# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_publication_text #TrackingRef '- SI-cif.txt' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Weisheng Liu' _publ_contact_author_address ; Key Laboratory of Nonferrous Metals Chemistry and Resources Utilization of Gansu Province and State Key Laboratory of Applied Organic Chemistry, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000 ; _publ_contact_author_email liuws@lzu.edu.cn _publ_contact_author_phone +86-931-8915151 loop_ _publ_author_name 'Xiong Hu.' 'Wei Dou.' 'Chan Xu.' 'Xiaoliang Tang.' 'Jiangrong Zheng.' ; Weisheng Liu ; data_Ce #TrackingRef '- SI-cif.txt' _database_code_depnum_ccdc_archive 'CCDC 793767' #TrackingRef '- Ce.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H74 Ce N3 O22 P4' _chemical_formula_weight 1213.03 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' Ce Ce -0.2486 2.6331 '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' H H 0.0000 0.0000 '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 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 19.7328(4) _cell_length_b 11.6301(2) _cell_length_c 23.7320(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.481(2) _cell_angle_gamma 90.00 _cell_volume 5444.54(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6828 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 29.23 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2516 _exptl_absorpt_coefficient_mu 1.032 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.814 _exptl_absorpt_correction_T_max 0.839 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14760 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5323 _reflns_number_gt 4467 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for O10 The larger than normal range of thermal motion is mostly due to the difference between the disordered group and the Ce atom which is not disordered. PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for Ce1 The middle Ce atom naturally has less thermal motion than the surrounding O atoms. PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O23 ...H's of the water molecule could not be located PLAT430_ALERT_2_A Short Inter D...A Contact O10 .. O23 .. 2.17 Ang. PLAT430_ALERT_2_A Short Inter D...A Contact O11 .. O23 .. 2.05 Ang. PLAT430_ALERT_2_A Short Inter D...A Contact O11 .. O23 .. 2.05 Ang. Short contacts between disordered solvent fragments are to be expected. ; _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^)+(0.0836P)^2^+16.8918P] 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 5323 _refine_ls_number_parameters 338 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1460 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.5000 0.25684(3) -0.2500 0.04615(15) Uani 1 2 d SD . . C1 C 0.5158(2) 0.1685(3) -0.00417(16) 0.0398(8) Uani 1 1 d . . . C2 C 0.4684(2) 0.1369(3) 0.03520(18) 0.0438(9) Uani 1 1 d . . . C3 C 0.4877(2) 0.1247(4) 0.09195(18) 0.0461(10) Uani 1 1 d . . . C4 C 0.5546(2) 0.1465(4) 0.10912(17) 0.0491(10) Uani 1 1 d . . . C5 C 0.6025(2) 0.1793(4) 0.06999(19) 0.0527(11) Uani 1 1 d . . . C6 C 0.5835(2) 0.1884(4) 0.01240(18) 0.0455(9) Uani 1 1 d . . . C7 C 0.4956(2) 0.1779(4) -0.06640(17) 0.0435(9) Uani 1 1 d . A . H7A H 0.4572 0.1273 -0.0735 0.052 Uiso 1 1 calc R . . H7B H 0.5329 0.1491 -0.0882 0.052 Uiso 1 1 calc R . . C8 C 0.3946(2) 0.1179(5) 0.0172(2) 0.0637(13) Uani 1 1 d . . . H8A H 0.3922 0.0963 -0.0219 0.095 Uiso 1 1 calc R . . H8B H 0.3696 0.1877 0.0224 0.095 Uiso 1 1 calc R . . H8C H 0.3757 0.0579 0.0396 0.095 Uiso 1 1 calc R . . C9 C 0.4362(3) 0.0913(5) 0.1351(2) 0.0691(15) Uani 1 1 d . . . H9A H 0.4063 0.1546 0.1417 0.083 Uiso 1 1 d R . . H9B H 0.4598 0.0713 0.1696 0.083 Uiso 1 1 d R . . H9C H 0.4104 0.0264 0.1217 0.083 Uiso 1 1 d R . . C10 C 0.5758(3) 0.1366(4) 0.17104(19) 0.0646(14) Uani 1 1 d . . . H10A H 0.5378 0.1596 0.1936 0.078 Uiso 1 1 calc R . . H10B H 0.6123 0.1907 0.1786 0.078 Uiso 1 1 calc R . . C11 C 0.6747(3) 0.2052(7) 0.0879(3) 0.094(2) Uani 1 1 d . . . H11A H 0.7043 0.1487 0.0723 0.141 Uiso 1 1 calc R . . H11B H 0.6789 0.2033 0.1283 0.141 Uiso 1 1 calc R . . H11C H 0.6870 0.2801 0.0746 0.141 Uiso 1 1 calc R . . C12 C 0.6369(3) 0.2169(6) -0.0292(2) 0.0661(14) Uani 1 1 d . . . H12A H 0.6513 0.2951 -0.0239 0.099 Uiso 1 1 calc R . . H12B H 0.6186 0.2076 -0.0668 0.099 Uiso 1 1 calc R . . H12C H 0.6750 0.1664 -0.0236 0.099 Uiso 1 1 calc R . . C13 C 0.5724(4) 0.4758(6) -0.1007(3) 0.0868(18) Uani 1 1 d . . . H13A H 0.6184 0.4675 -0.0859 0.104 Uiso 1 1 calc R . . H13B H 0.5713 0.4499 -0.1395 0.104 Uiso 1 1 calc R . . C14 C 0.5537(6) 0.5893(7) -0.0986(4) 0.129(3) Uani 1 1 d . . . H14A H 0.5064 0.5962 -0.1086 0.194 Uiso 1 1 calc R . . H14B H 0.5799 0.6327 -0.1246 0.194 Uiso 1 1 calc R . . H14C H 0.5616 0.6182 -0.0611 0.194 Uiso 1 1 calc R . . C15 C 0.3740(3) 0.4581(6) -0.0682(3) 0.0818(18) Uani 1 1 d . . . H15A H 0.3696 0.4779 -0.1078 0.098 Uiso 1 1 calc R . . H15B H 0.4008 0.5171 -0.0492 0.098 Uiso 1 1 calc R . . C16 C 0.3062(3) 0.4502(7) -0.0432(3) 0.099(2) Uani 1 1 d . . . H16A H 0.2818 0.3866 -0.0596 0.148 Uiso 1 1 calc R . . H16B H 0.2816 0.5201 -0.0504 0.148 Uiso 1 1 calc R . . H16C H 0.3112 0.4388 -0.0032 0.148 Uiso 1 1 calc R . . C17 C 0.6935(3) -0.1429(6) 0.1498(3) 0.0794(17) Uani 1 1 d . . . H17A H 0.7099 -0.1558 0.1882 0.095 Uiso 1 1 calc R . . H17B H 0.6655 -0.2078 0.1385 0.095 Uiso 1 1 calc R . . C18 C 0.7500(5) -0.1330(10) 0.1131(5) 0.149(4) Uani 1 1 d . . . H18A H 0.7346 -0.1445 0.0748 0.223 Uiso 1 1 calc R . . H18B H 0.7833 -0.1901 0.1231 0.223 Uiso 1 1 calc R . . H18C H 0.7696 -0.0578 0.1169 0.223 Uiso 1 1 calc R . . C19 C 0.7446(4) 0.0467(10) 0.3045(4) 0.141(4) Uani 1 1 d . . . H19A H 0.7596 -0.0311 0.2997 0.169 Uiso 1 1 d R . . H19B H 0.7170 0.0515 0.3371 0.169 Uiso 1 1 d R . . H19C H 0.7833 0.0962 0.3094 0.169 Uiso 1 1 d R . . C20 C 0.7064(4) 0.0801(7) 0.2558(3) 0.099(2) Uani 1 1 d . . . H20A H 0.7334 0.0696 0.2226 0.119 Uiso 1 1 calc R . . H20B H 0.6947 0.1609 0.2584 0.119 Uiso 1 1 calc R . . N1 N 0.6424(3) 0.2424(5) -0.1974(2) 0.0762(16) Uani 1 1 d . . . N2 N 0.5000 0.51460(18) -0.2500 0.219(3) Uani 1 2 d SDU . . O1 O 0.46594(18) 0.3241(3) -0.15457(11) 0.0551(8) Uani 1 1 d . A . O2 O 0.52636(19) 0.4042(3) -0.06740(14) 0.0623(9) Uani 1 1 d . A . O3 O 0.40676(18) 0.3460(3) -0.06146(13) 0.0594(8) Uani 1 1 d . A . O4 O 0.54901(16) -0.0859(3) 0.20271(12) 0.0510(7) Uani 1 1 d . . . O5 O 0.65367(19) -0.0379(3) 0.14713(13) 0.0651(9) Uani 1 1 d . . . O6 O 0.64492(18) 0.0121(3) 0.25029(13) 0.0635(9) Uani 1 1 d . . . O7 O 0.59133(17) 0.2024(4) -0.17441(14) 0.0621(9) Uani 1 1 d . A . O9 O 0.6976(3) 0.2416(6) -0.1744(3) 0.122(2) Uani 1 1 d . A . O10 O 0.4526(5) 0.4602(3) -0.2599(5) 0.219(3) Uani 1 1 d DU A . O11 O 0.5000 0.6324(11) -0.2500 0.221(3) Uani 1 2 d SDU A . O8A O 0.624(3) 0.304(6) -0.241(2) 0.084(13) Uani 0.41(14) 1 d P A 1 O8B O 0.638(2) 0.269(5) -0.2487(10) 0.110(9) Uani 0.59(14) 1 d P A 2 P1 P 0.47372(6) 0.31716(9) -0.09240(4) 0.0430(3) Uani 1 1 d . . . P2 P 0.60321(6) -0.00292(11) 0.19386(4) 0.0491(3) Uani 1 1 d . . . O23 O 0.8967(12) 0.881(2) 0.2511(11) 0.479(16) 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 Ce1 0.0754(3) 0.0410(2) 0.02218(18) 0.000 0.00543(15) 0.000 C1 0.053(2) 0.038(2) 0.0294(18) 0.0022(15) 0.0007(16) 0.0000(17) C2 0.050(2) 0.037(2) 0.044(2) 0.0053(17) 0.0026(18) -0.0033(17) C3 0.063(3) 0.038(2) 0.038(2) 0.0071(17) 0.0097(19) 0.0012(19) C4 0.075(3) 0.040(2) 0.032(2) 0.0071(17) -0.0041(19) -0.008(2) C5 0.063(3) 0.052(3) 0.042(2) 0.0139(19) -0.009(2) -0.014(2) C6 0.049(2) 0.047(2) 0.040(2) 0.0116(18) 0.0011(18) -0.0033(19) C7 0.053(2) 0.045(2) 0.033(2) -0.0027(17) 0.0002(17) 0.0017(18) C8 0.051(3) 0.074(3) 0.067(3) 0.018(3) 0.001(2) -0.009(2) C9 0.083(4) 0.068(3) 0.057(3) 0.020(3) 0.025(3) 0.010(3) C10 0.111(4) 0.049(3) 0.034(2) 0.0053(19) -0.008(2) -0.012(3) C11 0.080(4) 0.120(5) 0.079(4) 0.052(4) -0.036(3) -0.052(4) C12 0.055(3) 0.087(4) 0.056(3) 0.023(3) 0.003(2) -0.010(3) C13 0.112(5) 0.070(4) 0.079(4) 0.004(3) 0.001(4) -0.019(4) C14 0.192(10) 0.072(5) 0.125(7) 0.001(5) 0.028(7) 0.002(6) C15 0.099(4) 0.075(4) 0.072(4) 0.006(3) 0.016(3) 0.034(3) C16 0.086(4) 0.111(6) 0.099(5) -0.013(4) 0.016(4) 0.030(4) C17 0.066(3) 0.096(5) 0.077(4) 0.008(3) 0.013(3) 0.001(3) C18 0.110(7) 0.182(11) 0.157(9) 0.010(8) 0.056(6) 0.017(7) C19 0.110(6) 0.221(12) 0.089(5) 0.028(6) -0.043(5) -0.069(7) C20 0.110(5) 0.123(6) 0.063(4) 0.014(4) -0.023(3) -0.053(5) N1 0.078(3) 0.106(4) 0.045(3) -0.023(2) 0.008(2) -0.038(3) N2 0.220(3) 0.219(3) 0.218(3) 0.000 0.0062(8) 0.000 O1 0.088(2) 0.0515(18) 0.0262(14) -0.0005(12) 0.0037(14) 0.0111(16) O2 0.083(2) 0.056(2) 0.0474(18) 0.0016(15) -0.0065(16) -0.0160(17) O3 0.076(2) 0.0577(19) 0.0454(18) 0.0041(15) 0.0132(15) 0.0167(17) O4 0.0607(18) 0.0498(17) 0.0423(16) 0.0092(13) -0.0030(13) -0.0060(14) O5 0.080(2) 0.078(2) 0.0377(17) 0.0097(16) 0.0072(16) -0.0063(19) O6 0.075(2) 0.084(2) 0.0317(15) 0.0091(15) -0.0103(14) -0.0258(19) O7 0.0560(19) 0.091(3) 0.0400(17) 0.0017(18) 0.0052(15) -0.0054(18) O9 0.068(3) 0.201(7) 0.095(4) -0.012(3) -0.011(3) -0.047(3) O10 0.220(3) 0.219(3) 0.218(3) 0.0006(7) 0.0065(8) 0.0003(6) O11 0.222(3) 0.219(3) 0.221(3) 0.000 0.0056(9) 0.000 O8A 0.096(16) 0.12(2) 0.040(13) 0.025(12) -0.006(10) -0.053(16) O8B 0.115(14) 0.164(19) 0.052(7) -0.027(12) 0.026(9) -0.082(13) P1 0.0614(7) 0.0422(6) 0.0255(5) -0.0013(4) 0.0013(4) 0.0031(5) P2 0.0678(7) 0.0530(7) 0.0262(5) 0.0062(4) -0.0040(5) -0.0108(5) O23 0.50(3) 0.42(3) 0.52(4) 0.27(3) 0.09(3) 0.01(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O4 2.491(3) 5_655 ? Ce1 O4 2.491(3) 6 ? Ce1 O8A 2.50(5) . ? Ce1 O8A 2.50(5) 2_654 ? Ce1 O1 2.504(3) . ? Ce1 O1 2.504(3) 2_654 ? Ce1 O10 2.5516(10) 2_654 ? Ce1 O10 2.5516(10) . ? Ce1 O7 2.588(3) . ? Ce1 O7 2.588(3) 2_654 ? Ce1 O8B 2.73(4) . ? Ce1 O8B 2.73(4) 2_654 ? C1 C2 1.389(6) . ? C1 C6 1.402(6) . ? C1 C7 1.524(5) . ? C2 C3 1.397(6) . ? C2 C8 1.522(6) . ? C3 C4 1.396(6) . ? C3 C9 1.511(6) . ? C4 C5 1.395(6) . ? C4 C10 1.522(6) . ? C5 C6 1.412(6) . ? C5 C11 1.508(7) . ? C6 C12 1.500(6) . ? C7 P1 1.783(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 P2 1.790(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.371(10) . ? C13 O2 1.476(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 O3 1.462(6) . ? C15 C16 1.481(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.436(10) . ? C17 O5 1.453(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.418(9) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 O6 1.451(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? N1 O9 1.206(7) . ? N1 O7 1.249(6) . ? N1 O8B 1.26(2) . ? N1 O8A 1.30(3) . ? N2 O10 1.149(10) 2_654 ? N2 O10 1.149(10) . ? N2 O11 1.370(13) . ? O1 P1 1.481(3) . ? O2 P1 1.557(3) . ? O3 P1 1.565(3) . ? O4 P2 1.460(3) . ? O4 Ce1 2.491(3) 5_655 ? O5 P2 1.563(4) . ? O6 P2 1.563(3) . ? 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 O4 Ce1 O4 74.08(15) 5_655 6 ? O4 Ce1 O8A 121.7(10) 5_655 . ? O4 Ce1 O8A 80(2) 6 . ? O4 Ce1 O8A 80(2) 5_655 2_654 ? O4 Ce1 O8A 121.7(10) 6 2_654 ? O8A Ce1 O8A 155(4) . 2_654 ? O4 Ce1 O1 74.06(11) 5_655 . ? O4 Ce1 O1 140.64(10) 6 . ? O8A Ce1 O1 98.0(18) . . ? O8A Ce1 O1 74.0(8) 2_654 . ? O4 Ce1 O1 140.64(10) 5_655 2_654 ? O4 Ce1 O1 74.06(11) 6 2_654 ? O8A Ce1 O1 74.0(8) . 2_654 ? O8A Ce1 O1 98.0(18) 2_654 2_654 ? O1 Ce1 O1 143.60(15) . 2_654 ? O4 Ce1 O10 147.6(3) 5_655 2_654 ? O4 Ce1 O10 129.4(2) 6 2_654 ? O8A Ce1 O10 55.6(19) . 2_654 ? O8A Ce1 O10 99.2(18) 2_654 2_654 ? O1 Ce1 O10 74.6(3) . 2_654 ? O1 Ce1 O10 71.8(3) 2_654 2_654 ? O4 Ce1 O10 129.4(2) 5_655 . ? O4 Ce1 O10 147.6(3) 6 . ? O8A Ce1 O10 99.2(18) . . ? O8A Ce1 O10 55.6(19) 2_654 . ? O1 Ce1 O10 71.8(3) . . ? O1 Ce1 O10 74.6(3) 2_654 . ? O10 Ce1 O10 44.1(4) 2_654 . ? O4 Ce1 O7 76.34(11) 5_655 . ? O4 Ce1 O7 81.11(11) 6 . ? O8A Ce1 O7 48.4(5) . . ? O8A Ce1 O7 140.5(14) 2_654 . ? O1 Ce1 O7 69.39(11) . . ? O1 Ce1 O7 120.32(11) 2_654 . ? O10 Ce1 O7 85.2(3) 2_654 . ? O10 Ce1 O7 122.5(3) . . ? O4 Ce1 O7 81.11(11) 5_655 2_654 ? O4 Ce1 O7 76.34(11) 6 2_654 ? O8A Ce1 O7 140.5(14) . 2_654 ? O8A Ce1 O7 48.4(5) 2_654 2_654 ? O1 Ce1 O7 120.32(11) . 2_654 ? O1 Ce1 O7 69.39(11) 2_654 2_654 ? O10 Ce1 O7 122.5(3) 2_654 2_654 ? O10 Ce1 O7 85.2(3) . 2_654 ? O7 Ce1 O7 151.67(19) . 2_654 ? O4 Ce1 O8B 115.8(11) 5_655 . ? O4 Ce1 O8B 69.3(12) 6 . ? O8A Ce1 O8B 10.6(15) . . ? O8A Ce1 O8B 164(3) 2_654 . ? O1 Ce1 O8B 105.4(7) . . ? O1 Ce1 O8B 72.7(5) 2_654 . ? O10 Ce1 O8B 65.7(13) 2_654 . ? O10 Ce1 O8B 108.5(13) . . ? O7 Ce1 O8B 47.7(6) . . ? O7 Ce1 O8B 134.2(7) 2_654 . ? O4 Ce1 O8B 69.3(12) 5_655 2_654 ? O4 Ce1 O8B 115.8(11) 6 2_654 ? O8A Ce1 O8B 164(3) . 2_654 ? O8A Ce1 O8B 10.6(15) 2_654 2_654 ? O1 Ce1 O8B 72.7(5) . 2_654 ? O1 Ce1 O8B 105.4(7) 2_654 2_654 ? O10 Ce1 O8B 108.5(13) 2_654 2_654 ? O10 Ce1 O8B 65.7(13) . 2_654 ? O7 Ce1 O8B 134.2(7) . 2_654 ? O7 Ce1 O8B 47.7(6) 2_654 2_654 ? O8B Ce1 O8B 174(3) . 2_654 ? C2 C1 C6 120.6(4) . . ? C2 C1 C7 120.5(4) . . ? C6 C1 C7 118.9(4) . . ? C1 C2 C3 120.3(4) . . ? C1 C2 C8 120.3(4) . . ? C3 C2 C8 119.4(4) . . ? C4 C3 C2 119.7(4) . . ? C4 C3 C9 119.7(4) . . ? C2 C3 C9 120.6(4) . . ? C5 C4 C3 120.5(4) . . ? C5 C4 C10 119.3(4) . . ? C3 C4 C10 120.2(4) . . ? C4 C5 C6 119.8(4) . . ? C4 C5 C11 121.2(4) . . ? C6 C5 C11 118.9(4) . . ? C1 C6 C5 119.1(4) . . ? C1 C6 C12 122.2(4) . . ? C5 C6 C12 118.7(4) . . ? C1 C7 P1 117.1(3) . . ? C1 C7 H7A 108.0 . . ? P1 C7 H7A 108.0 . . ? C1 C7 H7B 108.0 . . ? P1 C7 H7B 108.0 . . ? H7A C7 H7B 107.3 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C9 H9A 109.9 . . ? C3 C9 H9B 108.8 . . ? H9A C9 H9B 109.5 . . ? C3 C9 H9C 109.7 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 P2 115.7(3) . . ? C4 C10 H10A 108.3 . . ? P2 C10 H10A 108.3 . . ? C4 C10 H10B 108.3 . . ? P2 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? C5 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 O2 110.7(7) . . ? C14 C13 H13A 109.5 . . ? O2 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? O2 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? 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 . . ? O3 C15 C16 107.6(5) . . ? O3 C15 H15A 110.2 . . ? C16 C15 H15A 110.2 . . ? O3 C15 H15B 110.2 . . ? C16 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 O5 109.5(7) . . ? C18 C17 H17A 109.8 . . ? O5 C17 H17A 109.8 . . ? C18 C17 H17B 109.8 . . ? O5 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? 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 . . ? C20 C19 H19A 108.7 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.8 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C19 C20 O6 110.5(6) . . ? C19 C20 H20A 109.6 . . ? O6 C20 H20A 109.6 . . ? C19 C20 H20B 109.6 . . ? O6 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? O9 N1 O7 121.8(6) . . ? O9 N1 O8B 119(2) . . ? O7 N1 O8B 118.7(16) . . ? O9 N1 O8A 126.9(18) . . ? O7 N1 O8A 110(2) . . ? O8B N1 O8A 24(3) . . ? O10 N2 O10 113.1(3) 2_654 . ? O10 N2 O11 123.44(14) 2_654 . ? O10 N2 O11 123.44(14) . . ? O10 N2 Ce1 56.56(14) 2_654 . ? O10 N2 Ce1 56.56(14) . . ? O11 N2 Ce1 180.000(1) . . ? P1 O1 Ce1 149.34(19) . . ? C13 O2 P1 125.2(4) . . ? C15 O3 P1 121.1(3) . . ? P2 O4 Ce1 152.50(18) . 5_655 ? C17 O5 P2 122.8(3) . . ? C20 O6 P2 123.9(3) . . ? N1 O7 Ce1 99.3(3) . . ? N2 O10 Ce1 101.4(3) . . ? N1 O8A Ce1 102(2) . . ? N1 O8B Ce1 92(2) . . ? O1 P1 O2 113.3(2) . . ? O1 P1 O3 112.87(19) . . ? O2 P1 O3 104.2(2) . . ? O1 P1 C7 114.34(19) . . ? O2 P1 C7 107.8(2) . . ? O3 P1 C7 103.44(19) . . ? O4 P2 O5 114.4(2) . . ? O4 P2 O6 108.80(18) . . ? O5 P2 O6 107.8(2) . . ? O4 P2 C10 115.2(2) . . ? O5 P2 C10 102.4(2) . . ? O6 P2 C10 107.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.0(6) . . . . ? C7 C1 C2 C3 177.9(4) . . . . ? C6 C1 C2 C8 178.7(4) . . . . ? C7 C1 C2 C8 -3.4(6) . . . . ? C1 C2 C3 C4 1.3(6) . . . . ? C8 C2 C3 C4 -177.4(4) . . . . ? C1 C2 C3 C9 179.5(4) . . . . ? C8 C2 C3 C9 0.8(7) . . . . ? C2 C3 C4 C5 -0.7(7) . . . . ? C9 C3 C4 C5 -178.9(5) . . . . ? C2 C3 C4 C10 178.3(4) . . . . ? C9 C3 C4 C10 0.1(7) . . . . ? C3 C4 C5 C6 -1.2(7) . . . . ? C10 C4 C5 C6 179.8(4) . . . . ? C3 C4 C5 C11 178.9(5) . . . . ? C10 C4 C5 C11 -0.1(8) . . . . ? C2 C1 C6 C5 -1.9(7) . . . . ? C7 C1 C6 C5 -179.8(4) . . . . ? C2 C1 C6 C12 177.0(5) . . . . ? C7 C1 C6 C12 -0.9(7) . . . . ? C4 C5 C6 C1 2.5(7) . . . . ? C11 C5 C6 C1 -177.7(5) . . . . ? C4 C5 C6 C12 -176.4(5) . . . . ? C11 C5 C6 C12 3.4(8) . . . . ? C2 C1 C7 P1 96.0(4) . . . . ? C6 C1 C7 P1 -86.1(4) . . . . ? C5 C4 C10 P2 -92.3(5) . . . . ? C3 C4 C10 P2 88.6(5) . . . . ? O4 Ce1 N2 O10 117.5(7) 5_655 . . 2_654 ? O4 Ce1 N2 O10 -62.5(7) 6 . . 2_654 ? O8A Ce1 N2 O10 -9.2(15) . . . 2_654 ? O8A Ce1 N2 O10 170.8(15) 2_654 . . 2_654 ? O1 Ce1 N2 O10 93.7(7) . . . 2_654 ? O1 Ce1 N2 O10 -86.3(7) 2_654 . . 2_654 ? O10 Ce1 N2 O10 180.0 . . . 2_654 ? O7 Ce1 N2 O10 31.5(7) . . . 2_654 ? O7 Ce1 N2 O10 -148.5(7) 2_654 . . 2_654 ? O8B Ce1 N2 O10 -13.5(8) . . . 2_654 ? O8B Ce1 N2 O10 166.5(8) 2_654 . . 2_654 ? O4 Ce1 N2 O10 -62.5(7) 5_655 . . . ? O4 Ce1 N2 O10 117.5(7) 6 . . . ? O8A Ce1 N2 O10 170.8(15) . . . . ? O8A Ce1 N2 O10 -9.2(15) 2_654 . . . ? O1 Ce1 N2 O10 -86.3(7) . . . . ? O1 Ce1 N2 O10 93.7(7) 2_654 . . . ? O10 Ce1 N2 O10 180.0 2_654 . . . ? O7 Ce1 N2 O10 -148.5(7) . . . . ? O7 Ce1 N2 O10 31.5(7) 2_654 . . . ? O8B Ce1 N2 O10 166.5(8) . . . . ? O8B Ce1 N2 O10 -13.5(8) 2_654 . . . ? O4 Ce1 N2 O11 0(100) 5_655 . . . ? O4 Ce1 N2 O11 0(100) 6 . . . ? O8A Ce1 N2 O11 0(100) . . . . ? O8A Ce1 N2 O11 0(100) 2_654 . . . ? O1 Ce1 N2 O11 0(100) . . . . ? O1 Ce1 N2 O11 0(100) 2_654 . . . ? O10 Ce1 N2 O11 0(100) 2_654 . . . ? O10 Ce1 N2 O11 0(100) . . . . ? O7 Ce1 N2 O11 0(100) . . . . ? O7 Ce1 N2 O11 0(100) 2_654 . . . ? O8B Ce1 N2 O11 0(100) . . . . ? O8B Ce1 N2 O11 0(100) 2_654 . . . ? O4 Ce1 O1 P1 62.8(4) 5_655 . . . ? O4 Ce1 O1 P1 25.7(5) 6 . . . ? O8A Ce1 O1 P1 -58.0(14) . . . . ? O8A Ce1 O1 P1 147(2) 2_654 . . . ? O1 Ce1 O1 P1 -131.8(4) 2_654 . . . ? O10 Ce1 O1 P1 -108.9(5) 2_654 . . . ? O10 Ce1 O1 P1 -155.1(5) . . . . ? O7 Ce1 O1 P1 -18.3(4) . . . . ? O7 Ce1 O1 P1 132.1(4) 2_654 . . . ? O8B Ce1 O1 P1 -50.2(13) . . . . ? O8B Ce1 O1 P1 135.5(14) 2_654 . . . ? C14 C13 O2 P1 109.7(7) . . . . ? C16 C15 O3 P1 169.1(4) . . . . ? C18 C17 O5 P2 -160.5(6) . . . . ? C19 C20 O6 P2 -159.8(6) . . . . ? O9 N1 O7 Ce1 175.6(5) . . . . ? O8B N1 O7 Ce1 -15(3) . . . . ? O8A N1 O7 Ce1 10(4) . . . . ? O4 Ce1 O7 N1 153.7(3) 5_655 . . . ? O4 Ce1 O7 N1 78.0(3) 6 . . . ? O8A Ce1 O7 N1 -6(3) . . . . ? O8A Ce1 O7 N1 -152(3) 2_654 . . . ? O1 Ce1 O7 N1 -128.5(3) . . . . ? O1 Ce1 O7 N1 12.5(4) 2_654 . . . ? O10 Ce1 O7 N1 -53.2(4) 2_654 . . . ? O10 Ce1 O7 N1 -77.9(4) . . . . ? O7 Ce1 O7 N1 115.5(3) 2_654 . . . ? O8B Ce1 O7 N1 8.0(17) . . . . ? O8B Ce1 O7 N1 -164.4(17) 2_654 . . . ? O10 N2 O10 Ce1 0.0 2_654 . . . ? O11 N2 O10 Ce1 180.0 . . . . ? O4 Ce1 O10 N2 136.2(5) 5_655 . . . ? O4 Ce1 O10 N2 -94.6(7) 6 . . . ? O8A Ce1 O10 N2 -9.1(15) . . . . ? O8A Ce1 O10 N2 169.1(16) 2_654 . . . ? O1 Ce1 O10 N2 86.4(6) . . . . ? O1 Ce1 O10 N2 -79.6(6) 2_654 . . . ? O10 Ce1 O10 N2 0.0 2_654 . . . ? O7 Ce1 O10 N2 36.9(8) . . . . ? O7 Ce1 O10 N2 -149.5(7) 2_654 . . . ? O8B Ce1 O10 N2 -14.2(9) . . . . ? O8B Ce1 O10 N2 165.2(9) 2_654 . . . ? O9 N1 O8A Ce1 -175.1(6) . . . . ? O7 N1 O8A Ce1 -10(4) . . . . ? O8B N1 O8A Ce1 107(8) . . . . ? O4 Ce1 O8A N1 -17(6) 5_655 . . . ? O4 Ce1 O8A N1 -81(5) 6 . . . ? O8A Ce1 O8A N1 128(5) 2_654 . . . ? O1 Ce1 O8A N1 59(5) . . . . ? O1 Ce1 O8A N1 -157(5) 2_654 . . . ? O10 Ce1 O8A N1 124(5) 2_654 . . . ? O10 Ce1 O8A N1 132(4) . . . . ? O7 Ce1 O8A N1 6(3) . . . . ? O7 Ce1 O8A N1 -135(3) 2_654 . . . ? O8B Ce1 O8A N1 -76(6) . . . . ? O8B Ce1 O8A N1 113(5) 2_654 . . . ? O9 N1 O8B Ce1 -176.2(6) . . . . ? O7 N1 O8B Ce1 14(3) . . . . ? O8A N1 O8B Ce1 -59(7) . . . . ? O4 Ce1 O8B N1 -45(3) 5_655 . . . ? O4 Ce1 O8B N1 -105(3) 6 . . . ? O8A Ce1 O8B N1 81(5) . . . . ? O8A Ce1 O8B N1 120(5) 2_654 . . . ? O1 Ce1 O8B N1 34(3) . . . . ? O1 Ce1 O8B N1 176(3) 2_654 . . . ? O10 Ce1 O8B N1 99(3) 2_654 . . . ? O10 Ce1 O8B N1 110(3) . . . . ? O7 Ce1 O8B N1 -7.9(17) . . . . ? O7 Ce1 O8B N1 -148.7(17) 2_654 . . . ? O8B Ce1 O8B N1 104(3) 2_654 . . . ? Ce1 O1 P1 O2 91.9(4) . . . . ? Ce1 O1 P1 O3 -150.0(4) . . . . ? Ce1 O1 P1 C7 -32.1(5) . . . . ? C13 O2 P1 O1 -8.8(5) . . . . ? C13 O2 P1 O3 -131.8(5) . . . . ? C13 O2 P1 C7 118.8(5) . . . . ? C15 O3 P1 O1 -60.2(5) . . . . ? C15 O3 P1 O2 63.1(4) . . . . ? C15 O3 P1 C7 175.7(4) . . . . ? C1 C7 P1 O1 170.2(3) . . . . ? C1 C7 P1 O2 43.2(4) . . . . ? C1 C7 P1 O3 -66.7(4) . . . . ? Ce1 O4 P2 O5 91.1(4) 5_655 . . . ? Ce1 O4 P2 O6 -29.5(5) 5_655 . . . ? Ce1 O4 P2 C10 -150.7(4) 5_655 . . . ? C17 O5 P2 O4 -59.6(5) . . . . ? C17 O5 P2 O6 61.5(5) . . . . ? C17 O5 P2 C10 175.1(4) . . . . ? C20 O6 P2 O4 174.2(5) . . . . ? C20 O6 P2 O5 49.6(6) . . . . ? C20 O6 P2 C10 -60.2(6) . . . . ? C4 C10 P2 O4 -77.2(5) . . . . ? C4 C10 P2 O5 47.5(5) . . . . ? C4 C10 P2 O6 161.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.585 _refine_diff_density_min -1.650 _refine_diff_density_rms 0.100 data_Dy #TrackingRef '- SI-cif.txt' _database_code_depnum_ccdc_archive 'CCDC 793768' #TrackingRef '- Dy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H38 Dy N3 O16 P2 ' _chemical_formula_sum 'C20 H38 Dy N3 O16 P2 ' _chemical_formula_weight 800.97 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.858(6) _cell_length_b 23.474(16) _cell_length_c 18.026(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.880(8) _cell_angle_gamma 90.00 _cell_volume 3254(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1782 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 18.60 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612.0 _exptl_absorpt_coefficient_mu 2.465 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_T_max 0.611 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15844 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0926 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6022 _reflns_number_gt 3746 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.81 Ratio Some terminal C atoms in disordered side chains have high isotropic U-values. ; _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^)+(0.0331P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00058(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6022 _refine_ls_number_parameters 388 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0932 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1110 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.020 _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 0.27327(5) 0.569477(14) 0.145648(18) 0.04625(15) Uani 1 1 d . . . C1 C 0.0219(9) 0.6198(3) 0.4053(4) 0.0494(19) Uani 1 1 d . . . C2 C -0.0347(9) 0.6664(3) 0.3585(4) 0.0482(18) Uani 1 1 d . . . C3 C -0.0254(10) 0.7212(3) 0.3891(4) 0.054(2) Uani 1 1 d . . . C4 C 0.0463(10) 0.7297(3) 0.4652(4) 0.0502(19) Uani 1 1 d . . . C5 C 0.1032(10) 0.6826(3) 0.5124(4) 0.0508(19) Uani 1 1 d . . . C6 C 0.0894(10) 0.6284(3) 0.4824(4) 0.0514(19) Uani 1 1 d . . . C7 C 0.0101(10) 0.5604(3) 0.3724(4) 0.059(2) Uani 1 1 d . . . H7A H -0.0907 0.5584 0.3311 0.070 Uiso 1 1 calc R . . H7B H -0.0082 0.5337 0.4111 0.070 Uiso 1 1 calc R . . C8 C -0.1127(10) 0.6589(3) 0.2753(4) 0.068(2) Uani 1 1 d . . . H8A H -0.2366 0.6636 0.2670 0.103 Uiso 1 1 calc R . . H8B H -0.0864 0.6215 0.2596 0.103 Uiso 1 1 calc R . . H8C H -0.0650 0.6869 0.2465 0.103 Uiso 1 1 calc R . . C9 C -0.0913(12) 0.7702(3) 0.3382(5) 0.086(3) Uani 1 1 d . . . H9A H -0.1866 0.7578 0.2993 0.129 Uiso 1 1 calc R . . H9B H 0.0003 0.7844 0.3154 0.129 Uiso 1 1 calc R . . H9C H -0.1301 0.8000 0.3673 0.129 Uiso 1 1 calc R . . C10 C 0.0661(9) 0.7891(3) 0.4989(4) 0.0523(19) Uani 1 1 d . . . H10A H 0.0546 0.7863 0.5513 0.063 Uiso 1 1 calc R . . H10B H -0.0305 0.8119 0.4725 0.063 Uiso 1 1 calc R . . C11 C 0.1746(11) 0.6906(3) 0.5965(4) 0.071(2) Uani 1 1 d . . . H11A H 0.1308 0.6611 0.6243 0.106 Uiso 1 1 calc R . . H11B H 0.1390 0.7271 0.6121 0.106 Uiso 1 1 calc R . . H11C H 0.2993 0.6888 0.6064 0.106 Uiso 1 1 calc R . . C12 C 0.1464(13) 0.5779(3) 0.5341(5) 0.083(3) Uani 1 1 d . . . H12A H 0.2524 0.5872 0.5690 0.125 Uiso 1 1 calc R . . H12B H 0.1652 0.5456 0.5043 0.125 Uiso 1 1 calc R . . H12C H 0.0576 0.5691 0.5618 0.125 Uiso 1 1 calc R . . C13 C 0.4742(18) 0.6011(7) 0.3897(6) 0.161(6) Uani 1 1 d DU . . H13A H 0.5472 0.5889 0.3553 0.193 Uiso 1 1 calc R . . H13B H 0.4025 0.6320 0.3651 0.193 Uiso 1 1 calc R . . C14 C 0.578(2) 0.6223(9) 0.4515(8) 0.279(11) Uani 1 1 d DU . . H14A H 0.5141 0.6270 0.4909 0.419 Uiso 1 1 calc R . . H14B H 0.6226 0.6586 0.4396 0.419 Uiso 1 1 calc R . . H14C H 0.6737 0.5966 0.4683 0.419 Uiso 1 1 calc R . . C15 C 0.3137(14) 0.4352(4) 0.3275(6) 0.093(3) Uani 1 1 d U . . H15A H 0.3521 0.4490 0.2830 0.111 Uiso 1 1 calc R . . H15B H 0.4132 0.4352 0.3695 0.111 Uiso 1 1 calc R . . C16 C 0.2520(17) 0.3794(5) 0.3144(9) 0.176(6) Uani 1 1 d U . . H16A H 0.2370 0.3628 0.3612 0.264 Uiso 1 1 calc R . . H16B H 0.3342 0.3573 0.2939 0.264 Uiso 1 1 calc R . . H16C H 0.1425 0.3799 0.2790 0.264 Uiso 1 1 calc R . . C17 C 0.5875(13) 0.7002(5) 0.0443(7) 0.108(4) Uani 1 1 d U . . H17A H 0.6048 0.6622 0.0658 0.129 Uiso 1 1 calc R . . H17B H 0.6237 0.7000 -0.0040 0.129 Uiso 1 1 calc R . . C18 C 0.6904(14) 0.7402(5) 0.0943(7) 0.141(5) Uani 1 1 d U . . H18A H 0.7013 0.7748 0.0673 0.212 Uiso 1 1 calc R . . H18B H 0.8037 0.7245 0.1133 0.212 Uiso 1 1 calc R . . H18C H 0.6350 0.7483 0.1359 0.212 Uiso 1 1 calc R . . C19 C 0.2921(17) 0.6157(4) -0.1241(5) 0.128(5) Uani 1 1 d U . . H19A H 0.1794 0.5971 -0.1354 0.154 Uiso 1 1 calc R . . H19B H 0.3730 0.5903 -0.0921 0.154 Uiso 1 1 calc R . . C20 C 0.3493(18) 0.6256(5) -0.1921(6) 0.162(6) Uani 1 1 d U . . H20A H 0.2943 0.6593 -0.2161 0.243 Uiso 1 1 calc R . . H20B H 0.3193 0.5936 -0.2254 0.243 Uiso 1 1 calc R . . H20C H 0.4732 0.6307 -0.1812 0.243 Uiso 1 1 calc R . . N1 N 0.1945(9) 0.4580(3) 0.0808(4) 0.069(2) Uani 1 1 d . . . N2 N 0.6281(10) 0.5301(3) 0.1817(4) 0.0574(17) Uani 1 1 d . . . N3 N 0.3462(12) 0.6799(3) 0.2099(4) 0.075(2) Uani 1 1 d . . . O1 O 0.2029(6) 0.55958(19) 0.2618(3) 0.0547(13) Uani 1 1 d . . . O2 O 0.3621(8) 0.5552(3) 0.3975(3) 0.0785(17) Uani 1 1 d . . . O3 O 0.1841(8) 0.4729(2) 0.3445(3) 0.0797(18) Uani 1 1 d . . . O4 O 0.2668(6) 0.61857(19) 0.0370(2) 0.0549(13) Uani 1 1 d . . . O5 O 0.4054(7) 0.7154(2) 0.0329(3) 0.0727(16) Uani 1 1 d . . . O6 O 0.2791(8) 0.6667(2) -0.0850(3) 0.0784(18) Uani 1 1 d . . . O7 O -0.0267(6) 0.5728(2) 0.1043(3) 0.0710(16) Uani 1 1 d D . . H1O7 H -0.0885 0.5515 0.1303 0.106 Uiso 1 1 d RD . . H2O7 H -0.0678 0.5639 0.0625 0.106 Uiso 1 1 d RD . . O8 O 0.2020(9) 0.4678(2) 0.1502(3) 0.095(2) Uani 1 1 d . . . O9 O 0.2224(7) 0.4985(2) 0.0418(3) 0.0701(16) Uani 1 1 d . . . O10 O 0.1548(9) 0.4112(2) 0.0533(4) 0.098(2) Uani 1 1 d . . . O11 O 0.5283(7) 0.5226(2) 0.2260(3) 0.0739(17) Uani 1 1 d . . . O12 O 0.5638(7) 0.5514(2) 0.1192(3) 0.0712(16) Uani 1 1 d . . . O13 O 0.7827(7) 0.5165(2) 0.1986(3) 0.0735(17) Uani 1 1 d . . . O14 O 0.1955(8) 0.6676(2) 0.1773(3) 0.0654(15) Uani 1 1 d . . . O15 O 0.4620(8) 0.6421(3) 0.2087(3) 0.0759(17) Uani 1 1 d . . . O16 O 0.3830(10) 0.7254(3) 0.2408(4) 0.119(3) Uani 1 1 d . . . P2 P 0.2584(3) 0.67354(8) -0.00295(11) 0.0529(5) Uani 1 1 d . . . P1 P 0.1958(3) 0.53863(9) 0.33809(11) 0.0563(6) 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 Dy1 0.0501(3) 0.0426(2) 0.0459(2) 0.00235(17) 0.00931(16) -0.00402(19) C1 0.047(5) 0.046(5) 0.061(5) -0.002(4) 0.023(4) -0.004(4) C2 0.051(5) 0.042(5) 0.052(4) -0.007(4) 0.011(4) -0.004(4) C3 0.056(5) 0.052(5) 0.053(5) -0.002(4) 0.007(4) 0.003(4) C4 0.059(5) 0.034(4) 0.058(5) 0.001(3) 0.012(4) -0.004(4) C5 0.064(6) 0.043(5) 0.049(4) -0.005(4) 0.021(4) -0.003(4) C6 0.072(6) 0.042(5) 0.046(4) 0.006(3) 0.027(4) 0.005(4) C7 0.078(6) 0.049(5) 0.054(4) -0.004(4) 0.027(4) -0.011(4) C8 0.065(6) 0.078(6) 0.052(5) -0.003(4) -0.011(4) -0.002(5) C9 0.100(8) 0.067(6) 0.078(6) 0.015(5) -0.011(5) 0.001(5) C10 0.061(5) 0.036(4) 0.059(4) -0.005(3) 0.011(4) 0.006(4) C11 0.098(7) 0.056(5) 0.058(5) -0.006(4) 0.018(5) -0.007(5) C12 0.122(9) 0.060(6) 0.070(6) 0.011(5) 0.023(6) 0.002(5) C13 0.161(13) 0.234(15) 0.086(8) -0.019(9) 0.024(8) -0.115(12) C14 0.24(2) 0.44(3) 0.158(14) -0.068(17) 0.047(13) -0.22(2) C15 0.120(9) 0.067(7) 0.094(7) 0.015(5) 0.029(7) 0.014(6) C16 0.202(15) 0.060(9) 0.292(18) -0.014(10) 0.112(14) -0.004(9) C17 0.074(8) 0.100(9) 0.157(11) -0.019(8) 0.042(8) -0.003(7) C18 0.098(10) 0.145(12) 0.181(13) -0.021(10) 0.030(9) -0.041(9) C19 0.256(15) 0.064(7) 0.081(7) 0.004(5) 0.073(8) 0.022(8) C20 0.299(18) 0.097(10) 0.126(10) 0.001(7) 0.131(11) 0.030(10) N1 0.072(5) 0.052(5) 0.073(5) -0.002(4) -0.011(4) -0.005(4) N2 0.055(5) 0.054(4) 0.060(4) -0.008(3) 0.002(4) -0.004(4) N3 0.094(7) 0.052(5) 0.073(5) -0.005(4) 0.004(5) -0.014(5) O1 0.053(3) 0.058(3) 0.055(3) 0.006(2) 0.016(3) -0.003(2) O2 0.074(4) 0.100(5) 0.057(3) 0.008(3) 0.003(3) 0.005(4) O3 0.106(5) 0.050(4) 0.095(4) 0.007(3) 0.047(4) 0.013(3) O4 0.070(4) 0.043(3) 0.054(3) 0.009(2) 0.018(3) 0.000(3) O5 0.063(4) 0.050(3) 0.106(4) -0.008(3) 0.019(3) -0.004(3) O6 0.125(5) 0.060(4) 0.059(3) 0.013(3) 0.042(4) 0.021(3) O7 0.056(4) 0.094(4) 0.060(3) 0.001(3) 0.006(3) -0.009(3) O8 0.162(7) 0.052(4) 0.056(4) 0.002(3) -0.010(4) -0.027(4) O9 0.093(5) 0.052(4) 0.069(4) -0.007(3) 0.026(3) -0.013(3) O10 0.128(6) 0.044(4) 0.105(5) -0.010(3) -0.016(4) -0.025(4) O11 0.067(4) 0.081(4) 0.080(4) 0.020(3) 0.029(3) 0.010(3) O12 0.060(4) 0.098(5) 0.057(3) 0.006(3) 0.018(3) 0.007(3) O13 0.046(4) 0.070(4) 0.101(5) -0.007(3) 0.008(3) 0.003(3) O14 0.074(4) 0.058(4) 0.065(4) -0.001(3) 0.017(3) 0.002(3) O15 0.059(4) 0.062(4) 0.098(4) -0.005(3) -0.004(3) -0.015(3) O16 0.162(7) 0.062(5) 0.115(6) -0.026(4) -0.011(5) -0.011(4) P2 0.0653(15) 0.0427(12) 0.0539(12) 0.0047(9) 0.0195(11) -0.0002(10) P1 0.0736(17) 0.0466(13) 0.0507(12) 0.0010(9) 0.0179(12) 0.0002(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O4 2.263(4) . ? Dy1 O1 2.284(5) . ? Dy1 O7 2.323(5) . ? Dy1 O15 2.388(5) . ? Dy1 O8 2.457(6) . ? Dy1 O12 2.463(5) . ? Dy1 O11 2.476(5) . ? Dy1 O9 2.477(5) . ? Dy1 O14 2.480(5) . ? C1 C6 1.396(9) . ? C1 C2 1.398(9) . ? C1 C7 1.511(9) . ? C2 C3 1.394(9) . ? C2 C8 1.508(9) . ? C3 C4 1.386(9) . ? C3 C9 1.497(10) . ? C4 C5 1.410(9) . ? C4 C10 1.517(9) . ? C5 C6 1.379(9) . ? C5 C11 1.516(9) . ? C6 C12 1.516(10) . ? C7 P1 1.773(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 P2 1.753(7) 4_576 ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.336(12) . ? C13 O2 1.416(12) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.398(12) . ? C15 O3 1.430(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.432(12) . ? C17 O5 1.449(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O6 1.404(10) . ? C19 C20 1.410(12) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? N1 O10 1.219(8) . ? N1 O9 1.229(8) . ? N1 O8 1.261(8) . ? N2 O13 1.232(7) . ? N2 O12 1.241(7) . ? N2 O11 1.241(7) . ? N3 O16 1.211(8) . ? N3 O14 1.243(8) . ? N3 O15 1.276(9) . ? O1 P1 1.473(5) . ? O2 P1 1.559(6) . ? O3 P1 1.551(6) . ? O4 P2 1.473(5) . ? O5 P2 1.553(6) . ? O6 P2 1.529(5) . ? O7 H1O7 0.8921 . ? O7 H2O7 0.7851 . ? P2 C10 1.753(7) 4_575 ? 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 O4 Dy1 O1 151.39(17) . . ? O4 Dy1 O7 82.26(17) . . ? O1 Dy1 O7 82.87(18) . . ? O4 Dy1 O15 87.12(19) . . ? O1 Dy1 O15 83.11(19) . . ? O7 Dy1 O15 128.2(2) . . ? O4 Dy1 O8 123.98(18) . . ? O1 Dy1 O8 76.74(19) . . ? O7 Dy1 O8 79.6(2) . . ? O15 Dy1 O8 143.2(2) . . ? O4 Dy1 O12 77.10(18) . . ? O1 Dy1 O12 124.67(18) . . ? O7 Dy1 O12 149.72(19) . . ? O15 Dy1 O12 72.9(2) . . ? O8 Dy1 O12 93.8(2) . . ? O4 Dy1 O11 127.12(18) . . ? O1 Dy1 O11 74.84(18) . . ? O7 Dy1 O11 148.01(18) . . ? O15 Dy1 O11 72.0(2) . . ? O8 Dy1 O11 73.2(2) . . ? O12 Dy1 O11 50.64(18) . . ? O4 Dy1 O9 73.57(18) . . ? O1 Dy1 O9 126.34(18) . . ? O7 Dy1 O9 77.56(18) . . ? O15 Dy1 O9 145.9(2) . . ? O8 Dy1 O9 50.90(18) . . ? O12 Dy1 O9 75.51(18) . . ? O11 Dy1 O9 97.4(2) . . ? O4 Dy1 O14 76.29(17) . . ? O1 Dy1 O14 76.49(16) . . ? O7 Dy1 O14 76.17(19) . . ? O15 Dy1 O14 52.1(2) . . ? O8 Dy1 O14 145.7(2) . . ? O12 Dy1 O14 119.10(19) . . ? O11 Dy1 O14 119.1(2) . . ? O9 Dy1 O14 142.15(19) . . ? C6 C1 C2 119.8(7) . . ? C6 C1 C7 120.2(6) . . ? C2 C1 C7 120.0(7) . . ? C3 C2 C1 119.8(7) . . ? C3 C2 C8 118.6(7) . . ? C1 C2 C8 121.5(6) . . ? C4 C3 C2 120.2(7) . . ? C4 C3 C9 121.0(7) . . ? C2 C3 C9 118.8(7) . . ? C3 C4 C5 119.9(7) . . ? C3 C4 C10 121.1(6) . . ? C5 C4 C10 119.0(6) . . ? C6 C5 C4 119.8(7) . . ? C6 C5 C11 119.3(7) . . ? C4 C5 C11 120.8(6) . . ? C5 C6 C1 120.4(6) . . ? C5 C6 C12 119.4(7) . . ? C1 C6 C12 120.2(7) . . ? C1 C7 P1 114.5(5) . . ? C1 C7 H7A 108.6 . . ? P1 C7 H7A 108.6 . . ? C1 C7 H7B 108.6 . . ? P1 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C9 H9A 109.5 . . ? C3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 P2 118.0(5) . 4_576 ? C4 C10 H10A 107.8 . . ? P2 C10 H10A 107.8 4_576 . ? C4 C10 H10B 107.8 . . ? P2 C10 H10B 107.8 4_576 . ? H10A C10 H10B 107.1 . . ? C5 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 O2 119.3(12) . . ? C14 C13 H13A 107.5 . . ? O2 C13 H13A 107.5 . . ? C14 C13 H13B 107.5 . . ? O2 C13 H13B 107.5 . . ? H13A C13 H13B 107.0 . . ? 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 . . ? C16 C15 O3 112.3(9) . . ? C16 C15 H15A 109.2 . . ? O3 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? O3 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 O5 109.9(9) . . ? C18 C17 H17A 109.7 . . ? O5 C17 H17A 109.7 . . ? C18 C17 H17B 109.7 . . ? O5 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? 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 . . ? O6 C19 C20 111.4(9) . . ? O6 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? O6 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O10 N1 O9 121.6(8) . . ? O10 N1 O8 121.6(8) . . ? O9 N1 O8 116.7(7) . . ? O13 N2 O12 121.7(7) . . ? O13 N2 O11 121.7(7) . . ? O12 N2 O11 116.6(7) . . ? O16 N3 O14 122.5(9) . . ? O16 N3 O15 121.2(9) . . ? O14 N3 O15 116.3(7) . . ? P1 O1 Dy1 162.3(3) . . ? C13 O2 P1 124.9(7) . . ? C15 O3 P1 123.0(6) . . ? P2 O4 Dy1 149.3(3) . . ? C17 O5 P2 122.0(6) . . ? C19 O6 P2 127.5(5) . . ? Dy1 O7 H1O7 116.0 . . ? Dy1 O7 H2O7 119.2 . . ? H1O7 O7 H2O7 101.4 . . ? N1 O8 Dy1 96.2(5) . . ? N1 O9 Dy1 96.1(5) . . ? N2 O11 Dy1 95.9(5) . . ? N2 O12 Dy1 96.6(5) . . ? N3 O14 Dy1 93.9(5) . . ? N3 O15 Dy1 97.5(5) . . ? O4 P2 O6 112.2(3) . . ? O4 P2 O5 113.4(3) . . ? O6 P2 O5 104.6(3) . . ? O4 P2 C10 112.4(3) . 4_575 ? O6 P2 C10 109.6(3) . 4_575 ? O5 P2 C10 104.2(3) . 4_575 ? O1 P1 O3 114.6(3) . . ? O1 P1 O2 111.8(3) . . ? O3 P1 O2 104.5(3) . . ? O1 P1 C7 114.9(3) . . ? O3 P1 C7 101.2(3) . . ? O2 P1 C7 108.8(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.814 _refine_diff_density_min -0.884 _refine_diff_density_rms 0.115 data_Er #TrackingRef '- SI-cif.txt' _database_code_depnum_ccdc_archive 'CCDC 793769' #TrackingRef '- Er.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H58 Er N3 O20 P3' _chemical_formula_weight 1040.96 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5103(4) _cell_length_b 15.1444(5) _cell_length_c 17.5398(6) _cell_angle_alpha 90.346(2) _cell_angle_beta 93.762(2) _cell_angle_gamma 95.568(2) _cell_volume 3036.26(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6906 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.34 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.516 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.702 _exptl_absorpt_correction_T_max 0.727 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15941 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.30 _reflns_number_total 10824 _reflns_number_gt 9136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.22 Ratio PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for C19B PLAT234_ALERT_4_A Large Hirshfeld Difference C19B -- C20B .. 0.42 Ang. Some terminal C atoms in disordered side chains have high isotropic U-values. PLAT602_ALERT_2_A VERY LARGE Solvent Accessible VOID(S) in Structure ! These three alerts arise from the fact that the highly disordered solvent. ; _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^)+(0.0756P)^2^+4.1853P] 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 10824 _refine_ls_number_parameters 548 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1447 _refine_ls_wR_factor_gt 0.1367 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.100 _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 Er1 Er 0.33156(2) 0.552043(18) 0.334551(14) 0.04183(11) Uani 1 1 d . . . C1 C 0.0866(6) 0.3564(5) -0.0747(4) 0.0622(18) Uani 1 1 d . . . C2 C 0.1175(6) 0.3762(6) 0.0018(4) 0.0658(19) Uani 1 1 d . . . C3 C 0.1650(6) 0.4589(6) 0.0249(4) 0.0625(19) Uani 1 1 d . . . C4 C 0.1786(6) 0.5270(6) -0.0277(4) 0.0650(19) Uani 1 1 d . . . C5 C 0.1487(6) 0.5076(5) -0.1054(4) 0.0604(18) Uani 1 1 d . . . C6 C 0.1049(5) 0.4234(5) -0.1279(3) 0.0558(17) Uani 1 1 d . . . C7 C 0.0333(8) 0.2644(6) -0.0998(5) 0.087(3) Uani 1 1 d . . . H7A H 0.0500 0.2537 -0.1518 0.131 Uiso 1 1 calc R . . H7B H -0.0499 0.2604 -0.0960 0.131 Uiso 1 1 calc R . . H7C H 0.0660 0.2209 -0.0675 0.131 Uiso 1 1 calc R . . C8 C 0.1000(9) 0.3021(8) 0.0603(5) 0.109(4) Uani 1 1 d . . . H8A H 0.1648 0.2666 0.0610 0.163 Uiso 1 1 calc R . . H8B H 0.0288 0.2656 0.0465 0.163 Uiso 1 1 calc R . . H8C H 0.0957 0.3278 0.1101 0.163 Uiso 1 1 calc R . . C9 C 0.2212(8) 0.6196(6) -0.0047(5) 0.096(3) Uani 1 1 d . . . H9A H 0.1938 0.6326 0.0443 0.144 Uiso 1 1 calc R . . H9B H 0.1922 0.6597 -0.0419 0.144 Uiso 1 1 calc R . . H9C H 0.3052 0.6263 -0.0015 0.144 Uiso 1 1 calc R . . C10 C 0.1677(8) 0.5799(6) -0.1643(5) 0.085(2) Uani 1 1 d . . . H10A H 0.1760 0.5533 -0.2132 0.128 Uiso 1 1 calc R . . H10B H 0.2373 0.6178 -0.1493 0.128 Uiso 1 1 calc R . . H10C H 0.1018 0.6143 -0.1675 0.128 Uiso 1 1 calc R . . C11 C 0.0712(6) 0.4031(6) -0.2125(4) 0.065(2) Uani 1 1 d . B . H11A H 0.0426 0.4558 -0.2353 0.079 Uiso 1 1 calc R . . H11B H 0.0066 0.3568 -0.2158 0.079 Uiso 1 1 calc R . . C12 C 0.1429(9) 0.3967(7) -0.4175(4) 0.110(4) Uani 1 1 d D . . H12A H 0.2256 0.4165 -0.4171 0.132 Uiso 1 1 calc R . . H12B H 0.0991 0.4483 -0.4191 0.132 Uiso 1 1 calc R . . C13 C 0.1066(14) 0.3374(10) -0.4848(5) 0.196(9) Uani 1 1 d D . . H13A H 0.1391 0.2818 -0.4776 0.295 Uiso 1 1 calc R . . H13B H 0.1345 0.3650 -0.5301 0.295 Uiso 1 1 calc R . . H13C H 0.0228 0.3273 -0.4899 0.295 Uiso 1 1 calc R . . C14 C 0.2979(10) 0.2309(9) -0.2638(9) 0.137(5) Uani 1 1 d D . . H14A H 0.3730 0.2609 -0.2498 0.165 Uiso 0.82(17) 1 d PR A 1 H14B H 0.2839 0.2231 -0.3169 0.165 Uiso 0.82(17) 1 d PR A 1 H14C H 0.3461 0.2096 -0.2198 0.165 Uiso 0.18(17) 1 d PR A 2 H14D H 0.3444 0.2714 -0.2909 0.165 Uiso 0.18(17) 1 d PR A 2 C16 C 0.1986(6) 0.4818(7) 0.1095(4) 0.075(2) Uani 1 1 d . . . H16A H 0.1469 0.4451 0.1404 0.090 Uiso 1 1 calc R . . H16B H 0.1847 0.5431 0.1184 0.090 Uiso 1 1 calc R . . C17 C 0.5444(7) 0.5484(9) 0.0993(5) 0.100(4) Uani 1 1 d . . . H17A H 0.5868 0.5093 0.0699 0.119 Uiso 1 1 calc R . . H17B H 0.5681 0.5424 0.1530 0.119 Uiso 1 1 calc R . . C18 C 0.5718(9) 0.6432(9) 0.0751(7) 0.115(4) Uani 1 1 d . . . H18A H 0.5479 0.6487 0.0220 0.173 Uiso 1 1 calc R . . H18B H 0.6544 0.6597 0.0829 0.173 Uiso 1 1 calc R . . H18C H 0.5305 0.6816 0.1050 0.173 Uiso 1 1 calc R . . C15A C 0.2910(18) 0.1443(10) -0.2241(11) 0.213 Uani 0.79 1 d PD B 1 H15A H 0.3219 0.1508 -0.1675 0.319 Uiso 0.79(3) 1 d PR B 1 H15B H 0.3401 0.1046 -0.2454 0.319 Uiso 0.79(3) 1 d PR B 1 H15C H 0.2136 0.1195 -0.2234 0.319 Uiso 0.79(3) 1 d PR B 1 C15B C 0.2579(18) 0.1461(10) -0.3058(11) 0.17(4) Uani 0.21(3) 1 d PRD B 2 H15D H 0.1689 0.1383 -0.3075 0.250 Uiso 0.21(3) 1 d PR B 2 H15E H 0.2935 0.1043 -0.2995 0.250 Uiso 0.21(3) 1 d PR B 2 H15F H 0.2608 0.1665 -0.3671 0.250 Uiso 0.21(3) 1 d PR B 2 C19A C 0.459(4) 0.327(2) 0.179(2) 0.187 Uani 0.42 1 d PD C 1 H19A H 0.4544 0.3449 0.2302 0.225 Uiso 0.42(3) 1 d PR C 1 H19B H 0.5413 0.3424 0.1649 0.225 Uiso 0.42(3) 1 d PR C 1 C19B C 0.384(2) 0.3011(13) 0.1880(11) 0.127(10) Uani 0.58(3) 1 d PD C 2 H19C H 0.3299 0.2489 0.1745 0.152 Uiso 0.58(3) 1 d PR C 2 H19D H 0.3593 0.3254 0.2367 0.152 Uiso 0.58(3) 1 d PR C 2 C20A C 0.427(5) 0.227(2) 0.169(4) 0.29(4) Uani 0.42(3) 1 d PD C 1 H20A H 0.3441 0.2172 0.1556 0.342 Uiso 0.42(3) 1 d PR C 1 H20B H 0.4486 0.1958 0.2121 0.342 Uiso 0.42(3) 1 d PR C 1 H20C H 0.4664 0.2055 0.1246 0.342 Uiso 0.42(3) 1 d PR C 1 C20B C 0.515(2) 0.292(3) 0.184(4) 0.33(4) Uani 0.58(3) 1 d PD C 2 H20D H 0.5215 0.2262 0.1779 0.393 Uiso 0.58(3) 1 d PR C 2 H20E H 0.5499 0.2996 0.2416 0.393 Uiso 0.58(3) 1 d PR C 2 H20F H 0.5531 0.3252 0.1553 0.393 Uiso 0.58(3) 1 d PR C 2 C21 C 0.4675(6) 0.9811(4) 0.4233(4) 0.0586(16) Uani 1 1 d . . . C22 C 0.4882(5) 0.9129(4) 0.4733(4) 0.0530(15) Uani 1 1 d . . . C23 C 0.5206(6) 0.9323(4) 0.5505(4) 0.0598(17) Uani 1 1 d . . . C24 C 0.5440(10) 0.8585(5) 0.6063(5) 0.098(3) Uani 1 1 d . . . H24A H 0.6249 0.8650 0.6245 0.148 Uiso 1 1 calc R . . H24B H 0.5259 0.8021 0.5809 0.148 Uiso 1 1 calc R . . H24C H 0.4959 0.8620 0.6488 0.148 Uiso 1 1 calc R . . C25 C 0.4345(9) 0.9641(6) 0.3388(5) 0.086(3) Uani 1 1 d . . . H25A H 0.3528 0.9705 0.3284 0.129 Uiso 1 1 calc R . . H25B H 0.4501 0.9051 0.3253 0.129 Uiso 1 1 calc R . . H25C H 0.4799 1.0062 0.3092 0.129 Uiso 1 1 calc R . . C26 C 0.4746(6) 0.8168(4) 0.4442(5) 0.0626(18) Uani 1 1 d . . . H26A H 0.5300 0.7845 0.4741 0.075 Uiso 1 1 calc R . . H26B H 0.4969 0.8167 0.3918 0.075 Uiso 1 1 calc R . . C27 C 0.1315(8) 0.7917(6) 0.3819(7) 0.098(3) Uani 1 1 d . . . H27A H 0.0881 0.7997 0.4266 0.117 Uiso 1 1 calc R . . H27B H 0.1196 0.7296 0.3668 0.117 Uiso 1 1 calc R . . C28 C 0.0882(10) 0.8459(9) 0.3197(8) 0.141(5) Uani 1 1 d . . . H28A H 0.1143 0.9072 0.3301 0.212 Uiso 1 1 calc R . . H28B H 0.0042 0.8383 0.3155 0.212 Uiso 1 1 calc R . . H28C H 0.1175 0.8280 0.2727 0.212 Uiso 1 1 calc R . . C29 C 0.2526(17) 0.6751(8) 0.5694(8) 0.187(9) Uani 1 1 d D . . H29A H 0.1687 0.6754 0.5718 0.225 Uiso 1 1 calc R . . H29B H 0.2665 0.6234 0.5397 0.225 Uiso 1 1 calc R . . C30 C 0.307(2) 0.6676(14) 0.6487(11) 0.280(14) Uani 1 1 d D . . H30A H 0.3900 0.6829 0.6487 0.420 Uiso 1 1 calc R . . H30B H 0.2920 0.6078 0.6660 0.420 Uiso 1 1 calc R . . H30C H 0.2742 0.7073 0.6824 0.420 Uiso 1 1 calc R . . N1 N 0.0978(5) 0.4714(4) 0.3426(4) 0.0650(16) Uani 1 1 d . . . N2 N 0.3807(5) 0.4150(4) 0.4430(3) 0.0526(13) Uani 1 1 d . . . N3 N 0.3068(7) 0.6952(5) 0.2322(4) 0.0793(19) Uani 1 1 d . . . O1 O 0.2870(4) 0.4320(4) -0.2729(3) 0.0801(16) Uani 1 1 d . B . O2 O 0.1178(5) 0.3435(5) -0.3485(3) 0.097(2) Uani 1 1 d D B . O3 O 0.2059(5) 0.2779(4) -0.2346(3) 0.0892(17) Uani 1 1 d D B . O4 O 0.3763(4) 0.4952(4) 0.2230(2) 0.0711(14) Uani 1 1 d . . . O5 O 0.4205(4) 0.5248(5) 0.0865(3) 0.0873(19) Uani 1 1 d . . . O6 O 0.3704(6) 0.3720(5) 0.1272(4) 0.103(2) Uani 1 1 d D . . O7 O 0.3311(4) 0.6674(3) 0.4148(3) 0.0641(12) Uani 1 1 d . . . O8 O 0.2556(4) 0.8167(3) 0.4007(4) 0.0770(15) Uani 1 1 d . . . O9 O 0.2992(6) 0.7573(4) 0.5291(3) 0.0866(17) Uani 1 1 d D . . O10 O 0.1588(5) 0.4540(4) 0.2881(3) 0.0774(15) Uani 1 1 d . . . O11 O 0.1446(4) 0.5294(4) 0.3889(3) 0.0786(15) Uani 1 1 d . . . O12 O 0.0001(5) 0.4358(5) 0.3475(4) 0.101(2) Uani 1 1 d . . . O13 O 0.3662(4) 0.4920(3) 0.4643(2) 0.0531(10) Uani 1 1 d . . . O14 O 0.4047(5) 0.3591(3) 0.4890(3) 0.0750(15) Uani 1 1 d . . . O15 O 0.3664(5) 0.4001(3) 0.3724(3) 0.0748(15) Uani 1 1 d . . . O16 O 0.4048(5) 0.6836(4) 0.2630(3) 0.0850(17) Uani 1 1 d . . . O17 O 0.2907(8) 0.7563(5) 0.1883(5) 0.134(3) Uani 1 1 d . . . O18 O 0.2219(4) 0.6430(3) 0.2503(3) 0.0706(14) Uani 1 1 d . . . O19 O 0.5344(4) 0.5636(4) 0.3599(2) 0.0690(14) Uani 1 1 d . . . H1W H 0.5676 0.6041 0.3908 0.083 Uiso 1 1 d R . . H2W H 0.5759 0.5276 0.3383 0.083 Uiso 1 1 d R . . O20 O 0.103(3) 0.221(2) 0.311(2) 0.289(17) Uani 0.50 1 d PD . . H3W H 0.1169 0.1699 0.2949 0.347 Uiso 0.50 1 d PRD . . H4W H 0.0387 0.2391 0.2920 0.347 Uiso 0.50 1 d PRD . . O21 O 0.155(5) 0.984(2) 0.549(3) 0.48(4) Uani 0.50 1 d PD . . H5W H 0.1753 1.0304 0.5231 0.577 Uiso 0.50 1 d PRD . . H6W H 0.2050 0.9736 0.5862 0.577 Uiso 0.50 1 d PRD . . P1 P 0.18236(16) 0.36927(16) -0.26900(10) 0.0673(5) Uani 1 1 d . . . P2 P 0.34647(16) 0.46817(16) 0.14201(9) 0.0660(5) Uani 1 1 d . C . P3 P 0.33532(16) 0.75786(11) 0.44651(10) 0.0535(4) 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 Er1 0.03807(16) 0.05176(17) 0.03430(15) -0.00117(10) -0.00222(9) 0.00079(10) C1 0.039(3) 0.099(6) 0.048(4) -0.006(4) 0.002(3) 0.002(3) C2 0.046(4) 0.106(6) 0.043(4) 0.006(4) -0.001(3) 0.000(4) C3 0.047(4) 0.106(6) 0.033(3) -0.010(4) 0.000(3) 0.002(4) C4 0.045(4) 0.099(6) 0.051(4) -0.017(4) -0.012(3) 0.019(4) C5 0.045(4) 0.093(5) 0.043(3) 0.000(3) -0.005(3) 0.014(3) C6 0.031(3) 0.097(5) 0.038(3) -0.004(3) -0.002(2) 0.004(3) C7 0.080(6) 0.108(7) 0.069(5) -0.007(5) 0.006(4) -0.018(5) C8 0.104(7) 0.152(10) 0.060(5) 0.031(6) -0.012(5) -0.034(7) C9 0.095(7) 0.105(7) 0.084(6) -0.043(5) -0.038(5) 0.022(5) C10 0.090(6) 0.102(7) 0.066(5) 0.007(5) -0.006(4) 0.023(5) C11 0.038(3) 0.114(6) 0.042(4) -0.009(4) -0.005(3) 0.001(4) C12 0.088(7) 0.174(11) 0.065(6) 0.009(6) 0.012(5) 0.002(7) C13 0.226(17) 0.28(2) 0.046(6) 0.015(8) -0.005(8) -0.149(16) C14 0.110(9) 0.154(12) 0.153(12) -0.017(11) 0.032(9) 0.023(9) C16 0.050(4) 0.136(7) 0.039(4) -0.010(4) -0.003(3) 0.014(4) C17 0.042(4) 0.195(12) 0.062(5) -0.008(6) 0.000(4) 0.020(6) C18 0.072(6) 0.174(12) 0.095(7) -0.009(8) 0.001(5) -0.012(7) C15A 0.218 0.215 0.230 -0.014 0.101 0.087 C15B 0.18(7) 0.12(5) 0.21(9) -0.07(5) 0.13(6) -0.01(4) C19A 0.158 0.227 0.192 -0.066 -0.032 0.130 C19B 0.14(2) 0.13(2) 0.106(16) -0.011(13) 0.018(14) 0.021(16) C20A 0.39(9) 0.15(4) 0.33(7) -0.07(5) -0.12(7) 0.19(6) C20B 0.30(7) 0.18(4) 0.49(10) -0.07(5) 0.09(6) -0.06(4) C21 0.054(4) 0.055(4) 0.062(4) 0.002(3) -0.009(3) -0.008(3) C22 0.045(3) 0.048(3) 0.063(4) 0.000(3) -0.011(3) -0.002(3) C23 0.065(4) 0.046(4) 0.065(4) 0.007(3) -0.012(3) -0.001(3) C24 0.146(9) 0.059(5) 0.080(6) 0.018(4) -0.041(6) -0.011(5) C25 0.109(7) 0.077(5) 0.067(5) 0.002(4) -0.002(5) -0.015(5) C26 0.057(4) 0.050(4) 0.080(5) 0.000(3) -0.003(3) 0.007(3) C27 0.064(5) 0.080(6) 0.147(9) -0.010(6) -0.005(6) 0.003(4) C28 0.101(8) 0.133(10) 0.187(14) 0.011(9) -0.050(9) 0.032(8) C29 0.32(2) 0.119(11) 0.118(11) -0.010(9) 0.090(14) -0.062(13) C30 0.43(4) 0.189(19) 0.19(2) 0.096(17) 0.01(2) -0.09(2) N1 0.045(3) 0.086(4) 0.062(4) 0.023(3) -0.002(3) -0.003(3) N2 0.057(3) 0.054(3) 0.046(3) -0.003(2) -0.010(2) 0.011(3) N3 0.085(5) 0.082(5) 0.067(4) 0.024(4) -0.009(4) 0.000(4) O1 0.049(3) 0.130(5) 0.057(3) -0.024(3) 0.009(2) -0.013(3) O2 0.079(4) 0.162(6) 0.040(3) -0.016(3) 0.005(2) -0.036(4) O3 0.079(4) 0.115(5) 0.076(4) -0.005(3) 0.018(3) 0.013(3) O4 0.057(3) 0.123(4) 0.034(2) -0.012(2) -0.007(2) 0.019(3) O5 0.049(3) 0.168(6) 0.043(3) -0.002(3) -0.002(2) 0.005(3) O6 0.107(5) 0.131(6) 0.071(4) -0.027(4) -0.017(3) 0.040(4) O7 0.081(3) 0.045(2) 0.063(3) -0.008(2) 0.002(2) -0.006(2) O8 0.061(3) 0.058(3) 0.109(4) 0.009(3) -0.008(3) -0.004(2) O9 0.112(5) 0.071(3) 0.073(4) -0.016(3) 0.023(3) -0.014(3) O10 0.067(3) 0.088(4) 0.072(3) -0.012(3) 0.002(3) -0.018(3) O11 0.054(3) 0.107(4) 0.071(3) -0.021(3) 0.009(3) -0.013(3) O12 0.057(3) 0.139(6) 0.099(5) 0.025(4) -0.004(3) -0.032(4) O13 0.064(3) 0.053(3) 0.044(2) -0.0026(19) 0.005(2) 0.012(2) O14 0.102(4) 0.062(3) 0.062(3) 0.012(2) -0.015(3) 0.022(3) O15 0.112(4) 0.066(3) 0.045(3) -0.012(2) -0.015(3) 0.015(3) O16 0.069(4) 0.103(4) 0.077(4) 0.027(3) -0.006(3) -0.016(3) O17 0.160(7) 0.126(6) 0.108(6) 0.067(5) -0.017(5) -0.007(5) O18 0.059(3) 0.072(3) 0.078(3) 0.018(3) -0.012(3) 0.001(3) O19 0.062(3) 0.104(4) 0.035(2) -0.003(2) -0.009(2) -0.016(3) O20 0.31(4) 0.22(3) 0.36(5) 0.00(3) 0.09(3) 0.08(3) O21 0.85(11) 0.20(3) 0.41(6) -0.17(4) 0.39(7) -0.06(5) P1 0.0479(10) 0.1096(16) 0.0415(9) -0.0149(10) 0.0033(7) -0.0073(10) P2 0.0498(10) 0.1163(17) 0.0326(8) -0.0128(9) -0.0043(7) 0.0174(10) P3 0.0602(10) 0.0407(8) 0.0578(10) -0.0047(7) 0.0006(8) -0.0013(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O7 2.238(4) . ? Er1 O4 2.243(4) . ? Er1 O19 2.338(5) . ? Er1 O11 2.406(5) . ? Er1 O18 2.406(5) . ? Er1 O10 2.454(5) . ? Er1 O15 2.462(5) . ? Er1 O16 2.469(5) . ? Er1 O13 2.478(4) . ? Er1 N3 2.847(7) . ? Er1 N1 2.858(6) . ? C1 C2 1.389(9) . ? C1 C6 1.392(10) . ? C1 C7 1.518(11) . ? C2 C3 1.365(11) . ? C2 C8 1.532(12) . ? C3 C4 1.393(11) . ? C3 C16 1.536(9) . ? C4 C5 1.405(9) . ? C4 C9 1.485(12) . ? C5 C6 1.370(10) . ? C5 C10 1.520(11) . ? C6 C11 1.532(8) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 P1 1.780(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O2 1.485(8) . ? C12 C13 1.491(9) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 O3 1.451(8) . ? C14 C15A 1.487(10) . ? C14 C15B 1.494(10) . ? C14 H14A 0.9534 . ? C14 H14B 0.9401 . ? C14 H14C 0.9946 . ? C14 H14D 0.9285 . ? C16 P2 1.791(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 O5 1.438(9) . ? C17 C18 1.510(16) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C15A H15A 1.0325 . ? C15A H15B 0.9561 . ? C15A H15C 0.9326 . ? C15B H15D 1.0179 . ? C15B H15E 0.7910 . ? C15B H15F 1.1222 . ? C19A O6 1.536(10) . ? C19A C20A 1.539(10) . ? C19A H19A 0.9330 . ? C19A H19B 1.0021 . ? C19B O6 1.529(10) . ? C19B C20B 1.535(10) . ? C19B H19C 0.9744 . ? C19B H19D 0.9965 . ? C20A H20A 0.9649 . ? C20A H20B 0.9252 . ? C20A H20C 0.9941 . ? C20A H20D 1.0887 . ? C20B H20D 1.0080 . ? C20B H20E 1.0720 . ? C20B H20F 0.8267 . ? C21 C23 1.377(9) 2_676 ? C21 C22 1.388(9) . ? C21 C25 1.520(10) . ? C22 C23 1.404(9) . ? C22 C26 1.528(9) . ? C23 C21 1.377(9) 2_676 ? C23 C24 1.522(10) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 P3 1.761(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O8 1.457(10) . ? C27 C28 1.460(15) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.498(10) . ? C29 O9 1.505(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? N1 O12 1.207(7) . ? N1 O11 1.251(8) . ? N1 O10 1.264(8) . ? N2 O14 1.212(7) . ? N2 O13 1.251(6) . ? N2 O15 1.254(7) . ? N3 O17 1.228(9) . ? N3 O16 1.247(8) . ? N3 O18 1.255(8) . ? O1 P1 1.465(5) . ? O2 P1 1.566(5) . ? O3 P1 1.553(7) . ? O4 P2 1.486(5) . ? O5 P2 1.545(6) . ? O6 P2 1.532(7) . ? O7 P3 1.471(5) . ? O8 P3 1.534(6) . ? O9 P3 1.534(6) . ? O19 H1W 0.8600 . ? O19 H2W 0.8600 . ? O20 H3W 0.8568 . ? O20 H4W 0.8639 . ? O21 H5W 0.8583 . ? O21 H6W 0.8632 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Er1 O4 150.5(2) . . ? O7 Er1 O19 86.69(19) . . ? O4 Er1 O19 82.80(17) . . ? O7 Er1 O11 75.90(18) . . ? O4 Er1 O11 125.68(18) . . ? O19 Er1 O11 145.42(18) . . ? O7 Er1 O18 82.89(19) . . ? O4 Er1 O18 81.73(19) . . ? O19 Er1 O18 127.10(18) . . ? O11 Er1 O18 80.7(2) . . ? O7 Er1 O10 125.52(19) . . ? O4 Er1 O10 74.09(19) . . ? O19 Er1 O10 145.1(2) . . ? O11 Er1 O10 51.81(18) . . ? O18 Er1 O10 75.41(19) . . ? O7 Er1 O15 125.26(16) . . ? O4 Er1 O15 79.11(19) . . ? O19 Er1 O15 77.61(19) . . ? O11 Er1 O15 88.3(2) . . ? O18 Er1 O15 146.22(18) . . ? O10 Er1 O15 72.7(2) . . ? O7 Er1 O16 74.4(2) . . ? O4 Er1 O16 76.3(2) . . ? O19 Er1 O16 75.37(19) . . ? O11 Er1 O16 126.0(2) . . ? O18 Er1 O16 51.85(18) . . ? O10 Er1 O16 122.15(19) . . ? O15 Er1 O16 145.3(2) . . ? O7 Er1 O13 74.39(16) . . ? O4 Er1 O13 127.81(17) . . ? O19 Er1 O13 73.73(15) . . ? O11 Er1 O13 72.89(18) . . ? O18 Er1 O13 148.48(17) . . ? O10 Er1 O13 100.23(17) . . ? O15 Er1 O13 50.89(14) . . ? O16 Er1 O13 136.83(17) . . ? O7 Er1 N3 77.9(2) . . ? O4 Er1 N3 77.3(2) . . ? O19 Er1 N3 101.2(2) . . ? O11 Er1 N3 104.0(2) . . ? O18 Er1 N3 25.96(18) . . ? O10 Er1 N3 98.8(2) . . ? O15 Er1 N3 156.3(2) . . ? O16 Er1 N3 25.90(19) . . ? O13 Er1 N3 152.04(19) . . ? O7 Er1 N1 100.9(2) . . ? O4 Er1 N1 100.2(2) . . ? O19 Er1 N1 154.95(18) . . ? O11 Er1 N1 25.71(18) . . ? O18 Er1 N1 77.78(17) . . ? O10 Er1 N1 26.14(18) . . ? O15 Er1 N1 78.57(19) . . ? O16 Er1 N1 129.61(18) . . ? O13 Er1 N1 85.27(16) . . ? N3 Er1 N1 103.74(19) . . ? C2 C1 C6 118.3(7) . . ? C2 C1 C7 120.9(7) . . ? C6 C1 C7 120.8(6) . . ? C3 C2 C1 121.3(7) . . ? C3 C2 C8 120.1(7) . . ? C1 C2 C8 118.5(8) . . ? C2 C3 C4 120.4(6) . . ? C2 C3 C16 121.9(7) . . ? C4 C3 C16 117.6(7) . . ? C3 C4 C5 118.7(7) . . ? C3 C4 C9 122.5(7) . . ? C5 C4 C9 118.8(8) . . ? C6 C5 C4 120.0(7) . . ? C6 C5 C10 120.3(6) . . ? C4 C5 C10 119.7(7) . . ? C5 C6 C1 121.1(6) . . ? C5 C6 C11 119.7(7) . . ? C1 C6 C11 119.2(7) . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 P1 117.1(4) . . ? C6 C11 H11A 108.0 . . ? P1 C11 H11A 108.0 . . ? C6 C11 H11B 108.0 . . ? P1 C11 H11B 108.0 . . ? H11A C11 H11B 107.3 . . ? O2 C12 C13 106.5(8) . . ? O2 C12 H12A 110.4 . . ? C13 C12 H12A 110.4 . . ? O2 C12 H12B 110.4 . . ? C13 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O3 C14 C15A 105.3(11) . . ? O3 C14 C15B 115.5(11) . . ? C15A C14 C15B 58.7(3) . . ? O3 C14 H14A 110.9 . . ? C15A C14 H14A 107.2 . . ? C15B C14 H14A 133.6 . . ? O3 C14 H14B 109.1 . . ? C15A C14 H14B 111.3 . . ? C15B C14 H14B 53.1 . . ? H14A C14 H14B 112.8 . . ? O3 C14 H14C 108.6 . . ? C15A C14 H14C 49.0 . . ? C15B C14 H14C 101.7 . . ? H14A C14 H14C 60.2 . . ? H14B C14 H14C 141.2 . . ? O3 C14 H14D 107.2 . . ? C15A C14 H14D 145.7 . . ? C15B C14 H14D 114.7 . . ? H14A C14 H14D 50.1 . . ? H14B C14 H14D 67.7 . . ? H14C C14 H14D 108.8 . . ? C3 C16 P2 116.0(5) . . ? C3 C16 H16A 108.3 . . ? P2 C16 H16A 108.3 . . ? C3 C16 H16B 108.3 . . ? P2 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? O5 C17 C18 108.6(8) . . ? O5 C17 H17A 110.0 . . ? C18 C17 H17A 110.0 . . ? O5 C17 H17B 110.0 . . ? C18 C17 H17B 110.0 . . ? H17A C17 H17B 108.3 . . ? 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 . . ? C14 C15A H14C 42.0 . . ? C14 C15A H15A 112.1 . . ? H14C C15A H15A 74.6 . . ? C14 C15A H15B 111.5 . . ? H14C C15A H15B 104.4 . . ? H15A C15A H15B 104.0 . . ? C14 C15A H15C 111.0 . . ? H14C C15A H15C 141.8 . . ? H15A C15A H15C 105.7 . . ? H15B C15A H15C 112.2 . . ? C14 C15A H15E 86.1 . . ? H14C C15A H15E 110.9 . . ? H15A C15A H15E 150.5 . . ? H15B C15A H15E 46.6 . . ? H15C C15A H15E 87.7 . . ? C14 C15B H14B 39.0 . . ? C14 C15B H15B 84.2 . . ? H14B C15B H15B 114.3 . . ? C14 C15B H15D 107.6 . . ? H14B C15B H15D 105.8 . . ? H15B C15B H15D 125.0 . . ? C14 C15B H15E 119.8 . . ? H14B C15B H15E 134.6 . . ? H15B C15B H15E 38.9 . . ? H15D C15B H15E 119.6 . . ? C14 C15B H15F 102.4 . . ? H14B C15B H15F 63.6 . . ? H15B C15B H15F 136.8 . . ? H15D C15B H15F 94.1 . . ? H15E C15B H15F 108.8 . . ? O6 C19A C20A 106(2) . . ? O6 C19A H19A 110.3 . . ? C20A C19A H19A 111.1 . . ? O6 C19A H19B 111.9 . . ? C20A C19A H19B 108.8 . . ? H19A C19A H19B 108.7 . . ? O6 C19A H19D 82.9 . . ? C20A C19A H19D 86.8 . . ? H19A C19A H19D 44.5 . . ? H19B C19A H19D 153.2 . . ? O6 C19A H20E 168.6 . . ? C20A C19A H20E 84.2 . . ? H19A C19A H20E 60.3 . . ? H19B C19A H20E 68.2 . . ? H19D C19A H20E 92.9 . . ? O6 C19A H20F 115.0 . . ? C20A C19A H20F 93.6 . . ? H19A C19A H20F 118.9 . . ? H19B C19A H20F 15.6 . . ? H19D C19A H20F 161.1 . . ? H20E C19A H20F 68.4 . . ? O6 C19B C20B 99(3) . . ? O6 C19B H19A 96.7 . . ? C20B C19B H19A 60.3 . . ? O6 C19B H19C 109.5 . . ? C20B C19B H19C 117.0 . . ? H19A C19B H19C 153.6 . . ? O6 C19B H19D 107.2 . . ? C20B C19B H19D 116.7 . . ? H19A C19B H19D 60.1 . . ? H19C C19B H19D 106.9 . . ? O6 C19B H20A 109.0 . . ? C20B C19B H20A 96.2 . . ? H19A C19B H20A 148.0 . . ? H19C C19B H20A 21.8 . . ? H19D C19B H20A 125.6 . . ? C19A C20A H19C 81.4 . . ? C19A C20A H20A 107.7 . . ? H19C C20A H20A 30.8 . . ? C19A C20A H20B 111.9 . . ? H19C C20A H20B 109.2 . . ? H20A C20A H20B 112.1 . . ? C19A C20A H20C 109.2 . . ? H19C C20A H20C 131.7 . . ? H20A C20A H20C 106.3 . . ? H20B C20A H20C 109.5 . . ? C19A C20A H20D 81.8 . . ? H19C C20A H20D 159.9 . . ? H20A C20A H20D 169.2 . . ? H20B C20A H20D 67.5 . . ? H20C C20A H20D 64.9 . . ? C19B C20B H19A 48.2 . . ? C19B C20B H19B 103.1 . . ? H19A C20B H19B 83.9 . . ? C19B C20B H20D 105.7 . . ? H19A C20B H20D 135.4 . . ? H19B C20B H20D 140.8 . . ? C19B C20B H20E 104.1 . . ? H19A C20B H20E 64.7 . . ? H19B C20B H20E 100.6 . . ? H20D C20B H20E 97.8 . . ? C19B C20B H20F 118.9 . . ? H19A C20B H20F 107.6 . . ? H19B C20B H20F 23.7 . . ? H20D C20B H20F 117.1 . . ? H20E C20B H20F 110.6 . . ? C23 C21 C22 120.0(6) 2_676 . ? C23 C21 C25 118.0(6) 2_676 . ? C22 C21 C25 122.0(7) . . ? C21 C22 C23 119.8(6) . . ? C21 C22 C26 119.9(6) . . ? C23 C22 C26 120.3(6) . . ? C21 C23 C22 120.3(6) 2_676 . ? C21 C23 C24 119.1(7) 2_676 . ? C22 C23 C24 120.6(6) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 P3 117.3(5) . . ? C22 C26 H26A 108.0 . . ? P3 C26 H26A 108.0 . . ? C22 C26 H26B 108.0 . . ? P3 C26 H26B 108.0 . . ? H26A C26 H26B 107.2 . . ? O8 C27 C28 110.5(9) . . ? O8 C27 H27A 109.6 . . ? C28 C27 H27A 109.6 . . ? O8 C27 H27B 109.6 . . ? C28 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? 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 . . ? C30 C29 O9 113.2(11) . . ? C30 C29 H29A 108.9 . . ? O9 C29 H29A 108.9 . . ? C30 C29 H29B 108.9 . . ? O9 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? 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 . . ? O12 N1 O11 123.1(7) . . ? O12 N1 O10 121.7(7) . . ? O11 N1 O10 115.2(6) . . ? O12 N1 Er1 178.2(5) . . ? O11 N1 Er1 56.5(3) . . ? O10 N1 Er1 58.8(3) . . ? O14 N2 O13 120.9(5) . . ? O14 N2 O15 123.3(6) . . ? O13 N2 O15 115.9(5) . . ? O17 N3 O16 123.0(8) . . ? O17 N3 O18 120.1(8) . . ? O16 N3 O18 116.9(6) . . ? O17 N3 Er1 177.1(7) . . ? O16 N3 Er1 59.9(4) . . ? O18 N3 Er1 57.0(3) . . ? C12 O2 P1 121.0(5) . . ? C14 O3 P1 118.9(7) . . ? P2 O4 Er1 151.9(3) . . ? C17 O5 P2 123.8(6) . . ? C19B O6 P2 125.8(10) . . ? C19B O6 C19A 36(2) . . ? P2 O6 C19A 120.6(16) . . ? P3 O7 Er1 162.9(3) . . ? C27 O8 P3 123.5(5) . . ? C29 O9 P3 123.9(6) . . ? N1 O10 Er1 95.1(4) . . ? N1 O11 Er1 97.8(4) . . ? N2 O13 Er1 96.2(3) . . ? N2 O15 Er1 96.9(4) . . ? N3 O16 Er1 94.2(4) . . ? N3 O18 Er1 97.0(4) . . ? Er1 O19 H1W 119.8 . . ? Er1 O19 H2W 120.2 . . ? H1W O19 H2W 120.0 . . ? H3W O20 H4W 114.3 . . ? H5W O21 H6W 114.6 . . ? O1 P1 O3 114.5(4) . . ? O1 P1 O2 114.2(3) . . ? O3 P1 O2 103.1(4) . . ? O1 P1 C11 116.3(4) . . ? O3 P1 C11 102.6(4) . . ? O2 P1 C11 104.6(3) . . ? O4 P2 O6 111.7(4) . . ? O4 P2 O5 112.2(3) . . ? O6 P2 O5 105.6(4) . . ? O4 P2 C16 113.9(3) . . ? O6 P2 C16 109.0(4) . . ? O5 P2 C16 103.9(4) . . ? O7 P3 O9 111.5(3) . . ? O7 P3 O8 113.1(3) . . ? O9 P3 O8 107.3(4) . . ? O7 P3 C26 112.7(3) . . ? O9 P3 C26 108.5(4) . . ? O8 P3 C26 103.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.2(11) . . . . ? C7 C1 C2 C3 -179.6(7) . . . . ? C6 C1 C2 C8 -178.7(7) . . . . ? C7 C1 C2 C8 1.9(11) . . . . ? C1 C2 C3 C4 3.0(11) . . . . ? C8 C2 C3 C4 -178.6(8) . . . . ? C1 C2 C3 C16 179.5(6) . . . . ? C8 C2 C3 C16 -2.0(11) . . . . ? C2 C3 C4 C5 -3.4(10) . . . . ? C16 C3 C4 C5 179.9(6) . . . . ? C2 C3 C4 C9 175.2(7) . . . . ? C16 C3 C4 C9 -1.5(10) . . . . ? C3 C4 C5 C6 1.2(10) . . . . ? C9 C4 C5 C6 -177.5(7) . . . . ? C3 C4 C5 C10 -177.5(7) . . . . ? C9 C4 C5 C10 3.9(10) . . . . ? C4 C5 C6 C1 1.6(10) . . . . ? C10 C5 C6 C1 -179.8(7) . . . . ? C4 C5 C6 C11 179.3(6) . . . . ? C10 C5 C6 C11 -2.1(10) . . . . ? C2 C1 C6 C5 -2.1(10) . . . . ? C7 C1 C6 C5 177.4(7) . . . . ? C2 C1 C6 C11 -179.8(6) . . . . ? C7 C1 C6 C11 -0.4(10) . . . . ? C5 C6 C11 P1 89.2(8) . . . . ? C1 C6 C11 P1 -93.0(7) . . . . ? C2 C3 C16 P2 92.2(8) . . . . ? C4 C3 C16 P2 -91.2(8) . . . . ? C23 C21 C22 C23 0.4(12) 2_676 . . . ? C25 C21 C22 C23 178.8(7) . . . . ? C23 C21 C22 C26 179.8(6) 2_676 . . . ? C25 C21 C22 C26 -1.8(10) . . . . ? C21 C22 C23 C21 -0.4(12) . . . 2_676 ? C26 C22 C23 C21 -179.8(6) . . . 2_676 ? C21 C22 C23 C24 -179.9(8) . . . . ? C26 C22 C23 C24 0.7(11) . . . . ? C21 C22 C26 P3 -89.2(8) . . . . ? C23 C22 C26 P3 90.2(7) . . . . ? O7 Er1 N1 O12 -93(21) . . . . ? O4 Er1 N1 O12 108(21) . . . . ? O19 Er1 N1 O12 13(22) . . . . ? O11 Er1 N1 O12 -79(21) . . . . ? O18 Er1 N1 O12 -173(21) . . . . ? O10 Er1 N1 O12 106(21) . . . . ? O15 Er1 N1 O12 32(21) . . . . ? O16 Er1 N1 O12 -171(21) . . . . ? O13 Er1 N1 O12 -19(21) . . . . ? N3 Er1 N1 O12 -173(21) . . . . ? O7 Er1 N1 O11 -13.7(5) . . . . ? O4 Er1 N1 O11 -173.0(4) . . . . ? O19 Er1 N1 O11 92.2(6) . . . . ? O18 Er1 N1 O11 -93.8(5) . . . . ? O10 Er1 N1 O11 -175.6(7) . . . . ? O15 Er1 N1 O11 110.5(5) . . . . ? O16 Er1 N1 O11 -92.4(5) . . . . ? O13 Er1 N1 O11 59.4(4) . . . . ? N3 Er1 N1 O11 -93.7(5) . . . . ? O7 Er1 N1 O10 161.9(4) . . . . ? O4 Er1 N1 O10 2.6(4) . . . . ? O19 Er1 N1 O10 -92.2(6) . . . . ? O11 Er1 N1 O10 175.6(7) . . . . ? O18 Er1 N1 O10 81.8(4) . . . . ? O15 Er1 N1 O10 -74.0(4) . . . . ? O16 Er1 N1 O10 83.2(5) . . . . ? O13 Er1 N1 O10 -125.0(4) . . . . ? N3 Er1 N1 O10 81.9(4) . . . . ? O7 Er1 N3 O17 -87(13) . . . . ? O4 Er1 N3 O17 109(13) . . . . ? O19 Er1 N3 O17 -172(13) . . . . ? O11 Er1 N3 O17 -16(13) . . . . ? O18 Er1 N3 O17 11(13) . . . . ? O10 Er1 N3 O17 37(13) . . . . ? O15 Er1 N3 O17 104(13) . . . . ? O16 Er1 N3 O17 -167(14) . . . . ? O13 Er1 N3 O17 -95(13) . . . . ? N1 Er1 N3 O17 11(13) . . . . ? O7 Er1 N3 O16 79.2(5) . . . . ? O4 Er1 N3 O16 -84.8(5) . . . . ? O19 Er1 N3 O16 -4.9(5) . . . . ? O11 Er1 N3 O16 151.2(5) . . . . ? O18 Er1 N3 O16 178.0(8) . . . . ? O10 Er1 N3 O16 -156.1(5) . . . . ? O15 Er1 N3 O16 -89.5(7) . . . . ? O13 Er1 N3 O16 71.4(7) . . . . ? N1 Er1 N3 O16 177.7(5) . . . . ? O7 Er1 N3 O18 -98.7(5) . . . . ? O4 Er1 N3 O18 97.3(5) . . . . ? O19 Er1 N3 O18 177.2(5) . . . . ? O11 Er1 N3 O18 -26.8(5) . . . . ? O10 Er1 N3 O18 25.9(5) . . . . ? O15 Er1 N3 O18 92.6(7) . . . . ? O16 Er1 N3 O18 -178.0(8) . . . . ? O13 Er1 N3 O18 -106.5(5) . . . . ? N1 Er1 N3 O18 -0.3(5) . . . . ? C13 C12 O2 P1 158.0(10) . . . . ? C15A C14 O3 P1 -175.5(7) . . . . ? C15B C14 O3 P1 -113.3(7) . . . . ? O7 Er1 O4 P2 -94.0(9) . . . . ? O19 Er1 O4 P2 -164.0(8) . . . . ? O11 Er1 O4 P2 37.4(9) . . . . ? O18 Er1 O4 P2 -34.7(8) . . . . ? O10 Er1 O4 P2 42.4(8) . . . . ? O15 Er1 O4 P2 117.3(8) . . . . ? O16 Er1 O4 P2 -87.3(8) . . . . ? O13 Er1 O4 P2 133.1(8) . . . . ? N3 Er1 O4 P2 -60.7(8) . . . . ? N1 Er1 O4 P2 41.2(8) . . . . ? C18 C17 O5 P2 -140.1(7) . . . . ? C20B C19B O6 P2 -111(2) . . . . ? C20B C19B O6 C19A -17(3) . . . . ? C20A C19A O6 C19B 48(3) . . . . ? C20A C19A O6 P2 158(3) . . . . ? O4 Er1 O7 P3 20.4(14) . . . . ? O19 Er1 O7 P3 89.5(12) . . . . ? O11 Er1 O7 P3 -120.6(12) . . . . ? O18 Er1 O7 P3 -38.5(11) . . . . ? O10 Er1 O7 P3 -104.9(11) . . . . ? O15 Er1 O7 P3 161.8(11) . . . . ? O16 Er1 O7 P3 13.8(11) . . . . ? O13 Er1 O7 P3 163.5(12) . . . . ? N3 Er1 O7 P3 -12.7(11) . . . . ? N1 Er1 O7 P3 -114.6(11) . . . . ? C28 C27 O8 P3 -162.5(8) . . . . ? C30 C29 O9 P3 134.4(15) . . . . ? O12 N1 O10 Er1 -178.0(6) . . . . ? O11 N1 O10 Er1 4.1(6) . . . . ? O7 Er1 O10 N1 -22.0(5) . . . . ? O4 Er1 O10 N1 -177.3(5) . . . . ? O19 Er1 O10 N1 132.3(4) . . . . ? O11 Er1 O10 N1 -2.4(4) . . . . ? O18 Er1 O10 N1 -91.9(4) . . . . ? O15 Er1 O10 N1 99.4(4) . . . . ? O16 Er1 O10 N1 -115.4(4) . . . . ? O13 Er1 O10 N1 56.1(4) . . . . ? N3 Er1 O10 N1 -103.3(4) . . . . ? O12 N1 O11 Er1 177.9(6) . . . . ? O10 N1 O11 Er1 -4.2(7) . . . . ? O7 Er1 O11 N1 166.2(5) . . . . ? O4 Er1 O11 N1 8.5(5) . . . . ? O19 Er1 O11 N1 -131.8(4) . . . . ? O18 Er1 O11 N1 81.2(4) . . . . ? O10 Er1 O11 N1 2.5(4) . . . . ? O15 Er1 O11 N1 -66.8(4) . . . . ? O16 Er1 O11 N1 107.8(4) . . . . ? O13 Er1 O11 N1 -116.1(5) . . . . ? N3 Er1 O11 N1 92.7(5) . . . . ? O14 N2 O13 Er1 177.7(5) . . . . ? O15 N2 O13 Er1 -3.7(6) . . . . ? O7 Er1 O13 N2 -176.0(4) . . . . ? O4 Er1 O13 N2 -18.0(4) . . . . ? O19 Er1 O13 N2 -84.9(4) . . . . ? O11 Er1 O13 N2 104.3(4) . . . . ? O18 Er1 O13 N2 138.5(4) . . . . ? O10 Er1 O13 N2 59.7(4) . . . . ? O15 Er1 O13 N2 2.2(3) . . . . ? O16 Er1 O13 N2 -130.8(4) . . . . ? N3 Er1 O13 N2 -168.1(4) . . . . ? N1 Er1 O13 N2 81.3(4) . . . . ? O14 N2 O15 Er1 -177.7(6) . . . . ? O13 N2 O15 Er1 3.7(6) . . . . ? O7 Er1 O15 N2 0.0(5) . . . . ? O4 Er1 O15 N2 161.8(4) . . . . ? O19 Er1 O15 N2 76.8(4) . . . . ? O11 Er1 O15 N2 -71.4(4) . . . . ? O18 Er1 O15 N2 -141.7(4) . . . . ? O10 Er1 O15 N2 -121.7(4) . . . . ? O16 Er1 O15 N2 116.3(4) . . . . ? O13 Er1 O15 N2 -2.2(3) . . . . ? N3 Er1 O15 N2 166.5(4) . . . . ? N1 Er1 O15 N2 -95.4(4) . . . . ? O17 N3 O16 Er1 179.2(8) . . . . ? O18 N3 O16 Er1 1.9(8) . . . . ? O7 Er1 O16 N3 -94.3(5) . . . . ? O4 Er1 O16 N3 89.1(5) . . . . ? O19 Er1 O16 N3 175.1(5) . . . . ? O11 Er1 O16 N3 -35.3(6) . . . . ? O18 Er1 O16 N3 -1.1(5) . . . . ? O10 Er1 O16 N3 28.2(6) . . . . ? O15 Er1 O16 N3 135.1(5) . . . . ? O13 Er1 O16 N3 -139.5(4) . . . . ? N1 Er1 O16 N3 -2.9(6) . . . . ? O17 N3 O18 Er1 -179.3(8) . . . . ? O16 N3 O18 Er1 -2.0(8) . . . . ? O7 Er1 O18 N3 76.9(5) . . . . ? O4 Er1 O18 N3 -77.9(5) . . . . ? O19 Er1 O18 N3 -3.5(6) . . . . ? O11 Er1 O18 N3 153.7(5) . . . . ? O10 Er1 O18 N3 -153.5(5) . . . . ? O15 Er1 O18 N3 -133.8(5) . . . . ? O16 Er1 O18 N3 1.1(4) . . . . ? O13 Er1 O18 N3 120.7(5) . . . . ? N1 Er1 O18 N3 179.7(5) . . . . ? C14 O3 P1 O1 -49.8(9) . . . . ? C14 O3 P1 O2 74.8(8) . . . . ? C14 O3 P1 C11 -176.7(8) . . . . ? C12 O2 P1 O1 -15.5(9) . . . . ? C12 O2 P1 O3 -140.3(7) . . . . ? C12 O2 P1 C11 112.7(7) . . . . ? C6 C11 P1 O1 -59.3(8) . . . . ? C6 C11 P1 O3 66.4(7) . . . . ? C6 C11 P1 O2 173.7(6) . . . . ? Er1 O4 P2 O6 -127.1(8) . . . . ? Er1 O4 P2 O5 114.5(8) . . . . ? Er1 O4 P2 C16 -3.2(10) . . . . ? C19B O6 P2 O4 19.1(15) . . . . ? C19A O6 P2 O4 -23(3) . . . . ? C19B O6 P2 O5 141.3(14) . . . . ? C19A O6 P2 O5 99(3) . . . . ? C19B O6 P2 C16 -107.6(14) . . . . ? C19A O6 P2 C16 -150(3) . . . . ? C17 O5 P2 O4 43.6(8) . . . . ? C17 O5 P2 O6 -78.3(8) . . . . ? C17 O5 P2 C16 167.1(8) . . . . ? C3 C16 P2 O4 177.3(6) . . . . ? C3 C16 P2 O6 -57.3(8) . . . . ? C3 C16 P2 O5 54.9(8) . . . . ? Er1 O7 P3 O9 169.0(11) . . . . ? Er1 O7 P3 O8 48.0(12) . . . . ? Er1 O7 P3 C26 -68.6(12) . . . . ? C29 O9 P3 O7 -6.3(12) . . . . ? C29 O9 P3 O8 118.1(11) . . . . ? C29 O9 P3 C26 -131.0(11) . . . . ? C27 O8 P3 O7 53.1(8) . . . . ? C27 O8 P3 O9 -70.3(8) . . . . ? C27 O8 P3 C26 175.2(7) . . . . ? C22 C26 P3 O7 178.0(5) . . . . ? C22 C26 P3 O9 -58.0(6) . . . . ? C22 C26 P3 O8 55.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.568 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.112 data_Eu #TrackingRef '- SI-cif.txt' _database_code_depnum_ccdc_archive 'CCDC 793770' #TrackingRef '- Eu.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H54 Eu N3 O18 P3' _chemical_formula_weight 989.63 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' Eu Eu -0.1578 3.6682 '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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.562(2) _cell_length_b 16.909(4) _cell_length_c 25.421(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.468(12) _cell_angle_gamma 90.00 _cell_volume 4375.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3924 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 23.96 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2028 _exptl_absorpt_coefficient_mu 1.614 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.731 _exptl_absorpt_correction_T_max 0.785 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22828 _diffrn_reflns_av_R_equivalents 0.2418 _diffrn_reflns_av_sigmaI/netI 0.1805 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8140 _reflns_number_gt 4551 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.59 Ratio Some terminal C atoms in disordered side chains have high isotropic U-values. PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for O14 The larger than normal range of thermal motion is mostly due to the difference between the disordered group and the other atoms which are not disordered. ; _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^)+(0.0039P)^2^+0.2000P] 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 SHELXL _refine_ls_extinction_coef 0.00099(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8140 _refine_ls_number_parameters 509 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1397 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 Eu1 Eu 0.29102(3) 0.69065(2) 0.769560(15) 0.03897(14) Uani 1 1 d . . . P2 P 0.28901(18) 0.47266(12) 0.79797(9) 0.0417(6) Uani 1 1 d . . . P3 P 0.74847(18) 0.31298(14) 1.08943(8) 0.0434(5) Uani 1 1 d . . . P4 P 0.2598(2) 0.61115(14) 0.62715(9) 0.0523(6) Uani 1 1 d . . . C1 C 0.4700(6) 0.4025(4) 0.8886(3) 0.043(2) Uani 1 1 d . . . C4 C 0.5710(6) 0.3913(4) 1.0025(3) 0.039(2) Uani 1 1 d . . . C2 C 0.5751(6) 0.4533(4) 0.9158(3) 0.042(2) Uani 1 1 d . . . C8 C 0.6329(6) 0.5121(5) 0.8842(3) 0.059(3) Uani 1 1 d . . . H8A H 0.5741 0.5191 0.8485 0.089 Uiso 1 1 calc R . . H8B H 0.7159 0.4929 0.8808 0.089 Uiso 1 1 calc R . . H8C H 0.6455 0.5618 0.9031 0.089 Uiso 1 1 calc R . . C6 C 0.4185(6) 0.3483(4) 0.9182(3) 0.045(2) Uani 1 1 d . . . C9 C 0.7408(6) 0.4996(5) 1.0019(3) 0.057(3) Uani 1 1 d . . . H9A H 0.7679 0.4874 1.0401 0.086 Uiso 1 1 calc R . . H9B H 0.7145 0.5541 0.9970 0.086 Uiso 1 1 calc R . . H9C H 0.8127 0.4906 0.9861 0.086 Uiso 1 1 calc R . . C5 C 0.4665(7) 0.3423(5) 0.9744(3) 0.042(2) Uani 1 1 d . . . C3 C 0.6226(6) 0.4455(4) 0.9731(3) 0.041(2) Uani 1 1 d . . . N1 N 0.3252(7) 0.8589(5) 0.7522(4) 0.070(2) Uani 1 1 d . . . O12 O 0.3005(7) 0.8339(4) 0.7960(3) 0.089(2) Uani 1 1 d . . . O11 O 0.3369(7) 0.8080(4) 0.7180(3) 0.093(2) Uani 1 1 d . . . C20 C 0.0672(7) 0.5167(5) 0.5533(3) 0.048(2) Uani 1 1 d . . . C21 C -0.0477(7) 0.5580(5) 0.5285(3) 0.051(2) Uani 1 1 d . . . C22 C 0.1152(7) 0.4592(5) 0.5252(4) 0.052(2) Uani 1 1 d . . . C25 C 0.2400(8) 0.4129(5) 0.5529(4) 0.095(4) Uani 1 1 d . . . H25A H 0.2720 0.4299 0.5901 0.143 Uiso 1 1 calc R . . H25B H 0.3059 0.4224 0.5339 0.143 Uiso 1 1 calc R . . H25C H 0.2203 0.3574 0.5519 0.143 Uiso 1 1 calc R . . N2 N 0.5750(9) 0.7042(6) 0.8197(4) 0.082(3) Uani 1 1 d . . . O15 O 0.4941(6) 0.7104(4) 0.8454(3) 0.077(2) Uani 1 1 d . . . O14 O 0.5288(5) 0.6836(5) 0.7705(3) 0.122(3) Uani 1 1 d . . . O3 O 0.1930(5) 0.4577(3) 0.8347(2) 0.0558(16) Uani 1 1 d . . . O1 O 0.3273(4) 0.5568(3) 0.7974(2) 0.0500(15) Uani 1 1 d . . . O2 O 0.2221(5) 0.4443(3) 0.7380(2) 0.0590(17) Uani 1 1 d . . . O18 O 0.0706(4) 0.6259(3) 0.7368(2) 0.0579(17) Uani 1 1 d . . . O17 O 0.0747(5) 0.7504(4) 0.7243(3) 0.080(2) Uani 1 1 d . . . C10 C 0.4036(7) 0.2839(5) 1.0031(4) 0.063(3) Uani 1 1 d . . . H10A H 0.3098 0.2879 0.9897 0.095 Uiso 1 1 calc R . . H10B H 0.4293 0.2945 1.0416 0.095 Uiso 1 1 calc R . . H10C H 0.4310 0.2315 0.9966 0.095 Uiso 1 1 calc R . . C11 C 0.3093(8) 0.2925(5) 0.8892(4) 0.075(3) Uani 1 1 d . . . H11A H 0.2266 0.3120 0.8926 0.112 Uiso 1 1 calc R . . H11B H 0.3253 0.2409 0.9054 0.112 Uiso 1 1 calc R . . H11C H 0.3072 0.2893 0.8513 0.112 Uiso 1 1 calc R . . C7 C 0.4221(6) 0.4076(4) 0.8276(3) 0.048(2) Uani 1 1 d . . . H7A H 0.3963 0.3548 0.8139 0.058 Uiso 1 1 calc R . . H7B H 0.4960 0.4229 0.8139 0.058 Uiso 1 1 calc R . . C12 C 0.1631(10) 0.3651(6) 0.7261(4) 0.104(4) Uani 1 1 d . . . H12A H 0.2253 0.3300 0.7159 0.125 Uiso 1 1 calc R . . H12B H 0.1445 0.3439 0.7587 0.125 Uiso 1 1 calc R . . C14 C 0.0627(8) 0.4937(6) 0.8253(4) 0.083(3) Uani 1 1 d . . . H14A H 0.0720 0.5479 0.8382 0.100 Uiso 1 1 calc R . . H14B H 0.0205 0.4946 0.7864 0.100 Uiso 1 1 calc R . . O6 O 0.7028(5) 0.2361(3) 1.0567(2) 0.0646(17) Uani 1 1 d . . . O5 O 0.8681(5) 0.3431(3) 1.0695(2) 0.0688(19) Uani 1 1 d . . . C18 C 0.9950(9) 0.3069(8) 1.0861(5) 0.129(5) Uani 1 1 d . . . H18A H 1.0360 0.3202 1.1239 0.155 Uiso 1 1 calc R . . H18B H 0.9849 0.2499 1.0836 0.155 Uiso 1 1 calc R . . O4 O 0.7815(4) 0.3033(3) 1.14890(19) 0.0480(14) Uani 1 1 d . . . O7 O 0.2816(5) 0.6432(3) 0.6829(2) 0.0577(16) Uani 1 1 d . . . O10 O 0.2072(5) 0.6727(3) 0.5810(2) 0.0657(18) Uani 1 1 d . . . O8 O 0.3881(6) 0.5784(4) 0.6160(3) 0.083(2) Uani 1 1 d . . . C26 C 0.2632(10) 0.7521(6) 0.5833(4) 0.090(4) Uani 1 1 d . . . H26A H 0.3385 0.7566 0.6149 0.108 Uiso 1 1 calc R . . H26B H 0.2924 0.7619 0.5508 0.108 Uiso 1 1 calc R . . C23 C 0.1373(7) 0.5358(5) 0.6140(3) 0.056(2) Uani 1 1 d . . . H23A H 0.1778 0.4874 0.6311 0.067 Uiso 1 1 calc R . . H23B H 0.0706 0.5507 0.6319 0.067 Uiso 1 1 calc R . . C24 C -0.1033(8) 0.6192(6) 0.5595(4) 0.087(4) Uani 1 1 d . . . H24A H -0.0419 0.6286 0.5943 0.131 Uiso 1 1 calc R . . H24B H -0.1846 0.6002 0.5649 0.131 Uiso 1 1 calc R . . H24C H -0.1187 0.6675 0.5390 0.131 Uiso 1 1 calc R . . C40 C 0.6219(6) 0.3847(4) 1.0632(3) 0.044(2) Uani 1 1 d . . . H40A H 0.5483 0.3726 1.0779 0.052 Uiso 1 1 calc R . . H40B H 0.6552 0.4361 1.0773 0.052 Uiso 1 1 calc R . . O16 O 0.6920(6) 0.7148(5) 0.8372(3) 0.146(4) Uani 1 1 d . . . O13 O 0.3365(7) 0.9303(4) 0.7429(4) 0.109(3) Uani 1 1 d . . . C16 C 0.7005(12) 0.1597(7) 1.0757(4) 0.110(4) Uani 1 1 d . . . H16A H 0.6308 0.1561 1.0939 0.132 Uiso 1 1 calc R . . H16B H 0.7827 0.1500 1.1029 0.132 Uiso 1 1 calc R . . C17 C 0.6822(17) 0.1003(7) 1.0370(6) 0.198(8) Uani 1 1 d . . . H17A H 0.6046 0.1111 1.0082 0.298 Uiso 1 1 calc R . . H17B H 0.6723 0.0505 1.0537 0.298 Uiso 1 1 calc R . . H17C H 0.7569 0.0979 1.0223 0.298 Uiso 1 1 calc R . . C19 C 1.0744(10) 0.3304(12) 1.0550(6) 0.217(10) Uani 1 1 d . . . H19A H 1.1423 0.2918 1.0573 0.326 Uiso 1 1 calc R . . H19B H 1.1134 0.3805 1.0680 0.326 Uiso 1 1 calc R . . H19C H 1.0238 0.3356 1.0177 0.326 Uiso 1 1 calc R . . C15 C -0.0158(10) 0.4525(8) 0.8517(6) 0.164(7) Uani 1 1 d . . . H15A H -0.0344 0.4009 0.8358 0.247 Uiso 1 1 calc R . . H15B H -0.0966 0.4807 0.8480 0.247 Uiso 1 1 calc R . . H15C H 0.0293 0.4474 0.8897 0.247 Uiso 1 1 calc R . . C27 C 0.1663(10) 0.8086(6) 0.5870(5) 0.110(4) Uani 1 1 d . . . H27A H 0.1014 0.8122 0.5525 0.166 Uiso 1 1 calc R . . H27B H 0.2070 0.8593 0.5964 0.166 Uiso 1 1 calc R . . H27C H 0.1249 0.7925 0.6146 0.166 Uiso 1 1 calc R . . C28 C 0.4958(11) 0.5477(9) 0.6564(6) 0.152(6) Uani 1 1 d . . . H28A H 0.4958 0.5699 0.6916 0.182 Uiso 1 1 calc R . . H28B H 0.4867 0.4908 0.6584 0.182 Uiso 1 1 calc R . . C13 C 0.0454(10) 0.3674(7) 0.6833(4) 0.140(6) Uani 1 1 d . . . H13A H -0.0192 0.3980 0.6946 0.209 Uiso 1 1 calc R . . H13B H 0.0133 0.3145 0.6748 0.209 Uiso 1 1 calc R . . H13C H 0.0625 0.3911 0.6516 0.209 Uiso 1 1 calc R . . N3 N 0.0113(7) 0.6871(5) 0.7194(3) 0.072(2) Uani 1 1 d . . . O19 O -0.1079(6) 0.6867(4) 0.6981(4) 0.139(4) Uani 1 1 d . . . C29 C 0.6120(12) 0.5651(9) 0.6451(7) 0.204(9) Uani 1 1 d . . . H29A H 0.6035 0.5569 0.6070 0.306 Uiso 1 1 calc R . . H29B H 0.6798 0.5312 0.6662 0.306 Uiso 1 1 calc R . . H29C H 0.6346 0.6193 0.6543 0.306 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 Eu1 0.0450(2) 0.0417(2) 0.0284(2) -0.0010(2) 0.00659(15) -0.00431(19) P2 0.0442(12) 0.0427(12) 0.0353(13) 0.0005(10) 0.0055(10) -0.0003(9) P3 0.0441(11) 0.0528(13) 0.0340(11) 0.0056(12) 0.0117(9) 0.0085(10) P4 0.0657(15) 0.0576(15) 0.0330(13) -0.0108(12) 0.0118(11) -0.0126(11) C1 0.039(4) 0.042(5) 0.044(5) 0.004(4) 0.005(4) 0.010(3) C4 0.036(4) 0.040(5) 0.041(5) 0.010(4) 0.008(4) 0.010(3) C2 0.039(4) 0.042(5) 0.045(5) 0.012(4) 0.011(4) 0.014(3) C8 0.048(5) 0.068(6) 0.061(6) 0.016(5) 0.013(4) 0.002(4) C6 0.043(4) 0.034(4) 0.055(6) 0.009(4) 0.004(4) -0.003(3) C9 0.053(5) 0.060(6) 0.052(6) -0.002(5) 0.002(4) -0.009(4) C5 0.039(4) 0.050(5) 0.040(5) 0.005(4) 0.013(4) 0.006(3) C3 0.038(4) 0.041(5) 0.043(5) 0.000(4) 0.008(4) 0.005(3) N1 0.080(5) 0.052(6) 0.083(7) 0.005(6) 0.032(5) -0.020(4) O12 0.154(6) 0.057(5) 0.074(5) -0.017(4) 0.061(5) -0.016(4) O11 0.157(6) 0.062(5) 0.087(5) -0.026(5) 0.078(5) -0.028(4) C20 0.061(5) 0.046(5) 0.038(5) -0.011(4) 0.013(4) -0.015(4) C21 0.062(5) 0.046(5) 0.050(6) -0.024(5) 0.021(4) -0.008(4) C22 0.055(5) 0.041(5) 0.061(6) -0.014(5) 0.019(4) -0.012(4) C25 0.097(7) 0.063(7) 0.103(9) -0.020(7) -0.016(6) 0.022(5) N2 0.075(7) 0.112(8) 0.046(5) 0.017(6) -0.006(5) -0.023(6) O15 0.060(4) 0.125(6) 0.043(4) 0.001(4) 0.010(3) -0.028(4) O14 0.043(4) 0.226(10) 0.099(6) 0.005(7) 0.024(4) -0.012(5) O3 0.051(3) 0.067(4) 0.054(4) 0.013(3) 0.023(3) 0.003(3) O1 0.040(3) 0.044(3) 0.061(4) 0.007(3) 0.005(2) 0.001(2) O2 0.075(3) 0.049(3) 0.045(4) -0.003(3) 0.001(3) -0.012(3) O18 0.044(3) 0.052(4) 0.070(4) 0.012(4) 0.003(3) 0.000(3) O17 0.071(4) 0.054(4) 0.106(6) 0.014(4) 0.009(4) 0.010(3) C10 0.056(5) 0.081(7) 0.055(6) 0.019(5) 0.016(4) -0.010(4) C11 0.093(6) 0.053(6) 0.064(6) 0.008(5) -0.004(5) -0.021(5) C7 0.053(5) 0.040(5) 0.049(5) -0.005(4) 0.010(4) 0.010(4) C12 0.143(9) 0.070(8) 0.075(8) -0.003(7) -0.014(7) -0.040(6) C14 0.065(6) 0.112(9) 0.082(8) 0.009(8) 0.035(6) 0.010(6) O6 0.098(4) 0.053(4) 0.039(4) -0.002(3) 0.011(3) 0.017(3) O5 0.039(3) 0.106(5) 0.070(4) 0.041(4) 0.028(3) 0.021(3) C18 0.056(7) 0.200(13) 0.140(12) 0.102(12) 0.041(7) 0.029(8) O4 0.045(3) 0.060(4) 0.037(3) 0.002(3) 0.008(2) 0.007(2) O7 0.064(3) 0.059(4) 0.047(4) -0.012(3) 0.010(3) -0.007(3) O10 0.095(4) 0.059(4) 0.038(3) -0.002(3) 0.009(3) -0.029(3) O8 0.074(4) 0.109(6) 0.070(5) -0.018(5) 0.028(4) 0.006(4) C26 0.135(9) 0.073(8) 0.059(7) -0.007(7) 0.021(7) -0.042(7) C23 0.072(5) 0.056(6) 0.045(5) -0.012(5) 0.027(4) -0.010(4) C24 0.078(6) 0.098(8) 0.093(8) -0.051(7) 0.033(6) -0.004(5) C40 0.039(4) 0.043(5) 0.051(5) -0.007(4) 0.015(4) 0.005(3) O16 0.043(4) 0.257(11) 0.116(7) 0.040(7) -0.017(4) -0.045(5) O13 0.171(7) 0.048(4) 0.134(7) 0.005(6) 0.086(6) -0.012(4) C16 0.193(11) 0.073(8) 0.048(7) 0.007(7) 0.005(7) -0.002(8) C17 0.44(2) 0.070(10) 0.096(11) -0.030(10) 0.096(14) 0.018(12) C19 0.061(8) 0.47(3) 0.125(12) 0.032(18) 0.027(8) -0.001(12) C15 0.089(9) 0.231(16) 0.199(16) 0.000(16) 0.081(10) -0.045(9) C27 0.133(10) 0.065(8) 0.132(11) 0.007(10) 0.033(8) -0.002(7) C28 0.078(9) 0.243(18) 0.130(13) -0.018(13) 0.024(9) 0.047(10) C13 0.161(10) 0.158(12) 0.076(8) 0.006(9) -0.011(8) -0.109(9) N3 0.052(5) 0.070(6) 0.084(6) 0.017(6) -0.002(4) 0.007(5) O19 0.052(4) 0.123(6) 0.212(9) 0.039(7) -0.017(5) 0.014(4) C29 0.098(10) 0.239(18) 0.28(2) 0.127(18) 0.053(12) -0.020(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O7 2.322(6) . ? Eu1 O1 2.371(5) . ? Eu1 O4 2.396(5) 3_667 ? Eu1 O17 2.482(5) . ? Eu1 O15 2.494(5) . ? Eu1 O11 2.495(7) . ? Eu1 O18 2.505(5) . ? Eu1 O12 2.508(6) . ? Eu1 O14 2.508(6) . ? P2 O1 1.481(5) . ? P2 O3 1.572(6) . ? P2 O2 1.575(5) . ? P2 C7 1.785(6) . ? P3 O4 1.467(5) . ? P3 O6 1.549(6) . ? P3 O5 1.567(6) . ? P3 C40 1.796(7) . ? P4 O7 1.476(6) . ? P4 O10 1.556(6) . ? P4 O8 1.559(7) . ? P4 C23 1.783(7) . ? C1 C6 1.386(10) . ? C1 C2 1.427(9) . ? C1 C7 1.500(10) . ? C4 C3 1.383(10) . ? C4 C5 1.413(9) . ? C4 C40 1.497(10) . ? C2 C3 1.414(10) . ? C2 C8 1.507(10) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C6 C5 1.388(10) . ? C6 C11 1.520(9) . ? C9 C3 1.563(9) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C5 C10 1.486(10) . ? N1 O13 1.242(9) . ? N1 O11 1.251(10) . ? N1 O12 1.280(10) . ? C20 C22 1.381(11) . ? C20 C21 1.397(10) . ? C20 C23 1.555(10) . ? C21 C22 1.391(10) 3_566 ? C21 C24 1.511(11) . ? C22 C21 1.391(10) 3_566 ? C22 C25 1.534(10) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? N2 O16 1.210(9) . ? N2 O15 1.210(10) . ? N2 O14 1.264(10) . ? O3 C14 1.465(9) . ? O2 C12 1.474(10) . ? O18 N3 1.229(8) . ? O17 N3 1.251(8) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C12 C13 1.416(11) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C15 1.386(14) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? O6 C16 1.382(11) . ? O5 C18 1.430(10) . ? C18 C19 1.356(15) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? O4 Eu1 2.396(5) 3_667 ? O10 C26 1.462(10) . ? O8 C28 1.412(11) . ? C26 C27 1.422(13) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C16 C17 1.384(13) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.365(14) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? N3 O19 1.230(7) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Eu1 O1 85.17(19) . . ? O7 Eu1 O4 153.23(18) . 3_667 ? O1 Eu1 O4 81.13(19) . 3_667 ? O7 Eu1 O17 84.2(2) . . ? O1 Eu1 O17 125.59(18) . . ? O4 Eu1 O17 85.2(2) 3_667 . ? O7 Eu1 O15 126.2(2) . . ? O1 Eu1 O15 81.93(19) . . ? O4 Eu1 O15 74.53(19) 3_667 . ? O17 Eu1 O15 143.1(2) . . ? O7 Eu1 O11 75.1(2) . . ? O1 Eu1 O11 151.3(2) . . ? O4 Eu1 O11 124.9(2) 3_667 . ? O17 Eu1 O11 73.5(2) . . ? O15 Eu1 O11 93.0(2) . . ? O7 Eu1 O18 74.51(19) . . ? O1 Eu1 O18 75.18(16) . . ? O4 Eu1 O18 79.79(17) 3_667 . ? O17 Eu1 O18 50.57(18) . . ? O15 Eu1 O18 147.8(2) . . ? O11 Eu1 O18 117.8(2) . . ? O7 Eu1 O12 125.2(2) . . ? O1 Eu1 O12 148.2(2) . . ? O4 Eu1 O12 74.1(2) 3_667 . ? O17 Eu1 O12 72.4(2) . . ? O15 Eu1 O12 72.5(2) . . ? O11 Eu1 O12 51.2(2) . . ? O18 Eu1 O12 118.6(2) . . ? O7 Eu1 O14 77.4(2) . . ? O1 Eu1 O14 82.5(2) . . ? O4 Eu1 O14 123.0(2) 3_667 . ? O17 Eu1 O14 145.0(3) . . ? O15 Eu1 O14 49.2(2) . . ? O11 Eu1 O14 73.1(3) . . ? O18 Eu1 O14 145.3(2) . . ? O12 Eu1 O14 94.3(3) . . ? O1 P2 O3 112.4(3) . . ? O1 P2 O2 109.7(3) . . ? O3 P2 O2 109.5(3) . . ? O1 P2 C7 114.2(3) . . ? O3 P2 C7 102.1(4) . . ? O2 P2 C7 108.6(3) . . ? O4 P3 O6 114.5(4) . . ? O4 P3 O5 112.2(3) . . ? O6 P3 O5 105.2(4) . . ? O4 P3 C40 114.0(3) . . ? O6 P3 C40 105.8(3) . . ? O5 P3 C40 104.2(3) . . ? O7 P4 O10 114.3(3) . . ? O7 P4 O8 112.7(3) . . ? O10 P4 O8 104.7(4) . . ? O7 P4 C23 111.2(4) . . ? O10 P4 C23 103.9(3) . . ? O8 P4 C23 109.5(4) . . ? C6 C1 C2 120.1(7) . . ? C6 C1 C7 121.7(7) . . ? C2 C1 C7 118.2(8) . . ? C3 C4 C5 118.9(7) . . ? C3 C4 C40 121.5(7) . . ? C5 C4 C40 119.6(7) . . ? C3 C2 C1 117.5(8) . . ? C3 C2 C8 121.8(7) . . ? C1 C2 C8 120.8(7) . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C1 C6 C5 121.3(7) . . ? C1 C6 C11 120.3(7) . . ? C5 C6 C11 118.4(8) . . ? C3 C9 H9A 109.5 . . ? C3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C5 C4 119.9(8) . . ? C6 C5 C10 117.8(7) . . ? C4 C5 C10 122.3(7) . . ? C4 C3 C2 122.3(7) . . ? C4 C3 C9 121.0(6) . . ? C2 C3 C9 116.7(7) . . ? O13 N1 O11 120.2(10) . . ? O13 N1 O12 122.6(10) . . ? O11 N1 O12 117.2(8) . . ? N1 O12 Eu1 95.1(6) . . ? N1 O11 Eu1 96.5(6) . . ? C22 C20 C21 120.8(7) . . ? C22 C20 C23 121.0(8) . . ? C21 C20 C23 118.1(8) . . ? C22 C21 C20 119.7(8) 3_566 . ? C22 C21 C24 119.1(8) 3_566 . ? C20 C21 C24 121.2(7) . . ? C20 C22 C21 119.5(8) . 3_566 ? C20 C22 C25 120.7(7) . . ? C21 C22 C25 119.7(8) 3_566 . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O16 N2 O15 126.0(9) . . ? O16 N2 O14 119.4(11) . . ? O15 N2 O14 114.6(8) . . ? N2 O15 Eu1 99.0(6) . . ? N2 O14 Eu1 96.7(7) . . ? C14 O3 P2 124.2(6) . . ? P2 O1 Eu1 153.8(3) . . ? C12 O2 P2 122.1(6) . . ? N3 O18 Eu1 95.2(5) . . ? N3 O17 Eu1 95.8(5) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C7 P2 118.8(6) . . ? C1 C7 H7A 107.6 . . ? P2 C7 H7A 107.6 . . ? C1 C7 H7B 107.6 . . ? P2 C7 H7B 107.6 . . ? H7A C7 H7B 107.1 . . ? C13 C12 O2 111.6(9) . . ? C13 C12 H12A 109.3 . . ? O2 C12 H12A 109.3 . . ? C13 C12 H12B 109.3 . . ? O2 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C15 C14 O3 111.6(10) . . ? C15 C14 H14A 109.3 . . ? O3 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? O3 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C16 O6 P3 128.9(6) . . ? C18 O5 P3 122.6(6) . . ? C19 C18 O5 112.3(11) . . ? C19 C18 H18A 109.1 . . ? O5 C18 H18A 109.1 . . ? C19 C18 H18B 109.1 . . ? O5 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? P3 O4 Eu1 147.5(3) . 3_667 ? P4 O7 Eu1 173.6(3) . . ? C26 O10 P4 121.6(5) . . ? C28 O8 P4 124.6(7) . . ? C27 C26 O10 109.2(9) . . ? C27 C26 H26A 109.8 . . ? O10 C26 H26A 109.8 . . ? C27 C26 H26B 109.8 . . ? O10 C26 H26B 109.8 . . ? H26A C26 H26B 108.3 . . ? C20 C23 P4 117.6(6) . . ? C20 C23 H23A 107.9 . . ? P4 C23 H23A 107.9 . . ? C20 C23 H23B 107.9 . . ? P4 C23 H23B 107.9 . . ? H23A C23 H23B 107.2 . . ? 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 . . ? C4 C40 P3 117.4(6) . . ? C4 C40 H40A 107.9 . . ? P3 C40 H40A 107.9 . . ? C4 C40 H40B 107.9 . . ? P3 C40 H40B 107.9 . . ? H40A C40 H40B 107.2 . . ? O6 C16 C17 116.3(10) . . ? O6 C16 H16A 108.2 . . ? C17 C16 H16A 108.2 . . ? O6 C16 H16B 108.2 . . ? C17 C16 H16B 108.2 . . ? H16A C16 H16B 107.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 O8 111.4(14) . . ? C29 C28 H28A 109.4 . . ? O8 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? O8 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O18 N3 O19 121.1(8) . . ? O18 N3 O17 118.4(7) . . ? O19 N3 O17 120.4(8) . . ? 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 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.0(11) . . . . ? C7 C1 C2 C3 -177.5(7) . . . . ? C6 C1 C2 C8 179.5(7) . . . . ? C7 C1 C2 C8 2.0(11) . . . . ? C2 C1 C6 C5 0.4(12) . . . . ? C7 C1 C6 C5 177.8(8) . . . . ? C2 C1 C6 C11 -178.2(7) . . . . ? C7 C1 C6 C11 -0.8(12) . . . . ? C1 C6 C5 C4 -0.8(12) . . . . ? C11 C6 C5 C4 177.8(7) . . . . ? C1 C6 C5 C10 178.6(7) . . . . ? C11 C6 C5 C10 -2.8(12) . . . . ? C3 C4 C5 C6 0.8(11) . . . . ? C40 C4 C5 C6 179.7(7) . . . . ? C3 C4 C5 C10 -178.6(8) . . . . ? C40 C4 C5 C10 0.4(11) . . . . ? C5 C4 C3 C2 -0.4(11) . . . . ? C40 C4 C3 C2 -179.4(7) . . . . ? C5 C4 C3 C9 -178.3(7) . . . . ? C40 C4 C3 C9 2.8(11) . . . . ? C1 C2 C3 C4 0.0(12) . . . . ? C8 C2 C3 C4 -179.5(7) . . . . ? C1 C2 C3 C9 178.0(6) . . . . ? C8 C2 C3 C9 -1.6(11) . . . . ? O13 N1 O12 Eu1 177.8(7) . . . . ? O11 N1 O12 Eu1 -1.6(9) . . . . ? O7 Eu1 O12 N1 -12.5(6) . . . . ? O1 Eu1 O12 N1 147.8(5) . . . . ? O4 Eu1 O12 N1 -171.8(6) 3_667 . . . ? O17 Eu1 O12 N1 -81.8(5) . . . . ? O15 Eu1 O12 N1 109.8(6) . . . . ? O11 Eu1 O12 N1 0.9(5) . . . . ? O18 Eu1 O12 N1 -103.2(5) . . . . ? O14 Eu1 O12 N1 65.1(6) . . . . ? O13 N1 O11 Eu1 -177.8(7) . . . . ? O12 N1 O11 Eu1 1.6(9) . . . . ? O7 Eu1 O11 N1 167.8(6) . . . . ? O1 Eu1 O11 N1 -144.2(5) . . . . ? O4 Eu1 O11 N1 7.6(6) 3_667 . . . ? O17 Eu1 O11 N1 79.5(5) . . . . ? O15 Eu1 O11 N1 -65.6(5) . . . . ? O18 Eu1 O11 N1 104.7(5) . . . . ? O12 Eu1 O11 N1 -0.9(5) . . . . ? O14 Eu1 O11 N1 -111.1(6) . . . . ? C22 C20 C21 C22 0.3(15) . . . 3_566 ? C23 C20 C21 C22 -178.0(7) . . . 3_566 ? C22 C20 C21 C24 178.0(8) . . . . ? C23 C20 C21 C24 -0.3(12) . . . . ? C21 C20 C22 C21 -0.3(15) . . . 3_566 ? C23 C20 C22 C21 178.0(7) . . . 3_566 ? C21 C20 C22 C25 -178.8(8) . . . . ? C23 C20 C22 C25 -0.5(13) . . . . ? O16 N2 O15 Eu1 174.4(9) . . . . ? O14 N2 O15 Eu1 -6.8(11) . . . . ? O7 Eu1 O15 N2 13.2(8) . . . . ? O1 Eu1 O15 N2 91.2(7) . . . . ? O4 Eu1 O15 N2 174.2(7) 3_667 . . . ? O17 Eu1 O15 N2 -126.6(7) . . . . ? O11 Eu1 O15 N2 -60.4(7) . . . . ? O18 Eu1 O15 N2 135.9(6) . . . . ? O12 Eu1 O15 N2 -108.0(7) . . . . ? O14 Eu1 O15 N2 4.1(7) . . . . ? O16 N2 O14 Eu1 -174.4(8) . . . . ? O15 N2 O14 Eu1 6.7(11) . . . . ? O7 Eu1 O14 N2 -176.3(7) . . . . ? O1 Eu1 O14 N2 -89.6(7) . . . . ? O4 Eu1 O14 N2 -15.3(8) 3_667 . . . ? O17 Eu1 O14 N2 123.6(6) . . . . ? O15 Eu1 O14 N2 -3.9(6) . . . . ? O11 Eu1 O14 N2 105.7(7) . . . . ? O18 Eu1 O14 N2 -139.7(6) . . . . ? O12 Eu1 O14 N2 58.5(7) . . . . ? O1 P2 O3 C14 61.2(7) . . . . ? O2 P2 O3 C14 -60.9(7) . . . . ? C7 P2 O3 C14 -175.9(7) . . . . ? O3 P2 O1 Eu1 -77.2(9) . . . . ? O2 P2 O1 Eu1 44.8(9) . . . . ? C7 P2 O1 Eu1 167.0(7) . . . . ? O7 Eu1 O1 P2 -64.4(8) . . . . ? O4 Eu1 O1 P2 92.5(8) 3_667 . . . ? O17 Eu1 O1 P2 14.9(10) . . . . ? O15 Eu1 O1 P2 168.0(9) . . . . ? O11 Eu1 O1 P2 -110.6(8) . . . . ? O18 Eu1 O1 P2 10.8(8) . . . . ? O12 Eu1 O1 P2 131.6(8) . . . . ? O14 Eu1 O1 P2 -142.3(9) . . . . ? O1 P2 O2 C12 -174.5(7) . . . . ? O3 P2 O2 C12 -50.7(8) . . . . ? C7 P2 O2 C12 60.1(8) . . . . ? O7 Eu1 O18 N3 -95.0(5) . . . . ? O1 Eu1 O18 N3 176.0(6) . . . . ? O4 Eu1 O18 N3 92.5(5) 3_667 . . . ? O17 Eu1 O18 N3 0.3(5) . . . . ? O15 Eu1 O18 N3 129.8(6) . . . . ? O11 Eu1 O18 N3 -31.7(6) . . . . ? O12 Eu1 O18 N3 27.0(6) . . . . ? O14 Eu1 O18 N3 -132.2(6) . . . . ? O7 Eu1 O17 N3 74.4(6) . . . . ? O1 Eu1 O17 N3 -5.5(7) . . . . ? O4 Eu1 O17 N3 -81.0(6) 3_667 . . . ? O15 Eu1 O17 N3 -137.2(6) . . . . ? O11 Eu1 O17 N3 150.5(7) . . . . ? O18 Eu1 O17 N3 -0.3(5) . . . . ? O12 Eu1 O17 N3 -155.8(7) . . . . ? O14 Eu1 O17 N3 132.6(6) . . . . ? C6 C1 C7 P2 90.3(9) . . . . ? C2 C1 C7 P2 -92.2(8) . . . . ? O1 P2 C7 C1 79.2(8) . . . . ? O3 P2 C7 C1 -42.5(7) . . . . ? O2 P2 C7 C1 -158.1(6) . . . . ? P2 O2 C12 C13 141.2(8) . . . . ? P2 O3 C14 C15 160.7(9) . . . . ? O4 P3 O6 C16 -6.4(10) . . . . ? O5 P3 O6 C16 117.3(9) . . . . ? C40 P3 O6 C16 -132.8(9) . . . . ? O4 P3 O5 C18 50.0(9) . . . . ? O6 P3 O5 C18 -75.1(8) . . . . ? C40 P3 O5 C18 173.8(8) . . . . ? P3 O5 C18 C19 166.1(11) . . . . ? O6 P3 O4 Eu1 -92.9(7) . . . 3_667 ? O5 P3 O4 Eu1 147.3(5) . . . 3_667 ? C40 P3 O4 Eu1 29.2(8) . . . 3_667 ? O10 P4 O7 Eu1 85(3) . . . . ? O8 P4 O7 Eu1 -155(3) . . . . ? C23 P4 O7 Eu1 -32(3) . . . . ? O1 Eu1 O7 P4 86(3) . . . . ? O4 Eu1 O7 P4 26(3) 3_667 . . . ? O17 Eu1 O7 P4 -41(3) . . . . ? O15 Eu1 O7 P4 162(3) . . . . ? O11 Eu1 O7 P4 -115(3) . . . . ? O18 Eu1 O7 P4 10(3) . . . . ? O12 Eu1 O7 P4 -105(3) . . . . ? O14 Eu1 O7 P4 169(3) . . . . ? O7 P4 O10 C26 45.0(8) . . . . ? O8 P4 O10 C26 -78.8(8) . . . . ? C23 P4 O10 C26 166.4(8) . . . . ? O7 P4 O8 C28 27.8(10) . . . . ? O10 P4 O8 C28 152.6(9) . . . . ? C23 P4 O8 C28 -96.5(10) . . . . ? P4 O10 C26 C27 -115.5(9) . . . . ? C22 C20 C23 P4 91.0(9) . . . . ? C21 C20 C23 P4 -90.7(9) . . . . ? O7 P4 C23 C20 158.8(6) . . . . ? O10 P4 C23 C20 35.4(8) . . . . ? O8 P4 C23 C20 -76.0(7) . . . . ? C3 C4 C40 P3 -93.5(8) . . . . ? C5 C4 C40 P3 87.6(8) . . . . ? O4 P3 C40 C4 -172.9(6) . . . . ? O6 P3 C40 C4 -46.2(7) . . . . ? O5 P3 C40 C4 64.4(7) . . . . ? P3 O6 C16 C17 -166.3(10) . . . . ? P4 O8 C28 C29 -145.2(11) . . . . ? Eu1 O18 N3 O19 -179.7(8) . . . . ? Eu1 O18 N3 O17 -0.5(9) . . . . ? Eu1 O17 N3 O18 0.5(10) . . . . ? Eu1 O17 N3 O19 179.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.511 _refine_diff_density_min -1.461 _refine_diff_density_rms 0.130 data_Nd #TrackingRef '- SI-cif.txt' _database_code_depnum_ccdc_archive 'CCDC 793771' #TrackingRef '- Nd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H54 N3 Nd O18 P3' _chemical_formula_weight 981.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 10.5749(9) _cell_length_b 16.9082(13) _cell_length_c 24.7932(19) _cell_angle_alpha 90.00 _cell_angle_beta 98.655(4) _cell_angle_gamma 90.00 _cell_volume 4382.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6772 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 26.14 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 1.365 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7533 _exptl_absorpt_correction_T_max 0.8112 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23830 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8146 _reflns_number_gt 6262 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for O8 The larger than normal range of thermal motion is mostly due to the difference between the disordered group and the Nd atom which is not disordered. ; _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^)+(0.0366P)^2^+1.4166P] 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 8146 _refine_ls_number_parameters 544 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C30A C 0.9805(9) 0.0480(12) 0.3617(8) 0.121(6) Uani 0.51(2) 1 d PDU A 1 C16A C 0.387(3) 0.4020(9) 0.0365(7) 0.111(6) Uani 0.55(4) 1 d PD B 1 C1 C 0.4309(3) 0.10918(19) 0.00122(13) 0.0423(8) Uani 1 1 d . . . C2 C 0.5083(3) 0.1579(2) -0.02555(14) 0.0472(8) Uani 1 1 d . . . C3 C 0.4999(3) 0.1530(2) -0.08247(14) 0.0501(9) Uani 1 1 d . . . C4 C 0.4170(3) 0.09792(19) -0.11135(13) 0.0455(8) Uani 1 1 d . . . C5 C 0.3425(3) 0.04790(19) -0.08444(13) 0.0433(8) Uani 1 1 d . . . C6 C 0.3479(3) 0.05445(18) -0.02760(13) 0.0425(8) Uani 1 1 d . . . C7 C 0.4393(3) 0.1157(2) 0.06297(13) 0.0491(8) Uani 1 1 d . . . H7A H 0.5273 0.1273 0.0781 0.059 Uiso 1 1 calc R . . H7B H 0.4187 0.0644 0.0769 0.059 Uiso 1 1 calc R . . C8 C 0.6026(4) 0.2155(2) 0.00446(17) 0.0670(11) Uani 1 1 d . . . H8A H 0.6045 0.2092 0.0431 0.101 Uiso 1 1 calc R . . H8B H 0.5772 0.2685 -0.0059 0.101 Uiso 1 1 calc R . . H8C H 0.6862 0.2054 -0.0047 0.101 Uiso 1 1 calc R . . C9 C 0.5808(5) 0.2079(2) -0.11136(18) 0.0820(14) Uani 1 1 d . . . H9A H 0.6673 0.1889 -0.1067 0.123 Uiso 1 1 calc R . . H9B H 0.5791 0.2601 -0.0962 0.123 Uiso 1 1 calc R . . H9C H 0.5473 0.2096 -0.1495 0.123 Uiso 1 1 calc R . . C10 C 0.4048(4) 0.0947(2) -0.17353(13) 0.0526(9) Uani 1 1 d . . . H10A H 0.4184 0.1476 -0.1866 0.063 Uiso 1 1 calc R . . H10B H 0.3176 0.0798 -0.1879 0.063 Uiso 1 1 calc R . . C11 C 0.2539(4) -0.0115(2) -0.11577(15) 0.0609(10) Uani 1 1 d . . . H11A H 0.1696 0.0106 -0.1238 0.091 Uiso 1 1 calc R . . H11B H 0.2513 -0.0585 -0.0943 0.091 Uiso 1 1 calc R . . H11C H 0.2845 -0.0244 -0.1492 0.091 Uiso 1 1 calc R . . C12 C 0.2644(4) 0.0012(2) 0.00148(16) 0.0624(10) Uani 1 1 d . . . H12A H 0.2857 -0.0531 -0.0041 0.094 Uiso 1 1 calc R . . H12B H 0.1761 0.0101 -0.0129 0.094 Uiso 1 1 calc R . . H12C H 0.2786 0.0129 0.0398 0.094 Uiso 1 1 calc R . . C15 C 0.3778(7) 0.3405(3) 0.0769(2) 0.116(2) Uani 1 1 d D . . C17 C 0.5692(6) 0.1357(3) -0.2722(2) 0.1002(17) Uani 1 1 d . . . H17A H 0.4989 0.1718 -0.2833 0.120 Uiso 1 1 calc R . . H17B H 0.6190 0.1562 -0.2391 0.120 Uiso 1 1 calc R . . C18 C 0.6491(7) 0.1309(4) -0.3146(2) 0.146(3) Uani 1 1 d . . . H18A H 0.7094 0.0885 -0.3066 0.219 Uiso 1 1 calc R . . H18B H 0.6941 0.1799 -0.3164 0.219 Uiso 1 1 calc R . . H18C H 0.5965 0.1210 -0.3490 0.219 Uiso 1 1 calc R . . C19 C 0.7602(4) 0.0075(3) -0.1765(2) 0.0966(16) Uani 1 1 d U . . H19A H 0.7627 -0.0469 -0.1639 0.116 Uiso 1 1 calc R . . H19B H 0.7629 0.0071 -0.2154 0.116 Uiso 1 1 calc R . . C20 C 0.8645(6) 0.0472(5) -0.1503(3) 0.168(3) Uani 1 1 d U . . H20A H 0.8652 0.1000 -0.1645 0.252 Uiso 1 1 calc R . . H20B H 0.9411 0.0202 -0.1561 0.252 Uiso 1 1 calc R . . H20C H 0.8602 0.0493 -0.1119 0.252 Uiso 1 1 calc R . . C21 C 0.5129(4) 0.0169(2) 0.44607(14) 0.0530(9) Uani 1 1 d . . . C22 C 0.5902(4) -0.0409(2) 0.47446(16) 0.0574(10) Uani 1 1 d . . . C23 C 0.4238(4) 0.0583(2) 0.47129(15) 0.0565(9) Uani 1 1 d . . . C24 C 0.5246(4) 0.0356(2) 0.38699(14) 0.0640(11) Uani 1 1 d . A . H24A H 0.4404 0.0505 0.3686 0.077 Uiso 1 1 calc R . . H24B H 0.5482 -0.0128 0.3701 0.077 Uiso 1 1 calc R . . C25 C 0.6880(5) -0.0856(3) 0.4473(2) 0.0961(16) Uani 1 1 d . . . H25A H 0.6914 -0.0634 0.4119 0.144 Uiso 1 1 calc R . . H25B H 0.6638 -0.1402 0.4435 0.144 Uiso 1 1 calc R . . H25C H 0.7706 -0.0813 0.4693 0.144 Uiso 1 1 calc R . . C26 C 0.3379(5) 0.1209(3) 0.4413(2) 0.0914(15) Uani 1 1 d . . . H26A H 0.3654 0.1319 0.4069 0.137 Uiso 1 1 calc R . . H26B H 0.3427 0.1683 0.4628 0.137 Uiso 1 1 calc R . . H26C H 0.2512 0.1021 0.4352 0.137 Uiso 1 1 calc R . . C27 C 0.6813(5) 0.2517(3) 0.41632(19) 0.0882(16) Uani 1 1 d . . . H27A H 0.7432 0.2625 0.4485 0.106 Uiso 1 1 calc R . . H27B H 0.7242 0.2557 0.3845 0.106 Uiso 1 1 calc R . . C28 C 0.5775(7) 0.3089(3) 0.4124(3) 0.115(2) Uani 1 1 d . . . H28A H 0.5244 0.3037 0.3776 0.172 Uiso 1 1 calc R . . H28B H 0.6123 0.3614 0.4160 0.172 Uiso 1 1 calc R . . H28C H 0.5273 0.2993 0.4409 0.172 Uiso 1 1 calc R . . C29 C 0.8389(6) 0.0453(5) 0.3439(3) 0.139(3) Uani 1 1 d D . . C13A C 0.0795(19) 0.1656(14) 0.0900(10) 0.070(8) Uani 0.268(15) 1 d PDU C 1 C14A C 0.003(2) 0.2288(16) 0.0555(9) 0.126(13) Uani 0.268(15) 1 d PDU C 1 H13A H 0.0884 0.1775 0.1272 0.152 Uiso 0.268(15) 1 d PR C 1 H13B H 0.0274 0.1145 0.0842 0.152 Uiso 0.268(15) 1 d PR C 1 H14A H -0.0726 0.2355 0.0662 0.152 Uiso 0.268(15) 1 d PR C 1 H14B H -0.0026 0.2135 0.0172 0.152 Uiso 0.268(15) 1 d PR C 1 H14C H 0.0504 0.2765 0.0602 0.152 Uiso 0.268(15) 1 d PR C 1 H15A H 0.3284 0.3615 0.1022 0.152 Uiso 0.55(4) 1 d PR B 1 H15B H 0.4744 0.3475 0.1002 0.152 Uiso 0.55(4) 1 d PR B 1 H16A H 0.4032 0.4507 0.0553 0.152 Uiso 0.55(4) 1 d PR B 1 H16B H 0.3002 0.4027 0.0163 0.152 Uiso 0.55(4) 1 d PR B 1 H16C H 0.4462 0.3887 0.0153 0.152 Uiso 0.55(4) 1 d PR B 1 H29A H 0.8044 0.0075 0.3292 0.152 Uiso 0.51(2) 1 d PR A 1 H29B H 0.8554 0.0905 0.3172 0.152 Uiso 0.51(2) 1 d PR A 1 H30A H 1.0312 -0.0029 0.3470 0.152 Uiso 0.51(2) 1 d PR A 1 H30B H 1.0212 0.0661 0.3870 0.152 Uiso 0.51(2) 1 d PR A 1 H30C H 0.9562 -0.0129 0.3970 0.152 Uiso 0.51(2) 1 d PR A 1 C13B C 0.0937(8) 0.1987(8) 0.0842(6) 0.103(5) Uani 0.732(15) 1 d PDU C 2 C14B C -0.0226(7) 0.1567(7) 0.0561(4) 0.117(4) Uani 0.732(15) 1 d PDU C 2 H13C H 0.0907 0.2533 0.0732 0.140 Uiso 0.732(15) 1 d PR C 2 H13D H 0.0957 0.1973 0.1232 0.140 Uiso 0.732(15) 1 d PR C 2 H14D H -0.0103 0.1023 0.0682 0.140 Uiso 0.732(15) 1 d PR C 2 H14E H -0.0203 0.1583 0.0172 0.140 Uiso 0.732(15) 1 d PR C 2 H14F H -0.0903 0.1803 0.0652 0.140 Uiso 0.732(15) 1 d PR C 2 C16B C 0.307(4) 0.3998(11) 0.0436(11) 0.119(9) Uani 0.45(4) 1 d PD B 2 H15C H 0.3835 0.3439 0.1115 0.143 Uiso 0.45(4) 1 d PR B 2 H15D H 0.4805 0.3559 0.0705 0.143 Uiso 0.45(4) 1 d PR B 2 H16D H 0.3196 0.4499 0.0560 0.143 Uiso 0.45(4) 1 d PR B 2 H16E H 0.2146 0.3839 0.0420 0.143 Uiso 0.45(4) 1 d PR B 2 H16F H 0.3186 0.3969 0.0040 0.143 Uiso 0.45(4) 1 d PR B 2 C30B C 0.9562(16) 0.0885(13) 0.3372(8) 0.145(7) Uani 0.49(2) 1 d PDU A 2 H29C H 0.7800 0.0850 0.3074 0.174 Uiso 0.49(2) 1 d PR A 2 H29D H 0.8160 0.0130 0.3334 0.174 Uiso 0.49(2) 1 d PR A 2 H30D H 0.9493 0.1465 0.3334 0.174 Uiso 0.49(2) 1 d PR A 2 H30E H 1.0003 0.0765 0.3734 0.174 Uiso 0.49(2) 1 d PR A 2 H30F H 0.9983 0.0675 0.3104 0.174 Uiso 0.49(2) 1 d PR A 2 N1 N 0.7572(4) 0.2054(3) 0.18096(18) 0.0915(13) Uani 1 1 d . . . N2 N 0.5733(4) 0.3622(2) 0.24799(15) 0.0735(10) Uani 1 1 d . . . N3 N 0.2856(4) 0.1867(2) 0.28053(15) 0.0708(10) Uani 1 1 d . . . Nd1 Nd 0.521119(18) 0.190805(11) 0.230394(7) 0.04350(7) Uani 1 1 d . . . O1 O 0.3667(2) 0.19754(13) 0.14827(9) 0.0521(6) Uani 1 1 d . . . O2 O 0.2018(2) 0.15697(18) 0.06850(11) 0.0742(8) Uani 1 1 d D . . O3 O 0.3525(3) 0.26514(16) 0.05604(10) 0.0714(8) Uani 1 1 d . B . O4 O 0.4703(2) -0.05457(13) -0.20313(9) 0.0530(6) Uani 1 1 d . . . O5 O 0.6416(2) 0.04449(16) -0.16609(11) 0.0651(7) Uani 1 1 d . . . O6 O 0.5179(3) 0.05677(15) -0.26117(9) 0.0624(7) Uani 1 1 d . . . O7 O 0.6512(3) 0.2105(2) 0.15391(12) 0.0858(10) Uani 1 1 d . . . O8 O 0.7600(3) 0.1863(3) 0.22931(16) 0.1359(18) Uani 1 1 d . . . O9 O 0.8537(4) 0.2172(4) 0.16167(19) 0.168(2) Uani 1 1 d . . . O10 O 0.5037(4) 0.33738(18) 0.20609(13) 0.0980(11) Uani 1 1 d . . . O11 O 0.6190(4) 0.31140(18) 0.28055(14) 0.1004(12) Uani 1 1 d . . . O12 O 0.5931(4) 0.43178(18) 0.25572(16) 0.1200(14) Uani 1 1 d . . . O13 O 0.3455(3) 0.24966(18) 0.27561(14) 0.0866(10) Uani 1 1 d . . . O14 O 0.3315(3) 0.12501(16) 0.26368(12) 0.0710(8) Uani 1 1 d . . . O15 O 0.1895(4) 0.1846(2) 0.3013(2) 0.1409(18) Uani 1 1 d . . . O16 O 0.6037(2) 0.14263(15) 0.31814(9) 0.0619(7) Uani 1 1 d . A . O17 O 0.7732(3) 0.0779(2) 0.38558(12) 0.0884(9) Uani 1 1 d . A . O18 O 0.6289(3) 0.17240(15) 0.41972(10) 0.0739(8) Uani 1 1 d . A . P1 P 0.34015(9) 0.18744(5) 0.08822(4) 0.0464(2) Uani 1 1 d . B . P2 P 0.50993(9) 0.02907(5) -0.20157(3) 0.0463(2) Uani 1 1 d . . . P3 P 0.63427(10) 0.11066(6) 0.37371(4) 0.0570(3) 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 C30A 0.102(8) 0.121(9) 0.142(10) -0.006(7) 0.023(6) -0.002(6) C16A 0.121(15) 0.077(7) 0.128(10) 0.026(7) 0.001(11) 0.011(9) C1 0.0461(19) 0.0471(19) 0.0344(17) -0.0019(15) 0.0079(15) 0.0101(15) C2 0.052(2) 0.0483(19) 0.0425(19) -0.0108(16) 0.0108(16) -0.0029(16) C3 0.064(2) 0.0421(19) 0.048(2) -0.0045(17) 0.0189(18) -0.0005(17) C4 0.058(2) 0.0417(18) 0.0374(18) -0.0038(15) 0.0102(16) 0.0087(16) C5 0.0442(19) 0.0429(18) 0.0429(19) -0.0075(15) 0.0066(15) 0.0057(15) C6 0.0455(19) 0.0405(18) 0.0426(19) -0.0006(15) 0.0104(15) 0.0050(15) C7 0.051(2) 0.057(2) 0.0385(18) 0.0005(16) 0.0034(16) 0.0074(17) C8 0.067(3) 0.077(3) 0.059(2) -0.015(2) 0.018(2) -0.018(2) C9 0.124(4) 0.066(3) 0.066(3) -0.011(2) 0.044(3) -0.033(3) C10 0.068(2) 0.051(2) 0.0379(19) 0.0002(16) 0.0053(17) 0.0078(18) C11 0.061(2) 0.071(3) 0.052(2) -0.018(2) 0.0104(19) -0.0089(19) C12 0.076(3) 0.058(2) 0.058(2) -0.0061(19) 0.024(2) -0.011(2) C15 0.224(7) 0.060(3) 0.068(3) -0.003(3) 0.032(4) -0.008(4) C17 0.162(5) 0.074(3) 0.070(3) 0.008(3) 0.034(3) -0.033(3) C18 0.213(7) 0.154(6) 0.077(4) 0.004(4) 0.045(4) -0.111(5) C19 0.061(3) 0.108(4) 0.120(4) -0.027(3) 0.011(3) -0.004(3) C20 0.072(4) 0.223(8) 0.207(8) 0.025(7) 0.013(5) -0.021(5) C21 0.073(3) 0.046(2) 0.0387(19) 0.0072(16) 0.0038(18) -0.0108(18) C22 0.073(3) 0.042(2) 0.059(2) 0.0041(18) 0.016(2) -0.0015(18) C23 0.065(2) 0.049(2) 0.054(2) 0.0180(18) 0.0044(19) -0.0005(18) C24 0.090(3) 0.059(2) 0.041(2) 0.0047(18) 0.003(2) -0.018(2) C25 0.129(4) 0.072(3) 0.098(4) 0.022(3) 0.051(3) 0.025(3) C26 0.093(3) 0.084(3) 0.096(4) 0.045(3) 0.010(3) 0.017(3) C27 0.120(4) 0.077(3) 0.063(3) 0.000(2) -0.003(3) -0.047(3) C28 0.161(6) 0.072(3) 0.115(5) -0.012(3) 0.035(4) -0.021(4) C29 0.107(5) 0.193(7) 0.120(5) -0.002(5) 0.023(4) 0.036(5) C13A 0.074(17) 0.075(17) 0.059(12) -0.042(11) 0.003(10) -0.008(11) C14A 0.11(2) 0.19(3) 0.091(17) 0.02(2) 0.055(15) 0.04(2) C13B 0.043(4) 0.100(9) 0.166(10) -0.053(8) 0.011(5) 0.004(5) C14B 0.055(5) 0.179(11) 0.120(7) -0.015(7) 0.026(5) -0.012(5) C16B 0.139(19) 0.086(10) 0.115(14) 0.001(9) -0.036(15) 0.036(12) C30B 0.147(10) 0.142(10) 0.142(10) 0.016(8) 0.013(8) -0.027(8) N1 0.082(3) 0.135(4) 0.066(3) -0.022(3) 0.037(2) -0.034(3) N2 0.098(3) 0.055(2) 0.062(2) -0.0017(19) -0.006(2) -0.015(2) N3 0.070(2) 0.079(3) 0.068(2) -0.008(2) 0.0290(19) 0.009(2) Nd1 0.05865(13) 0.04472(11) 0.02730(10) 0.00074(8) 0.00702(8) -0.00438(9) O1 0.0622(15) 0.0622(15) 0.0319(12) -0.0048(11) 0.0064(11) 0.0018(12) O2 0.0492(16) 0.106(2) 0.0654(18) -0.0343(17) 0.0033(13) 0.0079(15) O3 0.115(2) 0.0580(16) 0.0403(14) 0.0020(13) 0.0086(15) 0.0154(16) O4 0.0682(16) 0.0452(13) 0.0501(14) -0.0003(11) 0.0239(12) 0.0000(11) O5 0.0604(17) 0.0732(17) 0.0609(16) -0.0139(14) 0.0068(13) -0.0002(14) O6 0.094(2) 0.0565(15) 0.0394(14) 0.0004(12) 0.0199(13) -0.0145(14) O7 0.080(2) 0.127(3) 0.0526(18) 0.0011(18) 0.0165(16) -0.031(2) O8 0.065(2) 0.272(6) 0.072(2) 0.014(3) 0.0158(18) 0.005(3) O9 0.102(3) 0.298(6) 0.120(3) -0.047(4) 0.066(3) -0.077(4) O10 0.156(3) 0.0603(18) 0.063(2) 0.0068(16) -0.030(2) -0.019(2) O11 0.135(3) 0.069(2) 0.079(2) 0.0166(18) -0.043(2) -0.0317(19) O12 0.170(4) 0.0488(19) 0.126(3) -0.007(2) -0.027(3) -0.023(2) O13 0.098(2) 0.0594(18) 0.111(3) -0.0195(18) 0.041(2) -0.0005(17) O14 0.0759(19) 0.0634(17) 0.082(2) -0.0096(15) 0.0384(16) -0.0045(14) O15 0.116(3) 0.131(3) 0.201(5) -0.025(3) 0.108(3) 0.002(2) O16 0.0806(18) 0.0706(17) 0.0335(13) 0.0140(12) 0.0056(12) -0.0071(14) O17 0.081(2) 0.114(3) 0.0666(19) 0.0177(19) -0.0008(16) 0.0163(19) O18 0.116(2) 0.0631(17) 0.0428(15) -0.0004(13) 0.0119(15) -0.0299(16) P1 0.0503(5) 0.0561(5) 0.0316(4) -0.0045(4) 0.0020(4) 0.0063(4) P2 0.0604(6) 0.0469(5) 0.0333(5) -0.0015(4) 0.0124(4) -0.0009(4) P3 0.0745(7) 0.0629(6) 0.0319(5) 0.0088(4) 0.0021(5) -0.0109(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C30A H30B 0.7688 . ? C30A C29 1.497(9) . ? C30A H30A 1.1039 . ? C30A H30B 0.7688 . ? C16A C15 1.458(13) . ? C16A H16A 0.9487 . ? C16A H16B 0.9813 . ? C16A H16C 0.9002 . ? C1 C6 1.396(4) . ? C1 C2 1.397(5) . ? C1 C7 1.524(4) . ? C2 C3 1.403(5) . ? C2 C8 1.508(5) . ? C3 C4 1.400(5) . ? C3 C9 1.514(5) . ? C4 C5 1.392(5) . ? C4 C10 1.528(4) . ? C5 C6 1.406(4) . ? C5 C11 1.507(5) . ? C6 C12 1.517(5) . ? C7 P1 1.777(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 P2 1.784(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C15 O3 1.386(5) . ? C15 C16B 1.435(13) . ? C15 H15A 0.9451 . ? C15 H15B 1.1023 . ? C15 H15C 0.8539 . ? C15 H15D 1.1510 . ? C17 C18 1.447(7) . ? C17 O6 1.481(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.368(7) . ? C19 O5 1.459(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C23 1.394(5) . ? C21 C22 1.395(5) . ? C21 C24 1.522(5) . ? C22 C23 1.406(5) 3_656 ? C22 C25 1.517(6) . ? C23 C22 1.406(5) 3_656 ? C23 C26 1.515(5) . ? C24 P3 1.783(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.454(7) . ? C27 O18 1.458(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 O17 1.439(7) . ? C29 C30B 1.471(9) . ? C29 H29A 0.7961 . ? C29 H29B 1.0426 . ? C29 H29C 1.2207 . ? C29 H29D 0.6369 . ? C13A O2 1.478(17) . ? C13A C14A 1.522(19) . ? C13A H13A 0.9357 . ? C13A H13B 1.0224 . ? C14A H14A 0.8856 . ? C14A H14B 0.9774 . ? C14A H14C 0.9490 . ? C13B O2 1.446(9) . ? C13B C14B 1.498(11) . ? C13B H13C 0.9613 . ? C13B H13D 0.9644 . ? C14B H14D 0.9694 . ? C14B H14E 0.9694 . ? C14B H14F 0.8783 . ? C16B H16D 0.9055 . ? C16B H16D 0.9055 . ? C16B H16E 1.0080 . ? C16B H16F 1.0084 . ? C30B H29B 1.1064 . ? C30B H30D 0.9870 . ? C30B H30E 0.9691 . ? C30B H30F 0.9240 . ? N1 O9 1.207(5) . ? N1 O7 1.219(5) . ? N1 O8 1.237(5) . ? N2 O12 1.205(4) . ? N2 O11 1.227(4) . ? N2 O10 1.252(4) . ? N3 O15 1.207(4) . ? N3 O14 1.249(4) . ? N3 O13 1.253(4) . ? Nd1 O16 2.364(2) . ? Nd1 O4 2.406(2) 3_655 ? Nd1 O1 2.413(2) . ? Nd1 O13 2.514(3) . ? Nd1 O7 2.527(3) . ? Nd1 O11 2.527(3) . ? Nd1 O8 2.531(3) . ? Nd1 O14 2.537(3) . ? Nd1 O10 2.551(3) . ? O1 P1 1.483(2) . ? O2 P1 1.559(3) . ? O3 P1 1.553(3) . ? O4 P2 1.474(2) . ? O4 Nd1 2.406(2) 3_655 ? O5 P2 1.553(3) . ? O6 P2 1.564(2) . ? O16 P3 1.470(2) . ? O17 P3 1.556(3) . ? O18 P3 1.554(3) . ? 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 H30B C30A C29 131.7 . . ? H30B C30A H30A 109.9 . . ? C29 C30A H30A 113.1 . . ? H30B C30A H30B 0.0 . . ? C29 C30A H30B 131.7 . . ? H30A C30A H30B 109.9 . . ? H30B C30A H30C 85.2 . . ? C29 C30A H30C 83.8 . . ? H30A C30A H30C 77.2 . . ? H30B C30A H30C 85.2 . . ? H30B C30A H30E 32.0 . . ? C29 C30A H30E 116.0 . . ? H30A C30A H30E 130.6 . . ? H30B C30A H30E 32.0 . . ? H30C C30A H30E 112.5 . . ? H30B C30A H30F 121.9 . . ? C29 C30A H30F 90.3 . . ? H30A C30A H30F 74.7 . . ? H30B C30A H30F 121.9 . . ? H30C C30A H30F 146.2 . . ? H30E C30A H30F 100.1 . . ? C15 C16A H16A 107.8 . . ? C15 C16A H16B 101.6 . . ? H16A C16A H16B 108.8 . . ? C15 C16A H16C 110.4 . . ? H16A C16A H16C 114.7 . . ? H16B C16A H16C 112.6 . . ? C15 C16A H15D 47.0 . . ? H16A C16A H15D 97.4 . . ? H16B C16A H15D 145.1 . . ? H16C C16A H15D 74.6 . . ? C15 C16A H16D 95.4 . . ? H16A C16A H16D 45.9 . . ? H16B C16A H16D 68.5 . . ? H16C C16A H16D 152.8 . . ? H15D C16A H16D 121.2 . . ? C15 C16A H16F 111.9 . . ? H16A C16A H16F 121.3 . . ? H16B C16A H16F 23.0 . . ? H16C C16A H16F 89.6 . . ? H15D C16A H16F 141.3 . . ? H16D C16A H16F 88.6 . . ? C6 C1 C2 121.0(3) . . ? C6 C1 C7 119.9(3) . . ? C2 C1 C7 119.0(3) . . ? C1 C2 C3 119.4(3) . . ? C1 C2 C8 122.5(3) . . ? C3 C2 C8 118.1(3) . . ? C4 C3 C2 119.6(3) . . ? C4 C3 C9 121.4(3) . . ? C2 C3 C9 119.0(3) . . ? C5 C4 C3 121.0(3) . . ? C5 C4 C10 119.6(3) . . ? C3 C4 C10 119.4(3) . . ? C4 C5 C6 119.5(3) . . ? C4 C5 C11 120.7(3) . . ? C6 C5 C11 119.8(3) . . ? C1 C6 C5 119.5(3) . . ? C1 C6 C12 121.1(3) . . ? C5 C6 C12 119.4(3) . . ? C1 C7 P1 117.1(2) . . ? C1 C7 H7A 108.0 . . ? P1 C7 H7A 108.0 . . ? C1 C7 H7B 108.0 . . ? P1 C7 H7B 108.0 . . ? H7A C7 H7B 107.3 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C9 H9A 109.5 . . ? C3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 P2 116.9(2) . . ? C4 C10 H10A 108.1 . . ? P2 C10 H10A 108.1 . . ? C4 C10 H10B 108.1 . . ? P2 C10 H10B 108.1 . . ? H10A C10 H10B 107.3 . . ? C5 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O3 C15 C16B 111.9(10) . . ? O3 C15 C16A 115.4(8) . . ? C16B C15 C16A 36.1(10) . . ? O3 C15 H15A 119.9 . . ? C16B C15 H15A 80.1 . . ? C16A C15 H15A 107.1 . . ? O3 C15 H15B 113.9 . . ? C16B C15 H15B 126.1 . . ? C16A C15 H15B 97.4 . . ? H15A C15 H15B 99.9 . . ? O3 C15 H15C 114.6 . . ? C16B C15 H15C 119.0 . . ? C16A C15 H15C 130.0 . . ? H15A C15 H15C 43.0 . . ? H15B C15 H15C 62.9 . . ? O3 C15 H15D 106.8 . . ? C16B C15 H15D 100.7 . . ? C16A C15 H15D 65.1 . . ? H15A C15 H15D 129.4 . . ? H15B C15 H15D 39.5 . . ? H15C C15 H15D 101.3 . . ? C18 C17 O6 110.7(4) . . ? C18 C17 H17A 109.5 . . ? O6 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? O6 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? 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 . . ? C20 C19 O5 111.0(5) . . ? C20 C19 H19A 109.4 . . ? O5 C19 H19A 109.4 . . ? C20 C19 H19B 109.4 . . ? O5 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 C22 120.6(3) . . ? C23 C21 C24 119.1(3) . . ? C22 C21 C24 120.3(4) . . ? C21 C22 C23 119.4(3) . 3_656 ? C21 C22 C25 120.8(4) . . ? C23 C22 C25 119.8(4) 3_656 . ? C21 C23 C22 120.0(3) . 3_656 ? C21 C23 C26 121.7(3) . . ? C22 C23 C26 118.3(4) 3_656 . ? C21 C24 P3 118.4(3) . . ? C21 C24 H24A 107.7 . . ? P3 C24 H24A 107.7 . . ? C21 C24 H24B 107.7 . . ? P3 C24 H24B 107.7 . . ? H24A C24 H24B 107.1 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 O18 109.0(4) . . ? C28 C27 H27A 109.9 . . ? O18 C27 H27A 109.9 . . ? C28 C27 H27B 109.9 . . ? O18 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? 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 . . ? O17 C29 C30B 113.5(9) . . ? O17 C29 C30A 110.3(8) . . ? C30B C29 C30A 36.4(7) . . ? O17 C29 H29A 113.4 . . ? C30B C29 H29A 133.1 . . ? C30A C29 H29A 121.9 . . ? O17 C29 H29B 108.6 . . ? C30B C29 H29B 48.7 . . ? C30A C29 H29B 84.8 . . ? H29A C29 H29B 114.0 . . ? O17 C29 H29C 94.3 . . ? C30B C29 H29C 89.3 . . ? C30A C29 H29C 125.3 . . ? H29A C29 H29C 87.4 . . ? H29B C29 H29C 40.6 . . ? O17 C29 H29D 115.4 . . ? C30B C29 H29D 130.8 . . ? C30A C29 H29D 116.6 . . ? H29A C29 H29D 5.8 . . ? H29B C29 H29D 117.2 . . ? H29C C29 H29D 92.7 . . ? O2 C13A C14A 106.7(16) . . ? O2 C13A H13A 114.4 . . ? C14A C13A H13A 111.7 . . ? O2 C13A H13B 110.4 . . ? C14A C13A H13B 106.5 . . ? H13A C13A H13B 107.0 . . ? O2 C13A H13C 83.8 . . ? C14A C13A H13C 40.0 . . ? H13A C13A H13C 93.3 . . ? H13B C13A H13C 146.3 . . ? O2 C13A H13D 107.8 . . ? C14A C13A H13D 95.7 . . ? H13A C13A H13D 21.6 . . ? H13B C13A H13D 127.2 . . ? H13C C13A H13D 72.0 . . ? O2 C13A H14D 110.2 . . ? C14A C13A H14D 92.6 . . ? H13A C13A H14D 118.7 . . ? H13B C13A H14D 15.1 . . ? H13C C13A H14D 131.8 . . ? H13D C13A H14D 136.7 . . ? C13A C14A H14A 110.5 . . ? C13A C14A H14B 108.0 . . ? H14A C14A H14B 113.6 . . ? C13A C14A H14C 107.5 . . ? H14A C14A H14C 109.8 . . ? H14B C14A H14C 107.2 . . ? C13A C14A H13C 71.4 . . ? H14A C14A H13C 127.1 . . ? H14B C14A H13C 115.4 . . ? H14C C14A H13C 36.3 . . ? C13A C14A H14E 79.8 . . ? H14A C14A H14E 102.7 . . ? H14B C14A H14E 37.4 . . ? H14C C14A H14E 140.9 . . ? H13C C14A H14E 128.3 . . ? C13A C14A H14F 79.2 . . ? H14A C14A H14F 45.6 . . ? H14B C14A H14F 94.4 . . ? H14C C14A H14F 153.4 . . ? H13C C14A H14F 143.1 . . ? H14E C14A H14F 64.9 . . ? O2 C13B C14B 105.7(8) . . ? O2 C13B H13A 104.5 . . ? C14B C13B H13A 97.7 . . ? O2 C13B H13B 85.9 . . ? C14B C13B H13B 40.8 . . ? H13A C13B H13B 68.4 . . ? O2 C13B H14C 122.1 . . ? C14B C13B H14C 93.0 . . ? H13A C13B H14C 126.9 . . ? H13B C13B H14C 133.2 . . ? O2 C13B H13C 112.7 . . ? C14B C13B H13C 109.5 . . ? H13A C13B H13C 124.5 . . ? H13B C13B H13C 150.0 . . ? H14C C13B H13C 16.8 . . ? O2 C13B H13D 111.0 . . ? C14B C13B H13D 110.3 . . ? H13A C13B H13D 17.5 . . ? H13B C13B H13D 85.5 . . ? H14C C13B H13D 112.5 . . ? H13C C13B H13D 107.7 . . ? C13B C14B H13B 74.0 . . ? C13B C14B H14A 77.4 . . ? H13B C14B H14A 130.1 . . ? C13B C14B H14B 78.2 . . ? H13B C14B H14B 142.0 . . ? H14A C14B H14B 65.8 . . ? C13B C14B H14D 104.1 . . ? H13B C14B H14D 31.1 . . ? H14A C14B H14D 147.4 . . ? H14B C14B H14D 146.8 . . ? C13B C14B H14E 107.9 . . ? H13B C14B H14E 125.3 . . ? H14A C14B H14E 101.9 . . ? H14B C14B H14E 42.7 . . ? H14D C14B H14E 108.2 . . ? C13B C14B H14F 108.0 . . ? H13B C14B H14F 118.4 . . ? H14A C14B H14F 38.3 . . ? H14B C14B H14F 94.5 . . ? H14D C14B H14F 115.4 . . ? H14E C14B H14F 112.7 . . ? H16D C16B C15 114.9 . . ? H16D C16B H15A 94.4 . . ? C15 C16B H15A 36.2 . . ? H16D C16B H16A 41.5 . . ? C15 C16B H16A 90.6 . . ? H15A C16B H16A 93.7 . . ? H16D C16B H16B 105.2 . . ? C15 C16B H16B 126.7 . . ? H15A C16B H16B 159.7 . . ? H16A C16B H16B 97.7 . . ? H16D C16B H16D 0.0 . . ? C15 C16B H16D 114.9 . . ? H15A C16B H16D 94.4 . . ? H16A C16B H16D 41.5 . . ? H16B C16B H16D 105.2 . . ? H16D C16B H16E 110.8 . . ? C15 C16B H16E 104.8 . . ? H15A C16B H16E 86.0 . . ? H16A C16B H16E 152.2 . . ? H16B C16B H16E 91.4 . . ? H16D C16B H16E 110.8 . . ? H16D C16B H16F 110.0 . . ? C15 C16B H16F 113.4 . . ? H15A C16B H16F 149.0 . . ? H16A C16B H16F 92.4 . . ? H16B C16B H16F 14.7 . . ? H16D C16B H16F 110.0 . . ? H16E C16B H16F 102.1 . . ? C29 C30B H29B 45.0 . . ? C29 C30B H30B 94.5 . . ? H29B C30B H30B 136.8 . . ? C29 C30B H30D 116.9 . . ? H29B C30B H30D 82.8 . . ? H30B C30B H30D 112.2 . . ? C29 C30B H30E 95.0 . . ? H29B C30B H30E 135.8 . . ? H30B C30B H30E 4.3 . . ? H30D C30B H30E 108.3 . . ? C29 C30B H30F 113.4 . . ? H29B C30B H30F 103.2 . . ? H30B C30B H30F 108.1 . . ? H30D C30B H30F 110.5 . . ? H30E C30B H30F 111.6 . . ? O9 N1 O7 122.1(5) . . ? O9 N1 O8 121.9(5) . . ? O7 N1 O8 115.9(4) . . ? O12 N2 O11 122.5(4) . . ? O12 N2 O10 121.7(4) . . ? O11 N2 O10 115.8(3) . . ? O15 N3 O14 120.8(4) . . ? O15 N3 O13 122.5(4) . . ? O14 N3 O13 116.7(3) . . ? O16 Nd1 O4 84.51(9) . 3_655 ? O16 Nd1 O1 154.44(8) . . ? O4 Nd1 O1 81.80(8) 3_655 . ? O16 Nd1 O13 85.49(10) . . ? O4 Nd1 O13 124.44(9) 3_655 . ? O1 Nd1 O13 84.62(10) . . ? O16 Nd1 O7 124.65(10) . . ? O4 Nd1 O7 82.38(9) 3_655 . ? O1 Nd1 O7 74.71(10) . . ? O13 Nd1 O7 143.58(11) . . ? O16 Nd1 O11 75.99(10) . . ? O4 Nd1 O11 151.72(10) 3_655 . ? O1 Nd1 O11 123.51(9) . . ? O13 Nd1 O11 74.73(12) . . ? O7 Nd1 O11 91.96(12) . . ? O16 Nd1 O8 76.60(11) . . ? O4 Nd1 O8 83.60(12) 3_655 . ? O1 Nd1 O8 122.82(10) . . ? O13 Nd1 O8 145.27(13) . . ? O7 Nd1 O8 48.63(11) . . ? O11 Nd1 O8 72.18(14) . . ? O16 Nd1 O14 75.53(9) . . ? O4 Nd1 O14 74.72(8) 3_655 . ? O1 Nd1 O14 80.08(9) . . ? O13 Nd1 O14 49.89(9) . . ? O7 Nd1 O14 148.00(10) . . ? O11 Nd1 O14 118.62(11) . . ? O8 Nd1 O14 145.99(12) . . ? O16 Nd1 O10 123.77(9) . . ? O4 Nd1 O10 150.26(9) 3_655 . ? O1 Nd1 O10 74.88(9) . . ? O13 Nd1 O10 71.87(12) . . ? O7 Nd1 O10 73.92(12) . . ? O11 Nd1 O10 48.86(9) . . ? O8 Nd1 O10 93.64(14) . . ? O14 Nd1 O10 118.06(11) . . ? P1 O1 Nd1 147.53(15) . . ? C13B O2 C13A 23.8(10) . . ? C13B O2 P1 119.8(4) . . ? C13A O2 P1 133.3(10) . . ? C15 O3 P1 127.8(3) . . ? P2 O4 Nd1 154.63(14) . 3_655 ? C19 O5 P2 123.3(3) . . ? C17 O6 P2 121.1(3) . . ? N1 O7 Nd1 97.9(2) . . ? N1 O8 Nd1 97.1(3) . . ? N2 O10 Nd1 96.7(2) . . ? N2 O11 Nd1 98.6(2) . . ? N3 O13 Nd1 97.2(2) . . ? N3 O14 Nd1 96.2(2) . . ? P3 O16 Nd1 171.12(17) . . ? C29 O17 P3 123.0(3) . . ? C27 O18 P3 121.3(3) . . ? O1 P1 O3 113.61(14) . . ? O1 P1 O2 112.34(15) . . ? O3 P1 O2 105.43(17) . . ? O1 P1 C7 113.54(15) . . ? O3 P1 C7 107.27(16) . . ? O2 P1 C7 103.86(16) . . ? O4 P2 O5 113.76(15) . . ? O4 P2 O6 108.54(14) . . ? O5 P2 O6 108.27(15) . . ? O4 P2 C10 114.55(16) . . ? O5 P2 C10 103.48(16) . . ? O6 P2 C10 107.91(15) . . ? O16 P3 O18 114.45(16) . . ? O16 P3 O17 112.11(17) . . ? O18 P3 O17 103.76(18) . . ? O16 P3 C24 112.17(17) . . ? O18 P3 C24 104.25(17) . . ? O17 P3 C24 109.5(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.398 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.061 data_Sm #TrackingRef '- SI-cif.txt' _database_code_depnum_ccdc_archive 'CCDC 793772' #TrackingRef '- Sm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H60 N3 O19 P3 Sm' _chemical_formula_weight 1034.09 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3803(10) _cell_length_b 10.8448(10) _cell_length_c 24.194(2) _cell_angle_alpha 93.937(4) _cell_angle_beta 93.343(4) _cell_angle_gamma 113.073(5) _cell_volume 2489.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3955 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 22.73 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.752 _exptl_absorpt_correction_T_max 0.818 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13547 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.85 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9172 _reflns_number_gt 7123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 8.40 Ratio PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for C19 Some terminal C atoms in disordered side chains have high isotropic U-values. PLAT242_ALERT_2_A Check Low Ueq as Compared to Neighbors for O6 The oxygen atom has less thermal motion than the side carbon atoms. ; _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^)+(0.0826P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9172 _refine_ls_number_parameters 534 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.075 _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 Sm1 Sm 0.09603(3) 0.32572(3) 0.732970(11) 0.04912(13) Uani 1 1 d . . . C1 C 0.0401(7) 0.1724(5) 0.3743(2) 0.0548(14) Uani 1 1 d . . . C2 C 0.1579(7) 0.2404(6) 0.4133(3) 0.0601(15) Uani 1 1 d . . . C3 C 0.1418(6) 0.2361(6) 0.4704(2) 0.0552(14) Uani 1 1 d . . . C4 C 0.0094(6) 0.1659(5) 0.4883(2) 0.0494(13) Uani 1 1 d . . . C5 C -0.1072(6) 0.0988(5) 0.4499(2) 0.0488(13) Uani 1 1 d . . . C6 C -0.0918(6) 0.1012(5) 0.3923(2) 0.0525(13) Uani 1 1 d . . . C7 C -0.2172(7) 0.0323(8) 0.3502(3) 0.0772(19) Uani 1 1 d . . . H7A H -0.2344 0.0986 0.3302 0.116 Uiso 1 1 calc R . . H7B H -0.2982 -0.0162 0.3690 0.116 Uiso 1 1 calc R . . H7C H -0.1988 -0.0292 0.3246 0.116 Uiso 1 1 calc R . . C8 C 0.0565(8) 0.1785(7) 0.3121(2) 0.0662(17) Uani 1 1 d . . . H8A H 0.1291 0.2653 0.3070 0.079 Uiso 1 1 calc R . . H8B H -0.0308 0.1746 0.2938 0.079 Uiso 1 1 calc R . . C9 C 0.3004(8) 0.3203(8) 0.3947(4) 0.096(3) Uani 1 1 d . . . H9A H 0.3420 0.4059 0.4166 0.144 Uiso 1 1 calc R . . H9B H 0.2905 0.3341 0.3562 0.144 Uiso 1 1 calc R . . H9C H 0.3596 0.2717 0.3994 0.144 Uiso 1 1 calc R . . C10 C 0.2710(7) 0.3128(7) 0.5110(3) 0.078(2) Uani 1 1 d . . . H10A H 0.2479 0.2943 0.5483 0.118 Uiso 1 1 calc R . . H10B H 0.3015 0.4076 0.5081 0.118 Uiso 1 1 calc R . . H10C H 0.3451 0.2847 0.5024 0.118 Uiso 1 1 calc R . . C11 C -0.0075(7) 0.1621(6) 0.5506(2) 0.0587(15) Uani 1 1 d . . . H11A H 0.0773 0.1605 0.5690 0.070 Uiso 1 1 calc R . . H11B H -0.0845 0.0782 0.5559 0.070 Uiso 1 1 calc R . . C12 C -0.2492(7) 0.0242(7) 0.4690(3) 0.0736(18) Uani 1 1 d . . . H12A H -0.2386 -0.0006 0.5058 0.110 Uiso 1 1 calc R . . H12B H -0.2994 -0.0555 0.4441 0.110 Uiso 1 1 calc R . . H12C H -0.3007 0.0809 0.4695 0.110 Uiso 1 1 calc R . . C13 C -0.2836(16) 0.3278(18) 0.5946(6) 0.225(9) Uani 1 1 d D . . H13A H -0.3280 0.3732 0.5720 0.270 Uiso 1 1 calc R . . H13B H -0.2374 0.3830 0.6290 0.270 Uiso 1 1 calc R . . C14 C -0.382(2) 0.184(2) 0.6034(11) 0.41(2) Uani 1 1 d D . . H14A H -0.4754 0.1656 0.5873 0.610 Uiso 1 1 d R . . H14B H -0.3833 0.1774 0.6427 0.610 Uiso 1 1 d R . . H14C H -0.3490 0.1208 0.5866 0.610 Uiso 1 1 d R . . C15 C 0.0884(10) 0.5624(5) 0.5824(3) 0.099(3) Uani 1 1 d D . . H15A H 0.0709 0.5658 0.6213 0.119 Uiso 1 1 calc R . . H15B H 0.0298 0.5980 0.5618 0.119 Uiso 1 1 calc R . . C16 C 0.2441(9) 0.6427(8) 0.5755(4) 0.114(3) Uani 1 1 d D . . H16A H 0.3007 0.6113 0.5987 0.171 Uiso 1 1 calc R . . H16B H 0.2681 0.7365 0.5861 0.171 Uiso 1 1 calc R . . H16C H 0.2611 0.6306 0.5373 0.171 Uiso 1 1 calc R . . C17 C -0.0004(8) 0.0479(10) 0.1738(3) 0.108(3) Uani 1 1 d D . . H17A H -0.0441 0.1123 0.1756 0.130 Uiso 1 1 calc R . . H17B H -0.0706 -0.0411 0.1777 0.130 Uiso 1 1 calc R . . C18 C 0.0690(13) 0.0497(13) 0.1194(3) 0.178(6) Uani 1 1 d D . . H18A H 0.1554 0.1282 0.1215 0.266 Uiso 1 1 calc R . . H18B H 0.0068 0.0519 0.0888 0.266 Uiso 1 1 calc R . . H18C H 0.0882 -0.0297 0.1137 0.266 Uiso 1 1 calc R . . C19 C 0.3513(11) 0.065(2) 0.2624(6) 0.270(11) Uani 1 1 d D . . H19A H 0.3396 0.0978 0.2270 0.325 Uiso 1 1 d R . . H19B H 0.3402 -0.0284 0.2560 0.325 Uiso 1 1 d R . . C20 C 0.4922(14) 0.1517(19) 0.2941(8) 0.250(10) Uani 1 1 d D . . H20A H 0.4931 0.2383 0.3060 0.376 Uiso 1 1 calc R . . H20B H 0.5660 0.1626 0.2703 0.376 Uiso 1 1 calc R . . H20C H 0.5065 0.1091 0.3260 0.376 Uiso 1 1 calc R . . C21 C 0.4143(18) -0.0053(14) 0.8648(6) 0.193(7) Uani 1 1 d D . . H21A H 0.4904 0.0368 0.8934 0.290 Uiso 1 1 calc R . . H21B H 0.4314 -0.0726 0.8422 0.290 Uiso 1 1 calc R . . H21C H 0.3279 -0.0467 0.8816 0.290 Uiso 1 1 calc R . . C22 C 0.4034(14) 0.1009(11) 0.8285(4) 0.161(5) Uani 1 1 d D . . H22A H 0.4906 0.1436 0.8116 0.193 Uiso 1 1 calc R . . H22B H 0.3280 0.0588 0.7990 0.193 Uiso 1 1 calc R . . C23 C 0.7044(16) 0.5521(14) 0.7782(7) 0.246(10) Uani 1 1 d D . . H23A H 0.6724 0.6237 0.7832 0.369 Uiso 1 1 calc R . . H23B H 0.7397 0.5525 0.7424 0.369 Uiso 1 1 calc R . . H23C H 0.7779 0.5647 0.8067 0.369 Uiso 1 1 calc R . . C24 C 0.5825(11) 0.4178(14) 0.7818(3) 0.165(5) Uani 1 1 d D . . H24A H 0.5136 0.3975 0.7500 0.198 Uiso 1 1 calc R . . H24B H 0.6160 0.3460 0.7822 0.198 Uiso 1 1 calc R . . C25 C 0.3104(8) 0.4081(9) 0.8979(3) 0.081(2) Uani 1 1 d . . . H25A H 0.2971 0.4857 0.8853 0.097 Uiso 1 1 calc R . . H25B H 0.2196 0.3447 0.9066 0.097 Uiso 1 1 calc R . . C26 C 0.2797(11) 0.2280(9) 0.9866(4) 0.130(4) Uani 1 1 d . . . H26A H 0.2121 0.2196 0.9562 0.195 Uiso 1 1 calc R . . H26B H 0.2341 0.2126 1.0204 0.195 Uiso 1 1 calc R . . H26C H 0.3196 0.1628 0.9797 0.195 Uiso 1 1 calc R . . C27 C 0.3964(8) 0.3698(7) 0.9924(3) 0.0741(19) Uani 1 1 d . . . C28 C 0.4102(7) 0.4542(7) 0.9517(2) 0.0671(17) Uani 1 1 d . . . C29 C 0.5135(8) 0.5870(7) 0.9587(3) 0.0758(19) Uani 1 1 d . . . C30 C 0.5282(12) 0.6808(9) 0.9140(3) 0.127(4) Uani 1 1 d . . . H30A H 0.6258 0.7271 0.9086 0.190 Uiso 1 1 calc R . . H30B H 0.4900 0.7453 0.9251 0.190 Uiso 1 1 calc R . . H30C H 0.4779 0.6298 0.8798 0.190 Uiso 1 1 calc R . . C31 C 0.781(3) 0.175(2) 0.0005(13) 0.43(2) Uani 1 1 d D . . H31A H 0.8260 0.1421 -0.0266 0.648 Uiso 1 1 d R . . H31B H 0.7044 0.1909 -0.0178 0.648 Uiso 1 1 d R . . H31C H 0.7448 0.1104 0.0267 0.648 Uiso 1 1 d R . . C32 C 0.886(3) 0.309(3) 0.0321(8) 0.309(16) Uani 1 1 d D . . H32A H 0.9308 0.3486 -0.0002 0.370 Uiso 1 1 d R . . H32B H 0.8209 0.3510 0.0385 0.370 Uiso 1 1 d R . . N1 N -0.1308(7) 0.2477(7) 0.8064(3) 0.0801(17) Uani 1 1 d . . . N2 N 0.1376(8) 0.6055(6) 0.7675(3) 0.0849(18) Uani 1 1 d . . . N3 N 0.3367(6) 0.4061(8) 0.6662(3) 0.0744(16) Uani 1 1 d . . . O1 O -0.0227(5) 0.3032(4) 0.64517(15) 0.0647(11) Uani 1 1 d . . . O2 O -0.1905(6) 0.2772(7) 0.5636(2) 0.1043(19) Uani 1 1 d D . . O3 O 0.0587(7) 0.4216(4) 0.5596(2) 0.0950(17) Uani 1 1 d D . . O4 O -0.0023(4) -0.0864(4) 0.28317(17) 0.0625(11) Uani 1 1 d . . . O5 O 0.1196(5) 0.0866(5) 0.21666(18) 0.0906(16) Uani 1 1 d D . . O6 O 0.2514(5) 0.0787(6) 0.3022(2) 0.0993(17) Uani 1 1 d D . . O7 O 0.2691(4) 0.2981(5) 0.79081(16) 0.0685(12) Uani 1 1 d . . . O8 O 0.3748(7) 0.2040(6) 0.8641(2) 0.0992(17) Uani 1 1 d D . . O9 O 0.5181(5) 0.4300(6) 0.8344(2) 0.0972(17) Uani 1 1 d D . . O10 O -0.1506(5) 0.2710(6) 0.7572(2) 0.0891(15) Uani 1 1 d . . . O11 O -0.2278(7) 0.2087(8) 0.8354(3) 0.132(3) Uani 1 1 d . . . O12 O -0.0086(5) 0.2637(6) 0.82286(19) 0.0832(14) Uani 1 1 d . . . O13 O 0.0574(6) 0.5400(5) 0.7257(2) 0.0862(15) Uani 1 1 d . . . O14 O 0.1884(7) 0.5413(5) 0.7959(2) 0.0948(17) Uani 1 1 d . . . O15 O 0.1587(8) 0.7222(6) 0.7801(3) 0.132(3) Uani 1 1 d . . . O16 O 0.3056(6) 0.4890(6) 0.6951(2) 0.0916(15) Uani 1 1 d . . . O17 O 0.4381(6) 0.4409(7) 0.6405(3) 0.117(2) Uani 1 1 d . . . O18 O 0.2566(5) 0.2858(5) 0.66516(18) 0.0705(12) Uani 1 1 d . . . O19 O 0.999(2) 0.396(3) 0.0763(10) 0.474(17) Uani 1 1 d D . . H19 H 0.9868 0.3632 0.1060 0.569 Uiso 1 1 d R . . P1 P 0.09921(18) 0.05134(17) 0.27786(7) 0.0618(4) Uani 1 1 d . . . P2 P -0.03981(19) 0.29664(17) 0.58443(6) 0.0574(4) Uani 1 1 d . . . P3 P 0.36593(18) 0.33171(19) 0.84213(6) 0.0637(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0563(2) 0.0565(2) 0.03452(16) 0.00148(12) -0.00259(12) 0.02388(14) C1 0.074(4) 0.041(3) 0.052(3) 0.006(2) 0.013(3) 0.024(3) C2 0.068(4) 0.043(3) 0.060(4) -0.004(3) 0.008(3) 0.014(3) C3 0.065(4) 0.042(3) 0.053(3) -0.007(2) -0.002(3) 0.019(3) C4 0.066(4) 0.040(3) 0.047(3) 0.001(2) -0.003(3) 0.027(3) C5 0.057(3) 0.038(3) 0.051(3) 0.000(2) 0.006(2) 0.019(3) C6 0.061(4) 0.044(3) 0.053(3) -0.001(2) -0.005(3) 0.024(3) C7 0.073(4) 0.091(5) 0.069(4) -0.012(4) -0.010(3) 0.040(4) C8 0.092(5) 0.058(4) 0.049(3) 0.008(3) 0.009(3) 0.030(3) C9 0.083(5) 0.075(5) 0.095(6) -0.002(4) 0.031(4) -0.007(4) C10 0.069(4) 0.076(5) 0.080(5) -0.010(4) -0.009(4) 0.023(4) C11 0.080(4) 0.055(4) 0.048(3) 0.008(3) 0.004(3) 0.034(3) C12 0.076(5) 0.063(4) 0.070(4) 0.001(3) 0.007(3) 0.017(4) C13 0.26(2) 0.28(2) 0.186(15) -0.093(15) -0.076(15) 0.195(19) C14 0.20(2) 0.43(4) 0.36(4) -0.03(3) 0.03(2) -0.11(2) C15 0.190(10) 0.061(5) 0.064(5) 0.012(4) 0.015(5) 0.069(6) C16 0.159(10) 0.065(5) 0.116(7) 0.002(5) -0.030(7) 0.049(6) C17 0.136(8) 0.105(7) 0.074(5) 0.009(5) -0.004(5) 0.040(6) C18 0.226(14) 0.181(12) 0.060(6) 0.022(7) 0.014(7) 0.010(11) C19 0.093(9) 0.28(2) 0.42(3) -0.05(2) 0.061(15) 0.055(12) C20 0.112(11) 0.27(2) 0.33(3) -0.058(19) 0.020(14) 0.047(12) C21 0.254(18) 0.144(12) 0.205(16) 0.047(11) 0.045(14) 0.095(12) C22 0.160(11) 0.152(11) 0.191(14) 0.013(10) 0.020(10) 0.085(10) C23 0.224(17) 0.25(2) 0.28(2) 0.130(18) 0.145(17) 0.080(16) C24 0.096(8) 0.226(15) 0.138(11) 0.049(10) 0.002(7) 0.025(9) C25 0.082(5) 0.113(6) 0.053(4) -0.011(4) -0.011(3) 0.049(4) C26 0.151(9) 0.104(7) 0.078(6) -0.007(5) 0.014(6) -0.008(6) C27 0.088(5) 0.073(4) 0.042(3) -0.001(3) 0.007(3) 0.011(4) C28 0.065(4) 0.094(5) 0.040(3) -0.010(3) -0.008(3) 0.034(4) C29 0.101(5) 0.076(5) 0.045(3) 0.007(3) 0.000(3) 0.030(4) C30 0.209(11) 0.088(6) 0.061(5) 0.021(4) -0.008(6) 0.037(7) C31 0.53(5) 0.24(3) 0.37(4) 0.10(3) 0.17(4) -0.05(3) C32 0.48(5) 0.33(4) 0.098(12) 0.038(17) -0.009(19) 0.14(4) N1 0.084(5) 0.088(4) 0.071(4) 0.000(3) 0.024(4) 0.036(4) N2 0.123(5) 0.067(4) 0.065(4) -0.004(3) -0.009(4) 0.042(4) N3 0.054(3) 0.094(5) 0.064(4) 0.019(3) 0.006(3) 0.016(3) O1 0.081(3) 0.081(3) 0.039(2) 0.0032(19) -0.0053(19) 0.041(2) O2 0.120(4) 0.156(5) 0.067(3) -0.032(3) -0.037(3) 0.100(4) O3 0.173(5) 0.054(3) 0.070(3) 0.007(2) 0.043(3) 0.053(3) O4 0.074(3) 0.055(2) 0.059(2) 0.0000(19) 0.006(2) 0.027(2) O5 0.107(4) 0.092(4) 0.054(3) 0.001(2) 0.023(3) 0.018(3) O6 0.070(3) 0.106(4) 0.102(4) -0.019(3) 0.004(3) 0.019(3) O7 0.069(3) 0.098(3) 0.044(2) -0.004(2) -0.0110(19) 0.043(2) O8 0.138(5) 0.122(5) 0.062(3) 0.010(3) -0.004(3) 0.079(4) O9 0.067(3) 0.137(5) 0.072(3) -0.012(3) 0.007(3) 0.027(3) O10 0.075(3) 0.125(5) 0.081(4) 0.011(3) 0.007(3) 0.054(3) O11 0.107(5) 0.186(7) 0.112(5) 0.025(5) 0.063(4) 0.060(5) O12 0.074(3) 0.122(4) 0.054(3) 0.008(3) 0.012(2) 0.039(3) O13 0.120(4) 0.080(3) 0.071(3) -0.008(3) -0.019(3) 0.059(3) O14 0.147(5) 0.083(3) 0.058(3) -0.010(3) -0.024(3) 0.058(4) O15 0.190(7) 0.068(4) 0.135(6) -0.022(4) -0.026(5) 0.060(4) O16 0.092(4) 0.074(3) 0.093(4) 0.015(3) 0.017(3) 0.015(3) O17 0.073(4) 0.146(6) 0.106(5) 0.027(4) 0.033(3) 0.012(4) O18 0.068(3) 0.083(3) 0.056(3) 0.009(2) 0.013(2) 0.024(3) O19 0.65(5) 0.57(5) 0.35(3) 0.16(3) 0.09(3) 0.37(4) P1 0.0699(11) 0.0615(10) 0.0477(9) -0.0019(7) 0.0097(7) 0.0201(8) P2 0.0838(11) 0.0644(10) 0.0361(7) 0.0023(7) -0.0033(7) 0.0441(9) P3 0.0592(10) 0.0903(12) 0.0431(8) -0.0001(8) -0.0077(7) 0.0341(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O7 2.337(4) . ? Sm1 O1 2.341(4) . ? Sm1 O4 2.382(4) 2_556 ? Sm1 O16 2.479(5) . ? Sm1 O12 2.503(4) . ? Sm1 O10 2.506(5) . ? Sm1 O14 2.508(5) . ? Sm1 O13 2.524(5) . ? Sm1 O18 2.539(4) . ? Sm1 N1 2.924(6) . ? Sm1 N3 2.927(6) . ? Sm1 N2 2.945(6) . ? C1 C6 1.395(8) . ? C1 C2 1.411(8) . ? C1 C8 1.527(8) . ? C2 C3 1.403(8) . ? C2 C9 1.506(9) . ? C3 C4 1.398(8) . ? C3 C10 1.522(8) . ? C4 C5 1.394(8) . ? C4 C11 1.528(8) . ? C5 C6 1.413(8) . ? C5 C12 1.496(8) . ? C6 C7 1.505(8) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 P1 1.776(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 P2 1.779(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 O2 1.498(5) . ? C13 C14 1.527(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 O3 1.492(4) . ? C15 C16 1.532(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O5 1.479(5) . ? C17 C18 1.534(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O6 1.499(5) . ? C19 C20 1.518(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.529(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 O8 1.495(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.522(5) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 O9 1.493(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C28 1.539(8) . ? C25 P3 1.775(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.531(11) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.365(9) . ? C27 C29 1.395(9) 2_667 ? C28 C29 1.410(10) . ? C29 C27 1.395(9) 2_667 ? C29 C30 1.509(10) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.544(5) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 O19 1.505(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? N1 O11 1.215(8) . ? N1 O12 1.248(8) . ? N1 O10 1.256(8) . ? N2 O15 1.209(8) . ? N2 O14 1.242(7) . ? N2 O13 1.250(7) . ? N3 O17 1.197(7) . ? N3 O18 1.239(8) . ? N3 O16 1.253(8) . ? O1 P2 1.463(4) . ? O2 P2 1.542(5) . ? O3 P2 1.530(5) . ? O4 P1 1.472(4) . ? O4 Sm1 2.382(4) 2_556 ? O5 P1 1.560(5) . ? O6 P1 1.559(6) . ? O7 P3 1.480(4) . ? O8 P3 1.551(6) . ? O9 P3 1.552(5) . ? O19 H19 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Sm1 O1 150.97(16) . . ? O7 Sm1 O4 84.24(16) . 2_556 ? O1 Sm1 O4 81.92(15) . 2_556 ? O7 Sm1 O16 81.71(18) . . ? O1 Sm1 O16 86.64(17) . . ? O4 Sm1 O16 127.40(18) 2_556 . ? O7 Sm1 O12 74.02(16) . . ? O1 Sm1 O12 127.74(16) . . ? O4 Sm1 O12 79.76(16) 2_556 . ? O16 Sm1 O12 141.54(19) . . ? O7 Sm1 O10 123.90(16) . . ? O1 Sm1 O10 78.48(17) . . ? O4 Sm1 O10 80.00(17) 2_556 . ? O16 Sm1 O10 146.8(2) . . ? O12 Sm1 O10 50.34(17) . . ? O7 Sm1 O14 78.33(17) . . ? O1 Sm1 O14 122.70(16) . . ? O4 Sm1 O14 152.29(16) 2_556 . ? O16 Sm1 O14 71.3(2) . . ? O12 Sm1 O14 74.85(19) . . ? O10 Sm1 O14 92.0(2) . . ? O7 Sm1 O13 126.69(17) . . ? O1 Sm1 O13 73.69(15) . . ? O4 Sm1 O13 147.71(17) 2_556 . ? O16 Sm1 O13 72.6(2) . . ? O12 Sm1 O13 98.60(18) . . ? O10 Sm1 O13 74.71(19) . . ? O14 Sm1 O13 49.56(16) . . ? O7 Sm1 O18 76.62(14) . . ? O1 Sm1 O18 75.53(15) . . ? O4 Sm1 O18 77.46(15) 2_556 . ? O16 Sm1 O18 49.99(18) . . ? O12 Sm1 O18 144.27(17) . . ? O10 Sm1 O18 147.56(18) . . ? O14 Sm1 O18 118.36(19) . . ? O13 Sm1 O18 115.26(17) . . ? O7 Sm1 N1 98.81(18) . . ? O1 Sm1 N1 103.16(18) . . ? O4 Sm1 N1 78.27(16) 2_556 . ? O16 Sm1 N1 154.0(2) . . ? O12 Sm1 N1 25.08(16) . . ? O10 Sm1 N1 25.27(17) . . ? O14 Sm1 N1 83.3(2) . . ? O13 Sm1 N1 86.90(19) . . ? O18 Sm1 N1 155.63(18) . . ? O7 Sm1 N3 77.37(16) . . ? O1 Sm1 N3 80.84(15) . . ? O4 Sm1 N3 102.32(18) 2_556 . ? O16 Sm1 N3 25.09(18) . . ? O12 Sm1 N3 150.96(17) . . ? O10 Sm1 N3 158.65(17) . . ? O14 Sm1 N3 94.7(2) . . ? O13 Sm1 N3 94.5(2) . . ? O18 Sm1 N3 24.92(17) . . ? N1 Sm1 N3 176.01(18) . . ? O7 Sm1 N2 102.14(18) . . ? O1 Sm1 N2 98.11(16) . . ? O4 Sm1 N2 163.84(18) 2_556 . ? O16 Sm1 N2 68.6(2) . . ? O12 Sm1 N2 87.69(18) . . ? O10 Sm1 N2 84.2(2) . . ? O14 Sm1 N2 24.71(15) . . ? O13 Sm1 N2 24.93(16) . . ? O18 Sm1 N2 118.32(18) . . ? N1 Sm1 N2 86.04(19) . . ? N3 Sm1 N2 93.6(2) . . ? C6 C1 C2 120.4(5) . . ? C6 C1 C8 119.7(5) . . ? C2 C1 C8 119.9(6) . . ? C3 C2 C1 119.6(6) . . ? C3 C2 C9 119.2(6) . . ? C1 C2 C9 121.1(6) . . ? C4 C3 C2 119.9(5) . . ? C4 C3 C10 122.1(5) . . ? C2 C3 C10 118.0(6) . . ? C5 C4 C3 120.5(5) . . ? C5 C4 C11 119.8(5) . . ? C3 C4 C11 119.7(5) . . ? C4 C5 C6 120.0(5) . . ? C4 C5 C12 120.6(5) . . ? C6 C5 C12 119.4(5) . . ? C1 C6 C5 119.5(5) . . ? C1 C6 C7 119.8(5) . . ? C5 C6 C7 120.7(6) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 C8 P1 116.7(4) . . ? C1 C8 H8A 108.1 . . ? P1 C8 H8A 108.1 . . ? C1 C8 H8B 108.1 . . ? P1 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C3 C10 H10A 109.5 . . ? C3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C4 C11 P2 116.6(4) . . ? C4 C11 H11A 108.1 . . ? P2 C11 H11A 108.1 . . ? C4 C11 H11B 108.1 . . ? P2 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C5 C12 H12A 109.5 . . ? C5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 C14 91.3(13) . . ? O2 C13 H13A 113.4 . . ? C14 C13 H13A 113.4 . . ? O2 C13 H13B 113.4 . . ? C14 C13 H13B 113.4 . . ? H13A C13 H13B 110.7 . . ? C13 C14 H14A 110.1 . . ? C13 C14 H14B 108.1 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 110.2 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 C16 105.2(6) . . ? O3 C15 H15A 110.7 . . ? C16 C15 H15A 110.7 . . ? O3 C15 H15B 110.7 . . ? C16 C15 H15B 110.7 . . ? H15A C15 H15B 108.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 C18 102.7(6) . . ? O5 C17 H17A 111.2 . . ? C18 C17 H17A 111.2 . . ? O5 C17 H17B 111.2 . . ? C18 C17 H17B 111.2 . . ? H17A C17 H17B 109.1 . . ? 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 . . ? O6 C19 C20 101.2(9) . . ? O6 C19 H19A 112.3 . . ? C20 C19 H19A 111.6 . . ? O6 C19 H19B 111.0 . . ? C20 C19 H19B 111.4 . . ? H19A C19 H19B 109.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O8 C22 C21 108.8(9) . . ? O8 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? O8 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O9 C24 C23 107.2(9) . . ? O9 C24 H24A 110.3 . . ? C23 C24 H24A 110.3 . . ? O9 C24 H24B 110.3 . . ? C23 C24 H24B 110.3 . . ? H24A C24 H24B 108.5 . . ? C28 C25 P3 115.9(5) . . ? C28 C25 H25A 108.3 . . ? P3 C25 H25A 108.3 . . ? C28 C25 H25B 108.3 . . ? P3 C25 H25B 108.3 . . ? H25A C25 H25B 107.4 . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 120.4(6) . 2_667 ? C28 C27 C26 121.3(7) . . ? C29 C27 C26 118.3(7) 2_667 . ? C27 C28 C29 120.8(6) . . ? C27 C28 C25 120.8(7) . . ? C29 C28 C25 118.3(6) . . ? C27 C29 C28 118.8(6) 2_667 . ? C27 C29 C30 120.3(7) 2_667 . ? C28 C29 C30 120.9(7) . . ? 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 . . ? C32 C31 H31A 110.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 108.8 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O19 C32 C31 156(3) . . ? O19 C32 H32A 98.2 . . ? C31 C32 H32A 96.5 . . ? O19 C32 H32B 96.6 . . ? C31 C32 H32B 97.9 . . ? H32A C32 H32B 103.6 . . ? O11 N1 O12 122.7(7) . . ? O11 N1 O10 120.7(7) . . ? O12 N1 O10 116.6(6) . . ? O11 N1 Sm1 176.6(6) . . ? O12 N1 Sm1 58.2(3) . . ? O10 N1 Sm1 58.4(3) . . ? O15 N2 O14 123.1(7) . . ? O15 N2 O13 121.3(7) . . ? O14 N2 O13 115.5(6) . . ? O15 N2 Sm1 177.2(6) . . ? O14 N2 Sm1 57.5(3) . . ? O13 N2 Sm1 58.3(3) . . ? O17 N3 O18 121.5(8) . . ? O17 N3 O16 121.9(7) . . ? O18 N3 O16 116.7(6) . . ? O17 N3 Sm1 177.8(5) . . ? O18 N3 Sm1 59.7(3) . . ? O16 N3 Sm1 57.0(3) . . ? P2 O1 Sm1 156.6(3) . . ? C13 O2 P2 125.6(7) . . ? C15 O3 P2 123.7(5) . . ? P1 O4 Sm1 155.0(3) . 2_556 ? C17 O5 P1 122.0(4) . . ? C19 O6 P1 117.5(7) . . ? P3 O7 Sm1 152.7(3) . . ? C22 O8 P3 123.3(6) . . ? C24 O9 P3 120.4(6) . . ? N1 O10 Sm1 96.3(4) . . ? N1 O12 Sm1 96.7(4) . . ? N2 O13 Sm1 96.8(4) . . ? N2 O14 Sm1 97.8(4) . . ? N3 O16 Sm1 97.9(4) . . ? N3 O18 Sm1 95.4(4) . . ? C32 O19 H19 110.2 . . ? O4 P1 O6 113.2(3) . . ? O4 P1 O5 114.4(3) . . ? O6 P1 O5 102.8(3) . . ? O4 P1 C8 113.7(3) . . ? O6 P1 C8 105.5(3) . . ? O5 P1 C8 106.2(3) . . ? O1 P2 O3 114.9(3) . . ? O1 P2 O2 111.1(3) . . ? O3 P2 O2 106.1(4) . . ? O1 P2 C11 113.2(3) . . ? O3 P2 C11 104.0(3) . . ? O2 P2 C11 106.9(3) . . ? O7 P3 O8 111.6(3) . . ? O7 P3 O9 113.3(3) . . ? O8 P3 O9 107.3(3) . . ? O7 P3 C25 112.7(3) . . ? O8 P3 C25 105.1(3) . . ? O9 P3 C25 106.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.1(9) . . . . ? C8 C1 C2 C3 179.0(5) . . . . ? C6 C1 C2 C9 -178.6(6) . . . . ? C8 C1 C2 C9 0.3(9) . . . . ? C1 C2 C3 C4 -0.7(9) . . . . ? C9 C2 C3 C4 178.0(6) . . . . ? C1 C2 C3 C10 -179.0(6) . . . . ? C9 C2 C3 C10 -0.3(9) . . . . ? C2 C3 C4 C5 0.6(8) . . . . ? C10 C3 C4 C5 178.8(5) . . . . ? C2 C3 C4 C11 -179.8(5) . . . . ? C10 C3 C4 C11 -1.5(8) . . . . ? C3 C4 C5 C6 0.1(8) . . . . ? C11 C4 C5 C6 -179.5(5) . . . . ? C3 C4 C5 C12 -179.7(5) . . . . ? C11 C4 C5 C12 0.7(8) . . . . ? C2 C1 C6 C5 0.6(8) . . . . ? C8 C1 C6 C5 -178.3(5) . . . . ? C2 C1 C6 C7 178.3(6) . . . . ? C8 C1 C6 C7 -0.6(8) . . . . ? C4 C5 C6 C1 -0.7(8) . . . . ? C12 C5 C6 C1 179.1(5) . . . . ? C4 C5 C6 C7 -178.4(5) . . . . ? C12 C5 C6 C7 1.4(8) . . . . ? C6 C1 C8 P1 -91.1(7) . . . . ? C2 C1 C8 P1 89.9(6) . . . . ? C5 C4 C11 P2 -92.9(6) . . . . ? C3 C4 C11 P2 87.5(6) . . . . ? C29 C27 C28 C29 -1.3(13) 2_667 . . . ? C26 C27 C28 C29 176.7(8) . . . . ? C29 C27 C28 C25 -179.3(7) 2_667 . . . ? C26 C27 C28 C25 -1.3(11) . . . . ? P3 C25 C28 C27 -90.8(8) . . . . ? P3 C25 C28 C29 91.2(8) . . . . ? C27 C28 C29 C27 1.3(12) . . . 2_667 ? C25 C28 C29 C27 179.4(6) . . . 2_667 ? C27 C28 C29 C30 -179.4(8) . . . . ? C25 C28 C29 C30 -1.3(11) . . . . ? O7 Sm1 N1 O11 -98(11) . . . . ? O1 Sm1 N1 O11 63(11) . . . . ? O4 Sm1 N1 O11 -16(11) 2_556 . . . ? O16 Sm1 N1 O11 173(10) . . . . ? O12 Sm1 N1 O11 -107(11) . . . . ? O10 Sm1 N1 O11 75(11) . . . . ? O14 Sm1 N1 O11 -175(11) . . . . ? O13 Sm1 N1 O11 135(11) . . . . ? O18 Sm1 N1 O11 -21(11) . . . . ? N3 Sm1 N1 O11 -115(10) . . . . ? N2 Sm1 N1 O11 160(11) . . . . ? O7 Sm1 N1 O12 8.7(4) . . . . ? O1 Sm1 N1 O12 169.6(4) . . . . ? O4 Sm1 N1 O12 90.9(4) 2_556 . . . ? O16 Sm1 N1 O12 -80.4(6) . . . . ? O10 Sm1 N1 O12 -177.7(7) . . . . ? O14 Sm1 N1 O12 -68.3(4) . . . . ? O13 Sm1 N1 O12 -118.0(4) . . . . ? O18 Sm1 N1 O12 85.7(6) . . . . ? N3 Sm1 N1 O12 -8(3) . . . . ? N2 Sm1 N1 O12 -93.0(4) . . . . ? O7 Sm1 N1 O10 -173.6(4) . . . . ? O1 Sm1 N1 O10 -12.7(5) . . . . ? O4 Sm1 N1 O10 -91.4(4) 2_556 . . . ? O16 Sm1 N1 O10 97.3(6) . . . . ? O12 Sm1 N1 O10 177.7(7) . . . . ? O14 Sm1 N1 O10 109.4(4) . . . . ? O13 Sm1 N1 O10 59.8(4) . . . . ? O18 Sm1 N1 O10 -96.6(6) . . . . ? N3 Sm1 N1 O10 170(3) . . . . ? N2 Sm1 N1 O10 84.7(4) . . . . ? O7 Sm1 N2 O15 88(12) . . . . ? O1 Sm1 N2 O15 -71(12) . . . . ? O4 Sm1 N2 O15 -160(12) 2_556 . . . ? O16 Sm1 N2 O15 12(12) . . . . ? O12 Sm1 N2 O15 161(12) . . . . ? O10 Sm1 N2 O15 -148(12) . . . . ? O14 Sm1 N2 O15 104(12) . . . . ? O13 Sm1 N2 O15 -82(12) . . . . ? O18 Sm1 N2 O15 7(12) . . . . ? N1 Sm1 N2 O15 -173(12) . . . . ? N3 Sm1 N2 O15 11(12) . . . . ? O7 Sm1 N2 O14 -15.7(5) . . . . ? O1 Sm1 N2 O14 -174.8(5) . . . . ? O4 Sm1 N2 O14 96.3(7) 2_556 . . . ? O16 Sm1 N2 O14 -91.6(5) . . . . ? O12 Sm1 N2 O14 57.4(5) . . . . ? O10 Sm1 N2 O14 107.8(5) . . . . ? O13 Sm1 N2 O14 173.6(8) . . . . ? O18 Sm1 N2 O14 -96.9(5) . . . . ? N1 Sm1 N2 O14 82.5(5) . . . . ? N3 Sm1 N2 O14 -93.5(5) . . . . ? O7 Sm1 N2 O13 170.7(4) . . . . ? O1 Sm1 N2 O13 11.6(5) . . . . ? O4 Sm1 N2 O13 -77.4(7) 2_556 . . . ? O16 Sm1 N2 O13 94.7(5) . . . . ? O12 Sm1 N2 O13 -116.2(5) . . . . ? O10 Sm1 N2 O13 -65.8(5) . . . . ? O14 Sm1 N2 O13 -173.6(8) . . . . ? O18 Sm1 N2 O13 89.5(5) . . . . ? N1 Sm1 N2 O13 -91.1(5) . . . . ? N3 Sm1 N2 O13 92.8(5) . . . . ? O7 Sm1 N3 O17 -37(16) . . . . ? O1 Sm1 N3 O17 162(16) . . . . ? O4 Sm1 N3 O17 -119(16) 2_556 . . . ? O16 Sm1 N3 O17 60(16) . . . . ? O12 Sm1 N3 O17 -27(17) . . . . ? O10 Sm1 N3 O17 147(16) . . . . ? O14 Sm1 N3 O17 40(16) . . . . ? O13 Sm1 N3 O17 89(16) . . . . ? O18 Sm1 N3 O17 -123(16) . . . . ? N1 Sm1 N3 O17 -21(18) . . . . ? N2 Sm1 N3 O17 64(16) . . . . ? O7 Sm1 N3 O18 85.4(4) . . . . ? O1 Sm1 N3 O18 -75.3(4) . . . . ? O4 Sm1 N3 O18 4.3(4) 2_556 . . . ? O16 Sm1 N3 O18 -177.1(6) . . . . ? O12 Sm1 N3 O18 95.3(5) . . . . ? O10 Sm1 N3 O18 -89.8(7) . . . . ? O14 Sm1 N3 O18 162.3(4) . . . . ? O13 Sm1 N3 O18 -148.0(4) . . . . ? N1 Sm1 N3 O18 102(3) . . . . ? N2 Sm1 N3 O18 -173.0(4) . . . . ? O7 Sm1 N3 O16 -97.5(4) . . . . ? O1 Sm1 N3 O16 101.8(4) . . . . ? O4 Sm1 N3 O16 -178.6(4) 2_556 . . . ? O12 Sm1 N3 O16 -87.6(6) . . . . ? O10 Sm1 N3 O16 87.4(7) . . . . ? O14 Sm1 N3 O16 -20.6(4) . . . . ? O13 Sm1 N3 O16 29.1(4) . . . . ? O18 Sm1 N3 O16 177.1(6) . . . . ? N1 Sm1 N3 O16 -81(3) . . . . ? N2 Sm1 N3 O16 4.2(4) . . . . ? O7 Sm1 O1 P2 -30.9(9) . . . . ? O4 Sm1 O1 P2 -93.3(7) 2_556 . . . ? O16 Sm1 O1 P2 35.3(7) . . . . ? O12 Sm1 O1 P2 -163.6(6) . . . . ? O10 Sm1 O1 P2 -174.6(7) . . . . ? O14 Sm1 O1 P2 100.5(7) . . . . ? O13 Sm1 O1 P2 108.1(7) . . . . ? O18 Sm1 O1 P2 -14.2(7) . . . . ? N1 Sm1 O1 P2 -169.1(7) . . . . ? N3 Sm1 O1 P2 10.7(7) . . . . ? N2 Sm1 O1 P2 103.1(7) . . . . ? C14 C13 O2 P2 -111.0(14) . . . . ? C16 C15 O3 P2 143.1(6) . . . . ? C18 C17 O5 P1 -158.0(7) . . . . ? C20 C19 O6 P1 157.3(11) . . . . ? O1 Sm1 O7 P3 157.9(5) . . . . ? O4 Sm1 O7 P3 -140.3(6) 2_556 . . . ? O16 Sm1 O7 P3 90.5(6) . . . . ? O12 Sm1 O7 P3 -59.4(6) . . . . ? O10 Sm1 O7 P3 -66.5(7) . . . . ? O14 Sm1 O7 P3 18.0(6) . . . . ? O13 Sm1 O7 P3 29.5(7) . . . . ? O18 Sm1 O7 P3 141.2(7) . . . . ? N1 Sm1 O7 P3 -63.2(7) . . . . ? N3 Sm1 O7 P3 115.6(7) . . . . ? N2 Sm1 O7 P3 24.6(7) . . . . ? C21 C22 O8 P3 176.3(9) . . . . ? C23 C24 O9 P3 160.2(9) . . . . ? O11 N1 O10 Sm1 -176.2(7) . . . . ? O12 N1 O10 Sm1 2.2(7) . . . . ? O7 Sm1 O10 N1 7.6(5) . . . . ? O1 Sm1 O10 N1 167.4(5) . . . . ? O4 Sm1 O10 N1 83.7(4) 2_556 . . . ? O16 Sm1 O10 N1 -127.5(5) . . . . ? O12 Sm1 O10 N1 -1.3(4) . . . . ? O14 Sm1 O10 N1 -69.6(4) . . . . ? O13 Sm1 O10 N1 -116.6(5) . . . . ? O18 Sm1 O10 N1 130.2(4) . . . . ? N3 Sm1 O10 N1 -178.1(5) . . . . ? N2 Sm1 O10 N1 -93.1(4) . . . . ? O11 N1 O12 Sm1 176.1(7) . . . . ? O10 N1 O12 Sm1 -2.2(7) . . . . ? O7 Sm1 O12 N1 -171.1(5) . . . . ? O1 Sm1 O12 N1 -12.9(5) . . . . ? O4 Sm1 O12 N1 -84.2(4) 2_556 . . . ? O16 Sm1 O12 N1 135.9(4) . . . . ? O10 Sm1 O12 N1 1.3(4) . . . . ? O14 Sm1 O12 N1 107.0(4) . . . . ? O13 Sm1 O12 N1 63.1(4) . . . . ? O18 Sm1 O12 N1 -135.2(4) . . . . ? N3 Sm1 O12 N1 178.9(4) . . . . ? N2 Sm1 O12 N1 85.6(4) . . . . ? O15 N2 O13 Sm1 176.8(7) . . . . ? O14 N2 O13 Sm1 -5.9(7) . . . . ? O7 Sm1 O13 N2 -11.4(5) . . . . ? O1 Sm1 O13 N2 -168.0(5) . . . . ? O4 Sm1 O13 N2 149.5(4) 2_556 . . . ? O16 Sm1 O13 N2 -76.5(5) . . . . ? O12 Sm1 O13 N2 65.0(5) . . . . ? O10 Sm1 O13 N2 109.8(5) . . . . ? O14 Sm1 O13 N2 3.5(4) . . . . ? O18 Sm1 O13 N2 -103.3(4) . . . . ? N1 Sm1 O13 N2 87.3(5) . . . . ? N3 Sm1 O13 N2 -88.9(5) . . . . ? O15 N2 O14 Sm1 -176.8(8) . . . . ? O13 N2 O14 Sm1 6.0(7) . . . . ? O7 Sm1 O14 N2 164.4(5) . . . . ? O1 Sm1 O14 N2 6.2(6) . . . . ? O4 Sm1 O14 N2 -143.5(4) 2_556 . . . ? O16 Sm1 O14 N2 79.3(5) . . . . ? O12 Sm1 O14 N2 -119.3(5) . . . . ? O10 Sm1 O14 N2 -71.4(5) . . . . ? O13 Sm1 O14 N2 -3.5(4) . . . . ? O18 Sm1 O14 N2 96.7(5) . . . . ? N1 Sm1 O14 N2 -95.2(5) . . . . ? N3 Sm1 O14 N2 88.3(5) . . . . ? O17 N3 O16 Sm1 -177.7(6) . . . . ? O18 N3 O16 Sm1 2.8(6) . . . . ? O7 Sm1 O16 N3 77.9(4) . . . . ? O1 Sm1 O16 N3 -75.5(4) . . . . ? O4 Sm1 O16 N3 1.7(5) 2_556 . . . ? O12 Sm1 O16 N3 128.8(4) . . . . ? O10 Sm1 O16 N3 -138.4(4) . . . . ? O14 Sm1 O16 N3 158.3(5) . . . . ? O13 Sm1 O16 N3 -149.4(4) . . . . ? O18 Sm1 O16 N3 -1.6(4) . . . . ? N1 Sm1 O16 N3 171.0(4) . . . . ? N2 Sm1 O16 N3 -175.5(5) . . . . ? O17 N3 O18 Sm1 177.8(6) . . . . ? O16 N3 O18 Sm1 -2.7(6) . . . . ? O7 Sm1 O18 N3 -88.8(4) . . . . ? O1 Sm1 O18 N3 99.5(4) . . . . ? O4 Sm1 O18 N3 -175.7(4) 2_556 . . . ? O16 Sm1 O18 N3 1.6(4) . . . . ? O12 Sm1 O18 N3 -124.1(4) . . . . ? O10 Sm1 O18 N3 137.2(4) . . . . ? O14 Sm1 O18 N3 -20.1(4) . . . . ? O13 Sm1 O18 N3 35.8(4) . . . . ? N1 Sm1 O18 N3 -170.5(4) . . . . ? N2 Sm1 O18 N3 8.0(4) . . . . ? Sm1 O4 P1 O6 -61.5(7) 2_556 . . . ? Sm1 O4 P1 O5 55.9(7) 2_556 . . . ? Sm1 O4 P1 C8 178.2(6) 2_556 . . . ? C19 O6 P1 O4 96.7(11) . . . . ? C19 O6 P1 O5 -27.3(11) . . . . ? C19 O6 P1 C8 -138.5(10) . . . . ? C17 O5 P1 O4 43.2(7) . . . . ? C17 O5 P1 O6 166.4(6) . . . . ? C17 O5 P1 C8 -83.0(6) . . . . ? C1 C8 P1 O4 57.1(6) . . . . ? C1 C8 P1 O6 -67.5(6) . . . . ? C1 C8 P1 O5 -176.2(5) . . . . ? Sm1 O1 P2 O3 -58.3(8) . . . . ? Sm1 O1 P2 O2 -178.8(6) . . . . ? Sm1 O1 P2 C11 61.0(8) . . . . ? C15 O3 P2 O1 -44.3(7) . . . . ? C15 O3 P2 O2 78.9(7) . . . . ? C15 O3 P2 C11 -168.6(6) . . . . ? C13 O2 P2 O1 30.5(11) . . . . ? C13 O2 P2 O3 -95.1(10) . . . . ? C13 O2 P2 C11 154.4(10) . . . . ? C4 C11 P2 O1 -166.8(4) . . . . ? C4 C11 P2 O3 -41.4(6) . . . . ? C4 C11 P2 O2 70.6(6) . . . . ? Sm1 O7 P3 O8 141.2(6) . . . . ? Sm1 O7 P3 O9 -97.6(7) . . . . ? Sm1 O7 P3 C25 23.1(8) . . . . ? C22 O8 P3 O7 50.9(9) . . . . ? C22 O8 P3 O9 -73.8(8) . . . . ? C22 O8 P3 C25 173.4(8) . . . . ? C24 O9 P3 O7 -38.3(8) . . . . ? C24 O9 P3 O8 85.4(8) . . . . ? C24 O9 P3 C25 -162.6(8) . . . . ? C28 C25 P3 O7 -176.4(5) . . . . ? C28 C25 P3 O8 61.8(7) . . . . ? C28 C25 P3 O9 -51.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.833 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.108