Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email DAVID.COLLISON@MAN.AC.UK _publ_contact_author_name 'Dr David Collison' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Chemistry Manchester University Manchester M13 9PL UNITED KINGDOM ; _publ_section_title ; The structural and spectroscopic characterisation of three actinyl complexes with coordinated, and uncoordinated, perrhenate; [UO2(ReO4)2(TPPO)3], [{(UO2)(TPPO)3}2(m2-O2)][ReO4]2 and [NpO2(TPPO)4][ReO4]. ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; loop_ _publ_author_name 'David Collison' 'Madeleine Helliwell' 'Gordon H. John' 'Iain May' 'James D. McKinney' ; M.Sarsfield ; 'Helen Steele' data_s870rx _database_code_depnum_ccdc_archive 'CCDC 222068' #------------------------------------------------------------------------------ _audit_creation_date 19100-10-03 _audit_creation_method 'by teXsan v1.7' _audit_update_record ; ? ; _publ_section_exptl_refinement ; The data were collected using the RAXIS in 90 x 3 degree phi oscillations, of 5 minutes per exposure. The structure was solved by direct methods and non-H atoms were refined anisotropically whilst H atoms were included in calculated positions. ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H45 O13 P3 Re2 U' _chemical_formula_weight 1605.24 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.98(1) _cell_length_b 15.93(1) _cell_length_c 13.23(1) _cell_angle_alpha 94.65(4) _cell_angle_beta 111.53(4) _cell_angle_gamma 83.36(3) _cell_volume 2719(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'one image' _cell_measurement_theta_min 5 _cell_measurement_theta_max 20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.961 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 7.562 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku RAXIS' _diffrn_measurement_method '90 x 3 degree phi scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 39405 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.08 _reflns_number_total 10237 _reflns_number_gt 9286 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1995)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'teXsan (MSC, 1995)' _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 w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+8.2353P] 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 SHELXL _refine_ls_extinction_coef 0.0047(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10237 _refine_ls_number_parameters 659 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0978 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U -0.641716(15) 0.235034(12) 0.415039(14) 0.03018(8) Uani 1 d . . . Re1 Re -0.64460(3) 0.31364(2) 0.69767(2) 0.06075(11) Uani 1 d . . . Re2 Re -0.37057(2) 0.18236(3) 0.66010(2) 0.06884(12) Uani 1 d . . . P1 P -0.92433(12) 0.23917(10) 0.39086(12) 0.0382(3) Uani 1 d . . . P2 P -0.77288(11) 0.26432(9) 0.11564(11) 0.0340(3) Uani 1 d . . . P3 P -0.42816(11) 0.22731(9) 0.31313(11) 0.0328(3) Uani 1 d . . . O1 O -0.6461(3) 0.1246(3) 0.3988(3) 0.0388(9) Uani 1 d . . . O2 O -0.6372(3) 0.3452(3) 0.4307(3) 0.0430(9) Uani 1 d . . . O3 O -0.8102(3) 0.2442(3) 0.4213(4) 0.0484(10) Uani 1 d . . . O4 O -0.7615(3) 0.2517(3) 0.2326(3) 0.0364(8) Uani 1 d . . . O5 O -0.5406(3) 0.2288(2) 0.3017(3) 0.0346(8) Uani 1 d . . . O6 O -0.6279(4) 0.2387(3) 0.6014(3) 0.0535(12) Uani 1 d . . . O7 O -0.7370(7) 0.3896(4) 0.6327(7) 0.109(3) Uani 1 d . . . O8 O -0.6827(9) 0.2665(6) 0.7848(6) 0.138(4) Uani 1 d . . . O9 O -0.5341(8) 0.3574(7) 0.7665(8) 0.159(4) Uani 1 d . . . O10 O -0.4642(4) 0.2054(3) 0.5319(3) 0.0510(11) Uani 1 d . . . O11 O -0.4151(6) 0.1317(7) 0.7359(7) 0.136(4) Uani 1 d . . . O12 O -0.2616(6) 0.1335(7) 0.6477(7) 0.138(4) Uani 1 d . . . O13 O -0.3371(8) 0.2761(8) 0.7318(7) 0.166(5) Uani 1 d . . . C1 C -0.9709(5) 0.1565(4) 0.2882(5) 0.0441(14) Uani 1 d . . . C2 C -0.9038(6) 0.0850(4) 0.2845(6) 0.0528(16) Uani 1 d . . . H2 H -0.8354 0.0816 0.3321 0.063 Uiso 1 calc R . . C3 C -0.9398(7) 0.0195(5) 0.2097(7) 0.069(2) Uani 1 d . . . H3 H -0.8959 -0.0284 0.2070 0.083 Uiso 1 calc R . . C4 C -1.0422(8) 0.0256(6) 0.1382(7) 0.077(3) Uani 1 d . . . H4 H -1.0664 -0.0184 0.0875 0.093 Uiso 1 calc R . . C5 C -1.1080(7) 0.0965(6) 0.1421(7) 0.072(2) Uani 1 d . . . H5 H -1.1763 0.1002 0.0943 0.086 Uiso 1 calc R . . C6 C -1.0729(6) 0.1604(5) 0.2156(6) 0.0560(17) Uani 1 d . . . H6 H -1.1177 0.2079 0.2177 0.067 Uiso 1 calc R . . C7 C -0.9552(5) 0.2171(4) 0.5065(5) 0.0440(14) Uani 1 d . . . C8 C -1.0023(5) 0.1452(5) 0.5085(6) 0.0524(16) Uani 1 d . . . H8 H -1.0177 0.1066 0.4494 0.063 Uiso 1 calc R . . C9 C -1.0269(7) 0.1307(6) 0.5991(7) 0.069(2) Uani 1 d . . . H9 H -1.0595 0.0831 0.5995 0.083 Uiso 1 calc R . . C10 C -1.0025(8) 0.1872(7) 0.6873(7) 0.077(3) Uani 1 d . . . H10 H -1.0185 0.1778 0.7475 0.093 Uiso 1 calc R . . C11 C -0.9546(8) 0.2574(7) 0.6862(6) 0.081(3) Uani 1 d . . . H11 H -0.9368 0.2946 0.7467 0.097 Uiso 1 calc R . . C12 C -0.9321(6) 0.2739(5) 0.5957(6) 0.0624(19) Uani 1 d . . . H12 H -0.9017 0.3227 0.5951 0.075 Uiso 1 calc R . . C13 C -0.9971(5) 0.3372(4) 0.3399(5) 0.0477(15) Uani 1 d . . . C14 C -1.0829(6) 0.3707(5) 0.3634(8) 0.069(2) Uani 1 d . . . H14 H -1.1040 0.3422 0.4092 0.083 Uiso 1 calc R . . C15 C -1.1377(7) 0.4450(6) 0.3209(9) 0.082(3) Uani 1 d . . . H15 H -1.1950 0.4657 0.3382 0.098 Uiso 1 calc R . . C16 C -1.1097(10) 0.4883(6) 0.2544(10) 0.099(4) Uani 1 d . . . H16 H -1.1456 0.5396 0.2278 0.119 Uiso 1 calc R . . C17 C -1.0267(14) 0.4548(8) 0.2268(15) 0.164(8) Uani 1 d . . . H17 H -1.0083 0.4825 0.1784 0.197 Uiso 1 calc R . . C18 C -0.9700(10) 0.3798(7) 0.2707(11) 0.114(5) Uani 1 d . . . H18 H -0.9132 0.3587 0.2526 0.137 Uiso 1 calc R . . C19 C -0.9074(5) 0.2872(4) 0.0320(4) 0.0415(13) Uani 1 d . . . C20 C -0.9744(6) 0.2247(5) 0.0175(6) 0.0597(18) Uani 1 d . . . H20 H -0.9494 0.1727 0.0491 0.072 Uiso 1 calc R . . C21 C -1.0787(6) 0.2408(6) -0.0444(7) 0.077(3) Uani 1 d . . . H21 H -1.1228 0.1988 -0.0550 0.092 Uiso 1 calc R . . C22 C -1.1179(6) 0.3174(6) -0.0902(7) 0.078(3) Uani 1 d . . . H22 H -1.1882 0.3278 -0.1296 0.094 Uiso 1 calc R . . C23 C -1.0528(7) 0.3780(7) -0.0773(8) 0.087(3) Uani 1 d . . . H23 H -1.0789 0.4299 -0.1090 0.104 Uiso 1 calc R . . C24 C -0.9473(6) 0.3634(5) -0.0171(6) 0.0621(19) Uani 1 d . . . H24 H -0.9036 0.4051 -0.0101 0.074 Uiso 1 calc R . . C25 C -0.7078(5) 0.3538(4) 0.1078(5) 0.0389(12) Uani 1 d . . . C26 C -0.7056(6) 0.4215(4) 0.1827(5) 0.0510(16) Uani 1 d . . . H26 H -0.7353 0.4184 0.2346 0.061 Uiso 1 calc R . . C27 C -0.6589(6) 0.4934(4) 0.1795(6) 0.0598(19) Uani 1 d . . . H27 H -0.6565 0.5381 0.2300 0.072 Uiso 1 calc R . . C28 C -0.6166(6) 0.4985(5) 0.1019(7) 0.066(2) Uani 1 d . . . H28 H -0.5864 0.5469 0.0990 0.080 Uiso 1 calc R . . C29 C -0.6189(7) 0.4313(6) 0.0277(7) 0.072(2) Uani 1 d . . . H29 H -0.5894 0.4348 -0.0242 0.087 Uiso 1 calc R . . C30 C -0.6640(6) 0.3597(4) 0.0295(6) 0.0530(16) Uani 1 d . . . H30 H -0.6654 0.3153 -0.0211 0.064 Uiso 1 calc R . . C31 C -0.7293(5) 0.1685(4) 0.0568(5) 0.0390(12) Uani 1 d . . . C32 C -0.7406(6) 0.1642(5) -0.0530(5) 0.0529(16) Uani 1 d . . . H32 H -0.7729 0.2097 -0.0966 0.064 Uiso 1 calc R . . C33 C -0.7032(7) 0.0912(5) -0.0959(6) 0.069(2) Uani 1 d . . . H33 H -0.7085 0.0887 -0.1682 0.083 Uiso 1 calc R . . C34 C -0.6583(7) 0.0228(5) -0.0331(7) 0.071(2) Uani 1 d . . . H34 H -0.6327 -0.0254 -0.0631 0.085 Uiso 1 calc R . . C35 C -0.6506(7) 0.0244(4) 0.0741(7) 0.064(2) Uani 1 d . . . H35 H -0.6217 -0.0227 0.1159 0.077 Uiso 1 calc R . . C36 C -0.6871(5) 0.0986(4) 0.1193(5) 0.0475(15) Uani 1 d . . . H36 H -0.6828 0.1006 0.1912 0.057 Uiso 1 calc R . . C37 C -0.3639(5) 0.3084(4) 0.4101(5) 0.0386(12) Uani 1 d . . . C38 C -0.4174(6) 0.3891(4) 0.3961(7) 0.0590(18) Uani 1 d . . . H38 H -0.4822 0.3974 0.3416 0.071 Uiso 1 calc R . . C39 C -0.3736(7) 0.4564(5) 0.4636(8) 0.073(2) Uani 1 d . . . H39 H -0.4086 0.5102 0.4548 0.088 Uiso 1 calc R . . C40 C -0.2777(7) 0.4430(5) 0.5440(7) 0.073(2) Uani 1 d . . . H40 H -0.2481 0.4883 0.5891 0.088 Uiso 1 calc R . . C41 C -0.2249(7) 0.3636(6) 0.5589(7) 0.071(2) Uani 1 d . . . H41 H -0.1605 0.3555 0.6139 0.085 Uiso 1 calc R . . C42 C -0.2684(5) 0.2953(4) 0.4910(5) 0.0492(15) Uani 1 d . . . H42 H -0.2332 0.2415 0.5004 0.059 Uiso 1 calc R . . C43 C -0.4127(5) 0.2476(4) 0.1871(5) 0.0407(13) Uani 1 d . . . C44 C -0.3494(6) 0.3048(5) 0.1812(6) 0.0581(18) Uani 1 d . . . H44 H -0.3162 0.3380 0.2426 0.070 Uiso 1 calc R . . C45 C -0.3337(8) 0.3141(6) 0.0846(7) 0.079(3) Uani 1 d . . . H45 H -0.2909 0.3538 0.0818 0.095 Uiso 1 calc R . . C46 C -0.3816(7) 0.2646(6) -0.0070(7) 0.069(2) Uani 1 d . . . H46 H -0.3708 0.2702 -0.0713 0.083 Uiso 1 calc R . . C47 C -0.4456(7) 0.2066(5) -0.0018(6) 0.063(2) Uani 1 d . . . H47 H -0.4779 0.1732 -0.0633 0.076 Uiso 1 calc R . . C48 C -0.4628(5) 0.1970(4) 0.0937(5) 0.0493(15) Uani 1 d . . . H48 H -0.5066 0.1581 0.0961 0.059 Uiso 1 calc R . . C49 C -0.3610(4) 0.1227(3) 0.3470(4) 0.0350(11) Uani 1 d . . . C50 C -0.2628(5) 0.1025(4) 0.3436(6) 0.0508(16) Uani 1 d . . . H50 H -0.2283 0.1438 0.3290 0.061 Uiso 1 calc R . . C51 C -0.2165(6) 0.0207(4) 0.3621(7) 0.0592(19) Uani 1 d . . . H51 H -0.1508 0.0073 0.3598 0.071 Uiso 1 calc R . . C52 C -0.2669(6) -0.0413(4) 0.3840(6) 0.0530(17) Uani 1 d . . . H52 H -0.2346 -0.0958 0.3979 0.064 Uiso 1 calc R . . C53 C -0.3644(6) -0.0220(4) 0.3852(6) 0.0563(17) Uani 1 d . . . H53 H -0.3993 -0.0638 0.3982 0.068 Uiso 1 calc R . . C54 C -0.4123(5) 0.0610(4) 0.3668(5) 0.0481(15) Uani 1 d . . . H54 H -0.4785 0.0741 0.3682 0.058 Uiso 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 0.03166(13) 0.03412(13) 0.02577(12) -0.00016(7) 0.01169(8) -0.00364(7) Re1 0.0801(2) 0.0629(2) 0.04404(17) -0.01686(13) 0.02955(15) -0.01508(15) Re2 0.03754(17) 0.1246(3) 0.03876(16) 0.02280(16) 0.00345(11) -0.00686(16) P1 0.0343(8) 0.0427(8) 0.0417(8) -0.0014(6) 0.0191(6) -0.0041(6) P2 0.0373(8) 0.0354(7) 0.0278(7) 0.0006(5) 0.0100(5) -0.0033(6) P3 0.0325(7) 0.0332(7) 0.0353(7) 0.0025(5) 0.0152(5) -0.0027(5) O1 0.039(2) 0.045(2) 0.036(2) 0.0006(17) 0.0192(17) -0.0050(17) O2 0.045(2) 0.047(2) 0.040(2) -0.0038(18) 0.0184(18) -0.0071(18) O3 0.035(2) 0.066(3) 0.051(2) -0.007(2) 0.0248(19) -0.006(2) O4 0.034(2) 0.049(2) 0.0236(18) 0.0005(16) 0.0075(14) -0.0030(16) O5 0.033(2) 0.040(2) 0.0345(19) 0.0016(16) 0.0159(15) -0.0040(16) O6 0.071(3) 0.059(3) 0.034(2) 0.007(2) 0.025(2) 0.004(2) O7 0.126(6) 0.060(4) 0.163(7) -0.008(4) 0.087(6) 0.010(4) O8 0.206(10) 0.167(8) 0.083(5) 0.003(5) 0.099(6) -0.020(7) O9 0.145(9) 0.156(9) 0.136(8) -0.040(7) -0.007(6) -0.078(7) O10 0.044(3) 0.068(3) 0.040(2) 0.004(2) 0.0131(18) -0.004(2) O11 0.085(6) 0.217(10) 0.103(6) 0.091(6) 0.010(4) -0.022(6) O12 0.076(5) 0.211(10) 0.118(6) 0.081(7) 0.031(4) 0.057(6) O13 0.149(9) 0.231(12) 0.081(5) -0.051(6) -0.012(5) -0.093(8) C1 0.049(4) 0.044(3) 0.044(3) 0.003(3) 0.020(3) -0.007(3) C2 0.054(4) 0.047(4) 0.058(4) 0.001(3) 0.020(3) -0.004(3) C3 0.086(6) 0.047(4) 0.076(5) -0.008(4) 0.033(5) -0.006(4) C4 0.100(7) 0.061(5) 0.074(6) -0.024(4) 0.033(5) -0.034(5) C5 0.068(5) 0.082(6) 0.058(5) -0.003(4) 0.010(4) -0.028(4) C6 0.052(4) 0.058(4) 0.056(4) 0.000(3) 0.015(3) -0.012(3) C7 0.037(3) 0.054(4) 0.042(3) 0.005(3) 0.016(2) 0.001(3) C8 0.048(4) 0.064(4) 0.055(4) 0.011(3) 0.028(3) -0.008(3) C9 0.065(5) 0.090(6) 0.064(5) 0.029(4) 0.034(4) 0.000(4) C10 0.083(6) 0.105(7) 0.053(5) 0.027(5) 0.035(4) 0.007(5) C11 0.098(7) 0.105(7) 0.038(4) -0.004(4) 0.024(4) -0.012(6) C12 0.063(5) 0.078(5) 0.050(4) -0.002(4) 0.023(3) -0.014(4) C13 0.052(4) 0.045(4) 0.055(4) 0.001(3) 0.030(3) -0.001(3) C14 0.062(5) 0.060(5) 0.100(6) 0.017(4) 0.047(5) 0.009(4) C15 0.062(5) 0.066(5) 0.122(8) 0.008(5) 0.044(5) 0.011(4) C16 0.125(10) 0.055(5) 0.131(9) 0.029(6) 0.068(8) 0.028(6) C17 0.237(18) 0.101(9) 0.242(18) 0.102(11) 0.194(16) 0.075(10) C18 0.145(11) 0.083(7) 0.171(11) 0.062(7) 0.130(10) 0.047(7) C19 0.042(3) 0.051(4) 0.030(3) 0.002(2) 0.011(2) -0.004(3) C20 0.048(4) 0.059(4) 0.064(5) 0.008(3) 0.009(3) -0.011(3) C21 0.048(5) 0.100(7) 0.071(5) 0.016(5) 0.002(4) -0.022(4) C22 0.042(4) 0.098(7) 0.076(6) 0.017(5) -0.006(4) -0.008(4) C23 0.053(5) 0.086(7) 0.100(7) 0.035(5) 0.000(5) 0.005(4) C24 0.051(4) 0.060(5) 0.064(5) 0.019(4) 0.005(3) -0.003(3) C25 0.040(3) 0.038(3) 0.036(3) 0.003(2) 0.010(2) -0.003(2) C26 0.066(5) 0.043(4) 0.044(4) 0.000(3) 0.020(3) -0.006(3) C27 0.078(5) 0.036(3) 0.056(4) -0.001(3) 0.009(4) -0.015(3) C28 0.070(5) 0.052(4) 0.071(5) 0.013(4) 0.011(4) -0.025(4) C29 0.077(6) 0.074(6) 0.078(6) 0.014(4) 0.037(5) -0.022(4) C30 0.066(5) 0.048(4) 0.053(4) -0.005(3) 0.030(3) -0.013(3) C31 0.044(3) 0.037(3) 0.038(3) -0.005(2) 0.017(2) -0.008(2) C32 0.070(5) 0.053(4) 0.034(3) -0.005(3) 0.017(3) -0.008(3) C33 0.105(7) 0.063(5) 0.047(4) -0.022(4) 0.038(4) -0.022(4) C34 0.098(7) 0.049(4) 0.073(5) -0.030(4) 0.047(5) -0.009(4) C35 0.081(6) 0.034(4) 0.077(5) -0.004(3) 0.028(4) -0.003(3) C36 0.060(4) 0.043(3) 0.039(3) -0.005(3) 0.019(3) -0.005(3) C37 0.039(3) 0.034(3) 0.049(3) 0.000(2) 0.023(3) -0.008(2) C38 0.058(4) 0.041(4) 0.074(5) -0.003(3) 0.020(4) -0.003(3) C39 0.076(6) 0.034(4) 0.112(7) -0.015(4) 0.041(5) -0.008(3) C40 0.079(6) 0.062(5) 0.084(6) -0.033(4) 0.037(5) -0.025(4) C41 0.061(5) 0.078(6) 0.065(5) -0.022(4) 0.013(4) -0.016(4) C42 0.042(4) 0.052(4) 0.049(4) -0.008(3) 0.014(3) -0.006(3) C43 0.039(3) 0.047(3) 0.039(3) 0.009(3) 0.018(2) 0.004(2) C44 0.057(5) 0.076(5) 0.049(4) 0.010(3) 0.023(3) -0.021(4) C45 0.084(7) 0.102(7) 0.068(5) 0.026(5) 0.037(5) -0.025(5) C46 0.074(6) 0.094(6) 0.054(4) 0.021(4) 0.040(4) 0.000(5) C47 0.080(6) 0.069(5) 0.044(4) 0.002(3) 0.029(4) 0.004(4) C48 0.056(4) 0.050(4) 0.046(4) 0.006(3) 0.024(3) -0.001(3) C49 0.035(3) 0.033(3) 0.035(3) 0.000(2) 0.011(2) -0.002(2) C50 0.048(4) 0.037(3) 0.070(4) -0.006(3) 0.025(3) -0.006(3) C51 0.043(4) 0.045(4) 0.083(5) -0.009(3) 0.019(3) 0.005(3) C52 0.062(4) 0.031(3) 0.052(4) 0.000(3) 0.007(3) 0.006(3) C53 0.071(5) 0.038(4) 0.064(4) 0.011(3) 0.029(4) 0.000(3) C54 0.051(4) 0.045(4) 0.056(4) 0.013(3) 0.029(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O2 1.756(4) . ? U1 O1 1.759(4) . ? U1 O3 2.374(4) . ? U1 O4 2.394(3) . ? U1 O6 2.398(4) . ? U1 O5 2.399(4) . ? U1 O10 2.408(4) . ? Re1 O9 1.677(8) . ? Re1 O8 1.690(7) . ? Re1 O7 1.693(8) . ? Re1 O6 1.734(4) . ? Re2 O11 1.658(7) . ? Re2 O12 1.685(8) . ? Re2 O13 1.719(10) . ? Re2 O10 1.756(4) . ? P1 O3 1.505(4) . ? P1 C13 1.796(7) . ? P1 C7 1.805(6) . ? P1 C1 1.806(7) . ? P2 O4 1.524(4) . ? P2 C31 1.802(6) . ? P2 C25 1.806(6) . ? P2 C19 1.809(6) . ? P3 O5 1.520(4) . ? P3 C37 1.809(6) . ? P3 C43 1.817(6) . ? P3 C49 1.819(6) . ? C1 C6 1.394(9) . ? C1 C2 1.399(9) . ? C2 C3 1.382(10) . ? C2 H2 0.9300 . ? C3 C4 1.393(13) . ? C3 H3 0.9300 . ? C4 C5 1.381(13) . ? C4 H4 0.9300 . ? C5 C6 1.352(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.389(10) . ? C7 C8 1.392(9) . ? C8 C9 1.404(9) . ? C8 H8 0.9300 . ? C9 C10 1.377(13) . ? C9 H9 0.9300 . ? C10 C11 1.372(14) . ? C10 H10 0.9300 . ? C11 C12 1.395(11) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.363(10) . ? C13 C14 1.386(9) . ? C14 C15 1.373(11) . ? C14 H14 0.9300 . ? C15 C16 1.347(14) . ? C15 H15 0.9300 . ? C16 C17 1.379(16) . ? C16 H16 0.9300 . ? C17 C18 1.397(14) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.382(9) . ? C19 C20 1.400(9) . ? C20 C21 1.390(10) . ? C20 H20 0.9300 . ? C21 C22 1.369(12) . ? C21 H21 0.9300 . ? C22 C23 1.362(13) . ? C22 H22 0.9300 . ? C23 C24 1.397(11) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.396(9) . ? C25 C26 1.400(9) . ? C26 C27 1.394(9) . ? C26 H26 0.9300 . ? C27 C28 1.371(12) . ? C27 H27 0.9300 . ? C28 C29 1.388(12) . ? C28 H28 0.9300 . ? C29 C30 1.371(10) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.383(9) . ? C31 C32 1.398(8) . ? C32 C33 1.384(10) . ? C32 H32 0.9300 . ? C33 C34 1.371(12) . ? C33 H33 0.9300 . ? C34 C35 1.381(11) . ? C34 H34 0.9300 . ? C35 C36 1.408(9) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C42 1.377(9) . ? C37 C38 1.400(9) . ? C38 C39 1.385(10) . ? C38 H38 0.9300 . ? C39 C40 1.377(13) . ? C39 H39 0.9300 . ? C40 C41 1.379(12) . ? C40 H40 0.9300 . ? C41 C42 1.398(10) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.366(9) . ? C43 C48 1.414(9) . ? C44 C45 1.396(10) . ? C44 H44 0.9300 . ? C45 C46 1.382(13) . ? C45 H45 0.9300 . ? C46 C47 1.380(12) . ? C46 H46 0.9300 . ? C47 C48 1.393(9) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C54 1.375(8) . ? C49 C50 1.389(9) . ? C50 C51 1.386(9) . ? C50 H50 0.9300 . ? C51 C52 1.382(10) . ? C51 H51 0.9300 . ? C52 C53 1.368(10) . ? C52 H52 0.9300 . ? C53 C54 1.408(9) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 U1 O1 179.73(17) . . ? O2 U1 O3 92.57(18) . . ? O1 U1 O3 87.59(17) . . ? O2 U1 O4 89.37(16) . . ? O1 U1 O4 90.46(16) . . ? O3 U1 O4 72.86(14) . . ? O2 U1 O6 86.69(17) . . ? O1 U1 O6 93.57(17) . . ? O3 U1 O6 71.14(16) . . ? O4 U1 O6 143.55(15) . . ? O2 U1 O5 89.56(16) . . ? O1 U1 O5 90.19(15) . . ? O3 U1 O5 146.28(14) . . ? O4 U1 O5 73.52(13) . . ? O6 U1 O5 142.56(15) . . ? O2 U1 O10 93.92(18) . . ? O1 U1 O10 86.10(18) . . ? O3 U1 O10 139.81(15) . . ? O4 U1 O10 146.74(14) . . ? O6 U1 O10 69.71(16) . . ? O5 U1 O10 73.42(14) . . ? O9 Re1 O8 109.8(5) . . ? O9 Re1 O7 109.4(5) . . ? O8 Re1 O7 109.6(5) . . ? O9 Re1 O6 110.6(5) . . ? O8 Re1 O6 109.0(4) . . ? O7 Re1 O6 108.4(3) . . ? O11 Re2 O12 113.5(5) . . ? O11 Re2 O13 104.5(5) . . ? O12 Re2 O13 106.2(6) . . ? O11 Re2 O10 112.9(3) . . ? O12 Re2 O10 110.8(3) . . ? O13 Re2 O10 108.4(4) . . ? O3 P1 C13 111.5(3) . . ? O3 P1 C7 111.6(3) . . ? C13 P1 C7 106.6(3) . . ? O3 P1 C1 111.5(3) . . ? C13 P1 C1 108.1(3) . . ? C7 P1 C1 107.3(3) . . ? O4 P2 C31 110.6(3) . . ? O4 P2 C25 111.1(2) . . ? C31 P2 C25 112.3(3) . . ? O4 P2 C19 110.5(2) . . ? C31 P2 C19 105.8(3) . . ? C25 P2 C19 106.3(3) . . ? O5 P3 C37 111.4(2) . . ? O5 P3 C43 113.1(3) . . ? C37 P3 C43 105.4(3) . . ? O5 P3 C49 110.9(2) . . ? C37 P3 C49 112.0(3) . . ? C43 P3 C49 103.8(3) . . ? P1 O3 U1 162.7(3) . . ? P2 O4 U1 145.0(2) . . ? P3 O5 U1 139.2(2) . . ? Re1 O6 U1 137.5(2) . . ? Re2 O10 U1 150.7(2) . . ? C6 C1 C2 119.2(6) . . ? C6 C1 P1 121.9(5) . . ? C2 C1 P1 118.9(5) . . ? C3 C2 C1 119.5(7) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.8(8) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.3(7) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 119.9(8) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 121.3(8) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? C12 C7 C8 119.1(6) . . ? C12 C7 P1 119.0(5) . . ? C8 C7 P1 121.9(5) . . ? C7 C8 C9 120.4(7) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 119.7(8) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 119.9(7) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 121.0(8) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C7 C12 C11 119.8(8) . . ? C7 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C18 C13 C14 117.5(7) . . ? C18 C13 P1 118.9(6) . . ? C14 C13 P1 123.6(5) . . ? C15 C14 C13 121.7(8) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C16 C15 C14 121.1(8) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 118.4(9) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C16 C17 C18 120.7(9) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C13 C18 C17 120.6(9) . . ? C13 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C24 C19 C20 118.6(6) . . ? C24 C19 P2 123.4(5) . . ? C20 C19 P2 118.0(5) . . ? C21 C20 C19 119.6(7) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C22 C21 C20 121.4(8) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C23 C22 C21 119.3(7) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C24 120.8(8) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C19 C24 C23 120.4(8) . . ? C19 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C30 C25 C26 119.4(6) . . ? C30 C25 P2 123.7(5) . . ? C26 C25 P2 116.9(5) . . ? C27 C26 C25 119.9(7) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 120.1(7) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 119.8(7) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C30 C29 C28 121.2(8) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C25 119.6(7) . . ? C29 C30 H30 120.2 . . ? C25 C30 H30 120.2 . . ? C36 C31 C32 119.9(6) . . ? C36 C31 P2 120.1(4) . . ? C32 C31 P2 120.0(5) . . ? C33 C32 C31 119.2(7) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C34 C33 C32 120.8(7) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 120.8(7) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C34 C35 C36 118.9(7) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C31 C36 C35 120.1(6) . . ? C31 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C42 C37 C38 120.5(6) . . ? C42 C37 P3 124.4(5) . . ? C38 C37 P3 115.0(5) . . ? C39 C38 C37 119.7(7) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C40 C39 C38 119.5(7) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 121.1(7) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C40 C41 C42 119.9(8) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C37 C42 C41 119.2(7) . . ? C37 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C44 C43 C48 119.4(6) . . ? C44 C43 P3 122.8(5) . . ? C48 C43 P3 117.7(5) . . ? C43 C44 C45 121.0(8) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C46 C45 C44 120.2(8) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C47 C46 C45 119.2(7) . . ? C47 C46 H46 120.4 . . ? C45 C46 H46 120.4 . . ? C46 C47 C48 121.4(8) . . ? C46 C47 H47 119.3 . . ? C48 C47 H47 119.3 . . ? C47 C48 C43 118.9(7) . . ? C47 C48 H48 120.6 . . ? C43 C48 H48 120.6 . . ? C54 C49 C50 119.9(5) . . ? C54 C49 P3 119.0(4) . . ? C50 C49 P3 120.9(5) . . ? C51 C50 C49 119.7(6) . . ? C51 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C52 C51 C50 120.8(7) . . ? C52 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C53 C52 C51 119.6(6) . . ? C53 C52 H52 120.2 . . ? C51 C52 H52 120.2 . . ? C52 C53 C54 120.2(7) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C49 C54 C53 119.8(6) . . ? C49 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 P1 O3 U1 -93.9(10) . . . . ? C7 P1 O3 U1 147.0(9) . . . . ? C1 P1 O3 U1 27.1(11) . . . . ? O2 U1 O3 P1 116.2(10) . . . . ? O1 U1 O3 P1 -63.6(10) . . . . ? O4 U1 O3 P1 27.7(10) . . . . ? O6 U1 O3 P1 -158.2(10) . . . . ? O5 U1 O3 P1 23.2(12) . . . . ? O10 U1 O3 P1 -144.6(9) . . . . ? C31 P2 O4 U1 72.4(5) . . . . ? C25 P2 O4 U1 -53.0(5) . . . . ? C19 P2 O4 U1 -170.8(4) . . . . ? O2 U1 O4 P2 81.3(4) . . . . ? O1 U1 O4 P2 -98.5(4) . . . . ? O3 U1 O4 P2 174.2(5) . . . . ? O6 U1 O4 P2 164.9(3) . . . . ? O5 U1 O4 P2 -8.4(4) . . . . ? O10 U1 O4 P2 -14.9(6) . . . . ? C37 P3 O5 U1 -47.5(4) . . . . ? C43 P3 O5 U1 -166.0(3) . . . . ? C49 P3 O5 U1 77.9(4) . . . . ? O2 U1 O5 P3 81.9(4) . . . . ? O1 U1 O5 P3 -98.2(4) . . . . ? O3 U1 O5 P3 175.8(3) . . . . ? O4 U1 O5 P3 171.4(4) . . . . ? O6 U1 O5 P3 -2.1(5) . . . . ? O10 U1 O5 P3 -12.3(3) . . . . ? O9 Re1 O6 U1 -89.2(6) . . . . ? O8 Re1 O6 U1 150.1(5) . . . . ? O7 Re1 O6 U1 30.8(5) . . . . ? O2 U1 O6 Re1 17.1(4) . . . . ? O1 U1 O6 Re1 -162.9(4) . . . . ? O3 U1 O6 Re1 -76.7(4) . . . . ? O4 U1 O6 Re1 -67.3(5) . . . . ? O5 U1 O6 Re1 102.1(4) . . . . ? O10 U1 O6 Re1 112.5(4) . . . . ? O11 Re2 O10 U1 28.1(7) . . . . ? O12 Re2 O10 U1 156.7(6) . . . . ? O13 Re2 O10 U1 -87.1(7) . . . . ? O2 U1 O10 Re2 95.3(6) . . . . ? O1 U1 O10 Re2 -85.0(6) . . . . ? O3 U1 O10 Re2 -3.4(7) . . . . ? O4 U1 O10 Re2 -169.9(4) . . . . ? O6 U1 O10 Re2 10.3(5) . . . . ? O5 U1 O10 Re2 -176.4(6) . . . . ? O3 P1 C1 C6 -152.7(5) . . . . ? C13 P1 C1 C6 -29.8(6) . . . . ? C7 P1 C1 C6 84.8(6) . . . . ? O3 P1 C1 C2 30.0(6) . . . . ? C13 P1 C1 C2 152.9(5) . . . . ? C7 P1 C1 C2 -92.5(6) . . . . ? C6 C1 C2 C3 -0.4(10) . . . . ? P1 C1 C2 C3 177.0(6) . . . . ? C1 C2 C3 C4 0.5(12) . . . . ? C2 C3 C4 C5 -0.3(13) . . . . ? C3 C4 C5 C6 0.1(14) . . . . ? C4 C5 C6 C1 0.0(13) . . . . ? C2 C1 C6 C5 0.2(11) . . . . ? P1 C1 C6 C5 -177.1(6) . . . . ? O3 P1 C7 C12 60.7(6) . . . . ? C13 P1 C7 C12 -61.2(6) . . . . ? C1 P1 C7 C12 -176.8(6) . . . . ? O3 P1 C7 C8 -119.9(5) . . . . ? C13 P1 C7 C8 118.2(6) . . . . ? C1 P1 C7 C8 2.6(6) . . . . ? C12 C7 C8 C9 0.5(11) . . . . ? P1 C7 C8 C9 -178.9(6) . . . . ? C7 C8 C9 C10 -1.1(12) . . . . ? C8 C9 C10 C11 0.1(13) . . . . ? C9 C10 C11 C12 1.6(15) . . . . ? C8 C7 C12 C11 1.2(11) . . . . ? P1 C7 C12 C11 -179.4(7) . . . . ? C10 C11 C12 C7 -2.2(14) . . . . ? O3 P1 C13 C18 41.7(10) . . . . ? C7 P1 C13 C18 163.7(9) . . . . ? C1 P1 C13 C18 -81.2(9) . . . . ? O3 P1 C13 C14 -141.1(7) . . . . ? C7 P1 C13 C14 -19.1(8) . . . . ? C1 P1 C13 C14 95.9(7) . . . . ? C18 C13 C14 C15 -1.4(15) . . . . ? P1 C13 C14 C15 -178.6(7) . . . . ? C13 C14 C15 C16 -0.1(16) . . . . ? C14 C15 C16 C17 2(2) . . . . ? C15 C16 C17 C18 -3(3) . . . . ? C14 C13 C18 C17 1(2) . . . . ? P1 C13 C18 C17 178.0(13) . . . . ? C16 C17 C18 C13 1(3) . . . . ? O4 P2 C19 C24 115.3(6) . . . . ? C31 P2 C19 C24 -124.9(6) . . . . ? C25 P2 C19 C24 -5.3(7) . . . . ? O4 P2 C19 C20 -63.9(6) . . . . ? C31 P2 C19 C20 55.8(6) . . . . ? C25 P2 C19 C20 175.4(5) . . . . ? C24 C19 C20 C21 -0.6(11) . . . . ? P2 C19 C20 C21 178.6(7) . . . . ? C19 C20 C21 C22 -1.2(14) . . . . ? C20 C21 C22 C23 1.9(16) . . . . ? C21 C22 C23 C24 -0.8(17) . . . . ? C20 C19 C24 C23 1.7(12) . . . . ? P2 C19 C24 C23 -177.5(7) . . . . ? C22 C23 C24 C19 -1.0(16) . . . . ? O4 P2 C25 C30 149.8(5) . . . . ? C31 P2 C25 C30 25.3(6) . . . . ? C19 P2 C25 C30 -89.9(6) . . . . ? O4 P2 C25 C26 -32.7(6) . . . . ? C31 P2 C25 C26 -157.2(5) . . . . ? C19 P2 C25 C26 87.6(5) . . . . ? C30 C25 C26 C27 -0.7(10) . . . . ? P2 C25 C26 C27 -178.4(5) . . . . ? C25 C26 C27 C28 1.0(11) . . . . ? C26 C27 C28 C29 -1.0(12) . . . . ? C27 C28 C29 C30 0.7(13) . . . . ? C28 C29 C30 C25 -0.5(13) . . . . ? C26 C25 C30 C29 0.5(11) . . . . ? P2 C25 C30 C29 177.9(6) . . . . ? O4 P2 C31 C36 -3.4(6) . . . . ? C25 P2 C31 C36 121.3(5) . . . . ? C19 P2 C31 C36 -123.1(5) . . . . ? O4 P2 C31 C32 174.9(5) . . . . ? C25 P2 C31 C32 -60.4(6) . . . . ? C19 P2 C31 C32 55.2(6) . . . . ? C36 C31 C32 C33 -4.1(11) . . . . ? P2 C31 C32 C33 177.6(6) . . . . ? C31 C32 C33 C34 2.0(12) . . . . ? C32 C33 C34 C35 0.9(14) . . . . ? C33 C34 C35 C36 -1.7(13) . . . . ? C32 C31 C36 C35 3.3(10) . . . . ? P2 C31 C36 C35 -178.4(6) . . . . ? C34 C35 C36 C31 -0.4(12) . . . . ? O5 P3 C37 C42 133.5(5) . . . . ? C43 P3 C37 C42 -103.6(6) . . . . ? C49 P3 C37 C42 8.6(6) . . . . ? O5 P3 C37 C38 -48.3(6) . . . . ? C43 P3 C37 C38 74.7(5) . . . . ? C49 P3 C37 C38 -173.2(5) . . . . ? C42 C37 C38 C39 0.5(11) . . . . ? P3 C37 C38 C39 -177.9(6) . . . . ? C37 C38 C39 C40 -0.1(13) . . . . ? C38 C39 C40 C41 -0.4(14) . . . . ? C39 C40 C41 C42 0.6(14) . . . . ? C38 C37 C42 C41 -0.3(10) . . . . ? P3 C37 C42 C41 177.8(6) . . . . ? C40 C41 C42 C37 -0.2(12) . . . . ? O5 P3 C43 C44 131.5(6) . . . . ? C37 P3 C43 C44 9.6(6) . . . . ? C49 P3 C43 C44 -108.3(6) . . . . ? O5 P3 C43 C48 -53.3(6) . . . . ? C37 P3 C43 C48 -175.2(5) . . . . ? C49 P3 C43 C48 66.9(5) . . . . ? C48 C43 C44 C45 0.1(11) . . . . ? P3 C43 C44 C45 175.3(7) . . . . ? C43 C44 C45 C46 -0.7(14) . . . . ? C44 C45 C46 C47 0.6(14) . . . . ? C45 C46 C47 C48 0.0(13) . . . . ? C46 C47 C48 C43 -0.5(11) . . . . ? C44 C43 C48 C47 0.4(10) . . . . ? P3 C43 C48 C47 -174.9(5) . . . . ? O5 P3 C49 C54 -5.2(6) . . . . ? C37 P3 C49 C54 119.9(5) . . . . ? C43 P3 C49 C54 -126.9(5) . . . . ? O5 P3 C49 C50 169.2(5) . . . . ? C37 P3 C49 C50 -65.7(6) . . . . ? C43 P3 C49 C50 47.5(6) . . . . ? C54 C49 C50 C51 -1.1(10) . . . . ? P3 C49 C50 C51 -175.4(5) . . . . ? C49 C50 C51 C52 0.0(11) . . . . ? C50 C51 C52 C53 1.4(11) . . . . ? C51 C52 C53 C54 -1.5(11) . . . . ? C50 C49 C54 C53 0.9(10) . . . . ? P3 C49 C54 C53 175.3(5) . . . . ? C52 C53 C54 C49 0.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.854 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.854 _refine_diff_density_max 2.932 _refine_diff_density_min -4.106 _refine_diff_density_rms 0.126 data_s836 _database_code_depnum_ccdc_archive 'CCDC 222069' #------------------------------------------------------------------------------ _audit_creation_date 19100-08-18 _audit_creation_method 'by teXsan v1.7' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_section_exptl_refinement ; The data were collected using the RAXIS in 90 x 3.0 degree phi oscillations, of 5 minutes per exposure. The asymmetric unit consists of half the molecule, with the other half generated by a centre of symmetry. O6 and its symmetry related equivalent in the same molecule, is within bonding distance at 1.489(9) A. All non-H atoms were refined anisotropically and H atoms were included in calculated positions. ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H45 O10 P3 Re U' _chemical_formula_weight 1371.04 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' P P 0.1023 0.0942 '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' 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 triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.624(2) _cell_length_b 16.507(3) _cell_length_c 17.381(3) _cell_angle_alpha 66.424(10) _cell_angle_beta 85.365(10) _cell_angle_gamma 77.024(10) _cell_volume 2722.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1322 _exptl_absorpt_coefficient_mu 5.334 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXIS' _diffrn_measurement_method '90 x 3.0 degree phi scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 41654 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 29.13 _reflns_number_total 10533 _reflns_number_gt 8980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1995)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'teXsan (MSC, 1995)' _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 w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+4.9268P] 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 SHELXL _refine_ls_extinction_coef 0.0079(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10533 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1482 _refine_ls_wR_factor_gt 0.1413 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.007 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.92122(2) 0.058472(16) 0.092394(14) 0.03932(12) Uani 1 d . . . P1 P 1.15103(17) -0.10541(13) 0.26906(11) 0.0457(4) Uani 1 d . . . P2 P 0.80472(18) 0.29688(12) -0.05636(12) 0.0463(4) Uani 1 d . . . P3 P 0.69682(19) 0.13750(14) 0.23736(12) 0.0501(4) Uani 1 d . . . O1 O 1.0366(5) -0.0602(3) 0.2094(3) 0.0509(11) Uani 1 d . . . O2 O 0.8058(5) 0.1984(3) -0.0050(3) 0.0508(11) Uani 1 d . . . O3 O 0.8181(5) 0.1171(4) 0.1900(3) 0.0541(12) Uani 1 d . . . O4 O 0.7889(5) 0.0057(4) 0.1071(4) 0.0587(13) Uani 1 d . . . O5 O 1.0510(5) 0.1144(4) 0.0808(3) 0.0529(12) Uani 1 d . . . O6 O 1.0362(5) -0.0405(3) 0.0344(3) 0.0557(13) Uani 1 d . . . C1 C 1.1478(8) -0.2223(6) 0.3295(5) 0.0543(18) Uani 1 d . . . C2 C 1.0581(9) -0.2448(7) 0.3931(6) 0.075(3) Uani 1 d . . . H2 H 1.0066 -0.2003 0.4085 0.090 Uiso 1 calc R . . C3 C 1.0455(12) -0.3346(8) 0.4337(7) 0.091(3) Uani 1 d . . . H3 H 0.9835 -0.3499 0.4749 0.109 Uiso 1 calc R . . C4 C 1.1245(13) -0.3996(8) 0.4127(8) 0.094(3) Uani 1 d . . . H4 H 1.1183 -0.4596 0.4419 0.113 Uiso 1 calc R . . C5 C 1.2131(11) -0.3791(7) 0.3497(7) 0.085(3) Uani 1 d . . . H5 H 1.2638 -0.4241 0.3347 0.102 Uiso 1 calc R . . C6 C 1.2255(9) -0.2912(6) 0.3095(6) 0.066(2) Uani 1 d . . . H6 H 1.2871 -0.2771 0.2677 0.079 Uiso 1 calc R . . C7 C 1.3031(7) -0.1024(5) 0.2147(5) 0.0494(16) Uani 1 d . . . C8 C 1.4158(9) -0.1199(7) 0.2576(6) 0.069(2) Uani 1 d . . . H8 H 1.4137 -0.1326 0.3148 0.083 Uiso 1 calc R . . C9 C 1.5334(9) -0.1187(8) 0.2155(7) 0.080(3) Uani 1 d . . . H9 H 1.6096 -0.1317 0.2450 0.096 Uiso 1 calc R . . C10 C 1.5370(9) -0.0990(7) 0.1324(6) 0.072(2) Uani 1 d . . . H10 H 1.6157 -0.0974 0.1047 0.087 Uiso 1 calc R . . C11 C 1.4273(9) -0.0813(6) 0.0887(6) 0.065(2) Uani 1 d . . . H11 H 1.4312 -0.0676 0.0313 0.078 Uiso 1 calc R . . C12 C 1.3090(8) -0.0835(6) 0.1289(5) 0.0563(18) Uani 1 d . . . H12 H 1.2341 -0.0724 0.0988 0.068 Uiso 1 calc R . . C13 C 1.1507(8) -0.0471(6) 0.3368(5) 0.0559(18) Uani 1 d . . . C14 C 1.1419(13) 0.0422(8) 0.2990(8) 0.099(4) Uani 1 d . . . H14 H 1.1340 0.0705 0.2409 0.119 Uiso 1 calc R . . C15 C 1.1445(17) 0.0939(9) 0.3462(11) 0.144(7) Uani 1 d . . . H15 H 1.1393 0.1559 0.3191 0.172 Uiso 1 calc R . . C16 C 1.1545(12) 0.0539(10) 0.4314(10) 0.108(5) Uani 1 d . . . H16 H 1.1532 0.0885 0.4627 0.130 Uiso 1 calc R . . C17 C 1.1661(11) -0.0359(11) 0.4700(7) 0.095(4) Uani 1 d . . . H17 H 1.1737 -0.0634 0.5281 0.114 Uiso 1 calc R . . C18 C 1.1670(9) -0.0891(7) 0.4235(5) 0.072(2) Uani 1 d . . . H18 H 1.1784 -0.1516 0.4505 0.086 Uiso 1 calc R . . C19 C 0.6550(7) 0.3489(5) -0.1149(5) 0.0517(17) Uani 1 d . . . C20 C 0.5602(9) 0.3011(7) -0.1001(7) 0.074(2) Uani 1 d . . . H20 H 0.5732 0.2429 -0.0587 0.089 Uiso 1 calc R . . C21 C 0.4448(10) 0.3370(8) -0.1452(8) 0.090(3) Uani 1 d . . . H21 H 0.3816 0.3031 -0.1347 0.108 Uiso 1 calc R . . C22 C 0.4260(11) 0.4230(10) -0.2053(7) 0.096(4) Uani 1 d . . . H22 H 0.3490 0.4479 -0.2359 0.115 Uiso 1 calc R . . C23 C 0.5190(12) 0.4729(8) -0.2209(7) 0.095(3) Uani 1 d . . . H23 H 0.5050 0.5316 -0.2617 0.114 Uiso 1 calc R . . C24 C 0.6325(10) 0.4362(7) -0.1764(6) 0.079(3) Uani 1 d . . . H24 H 0.6957 0.4703 -0.1874 0.094 Uiso 1 calc R . . C25 C 0.8178(9) 0.3599(6) 0.0054(5) 0.0594(19) Uani 1 d . . . C26 C 0.7145(11) 0.4173(7) 0.0211(7) 0.081(3) Uani 1 d . . . H26 H 0.6338 0.4236 -0.0003 0.097 Uiso 1 calc R . . C27 C 0.7259(14) 0.4661(9) 0.0678(8) 0.104(4) Uani 1 d . . . H27 H 0.6536 0.5041 0.0780 0.125 Uiso 1 calc R . . C28 C 0.8421(17) 0.4585(9) 0.0982(9) 0.112(5) Uani 1 d . . . H28 H 0.8505 0.4920 0.1289 0.134 Uiso 1 calc R . . C29 C 0.9475(15) 0.4020(10) 0.0845(9) 0.111(4) Uani 1 d . . . H29 H 1.0279 0.3979 0.1050 0.134 Uiso 1 calc R . . C30 C 0.9361(10) 0.3495(8) 0.0396(7) 0.088(3) Uani 1 d . . . H30 H 1.0074 0.3084 0.0329 0.105 Uiso 1 calc R . . C31 C 0.9352(7) 0.3121(5) -0.1293(5) 0.0519(17) Uani 1 d . . . C32 C 0.9679(9) 0.3963(6) -0.1699(6) 0.069(2) Uani 1 d . . . H32 H 0.9256 0.4450 -0.1569 0.082 Uiso 1 calc R . . C33 C 1.0649(10) 0.4067(8) -0.2303(7) 0.084(3) Uani 1 d . . . H33 H 1.0867 0.4627 -0.2585 0.101 Uiso 1 calc R . . C34 C 1.1285(10) 0.3331(9) -0.2481(7) 0.090(3) Uani 1 d . . . H34 H 1.1937 0.3400 -0.2878 0.108 Uiso 1 calc R . . C35 C 1.0971(10) 0.2520(8) -0.2085(7) 0.083(3) Uani 1 d . . . H35 H 1.1410 0.2034 -0.2211 0.100 Uiso 1 calc R . . C36 C 1.0005(9) 0.2396(6) -0.1493(6) 0.065(2) Uani 1 d . . . H36 H 0.9790 0.1833 -0.1229 0.078 Uiso 1 calc R . . C37 C 0.6608(7) 0.0360(6) 0.3166(4) 0.0506(17) Uani 1 d . . . C38 C 0.5387(9) 0.0373(7) 0.3543(6) 0.074(2) Uani 1 d . . . H38 H 0.4753 0.0901 0.3367 0.088 Uiso 1 calc R . . C39 C 0.5135(10) -0.0413(9) 0.4182(7) 0.082(3) Uani 1 d . . . H39 H 0.4339 -0.0399 0.4447 0.099 Uiso 1 calc R . . C40 C 0.6041(10) -0.1205(8) 0.4425(6) 0.078(3) Uani 1 d . . . H40 H 0.5867 -0.1731 0.4847 0.094 Uiso 1 calc R . . C41 C 0.7229(10) -0.1203(7) 0.4025(7) 0.083(3) Uani 1 d . . . H41 H 0.7849 -0.1739 0.4181 0.099 Uiso 1 calc R . . C42 C 0.7519(9) -0.0436(6) 0.3407(5) 0.066(2) Uani 1 d . . . H42 H 0.8324 -0.0455 0.3153 0.079 Uiso 1 calc R . . C43 C 0.5543(7) 0.1916(6) 0.1722(5) 0.0574(19) Uani 1 d . . . C44 C 0.4905(11) 0.2770(8) 0.1575(7) 0.090(3) Uani 1 d . . . H44 H 0.5206 0.3096 0.1824 0.108 Uiso 1 calc R . . C45 C 0.3802(14) 0.3177(12) 0.1059(9) 0.132(6) Uani 1 d . . . H45 H 0.3461 0.3794 0.0880 0.158 Uiso 1 calc R . . C46 C 0.3230(13) 0.2625(12) 0.0819(10) 0.125(6) Uani 1 d . . . H46 H 0.2426 0.2853 0.0553 0.150 Uiso 1 calc R . . C47 C 0.3861(13) 0.1737(12) 0.0978(9) 0.122(5) Uani 1 d . . . H47 H 0.3501 0.1380 0.0795 0.147 Uiso 1 calc R . . C48 C 0.5053(11) 0.1382(8) 0.1417(7) 0.085(3) Uani 1 d . . . H48 H 0.5505 0.0801 0.1502 0.102 Uiso 1 calc R . . C49 C 0.7218(8) 0.2098(6) 0.2882(5) 0.0581(19) Uani 1 d . . . C50 C 0.6315(12) 0.2316(8) 0.3425(7) 0.085(3) Uani 1 d . . . H50 H 0.5541 0.2119 0.3521 0.102 Uiso 1 calc R . . C51 C 0.6592(14) 0.2841(8) 0.3828(7) 0.100(4) Uani 1 d . . . H51 H 0.6006 0.2970 0.4211 0.119 Uiso 1 calc R . . C52 C 0.7680(15) 0.3162(8) 0.3675(8) 0.103(4) Uani 1 d . . . H52 H 0.7845 0.3498 0.3961 0.123 Uiso 1 calc R . . C53 C 0.8568(15) 0.2995(10) 0.3089(10) 0.125(5) Uani 1 d . . . H53 H 0.9299 0.3244 0.2950 0.150 Uiso 1 calc R . . C54 C 0.8301(11) 0.2426(8) 0.2716(8) 0.092(3) Uani 1 d . . . H54 H 0.8895 0.2276 0.2346 0.111 Uiso 1 calc R . . Re1 Re 1.22073(5) 0.33482(3) 0.34196(3) 0.08501(16) Uani 1 d . . . O7 O 1.1110(12) 0.2940(12) 0.4108(9) 0.195(6) Uani 1 d . . . O8 O 1.1553(13) 0.3880(7) 0.2461(6) 0.150(4) Uani 1 d . . . O9 O 1.302(2) 0.3956(12) 0.3647(11) 0.243(9) Uani 1 d . . . O10 O 1.3259(12) 0.2360(8) 0.3493(8) 0.163(5) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.04090(17) 0.04112(17) 0.04018(17) -0.02382(11) -0.00415(9) -0.00042(9) P1 0.0449(10) 0.0511(10) 0.0399(9) -0.0213(8) -0.0052(6) 0.0003(7) P2 0.0475(10) 0.0418(9) 0.0517(10) -0.0245(8) -0.0067(7) 0.0009(7) P3 0.0503(11) 0.0558(11) 0.0468(10) -0.0295(9) 0.0023(7) 0.0005(8) O1 0.051(3) 0.054(3) 0.045(3) -0.023(2) -0.008(2) 0.003(2) O2 0.054(3) 0.044(3) 0.052(3) -0.020(2) -0.006(2) 0.000(2) O3 0.057(3) 0.058(3) 0.050(3) -0.032(3) 0.007(2) 0.002(2) O4 0.052(3) 0.059(3) 0.066(3) -0.028(3) -0.008(2) -0.006(2) O5 0.049(3) 0.065(3) 0.049(3) -0.030(3) -0.002(2) -0.006(2) O6 0.071(3) 0.056(3) 0.037(3) -0.029(2) -0.012(2) 0.019(2) C1 0.051(4) 0.059(5) 0.050(4) -0.023(4) -0.006(3) -0.001(3) C2 0.070(6) 0.073(6) 0.077(6) -0.031(5) 0.015(4) -0.005(4) C3 0.096(8) 0.078(7) 0.080(7) -0.013(6) 0.021(6) -0.022(6) C4 0.122(10) 0.061(6) 0.089(8) -0.018(6) 0.003(7) -0.021(6) C5 0.092(8) 0.060(6) 0.100(8) -0.037(6) 0.006(6) -0.004(5) C6 0.068(6) 0.062(5) 0.060(5) -0.023(4) 0.005(4) -0.002(4) C7 0.046(4) 0.051(4) 0.047(4) -0.019(3) -0.005(3) -0.002(3) C8 0.057(5) 0.097(7) 0.064(5) -0.041(5) -0.005(4) -0.017(4) C9 0.048(6) 0.110(8) 0.092(7) -0.048(6) -0.003(4) -0.019(5) C10 0.059(6) 0.078(6) 0.088(7) -0.040(5) 0.016(4) -0.020(4) C11 0.063(5) 0.077(6) 0.056(5) -0.029(4) 0.013(4) -0.015(4) C12 0.052(5) 0.067(5) 0.055(5) -0.030(4) -0.003(3) -0.009(3) C13 0.053(5) 0.065(5) 0.054(4) -0.034(4) -0.007(3) 0.000(3) C14 0.129(10) 0.087(8) 0.095(8) -0.053(7) -0.046(7) -0.001(7) C15 0.198(16) 0.092(9) 0.169(14) -0.088(10) -0.104(12) 0.022(9) C16 0.094(9) 0.130(11) 0.141(12) -0.107(10) -0.039(7) 0.014(7) C17 0.077(7) 0.170(13) 0.064(6) -0.076(8) 0.003(5) -0.023(7) C18 0.075(6) 0.097(7) 0.051(5) -0.039(5) -0.002(4) -0.014(5) C19 0.053(4) 0.052(4) 0.053(4) -0.028(4) -0.002(3) 0.001(3) C20 0.067(6) 0.067(6) 0.088(7) -0.029(5) -0.018(5) -0.008(4) C21 0.063(7) 0.099(8) 0.114(9) -0.047(7) -0.028(6) -0.008(5) C22 0.061(7) 0.136(11) 0.087(8) -0.059(8) -0.022(5) 0.023(6) C23 0.081(8) 0.078(7) 0.091(8) -0.012(6) -0.021(6) 0.018(6) C24 0.072(6) 0.071(6) 0.064(6) -0.005(5) -0.010(4) 0.003(5) C25 0.070(5) 0.056(5) 0.061(5) -0.035(4) 0.000(4) -0.010(4) C26 0.084(7) 0.084(7) 0.089(7) -0.061(6) -0.006(5) 0.007(5) C27 0.122(11) 0.106(9) 0.111(9) -0.084(8) -0.003(7) 0.004(7) C28 0.167(14) 0.097(9) 0.108(10) -0.073(8) 0.001(9) -0.036(9) C29 0.117(11) 0.142(12) 0.129(11) -0.097(10) -0.001(8) -0.049(9) C30 0.070(7) 0.121(9) 0.107(8) -0.080(8) -0.008(5) -0.018(6) C31 0.047(4) 0.052(4) 0.060(4) -0.029(4) -0.005(3) -0.002(3) C32 0.070(6) 0.062(5) 0.080(6) -0.030(5) 0.000(4) -0.022(4) C33 0.078(7) 0.090(7) 0.093(7) -0.034(6) 0.013(5) -0.043(6) C34 0.068(7) 0.119(10) 0.093(8) -0.051(7) 0.024(5) -0.031(6) C35 0.073(7) 0.096(8) 0.094(7) -0.057(7) 0.017(5) -0.010(5) C36 0.065(5) 0.063(5) 0.072(6) -0.037(5) 0.009(4) -0.007(4) C37 0.048(4) 0.067(5) 0.044(4) -0.031(4) 0.007(3) -0.010(3) C38 0.059(6) 0.080(6) 0.086(7) -0.045(5) 0.018(4) -0.005(4) C39 0.070(7) 0.112(9) 0.072(6) -0.042(6) 0.024(5) -0.032(6) C40 0.078(7) 0.087(7) 0.060(5) -0.013(5) 0.000(4) -0.028(5) C41 0.059(6) 0.075(7) 0.086(7) -0.009(5) -0.002(4) 0.002(4) C42 0.057(5) 0.073(6) 0.055(5) -0.017(4) 0.005(3) -0.005(4) C43 0.048(4) 0.069(5) 0.051(4) -0.027(4) 0.003(3) 0.001(3) C44 0.095(8) 0.087(7) 0.078(7) -0.041(6) -0.020(5) 0.023(6) C45 0.101(11) 0.151(14) 0.114(10) -0.060(10) -0.027(8) 0.055(9) C46 0.066(9) 0.174(15) 0.132(12) -0.085(12) -0.032(7) 0.036(8) C47 0.072(9) 0.172(15) 0.111(10) -0.038(10) -0.021(7) -0.027(9) C48 0.082(7) 0.096(8) 0.076(6) -0.034(6) -0.021(5) -0.009(5) C49 0.062(5) 0.055(5) 0.062(5) -0.034(4) -0.001(3) -0.001(3) C50 0.099(8) 0.098(8) 0.084(7) -0.065(6) 0.014(6) -0.021(6) C51 0.127(11) 0.104(9) 0.089(8) -0.074(7) 0.002(7) 0.001(7) C52 0.139(12) 0.087(8) 0.102(9) -0.064(7) -0.031(8) 0.000(7) C53 0.117(11) 0.147(13) 0.161(14) -0.105(12) 0.006(9) -0.042(9) C54 0.078(7) 0.118(9) 0.118(9) -0.085(8) 0.010(6) -0.024(6) Re1 0.0880(3) 0.0844(3) 0.0792(3) -0.0277(2) -0.0060(2) -0.0175(2) O7 0.119(10) 0.32(2) 0.169(11) -0.138(13) 0.021(8) -0.025(10) O8 0.212(12) 0.109(7) 0.103(7) -0.042(6) -0.036(7) 0.030(7) O9 0.30(2) 0.187(14) 0.28(2) -0.102(14) -0.131(18) -0.053(14) O10 0.154(10) 0.118(8) 0.174(11) -0.041(8) -0.028(8) 0.034(7) _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 O4 1.765(6) . ? U1 O5 1.780(5) . ? U1 O6 2.324(4) . ? U1 O6 2.334(4) 2_755 ? U1 O3 2.357(4) . ? U1 O1 2.369(5) . ? U1 O2 2.375(5) . ? P1 O1 1.513(5) . ? P1 C13 1.794(7) . ? P1 C1 1.797(9) . ? P1 C7 1.804(8) . ? P2 O2 1.507(5) . ? P2 C31 1.792(8) . ? P2 C25 1.798(8) . ? P2 C19 1.803(8) . ? P3 O3 1.518(5) . ? P3 C37 1.792(8) . ? P3 C43 1.799(8) . ? P3 C49 1.816(8) . ? O6 O6 1.489(9) 2_755 ? O6 U1 2.334(4) 2_755 ? C1 C2 1.388(12) . ? C1 C6 1.396(11) . ? C2 C3 1.396(14) . ? C2 H2 0.9300 . ? C3 C4 1.359(16) . ? C3 H3 0.9300 . ? C4 C5 1.370(15) . ? C4 H4 0.9300 . ? C5 C6 1.367(13) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.375(11) . ? C7 C12 1.395(10) . ? C8 C9 1.396(13) . ? C8 H8 0.9300 . ? C9 C10 1.348(14) . ? C9 H9 0.9300 . ? C10 C11 1.354(13) . ? C10 H10 0.9300 . ? C11 C12 1.389(11) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.337(14) . ? C13 C18 1.390(11) . ? C14 C15 1.406(14) . ? C14 H14 0.9300 . ? C15 C16 1.36(2) . ? C15 H15 0.9300 . ? C16 C17 1.340(18) . ? C16 H16 0.9300 . ? C17 C18 1.410(14) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.362(12) . ? C19 C24 1.390(12) . ? C20 C21 1.388(13) . ? C20 H20 0.9300 . ? C21 C22 1.367(16) . ? C21 H21 0.9300 . ? C22 C23 1.368(17) . ? C22 H22 0.9300 . ? C23 C24 1.367(14) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.367(12) . ? C25 C30 1.380(13) . ? C26 C27 1.381(13) . ? C26 H26 0.9300 . ? C27 C28 1.342(18) . ? C27 H27 0.9300 . ? C28 C29 1.359(19) . ? C28 H28 0.9300 . ? C29 C30 1.406(14) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.394(11) . ? C31 C36 1.398(10) . ? C32 C33 1.398(13) . ? C32 H32 0.9300 . ? C33 C34 1.387(15) . ? C33 H33 0.9300 . ? C34 C35 1.343(15) . ? C34 H34 0.9300 . ? C35 C36 1.381(13) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C42 1.375(11) . ? C37 C38 1.404(11) . ? C38 C39 1.395(14) . ? C38 H38 0.9300 . ? C39 C40 1.368(15) . ? C39 H39 0.9300 . ? C40 C41 1.392(14) . ? C40 H40 0.9300 . ? C41 C42 1.373(13) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.350(13) . ? C43 C48 1.398(13) . ? C44 C45 1.402(16) . ? C44 H44 0.9300 . ? C45 C46 1.40(2) . ? C45 H45 0.9300 . ? C46 C47 1.39(2) . ? C46 H46 0.9300 . ? C47 C48 1.412(15) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C54 1.343(14) . ? C49 C50 1.382(12) . ? C50 C51 1.399(15) . ? C50 H50 0.9300 . ? C51 C52 1.342(18) . ? C51 H51 0.9300 . ? C52 C53 1.398(19) . ? C52 H52 0.9300 . ? C53 C54 1.421(15) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? Re1 O9 1.631(13) . ? Re1 O7 1.651(14) . ? Re1 O8 1.665(10) . ? Re1 O10 1.722(10) . ? 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 O4 U1 O5 177.2(2) . . ? O4 U1 O6 89.3(2) . . ? O5 U1 O6 93.4(2) . . ? O4 U1 O6 89.2(2) . 2_755 ? O5 U1 O6 93.4(2) . 2_755 ? O6 U1 O6 37.3(2) . 2_755 ? O4 U1 O3 85.4(2) . . ? O5 U1 O3 91.8(2) . . ? O6 U1 O3 161.89(18) . . ? O6 U1 O3 159.36(17) 2_755 . ? O4 U1 O1 93.2(2) . . ? O5 U1 O1 86.8(2) . . ? O6 U1 O1 77.19(16) . . ? O6 U1 O1 114.41(16) 2_755 . ? O3 U1 O1 85.80(17) . . ? O4 U1 O2 93.0(2) . . ? O5 U1 O2 86.4(2) . . ? O6 U1 O2 115.46(16) . . ? O6 U1 O2 78.24(16) 2_755 . ? O3 U1 O2 82.16(17) . . ? O1 U1 O2 165.99(17) . . ? O1 P1 C13 109.9(3) . . ? O1 P1 C1 110.5(3) . . ? C13 P1 C1 110.6(4) . . ? O1 P1 C7 112.3(3) . . ? C13 P1 C7 106.3(4) . . ? C1 P1 C7 107.1(4) . . ? O2 P2 C31 112.1(3) . . ? O2 P2 C25 113.8(4) . . ? C31 P2 C25 106.0(4) . . ? O2 P2 C19 109.1(3) . . ? C31 P2 C19 108.2(4) . . ? C25 P2 C19 107.4(4) . . ? O3 P3 C37 111.2(3) . . ? O3 P3 C43 113.9(3) . . ? C37 P3 C43 105.6(4) . . ? O3 P3 C49 109.0(4) . . ? C37 P3 C49 108.2(4) . . ? C43 P3 C49 108.7(4) . . ? P1 O1 U1 153.4(3) . . ? P2 O2 U1 146.7(3) . . ? P3 O3 U1 149.0(3) . . ? O6 O6 U1 71.8(3) 2_755 . ? O6 O6 U1 71.0(3) 2_755 2_755 ? U1 O6 U1 142.7(2) . 2_755 ? C2 C1 C6 118.5(8) . . ? C2 C1 P1 119.7(6) . . ? C6 C1 P1 121.6(6) . . ? C1 C2 C3 119.7(9) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 119.6(10) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 121.8(10) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 118.8(9) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? C5 C6 C1 121.5(9) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? C8 C7 C12 118.7(7) . . ? C8 C7 P1 120.4(6) . . ? C12 C7 P1 120.9(6) . . ? C7 C8 C9 120.2(8) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 120.2(9) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.7(8) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 120.5(8) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 119.7(7) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C14 C13 C18 119.2(8) . . ? C14 C13 P1 116.2(7) . . ? C18 C13 P1 124.5(7) . . ? C13 C14 C15 120.7(12) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 120.5(13) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 119.4(10) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 120.9(10) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C13 C18 C17 119.2(10) . . ? C13 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C20 C19 C24 117.9(8) . . ? C20 C19 P2 119.5(7) . . ? C24 C19 P2 122.5(7) . . ? C19 C20 C21 121.8(10) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C22 C21 C20 118.7(11) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C21 C22 C23 120.8(9) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 119.7(11) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C19 121.0(11) . . ? C23 C24 H24 119.5 . . ? C19 C24 H24 119.5 . . ? C26 C25 C30 118.1(8) . . ? C26 C25 P2 122.7(7) . . ? C30 C25 P2 119.2(7) . . ? C25 C26 C27 122.2(11) . . ? C25 C26 H26 118.9 . . ? C27 C26 H26 118.9 . . ? C28 C27 C26 119.5(11) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 120.4(11) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C30 120.5(12) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C25 C30 C29 119.1(11) . . ? C25 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C32 C31 C36 119.5(8) . . ? C32 C31 P2 121.0(6) . . ? C36 C31 P2 119.4(6) . . ? C31 C32 C33 119.2(9) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 119.8(10) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C35 C34 C33 120.7(10) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 121.0(10) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 119.7(9) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C42 C37 C38 119.6(8) . . ? C42 C37 P3 120.4(6) . . ? C38 C37 P3 119.9(7) . . ? C39 C38 C37 119.4(9) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C40 C39 C38 121.0(9) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C39 C40 C41 118.2(9) . . ? C39 C40 H40 120.9 . . ? C41 C40 H40 120.9 . . ? C42 C41 C40 122.2(9) . . ? C42 C41 H41 118.9 . . ? C40 C41 H41 118.9 . . ? C41 C42 C37 119.5(8) . . ? C41 C42 H42 120.3 . . ? C37 C42 H42 120.3 . . ? C44 C43 C48 120.4(9) . . ? C44 C43 P3 123.0(8) . . ? C48 C43 P3 116.4(7) . . ? C43 C44 C45 121.8(13) . . ? C43 C44 H44 119.1 . . ? C45 C44 H44 119.1 . . ? C44 C45 C46 117.9(14) . . ? C44 C45 H45 121.0 . . ? C46 C45 H45 121.0 . . ? C47 C46 C45 120.2(12) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C46 C47 C48 119.6(15) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? C43 C48 C47 119.1(12) . . ? C43 C48 H48 120.4 . . ? C47 C48 H48 120.4 . . ? C54 C49 C50 120.1(9) . . ? C54 C49 P3 118.6(7) . . ? C50 C49 P3 121.3(8) . . ? C49 C50 C51 118.5(11) . . ? C49 C50 H50 120.7 . . ? C51 C50 H50 120.7 . . ? C52 C51 C50 121.8(11) . . ? C52 C51 H51 119.1 . . ? C50 C51 H51 119.1 . . ? C51 C52 C53 120.5(10) . . ? C51 C52 H52 119.7 . . ? C53 C52 H52 119.7 . . ? C52 C53 C54 116.9(13) . . ? C52 C53 H53 121.6 . . ? C54 C53 H53 121.6 . . ? C49 C54 C53 122.0(11) . . ? C49 C54 H54 119.0 . . ? C53 C54 H54 119.0 . . ? O9 Re1 O7 115.9(9) . . ? O9 Re1 O8 112.3(8) . . ? O7 Re1 O8 110.0(7) . . ? O9 Re1 O10 107.7(9) . . ? O7 Re1 O10 100.4(7) . . ? O8 Re1 O10 109.9(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 P1 O1 U1 72.3(7) . . . . ? C1 P1 O1 U1 -165.4(6) . . . . ? C7 P1 O1 U1 -45.8(7) . . . . ? O4 U1 O1 P1 -179.1(7) . . . . ? O5 U1 O1 P1 -1.9(6) . . . . ? O6 U1 O1 P1 92.3(7) . . . . ? O6 U1 O1 P1 90.3(7) 2_755 . . . ? O3 U1 O1 P1 -94.0(6) . . . . ? O2 U1 O1 P1 -63.1(11) . . . . ? C31 P2 O2 U1 60.5(6) . . . . ? C25 P2 O2 U1 -59.8(6) . . . . ? C19 P2 O2 U1 -179.6(5) . . . . ? O4 U1 O2 P2 172.0(6) . . . . ? O5 U1 O2 P2 -5.3(5) . . . . ? O6 U1 O2 P2 -97.4(6) . . . . ? O6 U1 O2 P2 -99.5(6) 2_755 . . . ? O3 U1 O2 P2 87.0(5) . . . . ? O1 U1 O2 P2 55.9(10) . . . . ? C37 P3 O3 U1 72.1(7) . . . . ? C43 P3 O3 U1 -47.0(7) . . . . ? C49 P3 O3 U1 -168.6(6) . . . . ? O4 U1 O3 P3 -16.5(6) . . . . ? O5 U1 O3 P3 163.3(6) . . . . ? O6 U1 O3 P3 -90.0(8) . . . . ? O6 U1 O3 P3 58.8(10) 2_755 . . . ? O1 U1 O3 P3 -110.0(6) . . . . ? O2 U1 O3 P3 77.2(6) . . . . ? O4 U1 O6 O6 89.5(5) . . . 2_755 ? O5 U1 O6 O6 -91.1(5) . . . 2_755 ? O3 U1 O6 O6 162.5(5) . . . 2_755 ? O1 U1 O6 O6 -177.1(5) . . . 2_755 ? O2 U1 O6 O6 -3.5(5) . . . 2_755 ? O4 U1 O6 U1 89.5(5) . . . 2_755 ? O5 U1 O6 U1 -91.1(5) . . . 2_755 ? O6 U1 O6 U1 0.000(1) 2_755 . . 2_755 ? O3 U1 O6 U1 162.5(5) . . . 2_755 ? O1 U1 O6 U1 -177.1(5) . . . 2_755 ? O2 U1 O6 U1 -3.5(5) . . . 2_755 ? O1 P1 C1 C2 -73.1(8) . . . . ? C13 P1 C1 C2 48.9(8) . . . . ? C7 P1 C1 C2 164.3(7) . . . . ? O1 P1 C1 C6 101.0(7) . . . . ? C13 P1 C1 C6 -137.0(7) . . . . ? C7 P1 C1 C6 -21.6(8) . . . . ? C6 C1 C2 C3 -1.5(15) . . . . ? P1 C1 C2 C3 172.7(8) . . . . ? C1 C2 C3 C4 2.4(18) . . . . ? C2 C3 C4 C5 -3(2) . . . . ? C3 C4 C5 C6 3(2) . . . . ? C4 C5 C6 C1 -1.8(16) . . . . ? C2 C1 C6 C5 1.3(14) . . . . ? P1 C1 C6 C5 -172.9(8) . . . . ? O1 P1 C7 C8 164.2(7) . . . . ? C13 P1 C7 C8 44.0(8) . . . . ? C1 P1 C7 C8 -74.2(8) . . . . ? O1 P1 C7 C12 -16.6(8) . . . . ? C13 P1 C7 C12 -136.8(7) . . . . ? C1 P1 C7 C12 105.0(7) . . . . ? C12 C7 C8 C9 -0.1(14) . . . . ? P1 C7 C8 C9 179.1(8) . . . . ? C7 C8 C9 C10 1.1(16) . . . . ? C8 C9 C10 C11 -1.0(16) . . . . ? C9 C10 C11 C12 -0.2(15) . . . . ? C10 C11 C12 C7 1.2(13) . . . . ? C8 C7 C12 C11 -1.0(12) . . . . ? P1 C7 C12 C11 179.8(7) . . . . ? O1 P1 C13 C14 -52.2(9) . . . . ? C1 P1 C13 C14 -174.5(8) . . . . ? C7 P1 C13 C14 69.5(8) . . . . ? O1 P1 C13 C18 132.1(7) . . . . ? C1 P1 C13 C18 9.8(9) . . . . ? C7 P1 C13 C18 -106.2(8) . . . . ? C18 C13 C14 C15 -2.3(18) . . . . ? P1 C13 C14 C15 -178.2(11) . . . . ? C13 C14 C15 C16 -1(2) . . . . ? C14 C15 C16 C17 2(2) . . . . ? C15 C16 C17 C18 -0.6(19) . . . . ? C14 C13 C18 C17 3.8(14) . . . . ? P1 C13 C18 C17 179.4(7) . . . . ? C16 C17 C18 C13 -2.4(16) . . . . ? O2 P2 C19 C20 7.5(8) . . . . ? C31 P2 C19 C20 129.7(7) . . . . ? C25 P2 C19 C20 -116.2(7) . . . . ? O2 P2 C19 C24 -171.3(7) . . . . ? C31 P2 C19 C24 -49.1(8) . . . . ? C25 P2 C19 C24 65.0(8) . . . . ? C24 C19 C20 C21 0.8(14) . . . . ? P2 C19 C20 C21 -178.0(8) . . . . ? C19 C20 C21 C22 -0.7(17) . . . . ? C20 C21 C22 C23 0.1(17) . . . . ? C21 C22 C23 C24 0.4(18) . . . . ? C22 C23 C24 C19 -0.3(17) . . . . ? C20 C19 C24 C23 -0.3(14) . . . . ? P2 C19 C24 C23 178.5(8) . . . . ? O2 P2 C25 C26 -103.7(9) . . . . ? C31 P2 C25 C26 132.7(9) . . . . ? C19 P2 C25 C26 17.1(10) . . . . ? O2 P2 C25 C30 75.5(9) . . . . ? C31 P2 C25 C30 -48.2(9) . . . . ? C19 P2 C25 C30 -163.7(8) . . . . ? C30 C25 C26 C27 1.7(17) . . . . ? P2 C25 C26 C27 -179.2(10) . . . . ? C25 C26 C27 C28 1(2) . . . . ? C26 C27 C28 C29 -1(2) . . . . ? C27 C28 C29 C30 -1(2) . . . . ? C26 C25 C30 C29 -3.8(17) . . . . ? P2 C25 C30 C29 177.0(10) . . . . ? C28 C29 C30 C25 4(2) . . . . ? O2 P2 C31 C32 -166.4(6) . . . . ? C25 P2 C31 C32 -41.7(8) . . . . ? C19 P2 C31 C32 73.3(7) . . . . ? O2 P2 C31 C36 17.2(8) . . . . ? C25 P2 C31 C36 141.9(7) . . . . ? C19 P2 C31 C36 -103.1(7) . . . . ? C36 C31 C32 C33 0.4(13) . . . . ? P2 C31 C32 C33 -176.0(7) . . . . ? C31 C32 C33 C34 -1.0(16) . . . . ? C32 C33 C34 C35 0.7(18) . . . . ? C33 C34 C35 C36 0.2(19) . . . . ? C34 C35 C36 C31 -0.8(17) . . . . ? C32 C31 C36 C35 0.5(14) . . . . ? P2 C31 C36 C35 176.9(8) . . . . ? O3 P3 C37 C42 14.1(8) . . . . ? C43 P3 C37 C42 138.1(7) . . . . ? C49 P3 C37 C42 -105.6(7) . . . . ? O3 P3 C37 C38 -165.6(7) . . . . ? C43 P3 C37 C38 -41.6(8) . . . . ? C49 P3 C37 C38 74.7(8) . . . . ? C42 C37 C38 C39 2.8(14) . . . . ? P3 C37 C38 C39 -177.5(7) . . . . ? C37 C38 C39 C40 -2.6(15) . . . . ? C38 C39 C40 C41 0.9(16) . . . . ? C39 C40 C41 C42 0.7(17) . . . . ? C40 C41 C42 C37 -0.4(16) . . . . ? C38 C37 C42 C41 -1.3(14) . . . . ? P3 C37 C42 C41 179.0(8) . . . . ? O3 P3 C43 C44 -114.0(9) . . . . ? C37 P3 C43 C44 123.8(9) . . . . ? C49 P3 C43 C44 7.8(10) . . . . ? O3 P3 C43 C48 70.9(8) . . . . ? C37 P3 C43 C48 -51.4(8) . . . . ? C49 P3 C43 C48 -167.4(7) . . . . ? C48 C43 C44 C45 -5.5(18) . . . . ? P3 C43 C44 C45 179.5(10) . . . . ? C43 C44 C45 C46 12(2) . . . . ? C44 C45 C46 C47 -10(2) . . . . ? C45 C46 C47 C48 3(2) . . . . ? C44 C43 C48 C47 -2.0(16) . . . . ? P3 C43 C48 C47 173.3(9) . . . . ? C46 C47 C48 C43 3(2) . . . . ? O3 P3 C49 C54 7.0(9) . . . . ? C37 P3 C49 C54 128.0(9) . . . . ? C43 P3 C49 C54 -117.7(9) . . . . ? O3 P3 C49 C50 -173.5(8) . . . . ? C37 P3 C49 C50 -52.4(9) . . . . ? C43 P3 C49 C50 61.8(9) . . . . ? C54 C49 C50 C51 -3.4(17) . . . . ? P3 C49 C50 C51 177.0(9) . . . . ? C49 C50 C51 C52 2.6(19) . . . . ? C50 C51 C52 C53 1(2) . . . . ? C51 C52 C53 C54 -4(2) . . . . ? C50 C49 C54 C53 0.5(19) . . . . ? P3 C49 C54 C53 -180.0(11) . . . . ? C52 C53 C54 C49 3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.719 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.719 _refine_diff_density_max 3.188 _refine_diff_density_min -2.561 _refine_diff_density_rms 0.154 data_s1263abs _database_code_depnum_ccdc_archive 'CCDC 222070' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains half the molecule. The Re atom lies on a centre of symmetry, and the O atoms are therefore disordered over 2 sites each at an occupancy of 0.5. The structure was also solved in the space group P1, and the ReO4 group was ordered in this space group. However, due to the correlations between coefficients, restraints were required on the thermal motion, and constraints on the bond lengths of the Ph groups, and high damping was also needed, Therefore, P-1 was chosen as the optimum space group. The non-H atoms were refined anisotropically. H atoms bonded were included in calculated positions. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H60 Np O10 P4 Re' _chemical_formula_weight 1632.28 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' Np Np -11.4937 4.1493 '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 9.066(5) _cell_length_b 13.361(5) _cell_length_c 13.894(5) _cell_angle_alpha 97.865(5) _cell_angle_beta 107.949(5) _cell_angle_gamma 91.510(5) _cell_volume 1581.8(12) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7134 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.38 _exptl_crystal_description irregular _exptl_crystal_colour 'very pale green' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 3.707 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5244 _exptl_absorpt_correction_T_max 0.6647 _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 12783 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.39 _reflns_number_total 6401 _reflns_number_gt 5725 _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^)+(0.0179P)^2^+1.7986P] 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 6401 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0482 _refine_ls_wR_factor_gt 0.0468 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Np1 Np 1.0000 0.0000 1.0000 0.00990(4) Uani 1 2 d S . . P1 P 1.15146(7) 0.26560(5) 1.05033(5) 0.01225(13) Uani 1 1 d . . . P2 P 0.75058(7) 0.03956(5) 0.73750(5) 0.01202(13) Uani 1 1 d . . . O1 O 1.1635(2) 0.15712(13) 1.06788(13) 0.0145(4) Uani 1 1 d . . . O2 O 0.8722(2) 0.06297(13) 0.84043(13) 0.0148(4) Uani 1 1 d . . . O3 O 0.8557(2) 0.05293(13) 1.05343(13) 0.0153(4) Uani 1 1 d . . . C1 C 1.1850(3) 0.27871(19) 0.93164(19) 0.0138(5) Uani 1 1 d . . . C2 C 1.1652(3) 0.3678(2) 0.8889(2) 0.0200(6) Uani 1 1 d . . . H2 H 1.1270 0.4228 0.9199 0.024 Uiso 1 1 calc R . . C3 C 1.2022(3) 0.3747(2) 0.8001(2) 0.0230(6) Uani 1 1 d . . . H3 H 1.1887 0.4341 0.7716 0.028 Uiso 1 1 calc R . . C4 C 1.2594(3) 0.2927(2) 0.7541(2) 0.0220(6) Uani 1 1 d . . . H4 H 1.2844 0.2975 0.6948 0.026 Uiso 1 1 calc R . . C5 C 1.2796(3) 0.2041(2) 0.7956(2) 0.0219(6) Uani 1 1 d . . . H5 H 1.3185 0.1495 0.7644 0.026 Uiso 1 1 calc R . . C6 C 1.2417(3) 0.1963(2) 0.8844(2) 0.0176(5) Uani 1 1 d . . . H6 H 1.2541 0.1363 0.9121 0.021 Uiso 1 1 calc R . . C7 C 1.2967(3) 0.34634(19) 1.15062(19) 0.0150(5) Uani 1 1 d . . . C8 C 1.3002(3) 0.4512(2) 1.1566(2) 0.0212(6) Uani 1 1 d . . . H8 H 1.2245 0.4810 1.1096 0.025 Uiso 1 1 calc R . . C9 C 1.4172(3) 0.5111(2) 1.2330(2) 0.0243(6) Uani 1 1 d . . . H9 H 1.4206 0.5812 1.2369 0.029 Uiso 1 1 calc R . . C10 C 1.5290(3) 0.4669(2) 1.3035(2) 0.0247(6) Uani 1 1 d . . . H10 H 1.6069 0.5075 1.3548 0.030 Uiso 1 1 calc R . . C11 C 1.5253(3) 0.3632(2) 1.2979(2) 0.0233(6) Uani 1 1 d . . . H11 H 1.6002 0.3339 1.3458 0.028 Uiso 1 1 calc R . . C12 C 1.4098(3) 0.3021(2) 1.2207(2) 0.0186(5) Uani 1 1 d . . . H12 H 1.4085 0.2320 1.2161 0.022 Uiso 1 1 calc R . . C13 C 0.9662(3) 0.30938(19) 1.0491(2) 0.0165(5) Uani 1 1 d . . . C14 C 0.8407(3) 0.2948(2) 0.9598(2) 0.0219(6) Uani 1 1 d . . . H14 H 0.8558 0.2737 0.8971 0.026 Uiso 1 1 calc R . . C15 C 0.6922(4) 0.3119(2) 0.9642(3) 0.0329(7) Uani 1 1 d . . . H15 H 0.6083 0.3031 0.9042 0.040 Uiso 1 1 calc R . . C16 C 0.6689(4) 0.3417(2) 1.0573(3) 0.0357(8) Uani 1 1 d . . . H16 H 0.5690 0.3519 1.0598 0.043 Uiso 1 1 calc R . . C17 C 0.7930(4) 0.3564(2) 1.1464(3) 0.0319(7) Uani 1 1 d . . . H17 H 0.7768 0.3767 1.2089 0.038 Uiso 1 1 calc R . . C18 C 0.9417(3) 0.3407(2) 1.1428(2) 0.0228(6) Uani 1 1 d . . . H18 H 1.0255 0.3511 1.2029 0.027 Uiso 1 1 calc R . . C19 C 0.8116(3) -0.04832(19) 0.64942(19) 0.0142(5) Uani 1 1 d . . . C20 C 0.8144(3) -0.0253(2) 0.55503(19) 0.0175(5) Uani 1 1 d . . . H20 H 0.7829 0.0366 0.5356 0.021 Uiso 1 1 calc R . . C21 C 0.8642(3) -0.0949(2) 0.4901(2) 0.0196(6) Uani 1 1 d . . . H21 H 0.8659 -0.0797 0.4271 0.024 Uiso 1 1 calc R . . C22 C 0.9111(3) -0.1865(2) 0.5189(2) 0.0202(6) Uani 1 1 d . . . H22 H 0.9446 -0.2330 0.4753 0.024 Uiso 1 1 calc R . . C23 C 0.9087(3) -0.2100(2) 0.6129(2) 0.0212(6) Uani 1 1 d . . . H23 H 0.9402 -0.2721 0.6319 0.025 Uiso 1 1 calc R . . C24 C 0.8595(3) -0.1410(2) 0.6783(2) 0.0189(6) Uani 1 1 d . . . H24 H 0.8584 -0.1565 0.7413 0.023 Uiso 1 1 calc R . . C25 C 0.5743(3) -0.01633(18) 0.74610(19) 0.0130(5) Uani 1 1 d . . . C26 C 0.4651(3) -0.07389(19) 0.66150(19) 0.0168(5) Uani 1 1 d . . . H26 H 0.4836 -0.0846 0.5988 0.020 Uiso 1 1 calc R . . C27 C 0.3287(3) -0.1152(2) 0.6709(2) 0.0207(6) Uani 1 1 d . . . H27 H 0.2551 -0.1526 0.6143 0.025 Uiso 1 1 calc R . . C28 C 0.3030(3) -0.1004(2) 0.7650(2) 0.0204(6) Uani 1 1 d . . . H28 H 0.2118 -0.1280 0.7713 0.024 Uiso 1 1 calc R . . C29 C 0.4119(3) -0.0450(2) 0.8494(2) 0.0191(6) Uani 1 1 d . . . H29 H 0.3946 -0.0363 0.9125 0.023 Uiso 1 1 calc R . . C30 C 0.5469(3) -0.0024(2) 0.84015(19) 0.0157(5) Uani 1 1 d . . . H30 H 0.6195 0.0356 0.8969 0.019 Uiso 1 1 calc R . . C31 C 0.7065(3) 0.15149(19) 0.67885(18) 0.0133(5) Uani 1 1 d . . . C32 C 0.5559(3) 0.1692(2) 0.62190(19) 0.0165(5) Uani 1 1 d . . . H32 H 0.4730 0.1242 0.6170 0.020 Uiso 1 1 calc R . . C33 C 0.5296(3) 0.2537(2) 0.5726(2) 0.0197(6) Uani 1 1 d . . . H33 H 0.4291 0.2649 0.5344 0.024 Uiso 1 1 calc R . . C34 C 0.6522(3) 0.3212(2) 0.5801(2) 0.0206(6) Uani 1 1 d . . . H34 H 0.6341 0.3775 0.5465 0.025 Uiso 1 1 calc R . . C35 C 0.8020(3) 0.3054(2) 0.6375(2) 0.0205(6) Uani 1 1 d . . . H35 H 0.8840 0.3515 0.6434 0.025 Uiso 1 1 calc R . . C36 C 0.8297(3) 0.2204(2) 0.6863(2) 0.0177(5) Uani 1 1 d . . . H36 H 0.9305 0.2094 0.7241 0.021 Uiso 1 1 calc R . . Re1 Re 1.0000 0.5000 0.5000 0.02786(5) Uani 1 2 d S . . O4 O 1.1668(5) 0.4725(3) 0.4663(4) 0.0360(11) Uani 0.50 1 d P . . O5 O 0.8801(5) 0.3762(3) 0.4515(3) 0.0249(9) Uani 0.50 1 d P . . O6 O 1.0302(6) 0.5237(3) 0.6223(3) 0.0376(11) Uani 0.50 1 d P . . O7 O 0.8964(5) 0.5810(3) 0.4277(3) 0.0278(9) Uani 0.50 1 d P . . 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 Np1 0.00970(7) 0.01171(7) 0.00861(7) 0.00184(5) 0.00324(5) 0.00052(5) P1 0.0125(3) 0.0115(3) 0.0125(3) 0.0016(2) 0.0038(3) -0.0004(2) P2 0.0109(3) 0.0160(3) 0.0095(3) 0.0038(2) 0.0029(2) 0.0005(2) O1 0.0150(9) 0.0122(8) 0.0157(9) 0.0028(7) 0.0039(7) -0.0001(7) O2 0.0142(9) 0.0186(9) 0.0108(8) 0.0042(7) 0.0023(7) 0.0003(7) O3 0.0143(9) 0.0181(9) 0.0156(9) 0.0009(7) 0.0082(7) 0.0020(7) C1 0.0132(12) 0.0154(12) 0.0127(12) 0.0024(10) 0.0037(10) -0.0010(9) C2 0.0250(15) 0.0152(13) 0.0191(13) 0.0004(10) 0.0071(11) -0.0008(11) C3 0.0281(16) 0.0220(14) 0.0187(14) 0.0056(11) 0.0065(12) -0.0077(12) C4 0.0194(14) 0.0322(16) 0.0137(13) 0.0039(11) 0.0045(11) -0.0055(12) C5 0.0182(14) 0.0295(15) 0.0176(13) 0.0009(11) 0.0063(11) 0.0038(11) C6 0.0167(13) 0.0202(13) 0.0151(12) 0.0042(10) 0.0032(11) 0.0021(10) C7 0.0149(13) 0.0161(12) 0.0142(12) -0.0003(10) 0.0062(10) -0.0040(10) C8 0.0231(15) 0.0179(13) 0.0213(14) 0.0011(11) 0.0061(12) -0.0001(11) C9 0.0279(16) 0.0193(14) 0.0247(15) -0.0016(11) 0.0095(13) -0.0057(12) C10 0.0210(15) 0.0301(16) 0.0199(14) -0.0060(12) 0.0067(12) -0.0080(12) C11 0.0203(14) 0.0290(15) 0.0171(13) 0.0003(11) 0.0024(11) -0.0001(12) C12 0.0214(14) 0.0182(13) 0.0167(13) 0.0010(10) 0.0074(11) -0.0003(11) C13 0.0157(13) 0.0127(12) 0.0237(14) 0.0042(10) 0.0093(11) 0.0011(10) C14 0.0203(14) 0.0201(14) 0.0252(15) 0.0060(11) 0.0058(12) 0.0009(11) C15 0.0181(15) 0.0341(17) 0.047(2) 0.0170(15) 0.0066(14) 0.0056(13) C16 0.0244(17) 0.0293(17) 0.066(2) 0.0173(16) 0.0281(17) 0.0094(13) C17 0.0357(18) 0.0235(15) 0.048(2) 0.0052(14) 0.0306(16) 0.0041(13) C18 0.0255(15) 0.0218(14) 0.0238(14) 0.0031(11) 0.0118(12) 0.0017(11) C19 0.0112(12) 0.0183(13) 0.0131(12) 0.0006(10) 0.0049(10) -0.0011(10) C20 0.0158(13) 0.0201(13) 0.0154(12) 0.0041(10) 0.0030(10) -0.0014(10) C21 0.0190(14) 0.0266(14) 0.0121(12) 0.0011(11) 0.0044(11) -0.0039(11) C22 0.0155(13) 0.0266(15) 0.0171(13) -0.0047(11) 0.0067(11) -0.0007(11) C23 0.0210(14) 0.0198(14) 0.0221(14) 0.0034(11) 0.0057(12) 0.0033(11) C24 0.0210(14) 0.0231(14) 0.0136(12) 0.0046(10) 0.0060(11) 0.0017(11) C25 0.0115(12) 0.0143(12) 0.0145(12) 0.0059(10) 0.0043(10) 0.0032(9) C26 0.0173(13) 0.0190(13) 0.0140(12) 0.0042(10) 0.0040(10) -0.0005(10) C27 0.0153(13) 0.0244(14) 0.0192(14) 0.0045(11) 0.0006(11) -0.0031(11) C28 0.0138(13) 0.0246(14) 0.0263(15) 0.0107(11) 0.0086(11) 0.0014(11) C29 0.0189(14) 0.0240(14) 0.0182(13) 0.0059(11) 0.0099(11) 0.0040(11) C30 0.0123(12) 0.0198(13) 0.0142(12) 0.0023(10) 0.0031(10) 0.0018(10) C31 0.0155(13) 0.0159(12) 0.0086(11) 0.0027(9) 0.0038(10) 0.0009(10) C32 0.0164(13) 0.0195(13) 0.0137(12) 0.0016(10) 0.0054(10) -0.0002(10) C33 0.0185(14) 0.0242(14) 0.0151(13) 0.0056(11) 0.0020(11) 0.0065(11) C34 0.0296(16) 0.0178(13) 0.0151(13) 0.0052(10) 0.0065(12) 0.0045(11) C35 0.0226(15) 0.0218(14) 0.0169(13) 0.0040(11) 0.0058(11) -0.0049(11) C36 0.0146(13) 0.0225(14) 0.0158(13) 0.0046(10) 0.0037(11) 0.0012(10) Re1 0.02066(9) 0.04173(11) 0.02741(10) 0.02306(8) 0.00848(7) 0.00838(7) O4 0.020(2) 0.037(3) 0.052(3) 0.005(2) 0.014(2) -0.0028(19) O5 0.023(2) 0.023(2) 0.028(2) 0.0053(17) 0.0068(18) 0.0060(16) O6 0.058(3) 0.033(2) 0.012(2) 0.0023(17) -0.002(2) 0.003(2) O7 0.031(2) 0.025(2) 0.023(2) 0.0107(17) -0.0016(18) -0.0004(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 Np1 O3 1.8071(18) . ? Np1 O3 1.8071(18) 2_757 ? Np1 O1 2.4345(18) 2_757 ? Np1 O1 2.4345(18) . ? Np1 O2 2.4380(18) . ? Np1 O2 2.4380(18) 2_757 ? P1 O1 1.5037(19) . ? P1 C13 1.789(3) . ? P1 C7 1.795(3) . ? P1 C1 1.797(3) . ? P2 O2 1.4989(18) . ? P2 C25 1.791(3) . ? P2 C31 1.796(3) . ? P2 C19 1.800(3) . ? C1 C2 1.393(4) . ? C1 C6 1.395(4) . ? C2 C3 1.388(4) . ? C2 H2 0.9300 . ? C3 C4 1.385(4) . ? C3 H3 0.9300 . ? C4 C5 1.379(4) . ? C4 H4 0.9300 . ? C5 C6 1.395(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.387(4) . ? C7 C8 1.392(4) . ? C8 C9 1.386(4) . ? C8 H8 0.9300 . ? C9 C10 1.382(4) . ? C9 H9 0.9300 . ? C10 C11 1.376(4) . ? C10 H10 0.9300 . ? C11 C12 1.391(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.387(4) . ? C13 C18 1.398(4) . ? C14 C15 1.389(4) . ? C14 H14 0.9300 . ? C15 C16 1.382(5) . ? C15 H15 0.9300 . ? C16 C17 1.379(5) . ? C16 H16 0.9300 . ? C17 C18 1.385(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.393(4) . ? C19 C20 1.395(4) . ? C20 C21 1.388(4) . ? C20 H20 0.9300 . ? C21 C22 1.377(4) . ? C21 H21 0.9300 . ? C22 C23 1.390(4) . ? C22 H22 0.9300 . ? C23 C24 1.384(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.392(3) . ? C25 C26 1.396(3) . ? C26 C27 1.391(4) . ? C26 H26 0.9300 . ? C27 C28 1.386(4) . ? C27 H27 0.9300 . ? C28 C29 1.382(4) . ? C28 H28 0.9300 . ? C29 C30 1.385(4) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.396(4) . ? C31 C36 1.398(4) . ? C32 C33 1.388(4) . ? C32 H32 0.9300 . ? C33 C34 1.382(4) . ? C33 H33 0.9300 . ? C34 C35 1.386(4) . ? C34 H34 0.9300 . ? C35 C36 1.389(4) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? Re1 O6 1.620(4) . ? Re1 O6 1.620(4) 2_766 ? Re1 O7 1.683(4) 2_766 ? Re1 O7 1.683(4) . ? Re1 O4 1.749(4) 2_766 ? Re1 O4 1.749(4) . ? Re1 O5 1.876(4) . ? Re1 O5 1.876(4) 2_766 ? O6 O7 1.717(6) 2_766 ? O7 O6 1.717(6) 2_766 ? 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 O3 Np1 O3 180.00(10) . 2_757 ? O3 Np1 O1 90.35(8) . 2_757 ? O3 Np1 O1 89.65(8) 2_757 2_757 ? O3 Np1 O1 89.65(8) . . ? O3 Np1 O1 90.35(8) 2_757 . ? O1 Np1 O1 180.00(5) 2_757 . ? O3 Np1 O2 89.80(7) . . ? O3 Np1 O2 90.20(7) 2_757 . ? O1 Np1 O2 88.72(6) 2_757 . ? O1 Np1 O2 91.28(6) . . ? O3 Np1 O2 90.20(7) . 2_757 ? O3 Np1 O2 89.80(7) 2_757 2_757 ? O1 Np1 O2 91.28(6) 2_757 2_757 ? O1 Np1 O2 88.72(6) . 2_757 ? O2 Np1 O2 180.00(5) . 2_757 ? O1 P1 C13 111.78(11) . . ? O1 P1 C7 110.34(11) . . ? C13 P1 C7 107.36(13) . . ? O1 P1 C1 109.72(11) . . ? C13 P1 C1 109.95(12) . . ? C7 P1 C1 107.58(12) . . ? O2 P2 C25 111.55(11) . . ? O2 P2 C31 111.42(11) . . ? C25 P2 C31 108.40(12) . . ? O2 P2 C19 112.28(11) . . ? C25 P2 C19 106.61(12) . . ? C31 P2 C19 106.28(12) . . ? P1 O1 Np1 135.84(10) . . ? P2 O2 Np1 145.33(10) . . ? C2 C1 C6 119.6(2) . . ? C2 C1 P1 123.2(2) . . ? C6 C1 P1 117.08(19) . . ? C3 C2 C1 120.2(3) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 119.8(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 119.9(3) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 119.8(3) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? C12 C7 C8 120.1(2) . . ? C12 C7 P1 118.7(2) . . ? C8 C7 P1 121.2(2) . . ? C9 C8 C7 119.6(3) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 120.3(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 120.2(3) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.1(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C7 C12 C11 119.7(3) . . ? C7 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C18 119.5(3) . . ? C14 C13 P1 121.0(2) . . ? C18 C13 P1 118.3(2) . . ? C13 C14 C15 119.9(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 120.3(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 119.9(3) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.2(3) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C24 C19 C20 119.8(2) . . ? C24 C19 P2 118.28(19) . . ? C20 C19 P2 121.9(2) . . ? C21 C20 C19 119.9(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.1(2) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.4(2) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 120.0(3) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C19 119.9(2) . . ? C23 C24 H24 120.1 . . ? C19 C24 H24 120.1 . . ? C30 C25 C26 119.5(2) . . ? C30 C25 P2 118.76(19) . . ? C26 C25 P2 121.71(19) . . ? C27 C26 C25 120.1(2) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 119.7(2) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C29 C28 C27 120.5(3) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 120.0(2) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C25 120.2(2) . . ? C29 C30 H30 119.9 . . ? C25 C30 H30 119.9 . . ? C32 C31 C36 119.1(2) . . ? C32 C31 P2 122.5(2) . . ? C36 C31 P2 118.23(19) . . ? C33 C32 C31 120.2(2) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 120.2(3) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 120.2(3) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C34 C35 C36 120.0(3) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 120.2(2) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? O6 Re1 O6 180.000(1) . 2_766 ? O6 Re1 O7 62.6(2) . 2_766 ? O6 Re1 O7 117.4(2) 2_766 2_766 ? O6 Re1 O7 117.4(2) . . ? O6 Re1 O7 62.6(2) 2_766 . ? O7 Re1 O7 180.000(1) 2_766 . ? O6 Re1 O4 66.0(2) . 2_766 ? O6 Re1 O4 114.0(2) 2_766 2_766 ? O7 Re1 O4 110.9(2) 2_766 2_766 ? O7 Re1 O4 69.1(2) . 2_766 ? O6 Re1 O4 114.0(2) . . ? O6 Re1 O4 66.0(2) 2_766 . ? O7 Re1 O4 69.1(2) 2_766 . ? O7 Re1 O4 110.9(2) . . ? O4 Re1 O4 180.000(1) 2_766 . ? O6 Re1 O5 107.3(2) . . ? O6 Re1 O5 72.7(2) 2_766 . ? O7 Re1 O5 76.05(18) 2_766 . ? O7 Re1 O5 103.95(19) . . ? O4 Re1 O5 78.62(19) 2_766 . ? O4 Re1 O5 101.38(19) . . ? O6 Re1 O5 72.7(2) . 2_766 ? O6 Re1 O5 107.3(2) 2_766 2_766 ? O7 Re1 O5 103.95(18) 2_766 2_766 ? O7 Re1 O5 76.05(18) . 2_766 ? O4 Re1 O5 101.38(19) 2_766 2_766 ? O4 Re1 O5 78.62(19) . 2_766 ? O5 Re1 O5 180.000(1) . 2_766 ? Re1 O6 O7 60.5(2) . 2_766 ? Re1 O7 O6 56.89(19) . 2_766 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 P1 O1 Np1 46.43(18) . . . . ? C7 P1 O1 Np1 165.82(13) . . . . ? C1 P1 O1 Np1 -75.82(17) . . . . ? O3 Np1 O1 P1 -63.98(15) . . . . ? O3 Np1 O1 P1 116.02(15) 2_757 . . . ? O1 Np1 O1 P1 21(100) 2_757 . . . ? O2 Np1 O1 P1 25.81(15) . . . . ? O2 Np1 O1 P1 -154.19(15) 2_757 . . . ? C25 P2 O2 Np1 44.8(2) . . . . ? C31 P2 O2 Np1 166.14(16) . . . . ? C19 P2 O2 Np1 -74.8(2) . . . . ? O3 Np1 O2 P2 -89.71(19) . . . . ? O3 Np1 O2 P2 90.29(19) 2_757 . . . ? O1 Np1 O2 P2 0.64(18) 2_757 . . . ? O1 Np1 O2 P2 -179.36(18) . . . . ? O2 Np1 O2 P2 -127(100) 2_757 . . . ? O1 P1 C1 C2 172.8(2) . . . . ? C13 P1 C1 C2 49.5(3) . . . . ? C7 P1 C1 C2 -67.1(3) . . . . ? O1 P1 C1 C6 -10.7(2) . . . . ? C13 P1 C1 C6 -134.0(2) . . . . ? C7 P1 C1 C6 109.4(2) . . . . ? C6 C1 C2 C3 -0.3(4) . . . . ? P1 C1 C2 C3 176.1(2) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C3 C4 C5 C6 0.3(4) . . . . ? C4 C5 C6 C1 -0.7(4) . . . . ? C2 C1 C6 C5 0.7(4) . . . . ? P1 C1 C6 C5 -175.9(2) . . . . ? O1 P1 C7 C12 8.2(2) . . . . ? C13 P1 C7 C12 130.2(2) . . . . ? C1 P1 C7 C12 -111.5(2) . . . . ? O1 P1 C7 C8 -174.0(2) . . . . ? C13 P1 C7 C8 -52.0(2) . . . . ? C1 P1 C7 C8 66.3(2) . . . . ? C12 C7 C8 C9 -0.1(4) . . . . ? P1 C7 C8 C9 -177.8(2) . . . . ? C7 C8 C9 C10 -0.6(4) . . . . ? C8 C9 C10 C11 0.3(4) . . . . ? C9 C10 C11 C12 0.6(4) . . . . ? C8 C7 C12 C11 1.0(4) . . . . ? P1 C7 C12 C11 178.8(2) . . . . ? C10 C11 C12 C7 -1.2(4) . . . . ? O1 P1 C13 C14 -86.6(2) . . . . ? C7 P1 C13 C14 152.3(2) . . . . ? C1 P1 C13 C14 35.5(3) . . . . ? O1 P1 C13 C18 81.2(2) . . . . ? C7 P1 C13 C18 -40.0(2) . . . . ? C1 P1 C13 C18 -156.7(2) . . . . ? C18 C13 C14 C15 0.3(4) . . . . ? P1 C13 C14 C15 167.9(2) . . . . ? C13 C14 C15 C16 -1.0(4) . . . . ? C14 C15 C16 C17 1.0(5) . . . . ? C15 C16 C17 C18 -0.3(5) . . . . ? C16 C17 C18 C13 -0.5(4) . . . . ? C14 C13 C18 C17 0.5(4) . . . . ? P1 C13 C18 C17 -167.5(2) . . . . ? O2 P2 C19 C24 55.3(2) . . . . ? C25 P2 C19 C24 -67.2(2) . . . . ? C31 P2 C19 C24 177.3(2) . . . . ? O2 P2 C19 C20 -123.7(2) . . . . ? C25 P2 C19 C20 113.9(2) . . . . ? C31 P2 C19 C20 -1.6(2) . . . . ? C24 C19 C20 C21 0.2(4) . . . . ? P2 C19 C20 C21 179.2(2) . . . . ? C19 C20 C21 C22 -0.1(4) . . . . ? C20 C21 C22 C23 0.1(4) . . . . ? C21 C22 C23 C24 -0.2(4) . . . . ? C22 C23 C24 C19 0.4(4) . . . . ? C20 C19 C24 C23 -0.4(4) . . . . ? P2 C19 C24 C23 -179.3(2) . . . . ? O2 P2 C25 C30 20.7(2) . . . . ? C31 P2 C25 C30 -102.3(2) . . . . ? C19 P2 C25 C30 143.6(2) . . . . ? O2 P2 C25 C26 -158.7(2) . . . . ? C31 P2 C25 C26 78.3(2) . . . . ? C19 P2 C25 C26 -35.8(2) . . . . ? C30 C25 C26 C27 1.3(4) . . . . ? P2 C25 C26 C27 -179.3(2) . . . . ? C25 C26 C27 C28 -1.1(4) . . . . ? C26 C27 C28 C29 -0.1(4) . . . . ? C27 C28 C29 C30 1.0(4) . . . . ? C28 C29 C30 C25 -0.8(4) . . . . ? C26 C25 C30 C29 -0.3(4) . . . . ? P2 C25 C30 C29 -179.7(2) . . . . ? O2 P2 C31 C32 -141.8(2) . . . . ? C25 P2 C31 C32 -18.7(2) . . . . ? C19 P2 C31 C32 95.6(2) . . . . ? O2 P2 C31 C36 41.8(2) . . . . ? C25 P2 C31 C36 164.88(19) . . . . ? C19 P2 C31 C36 -80.8(2) . . . . ? C36 C31 C32 C33 0.6(4) . . . . ? P2 C31 C32 C33 -175.8(2) . . . . ? C31 C32 C33 C34 -0.4(4) . . . . ? C32 C33 C34 C35 -0.5(4) . . . . ? C33 C34 C35 C36 1.1(4) . . . . ? C34 C35 C36 C31 -0.9(4) . . . . ? C32 C31 C36 C35 0.0(4) . . . . ? P2 C31 C36 C35 176.6(2) . . . . ? O6 Re1 O6 O7 -43(100) 2_766 . . 2_766 ? O7 Re1 O6 O7 180.000(2) . . . 2_766 ? O4 Re1 O6 O7 132.1(3) 2_766 . . 2_766 ? O4 Re1 O6 O7 -47.9(3) . . . 2_766 ? O5 Re1 O6 O7 63.5(2) . . . 2_766 ? O5 Re1 O6 O7 -116.5(2) 2_766 . . 2_766 ? O6 Re1 O7 O6 180.000(2) . . . 2_766 ? O7 Re1 O7 O6 -115(100) 2_766 . . 2_766 ? O4 Re1 O7 O6 -133.5(3) 2_766 . . 2_766 ? O4 Re1 O7 O6 46.5(3) . . . 2_766 ? O5 Re1 O7 O6 -61.7(3) . . . 2_766 ? O5 Re1 O7 O6 118.3(3) 2_766 . . 2_766 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.781 _refine_diff_density_min -1.390 _refine_diff_density_rms 0.085