# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Zheng, Zhiping' _publ_contact_author_email zhiping@u.arizona.edu loop_ _publ_author_name Z.Zheng Y.Wu S.Morton X.-J.Kong data_Pr2 _database_code_depnum_ccdc_archive 'CCDC 778769' #TrackingRef '- Pr2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H21 O7 Pr' _chemical_formula_sum 'C13 H21 O7 Pr' _chemical_formula_weight 430.21 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9046(11) _cell_length_b 10.4942(17) _cell_length_c 12.242(2) _cell_angle_alpha 72.367(2) _cell_angle_beta 87.269(2) _cell_angle_gamma 76.238(3) _cell_volume 820.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5395 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 33.99 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 428 _exptl_absorpt_coefficient_mu 2.995 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3626 _exptl_absorpt_correction_T_max 0.8671 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube with Miracol optics' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEXII DUO CCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7987 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 33.99 _reflns_number_total 5241 _reflns_number_gt 4813 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction SAINT _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement SHELXTL _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 1999)' _computing_publication_material 'SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5241 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Pr1 Pr 0.243491(17) 0.039048(12) 0.384677(9) 0.01052(4) Uani 1 1 d . . . O1 O 0.0826(3) 0.17118(19) 0.19754(15) 0.0187(3) Uani 1 1 d . . . O2 O 0.3149(3) -0.09644(19) 0.25456(15) 0.0176(3) Uani 1 1 d . . . O3 O 0.0625(3) 0.27089(18) 0.39343(15) 0.0159(3) Uani 1 1 d . . . O4 O 0.4361(3) 0.19982(19) 0.28788(16) 0.0187(3) Uani 1 1 d . . . O5 O 0.6153(2) -0.06536(18) 0.42668(14) 0.0136(3) Uani 1 1 d . . . O6 O 0.9083(2) -0.01540(17) 0.41159(14) 0.0136(3) Uani 1 1 d . . . O7 O 0.2850(3) -0.21183(18) 0.50276(15) 0.0176(3) Uani 1 1 d . . . H7O H 0.1790 -0.2339 0.5289 0.021 Uiso 1 1 calc R . . C1 C 0.0485(5) 0.3010(3) 0.0017(2) 0.0299(6) Uani 1 1 d . . . H1A H -0.0930 0.3392 0.0114 0.045 Uiso 1 1 calc R . . H1B H 0.0659 0.2834 -0.0728 0.045 Uiso 1 1 calc R . . H1C H 0.1262 0.3667 0.0051 0.045 Uiso 1 1 calc R . . C2 C 0.1199(4) 0.1679(3) 0.0962(2) 0.0189(5) Uani 1 1 d . . . C3 C 0.2219(4) 0.0497(3) 0.0670(2) 0.0221(5) Uani 1 1 d . . . H3 H 0.2342 0.0561 -0.0120 0.026 Uiso 1 1 calc R . . C4 C 0.3056(4) -0.0755(3) 0.1469(2) 0.0183(5) Uani 1 1 d . . . C5 C 0.3939(5) -0.1984(3) 0.1057(3) 0.0280(6) Uani 1 1 d . . . H5A H 0.5275 -0.2426 0.1404 0.042 Uiso 1 1 calc R . . H5B H 0.4030 -0.1682 0.0221 0.042 Uiso 1 1 calc R . . H5C H 0.3087 -0.2641 0.1281 0.042 Uiso 1 1 calc R . . C6 C -0.0868(5) 0.5099(3) 0.3492(3) 0.0259(6) Uani 1 1 d . . . H6A H -0.2033 0.5150 0.3040 0.039 Uiso 1 1 calc R . . H6B H -0.0432 0.5962 0.3204 0.039 Uiso 1 1 calc R . . H6C H -0.1223 0.4952 0.4298 0.039 Uiso 1 1 calc R . . C7 C 0.0811(4) 0.3914(3) 0.3390(2) 0.0176(4) Uani 1 1 d . . . C8 C 0.2406(4) 0.4237(3) 0.2697(2) 0.0207(5) Uani 1 1 d . . . H8 H 0.2357 0.5184 0.2339 0.025 Uiso 1 1 calc R . . C9 C 0.4072(4) 0.3284(3) 0.2484(2) 0.0181(4) Uani 1 1 d . . . C10 C 0.5664(5) 0.3814(3) 0.1696(3) 0.0279(6) Uani 1 1 d . . . H10A H 0.6987 0.3326 0.2045 0.042 Uiso 1 1 calc R . . H10B H 0.5478 0.4802 0.1582 0.042 Uiso 1 1 calc R . . H10C H 0.5553 0.3657 0.0955 0.042 Uiso 1 1 calc R . . C11 C 0.7666(3) -0.0439(2) 0.36809(19) 0.0124(4) Uani 1 1 d . . . C12 C 0.7826(4) -0.0539(3) 0.2479(2) 0.0193(5) Uani 1 1 d . . . H12A H 0.7179 -0.1253 0.2421 0.029 Uiso 1 1 calc R . . H12B H 0.9236 -0.0775 0.2290 0.029 Uiso 1 1 calc R . . H12C H 0.7168 0.0347 0.1941 0.029 Uiso 1 1 calc R . . C13 C 0.4188(4) -0.3270(3) 0.4795(2) 0.0227(5) Uani 1 1 d . . . H13A H 0.3540 -0.3578 0.4259 0.034 Uiso 1 1 calc R . . H13B H 0.4542 -0.4021 0.5512 0.034 Uiso 1 1 calc R . . H13C H 0.5398 -0.2999 0.4455 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.00976(6) 0.01461(6) 0.00727(6) -0.00340(4) 0.00105(4) -0.00299(4) O1 0.0191(9) 0.0246(9) 0.0116(8) -0.0056(7) -0.0001(6) -0.0033(7) O2 0.0194(9) 0.0223(9) 0.0133(8) -0.0081(7) 0.0022(6) -0.0058(7) O3 0.0157(8) 0.0177(8) 0.0136(7) -0.0041(6) 0.0019(6) -0.0035(6) O4 0.0158(8) 0.0195(8) 0.0189(8) -0.0020(7) 0.0023(6) -0.0059(6) O5 0.0108(7) 0.0196(8) 0.0108(7) -0.0056(6) 0.0020(5) -0.0034(6) O6 0.0115(7) 0.0189(8) 0.0113(7) -0.0048(6) 0.0008(6) -0.0046(6) O7 0.0144(8) 0.0163(8) 0.0200(8) -0.0045(7) 0.0047(6) -0.0020(6) C1 0.0291(15) 0.0359(16) 0.0148(12) 0.0017(11) 0.0000(10) -0.0012(12) C2 0.0157(11) 0.0280(13) 0.0124(10) -0.0038(9) -0.0001(8) -0.0070(9) C3 0.0253(13) 0.0333(14) 0.0102(10) -0.0087(10) 0.0033(9) -0.0094(11) C4 0.0191(11) 0.0262(12) 0.0150(10) -0.0104(9) 0.0041(8) -0.0110(9) C5 0.0387(17) 0.0299(14) 0.0231(13) -0.0167(11) 0.0122(11) -0.0136(12) C6 0.0292(14) 0.0175(12) 0.0267(13) -0.0049(10) 0.0048(11) -0.0001(10) C7 0.0186(11) 0.0184(11) 0.0140(10) -0.0028(9) -0.0004(8) -0.0032(9) C8 0.0215(12) 0.0169(11) 0.0211(12) -0.0012(9) 0.0030(9) -0.0062(9) C9 0.0187(11) 0.0219(11) 0.0143(10) -0.0040(9) 0.0003(8) -0.0079(9) C10 0.0263(14) 0.0268(14) 0.0278(14) -0.0022(11) 0.0100(11) -0.0107(11) C11 0.0129(10) 0.0144(9) 0.0096(9) -0.0042(7) 0.0013(7) -0.0017(8) C12 0.0176(11) 0.0323(13) 0.0129(10) -0.0114(10) 0.0039(8) -0.0094(10) C13 0.0230(13) 0.0178(11) 0.0250(13) -0.0076(10) 0.0058(10) -0.0002(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 Pr1 O1 2.4476(18) . ? Pr1 O2 2.4011(17) . ? Pr1 O3 2.4883(18) . ? Pr1 O4 2.3929(18) . ? Pr1 O5 2.5496(17) . ? Pr1 O5 2.6625(16) 2_656 ? Pr1 O6 2.4967(17) 1_455 ? Pr1 O6 2.6230(16) 2_656 ? Pr1 O7 2.5452(18) . ? Pr1 C11 3.040(2) 2_656 ? O1 C2 1.264(3) . ? O2 C4 1.272(3) . ? O3 C7 1.272(3) . ? O4 C9 1.257(3) . ? O5 Pr1 2.6625(16) 2_656 ? O5 C11 1.265(3) . ? O6 Pr1 2.4967(17) 1_655 ? O6 Pr1 2.6230(16) 2_656 ? O6 C11 1.271(3) . ? O7 H7O 0.840 . ? O7 C13 1.431(3) . ? C1 H1A 0.980 . ? C1 H1B 0.980 . ? C1 H1C 0.980 . ? C1 C2 1.510(4) . ? C2 C3 1.411(4) . ? C3 H3 0.950 . ? C3 C4 1.389(4) . ? C4 C5 1.509(4) . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C6 C7 1.517(4) . ? C7 C8 1.401(4) . ? C8 H8 0.950 . ? C8 C9 1.405(4) . ? C9 C10 1.521(4) . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 Pr1 3.040(2) 2_656 ? C11 C12 1.504(3) . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 H13A 0.980 . ? C13 H13B 0.980 . ? C13 H13C 0.980 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pr1 O2 69.93(6) . . ? O1 Pr1 O3 71.34(6) . . ? O1 Pr1 O4 71.92(6) . . ? O1 Pr1 O5 126.87(6) . . ? O1 Pr1 O5 142.83(6) . 2_656 ? O1 Pr1 O6 78.84(6) . 1_455 ? O1 Pr1 O6 128.21(6) . 2_656 ? O1 Pr1 O7 131.94(6) . . ? O1 Pr1 C11 140.47(6) . 2_656 ? O2 Pr1 O3 141.27(6) . . ? O2 Pr1 O4 95.40(6) . . ? O2 Pr1 O5 79.34(6) . . ? O2 Pr1 O5 141.96(6) . 2_656 ? O2 Pr1 O6 88.28(6) . 1_455 ? O2 Pr1 O6 137.28(6) . 2_656 ? O2 Pr1 O7 72.51(6) . . ? O2 Pr1 C11 147.42(6) . 2_656 ? O3 Pr1 O4 71.97(6) . . ? O3 Pr1 O5 125.47(6) . . ? O3 Pr1 O5 74.59(5) . 2_656 ? O3 Pr1 O6 84.82(6) . 1_455 ? O3 Pr1 O6 71.08(5) . 2_656 ? O3 Pr1 O7 138.80(6) . . ? O3 Pr1 C11 70.44(6) . 2_656 ? O4 Pr1 O5 69.03(6) . . ? O4 Pr1 O5 83.89(6) . 2_656 ? O4 Pr1 O6 147.12(6) . 1_455 ? O4 Pr1 O6 125.97(6) . 2_656 ? O4 Pr1 O7 140.99(6) . . ? O4 Pr1 C11 104.98(6) . 2_656 ? O5 Pr1 O5 64.84(6) . 2_656 ? O5 Pr1 O6 143.33(6) . 1_455 ? O5 Pr1 O6 103.85(5) . 2_656 ? O5 Pr1 O6 112.56(5) 2_656 1_455 ? O5 Pr1 O6 49.04(5) 2_656 2_656 ? O5 Pr1 O7 72.28(6) . . ? O5 Pr1 O7 84.27(6) 2_656 . ? O5 Pr1 C11 84.50(6) . 2_656 ? O5 Pr1 C11 24.50(6) 2_656 2_656 ? O6 Pr1 O6 63.52(6) 1_455 2_656 ? O6 Pr1 O7 71.09(6) 1_455 . ? O6 Pr1 O7 68.36(5) 2_656 . ? O6 Pr1 C11 88.06(6) 1_455 2_656 ? O6 Pr1 C11 24.55(6) 2_656 2_656 ? O7 Pr1 C11 75.69(6) . 2_656 ? Pr1 O1 C2 133.82(17) . . ? Pr1 O2 C4 137.20(17) . . ? Pr1 O3 C7 132.36(16) . . ? Pr1 O4 C9 136.43(17) . . ? Pr1 O5 Pr1 115.15(6) . 2_656 ? Pr1 O5 C11 131.65(15) . . ? Pr1 O5 C11 94.69(13) 2_656 . ? Pr1 O6 Pr1 116.48(6) 1_655 2_656 ? Pr1 O6 C11 147.05(14) 1_655 . ? Pr1 O6 C11 96.41(13) 2_656 . ? Pr1 O7 H7O 115.0 . . ? Pr1 O7 C13 125.82(15) . . ? H7O O7 C13 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1A C1 C2 109.5 . . ? H1B C1 H1C 109.5 . . ? H1B C1 C2 109.5 . . ? H1C C1 C2 109.5 . . ? O1 C2 C1 116.5(2) . . ? O1 C2 C3 124.5(2) . . ? C1 C2 C3 119.0(2) . . ? C2 C3 H3 118.0 . . ? C2 C3 C4 124.0(2) . . ? H3 C3 C4 118.0 . . ? O2 C4 C3 125.0(2) . . ? O2 C4 C5 115.9(2) . . ? C3 C4 C5 119.1(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6A C6 C7 109.5 . . ? H6B C6 H6C 109.5 . . ? H6B C6 C7 109.5 . . ? H6C C6 C7 109.5 . . ? O3 C7 C6 116.6(2) . . ? O3 C7 C8 125.9(2) . . ? C6 C7 C8 117.5(2) . . ? C7 C8 H8 117.1 . . ? C7 C8 C9 125.7(2) . . ? H8 C8 C9 117.1 . . ? O4 C9 C8 125.3(2) . . ? O4 C9 C10 115.8(2) . . ? C8 C9 C10 118.9(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Pr1 C11 O5 60.81(11) 2_656 . ? Pr1 C11 O6 59.04(11) 2_656 . ? Pr1 C11 C12 176.43(17) 2_656 . ? O5 C11 O6 119.8(2) . . ? O5 C11 C12 120.8(2) . . ? O6 C11 C12 119.4(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O7 C13 H13A 109.5 . . ? O7 C13 H13B 109.5 . . ? O7 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 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 O2 Pr1 O1 C2 -26.4(2) . . . . ? O3 Pr1 O1 C2 153.1(2) . . . . ? O4 Pr1 O1 C2 76.6(2) . . . . ? O5 Pr1 O1 C2 32.2(3) . . . . ? O5 Pr1 O1 C2 128.5(2) 2_656 . . . ? O6 Pr1 O1 C2 -118.7(2) 1_455 . . . ? O6 Pr1 O1 C2 -161.5(2) 2_656 . . . ? O7 Pr1 O1 C2 -67.1(3) . . . . ? C11 Pr1 O1 C2 168.4(2) 2_656 . . . ? O1 Pr1 O2 C4 16.5(2) . . . . ? O3 Pr1 O2 C4 15.7(3) . . . . ? O4 Pr1 O2 C4 -52.0(2) . . . . ? O5 Pr1 O2 C4 -119.4(2) . . . . ? O5 Pr1 O2 C4 -139.0(2) 2_656 . . . ? O6 Pr1 O2 C4 95.3(2) 1_455 . . . ? O6 Pr1 O2 C4 141.6(2) 2_656 . . . ? O7 Pr1 O2 C4 166.0(2) . . . . ? C11 Pr1 O2 C4 179.0(2) 2_656 . . . ? O1 Pr1 O3 C7 -61.6(2) . . . . ? O2 Pr1 O3 C7 -60.8(2) . . . . ? O4 Pr1 O3 C7 14.9(2) . . . . ? O5 Pr1 O3 C7 60.9(2) . . . . ? O5 Pr1 O3 C7 103.4(2) 2_656 . . . ? O6 Pr1 O3 C7 -141.5(2) 1_455 . . . ? O6 Pr1 O3 C7 154.7(2) 2_656 . . . ? O7 Pr1 O3 C7 165.2(2) . . . . ? C11 Pr1 O3 C7 128.7(2) 2_656 . . . ? O1 Pr1 O4 C9 60.5(2) . . . . ? O2 Pr1 O4 C9 127.3(2) . . . . ? O3 Pr1 O4 C9 -15.2(2) . . . . ? O5 Pr1 O4 C9 -156.3(3) . . . . ? O5 Pr1 O4 C9 -90.9(2) 2_656 . . . ? O6 Pr1 O4 C9 32.1(3) 1_455 . . . ? O6 Pr1 O4 C9 -64.1(3) 2_656 . . . ? O7 Pr1 O4 C9 -164.0(2) . . . . ? C11 Pr1 O4 C9 -78.3(2) 2_656 . . . ? O1 Pr1 O5 Pr1 138.44(7) . . . 2_656 ? O1 Pr1 O5 C11 15.8(2) . . . . ? O2 Pr1 O5 Pr1 -166.84(8) . . . 2_656 ? O2 Pr1 O5 C11 70.57(19) . . . . ? O3 Pr1 O5 Pr1 45.95(9) . . . 2_656 ? O3 Pr1 O5 C11 -76.6(2) . . . . ? O4 Pr1 O5 Pr1 93.10(8) . . . 2_656 ? O4 Pr1 O5 C11 -29.48(19) . . . . ? O5 Pr1 O5 Pr1 0.0 2_656 . . 2_656 ? O5 Pr1 O5 C11 -122.6(2) 2_656 . . . ? O6 Pr1 O5 Pr1 -94.52(10) 1_455 . . 2_656 ? O6 Pr1 O5 Pr1 -30.49(8) 2_656 . . 2_656 ? O6 Pr1 O5 C11 142.89(18) 1_455 . . . ? O6 Pr1 O5 C11 -153.08(19) 2_656 . . . ? O7 Pr1 O5 Pr1 -91.96(7) . . . 2_656 ? O7 Pr1 O5 C11 145.4(2) . . . . ? C11 Pr1 O5 Pr1 -15.26(7) 2_656 . . 2_656 ? C11 Pr1 O5 C11 -137.85(17) 2_656 . . . ? O1 Pr1 O7 C13 74.1(2) . . . . ? O2 Pr1 O7 C13 34.20(19) . . . . ? O3 Pr1 O7 C13 -173.95(18) . . . . ? O4 Pr1 O7 C13 -42.4(2) . . . . ? O5 Pr1 O7 C13 -49.90(19) . . . . ? O5 Pr1 O7 C13 -115.3(2) 2_656 . . . ? O6 Pr1 O7 C13 128.5(2) 1_455 . . . ? O6 Pr1 O7 C13 -163.3(2) 2_656 . . . ? C11 Pr1 O7 C13 -138.6(2) 2_656 . . . ? Pr1 O1 C2 C1 -152.7(2) . . . . ? Pr1 O1 C2 C3 27.4(4) . . . . ? O1 C2 C3 C4 -4.5(4) . . . . ? C1 C2 C3 C4 175.6(3) . . . . ? Pr1 O2 C4 C3 -7.0(4) . . . . ? Pr1 O2 C4 C5 172.86(18) . . . . ? C2 C3 C4 O2 -5.9(4) . . . . ? C2 C3 C4 C5 174.2(3) . . . . ? Pr1 O3 C7 C6 166.85(17) . . . . ? Pr1 O3 C7 C8 -12.2(4) . . . . ? O3 C7 C8 C9 0.1(4) . . . . ? C6 C7 C8 C9 -179.0(3) . . . . ? Pr1 O4 C9 C8 12.0(4) . . . . ? Pr1 O4 C9 C10 -166.73(19) . . . . ? C7 C8 C9 O4 0.7(4) . . . . ? C7 C8 C9 C10 179.4(3) . . . . ? Pr1 O5 C11 Pr1 130.07(18) . . . 2_656 ? Pr1 O5 C11 O6 127.31(19) . . . . ? Pr1 O5 C11 O6 -2.8(2) 2_656 . . . ? Pr1 O5 C11 C12 -53.6(3) . . . . ? Pr1 O5 C11 C12 176.3(2) 2_656 . . . ? Pr1 O6 C11 Pr1 176.5(3) 1_655 . . 2_656 ? Pr1 O6 C11 O5 179.31(17) 1_655 . . . ? Pr1 O6 C11 O5 2.8(2) 2_656 . . . ? Pr1 O6 C11 C12 0.2(4) 1_655 . . . ? Pr1 O6 C11 C12 -176.26(19) 2_656 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7O O3 0.84 1.94 2.774(3) 171.2 2_556 _diffrn_measured_fraction_theta_max 0.784 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.233 _refine_diff_density_min -1.108 _refine_diff_density_rms 0.139 # Attachment '- sm4.cif' data_sm4 _database_code_depnum_ccdc_archive 'CCDC 778770' #TrackingRef '- sm4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H78 O24 Sm4' _chemical_formula_weight 1616.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 14.517(2) _cell_length_b 19.882(3) _cell_length_c 21.190(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6115.9(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3176 _exptl_absorpt_coefficient_mu 3.856 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2487 _exptl_absorpt_correction_T_max 0.5127 _exptl_absorpt_process_details sadabs _exptl_special_details ; Due to the inability to locate H atoms on O2 and O3 from a difference map, and the H atoms of the two disordered methanol molecules, there is 10 H atoms missing in the calculated molecular formula. Shelx commands, SADI, SAME, PART, SIMU, DELU and ISOR were applied to refine the disorder. Some of the terminal carbon atoms were refined using approximate isotropic restraints. one of the methanol molecules has been refined using a two-part disorder model, since this was strongly indicated by oblate ellipsoids. However, when refined anisotropically, the minor disorder component (60/40) became unstable, so the disordered methanol has been refined using an isotropic model. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7676 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.34 _reflns_number_total 7676 _reflns_number_gt 6533 _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. ; _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^)+(0.0719P)^2^+54.5423P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.42(7) _refine_ls_number_reflns 7676 _refine_ls_number_parameters 667 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1507 _refine_ls_wR_factor_gt 0.1451 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.081 _refine_ls_shift/su_mean 0.002 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 0.71505(5) 0.51187(4) 0.27172(3) 0.03122(17) Uani 1 1 d . . . Sm2 Sm 0.93708(5) 0.57702(4) 0.35017(4) 0.03870(19) Uani 1 1 d . . . Sm3 Sm 0.90375(5) 0.39049(4) 0.35257(6) 0.0429(2) Uani 1 1 d . . . Sm4 Sm 0.73150(5) 0.49382(4) 0.44449(3) 0.03203(17) Uani 1 1 d . . . O1 O 0.7442(6) 0.4248(5) 0.3484(6) 0.0301(19) Uani 1 1 d . . . C1M C 0.656(3) 0.759(2) 0.370(2) 0.091(14) Uiso 0.62(3) 1 d PD A 1 O1M O 0.7297(19) 0.7279(15) 0.3328(14) 0.082(9) Uiso 0.62(3) 1 d PD A 1 C1M' C 0.568(4) 0.737(3) 0.374(3) 0.076(19) Uiso 0.38(3) 1 d PD A 2 O1M' O 0.625(3) 0.6789(19) 0.3809(19) 0.067(12) Uiso 0.38(3) 1 d PD A 2 C1 C 0.5904(17) 0.6527(14) 0.2207(13) 0.076(6) Uani 1 1 d U . . H1A H 0.5757 0.6992 0.2323 0.114 Uiso 1 1 calc R . . H1B H 0.5334 0.6265 0.2179 0.114 Uiso 1 1 calc R . . H1C H 0.6218 0.6522 0.1798 0.114 Uiso 1 1 calc R . . O2 O 0.8905(7) 0.4893(6) 0.4193(5) 0.032(2) Uani 1 1 d . . . C2 C 0.6786(10) 0.3736(7) 0.3475(8) 0.033(3) Uani 1 1 d . . . H2A H 0.6856 0.3471 0.3088 0.050 Uiso 1 1 calc R . . H2B H 0.6168 0.3933 0.3487 0.050 Uiso 1 1 calc R . . H2C H 0.6873 0.3444 0.3843 0.050 Uiso 1 1 calc R . . O3 O 0.7732(6) 0.5709(5) 0.3623(5) 0.030(2) Uani 1 1 d . . . C3 C 0.9281(13) 0.4836(10) 0.2239(10) 0.054(5) Uani 1 1 d . . . H3A H 0.9043 0.4471 0.1974 0.082 Uiso 1 1 calc R . . H3B H 0.9936 0.4761 0.2324 0.082 Uiso 1 1 calc R . . H3C H 0.9202 0.5266 0.2020 0.082 Uiso 1 1 calc R . . O4 O 0.8798(8) 0.4850(6) 0.2809(6) 0.039(3) Uani 1 1 d . . . C4 C 0.876(2) 0.2802(16) 0.2138(18) 0.119(14) Uani 1 1 d . . . H4A H 0.8288 0.2697 0.1823 0.179 Uiso 1 1 calc R . . H4B H 0.8915 0.2395 0.2376 0.179 Uiso 1 1 calc R . . H4C H 0.9315 0.2970 0.1924 0.179 Uiso 1 1 calc R . . O5 O 0.6493(10) 0.6239(6) 0.2677(7) 0.055(3) Uani 1 1 d . . . O7 O 0.8400(10) 0.3339(7) 0.2588(7) 0.063(4) Uani 1 1 d . . . C101 C 0.608(3) 0.6859(18) 0.5430(14) 0.116(12) Uani 1 1 d . . . H10A H 0.5764 0.6933 0.5028 0.174 Uiso 1 1 calc R . . H10B H 0.6423 0.7266 0.5547 0.174 Uiso 1 1 calc R . . H10C H 0.5630 0.6754 0.5759 0.174 Uiso 1 1 calc R . . C102 C 0.6749(12) 0.6276(12) 0.5361(9) 0.053(5) Uani 1 1 d . . . C103 C 0.7283(14) 0.6066(11) 0.5862(9) 0.055(5) Uani 1 1 d . . . H10D H 0.7216 0.6314 0.6243 0.066 Uiso 1 1 calc R . . C104 C 0.7925(12) 0.5520(9) 0.5879(7) 0.042(4) Uani 1 1 d . . . C105 C 0.8492(17) 0.5413(14) 0.6460(11) 0.077(7) Uani 1 1 d . . . H10E H 0.8891 0.5021 0.6401 0.115 Uiso 1 1 calc R . . H10F H 0.8084 0.5336 0.6822 0.115 Uiso 1 1 calc R . . H10G H 0.8872 0.5812 0.6538 0.115 Uiso 1 1 calc R . . O101 O 0.6762(9) 0.5965(6) 0.4845(6) 0.047(3) Uani 1 1 d . . . O102 O 0.8026(9) 0.5120(6) 0.5426(6) 0.043(3) Uani 1 1 d . . . C111 C 0.834(3) 0.751(2) 0.478(3) 0.20(2) Uani 1 1 d DU . . H11A H 0.8478 0.7665 0.5207 0.301 Uiso 1 1 calc R . . H11B H 0.7742 0.7273 0.4782 0.301 Uiso 1 1 calc R . . H11C H 0.8303 0.7894 0.4492 0.301 Uiso 1 1 calc R . . C112 C 0.904(3) 0.7058(19) 0.4572(19) 0.112(8) Uani 1 1 d U . . C113 C 0.956(2) 0.6722(18) 0.4969(18) 0.109(8) Uani 1 1 d DU . . H11D H 0.9476 0.6877 0.5389 0.130 Uiso 1 1 calc R . . C114 C 1.016(2) 0.6245(16) 0.4950(13) 0.138(13) Uani 1 1 d DU . . C115 C 1.089(3) 0.6129(17) 0.5377(19) 0.146(13) Uani 1 1 d DU . . H11E H 1.1252 0.5741 0.5235 0.219 Uiso 1 1 calc R . . H11F H 1.0640 0.6038 0.5798 0.219 Uiso 1 1 calc R . . H11G H 1.1288 0.6527 0.5395 0.219 Uiso 1 1 calc R . . O111 O 0.8893(15) 0.6833(12) 0.3975(11) 0.104(6) Uani 1 1 d U . . O112 O 1.0241(13) 0.5939(10) 0.4402(10) 0.092(5) Uani 1 1 d DU . . C131 C 0.846(2) 0.6961(17) 0.1737(13) 0.105(8) Uani 1 1 d U . . H13A H 0.7834 0.6909 0.1903 0.158 Uiso 1 1 calc R . . H13B H 0.8507 0.6730 0.1329 0.158 Uiso 1 1 calc R . . H13C H 0.8596 0.7440 0.1680 0.158 Uiso 1 1 calc R . . C132 C 0.911(2) 0.6671(18) 0.2175(13) 0.097(6) Uani 1 1 d U . . C133 C 1.0109(18) 0.6694(13) 0.2050(11) 0.075(7) Uani 1 1 d . . . H13D H 1.0301 0.6909 0.1672 0.090 Uiso 1 1 calc R . . C134 C 1.0802(18) 0.6427(13) 0.2439(13) 0.076(7) Uani 1 1 d . . . C135 C 1.1798(16) 0.6497(16) 0.2198(14) 0.096(10) Uani 1 1 d . . . H13E H 1.2221 0.6293 0.2504 0.145 Uiso 1 1 calc R . . H13F H 1.1949 0.6974 0.2147 0.145 Uiso 1 1 calc R . . H13G H 1.1858 0.6268 0.1791 0.145 Uiso 1 1 calc R . . O131 O 0.8750(14) 0.6349(11) 0.2635(8) 0.099(5) Uani 1 1 d U . . O132 O 1.0627(10) 0.6135(8) 0.2896(7) 0.066(4) Uani 1 1 d . . . C141 C 0.5304(15) 0.3818(13) 0.5811(10) 0.074(7) Uani 1 1 d . . . H14A H 0.4842 0.4146 0.5674 0.111 Uiso 1 1 calc R . . H14B H 0.5436 0.3883 0.6260 0.111 Uiso 1 1 calc R . . H14C H 0.5068 0.3361 0.5743 0.111 Uiso 1 1 calc R . . C142 C 0.6184(13) 0.3915(11) 0.5431(8) 0.052(5) Uani 1 1 d . . . C143 C 0.6966(12) 0.3518(9) 0.5548(8) 0.040(4) Uani 1 1 d . . . H14D H 0.6952 0.3250 0.5920 0.048 Uiso 1 1 calc R . . C144 C 0.7752(11) 0.3472(9) 0.5185(8) 0.039(3) Uani 1 1 d . . . C145 C 0.8419(13) 0.2943(10) 0.5350(9) 0.047(4) Uani 1 1 d . . . H14E H 0.8943 0.2962 0.5059 0.071 Uiso 1 1 calc R . . H14F H 0.8122 0.2502 0.5318 0.071 Uiso 1 1 calc R . . H14G H 0.8637 0.3012 0.5783 0.071 Uiso 1 1 calc R . . O141 O 0.6158(9) 0.4372(7) 0.5012(6) 0.048(3) Uani 1 1 d . . . O142 O 0.7900(7) 0.3834(5) 0.4709(5) 0.034(2) Uani 1 1 d . . . C151 C 0.7154(15) 0.5674(14) 0.0566(10) 0.070(7) Uani 1 1 d . . . H15A H 0.7393 0.6115 0.0692 0.104 Uiso 1 1 calc R . . H15B H 0.6543 0.5729 0.0376 0.104 Uiso 1 1 calc R . . H15C H 0.7573 0.5470 0.0258 0.104 Uiso 1 1 calc R . . C152 C 0.7085(15) 0.5250(11) 0.1107(11) 0.059(5) Uani 1 1 d U . . C153 C 0.6731(17) 0.4536(12) 0.1045(13) 0.073(6) Uani 1 1 d U . . H15D H 0.6417 0.4418 0.0667 0.087 Uiso 1 1 calc R . . C154 C 0.6832(15) 0.4053(11) 0.1491(11) 0.058(5) Uani 1 1 d U . . C155 C 0.650(3) 0.343(2) 0.130(2) 0.157(15) Uani 1 1 d U . . H15E H 0.6588 0.3099 0.1641 0.236 Uiso 1 1 calc R . . H15F H 0.6832 0.3277 0.0924 0.236 Uiso 1 1 calc R . . H15G H 0.5840 0.3463 0.1204 0.236 Uiso 1 1 calc R . . O151 O 0.7284(8) 0.5451(7) 0.1645(5) 0.049(3) Uani 1 1 d . . . O152 O 0.7186(12) 0.4129(8) 0.2047(7) 0.068(4) Uani 1 1 d . . . C161 C 0.9115(17) 0.1581(9) 0.3887(14) 0.077(8) Uani 1 1 d . . . H16A H 0.8533 0.1494 0.3668 0.115 Uiso 1 1 calc R . . H16B H 0.9063 0.1435 0.4327 0.115 Uiso 1 1 calc R . . H16C H 0.9613 0.1331 0.3680 0.115 Uiso 1 1 calc R . . C162 C 0.9318(13) 0.2292(9) 0.3867(11) 0.060(6) Uani 1 1 d . . . C163 C 1.0190(13) 0.2407(12) 0.4218(11) 0.064(6) Uani 1 1 d . . . H16D H 1.0549 0.2025 0.4327 0.077 Uiso 1 1 calc R . . C164 C 1.0544(13) 0.3087(13) 0.4414(12) 0.072(7) Uani 1 1 d . . . C165 C 1.132(2) 0.3116(17) 0.484(3) 0.18(3) Uani 1 1 d . . . H16E H 1.1457 0.3586 0.4945 0.274 Uiso 1 1 calc R . . H16F H 1.1858 0.2908 0.4644 0.274 Uiso 1 1 calc R . . H16G H 1.1168 0.2872 0.5232 0.274 Uiso 1 1 calc R . . O161 O 0.8832(7) 0.2748(5) 0.3733(6) 0.045(3) Uani 1 1 d . . . O162 O 1.0119(9) 0.3624(7) 0.4308(8) 0.057(4) Uani 1 1 d . . . C171 C 1.1651(19) 0.2950(14) 0.2546(17) 0.102(11) Uani 1 1 d . . . H17A H 1.1282 0.2581 0.2373 0.152 Uiso 1 1 calc R . . H17B H 1.2112 0.2768 0.2838 0.152 Uiso 1 1 calc R . . H17C H 1.1963 0.3188 0.2202 0.152 Uiso 1 1 calc R . . C172 C 1.1067(16) 0.3405(17) 0.2875(10) 0.080(8) Uani 1 1 d . . . C173 C 1.1630(19) 0.3978(19) 0.3153(10) 0.102(12) Uani 1 1 d . . . H17D H 1.2280 0.3925 0.3150 0.122 Uiso 1 1 calc R . . C174 C 1.1256(15) 0.4633(16) 0.3439(11) 0.080(7) Uani 1 1 d . . . C175 C 1.185(2) 0.5125(15) 0.3715(18) 0.119(14) Uani 1 1 d . . . H17E H 1.1483 0.5502 0.3873 0.178 Uiso 1 1 calc R . . H17F H 1.2286 0.5289 0.3396 0.178 Uiso 1 1 calc R . . H17G H 1.2193 0.4922 0.4066 0.178 Uiso 1 1 calc R . . O171 O 1.0252(11) 0.3468(9) 0.2886(10) 0.079(5) Uani 1 1 d . . . O172 O 1.0394(9) 0.4729(8) 0.3421(8) 0.067(4) Uani 1 1 d . . . C181 C 0.409(2) 0.4835(16) 0.2082(17) 0.102(9) Uani 1 1 d U . . H18A H 0.4368 0.4745 0.1667 0.152 Uiso 1 1 calc R . . H18B H 0.3673 0.5219 0.2050 0.152 Uiso 1 1 calc R . . H18C H 0.3753 0.4438 0.2224 0.152 Uiso 1 1 calc R . . C182 C 0.4827(14) 0.4990(13) 0.2537(10) 0.066(6) Uani 1 1 d . . . C183 C 0.4578(13) 0.5178(12) 0.3191(9) 0.057(5) Uani 1 1 d . . . H18D H 0.3945 0.5264 0.3268 0.068 Uiso 1 1 calc R . . C184 C 0.5138(10) 0.5240(8) 0.3681(8) 0.038(4) Uani 1 1 d . . . C185 C 0.4729(12) 0.5387(11) 0.4314(9) 0.050(4) Uani 1 1 d . . . H18E H 0.5222 0.5427 0.4628 0.074 Uiso 1 1 calc R . . H18F H 0.4313 0.5021 0.4435 0.074 Uiso 1 1 calc R . . H18G H 0.4383 0.5810 0.4295 0.074 Uiso 1 1 calc R . . O181 O 0.5634(9) 0.4878(9) 0.2378(6) 0.069(5) Uani 1 1 d . . . O182 O 0.6019(7) 0.5141(6) 0.3657(5) 0.039(3) Uani 1 1 d . . . O2M O 1.037(3) 0.466(2) 0.510(2) 0.197(14) Uani 1 1 d DU . . C2M C 1.011(4) 0.419(3) 0.560(3) 0.193(19) Uani 1 1 d DU . . 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 0.0397(3) 0.0321(4) 0.0219(3) -0.0005(3) -0.0057(3) -0.0001(3) Sm2 0.0396(4) 0.0458(4) 0.0307(3) 0.0062(4) -0.0080(4) -0.0159(3) Sm3 0.0329(3) 0.0290(4) 0.0666(5) 0.0015(5) -0.0096(5) 0.0019(3) Sm4 0.0351(3) 0.0380(4) 0.0230(3) 0.0021(4) 0.0013(3) 0.0024(3) O1 0.031(4) 0.026(5) 0.033(5) 0.004(5) 0.000(5) -0.003(4) C1 0.076(7) 0.076(7) 0.076(7) 0.0001(10) -0.0003(10) 0.0001(10) O2 0.041(5) 0.027(5) 0.027(5) 0.010(4) -0.008(4) -0.003(5) C2 0.044(7) 0.023(7) 0.033(7) -0.009(7) 0.017(7) -0.001(6) O3 0.034(4) 0.031(5) 0.026(5) 0.006(4) -0.012(4) -0.005(4) C3 0.052(10) 0.058(12) 0.054(11) 0.003(9) 0.024(9) -0.006(9) O4 0.040(5) 0.038(6) 0.039(6) -0.001(5) 0.018(5) -0.015(5) C4 0.12(3) 0.09(2) 0.14(3) 0.04(2) -0.06(2) -0.06(2) O5 0.074(8) 0.044(7) 0.047(7) 0.011(6) -0.022(7) 0.025(6) O7 0.080(9) 0.044(7) 0.064(9) -0.028(7) 0.030(7) -0.007(7) C101 0.15(3) 0.13(3) 0.064(17) -0.046(19) 0.003(19) 0.01(2) C102 0.041(9) 0.080(15) 0.038(9) -0.013(9) -0.006(7) 0.001(9) C103 0.064(12) 0.061(12) 0.042(10) -0.010(9) -0.019(9) 0.008(10) C104 0.051(9) 0.054(10) 0.022(7) 0.002(7) -0.006(6) -0.027(8) C105 0.076(15) 0.098(18) 0.055(12) -0.016(13) -0.042(11) 0.007(13) O101 0.059(7) 0.050(7) 0.033(6) -0.008(5) -0.002(5) 0.006(6) O102 0.057(7) 0.040(6) 0.032(6) -0.001(5) -0.004(5) -0.001(5) C111 0.20(2) 0.20(2) 0.20(2) 0.0000(10) 0.0000(10) 0.0000(10) C112 0.112(8) 0.112(8) 0.112(8) -0.0001(10) -0.0002(10) 0.0000(10) C113 0.104(11) 0.108(11) 0.114(11) -0.006(9) -0.001(8) 0.001(9) C114 0.21(4) 0.075(17) 0.13(2) -0.027(17) -0.09(2) -0.02(2) C115 0.22(4) 0.090(19) 0.13(2) -0.010(18) -0.09(2) -0.02(2) O111 0.104(6) 0.104(6) 0.104(6) -0.0002(10) -0.0001(10) -0.0002(10) O112 0.092(5) 0.092(5) 0.092(5) 0.0000(10) -0.0002(10) -0.0003(10) C131 0.120(17) 0.127(18) 0.069(13) 0.043(14) 0.004(12) 0.051(15) C132 0.111(13) 0.125(14) 0.054(9) 0.047(10) 0.006(9) 0.024(11) C133 0.091(17) 0.088(17) 0.045(12) 0.007(12) 0.008(11) -0.043(14) C134 0.081(16) 0.073(16) 0.074(16) 0.005(13) 0.003(13) -0.044(14) C135 0.055(13) 0.15(3) 0.087(18) 0.061(19) 0.024(13) -0.003(15) O131 0.111(12) 0.128(13) 0.060(9) 0.053(9) 0.011(8) 0.030(10) O132 0.069(9) 0.065(10) 0.063(9) 0.011(8) 0.020(7) -0.032(8) C141 0.069(13) 0.104(19) 0.050(12) 0.016(12) 0.047(10) 0.005(12) C142 0.053(10) 0.073(14) 0.030(8) 0.018(8) 0.025(7) -0.006(9) C143 0.048(9) 0.042(10) 0.030(8) 0.013(7) -0.001(6) 0.006(7) C144 0.046(8) 0.042(9) 0.029(7) 0.008(7) 0.009(6) 0.001(7) C145 0.057(10) 0.042(10) 0.042(10) 0.017(8) 0.000(8) 0.000(8) O141 0.052(7) 0.055(8) 0.037(6) 0.006(6) 0.013(5) -0.001(6) O142 0.044(6) 0.033(6) 0.024(5) 0.004(4) 0.006(4) 0.006(5) C151 0.059(12) 0.11(2) 0.040(10) 0.023(11) -0.018(9) -0.020(12) C152 0.059(5) 0.059(5) 0.059(5) 0.0002(10) 0.0000(10) 0.0001(10) C153 0.073(6) 0.073(6) 0.073(6) 0.0000(10) -0.0001(10) 0.0000(10) C154 0.058(5) 0.058(5) 0.058(5) -0.0001(10) 0.0000(10) -0.0002(10) C155 0.157(15) 0.157(15) 0.157(15) 0.0000(10) 0.0000(10) 0.0000(10) O151 0.044(6) 0.075(9) 0.028(6) 0.010(6) 0.004(5) 0.006(6) O152 0.109(13) 0.064(9) 0.032(7) -0.012(7) -0.006(7) -0.018(9) C161 0.079(15) 0.025(9) 0.13(2) 0.000(11) 0.009(15) 0.007(10) C162 0.053(10) 0.038(10) 0.088(15) -0.007(10) 0.041(11) 0.007(9) C163 0.042(10) 0.070(15) 0.080(15) 0.019(12) -0.004(10) 0.018(10) C164 0.045(10) 0.098(18) 0.072(14) 0.031(14) 0.020(11) 0.024(11) C165 0.10(2) 0.08(2) 0.37(8) 0.08(3) -0.13(4) -0.038(18) O161 0.036(5) 0.030(6) 0.069(9) 0.000(5) -0.003(5) 0.002(5) O162 0.053(7) 0.039(7) 0.079(10) 0.020(7) -0.013(7) -0.010(6) C171 0.072(16) 0.076(18) 0.16(3) 0.025(19) 0.031(18) 0.036(14) C172 0.062(13) 0.15(3) 0.031(10) 0.009(12) 0.013(9) -0.003(15) C173 0.087(17) 0.19(3) 0.031(10) 0.001(15) -0.010(11) 0.07(2) C174 0.060(12) 0.14(2) 0.044(12) 0.012(14) 0.001(10) -0.001(14) C175 0.097(19) 0.12(2) 0.14(3) -0.06(2) 0.06(2) -0.083(18) O171 0.051(8) 0.079(12) 0.107(15) 0.028(10) 0.017(9) 0.020(8) O172 0.044(7) 0.093(11) 0.065(10) 0.016(8) 0.003(7) -0.002(7) C181 0.102(9) 0.102(9) 0.102(9) -0.0001(10) -0.0001(10) -0.0002(10) C182 0.053(11) 0.094(17) 0.050(11) -0.013(11) -0.002(9) -0.045(12) C183 0.040(9) 0.093(17) 0.038(9) -0.004(10) 0.015(7) -0.011(10) C184 0.033(7) 0.038(9) 0.044(9) 0.008(7) 0.001(6) 0.003(6) C185 0.037(8) 0.061(12) 0.050(11) -0.007(9) 0.005(7) -0.005(8) O181 0.043(7) 0.124(14) 0.040(7) -0.026(8) 0.004(5) -0.046(8) O182 0.034(5) 0.054(7) 0.029(6) 0.000(5) -0.002(4) 0.012(5) O2M 0.197(14) 0.197(14) 0.197(14) 0.0000(10) -0.0001(10) 0.0000(10) C2M 0.192(19) 0.193(19) 0.193(19) 0.0000(10) 0.0000(10) -0.0001(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 Sm1 O181 2.364(12) . ? Sm1 O151 2.373(12) . ? Sm1 O3 2.403(10) . ? Sm1 O1 2.412(11) . ? Sm1 O5 2.424(11) . ? Sm1 O152 2.428(15) . ? Sm1 O4 2.458(12) . ? Sm1 O182 2.582(11) . ? Sm1 Sm4 3.6863(11) . ? Sm1 Sm2 3.8510(11) . ? Sm1 Sm3 4.0327(12) . ? Sm2 O112 2.31(2) . ? Sm2 O132 2.344(13) . ? Sm2 O131 2.347(16) . ? Sm2 O2 2.375(11) . ? Sm2 O3 2.396(9) . ? Sm2 O111 2.44(2) . ? Sm2 O4 2.488(12) . ? Sm2 O172 2.554(15) . ? Sm2 Sm3 3.7405(13) . ? Sm2 Sm4 3.9545(11) . ? Sm3 O162 2.350(14) . ? Sm3 O161 2.361(11) . ? Sm3 O171 2.388(16) . ? Sm3 O1 2.416(9) . ? Sm3 O2 2.428(12) . ? Sm3 O4 2.442(13) . ? Sm3 O7 2.464(15) . ? Sm3 O172 2.572(14) . ? Sm3 Sm4 3.7771(13) . ? Sm4 O102 2.350(12) . ? Sm4 O101 2.352(12) . ? Sm4 O141 2.353(12) . ? Sm4 O2 2.371(11) . ? Sm4 O3 2.397(10) . ? Sm4 O142 2.419(10) . ? Sm4 O1 2.463(12) . ? Sm4 O182 2.548(10) . ? O1 C2 1.393(16) . ? C1M O1M 1.473(19) . ? C1M' O1M' 1.43(2) . ? C1 O5 1.43(3) . ? C3 O4 1.40(2) . ? C4 O7 1.52(4) . ? C101 C102 1.52(4) . ? C102 O101 1.26(2) . ? C102 C103 1.38(3) . ? C103 C104 1.43(3) . ? C104 O102 1.25(2) . ? C104 C105 1.50(2) . ? C111 C112 1.43(5) . ? C112 C113 1.32(4) . ? C112 O111 1.36(4) . ? C113 C114 1.29(3) . ? C114 O112 1.317(19) . ? C114 C115 1.412(19) . ? C131 C132 1.45(4) . ? C132 O131 1.28(3) . ? C132 C133 1.47(4) . ? C133 C134 1.40(4) . ? C134 O132 1.16(3) . ? C134 C135 1.54(3) . ? C141 C142 1.52(2) . ? C142 O141 1.27(2) . ? C142 C143 1.41(3) . ? C143 C144 1.38(2) . ? C144 O142 1.257(18) . ? C144 C145 1.47(2) . ? C151 C152 1.43(3) . ? C152 O151 1.24(3) . ? C152 C153 1.52(3) . ? C153 C154 1.36(3) . ? C154 O152 1.29(2) . ? C154 C155 1.40(5) . ? C161 C162 1.45(3) . ? C162 O161 1.18(2) . ? C162 C163 1.49(3) . ? C163 C164 1.51(4) . ? C164 O162 1.25(3) . ? C164 C165 1.45(4) . ? C171 C172 1.42(4) . ? C172 O171 1.19(3) . ? C172 C173 1.52(4) . ? C173 C174 1.53(4) . ? C174 O172 1.27(3) . ? C174 C175 1.43(4) . ? C181 C182 1.47(4) . ? C182 O181 1.24(3) . ? C182 C183 1.48(3) . ? C183 C184 1.32(3) . ? C184 O182 1.295(18) . ? C184 C185 1.50(2) . ? O2M C2M 1.46(2) . ? 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 O181 Sm1 O151 80.9(5) . . ? O181 Sm1 O3 131.9(4) . . ? O151 Sm1 O3 126.9(4) . . ? O181 Sm1 O1 102.9(5) . . ? O151 Sm1 O1 146.1(4) . . ? O3 Sm1 O1 75.6(4) . . ? O181 Sm1 O5 79.0(6) . . ? O151 Sm1 O5 75.1(5) . . ? O3 Sm1 O5 73.6(4) . . ? O1 Sm1 O5 138.8(5) . . ? O181 Sm1 O152 71.2(6) . . ? O151 Sm1 O152 70.3(5) . . ? O3 Sm1 O152 148.9(5) . . ? O1 Sm1 O152 78.9(4) . . ? O5 Sm1 O152 137.1(5) . . ? O181 Sm1 O4 152.4(5) . . ? O151 Sm1 O4 93.2(4) . . ? O3 Sm1 O4 72.6(4) . . ? O1 Sm1 O4 67.7(3) . . ? O5 Sm1 O4 125.8(4) . . ? O152 Sm1 O4 81.3(5) . . ? O181 Sm1 O182 69.2(4) . . ? O151 Sm1 O182 141.8(4) . . ? O3 Sm1 O182 66.3(3) . . ? O1 Sm1 O182 66.7(3) . . ? O5 Sm1 O182 76.1(4) . . ? O152 Sm1 O182 118.6(5) . . ? O4 Sm1 O182 124.2(4) . . ? O181 Sm1 Sm4 110.0(3) . . ? O151 Sm1 Sm4 166.5(3) . . ? O3 Sm1 Sm4 39.8(2) . . ? O1 Sm1 Sm4 41.4(3) . . ? O5 Sm1 Sm4 98.6(3) . . ? O152 Sm1 Sm4 120.1(4) . . ? O4 Sm1 Sm4 80.7(3) . . ? O182 Sm1 Sm4 43.7(2) . . ? O181 Sm1 Sm2 168.1(4) . . ? O151 Sm1 Sm2 104.5(3) . . ? O3 Sm1 Sm2 36.6(2) . . ? O1 Sm1 Sm2 78.7(2) . . ? O5 Sm1 Sm2 92.0(3) . . ? O152 Sm1 Sm2 120.5(4) . . ? O4 Sm1 Sm2 39.2(3) . . ? O182 Sm1 Sm2 101.2(2) . . ? Sm4 Sm1 Sm2 63.24(2) . . ? O181 Sm1 Sm3 129.8(5) . . ? O151 Sm1 Sm3 121.2(3) . . ? O3 Sm1 Sm3 73.4(2) . . ? O1 Sm1 Sm3 33.4(2) . . ? O5 Sm1 Sm3 146.3(3) . . ? O152 Sm1 Sm3 75.5(4) . . ? O4 Sm1 Sm3 34.5(3) . . ? O182 Sm1 Sm3 96.6(2) . . ? Sm4 Sm1 Sm3 58.39(2) . . ? Sm2 Sm1 Sm3 56.59(2) . . ? O112 Sm2 O132 89.0(7) . . ? O112 Sm2 O131 141.7(8) . . ? O132 Sm2 O131 73.7(7) . . ? O112 Sm2 O2 75.7(6) . . ? O132 Sm2 O2 141.8(5) . . ? O131 Sm2 O2 137.1(6) . . ? O112 Sm2 O3 117.5(6) . . ? O132 Sm2 O3 147.8(5) . . ? O131 Sm2 O3 74.2(5) . . ? O2 Sm2 O3 67.3(4) . . ? O112 Sm2 O111 72.0(7) . . ? O132 Sm2 O111 100.3(7) . . ? O131 Sm2 O111 77.8(8) . . ? O2 Sm2 O111 107.5(6) . . ? O3 Sm2 O111 73.6(6) . . ? O112 Sm2 O4 140.9(6) . . ? O132 Sm2 O4 99.4(5) . . ? O131 Sm2 O4 76.7(7) . . ? O2 Sm2 O4 74.3(3) . . ? O3 Sm2 O4 72.2(3) . . ? O111 Sm2 O4 141.7(6) . . ? O112 Sm2 O172 81.6(6) . . ? O132 Sm2 O172 76.2(5) . . ? O131 Sm2 O172 124.6(6) . . ? O2 Sm2 O172 67.2(4) . . ? O3 Sm2 O172 122.9(4) . . ? O111 Sm2 O172 153.5(7) . . ? O4 Sm2 O172 63.9(5) . . ? O112 Sm2 Sm3 101.7(5) . . ? O132 Sm2 Sm3 114.5(4) . . ? O131 Sm2 Sm3 116.5(6) . . ? O2 Sm2 Sm3 39.4(3) . . ? O3 Sm2 Sm3 79.6(2) . . ? O111 Sm2 Sm3 144.7(5) . . ? O4 Sm2 Sm3 40.2(3) . . ? O172 Sm2 Sm3 43.3(3) . . ? O112 Sm2 Sm1 149.5(5) . . ? O132 Sm2 Sm1 121.2(4) . . ? O131 Sm2 Sm1 60.4(6) . . ? O2 Sm2 Sm1 77.4(3) . . ? O3 Sm2 Sm1 36.7(3) . . ? O111 Sm2 Sm1 103.4(5) . . ? O4 Sm2 Sm1 38.6(3) . . ? O172 Sm2 Sm1 100.7(3) . . ? Sm3 Sm2 Sm1 64.16(2) . . ? O112 Sm2 Sm4 93.2(5) . . ? O132 Sm2 Sm4 173.2(4) . . ? O131 Sm2 Sm4 108.1(5) . . ? O2 Sm2 Sm4 33.5(3) . . ? O3 Sm2 Sm4 34.4(2) . . ? O111 Sm2 Sm4 86.6(5) . . ? O4 Sm2 Sm4 74.9(2) . . ? O172 Sm2 Sm4 97.7(3) . . ? Sm3 Sm2 Sm4 58.72(2) . . ? Sm1 Sm2 Sm4 56.34(2) . . ? O162 Sm3 O161 73.8(4) . . ? O162 Sm3 O171 79.7(6) . . ? O161 Sm3 O171 81.1(5) . . ? O162 Sm3 O1 137.2(5) . . ? O161 Sm3 O1 99.2(3) . . ? O171 Sm3 O1 142.1(6) . . ? O162 Sm3 O2 80.5(5) . . ? O161 Sm3 O2 132.1(4) . . ? O171 Sm3 O2 133.1(5) . . ? O1 Sm3 O2 73.6(4) . . ? O162 Sm3 O4 135.8(4) . . ? O161 Sm3 O4 148.0(4) . . ? O171 Sm3 O4 91.8(5) . . ? O1 Sm3 O4 67.9(4) . . ? O2 Sm3 O4 74.2(3) . . ? O162 Sm3 O7 135.3(5) . . ? O161 Sm3 O7 70.0(5) . . ? O171 Sm3 O7 69.7(6) . . ? O1 Sm3 O7 74.9(4) . . ? O2 Sm3 O7 144.0(4) . . ? O4 Sm3 O7 78.3(5) . . ? O162 Sm3 O172 72.6(5) . . ? O161 Sm3 O172 137.2(4) . . ? O171 Sm3 O172 67.5(6) . . ? O1 Sm3 O172 123.5(4) . . ? O2 Sm3 O172 66.1(5) . . ? O4 Sm3 O172 64.2(4) . . ? O7 Sm3 O172 120.6(5) . . ? O162 Sm3 Sm2 99.1(3) . . ? O161 Sm3 Sm2 170.0(3) . . ? O171 Sm3 Sm2 104.9(4) . . ? O1 Sm3 Sm2 81.0(2) . . ? O2 Sm3 Sm2 38.4(3) . . ? O4 Sm3 Sm2 41.1(3) . . ? O7 Sm3 Sm2 119.4(3) . . ? O172 Sm3 Sm2 42.9(3) . . ? O162 Sm3 Sm4 102.0(4) . . ? O161 Sm3 Sm4 110.5(3) . . ? O171 Sm3 Sm4 168.4(4) . . ? O1 Sm3 Sm4 39.7(3) . . ? O2 Sm3 Sm4 37.6(3) . . ? O4 Sm3 Sm4 78.9(3) . . ? O7 Sm3 Sm4 114.6(3) . . ? O172 Sm3 Sm4 101.8(4) . . ? Sm2 Sm3 Sm4 63.47(2) . . ? O162 Sm3 Sm1 153.6(4) . . ? O161 Sm3 Sm1 125.2(3) . . ? O171 Sm3 Sm1 118.6(4) . . ? O1 Sm3 Sm1 33.3(3) . . ? O2 Sm3 Sm1 73.1(2) . . ? O4 Sm3 Sm1 34.7(2) . . ? O7 Sm3 Sm1 71.1(3) . . ? O172 Sm3 Sm1 95.9(3) . . ? Sm2 Sm3 Sm1 59.25(2) . . ? Sm4 Sm3 Sm1 56.21(2) . . ? O102 Sm4 O101 72.3(4) . . ? O102 Sm4 O141 86.3(5) . . ? O101 Sm4 O141 89.3(5) . . ? O102 Sm4 O2 77.2(4) . . ? O101 Sm4 O2 116.5(4) . . ? O141 Sm4 O2 142.4(4) . . ? O102 Sm4 O3 115.7(4) . . ? O101 Sm4 O3 78.1(4) . . ? O141 Sm4 O3 149.0(4) . . ? O2 Sm4 O3 67.3(3) . . ? O102 Sm4 O142 77.3(4) . . ? O101 Sm4 O142 145.5(4) . . ? O141 Sm4 O142 72.4(4) . . ? O2 Sm4 O142 71.1(4) . . ? O3 Sm4 O142 131.3(4) . . ? O102 Sm4 O1 141.7(4) . . ? O101 Sm4 O1 143.9(4) . . ? O141 Sm4 O1 102.1(4) . . ? O2 Sm4 O1 73.7(4) . . ? O3 Sm4 O1 74.7(4) . . ? O142 Sm4 O1 70.1(3) . . ? O102 Sm4 O182 151.6(4) . . ? O101 Sm4 O182 81.2(4) . . ? O141 Sm4 O182 83.3(4) . . ? O2 Sm4 O182 125.3(4) . . ? O3 Sm4 O182 67.0(3) . . ? O142 Sm4 O182 123.7(4) . . ? O1 Sm4 O182 66.5(3) . . ? O102 Sm4 Sm1 153.2(3) . . ? O101 Sm4 Sm1 104.6(3) . . ? O141 Sm4 Sm1 120.5(3) . . ? O2 Sm4 Sm1 81.0(3) . . ? O3 Sm4 Sm1 39.9(2) . . ? O142 Sm4 Sm1 109.9(2) . . ? O1 Sm4 Sm1 40.3(2) . . ? O182 Sm4 Sm1 44.4(2) . . ? O102 Sm4 Sm3 104.5(3) . . ? O101 Sm4 Sm3 152.1(3) . . ? O141 Sm4 Sm3 118.4(3) . . ? O2 Sm4 Sm3 38.6(3) . . ? O3 Sm4 Sm3 78.8(2) . . ? O142 Sm4 Sm3 52.7(2) . . ? O1 Sm4 Sm3 38.8(2) . . ? O182 Sm4 Sm3 103.7(2) . . ? Sm1 Sm4 Sm3 65.40(2) . . ? O102 Sm4 Sm2 93.0(3) . . ? O101 Sm4 Sm2 94.4(3) . . ? O141 Sm4 Sm2 175.8(3) . . ? O2 Sm4 Sm2 33.6(3) . . ? O3 Sm4 Sm2 34.4(2) . . ? O142 Sm4 Sm2 103.4(2) . . ? O1 Sm4 Sm2 76.0(2) . . ? O182 Sm4 Sm2 99.2(3) . . ? Sm1 Sm4 Sm2 60.41(2) . . ? Sm3 Sm4 Sm2 57.81(2) . . ? C2 O1 Sm1 113.3(9) . . ? C2 O1 Sm3 116.7(8) . . ? Sm1 O1 Sm3 113.3(4) . . ? C2 O1 Sm4 111.5(9) . . ? Sm1 O1 Sm4 98.3(3) . . ? Sm3 O1 Sm4 101.4(4) . . ? Sm4 O2 Sm2 112.8(4) . . ? Sm4 O2 Sm3 103.8(4) . . ? Sm2 O2 Sm3 102.3(4) . . ? Sm4 O3 Sm2 111.2(4) . . ? Sm4 O3 Sm1 100.3(3) . . ? Sm2 O3 Sm1 106.7(4) . . ? C3 O4 Sm3 116.8(11) . . ? C3 O4 Sm1 115.1(12) . . ? Sm3 O4 Sm1 110.8(4) . . ? C3 O4 Sm2 110.9(10) . . ? Sm3 O4 Sm2 98.7(5) . . ? Sm1 O4 Sm2 102.2(4) . . ? C1 O5 Sm1 128.8(14) . . ? C4 O7 Sm3 134.0(15) . . ? O101 C102 C103 120.9(19) . . ? O101 C102 C101 118.0(19) . . ? C103 C102 C101 121.1(19) . . ? C102 C103 C104 128.0(18) . . ? O102 C104 C103 122.4(15) . . ? O102 C104 C105 118.4(19) . . ? C103 C104 C105 119.2(17) . . ? C102 O101 Sm4 138.3(13) . . ? C104 O102 Sm4 136.4(12) . . ? C113 C112 O111 121(4) . . ? C113 C112 C111 122(4) . . ? O111 C112 C111 112(4) . . ? C114 C113 C112 138(4) . . ? C113 C114 O112 115(3) . . ? C113 C114 C115 127(3) . . ? O112 C114 C115 115(3) . . ? C112 O111 Sm2 129(2) . . ? C114 O112 Sm2 138.3(19) . . ? O131 C132 C131 115(3) . . ? O131 C132 C133 124(2) . . ? C131 C132 C133 121(2) . . ? C134 C133 C132 126(2) . . ? O132 C134 C133 122(2) . . ? O132 C134 C135 122(3) . . ? C133 C134 C135 116(2) . . ? C132 O131 Sm2 133.2(19) . . ? C134 O132 Sm2 141.6(19) . . ? O141 C142 C143 123.4(15) . . ? O141 C142 C141 115.8(18) . . ? C143 C142 C141 120.8(17) . . ? C144 C143 C142 127.3(15) . . ? O142 C144 C143 123.5(15) . . ? O142 C144 C145 119.1(14) . . ? C143 C144 C145 117.3(14) . . ? C142 O141 Sm4 132.7(12) . . ? C144 O142 Sm4 130.1(10) . . ? O151 C152 C151 122(2) . . ? O151 C152 C153 117(2) . . ? C151 C152 C153 120(2) . . ? C154 C153 C152 125(2) . . ? O152 C154 C153 126(2) . . ? O152 C154 C155 120(3) . . ? C153 C154 C155 113(3) . . ? C152 O151 Sm1 140.4(14) . . ? C154 O152 Sm1 128.3(15) . . ? O161 C162 C161 129(2) . . ? O161 C162 C163 120.7(18) . . ? C161 C162 C163 108(2) . . ? C162 C163 C164 124.5(18) . . ? O162 C164 C165 118(3) . . ? O162 C164 C163 123(2) . . ? C165 C164 C163 118(2) . . ? C162 O161 Sm3 135.7(12) . . ? C164 O162 Sm3 131.2(17) . . ? O171 C172 C171 132(3) . . ? O171 C172 C173 117(3) . . ? C171 C172 C173 110(2) . . ? C172 C173 C174 127(2) . . ? O172 C174 C175 120(3) . . ? O172 C174 C173 118(2) . . ? C175 C174 C173 122(2) . . ? C172 O171 Sm3 141.6(19) . . ? C174 O172 Sm2 134.1(18) . . ? C174 O172 Sm3 131.1(17) . . ? Sm2 O172 Sm3 93.7(4) . . ? O181 C182 C181 118(2) . . ? O181 C182 C183 122.0(18) . . ? C181 C182 C183 119(2) . . ? C184 C183 C182 127.5(18) . . ? O182 C184 C183 124.1(16) . . ? O182 C184 C185 117.2(15) . . ? C183 C184 C185 118.6(15) . . ? C182 O181 Sm1 139.6(13) . . ? C184 O182 Sm4 136.7(10) . . ? C184 O182 Sm1 131.4(10) . . ? Sm4 O182 Sm1 91.9(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 3.057 _refine_diff_density_min -2.350 _refine_diff_density_rms 0.187 # Attachment '- Tb9.CIF' data_Tb9 _database_code_depnum_ccdc_archive 'CCDC 778771' #TrackingRef '- Tb9.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C80 H121 O42 Tb9, 4 H2 O' _chemical_formula_sum 'C80 H129 O46 Tb9' _chemical_formula_weight 3241.15 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/n' _symmetry_space_group_name_Hall '-P 4a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 18.8879(9) _cell_length_b 18.8879(9) _cell_length_c 15.3095(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5461.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4096 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 25.92 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.971 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3108 _exptl_absorpt_coefficient_mu 5.823 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6253 _exptl_absorpt_correction_T_max 0.7251 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1996' _exptl_special_details ; Four molecules of water per asymmetric unit removed with SQUEEZE ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube with Miracol optics' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEXII DUO CCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27009 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.04 _reflns_number_total 5403 _reflns_number_gt 3937 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement SHELXTL _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 1999)' _computing_publication_material 'SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5403 _refine_ls_number_parameters 314 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0619 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.613946(15) 0.755407(15) -0.033985(16) 0.01212(7) Uani 1 1 d . . . Tb2 Tb 0.661639(15) 0.852049(15) 0.319296(17) 0.01273(7) Uani 1 1 d . . . Tb3 Tb 0.7500 0.7500 0.14161(3) 0.01108(13) Uani 1 4 d S . . O1 O 0.6650(2) 0.8422(2) -0.1329(2) 0.0151(9) Uani 1 1 d . . . O2 O 0.5240(2) 0.8312(2) -0.0846(3) 0.0212(10) Uani 1 1 d . . . O3 O 0.5174(2) 0.6852(2) -0.0688(2) 0.0177(9) Uani 1 1 d . . . O4 O 0.5414(2) 0.7575(2) 0.0888(2) 0.0158(9) Uani 1 1 d . . . O5 O 0.6069(2) 0.9012(2) 0.1969(2) 0.0170(9) Uani 1 1 d . . . O6 O 0.5491(2) 0.8789(2) 0.3624(3) 0.0215(10) Uani 1 1 d . . . O7 O 0.5258(2) 0.6654(2) 0.3531(2) 0.0194(10) Uani 1 1 d . . . O8 O 0.6254(2) 0.7572(2) 0.4197(2) 0.0164(9) Uani 1 1 d . . . O9 O 0.7500 0.7500 -0.0483(5) 0.0156(18) Uani 1 4 d SD . . H9O H 0.7500 0.7500 -0.1032(8) 0.019 Uiso 1 4 d SD . . O10 O 0.6698(2) 0.6755(2) 0.0585(2) 0.0134(9) Uani 1 1 d D . . H10O H 0.641(2) 0.654(3) 0.090(3) 0.016 Uiso 1 1 d D . . O11 O 0.6405(2) 0.7563(2) 0.2251(2) 0.0127(9) Uani 1 1 d D . . H11O H 0.6047(18) 0.763(3) 0.194(3) 0.015 Uiso 1 1 d D . . O12 O 0.7500 0.7500 0.3359(4) 0.0127(17) Uani 1 4 d S . . C1 C 0.6899(3) 0.9068(4) -0.2633(4) 0.0232(15) Uani 1 1 d . . . H1A H 0.7123 0.9478 -0.2356 0.035 Uiso 1 1 calc R . . H1B H 0.6655 0.9219 -0.3166 0.035 Uiso 1 1 calc R . . H1C H 0.7262 0.8717 -0.2782 0.035 Uiso 1 1 calc R . . C2 C 0.6370(3) 0.8741(3) -0.2009(4) 0.0159(13) Uani 1 1 d . . . C3 C 0.5655(3) 0.8779(3) -0.2170(4) 0.0166(13) Uani 1 1 d . . . H3 H 0.5511 0.8955 -0.2724 0.020 Uiso 1 1 calc R . . C4 C 0.5119(3) 0.8580(3) -0.1581(4) 0.0189(14) Uani 1 1 d . . . C5 C 0.4360(3) 0.8691(3) -0.1834(4) 0.0253(15) Uani 1 1 d . . . H5A H 0.4189 0.8277 -0.2158 0.038 Uiso 1 1 calc R . . H5B H 0.4321 0.9113 -0.2202 0.038 Uiso 1 1 calc R . . H5C H 0.4073 0.8754 -0.1306 0.038 Uiso 1 1 calc R . . C6 C 0.3984(3) 0.6584(4) -0.1037(4) 0.0300(16) Uani 1 1 d . . . H6A H 0.4031 0.6802 -0.1615 0.045 Uiso 1 1 calc R . . H6B H 0.3511 0.6683 -0.0803 0.045 Uiso 1 1 calc R . . H6C H 0.4049 0.6071 -0.1088 0.045 Uiso 1 1 calc R . . C7 C 0.4532(3) 0.6881(3) -0.0436(4) 0.0203(14) Uani 1 1 d . . . C8 C 0.4310(3) 0.7140(3) 0.0376(4) 0.0185(13) Uani 1 1 d . . . H8 H 0.3819 0.7115 0.0508 0.022 Uiso 1 1 calc R . . C9 C 0.4755(3) 0.7431(3) 0.1000(4) 0.0160(13) Uani 1 1 d . . . C10 C 0.4472(3) 0.7581(3) 0.1898(4) 0.0218(14) Uani 1 1 d . . . H10A H 0.4646 0.7221 0.2307 0.033 Uiso 1 1 calc R . . H10B H 0.3953 0.7569 0.1885 0.033 Uiso 1 1 calc R . . H10C H 0.4631 0.8050 0.2089 0.033 Uiso 1 1 calc R . . C11 C 0.5357(3) 0.9600(3) 0.0928(4) 0.0227(15) Uani 1 1 d . . . H11A H 0.5785 0.9828 0.0700 0.034 Uiso 1 1 calc R . . H11B H 0.4967 0.9942 0.0931 0.034 Uiso 1 1 calc R . . H11C H 0.5232 0.9196 0.0557 0.034 Uiso 1 1 calc R . . C12 C 0.5492(3) 0.9345(3) 0.1847(4) 0.0188(13) Uani 1 1 d . . . C13 C 0.4986(3) 0.9464(3) 0.2491(4) 0.0204(14) Uani 1 1 d . . . H13 H 0.4596 0.9758 0.2344 0.024 Uiso 1 1 calc R . . C14 C 0.5006(3) 0.9187(3) 0.3338(4) 0.0181(14) Uani 1 1 d . . . C15 C 0.4406(4) 0.9349(4) 0.3955(4) 0.041(2) Uani 1 1 d . . . H15A H 0.4067 0.8955 0.3951 0.061 Uiso 1 1 calc R . . H15B H 0.4167 0.9783 0.3768 0.061 Uiso 1 1 calc R . . H15C H 0.4593 0.9412 0.4547 0.061 Uiso 1 1 calc R . . C16 C 0.4113(3) 0.6691(4) 0.4124(4) 0.0342(19) Uani 1 1 d . . . H16A H 0.3874 0.6982 0.3684 0.051 Uiso 1 1 calc R . . H16B H 0.3905 0.6783 0.4699 0.051 Uiso 1 1 calc R . . H16C H 0.4056 0.6190 0.3976 0.051 Uiso 1 1 calc R . . C17 C 0.4888(3) 0.6874(3) 0.4142(4) 0.0224(15) Uani 1 1 d . . . C18 C 0.5146(3) 0.7295(3) 0.4832(4) 0.0220(15) Uani 1 1 d . . . H18 H 0.4861 0.7340 0.5341 0.026 Uiso 1 1 calc R . . C19 C 0.5784(3) 0.7645(3) 0.4814(4) 0.0178(14) Uani 1 1 d . . . C20 C 0.5991(4) 0.8159(3) 0.5515(4) 0.0283(16) Uani 1 1 d . . . H20A H 0.6459 0.8033 0.5744 0.043 Uiso 1 1 calc R . . H20B H 0.5642 0.8143 0.5988 0.043 Uiso 1 1 calc R . . H20C H 0.6007 0.8639 0.5270 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01332(16) 0.01382(16) 0.00921(12) 0.00038(11) -0.00054(12) -0.00025(13) Tb2 0.01443(15) 0.01458(16) 0.00917(12) -0.00036(12) 0.00117(12) 0.00065(13) Tb3 0.01268(18) 0.01268(18) 0.0079(2) 0.000 0.000 0.000 O1 0.018(2) 0.017(2) 0.0104(19) 0.0020(17) -0.0067(17) 0.0014(19) O2 0.020(2) 0.023(2) 0.021(2) 0.0068(19) 0.0033(19) 0.005(2) O3 0.016(2) 0.018(2) 0.020(2) -0.0046(18) -0.0019(18) -0.0026(18) O4 0.012(2) 0.024(2) 0.0105(19) 0.0003(17) 0.0018(17) 0.0024(18) O5 0.020(2) 0.019(2) 0.012(2) -0.0004(17) 0.0021(17) 0.0036(19) O6 0.021(2) 0.024(2) 0.019(2) 0.0046(19) 0.0047(19) 0.008(2) O7 0.018(2) 0.025(2) 0.015(2) 0.0026(18) 0.0026(19) -0.0023(19) O8 0.020(2) 0.021(2) 0.0081(18) 0.0013(17) 0.0076(17) 0.0000(19) O9 0.017(3) 0.017(3) 0.012(4) 0.000 0.000 0.000 O10 0.015(2) 0.016(2) 0.0097(18) 0.0030(17) 0.0018(16) -0.0025(18) O11 0.012(2) 0.015(2) 0.0106(19) 0.0007(17) -0.0035(16) -0.0023(18) O12 0.014(3) 0.014(3) 0.009(4) 0.000 0.000 0.000 C1 0.023(4) 0.035(4) 0.011(3) 0.008(3) 0.000(3) -0.002(3) C2 0.025(4) 0.009(3) 0.014(3) -0.009(2) 0.000(3) -0.002(3) C3 0.019(3) 0.015(3) 0.016(3) 0.002(2) -0.004(3) 0.005(3) C4 0.022(3) 0.015(3) 0.020(3) 0.001(3) -0.006(3) 0.003(3) C5 0.019(3) 0.027(4) 0.030(3) 0.002(3) 0.004(3) 0.004(3) C6 0.022(4) 0.034(4) 0.034(4) -0.010(3) -0.004(3) 0.001(3) C7 0.019(3) 0.019(3) 0.022(3) 0.001(3) -0.002(3) 0.003(3) C8 0.017(3) 0.021(3) 0.018(3) -0.004(3) 0.002(3) 0.000(3) C9 0.023(4) 0.013(3) 0.012(3) 0.005(2) 0.004(3) 0.007(3) C10 0.021(3) 0.024(4) 0.020(3) 0.004(3) 0.003(3) 0.004(3) C11 0.019(4) 0.023(4) 0.026(3) 0.000(3) -0.003(3) 0.000(3) C12 0.025(4) 0.011(3) 0.020(3) -0.002(3) -0.008(3) -0.002(3) C13 0.021(3) 0.016(3) 0.025(3) -0.001(3) -0.004(3) 0.008(3) C14 0.016(3) 0.019(3) 0.019(3) -0.002(3) 0.003(3) 0.001(3) C15 0.032(4) 0.056(5) 0.034(4) 0.014(4) 0.008(4) 0.022(4) C16 0.020(4) 0.059(5) 0.023(4) 0.008(4) 0.004(3) -0.004(4) C17 0.022(4) 0.025(4) 0.021(3) 0.007(3) 0.004(3) 0.002(3) C18 0.022(4) 0.028(4) 0.017(3) 0.002(3) 0.006(3) 0.003(3) C19 0.023(3) 0.020(3) 0.011(3) 0.003(3) 0.003(3) 0.007(3) C20 0.043(4) 0.026(4) 0.016(3) 0.001(3) 0.009(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 Tb1 3.6371(4) 3_655 ? Tb1 Tb1 3.6371(4) 4_565 ? Tb1 Tb3 3.7203(5) . ? Tb1 O1 2.430(4) . ? Tb1 O1 2.428(4) 3_655 ? Tb1 O2 2.352(4) . ? Tb1 O3 2.316(4) . ? Tb1 O4 2.327(4) . ? Tb1 O9 2.5811(7) . ? Tb1 O10 2.322(4) . ? Tb1 O10 2.314(4) 4_565 ? Tb2 Tb2 3.6058(4) 4_565 ? Tb2 Tb2 3.6058(4) 3_655 ? Tb2 Tb3 3.7284(5) . ? Tb2 O5 2.334(4) . ? Tb2 O6 2.282(4) . ? Tb2 O7 2.366(4) 4_565 ? Tb2 O8 2.458(4) . ? Tb2 O8 2.409(4) 4_565 ? Tb2 O11 2.347(4) . ? Tb2 O11 2.301(4) 4_565 ? Tb2 O12 2.5622(7) . ? Tb3 Tb1 3.7203(5) 3_655 ? Tb3 Tb1 3.7203(5) 2_665 ? Tb3 Tb1 3.7203(5) 4_565 ? Tb3 O9 2.907(7) . ? Tb3 O10 2.428(4) . ? Tb3 O10 2.428(4) 2_665 ? Tb3 O10 2.428(4) 3_655 ? Tb3 O10 2.428(4) 4_565 ? Tb3 O11 2.434(4) . ? Tb3 O11 2.434(4) 4_565 ? Tb3 O11 2.434(4) 2_665 ? Tb3 O11 2.434(4) 3_655 ? O1 Tb1 2.428(4) 4_565 ? O1 C2 1.314(7) . ? O2 C4 1.255(6) . ? O3 C7 1.274(7) . ? O4 C9 1.284(7) . ? O5 C12 1.272(7) . ? O6 C14 1.263(7) . ? O7 Tb2 2.366(4) 3_655 ? O7 C17 1.240(7) . ? O8 Tb2 2.409(4) 3_655 ? O8 C19 1.303(7) . ? O9 Tb1 2.5811(7) 4_565 ? O9 Tb1 2.5811(7) 2_665 ? O9 Tb1 2.5811(7) 3_655 ? O9 H9O 0.841(10) . ? O10 Tb1 2.314(4) 3_655 ? O10 H10O 0.837(10) . ? O11 Tb2 2.301(4) 3_655 ? O11 H11O 0.839(10) . ? O12 Tb2 2.5623(7) 3_655 ? O12 Tb2 2.5623(7) 4_565 ? O12 Tb2 2.5623(7) 2_665 ? C1 H1A 0.980 . ? C1 H1B 0.980 . ? C1 H1C 0.980 . ? C1 C2 1.514(8) . ? C2 C3 1.375(8) . ? C3 H3 0.950 . ? C3 C4 1.408(8) . ? C4 C5 1.499(8) . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C6 C7 1.495(8) . ? C7 C8 1.401(8) . ? C8 H8 0.950 . ? C8 C9 1.386(8) . ? C9 C10 1.503(8) . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C11 C12 1.509(8) . ? C12 C13 1.390(8) . ? C13 H13 0.950 . ? C13 C14 1.400(8) . ? C14 C15 1.507(8) . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C16 C17 1.504(9) . ? C17 C18 1.408(9) . ? C18 H18 0.950 . ? C18 C19 1.375(8) . ? C19 C20 1.499(8) . ? C20 H20A 0.980 . ? C20 H20B 0.980 . ? C20 H20C 0.980 . ? 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 Tb1 Tb1 Tb1 90.0 3_655 4_565 ? Tb1 Tb1 Tb3 60.737(4) 3_655 . ? Tb1 Tb1 Tb3 60.736(4) 4_565 . ? Tb1 Tb1 O1 41.55(9) 3_655 3_655 ? Tb1 Tb1 O1 103.10(9) 3_655 . ? Tb1 Tb1 O1 103.11(9) 4_565 3_655 ? Tb1 Tb1 O1 41.51(9) 4_565 . ? Tb1 Tb1 O2 159.53(10) 3_655 . ? Tb1 Tb1 O2 96.76(10) 4_565 . ? Tb1 Tb1 O3 96.51(10) 3_655 . ? Tb1 Tb1 O3 165.13(10) 4_565 . ? Tb1 Tb1 O4 114.35(10) 3_655 . ? Tb1 Tb1 O4 114.90(10) 4_565 . ? Tb1 Tb1 O9 45.206(14) 3_655 . ? Tb1 Tb1 O9 45.206(14) 4_565 . ? Tb1 Tb1 O10 96.19(9) 3_655 4_565 ? Tb1 Tb1 O10 38.25(9) 3_655 . ? Tb1 Tb1 O10 38.41(9) 4_565 4_565 ? Tb1 Tb1 O10 96.16(9) 4_565 . ? Tb3 Tb1 O1 101.23(9) . . ? Tb3 Tb1 O1 101.27(9) . 3_655 ? Tb3 Tb1 O2 138.89(10) . . ? Tb3 Tb1 O3 133.96(10) . . ? Tb3 Tb1 O4 79.84(9) . . ? Tb3 Tb1 O9 51.13(16) . . ? Tb3 Tb1 O10 39.47(9) . . ? Tb3 Tb1 O10 39.42(9) . 4_565 ? O1 Tb1 O1 87.20(17) . 3_655 ? O1 Tb1 O2 70.78(13) . . ? O1 Tb1 O2 117.98(13) 3_655 . ? O1 Tb1 O3 123.69(13) . . ? O1 Tb1 O3 73.87(13) 3_655 . ? O1 Tb1 O4 136.47(13) . . ? O1 Tb1 O4 135.78(13) 3_655 . ? O1 Tb1 O9 65.12(14) . . ? O1 Tb1 O9 65.15(14) 3_655 . ? O1 Tb1 O10 129.65(13) . . ? O1 Tb1 O10 129.77(13) 3_655 4_565 ? O1 Tb1 O10 76.58(13) 3_655 . ? O1 Tb1 O10 76.69(13) . 4_565 ? O2 Tb1 O3 72.79(14) . . ? O2 Tb1 O4 80.22(13) . . ? O2 Tb1 O9 135.65(13) . . ? O2 Tb1 O10 157.50(13) . . ? O2 Tb1 O10 101.12(14) . 4_565 ? O3 Tb1 O4 74.47(14) . . ? O3 Tb1 O9 137.85(12) . . ? O3 Tb1 O10 97.22(14) . . ? O3 Tb1 O10 152.37(13) . 4_565 ? O4 Tb1 O9 130.97(19) . . ? O4 Tb1 O10 77.65(13) . . ? O4 Tb1 O10 77.95(13) . 4_565 ? O9 Tb1 O10 64.79(15) . . ? O9 Tb1 O10 64.89(15) . 4_565 ? O10 Tb1 O10 78.21(18) . 4_565 ? Tb2 Tb2 Tb2 90.0 4_565 3_655 ? Tb2 Tb2 Tb3 61.083(4) 4_565 . ? Tb2 Tb2 Tb3 61.083(4) 3_655 . ? Tb2 Tb2 O5 118.08(10) 4_565 . ? Tb2 Tb2 O5 111.41(10) 3_655 . ? Tb2 Tb2 O6 160.87(10) 4_565 . ? Tb2 Tb2 O6 98.89(11) 3_655 . ? Tb2 Tb2 O7 92.30(10) 4_565 4_565 ? Tb2 Tb2 O7 167.17(9) 3_655 4_565 ? Tb2 Tb2 O8 42.72(9) 4_565 4_565 ? Tb2 Tb2 O8 103.04(9) 4_565 . ? Tb2 Tb2 O8 103.31(9) 3_655 4_565 ? Tb2 Tb2 O8 41.67(9) 3_655 . ? Tb2 Tb2 O11 39.58(9) 4_565 4_565 ? Tb2 Tb2 O11 96.55(9) 4_565 . ? Tb2 Tb2 O11 96.68(9) 3_655 4_565 ? Tb2 Tb2 O11 38.66(9) 3_655 . ? Tb2 Tb2 O12 45.281(15) 4_565 . ? Tb2 Tb2 O12 45.281(15) 3_655 . ? Tb3 Tb2 O5 79.52(9) . . ? Tb3 Tb2 O6 137.93(10) . . ? Tb3 Tb2 O7 130.56(9) . 4_565 ? Tb3 Tb2 O8 101.78(9) . . ? Tb3 Tb2 O8 102.81(9) . 4_565 ? Tb3 Tb2 O11 39.60(9) . . ? Tb3 Tb2 O11 39.33(9) . 4_565 ? Tb3 Tb2 O12 52.53(15) . . ? O5 Tb2 O6 74.39(14) . . ? O5 Tb2 O7 78.50(13) . 4_565 ? O5 Tb2 O8 131.98(14) . . ? O5 Tb2 O8 140.76(14) . 4_565 ? O5 Tb2 O11 74.81(13) . . ? O5 Tb2 O11 79.46(13) . 4_565 ? O5 Tb2 O12 131.88(18) . . ? O6 Tb2 O7 75.42(14) . 4_565 ? O6 Tb2 O8 73.83(14) . . ? O6 Tb2 O8 118.30(13) . 4_565 ? O6 Tb2 O11 100.97(14) . . ? O6 Tb2 O11 153.02(13) . 4_565 ? O6 Tb2 O12 138.15(13) . . ? O7 Tb2 O8 70.47(13) 4_565 4_565 ? O7 Tb2 O8 125.64(13) 4_565 . ? O7 Tb2 O11 93.11(13) 4_565 4_565 ? O7 Tb2 O11 152.99(13) 4_565 . ? O7 Tb2 O12 133.84(12) 4_565 . ? O8 Tb2 O8 86.47(18) . 4_565 ? O8 Tb2 O11 77.01(12) . . ? O8 Tb2 O11 78.86(13) 4_565 4_565 ? O8 Tb2 O11 130.96(13) 4_565 . ? O8 Tb2 O11 130.74(13) . 4_565 ? O8 Tb2 O12 64.61(13) . . ? O8 Tb2 O12 65.29(13) 4_565 . ? O11 Tb2 O11 78.11(18) . 4_565 ? O11 Tb2 O12 65.90(14) . . ? O11 Tb2 O12 66.52(14) 4_565 . ? Tb1 Tb3 Tb1 58.526(8) 3_655 2_665 ? Tb1 Tb3 Tb1 87.466(14) 3_655 4_565 ? Tb1 Tb3 Tb1 58.526(8) 2_665 4_565 ? Tb1 Tb3 O9 43.733(7) 3_655 . ? Tb1 Tb3 O9 43.733(7) 2_665 . ? Tb1 Tb3 O9 43.733(7) 4_565 . ? Tb1 Tb3 O10 92.22(9) 3_655 2_665 ? Tb1 Tb3 O10 37.45(9) 3_655 3_655 ? Tb1 Tb3 O10 92.10(9) 3_655 4_565 ? Tb1 Tb3 O10 37.25(9) 3_655 . ? Tb1 Tb3 O10 37.45(9) 2_665 2_665 ? Tb1 Tb3 O10 37.24(9) 2_665 3_655 ? Tb1 Tb3 O10 92.22(9) 2_665 4_565 ? Tb1 Tb3 O10 92.10(9) 2_665 . ? Tb1 Tb3 O10 37.24(9) 4_565 2_665 ? Tb1 Tb3 O10 92.10(9) 4_565 3_655 ? Tb1 Tb3 O10 37.45(9) 4_565 4_565 ? Tb1 Tb3 O10 92.22(9) 4_565 . ? Tb1 Tb3 O11 112.96(9) 3_655 . ? Tb1 Tb3 O11 165.41(8) 3_655 4_565 ? Tb1 Tb3 O11 111.67(9) 3_655 2_665 ? Tb1 Tb3 O11 77.97(8) 3_655 3_655 ? Tb1 Tb3 O11 165.41(8) 2_665 . ? Tb1 Tb3 O11 111.67(9) 2_665 4_565 ? Tb1 Tb3 O11 77.97(8) 2_665 2_665 ? Tb1 Tb3 O11 112.96(9) 2_665 3_655 ? Tb1 Tb3 O11 111.67(9) 4_565 . ? Tb1 Tb3 O11 77.97(8) 4_565 4_565 ? Tb1 Tb3 O11 112.96(9) 4_565 2_665 ? Tb1 Tb3 O11 165.41(8) 4_565 3_655 ? O9 Tb3 O10 58.40(8) . . ? O9 Tb3 O10 58.39(8) . 2_665 ? O9 Tb3 O10 58.39(8) . 3_655 ? O9 Tb3 O10 58.39(8) . 4_565 ? O9 Tb3 O11 121.70(8) . . ? O9 Tb3 O11 121.70(8) . 4_565 ? O9 Tb3 O11 121.70(8) . 2_665 ? O9 Tb3 O11 121.70(8) . 3_655 ? O10 Tb3 O10 74.06(8) 2_665 3_655 ? O10 Tb3 O10 74.06(8) 2_665 4_565 ? O10 Tb3 O10 116.79(17) 3_655 4_565 ? O10 Tb3 O10 116.79(17) . 2_665 ? O10 Tb3 O10 74.06(8) . 3_655 ? O10 Tb3 O10 74.06(8) . 4_565 ? O10 Tb3 O11 76.91(12) . . ? O10 Tb3 O11 141.01(13) 2_665 . ? O10 Tb3 O11 142.95(13) 3_655 . ? O10 Tb3 O11 75.68(12) 4_565 . ? O10 Tb3 O11 75.68(12) 2_665 4_565 ? O10 Tb3 O11 141.01(13) 3_655 4_565 ? O10 Tb3 O11 76.91(12) 4_565 4_565 ? O10 Tb3 O11 142.95(13) . 4_565 ? O10 Tb3 O11 76.91(12) 2_665 2_665 ? O10 Tb3 O11 75.68(12) 3_655 2_665 ? O10 Tb3 O11 142.95(13) 4_565 2_665 ? O10 Tb3 O11 141.01(13) . 2_665 ? O10 Tb3 O11 142.95(13) 2_665 3_655 ? O10 Tb3 O11 76.91(12) 3_655 3_655 ? O10 Tb3 O11 141.01(13) 4_565 3_655 ? O10 Tb3 O11 75.68(12) . 3_655 ? O11 Tb3 O11 73.97(8) . 4_565 ? O11 Tb3 O11 116.60(17) . 2_665 ? O11 Tb3 O11 73.97(8) 4_565 2_665 ? O11 Tb3 O11 73.97(8) . 3_655 ? O11 Tb3 O11 116.60(17) 4_565 3_655 ? O11 Tb3 O11 73.97(8) 2_665 3_655 ? Tb1 O1 Tb1 96.94(12) . 4_565 ? Tb1 O1 C2 130.1(4) . . ? Tb1 O1 C2 128.3(3) 4_565 . ? Tb1 O2 C4 132.3(4) . . ? Tb1 O3 C7 130.9(4) . . ? Tb1 O4 C9 132.4(4) . . ? Tb2 O5 C12 133.9(4) . . ? Tb2 O6 C14 135.0(4) . . ? Tb2 O7 C17 136.4(4) 3_655 . ? Tb2 O8 Tb2 95.61(12) . 3_655 ? Tb2 O8 C19 124.5(4) . . ? Tb2 O8 C19 131.5(4) 3_655 . ? Tb1 O9 Tb1 89.59(3) . 4_565 ? Tb1 O9 Tb1 170.3(3) . 2_665 ? Tb1 O9 Tb1 89.59(3) 4_565 2_665 ? Tb1 O9 Tb1 89.59(3) . 3_655 ? Tb1 O9 Tb1 170.3(3) 4_565 3_655 ? Tb1 O9 Tb1 89.59(3) 2_665 3_655 ? Tb1 O9 Tb3 85.14(16) . . ? Tb1 O9 Tb3 85.14(16) 4_565 . ? Tb1 O9 Tb3 85.14(16) 2_665 . ? Tb1 O9 Tb3 85.14(16) 3_655 . ? Tb1 O9 H9O 94.86(16) . . ? Tb1 O9 H9O 94.86(16) 4_565 . ? Tb1 O9 H9O 94.86(16) 2_665 . ? Tb1 O9 H9O 94.86(16) 3_655 . ? Tb3 O9 H9O 180.000(4) . . ? Tb1 O10 Tb1 103.35(13) . 3_655 ? Tb1 O10 Tb3 103.08(15) . . ? Tb1 O10 Tb3 103.33(15) 3_655 . ? Tb1 O10 H10O 111(4) . . ? Tb1 O10 H10O 121(4) 3_655 . ? Tb3 O10 H10O 112(4) . . ? Tb2 O11 Tb2 101.76(13) . 3_655 ? Tb2 O11 Tb3 102.48(14) . . ? Tb2 O11 Tb3 103.86(15) 3_655 . ? Tb2 O11 H11O 112(4) . . ? Tb2 O11 H11O 122(4) 3_655 . ? Tb3 O11 H11O 113(4) . . ? Tb2 O12 Tb2 89.44(3) . 3_655 ? Tb2 O12 Tb2 89.44(3) . 4_565 ? Tb2 O12 Tb2 168.6(3) 3_655 4_565 ? Tb2 O12 Tb2 168.6(3) . 2_665 ? Tb2 O12 Tb2 89.44(3) 3_655 2_665 ? Tb2 O12 Tb2 89.44(3) 4_565 2_665 ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1A C1 C2 109.5 . . ? H1B C1 H1C 109.5 . . ? H1B C1 C2 109.5 . . ? H1C C1 C2 109.5 . . ? O1 C2 C1 115.0(5) . . ? O1 C2 C3 124.1(5) . . ? C1 C2 C3 120.9(5) . . ? C2 C3 H3 117.4 . . ? C2 C3 C4 125.3(5) . . ? H3 C3 C4 117.4 . . ? O2 C4 C3 123.4(6) . . ? O2 C4 C5 117.6(6) . . ? C3 C4 C5 119.0(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6A C6 C7 109.5 . . ? H6B C6 H6C 109.5 . . ? H6B C6 C7 109.5 . . ? H6C C6 C7 109.5 . . ? O3 C7 C6 117.2(5) . . ? O3 C7 C8 124.7(6) . . ? C6 C7 C8 118.0(6) . . ? C7 C8 H8 117.7 . . ? C7 C8 C9 124.6(6) . . ? H8 C8 C9 117.7 . . ? O4 C9 C8 125.5(5) . . ? O4 C9 C10 115.3(5) . . ? C8 C9 C10 119.3(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11A C11 C12 109.5 . . ? H11B C11 H11C 109.5 . . ? H11B C11 C12 109.5 . . ? H11C C11 C12 109.5 . . ? O5 C12 C11 116.0(5) . . ? O5 C12 C13 124.4(5) . . ? C11 C12 C13 119.6(5) . . ? C12 C13 H13 117.4 . . ? C12 C13 C14 125.3(6) . . ? H13 C13 C14 117.4 . . ? O6 C14 C13 124.3(5) . . ? O6 C14 C15 116.7(5) . . ? C13 C14 C15 119.0(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16A C16 C17 109.5 . . ? H16B C16 H16C 109.5 . . ? H16B C16 C17 109.5 . . ? H16C C16 C17 109.5 . . ? O7 C17 C16 117.2(6) . . ? O7 C17 C18 124.1(6) . . ? C16 C17 C18 118.7(6) . . ? C17 C18 H18 118.0 . . ? C17 C18 C19 124.0(6) . . ? H18 C18 C19 118.0 . . ? O8 C19 C18 124.1(5) . . ? O8 C19 C20 114.2(5) . . ? C18 C19 C20 121.7(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O10 H10O O5 0.837(10) 2.02(2) 2.822(5) 160(6) 3_655 O11 H11O O4 0.839(10) 2.01(2) 2.805(5) 159(5) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.840 _refine_diff_density_min -0.888 _refine_diff_density_rms 0.177 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 0.750 -0.016 276 80 ' ' 2 0.750 0.250 -0.016 276 80 ' ' 3 0.250 0.250 0.236 6 1 ' ' 4 0.250 0.250 0.356 8 1 ' ' 5 0.750 0.750 0.659 9 1 ' ' 6 0.750 0.750 0.781 5 1 ' ' _platon_squeeze_details ; Four molecules of water per asymmetric unit removed with SQUEEZE ;