# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_P(phi)~4~.NO~2~.EtOH _database_code_depnum_ccdc_archive 'CCDC 915618' #TrackingRef 'web_deposit_cif_file_0_P.Thuery_1355410149.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H26 N O3 P' _chemical_formula_weight 431.45 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.7202(5) _cell_length_b 7.6215(2) _cell_length_c 15.8566(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2262.36(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 57297 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 30.51 _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.808 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and three \w scans with 2\% steps (333 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 57297 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 30.51 _reflns_number_total 6561 _reflns_number_gt 5699 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atom bound to O3 was found on a Fourier-difference map and all the others were introduced at calculated positions; all were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom (1.5 for CH~3~). 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^)+(0.0839P)^2^+0.3692P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.41(8) _refine_ls_number_reflns 6561 _refine_ls_number_parameters 282 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.964 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.048 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 P1 P 0.20280(2) 0.45275(5) 0.95838(3) 0.02754(11) Uani 1 1 d . . . O1 O 0.64236(16) 0.3751(4) 0.64724(18) 0.0891(8) Uani 1 1 d . . . O2 O 0.54468(11) 0.2420(2) 0.61679(17) 0.0645(5) Uani 1 1 d . . . O3 O 0.42420(8) 0.1830(2) 0.70960(11) 0.0453(4) Uani 1 1 d . . . H3 H 0.4625 0.2102 0.6771 0.054 Uiso 1 1 d R . . N1 N 0.58859(12) 0.3141(3) 0.6798(2) 0.0713(8) Uani 1 1 d . . . C1 C 0.15093(9) 0.3116(2) 0.89183(12) 0.0290(3) Uani 1 1 d . . . C2 C 0.09894(11) 0.3840(3) 0.83898(13) 0.0355(4) Uani 1 1 d . . . H2 H 0.0936 0.5052 0.8360 0.043 Uiso 1 1 calc R . . C3 C 0.05548(11) 0.2765(3) 0.79123(15) 0.0392(4) Uani 1 1 d . . . H3A H 0.0213 0.3255 0.7558 0.047 Uiso 1 1 calc R . . C4 C 0.06278(12) 0.0951(3) 0.79593(13) 0.0392(4) Uani 1 1 d . . . H4 H 0.0326 0.0228 0.7649 0.047 Uiso 1 1 calc R . . C5 C 0.11483(13) 0.0229(3) 0.84670(16) 0.0441(5) Uani 1 1 d . . . H5 H 0.1203 -0.0983 0.8488 0.053 Uiso 1 1 calc R . . C6 C 0.15935(11) 0.1294(3) 0.89494(14) 0.0366(4) Uani 1 1 d . . . H6 H 0.1944 0.0798 0.9290 0.044 Uiso 1 1 calc R . . C7 C 0.14139(10) 0.5940(2) 1.01253(12) 0.0299(3) Uani 1 1 d . . . C8 C 0.07255(10) 0.5346(3) 1.03188(14) 0.0357(4) Uani 1 1 d . . . H8 H 0.0593 0.4204 1.0185 0.043 Uiso 1 1 calc R . . C9 C 0.02403(11) 0.6462(3) 1.07106(14) 0.0386(4) Uani 1 1 d . . . H9 H -0.0217 0.6069 1.0839 0.046 Uiso 1 1 calc R . . C10 C 0.04412(12) 0.8162(3) 1.09088(13) 0.0389(4) Uani 1 1 d . . . H10 H 0.0112 0.8923 1.1152 0.047 Uiso 1 1 calc R . . C11 C 0.11360(12) 0.8739(3) 1.07459(13) 0.0397(4) Uani 1 1 d . . . H11 H 0.1274 0.9864 1.0904 0.048 Uiso 1 1 calc R . . C12 C 0.16195(11) 0.7643(2) 1.03506(13) 0.0332(4) Uani 1 1 d . . . H12 H 0.2080 0.8035 1.0235 0.040 Uiso 1 1 calc R . . C13 C 0.25074(9) 0.3197(2) 1.03182(12) 0.0293(3) Uani 1 1 d . . . C14 C 0.22565(11) 0.2987(3) 1.11332(14) 0.0389(4) Uani 1 1 d . . . H14 H 0.1872 0.3651 1.1324 0.047 Uiso 1 1 calc R . . C15 C 0.25839(15) 0.1773(3) 1.16649(14) 0.0474(5) Uani 1 1 d . . . H15 H 0.2421 0.1630 1.2215 0.057 Uiso 1 1 calc R . . C16 C 0.31554(13) 0.0773(3) 1.13717(16) 0.0448(5) Uani 1 1 d . . . H16 H 0.3364 -0.0062 1.1721 0.054 Uiso 1 1 calc R . . C17 C 0.34144(12) 0.1016(3) 1.05633(16) 0.0438(5) Uani 1 1 d . . . H17 H 0.3804 0.0366 1.0376 0.053 Uiso 1 1 calc R . . C18 C 0.30958(11) 0.2220(3) 1.00353(14) 0.0393(4) Uani 1 1 d . . . H18 H 0.3271 0.2385 0.9492 0.047 Uiso 1 1 calc R . . C19 C 0.26423(9) 0.5833(2) 0.89812(12) 0.0304(3) Uani 1 1 d . . . C20 C 0.32525(10) 0.6501(3) 0.93789(13) 0.0355(4) Uani 1 1 d . . . H20 H 0.3354 0.6206 0.9935 0.043 Uiso 1 1 calc R . . C21 C 0.37081(12) 0.7616(3) 0.89302(16) 0.0417(4) Uani 1 1 d . . . H21 H 0.4115 0.8065 0.9189 0.050 Uiso 1 1 calc R . . C22 C 0.35547(13) 0.8055(3) 0.80976(16) 0.0438(5) Uani 1 1 d . . . H22 H 0.3855 0.8812 0.7804 0.053 Uiso 1 1 calc R . . C23 C 0.29557(13) 0.7366(3) 0.77057(15) 0.0434(5) Uani 1 1 d . . . H23 H 0.2858 0.7655 0.7148 0.052 Uiso 1 1 calc R . . C24 C 0.24976(12) 0.6242(3) 0.81429(13) 0.0368(4) Uani 1 1 d . . . H24 H 0.2099 0.5770 0.7876 0.044 Uiso 1 1 calc R . . C25 C 0.41410(13) 0.3172(3) 0.77102(16) 0.0469(5) Uani 1 1 d . . . H25A H 0.3637 0.3259 0.7844 0.056 Uiso 1 1 calc R . . H25B H 0.4291 0.4287 0.7475 0.056 Uiso 1 1 calc R . . C26 C 0.45491(12) 0.2832(3) 0.85001(17) 0.0467(5) Uani 1 1 d . . . H26A H 0.4388 0.1754 0.8749 0.070 Uiso 1 1 calc R . . H26B H 0.4473 0.3779 0.8889 0.070 Uiso 1 1 calc R . . H26C H 0.5049 0.2745 0.8372 0.070 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 P1 0.02802(19) 0.02721(19) 0.02741(19) 0.00116(17) 0.00059(17) -0.00021(15) O1 0.0932(18) 0.1069(19) 0.0673(15) 0.0014(14) 0.0013(13) -0.0188(15) O2 0.0546(11) 0.0551(10) 0.0838(15) -0.0034(10) 0.0002(10) 0.0061(8) O3 0.0464(8) 0.0418(8) 0.0478(9) -0.0077(7) -0.0015(7) -0.0039(6) N1 0.0421(10) 0.0354(10) 0.136(3) 0.0042(13) 0.0042(14) -0.0007(8) C1 0.0299(8) 0.0301(8) 0.0270(8) 0.0010(7) 0.0000(6) -0.0010(6) C2 0.0366(9) 0.0306(9) 0.0395(10) 0.0014(8) -0.0032(8) 0.0033(7) C3 0.0352(9) 0.0431(10) 0.0393(10) -0.0023(8) -0.0078(8) 0.0014(8) C4 0.0422(10) 0.0404(10) 0.0349(10) -0.0036(8) -0.0058(8) -0.0055(8) C5 0.0566(13) 0.0301(9) 0.0456(12) -0.0014(8) -0.0105(10) -0.0031(9) C6 0.0414(10) 0.0321(9) 0.0362(9) 0.0034(8) -0.0069(8) -0.0002(7) C7 0.0321(8) 0.0298(8) 0.0278(8) 0.0007(7) -0.0001(6) 0.0009(6) C8 0.0337(9) 0.0347(9) 0.0387(10) -0.0032(8) 0.0038(8) -0.0018(7) C9 0.0353(9) 0.0444(10) 0.0360(9) -0.0023(8) 0.0049(8) 0.0018(8) C10 0.0458(11) 0.0381(10) 0.0329(9) -0.0030(7) 0.0048(8) 0.0075(8) C11 0.0521(11) 0.0303(9) 0.0368(10) -0.0024(8) 0.0054(9) -0.0001(8) C12 0.0384(9) 0.0301(8) 0.0310(8) 0.0009(7) 0.0013(7) -0.0039(7) C13 0.0280(7) 0.0279(7) 0.0321(8) 0.0019(7) -0.0025(7) -0.0008(6) C14 0.0411(10) 0.0409(10) 0.0346(9) 0.0046(8) 0.0004(8) 0.0076(8) C15 0.0605(14) 0.0484(11) 0.0333(10) 0.0104(9) 0.0001(9) 0.0092(10) C16 0.0471(11) 0.0393(10) 0.0480(12) 0.0034(9) -0.0146(10) 0.0039(9) C17 0.0377(10) 0.0415(10) 0.0524(13) -0.0035(9) -0.0095(9) 0.0087(8) C18 0.0357(10) 0.0430(10) 0.0391(10) 0.0015(8) 0.0008(8) 0.0057(8) C19 0.0311(8) 0.0287(7) 0.0315(8) 0.0022(7) 0.0039(7) 0.0004(6) C20 0.0346(9) 0.0378(9) 0.0340(9) -0.0009(7) 0.0024(7) -0.0041(7) C21 0.0367(9) 0.0394(10) 0.0490(11) -0.0021(9) 0.0062(9) -0.0086(8) C22 0.0445(11) 0.0372(10) 0.0497(13) 0.0044(9) 0.0141(9) -0.0040(8) C23 0.0498(12) 0.0420(11) 0.0384(11) 0.0101(9) 0.0052(9) 0.0003(9) C24 0.0387(9) 0.0367(9) 0.0350(9) 0.0042(8) 0.0016(7) 0.0037(8) C25 0.0486(12) 0.0401(11) 0.0519(13) -0.0073(10) -0.0004(10) 0.0054(9) C26 0.0400(11) 0.0538(12) 0.0462(12) -0.0126(10) 0.0031(9) -0.0020(9) _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 P1 C13 1.7859(18) . ? P1 C1 1.7924(18) . ? P1 C7 1.7940(19) . ? P1 C19 1.7959(18) . ? O1 N1 1.223(4) . ? O2 N1 1.406(4) . ? O3 C25 1.425(3) . ? O3 H3 0.9071 . ? C1 C2 1.398(3) . ? C1 C6 1.399(3) . ? C2 C3 1.381(3) . ? C2 H2 0.9300 . ? C3 C4 1.391(3) . ? C3 H3A 0.9300 . ? C4 C5 1.379(3) . ? C4 H4 0.9300 . ? C5 C6 1.392(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.400(3) . ? C7 C12 1.400(3) . ? C8 C9 1.391(3) . ? C8 H8 0.9300 . ? C9 C10 1.385(3) . ? C9 H9 0.9300 . ? C10 C11 1.397(3) . ? C10 H10 0.9300 . ? C11 C12 1.382(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.384(3) . ? C13 C18 1.403(3) . ? C14 C15 1.394(3) . ? C14 H14 0.9300 . ? C15 C16 1.393(3) . ? C15 H15 0.9300 . ? C16 C17 1.383(4) . ? C16 H16 0.9300 . ? C17 C18 1.378(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.392(3) . ? C19 C20 1.401(3) . ? C20 C21 1.399(3) . ? C20 H20 0.9300 . ? C21 C22 1.392(4) . ? C21 H21 0.9300 . ? C22 C23 1.385(3) . ? C22 H22 0.9300 . ? C23 C24 1.397(3) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.490(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 P1 C1 108.39(8) . . ? C13 P1 C7 110.53(9) . . ? C1 P1 C7 107.14(8) . . ? C13 P1 C19 109.86(8) . . ? C1 P1 C19 111.48(9) . . ? C7 P1 C19 109.41(8) . . ? C25 O3 H3 109.2 . . ? O1 N1 O2 109.3(3) . . ? C2 C1 C6 119.43(17) . . ? C2 C1 P1 119.57(14) . . ? C6 C1 P1 120.93(14) . . ? C3 C2 C1 120.33(18) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 120.16(19) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C5 C4 C3 119.83(19) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.73(19) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 119.49(18) . . ? C5 C6 H6 120.3 . . ? C1 C6 H6 120.3 . . ? C8 C7 C12 119.80(17) . . ? C8 C7 P1 120.04(14) . . ? C12 C7 P1 120.16(14) . . ? C9 C8 C7 120.08(18) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 119.73(19) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.36(19) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 120.22(19) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C7 119.74(18) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C14 C13 C18 120.22(18) . . ? C14 C13 P1 120.25(14) . . ? C18 C13 P1 119.17(15) . . ? C13 C14 C15 119.48(19) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 119.9(2) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.4(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 120.0(2) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 119.9(2) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C24 C19 C20 120.49(18) . . ? C24 C19 P1 120.50(15) . . ? C20 C19 P1 118.95(15) . . ? C21 C20 C19 119.29(19) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C22 C21 C20 120.2(2) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 120.1(2) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.5(2) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 119.5(2) . . ? C19 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? O3 C25 C26 112.44(19) . . ? O3 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? O3 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? data_1.py _database_code_depnum_ccdc_archive 'CCDC 915619' #TrackingRef 'web_deposit_cif_file_0_P.Thuery_1355410149.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H45 N7 O12 P2 Th' _chemical_formula_weight 1265.94 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' N N 0.0061 0.0033 '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' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/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 17.6259(4) _cell_length_b 13.8559(4) _cell_length_c 23.1389(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.6431(14) _cell_angle_gamma 90.00 _cell_volume 5288.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 191840 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 30.51 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 2.949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.632 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and five \w scans with 2\% steps (463 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 191840 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 30.51 _reflns_number_total 16114 _reflns_number_gt 12394 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0426P)^2^] 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 16114 _refine_ls_number_parameters 676 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.718 _refine_diff_density_min -1.178 _refine_diff_density_rms 0.132 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 Th Th 0.273356(5) 0.136579(7) 0.237577(4) 0.02576(4) Uani 1 1 d . . . P1 P 0.65742(4) 0.12833(5) 0.10519(3) 0.02941(15) Uani 1 1 d . . . P2 P 0.16561(4) 0.87933(5) 0.56358(3) 0.02651(14) Uani 1 1 d . . . O1 O 0.18870(14) 0.16258(17) 0.12194(9) 0.0443(5) Uani 1 1 d . . . O2 O 0.23051(12) 0.29111(15) 0.17183(10) 0.0414(5) Uani 1 1 d . . . O3 O 0.35932(13) 0.17195(17) 0.17135(10) 0.0442(5) Uani 1 1 d . . . O4 O 0.39734(12) 0.24735(15) 0.25600(10) 0.0402(5) Uani 1 1 d . . . O5 O 0.40916(12) 0.04519(15) 0.28056(9) 0.0403(5) Uani 1 1 d . . . O6 O 0.31389(13) -0.02031(15) 0.30090(9) 0.0395(5) Uani 1 1 d . . . O7 O 0.18131(12) 0.10306(18) 0.30040(9) 0.0435(5) Uani 1 1 d . . . O8 O 0.12717(11) 0.18854(17) 0.22170(9) 0.0436(5) Uani 1 1 d . . . O9 O 0.27812(15) -0.00692(16) 0.16904(9) 0.0470(5) Uani 1 1 d . . . O10 O 0.17171(13) 0.00170(17) 0.19073(10) 0.0499(6) Uani 1 1 d . . . O11 O 0.34882(13) 0.16832(18) 0.35205(9) 0.0442(5) Uani 1 1 d . . . O12 O 0.27391(13) 0.28262(16) 0.30521(10) 0.0445(5) Uani 1 1 d . . . N1 N 0.19044(16) 0.2540(2) 0.11983(12) 0.0482(7) Uani 1 1 d . . . N2 N 0.40888(17) 0.2332(2) 0.20574(15) 0.0515(7) Uani 1 1 d . . . N3 N 0.38829(16) -0.0242(2) 0.30660(12) 0.0459(6) Uani 1 1 d . . . N4 N 0.11728(17) 0.1446(2) 0.26656(13) 0.0487(7) Uani 1 1 d . . . N5 N 0.2076(2) -0.0409(2) 0.15887(13) 0.0573(8) Uani 1 1 d . . . N6 N 0.32481(18) 0.2530(2) 0.35613(13) 0.0535(7) Uani 1 1 d . . . C1 C 0.61854(15) 0.0736(2) 0.15909(11) 0.0292(6) Uani 1 1 d . . . C2 C 0.67053(16) 0.0302(2) 0.21229(13) 0.0338(6) Uani 1 1 d . . . H2 H 0.7263 0.0353 0.2224 0.041 Uiso 1 1 calc R . . C3 C 0.63940(17) -0.0207(2) 0.25026(14) 0.0376(6) Uani 1 1 d . . . H3 H 0.6742 -0.0503 0.2858 0.045 Uiso 1 1 calc R . . C4 C 0.55632(18) -0.0274(2) 0.23530(14) 0.0400(7) Uani 1 1 d . . . H4 H 0.5353 -0.0614 0.2609 0.048 Uiso 1 1 calc R . . C5 C 0.50459(17) 0.0163(2) 0.18267(14) 0.0407(7) Uani 1 1 d . . . H5 H 0.4488 0.0119 0.1730 0.049 Uiso 1 1 calc R . . C6 C 0.53491(16) 0.0661(2) 0.14454(13) 0.0394(7) Uani 1 1 d . . . H6 H 0.4997 0.0951 0.1089 0.047 Uiso 1 1 calc R . . C7 C 0.58895(16) 0.2207(2) 0.06254(13) 0.0348(6) Uani 1 1 d . . . C8 C 0.55723(19) 0.2865(2) 0.09332(15) 0.0466(8) Uani 1 1 d . . . H8 H 0.5704 0.2817 0.1358 0.056 Uiso 1 1 calc R . . C9 C 0.5065(2) 0.3587(2) 0.06104(19) 0.0576(10) Uani 1 1 d . . . H9 H 0.4855 0.4028 0.0818 0.069 Uiso 1 1 calc R . . C10 C 0.4864(2) 0.3662(2) -0.00242(19) 0.0565(10) Uani 1 1 d . . . H10 H 0.4516 0.4148 -0.0241 0.068 Uiso 1 1 calc R . . C11 C 0.51776(19) 0.3019(3) -0.03333(16) 0.0515(9) Uani 1 1 d . . . H11 H 0.5048 0.3079 -0.0758 0.062 Uiso 1 1 calc R . . C12 C 0.56845(18) 0.2285(2) -0.00155(14) 0.0441(7) Uani 1 1 d . . . H12 H 0.5889 0.1845 -0.0226 0.053 Uiso 1 1 calc R . . C13 C 0.66634(16) 0.0374(2) 0.05307(12) 0.0325(6) Uani 1 1 d . . . C14 C 0.62724(17) -0.0514(2) 0.04899(13) 0.0356(6) Uani 1 1 d . . . H14 H 0.5988 -0.0650 0.0751 0.043 Uiso 1 1 calc R . . C15 C 0.6308(2) -0.1189(2) 0.00619(14) 0.0429(7) Uani 1 1 d . . . H15 H 0.6057 -0.1785 0.0040 0.051 Uiso 1 1 calc R . . C16 C 0.67166(19) -0.0978(3) -0.03342(14) 0.0467(8) Uani 1 1 d . . . H16 H 0.6727 -0.1428 -0.0629 0.056 Uiso 1 1 calc R . . C17 C 0.7108(2) -0.0109(3) -0.02958(14) 0.0497(8) Uani 1 1 d . . . H17 H 0.7385 0.0025 -0.0562 0.060 Uiso 1 1 calc R . . C18 C 0.70884(19) 0.0570(2) 0.01408(14) 0.0431(7) Uani 1 1 d . . . H18 H 0.7359 0.1154 0.0172 0.052 Uiso 1 1 calc R . . C19 C 0.75612(16) 0.1795(2) 0.14389(12) 0.0322(6) Uani 1 1 d . . . C20 C 0.82357(18) 0.1186(2) 0.16249(14) 0.0387(7) Uani 1 1 d . . . H20 H 0.8175 0.0532 0.1529 0.046 Uiso 1 1 calc R . . C21 C 0.89925(19) 0.1558(2) 0.19523(15) 0.0450(8) Uani 1 1 d . . . H21 H 0.9443 0.1154 0.2071 0.054 Uiso 1 1 calc R . . C22 C 0.90831(19) 0.2526(3) 0.21036(14) 0.0475(8) Uani 1 1 d . . . H22 H 0.9593 0.2771 0.2328 0.057 Uiso 1 1 calc R . . C23 C 0.84167(19) 0.3130(2) 0.19213(15) 0.0454(8) Uani 1 1 d . . . H23 H 0.8480 0.3783 0.2021 0.055 Uiso 1 1 calc R . . C24 C 0.76548(18) 0.2767(2) 0.15904(13) 0.0371(6) Uani 1 1 d . . . H24 H 0.7207 0.3174 0.1470 0.045 Uiso 1 1 calc R . . C25 C 0.09884(15) 0.92745(19) 0.60020(12) 0.0286(5) Uani 1 1 d . . . C26 C 0.02024(17) 0.8924(2) 0.58542(14) 0.0372(6) Uani 1 1 d . . . H26 H -0.0004 0.8476 0.5538 0.045 Uiso 1 1 calc R . . C27 C -0.02707(18) 0.9254(2) 0.61850(15) 0.0446(7) Uani 1 1 d . . . H27 H -0.0795 0.9019 0.6090 0.054 Uiso 1 1 calc R . . C28 C 0.00250(19) 0.9918(2) 0.66476(14) 0.0461(8) Uani 1 1 d . . . H28 H -0.0296 1.0125 0.6868 0.055 Uiso 1 1 calc R . . C29 C 0.07966(19) 1.0282(2) 0.67879(13) 0.0413(7) Uani 1 1 d . . . H29 H 0.0988 1.0750 0.7093 0.050 Uiso 1 1 calc R . . C30 C 0.12880(17) 0.9954(2) 0.64771(12) 0.0341(6) Uani 1 1 d . . . H30 H 0.1815 1.0184 0.6583 0.041 Uiso 1 1 calc R . . C31 C 0.11323(16) 0.7870(2) 0.51050(12) 0.0310(6) Uani 1 1 d . . . C32 C 0.05256(17) 0.8146(2) 0.45524(13) 0.0387(7) Uani 1 1 d . . . H32 H 0.0416 0.8797 0.4462 0.046 Uiso 1 1 calc R . . C33 C 0.00906(18) 0.7450(2) 0.41423(14) 0.0445(7) Uani 1 1 d . . . H33 H -0.0314 0.7631 0.3776 0.053 Uiso 1 1 calc R . . C34 C 0.0256(2) 0.6489(2) 0.42759(16) 0.0466(8) Uani 1 1 d . . . H34 H -0.0043 0.6023 0.3999 0.056 Uiso 1 1 calc R . . C35 C 0.0858(2) 0.6205(2) 0.48133(15) 0.0427(7) Uani 1 1 d . . . H35 H 0.0967 0.5552 0.4895 0.051 Uiso 1 1 calc R . . C36 C 0.13073(17) 0.6897(2) 0.52381(13) 0.0351(6) Uani 1 1 d . . . H36 H 0.1715 0.6711 0.5602 0.042 Uiso 1 1 calc R . . C37 C 0.19942(15) 0.96749(19) 0.52114(12) 0.0286(5) Uani 1 1 d . . . C38 C 0.22233(17) 0.9381(2) 0.47220(13) 0.0364(6) Uani 1 1 d . . . H38 H 0.2152 0.8743 0.4590 0.044 Uiso 1 1 calc R . . C39 C 0.25569(19) 1.0041(2) 0.44324(13) 0.0413(7) Uani 1 1 d . . . H39 H 0.2702 0.9847 0.4101 0.050 Uiso 1 1 calc R . . C40 C 0.2676(2) 1.0979(2) 0.46291(14) 0.0454(7) Uani 1 1 d . . . H40 H 0.2915 1.1414 0.4439 0.054 Uiso 1 1 calc R . . C41 C 0.2440(3) 1.1277(2) 0.51105(17) 0.0543(10) Uani 1 1 d . . . H41 H 0.2513 1.1916 0.5241 0.065 Uiso 1 1 calc R . . C42 C 0.2096(2) 1.0629(2) 0.53973(14) 0.0439(7) Uani 1 1 d . . . H42 H 0.1931 1.0834 0.5717 0.053 Uiso 1 1 calc R . . C43 C 0.25285(16) 0.8312(2) 0.62336(12) 0.0293(5) Uani 1 1 d . . . C44 C 0.33050(18) 0.8444(2) 0.62142(14) 0.0417(7) Uani 1 1 d . . . H44 H 0.3379 0.8802 0.5898 0.050 Uiso 1 1 calc R . . C45 C 0.39660(18) 0.8035(3) 0.66715(14) 0.0493(8) Uani 1 1 d . . . H45 H 0.4487 0.8128 0.6667 0.059 Uiso 1 1 calc R . . C46 C 0.38485(19) 0.7491(2) 0.71321(14) 0.0453(8) Uani 1 1 d . . . H46 H 0.4291 0.7211 0.7435 0.054 Uiso 1 1 calc R . . C47 C 0.30843(18) 0.7358(2) 0.71480(13) 0.0387(7) Uani 1 1 d . . . H47 H 0.3014 0.6982 0.7458 0.046 Uiso 1 1 calc R . . C48 C 0.24206(17) 0.7777(2) 0.67086(12) 0.0337(6) Uani 1 1 d . . . H48 H 0.1906 0.7703 0.6729 0.040 Uiso 1 1 calc R . . N7 N 0.9441(2) 0.6046(3) 0.68327(15) 0.0640(8) Uani 1 1 d . . . C49 C 0.8744(2) 0.6397(2) 0.6520(2) 0.0588(10) Uani 1 1 d . . . H49 H 0.8386 0.6494 0.6730 0.071 Uiso 1 1 calc R . . C50 C 0.8488(3) 0.6633(3) 0.5937(2) 0.0793(14) Uani 1 1 d . . . H50 H 0.7962 0.6856 0.5741 0.095 Uiso 1 1 calc R . . C51 C 0.9007(5) 0.6545(3) 0.5620(2) 0.0978(17) Uani 1 1 d U . . H51 H 0.8850 0.6713 0.5206 0.117 Uiso 1 1 calc R . . C52 C 0.9794(4) 0.6188(3) 0.5950(3) 0.0856(15) Uani 1 1 d U . . H52 H 1.0183 0.6122 0.5766 0.103 Uiso 1 1 calc R . . C53 C 0.9950(2) 0.5951(3) 0.6545(2) 0.0769(13) Uani 1 1 d . . . H53 H 1.0460 0.5700 0.6767 0.092 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 Th 0.02590(6) 0.02758(6) 0.02302(5) 0.00059(4) 0.00764(4) -0.00148(4) P1 0.0301(4) 0.0295(4) 0.0267(3) -0.0002(3) 0.0077(3) 0.0007(3) P2 0.0263(3) 0.0275(3) 0.0243(3) 0.0001(3) 0.0073(3) -0.0018(3) O1 0.0518(13) 0.0464(13) 0.0285(10) 0.0065(10) 0.0063(10) 0.0005(11) O2 0.0433(12) 0.0335(11) 0.0468(12) 0.0112(10) 0.0150(10) 0.0056(9) O3 0.0497(13) 0.0491(13) 0.0433(12) 0.0058(11) 0.0281(11) 0.0081(11) O4 0.0335(11) 0.0365(11) 0.0531(13) -0.0059(10) 0.0184(10) -0.0085(9) O5 0.0357(11) 0.0426(12) 0.0446(12) 0.0087(10) 0.0167(9) 0.0079(9) O6 0.0444(12) 0.0352(11) 0.0365(11) 0.0069(9) 0.0114(9) -0.0019(9) O7 0.0346(11) 0.0636(14) 0.0346(11) 0.0093(11) 0.0150(9) -0.0013(11) O8 0.0290(10) 0.0601(15) 0.0408(12) 0.0089(11) 0.0110(9) 0.0035(10) O9 0.0684(16) 0.0358(12) 0.0353(11) -0.0028(9) 0.0162(11) 0.0024(11) O10 0.0472(13) 0.0459(13) 0.0458(13) -0.0026(11) 0.0032(11) -0.0186(11) O11 0.0434(12) 0.0557(14) 0.0284(10) -0.0081(10) 0.0062(9) -0.0037(11) O12 0.0477(13) 0.0415(12) 0.0505(13) -0.0117(10) 0.0250(11) 0.0008(10) N1 0.0442(15) 0.0541(18) 0.0432(16) 0.0166(14) 0.0116(13) 0.0023(13) N2 0.0503(17) 0.0414(16) 0.070(2) 0.0008(15) 0.0307(15) 0.0031(13) N3 0.0478(16) 0.0425(16) 0.0449(15) 0.0086(12) 0.0132(13) 0.0060(12) N4 0.0324(14) 0.070(2) 0.0451(16) 0.0061(14) 0.0155(12) 0.0006(13) N5 0.077(2) 0.0390(16) 0.0404(15) -0.0041(13) 0.0011(15) -0.0061(16) N6 0.0541(17) 0.062(2) 0.0439(16) -0.0161(15) 0.0166(14) -0.0050(15) C1 0.0312(13) 0.0302(14) 0.0266(12) -0.0033(11) 0.0105(11) 0.0033(11) C2 0.0287(13) 0.0339(15) 0.0370(15) 0.0034(12) 0.0095(11) 0.0004(11) C3 0.0364(15) 0.0355(16) 0.0385(15) 0.0058(13) 0.0102(13) 0.0007(12) C4 0.0462(17) 0.0369(17) 0.0435(17) 0.0067(13) 0.0239(14) 0.0048(13) C5 0.0271(14) 0.0507(19) 0.0467(17) 0.0023(15) 0.0161(13) 0.0055(13) C6 0.0280(14) 0.0530(19) 0.0350(15) 0.0061(14) 0.0085(12) 0.0074(13) C7 0.0304(14) 0.0340(15) 0.0334(14) 0.0036(12) 0.0033(11) -0.0011(12) C8 0.0494(18) 0.0397(18) 0.0392(16) -0.0047(14) 0.0014(14) 0.0095(15) C9 0.054(2) 0.040(2) 0.059(2) -0.0088(16) -0.0048(18) 0.0095(15) C10 0.0410(19) 0.047(2) 0.062(2) 0.0209(17) -0.0057(17) -0.0002(15) C11 0.0377(17) 0.064(2) 0.0482(19) 0.0202(18) 0.0096(15) 0.0009(16) C12 0.0356(16) 0.056(2) 0.0380(16) 0.0112(15) 0.0095(13) -0.0010(14) C13 0.0332(14) 0.0353(15) 0.0290(13) -0.0029(12) 0.0108(11) 0.0005(12) C14 0.0348(15) 0.0385(16) 0.0322(14) -0.0003(12) 0.0102(12) -0.0009(12) C15 0.0438(18) 0.0376(17) 0.0394(17) -0.0080(13) 0.0049(14) 0.0008(13) C16 0.0488(18) 0.056(2) 0.0308(15) -0.0100(15) 0.0087(14) 0.0115(17) C17 0.056(2) 0.065(2) 0.0335(16) -0.0001(16) 0.0232(15) 0.0067(18) C18 0.0502(18) 0.0449(18) 0.0391(16) -0.0015(14) 0.0220(14) -0.0060(15) C19 0.0329(14) 0.0342(15) 0.0285(13) 0.0028(12) 0.0095(11) -0.0014(12) C20 0.0342(16) 0.0367(16) 0.0425(17) 0.0003(13) 0.0100(13) -0.0006(12) C21 0.0328(16) 0.055(2) 0.0446(18) 0.0014(15) 0.0106(14) 0.0013(14) C22 0.0370(17) 0.061(2) 0.0411(17) -0.0072(16) 0.0098(14) -0.0126(15) C23 0.0443(18) 0.0432(19) 0.0484(18) -0.0082(15) 0.0158(15) -0.0132(15) C24 0.0395(16) 0.0364(16) 0.0371(15) -0.0006(13) 0.0154(13) -0.0014(13) C25 0.0304(13) 0.0278(14) 0.0272(12) 0.0040(11) 0.0097(11) 0.0019(11) C26 0.0314(15) 0.0375(16) 0.0412(16) -0.0005(13) 0.0107(12) -0.0030(12) C27 0.0336(15) 0.050(2) 0.0544(19) 0.0075(16) 0.0201(14) 0.0040(14) C28 0.0473(18) 0.054(2) 0.0440(17) 0.0110(16) 0.0244(15) 0.0149(16) C29 0.0485(18) 0.0449(18) 0.0327(15) -0.0004(13) 0.0171(14) 0.0032(14) C30 0.0335(14) 0.0385(16) 0.0295(13) -0.0010(12) 0.0101(12) -0.0012(12) C31 0.0328(14) 0.0317(15) 0.0292(13) -0.0018(11) 0.0118(11) -0.0036(11) C32 0.0374(15) 0.0376(17) 0.0350(15) 0.0006(13) 0.0051(12) -0.0009(13) C33 0.0386(16) 0.053(2) 0.0345(15) -0.0062(14) 0.0036(13) -0.0091(14) C34 0.0464(19) 0.053(2) 0.0419(18) -0.0208(15) 0.0167(15) -0.0193(15) C35 0.0462(18) 0.0340(16) 0.0496(19) -0.0100(14) 0.0190(15) -0.0066(13) C36 0.0362(15) 0.0348(16) 0.0348(14) -0.0046(12) 0.0133(12) -0.0022(12) C37 0.0275(13) 0.0284(14) 0.0276(13) 0.0039(11) 0.0070(10) -0.0007(11) C38 0.0404(16) 0.0352(16) 0.0360(15) 0.0009(12) 0.0166(13) -0.0015(12) C39 0.0474(18) 0.0500(19) 0.0316(15) 0.0045(14) 0.0204(13) 0.0013(14) C40 0.0508(19) 0.0463(19) 0.0444(17) 0.0109(16) 0.0234(15) -0.0049(16) C41 0.084(3) 0.0309(17) 0.056(2) -0.0056(14) 0.035(2) -0.0174(16) C42 0.065(2) 0.0352(17) 0.0409(16) -0.0060(13) 0.0295(16) -0.0091(15) C43 0.0299(13) 0.0289(13) 0.0278(13) 0.0004(11) 0.0085(11) 0.0012(11) C44 0.0333(16) 0.056(2) 0.0359(16) 0.0076(14) 0.0127(13) 0.0034(14) C45 0.0311(15) 0.073(2) 0.0419(17) 0.0087(17) 0.0103(13) 0.0075(16) C46 0.0385(17) 0.054(2) 0.0365(16) 0.0063(15) 0.0046(13) 0.0124(15) C47 0.0466(18) 0.0341(16) 0.0309(14) 0.0029(12) 0.0081(13) 0.0030(13) C48 0.0379(15) 0.0302(15) 0.0312(14) 0.0009(12) 0.0099(12) -0.0009(12) N7 0.065(2) 0.064(2) 0.064(2) -0.0019(17) 0.0240(17) 0.0197(17) C49 0.050(2) 0.050(2) 0.083(3) -0.0116(19) 0.031(2) -0.0037(16) C50 0.076(3) 0.054(2) 0.078(3) -0.008(2) -0.012(3) 0.004(2) C51 0.168(4) 0.061(3) 0.056(2) -0.003(2) 0.030(3) -0.031(3) C52 0.103(3) 0.080(3) 0.107(3) -0.040(2) 0.079(3) -0.040(2) C53 0.043(2) 0.076(3) 0.105(4) -0.035(3) 0.018(2) 0.005(2) _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 Th O11 2.548(2) . ? Th O10 2.551(2) . ? Th O3 2.5536(19) . ? Th O12 2.556(2) . ? Th O9 2.563(2) . ? Th O7 2.5736(19) . ? Th O8 2.5738(19) . ? Th O6 2.578(2) . ? Th O5 2.5775(19) . ? Th O4 2.5799(19) . ? Th O2 2.581(2) . ? Th O1 2.588(2) . ? P1 C1 1.789(3) . ? P1 C13 1.789(3) . ? P1 C7 1.797(3) . ? P1 C19 1.798(3) . ? P2 C31 1.789(3) . ? P2 C43 1.795(3) . ? P2 C37 1.796(3) . ? P2 C25 1.803(3) . ? O1 N1 1.268(3) . ? O2 N1 1.270(3) . ? O3 N2 1.276(4) . ? O4 N2 1.265(3) . ? O5 N3 1.257(3) . ? O6 N3 1.272(3) . ? O7 N4 1.263(3) . ? O8 N4 1.268(3) . ? O9 N5 1.272(4) . ? O10 N5 1.273(4) . ? O11 N6 1.262(4) . ? O12 N6 1.271(3) . ? C1 C2 1.386(4) . ? C1 C6 1.395(4) . ? C2 C3 1.382(4) . ? C2 H2 0.9300 . ? C3 C4 1.384(4) . ? C3 H3 0.9300 . ? C4 C5 1.377(4) . ? C4 H4 0.9300 . ? C5 C6 1.369(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.390(4) . ? C7 C12 1.401(4) . ? C8 C9 1.374(4) . ? C8 H8 0.9300 . ? C9 C10 1.388(6) . ? C9 H9 0.9300 . ? C10 C11 1.374(5) . ? C10 H10 0.9300 . ? C11 C12 1.382(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.388(4) . ? C13 C14 1.397(4) . ? C14 C15 1.379(4) . ? C14 H14 0.9300 . ? C15 C16 1.382(4) . ? C15 H15 0.9300 . ? C16 C17 1.375(5) . ? C16 H16 0.9300 . ? C17 C18 1.389(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.386(4) . ? C19 C20 1.397(4) . ? C20 C21 1.381(4) . ? C20 H20 0.9300 . ? C21 C22 1.381(5) . ? C21 H21 0.9300 . ? C22 C23 1.382(5) . ? C22 H22 0.9300 . ? C23 C24 1.385(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.392(4) . ? C25 C30 1.402(4) . ? C26 C27 1.393(4) . ? C26 H26 0.9300 . ? C27 C28 1.368(5) . ? C27 H27 0.9300 . ? C28 C29 1.377(4) . ? C28 H28 0.9300 . ? C29 C30 1.383(4) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.392(4) . ? C31 C32 1.400(4) . ? C32 C33 1.381(4) . ? C32 H32 0.9300 . ? C33 C34 1.375(5) . ? C33 H33 0.9300 . ? C34 C35 1.377(5) . ? C34 H34 0.9300 . ? C35 C36 1.402(4) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C42 1.382(4) . ? C37 C38 1.390(4) . ? C38 C39 1.382(4) . ? C38 H38 0.9300 . ? C39 C40 1.367(5) . ? C39 H39 0.9300 . ? C40 C41 1.383(5) . ? C40 H40 0.9300 . ? C41 C42 1.378(4) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C48 1.393(4) . ? C43 C44 1.397(4) . ? C44 C45 1.389(4) . ? C44 H44 0.9300 . ? C45 C46 1.380(4) . ? C45 H45 0.9300 . ? C46 C47 1.373(4) . ? C46 H46 0.9300 . ? C47 C48 1.378(4) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? N7 C49 1.282(5) . ? N7 C53 1.298(5) . ? C49 C50 1.305(6) . ? C49 H49 0.9300 . ? C50 C51 1.363(7) . ? C50 H50 0.9300 . ? C51 C52 1.417(8) . ? C51 H51 0.9300 . ? C52 C53 1.347(7) . ? C52 H52 0.9300 . ? C53 H53 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 O11 Th O10 126.81(7) . . ? O11 Th O3 112.82(7) . . ? O10 Th O3 111.22(8) . . ? O11 Th O12 48.63(8) . . ? O10 Th O12 133.68(7) . . ? O3 Th O12 109.91(7) . . ? O11 Th O9 131.15(8) . . ? O10 Th O9 48.71(8) . . ? O3 Th O9 67.78(8) . . ? O12 Th O9 177.57(7) . . ? O11 Th O7 69.27(7) . . ? O10 Th O7 67.65(8) . . ? O3 Th O7 177.55(6) . . ? O12 Th O7 70.37(7) . . ? O9 Th O7 111.97(8) . . ? O11 Th O8 103.27(7) . . ? O10 Th O8 68.07(8) . . ? O3 Th O8 129.53(7) . . ? O12 Th O8 69.73(7) . . ? O9 Th O8 112.22(7) . . ? O7 Th O8 48.12(7) . . ? O11 Th O6 67.43(7) . . ? O10 Th O6 68.66(7) . . ? O3 Th O6 113.50(7) . . ? O12 Th O6 112.28(7) . . ? O9 Th O6 68.56(7) . . ? O7 Th O6 68.31(7) . . ? O8 Th O6 112.33(7) . . ? O11 Th O5 67.06(7) . . ? O10 Th O5 102.80(7) . . ? O3 Th O5 70.07(7) . . ? O12 Th O5 110.50(7) . . ? O9 Th O5 68.23(7) . . ? O7 Th O5 112.21(7) . . ? O8 Th O5 159.93(7) . . ? O6 Th O5 48.15(6) . . ? O11 Th O4 67.93(7) . . ? O10 Th O4 158.92(7) . . ? O3 Th O4 48.53(7) . . ? O12 Th O4 66.90(6) . . ? O9 Th O4 110.68(7) . . ? O7 Th O4 132.84(7) . . ? O8 Th O4 127.17(7) . . ? O6 Th O4 111.03(7) . . ? O5 Th O4 67.12(7) . . ? O11 Th O2 113.99(8) . . ? O10 Th O2 109.97(7) . . ? O3 Th O2 66.37(7) . . ? O12 Th O2 68.98(7) . . ? O9 Th O2 110.21(7) . . ? O7 Th O2 111.78(7) . . ? O8 Th O2 67.27(7) . . ? O6 Th O2 178.55(7) . . ? O5 Th O2 132.38(6) . . ? O4 Th O2 70.04(7) . . ? O11 Th O1 161.77(9) . . ? O10 Th O1 66.43(7) . . ? O3 Th O1 66.47(7) . . ? O12 Th O1 113.52(7) . . ? O9 Th O1 66.49(7) . . ? O7 Th O1 111.13(7) . . ? O8 Th O1 68.30(7) . . ? O6 Th O1 130.40(7) . . ? O5 Th O1 125.85(7) . . ? O4 Th O1 103.54(7) . . ? O2 Th O1 48.15(7) . . ? C1 P1 C13 108.52(13) . . ? C1 P1 C7 109.66(13) . . ? C13 P1 C7 109.46(13) . . ? C1 P1 C19 111.17(12) . . ? C13 P1 C19 108.30(13) . . ? C7 P1 C19 109.70(13) . . ? C31 P2 C43 110.95(13) . . ? C31 P2 C37 107.55(12) . . ? C43 P2 C37 108.36(12) . . ? C31 P2 C25 108.84(12) . . ? C43 P2 C25 107.41(12) . . ? C37 P2 C25 113.76(13) . . ? N1 O1 Th 99.55(17) . . ? N1 O2 Th 99.89(17) . . ? N2 O3 Th 100.03(17) . . ? N2 O4 Th 99.06(17) . . ? N3 O5 Th 99.91(16) . . ? N3 O6 Th 99.43(16) . . ? N4 O7 Th 99.85(16) . . ? N4 O8 Th 99.70(16) . . ? N5 O9 Th 99.13(18) . . ? N5 O10 Th 99.69(18) . . ? N6 O11 Th 99.92(18) . . ? N6 O12 Th 99.25(18) . . ? O1 N1 O2 112.4(2) . . ? O4 N2 O3 112.3(2) . . ? O5 N3 O6 112.5(2) . . ? O7 N4 O8 112.1(2) . . ? O9 N5 O10 111.9(3) . . ? O11 N6 O12 112.1(2) . . ? C2 C1 C6 119.6(3) . . ? C2 C1 P1 120.5(2) . . ? C6 C1 P1 119.7(2) . . ? C3 C2 C1 120.0(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119.8(3) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.3(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C6 C5 C4 120.3(3) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 120.1(3) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C8 C7 C12 119.4(3) . . ? C8 C7 P1 120.0(2) . . ? C12 C7 P1 120.6(2) . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.3(4) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 120.2(3) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.2(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 119.8(3) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C18 C13 C14 119.7(3) . . ? C18 C13 P1 119.7(2) . . ? C14 C13 P1 120.5(2) . . ? C15 C14 C13 119.9(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.0(3) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.6(3) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.0(3) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C13 C18 C17 119.8(3) . . ? C13 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C24 C19 C20 119.8(3) . . ? C24 C19 P1 121.1(2) . . ? C20 C19 P1 118.9(2) . . ? C21 C20 C19 119.8(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 120.3(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 120.1(3) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 120.2(3) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C19 119.9(3) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C26 C25 C30 119.6(2) . . ? C26 C25 P2 120.9(2) . . ? C30 C25 P2 119.3(2) . . ? C27 C26 C25 119.2(3) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C28 C27 C26 120.9(3) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 120.2(3) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C30 120.3(3) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C25 119.8(3) . . ? C29 C30 H30 120.1 . . ? C25 C30 H30 120.1 . . ? C36 C31 C32 120.3(3) . . ? C36 C31 P2 121.3(2) . . ? C32 C31 P2 118.3(2) . . ? C33 C32 C31 119.8(3) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C34 C33 C32 120.0(3) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 121.0(3) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C36 120.2(3) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C31 C36 C35 118.7(3) . . ? C31 C36 H36 120.6 . . ? C35 C36 H36 120.6 . . ? C42 C37 C38 119.4(3) . . ? C42 C37 P2 120.8(2) . . ? C38 C37 P2 119.6(2) . . ? C39 C38 C37 119.8(3) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C40 C39 C38 120.6(3) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 119.9(3) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C42 C41 C40 120.1(3) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C37 120.3(3) . . ? C41 C42 H42 119.9 . . ? C37 C42 H42 119.9 . . ? C48 C43 C44 120.2(3) . . ? C48 C43 P2 119.2(2) . . ? C44 C43 P2 120.6(2) . . ? C45 C44 C43 119.4(3) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C46 C45 C44 119.8(3) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C47 C46 C45 120.6(3) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C46 C47 C48 120.6(3) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C47 C48 C43 119.3(3) . . ? C47 C48 H48 120.3 . . ? C43 C48 H48 120.3 . . ? C49 N7 C53 116.6(4) . . ? N7 C49 C50 126.2(4) . . ? N7 C49 H49 116.9 . . ? C50 C49 H49 116.9 . . ? C49 C50 C51 118.7(5) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? C50 C51 C52 117.2(5) . . ? C50 C51 H51 121.4 . . ? C52 C51 H51 121.4 . . ? C53 C52 C51 116.4(4) . . ? C53 C52 H52 121.8 . . ? C51 C52 H52 121.8 . . ? N7 C53 C52 124.8(4) . . ? N7 C53 H53 117.6 . . ? C52 C53 H53 117.6 . . ? data_1~2~.MeCN.Et~2~O _database_code_depnum_ccdc_archive 'CCDC 915620' #TrackingRef 'web_deposit_cif_file_0_P.Thuery_1355410149.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H46.50 N6.50 O12.50 P2 Th' _chemical_formula_weight 1244.43 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' N N 0.0061 0.0033 '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' Th Th -7.2400 8.8979 '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 11.2048(3) _cell_length_b 21.6990(6) _cell_length_c 22.4861(4) _cell_angle_alpha 78.0104(15) _cell_angle_beta 81.8288(15) _cell_angle_gamma 75.3495(13) _cell_volume 5150.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 297726 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 30.51 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2472 _exptl_absorpt_coefficient_mu 3.026 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.502 _exptl_absorpt_correction_T_max 0.635 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and twelve \w scans with 2\% steps (736 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 297726 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 30.51 _reflns_number_total 31356 _reflns_number_gt 22646 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints for some bond lengths and displacement parameters in the solvent molecules. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom (1.5 for CH~3~). 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^)+(0.0400P)^2^+0.3884P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 31356 _refine_ls_number_parameters 1318 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.467 _refine_diff_density_min -2.038 _refine_diff_density_rms 0.089 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 0.438474(10) 0.152800(5) 0.726455(5) 0.03696(4) Uani 1 1 d . . . Th2 Th 0.921454(9) 0.658477(5) 0.744424(5) 0.03296(3) Uani 1 1 d . . . P1 P 0.62098(7) 0.38774(4) 0.91831(4) 0.03543(16) Uani 1 1 d . . . P2 P 0.12853(8) 0.88652(4) 0.93724(4) 0.03559(16) Uani 1 1 d . . . P3 P 0.20911(7) 0.89670(4) 0.53987(3) 0.03200(15) Uani 1 1 d . . . P4 P 0.72370(7) 0.44307(4) 0.58371(4) 0.03599(17) Uani 1 1 d . . . O1 O 0.4276(3) 0.04935(15) 0.69213(14) 0.0737(9) Uani 1 1 d . . . O2 O 0.4333(3) 0.12943(17) 0.61967(12) 0.0735(8) Uani 1 1 d . . . O3 O 0.2190(3) 0.15418(16) 0.70517(14) 0.0683(8) Uani 1 1 d . . . O4 O 0.2242(3) 0.21007(14) 0.77041(13) 0.0638(7) Uani 1 1 d . . . O5 O 0.4405(3) 0.17973(16) 0.83270(12) 0.0680(8) Uani 1 1 d . . . O6 O 0.4476(3) 0.25725(14) 0.76187(16) 0.0713(8) Uani 1 1 d . . . O7 O 0.6594(2) 0.14826(14) 0.74880(13) 0.0592(7) Uani 1 1 d . . . O8 O 0.6521(2) 0.09145(13) 0.68533(12) 0.0585(7) Uani 1 1 d . . . O9 O 0.5345(3) 0.05182(14) 0.80297(13) 0.0658(7) Uani 1 1 d . . . O10 O 0.3421(3) 0.07736(14) 0.81229(12) 0.0637(7) Uani 1 1 d . . . O11 O 0.3488(2) 0.25582(14) 0.65225(13) 0.0671(8) Uani 1 1 d . . . O12 O 0.5439(2) 0.22794(13) 0.64403(13) 0.0666(8) Uani 1 1 d . . . O13 O 1.0733(3) 0.58619(12) 0.67641(12) 0.0615(7) Uani 1 1 d . . . O14 O 0.8972(3) 0.56825(13) 0.69318(13) 0.0600(7) Uani 1 1 d . . . O15 O 1.0207(3) 0.54512(13) 0.80344(13) 0.0639(7) Uani 1 1 d . . . O16 O 0.8270(3) 0.57263(13) 0.82024(12) 0.0586(7) Uani 1 1 d . . . O17 O 0.9391(2) 0.66120(14) 0.85640(11) 0.0592(7) Uani 1 1 d . . . O18 O 0.9427(2) 0.74889(12) 0.79737(13) 0.0528(6) Uani 1 1 d . . . O19 O 0.8304(2) 0.77278(11) 0.68585(11) 0.0483(6) Uani 1 1 d . . . O20 O 0.8889(2) 0.70189(12) 0.63089(10) 0.0486(6) Uani 1 1 d . . . O21 O 1.0948(2) 0.71267(11) 0.68587(11) 0.0454(5) Uani 1 1 d . . . O22 O 1.1494(2) 0.64424(13) 0.76303(12) 0.0525(6) Uani 1 1 d . . . O23 O 0.6991(2) 0.66784(13) 0.72317(12) 0.0529(6) Uani 1 1 d . . . O24 O 0.7130(2) 0.70939(13) 0.79792(12) 0.0582(7) Uani 1 1 d . . . N1 N 0.4272(4) 0.0701(2) 0.63502(19) 0.0899(13) Uani 1 1 d . . . N2 N 0.1603(3) 0.18970(16) 0.74426(17) 0.0573(8) Uani 1 1 d . . . N3 N 0.4377(3) 0.23934(15) 0.81539(15) 0.0502(7) Uani 1 1 d . . . N4 N 0.7204(3) 0.10955(17) 0.71488(17) 0.0648(9) Uani 1 1 d . . . N5 N 0.4319(3) 0.04409(19) 0.83187(14) 0.0583(8) Uani 1 1 d . . . N6 N 0.4494(3) 0.26851(19) 0.62426(18) 0.0789(12) Uani 1 1 d . . . N7 N 1.0065(3) 0.55686(13) 0.66705(13) 0.0445(6) Uani 1 1 d . . . N8 N 0.9214(4) 0.5311(2) 0.83148(16) 0.0707(10) Uani 1 1 d . . . N9 N 0.9421(3) 0.72105(16) 0.84881(15) 0.0532(8) Uani 1 1 d . . . N10 N 0.8473(3) 0.76007(14) 0.63375(13) 0.0436(6) Uani 1 1 d . . . N11 N 1.1804(3) 0.68086(13) 0.71594(12) 0.0423(6) Uani 1 1 d . . . N12 N 0.6427(3) 0.69657(18) 0.76648(15) 0.0607(8) Uani 1 1 d . . . N13 N 0.1408(6) 0.4014(3) 0.9436(3) 0.143(2) Uani 1 1 d . . . C1 C 0.7148(3) 0.40769(15) 0.96636(14) 0.0369(6) Uani 1 1 d . . . C2 C 0.7498(3) 0.36332(16) 1.01899(15) 0.0470(8) Uani 1 1 d . . . H2 H 0.7217 0.3253 1.0294 0.056 Uiso 1 1 calc R . . C3 C 0.8266(3) 0.37631(18) 1.05570(16) 0.0517(9) Uani 1 1 d . . . H3 H 0.8499 0.3469 1.0908 0.062 Uiso 1 1 calc R . . C4 C 0.8687(3) 0.43273(19) 1.04036(17) 0.0533(9) Uani 1 1 d . . . H4 H 0.9211 0.4409 1.0648 0.064 Uiso 1 1 calc R . . C5 C 0.8329(4) 0.47676(19) 0.98884(17) 0.0543(9) Uani 1 1 d . . . H5 H 0.8604 0.5149 0.9791 0.065 Uiso 1 1 calc R . . C6 C 0.7565(3) 0.46498(16) 0.95152(15) 0.0442(7) Uani 1 1 d . . . H6 H 0.7331 0.4950 0.9167 0.053 Uiso 1 1 calc R . . C7 C 0.5469(3) 0.45795(14) 0.86756(14) 0.0380(7) Uani 1 1 d . . . C8 C 0.4189(3) 0.48257(18) 0.87463(16) 0.0526(9) Uani 1 1 d . . . H8 H 0.3707 0.4637 0.9070 0.063 Uiso 1 1 calc R . . C9 C 0.3641(4) 0.5355(2) 0.83295(17) 0.0620(11) Uani 1 1 d . . . H9 H 0.2787 0.5515 0.8366 0.074 Uiso 1 1 calc R . . C10 C 0.4374(4) 0.56435(17) 0.78594(16) 0.0536(9) Uani 1 1 d . . . H10 H 0.4006 0.6002 0.7585 0.064 Uiso 1 1 calc R . . C11 C 0.5653(4) 0.54048(16) 0.77910(16) 0.0507(8) Uani 1 1 d . . . H11 H 0.6139 0.5605 0.7478 0.061 Uiso 1 1 calc R . . C12 C 0.6194(3) 0.48650(16) 0.81958(15) 0.0458(8) Uani 1 1 d . . . H12 H 0.7043 0.4693 0.8146 0.055 Uiso 1 1 calc R . . C13 C 0.7161(3) 0.33273(14) 0.87141(14) 0.0367(6) Uani 1 1 d . . . C14 C 0.8399(3) 0.30482(16) 0.88052(15) 0.0443(7) Uani 1 1 d . . . H14 H 0.8757 0.3143 0.9114 0.053 Uiso 1 1 calc R . . C15 C 0.9092(3) 0.26274(16) 0.84300(17) 0.0510(9) Uani 1 1 d . . . H15 H 0.9922 0.2441 0.8485 0.061 Uiso 1 1 calc R . . C16 C 0.8556(3) 0.24853(16) 0.79769(17) 0.0506(9) Uani 1 1 d . . . H16 H 0.9030 0.2203 0.7727 0.061 Uiso 1 1 calc R . . C17 C 0.7342(3) 0.27505(16) 0.78873(16) 0.0468(8) Uani 1 1 d . . . H17 H 0.6987 0.2642 0.7585 0.056 Uiso 1 1 calc R . . C18 C 0.6635(3) 0.31845(16) 0.82500(15) 0.0449(8) Uani 1 1 d . . . H18 H 0.5814 0.3379 0.8182 0.054 Uiso 1 1 calc R . . C19 C 0.5083(3) 0.35012(15) 0.96696(14) 0.0385(7) Uani 1 1 d . . . C20 C 0.4859(3) 0.29297(17) 0.95822(15) 0.0460(8) Uani 1 1 d . . . H20 H 0.5290 0.2734 0.9259 0.055 Uiso 1 1 calc R . . C21 C 0.3995(4) 0.2647(2) 0.99747(17) 0.0556(9) Uani 1 1 d . . . H21 H 0.3853 0.2259 0.9919 0.067 Uiso 1 1 calc R . . C22 C 0.3342(3) 0.2947(2) 1.04508(17) 0.0572(10) Uani 1 1 d . . . H22 H 0.2766 0.2757 1.0716 0.069 Uiso 1 1 calc R . . C23 C 0.3538(3) 0.35211(19) 1.05349(16) 0.0517(9) Uani 1 1 d . . . H23 H 0.3082 0.3721 1.0850 0.062 Uiso 1 1 calc R . . C24 C 0.4411(3) 0.38026(17) 1.01537(15) 0.0449(7) Uani 1 1 d . . . H24 H 0.4554 0.4187 1.0215 0.054 Uiso 1 1 calc R . . C25 C 0.0581(3) 0.95786(15) 0.88682(15) 0.0442(8) Uani 1 1 d . . . C26 C 0.1337(4) 0.9866(2) 0.8405(2) 0.0680(12) Uani 1 1 d . . . H26 H 0.2189 0.9698 0.8374 0.082 Uiso 1 1 calc R . . C27 C 0.0828(6) 1.0401(2) 0.7991(2) 0.0876(17) Uani 1 1 d . . . H27 H 0.1331 1.0600 0.7686 0.105 Uiso 1 1 calc R . . C28 C -0.0464(6) 1.06385(19) 0.8039(2) 0.0819(17) Uani 1 1 d . . . H28 H -0.0816 1.1006 0.7771 0.098 Uiso 1 1 calc R . . C29 C -0.1196(5) 1.0341(2) 0.8468(2) 0.0805(16) Uani 1 1 d . . . H29 H -0.2051 1.0491 0.8478 0.097 Uiso 1 1 calc R . . C30 C -0.0691(4) 0.9815(2) 0.88929(17) 0.0619(10) Uani 1 1 d . . . H30 H -0.1206 0.9620 0.9195 0.074 Uiso 1 1 calc R . . C31 C 0.2316(3) 0.90277(16) 0.98318(14) 0.0412(7) Uani 1 1 d . . . C32 C 0.2814(4) 0.9570(2) 0.96550(19) 0.0710(13) Uani 1 1 d . . . H32 H 0.2597 0.9866 0.9303 0.085 Uiso 1 1 calc R . . C33 C 0.3640(5) 0.9659(3) 1.0014(2) 0.0976(19) Uani 1 1 d . . . H33 H 0.3968 1.0024 0.9906 0.117 Uiso 1 1 calc R . . C34 C 0.3985(4) 0.9215(2) 1.05298(19) 0.0751(13) Uani 1 1 d . . . H34 H 0.4579 0.9270 1.0752 0.090 Uiso 1 1 calc R . . C35 C 0.3460(4) 0.86983(18) 1.07158(16) 0.0522(9) Uani 1 1 d . . . H35 H 0.3673 0.8406 1.1071 0.063 Uiso 1 1 calc R . . C36 C 0.2606(4) 0.86100(17) 1.03718(16) 0.0495(8) Uani 1 1 d . . . H36 H 0.2224 0.8266 1.0506 0.059 Uiso 1 1 calc R . . C37 C 0.2151(3) 0.83051(14) 0.88983(13) 0.0359(6) Uani 1 1 d . . . C38 C 0.3362(3) 0.79893(16) 0.89707(15) 0.0451(7) Uani 1 1 d . . . H38 H 0.3761 0.8061 0.9277 0.054 Uiso 1 1 calc R . . C39 C 0.3994(3) 0.75621(18) 0.85874(16) 0.0546(9) Uani 1 1 d . . . H39 H 0.4819 0.7354 0.8631 0.066 Uiso 1 1 calc R . . C40 C 0.3392(4) 0.74503(18) 0.81445(17) 0.0540(9) Uani 1 1 d . . . H40 H 0.3806 0.7153 0.7898 0.065 Uiso 1 1 calc R . . C41 C 0.2182(4) 0.77718(19) 0.80591(17) 0.0552(10) Uani 1 1 d . . . H41 H 0.1793 0.7697 0.7751 0.066 Uiso 1 1 calc R . . C42 C 0.1548(3) 0.82060(18) 0.84312(16) 0.0476(8) Uani 1 1 d . . . H42 H 0.0735 0.8429 0.8373 0.057 Uiso 1 1 calc R . . C43 C 0.0121(3) 0.85303(15) 0.98727(14) 0.0400(7) Uani 1 1 d . . . C44 C -0.0173(3) 0.79685(17) 0.97901(16) 0.0461(8) Uani 1 1 d . . . H44 H 0.0251 0.7753 0.9478 0.055 Uiso 1 1 calc R . . C45 C -0.1096(4) 0.7734(2) 1.01746(18) 0.0585(10) Uani 1 1 d . . . H45 H -0.1295 0.7359 1.0122 0.070 Uiso 1 1 calc R . . C46 C -0.1723(4) 0.8054(2) 1.06353(17) 0.0604(10) Uani 1 1 d . . . H46 H -0.2341 0.7891 1.0893 0.072 Uiso 1 1 calc R . . C47 C -0.1450(4) 0.8609(2) 1.07205(17) 0.0589(10) Uani 1 1 d . . . H47 H -0.1888 0.8823 1.1031 0.071 Uiso 1 1 calc R . . C48 C -0.0518(3) 0.88511(17) 1.03415(16) 0.0493(8) Uani 1 1 d . . . H48 H -0.0321 0.9224 1.0400 0.059 Uiso 1 1 calc R . . C49 C 0.1061(3) 0.91830(14) 0.60459(14) 0.0353(6) Uani 1 1 d . . . C50 C 0.0749(3) 0.98185(15) 0.61555(14) 0.0390(7) Uani 1 1 d . . . H50 H 0.1062 1.0139 0.5884 0.047 Uiso 1 1 calc R . . C51 C -0.0020(3) 0.99698(17) 0.66645(15) 0.0479(8) Uani 1 1 d . . . H51 H -0.0220 1.0392 0.6737 0.057 Uiso 1 1 calc R . . C52 C -0.0499(3) 0.94972(18) 0.70709(15) 0.0496(8) Uani 1 1 d . . . H52 H -0.1014 0.9603 0.7415 0.059 Uiso 1 1 calc R . . C53 C -0.0214(3) 0.88730(17) 0.69651(15) 0.0454(8) Uani 1 1 d . . . H53 H -0.0532 0.8557 0.7240 0.055 Uiso 1 1 calc R . . C54 C 0.0550(3) 0.87106(15) 0.64484(14) 0.0406(7) Uani 1 1 d . . . H54 H 0.0720 0.8291 0.6371 0.049 Uiso 1 1 calc R . . C55 C 0.2567(3) 0.96674(13) 0.49527(13) 0.0332(6) Uani 1 1 d . . . C56 C 0.2347(3) 0.98824(15) 0.43466(14) 0.0393(7) Uani 1 1 d . . . H56 H 0.1934 0.9665 0.4158 0.047 Uiso 1 1 calc R . . C57 C 0.2743(3) 1.04239(16) 0.40191(15) 0.0459(8) Uani 1 1 d . . . H57 H 0.2609 1.0566 0.3609 0.055 Uiso 1 1 calc R . . C58 C 0.3341(3) 1.07536(16) 0.43068(16) 0.0441(7) Uani 1 1 d . . . H58 H 0.3583 1.1124 0.4092 0.053 Uiso 1 1 calc R . . C59 C 0.3576(3) 1.05338(15) 0.49066(16) 0.0430(7) Uani 1 1 d . . . H59 H 0.3983 1.0754 0.5094 0.052 Uiso 1 1 calc R . . C60 C 0.3212(3) 0.99862(14) 0.52337(14) 0.0387(7) Uani 1 1 d . . . H60 H 0.3394 0.9831 0.5636 0.046 Uiso 1 1 calc R . . C61 C 0.3487(3) 0.83978(14) 0.56433(14) 0.0335(6) Uani 1 1 d . . . C62 C 0.4511(3) 0.83041(14) 0.52099(14) 0.0364(6) Uani 1 1 d . . . H62 H 0.4472 0.8540 0.4815 0.044 Uiso 1 1 calc R . . C63 C 0.5586(3) 0.78552(15) 0.53755(16) 0.0426(7) Uani 1 1 d . . . H63 H 0.6271 0.7791 0.5090 0.051 Uiso 1 1 calc R . . C64 C 0.5648(3) 0.75033(17) 0.59597(17) 0.0497(8) Uani 1 1 d . . . H64 H 0.6369 0.7198 0.6064 0.060 Uiso 1 1 calc R . . C65 C 0.4651(3) 0.76019(19) 0.63876(18) 0.0577(10) Uani 1 1 d . . . H65 H 0.4706 0.7367 0.6783 0.069 Uiso 1 1 calc R . . C66 C 0.3561(3) 0.80482(17) 0.62376(15) 0.0474(8) Uani 1 1 d . . . H66 H 0.2887 0.8113 0.6530 0.057 Uiso 1 1 calc R . . C67 C 0.1327(3) 0.86240(13) 0.49380(13) 0.0335(6) Uani 1 1 d . . . C68 C 0.2012(3) 0.83218(15) 0.44665(14) 0.0414(7) Uani 1 1 d . . . H68 H 0.2864 0.8282 0.4401 0.050 Uiso 1 1 calc R . . C69 C 0.1423(3) 0.80813(16) 0.40953(15) 0.0468(8) Uani 1 1 d . . . H69 H 0.1879 0.7877 0.3782 0.056 Uiso 1 1 calc R . . C70 C 0.0163(3) 0.81450(16) 0.41910(16) 0.0483(8) Uani 1 1 d . . . H70 H -0.0231 0.7989 0.3937 0.058 Uiso 1 1 calc R . . C71 C -0.0523(3) 0.84352(16) 0.46554(18) 0.0512(9) Uani 1 1 d . . . H71 H -0.1374 0.8470 0.4717 0.061 Uiso 1 1 calc R . . C72 C 0.0056(3) 0.86769(15) 0.50338(16) 0.0429(7) Uani 1 1 d . . . H72 H -0.0407 0.8873 0.5350 0.051 Uiso 1 1 calc R . . C73 C 0.7240(3) 0.39037(14) 0.53145(14) 0.0376(7) Uani 1 1 d . . . C74 C 0.8256(3) 0.37734(16) 0.48963(15) 0.0450(8) Uani 1 1 d . . . H74 H 0.8922 0.3961 0.4884 0.054 Uiso 1 1 calc R . . C75 C 0.8285(4) 0.33646(16) 0.44957(15) 0.0528(9) Uani 1 1 d . . . H75 H 0.8982 0.3263 0.4224 0.063 Uiso 1 1 calc R . . C76 C 0.7293(4) 0.31114(17) 0.45000(16) 0.0589(10) Uani 1 1 d . . . H76 H 0.7312 0.2842 0.4225 0.071 Uiso 1 1 calc R . . C77 C 0.6255(4) 0.32467(17) 0.49059(17) 0.0548(9) Uani 1 1 d . . . H77 H 0.5576 0.3076 0.4899 0.066 Uiso 1 1 calc R . . C78 C 0.6234(3) 0.36399(15) 0.53241(15) 0.0444(8) Uani 1 1 d . . . H78 H 0.5551 0.3725 0.5608 0.053 Uiso 1 1 calc R . . C79 C 0.8405(3) 0.40560(14) 0.63542(14) 0.0390(7) Uani 1 1 d . . . C80 C 0.9368(3) 0.35336(16) 0.62285(16) 0.0486(8) Uani 1 1 d . . . H80 H 0.9382 0.3351 0.5888 0.058 Uiso 1 1 calc R . . C81 C 1.0297(3) 0.32924(17) 0.66142(16) 0.0522(9) Uani 1 1 d . . . H81 H 1.0940 0.2946 0.6531 0.063 Uiso 1 1 calc R . . C82 C 1.0281(3) 0.35576(17) 0.71187(17) 0.0533(9) Uani 1 1 d . . . H82 H 1.0916 0.3392 0.7374 0.064 Uiso 1 1 calc R . . C83 C 0.9323(4) 0.40708(17) 0.72516(17) 0.0539(9) Uani 1 1 d . . . H83 H 0.9316 0.4248 0.7595 0.065 Uiso 1 1 calc R . . C84 C 0.8384(3) 0.43170(15) 0.68744(15) 0.0474(8) Uani 1 1 d . . . H84 H 0.7735 0.4657 0.6966 0.057 Uiso 1 1 calc R . . C85 C 0.7519(3) 0.51782(14) 0.53989(14) 0.0366(6) Uani 1 1 d . . . C86 C 0.7992(3) 0.55823(16) 0.56608(15) 0.0444(7) Uani 1 1 d . . . H86 H 0.8232 0.5449 0.6055 0.053 Uiso 1 1 calc R . . C87 C 0.8106(3) 0.61839(16) 0.53322(16) 0.0492(8) Uani 1 1 d . . . H87 H 0.8407 0.6457 0.5510 0.059 Uiso 1 1 calc R . . C88 C 0.7777(3) 0.63759(15) 0.47497(15) 0.0449(8) Uani 1 1 d . . . H88 H 0.7856 0.6780 0.4533 0.054 Uiso 1 1 calc R . . C89 C 0.7332(3) 0.59815(17) 0.44806(16) 0.0495(8) Uani 1 1 d . . . H89 H 0.7117 0.6116 0.4082 0.059 Uiso 1 1 calc R . . C90 C 0.7200(3) 0.53770(16) 0.48040(15) 0.0470(8) Uani 1 1 d . . . H90 H 0.6898 0.5108 0.4621 0.056 Uiso 1 1 calc R . . C91 C 0.5760(3) 0.45839(15) 0.62764(14) 0.0390(7) Uani 1 1 d . . . C92 C 0.4927(3) 0.51826(16) 0.61707(14) 0.0419(7) Uani 1 1 d . . . H92 H 0.5153 0.5522 0.5888 0.050 Uiso 1 1 calc R . . C93 C 0.3764(3) 0.52703(17) 0.64873(15) 0.0472(8) Uani 1 1 d . . . H93 H 0.3210 0.5671 0.6418 0.057 Uiso 1 1 calc R . . C94 C 0.3420(3) 0.47736(17) 0.69011(16) 0.0503(8) Uani 1 1 d . . . H94 H 0.2634 0.4838 0.7111 0.060 Uiso 1 1 calc R . . C95 C 0.4237(3) 0.41752(18) 0.70083(17) 0.0536(9) Uani 1 1 d . . . H95 H 0.3997 0.3837 0.7287 0.064 Uiso 1 1 calc R . . C96 C 0.5415(3) 0.40805(16) 0.66993(16) 0.0483(8) Uani 1 1 d . . . H96 H 0.5971 0.3681 0.6776 0.058 Uiso 1 1 calc R . . C97 C 0.1567(5) 0.3918(3) 0.8946(3) 0.0794(14) Uani 1 1 d D . . C98 C 0.1810(7) 0.3787(4) 0.8351(3) 0.147(3) Uani 1 1 d D . . H98A H 0.2210 0.4104 0.8095 0.220 Uiso 1 1 calc R . . H98B H 0.1045 0.3806 0.8195 0.220 Uiso 1 1 calc R . . H98C H 0.2341 0.3364 0.8354 0.220 Uiso 1 1 calc R . . O25 O 0.4652(8) 0.1071(3) 0.1973(3) 0.211(3) Uani 1 1 d DU . . C99 C 0.3406(8) 0.1165(5) 0.1755(5) 0.190(4) Uani 1 1 d DU . . H99A H 0.2915 0.1586 0.1822 0.228 Uiso 1 1 calc R . . H99B H 0.3001 0.0843 0.2008 0.228 Uiso 1 1 calc R . . C100 C 0.3373(9) 0.1123(4) 0.1078(5) 0.177(4) Uani 1 1 d DU . . H10A H 0.3524 0.1513 0.0821 0.265 Uiso 1 1 calc R . . H10B H 0.2574 0.1071 0.1020 0.265 Uiso 1 1 calc R . . H10C H 0.4000 0.0759 0.0974 0.265 Uiso 1 1 calc R . . C101 C 0.4879(9) 0.1094(5) 0.2594(4) 0.187(4) Uani 1 1 d DU . . H10D H 0.4403 0.0823 0.2877 0.224 Uiso 1 1 calc R . . H10E H 0.4541 0.1535 0.2662 0.224 Uiso 1 1 calc R . . C102 C 0.6218(9) 0.0889(4) 0.2773(4) 0.187(4) Uani 1 1 d DU . . H10F H 0.6582 0.0456 0.2706 0.281 Uiso 1 1 calc R . . H10G H 0.6215 0.0906 0.3197 0.281 Uiso 1 1 calc R . . H10H H 0.6693 0.1178 0.2528 0.281 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 0.03346(6) 0.04280(7) 0.03088(6) 0.00137(4) -0.00388(4) -0.00805(5) Th2 0.02997(6) 0.03622(6) 0.03199(6) -0.00157(4) -0.00576(4) -0.00849(4) P1 0.0344(4) 0.0345(4) 0.0355(4) -0.0055(3) -0.0028(3) -0.0053(3) P2 0.0397(4) 0.0345(4) 0.0342(4) -0.0078(3) -0.0036(3) -0.0103(3) P3 0.0319(4) 0.0291(4) 0.0343(4) -0.0048(3) -0.0043(3) -0.0059(3) P4 0.0372(4) 0.0325(4) 0.0360(4) -0.0069(3) -0.0008(3) -0.0048(3) O1 0.099(2) 0.0703(19) 0.0602(18) -0.0151(15) -0.0121(17) -0.0304(18) O2 0.089(2) 0.096(2) 0.0346(14) -0.0074(14) -0.0046(14) -0.0252(19) O3 0.0525(17) 0.080(2) 0.0717(19) 0.0110(16) -0.0202(15) -0.0257(16) O4 0.0475(16) 0.0689(18) 0.0603(17) -0.0050(14) 0.0010(13) 0.0047(14) O5 0.0601(18) 0.088(2) 0.0536(16) -0.0186(15) -0.0098(13) -0.0067(16) O6 0.0666(19) 0.0547(17) 0.094(2) -0.0159(16) -0.0050(17) -0.0153(14) O7 0.0376(13) 0.0676(18) 0.0728(18) -0.0205(15) -0.0128(13) -0.0023(12) O8 0.0520(15) 0.0620(16) 0.0537(15) -0.0147(13) -0.0007(12) 0.0022(13) O9 0.0620(18) 0.0631(17) 0.0597(17) 0.0055(13) -0.0156(14) 0.0004(14) O10 0.0705(19) 0.0666(18) 0.0493(16) 0.0011(13) 0.0037(14) -0.0216(16) O11 0.0410(14) 0.0687(18) 0.0662(17) 0.0296(14) -0.0020(12) -0.0021(13) O12 0.0399(14) 0.0622(17) 0.0753(19) 0.0211(14) 0.0060(13) -0.0048(12) O13 0.0594(17) 0.0498(15) 0.0635(17) -0.0114(13) 0.0017(13) 0.0054(13) O14 0.0658(18) 0.0537(16) 0.0682(18) -0.0108(13) -0.0147(14) -0.0232(14) O15 0.0520(16) 0.0557(16) 0.0728(19) 0.0137(13) -0.0126(14) -0.0088(13) O16 0.0546(16) 0.0612(17) 0.0565(16) 0.0093(12) -0.0044(13) -0.0239(14) O17 0.0576(16) 0.0774(19) 0.0416(14) -0.0014(12) -0.0115(12) -0.0177(14) O18 0.0513(15) 0.0515(15) 0.0600(17) -0.0205(13) -0.0107(12) -0.0086(12) O19 0.0498(14) 0.0412(13) 0.0505(14) -0.0041(10) -0.0108(11) -0.0044(11) O20 0.0492(14) 0.0575(15) 0.0397(12) -0.0069(11) -0.0093(10) -0.0120(12) O21 0.0439(13) 0.0455(13) 0.0499(14) -0.0134(11) 0.0020(11) -0.0154(11) O22 0.0370(13) 0.0572(15) 0.0618(16) -0.0059(12) -0.0157(11) -0.0060(11) O23 0.0385(13) 0.0672(17) 0.0517(15) 0.0044(12) -0.0143(11) -0.0167(12) O24 0.0409(14) 0.0726(18) 0.0509(15) -0.0070(13) 0.0003(11) -0.0001(12) N1 0.105(3) 0.116(4) 0.057(2) -0.027(2) -0.017(2) -0.026(3) N2 0.0386(17) 0.0485(18) 0.071(2) 0.0057(16) 0.0092(16) -0.0065(14) N3 0.0574(19) 0.0432(17) 0.0507(18) -0.0131(14) 0.0064(15) -0.0155(15) N4 0.0493(19) 0.069(2) 0.065(2) -0.0105(18) -0.0080(17) 0.0057(17) N5 0.0464(19) 0.089(3) 0.0360(16) -0.0006(16) 0.0014(14) -0.0202(18) N6 0.053(2) 0.078(3) 0.082(3) 0.027(2) 0.0077(19) -0.0133(19) N7 0.0345(15) 0.0388(15) 0.0571(18) -0.0038(12) 0.0001(13) -0.0093(12) N8 0.060(2) 0.091(3) 0.057(2) 0.0215(18) -0.0109(17) -0.034(2) N9 0.0436(17) 0.063(2) 0.059(2) -0.0224(16) 0.0067(14) -0.0193(15) N10 0.0441(16) 0.0435(16) 0.0450(16) -0.0056(12) -0.0034(12) -0.0159(13) N11 0.0406(15) 0.0431(15) 0.0408(15) -0.0134(12) 0.0037(12) -0.0048(12) N12 0.0447(18) 0.078(2) 0.0503(19) 0.0030(17) -0.0048(15) -0.0089(17) N13 0.158(6) 0.140(5) 0.124(5) -0.056(4) 0.004(4) -0.003(4) C1 0.0334(15) 0.0403(16) 0.0361(16) -0.0081(13) -0.0017(12) -0.0065(13) C2 0.054(2) 0.0391(18) 0.0471(19) -0.0015(14) -0.0134(16) -0.0087(15) C3 0.055(2) 0.057(2) 0.0437(19) -0.0038(16) -0.0146(16) -0.0134(18) C4 0.049(2) 0.067(2) 0.052(2) -0.0147(18) -0.0103(16) -0.0193(18) C5 0.060(2) 0.060(2) 0.051(2) -0.0073(17) -0.0076(17) -0.0297(19) C6 0.0474(19) 0.0449(18) 0.0385(17) -0.0016(14) -0.0024(14) -0.0131(15) C7 0.0411(17) 0.0336(15) 0.0369(16) -0.0076(12) -0.0063(13) -0.0019(13) C8 0.045(2) 0.059(2) 0.0422(19) -0.0045(16) -0.0026(15) 0.0034(17) C9 0.054(2) 0.066(3) 0.049(2) -0.0063(18) -0.0066(18) 0.0141(19) C10 0.068(3) 0.0419(19) 0.0437(19) -0.0067(15) -0.0165(18) 0.0050(17) C11 0.067(2) 0.0411(18) 0.0426(19) -0.0015(14) -0.0084(17) -0.0128(17) C12 0.048(2) 0.0427(18) 0.0461(19) -0.0087(14) -0.0065(15) -0.0073(15) C13 0.0360(16) 0.0325(15) 0.0377(16) -0.0030(12) -0.0002(12) -0.0054(13) C14 0.0440(18) 0.0395(17) 0.0447(18) -0.0019(14) -0.0037(14) -0.0061(14) C15 0.0415(19) 0.0405(18) 0.061(2) -0.0025(16) 0.0016(16) 0.0005(15) C16 0.058(2) 0.0330(17) 0.055(2) -0.0117(15) 0.0120(17) -0.0075(16) C17 0.051(2) 0.0451(19) 0.0471(19) -0.0145(15) 0.0023(16) -0.0147(16) C18 0.0410(18) 0.0469(19) 0.0481(19) -0.0118(15) -0.0026(15) -0.0109(15) C19 0.0313(15) 0.0451(17) 0.0361(16) -0.0040(13) -0.0036(12) -0.0059(13) C20 0.0411(18) 0.055(2) 0.0431(18) -0.0117(15) -0.0002(14) -0.0136(16) C21 0.053(2) 0.062(2) 0.058(2) -0.0114(18) 0.0005(18) -0.0264(19) C22 0.043(2) 0.074(3) 0.054(2) 0.0000(19) 0.0003(17) -0.0234(19) C23 0.045(2) 0.068(2) 0.0374(18) -0.0067(16) 0.0019(15) -0.0100(18) C24 0.0454(19) 0.0443(18) 0.0409(18) -0.0047(14) -0.0039(14) -0.0054(15) C25 0.061(2) 0.0333(16) 0.0439(18) -0.0098(13) -0.0134(16) -0.0131(15) C26 0.076(3) 0.059(2) 0.075(3) 0.016(2) -0.032(2) -0.037(2) C27 0.141(5) 0.061(3) 0.076(3) 0.023(2) -0.052(3) -0.058(3) C28 0.141(5) 0.035(2) 0.075(3) -0.009(2) -0.058(3) -0.004(3) C29 0.093(4) 0.075(3) 0.058(3) -0.031(2) -0.027(3) 0.036(3) C30 0.062(3) 0.070(3) 0.046(2) -0.0190(18) -0.0127(18) 0.011(2) C31 0.0503(19) 0.0423(17) 0.0355(16) -0.0091(13) -0.0068(14) -0.0160(15) C32 0.088(3) 0.085(3) 0.055(2) 0.007(2) -0.022(2) -0.053(3) C33 0.117(4) 0.122(5) 0.079(3) 0.019(3) -0.039(3) -0.086(4) C34 0.081(3) 0.103(4) 0.059(3) -0.004(2) -0.028(2) -0.048(3) C35 0.066(2) 0.053(2) 0.0376(18) -0.0084(15) -0.0135(16) -0.0096(18) C36 0.063(2) 0.0431(19) 0.0455(19) -0.0047(15) -0.0137(16) -0.0164(17) C37 0.0386(16) 0.0352(15) 0.0337(15) -0.0071(12) -0.0010(12) -0.0090(13) C38 0.0438(18) 0.0500(19) 0.0362(17) -0.0007(14) -0.0055(14) -0.0060(15) C39 0.046(2) 0.058(2) 0.047(2) -0.0081(17) 0.0011(16) 0.0052(17) C40 0.062(2) 0.049(2) 0.050(2) -0.0198(16) 0.0133(18) -0.0122(18) C41 0.055(2) 0.067(2) 0.055(2) -0.0323(19) 0.0038(18) -0.0214(19) C42 0.0432(19) 0.057(2) 0.0481(19) -0.0223(16) -0.0034(15) -0.0112(16) C43 0.0383(17) 0.0422(17) 0.0392(17) -0.0074(13) -0.0019(13) -0.0095(14) C44 0.0468(19) 0.050(2) 0.0471(19) -0.0119(15) 0.0009(15) -0.0216(16) C45 0.058(2) 0.065(3) 0.058(2) -0.0042(19) -0.0025(19) -0.031(2) C46 0.047(2) 0.079(3) 0.049(2) 0.0048(19) -0.0009(17) -0.020(2) C47 0.054(2) 0.067(3) 0.043(2) -0.0033(17) 0.0078(17) -0.0034(19) C48 0.054(2) 0.0472(19) 0.0427(19) -0.0090(15) 0.0024(16) -0.0074(16) C49 0.0327(15) 0.0357(15) 0.0367(16) -0.0071(12) -0.0048(12) -0.0054(12) C50 0.0415(17) 0.0372(16) 0.0364(16) -0.0069(13) -0.0051(13) -0.0046(13) C51 0.055(2) 0.0436(18) 0.0452(19) -0.0185(15) -0.0042(16) -0.0042(16) C52 0.053(2) 0.058(2) 0.0392(18) -0.0155(16) 0.0037(15) -0.0142(17) C53 0.0474(19) 0.050(2) 0.0377(17) -0.0060(14) 0.0017(14) -0.0132(16) C54 0.0394(17) 0.0388(17) 0.0426(17) -0.0085(13) -0.0041(13) -0.0061(14) C55 0.0343(15) 0.0266(14) 0.0376(15) -0.0055(11) -0.0017(12) -0.0061(12) C56 0.0353(16) 0.0404(17) 0.0432(17) -0.0098(13) -0.0045(13) -0.0082(13) C57 0.0452(19) 0.0458(19) 0.0427(18) 0.0013(14) -0.0032(14) -0.0111(15) C58 0.0398(18) 0.0367(17) 0.054(2) -0.0015(14) -0.0012(15) -0.0119(14) C59 0.0374(17) 0.0371(17) 0.057(2) -0.0077(14) -0.0062(15) -0.0126(14) C60 0.0394(17) 0.0383(16) 0.0397(17) -0.0048(13) -0.0070(13) -0.0112(14) C61 0.0298(14) 0.0303(14) 0.0410(16) -0.0059(12) -0.0080(12) -0.0057(12) C62 0.0358(16) 0.0331(15) 0.0418(17) -0.0072(12) -0.0026(13) -0.0111(13) C63 0.0332(16) 0.0415(17) 0.056(2) -0.0153(15) -0.0037(14) -0.0087(13) C64 0.0377(18) 0.048(2) 0.060(2) -0.0075(16) -0.0167(16) -0.0003(15) C65 0.049(2) 0.059(2) 0.054(2) 0.0067(17) -0.0161(17) -0.0005(18) C66 0.0392(18) 0.054(2) 0.0415(18) -0.0006(15) -0.0056(14) -0.0018(15) C67 0.0377(16) 0.0252(14) 0.0379(16) -0.0034(11) -0.0072(12) -0.0075(12) C68 0.0394(17) 0.0442(18) 0.0427(18) -0.0097(14) -0.0031(14) -0.0120(14) C69 0.052(2) 0.0464(19) 0.0463(19) -0.0166(15) -0.0025(15) -0.0138(16) C70 0.054(2) 0.0403(18) 0.058(2) -0.0177(16) -0.0132(17) -0.0128(16) C71 0.0371(18) 0.0475(19) 0.076(3) -0.0235(18) -0.0076(17) -0.0104(15) C72 0.0352(16) 0.0405(17) 0.056(2) -0.0188(15) -0.0021(14) -0.0080(14) C73 0.0391(17) 0.0322(15) 0.0383(16) -0.0062(12) -0.0016(13) -0.0035(13) C74 0.0461(19) 0.0445(18) 0.0406(18) -0.0094(14) 0.0038(14) -0.0065(15) C75 0.072(3) 0.0403(18) 0.0378(18) -0.0102(14) 0.0046(17) -0.0008(18) C76 0.099(3) 0.0363(18) 0.042(2) -0.0108(15) -0.001(2) -0.017(2) C77 0.078(3) 0.043(2) 0.052(2) -0.0080(16) -0.0097(19) -0.0286(19) C78 0.051(2) 0.0383(17) 0.0413(18) -0.0019(13) 0.0018(15) -0.0134(15) C79 0.0407(17) 0.0340(15) 0.0388(16) -0.0044(12) -0.0003(13) -0.0061(13) C80 0.047(2) 0.0471(19) 0.0450(19) -0.0061(15) -0.0022(15) -0.0017(16) C81 0.046(2) 0.051(2) 0.050(2) -0.0043(16) -0.0024(16) 0.0026(16) C82 0.051(2) 0.048(2) 0.055(2) 0.0079(16) -0.0160(17) -0.0090(17) C83 0.071(3) 0.0426(19) 0.047(2) -0.0021(15) -0.0182(18) -0.0100(18) C84 0.056(2) 0.0341(17) 0.0483(19) -0.0059(14) -0.0058(16) -0.0047(15) C85 0.0354(16) 0.0329(15) 0.0396(16) -0.0067(12) -0.0023(13) -0.0052(12) C86 0.0501(19) 0.0442(18) 0.0407(18) -0.0084(14) -0.0054(14) -0.0131(15) C87 0.055(2) 0.0410(18) 0.055(2) -0.0130(15) -0.0003(16) -0.0157(16) C88 0.0464(19) 0.0343(16) 0.0486(19) -0.0018(14) 0.0026(15) -0.0079(14) C89 0.056(2) 0.0461(19) 0.0433(19) 0.0007(15) -0.0080(16) -0.0110(17) C90 0.055(2) 0.0430(18) 0.0446(18) -0.0012(14) -0.0142(15) -0.0145(16) C91 0.0410(17) 0.0389(16) 0.0350(16) -0.0087(13) 0.0004(13) -0.0061(14) C92 0.0440(18) 0.0405(17) 0.0386(17) -0.0075(13) -0.0037(14) -0.0050(14) C93 0.0421(18) 0.0477(19) 0.0457(19) -0.0106(15) -0.0038(15) 0.0020(15) C94 0.0399(18) 0.058(2) 0.0474(19) -0.0096(16) 0.0021(15) -0.0046(16) C95 0.052(2) 0.052(2) 0.050(2) -0.0064(16) 0.0106(17) -0.0095(17) C96 0.047(2) 0.0402(18) 0.049(2) -0.0056(15) 0.0070(15) -0.0027(15) C97 0.075(3) 0.072(3) 0.087(4) 0.002(3) -0.015(3) -0.018(3) C98 0.169(7) 0.180(8) 0.071(4) -0.017(4) -0.025(4) 0.000(6) O25 0.295(7) 0.147(5) 0.203(6) -0.052(4) -0.020(6) -0.059(5) C99 0.140(6) 0.120(6) 0.275(9) 0.009(6) 0.004(7) -0.017(5) C100 0.204(8) 0.081(4) 0.243(8) 0.008(5) -0.039(7) -0.049(5) C101 0.234(8) 0.171(7) 0.128(6) -0.044(5) 0.043(6) -0.016(6) C102 0.244(8) 0.140(6) 0.190(7) -0.016(5) -0.005(7) -0.086(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 O1 2.556(3) . ? Th1 O10 2.561(3) . ? Th1 O3 2.562(3) . ? Th1 O11 2.565(2) . ? Th1 O12 2.566(2) . ? Th1 O2 2.566(3) . ? Th1 O7 2.569(3) . ? Th1 O4 2.572(3) . ? Th1 O8 2.574(2) . ? Th1 O5 2.579(3) . ? Th1 O6 2.583(3) . ? Th1 O9 2.586(3) . ? Th2 O23 2.554(2) . ? Th2 O14 2.555(2) . ? Th2 O24 2.564(2) . ? Th2 O17 2.567(2) . ? Th2 O13 2.569(2) . ? Th2 O18 2.571(2) . ? Th2 O20 2.575(2) . ? Th2 O22 2.577(2) . ? Th2 O16 2.581(2) . ? Th2 O19 2.583(2) . ? Th2 O21 2.584(2) . ? Th2 O15 2.594(3) . ? P1 C1 1.791(3) . ? P1 C19 1.793(3) . ? P1 C7 1.794(3) . ? P1 C13 1.798(3) . ? P2 C37 1.790(3) . ? P2 C25 1.792(3) . ? P2 C43 1.794(3) . ? P2 C31 1.795(3) . ? P3 C49 1.789(3) . ? P3 C55 1.796(3) . ? P3 C67 1.804(3) . ? P3 C61 1.805(3) . ? P4 C85 1.791(3) . ? P4 C91 1.794(3) . ? P4 C79 1.797(3) . ? P4 C73 1.801(3) . ? O1 N1 1.270(5) . ? O2 N1 1.278(5) . ? O3 N2 1.288(4) . ? O4 N2 1.200(4) . ? O5 N3 1.265(4) . ? O6 N3 1.184(4) . ? O7 N4 1.258(4) . ? O8 N4 1.260(4) . ? O9 N5 1.270(4) . ? O10 N5 1.164(4) . ? O11 N6 1.275(4) . ? O12 N6 1.263(4) . ? O13 N7 1.163(4) . ? O14 N7 1.268(4) . ? O15 N8 1.272(4) . ? O16 N8 1.222(4) . ? O17 N9 1.283(4) . ? O18 N9 1.188(4) . ? O19 N10 1.237(3) . ? O20 N10 1.242(3) . ? O21 N11 1.228(3) . ? O22 N11 1.249(4) . ? O23 N12 1.270(4) . ? O24 N12 1.244(4) . ? N13 C97 1.145(7) . ? C1 C2 1.396(4) . ? C1 C6 1.397(4) . ? C2 C3 1.386(5) . ? C2 H2 0.9300 . ? C3 C4 1.382(5) . ? C3 H3 0.9300 . ? C4 C5 1.376(5) . ? C4 H4 0.9300 . ? C5 C6 1.380(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.391(5) . ? C7 C8 1.396(5) . ? C8 C9 1.391(5) . ? C8 H8 0.9300 . ? C9 C10 1.386(6) . ? C9 H9 0.9300 . ? C10 C11 1.394(5) . ? C10 H10 0.9300 . ? C11 C12 1.387(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.390(4) . ? C13 C14 1.392(4) . ? C14 C15 1.387(5) . ? C14 H14 0.9300 . ? C15 C16 1.376(5) . ? C15 H15 0.9300 . ? C16 C17 1.362(5) . ? C16 H16 0.9300 . ? C17 C18 1.392(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.382(4) . ? C19 C24 1.412(4) . ? C20 C21 1.388(5) . ? C20 H20 0.9300 . ? C21 C22 1.390(5) . ? C21 H21 0.9300 . ? C22 C23 1.372(5) . ? C22 H22 0.9300 . ? C23 C24 1.382(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.385(5) . ? C25 C26 1.393(5) . ? C26 C27 1.380(6) . ? C26 H26 0.9300 . ? C27 C28 1.405(8) . ? C27 H27 0.9300 . ? C28 C29 1.342(7) . ? C28 H28 0.9300 . ? C29 C30 1.382(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.381(4) . ? C31 C32 1.388(5) . ? C32 C33 1.384(6) . ? C32 H32 0.9300 . ? C33 C34 1.377(6) . ? C33 H33 0.9300 . ? C34 C35 1.360(5) . ? C34 H34 0.9300 . ? C35 C36 1.383(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.372(4) . ? C37 C42 1.406(4) . ? C38 C39 1.389(5) . ? C38 H38 0.9300 . ? C39 C40 1.371(5) . ? C39 H39 0.9300 . ? C40 C41 1.379(5) . ? C40 H40 0.9300 . ? C41 C42 1.383(5) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.394(4) . ? C43 C48 1.395(5) . ? C44 C45 1.381(5) . ? C44 H44 0.9300 . ? C45 C46 1.376(6) . ? C45 H45 0.9300 . ? C46 C47 1.372(6) . ? C46 H46 0.9300 . ? C47 C48 1.390(5) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.399(4) . ? C49 C54 1.401(4) . ? C50 C51 1.376(4) . ? C50 H50 0.9300 . ? C51 C52 1.388(5) . ? C51 H51 0.9300 . ? C52 C53 1.374(5) . ? C52 H52 0.9300 . ? C53 C54 1.393(4) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C56 1.382(4) . ? C55 C60 1.402(4) . ? C56 C57 1.390(4) . ? C56 H56 0.9300 . ? C57 C58 1.392(5) . ? C57 H57 0.9300 . ? C58 C59 1.373(5) . ? C58 H58 0.9300 . ? C59 C60 1.384(4) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 C66 1.395(4) . ? C61 C62 1.398(4) . ? C62 C63 1.386(4) . ? C62 H62 0.9300 . ? C63 C64 1.377(5) . ? C63 H63 0.9300 . ? C64 C65 1.371(5) . ? C64 H64 0.9300 . ? C65 C66 1.388(5) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 C72 1.388(4) . ? C67 C68 1.395(4) . ? C68 C69 1.384(4) . ? C68 H68 0.9300 . ? C69 C70 1.374(5) . ? C69 H69 0.9300 . ? C70 C71 1.370(5) . ? C70 H70 0.9300 . ? C71 C72 1.391(4) . ? C71 H71 0.9300 . ? C72 H72 0.9300 . ? C73 C74 1.380(4) . ? C73 C78 1.383(4) . ? C74 C75 1.382(5) . ? C74 H74 0.9300 . ? C75 C76 1.357(5) . ? C75 H75 0.9300 . ? C76 C77 1.382(6) . ? C76 H76 0.9300 . ? C77 C78 1.389(5) . ? C77 H77 0.9300 . ? C78 H78 0.9300 . ? C79 C84 1.397(4) . ? C79 C80 1.399(4) . ? C80 C81 1.379(5) . ? C80 H80 0.9300 . ? C81 C82 1.371(5) . ? C81 H81 0.9300 . ? C82 C83 1.387(5) . ? C82 H82 0.9300 . ? C83 C84 1.376(5) . ? C83 H83 0.9300 . ? C84 H84 0.9300 . ? C85 C90 1.386(4) . ? C85 C86 1.391(4) . ? C86 C87 1.387(4) . ? C86 H86 0.9300 . ? C87 C88 1.363(5) . ? C87 H87 0.9300 . ? C88 C89 1.365(5) . ? C88 H88 0.9300 . ? C89 C90 1.394(4) . ? C89 H89 0.9300 . ? C90 H90 0.9300 . ? C91 C96 1.387(4) . ? C91 C92 1.392(4) . ? C92 C93 1.381(5) . ? C92 H92 0.9300 . ? C93 C94 1.367(5) . ? C93 H93 0.9300 . ? C94 C95 1.383(5) . ? C94 H94 0.9300 . ? C95 C96 1.389(5) . ? C95 H95 0.9300 . ? C96 H96 0.9300 . ? C97 C98 1.400(6) . ? C98 H98A 0.9600 . ? C98 H98B 0.9600 . ? C98 H98C 0.9600 . ? O25 C101 1.467(7) . ? O25 C99 1.498(7) . ? C99 C100 1.549(8) . ? C99 H99A 0.9700 . ? C99 H99B 0.9700 . ? C100 H10A 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? C101 C102 1.540(7) . ? C101 H10D 0.9700 . ? C101 H10E 0.9700 . ? C102 H10F 0.9600 . ? C102 H10G 0.9600 . ? C102 H10H 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Th1 O10 68.24(9) . . ? O1 Th1 O3 67.62(11) . . ? O10 Th1 O3 69.80(10) . . ? O1 Th1 O11 112.85(11) . . ? O10 Th1 O11 133.76(9) . . ? O3 Th1 O11 68.99(9) . . ? O1 Th1 O12 113.25(10) . . ? O10 Th1 O12 177.01(9) . . ? O3 Th1 O12 113.11(9) . . ? O11 Th1 O12 48.51(8) . . ? O1 Th1 O2 49.09(10) . . ? O10 Th1 O2 113.43(10) . . ? O3 Th1 O2 67.94(10) . . ? O11 Th1 O2 68.20(11) . . ? O12 Th1 O2 68.88(10) . . ? O1 Th1 O7 111.16(10) . . ? O10 Th1 O7 109.06(10) . . ? O3 Th1 O7 178.52(9) . . ? O11 Th1 O7 112.41(9) . . ? O12 Th1 O7 68.04(9) . . ? O2 Th1 O7 111.99(10) . . ? O1 Th1 O4 110.93(11) . . ? O10 Th1 O4 67.95(9) . . ? O3 Th1 O4 48.38(10) . . ? O11 Th1 O4 69.36(9) . . ? O12 Th1 O4 113.27(9) . . ? O2 Th1 O4 112.14(10) . . ? O7 Th1 O4 132.30(9) . . ? O1 Th1 O8 67.76(10) . . ? O10 Th1 O8 109.85(9) . . ? O3 Th1 O8 131.24(10) . . ? O11 Th1 O8 112.72(8) . . ? O12 Th1 O8 68.94(9) . . ? O2 Th1 O8 68.50(10) . . ? O7 Th1 O8 48.02(9) . . ? O4 Th1 O8 177.79(8) . . ? O1 Th1 O5 132.35(10) . . ? O10 Th1 O5 67.55(10) . . ? O3 Th1 O5 111.53(10) . . ? O11 Th1 O5 110.14(10) . . ? O12 Th1 O5 110.19(10) . . ? O2 Th1 O5 178.34(10) . . ? O7 Th1 O5 68.58(9) . . ? O4 Th1 O5 66.83(9) . . ? O8 Th1 O5 112.59(9) . . ? O1 Th1 O6 179.43(10) . . ? O10 Th1 O6 111.27(10) . . ? O3 Th1 O6 111.99(10) . . ? O11 Th1 O6 67.24(11) . . ? O12 Th1 O6 67.25(10) . . ? O2 Th1 O6 131.24(11) . . ? O7 Th1 O6 69.23(9) . . ? O4 Th1 O6 68.55(10) . . ? O8 Th1 O6 112.75(9) . . ? O5 Th1 O6 47.31(10) . . ? O1 Th1 O9 69.48(10) . . ? O10 Th1 O9 47.60(10) . . ? O3 Th1 O9 113.19(10) . . ? O11 Th1 O9 177.47(9) . . ? O12 Th1 O9 130.04(9) . . ? O2 Th1 O9 113.61(10) . . ? O7 Th1 O9 65.42(9) . . ? O4 Th1 O9 110.97(9) . . ? O8 Th1 O9 66.99(9) . . ? O5 Th1 O9 68.05(10) . . ? O6 Th1 O9 110.43(10) . . ? O23 Th2 O14 66.31(9) . . ? O23 Th2 O24 48.62(9) . . ? O14 Th2 O24 110.11(9) . . ? O23 Th2 O17 112.56(9) . . ? O14 Th2 O17 131.42(9) . . ? O24 Th2 O17 68.20(9) . . ? O23 Th2 O13 109.91(9) . . ? O14 Th2 O13 47.76(9) . . ? O24 Th2 O13 157.60(10) . . ? O17 Th2 O13 126.61(9) . . ? O23 Th2 O18 113.05(9) . . ? O14 Th2 O18 179.00(9) . . ? O24 Th2 O18 69.02(9) . . ? O17 Th2 O18 47.94(9) . . ? O13 Th2 O18 133.15(9) . . ? O23 Th2 O20 68.26(8) . . ? O14 Th2 O20 69.69(8) . . ? O24 Th2 O20 102.27(8) . . ? O17 Th2 O20 158.33(9) . . ? O13 Th2 O20 69.19(8) . . ? O18 Th2 O20 110.87(8) . . ? O23 Th2 O22 177.15(8) . . ? O14 Th2 O22 110.85(9) . . ? O24 Th2 O22 134.01(9) . . ? O17 Th2 O22 69.37(9) . . ? O13 Th2 O22 67.33(9) . . ? O18 Th2 O22 69.79(8) . . ? O20 Th2 O22 110.79(8) . . ? O23 Th2 O16 69.68(9) . . ? O14 Th2 O16 67.89(9) . . ? O24 Th2 O16 68.28(9) . . ? O17 Th2 O16 67.08(9) . . ? O13 Th2 O16 100.34(9) . . ? O18 Th2 O16 111.21(9) . . ? O20 Th2 O16 129.02(8) . . ? O22 Th2 O16 109.77(9) . . ? O23 Th2 O19 69.65(8) . . ? O14 Th2 O19 112.88(8) . . ? O24 Th2 O19 69.04(8) . . ? O17 Th2 O19 111.06(8) . . ? O13 Th2 O19 113.02(8) . . ? O18 Th2 O19 67.35(8) . . ? O20 Th2 O19 47.83(8) . . ? O22 Th2 O19 111.86(8) . . ? O16 Th2 O19 133.99(9) . . ? O23 Th2 O21 132.44(8) . . ? O14 Th2 O21 111.02(8) . . ? O24 Th2 O21 129.51(8) . . ? O17 Th2 O21 103.22(8) . . ? O13 Th2 O21 67.64(8) . . ? O18 Th2 O21 69.97(8) . . ? O20 Th2 O21 67.02(7) . . ? O22 Th2 O21 47.73(8) . . ? O16 Th2 O21 156.74(9) . . ? O19 Th2 O21 68.82(8) . . ? O23 Th2 O15 112.57(9) . . ? O14 Th2 O15 68.59(9) . . ? O24 Th2 O15 112.22(9) . . ? O17 Th2 O15 68.19(9) . . ? O13 Th2 O15 66.58(9) . . ? O18 Th2 O15 111.21(9) . . ? O20 Th2 O15 132.67(9) . . ? O22 Th2 O15 65.92(9) . . ? O16 Th2 O15 47.91(9) . . ? O19 Th2 O15 177.78(8) . . ? O21 Th2 O15 109.19(8) . . ? C1 P1 C19 107.58(14) . . ? C1 P1 C7 111.73(14) . . ? C19 P1 C7 110.82(15) . . ? C1 P1 C13 109.86(15) . . ? C19 P1 C13 109.97(14) . . ? C7 P1 C13 106.89(14) . . ? C37 P2 C25 106.47(15) . . ? C37 P2 C43 110.59(14) . . ? C25 P2 C43 110.40(16) . . ? C37 P2 C31 109.06(15) . . ? C25 P2 C31 112.05(15) . . ? C43 P2 C31 108.27(15) . . ? C49 P3 C55 110.15(13) . . ? C49 P3 C67 109.63(14) . . ? C55 P3 C67 109.98(13) . . ? C49 P3 C61 110.37(14) . . ? C55 P3 C61 106.32(14) . . ? C67 P3 C61 110.35(13) . . ? C85 P4 C91 109.42(14) . . ? C85 P4 C79 110.97(14) . . ? C91 P4 C79 108.32(15) . . ? C85 P4 C73 108.09(14) . . ? C91 P4 C73 110.01(15) . . ? C79 P4 C73 110.03(14) . . ? N1 O1 Th1 99.2(3) . . ? N1 O2 Th1 98.4(2) . . ? N2 O3 Th1 97.0(2) . . ? N2 O4 Th1 99.1(2) . . ? N3 O5 Th1 97.2(2) . . ? N3 O6 Th1 99.4(2) . . ? N4 O7 Th1 99.9(2) . . ? N4 O8 Th1 99.6(2) . . ? N5 O9 Th1 95.3(2) . . ? N5 O10 Th1 99.6(2) . . ? N6 O11 Th1 99.4(2) . . ? N6 O12 Th1 99.7(2) . . ? N7 O13 Th2 98.7(2) . . ? N7 O14 Th2 96.37(19) . . ? N8 O15 Th2 97.6(2) . . ? N8 O16 Th2 99.7(2) . . ? N9 O17 Th2 97.0(2) . . ? N9 O18 Th2 99.6(2) . . ? N10 O19 Th2 98.33(18) . . ? N10 O20 Th2 98.57(18) . . ? N11 O21 Th2 98.48(18) . . ? N11 O22 Th2 98.20(19) . . ? N12 O23 Th2 98.6(2) . . ? N12 O24 Th2 98.9(2) . . ? O1 N1 O2 113.3(4) . . ? O4 N2 O3 115.4(3) . . ? O6 N3 O5 115.5(3) . . ? O7 N4 O8 112.4(3) . . ? O10 N5 O9 117.2(3) . . ? O12 N6 O11 112.3(3) . . ? O13 N7 O14 117.1(3) . . ? O16 N8 O15 114.8(3) . . ? O18 N9 O17 115.2(3) . . ? O19 N10 O20 115.0(3) . . ? O21 N11 O22 114.9(3) . . ? O24 N12 O23 113.8(3) . . ? C2 C1 C6 119.7(3) . . ? C2 C1 P1 118.4(2) . . ? C6 C1 P1 121.9(2) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 119.9(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.8(3) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 119.6(3) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? C12 C7 C8 120.3(3) . . ? C12 C7 P1 118.5(3) . . ? C8 C7 P1 121.1(3) . . ? C9 C8 C7 119.5(3) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 119.7(4) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 121.0(3) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 119.2(3) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C7 120.2(3) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C18 C13 C14 120.0(3) . . ? C18 C13 P1 118.5(2) . . ? C14 C13 P1 121.5(2) . . ? C15 C14 C13 119.2(3) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 121.1(3) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 119.7(3) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C13 C18 C17 119.8(3) . . ? C13 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C20 C19 C24 119.7(3) . . ? C20 C19 P1 121.9(2) . . ? C24 C19 P1 118.5(2) . . ? C19 C20 C21 120.2(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C22 119.5(3) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 120.8(3) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 120.3(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 119.5(3) . . ? C23 C24 H24 120.3 . . ? C19 C24 H24 120.3 . . ? C30 C25 C26 119.4(4) . . ? C30 C25 P2 122.0(3) . . ? C26 C25 P2 118.4(3) . . ? C27 C26 C25 120.3(5) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C28 118.7(5) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? C29 C28 C27 120.8(4) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.7(5) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C29 C30 C25 119.9(4) . . ? C29 C30 H30 120.1 . . ? C25 C30 H30 120.1 . . ? C36 C31 C32 119.7(3) . . ? C36 C31 P2 119.4(2) . . ? C32 C31 P2 121.0(3) . . ? C33 C32 C31 118.6(4) . . ? C33 C32 H32 120.7 . . ? C31 C32 H32 120.7 . . ? C34 C33 C32 121.1(4) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C35 C34 C33 120.3(4) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 119.5(3) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C31 C36 C35 120.7(3) . . ? C31 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C38 C37 C42 120.3(3) . . ? C38 C37 P2 122.5(2) . . ? C42 C37 P2 117.2(2) . . ? C37 C38 C39 120.1(3) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 119.5(3) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 121.1(3) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C40 C41 C42 120.0(3) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C41 C42 C37 118.9(3) . . ? C41 C42 H42 120.5 . . ? C37 C42 H42 120.5 . . ? C44 C43 C48 119.9(3) . . ? C44 C43 P2 121.2(2) . . ? C48 C43 P2 118.9(2) . . ? C45 C44 C43 119.6(3) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C46 C45 C44 120.1(4) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C47 C46 C45 121.0(4) . . ? C47 C46 H46 119.5 . . ? C45 C46 H46 119.5 . . ? C46 C47 C48 119.8(4) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C47 C48 C43 119.6(3) . . ? C47 C48 H48 120.2 . . ? C43 C48 H48 120.2 . . ? C50 C49 C54 119.3(3) . . ? C50 C49 P3 121.1(2) . . ? C54 C49 P3 119.7(2) . . ? C51 C50 C49 120.1(3) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C50 C51 C52 120.5(3) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C53 C52 C51 120.0(3) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 120.4(3) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? C53 C54 C49 119.7(3) . . ? C53 C54 H54 120.2 . . ? C49 C54 H54 120.2 . . ? C56 C55 C60 120.1(3) . . ? C56 C55 P3 122.1(2) . . ? C60 C55 P3 117.8(2) . . ? C55 C56 C57 119.9(3) . . ? C55 C56 H56 120.1 . . ? C57 C56 H56 120.1 . . ? C56 C57 C58 119.8(3) . . ? C56 C57 H57 120.1 . . ? C58 C57 H57 120.1 . . ? C59 C58 C57 120.3(3) . . ? C59 C58 H58 119.9 . . ? C57 C58 H58 119.9 . . ? C58 C59 C60 120.5(3) . . ? C58 C59 H59 119.7 . . ? C60 C59 H59 119.7 . . ? C59 C60 C55 119.4(3) . . ? C59 C60 H60 120.3 . . ? C55 C60 H60 120.3 . . ? C66 C61 C62 119.9(3) . . ? C66 C61 P3 122.4(2) . . ? C62 C61 P3 117.6(2) . . ? C63 C62 C61 119.3(3) . . ? C63 C62 H62 120.4 . . ? C61 C62 H62 120.4 . . ? C64 C63 C62 120.6(3) . . ? C64 C63 H63 119.7 . . ? C62 C63 H63 119.7 . . ? C65 C64 C63 120.2(3) . . ? C65 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C64 C65 C66 120.7(3) . . ? C64 C65 H65 119.6 . . ? C66 C65 H65 119.6 . . ? C65 C66 C61 119.2(3) . . ? C65 C66 H66 120.4 . . ? C61 C66 H66 120.4 . . ? C72 C67 C68 119.5(3) . . ? C72 C67 P3 120.7(2) . . ? C68 C67 P3 119.7(2) . . ? C69 C68 C67 120.0(3) . . ? C69 C68 H68 120.0 . . ? C67 C68 H68 120.0 . . ? C70 C69 C68 119.7(3) . . ? C70 C69 H69 120.1 . . ? C68 C69 H69 120.1 . . ? C71 C70 C69 121.0(3) . . ? C71 C70 H70 119.5 . . ? C69 C70 H70 119.5 . . ? C70 C71 C72 119.9(3) . . ? C70 C71 H71 120.0 . . ? C72 C71 H71 120.0 . . ? C67 C72 C71 119.8(3) . . ? C67 C72 H72 120.1 . . ? C71 C72 H72 120.1 . . ? C74 C73 C78 120.3(3) . . ? C74 C73 P4 118.9(3) . . ? C78 C73 P4 120.8(2) . . ? C73 C74 C75 120.0(3) . . ? C73 C74 H74 120.0 . . ? C75 C74 H74 120.0 . . ? C76 C75 C74 119.8(3) . . ? C76 C75 H75 120.1 . . ? C74 C75 H75 120.1 . . ? C75 C76 C77 121.2(3) . . ? C75 C76 H76 119.4 . . ? C77 C76 H76 119.4 . . ? C76 C77 C78 119.5(4) . . ? C76 C77 H77 120.3 . . ? C78 C77 H77 120.3 . . ? C73 C78 C77 119.3(3) . . ? C73 C78 H78 120.4 . . ? C77 C78 H78 120.4 . . ? C84 C79 C80 119.6(3) . . ? C84 C79 P4 118.9(2) . . ? C80 C79 P4 121.4(2) . . ? C81 C80 C79 119.4(3) . . ? C81 C80 H80 120.3 . . ? C79 C80 H80 120.3 . . ? C82 C81 C80 120.6(3) . . ? C82 C81 H81 119.7 . . ? C80 C81 H81 119.7 . . ? C81 C82 C83 120.4(3) . . ? C81 C82 H82 119.8 . . ? C83 C82 H82 119.8 . . ? C84 C83 C82 119.9(3) . . ? C84 C83 H83 120.1 . . ? C82 C83 H83 120.1 . . ? C83 C84 C79 120.0(3) . . ? C83 C84 H84 120.0 . . ? C79 C84 H84 120.0 . . ? C90 C85 C86 119.2(3) . . ? C90 C85 P4 120.0(2) . . ? C86 C85 P4 120.6(2) . . ? C87 C86 C85 119.9(3) . . ? C87 C86 H86 120.1 . . ? C85 C86 H86 120.1 . . ? C88 C87 C86 120.3(3) . . ? C88 C87 H87 119.9 . . ? C86 C87 H87 119.9 . . ? C87 C88 C89 120.8(3) . . ? C87 C88 H88 119.6 . . ? C89 C88 H88 119.6 . . ? C88 C89 C90 120.0(3) . . ? C88 C89 H89 120.0 . . ? C90 C89 H89 120.0 . . ? C85 C90 C89 119.9(3) . . ? C85 C90 H90 120.1 . . ? C89 C90 H90 120.1 . . ? C96 C91 C92 119.7(3) . . ? C96 C91 P4 118.9(2) . . ? C92 C91 P4 121.2(2) . . ? C93 C92 C91 119.7(3) . . ? C93 C92 H92 120.1 . . ? C91 C92 H92 120.1 . . ? C94 C93 C92 120.7(3) . . ? C94 C93 H93 119.7 . . ? C92 C93 H93 119.7 . . ? C93 C94 C95 120.2(3) . . ? C93 C94 H94 119.9 . . ? C95 C94 H94 119.9 . . ? C94 C95 C96 119.9(3) . . ? C94 C95 H95 120.0 . . ? C96 C95 H95 120.0 . . ? C91 C96 C95 119.8(3) . . ? C91 C96 H96 120.1 . . ? C95 C96 H96 120.1 . . ? N13 C97 C98 177.7(7) . . ? C97 C98 H98A 109.5 . . ? C97 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C97 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C101 O25 C99 125.5(8) . . ? O25 C99 C100 117.2(8) . . ? O25 C99 H99A 108.0 . . ? C100 C99 H99A 108.0 . . ? O25 C99 H99B 108.0 . . ? C100 C99 H99B 108.0 . . ? H99A C99 H99B 107.2 . . ? C99 C100 H10A 109.5 . . ? C99 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C99 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? O25 C101 C102 119.1(7) . . ? O25 C101 H10D 107.5 . . ? C102 C101 H10D 107.5 . . ? O25 C101 H10E 107.5 . . ? C102 C101 H10E 107.5 . . ? H10D C101 H10E 107.0 . . ? C101 C102 H10F 109.5 . . ? C101 C102 H10G 109.5 . . ? H10F C102 H10G 109.5 . . ? C101 C102 H10H 109.5 . . ? H10F C102 H10H 109.5 . . ? H10G C102 H10H 109.5 . . ? data_2 _database_code_depnum_ccdc_archive 'CCDC 915621' #TrackingRef 'web_deposit_cif_file_0_P.Thuery_1355410149.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H40 N4 O10 P2 U' _chemical_formula_weight 1132.81 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _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 10.0718(2) _cell_length_b 10.7528(2) _cell_length_c 11.7809(3) _cell_angle_alpha 99.5411(7) _cell_angle_beta 93.7891(7) _cell_angle_gamma 114.6103(9) _cell_volume 1130.86(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 71913 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 30.51 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 558 _exptl_absorpt_coefficient_mu 3.723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.613 _exptl_absorpt_correction_T_max 0.771 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and twelve \w scans with 1\% steps (1531 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 71913 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 30.51 _reflns_number_total 6903 _reflns_number_gt 6859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. 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^)+(0.0191P)^2^+0.1655P] 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 6903 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0214 _refine_ls_wR_factor_ref 0.0514 _refine_ls_wR_factor_gt 0.0513 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.537 _refine_diff_density_min -1.140 _refine_diff_density_rms 0.129 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 U U 0.0000 0.5000 0.0000 0.02393(3) Uani 1 2 d S . . P1 P 0.62025(5) 0.69519(5) 0.31839(4) 0.02120(9) Uani 1 1 d . . . O1 O -0.16520(16) 0.50718(18) -0.05091(12) 0.0319(3) Uani 1 1 d . . . O2 O -0.1204(2) 0.36010(19) 0.14848(14) 0.0420(4) Uani 1 1 d . . . O3 O -0.03933(19) 0.5763(2) 0.20649(12) 0.0378(4) Uani 1 1 d . . . O4 O 0.11157(17) 0.74657(18) 0.07273(13) 0.0357(3) Uani 1 1 d . . . O5 O 0.2981(2) 0.9359(2) 0.15000(17) 0.0523(5) Uani 1 1 d . . . N1 N -0.1003(3) 0.4585(3) 0.23179(16) 0.0421(5) Uani 1 1 d . . . N2 N 0.2539(2) 0.8128(2) 0.10699(17) 0.0422(5) Uani 1 1 d . . . C1 C 0.7144(2) 0.8269(2) 0.23843(14) 0.0225(3) Uani 1 1 d . . . C2 C 0.8485(2) 0.8375(2) 0.20239(15) 0.0254(4) Uani 1 1 d . . . H2 H 0.8858 0.7750 0.2174 0.030 Uiso 1 1 calc R . . C3 C 0.9245(2) 0.9417(2) 0.14440(16) 0.0293(4) Uani 1 1 d . . . H3 H 1.0126 0.9484 0.1197 0.035 Uiso 1 1 calc R . . C4 C 0.8704(2) 1.0365(2) 0.12271(15) 0.0298(4) Uani 1 1 d . . . H4 H 0.9232 1.1075 0.0853 0.036 Uiso 1 1 calc R . . C5 C 0.7371(2) 1.0247(2) 0.15699(16) 0.0291(4) Uani 1 1 d . . . H5 H 0.7003 1.0874 0.1416 0.035 Uiso 1 1 calc R . . C6 C 0.6587(2) 0.9207(2) 0.21380(15) 0.0257(4) Uani 1 1 d . . . H6 H 0.5690 0.9128 0.2357 0.031 Uiso 1 1 calc R . . C7 C 0.4952(2) 0.7420(2) 0.39795(15) 0.0243(3) Uani 1 1 d . . . C8 C 0.5300(2) 0.7931(2) 0.51799(16) 0.0296(4) Uani 1 1 d . . . H8 H 0.6140 0.7957 0.5584 0.036 Uiso 1 1 calc R . . C9 C 0.4394(3) 0.8399(3) 0.57716(18) 0.0364(5) Uani 1 1 d . . . H9 H 0.4621 0.8735 0.6574 0.044 Uiso 1 1 calc R . . C10 C 0.3156(2) 0.8364(3) 0.5167(2) 0.0383(5) Uani 1 1 d . . . H10 H 0.2568 0.8709 0.5560 0.046 Uiso 1 1 calc R . . C11 C 0.2779(2) 0.7823(3) 0.3980(2) 0.0361(5) Uani 1 1 d . . . H11 H 0.1925 0.7781 0.3585 0.043 Uiso 1 1 calc R . . C12 C 0.3670(2) 0.7341(2) 0.33761(18) 0.0301(4) Uani 1 1 d . . . H12 H 0.3416 0.6971 0.2579 0.036 Uiso 1 1 calc R . . C13 C 0.5235(2) 0.5248(2) 0.22660(15) 0.0235(3) Uani 1 1 d . . . C14 C 0.3994(2) 0.4262(2) 0.25931(17) 0.0330(4) Uani 1 1 d . . . H14 H 0.3583 0.4526 0.3220 0.040 Uiso 1 1 calc R . . C15 C 0.3369(3) 0.2882(3) 0.19805(19) 0.0405(5) Uani 1 1 d . . . H15 H 0.2531 0.2220 0.2189 0.049 Uiso 1 1 calc R . . C16 C 0.3999(3) 0.2490(3) 0.10540(18) 0.0380(5) Uani 1 1 d . . . H16 H 0.3597 0.1560 0.0658 0.046 Uiso 1 1 calc R . . C17 C 0.5217(2) 0.3475(3) 0.07182(17) 0.0339(5) Uani 1 1 d . . . H17 H 0.5622 0.3209 0.0089 0.041 Uiso 1 1 calc R . . C18 C 0.5842(2) 0.4863(2) 0.13156(15) 0.0273(4) Uani 1 1 d . . . H18 H 0.6656 0.5529 0.1084 0.033 Uiso 1 1 calc R . . C19 C 0.7575(2) 0.6919(2) 0.42217(14) 0.0224(3) Uani 1 1 d . . . C20 C 0.7564(2) 0.5664(2) 0.43690(16) 0.0259(4) Uani 1 1 d . . . H20 H 0.6884 0.4823 0.3895 0.031 Uiso 1 1 calc R . . C21 C 0.8585(2) 0.5672(3) 0.52364(17) 0.0311(4) Uani 1 1 d . . . H21 H 0.8590 0.4834 0.5336 0.037 Uiso 1 1 calc R . . C22 C 0.9580(2) 0.6914(3) 0.59424(17) 0.0325(4) Uani 1 1 d . . . H22 H 1.0244 0.6910 0.6528 0.039 Uiso 1 1 calc R . . C23 C 0.9605(2) 0.8178(2) 0.57892(16) 0.0305(4) Uani 1 1 d . . . H23 H 1.0288 0.9016 0.6265 0.037 Uiso 1 1 calc R . . C24 C 0.8608(2) 0.8183(2) 0.49246(15) 0.0268(4) Uani 1 1 d . . . H24 H 0.8626 0.9025 0.4812 0.032 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 U 0.02809(5) 0.02248(6) 0.02418(5) 0.00660(4) 0.00496(3) 0.01306(4) P1 0.0231(2) 0.0189(2) 0.02083(19) 0.00386(17) 0.00389(16) 0.00838(18) O1 0.0322(7) 0.0341(9) 0.0344(7) 0.0097(6) 0.0049(6) 0.0182(7) O2 0.0618(11) 0.0326(10) 0.0399(8) 0.0172(7) 0.0214(7) 0.0232(9) O3 0.0550(10) 0.0365(10) 0.0292(7) 0.0074(6) 0.0108(6) 0.0259(9) O4 0.0370(8) 0.0257(9) 0.0424(8) 0.0062(6) 0.0049(6) 0.0124(7) O5 0.0574(11) 0.0262(10) 0.0578(11) 0.0060(8) -0.0064(9) 0.0064(9) N1 0.0603(13) 0.0454(14) 0.0349(9) 0.0150(9) 0.0150(9) 0.0331(12) N2 0.0441(11) 0.0328(12) 0.0444(10) 0.0094(9) -0.0027(8) 0.0124(9) C1 0.0266(8) 0.0192(9) 0.0191(7) 0.0027(6) 0.0030(6) 0.0080(7) C2 0.0302(9) 0.0239(10) 0.0239(8) 0.0049(7) 0.0068(7) 0.0131(8) C3 0.0318(10) 0.0276(11) 0.0262(8) 0.0054(7) 0.0100(7) 0.0098(8) C4 0.0397(11) 0.0240(10) 0.0219(8) 0.0055(7) 0.0068(7) 0.0095(9) C5 0.0393(10) 0.0235(10) 0.0245(8) 0.0043(7) 0.0021(7) 0.0144(9) C6 0.0308(9) 0.0225(10) 0.0240(8) 0.0041(7) 0.0048(7) 0.0120(8) C7 0.0257(8) 0.0210(9) 0.0264(8) 0.0055(7) 0.0076(7) 0.0097(7) C8 0.0317(10) 0.0294(11) 0.0281(9) 0.0049(8) 0.0082(7) 0.0136(9) C9 0.0398(11) 0.0335(13) 0.0342(10) 0.0019(9) 0.0138(8) 0.0150(10) C10 0.0348(11) 0.0312(12) 0.0503(12) 0.0052(10) 0.0190(9) 0.0151(10) C11 0.0254(9) 0.0320(12) 0.0517(12) 0.0086(10) 0.0079(9) 0.0131(9) C12 0.0271(9) 0.0275(11) 0.0339(9) 0.0063(8) 0.0042(7) 0.0103(8) C13 0.0249(8) 0.0196(9) 0.0225(7) 0.0022(6) 0.0006(6) 0.0077(7) C14 0.0327(10) 0.0270(11) 0.0287(9) 0.0033(8) 0.0082(8) 0.0032(9) C15 0.0399(12) 0.0259(12) 0.0375(11) 0.0037(9) 0.0065(9) -0.0023(9) C16 0.0485(13) 0.0227(11) 0.0310(10) -0.0019(8) -0.0042(9) 0.0083(10) C17 0.0408(11) 0.0276(12) 0.0281(9) -0.0020(8) 0.0013(8) 0.0134(9) C18 0.0291(9) 0.0235(10) 0.0259(8) 0.0028(7) 0.0036(7) 0.0092(8) C19 0.0250(8) 0.0221(9) 0.0215(7) 0.0057(6) 0.0056(6) 0.0107(7) C20 0.0285(9) 0.0231(10) 0.0277(8) 0.0064(7) 0.0078(7) 0.0118(8) C21 0.0345(10) 0.0312(12) 0.0358(10) 0.0161(8) 0.0105(8) 0.0181(9) C22 0.0306(10) 0.0405(13) 0.0298(9) 0.0152(9) 0.0046(7) 0.0157(9) C23 0.0294(9) 0.0293(11) 0.0277(8) 0.0051(8) -0.0007(7) 0.0091(8) C24 0.0302(9) 0.0227(10) 0.0273(8) 0.0058(7) 0.0024(7) 0.0114(8) _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 U O1 1.7676(13) . ? U O1 1.7677(13) 2_565 ? U O4 2.3800(17) 2_565 ? U O4 2.3800(17) . ? U O2 2.5349(17) . ? U O2 2.5349(17) 2_565 ? U O3 2.5465(14) 2_565 ? U O3 2.5465(14) . ? P1 C13 1.7871(19) . ? P1 C1 1.798(2) . ? P1 C19 1.7995(17) . ? P1 C7 1.8014(18) . ? O2 N1 1.255(3) . ? O3 N1 1.254(3) . ? O4 N2 1.305(3) . ? O5 N2 1.211(3) . ? C1 C6 1.400(3) . ? C1 C2 1.408(2) . ? C2 C3 1.384(3) . ? C2 H2 0.9300 . ? C3 C4 1.390(3) . ? C3 H3 0.9300 . ? C4 C5 1.389(3) . ? C4 H4 0.9300 . ? C5 C6 1.380(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.393(3) . ? C7 C12 1.396(3) . ? C8 C9 1.387(3) . ? C8 H8 0.9300 . ? C9 C10 1.378(3) . ? C9 H9 0.9300 . ? C10 C11 1.384(3) . ? C10 H10 0.9300 . ? C11 C12 1.389(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.390(3) . ? C13 C18 1.395(3) . ? C14 C15 1.388(3) . ? C14 H14 0.9300 . ? C15 C16 1.390(3) . ? C15 H15 0.9300 . ? C16 C17 1.380(3) . ? C16 H16 0.9300 . ? C17 C18 1.389(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.385(3) . ? C19 C24 1.396(3) . ? C20 C21 1.397(3) . ? C20 H20 0.9300 . ? C21 C22 1.374(3) . ? C21 H21 0.9300 . ? C22 C23 1.390(3) . ? C22 H22 0.9300 . ? C23 C24 1.385(3) . ? C23 H23 0.9300 . ? C24 H24 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 O1 U O1 180.0 . 2_565 ? O1 U O4 90.18(6) . 2_565 ? O1 U O4 89.82(6) 2_565 2_565 ? O1 U O4 89.82(6) . . ? O1 U O4 90.18(6) 2_565 . ? O4 U O4 180.00(9) 2_565 . ? O1 U O2 92.29(6) . . ? O1 U O2 87.71(6) 2_565 . ? O4 U O2 66.29(5) 2_565 . ? O4 U O2 113.71(5) . . ? O1 U O2 87.71(6) . 2_565 ? O1 U O2 92.29(7) 2_565 2_565 ? O4 U O2 113.71(5) 2_565 2_565 ? O4 U O2 66.29(5) . 2_565 ? O2 U O2 180.00(8) . 2_565 ? O1 U O3 91.88(6) . 2_565 ? O1 U O3 88.12(6) 2_565 2_565 ? O4 U O3 65.38(6) 2_565 2_565 ? O4 U O3 114.62(6) . 2_565 ? O2 U O3 131.48(6) . 2_565 ? O2 U O3 48.52(6) 2_565 2_565 ? O1 U O3 88.12(6) . . ? O1 U O3 91.88(6) 2_565 . ? O4 U O3 114.62(6) 2_565 . ? O4 U O3 65.38(6) . . ? O2 U O3 48.52(6) . . ? O2 U O3 131.48(6) 2_565 . ? O3 U O3 180.00(9) 2_565 . ? C13 P1 C1 112.46(8) . . ? C13 P1 C19 108.51(9) . . ? C1 P1 C19 107.54(9) . . ? C13 P1 C7 110.39(9) . . ? C1 P1 C7 109.81(9) . . ? C19 P1 C7 107.99(8) . . ? N1 O2 U 99.67(14) . . ? N1 O3 U 99.11(12) . . ? N2 O4 U 119.69(14) . . ? O3 N1 O2 112.61(18) . . ? O5 N2 O4 114.5(2) . . ? C6 C1 C2 119.60(18) . . ? C6 C1 P1 121.37(14) . . ? C2 C1 P1 119.01(14) . . ? C3 C2 C1 119.46(18) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 120.61(18) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 119.8(2) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C6 C5 C4 120.50(19) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 119.99(18) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C8 C7 C12 120.10(17) . . ? C8 C7 P1 120.35(14) . . ? C12 C7 P1 119.46(14) . . ? C9 C8 C7 119.97(18) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 119.74(19) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.71(19) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 120.21(19) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 119.21(19) . . ? C11 C12 H12 120.4 . . ? C7 C12 H12 120.4 . . ? C14 C13 C18 120.40(19) . . ? C14 C13 P1 119.48(14) . . ? C18 C13 P1 119.57(16) . . ? C15 C14 C13 119.68(19) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 119.9(2) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 120.3(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.3(2) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 119.3(2) . . ? C17 C18 H18 120.3 . . ? C13 C18 H18 120.3 . . ? C20 C19 C24 120.30(17) . . ? C20 C19 P1 120.93(15) . . ? C24 C19 P1 118.68(14) . . ? C19 C20 C21 119.41(19) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C22 C21 C20 120.2(2) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.59(18) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 119.7(2) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C19 119.82(19) . . ? C23 C24 H24 120.1 . . ? C19 C24 H24 120.1 . . ? data_2a _database_code_depnum_ccdc_archive 'CCDC 915622' #TrackingRef 'web_deposit_cif_file_0_P.Thuery_1355410149.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H45 N5 O10 P2 U' _chemical_formula_weight 1211.91 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.1742(9) _cell_length_b 13.8266(8) _cell_length_c 38.374(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.580(3) _cell_angle_gamma 90.00 _cell_volume 10031.6(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 128712 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 28.70 _exptl_crystal_description platelet _exptl_crystal_colour 'translucent light orange' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4800 _exptl_absorpt_coefficient_mu 3.364 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.547 _exptl_absorpt_correction_T_max 0.817 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details 'crystal-to-detector distance 50 mm' _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and seven \w scans with 2\% steps (616 frames)' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 128712 _diffrn_reflns_av_R_equivalents 0.0839 _diffrn_reflns_av_sigmaI/netI 0.0901 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 28.70 _reflns_number_total 12907 _reflns_number_gt 8968 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by Patterson map interpretation and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 times that of the parent atom. The highest residual electron density peak is located near the U atom. 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^)+(0.0621P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 12907 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1361 _refine_ls_wR_factor_gt 0.1238 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.757 _refine_diff_density_min -1.935 _refine_diff_density_rms 0.136 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 U U 0.928568(9) 0.037129(14) 0.612033(5) 0.03718(8) Uani 1 1 d . . . P1 P 0.82633(6) 0.52568(9) 0.24750(3) 0.0307(3) Uani 1 1 d . . . P2 P 0.85437(6) 0.49284(10) 0.53160(3) 0.0341(3) Uani 1 1 d . . . O1 O 1.00618(17) 0.0976(3) 0.63290(10) 0.0534(10) Uani 1 1 d . . . O2 O 0.85130(17) -0.0225(2) 0.59073(10) 0.0433(9) Uani 1 1 d . . . O3 O 0.9299(2) -0.0800(4) 0.66399(11) 0.0644(11) Uani 1 1 d . . . O4 O 0.8777(3) 0.0485(4) 0.66999(13) 0.0708(14) Uani 1 1 d . . . O5 O 0.85954(18) 0.1750(3) 0.61762(9) 0.0476(9) Uani 1 1 d . . . O6 O 0.8334(2) 0.2946(3) 0.64636(10) 0.0605(11) Uani 1 1 d . . . O7 O 0.9212(2) 0.1487(3) 0.55916(10) 0.0595(11) Uani 1 1 d . . . O8 O 0.9750(3) 0.0211(4) 0.55395(12) 0.0675(13) Uani 1 1 d . . . O9 O 1.00362(19) -0.0947(3) 0.61090(11) 0.0559(10) Uani 1 1 d . . . O10 O 1.0190(3) -0.2417(4) 0.60123(12) 0.0743(13) Uani 1 1 d . . . N1 N 0.8986(3) -0.0289(5) 0.68346(14) 0.0622(15) Uani 1 1 d . . . N2 N 0.8794(3) 0.2413(4) 0.64087(11) 0.0511(12) Uani 1 1 d . . . N3 N 0.9535(3) 0.1000(5) 0.53953(14) 0.0673(15) Uani 1 1 d . . . N4 N 0.9768(3) -0.1816(4) 0.60373(13) 0.0614(13) Uani 1 1 d . . . N5 N 0.7232(2) 0.8272(4) 0.66417(11) 0.0477(11) Uani 1 1 d . . . C1 C 0.8626(2) 0.4670(3) 0.21271(11) 0.0322(10) Uani 1 1 d . . . C2 C 0.8988(2) 0.5202(4) 0.19048(11) 0.0341(11) Uani 1 1 d . . . H2 H 0.9072 0.5858 0.1945 0.041 Uiso 1 1 calc R . . C3 C 0.9219(3) 0.4750(4) 0.16251(13) 0.0428(13) Uani 1 1 d . . . H3 H 0.9453 0.5107 0.1475 0.051 Uiso 1 1 calc R . . C4 C 0.9109(2) 0.3781(4) 0.15663(12) 0.0412(12) Uani 1 1 d . . . H4 H 0.9271 0.3484 0.1378 0.049 Uiso 1 1 calc R . . C5 C 0.8754(3) 0.3238(4) 0.17877(13) 0.0426(12) Uani 1 1 d . . . H5 H 0.8677 0.2580 0.1748 0.051 Uiso 1 1 calc R . . C6 C 0.8520(2) 0.3685(4) 0.20652(12) 0.0390(11) Uani 1 1 d . . . H6 H 0.8287 0.3324 0.2215 0.047 Uiso 1 1 calc R . . C7 C 0.8354(2) 0.4420(4) 0.28405(11) 0.0325(10) Uani 1 1 d . . . C8 C 0.8978(2) 0.3924(4) 0.29342(12) 0.0378(11) Uani 1 1 d . . . H8 H 0.9351 0.4030 0.2812 0.045 Uiso 1 1 calc R . . C9 C 0.9051(3) 0.3263(4) 0.32109(12) 0.0394(11) Uani 1 1 d . . . H9 H 0.9474 0.2928 0.3274 0.047 Uiso 1 1 calc R . . C10 C 0.8497(3) 0.3106(4) 0.33909(13) 0.0459(13) Uani 1 1 d . . . H10 H 0.8544 0.2656 0.3574 0.055 Uiso 1 1 calc R . . C11 C 0.7874(3) 0.3613(4) 0.33012(13) 0.0473(14) Uani 1 1 d . . . H11 H 0.7504 0.3503 0.3425 0.057 Uiso 1 1 calc R . . C12 C 0.7789(3) 0.4284(4) 0.30290(12) 0.0382(11) Uani 1 1 d . . . H12 H 0.7372 0.4634 0.2972 0.046 Uiso 1 1 calc R . . C13 C 0.8714(2) 0.6368(3) 0.26003(11) 0.0298(10) Uani 1 1 d . . . C14 C 0.9272(2) 0.6404(4) 0.28863(11) 0.0338(11) Uani 1 1 d . . . H14 H 0.9403 0.5847 0.3017 0.041 Uiso 1 1 calc R . . C15 C 0.9628(2) 0.7256(4) 0.29760(12) 0.0373(11) Uani 1 1 d . . . H15 H 0.9998 0.7275 0.3166 0.045 Uiso 1 1 calc R . . C16 C 0.9432(2) 0.8091(4) 0.27802(13) 0.0412(12) Uani 1 1 d . . . H16 H 0.9673 0.8667 0.2840 0.049 Uiso 1 1 calc R . . C17 C 0.8886(3) 0.8065(4) 0.25000(13) 0.0406(12) Uani 1 1 d . . . H17 H 0.8756 0.8625 0.2371 0.049 Uiso 1 1 calc R . . C18 C 0.8523(2) 0.7203(4) 0.24063(12) 0.0349(11) Uani 1 1 d . . . H18 H 0.8155 0.7189 0.2215 0.042 Uiso 1 1 calc R . . C19 C 0.7355(2) 0.5520(3) 0.23161(12) 0.0328(10) Uani 1 1 d . . . C20 C 0.6980(2) 0.6094(4) 0.25213(13) 0.0411(12) Uani 1 1 d . . . H20 H 0.7206 0.6350 0.2735 0.049 Uiso 1 1 calc R . . C21 C 0.6275(3) 0.6277(4) 0.24050(13) 0.0457(13) Uani 1 1 d . . . H21 H 0.6022 0.6650 0.2543 0.055 Uiso 1 1 calc R . . C22 C 0.5938(3) 0.5913(4) 0.20846(14) 0.0467(13) Uani 1 1 d . . . H22 H 0.5463 0.6049 0.2006 0.056 Uiso 1 1 calc R . . C23 C 0.6303(3) 0.5353(4) 0.18845(14) 0.0471(14) Uani 1 1 d . . . H23 H 0.6081 0.5116 0.1668 0.057 Uiso 1 1 calc R . . C24 C 0.7006(3) 0.5141(4) 0.20051(12) 0.0407(12) Uani 1 1 d . . . H24 H 0.7247 0.4734 0.1873 0.049 Uiso 1 1 calc R . . C25 C 0.8471(3) 0.4143(4) 0.49437(14) 0.0447(13) Uani 1 1 d . . . C26 C 0.7986(4) 0.4351(7) 0.4638(2) 0.096(3) Uani 1 1 d . . . H26 H 0.7730 0.4926 0.4622 0.116 Uiso 1 1 calc R . . C27 C 0.7885(4) 0.3712(7) 0.4362(2) 0.107(3) Uani 1 1 d . . . H27 H 0.7529 0.3825 0.4170 0.129 Uiso 1 1 calc R . . C28 C 0.8295(4) 0.2924(5) 0.43638(16) 0.0641(17) Uani 1 1 d . . . H28 H 0.8205 0.2470 0.4183 0.077 Uiso 1 1 calc R . . C29 C 0.8826(4) 0.2804(5) 0.46246(16) 0.074(2) Uani 1 1 d . . . H29 H 0.9147 0.2306 0.4613 0.089 Uiso 1 1 calc R . . C30 C 0.8913(3) 0.3414(5) 0.49183(15) 0.0625(17) Uani 1 1 d . . . H30 H 0.9289 0.3308 0.5101 0.075 Uiso 1 1 calc R . . C31 C 0.9325(2) 0.4638(3) 0.56246(12) 0.0309(10) Uani 1 1 d . . . C32 C 0.9413(2) 0.3719(4) 0.57749(12) 0.0355(11) Uani 1 1 d . . . H32 H 0.9061 0.3254 0.5719 0.043 Uiso 1 1 calc R . . C33 C 1.0023(3) 0.3499(4) 0.60056(12) 0.0390(12) Uani 1 1 d . . . H33 H 1.0083 0.2883 0.6103 0.047 Uiso 1 1 calc R . . C34 C 1.0544(2) 0.4186(4) 0.60932(12) 0.0398(12) Uani 1 1 d . . . H34 H 1.0953 0.4034 0.6250 0.048 Uiso 1 1 calc R . . C35 C 1.0459(3) 0.5088(4) 0.59496(13) 0.0412(12) Uani 1 1 d . . . H35 H 1.0811 0.5550 0.6009 0.049 Uiso 1 1 calc R . . C36 C 0.9856(3) 0.5323(4) 0.57169(13) 0.0387(12) Uani 1 1 d . . . H36 H 0.9803 0.5941 0.5621 0.046 Uiso 1 1 calc R . . C37 C 0.7772(3) 0.4811(4) 0.55238(14) 0.0387(11) Uani 1 1 d . . . C38 C 0.7841(3) 0.4598(4) 0.58824(15) 0.0515(16) Uani 1 1 d . . . H38 H 0.8287 0.4537 0.6019 0.062 Uiso 1 1 calc R . . C39 C 0.7242(3) 0.4479(5) 0.60331(16) 0.0566(17) Uani 1 1 d . . . H39 H 0.7287 0.4320 0.6271 0.068 Uiso 1 1 calc R . . C40 C 0.6571(3) 0.4594(4) 0.58354(18) 0.0525(15) Uani 1 1 d . . . H40 H 0.6171 0.4527 0.5941 0.063 Uiso 1 1 calc R . . C41 C 0.6506(3) 0.4806(5) 0.54826(19) 0.070(2) Uani 1 1 d . . . H41 H 0.6059 0.4878 0.5347 0.085 Uiso 1 1 calc R . . C42 C 0.7103(3) 0.4912(6) 0.53275(18) 0.077(2) Uani 1 1 d . . . H42 H 0.7054 0.5055 0.5088 0.092 Uiso 1 1 calc R . . C43 C 0.8626(2) 0.6153(4) 0.51764(12) 0.0350(11) Uani 1 1 d . . . C44 C 0.8443(3) 0.6912(4) 0.53790(13) 0.0432(12) Uani 1 1 d . . . H44 H 0.8190 0.6795 0.5561 0.052 Uiso 1 1 calc R . . C45 C 0.8637(3) 0.7834(4) 0.53091(15) 0.0513(14) Uani 1 1 d . . . H45 H 0.8511 0.8341 0.5445 0.062 Uiso 1 1 calc R . . C46 C 0.9011(3) 0.8029(5) 0.50443(16) 0.0557(15) Uani 1 1 d . . . H46 H 0.9150 0.8659 0.5006 0.067 Uiso 1 1 calc R . . C47 C 0.9182(3) 0.7288(5) 0.48338(15) 0.0588(16) Uani 1 1 d . . . H47 H 0.9424 0.7422 0.4648 0.071 Uiso 1 1 calc R . . C48 C 0.8998(3) 0.6350(4) 0.48970(13) 0.0446(13) Uani 1 1 d . . . H48 H 0.9119 0.5849 0.4756 0.054 Uiso 1 1 calc R . . C49 C 0.7447(3) 0.8603(5) 0.63505(14) 0.0498(14) Uani 1 1 d . . . H49 H 0.7694 0.9184 0.6363 0.060 Uiso 1 1 calc R . . C50 C 0.7320(3) 0.8118(5) 0.60309(14) 0.0498(14) Uani 1 1 d . . . H50 H 0.7481 0.8369 0.5834 0.060 Uiso 1 1 calc R . . C51 C 0.6957(3) 0.7277(4) 0.60089(14) 0.0514(14) Uani 1 1 d . . . H51 H 0.6870 0.6938 0.5797 0.062 Uiso 1 1 calc R . . C52 C 0.6719(3) 0.6928(4) 0.63031(15) 0.0482(13) Uani 1 1 d . . . H52 H 0.6461 0.6357 0.6296 0.058 Uiso 1 1 calc R . . C53 C 0.6880(3) 0.7467(4) 0.66132(14) 0.0462(13) Uani 1 1 d . . . H53 H 0.6724 0.7233 0.6814 0.055 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 U 0.02797(10) 0.03964(14) 0.04316(12) 0.00435(8) 0.00363(7) -0.00286(8) P1 0.0293(6) 0.0354(7) 0.0266(5) 0.0003(5) 0.0027(4) -0.0034(5) P2 0.0313(6) 0.0340(7) 0.0358(6) -0.0043(6) 0.0019(5) 0.0034(6) O1 0.0374(19) 0.055(3) 0.064(2) 0.005(2) -0.0026(17) -0.0072(18) O2 0.0322(17) 0.041(2) 0.056(2) -0.0034(17) 0.0046(15) -0.0097(15) O3 0.053(2) 0.081(3) 0.060(3) 0.014(2) 0.012(2) 0.007(2) O4 0.071(3) 0.087(4) 0.059(3) 0.002(2) 0.025(2) 0.000(3) O5 0.047(2) 0.051(2) 0.0424(19) -0.0096(18) -0.0009(16) -0.0001(18) O6 0.077(3) 0.052(3) 0.057(2) -0.012(2) 0.021(2) -0.006(2) O7 0.087(3) 0.045(2) 0.051(2) 0.0027(19) 0.022(2) 0.001(2) O8 0.076(3) 0.072(3) 0.065(3) 0.012(2) 0.041(2) 0.020(3) O9 0.046(2) 0.048(3) 0.076(3) 0.008(2) 0.0162(19) 0.007(2) O10 0.082(3) 0.062(3) 0.078(3) 0.005(2) 0.014(2) 0.025(3) N1 0.054(3) 0.079(5) 0.053(3) 0.014(3) 0.009(2) 0.011(3) N2 0.058(3) 0.055(3) 0.040(2) -0.002(2) 0.007(2) -0.014(3) N3 0.079(4) 0.066(4) 0.063(3) 0.005(3) 0.030(3) -0.013(3) N4 0.066(3) 0.048(3) 0.070(3) 0.003(3) 0.009(3) 0.003(3) N5 0.043(2) 0.058(3) 0.041(2) -0.002(2) 0.0048(19) 0.000(2) C1 0.030(2) 0.039(3) 0.028(2) -0.001(2) 0.0070(17) -0.002(2) C2 0.038(2) 0.035(3) 0.031(2) 0.000(2) 0.0074(19) -0.005(2) C3 0.039(3) 0.055(4) 0.035(3) 0.008(2) 0.010(2) 0.000(3) C4 0.038(3) 0.052(4) 0.034(2) -0.010(2) 0.004(2) 0.003(3) C5 0.046(3) 0.037(3) 0.046(3) -0.007(2) 0.009(2) -0.002(2) C6 0.043(3) 0.036(3) 0.039(3) 0.002(2) 0.009(2) -0.007(2) C7 0.036(2) 0.034(3) 0.026(2) -0.0015(19) 0.0009(18) -0.006(2) C8 0.035(2) 0.044(3) 0.035(2) 0.007(2) 0.0065(19) -0.004(2) C9 0.044(3) 0.037(3) 0.035(2) 0.002(2) 0.001(2) -0.004(2) C10 0.058(3) 0.043(3) 0.035(3) 0.009(2) 0.000(2) -0.015(3) C11 0.050(3) 0.059(4) 0.035(3) 0.005(2) 0.012(2) -0.014(3) C12 0.036(2) 0.042(3) 0.037(3) -0.002(2) 0.006(2) -0.008(2) C13 0.029(2) 0.032(3) 0.029(2) -0.0021(19) 0.0066(17) -0.003(2) C14 0.033(2) 0.040(3) 0.028(2) -0.003(2) 0.0025(18) -0.001(2) C15 0.027(2) 0.048(3) 0.037(2) -0.011(2) 0.0034(19) -0.002(2) C16 0.035(3) 0.041(3) 0.050(3) -0.013(2) 0.014(2) -0.007(2) C17 0.044(3) 0.036(3) 0.041(3) 0.004(2) 0.007(2) 0.001(2) C18 0.035(2) 0.039(3) 0.030(2) 0.003(2) 0.0030(18) -0.003(2) C19 0.030(2) 0.035(3) 0.033(2) 0.004(2) 0.0039(18) -0.002(2) C20 0.037(3) 0.046(3) 0.039(3) -0.003(2) 0.003(2) -0.001(2) C21 0.035(3) 0.054(4) 0.048(3) 0.001(3) 0.006(2) -0.001(3) C22 0.032(2) 0.047(3) 0.057(3) 0.005(3) -0.006(2) -0.002(2) C23 0.043(3) 0.050(4) 0.042(3) -0.008(3) -0.010(2) -0.010(3) C24 0.047(3) 0.044(3) 0.030(2) 0.000(2) 0.001(2) 0.000(3) C25 0.041(3) 0.039(3) 0.050(3) -0.014(2) -0.005(2) 0.003(2) C26 0.065(4) 0.125(7) 0.086(5) -0.054(5) -0.028(4) 0.037(5) C27 0.071(5) 0.149(9) 0.087(5) -0.073(6) -0.031(4) 0.026(5) C28 0.089(5) 0.055(4) 0.047(3) -0.014(3) 0.007(3) -0.012(4) C29 0.100(5) 0.075(5) 0.046(3) -0.016(3) 0.006(3) 0.023(4) C30 0.063(4) 0.077(5) 0.045(3) -0.015(3) 0.001(3) 0.018(4) C31 0.027(2) 0.035(3) 0.031(2) 0.000(2) 0.0056(17) 0.000(2) C32 0.036(2) 0.034(3) 0.039(3) -0.001(2) 0.011(2) -0.001(2) C33 0.041(3) 0.044(3) 0.033(2) 0.004(2) 0.010(2) 0.003(2) C34 0.034(2) 0.052(3) 0.032(2) 0.002(2) 0.0020(19) 0.005(2) C35 0.032(2) 0.052(3) 0.039(3) -0.007(2) 0.004(2) -0.004(2) C36 0.040(3) 0.034(3) 0.039(3) -0.002(2) 0.001(2) 0.001(2) C37 0.033(2) 0.034(3) 0.049(3) 0.002(2) 0.006(2) 0.006(2) C38 0.037(3) 0.072(4) 0.045(3) -0.021(3) 0.007(2) -0.001(3) C39 0.049(3) 0.076(5) 0.049(3) -0.012(3) 0.019(3) 0.000(3) C40 0.041(3) 0.037(3) 0.084(4) -0.002(3) 0.025(3) -0.001(2) C41 0.036(3) 0.087(5) 0.089(5) 0.042(4) 0.011(3) 0.003(3) C42 0.036(3) 0.119(6) 0.075(4) 0.055(5) 0.008(3) 0.006(4) C43 0.033(2) 0.036(3) 0.034(2) -0.001(2) 0.0027(19) 0.006(2) C44 0.053(3) 0.039(3) 0.041(3) -0.003(2) 0.017(2) 0.006(3) C45 0.061(4) 0.036(3) 0.058(3) -0.007(3) 0.013(3) 0.009(3) C46 0.058(4) 0.041(3) 0.069(4) 0.010(3) 0.010(3) 0.005(3) C47 0.063(4) 0.063(4) 0.053(3) 0.026(3) 0.019(3) 0.020(3) C48 0.055(3) 0.042(3) 0.037(3) 0.003(2) 0.009(2) 0.017(3) C49 0.036(3) 0.056(4) 0.059(3) -0.009(3) 0.012(2) -0.009(3) C50 0.052(3) 0.059(4) 0.041(3) 0.004(3) 0.016(2) -0.003(3) C51 0.051(3) 0.059(4) 0.043(3) -0.008(3) 0.006(2) 0.003(3) C52 0.038(3) 0.043(3) 0.065(4) 0.003(3) 0.011(2) -0.003(3) C53 0.044(3) 0.047(4) 0.050(3) 0.009(3) 0.019(2) 0.014(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 U O2 1.772(3) . ? U O1 1.777(3) . ? U O9 2.327(4) . ? U O5 2.350(4) . ? U O7 2.534(4) . ? U O8 2.543(4) . ? U O3 2.565(4) . ? U O4 2.577(5) . ? P1 C19 1.784(5) . ? P1 C13 1.788(5) . ? P1 C1 1.799(4) . ? P1 C7 1.804(5) . ? P2 C25 1.781(5) . ? P2 C43 1.791(5) . ? P2 C31 1.793(5) . ? P2 C37 1.802(5) . ? O3 N1 1.252(7) . ? O4 N1 1.226(6) . ? O5 N2 1.292(5) . ? O6 N2 1.195(6) . ? O7 N3 1.250(6) . ? O8 N3 1.260(7) . ? O9 N4 1.319(6) . ? O10 N4 1.175(6) . ? N5 C53 1.296(7) . ? N5 C49 1.335(7) . ? C1 C6 1.391(6) . ? C1 C2 1.396(6) . ? C2 C3 1.377(7) . ? C2 H2 0.9300 . ? C3 C4 1.369(7) . ? C3 H3 0.9300 . ? C4 C5 1.393(7) . ? C4 H4 0.9300 . ? C5 C6 1.370(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.374(6) . ? C7 C12 1.411(6) . ? C8 C9 1.390(6) . ? C8 H8 0.9300 . ? C9 C10 1.377(7) . ? C9 H9 0.9300 . ? C10 C11 1.380(7) . ? C10 H10 0.9300 . ? C11 C12 1.386(7) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.390(6) . ? C13 C14 1.400(6) . ? C14 C15 1.376(7) . ? C14 H14 0.9300 . ? C15 C16 1.395(7) . ? C15 H15 0.9300 . ? C16 C17 1.371(7) . ? C16 H16 0.9300 . ? C17 C18 1.396(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.372(7) . ? C19 C20 1.398(7) . ? C20 C21 1.375(6) . ? C20 H20 0.9300 . ? C21 C22 1.385(7) . ? C21 H21 0.9300 . ? C22 C23 1.363(7) . ? C22 H22 0.9300 . ? C23 C24 1.381(7) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.331(8) . ? C25 C26 1.401(8) . ? C26 C27 1.369(9) . ? C26 H26 0.9300 . ? C27 C28 1.342(10) . ? C27 H27 0.9300 . ? C28 C29 1.313(9) . ? C28 H28 0.9300 . ? C29 C30 1.395(8) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.392(7) . ? C31 C32 1.395(6) . ? C32 C33 1.378(6) . ? C32 H32 0.9300 . ? C33 C34 1.378(7) . ? C33 H33 0.9300 . ? C34 C35 1.362(8) . ? C34 H34 0.9300 . ? C35 C36 1.376(7) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C42 1.382(7) . ? C37 C38 1.392(8) . ? C38 C39 1.380(8) . ? C38 H38 0.9300 . ? C39 C40 1.388(8) . ? C39 H39 0.9300 . ? C40 C41 1.371(9) . ? C40 H40 0.9300 . ? C41 C42 1.383(8) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.385(7) . ? C43 C48 1.409(7) . ? C44 C45 1.367(7) . ? C44 H44 0.9300 . ? C45 C46 1.364(8) . ? C45 H45 0.9300 . ? C46 C47 1.378(8) . ? C46 H46 0.9300 . ? C47 C48 1.376(8) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.383(7) . ? C49 H49 0.9300 . ? C50 C51 1.350(8) . ? C50 H50 0.9300 . ? C51 C52 1.374(8) . ? C51 H51 0.9300 . ? C52 C53 1.395(8) . ? C52 H52 0.9300 . ? C53 H53 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 U O1 179.28(17) . . ? O2 U O9 95.71(16) . . ? O1 U O9 84.42(16) . . ? O2 U O5 88.78(14) . . ? O1 U O5 91.12(15) . . ? O9 U O5 174.95(13) . . ? O2 U O7 88.99(15) . . ? O1 U O7 90.32(16) . . ? O9 U O7 114.47(13) . . ? O5 U O7 67.79(13) . . ? O2 U O8 86.72(17) . . ? O1 U O8 92.69(17) . . ? O9 U O8 66.91(14) . . ? O5 U O8 115.78(14) . . ? O7 U O8 48.12(14) . . ? O2 U O3 87.98(15) . . ? O1 U O3 92.72(16) . . ? O9 U O3 66.04(14) . . ? O5 U O3 111.96(14) . . ? O7 U O3 176.96(14) . . ? O8 U O3 131.79(15) . . ? O2 U O4 91.09(16) . . ? O1 U O4 89.50(17) . . ? O9 U O4 112.81(16) . . ? O5 U O4 64.68(15) . . ? O7 U O4 132.46(16) . . ? O8 U O4 177.74(15) . . ? O3 U O4 47.48(16) . . ? C19 P1 C13 108.5(2) . . ? C19 P1 C1 108.3(2) . . ? C13 P1 C1 111.0(2) . . ? C19 P1 C7 111.0(2) . . ? C13 P1 C7 111.2(2) . . ? C1 P1 C7 106.8(2) . . ? C25 P2 C43 109.6(2) . . ? C25 P2 C31 109.8(2) . . ? C43 P2 C31 107.7(2) . . ? C25 P2 C37 109.9(3) . . ? C43 P2 C37 109.8(2) . . ? C31 P2 C37 110.2(2) . . ? N1 O3 U 99.4(4) . . ? N1 O4 U 99.6(4) . . ? N2 O5 U 122.2(3) . . ? N3 O7 U 100.8(4) . . ? N3 O8 U 100.0(3) . . ? N4 O9 U 119.8(3) . . ? O4 N1 O3 113.4(5) . . ? O6 N2 O5 114.8(4) . . ? O7 N3 O8 111.1(5) . . ? O10 N4 O9 114.3(5) . . ? C53 N5 C49 116.9(5) . . ? C6 C1 C2 119.0(4) . . ? C6 C1 P1 120.3(4) . . ? C2 C1 P1 120.6(4) . . ? C3 C2 C1 119.6(5) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 120.8(5) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.3(5) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 119.1(5) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C5 C6 C1 121.2(5) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? C8 C7 C12 120.5(4) . . ? C8 C7 P1 119.4(4) . . ? C12 C7 P1 120.1(4) . . ? C7 C8 C9 120.1(4) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 119.9(5) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.2(5) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 121.1(5) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C7 118.2(5) . . ? C11 C12 H12 120.9 . . ? C7 C12 H12 120.9 . . ? C18 C13 C14 119.2(4) . . ? C18 C13 P1 119.8(3) . . ? C14 C13 P1 120.9(4) . . ? C15 C14 C13 120.6(4) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.7(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 120.2(5) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.5(5) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C13 C18 C17 119.7(4) . . ? C13 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C24 C19 C20 118.9(4) . . ? C24 C19 P1 121.8(4) . . ? C20 C19 P1 119.2(4) . . ? C21 C20 C19 119.5(5) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C22 120.6(5) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 119.9(5) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 119.7(5) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C19 C24 C23 121.2(5) . . ? C19 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C30 C25 C26 115.9(5) . . ? C30 C25 P2 123.7(4) . . ? C26 C25 P2 119.9(5) . . ? C27 C26 C25 120.3(7) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 120.8(7) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C29 C28 C27 119.1(6) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C28 C29 C30 120.8(7) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C25 C30 C29 121.7(6) . . ? C25 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C36 C31 C32 118.8(4) . . ? C36 C31 P2 120.7(4) . . ? C32 C31 P2 120.5(4) . . ? C33 C32 C31 119.8(5) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 120.5(5) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C35 C34 C33 119.9(4) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.6(5) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C31 120.3(5) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C42 C37 C38 119.2(5) . . ? C42 C37 P2 120.4(4) . . ? C38 C37 P2 120.4(4) . . ? C39 C38 C37 119.4(5) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C38 C39 C40 121.2(6) . . ? C38 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? C41 C40 C39 119.2(5) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C40 C41 C42 120.1(6) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C37 C42 C41 120.9(6) . . ? C37 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C44 C43 C48 119.2(5) . . ? C44 C43 P2 120.3(4) . . ? C48 C43 P2 119.4(4) . . ? C45 C44 C43 119.6(5) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C46 C45 C44 121.6(5) . . ? C46 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C45 C46 C47 119.8(6) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C48 C47 C46 120.3(5) . . ? C48 C47 H47 119.9 . . ? C46 C47 H47 119.9 . . ? C47 C48 C43 119.5(5) . . ? C47 C48 H48 120.2 . . ? C43 C48 H48 120.2 . . ? N5 C49 C50 122.9(5) . . ? N5 C49 H49 118.6 . . ? C50 C49 H49 118.6 . . ? C51 C50 C49 119.1(5) . . ? C51 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? C50 C51 C52 119.3(5) . . ? C50 C51 H51 120.4 . . ? C52 C51 H51 120.4 . . ? C51 C52 C53 117.2(5) . . ? C51 C52 H52 121.4 . . ? C53 C52 H52 121.4 . . ? N5 C53 C52 124.7(5) . . ? N5 C53 H53 117.7 . . ? C52 C53 H53 117.7 . . ?