# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Zhen-Gang Sun' _publ_contact_author_email szg188@163.com loop_ _publ_author_name K.Chen Z.-G.Sun C.-Q.Jiao C.Li C.-L.Wang Y.Zhu D.-P.Dong ; Y.Zhao ; J.Zhu S.-H.Sun M.-J.Zheng H.Tian W.Chu data_szg166 _database_code_depnum_ccdc_archive 'CCDC 849251' #TrackingRef 'szg166.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H61 La3 N3 O31 P3' _chemical_formula_weight 1553.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.2688(15) _cell_length_b 15.3552(16) _cell_length_c 15.403(3) _cell_angle_alpha 106.787(2) _cell_angle_beta 117.059(2) _cell_angle_gamma 103.1950(10) _cell_volume 2791.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3411 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 26.92 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 2.433 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6444 _exptl_absorpt_correction_T_max 0.7491 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Smart Apex II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15835 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0788 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 26.50 _reflns_number_total 11253 _reflns_number_gt 8385 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0955P)^2^+50.1940P] 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 11253 _refine_ls_number_parameters 694 _refine_ls_number_restraints 3421 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.2004 _refine_ls_wR_factor_gt 0.1802 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.05702(5) 0.19746(4) 0.36576(5) 0.01471(16) Uani 1 1 d . . . La2 La 0.32161(5) 0.18393(4) 0.61665(5) 0.01515(17) Uani 1 1 d . . . La3 La -0.08488(5) 0.14639(5) 0.56324(5) 0.01552(17) Uani 1 1 d . . . P1 P 0.1259(2) 0.0168(2) 0.3090(2) 0.0172(6) Uani 1 1 d . . . P2 P 0.1967(2) 0.3066(2) 0.6756(2) 0.0171(6) Uani 1 1 d . . . P3 P -0.1175(2) -0.0251(2) 0.3561(2) 0.0138(5) Uani 1 1 d . . . O1 O 0.0236(7) 0.0253(7) 0.2338(8) 0.0319(14) Uani 1 1 d U . . O2 O 0.1867(7) 0.1083(7) 0.4215(8) 0.0309(14) Uani 1 1 d U . . O3 O 0.1138(7) -0.0810(7) 0.3150(8) 0.0315(14) Uani 1 1 d U . . O4 O 0.7125(8) 0.0967(7) 0.4612(8) 0.0377(15) Uani 1 1 d U . . O5 O 0.6353(7) -0.0447(7) 0.4608(8) 0.0325(14) Uani 1 1 d U . . O6 O 0.2792(7) 0.2777(7) 0.7498(8) 0.0305(14) Uani 1 1 d U . . O7 O 0.1753(7) 0.2560(7) 0.5624(8) 0.0317(14) Uani 1 1 d U . . O8 O 0.0969(7) 0.2926(7) 0.6772(8) 0.0321(14) Uani 1 1 d U . . O9 O 0.1304(8) 0.7432(7) 0.5311(8) 0.0353(15) Uani 1 1 d U . . O10 O -0.0034(7) 0.6781(7) 0.5495(8) 0.0317(14) Uani 1 1 d U . . O11 O -0.0571(7) 0.0889(7) 0.4026(8) 0.0294(13) Uani 1 1 d U . . O12 O -0.0469(7) -0.0803(7) 0.3712(8) 0.0314(14) Uani 1 1 d U . . O13 O -0.1822(7) -0.0391(7) 0.4072(8) 0.0294(13) Uani 1 1 d U . . O14 O -0.2766(12) -0.5072(10) -0.1117(13) 0.085(3) Uani 1 1 d U . . H21A H -0.2933 -0.5247 -0.1767 0.103 Uiso 1 1 d RU . . O15 O -0.4198(11) -0.5319(10) -0.1030(12) 0.075(3) Uani 1 1 d U . . O16 O 0.5251(8) 0.2721(7) 0.7920(9) 0.0409(16) Uani 1 1 d U . . O17 O 0.4166(8) 0.1407(7) 0.7755(8) 0.0389(15) Uani 1 1 d U . . O18 O 0.9639(8) 0.2345(7) 1.1956(9) 0.0403(16) Uani 1 1 d U . . O19 O 0.8516(8) 0.1408(7) 1.2166(9) 0.0409(16) Uani 1 1 d U . . O20 O 0.4070(8) 0.3612(7) 0.6407(8) 0.0384(15) Uani 1 1 d U . . O21 O 0.4439(8) 0.2493(7) 0.5558(8) 0.0382(15) Uani 1 1 d U . . O22 O 0.7980(8) 0.7412(7) 0.6757(8) 0.0376(15) Uani 1 1 d U . . O23 O 0.8161(8) 0.6246(7) 0.5722(8) 0.0381(15) Uani 1 1 d U . . O24 O -0.0968(9) 0.2821(8) 0.6954(9) 0.050(2) Uani 1 1 d U . . H24C H -0.0380 0.3350 0.7338 0.076 Uiso 1 1 d RU . . H24D H -0.1493 0.2948 0.6587 0.076 Uiso 1 1 d RU . . O1W O 0.4784(9) 0.8081(9) 0.8126(10) 0.0600(18) Uani 1 1 d U . . H1WA H 0.4505 0.8450 0.7890 0.090 Uiso 1 1 d RU . . H1WB H 0.4878 0.8193 0.8743 0.090 Uiso 1 1 d RU . . O2W O 0.3356(8) 0.9028(8) 0.7559(9) 0.0473(17) Uani 1 1 d U . . H2WA H 0.2928 0.9238 0.7186 0.071 Uiso 1 1 d RU . . H2WB H 0.3415 0.9178 0.8166 0.071 Uiso 1 1 d RU . . O3W O 0.9102(13) 0.9836(13) 0.0182(13) 0.099(4) Uani 1 1 d U . . H3WC H 0.9375 1.0259 0.0834 0.119 Uiso 1 1 d RU . . H3WB H 0.8873 0.9244 0.0110 0.149 Uiso 1 1 d RU . . O4W O 0.7197(10) 0.9401(9) 0.9418(10) 0.0627(18) Uani 1 1 d U . . H4WA H 0.6611 0.9412 0.9337 0.094 Uiso 1 1 d RU . . H4WB H 0.7300 0.9587 0.8991 0.094 Uiso 1 1 d RU . . O5W O 0.9445(9) 0.4921(9) 0.7489(10) 0.0630(18) Uani 1 1 d U . . H5WA H 0.8907 0.5038 0.7132 0.094 Uiso 1 1 d RU . . H5WB H 0.9297 0.4588 0.7797 0.094 Uiso 1 1 d RU . . O6W O 0.7361(10) 0.3068(9) 0.7478(10) 0.0647(18) Uani 1 1 d U . . H6WA H 0.6782 0.3117 0.7085 0.097 Uiso 1 1 d RU . . H6WB H 0.7207 0.2576 0.7611 0.097 Uiso 1 1 d RU . . O7W O 0.9144(10) 0.2966(9) 0.8831(10) 0.0655(19) Uani 1 1 d U . . H7WC H 0.9661 0.3489 0.9413 0.079 Uiso 1 1 d RU . . H7WB H 0.9074 0.2460 0.8958 0.098 Uiso 1 1 d RU . . N1 N 0.3210(7) 0.0403(7) 0.3233(8) 0.019(2) Uani 1 1 d . . . H3C H 0.3376 0.0549 0.3914 0.022 Uiso 1 1 d RU . . N2 N 0.2116(7) 0.4865(7) 0.6638(8) 0.019(2) Uani 1 1 d . . . H2C H 0.1587 0.4378 0.5958 0.022 Uiso 1 1 d RU . . N3 N -0.2480(8) -0.1817(7) 0.1408(8) 0.024(2) Uani 1 1 d . . . H1C H -0.2542 -0.2141 0.1794 0.028 Uiso 1 1 d RU . . C1 C 0.2112(9) 0.0405(10) 0.2585(10) 0.025(2) Uani 1 1 d U . . H28A H 0.1728 -0.0101 0.1834 0.030 Uiso 1 1 calc RU . . H28B H 0.2221 0.1051 0.2582 0.030 Uiso 1 1 calc RU . . C2 C 0.4050(9) 0.1183(9) 0.3319(11) 0.027(2) Uani 1 1 d U . . H30A H 0.4049 0.1829 0.3631 0.033 Uiso 1 1 calc RU . . H30B H 0.3891 0.1044 0.2594 0.033 Uiso 1 1 calc RU . . C3 C 0.5173(10) 0.1227(9) 0.4035(11) 0.026(2) Uani 1 1 d U . . H32A H 0.5706 0.1727 0.4050 0.031 Uiso 1 1 calc RU . . H32B H 0.5360 0.1431 0.4777 0.031 Uiso 1 1 calc RU . . C4 C 0.5210(9) 0.0222(9) 0.3617(11) 0.023(2) Uani 1 1 d U . . H33A H 0.5085 0.0071 0.2896 0.028 Uiso 1 1 calc RU . . C5 C 0.4275(9) -0.0609(9) 0.3446(11) 0.024(2) Uani 1 1 d U . . H31A H 0.4251 -0.1255 0.3085 0.029 Uiso 1 1 calc RU . . H31B H 0.4418 -0.0524 0.4154 0.029 Uiso 1 1 calc RU . . C6 C 0.3183(10) -0.0606(9) 0.2771(11) 0.028(2) Uani 1 1 d U . . H29A H 0.2983 -0.0797 0.2026 0.034 Uiso 1 1 calc RU . . H29B H 0.2637 -0.1096 0.2752 0.034 Uiso 1 1 calc RU . . C7 C 0.6308(9) 0.0247(8) 0.4332(10) 0.020(2) Uani 1 1 d U . . C8 C 0.2752(9) 0.4406(8) 0.7279(10) 0.023(2) Uani 1 1 d U . . H2A H 0.2993 0.4756 0.8036 0.028 Uiso 1 1 calc RU . . H2B H 0.3391 0.4496 0.7258 0.028 Uiso 1 1 calc RU . . C9 C 0.1594(10) 0.5308(9) 0.7168(10) 0.024(2) Uani 1 1 d U . . H4A H 0.2151 0.5815 0.7913 0.029 Uiso 1 1 calc RU . . H4B H 0.1123 0.4786 0.7193 0.029 Uiso 1 1 calc RU . . C10 C 0.0935(9) 0.5776(9) 0.6532(10) 0.022(2) Uani 1 1 d U . . H6A H 0.0308 0.5246 0.5831 0.026 Uiso 1 1 calc RU . . H6B H 0.0674 0.6114 0.6931 0.026 Uiso 1 1 calc RU . . C11 C 0.1572(9) 0.6512(9) 0.6344(10) 0.022(2) Uani 1 1 d U . . H7A H 0.2142 0.7076 0.7065 0.026 Uiso 1 1 calc RU . . C12 C 0.2145(9) 0.6072(9) 0.5868(10) 0.021(2) Uani 1 1 d U . . H5A H 0.1611 0.5546 0.5126 0.026 Uiso 1 1 calc RU . . H5B H 0.2620 0.6591 0.5844 0.026 Uiso 1 1 calc RU . . C13 C 0.2806(9) 0.5642(9) 0.6558(10) 0.023(2) Uani 1 1 d U . . H3A H 0.3150 0.5352 0.6232 0.028 Uiso 1 1 calc RU . . H3B H 0.3373 0.6177 0.7285 0.028 Uiso 1 1 calc RU . . C14 C 0.0900(9) 0.6947(9) 0.5658(10) 0.022(2) Uani 1 1 d U . . C15 C -0.2121(10) -0.0736(9) 0.2073(10) 0.025(2) Uani 1 1 d U . . H1A H -0.2758 -0.0616 0.1938 0.030 Uiso 1 1 calc RU . . H1B H -0.1776 -0.0354 0.1825 0.030 Uiso 1 1 calc RU . . C16 C -0.1671(12) -0.2002(10) 0.1174(11) 0.035(3) Uani 1 1 d U . . H23A H -0.0957 -0.1665 0.1851 0.042 Uiso 1 1 calc RU . . H23B H -0.1646 -0.1721 0.0692 0.042 Uiso 1 1 calc RU . . C17 C -0.1959(13) -0.3101(11) 0.0650(13) 0.047(3) Uani 1 1 d U . . H25A H -0.1929 -0.3371 0.1155 0.057 Uiso 1 1 calc RU . . H25B H -0.1432 -0.3198 0.0491 0.057 Uiso 1 1 calc RU . . C18 C -0.3111(14) -0.3677(12) -0.0423(13) 0.050(3) Uani 1 1 d U . . H27A H -0.3091 -0.3450 -0.0950 0.061 Uiso 1 1 calc RU . . C19 C -0.3932(14) -0.3419(12) -0.0230(14) 0.054(3) Uani 1 1 d U . . H26A H -0.4042 -0.3715 0.0210 0.065 Uiso 1 1 calc RU . . H26B H -0.4621 -0.3704 -0.0926 0.065 Uiso 1 1 calc RU . . C20 C -0.3547(12) -0.2266(11) 0.0360(12) 0.043(3) Uani 1 1 d U . . H24A H -0.3490 -0.1972 -0.0102 0.051 Uiso 1 1 calc RU . . H24B H -0.4073 -0.2125 0.0495 0.051 Uiso 1 1 calc RU . . C21 C -0.3394(16) -0.4797(14) -0.0897(15) 0.062(4) Uani 1 1 d U . . C22 C 0.5093(10) 0.2076(10) 0.8238(11) 0.028(2) Uani 1 1 d U . . C23 C 0.6030(10) 0.2066(10) 0.9155(11) 0.031(2) Uani 1 1 d U . . C24 C 0.7083(10) 0.2700(10) 0.9622(11) 0.034(2) Uani 1 1 d U . . H11A H 0.7220 0.3170 0.9378 0.041 Uiso 1 1 calc RU . . C25 C 0.7945(11) 0.2661(11) 1.0441(11) 0.036(3) Uani 1 1 d U . . H13A H 0.8649 0.3123 1.0768 0.043 Uiso 1 1 calc RU . . C26 C 0.7765(10) 0.1941(10) 1.0776(11) 0.029(2) Uani 1 1 d U . . C27 C 0.6712(10) 0.1302(10) 1.0327(11) 0.035(2) Uani 1 1 d U . . H37A H 0.6581 0.0853 1.0596 0.042 Uiso 1 1 calc RU . . C28 C 0.5843(11) 0.1322(11) 0.9479(11) 0.037(3) Uani 1 1 d U . . H12A H 0.5143 0.0842 0.9129 0.044 Uiso 1 1 calc RU . . C29 C 0.8710(10) 0.1895(10) 1.1690(11) 0.030(2) Uani 1 1 d U . . C30 C 0.4589(11) 0.3370(9) 0.6002(11) 0.030(2) Uani 1 1 d U . . C31 C 0.5382(10) 0.4179(9) 0.6049(11) 0.026(2) Uani 1 1 d U . . C32 C 0.5507(10) 0.5186(9) 0.6464(11) 0.028(2) Uani 1 1 d U . . H18A H 0.5086 0.5352 0.6712 0.033 Uiso 1 1 calc RU . . C33 C 0.6262(10) 0.5918(9) 0.6496(11) 0.030(2) Uani 1 1 d U . . H19A H 0.6311 0.6567 0.6731 0.036 Uiso 1 1 calc RU . . C34 C 0.6938(10) 0.5721(9) 0.6195(11) 0.030(2) Uani 1 1 d U . . C35 C 0.6837(11) 0.4727(9) 0.5819(11) 0.031(2) Uani 1 1 d U . . H22A H 0.7287 0.4576 0.5607 0.037 Uiso 1 1 calc RU . . C36 C 0.6079(10) 0.3970(9) 0.5760(11) 0.030(2) Uani 1 1 d U . . H35A H 0.6037 0.3322 0.5527 0.036 Uiso 1 1 calc RU . . C37 C 0.7738(10) 0.6498(9) 0.6223(11) 0.026(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0116(3) 0.0165(3) 0.0192(3) 0.0115(3) 0.0083(3) 0.0070(2) La2 0.0110(3) 0.0164(3) 0.0201(3) 0.0116(3) 0.0078(3) 0.0064(2) La3 0.0136(3) 0.0162(3) 0.0205(3) 0.0107(3) 0.0097(3) 0.0084(2) P1 0.0151(13) 0.0211(14) 0.0215(15) 0.0127(12) 0.0113(12) 0.0108(11) P2 0.0122(13) 0.0151(13) 0.0204(15) 0.0092(11) 0.0061(12) 0.0056(11) P3 0.0112(12) 0.0146(12) 0.0163(14) 0.0096(11) 0.0063(11) 0.0062(10) O1 0.033(2) 0.038(2) 0.045(2) 0.0283(18) 0.0283(18) 0.0209(18) O2 0.033(2) 0.037(2) 0.045(2) 0.0290(18) 0.0285(18) 0.0217(18) O3 0.033(2) 0.038(2) 0.046(2) 0.0291(18) 0.0288(18) 0.0227(18) O4 0.034(2) 0.040(2) 0.051(2) 0.0276(19) 0.0257(19) 0.0206(19) O5 0.033(2) 0.038(2) 0.046(2) 0.0278(19) 0.0273(19) 0.0236(19) O6 0.034(2) 0.036(2) 0.045(2) 0.0298(18) 0.0277(18) 0.0224(18) O7 0.033(2) 0.038(2) 0.045(2) 0.0276(18) 0.0282(18) 0.0224(18) O8 0.034(2) 0.038(2) 0.046(2) 0.0275(19) 0.0298(18) 0.0205(18) O9 0.036(2) 0.039(2) 0.048(2) 0.030(2) 0.0272(19) 0.0224(19) O10 0.033(2) 0.037(2) 0.046(2) 0.027(2) 0.0287(19) 0.0236(19) O11 0.033(2) 0.036(2) 0.044(2) 0.0294(18) 0.0292(18) 0.0214(18) O12 0.033(2) 0.037(2) 0.045(2) 0.0268(19) 0.0280(18) 0.0241(18) O13 0.033(2) 0.037(2) 0.044(2) 0.0304(18) 0.0294(18) 0.0203(18) O14 0.066(4) 0.061(4) 0.075(5) 0.008(4) 0.020(4) 0.016(4) O15 0.060(4) 0.052(4) 0.070(5) 0.016(4) 0.019(4) 0.010(4) O16 0.039(2) 0.039(2) 0.050(2) 0.0289(19) 0.0221(19) 0.0194(19) O17 0.036(2) 0.043(2) 0.048(2) 0.0286(19) 0.0254(19) 0.0182(19) O18 0.036(2) 0.044(2) 0.049(2) 0.029(2) 0.025(2) 0.020(2) O19 0.039(2) 0.041(2) 0.049(2) 0.030(2) 0.023(2) 0.018(2) O20 0.037(2) 0.041(2) 0.050(2) 0.0277(19) 0.0284(19) 0.0177(19) O21 0.038(2) 0.041(2) 0.049(2) 0.0257(19) 0.0303(19) 0.0176(19) O22 0.037(2) 0.041(2) 0.049(2) 0.0272(19) 0.0299(18) 0.0183(19) O23 0.038(2) 0.042(2) 0.048(2) 0.0262(19) 0.0307(18) 0.0170(19) O24 0.043(3) 0.046(3) 0.057(4) 0.016(3) 0.029(3) 0.020(3) O1W 0.048(2) 0.051(2) 0.059(2) 0.023(2) 0.019(2) 0.016(2) O2W 0.043(2) 0.047(2) 0.051(2) 0.027(2) 0.023(2) 0.017(2) O3W 0.089(6) 0.093(6) 0.066(5) 0.026(5) 0.028(5) 0.008(5) O4W 0.051(2) 0.053(2) 0.060(2) 0.021(2) 0.020(2) 0.014(2) O5W 0.050(2) 0.054(2) 0.061(2) 0.020(2) 0.020(2) 0.015(2) O6W 0.051(2) 0.054(2) 0.061(2) 0.021(2) 0.018(2) 0.015(2) O7W 0.052(2) 0.056(2) 0.061(2) 0.020(2) 0.020(2) 0.012(2) N1 0.017(5) 0.029(5) 0.023(5) 0.018(4) 0.014(4) 0.015(4) N2 0.017(5) 0.014(4) 0.021(5) 0.009(4) 0.007(4) 0.006(4) N3 0.018(5) 0.030(5) 0.016(5) 0.010(4) 0.007(4) 0.005(4) C1 0.019(4) 0.037(5) 0.032(5) 0.022(4) 0.017(4) 0.017(4) C2 0.020(4) 0.031(4) 0.038(4) 0.019(4) 0.017(3) 0.016(3) C3 0.021(4) 0.025(4) 0.038(4) 0.017(3) 0.017(3) 0.014(3) C4 0.018(4) 0.023(4) 0.037(4) 0.019(3) 0.017(3) 0.014(3) C5 0.019(4) 0.022(4) 0.036(4) 0.016(3) 0.016(3) 0.012(3) C6 0.021(4) 0.029(4) 0.039(4) 0.018(4) 0.016(3) 0.014(3) C7 0.018(4) 0.021(4) 0.032(5) 0.013(4) 0.019(4) 0.013(3) C8 0.018(4) 0.022(4) 0.034(5) 0.019(4) 0.012(4) 0.012(4) C9 0.022(4) 0.024(4) 0.032(4) 0.019(3) 0.016(3) 0.012(3) C10 0.025(4) 0.025(4) 0.027(4) 0.019(3) 0.016(3) 0.016(3) C11 0.021(4) 0.024(4) 0.031(4) 0.017(3) 0.017(3) 0.014(3) C12 0.020(4) 0.026(4) 0.031(4) 0.017(3) 0.020(3) 0.014(3) C13 0.021(4) 0.023(4) 0.034(4) 0.018(3) 0.017(3) 0.012(3) C14 0.022(4) 0.022(4) 0.032(5) 0.016(4) 0.016(4) 0.015(4) C15 0.033(5) 0.031(5) 0.021(4) 0.015(4) 0.018(4) 0.021(4) C16 0.041(5) 0.038(5) 0.027(4) 0.012(4) 0.021(4) 0.018(4) C17 0.050(5) 0.042(5) 0.034(4) 0.008(4) 0.017(4) 0.020(4) C18 0.052(5) 0.042(5) 0.038(5) 0.011(4) 0.017(4) 0.017(4) C19 0.051(5) 0.043(5) 0.038(5) 0.012(4) 0.011(4) 0.012(4) C20 0.044(5) 0.040(5) 0.031(5) 0.012(4) 0.015(4) 0.014(4) C21 0.054(5) 0.054(5) 0.050(5) 0.012(5) 0.018(4) 0.021(5) C22 0.021(4) 0.036(4) 0.029(4) 0.019(4) 0.011(3) 0.015(3) C23 0.026(4) 0.037(4) 0.026(4) 0.018(3) 0.010(3) 0.012(3) C24 0.026(4) 0.036(4) 0.030(4) 0.020(3) 0.006(3) 0.012(3) C25 0.025(4) 0.039(4) 0.032(4) 0.019(3) 0.006(3) 0.012(3) C26 0.024(4) 0.036(4) 0.027(4) 0.017(3) 0.012(3) 0.014(3) C27 0.025(4) 0.039(4) 0.032(4) 0.023(3) 0.006(3) 0.012(3) C28 0.025(4) 0.041(4) 0.033(4) 0.021(4) 0.007(4) 0.009(4) C29 0.028(4) 0.034(4) 0.028(4) 0.017(4) 0.012(4) 0.016(4) C30 0.030(4) 0.025(4) 0.037(4) 0.017(4) 0.019(4) 0.009(3) C31 0.029(4) 0.026(4) 0.033(4) 0.017(3) 0.024(3) 0.008(3) C32 0.029(4) 0.026(4) 0.039(4) 0.016(3) 0.025(3) 0.010(3) C33 0.031(4) 0.024(4) 0.039(4) 0.016(3) 0.021(3) 0.011(3) C34 0.029(4) 0.026(4) 0.039(4) 0.016(3) 0.023(3) 0.008(3) C35 0.030(4) 0.026(4) 0.042(4) 0.015(3) 0.024(3) 0.010(3) C36 0.031(4) 0.024(3) 0.040(4) 0.018(3) 0.024(3) 0.009(3) C37 0.027(4) 0.020(4) 0.039(4) 0.016(3) 0.022(3) 0.009(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 La1 O7 2.439(10) . ? La1 O11 2.501(8) . ? La1 O10 2.504(9) 2_566 ? La1 O23 2.553(9) 2_666 ? La1 O1 2.592(9) . ? La1 O22 2.622(9) 2_666 ? La1 O2 2.627(8) . ? La1 O19 2.630(10) 1_454 ? La1 O18 2.656(10) 1_454 ? La1 C37 2.960(12) 2_666 ? La1 C29 3.011(13) 1_454 ? La1 P1 3.214(3) . ? La2 O2 2.426(10) . ? La2 O13 2.503(8) 2_556 ? La2 O5 2.511(9) 2_656 ? La2 O20 2.570(9) . ? La2 O6 2.574(9) . ? La2 O21 2.579(9) . ? La2 O17 2.584(10) . ? La2 O7 2.623(8) . ? La2 O16 2.667(10) . ? La2 C30 2.926(12) . ? La2 C22 3.010(12) . ? La2 P2 3.200(3) . ? La3 O12 2.402(8) 2_556 ? La3 O8 2.504(9) . ? La3 O3 2.522(9) 2_556 ? La3 O4 2.536(9) 1_455 ? La3 O9 2.552(9) 2_566 ? La3 O24 2.566(11) . ? La3 O11 2.636(9) . ? La3 O13 2.638(9) . ? La3 P3 3.234(3) . ? P1 O3 1.506(9) . ? P1 O1 1.527(9) . ? P1 O2 1.540(10) . ? P1 C1 1.817(12) . ? P2 O8 1.503(9) . ? P2 O6 1.526(9) . ? P2 O7 1.528(10) . ? P2 C8 1.832(11) . ? P3 O12 1.497(9) . ? P3 O13 1.532(9) . ? P3 O11 1.539(9) . ? P3 C15 1.845(12) . ? O3 La3 2.522(9) 2_556 ? O4 C7 1.253(14) . ? O4 La3 2.536(9) 1_655 ? O5 C7 1.262(14) . ? O5 La2 2.511(9) 2_656 ? O9 C14 1.241(15) . ? O9 La3 2.552(9) 2_566 ? O10 C14 1.279(14) . ? O10 La1 2.504(9) 2_566 ? O12 La3 2.402(8) 2_556 ? O13 La2 2.503(8) 2_556 ? O14 C21 1.27(2) . ? O14 H21A 0.8500 . ? O15 C21 1.19(2) . ? O16 C22 1.249(15) . ? O17 C22 1.244(15) . ? O18 C29 1.233(16) . ? O18 La1 2.656(10) 1_656 ? O19 C29 1.264(16) . ? O19 La1 2.630(10) 1_656 ? O20 C30 1.266(16) . ? O21 C30 1.233(16) . ? O22 C37 1.267(15) . ? O22 La1 2.622(9) 2_666 ? O23 C37 1.249(15) . ? O23 La1 2.553(9) 2_666 ? O24 H24C 0.8498 . ? O24 H24D 0.8496 . ? O1W H1WA 0.8501 . ? O1W H1WB 0.8503 . ? O2W H2WA 0.8503 . ? O2W H2WB 0.8499 . ? O3W H3WC 0.8499 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8501 . ? O4W H4WB 0.8500 . ? O5W H5WA 0.8500 . ? O5W H5WB 0.8500 . ? O6W H6WA 0.8500 . ? O6W H6WB 0.8498 . ? O7W H7WC 0.8500 . ? O7W H7WB 0.8500 . ? N1 C2 1.467(15) . ? N1 C6 1.489(15) . ? N1 C1 1.513(14) . ? N1 H3C 0.8999 . ? N2 C13 1.475(14) . ? N2 C8 1.502(13) . ? N2 C9 1.511(15) . ? N2 H2C 0.9002 . ? N3 C20 1.480(17) . ? N3 C15 1.483(15) . ? N3 C16 1.497(17) . ? N3 H1C 0.8998 . ? C1 H28A 0.9700 . ? C1 H28B 0.9700 . ? C2 C3 1.530(16) . ? C2 H30A 0.9700 . ? C2 H30B 0.9700 . ? C3 C4 1.516(16) . ? C3 H32A 0.9700 . ? C3 H32B 0.9700 . ? C4 C7 1.513(15) . ? C4 C5 1.539(15) . ? C4 H33A 0.9800 . ? C5 C6 1.514(16) . ? C5 H31A 0.9700 . ? C5 H31B 0.9700 . ? C6 H29A 0.9700 . ? C6 H29B 0.9700 . ? C8 H2A 0.9700 . ? C8 H2B 0.9700 . ? C9 C10 1.526(15) . ? C9 H4A 0.9700 . ? C9 H4B 0.9700 . ? C10 C11 1.500(16) . ? C10 H6A 0.9700 . ? C10 H6B 0.9700 . ? C11 C12 1.526(16) . ? C11 C14 1.534(15) . ? C11 H7A 0.9800 . ? C12 C13 1.522(15) . ? C12 H5A 0.9700 . ? C12 H5B 0.9700 . ? C13 H3A 0.9700 . ? C13 H3B 0.9700 . ? C15 H1A 0.9700 . ? C15 H1B 0.9700 . ? C16 C17 1.50(2) . ? C16 H23A 0.9700 . ? C16 H23B 0.9700 . ? C17 C18 1.55(2) . ? C17 H25A 0.9700 . ? C17 H25B 0.9700 . ? C18 C19 1.52(2) . ? C18 C21 1.53(2) . ? C18 H27A 0.9800 . ? C19 C20 1.55(2) . ? C19 H26A 0.9700 . ? C19 H26B 0.9700 . ? C20 H24A 0.9700 . ? C20 H24B 0.9700 . ? C22 C23 1.492(17) . ? C23 C24 1.371(18) . ? C23 C28 1.395(18) . ? C24 C25 1.377(17) . ? C24 H11A 0.9300 . ? C25 C26 1.372(19) . ? C25 H13A 0.9300 . ? C26 C27 1.379(18) . ? C26 C29 1.524(17) . ? C27 C28 1.390(18) . ? C27 H37A 0.9300 . ? C28 H12A 0.9300 . ? C29 La1 3.011(12) 1_656 ? C30 C31 1.482(16) . ? C31 C36 1.392(17) . ? C31 C32 1.421(17) . ? C32 C33 1.386(17) . ? C32 H18A 0.9300 . ? C33 C34 1.367(18) . ? C33 H19A 0.9300 . ? C34 C35 1.410(17) . ? C34 C37 1.473(16) . ? C35 C36 1.389(17) . ? C35 H22A 0.9300 . ? C36 H35A 0.9300 . ? C37 La1 2.960(12) 2_666 ? 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 O7 La1 O11 77.1(3) . . ? O7 La1 O10 74.7(3) . 2_566 ? O11 La1 O10 80.9(3) . 2_566 ? O7 La1 O23 78.6(3) . 2_666 ? O11 La1 O23 146.0(3) . 2_666 ? O10 La1 O23 69.9(3) 2_566 2_666 ? O7 La1 O1 118.8(3) . . ? O11 La1 O1 82.3(3) . . ? O10 La1 O1 155.2(3) 2_566 . ? O23 La1 O1 130.7(3) 2_666 . ? O7 La1 O22 100.0(3) . 2_666 ? O11 La1 O22 158.7(3) . 2_666 ? O10 La1 O22 119.1(3) 2_566 2_666 ? O23 La1 O22 50.1(3) 2_666 2_666 ? O1 La1 O22 80.8(3) . 2_666 ? O7 La1 O2 65.6(3) . . ? O11 La1 O2 87.1(3) . . ? O10 La1 O2 140.1(3) 2_566 . ? O23 La1 O2 104.1(3) 2_666 . ? O1 La1 O2 56.3(3) . . ? O22 La1 O2 72.8(3) 2_666 . ? O7 La1 O19 138.9(3) . 1_454 ? O11 La1 O19 71.4(3) . 1_454 ? O10 La1 O19 74.9(3) 2_566 1_454 ? O23 La1 O19 115.3(3) 2_666 1_454 ? O1 La1 O19 82.6(3) . 1_454 ? O22 La1 O19 118.7(3) 2_666 1_454 ? O2 La1 O19 136.1(3) . 1_454 ? O7 La1 O18 150.5(3) . 1_454 ? O11 La1 O18 120.2(3) . 1_454 ? O10 La1 O18 84.3(3) 2_566 1_454 ? O23 La1 O18 74.9(3) 2_666 1_454 ? O1 La1 O18 88.6(3) . 1_454 ? O22 La1 O18 72.2(3) 2_666 1_454 ? O2 La1 O18 133.5(3) . 1_454 ? O19 La1 O18 48.8(3) 1_454 1_454 ? O7 La1 C37 89.8(3) . 2_666 ? O11 La1 C37 166.8(3) . 2_666 ? O10 La1 C37 94.1(3) 2_566 2_666 ? O23 La1 C37 24.8(3) 2_666 2_666 ? O1 La1 C37 106.0(3) . 2_666 ? O22 La1 C37 25.3(3) 2_666 2_666 ? O2 La1 C37 89.1(3) . 2_666 ? O19 La1 C37 119.3(3) 1_454 2_666 ? O18 La1 C37 71.1(3) 1_454 2_666 ? O7 La1 C29 152.0(3) . 1_454 ? O11 La1 C29 96.1(3) . 1_454 ? O10 La1 C29 77.5(3) 2_566 1_454 ? O23 La1 C29 94.3(3) 2_666 1_454 ? O1 La1 C29 86.4(3) . 1_454 ? O22 La1 C29 95.6(3) 2_666 1_454 ? O2 La1 C29 141.9(3) . 1_454 ? O19 La1 C29 24.7(3) 1_454 1_454 ? O18 La1 C29 24.1(3) 1_454 1_454 ? C37 La1 C29 94.7(4) 2_666 1_454 ? O7 La1 P1 92.9(2) . . ? O11 La1 P1 85.3(2) . . ? O10 La1 P1 163.1(2) 2_566 . ? O23 La1 P1 119.5(2) 2_666 . ? O1 La1 P1 28.0(2) . . ? O22 La1 P1 73.7(2) 2_666 . ? O2 La1 P1 28.4(2) . . ? O19 La1 P1 109.8(2) 1_454 . ? O18 La1 P1 111.2(2) 1_454 . ? C37 La1 P1 97.3(2) 2_666 . ? C29 La1 P1 113.8(3) 1_454 . ? O2 La2 O13 79.1(3) . 2_556 ? O2 La2 O5 76.6(3) . 2_656 ? O13 La2 O5 80.4(3) 2_556 2_656 ? O2 La2 O20 96.6(3) . . ? O13 La2 O20 156.0(3) 2_556 . ? O5 La2 O20 121.9(3) 2_656 . ? O2 La2 O6 119.0(3) . . ? O13 La2 O6 79.8(3) 2_556 . ? O5 La2 O6 151.6(3) 2_656 . ? O20 La2 O6 81.9(3) . . ? O2 La2 O21 80.8(3) . . ? O13 La2 O21 148.7(3) 2_556 . ? O5 La2 O21 71.8(3) 2_656 . ? O20 La2 O21 50.3(3) . . ? O6 La2 O21 131.2(3) . . ? O2 La2 O17 142.6(3) . . ? O13 La2 O17 71.8(3) 2_556 . ? O5 La2 O17 75.7(3) 2_656 . ? O20 La2 O17 119.4(3) . . ? O6 La2 O17 78.8(3) . . ? O21 La2 O17 113.4(3) . . ? O2 La2 O7 65.9(3) . . ? O13 La2 O7 86.5(3) 2_556 . ? O5 La2 O7 142.0(3) 2_656 . ? O20 La2 O7 70.4(3) . . ? O6 La2 O7 56.2(3) . . ? O21 La2 O7 106.6(3) . . ? O17 La2 O7 133.1(3) . . ? O2 La2 O16 153.1(3) . . ? O13 La2 O16 120.3(3) 2_556 . ? O5 La2 O16 87.9(3) 2_656 . ? O20 La2 O16 72.9(3) . . ? O6 La2 O16 84.7(3) . . ? O21 La2 O16 73.5(3) . . ? O17 La2 O16 48.6(3) . . ? O7 La2 O16 129.0(3) . . ? O2 La2 C30 90.3(3) . . ? O13 La2 C30 169.3(3) 2_556 . ? O5 La2 C30 96.3(3) 2_656 . ? O20 La2 C30 25.6(3) . . ? O6 La2 C30 106.6(3) . . ? O21 La2 C30 24.9(3) . . ? O17 La2 C30 117.4(3) . . ? O7 La2 C30 90.1(3) . . ? O16 La2 C30 69.4(3) . . ? O2 La2 C22 156.4(3) . . ? O13 La2 C22 96.0(3) 2_556 . ? O5 La2 C22 79.8(3) 2_656 . ? O20 La2 C22 96.7(3) . . ? O6 La2 C22 82.2(3) . . ? O21 La2 C22 93.0(3) . . ? O17 La2 C22 24.2(3) . . ? O7 La2 C22 137.3(3) . . ? O16 La2 C22 24.5(3) . . ? C30 La2 C22 93.3(4) . . ? O2 La2 P2 93.1(2) . . ? O13 La2 P2 84.1(2) 2_556 . ? O5 La2 P2 162.7(2) 2_656 . ? O20 La2 P2 72.5(2) . . ? O6 La2 P2 28.1(2) . . ? O21 La2 P2 120.8(2) . . ? O17 La2 P2 106.5(2) . . ? O7 La2 P2 28.3(2) . . ? O16 La2 P2 106.6(2) . . ? C30 La2 P2 97.6(3) . . ? C22 La2 P2 109.4(3) . . ? O12 La3 O8 73.9(3) 2_556 . ? O12 La3 O3 73.6(3) 2_556 2_556 ? O8 La3 O3 108.9(3) . 2_556 ? O12 La3 O4 141.7(3) 2_556 1_455 ? O8 La3 O4 143.9(3) . 1_455 ? O3 La3 O4 83.9(3) 2_556 1_455 ? O12 La3 O9 141.5(3) 2_556 2_566 ? O8 La3 O9 80.2(3) . 2_566 ? O3 La3 O9 143.1(3) 2_556 2_566 ? O4 La3 O9 70.8(3) 1_455 2_566 ? O12 La3 O24 121.4(3) 2_556 . ? O8 La3 O24 74.5(3) . . ? O3 La3 O24 72.0(3) 2_556 . ? O4 La3 O24 78.1(3) 1_455 . ? O9 La3 O24 76.7(3) 2_566 . ? O12 La3 O11 77.7(3) 2_556 . ? O8 La3 O11 89.7(3) . . ? O3 La3 O11 139.2(3) 2_556 . ? O4 La3 O11 102.3(3) 1_455 . ? O9 La3 O11 74.1(3) 2_566 . ? O24 La3 O11 148.8(3) . . ? O12 La3 O13 76.8(3) 2_556 . ? O8 La3 O13 138.5(3) . . ? O3 La3 O13 89.9(3) 2_556 . ? O4 La3 O13 72.5(3) 1_455 . ? O9 La3 O13 106.8(3) 2_566 . ? O24 La3 O13 146.9(3) . . ? O11 La3 O13 55.4(3) . . ? O12 La3 P3 71.1(2) 2_556 . ? O8 La3 P3 112.8(2) . . ? O3 La3 P3 113.2(2) 2_556 . ? O4 La3 P3 90.9(2) 1_455 . ? O9 La3 P3 94.1(2) 2_566 . ? O24 La3 P3 167.4(3) . . ? O11 La3 P3 28.10(19) . . ? O13 La3 P3 27.96(18) . . ? O3 P1 O1 118.1(5) . . ? O3 P1 O2 113.5(5) . . ? O1 P1 O2 106.7(5) . . ? O3 P1 C1 108.3(5) . . ? O1 P1 C1 104.8(5) . . ? O2 P1 C1 104.2(5) . . ? O3 P1 La1 140.2(4) . . ? O1 P1 La1 52.7(4) . . ? O2 P1 La1 54.1(3) . . ? C1 P1 La1 111.5(4) . . ? O8 P2 O6 116.9(5) . . ? O8 P2 O7 115.1(5) . . ? O6 P2 O7 106.6(5) . . ? O8 P2 C8 108.9(5) . . ? O6 P2 C8 102.7(5) . . ? O7 P2 C8 105.3(6) . . ? O8 P2 La2 141.8(4) . . ? O6 P2 La2 52.5(4) . . ? O7 P2 La2 54.4(3) . . ? C8 P2 La2 109.2(4) . . ? O12 P3 O13 113.5(5) . . ? O12 P3 O11 114.8(5) . . ? O13 P3 O11 105.9(5) . . ? O12 P3 C15 106.6(5) . . ? O13 P3 C15 109.4(5) . . ? O11 P3 C15 106.3(5) . . ? O12 P3 La3 121.4(4) . . ? O13 P3 La3 53.8(4) . . ? O11 P3 La3 53.8(3) . . ? C15 P3 La3 132.0(4) . . ? P1 O1 La1 99.3(5) . . ? P1 O2 La2 147.5(5) . . ? P1 O2 La1 97.5(4) . . ? La2 O2 La1 113.8(4) . . ? P1 O3 La3 132.8(5) . 2_556 ? C7 O4 La3 136.1(8) . 1_655 ? C7 O5 La2 125.0(8) . 2_656 ? P2 O6 La2 99.4(4) . . ? P2 O7 La1 148.2(5) . . ? P2 O7 La2 97.4(4) . . ? La1 O7 La2 113.6(3) . . ? P2 O8 La3 131.1(5) . . ? C14 O9 La3 136.6(8) . 2_566 ? C14 O10 La1 126.7(8) . 2_566 ? P3 O11 La1 134.3(5) . . ? P3 O11 La3 98.1(4) . . ? La1 O11 La3 127.1(4) . . ? P3 O12 La3 167.5(6) . 2_556 ? P3 O13 La2 136.1(5) . 2_556 ? P3 O13 La3 98.2(4) . . ? La2 O13 La3 125.4(3) 2_556 . ? C21 O14 H21A 117.2 . . ? C22 O16 La2 93.3(8) . . ? C22 O17 La2 97.5(8) . . ? C29 O18 La1 94.3(8) . 1_656 ? C29 O19 La1 94.8(8) . 1_656 ? C30 O20 La2 93.2(8) . . ? C30 O21 La2 93.5(8) . . ? C37 O22 La1 92.5(7) . 2_666 ? C37 O23 La1 96.2(8) . 2_666 ? La3 O24 H24C 109.3 . . ? La3 O24 H24D 109.0 . . ? H24C O24 H24D 109.5 . . ? H1WA O1W H1WB 109.5 . . ? H2WA O2W H2WB 109.5 . . ? H3WC O3W H3WB 109.8 . . ? H4WA O4W H4WB 109.5 . . ? H5WA O5W H5WB 109.5 . . ? H6WA O6W H6WB 109.5 . . ? H7WC O7W H7WB 109.8 . . ? C2 N1 C6 111.8(9) . . ? C2 N1 C1 111.0(9) . . ? C6 N1 C1 111.5(9) . . ? C2 N1 H3C 107.7 . . ? C6 N1 H3C 107.1 . . ? C1 N1 H3C 107.5 . . ? C13 N2 C8 111.7(9) . . ? C13 N2 C9 110.2(9) . . ? C8 N2 C9 109.4(9) . . ? C13 N2 H2C 108.6 . . ? C8 N2 H2C 108.6 . . ? C9 N2 H2C 108.3 . . ? C20 N3 C15 112.7(10) . . ? C20 N3 C16 108.7(10) . . ? C15 N3 C16 111.9(9) . . ? C20 N3 H1C 107.7 . . ? C15 N3 H1C 108.0 . . ? C16 N3 H1C 107.7 . . ? N1 C1 P1 115.1(8) . . ? N1 C1 H28A 108.5 . . ? P1 C1 H28A 108.5 . . ? N1 C1 H28B 108.5 . . ? P1 C1 H28B 108.5 . . ? H28A C1 H28B 107.5 . . ? N1 C2 C3 111.1(10) . . ? N1 C2 H30A 109.4 . . ? C3 C2 H30A 109.4 . . ? N1 C2 H30B 109.4 . . ? C3 C2 H30B 109.4 . . ? H30A C2 H30B 108.0 . . ? C4 C3 C2 111.8(10) . . ? C4 C3 H32A 109.2 . . ? C2 C3 H32A 109.2 . . ? C4 C3 H32B 109.2 . . ? C2 C3 H32B 109.2 . . ? H32A C3 H32B 107.9 . . ? C7 C4 C3 112.5(10) . . ? C7 C4 C5 112.9(9) . . ? C3 C4 C5 110.2(10) . . ? C7 C4 H33A 107.0 . . ? C3 C4 H33A 107.0 . . ? C5 C4 H33A 107.0 . . ? C6 C5 C4 112.9(10) . . ? C6 C5 H31A 109.0 . . ? C4 C5 H31A 109.0 . . ? C6 C5 H31B 109.0 . . ? C4 C5 H31B 109.0 . . ? H31A C5 H31B 107.8 . . ? N1 C6 C5 111.1(10) . . ? N1 C6 H29A 109.4 . . ? C5 C6 H29A 109.4 . . ? N1 C6 H29B 109.4 . . ? C5 C6 H29B 109.4 . . ? H29A C6 H29B 108.0 . . ? O4 C7 O5 123.8(11) . . ? O4 C7 C4 117.1(10) . . ? O5 C7 C4 119.0(10) . . ? N2 C8 P2 112.9(8) . . ? N2 C8 H2A 109.0 . . ? P2 C8 H2A 109.0 . . ? N2 C8 H2B 109.0 . . ? P2 C8 H2B 109.0 . . ? H2A C8 H2B 107.8 . . ? N2 C9 C10 110.8(10) . . ? N2 C9 H4A 109.5 . . ? C10 C9 H4A 109.5 . . ? N2 C9 H4B 109.5 . . ? C10 C9 H4B 109.5 . . ? H4A C9 H4B 108.1 . . ? C11 C10 C9 113.1(10) . . ? C11 C10 H6A 109.0 . . ? C9 C10 H6A 109.0 . . ? C11 C10 H6B 109.0 . . ? C9 C10 H6B 109.0 . . ? H6A C10 H6B 107.8 . . ? C10 C11 C12 111.7(9) . . ? C10 C11 C14 113.4(10) . . ? C12 C11 C14 111.4(10) . . ? C10 C11 H7A 106.6 . . ? C12 C11 H7A 106.6 . . ? C14 C11 H7A 106.6 . . ? C13 C12 C11 110.7(10) . . ? C13 C12 H5A 109.5 . . ? C11 C12 H5A 109.5 . . ? C13 C12 H5B 109.5 . . ? C11 C12 H5B 109.5 . . ? H5A C12 H5B 108.1 . . ? N2 C13 C12 111.2(9) . . ? N2 C13 H3A 109.4 . . ? C12 C13 H3A 109.4 . . ? N2 C13 H3B 109.4 . . ? C12 C13 H3B 109.4 . . ? H3A C13 H3B 108.0 . . ? O9 C14 O10 125.4(11) . . ? O9 C14 C11 117.8(10) . . ? O10 C14 C11 116.8(10) . . ? N3 C15 P3 115.3(8) . . ? N3 C15 H1A 108.5 . . ? P3 C15 H1A 108.5 . . ? N3 C15 H1B 108.5 . . ? P3 C15 H1B 108.5 . . ? H1A C15 H1B 107.5 . . ? N3 C16 C17 111.3(12) . . ? N3 C16 H23A 109.4 . . ? C17 C16 H23A 109.4 . . ? N3 C16 H23B 109.4 . . ? C17 C16 H23B 109.4 . . ? H23A C16 H23B 108.0 . . ? C16 C17 C18 111.2(13) . . ? C16 C17 H25A 109.4 . . ? C18 C17 H25A 109.4 . . ? C16 C17 H25B 109.4 . . ? C18 C17 H25B 109.4 . . ? H25A C17 H25B 108.0 . . ? C19 C18 C21 113.8(15) . . ? C19 C18 C17 110.6(13) . . ? C21 C18 C17 109.5(14) . . ? C19 C18 H27A 107.6 . . ? C21 C18 H27A 107.6 . . ? C17 C18 H27A 107.6 . . ? C18 C19 C20 111.6(14) . . ? C18 C19 H26A 109.3 . . ? C20 C19 H26A 109.3 . . ? C18 C19 H26B 109.3 . . ? C20 C19 H26B 109.3 . . ? H26A C19 H26B 108.0 . . ? N3 C20 C19 109.9(12) . . ? N3 C20 H24A 109.7 . . ? C19 C20 H24A 109.7 . . ? N3 C20 H24B 109.7 . . ? C19 C20 H24B 109.7 . . ? H24A C20 H24B 108.2 . . ? O15 C21 O14 127.4(19) . . ? O15 C21 C18 115.3(19) . . ? O14 C21 C18 117.3(18) . . ? O17 C22 O16 120.3(12) . . ? O17 C22 C23 119.7(12) . . ? O16 C22 C23 119.9(12) . . ? O17 C22 La2 58.3(7) . . ? O16 C22 La2 62.2(7) . . ? C23 C22 La2 171.4(10) . . ? C24 C23 C28 118.2(12) . . ? C24 C23 C22 122.3(12) . . ? C28 C23 C22 119.1(12) . . ? C23 C24 C25 122.0(13) . . ? C23 C24 H11A 119.0 . . ? C25 C24 H11A 119.0 . . ? C26 C25 C24 120.0(13) . . ? C26 C25 H13A 120.0 . . ? C24 C25 H13A 120.0 . . ? C25 C26 C27 119.0(12) . . ? C25 C26 C29 120.6(12) . . ? C27 C26 C29 120.2(12) . . ? C26 C27 C28 120.9(13) . . ? C26 C27 H37A 119.6 . . ? C28 C27 H37A 119.6 . . ? C27 C28 C23 119.6(13) . . ? C27 C28 H12A 120.2 . . ? C23 C28 H12A 120.2 . . ? O18 C29 O19 121.9(12) . . ? O18 C29 C26 119.3(12) . . ? O19 C29 C26 118.8(12) . . ? O18 C29 La1 61.6(7) . 1_656 ? O19 C29 La1 60.5(7) . 1_656 ? C26 C29 La1 174.2(9) . 1_656 ? O21 C30 O20 122.3(12) . . ? O21 C30 C31 119.7(12) . . ? O20 C30 C31 118.0(11) . . ? O21 C30 La2 61.6(7) . . ? O20 C30 La2 61.3(7) . . ? C31 C30 La2 173.5(9) . . ? C36 C31 C32 118.8(11) . . ? C36 C31 C30 119.7(11) . . ? C32 C31 C30 121.3(11) . . ? C33 C32 C31 119.2(12) . . ? C33 C32 H18A 120.4 . . ? C31 C32 H18A 120.4 . . ? C34 C33 C32 122.5(12) . . ? C34 C33 H19A 118.7 . . ? C32 C33 H19A 118.7 . . ? C33 C34 C35 117.9(11) . . ? C33 C34 C37 122.6(12) . . ? C35 C34 C37 119.5(12) . . ? C36 C35 C34 121.2(12) . . ? C36 C35 H22A 119.4 . . ? C34 C35 H22A 119.4 . . ? C35 C36 C31 120.0(12) . . ? C35 C36 H35A 120.0 . . ? C31 C36 H35A 120.0 . . ? O23 C37 O22 121.2(11) . . ? O23 C37 C34 119.8(11) . . ? O22 C37 C34 119.0(11) . . ? O23 C37 La1 59.0(6) . 2_666 ? O22 C37 La1 62.2(6) . 2_666 ? C34 C37 La1 177.1(9) . 2_666 ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.995 _refine_diff_density_min -5.092 _refine_diff_density_rms 0.265 # Attachment 'szg167.cif' data_szg167 _database_code_depnum_ccdc_archive 'CCDC 849252' #TrackingRef 'szg167.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H61 Ce3 N3 O31 P3' _chemical_formula_weight 1557.16 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.2095(12) _cell_length_b 15.3049(12) _cell_length_c 15.3698(12) _cell_angle_alpha 106.4850(10) _cell_angle_beta 117.1430(10) _cell_angle_gamma 103.2360(10) _cell_volume 2770.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3962 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 28.64 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.867 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1542 _exptl_absorpt_coefficient_mu 2.603 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6161 _exptl_absorpt_correction_T_max 0.7557 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Smart Apex II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15700 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.50 _reflns_number_total 11153 _reflns_number_gt 8523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0946P)^2^+52.8413P] 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 11153 _refine_ls_number_parameters 694 _refine_ls_number_restraints 2130 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1953 _refine_ls_wR_factor_gt 0.1756 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.05686(4) 0.19758(4) 0.36611(4) 0.01542(14) Uani 1 1 d . . . Ce2 Ce 0.32052(4) 0.18275(4) 0.61513(4) 0.01586(14) Uani 1 1 d . . . Ce3 Ce -0.08463(4) 0.14570(4) 0.56272(4) 0.01636(15) Uani 1 1 d . . . P1 P 0.12575(19) 0.01765(19) 0.3101(2) 0.0174(5) Uani 1 1 d . . . P2 P 0.19642(19) 0.30505(18) 0.6739(2) 0.0173(5) Uani 1 1 d . . . P3 P -0.11717(18) -0.02455(18) 0.3573(2) 0.0147(5) Uani 1 1 d . . . O1 O 0.0232(7) 0.0269(6) 0.2355(7) 0.0359(10) Uani 1 1 d U . . O2 O 0.1863(7) 0.1081(6) 0.4208(7) 0.0386(10) Uani 1 1 d U . . O3 O 0.1127(7) -0.0797(6) 0.3165(7) 0.0366(10) Uani 1 1 d U . . O4 O 0.7135(7) 0.0975(7) 0.4611(8) 0.0396(15) Uani 1 1 d U . . O5 O 0.6364(7) -0.0446(6) 0.4614(7) 0.0350(14) Uani 1 1 d U . . O6 O 0.2791(6) 0.2757(6) 0.7473(7) 0.0337(11) Uani 1 1 d U . . O7 O 0.1745(6) 0.2548(6) 0.5609(7) 0.0337(11) Uani 1 1 d U . . O8 O 0.0953(6) 0.2903(6) 0.6742(7) 0.0327(11) Uani 1 1 d U . . O9 O 0.1297(7) 0.7435(6) 0.5292(7) 0.0364(12) Uani 1 1 d U . . O10 O -0.0028(7) 0.6801(6) 0.5498(7) 0.0345(12) Uani 1 1 d U . . O11 O -0.0564(7) 0.0897(6) 0.4033(7) 0.0354(10) Uani 1 1 d U . . O12 O -0.0461(7) -0.0806(6) 0.3723(7) 0.0358(10) Uani 1 1 d U . . O13 O -0.1813(7) -0.0384(6) 0.4086(7) 0.0351(10) Uani 1 1 d U . . O14 O -0.2781(7) -0.5079(7) -0.1118(8) 0.0434(9) Uani 1 1 d U . . H21A H -0.2948 -0.5254 -0.1769 0.052 Uiso 1 1 d R . . O15 O -0.4228(7) -0.5318(7) -0.1065(8) 0.0427(9) Uani 1 1 d U . . O16 O 0.5238(7) 0.2721(7) 0.7909(8) 0.0421(12) Uani 1 1 d U . . O17 O 0.4149(7) 0.1389(7) 0.7730(7) 0.0386(12) Uani 1 1 d U . . O18 O 0.9662(7) 0.2363(7) 1.1981(8) 0.0424(16) Uani 1 1 d U . . O19 O 0.8511(7) 0.1399(7) 1.2171(7) 0.0407(17) Uani 1 1 d U . . O20 O 0.4052(7) 0.3585(6) 0.6390(7) 0.0384(11) Uani 1 1 d U . . O21 O 0.4433(7) 0.2477(7) 0.5551(7) 0.0401(12) Uani 1 1 d U . . O22 O 0.7997(7) 0.7426(7) 0.6773(8) 0.0399(15) Uani 1 1 d U . . O23 O 0.8174(7) 0.6252(7) 0.5727(8) 0.0412(15) Uani 1 1 d U . . O24 O -0.0968(7) 0.2799(7) 0.6922(7) 0.0392(6) Uani 1 1 d U . . H24C H -0.0379 0.3327 0.7306 0.059 Uiso 1 1 d R . . H24D H -0.1492 0.2926 0.6555 0.059 Uiso 1 1 d R . . O1W O 0.4811(8) 0.8105(8) 0.8169(9) 0.0573(14) Uani 1 1 d U . . H1WA H 0.4532 0.8474 0.7933 0.086 Uiso 1 1 d R . . H1WB H 0.4905 0.8217 0.8786 0.086 Uiso 1 1 d R . . O2W O 0.3359(7) 0.9019(7) 0.7557(8) 0.0472(14) Uani 1 1 d U . . H2WA H 0.2931 0.9229 0.7183 0.071 Uiso 1 1 d R . . H2WB H 0.3418 0.9169 0.8163 0.071 Uiso 1 1 d R . . O3W O 0.9088(19) 0.9872(18) 0.0183(18) 0.172(9) Uani 1 1 d U . . H3WC H 0.9360 1.0295 0.0835 0.207 Uiso 1 1 d R . . H3WB H 0.8858 0.9280 0.0111 0.258 Uiso 1 1 d R . . O4W O 0.7214(10) 0.9377(9) 0.9375(10) 0.077(2) Uani 1 1 d U . . H4WA H 0.6628 0.9388 0.9294 0.116 Uiso 1 1 d R . . H4WB H 0.7317 0.9564 0.8947 0.116 Uiso 1 1 d R . . O5W O 0.9442(9) 0.4912(9) 0.7520(10) 0.077(2) Uani 1 1 d U . . H5WA H 0.8905 0.5029 0.7162 0.115 Uiso 1 1 d R . . H5WB H 0.9295 0.4578 0.7828 0.115 Uiso 1 1 d R . . O6W O 0.7384(9) 0.3097(8) 0.7515(9) 0.0694(18) Uani 1 1 d U . . H6WA H 0.6805 0.3146 0.7122 0.104 Uiso 1 1 d R . . H6WB H 0.7230 0.2604 0.7649 0.104 Uiso 1 1 d R . . O7W O 0.9141(9) 0.2941(9) 0.8810(10) 0.075(2) Uani 1 1 d U . . H7WC H 0.9658 0.3464 0.9391 0.090 Uiso 1 1 d R . . H7WB H 0.9071 0.2435 0.8937 0.113 Uiso 1 1 d R . . N1 N 0.3200(7) 0.0410(7) 0.3229(7) 0.0247(19) Uani 1 1 d . . . H3C H 0.3367 0.0555 0.3910 0.030 Uiso 1 1 d R . . N2 N 0.2118(6) 0.4865(6) 0.6644(7) 0.0196(17) Uani 1 1 d . . . H2C H 0.1589 0.4379 0.5964 0.024 Uiso 1 1 d R . . N3 N -0.2480(7) -0.1813(7) 0.1418(7) 0.027(2) Uani 1 1 d . . . H1C H -0.2542 -0.2137 0.1804 0.032 Uiso 1 1 d R . . C1 C 0.2106(8) 0.0411(9) 0.2586(9) 0.027(2) Uani 1 1 d U . . H28A H 0.1720 -0.0097 0.1837 0.033 Uiso 1 1 calc R . . H28B H 0.2213 0.1057 0.2577 0.033 Uiso 1 1 calc R . . C2 C 0.4050(8) 0.1187(9) 0.3321(10) 0.029(2) Uani 1 1 d U . . H30A H 0.4049 0.1834 0.3635 0.035 Uiso 1 1 calc R . . H30B H 0.3887 0.1054 0.2596 0.035 Uiso 1 1 calc R . . C3 C 0.5178(9) 0.1236(8) 0.4028(10) 0.0284(19) Uani 1 1 d U . . H32A H 0.5706 0.1729 0.4025 0.034 Uiso 1 1 calc R . . H32B H 0.5381 0.1450 0.4776 0.034 Uiso 1 1 calc R . . C4 C 0.5202(8) 0.0224(8) 0.3612(10) 0.028(2) Uani 1 1 d U . . H33A H 0.5075 0.0075 0.2891 0.033 Uiso 1 1 calc R . . C5 C 0.4266(8) -0.0618(8) 0.3436(9) 0.0252(19) Uani 1 1 d U . . H31A H 0.4235 -0.1262 0.3059 0.030 Uiso 1 1 calc R . . H31B H 0.4413 -0.0549 0.4142 0.030 Uiso 1 1 calc R . . C6 C 0.3182(8) -0.0598(8) 0.2784(10) 0.0278(19) Uani 1 1 d U . . H29A H 0.2968 -0.0798 0.2034 0.033 Uiso 1 1 calc R . . H29B H 0.2640 -0.1083 0.2779 0.033 Uiso 1 1 calc R . . C7 C 0.6325(9) 0.0247(8) 0.4332(9) 0.028(2) Uani 1 1 d U . . C8 C 0.2754(8) 0.4392(8) 0.7273(9) 0.024(2) Uani 1 1 d U . . H2A H 0.2999 0.4732 0.8032 0.029 Uiso 1 1 calc R . . H2B H 0.3394 0.4484 0.7249 0.029 Uiso 1 1 calc R . . C9 C 0.1585(8) 0.5290(8) 0.7139(9) 0.0254(19) Uani 1 1 d U . . H4A H 0.2138 0.5790 0.7888 0.030 Uiso 1 1 calc R . . H4B H 0.1111 0.4759 0.7156 0.030 Uiso 1 1 calc R . . C10 C 0.0928(8) 0.5764(8) 0.6535(9) 0.0252(19) Uani 1 1 d U . . H6A H 0.0285 0.5242 0.5839 0.030 Uiso 1 1 calc R . . H6B H 0.0687 0.6109 0.6956 0.030 Uiso 1 1 calc R . . C11 C 0.1570(9) 0.6510(8) 0.6330(9) 0.0259(19) Uani 1 1 d U . . H7A H 0.2137 0.7076 0.7049 0.031 Uiso 1 1 calc R . . C12 C 0.2160(8) 0.6089(8) 0.5880(9) 0.0247(18) Uani 1 1 d U . . H5A H 0.1632 0.5582 0.5128 0.030 Uiso 1 1 calc R . . H5B H 0.2648 0.6622 0.5880 0.030 Uiso 1 1 calc R . . C13 C 0.2813(8) 0.5623(8) 0.6532(9) 0.0254(19) Uani 1 1 d U . . H3A H 0.3113 0.5305 0.6166 0.030 Uiso 1 1 calc R . . H3B H 0.3415 0.6145 0.7253 0.030 Uiso 1 1 calc R . . C14 C 0.0901(8) 0.6946(8) 0.5654(9) 0.0248(19) Uani 1 1 d U . . C15 C -0.2114(9) -0.0720(8) 0.2090(8) 0.0255(19) Uani 1 1 d U . . H1A H -0.2752 -0.0597 0.1954 0.031 Uiso 1 1 calc R . . H1B H -0.1764 -0.0337 0.1843 0.031 Uiso 1 1 calc R . . C16 C -0.1662(10) -0.1992(9) 0.1187(10) 0.037(2) Uani 1 1 d U . . H23A H -0.0947 -0.1665 0.1865 0.044 Uiso 1 1 calc R . . H23B H -0.1632 -0.1705 0.0709 0.044 Uiso 1 1 calc R . . C17 C -0.1970(11) -0.3098(10) 0.0654(11) 0.047(3) Uani 1 1 d U . . H25A H -0.1944 -0.3372 0.1158 0.057 Uiso 1 1 calc R . . H25B H -0.1448 -0.3203 0.0488 0.057 Uiso 1 1 calc R . . C18 C -0.3117(12) -0.3650(11) -0.0403(12) 0.054(3) Uani 1 1 d U . . H27A H -0.3093 -0.3415 -0.0926 0.064 Uiso 1 1 calc R . . C19 C -0.3951(12) -0.3393(11) -0.0213(12) 0.054(3) Uani 1 1 d U . . H26A H -0.4068 -0.3697 0.0222 0.064 Uiso 1 1 calc R . . H26B H -0.4640 -0.3671 -0.0911 0.064 Uiso 1 1 calc R . . C20 C -0.3567(11) -0.2263(10) 0.0371(10) 0.041(2) Uani 1 1 d U . . H24A H -0.3521 -0.1965 -0.0094 0.049 Uiso 1 1 calc R . . H24B H -0.4088 -0.2123 0.0519 0.049 Uiso 1 1 calc R . . C21 C -0.3373(14) -0.4796(13) -0.0883(13) 0.065(4) Uani 1 1 d U . . C22 C 0.5077(8) 0.2076(9) 0.8221(9) 0.027(2) Uani 1 1 d U . . C23 C 0.6026(9) 0.2045(9) 0.9135(9) 0.030(2) Uani 1 1 d U . . C24 C 0.7076(9) 0.2725(9) 0.9636(10) 0.037(2) Uani 1 1 d U . . H11A H 0.7209 0.3226 0.9425 0.045 Uiso 1 1 calc R . . C25 C 0.7939(10) 0.2665(10) 1.0457(10) 0.038(2) Uani 1 1 d U . . H13A H 0.8648 0.3125 1.0788 0.045 Uiso 1 1 calc R . . C26 C 0.7756(9) 0.1946(9) 1.0776(9) 0.031(2) Uani 1 1 d U . . C27 C 0.6710(9) 0.1277(10) 1.0306(10) 0.038(2) Uani 1 1 d U . . H37A H 0.6587 0.0803 1.0553 0.046 Uiso 1 1 calc R . . C28 C 0.5841(9) 0.1304(9) 0.9471(10) 0.035(2) Uani 1 1 d U . . H12A H 0.5137 0.0831 0.9133 0.042 Uiso 1 1 calc R . . C29 C 0.8711(9) 0.1900(9) 1.1694(9) 0.031(2) Uani 1 1 d U . . C30 C 0.4581(8) 0.3366(8) 0.5985(10) 0.0275(19) Uani 1 1 d U . . C31 C 0.5401(9) 0.4192(8) 0.6081(10) 0.031(2) Uani 1 1 d U . . C32 C 0.5495(9) 0.5172(8) 0.6450(10) 0.0293(19) Uani 1 1 d U . . H18A H 0.5039 0.5321 0.6656 0.035 Uiso 1 1 calc R . . C33 C 0.6252(9) 0.5917(9) 0.6513(10) 0.031(2) Uani 1 1 d U . . H19A H 0.6312 0.6570 0.6773 0.037 Uiso 1 1 calc R . . C34 C 0.6947(8) 0.5713(8) 0.6188(9) 0.0266(19) Uani 1 1 d U . . C35 C 0.6858(9) 0.4739(9) 0.5832(10) 0.033(2) Uani 1 1 d U . . H22A H 0.7327 0.4595 0.5643 0.039 Uiso 1 1 calc R . . C36 C 0.6081(9) 0.3970(9) 0.5752(10) 0.033(2) Uani 1 1 d U . . H35A H 0.6013 0.3315 0.5483 0.039 Uiso 1 1 calc R . . C37 C 0.7747(9) 0.6507(8) 0.6225(10) 0.029(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.0111(2) 0.0175(3) 0.0192(3) 0.0122(2) 0.0074(2) 0.0056(2) Ce2 0.0101(2) 0.0177(3) 0.0199(3) 0.0118(2) 0.0070(2) 0.0048(2) Ce3 0.0129(3) 0.0177(3) 0.0212(3) 0.0114(2) 0.0095(2) 0.0071(2) P1 0.0135(11) 0.0228(13) 0.0211(13) 0.0135(11) 0.0105(10) 0.0093(10) P2 0.0132(11) 0.0159(12) 0.0196(12) 0.0094(10) 0.0067(10) 0.0050(9) P3 0.0106(10) 0.0159(11) 0.0170(12) 0.0098(10) 0.0064(10) 0.0047(9) O1 0.0358(13) 0.0397(14) 0.0473(15) 0.0259(13) 0.0285(13) 0.0196(12) O2 0.0373(13) 0.0406(14) 0.0489(14) 0.0259(13) 0.0267(12) 0.0198(12) O3 0.0363(13) 0.0399(14) 0.0479(15) 0.0261(13) 0.0278(13) 0.0202(12) O4 0.034(2) 0.040(2) 0.054(2) 0.028(2) 0.0256(19) 0.0194(19) O5 0.035(2) 0.040(2) 0.047(2) 0.0279(19) 0.0273(18) 0.0213(18) O6 0.0349(15) 0.0389(16) 0.0466(16) 0.0284(14) 0.0284(14) 0.0209(14) O7 0.0345(15) 0.0388(16) 0.0467(16) 0.0273(14) 0.0286(14) 0.0213(14) O8 0.0336(16) 0.0384(17) 0.0468(17) 0.0269(15) 0.0297(14) 0.0210(15) O9 0.0365(17) 0.0398(17) 0.0490(18) 0.0298(16) 0.0272(15) 0.0209(15) O10 0.0344(17) 0.0391(17) 0.0477(18) 0.0272(16) 0.0278(15) 0.0224(15) O11 0.0361(13) 0.0393(14) 0.0470(15) 0.0266(13) 0.0288(13) 0.0192(12) O12 0.0358(14) 0.0393(14) 0.0475(15) 0.0256(13) 0.0282(13) 0.0206(12) O13 0.0356(14) 0.0390(14) 0.0470(15) 0.0264(13) 0.0286(13) 0.0197(12) O14 0.0397(12) 0.0423(13) 0.0510(13) 0.0234(12) 0.0253(12) 0.0186(11) O15 0.0395(12) 0.0419(13) 0.0507(13) 0.0242(12) 0.0253(12) 0.0184(11) O16 0.0389(16) 0.0415(16) 0.0503(17) 0.0279(15) 0.0231(15) 0.0186(14) O17 0.0369(16) 0.0419(16) 0.0481(17) 0.0282(15) 0.0264(15) 0.0180(15) O18 0.037(2) 0.048(3) 0.049(3) 0.032(2) 0.023(2) 0.018(2) O19 0.036(3) 0.043(3) 0.048(3) 0.033(2) 0.019(2) 0.019(2) O20 0.0370(15) 0.0412(16) 0.0500(16) 0.0272(14) 0.0284(14) 0.0188(14) O21 0.0391(16) 0.0426(16) 0.0494(16) 0.0258(15) 0.0300(14) 0.0158(15) O22 0.038(2) 0.042(2) 0.052(2) 0.028(2) 0.031(2) 0.016(2) O23 0.039(2) 0.043(2) 0.052(2) 0.025(2) 0.032(2) 0.013(2) O24 0.0376(10) 0.0412(11) 0.0492(12) 0.0261(10) 0.0270(10) 0.0193(9) O1W 0.0469(17) 0.0495(17) 0.0580(18) 0.0234(16) 0.0189(16) 0.0166(16) O2W 0.0417(18) 0.0460(18) 0.0520(19) 0.0259(17) 0.0230(17) 0.0176(17) O3W 0.181(12) 0.184(12) 0.143(11) 0.083(9) 0.091(9) 0.052(8) O4W 0.060(3) 0.064(3) 0.068(3) 0.020(2) 0.018(2) 0.013(2) O5W 0.058(2) 0.062(2) 0.069(3) 0.018(2) 0.020(2) 0.013(2) O6W 0.054(2) 0.057(2) 0.065(2) 0.021(2) 0.018(2) 0.014(2) O7W 0.058(2) 0.062(2) 0.067(2) 0.020(2) 0.019(2) 0.010(2) N1 0.019(4) 0.036(5) 0.028(5) 0.019(4) 0.015(4) 0.015(4) N2 0.014(4) 0.017(4) 0.021(4) 0.011(3) 0.006(4) 0.004(3) N3 0.026(5) 0.024(5) 0.028(5) 0.015(4) 0.012(4) 0.009(4) C1 0.019(4) 0.039(5) 0.036(5) 0.025(4) 0.017(4) 0.015(4) C2 0.022(3) 0.030(4) 0.039(4) 0.018(3) 0.017(3) 0.015(3) C3 0.023(3) 0.029(3) 0.037(4) 0.019(3) 0.017(3) 0.013(3) C4 0.023(3) 0.026(4) 0.036(4) 0.015(3) 0.015(3) 0.016(3) C5 0.021(3) 0.025(4) 0.036(4) 0.017(3) 0.017(3) 0.015(3) C6 0.020(3) 0.031(4) 0.037(4) 0.019(3) 0.017(3) 0.012(3) C7 0.023(4) 0.028(4) 0.036(4) 0.014(3) 0.018(3) 0.015(3) C8 0.017(4) 0.025(4) 0.034(4) 0.020(3) 0.011(3) 0.013(3) C9 0.024(3) 0.029(4) 0.033(4) 0.020(3) 0.018(3) 0.013(3) C10 0.024(3) 0.027(4) 0.036(4) 0.022(3) 0.020(3) 0.011(3) C11 0.026(3) 0.028(4) 0.032(4) 0.017(3) 0.019(3) 0.014(3) C12 0.022(3) 0.029(3) 0.034(4) 0.020(3) 0.019(3) 0.014(3) C13 0.023(3) 0.028(4) 0.037(4) 0.020(3) 0.019(3) 0.014(3) C14 0.021(4) 0.025(4) 0.035(4) 0.018(3) 0.017(3) 0.012(3) C15 0.034(4) 0.033(4) 0.024(4) 0.017(3) 0.020(3) 0.022(3) C16 0.041(4) 0.037(4) 0.029(4) 0.010(3) 0.019(3) 0.017(4) C17 0.048(4) 0.042(4) 0.035(4) 0.010(4) 0.016(4) 0.018(4) C18 0.052(5) 0.044(5) 0.037(4) 0.009(4) 0.013(4) 0.012(4) C19 0.050(5) 0.043(5) 0.036(4) 0.007(4) 0.013(4) 0.009(4) C20 0.042(4) 0.038(4) 0.031(4) 0.015(3) 0.013(4) 0.013(4) C21 0.052(5) 0.058(6) 0.045(5) 0.005(5) 0.015(5) 0.012(5) C22 0.020(3) 0.036(4) 0.027(4) 0.018(3) 0.010(3) 0.015(3) C23 0.021(3) 0.037(4) 0.029(4) 0.021(3) 0.009(3) 0.012(3) C24 0.027(3) 0.039(4) 0.033(3) 0.024(3) 0.005(3) 0.009(3) C25 0.027(3) 0.040(4) 0.032(3) 0.022(3) 0.005(3) 0.009(3) C26 0.024(3) 0.040(4) 0.027(3) 0.022(3) 0.007(3) 0.013(3) C27 0.025(3) 0.042(4) 0.033(4) 0.022(3) 0.005(3) 0.010(3) C28 0.022(3) 0.041(4) 0.033(3) 0.023(3) 0.007(3) 0.009(3) C29 0.023(4) 0.038(4) 0.030(4) 0.020(3) 0.009(3) 0.016(3) C30 0.022(3) 0.028(4) 0.038(4) 0.018(3) 0.020(3) 0.008(3) C31 0.027(3) 0.028(4) 0.040(4) 0.018(3) 0.021(3) 0.004(3) C32 0.023(3) 0.030(3) 0.041(4) 0.018(3) 0.022(3) 0.007(3) C33 0.026(3) 0.028(3) 0.041(4) 0.017(3) 0.020(3) 0.010(3) C34 0.023(3) 0.027(3) 0.037(4) 0.019(3) 0.021(3) 0.007(3) C35 0.026(3) 0.030(3) 0.043(4) 0.015(3) 0.023(3) 0.005(3) C36 0.027(3) 0.027(3) 0.042(3) 0.015(3) 0.020(3) 0.007(3) C37 0.023(3) 0.028(4) 0.038(4) 0.019(3) 0.019(3) 0.007(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 Ce1 O7 2.416(9) . ? Ce1 O11 2.480(8) . ? Ce1 O10 2.480(8) 2_566 ? Ce1 O23 2.537(8) 2_666 ? Ce1 O1 2.567(9) . ? Ce1 O22 2.608(8) 2_666 ? Ce1 O2 2.614(8) . ? Ce1 O19 2.621(8) 1_454 ? Ce1 O18 2.630(9) 1_454 ? Ce1 C37 2.936(10) 2_666 ? Ce1 C29 2.999(11) 1_454 ? Ce1 P1 3.197(3) . ? Ce2 O2 2.414(9) . ? Ce2 O13 2.488(8) 2_556 ? Ce2 O5 2.492(8) 2_656 ? Ce2 O20 2.540(8) . ? Ce2 O21 2.563(8) . ? Ce2 O17 2.567(8) . ? Ce2 O6 2.547(8) . ? Ce2 O7 2.608(8) . ? Ce2 O16 2.659(9) . ? Ce2 C30 2.926(10) . ? Ce2 C22 2.987(10) . ? Ce2 P2 3.177(3) . ? Ce3 O12 2.367(8) 2_556 ? Ce3 O8 2.474(8) . ? Ce3 O3 2.497(8) 2_556 ? Ce3 O4 2.519(8) 1_455 ? Ce3 O9 2.520(8) 2_566 ? Ce3 O24 2.530(9) . ? Ce3 O11 2.619(8) . ? Ce3 O13 2.617(9) . ? Ce3 P3 3.213(3) . ? P1 O3 1.495(8) . ? P1 O1 1.526(8) . ? P1 O2 1.520(9) . ? P1 C1 1.817(10) . ? P2 O8 1.505(8) . ? P2 O6 1.519(8) . ? P2 O7 1.522(9) . ? P2 C8 1.829(10) . ? P3 O12 1.506(8) . ? P3 O13 1.525(8) . ? P3 O11 1.540(9) . ? P3 C15 1.838(11) . ? O3 Ce3 2.497(8) 2_556 ? O4 C7 1.250(13) . ? O4 Ce3 2.519(8) 1_655 ? O5 C7 1.259(13) . ? O5 Ce2 2.492(8) 2_656 ? O9 C14 1.251(13) . ? O9 Ce3 2.520(8) 2_566 ? O10 C14 1.273(12) . ? O10 Ce1 2.480(8) 2_566 ? O12 Ce3 2.367(8) 2_556 ? O13 Ce2 2.488(8) 2_556 ? O14 C21 1.230(19) . ? O14 H21A 0.8495 . ? O15 C21 1.214(19) . ? O16 C22 1.236(14) . ? O17 C22 1.251(14) . ? O18 C29 1.249(14) . ? O18 Ce1 2.630(9) 1_656 ? O19 C29 1.278(14) . ? O19 Ce1 2.621(8) 1_656 ? O20 C30 1.267(14) . ? O21 C30 1.247(14) . ? O22 C37 1.274(14) . ? O22 Ce1 2.608(8) 2_666 ? O23 C37 1.249(14) . ? O23 Ce1 2.537(8) 2_666 ? O24 H24C 0.8482 . ? O24 H24D 0.8455 . ? O1W H1WA 0.8461 . ? O1W H1WB 0.8494 . ? O2W H2WA 0.8460 . ? O2W H2WB 0.8492 . ? O3W H3WC 0.8511 . ? O3W H3WB 0.8475 . ? O4W H4WA 0.8466 . ? O4W H4WB 0.8468 . ? O5W H5WA 0.8459 . ? O5W H5WB 0.8462 . ? O6W H6WA 0.8460 . ? O6W H6WB 0.8462 . ? O7W H7WC 0.8501 . ? O7W H7WB 0.8464 . ? N1 C2 1.463(13) . ? N1 C6 1.488(14) . ? N1 C1 1.499(12) . ? N1 H3C 0.8991 . ? N2 C13 1.486(12) . ? N2 C8 1.504(12) . ? N2 C9 1.478(13) . ? N2 H2C 0.9004 . ? N3 C20 1.490(15) . ? N3 C15 1.499(14) . ? N3 C16 1.500(15) . ? N3 H1C 0.8958 . ? C1 H28A 0.9700 . ? C1 H28B 0.9700 . ? C2 C3 1.525(14) . ? C2 H30A 0.9700 . ? C2 H30B 0.9700 . ? C3 C4 1.514(15) . ? C3 H32A 0.9700 . ? C3 H32B 0.9700 . ? C4 C7 1.540(14) . ? C4 C5 1.540(14) . ? C4 H33A 0.9800 . ? C5 C6 1.502(14) . ? C5 H31A 0.9700 . ? C5 H31B 0.9700 . ? C6 H29A 0.9700 . ? C6 H29B 0.9700 . ? C8 H2A 0.9700 . ? C8 H2B 0.9700 . ? C9 C10 1.501(14) . ? C9 H4A 0.9700 . ? C9 H4B 0.9700 . ? C10 C11 1.528(14) . ? C10 H6A 0.9700 . ? C10 H6B 0.9700 . ? C11 C12 1.509(14) . ? C11 C14 1.517(14) . ? C11 H7A 0.9800 . ? C12 C13 1.523(14) . ? C12 H5A 0.9700 . ? C12 H5B 0.9700 . ? C13 H3A 0.9700 . ? C13 H3B 0.9700 . ? C15 H1A 0.9700 . ? C15 H1B 0.9700 . ? C16 C17 1.502(18) . ? C16 H23A 0.9700 . ? C16 H23B 0.9700 . ? C17 C18 1.535(19) . ? C17 H25A 0.9700 . ? C17 H25B 0.9700 . ? C18 C19 1.53(2) . ? C18 C21 1.57(2) . ? C18 H27A 0.9800 . ? C19 C20 1.522(19) . ? C19 H26A 0.9700 . ? C19 H26B 0.9700 . ? C20 H24A 0.9700 . ? C20 H24B 0.9700 . ? C22 C23 1.509(14) . ? C23 C24 1.374(16) . ? C23 C28 1.397(16) . ? C24 C25 1.390(16) . ? C24 H11A 0.9300 . ? C25 C26 1.350(16) . ? C25 H13A 0.9300 . ? C26 C27 1.373(16) . ? C26 C29 1.530(14) . ? C27 C28 1.379(15) . ? C27 H37A 0.9300 . ? C28 H12A 0.9300 . ? C29 Ce1 2.999(11) 1_656 ? C30 C31 1.475(14) . ? C31 C36 1.408(16) . ? C31 C32 1.392(16) . ? C32 C33 1.368(14) . ? C32 H18A 0.9300 . ? C33 C34 1.417(15) . ? C33 H19A 0.9300 . ? C34 C35 1.385(16) . ? C34 C37 1.477(13) . ? C35 C36 1.395(15) . ? C35 H22A 0.9300 . ? C36 H35A 0.9300 . ? C37 Ce1 2.936(10) 2_666 ? 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 O7 Ce1 O11 77.0(3) . . ? O7 Ce1 O10 74.6(3) . 2_566 ? O11 Ce1 O10 80.4(3) . 2_566 ? O7 Ce1 O23 78.7(3) . 2_666 ? O11 Ce1 O23 145.8(3) . 2_666 ? O10 Ce1 O23 70.1(3) 2_566 2_666 ? O7 Ce1 O1 118.8(3) . . ? O11 Ce1 O1 82.2(3) . . ? O10 Ce1 O1 154.8(3) 2_566 . ? O23 Ce1 O1 131.1(3) 2_666 . ? O7 Ce1 O22 100.5(3) . 2_666 ? O11 Ce1 O22 158.5(3) . 2_666 ? O10 Ce1 O22 119.9(3) 2_566 2_666 ? O23 Ce1 O22 50.7(3) 2_666 2_666 ? O1 Ce1 O22 80.5(3) . 2_666 ? O7 Ce1 O2 65.9(3) . . ? O11 Ce1 O2 87.2(3) . . ? O10 Ce1 O2 140.3(3) 2_566 . ? O23 Ce1 O2 104.3(3) 2_666 . ? O1 Ce1 O2 56.1(3) . . ? O22 Ce1 O2 72.6(3) 2_666 . ? O7 Ce1 O19 139.0(3) . 1_454 ? O11 Ce1 O19 71.2(3) . 1_454 ? O10 Ce1 O19 75.2(3) 2_566 1_454 ? O23 Ce1 O19 115.5(3) 2_666 1_454 ? O1 Ce1 O19 82.0(3) . 1_454 ? O22 Ce1 O19 118.4(3) 2_666 1_454 ? O2 Ce1 O19 135.5(3) . 1_454 ? O7 Ce1 O18 150.2(3) . 1_454 ? O11 Ce1 O18 120.8(3) . 1_454 ? O10 Ce1 O18 84.7(3) 2_566 1_454 ? O23 Ce1 O18 74.2(3) 2_666 1_454 ? O1 Ce1 O18 88.8(3) . 1_454 ? O22 Ce1 O18 71.4(3) 2_666 1_454 ? O2 Ce1 O18 133.1(3) . 1_454 ? O19 Ce1 O18 49.6(3) 1_454 1_454 ? O7 Ce1 C37 89.8(3) . 2_666 ? O11 Ce1 C37 166.7(3) . 2_666 ? O10 Ce1 C37 94.6(3) 2_566 2_666 ? O23 Ce1 C37 25.0(3) 2_666 2_666 ? O1 Ce1 C37 106.1(3) . 2_666 ? O22 Ce1 C37 25.7(3) 2_666 2_666 ? O2 Ce1 C37 88.9(3) . 2_666 ? O19 Ce1 C37 119.7(3) 1_454 2_666 ? O18 Ce1 C37 70.5(3) 1_454 2_666 ? O7 Ce1 C29 152.3(3) . 1_454 ? O11 Ce1 C29 96.3(3) . 1_454 ? O10 Ce1 C29 77.8(3) 2_566 1_454 ? O23 Ce1 C29 94.1(3) 2_666 1_454 ? O1 Ce1 C29 86.2(3) . 1_454 ? O22 Ce1 C29 95.1(3) 2_666 1_454 ? O2 Ce1 C29 141.4(3) . 1_454 ? O19 Ce1 C29 25.2(3) 1_454 1_454 ? O18 Ce1 C29 24.5(3) 1_454 1_454 ? C37 Ce1 C29 94.6(3) 2_666 1_454 ? O7 Ce1 P1 92.78(19) . . ? O11 Ce1 P1 85.3(2) . . ? O10 Ce1 P1 162.67(19) 2_566 . ? O23 Ce1 P1 119.7(2) 2_666 . ? O1 Ce1 P1 28.08(19) . . ? O22 Ce1 P1 73.5(2) 2_666 . ? O2 Ce1 P1 28.1(2) . . ? O19 Ce1 P1 109.4(2) 1_454 . ? O18 Ce1 P1 111.2(2) 1_454 . ? C37 Ce1 P1 97.2(2) 2_666 . ? C29 Ce1 P1 113.6(2) 1_454 . ? O2 Ce2 O13 79.1(3) . 2_556 ? O2 Ce2 O5 76.6(3) . 2_656 ? O13 Ce2 O5 80.4(3) 2_556 2_656 ? O2 Ce2 O20 96.6(3) . . ? O13 Ce2 O20 156.0(3) 2_556 . ? O5 Ce2 O20 122.0(3) 2_656 . ? O2 Ce2 O21 80.8(3) . . ? O13 Ce2 O21 148.6(3) 2_556 . ? O5 Ce2 O21 71.6(3) 2_656 . ? O20 Ce2 O21 50.6(3) . . ? O2 Ce2 O17 142.5(3) . . ? O13 Ce2 O17 71.8(3) 2_556 . ? O5 Ce2 O17 75.7(3) 2_656 . ? O20 Ce2 O17 119.4(3) . . ? O21 Ce2 O17 113.2(3) . . ? O2 Ce2 O6 119.3(3) . . ? O13 Ce2 O6 80.0(3) 2_556 . ? O5 Ce2 O6 151.6(3) 2_656 . ? O20 Ce2 O6 81.7(3) . . ? O21 Ce2 O6 131.2(3) . . ? O17 Ce2 O6 78.7(3) . . ? O2 Ce2 O7 66.0(3) . . ? O13 Ce2 O7 86.5(3) 2_556 . ? O5 Ce2 O7 142.0(3) 2_656 . ? O20 Ce2 O7 70.4(3) . . ? O21 Ce2 O7 106.9(3) . . ? O17 Ce2 O7 133.1(3) . . ? O6 Ce2 O7 56.4(3) . . ? O2 Ce2 O16 153.2(3) . . ? O13 Ce2 O16 120.6(3) 2_556 . ? O5 Ce2 O16 88.5(3) 2_656 . ? O20 Ce2 O16 72.5(3) . . ? O21 Ce2 O16 73.4(3) . . ? O17 Ce2 O16 48.9(3) . . ? O6 Ce2 O16 84.0(3) . . ? O7 Ce2 O16 128.4(3) . . ? O2 Ce2 C30 90.2(3) . . ? O13 Ce2 C30 169.3(3) 2_556 . ? O5 Ce2 C30 96.4(3) 2_656 . ? O20 Ce2 C30 25.6(3) . . ? O21 Ce2 C30 25.1(3) . . ? O17 Ce2 C30 117.5(3) . . ? O6 Ce2 C30 106.3(3) . . ? O7 Ce2 C30 90.0(3) . . ? O16 Ce2 C30 69.3(3) . . ? O2 Ce2 C22 156.9(3) . . ? O13 Ce2 C22 96.4(3) 2_556 . ? O5 Ce2 C22 80.3(3) 2_656 . ? O20 Ce2 C22 96.2(3) . . ? O21 Ce2 C22 92.7(3) . . ? O17 Ce2 C22 24.6(3) . . ? O6 Ce2 C22 81.6(3) . . ? O7 Ce2 C22 136.8(3) . . ? O16 Ce2 C22 24.4(3) . . ? C30 Ce2 C22 93.1(3) . . ? O2 Ce2 P2 93.4(2) . . ? O13 Ce2 P2 84.18(19) 2_556 . ? O5 Ce2 P2 162.91(19) 2_656 . ? O20 Ce2 P2 72.4(2) . . ? O21 Ce2 P2 121.0(2) . . ? O17 Ce2 P2 106.4(2) . . ? O6 Ce2 P2 28.11(18) . . ? O7 Ce2 P2 28.38(19) . . ? O16 Ce2 P2 105.8(2) . . ? C30 Ce2 P2 97.4(2) . . ? C22 Ce2 P2 108.8(2) . . ? O12 Ce3 O8 73.9(3) 2_556 . ? O12 Ce3 O3 73.3(3) 2_556 2_556 ? O8 Ce3 O3 109.2(3) . 2_556 ? O12 Ce3 O4 142.2(3) 2_556 1_455 ? O8 Ce3 O4 143.4(3) . 1_455 ? O3 Ce3 O4 84.4(3) 2_556 1_455 ? O12 Ce3 O9 141.6(3) 2_556 2_566 ? O8 Ce3 O9 79.8(3) . 2_566 ? O3 Ce3 O9 143.0(3) 2_556 2_566 ? O4 Ce3 O9 70.4(3) 1_455 2_566 ? O12 Ce3 O24 121.7(3) 2_556 . ? O8 Ce3 O24 74.5(3) . . ? O3 Ce3 O24 72.6(3) 2_556 . ? O4 Ce3 O24 77.9(3) 1_455 . ? O9 Ce3 O24 75.8(3) 2_566 . ? O12 Ce3 O11 77.6(3) 2_556 . ? O8 Ce3 O11 89.3(3) . . ? O3 Ce3 O11 139.1(3) 2_556 . ? O4 Ce3 O11 102.3(3) 1_455 . ? O9 Ce3 O11 74.5(3) 2_566 . ? O24 Ce3 O11 148.3(3) . . ? O12 Ce3 O13 76.8(3) 2_556 . ? O8 Ce3 O13 138.5(2) . . ? O3 Ce3 O13 89.5(3) 2_556 . ? O4 Ce3 O13 72.8(3) 1_455 . ? O9 Ce3 O13 107.4(3) 2_566 . ? O24 Ce3 O13 146.9(3) . . ? O11 Ce3 O13 55.7(3) . . ? O12 Ce3 P3 71.1(2) 2_556 . ? O8 Ce3 P3 112.73(19) . . ? O3 Ce3 P3 112.9(2) 2_556 . ? O4 Ce3 P3 91.0(2) 1_455 . ? O9 Ce3 P3 94.7(2) 2_566 . ? O24 Ce3 P3 167.2(2) . . ? O11 Ce3 P3 28.37(18) . . ? O13 Ce3 P3 28.01(17) . . ? O3 P1 O1 117.8(5) . . ? O3 P1 O2 113.5(5) . . ? O1 P1 O2 106.3(5) . . ? O3 P1 C1 109.0(5) . . ? O1 P1 C1 104.9(5) . . ? O2 P1 C1 104.2(5) . . ? O3 P1 Ce1 139.4(3) . . ? O1 P1 Ce1 52.3(3) . . ? O2 P1 Ce1 54.1(3) . . ? C1 P1 Ce1 111.5(4) . . ? O8 P2 O6 117.6(4) . . ? O8 P2 O7 114.2(5) . . ? O6 P2 O7 106.4(5) . . ? O8 P2 C8 109.1(5) . . ? O6 P2 C8 102.4(5) . . ? O7 P2 C8 106.0(5) . . ? O8 P2 Ce2 141.5(3) . . ? O6 P2 Ce2 52.2(3) . . ? O7 P2 Ce2 54.5(3) . . ? C8 P2 Ce2 109.5(3) . . ? O12 P3 O13 113.4(5) . . ? O12 P3 O11 114.9(5) . . ? O13 P3 O11 106.0(5) . . ? O12 P3 C15 106.5(5) . . ? O13 P3 C15 109.8(5) . . ? O11 P3 C15 106.0(5) . . ? O12 P3 Ce3 121.5(4) . . ? O13 P3 Ce3 53.7(3) . . ? O11 P3 Ce3 53.9(3) . . ? C15 P3 Ce3 131.9(3) . . ? P1 O1 Ce1 99.6(4) . . ? P1 O2 Ce2 147.4(5) . . ? P1 O2 Ce1 97.8(4) . . ? Ce2 O2 Ce1 113.5(3) . . ? P1 O3 Ce3 133.8(5) . 2_556 ? C7 O4 Ce3 134.8(7) . 1_655 ? C7 O5 Ce2 124.3(7) . 2_656 ? P2 O6 Ce2 99.7(4) . . ? P2 O7 Ce1 148.4(5) . . ? P2 O7 Ce2 97.1(4) . . ? Ce1 O7 Ce2 113.6(3) . . ? P2 O8 Ce3 131.7(5) . . ? C14 O9 Ce3 137.0(7) . 2_566 ? C14 O10 Ce1 128.2(7) . 2_566 ? P3 O11 Ce1 134.4(5) . . ? P3 O11 Ce3 97.7(4) . . ? Ce1 O11 Ce3 127.4(3) . . ? P3 O12 Ce3 167.4(6) . 2_556 ? P3 O13 Ce2 135.9(5) . 2_556 ? P3 O13 Ce3 98.3(4) . . ? Ce2 O13 Ce3 125.5(3) 2_556 . ? C21 O14 H21A 118.5 . . ? C22 O16 Ce2 92.8(7) . . ? C22 O17 Ce2 96.9(7) . . ? C29 O18 Ce1 94.5(7) . 1_656 ? C29 O19 Ce1 94.2(7) . 1_656 ? C30 O20 Ce2 94.5(7) . . ? C30 O21 Ce2 94.0(7) . . ? C37 O22 Ce1 91.7(7) . 2_666 ? C37 O23 Ce1 95.7(7) . 2_666 ? Ce3 O24 H24C 109.6 . . ? Ce3 O24 H24D 109.1 . . ? H24C O24 H24D 109.5 . . ? H1WA O1W H1WB 109.3 . . ? H2WA O2W H2WB 109.4 . . ? H3WC O3W H3WB 110.0 . . ? H4WA O4W H4WB 109.5 . . ? H5WA O5W H5WB 109.4 . . ? H6WA O6W H6WB 109.4 . . ? H7WC O7W H7WB 109.9 . . ? C2 N1 C6 111.8(8) . . ? C2 N1 C1 111.7(8) . . ? C6 N1 C1 111.9(8) . . ? C2 N1 H3C 107.2 . . ? C6 N1 H3C 106.6 . . ? C1 N1 H3C 107.3 . . ? C13 N2 C8 111.2(7) . . ? C13 N2 C9 112.1(8) . . ? C8 N2 C9 111.0(8) . . ? C13 N2 H2C 107.1 . . ? C8 N2 H2C 107.7 . . ? C9 N2 H2C 107.4 . . ? C20 N3 C15 112.7(9) . . ? C20 N3 C16 109.7(9) . . ? C15 N3 C16 111.4(8) . . ? C20 N3 H1C 107.1 . . ? C15 N3 H1C 107.9 . . ? C16 N3 H1C 107.9 . . ? N1 C1 P1 114.9(7) . . ? N1 C1 H28A 108.5 . . ? P1 C1 H28A 108.5 . . ? N1 C1 H28B 108.5 . . ? P1 C1 H28B 108.5 . . ? H28A C1 H28B 107.5 . . ? N1 C2 C3 112.4(9) . . ? N1 C2 H30A 109.1 . . ? C3 C2 H30A 109.1 . . ? N1 C2 H30B 109.1 . . ? C3 C2 H30B 109.1 . . ? H30A C2 H30B 107.9 . . ? C4 C3 C2 111.1(9) . . ? C4 C3 H32A 109.4 . . ? C2 C3 H32A 109.4 . . ? C4 C3 H32B 109.4 . . ? C2 C3 H32B 109.4 . . ? H32A C3 H32B 108.0 . . ? C7 C4 C3 112.1(9) . . ? C7 C4 C5 112.9(9) . . ? C3 C4 C5 111.7(9) . . ? C7 C4 H33A 106.5 . . ? C3 C4 H33A 106.5 . . ? C5 C4 H33A 106.5 . . ? C6 C5 C4 112.5(9) . . ? C6 C5 H31A 109.1 . . ? C4 C5 H31A 109.1 . . ? C6 C5 H31B 109.1 . . ? C4 C5 H31B 109.1 . . ? H31A C5 H31B 107.8 . . ? N1 C6 C5 112.5(9) . . ? N1 C6 H29A 109.1 . . ? C5 C6 H29A 109.1 . . ? N1 C6 H29B 109.1 . . ? C5 C6 H29B 109.1 . . ? H29A C6 H29B 107.8 . . ? O4 C7 O5 125.1(10) . . ? O4 C7 C4 116.6(10) . . ? O5 C7 C4 118.3(10) . . ? N2 C8 P2 113.0(7) . . ? N2 C8 H2A 109.0 . . ? P2 C8 H2A 109.0 . . ? N2 C8 H2B 109.0 . . ? P2 C8 H2B 109.0 . . ? H2A C8 H2B 107.8 . . ? N2 C9 C10 113.3(9) . . ? N2 C9 H4A 108.9 . . ? C10 C9 H4A 108.9 . . ? N2 C9 H4B 108.9 . . ? C10 C9 H4B 108.9 . . ? H4A C9 H4B 107.7 . . ? C11 C10 C9 112.6(8) . . ? C11 C10 H6A 109.1 . . ? C9 C10 H6A 109.1 . . ? C11 C10 H6B 109.1 . . ? C9 C10 H6B 109.1 . . ? H6A C10 H6B 107.8 . . ? C10 C11 C12 112.2(9) . . ? C10 C11 C14 113.6(9) . . ? C12 C11 C14 112.3(9) . . ? C10 C11 H7A 106.0 . . ? C12 C11 H7A 106.0 . . ? C14 C11 H7A 106.0 . . ? C13 C12 C11 113.0(9) . . ? C13 C12 H5A 109.0 . . ? C11 C12 H5A 109.0 . . ? C13 C12 H5B 109.0 . . ? C11 C12 H5B 109.0 . . ? H5A C12 H5B 107.8 . . ? N2 C13 C12 110.9(8) . . ? N2 C13 H3A 109.5 . . ? C12 C13 H3A 109.5 . . ? N2 C13 H3B 109.5 . . ? C12 C13 H3B 109.5 . . ? H3A C13 H3B 108.0 . . ? O9 C14 O10 123.8(10) . . ? O9 C14 C11 118.3(9) . . ? O10 C14 C11 117.8(9) . . ? N3 C15 P3 115.3(7) . . ? N3 C15 H1A 108.5 . . ? P3 C15 H1A 108.5 . . ? N3 C15 H1B 108.5 . . ? P3 C15 H1B 108.5 . . ? H1A C15 H1B 107.5 . . ? N3 C16 C17 110.2(11) . . ? N3 C16 H23A 109.6 . . ? C17 C16 H23A 109.6 . . ? N3 C16 H23B 109.6 . . ? C17 C16 H23B 109.6 . . ? H23A C16 H23B 108.1 . . ? C16 C17 C18 111.3(12) . . ? C16 C17 H25A 109.4 . . ? C18 C17 H25A 109.4 . . ? C16 C17 H25B 109.4 . . ? C18 C17 H25B 109.4 . . ? H25A C17 H25B 108.0 . . ? C19 C18 C21 115.4(13) . . ? C19 C18 C17 111.5(12) . . ? C21 C18 C17 107.4(12) . . ? C19 C18 H27A 107.4 . . ? C21 C18 H27A 107.4 . . ? C17 C18 H27A 107.4 . . ? C18 C19 C20 111.3(12) . . ? C18 C19 H26A 109.4 . . ? C20 C19 H26A 109.4 . . ? C18 C19 H26B 109.4 . . ? C20 C19 H26B 109.4 . . ? H26A C19 H26B 108.0 . . ? N3 C20 C19 110.3(11) . . ? N3 C20 H24A 109.6 . . ? C19 C20 H24A 109.6 . . ? N3 C20 H24B 109.6 . . ? C19 C20 H24B 109.6 . . ? H24A C20 H24B 108.1 . . ? O15 C21 O14 127.3(16) . . ? O15 C21 C18 112.4(15) . . ? O14 C21 C18 120.0(15) . . ? O17 C22 O16 121.2(10) . . ? O17 C22 C23 118.6(10) . . ? O16 C22 C23 119.9(10) . . ? O17 C22 Ce2 58.6(6) . . ? O16 C22 Ce2 62.8(6) . . ? C23 C22 Ce2 169.8(8) . . ? C24 C23 C28 119.0(10) . . ? C24 C23 C22 121.3(10) . . ? C28 C23 C22 119.7(10) . . ? C23 C24 C25 120.3(11) . . ? C23 C24 H11A 119.9 . . ? C25 C24 H11A 119.9 . . ? C26 C25 C24 120.4(11) . . ? C26 C25 H13A 119.8 . . ? C24 C25 H13A 119.8 . . ? C25 C26 C27 120.2(11) . . ? C25 C26 C29 119.9(10) . . ? C27 C26 C29 119.9(10) . . ? C26 C27 C28 120.5(11) . . ? C26 C27 H37A 119.7 . . ? C28 C27 H37A 119.7 . . ? C27 C28 C23 119.6(11) . . ? C27 C28 H12A 120.2 . . ? C23 C28 H12A 120.2 . . ? O18 C29 O19 121.4(10) . . ? O18 C29 C26 120.3(10) . . ? O19 C29 C26 118.3(10) . . ? O18 C29 Ce1 60.9(6) . 1_656 ? O19 C29 Ce1 60.6(6) . 1_656 ? C26 C29 Ce1 173.9(9) . 1_656 ? O21 C30 O20 120.4(10) . . ? O21 C30 C31 121.2(10) . . ? O20 C30 C31 118.4(10) . . ? O21 C30 Ce2 60.9(6) . . ? O20 C30 Ce2 59.9(6) . . ? C31 C30 Ce2 171.1(8) . . ? C36 C31 C32 119.2(10) . . ? C36 C31 C30 118.7(10) . . ? C32 C31 C30 122.0(10) . . ? C33 C32 C31 120.6(11) . . ? C33 C32 H18A 119.7 . . ? C31 C32 H18A 119.7 . . ? C34 C33 C32 121.2(11) . . ? C34 C33 H19A 119.4 . . ? C32 C33 H19A 119.4 . . ? C33 C34 C35 118.0(10) . . ? C33 C34 C37 121.6(10) . . ? C35 C34 C37 120.4(10) . . ? C36 C35 C34 121.3(11) . . ? C36 C35 H22A 119.3 . . ? C34 C35 H22A 119.3 . . ? C35 C36 C31 119.6(11) . . ? C35 C36 H35A 120.2 . . ? C31 C36 H35A 120.2 . . ? O23 C37 O22 121.9(10) . . ? O23 C37 C34 118.4(10) . . ? O22 C37 C34 119.7(10) . . ? O23 C37 Ce1 59.3(6) . 2_666 ? O22 C37 Ce1 62.6(6) . 2_666 ? C34 C37 Ce1 176.3(8) . 2_666 ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 2.684 _refine_diff_density_min -4.982 _refine_diff_density_rms 0.265 # Attachment 'szg168.cif' data_szg168 _database_code_depnum_ccdc_archive 'CCDC 849253' #TrackingRef 'szg168.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H61 N3 O31 P3 Pr3' _chemical_formula_weight 1559.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.122(3) _cell_length_b 15.167(4) _cell_length_c 15.242(3) _cell_angle_alpha 106.199(4) _cell_angle_beta 103.350(4) _cell_angle_gamma 116.990(4) _cell_volume 2717.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 624 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 19.84 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 2.830 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4552 _exptl_absorpt_correction_T_max 0.8485 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Smart Apex II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11818 _diffrn_reflns_av_R_equivalents 0.0838 _diffrn_reflns_av_sigmaI/netI 0.1676 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 23.29 _reflns_number_total 7725 _reflns_number_gt 4398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7725 _refine_ls_number_parameters 694 _refine_ls_number_restraints 306 _refine_ls_R_factor_all 0.1403 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.2131 _refine_ls_wR_factor_gt 0.1694 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.18107(8) 0.88572(8) 0.31789(8) 0.0211(3) Uani 1 1 d . . . Pr2 Pr 0.55711(8) 0.86584(8) 0.69764(8) 0.0208(3) Uani 1 1 d . . . Pr3 Pr 0.58479(8) 0.93663(8) 0.35524(8) 0.0214(3) Uani 1 1 d . . . P1 P 0.6167(4) 1.1424(4) 0.5236(4) 0.0218(11) Uani 1 1 d . . . P2 P 0.3051(4) 0.8258(4) 0.1963(3) 0.0225(12) Uani 1 1 d . . . P3 P 0.6253(4) 0.8084(4) 0.5185(4) 0.0242(12) Uani 1 1 d . . . O1 O 0.5582(9) 1.0983(9) 0.4113(8) 0.019(3) Uani 1 1 d U . . O2 O 0.5452(9) 1.1263(9) 0.5798(9) 0.024(3) Uani 1 1 d . . . O3 O 0.6825(9) 1.0914(10) 0.5375(8) 0.027(3) Uani 1 1 d . . . O4 O 0.9266(16) 1.6076(18) 1.0338(13) 0.108(8) Uani 1 1 d . . . O5 O 0.774(2) 1.603(2) 1.0014(17) 0.148(11) Uani 1 1 d . . . H5C H 0.7991 1.6269 1.0653 0.223 Uiso 1 1 d R . . O6 O 0.2207(9) 0.7515(9) 0.2260(8) 0.020(3) Uani 1 1 d U . . O7 O 0.3285(9) 0.9421(9) 0.2479(8) 0.024(3) Uani 1 1 d U . . O8 O 0.4075(9) 0.8257(10) 0.2134(8) 0.026(3) Uani 1 1 d . . . O9 O 0.5020(10) 0.9500(9) -0.1811(9) 0.028(3) Uani 1 1 d . . . O10 O 0.3718(12) 0.9736(12) -0.2436(10) 0.043(4) Uani 1 1 d . . . O11 O 0.6134(10) 0.8163(9) 0.4213(8) 0.025(3) Uani 1 1 d . . . O12 O 0.6879(8) 0.9223(9) 0.6101(8) 0.022(3) Uani 1 1 d . . . O13 O 0.5236(8) 0.7358(9) 0.5298(8) 0.020(3) Uani 1 1 d . . . O14 O 1.2135(10) 0.9619(11) 0.5971(9) 0.038(4) Uani 1 1 d . . . O15 O 1.1357(10) 0.9604(10) 0.4544(9) 0.029(3) Uani 1 1 d . . . O16 O 0.0858(10) 0.7254(10) 0.3623(9) 0.033(3) Uani 1 1 d . . . O17 O -0.0213(11) 0.7092(11) 0.2256(10) 0.041(4) Uani 1 1 d . . . O18 O -0.3512(10) 0.2824(11) 0.3585(10) 0.038(4) Uani 1 1 d U . . O19 O -0.4647(11) 0.3057(11) 0.2643(11) 0.045(4) Uani 1 1 d . . . O20 O 0.0582(11) 0.9468(11) 0.2553(9) 0.038(4) Uani 1 1 d . . . O21 O 0.0979(11) 0.8642(12) 0.1457(10) 0.045(4) Uani 1 1 d . . . O22 O -0.3012(10) 0.8206(11) -0.2411(10) 0.037(4) Uani 1 1 d . . . O23 O -0.3183(11) 0.9275(12) -0.1260(10) 0.044(4) Uani 1 1 d . . . O24 O 0.5959(13) 0.8046(13) 0.2221(11) 0.066(5) Uani 1 1 d . . . H24C H 0.6572 0.8394 0.2180 0.079 Uiso 1 1 d R . . H24A H 0.5908 0.7527 0.2376 0.099 Uiso 1 1 d R . . O1W O 0.8326(13) 0.2576(13) 0.4024(13) 0.076(5) Uani 1 1 d . . . H1WA H 0.8297 0.2379 0.4500 0.114 Uiso 1 1 d R . . H1WB H 0.8016 0.2008 0.3471 0.114 Uiso 1 1 d R . . O2W O 0.401(2) 0.5192(17) 0.490(2) 0.176(13) Uani 1 1 d . . . H2WB H 0.4708 0.5545 0.5112 0.212 Uiso 1 1 d R . . H2WA H 0.3823 0.5075 0.5366 0.265 Uiso 1 1 d R . . O3W O 0.659(3) 0.608(3) 0.696(3) 0.259(18) Uani 1 1 d U . . H3WA H 0.7265 0.6507 0.7095 0.311 Uiso 1 1 d R . . H3WB H 0.6362 0.5426 0.6568 0.389 Uiso 1 1 d R . . O4W O 0.583(4) 0.611(3) 0.206(3) 0.299(13) Uani 1 1 d U . . H4WA H 0.5968 0.5880 0.2495 0.448 Uiso 1 1 d R . . H4WB H 0.5475 0.5576 0.1470 0.448 Uiso 1 1 d R . . O5W O 0.795(8) 0.776(8) 0.198(7) 0.70(2) Uani 1 1 d U . . H5WA H 0.8301 0.8205 0.1768 0.844 Uiso 1 1 d R . . H5WB H 0.7619 0.7099 0.1539 1.055 Uiso 1 1 d R . . O6W O 0.028(3) 0.677(3) 0.685(3) 0.291(15) Uani 1 1 d U . . H6WA H -0.0047 0.7036 0.7087 0.437 Uiso 1 1 d R . . H6WB H -0.0148 0.6066 0.6560 0.437 Uiso 1 1 d R . . O7W O 0.493(4) 0.471(3) 0.288(3) 0.29(2) Uani 1 1 d U . . H7WA H 0.4836 0.4397 0.3266 0.429 Uiso 1 1 d R . . H7WB H 0.4612 0.4229 0.2270 0.429 Uiso 1 1 d R . . N1 N 0.7453(14) 1.3586(14) 0.6773(12) 0.040(5) Uani 1 1 d . . . H1C H 0.7513 1.3191 0.7111 0.048 Uiso 1 1 d R . . N2 N 0.2873(11) 0.8346(12) 0.0132(10) 0.024(4) Uani 1 1 d U . . H2A H 0.3417 0.9033 0.0608 0.029 Uiso 1 1 d R . . N3 N 0.8221(12) 0.8225(12) 0.5409(11) 0.031(4) Uani 1 1 d . . . H3C H 0.8394 0.8918 0.5558 0.037 Uiso 1 1 d R . . C1 C 0.7085(14) 1.2898(14) 0.5678(12) 0.024(4) Uani 1 1 d U . . H1A H 0.6731 1.3145 0.5284 0.028 Uiso 1 1 d R . . H1B H 0.7734 1.3043 0.5569 0.028 Uiso 1 1 d R . . C2 C 0.8532(16) 1.4656(17) 0.7238(15) 0.046(5) Uani 1 1 d U . . H2B H 0.8461 1.5124 0.6941 0.055 Uiso 1 1 d R . . H2C H 0.9063 1.4529 0.7091 0.055 Uiso 1 1 d R . . C3 C 0.8953(19) 1.5259(19) 0.8369(16) 0.062(6) Uani 1 1 d U . . H3A H 0.9657 1.5949 0.8654 0.075 Uiso 1 1 d R . . H3B H 0.9041 1.4799 0.8668 0.075 Uiso 1 1 d R . . C4 C 0.8070(19) 1.5443(19) 0.8629(18) 0.064(5) Uani 1 1 d U . . H4A H 0.8048 1.5973 0.8401 0.076 Uiso 1 1 d R . . C5 C 0.6944(17) 1.4362(17) 0.8066(15) 0.047(5) Uani 1 1 d U . . H5A H 0.6412 1.4515 0.8169 0.057 Uiso 1 1 d R . . H5B H 0.6940 1.3861 0.8349 0.057 Uiso 1 1 d R . . C6 C 0.6620(16) 1.3817(17) 0.6943(15) 0.040(5) Uani 1 1 d U . . H6A H 0.5892 1.3147 0.6599 0.048 Uiso 1 1 d R . . H6B H 0.6622 1.4323 0.6667 0.048 Uiso 1 1 d R . . C7 C 0.842(3) 1.589(2) 0.976(2) 0.076(7) Uani 1 1 d U . . C8 C 0.2253(14) 0.7730(16) 0.0608(12) 0.030(5) Uani 1 1 d . . . H8A H 0.1626 0.7783 0.0521 0.036 Uiso 1 1 d R . . H8B H 0.1982 0.6964 0.0273 0.036 Uiso 1 1 d R . . C9 C 0.3395(15) 0.7809(15) -0.0313(13) 0.025(4) Uani 1 1 d U . . H9A H 0.2820 0.7068 -0.0809 0.030 Uiso 1 1 d R . . H9B H 0.3861 0.7770 0.0213 0.030 Uiso 1 1 d R . . C10 C 0.4073(15) 0.8467(15) -0.0758(13) 0.027(4) Uani 1 1 d U . . H10A H 0.4343 0.8065 -0.1074 0.033 Uiso 1 1 d R . . H10B H 0.4702 0.9173 -0.0244 0.033 Uiso 1 1 d R . . C11 C 0.3421(14) 0.8653(15) -0.1518(13) 0.021(3) Uani 1 1 d U . . H11A H 0.2859 0.7937 -0.2062 0.025 Uiso 1 1 d R . . C12 C 0.2835(14) 0.9119(15) -0.1096(13) 0.024(4) Uani 1 1 d U . . H12A H 0.2338 0.9118 -0.1632 0.029 Uiso 1 1 d R . . H12B H 0.3372 0.9873 -0.0607 0.029 Uiso 1 1 d R . . C13 C 0.2218(14) 0.8481(16) -0.0617(13) 0.027(4) Uani 1 1 d U . . H13A H 0.1901 0.8837 -0.0322 0.032 Uiso 1 1 d R . . H13B H 0.1625 0.7750 -0.1119 0.032 Uiso 1 1 d R . . C14 C 0.4087(15) 0.9324(15) -0.1953(13) 0.023(4) Uani 1 1 d U . . C15 C 0.7094(14) 0.7536(15) 0.5399(15) 0.034(5) Uani 1 1 d . . . H15A H 0.6703 0.6807 0.4864 0.040 Uiso 1 1 d R . . H15B H 0.7189 0.7471 0.6025 0.040 Uiso 1 1 d R . . C16 C 0.9050(14) 0.8284(16) 0.6183(14) 0.032(4) Uani 1 1 d U . . H16A H 0.8876 0.7546 0.6002 0.038 Uiso 1 1 d R . . H16B H 0.9046 0.8544 0.6832 0.038 Uiso 1 1 d R . . C17 C 1.0174(16) 0.8973(16) 0.6223(14) 0.034(4) Uani 1 1 d U . . H17A H 1.0714 0.8976 0.6719 0.040 Uiso 1 1 d R . . H17B H 1.0362 0.9717 0.6418 0.040 Uiso 1 1 d R . . C18 C 1.0197(14) 0.8584(15) 0.5205(13) 0.027(3) Uani 1 1 d U . . H18A H 1.0055 0.7859 0.5049 0.032 Uiso 1 1 d R . . C19 C 0.9263(14) 0.8449(16) 0.4387(14) 0.032(4) Uani 1 1 d U . . H19A H 0.9235 0.8115 0.3738 0.038 Uiso 1 1 d R . . H19B H 0.9420 0.9172 0.4497 0.038 Uiso 1 1 d R . . C20 C 0.8190(16) 0.7768(16) 0.4400(14) 0.034(4) Uani 1 1 d U . . H20A H 0.7623 0.7731 0.3902 0.041 Uiso 1 1 d R . . H20B H 0.8007 0.7030 0.4243 0.041 Uiso 1 1 d R . . C21 C 1.1303(16) 0.9326(16) 0.5228(15) 0.029(4) Uani 1 1 d U . . C22 C 0.0451(17) 0.9029(18) 0.1661(16) 0.039(5) Uani 1 1 d U . . C23 C -0.0411(16) 0.8912(17) 0.0798(14) 0.033(4) Uani 1 1 d U . . C24 C -0.0477(15) 0.8574(16) -0.0162(14) 0.030(4) Uani 1 1 d U . . H24B H -0.0002 0.8345 -0.0291 0.036 Uiso 1 1 d R . . C25 C -0.1250(15) 0.8485(16) -0.0908(14) 0.031(4) Uani 1 1 d U . . H25A H -0.1288 0.8250 -0.1578 0.037 Uiso 1 1 d R . . C26 C -0.1965(16) 0.8796(17) -0.0715(14) 0.036(4) Uani 1 1 d U . . C27 C -0.1912(16) 0.9101(17) 0.0258(14) 0.038(4) Uani 1 1 d U . . H27A H -0.2406 0.9303 0.0384 0.045 Uiso 1 1 d R . . C28 C -0.1122(17) 0.9192(18) 0.1061(15) 0.043(4) Uani 1 1 d U . . H28A H -0.0618 0.9948 0.1218 0.052 Uiso 1 1 d R . . C29 C -0.2771(15) 0.8769(16) -0.1489(15) 0.030(4) Uani 1 1 d U . . C30 C -0.0085(15) 0.6771(15) 0.2922(14) 0.027(4) Uani 1 1 d U . . C31 C -0.1028(16) 0.5843(16) 0.2951(14) 0.036(4) Uani 1 1 d U . . C32 C -0.0858(17) 0.5524(16) 0.3669(15) 0.038(4) Uani 1 1 d U . . H32A H -0.0119 0.5894 0.4169 0.046 Uiso 1 1 d R . . C33 C -0.1693(15) 0.4729(16) 0.3749(14) 0.035(4) Uani 1 1 d U . . H33A H -0.1577 0.4498 0.4275 0.042 Uiso 1 1 d R . . C34 C -0.2767(15) 0.4198(15) 0.3043(13) 0.026(4) Uani 1 1 d U . . C35 C -0.2957(15) 0.4558(16) 0.2312(14) 0.036(4) Uani 1 1 d U . . H35A H -0.3694 0.4216 0.1821 0.043 Uiso 1 1 d R . . C36 C -0.2066(15) 0.5369(15) 0.2267(14) 0.033(4) Uani 1 1 d U . . H36A H -0.2169 0.5560 0.1711 0.039 Uiso 1 1 d R . . C37 C -0.3703(16) 0.3315(16) 0.3106(14) 0.028(4) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.0153(6) 0.0286(6) 0.0238(6) 0.0156(5) 0.0093(5) 0.0125(5) Pr2 0.0155(6) 0.0269(6) 0.0252(6) 0.0159(5) 0.0104(5) 0.0122(5) Pr3 0.0180(6) 0.0283(6) 0.0246(6) 0.0156(5) 0.0118(5) 0.0141(5) P1 0.019(3) 0.026(3) 0.025(3) 0.016(2) 0.010(2) 0.014(2) P2 0.012(3) 0.034(3) 0.024(3) 0.016(2) 0.009(2) 0.012(2) P3 0.021(3) 0.030(3) 0.025(3) 0.013(2) 0.011(2) 0.016(2) O1 0.022(6) 0.027(6) 0.015(6) 0.015(5) 0.014(4) 0.014(5) O2 0.010(6) 0.026(7) 0.034(8) 0.017(6) 0.014(6) 0.004(6) O3 0.018(7) 0.039(8) 0.031(8) 0.025(6) 0.014(6) 0.015(7) O4 0.060(14) 0.134(19) 0.054(13) 0.016(12) -0.005(11) 0.026(14) O5 0.13(2) 0.18(3) 0.081(18) 0.036(17) 0.031(17) 0.07(2) O6 0.020(3) 0.020(3) 0.020(3) 0.0093(15) 0.0087(15) 0.0105(18) O7 0.018(6) 0.022(6) 0.025(6) 0.003(5) 0.002(5) 0.012(5) O8 0.027(7) 0.043(8) 0.025(7) 0.019(6) 0.015(6) 0.028(7) O9 0.026(8) 0.023(7) 0.033(8) 0.014(6) 0.015(6) 0.010(6) O10 0.055(10) 0.066(11) 0.052(10) 0.051(9) 0.037(8) 0.043(9) O11 0.031(8) 0.022(7) 0.025(7) 0.010(6) 0.012(6) 0.016(6) O12 0.003(6) 0.025(7) 0.025(7) 0.012(6) 0.003(5) 0.000(6) O13 0.008(6) 0.022(7) 0.020(7) 0.012(5) 0.006(5) -0.001(6) O14 0.017(7) 0.060(10) 0.031(8) 0.023(7) 0.011(6) 0.014(7) O15 0.029(8) 0.050(9) 0.039(8) 0.031(7) 0.030(7) 0.029(7) O16 0.021(7) 0.044(9) 0.031(8) 0.023(7) 0.011(6) 0.012(7) O17 0.033(8) 0.037(9) 0.042(9) 0.024(7) 0.009(7) 0.011(7) O18 0.031(7) 0.048(7) 0.043(7) 0.041(6) 0.014(5) 0.016(5) O19 0.033(9) 0.035(9) 0.070(11) 0.033(8) 0.027(8) 0.012(8) O20 0.045(9) 0.045(9) 0.014(8) 0.008(6) -0.003(6) 0.028(8) O21 0.037(9) 0.066(11) 0.052(10) 0.026(8) 0.020(8) 0.041(9) O22 0.032(8) 0.051(9) 0.041(9) 0.026(8) 0.013(7) 0.030(8) O23 0.045(9) 0.078(11) 0.041(9) 0.037(8) 0.018(7) 0.050(9) O24 0.067(12) 0.071(12) 0.065(11) 0.028(9) 0.032(10) 0.042(11) O1W 0.063(12) 0.057(12) 0.082(13) 0.029(10) 0.029(10) 0.017(10) O2W 0.18(3) 0.057(16) 0.20(3) 0.034(16) 0.03(2) 0.027(18) O3W 0.27(2) 0.25(2) 0.26(2) 0.122(12) 0.106(12) 0.139(13) O4W 0.299(13) 0.299(13) 0.299(13) 0.132(6) 0.125(5) 0.166(7) O5W 0.70(2) 0.70(2) 0.70(2) 0.311(10) 0.294(9) 0.390(12) O6W 0.291(15) 0.291(15) 0.291(15) 0.129(7) 0.122(7) 0.161(9) O7W 0.29(2) 0.28(2) 0.29(2) 0.123(13) 0.119(13) 0.167(15) N1 0.049(12) 0.056(12) 0.043(11) 0.043(10) 0.022(9) 0.036(11) N2 0.019(7) 0.033(7) 0.014(6) 0.012(5) 0.012(5) 0.007(5) N3 0.022(9) 0.023(9) 0.043(11) 0.019(8) 0.011(8) 0.008(8) C1 0.021(8) 0.026(8) 0.022(8) 0.016(6) 0.016(6) 0.006(6) C2 0.029(9) 0.047(10) 0.040(9) 0.020(8) 0.011(8) 0.008(8) C3 0.042(9) 0.050(9) 0.050(8) 0.011(8) 0.007(8) 0.006(8) C4 0.046(8) 0.048(8) 0.055(8) 0.011(7) 0.009(7) 0.008(7) C5 0.043(8) 0.038(8) 0.051(8) 0.017(7) 0.013(7) 0.020(7) C6 0.031(9) 0.042(9) 0.047(9) 0.014(8) 0.009(8) 0.026(8) C7 0.049(11) 0.056(11) 0.064(11) 0.008(10) 0.017(10) 0.002(10) C8 0.015(10) 0.046(13) 0.018(11) 0.013(9) 0.014(8) 0.006(10) C9 0.026(8) 0.038(8) 0.031(8) 0.026(7) 0.017(7) 0.024(7) C10 0.028(7) 0.031(7) 0.030(7) 0.018(6) 0.018(6) 0.017(6) C11 0.022(6) 0.035(7) 0.021(6) 0.022(5) 0.012(5) 0.020(5) C12 0.024(7) 0.040(7) 0.025(7) 0.024(6) 0.012(6) 0.023(6) C13 0.022(8) 0.051(9) 0.024(8) 0.023(7) 0.017(6) 0.025(7) C14 0.023(8) 0.035(8) 0.016(8) 0.010(7) 0.008(6) 0.021(7) C15 0.014(10) 0.024(11) 0.042(13) 0.019(10) 0.005(9) -0.003(9) C16 0.026(7) 0.045(8) 0.031(7) 0.024(6) 0.019(6) 0.017(6) C17 0.033(4) 0.034(4) 0.033(4) 0.0152(19) 0.0141(18) 0.018(2) C18 0.026(6) 0.034(6) 0.033(6) 0.017(5) 0.017(5) 0.022(5) C19 0.025(6) 0.041(6) 0.031(6) 0.011(5) 0.023(5) 0.017(5) C20 0.032(8) 0.043(9) 0.032(8) 0.016(7) 0.021(7) 0.019(7) C21 0.031(8) 0.036(8) 0.034(8) 0.021(7) 0.018(7) 0.023(7) C22 0.036(9) 0.050(9) 0.038(9) 0.024(8) 0.011(7) 0.027(8) C23 0.034(7) 0.050(7) 0.034(7) 0.024(6) 0.016(6) 0.031(6) C24 0.033(7) 0.048(7) 0.031(7) 0.020(6) 0.021(6) 0.032(6) C25 0.032(7) 0.055(7) 0.028(7) 0.022(6) 0.023(6) 0.033(6) C26 0.035(6) 0.051(7) 0.027(6) 0.022(5) 0.015(5) 0.024(5) C27 0.038(6) 0.051(6) 0.032(6) 0.019(5) 0.016(5) 0.029(5) C28 0.042(7) 0.051(7) 0.038(7) 0.026(6) 0.011(6) 0.027(6) C29 0.027(7) 0.042(7) 0.025(7) 0.021(6) 0.007(5) 0.021(6) C30 0.029(7) 0.030(7) 0.024(7) 0.011(5) 0.014(5) 0.017(5) C31 0.031(6) 0.036(6) 0.030(6) 0.014(5) 0.011(5) 0.012(5) C32 0.032(6) 0.041(6) 0.036(6) 0.019(5) 0.011(5) 0.015(5) C33 0.025(7) 0.039(7) 0.032(7) 0.021(6) 0.012(6) 0.008(6) C34 0.022(6) 0.033(6) 0.026(6) 0.016(5) 0.014(5) 0.013(5) C35 0.015(6) 0.043(7) 0.039(7) 0.012(6) 0.009(6) 0.012(6) C36 0.021(6) 0.038(7) 0.033(7) 0.018(6) 0.011(6) 0.010(6) C37 0.026(8) 0.036(8) 0.022(8) 0.007(7) 0.017(7) 0.017(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O12 2.363(11) 2_676 ? Pr1 O3 2.461(11) 2_676 ? Pr1 O15 2.476(12) 1_455 ? Pr1 O21 2.490(13) . ? Pr1 O6 2.524(11) . ? Pr1 O20 2.541(12) . ? Pr1 O16 2.576(12) . ? Pr1 O7 2.591(12) . ? Pr1 O17 2.643(13) . ? Pr1 C22 2.88(2) . ? Pr1 C30 2.990(19) . ? Pr1 P2 3.160(5) . ? Pr2 O7 2.363(12) 2_676 ? Pr2 O9 2.470(12) 1_556 ? Pr2 O1 2.474(10) 2_676 ? Pr2 O23 2.512(13) 1_656 ? Pr2 O13 2.524(11) . ? Pr2 O22 2.588(12) 1_656 ? Pr2 O12 2.597(11) . ? Pr2 O18 2.613(13) 2_566 ? Pr2 O19 2.640(13) 2_566 ? Pr2 C29 2.911(18) 1_656 ? Pr2 C37 2.98(2) 2_566 ? Pr2 P3 3.173(5) . ? Pr3 O2 2.341(11) 2_676 ? Pr3 O8 2.427(11) . ? Pr3 O11 2.465(11) . ? Pr3 O10 2.486(12) 2_675 ? Pr3 O14 2.508(12) 2_776 ? Pr3 O24 2.521(14) . ? Pr3 O3 2.594(12) . ? Pr3 O1 2.606(11) . ? Pr3 P1 3.186(5) . ? P1 O2 1.505(12) . ? P1 O1 1.512(11) . ? P1 O3 1.525(12) . ? P1 C1 1.814(17) . ? P2 O8 1.511(12) . ? P2 O6 1.532(12) . ? P2 O7 1.544(12) . ? P2 C8 1.847(17) . ? P3 O11 1.495(12) . ? P3 O13 1.516(11) . ? P3 O12 1.546(12) . ? P3 C15 1.826(19) . ? O1 Pr2 2.474(10) 2_676 ? O2 Pr3 2.341(11) 2_676 ? O3 Pr1 2.461(11) 2_676 ? O4 C7 1.22(3) . ? O5 C7 1.25(3) . ? O5 H5C 0.8540 . ? O7 Pr2 2.363(11) 2_676 ? O9 C14 1.26(2) . ? O9 Pr2 2.470(12) 1_554 ? O10 C14 1.28(2) . ? O10 Pr3 2.486(12) 2_675 ? O12 Pr1 2.363(11) 2_676 ? O14 C21 1.27(2) . ? O14 Pr3 2.508(12) 2_776 ? O15 C21 1.23(2) . ? O15 Pr1 2.476(12) 1_655 ? O16 C30 1.27(2) . ? O17 C30 1.25(2) . ? O18 C37 1.25(2) . ? O18 Pr2 2.613(13) 2_566 ? O19 C37 1.25(2) . ? O19 Pr2 2.640(13) 2_566 ? O20 C22 1.26(2) . ? O21 C22 1.23(2) . ? O22 C29 1.28(2) . ? O22 Pr2 2.588(12) 1_454 ? O23 C29 1.22(2) . ? O23 Pr2 2.512(13) 1_454 ? O24 H24C 0.8613 . ? O24 H24A 0.8591 . ? O1W H1WA 0.8608 . ? O1W H1WB 0.8473 . ? O2W H2WB 0.8613 . ? O2W H2WA 0.8584 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8471 . ? O4W H4WA 0.8619 . ? O4W H4WB 0.8488 . ? O5W H5WA 0.8501 . ? O5W H5WB 0.8478 . ? O6W H6WA 0.8513 . ? O6W H6WB 0.8525 . ? O7W H7WA 0.8616 . ? O7W H7WB 0.8490 . ? N1 C2 1.49(2) . ? N1 C1 1.50(2) . ? N1 C6 1.51(2) . ? N1 H1C 0.9124 . ? N2 C13 1.46(2) . ? N2 C8 1.47(2) . ? N2 C9 1.51(2) . ? N2 H2A 0.9021 . ? N3 C16 1.46(2) . ? N3 C20 1.48(2) . ? N3 C15 1.54(2) . ? N3 H3C 0.9026 . ? C1 H1A 0.9730 . ? C1 H1B 0.9701 . ? C2 C3 1.52(3) . ? C2 H2B 0.9720 . ? C2 H2C 0.9658 . ? C3 C4 1.59(3) . ? C3 H3A 0.9693 . ? C3 H3B 0.9719 . ? C4 C5 1.53(3) . ? C4 C7 1.53(4) . ? C4 H4A 0.9708 . ? C5 C6 1.52(3) . ? C5 H5A 0.9660 . ? C5 H5B 0.9719 . ? C6 H6A 0.9690 . ? C6 H6B 0.9719 . ? C8 H8A 0.9699 . ? C8 H8B 0.9591 . ? C9 C10 1.51(2) . ? C9 H9A 0.9622 . ? C9 H9B 0.9730 . ? C10 C11 1.52(2) . ? C10 H10A 0.9595 . ? C10 H10B 0.9636 . ? C11 C14 1.50(2) . ? C11 C12 1.51(2) . ? C11 H11A 0.9614 . ? C12 C13 1.49(2) . ? C12 H12A 0.9731 . ? C12 H12B 0.9612 . ? C13 H13A 0.9603 . ? C13 H13B 0.9626 . ? C15 H15A 0.9577 . ? C15 H15B 0.9704 . ? C16 C17 1.51(2) . ? C16 H16A 0.9619 . ? C16 H16B 0.9610 . ? C17 C18 1.51(2) . ? C17 H17A 0.9733 . ? C17 H17B 0.9618 . ? C18 C21 1.52(3) . ? C18 C19 1.54(2) . ? C18 H18A 0.9624 . ? C19 C20 1.48(2) . ? C19 H19A 0.9592 . ? C19 H19B 0.9638 . ? C20 H20A 0.9731 . ? C20 H20B 0.9626 . ? C22 C23 1.53(3) . ? C23 C24 1.37(2) . ? C23 C28 1.42(3) . ? C24 C25 1.35(2) . ? C24 H24B 0.9646 . ? C25 C26 1.42(3) . ? C25 H25A 0.9619 . ? C26 C27 1.40(2) . ? C26 C29 1.46(2) . ? C27 C28 1.42(2) . ? C27 H27A 0.9653 . ? C28 H28A 0.9600 . ? C29 Pr2 2.911(18) 1_454 ? C30 C31 1.50(3) . ? C31 C32 1.33(3) . ? C31 C36 1.37(3) . ? C32 C33 1.35(3) . ? C32 H32A 0.9715 . ? C33 C34 1.40(2) . ? C33 H33A 0.9731 . ? C34 C35 1.40(3) . ? C34 C37 1.49(3) . ? C35 C36 1.38(3) . ? C35 H35A 0.9719 . ? C36 H36A 0.9725 . ? C37 Pr2 2.98(2) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Pr1 O3 79.6(4) 2_676 2_676 ? O12 Pr1 O15 77.2(4) 2_676 1_455 ? O3 Pr1 O15 79.9(4) 2_676 1_455 ? O12 Pr1 O21 96.0(4) 2_676 . ? O3 Pr1 O21 157.1(4) 2_676 . ? O15 Pr1 O21 121.4(4) 1_455 . ? O12 Pr1 O6 120.1(4) 2_676 . ? O3 Pr1 O6 80.7(4) 2_676 . ? O15 Pr1 O6 150.9(4) 1_455 . ? O21 Pr1 O6 82.2(4) . . ? O12 Pr1 O20 80.5(4) 2_676 . ? O3 Pr1 O20 147.4(4) 2_676 . ? O15 Pr1 O20 70.6(4) 1_455 . ? O21 Pr1 O20 51.0(4) . . ? O6 Pr1 O20 131.9(4) . . ? O12 Pr1 O16 142.8(4) 2_676 . ? O3 Pr1 O16 71.4(4) 2_676 . ? O15 Pr1 O16 75.3(4) 1_455 . ? O21 Pr1 O16 119.6(4) . . ? O6 Pr1 O16 78.1(4) . . ? O20 Pr1 O16 112.6(4) . . ? O12 Pr1 O7 65.4(4) 2_676 . ? O3 Pr1 O7 86.9(4) 2_676 . ? O15 Pr1 O7 142.0(4) 1_455 . ? O21 Pr1 O7 71.0(4) . . ? O6 Pr1 O7 57.5(4) . . ? O20 Pr1 O7 107.8(4) . . ? O16 Pr1 O7 133.4(4) . . ? O12 Pr1 O17 153.1(4) 2_676 . ? O3 Pr1 O17 120.9(4) 2_676 . ? O15 Pr1 O17 88.9(4) 1_455 . ? O21 Pr1 O17 71.6(4) . . ? O6 Pr1 O17 82.7(4) . . ? O20 Pr1 O17 73.1(4) . . ? O16 Pr1 O17 49.7(4) . . ? O7 Pr1 O17 127.9(4) . . ? O12 Pr1 C22 90.0(5) 2_676 . ? O3 Pr1 C22 169.4(5) 2_676 . ? O15 Pr1 C22 96.2(5) 1_455 . ? O21 Pr1 C22 25.2(5) . . ? O6 Pr1 C22 106.4(5) . . ? O20 Pr1 C22 25.9(5) . . ? O16 Pr1 C22 117.3(5) . . ? O7 Pr1 C22 90.4(5) . . ? O17 Pr1 C22 68.5(5) . . ? O12 Pr1 C30 156.9(4) 2_676 . ? O3 Pr1 C30 96.5(5) 2_676 . ? O15 Pr1 C30 79.7(5) 1_455 . ? O21 Pr1 C30 95.9(5) . . ? O6 Pr1 C30 81.2(4) . . ? O20 Pr1 C30 91.8(5) . . ? O16 Pr1 C30 25.1(4) . . ? O7 Pr1 C30 137.5(4) . . ? O17 Pr1 C30 24.8(4) . . ? C22 Pr1 C30 92.4(6) . . ? O12 Pr1 P2 93.6(3) 2_676 . ? O3 Pr1 P2 84.9(3) 2_676 . ? O15 Pr1 P2 163.4(3) 1_455 . ? O21 Pr1 P2 72.8(3) . . ? O6 Pr1 P2 28.6(3) . . ? O20 Pr1 P2 122.0(3) . . ? O16 Pr1 P2 106.2(3) . . ? O7 Pr1 P2 29.1(3) . . ? O17 Pr1 P2 104.7(3) . . ? C22 Pr1 P2 97.6(5) . . ? C30 Pr1 P2 108.9(4) . . ? O7 Pr2 O9 74.8(4) 2_676 1_556 ? O7 Pr2 O1 77.2(4) 2_676 2_676 ? O9 Pr2 O1 80.3(4) 1_556 2_676 ? O7 Pr2 O23 78.8(4) 2_676 1_656 ? O9 Pr2 O23 69.9(4) 1_556 1_656 ? O1 Pr2 O23 145.7(4) 2_676 1_656 ? O7 Pr2 O13 118.8(4) 2_676 . ? O9 Pr2 O13 154.5(4) 1_556 . ? O1 Pr2 O13 82.0(3) 2_676 . ? O23 Pr2 O13 131.5(4) 1_656 . ? O7 Pr2 O22 101.3(4) 2_676 1_656 ? O9 Pr2 O22 119.5(4) 1_556 1_656 ? O1 Pr2 O22 159.4(4) 2_676 1_656 ? O23 Pr2 O22 50.7(4) 1_656 1_656 ? O13 Pr2 O22 80.8(4) . 1_656 ? O7 Pr2 O12 65.3(4) 2_676 . ? O9 Pr2 O12 140.0(4) 1_556 . ? O1 Pr2 O12 87.8(3) 2_676 . ? O23 Pr2 O12 104.0(4) 1_656 . ? O13 Pr2 O12 56.9(3) . . ? O22 Pr2 O12 73.2(4) 1_656 . ? O7 Pr2 O18 138.3(4) 2_676 2_566 ? O9 Pr2 O18 74.5(4) 1_556 2_566 ? O1 Pr2 O18 70.4(4) 2_676 2_566 ? O23 Pr2 O18 115.3(4) 1_656 2_566 ? O13 Pr2 O18 82.3(4) . 2_566 ? O22 Pr2 O18 118.2(4) 1_656 2_566 ? O12 Pr2 O18 136.4(4) . 2_566 ? O7 Pr2 O19 151.0(4) 2_676 2_566 ? O9 Pr2 O19 84.9(4) 1_556 2_566 ? O1 Pr2 O19 119.8(4) 2_676 2_566 ? O23 Pr2 O19 74.9(5) 1_656 2_566 ? O13 Pr2 O19 88.2(4) . 2_566 ? O22 Pr2 O19 70.9(4) 1_656 2_566 ? O12 Pr2 O19 133.1(4) . 2_566 ? O18 Pr2 O19 49.4(4) 2_566 2_566 ? O7 Pr2 C29 90.3(5) 2_676 1_656 ? O9 Pr2 C29 93.8(5) 1_556 1_656 ? O1 Pr2 C29 167.2(5) 2_676 1_656 ? O23 Pr2 C29 24.6(5) 1_656 1_656 ? O13 Pr2 C29 106.9(5) . 1_656 ? O22 Pr2 C29 26.2(5) 1_656 1_656 ? O12 Pr2 C29 89.5(5) . 1_656 ? O18 Pr2 C29 119.1(5) 2_566 1_656 ? O19 Pr2 C29 70.4(5) 2_566 1_656 ? O7 Pr2 C37 152.2(4) 2_676 2_566 ? O9 Pr2 C37 77.7(4) 1_556 2_566 ? O1 Pr2 C37 95.2(5) 2_676 2_566 ? O23 Pr2 C37 94.7(5) 1_656 2_566 ? O13 Pr2 C37 85.8(4) . 2_566 ? O22 Pr2 C37 94.9(5) 1_656 2_566 ? O12 Pr2 C37 141.9(4) . 2_566 ? O18 Pr2 C37 24.7(4) 2_566 2_566 ? O19 Pr2 C37 24.7(4) 2_566 2_566 ? C29 Pr2 C37 94.6(5) 1_656 2_566 ? O7 Pr2 P3 92.9(3) 2_676 . ? O9 Pr2 P3 162.9(3) 1_556 . ? O1 Pr2 P3 85.4(3) 2_676 . ? O23 Pr2 P3 120.1(3) 1_656 . ? O13 Pr2 P3 28.0(3) . . ? O22 Pr2 P3 74.1(3) 1_656 . ? O12 Pr2 P3 28.9(3) . . ? O18 Pr2 P3 109.6(3) 2_566 . ? O19 Pr2 P3 110.6(3) 2_566 . ? C29 Pr2 P3 98.2(4) 1_656 . ? C37 Pr2 P3 113.3(3) 2_566 . ? O2 Pr3 O8 73.7(4) 2_676 . ? O2 Pr3 O11 74.1(4) 2_676 . ? O8 Pr3 O11 109.0(4) . . ? O2 Pr3 O10 141.1(4) 2_676 2_675 ? O8 Pr3 O10 79.7(4) . 2_675 ? O11 Pr3 O10 142.6(4) . 2_675 ? O2 Pr3 O14 142.4(4) 2_676 2_776 ? O8 Pr3 O14 143.5(4) . 2_776 ? O11 Pr3 O14 84.2(4) . 2_776 ? O10 Pr3 O14 70.7(4) 2_675 2_776 ? O2 Pr3 O24 121.6(5) 2_676 . ? O8 Pr3 O24 74.2(4) . . ? O11 Pr3 O24 72.1(4) . . ? O10 Pr3 O24 75.9(5) 2_675 . ? O14 Pr3 O24 78.2(5) 2_776 . ? O2 Pr3 O3 77.1(4) 2_676 . ? O8 Pr3 O3 139.1(4) . . ? O11 Pr3 O3 89.6(4) . . ? O10 Pr3 O3 107.6(4) 2_675 . ? O14 Pr3 O3 72.2(4) 2_776 . ? O24 Pr3 O3 146.6(4) . . ? O2 Pr3 O1 77.3(4) 2_676 . ? O8 Pr3 O1 90.1(4) . . ? O11 Pr3 O1 139.1(3) . . ? O10 Pr3 O1 74.9(4) 2_675 . ? O14 Pr3 O1 101.8(4) 2_776 . ? O24 Pr3 O1 148.9(4) . . ? O3 Pr3 O1 55.5(3) . . ? O2 Pr3 P1 70.6(3) 2_676 . ? O8 Pr3 P1 112.9(3) . . ? O11 Pr3 P1 112.9(3) . . ? O10 Pr3 P1 95.2(3) 2_675 . ? O14 Pr3 P1 91.0(3) 2_776 . ? O24 Pr3 P1 167.8(4) . . ? O3 Pr3 P1 28.3(3) . . ? O1 Pr3 P1 28.0(2) . . ? O2 P1 O1 115.5(7) . . ? O2 P1 O3 113.6(7) . . ? O1 P1 O3 105.8(7) . . ? O2 P1 C1 107.3(7) . . ? O1 P1 C1 104.3(7) . . ? O3 P1 C1 109.8(8) . . ? O2 P1 Pr3 121.1(5) . . ? O1 P1 Pr3 54.1(4) . . ? O3 P1 Pr3 53.7(5) . . ? C1 P1 Pr3 131.6(6) . . ? O8 P2 O6 117.5(7) . . ? O8 P2 O7 113.2(7) . . ? O6 P2 O7 106.2(7) . . ? O8 P2 C8 110.4(8) . . ? O6 P2 C8 102.3(7) . . ? O7 P2 C8 106.1(8) . . ? O8 P2 Pr1 140.4(5) . . ? O6 P2 Pr1 52.0(4) . . ? O7 P2 Pr1 54.6(5) . . ? C8 P2 Pr1 109.2(6) . . ? O11 P3 O13 118.9(7) . . ? O11 P3 O12 112.8(7) . . ? O13 P3 O12 105.7(7) . . ? O11 P3 C15 108.2(8) . . ? O13 P3 C15 105.1(7) . . ? O12 P3 C15 105.0(8) . . ? O11 P3 Pr2 139.3(5) . . ? O13 P3 Pr2 51.5(4) . . ? O12 P3 Pr2 54.4(4) . . ? C15 P3 Pr2 112.4(7) . . ? P1 O1 Pr2 134.7(6) . 2_676 ? P1 O1 Pr3 97.8(5) . . ? Pr2 O1 Pr3 126.7(4) 2_676 . ? P1 O2 Pr3 168.4(7) . 2_676 ? P1 O3 Pr1 135.2(7) . 2_676 ? P1 O3 Pr3 98.0(5) . . ? Pr1 O3 Pr3 126.2(5) 2_676 . ? C7 O5 H5C 105.9 . . ? P2 O6 Pr1 99.5(5) . . ? P2 O7 Pr2 148.8(7) . 2_676 ? P2 O7 Pr1 96.4(6) . . ? Pr2 O7 Pr1 114.2(4) 2_676 . ? P2 O8 Pr3 132.5(7) . . ? C14 O9 Pr2 128.2(11) . 1_554 ? C14 O10 Pr3 138.2(12) . 2_675 ? P3 O11 Pr3 133.9(7) . . ? P3 O12 Pr1 147.8(7) . 2_676 ? P3 O12 Pr2 96.7(5) . . ? Pr1 O12 Pr2 114.0(4) 2_676 . ? P3 O13 Pr2 100.5(5) . . ? C21 O14 Pr3 135.2(12) . 2_776 ? C21 O15 Pr1 125.5(12) . 1_655 ? C30 O16 Pr1 95.9(11) . . ? C30 O17 Pr1 93.3(11) . . ? C37 O18 Pr2 94.5(11) . 2_566 ? C37 O19 Pr2 93.2(12) . 2_566 ? C22 O20 Pr1 92.1(12) . . ? C22 O21 Pr1 95.2(13) . . ? C29 O22 Pr2 91.1(11) . 1_454 ? C29 O23 Pr2 96.4(12) . 1_454 ? Pr3 O24 H24C 109.5 . . ? Pr3 O24 H24A 109.3 . . ? H24C O24 H24A 109.9 . . ? H1WA O1W H1WB 109.3 . . ? H2WB O2W H2WA 109.7 . . ? H3WA O3W H3WB 109.6 . . ? H4WA O4W H4WB 109.7 . . ? H5WA O5W H5WB 110.1 . . ? H6WA O6W H6WB 108.6 . . ? H7WA O7W H7WB 109.6 . . ? C2 N1 C1 114.3(15) . . ? C2 N1 C6 108.5(16) . . ? C1 N1 C6 111.2(15) . . ? C2 N1 H1C 107.4 . . ? C1 N1 H1C 107.9 . . ? C6 N1 H1C 107.3 . . ? C13 N2 C8 113.1(13) . . ? C13 N2 C9 110.9(13) . . ? C8 N2 C9 110.4(14) . . ? C13 N2 H2A 106.1 . . ? C8 N2 H2A 108.9 . . ? C9 N2 H2A 107.2 . . ? C16 N3 C20 112.2(15) . . ? C16 N3 C15 110.1(14) . . ? C20 N3 C15 110.3(14) . . ? C16 N3 H3C 108.0 . . ? C20 N3 H3C 107.2 . . ? C15 N3 H3C 108.9 . . ? N1 C1 P1 115.0(11) . . ? N1 C1 H1A 108.7 . . ? P1 C1 H1A 109.1 . . ? N1 C1 H1B 107.3 . . ? P1 C1 H1B 108.9 . . ? H1A C1 H1B 107.6 . . ? N1 C2 C3 113.0(17) . . ? N1 C2 H2B 108.6 . . ? C3 C2 H2B 108.9 . . ? N1 C2 H2C 109.6 . . ? C3 C2 H2C 108.5 . . ? H2B C2 H2C 108.1 . . ? C2 C3 C4 109.3(18) . . ? C2 C3 H3A 111.4 . . ? C4 C3 H3A 111.6 . . ? C2 C3 H3B 109.0 . . ? C4 C3 H3B 107.3 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C7 111(2) . . ? C5 C4 C3 110.2(19) . . ? C7 C4 C3 109(2) . . ? C5 C4 H4A 108.8 . . ? C7 C4 H4A 110.8 . . ? C3 C4 H4A 107.3 . . ? C6 C5 C4 112.9(19) . . ? C6 C5 H5A 108.7 . . ? C4 C5 H5A 108.4 . . ? C6 C5 H5B 109.5 . . ? C4 C5 H5B 108.9 . . ? H5A C5 H5B 108.3 . . ? N1 C6 C5 109.2(16) . . ? N1 C6 H6A 111.1 . . ? C5 C6 H6A 111.5 . . ? N1 C6 H6B 108.1 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 108.0 . . ? O4 C7 O5 126(3) . . ? O4 C7 C4 122(3) . . ? O5 C7 C4 112(3) . . ? N2 C8 P2 113.6(12) . . ? N2 C8 H8A 107.5 . . ? P2 C8 H8A 108.9 . . ? N2 C8 H8B 110.3 . . ? P2 C8 H8B 108.8 . . ? H8A C8 H8B 107.5 . . ? C10 C9 N2 110.6(14) . . ? C10 C9 H9A 112.0 . . ? N2 C9 H9A 107.6 . . ? C10 C9 H9B 109.4 . . ? N2 C9 H9B 108.9 . . ? H9A C9 H9B 108.2 . . ? C9 C10 C11 112.2(15) . . ? C9 C10 H10A 107.4 . . ? C11 C10 H10A 110.1 . . ? C9 C10 H10B 111.4 . . ? C11 C10 H10B 108.6 . . ? H10A C10 H10B 106.9 . . ? C14 C11 C12 112.1(14) . . ? C14 C11 C10 113.0(14) . . ? C12 C11 C10 111.7(14) . . ? C14 C11 H11A 107.2 . . ? C12 C11 H11A 105.9 . . ? C10 C11 H11A 106.4 . . ? C13 C12 C11 111.9(15) . . ? C13 C12 H12A 109.9 . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12B 109.9 . . ? C11 C12 H12B 107.9 . . ? H12A C12 H12B 107.9 . . ? N2 C13 C12 114.0(14) . . ? N2 C13 H13A 110.2 . . ? C12 C13 H13A 108.7 . . ? N2 C13 H13B 106.5 . . ? C12 C13 H13B 110.1 . . ? H13A C13 H13B 107.1 . . ? O9 C14 O10 121.0(17) . . ? O9 C14 C11 119.4(15) . . ? O10 C14 C11 119.5(16) . . ? N3 C15 P3 113.5(12) . . ? N3 C15 H15A 108.8 . . ? P3 C15 H15A 106.9 . . ? N3 C15 H15B 109.2 . . ? P3 C15 H15B 110.7 . . ? H15A C15 H15B 107.6 . . ? N3 C16 C17 111.4(15) . . ? N3 C16 H16A 107.4 . . ? C17 C16 H16A 107.4 . . ? N3 C16 H16B 112.3 . . ? C17 C16 H16B 111.0 . . ? H16A C16 H16B 107.0 . . ? C16 C17 C18 112.0(16) . . ? C16 C17 H17A 110.7 . . ? C18 C17 H17A 110.6 . . ? C16 C17 H17B 107.9 . . ? C18 C17 H17B 106.9 . . ? H17A C17 H17B 108.7 . . ? C17 C18 C21 112.0(16) . . ? C17 C18 C19 111.1(14) . . ? C21 C18 C19 111.9(15) . . ? C17 C18 H18A 105.1 . . ? C21 C18 H18A 109.2 . . ? C19 C18 H18A 107.1 . . ? C20 C19 C18 111.8(16) . . ? C20 C19 H19A 109.4 . . ? C18 C19 H19A 109.8 . . ? C20 C19 H19B 110.1 . . ? C18 C19 H19B 108.5 . . ? H19A C19 H19B 107.2 . . ? N3 C20 C19 110.9(15) . . ? N3 C20 H20A 110.0 . . ? C19 C20 H20A 110.0 . . ? N3 C20 H20B 107.0 . . ? C19 C20 H20B 110.3 . . ? H20A C20 H20B 108.6 . . ? O15 C21 O14 123.6(18) . . ? O15 C21 C18 120.0(17) . . ? O14 C21 C18 116.3(16) . . ? O21 C22 O20 121.1(19) . . ? O21 C22 C23 118.3(19) . . ? O20 C22 C23 120.5(19) . . ? O21 C22 Pr1 59.6(11) . . ? O20 C22 Pr1 62.0(10) . . ? C23 C22 Pr1 170.3(15) . . ? C24 C23 C28 122.6(18) . . ? C24 C23 C22 121.9(18) . . ? C28 C23 C22 115.5(18) . . ? C25 C24 C23 120.2(17) . . ? C25 C24 H24B 122.0 . . ? C23 C24 H24B 117.6 . . ? C24 C25 C26 121.6(18) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 118.8 . . ? C27 C26 C25 117.3(18) . . ? C27 C26 C29 119.4(18) . . ? C25 C26 C29 123.3(18) . . ? C26 C27 C28 122.7(19) . . ? C26 C27 H27A 117.0 . . ? C28 C27 H27A 120.1 . . ? C23 C28 C27 115.4(18) . . ? C23 C28 H28A 90.4 . . ? C27 C28 H28A 90.5 . . ? O23 C29 O22 121.7(17) . . ? O23 C29 C26 120.8(19) . . ? O22 C29 C26 117.4(18) . . ? O23 C29 Pr2 59.0(10) . 1_454 ? O22 C29 Pr2 62.8(9) . 1_454 ? C26 C29 Pr2 178.2(14) . 1_454 ? O17 C30 O16 120.5(18) . . ? O17 C30 C31 122.0(17) . . ? O16 C30 C31 117.4(17) . . ? O17 C30 Pr1 62.0(10) . . ? O16 C30 Pr1 59.0(10) . . ? C31 C30 Pr1 170.4(13) . . ? C32 C31 C36 120(2) . . ? C32 C31 C30 120.2(18) . . ? C36 C31 C30 119.4(18) . . ? C31 C32 C33 122(2) . . ? C31 C32 H32A 119.4 . . ? C33 C32 H32A 118.8 . . ? C32 C33 C34 119.7(18) . . ? C32 C33 H33A 122.3 . . ? C34 C33 H33A 118.0 . . ? C35 C34 C33 118.8(18) . . ? C35 C34 C37 120.0(17) . . ? C33 C34 C37 121.0(17) . . ? C36 C35 C34 118.4(18) . . ? C36 C35 H35A 120.7 . . ? C34 C35 H35A 120.8 . . ? C31 C36 C35 120.8(19) . . ? C31 C36 H36A 119.0 . . ? C35 C36 H36A 119.9 . . ? O19 C37 O18 122.7(18) . . ? O19 C37 C34 119.1(18) . . ? O18 C37 C34 118.1(17) . . ? O19 C37 Pr2 62.1(10) . 2_566 ? O18 C37 Pr2 60.8(10) . 2_566 ? C34 C37 Pr2 172.6(13) . 2_566 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.466 _refine_diff_density_min -1.190 _refine_diff_density_rms 0.251 # Attachment 'szg169.cif' data_szg169 _database_code_depnum_ccdc_archive 'CCDC 849254' #TrackingRef 'szg169.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H61 N3 O31 P3 Sm3' _chemical_formula_weight 1587.85 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.040(3) _cell_length_b 15.090(3) _cell_length_c 15.179(5) _cell_angle_alpha 105.689(4) _cell_angle_beta 103.559(4) _cell_angle_gamma 117.111(3) _cell_volume 2682.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 695 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 19.01 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.966 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1566 _exptl_absorpt_coefficient_mu 3.426 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7411 _exptl_absorpt_correction_T_max 0.8446 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Smart Apex II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11278 _diffrn_reflns_av_R_equivalents 0.0738 _diffrn_reflns_av_sigmaI/netI 0.1502 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 22.90 _reflns_number_total 7286 _reflns_number_gt 4432 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7286 _refine_ls_number_parameters 694 _refine_ls_number_restraints 168 _refine_ls_R_factor_all 0.1268 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.1890 _refine_ls_wR_factor_gt 0.1541 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.001 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 Sm1 Sm 0.18247(7) 0.88732(8) 0.31907(7) 0.0181(3) Uani 1 1 d . . . Sm2 Sm 0.55724(7) 0.86681(8) 0.69783(7) 0.0185(3) Uani 1 1 d . . . Sm3 Sm 0.58430(7) 0.93771(8) 0.35706(7) 0.0184(3) Uani 1 1 d . . . P1 P 0.6169(4) 1.1417(4) 0.5226(3) 0.0175(11) Uani 1 1 d . . . P2 P 0.3054(4) 0.8281(4) 0.1991(3) 0.0206(12) Uani 1 1 d . . . P3 P 0.6250(4) 0.8105(4) 0.5212(4) 0.0202(12) Uani 1 1 d . . . O1 O 0.5540(8) 1.0943(9) 0.4087(8) 0.014(3) Uani 1 1 d . . . O2 O 0.5462(9) 1.1266(9) 0.5792(8) 0.017(3) Uani 1 1 d U . . O3 O 0.6816(8) 1.0893(9) 0.5368(8) 0.016(3) Uani 1 1 d U . . O4 O 0.9272(16) 1.6124(18) 1.0286(13) 0.092(7) Uani 1 1 d . . . O5 O 0.7735(18) 1.6012(19) 1.0035(17) 0.112(7) Uani 1 1 d U . . H5C H 0.7984 1.6252 1.0673 0.169 Uiso 1 1 d R . . O6 O 0.2208(9) 0.7524(10) 0.2289(8) 0.019(3) Uani 1 1 d . . . O7 O 0.3299(9) 0.9445(10) 0.2505(8) 0.022(3) Uani 1 1 d . . . O8 O 0.4062(9) 0.8271(10) 0.2144(8) 0.022(3) Uani 1 1 d . . . O9 O 0.5038(9) 0.9480(10) -0.1826(9) 0.024(3) Uani 1 1 d . . . O10 O 0.3708(10) 0.9748(11) -0.2465(9) 0.029(3) Uani 1 1 d . . . O11 O 0.6127(9) 0.8207(11) 0.4230(9) 0.028(3) Uani 1 1 d . . . O12 O 0.6878(9) 0.9228(10) 0.6119(8) 0.021(3) Uani 1 1 d . . . O13 O 0.5226(9) 0.7378(11) 0.5324(9) 0.024(3) Uani 1 1 d . . . O14 O 1.2175(9) 0.9643(11) 0.5979(9) 0.027(3) Uani 1 1 d . . . O15 O 1.1403(9) 0.9612(12) 0.4529(9) 0.031(4) Uani 1 1 d . . . O16 O 0.0878(9) 0.7289(12) 0.3624(9) 0.033(4) Uani 1 1 d . . . O17 O -0.0190(10) 0.7108(11) 0.2255(10) 0.034(4) Uani 1 1 d . . . O18 O -0.3545(10) 0.2806(11) 0.3571(10) 0.032(4) Uani 1 1 d . . . O19 O -0.4699(11) 0.3014(11) 0.2617(10) 0.038(4) Uani 1 1 d . . . O20 O 0.0564(10) 0.9480(12) 0.2574(9) 0.036(4) Uani 1 1 d . . . O21 O 0.1011(10) 0.8669(11) 0.1485(9) 0.033(3) Uani 1 1 d . . . O22 O -0.3017(10) 0.8203(11) -0.2437(9) 0.032(3) Uani 1 1 d . . . O23 O -0.3191(10) 0.9277(12) -0.1269(9) 0.036(4) Uani 1 1 d . . . O24 O 0.5972(12) 0.8116(14) 0.2273(10) 0.056(5) Uani 1 1 d . . . H24C H 0.6585 0.8465 0.2232 0.068 Uiso 1 1 d R . . H24A H 0.5921 0.7597 0.2428 0.085 Uiso 1 1 d R . . O1W O 0.8334(12) 0.2574(13) 0.4029(11) 0.062(5) Uani 1 1 d . . . H1WA H 0.8305 0.2377 0.4505 0.093 Uiso 1 1 d R . . H1WB H 0.8024 0.2006 0.3476 0.093 Uiso 1 1 d R . . O2W O 0.3959(19) 0.5191(17) 0.4920(16) 0.133(10) Uani 1 1 d . . . H2WB H 0.4659 0.5544 0.5134 0.159 Uiso 1 1 d R . . H2WA H 0.3774 0.5074 0.5388 0.199 Uiso 1 1 d R . . O3W O 0.664(3) 0.612(3) 0.701(3) 0.250(14) Uani 1 1 d U . . H3WA H 0.6412 0.5470 0.6615 0.300 Uiso 1 1 d R . . H3WB H 0.7318 0.6554 0.7144 0.300 Uiso 1 1 d R . . O4W O 0.583(3) 0.615(3) 0.211(3) 0.274(15) Uani 1 1 d U . . H4WA H 0.5966 0.5921 0.2546 0.410 Uiso 1 1 d R . . H4WB H 0.5473 0.5617 0.1521 0.410 Uiso 1 1 d R . . O5W O 0.781(8) 0.753(8) 0.198(7) 0.70(2) Uani 1 1 d U . . H5WA H 0.8170 0.7975 0.1767 0.841 Uiso 1 1 d R . . H5WB H 0.7480 0.6869 0.1539 1.051 Uiso 1 1 d R . . O6W O 0.030(4) 0.681(4) 0.684(3) 0.305(16) Uani 1 1 d U . . H6WA H -0.0025 0.7083 0.7074 0.457 Uiso 1 1 d R . . H6WB H -0.0126 0.6113 0.6547 0.457 Uiso 1 1 d R . . O7W O 0.500(4) 0.475(4) 0.299(3) 0.303(16) Uani 1 1 d U . . H7WA H 0.4907 0.4436 0.3376 0.454 Uiso 1 1 d R . . H7WB H 0.4682 0.4267 0.2380 0.454 Uiso 1 1 d R . . N1 N 0.7439(12) 1.3597(12) 0.6759(11) 0.028(4) Uani 1 1 d . . . H1C H 0.7498 1.3203 0.7097 0.034 Uiso 1 1 d R . . N2 N 0.2885(11) 0.8377(12) 0.0157(10) 0.018(4) Uani 1 1 d . . . H2A H 0.3429 0.9064 0.0632 0.021 Uiso 1 1 d R . . N3 N 0.8193(11) 0.8210(13) 0.5419(11) 0.027(4) Uani 1 1 d . . . H3C H 0.8366 0.8903 0.5568 0.032 Uiso 1 1 d R . . C1 C 0.7102(14) 1.2901(15) 0.5681(13) 0.023(4) Uani 1 1 d U . . H1A H 0.6749 1.3148 0.5286 0.028 Uiso 1 1 d R . . H1B H 0.7752 1.3046 0.5571 0.028 Uiso 1 1 d R . . C2 C 0.8553(15) 1.4626(16) 0.7186(14) 0.032(5) Uani 1 1 d U . . H2B H 0.8482 1.5094 0.6889 0.039 Uiso 1 1 d R . . H2C H 0.9084 1.4499 0.7039 0.039 Uiso 1 1 d R . . C3 C 0.8936(19) 1.5228(19) 0.8328(15) 0.061(8) Uani 1 1 d . . . H3A H 0.9640 1.5919 0.8613 0.073 Uiso 1 1 d R . . H3B H 0.9024 1.4769 0.8627 0.073 Uiso 1 1 d R . . C4 C 0.8095(16) 1.5419(18) 0.8611(15) 0.039(6) Uani 1 1 d U . . H4A H 0.8073 1.5949 0.8383 0.047 Uiso 1 1 d R . . C5 C 0.6935(16) 1.4381(17) 0.8039(13) 0.040(6) Uani 1 1 d . . . H5A H 0.6403 1.4534 0.8142 0.048 Uiso 1 1 d R . . H5B H 0.6931 1.3879 0.8322 0.048 Uiso 1 1 d R . . C6 C 0.6603(15) 1.3809(18) 0.6930(14) 0.036(6) Uani 1 1 d . . . H6A H 0.5875 1.3139 0.6586 0.043 Uiso 1 1 d R . . H6B H 0.6605 1.4315 0.6654 0.043 Uiso 1 1 d R . . C7 C 0.842(3) 1.589(2) 0.974(2) 0.069(9) Uani 1 1 d . . . C8 C 0.2269(14) 0.7750(16) 0.0644(13) 0.025(5) Uani 1 1 d U . . H8A H 0.1642 0.7803 0.0557 0.030 Uiso 1 1 d R . . H8B H 0.1999 0.6983 0.0309 0.030 Uiso 1 1 d R . . C9 C 0.3396(15) 0.7841(16) -0.0287(14) 0.029(5) Uani 1 1 d U . . H9A H 0.2821 0.7100 -0.0782 0.035 Uiso 1 1 d R . . H9B H 0.3862 0.7801 0.0240 0.035 Uiso 1 1 d R . . C10 C 0.4087(14) 0.8456(16) -0.0760(13) 0.022(5) Uani 1 1 d . . . H10A H 0.4357 0.8055 -0.1076 0.027 Uiso 1 1 d R . . H10B H 0.4716 0.9163 -0.0246 0.027 Uiso 1 1 d R . . C11 C 0.3417(14) 0.8647(15) -0.1529(13) 0.018(4) Uani 1 1 d U . . H11A H 0.2855 0.7930 -0.2073 0.022 Uiso 1 1 d R . . C12 C 0.2841(14) 0.9137(16) -0.1092(13) 0.024(5) Uani 1 1 d U . . H12A H 0.2344 0.9136 -0.1629 0.028 Uiso 1 1 d R . . H12B H 0.3378 0.9891 -0.0603 0.028 Uiso 1 1 d R . . C13 C 0.2189(15) 0.8466(16) -0.0627(14) 0.028(5) Uani 1 1 d U . . H13A H 0.1872 0.8822 -0.0333 0.034 Uiso 1 1 d R . . H13B H 0.1596 0.7735 -0.1130 0.034 Uiso 1 1 d R . . C14 C 0.4110(14) 0.9365(15) -0.1973(13) 0.019(4) Uani 1 1 d U . . C15 C 0.7081(12) 0.7538(14) 0.5417(12) 0.014(4) Uani 1 1 d U . . H15A H 0.6690 0.6810 0.4882 0.017 Uiso 1 1 d R . . H15B H 0.7177 0.7474 0.6043 0.017 Uiso 1 1 d R . . C16 C 0.9063(15) 0.8297(19) 0.6193(14) 0.038(6) Uani 1 1 d . . . H16A H 0.8889 0.7559 0.6013 0.045 Uiso 1 1 d R . . H16B H 0.9060 0.8558 0.6843 0.045 Uiso 1 1 d R . . C17 C 1.0184(15) 0.8991(18) 0.6244(13) 0.033(5) Uani 1 1 d . . . H17A H 1.0724 0.8995 0.6741 0.040 Uiso 1 1 d R . . H17B H 1.0372 0.9735 0.6440 0.040 Uiso 1 1 d R . . C18 C 1.0230(14) 0.8623(16) 0.5218(13) 0.022(4) Uani 1 1 d U . . H18A H 1.0088 0.7899 0.5062 0.026 Uiso 1 1 d R . . C19 C 0.9277(13) 0.8453(16) 0.4404(13) 0.024(5) Uani 1 1 d U . . H19A H 0.9249 0.8119 0.3755 0.028 Uiso 1 1 d R . . H19B H 0.9434 0.9176 0.4514 0.028 Uiso 1 1 d R . . C20 C 0.8183(14) 0.7756(16) 0.4393(13) 0.025(5) Uani 1 1 d U . . H20A H 0.7616 0.7719 0.3895 0.030 Uiso 1 1 d R . . H20B H 0.8000 0.7018 0.4237 0.030 Uiso 1 1 d R . . C21 C 1.1344(16) 0.9333(17) 0.5234(15) 0.030(5) Uani 1 1 d U . . C22 C 0.0480(15) 0.9044(16) 0.1682(14) 0.023(4) Uani 1 1 d U . . C23 C -0.0403(15) 0.8932(16) 0.0852(14) 0.029(5) Uani 1 1 d U . . C24 C -0.0488(16) 0.8552(18) -0.0124(16) 0.044(6) Uani 1 1 d . . . H24B H -0.0013 0.8322 -0.0253 0.052 Uiso 1 1 d R . . C25 C -0.1271(14) 0.8484(16) -0.0916(13) 0.025(5) Uani 1 1 d . . . H25A H -0.1309 0.8249 -0.1586 0.031 Uiso 1 1 d R . . C26 C -0.1985(15) 0.8808(16) -0.0724(14) 0.029(5) Uani 1 1 d U . . C27 C -0.1891(17) 0.9120(19) 0.0273(15) 0.044(6) Uani 1 1 d . . . H27A H -0.2385 0.9322 0.0399 0.053 Uiso 1 1 d R . . C28 C -0.1118(15) 0.9213(17) 0.1038(13) 0.029(5) Uani 1 1 d . . . H28A H -0.1109 0.9414 0.1699 0.035 Uiso 1 1 d R . . C29 C -0.2789(14) 0.8733(15) -0.1526(13) 0.017(4) Uani 1 1 d U . . C30 C -0.0018(15) 0.6802(15) 0.2940(14) 0.020(4) Uani 1 1 d . . . C31 C -0.1022(15) 0.5860(17) 0.2959(15) 0.032(5) Uani 1 1 d . . . C32 C -0.0845(15) 0.5562(17) 0.3719(15) 0.034(6) Uani 1 1 d . . . H32A H -0.0106 0.5932 0.4219 0.041 Uiso 1 1 d R . . C33 C -0.1735(14) 0.4732(16) 0.3749(14) 0.026(5) Uani 1 1 d U . . H33A H -0.1618 0.4500 0.4275 0.031 Uiso 1 1 d R . . C34 C -0.2802(15) 0.4195(18) 0.3023(14) 0.030(5) Uani 1 1 d . . . C35 C -0.2926(18) 0.4542(19) 0.2291(16) 0.043(6) Uani 1 1 d U . . H35A H -0.3662 0.4199 0.1799 0.052 Uiso 1 1 d R . . C36 C -0.2074(16) 0.5344(18) 0.2229(15) 0.039(6) Uani 1 1 d . . . H36A H -0.2177 0.5535 0.1672 0.047 Uiso 1 1 d R . . C37 C -0.3724(16) 0.3307(16) 0.3090(15) 0.027(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0118(5) 0.0258(6) 0.0160(6) 0.0108(5) 0.0054(4) 0.0091(5) Sm2 0.0137(5) 0.0271(6) 0.0163(6) 0.0120(5) 0.0067(4) 0.0110(5) Sm3 0.0148(5) 0.0264(6) 0.0171(6) 0.0118(5) 0.0083(4) 0.0116(5) P1 0.013(2) 0.023(3) 0.017(3) 0.011(2) 0.005(2) 0.009(2) P2 0.014(3) 0.029(3) 0.014(3) 0.013(2) 0.006(2) 0.006(2) P3 0.018(3) 0.024(3) 0.020(3) 0.010(2) 0.010(2) 0.012(2) O1 0.005(6) 0.010(7) 0.020(7) 0.005(5) 0.007(5) -0.001(5) O2 0.018(3) 0.018(3) 0.017(3) 0.0077(15) 0.0076(15) 0.0096(18) O3 0.016(3) 0.017(3) 0.016(3) 0.0073(15) 0.0072(15) 0.0088(18) O4 0.079(15) 0.119(19) 0.038(12) 0.017(12) 0.005(10) 0.045(14) O5 0.112(7) 0.113(7) 0.112(7) 0.049(3) 0.047(3) 0.062(4) O6 0.023(7) 0.020(8) 0.026(7) 0.018(6) 0.017(6) 0.012(6) O7 0.023(7) 0.018(8) 0.022(7) 0.011(6) 0.006(6) 0.009(6) O8 0.015(7) 0.037(9) 0.011(7) 0.012(6) 0.004(5) 0.011(6) O9 0.023(7) 0.029(8) 0.023(7) 0.016(6) 0.012(6) 0.012(7) O10 0.031(8) 0.054(10) 0.018(7) 0.024(7) 0.014(6) 0.027(8) O11 0.024(7) 0.052(10) 0.025(8) 0.023(7) 0.020(6) 0.025(7) O12 0.013(6) 0.024(8) 0.024(7) 0.008(6) 0.001(6) 0.012(6) O13 0.024(7) 0.042(9) 0.027(7) 0.025(7) 0.019(6) 0.024(7) O14 0.012(7) 0.040(9) 0.028(8) 0.012(7) 0.013(6) 0.014(7) O15 0.019(7) 0.058(10) 0.021(8) 0.019(7) 0.004(6) 0.025(7) O16 0.007(7) 0.052(10) 0.025(8) 0.017(7) 0.005(6) 0.008(7) O17 0.018(7) 0.036(9) 0.029(8) 0.015(7) 0.002(6) 0.005(7) O18 0.021(7) 0.038(9) 0.035(8) 0.030(8) 0.008(6) 0.008(7) O19 0.027(8) 0.030(9) 0.053(10) 0.029(8) 0.021(8) 0.005(7) O20 0.039(8) 0.057(10) 0.013(7) 0.016(7) 0.000(6) 0.032(8) O21 0.032(8) 0.052(10) 0.034(8) 0.023(7) 0.010(7) 0.037(8) O22 0.033(8) 0.036(9) 0.021(8) 0.007(7) 0.000(6) 0.024(7) O23 0.038(8) 0.053(10) 0.020(8) 0.011(7) 0.001(6) 0.034(8) O24 0.074(11) 0.086(14) 0.034(9) 0.023(9) 0.032(8) 0.059(11) O1W 0.068(12) 0.059(12) 0.055(11) 0.033(9) 0.026(9) 0.027(10) O2W 0.15(2) 0.071(17) 0.12(2) 0.047(15) 0.027(17) 0.031(16) O3W 0.250(14) 0.250(14) 0.250(14) 0.109(6) 0.104(6) 0.139(8) O4W 0.274(15) 0.273(15) 0.274(15) 0.119(7) 0.114(6) 0.152(8) O5W 0.70(2) 0.70(2) 0.70(2) 0.306(10) 0.293(9) 0.389(12) O6W 0.305(16) 0.305(16) 0.305(16) 0.133(7) 0.127(7) 0.169(9) O7W 0.303(16) 0.303(16) 0.303(16) 0.132(7) 0.126(7) 0.168(9) N1 0.038(10) 0.019(10) 0.026(10) 0.011(8) 0.007(8) 0.017(9) N2 0.015(8) 0.022(10) 0.015(8) 0.012(7) 0.006(7) 0.008(7) N3 0.017(8) 0.035(11) 0.032(10) 0.016(8) 0.018(8) 0.012(8) C1 0.023(5) 0.024(5) 0.023(5) 0.010(2) 0.010(2) 0.013(3) C2 0.032(5) 0.032(5) 0.032(5) 0.014(2) 0.014(2) 0.018(3) C3 0.058(17) 0.033(16) 0.034(14) 0.016(12) -0.007(12) -0.003(13) C4 0.039(6) 0.039(6) 0.039(6) 0.017(3) 0.016(3) 0.022(3) C5 0.042(13) 0.034(14) 0.022(12) -0.003(10) 0.016(10) 0.012(12) C6 0.022(11) 0.050(16) 0.035(13) 0.011(11) 0.013(10) 0.022(11) C7 0.08(2) 0.06(2) 0.052(18) -0.003(15) 0.007(16) 0.056(19) C8 0.025(5) 0.025(5) 0.025(5) 0.011(2) 0.010(2) 0.014(3) C9 0.029(5) 0.029(5) 0.029(5) 0.013(2) 0.012(2) 0.016(3) C10 0.019(10) 0.030(13) 0.015(10) 0.014(9) 0.008(8) 0.008(10) C11 0.018(4) 0.018(4) 0.018(4) 0.008(2) 0.008(2) 0.010(2) C12 0.024(5) 0.024(5) 0.024(5) 0.010(2) 0.010(2) 0.013(3) C13 0.028(5) 0.028(5) 0.028(5) 0.013(2) 0.012(2) 0.016(3) C14 0.019(4) 0.019(4) 0.019(4) 0.008(2) 0.008(2) 0.010(3) C15 0.014(4) 0.014(4) 0.014(4) 0.006(2) 0.0060(19) 0.008(2) C16 0.030(12) 0.075(18) 0.025(12) 0.027(12) 0.022(10) 0.033(13) C17 0.026(11) 0.060(16) 0.024(12) 0.028(11) 0.012(10) 0.025(12) C18 0.022(4) 0.022(4) 0.022(4) 0.009(2) 0.009(2) 0.012(3) C19 0.024(5) 0.024(5) 0.024(5) 0.011(2) 0.010(2) 0.013(3) C20 0.025(5) 0.025(5) 0.025(5) 0.011(2) 0.011(2) 0.014(3) C21 0.030(5) 0.030(5) 0.030(5) 0.013(2) 0.012(2) 0.017(3) C22 0.023(5) 0.023(5) 0.023(5) 0.010(2) 0.009(2) 0.013(3) C23 0.029(5) 0.029(5) 0.029(5) 0.013(2) 0.012(2) 0.016(3) C24 0.029(12) 0.050(17) 0.046(15) 0.017(12) 0.020(11) 0.017(12) C25 0.016(10) 0.039(13) 0.010(10) 0.005(9) 0.002(8) 0.012(10) C26 0.029(5) 0.029(5) 0.029(5) 0.013(2) 0.012(2) 0.016(3) C27 0.045(14) 0.057(17) 0.037(14) 0.020(12) 0.009(12) 0.037(14) C28 0.036(12) 0.042(14) 0.011(11) 0.007(10) 0.012(9) 0.024(11) C29 0.017(4) 0.017(4) 0.016(4) 0.007(2) 0.007(2) 0.009(2) C30 0.019(11) 0.015(11) 0.019(11) 0.002(9) 0.003(9) 0.009(10) C31 0.022(11) 0.028(13) 0.035(13) 0.007(11) 0.006(10) 0.013(10) C32 0.013(10) 0.036(14) 0.040(13) 0.024(11) 0.008(10) 0.002(10) C33 0.026(5) 0.026(5) 0.026(5) 0.012(2) 0.011(2) 0.014(3) C34 0.019(11) 0.052(15) 0.033(12) 0.026(11) 0.018(10) 0.021(11) C35 0.043(6) 0.043(6) 0.043(6) 0.019(3) 0.018(3) 0.024(3) C36 0.037(13) 0.047(15) 0.033(13) 0.032(12) 0.017(11) 0.012(12) C37 0.027(12) 0.025(13) 0.027(12) 0.012(10) 0.011(10) 0.013(11) _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 Sm1 O12 2.332(12) 2_676 ? Sm1 O15 2.407(12) 1_455 ? Sm1 O3 2.433(11) 2_676 ? Sm1 O21 2.457(12) . ? Sm1 O6 2.507(12) . ? Sm1 O16 2.522(14) . ? Sm1 O20 2.554(13) . ? Sm1 O7 2.564(11) . ? Sm1 O17 2.622(12) . ? Sm1 C22 2.832(19) . ? Sm1 C30 2.926(19) . ? Sm1 P2 3.121(5) . ? Sm2 O7 2.316(12) 2_676 ? Sm2 O9 2.413(12) 1_556 ? Sm2 O1 2.428(11) 2_676 ? Sm2 O23 2.486(12) 1_656 ? Sm2 O13 2.487(12) . ? Sm2 O12 2.561(12) . ? Sm2 O18 2.562(12) 2_566 ? Sm2 O22 2.568(12) 1_656 ? Sm2 O19 2.594(13) 2_566 ? Sm2 C29 2.877(18) 1_656 ? Sm2 C37 2.96(2) 2_566 ? Sm2 P3 3.128(5) . ? Sm3 O2 2.322(11) 2_676 ? Sm3 O11 2.397(13) . ? Sm3 O8 2.429(11) . ? Sm3 O10 2.436(12) 2_675 ? Sm3 O14 2.454(11) 2_776 ? Sm3 O24 2.455(14) . ? Sm3 O3 2.553(11) . ? Sm3 O1 2.560(11) . ? Sm3 P1 3.146(5) . ? P1 O2 1.495(12) . ? P1 O3 1.521(12) . ? P1 O1 1.532(11) . ? P1 C1 1.818(18) . ? P2 O8 1.487(12) . ? P2 O6 1.534(12) . ? P2 O7 1.538(13) . ? P2 C8 1.827(18) . ? P3 O13 1.512(12) . ? P3 O11 1.517(12) . ? P3 O12 1.526(12) . ? P3 C15 1.824(16) . ? O1 Sm2 2.428(11) 2_676 ? O2 Sm3 2.322(11) 2_676 ? O3 Sm1 2.433(11) 2_676 ? O4 C7 1.18(3) . ? O5 C7 1.29(3) . ? O5 H5C 0.8524 . ? O7 Sm2 2.316(12) 2_676 ? O9 C14 1.28(2) . ? O9 Sm2 2.413(12) 1_554 ? O10 C14 1.26(2) . ? O10 Sm3 2.436(12) 2_675 ? O12 Sm1 2.332(12) 2_676 ? O14 C21 1.26(2) . ? O14 Sm3 2.454(11) 2_776 ? O15 C21 1.26(2) . ? O15 Sm1 2.407(12) 1_655 ? O16 C30 1.21(2) . ? O17 C30 1.27(2) . ? O18 C37 1.25(2) . ? O18 Sm2 2.562(12) 2_566 ? O19 C37 1.27(2) . ? O19 Sm2 2.594(13) 2_566 ? O20 C22 1.28(2) . ? O21 C22 1.22(2) . ? O22 C29 1.26(2) . ? O22 Sm2 2.568(12) 1_454 ? O23 C29 1.26(2) . ? O23 Sm2 2.486(12) 1_454 ? O24 H24C 0.8553 . ? O24 H24A 0.8529 . ? O1W H1WA 0.8548 . ? O1W H1WB 0.8483 . ? O2W H2WB 0.8557 . ? O2W H2WA 0.8541 . ? O3W H3WA 0.8499 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8554 . ? O4W H4WB 0.8493 . ? O5W H5WA 0.8500 . ? O5W H5WB 0.8480 . ? O6W H6WA 0.8495 . ? O6W H6WB 0.8502 . ? O7W H7WA 0.8551 . ? O7W H7WB 0.8495 . ? N1 C2 1.49(2) . ? N1 C6 1.49(2) . ? N1 C1 1.49(2) . ? N1 H1C 0.9049 . ? N2 C13 1.47(2) . ? N2 C8 1.48(2) . ? N2 C9 1.49(2) . ? N2 H2A 0.9006 . ? N3 C16 1.47(2) . ? N3 C15 1.508(19) . ? N3 C20 1.52(2) . ? N3 H3C 0.8995 . ? C1 H1A 0.9653 . ? C1 H1B 0.9648 . ? C2 C3 1.54(3) . ? C2 H2B 0.9645 . ? C2 H2C 0.9622 . ? C3 C4 1.54(3) . ? C3 H3A 0.9644 . ? C3 H3B 0.9643 . ? C4 C7 1.52(3) . ? C4 C5 1.52(3) . ? C4 H4A 0.9637 . ? C5 C6 1.50(2) . ? C5 H5A 0.9620 . ? C5 H5B 0.9645 . ? C6 H6A 0.9643 . ? C6 H6B 0.9644 . ? C8 H8A 0.9643 . ? C8 H8B 0.9579 . ? C9 C10 1.51(2) . ? C9 H9A 0.9606 . ? C9 H9B 0.9662 . ? C10 C11 1.53(2) . ? C10 H10A 0.9585 . ? C10 H10B 0.9616 . ? C11 C12 1.53(2) . ? C11 C14 1.55(2) . ? C11 H11A 0.9604 . ? C12 C13 1.51(2) . ? C12 H12A 0.9664 . ? C12 H12B 0.9601 . ? C13 H13A 0.9589 . ? C13 H13B 0.9609 . ? C15 H15A 0.9581 . ? C15 H15B 0.9652 . ? C16 C17 1.49(2) . ? C16 H16A 0.9590 . ? C16 H16B 0.9605 . ? C17 C18 1.54(2) . ? C17 H17A 0.9664 . ? C17 H17B 0.9589 . ? C18 C21 1.51(2) . ? C18 C19 1.52(2) . ? C18 H18A 0.9591 . ? C19 C20 1.49(2) . ? C19 H19A 0.9594 . ? C19 H19B 0.9598 . ? C20 H20A 0.9662 . ? C20 H20B 0.9593 . ? C22 C23 1.51(3) . ? C23 C28 1.38(3) . ? C23 C24 1.39(3) . ? C24 C25 1.41(3) . ? C24 H24B 0.9613 . ? C25 C26 1.42(3) . ? C25 H25A 0.9610 . ? C26 C27 1.41(3) . ? C26 C29 1.44(2) . ? C27 C28 1.36(2) . ? C27 H27A 0.9617 . ? C28 H28A 0.9615 . ? C29 Sm2 2.877(18) 1_454 ? C30 C31 1.55(3) . ? C31 C32 1.36(3) . ? C31 C36 1.39(3) . ? C32 C33 1.38(2) . ? C32 H32A 0.9660 . ? C33 C34 1.40(2) . ? C33 H33A 0.9660 . ? C34 C35 1.36(3) . ? C34 C37 1.47(3) . ? C35 C36 1.35(3) . ? C35 H35A 0.9662 . ? C36 H36A 0.9658 . ? C37 Sm2 2.96(2) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Sm1 O15 77.0(4) 2_676 1_455 ? O12 Sm1 O3 79.7(4) 2_676 2_676 ? O15 Sm1 O3 79.1(4) 1_455 2_676 ? O12 Sm1 O21 95.3(4) 2_676 . ? O15 Sm1 O21 122.1(4) 1_455 . ? O3 Sm1 O21 156.8(4) 2_676 . ? O12 Sm1 O6 120.5(4) 2_676 . ? O15 Sm1 O6 150.4(4) 1_455 . ? O3 Sm1 O6 80.9(4) 2_676 . ? O21 Sm1 O6 82.3(4) . . ? O12 Sm1 O16 143.7(4) 2_676 . ? O15 Sm1 O16 75.8(5) 1_455 . ? O3 Sm1 O16 71.9(4) 2_676 . ? O21 Sm1 O16 119.5(4) . . ? O6 Sm1 O16 77.3(4) . . ? O12 Sm1 O20 80.7(4) 2_676 . ? O15 Sm1 O20 70.1(4) 1_455 . ? O3 Sm1 O20 146.5(4) 2_676 . ? O21 Sm1 O20 52.1(4) . . ? O6 Sm1 O20 132.6(4) . . ? O16 Sm1 O20 111.6(4) . . ? O12 Sm1 O7 64.9(4) 2_676 . ? O15 Sm1 O7 141.2(4) 1_455 . ? O3 Sm1 O7 86.8(4) 2_676 . ? O21 Sm1 O7 70.8(4) . . ? O6 Sm1 O7 58.3(4) . . ? O16 Sm1 O7 133.4(4) . . ? O20 Sm1 O7 108.9(4) . . ? O12 Sm1 O17 153.2(4) 2_676 . ? O15 Sm1 O17 90.4(4) 1_455 . ? O3 Sm1 O17 121.4(4) 2_676 . ? O21 Sm1 O17 71.3(4) . . ? O6 Sm1 O17 81.6(4) . . ? O16 Sm1 O17 49.8(4) . . ? O20 Sm1 O17 72.8(4) . . ? O7 Sm1 O17 127.3(4) . . ? O12 Sm1 C22 89.6(5) 2_676 . ? O15 Sm1 C22 96.8(5) 1_455 . ? O3 Sm1 C22 169.2(5) 2_676 . ? O21 Sm1 C22 25.3(5) . . ? O6 Sm1 C22 106.4(5) . . ? O16 Sm1 C22 117.1(5) . . ? O20 Sm1 C22 26.9(4) . . ? O7 Sm1 C22 90.3(5) . . ? O17 Sm1 C22 68.3(5) . . ? O12 Sm1 C30 158.0(5) 2_676 . ? O15 Sm1 C30 81.0(5) 1_455 . ? O3 Sm1 C30 96.1(5) 2_676 . ? O21 Sm1 C30 96.4(5) . . ? O6 Sm1 C30 79.5(4) . . ? O16 Sm1 C30 24.2(4) . . ? O20 Sm1 C30 92.1(5) . . ? O7 Sm1 C30 136.8(4) . . ? O17 Sm1 C30 25.6(4) . . ? C22 Sm1 C30 93.2(5) . . ? O12 Sm1 P2 93.5(3) 2_676 . ? O15 Sm1 P2 162.8(3) 1_455 . ? O3 Sm1 P2 85.2(3) 2_676 . ? O21 Sm1 P2 72.4(3) . . ? O6 Sm1 P2 29.1(3) . . ? O16 Sm1 P2 106.0(3) . . ? O20 Sm1 P2 123.0(3) . . ? O7 Sm1 P2 29.3(3) . . ? O17 Sm1 P2 103.8(3) . . ? C22 Sm1 P2 97.4(4) . . ? C30 Sm1 P2 107.7(4) . . ? O7 Sm2 O9 75.3(4) 2_676 1_556 ? O7 Sm2 O1 76.1(4) 2_676 2_676 ? O9 Sm2 O1 80.8(4) 1_556 2_676 ? O7 Sm2 O23 79.1(4) 2_676 1_656 ? O9 Sm2 O23 69.1(4) 1_556 1_656 ? O1 Sm2 O23 144.9(4) 2_676 1_656 ? O7 Sm2 O13 118.8(4) 2_676 . ? O9 Sm2 O13 154.4(4) 1_556 . ? O1 Sm2 O13 82.3(4) 2_676 . ? O23 Sm2 O13 131.9(4) 1_656 . ? O7 Sm2 O12 65.1(4) 2_676 . ? O9 Sm2 O12 140.4(4) 1_556 . ? O1 Sm2 O12 87.7(3) 2_676 . ? O23 Sm2 O12 103.8(4) 1_656 . ? O13 Sm2 O12 57.3(4) . . ? O7 Sm2 O18 139.0(4) 2_676 2_566 ? O9 Sm2 O18 74.9(4) 1_556 2_566 ? O1 Sm2 O18 71.9(4) 2_676 2_566 ? O23 Sm2 O18 115.0(4) 1_656 2_566 ? O13 Sm2 O18 81.6(4) . 2_566 ? O12 Sm2 O18 136.5(4) . 2_566 ? O7 Sm2 O22 101.5(4) 2_676 1_656 ? O9 Sm2 O22 119.8(4) 1_556 1_656 ? O1 Sm2 O22 158.3(4) 2_676 1_656 ? O23 Sm2 O22 51.9(4) 1_656 1_656 ? O13 Sm2 O22 80.1(4) . 1_656 ? O12 Sm2 O22 72.1(4) . 1_656 ? O18 Sm2 O22 117.6(4) 2_566 1_656 ? O7 Sm2 O19 150.8(4) 2_676 2_566 ? O9 Sm2 O19 84.7(4) 1_556 2_566 ? O1 Sm2 O19 121.9(4) 2_676 2_566 ? O23 Sm2 O19 73.9(5) 1_656 2_566 ? O13 Sm2 O19 88.1(4) . 2_566 ? O12 Sm2 O19 132.3(4) . 2_566 ? O18 Sm2 O19 50.1(4) 2_566 2_566 ? O22 Sm2 O19 70.1(4) 1_656 2_566 ? O7 Sm2 C29 91.3(5) 2_676 1_656 ? O9 Sm2 C29 94.1(4) 1_556 1_656 ? O1 Sm2 C29 167.3(4) 2_676 1_656 ? O23 Sm2 C29 25.8(4) 1_656 1_656 ? O13 Sm2 C29 106.0(4) . 1_656 ? O12 Sm2 C29 88.8(4) . 1_656 ? O18 Sm2 C29 118.3(4) 2_566 1_656 ? O22 Sm2 C29 26.1(4) 1_656 1_656 ? O19 Sm2 C29 68.8(5) 2_566 1_656 ? O7 Sm2 C37 152.9(5) 2_676 2_566 ? O9 Sm2 C37 77.7(5) 1_556 2_566 ? O1 Sm2 C37 96.7(5) 2_676 2_566 ? O23 Sm2 C37 94.2(5) 1_656 2_566 ? O13 Sm2 C37 85.3(5) . 2_566 ? O12 Sm2 C37 141.5(5) . 2_566 ? O18 Sm2 C37 24.9(4) 2_566 2_566 ? O22 Sm2 C37 94.4(5) 1_656 2_566 ? O19 Sm2 C37 25.3(5) 2_566 2_566 ? C29 Sm2 C37 93.6(5) 1_656 2_566 ? O7 Sm2 P3 92.7(3) 2_676 . ? O9 Sm2 P3 163.6(3) 1_556 . ? O1 Sm2 P3 85.5(3) 2_676 . ? O23 Sm2 P3 120.2(3) 1_656 . ? O13 Sm2 P3 28.4(3) . . ? O12 Sm2 P3 29.0(3) . . ? O18 Sm2 P3 109.3(3) 2_566 . ? O22 Sm2 P3 73.1(3) 1_656 . ? O19 Sm2 P3 110.4(3) 2_566 . ? C29 Sm2 P3 97.4(4) 1_656 . ? C37 Sm2 P3 113.0(4) 2_566 . ? O2 Sm3 O11 73.9(4) 2_676 . ? O2 Sm3 O8 73.7(4) 2_676 . ? O11 Sm3 O8 109.4(4) . . ? O2 Sm3 O10 142.1(4) 2_676 2_675 ? O11 Sm3 O10 141.8(4) . 2_675 ? O8 Sm3 O10 79.7(4) . 2_675 ? O2 Sm3 O14 143.0(4) 2_676 2_776 ? O11 Sm3 O14 84.0(4) . 2_776 ? O8 Sm3 O14 142.7(4) . 2_776 ? O10 Sm3 O14 69.8(4) 2_675 2_776 ? O2 Sm3 O24 122.1(5) 2_676 . ? O11 Sm3 O24 73.0(5) . . ? O8 Sm3 O24 74.4(4) . . ? O10 Sm3 O24 74.3(5) 2_675 . ? O14 Sm3 O24 77.0(5) 2_776 . ? O2 Sm3 O3 77.5(4) 2_676 . ? O11 Sm3 O3 88.9(4) . . ? O8 Sm3 O3 139.5(4) . . ? O10 Sm3 O3 108.2(4) 2_675 . ? O14 Sm3 O3 72.7(4) 2_776 . ? O24 Sm3 O3 146.1(4) . . ? O2 Sm3 O1 77.1(4) 2_676 . ? O11 Sm3 O1 139.2(4) . . ? O8 Sm3 O1 88.9(4) . . ? O10 Sm3 O1 75.7(4) 2_675 . ? O14 Sm3 O1 103.4(4) 2_776 . ? O24 Sm3 O1 147.8(4) . . ? O3 Sm3 O1 56.9(4) . . ? O2 Sm3 P1 71.2(3) 2_676 . ? O11 Sm3 P1 112.8(3) . . ? O8 Sm3 P1 113.1(3) . . ? O10 Sm3 P1 95.8(3) 2_675 . ? O14 Sm3 P1 91.4(3) 2_776 . ? O24 Sm3 P1 166.7(4) . . ? O3 Sm3 P1 28.6(3) . . ? O1 Sm3 P1 28.9(2) . . ? O2 P1 O3 113.3(7) . . ? O2 P1 O1 114.3(6) . . ? O3 P1 O1 105.8(7) . . ? O2 P1 C1 106.4(8) . . ? O3 P1 C1 110.2(8) . . ? O1 P1 C1 106.7(7) . . ? O2 P1 Sm3 121.3(5) . . ? O3 P1 Sm3 53.5(4) . . ? O1 P1 Sm3 53.8(4) . . ? C1 P1 Sm3 132.2(6) . . ? O8 P2 O6 117.3(7) . . ? O8 P2 O7 113.2(7) . . ? O6 P2 O7 107.1(7) . . ? O8 P2 C8 108.7(8) . . ? O6 P2 C8 102.5(7) . . ? O7 P2 C8 107.1(8) . . ? O8 P2 Sm1 141.3(5) . . ? O6 P2 Sm1 52.7(5) . . ? O7 P2 Sm1 54.8(5) . . ? C8 P2 Sm1 110.0(6) . . ? O13 P3 O11 118.7(7) . . ? O13 P3 O12 105.8(7) . . ? O11 P3 O12 112.2(8) . . ? O13 P3 C15 105.0(7) . . ? O11 P3 C15 108.8(7) . . ? O12 P3 C15 105.3(7) . . ? O13 P3 Sm2 51.5(5) . . ? O11 P3 Sm2 138.3(5) . . ? O12 P3 Sm2 54.4(5) . . ? C15 P3 Sm2 112.8(6) . . ? P1 O1 Sm2 134.2(6) . 2_676 ? P1 O1 Sm3 97.3(5) . . ? Sm2 O1 Sm3 128.3(4) 2_676 . ? P1 O2 Sm3 167.4(7) . 2_676 ? P1 O3 Sm1 134.8(6) . 2_676 ? P1 O3 Sm3 97.9(5) . . ? Sm1 O3 Sm3 126.9(5) 2_676 . ? C7 O5 H5C 109.0 . . ? P2 O6 Sm1 98.2(6) . . ? P2 O7 Sm2 149.0(7) . 2_676 ? P2 O7 Sm1 95.8(5) . . ? Sm2 O7 Sm1 114.7(5) 2_676 . ? P2 O8 Sm3 131.5(7) . . ? C14 O9 Sm2 128.6(11) . 1_554 ? C14 O10 Sm3 135.7(11) . 2_675 ? P3 O11 Sm3 135.2(7) . . ? P3 O12 Sm1 147.3(7) . 2_676 ? P3 O12 Sm2 96.6(6) . . ? Sm1 O12 Sm2 114.3(5) 2_676 . ? P3 O13 Sm2 100.1(6) . . ? C21 O14 Sm3 135.1(12) . 2_776 ? C21 O15 Sm1 126.3(13) . 1_655 ? C30 O16 Sm1 96.9(12) . . ? C30 O17 Sm1 90.7(10) . . ? C37 O18 Sm2 95.7(11) . 2_566 ? C37 O19 Sm2 93.8(12) . 2_566 ? C22 O20 Sm1 88.7(11) . . ? C22 O21 Sm1 94.8(12) . . ? C29 O22 Sm2 90.7(11) . 1_454 ? C29 O23 Sm2 94.7(10) . 1_454 ? Sm3 O24 H24C 110.3 . . ? Sm3 O24 H24A 108.7 . . ? H24C O24 H24A 109.9 . . ? H1WA O1W H1WB 109.5 . . ? H2WB O2W H2WA 109.6 . . ? H3WA O3W H3WB 109.4 . . ? H4WA O4W H4WB 109.7 . . ? H5WA O5W H5WB 109.5 . . ? H6WA O6W H6WB 108.9 . . ? H7WA O7W H7WB 109.6 . . ? C2 N1 C6 113.2(15) . . ? C2 N1 C1 110.8(14) . . ? C6 N1 C1 113.5(14) . . ? C2 N1 H1C 106.2 . . ? C6 N1 H1C 106.4 . . ? C1 N1 H1C 106.1 . . ? C13 N2 C8 112.7(13) . . ? C13 N2 C9 109.5(14) . . ? C8 N2 C9 109.7(14) . . ? C13 N2 H2A 108.5 . . ? C8 N2 H2A 108.5 . . ? C9 N2 H2A 107.9 . . ? C16 N3 C15 112.3(14) . . ? C16 N3 C20 110.4(14) . . ? C15 N3 C20 111.6(13) . . ? C16 N3 H3C 106.6 . . ? C15 N3 H3C 108.3 . . ? C20 N3 H3C 107.3 . . ? N1 C1 P1 116.1(12) . . ? N1 C1 H1A 106.4 . . ? P1 C1 H1A 108.4 . . ? N1 C1 H1B 109.0 . . ? P1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? N1 C2 C3 109.0(16) . . ? N1 C2 H2B 107.0 . . ? C3 C2 H2B 108.0 . . ? N1 C2 H2C 113.5 . . ? C3 C2 H2C 111.0 . . ? H2B C2 H2C 108.1 . . ? C2 C3 C4 113.3(18) . . ? C2 C3 H3A 110.2 . . ? C4 C3 H3A 110.6 . . ? C2 C3 H3B 108.0 . . ? C4 C3 H3B 106.5 . . ? H3A C3 H3B 108.1 . . ? C7 C4 C5 111(2) . . ? C7 C4 C3 112.6(19) . . ? C5 C4 C3 111.9(18) . . ? C7 C4 H4A 108.4 . . ? C5 C4 H4A 105.4 . . ? C3 C4 H4A 106.6 . . ? C6 C5 C4 114.2(17) . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5A 111.4 . . ? C6 C5 H5B 107.6 . . ? C4 C5 H5B 105.7 . . ? H5A C5 H5B 108.3 . . ? N1 C6 C5 110.0(16) . . ? N1 C6 H6A 111.5 . . ? C5 C6 H6A 112.9 . . ? N1 C6 H6B 107.2 . . ? C5 C6 H6B 107.0 . . ? H6A C6 H6B 108.0 . . ? O4 C7 O5 124(3) . . ? O4 C7 C4 120(3) . . ? O5 C7 C4 117(3) . . ? N2 C8 P2 114.2(12) . . ? N2 C8 H8A 106.7 . . ? P2 C8 H8A 108.0 . . ? N2 C8 H8B 110.3 . . ? P2 C8 H8B 109.7 . . ? H8A C8 H8B 107.6 . . ? N2 C9 C10 113.5(16) . . ? N2 C9 H9A 108.4 . . ? C10 C9 H9A 109.8 . . ? N2 C9 H9B 108.5 . . ? C10 C9 H9B 108.3 . . ? H9A C9 H9B 108.3 . . ? C9 C10 C11 110.5(14) . . ? C9 C10 H10A 110.4 . . ? C11 C10 H10A 110.3 . . ? C9 C10 H10B 109.5 . . ? C11 C10 H10B 108.7 . . ? H10A C10 H10B 107.4 . . ? C12 C11 C10 111.7(14) . . ? C12 C11 C14 110.5(15) . . ? C10 C11 C14 113.0(14) . . ? C12 C11 H11A 107.2 . . ? C10 C11 H11A 106.4 . . ? C14 C11 H11A 107.7 . . ? C13 C12 C11 111.2(16) . . ? C13 C12 H12A 108.8 . . ? C11 C12 H12A 108.6 . . ? C13 C12 H12B 110.8 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? N2 C13 C12 111.8(14) . . ? N2 C13 H13A 109.0 . . ? C12 C13 H13A 108.4 . . ? N2 C13 H13B 108.9 . . ? C12 C13 H13B 111.1 . . ? H13A C13 H13B 107.5 . . ? O10 C14 O9 126.1(16) . . ? O10 C14 C11 118.5(15) . . ? O9 C14 C11 115.4(16) . . ? N3 C15 P3 113.4(12) . . ? N3 C15 H15A 108.1 . . ? P3 C15 H15A 107.8 . . ? N3 C15 H15B 109.3 . . ? P3 C15 H15B 110.2 . . ? H15A C15 H15B 107.9 . . ? N3 C16 C17 113.9(16) . . ? N3 C16 H16A 106.0 . . ? C17 C16 H16A 107.7 . . ? N3 C16 H16B 111.2 . . ? C17 C16 H16B 110.3 . . ? H16A C16 H16B 107.5 . . ? C16 C17 C18 112.4(16) . . ? C16 C17 H17A 110.9 . . ? C18 C17 H17A 110.3 . . ? C16 C17 H17B 108.2 . . ? C18 C17 H17B 106.4 . . ? H17A C17 H17B 108.4 . . ? C21 C18 C19 114.6(15) . . ? C21 C18 C17 113.9(15) . . ? C19 C18 C17 110.5(15) . . ? C21 C18 H18A 107.0 . . ? C19 C18 H18A 105.2 . . ? C17 C18 H18A 104.6 . . ? C20 C19 C18 114.4(15) . . ? C20 C19 H19A 108.1 . . ? C18 C19 H19A 109.8 . . ? C20 C19 H19B 110.1 . . ? C18 C19 H19B 106.6 . . ? H19A C19 H19B 107.6 . . ? C19 C20 N3 110.7(14) . . ? C19 C20 H20A 111.0 . . ? N3 C20 H20A 109.3 . . ? C19 C20 H20B 110.4 . . ? N3 C20 H20B 107.1 . . ? H20A C20 H20B 108.3 . . ? O14 C21 O15 123.1(18) . . ? O14 C21 C18 117.4(17) . . ? O15 C21 C18 119.5(17) . . ? O21 C22 O20 123.9(18) . . ? O21 C22 C23 120.5(17) . . ? O20 C22 C23 115.5(17) . . ? O21 C22 Sm1 59.8(10) . . ? O20 C22 Sm1 64.4(10) . . ? C23 C22 Sm1 169.5(13) . . ? C28 C23 C24 119.0(19) . . ? C28 C23 C22 121.9(17) . . ? C24 C23 C22 119.1(18) . . ? C23 C24 C25 121(2) . . ? C23 C24 H24B 118.4 . . ? C25 C24 H24B 120.7 . . ? C24 C25 C26 120.4(17) . . ? C24 C25 H25A 120.6 . . ? C26 C25 H25A 118.9 . . ? C27 C26 C25 115.2(18) . . ? C27 C26 C29 123.9(18) . . ? C25 C26 C29 120.8(17) . . ? C28 C27 C26 124(2) . . ? C28 C27 H27A 120.7 . . ? C26 C27 H27A 115.1 . . ? C27 C28 C23 120.2(18) . . ? C27 C28 H28A 119.9 . . ? C23 C28 H28A 119.7 . . ? O23 C29 O22 122.5(17) . . ? O23 C29 C26 116.4(16) . . ? O22 C29 C26 120.9(17) . . ? O23 C29 Sm2 59.5(9) . 1_454 ? O22 C29 Sm2 63.2(9) . 1_454 ? C26 C29 Sm2 175.9(13) . 1_454 ? O16 C30 O17 122.3(18) . . ? O16 C30 C31 119.5(18) . . ? O17 C30 C31 117.9(16) . . ? O16 C30 Sm1 58.8(10) . . ? O17 C30 Sm1 63.7(10) . . ? C31 C30 Sm1 168.7(12) . . ? C32 C31 C36 121(2) . . ? C32 C31 C30 118.0(17) . . ? C36 C31 C30 120.9(19) . . ? C31 C32 C33 118.5(18) . . ? C31 C32 H32A 119.8 . . ? C33 C32 H32A 121.8 . . ? C32 C33 C34 121.8(19) . . ? C32 C33 H33A 119.3 . . ? C34 C33 H33A 118.9 . . ? C35 C34 C33 117(2) . . ? C35 C34 C37 123.7(18) . . ? C33 C34 C37 119.4(18) . . ? C36 C35 C34 123(2) . . ? C36 C35 H35A 118.9 . . ? C34 C35 H35A 117.9 . . ? C35 C36 C31 119(2) . . ? C35 C36 H36A 121.5 . . ? C31 C36 H36A 119.8 . . ? O18 C37 O19 120.2(18) . . ? O18 C37 C34 119.7(18) . . ? O19 C37 C34 119.9(18) . . ? O18 C37 Sm2 59.4(10) . 2_566 ? O19 C37 Sm2 60.9(10) . 2_566 ? C34 C37 Sm2 173.0(14) . 2_566 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 22.90 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.566 _refine_diff_density_min -1.210 _refine_diff_density_rms 0.261 # Attachment 'szg170.cif' data_szg170 _database_code_depnum_ccdc_archive 'CCDC 849255' #TrackingRef 'szg170.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H61 N3 O31 P3 Tb3' _chemical_formula_weight 1613.56 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' Tb Tb -0.1723 4.1537 '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 14.976(4) _cell_length_b 15.080(4) _cell_length_c 15.116(5) _cell_angle_alpha 105.192(4) _cell_angle_beta 103.772(4) _cell_angle_gamma 117.338(4) _cell_volume 2658.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1478 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 20.96 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 4.135 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7306 _exptl_absorpt_correction_T_max 0.9521 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Smart Apex II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16484 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.1512 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.99 _reflns_number_total 12038 _reflns_number_gt 7245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12038 _refine_ls_number_parameters 694 _refine_ls_number_restraints 672 _refine_ls_R_factor_all 0.1280 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1661 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.18351(5) 0.88878(5) 0.32022(4) 0.01492(15) Uani 1 1 d . . . Tb2 Tb 0.55734(5) 0.86790(5) 0.69755(4) 0.01482(15) Uani 1 1 d . . . Tb3 Tb 0.58388(5) 0.93913(5) 0.35849(4) 0.01523(15) Uani 1 1 d . . . P1 P 0.6159(2) 1.1394(3) 0.5220(2) 0.0137(6) Uani 1 1 d . . . P2 P 0.3064(2) 0.8310(3) 0.2016(2) 0.0164(7) Uani 1 1 d . . . P3 P 0.6259(3) 0.8137(3) 0.5232(2) 0.0158(7) Uani 1 1 d . . . O1 O 0.5556(6) 1.0936(6) 0.4070(5) 0.0165(18) Uani 1 1 d . . . O2 O 0.5436(6) 1.1240(7) 0.5785(6) 0.0172(18) Uani 1 1 d U . . O3 O 0.6818(6) 1.0872(6) 0.5367(5) 0.0140(17) Uani 1 1 d . . . O4 O 0.9344(11) 1.6155(12) 1.0304(8) 0.083(5) Uani 1 1 d . . . O5 O 0.7744(14) 1.5982(15) 1.0021(10) 0.138(8) Uani 1 1 d . . . H5C H 0.7993 1.6222 1.0659 0.207 Uiso 1 1 d R . . O6 O 0.2204(6) 0.7573(6) 0.2320(6) 0.0163(18) Uani 1 1 d . . . O7 O 0.3269(6) 0.9442(7) 0.2509(6) 0.0185(19) Uani 1 1 d . . . O8 O 0.4075(6) 0.8297(6) 0.2176(6) 0.0179(18) Uani 1 1 d . . . O9 O 0.5037(7) 0.9464(7) -0.1845(6) 0.022(2) Uani 1 1 d . . . O10 O 0.3707(7) 0.9732(7) -0.2487(6) 0.026(2) Uani 1 1 d U . . O11 O 0.6123(6) 0.8223(7) 0.4239(6) 0.0193(19) Uani 1 1 d . . . O12 O 0.6892(6) 0.9239(6) 0.6143(6) 0.0199(19) Uani 1 1 d . . . O13 O 0.5211(6) 0.7399(7) 0.5343(6) 0.0202(19) Uani 1 1 d . . . O14 O 1.2185(6) 0.9621(7) 0.5974(6) 0.028(2) Uani 1 1 d . . . O15 O 1.1390(7) 0.9583(7) 0.4515(6) 0.023(2) Uani 1 1 d . . . O16 O 0.0907(7) 0.7330(7) 0.3639(7) 0.031(2) Uani 1 1 d . . . O17 O -0.0175(7) 0.7144(7) 0.2250(7) 0.032(2) Uani 1 1 d . . . O18 O -0.3560(7) 0.2757(7) 0.3555(6) 0.027(2) Uani 1 1 d . . . O19 O -0.4722(8) 0.2980(8) 0.2600(8) 0.040(3) Uani 1 1 d . . . O20 O 0.0588(7) 0.9461(8) 0.2602(6) 0.033(2) Uani 1 1 d . . . O21 O 0.1030(7) 0.8686(8) 0.1511(6) 0.031(2) Uani 1 1 d . . . O22 O -0.3045(7) 0.8201(8) -0.2451(6) 0.030(2) Uani 1 1 d . . . O23 O -0.3200(7) 0.9275(8) -0.1308(7) 0.032(2) Uani 1 1 d . . . O24 O 0.5946(8) 0.8141(8) 0.2304(7) 0.044(3) Uani 1 1 d . . . H24C H 0.6558 0.8489 0.2264 0.052 Uiso 1 1 d R . . H24A H 0.5894 0.7622 0.2459 0.065 Uiso 1 1 d R . . O1W O 0.8325(8) 0.2555(8) 0.4005(7) 0.051(3) Uani 1 1 d . . . H1WA H 0.8296 0.2358 0.4481 0.076 Uiso 1 1 d R . . H1WB H 0.8015 0.1988 0.3451 0.076 Uiso 1 1 d R . . O2W O 0.3937(14) 0.5203(11) 0.4940(12) 0.126(7) Uani 1 1 d . . . H2WB H 0.4637 0.5556 0.5154 0.151 Uiso 1 1 d R . . H2WA H 0.3752 0.5086 0.5408 0.189 Uiso 1 1 d R . . O3W O 0.6815(19) 0.6191(19) 0.7003(17) 0.204(10) Uani 1 1 d U . . H3WA H 0.6739 0.6201 0.7545 0.306 Uiso 1 1 d R . . H3WB H 0.6583 0.5538 0.6614 0.306 Uiso 1 1 d R . . O4W O 0.5873(19) 0.6199(17) 0.2059(19) 0.214(12) Uani 1 1 d . . . H4WA H 0.6009 0.5969 0.2498 0.321 Uiso 1 1 d R . . H4WB H 0.5516 0.5666 0.1474 0.321 Uiso 1 1 d R . . O5W O 0.764(4) 0.754(4) 0.186(4) 0.51(3) Uani 1 1 d U . . H5WA H 0.8081 0.7630 0.2406 0.760 Uiso 1 1 d R . . H5WB H 0.7317 0.6876 0.1421 0.760 Uiso 1 1 d R . . O6W O 0.0273(19) 0.679(2) 0.690(2) 0.261(15) Uani 1 1 d . . . H6WA H -0.0056 0.7062 0.7132 0.391 Uiso 1 1 d R . . H6WB H -0.0157 0.6092 0.6604 0.391 Uiso 1 1 d R . . O7W O 0.505(2) 0.477(3) 0.290(2) 0.300(16) Uani 1 1 d U . . H7WA H 0.4953 0.4453 0.3291 0.450 Uiso 1 1 d R . . H7WB H 0.4728 0.4284 0.2295 0.450 Uiso 1 1 d R . . N1 N 0.7467(8) 1.3575(8) 0.6754(7) 0.021(2) Uani 1 1 d . . . H1C H 0.7527 1.3181 0.7092 0.025 Uiso 1 1 d R . . N2 N 0.2893(8) 0.8396(8) 0.0161(7) 0.018(2) Uani 1 1 d U . . H2A H 0.3437 0.9084 0.0637 0.022 Uiso 1 1 d R . . N3 N 0.8187(8) 0.8225(8) 0.5423(7) 0.021(2) Uani 1 1 d . . . H3C H 0.8360 0.8918 0.5572 0.025 Uiso 1 1 d R . . C1 C 0.7107(10) 1.2904(10) 0.5673(9) 0.023(3) Uani 1 1 d U . . H1A H 0.6754 1.3151 0.5279 0.027 Uiso 1 1 d R . . H1B H 0.7757 1.3049 0.5564 0.027 Uiso 1 1 d R . . C2 C 0.8561(11) 1.4654(11) 0.7209(10) 0.036(3) Uani 1 1 d U . . H2B H 0.8491 1.5122 0.6912 0.043 Uiso 1 1 d R . . H2C H 0.9093 1.4527 0.7062 0.043 Uiso 1 1 d R . . C3 C 0.8957(12) 1.5232(12) 0.8333(11) 0.045(3) Uani 1 1 d U . . H3A H 0.9661 1.5923 0.8618 0.053 Uiso 1 1 d R . . H3B H 0.9045 1.4772 0.8632 0.053 Uiso 1 1 d R . . C4 C 0.8109(12) 1.5423(12) 0.8588(11) 0.044(3) Uani 1 1 d U . . H4A H 0.8087 1.5954 0.8361 0.052 Uiso 1 1 d R . . C5 C 0.6940(12) 1.4345(12) 0.8040(10) 0.043(3) Uani 1 1 d U . . H5A H 0.6408 1.4497 0.8143 0.051 Uiso 1 1 d R . . H5B H 0.6936 1.3843 0.8323 0.051 Uiso 1 1 d R . . C6 C 0.6631(11) 1.3807(12) 0.6925(10) 0.034(3) Uani 1 1 d U . . H6A H 0.5904 1.3137 0.6580 0.041 Uiso 1 1 d R . . H6B H 0.6634 1.4312 0.6648 0.041 Uiso 1 1 d R . . C7 C 0.8412(17) 1.5880(14) 0.9757(14) 0.058(4) Uani 1 1 d U . . C8 C 0.2257(10) 0.7782(11) 0.0662(9) 0.023(2) Uani 1 1 d U . . H8A H 0.1630 0.7835 0.0575 0.027 Uiso 1 1 d R . . H8B H 0.1987 0.7015 0.0327 0.027 Uiso 1 1 d R . . C9 C 0.3401(10) 0.7839(10) -0.0277(9) 0.022(2) Uani 1 1 d U . . H9A H 0.2826 0.7098 -0.0773 0.027 Uiso 1 1 d R . . H9B H 0.3866 0.7799 0.0249 0.027 Uiso 1 1 d R . . C10 C 0.4076(10) 0.8464(11) -0.0761(9) 0.024(2) Uani 1 1 d U . . H10A H 0.4346 0.8062 -0.1077 0.029 Uiso 1 1 d R . . H10B H 0.4705 0.9170 -0.0247 0.029 Uiso 1 1 d R . . C11 C 0.3426(10) 0.8658(11) -0.1535(9) 0.021(2) Uani 1 1 d U . . H11A H 0.2863 0.7942 -0.2079 0.026 Uiso 1 1 d R . . C12 C 0.2811(10) 0.9114(10) -0.1127(9) 0.021(2) Uani 1 1 d U . . H12A H 0.2314 0.9112 -0.1664 0.026 Uiso 1 1 d R . . H12B H 0.3348 0.9867 -0.0638 0.026 Uiso 1 1 d R . . C13 C 0.2190(10) 0.8491(11) -0.0623(9) 0.023(2) Uani 1 1 d U . . H13A H 0.1873 0.8848 -0.0329 0.027 Uiso 1 1 d R . . H13B H 0.1597 0.7760 -0.1125 0.027 Uiso 1 1 d R . . C14 C 0.4123(10) 0.9348(10) -0.1993(9) 0.020(2) Uani 1 1 d U . . C15 C 0.7085(9) 0.7555(10) 0.5416(9) 0.018(2) Uani 1 1 d U . . H15A H 0.6694 0.6827 0.4881 0.022 Uiso 1 1 d R . . H15B H 0.7181 0.7491 0.6042 0.022 Uiso 1 1 d R . . C16 C 0.9059(9) 0.8274(10) 0.6188(9) 0.019(2) Uani 1 1 d U . . H16A H 0.8885 0.7536 0.6007 0.023 Uiso 1 1 d R . . H16B H 0.9055 0.8535 0.6838 0.023 Uiso 1 1 d R . . C17 C 1.0203(10) 0.9000(10) 0.6239(9) 0.021(2) Uani 1 1 d U . . H17A H 1.0743 0.9004 0.6735 0.025 Uiso 1 1 d R . . H17B H 1.0391 0.9744 0.6434 0.025 Uiso 1 1 d R . . C18 C 1.0223(10) 0.8593(10) 0.5210(8) 0.018(2) Uani 1 1 d U . . H18A H 1.0081 0.7869 0.5054 0.022 Uiso 1 1 d R . . C19 C 0.9293(10) 0.8474(10) 0.4394(9) 0.022(2) Uani 1 1 d U . . H19A H 0.9265 0.8139 0.3744 0.026 Uiso 1 1 d R . . H19B H 0.9450 0.9196 0.4503 0.026 Uiso 1 1 d R . . C20 C 0.8158(10) 0.7771(10) 0.4419(9) 0.024(2) Uani 1 1 d U . . H20A H 0.7590 0.7734 0.3921 0.028 Uiso 1 1 d R . . H20B H 0.7974 0.7032 0.4263 0.028 Uiso 1 1 d R . . C21 C 1.1365(10) 0.9334(10) 0.5233(9) 0.019(2) Uani 1 1 d U . . C22 C 0.0451(11) 0.9038(11) 0.1700(10) 0.025(2) Uani 1 1 d U . . C23 C -0.0374(11) 0.8974(11) 0.0871(10) 0.028(2) Uani 1 1 d U . . C24 C -0.0470(10) 0.8574(11) -0.0106(9) 0.026(2) Uani 1 1 d U . . H24B H 0.0005 0.8344 -0.0235 0.032 Uiso 1 1 d R . . C25 C -0.1257(10) 0.8495(11) -0.0916(10) 0.027(2) Uani 1 1 d U . . H25A H -0.1295 0.8260 -0.1586 0.032 Uiso 1 1 d R . . C26 C -0.1965(11) 0.8767(11) -0.0712(10) 0.026(2) Uani 1 1 d U . . C27 C -0.1907(11) 0.9124(11) 0.0243(9) 0.028(2) Uani 1 1 d U . . H27A H -0.2401 0.9326 0.0368 0.034 Uiso 1 1 d R . . C28 C -0.1125(10) 0.9202(11) 0.1039(10) 0.030(2) Uani 1 1 d U . . H28A H -0.1116 0.9403 0.1700 0.036 Uiso 1 1 d R . . C29 C -0.2782(10) 0.8736(11) -0.1542(10) 0.023(2) Uani 1 1 d U . . C30 C -0.0036(10) 0.6831(10) 0.2934(9) 0.022(2) Uani 1 1 d U . . C31 C -0.1017(10) 0.5873(11) 0.2946(9) 0.026(2) Uani 1 1 d U . . C32 C -0.0842(10) 0.5572(11) 0.3702(10) 0.027(2) Uani 1 1 d U . . H32A H -0.0103 0.5942 0.4202 0.033 Uiso 1 1 d R . . C33 C -0.1726(10) 0.4730(11) 0.3757(10) 0.027(2) Uani 1 1 d U . . H33A H -0.1609 0.4498 0.4284 0.033 Uiso 1 1 d R . . C34 C -0.2781(10) 0.4228(11) 0.3042(10) 0.028(2) Uani 1 1 d U . . C35 C -0.2946(11) 0.4527(11) 0.2269(10) 0.032(3) Uani 1 1 d U . . H35A H -0.3683 0.4185 0.1777 0.039 Uiso 1 1 d R . . C36 C -0.2051(10) 0.5342(11) 0.2219(9) 0.028(2) Uani 1 1 d U . . H36A H -0.2155 0.5533 0.1663 0.033 Uiso 1 1 d R . . C37 C -0.3742(11) 0.3274(11) 0.3065(10) 0.026(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0116(3) 0.0205(3) 0.0129(3) 0.0099(2) 0.0053(2) 0.0076(3) Tb2 0.0126(3) 0.0202(3) 0.0136(3) 0.0103(2) 0.0061(2) 0.0087(3) Tb3 0.0134(3) 0.0220(3) 0.0130(3) 0.0103(3) 0.0072(2) 0.0096(3) P1 0.0103(15) 0.0178(17) 0.0116(15) 0.0076(13) 0.0047(12) 0.0062(13) P2 0.0112(16) 0.0211(18) 0.0124(16) 0.0081(14) 0.0038(13) 0.0061(14) P3 0.0136(16) 0.0193(17) 0.0169(16) 0.0107(14) 0.0088(13) 0.0082(14) O1 0.018(4) 0.027(5) 0.010(4) 0.013(4) 0.009(3) 0.013(4) O2 0.015(4) 0.030(5) 0.018(4) 0.015(3) 0.013(3) 0.015(3) O3 0.011(4) 0.018(4) 0.016(4) 0.009(4) 0.003(3) 0.011(4) O4 0.064(9) 0.117(12) 0.020(6) 0.008(7) 0.005(6) 0.034(9) O5 0.146(16) 0.19(2) 0.045(9) 0.003(11) 0.042(10) 0.098(15) O6 0.019(5) 0.020(5) 0.012(4) 0.010(4) 0.007(3) 0.010(4) O7 0.015(4) 0.025(5) 0.018(4) 0.011(4) 0.008(4) 0.011(4) O8 0.020(5) 0.022(5) 0.014(4) 0.007(4) 0.008(4) 0.013(4) O9 0.026(5) 0.034(5) 0.021(5) 0.022(4) 0.018(4) 0.018(4) O10 0.028(5) 0.034(5) 0.026(5) 0.024(4) 0.013(4) 0.018(4) O11 0.022(5) 0.030(5) 0.013(4) 0.014(4) 0.011(4) 0.014(4) O12 0.015(4) 0.012(4) 0.020(5) 0.002(4) 0.004(4) 0.002(4) O13 0.014(4) 0.030(5) 0.018(4) 0.015(4) 0.005(4) 0.011(4) O14 0.010(4) 0.046(6) 0.023(5) 0.019(5) 0.007(4) 0.010(4) O15 0.021(5) 0.038(6) 0.019(5) 0.018(4) 0.010(4) 0.018(4) O16 0.011(5) 0.035(6) 0.034(5) 0.018(5) 0.001(4) 0.006(4) O17 0.026(5) 0.027(5) 0.026(5) 0.015(4) 0.008(4) 0.002(4) O18 0.026(5) 0.034(6) 0.029(5) 0.025(5) 0.015(4) 0.015(4) O19 0.026(6) 0.041(6) 0.060(7) 0.032(6) 0.026(5) 0.015(5) O20 0.038(6) 0.043(6) 0.015(5) 0.006(4) 0.000(4) 0.028(5) O21 0.023(5) 0.055(7) 0.022(5) 0.025(5) 0.010(4) 0.023(5) O22 0.020(5) 0.046(6) 0.021(5) 0.013(5) 0.008(4) 0.019(5) O23 0.029(6) 0.041(6) 0.027(5) 0.018(5) 0.003(4) 0.022(5) O24 0.053(7) 0.051(7) 0.034(6) 0.015(5) 0.022(5) 0.035(6) O1W 0.057(8) 0.048(7) 0.030(6) 0.015(5) 0.012(5) 0.021(6) O2W 0.178(17) 0.050(10) 0.117(14) 0.035(10) 0.060(13) 0.043(11) O3W 0.229(13) 0.191(13) 0.198(13) 0.098(9) 0.076(9) 0.121(9) O4W 0.22(3) 0.13(2) 0.25(3) 0.071(19) 0.04(2) 0.104(19) O5W 0.51(3) 0.51(3) 0.50(3) 0.218(17) 0.211(16) 0.28(2) O6W 0.19(2) 0.28(3) 0.38(4) 0.18(3) 0.20(3) 0.12(2) O7W 0.304(17) 0.297(17) 0.305(17) 0.129(9) 0.125(9) 0.173(11) N1 0.012(5) 0.014(5) 0.013(5) 0.003(4) -0.009(4) -0.002(4) N2 0.011(5) 0.022(5) 0.013(5) 0.008(4) 0.009(4) 0.002(4) N3 0.017(6) 0.023(6) 0.022(6) 0.011(5) 0.010(5) 0.010(5) C1 0.024(5) 0.029(5) 0.018(5) 0.009(4) 0.013(4) 0.014(4) C2 0.037(5) 0.030(5) 0.028(5) 0.006(4) 0.014(4) 0.011(4) C3 0.042(5) 0.032(5) 0.033(5) 0.007(4) 0.011(4) 0.008(4) C4 0.043(5) 0.033(5) 0.032(5) 0.001(4) 0.015(4) 0.011(4) C5 0.044(5) 0.031(5) 0.034(5) 0.005(4) 0.015(4) 0.012(4) C6 0.036(5) 0.031(5) 0.026(5) 0.005(4) 0.012(4) 0.016(4) C7 0.054(6) 0.039(6) 0.040(6) 0.002(5) 0.015(5) 0.007(5) C8 0.018(4) 0.034(5) 0.021(4) 0.015(4) 0.013(4) 0.013(4) C9 0.022(4) 0.030(4) 0.021(4) 0.014(3) 0.012(3) 0.016(3) C10 0.022(4) 0.032(4) 0.022(4) 0.012(4) 0.014(3) 0.015(3) C11 0.020(4) 0.029(4) 0.019(4) 0.015(3) 0.011(3) 0.013(3) C12 0.020(4) 0.033(4) 0.020(4) 0.018(3) 0.010(3) 0.016(3) C13 0.017(4) 0.035(4) 0.019(4) 0.015(3) 0.013(3) 0.013(3) C14 0.017(4) 0.031(5) 0.015(4) 0.010(4) 0.011(4) 0.013(4) C15 0.018(4) 0.022(4) 0.024(4) 0.016(4) 0.014(4) 0.011(3) C16 0.022(4) 0.024(4) 0.017(4) 0.012(3) 0.013(3) 0.013(3) C17 0.024(4) 0.023(4) 0.017(4) 0.009(3) 0.010(3) 0.013(3) C18 0.023(4) 0.021(4) 0.014(3) 0.012(3) 0.010(3) 0.011(3) C19 0.025(4) 0.023(4) 0.019(4) 0.005(3) 0.009(3) 0.017(3) C20 0.023(4) 0.027(4) 0.018(4) 0.008(3) 0.008(3) 0.013(3) C21 0.023(5) 0.021(4) 0.018(4) 0.003(4) 0.012(4) 0.017(4) C22 0.022(4) 0.034(4) 0.027(4) 0.018(3) 0.010(3) 0.018(3) C23 0.025(4) 0.038(4) 0.026(4) 0.019(4) 0.011(3) 0.018(4) C24 0.025(4) 0.039(4) 0.023(4) 0.019(3) 0.012(3) 0.019(3) C25 0.027(4) 0.037(4) 0.024(4) 0.019(3) 0.012(3) 0.021(3) C26 0.026(4) 0.036(4) 0.026(4) 0.020(4) 0.007(3) 0.023(3) C27 0.027(4) 0.038(4) 0.025(4) 0.018(3) 0.010(3) 0.020(3) C28 0.025(4) 0.042(4) 0.025(4) 0.018(4) 0.009(3) 0.020(3) C29 0.024(4) 0.038(4) 0.022(4) 0.020(4) 0.014(3) 0.021(4) C30 0.014(4) 0.026(4) 0.020(4) 0.010(3) 0.007(3) 0.008(3) C31 0.018(4) 0.029(4) 0.021(4) 0.011(3) 0.006(3) 0.008(3) C32 0.018(4) 0.031(4) 0.023(4) 0.014(3) 0.002(3) 0.008(3) C33 0.018(4) 0.030(4) 0.024(4) 0.014(3) 0.007(3) 0.006(3) C34 0.018(4) 0.030(4) 0.025(4) 0.011(3) 0.008(3) 0.007(3) C35 0.019(4) 0.033(4) 0.024(4) 0.012(3) 0.003(3) 0.003(3) C36 0.021(4) 0.031(4) 0.020(4) 0.015(3) 0.005(3) 0.005(3) C37 0.019(4) 0.031(4) 0.021(4) 0.009(4) 0.009(3) 0.010(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 Tb1 O12 2.299(8) 2_676 ? Tb1 O15 2.379(8) 1_455 ? Tb1 O3 2.392(7) 2_676 ? Tb1 O21 2.423(8) . ? Tb1 O6 2.447(8) . ? Tb1 O16 2.477(9) . ? Tb1 O20 2.479(9) . ? Tb1 O7 2.508(8) . ? Tb1 O17 2.595(8) . ? Tb1 C22 2.822(13) . ? Tb1 C30 2.908(12) . ? Tb1 P2 3.096(3) . ? Tb2 O7 2.309(8) 2_676 ? Tb2 O9 2.382(8) 1_556 ? Tb2 O1 2.410(8) 2_676 ? Tb2 O23 2.430(9) 1_656 ? Tb2 O13 2.452(8) . ? Tb2 O18 2.524(8) 2_566 ? Tb2 O22 2.528(9) 1_656 ? Tb2 O12 2.531(8) . ? Tb2 O19 2.569(9) 2_566 ? Tb2 C29 2.858(13) 1_656 ? Tb2 C37 2.934(13) 2_566 ? Tb2 P3 3.098(3) . ? Tb3 O2 2.265(7) 2_676 ? Tb3 O11 2.380(8) . ? Tb3 O8 2.390(8) . ? Tb3 O10 2.414(8) 2_675 ? Tb3 O24 2.416(9) . ? Tb3 O14 2.432(8) 2_776 ? Tb3 O1 2.510(8) . ? Tb3 O3 2.520(7) . ? Tb3 P1 3.107(3) . ? P1 O2 1.505(8) . ? P1 O3 1.531(8) . ? P1 O1 1.539(8) . ? P1 C1 1.849(12) . ? P2 O8 1.485(8) . ? P2 O7 1.519(8) . ? P2 O6 1.529(8) . ? P2 C8 1.835(12) . ? P3 O12 1.513(8) . ? P3 O11 1.514(8) . ? P3 O13 1.532(8) . ? P3 C15 1.828(12) . ? O1 Tb2 2.410(8) 2_676 ? O2 Tb3 2.265(7) 2_676 ? O3 Tb1 2.392(7) 2_676 ? O4 C7 1.24(2) . ? O5 C7 1.22(2) . ? O5 H5C 0.8500 . ? O7 Tb2 2.309(8) 2_676 ? O9 C14 1.252(13) . ? O9 Tb2 2.382(8) 1_554 ? O10 C14 1.272(15) . ? O10 Tb3 2.414(8) 2_675 ? O12 Tb1 2.299(8) 2_676 ? O14 C21 1.246(14) . ? O14 Tb3 2.432(8) 2_776 ? O15 C21 1.241(14) . ? O15 Tb1 2.379(8) 1_655 ? O16 C30 1.258(13) . ? O17 C30 1.256(15) . ? O18 C37 1.277(15) . ? O18 Tb2 2.524(8) 2_566 ? O19 C37 1.262(14) . ? O19 Tb2 2.569(9) 2_566 ? O20 C22 1.265(15) . ? O21 C22 1.255(15) . ? O22 C29 1.251(14) . ? O22 Tb2 2.528(9) 1_454 ? O23 C29 1.263(15) . ? O23 Tb2 2.430(8) 1_454 ? O24 H24C 0.8500 . ? O24 H24A 0.8500 . ? O1W H1WA 0.8499 . ? O1W H1WB 0.8500 . ? O2W H2WB 0.8500 . ? O2W H2WA 0.8502 . ? O3W H3WA 0.8501 . ? O3W H3WB 0.8499 . ? O4W H4WA 0.8501 . ? O4W H4WB 0.8500 . ? O5W H5WA 0.8500 . ? O5W H5WB 0.8500 . ? O6W H6WA 0.8499 . ? O6W H6WB 0.8500 . ? O7W H7WA 0.8499 . ? O7W H7WB 0.8501 . ? N1 C1 1.483(14) . ? N1 C2 1.494(15) . ? N1 C6 1.504(16) . ? N1 H1C 0.9001 . ? N2 C13 1.472(15) . ? N2 C8 1.496(14) . ? N2 C9 1.504(15) . ? N2 H2A 0.9000 . ? N3 C20 1.473(14) . ? N3 C16 1.481(15) . ? N3 C15 1.483(14) . ? N3 H3C 0.9001 . ? C1 H1A 0.9599 . ? C1 H1B 0.9601 . ? C2 C3 1.507(18) . ? C2 H2B 0.9600 . ? C2 H2C 0.9601 . ? C3 C4 1.53(2) . ? C3 H3A 0.9601 . ? C3 H3B 0.9600 . ? C4 C5 1.545(18) . ? C4 C7 1.58(2) . ? C4 H4A 0.9600 . ? C5 C6 1.511(18) . ? C5 H5A 0.9599 . ? C5 H5B 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C8 H8A 0.9601 . ? C8 H8B 0.9600 . ? C9 C10 1.511(16) . ? C9 H9A 0.9600 . ? C9 H9B 0.9599 . ? C10 C11 1.519(17) . ? C10 H10A 0.9601 . ? C10 H10B 0.9600 . ? C11 C12 1.526(16) . ? C11 C14 1.541(16) . ? C11 H11A 0.9600 . ? C12 C13 1.496(15) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C13 H13A 0.9599 . ? C13 H13B 0.9600 . ? C15 H15A 0.9601 . ? C15 H15B 0.9600 . ? C16 C17 1.520(15) . ? C16 H16A 0.9600 . ? C16 H16B 0.9601 . ? C17 C18 1.528(15) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C18 C19 1.526(16) . ? C18 C21 1.539(16) . ? C18 H18A 0.9600 . ? C19 C20 1.553(16) . ? C19 H19A 0.9599 . ? C19 H19B 0.9600 . ? C20 H20A 0.9598 . ? C20 H20B 0.9599 . ? C22 C23 1.482(17) . ? C23 C28 1.376(18) . ? C23 C24 1.386(17) . ? C24 C25 1.418(17) . ? C24 H24B 0.9599 . ? C25 C26 1.369(17) . ? C25 H25A 0.9599 . ? C26 C27 1.368(17) . ? C26 C29 1.503(17) . ? C27 C28 1.401(17) . ? C27 H27A 0.9601 . ? C28 H28A 0.9600 . ? C29 Tb2 2.858(13) 1_454 ? C30 C31 1.524(17) . ? C31 C32 1.349(17) . ? C31 C36 1.355(16) . ? C32 C33 1.391(17) . ? C32 H32A 0.9600 . ? C33 C34 1.378(16) . ? C33 H33A 0.9601 . ? C34 C35 1.368(18) . ? C34 C37 1.513(17) . ? C35 C36 1.377(17) . ? C35 H35A 0.9600 . ? C36 H36A 0.9599 . ? C37 Tb2 2.934(13) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Tb1 O15 78.2(3) 2_676 1_455 ? O12 Tb1 O3 80.3(3) 2_676 2_676 ? O15 Tb1 O3 79.1(3) 1_455 2_676 ? O12 Tb1 O21 94.5(3) 2_676 . ? O15 Tb1 O21 122.3(3) 1_455 . ? O3 Tb1 O21 156.8(3) 2_676 . ? O12 Tb1 O6 120.7(3) 2_676 . ? O15 Tb1 O6 150.0(3) 1_455 . ? O3 Tb1 O6 81.5(2) 2_676 . ? O21 Tb1 O6 81.8(3) . . ? O12 Tb1 O16 144.3(3) 2_676 . ? O15 Tb1 O16 75.0(3) 1_455 . ? O3 Tb1 O16 71.8(3) 2_676 . ? O21 Tb1 O16 119.7(3) . . ? O6 Tb1 O16 77.3(3) . . ? O12 Tb1 O20 80.4(3) 2_676 . ? O15 Tb1 O20 69.7(3) 1_455 . ? O3 Tb1 O20 146.0(3) 2_676 . ? O21 Tb1 O20 52.7(3) . . ? O6 Tb1 O20 132.5(3) . . ? O16 Tb1 O20 111.1(3) . . ? O12 Tb1 O7 65.1(3) 2_676 . ? O15 Tb1 O7 142.6(3) 1_455 . ? O3 Tb1 O7 87.5(3) 2_676 . ? O21 Tb1 O7 70.0(3) . . ? O6 Tb1 O7 58.1(3) . . ? O16 Tb1 O7 133.3(3) . . ? O20 Tb1 O7 109.1(3) . . ? O12 Tb1 O17 152.2(3) 2_676 . ? O15 Tb1 O17 90.0(3) 1_455 . ? O3 Tb1 O17 122.5(3) 2_676 . ? O21 Tb1 O17 70.4(3) . . ? O6 Tb1 O17 81.3(3) . . ? O16 Tb1 O17 50.9(3) . . ? O20 Tb1 O17 71.8(3) . . ? O7 Tb1 O17 126.0(3) . . ? O12 Tb1 C22 89.3(3) 2_676 . ? O15 Tb1 C22 96.0(3) 1_455 . ? O3 Tb1 C22 169.2(3) 2_676 . ? O21 Tb1 C22 26.3(3) . . ? O6 Tb1 C22 106.6(3) . . ? O16 Tb1 C22 116.4(3) . . ? O20 Tb1 C22 26.6(3) . . ? O7 Tb1 C22 90.8(3) . . ? O17 Tb1 C22 66.6(3) . . ? O12 Tb1 C30 158.2(3) 2_676 . ? O15 Tb1 C30 80.0(3) 1_455 . ? O3 Tb1 C30 97.3(3) 2_676 . ? O21 Tb1 C30 95.6(3) . . ? O6 Tb1 C30 79.9(3) . . ? O16 Tb1 C30 25.5(3) . . ? O20 Tb1 C30 90.5(4) . . ? O7 Tb1 C30 136.7(3) . . ? O17 Tb1 C30 25.6(3) . . ? C22 Tb1 C30 91.2(4) . . ? O12 Tb1 P2 93.4(2) 2_676 . ? O15 Tb1 P2 163.3(2) 1_455 . ? O3 Tb1 P2 85.37(19) 2_676 . ? O21 Tb1 P2 72.3(2) . . ? O6 Tb1 P2 29.13(19) . . ? O16 Tb1 P2 105.9(2) . . ? O20 Tb1 P2 123.6(2) . . ? O7 Tb1 P2 29.11(19) . . ? O17 Tb1 P2 103.4(2) . . ? C22 Tb1 P2 98.3(3) . . ? C30 Tb1 P2 108.1(3) . . ? O7 Tb2 O9 76.3(3) 2_676 1_556 ? O7 Tb2 O1 77.1(3) 2_676 2_676 ? O9 Tb2 O1 80.0(3) 1_556 2_676 ? O7 Tb2 O23 78.4(3) 2_676 1_656 ? O9 Tb2 O23 69.4(3) 1_556 1_656 ? O1 Tb2 O23 144.5(3) 2_676 1_656 ? O7 Tb2 O13 119.0(3) 2_676 . ? O9 Tb2 O13 153.8(3) 1_556 . ? O1 Tb2 O13 83.0(3) 2_676 . ? O23 Tb2 O13 131.8(3) 1_656 . ? O7 Tb2 O18 139.3(3) 2_676 2_566 ? O9 Tb2 O18 74.0(3) 1_556 2_566 ? O1 Tb2 O18 70.8(3) 2_676 2_566 ? O23 Tb2 O18 115.3(3) 1_656 2_566 ? O13 Tb2 O18 81.6(3) . 2_566 ? O7 Tb2 O22 101.2(3) 2_676 1_656 ? O9 Tb2 O22 119.9(3) 1_556 1_656 ? O1 Tb2 O22 159.4(3) 2_676 1_656 ? O23 Tb2 O22 52.0(3) 1_656 1_656 ? O13 Tb2 O22 79.9(3) . 1_656 ? O18 Tb2 O22 117.6(3) 2_566 1_656 ? O7 Tb2 O12 64.6(3) 2_676 . ? O9 Tb2 O12 140.9(3) 1_556 . ? O1 Tb2 O12 89.6(3) 2_676 . ? O23 Tb2 O12 102.7(3) 1_656 . ? O13 Tb2 O12 58.2(2) . . ? O18 Tb2 O12 137.5(3) 2_566 . ? O22 Tb2 O12 71.6(3) 1_656 . ? O7 Tb2 O19 150.1(3) 2_676 2_566 ? O9 Tb2 O19 84.3(3) 1_556 2_566 ? O1 Tb2 O19 121.9(3) 2_676 2_566 ? O23 Tb2 O19 73.5(3) 1_656 2_566 ? O13 Tb2 O19 88.0(3) . 2_566 ? O18 Tb2 O19 51.1(3) 2_566 2_566 ? O22 Tb2 O19 69.1(3) 1_656 2_566 ? O12 Tb2 O19 131.7(3) . 2_566 ? O7 Tb2 C29 90.6(3) 2_676 1_656 ? O9 Tb2 C29 94.6(3) 1_556 1_656 ? O1 Tb2 C29 167.4(3) 2_676 1_656 ? O23 Tb2 C29 26.1(3) 1_656 1_656 ? O13 Tb2 C29 105.7(3) . 1_656 ? O18 Tb2 C29 118.8(3) 2_566 1_656 ? O22 Tb2 C29 25.9(3) 1_656 1_656 ? O12 Tb2 C29 87.6(3) . 1_656 ? O19 Tb2 C29 68.3(3) 2_566 1_656 ? O7 Tb2 C37 153.3(3) 2_676 2_566 ? O9 Tb2 C37 77.1(3) 1_556 2_566 ? O1 Tb2 C37 96.5(3) 2_676 2_566 ? O23 Tb2 C37 93.9(3) 1_656 2_566 ? O13 Tb2 C37 85.2(3) . 2_566 ? O18 Tb2 C37 25.7(3) 2_566 2_566 ? O22 Tb2 C37 93.6(3) 1_656 2_566 ? O12 Tb2 C37 141.9(3) . 2_566 ? O19 Tb2 C37 25.4(3) 2_566 2_566 ? C29 Tb2 C37 93.3(4) 1_656 2_566 ? O7 Tb2 P3 92.0(2) 2_676 . ? O9 Tb2 P3 163.9(2) 1_556 . ? O1 Tb2 P3 86.68(18) 2_676 . ? O23 Tb2 P3 119.6(2) 1_656 . ? O13 Tb2 P3 29.19(19) . . ? O18 Tb2 P3 110.1(2) 2_566 . ? O22 Tb2 P3 72.8(2) 1_656 . ? O12 Tb2 P3 29.01(18) . . ? O19 Tb2 P3 110.6(2) 2_566 . ? C29 Tb2 P3 96.7(3) 1_656 . ? C37 Tb2 P3 113.6(3) 2_566 . ? O2 Tb3 O11 74.0(3) 2_676 . ? O2 Tb3 O8 74.0(3) 2_676 . ? O11 Tb3 O8 109.1(3) . . ? O2 Tb3 O10 142.4(3) 2_676 2_675 ? O11 Tb3 O10 141.4(3) . 2_675 ? O8 Tb3 O10 80.0(3) . 2_675 ? O2 Tb3 O24 121.6(3) 2_676 . ? O11 Tb3 O24 72.5(3) . . ? O8 Tb3 O24 73.7(3) . . ? O10 Tb3 O24 74.6(3) 2_675 . ? O2 Tb3 O14 143.1(3) 2_676 2_776 ? O11 Tb3 O14 84.5(3) . 2_776 ? O8 Tb3 O14 142.4(3) . 2_776 ? O10 Tb3 O14 69.1(3) 2_675 2_776 ? O24 Tb3 O14 77.7(3) . 2_776 ? O2 Tb3 O1 78.0(3) 2_676 . ? O11 Tb3 O1 140.3(2) . . ? O8 Tb3 O1 89.2(3) . . ? O10 Tb3 O1 74.9(3) 2_675 . ? O24 Tb3 O1 147.1(3) . . ? O14 Tb3 O1 102.4(3) 2_776 . ? O2 Tb3 O3 77.4(3) 2_676 . ? O11 Tb3 O3 88.6(3) . . ? O8 Tb3 O3 140.2(3) . . ? O10 Tb3 O3 108.5(3) 2_675 . ? O24 Tb3 O3 146.0(3) . . ? O14 Tb3 O3 72.4(3) 2_776 . ? O1 Tb3 O3 57.9(2) . . ? O2 Tb3 P1 70.9(2) 2_676 . ? O11 Tb3 P1 112.93(19) . . ? O8 Tb3 P1 113.3(2) . . ? O10 Tb3 P1 95.9(2) 2_675 . ? O24 Tb3 P1 167.5(3) . . ? O14 Tb3 P1 91.4(2) 2_776 . ? O1 Tb3 P1 29.41(17) . . ? O3 Tb3 P1 29.26(17) . . ? O2 P1 O3 114.0(5) . . ? O2 P1 O1 115.7(4) . . ? O3 P1 O1 104.9(4) . . ? O2 P1 C1 106.3(5) . . ? O3 P1 C1 110.3(5) . . ? O1 P1 C1 105.4(5) . . ? O2 P1 Tb3 121.7(3) . . ? O3 P1 Tb3 53.6(3) . . ? O1 P1 Tb3 53.2(3) . . ? C1 P1 Tb3 132.0(4) . . ? O8 P2 O7 115.3(4) . . ? O8 P2 O6 118.3(5) . . ? O7 P2 O6 104.4(5) . . ? O8 P2 C8 109.7(5) . . ? O7 P2 C8 105.8(5) . . ? O6 P2 C8 102.0(5) . . ? O8 P2 Tb1 141.1(3) . . ? O7 P2 Tb1 53.4(3) . . ? O6 P2 Tb1 51.2(3) . . ? C8 P2 Tb1 109.2(4) . . ? O12 P3 O11 114.1(5) . . ? O12 P3 O13 105.5(5) . . ? O11 P3 O13 117.9(5) . . ? O12 P3 C15 105.4(5) . . ? O11 P3 C15 107.6(5) . . ? O13 P3 C15 105.4(5) . . ? O12 P3 Tb2 54.2(3) . . ? O11 P3 Tb2 138.5(4) . . ? O13 P3 Tb2 51.3(3) . . ? C15 P3 Tb2 113.9(4) . . ? P1 O1 Tb2 132.7(5) . 2_676 ? P1 O1 Tb3 97.4(4) . . ? Tb2 O1 Tb3 129.2(3) 2_676 . ? P1 O2 Tb3 167.4(5) . 2_676 ? P1 O3 Tb1 134.4(4) . 2_676 ? P1 O3 Tb3 97.2(4) . . ? Tb1 O3 Tb3 128.0(3) 2_676 . ? C7 O5 H5C 108.2 . . ? P2 O6 Tb1 99.7(4) . . ? P2 O7 Tb2 146.5(5) . 2_676 ? P2 O7 Tb1 97.5(4) . . ? Tb2 O7 Tb1 115.1(3) 2_676 . ? P2 O8 Tb3 131.3(4) . . ? C14 O9 Tb2 128.7(8) . 1_554 ? C14 O10 Tb3 134.8(8) . 2_675 ? P3 O11 Tb3 134.2(5) . . ? P3 O12 Tb1 145.9(5) . 2_676 ? P3 O12 Tb2 96.8(4) . . ? Tb1 O12 Tb2 114.6(3) 2_676 . ? P3 O13 Tb2 99.5(4) . . ? C21 O14 Tb3 133.9(8) . 2_776 ? C21 O15 Tb1 127.0(8) . 1_655 ? C30 O16 Tb1 96.8(8) . . ? C30 O17 Tb1 91.3(7) . . ? C37 O18 Tb2 95.4(8) . 2_566 ? C37 O19 Tb2 93.7(8) . 2_566 ? C22 O20 Tb1 92.0(8) . . ? C22 O21 Tb1 94.9(8) . . ? C29 O22 Tb2 91.9(8) . 1_454 ? C29 O23 Tb2 96.3(8) . 1_454 ? Tb3 O24 H24C 109.7 . . ? Tb3 O24 H24A 109.2 . . ? H24C O24 H24A 109.8 . . ? H1WA O1W H1WB 109.5 . . ? H2WB O2W H2WA 109.6 . . ? H3WA O3W H3WB 109.5 . . ? H4WA O4W H4WB 109.5 . . ? H5WA O5W H5WB 109.5 . . ? H6WA O6W H6WB 109.5 . . ? H7WA O7W H7WB 109.5 . . ? C1 N1 C2 113.5(10) . . ? C1 N1 C6 111.9(9) . . ? C2 N1 C6 108.2(10) . . ? C1 N1 H1C 107.7 . . ? C2 N1 H1C 108.0 . . ? C6 N1 H1C 107.4 . . ? C13 N2 C8 111.6(9) . . ? C13 N2 C9 110.6(9) . . ? C8 N2 C9 110.1(10) . . ? C13 N2 H2A 108.0 . . ? C8 N2 H2A 107.6 . . ? C9 N2 H2A 108.9 . . ? C20 N3 C16 109.5(9) . . ? C20 N3 C15 110.3(9) . . ? C16 N3 C15 111.8(9) . . ? C20 N3 H3C 108.2 . . ? C16 N3 H3C 108.4 . . ? C15 N3 H3C 108.4 . . ? N1 C1 P1 115.2(8) . . ? N1 C1 H1A 108.3 . . ? P1 C1 H1A 108.9 . . ? N1 C1 H1B 107.9 . . ? P1 C1 H1B 108.5 . . ? H1A C1 H1B 107.7 . . ? N1 C2 C3 111.3(11) . . ? N1 C2 H2B 109.2 . . ? C3 C2 H2B 108.8 . . ? N1 C2 H2C 109.3 . . ? C3 C2 H2C 109.9 . . ? H2B C2 H2C 108.3 . . ? C2 C3 C4 110.9(13) . . ? C2 C3 H3A 110.6 . . ? C4 C3 H3A 110.2 . . ? C2 C3 H3B 108.8 . . ? C4 C3 H3B 108.0 . . ? H3A C3 H3B 108.2 . . ? C3 C4 C5 111.2(12) . . ? C3 C4 C7 112.6(14) . . ? C5 C4 C7 108.0(13) . . ? C3 C4 H4A 108.0 . . ? C5 C4 H4A 108.2 . . ? C7 C4 H4A 108.7 . . ? C6 C5 C4 111.0(12) . . ? C6 C5 H5A 110.1 . . ? C4 C5 H5A 110.0 . . ? C6 C5 H5B 108.7 . . ? C4 C5 H5B 108.5 . . ? H5A C5 H5B 108.5 . . ? N1 C6 C5 110.5(12) . . ? N1 C6 H6A 110.2 . . ? C5 C6 H6A 111.4 . . ? N1 C6 H6B 108.3 . . ? C5 C6 H6B 108.1 . . ? H6A C6 H6B 108.2 . . ? O5 C7 O4 127.6(19) . . ? O5 C7 C4 117.0(19) . . ? O4 C7 C4 115.2(17) . . ? N2 C8 P2 113.8(8) . . ? N2 C8 H8A 108.1 . . ? P2 C8 H8A 108.6 . . ? N2 C8 H8B 108.7 . . ? P2 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? N2 C9 C10 111.1(10) . . ? N2 C9 H9A 109.4 . . ? C10 C9 H9A 109.5 . . ? N2 C9 H9B 109.1 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C9 C10 C11 112.8(10) . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10B 109.1 . . ? C11 C10 H10B 108.2 . . ? H10A C10 H10B 107.9 . . ? C10 C11 C12 111.7(10) . . ? C10 C11 C14 113.3(10) . . ? C12 C11 C14 112.8(11) . . ? C10 C11 H11A 106.1 . . ? C12 C11 H11A 105.8 . . ? C14 C11 H11A 106.5 . . ? C13 C12 C11 113.1(11) . . ? C13 C12 H12A 109.9 . . ? C11 C12 H12A 109.7 . . ? C13 C12 H12B 108.2 . . ? C11 C12 H12B 107.9 . . ? H12A C12 H12B 107.9 . . ? N2 C13 C12 112.5(9) . . ? N2 C13 H13A 109.3 . . ? C12 C13 H13A 109.9 . . ? N2 C13 H13B 108.5 . . ? C12 C13 H13B 108.5 . . ? H13A C13 H13B 108.1 . . ? O9 C14 O10 126.8(11) . . ? O9 C14 C11 116.5(11) . . ? O10 C14 C11 116.7(11) . . ? N3 C15 P3 113.2(8) . . ? N3 C15 H15A 108.2 . . ? P3 C15 H15A 109.0 . . ? N3 C15 H15B 109.2 . . ? P3 C15 H15B 109.1 . . ? H15A C15 H15B 108.0 . . ? N3 C16 C17 112.6(10) . . ? N3 C16 H16A 107.9 . . ? C17 C16 H16A 108.4 . . ? N3 C16 H16B 109.7 . . ? C17 C16 H16B 110.1 . . ? H16A C16 H16B 108.0 . . ? C16 C17 C18 110.7(10) . . ? C16 C17 H17A 110.1 . . ? C18 C17 H17A 110.0 . . ? C16 C17 H17B 109.0 . . ? C18 C17 H17B 108.6 . . ? H17A C17 H17B 108.3 . . ? C19 C18 C17 110.6(10) . . ? C19 C18 C21 112.4(10) . . ? C17 C18 C21 111.7(10) . . ? C19 C18 H18A 107.4 . . ? C17 C18 H18A 106.8 . . ? C21 C18 H18A 107.6 . . ? C18 C19 C20 111.4(10) . . ? C18 C19 H19A 109.5 . . ? C20 C19 H19A 110.0 . . ? C18 C19 H19B 108.8 . . ? C20 C19 H19B 108.9 . . ? H19A C19 H19B 108.1 . . ? N3 C20 C19 111.6(10) . . ? N3 C20 H20A 109.7 . . ? C19 C20 H20A 110.1 . . ? N3 C20 H20B 108.0 . . ? C19 C20 H20B 109.1 . . ? H20A C20 H20B 108.2 . . ? O15 C21 O14 125.8(12) . . ? O15 C21 C18 117.7(11) . . ? O14 C21 C18 116.5(11) . . ? O21 C22 O20 119.6(12) . . ? O21 C22 C23 120.1(12) . . ? O20 C22 C23 120.3(12) . . ? O21 C22 Tb1 58.8(6) . . ? O20 C22 Tb1 61.4(7) . . ? C23 C22 Tb1 173.1(10) . . ? C28 C23 C24 119.0(13) . . ? C28 C23 C22 120.7(12) . . ? C24 C23 C22 119.9(12) . . ? C23 C24 C25 121.2(13) . . ? C23 C24 H24B 119.1 . . ? C25 C24 H24B 119.7 . . ? C26 C25 C24 117.9(12) . . ? C26 C25 H25A 120.8 . . ? C24 C25 H25A 121.3 . . ? C27 C26 C25 121.4(12) . . ? C27 C26 C29 119.0(12) . . ? C25 C26 C29 119.5(12) . . ? C26 C27 C28 120.4(13) . . ? C26 C27 H27A 119.8 . . ? C28 C27 H27A 119.8 . . ? C23 C28 C27 119.8(13) . . ? C23 C28 H28A 119.7 . . ? C27 C28 H28A 120.5 . . ? O22 C29 O23 119.7(12) . . ? O22 C29 C26 121.5(12) . . ? O23 C29 C26 118.8(11) . . ? O22 C29 Tb2 62.1(7) . 1_454 ? O23 C29 Tb2 57.7(6) . 1_454 ? C26 C29 Tb2 175.6(9) . 1_454 ? O17 C30 O16 120.5(11) . . ? O17 C30 C31 120.4(11) . . ? O16 C30 C31 119.1(11) . . ? O17 C30 Tb1 63.1(7) . . ? O16 C30 Tb1 57.8(6) . . ? C31 C30 Tb1 170.5(9) . . ? C32 C31 C36 120.4(12) . . ? C32 C31 C30 118.9(12) . . ? C36 C31 C30 120.7(12) . . ? C31 C32 C33 120.3(12) . . ? C31 C32 H32A 119.6 . . ? C33 C32 H32A 120.1 . . ? C34 C33 C32 118.9(13) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 121.0 . . ? C35 C34 C33 120.2(12) . . ? C35 C34 C37 120.2(12) . . ? C33 C34 C37 119.4(12) . . ? C34 C35 C36 119.4(13) . . ? C34 C35 H35A 120.1 . . ? C36 C35 H35A 120.5 . . ? C31 C36 C35 120.6(13) . . ? C31 C36 H36A 119.3 . . ? C35 C36 H36A 120.1 . . ? O19 C37 O18 119.7(12) . . ? O19 C37 C34 120.6(12) . . ? O18 C37 C34 119.7(12) . . ? O19 C37 Tb2 60.9(7) . 2_566 ? O18 C37 Tb2 58.9(7) . 2_566 ? C34 C37 Tb2 176.0(10) . 2_566 ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 2.697 _refine_diff_density_min -1.641 _refine_diff_density_rms 0.314