# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Kathryn Preuss' _publ_contact_author_address ;Dept. of Chemistry University of Guelph 50 Stone Rd. E. Guelph, ON., Canada N1G 2W1 ; _publ_contact_author_email kpreuss@uoguelph.ca _publ_contact_author_phone '519-824-4120 x.56711' loop_ _publ_author_name _publ_author_address K.E.Preuss ;Dept. of Chemistry University of Guelph 50 Stone Rd. E. Guelph, ON., Canada N1G 2W1 ; E.M.Fatila ;Dept. of Chemistry University of Guelph 50 Stone Rd. E. Guelph, ON., Canada N1G 2W1 ; E.E.Hetherington ;Dept. of Chemistry University of Guelph 50 Stone Rd. E. Guelph, ON., Canada N1G 2W1 ; M.Jennings ;Dept. of Chemistry University of Western Ontario 185 Chelsea Ave. London, ON., Canada N6J 3J5 ; A.Lough ;Dept. of Chemistry University of Toronto Lash Miller Building Toronto, ON., Canada M5S 3H6 ; _publ_section_title ; Syntheses and Crystal Structures of Anhydrous Ln(hfac)3(monoglyme). Ln = La, Ce, Pr, Sm, Eu, Gd, Tb, Dy, Er, Tm. ; # Attachment '- DyCif.txt' data_pbca _database_code_depnum_ccdc_archive 'CCDC 833373' #TrackingRef '- DyCif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H13 Dy F18 O8' _chemical_formula_sum 'C19 H13 Dy F18 O8' _chemical_formula_weight 873.79 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' F F 0.0171 0.0103 '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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.516(2) _cell_length_b 15.7494(18) _cell_length_c 20.804(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5739.0(11) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9924 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.05 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3352 _exptl_absorpt_coefficient_mu 2.762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3879 _exptl_absorpt_correction_T_max 0.8697 _exptl_absorpt_process_details SADABS _exptl_special_details ; 2 disordered CF3's 60/40 isotropic ; _diffrn_ambient_temperature 150(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_reflns_number 56889 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5065 _reflns_number_gt 3645 _reflns_threshold_expression I>\2(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0506P)^2^+24.9189P] 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 5065 _refine_ls_number_parameters 409 _refine_ls_number_restraints 160 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.073 _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 0.13396(2) 0.653046(19) 0.239990(15) 0.03784(13) Uani 1 1 d U . . O1 O 0.2707(3) 0.6735(4) 0.2341(2) 0.0585(13) Uani 1 1 d U . . C2 C 0.3248(6) 0.6210(8) 0.2675(5) 0.091(3) Uani 1 1 d U . . H2A H 0.3318 0.5678 0.2439 0.137 Uiso 1 1 calc R . . H2B H 0.3056 0.6086 0.3107 0.137 Uiso 1 1 calc R . . H2C H 0.3737 0.6508 0.2707 0.137 Uiso 1 1 calc R . . C3 C 0.2989(5) 0.7032(6) 0.1734(4) 0.070(2) Uani 1 1 d U . . H3A H 0.2912 0.6594 0.1399 0.084 Uiso 1 1 calc R . . H3B H 0.3542 0.7158 0.1765 0.084 Uiso 1 1 calc R . . C4 C 0.2566(6) 0.7797(6) 0.1573(4) 0.074(2) Uani 1 1 d U . . H4A H 0.2675 0.7962 0.1123 0.089 Uiso 1 1 calc R . . H4B H 0.2729 0.8268 0.1857 0.089 Uiso 1 1 calc R . . O5 O 0.1750(4) 0.7646(3) 0.1652(3) 0.0618(14) Uani 1 1 d U . . C6 C 0.1326(6) 0.8386(5) 0.1500(5) 0.081(3) Uani 1 1 d U . . H6A H 0.1429 0.8826 0.1821 0.122 Uiso 1 1 calc R . . H6B H 0.0780 0.8250 0.1500 0.122 Uiso 1 1 calc R . . H6C H 0.1475 0.8592 0.1074 0.122 Uiso 1 1 calc R . . O11 O 0.0755(3) 0.7764(3) 0.2763(2) 0.0436(11) Uani 1 1 d U . . C12 C 0.0651(4) 0.8097(4) 0.3301(4) 0.0403(16) Uani 1 1 d U . . C13 C 0.0972(4) 0.7865(4) 0.3882(3) 0.0429(16) Uani 1 1 d U . . H13A H 0.0825 0.8149 0.4265 0.052 Uiso 1 1 calc R . . C14 C 0.1512(4) 0.7215(4) 0.3909(3) 0.0365(15) Uani 1 1 d U A . O15 O 0.1761(3) 0.6779(3) 0.3450(2) 0.0417(11) Uani 1 1 d U . . C16 C 0.0109(5) 0.8851(5) 0.3286(4) 0.057(2) Uani 1 1 d U . . C17 C 0.1852(4) 0.6992(4) 0.4556(3) 0.0471(18) Uani 1 1 d DU . . F11 F -0.0567(4) 0.8643(4) 0.3076(4) 0.126(3) Uani 1 1 d U . . F12 F 0.0015(4) 0.9220(4) 0.3845(3) 0.126(3) Uani 1 1 d U . . F13 F 0.0337(4) 0.9444(3) 0.2897(3) 0.104(2) Uani 1 1 d U . . F14A F 0.2622(4) 0.6996(6) 0.4542(4) 0.066(2) Uiso 0.60 1 d PDU A 1 F15A F 0.1686(6) 0.6213(5) 0.4741(4) 0.074(3) Uiso 0.60 1 d PDU A 1 F16A F 0.1664(6) 0.7514(5) 0.5034(4) 0.065(2) Uiso 0.60 1 d PDU A 1 F14B F 0.1348(8) 0.6457(8) 0.4847(6) 0.067(4) Uiso 0.40 1 d PDU A 2 F15B F 0.1984(8) 0.7667(7) 0.4935(6) 0.057(3) Uiso 0.40 1 d PDU A 2 F16B F 0.2476(7) 0.6523(9) 0.4521(7) 0.076(4) Uiso 0.40 1 d PDU A 2 O21 O 0.0354(3) 0.5985(3) 0.3032(2) 0.0455(11) Uani 1 1 d U . . C22 C 0.0350(4) 0.5455(5) 0.3486(3) 0.0458(16) Uani 1 1 d U . . C23 C 0.0911(5) 0.4864(5) 0.3638(4) 0.0530(18) Uani 1 1 d U . . H23A H 0.0853 0.4516 0.4007 0.064 Uiso 1 1 calc R . . C24 C 0.1557(5) 0.4778(4) 0.3253(4) 0.0519(18) Uani 1 1 d U . . O25 O 0.1738(3) 0.5208(3) 0.2769(2) 0.0481(12) Uani 1 1 d U . . C26 C -0.0349(5) 0.5508(6) 0.3913(4) 0.062(2) Uani 1 1 d U . . C27 C 0.2132(8) 0.4086(6) 0.3425(5) 0.088(3) Uani 1 1 d U . . F21 F -0.0422(4) 0.6252(4) 0.4177(3) 0.108(2) Uani 1 1 d U . . F22 F -0.0359(3) 0.4909(4) 0.4374(3) 0.102(2) Uani 1 1 d U . . F23 F -0.0979(3) 0.5362(3) 0.3578(3) 0.0761(14) Uani 1 1 d U . . F24 F 0.2806(5) 0.4336(7) 0.3365(7) 0.253(6) Uani 1 1 d U . . F25 F 0.2052(9) 0.3451(6) 0.3060(4) 0.250(6) Uani 1 1 d U . . F26 F 0.2064(4) 0.3772(4) 0.3997(3) 0.0961(18) Uani 1 1 d U . . O31 O 0.0329(3) 0.6627(3) 0.1679(2) 0.0557(13) Uani 1 1 d U . . C32 C 0.0248(5) 0.6473(5) 0.1090(4) 0.0553(19) Uani 1 1 d U B . C33 C 0.0740(5) 0.6002(5) 0.0700(4) 0.0510(18) Uani 1 1 d U . . H33A H 0.0611 0.5910 0.0262 0.061 Uiso 1 1 calc R . . C34 C 0.1401(5) 0.5673(4) 0.0937(3) 0.0447(16) Uani 1 1 d U . . O35 O 0.1669(3) 0.5737(3) 0.1495(2) 0.0465(12) Uani 1 1 d U . . C36 C -0.0475(6) 0.6832(7) 0.0786(4) 0.098(4) Uani 1 1 d DU . . C37 C 0.1908(7) 0.5162(6) 0.0481(4) 0.071(2) Uani 1 1 d U . . F31A F -0.0770(7) 0.7450(7) 0.1098(5) 0.100(3) Uiso 0.60 1 d PDU B 1 F32A F -0.1021(6) 0.6178(7) 0.0921(5) 0.097(3) Uiso 0.60 1 d PDU B 1 F33A F -0.0470(6) 0.6925(7) 0.0168(4) 0.086(3) Uiso 0.60 1 d PDU B 1 F31B F -0.0576(9) 0.6498(10) 0.0182(6) 0.084(5) Uiso 0.40 1 d PDU B 2 F32B F -0.0351(10) 0.7740(9) 0.0755(9) 0.107(5) Uiso 0.40 1 d PDU B 2 F33B F -0.1085(8) 0.6895(13) 0.1110(8) 0.110(5) Uiso 0.40 1 d PDU B 2 F34 F 0.1907(6) 0.4352(4) 0.0665(3) 0.154(4) Uani 1 1 d U . . F35 F 0.2602(4) 0.5420(6) 0.0477(3) 0.146(3) Uani 1 1 d U . . F36 F 0.1691(4) 0.5156(4) -0.0117(2) 0.101(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0506(2) 0.03439(19) 0.0286(2) -0.00318(13) -0.00035(15) 0.00617(14) O1 0.056(3) 0.081(4) 0.038(3) -0.006(3) 0.002(2) -0.006(3) C2 0.055(5) 0.158(10) 0.061(6) 0.007(6) 0.002(5) 0.020(6) C3 0.062(5) 0.090(6) 0.058(5) 0.000(5) 0.011(4) -0.019(4) C4 0.094(6) 0.072(5) 0.056(5) -0.006(4) 0.004(5) -0.028(4) O5 0.092(4) 0.046(3) 0.047(3) 0.005(2) 0.016(3) 0.004(3) C6 0.144(9) 0.050(5) 0.051(5) 0.013(4) 0.017(6) 0.025(5) O11 0.058(3) 0.036(2) 0.037(3) -0.0007(19) 0.000(2) 0.010(2) C12 0.046(4) 0.028(3) 0.047(4) -0.002(3) 0.010(3) 0.003(3) C13 0.053(4) 0.039(4) 0.037(4) -0.004(3) 0.004(3) 0.002(3) C14 0.043(4) 0.038(4) 0.028(3) -0.004(3) 0.006(3) -0.005(3) O15 0.051(3) 0.041(2) 0.032(2) -0.0036(19) 0.003(2) 0.010(2) C16 0.065(5) 0.048(4) 0.057(5) -0.002(4) 0.008(4) 0.020(4) C17 0.061(5) 0.042(4) 0.038(4) -0.006(3) 0.005(4) 0.005(4) F11 0.061(4) 0.090(4) 0.227(9) -0.027(5) -0.024(4) 0.030(3) F12 0.183(7) 0.113(5) 0.083(4) -0.028(3) -0.002(4) 0.102(5) F13 0.131(5) 0.052(3) 0.128(5) 0.030(3) 0.025(4) 0.038(3) O21 0.053(3) 0.043(3) 0.040(3) 0.001(2) -0.002(2) 0.002(2) C22 0.055(4) 0.047(4) 0.035(4) -0.001(3) -0.005(3) -0.008(3) C23 0.070(5) 0.046(4) 0.042(4) 0.007(3) -0.003(4) -0.004(4) C24 0.076(5) 0.033(4) 0.047(5) 0.000(3) -0.004(4) 0.006(3) O25 0.069(3) 0.040(2) 0.035(3) -0.004(2) 0.000(2) 0.014(2) C26 0.061(5) 0.076(5) 0.049(5) 0.006(4) 0.003(4) -0.009(4) C27 0.128(8) 0.071(6) 0.065(6) 0.022(4) 0.014(6) 0.048(6) F21 0.100(5) 0.109(4) 0.116(5) -0.052(4) 0.061(4) -0.036(4) F22 0.079(4) 0.148(5) 0.080(4) 0.057(4) 0.010(3) -0.005(4) F23 0.060(3) 0.081(3) 0.087(4) 0.016(3) -0.002(3) -0.009(3) F24 0.111(6) 0.239(9) 0.409(16) 0.244(10) 0.094(8) 0.105(6) F25 0.523(18) 0.137(6) 0.089(5) -0.044(5) -0.083(9) 0.223(8) F26 0.124(5) 0.090(4) 0.074(4) 0.028(3) -0.013(3) 0.035(4) O31 0.052(3) 0.080(4) 0.035(3) -0.001(2) -0.003(2) 0.012(3) C32 0.053(5) 0.078(6) 0.035(4) 0.012(4) -0.004(3) -0.010(4) C33 0.066(5) 0.051(4) 0.035(4) 0.005(3) -0.006(3) -0.013(3) C34 0.077(5) 0.026(3) 0.032(4) -0.003(3) 0.005(3) -0.006(3) O35 0.063(3) 0.045(3) 0.032(3) -0.008(2) 0.000(2) 0.009(2) C36 0.069(7) 0.195(13) 0.030(5) 0.010(6) -0.003(4) 0.004(7) C37 0.111(7) 0.068(5) 0.035(4) -0.012(4) -0.008(5) 0.036(5) F34 0.317(11) 0.070(3) 0.074(4) 0.011(3) 0.058(6) 0.088(5) F35 0.092(4) 0.237(8) 0.108(5) -0.091(6) 0.024(4) 0.025(5) F36 0.161(6) 0.108(4) 0.035(3) -0.020(3) 0.000(3) 0.042(4) _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 O11 2.322(4) . ? Dy1 O31 2.325(5) . ? Dy1 O25 2.327(5) . ? Dy1 O35 2.331(4) . ? Dy1 O21 2.335(5) . ? Dy1 O15 2.340(5) . ? Dy1 O1 2.420(6) . ? Dy1 O5 2.456(5) . ? O1 C3 1.434(10) . ? O1 C2 1.436(11) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.454(13) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O5 1.458(11) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O5 C6 1.417(10) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O11 C12 1.249(8) . ? C12 C13 1.384(10) . ? C12 C16 1.519(10) . ? C13 C14 1.395(9) . ? C13 H13A 0.9500 . ? C14 O15 1.253(7) . ? C14 C17 1.514(10) . ? C16 F13 1.299(10) . ? C16 F11 1.305(10) . ? C16 F12 1.310(10) . ? C17 F15A 1.319(9) . ? C17 F16B 1.322(11) . ? C17 F16A 1.331(9) . ? C17 F15B 1.344(11) . ? C17 F14A 1.350(9) . ? C17 F14B 1.362(11) . ? O21 C22 1.259(8) . ? C22 C23 1.389(10) . ? C22 C26 1.515(11) . ? C23 C24 1.393(11) . ? C23 H23A 0.9500 . ? C24 O25 1.254(9) . ? C24 C27 1.526(12) . ? C26 F21 1.300(10) . ? C26 F23 1.326(10) . ? C26 F22 1.345(10) . ? C27 F24 1.251(15) . ? C27 F25 1.264(13) . ? C27 F26 1.294(11) . ? O31 C32 1.257(9) . ? C32 C33 1.397(11) . ? C32 C36 1.525(13) . ? C33 C34 1.361(11) . ? C33 H33A 0.9500 . ? C34 O35 1.257(8) . ? C34 C37 1.529(11) . ? C36 F33B 1.267(13) . ? C36 F31A 1.279(11) . ? C36 F33A 1.293(10) . ? C36 F31B 1.372(12) . ? C36 F32A 1.433(11) . ? C36 F32B 1.447(13) . ? C37 F35 1.281(12) . ? C37 F36 1.299(9) . ? C37 F34 1.331(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Dy1 O31 79.60(18) . . ? O11 Dy1 O25 140.68(16) . . ? O31 Dy1 O25 119.98(19) . . ? O11 Dy1 O35 145.09(16) . . ? O31 Dy1 O35 72.70(18) . . ? O25 Dy1 O35 73.28(16) . . ? O11 Dy1 O21 78.37(16) . . ? O31 Dy1 O21 79.92(18) . . ? O25 Dy1 O21 72.91(17) . . ? O35 Dy1 O21 116.14(17) . . ? O11 Dy1 O15 72.28(16) . . ? O31 Dy1 O15 146.32(17) . . ? O25 Dy1 O15 75.33(16) . . ? O35 Dy1 O15 139.93(17) . . ? O21 Dy1 O15 76.62(17) . . ? O11 Dy1 O1 109.99(18) . . ? O31 Dy1 O1 135.39(18) . . ? O25 Dy1 O1 80.7(2) . . ? O35 Dy1 O1 77.61(18) . . ? O21 Dy1 O1 144.04(18) . . ? O15 Dy1 O1 73.29(17) . . ? O11 Dy1 O5 74.74(17) . . ? O31 Dy1 O5 76.5(2) . . ? O25 Dy1 O5 139.64(19) . . ? O35 Dy1 O5 78.43(17) . . ? O21 Dy1 O5 146.87(18) . . ? O15 Dy1 O5 112.33(18) . . ? O1 Dy1 O5 65.3(2) . . ? C3 O1 C2 112.7(7) . . ? C3 O1 Dy1 115.4(5) . . ? C2 O1 Dy1 123.5(6) . . ? O1 C2 H2A 109.5 . . ? O1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O1 C3 C4 107.3(8) . . ? O1 C3 H3A 110.2 . . ? C4 C3 H3A 110.2 . . ? O1 C3 H3B 110.2 . . ? C4 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? C3 C4 O5 109.8(7) . . ? C3 C4 H4A 109.7 . . ? O5 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? O5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C6 O5 C4 110.8(7) . . ? C6 O5 Dy1 125.1(5) . . ? C4 O5 Dy1 118.4(5) . . ? O5 C6 H6A 109.5 . . ? O5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 O11 Dy1 135.1(4) . . ? O11 C12 C13 127.7(6) . . ? O11 C12 C16 113.7(7) . . ? C13 C12 C16 118.6(6) . . ? C12 C13 C14 120.3(6) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? O15 C14 C13 127.4(6) . . ? O15 C14 C17 114.4(6) . . ? C13 C14 C17 118.1(6) . . ? C14 O15 Dy1 133.8(4) . . ? F13 C16 F11 104.5(8) . . ? F13 C16 F12 105.9(7) . . ? F11 C16 F12 107.1(8) . . ? F13 C16 C12 112.5(7) . . ? F11 C16 C12 112.1(7) . . ? F12 C16 C12 114.0(7) . . ? F15A C17 F16B 71.3(8) . . ? F15A C17 F16A 107.6(8) . . ? F16B C17 F16A 126.2(9) . . ? F15A C17 F15B 127.1(9) . . ? F16B C17 F15B 109.4(10) . . ? F16A C17 F15B 27.8(6) . . ? F15A C17 F14A 103.4(8) . . ? F16B C17 F14A 34.3(6) . . ? F16A C17 F14A 105.1(8) . . ? F15B C17 F14A 80.6(8) . . ? F15A C17 F14B 31.9(6) . . ? F16B C17 F14B 102.4(10) . . ? F16A C17 F14B 83.7(8) . . ? F15B C17 F14B 109.9(10) . . ? F14A C17 F14B 131.3(9) . . ? F15A C17 C14 112.9(7) . . ? F16B C17 C14 113.9(8) . . ? F16A C17 C14 115.2(7) . . ? F15B C17 C14 114.0(7) . . ? F14A C17 C14 111.8(6) . . ? F14B C17 C14 106.6(8) . . ? C22 O21 Dy1 132.1(5) . . ? O21 C22 C23 127.6(7) . . ? O21 C22 C26 114.0(7) . . ? C23 C22 C26 118.3(7) . . ? C22 C23 C24 120.6(7) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? O25 C24 C23 127.9(7) . . ? O25 C24 C27 114.0(8) . . ? C23 C24 C27 118.1(8) . . ? C24 O25 Dy1 132.2(5) . . ? F21 C26 F23 107.2(8) . . ? F21 C26 F22 109.3(8) . . ? F23 C26 F22 104.0(7) . . ? F21 C26 C22 112.1(7) . . ? F23 C26 C22 110.8(7) . . ? F22 C26 C22 112.9(8) . . ? F24 C27 F25 106.9(12) . . ? F24 C27 F26 107.4(11) . . ? F25 C27 F26 103.9(9) . . ? F24 C27 C24 112.0(9) . . ? F25 C27 C24 110.6(10) . . ? F26 C27 C24 115.4(9) . . ? C32 O31 Dy1 134.7(5) . . ? O31 C32 C33 126.7(8) . . ? O31 C32 C36 115.3(7) . . ? C33 C32 C36 118.0(7) . . ? C34 C33 C32 121.2(7) . . ? C34 C33 H33A 119.4 . . ? C32 C33 H33A 119.4 . . ? O35 C34 C33 128.4(7) . . ? O35 C34 C37 113.5(7) . . ? C33 C34 C37 118.0(7) . . ? C34 O35 Dy1 134.2(5) . . ? F33B C36 F31A 47.9(9) . . ? F33B C36 F33A 121.8(13) . . ? F31A C36 F33A 115.0(12) . . ? F33B C36 F31B 114.1(13) . . ? F31A C36 F31B 134.8(12) . . ? F33A C36 F31B 30.2(7) . . ? F33B C36 F32A 52.3(10) . . ? F31A C36 F32A 100.2(9) . . ? F33A C36 F32A 106.3(9) . . ? F31B C36 F32A 79.6(10) . . ? F33B C36 F32B 94.2(14) . . ? F31A C36 F32B 48.1(9) . . ? F33A C36 F32B 81.0(11) . . ? F31B C36 F32B 111.0(12) . . ? F32A C36 F32B 145.0(12) . . ? F33B C36 C32 120.5(11) . . ? F31A C36 C32 114.0(9) . . ? F33A C36 C32 116.6(9) . . ? F31B C36 C32 110.1(10) . . ? F32A C36 C32 101.9(9) . . ? F32B C36 C32 105.0(10) . . ? F35 C37 F36 105.9(9) . . ? F35 C37 F34 107.9(10) . . ? F36 C37 F34 105.5(8) . . ? F35 C37 C34 112.7(8) . . ? F36 C37 C34 115.3(8) . . ? F34 C37 C34 109.0(8) . . ? 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 O11 Dy1 O1 C3 -91.3(6) . . . . ? O31 Dy1 O1 C3 4.2(7) . . . . ? O25 Dy1 O1 C3 127.9(6) . . . . ? O35 Dy1 O1 C3 53.1(6) . . . . ? O21 Dy1 O1 C3 170.9(5) . . . . ? O15 Dy1 O1 C3 -154.7(6) . . . . ? O5 Dy1 O1 C3 -29.7(5) . . . . ? O11 Dy1 O1 C2 122.9(7) . . . . ? O31 Dy1 O1 C2 -141.6(6) . . . . ? O25 Dy1 O1 C2 -17.8(7) . . . . ? O35 Dy1 O1 C2 -92.6(7) . . . . ? O21 Dy1 O1 C2 25.1(8) . . . . ? O15 Dy1 O1 C2 59.5(7) . . . . ? O5 Dy1 O1 C2 -175.4(7) . . . . ? C2 O1 C3 C4 -156.8(8) . . . . ? Dy1 O1 C3 C4 53.8(8) . . . . ? O1 C3 C4 O5 -48.9(9) . . . . ? C3 C4 O5 C6 179.7(7) . . . . ? C3 C4 O5 Dy1 24.9(9) . . . . ? O11 Dy1 O5 C6 -28.3(6) . . . . ? O31 Dy1 O5 C6 54.4(7) . . . . ? O25 Dy1 O5 C6 175.2(6) . . . . ? O35 Dy1 O5 C6 129.2(7) . . . . ? O21 Dy1 O5 C6 8.6(8) . . . . ? O15 Dy1 O5 C6 -91.3(7) . . . . ? O1 Dy1 O5 C6 -149.3(7) . . . . ? O11 Dy1 O5 C4 122.6(5) . . . . ? O31 Dy1 O5 C4 -154.7(6) . . . . ? O25 Dy1 O5 C4 -33.9(6) . . . . ? O35 Dy1 O5 C4 -79.9(5) . . . . ? O21 Dy1 O5 C4 159.5(5) . . . . ? O15 Dy1 O5 C4 59.6(5) . . . . ? O1 Dy1 O5 C4 1.6(5) . . . . ? O31 Dy1 O11 C12 144.6(7) . . . . ? O25 Dy1 O11 C12 19.4(8) . . . . ? O35 Dy1 O11 C12 -177.7(6) . . . . ? O21 Dy1 O11 C12 62.9(7) . . . . ? O15 Dy1 O11 C12 -16.6(6) . . . . ? O1 Dy1 O11 C12 -80.6(7) . . . . ? O5 Dy1 O11 C12 -136.6(7) . . . . ? Dy1 O11 C12 C13 10.5(12) . . . . ? Dy1 O11 C12 C16 -170.3(5) . . . . ? O11 C12 C13 C14 3.6(12) . . . . ? C16 C12 C13 C14 -175.5(7) . . . . ? C12 C13 C14 O15 -0.4(11) . . . . ? C12 C13 C14 C17 179.4(6) . . . . ? C13 C14 O15 Dy1 -16.6(11) . . . . ? C17 C14 O15 Dy1 163.6(4) . . . . ? O11 Dy1 O15 C14 19.4(6) . . . . ? O31 Dy1 O15 C14 -15.4(8) . . . . ? O25 Dy1 O15 C14 -138.0(6) . . . . ? O35 Dy1 O15 C14 -177.4(5) . . . . ? O21 Dy1 O15 C14 -62.5(6) . . . . ? O1 Dy1 O15 C14 137.4(6) . . . . ? O5 Dy1 O15 C14 83.9(6) . . . . ? O11 C12 C16 F13 -57.5(10) . . . . ? C13 C12 C16 F13 121.8(8) . . . . ? O11 C12 C16 F11 59.9(10) . . . . ? C13 C12 C16 F11 -120.8(9) . . . . ? O11 C12 C16 F12 -178.1(8) . . . . ? C13 C12 C16 F12 1.2(12) . . . . ? O15 C14 C17 F15A -63.7(9) . . . . ? C13 C14 C17 F15A 116.5(8) . . . . ? O15 C14 C17 F16B 15.1(11) . . . . ? C13 C14 C17 F16B -164.7(9) . . . . ? O15 C14 C17 F16A 172.2(7) . . . . ? C13 C14 C17 F16A -7.7(10) . . . . ? O15 C14 C17 F15B 141.6(9) . . . . ? C13 C14 C17 F15B -38.3(11) . . . . ? O15 C14 C17 F14A 52.4(8) . . . . ? C13 C14 C17 F14A -127.5(7) . . . . ? O15 C14 C17 F14B -97.0(9) . . . . ? C13 C14 C17 F14B 83.1(10) . . . . ? O11 Dy1 O21 C22 -127.5(6) . . . . ? O31 Dy1 O21 C22 151.2(6) . . . . ? O25 Dy1 O21 C22 25.3(6) . . . . ? O35 Dy1 O21 C22 86.2(6) . . . . ? O15 Dy1 O21 C22 -53.2(6) . . . . ? O1 Dy1 O21 C22 -19.4(7) . . . . ? O5 Dy1 O21 C22 -163.7(5) . . . . ? Dy1 O21 C22 C23 -18.8(11) . . . . ? Dy1 O21 C22 C26 159.5(5) . . . . ? O21 C22 C23 C24 -3.1(12) . . . . ? C26 C22 C23 C24 178.7(7) . . . . ? C22 C23 C24 O25 3.4(13) . . . . ? C22 C23 C24 C27 -176.8(8) . . . . ? C23 C24 O25 Dy1 18.5(12) . . . . ? C27 C24 O25 Dy1 -161.3(6) . . . . ? O11 Dy1 O25 C24 19.8(8) . . . . ? O31 Dy1 O25 C24 -92.3(7) . . . . ? O35 Dy1 O25 C24 -150.2(7) . . . . ? O21 Dy1 O25 C24 -25.1(7) . . . . ? O15 Dy1 O25 C24 55.1(7) . . . . ? O1 Dy1 O25 C24 130.1(7) . . . . ? O5 Dy1 O25 C24 162.5(6) . . . . ? O21 C22 C26 F21 -59.2(10) . . . . ? C23 C22 C26 F21 119.2(9) . . . . ? O21 C22 C26 F23 60.6(9) . . . . ? C23 C22 C26 F23 -121.0(8) . . . . ? O21 C22 C26 F22 176.8(7) . . . . ? C23 C22 C26 F22 -4.8(11) . . . . ? O25 C24 C27 F24 40.7(14) . . . . ? C23 C24 C27 F24 -139.1(12) . . . . ? O25 C24 C27 F25 -78.4(13) . . . . ? C23 C24 C27 F25 101.8(12) . . . . ? O25 C24 C27 F26 164.1(9) . . . . ? C23 C24 C27 F26 -15.7(14) . . . . ? O11 Dy1 O31 C32 142.5(8) . . . . ? O25 Dy1 O31 C32 -74.2(8) . . . . ? O35 Dy1 O31 C32 -16.0(7) . . . . ? O21 Dy1 O31 C32 -137.6(8) . . . . ? O15 Dy1 O31 C32 176.0(6) . . . . ? O1 Dy1 O31 C32 34.5(8) . . . . ? O5 Dy1 O31 C32 65.9(7) . . . . ? Dy1 O31 C32 C33 15.2(13) . . . . ? Dy1 O31 C32 C36 -166.0(6) . . . . ? O31 C32 C33 C34 -2.2(13) . . . . ? C36 C32 C33 C34 179.1(7) . . . . ? C32 C33 C34 O35 -0.9(12) . . . . ? C32 C33 C34 C37 179.7(8) . . . . ? C33 C34 O35 Dy1 -8.7(12) . . . . ? C37 C34 O35 Dy1 170.6(6) . . . . ? O11 Dy1 O35 C34 -26.3(8) . . . . ? O31 Dy1 O35 C34 12.8(6) . . . . ? O25 Dy1 O35 C34 142.6(7) . . . . ? O21 Dy1 O35 C34 81.9(7) . . . . ? O15 Dy1 O35 C34 -177.6(6) . . . . ? O1 Dy1 O35 C34 -133.5(7) . . . . ? O5 Dy1 O35 C34 -66.5(6) . . . . ? O31 C32 C36 F33B -32.6(17) . . . . ? C33 C32 C36 F33B 146.2(14) . . . . ? O31 C32 C36 F31A 21.3(13) . . . . ? C33 C32 C36 F31A -159.9(10) . . . . ? O31 C32 C36 F33A 159.0(10) . . . . ? C33 C32 C36 F33A -22.1(14) . . . . ? O31 C32 C36 F31B -168.8(10) . . . . ? C33 C32 C36 F31B 10.1(13) . . . . ? O31 C32 C36 F32A -85.7(10) . . . . ? C33 C32 C36 F32A 93.2(9) . . . . ? O31 C32 C36 F32B 71.6(11) . . . . ? C33 C32 C36 F32B -109.5(11) . . . . ? O35 C34 C37 F35 -51.3(10) . . . . ? C33 C34 C37 F35 128.1(9) . . . . ? O35 C34 C37 F36 -173.2(8) . . . . ? C33 C34 C37 F36 6.3(13) . . . . ? O35 C34 C37 F34 68.5(11) . . . . ? C33 C34 C37 F34 -112.1(9) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.143 _refine_diff_density_min -0.895 _refine_diff_density_rms 0.118 # Attachment '- ErCif.txt' data_k1183m _database_code_depnum_ccdc_archive 'CCDC 833374' #TrackingRef '- ErCif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H13 Er F18 O8' _chemical_formula_sum 'C19 H13 Er F18 O8' _chemical_formula_weight 878.55 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.668(4) _cell_length_b 15.680(3) _cell_length_c 20.707(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5737(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23693 _cell_measurement_theta_min 2.655 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.034 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3368 _exptl_absorpt_coefficient_mu 3.084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.617 _exptl_absorpt_correction_T_max 0.695 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; -CF3, ANISO, 53/47, SADI C-F -CF3, ANISO, 57/43, SADI C-F -CF3, ANISO, 59/41, SADI C-F ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 31066 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5067 _reflns_number_gt 3668 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V., 1997-2002)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXTL V6.1 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0536P)^2^+11.2410P] 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 5067 _refine_ls_number_parameters 496 _refine_ls_number_restraints 220 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1093 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.063 _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 Er Er 0.132647(15) 0.654832(17) 0.239965(12) 0.04241(13) Uani 1 1 d U . . O1 O 0.2668(3) 0.6758(3) 0.23382(19) 0.0640(12) Uani 1 1 d U . . C2 C 0.3209(4) 0.6219(7) 0.2658(4) 0.094(3) Uani 1 1 d U . . H2A H 0.3291 0.5703 0.2401 0.141 Uiso 1 1 calc R . . H2B H 0.3015 0.6061 0.3086 0.141 Uiso 1 1 calc R . . H2C H 0.3688 0.6526 0.2706 0.141 Uiso 1 1 calc R . . C3 C 0.2948(4) 0.7059(6) 0.1726(4) 0.084(2) Uani 1 1 d U . . H3A H 0.2871 0.6621 0.1387 0.100 Uiso 1 1 calc R . . H3B H 0.3496 0.7188 0.1755 0.100 Uiso 1 1 calc R . . C4 C 0.2525(5) 0.7821(5) 0.1575(4) 0.086(2) Uani 1 1 d U . . H4A H 0.2638 0.8003 0.1128 0.103 Uiso 1 1 calc R . . H4B H 0.2677 0.8286 0.1871 0.103 Uiso 1 1 calc R . . O5 O 0.1706(3) 0.7655(3) 0.1642(2) 0.0716(12) Uani 1 1 d U . . C6 C 0.1263(6) 0.8382(5) 0.1492(4) 0.100(3) Uani 1 1 d U . . H6A H 0.1376 0.8839 0.1800 0.151 Uiso 1 1 calc R . . H6B H 0.0725 0.8234 0.1518 0.151 Uiso 1 1 calc R . . H6C H 0.1383 0.8575 0.1053 0.151 Uiso 1 1 calc R . . O11 O 0.0761(2) 0.7777(3) 0.27579(18) 0.0519(10) Uani 1 1 d U . . C12 C 0.0662(3) 0.8112(4) 0.3300(3) 0.0462(13) Uani 1 1 d U A . C13 C 0.0992(3) 0.7872(4) 0.3880(3) 0.0462(13) Uani 1 1 d U . . H13A H 0.0847 0.8153 0.4267 0.055 Uiso 1 1 calc R . . C14 C 0.1525(3) 0.7234(4) 0.3904(3) 0.0413(12) Uani 1 1 d U B . O15 O 0.1761(2) 0.6783(3) 0.34462(18) 0.0471(9) Uani 1 1 d U . . C16 C 0.0113(4) 0.8867(4) 0.3294(3) 0.0649(17) Uani 1 1 d DU . . C17 C 0.1880(3) 0.7007(4) 0.4559(3) 0.0530(14) Uani 1 1 d DU . . F11A F -0.0564(9) 0.859(2) 0.314(2) 0.148(11) Uani 0.47 1 d PDU A 1 F12A F -0.007(2) 0.909(2) 0.3882(9) 0.155(12) Uani 0.47 1 d PDU A 1 F13A F 0.034(3) 0.952(2) 0.296(2) 0.110(11) Uani 0.47 1 d PDU A 1 F11B F 0.0076(15) 0.9298(16) 0.3836(7) 0.097(5) Uani 0.53 1 d PDU A 2 F12B F 0.034(2) 0.940(2) 0.2853(18) 0.101(7) Uani 0.53 1 d PDU A 2 F13B F -0.0537(9) 0.8686(16) 0.3029(15) 0.112(6) Uani 0.53 1 d PDU A 2 F14A F 0.1730(13) 0.7569(13) 0.5006(9) 0.082(4) Uani 0.57 1 d PDU B 1 F15A F 0.1650(12) 0.6260(8) 0.4744(10) 0.086(4) Uani 0.57 1 d PDU B 1 F16A F 0.2613(5) 0.7003(10) 0.4499(8) 0.083(4) Uani 0.57 1 d PDU B 1 F14B F 0.2520(11) 0.6610(18) 0.4547(12) 0.155(12) Uani 0.43 1 d PDU B 2 F15B F 0.193(2) 0.761(2) 0.4974(16) 0.127(12) Uani 0.43 1 d PDU B 2 F16B F 0.1449(19) 0.6466(16) 0.4864(15) 0.150(12) Uani 0.43 1 d PDU B 2 O21 O 0.0352(2) 0.6029(3) 0.30274(18) 0.0505(10) Uani 1 1 d U . . C22 C 0.0357(3) 0.5498(4) 0.3487(3) 0.0515(14) Uani 1 1 d U . . C23 C 0.0900(4) 0.4904(4) 0.3637(3) 0.0599(16) Uani 1 1 d U . . H23A H 0.0841 0.4561 0.4012 0.072 Uiso 1 1 calc R . . C24 C 0.1528(4) 0.4797(4) 0.3254(3) 0.0543(15) Uani 1 1 d U . . O25 O 0.1710(2) 0.5233(3) 0.27654(19) 0.0534(10) Uani 1 1 d U . . C26 C -0.0349(4) 0.5557(6) 0.3919(3) 0.0708(19) Uani 1 1 d U . . C27 C 0.2080(6) 0.4087(6) 0.3419(4) 0.090(2) Uani 1 1 d U . . F21 F -0.0421(3) 0.6302(4) 0.4170(3) 0.137(2) Uani 1 1 d U . . F22 F -0.0361(2) 0.4960(4) 0.4380(2) 0.1164(19) Uani 1 1 d U . . F23 F -0.0971(2) 0.5404(3) 0.3584(2) 0.0821(12) Uani 1 1 d U . . F24 F 0.2756(4) 0.4294(6) 0.3306(5) 0.235(5) Uani 1 1 d U . . F25 F 0.1933(6) 0.3417(4) 0.3061(3) 0.202(4) Uani 1 1 d U . . F26 F 0.2039(3) 0.3797(3) 0.3997(2) 0.1016(15) Uani 1 1 d U . . O31 O 0.0334(2) 0.6618(3) 0.16945(19) 0.0608(12) Uani 1 1 d U . . C32 C 0.0248(4) 0.6450(5) 0.1100(3) 0.0595(17) Uani 1 1 d U C . C33 C 0.0743(3) 0.6001(4) 0.0710(3) 0.0517(15) Uani 1 1 d U . . H33A H 0.0616 0.5912 0.0269 0.062 Uiso 1 1 calc R . . C34 C 0.1405(4) 0.5684(4) 0.0939(3) 0.0479(14) Uani 1 1 d U . . O35 O 0.1674(2) 0.5761(3) 0.14986(18) 0.0504(10) Uani 1 1 d U . . C36 C -0.0482(5) 0.6767(8) 0.0812(4) 0.113(3) Uani 1 1 d DU . . C37 C 0.1910(5) 0.5169(5) 0.0480(3) 0.0720(19) Uani 1 1 d U . . F31A F -0.0471(11) 0.6812(19) 0.0191(5) 0.177(9) Uani 0.59 1 d PDU C 1 F32A F -0.0993(8) 0.6136(13) 0.0922(9) 0.145(5) Uani 0.59 1 d PDU C 1 F33A F -0.0783(10) 0.7396(10) 0.1105(9) 0.144(5) Uani 0.59 1 d PDU C 1 F31B F -0.1095(14) 0.654(3) 0.1092(16) 0.28(2) Uani 0.41 1 d PDU C 2 F32B F -0.0459(14) 0.7625(10) 0.0820(13) 0.204(12) Uani 0.41 1 d PDU C 2 F33B F -0.0561(15) 0.665(2) 0.0193(6) 0.125(8) Uani 0.41 1 d PDU C 2 F34 F 0.1885(4) 0.4352(3) 0.0650(2) 0.143(2) Uani 1 1 d U . . F35 F 0.2599(3) 0.5412(5) 0.0497(3) 0.148(3) Uani 1 1 d U . . F36 F 0.1699(3) 0.5192(3) -0.01202(18) 0.1031(16) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er 0.0577(2) 0.04008(19) 0.02947(17) -0.00310(11) -0.00034(11) 0.00638(12) O1 0.064(3) 0.089(3) 0.039(2) -0.006(2) 0.0036(19) -0.013(2) C2 0.055(4) 0.164(9) 0.063(5) 0.006(5) -0.001(4) 0.017(5) C3 0.082(5) 0.109(7) 0.060(4) 0.007(4) 0.013(4) -0.034(4) C4 0.122(5) 0.085(6) 0.051(4) -0.002(4) 0.011(4) -0.048(4) O5 0.114(3) 0.055(3) 0.045(3) 0.006(2) 0.016(2) 0.005(3) C6 0.195(9) 0.062(5) 0.044(4) 0.011(4) 0.018(5) 0.032(6) O11 0.074(3) 0.045(2) 0.037(2) -0.0008(18) -0.0018(19) 0.013(2) C12 0.057(3) 0.036(3) 0.046(3) -0.002(3) 0.009(3) 0.009(3) C13 0.057(3) 0.049(4) 0.032(3) -0.006(3) 0.004(3) 0.002(3) C14 0.051(3) 0.040(3) 0.034(3) -0.005(2) 0.002(2) -0.002(2) O15 0.060(2) 0.051(3) 0.031(2) -0.0046(17) 0.0023(17) 0.0126(19) C16 0.082(4) 0.058(4) 0.055(4) -0.004(3) -0.001(3) 0.023(3) C17 0.066(4) 0.059(4) 0.033(3) 0.000(3) 0.003(3) 0.010(3) F11A 0.044(7) 0.14(2) 0.26(3) 0.010(16) 0.005(11) 0.021(7) F12A 0.24(3) 0.16(3) 0.070(9) 0.006(9) 0.049(10) 0.142(19) F13A 0.127(15) 0.053(11) 0.15(3) 0.023(14) 0.046(16) 0.036(8) F11B 0.148(12) 0.068(8) 0.074(7) -0.027(7) -0.024(8) 0.061(7) F12B 0.162(16) 0.057(10) 0.085(8) 0.019(8) 0.006(10) 0.047(8) F13B 0.099(9) 0.085(11) 0.153(14) -0.036(9) -0.049(10) 0.045(6) F14A 0.113(9) 0.096(9) 0.038(5) -0.019(6) -0.021(5) 0.057(7) F15A 0.151(10) 0.067(5) 0.040(7) 0.014(4) -0.029(6) -0.020(5) F16A 0.055(4) 0.143(11) 0.052(6) 0.033(6) -0.013(4) 0.014(5) F14B 0.166(15) 0.25(3) 0.048(9) 0.032(15) 0.011(11) 0.147(18) F15B 0.19(3) 0.100(14) 0.087(14) -0.041(11) -0.069(17) 0.015(13) F16B 0.20(2) 0.20(2) 0.051(13) 0.055(16) -0.019(12) -0.11(2) O21 0.056(2) 0.059(3) 0.037(2) 0.0010(19) -0.0019(17) 0.0034(19) C22 0.061(3) 0.058(4) 0.035(3) -0.002(3) -0.004(3) -0.010(3) C23 0.072(4) 0.060(4) 0.048(4) 0.008(3) -0.005(3) -0.005(3) C24 0.079(4) 0.043(4) 0.041(3) 0.001(3) -0.011(3) 0.006(3) O25 0.074(3) 0.045(2) 0.041(2) -0.0006(18) 0.0029(19) 0.014(2) C26 0.068(4) 0.096(6) 0.048(4) 0.010(4) 0.002(3) -0.007(4) C27 0.123(6) 0.076(6) 0.069(5) 0.024(4) 0.013(5) 0.038(5) F21 0.130(4) 0.138(4) 0.142(5) -0.081(4) 0.088(4) -0.058(4) F22 0.083(3) 0.189(5) 0.078(3) 0.060(3) 0.013(2) -0.006(3) F23 0.062(2) 0.098(3) 0.086(3) 0.014(2) -0.005(2) -0.008(2) F24 0.110(4) 0.236(8) 0.360(12) 0.223(8) 0.085(6) 0.099(4) F25 0.406(11) 0.112(5) 0.089(4) -0.027(4) -0.037(6) 0.146(6) F26 0.134(4) 0.100(4) 0.071(3) 0.030(3) -0.017(3) 0.036(3) O31 0.060(2) 0.090(3) 0.032(2) -0.001(2) -0.0021(18) 0.017(2) C32 0.054(3) 0.090(5) 0.034(3) 0.011(3) -0.004(3) -0.002(3) C33 0.067(4) 0.057(4) 0.031(3) 0.002(3) -0.005(3) -0.008(3) C34 0.074(4) 0.036(3) 0.034(3) -0.004(2) 0.005(3) -0.003(3) O35 0.066(3) 0.051(2) 0.034(2) -0.0088(18) -0.0027(18) 0.008(2) C36 0.062(5) 0.223(10) 0.054(4) 0.003(6) -0.005(4) 0.033(5) C37 0.107(5) 0.071(5) 0.038(3) -0.009(3) -0.007(4) 0.031(4) F31A 0.121(13) 0.35(3) 0.057(6) 0.048(9) -0.002(7) 0.127(14) F32A 0.049(7) 0.278(11) 0.108(10) -0.053(9) -0.008(6) 0.004(8) F33A 0.104(11) 0.229(11) 0.099(11) -0.008(9) -0.025(8) 0.085(8) F31B 0.062(8) 0.67(6) 0.12(2) 0.12(4) 0.040(14) 0.07(3) F32B 0.22(3) 0.233(12) 0.16(2) -0.076(16) -0.116(18) 0.193(16) F33B 0.077(12) 0.24(2) 0.054(7) -0.005(11) -0.035(7) -0.028(13) F34 0.277(7) 0.078(3) 0.073(3) 0.009(3) 0.046(4) 0.079(4) F35 0.085(3) 0.257(7) 0.101(4) -0.092(5) 0.015(3) 0.024(4) F36 0.162(4) 0.114(4) 0.032(2) -0.018(2) 0.000(2) 0.041(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 Er O31 2.284(4) . ? Er O11 2.294(4) . ? Er O25 2.299(4) . ? Er O21 2.306(4) . ? Er O35 2.320(4) . ? Er O15 2.328(4) . ? Er O1 2.396(5) . ? Er O5 2.433(5) . ? O1 C2 1.437(9) . ? O1 C3 1.441(8) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.443(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O5 1.478(10) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O5 C6 1.416(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O11 C12 1.251(7) . ? C12 C13 1.386(8) . ? C12 C16 1.531(9) . ? C13 C14 1.376(8) . ? C13 H13A 0.9500 . ? C14 O15 1.253(6) . ? C14 C17 1.536(8) . ? C16 F13A 1.302(14) . ? C16 F13B 1.305(12) . ? C16 F12B 1.308(13) . ? C16 F12A 1.308(13) . ? C16 F11B 1.311(12) . ? C16 F11A 1.314(13) . ? C17 F15B 1.286(13) . ? C17 F14B 1.292(13) . ? C17 F15A 1.297(11) . ? C17 F16A 1.302(10) . ? C17 F16B 1.302(13) . ? C17 F14A 1.305(10) . ? O21 C22 1.264(7) . ? C22 C23 1.373(9) . ? C22 C26 1.537(9) . ? C23 C24 1.374(9) . ? C23 H23A 0.9500 . ? C24 O25 1.263(7) . ? C24 C27 1.519(10) . ? C26 F21 1.286(9) . ? C26 F23 1.320(8) . ? C26 F22 1.337(8) . ? C27 F24 1.260(11) . ? C27 F26 1.282(9) . ? C27 F25 1.311(11) . ? O31 C32 1.267(7) . ? C32 C33 1.383(9) . ? C32 C36 1.506(11) . ? C33 C34 1.358(8) . ? C33 H33A 0.9500 . ? C34 O35 1.257(7) . ? C34 C37 1.533(9) . ? C36 F33A 1.274(12) . ? C36 F31B 1.280(14) . ? C36 F31A 1.289(12) . ? C36 F33B 1.304(13) . ? C36 F32B 1.346(14) . ? C36 F32A 1.359(12) . ? C37 F35 1.277(9) . ? C37 F36 1.298(7) . ? C37 F34 1.328(9) . ? 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 O31 Er O11 80.36(15) . . ? O31 Er O25 118.65(16) . . ? O11 Er O25 140.85(14) . . ? O31 Er O21 78.70(15) . . ? O11 Er O21 77.85(15) . . ? O25 Er O21 73.59(15) . . ? O31 Er O35 73.39(14) . . ? O11 Er O35 145.31(13) . . ? O25 Er O35 73.13(14) . . ? O21 Er O35 117.58(14) . . ? O31 Er O15 147.18(14) . . ? O11 Er O15 73.13(13) . . ? O25 Er O15 74.81(14) . . ? O21 Er O15 77.12(14) . . ? O35 Er O15 138.21(13) . . ? O31 Er O1 135.95(15) . . ? O11 Er O1 109.43(16) . . ? O25 Er O1 81.31(17) . . ? O21 Er O1 144.77(14) . . ? O35 Er O1 76.62(14) . . ? O15 Er O1 72.65(13) . . ? O31 Er O5 76.43(17) . . ? O11 Er O5 74.27(15) . . ? O25 Er O5 140.44(16) . . ? O21 Er O5 145.17(16) . . ? O35 Er O5 77.77(15) . . ? O15 Er O5 113.37(16) . . ? O1 Er O5 66.16(17) . . ? C2 O1 C3 111.7(6) . . ? C2 O1 Er 123.6(5) . . ? C3 O1 Er 115.6(4) . . ? O1 C2 H2A 109.5 . . ? O1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O1 C3 C4 106.4(7) . . ? O1 C3 H3A 110.4 . . ? C4 C3 H3A 110.4 . . ? O1 C3 H3B 110.4 . . ? C4 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? C3 C4 O5 110.0(6) . . ? C3 C4 H4A 109.7 . . ? O5 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? O5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C6 O5 C4 112.2(6) . . ? C6 O5 Er 124.3(5) . . ? C4 O5 Er 117.1(4) . . ? O5 C6 H6A 109.5 . . ? O5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 O11 Er 134.7(4) . . ? O11 C12 C13 127.2(5) . . ? O11 C12 C16 113.9(5) . . ? C13 C12 C16 118.9(5) . . ? C14 C13 C12 121.1(5) . . ? C14 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? O15 C14 C13 127.7(5) . . ? O15 C14 C17 113.7(5) . . ? C13 C14 C17 118.7(5) . . ? C14 O15 Er 133.1(4) . . ? F13A C16 F13B 103(3) . . ? F13A C16 F12B 13(5) . . ? F13B C16 F12B 97(3) . . ? F13A C16 F12A 111(3) . . ? F13B C16 F12A 104(2) . . ? F12B C16 F12A 123(3) . . ? F13A C16 F11B 93(3) . . ? F13B C16 F11B 115.3(18) . . ? F12B C16 F11B 106(2) . . ? F12A C16 F11B 18(3) . . ? F13A C16 F11A 115(3) . . ? F13B C16 F11A 13(3) . . ? F12B C16 F11A 109(3) . . ? F12A C16 F11A 95(3) . . ? F11B C16 F11A 109(2) . . ? F13A C16 C12 115(2) . . ? F13B C16 C12 113.1(12) . . ? F12B C16 C12 107.9(19) . . ? F12A C16 C12 111.1(16) . . ? F11B C16 C12 115.1(13) . . ? F11A C16 C12 108.6(16) . . ? F15B C17 F14B 108(2) . . ? F15B C17 F15A 120(2) . . ? F14B C17 F15A 81.1(16) . . ? F15B C17 F16A 90(2) . . ? F14B C17 F16A 28.8(17) . . ? F15A C17 F16A 109.6(12) . . ? F15B C17 F16B 102(2) . . ? F14B C17 F16B 102(2) . . ? F15A C17 F16B 24(2) . . ? F16A C17 F16B 129(2) . . ? F15B C17 F14A 16(3) . . ? F14B C17 F14A 121.0(19) . . ? F15A C17 F14A 109.6(15) . . ? F16A C17 F14A 105.8(13) . . ? F16B C17 F14A 89(2) . . ? F15B C17 C14 116.6(18) . . ? F14B C17 C14 116.9(12) . . ? F15A C17 C14 110.1(11) . . ? F16A C17 C14 108.8(8) . . ? F16B C17 C14 109.9(17) . . ? F14A C17 C14 112.8(11) . . ? C22 O21 Er 130.7(4) . . ? O21 C22 C23 128.5(6) . . ? O21 C22 C26 113.1(6) . . ? C23 C22 C26 118.4(6) . . ? C22 C23 C24 121.1(6) . . ? C22 C23 H23A 119.5 . . ? C24 C23 H23A 119.5 . . ? O25 C24 C23 127.0(6) . . ? O25 C24 C27 114.5(6) . . ? C23 C24 C27 118.5(6) . . ? C24 O25 Er 132.4(4) . . ? F21 C26 F23 107.2(7) . . ? F21 C26 F22 110.2(7) . . ? F23 C26 F22 103.5(6) . . ? F21 C26 C22 111.7(6) . . ? F23 C26 C22 111.1(6) . . ? F22 C26 C22 112.7(6) . . ? F24 C27 F26 108.6(9) . . ? F24 C27 F25 106.8(9) . . ? F26 C27 F25 103.4(8) . . ? F24 C27 C24 112.1(7) . . ? F26 C27 C24 115.7(7) . . ? F25 C27 C24 109.5(8) . . ? C32 O31 Er 134.6(4) . . ? O31 C32 C33 126.7(6) . . ? O31 C32 C36 114.7(6) . . ? C33 C32 C36 118.5(6) . . ? C34 C33 C32 121.7(5) . . ? C34 C33 H33A 119.1 . . ? C32 C33 H33A 119.1 . . ? O35 C34 C33 127.8(6) . . ? O35 C34 C37 113.8(6) . . ? C33 C34 C37 118.4(5) . . ? C34 O35 Er 133.8(4) . . ? F33A C36 F31B 70(2) . . ? F33A C36 F31A 116.1(16) . . ? F31B C36 F31A 119(2) . . ? F33A C36 F33B 122(2) . . ? F31B C36 F33B 108(2) . . ? F31A C36 F33B 13(3) . . ? F33A C36 F32B 40.0(14) . . ? F31B C36 F32B 108(3) . . ? F31A C36 F32B 87.5(18) . . ? F33B C36 F32B 99(2) . . ? F33A C36 F32A 101.9(13) . . ? F31B C36 F32A 32(3) . . ? F31A C36 F32A 102.5(16) . . ? F33B C36 F32A 89.4(16) . . ? F32B C36 F32A 138.3(16) . . ? F33A C36 C32 115.1(11) . . ? F31B C36 C32 117(2) . . ? F31A C36 C32 113.6(10) . . ? F33B C36 C32 115.8(16) . . ? F32B C36 C32 107.4(12) . . ? F32A C36 C32 105.2(11) . . ? F35 C37 F36 106.9(7) . . ? F35 C37 F34 108.2(7) . . ? F36 C37 F34 105.8(6) . . ? F35 C37 C34 112.3(6) . . ? F36 C37 C34 114.4(6) . . ? F34 C37 C34 108.9(6) . . ? 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 O31 Er O1 C2 -138.8(5) . . . . ? O11 Er O1 C2 124.9(5) . . . . ? O25 Er O1 C2 -16.1(5) . . . . ? O21 Er O1 C2 28.5(6) . . . . ? O35 Er O1 C2 -90.7(5) . . . . ? O15 Er O1 C2 60.6(5) . . . . ? O5 Er O1 C2 -173.1(6) . . . . ? O31 Er O1 C3 5.2(6) . . . . ? O11 Er O1 C3 -91.1(5) . . . . ? O25 Er O1 C3 127.9(5) . . . . ? O21 Er O1 C3 172.5(5) . . . . ? O35 Er O1 C3 53.3(5) . . . . ? O15 Er O1 C3 -155.4(5) . . . . ? O5 Er O1 C3 -29.1(5) . . . . ? C2 O1 C3 C4 -157.9(7) . . . . ? Er O1 C3 C4 53.9(7) . . . . ? O1 C3 C4 O5 -50.5(8) . . . . ? C3 C4 O5 C6 -179.3(6) . . . . ? C3 C4 O5 Er 27.4(7) . . . . ? O31 Er O5 C6 54.2(6) . . . . ? O11 Er O5 C6 -29.5(6) . . . . ? O25 Er O5 C6 173.0(5) . . . . ? O21 Er O5 C6 8.6(7) . . . . ? O35 Er O5 C6 129.8(6) . . . . ? O15 Er O5 C6 -92.7(6) . . . . ? O1 Er O5 C6 -149.6(6) . . . . ? O31 Er O5 C4 -156.0(5) . . . . ? O11 Er O5 C4 120.4(5) . . . . ? O25 Er O5 C4 -37.2(6) . . . . ? O21 Er O5 C4 158.4(4) . . . . ? O35 Er O5 C4 -80.4(4) . . . . ? O15 Er O5 C4 57.1(5) . . . . ? O1 Er O5 C4 0.2(4) . . . . ? O31 Er O11 C12 143.5(6) . . . . ? O25 Er O11 C12 19.4(7) . . . . ? O21 Er O11 C12 63.1(6) . . . . ? O35 Er O11 C12 -175.5(5) . . . . ? O15 Er O11 C12 -16.9(6) . . . . ? O1 Er O11 C12 -81.0(6) . . . . ? O5 Er O11 C12 -138.0(6) . . . . ? Er O11 C12 C13 11.2(10) . . . . ? Er O11 C12 C16 -169.0(4) . . . . ? O11 C12 C13 C14 4.0(10) . . . . ? C16 C12 C13 C14 -175.8(6) . . . . ? C12 C13 C14 O15 -2.5(10) . . . . ? C12 C13 C14 C17 179.0(5) . . . . ? C13 C14 O15 Er -13.7(9) . . . . ? C17 C14 O15 Er 164.9(4) . . . . ? O31 Er O15 C14 -19.6(7) . . . . ? O11 Er O15 C14 18.0(5) . . . . ? O25 Er O15 C14 -139.3(5) . . . . ? O21 Er O15 C14 -63.1(5) . . . . ? O35 Er O15 C14 179.8(5) . . . . ? O1 Er O15 C14 135.3(5) . . . . ? O5 Er O15 C14 81.9(5) . . . . ? O11 C12 C16 F13A -64(3) . . . . ? C13 C12 C16 F13A 115(3) . . . . ? O11 C12 C16 F13B 53.1(18) . . . . ? C13 C12 C16 F13B -127.1(18) . . . . ? O11 C12 C16 F12B -53(2) . . . . ? C13 C12 C16 F12B 127(2) . . . . ? O11 C12 C16 F12A 169(2) . . . . ? C13 C12 C16 F12A -11(2) . . . . ? O11 C12 C16 F11B -171.4(15) . . . . ? C13 C12 C16 F11B 8.4(16) . . . . ? O11 C12 C16 F11A 66(2) . . . . ? C13 C12 C16 F11A -115(2) . . . . ? O15 C14 C17 F15B 151(2) . . . . ? C13 C14 C17 F15B -30(2) . . . . ? O15 C14 C17 F14B 21.8(18) . . . . ? C13 C14 C17 F14B -159.5(17) . . . . ? O15 C14 C17 F15A -68.2(11) . . . . ? C13 C14 C17 F15A 110.5(11) . . . . ? O15 C14 C17 F16A 51.9(10) . . . . ? C13 C14 C17 F16A -129.3(10) . . . . ? O15 C14 C17 F16B -93.8(17) . . . . ? C13 C14 C17 F16B 84.9(17) . . . . ? O15 C14 C17 F14A 169.0(14) . . . . ? C13 C14 C17 F14A -12.3(15) . . . . ? O31 Er O21 C22 150.3(5) . . . . ? O11 Er O21 C22 -127.3(5) . . . . ? O25 Er O21 C22 25.6(5) . . . . ? O35 Er O21 C22 85.9(5) . . . . ? O15 Er O21 C22 -52.1(5) . . . . ? O1 Er O21 C22 -20.7(6) . . . . ? O5 Er O21 C22 -164.7(5) . . . . ? Er O21 C22 C23 -19.6(9) . . . . ? Er O21 C22 C26 160.3(4) . . . . ? O21 C22 C23 C24 -2.9(11) . . . . ? C26 C22 C23 C24 177.3(6) . . . . ? C22 C23 C24 O25 4.4(11) . . . . ? C22 C23 C24 C27 -175.7(7) . . . . ? C23 C24 O25 Er 17.2(10) . . . . ? C27 C24 O25 Er -162.7(5) . . . . ? O31 Er O25 C24 -91.8(6) . . . . ? O11 Er O25 C24 19.9(7) . . . . ? O21 Er O25 C24 -24.9(5) . . . . ? O35 Er O25 C24 -151.4(6) . . . . ? O15 Er O25 C24 55.8(5) . . . . ? O1 Er O25 C24 130.1(6) . . . . ? O5 Er O25 C24 164.3(5) . . . . ? O21 C22 C26 F21 -59.1(8) . . . . ? C23 C22 C26 F21 120.8(7) . . . . ? O21 C22 C26 F23 60.5(8) . . . . ? C23 C22 C26 F23 -119.6(7) . . . . ? O21 C22 C26 F22 176.1(6) . . . . ? C23 C22 C26 F22 -4.0(9) . . . . ? O25 C24 C27 F24 35.6(12) . . . . ? C23 C24 C27 F24 -144.4(9) . . . . ? O25 C24 C27 F26 160.9(8) . . . . ? C23 C24 C27 F26 -19.1(12) . . . . ? O25 C24 C27 F25 -82.8(9) . . . . ? C23 C24 C27 F25 97.2(9) . . . . ? O11 Er O31 C32 142.1(6) . . . . ? O25 Er O31 C32 -74.4(6) . . . . ? O21 Er O31 C32 -138.5(6) . . . . ? O35 Er O31 C32 -14.9(6) . . . . ? O15 Er O31 C32 178.4(5) . . . . ? O1 Er O31 C32 34.1(7) . . . . ? O5 Er O31 C32 66.1(6) . . . . ? Er O31 C32 C33 13.3(11) . . . . ? Er O31 C32 C36 -168.1(6) . . . . ? O31 C32 C33 C34 -0.3(11) . . . . ? C36 C32 C33 C34 -178.9(7) . . . . ? C32 C33 C34 O35 -2.3(11) . . . . ? C32 C33 C34 C37 178.0(6) . . . . ? C33 C34 O35 Er -7.7(10) . . . . ? C37 C34 O35 Er 172.0(5) . . . . ? O31 Er O35 C34 12.2(5) . . . . ? O11 Er O35 C34 -30.2(7) . . . . ? O25 Er O35 C34 140.0(6) . . . . ? O21 Er O35 C34 79.5(6) . . . . ? O15 Er O35 C34 -178.6(5) . . . . ? O1 Er O35 C34 -135.1(6) . . . . ? O5 Er O35 C34 -67.1(5) . . . . ? O31 C32 C36 F33A 24.1(15) . . . . ? C33 C32 C36 F33A -157.2(12) . . . . ? O31 C32 C36 F31B -55(3) . . . . ? C33 C32 C36 F31B 124(3) . . . . ? O31 C32 C36 F31A 161.4(17) . . . . ? C33 C32 C36 F31A -19.9(19) . . . . ? O31 C32 C36 F33B 175.8(18) . . . . ? C33 C32 C36 F33B -5(2) . . . . ? O31 C32 C36 F32B 66.4(15) . . . . ? C33 C32 C36 F32B -114.9(14) . . . . ? O31 C32 C36 F32A -87.3(10) . . . . ? C33 C32 C36 F32A 91.4(10) . . . . ? O35 C34 C37 F35 -48.0(9) . . . . ? C33 C34 C37 F35 131.7(7) . . . . ? O35 C34 C37 F36 -170.1(7) . . . . ? C33 C34 C37 F36 9.6(10) . . . . ? O35 C34 C37 F34 71.8(8) . . . . ? C33 C34 C37 F34 -108.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.606 _refine_diff_density_min -1.707 _refine_diff_density_rms 0.108 # Attachment '- EuCif.txt' data_eu _database_code_depnum_ccdc_archive 'CCDC 833375' #TrackingRef '- EuCif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H13 Eu F18 O8' _chemical_formula_sum 'C19 H13 Eu F18 O8' _chemical_formula_weight 863.25 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.455(4) _cell_length_b 15.928(3) _cell_length_c 20.994(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5837(2) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 14532 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.965 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3328 _exptl_absorpt_coefficient_mu 2.305 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.610 _exptl_absorpt_correction_T_max 0.849 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; -CF3, ANISO, 70/30, SADI C-F -CF3, ANISO, 64/36, SADI C-F -CF3, ANISO, 52/48, SADI C-F ; _diffrn_ambient_temperature 200(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 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 34891 _diffrn_reflns_av_R_equivalents 0.1109 _diffrn_reflns_av_sigmaI/netI 0.1034 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6679 _reflns_number_gt 2892 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V., 1997-2002)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXTL V6.1 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.1178P)^2^] 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 0.00059(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6679 _refine_ls_number_parameters 497 _refine_ls_number_restraints 235 _refine_ls_R_factor_all 0.1733 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.2196 _refine_ls_wR_factor_gt 0.1600 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.969 _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 Eu Eu 0.13423(3) 0.65352(3) 0.24030(2) 0.0570(2) Uani 1 1 d U . . O1 O 0.2744(4) 0.6717(5) 0.2344(3) 0.0820(18) Uani 1 1 d U . . C2 C 0.3287(8) 0.6216(12) 0.2690(6) 0.147(6) Uani 1 1 d U . . H2A H 0.3535 0.5820 0.2398 0.220 Uiso 1 1 calc R . . H2B H 0.3021 0.5903 0.3026 0.220 Uiso 1 1 calc R . . H2C H 0.3674 0.6582 0.2882 0.220 Uiso 1 1 calc R . . C3 C 0.2998(7) 0.7060(9) 0.1747(7) 0.117(4) Uani 1 1 d U . . H3A H 0.3551 0.7189 0.1777 0.141 Uiso 1 1 calc R . . H3B H 0.2930 0.6631 0.1410 0.141 Uiso 1 1 calc R . . C4 C 0.2612(7) 0.7778(8) 0.1571(6) 0.113(4) Uani 1 1 d U . . H4A H 0.2713 0.7903 0.1116 0.135 Uiso 1 1 calc R . . H4B H 0.2794 0.8259 0.1828 0.135 Uiso 1 1 calc R . . O5 O 0.1795(4) 0.7657(4) 0.1670(3) 0.0876(19) Uani 1 1 d U . . C6 C 0.1393(7) 0.8394(7) 0.1518(6) 0.100(4) Uani 1 1 d U . . H6A H 0.1525 0.8835 0.1824 0.150 Uiso 1 1 calc R . . H6B H 0.0841 0.8284 0.1537 0.150 Uiso 1 1 calc R . . H6C H 0.1532 0.8576 0.1088 0.150 Uiso 1 1 calc R . . O11 O 0.0756(3) 0.7781(4) 0.2768(3) 0.0670(16) Uani 1 1 d U . . C12 C 0.0649(5) 0.8117(6) 0.3306(5) 0.061(2) Uani 1 1 d U A . C13 C 0.0973(5) 0.7873(6) 0.3876(4) 0.061(2) Uani 1 1 d U . . H13A H 0.0823 0.8152 0.4256 0.073 Uiso 1 1 calc R . . C14 C 0.1510(4) 0.7235(5) 0.3914(4) 0.0533(19) Uani 1 1 d U B . O15 O 0.1765(3) 0.6787(4) 0.3464(3) 0.0633(15) Uani 1 1 d U . . C16 C 0.0127(6) 0.8855(7) 0.3302(5) 0.083(3) Uani 1 1 d DU . . C17 C 0.1831(5) 0.6995(6) 0.4563(5) 0.075(2) Uani 1 1 d DU . . F11A F -0.0589(7) 0.8686(12) 0.3153(11) 0.135(6) Uani 0.70 1 d PDU A 1 F12A F 0.0097(10) 0.9261(10) 0.3849(6) 0.133(6) Uani 0.70 1 d PDU A 1 F13A F 0.0323(9) 0.9420(9) 0.2882(9) 0.109(4) Uani 0.70 1 d PDU A 1 F11B F 0.049(3) 0.954(3) 0.313(3) 0.23(3) Uani 0.30 1 d PDU A 2 F12B F -0.0406(16) 0.866(4) 0.288(2) 0.16(2) Uani 0.30 1 d PDU A 2 F13B F -0.034(3) 0.888(4) 0.3800(17) 0.21(2) Uani 0.30 1 d PDU A 2 F14A F 0.1652(17) 0.7517(18) 0.5020(14) 0.140(9) Uani 0.64 1 d PDU B 1 F15A F 0.1587(14) 0.6275(11) 0.4778(11) 0.133(8) Uani 0.64 1 d PDU B 1 F16A F 0.2579(6) 0.6973(13) 0.4543(8) 0.123(6) Uani 0.64 1 d PDU B 1 F14B F 0.234(2) 0.641(2) 0.4582(11) 0.147(15) Uani 0.36 1 d PDU B 2 F15B F 0.202(3) 0.764(3) 0.491(3) 0.133(15) Uani 0.36 1 d PDU B 2 F16B F 0.1258(14) 0.668(3) 0.489(2) 0.148(17) Uani 0.36 1 d PDU B 2 O21 O 0.0340(3) 0.5970(4) 0.3032(3) 0.0679(15) Uani 1 1 d DU . . C22 C 0.0351(5) 0.5455(6) 0.3490(4) 0.070(2) Uani 1 1 d DU . . C23 C 0.0907(5) 0.4891(6) 0.3642(5) 0.079(3) Uani 1 1 d DU . . H23A H 0.0851 0.4560 0.4016 0.094 Uiso 1 1 calc R . . C24 C 0.1557(6) 0.4786(6) 0.3263(5) 0.075(2) Uani 1 1 d DU . . O25 O 0.1738(4) 0.5218(4) 0.2781(3) 0.0738(16) Uani 1 1 d DU . . C26 C -0.0364(6) 0.5493(9) 0.3916(5) 0.092(3) Uani 1 1 d DU . . C27 C 0.2121(9) 0.4103(9) 0.3444(7) 0.117(4) Uani 1 1 d DU . . F21 F -0.0436(5) 0.6238(5) 0.4172(4) 0.148(3) Uani 1 1 d U . . F22 F -0.0365(4) 0.4918(6) 0.4362(4) 0.146(3) Uani 1 1 d U . . F23 F -0.0994(4) 0.5356(5) 0.3582(3) 0.110(2) Uani 1 1 d U . . F24 F 0.2811(6) 0.4436(8) 0.3463(8) 0.268(7) Uani 1 1 d U . . F25 F 0.2174(11) 0.3545(8) 0.3060(5) 0.306(9) Uani 1 1 d U . . F26 F 0.2056(5) 0.3765(6) 0.3980(4) 0.145(3) Uani 1 1 d U . . O31 O 0.0337(4) 0.6664(4) 0.1664(3) 0.0752(17) Uani 1 1 d DU . . C32 C 0.0253(5) 0.6507(6) 0.1079(4) 0.072(2) Uani 1 1 d DU C . C33 C 0.0730(5) 0.6021(6) 0.0702(4) 0.076(3) Uani 1 1 d DU . . H33A H 0.0598 0.5936 0.0268 0.091 Uiso 1 1 calc R . . C34 C 0.1380(5) 0.5661(5) 0.0931(4) 0.064(2) Uani 1 1 d DU . . O35 O 0.1658(3) 0.5732(4) 0.1489(3) 0.0687(16) Uani 1 1 d DU . . C36 C -0.0466(6) 0.6858(9) 0.0784(5) 0.129(4) Uani 1 1 d DU . . C37 C 0.1873(8) 0.5147(8) 0.0480(5) 0.095(3) Uani 1 1 d DU . . F31A F -0.0428(15) 0.692(2) 0.0159(7) 0.122(8) Uani 0.52 1 d PDU C 1 F32A F -0.1027(8) 0.6312(14) 0.0922(8) 0.163(8) Uani 0.52 1 d PDU C 1 F33A F -0.0650(14) 0.7586(14) 0.1024(14) 0.186(13) Uani 0.52 1 d PDU C 1 F31B F -0.1051(18) 0.709(3) 0.1136(18) 0.25(2) Uani 0.48 1 d PDU C 2 F32B F -0.0316(15) 0.7687(11) 0.0682(14) 0.167(10) Uani 0.48 1 d PDU C 2 F33B F -0.061(2) 0.662(3) 0.0198(8) 0.186(15) Uani 0.48 1 d PDU C 2 F34 F 0.1906(7) 0.4374(5) 0.0681(4) 0.190(4) Uani 1 1 d U . . F35 F 0.2574(5) 0.5397(7) 0.0458(4) 0.185(4) Uani 1 1 d U . . F36 F 0.1634(5) 0.5115(5) -0.0096(3) 0.148(3) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu 0.0730(4) 0.0543(4) 0.0437(3) -0.0043(2) -0.0023(2) 0.0075(2) O1 0.074(4) 0.114(6) 0.058(4) -0.016(3) 0.008(3) -0.008(3) C2 0.084(7) 0.26(2) 0.093(10) 0.016(10) 0.010(7) 0.062(10) C3 0.111(7) 0.125(11) 0.116(9) 0.021(8) 0.044(8) -0.010(7) C4 0.123(7) 0.124(10) 0.090(9) 0.008(7) 0.020(7) -0.026(6) O5 0.119(5) 0.070(4) 0.073(4) 0.006(3) 0.027(4) 0.003(4) C6 0.169(10) 0.070(7) 0.062(8) 0.014(5) 0.030(7) 0.015(7) O11 0.084(4) 0.064(4) 0.053(3) 0.000(3) 0.005(3) 0.017(3) C12 0.079(5) 0.047(5) 0.056(5) -0.001(4) 0.007(4) 0.013(4) C13 0.076(5) 0.059(6) 0.048(5) -0.007(4) 0.009(4) 0.001(4) C14 0.060(5) 0.061(6) 0.039(4) 0.000(3) -0.001(3) -0.006(4) O15 0.078(4) 0.066(4) 0.045(3) -0.012(3) -0.001(3) 0.016(3) C16 0.098(6) 0.073(7) 0.078(7) -0.007(5) 0.002(5) 0.032(5) C17 0.091(6) 0.087(7) 0.046(5) 0.005(4) 0.005(5) 0.014(5) F11A 0.074(6) 0.104(10) 0.23(2) -0.045(11) 0.007(9) 0.038(6) F12A 0.194(16) 0.104(9) 0.101(7) -0.039(6) -0.018(7) 0.097(9) F13A 0.127(9) 0.078(7) 0.123(9) 0.020(6) 0.009(8) 0.045(6) F11B 0.27(5) 0.072(15) 0.34(8) 0.10(3) -0.06(4) 0.004(17) F12B 0.10(2) 0.22(4) 0.16(3) -0.11(3) -0.04(2) 0.11(2) F13B 0.19(5) 0.32(6) 0.11(2) 0.00(3) 0.05(2) 0.17(4) F14A 0.21(3) 0.152(17) 0.056(8) -0.022(12) -0.019(14) 0.081(15) F15A 0.197(18) 0.121(12) 0.083(12) 0.042(10) -0.041(14) -0.047(14) F16A 0.088(5) 0.195(17) 0.085(9) 0.047(12) -0.014(6) 0.025(8) F14B 0.24(3) 0.17(3) 0.035(11) 0.028(17) -0.004(18) 0.12(3) F15B 0.19(4) 0.119(17) 0.09(3) -0.012(15) -0.08(3) 0.00(2) F16B 0.136(18) 0.22(4) 0.09(2) 0.10(3) -0.018(15) -0.04(2) O21 0.076(3) 0.071(4) 0.057(4) 0.003(3) -0.001(3) 0.007(3) C22 0.080(5) 0.083(7) 0.046(5) 0.008(4) -0.009(4) -0.001(4) C23 0.090(6) 0.069(7) 0.077(7) 0.013(5) -0.013(5) -0.005(5) C24 0.106(6) 0.051(5) 0.069(7) -0.001(4) -0.015(5) 0.010(5) O25 0.103(4) 0.059(4) 0.059(4) -0.004(3) -0.004(3) 0.020(3) C26 0.100(6) 0.110(8) 0.067(8) 0.008(6) 0.011(5) -0.017(6) C27 0.158(8) 0.107(10) 0.086(8) 0.021(6) 0.006(9) 0.068(7) F21 0.148(6) 0.146(6) 0.149(7) -0.060(5) 0.083(5) -0.051(5) F22 0.124(5) 0.197(7) 0.116(6) 0.076(6) 0.021(4) -0.013(5) F23 0.090(4) 0.124(5) 0.118(5) 0.018(4) 0.004(4) -0.015(4) F24 0.129(6) 0.240(11) 0.44(2) 0.201(10) 0.032(9) 0.079(7) F25 0.60(2) 0.195(10) 0.127(8) -0.061(8) -0.109(12) 0.275(12) F26 0.165(6) 0.156(7) 0.113(6) 0.050(5) -0.018(5) 0.060(5) O31 0.082(4) 0.094(5) 0.050(4) -0.003(3) -0.006(3) 0.009(3) C32 0.068(5) 0.095(7) 0.053(5) 0.020(5) -0.007(4) -0.017(4) C33 0.091(6) 0.085(8) 0.051(6) 0.006(5) -0.008(4) -0.006(5) C34 0.094(5) 0.050(5) 0.048(5) -0.004(4) 0.003(4) -0.014(4) O35 0.095(4) 0.067(4) 0.045(3) -0.014(3) -0.003(3) 0.011(3) C36 0.098(8) 0.212(12) 0.076(7) 0.020(9) -0.013(6) 0.033(8) C37 0.143(8) 0.089(8) 0.052(6) -0.008(6) -0.009(6) 0.033(6) F31A 0.102(14) 0.19(2) 0.073(7) 0.021(9) -0.007(7) 0.047(15) F32A 0.051(7) 0.36(2) 0.073(10) -0.010(13) 0.006(7) -0.008(11) F33A 0.13(2) 0.298(19) 0.13(3) -0.07(2) -0.056(18) 0.125(15) F31B 0.12(2) 0.49(6) 0.15(2) 0.10(3) 0.040(19) 0.13(3) F32B 0.16(2) 0.181(12) 0.16(3) 0.016(14) -0.020(15) 0.108(12) F33B 0.16(2) 0.30(3) 0.099(12) 0.023(16) -0.077(14) -0.04(2) F34 0.378(13) 0.095(5) 0.098(6) 0.014(4) 0.075(7) 0.101(6) F35 0.134(6) 0.275(10) 0.146(8) -0.114(8) 0.040(5) 0.002(6) F36 0.235(7) 0.156(7) 0.052(4) -0.035(4) -0.021(5) 0.070(6) _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 Eu O25 2.347(6) . ? Eu O31 2.352(6) . ? Eu O11 2.360(6) . ? Eu O21 2.368(6) . ? Eu O35 2.370(6) . ? Eu O15 2.381(6) . ? Eu O1 2.466(7) . ? Eu O5 2.487(7) . ? O1 C2 1.436(14) . ? O1 C3 1.439(13) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.377(16) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O5 1.454(13) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O5 C6 1.404(11) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O11 C12 1.264(10) . ? C12 C13 1.379(12) . ? C12 C16 1.487(13) . ? C13 C14 1.385(11) . ? C13 H13A 0.9500 . ? C14 O15 1.264(9) . ? C14 C17 1.523(12) . ? C16 F13A 1.306(12) . ? C16 F11A 1.316(12) . ? C16 F11B 1.318(16) . ? C16 F12A 1.321(11) . ? C16 F13B 1.323(16) . ? C16 F12B 1.323(16) . ? C17 F14B 1.293(14) . ? C17 F15A 1.303(12) . ? C17 F16B 1.306(15) . ? C17 F15B 1.308(15) . ? C17 F16A 1.308(11) . ? C17 F14A 1.308(13) . ? O21 C22 1.265(9) . ? C22 C23 1.361(11) . ? C22 C26 1.536(12) . ? C23 C24 1.396(11) . ? C23 H23A 0.9500 . ? C24 O25 1.265(10) . ? C24 C27 1.514(13) . ? C26 F21 1.308(13) . ? C26 F22 1.309(12) . ? C26 F23 1.323(12) . ? C27 F25 1.204(15) . ? C27 F26 1.254(14) . ? C27 F24 1.317(17) . ? O31 C32 1.262(10) . ? C32 C33 1.385(12) . ? C32 C36 1.507(8) . ? C33 C34 1.359(11) . ? C33 H33A 0.9500 . ? C34 O35 1.274(9) . ? C34 C37 1.519(12) . ? C36 F33A 1.305(15) . ? C36 F33B 1.314(15) . ? C36 F31B 1.314(15) . ? C36 F31A 1.318(14) . ? C36 F32A 1.341(14) . ? C36 F32B 1.363(15) . ? C37 F36 1.280(11) . ? C37 F35 1.287(14) . ? C37 F34 1.303(13) . ? 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 O25 Eu O31 121.4(2) . . ? O25 Eu O11 140.3(2) . . ? O31 Eu O11 79.5(2) . . ? O25 Eu O21 71.9(2) . . ? O31 Eu O21 81.3(2) . . ? O11 Eu O21 79.6(2) . . ? O25 Eu O35 73.9(2) . . ? O31 Eu O35 71.7(2) . . ? O11 Eu O35 144.8(2) . . ? O21 Eu O35 114.7(2) . . ? O25 Eu O15 75.1(2) . . ? O31 Eu O15 146.5(2) . . ? O11 Eu O15 71.9(2) . . ? O21 Eu O15 76.8(2) . . ? O35 Eu O15 140.9(2) . . ? O25 Eu O1 80.2(3) . . ? O31 Eu O1 134.2(2) . . ? O11 Eu O1 110.3(2) . . ? O21 Eu O1 143.6(2) . . ? O35 Eu O1 78.0(2) . . ? O15 Eu O1 73.7(2) . . ? O25 Eu O5 139.3(2) . . ? O31 Eu O5 76.5(2) . . ? O11 Eu O5 74.6(2) . . ? O21 Eu O5 148.5(2) . . ? O35 Eu O5 79.2(2) . . ? O15 Eu O5 111.1(2) . . ? O1 Eu O5 64.5(3) . . ? C2 O1 C3 116.7(9) . . ? C2 O1 Eu 124.4(8) . . ? C3 O1 Eu 113.2(7) . . ? O1 C2 H2A 109.5 . . ? O1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 O1 113.5(11) . . ? C4 C3 H3A 108.9 . . ? O1 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? O1 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C3 C4 O5 109.3(10) . . ? C3 C4 H4A 109.8 . . ? O5 C4 H4A 109.8 . . ? C3 C4 H4B 109.8 . . ? O5 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? C6 O5 C4 110.3(9) . . ? C6 O5 Eu 125.5(6) . . ? C4 O5 Eu 119.7(7) . . ? O5 C6 H6A 109.5 . . ? O5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 O11 Eu 135.2(6) . . ? O11 C12 C13 126.5(8) . . ? O11 C12 C16 114.8(8) . . ? C13 C12 C16 118.7(8) . . ? C12 C13 C14 122.3(8) . . ? C12 C13 H13A 118.8 . . ? C14 C13 H13A 118.8 . . ? O15 C14 C13 127.6(8) . . ? O15 C14 C17 113.4(7) . . ? C13 C14 C17 119.0(8) . . ? C14 O15 Eu 133.2(5) . . ? F13A C16 F11A 103.3(15) . . ? F13A C16 F11B 27(4) . . ? F11A C16 F11B 124(3) . . ? F13A C16 F12A 105.1(13) . . ? F11A C16 F12A 105.6(13) . . ? F11B C16 F12A 82(3) . . ? F13A C16 F13B 133(3) . . ? F11A C16 F13B 67(3) . . ? F11B C16 F13B 119(4) . . ? F12A C16 F13B 43(3) . . ? F13A C16 F12B 84(3) . . ? F11A C16 F12B 29(2) . . ? F11B C16 F12B 110(4) . . ? F12A C16 F12B 132.1(17) . . ? F13B C16 F12B 96(3) . . ? F13A C16 C12 112.8(11) . . ? F11A C16 C12 114.9(11) . . ? F11B C16 C12 112(3) . . ? F12A C16 C12 114.0(11) . . ? F13B C16 C12 113(2) . . ? F12B C16 C12 105(2) . . ? F14B C17 F15A 65.3(18) . . ? F14B C17 F16B 104(2) . . ? F15A C17 F16B 40(2) . . ? F14B C17 F15B 112(3) . . ? F15A C17 F15B 125(3) . . ? F16B C17 F15B 101(3) . . ? F14B C17 F16A 45(2) . . ? F15A C17 F16A 108.3(13) . . ? F16B C17 F16A 140.4(17) . . ? F15B C17 F16A 78(2) . . ? F14B C17 F14A 127(2) . . ? F15A C17 F14A 103.2(18) . . ? F16B C17 F14A 71(3) . . ? F15B C17 F14A 31(3) . . ? F16A C17 F14A 106.2(16) . . ? F14B C17 C14 117.6(13) . . ? F15A C17 C14 114.2(13) . . ? F16B C17 C14 106.2(19) . . ? F15B C17 C14 114(3) . . ? F16A C17 C14 110.2(10) . . ? F14A C17 C14 114.2(18) . . ? C22 O21 Eu 131.3(5) . . ? O21 C22 C23 128.1(8) . . ? O21 C22 C26 114.0(8) . . ? C23 C22 C26 117.9(9) . . ? C22 C23 C24 121.7(9) . . ? C22 C23 H23A 119.2 . . ? C24 C23 H23A 119.2 . . ? O25 C24 C23 126.4(8) . . ? O25 C24 C27 115.4(10) . . ? C23 C24 C27 118.2(9) . . ? C24 O25 Eu 133.2(6) . . ? F21 C26 F22 109.9(11) . . ? F21 C26 F23 106.7(11) . . ? F22 C26 F23 105.2(10) . . ? F21 C26 C22 110.7(9) . . ? F22 C26 C22 113.0(10) . . ? F23 C26 C22 111.1(9) . . ? F25 C27 F26 106.9(14) . . ? F25 C27 F24 104.4(16) . . ? F26 C27 F24 103.2(13) . . ? F25 C27 C24 114.4(13) . . ? F26 C27 C24 118.3(11) . . ? F24 C27 C24 108.3(12) . . ? C32 O31 Eu 135.3(6) . . ? O31 C32 C33 126.7(8) . . ? O31 C32 C36 115.0(9) . . ? C33 C32 C36 118.3(9) . . ? C34 C33 C32 122.4(9) . . ? C34 C33 H33A 118.8 . . ? C32 C33 H33A 118.8 . . ? O35 C34 C33 127.3(8) . . ? O35 C34 C37 113.9(8) . . ? C33 C34 C37 118.7(8) . . ? C34 O35 Eu 134.8(6) . . ? F33A C36 F33B 125(3) . . ? F33A C36 F31B 48(2) . . ? F33B C36 F31B 117(3) . . ? F33A C36 F31A 110(2) . . ? F33B C36 F31A 26(3) . . ? F31B C36 F31A 125(2) . . ? F33A C36 F32A 108.2(17) . . ? F33B C36 F32A 82.7(19) . . ? F31B C36 F32A 60(2) . . ? F31A C36 F32A 107.4(19) . . ? F33A C36 F32B 41.1(14) . . ? F33B C36 F32B 100(2) . . ? F31B C36 F32B 88(2) . . ? F31A C36 F32B 76.4(19) . . ? F32A C36 F32B 143.4(16) . . ? F33A C36 C32 112.1(15) . . ? F33B C36 C32 116(2) . . ? F31B C36 C32 122(2) . . ? F31A C36 C32 113.2(14) . . ? F32A C36 C32 106.1(12) . . ? F32B C36 C32 105.3(14) . . ? F36 C37 F35 106.7(12) . . ? F36 C37 F34 106.4(11) . . ? F35 C37 F34 105.2(11) . . ? F36 C37 C34 115.2(10) . . ? F35 C37 C34 113.2(10) . . ? F34 C37 C34 109.4(10) . . ? 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 O25 Eu O1 C2 -19.7(9) . . . . ? O31 Eu O1 C2 -144.4(9) . . . . ? O11 Eu O1 C2 120.5(9) . . . . ? O21 Eu O1 C2 20.3(11) . . . . ? O35 Eu O1 C2 -95.2(9) . . . . ? O15 Eu O1 C2 57.5(9) . . . . ? O5 Eu O1 C2 -178.9(10) . . . . ? O25 Eu O1 C3 132.5(8) . . . . ? O31 Eu O1 C3 7.8(9) . . . . ? O11 Eu O1 C3 -87.3(8) . . . . ? O21 Eu O1 C3 172.5(7) . . . . ? O35 Eu O1 C3 57.0(8) . . . . ? O15 Eu O1 C3 -150.3(8) . . . . ? O5 Eu O1 C3 -26.7(7) . . . . ? C2 O1 C3 C4 -154.6(13) . . . . ? Eu O1 C3 C4 50.9(14) . . . . ? O1 C3 C4 O5 -45.2(16) . . . . ? C3 C4 O5 C6 177.5(11) . . . . ? C3 C4 O5 Eu 19.8(14) . . . . ? O25 Eu O5 C6 177.3(8) . . . . ? O31 Eu O5 C6 54.5(8) . . . . ? O11 Eu O5 C6 -28.1(8) . . . . ? O21 Eu O5 C6 7.9(11) . . . . ? O35 Eu O5 C6 128.1(9) . . . . ? O15 Eu O5 C6 -91.3(8) . . . . ? O1 Eu O5 C6 -150.2(9) . . . . ? O25 Eu O5 C4 -28.7(9) . . . . ? O31 Eu O5 C4 -151.5(8) . . . . ? O11 Eu O5 C4 125.9(8) . . . . ? O21 Eu O5 C4 162.0(7) . . . . ? O35 Eu O5 C4 -77.9(8) . . . . ? O15 Eu O5 C4 62.8(8) . . . . ? O1 Eu O5 C4 3.9(7) . . . . ? O25 Eu O11 C12 18.4(10) . . . . ? O31 Eu O11 C12 145.7(9) . . . . ? O21 Eu O11 C12 62.7(8) . . . . ? O35 Eu O11 C12 -179.0(8) . . . . ? O15 Eu O11 C12 -16.7(8) . . . . ? O1 Eu O11 C12 -80.9(9) . . . . ? O5 Eu O11 C12 -135.6(9) . . . . ? Eu O11 C12 C13 10.7(15) . . . . ? Eu O11 C12 C16 -170.3(6) . . . . ? O11 C12 C13 C14 4.0(15) . . . . ? C16 C12 C13 C14 -174.9(8) . . . . ? C12 C13 C14 O15 -1.5(15) . . . . ? C12 C13 C14 C17 -179.0(8) . . . . ? C13 C14 O15 Eu -15.2(13) . . . . ? C17 C14 O15 Eu 162.4(6) . . . . ? O25 Eu O15 C14 -139.1(8) . . . . ? O31 Eu O15 C14 -14.1(10) . . . . ? O11 Eu O15 C14 18.6(7) . . . . ? O21 Eu O15 C14 -64.6(7) . . . . ? O35 Eu O15 C14 -177.6(7) . . . . ? O1 Eu O15 C14 137.0(8) . . . . ? O5 Eu O15 C14 83.4(8) . . . . ? O11 C12 C16 F13A -52.1(15) . . . . ? C13 C12 C16 F13A 126.9(13) . . . . ? O11 C12 C16 F11A 66.0(16) . . . . ? C13 C12 C16 F11A -115.0(15) . . . . ? O11 C12 C16 F11B -82(4) . . . . ? C13 C12 C16 F11B 98(4) . . . . ? O11 C12 C16 F12A -171.9(12) . . . . ? C13 C12 C16 F12A 7.2(16) . . . . ? O11 C12 C16 F13B 141(3) . . . . ? C13 C12 C16 F13B -40(3) . . . . ? O11 C12 C16 F12B 37(3) . . . . ? C13 C12 C16 F12B -144(3) . . . . ? O15 C14 C17 F14B 4(3) . . . . ? C13 C14 C17 F14B -178(3) . . . . ? O15 C14 C17 F15A -69.9(17) . . . . ? C13 C14 C17 F15A 107.9(16) . . . . ? O15 C14 C17 F16B -112(3) . . . . ? C13 C14 C17 F16B 66(3) . . . . ? O15 C14 C17 F15B 137(3) . . . . ? C13 C14 C17 F15B -45(3) . . . . ? O15 C14 C17 F16A 52.2(14) . . . . ? C13 C14 C17 F16A -129.9(13) . . . . ? O15 C14 C17 F14A 171.6(17) . . . . ? C13 C14 C17 F14A -10.6(19) . . . . ? O25 Eu O21 C22 26.9(8) . . . . ? O31 Eu O21 C22 154.1(8) . . . . ? O11 Eu O21 C22 -125.1(8) . . . . ? O35 Eu O21 C22 88.9(8) . . . . ? O15 Eu O21 C22 -51.4(8) . . . . ? O1 Eu O21 C22 -14.9(10) . . . . ? O5 Eu O21 C22 -160.3(7) . . . . ? Eu O21 C22 C23 -20.8(15) . . . . ? Eu O21 C22 C26 159.0(7) . . . . ? O21 C22 C23 C24 -3.3(17) . . . . ? C26 C22 C23 C24 176.8(10) . . . . ? C22 C23 C24 O25 5.5(17) . . . . ? C22 C23 C24 C27 -176.0(11) . . . . ? C23 C24 O25 Eu 17.3(16) . . . . ? C27 C24 O25 Eu -161.3(8) . . . . ? O31 Eu O25 C24 -93.0(9) . . . . ? O11 Eu O25 C24 20.6(11) . . . . ? O21 Eu O25 C24 -25.6(9) . . . . ? O35 Eu O25 C24 -149.0(9) . . . . ? O15 Eu O25 C24 55.1(9) . . . . ? O1 Eu O25 C24 130.7(9) . . . . ? O5 Eu O25 C24 160.2(8) . . . . ? O21 C22 C26 F21 -60.5(13) . . . . ? C23 C22 C26 F21 119.4(12) . . . . ? O21 C22 C26 F22 175.7(10) . . . . ? C23 C22 C26 F22 -4.4(15) . . . . ? O21 C22 C26 F23 57.8(13) . . . . ? C23 C22 C26 F23 -122.3(11) . . . . ? O25 C24 C27 F25 -66(2) . . . . ? C23 C24 C27 F25 114.8(18) . . . . ? O25 C24 C27 F26 166.2(13) . . . . ? C23 C24 C27 F26 -12(2) . . . . ? O25 C24 C27 F24 49.5(16) . . . . ? C23 C24 C27 F24 -129.3(13) . . . . ? O25 Eu O31 C32 -72.1(9) . . . . ? O11 Eu O31 C32 144.4(9) . . . . ? O21 Eu O31 C32 -134.7(9) . . . . ? O35 Eu O31 C32 -15.0(8) . . . . ? O15 Eu O31 C32 175.8(8) . . . . ? O1 Eu O31 C32 36.2(10) . . . . ? O5 Eu O31 C32 67.9(9) . . . . ? Eu O31 C32 C33 14.7(16) . . . . ? Eu O31 C32 C36 -168.5(8) . . . . ? O31 C32 C33 C34 -1.7(16) . . . . ? C36 C32 C33 C34 -178.3(10) . . . . ? C32 C33 C34 O35 -2.7(16) . . . . ? C32 C33 C34 C37 -179.3(10) . . . . ? C33 C34 O35 Eu -5.6(15) . . . . ? C37 C34 O35 Eu 171.1(7) . . . . ? O25 Eu O35 C34 142.3(8) . . . . ? O31 Eu O35 C34 10.5(8) . . . . ? O11 Eu O35 C34 -26.3(10) . . . . ? O21 Eu O35 C34 81.5(8) . . . . ? O15 Eu O35 C34 -179.0(7) . . . . ? O1 Eu O35 C34 -134.6(8) . . . . ? O5 Eu O35 C34 -68.7(8) . . . . ? O31 C32 C36 F33A 36(2) . . . . ? C33 C32 C36 F33A -147.3(19) . . . . ? O31 C32 C36 F33B -172(2) . . . . ? C33 C32 C36 F33B 5(3) . . . . ? O31 C32 C36 F31B -18(4) . . . . ? C33 C32 C36 F31B 159(3) . . . . ? O31 C32 C36 F31A 160.1(19) . . . . ? C33 C32 C36 F31A -23(2) . . . . ? O31 C32 C36 F32A -82.4(13) . . . . ? C33 C32 C36 F32A 94.6(13) . . . . ? O31 C32 C36 F32B 78.6(16) . . . . ? C33 C32 C36 F32B -104.4(16) . . . . ? O35 C34 C37 F36 -175.3(11) . . . . ? C33 C34 C37 F36 1.7(16) . . . . ? O35 C34 C37 F35 -52.2(14) . . . . ? C33 C34 C37 F35 124.8(12) . . . . ? O35 C34 C37 F34 64.9(14) . . . . ? C33 C34 C37 F34 -118.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.921 _refine_diff_density_min -1.647 _refine_diff_density_rms 0.137 # Attachment '- GdCif.txt' data_k1162m _database_code_depnum_ccdc_archive 'CCDC 833376' #TrackingRef '- GdCif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H13 F18 Gd O8' _chemical_formula_sum 'C19 H13 F18 Gd O8' _chemical_formula_weight 868.54 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.5673(3) _cell_length_b 15.9349(3) _cell_length_c 20.9592(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5867.17(19) _cell_formula_units_Z 8 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 9896 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.00 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.967 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3336 _exptl_absorpt_coefficient_mu 2.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4450 _exptl_absorpt_correction_T_max 0.8686 _exptl_absorpt_process_details SADABS _exptl_special_details ; -CF3, ANISO, 60/40, SADI C-F -CF3, ANISO, 52/48, SADI C-F -CF3, ANISO, 54/46, SADI C-F ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27100 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6400 _reflns_number_gt 4352 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0418P)^2^+10.2390P] 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 6400 _refine_ls_number_parameters 496 _refine_ls_number_restraints 221 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd Gd 0.134302(15) 0.654861(14) 0.240643(10) 0.05188(10) Uani 1 1 d U . . O1 O 0.2725(2) 0.6729(3) 0.23391(17) 0.0836(11) Uani 1 1 d U . . C2 C 0.3254(5) 0.6247(7) 0.2684(4) 0.134(3) Uani 1 1 d U . . H2A H 0.3362 0.5734 0.2453 0.202 Uiso 1 1 calc R . . H2B H 0.3045 0.6111 0.3099 0.202 Uiso 1 1 calc R . . H2C H 0.3721 0.6565 0.2738 0.202 Uiso 1 1 calc R . . C3 C 0.2986(4) 0.7068(5) 0.1749(4) 0.112(2) Uani 1 1 d U . . H3A H 0.3529 0.7202 0.1784 0.135 Uiso 1 1 calc R . . H3B H 0.2925 0.6647 0.1412 0.135 Uiso 1 1 calc R . . C4 C 0.2584(5) 0.7792(5) 0.1584(3) 0.107(2) Uani 1 1 d U . . H4A H 0.2690 0.7936 0.1138 0.128 Uiso 1 1 calc R . . H4B H 0.2754 0.8260 0.1852 0.128 Uiso 1 1 calc R . . O5 O 0.1777(3) 0.7670(2) 0.16662(18) 0.0861(11) Uani 1 1 d U . . C6 C 0.1366(5) 0.8405(4) 0.1517(3) 0.111(3) Uani 1 1 d U . . H6A H 0.1514 0.8851 0.1806 0.167 Uiso 1 1 calc R . . H6B H 0.0825 0.8297 0.1560 0.167 Uiso 1 1 calc R . . H6C H 0.1478 0.8572 0.1081 0.167 Uiso 1 1 calc R . . O11 O 0.0761(2) 0.77846(19) 0.27752(14) 0.0599(8) Uani 1 1 d U . . C12 C 0.0664(3) 0.8112(3) 0.3309(2) 0.0541(11) Uani 1 1 d U A . C13 C 0.0991(3) 0.7877(3) 0.3882(2) 0.0559(11) Uani 1 1 d U . . H13A H 0.0850 0.8159 0.4258 0.067 Uiso 1 1 calc R . . C14 C 0.1519(3) 0.7239(3) 0.3914(2) 0.0499(10) Uani 1 1 d U B . O15 O 0.17678(19) 0.68032(19) 0.34664(14) 0.0555(8) Uani 1 1 d U . . C16 C 0.0125(4) 0.8861(4) 0.3304(3) 0.0785(15) Uani 1 1 d DU . . C17 C 0.1855(3) 0.7014(3) 0.4568(2) 0.0673(13) Uani 1 1 d DU . . F11A F -0.0492(7) 0.8654(15) 0.2998(12) 0.133(6) Uani 0.54 1 d PDU A 1 F12A F -0.0070(17) 0.9099(14) 0.3871(7) 0.164(9) Uani 0.54 1 d PDU A 1 F13A F 0.0420(16) 0.9476(12) 0.2994(11) 0.133(7) Uani 0.54 1 d PDU A 1 F11B F 0.0181(19) 0.9355(15) 0.3797(9) 0.139(8) Uani 0.46 1 d PDU A 2 F12B F 0.0230(18) 0.9352(15) 0.2826(11) 0.141(10) Uani 0.46 1 d PDU A 2 F13B F -0.0590(9) 0.868(2) 0.3269(17) 0.183(13) Uani 0.46 1 d PDU A 2 F14A F 0.1678(9) 0.7530(9) 0.5022(6) 0.117(5) Uani 0.60 1 d PDU B 1 F15A F 0.1645(9) 0.6276(5) 0.4758(6) 0.120(4) Uani 0.60 1 d PDU B 1 F16A F 0.2593(4) 0.7030(9) 0.4539(6) 0.125(4) Uani 0.60 1 d PDU B 1 F14B F 0.2389(14) 0.6470(14) 0.4555(7) 0.159(10) Uani 0.40 1 d PDU B 2 F15B F 0.2048(16) 0.7653(13) 0.4890(11) 0.139(9) Uani 0.40 1 d PDU B 2 F16B F 0.1312(9) 0.6682(15) 0.4904(9) 0.145(8) Uani 0.40 1 d PDU B 2 O21 O 0.0347(2) 0.6002(2) 0.30367(15) 0.0630(8) Uani 1 1 d U . . C22 C 0.0349(3) 0.5479(3) 0.3489(2) 0.0659(13) Uani 1 1 d U . . C23 C 0.0906(4) 0.4900(3) 0.3636(3) 0.0757(14) Uani 1 1 d U . . H23A H 0.0848 0.4557 0.3998 0.091 Uiso 1 1 calc R . . C24 C 0.1543(4) 0.4816(3) 0.3262(3) 0.0703(14) Uani 1 1 d U . . O25 O 0.1732(2) 0.5231(2) 0.27858(16) 0.0683(9) Uani 1 1 d U . . C26 C -0.0360(4) 0.5531(5) 0.3913(3) 0.0948(18) Uani 1 1 d U . . C27 C 0.2093(6) 0.4123(5) 0.3439(4) 0.117(3) Uani 1 1 d U . . F21 F -0.0442(3) 0.6262(4) 0.4154(3) 0.163(2) Uani 1 1 d U . . F22 F -0.0371(3) 0.4950(4) 0.4362(2) 0.158(2) Uani 1 1 d U . . F23 F -0.0978(2) 0.5374(3) 0.3573(2) 0.1178(13) Uani 1 1 d U . . F24 F 0.2780(4) 0.4434(5) 0.3485(5) 0.266(4) Uani 1 1 d U . . F25 F 0.2152(7) 0.3568(5) 0.3057(3) 0.315(6) Uani 1 1 d U . . F26 F 0.2026(3) 0.3795(3) 0.3986(2) 0.1493(19) Uani 1 1 d U . . O31 O 0.0342(2) 0.6663(2) 0.16738(16) 0.0730(10) Uani 1 1 d U . . C32 C 0.0258(3) 0.6491(4) 0.1089(2) 0.0678(13) Uani 1 1 d DU C . C33 C 0.0734(3) 0.6015(3) 0.0715(2) 0.0660(13) Uani 1 1 d U . . H33A H 0.0603 0.5922 0.0286 0.079 Uiso 1 1 calc R . . C34 C 0.1389(3) 0.5673(3) 0.0944(2) 0.0613(12) Uani 1 1 d U . . O35 O 0.1662(2) 0.5749(2) 0.14947(15) 0.0648(9) Uani 1 1 d U . . C36 C -0.0439(4) 0.6883(7) 0.0789(3) 0.125(3) Uani 1 1 d DU . . C37 C 0.1867(5) 0.5149(4) 0.0493(3) 0.0923(19) Uani 1 1 d U . . F31A F -0.0425(12) 0.6950(19) 0.0187(6) 0.214(11) Uani 0.52 1 d PDU C 1 F32A F -0.0988(9) 0.6298(14) 0.0864(10) 0.189(7) Uani 0.52 1 d PDU C 1 F33A F -0.0752(12) 0.7469(12) 0.1099(11) 0.195(9) Uani 0.52 1 d PDU C 1 F31B F -0.1062(10) 0.673(3) 0.1072(11) 0.278(16) Uani 0.48 1 d PDU C 2 F32B F -0.0350(11) 0.7723(9) 0.0769(10) 0.202(9) Uani 0.48 1 d PDU C 2 F33B F -0.0531(11) 0.6680(18) 0.0197(5) 0.158(8) Uani 0.48 1 d PDU C 2 F34 F 0.1890(4) 0.4372(3) 0.0684(2) 0.180(3) Uani 1 1 d U . . F35 F 0.2563(3) 0.5399(4) 0.0475(3) 0.182(3) Uani 1 1 d U . . F36 F 0.1643(3) 0.5134(3) -0.00857(17) 0.1470(19) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd 0.06862(18) 0.05036(14) 0.03667(13) -0.00432(9) -0.00058(10) 0.00940(11) O1 0.076(3) 0.122(3) 0.052(2) -0.009(2) 0.0051(18) -0.007(2) C2 0.081(5) 0.229(10) 0.093(5) 0.007(6) 0.005(4) 0.035(6) C3 0.099(5) 0.134(6) 0.103(5) 0.011(5) 0.028(4) -0.018(4) C4 0.126(5) 0.108(5) 0.085(4) 0.000(4) 0.020(4) -0.037(4) O5 0.117(3) 0.067(2) 0.074(2) 0.0043(19) 0.029(2) 0.004(2) C6 0.198(8) 0.071(4) 0.065(4) 0.019(3) 0.028(4) 0.029(4) O11 0.080(2) 0.0543(17) 0.0448(17) 0.0004(14) 0.0010(16) 0.0164(17) C12 0.063(3) 0.043(2) 0.056(3) -0.003(2) 0.008(2) 0.005(2) C13 0.072(3) 0.055(3) 0.041(2) -0.010(2) 0.008(2) 0.005(2) C14 0.061(3) 0.051(2) 0.038(2) -0.0020(18) 0.0051(19) -0.005(2) O15 0.066(2) 0.0585(18) 0.0419(16) -0.0064(14) 0.0001(15) 0.0141(16) C16 0.089(4) 0.068(4) 0.079(4) -0.008(3) 0.001(3) 0.028(3) C17 0.081(4) 0.076(3) 0.044(3) -0.004(2) 0.000(3) 0.008(3) F11A 0.074(6) 0.126(10) 0.200(14) -0.031(10) -0.019(8) 0.053(6) F12A 0.24(2) 0.155(19) 0.103(7) -0.011(7) 0.038(8) 0.135(15) F13A 0.153(12) 0.056(5) 0.191(17) 0.036(8) 0.008(11) 0.019(5) F11B 0.21(2) 0.079(9) 0.132(10) -0.054(9) -0.038(12) 0.069(9) F12B 0.19(2) 0.115(15) 0.118(9) 0.038(10) 0.018(13) 0.097(14) F13B 0.071(6) 0.127(12) 0.35(4) -0.079(18) 0.020(11) 0.029(6) F14A 0.174(12) 0.127(8) 0.050(4) -0.026(6) -0.016(6) 0.069(8) F15A 0.209(13) 0.080(4) 0.070(6) 0.024(4) -0.031(7) -0.017(6) F16A 0.071(4) 0.217(12) 0.086(6) 0.040(8) -0.014(4) 0.030(6) F14B 0.224(19) 0.210(19) 0.043(6) 0.022(10) -0.003(10) 0.147(16) F15B 0.21(2) 0.121(9) 0.086(14) -0.014(8) -0.075(14) -0.031(12) F16B 0.140(11) 0.22(2) 0.071(10) 0.077(14) -0.006(7) -0.048(12) O21 0.068(2) 0.064(2) 0.0566(19) 0.0090(16) -0.0047(16) 0.0042(16) C22 0.078(3) 0.066(3) 0.054(3) 0.006(2) -0.008(2) -0.011(3) C23 0.098(4) 0.066(3) 0.064(3) 0.013(3) -0.009(3) -0.003(3) C24 0.101(4) 0.053(3) 0.056(3) -0.006(2) -0.018(3) 0.014(3) O25 0.096(3) 0.0585(19) 0.0510(19) -0.0041(15) -0.0042(18) 0.0223(19) C26 0.090(4) 0.118(5) 0.076(4) 0.017(4) 0.004(3) -0.013(4) C27 0.161(7) 0.100(5) 0.090(5) 0.017(4) -0.006(5) 0.062(5) F21 0.157(5) 0.159(4) 0.174(5) -0.072(4) 0.098(4) -0.056(4) F22 0.127(4) 0.223(5) 0.122(4) 0.092(4) 0.033(3) 0.001(4) F23 0.085(3) 0.131(3) 0.137(4) 0.024(3) -0.001(2) -0.016(3) F24 0.132(5) 0.232(7) 0.433(13) 0.194(7) 0.021(6) 0.082(5) F25 0.602(15) 0.206(6) 0.136(5) -0.078(5) -0.128(7) 0.295(8) F26 0.192(5) 0.137(4) 0.119(3) 0.053(3) -0.023(3) 0.059(3) O31 0.073(2) 0.098(3) 0.0475(19) -0.0022(17) -0.0031(16) 0.018(2) C32 0.062(3) 0.093(4) 0.049(3) 0.014(3) -0.006(2) -0.011(3) C33 0.088(4) 0.069(3) 0.042(3) 0.004(2) -0.006(2) -0.011(3) C34 0.098(4) 0.046(2) 0.039(2) -0.0030(19) 0.007(2) -0.003(2) O35 0.087(3) 0.064(2) 0.0432(17) -0.0089(15) -0.0022(16) 0.0147(18) C36 0.073(5) 0.235(9) 0.068(4) 0.012(5) -0.011(3) 0.034(5) C37 0.142(6) 0.087(4) 0.048(3) -0.010(3) 0.003(4) 0.034(4) F31A 0.167(16) 0.38(3) 0.091(7) 0.088(10) 0.013(8) 0.161(17) F32A 0.062(7) 0.344(15) 0.160(14) -0.054(11) -0.001(7) -0.010(9) F33A 0.143(19) 0.283(15) 0.157(16) -0.046(15) -0.063(13) 0.125(12) F31B 0.079(8) 0.64(5) 0.115(15) 0.11(3) 0.019(11) 0.07(2) F32B 0.21(2) 0.214(8) 0.180(18) -0.030(11) -0.091(13) 0.152(11) F33B 0.104(10) 0.30(2) 0.070(6) 0.002(9) -0.052(7) -0.017(11) F34 0.347(8) 0.087(3) 0.106(3) 0.010(2) 0.067(4) 0.093(4) F35 0.129(4) 0.263(6) 0.153(5) -0.114(5) 0.047(3) 0.013(4) F36 0.234(5) 0.159(4) 0.048(2) -0.029(2) -0.003(3) 0.068(4) _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 Gd O31 2.341(4) . ? Gd O25 2.346(3) . ? Gd O11 2.350(3) . ? Gd O21 2.359(3) . ? Gd O35 2.364(3) . ? Gd O15 2.379(3) . ? Gd O1 2.449(4) . ? Gd O5 2.487(4) . ? O1 C2 1.405(9) . ? O1 C3 1.424(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.396(10) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 O5 1.441(8) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? O5 C6 1.410(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? O11 C12 1.247(5) . ? C12 C13 1.383(6) . ? C12 C16 1.523(7) . ? C13 C14 1.378(6) . ? C13 H13A 0.9400 . ? C14 O15 1.246(5) . ? C14 C17 1.533(7) . ? C16 F12B 1.285(13) . ? C16 F13A 1.285(12) . ? C16 F12A 1.293(12) . ? C16 F13B 1.293(13) . ? C16 F11B 1.302(12) . ? C16 F11A 1.302(12) . ? C17 F15B 1.268(12) . ? C17 F14B 1.278(11) . ? C17 F14A 1.295(9) . ? C17 F15A 1.295(9) . ? C17 F16A 1.298(9) . ? C17 F16B 1.299(11) . ? O21 C22 1.262(6) . ? C22 C23 1.381(8) . ? C22 C26 1.531(9) . ? C23 C24 1.374(8) . ? C23 H23A 0.9400 . ? C24 O25 1.242(6) . ? C24 C27 1.514(9) . ? C26 F21 1.279(8) . ? C26 F22 1.320(8) . ? C26 F23 1.322(8) . ? C27 F25 1.197(9) . ? C27 F26 1.266(8) . ? C27 F24 1.308(11) . ? O31 C32 1.265(6) . ? C32 C33 1.374(7) . ? C32 C36 1.512(7) . ? C33 C34 1.361(7) . ? C33 H33A 0.9400 . ? C34 O35 1.254(6) . ? C34 C37 1.516(8) . ? C36 F33A 1.263(12) . ? C36 F31A 1.267(12) . ? C36 F31B 1.268(13) . ? C36 F33B 1.294(12) . ? C36 F32B 1.348(13) . ? C36 F32A 1.350(13) . ? C37 F36 1.275(7) . ? C37 F35 1.287(9) . ? C37 F34 1.301(7) . ? 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 O31 Gd O25 120.69(13) . . ? O31 Gd O11 79.86(12) . . ? O25 Gd O11 139.91(11) . . ? O31 Gd O21 80.73(12) . . ? O25 Gd O21 72.28(13) . . ? O11 Gd O21 78.63(12) . . ? O31 Gd O35 71.91(12) . . ? O25 Gd O35 73.90(11) . . ? O11 Gd O35 145.16(11) . . ? O21 Gd O35 115.40(12) . . ? O31 Gd O15 146.61(11) . . ? O25 Gd O15 75.21(11) . . ? O11 Gd O15 71.72(10) . . ? O21 Gd O15 76.86(11) . . ? O35 Gd O15 140.60(11) . . ? O31 Gd O1 134.23(13) . . ? O25 Gd O1 80.56(15) . . ? O11 Gd O1 110.59(14) . . ? O21 Gd O1 144.19(12) . . ? O35 Gd O1 77.42(13) . . ? O15 Gd O1 73.90(12) . . ? O31 Gd O5 76.43(15) . . ? O25 Gd O5 139.92(14) . . ? O11 Gd O5 74.70(12) . . ? O21 Gd O5 147.39(13) . . ? O35 Gd O5 79.09(12) . . ? O15 Gd O5 111.34(13) . . ? O1 Gd O5 64.88(15) . . ? C2 O1 C3 116.2(6) . . ? C2 O1 Gd 124.2(5) . . ? C3 O1 Gd 114.4(4) . . ? O1 C2 H2A 109.5 . . ? O1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 O1 111.5(6) . . ? C4 C3 H3A 109.3 . . ? O1 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? O1 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C3 C4 O5 110.9(6) . . ? C3 C4 H4A 109.5 . . ? O5 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? O5 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? C6 O5 C4 111.4(5) . . ? C6 O5 Gd 125.3(4) . . ? C4 O5 Gd 118.2(4) . . ? O5 C6 H6A 109.5 . . ? O5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 O11 Gd 134.9(3) . . ? O11 C12 C13 127.5(4) . . ? O11 C12 C16 114.1(4) . . ? C13 C12 C16 118.4(4) . . ? C14 C13 C12 121.5(4) . . ? C14 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? O15 C14 C13 127.6(4) . . ? O15 C14 C17 114.0(4) . . ? C13 C14 C17 118.4(4) . . ? C14 O15 Gd 133.5(3) . . ? F12B C16 F13A 24(3) . . ? F12B C16 F12A 125.3(19) . . ? F13A C16 F12A 110.4(15) . . ? F12B C16 F13B 104(2) . . ? F13A C16 F13B 123(2) . . ? F12A C16 F13B 82(2) . . ? F12B C16 F11B 104.0(16) . . ? F13A C16 F11B 84.9(19) . . ? F12A C16 F11B 28(2) . . ? F13B C16 F11B 104.9(19) . . ? F12B C16 F11A 84(2) . . ? F13A C16 F11A 106.2(16) . . ? F12A C16 F11A 107.8(16) . . ? F13B C16 F11A 26(2) . . ? F11B C16 F11A 127.4(19) . . ? F12B C16 C12 113.1(14) . . ? F13A C16 C12 110.5(13) . . ? F12A C16 C12 112.8(13) . . ? F13B C16 C12 115.1(16) . . ? F11B C16 C12 114.9(15) . . ? F11A C16 C12 108.8(11) . . ? F15B C17 F14B 111.1(17) . . ? F15B C17 F14A 33.1(13) . . ? F14B C17 F14A 128.4(12) . . ? F15B C17 F15A 129.8(13) . . ? F14B C17 F15A 66.4(12) . . ? F14A C17 F15A 106.3(9) . . ? F15B C17 F16A 75.1(13) . . ? F14B C17 F16A 43.8(13) . . ? F14A C17 F16A 105.1(10) . . ? F15A C17 F16A 108.4(9) . . ? F15B C17 F16B 103.5(14) . . ? F14B C17 F16B 105.9(13) . . ? F14A C17 F16B 71.6(12) . . ? F15A C17 F16B 41.7(9) . . ? F16A C17 F16B 140.0(10) . . ? F15B C17 C14 113.0(13) . . ? F14B C17 C14 115.0(8) . . ? F14A C17 C14 114.6(8) . . ? F15A C17 C14 112.2(7) . . ? F16A C17 C14 109.8(6) . . ? F16B C17 C14 107.3(9) . . ? C22 O21 Gd 131.5(3) . . ? O21 C22 C23 127.7(5) . . ? O21 C22 C26 113.5(5) . . ? C23 C22 C26 118.8(5) . . ? C24 C23 C22 121.0(5) . . ? C24 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? O25 C24 C23 128.7(5) . . ? O25 C24 C27 114.6(6) . . ? C23 C24 C27 116.8(6) . . ? C24 O25 Gd 132.1(3) . . ? F21 C26 F22 110.8(7) . . ? F21 C26 F23 107.0(7) . . ? F22 C26 F23 103.9(6) . . ? F21 C26 C22 111.7(6) . . ? F22 C26 C22 112.8(6) . . ? F23 C26 C22 110.2(6) . . ? F25 C27 F26 108.0(8) . . ? F25 C27 F24 104.5(10) . . ? F26 C27 F24 100.2(8) . . ? F25 C27 C24 115.4(7) . . ? F26 C27 C24 117.6(7) . . ? F24 C27 C24 109.3(7) . . ? C32 O31 Gd 135.0(3) . . ? O31 C32 C33 126.9(5) . . ? O31 C32 C36 114.0(5) . . ? C33 C32 C36 119.0(5) . . ? C34 C33 C32 122.3(5) . . ? C34 C33 H33A 118.9 . . ? C32 C33 H33A 118.9 . . ? O35 C34 C33 127.5(5) . . ? O35 C34 C37 114.6(5) . . ? C33 C34 C37 117.9(5) . . ? C34 O35 Gd 134.8(3) . . ? F33A C36 F31A 117.4(17) . . ? F33A C36 F31B 61.7(16) . . ? F31A C36 F31B 119.9(17) . . ? F33A C36 F33B 128.7(17) . . ? F31A C36 F33B 21(2) . . ? F31B C36 F33B 107.1(17) . . ? F33A C36 F32B 48.2(13) . . ? F31A C36 F32B 83.3(16) . . ? F31B C36 F32B 108(2) . . ? F33B C36 F32B 103.4(17) . . ? F33A C36 F32A 98.1(15) . . ? F31A C36 F32A 100.8(17) . . ? F31B C36 F32A 37(2) . . ? F33B C36 F32A 81.3(15) . . ? F32B C36 F32A 140.6(15) . . ? F33A C36 C32 116.4(11) . . ? F31A C36 C32 115.5(10) . . ? F31B C36 C32 115.3(15) . . ? F33B C36 C32 113.3(12) . . ? F32B C36 C32 109.3(10) . . ? F32A C36 C32 104.2(12) . . ? F36 C37 F35 105.8(7) . . ? F36 C37 F34 106.5(6) . . ? F35 C37 F34 105.9(7) . . ? F36 C37 C34 115.7(6) . . ? F35 C37 C34 111.9(6) . . ? F34 C37 C34 110.5(6) . . ? 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 O31 Gd O1 C2 -144.8(5) . . . . ? O25 Gd O1 C2 -20.7(5) . . . . ? O11 Gd O1 C2 119.3(5) . . . . ? O21 Gd O1 C2 20.0(6) . . . . ? O35 Gd O1 C2 -96.2(5) . . . . ? O15 Gd O1 C2 56.5(5) . . . . ? O5 Gd O1 C2 -179.9(6) . . . . ? O31 Gd O1 C3 8.5(5) . . . . ? O25 Gd O1 C3 132.5(5) . . . . ? O11 Gd O1 C3 -87.5(5) . . . . ? O21 Gd O1 C3 173.3(4) . . . . ? O35 Gd O1 C3 57.1(5) . . . . ? O15 Gd O1 C3 -150.3(5) . . . . ? O5 Gd O1 C3 -26.6(5) . . . . ? C2 O1 C3 C4 -154.2(7) . . . . ? Gd O1 C3 C4 50.3(8) . . . . ? O1 C3 C4 O5 -46.2(9) . . . . ? C3 C4 O5 C6 178.5(6) . . . . ? C3 C4 O5 Gd 22.2(8) . . . . ? O31 Gd O5 C6 54.7(5) . . . . ? O25 Gd O5 C6 176.6(5) . . . . ? O11 Gd O5 C6 -28.3(5) . . . . ? O21 Gd O5 C6 7.9(6) . . . . ? O35 Gd O5 C6 128.5(5) . . . . ? O15 Gd O5 C6 -91.2(5) . . . . ? O1 Gd O5 C6 -150.4(5) . . . . ? O31 Gd O5 C4 -152.7(4) . . . . ? O25 Gd O5 C4 -30.8(5) . . . . ? O11 Gd O5 C4 124.3(4) . . . . ? O21 Gd O5 C4 160.5(4) . . . . ? O35 Gd O5 C4 -78.9(4) . . . . ? O15 Gd O5 C4 61.5(4) . . . . ? O1 Gd O5 C4 2.3(4) . . . . ? O31 Gd O11 C12 145.9(5) . . . . ? O25 Gd O11 C12 19.6(6) . . . . ? O21 Gd O11 C12 63.5(5) . . . . ? O35 Gd O11 C12 -178.1(4) . . . . ? O15 Gd O11 C12 -16.3(5) . . . . ? O1 Gd O11 C12 -80.4(5) . . . . ? O5 Gd O11 C12 -135.5(5) . . . . ? Gd O11 C12 C13 10.6(8) . . . . ? Gd O11 C12 C16 -170.2(4) . . . . ? O11 C12 C13 C14 3.2(8) . . . . ? C16 C12 C13 C14 -176.0(5) . . . . ? C12 C13 C14 O15 0.0(8) . . . . ? C12 C13 C14 C17 -179.9(5) . . . . ? C13 C14 O15 Gd -16.6(7) . . . . ? C17 C14 O15 Gd 163.3(3) . . . . ? O31 Gd O15 C14 -14.0(5) . . . . ? O25 Gd O15 C14 -137.9(4) . . . . ? O11 Gd O15 C14 19.1(4) . . . . ? O21 Gd O15 C14 -63.1(4) . . . . ? O35 Gd O15 C14 -177.3(4) . . . . ? O1 Gd O15 C14 137.8(4) . . . . ? O5 Gd O15 C14 83.8(4) . . . . ? O11 C12 C16 F12B -41.8(18) . . . . ? C13 C12 C16 F12B 137.5(17) . . . . ? O11 C12 C16 F13A -67.1(15) . . . . ? C13 C12 C16 F13A 112.2(14) . . . . ? O11 C12 C16 F12A 168.8(15) . . . . ? C13 C12 C16 F12A -11.9(16) . . . . ? O11 C12 C16 F13B 76.9(19) . . . . ? C13 C12 C16 F13B -103.7(19) . . . . ? O11 C12 C16 F11B -161.0(15) . . . . ? C13 C12 C16 F11B 18.3(16) . . . . ? O11 C12 C16 F11A 49.2(14) . . . . ? C13 C12 C16 F11A -131.5(13) . . . . ? O15 C14 C17 F15B 135.1(14) . . . . ? C13 C14 C17 F15B -45.0(15) . . . . ? O15 C14 C17 F14B 6.1(17) . . . . ? C13 C14 C17 F14B -174.0(16) . . . . ? O15 C14 C17 F14A 171.4(9) . . . . ? C13 C14 C17 F14A -8.7(11) . . . . ? O15 C14 C17 F15A -67.2(9) . . . . ? C13 C14 C17 F15A 112.7(9) . . . . ? O15 C14 C17 F16A 53.4(9) . . . . ? C13 C14 C17 F16A -126.7(9) . . . . ? O15 C14 C17 F16B -111.4(13) . . . . ? C13 C14 C17 F16B 68.5(14) . . . . ? O31 Gd O21 C22 152.0(4) . . . . ? O25 Gd O21 C22 25.5(4) . . . . ? O11 Gd O21 C22 -126.6(4) . . . . ? O35 Gd O21 C22 87.2(4) . . . . ? O15 Gd O21 C22 -52.9(4) . . . . ? O1 Gd O21 C22 -17.0(5) . . . . ? O5 Gd O21 C22 -162.1(4) . . . . ? Gd O21 C22 C23 -19.7(8) . . . . ? Gd O21 C22 C26 159.6(4) . . . . ? O21 C22 C23 C24 -2.4(9) . . . . ? C26 C22 C23 C24 178.4(6) . . . . ? C22 C23 C24 O25 3.3(10) . . . . ? C22 C23 C24 C27 -176.0(6) . . . . ? C23 C24 O25 Gd 18.3(9) . . . . ? C27 C24 O25 Gd -162.4(5) . . . . ? O31 Gd O25 C24 -92.3(5) . . . . ? O11 Gd O25 C24 20.5(6) . . . . ? O21 Gd O25 C24 -25.0(5) . . . . ? O35 Gd O25 C24 -149.1(5) . . . . ? O15 Gd O25 C24 55.7(5) . . . . ? O1 Gd O25 C24 131.4(5) . . . . ? O5 Gd O25 C24 161.4(5) . . . . ? O21 C22 C26 F21 -58.0(8) . . . . ? C23 C22 C26 F21 121.4(7) . . . . ? O21 C22 C26 F22 176.4(6) . . . . ? C23 C22 C26 F22 -4.3(9) . . . . ? O21 C22 C26 F23 60.8(8) . . . . ? C23 C22 C26 F23 -119.9(6) . . . . ? O25 C24 C27 F25 -65.2(13) . . . . ? C23 C24 C27 F25 114.2(11) . . . . ? O25 C24 C27 F26 165.4(8) . . . . ? C23 C24 C27 F26 -15.3(12) . . . . ? O25 C24 C27 F24 52.2(9) . . . . ? C23 C24 C27 F24 -128.5(8) . . . . ? O25 Gd O31 C32 -71.6(5) . . . . ? O11 Gd O31 C32 145.5(5) . . . . ? O21 Gd O31 C32 -134.5(5) . . . . ? O35 Gd O31 C32 -13.8(5) . . . . ? O15 Gd O31 C32 177.2(4) . . . . ? O1 Gd O31 C32 36.5(6) . . . . ? O5 Gd O31 C32 68.9(5) . . . . ? Gd O31 C32 C33 13.2(9) . . . . ? Gd O31 C32 C36 -165.2(5) . . . . ? O31 C32 C33 C34 -1.4(9) . . . . ? C36 C32 C33 C34 177.0(6) . . . . ? C32 C33 C34 O35 -1.9(9) . . . . ? C32 C33 C34 C37 179.2(6) . . . . ? C33 C34 O35 Gd -6.5(8) . . . . ? C37 C34 O35 Gd 172.5(4) . . . . ? O31 Gd O35 C34 10.6(5) . . . . ? O25 Gd O35 C34 141.4(5) . . . . ? O11 Gd O35 C34 -26.9(6) . . . . ? O21 Gd O35 C34 80.5(5) . . . . ? O15 Gd O35 C34 -179.0(4) . . . . ? O1 Gd O35 C34 -135.0(5) . . . . ? O5 Gd O35 C34 -68.6(5) . . . . ? O31 C32 C36 F33A 15.3(19) . . . . ? C33 C32 C36 F33A -163.3(16) . . . . ? O31 C32 C36 F31A 159.1(18) . . . . ? C33 C32 C36 F31A -20(2) . . . . ? O31 C32 C36 F31B -54(2) . . . . ? C33 C32 C36 F31B 127(2) . . . . ? O31 C32 C36 F33B -177.9(14) . . . . ? C33 C32 C36 F33B 3.5(16) . . . . ? O31 C32 C36 F32B 67.4(13) . . . . ? C33 C32 C36 F32B -111.2(12) . . . . ? O31 C32 C36 F32A -91.4(11) . . . . ? C33 C32 C36 F32A 90.0(10) . . . . ? O35 C34 C37 F36 -173.1(6) . . . . ? C33 C34 C37 F36 5.9(9) . . . . ? O35 C34 C37 F35 -51.9(8) . . . . ? C33 C34 C37 F35 127.2(7) . . . . ? O35 C34 C37 F34 65.8(8) . . . . ? C33 C34 C37 F34 -115.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.052 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.081 # Attachment '- LaCif.txt' data_k11104m _database_code_depnum_ccdc_archive 'CCDC 833377' #TrackingRef '- LaCif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H13 F18 La O8' _chemical_formula_sum 'C19 H13 F18 La O8' _chemical_formula_weight 850.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.899(3) _cell_length_b 16.105(3) _cell_length_c 21.124(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5749(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 61257 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.965 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 1.644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.645 _exptl_absorpt_correction_T_max 0.703 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; -CF3, ANISO, 60/40, SADI C-F -CF3, ANISO, 60/40, SADI C-F -CF3, ANISO, 50/50, SADI C-F ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 48471 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6579 _reflns_number_gt 4378 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V., 1997-2002)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXTL V6.1 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0684P)^2^+12.5170P] 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 6579 _refine_ls_number_parameters 496 _refine_ls_number_restraints 220 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1426 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.049 _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 La La 0.131036(17) 0.651637(17) 0.235915(12) 0.03855(12) Uani 1 1 d U . . O1 O 0.2809(2) 0.6675(3) 0.23010(17) 0.0576(10) Uani 1 1 d U . . C2 C 0.3357(5) 0.6265(8) 0.2713(4) 0.118(4) Uani 1 1 d U . . H2A H 0.3561 0.5765 0.2504 0.177 Uiso 1 1 calc R . . H2B H 0.3088 0.6108 0.3106 0.177 Uiso 1 1 calc R . . H2C H 0.3797 0.6640 0.2810 0.177 Uiso 1 1 calc R . . C3 C 0.3102(5) 0.7062(6) 0.1749(4) 0.109(3) Uani 1 1 d U . . H3A H 0.3647 0.7255 0.1839 0.130 Uiso 1 1 calc R . . H3B H 0.3141 0.6634 0.1414 0.130 Uiso 1 1 calc R . . C4 C 0.2697(4) 0.7703(7) 0.1513(4) 0.117(4) Uani 1 1 d U . . H4A H 0.2800 0.7738 0.1052 0.141 Uiso 1 1 calc R . . H4B H 0.2897 0.8221 0.1708 0.141 Uiso 1 1 calc R . . O5 O 0.1868(2) 0.7657(2) 0.1611(2) 0.0633(10) Uani 1 1 d U . . C6 C 0.1508(5) 0.8441(4) 0.1502(3) 0.0716(19) Uani 1 1 d U . . H6A H 0.1748 0.8857 0.1781 0.107 Uiso 1 1 calc R . . H6B H 0.0940 0.8403 0.1590 0.107 Uiso 1 1 calc R . . H6C H 0.1588 0.8605 0.1060 0.107 Uiso 1 1 calc R . . O11 O 0.0724(2) 0.7807(2) 0.27598(15) 0.0455(8) Uani 1 1 d U . . C12 C 0.0630(3) 0.8139(3) 0.3293(2) 0.0418(11) Uani 1 1 d U A . C13 C 0.0942(3) 0.7883(3) 0.3868(2) 0.0433(11) Uani 1 1 d U . . H13A H 0.0797 0.8172 0.4243 0.052 Uiso 1 1 calc R . . C14 C 0.1459(3) 0.7216(3) 0.3912(2) 0.0397(10) Uani 1 1 d U B . O15 O 0.1731(2) 0.6781(2) 0.34723(15) 0.0438(8) Uani 1 1 d U . . C16 C 0.0114(4) 0.8913(4) 0.3283(2) 0.0587(14) Uani 1 1 d DU . . C17 C 0.1743(3) 0.6969(3) 0.4579(2) 0.0502(12) Uani 1 1 d DU . . F11A F -0.0606(9) 0.869(2) 0.3128(19) 0.125(8) Uani 0.40 1 d PDU A 1 F12A F -0.015(2) 0.917(2) 0.3832(9) 0.163(12) Uani 0.40 1 d PDU A 1 F13A F 0.0412(16) 0.9540(16) 0.2970(15) 0.094(8) Uani 0.40 1 d PDU A 1 F11B F 0.0134(10) 0.9324(11) 0.3819(6) 0.088(4) Uani 0.60 1 d PDU A 2 F12B F 0.0353(14) 0.9412(11) 0.2835(9) 0.089(5) Uani 0.60 1 d PDU A 2 F13B F -0.0589(7) 0.8775(11) 0.3053(10) 0.106(5) Uani 0.60 1 d PDU A 2 F14A F 0.1639(15) 0.7520(11) 0.5012(6) 0.119(6) Uani 0.40 1 d PDU B 1 F15A F 0.1342(14) 0.6335(12) 0.4786(7) 0.123(7) Uani 0.40 1 d PDU B 1 F16A F 0.2470(8) 0.6747(18) 0.4599(8) 0.135(8) Uani 0.40 1 d PDU B 1 F14B F 0.2148(9) 0.6297(6) 0.4577(5) 0.097(4) Uani 0.60 1 d PDU B 2 F15B F 0.2176(7) 0.7542(6) 0.4839(4) 0.089(3) Uani 0.60 1 d PDU B 2 F16B F 0.1136(5) 0.6873(9) 0.4954(4) 0.092(3) Uani 0.60 1 d PDU B 2 O21 O 0.0275(2) 0.5913(2) 0.30498(16) 0.0474(8) Uani 1 1 d U . . C22 C 0.0298(3) 0.5397(3) 0.3499(2) 0.0497(12) Uani 1 1 d U . . C23 C 0.0892(4) 0.4836(4) 0.3637(3) 0.0586(14) Uani 1 1 d U . . H23A H 0.0841 0.4493 0.4000 0.070 Uiso 1 1 calc R . . C24 C 0.1561(4) 0.4758(3) 0.3261(3) 0.0562(13) Uani 1 1 d U . . O25 O 0.1731(2) 0.5160(2) 0.27682(17) 0.0535(9) Uani 1 1 d U . . C26 C -0.0421(4) 0.5425(4) 0.3936(3) 0.0622(15) Uani 1 1 d U . . C27 C 0.2182(5) 0.4098(4) 0.3430(3) 0.0802(19) Uani 1 1 d U . . F21 F -0.0471(2) 0.6160(3) 0.42168(19) 0.0835(11) Uani 1 1 d U . . F22 F -0.0411(3) 0.4840(3) 0.4380(2) 0.0962(14) Uani 1 1 d U . . F23 F -0.1084(2) 0.5320(3) 0.36087(19) 0.0803(11) Uani 1 1 d U . . F24 F 0.2903(3) 0.4504(4) 0.3527(3) 0.150(2) Uani 1 1 d U . . F25 F 0.2331(5) 0.3595(4) 0.3022(3) 0.193(4) Uani 1 1 d U . . F26 F 0.2082(3) 0.3754(3) 0.3982(2) 0.0996(14) Uani 1 1 d U . . O31 O 0.0256(2) 0.6720(2) 0.15691(16) 0.0512(9) Uani 1 1 d U . . C32 C 0.0173(3) 0.6575(3) 0.0985(3) 0.0471(12) Uani 1 1 d U C . C33 C 0.0630(3) 0.6048(3) 0.0611(2) 0.0498(12) Uani 1 1 d U . . H33A H 0.0486 0.5965 0.0181 0.060 Uiso 1 1 calc R . . C34 C 0.1286(3) 0.5643(3) 0.0847(2) 0.0457(12) Uani 1 1 d U . . O35 O 0.1564(2) 0.5686(2) 0.13960(15) 0.0494(8) Uani 1 1 d U . . C36 C -0.0512(4) 0.7068(4) 0.0677(3) 0.0683(16) Uani 1 1 d DU . . C37 C 0.1745(4) 0.5086(4) 0.0400(3) 0.0634(15) Uani 1 1 d U . . F31A F -0.0518(14) 0.7004(15) 0.0045(6) 0.071(4) Uani 0.50 1 d PDU C 1 F32A F -0.1166(8) 0.6692(14) 0.0876(9) 0.122(8) Uani 0.50 1 d PDU C 1 F33A F -0.049(2) 0.7860(9) 0.0819(15) 0.117(9) Uani 0.50 1 d PDU C 1 F31B F -0.1182(8) 0.7013(14) 0.0990(10) 0.119(7) Uani 0.50 1 d PDU C 2 F32B F -0.033(2) 0.7869(7) 0.0691(14) 0.090(6) Uani 0.50 1 d PDU C 2 F33B F -0.0618(17) 0.6823(18) 0.0080(6) 0.101(8) Uani 0.50 1 d PDU C 2 F34 F 0.1819(3) 0.4333(2) 0.06314(18) 0.1035(16) Uani 1 1 d U . . F35 F 0.2472(3) 0.5372(3) 0.0326(2) 0.1089(15) Uani 1 1 d U . . F36 F 0.1437(3) 0.5011(3) -0.01656(17) 0.1017(15) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La 0.0478(2) 0.03721(18) 0.03068(17) -0.00201(11) -0.00183(12) 0.00221(12) O1 0.047(2) 0.081(3) 0.045(2) -0.0034(18) -0.0011(16) -0.0006(18) C2 0.053(4) 0.227(12) 0.074(5) 0.026(6) 0.002(4) 0.041(6) C3 0.077(5) 0.128(7) 0.120(7) 0.050(6) 0.051(5) 0.026(5) C4 0.060(4) 0.172(9) 0.120(7) 0.079(7) 0.016(4) -0.003(5) O5 0.063(2) 0.050(2) 0.077(3) 0.0119(19) 0.014(2) 0.0020(19) C6 0.122(6) 0.044(3) 0.048(3) 0.009(3) 0.004(4) 0.004(3) O11 0.058(2) 0.0407(18) 0.0374(17) 0.0003(14) -0.0033(15) 0.0073(16) C12 0.049(3) 0.035(2) 0.042(3) 0.003(2) 0.003(2) -0.003(2) C13 0.055(3) 0.041(3) 0.033(2) -0.003(2) 0.003(2) 0.002(2) C14 0.051(3) 0.033(2) 0.036(2) 0.0020(19) 0.001(2) -0.006(2) O15 0.048(2) 0.0466(19) 0.0369(17) -0.0033(15) 0.0010(15) 0.0068(16) C16 0.070(4) 0.051(3) 0.055(3) -0.003(3) -0.004(3) 0.016(3) C17 0.061(3) 0.055(3) 0.035(2) 0.002(2) 0.000(2) 0.002(3) F11A 0.039(7) 0.101(15) 0.24(2) 0.046(14) 0.012(10) 0.008(7) F12A 0.24(3) 0.17(2) 0.081(10) 0.013(9) 0.040(11) 0.16(2) F13A 0.076(10) 0.033(7) 0.17(2) 0.013(11) 0.014(12) 0.011(6) F11B 0.117(8) 0.072(5) 0.075(6) -0.042(5) -0.026(5) 0.047(5) F12B 0.144(10) 0.046(7) 0.075(5) 0.014(5) -0.006(5) 0.021(6) F13B 0.076(6) 0.075(8) 0.168(13) -0.051(9) -0.039(7) 0.030(5) F14A 0.205(19) 0.101(10) 0.051(7) -0.026(8) -0.045(12) 0.067(11) F15A 0.185(17) 0.126(12) 0.057(9) 0.051(9) -0.043(10) -0.086(13) F16A 0.079(7) 0.28(3) 0.044(7) 0.017(15) 0.000(7) 0.063(11) F14B 0.164(10) 0.079(5) 0.049(4) 0.008(4) -0.032(7) 0.052(6) F15B 0.118(7) 0.094(6) 0.053(5) 0.009(4) -0.042(5) -0.041(6) F16B 0.073(5) 0.155(10) 0.047(5) 0.039(7) 0.008(3) -0.013(6) O21 0.049(2) 0.0445(19) 0.0491(19) 0.0029(16) -0.0027(16) -0.0050(15) C22 0.056(3) 0.047(3) 0.045(3) -0.001(2) -0.001(2) -0.012(2) C23 0.077(4) 0.050(3) 0.049(3) 0.012(3) -0.002(3) -0.003(3) C24 0.077(4) 0.041(3) 0.051(3) -0.002(2) -0.007(3) 0.008(3) O25 0.068(3) 0.049(2) 0.0432(19) -0.0009(16) -0.0005(17) 0.0102(18) C26 0.068(4) 0.061(4) 0.057(3) 0.005(3) 0.003(3) -0.015(3) C27 0.112(5) 0.058(4) 0.070(4) 0.013(3) -0.012(4) 0.028(4) F21 0.087(3) 0.086(3) 0.078(3) -0.021(2) 0.025(2) -0.018(2) F22 0.097(3) 0.105(3) 0.087(3) 0.042(3) 0.027(2) -0.003(2) F23 0.062(2) 0.089(3) 0.089(3) 0.003(2) 0.005(2) -0.022(2) F24 0.098(3) 0.131(5) 0.220(7) 0.071(4) -0.019(4) 0.024(3) F25 0.338(10) 0.150(5) 0.090(3) -0.050(3) -0.082(5) 0.181(6) F26 0.108(3) 0.098(3) 0.092(3) 0.043(3) -0.006(3) 0.029(3) O31 0.051(2) 0.062(2) 0.0403(18) -0.0027(16) -0.0016(16) 0.0033(17) C32 0.044(3) 0.055(3) 0.042(3) 0.007(2) -0.004(2) -0.013(2) C33 0.071(4) 0.047(3) 0.031(2) 0.004(2) -0.004(2) -0.005(2) C34 0.071(3) 0.034(3) 0.032(2) 0.0014(19) 0.003(2) -0.005(2) O35 0.069(2) 0.0447(19) 0.0344(17) -0.0010(15) -0.0013(16) 0.0049(17) C36 0.057(4) 0.091(4) 0.058(3) 0.005(3) -0.008(3) 0.006(3) C37 0.095(5) 0.056(3) 0.039(3) 0.000(3) 0.006(3) 0.006(3) F31A 0.083(10) 0.078(8) 0.052(5) 0.008(4) -0.006(5) 0.029(8) F32A 0.040(5) 0.26(2) 0.070(6) -0.002(10) 0.002(5) -0.022(9) F33A 0.116(15) 0.112(7) 0.123(18) -0.043(10) -0.057(15) 0.065(8) F31B 0.060(6) 0.178(14) 0.118(13) 0.080(12) 0.015(7) 0.050(7) F32B 0.118(15) 0.065(5) 0.086(9) 0.014(6) -0.016(8) 0.028(6) F33B 0.100(10) 0.139(17) 0.062(6) 0.006(7) -0.046(7) -0.016(9) F34 0.191(5) 0.058(2) 0.062(2) 0.0029(18) 0.025(3) 0.047(3) F35 0.102(3) 0.129(4) 0.096(3) -0.037(3) 0.043(3) 0.003(3) F36 0.161(4) 0.103(3) 0.0414(19) -0.024(2) -0.011(2) 0.048(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 La O11 2.454(3) . ? La O25 2.454(4) . ? La O31 2.464(4) . ? La O35 2.472(3) . ? La O21 2.476(3) . ? La O15 2.493(3) . ? La O1 2.548(4) . ? La O5 2.600(4) . ? O1 C3 1.412(8) . ? O1 C2 1.433(8) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.336(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O5 1.417(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O5 C6 1.421(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O11 C12 1.258(6) . ? C12 C13 1.386(7) . ? C12 C16 1.521(8) . ? C13 C14 1.388(7) . ? C13 H13A 0.9500 . ? C14 O15 1.251(6) . ? C14 C17 1.541(7) . ? C16 F13B 1.303(10) . ? C16 F12B 1.306(10) . ? C16 F13A 1.308(13) . ? C16 F11A 1.309(13) . ? C16 F12A 1.309(13) . ? C16 F11B 1.312(9) . ? C17 F16A 1.280(11) . ? C17 F14B 1.281(9) . ? C17 F14A 1.286(10) . ? C17 F15B 1.299(8) . ? C17 F15A 1.301(11) . ? C17 F16B 1.304(8) . ? O21 C22 1.263(6) . ? C22 C23 1.381(8) . ? C22 C26 1.525(8) . ? C23 C24 1.388(9) . ? C23 H23A 0.9500 . ? C24 O25 1.258(7) . ? C24 C27 1.535(9) . ? C26 F21 1.327(7) . ? C26 F23 1.328(7) . ? C26 F22 1.328(7) . ? C27 F25 1.209(8) . ? C27 F26 1.303(8) . ? C27 F24 1.397(10) . ? O31 C32 1.263(6) . ? C32 C33 1.393(8) . ? C32 C36 1.548(8) . ? C33 C34 1.378(7) . ? C33 H33A 0.9500 . ? C34 O35 1.254(6) . ? C34 C37 1.516(8) . ? C36 F33A 1.311(13) . ? C36 F31B 1.314(12) . ? C36 F32A 1.328(12) . ? C36 F32B 1.329(12) . ? C36 F33B 1.332(12) . ? C36 F31A 1.340(12) . ? C37 F36 1.308(7) . ? C37 F34 1.314(7) . ? C37 F35 1.321(8) . ? 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 O11 La O25 138.57(11) . . ? O11 La O31 80.14(12) . . ? O25 La O31 124.50(13) . . ? O11 La O35 144.30(11) . . ? O25 La O35 76.01(11) . . ? O31 La O35 68.88(12) . . ? O11 La O21 81.05(12) . . ? O25 La O21 69.37(12) . . ? O31 La O21 86.58(12) . . ? O35 La O21 113.26(12) . . ? O11 La O15 69.19(11) . . ? O25 La O15 74.80(11) . . ? O31 La O15 145.31(12) . . ? O35 La O15 145.04(12) . . ? O21 La O15 73.31(11) . . ? O11 La O1 109.42(13) . . ? O25 La O1 79.56(14) . . ? O31 La O1 132.29(12) . . ? O35 La O1 80.95(12) . . ? O21 La O1 140.33(12) . . ? O15 La O1 75.23(11) . . ? O11 La O5 75.97(12) . . ? O25 La O5 137.54(13) . . ? O31 La O5 75.90(13) . . ? O35 La O5 79.55(12) . . ? O21 La O5 153.07(12) . . ? O15 La O5 110.45(13) . . ? O1 La O5 62.57(13) . . ? C3 O1 C2 118.5(6) . . ? C3 O1 La 115.7(4) . . ? C2 O1 La 124.5(5) . . ? O1 C2 H2A 109.5 . . ? O1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 O1 118.0(7) . . ? C4 C3 H3A 107.8 . . ? O1 C3 H3A 107.8 . . ? C4 C3 H3B 107.8 . . ? O1 C3 H3B 107.8 . . ? H3A C3 H3B 107.1 . . ? C3 C4 O5 114.3(7) . . ? C3 C4 H4A 108.7 . . ? O5 C4 H4A 108.7 . . ? C3 C4 H4B 108.7 . . ? O5 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C4 O5 C6 110.6(6) . . ? C4 O5 La 119.0(4) . . ? C6 O5 La 124.8(4) . . ? O5 C6 H6A 109.5 . . ? O5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 O11 La 136.1(3) . . ? O11 C12 C13 127.6(5) . . ? O11 C12 C16 114.1(4) . . ? C13 C12 C16 118.3(4) . . ? C12 C13 C14 121.9(5) . . ? C12 C13 H13A 119.0 . . ? C14 C13 H13A 119.0 . . ? O15 C14 C13 127.9(4) . . ? O15 C14 C17 114.8(4) . . ? C13 C14 C17 117.2(4) . . ? C14 O15 La 133.8(3) . . ? F13B C16 F12B 96.7(16) . . ? F13B C16 F13A 107.1(17) . . ? F12B C16 F13A 16(3) . . ? F13B C16 F11A 9(3) . . ? F12B C16 F11A 106(2) . . ? F13A C16 F11A 116(2) . . ? F13B C16 F12A 94.4(19) . . ? F12B C16 F12A 123(2) . . ? F13A C16 F12A 109(2) . . ? F11A C16 F12A 90(2) . . ? F13B C16 F11B 115.6(12) . . ? F12B C16 F11B 107.9(12) . . ? F13A C16 F11B 92(2) . . ? F11A C16 F11B 112.2(18) . . ? F12A C16 F11B 24(2) . . ? F13B C16 C12 112.9(9) . . ? F12B C16 C12 109.7(11) . . ? F13A C16 C12 114.8(14) . . ? F11A C16 C12 108.2(15) . . ? F12A C16 C12 116.2(15) . . ? F11B C16 C12 112.7(9) . . ? F16A C17 F14B 41.5(11) . . ? F16A C17 F14A 107.5(14) . . ? F14B C17 F14A 131.2(9) . . ? F16A C17 F15B 69.1(12) . . ? F14B C17 F15B 107.4(8) . . ? F14A C17 F15B 44.5(10) . . ? F16A C17 F15A 105.7(15) . . ? F14B C17 F15A 67.5(12) . . ? F14A C17 F15A 103.5(14) . . ? F15B C17 F15A 135.2(8) . . ? F16A C17 F16B 134.6(10) . . ? F14B C17 F16B 108.8(9) . . ? F14A C17 F16B 62.9(12) . . ? F15B C17 F16B 105.8(8) . . ? F15A C17 F16B 45.1(10) . . ? F16A C17 C14 113.6(9) . . ? F14B C17 C14 112.5(6) . . ? F14A C17 C14 115.4(8) . . ? F15B C17 C14 112.2(6) . . ? F15A C17 C14 110.4(8) . . ? F16B C17 C14 110.0(6) . . ? C22 O21 La 132.9(3) . . ? O21 C22 C23 127.6(5) . . ? O21 C22 C26 114.3(5) . . ? C23 C22 C26 118.1(5) . . ? C22 C23 C24 122.1(5) . . ? C22 C23 H23A 118.9 . . ? C24 C23 H23A 118.9 . . ? O25 C24 C23 127.7(5) . . ? O25 C24 C27 113.1(6) . . ? C23 C24 C27 119.1(6) . . ? C24 O25 La 133.1(4) . . ? F21 C26 F23 107.0(6) . . ? F21 C26 F22 108.5(5) . . ? F23 C26 F22 106.7(5) . . ? F21 C26 C22 110.3(5) . . ? F23 C26 C22 110.7(5) . . ? F22 C26 C22 113.3(5) . . ? F25 C27 F26 112.3(7) . . ? F25 C27 F24 103.8(8) . . ? F26 C27 F24 100.3(6) . . ? F25 C27 C24 116.2(6) . . ? F26 C27 C24 114.5(7) . . ? F24 C27 C24 107.9(6) . . ? C32 O31 La 135.8(3) . . ? O31 C32 C33 127.3(5) . . ? O31 C32 C36 113.5(5) . . ? C33 C32 C36 119.2(5) . . ? C34 C33 C32 121.9(5) . . ? C34 C33 H33A 119.1 . . ? C32 C33 H33A 119.1 . . ? O35 C34 C33 127.5(5) . . ? O35 C34 C37 114.7(5) . . ? C33 C34 C37 117.8(5) . . ? C34 O35 La 136.6(3) . . ? F33A C36 F31B 89(2) . . ? F33A C36 F32A 113.3(18) . . ? F31B C36 F32A 24.9(18) . . ? F33A C36 F32B 17(3) . . ? F31B C36 F32B 105.0(17) . . ? F32A C36 F32B 129(2) . . ? F33A C36 F33B 121(2) . . ? F31B C36 F33B 109.9(17) . . ? F32A C36 F33B 93.0(18) . . ? F32B C36 F33B 110.0(17) . . ? F33A C36 F31A 107.7(17) . . ? F31B C36 F31A 119.3(16) . . ? F32A C36 F31A 105.9(14) . . ? F32B C36 F31A 95.7(19) . . ? F33B C36 F31A 15(3) . . ? F33A C36 C32 112.3(15) . . ? F31B C36 C32 113.4(9) . . ? F32A C36 C32 104.8(10) . . ? F32B C36 C32 108.1(14) . . ? F33B C36 C32 110.3(12) . . ? F31A C36 C32 112.7(10) . . ? F36 C37 F34 107.0(5) . . ? F36 C37 F35 107.1(5) . . ? F34 C37 F35 106.1(6) . . ? F36 C37 C34 114.8(6) . . ? F34 C37 C34 111.3(5) . . ? F35 C37 C34 110.1(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 O11 La O1 C3 -83.9(5) . . . . ? O25 La O1 C3 138.1(5) . . . . ? O31 La O1 C3 10.5(6) . . . . ? O35 La O1 C3 60.8(5) . . . . ? O21 La O1 C3 176.6(5) . . . . ? O15 La O1 C3 -145.0(6) . . . . ? O5 La O1 C3 -22.0(5) . . . . ? O11 La O1 C2 109.1(6) . . . . ? O25 La O1 C2 -28.9(6) . . . . ? O31 La O1 C2 -156.6(6) . . . . ? O35 La O1 C2 -106.2(6) . . . . ? O21 La O1 C2 9.5(7) . . . . ? O15 La O1 C2 48.0(6) . . . . ? O5 La O1 C2 170.9(6) . . . . ? C2 O1 C3 C4 -153.0(10) . . . . ? La O1 C3 C4 39.2(12) . . . . ? O1 C3 C4 O5 -31.8(15) . . . . ? C3 C4 O5 C6 164.6(9) . . . . ? C3 C4 O5 La 9.6(12) . . . . ? O11 La O5 C4 127.9(6) . . . . ? O25 La O5 C4 -22.7(7) . . . . ? O31 La O5 C4 -148.9(6) . . . . ? O35 La O5 C4 -78.3(6) . . . . ? O21 La O5 C4 160.2(6) . . . . ? O15 La O5 C4 66.9(6) . . . . ? O1 La O5 C4 6.9(6) . . . . ? O11 La O5 C6 -23.2(5) . . . . ? O25 La O5 C6 -173.8(4) . . . . ? O31 La O5 C6 60.0(5) . . . . ? O35 La O5 C6 130.6(5) . . . . ? O21 La O5 C6 9.0(6) . . . . ? O15 La O5 C6 -84.2(5) . . . . ? O1 La O5 C6 -144.2(5) . . . . ? O25 La O11 C12 16.2(6) . . . . ? O31 La O11 C12 148.4(5) . . . . ? O35 La O11 C12 178.1(4) . . . . ? O21 La O11 C12 60.3(5) . . . . ? O15 La O11 C12 -15.1(5) . . . . ? O1 La O11 C12 -80.1(5) . . . . ? O5 La O11 C12 -133.8(5) . . . . ? La O11 C12 C13 8.7(9) . . . . ? La O11 C12 C16 -171.8(3) . . . . ? O11 C12 C13 C14 3.8(9) . . . . ? C16 C12 C13 C14 -175.7(5) . . . . ? C12 C13 C14 O15 2.2(9) . . . . ? C12 C13 C14 C17 -177.8(5) . . . . ? C13 C14 O15 La -19.8(8) . . . . ? C17 C14 O15 La 160.1(3) . . . . ? O11 La O15 C14 20.3(4) . . . . ? O25 La O15 C14 -138.9(5) . . . . ? O31 La O15 C14 -9.2(5) . . . . ? O35 La O15 C14 -173.2(4) . . . . ? O21 La O15 C14 -66.3(4) . . . . ? O1 La O15 C14 138.2(4) . . . . ? O5 La O15 C14 85.5(4) . . . . ? O11 C12 C16 F13B 57.7(13) . . . . ? C13 C12 C16 F13B -122.7(13) . . . . ? O11 C12 C16 F12B -48.9(13) . . . . ? C13 C12 C16 F12B 130.7(12) . . . . ? O11 C12 C16 F13A -65.4(18) . . . . ? C13 C12 C16 F13A 114.2(18) . . . . ? O11 C12 C16 F11A 66.3(19) . . . . ? C13 C12 C16 F11A -114.2(19) . . . . ? O11 C12 C16 F12A 165.2(19) . . . . ? C13 C12 C16 F12A -15(2) . . . . ? O11 C12 C16 F11B -169.1(9) . . . . ? C13 C12 C16 F11B 10.5(11) . . . . ? O15 C14 C17 F16A 38.3(16) . . . . ? C13 C14 C17 F16A -141.7(15) . . . . ? O15 C14 C17 F14B -6.9(10) . . . . ? C13 C14 C17 F14B 173.0(9) . . . . ? O15 C14 C17 F14A 163.1(15) . . . . ? C13 C14 C17 F14A -17.0(16) . . . . ? O15 C14 C17 F15B 114.3(8) . . . . ? C13 C14 C17 F15B -65.7(9) . . . . ? O15 C14 C17 F15A -80.1(15) . . . . ? C13 C14 C17 F15A 99.8(15) . . . . ? O15 C14 C17 F16B -128.3(8) . . . . ? C13 C14 C17 F16B 51.6(9) . . . . ? O11 La O21 C22 -125.1(4) . . . . ? O25 La O21 C22 25.4(4) . . . . ? O31 La O21 C22 154.3(5) . . . . ? O35 La O21 C22 89.1(4) . . . . ? O15 La O21 C22 -54.3(4) . . . . ? O1 La O21 C22 -15.4(5) . . . . ? O5 La O21 C22 -156.7(4) . . . . ? La O21 C22 C23 -19.3(8) . . . . ? La O21 C22 C26 159.8(4) . . . . ? O21 C22 C23 C24 -2.0(9) . . . . ? C26 C22 C23 C24 179.0(5) . . . . ? C22 C23 C24 O25 0.5(10) . . . . ? C22 C23 C24 C27 -177.8(6) . . . . ? C23 C24 O25 La 22.6(9) . . . . ? C27 C24 O25 La -159.1(4) . . . . ? O11 La O25 C24 20.3(6) . . . . ? O31 La O25 C24 -97.3(5) . . . . ? O35 La O25 C24 -148.9(5) . . . . ? O21 La O25 C24 -27.0(5) . . . . ? O15 La O25 C24 50.6(5) . . . . ? O1 La O25 C24 127.9(5) . . . . ? O5 La O25 C24 154.4(5) . . . . ? O21 C22 C26 F21 -62.4(7) . . . . ? C23 C22 C26 F21 116.8(6) . . . . ? O21 C22 C26 F23 55.8(7) . . . . ? C23 C22 C26 F23 -125.0(6) . . . . ? O21 C22 C26 F22 175.7(5) . . . . ? C23 C22 C26 F22 -5.2(8) . . . . ? O25 C24 C27 F25 -55.9(11) . . . . ? C23 C24 C27 F25 122.6(9) . . . . ? O25 C24 C27 F26 170.7(6) . . . . ? C23 C24 C27 F26 -10.7(10) . . . . ? O25 C24 C27 F24 60.0(8) . . . . ? C23 C24 C27 F24 -121.5(7) . . . . ? O11 La O31 C32 146.3(5) . . . . ? O25 La O31 C32 -70.2(5) . . . . ? O35 La O31 C32 -15.6(5) . . . . ? O21 La O31 C32 -132.2(5) . . . . ? O15 La O31 C32 174.1(4) . . . . ? O1 La O31 C32 39.0(5) . . . . ? O5 La O31 C32 68.5(5) . . . . ? La O31 C32 C33 16.6(9) . . . . ? La O31 C32 C36 -162.2(4) . . . . ? O31 C32 C33 C34 -4.0(9) . . . . ? C36 C32 C33 C34 174.8(5) . . . . ? C32 C33 C34 O35 -0.7(9) . . . . ? C32 C33 C34 C37 -179.8(5) . . . . ? C33 C34 O35 La -7.2(9) . . . . ? C37 C34 O35 La 171.9(4) . . . . ? O11 La O35 C34 -20.5(6) . . . . ? O25 La O35 C34 147.3(5) . . . . ? O31 La O35 C34 11.1(5) . . . . ? O21 La O35 C34 87.5(5) . . . . ? O15 La O35 C34 -178.6(4) . . . . ? O1 La O35 C34 -131.3(5) . . . . ? O5 La O35 C34 -67.7(5) . . . . ? O31 C32 C36 F33A 48.8(18) . . . . ? C33 C32 C36 F33A -130.1(18) . . . . ? O31 C32 C36 F31B -49.8(14) . . . . ? C33 C32 C36 F31B 131.2(14) . . . . ? O31 C32 C36 F32A -74.6(11) . . . . ? C33 C32 C36 F32A 106.4(11) . . . . ? O31 C32 C36 F32B 66.1(15) . . . . ? C33 C32 C36 F32B -112.8(15) . . . . ? O31 C32 C36 F33B -173.6(15) . . . . ? C33 C32 C36 F33B 7.5(16) . . . . ? O31 C32 C36 F31A 170.7(14) . . . . ? C33 C32 C36 F31A -8.3(15) . . . . ? O35 C34 C37 F36 177.1(5) . . . . ? C33 C34 C37 F36 -3.7(8) . . . . ? O35 C34 C37 F34 55.4(8) . . . . ? C33 C34 C37 F34 -125.4(6) . . . . ? O35 C34 C37 F35 -61.9(6) . . . . ? C33 C34 C37 F35 117.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.653 _refine_diff_density_min -1.134 _refine_diff_density_rms 0.114 # Attachment '- PrCif.txt' data_ef634 _database_code_depnum_ccdc_archive 'CCDC 833378' #TrackingRef '- PrCif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H13 F18 O8 Pr' _chemical_formula_sum 'C19 H13 F18 O8 Pr' _chemical_formula_weight 852.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.322(4) _cell_length_b 16.072(3) _cell_length_c 21.175(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5895(2) _cell_formula_units_Z 8 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 29651 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description chip _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.920 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 1.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.688 _exptl_absorpt_correction_T_max 0.954 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ANISO two -CF3 disordered C-F SADI, 52/48 and 35/65 C32-C36 1.51 DFIX ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 29019 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5185 _reflns_number_gt 3936 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V., 1997-2002)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0629P)^2^+12.0918P] 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 5185 _refine_ls_number_parameters 469 _refine_ls_number_restraints 197 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.017 _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 Pr Pr 0.133841(19) 0.652035(19) 0.239948(14) 0.05605(14) Uani 1 1 d U . . O1 O 0.2783(3) 0.6681(3) 0.2334(2) 0.0874(13) Uani 1 1 d U . . C2 C 0.3308(5) 0.6200(9) 0.2708(4) 0.150(4) Uani 1 1 d U . . H2A H 0.3657 0.5898 0.2433 0.225 Uiso 1 1 calc R . . H2B H 0.3019 0.5808 0.2964 0.225 Uiso 1 1 calc R . . H2C H 0.3602 0.6567 0.2980 0.225 Uiso 1 1 calc R . . C3 C 0.3050(5) 0.7052(6) 0.1772(5) 0.138(3) Uani 1 1 d U . . H3A H 0.3595 0.7198 0.1828 0.165 Uiso 1 1 calc R . . H3B H 0.3021 0.6638 0.1433 0.165 Uiso 1 1 calc R . . C4 C 0.2663(5) 0.7746(6) 0.1581(4) 0.120(3) Uani 1 1 d U . . H4A H 0.2768 0.7848 0.1133 0.144 Uiso 1 1 calc R . . H4B H 0.2849 0.8228 0.1821 0.144 Uiso 1 1 calc R . . O5 O 0.1852(3) 0.7657(3) 0.1673(2) 0.0911(13) Uani 1 1 d U . . C6 C 0.1470(5) 0.8401(4) 0.1529(4) 0.105(3) Uani 1 1 d U . . H6A H 0.1676 0.8847 0.1789 0.158 Uiso 1 1 calc R . . H6B H 0.0923 0.8339 0.1612 0.158 Uiso 1 1 calc R . . H6C H 0.1548 0.8534 0.1087 0.158 Uiso 1 1 calc R . . O11 O 0.0746(2) 0.7780(2) 0.27870(17) 0.0659(9) Uani 1 1 d U . . C12 C 0.0654(3) 0.8114(3) 0.3314(3) 0.0595(12) Uani 1 1 d U . . C13 C 0.0974(3) 0.7872(3) 0.3881(2) 0.0620(13) Uani 1 1 d U . . H13A H 0.0833 0.8157 0.4251 0.074 Uiso 1 1 calc R . . C14 C 0.1497(3) 0.7224(3) 0.3922(2) 0.0550(11) Uani 1 1 d U A . O15 O 0.1753(2) 0.6787(2) 0.34815(16) 0.0616(9) Uani 1 1 d U . . C16 C 0.0125(4) 0.8864(4) 0.3304(3) 0.0832(17) Uani 1 1 d U . . C17 C 0.1811(4) 0.6992(4) 0.4576(3) 0.0726(14) Uani 1 1 d DU . . F11 F -0.0546(3) 0.8698(3) 0.3113(4) 0.192(3) Uani 1 1 d U . . F12 F 0.0070(4) 0.9248(4) 0.3837(3) 0.192(3) Uani 1 1 d U . . F13 F 0.0359(4) 0.9426(3) 0.2909(3) 0.159(2) Uani 1 1 d U . . F14A F 0.2560(5) 0.6987(13) 0.4570(6) 0.124(5) Uani 0.52 1 d PDU A 1 F15A F 0.1578(13) 0.6274(8) 0.4760(7) 0.130(6) Uani 0.52 1 d PDU A 1 F16A F 0.1608(11) 0.7489(10) 0.5032(6) 0.126(6) Uani 0.52 1 d PDU A 1 F14B F 0.1250(8) 0.6710(16) 0.4918(9) 0.149(8) Uani 0.48 1 d PDU A 2 F15B F 0.2079(15) 0.7611(10) 0.4878(8) 0.148(7) Uani 0.48 1 d PDU A 2 F16B F 0.2310(14) 0.6397(13) 0.4559(7) 0.154(8) Uani 0.48 1 d PDU A 2 O21 O 0.0319(2) 0.5938(2) 0.30486(18) 0.0703(10) Uani 1 1 d U . . C22 C 0.0327(4) 0.5427(4) 0.3496(3) 0.0706(14) Uani 1 1 d U . . C23 C 0.0895(4) 0.4856(4) 0.3645(3) 0.0831(17) Uani 1 1 d U . . H23A H 0.0836 0.4517 0.4003 0.100 Uiso 1 1 calc R . . C24 C 0.1553(4) 0.4773(4) 0.3274(3) 0.0768(16) Uani 1 1 d U . . O25 O 0.1734(3) 0.5182(2) 0.27975(19) 0.0751(11) Uani 1 1 d U . . C26 C -0.0384(5) 0.5455(5) 0.3925(4) 0.0959(19) Uani 1 1 d U . . C27 C 0.2148(7) 0.4100(5) 0.3446(4) 0.115(3) Uani 1 1 d U . . F21 F -0.0455(3) 0.6186(4) 0.4183(3) 0.146(2) Uani 1 1 d U . . F22 F -0.0399(3) 0.4877(4) 0.4358(3) 0.155(2) Uani 1 1 d U . . F23 F -0.1020(3) 0.5335(3) 0.3592(2) 0.1222(15) Uani 1 1 d U . . F24 F 0.2833(4) 0.4488(5) 0.3570(4) 0.213(3) Uani 1 1 d U . . F25 F 0.2272(7) 0.3600(5) 0.3060(3) 0.287(6) Uani 1 1 d U . . F26 F 0.2041(4) 0.3761(4) 0.3994(3) 0.156(2) Uani 1 1 d U . . O31 O 0.0323(2) 0.6682(3) 0.16286(19) 0.0762(11) Uani 1 1 d U . . C32 C 0.0236(3) 0.6530(4) 0.1048(3) 0.0721(15) Uani 1 1 d DU B . C33 C 0.0701(4) 0.6022(4) 0.0681(3) 0.0719(15) Uani 1 1 d U . . H33A H 0.0564 0.5927 0.0258 0.086 Uiso 1 1 calc R . . C34 C 0.1356(4) 0.5651(3) 0.0915(3) 0.0680(14) Uani 1 1 d U . . O35 O 0.1625(2) 0.5704(2) 0.14640(17) 0.0715(10) Uani 1 1 d U . . C36 C -0.0460(4) 0.6960(6) 0.0743(3) 0.112(2) Uani 1 1 d DU . . C37 C 0.1816(6) 0.5112(5) 0.0471(3) 0.098(2) Uani 1 1 d U . . F31A F -0.1035(15) 0.712(2) 0.1113(13) 0.179(12) Uani 0.35 1 d PDU B 1 F32A F -0.024(2) 0.7738(11) 0.0617(17) 0.157(11) Uani 0.35 1 d PDU B 1 F33A F -0.061(2) 0.660(2) 0.0198(9) 0.179(14) Uani 0.35 1 d PDU B 1 F31B F -0.0459(10) 0.6927(11) 0.0122(5) 0.130(5) Uani 0.65 1 d PDU B 2 F32B F -0.1060(6) 0.6493(10) 0.0908(6) 0.200(7) Uani 0.65 1 d PDU B 2 F33B F -0.0526(14) 0.7727(9) 0.0910(10) 0.220(10) Uani 0.65 1 d PDU B 2 F34 F 0.1885(5) 0.4362(3) 0.0677(2) 0.175(3) Uani 1 1 d U . . F35 F 0.2528(4) 0.5392(5) 0.0419(3) 0.177(3) Uani 1 1 d U . . F36 F 0.1576(4) 0.5075(4) -0.0099(2) 0.162(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr 0.0701(2) 0.0551(2) 0.0430(2) -0.00415(12) -0.00147(12) 0.00728(13) O1 0.070(3) 0.130(4) 0.062(3) -0.009(2) 0.0029(19) -0.002(2) C2 0.075(5) 0.265(13) 0.109(7) 0.012(7) 0.000(5) 0.040(7) C3 0.103(6) 0.144(8) 0.166(8) 0.036(6) 0.058(6) 0.005(5) C4 0.116(5) 0.132(7) 0.113(6) 0.014(5) 0.033(5) -0.021(5) O5 0.109(3) 0.069(3) 0.096(3) 0.008(2) 0.029(3) 0.005(2) C6 0.169(7) 0.074(4) 0.073(5) 0.014(3) 0.023(5) 0.011(4) O11 0.086(3) 0.059(2) 0.052(2) -0.0009(16) -0.0014(18) 0.0147(18) C12 0.065(3) 0.050(3) 0.064(3) 0.000(2) 0.007(2) 0.005(2) C13 0.074(3) 0.065(3) 0.048(3) -0.008(2) 0.008(2) 0.003(3) C14 0.067(3) 0.055(3) 0.043(2) -0.001(2) 0.004(2) -0.006(2) O15 0.072(2) 0.066(2) 0.0466(19) -0.0047(16) -0.0006(17) 0.0107(18) C16 0.098(5) 0.069(4) 0.083(4) -0.009(3) 0.001(4) 0.028(3) C17 0.091(4) 0.080(4) 0.047(3) -0.002(3) 0.000(3) 0.010(3) F11 0.083(3) 0.118(4) 0.374(11) -0.048(5) -0.043(5) 0.041(3) F12 0.282(8) 0.163(5) 0.130(4) -0.052(4) -0.022(4) 0.149(5) F13 0.183(5) 0.087(3) 0.209(6) 0.058(4) 0.039(5) 0.053(3) F14A 0.080(5) 0.221(16) 0.072(6) 0.020(10) -0.015(4) 0.030(8) F15A 0.215(17) 0.100(7) 0.075(10) 0.031(6) -0.035(11) -0.025(9) F16A 0.185(15) 0.140(11) 0.053(5) -0.025(8) -0.011(8) 0.073(10) F14B 0.134(10) 0.24(2) 0.076(11) 0.078(15) 0.000(6) -0.042(12) F15B 0.24(2) 0.128(9) 0.080(12) 0.002(7) -0.073(12) -0.052(12) F16B 0.223(18) 0.185(15) 0.055(6) 0.012(10) -0.020(10) 0.117(14) O21 0.074(2) 0.070(2) 0.067(2) 0.0092(19) -0.0050(18) -0.0011(18) C22 0.083(3) 0.070(4) 0.059(3) 0.004(3) -0.007(3) -0.009(3) C23 0.105(4) 0.071(4) 0.073(4) 0.015(3) -0.013(3) -0.006(3) C24 0.108(4) 0.056(3) 0.066(4) -0.003(3) -0.015(3) 0.011(3) O25 0.099(3) 0.066(2) 0.060(2) -0.0033(18) -0.004(2) 0.020(2) C26 0.097(5) 0.110(5) 0.081(5) 0.017(4) 0.006(3) -0.016(4) C27 0.165(7) 0.087(5) 0.094(5) 0.017(4) -0.024(5) 0.044(5) F21 0.143(4) 0.151(4) 0.145(5) -0.047(4) 0.068(4) -0.037(4) F22 0.136(4) 0.198(5) 0.129(4) 0.084(4) 0.032(3) -0.004(4) F23 0.091(3) 0.141(4) 0.134(4) 0.021(3) 0.002(3) -0.025(3) F24 0.141(5) 0.183(6) 0.314(10) 0.096(6) -0.035(5) 0.050(4) F25 0.517(15) 0.204(6) 0.140(5) -0.083(5) -0.134(7) 0.265(8) F26 0.172(5) 0.150(4) 0.146(4) 0.065(4) -0.021(4) 0.050(4) O31 0.079(3) 0.096(3) 0.053(2) -0.004(2) -0.0033(19) 0.013(2) C32 0.067(3) 0.096(4) 0.053(3) 0.010(3) -0.007(3) -0.013(3) C33 0.096(4) 0.075(4) 0.044(3) 0.006(3) -0.009(3) -0.013(3) C34 0.102(4) 0.054(3) 0.048(3) 0.003(2) 0.008(3) -0.008(3) O35 0.100(3) 0.067(2) 0.048(2) -0.0076(17) -0.0009(19) 0.012(2) C36 0.086(5) 0.176(7) 0.075(4) 0.011(5) -0.013(4) 0.013(5) C37 0.153(6) 0.087(5) 0.052(4) -0.004(3) 0.009(4) 0.023(4) F31A 0.127(16) 0.26(3) 0.152(17) 0.088(18) 0.025(14) 0.097(18) F32A 0.121(14) 0.157(11) 0.19(3) 0.059(15) -0.032(17) 0.042(12) F33A 0.154(18) 0.29(3) 0.095(12) 0.016(15) -0.078(13) -0.044(19) F31B 0.128(9) 0.186(11) 0.076(4) 0.028(5) -0.015(4) 0.041(9) F32B 0.064(5) 0.42(2) 0.120(8) 0.029(11) 0.003(5) -0.019(9) F33B 0.25(3) 0.226(11) 0.18(2) -0.071(13) -0.121(17) 0.153(10) F34 0.331(8) 0.095(3) 0.099(3) 0.010(3) 0.061(4) 0.089(4) F35 0.157(4) 0.225(6) 0.148(5) -0.083(5) 0.062(4) 0.003(5) F36 0.264(6) 0.169(5) 0.053(3) -0.034(3) -0.011(3) 0.075(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 Pr O25 2.410(4) . ? Pr O11 2.413(4) . ? Pr O31 2.414(4) . ? Pr O21 2.426(4) . ? Pr O35 2.427(4) . ? Pr O15 2.439(3) . ? Pr O1 2.519(5) . ? Pr O5 2.548(4) . ? O1 C3 1.409(9) . ? O1 C2 1.432(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.362(11) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 O5 1.426(9) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? O5 C6 1.400(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? O11 C12 1.249(6) . ? C12 C13 1.377(7) . ? C12 C16 1.515(8) . ? C13 C14 1.383(7) . ? C13 H13A 0.9400 . ? C14 O15 1.250(6) . ? C14 C17 1.533(8) . ? C16 F11 1.258(8) . ? C16 F12 1.290(8) . ? C16 F13 1.295(8) . ? C17 F15B 1.271(11) . ? C17 F15A 1.282(10) . ? C17 F16B 1.290(11) . ? C17 F14B 1.292(11) . ? C17 F14A 1.299(10) . ? C17 F16A 1.301(10) . ? O21 C22 1.254(7) . ? C22 C23 1.382(9) . ? C22 C26 1.530(9) . ? C23 C24 1.390(10) . ? C23 H23A 0.9400 . ? C24 O25 1.244(7) . ? C24 C27 1.537(10) . ? C26 F21 1.301(9) . ? C26 F22 1.306(8) . ? C26 F23 1.322(8) . ? C27 F25 1.167(10) . ? C27 F26 1.294(10) . ? C27 F24 1.365(11) . ? O31 C32 1.263(7) . ? C32 C33 1.385(9) . ? C32 C36 1.533(7) . ? C33 C34 1.374(8) . ? C33 H33A 0.9400 . ? C34 O35 1.256(7) . ? C34 C37 1.506(9) . ? C36 F33B 1.287(12) . ? C36 F31A 1.292(14) . ? C36 F31B 1.315(11) . ? C36 F33A 1.316(14) . ? C36 F32B 1.328(11) . ? C36 F32A 1.335(14) . ? C37 F36 1.277(8) . ? C37 F34 1.286(8) . ? C37 F35 1.317(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O25 Pr O11 138.66(13) . . ? O25 Pr O31 122.68(15) . . ? O11 Pr O31 80.20(13) . . ? O25 Pr O21 70.38(14) . . ? O11 Pr O21 79.73(13) . . ? O31 Pr O21 83.93(14) . . ? O25 Pr O35 75.21(13) . . ? O11 Pr O35 144.88(12) . . ? O31 Pr O35 69.86(14) . . ? O21 Pr O35 113.75(14) . . ? O25 Pr O15 75.19(13) . . ? O11 Pr O15 70.04(12) . . ? O31 Pr O15 146.21(13) . . ? O21 Pr O15 75.53(13) . . ? O35 Pr O15 143.23(13) . . ? O25 Pr O1 80.12(16) . . ? O11 Pr O1 110.78(15) . . ? O31 Pr O1 132.50(14) . . ? O21 Pr O1 142.54(14) . . ? O35 Pr O1 78.88(14) . . ? O15 Pr O1 74.98(13) . . ? O25 Pr O5 138.75(15) . . ? O11 Pr O5 75.64(13) . . ? O31 Pr O5 76.65(16) . . ? O21 Pr O5 150.78(14) . . ? O35 Pr O5 79.85(14) . . ? O15 Pr O5 109.75(15) . . ? O1 Pr O5 63.04(16) . . ? C3 O1 C2 119.2(7) . . ? C3 O1 Pr 114.6(5) . . ? C2 O1 Pr 123.0(6) . . ? O1 C2 H2A 109.5 . . ? O1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 O1 115.8(8) . . ? C4 C3 H3A 108.3 . . ? O1 C3 H3A 108.3 . . ? C4 C3 H3B 108.3 . . ? O1 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? C3 C4 O5 111.2(7) . . ? C3 C4 H4A 109.4 . . ? O5 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? O5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 O5 C4 110.5(6) . . ? C6 O5 Pr 125.4(4) . . ? C4 O5 Pr 119.9(5) . . ? O5 C6 H6A 109.5 . . ? O5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 O11 Pr 135.9(3) . . ? O11 C12 C13 127.3(5) . . ? O11 C12 C16 114.0(5) . . ? C13 C12 C16 118.8(5) . . ? C12 C13 C14 122.1(5) . . ? C12 C13 H13A 118.9 . . ? C14 C13 H13A 118.9 . . ? O15 C14 C13 127.4(5) . . ? O15 C14 C17 114.4(5) . . ? C13 C14 C17 118.2(5) . . ? C14 O15 Pr 134.1(3) . . ? F11 C16 F12 108.4(7) . . ? F11 C16 F13 103.3(7) . . ? F12 C16 F13 104.7(7) . . ? F11 C16 C12 113.3(6) . . ? F12 C16 C12 114.3(6) . . ? F13 C16 C12 112.0(6) . . ? F15B C17 F15A 131.9(11) . . ? F15B C17 F16B 110.5(14) . . ? F15A C17 F16B 63.5(11) . . ? F15B C17 F14B 105.6(13) . . ? F15A C17 F14B 43.8(10) . . ? F16B C17 F14B 105.1(13) . . ? F15B C17 F14A 69.1(12) . . ? F15A C17 F14A 108.2(11) . . ? F16B C17 F14A 47.5(10) . . ? F14B C17 F14A 139.0(11) . . ? F15B C17 F16A 41.0(10) . . ? F15A C17 F16A 104.0(11) . . ? F16B C17 F16A 131.1(11) . . ? F14B C17 F16A 66.3(12) . . ? F14A C17 F16A 106.4(11) . . ? F15B C17 C14 113.1(10) . . ? F15A C17 C14 112.4(9) . . ? F16B C17 C14 113.0(8) . . ? F14B C17 C14 108.9(9) . . ? F14A C17 C14 110.2(7) . . ? F16A C17 C14 115.1(9) . . ? C22 O21 Pr 132.3(4) . . ? O21 C22 C23 127.9(6) . . ? O21 C22 C26 114.9(6) . . ? C23 C22 C26 117.2(6) . . ? C22 C23 C24 121.3(6) . . ? C22 C23 H23A 119.4 . . ? C24 C23 H23A 119.4 . . ? O25 C24 C23 127.9(6) . . ? O25 C24 C27 113.3(7) . . ? C23 C24 C27 118.9(7) . . ? C24 O25 Pr 133.1(4) . . ? F21 C26 F22 110.2(7) . . ? F21 C26 F23 106.1(7) . . ? F22 C26 F23 104.7(7) . . ? F21 C26 C22 110.6(6) . . ? F22 C26 C22 114.4(7) . . ? F23 C26 C22 110.5(6) . . ? F25 C27 F26 111.3(9) . . ? F25 C27 F24 106.7(11) . . ? F26 C27 F24 98.4(8) . . ? F25 C27 C24 116.2(8) . . ? F26 C27 C24 114.4(8) . . ? F24 C27 C24 107.9(7) . . ? C32 O31 Pr 136.4(4) . . ? O31 C32 C33 126.2(5) . . ? O31 C32 C36 114.6(6) . . ? C33 C32 C36 119.2(6) . . ? C34 C33 C32 122.3(5) . . ? C34 C33 H33A 118.9 . . ? C32 C33 H33A 118.9 . . ? O35 C34 C33 127.6(6) . . ? O35 C34 C37 114.9(6) . . ? C33 C34 C37 117.5(6) . . ? C34 O35 Pr 135.7(4) . . ? F33B C36 F31A 64.8(15) . . ? F33B C36 F31B 108.3(13) . . ? F31A C36 F31B 127.9(17) . . ? F33B C36 F33A 130(2) . . ? F31A C36 F33A 118(2) . . ? F31B C36 F33A 27(2) . . ? F33B C36 F32B 113.5(13) . . ? F31A C36 F32B 49.5(16) . . ? F31B C36 F32B 104.0(11) . . ? F33A C36 F32B 80.4(17) . . ? F33B C36 F32A 35.3(19) . . ? F31A C36 F32A 99(2) . . ? F31B C36 F32A 80.7(18) . . ? F33A C36 F32A 107(2) . . ? F32B C36 F32A 143.7(19) . . ? F33B C36 C32 112.7(11) . . ? F31A C36 C32 116.2(13) . . ? F31B C36 C32 113.6(9) . . ? F33A C36 C32 108.8(17) . . ? F32B C36 C32 104.5(9) . . ? F32A C36 C32 106.3(17) . . ? F36 C37 F34 107.8(7) . . ? F36 C37 F35 104.0(7) . . ? F34 C37 F35 105.2(8) . . ? F36 C37 C34 116.3(7) . . ? F34 C37 C34 112.1(6) . . ? F35 C37 C34 110.5(6) . . ? 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 O25 Pr O1 C3 136.6(6) . . . . ? O11 Pr O1 C3 -84.9(6) . . . . ? O31 Pr O1 C3 10.9(7) . . . . ? O21 Pr O1 C3 174.6(5) . . . . ? O35 Pr O1 C3 59.9(6) . . . . ? O15 Pr O1 C3 -146.2(6) . . . . ? O5 Pr O1 C3 -24.3(6) . . . . ? O25 Pr O1 C2 -22.7(6) . . . . ? O11 Pr O1 C2 115.8(6) . . . . ? O31 Pr O1 C2 -148.4(6) . . . . ? O21 Pr O1 C2 15.4(7) . . . . ? O35 Pr O1 C2 -99.4(7) . . . . ? O15 Pr O1 C2 54.5(6) . . . . ? O5 Pr O1 C2 176.5(7) . . . . ? C2 O1 C3 C4 -153.9(10) . . . . ? Pr O1 C3 C4 46.0(11) . . . . ? O1 C3 C4 O5 -40.5(13) . . . . ? C3 C4 O5 C6 174.7(8) . . . . ? C3 C4 O5 Pr 16.6(11) . . . . ? O25 Pr O5 C6 -179.7(5) . . . . ? O11 Pr O5 C6 -27.7(6) . . . . ? O31 Pr O5 C6 55.5(6) . . . . ? O21 Pr O5 C6 5.8(7) . . . . ? O35 Pr O5 C6 127.0(6) . . . . ? O15 Pr O5 C6 -89.9(6) . . . . ? O1 Pr O5 C6 -150.4(6) . . . . ? O25 Pr O5 C4 -25.1(6) . . . . ? O11 Pr O5 C4 126.9(6) . . . . ? O31 Pr O5 C4 -149.9(6) . . . . ? O21 Pr O5 C4 160.4(5) . . . . ? O35 Pr O5 C4 -78.4(6) . . . . ? O15 Pr O5 C4 64.7(6) . . . . ? O1 Pr O5 C4 4.2(5) . . . . ? O25 Pr O11 C12 19.8(6) . . . . ? O31 Pr O11 C12 149.0(5) . . . . ? O21 Pr O11 C12 63.5(5) . . . . ? O35 Pr O11 C12 -179.5(5) . . . . ? O15 Pr O11 C12 -14.7(5) . . . . ? O1 Pr O11 C12 -79.1(5) . . . . ? O5 Pr O11 C12 -132.4(5) . . . . ? Pr O11 C12 C13 8.5(9) . . . . ? Pr O11 C12 C16 -171.3(4) . . . . ? O11 C12 C13 C14 4.0(9) . . . . ? C16 C12 C13 C14 -176.2(6) . . . . ? C12 C13 C14 O15 0.8(9) . . . . ? C12 C13 C14 C17 -178.9(5) . . . . ? C13 C14 O15 Pr -17.6(8) . . . . ? C17 C14 O15 Pr 162.2(4) . . . . ? O25 Pr O15 C14 -138.4(5) . . . . ? O11 Pr O15 C14 18.9(5) . . . . ? O31 Pr O15 C14 -10.8(6) . . . . ? O21 Pr O15 C14 -65.3(5) . . . . ? O35 Pr O15 C14 -175.7(4) . . . . ? O1 Pr O15 C14 138.1(5) . . . . ? O5 Pr O15 C14 84.6(5) . . . . ? O11 C12 C16 F11 59.9(9) . . . . ? C13 C12 C16 F11 -119.9(8) . . . . ? O11 C12 C16 F12 -175.3(7) . . . . ? C13 C12 C16 F12 4.9(10) . . . . ? O11 C12 C16 F13 -56.4(8) . . . . ? C13 C12 C16 F13 123.8(7) . . . . ? O15 C14 C17 F15B 128.7(14) . . . . ? C13 C14 C17 F15B -51.6(15) . . . . ? O15 C14 C17 F15A -67.3(13) . . . . ? C13 C14 C17 F15A 112.4(13) . . . . ? O15 C14 C17 F16B 2.2(17) . . . . ? C13 C14 C17 F16B -178.1(16) . . . . ? O15 C14 C17 F14B -114.2(14) . . . . ? C13 C14 C17 F14B 65.5(15) . . . . ? O15 C14 C17 F14A 53.5(12) . . . . ? C13 C14 C17 F14A -126.8(11) . . . . ? O15 C14 C17 F16A 173.8(12) . . . . ? C13 C14 C17 F16A -6.5(13) . . . . ? O25 Pr O21 C22 26.1(5) . . . . ? O11 Pr O21 C22 -124.9(5) . . . . ? O31 Pr O21 C22 154.0(5) . . . . ? O35 Pr O21 C22 89.1(5) . . . . ? O15 Pr O21 C22 -53.1(5) . . . . ? O1 Pr O21 C22 -14.0(6) . . . . ? O5 Pr O21 C22 -157.8(5) . . . . ? Pr O21 C22 C23 -20.5(9) . . . . ? Pr O21 C22 C26 159.2(5) . . . . ? O21 C22 C23 C24 -1.7(10) . . . . ? C26 C22 C23 C24 178.5(6) . . . . ? C22 C23 C24 O25 2.0(11) . . . . ? C22 C23 C24 C27 -177.3(7) . . . . ? C23 C24 O25 Pr 20.3(10) . . . . ? C27 C24 O25 Pr -160.3(5) . . . . ? O11 Pr O25 C24 20.1(7) . . . . ? O31 Pr O25 C24 -94.9(6) . . . . ? O21 Pr O25 C24 -26.2(6) . . . . ? O35 Pr O25 C24 -148.6(6) . . . . ? O15 Pr O25 C24 53.5(6) . . . . ? O1 Pr O25 C24 130.4(6) . . . . ? O5 Pr O25 C24 156.7(5) . . . . ? O21 C22 C26 F21 -60.2(8) . . . . ? C23 C22 C26 F21 119.5(7) . . . . ? O21 C22 C26 F22 174.8(6) . . . . ? C23 C22 C26 F22 -5.5(10) . . . . ? O21 C22 C26 F23 56.9(9) . . . . ? C23 C22 C26 F23 -123.3(7) . . . . ? O25 C24 C27 F25 -58.9(14) . . . . ? C23 C24 C27 F25 120.6(12) . . . . ? O25 C24 C27 F26 169.2(8) . . . . ? C23 C24 C27 F26 -11.4(12) . . . . ? O25 C24 C27 F24 60.8(9) . . . . ? C23 C24 C27 F24 -119.7(9) . . . . ? O25 Pr O31 C32 -70.9(6) . . . . ? O11 Pr O31 C32 146.5(6) . . . . ? O21 Pr O31 C32 -132.9(6) . . . . ? O35 Pr O31 C32 -14.9(6) . . . . ? O15 Pr O31 C32 174.7(5) . . . . ? O1 Pr O31 C32 37.2(7) . . . . ? O5 Pr O31 C32 69.0(6) . . . . ? Pr O31 C32 C33 15.4(10) . . . . ? Pr O31 C32 C36 -164.9(5) . . . . ? O31 C32 C33 C34 -3.7(10) . . . . ? C36 C32 C33 C34 176.6(6) . . . . ? C32 C33 C34 O35 0.3(10) . . . . ? C32 C33 C34 C37 -180.0(6) . . . . ? C33 C34 O35 Pr -8.0(10) . . . . ? C37 C34 O35 Pr 172.2(5) . . . . ? O25 Pr O35 C34 144.9(6) . . . . ? O11 Pr O35 C34 -22.1(7) . . . . ? O31 Pr O35 C34 11.1(5) . . . . ? O21 Pr O35 C34 84.6(6) . . . . ? O15 Pr O35 C34 -177.7(5) . . . . ? O1 Pr O35 C34 -132.5(6) . . . . ? O5 Pr O35 C34 -68.2(6) . . . . ? O31 C32 C36 F33B 44.0(15) . . . . ? C33 C32 C36 F33B -136.3(14) . . . . ? O31 C32 C36 F31A -28(2) . . . . ? C33 C32 C36 F31A 152(2) . . . . ? O31 C32 C36 F31B 167.7(11) . . . . ? C33 C32 C36 F31B -12.6(13) . . . . ? O31 C32 C36 F33A -164.3(17) . . . . ? C33 C32 C36 F33A 15.5(19) . . . . ? O31 C32 C36 F32B -79.7(10) . . . . ? C33 C32 C36 F32B 100.0(9) . . . . ? O31 C32 C36 F32A 80.9(17) . . . . ? C33 C32 C36 F32A -99.4(17) . . . . ? O35 C34 C37 F36 -177.1(7) . . . . ? C33 C34 C37 F36 3.2(11) . . . . ? O35 C34 C37 F34 58.2(10) . . . . ? C33 C34 C37 F34 -121.6(8) . . . . ? O35 C34 C37 F35 -58.8(8) . . . . ? C33 C34 C37 F35 121.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.738 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.081 # Attachment '- SmCif.txt' data_eh13 _database_code_depnum_ccdc_archive 'CCDC 833379' #TrackingRef '- SmCif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H13 F18 O8 Sm' _chemical_formula_sum 'C19 H13 F18 O8 Sm' _chemical_formula_weight 861.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.451(4) _cell_length_b 15.990(3) _cell_length_c 21.051(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5874(2) _cell_formula_units_Z 8 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 16330 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.949 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3320 _exptl_absorpt_coefficient_mu 2.154 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.493 _exptl_absorpt_correction_T_max 0.740 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ANISO two -CF3 disordered C-F SADI, 52/48 and 52/48 C32-C36 1.51 DFIX ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 30963 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5187 _reflns_number_gt 3493 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V., 1997-2002)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0686P)^2^+10.2929P] 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 0.00015(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5187 _refine_ls_number_parameters 470 _refine_ls_number_restraints 197 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1344 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.010 _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 Sm Sm 0.13402(2) 0.653552(19) 0.240570(15) 0.05856(18) Uani 1 1 d U . . O1 O 0.2752(3) 0.6714(4) 0.2341(2) 0.0903(14) Uani 1 1 d U . . C2 C 0.3280(6) 0.6225(9) 0.2698(5) 0.152(5) Uani 1 1 d U . . H2A H 0.3445 0.5750 0.2445 0.227 Uiso 1 1 calc R . . H2B H 0.3035 0.6028 0.3083 0.227 Uiso 1 1 calc R . . H2C H 0.3722 0.6565 0.2807 0.227 Uiso 1 1 calc R . . C3 C 0.3007(6) 0.7063(7) 0.1760(5) 0.126(3) Uani 1 1 d U . . H3A H 0.3553 0.7199 0.1797 0.151 Uiso 1 1 calc R . . H3B H 0.2951 0.6644 0.1423 0.151 Uiso 1 1 calc R . . C4 C 0.2611(6) 0.7776(6) 0.1587(4) 0.118(3) Uani 1 1 d U . . H4A H 0.2719 0.7907 0.1141 0.142 Uiso 1 1 calc R . . H4B H 0.2786 0.8248 0.1847 0.142 Uiso 1 1 calc R . . O5 O 0.1803(3) 0.7663(3) 0.1671(2) 0.0942(15) Uani 1 1 d U . . C6 C 0.1403(6) 0.8403(5) 0.1518(4) 0.114(3) Uani 1 1 d U . . H6A H 0.1643 0.8875 0.1729 0.171 Uiso 1 1 calc R . . H6B H 0.0875 0.8355 0.1658 0.171 Uiso 1 1 calc R . . H6C H 0.1416 0.8489 0.1062 0.171 Uiso 1 1 calc R . . O11 O 0.0755(3) 0.7780(2) 0.27791(19) 0.0681(12) Uani 1 1 d U . . C12 C 0.0655(4) 0.8110(4) 0.3313(3) 0.0603(15) Uani 1 1 d U . . C13 C 0.0985(4) 0.7871(4) 0.3878(3) 0.0627(15) Uani 1 1 d U . . H13A H 0.0845 0.8155 0.4251 0.075 Uiso 1 1 calc R . . C14 C 0.1511(3) 0.7231(4) 0.3919(3) 0.0565(14) Uani 1 1 d U A . O15 O 0.1758(3) 0.6796(2) 0.34711(19) 0.0632(10) Uani 1 1 d U . . C16 C 0.0124(5) 0.8852(5) 0.3306(4) 0.087(2) Uani 1 1 d U . . C17 C 0.1836(4) 0.7007(4) 0.4573(3) 0.0746(17) Uani 1 1 d DU . . F11 F -0.0537(3) 0.8679(4) 0.3106(5) 0.196(4) Uani 1 1 d U . . F12 F 0.0047(5) 0.9233(4) 0.3839(3) 0.197(3) Uani 1 1 d U . . F13 F 0.0349(4) 0.9429(3) 0.2916(4) 0.162(3) Uani 1 1 d U . . F14A F 0.2575(6) 0.7065(13) 0.4559(10) 0.134(7) Uani 0.52 1 d PDU A 1 F15A F 0.1661(12) 0.6254(7) 0.4742(9) 0.123(6) Uani 0.52 1 d PDU A 1 F16A F 0.1612(14) 0.7491(14) 0.5024(10) 0.135(8) Uani 0.52 1 d PDU A 1 F14B F 0.1304(9) 0.6626(15) 0.4879(9) 0.142(8) Uani 0.48 1 d PDU A 2 F16B F 0.2418(13) 0.6513(16) 0.4562(8) 0.159(10) Uani 0.48 1 d PDU A 2 F15B F 0.1989(18) 0.7640(15) 0.4922(13) 0.146(9) Uani 0.48 1 d PDU A 2 O21 O 0.0339(3) 0.5977(3) 0.3042(2) 0.0716(11) Uani 1 1 d U . . C22 C 0.0340(4) 0.5455(4) 0.3492(3) 0.0740(16) Uani 1 1 d U . . C23 C 0.0905(5) 0.4879(4) 0.3639(4) 0.0844(19) Uani 1 1 d U . . H23A H 0.0848 0.4539 0.4000 0.101 Uiso 1 1 calc R . . C24 C 0.1548(5) 0.4795(4) 0.3266(4) 0.0798(19) Uani 1 1 d U . . O25 O 0.1732(3) 0.5212(3) 0.2791(2) 0.0752(12) Uani 1 1 d U . . C26 C -0.0366(6) 0.5503(6) 0.3923(4) 0.100(2) Uani 1 1 d U . . C27 C 0.2104(8) 0.4112(6) 0.3442(5) 0.124(3) Uani 1 1 d U . . F21 F -0.0449(4) 0.6230(4) 0.4166(3) 0.161(3) Uani 1 1 d U . . F22 F -0.0378(3) 0.4918(4) 0.4360(3) 0.157(2) Uani 1 1 d U . . F23 F -0.0993(3) 0.5359(4) 0.3585(3) 0.1255(17) Uani 1 1 d U . . F24 F 0.2804(5) 0.4452(6) 0.3523(6) 0.255(5) Uani 1 1 d U . . F25 F 0.2197(8) 0.3581(6) 0.3062(4) 0.320(7) Uani 1 1 d U . . F26 F 0.2039(4) 0.3781(4) 0.3994(3) 0.158(2) Uani 1 1 d U . . O31 O 0.0335(3) 0.6667(3) 0.1656(2) 0.0798(13) Uani 1 1 d U . . C32 C 0.0249(4) 0.6510(5) 0.1076(3) 0.0750(17) Uani 1 1 d DU B . C33 C 0.0728(4) 0.6014(4) 0.0703(3) 0.0739(17) Uani 1 1 d U . . H33A H 0.0595 0.5915 0.0277 0.089 Uiso 1 1 calc R . . C34 C 0.1382(4) 0.5669(4) 0.0940(3) 0.0685(16) Uani 1 1 d U . . O35 O 0.1650(3) 0.5731(3) 0.1486(2) 0.0735(12) Uani 1 1 d U . . C36 C -0.0458(5) 0.6887(8) 0.0777(4) 0.128(3) Uani 1 1 d DU . . C37 C 0.1853(7) 0.5140(5) 0.0490(4) 0.097(2) Uani 1 1 d U . . F31A F -0.0655(13) 0.7598(13) 0.1010(12) 0.207(12) Uani 0.52 1 d PDU B 1 F32A F -0.1017(7) 0.6330(12) 0.0908(7) 0.178(7) Uani 0.52 1 d PDU B 1 F33A F -0.0415(14) 0.6929(18) 0.0160(6) 0.145(8) Uani 0.52 1 d PDU B 1 F31B F -0.0573(17) 0.664(2) 0.0195(7) 0.191(12) Uani 0.48 1 d PDU B 2 F32B F -0.0280(12) 0.7707(10) 0.0683(13) 0.180(9) Uani 0.48 1 d PDU B 2 F33B F -0.1051(15) 0.704(3) 0.1126(15) 0.258(17) Uani 0.48 1 d PDU B 2 F34 F 0.1896(5) 0.4372(4) 0.0686(3) 0.194(3) Uani 1 1 d U . . F35 F 0.2559(4) 0.5396(5) 0.0460(3) 0.188(3) Uani 1 1 d U . . F36 F 0.1626(4) 0.5112(4) -0.0086(2) 0.162(3) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm 0.0725(3) 0.0583(2) 0.0449(2) -0.00460(13) -0.00181(16) 0.00855(15) O1 0.075(3) 0.134(4) 0.062(3) -0.011(3) 0.002(2) -0.010(3) C2 0.075(6) 0.281(15) 0.098(7) 0.013(7) 0.008(5) 0.041(8) C3 0.101(6) 0.143(8) 0.133(8) 0.017(6) 0.045(6) -0.005(5) C4 0.128(6) 0.125(7) 0.102(6) 0.003(5) 0.027(6) -0.031(5) O5 0.118(4) 0.075(3) 0.090(3) 0.009(2) 0.032(3) 0.003(3) C6 0.197(9) 0.076(5) 0.068(5) 0.015(4) 0.024(6) 0.021(5) O11 0.089(3) 0.061(2) 0.054(2) -0.0013(18) 0.000(2) 0.020(2) C12 0.063(4) 0.053(3) 0.065(4) -0.003(3) 0.009(3) 0.008(3) C13 0.073(4) 0.065(4) 0.049(3) -0.013(3) 0.008(3) 0.004(3) C14 0.065(4) 0.061(3) 0.043(3) 0.000(2) 0.005(3) -0.006(3) O15 0.073(3) 0.066(2) 0.051(2) -0.0063(18) -0.002(2) 0.013(2) C16 0.097(6) 0.074(5) 0.089(5) -0.013(4) -0.003(4) 0.023(4) C17 0.084(5) 0.088(4) 0.052(4) -0.002(3) 0.002(3) 0.007(4) F11 0.084(4) 0.126(5) 0.380(12) -0.056(6) -0.046(5) 0.045(3) F12 0.286(9) 0.178(6) 0.128(4) -0.050(4) -0.021(5) 0.161(6) F13 0.182(6) 0.093(4) 0.210(6) 0.050(4) 0.042(5) 0.060(3) F14A 0.079(6) 0.227(19) 0.096(9) 0.055(13) -0.022(6) 0.012(8) F15A 0.191(16) 0.090(6) 0.087(11) 0.028(6) -0.044(12) -0.013(9) F16A 0.20(2) 0.150(13) 0.056(6) -0.031(10) -0.033(11) 0.093(14) F14B 0.145(12) 0.21(2) 0.074(10) 0.073(14) -0.008(8) -0.045(13) F16B 0.185(16) 0.24(2) 0.054(7) 0.016(13) -0.003(11) 0.132(16) F15B 0.21(2) 0.131(10) 0.100(15) -0.028(8) -0.068(15) -0.013(12) O21 0.074(3) 0.072(3) 0.068(3) 0.010(2) -0.003(2) 0.003(2) C22 0.087(4) 0.077(4) 0.058(4) 0.003(3) -0.007(3) -0.012(3) C23 0.104(5) 0.075(4) 0.074(5) 0.020(4) -0.010(4) -0.004(4) C24 0.106(5) 0.064(4) 0.069(5) 0.001(3) -0.014(4) 0.012(4) O25 0.100(4) 0.066(3) 0.059(3) -0.0052(19) -0.005(2) 0.024(2) C26 0.102(6) 0.118(6) 0.080(6) 0.016(4) 0.010(4) -0.014(5) C27 0.174(8) 0.108(7) 0.090(6) 0.020(4) -0.011(7) 0.057(6) F21 0.148(5) 0.163(5) 0.170(6) -0.064(4) 0.084(5) -0.044(4) F22 0.131(5) 0.216(6) 0.123(4) 0.080(4) 0.028(3) -0.010(4) F23 0.092(3) 0.144(4) 0.141(5) 0.024(3) 0.000(3) -0.021(3) F24 0.142(6) 0.221(8) 0.403(14) 0.156(7) -0.003(7) 0.075(5) F25 0.594(18) 0.220(7) 0.146(6) -0.086(6) -0.143(9) 0.297(10) F26 0.187(6) 0.150(5) 0.136(5) 0.055(4) -0.025(4) 0.055(4) O31 0.080(3) 0.104(3) 0.056(3) -0.002(2) -0.003(2) 0.012(3) C32 0.066(4) 0.106(5) 0.053(4) 0.014(3) -0.007(3) -0.014(3) C33 0.093(5) 0.081(5) 0.048(3) 0.008(3) -0.008(3) -0.011(3) C34 0.102(5) 0.056(3) 0.048(3) -0.003(3) 0.009(3) -0.008(3) O35 0.098(3) 0.074(3) 0.048(2) -0.0107(19) -0.004(2) 0.014(2) C36 0.095(6) 0.217(9) 0.071(5) 0.014(6) -0.010(5) 0.031(6) C37 0.148(7) 0.093(5) 0.051(4) -0.009(4) 0.007(5) 0.024(5) F31A 0.16(3) 0.306(17) 0.16(2) -0.08(2) -0.075(17) 0.147(14) F32A 0.048(6) 0.39(2) 0.100(9) -0.006(12) 0.008(6) -0.010(10) F33A 0.138(16) 0.226(18) 0.072(6) 0.037(8) -0.003(7) 0.076(15) F31B 0.131(14) 0.33(3) 0.106(10) 0.008(13) -0.081(11) -0.027(16) F32B 0.147(17) 0.189(10) 0.21(2) 0.026(12) -0.037(14) 0.099(10) F33B 0.112(17) 0.50(5) 0.159(17) 0.11(2) 0.034(15) 0.12(2) F34 0.371(10) 0.101(3) 0.110(4) 0.013(3) 0.074(6) 0.097(5) F35 0.143(5) 0.261(7) 0.159(6) -0.108(6) 0.052(4) 0.007(5) F36 0.258(7) 0.174(5) 0.054(3) -0.035(3) -0.008(4) 0.074(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 Sm O25 2.368(4) . ? Sm O31 2.369(5) . ? Sm O11 2.371(4) . ? Sm O21 2.375(4) . ? Sm O35 2.386(4) . ? Sm O15 2.395(4) . ? Sm O1 2.483(5) . ? Sm O5 2.508(5) . ? O1 C3 1.417(10) . ? O1 C2 1.423(11) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.380(12) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 O5 1.433(11) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? O5 C6 1.412(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? O11 C12 1.254(7) . ? C12 C13 1.375(8) . ? C12 C16 1.506(10) . ? C13 C14 1.378(8) . ? C13 H13A 0.9400 . ? C14 O15 1.249(7) . ? C14 C17 1.532(9) . ? C16 F11 1.258(10) . ? C16 F12 1.283(9) . ? C16 F13 1.295(10) . ? C17 F15B 1.279(13) . ? C17 F14B 1.284(12) . ? C17 F16B 1.286(12) . ? C17 F16A 1.287(12) . ? C17 F15A 1.291(11) . ? C17 F14A 1.293(11) . ? O21 C22 1.264(7) . ? C22 C23 1.383(10) . ? C22 C26 1.532(11) . ? C23 C24 1.376(11) . ? C23 H23A 0.9400 . ? C24 O25 1.243(8) . ? C24 C27 1.508(12) . ? C26 F21 1.278(10) . ? C26 F22 1.312(9) . ? C26 F23 1.325(10) . ? C27 F25 1.177(11) . ? C27 F26 1.281(10) . ? C27 F24 1.349(14) . ? O31 C32 1.256(8) . ? C32 C33 1.394(10) . ? C32 C36 1.510(8) . ? C33 C34 1.363(10) . ? C33 H33A 0.9400 . ? C34 O35 1.246(7) . ? C34 C37 1.512(10) . ? C36 F31A 1.284(13) . ? C36 F33B 1.293(14) . ? C36 F33A 1.304(13) . ? C36 F31B 1.305(14) . ? C36 F32A 1.349(13) . ? C36 F32B 1.362(14) . ? C37 F36 1.277(9) . ? C37 F34 1.298(9) . ? C37 F35 1.300(11) . ? 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 O25 Sm O31 121.44(17) . . ? O25 Sm O11 139.57(15) . . ? O31 Sm O11 80.04(15) . . ? O25 Sm O21 71.53(16) . . ? O31 Sm O21 82.17(16) . . ? O11 Sm O21 79.17(15) . . ? O25 Sm O35 74.36(15) . . ? O31 Sm O35 71.09(16) . . ? O11 Sm O35 145.00(14) . . ? O21 Sm O35 114.90(16) . . ? O25 Sm O15 75.32(14) . . ? O31 Sm O15 146.47(15) . . ? O11 Sm O15 71.01(14) . . ? O21 Sm O15 76.21(15) . . ? O35 Sm O15 141.66(15) . . ? O25 Sm O1 80.49(19) . . ? O31 Sm O1 133.49(17) . . ? O11 Sm O1 110.42(17) . . ? O21 Sm O1 143.47(16) . . ? O35 Sm O1 78.04(16) . . ? O15 Sm O1 74.29(15) . . ? O25 Sm O5 139.51(18) . . ? O31 Sm O5 76.37(19) . . ? O11 Sm O5 74.92(15) . . ? O21 Sm O5 148.70(17) . . ? O35 Sm O5 79.31(16) . . ? O15 Sm O5 110.74(17) . . ? O1 Sm O5 64.17(19) . . ? C3 O1 C2 117.9(7) . . ? C3 O1 Sm 113.8(5) . . ? C2 O1 Sm 123.5(6) . . ? O1 C2 H2A 109.5 . . ? O1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 O1 113.3(8) . . ? C4 C3 H3A 108.9 . . ? O1 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? O1 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C3 C4 O5 110.8(8) . . ? C3 C4 H4A 109.5 . . ? O5 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? O5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C6 O5 C4 110.6(7) . . ? C6 O5 Sm 125.8(5) . . ? C4 O5 Sm 118.9(5) . . ? O5 C6 H6A 109.5 . . ? O5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 O11 Sm 135.3(4) . . ? O11 C12 C13 126.9(6) . . ? O11 C12 C16 114.1(6) . . ? C13 C12 C16 119.1(6) . . ? C12 C13 C14 122.7(5) . . ? C12 C13 H13A 118.7 . . ? C14 C13 H13A 118.7 . . ? O15 C14 C13 126.6(6) . . ? O15 C14 C17 114.8(5) . . ? C13 C14 C17 118.5(5) . . ? C14 O15 Sm 134.4(4) . . ? F11 C16 F12 107.5(9) . . ? F11 C16 F13 102.9(8) . . ? F12 C16 F13 104.3(8) . . ? F11 C16 C12 113.2(7) . . ? F12 C16 C12 115.4(7) . . ? F13 C16 C12 112.4(7) . . ? F15B C17 F14B 103.8(17) . . ? F15B C17 F16B 109.4(18) . . ? F14B C17 F16B 106.7(14) . . ? F15B C17 F16A 33.1(18) . . ? F14B C17 F16A 72.3(15) . . ? F16B C17 F16A 128.5(16) . . ? F15B C17 F15A 129.0(17) . . ? F14B C17 F15A 41.3(10) . . ? F16B C17 F15A 67.6(12) . . ? F16A C17 F15A 106.6(15) . . ? F15B C17 F14A 75.5(16) . . ? F14B C17 F14A 140.1(12) . . ? F16B C17 F14A 42.0(13) . . ? F16A C17 F14A 106.1(15) . . ? F15A C17 F14A 108.0(12) . . ? F15B C17 C14 114.0(16) . . ? F14B C17 C14 107.1(10) . . ? F16B C17 C14 114.9(9) . . ? F16A C17 C14 114.2(12) . . ? F15A C17 C14 112.2(9) . . ? F14A C17 C14 109.4(9) . . ? C22 O21 Sm 132.1(5) . . ? O21 C22 C23 127.5(7) . . ? O21 C22 C26 114.2(7) . . ? C23 C22 C26 118.3(7) . . ? C24 C23 C22 121.2(7) . . ? C24 C23 H23A 119.4 . . ? C22 C23 H23A 119.4 . . ? O25 C24 C23 128.2(7) . . ? O25 C24 C27 114.7(8) . . ? C23 C24 C27 117.1(8) . . ? C24 O25 Sm 132.8(5) . . ? F21 C26 F22 111.5(9) . . ? F21 C26 F23 106.2(9) . . ? F22 C26 F23 103.8(8) . . ? F21 C26 C22 112.0(7) . . ? F22 C26 C22 113.0(8) . . ? F23 C26 C22 109.7(7) . . ? F25 C27 F26 109.3(10) . . ? F25 C27 F24 104.6(13) . . ? F26 C27 F24 97.6(10) . . ? F25 C27 C24 116.4(9) . . ? F26 C27 C24 117.7(10) . . ? F24 C27 C24 108.8(9) . . ? C32 O31 Sm 135.9(5) . . ? O31 C32 C33 126.2(6) . . ? O31 C32 C36 115.0(7) . . ? C33 C32 C36 118.8(7) . . ? C34 C33 C32 121.8(6) . . ? C34 C33 H33A 119.1 . . ? C32 C33 H33A 119.1 . . ? O35 C34 C33 128.3(6) . . ? O35 C34 C37 114.7(7) . . ? C33 C34 C37 116.9(6) . . ? C34 O35 Sm 135.0(4) . . ? F31A C36 F33B 53.1(17) . . ? F31A C36 F33A 110.4(18) . . ? F33B C36 F33A 127(2) . . ? F31A C36 F31B 126(2) . . ? F33B C36 F31B 118(2) . . ? F33A C36 F31B 24(3) . . ? F31A C36 F32A 108.2(16) . . ? F33B C36 F32A 55(2) . . ? F33A C36 F32A 106.2(17) . . ? F31B C36 F32A 83.1(17) . . ? F31A C36 F32B 42.7(14) . . ? F33B C36 F32B 95(2) . . ? F33A C36 F32B 78.0(17) . . ? F31B C36 F32B 101(2) . . ? F32A C36 F32B 146.0(14) . . ? F31A C36 C32 114.4(12) . . ? F33B C36 C32 119.6(17) . . ? F33A C36 C32 112.9(12) . . ? F31B C36 C32 113.3(15) . . ? F32A C36 C32 104.0(10) . . ? F32B C36 C32 105.0(12) . . ? F36 C37 F34 106.6(7) . . ? F36 C37 F35 105.0(8) . . ? F34 C37 F35 105.0(9) . . ? F36 C37 C34 116.5(8) . . ? F34 C37 C34 111.2(7) . . ? F35 C37 C34 111.7(7) . . ? 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 O25 Sm O1 C3 133.8(6) . . . . ? O31 Sm O1 C3 9.0(7) . . . . ? O11 Sm O1 C3 -86.7(6) . . . . ? O21 Sm O1 C3 173.8(5) . . . . ? O35 Sm O1 C3 57.9(6) . . . . ? O15 Sm O1 C3 -148.9(6) . . . . ? O5 Sm O1 C3 -25.9(6) . . . . ? O25 Sm O1 C2 -21.1(7) . . . . ? O31 Sm O1 C2 -145.8(7) . . . . ? O11 Sm O1 C2 118.5(7) . . . . ? O21 Sm O1 C2 19.0(8) . . . . ? O35 Sm O1 C2 -96.9(7) . . . . ? O15 Sm O1 C2 56.2(7) . . . . ? O5 Sm O1 C2 179.3(8) . . . . ? C2 O1 C3 C4 -154.2(10) . . . . ? Sm O1 C3 C4 49.4(11) . . . . ? O1 C3 C4 O5 -45.1(12) . . . . ? C3 C4 O5 C6 177.7(8) . . . . ? C3 C4 O5 Sm 20.5(11) . . . . ? O25 Sm O5 C6 177.6(6) . . . . ? O31 Sm O5 C6 54.7(6) . . . . ? O11 Sm O5 C6 -28.5(6) . . . . ? O21 Sm O5 C6 6.7(8) . . . . ? O35 Sm O5 C6 127.6(6) . . . . ? O15 Sm O5 C6 -90.9(6) . . . . ? O1 Sm O5 C6 -150.6(7) . . . . ? O25 Sm O5 C4 -28.9(7) . . . . ? O31 Sm O5 C4 -151.8(6) . . . . ? O11 Sm O5 C4 125.0(6) . . . . ? O21 Sm O5 C4 160.2(5) . . . . ? O35 Sm O5 C4 -78.9(6) . . . . ? O15 Sm O5 C4 62.6(6) . . . . ? O1 Sm O5 C4 2.9(5) . . . . ? O25 Sm O11 C12 19.1(7) . . . . ? O31 Sm O11 C12 146.7(6) . . . . ? O21 Sm O11 C12 62.9(6) . . . . ? O35 Sm O11 C12 -178.8(5) . . . . ? O15 Sm O11 C12 -16.1(6) . . . . ? O1 Sm O11 C12 -80.4(6) . . . . ? O5 Sm O11 C12 -134.9(6) . . . . ? Sm O11 C12 C13 10.8(11) . . . . ? Sm O11 C12 C16 -170.2(5) . . . . ? O11 C12 C13 C14 2.8(11) . . . . ? C16 C12 C13 C14 -176.1(7) . . . . ? C12 C13 C14 O15 0.2(11) . . . . ? C12 C13 C14 C17 -179.2(6) . . . . ? C13 C14 O15 Sm -16.6(10) . . . . ? C17 C14 O15 Sm 162.8(4) . . . . ? O25 Sm O15 C14 -138.3(6) . . . . ? O31 Sm O15 C14 -12.8(7) . . . . ? O11 Sm O15 C14 19.0(5) . . . . ? O21 Sm O15 C14 -64.1(5) . . . . ? O35 Sm O15 C14 -177.0(5) . . . . ? O1 Sm O15 C14 137.7(6) . . . . ? O5 Sm O15 C14 83.8(6) . . . . ? O11 C12 C16 F11 59.5(10) . . . . ? C13 C12 C16 F11 -121.5(9) . . . . ? O11 C12 C16 F12 -176.0(8) . . . . ? C13 C12 C16 F12 3.0(12) . . . . ? O11 C12 C16 F13 -56.6(10) . . . . ? C13 C12 C16 F13 122.4(8) . . . . ? O15 C14 C17 F15B 139.7(16) . . . . ? C13 C14 C17 F15B -40.7(17) . . . . ? O15 C14 C17 F14B -106.1(14) . . . . ? C13 C14 C17 F14B 73.5(14) . . . . ? O15 C14 C17 F16B 12.2(18) . . . . ? C13 C14 C17 F16B -168.2(17) . . . . ? O15 C14 C17 F16A 176.1(15) . . . . ? C13 C14 C17 F16A -4.4(17) . . . . ? O15 C14 C17 F15A -62.4(13) . . . . ? C13 C14 C17 F15A 117.1(13) . . . . ? O15 C14 C17 F14A 57.4(13) . . . . ? C13 C14 C17 F14A -123.0(13) . . . . ? O25 Sm O21 C22 25.4(5) . . . . ? O31 Sm O21 C22 152.3(6) . . . . ? O11 Sm O21 C22 -126.4(6) . . . . ? O35 Sm O21 C22 87.5(6) . . . . ? O15 Sm O21 C22 -53.5(6) . . . . ? O1 Sm O21 C22 -16.6(7) . . . . ? O5 Sm O21 C22 -160.8(5) . . . . ? Sm O21 C22 C23 -19.4(10) . . . . ? Sm O21 C22 C26 158.9(5) . . . . ? O21 C22 C23 C24 -2.8(12) . . . . ? C26 C22 C23 C24 179.0(7) . . . . ? C22 C23 C24 O25 3.3(13) . . . . ? C22 C23 C24 C27 -176.1(8) . . . . ? C23 C24 O25 Sm 18.7(12) . . . . ? C27 C24 O25 Sm -162.0(6) . . . . ? O31 Sm O25 C24 -93.3(7) . . . . ? O11 Sm O25 C24 20.5(8) . . . . ? O21 Sm O25 C24 -25.2(6) . . . . ? O35 Sm O25 C24 -148.9(7) . . . . ? O15 Sm O25 C24 54.8(7) . . . . ? O1 Sm O25 C24 131.0(7) . . . . ? O5 Sm O25 C24 159.7(6) . . . . ? O21 C22 C26 F21 -57.5(10) . . . . ? C23 C22 C26 F21 120.9(9) . . . . ? O21 C22 C26 F22 175.5(7) . . . . ? C23 C22 C26 F22 -6.1(12) . . . . ? O21 C22 C26 F23 60.1(9) . . . . ? C23 C22 C26 F23 -121.4(8) . . . . ? O25 C24 C27 F25 -62.0(16) . . . . ? C23 C24 C27 F25 117.5(14) . . . . ? O25 C24 C27 F26 165.4(10) . . . . ? C23 C24 C27 F26 -15.2(15) . . . . ? O25 C24 C27 F24 55.7(12) . . . . ? C23 C24 C27 F24 -124.8(10) . . . . ? O25 Sm O31 C32 -71.8(7) . . . . ? O11 Sm O31 C32 145.2(7) . . . . ? O21 Sm O31 C32 -134.5(7) . . . . ? O35 Sm O31 C32 -14.7(6) . . . . ? O15 Sm O31 C32 175.6(6) . . . . ? O1 Sm O31 C32 36.4(7) . . . . ? O5 Sm O31 C32 68.5(6) . . . . ? Sm O31 C32 C33 14.9(11) . . . . ? Sm O31 C32 C36 -166.9(6) . . . . ? O31 C32 C33 C34 -3.2(11) . . . . ? C36 C32 C33 C34 178.7(8) . . . . ? C32 C33 C34 O35 -0.2(11) . . . . ? C32 C33 C34 C37 179.8(7) . . . . ? C33 C34 O35 Sm -7.7(11) . . . . ? C37 C34 O35 Sm 172.3(5) . . . . ? O25 Sm O35 C34 143.0(6) . . . . ? O31 Sm O35 C34 11.1(6) . . . . ? O11 Sm O35 C34 -25.0(8) . . . . ? O21 Sm O35 C34 82.5(6) . . . . ? O15 Sm O35 C34 -178.1(5) . . . . ? O1 Sm O35 C34 -133.6(6) . . . . ? O5 Sm O35 C34 -68.0(6) . . . . ? O31 C32 C36 F31A 33(2) . . . . ? C33 C32 C36 F31A -148.4(18) . . . . ? O31 C32 C36 F33B -27(3) . . . . ? C33 C32 C36 F33B 152(3) . . . . ? O31 C32 C36 F33A 160.8(17) . . . . ? C33 C32 C36 F33A -20.9(19) . . . . ? O31 C32 C36 F31B -173.0(18) . . . . ? C33 C32 C36 F31B 5(2) . . . . ? O31 C32 C36 F32A -84.6(11) . . . . ? C33 C32 C36 F32A 93.8(10) . . . . ? O31 C32 C36 F32B 77.7(14) . . . . ? C33 C32 C36 F32B -103.9(14) . . . . ? O35 C34 C37 F36 -175.1(8) . . . . ? C33 C34 C37 F36 5.0(12) . . . . ? O35 C34 C37 F34 62.4(11) . . . . ? C33 C34 C37 F34 -117.5(9) . . . . ? O35 C34 C37 F35 -54.5(10) . . . . ? C33 C34 C37 F35 125.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.975 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.091 # Attachment '- TbCif.txt' data_ef648 _database_code_depnum_ccdc_archive 'CCDC 833380' #TrackingRef '- TbCif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H13 F18 O8 Tb' _chemical_formula_sum 'C19 H13 F18 O8 Tb' _chemical_formula_weight 870.21 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' F F 0.0171 0.0103 '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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.646(4) _cell_length_b 15.919(3) _cell_length_c 20.892(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5868(2) _cell_formula_units_Z 8 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 19283 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.970 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 2.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.564 _exptl_absorpt_correction_T_max 0.686 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ANISO two -CF3 disordered C-F SADI, 42/58 and 75/25 C32-C36 1.51 DFIX ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 36842 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5181 _reflns_number_gt 3387 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V., 1997-2002)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0698P)^2^+10.7864P] 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 0.00014(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5181 _refine_ls_number_parameters 470 _refine_ls_number_restraints 197 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.025 _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 Tb Tb 0.13347(2) 0.65574(2) 0.241060(15) 0.06090(18) Uani 1 1 d U . . O1 O 0.2705(3) 0.6745(4) 0.2344(2) 0.0942(16) Uani 1 1 d U . . C2 C 0.3231(6) 0.6230(9) 0.2678(5) 0.148(5) Uani 1 1 d U . . H2A H 0.3438 0.5813 0.2389 0.222 Uiso 1 1 calc R . . H2B H 0.2975 0.5951 0.3030 0.222 Uiso 1 1 calc R . . H2C H 0.3639 0.6576 0.2845 0.222 Uiso 1 1 calc R . . C3 C 0.2965(6) 0.7083(7) 0.1752(5) 0.121(3) Uani 1 1 d U . . H3A H 0.3506 0.7214 0.1785 0.146 Uiso 1 1 calc R . . H3B H 0.2899 0.6665 0.1412 0.146 Uiso 1 1 calc R . . C4 C 0.2564(7) 0.7814(7) 0.1593(5) 0.126(3) Uani 1 1 d U . . H4A H 0.2674 0.7973 0.1150 0.151 Uiso 1 1 calc R . . H4B H 0.2724 0.8276 0.1872 0.151 Uiso 1 1 calc R . . O5 O 0.1755(4) 0.7672(4) 0.1667(3) 0.0998(16) Uani 1 1 d U . . C6 C 0.1335(7) 0.8394(6) 0.1517(5) 0.132(4) Uani 1 1 d U . . H6A H 0.1478 0.8847 0.1803 0.197 Uiso 1 1 calc R . . H6B H 0.0799 0.8276 0.1565 0.197 Uiso 1 1 calc R . . H6C H 0.1438 0.8558 0.1078 0.197 Uiso 1 1 calc R . . O11 O 0.0764(3) 0.7792(3) 0.2777(2) 0.0716(13) Uani 1 1 d U . . C12 C 0.0663(4) 0.8118(4) 0.3318(3) 0.0631(16) Uani 1 1 d U . . C13 C 0.0999(4) 0.7882(4) 0.3888(3) 0.0646(16) Uani 1 1 d U . . H13A H 0.0862 0.8163 0.4266 0.078 Uiso 1 1 calc R . . C14 C 0.1528(4) 0.7251(4) 0.3918(3) 0.0601(15) Uani 1 1 d U A . O15 O 0.1765(3) 0.6804(3) 0.3464(2) 0.0676(12) Uani 1 1 d U . . C16 C 0.0136(6) 0.8861(6) 0.3309(4) 0.091(2) Uani 1 1 d U . . C17 C 0.1868(4) 0.7021(5) 0.4566(3) 0.0773(19) Uani 1 1 d DU . . F11 F -0.0527(4) 0.8669(5) 0.3119(5) 0.203(4) Uani 1 1 d U . . F12 F 0.0050(5) 0.9228(5) 0.3854(3) 0.199(4) Uani 1 1 d U . . F13 F 0.0343(4) 0.9442(4) 0.2923(4) 0.173(3) Uani 1 1 d U . . F14A F 0.2578(9) 0.7207(19) 0.4586(16) 0.151(11) Uani 0.42 1 d PDU A 1 F15A F 0.1799(18) 0.6236(10) 0.4710(15) 0.127(9) Uani 0.42 1 d PDU A 1 F16A F 0.160(2) 0.742(2) 0.5051(12) 0.165(14) Uani 0.42 1 d PDU A 1 F14B F 0.1425(11) 0.6481(12) 0.4842(11) 0.147(8) Uani 0.58 1 d PDU A 2 F15B F 0.1871(14) 0.7661(11) 0.4945(8) 0.124(7) Uani 0.58 1 d PDU A 2 F16B F 0.2534(9) 0.6705(16) 0.4525(9) 0.157(9) Uani 0.58 1 d PDU A 2 O21 O 0.0350(3) 0.6022(3) 0.3036(2) 0.0737(12) Uani 1 1 d U . . C22 C 0.0347(5) 0.5508(5) 0.3492(3) 0.0765(18) Uani 1 1 d U . . C23 C 0.0897(5) 0.4923(5) 0.3643(4) 0.087(2) Uani 1 1 d U . . H23A H 0.0840 0.4592 0.4012 0.105 Uiso 1 1 calc R . . C24 C 0.1523(5) 0.4818(5) 0.3263(4) 0.080(2) Uani 1 1 d U . . O25 O 0.1716(3) 0.5244(3) 0.2789(2) 0.0784(13) Uani 1 1 d U . . C26 C -0.0357(6) 0.5556(8) 0.3919(5) 0.105(3) Uani 1 1 d U . . C27 C 0.2068(8) 0.4130(8) 0.3448(5) 0.129(3) Uani 1 1 d U . . F21 F -0.0444(4) 0.6292(5) 0.4153(4) 0.187(4) Uani 1 1 d U . . F22 F -0.0372(4) 0.4978(5) 0.4369(3) 0.174(3) Uani 1 1 d U . . F23 F -0.0973(3) 0.5398(4) 0.3583(3) 0.1303(19) Uani 1 1 d U . . F24 F 0.2755(5) 0.4404(7) 0.3441(7) 0.300(7) Uani 1 1 d U . . F25 F 0.2071(10) 0.3541(6) 0.3077(4) 0.309(7) Uani 1 1 d U . . F26 F 0.2015(4) 0.3812(4) 0.3994(3) 0.161(3) Uani 1 1 d U . . O31 O 0.0346(3) 0.6661(3) 0.1680(2) 0.0823(14) Uani 1 1 d U . . C32 C 0.0254(4) 0.6493(5) 0.1097(4) 0.078(2) Uani 1 1 d DU B . C33 C 0.0734(4) 0.6010(5) 0.0720(3) 0.0732(18) Uani 1 1 d U . . H33A H 0.0601 0.5908 0.0292 0.088 Uiso 1 1 calc R . . C34 C 0.1396(4) 0.5676(4) 0.0952(3) 0.0666(17) Uani 1 1 d U . . O35 O 0.1665(3) 0.5767(3) 0.1507(2) 0.0725(12) Uani 1 1 d U . . C36 C -0.0472(6) 0.6819(8) 0.0804(4) 0.138(4) Uani 1 1 d DU . . C37 C 0.1887(7) 0.5167(6) 0.0502(4) 0.100(3) Uani 1 1 d U . . F31A F -0.0607(13) 0.7573(11) 0.0982(11) 0.264(12) Uani 0.75 1 d PDU B 1 F32A F -0.1036(5) 0.6326(12) 0.0966(6) 0.227(7) Uani 0.75 1 d PDU B 1 F33A F -0.0467(11) 0.6795(13) 0.0188(4) 0.176(6) Uani 0.75 1 d PDU B 1 F31B F -0.064(3) 0.651(5) 0.0253(18) 0.27(3) Uani 0.25 1 d PDU B 2 F32B F -0.028(2) 0.7556(16) 0.056(2) 0.176(15) Uani 0.25 1 d PDU B 2 F33B F -0.090(3) 0.720(3) 0.120(3) 0.149(13) Uani 0.25 1 d PDU B 2 F34 F 0.1884(6) 0.4379(4) 0.0687(3) 0.193(4) Uani 1 1 d U . . F35 F 0.2574(4) 0.5402(6) 0.0499(4) 0.195(4) Uani 1 1 d U . . F36 F 0.1662(4) 0.5150(4) -0.0082(2) 0.154(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb 0.0785(3) 0.0589(3) 0.0454(2) -0.00484(14) -0.00104(15) 0.00933(16) O1 0.086(3) 0.139(5) 0.057(3) -0.016(3) 0.006(2) -0.015(3) C2 0.080(6) 0.264(15) 0.099(7) 0.004(7) 0.002(5) 0.032(8) C3 0.113(7) 0.142(9) 0.109(7) -0.002(6) 0.034(6) -0.032(6) C4 0.158(7) 0.123(8) 0.097(7) 0.002(6) 0.018(7) -0.054(6) O5 0.145(5) 0.079(3) 0.076(3) 0.008(3) 0.029(3) 0.002(3) C6 0.240(12) 0.080(6) 0.075(6) 0.016(5) 0.031(7) 0.029(7) O11 0.096(4) 0.067(3) 0.052(2) 0.000(2) -0.002(2) 0.019(3) C12 0.073(4) 0.049(4) 0.067(4) -0.002(3) 0.008(3) 0.008(3) C13 0.075(4) 0.068(4) 0.052(3) -0.010(3) 0.008(3) 0.005(3) C14 0.068(4) 0.066(4) 0.046(3) -0.005(3) 0.004(3) -0.002(3) O15 0.080(3) 0.072(3) 0.051(2) -0.008(2) 0.001(2) 0.018(2) C16 0.103(6) 0.076(6) 0.093(6) -0.006(4) 0.003(5) 0.032(4) C17 0.092(5) 0.090(5) 0.050(4) -0.005(3) 0.001(4) 0.012(4) F11 0.090(4) 0.140(6) 0.378(13) -0.057(6) -0.044(6) 0.049(4) F12 0.289(9) 0.180(6) 0.127(5) -0.051(4) -0.015(5) 0.165(7) F13 0.215(7) 0.092(4) 0.211(7) 0.050(5) 0.044(6) 0.069(4) F14A 0.102(9) 0.22(3) 0.129(19) 0.069(18) -0.053(10) -0.026(13) F15A 0.20(2) 0.087(7) 0.096(17) 0.022(8) -0.062(17) 0.006(11) F16A 0.28(3) 0.18(2) 0.041(6) 0.002(11) 0.018(13) 0.12(2) F14B 0.191(16) 0.177(15) 0.073(9) 0.055(12) -0.025(11) -0.055(13) F15B 0.182(14) 0.117(9) 0.074(10) -0.029(9) -0.053(9) 0.028(8) F16B 0.142(10) 0.27(3) 0.060(6) 0.004(13) -0.005(8) 0.114(12) O21 0.077(3) 0.078(3) 0.066(3) 0.009(2) -0.004(2) 0.006(2) C22 0.091(4) 0.080(5) 0.059(4) 0.007(3) -0.006(3) -0.011(4) C23 0.106(6) 0.081(6) 0.076(5) 0.019(4) -0.010(4) -0.004(4) C24 0.109(5) 0.061(4) 0.070(5) 0.000(3) -0.016(4) 0.007(4) O25 0.108(4) 0.067(3) 0.060(3) -0.004(2) -0.001(3) 0.023(3) C26 0.098(6) 0.139(8) 0.077(6) 0.017(5) 0.005(4) -0.004(6) C27 0.174(8) 0.121(9) 0.092(6) 0.017(5) -0.005(7) 0.067(7) F21 0.178(7) 0.187(6) 0.196(7) -0.087(5) 0.118(6) -0.067(5) F22 0.132(5) 0.263(7) 0.127(5) 0.097(5) 0.032(4) 0.000(5) F23 0.094(3) 0.163(5) 0.134(5) 0.024(4) -0.001(3) -0.016(4) F24 0.143(6) 0.271(10) 0.486(19) 0.233(10) 0.041(8) 0.100(7) F25 0.591(19) 0.191(8) 0.145(6) -0.055(6) -0.092(10) 0.263(10) F26 0.210(7) 0.153(5) 0.120(4) 0.046(4) -0.023(5) 0.063(5) O31 0.088(3) 0.105(4) 0.053(3) -0.001(2) -0.003(2) 0.019(3) C32 0.071(4) 0.109(6) 0.055(4) 0.013(4) -0.005(3) -0.009(4) C33 0.088(5) 0.082(5) 0.050(4) 0.004(3) -0.005(3) -0.013(4) C34 0.097(5) 0.056(4) 0.047(3) -0.001(3) 0.006(3) -0.002(3) O35 0.092(3) 0.077(3) 0.049(2) -0.010(2) -0.005(2) 0.015(3) C36 0.107(7) 0.237(12) 0.072(5) 0.011(7) -0.012(5) 0.039(7) C37 0.143(7) 0.102(6) 0.056(4) -0.010(4) 0.000(5) 0.036(6) F31A 0.26(3) 0.313(15) 0.22(3) -0.082(19) -0.136(17) 0.193(15) F32A 0.063(5) 0.49(2) 0.134(9) 0.016(11) 0.002(5) -0.014(9) F33A 0.145(13) 0.310(16) 0.072(5) 0.032(6) -0.028(5) 0.070(12) F31B 0.10(2) 0.52(7) 0.18(4) -0.14(5) -0.08(3) 0.01(4) F32B 0.14(2) 0.24(2) 0.14(3) 0.07(2) 0.02(2) 0.11(2) F33B 0.091(18) 0.24(4) 0.12(2) 0.01(2) -0.011(14) 0.047(19) F34 0.361(10) 0.106(4) 0.113(4) 0.011(4) 0.072(6) 0.097(5) F35 0.126(5) 0.296(9) 0.163(6) -0.122(7) 0.041(4) 0.019(5) F36 0.244(6) 0.167(6) 0.052(3) -0.030(3) -0.005(3) 0.065(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 Tb O31 2.324(5) . ? Tb O25 2.334(5) . ? Tb O21 2.335(5) . ? Tb O11 2.337(4) . ? Tb O35 2.343(4) . ? Tb O15 2.360(4) . ? Tb O1 2.441(6) . ? Tb O5 2.472(5) . ? O1 C2 1.422(12) . ? O1 C3 1.424(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.402(14) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 O5 1.453(12) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? O5 C6 1.403(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? O11 C12 1.257(7) . ? C12 C13 1.382(9) . ? C12 C16 1.505(11) . ? C13 C14 1.373(9) . ? C13 H13A 0.9400 . ? C14 O15 1.257(7) . ? C14 C17 1.526(9) . ? C16 F11 1.273(11) . ? C16 F13 1.281(10) . ? C16 F12 1.289(10) . ? C17 F16B 1.281(12) . ? C17 F16A 1.287(14) . ? C17 F14A 1.288(13) . ? C17 F15A 1.291(13) . ? C17 F15B 1.291(11) . ? C17 F14B 1.297(12) . ? O21 C22 1.256(8) . ? C22 C23 1.381(11) . ? C22 C26 1.532(12) . ? C23 C24 1.371(11) . ? C23 H23A 0.9400 . ? C24 O25 1.248(9) . ? C24 C27 1.508(12) . ? C26 F21 1.279(12) . ? C26 F22 1.314(11) . ? C26 F23 1.318(10) . ? C27 F25 1.218(13) . ? C27 F26 1.251(11) . ? C27 F24 1.287(15) . ? O31 C32 1.258(9) . ? C32 C33 1.388(10) . ? C32 C36 1.511(8) . ? C33 C34 1.371(10) . ? C33 H33A 0.9400 . ? C34 O35 1.261(8) . ? C34 C37 1.514(11) . ? C36 F33B 1.278(16) . ? C36 F31A 1.279(13) . ? C36 F31B 1.287(16) . ? C36 F33A 1.288(11) . ? C36 F32A 1.313(12) . ? C36 F32B 1.319(16) . ? C37 F35 1.268(12) . ? C37 F36 1.284(9) . ? C37 F34 1.314(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O31 Tb O25 120.14(19) . . ? O31 Tb O21 80.47(18) . . ? O25 Tb O21 72.43(18) . . ? O31 Tb O11 80.34(17) . . ? O25 Tb O11 140.06(16) . . ? O21 Tb O11 78.67(17) . . ? O31 Tb O35 72.26(17) . . ? O25 Tb O35 73.72(16) . . ? O21 Tb O35 116.07(17) . . ? O11 Tb O35 145.36(15) . . ? O31 Tb O15 147.35(16) . . ? O25 Tb O15 74.99(16) . . ? O21 Tb O15 77.23(17) . . ? O11 Tb O15 72.15(15) . . ? O35 Tb O15 139.52(16) . . ? O31 Tb O1 134.23(18) . . ? O25 Tb O1 81.0(2) . . ? O21 Tb O1 144.51(18) . . ? O11 Tb O1 110.04(19) . . ? O35 Tb O1 76.89(17) . . ? O15 Tb O1 73.40(16) . . ? O31 Tb O5 76.2(2) . . ? O25 Tb O5 140.3(2) . . ? O21 Tb O5 146.80(19) . . ? O11 Tb O5 74.40(17) . . ? O35 Tb O5 78.76(17) . . ? O15 Tb O5 111.68(19) . . ? O1 Tb O5 65.1(2) . . ? C2 O1 C3 115.8(8) . . ? C2 O1 Tb 123.2(7) . . ? C3 O1 Tb 114.5(6) . . ? O1 C2 H2A 109.5 . . ? O1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 O1 110.9(9) . . ? C4 C3 H3A 109.5 . . ? O1 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? O1 C3 H3B 109.5 . . ? H3A C3 H3B 108.0 . . ? C3 C4 O5 110.0(8) . . ? C3 C4 H4A 109.7 . . ? O5 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? O5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C6 O5 C4 111.5(8) . . ? C6 O5 Tb 124.8(6) . . ? C4 O5 Tb 118.2(6) . . ? O5 C6 H6A 109.5 . . ? O5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 O11 Tb 134.7(4) . . ? O11 C12 C13 127.0(6) . . ? O11 C12 C16 113.7(6) . . ? C13 C12 C16 119.3(7) . . ? C14 C13 C12 122.0(6) . . ? C14 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? O15 C14 C13 127.2(6) . . ? O15 C14 C17 113.8(6) . . ? C13 C14 C17 118.9(6) . . ? C14 O15 Tb 133.7(4) . . ? F11 C16 F13 103.8(9) . . ? F11 C16 F12 106.1(9) . . ? F13 C16 F12 105.2(9) . . ? F11 C16 C12 112.6(8) . . ? F13 C16 C12 113.5(8) . . ? F12 C16 C12 114.7(8) . . ? F16B C17 F16A 126(2) . . ? F16B C17 F14A 36.9(17) . . ? F16A C17 F14A 103(2) . . ? F16B C17 F15A 73.9(15) . . ? F16A C17 F15A 105(2) . . ? F14A C17 F15A 107.9(18) . . ? F16B C17 F15B 110.3(14) . . ? F16A C17 F15B 29(2) . . ? F14A C17 F15B 78.1(17) . . ? F15A C17 F15B 128.4(19) . . ? F16B C17 F14B 108.9(14) . . ? F16A C17 F14B 76(2) . . ? F14A C17 F14B 136.4(17) . . ? F15A C17 F14B 36.7(15) . . ? F15B C17 F14B 104.6(15) . . ? F16B C17 C14 113.3(10) . . ? F16A C17 C14 115.8(17) . . ? F14A C17 C14 110.9(14) . . ? F15A C17 C14 113.7(15) . . ? F15B C17 C14 110.9(11) . . ? F14B C17 C14 108.4(12) . . ? C22 O21 Tb 131.7(5) . . ? O21 C22 C23 127.5(8) . . ? O21 C22 C26 114.4(8) . . ? C23 C22 C26 118.0(7) . . ? C24 C23 C22 121.1(7) . . ? C24 C23 H23A 119.4 . . ? C22 C23 H23A 119.4 . . ? O25 C24 C23 127.8(8) . . ? O25 C24 C27 115.2(9) . . ? C23 C24 C27 117.0(8) . . ? C24 O25 Tb 132.6(5) . . ? F21 C26 F22 111.4(9) . . ? F21 C26 F23 106.2(10) . . ? F22 C26 F23 103.3(9) . . ? F21 C26 C22 111.5(9) . . ? F22 C26 C22 113.5(9) . . ? F23 C26 C22 110.4(8) . . ? F25 C27 F26 105.7(11) . . ? F25 C27 F24 104.4(14) . . ? F26 C27 F24 102.7(12) . . ? F25 C27 C24 113.4(10) . . ? F26 C27 C24 118.7(10) . . ? F24 C27 C24 110.5(11) . . ? C32 O31 Tb 135.9(5) . . ? O31 C32 C33 126.0(7) . . ? O31 C32 C36 115.4(7) . . ? C33 C32 C36 118.6(7) . . ? C34 C33 C32 122.3(6) . . ? C34 C33 H33A 118.9 . . ? C32 C33 H33A 118.9 . . ? O35 C34 C33 127.0(6) . . ? O35 C34 C37 114.6(7) . . ? C33 C34 C37 118.4(7) . . ? C34 O35 Tb 135.1(5) . . ? F33B C36 F31A 42(2) . . ? F33B C36 F31B 128(4) . . ? F31A C36 F31B 125(4) . . ? F33B C36 F33A 132(3) . . ? F31A C36 F33A 108.7(15) . . ? F31B C36 F33A 25(4) . . ? F33B C36 F32A 70(2) . . ? F31A C36 F32A 110.2(15) . . ? F31B C36 F32A 80(3) . . ? F33A C36 F32A 104.2(14) . . ? F33B C36 F32B 88(3) . . ? F31A C36 F32B 47.4(16) . . ? F31B C36 F32B 93(4) . . ? F33A C36 F32B 69(2) . . ? F32A C36 F32B 145(2) . . ? F33B C36 C32 114(3) . . ? F31A C36 C32 111.2(13) . . ? F31B C36 C32 115(3) . . ? F33A C36 C32 112.9(11) . . ? F32A C36 C32 109.3(10) . . ? F32B C36 C32 104(2) . . ? F35 C37 F36 107.2(9) . . ? F35 C37 F34 106.7(10) . . ? F36 C37 F34 104.9(9) . . ? F35 C37 C34 113.2(8) . . ? F36 C37 C34 115.2(8) . . ? F34 C37 C34 109.1(8) . . ? 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 O31 Tb O1 C2 -141.9(7) . . . . ? O25 Tb O1 C2 -18.2(7) . . . . ? O21 Tb O1 C2 23.4(8) . . . . ? O11 Tb O1 C2 122.1(7) . . . . ? O35 Tb O1 C2 -93.4(7) . . . . ? O15 Tb O1 C2 58.7(7) . . . . ? O5 Tb O1 C2 -177.0(7) . . . . ? O31 Tb O1 C3 8.6(7) . . . . ? O25 Tb O1 C3 132.3(6) . . . . ? O21 Tb O1 C3 173.8(6) . . . . ? O11 Tb O1 C3 -87.5(6) . . . . ? O35 Tb O1 C3 57.0(6) . . . . ? O15 Tb O1 C3 -150.8(7) . . . . ? O5 Tb O1 C3 -26.5(6) . . . . ? C2 O1 C3 C4 -156.1(10) . . . . ? Tb O1 C3 C4 51.1(10) . . . . ? O1 C3 C4 O5 -47.8(12) . . . . ? C3 C4 O5 C6 179.5(9) . . . . ? C3 C4 O5 Tb 24.3(11) . . . . ? O31 Tb O5 C6 54.3(7) . . . . ? O25 Tb O5 C6 175.2(7) . . . . ? O21 Tb O5 C6 7.6(9) . . . . ? O11 Tb O5 C6 -29.3(7) . . . . ? O35 Tb O5 C6 128.6(7) . . . . ? O15 Tb O5 C6 -92.4(7) . . . . ? O1 Tb O5 C6 -150.8(8) . . . . ? O31 Tb O5 C4 -154.0(6) . . . . ? O25 Tb O5 C4 -33.1(7) . . . . ? O21 Tb O5 C4 159.3(6) . . . . ? O11 Tb O5 C4 122.4(6) . . . . ? O35 Tb O5 C4 -79.7(6) . . . . ? O15 Tb O5 C4 59.3(6) . . . . ? O1 Tb O5 C4 0.9(6) . . . . ? O31 Tb O11 C12 144.9(7) . . . . ? O25 Tb O11 C12 18.7(8) . . . . ? O21 Tb O11 C12 62.7(7) . . . . ? O35 Tb O11 C12 -177.4(6) . . . . ? O15 Tb O11 C12 -17.3(6) . . . . ? O1 Tb O11 C12 -81.4(7) . . . . ? O5 Tb O11 C12 -136.9(7) . . . . ? Tb O11 C12 C13 12.5(12) . . . . ? Tb O11 C12 C16 -169.8(6) . . . . ? O11 C12 C13 C14 2.5(12) . . . . ? C16 C12 C13 C14 -175.1(7) . . . . ? C12 C13 C14 O15 -1.4(12) . . . . ? C12 C13 C14 C17 -179.4(7) . . . . ? C13 C14 O15 Tb -14.4(11) . . . . ? C17 C14 O15 Tb 163.7(5) . . . . ? O31 Tb O15 C14 -15.8(8) . . . . ? O25 Tb O15 C14 -138.8(6) . . . . ? O21 Tb O15 C14 -63.9(6) . . . . ? O11 Tb O15 C14 18.2(6) . . . . ? O35 Tb O15 C14 -179.2(5) . . . . ? O1 Tb O15 C14 136.3(6) . . . . ? O5 Tb O15 C14 82.6(6) . . . . ? O11 C12 C16 F11 61.5(11) . . . . ? C13 C12 C16 F11 -120.6(10) . . . . ? O11 C12 C16 F13 -56.1(11) . . . . ? C13 C12 C16 F13 121.8(9) . . . . ? O11 C12 C16 F12 -177.1(9) . . . . ? C13 C12 C16 F12 0.9(13) . . . . ? O15 C14 C17 F16B 28.7(16) . . . . ? C13 C14 C17 F16B -153.0(15) . . . . ? O15 C14 C17 F16A -175(2) . . . . ? C13 C14 C17 F16A 3(2) . . . . ? O15 C14 C17 F14A 68.6(18) . . . . ? C13 C14 C17 F14A -113.1(17) . . . . ? O15 C14 C17 F15A -53.2(18) . . . . ? C13 C14 C17 F15A 125.1(17) . . . . ? O15 C14 C17 F15B 153.4(13) . . . . ? C13 C14 C17 F15B -28.3(15) . . . . ? O15 C14 C17 F14B -92.3(13) . . . . ? C13 C14 C17 F14B 86.1(14) . . . . ? O31 Tb O21 C22 152.2(6) . . . . ? O25 Tb O21 C22 26.3(6) . . . . ? O11 Tb O21 C22 -125.8(6) . . . . ? O35 Tb O21 C22 87.5(6) . . . . ? O15 Tb O21 C22 -51.8(6) . . . . ? O1 Tb O21 C22 -17.1(8) . . . . ? O5 Tb O21 C22 -162.0(6) . . . . ? Tb O21 C22 C23 -20.6(12) . . . . ? Tb O21 C22 C26 159.4(6) . . . . ? O21 C22 C23 C24 -3.3(13) . . . . ? C26 C22 C23 C24 176.8(8) . . . . ? C22 C23 C24 O25 6.1(14) . . . . ? C22 C23 C24 C27 -176.7(9) . . . . ? C23 C24 O25 Tb 15.3(13) . . . . ? C27 C24 O25 Tb -162.0(7) . . . . ? O31 Tb O25 C24 -91.4(7) . . . . ? O21 Tb O25 C24 -24.0(7) . . . . ? O11 Tb O25 C24 21.6(8) . . . . ? O35 Tb O25 C24 -148.9(7) . . . . ? O15 Tb O25 C24 57.1(7) . . . . ? O1 Tb O25 C24 132.2(7) . . . . ? O5 Tb O25 C24 163.1(6) . . . . ? O21 C22 C26 F21 -57.3(11) . . . . ? C23 C22 C26 F21 122.6(10) . . . . ? O21 C22 C26 F22 175.9(8) . . . . ? C23 C22 C26 F22 -4.1(13) . . . . ? O21 C22 C26 F23 60.4(11) . . . . ? C23 C22 C26 F23 -119.6(9) . . . . ? O25 C24 C27 F25 -71.9(16) . . . . ? C23 C24 C27 F25 110.5(14) . . . . ? O25 C24 C27 F26 163.2(11) . . . . ? C23 C24 C27 F26 -14.5(17) . . . . ? O25 C24 C27 F24 45.0(14) . . . . ? C23 C24 C27 F24 -132.6(12) . . . . ? O25 Tb O31 C32 -72.0(8) . . . . ? O21 Tb O31 C32 -135.2(7) . . . . ? O11 Tb O31 C32 144.8(7) . . . . ? O35 Tb O31 C32 -13.7(7) . . . . ? O15 Tb O31 C32 177.5(6) . . . . ? O1 Tb O31 C32 36.2(8) . . . . ? O5 Tb O31 C32 68.7(7) . . . . ? Tb O31 C32 C33 13.6(13) . . . . ? Tb O31 C32 C36 -169.6(7) . . . . ? O31 C32 C33 C34 -2.1(13) . . . . ? C36 C32 C33 C34 -178.8(8) . . . . ? C32 C33 C34 O35 -1.7(12) . . . . ? C32 C33 C34 C37 -179.2(8) . . . . ? C33 C34 O35 Tb -5.5(12) . . . . ? C37 C34 O35 Tb 172.0(6) . . . . ? O31 Tb O35 C34 9.6(6) . . . . ? O25 Tb O35 C34 139.6(7) . . . . ? O21 Tb O35 C34 79.1(7) . . . . ? O11 Tb O35 C34 -29.7(8) . . . . ? O15 Tb O35 C34 -179.7(6) . . . . ? O1 Tb O35 C34 -136.1(7) . . . . ? O5 Tb O35 C34 -69.3(7) . . . . ? O31 C32 C36 F33B -2(3) . . . . ? C33 C32 C36 F33B 175(3) . . . . ? O31 C32 C36 F31A 43.2(18) . . . . ? C33 C32 C36 F31A -139.8(15) . . . . ? O31 C32 C36 F31B -166(4) . . . . ? C33 C32 C36 F31B 10(4) . . . . ? O31 C32 C36 F33A 165.8(14) . . . . ? C33 C32 C36 F33A -17.2(18) . . . . ? O31 C32 C36 F32A -78.7(13) . . . . ? C33 C32 C36 F32A 98.3(12) . . . . ? O31 C32 C36 F32B 93(2) . . . . ? C33 C32 C36 F32B -90(2) . . . . ? O35 C34 C37 F35 -48.6(11) . . . . ? C33 C34 C37 F35 129.1(9) . . . . ? O35 C34 C37 F36 -172.5(9) . . . . ? C33 C34 C37 F36 5.3(13) . . . . ? O35 C34 C37 F34 69.9(11) . . . . ? C33 C34 C37 F34 -112.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.322 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.096 # Attachment '- TmCif.txt' data_ef650 _database_code_depnum_ccdc_archive 'CCDC 833381' #TrackingRef '- TmCif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H13 F18 O8 Tm' _chemical_formula_sum 'C19 H13 F18 O8 Tm' _chemical_formula_weight 880.22 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.899(4) _cell_length_b 15.821(3) _cell_length_c 20.655(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5849(2) _cell_formula_units_Z 8 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 14004 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.999 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3376 _exptl_absorpt_coefficient_mu 3.189 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.495 _exptl_absorpt_correction_T_max 0.538 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ANISO two -CF3 disordered C-F SADI, 43/57 and 79/21 C32-C36 1.51 DFIX ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 26562 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5172 _reflns_number_gt 3256 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V., 1997-2002)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0650P)^2^+8.8400P] 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 5172 _refine_ls_number_parameters 471 _refine_ls_number_restraints 200 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1305 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 0.991 _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 Tm Tm 0.131885(18) 0.65936(2) 0.240896(15) 0.06011(16) Uani 1 1 d U . . O1 O 0.2642(3) 0.6802(4) 0.2333(3) 0.0961(17) Uani 1 1 d U . . C2 C 0.3172(6) 0.6276(9) 0.2638(5) 0.141(4) Uani 1 1 d U . . H2A H 0.3222 0.5754 0.2396 0.212 Uiso 1 1 calc R . . H2B H 0.3007 0.6150 0.3075 0.212 Uiso 1 1 calc R . . H2C H 0.3651 0.6562 0.2654 0.212 Uiso 1 1 calc R . . C3 C 0.2891(6) 0.7138(8) 0.1733(5) 0.123(3) Uani 1 1 d U . . H3A H 0.2821 0.6718 0.1389 0.147 Uiso 1 1 calc R . . H3B H 0.3425 0.7272 0.1760 0.147 Uiso 1 1 calc R . . C4 C 0.2478(8) 0.7882(7) 0.1585(5) 0.134(3) Uani 1 1 d U . . H4A H 0.2589 0.8066 0.1142 0.160 Uiso 1 1 calc R . . H4B H 0.2618 0.8338 0.1883 0.160 Uiso 1 1 calc R . . O5 O 0.1676(4) 0.7695(4) 0.1649(3) 0.1017(17) Uani 1 1 d U . . C6 C 0.1234(7) 0.8407(6) 0.1494(5) 0.149(5) Uani 1 1 d U . . H6A H 0.1360 0.8870 0.1781 0.223 Uiso 1 1 calc R . . H6B H 0.0710 0.8265 0.1544 0.223 Uiso 1 1 calc R . . H6C H 0.1329 0.8573 0.1049 0.223 Uiso 1 1 calc R . . O11 O 0.0773(3) 0.7814(3) 0.2773(2) 0.0708(13) Uani 1 1 d U . . C12 C 0.0685(4) 0.8142(4) 0.3316(4) 0.0659(18) Uani 1 1 d U . . C13 C 0.1024(4) 0.7905(5) 0.3886(3) 0.0658(18) Uani 1 1 d U . . H13A H 0.0894 0.8183 0.4272 0.079 Uiso 1 1 calc R . . C14 C 0.1548(4) 0.7271(5) 0.3905(3) 0.0584(16) Uani 1 1 d U A . O15 O 0.1760(3) 0.6819(3) 0.3444(2) 0.0665(12) Uani 1 1 d U . . C16 C 0.0158(6) 0.8882(7) 0.3314(5) 0.100(3) Uani 1 1 d U . . C17 C 0.1913(4) 0.7050(5) 0.4551(4) 0.0754(19) Uani 1 1 d DU . . F11 F -0.0501(4) 0.8680(5) 0.3118(5) 0.200(4) Uani 1 1 d U . . F12 F 0.0063(5) 0.9237(5) 0.3870(3) 0.189(4) Uani 1 1 d U . . F13 F 0.0355(5) 0.9469(4) 0.2925(4) 0.180(3) Uani 1 1 d U . . F14A F 0.2614(8) 0.7242(17) 0.4542(16) 0.132(10) Uani 0.43 1 d PDU A 1 F15A F 0.1857(16) 0.6264(11) 0.4720(17) 0.119(8) Uani 0.43 1 d PDU A 1 F16A F 0.168(3) 0.748(2) 0.5044(14) 0.148(13) Uani 0.43 1 d PDU A 1 F14B F 0.1500(11) 0.6467(12) 0.4814(13) 0.152(9) Uani 0.57 1 d PDU A 2 F15B F 0.1909(18) 0.7673(15) 0.4956(11) 0.130(9) Uani 0.57 1 d PDU A 2 F16B F 0.2582(8) 0.6755(16) 0.4510(10) 0.152(9) Uani 0.57 1 d PDU A 2 O21 O 0.0353(3) 0.6107(3) 0.3038(2) 0.0710(12) Uani 1 1 d U . . C22 C 0.0341(5) 0.5582(5) 0.3497(4) 0.0755(19) Uani 1 1 d U . . C23 C 0.0874(5) 0.4975(5) 0.3646(4) 0.079(2) Uani 1 1 d U . . H23A H 0.0809 0.4634 0.4014 0.095 Uiso 1 1 calc R . . C24 C 0.1493(5) 0.4865(5) 0.3265(4) 0.0735(19) Uani 1 1 d U . . O25 O 0.1675(3) 0.5292(3) 0.2777(2) 0.0732(13) Uani 1 1 d U . . C26 C -0.0349(6) 0.5664(9) 0.3933(5) 0.107(3) Uani 1 1 d U . . C27 C 0.2026(8) 0.4166(7) 0.3436(6) 0.119(3) Uani 1 1 d U . . F21 F -0.0454(5) 0.6388(6) 0.4129(5) 0.218(5) Uani 1 1 d U . . F22 F -0.0369(4) 0.5080(6) 0.4384(3) 0.196(3) Uani 1 1 d U . . F23 F -0.0952(4) 0.5456(4) 0.3601(3) 0.142(2) Uani 1 1 d U . . F24 F 0.2692(5) 0.4356(7) 0.3345(7) 0.293(7) Uani 1 1 d U . . F25 F 0.1901(8) 0.3506(5) 0.3071(4) 0.249(5) Uani 1 1 d U . . F26 F 0.1964(4) 0.3853(4) 0.4003(3) 0.158(3) Uani 1 1 d U . . O31 O 0.0337(3) 0.6650(3) 0.1701(2) 0.0818(15) Uani 1 1 d U . . C32 C 0.0253(4) 0.6460(5) 0.1122(4) 0.076(2) Uani 1 1 d DU B . C33 C 0.0734(4) 0.6008(5) 0.0733(3) 0.0685(19) Uani 1 1 d U . . H33A H 0.0603 0.5903 0.0300 0.082 Uiso 1 1 calc R . . C34 C 0.1393(5) 0.5712(4) 0.0963(3) 0.0644(17) Uani 1 1 d U . . O35 O 0.1663(3) 0.5814(3) 0.1515(2) 0.0701(13) Uani 1 1 d U . . C36 C -0.0486(5) 0.6747(9) 0.0837(5) 0.133(4) Uani 1 1 d DU . . C37 C 0.1880(6) 0.5186(6) 0.0513(4) 0.093(2) Uani 1 1 d U . . F31A F -0.0651(11) 0.7494(12) 0.1038(9) 0.284(12) Uani 0.79 1 d PDU B 1 F32A F -0.1033(5) 0.6257(13) 0.1023(7) 0.239(7) Uani 0.79 1 d PDU B 1 F33A F -0.0499(8) 0.6772(11) 0.0212(4) 0.175(6) Uani 0.79 1 d PDU B 1 F31B F -0.067(3) 0.631(4) 0.034(3) 0.24(3) Uani 0.21 1 d PDU B 2 F32B F -0.035(3) 0.7502(17) 0.0597(18) 0.151(11) Uani 0.21 1 d PDU B 2 F33B F -0.086(2) 0.724(3) 0.121(3) 0.185(19) Uani 0.21 1 d PDU B 2 F34 F 0.1848(5) 0.4382(4) 0.0682(3) 0.177(3) Uani 1 1 d U . . F35 F 0.2564(4) 0.5385(6) 0.0528(3) 0.185(3) Uani 1 1 d U . . F36 F 0.1682(4) 0.5193(4) -0.0087(2) 0.144(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tm 0.0799(3) 0.0588(2) 0.0416(2) -0.00434(14) 0.00022(15) 0.00914(16) O1 0.093(3) 0.143(5) 0.053(3) -0.017(3) 0.009(3) -0.023(3) C2 0.079(6) 0.253(14) 0.092(8) 0.001(8) 0.002(5) 0.013(8) C3 0.114(7) 0.166(10) 0.088(7) 0.000(7) 0.024(6) -0.058(6) C4 0.198(9) 0.122(8) 0.081(7) -0.003(6) 0.020(7) -0.078(7) O5 0.161(5) 0.083(4) 0.061(3) 0.009(3) 0.030(4) -0.001(4) C6 0.305(14) 0.077(6) 0.064(6) 0.018(5) 0.040(8) 0.042(8) O11 0.100(4) 0.065(3) 0.047(3) 0.003(2) 0.000(2) 0.015(3) C12 0.080(5) 0.060(4) 0.058(4) -0.005(3) 0.009(4) 0.016(3) C13 0.084(5) 0.070(5) 0.044(4) -0.011(3) 0.008(3) 0.009(4) C14 0.065(4) 0.069(4) 0.041(3) -0.006(3) 0.002(3) -0.006(3) O15 0.079(3) 0.076(3) 0.044(3) -0.005(2) 0.002(2) 0.019(2) C16 0.118(7) 0.105(7) 0.077(6) -0.008(5) -0.002(5) 0.048(5) C17 0.087(5) 0.091(5) 0.048(4) -0.003(4) -0.005(4) 0.008(4) F11 0.114(5) 0.153(6) 0.333(12) -0.054(6) -0.053(6) 0.070(4) F12 0.274(9) 0.176(6) 0.117(5) -0.044(4) -0.010(5) 0.159(6) F13 0.236(8) 0.110(5) 0.193(7) 0.051(5) 0.048(6) 0.087(5) F14A 0.092(8) 0.19(2) 0.118(16) 0.056(17) -0.038(9) -0.014(11) F15A 0.169(19) 0.087(7) 0.102(15) 0.024(8) -0.062(16) 0.006(10) F16A 0.24(3) 0.164(19) 0.038(7) -0.005(10) 0.010(13) 0.09(2) F14B 0.195(17) 0.174(15) 0.087(11) 0.069(13) -0.046(13) -0.065(14) F15B 0.185(16) 0.124(11) 0.082(13) -0.041(11) -0.059(12) 0.033(10) F16B 0.131(10) 0.26(3) 0.065(8) 0.008(14) -0.007(8) 0.107(12) O21 0.074(3) 0.082(3) 0.057(3) 0.007(3) -0.005(2) 0.003(2) C22 0.090(5) 0.085(5) 0.051(4) 0.004(4) -0.005(3) -0.005(4) C23 0.095(5) 0.076(5) 0.067(5) 0.014(4) -0.012(4) -0.007(4) C24 0.104(5) 0.058(4) 0.059(5) -0.004(3) -0.018(4) 0.007(4) O25 0.097(4) 0.067(3) 0.055(3) -0.006(2) -0.003(3) 0.021(3) C26 0.090(6) 0.151(8) 0.078(7) 0.018(6) 0.008(4) -0.003(6) C27 0.160(8) 0.090(7) 0.106(8) 0.026(5) 0.011(8) 0.050(6) F21 0.217(8) 0.189(6) 0.248(10) -0.108(6) 0.170(7) -0.081(6) F22 0.141(6) 0.315(9) 0.132(6) 0.114(6) 0.041(4) 0.017(6) F23 0.095(4) 0.171(6) 0.160(6) 0.029(4) -0.003(4) -0.012(4) F24 0.134(6) 0.260(9) 0.486(18) 0.243(10) 0.055(8) 0.099(6) F25 0.468(15) 0.132(6) 0.147(7) -0.032(5) -0.037(9) 0.163(7) F26 0.214(7) 0.150(5) 0.110(5) 0.040(4) -0.024(5) 0.071(5) O31 0.088(3) 0.110(4) 0.047(3) -0.002(3) -0.003(2) 0.022(3) C32 0.070(4) 0.113(7) 0.045(4) 0.012(4) -0.007(3) 0.000(4) C33 0.081(5) 0.079(5) 0.046(4) 0.002(4) -0.004(3) -0.007(4) C34 0.099(5) 0.053(4) 0.041(4) -0.002(3) 0.000(3) 0.003(4) O35 0.087(3) 0.077(3) 0.046(3) -0.012(2) -0.008(2) 0.015(3) C36 0.095(7) 0.233(12) 0.070(6) 0.011(7) -0.016(5) 0.047(7) C37 0.127(6) 0.100(6) 0.051(4) -0.010(4) -0.003(5) 0.037(6) F31A 0.31(2) 0.335(14) 0.211(16) -0.100(14) -0.167(19) 0.230(14) F32A 0.059(5) 0.51(2) 0.149(9) 0.044(12) 0.002(6) -0.003(9) F33A 0.131(10) 0.329(18) 0.066(5) 0.022(6) -0.032(5) 0.068(11) F31B 0.08(2) 0.34(5) 0.29(6) -0.14(5) -0.11(3) -0.01(4) F32B 0.16(3) 0.22(2) 0.08(2) 0.01(2) -0.07(2) 0.072(19) F33B 0.037(15) 0.27(5) 0.25(5) -0.05(3) 0.03(2) 0.020(16) F34 0.321(10) 0.102(4) 0.108(5) 0.005(4) 0.057(6) 0.086(5) F35 0.112(4) 0.299(9) 0.144(6) -0.124(6) 0.026(4) 0.023(5) F36 0.220(6) 0.163(5) 0.049(3) -0.029(3) -0.003(3) 0.061(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 Tm O25 2.285(5) . ? Tm O31 2.287(5) . ? Tm O11 2.291(5) . ? Tm O21 2.295(5) . ? Tm O35 2.305(5) . ? Tm O15 2.307(5) . ? Tm O1 2.396(6) . ? Tm O5 2.431(6) . ? O1 C2 1.411(12) . ? O1 C3 1.420(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.424(15) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 O5 1.472(13) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? O5 C6 1.413(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? O11 C12 1.245(8) . ? C12 C13 1.378(10) . ? C12 C16 1.504(12) . ? C13 C14 1.374(10) . ? C13 H13A 0.9400 . ? C14 O15 1.250(7) . ? C14 C17 1.526(10) . ? C16 F13 1.278(12) . ? C16 F11 1.287(12) . ? C16 F12 1.290(10) . ? C17 F16B 1.289(12) . ? C17 F15B 1.291(12) . ? C17 F16A 1.291(14) . ? C17 F14A 1.292(13) . ? C17 F15A 1.296(13) . ? C17 F14B 1.301(12) . ? O21 C22 1.260(8) . ? C22 C23 1.389(11) . ? C22 C26 1.535(12) . ? C23 C24 1.370(11) . ? C23 H23A 0.9400 . ? C24 O25 1.257(9) . ? C24 C27 1.502(12) . ? C26 F21 1.229(13) . ? C26 F22 1.312(12) . ? C26 F23 1.322(11) . ? C27 F24 1.244(14) . ? C27 F26 1.277(11) . ? C27 F25 1.307(14) . ? O31 C32 1.242(9) . ? C32 C33 1.379(10) . ? C32 C36 1.519(8) . ? C33 C34 1.355(10) . ? C33 H33A 0.9400 . ? C34 O35 1.249(8) . ? C34 C37 1.521(11) . ? C36 F31A 1.286(13) . ? C36 F33B 1.287(16) . ? C36 F31B 1.288(17) . ? C36 F33A 1.291(11) . ? C36 F32A 1.308(12) . ? C36 F32B 1.313(16) . ? C37 F35 1.264(11) . ? C37 F36 1.289(9) . ? C37 F34 1.320(10) . ? F32B F33B 1.62(8) . ? 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 O25 Tm O31 117.50(19) . . ? O25 Tm O11 140.29(17) . . ? O31 Tm O11 81.33(18) . . ? O25 Tm O21 73.70(18) . . ? O31 Tm O21 78.24(18) . . ? O11 Tm O21 77.07(18) . . ? O25 Tm O35 73.11(17) . . ? O31 Tm O35 73.41(17) . . ? O11 Tm O35 145.91(16) . . ? O21 Tm O35 118.37(18) . . ? O25 Tm O15 74.67(17) . . ? O31 Tm O15 148.15(17) . . ? O11 Tm O15 73.25(16) . . ? O21 Tm O15 77.62(17) . . ? O35 Tm O15 137.17(16) . . ? O25 Tm O1 82.5(2) . . ? O31 Tm O1 135.39(19) . . ? O11 Tm O1 109.1(2) . . ? O21 Tm O1 145.85(19) . . ? O35 Tm O1 75.91(18) . . ? O15 Tm O1 72.60(18) . . ? O25 Tm O5 141.9(2) . . ? O31 Tm O5 76.2(2) . . ? O11 Tm O5 73.70(18) . . ? O21 Tm O5 143.5(2) . . ? O35 Tm O5 78.24(18) . . ? O15 Tm O5 113.4(2) . . ? O1 Tm O5 66.4(2) . . ? C2 O1 C3 113.5(8) . . ? C2 O1 Tm 123.7(7) . . ? C3 O1 Tm 114.8(6) . . ? O1 C2 H2A 109.5 . . ? O1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O1 C3 C4 109.5(10) . . ? O1 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? O1 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C3 C4 O5 108.7(8) . . ? C3 C4 H4A 109.9 . . ? O5 C4 H4A 109.9 . . ? C3 C4 H4B 109.9 . . ? O5 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C6 O5 C4 111.4(8) . . ? C6 O5 Tm 124.8(6) . . ? C4 O5 Tm 117.3(6) . . ? O5 C6 H6A 109.5 . . ? O5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 O11 Tm 134.5(5) . . ? O11 C12 C13 126.9(7) . . ? O11 C12 C16 113.7(7) . . ? C13 C12 C16 119.4(7) . . ? C14 C13 C12 121.6(6) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? O15 C14 C13 127.1(6) . . ? O15 C14 C17 114.0(6) . . ? C13 C14 C17 118.9(6) . . ? C14 O15 Tm 133.7(4) . . ? F13 C16 F11 103.6(9) . . ? F13 C16 F12 106.2(10) . . ? F11 C16 F12 105.5(10) . . ? F13 C16 C12 113.3(9) . . ? F11 C16 C12 112.5(9) . . ? F12 C16 C12 114.8(8) . . ? F16B C17 F15B 108.9(16) . . ? F16B C17 F16A 123(3) . . ? F15B C17 F16A 24(3) . . ? F16B C17 F14A 35.0(16) . . ? F15B C17 F14A 81(2) . . ? F16A C17 F14A 101(2) . . ? F16B C17 F15A 75.1(14) . . ? F15B C17 F15A 124(2) . . ? F16A C17 F15A 106(2) . . ? F14A C17 F15A 107.8(17) . . ? F16B C17 F14B 107.4(15) . . ? F15B C17 F14B 105.6(19) . . ? F16A C17 F14B 82(3) . . ? F14A C17 F14B 136.5(17) . . ? F15A C17 F14B 33.1(17) . . ? F16B C17 C14 114.9(11) . . ? F15B C17 C14 112.9(15) . . ? F16A C17 C14 116(2) . . ? F14A C17 C14 110.4(15) . . ? F15A C17 C14 114.9(16) . . ? F14B C17 C14 106.5(12) . . ? C22 O21 Tm 131.3(5) . . ? O21 C22 C23 127.6(8) . . ? O21 C22 C26 113.6(8) . . ? C23 C22 C26 118.7(8) . . ? C24 C23 C22 121.1(7) . . ? C24 C23 H23A 119.4 . . ? C22 C23 H23A 119.4 . . ? O25 C24 C23 126.9(7) . . ? O25 C24 C27 114.9(8) . . ? C23 C24 C27 118.2(8) . . ? C24 O25 Tm 132.8(5) . . ? F21 C26 F22 114.8(11) . . ? F21 C26 F23 106.1(11) . . ? F22 C26 F23 99.8(10) . . ? F21 C26 C22 113.3(10) . . ? F22 C26 C22 112.3(9) . . ? F23 C26 C22 109.3(9) . . ? F24 C27 F26 108.4(12) . . ? F24 C27 F25 105.7(13) . . ? F26 C27 F25 101.8(10) . . ? F24 C27 C24 113.2(10) . . ? F26 C27 C24 116.5(10) . . ? F25 C27 C24 110.1(10) . . ? C32 O31 Tm 134.3(5) . . ? O31 C32 C33 127.7(7) . . ? O31 C32 C36 114.0(7) . . ? C33 C32 C36 118.2(7) . . ? C34 C33 C32 121.2(7) . . ? C34 C33 H33A 119.4 . . ? C32 C33 H33A 119.4 . . ? O35 C34 C33 127.8(7) . . ? O35 C34 C37 114.0(7) . . ? C33 C34 C37 118.2(7) . . ? C34 O35 Tm 134.2(5) . . ? F31A C36 F33B 30(3) . . ? F31A C36 F31B 134(3) . . ? F33B C36 F31B 132(3) . . ? F31A C36 F33A 107.0(13) . . ? F33B C36 F33A 125(4) . . ? F31B C36 F33A 38(4) . . ? F31A C36 F32A 106.2(15) . . ? F33B C36 F32A 78(2) . . ? F31B C36 F32A 74(3) . . ? F33A C36 F32A 107.3(12) . . ? F31A C36 F32B 47.8(19) . . ? F33B C36 F32B 77(4) . . ? F31B C36 F32B 104(4) . . ? F33A C36 F32B 66.4(17) . . ? F32A C36 F32B 142(2) . . ? F31A C36 C32 110.4(12) . . ? F33B C36 C32 114(3) . . ? F31B C36 C32 112(3) . . ? F33A C36 C32 114.4(10) . . ? F32A C36 C32 111.1(9) . . ? F32B C36 C32 105(2) . . ? F35 C37 F36 106.7(9) . . ? F35 C37 F34 105.9(9) . . ? F36 C37 F34 104.5(8) . . ? F35 C37 C34 113.9(8) . . ? F36 C37 C34 115.2(8) . . ? F34 C37 C34 109.9(8) . . ? C36 F32B F33B 51(2) . . ? C36 F33B F32B 52(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 O25 Tm O1 C2 -15.4(7) . . . . ? O31 Tm O1 C2 -137.5(7) . . . . ? O11 Tm O1 C2 125.4(7) . . . . ? O21 Tm O1 C2 30.4(9) . . . . ? O35 Tm O1 C2 -89.8(7) . . . . ? O15 Tm O1 C2 60.8(7) . . . . ? O5 Tm O1 C2 -173.0(8) . . . . ? O25 Tm O1 C3 131.3(7) . . . . ? O31 Tm O1 C3 9.3(8) . . . . ? O11 Tm O1 C3 -87.8(7) . . . . ? O21 Tm O1 C3 177.1(6) . . . . ? O35 Tm O1 C3 56.9(7) . . . . ? O15 Tm O1 C3 -152.5(7) . . . . ? O5 Tm O1 C3 -26.2(7) . . . . ? C2 O1 C3 C4 -157.7(10) . . . . ? Tm O1 C3 C4 52.1(10) . . . . ? O1 C3 C4 O5 -50.5(11) . . . . ? C3 C4 O5 C6 -178.7(9) . . . . ? C3 C4 O5 Tm 28.1(11) . . . . ? O25 Tm O5 C6 171.1(7) . . . . ? O31 Tm O5 C6 53.9(8) . . . . ? O11 Tm O5 C6 -31.0(7) . . . . ? O21 Tm O5 C6 7.1(9) . . . . ? O35 Tm O5 C6 129.4(8) . . . . ? O15 Tm O5 C6 -94.0(8) . . . . ? O1 Tm O5 C6 -150.9(8) . . . . ? O25 Tm O5 C4 -39.6(7) . . . . ? O31 Tm O5 C4 -156.8(6) . . . . ? O11 Tm O5 C4 118.3(6) . . . . ? O21 Tm O5 C4 156.4(6) . . . . ? O35 Tm O5 C4 -81.3(6) . . . . ? O15 Tm O5 C4 55.3(6) . . . . ? O1 Tm O5 C4 -1.6(6) . . . . ? O25 Tm O11 C12 20.3(8) . . . . ? O31 Tm O11 C12 143.5(7) . . . . ? O21 Tm O11 C12 63.6(7) . . . . ? O35 Tm O11 C12 -174.3(6) . . . . ? O15 Tm O11 C12 -17.1(7) . . . . ? O1 Tm O11 C12 -81.4(7) . . . . ? O5 Tm O11 C12 -138.5(7) . . . . ? Tm O11 C12 C13 12.3(13) . . . . ? Tm O11 C12 C16 -169.1(6) . . . . ? O11 C12 C13 C14 3.1(13) . . . . ? C16 C12 C13 C14 -175.5(8) . . . . ? C12 C13 C14 O15 -3.0(12) . . . . ? C12 C13 C14 C17 178.9(7) . . . . ? C13 C14 O15 Tm -12.2(11) . . . . ? C17 C14 O15 Tm 166.0(5) . . . . ? O25 Tm O15 C14 -139.3(7) . . . . ? O31 Tm O15 C14 -21.6(8) . . . . ? O11 Tm O15 C14 17.0(6) . . . . ? O21 Tm O15 C14 -63.1(6) . . . . ? O35 Tm O15 C14 178.3(6) . . . . ? O1 Tm O15 C14 133.8(7) . . . . ? O5 Tm O15 C14 80.2(7) . . . . ? O11 C12 C16 F13 -57.1(12) . . . . ? C13 C12 C16 F13 121.6(10) . . . . ? O11 C12 C16 F11 60.0(12) . . . . ? C13 C12 C16 F11 -121.2(10) . . . . ? O11 C12 C16 F12 -179.3(9) . . . . ? C13 C12 C16 F12 -0.6(15) . . . . ? O15 C14 C17 F16B 30.8(16) . . . . ? C13 C14 C17 F16B -150.9(15) . . . . ? O15 C14 C17 F15B 156.6(17) . . . . ? C13 C14 C17 F15B -25.1(18) . . . . ? O15 C14 C17 F16A -177(2) . . . . ? C13 C14 C17 F16A 1(3) . . . . ? O15 C14 C17 F14A 68.5(16) . . . . ? C13 C14 C17 F14A -113.2(16) . . . . ? O15 C14 C17 F15A -53.6(18) . . . . ? C13 C14 C17 F15A 124.7(17) . . . . ? O15 C14 C17 F14B -88.0(15) . . . . ? C13 C14 C17 F14B 90.3(15) . . . . ? O25 Tm O21 C22 25.0(6) . . . . ? O31 Tm O21 C22 148.6(7) . . . . ? O11 Tm O21 C22 -127.8(7) . . . . ? O35 Tm O21 C22 84.9(7) . . . . ? O15 Tm O21 C22 -52.4(6) . . . . ? O1 Tm O21 C22 -22.7(8) . . . . ? O5 Tm O21 C22 -165.2(6) . . . . ? Tm O21 C22 C23 -19.0(12) . . . . ? Tm O21 C22 C26 159.8(6) . . . . ? O21 C22 C23 C24 -2.5(13) . . . . ? C26 C22 C23 C24 178.7(9) . . . . ? C22 C23 C24 O25 3.3(13) . . . . ? C22 C23 C24 C27 -176.8(9) . . . . ? C23 C24 O25 Tm 18.0(13) . . . . ? C27 C24 O25 Tm -161.9(7) . . . . ? O31 Tm O25 C24 -91.9(7) . . . . ? O11 Tm O25 C24 19.3(8) . . . . ? O21 Tm O25 C24 -25.0(7) . . . . ? O35 Tm O25 C24 -152.3(7) . . . . ? O15 Tm O25 C24 56.3(7) . . . . ? O1 Tm O25 C24 130.3(7) . . . . ? O5 Tm O25 C24 164.9(6) . . . . ? O21 C22 C26 F21 -51.7(13) . . . . ? C23 C22 C26 F21 127.2(11) . . . . ? O21 C22 C26 F22 176.3(9) . . . . ? C23 C22 C26 F22 -4.8(14) . . . . ? O21 C22 C26 F23 66.5(12) . . . . ? C23 C22 C26 F23 -114.6(10) . . . . ? O25 C24 C27 F24 37.1(16) . . . . ? C23 C24 C27 F24 -142.8(13) . . . . ? O25 C24 C27 F26 163.8(10) . . . . ? C23 C24 C27 F26 -16.1(16) . . . . ? O25 C24 C27 F25 -81.0(13) . . . . ? C23 C24 C27 F25 99.1(12) . . . . ? O25 Tm O31 C32 -72.8(8) . . . . ? O11 Tm O31 C32 144.2(8) . . . . ? O21 Tm O31 C32 -137.3(8) . . . . ? O35 Tm O31 C32 -12.6(7) . . . . ? O15 Tm O31 C32 -178.7(6) . . . . ? O1 Tm O31 C32 35.8(9) . . . . ? O5 Tm O31 C32 69.0(7) . . . . ? Tm O31 C32 C33 11.4(14) . . . . ? Tm O31 C32 C36 -170.8(7) . . . . ? O31 C32 C33 C34 -0.3(13) . . . . ? C36 C32 C33 C34 -178.1(8) . . . . ? C32 C33 C34 O35 -2.3(13) . . . . ? C32 C33 C34 C37 177.4(8) . . . . ? C33 C34 O35 Tm -5.9(12) . . . . ? C37 C34 O35 Tm 174.3(6) . . . . ? O25 Tm O35 C34 136.5(7) . . . . ? O31 Tm O35 C34 10.0(7) . . . . ? O11 Tm O35 C34 -33.9(8) . . . . ? O21 Tm O35 C34 76.3(7) . . . . ? O15 Tm O35 C34 179.2(6) . . . . ? O1 Tm O35 C34 -137.2(7) . . . . ? O5 Tm O35 C34 -68.9(7) . . . . ? O31 C32 C36 F31A 40.8(17) . . . . ? C33 C32 C36 F31A -141.1(15) . . . . ? O31 C32 C36 F33B 9(4) . . . . ? C33 C32 C36 F33B -173(3) . . . . ? O31 C32 C36 F31B -157(4) . . . . ? C33 C32 C36 F31B 21(4) . . . . ? O31 C32 C36 F33A 161.5(13) . . . . ? C33 C32 C36 F33A -20.4(18) . . . . ? O31 C32 C36 F32A -76.7(14) . . . . ? C33 C32 C36 F32A 101.3(13) . . . . ? O31 C32 C36 F32B 91(2) . . . . ? C33 C32 C36 F32B -91(2) . . . . ? O35 C34 C37 F35 -44.8(11) . . . . ? C33 C34 C37 F35 135.4(9) . . . . ? O35 C34 C37 F36 -168.5(9) . . . . ? C33 C34 C37 F36 11.7(13) . . . . ? O35 C34 C37 F34 73.9(11) . . . . ? C33 C34 C37 F34 -105.9(9) . . . . ? F31A C36 F32B F33B -8(3) . . . . ? F31B C36 F32B F33B 131(3) . . . . ? F33A C36 F32B F33B 138(3) . . . . ? F32A C36 F32B F33B 50(4) . . . . ? C32 C36 F32B F33B -112(2) . . . . ? F31A C36 F33B F32B 11(6) . . . . ? F31B C36 F33B F32B -97(6) . . . . ? F33A C36 F33B F32B -48(3) . . . . ? F32A C36 F33B F32B -151(2) . . . . ? C32 C36 F33B F32B 101(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.162 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.100 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # If this CIF has been generated directly or indirectly from an entry in the # Cambridge Structural Database, then it will include bibliographic, chemical, # crystal, experimental, refinement or atomic coordinate data resulting from # the CCDC's data processing and validation procedures. Files generated from # CSD entries are Copyright 2011 Cambridge Crystallographic Data Centre. They # may be used in bona fide research applications only, and may not be copied or # further disseminated in any form, whether machine-readable or not, except for # the purposes of generating routine backup copies on your local computer # system. # # Files arising from any other source may also contain material that is the # copyright of third parties, including the originator, and you should check # with the originator concerning the permitted uses of the information # contained in this CIF. # # For further information on the CCDC and the free tools enCIFer and Mercury # for validating and visualising CIF files, please visit www.ccdc.cam.ac.uk # ####################################################################### data_k11231a _database_code_depnum_ccdc_archive 'CCDC 851921' #TrackingRef '- Ce_H2O.txt' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 21.870(4) _cell_length_b 13.012(3) _cell_length_c 21.537(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.14(3) _cell_angle_gamma 90.00 _cell_volume 5716.38 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Ce1 Ce 0.008228(13) 0.33906(2) 0.254705(14) O1 O 0.04139(18) 0.2674(3) 0.16018(19) C2 C -0.0008(3) 0.1970(5) 0.1125(3) H2A H -0.0350 0.2354 0.0781 H2B H -0.0211 0.1501 0.1350 H2C H 0.0250 0.1573 0.0920 C3 C 0.0761(3) 0.3348(5) 0.1310(3) H3A H 0.0449 0.3822 0.0991 H3B H 0.0985 0.2940 0.1067 C4 C 0.1249(3) 0.3942(5) 0.1853(3) H4A H 0.1576 0.3471 0.2159 H4B H 0.1483 0.4430 0.1664 O5 O 0.09078(17) 0.4492(3) 0.22074(18) C6 C 0.1329(3) 0.5233(5) 0.2666(3) H6A H 0.1693 0.4873 0.3001 H6B H 0.1076 0.5610 0.2887 H6C H 0.1501 0.5716 0.2421 O7 O 0.01583(19) 0.1401(3) 0.2614(2) H7A H 0.017(3) 0.117(5) 0.298(4) H7B H 0.044(3) 0.105(5) 0.257(3) O11 O -0.10282(17) 0.2707(3) 0.1882(2) C12 C -0.1522(3) 0.3026(4) 0.1406(3) C13 C -0.1556(3) 0.3835(5) 0.0978(3) H13A H -0.1957 0.3964 0.0620 C14 C -0.1021(2) 0.4464(4) 0.1054(3) O15 O -0.04709(17) 0.4459(3) 0.15241(18) C16 C -0.2151(3) 0.2418(6) 0.1306(4) C17 C -0.1076(3) 0.5279(5) 0.0521(3) F11 F -0.16761(17) 0.5350(3) 0.00631(19) F12 F -0.06691(19) 0.5038(3) 0.02018(17) F13 F -0.09027(17) 0.6202(3) 0.07889(17) F14 F -0.26825(19) 0.2832(4) 0.0868(3) F15 F -0.2103(2) 0.1469(4) 0.1097(3) F16 F -0.2246(2) 0.2306(4) 0.1878(3) O21 O -0.07521(17) 0.4524(3) 0.27404(19) C22 C -0.1133(2) 0.4412(4) 0.3059(3) C23 C -0.1138(3) 0.3652(5) 0.3500(3) H23A H -0.1446 0.3698 0.3717 C24 C -0.0709(3) 0.2818(5) 0.3644(3) O25 O -0.02923(19) 0.2611(3) 0.33849(19) C26 C -0.1674(3) 0.5237(5) 0.2895(3) C27 C -0.0725(3) 0.2033(5) 0.4166(3) F21 F -0.1952(2) 0.5306(4) 0.3345(2) F22 F -0.21568(17) 0.4986(3) 0.23244(19) F23 F -0.14602(18) 0.6146(3) 0.2798(2) F24 F -0.0788(3) 0.1090(3) 0.3928(2) F25 F -0.1178(2) 0.2225(4) 0.4424(2) F26 F -0.01577(19) 0.2038(3) 0.46763(18) O31 O 0.06152(19) 0.4335(3) 0.36219(19) C32 C 0.1110(3) 0.4187(5) 0.4137(3) C33 C 0.1639(3) 0.3547(5) 0.4222(3) H33A H 0.1994 0.3540 0.4637 C34 C 0.1661(2) 0.2914(4) 0.3712(3) O35 O 0.12238(17) 0.2793(3) 0.31505(18) C36 C 0.1117(5) 0.4810(8) 0.4758(4) C37 C 0.2278(3) 0.2266(5) 0.3822(3) F31A F 0.1524(5) 0.4461(8) 0.5307(5) F32A F 0.0509(4) 0.4866(6) 0.4777(4) F33A F 0.1254(4) 0.5811(6) 0.4665(4) F34 F 0.27591(17) 0.2472(4) 0.4399(2) F35 F 0.25096(17) 0.2424(3) 0.3337(2) F36 F 0.21389(19) 0.1271(3) 0.3812(2) Ce2 Ce 0.498321(13) 0.39650(2) 0.241726(14) O41 O 0.53522(18) 0.2863(3) 0.16012(18) C42 C 0.4916(3) 0.2128(5) 0.1161(3) H42A H 0.4582 0.2490 0.0796 H42B H 0.4704 0.1720 0.1409 H42C H 0.5167 0.1672 0.0979 C43 C 0.5712(3) 0.3421(5) 0.1269(3) H43A H 0.5414 0.3889 0.0932 H43B H 0.5910 0.2937 0.1041 C44 C 0.6239(3) 0.4029(5) 0.1783(3) H44A H 0.6552 0.3560 0.2105 H44B H 0.6484 0.4445 0.1565 O45 O 0.59341(17) 0.4685(3) 0.21179(19) C46 C 0.6396(3) 0.5397(5) 0.2556(3) H46A H 0.6750 0.5014 0.2888 H46B H 0.6172 0.5828 0.2781 H46C H 0.6580 0.5834 0.2295 O47 O 0.4904(2) 0.5958(3) 0.2337(2) H47A H 0.457(3) 0.615(5) 0.237(3) H47B H 0.493(3) 0.631(5) 0.203(4) O51 O 0.39364(17) 0.3013(3) 0.18432(19) C52 C 0.3421(3) 0.3210(4) 0.1359(3) C53 C 0.3341(3) 0.3902(5) 0.0843(3) H53A H 0.2924 0.3962 0.0497 C54 C 0.3857(2) 0.4506(4) 0.0820(3) O55 O 0.44165(17) 0.4569(3) 0.12519(18) C56 C 0.2825(3) 0.2572(5) 0.1340(3) C57 C 0.3747(3) 0.5196(5) 0.0220(3) F51 F 0.22601(17) 0.2926(4) 0.0909(3) F52 F 0.27775(19) 0.2521(4) 0.1935(2) F53 F 0.2875(2) 0.1605(3) 0.1159(2) F54 F 0.31767(19) 0.5053(3) -0.02741(19) F55 F 0.42145(19) 0.5058(3) -0.00369(17) F56 F 0.37796(18) 0.6187(3) 0.03920(18) O61 O 0.5602(2) 0.4662(3) 0.35524(19) C62 C 0.6057(4) 0.4355(5) 0.4055(3) C63 C 0.6497(3) 0.3552(5) 0.4107(3) H63A H 0.6850 0.3445 0.4516 C64 C 0.6427(3) 0.2912(4) 0.3576(3) O65 O 0.59783(17) 0.2911(3) 0.30116(17) C66 C 0.6146(4) 0.4940(8) 0.4720(5) C67 C 0.6962(3) 0.2102(5) 0.3650(3) F61A F 0.6553(8) 0.4495(12) 0.5265(7) F62A F 0.5566(4) 0.5072(7) 0.4771(4) F63A F 0.6348(5) 0.5923(7) 0.4600(5) F64 F 0.73144(17) 0.2372(3) 0.3282(2) F65 F 0.67025(17) 0.1189(3) 0.34453(18) F66 F 0.73802(17) 0.2003(3) 0.42788(19) O71 O 0.41127(18) 0.4732(3) 0.27331(19) C72 C 0.3822(2) 0.4496(4) 0.3116(3) C73 C 0.3945(3) 0.3683(4) 0.3561(3) H73A H 0.3703 0.3636 0.3848 C74 C 0.4411(3) 0.2935(4) 0.3599(3) O75 O 0.47585(18) 0.2835(3) 0.32489(18) C76 C 0.3253(3) 0.5223(5) 0.3065(3) C77 C 0.4531(3) 0.2117(5) 0.4141(3) F71 F 0.3450(2) 0.6189(3) 0.3145(3) F72 F 0.27868(16) 0.5158(3) 0.24645(18) F73 F 0.29648(18) 0.5010(3) 0.34990(19) F74 F 0.4066(2) 0.2046(4) 0.4388(2) F75 F 0.5074(2) 0.2372(4) 0.46662(19) F76 F 0.4658(2) 0.1204(3) 0.39458(19) F31B F 0.0815(11) 0.5448(18) 0.4749(10) F32B F 0.1767(5) 0.4915(9) 0.5223(6) F33B F 0.1124(8) 0.4057(12) 0.5273(8) F61B F 0.6140(9) 0.5881(10) 0.4761(9) F62B F 0.6849(4) 0.4966(8) 0.5101(5) F63B F 0.6140(6) 0.4246(9) 0.5210(6) ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # If this CIF has been generated directly or indirectly from an entry in the # Cambridge Structural Database, then it will include bibliographic, chemical, # crystal, experimental, refinement or atomic coordinate data resulting from # the CCDC's data processing and validation procedures. Files generated from # CSD entries are Copyright 2011 Cambridge Crystallographic Data Centre. They # may be used in bona fide research applications only, and may not be copied or # further disseminated in any form, whether machine-readable or not, except for # the purposes of generating routine backup copies on your local computer # system. # # Files arising from any other source may also contain material that is the # copyright of third parties, including the originator, and you should check # with the originator concerning the permitted uses of the information # contained in this CIF. # # For further information on the CCDC and the free tools enCIFer and Mercury # for validating and visualising CIF files, please visit www.ccdc.cam.ac.uk # ####################################################################### data_k11238 _database_code_depnum_ccdc_archive 'CCDC 851922' #TrackingRef '- La_bismg.txt' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 11.8739(6) _cell_length_b 22.9990(11) _cell_length_c 12.5329(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.168(2) _cell_angle_gamma 90.00 _cell_volume 3413.53 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z La La 0.710982(16) 0.906433(8) 0.737066(15) O1 O 0.9029(2) 0.85246(11) 0.6691(2) C2 C 0.9504(4) 0.8680(2) 0.5714(3) H2A H 0.9932 0.9043 0.5817 H2B H 0.8896 0.8735 0.5151 H2C H 1.0009 0.8370 0.5505 C3 C 0.9913(3) 0.8422(2) 0.7504(4) H3A H 1.0332 0.8787 0.7666 H3B H 1.0448 0.8132 0.7252 C4 C 0.9417(4) 0.82050(19) 0.8484(4) H4A H 0.9011 0.7836 0.8326 H4B H 1.0024 0.8131 0.9051 O5 O 0.8651(2) 0.86323(12) 0.8840(2) C6 C 0.8379(4) 0.8518(2) 0.9919(3) H6A H 0.8001 0.8140 0.9949 H6B H 0.7876 0.8823 1.0153 H6C H 0.9074 0.8512 1.0391 O11 O 0.6697(2) 0.98485(12) 0.5750(2) C12 C 0.7469(4) 0.9897(2) 0.4926(3) H12A H 0.7117 1.0123 0.4327 H12B H 0.7659 0.9508 0.4676 H12C H 0.8158 1.0094 0.5211 C13 C 0.6306(6) 1.0403(2) 0.6053(5) H13A H 0.6050 1.0629 0.5409 H13B H 0.6923 1.0620 0.6449 C14 C 0.5364(6) 1.0320(3) 0.6734(5) H14A H 0.5097 1.0702 0.6978 H14B H 0.4729 1.0125 0.6322 O15 O 0.5727(2) 0.99776(13) 0.7624(2) C16 C 0.4898(4) 0.9947(2) 0.8396(5) H16A H 0.4687 1.0341 0.8601 H16B H 0.5210 0.9737 0.9030 H16C H 0.4228 0.9742 0.8085 O21 O 0.8746(2) 0.97299(11) 0.7170(2) C22 C 0.9286(3) 1.01148(15) 0.7694(3) C23 C 0.9104(3) 1.03267(17) 0.8694(3) H23A H 0.9599 1.0612 0.9014 C24 C 0.8199(3) 1.01276(16) 0.9242(3) O25 O 0.7543(2) 0.97264(12) 0.9000(2) C26 C 1.0252(4) 1.0378(2) 0.7099(3) C27 C 0.7928(4) 1.0454(2) 1.0260(4) F21 F 0.9838(3) 1.06404(18) 0.6216(3) F22 F 1.0959(2) 0.99636(14) 0.6819(3) F23 F 1.0866(2) 1.07681(13) 0.7659(2) F24 F 0.8701(3) 1.08320(19) 1.0593(3) F25 F 0.7808(3) 1.00914(16) 1.1058(2) F26 F 0.6955(3) 1.07292(16) 1.0106(3) O31 O 0.6959(2) 0.79808(12) 0.7460(2) C32 C 0.6830(4) 0.7584(2) 0.6846(4) C33 C 0.6716(4) 0.7600(2) 0.5731(4) H33A H 0.6612 0.7247 0.5342 C34 C 0.6754(4) 0.8132(2) 0.5169(4) O35 O 0.6873(2) 0.86287(12) 0.5528(2) C36 C 0.6780(6) 0.6973(2) 0.7373(5) C37 C 0.6584(5) 0.8114(2) 0.3927(4) F31A F 0.640(2) 0.6635(7) 0.6714(16) F32A F 0.7797(9) 0.6817(4) 0.7657(14) F33A F 0.6226(19) 0.6887(12) 0.8161(16) F34 F 0.7215(4) 0.8489(2) 0.3483(3) F35 F 0.5558(4) 0.8207(2) 0.3565(3) F36 F 0.6806(3) 0.75851(18) 0.3581(3) O41 O 0.5056(2) 0.88213(13) 0.6788(2) C42 C 0.4353(4) 0.8487(2) 0.7134(4) C43 C 0.4360(4) 0.8255(2) 0.8170(4) H43A H 0.3795 0.7983 0.8329 C44 C 0.5175(4) 0.8415(2) 0.8968(4) O45 O 0.6021(2) 0.87357(13) 0.8897(2) C46 C 0.3377(4) 0.8321(2) 0.6346(4) C47 C 0.5098(4) 0.8169(2) 1.0106(4) F41 F 0.3716(4) 0.8216(2) 0.5370(3) F42 F 0.2646(3) 0.8749(2) 0.6223(4) F43 F 0.2835(4) 0.78522(18) 0.6603(3) F44 F 0.5874(3) 0.77754(19) 1.0311(4) F45 F 0.5214(4) 0.85761(17) 1.0809(3) F46 F 0.4128(3) 0.79012(19) 1.0219(3) F31B F 0.717(2) 0.6976(3) 0.8323(10) F32B F 0.5753(10) 0.6819(6) 0.7382(17) F33B F 0.7292(16) 0.6582(4) 0.6857(14)