# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' #TrackingRef 'DyTCNQF4-final.cif' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Nazario Lopez' _publ_contact_author_email nlopez@mail.chem.tamu.edu loop_ _publ_author_name _publ_author_address N.Lopez '' A.V.Prosvirin '' H.Zhao '' W.Wernsdorfer '' K.R.Dunbar '' # Attachment 'HoTCNQF4-final.cif' data_c:\docume~1\hanhua\hotcnqf4 _database_code_depnum_ccdc_archive 'CCDC 669348' #TrackingRef 'HoTCNQF4-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Holmium(III) 2,3,5,6-Tetrafluoro-7,7,8,8-Tetracyanoquinodimethane ; _chemical_name_common ;Holmium(iii) 2,3,5,6-Tetrafluoro-7,7,8,8- Tetracyanoquinodimethane ; _chemical_melting_point ? _chemical_formula_sum 'C36 H18 F12 Ho N12 O9' _chemical_formula_weight 1155.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.666(2) _cell_length_b 17.643(2) _cell_length_c 17.045(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.119(7) _cell_angle_gamma 90.00 _cell_volume 4002.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2260 _exptl_absorpt_coefficient_mu 2.106 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4508 _exptl_absorpt_correction_T_max 0.6544 _exptl_absorpt_process_details 'SADABS v2.03 (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 1000 CCD area-detector' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40702 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.27 _reflns_number_total 9584 _reflns_number_gt 8975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2000)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2000)' _computing_data_reduction 'SAINT V6.32 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0193P)^2^+2.1154P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9584 _refine_ls_number_parameters 703 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0172 _refine_ls_wR_factor_ref 0.0436 _refine_ls_wR_factor_gt 0.0429 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.301686(5) 0.409314(4) 0.064333(4) 0.01130(3) Uani 1 1 d . . . F1 F 0.29450(7) 0.15930(5) -0.00140(6) 0.02025(19) Uani 1 1 d . . . F2 F 0.43699(7) -0.00883(5) 0.21146(5) 0.01971(19) Uani 1 1 d . . . F3 F 0.30648(7) 0.05428(5) -0.10605(5) 0.0214(2) Uani 1 1 d . . . F4 F 0.45468(7) -0.11290(5) 0.10532(6) 0.0224(2) Uani 1 1 d . . . F5 F -0.02464(7) 0.30953(5) -0.09441(6) 0.02021(19) Uani 1 1 d . . . F6 F 0.04466(7) 0.12321(5) -0.27430(5) 0.01727(18) Uani 1 1 d . . . F7 F -0.21797(7) 0.28997(5) -0.15053(6) 0.02006(19) Uani 1 1 d . . . F8 F -0.14833(7) 0.10075(5) -0.32828(6) 0.01816(19) Uani 1 1 d . . . F9 F 0.05079(7) 0.13147(5) -0.02848(6) 0.01946(19) Uani 1 1 d . . . F10 F 0.21027(7) -0.03299(5) 0.18200(5) 0.01928(19) Uani 1 1 d . . . F11 F 0.06458(7) 0.02738(5) -0.13493(5) 0.0209(2) Uani 1 1 d . . . F12 F 0.22398(7) -0.13752(5) 0.07604(6) 0.02008(19) Uani 1 1 d . . . O1 O 0.14506(9) 0.39713(7) 0.09118(8) 0.0205(2) Uani 1 1 d . . . O2 O 0.25453(9) 0.47229(7) -0.05773(7) 0.0192(2) Uani 1 1 d . . . O3 O 0.24817(10) 0.52826(7) 0.10142(9) 0.0234(3) Uani 1 1 d . . . O4 O 0.43434(9) 0.49632(7) 0.07236(7) 0.0190(2) Uani 1 1 d . . . O5 O 0.37054(10) 0.41464(8) 0.20223(7) 0.0213(3) Uani 1 1 d . . . O6 O 0.41445(9) 0.35411(7) -0.00348(8) 0.0174(2) Uani 1 1 d . . . N1 N 0.32876(10) 0.27883(8) 0.12204(8) 0.0176(3) Uani 1 1 d . . . N2 N 0.38547(11) 0.12050(8) 0.32086(9) 0.0224(3) Uani 1 1 d . . . N3 N 0.35434(11) -0.06497(8) -0.21799(9) 0.0239(3) Uani 1 1 d . . . N4 N 0.45597(12) -0.22630(9) -0.03651(10) 0.0294(3) Uani 1 1 d . . . N5 N 0.20292(9) 0.32024(8) -0.03589(8) 0.0162(3) Uani 1 1 d . . . N6 N 0.26592(10) 0.18151(8) -0.21678(8) 0.0208(3) Uani 1 1 d . . . N7 N -0.43853(11) 0.25856(9) -0.22944(10) 0.0291(3) Uani 1 1 d . . . N8 N -0.37356(11) 0.08489(8) -0.38247(10) 0.0245(3) Uani 1 1 d . . . N9 N 0.06851(11) 0.24953(8) 0.10706(9) 0.0235(3) Uani 1 1 d . . . N10 N 0.14967(11) 0.08282(8) 0.29195(9) 0.0227(3) Uani 1 1 d . . . N11 N 0.10405(13) -0.09659(9) -0.24516(10) 0.0282(3) Uani 1 1 d . . . N12 N 0.19936(13) -0.25785(9) -0.05452(10) 0.0307(4) Uani 1 1 d . . . C1 C 0.34206(11) 0.21691(9) 0.14281(9) 0.0151(3) Uani 1 1 d . . . C2 C 0.37677(11) 0.12799(9) 0.25278(10) 0.0164(3) Uani 1 1 d . . . C3 C 0.35988(11) 0.14015(9) 0.16793(9) 0.0147(3) Uani 1 1 d . . . C4 C 0.36770(11) 0.08234(8) 0.11151(10) 0.0143(3) Uani 1 1 d . . . C5 C 0.33679(12) 0.09303(8) 0.02714(10) 0.0148(3) Uani 1 1 d . . . C6 C 0.40610(11) 0.00844(9) 0.13298(9) 0.0153(3) Uani 1 1 d . . . C7 C 0.34281(11) 0.03817(9) -0.02784(9) 0.0157(3) Uani 1 1 d . . . C8 C 0.41433(11) -0.04585(9) 0.07790(10) 0.0158(3) Uani 1 1 d . . . C9 C 0.38253(11) -0.03507(9) -0.00678(9) 0.0148(3) Uani 1 1 d . . . C10 C 0.38764(12) -0.09108(8) -0.06533(10) 0.0163(3) Uani 1 1 d . . . C11 C 0.36749(12) -0.07513(9) -0.14970(10) 0.0182(3) Uani 1 1 d . . . C12 C 0.42586(12) -0.16553(9) -0.04632(10) 0.0197(3) Uani 1 1 d . . . C13 C 0.16414(11) 0.28256(9) -0.08904(9) 0.0154(3) Uani 1 1 d . . . C14 C 0.20048(11) 0.20326(9) -0.19072(9) 0.0161(3) Uani 1 1 d . . . C15 C 0.12486(11) 0.23425(8) -0.15517(9) 0.0147(3) Uani 1 1 d . . . C16 C 0.02037(11) 0.22021(8) -0.18385(9) 0.0141(3) Uani 1 1 d . . . C17 C -0.05414(11) 0.25870(8) -0.15356(9) 0.0148(3) Uani 1 1 d . . . C18 C -0.01911(11) 0.16633(8) -0.24424(9) 0.0143(3) Uani 1 1 d . . . C19 C -0.15454(11) 0.24820(9) -0.18253(9) 0.0150(3) Uani 1 1 d . . . C20 C -0.11965(11) 0.15486(8) -0.27228(9) 0.0143(3) Uani 1 1 d . . . C21 C -0.19462(11) 0.19591(8) -0.24483(9) 0.0142(3) Uani 1 1 d . . . C22 C -0.29893(11) 0.18471(9) -0.27558(9) 0.0163(3) Uani 1 1 d . . . C23 C -0.37461(12) 0.22647(9) -0.24872(10) 0.0195(3) Uani 1 1 d . . . C24 C -0.33801(11) 0.12940(9) -0.33493(10) 0.0181(3) Uani 1 1 d . . . C25 C 0.09218(11) 0.18732(9) 0.11989(10) 0.0174(3) Uani 1 1 d . . . C26 C 0.13930(12) 0.09460(9) 0.22441(10) 0.0169(3) Uani 1 1 d . . . C27 C 0.12334(11) 0.11150(9) 0.14078(9) 0.0154(3) Uani 1 1 d . . . C28 C 0.12985(11) 0.05521(9) 0.08276(9) 0.0143(3) Uani 1 1 d . . . C29 C 0.09581(11) 0.06563(9) -0.00160(9) 0.0149(3) Uani 1 1 d . . . C30 C 0.17179(11) -0.01758(9) 0.10392(9) 0.0148(3) Uani 1 1 d . . . C31 C 0.10271(11) 0.01135(9) -0.05682(9) 0.0153(3) Uani 1 1 d . . . C32 C 0.17879(11) -0.07186(9) 0.04856(10) 0.0154(3) Uani 1 1 d . . . C33 C 0.14492(11) -0.06164(9) -0.03560(9) 0.0152(3) Uani 1 1 d . . . C34 C 0.15299(12) -0.11883(9) -0.09223(10) 0.0176(3) Uani 1 1 d . . . C35 C 0.12536(13) -0.10577(10) -0.17674(11) 0.0210(3) Uani 1 1 d . . . C36 C 0.17972(13) -0.19532(10) -0.06954(10) 0.0211(3) Uani 1 1 d . . . H1A H 0.1176(18) 0.3572(15) 0.0938(14) 0.038(7) Uiso 1 1 d . . . H2A H 0.2211(19) 0.4553(15) -0.0974(16) 0.043(7) Uiso 1 1 d . . . H3A H 0.210(2) 0.5533(15) 0.0692(16) 0.043(7) Uiso 1 1 d . . . H4A H 0.433(2) 0.5450(17) 0.0800(16) 0.054(8) Uiso 1 1 d . . . H5A H 0.379(2) 0.4568(18) 0.2262(17) 0.060(9) Uiso 1 1 d . . . H6A H 0.4530(18) 0.3182(14) 0.0116(14) 0.037(6) Uiso 1 1 d . . . H1B H 0.1093(19) 0.4311(15) 0.0999(15) 0.041(7) Uiso 1 1 d . . . H2B H 0.2898(19) 0.5056(15) -0.0712(15) 0.041(7) Uiso 1 1 d . . . H3B H 0.271(4) 0.559(3) 0.138(3) 0.145(18) Uiso 1 1 d . . . H4B H 0.4916(18) 0.4844(13) 0.0798(13) 0.031(6) Uiso 1 1 d . . . H5B H 0.3504(19) 0.3865(15) 0.2329(15) 0.040(7) Uiso 1 1 d . . . H6B H 0.4107(17) 0.3613(13) -0.0484(15) 0.030(6) Uiso 1 1 d . . . O1S O 0.01404(10) 0.51401(7) 0.10298(9) 0.0233(3) Uani 1 1 d . . . O2S O 0.10503(11) 0.59658(8) -0.00864(8) 0.0256(3) Uani 1 1 d . . . O3S O 0.39713(11) 0.64708(8) 0.08101(9) 0.0295(3) Uani 1 1 d D . . H1SA H 0.024(2) 0.5467(17) 0.0708(18) 0.055(8) Uiso 1 1 d . . . H2SA H 0.087(2) 0.5655(16) -0.0492(17) 0.049(7) Uiso 1 1 d . . . H1SB H 0.026(2) 0.5341(17) 0.147(2) 0.063(9) Uiso 1 1 d . . . H2SB H 0.1239(18) 0.6403(15) -0.0261(15) 0.044(7) Uiso 1 1 d . . . H3SB H 0.420(2) 0.6760(14) 0.1212(13) 0.055(8) Uiso 1 1 d D . . H3SA H 0.364(2) 0.6728(16) 0.0422(14) 0.069(10) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.01133(4) 0.01088(4) 0.01135(4) -0.00107(2) 0.00190(3) -0.00024(2) F1 0.0297(5) 0.0130(4) 0.0156(4) 0.0018(4) 0.0002(4) 0.0069(4) F2 0.0239(5) 0.0197(5) 0.0135(4) 0.0044(4) 0.0000(4) 0.0038(4) F3 0.0321(5) 0.0180(5) 0.0124(4) 0.0019(4) 0.0017(4) 0.0060(4) F4 0.0294(5) 0.0141(4) 0.0217(5) 0.0041(4) 0.0021(4) 0.0080(4) F5 0.0186(4) 0.0213(5) 0.0193(5) -0.0107(4) 0.0011(4) 0.0001(4) F6 0.0176(4) 0.0175(5) 0.0178(5) -0.0054(4) 0.0062(4) 0.0010(3) F7 0.0178(4) 0.0212(5) 0.0215(5) -0.0078(4) 0.0052(4) 0.0027(4) F8 0.0183(4) 0.0175(5) 0.0184(5) -0.0081(4) 0.0034(4) -0.0023(3) F9 0.0233(5) 0.0159(5) 0.0182(5) 0.0036(4) 0.0027(4) 0.0051(4) F10 0.0272(5) 0.0173(5) 0.0125(4) 0.0022(4) 0.0027(4) 0.0032(4) F11 0.0268(5) 0.0230(5) 0.0115(4) 0.0008(4) 0.0011(4) 0.0034(4) F12 0.0275(5) 0.0135(4) 0.0194(5) 0.0025(4) 0.0056(4) 0.0043(4) O1 0.0180(6) 0.0161(6) 0.0300(7) -0.0035(5) 0.0112(5) -0.0012(5) O2 0.0200(6) 0.0187(6) 0.0171(6) 0.0033(5) 0.0002(5) -0.0034(5) O3 0.0187(6) 0.0169(6) 0.0326(7) -0.0086(5) 0.0019(5) 0.0014(5) O4 0.0144(5) 0.0154(6) 0.0258(6) -0.0002(5) 0.0018(5) -0.0015(4) O5 0.0278(6) 0.0221(6) 0.0135(6) -0.0021(5) 0.0035(5) -0.0094(5) O6 0.0182(5) 0.0175(6) 0.0170(6) 0.0004(5) 0.0050(5) 0.0048(4) N1 0.0220(6) 0.0175(7) 0.0130(6) -0.0024(5) 0.0032(5) 0.0009(5) N2 0.0239(7) 0.0240(7) 0.0189(7) 0.0007(6) 0.0037(6) -0.0039(6) N3 0.0311(8) 0.0200(7) 0.0220(7) 0.0013(6) 0.0087(6) 0.0025(6) N4 0.0352(8) 0.0217(8) 0.0293(8) -0.0019(6) 0.0028(7) 0.0088(6) N5 0.0160(6) 0.0166(6) 0.0155(6) -0.0017(5) 0.0025(5) -0.0011(5) N6 0.0203(7) 0.0244(7) 0.0183(7) -0.0005(6) 0.0052(6) 0.0010(5) N7 0.0199(7) 0.0320(9) 0.0345(9) -0.0101(7) 0.0042(6) 0.0027(6) N8 0.0171(7) 0.0262(8) 0.0277(8) -0.0084(6) 0.0002(6) 0.0012(6) N9 0.0267(7) 0.0180(7) 0.0260(8) -0.0008(6) 0.0065(6) 0.0002(6) N10 0.0266(7) 0.0233(7) 0.0177(7) -0.0033(6) 0.0042(6) 0.0008(6) N11 0.0349(9) 0.0286(8) 0.0193(8) -0.0052(6) 0.0025(7) 0.0030(6) N12 0.0451(10) 0.0201(8) 0.0290(8) -0.0034(6) 0.0128(8) -0.0011(6) C1 0.0148(7) 0.0181(8) 0.0122(7) -0.0028(6) 0.0029(6) -0.0013(6) C2 0.0167(7) 0.0136(7) 0.0181(8) -0.0002(6) 0.0022(6) -0.0022(6) C3 0.0155(7) 0.0147(7) 0.0133(7) 0.0011(6) 0.0017(6) 0.0000(5) C4 0.0122(7) 0.0143(7) 0.0157(7) 0.0013(6) 0.0020(6) -0.0008(5) C5 0.0157(7) 0.0117(7) 0.0163(7) 0.0029(5) 0.0020(6) 0.0014(5) C6 0.0146(7) 0.0170(7) 0.0133(7) 0.0042(6) 0.0009(6) 0.0004(6) C7 0.0168(7) 0.0160(7) 0.0138(7) 0.0023(6) 0.0024(6) 0.0003(6) C8 0.0151(7) 0.0121(7) 0.0197(8) 0.0038(6) 0.0030(6) 0.0025(5) C9 0.0130(6) 0.0142(7) 0.0174(7) 0.0009(6) 0.0037(6) -0.0002(5) C10 0.0167(7) 0.0142(7) 0.0184(8) 0.0004(6) 0.0046(6) 0.0012(5) C11 0.0196(7) 0.0127(7) 0.0237(9) -0.0015(6) 0.0077(7) 0.0010(6) C12 0.0195(7) 0.0200(8) 0.0192(8) -0.0020(6) 0.0038(6) 0.0013(6) C13 0.0154(7) 0.0150(7) 0.0167(7) 0.0031(6) 0.0055(6) 0.0014(6) C14 0.0182(7) 0.0156(7) 0.0129(7) 0.0010(6) 0.0000(6) -0.0018(6) C15 0.0169(7) 0.0135(7) 0.0137(7) -0.0007(6) 0.0032(6) -0.0007(6) C16 0.0171(7) 0.0129(7) 0.0117(7) 0.0011(5) 0.0023(6) -0.0004(5) C17 0.0188(7) 0.0124(7) 0.0129(7) -0.0029(5) 0.0026(6) -0.0010(5) C18 0.0176(7) 0.0129(7) 0.0133(7) -0.0004(6) 0.0056(6) 0.0017(5) C19 0.0172(7) 0.0134(7) 0.0147(7) -0.0012(6) 0.0044(6) 0.0012(5) C20 0.0192(7) 0.0120(7) 0.0117(7) -0.0025(5) 0.0033(6) -0.0015(5) C21 0.0161(7) 0.0134(7) 0.0129(7) 0.0011(5) 0.0027(6) -0.0009(5) C22 0.0171(7) 0.0147(7) 0.0166(7) -0.0004(6) 0.0028(6) 0.0001(6) C23 0.0179(7) 0.0193(8) 0.0195(8) -0.0025(6) 0.0008(6) -0.0017(6) C24 0.0135(7) 0.0197(8) 0.0205(8) 0.0000(6) 0.0024(6) 0.0026(6) C25 0.0168(7) 0.0193(8) 0.0165(7) -0.0031(6) 0.0046(6) -0.0022(6) C26 0.0163(7) 0.0160(7) 0.0184(8) -0.0044(6) 0.0037(6) 0.0007(5) C27 0.0158(7) 0.0150(7) 0.0154(7) -0.0006(6) 0.0032(6) -0.0008(6) C28 0.0129(6) 0.0150(7) 0.0147(7) -0.0002(6) 0.0025(6) -0.0016(5) C29 0.0144(7) 0.0129(7) 0.0171(7) 0.0026(6) 0.0026(6) 0.0012(5) C30 0.0160(7) 0.0161(7) 0.0121(7) 0.0019(6) 0.0027(6) -0.0009(5) C31 0.0143(7) 0.0193(8) 0.0116(7) 0.0013(6) 0.0017(6) -0.0012(6) C32 0.0157(7) 0.0129(7) 0.0181(8) 0.0011(6) 0.0045(6) -0.0004(5) C33 0.0140(7) 0.0162(7) 0.0158(7) -0.0012(6) 0.0038(6) -0.0029(5) C34 0.0190(7) 0.0171(8) 0.0166(7) -0.0025(6) 0.0042(6) -0.0023(6) C35 0.0207(8) 0.0200(8) 0.0220(9) -0.0057(6) 0.0044(7) -0.0002(6) C36 0.0259(8) 0.0205(9) 0.0184(8) -0.0047(6) 0.0080(7) -0.0033(6) O1S 0.0290(6) 0.0201(6) 0.0225(6) -0.0003(5) 0.0097(5) 0.0011(5) O2S 0.0352(7) 0.0195(6) 0.0249(7) 0.0009(5) 0.0126(6) 0.0037(5) O3S 0.0361(7) 0.0190(6) 0.0312(8) -0.0048(6) 0.0027(6) 0.0020(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 Ho1 O1 2.2982(12) . ? Ho1 O2 2.3172(12) . ? Ho1 O5 2.3269(13) . ? Ho1 O6 2.3384(11) . ? Ho1 O4 2.3556(12) . ? Ho1 O3 2.3555(12) . ? Ho1 N5 2.4825(13) . ? Ho1 N1 2.4978(14) . ? F1 C5 1.3454(17) . ? F2 C6 1.3433(17) . ? F3 C7 1.3431(17) . ? F4 C8 1.3434(17) . ? F5 C17 1.3412(17) . ? F6 C18 1.3430(16) . ? F7 C19 1.3441(17) . ? F8 C20 1.3439(17) . ? F9 C29 1.3452(18) . ? F10 C30 1.3431(17) . ? F11 C31 1.3450(17) . ? F12 C32 1.3458(18) . ? O1 H1A 0.80(3) . ? O1 H1B 0.81(3) . ? O2 H2A 0.78(3) . ? O2 H2B 0.83(3) . ? O3 H3A 0.80(3) . ? O3 H3B 0.83(5) . ? O4 H4A 0.87(3) . ? O4 H4B 0.79(2) . ? O5 H5A 0.84(3) . ? O5 H5B 0.81(3) . ? O6 H6A 0.83(3) . ? O6 H6B 0.77(2) . ? N1 C1 1.150(2) . ? N2 C2 1.147(2) . ? N3 C11 1.151(2) . ? N4 C12 1.147(2) . ? N5 C13 1.151(2) . ? N6 C14 1.151(2) . ? N7 C23 1.150(2) . ? N8 C24 1.154(2) . ? N9 C25 1.151(2) . ? N10 C26 1.147(2) . ? N11 C35 1.148(2) . ? N12 C36 1.150(2) . ? C1 C3 1.425(2) . ? C2 C3 1.428(2) . ? C3 C4 1.422(2) . ? C4 C5 1.416(2) . ? C4 C6 1.422(2) . ? C5 C7 1.363(2) . ? C6 C8 1.364(2) . ? C7 C9 1.416(2) . ? C8 C9 1.423(2) . ? C9 C10 1.417(2) . ? C10 C12 1.424(2) . ? C10 C11 1.430(2) . ? C13 C15 1.418(2) . ? C14 C15 1.421(2) . ? C15 C16 1.422(2) . ? C16 C18 1.415(2) . ? C16 C17 1.415(2) . ? C17 C19 1.361(2) . ? C18 C20 1.363(2) . ? C19 C21 1.419(2) . ? C20 C21 1.418(2) . ? C21 C22 1.417(2) . ? C22 C24 1.420(2) . ? C22 C23 1.427(2) . ? C25 C27 1.424(2) . ? C26 C27 1.424(2) . ? C27 C28 1.418(2) . ? C28 C29 1.419(2) . ? C28 C30 1.419(2) . ? C29 C31 1.361(2) . ? C30 C32 1.363(2) . ? C31 C33 1.424(2) . ? C32 C33 1.415(2) . ? C33 C34 1.418(2) . ? C34 C35 1.423(2) . ? C34 C36 1.428(2) . ? O1S H1SA 0.83(3) . ? O1S H1SB 0.81(3) . ? O2S H2SA 0.87(3) . ? O2S H2SB 0.89(3) . ? O3S H3SB 0.854(17) . ? O3S H3SA 0.843(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ho1 O2 98.15(5) . . ? O1 Ho1 O5 89.09(5) . . ? O2 Ho1 O5 148.63(5) . . ? O1 Ho1 O6 143.85(4) . . ? O2 Ho1 O6 80.57(4) . . ? O5 Ho1 O6 110.81(5) . . ? O1 Ho1 O4 142.06(5) . . ? O2 Ho1 O4 78.07(4) . . ? O5 Ho1 O4 77.62(4) . . ? O6 Ho1 O4 73.46(4) . . ? O1 Ho1 O3 70.73(5) . . ? O2 Ho1 O3 76.92(5) . . ? O5 Ho1 O3 76.82(5) . . ? O6 Ho1 O3 141.57(4) . . ? O4 Ho1 O3 71.67(4) . . ? O1 Ho1 N5 72.08(4) . . ? O2 Ho1 N5 71.86(5) . . ? O5 Ho1 N5 138.82(4) . . ? O6 Ho1 N5 73.29(4) . . ? O4 Ho1 N5 138.03(4) . . ? O3 Ho1 N5 126.53(5) . . ? O1 Ho1 N1 84.08(5) . . ? O2 Ho1 N1 141.41(4) . . ? O5 Ho1 N1 69.49(4) . . ? O6 Ho1 N1 75.84(4) . . ? O4 Ho1 N1 122.31(4) . . ? O3 Ho1 N1 137.97(5) . . ? N5 Ho1 N1 72.32(4) . . ? Ho1 O1 H1A 124.1(17) . . ? Ho1 O1 H1B 126.6(18) . . ? H1A O1 H1B 109(2) . . ? Ho1 O2 H2A 125.4(19) . . ? Ho1 O2 H2B 122.0(17) . . ? H2A O2 H2B 107(2) . . ? Ho1 O3 H3A 120.1(19) . . ? Ho1 O3 H3B 134(3) . . ? H3A O3 H3B 103(4) . . ? Ho1 O4 H4A 127.5(18) . . ? Ho1 O4 H4B 123.7(16) . . ? H4A O4 H4B 107(2) . . ? Ho1 O5 H5A 120(2) . . ? Ho1 O5 H5B 120.4(18) . . ? H5A O5 H5B 105(3) . . ? Ho1 O6 H6A 127.6(16) . . ? Ho1 O6 H6B 121.5(17) . . ? H6A O6 H6B 109(2) . . ? C1 N1 Ho1 174.67(12) . . ? C13 N5 Ho1 171.20(12) . . ? N1 C1 C3 179.07(17) . . ? N2 C2 C3 176.14(17) . . ? C4 C3 C1 120.83(14) . . ? C4 C3 C2 123.88(14) . . ? C1 C3 C2 115.11(13) . . ? C5 C4 C6 113.01(14) . . ? C5 C4 C3 122.70(14) . . ? C6 C4 C3 124.29(14) . . ? F1 C5 C7 117.18(14) . . ? F1 C5 C4 119.17(13) . . ? C7 C5 C4 123.57(14) . . ? F2 C6 C8 118.03(14) . . ? F2 C6 C4 118.58(14) . . ? C8 C6 C4 123.38(14) . . ? F3 C7 C5 117.77(14) . . ? F3 C7 C9 118.60(14) . . ? C5 C7 C9 123.61(14) . . ? F4 C8 C6 118.07(14) . . ? F4 C8 C9 118.52(14) . . ? C6 C8 C9 123.41(14) . . ? C7 C9 C10 122.35(14) . . ? C7 C9 C8 112.98(14) . . ? C10 C9 C8 124.66(14) . . ? C9 C10 C12 123.86(15) . . ? C9 C10 C11 122.83(14) . . ? C12 C10 C11 112.80(14) . . ? N3 C11 C10 176.80(17) . . ? N4 C12 C10 175.34(18) . . ? N5 C13 C15 175.00(16) . . ? N6 C14 C15 175.62(17) . . ? C13 C15 C14 112.93(13) . . ? C13 C15 C16 123.18(13) . . ? C14 C15 C16 123.86(14) . . ? C18 C16 C17 113.61(13) . . ? C18 C16 C15 123.67(14) . . ? C17 C16 C15 122.72(14) . . ? F5 C17 C19 118.03(13) . . ? F5 C17 C16 118.47(13) . . ? C19 C17 C16 123.49(14) . . ? F6 C18 C20 118.15(13) . . ? F6 C18 C16 119.00(13) . . ? C20 C18 C16 122.84(14) . . ? F7 C19 C17 117.90(13) . . ? F7 C19 C21 119.02(13) . . ? C17 C19 C21 123.08(14) . . ? F8 C20 C18 117.56(13) . . ? F8 C20 C21 118.75(13) . . ? C18 C20 C21 123.68(14) . . ? C22 C21 C20 123.26(14) . . ? C22 C21 C19 123.54(14) . . ? C20 C21 C19 113.19(13) . . ? C21 C22 C24 122.94(14) . . ? C21 C22 C23 123.43(14) . . ? C24 C22 C23 113.62(14) . . ? N7 C23 C22 177.16(18) . . ? N8 C24 C22 177.21(17) . . ? N9 C25 C27 176.55(18) . . ? N10 C26 C27 177.64(17) . . ? C28 C27 C26 122.13(14) . . ? C28 C27 C25 123.08(14) . . ? C26 C27 C25 114.58(14) . . ? C27 C28 C29 123.89(14) . . ? C27 C28 C30 122.82(14) . . ? C29 C28 C30 113.29(13) . . ? F9 C29 C31 118.04(14) . . ? F9 C29 C28 118.45(13) . . ? C31 C29 C28 123.46(14) . . ? F10 C30 C32 118.07(14) . . ? F10 C30 C28 118.67(13) . . ? C32 C30 C28 123.21(14) . . ? F11 C31 C29 117.68(14) . . ? F11 C31 C33 119.03(13) . . ? C29 C31 C33 123.26(14) . . ? F12 C32 C30 117.56(14) . . ? F12 C32 C33 118.76(14) . . ? C30 C32 C33 123.63(15) . . ? C32 C33 C34 122.76(15) . . ? C32 C33 C31 113.16(14) . . ? C34 C33 C31 124.08(15) . . ? C33 C34 C35 122.03(15) . . ? C33 C34 C36 122.87(15) . . ? C35 C34 C36 114.83(14) . . ? N11 C35 C34 178.60(19) . . ? N12 C36 C34 177.11(19) . . ? H1SA O1S H1SB 106(3) . . ? H2SA O2S H2SB 109(2) . . ? H3SB O3S H3SA 110(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ho1 N1 C1 116.9(13) . . . . ? O2 Ho1 N1 C1 21.3(14) . . . . ? O5 Ho1 N1 C1 -151.8(13) . . . . ? O6 Ho1 N1 C1 -32.8(13) . . . . ? O4 Ho1 N1 C1 -92.3(13) . . . . ? O3 Ho1 N1 C1 169.3(13) . . . . ? N5 Ho1 N1 C1 43.9(13) . . . . ? O1 Ho1 N5 C13 148.1(8) . . . . ? O2 Ho1 N5 C13 42.9(8) . . . . ? O5 Ho1 N5 C13 -145.2(8) . . . . ? O6 Ho1 N5 C13 -42.4(8) . . . . ? O4 Ho1 N5 C13 -3.5(8) . . . . ? O3 Ho1 N5 C13 100.3(8) . . . . ? N1 Ho1 N5 C13 -122.5(8) . . . . ? Ho1 N1 C1 C3 46(13) . . . . ? N1 C1 C3 C4 -52(12) . . . . ? N1 C1 C3 C2 123(12) . . . . ? N2 C2 C3 C4 -134(3) . . . . ? N2 C2 C3 C1 51(3) . . . . ? C1 C3 C4 C5 -14.5(2) . . . . ? C2 C3 C4 C5 170.69(14) . . . . ? C1 C3 C4 C6 165.94(14) . . . . ? C2 C3 C4 C6 -8.9(2) . . . . ? C6 C4 C5 F1 176.87(13) . . . . ? C3 C4 C5 F1 -2.7(2) . . . . ? C6 C4 C5 C7 0.2(2) . . . . ? C3 C4 C5 C7 -179.38(15) . . . . ? C5 C4 C6 F2 -179.36(13) . . . . ? C3 C4 C6 F2 0.2(2) . . . . ? C5 C4 C6 C8 1.4(2) . . . . ? C3 C4 C6 C8 -179.01(15) . . . . ? F1 C5 C7 F3 0.1(2) . . . . ? C4 C5 C7 F3 176.84(13) . . . . ? F1 C5 C7 C9 -178.05(13) . . . . ? C4 C5 C7 C9 -1.3(2) . . . . ? F2 C6 C8 F4 -1.3(2) . . . . ? C4 C6 C8 F4 177.96(13) . . . . ? F2 C6 C8 C9 178.75(13) . . . . ? C4 C6 C8 C9 -2.0(2) . . . . ? F3 C7 C9 C10 1.7(2) . . . . ? C5 C7 C9 C10 179.86(15) . . . . ? F3 C7 C9 C8 -177.38(13) . . . . ? C5 C7 C9 C8 0.8(2) . . . . ? F4 C8 C9 C7 -179.13(13) . . . . ? C6 C8 C9 C7 0.8(2) . . . . ? F4 C8 C9 C10 1.8(2) . . . . ? C6 C8 C9 C10 -178.22(15) . . . . ? C7 C9 C10 C12 -179.16(15) . . . . ? C8 C9 C10 C12 -0.2(2) . . . . ? C7 C9 C10 C11 9.6(2) . . . . ? C8 C9 C10 C11 -171.46(15) . . . . ? C9 C10 C11 N3 151(3) . . . . ? C12 C10 C11 N3 -21(3) . . . . ? C9 C10 C12 N4 -174(2) . . . . ? C11 C10 C12 N4 -2(2) . . . . ? Ho1 N5 C13 C15 51(2) . . . . ? N5 C13 C15 C14 -6(2) . . . . ? N5 C13 C15 C16 175.5(18) . . . . ? N6 C14 C15 C13 -14(2) . . . . ? N6 C14 C15 C16 165(2) . . . . ? C13 C15 C16 C18 -173.27(15) . . . . ? C14 C15 C16 C18 8.5(2) . . . . ? C13 C15 C16 C17 6.0(2) . . . . ? C14 C15 C16 C17 -172.26(15) . . . . ? C18 C16 C17 F5 178.15(13) . . . . ? C15 C16 C17 F5 -1.2(2) . . . . ? C18 C16 C17 C19 -3.4(2) . . . . ? C15 C16 C17 C19 177.25(15) . . . . ? C17 C16 C18 F6 -176.27(13) . . . . ? C15 C16 C18 F6 3.1(2) . . . . ? C17 C16 C18 C20 2.2(2) . . . . ? C15 C16 C18 C20 -178.46(15) . . . . ? F5 C17 C19 F7 0.6(2) . . . . ? C16 C17 C19 F7 -177.85(14) . . . . ? F5 C17 C19 C21 -179.83(14) . . . . ? C16 C17 C19 C21 1.7(2) . . . . ? F6 C18 C20 F8 0.2(2) . . . . ? C16 C18 C20 F8 -178.32(13) . . . . ? F6 C18 C20 C21 179.22(13) . . . . ? C16 C18 C20 C21 0.7(2) . . . . ? F8 C20 C21 C22 -2.4(2) . . . . ? C18 C20 C21 C22 178.60(15) . . . . ? F8 C20 C21 C19 176.55(13) . . . . ? C18 C20 C21 C19 -2.5(2) . . . . ? F7 C19 C21 C22 -0.2(2) . . . . ? C17 C19 C21 C22 -179.80(15) . . . . ? F7 C19 C21 C20 -179.13(13) . . . . ? C17 C19 C21 C20 1.3(2) . . . . ? C20 C21 C22 C24 2.2(2) . . . . ? C19 C21 C22 C24 -176.59(15) . . . . ? C20 C21 C22 C23 -179.31(15) . . . . ? C19 C21 C22 C23 1.9(2) . . . . ? C21 C22 C23 N7 177(100) . . . . ? C24 C22 C23 N7 -5(4) . . . . ? C21 C22 C24 N8 167(4) . . . . ? C23 C22 C24 N8 -12(4) . . . . ? N10 C26 C27 C28 -145(4) . . . . ? N10 C26 C27 C25 30(5) . . . . ? N9 C25 C27 C28 -170(3) . . . . ? N9 C25 C27 C26 15(3) . . . . ? C26 C27 C28 C29 167.17(14) . . . . ? C25 C27 C28 C29 -7.3(2) . . . . ? C26 C27 C28 C30 -13.0(2) . . . . ? C25 C27 C28 C30 172.51(14) . . . . ? C27 C28 C29 F9 -2.9(2) . . . . ? C30 C28 C29 F9 177.26(12) . . . . ? C27 C28 C29 C31 179.76(14) . . . . ? C30 C28 C29 C31 -0.1(2) . . . . ? C27 C28 C30 F10 -2.5(2) . . . . ? C29 C28 C30 F10 177.37(12) . . . . ? C27 C28 C30 C32 -179.67(14) . . . . ? C29 C28 C30 C32 0.2(2) . . . . ? F9 C29 C31 F11 0.5(2) . . . . ? C28 C29 C31 F11 177.80(13) . . . . ? F9 C29 C31 C33 -177.35(13) . . . . ? C28 C29 C31 C33 0.0(2) . . . . ? F10 C30 C32 F12 0.0(2) . . . . ? C28 C30 C32 F12 177.24(13) . . . . ? F10 C30 C32 C33 -177.40(13) . . . . ? C28 C30 C32 C33 -0.2(2) . . . . ? F12 C32 C33 C34 2.5(2) . . . . ? C30 C32 C33 C34 179.93(15) . . . . ? F12 C32 C33 C31 -177.31(13) . . . . ? C30 C32 C33 C31 0.1(2) . . . . ? F11 C31 C33 C32 -177.78(12) . . . . ? C29 C31 C33 C32 0.0(2) . . . . ? F11 C31 C33 C34 2.4(2) . . . . ? C29 C31 C33 C34 -179.83(15) . . . . ? C32 C33 C34 C35 -175.29(15) . . . . ? C31 C33 C34 C35 4.5(2) . . . . ? C32 C33 C34 C36 11.0(2) . . . . ? C31 C33 C34 C36 -169.15(15) . . . . ? C33 C34 C35 N11 167(9) . . . . ? C36 C34 C35 N11 -19(9) . . . . ? C33 C34 C36 N12 158(4) . . . . ? C35 C34 C36 N12 -16(4) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.396 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.064 data_c:\docume~1\hanhua\nl033 _database_code_depnum_ccdc_archive 'CCDC 749360' #TrackingRef 'DyTCNQF4-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Dysprosium(III) 2,3,5,6-Tetrafluoro-7,7,8,8-Tetracyanoquinodimethane ; _chemical_name_common ;Dysprosium(iii) 2,3,5,6-Tetrafluoro-7,7,8,8- Tetracyanoquinodimethane ; _chemical_melting_point ? _chemical_formula_sum 'C36 H18 Dy F12 N12 O9' _chemical_formula_weight 1153.12 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.694(3) _cell_length_b 17.664(4) _cell_length_c 17.068(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.12(3) _cell_angle_gamma 90.00 _cell_volume 4021.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 1.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5391 _exptl_absorpt_correction_T_max 0.6921 _exptl_absorpt_process_details 'SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 1000 CCD area-detector' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24979 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.56 _reflns_number_total 9244 _reflns_number_gt 8156 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2000)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2000)' _computing_data_reduction 'SAINT V6.32 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0283P)^2^+1.5821P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9244 _refine_ls_number_parameters 698 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0552 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.198148(7) 0.590816(5) 0.435761(5) 0.01413(4) Uani 1 1 d . . . F7 F 0.64819(10) 0.89878(7) 0.82791(8) 0.0234(3) Uani 1 1 d . . . F6 F 0.45594(9) 0.87648(7) 0.77436(7) 0.0217(3) Uani 1 1 d . . . F5 F 0.52404(10) 0.69025(7) 0.59470(8) 0.0254(3) Uani 1 1 d . . . F2 F 0.19272(11) 0.94563(7) 0.60531(7) 0.0275(3) Uani 1 1 d . . . F3 F 0.04611(11) 1.11285(7) 0.39457(8) 0.0291(3) Uani 1 1 d . . . F4 F 0.06362(10) 1.00891(7) 0.28880(7) 0.0255(3) Uani 1 1 d . . . F8 F 0.71721(10) 0.70969(7) 0.65059(8) 0.0263(3) Uani 1 1 d . . . F1 F 0.20482(10) 0.84094(7) 0.50108(7) 0.0257(3) Uani 1 1 d . . . O5 O 0.13021(14) 0.58491(11) 0.29726(10) 0.0274(4) Uani 1 1 d . . . O4 O 0.06482(14) 0.50401(10) 0.42757(11) 0.0246(3) Uani 1 1 d . . . N1 N 0.17078(14) 0.72182(10) 0.37760(10) 0.0220(4) Uani 1 1 d . . . O1 O 0.35499(13) 0.60279(10) 0.40889(11) 0.0261(4) Uani 1 1 d . . . O3 O 0.25145(14) 0.47104(10) 0.39899(12) 0.0293(4) Uani 1 1 d . . . C19 C 0.16273(17) 0.90734(11) 0.47257(13) 0.0190(4) Uani 1 1 d . . . O2 O 0.24506(13) 0.52768(10) 0.55817(10) 0.0237(3) Uani 1 1 d . . . O6 O 0.08521(12) 0.64645(10) 0.50396(11) 0.0214(3) Uani 1 1 d . . . N7 N 0.87272(16) 0.91428(12) 0.88197(14) 0.0327(5) Uani 1 1 d . . . C28 C 0.79823(16) 0.81475(12) 0.77544(13) 0.0201(4) Uani 1 1 d . . . C6 C 0.30002(16) 0.79707(12) 0.69072(12) 0.0194(4) Uani 1 1 d . . . C16 C 0.08586(16) 1.04580(12) 0.42175(13) 0.0203(4) Uani 1 1 d . . . C26 C 0.65378(16) 0.75135(12) 0.68263(12) 0.0188(4) Uani 1 1 d . . . C13 C 0.14000(16) 0.86015(12) 0.33205(12) 0.0186(4) Uani 1 1 d . . . C20 C 0.11250(17) 1.09093(11) 0.56503(13) 0.0203(4) Uani 1 1 d . . . N6 N 0.23522(15) 0.81883(12) 0.71677(12) 0.0274(4) Uani 1 1 d . . . C4 C 0.13243(18) 1.07513(12) 0.64912(14) 0.0233(5) Uani 1 1 d . . . C5 C 0.33598(16) 0.71763(12) 0.58938(12) 0.0178(4) Uani 1 1 d . . . N5 N 0.29730(14) 0.68011(10) 0.53645(11) 0.0204(4) Uani 1 1 d . . . C24 C 0.61905(16) 0.84460(11) 0.77192(12) 0.0173(4) Uani 1 1 d . . . C21 C 0.37535(16) 0.76595(12) 0.65538(12) 0.0174(4) Uani 1 1 d . . . C27 C 0.55402(16) 0.74106(11) 0.65366(12) 0.0185(4) Uani 1 1 d . . . C18 C 0.15682(16) 0.96205(12) 0.52743(12) 0.0197(4) Uani 1 1 d . . . N2 N 0.11416(16) 0.87965(12) 0.17949(11) 0.0276(4) Uani 1 1 d . . . C14 C 0.13253(16) 0.91776(12) 0.38851(13) 0.0177(4) Uani 1 1 d . . . C17 C 0.11764(16) 1.03525(12) 0.50640(13) 0.0188(4) Uani 1 1 d . . . C25 C 0.69396(16) 0.80366(12) 0.74453(12) 0.0178(4) Uani 1 1 d . . . C7 C 0.83716(17) 0.86984(13) 0.83474(14) 0.0238(5) Uani 1 1 d . . . C23 C 0.51962(16) 0.83321(11) 0.74437(12) 0.0176(4) Uani 1 1 d . . . C22 C 0.47968(16) 0.77955(11) 0.68388(12) 0.0169(4) Uani 1 1 d . . . C15 C 0.09430(16) 0.99185(12) 0.36713(12) 0.0187(4) Uani 1 1 d . . . C2 C 0.12359(16) 0.87237(12) 0.24755(13) 0.0208(4) Uani 1 1 d . . . N4 N 0.14527(17) 1.06494(12) 0.71721(12) 0.0314(5) Uani 1 1 d . . . N3 N 0.04437(18) 1.22614(12) 0.53576(14) 0.0372(5) Uani 1 1 d . . . C1 C 0.15758(16) 0.78355(12) 0.35712(12) 0.0189(4) Uani 1 1 d . . . C3 C 0.07424(18) 1.16529(13) 0.54568(14) 0.0250(5) Uani 1 1 d . . . F9 F 0.44836(10) 0.63170(7) 1.02803(7) 0.0245(3) Uani 1 1 d . . . F12 F 0.29084(10) 0.46682(7) 0.81840(7) 0.0245(3) Uani 1 1 d . . . F11 F 0.27746(10) 0.36271(7) 0.92439(7) 0.0255(3) Uani 1 1 d . . . F10 F 0.43496(10) 0.52805(7) 1.13444(7) 0.0264(3) Uani 1 1 d . . . C9 C 0.36059(17) 0.59445(12) 0.77590(14) 0.0220(5) Uani 1 1 d . . . C30 C 0.37020(15) 0.55515(12) 0.91729(12) 0.0174(4) Uani 1 1 d . . . C35 C 0.40393(16) 0.56576(12) 1.00143(12) 0.0180(4) Uani 1 1 d . . . N12 N 0.39555(19) 0.40421(13) 1.24463(13) 0.0369(5) Uani 1 1 d . . . C36 C 0.34762(17) 0.38175(13) 1.09203(13) 0.0219(4) Uani 1 1 d . . . C31 C 0.32906(16) 0.48254(12) 0.89659(12) 0.0180(4) Uani 1 1 d . . . C11 C 0.32134(19) 0.30524(14) 1.06999(13) 0.0271(5) Uani 1 1 d . . . C29 C 0.37635(16) 0.61149(12) 0.85941(13) 0.0191(4) Uani 1 1 d . . . C34 C 0.39738(16) 0.51172(12) 1.05646(12) 0.0189(4) Uani 1 1 d . . . C33 C 0.35533(16) 0.43867(12) 1.03564(12) 0.0181(4) Uani 1 1 d . . . N11 N 0.30237(18) 0.24292(13) 1.05495(13) 0.0386(6) Uani 1 1 d . . . C10 C 0.40696(17) 0.68722(13) 0.87980(13) 0.0216(4) Uani 1 1 d . . . C32 C 0.32192(16) 0.42831(12) 0.95157(13) 0.0188(4) Uani 1 1 d . . . N10 N 0.42998(16) 0.74941(11) 0.89287(12) 0.0298(5) Uani 1 1 d . . . C12 C 0.37450(18) 0.39514(13) 1.17635(14) 0.0260(5) Uani 1 1 d . . . O8 O 0.39514(16) 0.40348(11) 0.50875(12) 0.0318(4) Uani 1 1 d . . . O7 O 0.48556(14) 0.48624(10) 0.39662(12) 0.0284(4) Uani 1 1 d . . . O9 O 0.10334(18) 0.14665(11) 0.91891(15) 0.0384(5) Uani 1 1 d . . . N9 N 0.35010(17) 0.58276(11) 0.70856(12) 0.0293(5) Uani 1 1 d . . . N8 N 0.06271(16) 0.25849(13) 0.27076(14) 0.0380(5) Uani 1 1 d . . . C8 C 0.12658(17) 0.22674(13) 0.25154(14) 0.0246(5) Uiso 1 1 d . . . H2A H 0.277(2) 0.5468(17) 0.5976(18) 0.031(8) Uiso 1 1 d . . . H1A H 0.387(2) 0.5697(16) 0.3990(16) 0.025(7) Uiso 1 1 d . . . H2B H 0.208(2) 0.4923(19) 0.5725(18) 0.048(9) Uiso 1 1 d . . . H5A H 0.121(3) 0.544(2) 0.280(2) 0.067(12) Uiso 1 1 d . . . H6B H 0.088(2) 0.6384(17) 0.5470(18) 0.032(8) Uiso 1 1 d . . . H5B H 0.148(3) 0.613(2) 0.269(2) 0.049(10) Uiso 1 1 d . . . H4B H 0.011(2) 0.5153(17) 0.4171(17) 0.036(9) Uiso 1 1 d . . . H7A H 0.476(2) 0.4541(18) 0.4276(19) 0.039(9) Uiso 1 1 d . . . H4A H 0.071(3) 0.457(2) 0.420(2) 0.062(11) Uiso 1 1 d . . . H3A H 0.296(3) 0.445(2) 0.434(2) 0.052(10) Uiso 1 1 d . . . H6A H 0.050(2) 0.6818(19) 0.4891(18) 0.042(9) Uiso 1 1 d . . . H1B H 0.384(2) 0.643(2) 0.4048(19) 0.050(10) Uiso 1 1 d . . . H8A H 0.413(3) 0.435(2) 0.549(2) 0.073(12) Uiso 1 1 d . . . H7B H 0.468(3) 0.465(2) 0.353(2) 0.063(11) Uiso 1 1 d . . . H8B H 0.380(3) 0.363(2) 0.525(2) 0.066(12) Uiso 1 1 d . . . H9A H 0.079(3) 0.171(2) 0.882(2) 0.065(13) Uiso 1 1 d . . . H9B H 0.134(3) 0.167(2) 0.956(2) 0.073(14) Uiso 1 1 d . . . H3B H 0.223(5) 0.439(3) 0.370(4) 0.15(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01652(6) 0.01195(5) 0.01407(5) -0.00132(3) 0.00375(4) -0.00036(3) F7 0.0253(7) 0.0220(7) 0.0227(6) -0.0104(5) 0.0050(5) -0.0040(5) F6 0.0240(7) 0.0205(6) 0.0227(6) -0.0065(5) 0.0094(5) 0.0006(5) F5 0.0263(7) 0.0245(7) 0.0241(6) -0.0131(5) 0.0030(5) 0.0007(5) F2 0.0441(8) 0.0202(7) 0.0163(6) 0.0021(5) 0.0026(6) 0.0078(6) F3 0.0401(8) 0.0169(6) 0.0287(7) 0.0057(5) 0.0046(6) 0.0108(6) F4 0.0338(7) 0.0228(7) 0.0181(6) 0.0052(5) 0.0020(5) 0.0056(5) F8 0.0237(7) 0.0269(7) 0.0294(7) -0.0104(6) 0.0082(6) 0.0042(5) F1 0.0408(8) 0.0137(6) 0.0199(6) 0.0029(5) 0.0017(6) 0.0083(6) O5 0.0391(10) 0.0263(10) 0.0169(8) -0.0030(7) 0.0062(7) -0.0138(8) O4 0.0208(9) 0.0173(9) 0.0351(9) 0.0001(7) 0.0051(7) -0.0017(7) N1 0.0307(10) 0.0184(10) 0.0170(8) -0.0015(7) 0.0055(8) 0.0004(8) O1 0.0281(9) 0.0173(9) 0.0376(10) -0.0046(7) 0.0174(8) -0.0011(7) O3 0.0253(9) 0.0186(9) 0.0428(11) -0.0101(8) 0.0053(8) 0.0009(7) C19 0.0227(11) 0.0128(10) 0.0206(10) 0.0039(8) 0.0032(8) 0.0034(8) O2 0.0289(9) 0.0191(8) 0.0208(8) 0.0038(7) 0.0008(7) -0.0048(7) O6 0.0249(8) 0.0196(8) 0.0213(9) 0.0009(7) 0.0086(7) 0.0062(7) N7 0.0243(11) 0.0329(12) 0.0381(12) -0.0125(9) 0.0011(9) -0.0001(9) C28 0.0233(11) 0.0159(10) 0.0210(10) -0.0008(8) 0.0051(9) 0.0001(8) C6 0.0243(11) 0.0168(10) 0.0154(9) 0.0007(8) 0.0012(8) -0.0024(8) C16 0.0209(11) 0.0153(10) 0.0245(11) 0.0058(8) 0.0048(9) 0.0027(8) C26 0.0234(11) 0.0156(10) 0.0191(10) -0.0006(8) 0.0083(8) 0.0027(8) C13 0.0206(10) 0.0165(10) 0.0183(10) 0.0016(8) 0.0038(8) -0.0016(8) C20 0.0236(11) 0.0155(10) 0.0231(11) 0.0019(8) 0.0077(9) 0.0021(8) N6 0.0289(11) 0.0308(11) 0.0233(10) -0.0015(8) 0.0075(8) 0.0018(8) C4 0.0265(12) 0.0157(10) 0.0292(12) -0.0029(9) 0.0099(10) 0.0010(8) C5 0.0204(10) 0.0155(10) 0.0182(10) 0.0043(8) 0.0058(8) 0.0021(8) N5 0.0223(9) 0.0191(9) 0.0195(9) -0.0021(7) 0.0043(7) -0.0006(7) C24 0.0247(11) 0.0136(10) 0.0143(9) -0.0026(8) 0.0055(8) -0.0032(8) C21 0.0227(10) 0.0159(10) 0.0136(9) 0.0002(8) 0.0042(8) -0.0018(8) C27 0.0265(11) 0.0141(10) 0.0149(9) -0.0023(8) 0.0049(8) 0.0005(8) C18 0.0229(11) 0.0187(11) 0.0168(10) 0.0013(8) 0.0032(8) 0.0004(8) N2 0.0350(11) 0.0283(11) 0.0187(9) 0.0012(8) 0.0047(8) -0.0064(9) C14 0.0172(10) 0.0171(10) 0.0190(10) 0.0018(8) 0.0044(8) -0.0018(8) C17 0.0181(10) 0.0161(10) 0.0224(10) 0.0016(8) 0.0051(8) -0.0008(8) C25 0.0232(11) 0.0146(10) 0.0159(9) 0.0034(8) 0.0052(8) -0.0006(8) C7 0.0203(11) 0.0240(12) 0.0266(11) 0.0002(9) 0.0043(9) 0.0030(9) C23 0.0262(11) 0.0134(10) 0.0147(9) 0.0005(8) 0.0081(8) 0.0016(8) C22 0.0232(10) 0.0136(10) 0.0139(9) 0.0012(8) 0.0044(8) 0.0005(8) C15 0.0201(10) 0.0185(10) 0.0160(10) 0.0048(8) 0.0012(8) -0.0001(8) C2 0.0223(11) 0.0149(10) 0.0241(11) -0.0007(8) 0.0034(9) -0.0034(8) N4 0.0442(13) 0.0240(11) 0.0284(11) 0.0011(9) 0.0132(9) 0.0031(9) N3 0.0459(13) 0.0247(11) 0.0392(12) -0.0028(9) 0.0060(10) 0.0124(10) C1 0.0212(10) 0.0209(11) 0.0149(9) -0.0027(8) 0.0045(8) -0.0011(8) C3 0.0278(12) 0.0222(12) 0.0257(11) -0.0026(9) 0.0075(9) 0.0024(9) F9 0.0325(7) 0.0182(7) 0.0221(6) -0.0047(5) 0.0049(5) -0.0062(5) F12 0.0378(8) 0.0197(6) 0.0150(6) -0.0034(5) 0.0043(5) -0.0043(5) F11 0.0391(8) 0.0152(6) 0.0226(6) -0.0026(5) 0.0081(6) -0.0039(5) F10 0.0378(8) 0.0258(7) 0.0140(6) -0.0015(5) 0.0026(5) -0.0038(6) C9 0.0225(11) 0.0202(11) 0.0230(11) 0.0075(9) 0.0043(9) 0.0012(8) C30 0.0181(10) 0.0167(10) 0.0179(10) -0.0004(8) 0.0051(8) 0.0027(8) C35 0.0182(10) 0.0160(10) 0.0193(10) -0.0041(8) 0.0035(8) -0.0014(8) N12 0.0489(14) 0.0378(13) 0.0222(11) 0.0068(9) 0.0040(10) -0.0063(10) C36 0.0261(12) 0.0191(11) 0.0209(10) 0.0027(9) 0.0063(9) 0.0035(9) C31 0.0215(11) 0.0179(10) 0.0144(9) -0.0026(8) 0.0036(8) 0.0010(8) C11 0.0375(14) 0.0233(13) 0.0228(11) 0.0076(9) 0.0116(10) 0.0040(10) C29 0.0218(11) 0.0168(10) 0.0190(10) 0.0010(8) 0.0053(8) 0.0008(8) C34 0.0204(10) 0.0210(11) 0.0146(9) -0.0021(8) 0.0024(8) 0.0017(8) C33 0.0192(10) 0.0173(10) 0.0180(10) 0.0013(8) 0.0049(8) 0.0040(8) N11 0.0620(16) 0.0202(12) 0.0369(13) 0.0038(9) 0.0182(12) 0.0020(10) C10 0.0239(11) 0.0211(12) 0.0208(10) 0.0047(9) 0.0075(9) 0.0021(9) C32 0.0221(11) 0.0137(10) 0.0212(10) -0.0028(8) 0.0065(9) 0.0002(8) N10 0.0376(12) 0.0194(10) 0.0328(11) 0.0019(8) 0.0090(9) 0.0001(8) C12 0.0285(12) 0.0235(12) 0.0261(12) 0.0074(9) 0.0062(10) 0.0006(9) O8 0.0466(12) 0.0224(10) 0.0298(10) 0.0011(8) 0.0154(9) 0.0047(8) O7 0.0378(10) 0.0222(9) 0.0283(9) -0.0007(8) 0.0140(8) 0.0003(7) O9 0.0484(13) 0.0234(10) 0.0417(12) 0.0068(9) 0.0067(10) 0.0001(9) N9 0.0389(12) 0.0297(11) 0.0186(10) 0.0026(8) 0.0055(9) -0.0024(9) N8 0.0290(11) 0.0371(13) 0.0478(14) -0.0146(10) 0.0087(10) 0.0039(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O1 2.3055(18) . ? Dy1 O2 2.3263(17) . ? Dy1 O5 2.3379(18) . ? Dy1 O6 2.3517(16) . ? Dy1 O4 2.3640(17) . ? Dy1 O3 2.3687(17) . ? Dy1 N5 2.4950(19) . ? Dy1 N1 2.5124(19) . ? F7 C24 1.347(2) . ? F6 C23 1.345(2) . ? F5 C27 1.341(2) . ? F2 C18 1.340(2) . ? F3 C16 1.342(2) . ? F4 C15 1.341(2) . ? F8 C26 1.346(2) . ? F1 C19 1.348(2) . ? O5 H5A 0.79(4) . ? O5 H5B 0.77(4) . ? O4 H4B 0.75(3) . ? O4 H4A 0.85(4) . ? N1 C1 1.147(3) . ? O1 H1A 0.77(3) . ? O1 H1B 0.82(4) . ? O3 H3A 0.89(4) . ? O3 H3B 0.80(6) . ? C19 C18 1.361(3) . ? C19 C14 1.412(3) . ? O2 H2A 0.79(3) . ? O2 H2B 0.87(3) . ? O6 H6B 0.74(3) . ? O6 H6A 0.80(3) . ? N7 C7 1.151(3) . ? C28 C7 1.418(3) . ? C28 C25 1.419(3) . ? C28 C8 1.423(3) 3_666 ? C6 N6 1.145(3) . ? C6 C21 1.419(3) . ? C16 C15 1.356(3) . ? C16 C17 1.423(3) . ? C26 C27 1.355(3) . ? C26 C25 1.417(3) . ? C13 C14 1.421(3) . ? C13 C1 1.423(3) . ? C13 C2 1.425(3) . ? C20 C17 1.416(3) . ? C20 C3 1.425(3) . ? C20 C4 1.426(3) . ? C4 N4 1.150(3) . ? C5 N5 1.148(3) . ? C5 C21 1.419(3) . ? C24 C23 1.351(3) . ? C24 C25 1.418(3) . ? C21 C22 1.421(3) . ? C27 C22 1.415(3) . ? C18 C17 1.415(3) . ? N2 C2 1.147(3) . ? C14 C15 1.426(3) . ? C23 C22 1.417(3) . ? N3 C3 1.149(3) . ? F9 C35 1.344(2) . ? F12 C31 1.347(2) . ? F11 C32 1.342(2) . ? F10 C34 1.345(2) . ? C9 N9 1.144(3) . ? C9 C29 1.424(3) . ? C30 C31 1.413(3) . ? C30 C35 1.418(3) . ? C30 C29 1.418(3) . ? C35 C34 1.356(3) . ? N12 C12 1.147(3) . ? C36 C33 1.412(3) . ? C36 C12 1.422(3) . ? C36 C11 1.427(3) . ? C31 C32 1.360(3) . ? C11 N11 1.147(3) . ? C29 C10 1.421(3) . ? C34 C33 1.425(3) . ? C33 C32 1.416(3) . ? C10 N10 1.151(3) . ? O8 H8A 0.87(4) . ? O8 H8B 0.81(4) . ? O7 H7A 0.81(3) . ? O7 H7B 0.82(4) . ? O9 H9A 0.77(4) . ? O9 H9B 0.77(4) . ? N8 C8 1.148(3) . ? C8 C28 1.423(3) 3_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Dy1 O2 98.21(7) . . ? O1 Dy1 O5 88.73(7) . . ? O2 Dy1 O5 148.43(7) . . ? O1 Dy1 O6 143.82(6) . . ? O2 Dy1 O6 80.46(6) . . ? O5 Dy1 O6 111.33(7) . . ? O1 Dy1 O4 142.15(6) . . ? O2 Dy1 O4 78.13(7) . . ? O5 Dy1 O4 77.68(7) . . ? O6 Dy1 O4 73.41(6) . . ? O1 Dy1 O3 70.86(6) . . ? O2 Dy1 O3 76.76(7) . . ? O5 Dy1 O3 76.59(7) . . ? O6 Dy1 O3 141.37(6) . . ? O4 Dy1 O3 71.66(7) . . ? O1 Dy1 N5 72.13(6) . . ? O2 Dy1 N5 71.84(6) . . ? O5 Dy1 N5 138.94(6) . . ? O6 Dy1 N5 73.21(6) . . ? O4 Dy1 N5 137.99(6) . . ? O3 Dy1 N5 126.50(7) . . ? O1 Dy1 N1 84.21(6) . . ? O2 Dy1 N1 141.48(6) . . ? O5 Dy1 N1 69.65(6) . . ? O6 Dy1 N1 75.81(6) . . ? O4 Dy1 N1 122.02(7) . . ? O3 Dy1 N1 138.19(6) . . ? N5 Dy1 N1 72.48(6) . . ? Dy1 O5 H5A 115(3) . . ? Dy1 O5 H5B 119(3) . . ? H5A O5 H5B 115(4) . . ? Dy1 O4 H4B 123(2) . . ? Dy1 O4 H4A 123(2) . . ? H4B O4 H4A 110(3) . . ? C1 N1 Dy1 174.44(16) . . ? Dy1 O1 H1A 125(2) . . ? Dy1 O1 H1B 125(2) . . ? H1A O1 H1B 109(3) . . ? Dy1 O3 H3A 120(2) . . ? Dy1 O3 H3B 132(4) . . ? H3A O3 H3B 102(5) . . ? F1 C19 C18 117.18(19) . . ? F1 C19 C14 118.87(18) . . ? C18 C19 C14 123.86(19) . . ? Dy1 O2 H2A 123(2) . . ? Dy1 O2 H2B 122(2) . . ? H2A O2 H2B 108(3) . . ? Dy1 O6 H6B 121(2) . . ? Dy1 O6 H6A 126(2) . . ? H6B O6 H6A 111(3) . . ? C7 C28 C25 122.9(2) . . ? C7 C28 C8 113.7(2) . 3_666 ? C25 C28 C8 123.3(2) . 3_666 ? N6 C6 C21 175.7(2) . . ? F3 C16 C15 118.28(19) . . ? F3 C16 C17 118.24(19) . . ? C15 C16 C17 123.48(19) . . ? F8 C26 C27 117.94(18) . . ? F8 C26 C25 118.83(19) . . ? C27 C26 C25 123.22(19) . . ? C14 C13 C1 120.68(19) . . ? C14 C13 C2 123.98(19) . . ? C1 C13 C2 115.17(18) . . ? C17 C20 C3 123.4(2) . . ? C17 C20 C4 123.11(19) . . ? C3 C20 C4 112.95(19) . . ? N4 C4 C20 176.8(2) . . ? N5 C5 C21 175.0(2) . . ? C5 N5 Dy1 171.26(17) . . ? F7 C24 C23 117.74(18) . . ? F7 C24 C25 118.43(18) . . ? C23 C24 C25 123.82(19) . . ? C5 C21 C6 112.88(18) . . ? C5 C21 C22 123.01(19) . . ? C6 C21 C22 124.09(19) . . ? F5 C27 C26 118.35(19) . . ? F5 C27 C22 118.16(19) . . ? C26 C27 C22 123.47(19) . . ? F2 C18 C19 117.59(19) . . ? F2 C18 C17 118.82(18) . . ? C19 C18 C17 123.56(19) . . ? C19 C14 C13 123.10(19) . . ? C19 C14 C15 112.67(18) . . ? C13 C14 C15 124.23(19) . . ? C18 C17 C20 122.16(19) . . ? C18 C17 C16 112.84(19) . . ? C20 C17 C16 125.0(2) . . ? C26 C25 C24 113.00(19) . . ? C26 C25 C28 123.70(19) . . ? C24 C25 C28 123.30(19) . . ? N7 C7 C28 177.0(2) . . ? F6 C23 C24 118.18(18) . . ? F6 C23 C22 118.75(19) . . ? C24 C23 C22 123.04(19) . . ? C27 C22 C23 113.35(19) . . ? C27 C22 C21 122.99(19) . . ? C23 C22 C21 123.66(19) . . ? F4 C15 C16 118.10(19) . . ? F4 C15 C14 118.35(18) . . ? C16 C15 C14 123.55(19) . . ? N2 C2 C13 176.6(3) . . ? N1 C1 C13 179.2(2) . . ? N3 C3 C20 175.2(3) . . ? N9 C9 C29 177.7(3) . . ? C31 C30 C35 113.15(18) . . ? C31 C30 C29 123.10(19) . . ? C35 C30 C29 123.8(2) . . ? F9 C35 C34 118.15(18) . . ? F9 C35 C30 118.37(18) . . ? C34 C35 C30 123.4(2) . . ? C33 C36 C12 121.9(2) . . ? C33 C36 C11 123.2(2) . . ? C12 C36 C11 114.6(2) . . ? F12 C31 C32 117.75(19) . . ? F12 C31 C30 118.55(18) . . ? C32 C31 C30 123.63(19) . . ? N11 C11 C36 177.5(3) . . ? C30 C29 C10 123.42(19) . . ? C30 C29 C9 122.0(2) . . ? C10 C29 C9 114.40(19) . . ? F10 C34 C35 117.63(19) . . ? F10 C34 C33 118.90(18) . . ? C35 C34 C33 123.45(19) . . ? C36 C33 C32 122.8(2) . . ? C36 C33 C34 124.3(2) . . ? C32 C33 C34 112.91(18) . . ? N10 C10 C29 177.0(2) . . ? F11 C32 C31 117.90(19) . . ? F11 C32 C33 118.62(18) . . ? C31 C32 C33 123.4(2) . . ? N12 C12 C36 178.4(3) . . ? H8A O8 H8B 109(4) . . ? H7A O7 H7B 103(3) . . ? H9A O9 H9B 118(4) . . ? N8 C8 C28 176.9(3) . 3_666 ? 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 O1 Dy1 N1 C1 -115.8(18) . . . . ? O2 Dy1 N1 C1 -19.9(19) . . . . ? O5 Dy1 N1 C1 153.4(19) . . . . ? O6 Dy1 N1 C1 33.8(18) . . . . ? O4 Dy1 N1 C1 93.4(18) . . . . ? O3 Dy1 N1 C1 -168.4(18) . . . . ? N5 Dy1 N1 C1 -42.8(18) . . . . ? C17 C20 C4 N4 -148(5) . . . . ? C3 C20 C4 N4 24(5) . . . . ? C21 C5 N5 Dy1 -52(3) . . . . ? O1 Dy1 N5 C5 -148.1(11) . . . . ? O2 Dy1 N5 C5 -42.9(11) . . . . ? O5 Dy1 N5 C5 145.8(11) . . . . ? O6 Dy1 N5 C5 42.4(11) . . . . ? O4 Dy1 N5 C5 3.7(12) . . . . ? O3 Dy1 N5 C5 -100.0(11) . . . . ? N1 Dy1 N5 C5 122.4(11) . . . . ? N5 C5 C21 C6 7(3) . . . . ? N5 C5 C21 C22 -175(3) . . . . ? N6 C6 C21 C5 16(3) . . . . ? N6 C6 C21 C22 -162(3) . . . . ? F8 C26 C27 F5 -0.2(3) . . . . ? C25 C26 C27 F5 179.72(19) . . . . ? F8 C26 C27 C22 177.97(18) . . . . ? C25 C26 C27 C22 -2.1(3) . . . . ? F1 C19 C18 F2 -0.3(3) . . . . ? C14 C19 C18 F2 -176.8(2) . . . . ? F1 C19 C18 C17 177.88(19) . . . . ? C14 C19 C18 C17 1.4(4) . . . . ? F1 C19 C14 C13 3.0(3) . . . . ? C18 C19 C14 C13 179.5(2) . . . . ? F1 C19 C14 C15 -176.87(18) . . . . ? C18 C19 C14 C15 -0.4(3) . . . . ? C1 C13 C14 C19 14.1(3) . . . . ? C2 C13 C14 C19 -170.7(2) . . . . ? C1 C13 C14 C15 -166.0(2) . . . . ? C2 C13 C14 C15 9.2(3) . . . . ? F2 C18 C17 C20 -1.9(3) . . . . ? C19 C18 C17 C20 180.0(2) . . . . ? F2 C18 C17 C16 177.67(19) . . . . ? C19 C18 C17 C16 -0.5(3) . . . . ? C3 C20 C17 C18 179.5(2) . . . . ? C4 C20 C17 C18 -9.2(3) . . . . ? C3 C20 C17 C16 0.0(4) . . . . ? C4 C20 C17 C16 171.3(2) . . . . ? F3 C16 C17 C18 179.17(18) . . . . ? C15 C16 C17 C18 -1.3(3) . . . . ? F3 C16 C17 C20 -1.3(3) . . . . ? C15 C16 C17 C20 178.2(2) . . . . ? F8 C26 C25 C24 179.04(18) . . . . ? C27 C26 C25 C24 -0.9(3) . . . . ? F8 C26 C25 C28 -0.3(3) . . . . ? C27 C26 C25 C28 179.8(2) . . . . ? F7 C24 C25 C26 -176.69(18) . . . . ? C23 C24 C25 C26 2.4(3) . . . . ? F7 C24 C25 C28 2.6(3) . . . . ? C23 C24 C25 C28 -178.3(2) . . . . ? C7 C28 C25 C26 176.9(2) . . . . ? C8 C28 C25 C26 -1.3(3) 3_666 . . . ? C7 C28 C25 C24 -2.3(3) . . . . ? C8 C28 C25 C24 179.5(2) 3_666 . . . ? C25 C28 C7 N7 -163(5) . . . . ? C8 C28 C7 N7 16(5) 3_666 . . . ? F7 C24 C23 F6 0.0(3) . . . . ? C25 C24 C23 F6 -179.08(18) . . . . ? F7 C24 C23 C22 178.07(18) . . . . ? C25 C24 C23 C22 -1.0(3) . . . . ? F5 C27 C22 C23 -178.44(17) . . . . ? C26 C27 C22 C23 3.4(3) . . . . ? F5 C27 C22 C21 0.9(3) . . . . ? C26 C27 C22 C21 -177.2(2) . . . . ? F6 C23 C22 C27 176.17(17) . . . . ? C24 C23 C22 C27 -1.9(3) . . . . ? F6 C23 C22 C21 -3.2(3) . . . . ? C24 C23 C22 C21 178.77(19) . . . . ? C5 C21 C22 C27 -5.8(3) . . . . ? C6 C21 C22 C27 172.4(2) . . . . ? C5 C21 C22 C23 173.53(19) . . . . ? C6 C21 C22 C23 -8.3(3) . . . . ? F3 C16 C15 F4 0.9(3) . . . . ? C17 C16 C15 F4 -178.62(19) . . . . ? F3 C16 C15 C14 -178.12(19) . . . . ? C17 C16 C15 C14 2.4(3) . . . . ? C19 C14 C15 F4 179.61(19) . . . . ? C13 C14 C15 F4 -0.3(3) . . . . ? C19 C14 C15 C16 -1.4(3) . . . . ? C13 C14 C15 C16 178.7(2) . . . . ? C14 C13 C2 N2 144(4) . . . . ? C1 C13 C2 N2 -41(4) . . . . ? Dy1 N1 C1 C13 -55(21) . . . . ? C14 C13 C1 N1 61(21) . . . . ? C2 C13 C1 N1 -115(20) . . . . ? C17 C20 C3 N3 176(3) . . . . ? C4 C20 C3 N3 4(3) . . . . ? C31 C30 C35 F9 177.27(18) . . . . ? C29 C30 C35 F9 -3.1(3) . . . . ? C31 C30 C35 C34 0.0(3) . . . . ? C29 C30 C35 C34 179.7(2) . . . . ? C35 C30 C31 F12 177.44(18) . . . . ? C29 C30 C31 F12 -2.2(3) . . . . ? C35 C30 C31 C32 0.3(3) . . . . ? C29 C30 C31 C32 -179.4(2) . . . . ? C33 C36 C11 N11 149(6) . . . . ? C12 C36 C11 N11 -26(6) . . . . ? C31 C30 C29 C10 172.6(2) . . . . ? C35 C30 C29 C10 -7.0(3) . . . . ? C31 C30 C29 C9 -13.1(3) . . . . ? C35 C30 C29 C9 167.2(2) . . . . ? N9 C9 C29 C30 -151(6) . . . . ? N9 C9 C29 C10 24(7) . . . . ? F9 C35 C34 F10 0.7(3) . . . . ? C30 C35 C34 F10 177.98(19) . . . . ? F9 C35 C34 C33 -177.68(18) . . . . ? C30 C35 C34 C33 -0.4(3) . . . . ? C12 C36 C33 C32 -175.1(2) . . . . ? C11 C36 C33 C32 10.7(3) . . . . ? C12 C36 C33 C34 5.3(3) . . . . ? C11 C36 C33 C34 -168.9(2) . . . . ? F10 C34 C33 C36 1.8(3) . . . . ? C35 C34 C33 C36 -179.8(2) . . . . ? F10 C34 C33 C32 -177.90(18) . . . . ? C35 C34 C33 C32 0.5(3) . . . . ? C30 C29 C10 N10 -164(5) . . . . ? C9 C29 C10 N10 22(5) . . . . ? F12 C31 C32 F11 0.1(3) . . . . ? C30 C31 C32 F11 177.24(18) . . . . ? F12 C31 C32 C33 -177.38(19) . . . . ? C30 C31 C32 C33 -0.2(3) . . . . ? C36 C33 C32 F11 2.7(3) . . . . ? C34 C33 C32 F11 -177.62(18) . . . . ? C36 C33 C32 C31 -179.9(2) . . . . ? C34 C33 C32 C31 -0.2(3) . . . . ? C33 C36 C12 N12 180(100) . . . . ? C11 C36 C12 N12 -6(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.362 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.080 # Attachment 'ErTCNQF4.CIF' data_g:\nazari~1\nazari~1\crysta~1\nl088e~1\platon _database_code_depnum_ccdc_archive 'CCDC 749361' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Erbium(III) 2,3,5,6-Tetrafluoro-7,7,8,8-Tetracyanoquinodimethane' ; _chemical_name_common ;Erbium(iii) 2,3,5,6-Tetrafluoro-7,7,8,8- Tetracyanoquinodimethane' ; _chemical_melting_point ? _chemical_formula_sum 'C36 H18 Er F12 N12 O9' _chemical_formula_weight 1157.88 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' Er Er -0.2586 4.9576 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.651(3) _cell_length_b 17.646(5) _cell_length_c 17.024(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.122(8) _cell_angle_gamma 90.00 _cell_volume 3993.8(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.926 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 2.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4704 _exptl_absorpt_correction_T_max 0.5947 _exptl_absorpt_process_details 'SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40642 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9597 _reflns_number_gt 9136 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0228P)^2^+4.3379P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9597 _refine_ls_number_parameters 672 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0514 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er -0.698182(6) 0.409124(4) -0.935615(5) 0.01125(3) Uani 1 1 d . . . F1 F -0.70586(9) 0.15939(6) -1.00162(7) 0.0199(2) Uani 1 1 d . . . F2 F -0.56260(9) -0.00854(7) -0.78847(7) 0.0193(2) Uani 1 1 d . . . F3 F -0.69391(9) 0.05437(7) -1.10634(7) 0.0215(2) Uani 1 1 d . . . F4 F -0.54497(9) -0.11274(7) -0.89460(7) 0.0220(2) Uani 1 1 d . . . F5 F -1.02422(9) 0.30966(7) -1.09416(7) 0.0201(2) Uani 1 1 d . . . F6 F -0.95476(8) 0.12321(6) -1.27410(7) 0.0171(2) Uani 1 1 d . . . F7 F -1.21768(8) 0.29003(7) -1.15039(7) 0.0200(2) Uani 1 1 d . . . F8 F -1.14799(9) 0.10073(6) -1.32825(7) 0.0180(2) Uani 1 1 d . . . F9 F -0.06452(9) 0.52723(7) -0.36498(7) 0.0206(2) Uani 1 1 d . . . F10 F -0.22454(9) 0.36251(6) -0.57630(7) 0.0198(2) Uani 1 1 d . . . F11 F -0.05060(9) 0.63131(6) -0.47152(7) 0.0191(2) Uani 1 1 d . . . F12 F -0.21075(9) 0.46698(6) -0.68227(7) 0.0190(2) Uani 1 1 d . . . O1 O -0.74522(12) 0.47204(9) -1.05683(9) 0.0186(3) Uani 1 1 d . . . O2 O -0.85389(11) 0.39653(9) -0.90841(9) 0.0199(3) Uani 1 1 d . . . O3 O -0.75151(12) 0.52744(9) -0.89853(11) 0.0226(3) Uani 1 1 d . . . O4 O -0.62890(12) 0.41418(9) -0.79831(9) 0.0211(3) Uani 1 1 d . . . O5 O -0.56607(11) 0.49575(9) -0.92746(9) 0.0191(3) Uani 1 1 d . . . O6 O -0.58542(11) 0.35405(8) -1.00279(9) 0.0174(3) Uani 1 1 d . . . N1 N -0.67161(13) 0.27898(9) -0.87825(10) 0.0175(3) Uani 1 1 d . . . N2 N -0.61456(13) 0.12065(10) -0.67894(10) 0.0219(4) Uani 1 1 d . . . N3 N -0.64618(14) -0.06480(10) -1.21857(11) 0.0239(4) Uani 1 1 d . . . N4 N -0.54357(15) -0.22607(11) -1.03693(12) 0.0286(4) Uani 1 1 d . . . N5 N -0.79653(12) 0.32053(9) -1.03558(10) 0.0159(3) Uani 1 1 d . . . N6 N -0.73352(13) 0.18183(10) -1.21671(10) 0.0209(3) Uani 1 1 d . . . N7 N -1.43829(14) 0.25843(11) -1.22942(12) 0.0283(4) Uani 1 1 d . . . N8 N -1.37323(13) 0.08476(10) -1.38239(12) 0.0238(4) Uani 1 1 d . . . N9 N -0.10402(16) 0.40328(11) -0.25479(12) 0.0285(4) Uani 1 1 d . . . N10 N -0.19991(16) 0.24198(11) -0.44580(12) 0.0301(4) Uani 1 1 d . . . N11 N -0.06852(14) 0.74942(10) -0.60718(11) 0.0236(4) Uani 1 1 d . . . N12 N -0.14976(14) 0.58250(10) -0.79251(11) 0.0227(4) Uani 1 1 d . . . C1 C -0.65812(14) 0.21705(11) -0.85748(11) 0.0151(4) Uani 1 1 d . . . C2 C -0.62353(14) 0.12832(11) -0.74711(12) 0.0167(4) Uani 1 1 d . . . C3 C -0.64033(14) 0.14055(11) -0.83220(11) 0.0149(3) Uani 1 1 d . . . C4 C -0.63228(14) 0.08252(10) -0.88855(11) 0.0140(3) Uani 1 1 d . . . C5 C -0.66353(15) 0.09309(10) -0.97324(12) 0.0154(4) Uani 1 1 d . . . C6 C -0.59376(14) 0.00867(11) -0.86702(11) 0.0155(4) Uani 1 1 d . . . C7 C -0.65727(14) 0.03839(11) -1.02793(11) 0.0154(3) Uani 1 1 d . . . C8 C -0.58549(14) -0.04571(10) -0.92210(12) 0.0156(3) Uani 1 1 d . . . C9 C -0.61763(14) -0.03493(10) -1.00700(11) 0.0150(3) Uani 1 1 d . . . C10 C -0.61244(15) -0.09100(10) -1.06564(12) 0.0167(4) Uani 1 1 d . . . C11 C -0.63277(15) -0.07502(11) -1.15006(12) 0.0181(4) Uani 1 1 d . . . C12 C -0.57400(15) -0.16539(12) -1.04653(12) 0.0196(4) Uani 1 1 d . . . C13 C -0.83537(14) 0.28280(11) -1.08877(11) 0.0150(3) Uani 1 1 d . . . C14 C -0.79918(14) 0.20358(11) -1.19066(11) 0.0160(4) Uani 1 1 d . . . C15 C -0.87462(14) 0.23442(10) -1.15502(11) 0.0144(3) Uani 1 1 d . . . C16 C -0.97901(14) 0.22036(10) -1.18358(11) 0.0138(3) Uani 1 1 d . . . C17 C -1.05376(14) 0.25870(10) -1.15339(11) 0.0147(3) Uani 1 1 d . . . C18 C -1.01887(14) 0.16634(10) -1.24415(11) 0.0142(3) Uani 1 1 d . . . C19 C -1.15415(14) 0.24821(10) -1.18233(11) 0.0150(3) Uani 1 1 d . . . C20 C -1.11921(14) 0.15491(10) -1.27225(11) 0.0146(3) Uani 1 1 d . . . C21 C -1.19410(14) 0.19596(10) -1.24477(11) 0.0140(3) Uani 1 1 d . . . C22 C -1.29874(14) 0.18478(11) -1.27543(11) 0.0158(4) Uani 1 1 d . . . C23 C -1.37439(15) 0.22629(11) -1.24879(12) 0.0193(4) Uani 1 1 d . . . C24 C -1.33765(14) 0.12937(11) -1.33497(12) 0.0175(4) Uani 1 1 d . . . C25 C -0.12548(15) 0.39422(12) -0.32317(13) 0.0204(4) Uani 1 1 d . . . C26 C -0.18000(16) 0.30452(12) -0.43057(12) 0.0206(4) Uani 1 1 d . . . C27 C -0.15314(15) 0.38109(11) -0.40782(12) 0.0180(4) Uani 1 1 d . . . C28 C -0.14503(14) 0.43826(11) -0.46440(11) 0.0153(3) Uani 1 1 d . . . C29 C -0.10263(14) 0.51115(11) -0.44320(11) 0.0153(3) Uani 1 1 d . . . C30 C -0.17900(14) 0.42812(11) -0.54881(12) 0.0151(3) Uani 1 1 d . . . C31 C -0.09574(14) 0.56555(11) -0.49853(11) 0.0151(3) Uani 1 1 d . . . C32 C -0.17192(14) 0.48236(11) -0.60408(11) 0.0150(3) Uani 1 1 d . . . C33 C -0.12992(13) 0.55497(10) -0.58302(11) 0.0141(3) Uani 1 1 d . . . C34 C -0.12343(14) 0.61133(11) -0.64083(11) 0.0156(3) Uani 1 1 d . . . C35 C -0.09219(14) 0.68720(11) -0.62007(11) 0.0174(4) Uani 1 1 d . . . C36 C -0.13933(15) 0.59435(11) -0.72468(12) 0.0172(4) Uani 1 1 d . . . H1A H -0.777(2) 0.4525(19) -1.094(2) 0.037(8) Uiso 1 1 d . . . H2A H -0.882(2) 0.3559(19) -0.9042(18) 0.039(8) Uiso 1 1 d . . . H3A H -0.789(2) 0.5551(17) -0.9296(17) 0.027(7) Uiso 1 1 d . . . H4A H -0.651(2) 0.3872(19) -0.769(2) 0.042(9) Uiso 1 1 d . . . H5A H -0.506(2) 0.4820(17) -0.9207(17) 0.033(7) Uiso 1 1 d . . . H6A H -0.589(2) 0.3612(17) -1.0470(18) 0.029(8) Uiso 1 1 d . . . H1B H -0.710(2) 0.5021(18) -1.0658(17) 0.032(8) Uiso 1 1 d . . . H2B H -0.888(3) 0.431(2) -0.898(2) 0.045(9) Uiso 1 1 d . . . H4B H -0.622(3) 0.456(2) -0.776(2) 0.052(10) Uiso 1 1 d . . . H5B H -0.570(2) 0.5398(17) -0.9211(17) 0.028(7) Uiso 1 1 d . . . H6B H -0.545(2) 0.3190(18) -0.9862(18) 0.038(8) Uiso 1 1 d . . . O1S O -0.39736(12) 0.14733(9) -0.58066(10) 0.0288(3) Uiso 1 1 d . . . O2S O -0.10529(12) 0.09657(9) -0.49131(10) 0.0249(3) Uiso 1 1 d . . . O3S O -0.01431(11) 0.01357(9) -0.60294(10) 0.0225(3) Uiso 1 1 d . . . H3SB H -0.021(3) 0.049(2) -0.571(2) 0.061(10) Uiso 1 1 d . . . H3SA H -0.035(3) 0.034(2) -0.646(2) 0.055(10) Uiso 1 1 d . . . H3B H -0.733(4) 0.553(3) -0.862(3) 0.12(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01204(5) 0.01026(5) 0.01141(5) -0.00097(3) 0.00258(3) -0.00025(3) F1 0.0299(6) 0.0128(5) 0.0150(5) 0.0026(4) 0.0010(4) 0.0069(4) F2 0.0246(6) 0.0183(6) 0.0134(5) 0.0044(4) 0.0007(4) 0.0035(4) F3 0.0330(7) 0.0173(6) 0.0129(5) 0.0023(4) 0.0022(5) 0.0062(5) F4 0.0300(6) 0.0135(5) 0.0211(6) 0.0042(5) 0.0029(5) 0.0080(5) F5 0.0196(6) 0.0202(6) 0.0192(6) -0.0108(5) 0.0021(4) -0.0003(4) F6 0.0176(5) 0.0172(6) 0.0179(5) -0.0048(4) 0.0070(4) 0.0009(4) F7 0.0178(5) 0.0203(6) 0.0227(6) -0.0080(5) 0.0061(4) 0.0026(4) F8 0.0185(6) 0.0173(6) 0.0180(6) -0.0080(4) 0.0037(4) -0.0024(4) F9 0.0269(6) 0.0222(6) 0.0116(5) -0.0011(4) 0.0020(4) -0.0032(5) F10 0.0277(6) 0.0130(5) 0.0186(6) -0.0027(4) 0.0055(5) -0.0039(4) F11 0.0232(6) 0.0157(6) 0.0178(5) -0.0033(4) 0.0031(4) -0.0049(4) F12 0.0270(6) 0.0171(6) 0.0123(5) -0.0022(4) 0.0032(4) -0.0034(4) O1 0.0205(7) 0.0167(7) 0.0171(7) 0.0029(6) 0.0012(6) -0.0041(6) O2 0.0191(7) 0.0151(7) 0.0283(8) -0.0027(6) 0.0115(6) -0.0016(6) O3 0.0193(7) 0.0164(7) 0.0312(8) -0.0078(6) 0.0034(6) 0.0015(6) O4 0.0287(8) 0.0201(8) 0.0140(7) -0.0023(6) 0.0036(6) -0.0093(6) O5 0.0164(7) 0.0130(7) 0.0273(8) -0.0006(6) 0.0038(6) -0.0014(5) O6 0.0193(7) 0.0176(7) 0.0166(7) 0.0007(6) 0.0065(5) 0.0044(5) N1 0.0229(8) 0.0157(8) 0.0135(7) -0.0009(6) 0.0036(6) 0.0008(6) N2 0.0240(9) 0.0232(9) 0.0179(8) 0.0001(7) 0.0037(7) -0.0041(7) N3 0.0320(10) 0.0192(9) 0.0219(9) 0.0001(7) 0.0093(7) 0.0017(7) N4 0.0360(11) 0.0200(9) 0.0281(10) -0.0005(7) 0.0035(8) 0.0084(8) N5 0.0156(7) 0.0164(8) 0.0156(7) -0.0012(6) 0.0037(6) -0.0007(6) N6 0.0215(8) 0.0233(9) 0.0191(8) 0.0002(7) 0.0071(7) 0.0011(7) N7 0.0207(9) 0.0296(10) 0.0338(10) -0.0094(8) 0.0048(8) 0.0023(7) N8 0.0166(8) 0.0248(9) 0.0288(10) -0.0076(7) 0.0024(7) 0.0002(7) N9 0.0359(11) 0.0288(10) 0.0192(9) 0.0045(7) 0.0027(8) -0.0040(8) N10 0.0454(12) 0.0185(10) 0.0289(10) 0.0031(7) 0.0138(9) 0.0013(8) N11 0.0275(9) 0.0185(9) 0.0255(9) 0.0015(7) 0.0074(7) 0.0005(7) N12 0.0277(9) 0.0223(9) 0.0174(9) 0.0022(7) 0.0038(7) -0.0016(7) C1 0.0162(8) 0.0181(9) 0.0114(8) -0.0034(7) 0.0039(6) -0.0017(7) C2 0.0175(9) 0.0129(9) 0.0192(9) 0.0003(7) 0.0034(7) -0.0022(7) C3 0.0165(9) 0.0137(9) 0.0141(8) 0.0012(7) 0.0024(7) -0.0008(6) C4 0.0136(8) 0.0135(8) 0.0148(9) 0.0006(7) 0.0031(7) -0.0015(6) C5 0.0174(9) 0.0116(9) 0.0168(9) 0.0034(7) 0.0029(7) 0.0021(6) C6 0.0159(8) 0.0164(9) 0.0131(8) 0.0039(7) 0.0010(6) -0.0008(7) C7 0.0171(9) 0.0157(9) 0.0130(8) 0.0028(7) 0.0026(7) 0.0013(7) C8 0.0154(8) 0.0118(8) 0.0192(9) 0.0040(7) 0.0034(7) 0.0025(6) C9 0.0136(8) 0.0133(9) 0.0184(9) 0.0008(7) 0.0044(7) 0.0002(6) C10 0.0181(9) 0.0142(9) 0.0185(9) 0.0002(7) 0.0058(7) 0.0006(7) C11 0.0186(9) 0.0128(8) 0.0242(10) -0.0018(7) 0.0073(7) 0.0003(7) C12 0.0202(9) 0.0201(10) 0.0185(9) -0.0018(7) 0.0043(7) 0.0021(7) C13 0.0154(8) 0.0144(9) 0.0158(8) 0.0026(7) 0.0046(7) 0.0012(7) C14 0.0194(9) 0.0148(9) 0.0124(8) 0.0000(7) 0.0007(7) -0.0024(7) C15 0.0170(9) 0.0132(8) 0.0131(8) -0.0007(7) 0.0036(7) -0.0003(7) C16 0.0167(9) 0.0122(8) 0.0122(8) 0.0007(6) 0.0025(6) -0.0003(6) C17 0.0194(9) 0.0118(8) 0.0131(8) -0.0023(7) 0.0042(7) -0.0003(7) C18 0.0183(9) 0.0122(8) 0.0137(8) -0.0005(7) 0.0066(7) 0.0013(6) C19 0.0191(9) 0.0121(8) 0.0150(8) -0.0007(7) 0.0065(7) 0.0017(6) C20 0.0203(9) 0.0118(8) 0.0118(8) -0.0025(7) 0.0036(7) -0.0017(7) C21 0.0162(8) 0.0131(8) 0.0129(8) 0.0007(7) 0.0035(6) -0.0007(6) C22 0.0173(9) 0.0139(9) 0.0157(8) -0.0024(7) 0.0029(7) -0.0003(7) C23 0.0195(9) 0.0182(9) 0.0188(9) -0.0030(7) 0.0012(7) -0.0019(7) C24 0.0143(8) 0.0186(9) 0.0191(9) -0.0002(7) 0.0028(7) 0.0016(7) C25 0.0201(10) 0.0194(9) 0.0219(10) 0.0051(8) 0.0049(8) 0.0004(7) C26 0.0255(10) 0.0196(10) 0.0180(9) 0.0054(8) 0.0077(7) 0.0033(8) C27 0.0208(9) 0.0165(9) 0.0168(9) 0.0025(7) 0.0047(7) 0.0020(7) C28 0.0149(8) 0.0148(9) 0.0166(9) 0.0015(7) 0.0044(7) 0.0031(7) C29 0.0164(8) 0.0178(9) 0.0111(8) -0.0014(7) 0.0020(6) 0.0011(7) C30 0.0163(9) 0.0115(8) 0.0177(9) -0.0021(7) 0.0045(7) 0.0003(7) C31 0.0144(8) 0.0138(9) 0.0171(9) -0.0027(7) 0.0034(7) -0.0002(6) C32 0.0168(9) 0.0152(9) 0.0129(8) -0.0019(7) 0.0029(7) 0.0008(7) C33 0.0137(8) 0.0138(9) 0.0150(8) -0.0004(7) 0.0035(6) 0.0009(6) C34 0.0163(9) 0.0149(9) 0.0157(9) 0.0002(7) 0.0038(7) 0.0016(7) C35 0.0174(9) 0.0187(10) 0.0168(9) 0.0035(7) 0.0056(7) 0.0017(7) C36 0.0179(9) 0.0156(9) 0.0182(9) 0.0043(7) 0.0046(7) 0.0000(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 O2 2.2867(15) . ? Er1 O1 2.3026(15) . ? Er1 O4 2.3156(16) . ? Er1 O6 2.3283(14) . ? Er1 O5 2.3441(15) . ? Er1 O3 2.3444(16) . ? Er1 N5 2.4709(17) . ? Er1 N1 2.4897(18) . ? F1 C5 1.345(2) . ? F2 C6 1.343(2) . ? F3 C7 1.345(2) . ? F4 C8 1.344(2) . ? F5 C17 1.343(2) . ? F6 C18 1.345(2) . ? F7 C19 1.344(2) . ? F8 C20 1.344(2) . ? F9 C29 1.345(2) . ? F10 C30 1.347(2) . ? F11 C31 1.345(2) . ? F12 C32 1.344(2) . ? O1 H1A 0.76(3) . ? O1 H1B 0.75(3) . ? O2 H2A 0.82(3) . ? O2 H2B 0.81(4) . ? O3 H3A 0.81(3) . ? O3 H3B 0.76(6) . ? O4 H4A 0.79(3) . ? O4 H4B 0.83(4) . ? O5 H5A 0.83(3) . ? O5 H5B 0.79(3) . ? O6 H6A 0.75(3) . ? O6 H6B 0.84(3) . ? N1 C1 1.150(3) . ? N2 C2 1.147(3) . ? N3 C11 1.153(3) . ? N4 C12 1.147(3) . ? N5 C13 1.152(3) . ? N6 C14 1.152(3) . ? N7 C23 1.150(3) . ? N8 C24 1.153(3) . ? N9 C25 1.145(3) . ? N10 C26 1.152(3) . ? N11 C35 1.151(3) . ? N12 C36 1.150(3) . ? C1 C3 1.421(3) . ? C2 C3 1.431(3) . ? C3 C4 1.424(3) . ? C4 C5 1.420(3) . ? C4 C6 1.422(3) . ? C5 C7 1.357(3) . ? C6 C8 1.364(3) . ? C7 C9 1.416(3) . ? C8 C9 1.425(3) . ? C9 C10 1.419(3) . ? C10 C12 1.424(3) . ? C10 C11 1.429(3) . ? C13 C15 1.419(3) . ? C14 C15 1.417(3) . ? C15 C16 1.419(3) . ? C16 C17 1.415(3) . ? C16 C18 1.419(3) . ? C17 C19 1.359(3) . ? C18 C20 1.360(3) . ? C19 C21 1.419(3) . ? C20 C21 1.416(3) . ? C21 C22 1.419(3) . ? C22 C23 1.422(3) . ? C22 C24 1.422(3) . ? C25 C27 1.423(3) . ? C26 C27 1.430(3) . ? C27 C28 1.417(3) . ? C28 C30 1.418(3) . ? C28 C29 1.423(3) . ? C29 C31 1.363(3) . ? C30 C32 1.361(3) . ? C31 C33 1.420(3) . ? C32 C33 1.416(3) . ? C33 C34 1.416(3) . ? C34 C35 1.425(3) . ? C34 C36 1.426(3) . ? O3S H3SB 0.85(4) . ? O3S H3SA 0.81(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Er1 O1 98.37(6) . . ? O2 Er1 O4 89.12(6) . . ? O1 Er1 O4 148.54(6) . . ? O2 Er1 O6 143.85(5) . . ? O1 Er1 O6 80.91(6) . . ? O4 Er1 O6 110.36(6) . . ? O2 Er1 O5 142.13(6) . . ? O1 Er1 O5 78.05(6) . . ? O4 Er1 O5 77.45(5) . . ? O6 Er1 O5 73.48(6) . . ? O2 Er1 O3 70.87(6) . . ? O1 Er1 O3 76.79(6) . . ? O4 Er1 O3 76.97(6) . . ? O6 Er1 O3 141.66(5) . . ? O5 Er1 O3 71.64(6) . . ? O2 Er1 N5 72.14(6) . . ? O1 Er1 N5 71.97(6) . . ? O4 Er1 N5 138.86(6) . . ? O6 Er1 N5 73.38(5) . . ? O5 Er1 N5 138.06(5) . . ? O3 Er1 N5 126.55(6) . . ? O2 Er1 N1 83.70(6) . . ? O1 Er1 N1 141.49(5) . . ? O4 Er1 N1 69.50(6) . . ? O6 Er1 N1 75.76(6) . . ? O5 Er1 N1 122.46(6) . . ? O3 Er1 N1 137.93(6) . . ? N5 Er1 N1 72.22(6) . . ? Er1 O1 H1A 121(2) . . ? Er1 O1 H1B 118(2) . . ? H1A O1 H1B 115(3) . . ? Er1 O2 H2A 125(2) . . ? Er1 O2 H2B 125(2) . . ? H2A O2 H2B 110(3) . . ? Er1 O3 H3A 123(2) . . ? Er1 O3 H3B 133(4) . . ? H3A O3 H3B 103(4) . . ? Er1 O4 H4A 119(2) . . ? Er1 O4 H4B 119(2) . . ? H4A O4 H4B 105(3) . . ? Er1 O5 H5A 122(2) . . ? Er1 O5 H5B 125(2) . . ? H5A O5 H5B 112(3) . . ? Er1 O6 H6A 121(2) . . ? Er1 O6 H6B 127(2) . . ? H6A O6 H6B 111(3) . . ? C1 N1 Er1 174.64(15) . . ? C13 N5 Er1 171.30(15) . . ? N1 C1 C3 179.3(2) . . ? N2 C2 C3 176.4(2) . . ? C1 C3 C4 120.87(17) . . ? C1 C3 C2 115.28(16) . . ? C4 C3 C2 123.67(17) . . ? C5 C4 C6 112.98(16) . . ? C5 C4 C3 122.55(17) . . ? C6 C4 C3 124.46(17) . . ? F1 C5 C7 117.45(17) . . ? F1 C5 C4 118.97(16) . . ? C7 C5 C4 123.50(17) . . ? F2 C6 C8 117.93(17) . . ? F2 C6 C4 118.63(17) . . ? C8 C6 C4 123.44(17) . . ? F3 C7 C5 117.69(16) . . ? F3 C7 C9 118.43(17) . . ? C5 C7 C9 123.85(17) . . ? F4 C8 C6 118.12(17) . . ? F4 C8 C9 118.58(17) . . ? C6 C8 C9 123.29(17) . . ? C7 C9 C10 122.50(17) . . ? C7 C9 C8 112.91(17) . . ? C10 C9 C8 124.58(17) . . ? C9 C10 C12 123.85(18) . . ? C9 C10 C11 122.74(17) . . ? C12 C10 C11 112.91(17) . . ? N3 C11 C10 176.8(2) . . ? N4 C12 C10 175.1(2) . . ? N5 C13 C15 174.9(2) . . ? N6 C14 C15 175.5(2) . . ? C14 C15 C13 113.04(16) . . ? C14 C15 C16 123.84(17) . . ? C13 C15 C16 123.10(17) . . ? C17 C16 C18 113.33(16) . . ? C17 C16 C15 122.88(17) . . ? C18 C16 C15 123.78(17) . . ? F5 C17 C19 118.00(16) . . ? F5 C17 C16 118.33(16) . . ? C19 C17 C16 123.65(17) . . ? F6 C18 C20 118.24(16) . . ? F6 C18 C16 118.72(16) . . ? C20 C18 C16 123.02(17) . . ? F7 C19 C17 117.94(16) . . ? F7 C19 C21 119.08(16) . . ? C17 C19 C21 122.97(17) . . ? F8 C20 C18 117.64(16) . . ? F8 C20 C21 118.77(16) . . ? C18 C20 C21 123.58(17) . . ? C20 C21 C19 113.34(16) . . ? C20 C21 C22 123.32(17) . . ? C19 C21 C22 123.33(17) . . ? C21 C22 C23 123.68(17) . . ? C21 C22 C24 122.68(17) . . ? C23 C22 C24 113.63(17) . . ? N7 C23 C22 177.4(2) . . ? N8 C24 C22 177.0(2) . . ? N9 C25 C27 178.5(2) . . ? N10 C26 C27 177.3(2) . . ? C28 C27 C25 121.92(18) . . ? C28 C27 C26 122.92(18) . . ? C25 C27 C26 114.88(18) . . ? C27 C28 C30 122.77(18) . . ? C27 C28 C29 124.15(18) . . ? C30 C28 C29 113.07(17) . . ? F9 C29 C31 117.62(17) . . ? F9 C29 C28 119.04(16) . . ? C31 C29 C28 123.32(17) . . ? F10 C30 C32 117.65(17) . . ? F10 C30 C28 118.67(17) . . ? C32 C30 C28 123.63(18) . . ? F11 C31 C29 118.00(16) . . ? F11 C31 C33 118.65(17) . . ? C29 C31 C33 123.29(17) . . ? F12 C32 C30 117.96(17) . . ? F12 C32 C33 118.65(16) . . ? C30 C32 C33 123.33(17) . . ? C34 C33 C32 123.03(17) . . ? C34 C33 C31 123.61(17) . . ? C32 C33 C31 113.36(17) . . ? C33 C34 C35 123.36(17) . . ? C33 C34 C36 121.92(17) . . ? C35 C34 C36 114.49(17) . . ? N11 C35 C34 176.7(2) . . ? N12 C36 C34 177.7(2) . . ? H3SB O3S H3SA 101(3) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.859 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.076 # Attachment 'EuTCNQF4.CIF' data_g:\nazari~1\nazari~1\crysta~1\nl085e~1\platon _database_code_depnum_ccdc_archive 'CCDC 749362' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Europium(III) 2,3,5,6-Tetrafluoro-7,7,8,8-Tetracyanoquinodimethane' ; _chemical_name_common "Europium(iii) 2,3,5,6-Tetrafluoro-7,7,8,8- Tetracyanoquinodimethane'" _chemical_melting_point ? _chemical_formula_sum 'C36 H20 Eu F12 N12 O10' _chemical_formula_weight 1160.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.5511(11) _cell_length_b 17.3987(13) _cell_length_c 21.5192(15) _cell_angle_alpha 90.00 _cell_angle_beta 122.257(4) _cell_angle_gamma 90.00 _cell_volume 4290.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2284 _exptl_absorpt_coefficient_mu 11.592 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2694 _exptl_absorpt_correction_T_max 0.5949 _exptl_absorpt_process_details 'SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25708 _diffrn_reflns_av_R_equivalents 0.1013 _diffrn_reflns_av_sigmaI/netI 0.1265 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 62.94 _reflns_number_total 6109 _reflns_number_gt 3553 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1174P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6109 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1256 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.2015 _refine_ls_wR_factor_gt 0.1793 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.34835(7) -0.52339(3) -0.41042(4) 0.0292(3) Uani 1 1 d . . . F1 F 0.0980(6) -0.4022(3) -0.3443(4) 0.0413(18) Uani 1 1 d . . . F2 F 0.3056(6) -0.2347(3) -0.1385(4) 0.0367(17) Uani 1 1 d . . . F3 F -0.0842(6) -0.3954(4) -0.3327(4) 0.0467(19) Uani 1 1 d . . . F4 F 0.1194(6) -0.2251(3) -0.1294(4) 0.0451(19) Uani 1 1 d . . . F5 F 0.5593(6) -0.4626(3) -0.1557(4) 0.0365(17) Uani 1 1 d . . . F6 F 0.6127(6) -0.6783(3) -0.0067(3) 0.0338(17) Uani 1 1 d . . . F7 F 0.6236(6) -0.3712(3) -0.0438(3) 0.0347(17) Uani 1 1 d . . . F8 F 0.6684(6) -0.5859(3) 0.1038(3) 0.0307(16) Uani 1 1 d . . . F9 F 0.8206(6) -0.4724(3) -0.1397(4) 0.0367(16) Uani 1 1 d . . . F10 F 0.8733(5) -0.6496(3) 0.0429(4) 0.0346(17) Uani 1 1 d . . . F11 F 0.8717(6) -0.3586(3) -0.0476(3) 0.0343(17) Uani 1 1 d . . . F12 F 0.9223(5) -0.5360(3) 0.1344(4) 0.0317(16) Uani 1 1 d . . . O1 O 0.2271(8) -0.5689(5) -0.3623(5) 0.049(2) Uani 1 1 d . . . O2 O 0.3085(7) -0.6599(4) -0.4357(5) 0.039(2) Uani 1 1 d . . . O3 O 0.1437(8) -0.5277(5) -0.5060(5) 0.061(3) Uani 1 1 d . . . O4 O 0.3507(8) -0.5289(4) -0.5216(5) 0.047(2) Uani 1 1 d . . . O5 O 0.2874(8) -0.3949(4) -0.4785(5) 0.048(2) Uani 1 1 d . . . O6 O 0.5066(7) -0.4327(4) -0.3548(5) 0.044(2) Uani 1 1 d . . . O7 O 0.5296(7) -0.5833(4) -0.3885(4) 0.034(2) Uani 1 1 d . . . N1 N 0.3234(8) -0.4244(5) -0.3325(5) 0.030(2) Uani 1 1 d . . . N2 N 0.5057(10) -0.2525(5) -0.1661(6) 0.041(3) Uani 1 1 d . . . N3 N -0.2628(12) -0.4022(7) -0.2931(8) 0.068(4) Uani 1 1 d . . . N4 N -0.1218(13) -0.2115(6) -0.1447(8) 0.074(5) Uani 1 1 d . . . N5 N 0.4745(9) -0.5759(5) -0.2784(6) 0.036(3) Uani 1 1 d . . . N6 N 0.5325(9) -0.7719(5) -0.1486(5) 0.034(3) Uani 1 1 d . . . N7 N 0.6583(9) -0.2767(5) 0.0863(6) 0.040(3) Uani 1 1 d . . . N8 N 0.7563(10) -0.4669(6) 0.2286(6) 0.043(3) Uani 1 1 d . . . N9 N 0.7396(9) -0.6152(5) -0.2425(6) 0.040(3) Uani 1 1 d . . . N10 N 0.8193(9) -0.7705(5) -0.0704(6) 0.047(3) Uani 1 1 d . . . N11 N 0.8891(9) -0.2362(5) 0.0595(6) 0.043(3) Uani 1 1 d . . . N12 N 0.9982(10) -0.3929(6) 0.2356(7) 0.046(3) Uani 1 1 d . . . C1 C 0.3197(10) -0.3807(6) -0.2930(7) 0.029(3) Uani 1 1 d . . . C2 C 0.4172(11) -0.2854(6) -0.2000(7) 0.029(3) Uani 1 1 d . . . C3 C 0.3135(10) -0.3285(6) -0.2454(6) 0.026(3) Uani 1 1 d . . . C4 C 0.2117(11) -0.3196(6) -0.2420(6) 0.029(3) Uani 1 1 d . . . C5 C 0.1059(11) -0.3580(6) -0.2891(7) 0.031(3) Uani 1 1 d . . . C6 C 0.2059(11) -0.2735(6) -0.1885(7) 0.031(3) Uani 1 1 d . . . C7 C 0.0125(11) -0.3552(6) -0.2841(7) 0.032(3) Uani 1 1 d . . . C8 C 0.1110(12) -0.2698(6) -0.1850(7) 0.033(3) Uani 1 1 d . . . C9 C 0.0080(11) -0.3084(6) -0.2304(7) 0.031(3) Uani 1 1 d . . . C10 C -0.0914(12) -0.3071(7) -0.2250(8) 0.047(4) Uani 1 1 d . . . C11 C -0.1857(14) -0.3594(8) -0.2627(9) 0.054(4) Uani 1 1 d . . . C12 C -0.1042(13) -0.2527(7) -0.1789(9) 0.057(4) Uani 1 1 d . . . C13 C 0.5072(11) -0.5955(6) -0.2202(8) 0.027(3) Uani 1 1 d . . . C14 C 0.5418(10) -0.7064(6) -0.1461(6) 0.024(3) Uani 1 1 d . . . C15 C 0.5472(10) -0.6251(5) -0.1494(7) 0.026(3) Uani 1 1 d . . . C16 C 0.5809(10) -0.5750(6) -0.0876(7) 0.029(3) Uani 1 1 d . . . C17 C 0.5858(11) -0.4939(6) -0.0916(6) 0.027(3) Uani 1 1 d . . . C18 C 0.6142(10) -0.6016(6) -0.0170(7) 0.027(3) Uani 1 1 d . . . C19 C 0.6181(10) -0.4475(6) -0.0335(6) 0.025(3) Uani 1 1 d . . . C20 C 0.6415(11) -0.5549(6) 0.0398(7) 0.028(3) Uani 1 1 d . . . C21 C 0.6484(9) -0.4742(6) 0.0365(6) 0.025(3) Uani 1 1 d . . . C22 C 0.6808(10) -0.4239(6) 0.0955(7) 0.028(3) Uani 1 1 d . . . C23 C 0.6704(10) -0.3417(6) 0.0886(7) 0.028(3) Uani 1 1 d . . . C24 C 0.7228(11) -0.4509(6) 0.1699(8) 0.031(3) Uani 1 1 d . . . C25 C 0.7718(10) -0.6182(6) -0.1811(8) 0.031(3) Uani 1 1 d . . . C26 C 0.8161(11) -0.7075(6) -0.0838(7) 0.034(3) Uani 1 1 d . . . C27 C 0.8097(10) -0.6278(6) -0.1055(7) 0.026(3) Uani 1 1 d . . . C28 C 0.8406(9) -0.5678(5) -0.0545(7) 0.024(3) Uani 1 1 d . . . C29 C 0.8437(10) -0.4897(6) -0.0725(7) 0.029(3) Uani 1 1 d . . . C30 C 0.8725(10) -0.5777(6) 0.0185(7) 0.031(3) Uani 1 1 d . . . C31 C 0.8700(10) -0.4298(5) -0.0240(7) 0.027(3) Uani 1 1 d . . . C32 C 0.8969(9) -0.5190(6) 0.0666(6) 0.021(3) Uani 1 1 d . . . C33 C 0.8981(10) -0.4397(5) 0.0487(6) 0.022(3) Uani 1 1 d . . . C34 C 0.9188(10) -0.3794(6) 0.0976(7) 0.029(3) Uani 1 1 d . . . C35 C 0.9008(10) -0.3015(6) 0.0752(6) 0.029(3) Uani 1 1 d . . . C36 C 0.9627(11) -0.3907(6) 0.1742(8) 0.030(3) Uani 1 1 d . . . O1S O 0.1965(13) -0.4339(9) -0.6270(9) 0.139(5) Uiso 1 1 d . . . O2S O 0.4892(7) -0.6437(4) -0.5174(4) 0.040(2) Uiso 1 1 d . . . O3S O 1.0094(10) -0.1147(6) -0.0125(6) 0.093(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0459(5) 0.0145(3) 0.0301(5) 0.0005(4) 0.0224(4) 0.0003(4) F1 0.040(4) 0.038(4) 0.050(5) -0.007(3) 0.027(4) 0.004(3) F2 0.048(5) 0.027(3) 0.036(4) -0.005(3) 0.023(4) 0.002(3) F3 0.036(4) 0.049(4) 0.069(6) 0.002(4) 0.036(4) -0.003(4) F4 0.075(5) 0.028(3) 0.052(5) 0.004(3) 0.047(4) 0.010(4) F5 0.060(5) 0.021(3) 0.031(5) 0.009(3) 0.026(4) 0.002(3) F6 0.050(5) 0.018(3) 0.039(5) 0.005(3) 0.028(4) 0.001(3) F7 0.050(4) 0.014(3) 0.036(4) 0.003(3) 0.020(4) 0.002(3) F8 0.048(4) 0.025(3) 0.021(4) 0.002(3) 0.020(4) 0.001(3) F9 0.046(4) 0.034(3) 0.032(4) 0.004(3) 0.022(4) 0.000(3) F10 0.045(4) 0.010(3) 0.051(5) 0.005(3) 0.027(4) 0.001(3) F11 0.048(4) 0.018(3) 0.042(5) 0.003(3) 0.028(4) -0.008(3) F12 0.038(4) 0.024(3) 0.033(5) 0.006(3) 0.019(4) 0.005(3) O1 0.073(7) 0.044(5) 0.047(6) -0.013(4) 0.042(6) -0.026(5) O2 0.050(6) 0.010(3) 0.062(6) -0.009(4) 0.032(5) -0.011(4) O3 0.045(6) 0.088(7) 0.047(6) 0.013(6) 0.022(5) 0.001(6) O4 0.076(7) 0.045(5) 0.037(6) 0.012(4) 0.041(5) 0.005(5) O5 0.057(6) 0.026(4) 0.047(6) 0.008(4) 0.018(5) 0.008(4) O6 0.048(6) 0.033(4) 0.064(7) -0.016(4) 0.038(5) -0.014(4) O7 0.056(6) 0.020(4) 0.041(6) -0.003(4) 0.035(5) -0.003(4) N1 0.044(7) 0.016(4) 0.048(7) -0.007(5) 0.038(6) 0.004(4) N2 0.049(7) 0.021(5) 0.050(8) -0.002(5) 0.025(7) 0.007(5) N3 0.063(9) 0.059(8) 0.095(12) 0.021(8) 0.052(9) 0.002(7) N4 0.122(13) 0.044(7) 0.115(13) 0.012(7) 0.103(11) 0.036(8) N5 0.059(8) 0.021(5) 0.044(8) 0.002(5) 0.037(7) -0.003(5) N6 0.041(7) 0.025(5) 0.042(7) -0.001(5) 0.025(6) -0.001(5) N7 0.046(7) 0.032(6) 0.049(8) -0.002(5) 0.030(6) 0.008(5) N8 0.062(8) 0.043(6) 0.031(8) -0.002(6) 0.031(7) 0.004(6) N9 0.046(7) 0.034(6) 0.043(8) -0.015(6) 0.026(7) -0.007(5) N10 0.044(7) 0.024(6) 0.053(8) 0.000(5) 0.012(6) 0.002(5) N11 0.053(7) 0.025(6) 0.047(8) 0.000(5) 0.024(6) -0.003(5) N12 0.052(8) 0.037(6) 0.044(9) 0.001(6) 0.023(7) 0.005(6) C1 0.028(7) 0.021(6) 0.043(9) 0.008(6) 0.022(7) -0.003(5) C2 0.034(8) 0.020(6) 0.038(9) -0.004(6) 0.023(7) 0.006(6) C3 0.039(8) 0.020(5) 0.028(8) -0.006(5) 0.024(7) 0.004(6) C4 0.039(8) 0.021(5) 0.032(8) 0.000(5) 0.022(7) 0.003(6) C5 0.037(8) 0.022(6) 0.042(9) 0.001(6) 0.027(7) 0.008(6) C6 0.043(8) 0.022(6) 0.038(9) 0.009(6) 0.028(7) 0.006(6) C7 0.026(7) 0.029(6) 0.042(9) 0.006(6) 0.019(7) 0.009(6) C8 0.055(9) 0.017(5) 0.040(9) -0.005(6) 0.034(8) 0.005(6) C9 0.046(8) 0.021(5) 0.041(9) 0.009(6) 0.033(7) 0.008(6) C10 0.056(10) 0.034(7) 0.074(12) 0.019(7) 0.050(9) 0.024(7) C11 0.064(11) 0.047(8) 0.077(13) 0.013(8) 0.055(10) 0.015(9) C12 0.073(11) 0.044(8) 0.074(12) 0.047(8) 0.052(10) 0.031(8) C13 0.039(8) 0.016(5) 0.041(10) -0.002(6) 0.031(7) 0.002(5) C14 0.027(7) 0.029(6) 0.019(8) -0.003(5) 0.015(6) -0.002(6) C15 0.035(7) 0.012(5) 0.047(9) 0.005(5) 0.033(7) 0.008(5) C16 0.037(8) 0.029(6) 0.033(9) 0.000(6) 0.025(7) 0.004(6) C17 0.044(8) 0.025(5) 0.017(8) 0.003(5) 0.019(7) 0.010(5) C18 0.029(7) 0.018(5) 0.031(9) 0.015(5) 0.012(6) 0.005(5) C19 0.033(7) 0.021(5) 0.022(8) 0.005(5) 0.016(6) -0.001(5) C20 0.043(8) 0.018(5) 0.036(9) 0.000(6) 0.029(7) -0.003(6) C21 0.017(6) 0.027(6) 0.032(8) -0.008(6) 0.015(6) -0.007(5) C22 0.031(7) 0.021(5) 0.042(9) 0.010(6) 0.026(7) 0.009(5) C23 0.034(8) 0.017(6) 0.039(8) -0.005(5) 0.024(7) 0.000(5) C24 0.043(8) 0.020(6) 0.039(10) -0.008(6) 0.027(8) -0.001(6) C25 0.032(8) 0.015(5) 0.048(11) -0.014(6) 0.024(8) 0.000(5) C26 0.040(8) 0.022(6) 0.040(9) -0.011(6) 0.021(7) -0.011(6) C27 0.027(7) 0.020(5) 0.045(9) -0.016(6) 0.028(7) -0.010(5) C28 0.020(7) 0.020(5) 0.034(8) 0.005(5) 0.015(6) 0.002(5) C29 0.029(7) 0.032(6) 0.037(9) 0.005(6) 0.024(7) 0.002(6) C30 0.039(8) 0.027(6) 0.035(9) 0.004(6) 0.025(7) 0.004(6) C31 0.031(7) 0.010(5) 0.050(9) 0.004(5) 0.029(7) 0.002(5) C32 0.019(6) 0.020(5) 0.026(8) 0.006(6) 0.013(6) -0.003(5) C33 0.030(7) 0.011(5) 0.027(8) -0.001(5) 0.016(6) 0.001(5) C34 0.021(7) 0.026(6) 0.036(9) -0.002(6) 0.013(7) 0.002(5) C35 0.031(7) 0.029(6) 0.030(8) -0.014(6) 0.018(7) -0.006(6) C36 0.030(8) 0.023(6) 0.030(10) -0.001(6) 0.011(7) 0.005(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O6 2.404(8) . ? Eu1 O4 2.411(8) . ? Eu1 O3 2.417(9) . ? Eu1 O2 2.431(7) . ? Eu1 O7 2.471(8) . ? Eu1 O1 2.493(8) . ? Eu1 N1 2.549(8) . ? Eu1 O5 2.556(7) . ? Eu1 N5 2.578(11) . ? F1 C5 1.371(12) . ? F2 C6 1.373(13) . ? F3 C7 1.356(13) . ? F4 C8 1.380(12) . ? F5 C17 1.342(12) . ? F6 C18 1.355(11) . ? F7 C19 1.353(11) . ? F8 C20 1.337(12) . ? F9 C29 1.341(13) . ? F10 C30 1.354(12) . ? F11 C31 1.342(11) . ? F12 C32 1.340(12) . ? N1 C1 1.162(13) . ? N2 C2 1.168(14) . ? N3 C11 1.159(18) . ? N4 C12 1.140(17) . ? N5 C13 1.135(14) . ? N6 C14 1.146(12) . ? N7 C23 1.139(12) . ? N8 C24 1.126(14) . ? N9 C25 1.152(15) . ? N10 C26 1.129(13) . ? N11 C35 1.173(13) . ? N12 C36 1.140(15) . ? C1 C3 1.404(15) . ? C2 C3 1.423(16) . ? C3 C4 1.428(15) . ? C4 C5 1.406(16) . ? C4 C6 1.440(15) . ? C5 C7 1.327(16) . ? C6 C8 1.330(16) . ? C7 C9 1.441(15) . ? C8 C9 1.376(16) . ? C9 C10 1.413(16) . ? C10 C11 1.42(2) . ? C10 C12 1.447(19) . ? C13 C15 1.413(17) . ? C14 C15 1.419(13) . ? C15 C16 1.446(15) . ? C16 C18 1.412(15) . ? C16 C17 1.416(14) . ? C17 C19 1.351(15) . ? C18 C20 1.346(15) . ? C19 C21 1.411(15) . ? C20 C21 1.411(14) . ? C21 C22 1.406(15) . ? C22 C23 1.438(13) . ? C22 C24 1.461(18) . ? C25 C27 1.430(18) . ? C26 C27 1.451(15) . ? C27 C28 1.408(14) . ? C28 C30 1.398(15) . ? C28 C29 1.420(14) . ? C29 C31 1.380(15) . ? C30 C32 1.364(15) . ? C31 C33 1.411(15) . ? C32 C33 1.434(13) . ? C33 C34 1.404(14) . ? C34 C35 1.416(15) . ? C34 C36 1.437(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Eu1 O4 92.2(3) . . ? O6 Eu1 O3 139.3(3) . . ? O4 Eu1 O3 76.8(3) . . ? O6 Eu1 O2 141.7(3) . . ? O4 Eu1 O2 81.8(3) . . ? O3 Eu1 O2 76.2(3) . . ? O6 Eu1 O7 69.5(2) . . ? O4 Eu1 O7 68.5(3) . . ? O3 Eu1 O7 136.2(3) . . ? O2 Eu1 O7 73.1(2) . . ? O6 Eu1 O1 127.8(3) . . ? O4 Eu1 O1 139.5(3) . . ? O3 Eu1 O1 68.4(3) . . ? O2 Eu1 O1 70.5(3) . . ? O7 Eu1 O1 126.5(3) . . ? O6 Eu1 N1 68.0(3) . . ? O4 Eu1 N1 139.1(3) . . ? O3 Eu1 N1 94.9(3) . . ? O2 Eu1 N1 135.7(3) . . ? O7 Eu1 N1 128.8(3) . . ? O1 Eu1 N1 66.0(3) . . ? O6 Eu1 O5 68.9(3) . . ? O4 Eu1 O5 68.7(3) . . ? O3 Eu1 O5 70.5(3) . . ? O2 Eu1 O5 139.5(3) . . ? O7 Eu1 O5 117.5(3) . . ? O1 Eu1 O5 115.7(3) . . ? N1 Eu1 O5 70.7(3) . . ? O6 Eu1 N5 78.1(3) . . ? O4 Eu1 N5 136.7(3) . . ? O3 Eu1 N5 135.4(3) . . ? O2 Eu1 N5 80.7(3) . . ? O7 Eu1 N5 68.5(3) . . ? O1 Eu1 N5 68.0(3) . . ? N1 Eu1 N5 75.9(3) . . ? O5 Eu1 N5 139.7(3) . . ? C1 N1 Eu1 175.3(10) . . ? C13 N5 Eu1 164.0(10) . . ? N1 C1 C3 179.1(12) . . ? N2 C2 C3 174.5(12) . . ? C1 C3 C2 114.9(10) . . ? C1 C3 C4 122.8(11) . . ? C2 C3 C4 122.3(9) . . ? C5 C4 C3 123.5(10) . . ? C5 C4 C6 111.8(11) . . ? C3 C4 C6 124.6(11) . . ? C7 C5 F1 117.0(11) . . ? C7 C5 C4 125.0(11) . . ? F1 C5 C4 118.0(10) . . ? C8 C6 F2 120.6(11) . . ? C8 C6 C4 122.6(12) . . ? F2 C6 C4 116.7(10) . . ? C5 C7 F3 119.4(11) . . ? C5 C7 C9 122.4(12) . . ? F3 C7 C9 118.2(10) . . ? C6 C8 C9 125.5(11) . . ? C6 C8 F4 116.2(11) . . ? C9 C8 F4 118.3(11) . . ? C8 C9 C10 125.6(12) . . ? C8 C9 C7 112.6(11) . . ? C10 C9 C7 121.7(12) . . ? C9 C10 C11 123.3(12) . . ? C9 C10 C12 122.4(13) . . ? C11 C10 C12 114.2(12) . . ? N3 C11 C10 179.5(17) . . ? N4 C12 C10 175.5(18) . . ? N5 C13 C15 176.0(11) . . ? N6 C14 C15 175.3(14) . . ? C13 C15 C14 114.7(10) . . ? C13 C15 C16 121.4(9) . . ? C14 C15 C16 123.7(10) . . ? C18 C16 C17 113.2(10) . . ? C18 C16 C15 123.6(10) . . ? C17 C16 C15 123.2(10) . . ? F5 C17 C19 119.1(9) . . ? F5 C17 C16 118.1(9) . . ? C19 C17 C16 122.8(10) . . ? C20 C18 F6 117.8(10) . . ? C20 C18 C16 123.6(10) . . ? F6 C18 C16 118.4(10) . . ? C17 C19 F7 117.0(10) . . ? C17 C19 C21 123.8(10) . . ? F7 C19 C21 119.1(10) . . ? F8 C20 C18 118.9(9) . . ? F8 C20 C21 117.7(10) . . ? C18 C20 C21 123.3(11) . . ? C22 C21 C20 124.8(10) . . ? C22 C21 C19 122.1(10) . . ? C20 C21 C19 113.1(10) . . ? C21 C22 C23 124.1(11) . . ? C21 C22 C24 122.8(9) . . ? C23 C22 C24 113.1(10) . . ? N7 C23 C22 174.6(12) . . ? N8 C24 C22 175.6(12) . . ? N9 C25 C27 175.7(11) . . ? N10 C26 C27 176.6(14) . . ? C28 C27 C25 125.2(10) . . ? C28 C27 C26 121.1(11) . . ? C25 C27 C26 113.7(9) . . ? C30 C28 C27 124.7(10) . . ? C30 C28 C29 112.9(10) . . ? C27 C28 C29 122.4(11) . . ? F9 C29 C31 117.6(9) . . ? F9 C29 C28 119.1(10) . . ? C31 C29 C28 123.3(11) . . ? F10 C30 C32 116.7(10) . . ? F10 C30 C28 118.9(10) . . ? C32 C30 C28 124.3(10) . . ? F11 C31 C29 117.5(10) . . ? F11 C31 C33 118.9(9) . . ? C29 C31 C33 123.7(9) . . ? F12 C32 C30 118.5(9) . . ? F12 C32 C33 118.1(9) . . ? C30 C32 C33 123.3(10) . . ? C34 C33 C31 124.6(9) . . ? C34 C33 C32 122.9(10) . . ? C31 C33 C32 112.4(9) . . ? C33 C34 C35 122.1(11) . . ? C33 C34 C36 123.6(10) . . ? C35 C34 C36 114.3(10) . . ? N11 C35 C34 177.3(14) . . ? N12 C36 C34 174.1(12) . . ? _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 62.94 _diffrn_measured_fraction_theta_full 0.882 _refine_diff_density_max 2.602 _refine_diff_density_min -1.414 _refine_diff_density_rms 0.142 # Attachment 'GdTCNQF4-final.cif' data_c:\docume~1\hanhua\nl032 _database_code_depnum_ccdc_archive 'CCDC 749363' #TrackingRef 'GdTCNQF4-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Gadolinium(III) 2,3,5,6-Tetrafluoro-7,7,8,8-Tetracyanoquinodimethane ; _chemical_name_common ;Gadolinium(iii) 2,3,5,6-Tetrafluoro-7,7,8,8- Tetracyanoquinodimethane ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H18 F12 Gd N12 O9' _chemical_formula_weight 1147.87 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.701(3) _cell_length_b 17.671(4) _cell_length_c 17.104(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.18(3) _cell_angle_gamma 90.00 _cell_volume 4032.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 1.773 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS v2.03 (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 1000 CCD area-detector' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25969 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.34 _reflns_number_total 9739 _reflns_number_gt 8443 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2000)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2000)' _computing_data_reduction 'SAINT V6.32 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0171P)^2^+2.2813P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9739 _refine_ls_number_parameters 703 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0543 _refine_ls_wR_factor_gt 0.0517 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 Gd1 Gd 0.301411(7) 0.590635(5) 0.064426(6) 0.01317(3) Uani 1 1 d . . . F8 F -0.14942(9) 0.89869(7) -0.32815(8) 0.0226(3) Uani 1 1 d . . . F5 F -0.02518(9) 0.69062(7) -0.09530(8) 0.0251(3) Uani 1 1 d . . . F7 F 0.04280(9) 0.87647(7) -0.27475(7) 0.0208(3) Uani 1 1 d . . . F3 F 0.43598(10) 1.00941(7) 0.21087(7) 0.0241(3) Uani 1 1 d . . . F6 F -0.21793(9) 0.71001(7) -0.15098(8) 0.0255(3) Uani 1 1 d . . . F2 F 0.30795(10) 0.94593(7) -0.10521(7) 0.0265(3) Uani 1 1 d . . . F4 F 0.45317(10) 1.11327(7) 0.10504(8) 0.0281(3) Uani 1 1 d . . . O6 O 0.14178(12) 0.60233(10) 0.09019(11) 0.0255(4) Uani 1 1 d . . . F1 F 0.29567(10) 0.84133(7) -0.00073(7) 0.0246(3) Uani 1 1 d . . . N1 N 0.32894(14) 0.72279(10) 0.12312(11) 0.0211(4) Uani 1 1 d . . . O2 O 0.36995(14) 0.58487(11) 0.20446(10) 0.0268(4) Uani 1 1 d . . . O3 O 0.43576(13) 0.50260(10) 0.07266(11) 0.0243(4) Uani 1 1 d . . . O5 O 0.25386(13) 0.52681(10) -0.05939(10) 0.0235(3) Uani 1 1 d . . . N7 N -0.37352(15) 0.91460(12) -0.38147(14) 0.0321(5) Uani 1 1 d . . . O1 O 0.41500(12) 0.64676(9) -0.00544(11) 0.0214(3) Uani 1 1 d . . . O4 O 0.24783(13) 0.46998(10) 0.10190(13) 0.0299(4) Uani 1 1 d D . . N5 N 0.20134(13) 0.68082(10) -0.03699(11) 0.0199(4) Uani 1 1 d . . . C5 C 0.33737(15) 0.90775(11) 0.02754(13) 0.0174(4) Uani 1 1 d . . . C3 C 0.36003(15) 0.86085(11) 0.16793(12) 0.0167(4) Uani 1 1 d . . . C22 C -0.29924(16) 0.81490(12) -0.27533(13) 0.0199(4) Uani 1 1 d . . . C8 C 0.41313(15) 1.04645(11) 0.07793(13) 0.0190(4) Uani 1 1 d . . . C9 C 0.38259(15) 1.03533(11) -0.00635(13) 0.0177(4) Uani 1 1 d . . . C11 C 0.36772(17) 1.07532(12) -0.14873(15) 0.0230(5) Uani 1 1 d . . . C15 C 0.12357(15) 0.76605(11) -0.15601(12) 0.0165(4) Uani 1 1 d . . . C10 C 0.38717(16) 1.09101(11) -0.06499(13) 0.0195(4) Uani 1 1 d . . . C14 C 0.19870(16) 0.79744(12) -0.19123(13) 0.0191(4) Uani 1 1 d . . . N6 N 0.26383(14) 0.81921(11) -0.21694(12) 0.0266(4) Uani 1 1 d . . . C20 C -0.12035(16) 0.84467(11) -0.27232(12) 0.0173(4) Uani 1 1 d . . . C18 C -0.15482(16) 0.75152(11) -0.18308(13) 0.0182(4) Uani 1 1 d . . . C17 C -0.05485(16) 0.74129(11) -0.15428(12) 0.0175(4) Uani 1 1 d . . . C24 C -0.33829(16) 0.87013(13) -0.33445(14) 0.0226(5) Uani 1 1 d . . . C6 C 0.34326(15) 0.96211(12) -0.02727(12) 0.0182(4) Uani 1 1 d . . . C13 C 0.16290(15) 0.71816(11) -0.08997(13) 0.0174(4) Uani 1 1 d . . . N2 N 0.38609(15) 0.88018(11) 0.32008(12) 0.0271(4) Uani 1 1 d . . . C21 C -0.19492(15) 0.80398(11) -0.24499(12) 0.0171(4) Uani 1 1 d . . . C7 C 0.40549(15) 0.99231(12) 0.13263(13) 0.0177(4) Uani 1 1 d . . . C4 C 0.36731(15) 0.91849(11) 0.11144(13) 0.0165(4) Uani 1 1 d . . . N3 N 0.35497(16) 1.06531(11) -0.21653(13) 0.0303(5) Uani 1 1 d . . . C19 C -0.02061(15) 0.83335(11) -0.24462(12) 0.0161(4) Uani 1 1 d . . . C16 C 0.01908(15) 0.77965(11) -0.18434(12) 0.0160(4) Uani 1 1 d . . . N4 N 0.45492(17) 1.22626(12) -0.03554(14) 0.0367(5) Uani 1 1 d . . . C1 C 0.34232(15) 0.78455(12) 0.14295(12) 0.0181(4) Uani 1 1 d . . . C2 C 0.37665(16) 0.87299(12) 0.25227(13) 0.0202(4) Uani 1 1 d . . . C12 C 0.42512(17) 1.16539(13) -0.04564(14) 0.0238(5) Uani 1 1 d . . . C23 C -0.37402(16) 0.77359(13) -0.24854(14) 0.0238(5) Uani 1 1 d . . . F10 F 0.05173(9) 0.63180(7) 0.47172(7) 0.0232(3) Uani 1 1 d . . . F12 F 0.20847(10) 0.46681(7) 0.68087(7) 0.0236(3) Uani 1 1 d . . . F11 F 0.22182(10) 0.36274(7) 0.57510(8) 0.0242(3) Uani 1 1 d . . . F9 F 0.06519(10) 0.52827(7) 0.36544(7) 0.0253(3) Uani 1 1 d . . . C36 C 0.13950(16) 0.59449(12) 0.72357(14) 0.0203(4) Uani 1 1 d . . . N12 N 0.10435(18) 0.40463(12) 0.25546(13) 0.0366(5) Uani 1 1 d . . . C31 C 0.17741(16) 0.42866(11) 0.54798(13) 0.0176(4) Uani 1 1 d . . . C27 C 0.15175(16) 0.38210(12) 0.40752(13) 0.0205(4) Uani 1 1 d . . . C28 C 0.14429(15) 0.43903(12) 0.46425(13) 0.0176(4) Uani 1 1 d . . . C32 C 0.17056(15) 0.48264(12) 0.60307(12) 0.0170(4) Uani 1 1 d . . . C33 C 0.12945(15) 0.55518(11) 0.58224(12) 0.0153(4) Uani 1 1 d . . . C30 C 0.09608(15) 0.56568(11) 0.49838(13) 0.0164(4) Uani 1 1 d . . . C26 C 0.17839(18) 0.30573(13) 0.42978(14) 0.0257(5) Uani 1 1 d . . . C34 C 0.12365(15) 0.61131(11) 0.64027(13) 0.0175(4) Uani 1 1 d . . . N11 N 0.19719(18) 0.24336(12) 0.44462(13) 0.0379(5) Uani 1 1 d . . . C29 C 0.10267(15) 0.51208(12) 0.44301(12) 0.0180(4) Uani 1 1 d . . . C25 C 0.12528(17) 0.39531(13) 0.32346(15) 0.0246(5) Uani 1 1 d . . . N9 N 0.06957(15) 0.74912(11) 0.60697(13) 0.0289(4) Uani 1 1 d . . . C35 C 0.09289(16) 0.68711(12) 0.61983(13) 0.0206(4) Uani 1 1 d . . . O1S O 0.01251(14) 0.48524(10) 0.10258(12) 0.0282(4) Uani 1 1 d . . . O2S O 0.10520(15) 0.40262(11) -0.00870(12) 0.0316(4) Uani 1 1 d . . . O3S O 0.39653(17) 0.14759(11) 0.58138(15) 0.0375(5) Uani 1 1 d . . . N10 N 0.15001(15) 0.58286(11) 0.79101(12) 0.0274(4) Uani 1 1 d . . . N8 N -0.43778(15) 0.74167(13) -0.22942(14) 0.0375(5) Uani 1 1 d . . . H2A H 0.347(2) 0.6123(17) 0.2309(18) 0.041(9) Uiso 1 1 d . . . H5B H 0.222(2) 0.5463(18) -0.1017(19) 0.043(9) Uiso 1 1 d . . . H1SA H 0.023(2) 0.452(2) 0.071(2) 0.060(11) Uiso 1 1 d . . . H2B H 0.381(3) 0.545(2) 0.225(2) 0.059(11) Uiso 1 1 d . . . H1B H 0.413(2) 0.6383(18) -0.053(2) 0.047(10) Uiso 1 1 d . . . H6A H 0.107(2) 0.5695(17) 0.0998(18) 0.039(9) Uiso 1 1 d . . . H4B H 0.209(2) 0.4447(19) 0.067(2) 0.050(10) Uiso 1 1 d . . . H1A H 0.450(2) 0.6814(18) 0.0089(19) 0.046(9) Uiso 1 1 d . . . H3B H 0.433(2) 0.453(2) 0.081(2) 0.060(10) Uiso 1 1 d . . . H5A H 0.289(3) 0.493(2) -0.073(2) 0.063(11) Uiso 1 1 d . . . H6B H 0.111(2) 0.6445(19) 0.0933(19) 0.055(10) Uiso 1 1 d . . . H1SB H 0.028(2) 0.4638(19) 0.147(2) 0.056(11) Uiso 1 1 d . . . H2SA H 0.119(3) 0.358(2) -0.024(2) 0.069(12) Uiso 1 1 d . . . H2SB H 0.091(3) 0.433(2) -0.047(2) 0.067(12) Uiso 1 1 d . . . H3A H 0.487(2) 0.5150(17) 0.0787(18) 0.037(9) Uiso 1 1 d . . . H3SA H 0.419(3) 0.173(2) 0.620(3) 0.079(14) Uiso 1 1 d . . . H4A H 0.273(3) 0.444(2) 0.142(2) 0.118(18) Uiso 1 1 d D . . H3SB H 0.364(3) 0.170(2) 0.546(2) 0.061(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01457(5) 0.01213(5) 0.01261(5) 0.00132(4) 0.00265(4) 0.00035(4) F8 0.0239(6) 0.0223(6) 0.0212(7) 0.0099(5) 0.0043(5) 0.0043(5) F5 0.0233(6) 0.0262(7) 0.0241(7) 0.0142(5) 0.0020(5) -0.0013(5) F7 0.0215(6) 0.0212(6) 0.0211(7) 0.0072(5) 0.0082(5) -0.0008(5) F3 0.0307(7) 0.0234(6) 0.0161(6) -0.0061(5) 0.0009(5) -0.0048(5) F6 0.0218(6) 0.0262(7) 0.0291(7) 0.0094(6) 0.0073(6) -0.0040(5) F2 0.0415(8) 0.0213(6) 0.0145(6) -0.0023(5) 0.0017(6) -0.0068(6) F4 0.0382(8) 0.0168(6) 0.0268(7) -0.0053(5) 0.0023(6) -0.0114(6) O6 0.0229(8) 0.0197(8) 0.0381(10) 0.0047(7) 0.0157(8) 0.0016(7) F1 0.0386(7) 0.0142(6) 0.0187(7) -0.0031(5) 0.0016(6) -0.0088(5) N1 0.0297(10) 0.0169(9) 0.0160(9) 0.0011(7) 0.0041(8) -0.0013(7) O2 0.0351(10) 0.0278(9) 0.0167(8) 0.0031(7) 0.0044(7) 0.0144(8) O3 0.0185(9) 0.0193(8) 0.0347(10) 0.0011(7) 0.0051(7) 0.0032(7) O5 0.0275(9) 0.0217(8) 0.0188(9) -0.0037(7) -0.0001(7) 0.0035(7) N7 0.0217(10) 0.0335(11) 0.0377(13) 0.0125(10) -0.0005(9) -0.0010(9) O1 0.0224(8) 0.0215(8) 0.0219(9) -0.0010(7) 0.0081(7) -0.0059(7) O4 0.0243(9) 0.0208(8) 0.0422(12) 0.0120(8) 0.0025(8) -0.0019(7) N5 0.0191(9) 0.0215(9) 0.0184(9) 0.0027(7) 0.0027(7) 0.0021(7) C5 0.0175(10) 0.0134(9) 0.0203(11) -0.0037(8) 0.0024(8) -0.0024(8) C3 0.0181(10) 0.0168(10) 0.0141(10) -0.0015(8) 0.0012(8) 0.0017(8) C22 0.0222(11) 0.0173(10) 0.0196(11) 0.0004(8) 0.0034(9) -0.0004(8) C8 0.0184(10) 0.0150(9) 0.0231(11) -0.0062(8) 0.0037(9) -0.0027(8) C9 0.0143(9) 0.0167(10) 0.0225(11) -0.0006(8) 0.0050(8) 0.0003(8) C11 0.0240(11) 0.0174(10) 0.0291(13) 0.0016(9) 0.0089(10) -0.0019(8) C15 0.0199(10) 0.0164(10) 0.0131(10) 0.0011(8) 0.0036(8) 0.0013(8) C10 0.0210(10) 0.0159(10) 0.0219(11) -0.0006(8) 0.0057(9) -0.0017(8) C14 0.0223(11) 0.0199(10) 0.0139(10) -0.0001(8) 0.0015(8) 0.0006(8) N6 0.0262(10) 0.0315(11) 0.0228(10) 0.0009(8) 0.0072(8) -0.0015(8) C20 0.0225(10) 0.0150(9) 0.0143(10) 0.0014(8) 0.0037(8) 0.0028(8) C18 0.0215(10) 0.0165(10) 0.0179(11) -0.0003(8) 0.0074(8) -0.0037(8) C17 0.0248(11) 0.0133(9) 0.0137(10) 0.0041(8) 0.0030(8) 0.0016(8) C24 0.0177(10) 0.0237(11) 0.0248(12) 0.0004(9) 0.0018(9) -0.0030(9) C6 0.0213(10) 0.0186(10) 0.0140(10) -0.0024(8) 0.0024(8) -0.0017(8) C13 0.0183(10) 0.0158(10) 0.0191(11) -0.0033(8) 0.0063(8) -0.0011(8) N2 0.0302(11) 0.0281(10) 0.0223(11) -0.0014(8) 0.0045(9) 0.0056(8) C21 0.0205(10) 0.0155(9) 0.0158(10) -0.0025(8) 0.0050(8) 0.0006(8) C7 0.0171(10) 0.0196(10) 0.0149(10) -0.0048(8) 0.0004(8) -0.0001(8) C4 0.0143(9) 0.0157(10) 0.0186(11) -0.0029(8) 0.0017(8) 0.0006(7) N3 0.0419(12) 0.0257(10) 0.0254(11) 0.0001(8) 0.0118(10) -0.0017(9) C19 0.0221(10) 0.0127(9) 0.0147(10) 0.0006(8) 0.0066(8) -0.0012(8) C16 0.0205(10) 0.0153(9) 0.0118(10) -0.0007(7) 0.0028(8) -0.0003(8) N4 0.0457(13) 0.0249(11) 0.0380(13) 0.0003(9) 0.0063(11) -0.0127(10) C1 0.0209(10) 0.0222(11) 0.0112(10) 0.0037(8) 0.0035(8) 0.0014(8) C2 0.0211(11) 0.0172(10) 0.0209(12) -0.0003(9) 0.0022(9) 0.0034(8) C12 0.0256(11) 0.0221(11) 0.0240(12) 0.0016(9) 0.0061(10) -0.0021(9) C23 0.0215(11) 0.0227(11) 0.0251(12) 0.0035(9) 0.0012(9) 0.0011(9) F10 0.0293(7) 0.0188(6) 0.0203(7) 0.0051(5) 0.0034(6) 0.0068(5) F12 0.0346(7) 0.0212(6) 0.0138(6) 0.0034(5) 0.0028(5) 0.0042(5) F11 0.0357(7) 0.0150(6) 0.0218(7) 0.0030(5) 0.0067(6) 0.0047(5) F9 0.0338(7) 0.0266(7) 0.0131(6) 0.0011(5) 0.0006(6) 0.0039(6) C36 0.0195(10) 0.0199(10) 0.0211(12) -0.0050(9) 0.0039(9) 0.0000(8) N12 0.0479(14) 0.0376(12) 0.0219(12) -0.0077(9) 0.0032(10) 0.0067(10) C31 0.0195(10) 0.0138(9) 0.0200(11) 0.0017(8) 0.0056(9) -0.0004(8) C27 0.0226(11) 0.0201(10) 0.0190(11) -0.0035(9) 0.0051(9) -0.0029(9) C28 0.0167(10) 0.0189(10) 0.0173(10) -0.0020(8) 0.0042(8) -0.0036(8) C32 0.0191(10) 0.0193(10) 0.0124(10) 0.0011(8) 0.0034(8) -0.0020(8) C33 0.0152(9) 0.0152(9) 0.0156(10) 0.0005(8) 0.0036(8) -0.0021(8) C30 0.0160(10) 0.0154(9) 0.0175(10) 0.0032(8) 0.0033(8) 0.0002(8) C26 0.0333(13) 0.0223(12) 0.0232(12) -0.0076(9) 0.0104(10) -0.0056(9) C34 0.0183(10) 0.0169(10) 0.0177(11) 0.0001(8) 0.0047(8) -0.0012(8) N11 0.0602(15) 0.0212(11) 0.0347(13) -0.0047(9) 0.0157(12) -0.0017(10) C29 0.0185(10) 0.0216(10) 0.0134(10) 0.0021(8) 0.0025(8) -0.0014(8) C25 0.0245(11) 0.0238(11) 0.0254(13) -0.0070(9) 0.0051(10) 0.0000(9) N9 0.0364(11) 0.0193(10) 0.0313(12) -0.0021(8) 0.0087(9) 0.0019(8) C35 0.0214(11) 0.0215(11) 0.0194(11) -0.0041(9) 0.0055(9) -0.0020(8) O1S 0.0368(10) 0.0235(9) 0.0267(10) 0.0010(8) 0.0122(8) -0.0024(7) O2S 0.0449(11) 0.0235(9) 0.0302(10) -0.0010(8) 0.0163(9) -0.0055(8) O3S 0.0455(12) 0.0236(9) 0.0424(13) -0.0056(9) 0.0077(10) 0.0016(9) N10 0.0350(11) 0.0275(10) 0.0189(10) -0.0026(8) 0.0045(9) 0.0024(8) N8 0.0254(11) 0.0394(13) 0.0466(14) 0.0155(11) 0.0061(10) -0.0047(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O6 2.3366(17) . ? Gd1 O5 2.3563(17) . ? Gd1 O2 2.3672(18) . ? Gd1 O1 2.3835(17) . ? Gd1 O3 2.3896(16) . ? Gd1 O4 2.3897(17) . ? Gd1 N5 2.5188(19) . ? Gd1 N1 2.5361(18) . ? F8 C20 1.345(2) . ? F5 C17 1.341(2) . ? F7 C19 1.344(2) . ? F3 C7 1.342(2) . ? F6 C18 1.343(2) . ? F2 C6 1.341(2) . ? F4 C8 1.340(2) . ? O6 H6A 0.80(3) . ? O6 H6B 0.86(3) . ? F1 C5 1.346(2) . ? N1 C1 1.145(3) . ? O2 H2A 0.78(3) . ? O2 H2B 0.79(4) . ? O3 H3B 0.89(4) . ? O3 H3A 0.72(3) . ? O5 H5B 0.83(3) . ? O5 H5A 0.83(4) . ? N7 C24 1.149(3) . ? O1 H1B 0.82(3) . ? O1 H1A 0.78(3) . ? O4 H4B 0.83(3) . ? O4 H4A 0.823(19) . ? N5 C13 1.147(3) . ? C5 C6 1.357(3) . ? C5 C4 1.413(3) . ? C3 C1 1.419(3) . ? C3 C4 1.423(3) . ? C3 C2 1.425(3) . ? C22 C23 1.417(3) . ? C22 C21 1.418(3) . ? C22 C24 1.419(3) . ? C8 C7 1.359(3) . ? C8 C9 1.420(3) . ? C9 C6 1.416(3) . ? C9 C10 1.417(3) . ? C11 N3 1.147(3) . ? C11 C10 1.423(3) . ? C15 C13 1.416(3) . ? C15 C14 1.419(3) . ? C15 C16 1.423(3) . ? C10 C12 1.424(3) . ? C14 N6 1.147(3) . ? C20 C19 1.355(3) . ? C20 C21 1.413(3) . ? C18 C17 1.358(3) . ? C18 C21 1.421(3) . ? C17 C16 1.410(3) . ? N2 C2 1.144(3) . ? C7 C4 1.421(3) . ? C19 C16 1.415(3) . ? N4 C12 1.150(3) . ? C23 N8 1.148(3) . ? F10 C30 1.348(2) . ? F12 C32 1.343(2) . ? F11 C31 1.347(2) . ? F9 C29 1.340(2) . ? C36 N10 1.148(3) . ? C36 C34 1.423(3) . ? N12 C25 1.145(3) . ? C31 C32 1.359(3) . ? C31 C28 1.412(3) . ? C27 C28 1.417(3) . ? C27 C25 1.420(3) . ? C27 C26 1.427(3) . ? C28 C29 1.424(3) . ? C32 C33 1.413(3) . ? C33 C30 1.415(3) . ? C33 C34 1.418(3) . ? C30 C29 1.357(3) . ? C26 N11 1.147(3) . ? C34 C35 1.424(3) . ? N9 C35 1.149(3) . ? O1S H1SA 0.83(4) . ? O1S H1SB 0.83(4) . ? O2S H2SA 0.87(4) . ? O2S H2SB 0.84(4) . ? O3S H3SA 0.79(4) . ? O3S H3SB 0.78(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Gd1 O5 97.64(7) . . ? O6 Gd1 O2 89.16(7) . . ? O5 Gd1 O2 148.58(6) . . ? O6 Gd1 O1 143.51(6) . . ? O5 Gd1 O1 80.03(6) . . ? O2 Gd1 O1 111.81(7) . . ? O6 Gd1 O3 142.00(6) . . ? O5 Gd1 O3 78.04(7) . . ? O2 Gd1 O3 77.87(7) . . ? O1 Gd1 O3 73.63(6) . . ? O6 Gd1 O4 70.75(6) . . ? O5 Gd1 O4 77.00(7) . . ? O2 Gd1 O4 76.43(7) . . ? O1 Gd1 O4 141.38(6) . . ? O3 Gd1 O4 71.51(6) . . ? O6 Gd1 N5 71.82(6) . . ? O5 Gd1 N5 71.84(6) . . ? O2 Gd1 N5 138.78(6) . . ? O1 Gd1 N5 72.93(6) . . ? O3 Gd1 N5 138.03(6) . . ? O4 Gd1 N5 126.66(6) . . ? O6 Gd1 N1 84.55(6) . . ? O5 Gd1 N1 141.47(6) . . ? O2 Gd1 N1 69.52(6) . . ? O1 Gd1 N1 76.12(6) . . ? O3 Gd1 N1 122.22(6) . . ? O4 Gd1 N1 137.95(7) . . ? N5 Gd1 N1 72.45(6) . . ? Gd1 O6 H6A 128(2) . . ? Gd1 O6 H6B 125(2) . . ? H6A O6 H6B 107(3) . . ? C1 N1 Gd1 173.82(17) . . ? Gd1 O2 H2A 116(2) . . ? Gd1 O2 H2B 119(2) . . ? H2A O2 H2B 111(3) . . ? Gd1 O3 H3B 126(2) . . ? Gd1 O3 H3A 121(2) . . ? H3B O3 H3A 110(3) . . ? Gd1 O5 H5B 125(2) . . ? Gd1 O5 H5A 122(2) . . ? H5B O5 H5A 106(3) . . ? Gd1 O1 H1B 123(2) . . ? Gd1 O1 H1A 126(2) . . ? H1B O1 H1A 110(3) . . ? Gd1 O4 H4B 118(2) . . ? Gd1 O4 H4A 128(3) . . ? H4B O4 H4A 112(4) . . ? C13 N5 Gd1 170.98(17) . . ? F1 C5 C6 117.14(19) . . ? F1 C5 C4 118.90(18) . . ? C6 C5 C4 123.87(19) . . ? C1 C3 C4 120.63(19) . . ? C1 C3 C2 115.15(18) . . ? C4 C3 C2 124.06(19) . . ? C23 C22 C21 123.68(19) . . ? C23 C22 C24 113.69(19) . . ? C21 C22 C24 122.6(2) . . ? F4 C8 C7 118.16(19) . . ? F4 C8 C9 118.43(19) . . ? C7 C8 C9 123.40(19) . . ? C6 C9 C10 122.1(2) . . ? C6 C9 C8 112.95(18) . . ? C10 C9 C8 124.90(19) . . ? N3 C11 C10 176.9(2) . . ? C13 C15 C14 113.05(18) . . ? C13 C15 C16 122.88(19) . . ? C14 C15 C16 124.06(18) . . ? C9 C10 C11 123.28(19) . . ? C9 C10 C12 123.3(2) . . ? C11 C10 C12 112.85(19) . . ? N6 C14 C15 175.4(2) . . ? F8 C20 C19 117.70(18) . . ? F8 C20 C21 118.47(18) . . ? C19 C20 C21 123.82(19) . . ? F6 C18 C17 117.98(18) . . ? F6 C18 C21 119.05(18) . . ? C17 C18 C21 122.96(19) . . ? F5 C17 C18 118.01(18) . . ? F5 C17 C16 118.41(18) . . ? C18 C17 C16 123.57(19) . . ? N7 C24 C22 177.3(2) . . ? F2 C6 C5 118.09(18) . . ? F2 C6 C9 118.43(18) . . ? C5 C6 C9 123.5(2) . . ? N5 C13 C15 175.2(2) . . ? C20 C21 C22 123.65(19) . . ? C20 C21 C18 113.13(18) . . ? C22 C21 C18 123.22(19) . . ? F3 C7 C8 118.21(18) . . ? F3 C7 C4 118.27(19) . . ? C8 C7 C4 123.52(19) . . ? C5 C4 C7 112.78(18) . . ? C5 C4 C3 123.00(18) . . ? C7 C4 C3 124.22(19) . . ? F7 C19 C20 118.08(18) . . ? F7 C19 C16 119.02(18) . . ? C20 C19 C16 122.89(19) . . ? C17 C16 C19 113.54(18) . . ? C17 C16 C15 123.03(18) . . ? C19 C16 C15 123.43(19) . . ? N1 C1 C3 179.4(3) . . ? N2 C2 C3 176.5(2) . . ? N4 C12 C10 175.3(3) . . ? N8 C23 C22 177.0(2) . . ? N10 C36 C34 177.6(2) . . ? F11 C31 C32 117.75(19) . . ? F11 C31 C28 118.49(18) . . ? C32 C31 C28 123.72(19) . . ? C28 C27 C25 122.3(2) . . ? C28 C27 C26 122.9(2) . . ? C25 C27 C26 114.61(19) . . ? C31 C28 C27 123.1(2) . . ? C31 C28 C29 113.18(18) . . ? C27 C28 C29 123.8(2) . . ? F12 C32 C31 117.94(18) . . ? F12 C32 C33 118.73(18) . . ? C31 C32 C33 123.27(19) . . ? C32 C33 C30 113.12(18) . . ? C32 C33 C34 122.75(19) . . ? C30 C33 C34 124.13(18) . . ? F10 C30 C29 117.76(18) . . ? F10 C30 C33 118.24(18) . . ? C29 C30 C33 123.95(19) . . ? N11 C26 C27 177.1(3) . . ? C33 C34 C36 122.31(19) . . ? C33 C34 C35 123.16(19) . . ? C36 C34 C35 114.30(19) . . ? F9 C29 C30 118.07(18) . . ? F9 C29 C28 119.13(18) . . ? C30 C29 C28 122.76(19) . . ? N12 C25 C27 178.8(3) . . ? N9 C35 C34 176.9(2) . . ? H1SA O1S H1SB 104(3) . . ? H2SA O2S H2SB 112(3) . . ? H3SA O3S H3SB 113(4) . . ? 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 O6 Gd1 N1 C1 -116.5(16) . . . . ? O5 Gd1 N1 C1 -21.1(17) . . . . ? O2 Gd1 N1 C1 152.4(16) . . . . ? O1 Gd1 N1 C1 32.3(16) . . . . ? O3 Gd1 N1 C1 92.4(16) . . . . ? O4 Gd1 N1 C1 -169.6(16) . . . . ? N5 Gd1 N1 C1 -43.9(16) . . . . ? O6 Gd1 N5 C13 -147.3(11) . . . . ? O5 Gd1 N5 C13 -42.5(11) . . . . ? O2 Gd1 N5 C13 146.2(11) . . . . ? O1 Gd1 N5 C13 42.3(11) . . . . ? O3 Gd1 N5 C13 3.8(11) . . . . ? O4 Gd1 N5 C13 -99.9(11) . . . . ? N1 Gd1 N5 C13 122.7(11) . . . . ? F4 C8 C9 C6 178.92(18) . . . . ? C7 C8 C9 C6 0.1(3) . . . . ? F4 C8 C9 C10 -2.8(3) . . . . ? C7 C8 C9 C10 178.4(2) . . . . ? C6 C9 C10 C11 -10.0(3) . . . . ? C8 C9 C10 C11 171.9(2) . . . . ? C6 C9 C10 C12 179.2(2) . . . . ? C8 C9 C10 C12 1.1(3) . . . . ? N3 C11 C10 C9 -151(5) . . . . ? N3 C11 C10 C12 21(5) . . . . ? C13 C15 C14 N6 15(3) . . . . ? C16 C15 C14 N6 -164(3) . . . . ? F6 C18 C17 F5 -0.3(3) . . . . ? C21 C18 C17 F5 179.52(18) . . . . ? F6 C18 C17 C16 178.12(18) . . . . ? C21 C18 C17 C16 -2.1(3) . . . . ? C23 C22 C24 N7 16(6) . . . . ? C21 C22 C24 N7 -162(5) . . . . ? F1 C5 C6 F2 -0.4(3) . . . . ? C4 C5 C6 F2 -176.89(19) . . . . ? F1 C5 C6 C9 178.17(18) . . . . ? C4 C5 C6 C9 1.7(3) . . . . ? C10 C9 C6 F2 -1.1(3) . . . . ? C8 C9 C6 F2 177.23(18) . . . . ? C10 C9 C6 C5 -179.6(2) . . . . ? C8 C9 C6 C5 -1.3(3) . . . . ? Gd1 N5 C13 C15 -51(3) . . . . ? C14 C15 C13 N5 5(3) . . . . ? C16 C15 C13 N5 -176(3) . . . . ? F8 C20 C21 C22 2.5(3) . . . . ? C19 C20 C21 C22 -178.6(2) . . . . ? F8 C20 C21 C18 -176.74(18) . . . . ? C19 C20 C21 C18 2.1(3) . . . . ? C23 C22 C21 C20 179.3(2) . . . . ? C24 C22 C21 C20 -2.3(3) . . . . ? C23 C22 C21 C18 -1.5(3) . . . . ? C24 C22 C21 C18 176.8(2) . . . . ? F6 C18 C21 C20 179.01(18) . . . . ? C17 C18 C21 C20 -0.8(3) . . . . ? F6 C18 C21 C22 -0.2(3) . . . . ? C17 C18 C21 C22 180.0(2) . . . . ? F4 C8 C7 F3 1.8(3) . . . . ? C9 C8 C7 F3 -179.44(18) . . . . ? F4 C8 C7 C4 -177.99(18) . . . . ? C9 C8 C7 C4 0.8(3) . . . . ? F1 C5 C4 C7 -177.11(17) . . . . ? C6 C5 C4 C7 -0.7(3) . . . . ? F1 C5 C4 C3 3.2(3) . . . . ? C6 C5 C4 C3 179.7(2) . . . . ? F3 C7 C4 C5 179.70(17) . . . . ? C8 C7 C4 C5 -0.5(3) . . . . ? F3 C7 C4 C3 -0.6(3) . . . . ? C8 C7 C4 C3 179.1(2) . . . . ? C1 C3 C4 C5 13.6(3) . . . . ? C2 C3 C4 C5 -171.1(2) . . . . ? C1 C3 C4 C7 -166.0(2) . . . . ? C2 C3 C4 C7 9.3(3) . . . . ? F8 C20 C19 F7 -0.2(3) . . . . ? C21 C20 C19 F7 -179.13(18) . . . . ? F8 C20 C19 C16 178.20(18) . . . . ? C21 C20 C19 C16 -0.7(3) . . . . ? F5 C17 C16 C19 -178.18(17) . . . . ? C18 C17 C16 C19 3.4(3) . . . . ? F5 C17 C16 C15 1.2(3) . . . . ? C18 C17 C16 C15 -177.2(2) . . . . ? F7 C19 C16 C17 176.36(17) . . . . ? C20 C19 C16 C17 -2.1(3) . . . . ? F7 C19 C16 C15 -3.0(3) . . . . ? C20 C19 C16 C15 178.6(2) . . . . ? C13 C15 C16 C17 -6.2(3) . . . . ? C14 C15 C16 C17 172.6(2) . . . . ? C13 C15 C16 C19 173.10(19) . . . . ? C14 C15 C16 C19 -8.1(3) . . . . ? Gd1 N1 C1 C3 -100(22) . . . . ? C4 C3 C1 N1 107(22) . . . . ? C2 C3 C1 N1 -69(22) . . . . ? C1 C3 C2 N2 -42(4) . . . . ? C4 C3 C2 N2 143(4) . . . . ? C9 C10 C12 N4 175(3) . . . . ? C11 C10 C12 N4 3(3) . . . . ? C21 C22 C23 N8 -175(5) . . . . ? C24 C22 C23 N8 7(5) . . . . ? F11 C31 C28 C27 2.8(3) . . . . ? C32 C31 C28 C27 -179.9(2) . . . . ? F11 C31 C28 C29 -177.40(17) . . . . ? C32 C31 C28 C29 0.0(3) . . . . ? C25 C27 C28 C31 -175.0(2) . . . . ? C26 C27 C28 C31 10.3(3) . . . . ? C25 C27 C28 C29 5.2(3) . . . . ? C26 C27 C28 C29 -169.6(2) . . . . ? F11 C31 C32 F12 0.0(3) . . . . ? C28 C31 C32 F12 -177.38(18) . . . . ? F11 C31 C32 C33 177.34(18) . . . . ? C28 C31 C32 C33 -0.1(3) . . . . ? F12 C32 C33 C30 177.44(17) . . . . ? C31 C32 C33 C30 0.1(3) . . . . ? F12 C32 C33 C34 -2.0(3) . . . . ? C31 C32 C33 C34 -179.3(2) . . . . ? C32 C33 C30 F10 177.35(17) . . . . ? C34 C33 C30 F10 -3.2(3) . . . . ? C32 C33 C30 C29 -0.1(3) . . . . ? C34 C33 C30 C29 179.3(2) . . . . ? C28 C27 C26 N11 147(5) . . . . ? C25 C27 C26 N11 -28(5) . . . . ? C32 C33 C34 C36 -13.1(3) . . . . ? C30 C33 C34 C36 167.5(2) . . . . ? C32 C33 C34 C35 172.72(19) . . . . ? C30 C33 C34 C35 -6.7(3) . . . . ? N10 C36 C34 C33 -149(6) . . . . ? N10 C36 C34 C35 26(6) . . . . ? F10 C30 C29 F9 0.3(3) . . . . ? C33 C30 C29 F9 177.79(18) . . . . ? F10 C30 C29 C28 -177.43(18) . . . . ? C33 C30 C29 C28 0.1(3) . . . . ? C31 C28 C29 F9 -177.68(18) . . . . ? C27 C28 C29 F9 2.2(3) . . . . ? C31 C28 C29 C30 0.0(3) . . . . ? C27 C28 C29 C30 179.9(2) . . . . ? C28 C27 C25 N12 -179(100) . . . . ? C26 C27 C25 N12 -4(13) . . . . ? C33 C34 C35 N9 -168(4) . . . . ? C36 C34 C35 N9 17(4) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.715 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.078 # Attachment 'LASMTQF4.CIF' data_g:\nazari~1\nazari~1\crysta~1\nl104l~1\lasmtqf4 _database_code_depnum_ccdc_archive 'CCDC 749364' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Lanthanum-Samarium(III) 2,3,5,6-Tetrafluoro-7,7,8,8-Tetracyanoquinodimethane' ; _chemical_name_common ;Lanthanum-Samarium(iii) 2,3,5,6-Tetrafluoro-7,7,8,8- Tetracyanoquinodimethane' ; _chemical_melting_point ? _chemical_formula_sum 'C36 H20 F12 La0.80 N12 O10 Sm0.20' _chemical_formula_weight 1149.84 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.6479(17) _cell_length_b 17.5557(15) _cell_length_c 18.3925(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.919(8) _cell_angle_gamma 90.00 _cell_volume 4374.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 383(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6374 _exptl_absorpt_correction_T_max 0.8440 _exptl_absorpt_process_details 'SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 383(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38452 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.32 _reflns_number_total 10612 _reflns_number_gt 9251 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0518P)^2^+19.8058P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10612 _refine_ls_number_parameters 679 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 1.115 _refine_ls_shift/su_mean 0.058 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.236380(13) 0.475082(10) 0.088524(10) 0.01338(7) Uani 0.034(17) 1 d P . . La1 La 0.236380(13) 0.475082(10) 0.088524(10) 0.01338(7) Uani 0.966(17) 1 d P . . F1 F 0.28257(19) 0.53298(12) 0.34480(12) 0.0274(5) Uani 1 1 d . . . F2 F 0.38267(18) 0.32033(12) 0.49552(12) 0.0250(5) Uani 1 1 d . . . F3 F 0.33059(19) 0.62448(12) 0.45587(12) 0.0280(5) Uani 1 1 d . . . F4 F 0.43769(18) 0.41278(13) 0.60530(12) 0.0258(5) Uani 1 1 d . . . F5 F 0.55384(16) 0.60138(13) 0.15447(12) 0.0243(5) Uani 1 1 d . . . F6 F 0.55599(17) 0.76455(12) 0.36127(12) 0.0237(5) Uani 1 1 d . . . F7 F 0.74602(17) 0.60829(14) 0.16556(13) 0.0283(5) Uani 1 1 d . . . F8 F 0.74945(17) 0.77444(12) 0.36972(12) 0.0260(5) Uani 1 1 d . . . F9 F 0.03863(18) 0.52351(13) 0.35968(12) 0.0267(5) Uani 1 1 d . . . F10 F 0.17168(17) 0.34925(12) 0.54325(12) 0.0252(5) Uani 1 1 d . . . F11 F 0.07901(18) 0.63680(12) 0.45142(12) 0.0269(5) Uani 1 1 d . . . F12 F 0.21370(18) 0.46221(13) 0.63417(12) 0.0253(5) Uani 1 1 d . . . O1 O 0.1362(2) 0.56553(15) 0.15150(16) 0.0235(6) Uani 1 1 d D . . O2 O 0.0750(2) 0.41305(15) 0.11020(15) 0.0228(5) Uani 1 1 d D . . O3 O 0.2265(2) 0.60650(15) 0.01989(15) 0.0242(6) Uani 1 1 d D . . O4 O 0.1223(2) 0.46789(17) -0.02709(16) 0.0293(6) Uani 1 1 d D . . O5 O 0.3531(2) 0.47487(19) -0.00879(18) 0.0343(7) Uani 1 1 d D . . O6 O 0.2545(2) 0.33679(15) 0.06105(16) 0.0278(6) Uani 1 1 d D . . O7 O 0.4084(2) 0.42870(17) 0.13981(16) 0.0284(6) Uani 1 1 d D . . O8 O 0.0094(2) 0.64880(16) 0.01787(16) 0.0276(6) Uani 1 1 d D . . O9 O 0.5242(3) 0.3869(2) 0.0109(2) 0.0472(9) Uiso 1 1 d D . . O10 O 0.8318(5) 0.4329(4) 0.1276(4) 0.1031(19) Uiso 1 1 d . . . N1 N 0.2418(2) 0.41951(18) 0.22384(17) 0.0225(6) Uani 1 1 d . . . N2 N 0.3227(3) 0.22616(19) 0.35289(19) 0.0272(7) Uani 1 1 d . . . N3 N 0.4267(3) 0.7199(2) 0.5850(2) 0.0334(8) Uani 1 1 d . . . N4 N 0.4723(3) 0.5310(2) 0.7281(2) 0.0371(9) Uani 1 1 d . . . N5 N 0.3425(2) 0.57767(18) 0.16878(18) 0.0229(6) Uani 1 1 d . . . N6 N 0.3290(3) 0.7441(2) 0.3362(2) 0.0285(7) Uani 1 1 d . . . N7 N 0.9637(3) 0.5970(3) 0.2090(3) 0.0421(10) Uani 1 1 d . . . N8 N 0.9737(3) 0.7874(3) 0.3550(3) 0.0496(12) Uani 1 1 d . . . N9 N 0.0169(3) 0.3818(2) 0.25882(19) 0.0290(7) Uani 1 1 d . . . N10 N 0.1175(3) 0.22788(19) 0.4303(2) 0.0309(8) Uani 1 1 d . . . N11 N 0.1672(3) 0.7585(2) 0.5578(2) 0.0349(8) Uani 1 1 d . . . N12 N 0.2360(3) 0.6050(2) 0.7343(2) 0.0362(9) Uani 1 1 d . . . C1 C 0.2694(3) 0.3997(2) 0.28221(19) 0.0184(7) Uani 1 1 d . . . C2 C 0.3158(3) 0.2913(2) 0.35575(19) 0.0205(7) Uani 1 1 d . . . C3 C 0.3034(3) 0.3722(2) 0.35341(19) 0.0181(7) Uani 1 1 d . . . C4 C 0.3313(2) 0.4214(2) 0.41339(18) 0.0166(6) Uani 1 1 d . . . C5 C 0.3214(3) 0.5018(2) 0.40853(19) 0.0186(7) Uani 1 1 d . . . C6 C 0.3711(3) 0.3954(2) 0.48432(19) 0.0181(7) Uani 1 1 d . . . C7 C 0.3469(3) 0.5495(2) 0.4665(2) 0.0191(7) Uani 1 1 d . . . C8 C 0.3982(3) 0.4434(2) 0.54159(19) 0.0187(7) Uani 1 1 d . . . C9 C 0.3869(3) 0.5239(2) 0.5367(2) 0.0180(7) Uani 1 1 d . . . C10 C 0.4130(3) 0.5741(2) 0.5962(2) 0.0208(7) Uani 1 1 d . . . C11 C 0.4182(3) 0.6549(2) 0.5885(2) 0.0248(8) Uani 1 1 d . . . C12 C 0.4458(3) 0.5480(2) 0.6685(2) 0.0251(8) Uani 1 1 d . . . C13 C 0.3869(3) 0.6202(2) 0.2069(2) 0.0191(7) Uani 1 1 d . . . C14 C 0.3809(3) 0.7135(2) 0.3009(2) 0.0217(7) Uani 1 1 d . . . C15 C 0.4403(3) 0.6731(2) 0.25500(19) 0.0187(7) Uani 1 1 d . . . C16 C 0.5442(3) 0.68178(19) 0.25793(19) 0.0172(7) Uani 1 1 d . . . C17 C 0.6010(3) 0.6435(2) 0.20951(19) 0.0189(7) Uani 1 1 d . . . C18 C 0.6021(3) 0.72726(19) 0.31098(19) 0.0188(7) Uani 1 1 d . . . C19 C 0.7011(3) 0.6473(2) 0.2148(2) 0.0212(7) Uani 1 1 d . . . C20 C 0.7024(3) 0.7320(2) 0.3153(2) 0.0212(7) Uani 1 1 d . . . C21 C 0.7587(3) 0.6918(2) 0.2683(2) 0.0202(7) Uani 1 1 d . . . C22 C 0.8633(3) 0.6937(2) 0.2745(2) 0.0261(8) Uani 1 1 d . . . C23 C 0.9179(3) 0.6407(3) 0.2368(3) 0.0306(9) Uani 1 1 d . . . C24 C 0.9218(3) 0.7462(3) 0.3202(3) 0.0341(10) Uani 1 1 d . . . C25 C 0.0466(3) 0.3787(2) 0.3199(2) 0.0221(7) Uani 1 1 d . . . C26 C 0.1033(3) 0.2913(2) 0.4157(2) 0.0234(8) Uani 1 1 d . . . C27 C 0.0864(3) 0.3689(2) 0.3950(2) 0.0200(7) Uani 1 1 d . . . C28 C 0.1052(2) 0.4299(2) 0.44530(19) 0.0175(7) Uani 1 1 d . . . C29 C 0.0836(3) 0.5077(2) 0.4269(2) 0.0190(7) Uani 1 1 d . . . C30 C 0.1483(3) 0.4200(2) 0.5189(2) 0.0188(7) Uani 1 1 d . . . C31 C 0.1051(3) 0.5665(2) 0.4748(2) 0.0187(7) Uani 1 1 d . . . C32 C 0.1697(3) 0.4789(2) 0.5666(2) 0.0189(7) Uani 1 1 d . . . C33 C 0.1511(3) 0.5564(2) 0.54784(19) 0.0179(7) Uani 1 1 d . . . C34 C 0.1770(3) 0.6173(2) 0.5964(2) 0.0215(7) Uani 1 1 d . . . C35 C 0.1702(3) 0.6950(2) 0.5739(2) 0.0242(8) Uani 1 1 d . . . C36 C 0.2106(3) 0.6076(2) 0.6727(2) 0.0248(8) Uani 1 1 d . . . H1A H 0.0756(19) 0.557(2) 0.167(3) 0.037 Uiso 1 1 d D . . H2A H 0.061(3) 0.402(3) 0.1566(9) 0.037 Uiso 1 1 d D . . H3A H 0.217(4) 0.606(3) -0.0307(6) 0.037 Uiso 1 1 d D . . H4A H 0.134(3) 0.488(3) -0.0715(13) 0.037 Uiso 1 1 d D . . H5A H 0.383(3) 0.5195(12) -0.021(3) 0.037 Uiso 1 1 d D . . H6A H 0.274(4) 0.314(2) 0.0201(16) 0.037 Uiso 1 1 d D . . H7A H 0.440(3) 0.453(2) 0.1806(17) 0.037 Uiso 1 1 d D . . H8A H 0.0753(11) 0.641(3) 0.032(3) 0.037 Uiso 1 1 d D . . H1B H 0.155(3) 0.6159(9) 0.153(3) 0.037 Uiso 1 1 d D . . H2B H 0.040(3) 0.385(2) 0.0741(15) 0.037 Uiso 1 1 d D . . H3B H 0.267(3) 0.6463(19) 0.038(2) 0.037 Uiso 1 1 d D . . H4B H 0.070(3) 0.434(2) -0.032(2) 0.037 Uiso 1 1 d D . . H5B H 0.392(3) 0.4325(13) -0.012(3) 0.037 Uiso 1 1 d D . . H6B H 0.231(3) 0.3030(19) 0.0927(19) 0.037 Uiso 1 1 d D . . H7B H 0.428(3) 0.3788(10) 0.136(2) 0.037 Uiso 1 1 d D . . H9B H 0.489(3) 0.3471(19) 0.024(3) 0.037 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.01565(10) 0.01103(10) 0.01302(10) -0.00013(6) -0.00004(7) 0.00094(6) La1 0.01565(10) 0.01103(10) 0.01302(10) -0.00013(6) -0.00004(7) 0.00094(6) F1 0.0448(14) 0.0187(11) 0.0164(10) 0.0043(8) -0.0053(10) 0.0026(10) F2 0.0378(13) 0.0147(10) 0.0216(11) 0.0028(8) -0.0006(9) 0.0058(9) F3 0.0459(14) 0.0137(10) 0.0227(11) 0.0021(8) -0.0031(10) -0.0004(9) F4 0.0364(12) 0.0223(11) 0.0167(10) 0.0039(8) -0.0054(9) 0.0031(9) F5 0.0228(11) 0.0279(12) 0.0221(11) -0.0100(9) 0.0017(8) -0.0029(9) F6 0.0306(11) 0.0200(10) 0.0202(11) -0.0051(8) 0.0022(9) 0.0006(9) F7 0.0247(11) 0.0309(12) 0.0306(12) -0.0075(10) 0.0084(9) 0.0014(9) F8 0.0298(12) 0.0197(11) 0.0254(11) -0.0026(9) -0.0087(9) -0.0055(9) F9 0.0366(13) 0.0224(11) 0.0190(11) 0.0014(8) -0.0048(9) 0.0023(9) F10 0.0340(12) 0.0153(10) 0.0254(11) 0.0037(8) 0.0003(9) 0.0028(9) F11 0.0397(13) 0.0143(10) 0.0251(11) 0.0019(8) -0.0022(10) 0.0052(9) F12 0.0343(12) 0.0228(11) 0.0173(10) 0.0038(8) -0.0025(9) 0.0000(9) O1 0.0231(13) 0.0147(12) 0.0345(15) -0.0025(11) 0.0106(11) -0.0009(10) O2 0.0233(13) 0.0238(13) 0.0203(13) -0.0005(10) -0.0014(10) -0.0052(10) O3 0.0343(15) 0.0174(12) 0.0213(13) -0.0002(10) 0.0053(11) -0.0013(11) O4 0.0350(16) 0.0305(15) 0.0204(13) 0.0069(11) -0.0046(12) -0.0093(12) O5 0.0359(17) 0.0391(18) 0.0296(16) 0.0043(13) 0.0105(13) 0.0140(14) O6 0.0415(16) 0.0160(12) 0.0284(15) -0.0006(11) 0.0137(13) -0.0001(12) O7 0.0252(14) 0.0311(15) 0.0268(14) -0.0078(12) -0.0054(11) 0.0118(12) O8 0.0279(14) 0.0239(14) 0.0285(15) -0.0025(11) -0.0077(11) -0.0009(11) N1 0.0269(16) 0.0198(15) 0.0202(15) -0.0009(12) 0.0002(12) -0.0004(12) N2 0.0331(18) 0.0193(16) 0.0283(17) 0.0009(13) 0.0005(14) 0.0001(13) N3 0.040(2) 0.0237(18) 0.035(2) -0.0037(15) 0.0000(16) -0.0082(15) N4 0.049(2) 0.035(2) 0.0242(18) -0.0031(15) -0.0086(16) 0.0012(17) N5 0.0192(14) 0.0202(15) 0.0291(17) -0.0019(13) 0.0024(12) 0.0010(12) N6 0.0321(18) 0.0222(16) 0.0325(18) -0.0010(14) 0.0099(15) -0.0006(14) N7 0.0237(18) 0.051(3) 0.054(3) 0.004(2) 0.0119(17) 0.0035(17) N8 0.038(2) 0.045(2) 0.061(3) 0.010(2) -0.016(2) -0.0190(19) N9 0.0343(18) 0.0289(18) 0.0238(17) -0.0049(14) 0.0035(14) -0.0044(15) N10 0.046(2) 0.0175(16) 0.0317(19) -0.0036(13) 0.0137(16) -0.0035(14) N11 0.052(2) 0.0224(18) 0.0313(19) -0.0019(14) 0.0082(17) -0.0039(16) N12 0.050(2) 0.037(2) 0.0210(18) -0.0057(15) 0.0036(16) -0.0039(18) C1 0.0183(16) 0.0171(16) 0.0200(17) -0.0022(13) 0.0025(13) -0.0023(13) C2 0.0230(17) 0.0213(18) 0.0171(16) 0.0017(13) 0.0019(13) 0.0012(14) C3 0.0208(16) 0.0167(16) 0.0165(16) 0.0010(13) 0.0007(13) 0.0000(13) C4 0.0167(15) 0.0178(16) 0.0154(15) 0.0019(12) 0.0028(12) 0.0008(13) C5 0.0234(17) 0.0162(16) 0.0156(16) 0.0035(13) 0.0005(13) 0.0006(13) C6 0.0201(16) 0.0150(16) 0.0195(16) 0.0029(13) 0.0032(13) 0.0034(13) C7 0.0232(17) 0.0144(15) 0.0196(17) 0.0027(13) 0.0017(13) -0.0007(13) C8 0.0181(16) 0.0214(17) 0.0162(16) 0.0044(13) 0.0003(12) 0.0007(13) C9 0.0168(15) 0.0191(17) 0.0178(16) 0.0005(13) 0.0008(13) -0.0013(13) C10 0.0212(17) 0.0209(17) 0.0196(17) -0.0010(14) -0.0008(13) -0.0029(14) C11 0.0253(18) 0.027(2) 0.0209(18) -0.0029(15) -0.0007(14) -0.0046(15) C12 0.0259(19) 0.0242(18) 0.0239(19) -0.0020(15) -0.0021(15) -0.0025(15) C13 0.0175(16) 0.0166(16) 0.0231(17) 0.0022(13) 0.0026(13) 0.0015(13) C14 0.0243(17) 0.0157(16) 0.0250(18) 0.0003(14) 0.0026(14) -0.0009(14) C15 0.0227(17) 0.0146(15) 0.0188(16) 0.0000(13) 0.0024(13) 0.0005(13) C16 0.0214(16) 0.0127(15) 0.0169(16) 0.0013(12) -0.0003(13) -0.0006(13) C17 0.0220(17) 0.0162(16) 0.0179(16) -0.0014(13) 0.0006(13) -0.0017(13) C18 0.0259(17) 0.0130(15) 0.0170(16) 0.0014(12) 0.0007(13) 0.0005(13) C19 0.0222(17) 0.0196(17) 0.0216(17) 0.0007(14) 0.0012(14) 0.0003(14) C20 0.0268(18) 0.0145(16) 0.0205(17) 0.0010(13) -0.0042(14) -0.0048(14) C21 0.0206(17) 0.0153(16) 0.0239(18) 0.0046(13) -0.0003(14) -0.0030(13) C22 0.0207(18) 0.0240(19) 0.033(2) 0.0059(16) 0.0009(15) -0.0050(15) C23 0.0192(18) 0.034(2) 0.038(2) 0.0080(18) 0.0029(16) -0.0039(16) C24 0.027(2) 0.031(2) 0.043(3) 0.0091(19) -0.0037(18) -0.0081(17) C25 0.0232(17) 0.0186(17) 0.0253(19) -0.0053(14) 0.0066(14) -0.0045(14) C26 0.0269(18) 0.0208(18) 0.0238(18) -0.0059(14) 0.0086(15) -0.0045(14) C27 0.0215(17) 0.0164(16) 0.0228(17) -0.0020(13) 0.0055(14) -0.0022(13) C28 0.0173(15) 0.0165(16) 0.0192(16) -0.0014(13) 0.0039(13) -0.0007(13) C29 0.0211(17) 0.0183(16) 0.0173(16) 0.0009(13) 0.0004(13) 0.0025(13) C30 0.0203(16) 0.0149(16) 0.0214(17) 0.0031(13) 0.0039(13) 0.0006(13) C31 0.0200(16) 0.0155(16) 0.0206(17) 0.0012(13) 0.0019(13) 0.0030(13) C32 0.0196(16) 0.0197(17) 0.0174(16) 0.0017(13) 0.0026(13) 0.0000(13) C33 0.0192(16) 0.0166(16) 0.0183(16) -0.0005(13) 0.0047(13) 0.0003(13) C34 0.0263(18) 0.0190(17) 0.0195(17) -0.0018(14) 0.0042(14) -0.0024(14) C35 0.032(2) 0.0217(19) 0.0198(17) -0.0049(14) 0.0069(15) -0.0035(15) C36 0.0305(19) 0.0207(18) 0.0242(19) -0.0047(14) 0.0073(15) -0.0040(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O1 2.473(3) . ? Sm1 O4 2.483(3) . ? Sm1 O6 2.498(3) . ? Sm1 O2 2.532(3) . ? Sm1 O5 2.535(3) . ? Sm1 O7 2.556(3) . ? Sm1 O3 2.625(3) . ? Sm1 N5 2.646(3) . ? Sm1 N1 2.666(3) . ? F1 C5 1.343(4) . ? F2 C6 1.341(4) . ? F3 C7 1.345(4) . ? F4 C8 1.342(4) . ? F5 C17 1.352(4) . ? F6 C18 1.349(4) . ? F7 C19 1.342(4) . ? F8 C20 1.347(4) . ? F9 C29 1.342(4) . ? F10 C30 1.346(4) . ? F11 C31 1.341(4) . ? F12 C32 1.346(4) . ? N1 C1 1.148(5) . ? N2 C2 1.149(5) . ? N3 C11 1.150(5) . ? N4 C12 1.151(5) . ? N5 C13 1.146(5) . ? N6 C14 1.150(5) . ? N7 C23 1.148(6) . ? N8 C24 1.152(6) . ? N9 C25 1.149(5) . ? N10 C26 1.157(5) . ? N11 C35 1.153(5) . ? N12 C36 1.144(5) . ? C1 C3 1.420(5) . ? C2 C3 1.431(5) . ? C3 C4 1.416(5) . ? C4 C5 1.420(5) . ? C4 C6 1.426(5) . ? C5 C7 1.367(5) . ? C6 C8 1.364(5) . ? C7 C9 1.414(5) . ? C8 C9 1.423(5) . ? C9 C10 1.417(5) . ? C10 C12 1.427(5) . ? C10 C11 1.428(5) . ? C13 C15 1.422(5) . ? C14 C15 1.428(5) . ? C15 C16 1.421(5) . ? C16 C17 1.419(5) . ? C16 C18 1.424(5) . ? C17 C19 1.359(5) . ? C18 C20 1.364(5) . ? C19 C21 1.417(5) . ? C20 C21 1.413(5) . ? C21 C22 1.420(5) . ? C22 C23 1.423(6) . ? C22 C24 1.425(6) . ? C25 C27 1.433(5) . ? C26 C27 1.425(5) . ? C27 C28 1.418(5) . ? C28 C30 1.420(5) . ? C28 C29 1.428(5) . ? C29 C31 1.366(5) . ? C30 C32 1.365(5) . ? C31 C33 1.424(5) . ? C32 C33 1.418(5) . ? C33 C34 1.411(5) . ? C34 C35 1.424(5) . ? C34 C36 1.434(5) . ? 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 Sm1 O4 96.24(10) . . ? O1 Sm1 O6 142.45(9) . . ? O4 Sm1 O6 81.06(10) . . ? O1 Sm1 O2 70.23(9) . . ? O4 Sm1 O2 69.21(9) . . ? O6 Sm1 O2 73.94(9) . . ? O1 Sm1 O5 139.60(10) . . ? O4 Sm1 O5 77.17(11) . . ? O6 Sm1 O5 76.68(10) . . ? O2 Sm1 O5 138.00(10) . . ? O1 Sm1 O7 124.54(9) . . ? O4 Sm1 O7 138.89(10) . . ? O6 Sm1 O7 69.87(10) . . ? O2 Sm1 O7 125.66(10) . . ? O5 Sm1 O7 68.45(10) . . ? O1 Sm1 O3 70.22(9) . . ? O4 Sm1 O3 69.04(9) . . ? O6 Sm1 O3 139.23(9) . . ? O2 Sm1 O3 117.28(9) . . ? O5 Sm1 O3 70.25(9) . . ? O7 Sm1 O3 116.69(10) . . ? O1 Sm1 N5 66.29(9) . . ? O4 Sm1 N5 139.18(10) . . ? O6 Sm1 N5 135.50(10) . . ? O2 Sm1 N5 129.26(9) . . ? O5 Sm1 N5 92.68(11) . . ? O7 Sm1 N5 66.07(10) . . ? O3 Sm1 N5 70.32(9) . . ? O1 Sm1 N1 75.66(10) . . ? O4 Sm1 N1 136.46(10) . . ? O6 Sm1 N1 80.85(10) . . ? O2 Sm1 N1 67.81(9) . . ? O5 Sm1 N1 135.19(10) . . ? O7 Sm1 N1 67.54(10) . . ? O3 Sm1 N1 139.86(9) . . ? N5 Sm1 N1 77.09(10) . . ? C1 N1 Sm1 162.3(3) . . ? C13 N5 Sm1 176.2(3) . . ? N1 C1 C3 177.7(4) . . ? N2 C2 C3 175.4(4) . . ? C4 C3 C1 122.6(3) . . ? C4 C3 C2 124.2(3) . . ? C1 C3 C2 112.9(3) . . ? C3 C4 C5 122.9(3) . . ? C3 C4 C6 123.7(3) . . ? C5 C4 C6 113.5(3) . . ? F1 C5 C7 117.8(3) . . ? F1 C5 C4 119.0(3) . . ? C7 C5 C4 123.2(3) . . ? F2 C6 C8 118.2(3) . . ? F2 C6 C4 118.7(3) . . ? C8 C6 C4 123.2(3) . . ? F3 C7 C5 117.7(3) . . ? F3 C7 C9 118.9(3) . . ? C5 C7 C9 123.4(3) . . ? F4 C8 C6 118.0(3) . . ? F4 C8 C9 118.8(3) . . ? C6 C8 C9 123.1(3) . . ? C7 C9 C10 122.8(3) . . ? C7 C9 C8 113.6(3) . . ? C10 C9 C8 123.6(3) . . ? C9 C10 C12 122.8(3) . . ? C9 C10 C11 123.5(3) . . ? C12 C10 C11 113.5(3) . . ? N3 C11 C10 176.3(4) . . ? N4 C12 C10 176.2(4) . . ? N5 C13 C15 178.8(4) . . ? N6 C14 C15 176.5(4) . . ? C16 C15 C13 121.8(3) . . ? C16 C15 C14 124.0(3) . . ? C13 C15 C14 114.1(3) . . ? C17 C16 C15 123.0(3) . . ? C17 C16 C18 113.3(3) . . ? C15 C16 C18 123.7(3) . . ? F5 C17 C19 117.7(3) . . ? F5 C17 C16 118.8(3) . . ? C19 C17 C16 123.5(3) . . ? F6 C18 C20 118.6(3) . . ? F6 C18 C16 118.4(3) . . ? C20 C18 C16 123.0(3) . . ? F7 C19 C17 117.6(3) . . ? F7 C19 C21 119.3(3) . . ? C17 C19 C21 123.1(3) . . ? F8 C20 C18 117.5(3) . . ? F8 C20 C21 119.1(3) . . ? C18 C20 C21 123.3(3) . . ? C20 C21 C19 113.8(3) . . ? C20 C21 C22 123.7(4) . . ? C19 C21 C22 122.5(4) . . ? C21 C22 C23 121.7(4) . . ? C21 C22 C24 123.3(4) . . ? C23 C22 C24 114.9(4) . . ? N7 C23 C22 177.4(5) . . ? N8 C24 C22 176.0(6) . . ? N9 C25 C27 175.5(4) . . ? N10 C26 C27 177.9(4) . . ? C28 C27 C26 122.5(3) . . ? C28 C27 C25 123.8(3) . . ? C26 C27 C25 113.7(3) . . ? C27 C28 C30 123.4(3) . . ? C27 C28 C29 123.5(3) . . ? C30 C28 C29 113.1(3) . . ? F9 C29 C31 118.4(3) . . ? F9 C29 C28 118.3(3) . . ? C31 C29 C28 123.2(3) . . ? F10 C30 C32 117.5(3) . . ? F10 C30 C28 119.0(3) . . ? C32 C30 C28 123.5(3) . . ? F11 C31 C29 117.5(3) . . ? F11 C31 C33 119.1(3) . . ? C29 C31 C33 123.4(3) . . ? F12 C32 C30 117.7(3) . . ? F12 C32 C33 118.7(3) . . ? C30 C32 C33 123.5(3) . . ? C34 C33 C32 123.3(3) . . ? C34 C33 C31 123.4(3) . . ? C32 C33 C31 113.2(3) . . ? C33 C34 C35 122.7(3) . . ? C33 C34 C36 123.7(3) . . ? C35 C34 C36 113.6(3) . . ? N11 C35 C34 177.6(5) . . ? N12 C36 C34 175.3(4) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 5.669 _refine_diff_density_min -1.434 _refine_diff_density_rms 0.125 # Attachment 'LATCNQF4.CIF' data_g:\nazari~1\nazari~1\crysta~1\nl082l~1\latcnqf4 _database_code_depnum_ccdc_archive 'CCDC 749365' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Lanthanum(III) 2,3,5,6-Tetrafluoro-7,7,8,8-Tetracyanoquinodimethane' ; _chemical_name_common ;Lanthanum(iii) 2,3,5,6-Tetrafluoro-7,7,8,8- Tetracyanoquinodimethane' ; _chemical_melting_point ? _chemical_formula_sum 'C36 H20 F12 La N12 O10' _chemical_formula_weight 1147.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.626(5) _cell_length_b 17.548(5) _cell_length_c 18.367(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.710(15) _cell_angle_gamma 90.00 _cell_volume 4362(3) _cell_formula_units_Z 4 _cell_measurement_temperature 383(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2260 _exptl_absorpt_coefficient_mu 1.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7601 _exptl_absorpt_correction_T_max 0.8435 _exptl_absorpt_process_details 'SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 383(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44243 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.31 _reflns_number_total 10298 _reflns_number_gt 8336 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0840P)^2^+18.0043P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10298 _refine_ls_number_parameters 652 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1480 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 15.000 _refine_ls_shift/su_mean 0.025 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 La1 La 0.236641(18) 0.024760(14) 0.088365(13) 0.02139(10) Uani 1 1 d . . . F1 F 0.5552(2) -0.10149(17) 0.15573(15) 0.0325(6) Uani 1 1 d . . . F2 F 0.5554(2) -0.26521(16) 0.36171(15) 0.0313(6) Uani 1 1 d . . . F3 F 0.7470(2) -0.10862(17) 0.16676(17) 0.0371(7) Uani 1 1 d . . . F4 F 0.7485(2) -0.27507(16) 0.37056(16) 0.0341(6) Uani 1 1 d . . . F5 F 0.2830(2) -0.03301(15) 0.34521(15) 0.0339(7) Uani 1 1 d . . . F6 F 0.3830(2) 0.17902(15) 0.49600(15) 0.0326(6) Uani 1 1 d . . . F7 F 0.3309(2) -0.12490(16) 0.45602(15) 0.0357(7) Uani 1 1 d . . . F8 F 0.4373(2) 0.08602(16) 0.60546(15) 0.0330(6) Uani 1 1 d . . . F9 F 0.0398(2) -0.02399(15) 0.36042(15) 0.0323(6) Uani 1 1 d . . . F10 F 0.1718(2) 0.15012(15) 0.54375(15) 0.0321(6) Uani 1 1 d . . . F11 F 0.0796(2) -0.13693(15) 0.45180(15) 0.0349(7) Uani 1 1 d . . . F12 F 0.2134(2) 0.03684(16) 0.63452(15) 0.0317(6) Uani 1 1 d . . . O1 O 0.4103(3) 0.0708(2) 0.1396(2) 0.0382(9) Uani 1 1 d . . . O2 O 0.2548(3) 0.16403(19) 0.0607(2) 0.0367(8) Uani 1 1 d . . . O3 O 0.3542(3) 0.0247(2) -0.0101(2) 0.0432(10) Uani 1 1 d . . . O4 O 0.1211(3) 0.0316(2) -0.0280(2) 0.0352(8) Uani 1 1 d . . . O5 O 0.2267(3) -0.10748(19) 0.0199(2) 0.0331(8) Uani 1 1 d . . . O6 O 0.1357(3) -0.06685(19) 0.1519(2) 0.0324(7) Uani 1 1 d . . . O7 O 0.0743(2) 0.08716(19) 0.11082(18) 0.0296(7) Uani 1 1 d . . . N1 N 0.3427(3) -0.0787(2) 0.1693(2) 0.0295(8) Uani 1 1 d . . . N2 N 0.3278(3) -0.2447(2) 0.3363(2) 0.0347(9) Uani 1 1 d . . . N3 N 0.9645(4) -0.0985(3) 0.2104(3) 0.0521(13) Uani 1 1 d . . . N4 N 0.9727(4) -0.2879(3) 0.3566(3) 0.0587(15) Uani 1 1 d . . . N5 N 0.2429(3) 0.0801(2) 0.2245(2) 0.0306(9) Uani 1 1 d . . . N6 N 0.3233(3) 0.2732(2) 0.3540(2) 0.0332(9) Uani 1 1 d . . . N7 N 0.4258(4) -0.2205(3) 0.5855(3) 0.0412(11) Uani 1 1 d . . . N8 N 0.4726(4) -0.0323(3) 0.7282(3) 0.0428(11) Uani 1 1 d . . . N9 N 0.0179(3) 0.1181(3) 0.2598(2) 0.0364(10) Uani 1 1 d . . . N10 N 0.1179(4) 0.2714(2) 0.4308(3) 0.0390(10) Uani 1 1 d . . . N11 N 0.1659(4) -0.2588(3) 0.5585(3) 0.0414(11) Uani 1 1 d . . . N12 N 0.2353(4) -0.1055(3) 0.7347(2) 0.0428(11) Uani 1 1 d . . . C1 C 0.3877(4) -0.1206(3) 0.2073(3) 0.0288(10) Uani 1 1 d . . . C2 C 0.3812(4) -0.2136(3) 0.3011(3) 0.0294(10) Uani 1 1 d . . . C3 C 0.4402(4) -0.1737(3) 0.2555(3) 0.0260(9) Uani 1 1 d . . . C4 C 0.5446(3) -0.1823(2) 0.2585(2) 0.0243(9) Uani 1 1 d . . . C5 C 0.6017(3) -0.1437(3) 0.2107(2) 0.0251(9) Uani 1 1 d . . . C6 C 0.6015(4) -0.2276(3) 0.3115(2) 0.0254(9) Uani 1 1 d . . . C7 C 0.7016(4) -0.1478(3) 0.2160(3) 0.0282(10) Uani 1 1 d . . . C8 C 0.7017(4) -0.2325(3) 0.3167(3) 0.0285(10) Uani 1 1 d . . . C9 C 0.7585(4) -0.1921(3) 0.2693(3) 0.0295(10) Uani 1 1 d . . . C10 C 0.8634(4) -0.1943(3) 0.2755(3) 0.0345(11) Uani 1 1 d . . . C11 C 0.9175(4) -0.1418(3) 0.2382(3) 0.0380(12) Uani 1 1 d . . . C12 C 0.9208(4) -0.2472(3) 0.3218(4) 0.0435(13) Uani 1 1 d . . . C13 C 0.2709(3) 0.0994(3) 0.2828(3) 0.0252(9) Uani 1 1 d . . . C14 C 0.3168(3) 0.2080(3) 0.3565(2) 0.0263(9) Uani 1 1 d . . . C15 C 0.3041(3) 0.1272(3) 0.3543(2) 0.0246(9) Uani 1 1 d . . . C16 C 0.3321(3) 0.0777(3) 0.4142(2) 0.0220(8) Uani 1 1 d . . . C17 C 0.3217(4) -0.0024(3) 0.4091(2) 0.0254(9) Uani 1 1 d . . . C18 C 0.3712(3) 0.1039(2) 0.4847(2) 0.0243(9) Uani 1 1 d . . . C19 C 0.3471(4) -0.0502(3) 0.4668(3) 0.0265(9) Uani 1 1 d . . . C20 C 0.3982(3) 0.0558(3) 0.5419(2) 0.0246(9) Uani 1 1 d . . . C21 C 0.3874(3) -0.0242(2) 0.5372(2) 0.0235(9) Uani 1 1 d . . . C22 C 0.4126(3) -0.0748(3) 0.5967(2) 0.0274(9) Uani 1 1 d . . . C23 C 0.4182(4) -0.1555(3) 0.5889(3) 0.0315(10) Uani 1 1 d . . . C24 C 0.4452(4) -0.0488(3) 0.6689(3) 0.0321(10) Uani 1 1 d . . . C25 C 0.0474(4) 0.1209(3) 0.3210(3) 0.0290(10) Uani 1 1 d . . . C26 C 0.1042(4) 0.2080(3) 0.4163(3) 0.0319(10) Uani 1 1 d . . . C27 C 0.0874(3) 0.1308(3) 0.3957(3) 0.0267(9) Uani 1 1 d . . . C28 C 0.1052(3) 0.0696(3) 0.4459(2) 0.0242(9) Uani 1 1 d . . . C29 C 0.0843(4) -0.0080(3) 0.4274(3) 0.0267(9) Uani 1 1 d . . . C30 C 0.1481(3) 0.0794(3) 0.5190(2) 0.0249(9) Uani 1 1 d . . . C31 C 0.1051(4) -0.0669(2) 0.4752(3) 0.0258(9) Uani 1 1 d . . . C32 C 0.1697(3) 0.0210(2) 0.5670(2) 0.0226(9) Uani 1 1 d . . . C33 C 0.1511(3) -0.0570(3) 0.5482(2) 0.0253(9) Uani 1 1 d . . . C34 C 0.1764(4) -0.1179(3) 0.5968(3) 0.0282(10) Uani 1 1 d . . . C35 C 0.1694(4) -0.1953(3) 0.5739(3) 0.0311(10) Uani 1 1 d . . . C36 C 0.2098(4) -0.1082(3) 0.6724(3) 0.0307(10) Uani 1 1 d . . . O1S O 0.5232(4) 0.1141(3) 0.0103(3) 0.0592(13) Uani 1 1 d . . . O2S O 0.2172(13) -0.0560(4) -0.1201(4) 0.193(7) Uani 1 1 d . . . O3S O -0.0099(3) 0.1488(2) -0.0174(2) 0.0361(8) Uani 1 1 d . . . H2SA H 0.150(3) -0.075(3) -0.133(3) 0.000(10) Uiso 1 1 d . . . H4WA H 0.077(5) 0.074(4) -0.034(3) 0.043(17) Uiso 1 1 d . . . H5WA H 0.220(6) -0.113(5) -0.024(5) 0.07(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.02501(15) 0.01812(14) 0.02042(14) 0.00005(9) -0.00001(10) -0.00066(9) F1 0.0319(15) 0.0353(15) 0.0300(14) 0.0120(12) 0.0021(12) 0.0012(12) F2 0.0397(16) 0.0257(14) 0.0279(14) 0.0073(11) 0.0014(12) -0.0027(11) F3 0.0325(15) 0.0370(16) 0.0429(17) 0.0095(13) 0.0096(13) -0.0006(12) F4 0.0392(16) 0.0253(14) 0.0349(15) 0.0017(11) -0.0079(12) 0.0064(12) F5 0.0532(19) 0.0250(14) 0.0211(13) -0.0037(10) -0.0057(12) -0.0019(12) F6 0.0481(17) 0.0215(13) 0.0272(14) -0.0039(11) 0.0005(12) -0.0060(12) F7 0.0566(19) 0.0206(13) 0.0284(14) -0.0020(11) -0.0016(13) 0.0004(12) F8 0.0430(17) 0.0317(15) 0.0223(13) -0.0045(11) -0.0051(12) -0.0041(12) F9 0.0443(17) 0.0275(14) 0.0232(13) -0.0010(10) -0.0042(12) -0.0030(12) F10 0.0462(17) 0.0188(13) 0.0308(14) -0.0040(11) 0.0019(12) -0.0023(11) F11 0.0526(18) 0.0196(13) 0.0305(15) -0.0009(11) -0.0035(13) -0.0068(12) F12 0.0402(16) 0.0307(15) 0.0227(13) -0.0035(11) -0.0021(12) -0.0016(12) O1 0.0331(19) 0.044(2) 0.0346(19) 0.0119(16) -0.0071(15) -0.0165(16) O2 0.050(2) 0.0208(17) 0.041(2) 0.0041(14) 0.0141(17) -0.0006(15) O3 0.044(2) 0.052(3) 0.035(2) -0.0051(17) 0.0138(17) -0.0163(18) O4 0.039(2) 0.037(2) 0.0264(18) -0.0056(14) -0.0094(15) 0.0092(16) O5 0.047(2) 0.0201(16) 0.0329(19) -0.0042(14) 0.0057(16) -0.0026(14) O6 0.0324(18) 0.0239(17) 0.042(2) 0.0020(14) 0.0081(15) -0.0037(14) O7 0.0300(17) 0.0297(17) 0.0283(17) -0.0004(13) 0.0003(13) 0.0049(13) N1 0.027(2) 0.025(2) 0.036(2) 0.0040(17) -0.0017(17) 0.0030(16) N2 0.040(2) 0.026(2) 0.039(2) 0.0033(18) 0.0103(19) 0.0015(18) N3 0.034(3) 0.060(3) 0.063(3) -0.004(3) 0.011(2) -0.005(2) N4 0.048(3) 0.051(3) 0.073(4) -0.011(3) -0.014(3) 0.020(3) N5 0.040(2) 0.026(2) 0.025(2) -0.0023(16) 0.0018(17) 0.0032(17) N6 0.040(2) 0.024(2) 0.035(2) -0.0035(16) -0.0006(18) 0.0002(17) N7 0.048(3) 0.034(3) 0.041(3) 0.0030(19) 0.001(2) 0.011(2) N8 0.052(3) 0.045(3) 0.028(2) 0.0029(19) -0.012(2) -0.003(2) N9 0.043(3) 0.035(2) 0.031(2) 0.0077(18) 0.0030(19) 0.0028(19) N10 0.057(3) 0.023(2) 0.039(2) 0.0015(18) 0.013(2) 0.0016(19) N11 0.061(3) 0.026(2) 0.038(2) 0.0017(18) 0.011(2) 0.006(2) N12 0.058(3) 0.042(3) 0.029(2) 0.0057(19) 0.005(2) 0.006(2) C1 0.031(2) 0.023(2) 0.032(2) -0.0034(19) 0.004(2) -0.0051(19) C2 0.035(3) 0.024(2) 0.029(2) -0.0040(18) 0.002(2) 0.0022(19) C3 0.032(2) 0.019(2) 0.027(2) 0.0016(17) 0.0007(18) 0.0003(17) C4 0.026(2) 0.020(2) 0.027(2) -0.0021(16) 0.0026(18) 0.0007(16) C5 0.030(2) 0.022(2) 0.023(2) 0.0028(16) 0.0003(18) 0.0022(17) C6 0.034(2) 0.020(2) 0.023(2) -0.0022(16) 0.0036(18) -0.0009(17) C7 0.034(2) 0.024(2) 0.028(2) -0.0004(18) 0.0076(19) -0.0015(18) C8 0.037(3) 0.019(2) 0.028(2) 0.0003(17) -0.0037(19) 0.0028(18) C9 0.027(2) 0.026(2) 0.034(3) -0.0067(19) 0.0012(19) 0.0023(18) C10 0.031(3) 0.032(3) 0.039(3) -0.008(2) -0.001(2) 0.001(2) C11 0.026(3) 0.040(3) 0.048(3) -0.009(2) 0.004(2) 0.003(2) C12 0.035(3) 0.037(3) 0.057(4) -0.010(3) -0.002(3) 0.010(2) C13 0.024(2) 0.023(2) 0.028(2) 0.0019(17) 0.0026(18) 0.0041(17) C14 0.028(2) 0.027(2) 0.022(2) 0.0000(17) -0.0018(17) -0.0019(18) C15 0.027(2) 0.023(2) 0.024(2) -0.0029(17) 0.0028(17) 0.0000(17) C16 0.023(2) 0.026(2) 0.0177(19) -0.0022(16) 0.0021(16) -0.0013(16) C17 0.030(2) 0.027(2) 0.018(2) -0.0047(17) -0.0010(17) -0.0010(18) C18 0.027(2) 0.020(2) 0.026(2) -0.0039(16) 0.0038(18) -0.0049(16) C19 0.033(2) 0.019(2) 0.027(2) -0.0022(17) 0.0047(19) 0.0027(18) C20 0.025(2) 0.027(2) 0.022(2) -0.0047(17) -0.0004(17) 0.0005(17) C21 0.022(2) 0.026(2) 0.022(2) -0.0011(16) 0.0027(17) 0.0009(16) C22 0.026(2) 0.031(2) 0.024(2) 0.0016(18) 0.0004(18) 0.0047(18) C23 0.031(3) 0.035(3) 0.028(2) 0.0055(19) 0.0017(19) 0.008(2) C24 0.035(3) 0.031(2) 0.030(3) 0.0039(19) -0.002(2) 0.001(2) C25 0.030(2) 0.025(2) 0.033(3) 0.0025(18) 0.006(2) 0.0045(18) C26 0.036(3) 0.031(3) 0.029(2) 0.005(2) 0.008(2) 0.005(2) C27 0.028(2) 0.023(2) 0.030(2) 0.0023(18) 0.0069(18) 0.0039(17) C28 0.025(2) 0.021(2) 0.027(2) 0.0015(17) 0.0082(17) 0.0013(17) C29 0.027(2) 0.030(2) 0.022(2) -0.0021(18) 0.0015(18) -0.0034(18) C30 0.029(2) 0.020(2) 0.026(2) -0.0008(17) 0.0055(18) -0.0012(17) C31 0.033(2) 0.018(2) 0.027(2) -0.0036(17) 0.0067(18) -0.0020(17) C32 0.022(2) 0.027(2) 0.019(2) -0.0002(16) 0.0015(16) 0.0017(16) C33 0.028(2) 0.026(2) 0.022(2) -0.0023(17) 0.0050(17) 0.0013(18) C34 0.034(2) 0.025(2) 0.026(2) 0.0015(18) 0.0045(19) 0.0020(18) C35 0.039(3) 0.027(3) 0.029(2) 0.0070(19) 0.009(2) 0.003(2) C36 0.037(3) 0.026(2) 0.030(3) 0.0020(19) 0.010(2) 0.0009(19) O1S 0.055(3) 0.065(3) 0.056(3) 0.018(2) 0.003(2) -0.024(2) O2S 0.49(2) 0.047(4) 0.047(4) 0.002(3) 0.049(8) 0.039(8) O3S 0.040(2) 0.0304(18) 0.0346(19) 0.0013(14) -0.0090(16) 0.0032(15) _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 La1 O6 2.492(3) . ? La1 O4 2.505(4) . ? La1 O2 2.514(3) . ? La1 O7 2.544(3) . ? La1 O3 2.552(4) . ? La1 O1 2.572(3) . ? La1 O5 2.635(3) . ? La1 N1 2.662(4) . ? La1 N5 2.675(4) . ? F1 C5 1.350(5) . ? F2 C6 1.348(5) . ? F3 C7 1.343(5) . ? F4 C8 1.340(5) . ? F5 C17 1.341(5) . ? F6 C18 1.341(5) . ? F7 C19 1.339(5) . ? F8 C20 1.334(5) . ? F9 C29 1.336(5) . ? F10 C30 1.348(5) . ? F11 C31 1.335(5) . ? F12 C32 1.341(5) . ? N1 C1 1.142(6) . ? N2 C2 1.164(7) . ? N3 C11 1.152(8) . ? N4 C12 1.146(8) . ? N5 C13 1.145(6) . ? N6 C14 1.150(6) . ? N7 C23 1.149(7) . ? N8 C24 1.147(7) . ? N9 C25 1.151(7) . ? N10 C26 1.154(7) . ? N11 C35 1.150(7) . ? N12 C36 1.156(7) . ? C1 C3 1.420(7) . ? C2 C3 1.412(7) . ? C3 C4 1.425(7) . ? C4 C5 1.411(6) . ? C4 C6 1.416(6) . ? C5 C7 1.355(7) . ? C6 C8 1.360(7) . ? C7 C9 1.410(7) . ? C8 C9 1.420(7) . ? C9 C10 1.421(7) . ? C10 C11 1.407(8) . ? C10 C12 1.428(8) . ? C13 C15 1.424(6) . ? C14 C15 1.429(6) . ? C15 C16 1.418(6) . ? C16 C17 1.415(6) . ? C16 C18 1.417(6) . ? C17 C19 1.365(7) . ? C18 C20 1.365(6) . ? C19 C21 1.420(6) . ? C20 C21 1.414(6) . ? C21 C22 1.419(6) . ? C22 C24 1.424(7) . ? C22 C23 1.425(7) . ? C25 C27 1.426(7) . ? C26 C27 1.418(7) . ? C27 C28 1.417(6) . ? C28 C30 1.411(6) . ? C28 C29 1.425(7) . ? C29 C31 1.364(7) . ? C30 C32 1.362(6) . ? C31 C33 1.422(6) . ? C32 C33 1.427(6) . ? C33 C34 1.408(6) . ? C34 C36 1.420(7) . ? C34 C35 1.422(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 La1 O4 95.97(13) . . ? O6 La1 O2 142.60(12) . . ? O4 La1 O2 81.26(13) . . ? O6 La1 O7 70.36(11) . . ? O4 La1 O7 69.30(12) . . ? O2 La1 O7 73.90(12) . . ? O6 La1 O3 139.26(12) . . ? O4 La1 O3 77.23(14) . . ? O2 La1 O3 76.84(13) . . ? O7 La1 O3 138.12(13) . . ? O6 La1 O1 124.45(12) . . ? O4 La1 O1 139.17(12) . . ? O2 La1 O1 70.15(13) . . ? O7 La1 O1 125.82(12) . . ? O3 La1 O1 68.47(13) . . ? O6 La1 O5 69.82(12) . . ? O4 La1 O5 69.05(12) . . ? O2 La1 O5 139.48(12) . . ? O7 La1 O5 117.32(12) . . ? O3 La1 O5 70.29(12) . . ? O1 La1 O5 116.43(13) . . ? O6 La1 N1 65.93(12) . . ? O4 La1 N1 139.00(12) . . ? O2 La1 N1 135.69(13) . . ? O7 La1 N1 128.91(12) . . ? O3 La1 N1 92.91(14) . . ? O1 La1 N1 66.05(12) . . ? O5 La1 N1 70.15(13) . . ? O6 La1 N5 75.86(12) . . ? O4 La1 N5 136.78(13) . . ? O2 La1 N5 80.97(12) . . ? O7 La1 N5 68.00(12) . . ? O3 La1 N5 135.14(13) . . ? O1 La1 N5 67.44(13) . . ? O5 La1 N5 139.48(12) . . ? N1 La1 N5 76.69(13) . . ? C1 N1 La1 176.3(4) . . ? C13 N5 La1 162.2(4) . . ? N1 C1 C3 177.8(5) . . ? N2 C2 C3 176.1(5) . . ? C2 C3 C1 114.5(4) . . ? C2 C3 C4 124.0(4) . . ? C1 C3 C4 121.4(4) . . ? C5 C4 C6 113.5(4) . . ? C5 C4 C3 123.1(4) . . ? C6 C4 C3 123.3(4) . . ? F1 C5 C7 117.5(4) . . ? F1 C5 C4 118.9(4) . . ? C7 C5 C4 123.5(4) . . ? F2 C6 C8 117.7(4) . . ? F2 C6 C4 119.0(4) . . ? C8 C6 C4 123.2(4) . . ? F3 C7 C5 117.6(4) . . ? F3 C7 C9 119.4(4) . . ? C5 C7 C9 123.0(4) . . ? F4 C8 C6 118.3(4) . . ? F4 C8 C9 119.0(4) . . ? C6 C8 C9 122.7(4) . . ? C7 C9 C8 114.0(4) . . ? C7 C9 C10 122.5(5) . . ? C8 C9 C10 123.5(5) . . ? C11 C10 C9 121.5(5) . . ? C11 C10 C12 115.7(5) . . ? C9 C10 C12 122.8(5) . . ? N3 C11 C10 177.0(6) . . ? N4 C12 C10 175.0(7) . . ? N5 C13 C15 177.1(5) . . ? N6 C14 C15 175.6(5) . . ? C16 C15 C13 122.2(4) . . ? C16 C15 C14 124.4(4) . . ? C13 C15 C14 112.9(4) . . ? C17 C16 C15 122.7(4) . . ? C17 C16 C18 114.0(4) . . ? C15 C16 C18 123.2(4) . . ? F5 C17 C19 118.1(4) . . ? F5 C17 C16 118.8(4) . . ? C19 C17 C16 123.0(4) . . ? F6 C18 C20 118.1(4) . . ? F6 C18 C16 119.1(4) . . ? C20 C18 C16 122.8(4) . . ? F7 C19 C17 117.6(4) . . ? F7 C19 C21 119.3(4) . . ? C17 C19 C21 123.1(4) . . ? F8 C20 C18 118.2(4) . . ? F8 C20 C21 118.5(4) . . ? C18 C20 C21 123.3(4) . . ? C20 C21 C22 124.1(4) . . ? C20 C21 C19 113.7(4) . . ? C22 C21 C19 122.2(4) . . ? C21 C22 C24 122.6(4) . . ? C21 C22 C23 123.7(4) . . ? C24 C22 C23 113.4(4) . . ? N7 C23 C22 176.8(6) . . ? N8 C24 C22 175.9(6) . . ? N9 C25 C27 174.9(5) . . ? N10 C26 C27 177.8(5) . . ? C28 C27 C26 122.7(4) . . ? C28 C27 C25 123.4(4) . . ? C26 C27 C25 113.9(4) . . ? C30 C28 C27 123.2(4) . . ? C30 C28 C29 113.1(4) . . ? C27 C28 C29 123.7(4) . . ? F9 C29 C31 118.2(4) . . ? F9 C29 C28 118.5(4) . . ? C31 C29 C28 123.4(4) . . ? F10 C30 C32 116.7(4) . . ? F10 C30 C28 119.3(4) . . ? C32 C30 C28 124.0(4) . . ? F11 C31 C29 117.6(4) . . ? F11 C31 C33 119.0(4) . . ? C29 C31 C33 123.4(4) . . ? F12 C32 C30 118.8(4) . . ? F12 C32 C33 118.0(4) . . ? C30 C32 C33 123.1(4) . . ? C34 C33 C31 123.6(4) . . ? C34 C33 C32 123.4(4) . . ? C31 C33 C32 113.0(4) . . ? C33 C34 C36 123.8(4) . . ? C33 C34 C35 122.2(4) . . ? C36 C34 C35 114.0(4) . . ? N11 C35 C34 176.8(6) . . ? N12 C36 C34 175.3(5) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 3.199 _refine_diff_density_min -1.200 _refine_diff_density_rms 0.172 # Attachment 'NDTCNQF4.CIF' data_g:\nazari~1\nazari~1\crysta~1\nl084n~1\ndtcnqf4 _database_code_depnum_ccdc_archive 'CCDC 749366' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Neodymium(III) 2,3,5,6-Tetrafluoro-7,7,8,8-Tetracyanoquinodimethane' ; _chemical_name_common ;Neodymium(iii) 2,3,5,6-Tetrafluoro-7,7,8,8- Tetracyanoquinodimethane' ; _chemical_melting_point ? _chemical_formula_sum 'C36 H20 F12 N12 Nd O10' _chemical_formula_weight 1152.88 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' 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.552(7) _cell_length_b 17.434(11) _cell_length_c 18.296(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.83(2) _cell_angle_gamma 90.00 _cell_volume 4292(4) _cell_formula_units_Z 4 _cell_measurement_temperature 383(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 1.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6793 _exptl_absorpt_correction_T_max 0.8251 _exptl_absorpt_process_details 'SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 383(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40335 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.39 _reflns_number_total 10301 _reflns_number_gt 8402 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0456P)^2^+33.3924P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10301 _refine_ls_number_parameters 687 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1507 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 15.000 _refine_ls_shift/su_mean 0.036 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 0.23791(2) 0.524222(15) 0.088870(15) 0.01286(9) Uani 1 1 d . . . F1 F 0.5549(3) 0.4001(2) 0.15452(19) 0.0234(7) Uani 1 1 d . . . F2 F 0.5563(3) 0.23531(18) 0.36095(18) 0.0225(7) Uani 1 1 d . . . F3 F 0.7472(3) 0.3935(2) 0.1658(2) 0.0298(8) Uani 1 1 d . . . F4 F 0.7504(3) 0.22571(19) 0.3698(2) 0.0276(8) Uani 1 1 d . . . F5 F 0.2827(3) 0.46449(17) 0.34470(18) 0.0241(8) Uani 1 1 d . . . F6 F 0.3822(3) 0.67919(18) 0.49484(18) 0.0214(7) Uani 1 1 d . . . F7 F 0.3314(3) 0.37318(18) 0.45613(19) 0.0249(8) Uani 1 1 d . . . F8 F 0.4375(3) 0.58676(18) 0.60506(18) 0.0228(7) Uani 1 1 d . . . F9 F 0.0389(3) 0.47452(19) 0.35988(18) 0.0260(8) Uani 1 1 d . . . F10 F 0.1713(3) 0.65025(18) 0.54342(19) 0.0229(7) Uani 1 1 d . . . F11 F 0.0799(3) 0.36112(18) 0.45165(19) 0.0248(8) Uani 1 1 d . . . F12 F 0.2138(3) 0.53703(18) 0.63452(18) 0.0228(7) Uani 1 1 d . . . O1 O 0.2282(4) 0.3947(2) 0.0207(2) 0.0271(10) Uani 1 1 d . . . O2 O 0.3515(4) 0.5250(3) -0.0078(3) 0.0386(12) Uani 1 1 d . . . O3 O 0.1247(4) 0.5308(3) -0.0241(3) 0.0288(11) Uani 1 1 d . . . O4 O 0.2550(4) 0.6610(2) 0.0629(3) 0.0277(10) Uani 1 1 d . . . O5 O 0.0788(3) 0.5850(3) 0.1107(3) 0.0223(9) Uani 1 1 d . . . O6 O 0.4084(4) 0.5698(3) 0.1383(3) 0.0313(11) Uani 1 1 d . . . O7 O 0.1371(3) 0.4346(3) 0.1492(3) 0.0244(10) Uani 1 1 d . . . N1 N 0.3424(4) 0.4233(3) 0.1684(3) 0.0209(10) Uani 1 1 d . . . N2 N 0.3290(4) 0.2545(3) 0.3344(3) 0.0281(12) Uani 1 1 d . . . N3 N 0.9654(4) 0.4033(4) 0.2079(4) 0.0459(17) Uani 1 1 d . . . N4 N 0.9750(5) 0.2125(4) 0.3550(4) 0.052(2) Uani 1 1 d . . . N5 N 0.2445(4) 0.5780(3) 0.2226(3) 0.0204(10) Uani 1 1 d . . . N6 N 0.3215(4) 0.7728(3) 0.3523(3) 0.0241(11) Uani 1 1 d . . . N7 N 0.4264(4) 0.2780(3) 0.5860(3) 0.0318(13) Uani 1 1 d . . . N8 N 0.4726(5) 0.4674(3) 0.7285(3) 0.0356(14) Uani 1 1 d . . . N9 N 0.0177(4) 0.6165(3) 0.2583(3) 0.0278(12) Uani 1 1 d . . . N10 N 0.1151(5) 0.7715(3) 0.4304(3) 0.0311(13) Uani 1 1 d . . . N11 N 0.1690(5) 0.2394(3) 0.5587(3) 0.0321(13) Uani 1 1 d . . . N12 N 0.2370(5) 0.3944(3) 0.7349(3) 0.0338(13) Uani 1 1 d . . . C1 C 0.3875(4) 0.3801(3) 0.2064(3) 0.0162(11) Uani 1 1 d . . . C2 C 0.3810(4) 0.2860(3) 0.3004(3) 0.0188(12) Uani 1 1 d . . . C3 C 0.4402(4) 0.3270(3) 0.2546(3) 0.0170(11) Uani 1 1 d . . . C4 C 0.5448(4) 0.3189(3) 0.2579(3) 0.0176(11) Uani 1 1 d . . . C5 C 0.6014(4) 0.3576(3) 0.2098(3) 0.0194(12) Uani 1 1 d . . . C6 C 0.6023(4) 0.2728(3) 0.3108(3) 0.0176(11) Uani 1 1 d . . . C7 C 0.7010(4) 0.3541(3) 0.2156(3) 0.0195(12) Uani 1 1 d . . . C8 C 0.7024(4) 0.2688(3) 0.3158(3) 0.0196(12) Uani 1 1 d . . . C9 C 0.7590(4) 0.3089(3) 0.2683(3) 0.0214(12) Uani 1 1 d . . . C10 C 0.8640(5) 0.3070(4) 0.2745(4) 0.0269(14) Uani 1 1 d . . . C11 C 0.9196(5) 0.3595(4) 0.2368(4) 0.0321(15) Uani 1 1 d . . . C12 C 0.9230(5) 0.2540(4) 0.3200(4) 0.0356(17) Uani 1 1 d . . . C13 C 0.2707(4) 0.5982(3) 0.2810(3) 0.0168(11) Uani 1 1 d . . . C14 C 0.3152(4) 0.7079(3) 0.3550(3) 0.0180(11) Uani 1 1 d . . . C15 C 0.3034(4) 0.6260(3) 0.3525(3) 0.0147(10) Uani 1 1 d . . . C16 C 0.3314(4) 0.5776(3) 0.4131(3) 0.0137(10) Uani 1 1 d . . . C17 C 0.3217(4) 0.4964(3) 0.4085(3) 0.0164(11) Uani 1 1 d . . . C18 C 0.3703(4) 0.6032(3) 0.4838(3) 0.0158(11) Uani 1 1 d . . . C19 C 0.3469(4) 0.4489(3) 0.4660(3) 0.0169(11) Uani 1 1 d . . . C20 C 0.3978(4) 0.5556(3) 0.5410(3) 0.0166(11) Uani 1 1 d . . . C21 C 0.3872(4) 0.4741(3) 0.5365(3) 0.0158(10) Uani 1 1 d . . . C22 C 0.4136(4) 0.4247(3) 0.5964(3) 0.0173(11) Uani 1 1 d . . . C23 C 0.4182(4) 0.3429(3) 0.5887(3) 0.0202(12) Uani 1 1 d . . . C24 C 0.4461(5) 0.4508(3) 0.6692(4) 0.0240(13) Uani 1 1 d . . . C25 C 0.0470(4) 0.6206(3) 0.3196(3) 0.0208(12) Uani 1 1 d . . . C26 C 0.1021(5) 0.7085(3) 0.4163(3) 0.0229(13) Uani 1 1 d . . . C27 C 0.0862(4) 0.6300(3) 0.3951(3) 0.0188(11) Uani 1 1 d . . . C28 C 0.1055(4) 0.5692(3) 0.4455(3) 0.0157(11) Uani 1 1 d . . . C29 C 0.0840(4) 0.4912(3) 0.4269(3) 0.0161(11) Uani 1 1 d . . . C30 C 0.1479(4) 0.5787(3) 0.5193(3) 0.0167(11) Uani 1 1 d . . . C31 C 0.1054(4) 0.4320(3) 0.4751(3) 0.0168(11) Uani 1 1 d . . . C32 C 0.1699(4) 0.5202(3) 0.5670(3) 0.0168(11) Uani 1 1 d . . . C33 C 0.1514(4) 0.4423(3) 0.5481(3) 0.0141(10) Uani 1 1 d . . . C34 C 0.1776(4) 0.3812(3) 0.5970(3) 0.0181(11) Uani 1 1 d . . . C35 C 0.1713(5) 0.3029(3) 0.5743(3) 0.0220(12) Uani 1 1 d . . . C36 C 0.2113(5) 0.3906(3) 0.6728(3) 0.0217(12) Uani 1 1 d . . . H1A H 0.268(5) 0.361(4) 0.031(4) 0.026 Uiso 1 1 d . . . H2A H 0.397(5) 0.567(4) -0.011(4) 0.017(16) Uiso 1 1 d . . . H3A H 0.133(6) 0.513(4) -0.053(4) 0.021 Uiso 1 1 d . . . H4A H 0.269(5) 0.683(4) 0.026(4) 0.021 Uiso 1 1 d . . . H5A H 0.051(5) 0.605(4) 0.085(4) 0.021 Uiso 1 1 d . . . H6A H 0.445(5) 0.551(4) 0.174(4) 0.022(18) Uiso 1 1 d . . . H7A H 0.143(8) 0.394(6) 0.145(6) 0.06(3) Uiso 1 1 d . . . H2B H 0.323(6) 0.569(4) -0.025(4) 0.024(19) Uiso 1 1 d . . . H3B H 0.068(7) 0.561(5) -0.036(5) 0.05(2) Uiso 1 1 d . . . H4B H 0.240(7) 0.696(6) 0.090(5) 0.061 Uiso 1 1 d . . . H5B H 0.077(7) 0.595(6) 0.150(6) 0.061 Uiso 1 1 d . . . H6B H 0.427(7) 0.612(6) 0.136(5) 0.06(3) Uiso 1 1 d . . . H7B H 0.073(12) 0.443(9) 0.162(8) 0.14(6) Uiso 1 1 d . . . O1S O 0.5253(5) 0.6115(4) 0.0110(4) 0.0549(16) Uiso 1 1 d . . . O2S O 0.1607(7) 0.4315(5) -0.1285(5) 0.088(2) Uiso 1 1 d . . . O3S O 0.0093(5) 0.3526(3) 0.0165(3) 0.0270(11) Uiso 1 1 d . . . H1WA H 0.493(4) 0.645(3) 0.022(3) 0.000(12) Uiso 1 1 d . . . H2WA H 0.239(4) 0.445(3) -0.118(3) 0.000(12) Uiso 1 1 d . . . H3WA H -0.020(4) 0.362(3) 0.038(3) 0.000(14) Uiso 1 1 d . . . H3WB H 0.063(9) 0.350(7) 0.018(6) 0.09(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.01681(15) 0.00902(13) 0.01210(14) -0.00009(11) -0.00090(10) -0.00065(11) F1 0.0224(18) 0.0255(18) 0.0225(18) 0.0093(14) 0.0033(14) 0.0050(14) F2 0.0292(19) 0.0169(16) 0.0202(17) 0.0037(13) -0.0019(14) 0.0012(14) F3 0.0249(19) 0.030(2) 0.036(2) 0.0061(16) 0.0095(16) -0.0007(15) F4 0.030(2) 0.0196(17) 0.030(2) 0.0003(15) -0.0115(16) 0.0065(14) F5 0.043(2) 0.0110(15) 0.0158(17) -0.0043(12) -0.0050(15) -0.0020(14) F6 0.0315(19) 0.0135(15) 0.0177(17) -0.0032(12) -0.0030(14) -0.0073(13) F7 0.045(2) 0.0088(15) 0.0199(18) -0.0025(13) -0.0012(16) 0.0019(14) F8 0.033(2) 0.0182(16) 0.0154(16) -0.0040(13) -0.0068(14) -0.0029(14) F9 0.038(2) 0.0210(17) 0.0172(17) -0.0006(14) -0.0053(15) -0.0053(15) F10 0.0315(19) 0.0121(15) 0.0248(18) -0.0037(13) 0.0013(15) -0.0012(13) F11 0.037(2) 0.0126(15) 0.0234(18) -0.0033(13) -0.0016(15) -0.0079(14) F12 0.034(2) 0.0169(16) 0.0169(17) -0.0056(13) -0.0017(14) -0.0007(14) O1 0.040(3) 0.014(2) 0.027(2) -0.0014(17) 0.004(2) 0.0045(18) O2 0.036(3) 0.046(3) 0.036(3) -0.002(3) 0.014(2) -0.015(3) O3 0.035(3) 0.032(3) 0.018(2) -0.0103(19) -0.006(2) 0.010(2) O4 0.043(3) 0.013(2) 0.029(3) 0.0018(18) 0.014(2) -0.0001(19) O5 0.026(2) 0.021(2) 0.018(2) 0.0027(17) -0.0040(19) 0.0085(17) O6 0.024(2) 0.037(3) 0.029(3) 0.015(2) -0.013(2) -0.017(2) O7 0.022(2) 0.013(2) 0.039(3) 0.0046(18) 0.0074(19) 0.0017(17) N1 0.016(2) 0.015(2) 0.031(3) 0.002(2) 0.001(2) -0.0004(18) N2 0.035(3) 0.020(3) 0.030(3) 0.003(2) 0.009(2) 0.000(2) N3 0.019(3) 0.057(4) 0.063(5) -0.012(4) 0.010(3) -0.004(3) N4 0.040(4) 0.043(4) 0.069(5) -0.013(3) -0.019(4) 0.020(3) N5 0.029(3) 0.015(2) 0.016(2) 0.0006(18) -0.003(2) 0.001(2) N6 0.029(3) 0.019(3) 0.023(3) -0.001(2) -0.002(2) -0.001(2) N7 0.037(3) 0.025(3) 0.031(3) 0.001(2) -0.003(3) 0.010(2) N8 0.046(4) 0.034(3) 0.024(3) 0.005(2) -0.010(3) 0.000(3) N9 0.033(3) 0.028(3) 0.022(3) 0.006(2) 0.003(2) 0.003(2) N10 0.046(4) 0.015(3) 0.035(3) 0.005(2) 0.015(3) 0.002(2) N11 0.054(4) 0.017(3) 0.027(3) 0.003(2) 0.010(3) 0.007(2) N12 0.048(4) 0.034(3) 0.020(3) 0.006(2) 0.006(3) 0.008(3) C1 0.013(3) 0.014(2) 0.022(3) -0.005(2) 0.006(2) -0.003(2) C2 0.021(3) 0.011(2) 0.023(3) 0.000(2) -0.001(2) 0.003(2) C3 0.021(3) 0.010(2) 0.019(3) 0.000(2) 0.000(2) 0.001(2) C4 0.023(3) 0.011(2) 0.019(3) -0.003(2) 0.003(2) 0.000(2) C5 0.022(3) 0.015(3) 0.021(3) -0.002(2) 0.000(2) 0.003(2) C6 0.026(3) 0.008(2) 0.019(3) -0.004(2) 0.004(2) 0.000(2) C7 0.024(3) 0.016(3) 0.019(3) 0.000(2) 0.004(2) 0.000(2) C8 0.027(3) 0.009(2) 0.021(3) -0.003(2) -0.007(2) 0.005(2) C9 0.020(3) 0.014(3) 0.029(3) -0.009(2) -0.002(2) 0.003(2) C10 0.018(3) 0.025(3) 0.038(4) -0.008(3) 0.002(3) 0.005(2) C11 0.016(3) 0.036(4) 0.044(4) -0.010(3) 0.003(3) 0.003(3) C12 0.028(4) 0.027(3) 0.050(5) -0.014(3) -0.005(3) 0.004(3) C13 0.019(3) 0.011(2) 0.020(3) 0.002(2) 0.001(2) 0.002(2) C14 0.019(3) 0.017(3) 0.017(3) -0.002(2) -0.001(2) 0.000(2) C15 0.018(3) 0.010(2) 0.015(3) -0.0010(19) 0.002(2) 0.001(2) C16 0.014(3) 0.014(2) 0.013(3) -0.0024(19) 0.001(2) -0.0011(19) C17 0.019(3) 0.014(2) 0.016(3) -0.004(2) 0.001(2) -0.001(2) C18 0.015(3) 0.014(2) 0.018(3) -0.004(2) 0.001(2) -0.005(2) C19 0.018(3) 0.013(2) 0.019(3) -0.005(2) 0.000(2) -0.001(2) C20 0.015(3) 0.018(3) 0.017(3) -0.007(2) 0.000(2) -0.002(2) C21 0.015(3) 0.015(2) 0.017(3) 0.001(2) 0.002(2) 0.001(2) C22 0.016(3) 0.019(3) 0.017(3) 0.001(2) -0.001(2) 0.004(2) C23 0.020(3) 0.021(3) 0.018(3) 0.000(2) -0.002(2) 0.005(2) C24 0.024(3) 0.021(3) 0.026(3) 0.003(2) -0.003(3) 0.001(2) C25 0.022(3) 0.015(3) 0.027(3) 0.007(2) 0.007(2) 0.005(2) C26 0.029(3) 0.020(3) 0.022(3) 0.008(2) 0.010(2) 0.005(2) C27 0.021(3) 0.014(3) 0.023(3) 0.003(2) 0.007(2) 0.002(2) C28 0.015(3) 0.012(2) 0.022(3) -0.002(2) 0.009(2) -0.0004(19) C29 0.013(3) 0.019(3) 0.016(3) -0.002(2) -0.001(2) -0.001(2) C30 0.017(3) 0.014(2) 0.019(3) -0.008(2) 0.004(2) -0.003(2) C31 0.018(3) 0.009(2) 0.022(3) -0.003(2) 0.001(2) -0.002(2) C32 0.017(3) 0.017(3) 0.017(3) -0.004(2) 0.003(2) -0.001(2) C33 0.016(3) 0.012(2) 0.015(3) 0.002(2) 0.005(2) 0.0014(19) C34 0.022(3) 0.015(3) 0.018(3) 0.001(2) 0.003(2) 0.001(2) C35 0.028(3) 0.024(3) 0.016(3) 0.006(2) 0.008(2) 0.003(2) C36 0.033(3) 0.013(3) 0.020(3) 0.003(2) 0.007(3) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O3 2.426(5) . ? Nd1 O7 2.426(5) . ? Nd1 O4 2.449(5) . ? Nd1 O5 2.478(5) . ? Nd1 O2 2.479(5) . ? Nd1 O6 2.508(5) . ? Nd1 O1 2.576(4) . ? Nd1 N1 2.593(5) . ? Nd1 N5 2.612(5) . ? F1 C5 1.349(6) . ? F2 C6 1.339(7) . ? F3 C7 1.353(7) . ? F4 C8 1.346(6) . ? F5 C17 1.342(6) . ? F6 C18 1.347(6) . ? F7 C19 1.345(6) . ? F8 C20 1.345(6) . ? F9 C29 1.335(6) . ? F10 C30 1.349(6) . ? F11 C31 1.340(6) . ? F12 C32 1.339(6) . ? N1 C1 1.150(7) . ? N2 C2 1.136(8) . ? N3 C11 1.152(10) . ? N4 C12 1.150(9) . ? N5 C13 1.141(7) . ? N6 C14 1.137(7) . ? N7 C23 1.138(8) . ? N8 C24 1.138(8) . ? N9 C25 1.148(8) . ? N10 C26 1.138(8) . ? N11 C35 1.142(8) . ? N12 C36 1.150(8) . ? C1 C3 1.412(8) . ? C2 C3 1.420(8) . ? C3 C4 1.419(8) . ? C4 C5 1.405(8) . ? C4 C6 1.418(8) . ? C5 C7 1.343(8) . ? C6 C8 1.350(8) . ? C7 C9 1.410(8) . ? C8 C9 1.411(9) . ? C9 C10 1.413(8) . ? C10 C11 1.416(10) . ? C10 C12 1.424(10) . ? C13 C15 1.415(8) . ? C14 C15 1.436(7) . ? C15 C16 1.409(7) . ? C16 C18 1.411(7) . ? C16 C17 1.424(7) . ? C17 C19 1.350(8) . ? C18 C20 1.353(8) . ? C19 C21 1.410(8) . ? C20 C21 1.429(8) . ? C21 C22 1.406(7) . ? C22 C24 1.428(8) . ? C22 C23 1.436(8) . ? C25 C27 1.429(9) . ? C26 C27 1.432(8) . ? C27 C28 1.409(8) . ? C28 C30 1.413(8) . ? C28 C29 1.424(7) . ? C29 C31 1.365(8) . ? C30 C32 1.351(8) . ? C31 C33 1.417(8) . ? C32 C33 1.416(7) . ? C33 C34 1.410(7) . ? C34 C36 1.417(8) . ? C34 C35 1.426(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 O3 Nd1 O7 94.86(18) . . ? O3 Nd1 O4 81.55(17) . . ? O7 Nd1 O4 141.95(17) . . ? O3 Nd1 O5 69.07(16) . . ? O7 Nd1 O5 69.77(16) . . ? O4 Nd1 O5 73.67(16) . . ? O3 Nd1 O2 77.00(19) . . ? O7 Nd1 O2 139.36(18) . . ? O4 Nd1 O2 77.01(18) . . ? O5 Nd1 O2 137.65(18) . . ? O3 Nd1 O6 138.96(17) . . ? O7 Nd1 O6 125.78(16) . . ? O4 Nd1 O6 69.93(17) . . ? O5 Nd1 O6 126.03(17) . . ? O2 Nd1 O6 68.42(18) . . ? O3 Nd1 O1 68.80(16) . . ? O7 Nd1 O1 69.91(16) . . ? O4 Nd1 O1 139.50(16) . . ? O5 Nd1 O1 117.27(16) . . ? O2 Nd1 O1 70.06(17) . . ? O6 Nd1 O1 116.37(18) . . ? O3 Nd1 N1 139.29(16) . . ? O7 Nd1 N1 66.86(16) . . ? O4 Nd1 N1 135.38(16) . . ? O5 Nd1 N1 128.83(16) . . ? O2 Nd1 N1 93.46(19) . . ? O6 Nd1 N1 66.10(16) . . ? O1 Nd1 N1 70.74(16) . . ? O3 Nd1 N5 136.77(16) . . ? O7 Nd1 N5 76.33(16) . . ? O4 Nd1 N5 80.72(16) . . ? O5 Nd1 N5 68.19(15) . . ? O2 Nd1 N5 135.38(17) . . ? O6 Nd1 N5 67.74(17) . . ? O1 Nd1 N5 139.71(14) . . ? N1 Nd1 N5 76.26(16) . . ? C1 N1 Nd1 177.0(5) . . ? C13 N5 Nd1 163.8(5) . . ? N1 C1 C3 178.0(6) . . ? N2 C2 C3 176.1(6) . . ? C1 C3 C4 121.3(5) . . ? C1 C3 C2 114.8(5) . . ? C4 C3 C2 123.8(5) . . ? C5 C4 C6 113.7(5) . . ? C5 C4 C3 122.9(5) . . ? C6 C4 C3 123.4(5) . . ? C7 C5 F1 117.4(5) . . ? C7 C5 C4 123.2(5) . . ? F1 C5 C4 119.5(5) . . ? F2 C6 C8 118.3(5) . . ? F2 C6 C4 118.8(5) . . ? C8 C6 C4 122.8(5) . . ? C5 C7 F3 117.7(5) . . ? C5 C7 C9 123.6(6) . . ? F3 C7 C9 118.6(5) . . ? F4 C8 C6 118.2(5) . . ? F4 C8 C9 118.5(5) . . ? C6 C8 C9 123.3(5) . . ? C8 C9 C7 113.4(5) . . ? C8 C9 C10 123.7(6) . . ? C7 C9 C10 122.8(6) . . ? C9 C10 C11 122.3(6) . . ? C9 C10 C12 123.5(6) . . ? C11 C10 C12 114.1(6) . . ? N3 C11 C10 178.2(8) . . ? N4 C12 C10 176.4(9) . . ? N5 C13 C15 177.9(6) . . ? N6 C14 C15 175.4(6) . . ? C16 C15 C13 123.2(5) . . ? C16 C15 C14 123.4(5) . . ? C13 C15 C14 113.1(5) . . ? C15 C16 C18 124.7(5) . . ? C15 C16 C17 122.3(5) . . ? C18 C16 C17 113.0(5) . . ? F5 C17 C19 117.4(5) . . ? F5 C17 C16 119.2(5) . . ? C19 C17 C16 123.4(5) . . ? F6 C18 C20 118.1(5) . . ? F6 C18 C16 118.3(5) . . ? C20 C18 C16 123.6(5) . . ? F7 C19 C17 118.4(5) . . ? F7 C19 C21 117.7(5) . . ? C17 C19 C21 123.8(5) . . ? F8 C20 C18 118.0(5) . . ? F8 C20 C21 118.6(5) . . ? C18 C20 C21 123.3(5) . . ? C22 C21 C19 123.9(5) . . ? C22 C21 C20 123.3(5) . . ? C19 C21 C20 112.8(5) . . ? C21 C22 C24 123.6(5) . . ? C21 C22 C23 122.8(5) . . ? C24 C22 C23 113.3(5) . . ? N7 C23 C22 175.9(6) . . ? N8 C24 C22 176.1(7) . . ? N9 C25 C27 176.6(6) . . ? N10 C26 C27 177.5(7) . . ? C28 C27 C25 124.4(5) . . ? C28 C27 C26 122.2(5) . . ? C25 C27 C26 113.4(5) . . ? C27 C28 C30 124.1(5) . . ? C27 C28 C29 123.0(5) . . ? C30 C28 C29 112.9(5) . . ? F9 C29 C31 117.9(5) . . ? F9 C29 C28 119.1(5) . . ? C31 C29 C28 123.0(5) . . ? F10 C30 C32 117.5(5) . . ? F10 C30 C28 118.3(5) . . ? C32 C30 C28 124.2(5) . . ? F11 C31 C29 117.6(5) . . ? F11 C31 C33 119.1(5) . . ? C29 C31 C33 123.3(5) . . ? F12 C32 C30 118.0(5) . . ? F12 C32 C33 118.8(5) . . ? C30 C32 C33 123.1(5) . . ? C34 C33 C32 123.0(5) . . ? C34 C33 C31 123.6(5) . . ? C32 C33 C31 113.4(5) . . ? C33 C34 C36 124.2(5) . . ? C33 C34 C35 122.4(5) . . ? C36 C34 C35 113.4(5) . . ? N11 C35 C34 177.2(7) . . ? N12 C36 C34 176.4(6) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 5.281 _refine_diff_density_min -2.214 _refine_diff_density_rms 0.167 # Attachment 'PRTCNQF4.CIF' data_g:\nazari~1\nazari~1\crysta~1\nl079b~1\prtcnqf4 _database_code_depnum_ccdc_archive 'CCDC 749367' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Praseodymium(III) 2,3,5,6-Tetrafluoro-7,7,8,8-Tetracyanoquinodimethane' ; _chemical_name_common ;Praseodymium(iii) 2,3,5,6-Tetrafluoro-7,7,8,8- Tetracyanoquinodimethane' ; _chemical_melting_point ? _chemical_formula_sum 'C36 H20 F12 N12 O10 Pr' _chemical_formula_weight 1149.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.818(15) _cell_length_b 17.65(2) _cell_length_c 18.57(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.10(2) _cell_angle_gamma 90.00 _cell_volume 4496(9) _cell_formula_units_Z 4 _cell_measurement_temperature 383(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2268 _exptl_absorpt_coefficient_mu 1.202 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7573 _exptl_absorpt_correction_T_max 0.8403 _exptl_absorpt_process_details 'SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 383(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24159 _diffrn_reflns_av_R_equivalents 0.1465 _diffrn_reflns_av_sigmaI/netI 0.1960 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.01 _reflns_number_total 10149 _reflns_number_gt 5675 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1313P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10149 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1513 _refine_ls_R_factor_gt 0.0998 _refine_ls_wR_factor_ref 0.2518 _refine_ls_wR_factor_gt 0.2263 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.23698(3) 0.52419(3) 0.08889(3) 0.01667(18) Uani 1 1 d . . . F1 F 0.5535(3) 0.3991(3) 0.1547(3) 0.0276(13) Uani 1 1 d . . . F2 F 0.5550(3) 0.2351(3) 0.3617(3) 0.0248(12) Uani 1 1 d . . . F3 F 0.7457(3) 0.3922(3) 0.1653(3) 0.0308(14) Uani 1 1 d . . . F4 F 0.7490(4) 0.2253(3) 0.3706(3) 0.0290(13) Uani 1 1 d . . . F5 F 0.2834(4) 0.4660(3) 0.3443(3) 0.0291(13) Uani 1 1 d . . . F6 F 0.3826(4) 0.6802(3) 0.4949(3) 0.0270(13) Uani 1 1 d . . . F7 F 0.3311(4) 0.3745(3) 0.4562(3) 0.0291(13) Uani 1 1 d . . . F8 F 0.4372(4) 0.5871(3) 0.6051(3) 0.0273(13) Uani 1 1 d . . . F9 F 0.5797(4) 1.1381(3) -0.0488(3) 0.0307(14) Uani 1 1 d . . . F10 F 0.7136(4) 0.9623(3) 0.1340(3) 0.0272(13) Uani 1 1 d . . . F11 F 0.5390(4) 1.0245(3) -0.1399(3) 0.0308(13) Uani 1 1 d . . . F12 F 0.6709(4) 0.8496(3) 0.0433(3) 0.0281(13) Uani 1 1 d . . . O1 O 0.4089(4) 0.5701(4) 0.1403(4) 0.0345(18) Uani 1 1 d . . . O2 O 0.2558(4) 0.6616(4) 0.0611(4) 0.0283(16) Uani 1 1 d . . . O3 O 0.3534(5) 0.5232(4) -0.0083(4) 0.0345(18) Uani 1 1 d . . . O4 O 0.1241(5) 0.5323(4) -0.0264(4) 0.0331(17) Uani 1 1 d . . . O5 O 0.2274(4) 0.3927(4) 0.0196(4) 0.0303(17) Uani 1 1 d . . . O6 O 0.1366(4) 0.4343(4) 0.1509(4) 0.0259(16) Uani 1 1 d . . . O7 O 0.0758(4) 0.5863(4) 0.1104(4) 0.0279(16) Uani 1 1 d . . . N1 N 0.3415(5) 0.4223(5) 0.1685(5) 0.0257(19) Uani 1 1 d . . . N2 N 0.3272(6) 0.2555(5) 0.3362(5) 0.031(2) Uani 1 1 d . . . N3 N 0.9642(6) 0.4026(6) 0.2087(6) 0.043(3) Uani 1 1 d . . . N4 N 0.9735(6) 0.2114(6) 0.3556(6) 0.046(3) Uani 1 1 d . . . N5 N 0.2434(5) 0.5792(4) 0.2231(5) 0.0245(18) Uani 1 1 d . . . N6 N 0.3226(5) 0.7729(5) 0.3531(5) 0.029(2) Uani 1 1 d . . . N7 N 0.4272(6) 0.2793(5) 0.5854(5) 0.037(2) Uani 1 1 d . . . N8 N 0.4724(7) 0.4679(5) 0.7280(6) 0.041(2) Uani 1 1 d . . . N9 N 0.6687(6) 1.2593(5) 0.0581(5) 0.036(2) Uani 1 1 d . . . N10 N 0.7357(7) 1.1046(5) 0.2348(6) 0.038(2) Uani 1 1 d . . . N11 N 0.5172(6) 0.8833(5) -0.2415(5) 0.028(2) Uani 1 1 d . . . N12 N 0.6168(6) 0.7281(5) -0.0698(5) 0.036(2) Uani 1 1 d . . . C1 C 0.3857(6) 0.3795(6) 0.2067(5) 0.022(2) Uani 1 1 d . . . C2 C 0.3795(6) 0.2854(5) 0.3001(5) 0.020(2) Uani 1 1 d . . . C3 C 0.4387(6) 0.3268(5) 0.2553(5) 0.023(2) Uani 1 1 d . . . C4 C 0.5448(6) 0.3181(5) 0.2575(5) 0.023(2) Uani 1 1 d . . . C5 C 0.6002(6) 0.3570(5) 0.2095(5) 0.021(2) Uani 1 1 d . . . C6 C 0.6004(6) 0.2731(5) 0.3110(5) 0.020(2) Uani 1 1 d . . . C7 C 0.7008(6) 0.3532(5) 0.2155(5) 0.022(2) Uani 1 1 d . . . C8 C 0.7011(6) 0.2678(5) 0.3163(5) 0.023(2) Uani 1 1 d . . . C9 C 0.7575(6) 0.3074(5) 0.2685(5) 0.022(2) Uani 1 1 d . . . C10 C 0.8632(6) 0.3059(5) 0.2757(6) 0.024(2) Uani 1 1 d . . . C11 C 0.9188(6) 0.3589(6) 0.2377(6) 0.028(2) Uani 1 1 d . . . C12 C 0.9212(7) 0.2528(6) 0.3208(7) 0.038(3) Uani 1 1 d . . . C13 C 0.2700(6) 0.5996(5) 0.2823(6) 0.024(2) Uani 1 1 d . . . C14 C 0.3157(5) 0.7077(5) 0.3557(5) 0.0177(19) Uani 1 1 d . . . C15 C 0.3040(6) 0.6276(5) 0.3527(5) 0.019(2) Uani 1 1 d . . . C16 C 0.3321(6) 0.5786(5) 0.4138(5) 0.022(2) Uani 1 1 d . . . C17 C 0.3214(6) 0.4980(5) 0.4093(5) 0.020(2) Uani 1 1 d . . . C18 C 0.3708(6) 0.6040(5) 0.4837(5) 0.020(2) Uani 1 1 d . . . C19 C 0.3469(6) 0.4503(5) 0.4663(5) 0.021(2) Uani 1 1 d . . . C20 C 0.3979(6) 0.5564(5) 0.5412(5) 0.0185(19) Uani 1 1 d . . . C21 C 0.3875(6) 0.4748(5) 0.5371(5) 0.021(2) Uani 1 1 d . . . C22 C 0.4136(6) 0.4258(5) 0.5961(5) 0.021(2) Uani 1 1 d . . . C23 C 0.4186(6) 0.3441(6) 0.5895(6) 0.025(2) Uani 1 1 d . . . C24 C 0.4458(6) 0.4521(6) 0.6691(7) 0.026(2) Uani 1 1 d . . . C25 C 0.6717(6) 1.1960(6) 0.0745(5) 0.026(2) Uani 1 1 d . . . C26 C 0.7118(7) 1.1081(5) 0.1721(6) 0.027(2) Uani 1 1 d . . . C27 C 0.6773(6) 1.1178(6) 0.0969(6) 0.027(2) Uani 1 1 d . . . C28 C 0.6509(6) 1.0570(5) 0.0471(5) 0.019(2) Uani 1 1 d . . . C29 C 0.6059(6) 1.0667(5) -0.0243(5) 0.021(2) Uani 1 1 d . . . C30 C 0.6696(6) 0.9783(5) 0.0672(6) 0.022(2) Uani 1 1 d . . . C31 C 0.5833(6) 1.0082(5) -0.0725(5) 0.019(2) Uani 1 1 d . . . C32 C 0.6481(6) 0.9214(5) 0.0194(5) 0.023(2) Uani 1 1 d . . . C33 C 0.6052(5) 0.9299(5) -0.0534(5) 0.0176(19) Uani 1 1 d . . . C34 C 0.5869(6) 0.8700(5) -0.1047(5) 0.023(2) Uani 1 1 d . . . C35 C 0.5484(6) 0.8791(5) -0.1800(6) 0.023(2) Uani 1 1 d . . . C36 C 0.6025(6) 0.7921(6) -0.0844(5) 0.024(2) Uani 1 1 d . . . O1S O 0.5244(5) 0.6127(5) 0.0109(5) 0.048(2) Uani 1 1 d . . . O2S O 0.8031(16) 0.5609(6) 0.1224(6) 0.177(9) Uani 1 1 d . . . O3S O 0.0091(4) 0.3522(4) 0.0170(4) 0.0278(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.0105(2) 0.0122(3) 0.0286(3) 0.0000(2) 0.00725(19) -0.00095(18) F1 0.021(3) 0.026(3) 0.038(3) 0.009(3) 0.012(2) 0.005(2) F2 0.024(3) 0.019(3) 0.033(3) 0.008(2) 0.008(2) -0.001(2) F3 0.022(3) 0.024(3) 0.050(4) 0.010(3) 0.018(3) -0.002(2) F4 0.027(3) 0.015(3) 0.045(4) 0.007(3) 0.005(3) 0.004(2) F5 0.036(3) 0.020(3) 0.031(4) -0.001(2) -0.001(3) 0.002(2) F6 0.032(3) 0.013(3) 0.035(3) -0.003(2) 0.004(3) -0.004(2) F7 0.041(3) 0.010(3) 0.036(4) 0.000(2) 0.005(3) 0.000(2) F8 0.026(3) 0.019(3) 0.035(4) -0.003(2) -0.001(2) 0.001(2) F9 0.034(3) 0.010(3) 0.047(4) 0.004(2) 0.003(3) 0.007(2) F10 0.032(3) 0.018(3) 0.032(4) 0.003(2) 0.004(3) -0.001(2) F11 0.034(3) 0.021(3) 0.037(4) -0.003(3) 0.005(3) 0.002(2) F12 0.030(3) 0.012(3) 0.043(4) 0.006(2) 0.006(3) 0.003(2) O1 0.016(3) 0.034(5) 0.053(5) 0.005(4) 0.002(3) -0.011(3) O2 0.027(3) 0.017(4) 0.044(4) -0.002(3) 0.016(3) -0.002(3) O3 0.025(3) 0.044(5) 0.038(4) 0.002(3) 0.019(3) -0.007(3) O4 0.031(4) 0.030(5) 0.038(5) -0.006(3) 0.003(3) 0.005(3) O5 0.021(3) 0.015(4) 0.057(5) -0.002(3) 0.013(3) 0.004(3) O6 0.018(3) 0.015(4) 0.049(4) 0.003(3) 0.020(3) -0.002(2) O7 0.018(3) 0.021(4) 0.045(4) -0.001(3) 0.007(3) 0.004(3) N1 0.007(3) 0.030(5) 0.039(5) 0.006(4) -0.001(3) 0.001(3) N2 0.032(4) 0.019(5) 0.047(6) 0.003(4) 0.022(4) 0.001(3) N3 0.020(4) 0.045(7) 0.067(7) -0.007(5) 0.016(5) -0.002(4) N4 0.030(5) 0.031(6) 0.075(8) -0.006(5) -0.007(5) 0.019(4) N5 0.022(4) 0.010(4) 0.043(6) -0.002(4) 0.006(4) 0.002(3) N6 0.023(4) 0.028(5) 0.036(5) 0.003(4) 0.007(4) -0.001(3) N7 0.032(5) 0.027(6) 0.050(6) -0.001(4) 0.002(4) 0.011(4) N8 0.040(5) 0.030(6) 0.050(7) 0.003(5) -0.001(5) 0.000(4) N9 0.046(5) 0.019(5) 0.045(6) -0.001(4) 0.017(4) -0.007(4) N10 0.047(5) 0.029(6) 0.040(7) -0.005(4) 0.012(5) -0.008(4) N11 0.029(4) 0.019(5) 0.039(6) -0.006(4) 0.010(4) -0.003(3) N12 0.041(5) 0.025(6) 0.049(6) -0.002(4) 0.025(5) -0.002(4) C1 0.013(4) 0.025(6) 0.032(6) -0.008(4) 0.012(4) -0.009(4) C2 0.017(4) 0.015(5) 0.029(6) 0.000(4) 0.006(4) 0.005(3) C3 0.016(4) 0.008(5) 0.047(7) 0.001(4) 0.011(4) 0.004(3) C4 0.016(4) 0.012(5) 0.042(6) 0.000(4) 0.013(4) 0.002(3) C5 0.013(4) 0.015(5) 0.035(6) 0.001(4) 0.005(4) 0.000(3) C6 0.018(4) 0.007(4) 0.035(6) -0.003(4) 0.010(4) -0.003(3) C7 0.011(4) 0.020(5) 0.035(6) -0.001(4) 0.007(4) 0.000(3) C8 0.022(4) 0.016(5) 0.031(6) -0.004(4) -0.002(4) 0.006(4) C9 0.015(4) 0.008(5) 0.042(6) -0.007(4) 0.005(4) 0.002(3) C10 0.012(4) 0.017(5) 0.043(6) -0.005(4) 0.002(4) 0.002(3) C11 0.012(4) 0.034(6) 0.041(6) -0.005(5) 0.011(4) -0.001(4) C12 0.021(5) 0.026(6) 0.067(8) -0.013(6) 0.007(5) -0.001(4) C13 0.016(4) 0.009(5) 0.049(7) 0.001(4) 0.017(5) 0.001(3) C14 0.011(4) 0.018(5) 0.025(5) -0.003(4) 0.005(4) -0.003(3) C15 0.018(4) 0.017(5) 0.024(5) -0.002(4) 0.010(4) 0.002(3) C16 0.014(4) 0.019(5) 0.037(6) -0.006(4) 0.017(4) -0.005(3) C17 0.023(4) 0.012(5) 0.025(5) -0.003(4) 0.008(4) -0.001(3) C18 0.013(4) 0.010(5) 0.040(6) -0.008(4) 0.010(4) -0.006(3) C19 0.017(4) 0.010(5) 0.035(6) -0.007(4) 0.004(4) 0.000(3) C20 0.015(4) 0.017(5) 0.024(5) -0.004(4) 0.004(4) -0.002(3) C21 0.010(4) 0.016(5) 0.039(6) 0.001(4) 0.007(4) 0.000(3) C22 0.013(4) 0.018(5) 0.032(6) -0.004(4) 0.005(4) 0.001(3) C23 0.016(4) 0.022(6) 0.036(6) -0.006(4) 0.000(4) 0.002(4) C24 0.018(4) 0.016(5) 0.045(7) 0.003(5) 0.009(5) 0.000(3) C25 0.027(5) 0.021(6) 0.033(6) 0.005(4) 0.014(4) -0.002(4) C26 0.031(5) 0.012(5) 0.039(7) -0.005(4) 0.010(5) -0.005(4) C27 0.022(4) 0.018(5) 0.043(7) 0.003(4) 0.017(5) 0.005(4) C28 0.014(4) 0.018(5) 0.028(6) -0.003(4) 0.012(4) -0.001(3) C29 0.025(4) 0.003(4) 0.038(6) 0.002(4) 0.011(4) 0.005(3) C30 0.011(4) 0.018(5) 0.038(6) 0.001(4) 0.007(4) 0.003(3) C31 0.012(4) 0.019(5) 0.028(6) -0.002(4) 0.003(4) 0.001(3) C32 0.021(4) 0.013(5) 0.040(6) 0.009(4) 0.019(4) 0.007(3) C33 0.010(4) 0.015(5) 0.029(6) -0.001(4) 0.008(4) -0.002(3) C34 0.022(4) 0.010(5) 0.039(6) -0.001(4) 0.013(4) -0.009(3) C35 0.017(4) 0.014(5) 0.041(7) -0.001(4) 0.015(4) -0.003(3) C36 0.024(4) 0.017(6) 0.035(6) -0.003(4) 0.015(4) -0.002(4) O1S 0.036(4) 0.044(5) 0.066(6) 0.015(4) 0.007(4) -0.022(4) O2S 0.46(3) 0.031(7) 0.058(7) 0.014(6) 0.090(12) 0.102(12) O3S 0.029(3) 0.015(4) 0.039(4) 0.004(3) -0.001(3) -0.001(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 Pr1 O6 2.482(6) . ? Pr1 O4 2.492(8) . ? Pr1 O2 2.500(7) . ? Pr1 O7 2.558(6) . ? Pr1 O3 2.563(6) . ? Pr1 O1 2.579(6) . ? Pr1 N1 2.641(8) . ? Pr1 O5 2.649(7) . ? Pr1 N5 2.667(9) . ? F1 C5 1.358(11) . ? F2 C6 1.369(10) . ? F3 C7 1.368(10) . ? F4 C8 1.361(11) . ? F5 C17 1.377(11) . ? F6 C18 1.368(10) . ? F7 C19 1.366(10) . ? F8 C20 1.355(10) . ? F9 C29 1.373(10) . ? F10 C30 1.343(11) . ? F11 C31 1.355(11) . ? F12 C32 1.367(10) . ? N1 C1 1.158(12) . ? N2 C2 1.171(11) . ? N3 C11 1.167(13) . ? N4 C12 1.167(14) . ? N5 C13 1.172(12) . ? N6 C14 1.155(12) . ? N7 C23 1.154(13) . ? N8 C24 1.146(13) . ? N9 C25 1.158(13) . ? N10 C26 1.173(13) . ? N11 C35 1.171(13) . ? N12 C36 1.173(13) . ? C1 C3 1.433(14) . ? C2 C3 1.437(12) . ? C3 C4 1.470(11) . ? C4 C6 1.421(13) . ? C4 C5 1.422(12) . ? C5 C7 1.382(11) . ? C6 C8 1.387(11) . ? C7 C9 1.429(13) . ? C8 C9 1.434(13) . ? C9 C10 1.451(11) . ? C10 C12 1.434(15) . ? C10 C11 1.447(13) . ? C13 C15 1.422(14) . ? C14 C15 1.424(13) . ? C15 C16 1.442(13) . ? C16 C18 1.415(13) . ? C16 C17 1.433(13) . ? C17 C19 1.364(14) . ? C18 C20 1.373(13) . ? C19 C21 1.432(14) . ? C20 C21 1.449(13) . ? C21 C22 1.407(13) . ? C22 C24 1.449(15) . ? C22 C23 1.449(13) . ? C25 C27 1.442(14) . ? C26 C27 1.428(16) . ? C27 C28 1.435(14) . ? C28 C29 1.403(13) . ? C28 C30 1.454(13) . ? C29 C31 1.377(13) . ? C30 C32 1.349(14) . ? C31 C33 1.450(13) . ? C32 C33 1.415(13) . ? C33 C34 1.424(13) . ? C34 C36 1.435(13) . ? C34 C35 1.443(15) . ? 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 Pr1 O4 96.2(2) . . ? O6 Pr1 O2 142.6(2) . . ? O4 Pr1 O2 80.6(2) . . ? O6 Pr1 O7 69.8(2) . . ? O4 Pr1 O7 69.2(2) . . ? O2 Pr1 O7 74.4(2) . . ? O6 Pr1 O3 139.3(2) . . ? O4 Pr1 O3 77.1(2) . . ? O2 Pr1 O3 76.8(2) . . ? O7 Pr1 O3 138.4(2) . . ? O6 Pr1 O1 124.8(2) . . ? O4 Pr1 O1 138.6(2) . . ? O2 Pr1 O1 70.0(2) . . ? O7 Pr1 O1 126.0(2) . . ? O3 Pr1 O1 68.5(2) . . ? O6 Pr1 N1 66.6(2) . . ? O4 Pr1 N1 139.5(3) . . ? O2 Pr1 N1 135.5(2) . . ? O7 Pr1 N1 129.1(2) . . ? O3 Pr1 N1 92.4(2) . . ? O1 Pr1 N1 65.9(2) . . ? O6 Pr1 O5 70.6(2) . . ? O4 Pr1 O5 69.2(2) . . ? O2 Pr1 O5 138.6(2) . . ? O7 Pr1 O5 117.3(2) . . ? O3 Pr1 O5 69.5(2) . . ? O1 Pr1 O5 116.3(2) . . ? N1 Pr1 O5 70.5(3) . . ? O6 Pr1 N5 75.8(2) . . ? O4 Pr1 N5 136.6(2) . . ? O2 Pr1 N5 81.3(2) . . ? O7 Pr1 N5 68.1(2) . . ? O3 Pr1 N5 135.3(2) . . ? O1 Pr1 N5 67.5(2) . . ? N1 Pr1 N5 76.8(3) . . ? O5 Pr1 N5 140.1(2) . . ? C1 N1 Pr1 176.3(8) . . ? C13 N5 Pr1 163.5(6) . . ? N1 C1 C3 178.5(9) . . ? N2 C2 C3 175.8(9) . . ? C1 C3 C2 114.3(7) . . ? C1 C3 C4 121.1(8) . . ? C2 C3 C4 124.6(8) . . ? C6 C4 C5 114.9(7) . . ? C6 C4 C3 122.0(8) . . ? C5 C4 C3 123.0(9) . . ? F1 C5 C7 117.9(8) . . ? F1 C5 C4 119.4(7) . . ? C7 C5 C4 122.7(9) . . ? F2 C6 C8 117.3(8) . . ? F2 C6 C4 120.0(7) . . ? C8 C6 C4 122.6(8) . . ? F3 C7 C5 117.1(8) . . ? F3 C7 C9 119.9(7) . . ? C5 C7 C9 122.9(8) . . ? F4 C8 C6 118.8(8) . . ? F4 C8 C9 118.5(7) . . ? C6 C8 C9 122.7(9) . . ? C7 C9 C8 114.1(7) . . ? C7 C9 C10 122.2(8) . . ? C8 C9 C10 123.5(9) . . ? C12 C10 C11 114.6(8) . . ? C12 C10 C9 123.3(9) . . ? C11 C10 C9 122.1(9) . . ? N3 C11 C10 178.2(12) . . ? N4 C12 C10 175.6(11) . . ? N5 C13 C15 177.3(10) . . ? N6 C14 C15 175.2(10) . . ? C13 C15 C14 113.9(8) . . ? C13 C15 C16 122.8(8) . . ? C14 C15 C16 123.1(8) . . ? C18 C16 C17 113.2(8) . . ? C18 C16 C15 124.6(9) . . ? C17 C16 C15 122.3(8) . . ? C19 C17 F5 117.5(8) . . ? C19 C17 C16 123.6(9) . . ? F5 C17 C16 118.9(8) . . ? F6 C18 C20 117.9(8) . . ? F6 C18 C16 118.4(8) . . ? C20 C18 C16 123.7(9) . . ? C17 C19 F7 118.5(8) . . ? C17 C19 C21 124.1(9) . . ? F7 C19 C21 117.4(8) . . ? F8 C20 C18 118.5(8) . . ? F8 C20 C21 118.0(8) . . ? C18 C20 C21 123.5(8) . . ? C22 C21 C19 124.3(9) . . ? C22 C21 C20 123.8(9) . . ? C19 C21 C20 111.9(8) . . ? C21 C22 C24 123.5(9) . . ? C21 C22 C23 123.7(9) . . ? C24 C22 C23 112.6(8) . . ? N7 C23 C22 176.7(10) . . ? N8 C24 C22 175.5(11) . . ? N9 C25 C27 178.3(12) . . ? N10 C26 C27 175.0(10) . . ? C26 C27 C28 124.7(9) . . ? C26 C27 C25 113.3(9) . . ? C28 C27 C25 122.0(10) . . ? C29 C28 C27 124.5(9) . . ? C29 C28 C30 113.8(8) . . ? C27 C28 C30 121.8(9) . . ? F9 C29 C31 116.3(9) . . ? F9 C29 C28 119.5(8) . . ? C31 C29 C28 124.1(9) . . ? F10 C30 C32 119.4(9) . . ? F10 C30 C28 118.9(8) . . ? C32 C30 C28 121.6(9) . . ? F11 C31 C29 118.8(8) . . ? F11 C31 C33 119.1(8) . . ? C29 C31 C33 122.1(9) . . ? C30 C32 F12 116.9(9) . . ? C30 C32 C33 125.6(9) . . ? F12 C32 C33 117.5(8) . . ? C32 C33 C34 125.4(9) . . ? C32 C33 C31 112.6(8) . . ? C34 C33 C31 122.0(9) . . ? C33 C34 C36 121.8(9) . . ? C33 C34 C35 125.5(9) . . ? C36 C34 C35 112.7(8) . . ? N11 C35 C34 177.4(10) . . ? N12 C36 C34 177.9(10) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 6.826 _refine_diff_density_min -4.078 _refine_diff_density_rms 0.297 # Attachment 'SMTCNQF4.CIF' data_g:\nazari~1\nazari~1\crysta~1\nl83sm~1\smtcnqf4 _database_code_depnum_ccdc_archive 'CCDC 749368' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Samarium(III) 2,3,5,6-Tetrafluoro-7,7,8,8-Tetracyanoquinodimethane' ; _chemical_name_common ;Samarium(iii) 2,3,5,6-Tetrafluoro-7,7,8,8- Tetracyanoquinodimethane' ; _chemical_melting_point ? _chemical_formula_moiety {[Sm(TCNQF4)2(H2O)7]}(TCNQF4)(3H2O) _chemical_formula_sum 'C36 H20 F12 N12 O10 Sm' _chemical_formula_weight 1158.99 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.562(2) _cell_length_b 17.394(3) _cell_length_c 18.316(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.016(4) _cell_angle_gamma 90.00 _cell_volume 4288.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 1.493 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5940 _exptl_absorpt_correction_T_max 0.9027 _exptl_absorpt_process_details 'SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43788 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.34 _reflns_number_total 10346 _reflns_number_gt 8412 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0550P)^2^+25.3988P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10346 _refine_ls_number_parameters 641 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1407 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 15.000 _refine_ls_shift/su_mean 0.024 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.23815(2) 0.975635(13) 0.089002(13) 0.01453(9) Uani 1 1 d . . . F1 F 0.5541(2) 1.09846(18) 0.15362(17) 0.0257(7) Uani 1 1 d . . . F2 F 0.5579(2) 1.26388(17) 0.36037(16) 0.0248(7) Uani 1 1 d . . . F3 F 0.7472(3) 1.1048(2) 0.16468(18) 0.0304(8) Uani 1 1 d . . . F4 F 0.7522(3) 1.27358(18) 0.36853(18) 0.0290(8) Uani 1 1 d . . . F5 F 0.2819(3) 1.03575(16) 0.34414(16) 0.0264(7) Uani 1 1 d . . . F6 F 0.3816(3) 0.82014(16) 0.49424(16) 0.0239(7) Uani 1 1 d . . . F7 F 0.3314(3) 1.12682(17) 0.45594(16) 0.0274(7) Uani 1 1 d . . . F8 F 0.4375(3) 0.91276(17) 0.60479(16) 0.0255(7) Uani 1 1 d . . . F9 F 0.0379(3) 1.02612(18) 0.35957(17) 0.0284(7) Uani 1 1 d . . . F10 F 0.1712(3) 0.84923(17) 0.54290(16) 0.0250(7) Uani 1 1 d . . . F11 F 0.0795(3) 1.13941(17) 0.45174(17) 0.0276(7) Uani 1 1 d . . . F12 F 0.2143(3) 0.96260(17) 0.63433(17) 0.0261(7) Uani 1 1 d . . . O1 O 0.4076(3) 0.9293(2) 0.1383(2) 0.0317(10) Uani 1 1 d . . . O2 O 0.2531(4) 0.8394(2) 0.0635(2) 0.0279(9) Uani 1 1 d . . . O3 O 0.3499(4) 0.9740(3) -0.0064(3) 0.0386(11) Uani 1 1 d . . . O4 O 0.1260(3) 0.9688(2) -0.0234(2) 0.0284(9) Uani 1 1 d . . . O5 O 0.2288(3) 1.1051(2) 0.0211(2) 0.0281(9) Uani 1 1 d . . . O6 O 0.0792(3) 0.9153(2) 0.11067(19) 0.0220(8) Uani 1 1 d . . . O7 O 0.1377(3) 1.0648(2) 0.1479(2) 0.0262(9) Uani 1 1 d . . . N1 N 0.2444(4) 0.9223(2) 0.2216(2) 0.0221(10) Uani 1 1 d . . . N2 N 0.3209(4) 0.7267(3) 0.3517(3) 0.0263(10) Uani 1 1 d . . . N3 N 0.4743(5) 1.0323(3) 0.7286(3) 0.0374(13) Uani 1 1 d . . . N4 N 0.4277(4) 1.2221(3) 0.5864(3) 0.0332(12) Uani 1 1 d . . . N5 N 0.3418(3) 1.0757(2) 0.1676(2) 0.0210(9) Uani 1 1 d . . . N6 N 0.3301(4) 1.2454(3) 0.3343(3) 0.0286(11) Uani 1 1 d . . . N7 N 0.9765(5) 1.2866(4) 0.3528(4) 0.0523(17) Uani 1 1 d . . . N8 N 0.9660(4) 1.0952(4) 0.2060(4) 0.0443(15) Uani 1 1 d . . . N9 N 0.0164(4) 0.8837(3) 0.2576(3) 0.0300(11) Uani 1 1 d . . . N10 N 0.1138(4) 0.7278(3) 0.4302(3) 0.0336(12) Uani 1 1 d . . . N11 N 0.2390(4) 1.1052(3) 0.7353(3) 0.0356(13) Uani 1 1 d . . . N12 N 0.1708(5) 1.2613(3) 0.5581(3) 0.0352(13) Uani 1 1 d . . . C1 C 0.2702(4) 0.9018(3) 0.2800(3) 0.0185(10) Uani 1 1 d . . . C2 C 0.3142(4) 0.7917(3) 0.3540(3) 0.0182(10) Uani 1 1 d . . . C3 C 0.3026(4) 0.8734(3) 0.3517(3) 0.0159(10) Uani 1 1 d . . . C4 C 0.3311(4) 0.9221(3) 0.4124(3) 0.0152(9) Uani 1 1 d . . . C5 C 0.3217(4) 1.0034(3) 0.4079(3) 0.0180(10) Uani 1 1 d . . . C6 C 0.3698(4) 0.8965(3) 0.4833(3) 0.0167(10) Uani 1 1 d . . . C7 C 0.3466(4) 1.0513(3) 0.4661(3) 0.0178(10) Uani 1 1 d . . . C8 C 0.3976(4) 0.9443(3) 0.5408(3) 0.0173(10) Uani 1 1 d . . . C9 C 0.3875(4) 1.0252(3) 0.5365(3) 0.0175(10) Uani 1 1 d . . . C10 C 0.4143(4) 1.0750(3) 0.5967(3) 0.0185(10) Uani 1 1 d . . . C11 C 0.4190(4) 1.1569(3) 0.5890(3) 0.0223(11) Uani 1 1 d . . . C12 C 0.4468(4) 1.0487(3) 0.6690(3) 0.0240(12) Uani 1 1 d . . . C13 C 0.3870(4) 1.1191(3) 0.2060(3) 0.0195(10) Uani 1 1 d . . . C14 C 0.3820(4) 1.2135(3) 0.2997(3) 0.0201(11) Uani 1 1 d . . . C15 C 0.4411(4) 1.1717(3) 0.2538(3) 0.0187(10) Uani 1 1 d . . . C16 C 0.5451(4) 1.1801(3) 0.2573(3) 0.0187(10) Uani 1 1 d . . . C17 C 0.6015(4) 1.1412(3) 0.2086(3) 0.0208(11) Uani 1 1 d . . . C18 C 0.6036(4) 1.2262(3) 0.3102(3) 0.0196(11) Uani 1 1 d . . . C19 C 0.7014(4) 1.1448(3) 0.2141(3) 0.0217(11) Uani 1 1 d . . . C20 C 0.7040(4) 1.2305(3) 0.3143(3) 0.0200(11) Uani 1 1 d . . . C21 C 0.7605(4) 1.1897(3) 0.2670(3) 0.0222(11) Uani 1 1 d . . . C22 C 0.8650(4) 1.1916(3) 0.2731(3) 0.0280(13) Uani 1 1 d . . . C23 C 0.9196(5) 1.1386(4) 0.2347(4) 0.0337(14) Uani 1 1 d . . . C24 C 0.9250(5) 1.2446(4) 0.3181(4) 0.0359(15) Uani 1 1 d . . . C25 C 0.0464(4) 0.8793(3) 0.3192(3) 0.0227(11) Uani 1 1 d . . . C26 C 0.1011(4) 0.7914(3) 0.4156(3) 0.0235(11) Uani 1 1 d . . . C27 C 0.0859(4) 0.8698(3) 0.3945(3) 0.0199(10) Uani 1 1 d . . . C28 C 0.1044(4) 0.9309(3) 0.4451(3) 0.0177(10) Uani 1 1 d . . . C29 C 0.0837(4) 1.0094(3) 0.4268(3) 0.0188(10) Uani 1 1 d . . . C30 C 0.1478(4) 0.9207(3) 0.5188(3) 0.0180(10) Uani 1 1 d . . . C31 C 0.1052(4) 1.0679(3) 0.4749(3) 0.0186(10) Uani 1 1 d . . . C32 C 0.1699(4) 0.9792(3) 0.5669(3) 0.0190(10) Uani 1 1 d . . . C33 C 0.1517(4) 1.0578(3) 0.5478(3) 0.0166(10) Uani 1 1 d . . . C34 C 0.1781(4) 1.1189(3) 0.5974(3) 0.0211(11) Uani 1 1 d . . . C35 C 0.1737(5) 1.1974(3) 0.5744(3) 0.0242(12) Uani 1 1 d . . . C36 C 0.2125(4) 1.1090(3) 0.6732(3) 0.0241(12) Uani 1 1 d . . . O1S O 0.0087(3) 0.1469(2) 0.0172(2) 0.0267(8) Uiso 1 1 d . . . O2S O 0.5243(5) 0.8870(4) 0.0137(3) 0.0620(15) Uiso 1 1 d . . . O3S O 0.8399(5) 0.9310(4) 0.1283(3) 0.0663(16) Uiso 1 1 d . . . H3SA H 0.758(4) 0.945(3) 0.117(3) 0.000(11) Uiso 1 1 d . . . H2WA H 0.268(6) 0.825(5) 0.030(4) 0.04(2) Uiso 1 1 d . . . H3WA H 0.396(6) 0.931(5) -0.006(4) 0.05(2) Uiso 1 1 d . . . H3WB H 0.327(8) 0.930(6) -0.031(5) 0.08(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02016(15) 0.01032(12) 0.01243(12) -0.00009(9) -0.00074(9) 0.00064(10) F1 0.0254(18) 0.0273(16) 0.0240(15) -0.0094(13) 0.0018(13) -0.0036(13) F2 0.0340(19) 0.0188(15) 0.0207(15) -0.0047(12) -0.0010(13) -0.0001(13) F3 0.0280(19) 0.0315(18) 0.0330(18) -0.0057(14) 0.0095(15) 0.0004(14) F4 0.035(2) 0.0188(15) 0.0295(17) -0.0017(13) -0.0096(14) -0.0055(13) F5 0.049(2) 0.0143(14) 0.0137(14) 0.0035(11) -0.0066(13) 0.0009(13) F6 0.037(2) 0.0136(14) 0.0196(14) 0.0034(11) -0.0006(13) 0.0060(13) F7 0.049(2) 0.0111(14) 0.0208(15) 0.0025(11) -0.0031(14) -0.0005(13) F8 0.038(2) 0.0207(15) 0.0150(14) 0.0035(12) -0.0069(13) 0.0030(13) F9 0.040(2) 0.0240(16) 0.0194(15) 0.0021(12) -0.0036(14) 0.0048(14) F10 0.038(2) 0.0129(14) 0.0232(15) 0.0033(12) 0.0000(14) 0.0017(13) F11 0.042(2) 0.0127(14) 0.0264(16) 0.0032(12) -0.0025(14) 0.0066(13) F12 0.039(2) 0.0193(15) 0.0198(15) 0.0041(12) 0.0007(13) -0.0015(13) O1 0.027(2) 0.035(2) 0.030(2) -0.0088(18) -0.0080(17) 0.0121(18) O2 0.042(3) 0.0140(18) 0.029(2) -0.0029(16) 0.0130(19) 0.0009(17) O3 0.041(3) 0.045(3) 0.033(2) 0.004(2) 0.014(2) 0.015(2) O4 0.032(2) 0.031(2) 0.0198(18) 0.0051(16) -0.0066(16) -0.0047(17) O5 0.042(3) 0.0173(18) 0.0253(19) 0.0028(15) 0.0072(18) -0.0013(17) O6 0.026(2) 0.0201(18) 0.0193(17) -0.0017(14) -0.0011(15) -0.0047(15) O7 0.024(2) 0.0178(18) 0.038(2) -0.0059(16) 0.0074(17) 0.0004(15) N1 0.034(3) 0.015(2) 0.016(2) -0.0007(16) 0.0004(18) -0.0025(18) N2 0.034(3) 0.019(2) 0.025(2) 0.0016(18) -0.002(2) 0.0025(19) N3 0.051(4) 0.034(3) 0.024(2) -0.003(2) -0.009(2) -0.003(2) N4 0.041(3) 0.026(3) 0.032(3) -0.003(2) 0.000(2) -0.010(2) N5 0.017(2) 0.018(2) 0.027(2) -0.0021(18) -0.0028(18) -0.0009(17) N6 0.035(3) 0.021(2) 0.031(3) 0.000(2) 0.009(2) -0.001(2) N7 0.046(4) 0.036(3) 0.069(4) 0.009(3) -0.017(3) -0.015(3) N8 0.024(3) 0.051(4) 0.059(4) 0.008(3) 0.012(3) 0.006(3) N9 0.035(3) 0.030(3) 0.025(2) -0.006(2) 0.005(2) -0.006(2) N10 0.047(3) 0.019(2) 0.037(3) -0.005(2) 0.013(2) -0.001(2) N11 0.049(4) 0.035(3) 0.023(3) -0.006(2) 0.006(2) -0.006(2) N12 0.057(4) 0.021(3) 0.029(3) -0.002(2) 0.011(2) -0.005(2) C1 0.024(3) 0.012(2) 0.019(2) -0.0008(18) 0.002(2) -0.0010(19) C2 0.020(3) 0.020(3) 0.013(2) 0.0030(18) -0.0025(19) -0.001(2) C3 0.023(3) 0.012(2) 0.013(2) 0.0027(17) 0.0007(19) -0.0003(19) C4 0.017(3) 0.014(2) 0.015(2) 0.0036(17) 0.0028(18) 0.0008(18) C5 0.025(3) 0.013(2) 0.015(2) 0.0023(17) -0.001(2) -0.0004(19) C6 0.018(3) 0.017(2) 0.015(2) 0.0037(18) -0.0002(19) 0.0030(19) C7 0.020(3) 0.013(2) 0.020(2) 0.0039(18) 0.003(2) -0.0007(19) C8 0.019(3) 0.020(2) 0.013(2) 0.0038(18) 0.0018(19) 0.001(2) C9 0.019(3) 0.017(2) 0.016(2) 0.0006(18) -0.0013(19) -0.002(2) C10 0.017(3) 0.020(2) 0.017(2) 0.0010(19) -0.0027(19) -0.004(2) C11 0.022(3) 0.022(3) 0.021(2) -0.001(2) -0.003(2) -0.007(2) C12 0.025(3) 0.021(3) 0.024(3) -0.002(2) -0.001(2) -0.002(2) C13 0.018(3) 0.016(2) 0.024(2) 0.002(2) 0.003(2) 0.005(2) C14 0.026(3) 0.014(2) 0.020(2) 0.0027(19) -0.001(2) -0.004(2) C15 0.024(3) 0.011(2) 0.020(2) 0.0013(18) -0.001(2) -0.0019(19) C16 0.027(3) 0.011(2) 0.018(2) 0.0023(18) 0.001(2) -0.0004(19) C17 0.027(3) 0.017(2) 0.018(2) -0.0007(19) 0.001(2) -0.002(2) C18 0.030(3) 0.011(2) 0.018(2) 0.0034(18) 0.003(2) 0.001(2) C19 0.026(3) 0.016(2) 0.023(3) 0.0028(19) 0.005(2) 0.000(2) C20 0.027(3) 0.010(2) 0.021(2) 0.0030(18) -0.006(2) -0.0056(19) C21 0.023(3) 0.012(2) 0.030(3) 0.008(2) -0.001(2) -0.003(2) C22 0.024(3) 0.023(3) 0.036(3) 0.008(2) -0.001(2) -0.003(2) C23 0.025(3) 0.035(3) 0.041(3) 0.010(3) 0.005(3) -0.006(3) C24 0.031(4) 0.026(3) 0.048(4) 0.013(3) -0.004(3) -0.006(3) C25 0.025(3) 0.018(2) 0.027(3) -0.008(2) 0.011(2) -0.006(2) C26 0.027(3) 0.019(3) 0.026(3) -0.004(2) 0.009(2) -0.004(2) C27 0.021(3) 0.017(2) 0.023(2) -0.002(2) 0.009(2) -0.002(2) C28 0.018(3) 0.016(2) 0.020(2) 0.0009(19) 0.005(2) -0.0021(19) C29 0.021(3) 0.019(2) 0.016(2) 0.0028(18) -0.001(2) 0.0014(19) C30 0.020(3) 0.013(2) 0.022(2) 0.0052(18) 0.004(2) 0.0016(19) C31 0.022(3) 0.014(2) 0.020(2) 0.0030(18) 0.003(2) 0.0026(19) C32 0.021(3) 0.019(2) 0.017(2) 0.0077(19) 0.0014(19) 0.003(2) C33 0.020(3) 0.011(2) 0.019(2) -0.0003(18) 0.0055(19) -0.0002(19) C34 0.024(3) 0.018(2) 0.021(2) 0.000(2) 0.004(2) -0.002(2) C35 0.035(3) 0.020(3) 0.019(2) -0.001(2) 0.006(2) -0.004(2) C36 0.029(3) 0.023(3) 0.020(3) -0.005(2) 0.005(2) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O7 2.405(4) . ? Sm1 O4 2.409(4) . ? Sm1 O2 2.429(4) . ? Sm1 O3 2.450(5) . ? Sm1 O6 2.473(4) . ? Sm1 O1 2.498(4) . ? Sm1 N5 2.566(4) . ? Sm1 O5 2.567(4) . ? Sm1 N1 2.591(4) . ? F1 C17 1.349(6) . ? F2 C18 1.341(6) . ? F3 C19 1.352(6) . ? F4 C20 1.347(6) . ? F5 C5 1.348(5) . ? F6 C6 1.349(6) . ? F7 C7 1.339(6) . ? F8 C8 1.346(5) . ? F9 C29 1.342(6) . ? F10 C30 1.344(5) . ? F11 C31 1.346(6) . ? F12 C32 1.338(6) . ? N1 C1 1.143(6) . ? N2 C2 1.136(7) . ? N3 C12 1.147(7) . ? N4 C11 1.141(7) . ? N5 C13 1.156(7) . ? N6 C14 1.145(7) . ? N7 C24 1.146(8) . ? N8 C23 1.150(9) . ? N9 C25 1.154(7) . ? N10 C26 1.147(7) . ? N11 C36 1.152(7) . ? N12 C35 1.149(7) . ? C1 C3 1.421(6) . ? C2 C3 1.429(7) . ? C3 C4 1.413(7) . ? C4 C6 1.412(6) . ? C4 C5 1.423(7) . ? C5 C7 1.363(7) . ? C6 C8 1.359(7) . ? C7 C9 1.414(7) . ? C8 C9 1.415(7) . ? C9 C10 1.416(7) . ? C10 C12 1.418(7) . ? C10 C11 1.434(7) . ? C13 C15 1.409(7) . ? C14 C15 1.431(8) . ? C15 C16 1.411(8) . ? C16 C17 1.416(7) . ? C16 C18 1.422(7) . ? C17 C19 1.348(8) . ? C18 C20 1.357(8) . ? C19 C21 1.415(7) . ? C20 C21 1.415(8) . ? C21 C22 1.408(8) . ? C22 C23 1.421(9) . ? C22 C24 1.424(8) . ? C25 C27 1.428(8) . ? C26 C27 1.425(7) . ? C27 C28 1.412(7) . ? C28 C30 1.416(7) . ? C28 C29 1.426(7) . ? C29 C31 1.355(7) . ? C30 C32 1.355(7) . ? C31 C33 1.417(7) . ? C32 C33 1.425(7) . ? C33 C34 1.415(7) . ? C34 C36 1.421(7) . ? C34 C35 1.428(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Sm1 O4 94.71(14) . . ? O7 Sm1 O2 141.34(14) . . ? O4 Sm1 O2 81.16(15) . . ? O7 Sm1 O3 139.54(15) . . ? O4 Sm1 O3 76.75(16) . . ? O2 Sm1 O3 77.19(16) . . ? O7 Sm1 O6 69.49(13) . . ? O4 Sm1 O6 69.16(13) . . ? O2 Sm1 O6 73.23(14) . . ? O3 Sm1 O6 137.49(16) . . ? O7 Sm1 O1 126.32(13) . . ? O4 Sm1 O1 138.61(14) . . ? O2 Sm1 O1 70.13(15) . . ? O3 Sm1 O1 68.42(15) . . ? O6 Sm1 O1 125.91(14) . . ? O7 Sm1 N5 67.18(14) . . ? O4 Sm1 N5 139.33(14) . . ? O2 Sm1 N5 135.80(15) . . ? O3 Sm1 N5 93.64(17) . . ? O6 Sm1 N5 128.80(13) . . ? O1 Sm1 N5 66.37(14) . . ? O7 Sm1 O5 69.78(13) . . ? O4 Sm1 O5 68.95(13) . . ? O2 Sm1 O5 139.72(14) . . ? O3 Sm1 O5 70.28(15) . . ? O6 Sm1 O5 117.24(13) . . ? O1 Sm1 O5 116.53(15) . . ? N5 Sm1 O5 70.61(13) . . ? O7 Sm1 N1 76.49(14) . . ? O4 Sm1 N1 136.73(14) . . ? O2 Sm1 N1 80.60(14) . . ? O3 Sm1 N1 135.43(16) . . ? O6 Sm1 N1 68.09(13) . . ? O1 Sm1 N1 67.81(15) . . ? N5 Sm1 N1 76.38(14) . . ? O5 Sm1 N1 139.63(13) . . ? C1 N1 Sm1 164.0(4) . . ? C13 N5 Sm1 176.6(4) . . ? N1 C1 C3 177.8(5) . . ? N2 C2 C3 176.1(5) . . ? C4 C3 C1 122.8(4) . . ? C4 C3 C2 123.7(4) . . ? C1 C3 C2 113.2(4) . . ? C6 C4 C3 124.7(4) . . ? C6 C4 C5 112.8(4) . . ? C3 C4 C5 122.5(4) . . ? F5 C5 C7 117.3(4) . . ? F5 C5 C4 119.2(4) . . ? C7 C5 C4 123.4(4) . . ? F6 C6 C8 118.0(4) . . ? F6 C6 C4 118.1(4) . . ? C8 C6 C4 123.8(5) . . ? F7 C7 C5 118.1(4) . . ? F7 C7 C9 118.6(4) . . ? C5 C7 C9 123.3(5) . . ? F8 C8 C6 118.0(4) . . ? F8 C8 C9 118.7(4) . . ? C6 C8 C9 123.3(4) . . ? C7 C9 C8 113.3(4) . . ? C7 C9 C10 123.3(5) . . ? C8 C9 C10 123.5(4) . . ? C9 C10 C12 123.4(5) . . ? C9 C10 C11 122.8(4) . . ? C12 C10 C11 113.6(4) . . ? N4 C11 C10 175.5(6) . . ? N3 C12 C10 175.6(6) . . ? N5 C13 C15 179.0(6) . . ? N6 C14 C15 176.3(6) . . ? C13 C15 C16 122.5(5) . . ? C13 C15 C14 114.1(5) . . ? C16 C15 C14 123.3(5) . . ? C15 C16 C17 122.4(5) . . ? C15 C16 C18 124.1(5) . . ? C17 C16 C18 113.5(5) . . ? C19 C17 F1 117.7(5) . . ? C19 C17 C16 123.1(5) . . ? F1 C17 C16 119.3(5) . . ? F2 C18 C20 118.7(5) . . ? F2 C18 C16 118.4(5) . . ? C20 C18 C16 122.8(5) . . ? C17 C19 F3 117.7(5) . . ? C17 C19 C21 123.9(5) . . ? F3 C19 C21 118.4(5) . . ? F4 C20 C18 117.7(5) . . ? F4 C20 C21 118.7(5) . . ? C18 C20 C21 123.6(5) . . ? C22 C21 C19 123.2(5) . . ? C22 C21 C20 123.7(5) . . ? C19 C21 C20 113.1(5) . . ? C21 C22 C23 121.7(5) . . ? C21 C22 C24 123.9(6) . . ? C23 C22 C24 114.3(6) . . ? N8 C23 C22 177.4(7) . . ? N7 C24 C22 177.2(9) . . ? N9 C25 C27 176.8(6) . . ? N10 C26 C27 177.8(6) . . ? C28 C27 C26 122.2(5) . . ? C28 C27 C25 124.2(5) . . ? C26 C27 C25 113.5(5) . . ? C27 C28 C30 123.5(5) . . ? C27 C28 C29 123.5(5) . . ? C30 C28 C29 113.0(4) . . ? F9 C29 C31 118.2(4) . . ? F9 C29 C28 118.6(4) . . ? C31 C29 C28 123.2(4) . . ? F10 C30 C32 117.2(4) . . ? F10 C30 C28 118.8(4) . . ? C32 C30 C28 124.0(4) . . ? F11 C31 C29 117.6(4) . . ? F11 C31 C33 118.7(4) . . ? C29 C31 C33 123.7(4) . . ? F12 C32 C30 118.5(4) . . ? F12 C32 C33 118.6(4) . . ? C30 C32 C33 122.9(4) . . ? C34 C33 C31 124.0(4) . . ? C34 C33 C32 122.8(5) . . ? C31 C33 C32 113.2(4) . . ? C33 C34 C36 124.2(5) . . ? C33 C34 C35 122.1(5) . . ? C36 C34 C35 113.7(5) . . ? N12 C35 C34 178.0(6) . . ? N11 C36 C34 176.1(6) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 4.267 _refine_diff_density_min -2.071 _refine_diff_density_rms 0.164 # Attachment 'YBTCNQF4.CIF' data_g:\nazari~1\nazari~1\crysta~1\nl080y~1\ybtcnqf4 _database_code_depnum_ccdc_archive 'CCDC 749369' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Ytterbium(III) 2,3,5,6-Tetrafluoro-7,7,8,8-Tetracyanoquinodimethane' ; _chemical_name_common ;Ytterbium(iii) 2,3,5,6-Tetrafluoro-7,7,8,8- Tetracyanoquinodimethane' ; _chemical_melting_point ? _chemical_formula_sum 'C36 H18 F12 N12 O9 Yb' _chemical_formula_weight 1163.66 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.649(8) _cell_length_b 17.653(14) _cell_length_c 16.977(14) _cell_angle_alpha 90.00 _cell_angle_beta 103.09(3) _cell_angle_gamma 90.00 _cell_volume 3985(5) _cell_formula_units_Z 4 _cell_measurement_temperature 383(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.940 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 2.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2761 _exptl_absorpt_correction_T_max 0.5237 _exptl_absorpt_process_details 'SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 383(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16036 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.32 _reflns_number_total 8617 _reflns_number_gt 7479 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0929P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8617 _refine_ls_number_parameters 655 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1332 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.197739(13) 0.591296(9) 0.935471(11) 0.01068(9) Uani 1 1 d . . . F1 F 0.2062(2) 0.84052(13) 1.00187(16) 0.0195(6) Uani 1 1 d . . . F2 F 0.0622(2) 1.00831(14) 0.78836(16) 0.0200(6) Uani 1 1 d . . . F3 F 0.1940(2) 0.94566(14) 1.10692(17) 0.0214(6) Uani 1 1 d . . . F4 F 0.0446(2) 1.11276(15) 0.89492(18) 0.0226(6) Uani 1 1 d . . . F5 F 0.5228(2) 0.68987(14) 1.09379(17) 0.0191(6) Uani 1 1 d . . . F6 F 0.45373(19) 0.87648(14) 1.27376(16) 0.0159(6) Uani 1 1 d . . . F7 F 0.71664(19) 0.70929(14) 1.15000(18) 0.0202(6) Uani 1 1 d . . . F8 F 0.6467(2) 0.89917(14) 1.32770(18) 0.0185(6) Uani 1 1 d . . . F9 F 0.2891(2) 0.46689(14) 0.31723(16) 0.0187(6) Uani 1 1 d . . . F10 F 0.44944(19) 0.63104(14) 0.52783(17) 0.0193(6) Uani 1 1 d . . . F11 F 0.2755(2) 0.36254(14) 0.42387(16) 0.0192(6) Uani 1 1 d . . . F12 F 0.4356(2) 0.52709(15) 0.63531(16) 0.0202(6) Uani 1 1 d . . . O1 O 0.0858(2) 0.64562(17) 1.0021(2) 0.0181(7) Uani 1 1 d . . . O2 O 0.1284(3) 0.58686(16) 0.7993(2) 0.0204(8) Uani 1 1 d . . . O3 O 0.0666(3) 0.50484(18) 0.9271(2) 0.0196(7) Uani 1 1 d . . . O4 O 0.2504(3) 0.47398(18) 0.8986(2) 0.0205(8) Uani 1 1 d . . . O5 O 0.2445(2) 0.52810(17) 1.0559(2) 0.0179(7) Uani 1 1 d . . . O6 O 0.3514(2) 0.60446(17) 0.9072(2) 0.0181(7) Uani 1 1 d . . . N1 N 0.1718(3) 0.7208(2) 0.8788(2) 0.0163(8) Uani 1 1 d . . . N2 N 0.1145(3) 0.8792(2) 0.6788(3) 0.0213(9) Uani 1 1 d . . . N3 N 0.1472(3) 1.0645(2) 1.2198(3) 0.0244(9) Uani 1 1 d . . . N4 N 0.0430(4) 1.2261(2) 1.0372(3) 0.0294(11) Uani 1 1 d . . . N5 N 0.2960(3) 0.67885(19) 1.0355(2) 0.0148(8) Uani 1 1 d . . . N6 N 0.2325(3) 0.8179(2) 1.2164(3) 0.0204(9) Uani 1 1 d . . . N7 N 0.9377(3) 0.7412(2) 1.2291(3) 0.0298(11) Uani 1 1 d . . . N8 N 0.8726(3) 0.9152(2) 1.3817(3) 0.0220(10) Uani 1 1 d . . . N9 N 0.3509(4) 0.5813(2) 0.2067(3) 0.0239(10) Uani 1 1 d . . . N10 N 0.4312(3) 0.7492(2) 0.3923(3) 0.0224(9) Uani 1 1 d . . . N11 N 0.3008(4) 0.2416(2) 0.5541(3) 0.0298(11) Uani 1 1 d . . . N12 N 0.3953(4) 0.4039(2) 0.7456(3) 0.0298(12) Uani 1 1 d . . . C1 C 0.1576(3) 0.7829(2) 0.8574(3) 0.0143(9) Uani 1 1 d . . . C2 C 0.1234(3) 0.8711(2) 0.7472(3) 0.0154(9) Uani 1 1 d . . . C3 C 0.1408(3) 0.8594(2) 0.8323(3) 0.0151(9) Uani 1 1 d . . . C4 C 0.1325(3) 0.9173(2) 0.8887(3) 0.0123(9) Uani 1 1 d . . . C5 C 0.1643(4) 0.9070(2) 0.9744(3) 0.0160(10) Uani 1 1 d . . . C6 C 0.0934(3) 0.9915(2) 0.8675(3) 0.0131(9) Uani 1 1 d . . . C7 C 0.1574(3) 0.9613(2) 1.0287(3) 0.0154(9) Uani 1 1 d . . . C8 C 0.0857(3) 1.0455(2) 0.9222(3) 0.0159(10) Uani 1 1 d . . . C9 C 0.1175(3) 1.0351(2) 1.0070(3) 0.0150(9) Uani 1 1 d . . . C10 C 0.1124(4) 1.0907(2) 1.0664(3) 0.0169(10) Uani 1 1 d . . . C11 C 0.1332(4) 1.0749(2) 1.1509(3) 0.0197(10) Uani 1 1 d . . . C12 C 0.0737(3) 1.1651(3) 1.0469(3) 0.0195(10) Uani 1 1 d . . . C13 C 0.3343(3) 0.7165(2) 1.0882(3) 0.0145(9) Uani 1 1 d . . . C14 C 0.2975(3) 0.7964(2) 1.1905(3) 0.0149(9) Uani 1 1 d . . . C15 C 0.3732(3) 0.7648(2) 1.1547(3) 0.0137(9) Uani 1 1 d . . . C16 C 0.4781(3) 0.7794(2) 1.1832(3) 0.0124(9) Uani 1 1 d . . . C17 C 0.5526(3) 0.7408(2) 1.1529(3) 0.0139(9) Uani 1 1 d . . . C18 C 0.5176(3) 0.8333(2) 1.2436(3) 0.0130(9) Uani 1 1 d . . . C19 C 0.6532(3) 0.7509(2) 1.1820(3) 0.0140(9) Uani 1 1 d . . . C20 C 0.6183(3) 0.8445(2) 1.2716(3) 0.0138(9) Uani 1 1 d . . . C21 C 0.6934(3) 0.8036(2) 1.2445(3) 0.0147(9) Uani 1 1 d . . . C22 C 0.7983(3) 0.8147(2) 1.2753(3) 0.0153(9) Uani 1 1 d . . . C23 C 0.8734(3) 0.7731(2) 1.2485(3) 0.0192(10) Uani 1 1 d . . . C24 C 0.8367(3) 0.8701(2) 1.3346(3) 0.0166(9) Uani 1 1 d . . . C25 C 0.3608(4) 0.5937(2) 0.2745(3) 0.0182(11) Uani 1 1 d . . . C26 C 0.4068(3) 0.6870(2) 0.3798(3) 0.0170(10) Uani 1 1 d . . . C27 C 0.3765(3) 0.6113(2) 0.3588(3) 0.0147(9) Uani 1 1 d . . . C28 C 0.3698(3) 0.5549(2) 0.4171(3) 0.0136(9) Uani 1 1 d . . . C29 C 0.3282(3) 0.4818(2) 0.3954(3) 0.0138(9) Uani 1 1 d . . . C30 C 0.4039(3) 0.5651(2) 0.5015(3) 0.0151(9) Uani 1 1 d . . . C31 C 0.3207(3) 0.4280(2) 0.4509(3) 0.0146(9) Uani 1 1 d . . . C32 C 0.3970(3) 0.5115(2) 0.5565(3) 0.0147(9) Uani 1 1 d . . . C33 C 0.3551(3) 0.4377(2) 0.5360(3) 0.0139(9) Uani 1 1 d . . . C34 C 0.3470(3) 0.3809(2) 0.5924(3) 0.0172(10) Uani 1 1 d . . . C35 C 0.3205(4) 0.3049(3) 0.5703(3) 0.0223(11) Uani 1 1 d . . . C36 C 0.3744(4) 0.3939(3) 0.6778(3) 0.0201(10) Uani 1 1 d . . . H1A H 0.048(4) 0.683(3) 0.991(3) 0.014(13) Uiso 1 1 d . . . H3A H 0.013(5) 0.516(3) 0.922(4) 0.032(18) Uiso 1 1 d . . . H4A H 0.231(8) 0.450(6) 0.863(6) 0.11(4) Uiso 1 1 d . . . O1S O 0.4847(3) 0.48768(19) 0.8966(3) 0.0224(8) Uani 1 1 d . . . O2S O 0.1013(3) 0.3536(2) 0.9200(3) 0.0301(9) Uani 1 1 d . . . O3S O 0.3933(3) 0.40387(17) 0.0084(2) 0.0243(8) Uani 1 1 d . . . H1SA H 0.469(4) 0.457(3) 0.930(4) 0.029(16) Uiso 1 1 d . . . H2SA H 0.142(5) 0.330(4) 0.960(4) 0.036(18) Uiso 1 1 d . . . H1SB H 0.468(8) 0.457(6) 0.848(7) 0.11(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.01005(13) 0.00798(12) 0.01375(13) -0.00096(6) 0.00215(9) -0.00039(5) F1 0.0287(14) 0.0100(11) 0.0179(14) 0.0015(10) 0.0009(12) 0.0069(10) F2 0.0246(14) 0.0160(12) 0.0166(14) 0.0065(11) -0.0015(12) 0.0044(10) F3 0.0335(16) 0.0154(13) 0.0141(13) 0.0023(11) 0.0029(12) 0.0075(11) F4 0.0289(15) 0.0122(12) 0.0242(15) 0.0043(12) 0.0010(13) 0.0080(11) F5 0.0176(13) 0.0170(12) 0.0215(15) -0.0108(11) 0.0020(11) 0.0000(10) F6 0.0147(13) 0.0136(12) 0.0208(14) -0.0049(11) 0.0068(11) 0.0030(9) F7 0.0162(13) 0.0187(13) 0.0260(15) -0.0096(11) 0.0056(12) 0.0025(10) F8 0.0189(14) 0.0163(12) 0.0203(15) -0.0075(11) 0.0046(12) -0.0025(9) F9 0.0262(14) 0.0128(12) 0.0158(14) -0.0032(10) 0.0024(11) -0.0033(10) F10 0.0214(14) 0.0136(12) 0.0206(14) -0.0040(11) -0.0001(11) -0.0051(10) F11 0.0255(14) 0.0110(11) 0.0205(14) -0.0023(11) 0.0037(12) -0.0044(10) F12 0.0247(14) 0.0194(13) 0.0146(14) -0.0017(11) 0.0007(12) -0.0024(10) O1 0.0154(16) 0.0129(15) 0.0262(19) 0.0002(14) 0.0054(14) 0.0057(12) O2 0.0257(19) 0.0177(16) 0.0145(17) -0.0024(12) -0.0020(15) -0.0064(12) O3 0.0136(17) 0.0158(15) 0.028(2) -0.0005(14) 0.0015(15) -0.0022(12) O4 0.0192(16) 0.0128(15) 0.029(2) -0.0106(14) 0.0041(15) 0.0006(12) O5 0.0181(16) 0.0157(14) 0.0189(17) 0.0008(13) 0.0018(14) -0.0006(11) O6 0.0173(16) 0.0142(14) 0.0248(19) -0.0041(13) 0.0094(15) -0.0016(11) N1 0.0214(19) 0.0143(17) 0.0144(19) -0.0011(15) 0.0067(16) -0.0003(14) N2 0.024(2) 0.021(2) 0.017(2) 0.0023(17) 0.0018(17) -0.0048(15) N3 0.031(2) 0.0189(19) 0.023(2) 0.0009(18) 0.0055(19) 0.0020(16) N4 0.037(3) 0.021(2) 0.029(2) 0.0014(19) 0.003(2) 0.0094(18) N5 0.0129(18) 0.0109(16) 0.019(2) -0.0006(15) -0.0001(15) -0.0011(12) N6 0.017(2) 0.0208(19) 0.024(2) 0.0019(17) 0.0059(18) 0.0023(15) N7 0.016(2) 0.031(2) 0.042(3) -0.011(2) 0.004(2) 0.0018(17) N8 0.016(2) 0.022(2) 0.027(2) -0.0086(17) 0.0037(19) 0.0017(14) N9 0.028(2) 0.022(2) 0.017(2) -0.0017(17) -0.0033(19) -0.0043(16) N10 0.024(2) 0.0165(19) 0.027(2) -0.0008(17) 0.0071(19) 0.0016(15) N11 0.049(3) 0.015(2) 0.028(3) 0.0023(17) 0.013(2) 0.0005(17) N12 0.041(3) 0.023(2) 0.022(3) 0.0041(17) 0.000(2) -0.0055(17) C1 0.014(2) 0.016(2) 0.013(2) -0.0022(17) 0.0041(18) -0.0016(15) C2 0.015(2) 0.0102(18) 0.021(2) 0.0016(17) 0.0037(19) -0.0019(14) C3 0.015(2) 0.0135(19) 0.016(2) 0.0002(17) 0.0016(18) -0.0012(15) C4 0.010(2) 0.0093(18) 0.017(2) 0.0025(16) 0.0011(18) -0.0009(13) C5 0.019(2) 0.0089(19) 0.019(2) 0.0061(16) 0.001(2) -0.0007(14) C6 0.014(2) 0.0109(18) 0.014(2) 0.0046(16) 0.0004(17) 0.0017(14) C7 0.015(2) 0.016(2) 0.015(2) 0.0056(17) 0.0025(18) 0.0015(15) C8 0.012(2) 0.0096(18) 0.024(2) 0.0088(17) -0.0002(18) 0.0028(14) C9 0.012(2) 0.0116(19) 0.021(2) -0.0019(17) 0.0030(18) -0.0012(14) C10 0.017(2) 0.010(2) 0.023(3) 0.0000(16) 0.004(2) 0.0012(14) C11 0.020(2) 0.0100(18) 0.030(3) 0.0002(19) 0.007(2) 0.0018(16) C12 0.019(2) 0.016(2) 0.022(3) -0.0009(18) 0.003(2) 0.0023(16) C13 0.013(2) 0.0133(19) 0.019(2) 0.0053(18) 0.0056(18) 0.0036(15) C14 0.016(2) 0.0142(19) 0.013(2) 0.0020(17) 0.0000(18) -0.0037(15) C15 0.013(2) 0.0105(18) 0.017(2) 0.0001(17) 0.0021(18) -0.0004(14) C16 0.016(2) 0.0085(17) 0.013(2) 0.0060(16) 0.0037(17) 0.0003(14) C17 0.018(2) 0.0082(18) 0.015(2) -0.0017(16) 0.0022(18) -0.0002(14) C18 0.015(2) 0.0095(18) 0.017(2) 0.0017(16) 0.0088(18) 0.0011(14) C19 0.016(2) 0.0087(18) 0.019(2) -0.0017(17) 0.0071(18) 0.0020(14) C20 0.020(2) 0.0089(17) 0.013(2) 0.0007(16) 0.0029(18) -0.0024(15) C21 0.019(2) 0.0093(18) 0.015(2) 0.0035(16) 0.0019(18) -0.0011(15) C22 0.016(2) 0.0123(19) 0.018(2) 0.0013(17) 0.0050(19) 0.0028(15) C23 0.015(2) 0.014(2) 0.026(3) -0.0016(19) 0.000(2) -0.0023(16) C24 0.013(2) 0.014(2) 0.023(2) 0.0035(18) 0.0039(19) 0.0023(15) C25 0.019(2) 0.009(2) 0.024(3) 0.0062(17) 0.001(2) 0.0018(14) C26 0.016(2) 0.016(2) 0.018(2) 0.0018(18) 0.0030(19) 0.0020(16) C27 0.016(2) 0.0102(18) 0.017(2) -0.0015(17) 0.0020(18) 0.0003(15) C28 0.0106(19) 0.0134(19) 0.017(2) 0.0041(17) 0.0040(17) 0.0011(14) C29 0.016(2) 0.0123(19) 0.014(2) -0.0045(16) 0.0040(18) -0.0013(15) C30 0.015(2) 0.0114(19) 0.018(2) 0.0004(17) 0.0018(18) 0.0020(15) C31 0.017(2) 0.0075(17) 0.020(2) -0.0011(17) 0.0059(19) 0.0011(15) C32 0.013(2) 0.016(2) 0.014(2) -0.0035(17) 0.0013(18) -0.0013(15) C33 0.0111(19) 0.0111(19) 0.019(2) -0.0009(17) 0.0031(17) 0.0025(14) C34 0.018(2) 0.014(2) 0.019(2) 0.0072(18) 0.0034(19) 0.0032(16) C35 0.022(2) 0.021(2) 0.024(3) 0.008(2) 0.005(2) 0.0044(18) C36 0.021(2) 0.017(2) 0.022(3) 0.0073(19) 0.004(2) -0.0012(17) O1S 0.0261(19) 0.0176(16) 0.025(2) 0.0015(15) 0.0096(16) 0.0006(13) O2S 0.038(2) 0.0179(17) 0.032(2) -0.0029(16) 0.0047(18) 0.0034(15) O3S 0.033(2) 0.0166(16) 0.025(2) 0.0042(13) 0.0112(18) 0.0062(12) _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 2.268(4) . ? Yb1 O5 2.289(4) . ? Yb1 O2 2.292(4) . ? Yb1 O1 2.306(4) . ? Yb1 O4 2.324(4) . ? Yb1 O3 2.332(3) . ? Yb1 N5 2.457(4) . ? Yb1 N1 2.475(4) . ? F1 C5 1.342(4) . ? F2 C6 1.347(5) . ? F3 C7 1.338(5) . ? F4 C8 1.350(5) . ? F5 C17 1.340(5) . ? F6 C18 1.344(5) . ? F7 C19 1.340(5) . ? F8 C20 1.350(5) . ? F9 C29 1.340(5) . ? F10 C30 1.347(5) . ? F11 C31 1.342(5) . ? F12 C32 1.350(5) . ? N1 C1 1.158(6) . ? N2 C2 1.148(6) . ? N3 C11 1.156(7) . ? N4 C12 1.154(6) . ? N5 C13 1.143(6) . ? N6 C14 1.140(6) . ? N7 C23 1.153(6) . ? N8 C24 1.156(6) . ? N9 C25 1.148(7) . ? N10 C26 1.154(6) . ? N11 C35 1.167(7) . ? N12 C36 1.135(7) . ? C1 C3 1.419(6) . ? C2 C3 1.425(7) . ? C3 C4 1.423(6) . ? C4 C6 1.429(5) . ? C4 C5 1.432(7) . ? C5 C7 1.348(7) . ? C6 C8 1.351(7) . ? C7 C9 1.427(6) . ? C8 C9 1.418(7) . ? C9 C10 1.420(6) . ? C10 C12 1.425(6) . ? C10 C11 1.426(7) . ? C13 C15 1.419(6) . ? C14 C15 1.426(7) . ? C15 C16 1.427(6) . ? C16 C18 1.413(6) . ? C16 C17 1.415(6) . ? C17 C19 1.362(6) . ? C18 C20 1.363(6) . ? C19 C21 1.424(6) . ? C20 C21 1.412(6) . ? C21 C22 1.423(6) . ? C22 C24 1.416(6) . ? C22 C23 1.416(7) . ? C25 C27 1.433(7) . ? C26 C27 1.420(6) . ? C27 C28 1.421(6) . ? C28 C30 1.415(6) . ? C28 C29 1.424(6) . ? C29 C31 1.358(7) . ? C30 C32 1.347(6) . ? C31 C33 1.424(6) . ? C32 C33 1.434(6) . ? C33 C34 1.408(6) . ? C34 C35 1.419(7) . ? C34 C36 1.431(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Yb1 O5 98.90(12) . . ? O6 Yb1 O2 88.86(14) . . ? O5 Yb1 O2 148.42(11) . . ? O6 Yb1 O1 143.99(11) . . ? O5 Yb1 O1 81.17(13) . . ? O2 Yb1 O1 109.94(13) . . ? O6 Yb1 O4 71.15(12) . . ? O5 Yb1 O4 76.42(13) . . ? O2 Yb1 O4 77.31(12) . . ? O1 Yb1 O4 141.49(13) . . ? O6 Yb1 O3 142.04(12) . . ? O5 Yb1 O3 77.90(12) . . ? O2 Yb1 O3 77.33(13) . . ? O1 Yb1 O3 73.57(13) . . ? O4 Yb1 O3 71.37(13) . . ? O6 Yb1 N5 72.28(13) . . ? O5 Yb1 N5 72.02(13) . . ? O2 Yb1 N5 138.96(12) . . ? O1 Yb1 N5 73.62(13) . . ? O4 Yb1 N5 126.36(12) . . ? O3 Yb1 N5 138.15(14) . . ? O6 Yb1 N1 83.14(12) . . ? O5 Yb1 N1 141.60(12) . . ? O2 Yb1 N1 69.50(11) . . ? O1 Yb1 N1 75.76(13) . . ? O4 Yb1 N1 138.12(14) . . ? O3 Yb1 N1 122.75(13) . . ? N5 Yb1 N1 72.22(13) . . ? C1 N1 Yb1 175.0(4) . . ? C13 N5 Yb1 171.5(4) . . ? N1 C1 C3 179.2(5) . . ? N2 C2 C3 176.3(5) . . ? C1 C3 C4 120.9(4) . . ? C1 C3 C2 114.9(4) . . ? C4 C3 C2 123.9(4) . . ? C3 C4 C6 124.8(4) . . ? C3 C4 C5 122.7(4) . . ? C6 C4 C5 112.5(4) . . ? F1 C5 C7 118.3(4) . . ? F1 C5 C4 118.2(4) . . ? C7 C5 C4 123.5(4) . . ? F2 C6 C8 118.3(4) . . ? F2 C6 C4 118.0(4) . . ? C8 C6 C4 123.8(4) . . ? F3 C7 C5 117.6(4) . . ? F3 C7 C9 118.6(4) . . ? C5 C7 C9 123.7(4) . . ? F4 C8 C6 118.4(4) . . ? F4 C8 C9 118.0(4) . . ? C6 C8 C9 123.6(4) . . ? C8 C9 C10 125.3(4) . . ? C8 C9 C7 113.0(4) . . ? C10 C9 C7 121.7(4) . . ? C9 C10 C12 123.2(5) . . ? C9 C10 C11 123.3(4) . . ? C12 C10 C11 113.1(4) . . ? N3 C11 C10 177.0(5) . . ? N4 C12 C10 175.0(6) . . ? N5 C13 C15 174.8(5) . . ? N6 C14 C15 175.3(5) . . ? C13 C15 C14 113.4(4) . . ? C13 C15 C16 123.0(4) . . ? C14 C15 C16 123.6(4) . . ? C18 C16 C17 113.6(4) . . ? C18 C16 C15 123.8(4) . . ? C17 C16 C15 122.6(4) . . ? F5 C17 C19 118.0(4) . . ? F5 C17 C16 118.3(4) . . ? C19 C17 C16 123.6(4) . . ? F6 C18 C20 118.4(4) . . ? F6 C18 C16 118.9(4) . . ? C20 C18 C16 122.6(4) . . ? F7 C19 C17 118.1(4) . . ? F7 C19 C21 119.0(4) . . ? C17 C19 C21 122.8(4) . . ? F8 C20 C18 117.0(4) . . ? F8 C20 C21 118.8(4) . . ? C18 C20 C21 124.2(4) . . ? C20 C21 C22 123.6(4) . . ? C20 C21 C19 113.0(4) . . ? C22 C21 C19 123.3(4) . . ? C24 C22 C23 114.1(4) . . ? C24 C22 C21 122.4(4) . . ? C23 C22 C21 123.5(4) . . ? N7 C23 C22 176.9(5) . . ? N8 C24 C22 176.6(5) . . ? N9 C25 C27 177.6(5) . . ? N10 C26 C27 176.1(5) . . ? C26 C27 C28 123.0(4) . . ? C26 C27 C25 115.1(4) . . ? C28 C27 C25 121.6(4) . . ? C30 C28 C27 123.9(4) . . ? C30 C28 C29 113.4(4) . . ? C27 C28 C29 122.7(4) . . ? F9 C29 C31 118.3(4) . . ? F9 C29 C28 118.7(4) . . ? C31 C29 C28 122.9(4) . . ? C32 C30 F10 118.4(4) . . ? C32 C30 C28 123.7(4) . . ? F10 C30 C28 117.9(4) . . ? F11 C31 C29 117.7(4) . . ? F11 C31 C33 118.1(4) . . ? C29 C31 C33 124.1(4) . . ? C30 C32 F12 118.1(4) . . ? C30 C32 C33 123.8(4) . . ? F12 C32 C33 118.0(4) . . ? C34 C33 C31 123.1(4) . . ? C34 C33 C32 124.8(4) . . ? C31 C33 C32 112.2(4) . . ? C33 C34 C35 123.3(5) . . ? C33 C34 C36 122.2(4) . . ? C35 C34 C36 114.3(4) . . ? N11 C35 C34 178.1(5) . . ? N12 C36 C34 179.4(6) . . ? _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.868 _refine_diff_density_max 3.955 _refine_diff_density_min -3.737 _refine_diff_density_rms 0.193 # Attachment 'YDYTF4.CIF' data_g:\nazario\struct~1\nl101\work\ydytf4 _database_code_depnum_ccdc_archive 'CCDC 749370' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Yttrium Dysprosium(III) 2,3,5,6-Tetrafluoro-7,7,8,8-Tetracyanoquinodimethane' ; _chemical_name_common ;Yttrium Dysprosium(iii) 2,3,5,6-Tetrafluoro-7,7,8,8- Tetracyanoquinodimethane' ; _chemical_melting_point ? _chemical_formula_sum 'C36 H18 Dy0.26 F12 N12 O9 Y0.74' _chemical_formula_weight 1099.04 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6435(19) _cell_length_b 17.639(2) _cell_length_c 17.018(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.198(7) _cell_angle_gamma 90.00 _cell_volume 3987.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2177 _exptl_absorpt_coefficient_mu 1.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5673 _exptl_absorpt_correction_T_max 0.8219 _exptl_absorpt_process_details 'SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35568 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.33 _reflns_number_total 9675 _reflns_number_gt 8859 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0276P)^2^+1.6948P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00038(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9675 _refine_ls_number_parameters 687 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0562 _refine_ls_wR_factor_gt 0.0546 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.198400(7) 0.409379(5) 0.935453(5) 0.01030(4) Uani 0.2659(12) 1 d P . . Y1 Y 0.198400(7) 0.409379(5) 0.935453(5) 0.01030(4) Uani 0.7341(12) 1 d P . . F1 F 0.52482(6) 0.30944(5) 1.09457(5) 0.02065(18) Uani 1 1 d . . . F2 F 0.45549(6) 0.12315(5) 1.27434(5) 0.01810(17) Uani 1 1 d . . . F3 F 0.64842(6) 0.10063(5) 1.32828(5) 0.01880(17) Uani 1 1 d . . . F4 F 0.71814(6) 0.28988(5) 1.15064(5) 0.02082(18) Uani 1 1 d . . . F5 F 0.20555(7) 0.15910(5) 1.00130(5) 0.02097(18) Uani 1 1 d . . . F6 F 0.06275(6) -0.00898(5) 0.78868(5) 0.02039(18) Uani 1 1 d . . . F7 F 0.04525(7) -0.11304(5) 0.89497(5) 0.02270(18) Uani 1 1 d . . . F8 F 0.19349(7) 0.05429(5) 1.10612(5) 0.02191(18) Uani 1 1 d . . . F9 F 0.28970(6) 0.53307(5) 0.31804(5) 0.01950(17) Uani 1 1 d . . . F10 F 0.44908(6) 0.36862(5) 0.52840(5) 0.02001(17) Uani 1 1 d . . . F11 F 0.43534(7) 0.47261(5) 0.63496(5) 0.02125(18) Uani 1 1 d . . . F12 F 0.27612(7) 0.63747(5) 0.42403(5) 0.02043(18) Uani 1 1 d . . . O1 O 0.06560(7) 0.49645(6) 0.92760(6) 0.0197(2) Uani 1 1 d D . . O2 O 0.24582(8) 0.47254(6) 1.05760(6) 0.0194(2) Uani 1 1 d D . . O3 O 0.25187(8) 0.52832(6) 0.89802(7) 0.0235(2) Uani 1 1 d D . . O4 O 0.35534(8) 0.39684(6) 0.90865(7) 0.0204(2) Uani 1 1 d D . . O5 O 0.08540(7) 0.35401(6) 1.00341(6) 0.0180(2) Uani 1 1 d D . . O6 O 0.12913(8) 0.41439(6) 0.79754(6) 0.0218(2) Uani 1 1 d D . . O7 O 0.10236(9) 0.64741(6) 0.91944(7) 0.0300(3) Uani 1 1 d D . . O8 O 0.39466(9) 0.59683(6) 1.00839(7) 0.0258(2) Uani 1 1 d D . . O9 O 0.48636(8) 0.51406(6) 0.89725(7) 0.0231(2) Uani 1 1 d D . . N1 N 0.29738(9) 0.32007(7) 1.03620(7) 0.0168(2) Uani 1 1 d . . . N2 N 0.23414(9) 0.18135(7) 1.21667(7) 0.0216(3) Uani 1 1 d . . . N3 N 0.87360(10) 0.08476(7) 1.38234(8) 0.0249(3) Uani 1 1 d . . . N4 N 0.93863(10) 0.25851(8) 1.22949(9) 0.0297(3) Uani 1 1 d . . . N5 N 0.17167(9) 0.27839(7) 0.87780(7) 0.0182(2) Uani 1 1 d . . . N6 N 0.11440(10) 0.12004(8) 0.67904(7) 0.0228(3) Uani 1 1 d . . . N7 N 0.04367(11) -0.22622(8) 1.03692(9) 0.0292(3) Uani 1 1 d . . . N8 N 0.14630(10) -0.06502(8) 1.21831(8) 0.0249(3) Uani 1 1 d . . . N9 N 0.35015(10) 0.41732(7) 0.20795(8) 0.0232(3) Uani 1 1 d . . . N10 N 0.43144(10) 0.25084(7) 0.39292(8) 0.0242(3) Uani 1 1 d . . . N11 N 0.39605(11) 0.59654(8) 0.74527(8) 0.0286(3) Uani 1 1 d . . . N12 N 0.30046(12) 0.75780(8) 0.55449(9) 0.0311(3) Uani 1 1 d . . . C1 C 0.33593(10) 0.28245(8) 1.08927(8) 0.0154(3) Uani 1 1 d . . . C2 C 0.37541(10) 0.23412(7) 1.15526(8) 0.0150(3) Uani 1 1 d . . . C3 C 0.29968(10) 0.20314(8) 1.19089(8) 0.0165(3) Uani 1 1 d . . . C4 C 0.47975(10) 0.22019(7) 1.18383(8) 0.0143(2) Uani 1 1 d . . . C5 C 0.55436(10) 0.25869(7) 1.15367(8) 0.0154(3) Uani 1 1 d . . . C6 C 0.51934(10) 0.16631(7) 1.24438(8) 0.0145(2) Uani 1 1 d . . . C7 C 0.65480(10) 0.24815(8) 1.18272(8) 0.0157(3) Uani 1 1 d . . . C8 C 0.61963(10) 0.15481(7) 1.27238(8) 0.0150(3) Uani 1 1 d . . . C9 C 0.69479(10) 0.19588(7) 1.24495(8) 0.0148(3) Uani 1 1 d . . . C10 C 0.79920(10) 0.18474(8) 1.27556(8) 0.0164(3) Uani 1 1 d . . . C11 C 0.87478(11) 0.22627(8) 1.24877(9) 0.0200(3) Uani 1 1 d . . . C12 C 0.83830(10) 0.12934(8) 1.33490(9) 0.0186(3) Uani 1 1 d . . . C13 C 0.15802(10) 0.21656(8) 0.85723(8) 0.0160(3) Uani 1 1 d . . . C14 C 0.14020(10) 0.13985(8) 0.83216(8) 0.0157(3) Uani 1 1 d . . . C15 C 0.12322(10) 0.12751(8) 0.74720(8) 0.0175(3) Uani 1 1 d . . . C16 C 0.13226(10) 0.08215(7) 0.88847(8) 0.0148(3) Uani 1 1 d . . . C17 C 0.16352(10) 0.09295(7) 0.97303(8) 0.0159(3) Uani 1 1 d . . . C18 C 0.09390(10) 0.00815(8) 0.86704(8) 0.0159(3) Uani 1 1 d . . . C19 C 0.15717(10) 0.03819(8) 1.02803(8) 0.0162(3) Uani 1 1 d . . . C20 C 0.08557(10) -0.04619(8) 0.92225(8) 0.0166(3) Uani 1 1 d . . . C21 C 0.11760(10) -0.03512(8) 1.00688(8) 0.0153(3) Uani 1 1 d . . . C22 C 0.11221(11) -0.09104(7) 1.06564(9) 0.0173(3) Uani 1 1 d . . . C23 C 0.13281(11) -0.07506(8) 1.15007(9) 0.0186(3) Uani 1 1 d . . . C24 C 0.07406(11) -0.16542(8) 1.04652(9) 0.0205(3) Uani 1 1 d . . . C25 C 0.36069(11) 0.40548(8) 0.27569(9) 0.0177(3) Uani 1 1 d . . . C26 C 0.37684(10) 0.38862(8) 0.35929(8) 0.0162(3) Uani 1 1 d . . . C27 C 0.40776(10) 0.31283(8) 0.37997(8) 0.0179(3) Uani 1 1 d . . . C28 C 0.37028(10) 0.44495(7) 0.41734(8) 0.0146(2) Uani 1 1 d . . . C29 C 0.32828(10) 0.51750(8) 0.39622(8) 0.0157(3) Uani 1 1 d . . . C30 C 0.40425(10) 0.43444(8) 0.50174(8) 0.0154(3) Uani 1 1 d . . . C31 C 0.32114(10) 0.57187(8) 0.45136(8) 0.0158(3) Uani 1 1 d . . . C32 C 0.35515(10) 0.56159(8) 0.53571(8) 0.0154(3) Uani 1 1 d . . . C33 C 0.39729(10) 0.48864(8) 0.55691(8) 0.0162(3) Uani 1 1 d . . . C34 C 0.34706(11) 0.61888(8) 0.59230(8) 0.0181(3) Uani 1 1 d . . . C35 C 0.32023(12) 0.69521(9) 0.56967(9) 0.0217(3) Uani 1 1 d . . . C36 C 0.37469(11) 0.60564(8) 0.67689(9) 0.0208(3) Uani 1 1 d . . . H1A H 0.0009(8) 0.4807(8) 0.9219(11) 0.025 Uiso 1 1 d D . . H2A H 0.2050(11) 0.5108(8) 1.0692(10) 0.025 Uiso 1 1 d D . . H3A H 0.2944(11) 0.5564(9) 0.9359(7) 0.025 Uiso 1 1 d D . . H4A H 0.3919(12) 0.4381(6) 0.8997(11) 0.025 Uiso 1 1 d D . . H5A H 0.0908(13) 0.3657(9) 1.0566(6) 0.025 Uiso 1 1 d D . . H6A H 0.1504(13) 0.3804(7) 0.7640(9) 0.025 Uiso 1 1 d D . . H7A H 0.0816(13) 0.6744(9) 0.8734(6) 0.025 Uiso 1 1 d D . . H8A H 0.3784(13) 0.6436(6) 1.0266(10) 0.025 Uiso 1 1 d D . . H9A H 0.4750(13) 0.5491(8) 0.9342(7) 0.025 Uiso 1 1 d D . . H1B H 0.0716(12) 0.5476(5) 0.9213(11) 0.025 Uiso 1 1 d D . . H2B H 0.2845(11) 0.4519(9) 1.1033(8) 0.025 Uiso 1 1 d D . . H3B H 0.2258(12) 0.5535(9) 0.8512(6) 0.025 Uiso 1 1 d D . . H4B H 0.3869(12) 0.3518(5) 0.9056(11) 0.025 Uiso 1 1 d D . . H5B H 0.0453(12) 0.3127(7) 0.9881(9) 0.025 Uiso 1 1 d D . . H6B H 0.1140(13) 0.4606(6) 0.7740(10) 0.025 Uiso 1 1 d D . . H7B H 0.1392(12) 0.6739(9) 0.9618(7) 0.025 Uiso 1 1 d D . . H8B H 0.4130(13) 0.5628(7) 1.0503(8) 0.025 Uiso 1 1 d D . . H9B H 0.4695(13) 0.5333(9) 0.8459(5) 0.025 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01076(5) 0.00968(6) 0.00996(5) 0.00093(3) 0.00132(3) 0.00020(3) Y1 0.01076(5) 0.00968(6) 0.00996(5) 0.00093(3) 0.00132(3) 0.00020(3) F1 0.0196(4) 0.0215(4) 0.0195(4) 0.0105(3) 0.0016(3) -0.0002(3) F2 0.0180(4) 0.0188(4) 0.0184(4) 0.0054(3) 0.0059(3) -0.0007(3) F3 0.0188(4) 0.0187(4) 0.0182(4) 0.0081(3) 0.0029(3) 0.0023(3) F4 0.0179(4) 0.0219(4) 0.0227(4) 0.0079(3) 0.0047(3) -0.0028(3) F5 0.0309(5) 0.0136(4) 0.0160(4) -0.0020(3) 0.0003(3) -0.0065(3) F6 0.0250(4) 0.0201(4) 0.0140(4) -0.0039(3) 0.0001(3) -0.0042(3) F7 0.0299(5) 0.0148(4) 0.0215(4) -0.0037(3) 0.0021(4) -0.0076(3) F8 0.0325(5) 0.0177(4) 0.0134(4) -0.0016(3) 0.0008(3) -0.0060(3) F9 0.0273(4) 0.0180(4) 0.0119(4) 0.0021(3) 0.0019(3) 0.0031(3) F10 0.0242(4) 0.0168(4) 0.0178(4) 0.0033(3) 0.0021(3) 0.0051(3) F11 0.0274(4) 0.0226(4) 0.0118(4) 0.0008(3) 0.0006(3) 0.0031(3) F12 0.0282(4) 0.0135(4) 0.0191(4) 0.0018(3) 0.0045(3) 0.0040(3) O1 0.0157(5) 0.0153(5) 0.0272(5) 0.0005(4) 0.0031(4) 0.0017(4) O2 0.0209(5) 0.0182(5) 0.0173(5) -0.0028(4) 0.0004(4) 0.0026(4) O3 0.0197(5) 0.0180(5) 0.0308(6) 0.0092(4) 0.0018(4) -0.0011(4) O4 0.0184(5) 0.0162(5) 0.0288(6) 0.0024(4) 0.0099(4) 0.0009(4) O5 0.0189(5) 0.0181(5) 0.0174(5) -0.0003(4) 0.0050(4) -0.0043(4) O6 0.0285(6) 0.0214(5) 0.0144(5) 0.0019(4) 0.0026(4) 0.0091(4) O7 0.0381(7) 0.0190(6) 0.0305(6) 0.0039(5) 0.0026(5) -0.0025(5) O8 0.0359(6) 0.0195(5) 0.0242(6) -0.0016(4) 0.0114(5) -0.0032(4) O9 0.0291(6) 0.0203(5) 0.0215(5) 0.0005(4) 0.0093(4) -0.0011(4) N1 0.0163(5) 0.0168(6) 0.0170(5) 0.0013(5) 0.0029(4) 0.0007(4) N2 0.0212(6) 0.0250(6) 0.0188(6) 0.0003(5) 0.0049(5) -0.0013(5) N3 0.0174(6) 0.0262(7) 0.0286(7) 0.0085(5) 0.0002(5) -0.0011(5) N4 0.0213(6) 0.0313(7) 0.0352(8) 0.0106(6) 0.0038(6) -0.0026(5) N5 0.0238(6) 0.0165(6) 0.0139(5) 0.0012(4) 0.0032(5) -0.0004(4) N6 0.0256(6) 0.0244(6) 0.0174(6) -0.0008(5) 0.0028(5) 0.0038(5) N7 0.0350(8) 0.0210(7) 0.0298(7) 0.0011(5) 0.0035(6) -0.0086(6) N8 0.0322(7) 0.0216(6) 0.0220(6) -0.0005(5) 0.0082(5) -0.0025(5) N9 0.0269(7) 0.0244(7) 0.0172(6) -0.0030(5) 0.0030(5) 0.0015(5) N10 0.0281(7) 0.0184(6) 0.0262(7) -0.0014(5) 0.0064(5) 0.0002(5) N11 0.0348(8) 0.0299(7) 0.0191(7) -0.0049(5) 0.0018(6) 0.0038(6) N12 0.0474(9) 0.0185(7) 0.0289(7) -0.0036(5) 0.0121(7) -0.0015(6) C1 0.0150(6) 0.0156(6) 0.0161(6) -0.0031(5) 0.0043(5) -0.0014(5) C2 0.0177(6) 0.0136(6) 0.0133(6) 0.0004(5) 0.0029(5) 0.0006(5) C3 0.0192(6) 0.0158(6) 0.0127(6) -0.0007(5) -0.0001(5) 0.0016(5) C4 0.0167(6) 0.0135(6) 0.0122(6) -0.0020(5) 0.0024(5) 0.0003(5) C5 0.0195(6) 0.0129(6) 0.0131(6) 0.0026(5) 0.0019(5) 0.0002(5) C6 0.0183(6) 0.0132(6) 0.0128(6) -0.0001(5) 0.0053(5) -0.0015(5) C7 0.0179(6) 0.0139(6) 0.0159(6) 0.0007(5) 0.0051(5) -0.0017(5) C8 0.0199(6) 0.0124(6) 0.0119(6) 0.0015(5) 0.0024(5) 0.0014(5) C9 0.0170(6) 0.0141(6) 0.0131(6) -0.0018(5) 0.0029(5) -0.0002(5) C10 0.0177(6) 0.0154(6) 0.0155(6) 0.0008(5) 0.0024(5) 0.0000(5) C11 0.0188(7) 0.0188(7) 0.0203(7) 0.0028(5) 0.0001(5) 0.0013(5) C12 0.0149(6) 0.0198(7) 0.0204(7) -0.0001(6) 0.0027(5) -0.0019(5) C13 0.0165(6) 0.0193(7) 0.0119(6) 0.0024(5) 0.0029(5) 0.0015(5) C14 0.0161(6) 0.0152(6) 0.0148(6) -0.0015(5) 0.0015(5) 0.0011(5) C15 0.0175(6) 0.0147(6) 0.0190(7) -0.0002(5) 0.0017(5) 0.0014(5) C16 0.0137(6) 0.0153(6) 0.0143(6) -0.0004(5) 0.0012(5) 0.0015(5) C17 0.0169(6) 0.0125(6) 0.0171(6) -0.0028(5) 0.0017(5) -0.0017(5) C18 0.0154(6) 0.0169(6) 0.0142(6) -0.0038(5) 0.0007(5) 0.0002(5) C19 0.0172(6) 0.0171(6) 0.0135(6) -0.0022(5) 0.0017(5) -0.0002(5) C20 0.0160(6) 0.0128(6) 0.0203(7) -0.0037(5) 0.0029(5) -0.0021(5) C21 0.0135(6) 0.0144(6) 0.0181(6) -0.0002(5) 0.0036(5) 0.0004(5) C22 0.0172(6) 0.0158(7) 0.0188(7) -0.0005(5) 0.0039(5) -0.0010(5) C23 0.0190(7) 0.0142(6) 0.0232(7) 0.0016(5) 0.0062(6) -0.0010(5) C24 0.0213(7) 0.0194(7) 0.0201(7) 0.0015(5) 0.0032(6) -0.0019(5) C25 0.0169(6) 0.0162(6) 0.0199(7) -0.0038(5) 0.0037(5) 0.0001(5) C26 0.0171(6) 0.0152(6) 0.0161(6) -0.0005(5) 0.0034(5) -0.0002(5) C27 0.0180(6) 0.0189(7) 0.0170(6) -0.0027(5) 0.0043(5) -0.0020(5) C28 0.0142(6) 0.0143(6) 0.0153(6) 0.0000(5) 0.0036(5) -0.0017(5) C29 0.0170(6) 0.0173(6) 0.0121(6) 0.0020(5) 0.0022(5) -0.0011(5) C30 0.0149(6) 0.0143(6) 0.0163(6) 0.0028(5) 0.0025(5) 0.0008(5) C31 0.0174(6) 0.0125(6) 0.0175(6) 0.0016(5) 0.0041(5) 0.0000(5) C32 0.0146(6) 0.0159(6) 0.0156(6) -0.0011(5) 0.0030(5) -0.0026(5) C33 0.0155(6) 0.0198(7) 0.0124(6) 0.0021(5) 0.0016(5) -0.0016(5) C34 0.0191(7) 0.0182(7) 0.0170(6) -0.0020(5) 0.0040(5) -0.0021(5) C35 0.0257(7) 0.0215(8) 0.0188(7) -0.0058(5) 0.0068(6) -0.0041(6) C36 0.0213(7) 0.0196(7) 0.0213(7) -0.0058(6) 0.0041(6) -0.0002(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 Dy1 O4 2.2995(11) . ? Dy1 O2 2.3166(10) . ? Dy1 O6 2.3230(11) . ? Dy1 O5 2.3414(10) . ? Dy1 O1 2.3556(10) . ? Dy1 O3 2.3562(11) . ? Dy1 N1 2.4875(12) . ? Dy1 N5 2.5042(12) . ? F1 C5 1.3381(15) . ? F2 C6 1.3422(15) . ? F3 C8 1.3424(15) . ? F4 C7 1.3424(15) . ? F5 C17 1.3400(15) . ? F6 C18 1.3385(15) . ? F7 C20 1.3386(15) . ? F8 C19 1.3385(15) . ? F9 C29 1.3428(15) . ? F10 C30 1.3421(15) . ? F11 C33 1.3412(15) . ? F12 C31 1.3424(15) . ? N1 C1 1.1471(18) . ? N2 C3 1.1484(19) . ? N3 C12 1.1508(19) . ? N4 C11 1.149(2) . ? N5 C13 1.1475(19) . ? N6 C15 1.1461(19) . ? N7 C24 1.148(2) . ? N8 C23 1.1473(19) . ? N9 C25 1.1478(19) . ? N10 C27 1.1471(19) . ? N11 C36 1.144(2) . ? N12 C35 1.152(2) . ? C1 C2 1.4148(19) . ? C2 C4 1.4168(18) . ? C2 C3 1.4212(19) . ? C4 C5 1.4140(19) . ? C4 C6 1.4152(18) . ? C5 C7 1.3591(19) . ? C6 C8 1.3575(19) . ? C7 C9 1.4161(19) . ? C8 C9 1.4188(19) . ? C9 C10 1.4144(19) . ? C10 C12 1.4189(19) . ? C10 C11 1.422(2) . ? C13 C14 1.4229(19) . ? C14 C16 1.4190(19) . ? C14 C15 1.4277(19) . ? C16 C17 1.4173(19) . ? C16 C18 1.4226(18) . ? C17 C19 1.3614(19) . ? C18 C20 1.365(2) . ? C19 C21 1.4157(19) . ? C20 C21 1.4199(19) . ? C21 C22 1.4184(19) . ? C22 C24 1.4214(19) . ? C22 C23 1.428(2) . ? C25 C26 1.4206(19) . ? C26 C28 1.4183(19) . ? C26 C27 1.4217(19) . ? C28 C29 1.4145(18) . ? C28 C30 1.4172(18) . ? C29 C31 1.3606(19) . ? C30 C33 1.3583(19) . ? C31 C32 1.4158(19) . ? C32 C34 1.4175(19) . ? C32 C33 1.4219(19) . ? C34 C36 1.422(2) . ? C34 C35 1.425(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Dy1 O2 98.18(4) . . ? O4 Dy1 O6 89.18(4) . . ? O2 Dy1 O6 148.66(4) . . ? O4 Dy1 O5 143.69(4) . . ? O2 Dy1 O5 80.67(4) . . ? O6 Dy1 O5 110.67(4) . . ? O4 Dy1 O1 142.23(4) . . ? O2 Dy1 O1 77.94(4) . . ? O6 Dy1 O1 77.74(4) . . ? O5 Dy1 O1 73.46(4) . . ? O4 Dy1 O3 70.87(4) . . ? O2 Dy1 O3 76.95(4) . . ? O6 Dy1 O3 76.86(4) . . ? O5 Dy1 O3 141.66(4) . . ? O1 Dy1 O3 71.68(4) . . ? O4 Dy1 N1 72.08(4) . . ? O2 Dy1 N1 71.92(4) . . ? O6 Dy1 N1 138.77(4) . . ? O5 Dy1 N1 73.17(4) . . ? O1 Dy1 N1 137.86(4) . . ? O3 Dy1 N1 126.68(4) . . ? O4 Dy1 N5 83.83(4) . . ? O2 Dy1 N5 141.37(4) . . ? O6 Dy1 N5 69.51(4) . . ? O5 Dy1 N5 75.83(4) . . ? O1 Dy1 N5 122.55(4) . . ? O3 Dy1 N5 137.90(4) . . ? N1 Dy1 N5 72.14(4) . . ? C1 N1 Dy1 171.20(11) . . ? C13 N5 Dy1 174.49(11) . . ? N1 C1 C2 175.24(14) . . ? C1 C2 C4 123.19(12) . . ? C1 C2 C3 112.84(12) . . ? C4 C2 C3 123.94(12) . . ? N2 C3 C2 175.52(15) . . ? C5 C4 C6 113.58(12) . . ? C5 C4 C2 122.85(12) . . ? C6 C4 C2 123.56(12) . . ? F1 C5 C7 118.07(12) . . ? F1 C5 C4 118.41(12) . . ? C7 C5 C4 123.50(12) . . ? F2 C6 C8 118.13(12) . . ? F2 C6 C4 118.99(12) . . ? C8 C6 C4 122.86(12) . . ? F4 C7 C5 117.79(12) . . ? F4 C7 C9 119.16(12) . . ? C5 C7 C9 123.05(12) . . ? F3 C8 C6 117.62(12) . . ? F3 C8 C9 118.70(12) . . ? C6 C8 C9 123.68(12) . . ? C10 C9 C7 123.34(12) . . ? C10 C9 C8 123.42(12) . . ? C7 C9 C8 113.23(12) . . ? C9 C10 C12 122.76(12) . . ? C9 C10 C11 123.60(12) . . ? C12 C10 C11 113.62(12) . . ? N4 C11 C10 177.31(16) . . ? N3 C12 C10 177.35(15) . . ? N5 C13 C14 179.37(16) . . ? C16 C14 C13 120.91(12) . . ? C16 C14 C15 123.71(12) . . ? C13 C14 C15 115.19(12) . . ? N6 C15 C14 176.09(16) . . ? C17 C16 C14 122.53(12) . . ? C17 C16 C18 113.05(12) . . ? C14 C16 C18 124.42(12) . . ? F5 C17 C19 117.39(12) . . ? F5 C17 C16 119.11(12) . . ? C19 C17 C16 123.44(12) . . ? F6 C18 C20 118.04(12) . . ? F6 C18 C16 118.50(12) . . ? C20 C18 C16 123.46(12) . . ? F8 C19 C17 117.70(12) . . ? F8 C19 C21 118.65(12) . . ? C17 C19 C21 123.62(13) . . ? F7 C20 C18 118.16(12) . . ? F7 C20 C21 118.68(12) . . ? C18 C20 C21 123.16(12) . . ? C19 C21 C22 122.28(13) . . ? C19 C21 C20 113.25(12) . . ? C22 C21 C20 124.47(12) . . ? C21 C22 C24 123.76(13) . . ? C21 C22 C23 122.83(12) . . ? C24 C22 C23 112.97(12) . . ? N8 C23 C22 176.70(16) . . ? N7 C24 C22 175.05(16) . . ? N9 C25 C26 177.65(16) . . ? C28 C26 C25 122.07(12) . . ? C28 C26 C27 123.27(12) . . ? C25 C26 C27 114.47(12) . . ? N10 C27 C26 176.81(15) . . ? C29 C28 C30 113.30(12) . . ? C29 C28 C26 122.90(12) . . ? C30 C28 C26 123.80(12) . . ? F9 C29 C31 117.75(12) . . ? F9 C29 C28 118.76(12) . . ? C31 C29 C28 123.44(12) . . ? F10 C30 C33 118.27(12) . . ? F10 C30 C28 118.30(12) . . ? C33 C30 C28 123.38(12) . . ? F12 C31 C29 117.89(12) . . ? F12 C31 C32 118.66(12) . . ? C29 C31 C32 123.40(13) . . ? C31 C32 C34 122.64(13) . . ? C31 C32 C33 113.14(12) . . ? C34 C32 C33 124.22(13) . . ? F11 C33 C30 117.63(12) . . ? F11 C33 C32 119.00(12) . . ? C30 C33 C32 123.34(12) . . ? C32 C34 C36 121.82(13) . . ? C32 C34 C35 123.01(13) . . ? C36 C34 C35 114.91(12) . . ? N12 C35 C34 177.23(16) . . ? N11 C36 C34 178.46(17) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.386 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.055 # Attachment 'YGdTCNQF4.CIF' data_g:\nazari~1\nazari~1\crysta~1\nl103y~1\mono _database_code_depnum_ccdc_archive 'CCDC 749371' _audit_creation_method SHELXL-97 _chemical_name_systematic ;Yttrium Gadolinium(III) 2,3,5,6-Tetrafluoro-7,7,8,8-Tetracyanoquinodimethane' ; _chemical_name_common ;Yttrium Gadolinium(iii) 2,3,5,6-Tetrafluoro-7,7,8,8- Tetracyanoquinodimethane' ; _chemical_melting_point ? _chemical_formula_sum 'C36 H18 F12 Gd0.28 N12 O9 Y0.72' _chemical_formula_weight 1098.84 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.668(3) _cell_length_b 17.670(3) _cell_length_c 17.065(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.126(11) _cell_angle_gamma 90.00 _cell_volume 4013.6(17) _cell_formula_units_Z 4 _cell_measurement_temperature 383(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 1.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6427 _exptl_absorpt_correction_T_max 0.8153 _exptl_absorpt_process_details 'SADABS, 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 383(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34184 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.27 _reflns_number_total 9602 _reflns_number_gt 8137 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0393P)^2^+3.9198P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9602 _refine_ls_number_parameters 671 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.067 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.301507(12) 0.409511(8) 0.064707(9) 0.01098(6) Uani 0.280(2) 1 d P . . Y1 Y 0.301507(12) 0.409511(8) 0.064707(9) 0.01098(6) Uani 0.720(2) 1 d P . . F1 F 0.29472(11) 0.15901(7) -0.00135(8) 0.0210(3) Uani 1 1 d . . . F2 F 0.30682(11) 0.05420(8) -0.10594(8) 0.0222(3) Uani 1 1 d . . . F3 F 0.45447(11) -0.11315(8) 0.10503(9) 0.0232(3) Uani 1 1 d . . . F4 F 0.43688(11) -0.00920(8) 0.21125(8) 0.0209(3) Uani 1 1 d . . . F5 F -0.02520(10) 0.30943(8) -0.09472(8) 0.0218(3) Uani 1 1 d . . . F6 F -0.21855(10) 0.28970(8) -0.15072(8) 0.0216(3) Uani 1 1 d . . . F7 F -0.14891(10) 0.10070(7) -0.32843(8) 0.0196(3) Uani 1 1 d . . . F8 F 0.04402(10) 0.12311(8) -0.27437(8) 0.0192(3) Uani 1 1 d . . . F9 F 0.05098(10) 0.13147(7) -0.02845(8) 0.0204(3) Uani 1 1 d . . . F10 F 0.06473(11) 0.02759(8) -0.13500(8) 0.0217(3) Uani 1 1 d . . . F11 F 0.22350(11) -0.13744(7) 0.07567(8) 0.0213(3) Uani 1 1 d . . . F12 F 0.20991(11) -0.03311(8) 0.18175(8) 0.0201(3) Uani 1 1 d . . . O1 O 0.41485(12) 0.35385(9) -0.00391(10) 0.0187(3) Uani 1 1 d D . . O2 O 0.14371(13) 0.39710(9) 0.09099(11) 0.0218(4) Uani 1 1 d D . . O3 O 0.25414(13) 0.47280(9) -0.05806(10) 0.0202(4) Uani 1 1 d D . . O4 O 0.24747(13) 0.52874(10) 0.10217(12) 0.0243(4) Uani 1 1 d D . . O5 O 0.43442(12) 0.49677(9) 0.07239(11) 0.0197(3) Uani 1 1 d D . . O6 O 0.37074(14) 0.41440(10) 0.20326(11) 0.0226(4) Uani 1 1 d D . . O7 O 0.01308(14) 0.51439(10) 0.10242(11) 0.0247(4) Uiso 1 1 d D . . O8 O 0.10541(14) 0.59715(10) -0.00867(11) 0.0265(4) Uiso 1 1 d D . . O9 O 0.39767(15) 0.64765(11) 0.08076(12) 0.0305(4) Uiso 1 1 d D . . N1 N 0.32836(15) 0.27831(11) 0.12242(12) 0.0187(4) Uani 1 1 d . . . N2 N 0.38577(16) 0.11991(12) 0.32081(13) 0.0236(4) Uani 1 1 d . . . N3 N 0.45579(18) -0.22637(13) -0.03657(14) 0.0297(5) Uani 1 1 d . . . N4 N 0.35425(17) -0.06512(12) -0.21830(13) 0.0257(5) Uani 1 1 d . . . N5 N 0.20211(14) 0.31985(11) -0.03637(12) 0.0179(4) Uani 1 1 d . . . N6 N 0.26570(16) 0.18116(12) -0.21685(13) 0.0233(4) Uani 1 1 d . . . N7 N -0.43892(17) 0.25836(13) -0.22934(15) 0.0302(5) Uani 1 1 d . . . N8 N -0.37370(16) 0.08471(12) -0.38197(14) 0.0252(5) Uani 1 1 d . . . N9 N 0.06858(16) 0.24914(12) 0.10703(13) 0.0238(5) Uani 1 1 d . . . N10 N 0.14995(17) 0.08274(12) 0.29184(13) 0.0243(5) Uani 1 1 d . . . N11 N 0.19916(19) -0.25758(13) -0.05486(14) 0.0321(5) Uani 1 1 d . . . N12 N 0.10394(19) -0.09626(13) -0.24538(14) 0.0296(5) Uani 1 1 d . . . C1 C 0.34185(17) 0.21632(13) 0.14278(13) 0.0162(4) Uani 1 1 d . . . C2 C 0.35995(17) 0.13957(13) 0.16768(13) 0.0159(4) Uani 1 1 d . . . C3 C 0.37666(17) 0.12744(12) 0.25262(14) 0.0180(5) Uani 1 1 d . . . C4 C 0.36776(16) 0.08206(12) 0.11142(14) 0.0153(4) Uani 1 1 d . . . C5 C 0.33686(17) 0.09265(12) 0.02683(14) 0.0164(4) Uani 1 1 d . . . C6 C 0.40597(17) 0.00805(13) 0.13279(14) 0.0162(4) Uani 1 1 d . . . C7 C 0.34276(17) 0.03820(13) -0.02802(14) 0.0164(4) Uani 1 1 d . . . C8 C 0.41438(17) -0.04613(12) 0.07767(14) 0.0174(5) Uani 1 1 d . . . C9 C 0.38240(16) -0.03512(12) -0.00697(14) 0.0161(4) Uani 1 1 d . . . C10 C 0.38781(18) -0.09103(12) -0.06552(14) 0.0178(5) Uani 1 1 d . . . C11 C 0.36726(18) -0.07525(13) -0.14978(15) 0.0193(5) Uani 1 1 d . . . C12 C 0.42568(18) -0.16561(14) -0.04637(15) 0.0204(5) Uani 1 1 d . . . C13 C 0.16368(17) 0.28228(12) -0.08933(14) 0.0156(4) Uani 1 1 d . . . C14 C 0.12428(17) 0.23404(12) -0.15532(13) 0.0157(4) Uani 1 1 d . . . C15 C 0.19965(17) 0.20299(13) -0.19072(13) 0.0168(4) Uani 1 1 d . . . C16 C 0.01964(17) 0.22022(12) -0.18378(13) 0.0145(4) Uani 1 1 d . . . C17 C -0.05483(17) 0.25863(12) -0.15378(13) 0.0154(4) Uani 1 1 d . . . C18 C -0.01959(17) 0.16618(12) -0.24433(13) 0.0155(4) Uani 1 1 d . . . C19 C -0.15523(17) 0.24809(12) -0.18279(14) 0.0154(4) Uani 1 1 d . . . C20 C -0.19492(17) 0.19574(12) -0.24488(13) 0.0159(4) Uani 1 1 d . . . C21 C -0.11994(18) 0.15478(12) -0.27260(13) 0.0163(4) Uani 1 1 d . . . C22 C -0.29950(17) 0.18465(13) -0.27562(14) 0.0171(4) Uani 1 1 d . . . C23 C -0.37482(18) 0.22634(14) -0.24887(15) 0.0208(5) Uani 1 1 d . . . C24 C -0.33854(17) 0.12914(13) -0.33500(15) 0.0189(5) Uani 1 1 d . . . C25 C 0.09243(17) 0.18730(13) 0.11988(14) 0.0179(5) Uani 1 1 d . . . C26 C 0.12319(17) 0.11120(13) 0.14068(14) 0.0157(4) Uani 1 1 d . . . C27 C 0.13903(17) 0.09460(13) 0.22404(15) 0.0180(5) Uani 1 1 d . . . C28 C 0.12966(16) 0.05525(12) 0.08266(14) 0.0153(4) Uani 1 1 d . . . C29 C 0.09582(17) 0.06556(13) -0.00192(14) 0.0162(4) Uani 1 1 d . . . C30 C 0.17156(17) -0.01750(13) 0.10368(13) 0.0155(4) Uani 1 1 d . . . C31 C 0.10262(17) 0.01150(13) -0.05700(13) 0.0165(4) Uani 1 1 d . . . C32 C 0.17852(17) -0.07161(12) 0.04832(14) 0.0170(5) Uani 1 1 d . . . C33 C 0.14482(16) -0.06141(13) -0.03598(13) 0.0152(4) Uani 1 1 d . . . C34 C 0.15266(18) -0.11864(13) -0.09240(14) 0.0175(5) Uani 1 1 d . . . C35 C 0.12520(19) -0.10547(13) -0.17695(15) 0.0215(5) Uani 1 1 d . . . C36 C 0.17963(19) -0.19501(14) -0.06997(14) 0.0212(5) Uani 1 1 d . . . H1A H 0.407(2) 0.3662(15) -0.0572(8) 0.032 Uiso 1 1 d D . . H2A H 0.1133(19) 0.3512(7) 0.0895(19) 0.032 Uiso 1 1 d D . . H3A H 0.2142(19) 0.4522(15) -0.1036(11) 0.032 Uiso 1 1 d D . . H4A H 0.273(2) 0.5527(14) 0.1503(9) 0.032 Uiso 1 1 d D . . H5A H 0.4994(10) 0.4826(14) 0.0743(19) 0.032 Uiso 1 1 d D . . H6A H 0.4335(11) 0.3979(14) 0.2009(19) 0.032 Uiso 1 1 d D . . H7A H 0.023(2) 0.5503(12) 0.0653(11) 0.032 Uiso 1 1 d D . . H8A H 0.129(2) 0.6425(9) -0.0245(15) 0.032 Uiso 1 1 d D . . H9A H 0.363(2) 0.6735(13) 0.0375(10) 0.032 Uiso 1 1 d D . . H1B H 0.4546(19) 0.3120(11) 0.0105(15) 0.032 Uiso 1 1 d D . . H2B H 0.1059(18) 0.4376(9) 0.0992(19) 0.032 Uiso 1 1 d D . . H3B H 0.2911(19) 0.5136(12) -0.0690(15) 0.032 Uiso 1 1 d D . . H4B H 0.209(2) 0.5590(13) 0.0640(12) 0.032 Uiso 1 1 d D . . H5B H 0.4283(19) 0.5479(7) 0.0806(19) 0.032 Uiso 1 1 d D . . H6B H 0.3719(19) 0.4608(10) 0.2281(17) 0.032 Uiso 1 1 d D . . H7B H 0.033(2) 0.5323(14) 0.1544(7) 0.032 Uiso 1 1 d D . . H8B H 0.083(2) 0.5647(12) -0.0513(12) 0.032 Uiso 1 1 d D . . H9B H 0.417(2) 0.6748(13) 0.1273(9) 0.032 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01119(9) 0.00953(9) 0.01135(9) -0.00100(6) 0.00075(6) -0.00020(6) Y1 0.01119(9) 0.00953(9) 0.01135(9) -0.00100(6) 0.00075(6) -0.00020(6) F1 0.0302(8) 0.0133(6) 0.0174(7) 0.0021(5) 0.0009(6) 0.0064(6) F2 0.0323(8) 0.0180(7) 0.0141(7) 0.0015(5) 0.0007(6) 0.0052(6) F3 0.0301(8) 0.0151(6) 0.0223(7) 0.0043(5) 0.0014(6) 0.0079(6) F4 0.0257(7) 0.0197(7) 0.0150(7) 0.0041(5) -0.0002(5) 0.0035(6) F5 0.0205(7) 0.0213(7) 0.0215(7) -0.0114(6) 0.0003(6) -0.0001(6) F6 0.0194(7) 0.0214(7) 0.0234(7) -0.0082(6) 0.0033(6) 0.0025(5) F7 0.0191(7) 0.0180(7) 0.0204(7) -0.0088(5) 0.0017(5) -0.0022(5) F8 0.0185(7) 0.0185(7) 0.0205(7) -0.0055(5) 0.0044(5) 0.0004(5) F9 0.0242(7) 0.0158(7) 0.0198(7) 0.0039(5) 0.0018(6) 0.0042(5) F10 0.0270(8) 0.0232(7) 0.0127(6) 0.0006(5) 0.0001(5) 0.0034(6) F11 0.0286(8) 0.0125(6) 0.0215(7) 0.0025(5) 0.0030(6) 0.0042(5) F12 0.0265(7) 0.0188(7) 0.0137(6) 0.0025(5) 0.0019(5) 0.0040(6) O1 0.0193(8) 0.0172(8) 0.0189(8) 0.0015(6) 0.0032(7) 0.0044(6) O2 0.0202(9) 0.0165(8) 0.0301(10) -0.0039(7) 0.0090(7) -0.0006(6) O3 0.0218(9) 0.0171(8) 0.0189(8) 0.0026(6) -0.0014(7) -0.0021(6) O4 0.0202(9) 0.0183(8) 0.0325(10) -0.0082(7) 0.0021(7) 0.0001(7) O5 0.0144(8) 0.0160(8) 0.0285(9) 0.0007(7) 0.0042(7) -0.0022(6) O6 0.0237(9) 0.0228(9) 0.0200(9) -0.0036(7) 0.0023(7) -0.0065(7) N1 0.0227(10) 0.0171(10) 0.0153(9) -0.0016(7) 0.0021(8) -0.0002(8) N2 0.0256(11) 0.0234(11) 0.0200(11) 0.0015(8) 0.0016(8) -0.0042(9) N3 0.0356(13) 0.0207(11) 0.0316(12) -0.0008(9) 0.0051(10) 0.0079(9) N4 0.0332(12) 0.0221(11) 0.0222(11) 0.0002(8) 0.0073(9) 0.0022(9) N5 0.0163(10) 0.0179(9) 0.0183(10) -0.0017(8) 0.0015(8) -0.0001(7) N6 0.0242(11) 0.0243(11) 0.0205(10) 0.0001(8) 0.0033(8) 0.0008(8) N7 0.0201(11) 0.0317(12) 0.0376(13) -0.0114(10) 0.0044(10) 0.0035(9) N8 0.0180(10) 0.0259(11) 0.0297(12) -0.0099(9) 0.0010(9) 0.0012(8) N9 0.0252(11) 0.0185(10) 0.0280(11) -0.0009(8) 0.0068(9) -0.0003(8) N10 0.0264(11) 0.0238(11) 0.0207(11) -0.0038(8) 0.0012(9) 0.0024(8) N11 0.0484(15) 0.0186(11) 0.0309(13) -0.0040(9) 0.0122(11) -0.0022(10) N12 0.0357(13) 0.0303(12) 0.0205(11) -0.0061(9) 0.0011(10) 0.0048(10) C1 0.0158(11) 0.0194(11) 0.0126(10) -0.0033(8) 0.0014(8) -0.0020(8) C2 0.0159(11) 0.0160(10) 0.0148(11) 0.0011(8) 0.0012(8) 0.0002(8) C3 0.0173(11) 0.0131(10) 0.0216(12) 0.0002(9) 0.0004(9) -0.0026(8) C4 0.0120(10) 0.0150(10) 0.0174(11) 0.0026(8) 0.0001(8) -0.0021(8) C5 0.0154(11) 0.0129(10) 0.0195(11) 0.0036(8) 0.0010(8) 0.0015(8) C6 0.0135(10) 0.0170(11) 0.0163(11) 0.0040(8) -0.0006(8) -0.0011(8) C7 0.0175(11) 0.0157(10) 0.0148(10) 0.0020(8) 0.0012(8) 0.0011(8) C8 0.0152(11) 0.0126(10) 0.0225(12) 0.0043(8) 0.0001(9) 0.0022(8) C9 0.0127(10) 0.0142(10) 0.0207(11) 0.0019(8) 0.0026(8) -0.0007(8) C10 0.0189(11) 0.0150(11) 0.0192(11) 0.0008(9) 0.0041(9) 0.0006(8) C11 0.0180(11) 0.0143(10) 0.0258(13) -0.0022(9) 0.0053(9) 0.0011(8) C12 0.0214(12) 0.0200(12) 0.0193(11) -0.0018(9) 0.0037(9) 0.0022(9) C13 0.0134(10) 0.0156(10) 0.0180(11) 0.0029(8) 0.0042(8) 0.0004(8) C14 0.0175(11) 0.0146(10) 0.0145(10) 0.0002(8) 0.0026(8) -0.0007(8) C15 0.0186(11) 0.0158(10) 0.0141(10) -0.0001(8) -0.0003(9) -0.0012(8) C16 0.0159(10) 0.0132(10) 0.0136(10) 0.0008(8) 0.0020(8) 0.0008(8) C17 0.0207(11) 0.0122(10) 0.0129(10) -0.0025(8) 0.0029(8) 0.0006(8) C18 0.0197(11) 0.0129(10) 0.0139(10) 0.0000(8) 0.0041(8) 0.0004(8) C19 0.0158(11) 0.0143(10) 0.0166(11) -0.0007(8) 0.0046(8) 0.0032(8) C20 0.0194(11) 0.0129(10) 0.0140(10) 0.0020(8) 0.0010(8) -0.0003(8) C21 0.0225(12) 0.0116(10) 0.0129(10) -0.0013(8) -0.0001(8) -0.0027(8) C22 0.0189(11) 0.0156(10) 0.0158(11) -0.0011(8) 0.0017(9) 0.0004(8) C23 0.0192(12) 0.0199(11) 0.0205(12) -0.0025(9) -0.0014(9) -0.0022(9) C24 0.0135(11) 0.0204(11) 0.0219(12) -0.0005(9) 0.0021(9) 0.0022(9) C25 0.0173(11) 0.0190(11) 0.0175(11) -0.0033(9) 0.0040(9) -0.0015(9) C26 0.0146(11) 0.0155(10) 0.0171(11) 0.0000(8) 0.0036(8) -0.0025(8) C27 0.0159(11) 0.0161(11) 0.0208(12) -0.0043(9) 0.0013(9) 0.0006(8) C28 0.0133(10) 0.0141(10) 0.0175(11) 0.0005(8) 0.0018(8) -0.0016(8) C29 0.0155(11) 0.0129(10) 0.0189(11) 0.0026(8) 0.0014(8) 0.0006(8) C30 0.0144(10) 0.0175(11) 0.0130(10) 0.0018(8) 0.0001(8) -0.0007(8) C31 0.0158(11) 0.0196(11) 0.0128(10) 0.0027(8) 0.0006(8) -0.0026(8) C32 0.0164(11) 0.0121(10) 0.0209(12) 0.0035(8) 0.0011(9) -0.0010(8) C33 0.0148(10) 0.0157(10) 0.0154(11) -0.0014(8) 0.0038(8) -0.0022(8) C34 0.0194(11) 0.0178(11) 0.0159(11) -0.0021(9) 0.0050(9) -0.0025(9) C35 0.0206(12) 0.0190(11) 0.0239(13) -0.0049(9) 0.0028(10) -0.0013(9) C36 0.0251(13) 0.0202(12) 0.0194(12) -0.0065(9) 0.0073(10) -0.0042(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O2 2.3108(18) . ? Gd1 O3 2.3330(17) . ? Gd1 O6 2.3403(19) . ? Gd1 O1 2.3585(17) . ? Gd1 O5 2.3636(16) . ? Gd1 O4 2.3679(17) . ? Gd1 N5 2.503(2) . ? Gd1 N1 2.513(2) . ? F1 C5 1.346(2) . ? F2 C7 1.339(3) . ? F3 C8 1.343(2) . ? F4 C6 1.344(3) . ? F5 C17 1.342(2) . ? F6 C19 1.343(3) . ? F7 C21 1.344(2) . ? F8 C18 1.342(3) . ? F9 C29 1.346(2) . ? F10 C31 1.345(3) . ? F11 C32 1.349(2) . ? F12 C30 1.345(3) . ? N1 C1 1.151(3) . ? N2 C3 1.149(3) . ? N3 C12 1.148(3) . ? N4 C11 1.156(3) . ? N5 C13 1.148(3) . ? N6 C15 1.160(3) . ? N7 C23 1.154(3) . ? N8 C24 1.147(3) . ? N9 C25 1.147(3) . ? N10 C27 1.152(3) . ? N11 C36 1.153(3) . ? N12 C35 1.149(3) . ? C1 C2 1.426(3) . ? C2 C4 1.419(3) . ? C2 C3 1.431(3) . ? C4 C5 1.421(3) . ? C4 C6 1.425(3) . ? C5 C7 1.357(3) . ? C6 C8 1.365(3) . ? C7 C9 1.419(3) . ? C8 C9 1.424(3) . ? C9 C10 1.419(3) . ? C10 C12 1.426(3) . ? C10 C11 1.429(3) . ? C13 C14 1.418(3) . ? C14 C15 1.418(3) . ? C14 C16 1.423(3) . ? C16 C17 1.413(3) . ? C16 C18 1.420(3) . ? C17 C19 1.362(3) . ? C18 C21 1.362(3) . ? C19 C20 1.418(3) . ? C20 C22 1.420(3) . ? C20 C21 1.421(3) . ? C22 C23 1.423(3) . ? C22 C24 1.424(3) . ? C25 C26 1.429(3) . ? C26 C28 1.416(3) . ? C26 C27 1.420(3) . ? C28 C30 1.420(3) . ? C28 C29 1.424(3) . ? C29 C31 1.358(3) . ? C30 C32 1.363(3) . ? C31 C33 1.424(3) . ? C32 C33 1.419(3) . ? C33 C34 1.417(3) . ? C34 C35 1.425(3) . ? C34 C36 1.428(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Gd1 O3 97.98(7) . . ? O2 Gd1 O6 89.34(7) . . ? O3 Gd1 O6 148.83(6) . . ? O2 Gd1 O1 143.52(6) . . ? O3 Gd1 O1 80.42(6) . . ? O6 Gd1 O1 110.89(6) . . ? O2 Gd1 O5 142.24(6) . . ? O3 Gd1 O5 77.89(6) . . ? O6 Gd1 O5 77.91(6) . . ? O1 Gd1 O5 73.52(6) . . ? O2 Gd1 O4 70.73(6) . . ? O3 Gd1 O4 77.05(7) . . ? O6 Gd1 O4 76.93(6) . . ? O1 Gd1 O4 141.75(6) . . ? O5 Gd1 O4 71.79(6) . . ? O2 Gd1 N5 71.90(7) . . ? O3 Gd1 N5 71.83(6) . . ? O6 Gd1 N5 138.69(6) . . ? O1 Gd1 N5 73.07(6) . . ? O5 Gd1 N5 137.83(7) . . ? O4 Gd1 N5 126.54(6) . . ? O2 Gd1 N1 84.03(6) . . ? O3 Gd1 N1 141.28(6) . . ? O6 Gd1 N1 69.42(6) . . ? O1 Gd1 N1 75.88(6) . . ? O5 Gd1 N1 122.55(6) . . ? O4 Gd1 N1 137.88(7) . . ? N5 Gd1 N1 72.20(6) . . ? C1 N1 Gd1 174.35(18) . . ? C13 N5 Gd1 171.17(19) . . ? N1 C1 C2 179.2(3) . . ? C4 C2 C1 120.9(2) . . ? C4 C2 C3 124.0(2) . . ? C1 C2 C3 114.9(2) . . ? N2 C3 C2 176.5(3) . . ? C2 C4 C5 122.8(2) . . ? C2 C4 C6 124.3(2) . . ? C5 C4 C6 112.8(2) . . ? F1 C5 C7 117.3(2) . . ? F1 C5 C4 118.8(2) . . ? C7 C5 C4 123.8(2) . . ? F4 C6 C8 118.1(2) . . ? F4 C6 C4 118.5(2) . . ? C8 C6 C4 123.4(2) . . ? F2 C7 C5 118.0(2) . . ? F2 C7 C9 118.5(2) . . ? C5 C7 C9 123.5(2) . . ? F3 C8 C6 118.1(2) . . ? F3 C8 C9 118.7(2) . . ? C6 C8 C9 123.3(2) . . ? C10 C9 C7 122.4(2) . . ? C10 C9 C8 124.5(2) . . ? C7 C9 C8 113.2(2) . . ? C9 C10 C12 123.8(2) . . ? C9 C10 C11 122.9(2) . . ? C12 C10 C11 112.9(2) . . ? N4 C11 C10 176.6(3) . . ? N3 C12 C10 175.2(3) . . ? N5 C13 C14 175.3(2) . . ? C13 C14 C15 112.9(2) . . ? C13 C14 C16 123.1(2) . . ? C15 C14 C16 124.0(2) . . ? N6 C15 C14 175.4(2) . . ? C17 C16 C18 113.8(2) . . ? C17 C16 C14 123.0(2) . . ? C18 C16 C14 123.2(2) . . ? F5 C17 C19 118.2(2) . . ? F5 C17 C16 118.3(2) . . ? C19 C17 C16 123.5(2) . . ? F8 C18 C21 117.95(19) . . ? F8 C18 C16 119.3(2) . . ? C21 C18 C16 122.8(2) . . ? F6 C19 C17 117.80(19) . . ? F6 C19 C20 119.3(2) . . ? C17 C19 C20 122.9(2) . . ? C19 C20 C22 123.2(2) . . ? C19 C20 C21 113.5(2) . . ? C22 C20 C21 123.3(2) . . ? F7 C21 C18 117.9(2) . . ? F7 C21 C20 118.7(2) . . ? C18 C21 C20 123.5(2) . . ? C20 C22 C23 123.4(2) . . ? C20 C22 C24 122.8(2) . . ? C23 C22 C24 113.8(2) . . ? N7 C23 C22 177.1(3) . . ? N8 C24 C22 177.2(3) . . ? N9 C25 C26 176.7(2) . . ? C28 C26 C27 122.5(2) . . ? C28 C26 C25 123.0(2) . . ? C27 C26 C25 114.4(2) . . ? N10 C27 C26 178.0(3) . . ? C26 C28 C30 122.8(2) . . ? C26 C28 C29 124.2(2) . . ? C30 C28 C29 113.1(2) . . ? F9 C29 C31 118.3(2) . . ? F9 C29 C28 118.0(2) . . ? C31 C29 C28 123.6(2) . . ? F12 C30 C32 118.0(2) . . ? F12 C30 C28 118.69(19) . . ? C32 C30 C28 123.2(2) . . ? F10 C31 C29 117.7(2) . . ? F10 C31 C33 118.9(2) . . ? C29 C31 C33 123.3(2) . . ? F11 C32 C30 117.6(2) . . ? F11 C32 C33 118.6(2) . . ? C30 C32 C33 123.8(2) . . ? C34 C33 C32 122.7(2) . . ? C34 C33 C31 124.3(2) . . ? C32 C33 C31 113.0(2) . . ? C33 C34 C35 121.9(2) . . ? C33 C34 C36 123.2(2) . . ? C35 C34 C36 114.7(2) . . ? N12 C35 C34 178.6(3) . . ? N11 C36 C34 177.2(3) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.707 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.092