Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Iain May' _publ_contact_author_address ; Department of Chemistry University of Manchester Oxford Road Manchester M13 9PL UNITED KINGDOM ; _publ_section_title ; The coordination of perrhenate and pertechnetate to thorium(IV) in the presence and absence of phosphine oxide or phosphate ligands ; _publ_contact_author_email IAIN.MAY@MAN.AC.UK loop_ _publ_author_name I.May M.Helliwell M.Sarsfield C.Sharrad A.D.Sutton data_s1837abs _database_code_depnum_ccdc_archive 'CCDC 616571' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit 1/4 of the molecule. The geometry of the OEt groups was restrained. The crystal was a merohedral twin such that the twin matrix was 0 1 0 1 0 0 0 0 -1 and the twin fraction was 0.42952. The Th, Re and P atoms were refined anisotropically; other non H atoms were refined isotropically. H atoms were included in calculated positions. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H60 O32 P4 Re4 Th' _chemical_formula_weight 1961.44 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 13.330(2) _cell_length_b 13.330(2) _cell_length_c 15.083(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2679.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3964 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 26.31 _exptl_crystal_description Prism _exptl_crystal_colour Clear _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1820 _exptl_absorpt_coefficient_mu 11.971 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3807 _exptl_absorpt_correction_T_max 0.5859 _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 7818 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.40 _reflns_number_total 2732 _reflns_number_gt 2714 _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^)+(0.0001P)^2^+229.5028P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 2732 _refine_ls_number_parameters 83 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1320 _refine_ls_wR_factor_gt 0.1318 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.006 _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 Th1 Th 0.0000 0.0000 0.0000 0.0113(3) Uani 1 4 d S . . Re1 Re 0.18495(9) -0.19476(9) 0.12388(6) 0.0250(2) Uani 1 1 d . . . P1 P 0.1459(9) 0.1489(14) 0.1597(6) 0.063(3) Uani 1 1 d . . . O1 O 0.1256(19) -0.107(2) 0.0499(12) 0.044(5) Uiso 1 1 d . . . O2 O 0.1364(17) -0.184(2) 0.2301(15) 0.058(7) Uiso 1 1 d . . . O3 O 0.3110(17) -0.1814(16) 0.0974(13) 0.034(5) Uiso 1 1 d . . . O4 O 0.1532(19) -0.307(2) 0.121(2) 0.055(6) Uiso 1 1 d . . . O5 O 0.0886(14) 0.0683(14) 0.1220(12) 0.029(4) Uiso 1 1 d . . . O6 O 0.171(2) 0.1406(19) 0.2530(15) 0.067(6) Uiso 1 1 d DU . . O7 O 0.2496(18) 0.179(2) 0.1133(18) 0.065(6) Uiso 1 1 d DU . . O8 O 0.075(2) 0.2499(18) 0.1454(17) 0.057(6) Uiso 1 1 d DU . . C1 C 0.099(2) 0.097(3) 0.3147(19) 0.065(6) Uiso 1 1 d DU . . H1A H 0.0487 0.0571 0.2817 0.077 Uiso 1 1 calc R . . H1B H 0.0629 0.1515 0.3464 0.077 Uiso 1 1 calc R . . C2 C 0.154(3) 0.030(3) 0.382(2) 0.059(8) Uiso 1 1 d DU . . H2A H 0.1575 -0.0386 0.3589 0.089 Uiso 1 1 calc R . . H2B H 0.1174 0.0302 0.4383 0.089 Uiso 1 1 calc R . . H2C H 0.2220 0.0558 0.3913 0.089 Uiso 1 1 calc R . . C3 C 0.325(3) 0.117(3) 0.148(2) 0.068(7) Uiso 1 1 d DU . . H3A H 0.2925 0.0531 0.1661 0.082 Uiso 1 1 calc R . . H3B H 0.3510 0.1490 0.2023 0.082 Uiso 1 1 calc R . . C4 C 0.412(3) 0.092(4) 0.089(3) 0.084(10) Uiso 1 1 d DU . . H4A H 0.4012 0.0265 0.0609 0.127 Uiso 1 1 calc R . . H4B H 0.4738 0.0892 0.1247 0.127 Uiso 1 1 calc R . . H4C H 0.4194 0.1435 0.0432 0.127 Uiso 1 1 calc R . . C5 C 0.072(3) 0.355(2) 0.157(3) 0.066(6) Uiso 1 1 d DU . . H5A H 0.0671 0.3710 0.2211 0.079 Uiso 1 1 calc R . . H5B H 0.0115 0.3827 0.1275 0.079 Uiso 1 1 calc R . . C6 C 0.166(3) 0.406(3) 0.118(4) 0.083(9) Uiso 1 1 d DU . . H6A H 0.2220 0.3997 0.1604 0.124 Uiso 1 1 calc R . . H6B H 0.1527 0.4768 0.1069 0.124 Uiso 1 1 calc R . . H6C H 0.1848 0.3727 0.0624 0.124 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Th1 0.0093(4) 0.0093(4) 0.0154(6) 0.000 0.000 0.000 Re1 0.0328(8) 0.0251(6) 0.0172(3) 0.0038(6) -0.0159(6) 0.0005(5) P1 0.025(6) 0.111(11) 0.052(4) -0.038(8) 0.000(5) -0.014(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 Th1 O1 2.327(19) 3 ? Th1 O1 2.327(19) 4 ? Th1 O1 2.327(19) 2 ? Th1 O1 2.328(19) . ? Th1 O5 2.368(17) . ? Th1 O5 2.368(17) 3 ? Th1 O5 2.368(17) 4 ? Th1 O5 2.368(17) 2 ? Re1 O4 1.56(3) . ? Re1 O2 1.73(2) . ? Re1 O3 1.74(2) . ? Re1 O1 1.797(19) . ? P1 O5 1.436(18) . ? P1 O6 1.45(3) . ? P1 O7 1.60(3) . ? P1 O8 1.66(3) . ? O6 C1 1.456(18) . ? O7 C3 1.401(19) . ? O8 C5 1.417(19) . ? C1 C2 1.54(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.508(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.546(19) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? 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 Th1 O1 142.3(9) 3 4 ? O1 Th1 O1 96.0(3) 3 2 ? O1 Th1 O1 96.0(3) 4 2 ? O1 Th1 O1 96.0(3) 3 . ? O1 Th1 O1 96.0(3) 4 . ? O1 Th1 O1 142.3(9) 2 . ? O1 Th1 O5 146.5(6) 3 . ? O1 Th1 O5 70.6(6) 4 . ? O1 Th1 O5 82.6(8) 2 . ? O1 Th1 O5 68.1(8) . . ? O1 Th1 O5 68.1(8) 3 3 ? O1 Th1 O5 82.6(8) 4 3 ? O1 Th1 O5 146.5(6) 2 3 ? O1 Th1 O5 70.6(6) . 3 ? O5 Th1 O5 127.1(5) . 3 ? O1 Th1 O5 82.6(8) 3 4 ? O1 Th1 O5 68.1(8) 4 4 ? O1 Th1 O5 70.6(6) 2 4 ? O1 Th1 O5 146.5(6) . 4 ? O5 Th1 O5 127.1(5) . 4 ? O5 Th1 O5 78.0(8) 3 4 ? O1 Th1 O5 70.6(6) 3 2 ? O1 Th1 O5 146.5(6) 4 2 ? O1 Th1 O5 68.1(8) 2 2 ? O1 Th1 O5 82.6(8) . 2 ? O5 Th1 O5 78.0(8) . 2 ? O5 Th1 O5 127.1(5) 3 2 ? O5 Th1 O5 127.1(5) 4 2 ? O4 Re1 O2 90.4(15) . . ? O4 Re1 O3 110.8(12) . . ? O2 Re1 O3 124.4(10) . . ? O4 Re1 O1 119.1(14) . . ? O2 Re1 O1 110.7(11) . . ? O3 Re1 O1 102.5(11) . . ? O5 P1 O6 116.7(15) . . ? O5 P1 O7 118.5(14) . . ? O6 P1 O7 104.2(15) . . ? O5 P1 O8 104.5(14) . . ? O6 P1 O8 108.5(17) . . ? O7 P1 O8 103.4(15) . . ? Re1 O1 Th1 156.4(12) . . ? P1 O5 Th1 149.4(12) . . ? P1 O6 C1 120(2) . . ? C3 O7 P1 108(2) . . ? C5 O8 P1 143(3) . . ? O6 C1 C2 110(2) . . ? O6 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? O6 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O7 C3 C4 118(3) . . ? O7 C3 H3A 107.9 . . ? C4 C3 H3A 107.9 . . ? O7 C3 H3B 107.9 . . ? C4 C3 H3B 107.9 . . ? H3A C3 H3B 107.2 . . ? 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 . . ? O8 C5 C6 111(2) . . ? O8 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? O8 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 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 O4 Re1 O1 Th1 80(4) . . . . ? O2 Re1 O1 Th1 -22(4) . . . . ? O3 Re1 O1 Th1 -157(4) . . . . ? O1 Th1 O1 Re1 -77(4) 3 . . . ? O1 Th1 O1 Re1 139(4) 4 . . . ? O1 Th1 O1 Re1 31(4) 2 . . . ? O5 Th1 O1 Re1 73(4) . . . . ? O5 Th1 O1 Re1 -141(4) 3 . . . ? O5 Th1 O1 Re1 -162(3) 4 . . . ? O5 Th1 O1 Re1 -7(4) 2 . . . ? O6 P1 O5 Th1 174(2) . . . . ? O7 P1 O5 Th1 -60(4) . . . . ? O8 P1 O5 Th1 54(3) . . . . ? O1 Th1 O5 P1 -169(3) 3 . . . ? O1 Th1 O5 P1 20(3) 4 . . . ? O1 Th1 O5 P1 -79(3) 2 . . . ? O1 Th1 O5 P1 125(3) . . . . ? O5 Th1 O5 P1 84(3) 3 . . . ? O5 Th1 O5 P1 -20(3) 4 . . . ? O5 Th1 O5 P1 -148(3) 2 . . . ? O5 P1 O6 C1 -37(4) . . . . ? O7 P1 O6 C1 -170(3) . . . . ? O8 P1 O6 C1 81(3) . . . . ? O5 P1 O7 C3 -86(3) . . . . ? O6 P1 O7 C3 46(3) . . . . ? O8 P1 O7 C3 159(2) . . . . ? O5 P1 O8 C5 -176(4) . . . . ? O6 P1 O8 C5 59(4) . . . . ? O7 P1 O8 C5 -52(4) . . . . ? P1 O6 C1 C2 140(3) . . . . ? P1 O7 C3 C4 150(4) . . . . ? P1 O8 C5 C6 50(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.422 _refine_diff_density_min -3.170 _refine_diff_density_rms 0.356 # Attachment 'Structure51.cif' data_s1811ccd _database_code_depnum_ccdc_archive 'CCDC 616572' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H51 O17 P3 Re3 Th' _chemical_formula_weight 1879.52 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' Th Th -7.2400 8.8979 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.342(13) _cell_length_b 13.669(8) _cell_length_c 22.453(14) _cell_angle_alpha 90.00 _cell_angle_beta 115.540(8) _cell_angle_gamma 90.00 _cell_volume 5910(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7597 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.24 _exptl_crystal_description rectangular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3532 _exptl_absorpt_coefficient_mu 8.782 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.412 _exptl_absorpt_correction_T_max 1.000 _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 31923 _diffrn_reflns_av_R_equivalents 0.0797 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.43 _reflns_number_total 11817 _reflns_number_gt 9375 _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^)+(0.0585P)^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 11817 _refine_ls_number_parameters 723 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Th1 Th 0.280444(15) 0.42266(2) 0.306833(15) 0.01280(9) Uani 1 1 d . . . Re1 Re 0.128651(18) 0.22266(3) 0.26873(2) 0.02159(11) Uani 1 1 d . . . Re2 Re 0.33629(2) 0.61149(3) 0.45643(2) 0.02691(12) Uani 1 1 d . . . Re3 Re 0.415675(18) 0.62277(3) 0.302228(19) 0.02310(11) Uani 1 1 d . . . P1 P 0.12213(11) 0.59134(17) 0.25898(12) 0.0175(5) Uani 1 1 d . . . P2 P 0.24555(11) 0.42441(17) 0.12146(12) 0.0154(5) Uani 1 1 d . . . P3 P 0.36466(10) 0.17836(17) 0.29657(11) 0.0148(5) Uani 1 1 d . . . O1 O 0.1851(3) 0.5327(5) 0.2679(3) 0.0205(14) Uani 1 1 d . . . O2 O 0.2471(3) 0.4144(4) 0.1883(3) 0.0200(14) Uani 1 1 d . . . O3 O 0.3218(3) 0.2669(4) 0.2965(3) 0.0169(13) Uani 1 1 d . . . O4 O 0.1751(3) 0.3194(5) 0.2549(3) 0.0220(14) Uani 1 1 d . . . O5 O 0.1808(4) 0.1476(6) 0.3308(5) 0.060(3) Uani 1 1 d . . . O6 O 0.0911(4) 0.1544(5) 0.1985(4) 0.0374(19) Uani 1 1 d . . . O7 O 0.0675(4) 0.2688(6) 0.2888(5) 0.049(2) Uani 1 1 d . . . O8 O 0.3144(3) 0.5737(5) 0.3752(3) 0.0236(15) Uani 1 1 d . . . O9 O 0.3997(4) 0.5373(6) 0.5120(4) 0.047(2) Uani 1 1 d . . . O10 O 0.3668(5) 0.7274(6) 0.4656(4) 0.061(3) Uani 1 1 d . . . O11 O 0.2649(5) 0.6104(6) 0.4725(5) 0.051(2) Uani 1 1 d . . . O12 O 0.3509(3) 0.5338(5) 0.2739(3) 0.0315(17) Uani 1 1 d . . . O13 O 0.4641(3) 0.6109(5) 0.2596(4) 0.0341(18) Uani 1 1 d . . . O14 O 0.4688(4) 0.6040(6) 0.3845(4) 0.048(2) Uani 1 1 d . . . O15 O 0.3810(4) 0.7374(7) 0.2908(4) 0.049(2) Uani 1 1 d . . . O16 O 0.2678(3) 0.3732(5) 0.3905(3) 0.0260(16) Uani 1 1 d . . . O17 O 0.4091(3) 0.4141(5) 0.3903(4) 0.0302(17) Uani 1 1 d . . . C1 C 0.1334(4) 0.7153(6) 0.2410(5) 0.019(2) Uani 1 1 d . . . C2 C 0.0760(5) 0.7751(7) 0.2027(5) 0.023(2) Uani 1 1 d . . . H2 H 0.0306 0.7479 0.1832 0.027 Uiso 1 1 calc R . . C3 C 0.0858(5) 0.8746(7) 0.1934(5) 0.026(2) Uani 1 1 d . . . H3 H 0.0472 0.9142 0.1669 0.031 Uiso 1 1 calc R . . C4 C 0.1503(5) 0.9142(7) 0.2222(6) 0.030(2) Uani 1 1 d . . . H4 H 0.1567 0.9819 0.2171 0.036 Uiso 1 1 calc R . . C5 C 0.2069(5) 0.8556(8) 0.2591(6) 0.035(3) Uani 1 1 d . . . H5 H 0.2522 0.8832 0.2776 0.042 Uiso 1 1 calc R . . C6 C 0.1986(5) 0.7573(7) 0.2696(5) 0.029(2) Uani 1 1 d . . . H6 H 0.2378 0.7189 0.2964 0.035 Uiso 1 1 calc R . . C7 C 0.1070(5) 0.5914(7) 0.3308(5) 0.022(2) Uani 1 1 d . . . C8 C 0.0882(5) 0.6736(7) 0.3545(5) 0.026(2) Uani 1 1 d . . . H8 H 0.0826 0.7339 0.3318 0.031 Uiso 1 1 calc R . . C9 C 0.0774(5) 0.6702(7) 0.4109(5) 0.029(2) Uani 1 1 d . . . H9 H 0.0665 0.7282 0.4278 0.034 Uiso 1 1 calc R . . C10 C 0.0828(5) 0.5800(8) 0.4431(5) 0.031(2) Uani 1 1 d . . . H10 H 0.0728 0.5764 0.4804 0.037 Uiso 1 1 calc R . . C11 C 0.1024(5) 0.4978(8) 0.4209(6) 0.034(3) Uani 1 1 d . . . H11 H 0.1088 0.4379 0.4443 0.040 Uiso 1 1 calc R . . C12 C 0.1129(5) 0.5015(7) 0.3641(5) 0.027(2) Uani 1 1 d . . . H12 H 0.1242 0.4435 0.3475 0.033 Uiso 1 1 calc R . . C13 C 0.0466(4) 0.5385(6) 0.1936(5) 0.020(2) Uani 1 1 d . . . C14 C -0.0151(5) 0.5240(7) 0.1997(5) 0.027(2) Uani 1 1 d . . . H14 H -0.0192 0.5452 0.2382 0.032 Uiso 1 1 calc R . . C15 C -0.0703(5) 0.4783(8) 0.1490(7) 0.042(3) Uani 1 1 d . . . H15 H -0.1125 0.4677 0.1528 0.050 Uiso 1 1 calc R . . C16 C -0.0646(5) 0.4482(8) 0.0936(6) 0.037(3) Uani 1 1 d . . . H16 H -0.1031 0.4176 0.0590 0.044 Uiso 1 1 calc R . . C17 C -0.0043(5) 0.4616(9) 0.0870(6) 0.043(3) Uani 1 1 d . . . H17 H -0.0007 0.4397 0.0484 0.052 Uiso 1 1 calc R . . C18 C 0.0522(5) 0.5077(9) 0.1378(6) 0.039(3) Uani 1 1 d . . . H18 H 0.0942 0.5177 0.1336 0.047 Uiso 1 1 calc R . . C19 C 0.3238(4) 0.3861(7) 0.1172(4) 0.0151(18) Uani 1 1 d . . . C20 C 0.3323(4) 0.2921(7) 0.0979(5) 0.020(2) Uani 1 1 d . . . H20 H 0.2952 0.2466 0.0857 0.024 Uiso 1 1 calc R . . C21 C 0.3940(5) 0.2633(7) 0.0960(5) 0.026(2) Uani 1 1 d . . . H21 H 0.3988 0.1995 0.0817 0.031 Uiso 1 1 calc R . . C22 C 0.4481(4) 0.3296(7) 0.1154(5) 0.025(2) Uani 1 1 d . . . H22 H 0.4910 0.3112 0.1153 0.030 Uiso 1 1 calc R . . C23 C 0.4397(4) 0.4243(7) 0.1352(5) 0.025(2) Uani 1 1 d . . . H23 H 0.4768 0.4698 0.1475 0.030 Uiso 1 1 calc R . . C24 C 0.3790(4) 0.4523(7) 0.1371(4) 0.0174(19) Uani 1 1 d . . . H24 H 0.3744 0.5159 0.1518 0.021 Uiso 1 1 calc R . . C25 C 0.1746(4) 0.3518(6) 0.0634(4) 0.017(2) Uani 1 1 d . . . C26 C 0.1596(5) 0.3459(7) -0.0032(5) 0.025(2) Uani 1 1 d . . . H26 H 0.1882 0.3788 -0.0196 0.030 Uiso 1 1 calc R . . C27 C 0.1028(5) 0.2920(7) -0.0458(5) 0.022(2) Uani 1 1 d . . . H27 H 0.0929 0.2869 -0.0912 0.027 Uiso 1 1 calc R . . C28 C 0.0612(5) 0.2461(7) -0.0220(5) 0.028(2) Uani 1 1 d . . . H28 H 0.0219 0.2102 -0.0516 0.034 Uiso 1 1 calc R . . C29 C 0.0748(5) 0.2507(8) 0.0429(6) 0.031(2) Uani 1 1 d . . . H29 H 0.0452 0.2185 0.0584 0.037 Uiso 1 1 calc R . . C30 C 0.1328(4) 0.3035(7) 0.0869(5) 0.022(2) Uani 1 1 d . . . H30 H 0.1433 0.3060 0.1325 0.026 Uiso 1 1 calc R . . C31 C 0.2347(4) 0.5516(6) 0.0954(5) 0.017(2) Uani 1 1 d . . . C32 C 0.2166(4) 0.6196(6) 0.1304(4) 0.0149(18) Uani 1 1 d . . . H32 H 0.2096 0.5990 0.1676 0.018 Uiso 1 1 calc R . . C33 C 0.2083(5) 0.7179(7) 0.1126(5) 0.029(2) Uani 1 1 d . . . H33 H 0.1971 0.7644 0.1379 0.034 Uiso 1 1 calc R . . C34 C 0.2167(5) 0.7469(7) 0.0578(5) 0.028(2) Uani 1 1 d . . . H34 H 0.2115 0.8139 0.0454 0.033 Uiso 1 1 calc R . . C35 C 0.2324(4) 0.6791(7) 0.0206(5) 0.025(2) Uani 1 1 d . . . H35 H 0.2373 0.6994 -0.0176 0.029 Uiso 1 1 calc R . . C36 C 0.2410(4) 0.5816(7) 0.0392(4) 0.0169(19) Uani 1 1 d . . . H36 H 0.2512 0.5350 0.0133 0.020 Uiso 1 1 calc R . . C37 C 0.4519(4) 0.2164(7) 0.3176(4) 0.0157(19) Uani 1 1 d . . . C38 C 0.5091(4) 0.1743(7) 0.3704(4) 0.019(2) Uani 1 1 d . . . H38 H 0.5026 0.1222 0.3952 0.023 Uiso 1 1 calc R . . C39 C 0.5752(4) 0.2097(7) 0.3859(5) 0.017(2) Uani 1 1 d . . . H39 H 0.6139 0.1817 0.4217 0.021 Uiso 1 1 calc R . . C40 C 0.5857(5) 0.2839(7) 0.3507(5) 0.022(2) Uani 1 1 d . . . H40 H 0.6313 0.3070 0.3617 0.027 Uiso 1 1 calc R . . C41 C 0.5279(4) 0.3264(7) 0.2974(5) 0.021(2) Uani 1 1 d . . . H41 H 0.5346 0.3787 0.2729 0.025 Uiso 1 1 calc R . . C42 C 0.4612(5) 0.2911(7) 0.2812(5) 0.023(2) Uani 1 1 d . . . H42 H 0.4224 0.3184 0.2452 0.027 Uiso 1 1 calc R . . C43 C 0.3647(4) 0.0893(6) 0.3556(5) 0.018(2) Uani 1 1 d . . . C44 C 0.3478(5) 0.1206(8) 0.4039(5) 0.030(2) Uani 1 1 d . . . H44 H 0.3351 0.1867 0.4059 0.036 Uiso 1 1 calc R . . C45 C 0.3499(5) 0.0514(9) 0.4512(5) 0.035(3) Uani 1 1 d . . . H45 H 0.3391 0.0725 0.4860 0.042 Uiso 1 1 calc R . . C46 C 0.3662(5) -0.0420(8) 0.4492(5) 0.028(2) Uani 1 1 d . . . H46 H 0.3668 -0.0865 0.4820 0.033 Uiso 1 1 calc R . . C47 C 0.3824(5) -0.0736(7) 0.3987(6) 0.032(3) Uani 1 1 d . . . H47 H 0.3947 -0.1401 0.3972 0.038 Uiso 1 1 calc R . . C48 C 0.3808(4) -0.0084(7) 0.3497(5) 0.019(2) Uani 1 1 d . . . H48 H 0.3903 -0.0296 0.3141 0.023 Uiso 1 1 calc R . . C49 C 0.3288(4) 0.1219(6) 0.2175(4) 0.0148(18) Uani 1 1 d . . . C50 C 0.2563(5) 0.1202(7) 0.1815(5) 0.026(2) Uani 1 1 d . . . H50 H 0.2279 0.1515 0.1987 0.031 Uiso 1 1 calc R . . C51 C 0.2259(5) 0.0734(7) 0.1211(5) 0.027(2) Uani 1 1 d . . . H51 H 0.1768 0.0722 0.0970 0.032 Uiso 1 1 calc R . . C52 C 0.2677(5) 0.0278(7) 0.0956(5) 0.031(3) Uani 1 1 d . . . H52 H 0.2471 -0.0046 0.0541 0.038 Uiso 1 1 calc R . . C53 C 0.3384(5) 0.0299(7) 0.1304(5) 0.023(2) Uani 1 1 d . . . H53 H 0.3664 -0.0009 0.1125 0.027 Uiso 1 1 calc R . . C54 C 0.3705(5) 0.0763(7) 0.1918(5) 0.021(2) Uani 1 1 d . . . H54 H 0.4196 0.0767 0.2156 0.025 Uiso 1 1 calc R . . C55 C 0.4443(7) 0.3555(10) 0.4502(7) 0.054(4) Uani 1 1 d . . . H55A H 0.4110 0.3104 0.4548 0.081 Uiso 1 1 calc R . . H55B H 0.4636 0.3988 0.4887 0.081 Uiso 1 1 calc R . . H55C H 0.4819 0.3179 0.4471 0.081 Uiso 1 1 calc R . . C56 C 0.2595(6) 0.3382(9) 0.4449(5) 0.039(3) Uani 1 1 d . . . H56A H 0.2320 0.2778 0.4329 0.059 Uiso 1 1 calc R . . H56B H 0.2354 0.3874 0.4591 0.059 Uiso 1 1 calc R . . H56C H 0.3051 0.3248 0.4811 0.059 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 Th1 0.01131(15) 0.01103(17) 0.01356(17) 0.00029(12) 0.00299(13) 0.00072(12) Re1 0.01624(18) 0.0187(2) 0.0279(2) 0.00063(16) 0.00761(17) -0.00501(14) Re2 0.0450(3) 0.0161(2) 0.0184(2) -0.00282(16) 0.01247(19) -0.00073(17) Re3 0.01873(18) 0.0265(2) 0.0199(2) -0.00371(16) 0.00446(16) -0.01102(16) P1 0.0137(10) 0.0127(11) 0.0242(13) -0.0018(10) 0.0062(10) 0.0004(9) P2 0.0121(10) 0.0117(11) 0.0177(12) 0.0004(9) 0.0020(9) -0.0005(8) P3 0.0111(9) 0.0122(11) 0.0179(12) 0.0005(9) 0.0033(9) 0.0024(9) O1 0.020(3) 0.016(3) 0.027(4) -0.006(3) 0.011(3) -0.002(3) O2 0.013(3) 0.016(3) 0.021(3) -0.001(3) -0.003(3) -0.006(2) O3 0.018(3) 0.009(3) 0.026(4) -0.002(3) 0.012(3) 0.006(2) O4 0.021(3) 0.017(3) 0.032(4) 0.003(3) 0.015(3) -0.003(3) O5 0.042(5) 0.041(5) 0.064(6) 0.026(5) -0.007(4) -0.017(4) O6 0.038(4) 0.025(4) 0.052(5) -0.006(4) 0.021(4) -0.014(3) O7 0.059(5) 0.038(5) 0.078(7) -0.005(5) 0.057(5) -0.005(4) O8 0.029(3) 0.019(4) 0.018(3) -0.002(3) 0.005(3) -0.002(3) O9 0.058(5) 0.044(5) 0.025(4) 0.004(4) 0.004(4) 0.007(4) O10 0.113(8) 0.037(5) 0.032(5) -0.010(4) 0.030(5) -0.029(5) O11 0.074(6) 0.041(5) 0.054(6) 0.003(4) 0.042(5) 0.018(4) O12 0.030(4) 0.037(4) 0.027(4) -0.013(3) 0.012(3) -0.022(3) O13 0.027(4) 0.034(4) 0.044(5) -0.001(4) 0.019(4) -0.008(3) O14 0.035(4) 0.067(6) 0.016(4) 0.002(4) -0.013(3) -0.019(4) O15 0.038(4) 0.064(6) 0.053(6) -0.013(5) 0.027(4) -0.008(4) O16 0.029(3) 0.025(4) 0.025(4) -0.003(3) 0.013(3) 0.002(3) O17 0.022(3) 0.031(4) 0.029(4) -0.001(3) 0.002(3) 0.003(3) C1 0.020(4) 0.011(4) 0.023(5) -0.006(4) 0.007(4) 0.005(4) C2 0.016(4) 0.024(5) 0.027(5) -0.001(4) 0.008(4) 0.002(4) C3 0.028(5) 0.018(5) 0.025(5) 0.008(4) 0.005(5) 0.007(4) C4 0.043(6) 0.012(5) 0.039(6) 0.004(5) 0.022(5) 0.005(4) C5 0.023(5) 0.030(6) 0.039(7) 0.002(5) 0.001(5) -0.018(4) C6 0.026(5) 0.019(5) 0.033(6) 0.000(5) 0.003(5) -0.004(4) C7 0.021(4) 0.013(5) 0.031(6) -0.004(4) 0.012(4) -0.006(4) C8 0.025(5) 0.022(5) 0.028(5) -0.002(4) 0.008(4) -0.001(4) C9 0.023(5) 0.018(5) 0.041(6) -0.014(5) 0.010(5) -0.006(4) C10 0.032(5) 0.036(6) 0.026(6) 0.001(5) 0.014(5) -0.010(5) C11 0.036(5) 0.027(6) 0.045(7) 0.002(5) 0.025(6) -0.004(5) C12 0.028(5) 0.014(5) 0.037(6) -0.002(4) 0.012(5) -0.006(4) C13 0.015(4) 0.006(4) 0.032(6) -0.001(4) 0.003(4) 0.000(3) C14 0.023(5) 0.025(5) 0.025(5) 0.011(5) 0.004(4) -0.002(4) C15 0.019(5) 0.020(6) 0.072(9) 0.001(6) 0.007(6) -0.001(4) C16 0.020(5) 0.021(5) 0.047(7) -0.003(5) -0.007(5) 0.001(4) C17 0.025(5) 0.038(7) 0.051(8) -0.021(6) 0.002(5) 0.007(5) C18 0.020(5) 0.040(7) 0.045(7) -0.001(6) 0.003(5) 0.004(5) C19 0.017(4) 0.020(5) 0.009(4) 0.001(4) 0.005(4) 0.001(4) C20 0.012(4) 0.022(5) 0.024(5) 0.000(4) 0.006(4) -0.003(4) C21 0.033(5) 0.014(5) 0.035(6) 0.000(4) 0.019(5) 0.002(4) C22 0.017(4) 0.023(5) 0.037(6) 0.015(5) 0.014(4) 0.006(4) C23 0.011(4) 0.024(5) 0.030(6) 0.008(4) -0.001(4) -0.005(4) C24 0.020(4) 0.016(5) 0.015(4) 0.003(4) 0.006(4) -0.001(4) C25 0.011(4) 0.013(4) 0.018(5) -0.004(4) -0.003(4) -0.001(3) C26 0.019(4) 0.027(5) 0.018(5) -0.003(4) 0.000(4) 0.001(4) C27 0.031(5) 0.021(5) 0.011(4) 0.003(4) 0.005(4) 0.002(4) C28 0.024(5) 0.024(5) 0.026(6) -0.007(4) 0.000(4) -0.004(4) C29 0.021(5) 0.030(6) 0.036(6) -0.004(5) 0.007(5) -0.007(4) C30 0.015(4) 0.020(5) 0.020(5) 0.000(4) -0.003(4) 0.001(4) C31 0.015(4) 0.007(4) 0.026(5) -0.002(4) 0.004(4) -0.007(3) C32 0.019(4) 0.013(4) 0.015(4) 0.005(4) 0.010(4) 0.003(3) C33 0.034(5) 0.024(5) 0.029(6) 0.005(5) 0.014(5) -0.002(4) C34 0.026(5) 0.011(5) 0.037(6) 0.002(4) 0.004(5) 0.000(4) C35 0.022(4) 0.017(5) 0.024(5) 0.011(4) 0.000(4) -0.007(4) C36 0.010(4) 0.019(5) 0.017(5) 0.001(4) 0.001(4) 0.001(3) C37 0.008(4) 0.023(5) 0.018(5) -0.004(4) 0.008(4) 0.004(3) C38 0.023(4) 0.021(5) 0.016(5) -0.003(4) 0.010(4) -0.003(4) C39 0.007(4) 0.018(5) 0.021(5) -0.001(4) 0.001(4) 0.009(3) C40 0.018(4) 0.026(5) 0.022(5) -0.013(4) 0.006(4) -0.001(4) C41 0.012(4) 0.020(5) 0.030(5) -0.001(4) 0.009(4) 0.001(4) C42 0.021(4) 0.012(5) 0.029(5) 0.000(4) 0.006(4) -0.003(4) C43 0.014(4) 0.007(4) 0.020(5) 0.003(4) -0.004(4) 0.003(3) C44 0.039(6) 0.024(6) 0.028(6) 0.008(5) 0.015(5) 0.004(5) C45 0.041(6) 0.046(7) 0.018(5) 0.010(5) 0.014(5) 0.003(5) C46 0.038(5) 0.024(5) 0.019(5) 0.000(4) 0.009(5) -0.005(5) C47 0.031(5) 0.007(5) 0.057(8) 0.008(5) 0.018(5) -0.003(4) C48 0.014(4) 0.016(5) 0.026(5) 0.000(4) 0.007(4) 0.000(4) C49 0.015(4) 0.013(4) 0.017(5) -0.002(4) 0.008(4) 0.002(3) C50 0.021(5) 0.030(6) 0.021(5) 0.001(4) 0.003(4) -0.007(4) C51 0.029(5) 0.024(5) 0.032(6) -0.010(5) 0.016(5) -0.005(4) C52 0.042(6) 0.013(5) 0.027(6) -0.004(4) 0.003(5) -0.006(4) C53 0.040(5) 0.016(5) 0.019(5) 0.008(4) 0.020(5) 0.005(4) C54 0.023(4) 0.020(5) 0.022(5) 0.004(4) 0.012(4) 0.002(4) C55 0.050(7) 0.052(8) 0.052(8) -0.014(7) 0.015(7) 0.013(6) C56 0.035(6) 0.054(8) 0.029(6) 0.020(6) 0.013(5) 0.021(6) _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 Th1 O16 2.121(7) . ? Th1 O3 2.355(6) . ? Th1 O1 2.373(6) . ? Th1 O2 2.443(7) . ? Th1 O12 2.464(7) . ? Th1 O4 2.479(6) . ? Th1 O8 2.487(6) . ? Th1 O17 2.574(6) . ? Re1 O7 1.678(8) . ? Re1 O5 1.703(8) . ? Re1 O6 1.706(8) . ? Re1 O4 1.759(6) . ? Re2 O10 1.692(8) . ? Re2 O11 1.711(9) . ? Re2 O9 1.721(8) . ? Re2 O8 1.753(7) . ? Re3 O13 1.692(8) . ? Re3 O15 1.704(9) . ? Re3 O14 1.721(7) . ? Re3 O12 1.743(6) . ? P1 O1 1.503(6) . ? P1 C7 1.775(11) . ? P1 C1 1.782(9) . ? P1 C13 1.799(9) . ? P2 O2 1.493(7) . ? P2 C19 1.791(9) . ? P2 C25 1.809(8) . ? P2 C31 1.817(9) . ? P3 O3 1.516(6) . ? P3 C49 1.778(9) . ? P3 C37 1.788(8) . ? P3 C43 1.799(10) . ? O16 C56 1.393(12) . ? O17 C55 1.465(15) . ? C1 C6 1.381(12) . ? C1 C2 1.414(12) . ? C2 C3 1.406(13) . ? C2 H2 0.9500 . ? C3 C4 1.355(14) . ? C3 H3 0.9500 . ? C4 C5 1.388(14) . ? C4 H4 0.9500 . ? C5 C6 1.389(14) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.376(13) . ? C7 C12 1.415(13) . ? C8 C9 1.381(15) . ? C8 H8 0.9500 . ? C9 C10 1.409(14) . ? C9 H9 0.9500 . ? C10 C11 1.367(15) . ? C10 H10 0.9500 . ? C11 C12 1.388(15) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.376(16) . ? C13 C14 1.396(13) . ? C14 C15 1.385(14) . ? C14 H14 0.9500 . ? C15 C16 1.365(18) . ? C15 H15 0.9500 . ? C16 C17 1.370(16) . ? C16 H16 0.9500 . ? C17 C18 1.402(14) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.393(13) . ? C19 C24 1.398(12) . ? C20 C21 1.392(12) . ? C20 H20 0.9500 . ? C21 C22 1.383(13) . ? C21 H21 0.9500 . ? C22 C23 1.406(14) . ? C22 H22 0.9500 . ? C23 C24 1.369(12) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.384(14) . ? C25 C26 1.391(13) . ? C26 C27 1.389(13) . ? C26 H26 0.9500 . ? C27 C28 1.371(14) . ? C27 H27 0.9500 . ? C28 C29 1.360(16) . ? C28 H28 0.9500 . ? C29 C30 1.406(12) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.375(13) . ? C31 C36 1.388(13) . ? C32 C33 1.392(13) . ? C32 H32 0.9500 . ? C33 C34 1.376(15) . ? C33 H33 0.9500 . ? C34 C35 1.381(15) . ? C34 H34 0.9500 . ? C35 C36 1.385(12) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.375(13) . ? C37 C38 1.408(12) . ? C38 C39 1.385(12) . ? C38 H38 0.9500 . ? C39 C40 1.362(13) . ? C39 H39 0.9500 . ? C40 C41 1.421(12) . ? C40 H40 0.9500 . ? C41 C42 1.395(12) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.352(15) . ? C43 C48 1.399(12) . ? C44 C45 1.408(14) . ? C44 H44 0.9500 . ? C45 C46 1.329(15) . ? C45 H45 0.9500 . ? C46 C47 1.391(16) . ? C46 H46 0.9500 . ? C47 C48 1.406(14) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C54 1.397(13) . ? C49 C50 1.403(12) . ? C50 C51 1.383(14) . ? C50 H50 0.9500 . ? C51 C52 1.398(15) . ? C51 H51 0.9500 . ? C52 C53 1.368(14) . ? C52 H52 0.9500 . ? C53 C54 1.399(13) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? 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 O16 Th1 O3 89.7(2) . . ? O16 Th1 O1 96.4(2) . . ? O3 Th1 O1 146.6(2) . . ? O16 Th1 O2 149.5(2) . . ? O3 Th1 O2 78.2(2) . . ? O1 Th1 O2 80.1(2) . . ? O16 Th1 O12 142.1(2) . . ? O3 Th1 O12 103.0(2) . . ? O1 Th1 O12 92.1(2) . . ? O2 Th1 O12 68.3(2) . . ? O16 Th1 O4 78.4(2) . . ? O3 Th1 O4 75.0(2) . . ? O1 Th1 O4 74.2(2) . . ? O2 Th1 O4 71.5(2) . . ? O12 Th1 O4 139.2(2) . . ? O16 Th1 O8 80.3(2) . . ? O3 Th1 O8 142.2(2) . . ? O1 Th1 O8 71.1(2) . . ? O2 Th1 O8 125.6(2) . . ? O12 Th1 O8 67.7(2) . . ? O4 Th1 O8 136.6(2) . . ? O16 Th1 O17 81.0(2) . . ? O3 Th1 O17 72.7(2) . . ? O1 Th1 O17 140.6(2) . . ? O2 Th1 O17 120.6(2) . . ? O12 Th1 O17 69.4(2) . . ? O4 Th1 O17 141.5(2) . . ? O8 Th1 O17 69.7(2) . . ? O7 Re1 O5 108.4(5) . . ? O7 Re1 O6 110.1(4) . . ? O5 Re1 O6 107.9(4) . . ? O7 Re1 O4 109.2(3) . . ? O5 Re1 O4 112.2(3) . . ? O6 Re1 O4 108.9(3) . . ? O10 Re2 O11 108.2(5) . . ? O10 Re2 O9 108.8(4) . . ? O11 Re2 O9 109.6(4) . . ? O10 Re2 O8 108.6(4) . . ? O11 Re2 O8 110.7(4) . . ? O9 Re2 O8 110.7(4) . . ? O13 Re3 O15 109.5(4) . . ? O13 Re3 O14 108.2(4) . . ? O15 Re3 O14 110.0(4) . . ? O13 Re3 O12 108.0(3) . . ? O15 Re3 O12 111.2(4) . . ? O14 Re3 O12 109.8(4) . . ? O1 P1 C7 112.4(4) . . ? O1 P1 C1 109.7(4) . . ? C7 P1 C1 107.5(4) . . ? O1 P1 C13 109.3(4) . . ? C7 P1 C13 106.9(5) . . ? C1 P1 C13 110.9(4) . . ? O2 P2 C19 114.2(4) . . ? O2 P2 C25 108.8(4) . . ? C19 P2 C25 108.1(4) . . ? O2 P2 C31 110.8(4) . . ? C19 P2 C31 104.8(4) . . ? C25 P2 C31 110.0(4) . . ? O3 P3 C49 110.2(4) . . ? O3 P3 C37 109.1(4) . . ? C49 P3 C37 109.9(4) . . ? O3 P3 C43 110.5(4) . . ? C49 P3 C43 107.8(4) . . ? C37 P3 C43 109.4(4) . . ? P1 O1 Th1 164.4(4) . . ? P2 O2 Th1 163.9(4) . . ? P3 O3 Th1 166.7(4) . . ? Re1 O4 Th1 144.2(4) . . ? Re2 O8 Th1 139.7(3) . . ? Re3 O12 Th1 144.2(4) . . ? C56 O16 Th1 178.5(7) . . ? C55 O17 Th1 131.1(7) . . ? C6 C1 C2 118.5(9) . . ? C6 C1 P1 119.8(7) . . ? C2 C1 P1 121.4(7) . . ? C3 C2 C1 120.2(8) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.1(9) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.9(9) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 121.1(9) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C1 C6 C5 120.1(9) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C12 118.6(10) . . ? C8 C7 P1 123.4(8) . . ? C12 C7 P1 118.1(8) . . ? C7 C8 C9 121.3(10) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C10 119.4(10) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C10 C9 120.1(10) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.1(10) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 120.3(10) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? C18 C13 C14 120.2(9) . . ? C18 C13 P1 117.8(7) . . ? C14 C13 P1 121.9(8) . . ? C15 C14 C13 119.2(11) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C16 C15 C14 120.4(11) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 121.1(10) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C16 C17 C18 119.4(12) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C13 C18 C17 119.7(11) . . ? C13 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C20 C19 C24 119.4(8) . . ? C20 C19 P2 122.5(7) . . ? C24 C19 P2 118.0(7) . . ? C21 C20 C19 121.6(8) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C22 C21 C20 118.5(9) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C21 C22 C23 120.0(8) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 121.3(8) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C19 119.2(9) . . ? C23 C24 H24 120.4 . . ? C19 C24 H24 120.4 . . ? C30 C25 C26 119.7(8) . . ? C30 C25 P2 117.6(7) . . ? C26 C25 P2 122.7(8) . . ? C27 C26 C25 120.0(10) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 119.6(9) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C29 C28 C27 121.5(9) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C29 C30 119.6(10) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C25 C30 C29 119.6(9) . . ? C25 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C32 C31 C36 118.7(8) . . ? C32 C31 P2 119.4(7) . . ? C36 C31 P2 121.8(7) . . ? C31 C32 C33 121.4(9) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C34 C33 C32 119.1(10) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 C35 120.4(9) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C36 119.9(10) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C35 C36 C31 120.4(9) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C42 C37 C38 120.6(8) . . ? C42 C37 P3 117.4(6) . . ? C38 C37 P3 122.0(7) . . ? C39 C38 C37 119.3(9) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C40 C39 C38 121.2(8) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C41 119.6(8) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C42 C41 C40 119.7(9) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C37 C42 C41 119.7(8) . . ? C37 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C44 C43 C48 122.7(9) . . ? C44 C43 P3 117.5(7) . . ? C48 C43 P3 119.8(8) . . ? C43 C44 C45 117.4(10) . . ? C43 C44 H44 121.3 . . ? C45 C44 H44 121.3 . . ? C46 C45 C44 122.9(11) . . ? C46 C45 H45 118.5 . . ? C44 C45 H45 118.5 . . ? C45 C46 C47 119.1(10) . . ? C45 C46 H46 120.4 . . ? C47 C46 H46 120.4 . . ? C46 C47 C48 120.7(9) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? C43 C48 C47 117.1(9) . . ? C43 C48 H48 121.5 . . ? C47 C48 H48 121.5 . . ? C54 C49 C50 119.6(9) . . ? C54 C49 P3 121.9(7) . . ? C50 C49 P3 118.4(7) . . ? C51 C50 C49 120.5(10) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C50 C51 C52 119.7(9) . . ? C50 C51 H51 120.1 . . ? C52 C51 H51 120.1 . . ? C53 C52 C51 119.8(10) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C52 C53 C54 121.6(10) . . ? C52 C53 H53 119.2 . . ? C54 C53 H53 119.2 . . ? C49 C54 C53 118.8(8) . . ? C49 C54 H54 120.6 . . ? C53 C54 H54 120.6 . . ? O17 C55 H55A 109.5 . . ? O17 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? O17 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O16 C56 H56A 109.5 . . ? O16 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O16 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 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 C7 P1 O1 Th1 16.7(15) . . . . ? C1 P1 O1 Th1 136.3(14) . . . . ? C13 P1 O1 Th1 -101.9(14) . . . . ? O16 Th1 O1 P1 -2.8(14) . . . . ? O3 Th1 O1 P1 96.5(14) . . . . ? O2 Th1 O1 P1 146.6(14) . . . . ? O12 Th1 O1 P1 -145.8(14) . . . . ? O4 Th1 O1 P1 73.2(14) . . . . ? O8 Th1 O1 P1 -80.3(14) . . . . ? O17 Th1 O1 P1 -86.5(14) . . . . ? C19 P2 O2 Th1 50.4(15) . . . . ? C25 P2 O2 Th1 171.2(13) . . . . ? C31 P2 O2 Th1 -67.7(15) . . . . ? O16 Th1 O2 P2 -164.3(12) . . . . ? O3 Th1 O2 P2 -95.6(14) . . . . ? O1 Th1 O2 P2 109.9(14) . . . . ? O12 Th1 O2 P2 13.6(14) . . . . ? O4 Th1 O2 P2 -173.5(15) . . . . ? O8 Th1 O2 P2 51.8(15) . . . . ? O17 Th1 O2 P2 -34.0(15) . . . . ? C49 P3 O3 Th1 -129.3(17) . . . . ? C37 P3 O3 Th1 -8.5(19) . . . . ? C43 P3 O3 Th1 111.7(18) . . . . ? O16 Th1 O3 P3 -104.0(18) . . . . ? O1 Th1 O3 P3 154.6(16) . . . . ? O2 Th1 O3 P3 104.2(18) . . . . ? O12 Th1 O3 P3 40.0(18) . . . . ? O4 Th1 O3 P3 177.9(18) . . . . ? O8 Th1 O3 P3 -30(2) . . . . ? O17 Th1 O3 P3 -23.3(17) . . . . ? O7 Re1 O4 Th1 94.7(6) . . . . ? O5 Re1 O4 Th1 -25.6(8) . . . . ? O6 Re1 O4 Th1 -145.0(6) . . . . ? O16 Th1 O4 Re1 -22.3(6) . . . . ? O3 Th1 O4 Re1 70.6(6) . . . . ? O1 Th1 O4 Re1 -122.4(6) . . . . ? O2 Th1 O4 Re1 153.0(6) . . . . ? O12 Th1 O4 Re1 163.2(5) . . . . ? O8 Th1 O4 Re1 -84.5(6) . . . . ? O17 Th1 O4 Re1 36.8(8) . . . . ? O10 Re2 O8 Th1 170.2(6) . . . . ? O11 Re2 O8 Th1 -71.1(6) . . . . ? O9 Re2 O8 Th1 50.7(6) . . . . ? O16 Th1 O8 Re2 13.3(5) . . . . ? O3 Th1 O8 Re2 -63.6(7) . . . . ? O1 Th1 O8 Re2 113.6(6) . . . . ? O2 Th1 O8 Re2 175.6(4) . . . . ? O12 Th1 O8 Re2 -146.0(6) . . . . ? O4 Th1 O8 Re2 74.8(6) . . . . ? O17 Th1 O8 Re2 -70.7(5) . . . . ? O13 Re3 O12 Th1 146.0(6) . . . . ? O15 Re3 O12 Th1 -93.8(7) . . . . ? O14 Re3 O12 Th1 28.2(8) . . . . ? O16 Th1 O12 Re3 -5.2(9) . . . . ? O3 Th1 O12 Re3 -112.0(7) . . . . ? O1 Th1 O12 Re3 98.0(7) . . . . ? O2 Th1 O12 Re3 176.5(8) . . . . ? O4 Th1 O12 Re3 166.1(5) . . . . ? O8 Th1 O12 Re3 29.4(6) . . . . ? O17 Th1 O12 Re3 -46.3(7) . . . . ? O3 Th1 O16 C56 -20(25) . . . . ? O1 Th1 O16 C56 127(25) . . . . ? O2 Th1 O16 C56 46(25) . . . . ? O12 Th1 O16 C56 -131(25) . . . . ? O4 Th1 O16 C56 55(25) . . . . ? O8 Th1 O16 C56 -163(25) . . . . ? O17 Th1 O16 C56 -92(25) . . . . ? O16 Th1 O17 C55 25.0(9) . . . . ? O3 Th1 O17 C55 -67.5(9) . . . . ? O1 Th1 O17 C55 114.2(9) . . . . ? O2 Th1 O17 C55 -131.9(8) . . . . ? O12 Th1 O17 C55 -179.1(9) . . . . ? O4 Th1 O17 C55 -33.3(10) . . . . ? O8 Th1 O17 C55 108.0(9) . . . . ? O1 P1 C1 C6 -34.7(10) . . . . ? C7 P1 C1 C6 87.8(9) . . . . ? C13 P1 C1 C6 -155.6(9) . . . . ? O1 P1 C1 C2 151.3(8) . . . . ? C7 P1 C1 C2 -86.1(9) . . . . ? C13 P1 C1 C2 30.5(10) . . . . ? C6 C1 C2 C3 1.1(16) . . . . ? P1 C1 C2 C3 175.1(8) . . . . ? C1 C2 C3 C4 -1.3(16) . . . . ? C2 C3 C4 C5 2.0(17) . . . . ? C3 C4 C5 C6 -2.6(19) . . . . ? C2 C1 C6 C5 -1.7(17) . . . . ? P1 C1 C6 C5 -175.8(9) . . . . ? C4 C5 C6 C1 2.5(18) . . . . ? O1 P1 C7 C8 137.3(8) . . . . ? C1 P1 C7 C8 16.5(9) . . . . ? C13 P1 C7 C8 -102.7(8) . . . . ? O1 P1 C7 C12 -44.3(8) . . . . ? C1 P1 C7 C12 -165.1(7) . . . . ? C13 P1 C7 C12 75.7(8) . . . . ? C12 C7 C8 C9 2.1(14) . . . . ? P1 C7 C8 C9 -179.6(7) . . . . ? C7 C8 C9 C10 -2.8(14) . . . . ? C8 C9 C10 C11 3.7(14) . . . . ? C9 C10 C11 C12 -3.9(15) . . . . ? C10 C11 C12 C7 3.2(15) . . . . ? C8 C7 C12 C11 -2.3(14) . . . . ? P1 C7 C12 C11 179.3(8) . . . . ? O1 P1 C13 C18 -42.0(9) . . . . ? C7 P1 C13 C18 -163.9(8) . . . . ? C1 P1 C13 C18 79.1(9) . . . . ? O1 P1 C13 C14 134.7(7) . . . . ? C7 P1 C13 C14 12.8(9) . . . . ? C1 P1 C13 C14 -104.2(8) . . . . ? C18 C13 C14 C15 0.1(14) . . . . ? P1 C13 C14 C15 -176.6(8) . . . . ? C13 C14 C15 C16 -0.3(15) . . . . ? C14 C15 C16 C17 0.7(17) . . . . ? C15 C16 C17 C18 -0.7(17) . . . . ? C14 C13 C18 C17 -0.1(16) . . . . ? P1 C13 C18 C17 176.7(9) . . . . ? C16 C17 C18 C13 0.4(17) . . . . ? O2 P2 C19 C20 94.4(8) . . . . ? C25 P2 C19 C20 -26.9(9) . . . . ? C31 P2 C19 C20 -144.1(8) . . . . ? O2 P2 C19 C24 -82.5(8) . . . . ? C25 P2 C19 C24 156.3(7) . . . . ? C31 P2 C19 C24 39.0(8) . . . . ? C24 C19 C20 C21 -2.0(14) . . . . ? P2 C19 C20 C21 -178.9(8) . . . . ? C19 C20 C21 C22 1.6(15) . . . . ? C20 C21 C22 C23 -1.2(15) . . . . ? C21 C22 C23 C24 1.4(15) . . . . ? C22 C23 C24 C19 -1.8(14) . . . . ? C20 C19 C24 C23 2.1(13) . . . . ? P2 C19 C24 C23 179.1(7) . . . . ? O2 P2 C25 C30 2.4(8) . . . . ? C19 P2 C25 C30 126.9(7) . . . . ? C31 P2 C25 C30 -119.2(8) . . . . ? O2 P2 C25 C26 -179.9(8) . . . . ? C19 P2 C25 C26 -55.4(9) . . . . ? C31 P2 C25 C26 58.5(9) . . . . ? C30 C25 C26 C27 0.2(14) . . . . ? P2 C25 C26 C27 -177.5(7) . . . . ? C25 C26 C27 C28 1.1(14) . . . . ? C26 C27 C28 C29 -1.1(16) . . . . ? C27 C28 C29 C30 -0.1(16) . . . . ? C26 C25 C30 C29 -1.4(14) . . . . ? P2 C25 C30 C29 176.4(7) . . . . ? C28 C29 C30 C25 1.4(15) . . . . ? O2 P2 C31 C32 -11.9(8) . . . . ? C19 P2 C31 C32 -135.5(7) . . . . ? C25 P2 C31 C32 108.6(7) . . . . ? O2 P2 C31 C36 171.2(6) . . . . ? C19 P2 C31 C36 47.6(8) . . . . ? C25 P2 C31 C36 -68.4(8) . . . . ? C36 C31 C32 C33 -3.5(13) . . . . ? P2 C31 C32 C33 179.4(7) . . . . ? C31 C32 C33 C34 1.7(14) . . . . ? C32 C33 C34 C35 0.6(14) . . . . ? C33 C34 C35 C36 -1.0(14) . . . . ? C34 C35 C36 C31 -0.8(13) . . . . ? C32 C31 C36 C35 3.0(12) . . . . ? P2 C31 C36 C35 180.0(6) . . . . ? O3 P3 C37 C42 -53.3(8) . . . . ? C49 P3 C37 C42 67.6(8) . . . . ? C43 P3 C37 C42 -174.2(7) . . . . ? O3 P3 C37 C38 124.9(8) . . . . ? C49 P3 C37 C38 -114.2(8) . . . . ? C43 P3 C37 C38 4.0(9) . . . . ? C42 C37 C38 C39 0.8(14) . . . . ? P3 C37 C38 C39 -177.4(7) . . . . ? C37 C38 C39 C40 -0.5(14) . . . . ? C38 C39 C40 C41 0.5(14) . . . . ? C39 C40 C41 C42 -0.7(14) . . . . ? C38 C37 C42 C41 -1.0(14) . . . . ? P3 C37 C42 C41 177.2(8) . . . . ? C40 C41 C42 C37 1.0(15) . . . . ? O3 P3 C43 C44 -19.7(8) . . . . ? C49 P3 C43 C44 -140.2(8) . . . . ? C37 P3 C43 C44 100.3(8) . . . . ? O3 P3 C43 C48 159.3(6) . . . . ? C49 P3 C43 C48 38.8(8) . . . . ? C37 P3 C43 C48 -80.7(7) . . . . ? C48 C43 C44 C45 2.8(14) . . . . ? P3 C43 C44 C45 -178.2(7) . . . . ? C43 C44 C45 C46 -1.3(16) . . . . ? C44 C45 C46 C47 0.3(16) . . . . ? C45 C46 C47 C48 -0.7(15) . . . . ? C44 C43 C48 C47 -3.2(13) . . . . ? P3 C43 C48 C47 177.8(7) . . . . ? C46 C47 C48 C43 2.1(13) . . . . ? O3 P3 C49 C54 146.4(7) . . . . ? C37 P3 C49 C54 26.2(9) . . . . ? C43 P3 C49 C54 -92.9(8) . . . . ? O3 P3 C49 C50 -36.2(9) . . . . ? C37 P3 C49 C50 -156.4(7) . . . . ? C43 P3 C49 C50 84.4(8) . . . . ? C54 C49 C50 C51 0.3(14) . . . . ? P3 C49 C50 C51 -177.1(8) . . . . ? C49 C50 C51 C52 -0.3(15) . . . . ? C50 C51 C52 C53 -0.1(16) . . . . ? C51 C52 C53 C54 0.5(15) . . . . ? C50 C49 C54 C53 0.1(14) . . . . ? P3 C49 C54 C53 177.4(7) . . . . ? C52 C53 C54 C49 -0.5(14) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 3.718 _refine_diff_density_min -2.762 _refine_diff_density_rms 0.291