data_La _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common La _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 La N3 O12 P2, 2(C2 H6 O)' _chemical_formula_sum 'C28 H68 La N3 O14 P2' _chemical_formula_weight 871.70 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 Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.3180(5) _cell_length_b 14.2982(5) _cell_length_c 17.5534(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.241(2) _cell_angle_gamma 90.00 _cell_volume 4151.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 85359 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 1.166 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8728 _exptl_absorpt_correction_T_max 0.9549 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50789 _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9504 _reflns_number_gt 7438 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _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^ > 2\s(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^+4.5509P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9504 _refine_ls_number_parameters 461 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7605(2) 0.4444(3) 0.7271(2) 0.0236(8) Uani 1 1 d . . . C2 C 0.7788(2) 0.5061(3) 0.6627(2) 0.0326(9) Uani 1 1 d . . . H2A H 0.8374 0.5151 0.6754 0.049 Uiso 1 1 calc R . . H2B H 0.7524 0.5670 0.6612 0.049 Uiso 1 1 calc R . . H2C H 0.7584 0.4756 0.6106 0.049 Uiso 1 1 calc R . . C3 C 0.8061(2) 0.3513(3) 0.7304(2) 0.0291(8) Uani 1 1 d . . . H3A H 0.7906 0.3226 0.6773 0.044 Uiso 1 1 calc R . . H3B H 0.7921 0.3089 0.7682 0.044 Uiso 1 1 calc R . . H3C H 0.8644 0.3630 0.7478 0.044 Uiso 1 1 calc R . . C4 C 0.7959(2) 0.4909(3) 0.8095(2) 0.0289(8) Uani 1 1 d . . . H4A H 0.7835 0.4524 0.8505 0.043 Uiso 1 1 calc R . . H4B H 0.7722 0.5532 0.8090 0.043 Uiso 1 1 calc R . . H4C H 0.8547 0.4966 0.8212 0.043 Uiso 1 1 calc R . . C5 C 0.6112(2) 0.3317(3) 0.6300(2) 0.0243(8) Uani 1 1 d . . . C6 C 0.6447(3) 0.2342(3) 0.6616(2) 0.0292(9) Uani 1 1 d . . . H6A H 0.6416 0.2262 0.7161 0.044 Uiso 1 1 calc R . . H6B H 0.7012 0.2293 0.6617 0.044 Uiso 1 1 calc R . . H6C H 0.6125 0.1856 0.6272 0.044 Uiso 1 1 calc R . . C7 C 0.5194(2) 0.3252(3) 0.6096(2) 0.0298(9) Uani 1 1 d . . . H7A H 0.4951 0.3834 0.5841 0.045 Uiso 1 1 calc R . . H7B H 0.5043 0.3152 0.6585 0.045 Uiso 1 1 calc R . . H7C H 0.4999 0.2727 0.5730 0.045 Uiso 1 1 calc R . . C8 C 0.6344(2) 0.3510(3) 0.5526(2) 0.0297(9) Uani 1 1 d . . . H8A H 0.6093 0.3039 0.5124 0.045 Uiso 1 1 calc R . . H8B H 0.6933 0.3482 0.5642 0.045 Uiso 1 1 calc R . . H8C H 0.6152 0.4133 0.5323 0.045 Uiso 1 1 calc R . . C9 C 0.5902(2) 0.5330(3) 0.6866(2) 0.0244(8) Uani 1 1 d . . . C10 C 0.6335(3) 0.6131(3) 0.7411(2) 0.0317(9) Uani 1 1 d . . . H10A H 0.6818 0.6316 0.7265 0.048 Uiso 1 1 calc R . . H10B H 0.6495 0.5921 0.7968 0.048 Uiso 1 1 calc R . . H10C H 0.5970 0.6668 0.7349 0.048 Uiso 1 1 calc R . . C11 C 0.5092(2) 0.5187(3) 0.7067(3) 0.0323(9) Uani 1 1 d . . . H11A H 0.4759 0.5751 0.6923 0.049 Uiso 1 1 calc R . . H11B H 0.5206 0.5066 0.7639 0.049 Uiso 1 1 calc R . . H11C H 0.4801 0.4652 0.6765 0.049 Uiso 1 1 calc R . . C12 C 0.5720(2) 0.5643(3) 0.5998(2) 0.0308(9) Uani 1 1 d . . . H12A H 0.5428 0.6240 0.5923 0.046 Uiso 1 1 calc R . . H12B H 0.5386 0.5169 0.5647 0.046 Uiso 1 1 calc R . . H12C H 0.6228 0.5720 0.5866 0.046 Uiso 1 1 calc R . . C13 C 0.7705(2) 0.2821(3) 1.1799(2) 0.0251(8) Uani 1 1 d . . . C14 C 0.7476(3) 0.3845(3) 1.1538(2) 0.0310(9) Uani 1 1 d . . . H14A H 0.7915 0.4263 1.1825 0.046 Uiso 1 1 calc R . . H14B H 0.6979 0.4015 1.1663 0.046 Uiso 1 1 calc R . . H14C H 0.7391 0.3904 1.0963 0.046 Uiso 1 1 calc R . . C15 C 0.8513(2) 0.2649(3) 1.1619(2) 0.0285(8) Uani 1 1 d . . . H15A H 0.8907 0.3124 1.1889 0.043 Uiso 1 1 calc R . . H15B H 0.8427 0.2686 1.1042 0.043 Uiso 1 1 calc R . . H15C H 0.8719 0.2027 1.1811 0.043 Uiso 1 1 calc R . . C16 C 0.7866(2) 0.2715(3) 1.2707(2) 0.0307(9) Uani 1 1 d . . . H16A H 0.8009 0.2064 1.2862 0.046 Uiso 1 1 calc R . . H16B H 0.7379 0.2887 1.2850 0.046 Uiso 1 1 calc R . . H16C H 0.8313 0.3126 1.2987 0.046 Uiso 1 1 calc R . . C17 C 0.7281(2) 0.0830(3) 1.1112(2) 0.0268(8) Uani 1 1 d . . . C18 C 0.7793(3) 0.0841(3) 1.0528(2) 0.0307(9) Uani 1 1 d . . . H18A H 0.7969 0.0203 1.0459 0.046 Uiso 1 1 calc R . . H18B H 0.8268 0.1240 1.0743 0.046 Uiso 1 1 calc R . . H18C H 0.7469 0.1087 1.0011 0.046 Uiso 1 1 calc R . . C19 C 0.7796(3) 0.0438(3) 1.1926(2) 0.0340(9) Uani 1 1 d . . . H19A H 0.7479 0.0452 1.2304 0.051 Uiso 1 1 calc R . . H19B H 0.8283 0.0822 1.2130 0.051 Uiso 1 1 calc R . . H19C H 0.7954 -0.0208 1.1857 0.051 Uiso 1 1 calc R . . C20 C 0.6576(3) 0.0152(3) 1.0745(3) 0.0378(10) Uani 1 1 d . . . H20A H 0.6791 -0.0444 1.0621 0.057 Uiso 1 1 calc R . . H20B H 0.6218 0.0424 1.0255 0.057 Uiso 1 1 calc R . . H20C H 0.6271 0.0044 1.1127 0.057 Uiso 1 1 calc R . . C21 C 0.5989(2) 0.2020(3) 1.1571(2) 0.0280(8) Uani 1 1 d . . . C22 C 0.6115(3) 0.1418(3) 1.2326(2) 0.0366(10) Uani 1 1 d . . . H22A H 0.5646 0.1484 1.2527 0.055 Uiso 1 1 calc R . . H22B H 0.6603 0.1625 1.2736 0.055 Uiso 1 1 calc R . . H22C H 0.6175 0.0760 1.2196 0.055 Uiso 1 1 calc R . . C23 C 0.5250(2) 0.1655(3) 1.0921(3) 0.0379(10) Uani 1 1 d . . . H23A H 0.4764 0.1741 1.1091 0.057 Uiso 1 1 calc R . . H23B H 0.5322 0.0988 1.0831 0.057 Uiso 1 1 calc R . . H23C H 0.5191 0.2001 1.0425 0.057 Uiso 1 1 calc R . . C24 C 0.5773(3) 0.3036(3) 1.1747(3) 0.0361(10) Uani 1 1 d . . . H24A H 0.5707 0.3423 1.1271 0.054 Uiso 1 1 calc R . . H24B H 0.6208 0.3292 1.2190 0.054 Uiso 1 1 calc R . . H24C H 0.5267 0.3034 1.1890 0.054 Uiso 1 1 calc R . . C25 C 0.7447(3) 0.6718(3) 1.0294(3) 0.0345(9) Uani 1 1 d . . . H25A H 0.7938 0.7111 1.0482 0.041 Uiso 1 1 calc R . . H25B H 0.7408 0.6319 1.0742 0.041 Uiso 1 1 calc R . . C26 C 0.6703(3) 0.7332(3) 1.0011(3) 0.0424(11) Uani 1 1 d . . . H26A H 0.6746 0.7723 0.9567 0.064 Uiso 1 1 calc R . . H26B H 0.6662 0.7732 1.0450 0.064 Uiso 1 1 calc R . . H26C H 0.6220 0.6937 0.9832 0.064 Uiso 1 1 calc R . . C27 C 0.5546(3) 0.0093(4) 0.4143(3) 0.0480(12) Uani 1 1 d . . . H27A H 0.5111 -0.0362 0.4128 0.058 Uiso 1 1 calc R . . H27B H 0.5767 -0.0043 0.3695 0.058 Uiso 1 1 calc R . . C28 C 0.5228(3) 0.1062(4) 0.4081(3) 0.0515(13) Uani 1 1 d . . . H28A H 0.5018 0.1189 0.4531 0.077 Uiso 1 1 calc R . . H28B H 0.4791 0.1132 0.3580 0.077 Uiso 1 1 calc R . . H28C H 0.5663 0.1504 0.4090 0.077 Uiso 1 1 calc R . . N11 N 0.79621(19) 0.2848(2) 0.93354(19) 0.0261(7) Uani 1 1 d . . . N21 N 0.5172(2) 0.1427(2) 0.8343(2) 0.0315(8) Uani 1 1 d . . . N31 N 0.45345(19) 0.4015(2) 0.90417(19) 0.0265(7) Uani 1 1 d . . . O1 O 0.63897(15) 0.38267(17) 0.78726(14) 0.0232(5) Uani 1 1 d . . . O2 O 0.66094(14) 0.24438(17) 1.03384(14) 0.0220(5) Uani 1 1 d . . . O5 O 0.74941(17) 0.6147(2) 0.96383(17) 0.0363(7) Uani 1 1 d . . . H5 H 0.7911 0.5812 0.9781 0.054 Uiso 1 1 calc R . . O6 O 0.61704(19) 0.0033(2) 0.4886(2) 0.0513(9) Uani 1 1 d . . . H6 H 0.6408 -0.0484 0.4916 0.077 Uiso 1 1 calc R . . O11 O 0.74424(15) 0.22853(17) 0.89118(15) 0.0246(5) Uani 1 1 d . . . O12 O 0.76872(15) 0.35666(18) 0.96122(15) 0.0255(6) Uani 1 1 d . . . O13 O 0.86892(16) 0.2732(2) 0.94721(19) 0.0391(7) Uani 1 1 d . . . O21 O 0.5594(2) 0.1878(2) 0.7990(2) 0.0466(8) Uani 1 1 d . . . O22 O 0.5167(3) 0.1741(3) 0.9003(2) 0.0638(12) Uani 1 1 d . . . O23 O 0.4785(2) 0.0735(2) 0.8049(2) 0.0464(8) Uani 1 1 d . . . O31 O 0.46898(16) 0.3801(2) 0.83958(15) 0.0332(6) Uani 1 1 d . . . O32 O 0.50414(15) 0.37709(19) 0.96936(15) 0.0281(6) Uani 1 1 d . . . O33 O 0.39184(16) 0.4447(2) 0.90308(17) 0.0336(6) Uani 1 1 d . . . O41 O 0.63148(17) 0.48481(19) 0.94995(17) 0.0303(6) Uani 1 1 d D . . P1 P 0.65013(6) 0.42160(6) 0.71048(5) 0.01969(19) Uani 1 1 d . . . P2 P 0.68871(6) 0.20401(6) 1.11775(5) 0.0207(2) Uani 1 1 d . . . La1 La 0.615056(12) 0.315778(14) 0.904733(12) 0.01947(8) Uani 1 1 d . . . H41 H 0.6677(19) 0.524(2) 0.948(2) 0.029 Uiso 1 1 d D . . H42 H 0.614(2) 0.503(3) 0.9871(19) 0.029 Uiso 1 1 d 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 C1 0.0256(19) 0.0238(18) 0.0231(18) 0.0046(15) 0.0098(15) -0.0031(15) C2 0.029(2) 0.036(2) 0.035(2) 0.0128(19) 0.0145(18) -0.0032(18) C3 0.027(2) 0.033(2) 0.027(2) 0.0027(17) 0.0077(16) 0.0032(17) C4 0.026(2) 0.027(2) 0.031(2) 0.0003(16) 0.0044(16) -0.0025(16) C5 0.029(2) 0.0248(19) 0.0211(18) -0.0030(15) 0.0104(16) -0.0033(16) C6 0.039(2) 0.0224(19) 0.029(2) -0.0025(16) 0.0144(18) -0.0001(17) C7 0.029(2) 0.030(2) 0.031(2) -0.0067(17) 0.0115(17) -0.0076(17) C8 0.035(2) 0.036(2) 0.0219(19) -0.0008(16) 0.0150(17) -0.0001(18) C9 0.0261(19) 0.0214(18) 0.0262(19) 0.0034(15) 0.0085(16) 0.0014(15) C10 0.038(2) 0.0221(19) 0.034(2) 0.0002(17) 0.0094(18) 0.0048(17) C11 0.033(2) 0.030(2) 0.040(2) 0.0015(18) 0.0192(19) 0.0072(18) C12 0.033(2) 0.027(2) 0.032(2) 0.0075(17) 0.0094(17) 0.0020(17) C13 0.028(2) 0.0261(19) 0.0211(18) -0.0008(15) 0.0077(16) -0.0006(16) C14 0.043(2) 0.0233(19) 0.028(2) -0.0040(16) 0.0133(18) -0.0011(18) C15 0.027(2) 0.035(2) 0.0241(19) 0.0006(17) 0.0082(16) -0.0006(17) C16 0.036(2) 0.037(2) 0.0209(19) -0.0025(17) 0.0105(17) 0.0002(19) C17 0.036(2) 0.0220(18) 0.0257(19) 0.0024(15) 0.0140(17) 0.0017(16) C18 0.043(2) 0.0236(19) 0.029(2) -0.0006(16) 0.0152(18) 0.0079(18) C19 0.044(2) 0.031(2) 0.031(2) 0.0087(17) 0.0164(19) 0.0119(19) C20 0.049(3) 0.027(2) 0.040(2) 0.0007(18) 0.017(2) -0.0028(19) C21 0.026(2) 0.038(2) 0.0246(19) 0.0010(16) 0.0139(16) -0.0002(17) C22 0.036(2) 0.052(3) 0.026(2) 0.0047(19) 0.0156(18) -0.004(2) C23 0.027(2) 0.057(3) 0.031(2) 0.006(2) 0.0107(18) -0.003(2) C24 0.030(2) 0.047(3) 0.036(2) -0.0025(19) 0.0172(19) 0.0083(19) C25 0.033(2) 0.039(2) 0.033(2) -0.0038(18) 0.0136(18) -0.0063(19) C26 0.047(3) 0.037(2) 0.049(3) -0.001(2) 0.022(2) 0.000(2) C27 0.047(3) 0.053(3) 0.039(3) 0.000(2) 0.005(2) -0.004(2) C28 0.040(3) 0.067(3) 0.049(3) 0.017(3) 0.015(2) 0.004(2) N11 0.0267(18) 0.0281(16) 0.0258(16) 0.0051(14) 0.0113(14) 0.0046(14) N21 0.0326(19) 0.0301(18) 0.0301(18) 0.0025(15) 0.0067(15) -0.0067(15) N31 0.0256(17) 0.0316(18) 0.0258(17) 0.0034(14) 0.0128(14) 0.0009(14) O1 0.0289(14) 0.0234(13) 0.0204(12) 0.0021(10) 0.0121(11) 0.0005(11) O2 0.0230(13) 0.0235(13) 0.0214(12) 0.0023(10) 0.0096(10) 0.0004(10) O5 0.0350(16) 0.0421(17) 0.0350(16) -0.0056(13) 0.0154(13) -0.0007(14) O6 0.0383(18) 0.0446(19) 0.065(2) 0.0092(17) 0.0060(17) 0.0058(15) O11 0.0270(14) 0.0244(13) 0.0248(13) -0.0028(11) 0.0113(11) 0.0006(11) O12 0.0273(14) 0.0254(13) 0.0257(13) -0.0011(11) 0.0110(11) 0.0009(11) O13 0.0219(15) 0.0454(18) 0.0506(19) -0.0004(15) 0.0116(13) 0.0054(13) O21 0.058(2) 0.0410(18) 0.055(2) -0.0185(15) 0.0384(18) -0.0227(15) O22 0.091(3) 0.077(3) 0.0299(17) -0.0130(17) 0.0272(18) -0.059(2) O23 0.051(2) 0.0342(17) 0.051(2) -0.0025(15) 0.0094(16) -0.0211(15) O31 0.0295(15) 0.0522(18) 0.0211(13) 0.0031(13) 0.0125(12) 0.0099(13) O32 0.0252(14) 0.0393(16) 0.0220(13) 0.0042(12) 0.0103(11) 0.0027(12) O33 0.0288(15) 0.0375(16) 0.0399(16) 0.0048(13) 0.0186(13) 0.0108(13) O41 0.0351(16) 0.0272(14) 0.0351(16) -0.0052(12) 0.0202(13) -0.0019(12) P1 0.0236(5) 0.0196(4) 0.0182(4) 0.0023(3) 0.0097(4) -0.0001(4) P2 0.0242(5) 0.0226(5) 0.0173(4) 0.0014(3) 0.0093(4) 0.0013(4) La1 0.02064(12) 0.02229(12) 0.01757(11) 0.00204(8) 0.00888(8) 0.00058(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.539(5) . ? C1 C3 1.540(5) . ? C1 C4 1.545(5) . ? C1 P1 1.874(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.525(5) . ? C5 C6 1.547(5) . ? C5 C8 1.551(5) . ? C5 P1 1.881(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C12 1.529(5) . ? C9 C10 1.538(5) . ? C9 C11 1.558(5) . ? C9 P1 1.880(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C16 1.542(5) . ? C13 C15 1.544(5) . ? C13 C14 1.550(5) . ? C13 P2 1.878(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C20 1.542(6) . ? C17 C18 1.542(5) . ? C17 C19 1.548(5) . ? C17 P2 1.876(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.532(6) . ? C21 C22 1.541(5) . ? C21 C24 1.554(6) . ? C21 P2 1.881(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 O5 1.433(5) . ? C25 C26 1.515(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 O6 1.429(6) . ? C27 C28 1.483(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? N11 O13 1.221(4) . ? N11 O11 1.270(4) . ? N11 O12 1.286(4) . ? N11 La1 3.058(3) . ? N21 O23 1.220(4) . ? N21 O22 1.245(5) . ? N21 O21 1.267(4) . ? N21 La1 3.047(3) . ? N31 O33 1.227(4) . ? N31 O32 1.268(4) . ? N31 O31 1.278(4) . ? N31 La1 3.053(3) . ? O1 P1 1.523(2) . ? O1 La1 2.418(2) . ? O2 P2 1.521(3) . ? O2 La1 2.396(2) . ? O5 H5 0.8400 . ? O6 H6 0.8400 . ? O11 La1 2.633(2) . ? O12 La1 2.616(3) . ? O21 La1 2.582(3) . ? O22 La1 2.633(3) . ? O31 La1 2.615(3) . ? O32 La1 2.653(2) . ? O41 La1 2.533(3) . ? O41 H41 0.846(18) . ? O41 H42 0.841(18) . ? 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 C2 C1 C3 108.0(3) . . ? C2 C1 C4 109.2(3) . . ? C3 C1 C4 106.2(3) . . ? C2 C1 P1 114.1(3) . . ? C3 C1 P1 110.1(3) . . ? C4 C1 P1 108.9(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C7 C5 C6 106.4(3) . . ? C7 C5 C8 109.1(3) . . ? C6 C5 C8 108.0(3) . . ? C7 C5 P1 109.5(3) . . ? C6 C5 P1 109.5(3) . . ? C8 C5 P1 114.0(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C12 C9 C10 108.7(3) . . ? C12 C9 C11 109.3(3) . . ? C10 C9 C11 105.3(3) . . ? C12 C9 P1 114.0(3) . . ? C10 C9 P1 110.9(3) . . ? C11 C9 P1 108.2(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C13 C15 107.4(3) . . ? C16 C13 C14 110.5(3) . . ? C15 C13 C14 104.9(3) . . ? C16 C13 P2 114.6(3) . . ? C15 C13 P2 111.1(3) . . ? C14 C13 P2 107.9(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C17 C18 105.6(3) . . ? C20 C17 C19 109.1(3) . . ? C18 C17 C19 109.2(3) . . ? C20 C17 P2 110.4(3) . . ? C18 C17 P2 108.8(2) . . ? C19 C17 P2 113.4(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 C22 108.9(3) . . ? C23 C21 C24 105.7(3) . . ? C22 C21 C24 109.5(3) . . ? C23 C21 P2 109.3(3) . . ? C22 C21 P2 113.8(3) . . ? C24 C21 P2 109.4(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O5 C25 C26 108.2(4) . . ? O5 C25 H25A 110.1 . . ? C26 C25 H25A 110.1 . . ? O5 C25 H25B 110.1 . . ? C26 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O6 C27 C28 106.7(4) . . ? O6 C27 H27A 110.4 . . ? C28 C27 H27A 110.4 . . ? O6 C27 H27B 110.4 . . ? C28 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O13 N11 O11 122.6(3) . . ? O13 N11 O12 120.7(3) . . ? O11 N11 O12 116.7(3) . . ? O13 N11 La1 178.2(3) . . ? O11 N11 La1 58.73(16) . . ? O12 N11 La1 58.03(16) . . ? O23 N21 O22 122.2(3) . . ? O23 N21 O21 121.9(4) . . ? O22 N21 O21 115.9(3) . . ? O23 N21 La1 178.8(3) . . ? O22 N21 La1 59.07(19) . . ? O21 N21 La1 56.85(19) . . ? O33 N31 O32 121.3(3) . . ? O33 N31 O31 121.2(3) . . ? O32 N31 O31 117.6(3) . . ? O33 N31 La1 173.5(2) . . ? O32 N31 La1 59.82(16) . . ? O31 N31 La1 58.17(17) . . ? P1 O1 La1 176.83(16) . . ? P2 O2 La1 176.80(15) . . ? C25 O5 H5 109.5 . . ? C27 O6 H6 109.5 . . ? N11 O11 La1 96.91(19) . . ? N11 O12 La1 97.3(2) . . ? N21 O21 La1 98.9(2) . . ? N21 O22 La1 97.0(2) . . ? N31 O31 La1 97.3(2) . . ? N31 O32 La1 95.78(19) . . ? La1 O41 H41 129(2) . . ? La1 O41 H42 120(3) . . ? H41 O41 H42 106(3) . . ? O1 P1 C1 108.50(15) . . ? O1 P1 C9 107.49(15) . . ? C1 P1 C9 110.95(17) . . ? O1 P1 C5 107.67(15) . . ? C1 P1 C5 110.92(17) . . ? C9 P1 C5 111.15(17) . . ? O2 P2 C17 107.87(15) . . ? O2 P2 C13 107.73(16) . . ? C17 P2 C13 111.02(18) . . ? O2 P2 C21 107.65(16) . . ? C17 P2 C21 111.33(17) . . ? C13 P2 C21 111.06(17) . . ? O2 La1 O1 151.96(8) . . ? O2 La1 O41 97.77(9) . . ? O1 La1 O41 81.84(9) . . ? O2 La1 O21 109.06(10) . . ? O1 La1 O21 77.81(9) . . ? O41 La1 O21 152.25(11) . . ? O2 La1 O31 124.76(8) . . ? O1 La1 O31 82.87(8) . . ? O41 La1 O31 78.79(9) . . ? O21 La1 O31 80.13(10) . . ? O2 La1 O12 73.85(8) . . ? O1 La1 O12 79.79(8) . . ? O41 La1 O12 70.18(8) . . ? O21 La1 O12 123.49(9) . . ? O31 La1 O12 146.18(9) . . ? O2 La1 O22 74.37(10) . . ? O1 La1 O22 123.50(9) . . ? O41 La1 O22 139.00(11) . . ? O21 La1 O22 48.17(10) . . ? O31 La1 O22 73.98(12) . . ? O12 La1 O22 139.45(12) . . ? O2 La1 O11 80.28(8) . . ? O1 La1 O11 75.25(8) . . ? O41 La1 O11 117.44(8) . . ? O21 La1 O11 75.23(9) . . ? O31 La1 O11 149.86(8) . . ? O12 La1 O11 49.00(8) . . ? O22 La1 O11 101.11(11) . . ? O2 La1 O32 79.37(8) . . ? O1 La1 O32 124.25(8) . . ? O41 La1 O32 65.10(8) . . ? O21 La1 O32 112.26(9) . . ? O31 La1 O32 48.82(8) . . ? O12 La1 O32 123.25(8) . . ? O22 La1 O32 73.90(11) . . ? O11 La1 O32 159.64(8) . . ? O2 La1 N21 91.51(9) . . ? O1 La1 N21 100.99(9) . . ? O41 La1 N21 154.06(9) . . ? O21 La1 N21 24.25(9) . . ? O31 La1 N21 76.03(10) . . ? O12 La1 N21 135.76(9) . . ? O22 La1 N21 23.92(9) . . ? O11 La1 N21 87.93(9) . . ? O32 La1 N21 93.19(9) . . ? O2 La1 N31 102.76(8) . . ? O1 La1 N31 103.12(8) . . ? O41 La1 N31 68.62(9) . . ? O21 La1 N31 97.83(10) . . ? O31 La1 N31 24.52(8) . . ? O12 La1 N31 137.74(8) . . ? O22 La1 N31 73.99(12) . . ? O11 La1 N31 173.04(8) . . ? O32 La1 N31 24.40(8) . . ? N21 La1 N31 85.74(9) . . ? O2 La1 N11 75.26(8) . . ? O1 La1 N11 76.80(8) . . ? O41 La1 N11 94.12(9) . . ? O21 La1 N11 99.33(10) . . ? O31 La1 N11 159.25(8) . . ? O12 La1 N11 24.65(8) . . ? O22 La1 N11 121.11(12) . . ? O11 La1 N11 24.36(8) . . ? O32 La1 N11 144.53(8) . . ? N21 La1 N11 111.69(9) . . ? N31 La1 N11 162.39(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O6 0.84 1.89 2.727(4) 178.3 2_656 O6 H6 O12 0.84 2.05 2.838(4) 155.2 2_646 O41 H42 O33 0.841(18) 2.10(2) 2.907(4) 162(4) 3_667 O41 H41 O5 0.846(18) 1.88(2) 2.718(4) 169(4) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.774 _refine_diff_density_min -1.237 _refine_diff_density_rms 0.114 #=== End Data_Nd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Nd _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 N3 Nd O12 P2, 2(C2 H6 O)' _chemical_formula_sum 'C28 H68 N3 Nd O14 P2' _chemical_formula_weight 877.03 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' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.2988(4) _cell_length_b 14.2475(4) _cell_length_c 17.4277(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.2710(10) _cell_angle_gamma 90.00 _cell_volume 4101.64(18) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 86117 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1836 _exptl_absorpt_coefficient_mu 1.404 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8496 _exptl_absorpt_correction_T_max 0.8723 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37716 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9345 _reflns_number_gt 8108 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _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^ > 2\s(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^)+(0.0004P)^2^+9.6375P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9345 _refine_ls_number_parameters 461 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.095 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.75978(16) 0.4445(2) 0.72833(16) 0.0198(6) Uani 1 1 d . . . C2 C 0.77823(18) 0.5068(2) 0.66397(19) 0.0286(7) Uani 1 1 d . . . H2A H 0.8370 0.5130 0.6752 0.043 Uiso 1 1 calc R . . H2B H 0.7543 0.5690 0.6647 0.043 Uiso 1 1 calc R . . H2C H 0.7552 0.4782 0.6109 0.043 Uiso 1 1 calc R . . C3 C 0.80538(17) 0.3512(2) 0.73150(19) 0.0253(6) Uani 1 1 d . . . H3A H 0.7906 0.3231 0.6778 0.038 Uiso 1 1 calc R . . H3B H 0.7908 0.3082 0.7688 0.038 Uiso 1 1 calc R . . H3C H 0.8638 0.3629 0.7499 0.038 Uiso 1 1 calc R . . C4 C 0.79539(18) 0.4905(2) 0.81165(18) 0.0254(6) Uani 1 1 d . . . H4A H 0.7828 0.4515 0.8527 0.038 Uiso 1 1 calc R . . H4B H 0.7717 0.5530 0.8115 0.038 Uiso 1 1 calc R . . H4C H 0.8542 0.4961 0.8236 0.038 Uiso 1 1 calc R . . C5 C 0.61114(16) 0.33169(19) 0.63072(16) 0.0192(6) Uani 1 1 d . . . C6 C 0.64487(19) 0.2337(2) 0.66203(18) 0.0249(6) Uani 1 1 d . . . H6A H 0.6453 0.2268 0.7181 0.037 Uiso 1 1 calc R . . H6B H 0.7001 0.2274 0.6585 0.037 Uiso 1 1 calc R . . H6C H 0.6105 0.1850 0.6293 0.037 Uiso 1 1 calc R . . C7 C 0.51870(17) 0.3244(2) 0.61064(19) 0.0252(6) Uani 1 1 d . . . H7A H 0.4938 0.3827 0.5851 0.038 Uiso 1 1 calc R . . H7B H 0.5041 0.3141 0.6602 0.038 Uiso 1 1 calc R . . H7C H 0.4992 0.2716 0.5739 0.038 Uiso 1 1 calc R . . C8 C 0.63337(18) 0.3517(2) 0.55257(17) 0.0250(6) Uani 1 1 d . . . H8A H 0.6074 0.3049 0.5118 0.037 Uiso 1 1 calc R . . H8B H 0.6922 0.3482 0.5636 0.037 Uiso 1 1 calc R . . H8C H 0.6145 0.4145 0.5328 0.037 Uiso 1 1 calc R . . C9 C 0.58909(17) 0.53281(19) 0.68839(17) 0.0206(6) Uani 1 1 d . . . C10 C 0.63268(19) 0.6137(2) 0.74288(19) 0.0286(7) Uani 1 1 d . . . H10A H 0.6813 0.6314 0.7283 0.043 Uiso 1 1 calc R . . H10B H 0.6482 0.5933 0.7991 0.043 Uiso 1 1 calc R . . H10C H 0.5963 0.6679 0.7358 0.043 Uiso 1 1 calc R . . C11 C 0.50856(18) 0.5189(2) 0.7082(2) 0.0289(7) Uani 1 1 d . . . H11A H 0.4752 0.5754 0.6931 0.043 Uiso 1 1 calc R . . H11B H 0.5198 0.5074 0.7659 0.043 Uiso 1 1 calc R . . H11C H 0.4796 0.4650 0.6780 0.043 Uiso 1 1 calc R . . C12 C 0.57138(19) 0.5649(2) 0.60085(18) 0.0270(6) Uani 1 1 d . . . H12A H 0.5434 0.6255 0.5938 0.041 Uiso 1 1 calc R . . H12B H 0.5370 0.5183 0.5652 0.041 Uiso 1 1 calc R . . H12C H 0.6224 0.5713 0.5877 0.041 Uiso 1 1 calc R . . C13 C 0.76987(16) 0.2845(2) 1.17915(17) 0.0205(6) Uani 1 1 d . . . C14 C 0.74631(18) 0.3869(2) 1.15349(18) 0.0252(6) Uani 1 1 d . . . H14A H 0.7898 0.4291 1.1828 0.038 Uiso 1 1 calc R . . H14B H 0.6962 0.4031 1.1657 0.038 Uiso 1 1 calc R . . H14C H 0.7381 0.3935 1.0956 0.038 Uiso 1 1 calc R . . C15 C 0.85063(17) 0.2675(2) 1.16073(18) 0.0256(6) Uani 1 1 d . . . H15A H 0.8900 0.3154 1.1879 0.038 Uiso 1 1 calc R . . H15B H 0.8418 0.2713 1.1026 0.038 Uiso 1 1 calc R . . H15C H 0.8714 0.2052 1.1800 0.038 Uiso 1 1 calc R . . C16 C 0.78583(19) 0.2736(2) 1.27014(17) 0.0273(7) Uani 1 1 d . . . H16A H 0.8010 0.2085 1.2857 0.041 Uiso 1 1 calc R . . H16B H 0.7367 0.2898 1.2843 0.041 Uiso 1 1 calc R . . H16C H 0.8300 0.3155 1.2985 0.041 Uiso 1 1 calc R . . C17 C 0.72733(18) 0.0843(2) 1.10988(18) 0.0234(6) Uani 1 1 d . . . C18 C 0.77889(19) 0.0855(2) 1.05128(18) 0.0261(6) Uani 1 1 d . . . H18A H 0.7984 0.0220 1.0461 0.039 Uiso 1 1 calc R . . H18B H 0.8252 0.1276 1.0720 0.039 Uiso 1 1 calc R . . H18C H 0.7458 0.1078 0.9985 0.039 Uiso 1 1 calc R . . C19 C 0.7790(2) 0.0456(2) 1.19174(18) 0.0297(7) Uani 1 1 d . . . H19A H 0.7475 0.0474 1.2300 0.045 Uiso 1 1 calc R . . H19B H 0.8278 0.0841 1.2120 0.045 Uiso 1 1 calc R . . H19C H 0.7946 -0.0194 1.1851 0.045 Uiso 1 1 calc R . . C20 C 0.6575(2) 0.0158(2) 1.0741(2) 0.0328(7) Uani 1 1 d . . . H20A H 0.6794 -0.0440 1.0621 0.049 Uiso 1 1 calc R . . H20B H 0.6213 0.0423 1.0245 0.049 Uiso 1 1 calc R . . H20C H 0.6272 0.0054 1.1127 0.049 Uiso 1 1 calc R . . C21 C 0.59846(17) 0.2029(2) 1.15688(17) 0.0237(6) Uani 1 1 d . . . C22 C 0.6111(2) 0.1427(3) 1.23288(19) 0.0335(8) Uani 1 1 d . . . H22A H 0.5641 0.1491 1.2529 0.050 Uiso 1 1 calc R . . H22B H 0.6599 0.1639 1.2742 0.050 Uiso 1 1 calc R . . H22C H 0.6175 0.0768 1.2200 0.050 Uiso 1 1 calc R . . C23 C 0.52407(18) 0.1657(3) 1.09135(19) 0.0322(7) Uani 1 1 d . . . H23A H 0.4759 0.1720 1.1095 0.048 Uiso 1 1 calc R . . H23B H 0.5323 0.0995 1.0809 0.048 Uiso 1 1 calc R . . H23C H 0.5166 0.2020 1.0419 0.048 Uiso 1 1 calc R . . C24 C 0.57655(19) 0.3040(2) 1.1746(2) 0.0326(7) Uani 1 1 d . . . H24A H 0.5691 0.3429 1.1266 0.049 Uiso 1 1 calc R . . H24B H 0.6203 0.3301 1.2189 0.049 Uiso 1 1 calc R . . H24C H 0.5263 0.3033 1.1897 0.049 Uiso 1 1 calc R . . C25 C 0.74422(18) 0.6698(2) 1.02930(19) 0.0288(7) Uani 1 1 d . . . H25A H 0.7937 0.7087 1.0479 0.035 Uiso 1 1 calc R . . H25B H 0.7398 0.6311 1.0750 0.035 Uiso 1 1 calc R . . C26 C 0.6710(2) 0.7316(2) 0.9999(2) 0.0345(8) Uani 1 1 d . . . H26A H 0.6770 0.7717 0.9563 0.052 Uiso 1 1 calc R . . H26B H 0.6658 0.7710 1.0442 0.052 Uiso 1 1 calc R . . H26C H 0.6225 0.6926 0.9801 0.052 Uiso 1 1 calc R . . C27 C 0.5527(2) 0.0091(3) 0.4136(2) 0.0439(9) Uani 1 1 d . . . H27A H 0.5088 -0.0360 0.4126 0.053 Uiso 1 1 calc R . . H27B H 0.5731 -0.0044 0.3673 0.053 Uiso 1 1 calc R . . C28 C 0.5217(2) 0.1074(3) 0.4089(2) 0.0464(10) Uani 1 1 d . . . H28A H 0.5022 0.1200 0.4553 0.070 Uiso 1 1 calc R . . H28B H 0.4770 0.1154 0.3593 0.070 Uiso 1 1 calc R . . H28C H 0.5654 0.1512 0.4091 0.070 Uiso 1 1 calc R . . N11 N 0.79168(14) 0.28423(17) 0.93251(14) 0.0208(5) Uani 1 1 d . . . N21 N 0.51898(15) 0.14549(18) 0.83507(15) 0.0261(6) Uani 1 1 d . . . N31 N 0.45573(14) 0.39830(17) 0.90410(15) 0.0216(5) Uani 1 1 d . . . O1 O 0.63814(11) 0.38235(13) 0.78932(11) 0.0186(4) Uani 1 1 d . . . O2 O 0.65976(11) 0.24633(13) 1.03236(11) 0.0188(4) Uani 1 1 d . . . O5 O 0.74902(13) 0.61044(17) 0.96448(13) 0.0307(5) Uani 1 1 d . . . H5 H 0.7921 0.5792 0.9788 0.046 Uiso 1 1 calc R . . O6 O 0.61618(15) 0.00071(18) 0.48661(16) 0.0443(6) Uani 1 1 d . . . H6 H 0.6384 -0.0520 0.4885 0.066 Uiso 1 1 calc R . . O11 O 0.73888(12) 0.22810(14) 0.89025(12) 0.0215(4) Uani 1 1 d . . . O12 O 0.76474(11) 0.35590(14) 0.96015(12) 0.0209(4) Uani 1 1 d . . . O13 O 0.86437(12) 0.27133(17) 0.94630(14) 0.0337(5) Uani 1 1 d . . . O21 O 0.55940(15) 0.19222(17) 0.79854(15) 0.0380(6) Uani 1 1 d . . . O22 O 0.52062(18) 0.17553(19) 0.90264(14) 0.0509(8) Uani 1 1 d . . . O23 O 0.48051(15) 0.07607(16) 0.80491(15) 0.0392(6) Uani 1 1 d . . . O31 O 0.47140(12) 0.37660(16) 0.83979(12) 0.0263(5) Uani 1 1 d . . . O32 O 0.50676(11) 0.37386(15) 0.96989(12) 0.0235(4) Uani 1 1 d . . . O33 O 0.39403(12) 0.44210(16) 0.90303(13) 0.0285(5) Uani 1 1 d . . . O41 O 0.62978(12) 0.48148(15) 0.94925(13) 0.0243(4) Uani 1 1 d D . . P1 P 0.64935(4) 0.42137(5) 0.71217(4) 0.01571(14) Uani 1 1 d . . . P2 P 0.68775(4) 0.20551(5) 1.11659(4) 0.01700(14) Uani 1 1 d . . . Nd1 Nd 0.614392(8) 0.315717(10) 0.904800(8) 0.01530(5) Uani 1 1 d . . . H41 H 0.6710(14) 0.515(2) 0.9535(18) 0.023 Uiso 1 1 d D . . H42 H 0.6087(16) 0.499(2) 0.9836(16) 0.023 Uiso 1 1 d 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 C1 0.0201(13) 0.0191(14) 0.0178(13) 0.0043(11) 0.0021(11) -0.0008(11) C2 0.0221(14) 0.0342(17) 0.0289(17) 0.0081(14) 0.0067(12) -0.0053(13) C3 0.0213(14) 0.0274(16) 0.0255(16) 0.0012(13) 0.0043(12) 0.0026(12) C4 0.0248(14) 0.0217(15) 0.0239(15) -0.0002(12) -0.0017(12) -0.0019(12) C5 0.0214(13) 0.0194(14) 0.0160(13) -0.0025(11) 0.0044(11) -0.0010(11) C6 0.0316(16) 0.0190(14) 0.0242(15) -0.0021(12) 0.0085(12) -0.0007(12) C7 0.0208(14) 0.0243(15) 0.0291(16) -0.0035(13) 0.0050(12) -0.0046(12) C8 0.0265(15) 0.0311(16) 0.0175(14) -0.0024(12) 0.0068(12) 0.0007(13) C9 0.0230(13) 0.0170(13) 0.0205(14) 0.0020(11) 0.0042(11) 0.0009(11) C10 0.0313(16) 0.0192(15) 0.0313(17) -0.0005(13) 0.0032(13) 0.0025(12) C11 0.0298(16) 0.0217(15) 0.0381(19) 0.0014(13) 0.0144(14) 0.0058(12) C12 0.0297(15) 0.0255(16) 0.0231(15) 0.0064(12) 0.0036(12) 0.0029(13) C13 0.0197(13) 0.0239(14) 0.0161(13) -0.0014(11) 0.0028(11) 0.0033(11) C14 0.0310(16) 0.0190(14) 0.0230(15) -0.0033(12) 0.0043(12) -0.0006(12) C15 0.0222(14) 0.0300(17) 0.0224(15) -0.0019(13) 0.0034(12) 0.0000(12) C16 0.0288(15) 0.0357(17) 0.0146(14) -0.0035(12) 0.0022(12) 0.0012(13) C17 0.0307(15) 0.0166(14) 0.0216(15) 0.0034(11) 0.0058(12) 0.0037(12) C18 0.0358(16) 0.0218(15) 0.0218(15) 0.0006(12) 0.0103(13) 0.0082(13) C19 0.0383(17) 0.0267(16) 0.0229(16) 0.0072(13) 0.0073(13) 0.0094(14) C20 0.0432(19) 0.0207(15) 0.0335(18) -0.0024(13) 0.0101(15) -0.0029(14) C21 0.0230(14) 0.0308(16) 0.0183(14) 0.0046(12) 0.0074(11) 0.0016(12) C22 0.0325(17) 0.048(2) 0.0225(16) 0.0093(15) 0.0112(13) -0.0020(15) C23 0.0213(14) 0.048(2) 0.0272(17) 0.0051(15) 0.0074(13) -0.0005(14) C24 0.0274(16) 0.043(2) 0.0295(17) -0.0022(15) 0.0117(13) 0.0109(14) C25 0.0266(15) 0.0342(18) 0.0259(16) -0.0044(13) 0.0081(13) -0.0052(13) C26 0.0367(18) 0.0297(18) 0.0386(19) 0.0012(15) 0.0133(15) 0.0007(14) C27 0.047(2) 0.044(2) 0.0320(19) 0.0019(17) -0.0008(16) -0.0041(18) C28 0.0311(18) 0.054(2) 0.049(2) 0.0160(19) 0.0049(17) 0.0060(17) N11 0.0198(11) 0.0231(12) 0.0188(12) 0.0046(10) 0.0048(9) 0.0020(10) N21 0.0252(13) 0.0226(13) 0.0250(14) 0.0015(11) -0.0012(10) -0.0047(10) N31 0.0175(11) 0.0246(13) 0.0232(13) 0.0026(10) 0.0066(10) 0.0013(10) O1 0.0214(9) 0.0182(9) 0.0159(9) 0.0020(8) 0.0048(8) 0.0004(8) O2 0.0199(9) 0.0205(10) 0.0143(9) 0.0021(8) 0.0025(7) 0.0011(8) O5 0.0228(11) 0.0398(13) 0.0290(12) -0.0061(10) 0.0071(9) 0.0012(10) O6 0.0315(13) 0.0354(14) 0.0549(17) 0.0086(12) -0.0041(12) 0.0030(11) O11 0.0231(10) 0.0213(10) 0.0193(10) -0.0012(8) 0.0052(8) 0.0015(8) O12 0.0211(10) 0.0216(10) 0.0197(10) -0.0007(8) 0.0056(8) 0.0007(8) O13 0.0169(10) 0.0432(14) 0.0390(13) 0.0016(11) 0.0053(9) 0.0058(9) O21 0.0452(14) 0.0346(13) 0.0434(14) -0.0147(11) 0.0273(12) -0.0191(11) O22 0.0769(19) 0.0567(17) 0.0210(12) -0.0093(12) 0.0172(13) -0.0412(15) O23 0.0435(14) 0.0276(12) 0.0402(14) -0.0035(10) 0.0028(11) -0.0185(11) O31 0.0209(10) 0.0406(13) 0.0173(10) 0.0001(9) 0.0056(8) 0.0042(9) O32 0.0196(9) 0.0296(11) 0.0196(10) 0.0042(9) 0.0029(8) 0.0018(8) O33 0.0214(10) 0.0342(12) 0.0314(12) 0.0031(10) 0.0100(9) 0.0092(9) O41 0.0229(10) 0.0229(11) 0.0297(12) -0.0033(9) 0.0117(9) -0.0006(8) P1 0.0175(3) 0.0148(3) 0.0140(3) 0.0018(3) 0.0035(3) -0.0001(3) P2 0.0178(3) 0.0195(3) 0.0129(3) 0.0022(3) 0.0034(3) 0.0021(3) Nd1 0.01472(7) 0.01709(8) 0.01319(7) 0.00148(6) 0.00277(5) 0.00015(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.537(4) . ? C1 C3 1.538(4) . ? C1 C4 1.545(4) . ? C1 P1 1.876(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.536(4) . ? C5 C8 1.548(4) . ? C5 C6 1.548(4) . ? C5 P1 1.878(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C12 1.534(4) . ? C9 C10 1.541(4) . ? C9 C11 1.544(4) . ? C9 P1 1.877(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C16 1.535(4) . ? C13 C15 1.543(4) . ? C13 C14 1.545(4) . ? C13 P2 1.885(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C20 1.534(4) . ? C17 C18 1.542(4) . ? C17 C19 1.543(4) . ? C17 P2 1.874(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.538(4) . ? C21 C23 1.539(4) . ? C21 C24 1.545(4) . ? C21 P2 1.877(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 O5 1.433(4) . ? C25 C26 1.503(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 O6 1.418(4) . ? C27 C28 1.494(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? N11 O13 1.222(3) . ? N11 O11 1.272(3) . ? N11 O12 1.275(3) . ? N11 Nd1 2.994(2) . ? N21 O23 1.220(3) . ? N21 O22 1.245(3) . ? N21 O21 1.266(3) . ? N21 Nd1 2.982(2) . ? N31 O33 1.232(3) . ? N31 O31 1.267(3) . ? N31 O32 1.270(3) . ? N31 Nd1 2.983(2) . ? O1 P1 1.520(2) . ? O1 Nd1 2.3688(18) . ? O2 P2 1.5184(19) . ? O2 Nd1 2.3451(18) . ? O5 H5 0.8400 . ? O6 H6 0.8400 . ? O11 Nd1 2.5660(19) . ? O12 Nd1 2.5559(19) . ? O21 Nd1 2.527(2) . ? O22 Nd1 2.566(2) . ? O31 Nd1 2.548(2) . ? O32 Nd1 2.587(2) . ? O41 Nd1 2.475(2) . ? O41 H41 0.839(17) . ? O41 H42 0.825(17) . ? 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 C2 C1 C3 108.1(2) . . ? C2 C1 C4 109.2(2) . . ? C3 C1 C4 106.0(2) . . ? C2 C1 P1 114.52(19) . . ? C3 C1 P1 110.03(19) . . ? C4 C1 P1 108.6(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C7 C5 C8 109.0(2) . . ? C7 C5 C6 106.1(2) . . ? C8 C5 C6 108.1(2) . . ? C7 C5 P1 109.11(19) . . ? C8 C5 P1 114.6(2) . . ? C6 C5 P1 109.61(19) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C12 C9 C10 107.9(2) . . ? C12 C9 C11 109.5(2) . . ? C10 C9 C11 105.5(2) . . ? C12 C9 P1 113.9(2) . . ? C10 C9 P1 111.02(19) . . ? C11 C9 P1 108.70(19) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C13 C15 107.6(2) . . ? C16 C13 C14 110.2(2) . . ? C15 C13 C14 105.4(2) . . ? C16 C13 P2 114.2(2) . . ? C15 C13 P2 111.08(19) . . ? C14 C13 P2 107.92(19) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C17 C18 106.1(3) . . ? C20 C17 C19 108.6(3) . . ? C18 C17 C19 109.0(2) . . ? C20 C17 P2 110.7(2) . . ? C18 C17 P2 109.0(2) . . ? C19 C17 P2 113.2(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C23 108.7(3) . . ? C22 C21 C24 109.1(3) . . ? C23 C21 C24 105.6(3) . . ? C22 C21 P2 114.2(2) . . ? C23 C21 P2 109.2(2) . . ? C24 C21 P2 109.5(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O5 C25 C26 108.5(3) . . ? O5 C25 H25A 110.0 . . ? C26 C25 H25A 110.0 . . ? O5 C25 H25B 110.0 . . ? C26 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O6 C27 C28 107.3(3) . . ? O6 C27 H27A 110.3 . . ? C28 C27 H27A 110.3 . . ? O6 C27 H27B 110.3 . . ? C28 C27 H27B 110.3 . . ? H27A C27 H27B 108.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O13 N11 O11 122.7(2) . . ? O13 N11 O12 121.1(2) . . ? O11 N11 O12 116.2(2) . . ? O13 N11 Nd1 178.04(19) . . ? O11 N11 Nd1 58.36(12) . . ? O12 N11 Nd1 57.92(12) . . ? O23 N21 O22 122.8(3) . . ? O23 N21 O21 121.5(3) . . ? O22 N21 O21 115.7(2) . . ? O23 N21 Nd1 178.5(2) . . ? O22 N21 Nd1 58.71(15) . . ? O21 N21 Nd1 57.01(14) . . ? O33 N31 O31 121.5(2) . . ? O33 N31 O32 121.3(2) . . ? O31 N31 O32 117.2(2) . . ? O33 N31 Nd1 172.76(19) . . ? O31 N31 Nd1 57.94(13) . . ? O32 N31 Nd1 59.75(13) . . ? P1 O1 Nd1 176.56(12) . . ? P2 O2 Nd1 177.27(12) . . ? C25 O5 H5 109.5 . . ? C27 O6 H6 109.5 . . ? N11 O11 Nd1 96.69(15) . . ? N11 O12 Nd1 97.08(15) . . ? N21 O21 Nd1 98.15(17) . . ? N21 O22 Nd1 96.79(17) . . ? N31 O31 Nd1 97.13(15) . . ? N31 O32 Nd1 95.15(15) . . ? Nd1 O41 H41 125(2) . . ? Nd1 O41 H42 119(2) . . ? H41 O41 H42 109(2) . . ? O1 P1 C1 108.86(11) . . ? O1 P1 C9 107.25(12) . . ? C1 P1 C9 111.02(13) . . ? O1 P1 C5 108.12(12) . . ? C1 P1 C5 110.31(13) . . ? C9 P1 C5 111.15(13) . . ? O2 P2 C17 108.06(12) . . ? O2 P2 C21 107.92(12) . . ? C17 P2 C21 111.19(14) . . ? O2 P2 C13 107.44(12) . . ? C17 P2 C13 111.08(13) . . ? C21 P2 C13 110.98(13) . . ? O2 Nd1 O1 151.73(6) . . ? O2 Nd1 O41 97.52(7) . . ? O1 Nd1 O41 81.59(7) . . ? O2 Nd1 O21 110.39(8) . . ? O1 Nd1 O21 77.23(7) . . ? O41 Nd1 O21 151.16(8) . . ? O2 Nd1 O31 124.93(6) . . ? O1 Nd1 O31 82.88(6) . . ? O41 Nd1 O31 79.30(7) . . ? O21 Nd1 O31 78.85(8) . . ? O2 Nd1 O12 73.74(6) . . ? O1 Nd1 O12 79.47(6) . . ? O41 Nd1 O12 70.45(6) . . ? O21 Nd1 O12 123.51(7) . . ? O31 Nd1 O12 146.76(7) . . ? O2 Nd1 O11 80.45(6) . . ? O1 Nd1 O11 75.45(6) . . ? O41 Nd1 O11 118.66(7) . . ? O21 Nd1 O11 74.52(7) . . ? O31 Nd1 O11 148.67(6) . . ? O12 Nd1 O11 49.95(6) . . ? O2 Nd1 O22 73.62(7) . . ? O1 Nd1 O22 124.59(7) . . ? O41 Nd1 O22 139.12(8) . . ? O21 Nd1 O22 49.34(7) . . ? O31 Nd1 O22 74.48(9) . . ? O12 Nd1 O22 138.40(8) . . ? O11 Nd1 O22 99.51(9) . . ? O2 Nd1 O32 78.54(6) . . ? O1 Nd1 O32 124.96(6) . . ? O41 Nd1 O32 65.28(7) . . ? O21 Nd1 O32 112.39(7) . . ? O31 Nd1 O32 49.90(6) . . ? O12 Nd1 O32 123.16(6) . . ? O11 Nd1 O32 158.97(6) . . ? O22 Nd1 O32 73.84(8) . . ? O2 Nd1 N21 91.86(7) . . ? O1 Nd1 N21 101.21(7) . . ? O41 Nd1 N21 153.99(7) . . ? O21 Nd1 N21 24.84(7) . . ? O31 Nd1 N21 75.45(7) . . ? O12 Nd1 N21 135.57(7) . . ? O11 Nd1 N21 86.75(7) . . ? O22 Nd1 N21 24.50(7) . . ? O32 Nd1 N21 93.20(7) . . ? O2 Nd1 N31 102.63(7) . . ? O1 Nd1 N31 103.29(6) . . ? O41 Nd1 N31 68.79(7) . . ? O21 Nd1 N31 97.24(7) . . ? O31 Nd1 N31 24.93(6) . . ? O12 Nd1 N31 138.17(6) . . ? O11 Nd1 N31 171.76(6) . . ? O22 Nd1 N31 74.34(9) . . ? O32 Nd1 N31 25.10(6) . . ? N21 Nd1 N31 85.52(7) . . ? O2 Nd1 N11 75.25(6) . . ? O1 Nd1 N11 76.66(6) . . ? O41 Nd1 N11 94.74(7) . . ? O21 Nd1 N11 99.13(7) . . ? O31 Nd1 N11 159.34(7) . . ? O12 Nd1 N11 25.00(6) . . ? O11 Nd1 N11 24.96(6) . . ? O22 Nd1 N11 119.91(9) . . ? O32 Nd1 N11 144.44(6) . . ? N21 Nd1 N11 111.13(7) . . ? N31 Nd1 N11 163.17(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O6 0.84 1.89 2.725(3) 175.2 2_656 O6 H6 O12 0.84 2.11 2.868(3) 150.5 2_646 O41 H42 O33 0.825(17) 2.16(2) 2.935(3) 156(3) 3_667 O41 H41 O5 0.839(17) 1.890(19) 2.716(3) 168(3) . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.164 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.095 #=== End data_Sm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Sm _chemical_melting_point ? _chemical_formula_moiety '2(C24 H54 N3 O11 P2 Sm), C2 H6 O' _chemical_formula_sum 'C50 H114 N6 O23 P4 Sm2' _chemical_formula_weight 1592.05 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 Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7793(3) _cell_length_b 16.6562(4) _cell_length_c 31.3629(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.2500(10) _cell_angle_gamma 90.00 _cell_volume 7186.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 58107 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 1.778 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8708 _exptl_absorpt_correction_T_max 0.9163 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48932 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16358 _reflns_number_gt 13201 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _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^ > 2\s(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^)+(0.0000P)^2^+41.1196P] 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 16358 _refine_ls_number_parameters 804 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 C1 C -0.0197(4) 0.2906(3) 0.08720(17) 0.0212(11) Uani 1 1 d . . . C2 C 0.0092(4) 0.2089(4) 0.0692(2) 0.0324(14) Uani 1 1 d . . . H2A H -0.0473 0.1843 0.0541 0.049 Uiso 1 1 calc R . . H2B H 0.0325 0.1738 0.0928 0.049 Uiso 1 1 calc R . . H2C H 0.0610 0.2164 0.0495 0.049 Uiso 1 1 calc R . . C3 C -0.0591(4) 0.3391(4) 0.04787(18) 0.0292(13) Uani 1 1 d . . . H3A H -0.0058 0.3506 0.0294 0.044 Uiso 1 1 calc R . . H3B H -0.0871 0.3897 0.0574 0.044 Uiso 1 1 calc R . . H3C H -0.1093 0.3078 0.0320 0.044 Uiso 1 1 calc R . . C4 C -0.1029(4) 0.2786(4) 0.1179(2) 0.0295(13) Uani 1 1 d . . . H4A H -0.1593 0.2549 0.1021 0.044 Uiso 1 1 calc R . . H4B H -0.1210 0.3306 0.1297 0.044 Uiso 1 1 calc R . . H4C H -0.0809 0.2426 0.1412 0.044 Uiso 1 1 calc R . . C5 C 0.0751(4) 0.4507(3) 0.11663(17) 0.0208(11) Uani 1 1 d . . . C6 C 0.0874(4) 0.4861(3) 0.07174(18) 0.0284(13) Uani 1 1 d . . . H6A H 0.0362 0.4651 0.0518 0.043 Uiso 1 1 calc R . . H6B H 0.1511 0.4710 0.0619 0.043 Uiso 1 1 calc R . . H6C H 0.0825 0.5448 0.0730 0.043 Uiso 1 1 calc R . . C7 C 0.1572(4) 0.4878(4) 0.1456(2) 0.0304(13) Uani 1 1 d . . . H7A H 0.1539 0.5464 0.1437 0.046 Uiso 1 1 calc R . . H7B H 0.2202 0.4693 0.1365 0.046 Uiso 1 1 calc R . . H7C H 0.1496 0.4712 0.1752 0.046 Uiso 1 1 calc R . . C8 C -0.0221(4) 0.4752(3) 0.13390(19) 0.0260(12) Uani 1 1 d . . . H8A H -0.0286 0.4506 0.1620 0.039 Uiso 1 1 calc R . . H8B H -0.0753 0.4569 0.1142 0.039 Uiso 1 1 calc R . . H8C H -0.0247 0.5338 0.1366 0.039 Uiso 1 1 calc R . . C9 C 0.1261(4) 0.2931(3) 0.16635(16) 0.0210(11) Uani 1 1 d . . . C10 C 0.2335(4) 0.3137(4) 0.17816(17) 0.0285(13) Uani 1 1 d . . . H10A H 0.2550 0.2851 0.2043 0.043 Uiso 1 1 calc R . . H10B H 0.2401 0.3717 0.1828 0.043 Uiso 1 1 calc R . . H10C H 0.2736 0.2973 0.1549 0.043 Uiso 1 1 calc R . . C11 C 0.0623(4) 0.3202(4) 0.20265(17) 0.0284(13) Uani 1 1 d . . . H11A H 0.0853 0.2943 0.2294 0.043 Uiso 1 1 calc R . . H11B H -0.0054 0.3048 0.1957 0.043 Uiso 1 1 calc R . . H11C H 0.0665 0.3786 0.2059 0.043 Uiso 1 1 calc R . . C12 C 0.1227(5) 0.2005(4) 0.1629(2) 0.0335(14) Uani 1 1 d . . . H12A H 0.1571 0.1833 0.1380 0.050 Uiso 1 1 calc R . . H12B H 0.0548 0.1828 0.1598 0.050 Uiso 1 1 calc R . . H12C H 0.1539 0.1768 0.1888 0.050 Uiso 1 1 calc R . . C13 C 0.4706(4) 0.3040(3) -0.08370(16) 0.0216(11) Uani 1 1 d . . . C14 C 0.3629(4) 0.2827(4) -0.09288(17) 0.0262(12) Uani 1 1 d . . . H14A H 0.3408 0.3036 -0.1210 0.039 Uiso 1 1 calc R . . H14B H 0.3241 0.3068 -0.0709 0.039 Uiso 1 1 calc R . . H14C H 0.3550 0.2243 -0.0926 0.039 Uiso 1 1 calc R . . C15 C 0.5314(5) 0.2678(4) -0.11839(17) 0.0317(14) Uani 1 1 d . . . H15A H 0.5242 0.2092 -0.1185 0.048 Uiso 1 1 calc R . . H15B H 0.5999 0.2818 -0.1126 0.048 Uiso 1 1 calc R . . H15C H 0.5089 0.2892 -0.1463 0.048 Uiso 1 1 calc R . . C16 C 0.4747(5) 0.3965(4) -0.08664(19) 0.0321(14) Uani 1 1 d . . . H16A H 0.4496 0.4137 -0.1150 0.048 Uiso 1 1 calc R . . H16B H 0.5422 0.4145 -0.0819 0.048 Uiso 1 1 calc R . . H16C H 0.4350 0.4201 -0.0649 0.048 Uiso 1 1 calc R . . C17 C 0.5274(4) 0.1591(3) -0.02625(17) 0.0223(11) Uani 1 1 d . . . C18 C 0.5220(4) 0.1307(3) 0.02049(17) 0.0263(12) Uani 1 1 d . . . H18A H 0.5177 0.0719 0.0212 0.039 Uiso 1 1 calc R . . H18B H 0.4644 0.1538 0.0327 0.039 Uiso 1 1 calc R . . H18C H 0.5805 0.1481 0.0372 0.039 Uiso 1 1 calc R . . C19 C 0.4436(5) 0.1159(3) -0.05165(19) 0.0308(13) Uani 1 1 d . . . H19A H 0.4475 0.1273 -0.0822 0.046 Uiso 1 1 calc R . . H19B H 0.3812 0.1352 -0.0421 0.046 Uiso 1 1 calc R . . H19C H 0.4488 0.0579 -0.0468 0.046 Uiso 1 1 calc R . . C20 C 0.6237(4) 0.1313(4) -0.04352(19) 0.0313(13) Uani 1 1 d . . . H20A H 0.6265 0.0725 -0.0433 0.047 Uiso 1 1 calc R . . H20B H 0.6780 0.1528 -0.0255 0.047 Uiso 1 1 calc R . . H20C H 0.6282 0.1508 -0.0728 0.047 Uiso 1 1 calc R . . C21 C 0.6165(4) 0.3271(4) -0.00555(17) 0.0244(12) Uani 1 1 d . . . C22 C 0.6993(4) 0.3348(4) -0.03626(19) 0.0327(14) Uani 1 1 d . . . H22A H 0.6755 0.3633 -0.0621 0.049 Uiso 1 1 calc R . . H22B H 0.7217 0.2812 -0.0440 0.049 Uiso 1 1 calc R . . H22C H 0.7533 0.3648 -0.0223 0.049 Uiso 1 1 calc R . . C23 C 0.5840(4) 0.4123(4) 0.0067(2) 0.0317(14) Uani 1 1 d . . . H23A H 0.6379 0.4399 0.0223 0.048 Uiso 1 1 calc R . . H23B H 0.5285 0.4086 0.0248 0.048 Uiso 1 1 calc R . . H23C H 0.5650 0.4425 -0.0193 0.048 Uiso 1 1 calc R . . C24 C 0.6552(4) 0.2867(4) 0.03626(19) 0.0343(14) Uani 1 1 d . . . H24A H 0.6869 0.2359 0.0296 0.051 Uiso 1 1 calc R . . H24B H 0.6010 0.2763 0.0544 0.051 Uiso 1 1 calc R . . H24C H 0.7023 0.3223 0.0513 0.051 Uiso 1 1 calc R . . C25 C 0.4888(4) 1.0805(4) 0.17346(17) 0.0249(12) Uani 1 1 d . . . C26 C 0.4037(4) 1.1403(4) 0.17727(19) 0.0334(14) Uani 1 1 d . . . H26A H 0.4231 1.1934 0.1672 0.050 Uiso 1 1 calc R . . H26B H 0.3871 1.1441 0.2072 0.050 Uiso 1 1 calc R . . H26C H 0.3470 1.1214 0.1598 0.050 Uiso 1 1 calc R . . C27 C 0.4513(4) 0.9952(4) 0.1816(2) 0.0342(14) Uani 1 1 d . . . H27A H 0.4217 0.9936 0.2093 0.051 Uiso 1 1 calc R . . H27B H 0.5057 0.9572 0.1818 0.051 Uiso 1 1 calc R . . H27C H 0.4027 0.9804 0.1590 0.051 Uiso 1 1 calc R . . C28 C 0.5199(4) 1.0793(4) 0.12671(18) 0.0340(15) Uani 1 1 d . . . H28A H 0.4632 1.0678 0.1074 0.051 Uiso 1 1 calc R . . H28B H 0.5693 1.0376 0.1236 0.051 Uiso 1 1 calc R . . H28C H 0.5470 1.1317 0.1196 0.051 Uiso 1 1 calc R . . C29 C 0.5790(4) 1.0705(4) 0.26551(16) 0.0242(12) Uani 1 1 d . . . C30 C 0.6577(5) 1.1071(4) 0.29669(18) 0.0369(16) Uani 1 1 d . . . H30A H 0.6528 1.0832 0.3250 0.055 Uiso 1 1 calc R . . H30B H 0.6480 1.1652 0.2985 0.055 Uiso 1 1 calc R . . H30C H 0.7221 1.0960 0.2863 0.055 Uiso 1 1 calc R . . C31 C 0.4783(4) 1.0918(4) 0.28094(17) 0.0295(13) Uani 1 1 d . . . H31A H 0.4281 1.0637 0.2633 0.044 Uiso 1 1 calc R . . H31B H 0.4679 1.1499 0.2785 0.044 Uiso 1 1 calc R . . H31C H 0.4746 1.0754 0.3108 0.044 Uiso 1 1 calc R . . C32 C 0.5953(5) 0.9800(4) 0.26751(19) 0.0346(14) Uani 1 1 d . . . H32A H 0.5908 0.9615 0.2970 0.052 Uiso 1 1 calc R . . H32B H 0.6599 0.9674 0.2578 0.052 Uiso 1 1 calc R . . H32C H 0.5457 0.9530 0.2490 0.052 Uiso 1 1 calc R . . C33 C 0.6286(4) 1.2146(3) 0.2074(2) 0.0295(13) Uani 1 1 d . . . C34 C 0.6258(5) 1.2424(4) 0.1600(2) 0.0384(15) Uani 1 1 d . . . H34A H 0.5597 1.2362 0.1471 0.058 Uiso 1 1 calc R . . H34B H 0.6708 1.2097 0.1442 0.058 Uiso 1 1 calc R . . H34C H 0.6451 1.2990 0.1587 0.058 Uiso 1 1 calc R . . C35 C 0.7360(5) 1.2247(4) 0.2234(2) 0.0400(16) Uani 1 1 d . . . H35A H 0.7558 1.2806 0.2198 0.060 Uiso 1 1 calc R . . H35B H 0.7770 1.1896 0.2070 0.060 Uiso 1 1 calc R . . H35C H 0.7433 1.2101 0.2537 0.060 Uiso 1 1 calc R . . C36 C 0.5634(5) 1.2695(4) 0.2329(3) 0.0466(18) Uani 1 1 d . . . H36A H 0.5671 1.2530 0.2630 0.070 Uiso 1 1 calc R . . H36B H 0.4960 1.2653 0.2214 0.070 Uiso 1 1 calc R . . H36C H 0.5854 1.3252 0.2308 0.070 Uiso 1 1 calc R . . C37 C 1.0282(4) 0.9115(3) 0.07295(16) 0.0215(11) Uani 1 1 d . . . C38 C 1.1222(4) 0.8882(3) 0.05248(18) 0.0270(12) Uani 1 1 d . . . H38A H 1.1207 0.9086 0.0231 0.040 Uiso 1 1 calc R . . H38B H 1.1284 0.8296 0.0522 0.040 Uiso 1 1 calc R . . H38C H 1.1778 0.9115 0.0690 0.040 Uiso 1 1 calc R . . C39 C 1.0207(4) 1.0033(3) 0.07445(17) 0.0248(12) Uani 1 1 d . . . H39A H 1.0847 1.0261 0.0824 0.037 Uiso 1 1 calc R . . H39B H 0.9747 1.0189 0.0957 0.037 Uiso 1 1 calc R . . H39C H 0.9979 1.0235 0.0463 0.037 Uiso 1 1 calc R . . C40 C 0.9404(4) 0.8815(4) 0.04450(17) 0.0289(13) Uani 1 1 d . . . H40A H 0.9414 0.9066 0.0163 0.043 Uiso 1 1 calc R . . H40B H 0.8800 0.8959 0.0577 0.043 Uiso 1 1 calc R . . H40C H 0.9441 0.8231 0.0415 0.043 Uiso 1 1 calc R . . C41 C 0.9852(4) 0.7627(3) 0.12829(17) 0.0233(11) Uani 1 1 d . . . C42 C 0.8757(4) 0.7543(4) 0.1166(2) 0.0325(14) Uani 1 1 d . . . H42A H 0.8574 0.6975 0.1172 0.049 Uiso 1 1 calc R . . H42B H 0.8611 0.7760 0.0879 0.049 Uiso 1 1 calc R . . H42C H 0.8389 0.7841 0.1373 0.049 Uiso 1 1 calc R . . C43 C 1.0423(5) 0.7125(3) 0.0968(2) 0.0316(14) Uani 1 1 d . . . H43A H 1.0244 0.6558 0.0992 0.047 Uiso 1 1 calc R . . H43B H 1.1122 0.7187 0.1036 0.047 Uiso 1 1 calc R . . H43C H 1.0266 0.7312 0.0676 0.047 Uiso 1 1 calc R . . C44 C 1.0018(5) 0.7258(4) 0.1729(2) 0.0351(14) Uani 1 1 d . . . H44A H 0.9701 0.7591 0.1938 0.053 Uiso 1 1 calc R . . H44B H 1.0717 0.7231 0.1805 0.053 Uiso 1 1 calc R . . H44C H 0.9743 0.6715 0.1730 0.053 Uiso 1 1 calc R . . C45 C 1.1304(4) 0.8917(3) 0.16313(17) 0.0234(11) Uani 1 1 d . . . C46 C 1.2160(4) 0.8353(4) 0.1550(2) 0.0321(14) Uani 1 1 d . . . H46A H 1.2305 0.8379 0.1248 0.048 Uiso 1 1 calc R . . H46B H 1.1986 0.7801 0.1623 0.048 Uiso 1 1 calc R . . H46C H 1.2734 0.8519 0.1727 0.048 Uiso 1 1 calc R . . C47 C 1.1630(4) 0.9788(4) 0.1568(2) 0.0313(13) Uani 1 1 d . . . H47A H 1.2144 0.9923 0.1785 0.047 Uiso 1 1 calc R . . H47B H 1.1076 1.0149 0.1596 0.047 Uiso 1 1 calc R . . H47C H 1.1879 0.9847 0.1283 0.047 Uiso 1 1 calc R . . C48 C 1.1056(4) 0.8847(4) 0.21049(18) 0.0311(13) Uani 1 1 d . . . H48A H 1.1602 0.9047 0.2288 0.047 Uiso 1 1 calc R . . H48B H 1.0933 0.8283 0.2173 0.047 Uiso 1 1 calc R . . H48C H 1.0474 0.9166 0.2153 0.047 Uiso 1 1 calc R . . C49 C 0.7284(7) 0.4825(6) 0.1715(4) 0.091(4) Uani 1 1 d . . . H49A H 0.7755 0.4396 0.1780 0.136 Uiso 1 1 calc R . . H49B H 0.7187 0.4884 0.1404 0.136 Uiso 1 1 calc R . . H49C H 0.6663 0.4690 0.1835 0.136 Uiso 1 1 calc R . . C50 C 0.7662(6) 0.5604(6) 0.1906(3) 0.062(2) Uani 1 1 d . . . H50A H 0.8306 0.5732 0.1799 0.075 Uiso 1 1 calc R . . H50B H 0.7210 0.6049 0.1828 0.075 Uiso 1 1 calc R . . N11 N 0.2677(3) 0.1360(3) 0.04804(17) 0.0278(11) Uani 1 1 d . . . N21 N 0.4248(3) 0.3909(3) 0.10412(14) 0.0250(10) Uani 1 1 d . . . N31 N 0.1897(4) 0.3993(3) -0.02558(15) 0.0303(11) Uani 1 1 d . . . N41 N 0.7700(4) 1.0505(3) 0.08424(16) 0.0316(11) Uani 1 1 d . . . N51 N 0.6958(4) 0.8405(3) 0.19417(15) 0.0274(11) Uani 1 1 d . . . N61 N 0.9405(4) 1.0608(3) 0.23023(16) 0.0322(12) Uani 1 1 d . . . O1 O 0.1740(2) 0.3241(2) 0.08453(11) 0.0181(7) Uani 1 1 d . . . O2 O 0.4242(2) 0.2889(2) -0.00035(11) 0.0176(7) Uani 1 1 d . . . O3 O 0.6826(2) 1.0590(2) 0.19396(11) 0.0194(8) Uani 1 1 d . . . O4 O 0.9358(2) 0.9163(2) 0.14814(11) 0.0182(7) Uani 1 1 d . . . O5 O 0.7742(5) 0.5506(6) 0.2364(2) 0.102(3) Uani 1 1 d . . . H5 H 0.8318 0.5596 0.2455 0.152 Uiso 1 1 calc R . . O11 O 0.2362(3) 0.1761(2) 0.01545(13) 0.0306(9) Uani 1 1 d . . . O12 O 0.3143(3) 0.1759(2) 0.07712(12) 0.0276(9) Uani 1 1 d . . . O13 O 0.2545(4) 0.0639(3) 0.05112(17) 0.0465(12) Uani 1 1 d . . . O21 O 0.3705(3) 0.4289(2) 0.07693(12) 0.0288(9) Uani 1 1 d . . . O22 O 0.4214(3) 0.3143(2) 0.10148(12) 0.0270(9) Uani 1 1 d . . . O23 O 0.4778(4) 0.4247(3) 0.13101(14) 0.0441(12) Uani 1 1 d . . . O31 O 0.1686(3) 0.3266(2) -0.01695(12) 0.0292(9) Uani 1 1 d . . . O32 O 0.2608(3) 0.4290(2) -0.00351(13) 0.0318(9) Uani 1 1 d . . . O33 O 0.1447(4) 0.4369(3) -0.05309(16) 0.0542(14) Uani 1 1 d . . . O41 O 0.7408(3) 0.9804(3) 0.09376(12) 0.0306(9) Uani 1 1 d . . . O42 O 0.8127(3) 1.0895(2) 0.11479(13) 0.0304(9) Uani 1 1 d . . . O43 O 0.7602(4) 1.0775(3) 0.04825(14) 0.0489(13) Uani 1 1 d . . . O51 O 0.7738(3) 0.8644(3) 0.21445(12) 0.0309(9) Uani 1 1 d . . . O52 O 0.6715(3) 0.8810(2) 0.16047(12) 0.0282(9) Uani 1 1 d . . . O53 O 0.6490(4) 0.7840(3) 0.20572(15) 0.0465(13) Uani 1 1 d . . . O61 O 0.9235(3) 1.0866(3) 0.19251(13) 0.0319(10) Uani 1 1 d . . . O62 O 0.8887(3) 1.0014(2) 0.24064(12) 0.0302(9) Uani 1 1 d . . . O63 O 1.0039(4) 1.0885(3) 0.25461(16) 0.0605(16) Uani 1 1 d . . . P1 P 0.09069(9) 0.33918(8) 0.11335(4) 0.0155(3) Uani 1 1 d . . . P2 P 0.50822(9) 0.27001(8) -0.02846(4) 0.0160(3) Uani 1 1 d . . . P3 P 0.59674(10) 1.10520(8) 0.20958(4) 0.0177(3) Uani 1 1 d . . . P4 P 1.01807(9) 0.87120(8) 0.12855(4) 0.0155(3) Uani 1 1 d . . . Sm1 Sm 0.297334(18) 0.307922(16) 0.041047(8) 0.01546(7) Uani 1 1 d . . . Sm2 Sm 0.802889(18) 0.982968(16) 0.169131(8) 0.01558(7) 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 C1 0.018(3) 0.021(3) 0.025(3) -0.002(2) 0.001(2) -0.002(2) C2 0.030(3) 0.030(3) 0.038(3) -0.013(3) 0.002(3) -0.004(3) C3 0.023(3) 0.037(3) 0.027(3) -0.002(3) -0.004(2) -0.004(2) C4 0.016(3) 0.032(3) 0.042(3) -0.006(3) 0.009(2) -0.006(2) C5 0.021(3) 0.014(2) 0.028(3) -0.005(2) 0.006(2) 0.000(2) C6 0.033(3) 0.017(3) 0.036(3) 0.004(2) 0.012(3) 0.003(2) C7 0.030(3) 0.022(3) 0.040(3) -0.008(3) 0.011(3) -0.007(2) C8 0.026(3) 0.019(3) 0.035(3) -0.003(2) 0.010(2) 0.007(2) C9 0.024(3) 0.019(3) 0.020(3) 0.003(2) 0.005(2) 0.002(2) C10 0.022(3) 0.041(4) 0.022(3) 0.004(3) -0.001(2) 0.004(3) C11 0.031(3) 0.034(3) 0.020(3) 0.003(2) 0.006(2) 0.002(3) C12 0.037(3) 0.030(3) 0.034(3) 0.006(3) 0.010(3) 0.008(3) C13 0.017(3) 0.027(3) 0.021(3) 0.002(2) 0.004(2) 0.004(2) C14 0.025(3) 0.032(3) 0.021(3) -0.001(2) -0.004(2) 0.007(2) C15 0.035(3) 0.042(4) 0.018(3) 0.002(3) 0.006(2) 0.001(3) C16 0.042(4) 0.026(3) 0.029(3) 0.010(2) 0.000(3) 0.002(3) C17 0.025(3) 0.021(3) 0.021(3) 0.003(2) 0.004(2) 0.006(2) C18 0.030(3) 0.023(3) 0.026(3) 0.007(2) 0.005(2) 0.007(2) C19 0.040(3) 0.018(3) 0.035(3) -0.005(2) 0.002(3) 0.001(2) C20 0.035(3) 0.030(3) 0.030(3) 0.005(3) 0.009(3) 0.013(3) C21 0.017(3) 0.035(3) 0.021(3) 0.001(2) 0.003(2) -0.003(2) C22 0.018(3) 0.045(4) 0.036(3) 0.002(3) 0.006(2) -0.004(3) C23 0.029(3) 0.032(3) 0.035(3) -0.008(3) 0.003(3) -0.009(3) C24 0.025(3) 0.048(4) 0.029(3) 0.000(3) -0.007(2) -0.001(3) C25 0.018(3) 0.038(3) 0.018(3) 0.001(2) -0.003(2) 0.006(2) C26 0.021(3) 0.049(4) 0.029(3) -0.001(3) -0.001(2) 0.010(3) C27 0.020(3) 0.044(4) 0.038(3) -0.007(3) 0.000(3) -0.003(3) C28 0.023(3) 0.056(4) 0.023(3) -0.006(3) 0.002(2) 0.003(3) C29 0.024(3) 0.032(3) 0.017(3) 0.003(2) 0.003(2) 0.007(2) C30 0.033(3) 0.059(4) 0.018(3) -0.007(3) -0.002(2) 0.014(3) C31 0.027(3) 0.046(4) 0.017(3) -0.002(3) 0.007(2) 0.008(3) C32 0.035(3) 0.040(4) 0.030(3) 0.016(3) 0.008(3) 0.005(3) C33 0.032(3) 0.020(3) 0.037(3) -0.001(2) 0.005(3) 0.006(2) C34 0.035(4) 0.029(3) 0.052(4) 0.013(3) 0.009(3) 0.010(3) C35 0.041(4) 0.026(3) 0.053(4) -0.013(3) 0.004(3) -0.006(3) C36 0.044(4) 0.027(4) 0.070(5) -0.015(3) 0.013(4) 0.008(3) C37 0.021(3) 0.025(3) 0.020(3) 0.003(2) 0.009(2) 0.004(2) C38 0.027(3) 0.025(3) 0.030(3) 0.002(2) 0.017(2) 0.005(2) C39 0.027(3) 0.024(3) 0.025(3) 0.009(2) 0.011(2) 0.005(2) C40 0.033(3) 0.036(3) 0.017(3) -0.001(2) -0.001(2) 0.003(3) C41 0.028(3) 0.014(3) 0.029(3) -0.005(2) 0.011(2) -0.001(2) C42 0.032(3) 0.024(3) 0.042(4) -0.011(3) 0.010(3) -0.009(3) C43 0.036(3) 0.015(3) 0.046(4) -0.004(2) 0.012(3) 0.000(2) C44 0.046(4) 0.020(3) 0.040(4) 0.008(3) 0.010(3) -0.002(3) C45 0.018(3) 0.027(3) 0.025(3) -0.002(2) 0.002(2) 0.000(2) C46 0.018(3) 0.042(4) 0.036(3) 0.007(3) -0.004(2) 0.007(3) C47 0.020(3) 0.031(3) 0.044(4) -0.003(3) 0.003(3) -0.010(2) C48 0.027(3) 0.039(4) 0.027(3) -0.002(3) -0.004(2) 0.003(3) C49 0.062(6) 0.075(7) 0.137(10) -0.029(7) 0.024(6) 0.008(5) C50 0.043(5) 0.077(6) 0.068(6) 0.019(5) 0.013(4) 0.011(4) N11 0.020(2) 0.023(3) 0.042(3) 0.003(2) 0.011(2) 0.0049(19) N21 0.024(2) 0.032(3) 0.020(2) 0.002(2) 0.0034(19) -0.010(2) N31 0.031(3) 0.036(3) 0.023(2) 0.002(2) -0.001(2) 0.012(2) N41 0.024(3) 0.039(3) 0.032(3) 0.007(2) 0.006(2) 0.009(2) N51 0.028(3) 0.030(3) 0.025(2) -0.007(2) 0.007(2) -0.006(2) N61 0.034(3) 0.030(3) 0.032(3) -0.012(2) -0.001(2) -0.002(2) O1 0.0152(17) 0.0228(19) 0.0165(17) -0.0019(14) 0.0047(14) 0.0003(14) O2 0.0143(17) 0.0165(18) 0.0223(18) -0.0007(14) 0.0051(14) 0.0023(14) O3 0.0142(17) 0.025(2) 0.0196(18) -0.0022(15) 0.0041(14) 0.0041(15) O4 0.0142(17) 0.0212(19) 0.0196(17) -0.0024(15) 0.0050(14) 0.0033(14) O5 0.072(5) 0.154(8) 0.077(5) 0.048(5) -0.008(4) 0.012(5) O11 0.027(2) 0.031(2) 0.034(2) -0.0027(18) -0.0016(18) -0.0038(18) O12 0.032(2) 0.024(2) 0.027(2) 0.0035(17) 0.0005(17) 0.0041(17) O13 0.047(3) 0.019(2) 0.074(4) 0.005(2) 0.011(3) -0.006(2) O21 0.030(2) 0.029(2) 0.027(2) 0.0015(17) -0.0029(17) -0.0023(17) O22 0.030(2) 0.025(2) 0.024(2) 0.0008(17) -0.0081(16) 0.0000(17) O23 0.056(3) 0.043(3) 0.032(2) -0.008(2) -0.011(2) -0.017(2) O31 0.029(2) 0.029(2) 0.028(2) 0.0009(17) -0.0055(17) -0.0016(17) O32 0.032(2) 0.027(2) 0.035(2) 0.0073(18) -0.0048(19) 0.0018(18) O33 0.066(4) 0.044(3) 0.050(3) 0.012(2) -0.026(3) 0.019(3) O41 0.030(2) 0.038(2) 0.023(2) 0.0014(18) -0.0015(17) -0.0036(19) O42 0.039(2) 0.024(2) 0.029(2) 0.0051(18) 0.0074(18) 0.0037(18) O43 0.046(3) 0.071(4) 0.029(2) 0.028(2) 0.002(2) 0.014(3) O51 0.032(2) 0.034(2) 0.027(2) 0.0089(18) -0.0023(18) -0.0057(18) O52 0.033(2) 0.023(2) 0.028(2) 0.0003(17) -0.0038(17) -0.0052(17) O53 0.059(3) 0.042(3) 0.040(3) 0.005(2) 0.012(2) -0.030(2) O61 0.031(2) 0.035(2) 0.030(2) -0.0056(19) -0.0014(18) -0.0073(19) O62 0.037(2) 0.031(2) 0.022(2) -0.0019(17) -0.0030(17) -0.0035(19) O63 0.067(4) 0.065(4) 0.047(3) -0.017(3) -0.022(3) -0.027(3) P1 0.0141(6) 0.0153(6) 0.0175(6) -0.0015(5) 0.0033(5) -0.0002(5) P2 0.0143(6) 0.0180(6) 0.0160(6) 0.0013(5) 0.0030(5) 0.0010(5) P3 0.0159(6) 0.0213(7) 0.0161(6) -0.0015(5) 0.0026(5) 0.0047(5) P4 0.0147(6) 0.0146(6) 0.0176(6) -0.0010(5) 0.0047(5) 0.0015(5) Sm1 0.01374(12) 0.01687(13) 0.01598(12) -0.00016(10) 0.00274(9) 0.00106(10) Sm2 0.01416(12) 0.01668(13) 0.01618(12) -0.00072(10) 0.00319(9) 0.00126(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.534(8) . ? C1 C3 1.547(8) . ? C1 C4 1.551(7) . ? C1 P1 1.870(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.529(7) . ? C5 C7 1.540(8) . ? C5 C6 1.545(8) . ? C5 P1 1.873(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.543(7) . ? C9 C11 1.545(7) . ? C9 C12 1.547(8) . ? C9 P1 1.870(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.534(7) . ? C13 C14 1.537(7) . ? C13 C16 1.546(8) . ? C13 P2 1.868(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C20 1.534(8) . ? C17 C19 1.543(8) . ? C17 C18 1.547(7) . ? C17 P2 1.866(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.540(8) . ? C21 C24 1.542(8) . ? C21 C23 1.543(8) . ? C21 P2 1.877(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.539(9) . ? C25 C26 1.549(8) . ? C25 C28 1.551(7) . ? C25 P3 1.864(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C32 1.525(8) . ? C29 C31 1.537(7) . ? C29 C30 1.543(8) . ? C29 P3 1.876(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C36 1.540(8) . ? C33 C35 1.545(9) . ? C33 C34 1.555(9) . ? C33 P3 1.877(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.528(7) . ? C37 C39 1.533(7) . ? C37 C40 1.545(8) . ? C37 P4 1.881(5) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C44 1.535(8) . ? C41 C42 1.538(8) . ? C41 C43 1.544(7) . ? C41 P4 1.863(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C47 1.534(8) . ? C45 C46 1.541(8) . ? C45 C48 1.548(8) . ? C45 P4 1.871(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.511(13) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 O5 1.443(10) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? N11 O13 1.219(6) . ? N11 O12 1.272(6) . ? N11 O11 1.277(6) . ? N11 Sm1 2.903(5) . ? N21 O23 1.221(6) . ? N21 O21 1.271(6) . ? N21 O22 1.279(6) . ? N21 Sm1 2.917(4) . ? N31 O33 1.208(6) . ? N31 O32 1.267(6) . ? N31 O31 1.278(6) . ? N31 Sm1 2.921(5) . ? N41 O43 1.216(6) . ? N41 O42 1.274(6) . ? N41 O41 1.277(6) . ? N41 Sm2 2.902(5) . ? N51 O53 1.209(6) . ? N51 O51 1.280(6) . ? N51 O52 1.282(6) . ? N51 Sm2 2.924(5) . ? N61 O63 1.218(6) . ? N61 O61 1.268(6) . ? N61 O62 1.273(6) . ? N61 Sm2 2.922(5) . ? O1 P1 1.522(4) . ? O1 Sm1 2.255(3) . ? O2 P2 1.527(4) . ? O2 Sm1 2.258(3) . ? O3 P3 1.516(4) . ? O3 Sm2 2.259(3) . ? O4 P4 1.518(3) . ? O4 Sm2 2.272(3) . ? O5 H5 0.8400 . ? O11 Sm1 2.469(4) . ? O12 Sm1 2.478(4) . ? O21 Sm1 2.493(4) . ? O22 Sm1 2.481(4) . ? O31 Sm1 2.487(4) . ? O32 Sm1 2.488(4) . ? O41 Sm2 2.468(4) . ? O42 Sm2 2.469(4) . ? O51 Sm2 2.480(4) . ? O52 Sm2 2.486(4) . ? O61 Sm2 2.478(4) . ? O62 Sm2 2.495(4) . ? 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 C2 C1 C3 104.9(5) . . ? C2 C1 C4 109.2(5) . . ? C3 C1 C4 108.9(5) . . ? C2 C1 P1 108.9(4) . . ? C3 C1 P1 111.3(4) . . ? C4 C1 P1 113.3(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C5 C7 108.2(4) . . ? C8 C5 C6 111.3(5) . . ? C7 C5 C6 105.7(5) . . ? C8 C5 P1 112.9(4) . . ? C7 C5 P1 110.4(4) . . ? C6 C5 P1 108.1(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C11 109.7(4) . . ? C10 C9 C12 105.3(5) . . ? C11 C9 C12 109.0(5) . . ? C10 C9 P1 108.7(4) . . ? C11 C9 P1 113.9(4) . . ? C12 C9 P1 110.0(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 109.7(5) . . ? C15 C13 C16 109.0(5) . . ? C14 C13 C16 104.9(5) . . ? C15 C13 P2 113.9(4) . . ? C14 C13 P2 108.6(4) . . ? C16 C13 P2 110.4(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C17 C19 108.3(5) . . ? C20 C17 C18 109.3(4) . . ? C19 C17 C18 105.8(5) . . ? C20 C17 P2 114.2(4) . . ? C19 C17 P2 110.0(4) . . ? C18 C17 P2 108.9(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C24 109.6(5) . . ? C22 C21 C23 108.3(5) . . ? C24 C21 C23 106.3(5) . . ? C22 C21 P2 113.8(4) . . ? C24 C21 P2 109.5(4) . . ? C23 C21 P2 109.0(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C26 108.6(5) . . ? C27 C25 C28 105.0(5) . . ? C26 C25 C28 109.4(5) . . ? C27 C25 P3 111.5(4) . . ? C26 C25 P3 113.1(4) . . ? C28 C25 P3 108.9(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C32 C29 C31 110.4(5) . . ? C32 C29 C30 105.5(5) . . ? C31 C29 C30 108.9(5) . . ? C32 C29 P3 108.4(4) . . ? C31 C29 P3 113.0(4) . . ? C30 C29 P3 110.3(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C36 C33 C35 110.0(5) . . ? C36 C33 C34 109.7(5) . . ? C35 C33 C34 104.6(5) . . ? C36 C33 P3 114.4(5) . . ? C35 C33 P3 108.3(4) . . ? C34 C33 P3 109.4(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C39 109.0(4) . . ? C38 C37 C40 109.3(5) . . ? C39 C37 C40 106.7(4) . . ? C38 C37 P4 114.1(4) . . ? C39 C37 P4 108.6(4) . . ? C40 C37 P4 108.9(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C44 C41 C42 105.9(5) . . ? C44 C41 C43 108.2(5) . . ? C42 C41 C43 109.1(5) . . ? C44 C41 P4 111.2(4) . . ? C42 C41 P4 108.9(4) . . ? C43 C41 P4 113.3(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C47 C45 C46 108.8(5) . . ? C47 C45 C48 106.2(5) . . ? C46 C45 C48 109.0(5) . . ? C47 C45 P4 109.7(4) . . ? C46 C45 P4 114.1(4) . . ? C48 C45 P4 108.8(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O5 C50 C49 107.7(9) . . ? O5 C50 H50A 110.2 . . ? C49 C50 H50A 110.2 . . ? O5 C50 H50B 110.2 . . ? C49 C50 H50B 110.2 . . ? H50A C50 H50B 108.5 . . ? O13 N11 O12 121.9(5) . . ? O13 N11 O11 122.2(5) . . ? O12 N11 O11 115.8(4) . . ? O13 N11 Sm1 179.4(4) . . ? O12 N11 Sm1 58.1(3) . . ? O11 N11 Sm1 57.7(3) . . ? O23 N21 O21 122.6(5) . . ? O23 N21 O22 121.5(5) . . ? O21 N21 O22 115.8(4) . . ? O23 N21 Sm1 179.0(4) . . ? O21 N21 Sm1 58.2(3) . . ? O22 N21 Sm1 57.7(2) . . ? O33 N31 O32 122.5(6) . . ? O33 N31 O31 121.9(5) . . ? O32 N31 O31 115.6(4) . . ? O33 N31 Sm1 179.7(5) . . ? O32 N31 Sm1 57.8(3) . . ? O31 N31 Sm1 57.8(2) . . ? O43 N41 O42 122.1(6) . . ? O43 N41 O41 122.4(6) . . ? O42 N41 O41 115.4(5) . . ? O43 N41 Sm2 177.1(4) . . ? O42 N41 Sm2 57.7(3) . . ? O41 N41 Sm2 57.7(3) . . ? O53 N51 O51 122.7(5) . . ? O53 N51 O52 122.5(5) . . ? O51 N51 O52 114.8(5) . . ? O53 N51 Sm2 176.8(4) . . ? O51 N51 Sm2 57.3(3) . . ? O52 N51 Sm2 57.6(3) . . ? O63 N61 O61 123.0(6) . . ? O63 N61 O62 121.7(5) . . ? O61 N61 O62 115.2(5) . . ? O63 N61 Sm2 174.3(5) . . ? O61 N61 Sm2 57.3(3) . . ? O62 N61 Sm2 58.1(3) . . ? P1 O1 Sm1 177.3(2) . . ? P2 O2 Sm1 176.1(2) . . ? P3 O3 Sm2 175.8(2) . . ? P4 O4 Sm2 172.7(2) . . ? C50 O5 H5 109.5 . . ? N11 O11 Sm1 96.4(3) . . ? N11 O12 Sm1 96.0(3) . . ? N21 O21 Sm1 96.1(3) . . ? N21 O22 Sm1 96.5(3) . . ? N31 O31 Sm1 96.4(3) . . ? N31 O32 Sm1 96.7(3) . . ? N41 O41 Sm2 96.4(3) . . ? N41 O42 Sm2 96.4(3) . . ? N51 O51 Sm2 96.9(3) . . ? N51 O52 Sm2 96.6(3) . . ? N61 O61 Sm2 97.2(3) . . ? N61 O62 Sm2 96.3(3) . . ? O1 P1 C9 107.0(2) . . ? O1 P1 C1 106.9(2) . . ? C9 P1 C1 112.2(2) . . ? O1 P1 C5 106.8(2) . . ? C9 P1 C5 112.5(2) . . ? C1 P1 C5 111.1(2) . . ? O2 P2 C17 107.0(2) . . ? O2 P2 C13 107.1(2) . . ? C17 P2 C13 111.4(2) . . ? O2 P2 C21 106.7(2) . . ? C17 P2 C21 112.3(3) . . ? C13 P2 C21 112.0(2) . . ? O3 P3 C25 107.6(2) . . ? O3 P3 C29 106.9(2) . . ? C25 P3 C29 111.0(3) . . ? O3 P3 C33 107.0(2) . . ? C25 P3 C33 111.8(3) . . ? C29 P3 C33 112.1(3) . . ? O4 P4 C41 107.2(2) . . ? O4 P4 C45 106.7(2) . . ? C41 P4 C45 111.9(3) . . ? O4 P4 C37 107.2(2) . . ? C41 P4 C37 111.9(2) . . ? C45 P4 C37 111.7(2) . . ? O1 Sm1 O2 177.65(12) . . ? O1 Sm1 O11 92.74(13) . . ? O2 Sm1 O11 87.08(13) . . ? O1 Sm1 O12 83.38(13) . . ? O2 Sm1 O12 94.69(13) . . ? O11 Sm1 O12 51.76(13) . . ? O1 Sm1 O22 92.46(13) . . ? O2 Sm1 O22 85.59(13) . . ? O11 Sm1 O22 119.59(13) . . ? O12 Sm1 O22 69.27(13) . . ? O1 Sm1 O31 84.07(13) . . ? O2 Sm1 O31 98.07(13) . . ? O11 Sm1 O31 69.96(13) . . ? O12 Sm1 O31 119.32(13) . . ? O22 Sm1 O31 170.09(13) . . ? O1 Sm1 O32 96.17(13) . . ? O2 Sm1 O32 85.95(13) . . ? O11 Sm1 O32 118.91(14) . . ? O12 Sm1 O32 170.51(13) . . ? O22 Sm1 O32 120.21(13) . . ? O31 Sm1 O32 51.31(13) . . ? O1 Sm1 O21 85.98(13) . . ? O2 Sm1 O21 93.82(13) . . ? O11 Sm1 O21 170.84(13) . . ? O12 Sm1 O21 119.08(13) . . ? O22 Sm1 O21 51.50(13) . . ? O31 Sm1 O21 118.84(13) . . ? O32 Sm1 O21 70.26(13) . . ? O1 Sm1 N11 87.60(13) . . ? O2 Sm1 N11 91.24(13) . . ? O11 Sm1 N11 25.92(13) . . ? O12 Sm1 N11 25.84(13) . . ? O22 Sm1 N11 94.47(14) . . ? O31 Sm1 N11 94.65(14) . . ? O32 Sm1 N11 144.79(14) . . ? O21 Sm1 N11 144.92(14) . . ? O1 Sm1 N21 88.78(12) . . ? O2 Sm1 N21 90.03(13) . . ? O11 Sm1 N21 145.35(14) . . ? O12 Sm1 N21 94.20(13) . . ? O22 Sm1 N21 25.83(13) . . ? O31 Sm1 N21 144.45(14) . . ? O32 Sm1 N21 95.27(13) . . ? O21 Sm1 N21 25.67(13) . . ? N11 Sm1 N21 119.85(14) . . ? O1 Sm1 N31 90.06(13) . . ? O2 Sm1 N31 92.29(13) . . ? O11 Sm1 N31 94.62(14) . . ? O12 Sm1 N31 145.08(14) . . ? O22 Sm1 N31 145.50(14) . . ? O31 Sm1 N31 25.78(14) . . ? O32 Sm1 N31 25.53(14) . . ? O21 Sm1 N31 94.45(14) . . ? N11 Sm1 N31 120.02(15) . . ? N21 Sm1 N31 120.00(14) . . ? O3 Sm2 O4 173.45(13) . . ? O3 Sm2 O41 96.82(13) . . ? O4 Sm2 O41 87.44(13) . . ? O3 Sm2 O42 84.54(13) . . ? O4 Sm2 O42 94.29(13) . . ? O41 Sm2 O42 51.77(14) . . ? O3 Sm2 O61 90.02(14) . . ? O4 Sm2 O61 83.56(13) . . ? O41 Sm2 O61 119.07(14) . . ? O42 Sm2 O61 69.01(14) . . ? O3 Sm2 O51 95.94(14) . . ? O4 Sm2 O51 86.33(13) . . ? O41 Sm2 O51 118.45(14) . . ? O42 Sm2 O51 170.09(14) . . ? O61 Sm2 O51 120.85(13) . . ? O3 Sm2 O52 82.93(13) . . ? O4 Sm2 O52 103.21(13) . . ? O41 Sm2 O52 70.89(13) . . ? O42 Sm2 O52 118.91(13) . . ? O61 Sm2 O52 168.59(13) . . ? O51 Sm2 O52 51.53(13) . . ? O3 Sm2 O62 86.59(13) . . ? O4 Sm2 O62 88.39(13) . . ? O41 Sm2 O62 169.79(14) . . ? O42 Sm2 O62 119.36(14) . . ? O61 Sm2 O62 51.12(13) . . ? O51 Sm2 O62 70.52(13) . . ? O52 Sm2 O62 119.18(13) . . ? O3 Sm2 N41 91.11(13) . . ? O4 Sm2 N41 90.59(13) . . ? O41 Sm2 N41 25.92(14) . . ? O42 Sm2 N41 25.86(14) . . ? O61 Sm2 N41 93.94(15) . . ? O51 Sm2 N41 144.37(15) . . ? O52 Sm2 N41 95.14(14) . . ? O62 Sm2 N41 144.94(15) . . ? O3 Sm2 N61 89.23(13) . . ? O4 Sm2 N61 84.43(13) . . ? O41 Sm2 N61 144.37(15) . . ? O42 Sm2 N61 94.30(15) . . ? O61 Sm2 N61 25.50(14) . . ? O51 Sm2 N61 95.60(14) . . ? O52 Sm2 N61 144.72(14) . . ? O62 Sm2 N61 25.67(14) . . ? N41 Sm2 N61 119.44(16) . . ? O3 Sm2 N51 88.35(13) . . ? O4 Sm2 N51 96.23(13) . . ? O41 Sm2 N51 95.17(14) . . ? O42 Sm2 N51 144.73(14) . . ? O61 Sm2 N51 145.65(13) . . ? O51 Sm2 N51 25.75(13) . . ? O52 Sm2 N51 25.82(12) . . ? O62 Sm2 N51 94.54(13) . . ? N41 Sm2 N51 120.39(14) . . ? N61 Sm2 N51 120.15(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.962 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.155 #===End data_Eu _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Eu _chemical_melting_point ? _chemical_formula_moiety 'C25 H57 Eu N3 O11.50 P2' _chemical_formula_sum 'C25 H57 Eu N3 O11.50 P2' _chemical_formula_weight 797.64 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' 'Eu' 'Eu' -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.2591(2) _cell_length_b 27.2034(3) _cell_length_c 13.8018(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.8050(10) _cell_angle_gamma 90.00 _cell_volume 7215.00(15) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 36275 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3304 _exptl_absorpt_coefficient_mu 1.882 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8056 _exptl_absorpt_correction_T_max 0.8954 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39965 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8253 _reflns_number_gt 7404 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+27.4816P] 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 8253 _refine_ls_number_parameters 401 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.004 _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 C1 C 0.94860(13) 0.09610(10) -0.02913(19) 0.0204(5) Uani 1 1 d . . . C2 C 1.00451(15) 0.09181(11) 0.0558(2) 0.0292(6) Uani 1 1 d . . . H2A H 1.0281 0.0600 0.0525 0.044 Uiso 1 1 calc R . . H2B H 0.9824 0.0944 0.1176 0.044 Uiso 1 1 calc R . . H2C H 1.0386 0.1183 0.0514 0.044 Uiso 1 1 calc R . . C3 C 0.90238(15) 0.04998(10) -0.0232(2) 0.0261(6) Uani 1 1 d . . . H3A H 0.8729 0.0467 -0.0836 0.039 Uiso 1 1 calc R . . H3B H 0.8729 0.0532 0.0316 0.039 Uiso 1 1 calc R . . H3C H 0.9319 0.0208 -0.0140 0.039 Uiso 1 1 calc R . . C4 C 0.98378(16) 0.09516(11) -0.1258(2) 0.0303(6) Uani 1 1 d . . . H4A H 1.0141 0.1239 -0.1298 0.045 Uiso 1 1 calc R . . H4B H 0.9481 0.0958 -0.1798 0.045 Uiso 1 1 calc R . . H4C H 1.0116 0.0651 -0.1295 0.045 Uiso 1 1 calc R . . C5 C 0.83333(14) 0.16481(11) -0.12052(18) 0.0239(6) Uani 1 1 d . . . C6 C 0.86821(18) 0.19020(12) -0.2046(2) 0.0358(7) Uani 1 1 d . . . H6A H 0.9062 0.1696 -0.2252 0.054 Uiso 1 1 calc R . . H6B H 0.8868 0.2221 -0.1826 0.054 Uiso 1 1 calc R . . H6C H 0.8338 0.1950 -0.2593 0.054 Uiso 1 1 calc R . . C7 C 0.79912(16) 0.11653(12) -0.1582(2) 0.0332(7) Uani 1 1 d . . . H7A H 0.7610 0.1241 -0.2066 0.050 Uiso 1 1 calc R . . H7B H 0.7807 0.0986 -0.1039 0.050 Uiso 1 1 calc R . . H7C H 0.8339 0.0962 -0.1882 0.050 Uiso 1 1 calc R . . C8 C 0.77285(16) 0.19700(12) -0.0885(2) 0.0330(7) Uani 1 1 d . . . H8A H 0.7373 0.2000 -0.1424 0.049 Uiso 1 1 calc R . . H8B H 0.7905 0.2297 -0.0701 0.049 Uiso 1 1 calc R . . H8C H 0.7524 0.1817 -0.0328 0.049 Uiso 1 1 calc R . . C9 C 0.94837(14) 0.20627(9) 0.02383(19) 0.0216(5) Uani 1 1 d . . . C10 C 0.97319(15) 0.20152(11) 0.1322(2) 0.0270(6) Uani 1 1 d . . . H10A H 1.0007 0.2305 0.1523 0.041 Uiso 1 1 calc R . . H10B H 1.0019 0.1720 0.1417 0.041 Uiso 1 1 calc R . . H10C H 0.9327 0.1991 0.1714 0.041 Uiso 1 1 calc R . . C11 C 0.90515(17) 0.25361(10) 0.0163(2) 0.0344(7) Uani 1 1 d . . . H11A H 0.8630 0.2494 0.0514 0.052 Uiso 1 1 calc R . . H11B H 0.8922 0.2607 -0.0522 0.052 Uiso 1 1 calc R . . H11C H 0.9327 0.2809 0.0447 0.052 Uiso 1 1 calc R . . C12 C 1.01239(16) 0.21210(11) -0.0368(2) 0.0325(7) Uani 1 1 d . . . H12A H 0.9970 0.2154 -0.1056 0.049 Uiso 1 1 calc R . . H12B H 1.0423 0.1831 -0.0279 0.049 Uiso 1 1 calc R . . H12C H 1.0385 0.2415 -0.0154 0.049 Uiso 1 1 calc R . . C13 C 0.73909(14) 0.08352(11) 0.51907(18) 0.0239(6) Uani 1 1 d . . . C14 C 0.70471(16) 0.05729(12) 0.6027(2) 0.0327(7) Uani 1 1 d . . . H14A H 0.7388 0.0536 0.6582 0.049 Uiso 1 1 calc R . . H14B H 0.6884 0.0248 0.5809 0.049 Uiso 1 1 calc R . . H14C H 0.6652 0.0768 0.6220 0.049 Uiso 1 1 calc R . . C15 C 0.77025(16) 0.13263(12) 0.5563(2) 0.0323(7) Uani 1 1 d . . . H15A H 0.7334 0.1530 0.5811 0.048 Uiso 1 1 calc R . . H15B H 0.7910 0.1498 0.5029 0.048 Uiso 1 1 calc R . . H15C H 0.8061 0.1263 0.6085 0.048 Uiso 1 1 calc R . . C16 C 0.80184(15) 0.05253(12) 0.4898(2) 0.0319(7) Uani 1 1 d . . . H16A H 0.8358 0.0495 0.5456 0.048 Uiso 1 1 calc R . . H16B H 0.8237 0.0687 0.4362 0.048 Uiso 1 1 calc R . . H16C H 0.7857 0.0198 0.4692 0.048 Uiso 1 1 calc R . . C17 C 0.62813(14) 0.03622(10) 0.3747(2) 0.0241(6) Uani 1 1 d . . . C18 C 0.60217(15) 0.03983(11) 0.2663(2) 0.0293(6) Uani 1 1 d . . . H18A H 0.5769 0.0098 0.2469 0.044 Uiso 1 1 calc R . . H18B H 0.6421 0.0438 0.2265 0.044 Uiso 1 1 calc R . . H18C H 0.5711 0.0682 0.2568 0.044 Uiso 1 1 calc R . . C19 C 0.67604(17) -0.00916(11) 0.3808(2) 0.0323(7) Uani 1 1 d . . . H19A H 0.6906 -0.0159 0.4489 0.048 Uiso 1 1 calc R . . H19B H 0.7172 -0.0028 0.3445 0.048 Uiso 1 1 calc R . . H19C H 0.6509 -0.0377 0.3528 0.048 Uiso 1 1 calc R . . C20 C 0.56596(16) 0.02672(12) 0.4369(2) 0.0345(7) Uani 1 1 d . . . H20A H 0.5329 0.0541 0.4290 0.052 Uiso 1 1 calc R . . H20B H 0.5826 0.0240 0.5053 0.052 Uiso 1 1 calc R . . H20C H 0.5428 -0.0039 0.4159 0.052 Uiso 1 1 calc R . . C21 C 0.62093(14) 0.14744(10) 0.42441(19) 0.0230(6) Uani 1 1 d . . . C22 C 0.56191(15) 0.14866(12) 0.3439(2) 0.0304(6) Uani 1 1 d . . . H22A H 0.5315 0.1202 0.3506 0.046 Uiso 1 1 calc R . . H22B H 0.5817 0.1477 0.2803 0.046 Uiso 1 1 calc R . . H22C H 0.5349 0.1789 0.3494 0.046 Uiso 1 1 calc R . . C23 C 0.58847(16) 0.14790(11) 0.5237(2) 0.0305(6) Uani 1 1 d . . . H23A H 0.5546 0.1747 0.5251 0.046 Uiso 1 1 calc R . . H23B H 0.6252 0.1528 0.5754 0.046 Uiso 1 1 calc R . . H23C H 0.5651 0.1165 0.5335 0.046 Uiso 1 1 calc R . . C24 C 0.66360(16) 0.19467(10) 0.4111(2) 0.0282(6) Uani 1 1 d . . . H24A H 0.6334 0.2234 0.4158 0.042 Uiso 1 1 calc R . . H24B H 0.6830 0.1942 0.3472 0.042 Uiso 1 1 calc R . . H24C H 0.7016 0.1964 0.4619 0.042 Uiso 1 1 calc R . . N11 N 0.86492(13) 0.03367(9) 0.23106(16) 0.0278(5) Uani 1 1 d . . . N21 N 0.65645(12) 0.12260(10) 0.08203(17) 0.0296(6) Uani 1 1 d . . . N32 N 0.82887(13) 0.21248(9) 0.30709(18) 0.0284(5) Uani 1 1 d . . . O1 O 0.84868(9) 0.14085(6) 0.07211(12) 0.0170(3) Uani 1 1 d . . . O2 O 0.72300(9) 0.10457(7) 0.32468(12) 0.0175(4) Uani 1 1 d . . . O11 O 0.88800(11) 0.07504(8) 0.26217(14) 0.0293(4) Uani 1 1 d . . . O12 O 0.80466(11) 0.03492(7) 0.18617(15) 0.0310(5) Uani 1 1 d . . . O13 O 0.89769(14) -0.00424(9) 0.24222(18) 0.0492(7) Uani 1 1 d . . . O21 O 0.69982(10) 0.08721(8) 0.08190(14) 0.0298(4) Uani 1 1 d . . . O22 O 0.67602(11) 0.16005(8) 0.13153(14) 0.0305(5) Uani 1 1 d . . . O23 O 0.59962(12) 0.12045(10) 0.03770(19) 0.0517(7) Uani 1 1 d . . . O31 O 0.78563(11) 0.21328(7) 0.23307(14) 0.0302(5) Uani 1 1 d . . . O32 O 0.85496(10) 0.17090(7) 0.32897(14) 0.0284(4) Uani 1 1 d . . . O33 O 0.84404(14) 0.24950(9) 0.35358(19) 0.0515(7) Uani 1 1 d . . . P1 P 0.89392(3) 0.15173(2) -0.01187(4) 0.01424(12) Uani 1 1 d . . . P2 P 0.67867(3) 0.09306(2) 0.40898(4) 0.01618(13) Uani 1 1 d . . . Eu1 Eu 0.787284(6) 0.123988(4) 0.200653(8) 0.01438(4) Uani 1 1 d . . . C41 C 0.4777(6) 0.1368(4) 0.7200(9) 0.077(2) Uiso 0.50 1 d PD A -1 H41A H 0.4534 0.1063 0.7016 0.115 Uiso 0.50 1 calc PR A -1 H41B H 0.4915 0.1537 0.6615 0.115 Uiso 0.50 1 calc PR A -1 H41C H 0.4468 0.1582 0.7547 0.115 Uiso 0.50 1 calc PR A -1 O4 O 0.5338(4) 0.0903(3) 0.8446(5) 0.084(2) Uiso 0.50 1 d PD A -1 H4 H 0.5668 0.0916 0.8875 0.126 Uiso 0.50 1 calc PR A -1 C42 C 0.5401(7) 0.1255(4) 0.7833(9) 0.077(2) Uiso 0.50 1 d PD A -1 H42A H 0.5783 0.1170 0.7418 0.092 Uiso 0.50 1 calc PR A -1 H42B H 0.5541 0.1556 0.8199 0.092 Uiso 0.50 1 calc PR A -1 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 C1 0.0209(12) 0.0191(13) 0.0224(12) -0.0032(10) 0.0103(10) -0.0012(10) C2 0.0232(14) 0.0256(15) 0.0388(16) 0.0007(12) 0.0020(12) 0.0084(12) C3 0.0305(15) 0.0192(13) 0.0295(14) -0.0016(11) 0.0095(12) -0.0011(11) C4 0.0315(15) 0.0287(15) 0.0327(15) -0.0105(12) 0.0173(12) -0.0027(12) C5 0.0256(14) 0.0307(15) 0.0152(12) 0.0042(11) -0.0007(10) -0.0017(12) C6 0.0481(19) 0.0427(19) 0.0168(13) 0.0118(12) 0.0040(12) -0.0037(15) C7 0.0337(16) 0.0440(19) 0.0214(14) -0.0035(12) -0.0021(12) -0.0104(14) C8 0.0313(16) 0.0387(18) 0.0282(15) 0.0066(13) -0.0038(12) 0.0101(13) C9 0.0245(13) 0.0170(13) 0.0237(13) -0.0032(10) 0.0038(10) -0.0060(10) C10 0.0257(14) 0.0307(15) 0.0246(14) -0.0091(11) 0.0013(11) -0.0053(12) C11 0.0442(18) 0.0174(14) 0.0415(17) -0.0044(12) 0.0018(14) -0.0009(13) C12 0.0340(16) 0.0309(16) 0.0341(16) -0.0015(13) 0.0128(13) -0.0166(13) C13 0.0233(13) 0.0341(15) 0.0144(12) 0.0032(11) 0.0027(10) 0.0090(12) C14 0.0370(17) 0.0410(18) 0.0208(14) 0.0130(12) 0.0070(12) 0.0143(14) C15 0.0329(16) 0.0449(18) 0.0185(13) -0.0027(12) -0.0018(11) 0.0003(14) C16 0.0261(15) 0.0459(19) 0.0236(14) 0.0058(13) 0.0012(11) 0.0139(13) C17 0.0231(13) 0.0228(14) 0.0274(14) 0.0005(11) 0.0105(11) -0.0018(11) C18 0.0252(14) 0.0321(16) 0.0309(15) -0.0058(12) 0.0024(12) -0.0075(12) C19 0.0400(17) 0.0216(15) 0.0367(16) 0.0043(12) 0.0139(13) 0.0019(13) C20 0.0309(16) 0.0362(17) 0.0385(17) 0.0040(14) 0.0174(13) -0.0063(13) C21 0.0229(13) 0.0260(14) 0.0208(12) 0.0053(11) 0.0065(10) 0.0093(11) C22 0.0246(14) 0.0364(17) 0.0302(15) 0.0063(13) 0.0018(11) 0.0122(13) C23 0.0341(16) 0.0304(16) 0.0288(15) 0.0035(12) 0.0152(12) 0.0126(13) C24 0.0367(16) 0.0205(14) 0.0286(14) 0.0023(11) 0.0109(12) 0.0084(12) N11 0.0400(14) 0.0250(13) 0.0197(11) 0.0069(9) 0.0114(10) 0.0100(11) N21 0.0236(12) 0.0407(15) 0.0242(12) 0.0071(11) -0.0006(9) -0.0026(11) N32 0.0291(13) 0.0249(13) 0.0320(13) -0.0082(10) 0.0084(10) -0.0048(10) O1 0.0178(8) 0.0198(9) 0.0141(8) 0.0015(7) 0.0049(7) -0.0006(7) O2 0.0169(8) 0.0218(9) 0.0144(8) 0.0019(7) 0.0054(6) 0.0005(7) O11 0.0309(11) 0.0305(11) 0.0256(10) 0.0009(8) -0.0041(8) 0.0056(9) O12 0.0340(11) 0.0223(10) 0.0373(11) -0.0047(9) 0.0076(9) -0.0006(9) O13 0.0715(18) 0.0320(13) 0.0447(14) 0.0118(11) 0.0099(12) 0.0272(12) O21 0.0251(10) 0.0357(12) 0.0281(10) -0.0076(9) -0.0006(8) -0.0036(9) O22 0.0304(11) 0.0306(11) 0.0296(10) 0.0024(9) -0.0057(9) 0.0050(9) O23 0.0284(12) 0.0696(19) 0.0542(15) 0.0054(13) -0.0200(11) -0.0058(12) O31 0.0410(12) 0.0213(10) 0.0281(10) -0.0021(8) 0.0007(9) 0.0039(9) O32 0.0264(10) 0.0269(11) 0.0314(11) -0.0058(8) -0.0017(8) -0.0022(8) O33 0.0570(16) 0.0342(13) 0.0625(16) -0.0277(12) -0.0019(13) -0.0061(12) P1 0.0170(3) 0.0144(3) 0.0116(3) 0.0003(2) 0.0034(2) -0.0015(2) P2 0.0158(3) 0.0193(3) 0.0139(3) 0.0031(2) 0.0051(2) 0.0043(2) Eu1 0.01594(7) 0.01587(7) 0.01170(6) 0.00017(4) 0.00369(4) -0.00020(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C4 1.536(4) . ? C1 C2 1.543(4) . ? C1 C3 1.544(4) . ? C1 P1 1.868(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.542(4) . ? C5 C7 1.544(4) . ? C5 C8 1.545(4) . ? C5 P1 1.872(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.533(4) . ? C9 C12 1.544(4) . ? C9 C10 1.545(4) . ? C9 P1 1.864(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.539(4) . ? C13 C14 1.543(4) . ? C13 C16 1.549(4) . ? C13 P2 1.870(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.540(4) . ? C17 C20 1.541(4) . ? C17 C18 1.549(4) . ? C17 P2 1.871(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.537(4) . ? C21 C24 1.543(4) . ? C21 C23 1.543(4) . ? C21 P2 1.871(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? N11 O13 1.214(3) . ? N11 O11 1.274(3) . ? N11 O12 1.279(3) . ? N11 Eu1 2.892(2) . ? N21 O23 1.219(3) . ? N21 O22 1.270(3) . ? N21 O21 1.274(3) . ? N21 Eu1 2.913(2) . ? N32 O33 1.219(3) . ? N32 O32 1.266(3) . ? N32 O31 1.275(3) . ? N32 Eu1 2.905(2) . ? O1 P1 1.5245(17) . ? O1 Eu1 2.2438(16) . ? O2 P2 1.5206(17) . ? O2 Eu1 2.2413(16) . ? O11 Eu1 2.4572(19) . ? O12 Eu1 2.456(2) . ? O21 Eu1 2.4816(19) . ? O22 Eu1 2.4885(19) . ? O31 Eu1 2.4705(19) . ? O32 Eu1 2.4815(19) . ? C41 C42 1.470(10) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? O4 C42 1.288(8) . ? O4 H4 0.8400 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? 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 C4 C1 C2 109.5(2) . . ? C4 C1 C3 108.7(2) . . ? C2 C1 C3 105.9(2) . . ? C4 C1 P1 114.15(19) . . ? C2 C1 P1 109.59(18) . . ? C3 C1 P1 108.64(18) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C7 109.0(2) . . ? C6 C5 C8 109.6(2) . . ? C7 C5 C8 105.4(2) . . ? C6 C5 P1 114.1(2) . . ? C7 C5 P1 109.73(19) . . ? C8 C5 P1 108.69(18) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 C12 109.0(2) . . ? C11 C9 C10 105.5(2) . . ? C12 C9 C10 109.1(2) . . ? C11 C9 P1 110.94(19) . . ? C12 C9 P1 113.20(19) . . ? C10 C9 P1 108.78(18) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 109.2(2) . . ? C15 C13 C16 105.4(2) . . ? C14 C13 C16 108.9(2) . . ? C15 C13 P2 111.00(19) . . ? C14 C13 P2 113.4(2) . . ? C16 C13 P2 108.54(18) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C20 108.7(2) . . ? C19 C17 C18 104.9(2) . . ? C20 C17 C18 109.6(2) . . ? C19 C17 P2 110.4(2) . . ? C20 C17 P2 114.1(2) . . ? C18 C17 P2 108.74(18) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C24 105.7(2) . . ? C22 C21 C23 108.5(2) . . ? C24 C21 C23 110.4(2) . . ? C22 C21 P2 110.58(19) . . ? C24 C21 P2 108.64(18) . . ? C23 C21 P2 112.73(18) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O13 N11 O11 122.7(3) . . ? O13 N11 O12 122.1(3) . . ? O11 N11 O12 115.1(2) . . ? O13 N11 Eu1 178.93(19) . . ? O11 N11 Eu1 57.59(12) . . ? O12 N11 Eu1 57.55(13) . . ? O23 N21 O22 122.2(3) . . ? O23 N21 O21 122.0(3) . . ? O22 N21 O21 115.8(2) . . ? O23 N21 Eu1 175.5(2) . . ? O22 N21 Eu1 58.15(13) . . ? O21 N21 Eu1 57.86(12) . . ? O33 N32 O32 122.3(3) . . ? O33 N32 O31 121.9(3) . . ? O32 N32 O31 115.7(2) . . ? O33 N32 Eu1 177.5(2) . . ? O32 N32 Eu1 58.13(12) . . ? O31 N32 Eu1 57.68(13) . . ? P1 O1 Eu1 176.95(11) . . ? P2 O2 Eu1 178.21(12) . . ? N11 O11 Eu1 96.45(15) . . ? N11 O12 Eu1 96.37(15) . . ? N21 O21 Eu1 96.36(15) . . ? N21 O22 Eu1 96.16(15) . . ? N32 O31 Eu1 96.47(15) . . ? N32 O32 Eu1 96.19(15) . . ? O1 P1 C9 107.05(11) . . ? O1 P1 C1 107.17(11) . . ? C9 P1 C1 111.50(12) . . ? O1 P1 C5 106.78(11) . . ? C9 P1 C5 111.73(12) . . ? C1 P1 C5 112.25(12) . . ? O2 P2 C13 107.43(11) . . ? O2 P2 C21 107.01(11) . . ? C13 P2 C21 111.09(12) . . ? O2 P2 C17 106.58(11) . . ? C13 P2 C17 112.10(13) . . ? C21 P2 C17 112.27(13) . . ? O2 Eu1 O1 177.28(6) . . ? O2 Eu1 O12 85.11(7) . . ? O1 Eu1 O12 93.18(7) . . ? O2 Eu1 O11 94.12(7) . . ? O1 Eu1 O11 86.48(6) . . ? O12 Eu1 O11 52.03(7) . . ? O2 Eu1 O31 94.53(7) . . ? O1 Eu1 O31 87.47(7) . . ? O12 Eu1 O31 171.20(7) . . ? O11 Eu1 O31 119.31(7) . . ? O2 Eu1 O32 82.34(6) . . ? O1 Eu1 O32 100.35(6) . . ? O12 Eu1 O32 119.84(7) . . ? O11 Eu1 O32 70.54(7) . . ? O31 Eu1 O32 51.50(7) . . ? O2 Eu1 O21 91.39(6) . . ? O1 Eu1 O21 86.01(6) . . ? O12 Eu1 O21 68.82(7) . . ? O11 Eu1 O21 119.70(7) . . ? O31 Eu1 O21 119.98(7) . . ? O32 Eu1 O21 168.54(7) . . ? O2 Eu1 O22 83.14(7) . . ? O1 Eu1 O22 95.84(6) . . ? O12 Eu1 O22 118.44(7) . . ? O11 Eu1 O22 170.40(7) . . ? O31 Eu1 O22 70.17(7) . . ? O32 Eu1 O22 117.97(7) . . ? O21 Eu1 O22 51.41(7) . . ? O2 Eu1 N11 89.73(6) . . ? O1 Eu1 N11 89.65(6) . . ? O12 Eu1 N11 26.07(7) . . ? O11 Eu1 N11 25.96(7) . . ? O31 Eu1 N11 145.26(7) . . ? O32 Eu1 N11 95.24(7) . . ? O21 Eu1 N11 94.31(7) . . ? O22 Eu1 N11 144.51(7) . . ? O2 Eu1 N32 87.52(7) . . ? O1 Eu1 N32 95.07(6) . . ? O12 Eu1 N32 145.51(7) . . ? O11 Eu1 N32 95.13(7) . . ? O31 Eu1 N32 25.85(7) . . ? O32 Eu1 N32 25.67(7) . . ? O21 Eu1 N32 145.12(7) . . ? O22 Eu1 N32 93.94(7) . . ? N11 Eu1 N32 120.53(7) . . ? O2 Eu1 N21 85.71(6) . . ? O1 Eu1 N21 92.28(6) . . ? O12 Eu1 N21 93.38(7) . . ? O11 Eu1 N21 145.17(7) . . ? O31 Eu1 N21 95.37(7) . . ? O32 Eu1 N21 143.29(7) . . ? O21 Eu1 N21 25.78(7) . . ? O22 Eu1 N21 25.69(7) . . ? N11 Eu1 N21 119.35(7) . . ? N32 Eu1 N21 119.62(7) . . ? O4 C42 C41 116.0(11) . . ? O4 C42 H42A 108.3 . . ? C41 C42 H42A 108.3 . . ? O4 C42 H42B 108.3 . . ? C41 C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.560 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.086 #===END data_Dy _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Dy _chemical_melting_point ? _chemical_formula_moiety 'C24 H54 Dy N3 O11 P2' _chemical_formula_sum 'C24 H54 Dy N3 O11 P2' _chemical_formula_weight 785.14 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' 'Dy' 'Dy' -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R3 _symmetry_space_group_name_Hall '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' _cell_length_a 28.2470(3) _cell_length_b 28.2470(3) _cell_length_c 15.0660(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10410.5(3) _cell_formula_units_Z 12 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 20424 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4836 _exptl_absorpt_coefficient_mu 2.299 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7390 _exptl_absorpt_correction_T_max 0.9555 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '9.091' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23210 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.0835 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10212 _reflns_number_gt 9210 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _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^ > 2\s(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. Crystal structure is a racemic twin with 70:30 % ratio Refined BASF = 0.69553 ; _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^)+(0.0000P)^2^+73.7087P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.696(10) _refine_ls_number_reflns 10212 _refine_ls_number_parameters 518 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _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 Dy1 Dy 0.712058(12) 0.864466(12) 0.85315(2) 0.01543(8) Uani 1 1 d . . . P1 P 0.65856(7) 0.80378(7) 1.07513(12) 0.0143(4) Uani 1 1 d . . . P2 P 0.67444(7) 0.85962(7) 0.61520(12) 0.0153(4) Uani 1 1 d . . . O1 O 0.68410(19) 0.83013(19) 0.9871(3) 0.0179(11) Uani 1 1 d . . . O2 O 0.6921(2) 0.86346(19) 0.7110(3) 0.0154(11) Uani 1 1 d . . . O11 O 0.79274(19) 0.9210(2) 0.9404(3) 0.0215(11) Uani 1 1 d . . . O12 O 0.7966(2) 0.9411(2) 0.8009(4) 0.0232(11) Uani 1 1 d . . . O13 O 0.86948(18) 0.98473(19) 0.8839(4) 0.0251(12) Uani 1 1 d . . . O21 O 0.6956(2) 0.9381(2) 0.8844(4) 0.0258(13) Uani 1 1 d . . . O22 O 0.6230(2) 0.8594(2) 0.8628(4) 0.0221(12) Uani 1 1 d . . . O23 O 0.6146(3) 0.9290(2) 0.9026(5) 0.0453(17) Uani 1 1 d . . . O31 O 0.6828(2) 0.7688(2) 0.8192(4) 0.0250(12) Uani 1 1 d . . . O32 O 0.7406(3) 0.7422(2) 0.7793(4) 0.0405(16) Uani 1 1 d . . . O33 O 0.7697(2) 0.8254(2) 0.8246(4) 0.0309(13) Uani 1 1 d . . . N11 N 0.8212(2) 0.9496(2) 0.8756(4) 0.0174(13) Uani 1 1 d . . . N21 N 0.6435(3) 0.9099(3) 0.8833(4) 0.0258(15) Uani 1 1 d . . . N31 N 0.7313(3) 0.7774(2) 0.8073(4) 0.0243(14) Uani 1 1 d . . . C1 C 0.5835(3) 0.7596(3) 1.0575(5) 0.0196(16) Uani 1 1 d . . . C2 C 0.5734(3) 0.7310(3) 0.9667(5) 0.0252(17) Uani 1 1 d . . . H2A H 0.5930 0.7105 0.9642 0.038 Uiso 1 1 calc R . . H2B H 0.5867 0.7584 0.9193 0.038 Uiso 1 1 calc R . . H2C H 0.5342 0.7058 0.9589 0.038 Uiso 1 1 calc R . . C3 C 0.5533(3) 0.7928(3) 1.0534(6) 0.0283(18) Uani 1 1 d . . . H3A H 0.5148 0.7683 1.0386 0.043 Uiso 1 1 calc R . . H3B H 0.5702 0.8213 1.0079 0.043 Uiso 1 1 calc R . . H3C H 0.5558 0.8098 1.1113 0.043 Uiso 1 1 calc R . . C4 C 0.5559(3) 0.7161(3) 1.1299(5) 0.0277(18) Uani 1 1 d . . . H4A H 0.5617 0.7339 1.1878 0.042 Uiso 1 1 calc R . . H4B H 0.5718 0.6921 1.1303 0.042 Uiso 1 1 calc R . . H4C H 0.5166 0.6943 1.1178 0.042 Uiso 1 1 calc R . . C5 C 0.6907(3) 0.7625(3) 1.1089(5) 0.0192(15) Uani 1 1 d . . . C6 C 0.6696(3) 0.7115(3) 1.0481(5) 0.0246(17) Uani 1 1 d . . . H6A H 0.6913 0.6937 1.0586 0.037 Uiso 1 1 calc R . . H6B H 0.6732 0.7227 0.9858 0.037 Uiso 1 1 calc R . . H6C H 0.6311 0.6858 1.0615 0.037 Uiso 1 1 calc R . . C7 C 0.7530(3) 0.7964(3) 1.0902(5) 0.0253(17) Uani 1 1 d . . . H7A H 0.7690 0.7726 1.0947 0.038 Uiso 1 1 calc R . . H7B H 0.7704 0.8260 1.1337 0.038 Uiso 1 1 calc R . . H7C H 0.7591 0.8119 1.0303 0.038 Uiso 1 1 calc R . . C8 C 0.6818(3) 0.7446(3) 1.2070(5) 0.0286(18) Uani 1 1 d . . . H8A H 0.6429 0.7283 1.2218 0.043 Uiso 1 1 calc R . . H8B H 0.7033 0.7764 1.2450 0.043 Uiso 1 1 calc R . . H8C H 0.6934 0.7176 1.2165 0.043 Uiso 1 1 calc R . . C9 C 0.6742(3) 0.8594(3) 1.1551(5) 0.0214(16) Uani 1 1 d . . . C10 C 0.7348(3) 0.8894(3) 1.1830(6) 0.034(2) Uani 1 1 d . . . H10A H 0.7580 0.9030 1.1301 0.051 Uiso 1 1 calc R . . H10B H 0.7429 0.8640 1.2150 0.051 Uiso 1 1 calc R . . H10C H 0.7421 0.9202 1.2218 0.051 Uiso 1 1 calc R . . C11 C 0.6664(3) 0.9039(3) 1.1080(5) 0.0276(18) Uani 1 1 d . . . H11A H 0.6714 0.9320 1.1511 0.041 Uiso 1 1 calc R . . H11B H 0.6296 0.8872 1.0829 0.041 Uiso 1 1 calc R . . H11C H 0.6935 0.9207 1.0604 0.041 Uiso 1 1 calc R . . C12 C 0.6392(3) 0.8409(4) 1.2402(5) 0.0322(19) Uani 1 1 d . . . H12A H 0.6442 0.8130 1.2704 0.048 Uiso 1 1 calc R . . H12B H 0.6006 0.8255 1.2245 0.048 Uiso 1 1 calc R . . H12C H 0.6505 0.8723 1.2796 0.048 Uiso 1 1 calc R . . C13 C 0.5982(3) 0.8206(3) 0.6116(5) 0.0184(15) Uani 1 1 d . . . C14 C 0.5751(3) 0.8565(3) 0.6477(5) 0.0250(17) Uani 1 1 d . . . H14A H 0.5866 0.8882 0.6088 0.038 Uiso 1 1 calc R . . H14B H 0.5891 0.8690 0.7077 0.038 Uiso 1 1 calc R . . H14C H 0.5351 0.8349 0.6492 0.038 Uiso 1 1 calc R . . C15 C 0.5773(3) 0.7716(3) 0.6772(6) 0.0295(19) Uani 1 1 d . . . H15A H 0.5916 0.7852 0.7367 0.044 Uiso 1 1 calc R . . H15B H 0.5897 0.7466 0.6573 0.044 Uiso 1 1 calc R . . H15C H 0.5372 0.7522 0.6788 0.044 Uiso 1 1 calc R . . C16 C 0.5743(3) 0.7985(3) 0.5189(5) 0.0290(19) Uani 1 1 d . . . H16A H 0.5344 0.7802 0.5215 0.044 Uiso 1 1 calc R . . H16B H 0.5855 0.7724 0.4997 0.044 Uiso 1 1 calc R . . H16C H 0.5880 0.8289 0.4766 0.044 Uiso 1 1 calc R . . C17 C 0.7045(3) 0.8235(3) 0.5550(5) 0.0233(16) Uani 1 1 d . . . C18 C 0.6740(4) 0.7622(3) 0.5810(6) 0.0320(19) Uani 1 1 d . . . H18A H 0.6932 0.7444 0.5561 0.048 Uiso 1 1 calc R . . H18B H 0.6366 0.7445 0.5576 0.048 Uiso 1 1 calc R . . H18C H 0.6728 0.7588 0.6458 0.048 Uiso 1 1 calc R . . C19 C 0.7035(3) 0.8270(4) 0.4530(5) 0.0286(18) Uani 1 1 d . . . H19A H 0.7188 0.8058 0.4268 0.043 Uiso 1 1 calc R . . H19B H 0.7253 0.8653 0.4345 0.043 Uiso 1 1 calc R . . H19C H 0.6657 0.8122 0.4328 0.043 Uiso 1 1 calc R . . C20 C 0.7645(3) 0.8469(4) 0.5861(5) 0.0307(19) Uani 1 1 d . . . H20A H 0.7657 0.8471 0.6511 0.046 Uiso 1 1 calc R . . H20B H 0.7868 0.8843 0.5639 0.046 Uiso 1 1 calc R . . H20C H 0.7787 0.8240 0.5630 0.046 Uiso 1 1 calc R . . C21 C 0.7023(3) 0.9309(3) 0.5747(5) 0.0237(16) Uani 1 1 d . . . C22 C 0.6754(3) 0.9342(3) 0.4875(5) 0.0269(17) Uani 1 1 d . . . H22A H 0.6919 0.9724 0.4688 0.040 Uiso 1 1 calc R . . H22B H 0.6361 0.9192 0.4972 0.040 Uiso 1 1 calc R . . H22C H 0.6810 0.9131 0.4413 0.040 Uiso 1 1 calc R . . C23 C 0.7641(3) 0.9577(3) 0.5587(6) 0.035(2) Uani 1 1 d . . . H23A H 0.7709 0.9396 0.5089 0.053 Uiso 1 1 calc R . . H23B H 0.7818 0.9542 0.6122 0.053 Uiso 1 1 calc R . . H23C H 0.7790 0.9965 0.5447 0.053 Uiso 1 1 calc R . . C24 C 0.6948(4) 0.9651(3) 0.6471(6) 0.0332(19) Uani 1 1 d . . . H24A H 0.7152 1.0038 0.6307 0.050 Uiso 1 1 calc R . . H24B H 0.7086 0.9598 0.7038 0.050 Uiso 1 1 calc R . . H24C H 0.6559 0.9533 0.6529 0.050 Uiso 1 1 calc R . . Dy2 Dy 1.0000 1.0000 0.38726(3) 0.01392(12) Uani 1 3 d S . . P3 P 1.0000 1.0000 0.6343(2) 0.0154(6) Uani 1 3 d S . . P4 P 1.0000 1.0000 0.1396(2) 0.0119(6) Uani 1 3 d S . . O3 O 1.0000 1.0000 0.5328(6) 0.022(2) Uani 1 3 d S . . O4 O 1.0000 1.0000 0.2408(5) 0.0156(17) Uani 1 3 d S . . O41 O 1.0831(2) 0.9944(2) 0.3817(4) 0.0237(12) Uani 1 1 d . . . O42 O 0.9096(2) 0.9916(2) 0.3903(4) 0.0326(14) Uani 1 1 d . . . O43 O 1.0862(3) 0.9189(2) 0.3816(5) 0.0463(17) Uani 1 1 d . . . N41 N 1.0599(3) 0.9426(3) 0.3852(5) 0.0292(15) Uani 1 1 d . . . C25 C 0.9755(3) 1.0471(3) 0.6707(5) 0.0219(16) Uani 1 1 d . . . C26 C 1.0022(3) 1.0981(3) 0.6125(5) 0.0279(17) Uani 1 1 d . . . H26A H 0.9909 1.0878 0.5507 0.042 Uiso 1 1 calc R . . H26B H 1.0420 1.1153 0.6169 0.042 Uiso 1 1 calc R . . H26C H 0.9907 1.1239 0.6325 0.042 Uiso 1 1 calc R . . C27 C 0.9140(3) 1.0221(3) 0.6554(5) 0.0278(18) Uani 1 1 d . . . H27A H 0.9033 1.0495 0.6679 0.042 Uiso 1 1 calc R . . H27B H 0.8940 0.9907 0.6949 0.042 Uiso 1 1 calc R . . H27C H 0.9053 1.0102 0.5935 0.042 Uiso 1 1 calc R . . C28 C 1.0592(3) 0.9927(3) 0.1025(4) 0.0171(14) Uani 1 1 d . . . C29 C 1.0463(3) 0.9335(3) 0.1200(5) 0.0259(17) Uani 1 1 d . . . H29A H 1.0160 0.9083 0.0819 0.039 Uiso 1 1 calc R . . H29B H 1.0360 0.9241 0.1824 0.039 Uiso 1 1 calc R . . H29C H 1.0787 0.9305 0.1069 0.039 Uiso 1 1 calc R . . C30 C 1.1100(3) 1.0294(3) 0.1612(5) 0.0245(17) Uani 1 1 d . . . H30A H 1.1395 1.0221 0.1471 0.037 Uiso 1 1 calc R . . H30B H 1.1001 1.0214 0.2240 0.037 Uiso 1 1 calc R . . H30C H 1.1222 1.0680 0.1495 0.037 Uiso 1 1 calc R . . C31 C 1.0743(3) 1.0074(3) 0.0052(5) 0.0217(16) Uani 1 1 d . . . H31A H 1.0884 1.0466 -0.0033 0.033 Uiso 1 1 calc R . . H31B H 1.0417 0.9866 -0.0318 0.033 Uiso 1 1 calc R . . H31C H 1.1023 0.9984 -0.0119 0.033 Uiso 1 1 calc R . . C61 C 0.9874(3) 1.0639(3) 0.7689(5) 0.0285(18) Uani 1 1 d . . . H61A H 1.0270 1.0853 0.7781 0.043 Uiso 1 1 calc R . . H61B H 0.9720 1.0310 0.8061 0.043 Uiso 1 1 calc R . . H61C H 0.9708 1.0860 0.7850 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01526(16) 0.01548(16) 0.01332(15) 0.00081(14) -0.00103(13) 0.00602(14) P1 0.0137(8) 0.0154(8) 0.0138(9) 0.0012(7) 0.0001(7) 0.0073(7) P2 0.0145(9) 0.0165(9) 0.0134(9) -0.0001(7) -0.0030(7) 0.0067(7) O1 0.014(2) 0.015(2) 0.018(3) 0.002(2) 0.003(2) 0.003(2) O2 0.016(2) 0.015(2) 0.014(3) 0.001(2) 0.000(2) 0.006(2) O11 0.020(3) 0.025(3) 0.016(3) 0.005(2) 0.002(2) 0.008(2) O12 0.017(3) 0.026(3) 0.020(3) 0.005(2) 0.001(2) 0.005(2) O13 0.010(2) 0.017(2) 0.040(3) -0.004(2) -0.003(2) 0.001(2) O21 0.028(3) 0.019(3) 0.028(3) 0.004(2) 0.000(2) 0.010(2) O22 0.020(3) 0.019(3) 0.026(3) -0.002(2) -0.001(2) 0.009(2) O23 0.041(4) 0.042(4) 0.068(5) -0.006(3) -0.005(3) 0.032(3) O31 0.025(3) 0.023(3) 0.023(3) -0.003(2) 0.000(2) 0.008(2) O32 0.054(4) 0.029(3) 0.050(4) -0.009(3) -0.017(3) 0.029(3) O33 0.029(3) 0.026(3) 0.040(4) -0.004(3) -0.008(3) 0.016(3) N11 0.014(3) 0.018(3) 0.019(3) -0.002(3) 0.002(2) 0.007(2) N21 0.026(3) 0.036(4) 0.021(4) 0.008(3) -0.001(3) 0.020(3) N31 0.031(4) 0.023(3) 0.020(4) -0.001(3) -0.007(3) 0.015(3) C1 0.013(3) 0.019(4) 0.020(4) 0.010(3) 0.001(3) 0.002(3) C2 0.014(3) 0.022(4) 0.031(5) -0.008(3) -0.007(3) 0.003(3) C3 0.022(4) 0.031(4) 0.033(5) 0.003(4) 0.001(3) 0.014(3) C4 0.019(4) 0.033(4) 0.021(4) 0.010(3) 0.000(3) 0.006(3) C5 0.020(4) 0.025(4) 0.017(4) 0.006(3) 0.004(3) 0.015(3) C6 0.036(4) 0.023(4) 0.022(4) -0.005(3) -0.004(3) 0.020(4) C7 0.027(4) 0.029(4) 0.028(5) 0.002(3) 0.001(3) 0.020(4) C8 0.026(4) 0.036(5) 0.023(4) 0.008(4) 0.001(3) 0.015(4) C9 0.030(4) 0.018(4) 0.018(4) -0.004(3) -0.004(3) 0.013(3) C10 0.041(5) 0.028(4) 0.034(5) -0.019(4) -0.022(4) 0.019(4) C11 0.038(5) 0.023(4) 0.026(5) -0.008(3) -0.015(4) 0.018(4) C12 0.032(5) 0.050(5) 0.022(4) -0.003(4) -0.003(4) 0.027(4) C13 0.016(3) 0.022(4) 0.017(4) -0.005(3) -0.002(3) 0.010(3) C14 0.023(4) 0.036(4) 0.020(4) -0.007(3) -0.008(3) 0.018(4) C15 0.018(4) 0.031(4) 0.032(5) 0.013(4) 0.002(3) 0.007(3) C16 0.022(4) 0.037(5) 0.025(5) -0.001(4) 0.003(3) 0.012(4) C17 0.025(4) 0.034(4) 0.018(4) -0.004(3) -0.004(3) 0.020(4) C18 0.043(5) 0.031(4) 0.029(5) -0.014(4) -0.012(4) 0.023(4) C19 0.029(4) 0.045(5) 0.016(4) -0.003(4) -0.003(3) 0.023(4) C20 0.023(4) 0.054(5) 0.022(4) -0.006(4) -0.005(3) 0.024(4) C21 0.027(4) 0.019(4) 0.021(4) 0.004(3) -0.001(3) 0.008(3) C22 0.036(4) 0.032(4) 0.011(4) 0.008(3) 0.001(3) 0.016(4) C23 0.033(5) 0.027(4) 0.027(5) 0.006(4) 0.002(4) 0.000(4) C24 0.039(5) 0.023(4) 0.038(5) -0.006(4) -0.007(4) 0.016(4) Dy2 0.01627(17) 0.01627(17) 0.0092(3) 0.000 0.000 0.00813(9) P3 0.0167(9) 0.0167(9) 0.0129(16) 0.000 0.000 0.0083(5) P4 0.0135(8) 0.0135(8) 0.0085(14) 0.000 0.000 0.0068(4) O3 0.026(3) 0.026(3) 0.016(5) 0.000 0.000 0.0129(15) O4 0.018(3) 0.018(3) 0.010(4) 0.000 0.000 0.0092(13) O41 0.022(3) 0.019(3) 0.025(3) 0.005(2) 0.001(2) 0.006(2) O42 0.024(3) 0.033(3) 0.044(4) 0.002(3) 0.006(3) 0.016(3) O43 0.052(4) 0.037(4) 0.069(5) -0.001(3) -0.001(4) 0.037(3) N41 0.036(4) 0.030(4) 0.029(4) -0.001(3) -0.003(3) 0.022(3) C25 0.031(4) 0.030(4) 0.012(4) 0.002(3) 0.000(3) 0.021(4) C26 0.043(5) 0.019(4) 0.024(4) 0.006(3) 0.006(4) 0.018(4) C27 0.034(4) 0.035(4) 0.021(4) 0.002(3) 0.004(3) 0.022(4) C28 0.023(4) 0.026(4) 0.008(3) -0.003(3) -0.001(3) 0.016(3) C29 0.032(4) 0.036(4) 0.025(4) 0.003(3) 0.009(3) 0.028(4) C30 0.016(4) 0.033(4) 0.027(5) 0.001(4) 0.002(3) 0.014(3) C31 0.021(4) 0.031(4) 0.014(4) -0.004(3) 0.002(3) 0.014(3) C61 0.037(5) 0.038(5) 0.018(4) 0.000(3) 0.008(3) 0.024(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Dy1 O1 2.207(5) . ? Dy1 O2 2.212(5) . ? Dy1 O21 2.394(5) . ? Dy1 O11 2.415(5) . ? Dy1 O12 2.416(5) . ? Dy1 O33 2.418(5) . ? Dy1 O22 2.453(5) . ? Dy1 O31 2.453(5) . ? Dy1 N11 2.827(6) . ? Dy1 N21 2.844(6) . ? Dy1 N31 2.857(6) . ? P1 O1 1.516(5) . ? P1 C9 1.850(7) . ? P1 C1 1.864(7) . ? P1 C5 1.871(7) . ? P2 O2 1.512(5) . ? P2 C17 1.859(8) . ? P2 C21 1.860(7) . ? P2 C13 1.866(7) . ? O11 N11 1.266(7) . ? O12 N11 1.280(7) . ? O13 N11 1.227(7) . ? O21 N21 1.277(8) . ? O22 N21 1.281(8) . ? O23 N21 1.217(8) . ? O31 N31 1.280(8) . ? O32 N31 1.222(8) . ? O33 N31 1.271(8) . ? C1 C4 1.534(10) . ? C1 C2 1.542(11) . ? C1 C3 1.553(10) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.542(10) . ? C5 C7 1.552(10) . ? C5 C6 1.554(10) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.541(11) . ? C9 C12 1.542(11) . ? C9 C11 1.551(10) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C16 1.541(10) . ? C13 C14 1.551(10) . ? C13 C15 1.556(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.541(10) . ? C17 C20 1.550(10) . ? C17 C18 1.551(11) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.535(11) . ? C21 C24 1.541(11) . ? C21 C22 1.544(10) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Dy2 O3 2.193(9) . ? Dy2 O4 2.206(8) . ? Dy2 O41 2.431(5) 3_675 ? Dy2 O41 2.431(5) . ? Dy2 O41 2.431(5) 2_765 ? Dy2 O42 2.445(5) . ? Dy2 O42 2.445(5) 3_675 ? Dy2 O42 2.445(5) 2_765 ? Dy2 N41 2.870(6) 3_675 ? Dy2 N41 2.870(6) . ? Dy2 N41 2.870(6) 2_765 ? P3 O3 1.530(10) . ? P3 C25 1.864(7) 2_765 ? P3 C25 1.864(7) . ? P3 C25 1.864(7) 3_675 ? P4 O4 1.525(8) . ? P4 C28 1.870(7) 3_675 ? P4 C28 1.870(7) 2_765 ? P4 C28 1.870(7) . ? O41 N41 1.272(8) . ? O42 N41 1.263(9) 3_675 ? O43 N41 1.225(8) . ? N41 O42 1.263(9) 2_765 ? C25 C26 1.525(10) . ? C25 C27 1.529(11) . ? C25 C61 1.538(10) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C31 1.526(10) . ? C28 C29 1.546(10) . ? C28 C30 1.557(10) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Dy1 O2 147.89(17) . . ? O1 Dy1 O21 91.14(18) . . ? O2 Dy1 O21 92.45(18) . . ? O1 Dy1 O11 78.76(17) . . ? O2 Dy1 O11 133.30(17) . . ? O21 Dy1 O11 81.22(18) . . ? O1 Dy1 O12 131.90(18) . . ? O2 Dy1 O12 80.06(18) . . ? O21 Dy1 O12 79.61(17) . . ? O11 Dy1 O12 53.25(17) . . ? O1 Dy1 O33 97.85(19) . . ? O2 Dy1 O33 92.73(19) . . ? O21 Dy1 O33 153.98(18) . . ? O11 Dy1 O33 76.71(18) . . ? O12 Dy1 O33 76.21(18) . . ? O1 Dy1 O22 77.80(18) . . ? O2 Dy1 O22 79.00(18) . . ? O21 Dy1 O22 53.13(18) . . ? O11 Dy1 O22 127.44(17) . . ? O12 Dy1 O22 126.67(17) . . ? O33 Dy1 O22 152.77(18) . . ? O1 Dy1 O31 81.78(18) . . ? O2 Dy1 O31 80.81(18) . . ? O21 Dy1 O31 153.32(18) . . ? O11 Dy1 O31 121.94(17) . . ? O12 Dy1 O31 123.86(17) . . ? O33 Dy1 O31 52.66(17) . . ? O22 Dy1 O31 100.19(17) . . ? O1 Dy1 N11 105.26(18) . . ? O2 Dy1 N11 106.81(18) . . ? O21 Dy1 N11 80.80(17) . . ? O11 Dy1 N11 26.50(16) . . ? O12 Dy1 N11 26.83(17) . . ? O33 Dy1 N11 73.29(17) . . ? O22 Dy1 N11 133.91(17) . . ? O31 Dy1 N11 125.88(17) . . ? O1 Dy1 N21 82.98(18) . . ? O2 Dy1 N21 86.18(19) . . ? O21 Dy1 N21 26.46(18) . . ? O11 Dy1 N21 104.19(18) . . ? O12 Dy1 N21 103.79(18) . . ? O33 Dy1 N21 178.9(2) . . ? O22 Dy1 N21 26.70(17) . . ? O31 Dy1 N21 126.87(19) . . ? N11 Dy1 N21 107.22(18) . . ? O1 Dy1 N31 91.32(18) . . ? O2 Dy1 N31 84.95(18) . . ? O21 Dy1 N31 177.35(18) . . ? O11 Dy1 N31 100.24(17) . . ? O12 Dy1 N31 99.46(18) . . ? O33 Dy1 N31 26.22(17) . . ? O22 Dy1 N31 126.56(18) . . ? O31 Dy1 N31 26.53(17) . . ? N11 Dy1 N31 99.51(17) . . ? N21 Dy1 N31 153.24(19) . . ? O1 P1 C9 107.4(3) . . ? O1 P1 C1 107.9(3) . . ? C9 P1 C1 111.7(3) . . ? O1 P1 C5 106.5(3) . . ? C9 P1 C5 111.6(3) . . ? C1 P1 C5 111.4(3) . . ? O2 P2 C17 106.3(3) . . ? O2 P2 C21 106.8(3) . . ? C17 P2 C21 111.8(4) . . ? O2 P2 C13 108.2(3) . . ? C17 P2 C13 111.8(3) . . ? C21 P2 C13 111.6(3) . . ? P1 O1 Dy1 173.7(3) . . ? P2 O2 Dy1 176.0(3) . . ? N11 O11 Dy1 95.2(4) . . ? N11 O12 Dy1 94.8(4) . . ? N21 O21 Dy1 96.9(4) . . ? N21 O22 Dy1 94.0(4) . . ? N31 O31 Dy1 94.6(4) . . ? N31 O33 Dy1 96.6(4) . . ? O13 N11 O11 122.1(6) . . ? O13 N11 O12 121.5(6) . . ? O11 N11 O12 116.4(5) . . ? O13 N11 Dy1 176.7(5) . . ? O11 N11 Dy1 58.3(3) . . ? O12 N11 Dy1 58.4(3) . . ? O23 N21 O21 122.7(7) . . ? O23 N21 O22 121.4(7) . . ? O21 N21 O22 115.9(6) . . ? O23 N21 Dy1 175.3(6) . . ? O21 N21 Dy1 56.7(3) . . ? O22 N21 Dy1 59.3(3) . . ? O32 N31 O33 121.6(7) . . ? O32 N31 O31 122.6(6) . . ? O33 N31 O31 115.8(6) . . ? O32 N31 Dy1 173.6(5) . . ? O33 N31 Dy1 57.2(3) . . ? O31 N31 Dy1 58.8(3) . . ? C4 C1 C2 108.9(6) . . ? C4 C1 C3 107.4(6) . . ? C2 C1 C3 105.6(6) . . ? C4 C1 P1 112.8(5) . . ? C2 C1 P1 109.1(5) . . ? C3 C1 P1 112.7(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C5 C7 109.0(6) . . ? C8 C5 C6 109.6(6) . . ? C7 C5 C6 104.7(6) . . ? C8 C5 P1 114.6(5) . . ? C7 C5 P1 108.7(5) . . ? C6 C5 P1 109.7(5) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C12 107.9(6) . . ? C10 C9 C11 104.4(6) . . ? C12 C9 C11 109.2(6) . . ? C10 C9 P1 111.8(5) . . ? C12 C9 P1 114.3(5) . . ? C11 C9 P1 108.7(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C13 C14 109.9(6) . . ? C16 C13 C15 108.6(6) . . ? C14 C13 C15 105.1(6) . . ? C16 C13 P2 114.1(5) . . ? C14 C13 P2 110.0(5) . . ? C15 C13 P2 108.7(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C20 109.0(6) . . ? C19 C17 C18 107.9(6) . . ? C20 C17 C18 106.2(6) . . ? C19 C17 P2 115.0(5) . . ? C20 C17 P2 108.7(5) . . ? C18 C17 P2 109.7(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 C24 106.3(6) . . ? C23 C21 C22 108.1(6) . . ? C24 C21 C22 109.8(6) . . ? C23 C21 P2 110.4(5) . . ? C24 C21 P2 109.2(5) . . ? C22 C21 P2 113.0(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O3 Dy2 O4 180.000(5) . . ? O3 Dy2 O41 91.97(14) . 3_675 ? O4 Dy2 O41 88.03(14) . 3_675 ? O3 Dy2 O41 91.97(14) . . ? O4 Dy2 O41 88.03(14) . . ? O41 Dy2 O41 119.883(17) 3_675 . ? O3 Dy2 O41 91.97(13) . 2_765 ? O4 Dy2 O41 88.03(13) . 2_765 ? O41 Dy2 O41 119.883(18) 3_675 2_765 ? O41 Dy2 O41 119.883(19) . 2_765 ? O3 Dy2 O42 88.92(15) . . ? O4 Dy2 O42 91.08(15) . . ? O41 Dy2 O42 52.07(18) 3_675 . ? O41 Dy2 O42 171.95(18) . . ? O41 Dy2 O42 68.06(18) 2_765 . ? O3 Dy2 O42 88.92(15) . 3_675 ? O4 Dy2 O42 91.08(15) . 3_675 ? O41 Dy2 O42 171.95(18) 3_675 3_675 ? O41 Dy2 O42 68.06(18) . 3_675 ? O41 Dy2 O42 52.07(18) 2_765 3_675 ? O42 Dy2 O42 119.965(11) . 3_675 ? O3 Dy2 O42 88.92(15) . 2_765 ? O4 Dy2 O42 91.08(15) . 2_765 ? O41 Dy2 O42 68.06(18) 3_675 2_765 ? O41 Dy2 O42 52.07(18) . 2_765 ? O41 Dy2 O42 171.95(18) 2_765 2_765 ? O42 Dy2 O42 119.965(13) . 2_765 ? O42 Dy2 O42 119.965(13) 3_675 2_765 ? O3 Dy2 N41 90.61(14) . 3_675 ? O4 Dy2 N41 89.39(14) . 3_675 ? O41 Dy2 N41 26.13(18) 3_675 3_675 ? O41 Dy2 N41 146.01(18) . 3_675 ? O41 Dy2 N41 93.88(18) 2_765 3_675 ? O42 Dy2 N41 25.95(19) . 3_675 ? O42 Dy2 N41 145.89(19) 3_675 3_675 ? O42 Dy2 N41 94.12(19) 2_765 3_675 ? O3 Dy2 N41 90.61(14) . . ? O4 Dy2 N41 89.39(14) . . ? O41 Dy2 N41 93.88(18) 3_675 . ? O41 Dy2 N41 26.13(18) . . ? O41 Dy2 N41 146.01(18) 2_765 . ? O42 Dy2 N41 145.89(19) . . ? O42 Dy2 N41 94.12(19) 3_675 . ? O42 Dy2 N41 25.95(19) 2_765 . ? N41 Dy2 N41 119.989(7) 3_675 . ? O3 Dy2 N41 90.61(14) . 2_765 ? O4 Dy2 N41 89.39(14) . 2_765 ? O41 Dy2 N41 146.01(18) 3_675 2_765 ? O41 Dy2 N41 93.88(18) . 2_765 ? O41 Dy2 N41 26.13(18) 2_765 2_765 ? O42 Dy2 N41 94.12(19) . 2_765 ? O42 Dy2 N41 25.95(19) 3_675 2_765 ? O42 Dy2 N41 145.89(19) 2_765 2_765 ? N41 Dy2 N41 119.989(6) 3_675 2_765 ? N41 Dy2 N41 119.989(9) . 2_765 ? O3 P3 C25 107.1(2) . 2_765 ? O3 P3 C25 107.1(2) . . ? C25 P3 C25 111.7(2) 2_765 . ? O3 P3 C25 107.1(2) . 3_675 ? C25 P3 C25 111.7(2) 2_765 3_675 ? C25 P3 C25 111.7(2) . 3_675 ? O4 P4 C28 107.4(2) . 3_675 ? O4 P4 C28 107.4(2) . 2_765 ? C28 P4 C28 111.5(2) 3_675 2_765 ? O4 P4 C28 107.4(2) . . ? C28 P4 C28 111.5(2) 3_675 . ? C28 P4 C28 111.5(2) 2_765 . ? P3 O3 Dy2 180.000(1) . . ? P4 O4 Dy2 180.000(1) . . ? N41 O41 Dy2 96.6(4) . . ? N41 O42 Dy2 96.2(4) 3_675 . ? O43 N41 O42 123.2(7) . 2_765 ? O43 N41 O41 121.6(7) . . ? O42 N41 O41 115.2(6) 2_765 . ? O43 N41 Dy2 177.8(6) . . ? O42 N41 Dy2 57.9(4) 2_765 . ? O41 N41 Dy2 57.3(3) . . ? C26 C25 C27 105.1(6) . . ? C26 C25 C61 109.5(7) . . ? C27 C25 C61 108.1(6) . . ? C26 C25 P3 108.7(5) . . ? C27 C25 P3 111.5(5) . . ? C61 C25 P3 113.6(5) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C31 C28 C29 109.9(6) . . ? C31 C28 C30 109.0(6) . . ? C29 C28 C30 105.4(6) . . ? C31 C28 P4 113.6(5) . . ? C29 C28 P4 109.1(5) . . ? C30 C28 P4 109.5(5) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C25 C61 H61A 109.5 . . ? C25 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C25 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.364 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.138 #===END data_Er _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Er _chemical_melting_point ? _chemical_formula_moiety 'C32 H72 Er1.33 N4 O14.67 P2.67' _chemical_formula_sum 'C32 H72 Er1.33 N4 O14.67 P2.67' _chemical_formula_weight 1053.20 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' 'Er' 'Er' -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R3 _symmetry_space_group_name_Hall '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' _cell_length_a 28.2812(4) _cell_length_b 28.2812(4) _cell_length_c 15.0594(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10431.2(3) _cell_formula_units_Z 9 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 24280 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4860 _exptl_absorpt_coefficient_mu 2.559 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6559 _exptl_absorpt_correction_T_max 0.8215 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '9.091' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27280 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10577 _reflns_number_gt 9846 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Crystal structure is a racemic twin with 47-53 % ratio Refined BASF = 0.47086 ; _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^)+(0.0000P)^2^+16.5578P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.471(5) _refine_ls_number_reflns 10577 _refine_ls_number_parameters 518 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0566 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.004 _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 Er1 Er 0.712386(7) 0.864854(7) 0.853313(12) 0.01436(5) Uani 1 1 d . . . P1 P 0.65852(4) 0.80382(4) 1.07435(7) 0.0137(2) Uani 1 1 d . . . P2 P 0.67445(4) 0.85977(4) 0.61588(7) 0.0148(2) Uani 1 1 d . . . O1 O 0.68414(11) 0.83006(11) 0.98687(19) 0.0156(7) Uani 1 1 d . . . O2 O 0.69209(12) 0.86357(11) 0.71206(19) 0.0153(6) Uani 1 1 d . . . O11 O 0.79172(11) 0.92040(11) 0.94022(19) 0.0200(7) Uani 1 1 d . . . O12 O 0.79585(12) 0.94025(12) 0.8006(2) 0.0230(7) Uani 1 1 d . . . O13 O 0.86873(11) 0.98433(11) 0.8836(2) 0.0225(7) Uani 1 1 d . . . O21 O 0.69709(13) 0.93822(12) 0.8839(2) 0.0231(7) Uani 1 1 d . . . O22 O 0.62401(12) 0.85925(13) 0.8626(2) 0.0203(7) Uani 1 1 d . . . O23 O 0.61587(14) 0.92954(14) 0.9001(3) 0.0416(10) Uani 1 1 d . . . O31 O 0.68219(12) 0.76981(12) 0.8190(2) 0.0241(7) Uani 1 1 d . . . O32 O 0.73999(15) 0.74273(14) 0.7825(2) 0.0405(10) Uani 1 1 d . . . O33 O 0.76931(13) 0.82650(12) 0.8268(2) 0.0283(8) Uani 1 1 d . . . N11 N 0.82116(14) 0.95003(14) 0.8753(3) 0.0186(8) Uani 1 1 d . . . N21 N 0.64429(16) 0.90959(16) 0.8824(3) 0.0250(9) Uani 1 1 d . . . N31 N 0.73091(16) 0.77801(15) 0.8087(3) 0.0251(9) Uani 1 1 d . . . C1 C 0.58278(16) 0.75948(17) 1.0574(3) 0.0166(9) Uani 1 1 d . . . C2 C 0.57317(17) 0.73102(18) 0.9661(3) 0.0237(10) Uani 1 1 d . . . H2A H 0.5919 0.7097 0.9645 0.035 Uiso 1 1 calc R . . H2B H 0.5876 0.7586 0.9191 0.035 Uiso 1 1 calc R . . H2C H 0.5339 0.7067 0.9570 0.035 Uiso 1 1 calc R . . C3 C 0.55325(17) 0.79254(19) 1.0520(3) 0.0258(11) Uani 1 1 d . . . H3A H 0.5149 0.7682 1.0361 0.039 Uiso 1 1 calc R . . H3B H 0.5707 0.8210 1.0068 0.039 Uiso 1 1 calc R . . H3C H 0.5553 0.8094 1.1098 0.039 Uiso 1 1 calc R . . C4 C 0.55533(17) 0.71591(19) 1.1304(3) 0.0260(11) Uani 1 1 d . . . H4A H 0.5624 0.7338 1.1885 0.039 Uiso 1 1 calc R . . H4B H 0.5702 0.6912 1.1293 0.039 Uiso 1 1 calc R . . H4C H 0.5159 0.6950 1.1199 0.039 Uiso 1 1 calc R . . C5 C 0.69060(17) 0.76251(17) 1.1085(3) 0.0181(9) Uani 1 1 d . . . C6 C 0.66957(19) 0.71160(17) 1.0487(3) 0.0247(11) Uani 1 1 d . . . H6A H 0.6910 0.6936 1.0599 0.037 Uiso 1 1 calc R . . H6B H 0.6734 0.7226 0.9862 0.037 Uiso 1 1 calc R . . H6C H 0.6310 0.6862 1.0620 0.037 Uiso 1 1 calc R . . C7 C 0.75284(17) 0.79615(19) 1.0902(3) 0.0231(10) Uani 1 1 d . . . H7A H 0.7689 0.7727 1.0977 0.035 Uiso 1 1 calc R . . H7B H 0.7698 0.8267 1.1321 0.035 Uiso 1 1 calc R . . H7C H 0.7591 0.8103 1.0294 0.035 Uiso 1 1 calc R . . C8 C 0.68180(18) 0.74462(19) 1.2066(3) 0.0256(10) Uani 1 1 d . . . H8A H 0.6426 0.7243 1.2196 0.038 Uiso 1 1 calc R . . H8B H 0.6997 0.7770 1.2448 0.038 Uiso 1 1 calc R . . H8C H 0.6975 0.7212 1.2178 0.038 Uiso 1 1 calc R . . C9 C 0.67429(17) 0.85978(17) 1.1552(3) 0.0203(10) Uani 1 1 d . . . C10 C 0.73457(18) 0.88896(19) 1.1831(3) 0.0308(12) Uani 1 1 d . . . H10A H 0.7577 0.9016 1.1301 0.046 Uiso 1 1 calc R . . H10B H 0.7420 0.8636 1.2162 0.046 Uiso 1 1 calc R . . H10C H 0.7424 0.9203 1.2208 0.046 Uiso 1 1 calc R . . C11 C 0.66639(19) 0.90380(18) 1.1070(3) 0.0256(11) Uani 1 1 d . . . H11A H 0.6751 0.9341 1.1478 0.038 Uiso 1 1 calc R . . H11B H 0.6284 0.8877 1.0873 0.038 Uiso 1 1 calc R . . H11C H 0.6907 0.9174 1.0553 0.038 Uiso 1 1 calc R . . C12 C 0.6388(2) 0.8405(2) 1.2398(3) 0.0323(12) Uani 1 1 d . . . H12A H 0.6434 0.8122 1.2693 0.048 Uiso 1 1 calc R . . H12B H 0.6003 0.8256 1.2237 0.048 Uiso 1 1 calc R . . H12C H 0.6500 0.8716 1.2802 0.048 Uiso 1 1 calc R . . C13 C 0.59837(17) 0.82046(18) 0.6123(3) 0.0214(10) Uani 1 1 d . . . C14 C 0.57469(19) 0.8555(2) 0.6472(3) 0.0290(11) Uani 1 1 d . . . H14A H 0.5846 0.8862 0.6066 0.043 Uiso 1 1 calc R . . H14B H 0.5896 0.8695 0.7063 0.043 Uiso 1 1 calc R . . H14C H 0.5348 0.8332 0.6507 0.043 Uiso 1 1 calc R . . C15 C 0.57787(19) 0.77134(19) 0.6771(3) 0.0301(12) Uani 1 1 d . . . H15A H 0.5939 0.7845 0.7359 0.045 Uiso 1 1 calc R . . H15B H 0.5887 0.7456 0.6548 0.045 Uiso 1 1 calc R . . H15C H 0.5380 0.7529 0.6815 0.045 Uiso 1 1 calc R . . C16 C 0.5747(2) 0.7986(2) 0.5192(3) 0.0299(12) Uani 1 1 d . . . H16A H 0.5349 0.7820 0.5208 0.045 Uiso 1 1 calc R . . H16B H 0.5843 0.7712 0.5011 0.045 Uiso 1 1 calc R . . H16C H 0.5899 0.8289 0.4765 0.045 Uiso 1 1 calc R . . C17 C 0.70570(18) 0.82414(18) 0.5550(3) 0.0197(10) Uani 1 1 d . . . C18 C 0.6746(2) 0.76286(19) 0.5815(3) 0.0297(12) Uani 1 1 d . . . H18A H 0.6939 0.7449 0.5578 0.045 Uiso 1 1 calc R . . H18B H 0.6376 0.7453 0.5570 0.045 Uiso 1 1 calc R . . H18C H 0.6727 0.7596 0.6463 0.045 Uiso 1 1 calc R . . C19 C 0.7041(2) 0.8281(2) 0.4537(3) 0.0305(12) Uani 1 1 d . . . H19A H 0.7182 0.8061 0.4265 0.046 Uiso 1 1 calc R . . H19B H 0.7268 0.8663 0.4354 0.046 Uiso 1 1 calc R . . H19C H 0.6664 0.8144 0.4343 0.046 Uiso 1 1 calc R . . C20 C 0.76469(18) 0.8475(2) 0.5865(3) 0.0253(11) Uani 1 1 d . . . H20A H 0.7660 0.8504 0.6514 0.038 Uiso 1 1 calc R . . H20B H 0.7875 0.8838 0.5605 0.038 Uiso 1 1 calc R . . H20C H 0.7783 0.8233 0.5677 0.038 Uiso 1 1 calc R . . C21 C 0.70192(18) 0.93114(17) 0.5745(3) 0.0227(10) Uani 1 1 d . . . C22 C 0.67501(19) 0.93450(19) 0.4882(3) 0.0271(11) Uani 1 1 d . . . H22A H 0.6931 0.9724 0.4676 0.041 Uiso 1 1 calc R . . H22B H 0.6363 0.9216 0.4990 0.041 Uiso 1 1 calc R . . H22C H 0.6785 0.9116 0.4428 0.041 Uiso 1 1 calc R . . C23 C 0.76415(18) 0.95872(19) 0.5602(3) 0.0331(12) Uani 1 1 d . . . H23A H 0.7717 0.9419 0.5093 0.050 Uiso 1 1 calc R . . H23B H 0.7813 0.9541 0.6135 0.050 Uiso 1 1 calc R . . H23C H 0.7790 0.9977 0.5487 0.050 Uiso 1 1 calc R . . C24 C 0.6942(2) 0.96490(18) 0.6482(3) 0.0282(11) Uani 1 1 d . . . H24A H 0.7091 1.0027 0.6281 0.042 Uiso 1 1 calc R . . H24B H 0.7135 0.9644 0.7020 0.042 Uiso 1 1 calc R . . H24C H 0.6553 0.9490 0.6613 0.042 Uiso 1 1 calc R . . Er2 Er 1.0000 1.0000 0.386840(19) 0.01347(7) Uani 1 3 d S . . P3 P 1.0000 1.0000 0.63375(12) 0.0137(4) Uani 1 3 d S . . P4 P 1.0000 1.0000 0.14003(12) 0.0119(4) Uani 1 3 d S . . O3 O 1.0000 1.0000 0.5321(3) 0.0150(12) Uani 1 3 d S . . O4 O 1.0000 1.0000 0.2410(3) 0.0151(11) Uani 1 3 d S . . O41 O 1.08214(12) 0.99442(13) 0.3818(2) 0.0226(7) Uani 1 1 d . . . O42 O 0.91124(13) 0.99295(13) 0.3901(2) 0.0301(8) Uani 1 1 d . . . O43 O 1.08447(15) 0.91847(15) 0.3822(3) 0.0473(10) Uani 1 1 d . . . N41 N 1.05892(17) 0.94259(16) 0.3845(3) 0.0249(9) Uani 1 1 d . . . C25 C 0.97478(18) 1.04654(18) 0.6709(3) 0.0181(9) Uani 1 1 d . . . C26 C 1.0014(2) 1.09801(18) 0.6112(3) 0.0283(11) Uani 1 1 d . . . H26A H 0.9905 1.0874 0.5493 0.042 Uiso 1 1 calc R . . H26B H 1.0412 1.1158 0.6160 0.042 Uiso 1 1 calc R . . H26C H 0.9893 1.1234 0.6304 0.042 Uiso 1 1 calc R . . C27 C 0.91276(18) 1.0207(2) 0.6546(3) 0.0285(11) Uani 1 1 d . . . H27A H 0.9017 1.0479 0.6660 0.043 Uiso 1 1 calc R . . H27B H 0.8928 0.9895 0.6945 0.043 Uiso 1 1 calc R . . H27C H 0.9044 1.0083 0.5928 0.043 Uiso 1 1 calc R . . C28 C 1.05965(16) 0.99297(17) 0.1027(3) 0.0158(9) Uani 1 1 d . . . C29 C 1.04678(19) 0.93388(18) 0.1199(3) 0.0260(11) Uani 1 1 d . . . H29A H 1.0175 0.9089 0.0800 0.039 Uiso 1 1 calc R . . H29B H 1.0351 0.9239 0.1817 0.039 Uiso 1 1 calc R . . H29C H 1.0796 0.9313 0.1090 0.039 Uiso 1 1 calc R . . C30 C 1.10987(18) 1.0298(2) 0.1615(3) 0.0252(11) Uani 1 1 d . . . H30A H 1.1398 1.0231 0.1470 0.038 Uiso 1 1 calc R . . H30B H 1.1000 1.0212 0.2242 0.038 Uiso 1 1 calc R . . H30C H 1.1215 1.0682 0.1505 0.038 Uiso 1 1 calc R . . C31 C 1.07461(17) 1.00666(18) 0.0044(3) 0.0198(10) Uani 1 1 d . . . H31A H 1.0853 1.0449 -0.0065 0.030 Uiso 1 1 calc R . . H31B H 1.0430 0.9829 -0.0326 0.030 Uiso 1 1 calc R . . H31C H 1.1051 1.0009 -0.0105 0.030 Uiso 1 1 calc R . . C61 C 0.98775(19) 1.06389(18) 0.7684(3) 0.0226(10) Uani 1 1 d . . . H61A H 1.0274 1.0866 0.7760 0.034 Uiso 1 1 calc R . . H61B H 0.9740 1.0314 0.8060 0.034 Uiso 1 1 calc R . . H61C H 0.9702 1.0848 0.7856 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01449(10) 0.01435(10) 0.01234(9) 0.00113(8) -0.00059(8) 0.00577(8) P1 0.0137(5) 0.0161(6) 0.0120(6) 0.0008(4) 0.0006(4) 0.0081(5) P2 0.0141(6) 0.0159(6) 0.0128(6) -0.0003(4) -0.0022(4) 0.0063(5) O1 0.0172(15) 0.0174(16) 0.0107(16) 0.0030(12) 0.0012(12) 0.0075(14) O2 0.0171(16) 0.0188(16) 0.0121(17) 0.0011(12) -0.0025(13) 0.0106(13) O11 0.0183(16) 0.0209(16) 0.0135(16) 0.0023(13) 0.0001(12) 0.0044(14) O12 0.0205(17) 0.0261(18) 0.0141(17) 0.0005(13) -0.0022(13) 0.0055(14) O13 0.0123(15) 0.0195(16) 0.0306(19) -0.0040(13) -0.0010(13) 0.0041(13) O21 0.0249(18) 0.0190(17) 0.027(2) 0.0013(14) -0.0013(14) 0.0120(15) O22 0.0210(17) 0.0202(17) 0.0208(18) -0.0002(13) -0.0014(14) 0.0111(14) O23 0.040(2) 0.039(2) 0.063(3) -0.0068(19) -0.0072(19) 0.0333(19) O31 0.0257(18) 0.0189(17) 0.0267(19) -0.0021(14) -0.0026(14) 0.0105(15) O32 0.053(2) 0.032(2) 0.053(3) -0.0095(18) -0.0122(19) 0.034(2) O33 0.0277(19) 0.0202(17) 0.038(2) -0.0036(15) -0.0045(16) 0.0129(16) N11 0.017(2) 0.0172(19) 0.025(2) -0.0019(16) -0.0017(16) 0.0108(17) N21 0.031(2) 0.031(2) 0.018(2) 0.0029(17) -0.0046(17) 0.019(2) N31 0.033(2) 0.025(2) 0.023(2) -0.0017(17) -0.0087(18) 0.018(2) C1 0.009(2) 0.021(2) 0.017(2) 0.0050(18) 0.0032(17) 0.0054(18) C2 0.016(2) 0.019(2) 0.030(3) -0.001(2) -0.008(2) 0.0040(19) C3 0.016(2) 0.036(3) 0.026(3) 0.004(2) 0.0025(19) 0.014(2) C4 0.013(2) 0.033(3) 0.027(3) 0.011(2) 0.0054(19) 0.008(2) C5 0.019(2) 0.020(2) 0.017(2) 0.0029(18) -0.0004(18) 0.011(2) C6 0.026(3) 0.019(2) 0.032(3) 0.000(2) 0.000(2) 0.013(2) C7 0.018(2) 0.028(3) 0.030(3) 0.002(2) 0.001(2) 0.016(2) C8 0.028(3) 0.032(3) 0.022(3) 0.008(2) -0.003(2) 0.018(2) C9 0.021(2) 0.021(2) 0.021(3) -0.0070(19) -0.0031(19) 0.013(2) C10 0.029(3) 0.026(3) 0.036(3) -0.014(2) -0.015(2) 0.013(2) C11 0.029(3) 0.021(3) 0.030(3) -0.010(2) -0.007(2) 0.016(2) C12 0.046(3) 0.045(3) 0.018(3) -0.009(2) -0.001(2) 0.032(3) C13 0.015(2) 0.025(2) 0.020(2) -0.0030(19) -0.0064(18) 0.006(2) C14 0.021(3) 0.036(3) 0.031(3) 0.000(2) -0.001(2) 0.016(2) C15 0.021(3) 0.026(3) 0.031(3) 0.007(2) -0.001(2) 0.003(2) C16 0.024(3) 0.032(3) 0.027(3) -0.007(2) -0.009(2) 0.010(2) C17 0.024(2) 0.025(2) 0.015(2) -0.0066(18) -0.0043(18) 0.016(2) C18 0.037(3) 0.028(3) 0.030(3) -0.006(2) -0.004(2) 0.021(2) C19 0.035(3) 0.042(3) 0.021(3) -0.006(2) 0.002(2) 0.024(3) C20 0.024(3) 0.039(3) 0.020(3) -0.007(2) -0.004(2) 0.020(2) C21 0.028(3) 0.015(2) 0.018(2) 0.0040(18) -0.0011(19) 0.005(2) C22 0.032(3) 0.028(3) 0.019(3) 0.002(2) -0.003(2) 0.014(2) C23 0.022(3) 0.025(3) 0.032(3) 0.006(2) 0.003(2) -0.004(2) C24 0.037(3) 0.016(2) 0.029(3) -0.001(2) -0.008(2) 0.011(2) Er2 0.01552(11) 0.01552(11) 0.00938(16) 0.000 0.000 0.00776(5) P3 0.0159(6) 0.0159(6) 0.0092(9) 0.000 0.000 0.0080(3) P4 0.0137(6) 0.0137(6) 0.0084(9) 0.000 0.000 0.0069(3) O3 0.0159(17) 0.0159(17) 0.013(3) 0.000 0.000 0.0079(9) O4 0.0197(17) 0.0197(17) 0.006(3) 0.000 0.000 0.0098(8) O41 0.0198(17) 0.0197(18) 0.027(2) 0.0009(14) 0.0002(14) 0.0086(15) O42 0.0201(17) 0.027(2) 0.046(2) 0.0000(16) 0.0036(16) 0.0136(16) O43 0.056(3) 0.050(2) 0.062(3) -0.001(2) -0.006(2) 0.046(2) N41 0.034(2) 0.031(2) 0.020(2) -0.0018(18) -0.0032(18) 0.025(2) C25 0.023(2) 0.024(2) 0.011(2) -0.0016(18) -0.0011(18) 0.016(2) C26 0.045(3) 0.022(3) 0.025(3) 0.008(2) 0.005(2) 0.022(2) C27 0.033(3) 0.044(3) 0.018(3) 0.001(2) 0.001(2) 0.026(3) C28 0.017(2) 0.023(2) 0.010(2) 0.0006(17) 0.0013(17) 0.0123(19) C29 0.036(3) 0.028(3) 0.025(3) 0.005(2) 0.003(2) 0.024(2) C30 0.021(2) 0.041(3) 0.017(2) 0.005(2) 0.0018(19) 0.018(2) C31 0.017(2) 0.028(2) 0.012(2) -0.0013(18) 0.0055(17) 0.010(2) C61 0.031(3) 0.024(2) 0.016(2) -0.0065(19) 0.003(2) 0.016(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Er1 O2 2.199(3) . ? Er1 O1 2.206(3) . ? Er1 O21 2.367(3) . ? Er1 O33 2.382(3) . ? Er1 O11 2.385(3) . ? Er1 O12 2.391(3) . ? Er1 O22 2.428(3) . ? Er1 O31 2.434(3) . ? Er1 N21 2.817(4) . ? Er1 N11 2.822(4) . ? Er1 N31 2.836(4) . ? P1 O1 1.508(3) . ? P1 C9 1.866(4) . ? P1 C5 1.874(4) . ? P1 C1 1.881(4) . ? P2 O2 1.518(3) . ? P2 C13 1.864(4) . ? P2 C21 1.870(4) . ? P2 C17 1.878(4) . ? O11 N11 1.286(4) . ? O12 N11 1.287(4) . ? O13 N11 1.209(4) . ? O21 N21 1.295(5) . ? O22 N21 1.276(5) . ? O23 N21 1.220(5) . ? O31 N31 1.287(5) . ? O32 N31 1.214(4) . ? O33 N31 1.283(4) . ? C1 C3 1.536(6) . ? C1 C4 1.540(6) . ? C1 C2 1.547(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.543(6) . ? C5 C8 1.542(6) . ? C5 C7 1.550(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.535(6) . ? C9 C12 1.543(6) . ? C9 C11 1.551(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.540(6) . ? C13 C16 1.544(6) . ? C13 C15 1.553(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C20 1.530(6) . ? C17 C19 1.533(6) . ? C17 C18 1.553(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.533(6) . ? C21 C23 1.542(6) . ? C21 C24 1.549(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Er2 O3 2.187(5) . ? Er2 O4 2.196(5) . ? Er2 O41 2.407(3) 3_675 ? Er2 O41 2.407(3) 2_765 ? Er2 O41 2.407(3) . ? Er2 O42 2.417(3) 3_675 ? Er2 O42 2.417(3) . ? Er2 O42 2.417(3) 2_765 ? Er2 N41 2.849(4) 3_675 ? Er2 N41 2.849(4) 2_765 ? Er2 N41 2.849(4) . ? P3 O3 1.531(6) . ? P3 C25 1.869(4) 3_675 ? P3 C25 1.869(4) 2_765 ? P3 C25 1.869(4) . ? P4 O4 1.521(5) . ? P4 C28 1.881(4) 3_675 ? P4 C28 1.881(4) . ? P4 C28 1.881(4) 2_765 ? O41 N41 1.272(5) . ? O42 N41 1.274(5) 3_675 ? O43 N41 1.217(4) . ? N41 O42 1.274(5) 2_765 ? C25 C61 1.534(6) . ? C25 C27 1.546(6) . ? C25 C26 1.549(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C31 1.536(6) . ? C28 C29 1.544(6) . ? C28 C30 1.551(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Er1 O1 147.29(10) . . ? O2 Er1 O21 92.40(10) . . ? O1 Er1 O21 91.71(11) . . ? O2 Er1 O33 93.49(11) . . ? O1 Er1 O33 97.24(11) . . ? O21 Er1 O33 153.28(11) . . ? O2 Er1 O11 133.91(10) . . ? O1 Er1 O11 78.76(10) . . ? O21 Er1 O11 80.79(11) . . ? O33 Er1 O11 76.38(11) . . ? O2 Er1 O12 80.02(10) . . ? O1 Er1 O12 132.57(11) . . ? O21 Er1 O12 79.30(11) . . ? O33 Er1 O12 76.10(11) . . ? O11 Er1 O12 53.89(10) . . ? O2 Er1 O22 78.64(10) . . ? O1 Er1 O22 77.70(10) . . ? O21 Er1 O22 54.03(11) . . ? O33 Er1 O22 152.62(10) . . ? O11 Er1 O22 127.58(10) . . ? O12 Er1 O22 127.05(10) . . ? O2 Er1 O31 80.31(10) . . ? O1 Er1 O31 81.50(11) . . ? O21 Er1 O31 153.17(11) . . ? O33 Er1 O31 53.52(10) . . ? O11 Er1 O31 122.61(10) . . ? O12 Er1 O31 123.99(10) . . ? O22 Er1 O31 99.14(10) . . ? O2 Er1 N21 85.78(11) . . ? O1 Er1 N21 83.23(11) . . ? O21 Er1 N21 27.19(10) . . ? O33 Er1 N21 179.21(12) . . ? O11 Er1 N21 104.36(11) . . ? O12 Er1 N21 104.06(11) . . ? O22 Er1 N21 26.87(10) . . ? O31 Er1 N21 125.99(11) . . ? O2 Er1 N11 106.95(11) . . ? O1 Er1 N11 105.72(11) . . ? O21 Er1 N11 80.09(10) . . ? O33 Er1 N11 73.25(10) . . ? O11 Er1 N11 26.96(10) . . ? O12 Er1 N11 26.99(10) . . ? O22 Er1 N11 134.12(10) . . ? O31 Er1 N11 126.74(10) . . ? N21 Er1 N11 107.25(11) . . ? O2 Er1 N31 85.21(11) . . ? O1 Er1 N31 90.69(11) . . ? O21 Er1 N31 177.51(11) . . ? O33 Er1 N31 26.68(10) . . ? O11 Er1 N31 100.37(10) . . ? O12 Er1 N31 99.57(11) . . ? O22 Er1 N31 125.94(11) . . ? O31 Er1 N31 26.91(10) . . ? N21 Er1 N31 152.80(12) . . ? N11 Er1 N31 99.93(11) . . ? O1 P1 C9 107.49(19) . . ? O1 P1 C5 106.44(18) . . ? C9 P1 C5 111.4(2) . . ? O1 P1 C1 108.46(18) . . ? C9 P1 C1 111.32(19) . . ? C5 P1 C1 111.49(19) . . ? O2 P2 C13 108.06(19) . . ? O2 P2 C21 107.28(18) . . ? C13 P2 C21 111.5(2) . . ? O2 P2 C17 106.11(18) . . ? C13 P2 C17 112.2(2) . . ? C21 P2 C17 111.3(2) . . ? P1 O1 Er1 173.67(18) . . ? P2 O2 Er1 176.4(2) . . ? N11 O11 Er1 95.8(2) . . ? N11 O12 Er1 95.5(2) . . ? N21 O21 Er1 96.2(2) . . ? N21 O22 Er1 93.8(2) . . ? N31 O31 Er1 94.2(2) . . ? N31 O33 Er1 96.8(2) . . ? O13 N11 O11 122.8(4) . . ? O13 N11 O12 122.6(4) . . ? O11 N11 O12 114.5(3) . . ? O13 N11 Er1 176.2(3) . . ? O11 N11 Er1 57.23(19) . . ? O12 N11 Er1 57.48(19) . . ? O23 N21 O22 122.3(4) . . ? O23 N21 O21 121.8(4) . . ? O22 N21 O21 115.9(4) . . ? O23 N21 Er1 176.2(3) . . ? O22 N21 Er1 59.3(2) . . ? O21 N21 Er1 56.6(2) . . ? O32 N31 O33 122.3(4) . . ? O32 N31 O31 122.6(4) . . ? O33 N31 O31 115.1(3) . . ? O32 N31 Er1 174.5(3) . . ? O33 N31 Er1 56.5(2) . . ? O31 N31 Er1 58.9(2) . . ? C3 C1 C4 108.3(3) . . ? C3 C1 C2 105.2(3) . . ? C4 C1 C2 109.3(4) . . ? C3 C1 P1 112.7(3) . . ? C4 C1 P1 112.8(3) . . ? C2 C1 P1 108.2(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C8 109.2(4) . . ? C6 C5 C7 105.0(4) . . ? C8 C5 C7 108.6(3) . . ? C6 C5 P1 109.9(3) . . ? C8 C5 P1 114.7(3) . . ? C7 C5 P1 108.9(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C12 108.4(4) . . ? C10 C9 C11 105.3(4) . . ? C12 C9 C11 109.9(4) . . ? C10 C9 P1 111.4(3) . . ? C12 C9 P1 113.7(3) . . ? C11 C9 P1 107.8(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C16 109.0(4) . . ? C14 C13 C15 105.9(4) . . ? C16 C13 C15 108.6(4) . . ? C14 C13 P2 110.5(3) . . ? C16 C13 P2 113.9(3) . . ? C15 C13 P2 108.6(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C17 C19 110.0(4) . . ? C20 C17 C18 106.8(4) . . ? C19 C17 C18 108.4(4) . . ? C20 C17 P2 108.7(3) . . ? C19 C17 P2 114.1(3) . . ? C18 C17 P2 108.5(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C23 109.1(4) . . ? C22 C21 C24 110.0(4) . . ? C23 C21 C24 105.3(4) . . ? C22 C21 P2 113.5(3) . . ? C23 C21 P2 110.2(3) . . ? C24 C21 P2 108.4(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O3 Er2 O4 180.000(3) . . ? O3 Er2 O41 91.82(8) . 3_675 ? O4 Er2 O41 88.18(8) . 3_675 ? O3 Er2 O41 91.82(8) . 2_765 ? O4 Er2 O41 88.18(8) . 2_765 ? O41 Er2 O41 119.900(10) 3_675 2_765 ? O3 Er2 O41 91.82(8) . . ? O4 Er2 O41 88.18(8) . . ? O41 Er2 O41 119.900(9) 3_675 . ? O41 Er2 O41 119.900(11) 2_765 . ? O3 Er2 O42 88.83(9) . 3_675 ? O4 Er2 O42 91.17(9) . 3_675 ? O41 Er2 O42 172.62(11) 3_675 3_675 ? O41 Er2 O42 52.72(11) 2_765 3_675 ? O41 Er2 O42 67.41(11) . 3_675 ? O3 Er2 O42 88.83(9) . . ? O4 Er2 O42 91.17(9) . . ? O41 Er2 O42 52.72(11) 3_675 . ? O41 Er2 O42 67.41(11) 2_765 . ? O41 Er2 O42 172.62(11) . . ? O42 Er2 O42 119.959(6) 3_675 . ? O3 Er2 O42 88.83(9) . 2_765 ? O4 Er2 O42 91.17(9) . 2_765 ? O41 Er2 O42 67.41(11) 3_675 2_765 ? O41 Er2 O42 172.62(11) 2_765 2_765 ? O41 Er2 O42 52.72(11) . 2_765 ? O42 Er2 O42 119.959(8) 3_675 2_765 ? O42 Er2 O42 119.959(8) . 2_765 ? O3 Er2 N41 90.70(8) . 3_675 ? O4 Er2 N41 89.30(8) . 3_675 ? O41 Er2 N41 26.33(10) 3_675 3_675 ? O41 Er2 N41 93.66(10) 2_765 3_675 ? O41 Er2 N41 146.23(10) . 3_675 ? O42 Er2 N41 146.33(10) 3_675 3_675 ? O42 Er2 N41 26.40(10) . 3_675 ? O42 Er2 N41 93.68(11) 2_765 3_675 ? O3 Er2 N41 90.70(8) . 2_765 ? O4 Er2 N41 89.30(8) . 2_765 ? O41 Er2 N41 146.23(10) 3_675 2_765 ? O41 Er2 N41 26.33(10) 2_765 2_765 ? O41 Er2 N41 93.66(10) . 2_765 ? O42 Er2 N41 26.40(10) 3_675 2_765 ? O42 Er2 N41 93.68(10) . 2_765 ? O42 Er2 N41 146.33(11) 2_765 2_765 ? N41 Er2 N41 119.985(4) 3_675 2_765 ? O3 Er2 N41 90.70(8) . . ? O4 Er2 N41 89.30(8) . . ? O41 Er2 N41 93.66(10) 3_675 . ? O41 Er2 N41 146.23(10) 2_765 . ? O41 Er2 N41 26.33(10) . . ? O42 Er2 N41 93.68(11) 3_675 . ? O42 Er2 N41 146.33(11) . . ? O42 Er2 N41 26.40(10) 2_765 . ? N41 Er2 N41 119.985(4) 3_675 . ? N41 Er2 N41 119.985(5) 2_765 . ? O3 P3 C25 107.41(14) . 3_675 ? O3 P3 C25 107.41(14) . 2_765 ? C25 P3 C25 111.45(13) 3_675 2_765 ? O3 P3 C25 107.41(14) . . ? C25 P3 C25 111.45(13) 3_675 . ? C25 P3 C25 111.45(13) 2_765 . ? O4 P4 C28 107.39(14) . 3_675 ? O4 P4 C28 107.39(14) . . ? C28 P4 C28 111.47(13) 3_675 . ? O4 P4 C28 107.39(14) . 2_765 ? C28 P4 C28 111.47(13) 3_675 2_765 ? C28 P4 C28 111.47(13) . 2_765 ? P3 O3 Er2 180.000(1) . . ? P4 O4 Er2 180.0 . . ? N41 O41 Er2 96.6(2) . . ? N41 O42 Er2 96.1(2) 3_675 . ? O43 N41 O41 122.4(4) . . ? O43 N41 O42 123.1(4) . 2_765 ? O41 N41 O42 114.5(3) . 2_765 ? O43 N41 Er2 178.9(3) . . ? O41 N41 Er2 57.0(2) . . ? O42 N41 Er2 57.5(2) 2_765 . ? C61 C25 C27 109.7(4) . . ? C61 C25 C26 109.2(4) . . ? C27 C25 C26 104.8(4) . . ? C61 C25 P3 113.4(3) . . ? C27 C25 P3 111.2(3) . . ? C26 C25 P3 108.1(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C31 C28 C29 108.7(3) . . ? C31 C28 C30 109.7(3) . . ? C29 C28 C30 105.7(3) . . ? C31 C28 P4 114.2(3) . . ? C29 C28 P4 109.0(3) . . ? C30 C28 P4 109.1(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C25 C61 H61A 109.5 . . ? C25 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C25 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.008 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.097 #===END data_Lu _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Lu _chemical_melting_point ? _chemical_formula_moiety 'C32 H72 Lu1.33 N4 O14.67 P2.67' _chemical_formula_sum 'C32 H72 Lu1.33 N4 O14.67 P2.67' _chemical_formula_weight 1063.48 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' 'Lu' 'Lu' -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R3 _symmetry_space_group_name_Hall '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' _cell_length_a 28.2896(4) _cell_length_b 28.2896(4) _cell_length_c 15.0017(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10397.4(3) _cell_formula_units_Z 9 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 17905 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4896 _exptl_absorpt_coefficient_mu 2.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4204 _exptl_absorpt_correction_T_max 0.5587 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '9.091' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24102 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9628 _reflns_number_gt 9534 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Crystal structure is an merohedral twin where an inversion twinning were taken into account as well. The twin law applied is 0 1 0 1 0 0 0 0 -1. The fractional contributions of each domain [1-(k1+k2+k3)] are refined to values given as: BASF 0.06424 0.47158 0.01175. Small fraction of merohedral twinning present has highly influenced a crystal stucture. Applying a twin law significantly improves R-factor from 5% down to 2.4%. ; _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^)+(0.0000P)^2^+13.0484P] 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 9628 _refine_ls_number_parameters 520 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0232 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0433 _refine_ls_wR_factor_gt 0.0431 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.712051(6) 0.865293(5) 0.853465(8) 0.01220(3) Uani 1 1 d . . . P1 P 0.65870(4) 0.80395(4) 1.07341(6) 0.01219(19) Uani 1 1 d . . . P2 P 0.67505(4) 0.86055(4) 0.61655(6) 0.01273(19) Uani 1 1 d . . . O1 O 0.68431(10) 0.83068(10) 0.98504(15) 0.0141(6) Uani 1 1 d . . . O2 O 0.69218(10) 0.86411(10) 0.71308(16) 0.0129(5) Uani 1 1 d . . . O11 O 0.79050(10) 0.91999(10) 0.94030(16) 0.0181(6) Uani 1 1 d . . . O12 O 0.79463(10) 0.93913(11) 0.80010(17) 0.0191(6) Uani 1 1 d . . . O13 O 0.86746(10) 0.98280(11) 0.88335(18) 0.0217(6) Uani 1 1 d . . . O21 O 0.69646(11) 0.93713(11) 0.88366(19) 0.0215(6) Uani 1 1 d . . . O22 O 0.62425(11) 0.85853(11) 0.86191(19) 0.0193(6) Uani 1 1 d . . . O23 O 0.61571(13) 0.92869(12) 0.8988(2) 0.0371(8) Uani 1 1 d . . . O31 O 0.67985(11) 0.77113(11) 0.81930(18) 0.0209(6) Uani 1 1 d . . . O32 O 0.73631(14) 0.74174(12) 0.7885(2) 0.0388(8) Uani 1 1 d . . . O33 O 0.76677(11) 0.82606(11) 0.8290(2) 0.0250(6) Uani 1 1 d . . . N11 N 0.81950(13) 0.94886(13) 0.8752(2) 0.0162(7) Uani 1 1 d . . . N21 N 0.64424(14) 0.90877(14) 0.8823(2) 0.0215(7) Uani 1 1 d . . . N31 N 0.72785(15) 0.77766(13) 0.8113(2) 0.0228(7) Uani 1 1 d . . . C1 C 0.58301(15) 0.75963(15) 1.0571(2) 0.0171(8) Uani 1 1 d . . . C2 C 0.57292(16) 0.73085(16) 0.9650(3) 0.0241(9) Uani 1 1 d . . . H2A H 0.5916 0.7096 0.9631 0.036 Uiso 1 1 calc R . . H2B H 0.5871 0.7584 0.9176 0.036 Uiso 1 1 calc R . . H2C H 0.5337 0.7064 0.9563 0.036 Uiso 1 1 calc R . . C3 C 0.55355(15) 0.79281(17) 1.0522(3) 0.0233(9) Uani 1 1 d . . . H3A H 0.5152 0.7686 1.0364 0.035 Uiso 1 1 calc R . . H3B H 0.5710 0.8214 1.0068 0.035 Uiso 1 1 calc R . . H3C H 0.5557 0.8097 1.1102 0.035 Uiso 1 1 calc R . . C4 C 0.55608(16) 0.71618(17) 1.1301(3) 0.0257(9) Uani 1 1 d . . . H4A H 0.5634 0.7340 1.1885 0.039 Uiso 1 1 calc R . . H4B H 0.5710 0.6915 1.1283 0.039 Uiso 1 1 calc R . . H4C H 0.5166 0.6953 1.1200 0.039 Uiso 1 1 calc R . . C5 C 0.69097(15) 0.76283(15) 1.1065(2) 0.0161(8) Uani 1 1 d . . . C6 C 0.67013(17) 0.71215(16) 1.0469(3) 0.0240(9) Uani 1 1 d . . . H6A H 0.6918 0.6945 1.0577 0.036 Uiso 1 1 calc R . . H6B H 0.6735 0.7231 0.9842 0.036 Uiso 1 1 calc R . . H6C H 0.6317 0.6865 1.0607 0.036 Uiso 1 1 calc R . . C7 C 0.75322(16) 0.79665(17) 1.0877(3) 0.0240(9) Uani 1 1 d . . . H7A H 0.7697 0.7737 1.0972 0.036 Uiso 1 1 calc R . . H7B H 0.7701 0.8280 1.1281 0.036 Uiso 1 1 calc R . . H7C H 0.7592 0.8095 1.0259 0.036 Uiso 1 1 calc R . . C8 C 0.68214(17) 0.74440(17) 1.2048(3) 0.0228(9) Uani 1 1 d . . . H8A H 0.6431 0.7262 1.2189 0.034 Uiso 1 1 calc R . . H8B H 0.7020 0.7763 1.2435 0.034 Uiso 1 1 calc R . . H8C H 0.6957 0.7190 1.2145 0.034 Uiso 1 1 calc R . . C9 C 0.67467(16) 0.85993(16) 1.1548(2) 0.0193(8) Uani 1 1 d . . . C10 C 0.73532(16) 0.88940(17) 1.1824(3) 0.0279(10) Uani 1 1 d . . . H10A H 0.7583 0.9011 1.1290 0.042 Uiso 1 1 calc R . . H10B H 0.7427 0.8644 1.2171 0.042 Uiso 1 1 calc R . . H10C H 0.7435 0.9214 1.2188 0.042 Uiso 1 1 calc R . . C11 C 0.66680(17) 0.90389(16) 1.1079(3) 0.0234(9) Uani 1 1 d . . . H11A H 0.6746 0.9334 1.1500 0.035 Uiso 1 1 calc R . . H11B H 0.6290 0.8877 1.0870 0.035 Uiso 1 1 calc R . . H11C H 0.6917 0.9185 1.0570 0.035 Uiso 1 1 calc R . . C12 C 0.63920(19) 0.84018(19) 1.2402(2) 0.0286(10) Uani 1 1 d . . . H12A H 0.6441 0.8119 1.2694 0.043 Uiso 1 1 calc R . . H12B H 0.6007 0.8251 1.2242 0.043 Uiso 1 1 calc R . . H12C H 0.6503 0.8710 1.2810 0.043 Uiso 1 1 calc R . . C13 C 0.59875(15) 0.82070(15) 0.6123(3) 0.0190(8) Uani 1 1 d . . . C14 C 0.57435(17) 0.85536(18) 0.6474(3) 0.0260(9) Uani 1 1 d . . . H14A H 0.5819 0.8846 0.6048 0.039 Uiso 1 1 calc R . . H14B H 0.5909 0.8714 0.7051 0.039 Uiso 1 1 calc R . . H14C H 0.5348 0.8321 0.6546 0.039 Uiso 1 1 calc R . . C15 C 0.57796(17) 0.77159(17) 0.6765(3) 0.0281(10) Uani 1 1 d . . . H15A H 0.5917 0.7847 0.7367 0.042 Uiso 1 1 calc R . . H15B H 0.5910 0.7472 0.6563 0.042 Uiso 1 1 calc R . . H15C H 0.5380 0.7517 0.6771 0.042 Uiso 1 1 calc R . . C16 C 0.57564(17) 0.79963(18) 0.5181(3) 0.0274(10) Uani 1 1 d . . . H16A H 0.5357 0.7812 0.5199 0.041 Uiso 1 1 calc R . . H16B H 0.5871 0.7739 0.4981 0.041 Uiso 1 1 calc R . . H16C H 0.5895 0.8305 0.4766 0.041 Uiso 1 1 calc R . . C17 C 0.70616(16) 0.82521(16) 0.5556(2) 0.0188(8) Uani 1 1 d . . . C18 C 0.67576(19) 0.76399(17) 0.5802(3) 0.0295(10) Uani 1 1 d . . . H18A H 0.6953 0.7466 0.5551 0.044 Uiso 1 1 calc R . . H18B H 0.6387 0.7465 0.5558 0.044 Uiso 1 1 calc R . . H18C H 0.6740 0.7600 0.6452 0.044 Uiso 1 1 calc R . . C19 C 0.70578(17) 0.83045(19) 0.4528(3) 0.0270(9) Uani 1 1 d . . . H19A H 0.7235 0.8118 0.4256 0.040 Uiso 1 1 calc R . . H19B H 0.7256 0.8691 0.4361 0.040 Uiso 1 1 calc R . . H19C H 0.6680 0.8137 0.4317 0.040 Uiso 1 1 calc R . . C20 C 0.76593(16) 0.84896(18) 0.5877(3) 0.0250(9) Uani 1 1 d . . . H20A H 0.7672 0.8513 0.6529 0.037 Uiso 1 1 calc R . . H20B H 0.7886 0.8855 0.5624 0.037 Uiso 1 1 calc R . . H20C H 0.7798 0.8251 0.5681 0.037 Uiso 1 1 calc R . . C21 C 0.70221(16) 0.93199(15) 0.5755(3) 0.0194(8) Uani 1 1 d . . . C22 C 0.67510(18) 0.93512(17) 0.4880(3) 0.0255(9) Uani 1 1 d . . . H22A H 0.6928 0.9731 0.4675 0.038 Uiso 1 1 calc R . . H22B H 0.6363 0.9218 0.4986 0.038 Uiso 1 1 calc R . . H22C H 0.6790 0.9125 0.4425 0.038 Uiso 1 1 calc R . . C23 C 0.76414(17) 0.95983(17) 0.5614(3) 0.0294(10) Uani 1 1 d . . . H23A H 0.7719 0.9431 0.5105 0.044 Uiso 1 1 calc R . . H23B H 0.7813 0.9554 0.6151 0.044 Uiso 1 1 calc R . . H23C H 0.7787 0.9988 0.5496 0.044 Uiso 1 1 calc R . . C24 C 0.69368(18) 0.96507(16) 0.6497(3) 0.0266(9) Uani 1 1 d . . . H24A H 0.7093 1.0031 0.6306 0.040 Uiso 1 1 calc R . . H24B H 0.7118 0.9636 0.7044 0.040 Uiso 1 1 calc R . . H24C H 0.6545 0.9494 0.6609 0.040 Uiso 1 1 calc R . . Lu2 Lu 1.0000 1.0000 0.386481(15) 0.01158(6) Uani 1 3 d S . . P3 P 1.0000 1.0000 0.63215(10) 0.0112(3) Uani 1 3 d S . . P4 P 1.0000 1.0000 0.14087(10) 0.0107(3) Uani 1 3 d S . . O3 O 1.0000 1.0000 0.5304(3) 0.0148(10) Uani 1 3 d S . . O4 O 1.0000 1.0000 0.2421(2) 0.0131(9) Uani 1 3 d S . . O41 O 1.08153(11) 0.99461(12) 0.38197(19) 0.0221(6) Uani 1 1 d . . . O42 O 0.91252(12) 0.99412(12) 0.3904(2) 0.0282(7) Uani 1 1 d . . . O43 O 1.08290(14) 0.91813(14) 0.3833(2) 0.0448(9) Uani 1 1 d . . . N41 N 1.05768(15) 0.94254(15) 0.3855(2) 0.0244(8) Uani 1 1 d . . . C25 C 0.97316(16) 1.04528(16) 0.6690(2) 0.0164(8) Uani 1 1 d . . . C26 C 0.99845(19) 1.09647(16) 0.6097(3) 0.0273(9) Uani 1 1 d . . . H26A H 0.9894 1.0856 0.5472 0.041 Uiso 1 1 calc R . . H26B H 1.0382 1.1163 0.6172 0.041 Uiso 1 1 calc R . . H26C H 0.9839 1.1201 0.6270 0.041 Uiso 1 1 calc R . . C27 C 0.91124(17) 1.01786(18) 0.6540(3) 0.0263(9) Uani 1 1 d . . . H27A H 0.8989 1.0438 0.6681 0.039 Uiso 1 1 calc R . . H27B H 0.8925 0.9858 0.6928 0.039 Uiso 1 1 calc R . . H27C H 0.9029 1.0065 0.5916 0.039 Uiso 1 1 calc R . . C28 C 1.05957(15) 0.99342(15) 0.1032(2) 0.0162(8) Uani 1 1 d . . . C29 C 1.04729(17) 0.93442(17) 0.1202(3) 0.0244(9) Uani 1 1 d . . . H29A H 1.0182 0.9094 0.0800 0.037 Uiso 1 1 calc R . . H29B H 1.0356 0.9243 0.1821 0.037 Uiso 1 1 calc R . . H29C H 1.0803 0.9322 0.1092 0.037 Uiso 1 1 calc R . . C30 C 1.11005(16) 1.03037(17) 0.1615(3) 0.0234(9) Uani 1 1 d . . . H30A H 1.1403 1.0244 0.1454 0.035 Uiso 1 1 calc R . . H30B H 1.1008 1.0213 0.2245 0.035 Uiso 1 1 calc R . . H30C H 1.1209 1.0687 0.1515 0.035 Uiso 1 1 calc R . . C31 C 1.07436(16) 1.00714(16) 0.0042(2) 0.0205(8) Uani 1 1 d . . . H31A H 1.0877 1.0460 -0.0057 0.031 Uiso 1 1 calc R . . H31B H 1.0419 0.9854 -0.0325 0.031 Uiso 1 1 calc R . . H31C H 1.1029 0.9987 -0.0121 0.031 Uiso 1 1 calc R . . C61 C 0.98591(17) 1.06265(17) 0.7675(3) 0.0221(9) Uani 1 1 d . . . H61A H 1.0255 1.0840 0.7760 0.033 Uiso 1 1 calc R . . H61B H 0.9707 1.0301 0.8054 0.033 Uiso 1 1 calc R . . H61C H 0.9696 1.0849 0.7838 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.01319(8) 0.01266(7) 0.00914(6) 0.00083(6) -0.00060(6) 0.00525(6) P1 0.0131(5) 0.0157(5) 0.0089(4) 0.0012(3) 0.0003(3) 0.0081(4) P2 0.0127(5) 0.0131(5) 0.0106(4) 0.0001(3) -0.0027(4) 0.0051(4) O1 0.0162(13) 0.0185(14) 0.0067(12) 0.0010(10) 0.0018(10) 0.0080(12) O2 0.0138(13) 0.0165(14) 0.0070(13) -0.0001(10) -0.0019(10) 0.0066(11) O11 0.0150(13) 0.0209(14) 0.0122(13) 0.0016(11) -0.0001(10) 0.0044(11) O12 0.0139(13) 0.0237(15) 0.0123(13) 0.0004(11) -0.0037(10) 0.0039(12) O13 0.0112(13) 0.0218(14) 0.0269(15) -0.0058(12) -0.0010(11) 0.0043(12) O21 0.0219(15) 0.0171(14) 0.0258(16) 0.0003(12) -0.0034(12) 0.0099(13) O22 0.0207(15) 0.0181(15) 0.0203(15) 0.0009(11) 0.0008(12) 0.0108(12) O23 0.0399(19) 0.0374(19) 0.052(2) -0.0028(16) -0.0020(16) 0.0326(17) O31 0.0233(15) 0.0195(14) 0.0182(14) -0.0015(11) -0.0031(12) 0.0094(12) O32 0.052(2) 0.0276(18) 0.051(2) -0.0100(15) -0.0134(17) 0.0305(17) O33 0.0242(16) 0.0196(15) 0.0320(16) -0.0044(12) -0.0060(13) 0.0116(13) N11 0.0152(17) 0.0188(17) 0.0149(16) -0.0014(13) 0.0015(12) 0.0087(14) N21 0.0256(19) 0.029(2) 0.0146(17) 0.0068(14) 0.0003(14) 0.0176(17) N31 0.036(2) 0.0196(18) 0.0191(17) 0.0009(14) -0.0068(15) 0.0188(17) C1 0.0102(18) 0.019(2) 0.0155(19) 0.0039(15) 0.0000(14) 0.0019(16) C2 0.018(2) 0.024(2) 0.023(2) 0.0003(17) -0.0064(17) 0.0049(18) C3 0.0155(19) 0.035(2) 0.021(2) 0.0030(17) 0.0003(15) 0.0137(18) C4 0.015(2) 0.034(2) 0.024(2) 0.0102(18) 0.0019(16) 0.0097(18) C5 0.021(2) 0.0183(19) 0.0151(18) 0.0014(15) -0.0016(15) 0.0147(17) C6 0.029(2) 0.023(2) 0.026(2) 0.0009(17) -0.0008(17) 0.0178(19) C7 0.019(2) 0.026(2) 0.034(2) 0.0022(18) 0.0006(18) 0.0173(19) C8 0.025(2) 0.030(2) 0.019(2) 0.0069(17) -0.0027(16) 0.0181(19) C9 0.022(2) 0.022(2) 0.0144(18) -0.0061(15) -0.0039(15) 0.0120(17) C10 0.028(2) 0.023(2) 0.032(2) -0.0109(18) -0.0151(19) 0.0126(19) C11 0.028(2) 0.021(2) 0.026(2) -0.0077(17) -0.0021(18) 0.0158(19) C12 0.042(3) 0.044(3) 0.0097(19) -0.0040(17) -0.0005(18) 0.029(2) C13 0.0158(19) 0.018(2) 0.021(2) 0.0005(15) -0.0051(15) 0.0068(16) C14 0.022(2) 0.039(3) 0.023(2) 0.0036(19) 0.0011(17) 0.020(2) C15 0.021(2) 0.023(2) 0.027(2) 0.0092(18) 0.0046(18) 0.0017(18) C16 0.021(2) 0.030(2) 0.023(2) -0.0062(19) -0.0097(17) 0.0073(19) C17 0.023(2) 0.024(2) 0.0146(19) -0.0039(15) -0.0044(15) 0.0158(18) C18 0.041(3) 0.027(2) 0.028(2) -0.0069(19) -0.007(2) 0.022(2) C19 0.030(2) 0.040(3) 0.014(2) -0.0058(18) -0.0026(16) 0.021(2) C20 0.022(2) 0.041(3) 0.021(2) -0.0053(18) -0.0043(17) 0.021(2) C21 0.025(2) 0.0145(19) 0.0157(19) 0.0036(15) -0.0025(16) 0.0080(17) C22 0.032(2) 0.025(2) 0.019(2) 0.0040(16) -0.0067(17) 0.0144(19) C23 0.024(2) 0.023(2) 0.026(2) 0.0068(18) 0.0023(18) -0.0001(19) C24 0.041(3) 0.018(2) 0.023(2) -0.0014(16) -0.0084(19) 0.016(2) Lu2 0.01434(8) 0.01434(8) 0.00607(11) 0.000 0.000 0.00717(4) P3 0.0140(5) 0.0140(5) 0.0057(7) 0.000 0.000 0.0070(2) P4 0.0130(5) 0.0130(5) 0.0062(7) 0.000 0.000 0.0065(2) O3 0.0186(15) 0.0186(15) 0.007(2) 0.000 0.000 0.0093(8) O4 0.0179(14) 0.0179(14) 0.0037(19) 0.000 0.000 0.0089(7) O41 0.0194(15) 0.0236(16) 0.0235(16) 0.0011(13) -0.0001(12) 0.0110(13) O42 0.0228(16) 0.0242(17) 0.0397(19) 0.0028(14) 0.0031(14) 0.0134(14) O43 0.052(2) 0.055(2) 0.053(2) 0.0004(18) -0.0055(18) 0.046(2) N41 0.036(2) 0.031(2) 0.0159(16) -0.0032(15) -0.0046(15) 0.0244(18) C25 0.021(2) 0.022(2) 0.0104(17) 0.0006(15) 0.0016(15) 0.0136(17) C26 0.043(3) 0.024(2) 0.023(2) 0.0054(17) 0.0046(19) 0.022(2) C27 0.032(2) 0.038(3) 0.017(2) 0.0012(18) 0.0008(17) 0.024(2) C28 0.0180(19) 0.025(2) 0.0093(17) 0.0033(15) 0.0028(14) 0.0136(17) C29 0.032(2) 0.029(2) 0.023(2) 0.0035(17) 0.0048(18) 0.023(2) C30 0.018(2) 0.033(2) 0.018(2) 0.0015(18) 0.0019(16) 0.0118(19) C31 0.020(2) 0.030(2) 0.0132(19) 0.0021(16) 0.0042(15) 0.0145(19) C61 0.030(2) 0.025(2) 0.015(2) -0.0036(16) 0.0005(16) 0.0170(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Lu1 O1 2.168(2) . ? Lu1 O2 2.176(2) . ? Lu1 O21 2.329(3) . ? Lu1 O33 2.341(3) . ? Lu1 O12 2.363(3) . ? Lu1 O11 2.363(3) . ? Lu1 O22 2.397(3) . ? Lu1 O31 2.400(3) . ? Lu1 N21 2.782(3) . ? Lu1 N11 2.784(3) . ? Lu1 N31 2.802(3) . ? P1 O1 1.519(3) . ? P1 C9 1.867(4) . ? P1 C5 1.870(4) . ? P1 C1 1.880(4) . ? P2 O2 1.514(3) . ? P2 C17 1.868(4) . ? P2 C13 1.871(4) . ? P2 C21 1.871(4) . ? O11 N11 1.274(4) . ? O12 N11 1.283(4) . ? O13 N11 1.214(4) . ? O21 N21 1.281(4) . ? O22 N21 1.276(4) . ? O23 N21 1.219(4) . ? O31 N31 1.281(4) . ? O32 N31 1.205(4) . ? O33 N31 1.285(4) . ? C1 C4 1.534(5) . ? C1 C3 1.537(5) . ? C1 C2 1.556(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.536(5) . ? C5 C8 1.542(5) . ? C5 C7 1.553(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.538(5) . ? C9 C10 1.543(5) . ? C9 C12 1.550(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.544(5) . ? C13 C16 1.546(5) . ? C13 C14 1.547(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.544(6) . ? C17 C19 1.550(5) . ? C17 C20 1.551(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.535(6) . ? C21 C22 1.545(5) . ? C21 C24 1.548(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Lu2 O3 2.159(4) . ? Lu2 O4 2.166(4) . ? Lu2 O41 2.387(3) 3_675 ? Lu2 O41 2.387(3) 2_765 ? Lu2 O41 2.387(3) . ? Lu2 O42 2.397(3) 3_675 ? Lu2 O42 2.397(3) . ? Lu2 O42 2.397(3) 2_765 ? Lu2 N41 2.821(3) 3_675 ? Lu2 N41 2.821(3) 2_765 ? Lu2 N41 2.821(3) . ? P3 O3 1.527(5) . ? P3 C25 1.870(4) 3_675 ? P3 C25 1.870(4) 2_765 ? P3 C25 1.870(4) . ? P4 O4 1.519(4) . ? P4 C28 1.873(4) 3_675 ? P4 C28 1.873(4) . ? P4 C28 1.873(4) 2_765 ? O41 N41 1.278(4) . ? O42 N41 1.272(4) 3_675 ? O43 N41 1.217(4) . ? N41 O42 1.272(4) 2_765 ? C25 C27 1.537(5) . ? C25 C26 1.538(5) . ? C25 C61 1.542(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C31 1.538(5) . ? C28 C29 1.547(5) . ? C28 C30 1.551(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Lu1 O2 147.32(9) . . ? O1 Lu1 O21 91.91(9) . . ? O2 Lu1 O21 92.38(10) . . ? O1 Lu1 O33 95.99(10) . . ? O2 Lu1 O33 93.90(10) . . ? O21 Lu1 O33 154.50(10) . . ? O1 Lu1 O12 133.02(9) . . ? O2 Lu1 O12 79.59(9) . . ? O21 Lu1 O12 80.18(9) . . ? O33 Lu1 O12 76.71(10) . . ? O1 Lu1 O11 78.65(9) . . ? O2 Lu1 O11 134.00(9) . . ? O21 Lu1 O11 81.20(9) . . ? O33 Lu1 O11 76.68(9) . . ? O12 Lu1 O11 54.41(9) . . ? O1 Lu1 O22 77.83(10) . . ? O2 Lu1 O22 78.49(9) . . ? O21 Lu1 O22 54.46(10) . . ? O33 Lu1 O22 151.02(10) . . ? O12 Lu1 O22 127.99(9) . . ? O11 Lu1 O22 128.29(9) . . ? O1 Lu1 O31 80.93(9) . . ? O2 Lu1 O31 79.89(9) . . ? O21 Lu1 O31 151.32(9) . . ? O33 Lu1 O31 54.16(9) . . ? O12 Lu1 O31 124.59(9) . . ? O11 Lu1 O31 123.75(9) . . ? O22 Lu1 O31 96.86(9) . . ? O1 Lu1 N21 83.36(9) . . ? O2 Lu1 N21 85.82(10) . . ? O21 Lu1 N21 27.23(9) . . ? O33 Lu1 N21 178.26(10) . . ? O12 Lu1 N21 104.92(10) . . ? O11 Lu1 N21 104.74(10) . . ? O22 Lu1 N21 27.26(9) . . ? O31 Lu1 N21 124.11(10) . . ? O1 Lu1 N11 105.78(9) . . ? O2 Lu1 N11 106.89(9) . . ? O21 Lu1 N11 80.73(9) . . ? O33 Lu1 N11 73.79(9) . . ? O12 Lu1 N11 27.33(8) . . ? O11 Lu1 N11 27.12(8) . . ? O22 Lu1 N11 135.19(9) . . ? O31 Lu1 N11 127.94(9) . . ? N21 Lu1 N11 107.93(10) . . ? O1 Lu1 N31 89.28(10) . . ? O2 Lu1 N31 85.55(9) . . ? O21 Lu1 N31 177.68(10) . . ? O33 Lu1 N31 27.07(10) . . ? O12 Lu1 N31 100.44(10) . . ? O11 Lu1 N31 100.99(9) . . ? O22 Lu1 N31 123.95(10) . . ? O31 Lu1 N31 27.13(9) . . ? N21 Lu1 N31 151.21(10) . . ? N11 Lu1 N31 100.86(10) . . ? O1 P1 C9 107.19(16) . . ? O1 P1 C5 106.38(15) . . ? C9 P1 C5 111.58(17) . . ? O1 P1 C1 108.60(16) . . ? C9 P1 C1 111.27(17) . . ? C5 P1 C1 111.56(17) . . ? O2 P2 C17 106.42(16) . . ? O2 P2 C13 107.88(16) . . ? C17 P2 C13 111.79(18) . . ? O2 P2 C21 107.33(16) . . ? C17 P2 C21 111.60(18) . . ? C13 P2 C21 111.51(17) . . ? P1 O1 Lu1 173.86(16) . . ? P2 O2 Lu1 176.66(17) . . ? N11 O11 Lu1 95.17(19) . . ? N11 O12 Lu1 94.93(19) . . ? N21 O21 Lu1 96.5(2) . . ? N21 O22 Lu1 93.4(2) . . ? N31 O31 Lu1 94.2(2) . . ? N31 O33 Lu1 96.9(2) . . ? O13 N11 O11 122.4(3) . . ? O13 N11 O12 122.3(3) . . ? O11 N11 O12 115.3(3) . . ? O13 N11 Lu1 175.6(2) . . ? O11 N11 Lu1 57.71(16) . . ? O12 N11 Lu1 57.73(17) . . ? O23 N21 O22 122.4(3) . . ? O23 N21 O21 122.0(3) . . ? O22 N21 O21 115.6(3) . . ? O23 N21 Lu1 176.9(3) . . ? O22 N21 Lu1 59.35(18) . . ? O21 N21 Lu1 56.31(17) . . ? O32 N31 O31 123.3(3) . . ? O32 N31 O33 122.1(4) . . ? O31 N31 O33 114.6(3) . . ? O32 N31 Lu1 175.9(3) . . ? O31 N31 Lu1 58.68(17) . . ? O33 N31 Lu1 56.04(17) . . ? C4 C1 C3 108.6(3) . . ? C4 C1 C2 109.1(3) . . ? C3 C1 C2 105.3(3) . . ? C4 C1 P1 112.7(3) . . ? C3 C1 P1 112.6(3) . . ? C2 C1 P1 108.3(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C8 108.7(3) . . ? C6 C5 C7 104.9(3) . . ? C8 C5 C7 108.9(3) . . ? C6 C5 P1 110.3(3) . . ? C8 C5 P1 114.7(3) . . ? C7 C5 P1 108.9(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 C10 104.9(3) . . ? C11 C9 C12 109.9(3) . . ? C10 C9 C12 108.5(3) . . ? C11 C9 P1 108.4(3) . . ? C10 C9 P1 111.5(3) . . ? C12 C9 P1 113.4(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C16 109.0(3) . . ? C15 C13 C14 105.6(3) . . ? C16 C13 C14 108.6(3) . . ? C15 C13 P2 109.1(3) . . ? C16 C13 P2 113.7(3) . . ? C14 C13 P2 110.6(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C19 108.5(3) . . ? C18 C17 C20 106.7(3) . . ? C19 C17 C20 109.0(3) . . ? C18 C17 P2 109.7(3) . . ? C19 C17 P2 114.1(3) . . ? C20 C17 P2 108.6(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 C22 109.0(3) . . ? C23 C21 C24 105.8(3) . . ? C22 C21 C24 110.1(3) . . ? C23 C21 P2 110.3(3) . . ? C22 C21 P2 113.2(3) . . ? C24 C21 P2 108.2(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O3 Lu2 O4 180.000(2) . . ? O3 Lu2 O41 91.63(7) . 3_675 ? O4 Lu2 O41 88.37(7) . 3_675 ? O3 Lu2 O41 91.63(7) . 2_765 ? O4 Lu2 O41 88.37(7) . 2_765 ? O41 Lu2 O41 119.920(8) 3_675 2_765 ? O3 Lu2 O41 91.63(7) . . ? O4 Lu2 O41 88.37(7) . . ? O41 Lu2 O41 119.920(7) 3_675 . ? O41 Lu2 O41 119.920(9) 2_765 . ? O3 Lu2 O42 88.60(8) . 3_675 ? O4 Lu2 O42 91.40(8) . 3_675 ? O41 Lu2 O42 173.38(10) 3_675 3_675 ? O41 Lu2 O42 53.46(10) 2_765 3_675 ? O41 Lu2 O42 66.68(10) . 3_675 ? O3 Lu2 O42 88.60(8) . . ? O4 Lu2 O42 91.40(8) . . ? O41 Lu2 O42 53.46(10) 3_675 . ? O41 Lu2 O42 66.68(10) 2_765 . ? O41 Lu2 O42 173.38(10) . . ? O42 Lu2 O42 119.940(7) 3_675 . ? O3 Lu2 O42 88.60(8) . 2_765 ? O4 Lu2 O42 91.40(8) . 2_765 ? O41 Lu2 O42 66.68(10) 3_675 2_765 ? O41 Lu2 O42 173.38(10) 2_765 2_765 ? O41 Lu2 O42 53.46(10) . 2_765 ? O42 Lu2 O42 119.940(8) 3_675 2_765 ? O42 Lu2 O42 119.940(8) . 2_765 ? O3 Lu2 N41 90.29(7) . 3_675 ? O4 Lu2 N41 89.71(7) . 3_675 ? O41 Lu2 N41 26.80(10) 3_675 3_675 ? O41 Lu2 N41 93.22(10) 2_765 3_675 ? O41 Lu2 N41 146.72(10) . 3_675 ? O42 Lu2 N41 146.60(10) 3_675 3_675 ? O42 Lu2 N41 26.67(10) . 3_675 ? O42 Lu2 N41 93.39(10) 2_765 3_675 ? O3 Lu2 N41 90.29(6) . 2_765 ? O4 Lu2 N41 89.71(6) . 2_765 ? O41 Lu2 N41 146.72(10) 3_675 2_765 ? O41 Lu2 N41 26.80(10) 2_765 2_765 ? O41 Lu2 N41 93.22(10) . 2_765 ? O42 Lu2 N41 26.67(10) 3_675 2_765 ? O42 Lu2 N41 93.39(10) . 2_765 ? O42 Lu2 N41 146.60(10) 2_765 2_765 ? N41 Lu2 N41 119.998(2) 3_675 2_765 ? O3 Lu2 N41 90.29(6) . . ? O4 Lu2 N41 89.71(6) . . ? O41 Lu2 N41 93.22(10) 3_675 . ? O41 Lu2 N41 146.72(10) 2_765 . ? O41 Lu2 N41 26.80(10) . . ? O42 Lu2 N41 93.39(10) 3_675 . ? O42 Lu2 N41 146.60(10) . . ? O42 Lu2 N41 26.67(10) 2_765 . ? N41 Lu2 N41 119.998(2) 3_675 . ? N41 Lu2 N41 119.998(3) 2_765 . ? O3 P3 C25 107.21(12) . 3_675 ? O3 P3 C25 107.21(12) . 2_765 ? C25 P3 C25 111.64(11) 3_675 2_765 ? O3 P3 C25 107.21(12) . . ? C25 P3 C25 111.64(11) 3_675 . ? C25 P3 C25 111.64(11) 2_765 . ? O4 P4 C28 107.58(12) . 3_675 ? O4 P4 C28 107.58(12) . . ? C28 P4 C28 111.29(11) 3_675 . ? O4 P4 C28 107.58(12) . 2_765 ? C28 P4 C28 111.29(11) 3_675 2_765 ? C28 P4 C28 111.29(11) . 2_765 ? P3 O3 Lu2 180.000(1) . . ? P4 O4 Lu2 180.0 . . ? N41 O41 Lu2 95.9(2) . . ? N41 O42 Lu2 95.6(2) 3_675 . ? O43 N41 O42 122.8(4) . 2_765 ? O43 N41 O41 122.1(4) . . ? O42 N41 O41 115.1(3) 2_765 . ? O43 N41 Lu2 178.6(3) . . ? O42 N41 Lu2 57.73(18) 2_765 . ? O41 N41 Lu2 57.34(18) . . ? C27 C25 C26 105.5(3) . . ? C27 C25 C61 109.1(3) . . ? C26 C25 C61 109.2(3) . . ? C27 C25 P3 111.2(3) . . ? C26 C25 P3 108.5(3) . . ? C61 C25 P3 113.0(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C31 C28 C29 108.5(3) . . ? C31 C28 C30 109.4(3) . . ? C29 C28 C30 105.6(3) . . ? C31 C28 P4 114.3(3) . . ? C29 C28 P4 109.2(3) . . ? C30 C28 P4 109.5(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C25 C61 H61A 109.5 . . ? C25 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C25 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.579 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.070 #===END data_Tb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C24 H54 N3 O11 P2 Tb), C2 H3 N' _chemical_formula_sum 'C33.33 H74 N4.67 O14.67 P2.67 Tb1.33' _chemical_formula_weight 1069.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7432(13) _cell_length_b 16.6395(16) _cell_length_c 31.248(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.244(2) _cell_angle_gamma 90.00 _cell_volume 7140.3(12) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 26900 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 31.3 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3304 _exptl_absorpt_coefficient_mu 2.125 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8484 _exptl_absorpt_correction_T_max 0.9012 _exptl_absorpt_process_details 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_source_power 1.2 _diffrn_source_voltage 50.0 _diffrn_source_current 24.0 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_source 'Rotating Anode' _diffrn_radiation_monochromator 'Confocal' _diffrn_measurement_specimen_support 'Mitegen' _diffrn_detector 'CCD' _diffrn_measurement_device ; AFC12 (Right): Kappa 3 circle ; _diffrn_measurement_device_type ; Rigaku Saturn724+ (2x2 bin mode) ; _diffrn_detector_area_resol_mean 28.5714 _diffrn_measurement_method 'profile data from \w-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46494 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16204 _reflns_number_gt 14844 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _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^ > 2\s(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^)+(0.0185P)^2^+9.6370P] 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 16204 _refine_ls_number_parameters 788 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.003 _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 C1 C -0.0235(2) 0.29037(18) 0.08728(11) 0.0184(6) Uani 1 1 d . . . C2 C 0.0073(2) 0.20816(19) 0.06984(12) 0.0255(7) Uani 1 1 d . . . H2A H -0.0493 0.1814 0.0561 0.038 Uiso 1 1 calc R . . H2B H 0.0334 0.1749 0.0935 0.038 Uiso 1 1 calc R . . H2C H 0.0575 0.2158 0.0488 0.038 Uiso 1 1 calc R . . C3 C -0.0622(2) 0.3377(2) 0.04779(11) 0.0250(7) Uani 1 1 d . . . H3A H -0.0089 0.3471 0.0285 0.037 Uiso 1 1 calc R . . H3B H -0.0885 0.3894 0.0570 0.037 Uiso 1 1 calc R . . H3C H -0.1137 0.3067 0.0328 0.037 Uiso 1 1 calc R . . C4 C -0.1075(2) 0.27838(19) 0.11830(11) 0.0230(7) Uani 1 1 d . . . H4A H -0.1640 0.2553 0.1026 0.034 Uiso 1 1 calc R . . H4B H -0.1254 0.3304 0.1304 0.034 Uiso 1 1 calc R . . H4C H -0.0863 0.2419 0.1414 0.034 Uiso 1 1 calc R . . C5 C 0.0699(2) 0.45145(17) 0.11585(10) 0.0177(6) Uani 1 1 d . . . C6 C 0.0830(2) 0.48592(18) 0.07025(11) 0.0236(7) Uani 1 1 d . . . H6A H 0.0331 0.4633 0.0505 0.035 Uiso 1 1 calc R . . H6B H 0.1477 0.4717 0.0606 0.035 Uiso 1 1 calc R . . H6C H 0.0764 0.5445 0.0709 0.035 Uiso 1 1 calc R . . C7 C 0.1509(2) 0.49019(18) 0.14435(11) 0.0240(7) Uani 1 1 d . . . H7A H 0.1473 0.5488 0.1416 0.036 Uiso 1 1 calc R . . H7B H 0.2145 0.4715 0.1353 0.036 Uiso 1 1 calc R . . H7C H 0.1424 0.4750 0.1743 0.036 Uiso 1 1 calc R . . C8 C -0.0298(2) 0.47609(18) 0.13238(11) 0.0228(7) Uani 1 1 d . . . H8A H -0.0374 0.4535 0.1610 0.034 Uiso 1 1 calc R . . H8B H -0.0816 0.4556 0.1129 0.034 Uiso 1 1 calc R . . H8C H -0.0338 0.5348 0.1338 0.034 Uiso 1 1 calc R . . C9 C 0.1201(2) 0.29548(17) 0.16641(10) 0.0161(6) Uani 1 1 d . . . C10 C 0.2276(2) 0.3164(2) 0.17796(11) 0.0248(7) Uani 1 1 d . . . H10A H 0.2484 0.2883 0.2043 0.037 Uiso 1 1 calc R . . H10B H 0.2340 0.3745 0.1822 0.037 Uiso 1 1 calc R . . H10C H 0.2686 0.2995 0.1546 0.037 Uiso 1 1 calc R . . C11 C 0.0553(2) 0.3238(2) 0.20277(10) 0.0240(7) Uani 1 1 d . . . H11A H 0.0761 0.2972 0.2296 0.036 Uiso 1 1 calc R . . H11B H -0.0127 0.3101 0.1956 0.036 Uiso 1 1 calc R . . H11C H 0.0615 0.3822 0.2062 0.036 Uiso 1 1 calc R . . C12 C 0.1164(2) 0.20274(18) 0.16416(11) 0.0244(7) Uani 1 1 d . . . H12A H 0.1565 0.1840 0.1409 0.037 Uiso 1 1 calc R . . H12B H 0.0489 0.1853 0.1587 0.037 Uiso 1 1 calc R . . H12C H 0.1413 0.1802 0.1914 0.037 Uiso 1 1 calc R . . C13 C 0.4707(2) 0.30563(18) -0.08264(10) 0.0171(6) Uani 1 1 d . . . C14 C 0.3625(2) 0.2838(2) -0.09216(11) 0.0237(7) Uani 1 1 d . . . H14A H 0.3410 0.3067 -0.1198 0.035 Uiso 1 1 calc R . . H14B H 0.3227 0.3058 -0.0696 0.035 Uiso 1 1 calc R . . H14C H 0.3553 0.2253 -0.0931 0.035 Uiso 1 1 calc R . . C15 C 0.5327(2) 0.2691(2) -0.11794(11) 0.0263(7) Uani 1 1 d . . . H15A H 0.5247 0.2106 -0.1183 0.039 Uiso 1 1 calc R . . H15B H 0.6014 0.2823 -0.1121 0.039 Uiso 1 1 calc R . . H15C H 0.5114 0.2911 -0.1458 0.039 Uiso 1 1 calc R . . C16 C 0.4760(3) 0.39817(19) -0.08494(11) 0.0288(8) Uani 1 1 d . . . H16A H 0.4479 0.4165 -0.1126 0.043 Uiso 1 1 calc R . . H16B H 0.5442 0.4153 -0.0820 0.043 Uiso 1 1 calc R . . H16C H 0.4394 0.4215 -0.0617 0.043 Uiso 1 1 calc R . . C17 C 0.5247(2) 0.15869(17) -0.02613(10) 0.0180(6) Uani 1 1 d . . . C18 C 0.5179(2) 0.13007(18) 0.02086(10) 0.0215(7) Uani 1 1 d . . . H18A H 0.5074 0.0718 0.0214 0.032 Uiso 1 1 calc R . . H18B H 0.4633 0.1572 0.0341 0.032 Uiso 1 1 calc R . . H18C H 0.5786 0.1431 0.0369 0.032 Uiso 1 1 calc R . . C19 C 0.4406(2) 0.11692(18) -0.05148(11) 0.0241(7) Uani 1 1 d . . . H19A H 0.4450 0.1292 -0.0820 0.036 Uiso 1 1 calc R . . H19B H 0.3782 0.1364 -0.0414 0.036 Uiso 1 1 calc R . . H19C H 0.4451 0.0587 -0.0472 0.036 Uiso 1 1 calc R . . C20 C 0.6223(2) 0.13088(19) -0.04317(11) 0.0261(8) Uani 1 1 d . . . H20A H 0.6257 0.0721 -0.0423 0.039 Uiso 1 1 calc R . . H20B H 0.6758 0.1534 -0.0253 0.039 Uiso 1 1 calc R . . H20C H 0.6278 0.1494 -0.0727 0.039 Uiso 1 1 calc R . . C21 C 0.6143(2) 0.32602(19) -0.00482(11) 0.0198(7) Uani 1 1 d . . . C22 C 0.6994(2) 0.3329(2) -0.03574(12) 0.0303(8) Uani 1 1 d . . . H22A H 0.6771 0.3613 -0.0618 0.045 Uiso 1 1 calc R . . H22B H 0.7217 0.2789 -0.0433 0.045 Uiso 1 1 calc R . . H22C H 0.7533 0.3627 -0.0217 0.045 Uiso 1 1 calc R . . C23 C 0.5823(2) 0.41125(19) 0.00823(11) 0.0254(7) Uani 1 1 d . . . H23A H 0.6348 0.4369 0.0254 0.038 Uiso 1 1 calc R . . H23B H 0.5238 0.4076 0.0251 0.038 Uiso 1 1 calc R . . H23C H 0.5681 0.4433 -0.0176 0.038 Uiso 1 1 calc R . . C24 C 0.6514(2) 0.2848(2) 0.03685(12) 0.0291(8) Uani 1 1 d . . . H24A H 0.6817 0.2333 0.0300 0.044 Uiso 1 1 calc R . . H24B H 0.5966 0.2755 0.0554 0.044 Uiso 1 1 calc R . . H24C H 0.6995 0.3195 0.0517 0.044 Uiso 1 1 calc R . . C25 C 0.4872(2) 1.08089(19) 0.17400(10) 0.0200(6) Uani 1 1 d . . . C26 C 0.4031(2) 1.1407(2) 0.17911(11) 0.0277(8) Uani 1 1 d . . . H26A H 0.4245 1.1947 0.1713 0.042 Uiso 1 1 calc R . . H26B H 0.3836 1.1407 0.2089 0.042 Uiso 1 1 calc R . . H26C H 0.3476 1.1248 0.1604 0.042 Uiso 1 1 calc R . . C27 C 0.4491(2) 0.9946(2) 0.18052(12) 0.0267(7) Uani 1 1 d . . . H27A H 0.4215 0.9902 0.2089 0.040 Uiso 1 1 calc R . . H27B H 0.5030 0.9564 0.1784 0.040 Uiso 1 1 calc R . . H27C H 0.3987 0.9824 0.1584 0.040 Uiso 1 1 calc R . . C28 C 0.5191(2) 1.0830(2) 0.12732(10) 0.0282(8) Uani 1 1 d . . . H28A H 0.4642 1.0677 0.1081 0.042 Uiso 1 1 calc R . . H28B H 0.5730 1.0452 0.1239 0.042 Uiso 1 1 calc R . . H28C H 0.5405 1.1374 0.1203 0.042 Uiso 1 1 calc R . . C29 C 0.5780(2) 1.0634(2) 0.26527(10) 0.0211(7) Uani 1 1 d . . . C30 C 0.6563(2) 1.0968(2) 0.29738(11) 0.0294(8) Uani 1 1 d . . . H30A H 0.6491 1.0715 0.3254 0.044 Uiso 1 1 calc R . . H30B H 0.6483 1.1551 0.3001 0.044 Uiso 1 1 calc R . . H30C H 0.7212 1.0849 0.2871 0.044 Uiso 1 1 calc R . . C31 C 0.4774(2) 1.0842(2) 0.28206(11) 0.0271(8) Uani 1 1 d . . . H31A H 0.4266 1.0594 0.2636 0.041 Uiso 1 1 calc R . . H31B H 0.4687 1.1427 0.2819 0.041 Uiso 1 1 calc R . . H31C H 0.4727 1.0639 0.3114 0.041 Uiso 1 1 calc R . . C32 C 0.5930(3) 0.9719(2) 0.26521(11) 0.0272(8) Uani 1 1 d . . . H32A H 0.5803 0.9503 0.2936 0.041 Uiso 1 1 calc R . . H32B H 0.6602 0.9597 0.2581 0.041 Uiso 1 1 calc R . . H32C H 0.5481 0.9473 0.2439 0.041 Uiso 1 1 calc R . . C33 C 0.6295(2) 1.21136(18) 0.20967(12) 0.0230(7) Uani 1 1 d . . . C34 C 0.6264(3) 1.2441(2) 0.16358(12) 0.0320(8) Uani 1 1 d . . . H34A H 0.5591 1.2438 0.1521 0.048 Uiso 1 1 calc R . . H34B H 0.6666 1.2100 0.1457 0.048 Uiso 1 1 calc R . . H34C H 0.6517 1.2991 0.1636 0.048 Uiso 1 1 calc R . . C35 C 0.7373(2) 1.2193(2) 0.22557(13) 0.0288(8) Uani 1 1 d . . . H35A H 0.7581 1.2754 0.2231 0.043 Uiso 1 1 calc R . . H35B H 0.7781 1.1851 0.2081 0.043 Uiso 1 1 calc R . . H35C H 0.7438 1.2024 0.2556 0.043 Uiso 1 1 calc R . . C36 C 0.5650(3) 1.2642(2) 0.23738(13) 0.0334(9) Uani 1 1 d . . . H36A H 0.5732 1.2478 0.2674 0.050 Uiso 1 1 calc R . . H36B H 0.4967 1.2577 0.2279 0.050 Uiso 1 1 calc R . . H36C H 0.5841 1.3206 0.2345 0.050 Uiso 1 1 calc R . . C37 C 1.0272(2) 0.91359(17) 0.07195(10) 0.0177(6) Uani 1 1 d . . . C38 C 1.1234(2) 0.89166(19) 0.05097(11) 0.0227(7) Uani 1 1 d . . . H38A H 1.1245 0.9159 0.0224 0.034 Uiso 1 1 calc R . . H38B H 1.1284 0.8331 0.0485 0.034 Uiso 1 1 calc R . . H38C H 1.1784 0.9120 0.0687 0.034 Uiso 1 1 calc R . . C39 C 1.0199(2) 1.00564(18) 0.07404(11) 0.0233(7) Uani 1 1 d . . . H39A H 1.0834 1.0280 0.0831 0.035 Uiso 1 1 calc R . . H39B H 0.9712 1.0209 0.0946 0.035 Uiso 1 1 calc R . . H39C H 1.0006 1.0267 0.0457 0.035 Uiso 1 1 calc R . . C40 C 0.9408(2) 0.8841(2) 0.04335(10) 0.0238(7) Uani 1 1 d . . . H40A H 0.9423 0.9106 0.0154 0.036 Uiso 1 1 calc R . . H40B H 0.8797 0.8972 0.0569 0.036 Uiso 1 1 calc R . . H40C H 0.9455 0.8258 0.0396 0.036 Uiso 1 1 calc R . . C41 C 0.9851(2) 0.76282(17) 0.12550(10) 0.0186(6) Uani 1 1 d . . . C42 C 0.8758(2) 0.75400(19) 0.11418(12) 0.0258(7) Uani 1 1 d . . . H42A H 0.8589 0.6969 0.1122 0.039 Uiso 1 1 calc R . . H42B H 0.8605 0.7802 0.0866 0.039 Uiso 1 1 calc R . . H42C H 0.8381 0.7793 0.1365 0.039 Uiso 1 1 calc R . . C43 C 1.0448(3) 0.71483(18) 0.09345(12) 0.0265(8) Uani 1 1 d . . . H43A H 1.0261 0.6580 0.0944 0.040 Uiso 1 1 calc R . . H43B H 1.1143 0.7201 0.1011 0.040 Uiso 1 1 calc R . . H43C H 1.0319 0.7358 0.0645 0.040 Uiso 1 1 calc R . . C44 C 1.0005(3) 0.72435(19) 0.17026(12) 0.0296(8) Uani 1 1 d . . . H44A H 0.9642 0.7550 0.1912 0.044 Uiso 1 1 calc R . . H44B H 1.0699 0.7250 0.1786 0.044 Uiso 1 1 calc R . . H44C H 0.9770 0.6687 0.1694 0.044 Uiso 1 1 calc R . . C45 C 1.1256(2) 0.89280(19) 0.16236(10) 0.0197(6) Uani 1 1 d . . . C46 C 1.2133(2) 0.8371(2) 0.15416(12) 0.0284(8) Uani 1 1 d . . . H46A H 1.2314 0.8423 0.1243 0.043 Uiso 1 1 calc R . . H46B H 1.1952 0.7812 0.1599 0.043 Uiso 1 1 calc R . . H46C H 1.2686 0.8525 0.1731 0.043 Uiso 1 1 calc R . . C47 C 1.1583(2) 0.9805(2) 0.15684(13) 0.0309(8) Uani 1 1 d . . . H47A H 1.2080 0.9938 0.1791 0.046 Uiso 1 1 calc R . . H47B H 1.1022 1.0163 0.1594 0.046 Uiso 1 1 calc R . . H47C H 1.1855 0.9873 0.1285 0.046 Uiso 1 1 calc R . . C48 C 1.0978(2) 0.8844(2) 0.20959(11) 0.0280(8) Uani 1 1 d . . . H48A H 1.1520 0.9029 0.2284 0.042 Uiso 1 1 calc R . . H48B H 1.0838 0.8280 0.2158 0.042 Uiso 1 1 calc R . . H48C H 1.0400 0.9171 0.2145 0.042 Uiso 1 1 calc R . . N11 N 0.26645(19) 0.13723(15) 0.04902(10) 0.0227(6) Uani 1 1 d . . . N21 N 0.4192(2) 0.38994(16) 0.10413(9) 0.0222(6) Uani 1 1 d . . . N31 N 0.1907(2) 0.39739(16) -0.02390(9) 0.0242(6) Uani 1 1 d . . . N41 N 0.76785(19) 1.04790(17) 0.08537(9) 0.0232(6) Uani 1 1 d . . . N51 N 0.69972(19) 0.83529(15) 0.19282(9) 0.0197(6) Uani 1 1 d . . . N61 N 0.9276(2) 1.05933(17) 0.23088(10) 0.0262(6) Uani 1 1 d . . . O1 O 0.17129(14) 0.32483(11) 0.08424(7) 0.0142(4) Uani 1 1 d . . . O2 O 0.42136(14) 0.28911(11) 0.00081(7) 0.0151(4) Uani 1 1 d . . . O3 O 0.68125(14) 1.05586(12) 0.19260(7) 0.0157(4) Uani 1 1 d . . . O4 O 0.93066(14) 0.91553(11) 0.14694(6) 0.0135(4) Uani 1 1 d . . . O11 O 0.23634(16) 0.17748(13) 0.01640(8) 0.0241(5) Uani 1 1 d . . . O12 O 0.31047(16) 0.17834(12) 0.07841(8) 0.0230(5) Uani 1 1 d . . . O13 O 0.25461(19) 0.06527(13) 0.05194(10) 0.0384(7) Uani 1 1 d . . . O21 O 0.36579(16) 0.42798(13) 0.07638(8) 0.0240(5) Uani 1 1 d . . . O22 O 0.41601(16) 0.31362(13) 0.10136(7) 0.0226(5) Uani 1 1 d . . . O23 O 0.4699(2) 0.42452(16) 0.13103(8) 0.0380(6) Uani 1 1 d . . . O31 O 0.16929(16) 0.32504(13) -0.01512(7) 0.0238(5) Uani 1 1 d . . . O32 O 0.26182(16) 0.42709(13) -0.00199(8) 0.0245(5) Uani 1 1 d . . . O33 O 0.1458(2) 0.43518(16) -0.05157(9) 0.0425(7) Uani 1 1 d . . . O41 O 0.73792(16) 0.97771(14) 0.09540(7) 0.0234(5) Uani 1 1 d . . . O42 O 0.81209(17) 1.08633(13) 0.11547(7) 0.0240(5) Uani 1 1 d . . . O43 O 0.75583(19) 1.07512(17) 0.04944(8) 0.0396(7) Uani 1 1 d . . . O51 O 0.77789(16) 0.85876(13) 0.21224(7) 0.0234(5) Uani 1 1 d . . . O52 O 0.67022(16) 0.87865(13) 0.16131(7) 0.0232(5) Uani 1 1 d . . . O53 O 0.65617(19) 0.77566(14) 0.20395(8) 0.0340(6) Uani 1 1 d . . . O61 O 0.91857(16) 1.08287(13) 0.19226(7) 0.0226(5) Uani 1 1 d . . . O62 O 0.87681(17) 0.99827(13) 0.24045(7) 0.0239(5) Uani 1 1 d . . . O63 O 0.9825(2) 1.09226(18) 0.25689(10) 0.0500(8) Uani 1 1 d . . . P1 P 0.08633(5) 0.34009(4) 0.11300(2) 0.01256(15) Uani 1 1 d . . . P2 P 0.50621(5) 0.27010(4) -0.02761(2) 0.01267(15) Uani 1 1 d . . . P3 P 0.59594(5) 1.10221(5) 0.21002(3) 0.01477(15) Uani 1 1 d . . . P4 P 1.01584(5) 0.87214(4) 0.12715(2) 0.01215(14) Uani 1 1 d . . . Tb1 Tb 0.295191(9) 0.307698(8) 0.041941(4) 0.01181(4) Uani 1 1 d . . . Tb2 Tb 0.800335(9) 0.980329(8) 0.169002(4) 0.01167(4) Uani 1 1 d . . . N71 N 0.2711(4) 0.9436(3) 0.29350(16) 0.0778(14) Uiso 1 1 d . . . C49 C 0.2150(4) 1.0924(3) 0.30252(19) 0.0735(16) Uiso 1 1 d . . . H49A H 0.2609 1.1274 0.2882 0.110 Uiso 1 1 calc R . . H49B H 0.2143 1.1063 0.3330 0.110 Uiso 1 1 calc R . . H49C H 0.1496 1.0996 0.2894 0.110 Uiso 1 1 calc R . . C50 C 0.2452(4) 1.0080(3) 0.29797(17) 0.0545(12) Uiso 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 C1 0.0120(14) 0.0187(14) 0.0246(18) -0.0066(12) 0.0030(12) -0.0010(12) C2 0.0218(16) 0.0228(16) 0.032(2) -0.0130(14) 0.0039(15) -0.0070(13) C3 0.0194(16) 0.0351(18) 0.0200(18) -0.0037(14) -0.0042(14) -0.0008(14) C4 0.0158(15) 0.0237(16) 0.0298(19) -0.0039(14) 0.0054(14) -0.0058(13) C5 0.0182(15) 0.0127(13) 0.0226(17) -0.0002(11) 0.0054(13) 0.0032(12) C6 0.0269(17) 0.0164(15) 0.0281(19) 0.0015(13) 0.0068(15) 0.0006(13) C7 0.0264(17) 0.0168(15) 0.0291(19) -0.0082(13) 0.0055(15) -0.0046(13) C8 0.0235(16) 0.0156(14) 0.0299(19) -0.0008(13) 0.0091(14) 0.0038(13) C9 0.0162(14) 0.0193(14) 0.0131(15) 0.0008(11) 0.0012(12) 0.0000(12) C10 0.0203(16) 0.0337(18) 0.0203(18) 0.0038(14) -0.0007(14) 0.0032(14) C11 0.0265(17) 0.0311(17) 0.0148(17) -0.0016(13) 0.0054(14) 0.0000(14) C12 0.0264(17) 0.0192(15) 0.0281(19) 0.0066(13) 0.0066(15) 0.0047(13) C13 0.0214(15) 0.0204(14) 0.0096(15) 0.0035(11) 0.0022(12) 0.0025(12) C14 0.0211(16) 0.0320(17) 0.0176(17) -0.0030(13) -0.0033(13) 0.0058(14) C15 0.0274(17) 0.0349(19) 0.0171(18) 0.0039(14) 0.0086(14) 0.0037(15) C16 0.041(2) 0.0231(16) 0.0219(19) 0.0077(13) 0.0003(16) 0.0040(15) C17 0.0200(15) 0.0159(14) 0.0187(17) 0.0014(12) 0.0064(13) 0.0042(12) C18 0.0251(16) 0.0196(15) 0.0201(17) 0.0073(12) 0.0045(14) 0.0052(13) C19 0.0324(18) 0.0168(15) 0.0232(18) -0.0019(12) 0.0021(15) -0.0016(13) C20 0.0277(18) 0.0238(16) 0.0274(19) 0.0009(14) 0.0093(15) 0.0139(14) C21 0.0123(14) 0.0249(16) 0.0223(18) -0.0003(13) 0.0019(13) -0.0032(12) C22 0.0154(16) 0.041(2) 0.035(2) 0.0002(16) 0.0067(15) -0.0075(15) C23 0.0244(17) 0.0239(16) 0.0280(19) -0.0061(14) 0.0019(15) -0.0085(14) C24 0.0205(16) 0.039(2) 0.028(2) -0.0018(15) -0.0062(15) 0.0011(15) C25 0.0140(14) 0.0316(17) 0.0143(16) -0.0005(13) -0.0005(12) 0.0039(13) C26 0.0172(16) 0.043(2) 0.0231(19) 0.0050(15) 0.0005(14) 0.0106(15) C27 0.0170(16) 0.0356(19) 0.027(2) -0.0058(15) -0.0003(14) -0.0012(14) C28 0.0200(16) 0.051(2) 0.0139(17) -0.0040(15) -0.0015(13) 0.0042(16) C29 0.0214(16) 0.0306(17) 0.0115(16) 0.0001(12) 0.0018(13) 0.0065(13) C30 0.0254(17) 0.046(2) 0.0164(18) -0.0039(15) -0.0023(14) 0.0105(16) C31 0.0248(17) 0.040(2) 0.0175(18) 0.0007(14) 0.0083(14) 0.0054(15) C32 0.0318(19) 0.0304(18) 0.0197(18) 0.0093(14) 0.0033(15) 0.0071(15) C33 0.0193(16) 0.0169(15) 0.033(2) -0.0013(13) 0.0026(14) 0.0056(12) C34 0.0313(19) 0.0290(18) 0.036(2) 0.0112(16) 0.0073(17) 0.0047(15) C35 0.0219(17) 0.0222(16) 0.042(2) -0.0082(15) -0.0004(16) -0.0013(14) C36 0.0306(19) 0.0245(17) 0.045(2) -0.0098(16) 0.0033(17) 0.0069(15) C37 0.0219(15) 0.0169(14) 0.0146(16) 0.0047(11) 0.0059(13) 0.0042(12) C38 0.0242(16) 0.0234(16) 0.0213(18) 0.0031(13) 0.0131(14) 0.0049(13) C39 0.0254(17) 0.0191(15) 0.0261(19) 0.0078(13) 0.0075(14) 0.0051(13) C40 0.0264(17) 0.0303(17) 0.0144(16) 0.0011(13) -0.0006(14) 0.0035(14) C41 0.0206(15) 0.0124(13) 0.0231(17) -0.0007(12) 0.0070(13) 0.0010(12) C42 0.0255(17) 0.0217(16) 0.031(2) -0.0072(14) 0.0070(15) -0.0094(14) C43 0.0327(19) 0.0140(14) 0.033(2) -0.0050(13) 0.0093(16) 0.0033(13) C44 0.039(2) 0.0174(15) 0.033(2) 0.0082(14) 0.0101(17) 0.0000(15) C45 0.0149(14) 0.0259(16) 0.0182(17) -0.0039(12) -0.0009(12) 0.0043(12) C46 0.0156(15) 0.040(2) 0.030(2) 0.0017(15) 0.0001(14) 0.0086(15) C47 0.0224(17) 0.0319(19) 0.038(2) -0.0090(16) 0.0006(16) -0.0082(15) C48 0.0245(17) 0.041(2) 0.0181(18) -0.0044(15) -0.0041(14) 0.0046(15) N11 0.0151(13) 0.0160(12) 0.0377(18) 0.0021(12) 0.0111(12) 0.0004(10) N21 0.0243(14) 0.0261(14) 0.0164(15) -0.0030(11) 0.0031(12) -0.0061(12) N31 0.0245(14) 0.0249(14) 0.0231(16) 0.0013(11) -0.0008(12) 0.0090(12) N41 0.0185(13) 0.0318(15) 0.0196(15) 0.0089(12) 0.0049(12) 0.0107(12) N51 0.0238(14) 0.0189(12) 0.0168(14) -0.0016(10) 0.0069(11) -0.0028(11) N61 0.0227(14) 0.0278(15) 0.0278(17) -0.0120(12) -0.0018(12) 0.0008(12) O1 0.0120(9) 0.0159(10) 0.0151(11) -0.0036(8) 0.0039(8) 0.0016(8) O2 0.0136(10) 0.0163(10) 0.0157(11) -0.0011(8) 0.0045(8) 0.0019(8) O3 0.0141(10) 0.0172(10) 0.0159(11) -0.0025(8) 0.0021(8) 0.0044(8) O4 0.0125(10) 0.0128(9) 0.0153(11) -0.0005(8) 0.0027(8) 0.0016(8) O11 0.0242(12) 0.0213(11) 0.0265(14) -0.0018(9) -0.0020(10) -0.0032(9) O12 0.0255(12) 0.0181(11) 0.0253(13) 0.0022(9) -0.0002(10) 0.0031(9) O13 0.0379(15) 0.0145(11) 0.063(2) 0.0035(12) 0.0110(14) -0.0037(11) O21 0.0250(12) 0.0201(11) 0.0265(13) 0.0002(9) -0.0026(10) -0.0020(9) O22 0.0257(12) 0.0205(11) 0.0214(13) -0.0008(9) -0.0033(10) -0.0010(9) O23 0.0478(16) 0.0406(15) 0.0248(15) -0.0061(11) -0.0095(12) -0.0169(13) O31 0.0248(12) 0.0240(11) 0.0222(13) -0.0002(9) -0.0049(10) 0.0002(10) O32 0.0231(12) 0.0213(11) 0.0287(14) 0.0057(10) -0.0034(10) 0.0002(9) O33 0.0501(17) 0.0379(15) 0.0377(17) 0.0090(12) -0.0212(14) 0.0156(13) O41 0.0224(12) 0.0316(12) 0.0163(12) 0.0011(9) -0.0001(9) 0.0011(10) O42 0.0289(12) 0.0203(11) 0.0233(13) 0.0032(9) 0.0063(10) 0.0003(10) O43 0.0368(15) 0.0587(18) 0.0236(15) 0.0193(13) 0.0035(12) 0.0126(13) O51 0.0206(11) 0.0260(12) 0.0236(13) 0.0065(9) -0.0016(10) -0.0051(9) O52 0.0248(12) 0.0200(11) 0.0245(13) 0.0017(9) -0.0046(10) -0.0044(9) O53 0.0435(15) 0.0251(12) 0.0340(16) 0.0028(11) 0.0088(12) -0.0161(11) O61 0.0239(12) 0.0229(11) 0.0211(13) -0.0041(9) 0.0028(10) -0.0065(9) O62 0.0277(12) 0.0258(12) 0.0177(12) 0.0000(9) -0.0034(10) -0.0020(10) O63 0.0535(18) 0.0550(18) 0.0399(19) -0.0176(14) -0.0204(15) -0.0170(15) P1 0.0117(3) 0.0114(3) 0.0147(4) -0.0014(3) 0.0031(3) 0.0003(3) P2 0.0110(3) 0.0146(3) 0.0127(4) 0.0007(3) 0.0027(3) 0.0005(3) P3 0.0133(4) 0.0188(4) 0.0123(4) -0.0013(3) 0.0013(3) 0.0045(3) P4 0.0117(3) 0.0112(3) 0.0138(4) 0.0001(3) 0.0023(3) 0.0015(3) Tb1 0.01048(7) 0.01295(6) 0.01211(7) -0.00018(5) 0.00179(5) 0.00084(5) Tb2 0.01056(7) 0.01266(6) 0.01190(7) -0.00074(5) 0.00199(5) 0.00109(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.538(4) . ? C1 C3 1.541(5) . ? C1 C4 1.549(4) . ? C1 P1 1.875(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.538(4) . ? C5 C7 1.540(4) . ? C5 C6 1.553(4) . ? C5 P1 1.869(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.545(4) . ? C9 C12 1.546(4) . ? C9 C10 1.546(4) . ? C9 P1 1.869(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C16 1.543(4) . ? C13 C15 1.545(4) . ? C13 C14 1.548(4) . ? C13 P2 1.865(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C20 1.534(4) . ? C17 C19 1.541(4) . ? C17 C18 1.550(4) . ? C17 P2 1.872(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.540(5) . ? C21 C23 1.544(4) . ? C21 C22 1.550(4) . ? C21 P2 1.871(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.539(4) . ? C25 C28 1.540(4) . ? C25 C27 1.545(4) . ? C25 P3 1.869(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C32 1.537(4) . ? C29 C31 1.538(4) . ? C29 C30 1.545(5) . ? C29 P3 1.869(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C36 1.538(4) . ? C33 C34 1.539(5) . ? C33 C35 1.550(4) . ? C33 P3 1.874(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C39 1.536(4) . ? C37 C40 1.538(4) . ? C37 C38 1.543(4) . ? C37 P4 1.870(3) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.538(4) . ? C41 C43 1.542(4) . ? C41 C44 1.545(5) . ? C41 P4 1.868(3) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C47 1.539(4) . ? C45 C48 1.545(4) . ? C45 C46 1.549(4) . ? C45 P4 1.864(3) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? N11 O13 1.212(3) . ? N11 O11 1.275(3) . ? N11 O12 1.278(4) . ? N11 Tb1 2.874(3) . ? N21 O23 1.215(3) . ? N21 O22 1.274(3) . ? N21 O21 1.281(3) . ? N21 Tb1 2.880(3) . ? N31 O33 1.218(4) . ? N31 O32 1.271(4) . ? N31 O31 1.272(3) . ? N31 Tb1 2.879(3) . ? N41 O43 1.216(3) . ? N41 O42 1.272(4) . ? N41 O41 1.281(3) . ? N41 Tb2 2.864(3) . ? N51 O53 1.217(3) . ? N51 O51 1.274(3) . ? N51 O52 1.274(3) . ? N51 Tb2 2.893(3) . ? N61 O63 1.217(4) . ? N61 O61 1.270(4) . ? N61 O62 1.275(3) . ? N61 Tb2 2.875(3) . ? O1 P1 1.522(2) . ? O1 Tb1 2.2145(19) . ? O2 P2 1.526(2) . ? O2 Tb1 2.2200(19) . ? O3 P3 1.522(2) . ? O3 Tb2 2.2127(19) . ? O4 P4 1.5267(19) . ? O4 Tb2 2.2232(18) . ? O11 Tb1 2.436(2) . ? O12 Tb1 2.441(2) . ? O21 Tb1 2.454(2) . ? O22 Tb1 2.444(2) . ? O31 Tb1 2.452(2) . ? O32 Tb1 2.448(2) . ? O41 Tb2 2.423(2) . ? O42 Tb2 2.441(2) . ? O51 Tb2 2.459(2) . ? O52 Tb2 2.467(2) . ? O61 Tb2 2.447(2) . ? O62 Tb2 2.448(2) . ? N71 C50 1.139(6) . ? C49 C50 1.472(7) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C3 105.2(3) . . ? C2 C1 C4 109.2(2) . . ? C3 C1 C4 109.0(3) . . ? C2 C1 P1 108.4(2) . . ? C3 C1 P1 111.4(2) . . ? C4 C1 P1 113.3(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C5 C7 109.1(3) . . ? C8 C5 C6 110.3(3) . . ? C7 C5 C6 105.6(3) . . ? C8 C5 P1 113.0(2) . . ? C7 C5 P1 110.9(2) . . ? C6 C5 P1 107.7(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 C12 108.6(2) . . ? C11 C9 C10 109.4(3) . . ? C12 C9 C10 105.4(3) . . ? C11 C9 P1 113.9(2) . . ? C12 C9 P1 110.4(2) . . ? C10 C9 P1 108.7(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C13 C15 109.3(3) . . ? C16 C13 C14 105.8(3) . . ? C15 C13 C14 108.9(3) . . ? C16 C13 P2 110.4(2) . . ? C15 C13 P2 113.7(2) . . ? C14 C13 P2 108.5(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C17 C19 109.5(3) . . ? C20 C17 C18 108.8(3) . . ? C19 C17 C18 106.0(2) . . ? C20 C17 P2 114.2(2) . . ? C19 C17 P2 109.6(2) . . ? C18 C17 P2 108.3(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 C23 105.9(3) . . ? C24 C21 C22 109.1(3) . . ? C23 C21 C22 109.1(3) . . ? C24 C21 P2 109.4(2) . . ? C23 C21 P2 109.1(2) . . ? C22 C21 P2 114.0(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C28 109.1(3) . . ? C26 C25 C27 109.1(3) . . ? C28 C25 C27 104.9(3) . . ? C26 C25 P3 113.6(2) . . ? C28 C25 P3 108.4(2) . . ? C27 C25 P3 111.3(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C32 C29 C31 110.3(3) . . ? C32 C29 C30 105.5(3) . . ? C31 C29 C30 108.1(3) . . ? C32 C29 P3 108.6(2) . . ? C31 C29 P3 112.9(2) . . ? C30 C29 P3 111.2(2) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C36 C33 C34 109.2(3) . . ? C36 C33 C35 109.6(3) . . ? C34 C33 C35 105.1(3) . . ? C36 C33 P3 113.8(2) . . ? C34 C33 P3 110.5(2) . . ? C35 C33 P3 108.2(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C40 107.0(3) . . ? C39 C37 C38 108.2(2) . . ? C40 C37 C38 109.4(3) . . ? C39 C37 P4 108.7(2) . . ? C40 C37 P4 109.2(2) . . ? C38 C37 P4 114.1(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C43 110.0(3) . . ? C42 C41 C44 105.4(3) . . ? C43 C41 C44 108.4(3) . . ? C42 C41 P4 108.5(2) . . ? C43 C41 P4 113.4(2) . . ? C44 C41 P4 110.8(2) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C47 C45 C48 106.1(3) . . ? C47 C45 C46 108.5(3) . . ? C48 C45 C46 109.1(3) . . ? C47 C45 P4 110.0(2) . . ? C48 C45 P4 108.8(2) . . ? C46 C45 P4 114.1(2) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O13 N11 O11 122.6(3) . . ? O13 N11 O12 122.4(3) . . ? O11 N11 O12 115.0(2) . . ? O13 N11 Tb1 179.8(3) . . ? O11 N11 Tb1 57.40(14) . . ? O12 N11 Tb1 57.62(14) . . ? O23 N21 O22 122.5(3) . . ? O23 N21 O21 122.1(3) . . ? O22 N21 O21 115.4(3) . . ? O23 N21 Tb1 178.5(2) . . ? O22 N21 Tb1 57.47(15) . . ? O21 N21 Tb1 57.98(14) . . ? O33 N31 O32 122.7(3) . . ? O33 N31 O31 121.8(3) . . ? O32 N31 O31 115.6(3) . . ? O33 N31 Tb1 179.4(3) . . ? O32 N31 Tb1 57.67(15) . . ? O31 N31 Tb1 57.88(15) . . ? O43 N41 O42 122.6(3) . . ? O43 N41 O41 122.2(3) . . ? O42 N41 O41 115.2(3) . . ? O43 N41 Tb2 178.3(2) . . ? O42 N41 Tb2 57.98(14) . . ? O41 N41 Tb2 57.25(15) . . ? O53 N51 O51 121.9(3) . . ? O53 N51 O52 122.5(3) . . ? O51 N51 O52 115.5(2) . . ? O53 N51 Tb2 177.9(2) . . ? O51 N51 Tb2 57.61(14) . . ? O52 N51 Tb2 57.97(14) . . ? O63 N61 O61 122.1(3) . . ? O63 N61 O62 122.2(3) . . ? O61 N61 O62 115.7(3) . . ? O63 N61 Tb2 179.2(3) . . ? O61 N61 Tb2 57.82(14) . . ? O62 N61 Tb2 57.91(15) . . ? P1 O1 Tb1 177.78(13) . . ? P2 O2 Tb1 175.99(13) . . ? P3 O3 Tb2 175.81(13) . . ? P4 O4 Tb2 174.16(13) . . ? N11 O11 Tb1 96.43(17) . . ? N11 O12 Tb1 96.13(17) . . ? N21 O21 Tb1 95.75(16) . . ? N21 O22 Tb1 96.46(18) . . ? N31 O31 Tb1 96.06(18) . . ? N31 O32 Tb1 96.30(17) . . ? N41 O41 Tb2 96.35(18) . . ? N41 O42 Tb2 95.80(17) . . ? N51 O51 Tb2 96.44(17) . . ? N51 O52 Tb2 96.06(17) . . ? N61 O61 Tb2 96.11(17) . . ? N61 O62 Tb2 95.91(18) . . ? O1 P1 C9 106.95(13) . . ? O1 P1 C5 106.89(12) . . ? C9 P1 C5 112.18(14) . . ? O1 P1 C1 107.26(13) . . ? C9 P1 C1 112.05(14) . . ? C5 P1 C1 111.16(14) . . ? O2 P2 C13 107.01(13) . . ? O2 P2 C21 106.80(13) . . ? C13 P2 C21 111.63(14) . . ? O2 P2 C17 107.27(12) . . ? C13 P2 C17 111.54(14) . . ? C21 P2 C17 112.23(14) . . ? O3 P3 C29 106.65(13) . . ? O3 P3 C25 107.29(13) . . ? C29 P3 C25 111.09(15) . . ? O3 P3 C33 107.21(13) . . ? C29 P3 C33 112.44(15) . . ? C25 P3 C33 111.81(15) . . ? O4 P4 C45 106.83(13) . . ? O4 P4 C41 107.20(12) . . ? C45 P4 C41 111.88(15) . . ? O4 P4 C37 106.98(12) . . ? C45 P4 C37 112.45(14) . . ? C41 P4 C37 111.15(14) . . ? O1 Tb1 O2 178.64(8) . . ? O1 Tb1 O11 93.26(7) . . ? O2 Tb1 O11 86.74(7) . . ? O1 Tb1 O12 83.62(7) . . ? O2 Tb1 O12 95.31(7) . . ? O11 Tb1 O12 52.41(8) . . ? O1 Tb1 O22 93.26(8) . . ? O2 Tb1 O22 85.56(8) . . ? O11 Tb1 O22 119.45(7) . . ? O12 Tb1 O22 68.74(7) . . ? O1 Tb1 O32 95.66(7) . . ? O2 Tb1 O32 85.52(7) . . ? O11 Tb1 O32 119.05(8) . . ? O12 Tb1 O32 171.25(8) . . ? O22 Tb1 O32 120.01(7) . . ? O1 Tb1 O31 83.20(8) . . ? O2 Tb1 O31 98.07(8) . . ? O11 Tb1 O31 69.56(8) . . ? O12 Tb1 O31 119.25(8) . . ? O22 Tb1 O31 170.61(7) . . ? O32 Tb1 O31 52.08(7) . . ? O1 Tb1 O21 86.18(7) . . ? O2 Tb1 O21 93.62(7) . . ? O11 Tb1 O21 171.64(8) . . ? O12 Tb1 O21 119.28(8) . . ? O22 Tb1 O21 52.32(7) . . ? O32 Tb1 O21 69.28(8) . . ? O31 Tb1 O21 118.58(7) . . ? O1 Tb1 N11 88.27(7) . . ? O2 Tb1 N11 91.14(7) . . ? O11 Tb1 N11 26.16(8) . . ? O12 Tb1 N11 26.24(8) . . ? O22 Tb1 N11 94.16(8) . . ? O32 Tb1 N11 145.19(8) . . ? O31 Tb1 N11 94.42(8) . . ? O21 Tb1 N11 145.52(8) . . ? O1 Tb1 N31 89.21(8) . . ? O2 Tb1 N31 92.15(8) . . ? O11 Tb1 N31 94.42(8) . . ? O12 Tb1 N31 145.29(8) . . ? O22 Tb1 N31 145.79(8) . . ? O32 Tb1 N31 26.03(7) . . ? O31 Tb1 N31 26.05(7) . . ? O21 Tb1 N31 93.91(8) . . ? N11 Tb1 N31 120.03(8) . . ? O1 Tb1 N21 89.13(7) . . ? O2 Tb1 N21 90.10(7) . . ? O11 Tb1 N21 145.46(8) . . ? O12 Tb1 N21 93.79(8) . . ? O22 Tb1 N21 26.06(7) . . ? O32 Tb1 N21 94.92(8) . . ? O31 Tb1 N21 144.76(8) . . ? O21 Tb1 N21 26.27(7) . . ? N11 Tb1 N21 119.77(8) . . ? N31 Tb1 N21 120.08(8) . . ? O3 Tb2 O4 173.81(7) . . ? O3 Tb2 O41 95.02(8) . . ? O4 Tb2 O41 87.50(7) . . ? O3 Tb2 O42 83.54(7) . . ? O4 Tb2 O42 93.57(7) . . ? O41 Tb2 O42 52.62(8) . . ? O3 Tb2 O61 89.78(7) . . ? O4 Tb2 O61 84.07(7) . . ? O41 Tb2 O61 120.04(8) . . ? O42 Tb2 O61 68.82(8) . . ? O3 Tb2 O62 85.62(8) . . ? O4 Tb2 O62 91.12(8) . . ? O41 Tb2 O62 172.29(7) . . ? O42 Tb2 O62 119.96(8) . . ? O61 Tb2 O62 52.25(7) . . ? O3 Tb2 O51 100.01(8) . . ? O4 Tb2 O51 83.76(7) . . ? O41 Tb2 O51 117.35(8) . . ? O42 Tb2 O51 169.84(8) . . ? O61 Tb2 O51 120.44(8) . . ? O62 Tb2 O51 69.99(8) . . ? O3 Tb2 O52 83.06(7) . . ? O4 Tb2 O52 103.11(7) . . ? O41 Tb2 O52 70.54(8) . . ? O42 Tb2 O52 119.74(8) . . ? O61 Tb2 O52 167.88(8) . . ? O62 Tb2 O52 117.14(8) . . ? O51 Tb2 O52 51.92(7) . . ? O3 Tb2 N41 89.44(8) . . ? O4 Tb2 N41 90.35(7) . . ? O41 Tb2 N41 26.40(8) . . ? O42 Tb2 N41 26.23(8) . . ? O61 Tb2 N41 94.32(8) . . ? O62 Tb2 N41 146.13(8) . . ? O51 Tb2 N41 143.71(8) . . ? O52 Tb2 N41 95.38(8) . . ? O3 Tb2 N61 87.41(8) . . ? O4 Tb2 N61 87.36(8) . . ? O41 Tb2 N61 146.11(8) . . ? O42 Tb2 N61 94.34(8) . . ? O61 Tb2 N61 26.07(8) . . ? O62 Tb2 N61 26.18(8) . . ? O51 Tb2 N61 95.32(8) . . ? O52 Tb2 N61 143.04(8) . . ? N41 Tb2 N61 120.22(9) . . ? O3 Tb2 N51 91.20(7) . . ? O4 Tb2 N51 94.25(7) . . ? O41 Tb2 N51 94.26(8) . . ? O42 Tb2 N51 145.52(8) . . ? O61 Tb2 N51 145.46(8) . . ? O62 Tb2 N51 93.41(8) . . ? O51 Tb2 N51 25.95(7) . . ? O52 Tb2 N51 25.97(7) . . ? N41 Tb2 N51 120.22(8) . . ? N61 Tb2 N51 119.52(8) . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N71 C50 C49 177.5(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.062 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.099 #===END