Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author ; Prof. Mike Ward Department of Chemistry University of Sheffield SHEFFIELD S3 7HF UK ; _publ_contact_author_fax '0114 2229346' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_section_title ; Anthracene as a sensitiser for near-infrared luminescence in complexes of Nd(III), Er(III) and Yb(III): an unexpected sensitisation mechanism based on electron transfer ; _publ_contact_letter ; This CIF file contains details of the 4 crystal structure in the paper 'Anthracene as a sensitiser for near-infrared luminescence...' by T. Lazarides et al, submitted to Dalton Trans. for publication. ; _publ_contact_author_name 'Prof. Mike Ward' loop_ _publ_author_name 'Mike Ward' 'Harry Adams' 'Mohammed Alamiry' 'Stephen Faulkner' 'Theodore Lazarides' 'Simon Pope' ; J.A.Weinstein ; #======================================================== data_imw355_0m _database_code_depnum_ccdc_archive 'CCDC 633721' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H22 F18 N3 Nd O6' _chemical_formula_weight 1150.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4875(15) _cell_length_b 12.8921(15) _cell_length_c 13.5629(17) _cell_angle_alpha 79.429(2) _cell_angle_beta 77.367(3) _cell_angle_gamma 85.850(2) _cell_volume 2093.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description colourless _exptl_crystal_colour block _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1130 _exptl_absorpt_coefficient_mu 1.374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7901 _exptl_absorpt_correction_T_max 0.8309 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _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 'Bruker CCD SMART area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44086 _diffrn_reflns_av_R_equivalents 0.1795 _diffrn_reflns_av_sigmaI/netI 0.1116 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.86 _reflns_number_total 9790 _reflns_number_gt 7521 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9790 _refine_ls_number_parameters 733 _refine_ls_number_restraints 176 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 1.021 _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 Nd1 Nd 0.20062(2) 0.230853(17) 0.208382(17) 0.02148(8) Uani 1 1 d . . . F1 F 0.2064(3) 0.1118(2) 0.6378(2) 0.0398(7) Uani 1 1 d . . . F2 F 0.0675(2) 0.0666(2) 0.58737(19) 0.0385(7) Uani 1 1 d . . . F3 F 0.0977(3) 0.2312(2) 0.5768(2) 0.0466(8) Uani 1 1 d . . . F4 F 0.5684(3) 0.1019(3) 0.2492(3) 0.0834(14) Uani 1 1 d . . . F5 F 0.5509(3) 0.0855(2) 0.4112(3) 0.0633(11) Uani 1 1 d . . . F6 F 0.5098(2) -0.0407(2) 0.3465(2) 0.0400(7) Uani 1 1 d . . . F7 F 0.0781(5) -0.1453(4) 0.2113(4) 0.0583(16) Uani 0.692(5) 1 d PDU A 1 F8 F -0.0392(4) -0.0343(4) 0.1600(4) 0.0616(14) Uani 0.692(5) 1 d PDU A 1 F9 F 0.0634(5) -0.1170(4) 0.0538(3) 0.0663(16) Uani 0.692(5) 1 d PDU A 1 F7' F 0.1332(9) -0.1532(7) 0.1010(8) 0.065(2) Uani 0.308(5) 1 d PDU A 2 F8' F 0.0295(9) -0.1134(9) 0.2314(7) 0.058(2) Uani 0.308(5) 1 d PDU A 2 F9' F -0.0173(8) -0.0757(10) 0.0890(8) 0.074(2) Uani 0.308(5) 1 d PDU A 2 F13 F -0.1717(3) 0.1213(2) 0.2969(2) 0.0456(8) Uani 1 1 d . . . F14 F -0.2130(2) 0.1657(2) 0.1481(2) 0.0428(7) Uani 1 1 d . . . F15 F -0.2427(3) 0.2741(2) 0.2537(2) 0.0498(8) Uani 1 1 d . . . F16 F -0.0222(4) 0.4421(5) -0.1035(4) 0.0715(17) Uani 0.717(7) 1 d PDU B 1 F17 F 0.1466(5) 0.4604(4) -0.1196(5) 0.0593(16) Uani 0.717(7) 1 d PDU B 1 F18 F 0.0889(6) 0.3215(4) -0.1519(4) 0.0722(17) Uani 0.717(7) 1 d PDU B 1 F16' F -0.0071(11) 0.3762(12) -0.1334(11) 0.080(3) Uani 0.283(7) 1 d PDU B 2 F17' F 0.1002(10) 0.4858(9) -0.1103(15) 0.064(3) Uani 0.283(7) 1 d PDU B 2 F18' F 0.1581(11) 0.3326(9) -0.1320(9) 0.070(2) Uani 0.283(7) 1 d PDU B 2 O1 O 0.1574(3) 0.1706(2) 0.3891(2) 0.0240(7) Uani 1 1 d . . . O2 O 0.3570(3) 0.1336(2) 0.2612(2) 0.0289(7) Uani 1 1 d . . . O3 O 0.3037(3) 0.1776(3) 0.0511(3) 0.0530(12) Uani 1 1 d . . . O4 O 0.1329(3) 0.0677(2) 0.1843(2) 0.0252(7) Uani 1 1 d . . . O5 O -0.0004(3) 0.2447(2) 0.2404(2) 0.0275(7) Uani 1 1 d . . . O6 O 0.1445(3) 0.3447(3) 0.0635(3) 0.0475(10) Uani 1 1 d . . . N1 N 0.1568(3) 0.4008(3) 0.2952(3) 0.0226(8) Uani 1 1 d . . . N2 N 0.3519(3) 0.3651(2) 0.1625(2) 0.0196(7) Uani 1 1 d . . . N3 N 0.4270(3) 0.5081(2) 0.1885(2) 0.0178(7) Uani 1 1 d . . . C1 C 0.0569(4) 0.4204(3) 0.3495(3) 0.0247(10) Uani 1 1 d . . . H1 H 0.0102 0.3629 0.3791 0.030 Uiso 1 1 calc R . . C2 C 0.0185(4) 0.5211(3) 0.3644(3) 0.0248(10) Uani 1 1 d . . . H2 H -0.0516 0.5318 0.4063 0.030 Uiso 1 1 calc R A . C3 C 0.0838(4) 0.6054(3) 0.3173(3) 0.0239(9) Uani 1 1 d . . . H3 H 0.0577 0.6756 0.3228 0.029 Uiso 1 1 calc R . . C4 C 0.1880(3) 0.5861(3) 0.2620(3) 0.0195(9) Uani 1 1 d . . . H4 H 0.2344 0.6430 0.2287 0.023 Uiso 1 1 calc R A . C5 C 0.2240(3) 0.4831(3) 0.2557(3) 0.0169(8) Uani 1 1 d . A . C6 C 0.3345(4) 0.4528(3) 0.2037(3) 0.0191(9) Uani 1 1 d . A . C7 C 0.5103(4) 0.4540(3) 0.1297(3) 0.0213(9) Uani 1 1 d . A . C8 C 0.6193(4) 0.4777(3) 0.0871(3) 0.0243(9) Uani 1 1 d . . . H8 H 0.6505 0.5391 0.0968 0.029 Uiso 1 1 calc R A . C9 C 0.6799(4) 0.4072(4) 0.0298(3) 0.0312(11) Uani 1 1 d . . . H9 H 0.7547 0.4205 -0.0009 0.037 Uiso 1 1 calc R . . C10 C 0.6337(4) 0.3160(4) 0.0156(3) 0.0293(11) Uani 1 1 d . . . H10 H 0.6780 0.2688 -0.0238 0.035 Uiso 1 1 calc R A . C11 C 0.5257(4) 0.2941(3) 0.0576(3) 0.0263(10) Uani 1 1 d . A . H11 H 0.4948 0.2324 0.0481 0.032 Uiso 1 1 calc R . . C12 C 0.4624(4) 0.3654(3) 0.1148(3) 0.0198(9) Uani 1 1 d . A . C13 C 0.4520(4) 0.5947(3) 0.2384(3) 0.0219(9) Uani 1 1 d . . . H13A H 0.4360 0.6631 0.1966 0.026 Uiso 1 1 calc R . . H13B H 0.5315 0.5907 0.2381 0.026 Uiso 1 1 calc R . . C14 C 0.3894(3) 0.5933(3) 0.3471(3) 0.0197(9) Uani 1 1 d . . . C15 C 0.3911(4) 0.5010(3) 0.4211(3) 0.0214(9) Uani 1 1 d . . . C16 C 0.4619(4) 0.4105(3) 0.4015(3) 0.0244(10) Uani 1 1 d . . . H16 H 0.5084 0.4111 0.3358 0.029 Uiso 1 1 calc R A . C17 C 0.4632(4) 0.3236(3) 0.4764(4) 0.0334(12) Uani 1 1 d . . . H17 H 0.5121 0.2655 0.4627 0.040 Uiso 1 1 calc R . . C18 C 0.3932(5) 0.3193(4) 0.5730(4) 0.0404(13) Uani 1 1 d . . . H18 H 0.3934 0.2573 0.6231 0.048 Uiso 1 1 calc R A . C19 C 0.3255(4) 0.4019(4) 0.5959(4) 0.0331(12) Uani 1 1 d . . . H19 H 0.2788 0.3973 0.6618 0.040 Uiso 1 1 calc R . . C20 C 0.3234(4) 0.4958(3) 0.5224(3) 0.0251(10) Uani 1 1 d . . . C21 C 0.2582(4) 0.5842(4) 0.5456(4) 0.0307(11) Uani 1 1 d . . . H21 H 0.2111 0.5802 0.6114 0.037 Uiso 1 1 calc R . . C22 C 0.2598(4) 0.6769(4) 0.4767(4) 0.0291(11) Uani 1 1 d . . . C23 C 0.1918(4) 0.7669(4) 0.5018(4) 0.0402(13) Uani 1 1 d . . . H23 H 0.1448 0.7622 0.5677 0.048 Uiso 1 1 calc R . . C24 C 0.1929(4) 0.8571(4) 0.4351(5) 0.0476(16) Uani 1 1 d . . . H24 H 0.1464 0.9152 0.4536 0.057 Uiso 1 1 calc R A . C25 C 0.2629(5) 0.8664(4) 0.3370(5) 0.0425(14) Uani 1 1 d . . . H25 H 0.2646 0.9316 0.2909 0.051 Uiso 1 1 calc R . . C26 C 0.3281(4) 0.7834(3) 0.3075(4) 0.0317(11) Uani 1 1 d . . . H26 H 0.3742 0.7917 0.2411 0.038 Uiso 1 1 calc R A . C27 C 0.3283(4) 0.6840(3) 0.3748(3) 0.0249(10) Uani 1 1 d . . . C28 C 0.1462(4) 0.1364(3) 0.5664(3) 0.0297(11) Uani 1 1 d . . . C29 C 0.2120(4) 0.1396(3) 0.4573(3) 0.0210(9) Uani 1 1 d . . . C30 C 0.3240(4) 0.1084(3) 0.4426(4) 0.0275(10) Uani 1 1 d . . . H30 H 0.3572 0.0886 0.5003 0.033 Uiso 1 1 calc R . . C31 C 0.3863(4) 0.1063(3) 0.3449(4) 0.0278(10) Uani 1 1 d . . . C32 C 0.5052(4) 0.0633(4) 0.3368(4) 0.0397(13) Uani 1 1 d . . . C33 C 0.0659(4) -0.0726(3) 0.1332(3) 0.0411(14) Uani 1 1 d D . . C34 C 0.1433(5) 0.0163(4) 0.1141(4) 0.0368(12) Uani 1 1 d . A . C35 C 0.2131(5) 0.0348(5) 0.0190(4) 0.062(2) Uani 1 1 d D . . H35 H 0.2169 -0.0135 -0.0270 0.075 Uiso 1 1 calc R A 1 C36 C 0.2807(6) 0.1272(6) -0.0120(6) 0.047(2) Uani 0.711(4) 1 d PDU A 1 C37 C 0.3501(5) 0.1419(4) -0.1154(5) 0.048(2) Uani 0.711(4) 1 d PDU A 1 F10 F 0.4525(4) 0.1063(5) -0.1148(4) 0.0884(19) Uani 0.711(4) 1 d PDU A 1 F11 F 0.3168(4) 0.0972(3) -0.1834(3) 0.0555(14) Uani 0.711(4) 1 d PDU A 1 F12 F 0.3572(5) 0.2443(4) -0.1550(3) 0.087(2) Uani 0.711(4) 1 d PDU A 1 C36' C 0.3114(12) 0.0953(18) 0.0055(18) 0.049(2) Uani 0.289(4) 1 d PDU A 2 C37' C 0.4086(13) 0.0914(8) -0.0768(12) 0.051(2) Uani 0.289(4) 1 d PDU A 2 F10' F 0.5073(10) 0.1083(10) -0.0642(10) 0.081(3) Uani 0.289(4) 1 d PDU A 2 F11' F 0.4281(11) 0.0036(10) -0.1149(9) 0.091(3) Uani 0.289(4) 1 d PDU A 2 F12' F 0.4044(13) 0.1608(11) -0.1604(10) 0.085(2) Uani 0.289(4) 1 d PDU A 2 C38 C -0.1728(4) 0.2006(4) 0.2191(3) 0.0303(11) Uani 1 1 d . . . C39 C -0.0576(4) 0.2447(3) 0.1756(4) 0.0304(11) Uani 1 1 d . A . C40 C -0.0320(4) 0.2838(4) 0.0704(4) 0.0350(12) Uani 1 1 d . . . H40 H -0.0817 0.2740 0.0292 0.042 Uiso 1 1 calc R A . C41 C 0.0647(5) 0.3371(4) 0.0240(4) 0.0472(15) Uani 1 1 d . B . C42 C 0.0714(3) 0.3867(4) -0.0852(4) 0.0595(18) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.02763(14) 0.02119(13) 0.01659(12) -0.00540(8) -0.00277(10) -0.00747(10) F1 0.050(2) 0.0472(17) 0.0240(14) -0.0002(12) -0.0163(14) -0.0050(15) F2 0.0325(16) 0.0525(18) 0.0268(15) 0.0010(12) -0.0011(13) -0.0133(14) F3 0.064(2) 0.0388(16) 0.0309(16) -0.0107(13) 0.0007(15) 0.0198(15) F4 0.0282(19) 0.081(3) 0.100(3) 0.042(2) 0.023(2) 0.0121(18) F5 0.0313(18) 0.052(2) 0.124(3) -0.041(2) -0.035(2) 0.0143(16) F6 0.0341(17) 0.0281(15) 0.0568(19) -0.0136(13) -0.0066(15) 0.0120(13) F7 0.066(4) 0.039(3) 0.068(3) 0.020(2) -0.025(3) -0.027(3) F8 0.065(3) 0.059(3) 0.065(3) -0.016(2) -0.011(3) -0.028(3) F9 0.088(4) 0.071(3) 0.046(3) -0.028(2) 0.004(3) -0.050(3) F7' 0.072(5) 0.061(4) 0.063(4) -0.012(4) -0.006(4) -0.033(4) F8' 0.068(5) 0.045(5) 0.058(4) 0.001(4) -0.006(4) -0.028(4) F9' 0.084(5) 0.073(5) 0.067(5) -0.009(4) -0.012(4) -0.033(4) F13 0.052(2) 0.0410(17) 0.0440(18) 0.0054(13) -0.0152(16) -0.0165(15) F14 0.0352(17) 0.0582(19) 0.0396(17) -0.0076(14) -0.0137(14) -0.0169(15) F15 0.042(2) 0.0532(19) 0.056(2) -0.0148(16) -0.0126(17) 0.0110(16) F16 0.076(3) 0.097(4) 0.042(3) 0.004(3) -0.024(3) -0.009(3) F17 0.071(4) 0.060(3) 0.044(3) 0.028(2) -0.030(3) -0.026(3) F18 0.120(5) 0.071(3) 0.025(2) -0.009(2) -0.011(3) -0.014(3) F16' 0.104(5) 0.096(5) 0.044(4) 0.000(4) -0.027(4) -0.027(5) F17' 0.070(5) 0.068(5) 0.049(4) 0.024(4) -0.026(5) -0.008(4) F18' 0.110(5) 0.072(4) 0.031(4) 0.011(4) -0.028(4) -0.022(5) O1 0.0236(17) 0.0251(16) 0.0227(16) -0.0040(12) -0.0044(14) 0.0013(13) O2 0.0292(19) 0.0209(16) 0.0324(18) -0.0048(13) 0.0031(15) -0.0013(14) O3 0.070(3) 0.055(2) 0.033(2) -0.0289(18) 0.0222(19) -0.040(2) O4 0.0351(19) 0.0218(15) 0.0200(15) -0.0083(12) -0.0027(14) -0.0067(14) O5 0.0278(18) 0.0353(17) 0.0238(16) -0.0080(13) -0.0109(14) -0.0052(14) O6 0.045(2) 0.071(3) 0.0291(19) 0.0094(17) -0.0189(18) -0.033(2) N1 0.023(2) 0.0254(19) 0.0190(18) -0.0047(14) -0.0019(16) -0.0064(16) N2 0.0206(19) 0.0191(17) 0.0192(18) -0.0056(13) -0.0029(15) -0.0004(15) N3 0.0167(18) 0.0199(17) 0.0176(17) -0.0032(13) -0.0037(15) -0.0047(14) C1 0.019(2) 0.032(2) 0.022(2) -0.0063(18) 0.0010(19) -0.0090(19) C2 0.021(2) 0.033(2) 0.022(2) -0.0084(18) -0.0034(19) 0.0004(19) C3 0.023(2) 0.024(2) 0.028(2) -0.0082(18) -0.010(2) 0.0016(19) C4 0.019(2) 0.020(2) 0.021(2) 0.0006(16) -0.0097(18) -0.0067(17) C5 0.016(2) 0.021(2) 0.0145(19) -0.0031(15) -0.0062(17) -0.0024(17) C6 0.023(2) 0.020(2) 0.015(2) 0.0016(15) -0.0067(18) -0.0048(17) C7 0.022(2) 0.027(2) 0.015(2) 0.0002(16) -0.0052(18) -0.0025(18) C8 0.017(2) 0.032(2) 0.023(2) 0.0006(18) -0.0058(19) -0.0020(19) C9 0.019(2) 0.046(3) 0.023(2) 0.004(2) -0.001(2) -0.001(2) C10 0.029(3) 0.036(3) 0.019(2) -0.0016(18) -0.002(2) 0.009(2) C11 0.030(3) 0.026(2) 0.021(2) -0.0027(17) -0.004(2) 0.003(2) C12 0.021(2) 0.022(2) 0.014(2) 0.0020(15) -0.0027(17) -0.0013(18) C13 0.023(2) 0.021(2) 0.024(2) -0.0052(17) -0.0062(19) -0.0070(18) C14 0.019(2) 0.018(2) 0.025(2) -0.0041(16) -0.0077(18) -0.0057(17) C15 0.024(2) 0.023(2) 0.021(2) -0.0045(16) -0.0089(19) -0.0087(18) C16 0.026(2) 0.022(2) 0.029(2) -0.0053(18) -0.013(2) -0.0028(19) C17 0.044(3) 0.021(2) 0.044(3) -0.005(2) -0.026(3) -0.006(2) C18 0.058(4) 0.033(3) 0.035(3) 0.011(2) -0.026(3) -0.026(3) C19 0.038(3) 0.040(3) 0.024(2) 0.001(2) -0.010(2) -0.023(2) C20 0.023(2) 0.031(2) 0.025(2) -0.0061(18) -0.0071(19) -0.0129(19) C21 0.025(3) 0.043(3) 0.027(2) -0.015(2) -0.003(2) -0.010(2) C22 0.020(2) 0.033(2) 0.040(3) -0.020(2) -0.006(2) -0.006(2) C23 0.025(3) 0.044(3) 0.062(4) -0.035(3) -0.009(3) -0.001(2) C24 0.032(3) 0.035(3) 0.089(5) -0.038(3) -0.020(3) 0.004(2) C25 0.045(3) 0.020(2) 0.072(4) -0.008(2) -0.033(3) -0.004(2) C26 0.032(3) 0.020(2) 0.048(3) -0.007(2) -0.017(2) -0.004(2) C27 0.022(2) 0.023(2) 0.034(2) -0.0082(18) -0.011(2) -0.0065(19) C28 0.036(3) 0.028(2) 0.026(2) -0.0016(18) -0.012(2) 0.004(2) C29 0.025(2) 0.019(2) 0.022(2) -0.0052(16) -0.0093(19) 0.0008(18) C30 0.025(3) 0.024(2) 0.036(3) -0.0035(19) -0.013(2) 0.0031(19) C31 0.022(2) 0.018(2) 0.042(3) -0.0060(19) -0.002(2) -0.0007(18) C32 0.025(3) 0.034(3) 0.056(3) -0.005(2) -0.003(3) 0.002(2) C33 0.058(4) 0.037(3) 0.028(3) -0.015(2) 0.006(3) -0.023(3) C34 0.051(3) 0.033(3) 0.028(3) -0.008(2) -0.005(2) -0.015(2) C35 0.082(5) 0.069(4) 0.036(3) -0.035(3) 0.022(3) -0.045(4) C36 0.041(4) 0.071(5) 0.034(4) -0.030(3) 0.008(3) -0.021(3) C37 0.040(4) 0.073(4) 0.035(3) -0.030(3) 0.010(3) -0.024(3) F10 0.071(4) 0.137(4) 0.054(4) -0.042(3) 0.020(3) -0.020(4) F11 0.067(3) 0.075(3) 0.027(2) -0.031(2) 0.013(2) -0.033(2) F12 0.129(5) 0.087(4) 0.037(3) -0.021(3) 0.031(3) -0.072(3) C36' 0.043(4) 0.072(5) 0.035(4) -0.028(4) 0.011(3) -0.023(4) C37' 0.044(5) 0.074(5) 0.035(4) -0.028(4) 0.012(3) -0.023(4) F10' 0.064(7) 0.128(6) 0.054(6) -0.050(5) 0.021(5) -0.024(6) F11' 0.080(6) 0.118(7) 0.067(6) -0.048(6) 0.032(5) -0.021(6) F12' 0.096(4) 0.101(4) 0.045(4) -0.018(4) 0.026(4) -0.034(4) C38 0.032(3) 0.031(2) 0.027(2) 0.0000(19) -0.009(2) 0.000(2) C39 0.038(3) 0.026(2) 0.032(3) -0.0078(19) -0.016(2) 0.000(2) C40 0.039(3) 0.042(3) 0.029(3) -0.001(2) -0.017(2) -0.015(2) C41 0.056(4) 0.056(3) 0.033(3) 0.002(2) -0.019(3) -0.025(3) C42 0.039(4) 0.102(5) 0.040(4) 0.005(3) -0.022(3) -0.020(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 Nd1 O1 2.385(3) . ? Nd1 O2 2.414(3) . ? Nd1 O4 2.423(3) . ? Nd1 O3 2.427(3) . ? Nd1 O6 2.430(4) . ? Nd1 O5 2.451(3) . ? Nd1 N2 2.552(3) . ? Nd1 N1 2.642(3) . ? F1 C28 1.332(5) . ? F2 C28 1.330(5) . ? F3 C28 1.342(5) . ? F4 C32 1.309(6) . ? F5 C32 1.345(6) . ? F6 C32 1.321(5) . ? F7 C33 1.309(4) . ? F8 C33 1.365(5) . ? F9 C33 1.316(4) . ? F7' C33 1.362(8) . ? F8' C33 1.331(9) . ? F9' C33 1.314(8) . ? F13 C38 1.329(5) . ? F14 C38 1.337(5) . ? F15 C38 1.320(5) . ? F16 C42 1.371(5) . ? F17 C42 1.333(5) . ? F18 C42 1.319(5) . ? F16' C42 1.319(10) . ? F17' C42 1.315(10) . ? F18' C42 1.346(10) . ? O1 C29 1.257(5) . ? O2 C31 1.250(6) . ? O3 C36 1.254(8) . ? O3 C36' 1.310(19) . ? O4 C34 1.236(5) . ? O5 C39 1.248(5) . ? O6 C41 1.247(6) . ? N1 C1 1.335(5) . ? N1 C5 1.356(5) . ? N2 C6 1.334(5) . ? N2 C12 1.390(5) . ? N3 C6 1.359(5) . ? N3 C7 1.394(5) . ? N3 C13 1.490(4) . ? C1 C2 1.385(6) . ? C1 H1 0.9500 . ? C2 C3 1.378(6) . ? C2 H2 0.9500 . ? C3 C4 1.383(6) . ? C3 H3 0.9500 . ? C4 C5 1.382(5) . ? C4 H4 0.9500 . ? C5 C6 1.467(6) . ? C7 C8 1.390(6) . ? C7 C12 1.393(5) . ? C8 C9 1.380(6) . ? C8 H8 0.9500 . ? C9 C10 1.408(6) . ? C9 H9 0.9500 . ? C10 C11 1.372(6) . ? C10 H10 0.9500 . ? C11 C12 1.400(5) . ? C11 H11 0.9500 . ? C13 C14 1.508(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.410(6) . ? C14 C27 1.413(6) . ? C15 C20 1.440(6) . ? C15 C16 1.441(6) . ? C16 C17 1.369(6) . ? C16 H16 0.9500 . ? C17 C18 1.401(7) . ? C17 H17 0.9500 . ? C18 C19 1.349(7) . ? C18 H18 0.9500 . ? C19 C20 1.422(6) . ? C19 H19 0.9500 . ? C20 C21 1.396(6) . ? C21 C22 1.374(7) . ? C21 H21 0.9500 . ? C22 C23 1.434(6) . ? C22 C27 1.449(6) . ? C23 C24 1.335(8) . ? C23 H23 0.9500 . ? C24 C25 1.413(8) . ? C24 H24 0.9500 . ? C25 C26 1.362(6) . ? C25 H25 0.9500 . ? C26 C27 1.431(6) . ? C26 H26 0.9500 . ? C28 C29 1.522(6) . ? C29 C30 1.408(6) . ? C30 C31 1.386(6) . ? C30 H30 0.9500 . ? C31 C32 1.534(7) . ? C33 C34 1.502(7) . ? C34 C35 1.381(7) . ? C35 C36 1.455(5) . ? C35 C36' 1.463(6) . ? C35 H35 0.9500 . ? C36 C37 1.466(6) . ? C37 F11 1.325(5) . ? C37 F10 1.329(5) . ? C37 F12 1.332(5) . ? C36' C37' 1.463(6) . ? C37' F11' 1.314(12) . ? C37' F12' 1.318(12) . ? C37' F10' 1.320(12) . ? C38 C39 1.537(7) . ? C39 C40 1.398(6) . ? C40 C41 1.399(7) . ? C40 H40 0.9500 . ? C41 C42 1.489(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 O1 Nd1 O2 70.57(10) . . ? O1 Nd1 O4 88.95(9) . . ? O2 Nd1 O4 89.43(10) . . ? O1 Nd1 O3 141.01(12) . . ? O2 Nd1 O3 76.95(13) . . ? O4 Nd1 O3 69.44(10) . . ? O1 Nd1 O6 145.98(12) . . ? O2 Nd1 O6 142.46(12) . . ? O4 Nd1 O6 97.35(11) . . ? O3 Nd1 O6 71.20(14) . . ? O1 Nd1 O5 79.81(10) . . ? O2 Nd1 O5 144.99(10) . . ? O4 Nd1 O5 71.39(10) . . ? O3 Nd1 O5 119.95(12) . . ? O6 Nd1 O5 70.82(11) . . ? O1 Nd1 N2 110.26(10) . . ? O2 Nd1 N2 75.45(10) . . ? O4 Nd1 N2 149.15(10) . . ? O3 Nd1 N2 80.89(10) . . ? O6 Nd1 N2 80.30(11) . . ? O5 Nd1 N2 134.10(10) . . ? O1 Nd1 N1 73.32(10) . . ? O2 Nd1 N1 109.95(11) . . ? O4 Nd1 N1 146.61(11) . . ? O3 Nd1 N1 139.98(11) . . ? O6 Nd1 N1 83.75(12) . . ? O5 Nd1 N1 77.66(10) . . ? N2 Nd1 N1 64.11(10) . . ? C29 O1 Nd1 135.3(3) . . ? C31 O2 Nd1 134.7(3) . . ? C36 O3 C36' 26.7(12) . . ? C36 O3 Nd1 133.8(4) . . ? C36' O3 Nd1 137.4(7) . . ? C34 O4 Nd1 137.0(3) . . ? C39 O5 Nd1 125.8(3) . . ? C41 O6 Nd1 129.0(3) . . ? C1 N1 C5 118.1(3) . . ? C1 N1 Nd1 121.3(3) . . ? C5 N1 Nd1 116.9(3) . . ? C6 N2 C12 105.0(3) . . ? C6 N2 Nd1 118.7(3) . . ? C12 N2 Nd1 135.4(2) . . ? C6 N3 C7 106.5(3) . . ? C6 N3 C13 131.0(3) . . ? C7 N3 C13 121.2(3) . . ? N1 C1 C2 122.8(4) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 118.8(4) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 118.9(4) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 119.2(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 121.8(4) . . ? N1 C5 C6 114.1(3) . . ? C4 C5 C6 124.1(4) . . ? N2 C6 N3 112.9(4) . . ? N2 C6 C5 120.8(4) . . ? N3 C6 C5 126.3(3) . . ? C8 C7 C12 122.7(4) . . ? C8 C7 N3 131.3(4) . . ? C12 C7 N3 105.9(4) . . ? C9 C8 C7 116.5(4) . . ? C9 C8 H8 121.8 . . ? C7 C8 H8 121.8 . . ? C8 C9 C10 121.7(4) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C11 C10 C9 121.1(4) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 118.1(4) . . ? C10 C11 H11 121.0 . . ? C12 C11 H11 121.0 . . ? N2 C12 C7 109.7(3) . . ? N2 C12 C11 130.4(4) . . ? C7 C12 C11 119.9(4) . . ? N3 C13 C14 115.2(3) . . ? N3 C13 H13A 108.5 . . ? C14 C13 H13A 108.5 . . ? N3 C13 H13B 108.5 . . ? C14 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C15 C14 C27 120.0(4) . . ? C15 C14 C13 119.9(4) . . ? C27 C14 C13 120.1(4) . . ? C14 C15 C20 120.2(4) . . ? C14 C15 C16 122.8(4) . . ? C20 C15 C16 117.0(4) . . ? C17 C16 C15 120.9(4) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 120.7(5) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C19 C18 C17 121.0(5) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 120.8(4) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 122.0(4) . . ? C21 C20 C15 118.5(4) . . ? C19 C20 C15 119.5(4) . . ? C22 C21 C20 122.3(4) . . ? C22 C21 H21 118.8 . . ? C20 C21 H21 118.8 . . ? C21 C22 C23 121.5(5) . . ? C21 C22 C27 119.9(4) . . ? C23 C22 C27 118.5(5) . . ? C24 C23 C22 121.7(5) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 C25 120.2(5) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 121.1(5) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 121.2(5) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C14 C27 C26 124.0(4) . . ? C14 C27 C22 118.8(4) . . ? C26 C27 C22 117.1(4) . . ? F2 C28 F1 107.8(4) . . ? F2 C28 F3 107.6(4) . . ? F1 C28 F3 107.0(3) . . ? F2 C28 C29 110.4(3) . . ? F1 C28 C29 113.9(4) . . ? F3 C28 C29 109.8(4) . . ? O1 C29 C30 127.1(4) . . ? O1 C29 C28 114.3(4) . . ? C30 C29 C28 118.6(4) . . ? C31 C30 C29 120.8(4) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? O2 C31 C30 127.8(4) . . ? O2 C31 C32 115.1(4) . . ? C30 C31 C32 117.1(4) . . ? F4 C32 F6 108.3(4) . . ? F4 C32 F5 106.9(5) . . ? F6 C32 F5 105.8(4) . . ? F4 C32 C31 112.1(5) . . ? F6 C32 C31 110.9(4) . . ? F5 C32 C31 112.5(4) . . ? F7 C33 F9' 119.6(7) . . ? F7 C33 F9 109.8(4) . . ? F9' C33 F9 52.0(5) . . ? F7 C33 F8' 32.4(4) . . ? F9' C33 F8' 105.2(5) . . ? F9 C33 F8' 126.2(7) . . ? F7 C33 F7' 69.5(5) . . ? F9' C33 F7' 102.5(5) . . ? F9 C33 F7' 53.7(4) . . ? F8' C33 F7' 100.7(5) . . ? F7 C33 F8 104.3(4) . . ? F9' C33 F8 51.1(5) . . ? F9 C33 F8 103.1(4) . . ? F8' C33 F8 73.3(5) . . ? F7' C33 F8 147.2(6) . . ? F7 C33 C34 113.1(4) . . ? F9' C33 C34 126.6(6) . . ? F9 C33 C34 116.4(4) . . ? F8' C33 C34 115.2(7) . . ? F7' C33 C34 102.8(6) . . ? F8 C33 C34 109.0(4) . . ? O4 C34 C35 127.6(5) . . ? O4 C34 C33 115.6(4) . . ? C35 C34 C33 116.7(4) . . ? C34 C35 C36 120.9(5) . . ? C34 C35 C36' 119.2(9) . . ? C36 C35 C36' 23.5(12) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C36' C35 H35 115.7 . . ? O3 C36 C35 122.9(6) . . ? O3 C36 C37 117.4(4) . . ? C35 C36 C37 117.1(5) . . ? F11 C37 F10 106.4(4) . . ? F11 C37 F12 105.8(4) . . ? F10 C37 F12 105.8(5) . . ? F11 C37 C36 116.0(5) . . ? F10 C37 C36 111.9(6) . . ? F12 C37 C36 110.3(5) . . ? O3 C36' C35 118.3(13) . . ? O3 C36' C37' 114.7(8) . . ? C35 C36' C37' 124.5(13) . . ? F11' C37' F12' 100.8(11) . . ? F11' C37' F10' 100.6(11) . . ? F12' C37' F10' 100.2(11) . . ? F11' C37' C36' 116.9(14) . . ? F12' C37' C36' 113.7(17) . . ? F10' C37' C36' 121.4(11) . . ? F15 C38 F13 107.4(4) . . ? F15 C38 F14 107.1(4) . . ? F13 C38 F14 108.1(4) . . ? F15 C38 C39 110.9(4) . . ? F13 C38 C39 111.3(4) . . ? F14 C38 C39 111.9(4) . . ? O5 C39 C40 128.3(5) . . ? O5 C39 C38 115.1(4) . . ? C40 C39 C38 116.6(4) . . ? C39 C40 C41 121.8(4) . . ? C39 C40 H40 119.1 . . ? C41 C40 H40 119.1 . . ? O6 C41 C40 127.2(5) . . ? O6 C41 C42 118.2(5) . . ? C40 C41 C42 114.6(4) . . ? F17' C42 F18 122.7(10) . . ? F17' C42 F16' 107.4(6) . . ? F18 C42 F16' 61.3(6) . . ? F17' C42 F17 28.1(6) . . ? F18 C42 F17 106.8(4) . . ? F16' C42 F17 123.0(8) . . ? F17' C42 F18' 104.4(6) . . ? F18 C42 F18' 43.5(5) . . ? F16' C42 F18' 104.1(6) . . ? F17 C42 F18' 77.6(6) . . ? F17' C42 F16 75.5(6) . . ? F18 C42 F16 103.1(4) . . ? F16' C42 F16 43.4(6) . . ? F17 C42 F16 101.7(4) . . ? F18' C42 F16 141.2(7) . . ? F17' C42 C41 116.2(10) . . ? F18 C42 C41 116.0(5) . . ? F16' C42 C41 121.3(8) . . ? F17 C42 C41 113.8(5) . . ? F18' C42 C41 101.0(7) . . ? F16 C42 C41 113.9(5) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.127 _refine_diff_density_min -1.172 _refine_diff_density_rms 0.126 #===END data_imw190m _database_code_depnum_ccdc_archive 'CCDC 633722' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H22 F18 Gd N3 O6' _chemical_formula_weight 1163.88 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6188(11) _cell_length_b 12.9157(11) _cell_length_c 13.4422(12) _cell_angle_alpha 79.8840(10) _cell_angle_beta 77.7500(10) _cell_angle_gamma 88.0070(10) _cell_volume 2107.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7160 _cell_measurement_theta_min 4.828 _cell_measurement_theta_max 55.069 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1138 _exptl_absorpt_coefficient_mu 1.706 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5414 _exptl_absorpt_correction_T_max 0.7720 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _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 'BRUKER CCD SMART area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24419 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.61 _reflns_number_total 9504 _reflns_number_gt 8381 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER XSCANS' _computing_cell_refinement 'BRUKER XSCANS' _computing_data_reduction 'BRUKER SHELXTL' _computing_structure_solution 'BRUKER SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL' _computing_publication_material 'BRUKER SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+5.2003P] 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 9504 _refine_ls_number_parameters 614 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1493 _refine_ls_wR_factor_gt 0.1426 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.074 _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 Gd1 Gd 0.200713(18) 0.223576(18) 0.208068(16) 0.03146(10) Uani 1 1 d . . . F1 F 0.5425(3) 0.0876(4) 0.4109(4) 0.0781(13) Uani 1 1 d . . . F2 F 0.4982(4) -0.0400(4) 0.3489(4) 0.0780(13) Uani 1 1 d . . . F3 F 0.5579(4) 0.1011(5) 0.2485(4) 0.110(2) Uani 1 1 d . . . F4 F 0.0636(3) 0.0631(3) 0.5863(3) 0.0595(9) Uani 1 1 d . . . F5 F 0.1992(3) 0.1126(3) 0.6393(3) 0.0587(9) Uani 1 1 d . . . F6 F 0.0948(4) 0.2283(3) 0.5753(3) 0.0696(12) Uani 1 1 d . . . F7 F -0.2187(8) 0.2812(6) 0.2451(6) 0.153(4) Uani 1 1 d . . . F8 F -0.2137(4) 0.1674(5) 0.1498(4) 0.0860(15) Uani 1 1 d . . . F9 F -0.1901(7) 0.1292(6) 0.3059(5) 0.146(3) Uani 1 1 d . . . F10 F 0.0174(8) -0.1039(8) 0.0743(8) 0.157(3) Uiso 1 1 d . . . F11 F 0.0626(5) -0.1479(5) 0.2208(5) 0.1003(17) Uiso 1 1 d D . . F13 F 0.3739(9) 0.2280(8) -0.1529(9) 0.102(5) Uiso 0.556(17) 1 d PD A 1 F13' F 0.370(3) 0.0207(16) -0.064(2) 0.214(14) Uiso 0.444(17) 1 d PD A 2 F12 F -0.0446(9) -0.0384(9) 0.1590(9) 0.060(4) Uiso 0.342(14) 1 d PD A 1 F12' F 0.1471(16) -0.1254(18) 0.0816(17) 0.250(11) Uiso 0.658(14) 1 d PD A 2 F16 F 0.0739(10) 0.3433(9) -0.1664(8) 0.105(3) Uiso 0.588(9) 1 d PDU B 1 F17 F -0.0160(9) 0.4262(10) -0.1065(10) 0.116(3) Uiso 0.588(9) 1 d PDU B 1 F18 F 0.1420(7) 0.4663(6) -0.1151(7) 0.071(2) Uiso 0.588(9) 1 d PDU B 1 F16' F 0.1366(14) 0.3235(12) -0.1444(12) 0.108(3) Uiso 0.412(9) 1 d PDU A 2 F17' F -0.0261(10) 0.3540(12) -0.0410(11) 0.097(4) Uiso 0.412(9) 1 d PDU B 2 F18' F 0.0964(11) 0.4833(8) -0.0865(9) 0.067(3) Uiso 0.412(9) 1 d PDU B 2 F14 F 0.4550(5) 0.1038(10) -0.1066(7) 0.182(5) Uani 1 1 d D . . F15 F 0.3189(5) 0.0870(6) -0.1791(4) 0.114(2) Uani 1 1 d D . . O1 O 0.3504(3) 0.1340(3) 0.2607(3) 0.0384(8) Uani 1 1 d . . . O2 O 0.1559(3) 0.1695(3) 0.3874(3) 0.0365(7) Uani 1 1 d . . . O3 O 0.0062(3) 0.2263(3) 0.2437(3) 0.0447(9) Uani 1 1 d . . . O4 O 0.1440(4) 0.3303(4) 0.0663(3) 0.0561(11) Uani 1 1 d . . . O5 O 0.3005(4) 0.1739(3) 0.0525(3) 0.0509(10) Uani 1 1 d . . . O6 O 0.1370(3) 0.0584(3) 0.1907(3) 0.0454(9) Uani 1 1 d . . . N1 N 0.3499(3) 0.3582(3) 0.1591(3) 0.0314(8) Uani 1 1 d . . . N2 N 0.4274(3) 0.5023(3) 0.1840(3) 0.0307(8) Uani 1 1 d . . . N3 N 0.1583(3) 0.3910(3) 0.2888(3) 0.0341(8) Uani 1 1 d . . . C1 C 0.4601(4) 0.3575(4) 0.1130(4) 0.0331(10) Uani 1 1 d . B . C2 C 0.5210(4) 0.2852(4) 0.0595(4) 0.0399(11) Uani 1 1 d . . . H2 H 0.4894 0.2227 0.0503 0.048 Uiso 1 1 calc R A . C3 C 0.6300(5) 0.3082(5) 0.0200(4) 0.0438(12) Uani 1 1 d . . . H3 H 0.6740 0.2601 -0.0166 0.053 Uiso 1 1 calc R . . C4 C 0.6770(4) 0.4005(5) 0.0327(4) 0.0446(12) Uani 1 1 d . . . H4 H 0.7516 0.4140 0.0033 0.054 Uiso 1 1 calc R A . C5 C 0.6181(4) 0.4722(5) 0.0867(4) 0.0410(11) Uani 1 1 d . B . H5 H 0.6502 0.5343 0.0960 0.049 Uiso 1 1 calc R . . C6 C 0.5085(4) 0.4486(4) 0.1271(3) 0.0330(10) Uani 1 1 d . B . C7 C 0.3342(4) 0.4459(4) 0.1985(3) 0.0301(9) Uani 1 1 d . B . C8 C 0.2251(4) 0.4749(4) 0.2495(4) 0.0308(9) Uani 1 1 d . B . C9 C 0.1911(4) 0.5761(4) 0.2558(4) 0.0350(10) Uani 1 1 d . . . H9 H 0.2370 0.6338 0.2209 0.042 Uiso 1 1 calc R A . C10 C 0.0891(4) 0.5932(4) 0.3138(4) 0.0410(11) Uani 1 1 d . . . H10 H 0.0651 0.6626 0.3210 0.049 Uiso 1 1 calc R . . C11 C 0.0231(4) 0.5076(5) 0.3608(4) 0.0430(12) Uani 1 1 d . . . H11 H -0.0461 0.5164 0.4029 0.052 Uiso 1 1 calc R A . C12 C 0.0606(4) 0.4082(5) 0.3448(4) 0.0426(12) Uani 1 1 d . . . H12 H 0.0144 0.3495 0.3752 0.051 Uiso 1 1 calc R . . C13 C 0.4528(4) 0.5911(4) 0.2316(4) 0.0374(11) Uani 1 1 d . . . H13A H 0.4372 0.6578 0.1882 0.045 Uiso 1 1 calc R . . H13B H 0.5314 0.5900 0.2309 0.045 Uiso 1 1 calc R . . C14 C 0.3909(4) 0.5909(4) 0.3419(4) 0.0351(10) Uani 1 1 d . . . C15 C 0.3920(4) 0.5000(4) 0.4172(4) 0.0403(11) Uani 1 1 d . . . C16 C 0.4603(5) 0.4115(4) 0.3987(5) 0.0465(13) Uani 1 1 d . . . H16 H 0.5066 0.4118 0.3330 0.056 Uiso 1 1 calc R A . C17 C 0.4590(8) 0.3262(6) 0.4758(7) 0.074(3) Uani 1 1 d . . . H17 H 0.5058 0.2688 0.4624 0.089 Uiso 1 1 calc R . . C18 C 0.3916(9) 0.3207(8) 0.5728(7) 0.087(3) Uani 1 1 d . . . H18 H 0.3916 0.2598 0.6240 0.104 Uiso 1 1 calc R A . C19 C 0.3259(8) 0.4027(9) 0.5941(6) 0.082(3) Uani 1 1 d . . . H19 H 0.2792 0.3981 0.6602 0.099 Uiso 1 1 calc R . . C20 C 0.3255(5) 0.4958(6) 0.5192(5) 0.0573(18) Uani 1 1 d . . . C21 C 0.2626(6) 0.5816(8) 0.5412(6) 0.071(2) Uani 1 1 d . . . H21 H 0.2163 0.5776 0.6074 0.085 Uiso 1 1 calc R . . C22 C 0.2649(5) 0.6724(7) 0.4707(7) 0.066(2) Uani 1 1 d . . . C23 C 0.1989(6) 0.7624(10) 0.4934(10) 0.097(4) Uani 1 1 d . . . H23 H 0.1528 0.7588 0.5597 0.117 Uiso 1 1 calc R . . C24 C 0.2008(7) 0.8499(10) 0.4246(13) 0.113(5) Uani 1 1 d . . . H24 H 0.1552 0.9070 0.4419 0.136 Uiso 1 1 calc R A . C25 C 0.2694(7) 0.8589(6) 0.3265(10) 0.091(3) Uani 1 1 d . . . H25 H 0.2716 0.9230 0.2790 0.109 Uiso 1 1 calc R . . C26 C 0.3326(6) 0.7772(5) 0.2986(7) 0.0637(19) Uani 1 1 d . . . H26 H 0.3778 0.7848 0.2315 0.076 Uiso 1 1 calc R A . C27 C 0.3320(4) 0.6797(5) 0.3688(5) 0.0487(14) Uani 1 1 d . . . C28 C 0.4957(5) 0.0640(5) 0.3367(5) 0.0490(13) Uani 1 1 d . . . C29 C 0.3787(4) 0.1061(4) 0.3449(4) 0.0375(11) Uani 1 1 d . . . C30 C 0.3164(4) 0.1064(4) 0.4439(4) 0.0396(11) Uani 1 1 d . . . H30 H 0.3476 0.0851 0.5027 0.047 Uiso 1 1 calc R . . C31 C 0.2088(4) 0.1378(4) 0.4564(4) 0.0343(10) Uani 1 1 d . . . C32 C 0.1409(5) 0.1353(5) 0.5661(4) 0.0431(12) Uani 1 1 d . . . C33 C 0.0764(5) 0.3838(6) -0.0843(5) 0.0612(18) Uani 1 1 d D . . C37 C -0.1707(5) 0.1992(5) 0.2223(5) 0.0502(14) Uani 1 1 d . A . C38 C 0.0633(7) -0.0789(5) 0.1371(5) 0.067(2) Uani 1 1 d D A . C42 C 0.3572(6) 0.1231(7) -0.1085(6) 0.078(3) Uani 1 1 d D A . C34 C 0.0650(8) 0.3327(8) 0.0283(8) 0.0430(16) Uiso 0.580(6) 1 d PU A 1 C35 C -0.0326(8) 0.2812(7) 0.0725(7) 0.0403(16) Uiso 0.580(6) 1 d PU A 1 H35 H -0.0838 0.2753 0.0312 0.048 Uiso 0.580(6) 1 calc PR A 1 C36 C -0.0559(7) 0.2380(7) 0.1776(7) 0.0368(17) Uiso 0.580(6) 1 d PU A 1 C39 C 0.1421(8) 0.0141(8) 0.1164(8) 0.0439(17) Uiso 0.580(6) 1 d PU A 1 C40 C 0.2085(8) 0.0330(8) 0.0200(8) 0.0465(18) Uiso 0.580(6) 1 d PU A 1 H40 H 0.2043 -0.0109 -0.0288 0.056 Uiso 0.580(6) 1 calc PR A 1 C41 C 0.2829(9) 0.1169(9) -0.0068(9) 0.046(2) Uiso 0.580(6) 1 d PU A 1 C34' C 0.1484(12) 0.3042(11) -0.0260(11) 0.047(2) Uiso 0.420(6) 1 d PU A 2 C35' C 0.2152(12) 0.2381(11) -0.0797(12) 0.048(2) Uiso 0.420(6) 1 d PU A 2 H35' H 0.2129 0.2374 -0.1498 0.058 Uiso 0.420(6) 1 calc PR A 2 C36' C 0.2864(12) 0.1721(13) -0.0332(12) 0.048(3) Uiso 0.420(6) 1 d PU A 2 C39' C 0.0648(11) 0.0229(11) 0.1691(11) 0.044(2) Uiso 0.420(6) 1 d PU A 2 C40' C -0.0351(11) 0.0741(11) 0.1703(11) 0.045(2) Uiso 0.420(6) 1 d PU A 2 H40' H -0.0886 0.0465 0.1418 0.054 Uiso 0.420(6) 1 calc PR A 2 C41' C -0.0561(11) 0.1648(11) 0.2128(11) 0.043(2) Uiso 0.420(6) 1 d PU A 2 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 Gd1 0.03583(15) 0.03568(15) 0.02375(13) -0.00657(9) -0.00572(9) -0.00797(9) F1 0.048(2) 0.100(3) 0.099(3) -0.039(3) -0.029(2) 0.016(2) F2 0.060(2) 0.063(3) 0.112(4) -0.022(2) -0.017(2) 0.019(2) F3 0.048(2) 0.165(6) 0.078(3) 0.047(3) 0.016(2) 0.028(3) F4 0.050(2) 0.080(3) 0.0405(18) 0.0018(17) 0.0011(15) -0.0163(18) F5 0.057(2) 0.089(3) 0.0283(15) -0.0048(16) -0.0097(14) -0.0002(19) F6 0.092(3) 0.062(2) 0.045(2) -0.0148(18) 0.0085(19) 0.022(2) F7 0.225(9) 0.153(6) 0.117(5) -0.075(5) -0.093(6) 0.128(6) F8 0.060(3) 0.135(4) 0.074(3) -0.024(3) -0.030(2) -0.023(3) F9 0.219(8) 0.145(6) 0.074(4) 0.023(4) -0.042(4) -0.127(6) F14 0.071(4) 0.300(12) 0.180(8) -0.140(8) 0.044(5) -0.023(6) F15 0.115(5) 0.164(6) 0.079(4) -0.076(4) -0.013(3) -0.001(4) O1 0.0405(19) 0.0400(19) 0.0317(17) -0.0066(14) -0.0006(14) 0.0009(15) O2 0.0357(17) 0.0439(19) 0.0272(16) -0.0021(14) -0.0033(13) -0.0017(15) O3 0.041(2) 0.058(2) 0.039(2) -0.0134(17) -0.0116(16) -0.0088(17) O4 0.052(2) 0.084(3) 0.032(2) 0.001(2) -0.0168(18) -0.006(2) O5 0.060(2) 0.060(3) 0.0335(19) -0.0214(18) 0.0014(17) -0.020(2) O6 0.054(2) 0.043(2) 0.039(2) -0.0151(16) -0.0006(17) -0.0183(17) N1 0.032(2) 0.034(2) 0.0262(18) -0.0026(15) -0.0031(15) -0.0043(16) N2 0.0292(19) 0.035(2) 0.0280(19) -0.0030(16) -0.0077(15) -0.0043(15) N3 0.036(2) 0.035(2) 0.0300(19) -0.0061(16) -0.0018(16) -0.0104(16) C1 0.036(2) 0.037(2) 0.025(2) 0.0004(18) -0.0066(18) -0.0036(19) C2 0.043(3) 0.045(3) 0.030(2) -0.005(2) -0.004(2) -0.003(2) C3 0.042(3) 0.053(3) 0.032(3) -0.003(2) -0.004(2) 0.005(2) C4 0.033(3) 0.061(3) 0.036(3) 0.000(2) -0.004(2) 0.000(2) C5 0.034(3) 0.051(3) 0.036(3) 0.000(2) -0.008(2) -0.008(2) C6 0.035(2) 0.037(2) 0.024(2) 0.0032(18) -0.0066(18) -0.0041(19) C7 0.033(2) 0.032(2) 0.025(2) -0.0011(17) -0.0073(17) -0.0055(18) C8 0.030(2) 0.037(2) 0.026(2) -0.0050(18) -0.0072(17) -0.0059(18) C9 0.033(2) 0.037(2) 0.037(2) -0.003(2) -0.0109(19) -0.0088(19) C10 0.037(3) 0.043(3) 0.047(3) -0.013(2) -0.013(2) 0.003(2) C11 0.033(3) 0.056(3) 0.040(3) -0.014(2) -0.002(2) -0.005(2) C12 0.036(3) 0.049(3) 0.040(3) -0.011(2) 0.001(2) -0.009(2) C13 0.037(2) 0.034(2) 0.040(3) -0.003(2) -0.009(2) -0.012(2) C14 0.024(2) 0.039(3) 0.044(3) -0.013(2) -0.0046(19) -0.0089(18) C15 0.041(3) 0.049(3) 0.035(3) -0.010(2) -0.012(2) -0.017(2) C16 0.059(3) 0.040(3) 0.047(3) -0.004(2) -0.028(3) -0.012(2) C17 0.103(6) 0.047(4) 0.086(6) 0.011(4) -0.066(5) -0.021(4) C18 0.118(8) 0.091(6) 0.056(5) 0.030(4) -0.052(5) -0.064(6) C19 0.095(6) 0.113(7) 0.041(4) 0.008(4) -0.024(4) -0.066(6) C20 0.055(3) 0.086(5) 0.034(3) -0.013(3) -0.008(3) -0.040(3) C21 0.050(4) 0.114(7) 0.055(4) -0.046(4) 0.006(3) -0.039(4) C22 0.038(3) 0.088(5) 0.086(5) -0.057(5) -0.007(3) -0.014(3) C23 0.046(4) 0.124(8) 0.147(10) -0.105(8) -0.008(5) -0.005(5) C24 0.051(5) 0.098(8) 0.224(15) -0.110(10) -0.038(7) 0.017(5) C25 0.072(5) 0.051(4) 0.177(11) -0.047(5) -0.064(7) 0.010(4) C26 0.048(3) 0.044(3) 0.110(6) -0.023(4) -0.033(4) -0.002(3) C27 0.033(3) 0.052(3) 0.070(4) -0.026(3) -0.017(3) -0.008(2) C28 0.042(3) 0.056(3) 0.045(3) -0.005(3) -0.004(2) 0.005(3) C29 0.038(3) 0.036(2) 0.037(3) -0.005(2) -0.005(2) -0.001(2) C30 0.041(3) 0.047(3) 0.032(2) -0.008(2) -0.009(2) 0.002(2) C31 0.039(3) 0.035(2) 0.027(2) -0.0058(18) -0.0032(19) -0.0058(19) C32 0.042(3) 0.055(3) 0.029(2) -0.004(2) -0.003(2) 0.003(2) C33 0.060(4) 0.083(5) 0.044(3) -0.002(3) -0.022(3) -0.017(3) C37 0.046(3) 0.061(4) 0.045(3) -0.004(3) -0.015(2) -0.006(3) C38 0.110(6) 0.061(4) 0.033(3) -0.015(3) -0.008(3) -0.043(4) C42 0.072(5) 0.105(7) 0.058(4) -0.041(4) 0.011(4) -0.032(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 Gd1 O2 2.340(3) . ? Gd1 O1 2.352(4) . ? Gd1 O6 2.372(4) . ? Gd1 O4 2.373(4) . ? Gd1 O5 2.381(4) . ? Gd1 O3 2.400(4) . ? Gd1 N1 2.509(4) . ? Gd1 N3 2.576(4) . ? F1 C28 1.344(8) . ? F2 C28 1.324(8) . ? F3 C28 1.297(7) . ? F4 C32 1.326(7) . ? F5 C32 1.336(6) . ? F6 C32 1.331(7) . ? F7 C37 1.254(9) . ? F8 C37 1.339(7) . ? F9 C37 1.298(8) . ? F9 C41' 1.895(15) . ? F10 C38 1.212(11) . ? F10 F12 1.593(15) . ? F10 F12' 1.67(2) . ? F11 C38 1.305(8) . ? F13 C42 1.385(11) . ? F13' C42 1.372(15) . ? F13' F14 1.49(3) . ? F12 C38 1.432(12) . ? F12' C38 1.345(15) . ? F16 C33 1.307(10) . ? F16 F17 1.706(16) . ? F17 C33 1.340(11) . ? F18 C33 1.325(9) . ? F16' C33 1.325(12) . ? F16' C34' 1.61(2) . ? F16' C35' 1.71(2) . ? F17' C33 1.340(11) . ? F18' C33 1.313(10) . ? F14 C42 1.254(10) . ? F15 C42 1.312(8) . ? O1 C29 1.248(6) . ? O2 C31 1.258(6) . ? O3 C36 1.291(10) . ? O3 C41' 1.310(14) . ? O4 C34 1.210(11) . ? O4 C34' 1.332(15) . ? O5 C36' 1.207(16) . ? O5 C41 1.233(11) . ? O6 C39' 1.146(14) . ? O6 C39 1.225(11) . ? N1 C7 1.324(6) . ? N1 C1 1.398(6) . ? N2 C7 1.365(6) . ? N2 C6 1.385(6) . ? N2 C13 1.483(6) . ? N3 C12 1.335(7) . ? N3 C8 1.355(6) . ? C1 C2 1.390(7) . ? C1 C6 1.404(7) . ? C2 C3 1.388(8) . ? C2 H2 0.9500 . ? C3 C4 1.402(9) . ? C3 H3 0.9500 . ? C4 C5 1.377(8) . ? C4 H4 0.9500 . ? C5 C6 1.398(7) . ? C5 H5 0.9500 . ? C7 C8 1.470(7) . ? C8 C9 1.373(7) . ? C9 C10 1.389(7) . ? C9 H9 0.9500 . ? C10 C11 1.383(8) . ? C10 H10 0.9500 . ? C11 C12 1.389(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.521(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C27 1.404(8) . ? C14 C15 1.411(8) . ? C15 C16 1.433(9) . ? C15 C20 1.441(8) . ? C16 C17 1.371(9) . ? C16 H16 0.9500 . ? C17 C18 1.389(14) . ? C17 H17 0.9500 . ? C18 C19 1.354(15) . ? C18 H18 0.9500 . ? C19 C20 1.427(12) . ? C19 H19 0.9500 . ? C20 C21 1.378(12) . ? C21 C22 1.369(13) . ? C21 H21 0.9500 . ? C22 C27 1.438(10) . ? C22 C23 1.446(12) . ? C23 C24 1.325(18) . ? C23 H23 0.9500 . ? C24 C25 1.405(17) . ? C24 H24 0.9500 . ? C25 C26 1.357(11) . ? C25 H25 0.9500 . ? C26 C27 1.435(10) . ? C26 H26 0.9500 . ? C28 C29 1.544(8) . ? C29 C30 1.395(7) . ? C30 C31 1.388(7) . ? C30 H30 0.9500 . ? C31 C32 1.535(7) . ? C33 C34 1.520(12) . ? C33 C34' 1.565(16) . ? C37 C41' 1.484(15) . ? C37 C36 1.511(11) . ? C38 C39' 1.456(15) . ? C38 C39 1.535(12) . ? C42 C36' 1.422(17) . ? C42 C41 1.475(13) . ? C34 C35 1.385(14) . ? C35 C36 1.397(13) . ? C35 H35 0.9500 . ? C39 C40 1.373(14) . ? C40 C41 1.406(15) . ? C40 H40 0.9500 . ? C34' C35' 1.37(2) . ? C35' C36' 1.39(2) . ? C35' H35' 0.9500 . ? C39' C40' 1.402(19) . ? C40' C41' 1.386(19) . ? C40' H40' 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Gd1 O1 71.69(12) . . ? O2 Gd1 O6 88.08(13) . . ? O1 Gd1 O6 87.49(14) . . ? O2 Gd1 O4 143.82(14) . . ? O1 Gd1 O4 143.52(14) . . ? O6 Gd1 O4 99.08(16) . . ? O2 Gd1 O5 142.86(15) . . ? O1 Gd1 O5 77.15(14) . . ? O6 Gd1 O5 70.62(13) . . ? O4 Gd1 O5 71.53(17) . . ? O2 Gd1 O3 77.47(13) . . ? O1 Gd1 O3 142.97(13) . . ? O6 Gd1 O3 71.27(14) . . ? O4 Gd1 O3 71.58(14) . . ? O5 Gd1 O3 120.61(14) . . ? O2 Gd1 N1 110.80(13) . . ? O1 Gd1 N1 75.42(13) . . ? O6 Gd1 N1 148.25(13) . . ? O4 Gd1 N1 80.85(14) . . ? O5 Gd1 N1 79.49(13) . . ? O3 Gd1 N1 136.19(14) . . ? O2 Gd1 N3 73.06(13) . . ? O1 Gd1 N3 111.05(13) . . ? O6 Gd1 N3 146.77(13) . . ? O4 Gd1 N3 82.41(16) . . ? O5 Gd1 N3 138.78(14) . . ? O3 Gd1 N3 77.95(13) . . ? N1 Gd1 N3 64.96(13) . . ? C37 F9 C41' 51.3(6) . . ? C38 F10 F12 59.6(7) . . ? C38 F10 F12' 52.8(8) . . ? F12 F10 F12' 112.2(10) . . ? C42 F13' F14 51.7(9) . . ? C38 F12 F10 46.9(5) . . ? C38 F12' F10 45.8(7) . . ? C33 F16 F17 50.7(6) . . ? C33 F17 F16 49.0(5) . . ? C33 F16' C34' 63.7(9) . . ? C33 F16' C35' 112.4(13) . . ? C34' F16' C35' 48.6(9) . . ? C42 F14 F13' 59.1(9) . . ? C29 O1 Gd1 135.3(3) . . ? C31 O2 Gd1 134.9(3) . . ? C36 O3 C41' 44.3(7) . . ? C36 O3 Gd1 127.4(5) . . ? C41' O3 Gd1 125.7(6) . . ? C34 O4 C34' 57.8(8) . . ? C34 O4 Gd1 134.9(6) . . ? C34' O4 Gd1 125.8(7) . . ? C36' O5 C41 35.1(7) . . ? C36' O5 Gd1 137.3(8) . . ? C41 O5 Gd1 135.1(6) . . ? C39' O6 C39 54.7(8) . . ? C39' O6 Gd1 140.0(8) . . ? C39 O6 Gd1 133.0(5) . . ? C7 N1 C1 105.7(4) . . ? C7 N1 Gd1 118.4(3) . . ? C1 N1 Gd1 134.6(3) . . ? C7 N2 C6 106.5(4) . . ? C7 N2 C13 131.1(4) . . ? C6 N2 C13 121.4(4) . . ? C12 N3 C8 117.6(4) . . ? C12 N3 Gd1 122.0(3) . . ? C8 N3 Gd1 117.7(3) . . ? C2 C1 N1 130.7(5) . . ? C2 C1 C6 120.7(5) . . ? N1 C1 C6 108.6(4) . . ? C3 C2 C1 117.1(5) . . ? C3 C2 H2 121.5 . . ? C1 C2 H2 121.5 . . ? C2 C3 C4 121.7(5) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C5 C4 C3 121.9(5) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 116.4(5) . . ? C4 C5 H5 121.8 . . ? C6 C5 H5 121.8 . . ? N2 C6 C5 131.4(5) . . ? N2 C6 C1 106.4(4) . . ? C5 C6 C1 122.2(5) . . ? N1 C7 N2 112.8(4) . . ? N1 C7 C8 120.6(4) . . ? N2 C7 C8 126.6(4) . . ? N3 C8 C9 122.2(4) . . ? N3 C8 C7 113.2(4) . . ? C9 C8 C7 124.6(4) . . ? C8 C9 C10 119.3(5) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C10 C9 118.8(5) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 118.2(5) . . ? C10 C11 H11 120.9 . . ? C12 C11 H11 120.9 . . ? N3 C12 C11 123.4(5) . . ? N3 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? N2 C13 C14 115.1(4) . . ? N2 C13 H13A 108.5 . . ? C14 C13 H13A 108.5 . . ? N2 C13 H13B 108.5 . . ? C14 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C27 C14 C15 119.9(5) . . ? C27 C14 C13 120.6(5) . . ? C15 C14 C13 119.5(5) . . ? C14 C15 C16 123.0(5) . . ? C14 C15 C20 119.7(6) . . ? C16 C15 C20 117.3(6) . . ? C17 C16 C15 120.1(7) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 122.4(9) . . ? C16 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C19 C18 C17 119.7(7) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 121.3(8) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C21 C20 C19 122.0(8) . . ? C21 C20 C15 118.9(7) . . ? C19 C20 C15 119.1(8) . . ? C22 C21 C20 122.1(6) . . ? C22 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? C21 C22 C27 120.2(7) . . ? C21 C22 C23 122.2(9) . . ? C27 C22 C23 117.5(9) . . ? C24 C23 C22 122.0(10) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 C24 C25 120.7(8) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 120.9(10) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 121.0(9) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C14 C27 C26 123.3(6) . . ? C14 C27 C22 118.8(6) . . ? C26 C27 C22 117.9(7) . . ? F3 C28 F2 108.2(6) . . ? F3 C28 F1 107.3(6) . . ? F2 C28 F1 104.8(5) . . ? F3 C28 C29 112.1(5) . . ? F2 C28 C29 111.5(5) . . ? F1 C28 C29 112.6(5) . . ? O1 C29 C30 127.6(5) . . ? O1 C29 C28 115.1(5) . . ? C30 C29 C28 117.2(5) . . ? C31 C30 C29 119.9(5) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? O2 C31 C30 128.1(5) . . ? O2 C31 C32 112.9(4) . . ? C30 C31 C32 119.1(5) . . ? F4 C32 F6 108.6(5) . . ? F4 C32 F5 107.3(5) . . ? F6 C32 F5 107.1(5) . . ? F4 C32 C31 110.0(5) . . ? F6 C32 C31 110.4(4) . . ? F5 C32 C31 113.2(4) . . ? F16 C33 F18' 123.9(9) . . ? F16 C33 F18 106.9(8) . . ? F18' C33 F18 29.6(5) . . ? F16 C33 F16' 40.7(8) . . ? F18' C33 F16' 124.5(11) . . ? F18 C33 F16' 95.4(9) . . ? F16 C33 F17 80.3(8) . . ? F18' C33 F17 80.4(9) . . ? F18 C33 F17 100.7(8) . . ? F16' C33 F17 120.9(11) . . ? F16 C33 F17' 91.9(9) . . ? F18' C33 F17' 114.4(10) . . ? F18 C33 F17' 143.5(10) . . ? F16' C33 F17' 118.2(11) . . ? F17 C33 F17' 51.1(7) . . ? F16 C33 C34 131.1(8) . . ? F18' C33 C34 104.9(8) . . ? F18 C33 C34 115.4(7) . . ? F16' C33 C34 109.7(10) . . ? F17 C33 C34 113.3(8) . . ? F17' C33 C34 68.4(8) . . ? F16 C33 C34' 103.1(9) . . ? F18' C33 C34' 114.9(9) . . ? F18 C33 C34' 100.7(8) . . ? F16' C33 C34' 66.9(10) . . ? F17 C33 C34' 156.3(9) . . ? F17' C33 C34' 105.2(9) . . ? C34 C33 C34' 47.1(7) . . ? F7 C37 F9 106.2(8) . . ? F7 C37 F8 108.4(6) . . ? F9 C37 F8 109.3(6) . . ? F7 C37 C41' 132.7(9) . . ? F9 C37 C41' 85.6(8) . . ? F8 C37 C41' 110.3(7) . . ? F7 C37 C36 102.3(7) . . ? F9 C37 C36 119.4(7) . . ? F8 C37 C36 110.5(6) . . ? C41' C37 C36 38.2(6) . . ? F10 C38 F11 116.6(8) . . ? F10 C38 F12' 81.4(11) . . ? F11 C38 F12' 93.1(12) . . ? F10 C38 F12 73.6(8) . . ? F11 C38 F12 100.7(7) . . ? F12' C38 F12 154.8(12) . . ? F10 C38 C39' 128.6(10) . . ? F11 C38 C39' 105.0(7) . . ? F12' C38 C39' 126.5(13) . . ? F12 C38 C39' 70.0(8) . . ? F10 C38 C39 125.1(8) . . ? F11 C38 C39 116.8(7) . . ? F12' C38 C39 84.1(12) . . ? F12 C38 C39 107.6(8) . . ? C39' C38 C39 42.7(7) . . ? F14 C42 F15 116.4(8) . . ? F14 C42 F13' 69.2(14) . . ? F15 C42 F13' 87.7(14) . . ? F14 C42 F13 95.3(9) . . ? F15 C42 F13 101.1(9) . . ? F13' C42 F13 164.5(16) . . ? F14 C42 C36' 123.4(9) . . ? F15 C42 C36' 120.0(9) . . ? F13' C42 C36' 107.3(16) . . ? F13 C42 C36' 79.5(10) . . ? F14 C42 C41 115.8(8) . . ? F15 C42 C41 115.7(7) . . ? F13' C42 C41 78.2(15) . . ? F13 C42 C41 108.6(9) . . ? C36' C42 C41 29.3(6) . . ? O4 C34 C35 126.4(9) . . ? O4 C34 C33 118.1(8) . . ? C35 C34 C33 114.9(8) . . ? C34 C35 C36 120.3(9) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? O3 C36 C35 129.6(8) . . ? O3 C36 C37 114.2(7) . . ? C35 C36 C37 116.2(7) . . ? O6 C39 C40 130.1(10) . . ? O6 C39 C38 113.9(8) . . ? C40 C39 C38 115.9(8) . . ? C39 C40 C41 120.3(10) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? O5 C41 C40 125.2(10) . . ? O5 C41 C42 118.5(9) . . ? C40 C41 C42 115.4(9) . . ? O4 C34' C35' 132.0(13) . . ? O4 C34' C33 107.9(10) . . ? C35' C34' C33 118.9(12) . . ? O4 C34' F16' 155.5(12) . . ? C35' C34' F16' 69.6(10) . . ? C33 C34' F16' 49.4(7) . . ? C34' C35' C36' 120.8(14) . . ? C34' C35' F16' 61.8(9) . . ? C36' C35' F16' 175.3(14) . . ? C34' C35' H35' 119.6 . . ? C36' C35' H35' 119.6 . . ? F16' C35' H35' 57.9 . . ? O5 C36' C35' 123.7(14) . . ? O5 C36' C42 124.7(13) . . ? C35' C36' C42 109.9(13) . . ? O6 C39' C40' 123.2(13) . . ? O6 C39' C38 125.7(12) . . ? C40' C39' C38 111.1(12) . . ? C41' C40' C39' 120.1(13) . . ? C41' C40' H40' 119.9 . . ? C39' C40' H40' 119.9 . . ? O3 C41' C40' 132.3(12) . . ? O3 C41' C37 114.7(10) . . ? C40' C41' C37 112.9(11) . . ? O3 C41' F9 114.6(9) . . ? C40' C41' F9 100.9(10) . . ? C37 C41' F9 43.1(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 F12' F10 F12 C38 -2.7(11) . . . . ? F12 F10 F12' C38 3.0(12) . . . . ? O2 Gd1 O1 C29 -15.4(5) . . . . ? O6 Gd1 O1 C29 -104.2(5) . . . . ? O4 Gd1 O1 C29 153.9(5) . . . . ? O5 Gd1 O1 C29 -174.9(5) . . . . ? O3 Gd1 O1 C29 -50.5(6) . . . . ? N1 Gd1 O1 C29 102.8(5) . . . . ? N3 Gd1 O1 C29 47.5(5) . . . . ? O1 Gd1 O2 C31 16.0(5) . . . . ? O6 Gd1 O2 C31 104.0(5) . . . . ? O4 Gd1 O2 C31 -153.2(4) . . . . ? O5 Gd1 O2 C31 50.4(6) . . . . ? O3 Gd1 O2 C31 175.2(5) . . . . ? N1 Gd1 O2 C31 -49.8(5) . . . . ? N3 Gd1 O2 C31 -103.7(5) . . . . ? O2 Gd1 O3 C36 -170.0(6) . . . . ? O1 Gd1 O3 C36 -136.0(6) . . . . ? O6 Gd1 O3 C36 -77.7(6) . . . . ? O4 Gd1 O3 C36 29.0(6) . . . . ? O5 Gd1 O3 C36 -25.2(6) . . . . ? N1 Gd1 O3 C36 82.9(6) . . . . ? N3 Gd1 O3 C36 114.9(6) . . . . ? O2 Gd1 O3 C41' -114.1(8) . . . . ? O1 Gd1 O3 C41' -80.1(8) . . . . ? O6 Gd1 O3 C41' -21.9(8) . . . . ? O4 Gd1 O3 C41' 84.9(8) . . . . ? O5 Gd1 O3 C41' 30.7(8) . . . . ? N1 Gd1 O3 C41' 138.8(8) . . . . ? N3 Gd1 O3 C41' 170.8(8) . . . . ? O2 Gd1 O4 C34 -61.0(9) . . . . ? O1 Gd1 O4 C34 136.4(8) . . . . ? O6 Gd1 O4 C34 38.3(8) . . . . ? O5 Gd1 O4 C34 104.2(8) . . . . ? O3 Gd1 O4 C34 -28.4(8) . . . . ? N1 Gd1 O4 C34 -173.9(8) . . . . ? N3 Gd1 O4 C34 -108.1(8) . . . . ? O2 Gd1 O4 C34' -138.9(8) . . . . ? O1 Gd1 O4 C34' 58.5(9) . . . . ? O6 Gd1 O4 C34' -39.6(9) . . . . ? O5 Gd1 O4 C34' 26.3(8) . . . . ? O3 Gd1 O4 C34' -106.3(9) . . . . ? N1 Gd1 O4 C34' 108.2(8) . . . . ? N3 Gd1 O4 C34' 173.9(9) . . . . ? O2 Gd1 O5 C36' 135.3(12) . . . . ? O1 Gd1 O5 C36' 168.7(13) . . . . ? O6 Gd1 O5 C36' 76.9(12) . . . . ? O4 Gd1 O5 C36' -30.2(12) . . . . ? O3 Gd1 O5 C36' 24.0(13) . . . . ? N1 Gd1 O5 C36' -114.0(13) . . . . ? N3 Gd1 O5 C36' -83.9(13) . . . . ? O2 Gd1 O5 C41 83.8(9) . . . . ? O1 Gd1 O5 C41 117.2(9) . . . . ? O6 Gd1 O5 C41 25.3(9) . . . . ? O4 Gd1 O5 C41 -81.7(9) . . . . ? O3 Gd1 O5 C41 -27.5(9) . . . . ? N1 Gd1 O5 C41 -165.5(9) . . . . ? N3 Gd1 O5 C41 -135.4(9) . . . . ? O2 Gd1 O6 C39' 106.6(12) . . . . ? O1 Gd1 O6 C39' 178.4(12) . . . . ? O4 Gd1 O6 C39' -37.7(12) . . . . ? O5 Gd1 O6 C39' -104.4(12) . . . . ? O3 Gd1 O6 C39' 29.2(12) . . . . ? N1 Gd1 O6 C39' -125.0(12) . . . . ? N3 Gd1 O6 C39' 52.3(12) . . . . ? O2 Gd1 O6 C39 -170.1(8) . . . . ? O1 Gd1 O6 C39 -98.4(7) . . . . ? O4 Gd1 O6 C39 45.5(8) . . . . ? O5 Gd1 O6 C39 -21.1(7) . . . . ? O3 Gd1 O6 C39 112.4(8) . . . . ? N1 Gd1 O6 C39 -41.7(8) . . . . ? N3 Gd1 O6 C39 135.5(7) . . . . ? O2 Gd1 N1 C7 -57.9(4) . . . . ? O1 Gd1 N1 C7 -121.5(3) . . . . ? O6 Gd1 N1 C7 179.0(3) . . . . ? O4 Gd1 N1 C7 86.5(3) . . . . ? O5 Gd1 N1 C7 159.2(4) . . . . ? O3 Gd1 N1 C7 35.5(4) . . . . ? N3 Gd1 N1 C7 0.6(3) . . . . ? O2 Gd1 N1 C1 106.9(4) . . . . ? O1 Gd1 N1 C1 43.4(4) . . . . ? O6 Gd1 N1 C1 -16.1(6) . . . . ? O4 Gd1 N1 C1 -108.6(4) . . . . ? O5 Gd1 N1 C1 -35.9(4) . . . . ? O3 Gd1 N1 C1 -159.6(4) . . . . ? N3 Gd1 N1 C1 165.5(5) . . . . ? O2 Gd1 N3 C12 -62.3(4) . . . . ? O1 Gd1 N3 C12 -124.3(4) . . . . ? O6 Gd1 N3 C12 -4.2(6) . . . . ? O4 Gd1 N3 C12 90.8(4) . . . . ? O5 Gd1 N3 C12 141.2(4) . . . . ? O3 Gd1 N3 C12 18.1(4) . . . . ? N1 Gd1 N3 C12 174.2(5) . . . . ? O2 Gd1 N3 C8 136.8(4) . . . . ? O1 Gd1 N3 C8 74.8(4) . . . . ? O6 Gd1 N3 C8 -165.1(3) . . . . ? O4 Gd1 N3 C8 -70.1(4) . . . . ? O5 Gd1 N3 C8 -19.6(5) . . . . ? O3 Gd1 N3 C8 -142.8(4) . . . . ? N1 Gd1 N3 C8 13.3(3) . . . . ? C7 N1 C1 C2 -179.4(5) . . . . ? Gd1 N1 C1 C2 14.4(8) . . . . ? C7 N1 C1 C6 0.1(5) . . . . ? Gd1 N1 C1 C6 -166.1(3) . . . . ? N1 C1 C2 C3 178.4(5) . . . . ? C6 C1 C2 C3 -1.0(7) . . . . ? C1 C2 C3 C4 -0.4(8) . . . . ? C2 C3 C4 C5 1.3(8) . . . . ? C3 C4 C5 C6 -0.8(8) . . . . ? C7 N2 C6 C5 177.0(5) . . . . ? C13 N2 C6 C5 -13.1(8) . . . . ? C7 N2 C6 C1 -2.3(5) . . . . ? C13 N2 C6 C1 167.6(4) . . . . ? C4 C5 C6 N2 -179.8(5) . . . . ? C4 C5 C6 C1 -0.6(7) . . . . ? C2 C1 C6 N2 -179.1(4) . . . . ? N1 C1 C6 N2 1.4(5) . . . . ? C2 C1 C6 C5 1.5(7) . . . . ? N1 C1 C6 C5 -178.0(4) . . . . ? C1 N1 C7 N2 -1.6(5) . . . . ? Gd1 N1 C7 N2 167.3(3) . . . . ? C1 N1 C7 C8 177.2(4) . . . . ? Gd1 N1 C7 C8 -13.9(6) . . . . ? C6 N2 C7 N1 2.5(5) . . . . ? C13 N2 C7 N1 -166.0(4) . . . . ? C6 N2 C7 C8 -176.3(4) . . . . ? C13 N2 C7 C8 15.3(8) . . . . ? C12 N3 C8 C9 -7.4(7) . . . . ? Gd1 N3 C8 C9 154.4(4) . . . . ? C12 N3 C8 C7 174.0(4) . . . . ? Gd1 N3 C8 C7 -24.2(5) . . . . ? N1 C7 C8 N3 25.7(6) . . . . ? N2 C7 C8 N3 -155.6(4) . . . . ? N1 C7 C8 C9 -152.9(5) . . . . ? N2 C7 C8 C9 25.8(7) . . . . ? N3 C8 C9 C10 7.2(7) . . . . ? C7 C8 C9 C10 -174.4(5) . . . . ? C8 C9 C10 C11 -2.1(8) . . . . ? C9 C10 C11 C12 -2.2(8) . . . . ? C8 N3 C12 C11 2.7(8) . . . . ? Gd1 N3 C12 C11 -158.2(4) . . . . ? C10 C11 C12 N3 2.0(9) . . . . ? C7 N2 C13 C14 30.7(7) . . . . ? C6 N2 C13 C14 -136.3(5) . . . . ? N2 C13 C14 C27 -126.7(5) . . . . ? N2 C13 C14 C15 52.7(6) . . . . ? C27 C14 C15 C16 -172.3(5) . . . . ? C13 C14 C15 C16 8.4(7) . . . . ? C27 C14 C15 C20 5.2(7) . . . . ? C13 C14 C15 C20 -174.2(4) . . . . ? C14 C15 C16 C17 178.9(5) . . . . ? C20 C15 C16 C17 1.4(8) . . . . ? C15 C16 C17 C18 1.1(9) . . . . ? C16 C17 C18 C19 -1.4(11) . . . . ? C17 C18 C19 C20 -0.9(11) . . . . ? C18 C19 C20 C21 -177.1(7) . . . . ? C18 C19 C20 C15 3.4(10) . . . . ? C14 C15 C20 C21 -0.6(8) . . . . ? C16 C15 C20 C21 176.9(5) . . . . ? C14 C15 C20 C19 178.9(5) . . . . ? C16 C15 C20 C19 -3.5(7) . . . . ? C19 C20 C21 C22 177.7(6) . . . . ? C15 C20 C21 C22 -2.8(9) . . . . ? C20 C21 C22 C27 1.7(9) . . . . ? C20 C21 C22 C23 179.8(6) . . . . ? C21 C22 C23 C24 -179.5(8) . . . . ? C27 C22 C23 C24 -1.3(11) . . . . ? C22 C23 C24 C25 -1.2(13) . . . . ? C23 C24 C25 C26 2.3(13) . . . . ? C24 C25 C26 C27 -0.7(11) . . . . ? C15 C14 C27 C26 175.8(5) . . . . ? C13 C14 C27 C26 -4.9(8) . . . . ? C15 C14 C27 C22 -6.2(7) . . . . ? C13 C14 C27 C22 173.1(5) . . . . ? C25 C26 C27 C14 176.2(6) . . . . ? C25 C26 C27 C22 -1.8(9) . . . . ? C21 C22 C27 C14 2.8(8) . . . . ? C23 C22 C27 C14 -175.3(5) . . . . ? C21 C22 C27 C26 -179.0(6) . . . . ? C23 C22 C27 C26 2.8(8) . . . . ? Gd1 O1 C29 C30 11.3(9) . . . . ? Gd1 O1 C29 C28 -170.4(4) . . . . ? F3 C28 C29 O1 25.3(8) . . . . ? F2 C28 C29 O1 -96.2(6) . . . . ? F1 C28 C29 O1 146.4(5) . . . . ? F3 C28 C29 C30 -156.1(6) . . . . ? F2 C28 C29 C30 82.4(7) . . . . ? F1 C28 C29 C30 -35.1(8) . . . . ? O1 C29 C30 C31 1.9(9) . . . . ? C28 C29 C30 C31 -176.4(5) . . . . ? Gd1 O2 C31 C30 -12.8(8) . . . . ? Gd1 O2 C31 C32 167.4(3) . . . . ? C29 C30 C31 O2 -1.1(9) . . . . ? C29 C30 C31 C32 178.7(5) . . . . ? O2 C31 C32 F4 66.6(6) . . . . ? C30 C31 C32 F4 -113.2(5) . . . . ? O2 C31 C32 F6 -53.2(6) . . . . ? C30 C31 C32 F6 126.9(5) . . . . ? O2 C31 C32 F5 -173.3(5) . . . . ? C30 C31 C32 F5 6.9(7) . . . . ? F17 F16 C33 F18' -71.4(11) . . . . ? F17 F16 C33 F18 -98.4(9) . . . . ? F17 F16 C33 F16' -176.7(15) . . . . ? F17 F16 C33 F17' 49.9(8) . . . . ? F17 F16 C33 C34 112.5(11) . . . . ? F17 F16 C33 C34' 156.0(9) . . . . ? C34' F16' C33 F16 -150.9(16) . . . . ? C35' F16' C33 F16 -151(2) . . . . ? C34' F16' C33 F18' 105.2(12) . . . . ? C35' F16' C33 F18' 104.7(13) . . . . ? C34' F16' C33 F18 99.3(8) . . . . ? C35' F16' C33 F18 98.8(12) . . . . ? C34' F16' C33 F17 -154.8(11) . . . . ? C35' F16' C33 F17 -155.2(11) . . . . ? C34' F16' C33 F17' -95.5(12) . . . . ? C35' F16' C33 F17' -95.9(15) . . . . ? C34' F16' C33 C34 -20.1(10) . . . . ? C35' F16' C33 C34 -20.5(15) . . . . ? C35' F16' C33 C34' -0.5(10) . . . . ? F16 F17 C33 F18' 127.1(9) . . . . ? F16 F17 C33 F18 105.5(8) . . . . ? F16 F17 C33 F16' 2.5(12) . . . . ? F16 F17 C33 F17' -100.4(11) . . . . ? F16 F17 C33 C34 -130.7(9) . . . . ? F16 F17 C33 C34' -100(2) . . . . ? C41' F9 C37 F7 -133.3(9) . . . . ? C41' F9 C37 F8 110.0(8) . . . . ? C41' F9 C37 C36 -18.6(7) . . . . ? F12 F10 C38 F11 94.0(9) . . . . ? F12' F10 C38 F11 -89.2(13) . . . . ? F12 F10 C38 F12' -176.8(13) . . . . ? F12' F10 C38 F12 176.8(13) . . . . ? F12 F10 C38 C39' -46.3(11) . . . . ? F12' F10 C38 C39' 130.5(15) . . . . ? F12 F10 C38 C39 -100.3(11) . . . . ? F12' F10 C38 C39 76.5(13) . . . . ? F10 F12' C38 F11 116.4(8) . . . . ? F10 F12' C38 F12 -7(3) . . . . ? F10 F12' C38 C39' -132.3(13) . . . . ? F10 F12' C38 C39 -126.9(8) . . . . ? F10 F12 C38 F11 -114.8(8) . . . . ? F10 F12 C38 F12' 7(3) . . . . ? F10 F12 C38 C39' 143.0(9) . . . . ? F10 F12 C38 C39 122.4(8) . . . . ? F13' F14 C42 F15 -76.3(15) . . . . ? F13' F14 C42 F13 178.4(16) . . . . ? F13' F14 C42 C36' 97.5(18) . . . . ? F13' F14 C42 C41 64.8(16) . . . . ? F14 F13' C42 F15 119.4(8) . . . . ? F14 F13' C42 F13 -6(6) . . . . ? F14 F13' C42 C36' -119.9(10) . . . . ? F14 F13' C42 C41 -123.7(10) . . . . ? C34' O4 C34 C35 124.6(14) . . . . ? Gd1 O4 C34 C35 14.3(15) . . . . ? C34' O4 C34 C33 -46.2(10) . . . . ? Gd1 O4 C34 C33 -156.5(5) . . . . ? F16 C33 C34 O4 111.6(12) . . . . ? F18' C33 C34 O4 -65.1(11) . . . . ? F18 C33 C34 O4 -35.5(12) . . . . ? F16' C33 C34 O4 70.7(13) . . . . ? F17 C33 C34 O4 -150.9(9) . . . . ? F17' C33 C34 O4 -175.8(12) . . . . ? C34' C33 C34 O4 45.2(10) . . . . ? F16 C33 C34 C35 -60.3(14) . . . . ? F18' C33 C34 C35 123.0(10) . . . . ? F18 C33 C34 C35 152.6(9) . . . . ? F16' C33 C34 C35 -101.1(12) . . . . ? F17 C33 C34 C35 37.3(12) . . . . ? F17' C33 C34 C35 12.3(10) . . . . ? C34' C33 C34 C35 -126.6(12) . . . . ? O4 C34 C35 C36 13.7(16) . . . . ? C33 C34 C35 C36 -175.2(8) . . . . ? C41' O3 C36 C35 -126.3(15) . . . . ? Gd1 O3 C36 C35 -20.7(13) . . . . ? C41' O3 C36 C37 54.1(10) . . . . ? Gd1 O3 C36 C37 159.7(4) . . . . ? C34 C35 C36 O3 -9.2(15) . . . . ? C34 C35 C36 C37 170.4(8) . . . . ? F7 C37 C36 O3 93.8(8) . . . . ? F9 C37 C36 O3 -22.9(11) . . . . ? F8 C37 C36 O3 -151.0(7) . . . . ? C41' C37 C36 O3 -53.9(10) . . . . ? F7 C37 C36 C35 -85.8(9) . . . . ? F9 C37 C36 C35 157.4(8) . . . . ? F8 C37 C36 C35 29.4(10) . . . . ? C41' C37 C36 C35 126.5(13) . . . . ? C39' O6 C39 C40 146.1(16) . . . . ? Gd1 O6 C39 C40 17.5(16) . . . . ? C39' O6 C39 C38 -35.8(10) . . . . ? Gd1 O6 C39 C38 -164.4(5) . . . . ? F10 C38 C39 O6 144.8(10) . . . . ? F11 C38 C39 O6 -49.5(11) . . . . ? F12' C38 C39 O6 -140.0(13) . . . . ? F12 C38 C39 O6 62.8(10) . . . . ? C39' C38 C39 O6 33.6(10) . . . . ? F10 C38 C39 C40 -36.8(14) . . . . ? F11 C38 C39 C40 128.9(9) . . . . ? F12' C38 C39 C40 38.4(14) . . . . ? F12 C38 C39 C40 -118.8(10) . . . . ? C39' C38 C39 C40 -148.0(14) . . . . ? O6 C39 C40 C41 -2.5(17) . . . . ? C38 C39 C40 C41 179.4(9) . . . . ? C36' O5 C41 C40 -137(2) . . . . ? Gd1 O5 C41 C40 -24.3(16) . . . . ? C36' O5 C41 C42 54.7(15) . . . . ? Gd1 O5 C41 C42 167.2(6) . . . . ? C39 C40 C41 O5 5.4(17) . . . . ? C39 C40 C41 C42 174.2(9) . . . . ? F14 C42 C41 O5 58.5(14) . . . . ? F15 C42 C41 O5 -160.2(9) . . . . ? F13' C42 C41 O5 118.2(17) . . . . ? F13 C42 C41 O5 -47.3(13) . . . . ? C36' C42 C41 O5 -54.3(15) . . . . ? F14 C42 C41 C40 -111.1(11) . . . . ? F15 C42 C41 C40 30.2(14) . . . . ? F13' C42 C41 C40 -51.3(16) . . . . ? F13 C42 C41 C40 143.1(10) . . . . ? C36' C42 C41 C40 136(2) . . . . ? C34 O4 C34' C35' -153(2) . . . . ? Gd1 O4 C34' C35' -28(2) . . . . ? C34 O4 C34' C33 40.5(8) . . . . ? Gd1 O4 C34' C33 165.6(5) . . . . ? C34 O4 C34' F16' 60(3) . . . . ? Gd1 O4 C34' F16' -175(3) . . . . ? F16 C33 C34' O4 -171.5(9) . . . . ? F18' C33 C34' O4 50.8(13) . . . . ? F18 C33 C34' O4 78.2(11) . . . . ? F16' C33 C34' O4 169.5(14) . . . . ? F17 C33 C34' O4 -76(2) . . . . ? F17' C33 C34' O4 -75.9(12) . . . . ? C34 C33 C34' O4 -36.7(8) . . . . ? F16 C33 C34' C35' 19.6(15) . . . . ? F18' C33 C34' C35' -118.1(14) . . . . ? F18 C33 C34' C35' -90.7(14) . . . . ? F16' C33 C34' C35' 0.6(14) . . . . ? F17 C33 C34' C35' 115(2) . . . . ? F17' C33 C34' C35' 115.2(14) . . . . ? C34 C33 C34' C35' 154.4(17) . . . . ? F16 C33 C34' F16' 19.0(11) . . . . ? F18' C33 C34' F16' -118.7(12) . . . . ? F18 C33 C34' F16' -91.3(10) . . . . ? F17 C33 C34' F16' 115(2) . . . . ? F17' C33 C34' F16' 114.6(12) . . . . ? C34 C33 C34' F16' 153.8(13) . . . . ? C33 F16' C34' O4 -25(3) . . . . ? C35' F16' C34' O4 155(3) . . . . ? C33 F16' C34' C35' -179.4(13) . . . . ? C35' F16' C34' C33 179.4(13) . . . . ? O4 C34' C35' C36' 9(3) . . . . ? C33 C34' C35' C36' 175.1(13) . . . . ? F16' C34' C35' C36' 175.6(17) . . . . ? O4 C34' C35' F16' -166.2(19) . . . . ? C33 C34' C35' F16' -0.5(11) . . . . ? C33 F16' C35' C34' 0.6(12) . . . . ? C33 F16' C35' C36' -125(17) . . . . ? C34' F16' C35' C36' -126(17) . . . . ? C41 O5 C36' C35' 132(2) . . . . ? Gd1 O5 C36' C35' 26(2) . . . . ? C41 O5 C36' C42 -64.7(17) . . . . ? Gd1 O5 C36' C42 -170.5(7) . . . . ? C34' C35' C36' O5 -6(2) . . . . ? F16' C35' C36' O5 118(17) . . . . ? C34' C35' C36' C42 -171.5(13) . . . . ? F16' C35' C36' C42 -48(18) . . . . ? F14 C42 C36' O5 -21(2) . . . . ? F15 C42 C36' O5 152.2(13) . . . . ? F13' C42 C36' O5 55(2) . . . . ? F13 C42 C36' O5 -110.9(16) . . . . ? C41 C42 C36' O5 62.4(17) . . . . ? F14 C42 C36' C35' 143.9(13) . . . . ? F15 C42 C36' C35' -42.5(17) . . . . ? F13' C42 C36' C35' -139.9(18) . . . . ? F13 C42 C36' C35' 54.4(12) . . . . ? C41 C42 C36' C35' -132(2) . . . . ? C39 O6 C39' C40' -135.9(18) . . . . ? Gd1 O6 C39' C40' -19(2) . . . . ? C39 O6 C39' C38 44.0(11) . . . . ? Gd1 O6 C39' C38 161.1(6) . . . . ? F10 C38 C39' O6 -144.6(13) . . . . ? F11 C38 C39' O6 71.6(15) . . . . ? F12' C38 C39' O6 -34(2) . . . . ? F12 C38 C39' O6 167.8(16) . . . . ? C39 C38 C39' O6 -41.8(11) . . . . ? F10 C38 C39' C40' 35.3(17) . . . . ? F11 C38 C39' C40' -108.5(11) . . . . ? F12' C38 C39' C40' 145.9(16) . . . . ? F12 C38 C39' C40' -12.3(11) . . . . ? C39 C38 C39' C40' 138.1(16) . . . . ? O6 C39' C40' C41' -10(2) . . . . ? C38 C39' C40' C41' 170.5(12) . . . . ? C36 O3 C41' C40' 122(2) . . . . ? Gd1 O3 C41' C40' 13(2) . . . . ? C36 O3 C41' C37 -56.0(10) . . . . ? Gd1 O3 C41' C37 -165.4(6) . . . . ? C36 O3 C41' F9 -103.6(12) . . . . ? Gd1 O3 C41' F9 146.9(6) . . . . ? C39' C40' C41' O3 11(2) . . . . ? C39' C40' C41' C37 -171.2(12) . . . . ? C39' C40' C41' F9 -127.8(12) . . . . ? F7 C37 C41' O3 7.8(17) . . . . ? F9 C37 C41' O3 -100.2(10) . . . . ? F8 C37 C41' O3 150.8(9) . . . . ? C36 C37 C41' O3 53.1(10) . . . . ? F7 C37 C41' C40' -170.7(10) . . . . ? F9 C37 C41' C40' 81.2(11) . . . . ? F8 C37 C41' C40' -27.8(13) . . . . ? C36 C37 C41' C40' -125.5(16) . . . . ? F7 C37 C41' F9 108.0(11) . . . . ? F8 C37 C41' F9 -109.0(7) . . . . ? C36 C37 C41' F9 153.3(10) . . . . ? C37 F9 C41' O3 100.6(11) . . . . ? C37 F9 C41' C40' -112.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.325 _refine_diff_density_min -1.288 _refine_diff_density_rms 0.138 #===END data_imw362m _database_code_depnum_ccdc_archive 'CCDC 633723' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H22 Er F18 N3 O6' _chemical_formula_weight 1173.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.810(4) _cell_length_b 12.924(4) _cell_length_c 13.320(4) _cell_angle_alpha 101.129(5) _cell_angle_beta 101.725(5) _cell_angle_gamma 91.392(5) _cell_volume 2113.9(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8687 _cell_measurement_theta_min 4.398 _cell_measurement_theta_max 56.754 _exptl_crystal_description block _exptl_crystal_colour clear _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1146 _exptl_absorpt_coefficient_mu 2.117 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.4629 _exptl_absorpt_correction_T_max 0.6648 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _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 'Bruker SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18158 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.53 _reflns_number_total 9387 _reflns_number_gt 7433 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.1170P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9387 _refine_ls_number_parameters 612 _refine_ls_number_restraints 275 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1574 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.19923(2) 0.213155(19) 0.29156(2) 0.02698(12) Uani 1 1 d . . . F1 F 0.1975(4) 0.1042(4) -0.1426(3) 0.0581(12) Uani 1 1 d . . . F2 F 0.0580(4) 0.0587(5) -0.0922(4) 0.0674(14) Uani 1 1 d . . . F3 F 0.1059(5) 0.2238(4) -0.0739(4) 0.0775(17) Uani 1 1 d . . . F4 F 0.4757(5) -0.0453(5) 0.1034(7) 0.110(3) Uani 1 1 d . . . F5 F 0.5106(7) 0.0305(8) 0.2576(5) 0.140(4) Uani 1 1 d . . . F6 F 0.5427(5) 0.1052(6) 0.1393(9) 0.142(4) Uani 1 1 d . . . F7 F 0.3957(8) 0.1720(8) 0.6960(7) 0.083(3) Uiso 0.521(7) 1 d PDU A 1 F8 F 0.4389(7) 0.0771(7) 0.5681(8) 0.073(3) Uiso 0.521(7) 1 d PDU A 1 F9 F 0.3040(8) 0.0324(7) 0.6203(9) 0.083(3) Uiso 0.521(7) 1 d PDU A 1 F7' F 0.4494(7) 0.1593(9) 0.6470(9) 0.086(3) Uiso 0.479(7) 1 d PDU A 2 F8' F 0.3725(10) 0.0216(7) 0.5475(9) 0.086(3) Uiso 0.479(7) 1 d PDU A 2 F9' F 0.3142(8) 0.0887(7) 0.6787(7) 0.060(2) Uiso 0.479(7) 1 d PDU A 2 F10 F 0.0965(6) 0.3720(6) 0.6852(5) 0.106(2) Uani 1 1 d . A . F11 F -0.0183(5) 0.3548(5) 0.5483(6) 0.0881(19) Uani 1 1 d . A . F12 F 0.1045(5) 0.4782(4) 0.5837(6) 0.090(2) Uani 1 1 d . A . F13 F -0.2143(5) 0.1723(6) 0.3466(6) 0.106(2) Uani 1 1 d . . . F14 F -0.2188(5) 0.1454(6) 0.1827(6) 0.099(2) Uani 1 1 d . . . F15 F -0.1664(6) 0.2964(5) 0.2758(7) 0.108(3) Uani 1 1 d . . . F16 F -0.0091(7) -0.1114(5) 0.4114(6) 0.110(3) Uani 1 1 d . . . F17 F 0.1558(7) -0.0942(7) 0.4317(8) 0.149(4) Uani 1 1 d . . . F18 F 0.0593(6) -0.1647(4) 0.2804(5) 0.091(2) Uani 1 1 d . . . O1 O 0.1568(4) 0.1640(4) 0.1126(4) 0.0346(10) Uani 1 1 d . . . O2 O 0.3402(4) 0.1267(3) 0.2408(4) 0.0331(10) Uani 1 1 d . . . O3 O 0.0122(4) 0.2065(4) 0.2532(4) 0.0375(11) Uani 1 1 d . . . O4 O 0.1382(4) 0.0468(4) 0.3034(4) 0.0450(12) Uani 1 1 d . . . O5 O 0.1435(4) 0.3145(4) 0.4329(4) 0.0395(11) Uani 1 1 d . . . O6 O 0.2958(4) 0.1676(4) 0.4435(4) 0.0372(11) Uani 1 1 d . . . N1 N 0.1593(4) 0.3774(4) 0.2197(4) 0.0313(12) Uani 1 1 d . . . N2 N 0.3476(4) 0.3484(4) 0.3433(4) 0.0279(11) Uani 1 1 d . . . N3 N 0.4279(4) 0.4980(4) 0.3251(4) 0.0315(12) Uani 1 1 d . . . C1 C 0.0646(6) 0.3909(6) 0.1641(6) 0.0409(13) Uani 1 1 d U . . H1 H 0.0167 0.3306 0.1333 0.049 Uiso 1 1 calc R . . C2 C 0.0319(6) 0.4902(6) 0.1487(6) 0.0409(11) Uani 1 1 d U . . H2 H -0.0349 0.4965 0.1047 0.049 Uiso 1 1 calc R . . C3 C 0.0967(6) 0.5765(6) 0.1973(6) 0.0399(11) Uani 1 1 d U . . H3 H 0.0737 0.6448 0.1912 0.048 Uiso 1 1 calc R . . C4 C 0.1976(5) 0.5660(5) 0.2565(6) 0.0364(10) Uani 1 1 d U . . H4 H 0.2440 0.6261 0.2923 0.044 Uiso 1 1 calc R . . C5 C 0.2277(5) 0.4638(5) 0.2611(6) 0.0324(10) Uani 1 1 d U . . C6 C 0.3339(5) 0.4380(5) 0.3092(5) 0.0303(11) Uani 1 1 d U . . C7 C 0.5070(5) 0.4428(5) 0.3751(5) 0.0340(10) Uani 1 1 d U . . C8 C 0.6167(5) 0.4670(6) 0.4108(6) 0.0378(11) Uani 1 1 d U . . H8 H 0.6505 0.5307 0.4037 0.045 Uiso 1 1 calc R . . C9 C 0.6736(6) 0.3919(6) 0.4576(6) 0.0416(11) Uani 1 1 d U . . H9 H 0.7484 0.4053 0.4841 0.050 Uiso 1 1 calc R . . C10 C 0.6240(6) 0.2972(6) 0.4670(6) 0.0413(11) Uani 1 1 d U . . H10 H 0.6661 0.2478 0.4984 0.050 Uiso 1 1 calc R . . C11 C 0.5161(6) 0.2744(6) 0.4318(6) 0.0377(11) Uani 1 1 d U . . H11 H 0.4826 0.2103 0.4382 0.045 Uiso 1 1 calc R . . C12 C 0.4573(5) 0.3494(5) 0.3861(5) 0.0334(10) Uani 1 1 d U . . C13 C 0.4535(6) 0.5877(5) 0.2787(6) 0.0380(12) Uani 1 1 d U B . H13A H 0.5313 0.5920 0.2817 0.046 Uiso 1 1 calc R . . H13B H 0.4366 0.6535 0.3224 0.046 Uiso 1 1 calc R . . C14 C 0.3954(6) 0.5830(5) 0.1659(6) 0.0396(11) Uiso 1 1 d U . . C15 C 0.4051(14) 0.4820(12) 0.0864(15) 0.0384(14) Uiso 0.545(8) 1 d PU B 1 C16 C 0.4763(13) 0.4044(14) 0.1146(15) 0.0391(17) Uiso 0.545(8) 1 d PU B 1 H16 H 0.5199 0.4149 0.1830 0.047 Uiso 0.545(8) 1 calc PR B 1 C17 C 0.4814(12) 0.3139(11) 0.0421(12) 0.0400(17) Uiso 0.545(8) 1 d PU B 1 H17 H 0.5286 0.2623 0.0618 0.048 Uiso 0.545(8) 1 calc PR B 1 C18 C 0.4191(13) 0.2958(12) -0.0599(13) 0.0423(17) Uiso 0.545(8) 1 d PU B 1 H18 H 0.4238 0.2326 -0.1084 0.051 Uiso 0.545(8) 1 calc PR B 1 C19 C 0.3520(13) 0.3694(13) -0.0886(12) 0.0401(17) Uiso 0.545(8) 1 d PU B 1 H19 H 0.3083 0.3568 -0.1571 0.048 Uiso 0.545(8) 1 calc PR B 1 C20 C 0.3462(12) 0.4684(11) -0.0150(12) 0.0390(15) Uiso 0.545(8) 1 d PU B 1 C21 C 0.2793(12) 0.5441(12) -0.0480(12) 0.0390(16) Uiso 0.545(8) 1 d PU B 1 H21 H 0.2366 0.5306 -0.1170 0.047 Uiso 0.545(8) 1 calc PR B 1 C22 C 0.2749(11) 0.6366(13) 0.0177(14) 0.0381(15) Uiso 0.545(8) 1 d PU B 1 C23 C 0.2089(11) 0.7216(11) -0.0128(13) 0.0421(16) Uiso 0.545(8) 1 d PU B 1 H23 H 0.1700 0.7136 -0.0829 0.051 Uiso 0.545(8) 1 calc PR B 1 C24 C 0.2028(12) 0.8116(14) 0.0578(14) 0.0438(17) Uiso 0.545(8) 1 d PU B 1 H24 H 0.1553 0.8621 0.0360 0.053 Uiso 0.545(8) 1 calc PR B 1 C25 C 0.2608(12) 0.8329(11) 0.1575(14) 0.0439(16) Uiso 0.545(8) 1 d PU B 1 H25 H 0.2559 0.8973 0.2043 0.053 Uiso 0.545(8) 1 calc PR B 1 C26 C 0.3276(12) 0.7566(11) 0.1886(13) 0.0409(16) Uiso 0.545(8) 1 d PU B 1 H26 H 0.3718 0.7719 0.2569 0.049 Uiso 0.545(8) 1 calc PR B 1 C27 C 0.3331(12) 0.6584(11) 0.1241(12) 0.0375(15) Uiso 0.545(8) 1 d PU B 1 C15' C 0.3900(16) 0.5018(14) 0.0909(18) 0.0386(15) Uiso 0.455(8) 1 d PU B 2 C16' C 0.4518(15) 0.4083(17) 0.0995(18) 0.0387(16) Uiso 0.455(8) 1 d PU B 2 H16' H 0.4964 0.4056 0.1652 0.046 Uiso 0.455(8) 1 calc PR B 2 C17' C 0.4484(15) 0.3286(14) 0.0210(16) 0.0406(16) Uiso 0.455(8) 1 d PU B 2 H17' H 0.4914 0.2713 0.0320 0.049 Uiso 0.455(8) 1 calc PR B 2 C18' C 0.3848(16) 0.3246(16) -0.0773(15) 0.0408(18) Uiso 0.455(8) 1 d PU B 2 H18' H 0.3844 0.2659 -0.1328 0.049 Uiso 0.455(8) 1 calc PR B 2 C19' C 0.3218(15) 0.4079(14) -0.0929(14) 0.0411(17) Uiso 0.455(8) 1 d PU B 2 H19' H 0.2766 0.4041 -0.1598 0.049 Uiso 0.455(8) 1 calc PR B 2 C20' C 0.3215(14) 0.5008(14) -0.0120(14) 0.0390(15) Uiso 0.455(8) 1 d PU B 2 C21' C 0.2658(14) 0.5857(16) -0.0265(16) 0.0389(17) Uiso 0.455(8) 1 d PU B 2 H21' H 0.2196 0.5842 -0.0924 0.047 Uiso 0.455(8) 1 calc PR B 2 C22' C 0.2739(13) 0.6755(14) 0.0523(15) 0.0392(15) Uiso 0.455(8) 1 d PU B 2 C23' C 0.2046(14) 0.7611(16) 0.0325(17) 0.0424(18) Uiso 0.455(8) 1 d PU B 2 H23' H 0.1574 0.7557 -0.0335 0.051 Uiso 0.455(8) 1 calc PR B 2 C24' C 0.2082(15) 0.8480(14) 0.1089(17) 0.0443(18) Uiso 0.455(8) 1 d PU B 2 H24' H 0.1643 0.9042 0.0959 0.053 Uiso 0.455(8) 1 calc PR B 2 C25' C 0.2796(14) 0.8556(14) 0.2116(16) 0.0433(18) Uiso 0.455(8) 1 d PU B 2 H25' H 0.2841 0.9182 0.2635 0.052 Uiso 0.455(8) 1 calc PR B 2 C26' C 0.3400(15) 0.7733(13) 0.2332(16) 0.0411(17) Uiso 0.455(8) 1 d PU B 2 H26' H 0.3833 0.7786 0.3012 0.049 Uiso 0.455(8) 1 calc PR B 2 C27' C 0.3392(15) 0.6816(13) 0.1575(15) 0.0385(15) Uiso 0.455(8) 1 d PU B 2 C28 C 0.1418(6) 0.1285(6) -0.0681(6) 0.0425(13) Uani 1 1 d U . . C29 C 0.2065(6) 0.1293(6) 0.0428(6) 0.0380(11) Uani 1 1 d U . . C30 C 0.3068(6) 0.0915(6) 0.0544(6) 0.0391(11) Uani 1 1 d U . . H30 H 0.3355 0.0652 -0.0052 0.047 Uiso 1 1 calc R . . C31 C 0.3661(6) 0.0925(6) 0.1557(6) 0.0399(11) Uani 1 1 d U . . C32 C 0.4765(6) 0.0479(6) 0.1654(6) 0.0446(13) Uani 1 1 d U . . C33 C 0.3556(5) 0.1129(5) 0.6032(5) 0.0474(14) Uani 1 1 d DU . . C34 C 0.2859(7) 0.1737(7) 0.5333(6) 0.0477(12) Uani 1 1 d U A . C35 C 0.2192(7) 0.2432(7) 0.5823(7) 0.0509(12) Uani 1 1 d U . . H35 H 0.2200 0.2472 0.6545 0.061 Uiso 1 1 calc R A . C36 C 0.1526(7) 0.3055(7) 0.5272(6) 0.0483(12) Uani 1 1 d U A . C37 C 0.0825(7) 0.3796(7) 0.5866(6) 0.0485(14) Uani 1 1 d U . . C38 C -0.1629(7) 0.1950(7) 0.2752(7) 0.0551(15) Uani 1 1 d U . . C39 C -0.0515(7) 0.1578(7) 0.2879(7) 0.0532(13) Uani 1 1 d U . . C40 C -0.0334(7) 0.0660(7) 0.3328(7) 0.0542(13) Uani 1 1 d U . . H40 H -0.0860 0.0393 0.3640 0.065 Uiso 1 1 calc R . . C41 C 0.0600(7) 0.0167(7) 0.3307(7) 0.0544(13) Uani 1 1 d U . . C42 C 0.0639(8) -0.0907(7) 0.3639(7) 0.0558(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 Er1 0.02973(18) 0.03099(16) 0.02180(17) 0.00652(11) 0.00861(12) -0.00287(11) F1 0.056(3) 0.093(4) 0.024(2) 0.006(2) 0.012(2) 0.002(3) F2 0.050(3) 0.108(4) 0.034(3) -0.001(3) 0.002(2) -0.019(3) F3 0.104(5) 0.085(4) 0.039(3) 0.018(3) -0.002(3) 0.028(3) F4 0.083(4) 0.088(4) 0.154(8) -0.009(4) 0.044(5) 0.039(4) F5 0.127(6) 0.256(10) 0.064(5) 0.063(6) 0.037(4) 0.139(7) F6 0.034(3) 0.135(6) 0.293(13) 0.120(7) 0.043(5) 0.019(4) F10 0.113(5) 0.161(7) 0.057(4) 0.025(4) 0.037(4) 0.061(5) F11 0.057(3) 0.098(4) 0.118(6) 0.025(4) 0.033(4) 0.015(3) F12 0.116(5) 0.047(3) 0.120(6) -0.006(3) 0.074(4) 0.007(3) F13 0.078(4) 0.148(6) 0.130(7) 0.061(5) 0.074(5) 0.026(4) F14 0.070(4) 0.110(5) 0.104(6) 0.023(4) -0.011(4) -0.027(4) F15 0.120(6) 0.080(4) 0.151(8) 0.033(4) 0.077(5) 0.038(4) F16 0.176(8) 0.075(4) 0.094(5) 0.024(4) 0.065(5) -0.029(4) F17 0.122(7) 0.165(8) 0.161(9) 0.123(7) -0.048(6) -0.030(6) F18 0.146(6) 0.052(3) 0.074(4) 0.009(3) 0.025(4) -0.001(3) O1 0.033(2) 0.043(2) 0.023(2) -0.0023(19) 0.004(2) 0.0008(19) O2 0.038(3) 0.039(2) 0.023(2) 0.0071(19) 0.007(2) 0.0043(19) O3 0.031(2) 0.047(3) 0.038(3) 0.014(2) 0.013(2) -0.004(2) O4 0.044(3) 0.038(2) 0.052(3) 0.016(2) 0.006(3) -0.013(2) O5 0.040(3) 0.053(3) 0.027(3) 0.004(2) 0.015(2) 0.003(2) O6 0.039(3) 0.048(3) 0.027(3) 0.011(2) 0.009(2) -0.001(2) N1 0.029(3) 0.035(3) 0.032(3) 0.012(2) 0.005(2) -0.004(2) N2 0.026(3) 0.031(2) 0.028(3) 0.005(2) 0.010(2) -0.001(2) N3 0.024(3) 0.035(3) 0.037(3) 0.002(2) 0.013(2) -0.002(2) C1 0.033(3) 0.044(2) 0.050(3) 0.018(2) 0.012(2) -0.002(2) C2 0.032(2) 0.045(2) 0.051(3) 0.018(2) 0.013(2) 0.0029(19) C3 0.032(2) 0.042(2) 0.050(3) 0.015(2) 0.015(2) 0.0052(18) C4 0.030(2) 0.038(2) 0.045(3) 0.010(2) 0.016(2) 0.0018(18) C5 0.031(2) 0.035(2) 0.036(2) 0.0092(19) 0.016(2) 0.0006(18) C6 0.030(2) 0.033(2) 0.032(3) 0.008(2) 0.015(2) -0.002(2) C7 0.031(2) 0.040(2) 0.032(2) 0.0036(19) 0.011(2) 0.0010(18) C8 0.032(2) 0.047(2) 0.034(2) 0.004(2) 0.011(2) -0.0013(19) C9 0.034(2) 0.053(2) 0.037(2) 0.006(2) 0.009(2) 0.0003(19) C10 0.036(2) 0.052(2) 0.036(2) 0.008(2) 0.008(2) 0.003(2) C11 0.036(2) 0.045(2) 0.033(2) 0.0082(19) 0.009(2) 0.0034(19) C12 0.032(2) 0.040(2) 0.030(2) 0.0048(19) 0.0120(19) 0.0015(17) C13 0.036(2) 0.037(2) 0.043(2) 0.008(2) 0.013(2) -0.001(2) C28 0.041(3) 0.055(3) 0.030(3) 0.005(2) 0.007(2) 0.003(2) C29 0.038(2) 0.048(2) 0.028(2) 0.007(2) 0.009(2) 0.001(2) C30 0.039(2) 0.052(2) 0.028(2) 0.008(2) 0.0103(19) 0.005(2) C31 0.039(2) 0.051(2) 0.031(2) 0.010(2) 0.009(2) 0.006(2) C32 0.042(3) 0.058(3) 0.034(3) 0.008(2) 0.009(2) 0.010(2) C33 0.045(3) 0.066(3) 0.035(3) 0.015(3) 0.012(3) 0.001(3) C34 0.046(3) 0.065(3) 0.036(3) 0.015(2) 0.013(2) 0.004(2) C35 0.050(3) 0.067(3) 0.037(3) 0.009(2) 0.012(2) 0.006(2) C36 0.049(3) 0.062(3) 0.036(3) 0.007(2) 0.015(2) 0.005(2) C37 0.049(3) 0.063(3) 0.034(3) 0.005(3) 0.016(3) 0.003(3) C38 0.055(3) 0.061(3) 0.053(3) 0.007(3) 0.025(3) -0.008(3) C39 0.056(3) 0.060(3) 0.046(3) 0.007(2) 0.022(3) -0.009(2) C40 0.060(3) 0.060(3) 0.044(3) 0.009(2) 0.019(3) -0.015(2) C41 0.063(3) 0.058(3) 0.043(3) 0.012(2) 0.015(3) -0.014(2) C42 0.067(4) 0.058(3) 0.042(3) 0.015(3) 0.011(3) -0.017(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 Er1 O1 2.292(5) . ? Er1 O2 2.295(4) . ? Er1 O4 2.315(5) . ? Er1 O5 2.326(5) . ? Er1 O6 2.334(5) . ? Er1 O3 2.342(5) . ? Er1 N2 2.446(5) . ? Er1 N1 2.515(5) . ? F1 C28 1.331(8) . ? F2 C28 1.331(9) . ? F3 C28 1.336(9) . ? F4 C32 1.320(10) . ? F5 C32 1.282(10) . ? F6 C32 1.257(10) . ? F7 C33 1.317(6) . ? F8 C33 1.310(6) . ? F9 C33 1.301(6) . ? F7' C33 1.300(6) . ? F8' C33 1.315(6) . ? F9' C33 1.312(6) . ? F10 C37 1.312(10) . ? F11 C37 1.296(10) . ? F12 C37 1.309(10) . ? F13 C38 1.333(10) . ? F14 C38 1.325(11) . ? F15 C38 1.311(10) . ? F16 C42 1.281(11) . ? F17 C42 1.338(11) . ? F18 C42 1.310(11) . ? O1 C29 1.251(8) . ? O2 C31 1.248(8) . ? O3 C39 1.232(9) . ? O4 C41 1.213(10) . ? O5 C36 1.266(9) . ? O6 C34 1.217(9) . ? N1 C1 1.321(9) . ? N1 C5 1.355(8) . ? N2 C6 1.327(8) . ? N2 C12 1.403(8) . ? N3 C6 1.372(8) . ? N3 C7 1.387(8) . ? N3 C13 1.475(8) . ? C1 C2 1.399(9) . ? C1 H1 0.9500 . ? C2 C3 1.345(11) . ? C2 H2 0.9500 . ? C3 C4 1.396(10) . ? C3 H3 0.9500 . ? C4 C5 1.394(9) . ? C4 H4 0.9500 . ? C5 C6 1.457(9) . ? C7 C8 1.396(9) . ? C7 C12 1.397(9) . ? C8 C9 1.395(10) . ? C8 H8 0.9500 . ? C9 C10 1.403(10) . ? C9 H9 0.9500 . ? C10 C11 1.372(10) . ? C10 H10 0.9500 . ? C11 C12 1.398(9) . ? C11 H11 0.9500 . ? C13 C14 1.523(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15' 1.29(2) . ? C14 C27 1.401(16) . ? C14 C27' 1.491(18) . ? C14 C15 1.539(17) . ? C15 C20 1.38(2) . ? C15 C16 1.43(2) . ? C16 C17 1.38(2) . ? C16 H16 0.9500 . ? C17 C18 1.40(2) . ? C17 H17 0.9500 . ? C18 C19 1.35(2) . ? C18 H18 0.9500 . ? C19 C20 1.47(2) . ? C19 H19 0.9500 . ? C20 C21 1.393(19) . ? C21 C22 1.348(19) . ? C21 H21 0.9500 . ? C22 C27 1.43(2) . ? C22 C23 1.470(19) . ? C23 C24 1.36(2) . ? C23 H23 0.9500 . ? C24 C25 1.36(2) . ? C24 H24 0.9500 . ? C25 C26 1.39(2) . ? C25 H25 0.9500 . ? C26 C27 1.401(19) . ? C26 H26 0.9500 . ? C15' C20' 1.47(3) . ? C15' C16' 1.47(2) . ? C16' C17' 1.31(3) . ? C16' H16' 0.9500 . ? C17' C18' 1.39(3) . ? C17' H17' 0.9500 . ? C18' C19' 1.38(2) . ? C18' H18' 0.9500 . ? C19' C20' 1.45(2) . ? C19' H19' 0.9500 . ? C20' C21' 1.35(2) . ? C21' C22' 1.39(2) . ? C21' H21' 0.9500 . ? C22' C27' 1.46(3) . ? C22' C23' 1.47(2) . ? C23' C24' 1.35(3) . ? C23' H23' 0.9500 . ? C24' C25' 1.47(3) . ? C24' H24' 0.9500 . ? C25' C26' 1.37(2) . ? C25' H25' 0.9500 . ? C26' C27' 1.40(2) . ? C26' H26' 0.9500 . ? C28 C29 1.538(10) . ? C29 C30 1.375(10) . ? C30 C31 1.405(10) . ? C30 H30 0.9500 . ? C31 C32 1.530(10) . ? C33 C34 1.502(11) . ? C34 C35 1.415(11) . ? C35 C36 1.387(11) . ? C35 H35 0.9500 . ? C36 C37 1.546(11) . ? C38 C39 1.505(12) . ? C39 C40 1.431(12) . ? C40 C41 1.372(12) . ? C40 H40 0.9500 . ? C41 C42 1.536(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Er1 O2 72.80(16) . . ? O1 Er1 O4 89.52(18) . . ? O2 Er1 O4 84.10(18) . . ? O1 Er1 O5 142.48(16) . . ? O2 Er1 O5 143.94(17) . . ? O4 Er1 O5 99.77(19) . . ? O1 Er1 O6 143.69(16) . . ? O2 Er1 O6 75.19(16) . . ? O4 Er1 O6 70.45(18) . . ? O5 Er1 O6 72.57(17) . . ? O1 Er1 O3 76.88(17) . . ? O2 Er1 O3 141.54(17) . . ? O4 Er1 O3 72.45(17) . . ? O5 Er1 O3 71.65(17) . . ? O6 Er1 O3 121.94(16) . . ? O1 Er1 N2 109.26(17) . . ? O2 Er1 N2 75.83(16) . . ? O4 Er1 N2 146.47(18) . . ? O5 Er1 N2 82.29(17) . . ? O6 Er1 N2 78.52(17) . . ? O3 Er1 N2 137.66(16) . . ? O1 Er1 N1 72.46(17) . . ? O2 Er1 N1 114.61(16) . . ? O4 Er1 N1 147.33(18) . . ? O5 Er1 N1 80.88(18) . . ? O6 Er1 N1 138.20(18) . . ? O3 Er1 N1 76.95(16) . . ? N2 Er1 N1 66.19(17) . . ? C29 O1 Er1 135.5(5) . . ? C31 O2 Er1 135.7(5) . . ? C39 O3 Er1 129.1(5) . . ? C41 O4 Er1 131.7(6) . . ? C36 O5 Er1 132.3(5) . . ? C34 O6 Er1 136.8(5) . . ? C1 N1 C5 118.0(6) . . ? C1 N1 Er1 122.5(4) . . ? C5 N1 Er1 117.4(4) . . ? C6 N2 C12 105.8(5) . . ? C6 N2 Er1 118.1(4) . . ? C12 N2 Er1 134.7(4) . . ? C6 N3 C7 106.3(5) . . ? C6 N3 C13 130.1(6) . . ? C7 N3 C13 121.9(5) . . ? N1 C1 C2 122.7(7) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.0(7) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 120.1(6) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 117.4(6) . . ? C5 C4 H4 121.3 . . ? C3 C4 H4 121.3 . . ? N1 C5 C4 122.4(6) . . ? N1 C5 C6 113.1(5) . . ? C4 C5 C6 124.6(6) . . ? N2 C6 N3 112.6(6) . . ? N2 C6 C5 120.5(6) . . ? N3 C6 C5 126.9(6) . . ? N3 C7 C8 131.1(6) . . ? N3 C7 C12 106.9(6) . . ? C8 C7 C12 122.1(6) . . ? C9 C8 C7 115.8(6) . . ? C9 C8 H8 122.1 . . ? C7 C8 H8 122.1 . . ? C8 C9 C10 122.1(7) . . ? C8 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C11 C10 C9 121.5(7) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 117.2(7) . . ? C10 C11 H11 121.4 . . ? C12 C11 H11 121.4 . . ? C7 C12 C11 121.2(6) . . ? C7 C12 N2 108.5(5) . . ? C11 C12 N2 130.3(6) . . ? N3 C13 C14 115.6(6) . . ? N3 C13 H13A 108.4 . . ? C14 C13 H13A 108.4 . . ? N3 C13 H13B 108.4 . . ? C14 C13 H13B 108.4 . . ? H13A C13 H13B 107.4 . . ? C15' C14 C27 106.8(12) . . ? C15' C14 C27' 125.4(13) . . ? C27 C14 C27' 18.6(9) . . ? C15' C14 C13 124.4(11) . . ? C27 C14 C13 128.7(8) . . ? C27' C14 C13 110.1(9) . . ? C15' C14 C15 8.8(13) . . ? C27 C14 C15 114.9(10) . . ? C27' C14 C15 133.5(11) . . ? C13 C14 C15 116.4(8) . . ? C20 C15 C16 119.7(15) . . ? C20 C15 C14 119.2(11) . . ? C16 C15 C14 121.1(15) . . ? C17 C16 C15 119.6(16) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 122.0(14) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C19 C18 C17 119.3(14) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 120.7(14) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C15 C20 C21 122.0(13) . . ? C15 C20 C19 118.6(13) . . ? C21 C20 C19 119.3(14) . . ? C22 C21 C20 120.2(14) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C27 121.9(13) . . ? C21 C22 C23 123.2(16) . . ? C27 C22 C23 114.8(15) . . ? C24 C23 C22 121.1(15) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C25 C24 C23 123.6(15) . . ? C25 C24 H24 118.2 . . ? C23 C24 H24 118.2 . . ? C24 C25 C26 117.3(16) . . ? C24 C25 H25 121.4 . . ? C26 C25 H25 121.4 . . ? C25 C26 C27 123.2(15) . . ? C25 C26 H26 118.4 . . ? C27 C26 H26 118.4 . . ? C26 C27 C14 118.9(13) . . ? C26 C27 C22 119.7(13) . . ? C14 C27 C22 121.4(11) . . ? C14 C15' C20' 119.9(14) . . ? C14 C15' C16' 124.2(19) . . ? C20' C15' C16' 115.9(17) . . ? C17' C16' C15' 123.2(19) . . ? C17' C16' H16' 118.4 . . ? C15' C16' H16' 118.4 . . ? C16' C17' C18' 122.7(17) . . ? C16' C17' H17' 118.6 . . ? C18' C17' H17' 118.6 . . ? C19' C18' C17' 118.5(17) . . ? C19' C18' H18' 120.7 . . ? C17' C18' H18' 120.7 . . ? C18' C19' C20' 123.1(17) . . ? C18' C19' H19' 118.5 . . ? C20' C19' H19' 118.5 . . ? C21' C20' C19' 124.4(19) . . ? C21' C20' C15' 119.0(16) . . ? C19' C20' C15' 116.6(15) . . ? C20' C21' C22' 121.9(17) . . ? C20' C21' H21' 119.1 . . ? C22' C21' H21' 119.1 . . ? C21' C22' C27' 122.2(15) . . ? C21' C22' C23' 118.3(17) . . ? C27' C22' C23' 119.0(17) . . ? C24' C23' C22' 119.7(17) . . ? C24' C23' H23' 120.2 . . ? C22' C23' H23' 120.2 . . ? C23' C24' C25' 120.3(17) . . ? C23' C24' H24' 119.9 . . ? C25' C24' H24' 119.9 . . ? C26' C25' C24' 120.6(17) . . ? C26' C25' H25' 119.7 . . ? C24' C25' H25' 119.7 . . ? C25' C26' C27' 121.5(19) . . ? C25' C26' H26' 119.3 . . ? C27' C26' H26' 119.3 . . ? C26' C27' C22' 118.6(16) . . ? C26' C27' C14 129.8(16) . . ? C22' C27' C14 111.5(13) . . ? F1 C28 F2 107.1(6) . . ? F1 C28 F3 106.7(6) . . ? F2 C28 F3 108.1(7) . . ? F1 C28 C29 113.9(6) . . ? F2 C28 C29 110.6(6) . . ? F3 C28 C29 110.2(6) . . ? O1 C29 C30 128.2(7) . . ? O1 C29 C28 112.8(6) . . ? C30 C29 C28 118.9(6) . . ? C29 C30 C31 119.0(7) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? O2 C31 C30 127.7(7) . . ? O2 C31 C32 114.8(6) . . ? C30 C31 C32 117.5(6) . . ? F6 C32 F5 111.7(9) . . ? F6 C32 F4 104.2(8) . . ? F5 C32 F4 104.0(8) . . ? F6 C32 C31 112.4(7) . . ? F5 C32 C31 110.9(7) . . ? F4 C32 C31 113.1(7) . . ? F7' C33 F9 132.0(10) . . ? F7' C33 F8 61.0(5) . . ? F9 C33 F8 106.9(6) . . ? F7' C33 F9' 106.5(6) . . ? F9 C33 F9' 42.3(5) . . ? F8 C33 F9' 129.6(9) . . ? F7' C33 F8' 106.1(6) . . ? F9 C33 F8' 66.0(5) . . ? F8 C33 F8' 47.4(5) . . ? F9' C33 F8' 104.9(6) . . ? F7' C33 F7 46.7(5) . . ? F9 C33 F7 105.9(6) . . ? F8 C33 F7 104.7(6) . . ? F9' C33 F7 66.0(5) . . ? F8' C33 F7 137.7(10) . . ? F7' C33 C34 114.3(8) . . ? F9 C33 C34 112.7(8) . . ? F8 C33 C34 114.2(7) . . ? F9' C33 C34 115.0(7) . . ? F8' C33 C34 109.3(8) . . ? F7 C33 C34 111.8(8) . . ? O6 C34 C35 124.4(7) . . ? O6 C34 C33 119.8(7) . . ? C35 C34 C33 115.5(7) . . ? C36 C35 C34 121.3(8) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? O5 C36 C35 128.8(7) . . ? O5 C36 C37 113.1(7) . . ? C35 C36 C37 118.1(7) . . ? F11 C37 F12 109.6(7) . . ? F11 C37 F10 104.9(7) . . ? F12 C37 F10 107.9(8) . . ? F11 C37 C36 111.4(7) . . ? F12 C37 C36 110.8(7) . . ? F10 C37 C36 112.1(7) . . ? F15 C38 F14 106.5(9) . . ? F15 C38 F13 108.7(8) . . ? F14 C38 F13 106.7(8) . . ? F15 C38 C39 113.3(7) . . ? F14 C38 C39 108.1(7) . . ? F13 C38 C39 113.2(8) . . ? O3 C39 C40 127.4(8) . . ? O3 C39 C38 116.0(8) . . ? C40 C39 C38 116.4(7) . . ? C41 C40 C39 119.8(8) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? O4 C41 C40 127.7(8) . . ? O4 C41 C42 116.6(8) . . ? C40 C41 C42 115.7(8) . . ? F16 C42 F18 109.5(8) . . ? F16 C42 F17 104.8(9) . . ? F18 C42 F17 109.0(9) . . ? F16 C42 C41 115.4(9) . . ? F18 C42 C41 108.3(7) . . ? F17 C42 C41 109.7(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 O2 Er1 O1 C29 -12.0(6) . . . . ? O4 Er1 O1 C29 -95.9(7) . . . . ? O5 Er1 O1 C29 158.5(6) . . . . ? O6 Er1 O1 C29 -41.2(8) . . . . ? O3 Er1 O1 C29 -168.0(7) . . . . ? N2 Er1 O1 C29 55.7(7) . . . . ? N1 Er1 O1 C29 111.7(7) . . . . ? O1 Er1 O2 C31 8.4(6) . . . . ? O4 Er1 O2 C31 99.7(7) . . . . ? O5 Er1 O2 C31 -161.8(6) . . . . ? O6 Er1 O2 C31 171.0(7) . . . . ? O3 Er1 O2 C31 47.9(7) . . . . ? N2 Er1 O2 C31 -107.4(7) . . . . ? N1 Er1 O2 C31 -52.4(7) . . . . ? O1 Er1 O3 C39 126.2(7) . . . . ? O2 Er1 O3 C39 87.7(7) . . . . ? O4 Er1 O3 C39 32.5(6) . . . . ? O5 Er1 O3 C39 -74.5(7) . . . . ? O6 Er1 O3 C39 -19.8(7) . . . . ? N2 Er1 O3 C39 -129.4(6) . . . . ? N1 Er1 O3 C39 -159.0(7) . . . . ? O1 Er1 O4 C41 -109.5(8) . . . . ? O2 Er1 O4 C41 177.8(8) . . . . ? O5 Er1 O4 C41 34.0(8) . . . . ? O6 Er1 O4 C41 101.4(8) . . . . ? O3 Er1 O4 C41 -33.1(7) . . . . ? N2 Er1 O4 C41 124.8(7) . . . . ? N1 Er1 O4 C41 -54.3(9) . . . . ? O1 Er1 O5 C36 150.6(6) . . . . ? O2 Er1 O5 C36 -45.0(8) . . . . ? O4 Er1 O5 C36 48.4(7) . . . . ? O6 Er1 O5 C36 -17.4(7) . . . . ? O3 Er1 O5 C36 116.1(7) . . . . ? N2 Er1 O5 C36 -97.7(7) . . . . ? N1 Er1 O5 C36 -164.7(7) . . . . ? O1 Er1 O6 C34 -146.4(7) . . . . ? O2 Er1 O6 C34 -175.2(8) . . . . ? O4 Er1 O6 C34 -86.3(8) . . . . ? O5 Er1 O6 C34 21.1(8) . . . . ? O3 Er1 O6 C34 -33.1(8) . . . . ? N2 Er1 O6 C34 106.6(8) . . . . ? N1 Er1 O6 C34 74.2(8) . . . . ? O1 Er1 N1 C1 62.4(5) . . . . ? O2 Er1 N1 C1 123.3(5) . . . . ? O4 Er1 N1 C1 3.0(7) . . . . ? O5 Er1 N1 C1 -90.9(6) . . . . ? O6 Er1 N1 C1 -141.5(5) . . . . ? O3 Er1 N1 C1 -17.7(5) . . . . ? N2 Er1 N1 C1 -176.4(6) . . . . ? O1 Er1 N1 C5 -134.3(5) . . . . ? O2 Er1 N1 C5 -73.4(5) . . . . ? O4 Er1 N1 C5 166.3(4) . . . . ? O5 Er1 N1 C5 72.4(5) . . . . ? O6 Er1 N1 C5 21.8(6) . . . . ? O3 Er1 N1 C5 145.5(5) . . . . ? N2 Er1 N1 C5 -13.1(4) . . . . ? O1 Er1 N2 C6 59.8(5) . . . . ? O2 Er1 N2 C6 125.5(5) . . . . ? O4 Er1 N2 C6 -179.4(4) . . . . ? O5 Er1 N2 C6 -83.4(5) . . . . ? O6 Er1 N2 C6 -157.1(5) . . . . ? O3 Er1 N2 C6 -31.7(6) . . . . ? N1 Er1 N2 C6 0.0(4) . . . . ? O1 Er1 N2 C12 -104.5(6) . . . . ? O2 Er1 N2 C12 -38.8(5) . . . . ? O4 Er1 N2 C12 16.2(7) . . . . ? O5 Er1 N2 C12 112.3(6) . . . . ? O6 Er1 N2 C12 38.6(5) . . . . ? O3 Er1 N2 C12 164.0(5) . . . . ? N1 Er1 N2 C12 -164.3(6) . . . . ? C5 N1 C1 C2 -1.6(11) . . . . ? Er1 N1 C1 C2 161.7(6) . . . . ? N1 C1 C2 C3 -3.9(12) . . . . ? C1 C2 C3 C4 4.0(11) . . . . ? C2 C3 C4 C5 1.1(11) . . . . ? C1 N1 C5 C4 7.0(10) . . . . ? Er1 N1 C5 C4 -157.0(5) . . . . ? C1 N1 C5 C6 -172.6(6) . . . . ? Er1 N1 C5 C6 23.3(7) . . . . ? C3 C4 C5 N1 -6.8(10) . . . . ? C3 C4 C5 C6 172.8(6) . . . . ? C12 N2 C6 N3 0.8(7) . . . . ? Er1 N2 C6 N3 -167.7(4) . . . . ? C12 N2 C6 C5 -179.0(6) . . . . ? Er1 N2 C6 C5 12.5(8) . . . . ? C7 N3 C6 N2 -1.1(7) . . . . ? C13 N3 C6 N2 163.8(6) . . . . ? C7 N3 C6 C5 178.6(6) . . . . ? C13 N3 C6 C5 -16.4(11) . . . . ? N1 C5 C6 N2 -24.1(9) . . . . ? C4 C5 C6 N2 156.2(7) . . . . ? N1 C5 C6 N3 156.1(6) . . . . ? C4 C5 C6 N3 -23.5(11) . . . . ? C6 N3 C7 C8 -179.3(7) . . . . ? C13 N3 C7 C8 14.3(11) . . . . ? C6 N3 C7 C12 0.9(7) . . . . ? C13 N3 C7 C12 -165.5(6) . . . . ? N3 C7 C8 C9 -179.5(7) . . . . ? C12 C7 C8 C9 0.3(10) . . . . ? C7 C8 C9 C10 0.9(11) . . . . ? C8 C9 C10 C11 -1.1(12) . . . . ? C9 C10 C11 C12 0.0(11) . . . . ? N3 C7 C12 C11 178.5(6) . . . . ? C8 C7 C12 C11 -1.3(10) . . . . ? N3 C7 C12 N2 -0.5(7) . . . . ? C8 C7 C12 N2 179.7(6) . . . . ? C10 C11 C12 C7 1.1(10) . . . . ? C10 C11 C12 N2 179.8(6) . . . . ? C6 N2 C12 C7 -0.2(7) . . . . ? Er1 N2 C12 C7 165.5(4) . . . . ? C6 N2 C12 C11 -179.1(7) . . . . ? Er1 N2 C12 C11 -13.4(11) . . . . ? C6 N3 C13 C14 -33.5(9) . . . . ? C7 N3 C13 C14 129.5(6) . . . . ? N3 C13 C14 C15' -49.6(15) . . . . ? N3 C13 C14 C27 125.6(10) . . . . ? N3 C13 C14 C27' 125.8(9) . . . . ? N3 C13 C14 C15 -54.0(11) . . . . ? C15' C14 C15 C20 18(9) . . . . ? C27 C14 C15 C20 -5.7(19) . . . . ? C27' C14 C15 C20 -6(2) . . . . ? C13 C14 C15 C20 173.9(12) . . . . ? C15' C14 C15 C16 -164(11) . . . . ? C27 C14 C15 C16 172.2(15) . . . . ? C27' C14 C15 C16 172.1(16) . . . . ? C13 C14 C15 C16 -8(2) . . . . ? C20 C15 C16 C17 -3(3) . . . . ? C14 C15 C16 C17 178.7(14) . . . . ? C15 C16 C17 C18 1(3) . . . . ? C16 C17 C18 C19 0(2) . . . . ? C17 C18 C19 C20 2(2) . . . . ? C16 C15 C20 C21 -177.0(16) . . . . ? C14 C15 C20 C21 1(2) . . . . ? C16 C15 C20 C19 5(2) . . . . ? C14 C15 C20 C19 -176.9(12) . . . . ? C18 C19 C20 C15 -4(2) . . . . ? C18 C19 C20 C21 177.7(14) . . . . ? C15 C20 C21 C22 4(2) . . . . ? C19 C20 C21 C22 -178.4(13) . . . . ? C20 C21 C22 C27 -4(2) . . . . ? C20 C21 C22 C23 177.8(14) . . . . ? C21 C22 C23 C24 176.6(14) . . . . ? C27 C22 C23 C24 -2(2) . . . . ? C22 C23 C24 C25 4(2) . . . . ? C23 C24 C25 C26 -2(2) . . . . ? C24 C25 C26 C27 -3(2) . . . . ? C25 C26 C27 C14 -174.0(13) . . . . ? C25 C26 C27 C22 6(2) . . . . ? C15' C14 C27 C26 -178.0(15) . . . . ? C27' C14 C27 C26 6(3) . . . . ? C13 C14 C27 C26 6.1(19) . . . . ? C15 C14 C27 C26 -174.3(13) . . . . ? C15' C14 C27 C22 2.4(19) . . . . ? C27' C14 C27 C22 -174(5) . . . . ? C13 C14 C27 C22 -173.5(10) . . . . ? C15 C14 C27 C22 6.1(18) . . . . ? C21 C22 C27 C26 178.6(14) . . . . ? C23 C22 C27 C26 -3(2) . . . . ? C21 C22 C27 C14 -2(2) . . . . ? C23 C22 C27 C14 177.0(12) . . . . ? C27 C14 C15' C20' -3(2) . . . . ? C27' C14 C15' C20' -2(3) . . . . ? C13 C14 C15' C20' 172.7(13) . . . . ? C15 C14 C15' C20' -161(11) . . . . ? C27 C14 C15' C16' 174.4(19) . . . . ? C27' C14 C15' C16' 175.8(17) . . . . ? C13 C14 C15' C16' -9(3) . . . . ? C15 C14 C15' C16' 17(8) . . . . ? C14 C15' C16' C17' -177.1(19) . . . . ? C20' C15' C16' C17' 1(3) . . . . ? C15' C16' C17' C18' -1(3) . . . . ? C16' C17' C18' C19' 0(3) . . . . ? C17' C18' C19' C20' 2(3) . . . . ? C18' C19' C20' C21' 176.0(17) . . . . ? C18' C19' C20' C15' -2(3) . . . . ? C14 C15' C20' C21' 1(3) . . . . ? C16' C15' C20' C21' -177.5(18) . . . . ? C14 C15' C20' C19' 178.5(16) . . . . ? C16' C15' C20' C19' 0(3) . . . . ? C19' C20' C21' C22' -175.8(16) . . . . ? C15' C20' C21' C22' 2(3) . . . . ? C20' C21' C22' C27' -3(3) . . . . ? C20' C21' C22' C23' -175.5(16) . . . . ? C21' C22' C23' C24' 177.9(16) . . . . ? C27' C22' C23' C24' 5(3) . . . . ? C22' C23' C24' C25' -1(3) . . . . ? C23' C24' C25' C26' -3(3) . . . . ? C24' C25' C26' C27' 3(3) . . . . ? C25' C26' C27' C22' 1(3) . . . . ? C25' C26' C27' C14 -177.8(17) . . . . ? C21' C22' C27' C26' -177.7(17) . . . . ? C23' C22' C27' C26' -5(2) . . . . ? C21' C22' C27' C14 2(2) . . . . ? C23' C22' C27' C14 173.9(14) . . . . ? C15' C14 C27' C26' -179.8(19) . . . . ? C27 C14 C27' C26' -176(5) . . . . ? C13 C14 C27' C26' 5(2) . . . . ? C15 C14 C27' C26' -175.4(17) . . . . ? C15' C14 C27' C22' 1(2) . . . . ? C27 C14 C27' C22' 5(3) . . . . ? C13 C14 C27' C22' -174.4(11) . . . . ? C15 C14 C27' C22' 5(2) . . . . ? Er1 O1 C29 C30 12.0(12) . . . . ? Er1 O1 C29 C28 -169.6(4) . . . . ? F1 C28 C29 O1 172.2(6) . . . . ? F2 C28 C29 O1 -67.2(8) . . . . ? F3 C28 C29 O1 52.3(9) . . . . ? F1 C28 C29 C30 -9.2(10) . . . . ? F2 C28 C29 C30 111.4(8) . . . . ? F3 C28 C29 C30 -129.1(7) . . . . ? O1 C29 C30 C31 -1.8(12) . . . . ? C28 C29 C30 C31 179.8(7) . . . . ? Er1 O2 C31 C30 -4.5(12) . . . . ? Er1 O2 C31 C32 174.9(5) . . . . ? C29 C30 C31 O2 -1.8(12) . . . . ? C29 C30 C31 C32 178.8(7) . . . . ? O2 C31 C32 F6 -110.1(9) . . . . ? C30 C31 C32 F6 69.3(11) . . . . ? O2 C31 C32 F5 15.8(11) . . . . ? C30 C31 C32 F5 -164.8(9) . . . . ? O2 C31 C32 F4 132.2(8) . . . . ? C30 C31 C32 F4 -48.4(10) . . . . ? Er1 O6 C34 C35 -20.1(14) . . . . ? Er1 O6 C34 C33 166.5(4) . . . . ? F7' C33 C34 O6 82.8(9) . . . . ? F9 C33 C34 O6 -107.2(8) . . . . ? F8 C33 C34 O6 15.1(10) . . . . ? F9' C33 C34 O6 -153.5(8) . . . . ? F8' C33 C34 O6 -35.9(10) . . . . ? F7 C33 C34 O6 133.7(8) . . . . ? F7' C33 C34 C35 -91.2(9) . . . . ? F9 C33 C34 C35 78.9(9) . . . . ? F8 C33 C34 C35 -158.8(7) . . . . ? F9' C33 C34 C35 32.5(10) . . . . ? F8' C33 C34 C35 150.2(8) . . . . ? F7 C33 C34 C35 -40.3(9) . . . . ? O6 C34 C35 C36 4.9(14) . . . . ? C33 C34 C35 C36 178.6(8) . . . . ? Er1 O5 C36 C35 15.0(14) . . . . ? Er1 O5 C36 C37 -168.2(5) . . . . ? C34 C35 C36 O5 -3.2(15) . . . . ? C34 C35 C36 C37 -179.8(8) . . . . ? O5 C36 C37 F11 65.4(10) . . . . ? C35 C36 C37 F11 -117.4(9) . . . . ? O5 C36 C37 F12 -56.8(10) . . . . ? C35 C36 C37 F12 120.3(9) . . . . ? O5 C36 C37 F10 -177.4(8) . . . . ? C35 C36 C37 F10 -0.3(12) . . . . ? Er1 O3 C39 C40 -22.9(13) . . . . ? Er1 O3 C39 C38 161.4(5) . . . . ? F15 C38 C39 O3 -30.2(12) . . . . ? F14 C38 C39 O3 87.6(9) . . . . ? F13 C38 C39 O3 -154.5(8) . . . . ? F15 C38 C39 C40 153.7(8) . . . . ? F14 C38 C39 C40 -88.6(9) . . . . ? F13 C38 C39 C40 29.4(12) . . . . ? O3 C39 C40 C41 -6.8(15) . . . . ? C38 C39 C40 C41 168.9(8) . . . . ? Er1 O4 C41 C40 22.1(14) . . . . ? Er1 O4 C41 C42 -159.9(5) . . . . ? C39 C40 C41 O4 7.9(15) . . . . ? C39 C40 C41 C42 -170.2(8) . . . . ? O4 C41 C42 F16 166.8(9) . . . . ? C40 C41 C42 F16 -14.9(13) . . . . ? O4 C41 C42 F18 -70.0(11) . . . . ? C40 C41 C42 F18 108.2(10) . . . . ? O4 C41 C42 F17 48.8(12) . . . . ? C40 C41 C42 F17 -132.9(10) . . . . ? _diffrn_measured_fraction_theta_max 0.872 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.008 _refine_diff_density_min -3.230 _refine_diff_density_rms 0.195 #===END data_imw352_0m _database_code_depnum_ccdc_archive 'CCDC 633724' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H22 F18 N3 O6 Yb' _chemical_formula_weight 1179.67 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.812(5) _cell_length_b 12.880(5) _cell_length_c 13.240(5) _cell_angle_alpha 101.505(5) _cell_angle_beta 101.437(5) _cell_angle_gamma 91.816(5) _cell_volume 2092.7(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8561 _cell_measurement_theta_min 5.459 _cell_measurement_theta_max 54.993 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.872 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1150 _exptl_absorpt_coefficient_mu 2.368 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6488 _exptl_absorpt_correction_T_max 0.7031 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _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 'BRUKER SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 49439 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.58 _reflns_number_total 9646 _reflns_number_gt 8936 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER XSCANS' _computing_cell_refinement 'BRUKER XSCANS' _computing_data_reduction 'BRUKER SHELXTL' _computing_structure_solution 'BRUKER SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXTL' _computing_publication_material 'BRUKER SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+7.6098P] 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 9646 _refine_ls_number_parameters 614 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.064 _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 Yb1 Yb 0.199008(12) 0.212532(12) 0.290205(12) 0.02012(6) Uani 1 1 d . . . F1 F 0.1060(3) 0.2238(3) -0.0748(2) 0.0554(9) Uani 1 1 d . . . F2 F 0.0558(2) 0.0580(3) -0.0936(2) 0.0484(8) Uani 1 1 d . . . F3 F 0.1965(2) 0.1025(3) -0.1451(2) 0.0436(7) Uani 1 1 d . . . F4 F 0.4737(3) -0.0452(3) 0.0917(3) 0.0598(9) Uani 1 1 d . . . F5 F 0.5034(3) 0.0173(4) 0.2564(3) 0.0675(11) Uani 1 1 d . . . F6 F 0.5457(3) 0.1109(3) 0.1518(4) 0.0733(12) Uani 1 1 d . . . F7 F -0.1613(4) 0.2983(3) 0.2776(4) 0.0869(15) Uani 1 1 d . A . F8 F -0.2174(3) 0.1437(3) 0.1791(3) 0.0739(11) Uani 1 1 d . A . F9 F -0.2155(4) 0.1692(4) 0.3428(4) 0.0937(16) Uani 1 1 d . A . F11 F 0.0581(4) -0.1671(3) 0.2796(3) 0.0709(11) Uani 1 1 d . A . F12 F -0.0212(5) -0.1061(6) 0.4037(6) 0.0552(17) Uiso 0.538(6) 1 d PDU A 1 F12' F 0.0117(8) -0.1219(8) 0.4281(7) 0.068(2) Uiso 0.462(6) 1 d PDU A 2 F13 F 0.1463(5) -0.0791(6) 0.4487(5) 0.0602(18) Uiso 0.538(6) 1 d PDU A 1 F13' F 0.1682(6) -0.1105(8) 0.4080(9) 0.077(3) Uiso 0.462(6) 1 d PDU A 2 F14 F -0.0208(3) 0.3513(3) 0.5440(3) 0.0599(9) Uani 1 1 d . . . F15 F 0.1018(3) 0.4786(2) 0.5804(3) 0.0642(10) Uani 1 1 d . . . F16 F 0.0949(4) 0.3734(4) 0.6851(3) 0.0822(14) Uani 1 1 d . . . F17 F 0.2976(6) 0.0348(6) 0.6206(7) 0.0661(18) Uiso 0.538(6) 1 d PDU A 1 F17' F 0.3058(5) 0.0799(5) 0.6732(5) 0.0379(14) Uiso 0.462(6) 1 d PU A 2 F18 F 0.4408(4) 0.0811(6) 0.5670(5) 0.0577(16) Uiso 0.538(6) 1 d PDU A 1 F18' F 0.3796(7) 0.0238(5) 0.5432(6) 0.0610(19) Uiso 0.462(6) 1 d PDU A 2 F19 F 0.4039(6) 0.1719(5) 0.6919(4) 0.0578(16) Uiso 0.538(6) 1 d PDU A 1 F19' F 0.4450(5) 0.1646(6) 0.6470(7) 0.066(2) Uiso 0.462(6) 1 d PDU A 2 O1 O 0.1382(3) 0.0462(2) 0.2998(3) 0.0383(8) Uani 1 1 d . . . O2 O 0.0135(2) 0.2050(2) 0.2509(2) 0.0305(6) Uani 1 1 d . . . O3 O 0.1429(2) 0.3129(2) 0.4307(2) 0.0291(6) Uani 1 1 d . . . O4 O 0.2947(2) 0.1673(2) 0.4415(2) 0.0280(6) Uani 1 1 d . . . O5 O 0.3376(2) 0.1254(2) 0.2395(2) 0.0253(6) Uani 1 1 d . . . O6 O 0.1565(2) 0.1638(2) 0.1123(2) 0.0272(6) Uani 1 1 d . . . N1 N 0.1602(3) 0.3763(3) 0.2206(3) 0.0237(7) Uani 1 1 d . . . N2 N 0.3485(3) 0.3469(3) 0.3431(3) 0.0227(6) Uani 1 1 d . . . N3 N 0.4294(3) 0.4975(3) 0.3258(3) 0.0246(7) Uani 1 1 d . . . C1 C 0.0649(3) 0.3894(4) 0.1637(3) 0.0285(8) Uani 1 1 d . . . H1 H 0.0171 0.3285 0.1321 0.034 Uiso 1 1 calc R . . C2 C 0.0326(3) 0.4882(4) 0.1486(4) 0.0344(10) Uani 1 1 d . . . H2 H -0.0340 0.4943 0.1041 0.041 Uiso 1 1 calc R . . C3 C 0.0991(3) 0.5769(4) 0.1994(4) 0.0358(10) Uani 1 1 d . . . H3 H 0.0773 0.6458 0.1941 0.043 Uiso 1 1 calc R . . C4 C 0.1988(3) 0.5647(3) 0.2586(4) 0.0317(9) Uani 1 1 d . . . H4 H 0.2454 0.6250 0.2959 0.038 Uiso 1 1 calc R . . C5 C 0.2286(3) 0.4632(3) 0.2620(3) 0.0236(8) Uani 1 1 d . . . C6 C 0.3354(3) 0.4372(3) 0.3103(3) 0.0224(7) Uani 1 1 d . . . C8 C 0.5084(3) 0.4419(3) 0.3755(3) 0.0258(8) Uani 1 1 d . . . C9 C 0.6179(3) 0.4659(4) 0.4107(4) 0.0319(9) Uani 1 1 d . . . H9 H 0.6517 0.5303 0.4043 0.038 Uiso 1 1 calc R . . C10 C 0.6749(3) 0.3911(4) 0.4556(4) 0.0352(10) Uani 1 1 d . . . H10 H 0.7498 0.4047 0.4812 0.042 Uiso 1 1 calc R . . C11 C 0.6248(4) 0.2956(4) 0.4641(4) 0.0341(9) Uani 1 1 d . . . H11 H 0.6668 0.2459 0.4947 0.041 Uiso 1 1 calc R . . C12 C 0.5158(3) 0.2718(3) 0.4289(3) 0.0279(8) Uani 1 1 d . . . H12 H 0.4824 0.2070 0.4347 0.033 Uiso 1 1 calc R . . C13 C 0.4570(3) 0.3475(3) 0.3846(3) 0.0232(7) Uani 1 1 d . . . C14 C 0.4547(3) 0.5888(3) 0.2796(4) 0.0321(9) Uani 1 1 d . B . H14A H 0.5325 0.5949 0.2828 0.039 Uiso 1 1 calc R . . H14B H 0.4366 0.6547 0.3235 0.039 Uiso 1 1 calc R . . C17 C 0.3970(3) 0.5815(4) 0.1668(4) 0.0376(11) Uani 1 1 d . . . C18 C 0.3999(4) 0.4891(4) 0.0898(4) 0.0428(12) Uani 1 1 d . B . C19 C 0.4658(4) 0.4057(4) 0.1089(4) 0.0423(12) Uani 1 1 d . . . H19A H 0.5057 0.4152 0.1791 0.051 Uiso 0.561(5) 1 calc PR B 1 H19B H 0.5138 0.4056 0.1715 0.051 Uiso 0.439(5) 1 d PR B 2 C20 C 0.4826(4) 0.3090(4) 0.0398(4) 0.0357(15) Uiso 0.561(5) 1 d PRU B 1 H20A H 0.5329 0.2607 0.0606 0.043 Uiso 0.561(5) 1 d PR B 1 C21 C 0.4143(8) 0.2924(8) -0.0655(7) 0.0366(13) Uiso 0.561(5) 1 d PU B 1 H21A H 0.4155 0.2282 -0.1151 0.044 Uiso 0.561(5) 1 calc PR B 1 C22 C 0.3497(8) 0.3671(9) -0.0931(7) 0.0343(13) Uiso 0.561(5) 1 d PU B 1 H22A H 0.3072 0.3557 -0.1624 0.041 Uiso 0.561(5) 1 calc PR B 1 C23 C 0.3444(7) 0.4630(8) -0.0199(7) 0.0324(13) Uiso 0.561(5) 1 d PU B 1 C20' C 0.4487(9) 0.3264(9) 0.0225(9) 0.0342(15) Uiso 0.439(5) 1 d PU B 2 H20C H 0.4862 0.2646 0.0279 0.041 Uiso 0.439(5) 1 calc PR B 2 C21' C 0.3801(11) 0.3267(11) -0.0754(9) 0.0342(15) Uiso 0.439(5) 1 d PU B 2 H21B H 0.3767 0.2678 -0.1324 0.041 Uiso 0.439(5) 1 calc PR B 2 C22' C 0.3200(10) 0.4077(10) -0.0897(9) 0.0355(14) Uiso 0.439(5) 1 d PU B 2 H22B H 0.2736 0.4041 -0.1560 0.043 Uiso 0.439(5) 1 calc PR B 2 C23' C 0.3239(9) 0.4991(10) -0.0083(9) 0.0326(14) Uiso 0.439(5) 1 d PU B 2 C24 C 0.2798(7) 0.5417(8) -0.0501(7) 0.0329(14) Uiso 0.561(5) 1 d PU B 1 H24A H 0.2373 0.5290 -0.1194 0.039 Uiso 0.561(5) 1 calc PR B 1 C25 C 0.2757(6) 0.6382(8) 0.0184(8) 0.0300(13) Uiso 0.561(5) 1 d PU B 1 C26 C 0.2109(7) 0.7174(8) -0.0132(8) 0.0368(13) Uiso 0.561(5) 1 d PU B 1 H26A H 0.1716 0.7075 -0.0837 0.044 Uiso 0.561(5) 1 calc PR B 1 C27 C 0.2050(7) 0.8101(9) 0.0597(8) 0.0364(13) Uiso 0.561(5) 1 d PU B 1 H27A H 0.1566 0.8603 0.0395 0.044 Uiso 0.561(5) 1 calc PR B 1 C28 C 0.2664(7) 0.8312(7) 0.1593(8) 0.0354(12) Uiso 0.561(5) 1 d PU B 1 H28A H 0.2641 0.8974 0.2056 0.043 Uiso 0.561(5) 1 calc PR B 1 C29 C 0.3312(7) 0.7568(7) 0.1924(8) 0.0309(12) Uiso 0.561(5) 1 d PU B 1 H29A H 0.3730 0.7718 0.2621 0.037 Uiso 0.561(5) 1 calc PR B 1 C30 C 0.3376(6) 0.6561(7) 0.1240(7) 0.0279(12) Uiso 0.561(5) 1 d PU B 1 C24' C 0.2669(9) 0.5868(11) -0.0216(10) 0.0319(17) Uiso 0.439(5) 1 d PU B 2 H24B H 0.2228 0.5861 -0.0885 0.038 Uiso 0.439(5) 1 calc PR B 2 C25' C 0.2716(8) 0.6754(9) 0.0584(10) 0.0315(13) Uiso 0.439(5) 1 d PU B 2 C26' C 0.2068(9) 0.7609(11) 0.0336(10) 0.0363(15) Uiso 0.439(5) 1 d PU B 2 H26B H 0.1636 0.7574 -0.0343 0.044 Uiso 0.439(5) 1 calc PR B 2 C27' C 0.2119(9) 0.8477(10) 0.1153(10) 0.0377(15) Uiso 0.439(5) 1 d PU B 2 H27B H 0.1688 0.9045 0.1033 0.045 Uiso 0.439(5) 1 calc PR B 2 C28' C 0.2780(9) 0.8559(9) 0.2154(10) 0.0356(14) Uiso 0.439(5) 1 d PU B 2 H28B H 0.2792 0.9184 0.2678 0.043 Uiso 0.439(5) 1 calc PR B 2 C29' C 0.3405(8) 0.7768(9) 0.2394(10) 0.0313(14) Uiso 0.439(5) 1 d PU B 2 H29B H 0.3848 0.7844 0.3075 0.038 Uiso 0.439(5) 1 calc PR B 2 C30' C 0.3384(8) 0.6804(9) 0.1596(9) 0.0277(14) Uiso 0.439(5) 1 d PU B 2 C31 C 0.4738(4) 0.0428(4) 0.1648(4) 0.0359(10) Uani 1 1 d . . . C32 C 0.3636(3) 0.0886(3) 0.1542(3) 0.0259(8) Uani 1 1 d . . . C33 C 0.3048(3) 0.0873(4) 0.0525(3) 0.0298(9) Uani 1 1 d . . . H33 H 0.3330 0.0592 -0.0077 0.036 Uiso 1 1 calc R . . C34 C 0.2053(3) 0.1275(3) 0.0409(3) 0.0261(8) Uani 1 1 d . . . C35 C 0.1405(4) 0.1274(4) -0.0698(3) 0.0353(10) Uani 1 1 d . . . C36 C 0.0670(4) -0.0914(5) 0.3616(4) 0.0581(17) Uani 1 1 d D . . C37 C 0.0615(5) 0.0167(4) 0.3303(4) 0.0486(14) Uani 1 1 d . A . C38 C -0.0327(5) 0.0680(5) 0.3346(4) 0.0487(14) Uani 1 1 d . . . H38 H -0.0842 0.0433 0.3686 0.058 Uiso 1 1 calc R A . C39 C -0.0502(4) 0.1565(4) 0.2878(4) 0.0422(11) Uani 1 1 d . A . C40 C -0.1638(5) 0.1933(5) 0.2722(5) 0.0511(14) Uani 1 1 d . . . C41 C 0.0800(4) 0.3796(4) 0.5843(4) 0.0376(10) Uani 1 1 d . . . C42 C 0.1525(4) 0.3060(4) 0.5263(4) 0.0356(10) Uani 1 1 d . . . C43 C 0.2182(4) 0.2436(4) 0.5823(4) 0.0430(12) Uani 1 1 d . . . H43 H 0.2182 0.2471 0.6546 0.052 Uiso 1 1 calc R . . C44 C 0.2845(4) 0.1756(4) 0.5323(4) 0.0347(10) Uani 1 1 d . A . C45 C 0.3541(3) 0.1118(3) 0.6005(3) 0.0338(9) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.02283(9) 0.01853(9) 0.01813(9) 0.00427(6) 0.00261(6) -0.00358(6) F1 0.074(2) 0.056(2) 0.0316(15) 0.0123(14) -0.0046(15) 0.0199(17) F2 0.0363(15) 0.071(2) 0.0276(13) -0.0023(13) -0.0020(11) -0.0155(14) F3 0.0437(16) 0.0638(19) 0.0208(12) 0.0051(12) 0.0061(11) -0.0032(14) F4 0.0518(19) 0.059(2) 0.066(2) -0.0008(17) 0.0170(17) 0.0231(16) F5 0.061(2) 0.111(3) 0.0430(18) 0.0318(19) 0.0165(16) 0.052(2) F6 0.0287(16) 0.078(3) 0.121(4) 0.039(3) 0.0172(19) 0.0010(17) F7 0.071(3) 0.058(2) 0.138(4) 0.001(3) 0.057(3) 0.007(2) F8 0.051(2) 0.076(3) 0.082(3) 0.012(2) -0.0067(19) -0.0237(19) F9 0.068(3) 0.126(4) 0.109(4) 0.031(3) 0.066(3) 0.003(3) F11 0.107(3) 0.0361(18) 0.067(2) 0.0081(17) 0.017(2) -0.0076(19) F14 0.0421(18) 0.063(2) 0.078(2) 0.0128(19) 0.0222(17) 0.0109(16) F15 0.071(2) 0.0301(16) 0.094(3) -0.0079(16) 0.043(2) 0.0077(15) F16 0.092(3) 0.117(4) 0.044(2) 0.013(2) 0.024(2) 0.058(3) O1 0.048(2) 0.0266(16) 0.0366(17) 0.0125(13) -0.0038(15) -0.0164(14) O2 0.0267(15) 0.0337(16) 0.0305(15) 0.0058(12) 0.0074(12) -0.0099(12) O3 0.0283(15) 0.0341(16) 0.0244(14) 0.0039(12) 0.0067(11) 0.0030(12) O4 0.0300(15) 0.0322(15) 0.0224(14) 0.0104(12) 0.0027(11) -0.0012(12) O5 0.0278(14) 0.0242(14) 0.0232(13) 0.0049(11) 0.0039(11) 0.0026(11) O6 0.0286(14) 0.0278(14) 0.0218(13) 0.0016(11) 0.0010(11) 0.0008(12) N1 0.0210(15) 0.0235(16) 0.0267(16) 0.0074(13) 0.0039(13) -0.0027(13) N2 0.0211(15) 0.0199(15) 0.0253(16) 0.0014(12) 0.0039(12) -0.0006(12) N3 0.0194(15) 0.0201(15) 0.0333(18) 0.0039(13) 0.0052(13) -0.0027(12) C1 0.0216(18) 0.032(2) 0.031(2) 0.0116(17) 0.0010(16) -0.0048(16) C2 0.0211(19) 0.039(2) 0.048(3) 0.022(2) 0.0060(18) 0.0041(18) C3 0.025(2) 0.029(2) 0.061(3) 0.019(2) 0.015(2) 0.0074(17) C4 0.0219(19) 0.023(2) 0.052(3) 0.0090(18) 0.0108(18) -0.0034(16) C5 0.0202(18) 0.0234(18) 0.0290(19) 0.0080(15) 0.0070(15) 0.0002(14) C6 0.0221(18) 0.0190(17) 0.0253(18) 0.0026(14) 0.0059(14) -0.0038(14) C8 0.0232(19) 0.0231(19) 0.029(2) 0.0011(15) 0.0046(15) -0.0002(15) C9 0.0225(19) 0.031(2) 0.037(2) -0.0001(18) 0.0033(17) -0.0045(17) C10 0.0205(19) 0.042(3) 0.039(2) 0.004(2) 0.0009(17) 0.0009(18) C11 0.027(2) 0.038(2) 0.035(2) 0.0070(19) 0.0002(17) 0.0073(18) C12 0.027(2) 0.027(2) 0.028(2) 0.0052(16) 0.0031(16) 0.0019(16) C13 0.0209(18) 0.0232(18) 0.0227(18) 0.0005(14) 0.0027(14) -0.0008(14) C14 0.0234(19) 0.0207(19) 0.054(3) 0.0103(18) 0.0096(18) -0.0036(16) C17 0.022(2) 0.035(2) 0.061(3) 0.025(2) 0.008(2) -0.0064(18) C18 0.037(3) 0.049(3) 0.044(3) 0.022(2) 0.005(2) -0.023(2) C19 0.050(3) 0.039(3) 0.042(3) 0.010(2) 0.022(2) -0.014(2) C31 0.032(2) 0.048(3) 0.031(2) 0.012(2) 0.0095(18) 0.009(2) C32 0.028(2) 0.0240(19) 0.0258(19) 0.0071(15) 0.0052(16) -0.0002(16) C33 0.030(2) 0.037(2) 0.0227(19) 0.0047(17) 0.0083(16) 0.0017(18) C34 0.032(2) 0.0224(18) 0.0207(18) 0.0027(14) 0.0019(15) -0.0048(16) C35 0.036(2) 0.044(3) 0.022(2) 0.0043(18) 0.0014(17) -0.001(2) C36 0.082(4) 0.050(3) 0.036(3) 0.022(2) -0.009(3) -0.033(3) C37 0.071(4) 0.038(3) 0.030(2) 0.007(2) 0.000(2) -0.022(3) C38 0.063(4) 0.050(3) 0.031(2) 0.004(2) 0.012(2) -0.024(3) C39 0.042(3) 0.049(3) 0.032(2) 0.000(2) 0.011(2) -0.015(2) C40 0.047(3) 0.044(3) 0.066(4) 0.001(3) 0.033(3) -0.007(2) C41 0.036(2) 0.043(3) 0.034(2) 0.001(2) 0.0131(19) 0.006(2) C42 0.037(2) 0.034(2) 0.033(2) 0.0004(18) 0.0072(19) 0.0038(19) C43 0.053(3) 0.053(3) 0.025(2) 0.008(2) 0.010(2) 0.017(2) C44 0.033(2) 0.044(3) 0.029(2) 0.0126(19) 0.0066(18) 0.006(2) C45 0.028(2) 0.048(3) 0.027(2) 0.0128(19) 0.0044(17) 0.0037(19) _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 Yb1 O6 2.262(3) . ? Yb1 O5 2.272(3) . ? Yb1 O1 2.293(3) . ? Yb1 O3 2.298(3) . ? Yb1 O4 2.322(3) . ? Yb1 O2 2.325(3) . ? Yb1 N2 2.435(3) . ? Yb1 N1 2.491(3) . ? F1 C35 1.342(6) . ? F2 C35 1.329(6) . ? F3 C35 1.336(5) . ? F4 C31 1.334(6) . ? F5 C31 1.307(6) . ? F6 C31 1.311(6) . ? F7 C40 1.339(7) . ? F8 C40 1.312(7) . ? F9 C40 1.325(7) . ? F11 C36 1.290(7) . ? F12 C36 1.379(5) . ? F12' C36 1.341(6) . ? F13 C36 1.357(5) . ? F13' C36 1.373(6) . ? F14 C41 1.306(6) . ? F15 C41 1.310(6) . ? F16 C41 1.328(6) . ? F17 C45 1.308(5) . ? F17' C45 1.361(7) . ? F18 C45 1.320(5) . ? F18' C45 1.321(5) . ? F19 C45 1.326(5) . ? F19' C45 1.303(5) . ? O1 C37 1.212(7) . ? O2 C39 1.242(6) . ? O3 C42 1.268(6) . ? O4 C44 1.219(5) . ? O5 C32 1.247(5) . ? O6 C34 1.258(5) . ? N1 C1 1.336(5) . ? N1 C5 1.350(5) . ? N2 C6 1.323(5) . ? N2 C13 1.389(5) . ? N3 C6 1.369(5) . ? N3 C8 1.394(5) . ? N3 C14 1.484(5) . ? C1 C2 1.390(6) . ? C1 H1 0.9500 . ? C2 C3 1.374(7) . ? C2 H2 0.9500 . ? C3 C4 1.392(6) . ? C3 H3 0.9500 . ? C4 C5 1.381(6) . ? C4 H4 0.9500 . ? C5 C6 1.470(5) . ? C8 C9 1.392(6) . ? C8 C13 1.402(6) . ? C9 C10 1.384(7) . ? C9 H9 0.9500 . ? C10 C11 1.405(7) . ? C10 H10 0.9500 . ? C11 C12 1.385(6) . ? C11 H11 0.9500 . ? C12 C13 1.401(6) . ? C12 H12 0.9500 . ? C14 C17 1.513(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C17 C30 1.384(9) . ? C17 C18 1.411(8) . ? C17 C30' 1.509(11) . ? C18 C19 1.418(8) . ? C18 C23 1.452(10) . ? C18 C23' 1.492(12) . ? C19 C20' 1.348(12) . ? C19 C20 1.4400 . ? C19 H19A 0.9500 . ? C19 H19B 0.9299 . ? C20 C21 1.464(11) . ? C20 H20A 0.9500 . ? C21 C22 1.347(13) . ? C21 H21A 0.9500 . ? C22 C23 1.422(13) . ? C22 H22A 0.9500 . ? C23 C24 1.399(12) . ? C20' C21' 1.415(17) . ? C20' H20A 1.4659 . ? C20' H20C 0.9500 . ? C21' C22' 1.338(17) . ? C21' H21B 0.9500 . ? C22' C23' 1.421(17) . ? C22' H22B 0.9500 . ? C23' C24' 1.386(17) . ? C24 C25 1.394(12) . ? C24 H24A 0.9500 . ? C25 C26 1.410(12) . ? C25 C30 1.434(12) . ? C26 C27 1.393(13) . ? C26 H26A 0.9500 . ? C27 C28 1.365(13) . ? C27 H27A 0.9500 . ? C28 C29 1.370(12) . ? C28 H28A 0.9500 . ? C29 C30 1.441(12) . ? C29 H29A 0.9500 . ? C24' C25' 1.385(16) . ? C24' H24B 0.9500 . ? C25' C30' 1.428(15) . ? C25' C26' 1.450(16) . ? C26' C27' 1.381(17) . ? C26' H26B 0.9500 . ? C27' C28' 1.407(17) . ? C27' H27B 0.9500 . ? C28' C29' 1.364(15) . ? C28' H28B 0.9500 . ? C29' C30' 1.456(15) . ? C29' H29B 0.9500 . ? C31 C32 1.539(6) . ? C32 C33 1.404(6) . ? C33 C34 1.382(6) . ? C33 H33 0.9500 . ? C34 C35 1.534(6) . ? C36 C37 1.529(8) . ? C37 C38 1.400(9) . ? C38 C39 1.405(8) . ? C38 H38 0.9500 . ? C39 C40 1.533(8) . ? C41 C42 1.549(6) . ? C42 C43 1.392(7) . ? C43 C44 1.401(7) . ? C43 H43 0.9500 . ? C44 C45 1.520(6) . ? 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 O6 Yb1 O5 73.25(10) . . ? O6 Yb1 O1 89.15(11) . . ? O5 Yb1 O1 83.15(12) . . ? O6 Yb1 O3 141.87(10) . . ? O5 Yb1 O3 144.25(10) . . ? O1 Yb1 O3 100.07(12) . . ? O6 Yb1 O4 143.81(11) . . ? O5 Yb1 O4 74.73(10) . . ? O1 Yb1 O4 70.62(11) . . ? O3 Yb1 O4 72.97(11) . . ? O6 Yb1 O2 76.20(11) . . ? O5 Yb1 O2 140.99(11) . . ? O1 Yb1 O2 72.65(12) . . ? O3 Yb1 O2 71.62(11) . . ? O4 Yb1 O2 122.37(10) . . ? O6 Yb1 N2 109.52(11) . . ? O5 Yb1 N2 75.82(11) . . ? O1 Yb1 N2 145.93(12) . . ? O3 Yb1 N2 82.87(11) . . ? O4 Yb1 N2 78.07(11) . . ? O2 Yb1 N2 138.31(11) . . ? O6 Yb1 N1 72.58(11) . . ? O5 Yb1 N1 115.45(10) . . ? O1 Yb1 N1 147.34(12) . . ? O3 Yb1 N1 80.51(11) . . ? O4 Yb1 N1 138.08(11) . . ? O2 Yb1 N1 76.74(11) . . ? N2 Yb1 N1 66.73(11) . . ? C37 O1 Yb1 131.0(4) . . ? C39 O2 Yb1 128.3(3) . . ? C42 O3 Yb1 133.0(3) . . ? C44 O4 Yb1 136.0(3) . . ? C32 O5 Yb1 136.2(3) . . ? C34 O6 Yb1 135.7(3) . . ? C1 N1 C5 117.8(3) . . ? C1 N1 Yb1 122.6(3) . . ? C5 N1 Yb1 117.8(3) . . ? C6 N2 C13 105.9(3) . . ? C6 N2 Yb1 117.8(3) . . ? C13 N2 Yb1 135.0(3) . . ? C6 N3 C8 106.0(3) . . ? C6 N3 C14 130.0(3) . . ? C8 N3 C14 122.4(3) . . ? N1 C1 C2 123.0(4) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 118.5(4) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 119.3(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 118.5(4) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 122.4(4) . . ? N1 C5 C6 112.8(3) . . ? C4 C5 C6 124.8(4) . . ? N2 C6 N3 112.9(3) . . ? N2 C6 C5 120.4(3) . . ? N3 C6 C5 126.7(3) . . ? C9 C8 N3 131.2(4) . . ? C9 C8 C13 122.6(4) . . ? N3 C8 C13 106.2(3) . . ? C10 C9 C8 116.5(4) . . ? C10 C9 H9 121.7 . . ? C8 C9 H9 121.7 . . ? C9 C10 C11 121.6(4) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C12 C11 C10 121.8(4) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C13 117.2(4) . . ? C11 C12 H12 121.4 . . ? C13 C12 H12 121.4 . . ? N2 C13 C12 130.7(4) . . ? N2 C13 C8 109.0(3) . . ? C12 C13 C8 120.3(4) . . ? N3 C14 C17 114.6(3) . . ? N3 C14 H14A 108.6 . . ? C17 C14 H14A 108.6 . . ? N3 C14 H14B 108.6 . . ? C17 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? C30 C17 C18 111.4(6) . . ? C30 C17 C30' 19.7(4) . . ? C18 C17 C30' 130.9(6) . . ? C30 C17 C14 128.6(6) . . ? C18 C17 C14 120.0(4) . . ? C30' C17 C14 109.0(6) . . ? C17 C18 C19 123.2(5) . . ? C17 C18 C23 128.7(6) . . ? C19 C18 C23 108.0(6) . . ? C17 C18 C23' 107.3(6) . . ? C19 C18 C23' 129.4(7) . . ? C23 C18 C23' 21.6(4) . . ? C20' C19 C18 109.9(6) . . ? C20' C19 C20 21.5(5) . . ? C18 C19 C20 131.0(3) . . ? C20' C19 H19A 135.2 . . ? C18 C19 H19A 114.5 . . ? C20 C19 H19A 114.5 . . ? C20' C19 H19B 125.0 . . ? C18 C19 H19B 125.1 . . ? C20 C19 H19B 103.8 . . ? H19A C19 H19B 11.6 . . ? C19 C20 C21 113.3(5) . . ? C19 C20 H20A 123.3 . . ? C21 C20 H20A 123.3 . . ? C22 C21 C20 120.8(8) . . ? C22 C21 H21A 119.6 . . ? C20 C21 H21A 119.6 . . ? C21 C22 C23 120.8(9) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? C24 C23 C22 120.5(9) . . ? C24 C23 C18 113.6(8) . . ? C22 C23 C18 125.8(8) . . ? C19 C20' C21' 126.1(10) . . ? C19 C20' H20A 97.5 . . ? C21' C20' H20A 135.6 . . ? C19 C20' H20C 117.0 . . ? C21' C20' H20C 117.0 . . ? H20A C20' H20C 21.3 . . ? C22' C21' C20' 121.7(11) . . ? C22' C21' H21B 119.2 . . ? C20' C21' H21B 119.2 . . ? C21' C22' C23' 121.8(11) . . ? C21' C22' H22B 119.1 . . ? C23' C22' H22B 119.1 . . ? C24' C23' C22' 123.5(11) . . ? C24' C23' C18 125.4(10) . . ? C22' C23' C18 111.0(10) . . ? C25 C24 C23 122.1(8) . . ? C25 C24 H24A 118.9 . . ? C23 C24 H24A 118.9 . . ? C24 C25 C26 121.6(9) . . ? C24 C25 C30 118.8(7) . . ? C26 C25 C30 119.6(9) . . ? C27 C26 C25 119.5(9) . . ? C27 C26 H26A 120.3 . . ? C25 C26 H26A 120.3 . . ? C28 C27 C26 122.2(9) . . ? C28 C27 H27A 118.9 . . ? C26 C27 H27A 118.9 . . ? C27 C28 C29 119.8(9) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C28 C29 C30 121.6(8) . . ? C28 C29 H29A 119.2 . . ? C30 C29 H29A 119.2 . . ? C17 C30 C25 124.9(8) . . ? C17 C30 C29 117.8(7) . . ? C25 C30 C29 117.2(8) . . ? C25' C24' C23' 122.8(10) . . ? C25' C24' H24B 118.6 . . ? C23' C24' H24B 118.6 . . ? C24' C25' C30' 120.4(10) . . ? C24' C25' C26' 116.9(11) . . ? C30' C25' C26' 122.8(11) . . ? C27' C26' C25' 115.6(11) . . ? C27' C26' H26B 122.2 . . ? C25' C26' H26B 122.2 . . ? C26' C27' C28' 123.1(11) . . ? C26' C27' H27B 118.5 . . ? C28' C27' H27B 118.5 . . ? C29' C28' C27' 121.9(11) . . ? C29' C28' H28B 119.0 . . ? C27' C28' H28B 119.0 . . ? C28' C29' C30' 119.3(11) . . ? C28' C29' H29B 120.4 . . ? C30' C29' H29B 120.4 . . ? C25' C30' C29' 117.3(10) . . ? C25' C30' C17 113.0(9) . . ? C29' C30' C17 129.7(9) . . ? F5 C31 F6 109.8(5) . . ? F5 C31 F4 106.8(4) . . ? F6 C31 F4 106.2(4) . . ? F5 C31 C32 111.0(4) . . ? F6 C31 C32 110.7(4) . . ? F4 C31 C32 112.1(4) . . ? O5 C32 C33 127.1(4) . . ? O5 C32 C31 114.9(4) . . ? C33 C32 C31 118.0(4) . . ? C34 C33 C32 119.1(4) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? O6 C34 C33 127.6(4) . . ? O6 C34 C35 112.7(4) . . ? C33 C34 C35 119.7(4) . . ? F2 C35 F3 107.6(4) . . ? F2 C35 F1 108.1(4) . . ? F3 C35 F1 106.8(4) . . ? F2 C35 C34 110.5(4) . . ? F3 C35 C34 113.2(4) . . ? F1 C35 C34 110.4(4) . . ? F11 C36 F12' 109.0(6) . . ? F11 C36 F13 124.3(6) . . ? F12' C36 F13 80.6(6) . . ? F11 C36 F13' 95.7(7) . . ? F12' C36 F13' 100.0(7) . . ? F13 C36 F13' 30.4(5) . . ? F11 C36 F12 106.0(5) . . ? F12' C36 F12 23.2(5) . . ? F13 C36 F12 100.8(6) . . ? F13' C36 F12 123.0(7) . . ? F11 C36 C37 110.8(4) . . ? F12' C36 C37 124.2(7) . . ? F13 C36 C37 106.3(5) . . ? F13' C36 C37 113.1(6) . . ? F12 C36 C37 107.1(6) . . ? O1 C37 C38 127.1(5) . . ? O1 C37 C36 115.7(6) . . ? C38 C37 C36 117.2(5) . . ? C37 C38 C39 119.3(5) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? O2 C39 C38 127.9(5) . . ? O2 C39 C40 115.2(5) . . ? C38 C39 C40 116.7(5) . . ? F8 C40 F9 107.2(5) . . ? F8 C40 F7 109.4(6) . . ? F9 C40 F7 109.4(5) . . ? F8 C40 C39 108.5(4) . . ? F9 C40 C39 112.0(6) . . ? F7 C40 C39 110.2(5) . . ? F14 C41 F15 110.3(4) . . ? F14 C41 F16 106.1(4) . . ? F15 C41 F16 108.0(5) . . ? F14 C41 C42 111.1(4) . . ? F15 C41 C42 110.2(4) . . ? F16 C41 C42 111.1(4) . . ? O3 C42 C43 128.7(4) . . ? O3 C42 C41 112.6(4) . . ? C43 C42 C41 118.6(4) . . ? C42 C43 C44 120.3(4) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? O4 C44 C43 125.9(4) . . ? O4 C44 C45 117.8(4) . . ? C43 C44 C45 116.2(4) . . ? F19' C45 F17 134.2(6) . . ? F19' C45 F18 61.6(5) . . ? F17 C45 F18 113.7(6) . . ? F19' C45 F18' 105.0(6) . . ? F17 C45 F18' 74.8(6) . . ? F18 C45 F18' 45.2(4) . . ? F19' C45 F19 38.3(4) . . ? F17 C45 F19 107.9(6) . . ? F18 C45 F19 96.6(5) . . ? F18' C45 F19 131.6(6) . . ? F19' C45 F17' 110.0(6) . . ? F17 C45 F17' 34.8(4) . . ? F18 C45 F17' 130.8(5) . . ? F18' C45 F17' 105.7(5) . . ? F19 C45 F17' 75.5(5) . . ? F19' C45 C44 110.9(5) . . ? F17 C45 C44 111.4(5) . . ? F18 C45 C44 114.5(4) . . ? F18' C45 C44 111.4(5) . . ? F19 C45 C44 111.8(4) . . ? F17' C45 C44 113.4(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.672 _refine_diff_density_min -1.660 _refine_diff_density_rms 0.128 #===END