? O12 C1 C2 108.5(6) . . ? O12 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? O12 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? C1 C2 C4 111.8(6) . . ? C1 C2 C3 109.3(6) . . ? C4 C2 C3 110.6(6) . . ? C1 C2 H2 108.3 . . ? C4 C2 H2 108.3 . . ? C3 C2 H2 108.3 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O13 C5 C6 108.4(6) . . ? O13 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? O13 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? C7 C6 C5 111.8(7) . . ? C7 C6 C8 113.1(7) . . ? C5 C6 C8 107.1(6) . . ? C7 C6 H6 108.2 . . ? C5 C6 H6 108.2 . . ? C8 C6 H6 108.2 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O14 C9 C10 109.7(6) . . ? O14 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? O14 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C9 111.9(6) . . ? C11 C10 C12 111.6(6) . . ? C9 C10 C12 108.6(6) . . ? C11 C10 H10 108.2 . . ? C9 C10 H10 108.2 . . ? C12 C10 H10 108.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O16 C13 C14 109.1(7) . . ? O16 C13 H13A 109.9 . . ? C14 C13 H13A 109.9 . . ? O16 C13 H13B 109.9 . . ? C14 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? C13 C14 C15 114.2(8) . . ? C13 C14 C16 106.5(7) . . ? C15 C14 C16 110.2(8) . . ? C13 C14 H14 108.6 . . ? C15 C14 H14 108.6 . . ? C16 C14 H14 108.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O17 C17 C18 108.7(9) . . ? O17 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? O17 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C19 C18 C17 120.8(12) . . ? C19 C18 C20 118.2(11) . . ? C17 C18 C20 112.3(8) . . ? C19 C18 H18 99.9 . . ? C17 C18 H18 99.9 . . ? C20 C18 H18 99.9 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O18 C21 C22 110.3(6) . . ? O18 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? O18 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C21 C22 C23 111.4(7) . . ? C21 C22 C24 108.5(7) . . ? C23 C22 C24 111.6(7) . . ? C21 C22 H22 108.4 . . ? C23 C22 H22 108.4 . . ? C24 C22 H22 108.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O19 U2 O20 177.5(2) . . ? O19 U2 O21 92.2(2) . . ? O20 U2 O21 90.3(2) . . ? O19 U2 O33 89.00(19) . . ? O20 U2 O33 91.5(2) . . ? O21 U2 O33 72.42(17) . . ? O19 U2 O29 91.16(19) . . ? O20 U2 O29 89.86(19) . . ? O21 U2 O29 72.46(16) . . ? O33 U2 O29 144.86(17) . . ? O19 U2 O25 89.93(19) . . ? O20 U2 O25 88.15(19) . . ? O21 U2 O25 145.03(16) . . ? O33 U2 O25 142.54(16) . . ? O29 U2 O25 72.60(15) . . ? O19 U2 O26 89.97(19) . 3_665 ? O20 U2 O26 87.8(2) . 3_665 ? O21 U2 O26 144.83(16) . 3_665 ? O33 U2 O26 72.52(16) . 3_665 ? O29 U2 O26 142.61(15) . 3_665 ? O25 U2 O26 70.03(15) . 3_665 ? O23 Re3 O24 109.2(3) . . ? O23 Re3 O22 108.7(3) . . ? O24 Re3 O22 109.2(3) . . ? O23 Re3 O21 109.9(3) . . ? O24 Re3 O21 108.9(3) . . ? O22 Re3 O21 110.9(3) . . ? O28 Re4 O27 109.5(3) . . ? O28 Re4 O26 109.8(2) . . ? O27 Re4 O26 109.2(3) . . ? O28 Re4 O25 108.8(2) . . ? O27 Re4 O25 109.3(2) . . ? O26 Re4 O25 110.1(2) . . ? O29 P3 O32 114.9(3) . . ? O29 P3 O31 109.8(3) . . ? O32 P3 O31 112.1(4) . . ? O29 P3 O30 113.2(3) . . ? O32 P3 O30 102.0(4) . . ? O31 P3 O30 104.2(3) . . ? O33 P4 O34 115.4(3) . . ? O33 P4 O35 114.2(3) . . ? O34 P4 O35 102.9(3) . . ? O33 P4 O36 110.3(3) . . ? O34 P4 O36 107.5(3) . . ? O35 P4 O36 105.7(3) . . ? Re3 O21 U2 159.3(3) . . ? Re4 O25 U2 146.1(2) . . ? Re4 O26 U2 165.1(3) . 3_665 ? P3 O29 U2 146.9(3) . . ? C25 O30 P3 117.7(5) . . ? C29 O31 P3 125.5(5) . . ? C33 O32 P3 127.2(5) . . ? P4 O33 U2 147.7(3) . . ? C37 O34 P4 123.7(4) . . ? C41 O35 P4 123.5(5) . . ? C45 O36 P4 121.4(4) . . ? O30 C25 C26 107.4(6) . . ? O30 C25 H25A 110.2 . . ? C26 C25 H25A 110.2 . . ? O30 C25 H25B 110.2 . . ? C26 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? C25 C26 C27 111.8(7) . . ? C25 C26 C28 107.9(6) . . ? C27 C26 C28 111.2(6) . . ? C25 C26 H26 108.6 . . ? C27 C26 H26 108.6 . . ? C28 C26 H26 108.6 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O31 C29 C30 110.2(6) . . ? O31 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? O31 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C29 C30 C31 111.9(6) . . ? C29 C30 C32 108.9(6) . . ? C31 C30 C32 111.9(6) . . ? C29 C30 H30 108.0 . . ? C31 C30 H30 108.0 . . ? C32 C30 H30 108.0 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 O32 108.9(7) . . ? C34 C33 H33A 109.9 . . ? O32 C33 H33A 109.9 . . ? C34 C33 H33B 109.9 . . ? O32 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? C33 C34 C35 112.2(8) . . ? C33 C34 C36 113.4(8) . . ? C35 C34 C36 112.5(8) . . ? C33 C34 H34 106.0 . . ? C35 C34 H34 106.0 . . ? C36 C34 H34 106.0 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O34 C37 C38 108.2(6) . . ? O34 C37 H37A 110.1 . . ? C38 C37 H37A 110.1 . . ? O34 C37 H37B 110.1 . . ? C38 C37 H37B 110.1 . . ? H37A C37 H37B 108.4 . . ? C37 C38 C40 111.8(6) . . ? C37 C38 C39 112.2(6) . . ? C40 C38 C39 111.2(7) . . ? C37 C38 H38 107.1 . . ? C40 C38 H38 107.1 . . ? C39 C38 H38 107.1 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O35 C41 C42 108.3(6) . . ? O35 C41 H41A 110.0 . . ? C42 C41 H41A 110.0 . . ? O35 C41 H41B 110.0 . . ? C42 C41 H41B 110.0 . . ? H41A C41 H41B 108.4 . . ? C41 C42 C44 112.5(7) . . ? C41 C42 C43 108.2(7) . . ? C44 C42 C43 110.9(7) . . ? C41 C42 H42 108.4 . . ? C44 C42 H42 108.4 . . ? C43 C42 H42 108.4 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O36 C45 C46 108.5(6) . . ? O36 C45 H45A 110.0 . . ? C46 C45 H45A 110.0 . . ? O36 C45 H45B 110.0 . . ? C46 C45 H45B 110.0 . . ? H45A C45 H45B 108.4 . . ? C45 C46 C47 110.4(7) . . ? C45 C46 C48 107.2(6) . . ? C47 C46 C48 111.4(7) . . ? C45 C46 H46 109.3 . . ? C47 C46 H46 109.3 . . ? C48 C46 H46 109.3 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Re1 O3 U1 103.8(4) . . . . ? O5 Re1 O3 U1 -15.4(4) . . . . ? O4 Re1 O3 U1 -135.9(3) . . . . ? O1 U1 O3 Re1 44.8(4) . . . . ? O2 U1 O3 Re1 -136.6(4) . . . . ? O7 U1 O3 Re1 -42.2(5) . . . . ? O15 U1 O3 Re1 133.7(3) . . . . ? O11 U1 O3 Re1 -47.1(3) . . . . ? O4 U1 O3 Re1 132.9(4) 3_666 . . . ? O6 Re1 O4 U1 119.8(6) . . . 3_666 ? O5 Re1 O4 U1 -120.8(6) . . . 3_666 ? O3 Re1 O4 U1 -0.8(6) . . . 3_666 ? O9 Re2 O7 U1 -168.1(16) . . . . ? O8 Re2 O7 U1 71.2(16) . . . . ? O10 Re2 O7 U1 -47.9(17) . . . . ? O1 U1 O7 Re2 -15.7(16) . . . . ? O2 U1 O7 Re2 164.4(16) . . . . ? O15 U1 O7 Re2 -106.8(16) . . . . ? O11 U1 O7 Re2 75.3(16) . . . . ? O4 U1 O7 Re2 -100.9(16) 3_666 . . . ? O3 U1 O7 Re2 70.6(17) . . . . ? O14 P1 O11 U1 -10.0(7) . . . . ? O12 P1 O11 U1 -129.0(6) . . . . ? O13 P1 O11 U1 112.3(6) . . . . ? O1 U1 O11 P1 127.2(6) . . . . ? O2 U1 O11 P1 -55.2(6) . . . . ? O7 U1 O11 P1 37.4(6) . . . . ? O15 U1 O11 P1 33.4(8) . . . . ? O4 U1 O11 P1 -145.7(5) 3_666 . . . ? O3 U1 O11 P1 -145.6(6) . . . . ? O11 P1 O12 C1 -62.2(6) . . . . ? O14 P1 O12 C1 176.5(5) . . . . ? O13 P1 O12 C1 60.7(6) . . . . ? O11 P1 O13 C5 -43.3(6) . . . . ? O14 P1 O13 C5 79.0(5) . . . . ? O12 P1 O13 C5 -168.2(5) . . . . ? O11 P1 O14 C9 -166.1(5) . . . . ? O12 P1 O14 C9 -41.5(6) . . . . ? O13 P1 O14 C9 70.3(5) . . . . ? O18 P2 O15 U1 175.4(10) . . . . ? O16 P2 O15 U1 -65.2(12) . . . . ? O17 P2 O15 U1 55.5(12) . . . . ? O1 U1 O15 P2 70.6(11) . . . . ? O2 U1 O15 P2 -107.0(11) . . . . ? O7 U1 O15 P2 160.4(11) . . . . ? O11 U1 O15 P2 164.3(9) . . . . ? O4 U1 O15 P2 -16.2(11) 3_666 . . . ? O3 U1 O15 P2 -17.1(12) . . . . ? O15 P2 O16 C13 34.3(8) . . . . ? O18 P2 O16 C13 158.3(6) . . . . ? O17 P2 O16 C13 -91.3(7) . . . . ? O15 P2 O17 C17 51.8(7) . . . . ? O18 P2 O17 C17 -72.9(7) . . . . ? O16 P2 O17 C17 176.4(7) . . . . ? O15 P2 O18 C21 46.6(6) . . . . ? O16 P2 O18 C21 -77.2(5) . . . . ? O17 P2 O18 C21 171.9(5) . . . . ? P1 O12 C1 C2 178.2(5) . . . . ? O12 C1 C2 C4 62.3(8) . . . . ? O12 C1 C2 C3 -174.9(6) . . . . ? P1 O13 C5 C6 -169.6(5) . . . . ? O13 C5 C6 C7 -54.8(8) . . . . ? O13 C5 C6 C8 -179.2(6) . . . . ? P1 O14 C9 C10 -137.9(5) . . . . ? O14 C9 C10 C11 71.3(8) . . . . ? O14 C9 C10 C12 -165.1(6) . . . . ? P2 O16 C13 C14 -169.2(6) . . . . ? O16 C13 C14 C15 60.0(10) . . . . ? O16 C13 C14 C16 -178.2(7) . . . . ? P2 O17 C17 C18 -167.9(7) . . . . ? O17 C17 C18 C19 81.9(17) . . . . ? O17 C17 C18 C20 -65.2(15) . . . . ? P2 O18 C21 C22 145.9(5) . . . . ? O18 C21 C22 C23 -65.4(9) . . . . ? O18 C21 C22 C24 171.3(6) . . . . ? O23 Re3 O21 U2 -88.5(9) . . . . ? O24 Re3 O21 U2 152.0(8) . . . . ? O22 Re3 O21 U2 31.8(9) . . . . ? O19 U2 O21 Re3 115.8(9) . . . . ? O20 U2 O21 Re3 -64.5(9) . . . . ? O33 U2 O21 Re3 -156.0(9) . . . . ? O29 U2 O21 Re3 25.3(8) . . . . ? O25 U2 O21 Re3 22.8(11) . . . . ? O26 U2 O21 Re3 -151.1(7) 3_665 . . . ? O28 Re4 O25 U2 171.6(4) . . . . ? O27 Re4 O25 U2 52.0(5) . . . . ? O26 Re4 O25 U2 -68.0(5) . . . . ? O19 U2 O25 Re4 152.7(5) . . . . ? O20 U2 O25 Re4 -25.6(5) . . . . ? O21 U2 O25 Re4 -113.6(5) . . . . ? O33 U2 O25 Re4 64.4(5) . . . . ? O29 U2 O25 Re4 -116.1(5) . . . . ? O26 U2 O25 Re4 62.7(4) 3_665 . . . ? O28 Re4 O26 U2 -22.5(11) . . . 3_665 ? O27 Re4 O26 U2 97.6(11) . . . 3_665 ? O25 Re4 O26 U2 -142.3(10) . . . 3_665 ? O32 P3 O29 U2 172.3(5) . . . . ? O31 P3 O29 U2 -60.3(6) . . . . ? O30 P3 O29 U2 55.6(6) . . . . ? O19 U2 O29 P3 91.4(5) . . . . ? O20 U2 O29 P3 -86.3(6) . . . . ? O21 U2 O29 P3 -176.7(6) . . . . ? O33 U2 O29 P3 -178.7(4) . . . . ? O25 U2 O29 P3 1.8(5) . . . . ? O26 U2 O29 P3 -0.1(7) 3_665 . . . ? O29 P3 O30 C25 50.2(7) . . . . ? O32 P3 O30 C25 -73.8(6) . . . . ? O31 P3 O30 C25 169.4(5) . . . . ? O29 P3 O31 C29 -172.5(5) . . . . ? O32 P3 O31 C29 -43.6(7) . . . . ? O30 P3 O31 C29 65.9(6) . . . . ? O29 P3 O32 C33 33.8(9) . . . . ? O31 P3 O32 C33 -92.4(8) . . . . ? O30 P3 O32 C33 156.7(7) . . . . ? O34 P4 O33 U2 78.4(6) . . . . ? O35 P4 O33 U2 -40.6(7) . . . . ? O36 P4 O33 U2 -159.5(5) . . . . ? O19 U2 O33 P4 -21.0(6) . . . . ? O20 U2 O33 P4 156.5(6) . . . . ? O21 U2 O33 P4 -113.7(6) . . . . ? O29 U2 O33 P4 -111.6(6) . . . . ? O25 U2 O33 P4 67.5(7) . . . . ? O26 U2 O33 P4 69.2(6) 3_665 . . . ? O33 P4 O34 C37 50.6(6) . . . . ? O35 P4 O34 C37 175.6(5) . . . . ? O36 P4 O34 C37 -73.1(6) . . . . ? O33 P4 O35 C41 81.8(6) . . . . ? O34 P4 O35 C41 -44.0(6) . . . . ? O36 P4 O35 C41 -156.7(5) . . . . ? O33 P4 O36 C45 11.8(6) . . . . ? O34 P4 O36 C45 138.5(5) . . . . ? O35 P4 O36 C45 -112.1(5) . . . . ? P3 O30 C25 C26 152.4(5) . . . . ? O30 C25 C26 C27 -73.6(8) . . . . ? O30 C25 C26 C28 163.8(7) . . . . ? P3 O31 C29 C30 -127.4(6) . . . . ? O31 C29 C30 C31 -55.0(8) . . . . ? O31 C29 C30 C32 -179.3(6) . . . . ? P3 O32 C33 C34 -139.4(8) . . . . ? O32 C33 C34 C35 179.4(8) . . . . ? O32 C33 C34 C36 -51.9(11) . . . . ? P4 O34 C37 C38 -149.3(5) . . . . ? O34 C37 C38 C40 -60.2(8) . . . . ? O34 C37 C38 C39 65.4(8) . . . . ? P4 O35 C41 C42 133.3(6) . . . . ? O35 C41 C42 C44 -65.6(9) . . . . ? O35 C41 C42 C43 171.5(6) . . . . ? P4 O36 C45 C46 179.6(5) . . . . ? O36 C45 C46 C47 -63.9(8) . . . . ? O36 C45 C46 C48 174.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.183 _refine_diff_density_min -1.251 _refine_diff_density_rms 0.201 data_s1082abs _database_code_depnum_ccdc_archive 'CCDC 623015' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H108 Cl8 O24 P4 Re4 U2' _chemical_formula_weight 2721.70 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' Re Re -1.0185 7.2310 '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' _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 15.002(3) _cell_length_b 16.580(3) _cell_length_c 17.205(3) _cell_angle_alpha 83.219(3) _cell_angle_beta 86.142(3) _cell_angle_gamma 78.133(3) _cell_volume 4154.6(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6987 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.24 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 10.084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1871 _exptl_absorpt_correction_T_max 0.4321 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46219 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0830 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.42 _reflns_number_total 18983 _reflns_number_gt 14562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+171.2372P] 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 18983 _refine_ls_number_parameters 825 _refine_ls_number_restraints 906 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.1876 _refine_ls_wR_factor_gt 0.1729 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.014 _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 0.30206(3) 0.14175(3) 0.47681(3) 0.01122(11) Uani 1 1 d U . . Re1 Re 0.55793(4) 0.09194(4) 0.56111(3) 0.01584(13) Uani 1 1 d U . . Re2 Re 0.08186(4) 0.32186(4) 0.43827(3) 0.01534(13) Uani 1 1 d U . . P1 P 0.1952(2) 0.0724(2) 0.3189(2) 0.0137(7) Uani 1 1 d U . . P2 P 0.3353(2) 0.3291(2) 0.56283(19) 0.0119(7) Uani 1 1 d U . . O1 O 0.2366(7) 0.0698(6) 0.3976(5) 0.0162(18) Uani 1 1 d U . . O2 O 0.2939(6) 0.2586(6) 0.5421(5) 0.0146(18) Uani 1 1 d U . . O3 O 0.4429(7) 0.1259(8) 0.5465(7) 0.033(3) Uani 1 1 d U . . O4 O 0.5763(8) 0.1033(8) 0.6558(7) 0.030(3) Uani 1 1 d U . . O5 O 0.6173(11) 0.1519(10) 0.5004(10) 0.057(4) Uani 1 1 d U . . O6 O 0.5916(8) -0.0116(8) 0.5450(8) 0.037(3) Uani 1 1 d U . . O7 O 0.1601(7) 0.2269(7) 0.4460(7) 0.026(2) Uani 1 1 d U . . O8 O 0.1376(8) 0.4013(8) 0.4155(6) 0.027(2) Uani 1 1 d U . . O9 O 0.0216(8) 0.3347(8) 0.5248(7) 0.030(3) Uani 1 1 d U . . O10 O 0.0080(7) 0.3212(7) 0.3647(6) 0.023(2) Uani 1 1 d U . . O11 O 0.2538(8) 0.0911(6) 0.5601(5) 0.019(2) Uani 1 1 d U . . O12 O 0.3532(8) 0.1890(8) 0.3941(6) 0.028(2) Uani 1 1 d U . . C1 C 0.2508(10) 0.1323(9) 0.2442(8) 0.015(2) Uani 1 1 d U . . H1A H 0.2158 0.1414 0.1961 0.018 Uiso 1 1 calc R . . H1B H 0.2498 0.1872 0.2618 0.018 Uiso 1 1 calc R . . C2 C 0.3512(11) 0.0914(10) 0.2238(8) 0.022(3) Uani 1 1 d U . . H2A H 0.3822 0.0685 0.2730 0.026 Uiso 1 1 calc R . . H2B H 0.3515 0.0445 0.1929 0.026 Uiso 1 1 calc R . . C3 C 0.4041(12) 0.1505(11) 0.1780(10) 0.027(3) Uani 1 1 d U . . H3A H 0.4680 0.1211 0.1701 0.033 Uiso 1 1 calc R . . H3B H 0.4047 0.1966 0.2096 0.033 Uiso 1 1 calc R . . C4 C 0.3669(12) 0.1871(11) 0.0979(9) 0.027(3) Uani 1 1 d U . . H4A H 0.3595 0.1422 0.0682 0.040 Uiso 1 1 calc R . . H4B H 0.4097 0.2184 0.0691 0.040 Uiso 1 1 calc R . . H4C H 0.3078 0.2242 0.1052 0.040 Uiso 1 1 calc R . . C5 C 0.2072(10) -0.0319(9) 0.2947(8) 0.017(3) Uani 1 1 d U . . H5A H 0.2728 -0.0575 0.2911 0.021 Uiso 1 1 calc R . . H5B H 0.1782 -0.0643 0.3375 0.021 Uiso 1 1 calc R . . C6 C 0.1644(11) -0.0368(9) 0.2176(7) 0.017(3) Uani 1 1 d U . . H6A H 0.0972 -0.0246 0.2254 0.020 Uiso 1 1 calc R . . H6B H 0.1815 0.0062 0.1777 0.020 Uiso 1 1 calc R . . C7 C 0.1942(11) -0.1212(10) 0.1870(9) 0.022(3) Uani 1 1 d U . . H7A H 0.2614 -0.1343 0.1795 0.026 Uiso 1 1 calc R . . H7B H 0.1756 -0.1644 0.2257 0.026 Uiso 1 1 calc R . . C8 C 0.1512(12) -0.1210(10) 0.1099(8) 0.023(3) Uani 1 1 d U . . H8A H 0.0847 -0.1050 0.1167 0.034 Uiso 1 1 calc R . . H8B H 0.1674 -0.1765 0.0925 0.034 Uiso 1 1 calc R . . H8C H 0.1735 -0.0813 0.0705 0.034 Uiso 1 1 calc R . . C9 C 0.0753(9) 0.1200(9) 0.3205(8) 0.015(2) Uani 1 1 d U . . H9A H 0.0686 0.1806 0.3205 0.018 Uiso 1 1 calc R . . H9B H 0.0484 0.1098 0.2725 0.018 Uiso 1 1 calc R . . C10 C 0.0240(10) 0.0863(10) 0.3917(9) 0.021(3) Uani 1 1 d U . . H10A H 0.0497 0.0978 0.4398 0.025 Uiso 1 1 calc R . . H10B H 0.0318 0.0255 0.3925 0.025 Uiso 1 1 calc R . . C11 C -0.0777(11) 0.1257(11) 0.3910(10) 0.026(3) Uani 1 1 d U . . H11A H -0.1035 0.1122 0.3437 0.031 Uiso 1 1 calc R . . H11B H -0.0849 0.1867 0.3875 0.031 Uiso 1 1 calc R . . C12 C -0.1318(10) 0.0962(11) 0.4638(9) 0.024(3) Uani 1 1 d U . . H12A H -0.1493 0.0441 0.4559 0.036 Uiso 1 1 calc R . . H12B H -0.1868 0.1383 0.4725 0.036 Uiso 1 1 calc R . . H12C H -0.0940 0.0875 0.5095 0.036 Uiso 1 1 calc R . . C13 C 0.2482(9) 0.4184(9) 0.5742(8) 0.014(2) Uani 1 1 d U . . H13A H 0.2762 0.4631 0.5893 0.017 Uiso 1 1 calc R . . H13B H 0.2200 0.4381 0.5233 0.017 Uiso 1 1 calc R . . C14 C 0.1737(9) 0.4023(9) 0.6359(8) 0.014(3) Uani 1 1 d U . . H14A H 0.1528 0.3517 0.6262 0.017 Uiso 1 1 calc R . . H14B H 0.1994 0.3925 0.6885 0.017 Uiso 1 1 calc R . . C15 C 0.0932(10) 0.4742(10) 0.6344(9) 0.021(3) Uani 1 1 d U . . H15A H 0.0671 0.4834 0.5819 0.025 Uiso 1 1 calc R . . H15B H 0.1144 0.5250 0.6432 0.025 Uiso 1 1 calc R . . C16 C 0.0178(11) 0.4589(11) 0.6975(9) 0.030(4) Uani 1 1 d U . . H16A H -0.0076 0.4120 0.6860 0.045 Uiso 1 1 calc R . . H16B H -0.0306 0.5086 0.6972 0.045 Uiso 1 1 calc R . . H16C H 0.0442 0.4466 0.7492 0.045 Uiso 1 1 calc R . . C17 C 0.3954(9) 0.3012(9) 0.6516(8) 0.015(3) Uani 1 1 d U . . H17A H 0.3507 0.2927 0.6952 0.018 Uiso 1 1 calc R . . H17B H 0.4378 0.2475 0.6474 0.018 Uiso 1 1 calc R . . C18 C 0.4493(10) 0.3624(10) 0.6729(8) 0.018(3) Uani 1 1 d U . . H18A H 0.4069 0.4146 0.6830 0.022 Uiso 1 1 calc R . . H18B H 0.4909 0.3751 0.6280 0.022 Uiso 1 1 calc R . . C19 C 0.5059(10) 0.3292(10) 0.7458(8) 0.020(3) Uani 1 1 d U . . H19A H 0.4640 0.3193 0.7913 0.024 Uiso 1 1 calc R . . H19B H 0.5458 0.2754 0.7367 0.024 Uiso 1 1 calc R . . C20 C 0.5643(12) 0.3885(12) 0.7651(9) 0.029(4) Uani 1 1 d U . . H20A H 0.6059 0.3986 0.7203 0.044 Uiso 1 1 calc R . . H20B H 0.5998 0.3641 0.8110 0.044 Uiso 1 1 calc R . . H20C H 0.5249 0.4411 0.7766 0.044 Uiso 1 1 calc R . . C21 C 0.4178(9) 0.3541(9) 0.4889(8) 0.016(2) Uani 1 1 d U . . H21A H 0.4456 0.3979 0.5061 0.019 Uiso 1 1 calc R . . H21B H 0.4667 0.3044 0.4851 0.019 Uiso 1 1 calc R . . C22 C 0.3828(10) 0.3834(10) 0.4081(8) 0.020(3) Uani 1 1 d U . . H22A H 0.3382 0.4363 0.4098 0.024 Uiso 1 1 calc R . . H22B H 0.3508 0.3420 0.3916 0.024 Uiso 1 1 calc R . . C23 C 0.4602(10) 0.3961(10) 0.3475(8) 0.019(3) Uani 1 1 d U . . H23A H 0.4332 0.4223 0.2974 0.023 Uiso 1 1 calc R . . H23B H 0.4943 0.4348 0.3660 0.023 Uiso 1 1 calc R . . C24 C 0.5261(12) 0.3170(11) 0.3326(10) 0.031(4) Uani 1 1 d U . . H24A H 0.5607 0.2955 0.3795 0.047 Uiso 1 1 calc R . . H24B H 0.5682 0.3283 0.2885 0.047 Uiso 1 1 calc R . . H24C H 0.4922 0.2760 0.3201 0.047 Uiso 1 1 calc R . . U2 U 0.87409(3) 0.84559(3) 0.01985(3) 0.01123(10) Uani 1 1 d U . . Re3 Re 0.77870(4) 0.64151(4) 0.08727(3) 0.01521(13) Uani 1 1 d U . . Re4 Re 0.90823(3) 1.06610(3) 0.09885(3) 0.01122(12) Uani 1 1 d U . . P3 P 1.0145(2) 0.6724(2) -0.0812(2) 0.0138(7) Uani 1 1 d U . . P4 P 0.6991(2) 0.8960(2) 0.17965(19) 0.0118(7) Uani 1 1 d U . . O13 O 0.9508(7) 0.7526(6) -0.0624(6) 0.0181(19) Uani 1 1 d U . . O14 O 0.7487(6) 0.8864(7) 0.1003(5) 0.0168(19) Uani 1 1 d U . . O15 O 0.7921(7) 0.7340(7) 0.0320(6) 0.022(2) Uani 1 1 d U . . O16 O 0.7231(8) 0.6622(8) 0.1753(6) 0.030(3) Uani 1 1 d U . . O17 O 0.7165(10) 0.5916(9) 0.0370(8) 0.041(3) Uani 1 1 d U . . O18 O 0.8820(9) 0.5793(8) 0.1038(8) 0.038(3) Uani 1 1 d U . . O19 O 0.8884(7) 0.9756(6) 0.0694(5) 0.0172(19) Uani 1 1 d U . . O20 O 0.8107(7) 1.1400(7) 0.0947(6) 0.024(2) Uani 1 1 d U . . O21 O 0.9396(8) 1.0485(7) 0.1933(6) 0.025(2) Uani 1 1 d U . . O22 O 0.9938(8) 1.1022(7) 0.0403(6) 0.027(2) Uani 1 1 d U . . O23 O 0.8100(6) 0.8993(6) -0.0600(6) 0.0167(19) Uani 1 1 d U . . O24 O 0.9387(7) 0.7931(6) 0.0993(6) 0.0173(19) Uani 1 1 d U . . C25 C 1.0875(10) 0.6940(9) -0.1662(8) 0.016(3) Uiso 1 1 d U . . H25A H 1.0494 0.7143 -0.2120 0.019 Uiso 1 1 calc R . . H25B H 1.1190 0.7386 -0.1566 0.019 Uiso 1 1 calc R . . C26 C 1.1587(10) 0.6177(9) -0.1852(8) 0.018(3) Uani 1 1 d U . . H26A H 1.1989 0.5987 -0.1405 0.022 Uiso 1 1 calc R . . H26B H 1.1278 0.5723 -0.1932 0.022 Uiso 1 1 calc R . . C27 C 1.2153(10) 0.6379(9) -0.2580(9) 0.020(3) Uiso 1 1 d U . . H27A H 1.2437 0.6851 -0.2504 0.024 Uiso 1 1 calc R . . H27B H 1.1749 0.6554 -0.3026 0.024 Uiso 1 1 calc R . . C28 C 1.2901(11) 0.5648(11) -0.2781(10) 0.027(4) Uani 1 1 d U . . H28A H 1.3379 0.5552 -0.2400 0.041 Uiso 1 1 calc R . . H28B H 1.3164 0.5772 -0.3308 0.041 Uiso 1 1 calc R . . H28C H 1.2640 0.5150 -0.2765 0.041 Uiso 1 1 calc R . . C29 C 0.9507(11) 0.5980(9) -0.1015(8) 0.020(3) Uani 1 1 d U . . H29A H 0.9935 0.5498 -0.1205 0.023 Uiso 1 1 calc R . . H29B H 0.9205 0.5782 -0.0521 0.023 Uiso 1 1 calc R . . C30 C 0.8777(10) 0.6312(10) -0.1626(8) 0.021(3) Uani 1 1 d U . . H30A H 0.8420 0.6854 -0.1492 0.026 Uiso 1 1 calc R . . H30B H 0.9082 0.6403 -0.2148 0.026 Uiso 1 1 calc R . . C31 C 0.8147(11) 0.5734(11) -0.1662(9) 0.024(3) Uani 1 1 d U . . H31A H 0.7809 0.5680 -0.1151 0.029 Uiso 1 1 calc R . . H31B H 0.8511 0.5180 -0.1750 0.029 Uiso 1 1 calc R . . C32 C 0.7461(11) 0.6009(13) -0.2307(11) 0.036(4) Uani 1 1 d U . . H32A H 0.7070 0.6541 -0.2207 0.054 Uiso 1 1 calc R . . H32B H 0.7084 0.5592 -0.2310 0.054 Uiso 1 1 calc R . . H32C H 0.7788 0.6071 -0.2815 0.054 Uiso 1 1 calc R . . C33 C 1.0837(10) 0.6269(9) -0.0004(8) 0.019(3) Uani 1 1 d U . . H33A H 1.0436 0.6170 0.0464 0.022 Uiso 1 1 calc R . . H33B H 1.1197 0.5724 -0.0127 0.022 Uiso 1 1 calc R . . C34 C 1.1490(10) 0.6809(9) 0.0190(7) 0.016(3) Uani 1 1 d U . . H34A H 1.1933 0.6856 -0.0258 0.019 Uiso 1 1 calc R . . H34B H 1.1136 0.7372 0.0255 0.019 Uiso 1 1 calc R . . C35 C 1.2012(11) 0.6474(9) 0.0930(8) 0.019(3) Uani 1 1 d U . . H35A H 1.2515 0.6774 0.0953 0.022 Uiso 1 1 calc R . . H35B H 1.2284 0.5880 0.0907 0.022 Uiso 1 1 calc R . . C36 C 1.1387(12) 0.6573(11) 0.1681(8) 0.026(3) Uani 1 1 d U . . H36A H 1.1134 0.7162 0.1717 0.040 Uiso 1 1 calc R . . H36B H 1.1742 0.6342 0.2142 0.040 Uiso 1 1 calc R . . H36C H 1.0888 0.6277 0.1661 0.040 Uiso 1 1 calc R . . C37 C 0.5944(10) 0.8620(9) 0.1792(8) 0.016(3) Uani 1 1 d U . . H37A H 0.6076 0.8017 0.1747 0.020 Uiso 1 1 calc R . . H37B H 0.5605 0.8711 0.2298 0.020 Uiso 1 1 calc R . . C38 C 0.5331(10) 0.9064(9) 0.1121(8) 0.017(3) Uiso 1 1 d U . . H38A H 0.5116 0.9651 0.1215 0.020 Uiso 1 1 calc R . . H38B H 0.5701 0.9053 0.0623 0.020 Uiso 1 1 calc R . . C39 C 0.4520(12) 0.8690(11) 0.1036(10) 0.028(3) Uani 1 1 d U . . H39A H 0.4137 0.8717 0.1527 0.034 Uiso 1 1 calc R . . H39B H 0.4731 0.8099 0.0955 0.034 Uiso 1 1 calc R . . C40 C 0.3944(13) 0.9125(13) 0.0357(11) 0.037(4) Uani 1 1 d U . . H40A H 0.3645 0.9682 0.0476 0.056 Uiso 1 1 calc R . . H40B H 0.3481 0.8807 0.0276 0.056 Uiso 1 1 calc R . . H40C H 0.4336 0.9166 -0.0120 0.056 Uiso 1 1 calc R . . C41 C 0.6732(9) 1.0025(9) 0.1980(8) 0.017(3) Uani 1 1 d U . . H41A H 0.7312 1.0217 0.2001 0.020 Uiso 1 1 calc R . . H41B H 0.6397 1.0356 0.1534 0.020 Uiso 1 1 calc R . . C42 C 0.6166(9) 1.0193(9) 0.2736(8) 0.015(3) Uani 1 1 d U . . H42A H 0.6438 0.9786 0.3167 0.018 Uiso 1 1 calc R . . H42B H 0.5543 1.0105 0.2675 0.018 Uiso 1 1 calc R . . C43 C 0.6098(11) 1.1070(10) 0.2970(9) 0.023(3) Uani 1 1 d U . . H43A H 0.5823 1.1479 0.2542 0.028 Uiso 1 1 calc R . . H43B H 0.5687 1.1140 0.3442 0.028 Uiso 1 1 calc R . . C44 C 0.7012(11) 1.1250(11) 0.3137(9) 0.025(3) Uani 1 1 d U . . H44A H 0.7292 1.0844 0.3556 0.037 Uiso 1 1 calc R . . H44B H 0.6924 1.1809 0.3301 0.037 Uiso 1 1 calc R . . H44C H 0.7411 1.1216 0.2662 0.037 Uiso 1 1 calc R . . C45 C 0.7646(9) 0.8364(9) 0.2571(8) 0.015(2) Uani 1 1 d U . . H45A H 0.7253 0.8350 0.3056 0.018 Uiso 1 1 calc R . . H45B H 0.7848 0.7788 0.2439 0.018 Uiso 1 1 calc R . . C46 C 0.8494(9) 0.8709(9) 0.2729(8) 0.016(3) Uani 1 1 d U . . H46A H 0.8812 0.8849 0.2224 0.020 Uiso 1 1 calc R . . H46B H 0.8293 0.9225 0.2983 0.020 Uiso 1 1 calc R . . C47 C 0.9156(10) 0.8097(10) 0.3248(9) 0.020(3) Uani 1 1 d U . . H47A H 0.9437 0.7622 0.2954 0.024 Uiso 1 1 calc R . . H47B H 0.8813 0.7881 0.3711 0.024 Uiso 1 1 calc R . . C48 C 0.9911(12) 0.8473(13) 0.3526(12) 0.038(4) Uani 1 1 d U . . H48A H 1.0248 0.8695 0.3071 0.057 Uiso 1 1 calc R . . H48B H 1.0328 0.8044 0.3840 0.057 Uiso 1 1 calc R . . H48C H 0.9640 0.8921 0.3845 0.057 Uiso 1 1 calc R . . C49 C 0.2511(10) 0.6537(10) 0.4438(8) 0.021(3) Uani 1 1 d U . . Cl1 Cl 0.3574(3) 0.5962(3) 0.4778(2) 0.0307(9) Uani 1 1 d U . . Cl2 Cl 0.1990(3) 0.5910(3) 0.3947(2) 0.0336(9) Uani 1 1 d U . . Cl3 Cl 0.1810(3) 0.6838(3) 0.5265(2) 0.0345(10) Uani 1 1 d U . . Cl4 Cl 0.2699(4) 0.7412(3) 0.3833(3) 0.0487(13) Uani 1 1 d U . . C50 C 0.5614(11) 0.3636(10) 0.0647(9) 0.023(3) Uani 1 1 d U . . Cl5 Cl 0.4608(3) 0.3872(3) 0.1241(2) 0.0340(10) Uani 1 1 d U . . Cl6 Cl 0.5324(3) 0.3448(3) -0.0274(2) 0.0371(10) Uani 1 1 d U . . Cl7 Cl 0.6335(3) 0.2749(3) 0.1082(3) 0.0392(10) Uani 1 1 d U . . Cl8 Cl 0.6166(3) 0.4485(3) 0.0540(3) 0.0310(9) Uani 1 1 d U . . 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 0.0101(2) 0.0179(3) 0.0064(2) -0.00712(18) 0.00107(16) -0.00155(18) Re1 0.0122(3) 0.0238(3) 0.0126(3) -0.0118(2) -0.00119(19) -0.0003(2) Re2 0.0131(3) 0.0194(3) 0.0136(3) -0.0063(2) -0.00079(19) -0.0008(2) P1 0.0141(16) 0.0196(19) 0.0082(15) -0.0054(13) 0.0002(12) -0.0034(14) P2 0.0123(16) 0.0156(18) 0.0082(15) -0.0073(13) 0.0052(12) -0.0017(13) O1 0.020(5) 0.019(5) 0.011(4) -0.005(3) -0.002(3) -0.008(4) O2 0.009(4) 0.020(4) 0.016(4) -0.012(4) 0.002(3) 0.001(3) O3 0.019(4) 0.046(7) 0.033(6) -0.031(5) -0.017(4) 0.015(4) O4 0.023(5) 0.044(7) 0.023(5) -0.022(5) -0.009(4) 0.004(5) O5 0.059(8) 0.055(8) 0.055(7) 0.001(7) 0.023(7) -0.020(7) O6 0.028(6) 0.033(5) 0.052(7) -0.026(5) -0.021(6) 0.009(5) O7 0.020(4) 0.029(5) 0.028(6) -0.011(4) -0.015(4) 0.004(4) O8 0.024(6) 0.038(6) 0.023(5) -0.004(5) -0.006(4) -0.012(4) O9 0.025(6) 0.042(7) 0.020(5) -0.007(5) 0.005(4) -0.003(5) O10 0.019(5) 0.031(6) 0.020(5) -0.006(4) -0.008(4) 0.001(4) O11 0.038(5) 0.011(4) 0.008(4) -0.005(3) -0.001(4) -0.004(4) O12 0.035(6) 0.045(7) 0.010(4) -0.013(4) 0.010(4) -0.022(5) C1 0.022(5) 0.019(6) 0.010(5) -0.008(4) -0.001(4) -0.009(5) C2 0.031(6) 0.026(7) 0.009(6) -0.009(5) 0.007(5) -0.006(6) C3 0.029(7) 0.028(8) 0.026(7) -0.001(6) -0.002(5) -0.010(6) C4 0.030(8) 0.034(9) 0.018(6) -0.002(5) 0.004(6) -0.013(7) C5 0.020(7) 0.021(5) 0.012(6) -0.006(5) -0.001(5) -0.004(5) C6 0.030(7) 0.019(6) 0.003(5) -0.005(4) 0.002(5) -0.010(5) C7 0.025(7) 0.024(7) 0.019(6) -0.011(5) -0.001(5) -0.006(6) C8 0.036(8) 0.027(8) 0.011(6) -0.005(5) -0.003(6) -0.016(7) C9 0.018(5) 0.019(6) 0.009(5) -0.003(5) -0.004(4) -0.001(5) C10 0.017(5) 0.027(7) 0.017(6) -0.008(5) 0.012(5) -0.003(5) C11 0.019(6) 0.032(8) 0.026(7) -0.003(6) 0.000(5) -0.007(6) C12 0.014(6) 0.038(9) 0.018(7) -0.001(6) 0.005(5) -0.005(6) C13 0.012(5) 0.017(6) 0.013(6) -0.005(5) 0.012(4) -0.004(4) C14 0.013(5) 0.021(7) 0.009(6) -0.007(5) 0.005(4) -0.002(5) C15 0.013(6) 0.027(7) 0.017(6) -0.003(6) 0.010(5) 0.002(5) C16 0.022(7) 0.040(9) 0.018(7) -0.004(6) 0.016(5) 0.008(6) C17 0.012(6) 0.022(7) 0.014(5) -0.009(5) 0.000(4) -0.006(5) C18 0.020(6) 0.026(7) 0.012(6) -0.005(5) -0.001(4) -0.007(5) C19 0.020(7) 0.029(8) 0.011(6) -0.003(5) 0.002(5) -0.008(5) C20 0.025(8) 0.050(10) 0.017(7) -0.007(7) -0.001(6) -0.014(7) C21 0.015(6) 0.021(7) 0.011(5) -0.009(5) 0.006(4) -0.003(5) C22 0.019(6) 0.024(7) 0.013(5) -0.004(5) 0.006(4) -0.001(5) C23 0.020(6) 0.029(7) 0.012(5) -0.003(5) 0.004(5) -0.014(5) C24 0.028(8) 0.034(8) 0.033(8) -0.015(7) 0.019(6) -0.011(6) U2 0.0081(2) 0.0141(3) 0.013 -0.00727(18) 0.00528(17) -0.00484(18) Re3 0.0192(3) 0.0180(3) 0.0099(2) -0.0050(2) 0.00711(19) -0.0075(2) Re4 0.0114(2) 0.0175(3) 0.0069(2) -0.00749(19) 0.00645(18) -0.0065(2) P3 0.0120(16) 0.0210(19) 0.0097(15) -0.0082(13) 0.0070(12) -0.0053(13) P4 0.0105(15) 0.0192(18) 0.0068(15) -0.0053(13) 0.0058(11) -0.0052(13) O13 0.017(5) 0.020(5) 0.017(4) -0.011(4) 0.009(3) -0.002(3) O14 0.009(4) 0.029(5) 0.010(4) -0.006(4) 0.006(3) 0.000(3) O15 0.020(5) 0.027(4) 0.024(5) -0.006(4) -0.001(4) -0.012(4) O16 0.032(6) 0.037(7) 0.019(5) -0.005(4) 0.011(4) -0.005(5) O17 0.054(7) 0.049(8) 0.032(6) -0.012(5) 0.002(5) -0.038(6) O18 0.029(5) 0.037(7) 0.037(7) 0.010(5) 0.013(5) 0.007(5) O19 0.028(5) 0.018(4) 0.009(4) -0.008(3) 0.008(4) -0.011(4) O20 0.022(5) 0.021(5) 0.025(5) -0.003(4) 0.008(4) 0.001(4) O21 0.029(6) 0.037(6) 0.011(4) -0.007(4) -0.002(4) -0.011(5) O22 0.027(5) 0.039(7) 0.023(5) -0.013(5) 0.011(4) -0.022(5) O23 0.011(4) 0.026(5) 0.015(4) -0.009(3) 0.002(3) -0.003(4) O24 0.012(4) 0.024(5) 0.016(4) -0.004(4) -0.006(3) 0.001(4) C26 0.015(6) 0.022(7) 0.018(6) -0.006(5) 0.008(5) -0.005(5) C28 0.020(7) 0.039(9) 0.025(7) -0.018(7) 0.011(6) -0.009(6) C29 0.028(7) 0.019(6) 0.013(6) -0.011(5) 0.006(5) -0.007(5) C30 0.019(6) 0.034(8) 0.014(6) -0.009(6) 0.005(5) -0.008(5) C31 0.024(7) 0.037(8) 0.016(6) -0.014(6) 0.010(5) -0.013(6) C32 0.017(7) 0.063(11) 0.032(8) -0.011(8) 0.007(5) -0.016(7) C33 0.020(6) 0.022(7) 0.013(6) 0.006(5) 0.007(4) -0.008(5) C34 0.020(6) 0.024(7) 0.003(5) -0.005(5) 0.001(4) -0.003(5) C35 0.030(7) 0.013(7) 0.013(6) -0.001(5) -0.005(5) -0.003(5) C36 0.038(8) 0.038(9) 0.005(5) -0.001(6) -0.002(5) -0.011(7) C37 0.022(5) 0.024(7) 0.006(5) -0.008(5) 0.002(4) -0.010(5) C39 0.028(7) 0.037(9) 0.024(7) 0.006(6) -0.008(6) -0.020(7) C40 0.031(9) 0.051(11) 0.033(8) -0.002(7) -0.010(7) -0.013(8) C41 0.011(6) 0.023(5) 0.019(6) -0.009(5) 0.009(5) -0.007(5) C42 0.008(6) 0.024(6) 0.014(6) -0.010(5) 0.005(4) -0.003(5) C43 0.024(7) 0.027(7) 0.022(7) -0.017(6) 0.000(6) -0.006(6) C44 0.027(7) 0.033(8) 0.021(7) -0.018(6) 0.001(6) -0.012(6) C45 0.015(5) 0.017(6) 0.013(5) -0.002(5) 0.005(4) -0.006(5) C46 0.015(6) 0.020(7) 0.014(6) -0.003(5) 0.007(4) -0.007(5) C47 0.022(6) 0.026(7) 0.015(6) 0.001(5) -0.001(5) -0.011(5) C48 0.027(8) 0.054(11) 0.040(9) 0.006(8) -0.004(6) -0.029(8) C49 0.021(6) 0.027(7) 0.015(6) -0.003(5) 0.008(5) -0.007(5) Cl1 0.0159(17) 0.047(3) 0.029(2) -0.0032(18) 0.0050(14) -0.0083(16) Cl2 0.034(2) 0.043(3) 0.026(2) -0.0151(18) -0.0065(17) -0.0033(18) Cl3 0.031(2) 0.051(3) 0.0214(19) -0.0148(18) 0.0136(16) -0.0068(19) Cl4 0.068(4) 0.035(3) 0.038(3) 0.006(2) 0.018(2) -0.011(2) C50 0.029(7) 0.025(7) 0.016(6) -0.008(5) 0.000(5) -0.005(5) Cl5 0.029(2) 0.049(3) 0.0236(19) -0.0103(18) 0.0147(16) -0.0075(18) Cl6 0.047(3) 0.050(3) 0.0183(18) -0.0164(18) 0.0036(17) -0.014(2) Cl7 0.035(2) 0.034(2) 0.043(3) 0.008(2) 0.0002(19) -0.0023(19) Cl8 0.032(2) 0.030(2) 0.033(2) -0.0039(17) -0.0013(17) -0.0105(17) _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 O12 1.751(11) . ? U1 O11 1.763(10) . ? U1 O1 2.300(9) . ? U1 O2 2.329(9) . ? U1 O7 2.355(10) . ? U1 O3 2.451(10) . ? U1 O6 2.457(11) 2_656 ? Re1 O5 1.693(15) . ? Re1 O4 1.708(10) . ? Re1 O3 1.727(10) . ? Re1 O6 1.737(12) . ? Re2 O8 1.695(12) . ? Re2 O9 1.701(11) . ? Re2 O10 1.740(10) . ? Re2 O7 1.757(11) . ? P1 O1 1.520(10) . ? P1 C1 1.797(15) . ? P1 C5 1.796(15) . ? P1 C9 1.809(14) . ? P2 O2 1.520(10) . ? P2 C13 1.783(14) . ? P2 C21 1.787(14) . ? P2 C17 1.790(14) . ? O6 U1 2.457(11) 2_656 ? C1 C2 1.56(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.51(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.53(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.530(18) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.523(19) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.513(19) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.515(19) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.53(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.53(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.530(18) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.511(19) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.55(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.510(19) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.545(19) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.52(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.509(19) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.538(19) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.51(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? U2 O24 1.765(9) . ? U2 O23 1.772(10) . ? U2 O14 2.293(9) . ? U2 O13 2.297(9) . ? U2 O15 2.406(10) . ? U2 O22 2.443(11) 2_775 ? U2 O19 2.463(9) . ? Re3 O18 1.697(12) . ? Re3 O17 1.703(12) . ? Re3 O16 1.715(11) . ? Re3 O15 1.748(11) . ? Re4 O21 1.698(10) . ? Re4 O20 1.704(11) . ? Re4 O19 1.727(10) . ? Re4 O22 1.738(11) . ? P3 O13 1.524(10) . ? P3 C29 1.786(15) . ? P3 C33 1.790(15) . ? P3 C25 1.814(15) . ? P4 O14 1.520(9) . ? P4 C37 1.775(14) . ? P4 C41 1.788(15) . ? P4 C45 1.785(14) . ? O22 U2 2.443(11) 2_775 ? C25 C26 1.531(19) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.509(19) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.53(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.54(2) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.49(2) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.53(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.53(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.527(18) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.55(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.543(19) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.50(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.52(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.528(18) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.53(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.51(2) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.549(19) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.52(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.53(2) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 Cl2 1.742(16) . ? C49 Cl4 1.744(16) . ? C49 Cl3 1.768(15) . ? C49 Cl1 1.779(16) . ? C50 Cl6 1.751(15) . ? C50 Cl7 1.757(17) . ? C50 Cl8 1.760(17) . ? C50 Cl5 1.766(16) . ? 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 O12 U1 O11 178.0(5) . . ? O12 U1 O1 89.9(4) . . ? O11 U1 O1 89.8(4) . . ? O12 U1 O2 90.6(4) . . ? O11 U1 O2 90.7(4) . . ? O1 U1 O2 149.5(3) . . ? O12 U1 O7 90.0(5) . . ? O11 U1 O7 91.9(5) . . ? O1 U1 O7 74.5(4) . . ? O2 U1 O7 74.9(3) . . ? O12 U1 O3 89.7(5) . . ? O11 U1 O3 89.1(5) . . ? O1 U1 O3 139.1(4) . . ? O2 U1 O3 71.5(3) . . ? O7 U1 O3 146.4(4) . . ? O12 U1 O6 88.1(5) . 2_656 ? O11 U1 O6 89.9(5) . 2_656 ? O1 U1 O6 71.0(4) . 2_656 ? O2 U1 O6 139.5(3) . 2_656 ? O7 U1 O6 145.5(4) . 2_656 ? O3 U1 O6 68.1(4) . 2_656 ? O5 Re1 O4 108.8(8) . . ? O5 Re1 O3 109.1(8) . . ? O4 Re1 O3 107.9(5) . . ? O5 Re1 O6 111.0(7) . . ? O4 Re1 O6 109.7(6) . . ? O3 Re1 O6 110.4(6) . . ? O8 Re2 O9 109.0(6) . . ? O8 Re2 O10 109.5(5) . . ? O9 Re2 O10 109.8(5) . . ? O8 Re2 O7 110.2(6) . . ? O9 Re2 O7 109.9(6) . . ? O10 Re2 O7 108.5(5) . . ? O1 P1 C1 110.5(6) . . ? O1 P1 C5 108.7(6) . . ? C1 P1 C5 110.2(7) . . ? O1 P1 C9 112.1(6) . . ? C1 P1 C9 106.9(7) . . ? C5 P1 C9 108.4(7) . . ? O2 P2 C13 110.1(6) . . ? O2 P2 C21 110.9(6) . . ? C13 P2 C21 109.7(7) . . ? O2 P2 C17 111.6(6) . . ? C13 P2 C17 108.8(7) . . ? C21 P2 C17 105.7(7) . . ? P1 O1 U1 145.4(6) . . ? P2 O2 U1 150.8(6) . . ? Re1 O3 U1 155.3(6) . . ? Re1 O6 U1 157.1(7) . 2_656 ? Re2 O7 U1 153.5(6) . . ? C2 C1 P1 114.0(10) . . ? C2 C1 H1A 108.7 . . ? P1 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? P1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C3 C2 C1 113.2(13) . . ? C3 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C2 C3 C4 114.7(14) . . ? C2 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? C2 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 P1 113.1(10) . . ? C6 C5 H5A 109.0 . . ? P1 C5 H5A 109.0 . . ? C6 C5 H5B 109.0 . . ? P1 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C7 C6 C5 113.0(12) . . ? C7 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? C7 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C6 110.2(13) . . ? C8 C7 H7A 109.6 . . ? C6 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P1 111.9(10) . . ? C10 C9 H9A 109.2 . . ? P1 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? P1 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 C11 111.1(13) . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 113.0(13) . . ? C10 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? C10 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 P2 113.2(10) . . ? C14 C13 H13A 108.9 . . ? P2 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? P2 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C15 C14 C13 111.9(12) . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C14 C15 C16 112.3(13) . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 P2 116.3(11) . . ? C18 C17 H17A 108.2 . . ? P2 C17 H17A 108.2 . . ? C18 C17 H17B 108.2 . . ? P2 C17 H17B 108.2 . . ? H17A C17 H17B 107.4 . . ? C17 C18 C19 112.4(13) . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? C19 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? C20 C19 C18 112.7(13) . . ? C20 C19 H19A 109.0 . . ? C18 C19 H19A 109.0 . . ? C20 C19 H19B 109.0 . . ? C18 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 P2 116.1(10) . . ? C22 C21 H21A 108.3 . . ? P2 C21 H21A 108.3 . . ? C22 C21 H21B 108.3 . . ? P2 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? C21 C22 C23 112.0(12) . . ? C21 C22 H22A 109.2 . . ? C23 C22 H22A 109.2 . . ? C21 C22 H22B 109.2 . . ? C23 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C24 C23 C22 113.7(13) . . ? C24 C23 H23A 108.8 . . ? C22 C23 H23A 108.8 . . ? C24 C23 H23B 108.8 . . ? C22 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O24 U2 O23 179.3(5) . . ? O24 U2 O14 92.3(4) . . ? O23 U2 O14 87.8(4) . . ? O24 U2 O13 91.1(4) . . ? O23 U2 O13 89.1(4) . . ? O14 U2 O13 148.5(4) . . ? O24 U2 O15 88.1(4) . . ? O23 U2 O15 92.5(4) . . ? O14 U2 O15 74.6(4) . . ? O13 U2 O15 74.3(4) . . ? O24 U2 O22 90.9(4) . 2_775 ? O23 U2 O22 88.5(4) . 2_775 ? O14 U2 O22 139.5(4) . 2_775 ? O13 U2 O22 71.7(4) . 2_775 ? O15 U2 O22 145.9(4) . 2_775 ? O24 U2 O19 87.1(4) . . ? O23 U2 O19 92.4(4) . . ? O14 U2 O19 71.8(3) . . ? O13 U2 O19 139.7(3) . . ? O15 U2 O19 145.8(3) . . ? O22 U2 O19 68.1(3) 2_775 . ? O18 Re3 O17 108.9(7) . . ? O18 Re3 O16 109.3(6) . . ? O17 Re3 O16 109.3(6) . . ? O18 Re3 O15 110.2(6) . . ? O17 Re3 O15 109.2(6) . . ? O16 Re3 O15 109.9(5) . . ? O21 Re4 O20 107.7(5) . . ? O21 Re4 O19 109.4(5) . . ? O20 Re4 O19 109.9(5) . . ? O21 Re4 O22 109.2(5) . . ? O20 Re4 O22 109.4(6) . . ? O19 Re4 O22 111.2(5) . . ? O13 P3 C29 110.6(7) . . ? O13 P3 C33 111.4(7) . . ? C29 P3 C33 107.3(7) . . ? O13 P3 C25 109.2(6) . . ? C29 P3 C25 109.1(7) . . ? C33 P3 C25 109.3(7) . . ? O14 P4 C37 108.7(6) . . ? O14 P4 C41 110.6(6) . . ? C37 P4 C41 107.8(7) . . ? O14 P4 C45 111.7(6) . . ? C37 P4 C45 108.8(7) . . ? C41 P4 C45 109.1(7) . . ? P3 O13 U2 154.3(6) . . ? P4 O14 U2 153.7(6) . . ? Re3 O15 U2 144.5(6) . . ? Re4 O19 U2 174.5(6) . . ? Re4 O22 U2 169.8(6) . 2_775 ? C26 C25 P3 112.5(10) . . ? C26 C25 H25A 109.1 . . ? P3 C25 H25A 109.1 . . ? C26 C25 H25B 109.1 . . ? P3 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C27 C26 C25 110.5(12) . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C26 C27 C28 112.9(13) . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27B 109.0 . . ? C28 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 P3 114.2(11) . . ? C30 C29 H29A 108.7 . . ? P3 C29 H29A 108.7 . . ? C30 C29 H29B 108.7 . . ? P3 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C31 C30 C29 112.2(14) . . ? C31 C30 H30A 109.2 . . ? C29 C30 H30A 109.2 . . ? C31 C30 H30B 109.2 . . ? C29 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C30 C31 C32 113.8(15) . . ? C30 C31 H31A 108.8 . . ? C32 C31 H31A 108.8 . . ? C30 C31 H31B 108.8 . . ? C32 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 P3 113.1(10) . . ? C34 C33 H33A 109.0 . . ? P3 C33 H33A 109.0 . . ? C34 C33 H33B 109.0 . . ? P3 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C35 C34 C33 113.7(12) . . ? C35 C34 H34A 108.8 . . ? C33 C34 H34A 108.8 . . ? C35 C34 H34B 108.8 . . ? C33 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? C34 C35 C36 111.9(12) . . ? C34 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? C34 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 P4 113.8(10) . . ? C38 C37 H37A 108.8 . . ? P4 C37 H37A 108.8 . . ? C38 C37 H37B 108.8 . . ? P4 C37 H37B 108.8 . . ? H37A C37 H37B 107.7 . . ? C39 C38 C37 114.0(12) . . ? C39 C38 H38A 108.7 . . ? C37 C38 H38A 108.7 . . ? C39 C38 H38B 108.7 . . ? C37 C38 H38B 108.7 . . ? H38A C38 H38B 107.6 . . ? C38 C39 C40 112.8(14) . . ? C38 C39 H39A 109.0 . . ? C40 C39 H39A 109.0 . . ? C38 C39 H39B 109.0 . . ? C40 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 P4 114.5(10) . . ? C42 C41 H41A 108.6 . . ? P4 C41 H41A 108.6 . . ? C42 C41 H41B 108.6 . . ? P4 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? C41 C42 C43 114.2(12) . . ? C41 C42 H42A 108.7 . . ? C43 C42 H42A 108.7 . . ? C41 C42 H42B 108.7 . . ? C43 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? C44 C43 C42 113.1(13) . . ? C44 C43 H43A 109.0 . . ? C42 C43 H43A 109.0 . . ? C44 C43 H43B 109.0 . . ? C42 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 P4 113.4(10) . . ? C46 C45 H45A 108.9 . . ? P4 C45 H45A 108.9 . . ? C46 C45 H45B 108.9 . . ? P4 C45 H45B 108.9 . . ? H45A C45 H45B 107.7 . . ? C47 C46 C45 112.5(12) . . ? C47 C46 H46A 109.1 . . ? C45 C46 H46A 109.1 . . ? C47 C46 H46B 109.1 . . ? C45 C46 H46B 109.1 . . ? H46A C46 H46B 107.8 . . ? C46 C47 C48 113.3(14) . . ? C46 C47 H47A 108.9 . . ? C48 C47 H47A 108.9 . . ? C46 C47 H47B 108.9 . . ? C48 C47 H47B 108.9 . . ? H47A C47 H47B 107.7 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Cl2 C49 Cl4 111.6(9) . . ? Cl2 C49 Cl3 108.8(8) . . ? Cl4 C49 Cl3 110.0(9) . . ? Cl2 C49 Cl1 109.5(9) . . ? Cl4 C49 Cl1 108.8(8) . . ? Cl3 C49 Cl1 107.9(8) . . ? Cl6 C50 Cl7 109.5(9) . . ? Cl6 C50 Cl8 109.4(9) . . ? Cl7 C50 Cl8 110.1(9) . . ? Cl6 C50 Cl5 108.9(9) . . ? Cl7 C50 Cl5 109.7(9) . . ? Cl8 C50 Cl5 109.2(8) . . ? 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 C1 P1 O1 U1 34.1(13) . . . . ? C5 P1 O1 U1 155.2(10) . . . . ? C9 P1 O1 U1 -85.1(12) . . . . ? O12 U1 O1 P1 -34.4(11) . . . . ? O11 U1 O1 P1 147.6(11) . . . . ? O2 U1 O1 P1 56.6(14) . . . . ? O7 U1 O1 P1 55.6(11) . . . . ? O3 U1 O1 P1 -123.9(11) . . . . ? O6 U1 O1 P1 -122.5(12) 2_656 . . . ? C13 P2 O2 U1 146.5(11) . . . . ? C21 P2 O2 U1 25.0(14) . . . . ? C17 P2 O2 U1 -92.6(13) . . . . ? O12 U1 O2 P2 -40.5(13) . . . . ? O11 U1 O2 P2 137.9(13) . . . . ? O1 U1 O2 P2 -131.3(11) . . . . ? O7 U1 O2 P2 -130.4(13) . . . . ? O3 U1 O2 P2 49.0(12) . . . . ? O6 U1 O2 P2 47.3(15) 2_656 . . . ? O5 Re1 O3 U1 76(2) . . . . ? O4 Re1 O3 U1 -165.5(18) . . . . ? O6 Re1 O3 U1 -46(2) . . . . ? O12 U1 O3 Re1 -58.3(19) . . . . ? O11 U1 O3 Re1 120.0(19) . . . . ? O1 U1 O3 Re1 31(2) . . . . ? O2 U1 O3 Re1 -149(2) . . . . ? O7 U1 O3 Re1 -147.9(15) . . . . ? O6 U1 O3 Re1 29.8(18) 2_656 . . . ? O5 Re1 O6 U1 46(2) . . . 2_656 ? O4 Re1 O6 U1 -75(2) . . . 2_656 ? O3 Re1 O6 U1 166.6(18) . . . 2_656 ? O8 Re2 O7 U1 33.1(16) . . . . ? O9 Re2 O7 U1 -87.0(15) . . . . ? O10 Re2 O7 U1 153.0(14) . . . . ? O12 U1 O7 Re2 -72.6(15) . . . . ? O11 U1 O7 Re2 108.2(15) . . . . ? O1 U1 O7 Re2 -162.5(16) . . . . ? O2 U1 O7 Re2 18.0(14) . . . . ? O3 U1 O7 Re2 17(2) . . . . ? O6 U1 O7 Re2 -159.3(12) 2_656 . . . ? O1 P1 C1 C2 68.4(11) . . . . ? C5 P1 C1 C2 -51.7(11) . . . . ? C9 P1 C1 C2 -169.3(9) . . . . ? P1 C1 C2 C3 -164.8(10) . . . . ? C1 C2 C3 C4 -61.9(18) . . . . ? O1 P1 C5 C6 177.9(10) . . . . ? C1 P1 C5 C6 -60.8(12) . . . . ? C9 P1 C5 C6 55.8(12) . . . . ? P1 C5 C6 C7 165.8(11) . . . . ? C5 C6 C7 C8 -178.7(13) . . . . ? O1 P1 C9 C10 -47.0(12) . . . . ? C1 P1 C9 C10 -168.3(10) . . . . ? C5 P1 C9 C10 72.9(11) . . . . ? P1 C9 C10 C11 -178.6(11) . . . . ? C9 C10 C11 C12 -177.6(13) . . . . ? O2 P2 C13 C14 57.0(11) . . . . ? C21 P2 C13 C14 179.2(10) . . . . ? C17 P2 C13 C14 -65.6(12) . . . . ? P2 C13 C14 C15 -170.1(10) . . . . ? C13 C14 C15 C16 -179.2(13) . . . . ? O2 P2 C17 C18 172.7(10) . . . . ? C13 P2 C17 C18 -65.7(12) . . . . ? C21 P2 C17 C18 52.0(12) . . . . ? P2 C17 C18 C19 -174.6(10) . . . . ? C17 C18 C19 C20 176.9(13) . . . . ? O2 P2 C21 C22 61.3(12) . . . . ? C13 P2 C21 C22 -60.4(13) . . . . ? C17 P2 C21 C22 -177.6(11) . . . . ? P2 C21 C22 C23 -175.1(10) . . . . ? C21 C22 C23 C24 66.1(17) . . . . ? C29 P3 O13 U2 101.8(15) . . . . ? C33 P3 O13 U2 -17.4(17) . . . . ? C25 P3 O13 U2 -138.1(14) . . . . ? O24 U2 O13 P3 11.8(15) . . . . ? O23 U2 O13 P3 -168.8(15) . . . . ? O14 U2 O13 P3 -84.5(16) . . . . ? O15 U2 O13 P3 -75.9(15) . . . . ? O22 U2 O13 P3 102.4(15) 2_775 . . . ? O19 U2 O13 P3 98.6(15) . . . . ? C37 P4 O14 U2 -132.4(14) . . . . ? C41 P4 O14 U2 109.4(15) . . . . ? C45 P4 O14 U2 -12.3(17) . . . . ? O24 U2 O14 P4 7.8(15) . . . . ? O23 U2 O14 P4 -171.5(15) . . . . ? O13 U2 O14 P4 103.8(15) . . . . ? O15 U2 O14 P4 95.3(15) . . . . ? O22 U2 O14 P4 -86.3(16) 2_775 . . . ? O19 U2 O14 P4 -78.3(15) . . . . ? O18 Re3 O15 U2 -47.7(12) . . . . ? O17 Re3 O15 U2 -167.2(10) . . . . ? O16 Re3 O15 U2 72.8(11) . . . . ? O24 U2 O15 Re3 4.0(10) . . . . ? O23 U2 O15 Re3 -176.0(10) . . . . ? O14 U2 O15 Re3 -88.9(10) . . . . ? O13 U2 O15 Re3 95.7(10) . . . . ? O22 U2 O15 Re3 92.9(12) 2_775 . . . ? O19 U2 O15 Re3 -78.0(12) . . . . ? O21 Re4 O19 U2 -106(6) . . . . ? O20 Re4 O19 U2 136(6) . . . . ? O22 Re4 O19 U2 14(6) . . . . ? O24 U2 O19 Re4 87(6) . . . . ? O23 U2 O19 Re4 -93(6) . . . . ? O14 U2 O19 Re4 -180(100) . . . . ? O13 U2 O19 Re4 -1(6) . . . . ? O15 U2 O19 Re4 169(6) . . . . ? O22 U2 O19 Re4 -5(6) 2_775 . . . ? O21 Re4 O22 U2 -9(4) . . . 2_775 ? O20 Re4 O22 U2 109(4) . . . 2_775 ? O19 Re4 O22 U2 -129(4) . . . 2_775 ? O13 P3 C25 C26 175.6(10) . . . . ? C29 P3 C25 C26 -63.4(12) . . . . ? C33 P3 C25 C26 53.5(12) . . . . ? P3 C25 C26 C27 177.8(10) . . . . ? C25 C26 C27 C28 177.9(12) . . . . ? O13 P3 C29 C30 50.7(12) . . . . ? C33 P3 C29 C30 172.3(10) . . . . ? C25 P3 C29 C30 -69.5(12) . . . . ? P3 C29 C30 C31 -168.8(10) . . . . ? C29 C30 C31 C32 -175.4(13) . . . . ? O13 P3 C33 C34 -64.1(11) . . . . ? C29 P3 C33 C34 174.8(10) . . . . ? C25 P3 C33 C34 56.6(12) . . . . ? P3 C33 C34 C35 173.8(10) . . . . ? C33 C34 C35 C36 -71.8(16) . . . . ? O14 P4 C37 C38 -55.5(12) . . . . ? C41 P4 C37 C38 64.4(11) . . . . ? C45 P4 C37 C38 -177.4(10) . . . . ? P4 C37 C38 C39 170.8(11) . . . . ? C37 C38 C39 C40 -178.4(14) . . . . ? O14 P4 C41 C42 175.4(10) . . . . ? C37 P4 C41 C42 56.6(12) . . . . ? C45 P4 C41 C42 -61.4(12) . . . . ? P4 C41 C42 C43 169.1(10) . . . . ? C41 C42 C43 C44 -62.6(17) . . . . ? O14 P4 C45 C46 70.4(11) . . . . ? C37 P4 C45 C46 -169.5(9) . . . . ? C41 P4 C45 C46 -52.2(11) . . . . ? P4 C45 C46 C47 -166.6(10) . . . . ? C45 C46 C47 C48 -170.1(13) . . . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 6.855 _refine_diff_density_min -10.471 _refine_diff_density_rms 0.441