# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1097 data_EUTPIP _audit_creation_date 97-10-10 _audit_creation_method CRYSTALS # eutpip in P-3 _computing_data_collection DIF4 _computing_cell_refinement DIF4 _computing_data_reduction REDU4 _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution DIRDIF #========================================================================== # NOW THE GOODIES TO BE ENTERED BY HAND #========================================================================== _chemical_melting_point ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device ; Stoe Stadi-4 diffractometer equipped with an Oxford Cryosystems l.t. device. ; _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary Patterson _atom_sites_solution_hydrogens 'Geometric (Full-weight only)' _refine_ls_hydrogen_treatment 'Placed geometrically after each cycle' #**************************************************************************** _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 23.418(2) _cell_angle_alpha 90 _cell_length_b 23.418(2) _cell_angle_beta 90 _cell_length_c 21.185(3) _cell_angle_gamma 120 _cell_volume 10061.4(19) _symmetry_cell_setting 'Trigonal ' _symmetry_space_group_name_H-M 'P -3 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-y,x-y,z' 'y,-x+y,-z' '-x+y,-x,z' 'x-y,x,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Eu ' -0.5420 3.6690 24.6274 2.3879 19.0886 0.1942 13.7603 13.7546 2.9227 123.1740 2.5745 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C72 H61.33 Eu1 N3 P6 O6.67 ' _chemical_formula_moiety '[Eu(Ph2P(O)NP(O)Ph2)3].0.67H2O ' _chemical_compound_source ; ? ; _chemical_formula_weight 1411.75 _cell_measurement_reflns_used 77 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _cell_measurement_temperature 220 _cell_formula_units_Z 6.00 _exptl_crystal_description block _exptl_crystal_colour Colourless _exptl_crystal_size_min 0.39 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_max 0.56 _exptl_crystal_density_diffrn 1.40 _exptl_crystal_density_meas ? _exptl_crystal_F_000 4316.65 _exptl_absorpt_coefficient_mu 1.13 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_T_max 0.907 _diffrn_standards_interval_time 60 _diffrn_standards_interval_count ? _diffrn_standards_number 3 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 220 _diffrn_reflns_number 17969 _reflns_number_total 11861 _diffrn_reflns_av_R_equivalents 0.02 _reflns_number_observed 8591 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -27 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 27 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _reflns_observed_criterion >2.00\s(I) _refine_diff_density_min -2.24 _refine_diff_density_max 1.73 _refine_ls_number_reflns 8591 _refine_ls_number_parameters 800 _refine_ls_R_factor_obs 0.0426 _refine_ls_wR_factor_obs 0.0418 _refine_ls_goodness_of_fit_obs 1.1338 _refine_ls_shift/esd_max 0.012633 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method 'Omega-theta with learnt-profile (Clegg)' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type EU1 0.6667 0.3333 0.06666(2) 0.0241 1.0000 Uani EU2 0.6667 0.3333 -0.42662(2) 0.0224 1.0000 Uani EU3 0.0000 0.0000 0.28557(2) 0.0331 1.0000 Uani N1 0.4837(2) 0.1965(2) 0.0611(2) 0.0355 1.0000 Uani N2 0.4768(2) 0.2370(2) -0.4356(2) 0.0312 1.0000 Uani N3 0.1394(2) -0.0462(2) 0.2835(2) 0.0475 1.0000 Uani P11 0.50950(6) 0.24093(6) -0.00078(6) 0.0324 1.0000 Uani P12 0.50963(5) 0.22715(5) 0.12917(5) 0.0272 1.0000 Uani P21 0.50583(5) 0.24215(5) -0.36664(5) 0.0257 1.0000 Uani P22 0.51326(5) 0.22933(6) -0.49592(5) 0.0274 1.0000 Uani P31 0.10159(6) -0.05597(6) 0.21890(7) 0.0397 1.0000 Uani P32 0.14531(6) 0.00299(6) 0.33794(7) 0.0393 1.0000 Uani O11 0.5769(1) 0.3025(2) 0.0038(1) 0.0354 1.0000 Uani O12 0.5839(1) 0.2685(1) 0.1368(1) 0.0293 1.0000 Uani O21 0.5782(1) 0.2924(1) -0.3577(1) 0.0286 1.0000 Uani O22 0.5865(1) 0.2536(1) -0.4887(1) 0.0302 1.0000 Uani O31 0.0389(2) -0.0520(2) 0.2198(2) 0.0401 1.0000 Uani O32 0.0872(2) 0.0143(2) 0.3451(2) 0.0415 1.0000 Uani C111 0.5119(3) 0.1880(3) -0.0612(2) 0.0432 1.0000 Uani C112 0.5490(4) 0.2164(3) -0.1148(3) 0.0648 1.0000 Uani C113 0.5556(4) 0.1762(5) -0.1604(3) 0.0882 1.0000 Uani C114 0.5252(4) 0.1095(5) -0.1496(4) 0.0839 1.0000 Uani C115 0.4889(4) 0.0812(4) -0.0967(4) 0.0749 1.0000 Uani C116 0.4824(3) 0.1208(3) -0.0520(3) 0.0575 1.0000 Uani C121 0.4518(2) 0.2671(2) -0.0238(2) 0.0346 1.0000 Uani C122 0.3866(2) 0.2211(3) -0.0373(3) 0.0459 1.0000 Uani C123 0.3421(3) 0.2421(3) -0.0508(3) 0.0599 1.0000 Uani C124 0.3618(3) 0.3076(4) -0.0515(3) 0.0639 1.0000 Uani C125 0.4264(3) 0.3531(3) -0.0394(3) 0.0698 1.0000 Uani C126 0.4716(3) 0.3329(3) -0.0258(3) 0.0555 1.0000 Uani C131 0.4791(2) 0.1589(2) 0.1835(2) 0.0329 1.0000 Uani C132 0.4503(3) 0.0947(2) 0.1620(3) 0.0467 1.0000 Uani C133 0.4314(3) 0.0435(3) 0.2043(3) 0.0607 1.0000 Uani C134 0.4416(3) 0.0564(3) 0.2677(3) 0.0587 1.0000 Uani C135 0.4714(3) 0.1198(3) 0.2889(3) 0.0598 1.0000 Uani C136 0.4909(3) 0.1714(3) 0.2471(2) 0.0496 1.0000 Uani C141 0.4752(2) 0.2776(2) 0.1526(2) 0.0312 1.0000 Uani C142 0.5149(2) 0.3434(2) 0.1662(2) 0.0402 1.0000 Uani C143 0.4868(3) 0.3824(3) 0.1781(3) 0.0514 1.0000 Uani C144 0.4205(3) 0.3560(3) 0.1770(3) 0.0583 1.0000 Uani C145 0.3809(3) 0.2908(3) 0.1639(3) 0.0660 1.0000 Uani C146 0.4078(3) 0.2517(3) 0.1513(3) 0.0535 1.0000 Uani C211 0.4574(2) 0.2604(2) -0.3133(2) 0.0300 1.0000 Uani C212 0.4744(3) 0.2695(3) -0.2500(2) 0.0443 1.0000 Uani C213 0.4375(3) 0.2824(3) -0.2072(2) 0.0542 1.0000 Uani C214 0.3832(3) 0.2848(3) -0.2279(3) 0.0510 1.0000 Uani C215 0.3671(3) 0.2774(3) -0.2905(3) 0.0528 1.0000 Uani C216 0.4041(2) 0.2655(2) -0.3336(2) 0.0405 1.0000 Uani C221 0.4941(2) 0.1630(2) -0.3420(2) 0.0306 1.0000 Uani C222 0.5480(2) 0.1537(2) -0.3350(2) 0.0358 1.0000 Uani C223 0.5386(3) 0.0922(3) -0.3205(3) 0.0476 1.0000 Uani C224 0.4761(3) 0.0392(2) -0.3131(3) 0.0512 1.0000 Uani C225 0.4228(3) 0.0483(2) -0.3197(3) 0.0515 1.0000 Uani C226 0.4312(2) 0.1092(2) -0.3347(3) 0.0429 1.0000 Uani C231 0.5030(2) 0.2753(2) -0.5584(2) 0.0313 1.0000 Uani C232 0.4590(3) 0.2984(3) -0.5522(2) 0.0430 1.0000 Uani C233 0.4552(3) 0.3374(3) -0.5994(3) 0.0555 1.0000 Uani C234 0.4949(3) 0.3535(3) -0.6519(3) 0.0539 1.0000 Uani C235 0.5384(3) 0.3309(3) -0.6580(2) 0.0542 1.0000 Uani C236 0.5430(3) 0.2919(3) -0.6114(2) 0.0462 1.0000 Uani C241 0.4738(2) 0.1440(2) -0.5200(2) 0.0318 1.0000 Uani C242 0.4060(3) 0.1059(3) -0.5228(3) 0.0511 1.0000 Uani C243 0.3764(3) 0.0395(3) -0.5403(3) 0.0633 1.0000 Uani C244 0.4140(3) 0.0118(3) -0.5541(3) 0.0552 1.0000 Uani C245 0.4812(3) 0.0494(3) -0.5520(3) 0.0518 1.0000 Uani C246 0.5114(2) 0.1155(2) -0.5351(2) 0.0392 1.0000 Uani C311 0.1567(3) 0.0028(2) 0.1613(3) 0.0529 1.0000 Uani C312 0.2244(3) 0.0282(3) 0.1654(4) 0.0714 1.0000 Uani C313 0.2659(4) 0.0708(4) 0.1195(6) 0.1126 1.0000 Uani C314 0.2399(7) 0.0866(4) 0.0705(6) 0.1202 1.0000 Uani C315 0.1742(7) 0.0629(5) 0.0642(5) 0.1190 1.0000 Uani C316 0.1318(4) 0.0196(4) 0.1110(4) 0.0817 1.0000 Uani C321 0.0838(2) -0.1342(2) 0.1862(3) 0.0410 1.0000 Uani C322 0.0434(3) -0.1581(3) 0.1338(3) 0.0617 1.0000 Uani C323 0.0331(4) -0.2150(3) 0.1042(3) 0.0746 1.0000 Uani C324 0.0626(3) -0.2485(3) 0.1263(4) 0.0697 1.0000 Uani C325 0.1016(3) -0.2266(3) 0.1784(4) 0.0729 1.0000 Uani C326 0.1129(3) -0.1688(3) 0.2085(3) 0.0613 1.0000 Uani C331 0.2177(2) 0.0829(2) 0.3265(2) 0.0388 1.0000 Uani C332 0.2111(3) 0.1337(3) 0.3027(3) 0.0653 1.0000 Uani C333 0.2666(4) 0.1949(3) 0.2904(4) 0.0930 1.0000 Uani C334 0.3277(3) 0.2049(3) 0.3035(3) 0.0700 1.0000 Uani C335 0.3348(3) 0.1557(4) 0.3277(3) 0.0677 1.0000 Uani C336 0.2805(3) 0.0943(3) 0.3392(3) 0.0590 1.0000 Uani C341 0.1606(2) -0.0278(3) 0.4108(3) 0.0504 1.0000 Uani C342 0.1681(3) 0.0062(3) 0.4670(4) 0.0709 1.0000 Uani C343 0.1819(4) -0.0155(4) 0.5227(3) 0.0800 1.0000 Uani C344 0.1881(3) -0.0701(4) 0.5230(4) 0.0793 1.0000 Uani C345 0.1798(4) -0.1044(4) 0.4695(4) 0.0757 1.0000 Uani C346 0.1663(3) -0.0832(3) 0.4122(3) 0.0635 1.0000 Uani O1 0.6667 0.3333 0.2546(4) 0.1055 1.0000 Uani O2 0.3333 0.6667 0.2372(5) 0.1349 1.0000 Uani H1121 0.5713 0.2653 -0.1211 0.0656 1.0000 Uiso H1131 0.5816 0.1959 -0.2000 0.0851 1.0000 Uiso H1141 0.5302 0.0812 -0.1820 0.0906 1.0000 Uiso H1151 0.4677 0.0327 -0.0903 0.0764 1.0000 Uiso H1161 0.4567 0.1006 -0.0125 0.0550 1.0000 Uiso H1221 0.3718 0.1730 -0.0376 0.0430 1.0000 Uiso H1231 0.2949 0.2091 -0.0600 0.0551 1.0000 Uiso H1241 0.3297 0.3230 -0.0607 0.0702 1.0000 Uiso H1251 0.4412 0.4014 -0.0403 0.0734 1.0000 Uiso H1261 0.5186 0.3666 -0.0178 0.0548 1.0000 Uiso H1321 0.4427 0.0853 0.1154 0.0396 1.0000 Uiso H1331 0.4102 -0.0030 0.1887 0.0547 1.0000 Uiso H1341 0.4269 0.0188 0.2982 0.0602 1.0000 Uiso H1351 0.4792 0.1290 0.3353 0.0606 1.0000 Uiso H1361 0.5133 0.2177 0.2630 0.0482 1.0000 Uiso H1421 0.5638 0.3631 0.1678 0.0388 1.0000 Uiso H1431 0.5157 0.4302 0.1876 0.0524 1.0000 Uiso H1441 0.4010 0.3847 0.1852 0.0649 1.0000 Uiso H1451 0.3320 0.2713 0.1642 0.0690 1.0000 Uiso H1461 0.3782 0.2042 0.1405 0.0500 1.0000 Uiso H2121 0.5137 0.2672 -0.2351 0.0454 1.0000 Uiso H2131 0.4499 0.2890 -0.1616 0.0518 1.0000 Uiso H2141 0.3556 0.2927 -0.1967 0.0506 1.0000 Uiso H2151 0.3278 0.2801 -0.3051 0.0546 1.0000 Uiso H2161 0.3924 0.2605 -0.3795 0.0387 1.0000 Uiso H2221 0.5935 0.1918 -0.3403 0.0358 1.0000 Uiso H2231 0.5778 0.0862 -0.3155 0.0479 1.0000 Uiso H2241 0.4696 -0.0053 -0.3030 0.0496 1.0000 Uiso H2251 0.3772 0.0102 -0.3137 0.0440 1.0000 Uiso H2261 0.3917 0.1148 -0.3403 0.0398 1.0000 Uiso H2321 0.4308 0.2874 -0.5137 0.0430 1.0000 Uiso H2331 0.4234 0.3539 -0.5956 0.0617 1.0000 Uiso H2341 0.4921 0.3819 -0.6856 0.0513 1.0000 Uiso H2351 0.5670 0.3425 -0.6965 0.0485 1.0000 Uiso H2361 0.5752 0.2759 -0.6160 0.0466 1.0000 Uiso H2421 0.3778 0.1258 -0.5128 0.0476 1.0000 Uiso H2431 0.3273 0.0118 -0.5419 0.0532 1.0000 Uiso H2441 0.3929 -0.0358 -0.5657 0.0475 1.0000 Uiso H2451 0.5088 0.0291 -0.5625 0.0528 1.0000 Uiso H2461 0.5607 0.1426 -0.5340 0.0403 1.0000 Uiso H3121 0.2430 0.0157 0.2015 0.0604 1.0000 Uiso H3131 0.3149 0.0898 0.1225 0.0851 1.0000 Uiso H3141 0.2697 0.1175 0.0378 0.1082 1.0000 Uiso H3151 0.1556 0.0752 0.0273 0.1220 1.0000 Uiso H3161 0.0828 0.0008 0.1074 0.0791 1.0000 Uiso H3221 0.0210 -0.1341 0.1175 0.0636 1.0000 Uiso H3231 0.0039 -0.2318 0.0660 0.0704 1.0000 Uiso H3241 0.0551 -0.2895 0.1045 0.0607 1.0000 Uiso H3251 0.1229 -0.2516 0.1954 0.0646 1.0000 Uiso H3261 0.1420 -0.1524 0.2463 0.0565 1.0000 Uiso H3321 0.1661 0.1268 0.2943 0.0572 1.0000 Uiso H3331 0.2611 0.2312 0.2721 0.0776 1.0000 Uiso H3341 0.3676 0.2491 0.2954 0.0568 1.0000 Uiso H3351 0.3799 0.1635 0.3375 0.0596 1.0000 Uiso H3361 0.2869 0.0583 0.3566 0.0564 1.0000 Uiso H3421 0.1630 0.0461 0.4676 0.0663 1.0000 Uiso H3431 0.1885 0.0096 0.5628 0.0766 1.0000 Uiso H3441 0.1988 -0.0853 0.5632 0.0765 1.0000 Uiso H3451 0.1826 -0.1457 0.4704 0.0812 1.0000 Uiso H3461 0.1608 -0.1087 0.3723 0.0673 1.0000 Uiso 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 EU1 0.0249(1) 0.0249(1) 0.0224(2) 0.0000 0.0000 0.01243(6) EU2 0.0217(1) 0.0217(1) 0.0239(2) 0.0000 0.0000 0.01083(6) EU3 0.0217(1) 0.0217(1) 0.0560(3) 0.0000 0.0000 0.01086(7) N1 0.037(2) 0.032(2) 0.032(2) -0.001(2) -0.002(2) 0.013(2) N2 0.031(2) 0.040(2) 0.026(2) 0.000(2) -0.003(2) 0.020(2) N3 0.032(2) 0.042(2) 0.075(3) -0.013(2) -0.014(2) 0.024(2) P11 0.0325(6) 0.0389(7) 0.0245(6) -0.0025(5) -0.0054(5) 0.0169(5) P12 0.0285(6) 0.0275(6) 0.0234(6) 0.0026(5) -0.0010(5) 0.0124(5) P21 0.0252(5) 0.0269(6) 0.0240(6) -0.0011(4) 0.0015(4) 0.0123(5) P22 0.0277(6) 0.0297(6) 0.0246(6) -0.0031(5) -0.0029(5) 0.0143(5) P31 0.0320(6) 0.0297(6) 0.0602(9) -0.0009(6) 0.0039(6) 0.0174(5) P32 0.0302(6) 0.0345(7) 0.0562(8) 0.0040(6) -0.0024(6) 0.0185(6) O11 0.034(2) 0.043(2) 0.025(2) 0.002(1) -0.003(1) 0.017(1) O12 0.027(2) 0.033(2) 0.025(2) 0.004(1) -0.001(1) 0.012(1) O21 0.028(2) 0.028(2) 0.027(2) 0.000(1) 0.004(1) 0.012(1) O22 0.030(2) 0.034(2) 0.027(2) -0.004(1) -0.002(1) 0.017(1) O31 0.036(2) 0.036(2) 0.052(2) -0.002(2) -0.004(2) 0.021(2) O32 0.034(2) 0.041(2) 0.054(2) 0.005(2) 0.001(2) 0.022(2) C111 0.043(3) 0.066(4) 0.028(3) -0.007(2) -0.013(2) 0.033(3) C112 0.090(5) 0.084(5) 0.036(3) -0.006(3) 0.002(3) 0.055(4) C113 0.114(7) 0.136(8) 0.041(4) -0.012(4) 0.001(4) 0.083(6) C114 0.102(6) 0.112(7) 0.065(5) -0.044(5) -0.027(4) 0.075(6) C115 0.086(5) 0.075(5) 0.072(5) -0.038(4) -0.026(4) 0.047(4) C116 0.054(3) 0.055(4) 0.060(4) -0.023(3) -0.015(3) 0.024(3) C121 0.036(3) 0.045(3) 0.022(2) 0.000(2) -0.003(2) 0.020(2) C122 0.034(3) 0.053(3) 0.045(3) 0.006(2) -0.003(2) 0.017(2) C123 0.034(3) 0.083(5) 0.058(4) 0.013(3) -0.001(3) 0.025(3) C124 0.059(4) 0.089(5) 0.062(4) 0.003(4) -0.004(3) 0.051(4) C125 0.073(4) 0.059(4) 0.089(5) -0.003(3) -0.018(4) 0.042(4) C126 0.051(3) 0.052(3) 0.065(4) -0.002(3) -0.016(3) 0.027(3) C131 0.025(2) 0.031(2) 0.040(3) 0.010(2) 0.004(2) 0.012(2) C132 0.047(3) 0.026(3) 0.051(3) 0.003(2) 0.003(3) 0.007(2) C133 0.055(4) 0.035(3) 0.080(5) 0.007(3) 0.006(3) 0.013(3) C134 0.055(4) 0.049(3) 0.077(4) 0.032(3) 0.017(3) 0.030(3) C135 0.079(4) 0.069(4) 0.039(3) 0.023(3) 0.010(3) 0.043(4) C136 0.076(4) 0.042(3) 0.032(3) 0.006(2) 0.001(3) 0.031(3) C141 0.034(2) 0.034(2) 0.026(2) 0.008(2) -0.003(2) 0.017(2) C142 0.035(3) 0.038(3) 0.042(3) -0.003(2) 0.003(2) 0.015(2) C143 0.069(4) 0.042(3) 0.050(3) -0.001(2) 0.009(3) 0.033(3) C144 0.083(5) 0.072(4) 0.049(3) 0.013(3) 0.015(3) 0.061(4) C145 0.045(3) 0.069(4) 0.098(5) 0.012(4) 0.005(3) 0.039(3) C146 0.036(3) 0.041(3) 0.084(4) 0.002(3) -0.004(3) 0.020(2) C211 0.030(2) 0.025(2) 0.030(2) 0.001(2) 0.005(2) 0.010(2) C212 0.046(3) 0.059(3) 0.034(3) -0.003(2) -0.001(2) 0.031(3) C213 0.071(4) 0.066(4) 0.031(3) -0.007(3) 0.010(3) 0.038(3) C214 0.048(3) 0.049(3) 0.055(3) -0.004(3) 0.024(3) 0.024(3) C215 0.040(3) 0.062(4) 0.064(4) -0.007(3) 0.006(3) 0.031(3) C216 0.029(2) 0.047(3) 0.043(3) -0.009(2) -0.001(2) 0.018(2) C221 0.036(2) 0.027(2) 0.027(2) -0.001(2) 0.003(2) 0.015(2) C222 0.035(3) 0.031(2) 0.041(3) 0.003(2) 0.004(2) 0.017(2) C223 0.054(3) 0.037(3) 0.059(4) 0.006(2) 0.006(3) 0.028(3) C224 0.062(4) 0.029(3) 0.061(4) 0.001(2) 0.003(3) 0.022(3) C225 0.046(3) 0.031(3) 0.062(4) 0.001(2) 0.000(3) 0.008(2) C226 0.038(3) 0.031(3) 0.053(3) 0.003(2) 0.001(2) 0.012(2) C231 0.036(2) 0.029(2) 0.024(2) -0.002(2) -0.005(2) 0.013(2) C232 0.047(3) 0.047(3) 0.039(3) -0.000(2) -0.008(2) 0.026(3) C233 0.063(4) 0.063(4) 0.056(4) 0.004(3) -0.010(3) 0.043(3) C234 0.082(4) 0.047(3) 0.038(3) 0.010(2) -0.006(3) 0.037(3) C235 0.080(4) 0.048(3) 0.028(3) 0.008(2) 0.005(3) 0.028(3) C236 0.058(3) 0.051(3) 0.033(3) 0.004(2) 0.001(2) 0.030(3) C241 0.037(2) 0.031(2) 0.025(2) -0.000(2) -0.001(2) 0.015(2) C242 0.035(3) 0.041(3) 0.072(4) -0.014(3) -0.005(3) 0.015(2) C243 0.042(3) 0.049(3) 0.076(4) -0.014(3) -0.003(3) 0.005(3) C244 0.071(4) 0.032(3) 0.046(3) -0.004(2) 0.002(3) 0.013(3) C245 0.068(4) 0.039(3) 0.054(3) -0.004(3) -0.002(3) 0.031(3) C246 0.042(3) 0.040(3) 0.038(3) -0.003(2) -0.006(2) 0.022(2) C311 0.063(4) 0.030(3) 0.069(4) -0.000(3) 0.017(3) 0.026(3) C312 0.047(4) 0.040(3) 0.117(6) -0.014(3) 0.026(4) 0.014(3) C313 0.080(6) 0.043(4) 0.19(1) -0.013(6) 0.065(7) 0.013(4) C314 0.16(1) 0.059(5) 0.14(1) 0.029(6) 0.096(9) 0.047(6) C315 0.17(1) 0.093(7) 0.108(7) 0.037(6) 0.052(8) 0.074(7) C316 0.094(6) 0.065(4) 0.083(5) 0.022(4) 0.026(4) 0.037(4) C321 0.032(3) 0.028(2) 0.062(3) -0.001(2) 0.007(2) 0.015(2) C322 0.083(5) 0.047(3) 0.065(4) -0.002(3) -0.004(3) 0.040(3) C323 0.108(6) 0.048(4) 0.066(4) -0.008(3) 0.001(4) 0.037(4) C324 0.060(4) 0.033(3) 0.107(6) -0.014(3) 0.034(4) 0.017(3) C325 0.048(4) 0.040(3) 0.139(7) -0.005(4) 0.006(4) 0.029(3) C326 0.044(3) 0.040(3) 0.104(5) -0.007(3) -0.006(3) 0.024(3) C331 0.032(3) 0.043(3) 0.036(3) -0.003(2) -0.000(2) 0.014(2) C332 0.044(3) 0.047(3) 0.090(5) 0.015(3) -0.017(3) 0.012(3) C333 0.072(5) 0.054(4) 0.125(7) 0.033(4) -0.023(5) 0.011(4) C334 0.042(3) 0.065(4) 0.063(4) 0.016(3) -0.003(3) -0.003(3) C335 0.038(3) 0.085(5) 0.064(4) -0.006(4) -0.002(3) 0.018(3) C336 0.038(3) 0.059(4) 0.078(4) -0.002(3) 0.004(3) 0.024(3) C341 0.035(3) 0.046(3) 0.076(4) 0.026(3) 0.007(3) 0.024(2) C342 0.079(5) 0.050(4) 0.076(5) 0.008(3) -0.015(4) 0.027(3) C343 0.089(5) 0.074(5) 0.066(5) 0.017(4) -0.011(4) 0.033(4) C344 0.056(4) 0.095(6) 0.082(5) 0.045(5) 0.015(4) 0.034(4) C345 0.078(5) 0.075(5) 0.092(6) 0.044(4) 0.019(4) 0.052(4) C346 0.060(4) 0.067(4) 0.077(4) 0.025(3) 0.028(3) 0.042(3) O1 0.134(5) 0.134(5) 0.049(5) 0.0000 0.0000 0.067(3) O2 0.173(7) 0.173(7) 0.059(6) 0.0000 0.0000 0.086(4) _refine_ls_extinction_coef 33.8(242) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag EU1 . O11 . 2.280(3) yes EU1 . O11 3_655 2.280(3) yes EU1 . O11 5_665 2.280(3) yes EU1 . O12 . 2.308(3) yes EU1 . O12 3_655 2.308(3) yes EU1 . O12 5_665 2.308(3) yes EU2 . O21 . 2.315(3) yes EU2 . O21 3_655 2.315(3) yes EU2 . O21 5_665 2.315(3) yes EU2 . O22 . 2.289(3) yes EU2 . O22 3_655 2.289(3) yes EU2 . O22 5_665 2.289(3) yes EU3 . O31 . 2.317(3) yes EU3 . O31 3_555 2.317(3) yes EU3 . O31 5_555 2.317(3) yes EU3 . O32 . 2.278(3) yes EU3 . O32 3_555 2.278(3) yes EU3 . O32 5_555 2.278(3) yes N1 . P11 . 1.593(4) yes N1 . P12 . 1.590(4) yes N2 . P21 . 1.590(4) yes N2 . P22 . 1.597(4) yes N3 . P31 . 1.584(5) yes N3 . P32 . 1.586(5) yes P11 . O11 . 1.518(3) yes P11 . C111 . 1.802(5) yes P11 . C121 . 1.808(5) yes P12 . O12 . 1.519(3) yes P12 . C131 . 1.802(4) yes P12 . C141 . 1.801(5) yes P21 . O21 . 1.516(3) yes P21 . C211 . 1.797(4) yes P21 . C221 . 1.810(4) yes P22 . O22 . 1.520(3) yes P22 . C231 . 1.796(4) yes P22 . C241 . 1.805(5) yes P31 . O31 . 1.516(3) yes P31 . C311 . 1.808(6) yes P31 . C321 . 1.802(5) yes P32 . O32 . 1.518(3) yes P32 . C331 . 1.806(5) yes P32 . C341 . 1.813(6) yes C111 . C112 . 1.382(8) yes C111 . C116 . 1.380(8) yes C112 . C113 . 1.409(9) yes C112 . H1121 . 1.004(7) no C113 . C114 . 1.37(1) yes C113 . H1131 . 1.004(8) no C114 . C115 . 1.36(1) yes C114 . H1141 . 1.003(7) no C115 . C116 . 1.386(8) yes C115 . H1151 . 0.996(8) no C116 . H1161 . 1.001(7) no C121 . C122 . 1.388(7) yes C121 . C126 . 1.370(7) yes C122 . C123 . 1.386(8) yes C122 . H1221 . 1.000(5) no C123 . C124 . 1.363(9) yes C123 . H1231 . 1.001(6) no C124 . C125 . 1.371(9) yes C124 . H1241 . 1.002(6) no C125 . C126 . 1.390(8) yes C125 . H1251 . 1.002(6) no C126 . H1261 . 0.997(6) no C131 . C132 . 1.382(7) yes C131 . C136 . 1.378(7) yes C132 . C133 . 1.380(8) yes C132 . H1321 . 1.006(5) no C133 . C134 . 1.370(9) yes C133 . H1331 . 1.002(6) no C134 . C135 . 1.364(9) yes C134 . H1341 . 1.004(5) no C135 . C136 . 1.380(7) yes C135 . H1351 . 1.003(6) no C136 . H1361 . 0.998(5) no C141 . C142 . 1.375(6) yes C141 . C146 . 1.381(7) yes C142 . C143 . 1.388(7) yes C142 . H1421 . 0.999(5) no C143 . C144 . 1.353(8) yes C143 . H1431 . 0.998(5) no C144 . C145 . 1.362(9) yes C144 . H1441 . 0.999(5) no C145 . C146 . 1.370(8) yes C145 . H1451 . 1.000(6) no C146 . H1461 . 1.000(5) no C211 . C212 . 1.384(6) yes C211 . C216 . 1.380(6) yes C212 . C213 . 1.386(7) yes C212 . H2121 . 1.001(5) no C213 . C214 . 1.373(8) yes C213 . H2131 . 0.998(5) no C214 . C215 . 1.366(8) yes C214 . H2141 . 1.003(5) no C215 . C216 . 1.380(7) yes C215 . H2151 . 1.003(5) no C216 . H2161 . 1.002(5) no C221 . C222 . 1.392(6) yes C221 . C226 . 1.387(6) yes C222 . C223 . 1.378(7) yes C222 . H2221 . 0.997(5) no C223 . C224 . 1.375(8) yes C223 . H2231 . 1.002(5) no C224 . C225 . 1.375(8) yes C224 . H2241 . 0.999(5) no C225 . C226 . 1.376(7) yes C225 . H2251 . 1.001(5) no C226 . H2261 . 1.004(5) no C231 . C232 . 1.388(7) yes C231 . C236 . 1.388(7) yes C232 . C233 . 1.387(7) yes C232 . H2321 . 0.999(5) no C233 . C234 . 1.375(8) yes C233 . H2331 . 1.000(6) no C234 . C235 . 1.369(8) yes C234 . H2341 . 1.000(5) no C235 . C236 . 1.386(7) yes C235 . H2351 . 1.002(6) no C236 . H2361 . 1.001(5) no C241 . C242 . 1.380(7) yes C241 . C246 . 1.383(7) yes C242 . C243 . 1.401(8) yes C242 . H2421 . 1.001(5) no C243 . C244 . 1.361(9) yes C243 . H2431 . 0.999(6) no C244 . C245 . 1.366(8) yes C244 . H2441 . 1.000(5) no C245 . C246 . 1.389(7) yes C245 . H2451 . 1.001(6) no C246 . H2461 . 1.002(5) no C311 . C312 . 1.392(8) yes C311 . C316 . 1.36(1) yes C312 . C313 . 1.38(1) yes C312 . H3121 . 0.993(8) no C313 . C314 . 1.34(2) yes C313 . H3131 . 1.00(1) no C314 . C315 . 1.36(2) yes C314 . H3141 . 0.993(9) no C315 . C316 . 1.41(1) yes C315 . H3151 . 1.01(1) no C316 . H3161 . 1.007(8) no C321 . C322 . 1.382(8) yes C321 . C326 . 1.378(7) yes C322 . C323 . 1.380(8) yes C322 . H3221 . 1.002(6) no C323 . C324 . 1.36(1) yes C323 . H3231 . 1.004(7) no C324 . C325 . 1.36(1) yes C324 . H3241 . 0.999(6) no C325 . C326 . 1.396(8) yes C325 . H3251 . 1.005(6) no C326 . H3261 . 0.996(7) no C331 . C332 . 1.372(8) yes C331 . C336 . 1.383(7) yes C332 . C333 . 1.395(9) yes C332 . H3321 . 1.000(6) no C333 . C334 . 1.36(1) yes C333 . H3331 . 0.999(7) no C334 . C335 . 1.34(1) yes C334 . H3341 . 1.003(6) no C335 . C336 . 1.385(9) yes C335 . H3351 . 1.000(6) no C336 . H3361 . 0.999(6) no C341 . C342 . 1.395(9) yes C341 . C346 . 1.370(8) yes C342 . C343 . 1.386(9) yes C342 . H3421 . 1.000(7) no C343 . C344 . 1.36(1) yes C343 . H3431 . 0.999(8) no C344 . C345 . 1.35(1) yes C344 . H3441 . 1.001(7) no C345 . C346 . 1.407(9) yes C345 . H3451 . 1.003(7) no C346 . H3461 . 1.005(7) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O11 . EU1 . O11 3_655 89.3(1) yes O11 . EU1 . O11 5_665 89.3(1) yes O11 3_655 EU1 . O11 5_665 89.3(1) yes O11 . EU1 . O12 . 80.2(1) yes O11 3_655 EU1 . O12 . 113.2(1) yes O11 5_665 EU1 . O12 . 154.8(1) yes O11 . EU1 . O12 3_655 154.8(1) yes O11 3_655 EU1 . O12 3_655 80.2(1) yes O11 5_665 EU1 . O12 3_655 113.2(1) yes O12 . EU1 . O12 3_655 83.0(1) yes O11 . EU1 . O12 5_665 113.2(1) yes O11 3_655 EU1 . O12 5_665 154.8(1) yes O11 5_665 EU1 . O12 5_665 80.2(1) yes O12 . EU1 . O12 5_665 83.0(1) yes O12 3_655 EU1 . O12 5_665 83.0(1) yes O21 . EU2 . O21 3_655 84.4(1) yes O21 . EU2 . O21 5_665 84.4(1) yes O21 3_655 EU2 . O21 5_665 84.4(1) yes O21 . EU2 . O22 . 80.0(1) yes O21 3_655 EU2 . O22 . 109.8(1) yes O21 5_665 EU2 . O22 . 157.6(1) yes O21 . EU2 . O22 3_655 157.6(1) yes O21 3_655 EU2 . O22 3_655 80.0(1) yes O21 5_665 EU2 . O22 3_655 109.8(1) yes O22 . EU2 . O22 3_655 90.2(1) yes O21 . EU2 . O22 5_665 109.8(1) yes O21 3_655 EU2 . O22 5_665 157.6(1) yes O21 5_665 EU2 . O22 5_665 80.0(1) yes O22 . EU2 . O22 5_665 90.2(1) yes O22 3_655 EU2 . O22 5_665 90.2(1) yes O31 . EU3 . O31 3_555 87.5(1) yes O31 . EU3 . O31 5_555 87.5(1) yes O31 3_555 EU3 . O31 5_555 87.5(1) yes O31 . EU3 . O32 . 81.4(1) yes O31 3_555 EU3 . O32 . 100.2(1) yes O31 5_555 EU3 . O32 . 166.2(1) yes O31 . EU3 . O32 3_555 166.2(1) yes O31 3_555 EU3 . O32 3_555 81.4(1) yes O31 5_555 EU3 . O32 3_555 100.2(1) yes O32 . EU3 . O32 3_555 92.3(1) yes O31 . EU3 . O32 5_555 100.2(1) yes O31 3_555 EU3 . O32 5_555 166.2(1) yes O31 5_555 EU3 . O32 5_555 81.4(1) yes O32 . EU3 . O32 5_555 92.3(1) yes O32 3_555 EU3 . O32 5_555 92.3(1) yes P11 . N1 . P12 . 121.1(2) yes P21 . N2 . P22 . 120.7(2) yes P31 . N3 . P32 . 124.9(3) yes N1 . P11 . O11 . 116.3(2) yes N1 . P11 . C111 . 105.5(2) yes O11 . P11 . C111 . 108.9(2) yes N1 . P11 . C121 . 109.9(2) yes O11 . P11 . C121 . 107.1(2) yes C111 . P11 . C121 . 109.1(2) yes N1 . P12 . O12 . 116.2(2) yes N1 . P12 . C131 . 106.6(2) yes O12 . P12 . C131 . 108.5(2) yes N1 . P12 . C141 . 110.6(2) yes O12 . P12 . C141 . 107.4(2) yes C131 . P12 . C141 . 107.3(2) yes N2 . P21 . O21 . 116.3(2) yes N2 . P21 . C211 . 107.4(2) yes O21 . P21 . C211 . 109.2(2) yes N2 . P21 . C221 . 110.4(2) yes O21 . P21 . C221 . 107.3(2) yes C211 . P21 . C221 . 105.7(2) yes N2 . P22 . O22 . 116.4(2) yes N2 . P22 . C231 . 106.4(2) yes O22 . P22 . C231 . 108.3(2) yes N2 . P22 . C241 . 110.1(2) yes O22 . P22 . C241 . 107.5(2) yes C231 . P22 . C241 . 107.9(2) yes N3 . P31 . O31 . 118.0(2) yes N3 . P31 . C311 . 109.8(3) yes O31 . P31 . C311 . 107.8(2) yes N3 . P31 . C321 . 107.9(2) yes O31 . P31 . C321 . 109.1(2) yes C311 . P31 . C321 . 103.2(2) yes N3 . P32 . O32 . 116.1(2) yes N3 . P32 . C331 . 110.6(2) yes O32 . P32 . C331 . 106.9(2) yes N3 . P32 . C341 . 107.0(3) yes O32 . P32 . C341 . 110.9(2) yes C331 . P32 . C341 . 104.9(2) yes EU1 . O11 . P11 . 134.0(2) yes EU1 5_665 O11 . P11 . 134.0(2) yes EU1 . O12 . P12 . 131.9(2) yes EU2 . O21 . P21 . 131.6(2) yes EU2 5_665 O21 . P21 . 131.6(2) yes EU2 . O22 . P22 . 132.4(2) yes EU3 . O31 . EU3 3_555 0.01 yes EU3 . O31 . P31 . 133.3(2) yes EU3 3_555 O31 . P31 . 133.4(2) yes EU3 . O32 . EU3 5_555 0.01 yes EU3 . O32 . P32 . 137.3(2) yes EU3 5_555 O32 . P32 . 137.3(2) yes P11 . C111 . C112 . 118.8(5) yes P11 . C111 . C116 . 121.0(4) yes C112 . C111 . C116 . 120.0(5) yes C111 . C112 . C113 . 119.7(7) yes C111 . C112 . H1121 . 120.1(6) no C113 . C112 . H1121 . 120.2(7) no C112 . C113 . C114 . 118.5(7) yes C112 . C113 . H1131 . 120.7(9) no C114 . C113 . H1131 . 120.8(8) no C113 . C114 . C115 . 122.2(7) yes C113 . C114 . H1141 . 118.2(9) no C115 . C114 . H1141 . 119.5(9) no C114 . C115 . C116 . 119.1(7) yes C114 . C115 . H1151 . 120.1(7) no C116 . C115 . H1151 . 120.8(8) no C111 . C116 . C115 . 120.5(6) yes C111 . C116 . H1161 . 119.8(5) no C115 . C116 . H1161 . 119.8(6) no P11 . C121 . C122 . 120.7(4) yes P11 . C121 . C126 . 119.9(4) yes C122 . C121 . C126 . 119.3(5) yes C121 . C122 . C123 . 119.9(5) yes C121 . C122 . H1221 . 120.2(5) no C123 . C122 . H1221 . 119.9(5) no C122 . C123 . C124 . 120.6(5) yes C122 . C123 . H1231 . 120.3(7) no C124 . C123 . H1231 . 119.1(6) no C123 . C124 . C125 . 119.6(6) yes C123 . C124 . H1241 . 121.0(7) no C125 . C124 . H1241 . 119.3(7) no C124 . C125 . C126 . 120.4(6) yes C124 . C125 . H1251 . 120.0(6) no C126 . C125 . H1251 . 119.6(6) no C121 . C126 . C125 . 120.1(5) yes C121 . C126 . H1261 . 120.3(5) no C125 . C126 . H1261 . 119.6(6) no P12 . C131 . C132 . 121.1(4) yes P12 . C131 . C136 . 119.2(4) yes C132 . C131 . C136 . 119.5(4) yes C131 . C132 . C133 . 120.0(5) yes C131 . C132 . H1321 . 119.8(5) no C133 . C132 . H1321 . 120.2(5) no C132 . C133 . C134 . 120.1(5) yes C132 . C133 . H1331 . 119.9(6) no C134 . C133 . H1331 . 120.0(6) no C133 . C134 . C135 . 120.0(5) yes C133 . C134 . H1341 . 119.6(6) no C135 . C134 . H1341 . 120.4(7) no C134 . C135 . C136 . 120.5(6) yes C134 . C135 . H1351 . 119.8(6) no C136 . C135 . H1351 . 119.8(6) no C131 . C136 . C135 . 119.9(5) yes C131 . C136 . H1361 . 120.2(5) no C135 . C136 . H1361 . 120.0(5) no P12 . C141 . C142 . 121.4(4) yes P12 . C141 . C146 . 119.7(4) yes C142 . C141 . C146 . 118.7(4) yes C141 . C142 . C143 . 119.9(5) yes C141 . C142 . H1421 . 120.0(5) no C143 . C142 . H1421 . 120.1(5) no C142 . C143 . C144 . 120.6(5) yes C142 . C143 . H1431 . 119.6(6) no C144 . C143 . H1431 . 119.8(5) no C143 . C144 . C145 . 119.8(5) yes C143 . C144 . H1441 . 119.8(6) no C145 . C144 . H1441 . 120.4(6) no C144 . C145 . C146 . 120.5(5) yes C144 . C145 . H1451 . 119.4(6) no C146 . C145 . H1451 . 120.1(6) no C141 . C146 . C145 . 120.5(5) yes C141 . C146 . H1461 . 119.8(5) no C145 . C146 . H1461 . 119.6(5) no P21 . C211 . C212 . 118.7(4) yes P21 . C211 . C216 . 122.0(4) yes C212 . C211 . C216 . 119.4(4) yes C211 . C212 . C213 . 120.4(5) yes C211 . C212 . H2121 . 119.8(5) no C213 . C212 . H2121 . 119.8(5) no C212 . C213 . C214 . 119.4(5) yes C212 . C213 . H2131 . 120.1(6) no C214 . C213 . H2131 . 120.5(5) no C213 . C214 . C215 . 120.5(5) yes C213 . C214 . H2141 . 119.4(6) no C215 . C214 . H2141 . 120.0(6) no C214 . C215 . C216 . 120.4(5) yes C214 . C215 . H2151 . 119.7(5) no C216 . C215 . H2151 . 119.9(6) no C211 . C216 . C215 . 119.9(5) yes C211 . C216 . H2161 . 120.0(4) no C215 . C216 . H2161 . 120.1(5) no P21 . C221 . C222 . 120.3(3) yes P21 . C221 . C226 . 120.7(4) yes C222 . C221 . C226 . 118.8(4) yes C221 . C222 . C223 . 120.2(4) yes C221 . C222 . H2221 . 119.7(4) no C223 . C222 . H2221 . 120.1(5) no C222 . C223 . C224 . 120.7(5) yes C222 . C223 . H2231 . 119.5(5) no C224 . C223 . H2231 . 119.7(5) no C223 . C224 . C225 . 119.2(5) yes C223 . C224 . H2241 . 120.4(6) no C225 . C224 . H2241 . 120.4(5) no C224 . C225 . C226 . 120.9(5) yes C224 . C225 . H2251 . 119.8(5) no C226 . C225 . H2251 . 119.3(6) no C221 . C226 . C225 . 120.2(5) yes C221 . C226 . H2261 . 119.8(5) no C225 . C226 . H2261 . 120.0(5) no P22 . C231 . C232 . 120.8(4) yes P22 . C231 . C236 . 119.3(4) yes C232 . C231 . C236 . 119.7(4) yes C231 . C232 . C233 . 119.4(5) yes C231 . C232 . H2321 . 120.1(5) no C233 . C232 . H2321 . 120.5(5) no C232 . C233 . C234 . 120.6(5) yes C232 . C233 . H2331 . 120.1(6) no C234 . C233 . H2331 . 119.3(5) no C233 . C234 . C235 . 120.1(5) yes C233 . C234 . H2341 . 120.2(6) no C235 . C234 . H2341 . 119.8(6) no C234 . C235 . C236 . 120.3(5) yes C234 . C235 . H2351 . 119.8(5) no C236 . C235 . H2351 . 119.8(6) no C231 . C236 . C235 . 119.8(5) yes C231 . C236 . H2361 . 120.3(5) no C235 . C236 . H2361 . 119.9(5) no P22 . C241 . C242 . 121.0(4) yes P22 . C241 . C246 . 120.1(4) yes C242 . C241 . C246 . 118.9(4) yes C241 . C242 . C243 . 120.0(5) yes C241 . C242 . H2421 . 120.2(5) no C243 . C242 . H2421 . 119.9(5) no C242 . C243 . C244 . 120.5(5) yes C242 . C243 . H2431 . 119.9(6) no C244 . C243 . H2431 . 119.6(6) no C243 . C244 . C245 . 119.8(5) yes C243 . C244 . H2441 . 120.5(6) no C245 . C244 . H2441 . 119.7(6) no C244 . C245 . C246 . 120.5(5) yes C244 . C245 . H2451 . 119.7(5) no C246 . C245 . H2451 . 119.8(6) no C241 . C246 . C245 . 120.3(5) yes C241 . C246 . H2461 . 120.0(5) no C245 . C246 . H2461 . 119.7(5) no P31 . C311 . C312 . 120.7(5) yes P31 . C311 . C316 . 120.1(5) yes C312 . C311 . C316 . 119.0(6) yes C311 . C312 . C313 . 120.3(8) yes C311 . C312 . H3121 . 119.6(6) no C313 . C312 . H3121 . 120.1(8) no C312 . C313 . C314 . 119.3(9) yes C312 . C313 . H3131 . 120.6(13) no C314 . C313 . H3131 . 120.1(12) no C313 . C314 . C315 . 122.7(9) yes C313 . C314 . H3141 . 119.3(15) no C315 . C314 . H3141 . 118.0(15) no C314 . C315 . C316 . 118.2(10) yes C314 . C315 . H3151 . 121.6(11) no C316 . C315 . H3151 . 120.2(12) no C311 . C316 . C315 . 120.5(8) yes C311 . C316 . H3161 . 119.5(6) no C315 . C316 . H3161 . 119.9(9) no P31 . C321 . C322 . 119.0(4) yes P31 . C321 . C326 . 122.4(4) yes C322 . C321 . C326 . 118.5(5) yes C321 . C322 . C323 . 120.7(6) yes C321 . C322 . H3221 . 119.6(5) no C323 . C322 . H3221 . 119.7(7) no C322 . C323 . C324 . 120.4(7) yes C322 . C323 . H3231 . 120.1(7) no C324 . C323 . H3231 . 119.5(6) no C323 . C324 . C325 . 120.0(5) yes C323 . C324 . H3241 . 120.0(8) no C325 . C324 . H3241 . 120.0(7) no C324 . C325 . C326 . 120.1(6) yes C324 . C325 . H3251 . 120.4(7) no C326 . C325 . H3251 . 119.5(8) no C321 . C326 . C325 . 120.3(6) yes C321 . C326 . H3261 . 119.5(5) no C325 . C326 . H3261 . 120.2(6) no P32 . C331 . C332 . 119.6(4) yes P32 . C331 . C336 . 122.1(4) yes C332 . C331 . C336 . 118.3(5) yes C331 . C332 . C333 . 120.6(6) yes C331 . C332 . H3321 . 119.6(5) no C333 . C332 . H3321 . 119.9(6) no C332 . C333 . C334 . 119.9(6) yes C332 . C333 . H3331 . 119.7(7) no C334 . C333 . H3331 . 120.3(7) no C333 . C334 . C335 . 120.1(6) yes C333 . C334 . H3341 . 120.0(7) no C335 . C334 . H3341 . 120.0(7) no C334 . C335 . C336 . 120.9(6) yes C334 . C335 . H3351 . 119.7(7) no C336 . C335 . H3351 . 119.4(7) no C331 . C336 . C335 . 120.2(6) yes C331 . C336 . H3361 . 120.2(5) no C335 . C336 . H3361 . 119.6(6) no P32 . C341 . C342 . 119.5(4) yes P32 . C341 . C346 . 121.9(5) yes C342 . C341 . C346 . 118.6(6) yes C341 . C342 . C343 . 120.2(7) yes C341 . C342 . H3421 . 120.4(6) no C343 . C342 . H3421 . 119.4(7) no C342 . C343 . C344 . 120.3(8) yes C342 . C343 . H3431 . 120.3(8) no C344 . C343 . H3431 . 119.4(7) no C343 . C344 . C345 . 120.4(7) yes C343 . C344 . H3441 . 120.2(9) no C345 . C344 . H3441 . 119.4(8) no C344 . C345 . C346 . 120.5(7) yes C344 . C345 . H3451 . 120.0(7) no C346 . C345 . H3451 . 119.5(8) no C341 . C346 . C345 . 119.9(7) yes C341 . C346 . H3461 . 120.0(6) no C345 . C346 . H3461 . 120.1(6) no #=END data_smtbp2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Tb(Ph2PONPOPh2)3].0.75H2O _chemical_formula_sum 'C72 H61.50 N3 O6.75 P6 Tb' _chemical_formula_weight 1421.48 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 Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 23.372(4) _cell_length_b 23.372(4) _cell_length_c 42.956(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 20320(6) _cell_formula_units_Z 12 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 11 _cell_measurement_theta_max 12 _exptl_crystal_description 'tablet developed in (001)' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8682 _exptl_absorpt_coefficient_mu 1.240 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.592 _exptl_absorpt_correction_T_max 0.886 _exptl_absorpt_process_details 'xshape vs psi-scans' _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 ? _diffrn_measurement_method 'Omega-theta with learnt-profile' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 9599 _diffrn_reflns_av_R_equivalents 0.1601 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.04 _reflns_number_total 7979 _reflns_number_gt 5674 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution SIR92 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics SHELXTL _computing_publication_material ? _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^)+(0.0859P)^2^+146.1677P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometric; disordered H not placed' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7979 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1744 _refine_ls_wR_factor_gt 0.1492 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 1.0000 0.0000 0.611166(14) 0.02450(17) Uani 1 3 d S . . O1 O 1.0728(2) 0.0815(2) 0.64257(11) 0.0318(11) Uani 1 1 d . . . P1 P 1.08765(9) 0.15216(9) 0.64795(4) 0.0281(4) Uani 1 1 d . . . O2 O 1.0125(2) 0.0860(2) 0.58269(11) 0.0328(12) Uani 1 1 d . . . P2 P 1.04175(10) 0.15998(9) 0.58738(4) 0.0305(4) Uani 1 1 d . . . N1 N 1.0735(3) 0.1883(3) 0.62064(14) 0.0347(15) Uani 1 1 d . . . C11 C 1.1731(4) 0.1999(4) 0.65919(17) 0.0330(17) Uani 1 1 d . . . C21 C 1.2048(4) 0.1680(5) 0.6711(2) 0.049(2) Uani 1 1 d . . . H21 H 1.1819 0.1216 0.6727 0.059 Uiso 1 1 calc R . . C31 C 1.2692(5) 0.2037(6) 0.6805(2) 0.069(3) Uani 1 1 d . . . H31 H 1.2901 0.1819 0.6892 0.083 Uiso 1 1 calc R . . C41 C 1.3039(5) 0.2718(7) 0.6774(3) 0.083(4) Uani 1 1 d . . . H41 H 1.3485 0.2961 0.6835 0.099 Uiso 1 1 calc R . . C51 C 1.2730(5) 0.3034(6) 0.6654(3) 0.075(3) Uani 1 1 d . . . H51 H 1.2965 0.3497 0.6636 0.090 Uiso 1 1 calc R . . C61 C 1.2078(4) 0.2687(4) 0.6557(2) 0.050(2) Uani 1 1 d . . . H61 H 1.1873 0.2908 0.6470 0.060 Uiso 1 1 calc R . . C12 C 1.0405(3) 0.1520(3) 0.68106(16) 0.0287(16) Uani 1 1 d . . . C22 C 1.0332(4) 0.1123(4) 0.70638(19) 0.045(2) Uani 1 1 d . . . H22 H 1.0522 0.0851 0.7061 0.054 Uiso 1 1 calc R . . C32 C 0.9977(5) 0.1126(5) 0.7322(2) 0.060(3) Uani 1 1 d . . . H32 H 0.9930 0.0857 0.7494 0.072 Uiso 1 1 calc R . . C42 C 0.9696(4) 0.1517(5) 0.7330(2) 0.055(3) Uani 1 1 d . . . H42 H 0.9462 0.1523 0.7507 0.066 Uiso 1 1 calc R . . C52 C 0.9759(5) 0.1894(5) 0.7080(2) 0.056(2) Uani 1 1 d . . . H52 H 0.9556 0.2155 0.7083 0.067 Uiso 1 1 calc R . . C62 C 1.0113(4) 0.1907(4) 0.6823(2) 0.046(2) Uani 1 1 d . . . H62 H 1.0156 0.2180 0.6653 0.055 Uiso 1 1 calc R . . C13 C 1.1042(4) 0.2030(4) 0.55829(18) 0.0369(18) Uani 1 1 d . . . C23 C 1.1699(5) 0.2409(5) 0.5674(2) 0.053(2) Uani 1 1 d . . . H23 H 1.1805 0.2470 0.5887 0.064 Uiso 1 1 calc R . . C33 C 1.2201(5) 0.2698(5) 0.5453(3) 0.067(3) Uani 1 1 d . . . H33 H 1.2646 0.2937 0.5515 0.081 Uiso 1 1 calc R . . C43 C 1.2037(6) 0.2627(5) 0.5147(3) 0.066(3) Uani 1 1 d . . . H43 H 1.2375 0.2834 0.4999 0.080 Uiso 1 1 calc R . . C53 C 1.1411(6) 0.2272(5) 0.5050(2) 0.059(3) Uani 1 1 d . . . H53 H 1.1316 0.2228 0.4836 0.071 Uiso 1 1 calc R . . C63 C 1.0894(5) 0.1963(4) 0.5268(2) 0.048(2) Uani 1 1 d . . . H63 H 1.0454 0.1713 0.5200 0.058 Uiso 1 1 calc R . . C14 C 0.9759(4) 0.1775(4) 0.58102(17) 0.0354(18) Uani 1 1 d . . . C24 C 0.9859(5) 0.2369(4) 0.56925(19) 0.045(2) Uani 1 1 d . . . H24 H 1.0286 0.2699 0.5633 0.054 Uiso 1 1 calc R . . C34 C 0.9328(6) 0.2476(6) 0.5662(2) 0.067(3) Uani 1 1 d . . . H34 H 0.9392 0.2878 0.5582 0.080 Uiso 1 1 calc R . . C44 C 0.8730(6) 0.2004(7) 0.5746(3) 0.080(4) Uani 1 1 d . . . H44 H 0.8379 0.2088 0.5722 0.096 Uiso 1 1 calc R . . C54 C 0.8589(6) 0.1401(7) 0.5864(3) 0.083(4) Uani 1 1 d . . . H54 H 0.8159 0.1082 0.5924 0.100 Uiso 1 1 calc R . . C64 C 0.9121(5) 0.1293(5) 0.5891(2) 0.062(3) Uani 1 1 d . . . H64 H 0.9047 0.0883 0.5965 0.075 Uiso 1 1 calc R . . Tb2 Tb 0.3333 -0.3333 0.540413(14) 0.02473(17) Uani 1 3 d S . . O3 O 0.4108(2) -0.2603(2) 0.57384(11) 0.0299(11) Uani 1 1 d . . . O4 O 0.4126(2) -0.2634(2) 0.50594(11) 0.0311(11) Uani 1 1 d . . . P3 P 0.48341(9) -0.20768(9) 0.57281(4) 0.0281(4) Uani 1 1 d . . . P4 P 0.48490(9) -0.21205(9) 0.50784(5) 0.0296(4) Uani 1 1 d . . . N2 N 0.5111(3) -0.1737(3) 0.53971(14) 0.0322(14) Uani 1 1 d . . . C15 C 0.5005(4) -0.1414(4) 0.59955(19) 0.0369(18) Uani 1 1 d . . . C25 C 0.4785(5) -0.1569(5) 0.6301(2) 0.053(2) Uani 1 1 d . . . H25 H 0.4547 -0.2010 0.6368 0.064 Uiso 1 1 calc R . . C35 C 0.4927(5) -0.1046(6) 0.6507(2) 0.067(3) Uani 1 1 d . . . H35 H 0.4774 -0.1145 0.6713 0.081 Uiso 1 1 calc R . . C45 C 0.5276(5) -0.0407(5) 0.6418(3) 0.062(3) Uani 1 1 d . . . H45 H 0.5368 -0.0068 0.6562 0.075 Uiso 1 1 calc R . . C55 C 0.5494(5) -0.0258(5) 0.6121(3) 0.063(3) Uani 1 1 d . . . H55 H 0.5738 0.0186 0.6057 0.076 Uiso 1 1 calc R . . C65 C 0.5357(4) -0.0762(4) 0.5908(2) 0.047(2) Uani 1 1 d . . . H65 H 0.5509 -0.0654 0.5702 0.057 Uiso 1 1 calc R . . C16 C 0.5296(4) -0.2449(4) 0.58729(17) 0.0305(16) Uani 1 1 d . . . C26 C 0.5969(4) -0.2063(4) 0.5932(2) 0.043(2) Uani 1 1 d . . . H26 H 0.6178 -0.1602 0.5911 0.051 Uiso 1 1 calc R . . C36 C 0.6331(4) -0.2357(4) 0.6020(2) 0.045(2) Uani 1 1 d . . . H36 H 0.6785 -0.2095 0.6061 0.054 Uiso 1 1 calc R . . C46 C 0.6031(4) -0.3022(5) 0.6049(2) 0.056(2) Uani 1 1 d . . . H46 H 0.6282 -0.3219 0.6105 0.067 Uiso 1 1 calc R . . C56 C 0.5365(5) -0.3413(5) 0.5997(2) 0.058(3) Uani 1 1 d . . . H56 H 0.5162 -0.3874 0.6022 0.070 Uiso 1 1 calc R . . C66 C 0.4987(4) -0.3127(4) 0.5908(2) 0.047(2) Uani 1 1 d . . . H66 H 0.4530 -0.3391 0.5872 0.057 Uiso 1 1 calc R . . C17 C 0.5036(3) -0.1496(4) 0.47859(18) 0.0307(16) Uani 1 1 d . . . C27 C 0.4901(4) -0.1669(4) 0.4476(2) 0.046(2) Uani 1 1 d . . . H27 H 0.4717 -0.2113 0.4417 0.056 Uiso 1 1 calc R . . C37 C 0.5036(5) -0.1191(5) 0.4254(2) 0.059(3) Uani 1 1 d . . . H37 H 0.4939 -0.1315 0.4044 0.071 Uiso 1 1 calc R . . C47 C 0.5302(4) -0.0553(5) 0.4333(2) 0.054(3) Uani 1 1 d . . . H47 H 0.5391 -0.0235 0.4178 0.065 Uiso 1 1 calc R . . C57 C 0.5444(5) -0.0360(5) 0.4638(2) 0.058(3) Uani 1 1 d . . . H57 H 0.5628 0.0086 0.4695 0.069 Uiso 1 1 calc R . . C67 C 0.5309(4) -0.0842(4) 0.4863(2) 0.047(2) Uani 1 1 d . . . H67 H 0.5409 -0.0715 0.5073 0.056 Uiso 1 1 calc R . . C18 C 0.5288(4) -0.2541(4) 0.49707(17) 0.0326(17) Uani 1 1 d . . . C28 C 0.4958(4) -0.3180(4) 0.4863(2) 0.042(2) Uani 1 1 d . . . H28 H 0.4496 -0.3401 0.4841 0.051 Uiso 1 1 calc R . . C38 C 0.5306(5) -0.3502(5) 0.4788(2) 0.056(2) Uani 1 1 d . . . H38 H 0.5076 -0.3940 0.4716 0.067 Uiso 1 1 calc R . . C48 C 0.5973(4) -0.3188(5) 0.4816(3) 0.062(3) Uani 1 1 d . . . H48 H 0.6205 -0.3403 0.4757 0.074 Uiso 1 1 calc R . . C58 C 0.6315(5) -0.2544(5) 0.4933(3) 0.071(3) Uani 1 1 d . . . H58 H 0.6775 -0.2332 0.4962 0.085 Uiso 1 1 calc R . . C68 C 0.5975(4) -0.2218(4) 0.5008(3) 0.057(3) Uani 1 1 d . . . H68 H 0.6204 -0.1781 0.5082 0.068 Uiso 1 1 calc R . . O1W O 0.6667 0.3333 0.1175(3) 0.117(6) Uani 1 3 d S . . O2W O 0.0000 0.0000 0.0188(5) 0.062(6) Uani 0.50 3 d SP . . 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 0.0227(2) 0.0227(2) 0.0282(3) 0.000 0.000 0.01133(11) O1 0.034(3) 0.028(3) 0.037(3) -0.001(2) -0.006(2) 0.018(2) P1 0.0284(10) 0.0240(9) 0.0272(10) -0.0009(8) -0.0017(8) 0.0096(8) O2 0.039(3) 0.031(3) 0.030(3) 0.004(2) -0.002(2) 0.018(2) P2 0.0398(11) 0.0285(10) 0.0268(10) 0.0050(8) 0.0024(8) 0.0198(9) N1 0.039(4) 0.030(3) 0.033(4) 0.001(3) -0.003(3) 0.015(3) C11 0.027(4) 0.028(4) 0.034(4) -0.005(3) 0.000(3) 0.006(3) C21 0.040(5) 0.056(6) 0.050(5) -0.008(4) -0.009(4) 0.023(4) C31 0.046(6) 0.106(9) 0.061(7) -0.019(6) -0.016(5) 0.042(7) C41 0.033(6) 0.104(10) 0.085(9) -0.039(8) -0.006(6) 0.015(6) C51 0.042(6) 0.061(7) 0.090(9) -0.021(6) -0.002(6) 0.001(5) C61 0.042(5) 0.042(5) 0.057(6) -0.005(4) 0.001(4) 0.015(4) C12 0.027(4) 0.025(4) 0.029(4) -0.002(3) 0.002(3) 0.009(3) C22 0.041(5) 0.055(6) 0.041(5) 0.009(4) 0.006(4) 0.026(4) C32 0.047(6) 0.091(8) 0.034(5) 0.014(5) 0.006(4) 0.029(6) C42 0.033(5) 0.081(7) 0.041(5) -0.015(5) 0.008(4) 0.020(5) C52 0.056(6) 0.058(6) 0.059(6) -0.002(5) 0.016(5) 0.034(5) C62 0.057(6) 0.047(5) 0.037(5) 0.000(4) 0.007(4) 0.028(5) C13 0.044(5) 0.035(4) 0.036(4) 0.005(3) 0.010(4) 0.023(4) C23 0.052(6) 0.057(6) 0.046(5) 0.000(4) 0.013(4) 0.024(5) C33 0.055(6) 0.075(7) 0.070(7) 0.006(6) 0.017(5) 0.030(6) C43 0.077(8) 0.075(7) 0.058(7) 0.024(6) 0.028(6) 0.046(7) C53 0.089(8) 0.078(7) 0.035(5) 0.014(5) 0.024(5) 0.060(7) C63 0.061(6) 0.051(5) 0.038(5) 0.004(4) -0.002(4) 0.032(5) C14 0.043(5) 0.048(5) 0.024(4) -0.002(3) -0.003(3) 0.030(4) C24 0.058(6) 0.049(5) 0.042(5) 0.000(4) -0.002(4) 0.038(5) C34 0.094(9) 0.086(8) 0.061(7) -0.010(6) -0.009(6) 0.076(8) C44 0.083(9) 0.134(12) 0.069(8) -0.014(8) -0.003(7) 0.089(9) C54 0.066(8) 0.105(10) 0.099(10) 0.019(8) 0.021(7) 0.058(8) C64 0.046(6) 0.067(7) 0.080(8) 0.012(6) 0.013(5) 0.032(5) Tb2 0.0219(2) 0.0219(2) 0.0304(4) 0.000 0.000 0.01094(10) O3 0.027(3) 0.029(3) 0.032(3) -0.003(2) -0.003(2) 0.013(2) O4 0.027(3) 0.035(3) 0.029(3) 0.000(2) 0.004(2) 0.014(2) P3 0.0249(10) 0.0269(10) 0.0294(10) -0.0039(8) -0.0026(8) 0.0107(8) P4 0.0256(10) 0.0270(10) 0.0320(11) 0.0016(8) 0.0026(8) 0.0099(8) N2 0.026(3) 0.024(3) 0.032(3) 0.001(3) -0.001(3) 0.002(3) C15 0.032(4) 0.039(5) 0.041(5) -0.011(4) -0.007(3) 0.018(4) C25 0.055(6) 0.056(6) 0.040(5) -0.013(4) 0.002(4) 0.022(5) C35 0.062(7) 0.091(8) 0.048(6) -0.033(6) -0.004(5) 0.038(6) C45 0.066(7) 0.049(6) 0.076(8) -0.036(5) -0.019(6) 0.032(5) C55 0.075(7) 0.038(5) 0.075(8) -0.016(5) -0.018(6) 0.028(5) C65 0.058(6) 0.034(5) 0.050(5) -0.012(4) -0.009(4) 0.024(4) C16 0.033(4) 0.033(4) 0.030(4) 0.003(3) 0.001(3) 0.019(3) C26 0.034(4) 0.042(5) 0.052(5) 0.000(4) 0.000(4) 0.018(4) C36 0.030(4) 0.046(5) 0.052(5) -0.001(4) -0.003(4) 0.015(4) C46 0.047(6) 0.065(7) 0.066(7) 0.013(5) 0.002(5) 0.036(5) C56 0.051(6) 0.049(6) 0.079(7) 0.012(5) -0.003(5) 0.029(5) C66 0.037(5) 0.038(5) 0.069(6) -0.003(4) -0.007(4) 0.020(4) C17 0.023(4) 0.030(4) 0.036(4) 0.004(3) 0.006(3) 0.011(3) C27 0.048(5) 0.032(4) 0.044(5) 0.004(4) -0.006(4) 0.008(4) C37 0.047(6) 0.062(7) 0.054(6) 0.005(5) -0.014(5) 0.016(5) C47 0.043(5) 0.046(6) 0.063(6) 0.031(5) 0.001(5) 0.014(4) C57 0.067(7) 0.036(5) 0.063(7) 0.012(5) 0.004(5) 0.020(5) C67 0.057(6) 0.031(4) 0.042(5) 0.006(4) 0.000(4) 0.014(4) C18 0.029(4) 0.035(4) 0.033(4) 0.007(3) 0.012(3) 0.015(3) C28 0.035(4) 0.042(5) 0.050(5) -0.006(4) 0.002(4) 0.019(4) C38 0.056(6) 0.047(5) 0.069(7) -0.006(5) 0.009(5) 0.029(5) C48 0.042(5) 0.062(6) 0.096(8) 0.016(6) 0.018(5) 0.037(5) C58 0.031(5) 0.050(6) 0.132(11) -0.005(6) 0.000(6) 0.020(5) C68 0.032(5) 0.036(5) 0.100(8) -0.014(5) -0.007(5) 0.015(4) O1W 0.149(9) 0.149(9) 0.054(9) 0.000 0.000 0.074(5) O2W 0.070(10) 0.070(10) 0.048(13) 0.000 0.000 0.035(5) _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 O2 2.244(5) 2_645 ? Tb1 O2 2.244(5) 3_765 ? Tb1 O2 2.244(5) . ? Tb1 O1 2.259(5) . ? Tb1 O1 2.259(5) 2_645 ? Tb1 O1 2.259(5) 3_765 ? O1 P1 1.526(5) . ? P1 N1 1.575(6) . ? P1 C12 1.798(7) . ? P1 C11 1.800(7) . ? O2 P2 1.521(5) . ? P2 N1 1.593(6) . ? P2 C13 1.799(8) . ? P2 C14 1.800(8) . ? C11 C21 1.386(11) . ? C11 C61 1.400(11) . ? C21 C31 1.369(12) . ? C31 C41 1.385(16) . ? C41 C51 1.368(17) . ? C51 C61 1.384(13) . ? C12 C62 1.380(11) . ? C12 C22 1.384(11) . ? C22 C32 1.388(12) . ? C32 C42 1.366(14) . ? C42 C52 1.351(13) . ? C52 C62 1.373(12) . ? C13 C63 1.388(11) . ? C13 C23 1.389(12) . ? C23 C33 1.394(13) . ? C33 C43 1.354(14) . ? C43 C53 1.338(14) . ? C53 C63 1.407(12) . ? C14 C24 1.383(11) . ? C14 C64 1.389(12) . ? C24 C34 1.390(12) . ? C34 C44 1.326(16) . ? C44 C54 1.373(16) . ? C54 C64 1.394(13) . ? Tb2 O3 2.272(5) 2_545 ? Tb2 O3 2.272(5) . ? Tb2 O3 2.272(5) 3_655 ? Tb2 O4 2.295(5) 2_545 ? Tb2 O4 2.295(5) . ? Tb2 O4 2.295(5) 3_655 ? O3 P3 1.519(5) . ? O4 P4 1.508(5) . ? P3 N2 1.599(6) . ? P3 C16 1.802(7) . ? P3 C15 1.806(8) . ? P4 N2 1.582(6) . ? P4 C18 1.801(7) . ? P4 C17 1.806(7) . ? C15 C65 1.372(11) . ? C15 C25 1.389(12) . ? C25 C35 1.408(12) . ? C35 C45 1.349(14) . ? C45 C55 1.356(14) . ? C55 C65 1.396(12) . ? C16 C66 1.381(11) . ? C16 C26 1.390(10) . ? C26 C36 1.383(11) . ? C36 C46 1.354(12) . ? C46 C56 1.372(12) . ? C56 C66 1.405(12) . ? C17 C67 1.370(11) . ? C17 C27 1.379(11) . ? C27 C37 1.382(12) . ? C37 C47 1.340(13) . ? C47 C57 1.374(13) . ? C57 C67 1.396(12) . ? C18 C28 1.373(11) . ? C18 C68 1.399(11) . ? C28 C38 1.395(11) . ? C38 C48 1.357(12) . ? C48 C58 1.398(14) . ? C58 C68 1.385(12) . ? O2W O2W 1.61(4) 10 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Tb1 O2 93.12(17) 2_645 3_765 ? O2 Tb1 O2 93.12(17) 2_645 . ? O2 Tb1 O2 93.12(17) 3_765 . ? O2 Tb1 O1 168.51(17) 2_645 . ? O2 Tb1 O1 97.60(18) 3_765 . ? O2 Tb1 O1 82.21(18) . . ? O2 Tb1 O1 82.21(18) 2_645 2_645 ? O2 Tb1 O1 168.51(17) 3_765 2_645 ? O2 Tb1 O1 97.60(18) . 2_645 ? O1 Tb1 O1 87.99(18) . 2_645 ? O2 Tb1 O1 97.60(18) 2_645 3_765 ? O2 Tb1 O1 82.21(17) 3_765 3_765 ? O2 Tb1 O1 168.51(18) . 3_765 ? O1 Tb1 O1 87.99(18) . 3_765 ? O1 Tb1 O1 87.99(18) 2_645 3_765 ? P1 O1 Tb1 132.1(3) . . ? O1 P1 N1 118.3(3) . . ? O1 P1 C12 108.1(3) . . ? N1 P1 C12 107.3(3) . . ? O1 P1 C11 107.1(3) . . ? N1 P1 C11 109.4(4) . . ? C12 P1 C11 106.1(3) . . ? P2 O2 Tb1 136.8(3) . . ? O2 P2 N1 116.3(3) . . ? O2 P2 C13 108.7(3) . . ? N1 P2 C13 108.1(4) . . ? O2 P2 C14 106.8(3) . . ? N1 P2 C14 108.3(3) . . ? C13 P2 C14 108.3(4) . . ? P1 N1 P2 128.6(4) . . ? C21 C11 C61 120.0(8) . . ? C21 C11 P1 119.4(6) . . ? C61 C11 P1 120.6(6) . . ? C31 C21 C11 120.1(9) . . ? C21 C31 C41 120.3(11) . . ? C51 C41 C31 119.6(10) . . ? C41 C51 C61 121.4(11) . . ? C51 C61 C11 118.4(10) . . ? C62 C12 C22 118.3(7) . . ? C62 C12 P1 122.1(6) . . ? C22 C12 P1 119.5(6) . . ? C12 C22 C32 119.9(8) . . ? C42 C32 C22 120.9(9) . . ? C52 C42 C32 118.9(9) . . ? C42 C52 C62 121.5(9) . . ? C52 C62 C12 120.4(8) . . ? C63 C13 C23 118.7(8) . . ? C63 C13 P2 121.9(7) . . ? C23 C13 P2 119.3(6) . . ? C13 C23 C33 120.8(9) . . ? C43 C33 C23 118.8(10) . . ? C53 C43 C33 122.3(10) . . ? C43 C53 C63 120.2(9) . . ? C13 C63 C53 119.2(9) . . ? C24 C14 C64 118.7(8) . . ? C24 C14 P2 123.2(7) . . ? C64 C14 P2 118.1(7) . . ? C14 C24 C34 119.8(9) . . ? C44 C34 C24 119.3(10) . . ? C34 C44 C54 124.5(10) . . ? C44 C54 C64 116.0(11) . . ? C14 C64 C54 121.7(10) . . ? O3 Tb2 O3 84.31(18) 2_545 . ? O3 Tb2 O3 84.31(18) 2_545 3_655 ? O3 Tb2 O3 84.31(18) . 3_655 ? O3 Tb2 O4 79.44(17) 2_545 2_545 ? O3 Tb2 O4 132.35(17) . 2_545 ? O3 Tb2 O4 137.13(17) 3_655 2_545 ? O3 Tb2 O4 137.13(17) 2_545 . ? O3 Tb2 O4 79.44(17) . . ? O3 Tb2 O4 132.35(17) 3_655 . ? O4 Tb2 O4 82.85(18) 2_545 . ? O3 Tb2 O4 132.35(17) 2_545 3_655 ? O3 Tb2 O4 137.13(17) . 3_655 ? O3 Tb2 O4 79.44(17) 3_655 3_655 ? O4 Tb2 O4 82.85(18) 2_545 3_655 ? O4 Tb2 O4 82.85(18) . 3_655 ? P3 O3 Tb2 137.5(3) . . ? P4 O4 Tb2 135.7(3) . . ? O3 P3 N2 116.0(3) . . ? O3 P3 C16 107.2(3) . . ? N2 P3 C16 110.8(3) . . ? O3 P3 C15 110.7(3) . . ? N2 P3 C15 106.2(4) . . ? C16 P3 C15 105.4(4) . . ? O4 P4 N2 117.4(3) . . ? O4 P4 C18 105.6(3) . . ? N2 P4 C18 111.5(4) . . ? O4 P4 C17 109.2(3) . . ? N2 P4 C17 106.0(3) . . ? C18 P4 C17 106.8(3) . . ? P4 N2 P3 122.8(4) . . ? C65 C15 C25 119.1(8) . . ? C65 C15 P3 122.1(6) . . ? C25 C15 P3 118.8(7) . . ? C15 C25 C35 118.1(9) . . ? C45 C35 C25 122.2(10) . . ? C35 C45 C55 119.5(9) . . ? C45 C55 C65 120.0(9) . . ? C15 C65 C55 121.1(9) . . ? C66 C16 C26 119.9(7) . . ? C66 C16 P3 119.6(6) . . ? C26 C16 P3 120.4(6) . . ? C36 C26 C16 120.2(8) . . ? C46 C36 C26 120.1(8) . . ? C36 C46 C56 120.9(9) . . ? C46 C56 C66 120.1(9) . . ? C16 C66 C56 118.9(8) . . ? C67 C17 C27 118.1(7) . . ? C67 C17 P4 121.4(6) . . ? C27 C17 P4 120.4(6) . . ? C17 C27 C37 120.2(8) . . ? C47 C37 C27 121.1(9) . . ? C37 C47 C57 120.5(9) . . ? C47 C57 C67 118.5(9) . . ? C17 C67 C57 121.5(9) . . ? C28 C18 C68 119.7(7) . . ? C28 C18 P4 121.0(6) . . ? C68 C18 P4 119.3(6) . . ? C18 C28 C38 120.1(8) . . ? C48 C38 C28 120.7(9) . . ? C38 C48 C58 119.8(9) . . ? C68 C58 C48 120.0(9) . . ? C58 C68 C18 119.7(8) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.605 _refine_diff_density_min -1.529 _refine_diff_density_rms 0.135