# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_kcd791_AquaF _database_code_depnum_ccdc_archive 'CCDC 878246' #TrackingRef 'Ln2Cr2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H21 Cr Dy F26 N3 O9, 0.82(C H2 Cl2)' _chemical_formula_sum 'C35.83 H22.65 Cl1.65 Cr Dy F26 N3 O9' _chemical_formula_weight 1406.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.404(3) _cell_length_b 20.093(3) _cell_length_c 20.130(2) _cell_angle_alpha 88.972(9) _cell_angle_beta 85.810(11) _cell_angle_gamma 83.452(11) _cell_volume 4970.7(14) _cell_formula_units_Z 4 _cell_measurement_temperature 122(1) _cell_measurement_reflns_used 61468 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.67 _exptl_crystal_description Prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.227 _exptl_crystal_size_mid 0.122 _exptl_crystal_size_min 0.091 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2731 _exptl_absorpt_coefficient_mu 1.949 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.733 _exptl_absorpt_correction_T_max 0.877 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 122(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\w and \f scans' _diffrn_reflns_number 184854 _diffrn_reflns_av_R_equivalents 0.1045 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 27.67 _reflns_number_total 22902 _reflns_number_gt 16551 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'COLLECT (Nonius, 1999)' _computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Ortep-3 (Farrugia, 1997) and Mercury (Macrae et. al., 2006) ; _computing_publication_material SHELXL-97 _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^)+(0.0000P)^2^+18.7631P] 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 22902 _refine_ls_number_parameters 1417 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 0.13046(2) 0.185261(12) 0.772492(12) 0.02195(7) Uani 1 1 d . . . Dy2 Dy 0.41218(2) 0.313600(12) 0.280773(12) 0.02457(7) Uani 1 1 d . . . Cr1 Cr -0.04657(8) 0.10992(5) 0.93537(4) 0.0333(2) Uani 1 1 d . . . Cr2 Cr 0.56126(7) 0.39239(4) 0.43501(4) 0.0283(2) Uani 1 1 d . . . O1 O 0.0766(3) 0.0378(2) 0.9197(2) 0.0383(10) Uani 1 1 d D . . H1A H 0.097(5) -0.0001(18) 0.938(3) 0.046 Uiso 1 1 d D . . H1B H 0.137(3) 0.051(3) 0.902(3) 0.046 Uiso 1 1 d D . . O2 O 0.4258(3) 0.4547(2) 0.4290(2) 0.0367(10) Uani 1 1 d D . . H2A H 0.411(5) 0.4912(19) 0.452(3) 0.044 Uiso 1 1 d D . . H2B H 0.406(5) 0.458(3) 0.3877(15) 0.044 Uiso 1 1 d D . . F1 F 0.0166(2) 0.15024(14) 0.85932(14) 0.0285(7) Uani 1 1 d . . . F2 F 0.5049(2) 0.34534(14) 0.36756(14) 0.0275(7) Uani 1 1 d . . . F3 F -0.1094(3) 0.06615(19) 1.00867(18) 0.0521(10) Uani 1 1 d . . . F4 F 0.6123(3) 0.44138(16) 0.50168(16) 0.0390(8) Uani 1 1 d . . . N1 N 0.0446(4) 0.1559(3) 0.9998(2) 0.0418(13) Uani 1 1 d . . . N2 N -0.1656(4) 0.1896(2) 0.9429(2) 0.0351(11) Uani 1 1 d . . . N3 N -0.1433(4) 0.0616(2) 0.8764(3) 0.0402(12) Uani 1 1 d . . . N4 N 0.4852(4) 0.3375(2) 0.5096(2) 0.0320(11) Uani 1 1 d . . . N5 N 0.6947(4) 0.3221(2) 0.4368(2) 0.0279(10) Uani 1 1 d . . . N6 N 0.6420(4) 0.4484(2) 0.3642(2) 0.0336(11) Uani 1 1 d . . . F11 F -0.0670(4) 0.34076(19) 0.93917(17) 0.0572(11) Uani 1 1 d . . . F12 F -0.1437(4) 0.4132(2) 0.8743(2) 0.0797(15) Uani 1 1 d . . . F13 F 0.0152(5) 0.4225(2) 0.9010(2) 0.0869(17) Uani 1 1 d . . . F14 F -0.0421(5) 0.3487(2) 0.6081(2) 0.0885(17) Uani 1 1 d . . . F15 F -0.0034(4) 0.43962(19) 0.6469(2) 0.0735(14) Uani 1 1 d . . . F16 F 0.1216(4) 0.3718(2) 0.6016(2) 0.0750(14) Uani 1 1 d . . . F17 F 0.3761(5) 0.0238(2) 0.8974(3) 0.107(2) Uani 1 1 d . . . F18 F 0.2981(4) 0.0734(3) 0.9835(2) 0.099(2) Uani 1 1 d . . . F19 F 0.4608(3) 0.0856(2) 0.9522(2) 0.0620(11) Uani 1 1 d . . . F20 F 0.4574(4) 0.3194(2) 0.8791(2) 0.0700(13) Uani 1 1 d . . . F21 F 0.3899(4) 0.3478(2) 0.7859(3) 0.0904(18) Uani 1 1 d . . . F22 F 0.5202(4) 0.2708(3) 0.7885(3) 0.0798(14) Uani 1 1 d . . . F23 F 0.1457(5) -0.0638(2) 0.8086(2) 0.099(2) Uani 1 1 d . . . F24 F 0.0751(4) -0.0486(2) 0.7147(3) 0.0871(17) Uani 1 1 d . . . F25 F 0.2384(3) -0.09669(16) 0.71872(19) 0.0545(10) Uani 1 1 d . . . F26 F 0.5320(3) 0.0271(2) 0.6866(3) 0.0764(14) Uani 1 1 d . . . F27 F 0.5236(4) 0.1316(3) 0.7042(4) 0.115(2) Uani 1 1 d . . . F28 F 0.4736(4) 0.0982(3) 0.6153(3) 0.1000(19) Uani 1 1 d . . . F29 F -0.2634(3) 0.1690(2) 0.7334(2) 0.0656(12) Uani 1 1 d . . . F30 F -0.2401(3) 0.2690(2) 0.7077(3) 0.0702(13) Uani 1 1 d . . . F31 F -0.2608(3) 0.1996(2) 0.6318(2) 0.0654(12) Uani 1 1 d . . . F32 F 0.0654(3) 0.10820(18) 0.50647(17) 0.0483(9) Uani 1 1 d . . . F33 F 0.1173(3) 0.20666(18) 0.50713(16) 0.0453(9) Uani 1 1 d . . . F34 F 0.2246(3) 0.1213(2) 0.53741(17) 0.0490(10) Uani 1 1 d . . . F35 F 0.1233(3) 0.3469(2) 0.46396(18) 0.0559(11) Uani 1 1 d . . . F36 F 0.1662(4) 0.4475(2) 0.4557(2) 0.0680(12) Uani 1 1 d . . . F37 F 0.0133(3) 0.4252(2) 0.42218(19) 0.0558(11) Uani 1 1 d . . . F38 F 0.0204(4) 0.4525(2) 0.1904(2) 0.0767(14) Uani 1 1 d . . . F39 F 0.0455(5) 0.3500(2) 0.1660(3) 0.0918(18) Uani 1 1 d . . . F40 F 0.1524(4) 0.4146(3) 0.1225(2) 0.0959(19) Uani 1 1 d . . . F41 F 0.4218(5) 0.5770(2) 0.3130(3) 0.111(2) Uani 1 1 d . . . F42 F 0.2657(6) 0.5542(2) 0.3183(4) 0.141(3) Uani 1 1 d . . . F43 F 0.3284(6) 0.6012(2) 0.2339(3) 0.123(3) Uani 1 1 d . . . F44 F 0.5851(5) 0.4176(3) 0.0613(3) 0.0907(17) Uani 1 1 d . . . F45 F 0.4265(5) 0.4701(2) 0.0464(2) 0.0880(17) Uani 1 1 d . . . F46 F 0.4499(5) 0.3627(3) 0.0510(2) 0.0901(17) Uani 1 1 d . . . F47 F 0.7978(3) 0.31179(19) 0.1799(2) 0.0636(12) Uani 1 1 d . . . F48 F 0.8219(3) 0.2555(3) 0.26930(19) 0.0712(14) Uani 1 1 d . . . F49 F 0.8443(3) 0.20661(19) 0.1749(2) 0.0536(10) Uani 1 1 d . . . F50 F 0.4070(4) 0.1218(2) 0.1253(2) 0.0817(15) Uani 1 1 d . . . F51 F 0.5652(4) 0.1224(2) 0.0751(2) 0.0732(14) Uani 1 1 d . . . F52 F 0.4364(4) 0.2007(2) 0.0584(2) 0.0756(14) Uani 1 1 d . . . F53 F 0.5040(3) 0.15956(18) 0.47345(17) 0.0487(9) Uani 1 1 d . . . F54 F 0.4343(3) 0.07246(18) 0.4450(2) 0.0547(10) Uani 1 1 d . . . F55 F 0.5751(3) 0.10266(18) 0.38967(18) 0.0465(9) Uani 1 1 d . . . F56 F 0.0945(3) 0.1292(2) 0.3556(2) 0.0598(11) Uani 1 1 d . . . F57 F 0.0524(3) 0.2315(2) 0.3353(3) 0.0852(16) Uani 1 1 d . . . F58 F 0.1058(5) 0.1663(4) 0.2566(2) 0.116(3) Uani 1 1 d . . . O17 O 0.1361(3) 0.06784(18) 0.76252(18) 0.0304(8) Uani 1 1 d . . . O19 O 0.3121(3) 0.14412(18) 0.72827(17) 0.0270(8) Uani 1 1 d . . . O22 O -0.0491(3) 0.18965(19) 0.73823(18) 0.0297(8) Uani 1 1 d . . . O24 O 0.1409(3) 0.15731(19) 0.65549(17) 0.0291(8) Uani 1 1 d . . . O27 O 0.0419(3) 0.27858(18) 0.83789(18) 0.0299(8) Uani 1 1 d . . . O29 O 0.1050(3) 0.28304(18) 0.70203(17) 0.0293(8) Uani 1 1 d . . . O32 O 0.2292(3) 0.13010(19) 0.86469(17) 0.0306(9) Uani 1 1 d . . . O34 O 0.2620(3) 0.25499(19) 0.8035(2) 0.0357(9) Uani 1 1 d . . . O52 O 0.6053(3) 0.28018(17) 0.25921(18) 0.0277(8) Uani 1 1 d . . . O54 O 0.4349(3) 0.23066(19) 0.19724(19) 0.0343(9) Uani 1 1 d . . . O57 O 0.4559(3) 0.21980(18) 0.35183(19) 0.0323(9) Uani 1 1 d . . . O59 O 0.2629(3) 0.24549(19) 0.29124(19) 0.0346(9) Uani 1 1 d . . . O62 O 0.2740(3) 0.3580(2) 0.36092(19) 0.0334(9) Uani 1 1 d . . . O64 O 0.2638(3) 0.36004(18) 0.21983(18) 0.0311(9) Uani 1 1 d . . . O67 O 0.4025(3) 0.44018(18) 0.29290(19) 0.0333(9) Uani 1 1 d . . . O69 O 0.4798(3) 0.36517(19) 0.1813(2) 0.0369(9) Uani 1 1 d . . . C1 C 0.0684(6) 0.1264(4) 1.0589(3) 0.056(2) Uani 1 1 d . . . H1 H 0.0423 0.0848 1.0706 0.067 Uiso 1 1 calc R . . C2 C 0.1298(7) 0.1554(5) 1.1023(4) 0.072(3) Uani 1 1 d . . . H2 H 0.1449 0.1340 1.1437 0.086 Uiso 1 1 calc R . . C3 C 0.1692(7) 0.2154(5) 1.0858(4) 0.067(2) Uani 1 1 d . . . H3 H 0.2115 0.2356 1.1155 0.081 Uiso 1 1 calc R . . C4 C 0.1466(6) 0.2458(4) 1.0253(3) 0.057(2) Uani 1 1 d . . . H4 H 0.1728 0.2872 1.0126 0.069 Uiso 1 1 calc R . . C5 C 0.0845(5) 0.2141(4) 0.9839(3) 0.0447(16) Uani 1 1 d . . . H5 H 0.0692 0.2345 0.9422 0.054 Uiso 1 1 calc R . . C6 C -0.1988(5) 0.2206(3) 0.8870(3) 0.0350(13) Uani 1 1 d . . . H6 H -0.1670 0.2045 0.8452 0.042 Uiso 1 1 calc R . . C7 C -0.2774(5) 0.2747(3) 0.8885(3) 0.0376(14) Uani 1 1 d . . . H7 H -0.3001 0.2950 0.8480 0.045 Uiso 1 1 calc R . . C8 C -0.3235(5) 0.2996(3) 0.9491(3) 0.0474(17) Uani 1 1 d . . . H8 H -0.3772 0.3374 0.9512 0.057 Uiso 1 1 calc R . . C9 C -0.2886(6) 0.2674(3) 1.0072(3) 0.0496(18) Uani 1 1 d . . . H9 H -0.3188 0.2827 1.0497 0.060 Uiso 1 1 calc R . . C10 C -0.2101(5) 0.2135(3) 1.0020(3) 0.0452(17) Uani 1 1 d . . . H10 H -0.1862 0.1922 1.0416 0.054 Uiso 1 1 calc R . . C11 C -0.1083(5) 0.0422(3) 0.8142(3) 0.0408(15) Uani 1 1 d . . . H11 H -0.0381 0.0515 0.7971 0.049 Uiso 1 1 calc R . . C12 C -0.1706(5) 0.0089(3) 0.7739(4) 0.0502(18) Uani 1 1 d . . . H12 H -0.1430 -0.0057 0.7306 0.060 Uiso 1 1 calc R . . C13 C -0.2747(6) -0.0025(4) 0.7988(4) 0.0563(19) Uani 1 1 d . . . H13 H -0.3203 -0.0239 0.7721 0.068 Uiso 1 1 calc R . . C14 C -0.3107(6) 0.0170(4) 0.8614(5) 0.062(2) Uani 1 1 d . . . H14 H -0.3811 0.0085 0.8790 0.075 Uiso 1 1 calc R . . C15 C -0.2447(5) 0.0494(3) 0.8996(4) 0.054(2) Uani 1 1 d . . . H15 H -0.2711 0.0635 0.9432 0.065 Uiso 1 1 calc R . . C16 C 0.1649(7) -0.0482(3) 0.7455(4) 0.053(2) Uani 1 1 d . . . C17 C 0.2070(5) 0.0217(3) 0.7403(3) 0.0307(13) Uani 1 1 d . . . C18 C 0.3112(5) 0.0268(3) 0.7153(3) 0.0358(14) Uani 1 1 d . . . H18 H 0.3551 -0.0126 0.7002 0.043 Uiso 1 1 calc R . . C19 C 0.3555(4) 0.0875(3) 0.7111(3) 0.0295(12) Uani 1 1 d . . . C20 C 0.4723(5) 0.0868(4) 0.6808(4) 0.0485(17) Uani 1 1 d . . . C21 C -0.2146(5) 0.2057(3) 0.6888(3) 0.0398(15) Uani 1 1 d . . . C22 C -0.0908(4) 0.1879(3) 0.6829(3) 0.0291(12) Uani 1 1 d . . . C23 C -0.0393(5) 0.1725(3) 0.6216(3) 0.0334(13) Uani 1 1 d . . . H23 H -0.0814 0.1716 0.5841 0.040 Uiso 1 1 calc R . . C24 C 0.0733(4) 0.1581(3) 0.6130(3) 0.0269(12) Uani 1 1 d . . . C25 C 0.1217(5) 0.1483(3) 0.5403(3) 0.0354(14) Uani 1 1 d . . . C26 C -0.0487(6) 0.3784(3) 0.8859(3) 0.0467(17) Uani 1 1 d . . . C27 C 0.0016(5) 0.3365(3) 0.8253(3) 0.0310(12) Uani 1 1 d . . . C28 C -0.0041(5) 0.3684(3) 0.7640(3) 0.0387(14) Uani 1 1 d . . . H28 H -0.0438 0.4115 0.7609 0.046 Uiso 1 1 calc R . . C29 C 0.0477(5) 0.3380(3) 0.7068(3) 0.0285(12) Uani 1 1 d . . . C30 C 0.0303(6) 0.3752(3) 0.6405(3) 0.0409(15) Uani 1 1 d . . . C31 C 0.3645(6) 0.0796(4) 0.9295(3) 0.0458(17) Uani 1 1 d . . . C32 C 0.3197(5) 0.1374(3) 0.8863(3) 0.0323(13) Uani 1 1 d . . . C33 C 0.3805(5) 0.1903(3) 0.8744(3) 0.0423(15) Uani 1 1 d . . . H33 H 0.4476 0.1899 0.8946 0.051 Uiso 1 1 calc R . . C34 C 0.3463(5) 0.2444(3) 0.8337(3) 0.0377(14) Uani 1 1 d . . . C35 C 0.4264(7) 0.2996(4) 0.8223(5) 0.064(2) Uani 1 1 d . . . C36 C 0.3864(5) 0.3186(3) 0.5023(3) 0.0338(13) Uani 1 1 d . . . H36 H 0.3521 0.3299 0.4623 0.041 Uiso 1 1 calc R . . C37 C 0.3331(6) 0.2832(3) 0.5513(3) 0.0443(16) Uani 1 1 d . . . H37 H 0.2629 0.2707 0.5452 0.053 Uiso 1 1 calc R . . C38 C 0.3835(6) 0.2658(3) 0.6101(3) 0.0455(16) Uani 1 1 d . . . H38 H 0.3486 0.2409 0.6443 0.055 Uiso 1 1 calc R . . C39 C 0.4853(5) 0.2856(3) 0.6173(3) 0.0460(17) Uani 1 1 d . . . H39 H 0.5213 0.2747 0.6567 0.055 Uiso 1 1 calc R . . C40 C 0.5339(5) 0.3213(3) 0.5662(3) 0.0397(15) Uani 1 1 d . . . H40 H 0.6037 0.3348 0.5713 0.048 Uiso 1 1 calc R . . C41 C 0.6888(5) 0.2605(3) 0.4142(3) 0.0339(13) Uani 1 1 d . . . H41 H 0.6241 0.2515 0.3952 0.041 Uiso 1 1 calc R . . C42 C 0.7728(5) 0.2096(3) 0.4172(3) 0.0360(14) Uani 1 1 d . . . H42 H 0.7660 0.1664 0.4006 0.043 Uiso 1 1 calc R . . C43 C 0.8663(5) 0.2223(3) 0.4444(3) 0.0379(14) Uani 1 1 d . . . H43 H 0.9250 0.1879 0.4472 0.045 Uiso 1 1 calc R . . C44 C 0.8744(5) 0.2857(3) 0.4677(3) 0.0397(15) Uani 1 1 d . . . H44 H 0.9388 0.2958 0.4863 0.048 Uiso 1 1 calc R . . C45 C 0.7862(5) 0.3341(3) 0.4632(3) 0.0342(13) Uani 1 1 d . . . H45 H 0.7910 0.3776 0.4797 0.041 Uiso 1 1 calc R . . C46 C 0.6833(5) 0.4217(3) 0.3053(3) 0.0392(14) Uani 1 1 d . . . H46 H 0.6764 0.3760 0.2973 0.047 Uiso 1 1 calc R . . C47 C 0.7354(6) 0.4582(3) 0.2559(4) 0.0535(18) Uani 1 1 d . . . H47 H 0.7631 0.4380 0.2150 0.064 Uiso 1 1 calc R . . C48 C 0.7458(6) 0.5239(3) 0.2676(4) 0.058(2) Uani 1 1 d . . . H48 H 0.7818 0.5499 0.2349 0.070 Uiso 1 1 calc R . . C49 C 0.7037(7) 0.5519(3) 0.3273(4) 0.060(2) Uani 1 1 d . . . H49 H 0.7094 0.5976 0.3359 0.071 Uiso 1 1 calc R . . C50 C 0.6531(6) 0.5128(3) 0.3743(4) 0.0447(16) Uani 1 1 d . . . H50 H 0.6250 0.5324 0.4155 0.054 Uiso 1 1 calc R . . C51 C 0.7829(5) 0.2539(3) 0.2105(3) 0.0343(13) Uani 1 1 d . . . C52 C 0.6608(4) 0.2456(3) 0.2156(3) 0.0263(11) Uani 1 1 d . . . C53 C 0.6245(5) 0.2039(3) 0.1691(3) 0.0327(13) Uani 1 1 d . . . H53 H 0.6761 0.1770 0.1409 0.039 Uiso 1 1 calc R . . C54 C 0.5135(5) 0.2013(3) 0.1634(3) 0.0335(13) Uani 1 1 d . . . C55 C 0.4825(6) 0.1600(4) 0.1053(4) 0.0532(19) Uani 1 1 d . . . C56 C 0.4799(5) 0.1252(3) 0.4212(3) 0.0356(14) Uani 1 1 d . . . C57 C 0.4093(5) 0.1704(3) 0.3751(3) 0.0284(12) Uani 1 1 d . . . C58 C 0.3071(5) 0.1550(3) 0.3648(3) 0.0318(13) Uani 1 1 d . . . H58 H 0.2813 0.1167 0.3860 0.038 Uiso 1 1 calc R . . C59 C 0.2409(5) 0.1949(3) 0.3237(3) 0.0295(12) Uani 1 1 d . . . C60 C 0.1235(5) 0.1782(3) 0.3172(3) 0.0393(15) Uani 1 1 d . . . C61 C 0.1202(5) 0.4023(3) 0.4244(3) 0.0404(15) Uani 1 1 d . . . C62 C 0.1779(5) 0.3853(3) 0.3574(3) 0.0323(13) Uani 1 1 d . . . C63 C 0.1229(5) 0.4006(3) 0.3003(3) 0.0345(13) Uani 1 1 d . . . H63 H 0.0504 0.4218 0.3050 0.041 Uiso 1 1 calc R . . C64 C 0.1697(5) 0.3859(3) 0.2364(3) 0.0321(13) Uani 1 1 d . . . C65 C 0.0976(5) 0.4013(3) 0.1781(3) 0.0432(16) Uani 1 1 d . . . C66 C 0.3501(6) 0.5555(3) 0.2776(4) 0.0457(16) Uani 1 1 d . . . C67 C 0.3906(5) 0.4861(3) 0.2500(3) 0.0351(13) Uani 1 1 d . . . C68 C 0.4098(5) 0.4799(3) 0.1817(3) 0.0419(15) Uani 1 1 d . . . H68 H 0.3931 0.5178 0.1538 0.050 Uiso 1 1 calc R . . C69 C 0.4530(5) 0.4196(3) 0.1532(3) 0.0403(15) Uani 1 1 d . . . C70 C 0.4776(8) 0.4178(4) 0.0769(4) 0.063(2) Uani 1 1 d . . . C80 C 0.7420(7) 0.0441(5) 0.5099(5) 0.071(3) Uani 0.90 1 d P . . H80A H 0.6895 0.0123 0.5008 0.086 Uiso 0.90 1 calc PR . . H80B H 0.7028 0.0898 0.5103 0.086 Uiso 0.90 1 calc PR . . Cl81 Cl 0.8470(2) 0.03890(11) 0.44549(13) 0.0738(7) Uani 0.90 1 d P . . Cl82 Cl 0.7920(2) 0.02558(12) 0.58896(13) 0.0787(7) Uani 0.90 1 d P . . C90 C 0.8118(11) 0.5079(6) 0.0217(6) 0.081(4) Uani 0.75 1 d P . . H90A H 0.7681 0.4934 -0.0135 0.098 Uiso 0.75 1 calc PR . . H90B H 0.8744 0.5281 -0.0003 0.098 Uiso 0.75 1 calc PR . . Cl91 Cl 0.8593(3) 0.43842(16) 0.06851(14) 0.0800(9) Uani 0.75 1 d P . . Cl92 Cl 0.7312(3) 0.5683(2) 0.0719(2) 0.1201(16) Uani 0.75 1 d P . . 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 0.02125(13) 0.02365(13) 0.01994(12) 0.00226(9) -0.00098(10) 0.00107(10) Dy2 0.02479(14) 0.02378(13) 0.02440(13) -0.00023(10) -0.00245(10) 0.00087(10) Cr1 0.0305(5) 0.0349(5) 0.0297(5) 0.0124(4) 0.0084(4) 0.0080(4) Cr2 0.0307(5) 0.0251(4) 0.0278(5) -0.0071(4) -0.0052(4) 0.0052(4) O1 0.036(2) 0.033(2) 0.041(2) 0.0141(19) 0.0086(19) 0.0097(19) O2 0.041(2) 0.031(2) 0.035(2) -0.0121(18) -0.0117(19) 0.0137(18) F1 0.0306(17) 0.0290(16) 0.0243(15) 0.0059(12) -0.0023(13) 0.0028(13) F2 0.0297(17) 0.0257(16) 0.0264(16) -0.0050(12) -0.0032(13) 0.0018(13) F3 0.042(2) 0.056(2) 0.048(2) 0.0273(18) 0.0200(17) 0.0163(18) F4 0.043(2) 0.0345(18) 0.0391(19) -0.0148(15) -0.0150(16) 0.0069(15) N1 0.048(3) 0.048(3) 0.024(3) 0.005(2) 0.000(2) 0.016(3) N2 0.028(3) 0.040(3) 0.033(3) 0.010(2) 0.006(2) 0.008(2) N3 0.028(3) 0.030(3) 0.059(4) 0.013(2) 0.005(2) 0.002(2) N4 0.030(3) 0.036(3) 0.027(2) -0.004(2) 0.002(2) 0.007(2) N5 0.030(3) 0.025(2) 0.027(2) -0.0038(19) -0.004(2) 0.0031(19) N6 0.033(3) 0.028(3) 0.039(3) -0.005(2) -0.005(2) 0.003(2) F11 0.089(3) 0.047(2) 0.0294(19) -0.0042(17) 0.016(2) 0.008(2) F12 0.091(4) 0.080(3) 0.053(3) -0.001(2) 0.018(2) 0.043(3) F13 0.129(5) 0.077(3) 0.059(3) -0.035(2) 0.025(3) -0.045(3) F14 0.136(5) 0.080(3) 0.064(3) 0.032(2) -0.064(3) -0.043(3) F15 0.123(4) 0.039(2) 0.049(2) 0.0135(19) 0.005(3) 0.023(2) F16 0.087(3) 0.086(3) 0.041(2) 0.029(2) 0.017(2) 0.020(3) F17 0.171(6) 0.043(3) 0.113(4) -0.010(3) -0.099(4) 0.025(3) F18 0.065(3) 0.146(5) 0.071(3) 0.071(3) 0.008(3) 0.025(3) F19 0.051(2) 0.073(3) 0.061(3) 0.008(2) -0.027(2) 0.013(2) F20 0.065(3) 0.070(3) 0.082(3) -0.022(2) -0.020(2) -0.023(2) F21 0.084(4) 0.063(3) 0.135(5) 0.041(3) -0.049(3) -0.036(3) F22 0.058(3) 0.096(4) 0.088(4) -0.003(3) 0.003(3) -0.026(3) F23 0.185(6) 0.036(2) 0.067(3) -0.005(2) 0.067(4) -0.018(3) F24 0.054(3) 0.057(3) 0.154(5) -0.040(3) 0.000(3) -0.021(2) F25 0.079(3) 0.0241(18) 0.058(2) -0.0124(17) 0.011(2) -0.0009(18) F26 0.038(2) 0.071(3) 0.113(4) 0.012(3) 0.008(2) 0.017(2) F27 0.030(2) 0.112(4) 0.204(7) -0.082(5) 0.033(3) -0.023(3) F28 0.059(3) 0.159(5) 0.071(3) 0.034(3) 0.029(3) 0.010(3) F29 0.027(2) 0.101(3) 0.069(3) 0.026(3) -0.0016(19) -0.012(2) F30 0.040(2) 0.059(3) 0.107(4) -0.020(2) -0.005(2) 0.018(2) F31 0.033(2) 0.112(4) 0.049(2) -0.010(2) -0.0162(18) 0.010(2) F32 0.054(2) 0.052(2) 0.038(2) -0.0182(17) -0.0108(17) 0.0063(18) F33 0.051(2) 0.053(2) 0.0294(18) 0.0082(16) 0.0030(16) 0.0000(18) F34 0.038(2) 0.071(3) 0.0324(19) -0.0111(17) 0.0011(16) 0.0160(18) F35 0.048(2) 0.071(3) 0.043(2) 0.021(2) 0.0075(18) 0.010(2) F36 0.064(3) 0.082(3) 0.057(3) -0.033(2) 0.019(2) -0.012(2) F37 0.038(2) 0.072(3) 0.050(2) 0.007(2) 0.0123(18) 0.0170(19) F38 0.079(3) 0.080(3) 0.062(3) 0.000(2) -0.027(2) 0.044(3) F39 0.115(4) 0.068(3) 0.104(4) 0.005(3) -0.074(4) -0.018(3) F40 0.060(3) 0.175(6) 0.045(3) 0.040(3) -0.009(2) 0.015(3) F41 0.120(5) 0.055(3) 0.164(6) -0.047(3) -0.076(4) 0.018(3) F42 0.129(5) 0.044(3) 0.232(8) -0.033(4) 0.105(6) 0.000(3) F43 0.254(8) 0.035(3) 0.071(3) -0.003(2) -0.045(4) 0.049(4) F44 0.090(4) 0.087(4) 0.081(3) 0.015(3) 0.052(3) 0.009(3) F45 0.130(5) 0.076(3) 0.044(2) 0.026(2) 0.012(3) 0.036(3) F46 0.154(5) 0.074(3) 0.040(2) -0.005(2) -0.008(3) -0.002(3) F47 0.043(2) 0.042(2) 0.105(4) 0.010(2) 0.009(2) -0.0115(18) F48 0.032(2) 0.143(4) 0.039(2) -0.010(2) -0.0044(18) -0.011(2) F49 0.034(2) 0.052(2) 0.071(3) -0.017(2) 0.0104(19) 0.0051(17) F50 0.102(4) 0.070(3) 0.083(3) -0.024(3) -0.010(3) -0.050(3) F51 0.069(3) 0.071(3) 0.079(3) -0.052(2) -0.020(2) 0.012(2) F52 0.091(4) 0.074(3) 0.063(3) -0.017(2) -0.036(3) 0.002(3) F53 0.068(3) 0.043(2) 0.0331(19) -0.0007(16) -0.0164(18) 0.0076(18) F54 0.055(2) 0.042(2) 0.067(3) 0.0272(19) -0.010(2) -0.0068(18) F55 0.042(2) 0.045(2) 0.047(2) 0.0011(17) 0.0015(17) 0.0146(17) F56 0.046(2) 0.066(3) 0.073(3) 0.019(2) -0.012(2) -0.026(2) F57 0.035(2) 0.072(3) 0.147(5) 0.012(3) -0.001(3) -0.008(2) F58 0.105(4) 0.230(7) 0.035(2) -0.014(3) -0.008(3) -0.112(5) O17 0.027(2) 0.031(2) 0.032(2) 0.0007(17) 0.0023(17) -0.0008(16) O19 0.026(2) 0.029(2) 0.0252(19) 0.0008(15) -0.0015(16) -0.0010(16) O22 0.026(2) 0.036(2) 0.026(2) 0.0032(16) -0.0023(16) -0.0013(16) O24 0.0226(19) 0.039(2) 0.0246(19) 0.0009(16) -0.0030(16) 0.0012(16) O27 0.035(2) 0.027(2) 0.027(2) -0.0001(16) 0.0005(17) 0.0022(17) O29 0.035(2) 0.029(2) 0.0227(19) 0.0017(15) -0.0004(16) 0.0018(17) O32 0.029(2) 0.038(2) 0.0232(19) 0.0057(16) -0.0015(16) -0.0002(17) O34 0.034(2) 0.034(2) 0.039(2) -0.0011(18) -0.0067(19) -0.0008(18) O52 0.029(2) 0.0260(19) 0.0270(19) -0.0053(16) -0.0021(16) 0.0021(16) O54 0.032(2) 0.033(2) 0.038(2) -0.0071(18) -0.0056(18) 0.0018(18) O57 0.034(2) 0.029(2) 0.034(2) 0.0036(17) -0.0049(18) -0.0029(17) O59 0.030(2) 0.037(2) 0.037(2) 0.0085(18) -0.0007(18) -0.0042(18) O62 0.029(2) 0.041(2) 0.029(2) 0.0028(17) -0.0034(17) 0.0012(18) O64 0.031(2) 0.031(2) 0.031(2) 0.0018(16) -0.0023(17) 0.0000(17) O67 0.036(2) 0.026(2) 0.037(2) 0.0012(17) -0.0083(18) 0.0012(17) O69 0.038(2) 0.030(2) 0.040(2) 0.0053(18) 0.0033(19) 0.0044(18) C1 0.067(5) 0.070(5) 0.024(3) 0.006(3) -0.002(3) 0.023(4) C2 0.089(6) 0.089(7) 0.027(4) 0.001(4) -0.011(4) 0.042(5) C3 0.070(6) 0.087(6) 0.040(4) -0.026(4) -0.020(4) 0.031(5) C4 0.067(5) 0.064(5) 0.039(4) -0.015(3) -0.013(4) 0.010(4) C5 0.046(4) 0.058(4) 0.027(3) -0.005(3) -0.004(3) 0.010(3) C6 0.036(3) 0.040(3) 0.028(3) 0.003(3) -0.001(3) 0.000(3) C7 0.040(4) 0.041(3) 0.029(3) 0.005(3) -0.004(3) 0.009(3) C8 0.045(4) 0.052(4) 0.038(4) 0.002(3) 0.000(3) 0.021(3) C9 0.055(4) 0.058(4) 0.028(3) 0.002(3) 0.009(3) 0.020(3) C10 0.043(4) 0.058(4) 0.027(3) 0.012(3) 0.009(3) 0.020(3) C11 0.033(3) 0.041(4) 0.048(4) 0.010(3) -0.001(3) -0.007(3) C12 0.040(4) 0.047(4) 0.065(5) 0.013(3) -0.011(3) -0.009(3) C13 0.040(4) 0.050(4) 0.082(6) 0.009(4) -0.012(4) -0.015(3) C14 0.030(4) 0.041(4) 0.115(7) 0.004(4) 0.007(4) -0.006(3) C15 0.035(4) 0.034(4) 0.089(6) 0.012(4) 0.020(4) -0.003(3) C16 0.075(6) 0.029(3) 0.052(4) -0.009(3) 0.028(4) -0.007(3) C17 0.039(3) 0.029(3) 0.024(3) -0.001(2) -0.002(2) 0.000(3) C18 0.034(3) 0.035(3) 0.035(3) -0.007(3) 0.002(3) 0.008(3) C19 0.028(3) 0.036(3) 0.023(3) 0.004(2) -0.004(2) 0.004(2) C20 0.025(3) 0.061(5) 0.056(4) -0.008(4) 0.000(3) 0.008(3) C21 0.029(3) 0.051(4) 0.039(4) 0.002(3) -0.008(3) 0.001(3) C22 0.029(3) 0.028(3) 0.030(3) 0.004(2) -0.006(2) 0.002(2) C23 0.030(3) 0.040(3) 0.030(3) -0.001(3) -0.010(3) -0.001(3) C24 0.030(3) 0.026(3) 0.023(3) -0.004(2) 0.000(2) 0.003(2) C25 0.031(3) 0.040(3) 0.035(3) -0.008(3) -0.007(3) 0.005(3) C26 0.064(5) 0.033(3) 0.039(4) -0.007(3) 0.009(3) 0.005(3) C27 0.030(3) 0.029(3) 0.034(3) -0.005(2) 0.000(2) -0.004(2) C28 0.046(4) 0.027(3) 0.039(3) 0.003(3) 0.002(3) 0.009(3) C29 0.036(3) 0.022(3) 0.028(3) 0.004(2) -0.004(2) -0.002(2) C30 0.057(4) 0.032(3) 0.030(3) 0.002(3) -0.002(3) 0.007(3) C31 0.044(4) 0.059(4) 0.033(3) 0.005(3) -0.013(3) 0.005(3) C32 0.031(3) 0.042(3) 0.022(3) 0.000(2) -0.003(2) 0.006(3) C33 0.031(3) 0.053(4) 0.044(4) 0.001(3) -0.014(3) 0.000(3) C34 0.032(3) 0.043(4) 0.040(3) -0.001(3) -0.006(3) -0.009(3) C35 0.052(5) 0.060(5) 0.086(6) 0.002(5) -0.030(5) -0.017(4) C36 0.034(3) 0.035(3) 0.030(3) -0.006(2) -0.004(3) 0.007(3) C37 0.042(4) 0.046(4) 0.042(4) 0.004(3) 0.009(3) 0.003(3) C38 0.051(4) 0.042(4) 0.039(4) 0.008(3) 0.004(3) 0.011(3) C39 0.043(4) 0.063(4) 0.028(3) 0.008(3) -0.002(3) 0.010(3) C40 0.033(3) 0.054(4) 0.029(3) -0.005(3) -0.007(3) 0.010(3) C41 0.034(3) 0.036(3) 0.032(3) -0.005(2) -0.009(3) 0.001(3) C42 0.044(4) 0.030(3) 0.033(3) -0.006(2) -0.010(3) 0.006(3) C43 0.032(3) 0.042(4) 0.036(3) -0.001(3) -0.001(3) 0.010(3) C44 0.029(3) 0.046(4) 0.044(4) -0.006(3) -0.010(3) 0.002(3) C45 0.033(3) 0.029(3) 0.041(3) -0.010(3) -0.005(3) -0.001(2) C46 0.045(4) 0.030(3) 0.044(4) -0.003(3) -0.003(3) -0.006(3) C47 0.064(5) 0.043(4) 0.053(4) 0.000(3) 0.013(4) -0.012(3) C48 0.062(5) 0.033(4) 0.080(6) 0.009(4) 0.007(4) -0.013(3) C49 0.071(5) 0.026(3) 0.082(6) -0.005(4) -0.013(4) -0.003(3) C50 0.052(4) 0.028(3) 0.054(4) -0.003(3) -0.008(3) -0.002(3) C51 0.028(3) 0.036(3) 0.036(3) -0.004(3) 0.007(3) 0.003(3) C52 0.028(3) 0.023(3) 0.027(3) 0.002(2) -0.001(2) 0.001(2) C53 0.035(3) 0.028(3) 0.033(3) -0.011(2) 0.001(3) 0.005(2) C54 0.035(3) 0.026(3) 0.041(3) -0.006(2) -0.009(3) -0.005(2) C55 0.057(5) 0.041(4) 0.063(5) -0.019(4) -0.011(4) -0.004(4) C56 0.037(3) 0.031(3) 0.037(3) 0.000(3) 0.002(3) 0.000(3) C57 0.034(3) 0.026(3) 0.023(3) -0.006(2) 0.001(2) 0.003(2) C58 0.038(3) 0.023(3) 0.034(3) 0.004(2) 0.001(3) -0.006(2) C59 0.033(3) 0.030(3) 0.025(3) -0.006(2) 0.003(2) -0.006(2) C60 0.035(3) 0.054(4) 0.032(3) 0.004(3) -0.004(3) -0.014(3) C61 0.028(3) 0.048(4) 0.041(4) 0.003(3) 0.004(3) 0.009(3) C62 0.029(3) 0.029(3) 0.038(3) 0.003(2) -0.001(3) 0.001(2) C63 0.027(3) 0.033(3) 0.041(3) 0.004(3) 0.002(3) 0.005(2) C64 0.035(3) 0.021(3) 0.040(3) 0.003(2) -0.010(3) 0.000(2) C65 0.039(4) 0.045(4) 0.044(4) 0.003(3) -0.010(3) 0.004(3) C66 0.054(4) 0.030(3) 0.052(4) -0.004(3) -0.011(4) 0.006(3) C67 0.035(3) 0.027(3) 0.043(4) 0.004(3) -0.005(3) -0.005(3) C68 0.054(4) 0.030(3) 0.040(4) 0.012(3) -0.002(3) 0.002(3) C69 0.036(3) 0.040(4) 0.040(4) 0.008(3) 0.008(3) 0.006(3) C70 0.086(6) 0.049(5) 0.051(5) 0.016(4) 0.003(4) 0.000(4) C80 0.061(6) 0.054(5) 0.100(8) 0.034(5) -0.027(5) -0.004(4) Cl81 0.0836(17) 0.0444(12) 0.0898(17) 0.0241(11) -0.0092(14) 0.0056(11) Cl82 0.0949(19) 0.0618(14) 0.0824(17) 0.0025(12) -0.0237(15) -0.0108(13) C90 0.092(9) 0.090(9) 0.055(7) -0.012(6) -0.011(6) 0.026(7) Cl91 0.098(2) 0.087(2) 0.0508(15) -0.0103(14) -0.0131(15) 0.0149(17) Cl92 0.115(3) 0.127(3) 0.108(3) -0.054(2) -0.036(2) 0.059(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 Dy1 F1 2.316(3) . ? Dy1 O17 2.364(4) . ? Dy1 O22 2.371(4) . ? Dy1 O34 2.391(4) . ? Dy1 O29 2.407(4) . ? Dy1 O19 2.421(4) . ? Dy1 O27 2.421(4) . ? Dy1 O24 2.422(4) . ? Dy1 O32 2.474(4) . ? Dy2 F2 2.298(3) . ? Dy2 O54 2.368(4) . ? Dy2 O62 2.374(4) . ? Dy2 O64 2.379(4) . ? Dy2 O69 2.380(4) . ? Dy2 O57 2.382(4) . ? Dy2 O59 2.420(4) . ? Dy2 O52 2.423(4) . ? Dy2 O67 2.548(4) . ? Cr1 F3 1.871(3) . ? Cr1 F1 1.881(3) . ? Cr1 O1 1.995(4) . ? Cr1 N2 2.050(5) . ? Cr1 N3 2.075(6) . ? Cr1 N1 2.076(6) . ? Cr2 F4 1.867(3) . ? Cr2 F2 1.887(3) . ? Cr2 O2 1.988(4) . ? Cr2 N5 2.051(4) . ? Cr2 N6 2.072(5) . ? Cr2 N4 2.081(5) . ? O1 H1A 0.86(2) . ? O1 H1B 0.87(2) . ? O2 H2A 0.87(2) . ? O2 H2B 0.88(2) . ? N1 C5 1.345(9) . ? N1 C1 1.356(8) . ? N2 C6 1.344(7) . ? N2 C10 1.346(7) . ? N3 C11 1.345(8) . ? N3 C15 1.357(8) . ? N4 C36 1.343(7) . ? N4 C40 1.346(7) . ? N5 C45 1.336(7) . ? N5 C41 1.338(7) . ? N6 C50 1.336(7) . ? N6 C46 1.352(8) . ? F11 C26 1.322(7) . ? F12 C26 1.333(8) . ? F13 C26 1.309(8) . ? F14 C30 1.312(8) . ? F15 C30 1.319(7) . ? F16 C30 1.324(8) . ? F17 C31 1.293(8) . ? F18 C31 1.329(8) . ? F19 C31 1.329(7) . ? F20 C35 1.315(9) . ? F21 C35 1.266(9) . ? F22 C35 1.378(10) . ? F23 C16 1.314(8) . ? F24 C16 1.315(9) . ? F25 C16 1.347(7) . ? F26 C20 1.343(8) . ? F27 C20 1.276(8) . ? F28 C20 1.334(8) . ? F29 C21 1.310(7) . ? F30 C21 1.330(7) . ? F31 C21 1.333(7) . ? F32 C25 1.349(7) . ? F33 C25 1.337(7) . ? F34 C25 1.326(6) . ? F35 C61 1.356(7) . ? F36 C61 1.319(8) . ? F37 C61 1.356(7) . ? F38 C65 1.337(7) . ? F39 C65 1.312(8) . ? F40 C65 1.307(8) . ? F41 C66 1.294(8) . ? F42 C66 1.283(9) . ? F43 C66 1.281(8) . ? F44 C70 1.347(10) . ? F45 C70 1.329(8) . ? F46 C70 1.324(9) . ? F47 C51 1.331(7) . ? F48 C51 1.313(7) . ? F49 C51 1.332(6) . ? F50 C55 1.314(9) . ? F51 C55 1.320(8) . ? F52 C55 1.353(8) . ? F53 C56 1.338(7) . ? F54 C56 1.324(7) . ? F55 C56 1.336(7) . ? F56 C60 1.307(7) . ? F57 C60 1.345(8) . ? F58 C60 1.286(7) . ? O17 C17 1.266(6) . ? O19 C19 1.245(6) . ? O22 C22 1.264(6) . ? O24 C24 1.239(6) . ? O27 C27 1.242(6) . ? O29 C29 1.244(6) . ? O32 C32 1.257(7) . ? O34 C34 1.243(7) . ? O52 C52 1.245(6) . ? O54 C54 1.244(7) . ? O57 C57 1.270(7) . ? O59 C59 1.245(6) . ? O62 C62 1.260(7) . ? O64 C64 1.247(7) . ? O67 C67 1.256(7) . ? O69 C69 1.245(7) . ? C1 C2 1.378(12) . ? C1 H1 0.9500 . ? C2 C3 1.379(12) . ? C2 H2 0.9500 . ? C3 C4 1.385(10) . ? C3 H3 0.9500 . ? C4 C5 1.386(10) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.375(8) . ? C6 H6 0.9500 . ? C7 C8 1.387(8) . ? C7 H7 0.9500 . ? C8 C9 1.398(9) . ? C8 H8 0.9500 . ? C9 C10 1.371(8) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.390(9) . ? C11 H11 0.9500 . ? C12 C13 1.394(10) . ? C12 H12 0.9500 . ? C13 C14 1.354(11) . ? C13 H13 0.9500 . ? C14 C15 1.385(11) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.553(9) . ? C17 C18 1.367(8) . ? C18 C19 1.393(8) . ? C18 H18 0.9500 . ? C19 C20 1.530(9) . ? C21 C22 1.533(8) . ? C22 C23 1.372(8) . ? C23 C24 1.393(8) . ? C23 H23 0.9500 . ? C24 C25 1.547(8) . ? C26 C27 1.547(8) . ? C27 C28 1.383(8) . ? C28 C29 1.393(8) . ? C28 H28 0.9500 . ? C29 C30 1.535(8) . ? C31 C32 1.516(8) . ? C32 C33 1.380(9) . ? C33 C34 1.397(9) . ? C33 H33 0.9500 . ? C34 C35 1.574(10) . ? C36 C37 1.379(9) . ? C36 H36 0.9500 . ? C37 C38 1.398(9) . ? C37 H37 0.9500 . ? C38 C39 1.385(10) . ? C38 H38 0.9500 . ? C39 C40 1.384(9) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.379(8) . ? C41 H41 0.9500 . ? C42 C43 1.369(8) . ? C42 H42 0.9500 . ? C43 C44 1.380(9) . ? C43 H43 0.9500 . ? C44 C45 1.385(8) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.389(9) . ? C46 H46 0.9500 . ? C47 C48 1.366(9) . ? C47 H47 0.9500 . ? C48 C49 1.378(11) . ? C48 H48 0.9500 . ? C49 C50 1.381(10) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.538(8) . ? C52 C53 1.400(7) . ? C53 C54 1.397(8) . ? C53 H53 0.9500 . ? C54 C55 1.542(9) . ? C56 C57 1.537(8) . ? C57 C58 1.369(8) . ? C58 C59 1.387(8) . ? C58 H58 0.9500 . ? C59 C60 1.547(8) . ? C61 C62 1.505(8) . ? C62 C63 1.392(8) . ? C63 C64 1.393(8) . ? C63 H63 0.9500 . ? C64 C65 1.532(8) . ? C66 C67 1.528(8) . ? C67 C68 1.383(9) . ? C68 C69 1.384(9) . ? C68 H68 0.9500 . ? C69 C70 1.543(10) . ? C80 Cl81 1.765(10) . ? C80 Cl82 1.768(9) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C90 Cl91 1.741(12) . ? C90 Cl92 1.765(11) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? 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 F1 Dy1 O17 73.63(11) . . ? F1 Dy1 O22 70.43(11) . . ? O17 Dy1 O22 85.56(13) . . ? F1 Dy1 O34 115.39(12) . . ? O17 Dy1 O34 132.21(13) . . ? O22 Dy1 O34 142.22(13) . . ? F1 Dy1 O29 129.16(11) . . ? O17 Dy1 O29 137.88(12) . . ? O22 Dy1 O29 74.01(13) . . ? O34 Dy1 O29 75.20(13) . . ? F1 Dy1 O19 133.19(11) . . ? O17 Dy1 O19 72.97(12) . . ? O22 Dy1 O19 137.09(12) . . ? O34 Dy1 O19 68.37(13) . . ? O29 Dy1 O19 97.50(12) . . ? F1 Dy1 O27 68.18(11) . . ? O17 Dy1 O27 141.73(13) . . ? O22 Dy1 O27 79.60(13) . . ? O34 Dy1 O27 69.88(13) . . ? O29 Dy1 O27 70.64(12) . . ? O19 Dy1 O27 138.24(12) . . ? F1 Dy1 O24 129.29(12) . . ? O17 Dy1 O24 71.09(13) . . ? O22 Dy1 O24 71.62(12) . . ? O34 Dy1 O24 115.25(13) . . ? O29 Dy1 O24 67.65(12) . . ? O19 Dy1 O24 66.44(12) . . ? O27 Dy1 O24 134.21(12) . . ? F1 Dy1 O32 66.54(11) . . ? O17 Dy1 O32 70.98(13) . . ? O22 Dy1 O32 135.15(12) . . ? O34 Dy1 O32 71.21(13) . . ? O29 Dy1 O32 146.35(13) . . ? O19 Dy1 O32 72.12(12) . . ? O27 Dy1 O32 95.51(12) . . ? O24 Dy1 O32 129.97(12) . . ? F2 Dy2 O54 138.10(12) . . ? F2 Dy2 O62 75.44(12) . . ? O54 Dy2 O62 137.73(14) . . ? F2 Dy2 O64 137.00(11) . . ? O54 Dy2 O64 84.11(13) . . ? O62 Dy2 O64 73.74(13) . . ? F2 Dy2 O69 108.42(13) . . ? O54 Dy2 O69 73.14(14) . . ? O62 Dy2 O69 128.44(13) . . ? O64 Dy2 O69 70.49(13) . . ? F2 Dy2 O57 70.15(12) . . ? O54 Dy2 O57 82.85(13) . . ? O62 Dy2 O57 90.27(13) . . ? O64 Dy2 O57 138.34(13) . . ? O69 Dy2 O57 140.51(13) . . ? F2 Dy2 O59 125.22(12) . . ? O54 Dy2 O59 69.80(14) . . ? O62 Dy2 O59 68.66(14) . . ? O64 Dy2 O59 68.25(13) . . ? O69 Dy2 O59 126.24(14) . . ? O57 Dy2 O59 70.11(13) . . ? F2 Dy2 O52 70.07(11) . . ? O54 Dy2 O52 71.96(12) . . ? O62 Dy2 O52 145.15(12) . . ? O64 Dy2 O52 137.59(12) . . ? O69 Dy2 O52 69.29(13) . . ? O57 Dy2 O52 73.72(13) . . ? O59 Dy2 O52 129.60(13) . . ? F2 Dy2 O67 66.63(11) . . ? O54 Dy2 O67 140.30(13) . . ? O62 Dy2 O67 66.70(13) . . ? O64 Dy2 O67 73.96(12) . . ? O69 Dy2 O67 68.52(13) . . ? O57 Dy2 O67 134.74(12) . . ? O59 Dy2 O67 127.53(13) . . ? O52 Dy2 O67 102.86(12) . . ? F3 Cr1 F1 177.29(17) . . ? F3 Cr1 O1 93.93(16) . . ? F1 Cr1 O1 84.44(15) . . ? F3 Cr1 N2 92.33(17) . . ? F1 Cr1 N2 89.31(16) . . ? O1 Cr1 N2 173.74(18) . . ? F3 Cr1 N3 87.4(2) . . ? F1 Cr1 N3 90.47(17) . . ? O1 Cr1 N3 91.28(19) . . ? N2 Cr1 N3 89.2(2) . . ? F3 Cr1 N1 88.9(2) . . ? F1 Cr1 N1 93.27(18) . . ? O1 Cr1 N1 89.5(2) . . ? N2 Cr1 N1 90.4(2) . . ? N3 Cr1 N1 176.2(2) . . ? F4 Cr2 F2 177.79(14) . . ? F4 Cr2 O2 93.60(15) . . ? F2 Cr2 O2 84.19(15) . . ? F4 Cr2 N5 91.18(16) . . ? F2 Cr2 N5 91.03(15) . . ? O2 Cr2 N5 175.01(17) . . ? F4 Cr2 N6 89.14(18) . . ? F2 Cr2 N6 90.84(16) . . ? O2 Cr2 N6 90.59(19) . . ? N5 Cr2 N6 90.89(19) . . ? F4 Cr2 N4 88.19(17) . . ? F2 Cr2 N4 91.87(16) . . ? O2 Cr2 N4 90.59(18) . . ? N5 Cr2 N4 88.15(18) . . ? N6 Cr2 N4 177.14(19) . . ? Cr1 O1 H1A 136(4) . . ? Cr1 O1 H1B 115(4) . . ? H1A O1 H1B 104(6) . . ? Cr2 O2 H2A 123(4) . . ? Cr2 O2 H2B 111(4) . . ? H2A O2 H2B 115(6) . . ? Cr1 F1 Dy1 166.84(16) . . ? Cr2 F2 Dy2 165.66(16) . . ? C5 N1 C1 118.0(6) . . ? C5 N1 Cr1 121.7(4) . . ? C1 N1 Cr1 120.2(5) . . ? C6 N2 C10 118.4(5) . . ? C6 N2 Cr1 119.1(4) . . ? C10 N2 Cr1 122.5(4) . . ? C11 N3 C15 118.1(6) . . ? C11 N3 Cr1 121.4(4) . . ? C15 N3 Cr1 120.5(5) . . ? C36 N4 C40 119.1(5) . . ? C36 N4 Cr2 120.5(4) . . ? C40 N4 Cr2 120.4(4) . . ? C45 N5 C41 118.0(5) . . ? C45 N5 Cr2 122.6(4) . . ? C41 N5 Cr2 119.3(4) . . ? C50 N6 C46 117.4(5) . . ? C50 N6 Cr2 121.3(4) . . ? C46 N6 Cr2 121.2(4) . . ? C17 O17 Dy1 134.6(4) . . ? C19 O19 Dy1 132.8(4) . . ? C22 O22 Dy1 135.2(4) . . ? C24 O24 Dy1 134.3(3) . . ? C27 O27 Dy1 135.3(3) . . ? C29 O29 Dy1 134.7(3) . . ? C32 O32 Dy1 132.1(4) . . ? C34 O34 Dy1 133.6(4) . . ? C52 O52 Dy2 133.9(3) . . ? C54 O54 Dy2 135.5(4) . . ? C57 O57 Dy2 136.8(3) . . ? C59 O59 Dy2 136.3(4) . . ? C62 O62 Dy2 133.9(4) . . ? C64 O64 Dy2 133.6(4) . . ? C67 O67 Dy2 130.2(4) . . ? C69 O69 Dy2 132.9(4) . . ? N1 C1 C2 121.5(8) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C1 C2 C3 119.9(7) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 119.3(7) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 117.9(8) . . ? C3 C4 H4 121.1 . . ? C5 C4 H4 121.1 . . ? N1 C5 C4 123.3(6) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? N2 C6 C7 122.2(5) . . ? N2 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C6 C7 C8 119.7(5) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C7 C8 C9 118.0(6) . . ? C7 C8 H8 121.0 . . ? C9 C8 H8 121.0 . . ? C10 C9 C8 119.1(6) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? N2 C10 C9 122.6(5) . . ? N2 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? N3 C11 C12 122.7(6) . . ? N3 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C11 C12 C13 117.9(7) . . ? C11 C12 H12 121.0 . . ? C13 C12 H12 121.0 . . ? C14 C13 C12 119.8(7) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 119.8(7) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? N3 C15 C14 121.7(7) . . ? N3 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? F23 C16 F24 109.2(7) . . ? F23 C16 F25 107.4(6) . . ? F24 C16 F25 107.7(6) . . ? F23 C16 C17 109.2(6) . . ? F24 C16 C17 111.1(6) . . ? F25 C16 C17 112.1(6) . . ? O17 C17 C18 128.4(5) . . ? O17 C17 C16 112.3(5) . . ? C18 C17 C16 119.3(5) . . ? C17 C18 C19 122.5(5) . . ? C17 C18 H18 118.7 . . ? C19 C18 H18 118.7 . . ? O19 C19 C18 128.7(5) . . ? O19 C19 C20 113.9(5) . . ? C18 C19 C20 117.5(5) . . ? F27 C20 F28 105.8(7) . . ? F27 C20 F26 108.5(6) . . ? F28 C20 F26 104.3(6) . . ? F27 C20 C19 113.6(6) . . ? F28 C20 C19 110.6(5) . . ? F26 C20 C19 113.3(6) . . ? F29 C21 F30 106.2(6) . . ? F29 C21 F31 107.1(5) . . ? F30 C21 F31 106.6(5) . . ? F29 C21 C22 112.6(5) . . ? F30 C21 C22 110.3(5) . . ? F31 C21 C22 113.5(5) . . ? O22 C22 C23 128.2(5) . . ? O22 C22 C21 112.8(5) . . ? C23 C22 C21 119.0(5) . . ? C22 C23 C24 121.5(5) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? O24 C24 C23 128.3(5) . . ? O24 C24 C25 115.3(5) . . ? C23 C24 C25 116.1(5) . . ? F34 C25 F33 108.1(5) . . ? F34 C25 F32 107.7(5) . . ? F33 C25 F32 106.3(5) . . ? F34 C25 C24 112.0(5) . . ? F33 C25 C24 111.1(5) . . ? F32 C25 C24 111.5(5) . . ? F13 C26 F11 108.4(6) . . ? F13 C26 F12 106.0(6) . . ? F11 C26 F12 106.6(6) . . ? F13 C26 C27 110.7(6) . . ? F11 C26 C27 112.2(5) . . ? F12 C26 C27 112.6(6) . . ? O27 C27 C28 128.3(5) . . ? O27 C27 C26 116.0(5) . . ? C28 C27 C26 115.7(5) . . ? C27 C28 C29 120.8(5) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? O29 C29 C28 128.1(5) . . ? O29 C29 C30 115.0(5) . . ? C28 C29 C30 116.8(5) . . ? F14 C30 F15 107.2(6) . . ? F14 C30 F16 107.6(6) . . ? F15 C30 F16 105.8(6) . . ? F14 C30 C29 110.5(5) . . ? F15 C30 C29 114.1(5) . . ? F16 C30 C29 111.3(5) . . ? F17 C31 F18 108.7(7) . . ? F17 C31 F19 105.9(6) . . ? F18 C31 F19 105.2(5) . . ? F17 C31 C32 111.2(5) . . ? F18 C31 C32 110.4(5) . . ? F19 C31 C32 115.2(6) . . ? O32 C32 C33 127.6(5) . . ? O32 C32 C31 114.0(5) . . ? C33 C32 C31 118.4(5) . . ? C32 C33 C34 121.8(5) . . ? C32 C33 H33 119.1 . . ? C34 C33 H33 119.1 . . ? O34 C34 C33 129.3(6) . . ? O34 C34 C35 114.5(6) . . ? C33 C34 C35 116.1(6) . . ? F21 C35 F20 113.0(7) . . ? F21 C35 F22 105.7(8) . . ? F20 C35 F22 105.1(6) . . ? F21 C35 C34 113.0(6) . . ? F20 C35 C34 111.4(7) . . ? F22 C35 C34 108.0(6) . . ? N4 C36 C37 121.9(6) . . ? N4 C36 H36 119.1 . . ? C37 C36 H36 119.1 . . ? C36 C37 C38 119.3(6) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C39 C38 C37 118.5(6) . . ? C39 C38 H38 120.8 . . ? C37 C38 H38 120.8 . . ? C40 C39 C38 119.2(6) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? N4 C40 C39 122.0(6) . . ? N4 C40 H40 119.0 . . ? C39 C40 H40 119.0 . . ? N5 C41 C42 122.7(5) . . ? N5 C41 H41 118.7 . . ? C42 C41 H41 118.7 . . ? C43 C42 C41 118.9(6) . . ? C43 C42 H42 120.6 . . ? C41 C42 H42 120.6 . . ? C42 C43 C44 119.4(5) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? C43 C44 C45 118.3(5) . . ? C43 C44 H44 120.9 . . ? C45 C44 H44 120.9 . . ? N5 C45 C44 122.7(5) . . ? N5 C45 H45 118.6 . . ? C44 C45 H45 118.6 . . ? N6 C46 C47 122.8(6) . . ? N6 C46 H46 118.6 . . ? C47 C46 H46 118.6 . . ? C48 C47 C46 118.6(7) . . ? C48 C47 H47 120.7 . . ? C46 C47 H47 120.7 . . ? C47 C48 C49 119.2(7) . . ? C47 C48 H48 120.4 . . ? C49 C48 H48 120.4 . . ? C48 C49 C50 119.3(6) . . ? C48 C49 H49 120.4 . . ? C50 C49 H49 120.4 . . ? N6 C50 C49 122.6(6) . . ? N6 C50 H50 118.7 . . ? C49 C50 H50 118.7 . . ? F48 C51 F47 107.2(5) . . ? F48 C51 F49 107.9(5) . . ? F47 C51 F49 106.1(5) . . ? F48 C51 C52 112.2(5) . . ? F47 C51 C52 109.0(5) . . ? F49 C51 C52 114.0(5) . . ? O52 C52 C53 127.9(5) . . ? O52 C52 C51 114.8(5) . . ? C53 C52 C51 117.1(5) . . ? C54 C53 C52 120.9(5) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? O54 C54 C53 128.7(5) . . ? O54 C54 C55 114.7(5) . . ? C53 C54 C55 116.5(5) . . ? F50 C55 F51 108.8(6) . . ? F50 C55 F52 104.5(6) . . ? F51 C55 F52 107.1(6) . . ? F50 C55 C54 111.0(6) . . ? F51 C55 C54 114.2(6) . . ? F52 C55 C54 110.7(5) . . ? F54 C56 F55 107.4(5) . . ? F54 C56 F53 107.2(5) . . ? F55 C56 F53 105.9(5) . . ? F54 C56 C57 114.1(5) . . ? F55 C56 C57 110.9(5) . . ? F53 C56 C57 110.9(5) . . ? O57 C57 C58 128.2(5) . . ? O57 C57 C56 112.8(5) . . ? C58 C57 C56 119.0(5) . . ? C57 C58 C59 120.6(5) . . ? C57 C58 H58 119.7 . . ? C59 C58 H58 119.7 . . ? O59 C59 C58 127.9(5) . . ? O59 C59 C60 113.3(5) . . ? C58 C59 C60 118.8(5) . . ? F58 C60 F56 109.4(6) . . ? F58 C60 F57 105.5(6) . . ? F56 C60 F57 104.8(5) . . ? F58 C60 C59 112.1(5) . . ? F56 C60 C59 114.8(5) . . ? F57 C60 C59 109.6(5) . . ? F36 C61 F35 106.8(5) . . ? F36 C61 F37 107.3(5) . . ? F35 C61 F37 105.7(5) . . ? F36 C61 C62 112.2(5) . . ? F35 C61 C62 110.0(5) . . ? F37 C61 C62 114.3(5) . . ? O62 C62 C63 127.6(5) . . ? O62 C62 C61 113.4(5) . . ? C63 C62 C61 119.0(5) . . ? C62 C63 C64 122.8(5) . . ? C62 C63 H63 118.6 . . ? C64 C63 H63 118.6 . . ? O64 C64 C63 128.3(5) . . ? O64 C64 C65 114.4(5) . . ? C63 C64 C65 117.4(5) . . ? F40 C65 F39 106.3(6) . . ? F40 C65 F38 107.6(6) . . ? F39 C65 F38 105.5(6) . . ? F40 C65 C64 113.2(5) . . ? F39 C65 C64 111.0(5) . . ? F38 C65 C64 112.8(5) . . ? F43 C66 F42 108.0(7) . . ? F43 C66 F41 106.0(7) . . ? F42 C66 F41 104.2(7) . . ? F43 C66 C67 115.4(6) . . ? F42 C66 C67 111.8(6) . . ? F41 C66 C67 110.8(6) . . ? O67 C67 C68 127.0(6) . . ? O67 C67 C66 115.2(5) . . ? C68 C67 C66 117.8(5) . . ? C67 C68 C69 121.2(5) . . ? C67 C68 H68 119.4 . . ? C69 C68 H68 119.4 . . ? O69 C69 C68 128.5(6) . . ? O69 C69 C70 113.4(6) . . ? C68 C69 C70 118.0(6) . . ? F46 C70 F45 108.0(7) . . ? F46 C70 F44 106.1(7) . . ? F45 C70 F44 107.9(6) . . ? F46 C70 C69 111.7(6) . . ? F45 C70 C69 112.4(6) . . ? F44 C70 C69 110.5(7) . . ? Cl81 C80 Cl82 112.2(5) . . ? Cl81 C80 H80A 109.2 . . ? Cl82 C80 H80A 109.2 . . ? Cl81 C80 H80B 109.2 . . ? Cl82 C80 H80B 109.2 . . ? H80A C80 H80B 107.9 . . ? Cl91 C90 Cl92 111.4(6) . . ? Cl91 C90 H90A 109.4 . . ? Cl92 C90 H90A 109.4 . . ? Cl91 C90 H90B 109.4 . . ? Cl92 C90 H90B 109.4 . . ? H90A C90 H90B 108.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A F3 0.86(2) 1.69(3) 2.527(5) 164(7) 2_557 O1 H1B O32 0.87(2) 2.16(4) 2.945(6) 150(6) . O2 H2A F4 0.87(2) 1.64(2) 2.512(5) 177(7) 2_666 O2 H2B O67 0.88(2) 1.95(3) 2.800(5) 161(6) . _diffrn_measured_fraction_theta_max .985 _diffrn_reflns_theta_full 27.67 _diffrn_measured_fraction_theta_full .985 _refine_diff_density_max 1.389 _refine_diff_density_min -.938 _refine_diff_density_rms .138 data_kcd796_2Ln _database_code_depnum_ccdc_archive 'CCDC 878247' #TrackingRef 'Ln2Cr2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H36 Cr2 F42 N6 O12 Tb2' _chemical_formula_sum 'C60 H36 Cr2 F42 N6 O12 Tb2' _chemical_formula_weight 2252.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5395(9) _cell_length_b 13.2423(10) _cell_length_c 15.094(2) _cell_angle_alpha 97.193(16) _cell_angle_beta 110.446(8) _cell_angle_gamma 116.354(7) _cell_volume 1983.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 122(1) _cell_measurement_reflns_used 68046 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 40.00 _exptl_crystal_description Rod _exptl_crystal_colour pink _exptl_crystal_size_max 0.369 _exptl_crystal_size_mid 0.132 _exptl_crystal_size_min 0.130 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.886 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1090 _exptl_absorpt_coefficient_mu 2.185 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.408 _exptl_absorpt_correction_T_max 0.795 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 122(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\w and \f scans' _diffrn_reflns_number 130374 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 40.00 _reflns_number_total 24542 _reflns_number_gt 20391 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'COLLECT (Nonius, 1999)' _computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Ortep-3 (Farrugia, 1997) and Mercury (Macrae et. al., 2006) ; _computing_publication_material SHELXL-97 _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^)+(0.0000P)^2^+1.2144P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24542 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0655 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.743197(6) 0.196845(6) 0.203274(4) 0.01445(2) Uani 1 1 d . . . Cr1 Cr 0.52223(2) 0.17082(2) -0.082221(15) 0.01587(4) Uani 1 1 d . . . F1 F 0.61360(8) 0.14678(8) 0.03726(6) 0.01813(14) Uani 1 1 d . . . F2 F 0.41011(8) 0.00106(8) -0.15073(6) 0.01816(14) Uani 1 1 d . . . F3 F 0.62250(10) 0.33296(9) -0.02005(7) 0.02463(17) Uani 1 1 d . . . N1 N 0.65686(12) 0.17395(12) -0.13319(9) 0.0204(2) Uani 1 1 d . . . N2 N 0.43159(13) 0.20366(12) -0.21044(9) 0.0211(2) Uani 1 1 d . . . N3 N 0.37996(13) 0.15631(12) -0.03633(9) 0.0208(2) Uani 1 1 d . . . O1 O 0.90564(10) 0.27676(11) 0.14127(8) 0.02222(19) Uani 1 1 d . . . O2 O 0.87221(11) 0.10448(11) 0.23249(9) 0.02283(19) Uani 1 1 d . . . O3 O 0.94832(11) 0.34458(12) 0.34028(8) 0.0265(2) Uani 1 1 d . . . O4 O 0.74647(13) 0.15058(13) 0.35177(9) 0.0286(2) Uani 1 1 d . . . O5 O 0.77385(11) 0.38247(10) 0.19244(8) 0.02185(18) Uani 1 1 d . . . O6 O 0.58143(11) 0.21695(10) 0.23343(9) 0.02236(19) Uani 1 1 d . . . C1 C 0.78428(15) 0.26564(17) -0.08495(12) 0.0275(3) Uani 1 1 d . . . H1 H 0.8111 0.3266 -0.0271 0.033 Uiso 1 1 calc R . . C2 C 0.87788(18) 0.2738(2) -0.11723(15) 0.0370(4) Uani 1 1 d . . . H2 H 0.9676 0.3395 -0.0819 0.044 Uiso 1 1 calc R . . C3 C 0.8391(2) 0.1853(2) -0.20133(16) 0.0382(4) Uani 1 1 d . . . H3 H 0.9016 0.1893 -0.2246 0.046 Uiso 1 1 calc R . . C4 C 0.7076(2) 0.09079(19) -0.25102(15) 0.0368(4) Uani 1 1 d . . . H4 H 0.6786 0.0290 -0.3090 0.044 Uiso 1 1 calc R . . C5 C 0.61889(18) 0.08742(16) -0.21504(13) 0.0287(3) Uani 1 1 d . . . H5 H 0.5288 0.0223 -0.2490 0.034 Uiso 1 1 calc R . . C6 C 0.30484(17) 0.12670(16) -0.27978(13) 0.0301(3) Uani 1 1 d . . . H6 H 0.2538 0.0541 -0.2706 0.036 Uiso 1 1 calc R . . C7 C 0.2459(2) 0.1501(2) -0.36470(15) 0.0424(5) Uani 1 1 d . . . H7 H 0.1556 0.0943 -0.4126 0.051 Uiso 1 1 calc R . . C8 C 0.3193(2) 0.2546(2) -0.37905(15) 0.0404(5) Uani 1 1 d . . . H8 H 0.2807 0.2718 -0.4370 0.048 Uiso 1 1 calc R . . C9 C 0.4497(2) 0.33394(18) -0.30773(15) 0.0359(4) Uani 1 1 d . . . H9 H 0.5025 0.4068 -0.3157 0.043 Uiso 1 1 calc R . . C10 C 0.50261(17) 0.30597(16) -0.22418(13) 0.0298(3) Uani 1 1 d . . . H10 H 0.5923 0.3612 -0.1749 0.036 Uiso 1 1 calc R . . C11 C 0.32335(15) 0.06617(14) -0.00418(11) 0.0226(2) Uani 1 1 d . . . H11 H 0.3542 0.0123 0.0018 0.027 Uiso 1 1 calc R . . C12 C 0.22158(18) 0.04880(18) 0.02059(14) 0.0307(3) Uani 1 1 d . . . H12 H 0.1823 -0.0164 0.0424 0.037 Uiso 1 1 calc R . . C13 C 0.1781(2) 0.1286(2) 0.01299(17) 0.0384(4) Uani 1 1 d . . . H13 H 0.1082 0.1187 0.0293 0.046 Uiso 1 1 calc R . . C14 C 0.2375(2) 0.2222(2) -0.01858(17) 0.0392(4) Uani 1 1 d . . . H14 H 0.2094 0.2780 -0.0241 0.047 Uiso 1 1 calc R . . C15 C 0.3387(2) 0.23400(18) -0.04210(14) 0.0306(3) Uani 1 1 d . . . H15 H 0.3803 0.2993 -0.0630 0.037 Uiso 1 1 calc R . . C21 C 1.12217(17) 0.40547(18) 0.16054(15) 0.0322(3) Uani 1 1 d . . . C22 C 1.02246(14) 0.29888(15) 0.17714(11) 0.0225(2) Uani 1 1 d . . . C23 C 1.07408(16) 0.23839(18) 0.23046(13) 0.0287(3) Uani 1 1 d . . . H23 H 1.1650 0.2621 0.2517 0.034 Uiso 1 1 calc R . . C24 C 0.99243(15) 0.14407(16) 0.25206(12) 0.0249(3) Uani 1 1 d . . . C25 C 1.0507(2) 0.0766(2) 0.30737(16) 0.0361(4) Uani 1 1 d . . . C31 C 1.1542(2) 0.4678(2) 0.48545(15) 0.0414(5) Uani 1 1 d . . . C32 C 1.00861(18) 0.36058(18) 0.43076(12) 0.0311(3) Uani 1 1 d . . . C33 C 0.9606(2) 0.2937(2) 0.48648(14) 0.0452(5) Uani 1 1 d . . . H33 H 1.0169 0.3150 0.5557 0.054 Uiso 1 1 calc R . . C34 C 0.8302(2) 0.1952(2) 0.44158(13) 0.0355(4) Uani 1 1 d . . . C35 C 0.7811(3) 0.1342(3) 0.51182(17) 0.0544(7) Uani 1 1 d . . . C41 C 0.7596(2) 0.54763(18) 0.16512(18) 0.0365(4) Uani 1 1 d . . . C42 C 0.70784(16) 0.42994(14) 0.18730(12) 0.0243(3) Uani 1 1 d . . . C43 C 0.59688(17) 0.39469(16) 0.20693(14) 0.0289(3) Uani 1 1 d . . . H43 H 0.5543 0.4394 0.2004 0.035 Uiso 1 1 calc R . . C44 C 0.55029(15) 0.29519(15) 0.23560(12) 0.0234(3) Uani 1 1 d . . . C45 C 0.45453(18) 0.27689(17) 0.28153(15) 0.0319(3) Uani 1 1 d . . . F4 F 1.1666(2) 0.37078(18) 0.10284(18) 0.0766(6) Uani 1 1 d . . . F5 F 1.22815(16) 0.48242(18) 0.24537(14) 0.0826(7) Uani 1 1 d . . . F6 F 1.06973(14) 0.46270(13) 0.11632(13) 0.0495(3) Uani 1 1 d . . . F7 F 1.18010(16) 0.1247(2) 0.33617(16) 0.0781(7) Uani 1 1 d . . . F8 F 0.9843(2) -0.03725(18) 0.25272(14) 0.0747(6) Uani 1 1 d . . . F9 F 1.03707(14) 0.07750(15) 0.39066(10) 0.0483(3) Uani 1 1 d . . . F10 F 1.23671(17) 0.43159(18) 0.5002(2) 0.1016(9) Uani 1 1 d . . . F11 F 1.1799(2) 0.5346(2) 0.57098(15) 0.0935(8) Uani 1 1 d . . . F12 F 1.18105(18) 0.54159(18) 0.43563(15) 0.0838(7) Uani 1 1 d . . . F13 F 0.7723(4) 0.2048(3) 0.5733(2) 0.1305(13) Uani 1 1 d . . . F14 F 0.8635(3) 0.1082(3) 0.56891(18) 0.1000(8) Uani 1 1 d . . . F15 F 0.6667(3) 0.0338(3) 0.46358(16) 0.1131(11) Uani 1 1 d . . . F16 F 0.84054(14) 0.56288(12) 0.12406(12) 0.0431(3) Uani 1 1 d . . . F17 F 0.8244(2) 0.64016(14) 0.24839(15) 0.0770(6) Uani 1 1 d . . . F18 F 0.65847(17) 0.55313(16) 0.10077(16) 0.0636(5) Uani 1 1 d . . . F19 F 0.51651(15) 0.3036(2) 0.37852(11) 0.0749(6) Uani 1 1 d . . . F20 F 0.39999(19) 0.34324(17) 0.26394(19) 0.0749(6) Uani 1 1 d . . . F21 F 0.35334(13) 0.16559(12) 0.24559(11) 0.0450(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01135(2) 0.01709(3) 0.01394(2) 0.00679(2) 0.00579(2) 0.00630(2) Cr1 0.01514(8) 0.01657(9) 0.01586(8) 0.00920(7) 0.00665(7) 0.00763(7) F1 0.0173(3) 0.0203(4) 0.0157(3) 0.0091(3) 0.0060(3) 0.0094(3) F2 0.0159(3) 0.0176(4) 0.0187(3) 0.0086(3) 0.0073(3) 0.0068(3) F3 0.0277(4) 0.0179(4) 0.0235(4) 0.0090(3) 0.0090(3) 0.0099(3) N1 0.0191(5) 0.0225(5) 0.0200(5) 0.0118(4) 0.0103(4) 0.0090(4) N2 0.0207(5) 0.0217(5) 0.0211(5) 0.0130(4) 0.0087(4) 0.0104(4) N3 0.0219(5) 0.0232(5) 0.0224(5) 0.0119(4) 0.0110(4) 0.0139(5) O1 0.0169(4) 0.0300(5) 0.0226(4) 0.0125(4) 0.0109(4) 0.0121(4) O2 0.0168(4) 0.0266(5) 0.0273(5) 0.0132(4) 0.0097(4) 0.0122(4) O3 0.0206(5) 0.0293(6) 0.0184(4) 0.0027(4) 0.0042(4) 0.0094(4) O4 0.0281(5) 0.0393(7) 0.0193(4) 0.0146(5) 0.0119(4) 0.0163(5) O5 0.0205(4) 0.0193(5) 0.0271(5) 0.0087(4) 0.0128(4) 0.0097(4) O6 0.0208(4) 0.0227(5) 0.0278(5) 0.0099(4) 0.0150(4) 0.0113(4) C1 0.0187(6) 0.0327(8) 0.0261(6) 0.0122(6) 0.0116(5) 0.0081(6) C2 0.0230(7) 0.0489(11) 0.0351(8) 0.0169(8) 0.0183(7) 0.0112(7) C3 0.0376(9) 0.0532(12) 0.0401(9) 0.0253(9) 0.0301(8) 0.0244(9) C4 0.0443(10) 0.0376(10) 0.0374(9) 0.0153(8) 0.0308(8) 0.0183(8) C5 0.0305(7) 0.0271(7) 0.0280(7) 0.0101(6) 0.0192(6) 0.0101(6) C6 0.0228(6) 0.0284(8) 0.0276(7) 0.0171(6) 0.0042(5) 0.0083(6) C7 0.0299(8) 0.0401(10) 0.0351(9) 0.0239(8) 0.0000(7) 0.0100(8) C8 0.0378(9) 0.0410(10) 0.0328(8) 0.0259(8) 0.0068(7) 0.0170(8) C9 0.0367(9) 0.0330(9) 0.0344(8) 0.0251(7) 0.0133(7) 0.0143(7) C10 0.0262(7) 0.0275(7) 0.0287(7) 0.0183(6) 0.0090(6) 0.0092(6) C11 0.0241(6) 0.0226(6) 0.0234(6) 0.0104(5) 0.0130(5) 0.0118(5) C12 0.0310(8) 0.0347(9) 0.0335(8) 0.0163(7) 0.0214(7) 0.0164(7) C13 0.0372(9) 0.0554(13) 0.0438(10) 0.0241(9) 0.0280(8) 0.0314(10) C14 0.0492(11) 0.0532(12) 0.0489(11) 0.0293(10) 0.0330(10) 0.0413(11) C15 0.0398(9) 0.0374(9) 0.0377(8) 0.0237(7) 0.0250(7) 0.0293(8) C21 0.0220(7) 0.0360(9) 0.0401(9) 0.0169(7) 0.0190(7) 0.0116(6) C22 0.0167(5) 0.0277(7) 0.0235(6) 0.0087(5) 0.0120(5) 0.0099(5) C23 0.0173(6) 0.0390(9) 0.0350(8) 0.0175(7) 0.0140(6) 0.0158(6) C24 0.0198(6) 0.0338(8) 0.0269(6) 0.0137(6) 0.0109(5) 0.0175(6) C25 0.0301(8) 0.0521(12) 0.0426(10) 0.0271(9) 0.0180(7) 0.0300(9) C31 0.0280(8) 0.0439(11) 0.0261(8) -0.0016(7) -0.0005(6) 0.0121(8) C32 0.0250(7) 0.0356(9) 0.0205(6) 0.0007(6) 0.0034(5) 0.0142(7) C33 0.0398(10) 0.0587(14) 0.0181(7) 0.0111(8) 0.0051(7) 0.0178(10) C34 0.0423(10) 0.0490(11) 0.0213(7) 0.0182(7) 0.0162(7) 0.0256(9) C35 0.0696(17) 0.0655(17) 0.0272(9) 0.0254(10) 0.0259(10) 0.0293(14) C41 0.0447(10) 0.0269(8) 0.0539(11) 0.0224(8) 0.0307(9) 0.0223(8) C42 0.0245(6) 0.0217(6) 0.0302(7) 0.0112(5) 0.0142(6) 0.0127(5) C43 0.0279(7) 0.0271(7) 0.0403(9) 0.0141(7) 0.0190(7) 0.0177(6) C44 0.0184(6) 0.0251(7) 0.0263(6) 0.0060(5) 0.0115(5) 0.0107(5) C45 0.0263(7) 0.0308(8) 0.0412(9) 0.0074(7) 0.0214(7) 0.0136(6) F4 0.1094(15) 0.0821(13) 0.1298(17) 0.0729(13) 0.1100(15) 0.0685(12) F5 0.0377(8) 0.0698(12) 0.0587(10) 0.0240(9) 0.0021(7) -0.0194(7) F6 0.0364(6) 0.0359(7) 0.0821(10) 0.0351(7) 0.0311(7) 0.0164(6) F7 0.0446(8) 0.1336(18) 0.1171(15) 0.0978(15) 0.0520(10) 0.0672(11) F8 0.1109(16) 0.0665(11) 0.0582(10) 0.0195(9) 0.0163(10) 0.0723(12) F9 0.0447(7) 0.0750(10) 0.0427(7) 0.0384(7) 0.0206(6) 0.0392(8) F10 0.0303(8) 0.0542(11) 0.182(3) 0.0153(14) 0.0183(11) 0.0221(8) F11 0.0625(12) 0.0799(14) 0.0583(11) -0.0342(10) 0.0132(9) 0.0022(10) F12 0.0480(9) 0.0570(11) 0.0671(11) 0.0191(9) -0.0059(8) -0.0080(8) F13 0.269(4) 0.132(2) 0.132(2) 0.098(2) 0.174(3) 0.137(3) F14 0.1166(19) 0.123(2) 0.0864(15) 0.0833(16) 0.0464(14) 0.0705(17) F15 0.0950(16) 0.128(2) 0.0586(11) 0.0546(14) 0.0395(12) 0.0050(15) F16 0.0413(7) 0.0327(6) 0.0689(9) 0.0293(6) 0.0370(7) 0.0177(5) F17 0.1211(17) 0.0232(7) 0.0754(12) 0.0115(7) 0.0572(12) 0.0212(9) F18 0.0621(10) 0.0669(11) 0.1118(14) 0.0684(11) 0.0540(10) 0.0510(9) F19 0.0398(8) 0.1229(17) 0.0331(7) -0.0003(8) 0.0233(6) 0.0225(9) F20 0.0758(11) 0.0662(11) 0.1559(19) 0.0618(12) 0.0927(14) 0.0564(10) F21 0.0336(6) 0.0364(6) 0.0570(8) 0.0072(6) 0.0317(6) 0.0061(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 Tb1 F2 2.2658(9) 2_655 ? Tb1 F1 2.2675(9) . ? Tb1 O6 2.3424(10) . ? Tb1 O5 2.3500(11) . ? Tb1 O3 2.3500(13) . ? Tb1 O2 2.3877(11) . ? Tb1 O4 2.3880(11) . ? Tb1 O1 2.4106(10) . ? Cr1 F3 1.8291(11) . ? Cr1 F1 1.9210(8) . ? Cr1 F2 1.9223(10) . ? Cr1 N3 2.0716(13) . ? Cr1 N1 2.0728(13) . ? Cr1 N2 2.0831(12) . ? F2 Tb1 2.2659(9) 2_655 ? N1 C1 1.342(2) . ? N1 C5 1.348(2) . ? N2 C6 1.339(2) . ? N2 C10 1.342(2) . ? N3 C15 1.341(2) . ? N3 C11 1.3408(19) . ? O1 C22 1.2450(17) . ? O2 C24 1.2582(18) . ? O3 C32 1.243(2) . ? O4 C34 1.242(2) . ? O5 C42 1.2311(19) . ? O6 C44 1.2596(19) . ? C1 C2 1.388(2) . ? C1 H1 0.9500 . ? C2 C3 1.383(3) . ? C2 H2 0.9500 . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.385(2) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.387(2) . ? C6 H6 0.9500 . ? C7 C8 1.376(3) . ? C7 H7 0.9500 . ? C8 C9 1.378(3) . ? C8 H8 0.9500 . ? C9 C10 1.385(2) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.384(2) . ? C11 H11 0.9500 . ? C12 C13 1.387(3) . ? C12 H12 0.9500 . ? C13 C14 1.377(3) . ? C13 H13 0.9500 . ? C14 C15 1.383(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C21 F6 1.310(2) . ? C21 F5 1.314(3) . ? C21 F4 1.321(2) . ? C21 C22 1.536(2) . ? C22 C23 1.402(2) . ? C23 C24 1.384(2) . ? C23 H23 0.9500 . ? C24 C25 1.539(2) . ? C25 F8 1.320(3) . ? C25 F7 1.322(2) . ? C25 F9 1.326(2) . ? C31 F10 1.287(3) . ? C31 F12 1.304(3) . ? C31 F11 1.312(3) . ? C31 C32 1.544(3) . ? C32 C33 1.386(3) . ? C33 C34 1.395(3) . ? C33 H33 0.9500 . ? C34 C35 1.544(3) . ? C35 F15 1.300(4) . ? C35 F13 1.302(4) . ? C35 F14 1.303(4) . ? C41 F16 1.321(2) . ? C41 F17 1.326(3) . ? C41 F18 1.340(3) . ? C41 C42 1.532(2) . ? C42 C43 1.410(2) . ? C43 C44 1.379(2) . ? C43 H43 0.9500 . ? C44 C45 1.532(2) . ? C45 F19 1.305(3) . ? C45 F21 1.317(2) . ? C45 F20 1.332(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 F2 Tb1 F1 74.52(4) 2_655 . ? F2 Tb1 O6 83.21(4) 2_655 . ? F1 Tb1 O6 88.07(4) . . ? F2 Tb1 O5 144.21(3) 2_655 . ? F1 Tb1 O5 78.71(4) . . ? O6 Tb1 O5 72.49(4) . . ? F2 Tb1 O3 139.94(4) 2_655 . ? F1 Tb1 O3 143.43(4) . . ? O6 Tb1 O3 104.97(4) . . ? O5 Tb1 O3 73.25(4) . . ? F2 Tb1 O2 75.53(4) 2_655 . ? F1 Tb1 O2 111.79(4) . . ? O6 Tb1 O2 145.13(4) . . ? O5 Tb1 O2 137.56(4) . . ? O3 Tb1 O2 76.44(4) . . ? F2 Tb1 O4 74.29(4) 2_655 . ? F1 Tb1 O4 144.43(4) . . ? O6 Tb1 O4 71.67(4) . . ? O5 Tb1 O4 119.91(5) . . ? O3 Tb1 O4 71.59(5) . . ? O2 Tb1 O4 76.09(4) . . ? F2 Tb1 O1 122.57(4) 2_655 . ? F1 Tb1 O1 77.30(4) . . ? O6 Tb1 O1 144.21(4) . . ? O5 Tb1 O1 72.69(4) . . ? O3 Tb1 O1 72.31(4) . . ? O2 Tb1 O1 70.22(4) . . ? O4 Tb1 O1 135.10(4) . . ? F3 Cr1 F1 91.30(4) . . ? F3 Cr1 F2 177.43(4) . . ? F1 Cr1 F2 90.77(4) . . ? F3 Cr1 N3 91.23(5) . . ? F1 Cr1 N3 89.57(4) . . ? F2 Cr1 N3 87.27(5) . . ? F3 Cr1 N1 92.36(5) . . ? F1 Cr1 N1 90.64(4) . . ? F2 Cr1 N1 89.14(5) . . ? N3 Cr1 N1 176.40(5) . . ? F3 Cr1 N2 86.68(5) . . ? F1 Cr1 N2 177.35(5) . . ? F2 Cr1 N2 91.30(5) . . ? N3 Cr1 N2 92.18(5) . . ? N1 Cr1 N2 87.73(5) . . ? Cr1 F1 Tb1 156.21(5) . . ? Cr1 F2 Tb1 165.32(5) . 2_655 ? C1 N1 C5 119.09(14) . . ? C1 N1 Cr1 119.30(11) . . ? C5 N1 Cr1 121.59(11) . . ? C6 N2 C10 118.56(13) . . ? C6 N2 Cr1 122.57(10) . . ? C10 N2 Cr1 118.87(11) . . ? C15 N3 C11 118.68(14) . . ? C15 N3 Cr1 120.64(11) . . ? C11 N3 Cr1 120.63(10) . . ? C22 O1 Tb1 129.04(10) . . ? C24 O2 Tb1 131.41(11) . . ? C32 O3 Tb1 136.59(13) . . ? C34 O4 Tb1 134.82(13) . . ? C42 O5 Tb1 134.72(10) . . ? C44 O6 Tb1 135.02(10) . . ? N1 C1 C2 121.76(17) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C3 C2 C1 119.26(18) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 118.92(16) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C3 C4 C5 119.15(19) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.82(17) . . ? N1 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? N2 C6 C7 121.82(16) . . ? N2 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C8 C7 C6 119.53(18) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 118.72(16) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C8 C9 C10 119.07(17) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N2 C10 C9 122.29(16) . . ? N2 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? N3 C11 C12 122.32(15) . . ? N3 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C11 C12 C13 118.64(17) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? C14 C13 C12 119.09(16) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C15 119.11(17) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? N3 C15 C14 122.14(17) . . ? N3 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? F6 C21 F5 108.2(2) . . ? F6 C21 F4 106.12(17) . . ? F5 C21 F4 106.20(19) . . ? F6 C21 C22 112.88(14) . . ? F5 C21 C22 111.63(16) . . ? F4 C21 C22 111.41(17) . . ? O1 C22 C23 128.07(14) . . ? O1 C22 C21 115.87(14) . . ? C23 C22 C21 116.06(13) . . ? C24 C23 C22 119.92(13) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? O2 C24 C23 127.88(14) . . ? O2 C24 C25 113.45(15) . . ? C23 C24 C25 118.67(14) . . ? F8 C25 F7 110.3(2) . . ? F8 C25 F9 105.50(19) . . ? F7 C25 F9 105.57(18) . . ? F8 C25 C24 111.02(16) . . ? F7 C25 C24 113.61(17) . . ? F9 C25 C24 110.43(16) . . ? F10 C31 F12 107.1(2) . . ? F10 C31 F11 110.0(2) . . ? F12 C31 F11 104.0(2) . . ? F10 C31 C32 110.5(2) . . ? F12 C31 C32 113.17(17) . . ? F11 C31 C32 111.8(2) . . ? O3 C32 C33 127.70(18) . . ? O3 C32 C31 114.85(18) . . ? C33 C32 C31 117.45(17) . . ? C32 C33 C34 120.40(16) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? O4 C34 C33 128.34(18) . . ? O4 C34 C35 115.1(2) . . ? C33 C34 C35 116.57(18) . . ? F15 C35 F13 109.1(3) . . ? F15 C35 F14 105.6(3) . . ? F13 C35 F14 105.2(3) . . ? F15 C35 C34 113.01(19) . . ? F13 C35 C34 111.1(2) . . ? F14 C35 C34 112.4(2) . . ? F16 C41 F17 107.86(19) . . ? F16 C41 F18 106.05(18) . . ? F17 C41 F18 107.34(19) . . ? F16 C41 C42 113.57(15) . . ? F17 C41 C42 110.69(18) . . ? F18 C41 C42 111.04(17) . . ? O5 C42 C43 128.15(15) . . ? O5 C42 C41 115.86(14) . . ? C43 C42 C41 115.79(15) . . ? C44 C43 C42 119.81(15) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? O6 C44 C43 127.93(14) . . ? O6 C44 C45 113.53(15) . . ? C43 C44 C45 118.44(15) . . ? F19 C45 F21 107.02(19) . . ? F19 C45 F20 107.85(19) . . ? F21 C45 F20 105.62(17) . . ? F19 C45 C44 110.72(15) . . ? F21 C45 C44 112.55(15) . . ? F20 C45 C44 112.74(17) . . ? _diffrn_measured_fraction_theta_max .998 _diffrn_reflns_theta_full 40.00 _diffrn_measured_fraction_theta_full .998 _refine_diff_density_max 2.128 _refine_diff_density_min -.899 _refine_diff_density_rms .119 data_kcd952_A2Y_1Ln _database_code_depnum_ccdc_archive 'CCDC 878248' #TrackingRef 'Ln2Cr2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H28 Cr2 F40 N4 O14 Y2' _chemical_formula_sum 'C50 H28 Cr2 F40 N4 O14 Y2' _chemical_formula_weight 1950.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.181(2) _cell_length_b 12.530(3) _cell_length_c 12.550(2) _cell_angle_alpha 65.253(11) _cell_angle_beta 78.007(12) _cell_angle_gamma 77.683(13) _cell_volume 1684.4(6) _cell_formula_units_Z 1 _cell_measurement_temperature 122(1) _cell_measurement_reflns_used 25052 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.07 _exptl_crystal_description Plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.196 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.034 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.923 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 954 _exptl_absorpt_coefficient_mu 2.193 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.629 _exptl_absorpt_correction_T_max 0.932 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 122(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\w and \f scans' _diffrn_reflns_number 63568 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 28.07 _reflns_number_total 8156 _reflns_number_gt 6691 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'COLLECT (Nonius, 1999)' _computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Ortep-3 (Farrugia, 1997) and Mercury (Macrae et. al., 2006) ; _computing_publication_material SHELXL-97 _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^)+(0.0184P)^2^+3.9479P] 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 8156 _refine_ls_number_parameters 508 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Y1 Y 0.20771(2) 0.20360(2) 0.87503(2) 0.01516(7) Uani 1 1 d . . . Cr1 Cr -0.07477(4) 0.08428(4) 0.91566(4) 0.01387(10) Uani 1 1 d . . . F1 F 0.03280(14) 0.19377(14) 0.85530(14) 0.0171(3) Uani 1 1 d . . . F2 F -0.18157(14) -0.02669(14) 0.97626(14) 0.0175(3) Uani 1 1 d . . . O O -0.04739(17) 0.04758(17) 1.07586(17) 0.0151(4) Uani 1 1 d D . . H H -0.105(2) 0.028(3) 1.125(2) 0.018 Uiso 1 1 d D . . N1 N -0.2048(2) 0.2209(2) 0.9170(2) 0.0177(5) Uani 1 1 d . . . N2 N -0.0884(2) 0.1133(2) 0.7436(2) 0.0167(5) Uani 1 1 d . . . O11 O 0.08754(17) 0.28418(18) 1.00260(18) 0.0198(4) Uani 1 1 d . . . O12 O 0.31687(18) 0.18183(19) 1.02031(18) 0.0216(4) Uani 1 1 d . . . O13 O 0.26096(18) 0.39083(19) 0.81933(19) 0.0234(5) Uani 1 1 d . . . O14 O 0.18621(18) 0.31335(19) 0.67426(18) 0.0233(5) Uani 1 1 d . . . O15 O 0.39661(18) 0.19047(19) 0.78797(18) 0.0217(4) Uani 1 1 d . . . O16 O 0.23810(17) 0.06399(18) 0.78588(18) 0.0207(4) Uani 1 1 d . . . F11 F -0.08087(17) 0.42350(18) 1.07392(18) 0.0342(5) Uani 1 1 d . . . F12 F -0.0606(2) 0.2663(3) 1.2290(2) 0.0780(10) Uani 1 1 d . . . F13 F 0.0118(2) 0.4193(3) 1.2028(3) 0.0722(9) Uani 1 1 d . . . F14 F 0.48662(18) 0.1206(2) 1.13993(19) 0.0395(5) Uani 1 1 d . . . F15 F 0.3678(2) 0.1278(2) 1.28983(19) 0.0523(7) Uani 1 1 d . . . F16 F 0.4331(2) 0.2861(2) 1.1600(2) 0.0520(6) Uani 1 1 d . . . F21 F 0.2953(2) 0.66716(18) 0.6840(2) 0.0468(6) Uani 1 1 d . . . F22 F 0.45811(18) 0.5649(2) 0.6664(2) 0.0478(6) Uani 1 1 d . . . F23 F 0.3666(2) 0.5384(2) 0.8383(2) 0.0505(6) Uani 1 1 d . . . F24 F 0.1053(3) 0.4526(4) 0.4560(2) 0.0848(11) Uani 1 1 d . . . F25 F 0.2615(3) 0.5109(3) 0.3856(2) 0.0848(11) Uani 1 1 d . . . F26 F 0.2474(4) 0.3294(3) 0.4447(2) 0.1056(15) Uani 1 1 d . . . F31 F 0.56789(19) 0.3083(2) 0.6476(2) 0.0483(6) Uani 1 1 d . . . F32 F 0.60254(19) 0.1996(2) 0.54679(19) 0.0472(6) Uani 1 1 d . . . F33 F 0.63580(18) 0.1244(2) 0.7275(2) 0.0475(6) Uani 1 1 d . . . F34 F 0.2484(6) -0.1165(4) 0.7205(4) 0.162(3) Uani 1 1 d . . . F35 F 0.3400(3) -0.0311(4) 0.5569(3) 0.1013(14) Uani 1 1 d . . . F36 F 0.1738(3) 0.0279(6) 0.6060(6) 0.163(3) Uani 1 1 d . . . C24 C 0.2985(3) 0.2157(3) 1.1037(3) 0.0214(6) Uani 1 1 d . . . C34 C 0.3049(3) 0.0578(3) 0.6972(3) 0.0223(6) Uani 1 1 d . . . C22 C 0.1010(3) 0.3034(3) 1.0889(3) 0.0200(6) Uani 1 1 d . . . C20 C -0.1074(3) 0.0232(3) 0.7220(3) 0.0218(6) Uani 1 1 d . . . H20 H -0.1145 -0.0513 0.7861 0.026 Uiso 1 1 calc R . . C27 C 0.2968(3) 0.4658(3) 0.7219(3) 0.0237(7) Uani 1 1 d . . . C32 C 0.4437(3) 0.1665(3) 0.7003(3) 0.0209(6) Uani 1 1 d . . . C33 C 0.4037(3) 0.1087(3) 0.6463(3) 0.0234(7) Uani 1 1 d . . . H33 H 0.4438 0.1038 0.5746 0.028 Uiso 1 1 calc R . . C11 C -0.3111(3) 0.2176(3) 0.9054(3) 0.0237(6) Uani 1 1 d . . . H11 H -0.3273 0.1490 0.9006 0.028 Uiso 1 1 calc R . . C23 C 0.1984(3) 0.2761(3) 1.1423(3) 0.0241(7) Uani 1 1 d . . . H23 H 0.1969 0.2989 1.2059 0.029 Uiso 1 1 calc R . . C29 C 0.2301(3) 0.3995(3) 0.5949(3) 0.0244(7) Uani 1 1 d . . . C16 C -0.0762(3) 0.2176(3) 0.6522(3) 0.0267(7) Uani 1 1 d . . . H16 H -0.0609 0.2813 0.6665 0.032 Uiso 1 1 calc R . . C18 C -0.1069(3) 0.1427(3) 0.5165(3) 0.0299(7) Uani 1 1 d . . . H18 H -0.1147 0.1534 0.4387 0.036 Uiso 1 1 calc R . . C15 C -0.1842(3) 0.3166(3) 0.9279(3) 0.0242(7) Uani 1 1 d . . . H15 H -0.1098 0.3191 0.9382 0.029 Uiso 1 1 calc R . . C26 C 0.3546(3) 0.5604(3) 0.7278(3) 0.0318(8) Uani 1 1 d . . . C12 C -0.3979(3) 0.3103(3) 0.9003(3) 0.0296(7) Uani 1 1 d . . . H12 H -0.4718 0.3062 0.8903 0.035 Uiso 1 1 calc R . . C17 C -0.0852(3) 0.2350(3) 0.5382(3) 0.0331(8) Uani 1 1 d . . . H17 H -0.0765 0.3098 0.4752 0.040 Uiso 1 1 calc R . . C25 C 0.3978(3) 0.1868(3) 1.1739(3) 0.0300(7) Uani 1 1 d . . . C13 C -0.3750(3) 0.4084(3) 0.9101(3) 0.0308(8) Uani 1 1 d . . . H13 H -0.4332 0.4734 0.9067 0.037 Uiso 1 1 calc R . . C30 C 0.2135(3) 0.4214(3) 0.4684(3) 0.0352(8) Uani 1 1 d . . . C21 C -0.0078(3) 0.3554(3) 1.1482(3) 0.0320(8) Uani 1 1 d . . . C19 C -0.1171(3) 0.0348(3) 0.6096(3) 0.0259(7) Uani 1 1 d . . . H19 H -0.1307 -0.0306 0.5968 0.031 Uiso 1 1 calc R . . C14 C -0.2672(3) 0.4117(3) 0.9248(3) 0.0305(8) Uani 1 1 d . . . H14 H -0.2502 0.4784 0.9327 0.037 Uiso 1 1 calc R . . C31 C 0.5634(3) 0.2009(3) 0.6538(3) 0.0305(8) Uani 1 1 d . . . C28 C 0.2883(3) 0.4755(3) 0.6087(3) 0.0297(7) Uani 1 1 d . . . H28 H 0.3226 0.5345 0.5409 0.036 Uiso 1 1 calc R . . C35 C 0.2721(4) -0.0173(4) 0.6428(4) 0.0478(11) 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 Y1 0.01670(14) 0.01568(14) 0.01376(13) -0.00657(10) 0.00139(10) -0.00530(10) Cr1 0.0158(2) 0.0141(2) 0.0118(2) -0.00478(17) -0.00067(17) -0.00392(17) F1 0.0181(8) 0.0175(8) 0.0157(8) -0.0059(7) 0.0004(6) -0.0063(7) F2 0.0193(8) 0.0181(8) 0.0148(8) -0.0054(7) -0.0002(6) -0.0062(7) O 0.0163(10) 0.0165(10) 0.0130(9) -0.0063(8) 0.0001(7) -0.0041(8) N1 0.0196(12) 0.0174(12) 0.0147(11) -0.0055(10) -0.0012(9) -0.0030(10) N2 0.0160(12) 0.0179(12) 0.0152(11) -0.0056(10) -0.0023(9) -0.0021(9) O11 0.0219(11) 0.0219(11) 0.0185(10) -0.0111(9) 0.0007(8) -0.0056(9) O12 0.0230(11) 0.0228(11) 0.0216(11) -0.0101(9) -0.0021(9) -0.0061(9) O13 0.0274(12) 0.0201(11) 0.0214(11) -0.0080(9) 0.0029(9) -0.0071(9) O14 0.0239(11) 0.0243(11) 0.0182(10) -0.0045(9) 0.0004(9) -0.0076(9) O15 0.0212(11) 0.0257(11) 0.0218(11) -0.0137(9) 0.0015(9) -0.0053(9) O16 0.0219(11) 0.0226(11) 0.0207(10) -0.0127(9) 0.0041(8) -0.0074(9) F11 0.0282(11) 0.0394(12) 0.0380(11) -0.0228(10) -0.0044(9) 0.0052(9) F12 0.0599(17) 0.0603(17) 0.0553(17) 0.0054(14) 0.0391(14) 0.0062(14) F13 0.0601(17) 0.109(2) 0.086(2) -0.087(2) -0.0311(15) 0.0338(16) F14 0.0319(11) 0.0457(13) 0.0410(12) -0.0164(10) -0.0148(9) 0.0029(10) F15 0.0472(14) 0.0784(18) 0.0228(11) -0.0095(11) -0.0123(10) -0.0063(13) F16 0.0500(15) 0.0484(14) 0.0759(18) -0.0305(13) -0.0268(13) -0.0134(11) F21 0.0457(13) 0.0218(11) 0.0709(16) -0.0178(11) -0.0045(12) -0.0045(9) F22 0.0287(11) 0.0480(14) 0.0724(17) -0.0316(13) 0.0123(11) -0.0183(10) F23 0.0681(17) 0.0516(15) 0.0432(13) -0.0187(12) -0.0055(12) -0.0338(13) F24 0.0548(18) 0.148(3) 0.0417(15) -0.0206(18) -0.0196(13) -0.0154(19) F25 0.133(3) 0.098(2) 0.0202(12) 0.0039(13) -0.0034(15) -0.073(2) F26 0.217(4) 0.0581(19) 0.0396(16) -0.0286(15) -0.050(2) 0.038(2) F31 0.0407(13) 0.0519(14) 0.0616(15) -0.0325(13) 0.0199(11) -0.0296(11) F32 0.0352(12) 0.0787(17) 0.0380(12) -0.0352(12) 0.0201(10) -0.0273(12) F33 0.0225(11) 0.0702(17) 0.0560(15) -0.0321(13) -0.0079(10) -0.0013(11) F34 0.315(7) 0.119(3) 0.106(3) -0.084(3) 0.073(4) -0.154(5) F35 0.088(2) 0.174(4) 0.115(3) -0.132(3) 0.063(2) -0.083(2) F36 0.066(2) 0.294(7) 0.275(7) -0.257(7) -0.042(3) 0.004(3) C24 0.0299(17) 0.0170(14) 0.0177(14) -0.0040(12) -0.0031(12) -0.0096(12) C34 0.0235(16) 0.0250(16) 0.0208(15) -0.0125(13) 0.0010(12) -0.0045(13) C22 0.0258(16) 0.0144(14) 0.0185(14) -0.0066(12) 0.0024(12) -0.0051(12) C20 0.0222(15) 0.0223(15) 0.0214(15) -0.0090(13) -0.0013(12) -0.0051(12) C27 0.0193(15) 0.0168(14) 0.0308(17) -0.0074(13) 0.0019(13) -0.0030(12) C32 0.0182(15) 0.0215(15) 0.0210(15) -0.0079(12) -0.0001(12) -0.0022(12) C33 0.0225(16) 0.0291(17) 0.0206(15) -0.0136(13) 0.0023(12) -0.0043(13) C11 0.0228(16) 0.0244(16) 0.0242(16) -0.0099(13) -0.0027(12) -0.0037(13) C23 0.0338(18) 0.0235(16) 0.0189(15) -0.0121(13) -0.0030(13) -0.0046(13) C29 0.0237(16) 0.0244(16) 0.0192(15) -0.0045(13) -0.0008(12) -0.0015(13) C16 0.040(2) 0.0211(16) 0.0185(15) -0.0062(13) -0.0037(14) -0.0072(14) C18 0.0326(18) 0.041(2) 0.0170(15) -0.0121(14) -0.0048(13) -0.0035(15) C15 0.0237(16) 0.0256(16) 0.0263(16) -0.0134(13) -0.0014(13) -0.0048(13) C26 0.0308(19) 0.0254(17) 0.0355(19) -0.0093(15) 0.0022(15) -0.0081(14) C12 0.0209(16) 0.0344(19) 0.0339(18) -0.0149(15) -0.0048(14) -0.0006(14) C17 0.047(2) 0.0295(18) 0.0179(15) -0.0031(14) -0.0062(15) -0.0067(16) C25 0.0316(18) 0.0343(19) 0.0274(17) -0.0120(15) -0.0068(14) -0.0087(15) C13 0.0286(18) 0.0256(17) 0.0366(19) -0.0155(15) -0.0030(15) 0.0050(14) C30 0.041(2) 0.037(2) 0.0205(17) -0.0026(15) -0.0031(15) -0.0108(17) C21 0.0349(19) 0.037(2) 0.0243(17) -0.0171(15) 0.0023(14) -0.0015(15) C19 0.0256(17) 0.0318(18) 0.0271(16) -0.0183(14) -0.0023(13) -0.0049(13) C14 0.0332(19) 0.0228(17) 0.040(2) -0.0171(15) -0.0045(15) -0.0026(14) C31 0.0237(17) 0.040(2) 0.0331(18) -0.0213(16) 0.0069(14) -0.0106(15) C28 0.0325(18) 0.0265(17) 0.0221(16) -0.0001(13) 0.0023(14) -0.0134(14) C35 0.041(2) 0.069(3) 0.059(3) -0.051(2) 0.020(2) -0.029(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 Y1 F1 2.2299(17) . ? Y1 F2 2.2558(16) 2_557 ? Y1 O15 2.337(2) . ? Y1 O11 2.340(2) . ? Y1 O13 2.346(2) . ? Y1 O14 2.351(2) . ? Y1 O12 2.367(2) . ? Y1 O16 2.375(2) . ? Cr1 F1 1.9123(17) . ? Cr1 F2 1.9183(17) . ? Cr1 O 1.950(2) . ? Cr1 O 1.956(2) 2_557 ? Cr1 N2 2.071(2) . ? Cr1 N1 2.072(3) . ? Cr1 Cr1 2.9117(10) 2_557 ? F2 Y1 2.2558(16) 2_557 ? O Cr1 1.956(2) 2_557 ? O H 0.836(18) . ? N1 C15 1.343(4) . ? N1 C11 1.344(4) . ? N2 C20 1.341(4) . ? N2 C16 1.342(4) . ? O11 C22 1.252(4) . ? O12 C24 1.249(4) . ? O13 C27 1.249(4) . ? O14 C29 1.252(4) . ? O15 C32 1.253(4) . ? O16 C34 1.256(4) . ? F11 C21 1.321(4) . ? F12 C21 1.332(4) . ? F13 C21 1.332(4) . ? F14 C25 1.327(4) . ? F15 C25 1.338(4) . ? F16 C25 1.334(4) . ? F21 C26 1.323(4) . ? F22 C26 1.333(4) . ? F23 C26 1.329(4) . ? F24 C30 1.315(5) . ? F25 C30 1.316(4) . ? F26 C30 1.273(5) . ? F31 C31 1.327(4) . ? F32 C31 1.334(4) . ? F33 C31 1.338(4) . ? F34 C35 1.265(6) . ? F35 C35 1.265(4) . ? F36 C35 1.300(6) . ? C24 C23 1.401(5) . ? C24 C25 1.536(5) . ? C34 C33 1.388(4) . ? C34 C35 1.524(5) . ? C22 C23 1.392(5) . ? C22 C21 1.537(4) . ? C20 C19 1.383(4) . ? C20 H20 0.9500 . ? C27 C28 1.399(5) . ? C27 C26 1.535(5) . ? C32 C33 1.386(4) . ? C32 C31 1.536(4) . ? C33 H33 0.9500 . ? C11 C12 1.383(5) . ? C11 H11 0.9500 . ? C23 H23 0.9500 . ? C29 C28 1.384(5) . ? C29 C30 1.544(5) . ? C16 C17 1.378(5) . ? C16 H16 0.9500 . ? C18 C19 1.377(5) . ? C18 C17 1.381(5) . ? C18 H18 0.9500 . ? C15 C14 1.381(5) . ? C15 H15 0.9500 . ? C12 C13 1.375(5) . ? C12 H12 0.9500 . ? C17 H17 0.9500 . ? C13 C14 1.375(5) . ? C13 H13 0.9500 . ? C19 H19 0.9500 . ? C14 H14 0.9500 . ? C28 H28 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Y1 F2 80.52(6) . 2_557 ? F1 Y1 O15 142.95(7) . . ? F2 Y1 O15 108.06(7) 2_557 . ? F1 Y1 O11 74.93(7) . . ? F2 Y1 O11 84.90(7) 2_557 . ? O15 Y1 O11 140.37(7) . . ? F1 Y1 O13 118.71(7) . . ? F2 Y1 O13 146.23(7) 2_557 . ? O15 Y1 O13 74.19(8) . . ? O11 Y1 O13 75.08(7) . . ? F1 Y1 O14 73.25(7) . . ? F2 Y1 O14 141.65(7) 2_557 . ? O15 Y1 O14 79.43(8) . . ? O11 Y1 O14 113.71(8) . . ? O13 Y1 O14 72.06(8) . . ? F1 Y1 O12 141.02(7) . . ? F2 Y1 O12 74.09(7) 2_557 . ? O15 Y1 O12 74.26(7) . . ? O11 Y1 O12 73.81(7) . . ? O13 Y1 O12 74.34(8) . . ? O14 Y1 O12 141.74(7) . . ? F1 Y1 O16 76.86(7) . . ? F2 Y1 O16 73.69(7) 2_557 . ? O15 Y1 O16 71.63(7) . . ? O11 Y1 O16 146.92(7) . . ? O13 Y1 O16 134.88(7) . . ? O14 Y1 O16 73.45(8) . . ? O12 Y1 O16 121.83(7) . . ? F1 Cr1 F2 179.49(7) . . ? F1 Cr1 O 89.27(8) . . ? F2 Cr1 O 90.67(8) . . ? F1 Cr1 O 90.68(8) . 2_557 ? F2 Cr1 O 88.81(8) . 2_557 ? O Cr1 O 83.61(9) . 2_557 ? F1 Cr1 N2 89.24(8) . . ? F2 Cr1 N2 90.77(8) . . ? O Cr1 N2 174.32(9) . . ? O Cr1 N2 90.93(9) 2_557 . ? F1 Cr1 N1 90.06(9) . . ? F2 Cr1 N1 90.45(9) . . ? O Cr1 N1 93.23(9) . . ? O Cr1 N1 176.74(9) 2_557 . ? N2 Cr1 N1 92.25(10) . . ? F1 Cr1 Cr1 89.97(6) . 2_557 ? F2 Cr1 Cr1 89.65(5) . 2_557 ? O Cr1 Cr1 41.87(6) . 2_557 ? O Cr1 Cr1 41.73(6) 2_557 2_557 ? N2 Cr1 Cr1 132.65(7) . 2_557 ? N1 Cr1 Cr1 135.10(7) . 2_557 ? Cr1 F1 Y1 139.99(9) . . ? Cr1 F2 Y1 139.26(9) . 2_557 ? Cr1 O Cr1 96.39(9) . 2_557 ? Cr1 O H 112(2) . . ? Cr1 O H 114(2) 2_557 . ? C15 N1 C11 118.0(3) . . ? C15 N1 Cr1 120.4(2) . . ? C11 N1 Cr1 121.6(2) . . ? C20 N2 C16 118.5(3) . . ? C20 N2 Cr1 118.6(2) . . ? C16 N2 Cr1 122.9(2) . . ? C22 O11 Y1 134.2(2) . . ? C24 O12 Y1 133.5(2) . . ? C27 O13 Y1 132.7(2) . . ? C29 O14 Y1 133.1(2) . . ? C32 O15 Y1 132.0(2) . . ? C34 O16 Y1 130.81(19) . . ? O12 C24 C23 128.3(3) . . ? O12 C24 C25 116.1(3) . . ? C23 C24 C25 115.6(3) . . ? O16 C34 C33 127.8(3) . . ? O16 C34 C35 114.3(3) . . ? C33 C34 C35 117.8(3) . . ? O11 C22 C23 128.7(3) . . ? O11 C22 C21 114.5(3) . . ? C23 C22 C21 116.6(3) . . ? N2 C20 C19 122.3(3) . . ? N2 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? O13 C27 C28 127.9(3) . . ? O13 C27 C26 115.7(3) . . ? C28 C27 C26 116.3(3) . . ? O15 C32 C33 128.3(3) . . ? O15 C32 C31 113.9(3) . . ? C33 C32 C31 117.7(3) . . ? C32 C33 C34 119.9(3) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? N1 C11 C12 122.5(3) . . ? N1 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C22 C23 C24 121.1(3) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? O14 C29 C28 127.7(3) . . ? O14 C29 C30 114.0(3) . . ? C28 C29 C30 118.2(3) . . ? N2 C16 C17 122.0(3) . . ? N2 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C19 C18 C17 118.8(3) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? N1 C15 C14 122.4(3) . . ? N1 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? F21 C26 F23 107.8(3) . . ? F21 C26 F22 107.6(3) . . ? F23 C26 F22 106.7(3) . . ? F21 C26 C27 111.1(3) . . ? F23 C26 C27 111.9(3) . . ? F22 C26 C27 111.5(3) . . ? C13 C12 C11 118.7(3) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C16 C17 C18 119.4(3) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? F14 C25 F16 107.1(3) . . ? F14 C25 F15 107.1(3) . . ? F16 C25 F15 107.6(3) . . ? F14 C25 C24 112.7(3) . . ? F16 C25 C24 110.7(3) . . ? F15 C25 C24 111.4(3) . . ? C14 C13 C12 119.4(3) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? F26 C30 F24 107.3(4) . . ? F26 C30 F25 109.2(4) . . ? F24 C30 F25 103.9(3) . . ? F26 C30 C29 112.6(3) . . ? F24 C30 C29 109.8(3) . . ? F25 C30 C29 113.6(3) . . ? F11 C21 F13 107.1(3) . . ? F11 C21 F12 106.3(3) . . ? F13 C21 F12 107.7(3) . . ? F11 C21 C22 113.4(3) . . ? F13 C21 C22 113.2(3) . . ? F12 C21 C22 108.7(3) . . ? C18 C19 C20 119.0(3) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C13 C14 C15 119.0(3) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? F31 C31 F32 107.6(3) . . ? F31 C31 F33 107.2(3) . . ? F32 C31 F33 107.2(3) . . ? F31 C31 C32 111.8(3) . . ? F32 C31 C32 113.2(3) . . ? F33 C31 C32 109.6(3) . . ? C29 C28 C27 120.3(3) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? F35 C35 F34 110.5(4) . . ? F35 C35 F36 107.0(5) . . ? F34 C35 F36 99.4(5) . . ? F35 C35 C34 116.6(3) . . ? F34 C35 C34 111.7(4) . . ? F36 C35 C34 110.1(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O H O16 0.836(18) 2.04(2) 2.836(3) 158(3) 2_557 _diffrn_measured_fraction_theta_max .995 _diffrn_reflns_theta_full 28.07 _diffrn_measured_fraction_theta_full .995 _refine_diff_density_max 1.236 _refine_diff_density_min -.905 _refine_diff_density_rms .089 data_kcd828_A2Gd_1Ln _database_code_depnum_ccdc_archive 'CCDC 878249' #TrackingRef 'Ln2Cr2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H28 Cr2 F40 Gd2 N4 O14' _chemical_formula_sum 'C50 H28 Cr2 F40 Gd2 N4 O14' _chemical_formula_weight 2087.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.158(3) _cell_length_b 12.5405(14) _cell_length_c 12.5573(10) _cell_angle_alpha 65.482(10) _cell_angle_beta 78.496(14) _cell_angle_gamma 77.792(12) _cell_volume 1689.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 122(1) _cell_measurement_reflns_used 38806 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 40.00 _exptl_crystal_description Prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.175 _exptl_crystal_size_mid 0.089 _exptl_crystal_size_min 0.072 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.052 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 2.424 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.668 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 122(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\w and \f scans' _diffrn_reflns_number 90679 _diffrn_reflns_av_R_equivalents 0.0935 _diffrn_reflns_av_sigmaI/netI 0.0799 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _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 2.29 _diffrn_reflns_theta_max 40.00 _reflns_number_total 20879 _reflns_number_gt 16431 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'COLLECT (Nonius, 1999)' _computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Ortep-3 (Farrugia, 1997) and Mercury (Macrae et. al., 2006) ; _computing_publication_material SHELXL-97 _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^)+(0.0000P)^2^+0.8938P] 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 20879 _refine_ls_number_parameters 508 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 Gd1 Gd 0.208508(8) 0.205531(8) 0.876120(7) 0.01604(3) Uani 1 1 d . . . Cr1 Cr -0.07558(3) 0.08433(3) 0.91575(2) 0.01524(5) Uani 1 1 d . . . F1 F 0.03010(11) 0.19473(10) 0.85649(10) 0.0190(2) Uani 1 1 d . . . F2 F -0.18199(11) -0.02570(10) 0.97374(10) 0.0190(2) Uani 1 1 d . . . O O -0.04724(13) 0.04705(12) 1.07565(12) 0.0174(2) Uani 1 1 d D . . H H -0.1094(18) 0.032(3) 1.115(2) 0.021 Uiso 1 1 d D . . N1 N -0.20633(15) 0.21971(15) 0.91822(15) 0.0192(3) Uani 1 1 d . . . N2 N -0.08958(15) 0.11281(15) 0.74429(14) 0.0185(3) Uani 1 1 d . . . O11 O 0.08768(14) 0.28717(14) 1.00625(13) 0.0218(3) Uani 1 1 d . . . O12 O 0.31847(14) 0.18532(14) 1.02416(14) 0.0228(3) Uani 1 1 d . . . O13 O 0.26325(15) 0.39532(14) 0.81744(15) 0.0254(3) Uani 1 1 d . . . O14 O 0.18635(15) 0.31625(14) 0.67294(13) 0.0242(3) Uani 1 1 d . . . O15 O 0.39951(14) 0.18978(15) 0.78812(14) 0.0232(3) Uani 1 1 d . . . O16 O 0.23839(14) 0.06354(14) 0.78596(13) 0.0220(3) Uani 1 1 d . . . F11 F -0.08098(14) 0.42367(15) 1.07797(15) 0.0363(3) Uani 1 1 d . . . F12 F -0.0569(2) 0.2709(2) 1.2344(2) 0.0893(11) Uani 1 1 d . . . F13 F 0.0148(2) 0.4267(3) 1.2009(3) 0.0785(9) Uani 1 1 d . . . F14 F 0.48796(16) 0.12403(17) 1.14461(16) 0.0413(4) Uani 1 1 d . . . F15 F 0.36989(19) 0.1321(2) 1.29333(15) 0.0542(5) Uani 1 1 d . . . F16 F 0.43468(19) 0.28959(19) 1.1640(2) 0.0556(6) Uani 1 1 d . . . F21 F 0.29710(17) 0.67072(14) 0.6801(2) 0.0469(5) Uani 1 1 d . . . F22 F 0.45946(16) 0.56814(18) 0.6637(2) 0.0506(5) Uani 1 1 d . . . F23 F 0.3696(2) 0.54391(18) 0.83492(18) 0.0519(5) Uani 1 1 d . . . F24 F 0.1048(2) 0.4542(3) 0.4550(2) 0.0875(10) Uani 1 1 d . . . F25 F 0.2609(3) 0.5115(3) 0.38559(17) 0.0820(10) Uani 1 1 d . . . F26 F 0.2471(4) 0.3299(2) 0.4452(2) 0.1075(14) Uani 1 1 d . . . F31 F 0.57090(17) 0.30528(18) 0.64779(19) 0.0502(5) Uani 1 1 d . . . F32 F 0.60229(16) 0.1960(2) 0.54775(16) 0.0481(5) Uani 1 1 d . . . F33 F 0.63781(15) 0.1213(2) 0.72681(19) 0.0484(5) Uani 1 1 d . . . F34 F 0.2374(5) -0.1101(4) 0.7172(3) 0.154(2) Uani 1 1 d . . . F35 F 0.3377(3) -0.0323(4) 0.5584(3) 0.1037(14) Uani 1 1 d . . . F36 F 0.1721(3) 0.0379(5) 0.5983(5) 0.158(2) Uani 1 1 d . . . C24 C 0.2997(2) 0.21845(18) 1.10766(18) 0.0220(3) Uani 1 1 d . . . C34 C 0.30364(19) 0.0584(2) 0.69685(19) 0.0232(4) Uani 1 1 d . . . C22 C 0.1018(2) 0.30614(18) 1.09273(18) 0.0220(4) Uani 1 1 d . . . C20 C -0.10741(19) 0.02229(19) 0.72215(18) 0.0226(4) Uani 1 1 d . . . H20 H -0.1141 -0.0520 0.7859 0.027 Uiso 1 1 calc R . . C27 C 0.2983(2) 0.46934(18) 0.7198(2) 0.0246(4) Uani 1 1 d . . . C32 C 0.44508(18) 0.16553(19) 0.70053(18) 0.0217(3) Uani 1 1 d . . . C33 C 0.40270(19) 0.1086(2) 0.64623(19) 0.0236(4) Uani 1 1 d . . . H33 H 0.4416 0.1040 0.5744 0.028 Uiso 1 1 calc R . . C11 C -0.31225(19) 0.2166(2) 0.9055(2) 0.0247(4) Uani 1 1 d . . . H11 H -0.3280 0.1486 0.8990 0.030 Uiso 1 1 calc R . . C23 C 0.1997(2) 0.2778(2) 1.14651(19) 0.0263(4) Uani 1 1 d . . . H23 H 0.1984 0.2994 1.2110 0.032 Uiso 1 1 calc R . . C29 C 0.2299(2) 0.4019(2) 0.59358(19) 0.0257(4) Uani 1 1 d . . . C16 C -0.0779(2) 0.2168(2) 0.65382(19) 0.0270(4) Uani 1 1 d . . . H16 H -0.0627 0.2804 0.6686 0.032 Uiso 1 1 calc R . . C18 C -0.1076(2) 0.1409(2) 0.51759(19) 0.0302(5) Uani 1 1 d . . . H18 H -0.1153 0.1511 0.4400 0.036 Uiso 1 1 calc R . . C15 C -0.1848(2) 0.3152(2) 0.9302(2) 0.0254(4) Uani 1 1 d . . . H15 H -0.1102 0.3175 0.9408 0.031 Uiso 1 1 calc R . . C26 C 0.3569(2) 0.5642(2) 0.7254(3) 0.0320(5) Uani 1 1 d . . . C12 C -0.3998(2) 0.3087(2) 0.9015(2) 0.0307(5) Uani 1 1 d . . . H12 H -0.4738 0.3044 0.8912 0.037 Uiso 1 1 calc R . . C17 C -0.0873(3) 0.2342(2) 0.5393(2) 0.0335(5) Uani 1 1 d . . . H17 H -0.0799 0.3091 0.4766 0.040 Uiso 1 1 calc R . . C25 C 0.3995(2) 0.1902(2) 1.1783(2) 0.0313(5) Uani 1 1 d . . . C13 C -0.3773(2) 0.4067(2) 0.9127(3) 0.0330(5) Uani 1 1 d . . . H13 H -0.4357 0.4710 0.9102 0.040 Uiso 1 1 calc R . . C30 C 0.2135(3) 0.4227(3) 0.4681(2) 0.0347(5) Uani 1 1 d . . . C21 C -0.0059(2) 0.3586(2) 1.1517(2) 0.0333(5) Uani 1 1 d . . . C19 C -0.1164(2) 0.0333(2) 0.6101(2) 0.0274(4) Uani 1 1 d . . . H19 H -0.1285 -0.0325 0.5970 0.033 Uiso 1 1 calc R . . C14 C -0.2685(2) 0.4097(2) 0.9275(3) 0.0323(5) Uani 1 1 d . . . H14 H -0.2514 0.4762 0.9358 0.039 Uiso 1 1 calc R . . C31 C 0.5651(2) 0.1977(3) 0.6540(2) 0.0327(5) Uani 1 1 d . . . C28 C 0.2892(2) 0.4778(2) 0.6077(2) 0.0317(5) Uani 1 1 d . . . H28 H 0.3238 0.5359 0.5401 0.038 Uiso 1 1 calc R . . C35 C 0.2692(3) -0.0145(3) 0.6408(3) 0.0471(8) 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 Gd1 0.01808(4) 0.01698(4) 0.01485(4) -0.00826(3) 0.00136(3) -0.00510(3) Cr1 0.01749(13) 0.01549(11) 0.01389(10) -0.00666(9) -0.00123(9) -0.00345(9) F1 0.0201(5) 0.0185(5) 0.0192(5) -0.0076(4) -0.0006(4) -0.0056(4) F2 0.0216(6) 0.0185(5) 0.0177(5) -0.0067(4) -0.0016(4) -0.0062(4) O 0.0189(6) 0.0193(6) 0.0151(5) -0.0082(4) -0.0007(4) -0.0035(5) N1 0.0191(7) 0.0203(7) 0.0190(6) -0.0090(5) -0.0022(5) -0.0018(6) N2 0.0205(7) 0.0190(6) 0.0165(6) -0.0078(5) -0.0022(5) -0.0023(5) O11 0.0231(7) 0.0251(7) 0.0209(6) -0.0133(5) 0.0011(5) -0.0052(5) O12 0.0245(7) 0.0234(6) 0.0238(6) -0.0118(5) -0.0038(5) -0.0040(5) O13 0.0300(8) 0.0207(6) 0.0262(7) -0.0108(6) 0.0029(6) -0.0076(6) O14 0.0276(8) 0.0238(7) 0.0194(6) -0.0059(5) -0.0004(5) -0.0081(6) O15 0.0207(7) 0.0297(7) 0.0238(6) -0.0164(6) 0.0024(5) -0.0057(6) O16 0.0243(7) 0.0238(6) 0.0217(6) -0.0138(5) 0.0035(5) -0.0070(5) F11 0.0309(8) 0.0413(8) 0.0405(8) -0.0252(7) -0.0031(6) 0.0055(6) F12 0.0690(17) 0.0668(14) 0.0616(15) 0.0103(12) 0.0452(13) 0.0109(12) F13 0.0612(14) 0.121(2) 0.1003(19) -0.1014(19) -0.0326(13) 0.0349(14) F14 0.0342(9) 0.0492(10) 0.0411(9) -0.0176(8) -0.0152(7) 0.0030(7) F15 0.0491(11) 0.0812(15) 0.0241(7) -0.0111(9) -0.0117(7) -0.0054(11) F16 0.0559(13) 0.0482(11) 0.0819(15) -0.0317(11) -0.0301(11) -0.0137(9) F21 0.0461(11) 0.0215(7) 0.0704(13) -0.0168(8) -0.0071(9) -0.0019(7) F22 0.0312(9) 0.0501(10) 0.0777(15) -0.0342(11) 0.0114(9) -0.0184(8) F23 0.0706(14) 0.0503(11) 0.0462(10) -0.0176(9) -0.0106(9) -0.0313(11) F24 0.0569(15) 0.154(3) 0.0413(12) -0.0226(16) -0.0216(11) -0.0125(18) F25 0.130(3) 0.0918(18) 0.0218(8) 0.0023(10) -0.0054(11) -0.0654(19) F26 0.221(4) 0.0593(14) 0.0404(12) -0.0309(11) -0.0480(18) 0.036(2) F31 0.0437(11) 0.0558(11) 0.0629(12) -0.0358(10) 0.0209(9) -0.0306(9) F32 0.0352(9) 0.0826(14) 0.0395(9) -0.0387(10) 0.0184(7) -0.0254(10) F33 0.0224(8) 0.0744(13) 0.0545(11) -0.0332(11) -0.0071(7) -0.0005(8) F34 0.288(6) 0.126(3) 0.105(3) -0.090(3) 0.081(3) -0.154(4) F35 0.086(2) 0.182(3) 0.120(2) -0.138(3) 0.0585(18) -0.078(2) F36 0.071(2) 0.268(6) 0.269(6) -0.239(6) -0.059(3) 0.019(3) C24 0.0276(10) 0.0205(8) 0.0200(7) -0.0077(6) -0.0041(7) -0.0071(7) C34 0.0249(10) 0.0260(9) 0.0228(8) -0.0154(7) 0.0021(7) -0.0047(7) C22 0.0277(10) 0.0203(8) 0.0199(7) -0.0114(6) 0.0020(7) -0.0044(7) C20 0.0265(10) 0.0241(8) 0.0204(8) -0.0117(7) -0.0019(7) -0.0050(7) C27 0.0251(10) 0.0185(8) 0.0285(9) -0.0085(7) 0.0012(7) -0.0051(7) C32 0.0196(9) 0.0248(8) 0.0209(8) -0.0110(7) 0.0017(6) -0.0029(7) C33 0.0218(9) 0.0306(10) 0.0222(8) -0.0167(7) 0.0036(7) -0.0045(7) C11 0.0214(9) 0.0260(9) 0.0299(9) -0.0148(8) -0.0035(7) -0.0016(7) C23 0.0338(11) 0.0278(9) 0.0224(8) -0.0147(8) -0.0040(8) -0.0041(8) C29 0.0258(10) 0.0256(9) 0.0204(8) -0.0054(7) -0.0012(7) -0.0018(8) C16 0.0387(12) 0.0218(9) 0.0195(8) -0.0058(7) -0.0058(8) -0.0047(8) C18 0.0336(12) 0.0406(12) 0.0188(8) -0.0139(8) -0.0066(8) -0.0022(10) C15 0.0255(10) 0.0242(9) 0.0320(10) -0.0172(8) -0.0016(8) -0.0035(7) C26 0.0303(12) 0.0241(9) 0.0413(13) -0.0122(9) 0.0012(10) -0.0094(9) C12 0.0227(10) 0.0323(11) 0.0401(12) -0.0191(10) -0.0045(9) 0.0012(8) C17 0.0506(16) 0.0293(10) 0.0170(8) -0.0039(8) -0.0083(9) -0.0051(10) C25 0.0351(13) 0.0342(11) 0.0290(10) -0.0129(9) -0.0092(9) -0.0078(10) C13 0.0280(11) 0.0296(11) 0.0429(13) -0.0201(10) -0.0037(10) 0.0049(9) C30 0.0390(14) 0.0380(12) 0.0221(9) -0.0054(9) -0.0023(9) -0.0099(11) C21 0.0365(13) 0.0402(13) 0.0243(9) -0.0200(9) 0.0034(9) 0.0005(10) C19 0.0308(11) 0.0357(11) 0.0221(8) -0.0161(8) -0.0036(8) -0.0074(9) C14 0.0310(12) 0.0266(10) 0.0438(13) -0.0201(10) -0.0039(10) -0.0006(9) C31 0.0239(11) 0.0461(14) 0.0350(12) -0.0252(11) 0.0082(9) -0.0110(10) C28 0.0376(13) 0.0274(10) 0.0242(9) -0.0020(8) 0.0002(9) -0.0132(9) C35 0.0481(17) 0.067(2) 0.0522(17) -0.0487(17) 0.0183(14) -0.0300(16) _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 F1 2.2692(13) . ? Gd1 F2 2.2979(12) 2_557 ? Gd1 O15 2.3699(16) . ? Gd1 O13 2.3809(15) . ? Gd1 O11 2.3815(15) . ? Gd1 O14 2.3844(16) . ? Gd1 O12 2.4010(16) . ? Gd1 O16 2.4123(14) . ? Cr1 F1 1.9072(12) . ? Cr1 F2 1.9112(12) . ? Cr1 O 1.9488(14) . ? Cr1 O 1.9576(15) 2_557 ? Cr1 N2 2.0674(16) . ? Cr1 N1 2.0719(18) . ? Cr1 Cr1 2.9190(8) 2_557 ? F2 Gd1 2.2979(12) 2_557 ? O Cr1 1.9575(15) 2_557 ? O H 0.826(17) . ? N1 C11 1.339(3) . ? N1 C15 1.350(3) . ? N2 C16 1.340(3) . ? N2 C20 1.343(3) . ? O11 C22 1.254(2) . ? O12 C24 1.245(3) . ? O13 C27 1.250(3) . ? O14 C29 1.252(3) . ? O15 C32 1.254(2) . ? O16 C34 1.253(2) . ? F11 C21 1.323(3) . ? F12 C21 1.325(3) . ? F13 C21 1.329(3) . ? F14 C25 1.325(3) . ? F15 C25 1.333(3) . ? F16 C25 1.333(3) . ? F21 C26 1.327(3) . ? F22 C26 1.329(3) . ? F23 C26 1.326(3) . ? F24 C30 1.320(4) . ? F25 C30 1.312(3) . ? F26 C30 1.279(4) . ? F31 C31 1.335(3) . ? F32 C31 1.329(3) . ? F33 C31 1.331(4) . ? F34 C35 1.265(5) . ? F35 C35 1.258(3) . ? F36 C35 1.320(6) . ? C24 C23 1.398(3) . ? C24 C25 1.540(3) . ? C34 C33 1.391(3) . ? C34 C35 1.524(3) . ? C22 C23 1.393(3) . ? C22 C21 1.533(3) . ? C20 C19 1.381(3) . ? C20 H20 0.9500 . ? C27 C28 1.392(3) . ? C27 C26 1.541(3) . ? C32 C33 1.393(3) . ? C32 C31 1.532(3) . ? C33 H33 0.9500 . ? C11 C12 1.386(3) . ? C11 H11 0.9500 . ? C23 H23 0.9500 . ? C29 C28 1.392(3) . ? C29 C30 1.534(3) . ? C16 C17 1.387(3) . ? C16 H16 0.9500 . ? C18 C19 1.376(4) . ? C18 C17 1.384(4) . ? C18 H18 0.9500 . ? C15 C14 1.383(3) . ? C15 H15 0.9500 . ? C12 C13 1.380(4) . ? C12 H12 0.9500 . ? C17 H17 0.9500 . ? C13 C14 1.383(4) . ? C13 H13 0.9500 . ? C19 H19 0.9500 . ? C14 H14 0.9500 . ? C28 H28 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Gd1 F2 79.96(5) . 2_557 ? F1 Gd1 O15 142.52(5) . . ? F2 Gd1 O15 107.71(5) 2_557 . ? F1 Gd1 O13 118.90(6) . . ? F2 Gd1 O13 147.25(5) 2_557 . ? O15 Gd1 O13 74.46(6) . . ? F1 Gd1 O11 75.14(5) . . ? F2 Gd1 O11 84.86(5) 2_557 . ? O15 Gd1 O11 140.87(5) . . ? O13 Gd1 O11 75.78(5) . . ? F1 Gd1 O14 73.75(5) . . ? F2 Gd1 O14 141.43(5) 2_557 . ? O15 Gd1 O14 79.16(6) . . ? O13 Gd1 O14 71.28(6) . . ? O11 Gd1 O14 114.16(6) . . ? F1 Gd1 O12 140.34(5) . . ? F2 Gd1 O12 74.55(5) 2_557 . ? O15 Gd1 O12 75.23(6) . . ? O13 Gd1 O12 74.60(6) . . ? O11 Gd1 O12 72.79(6) . . ? O14 Gd1 O12 141.63(5) . . ? F1 Gd1 O16 76.74(5) . . ? F2 Gd1 O16 73.35(5) 2_557 . ? O15 Gd1 O16 70.99(5) . . ? O13 Gd1 O16 134.23(5) . . ? O11 Gd1 O16 146.91(5) . . ? O14 Gd1 O16 73.48(6) . . ? O12 Gd1 O16 122.50(6) . . ? F1 Cr1 F2 179.47(5) . . ? F1 Cr1 O 89.43(6) . . ? F2 Cr1 O 91.08(6) . . ? F1 Cr1 O 91.17(6) . 2_557 ? F2 Cr1 O 89.02(6) . 2_557 ? O Cr1 O 83.29(6) . 2_557 ? F1 Cr1 N2 89.25(6) . . ? F2 Cr1 N2 90.25(6) . . ? O Cr1 N2 173.97(7) . . ? O Cr1 N2 90.85(6) 2_557 . ? F1 Cr1 N1 89.74(6) . . ? F2 Cr1 N1 90.11(6) . . ? O Cr1 N1 93.18(7) . . ? O Cr1 N1 176.35(6) 2_557 . ? N2 Cr1 N1 92.70(7) . . ? F1 Cr1 Cr1 90.41(4) . 2_557 ? F2 Cr1 Cr1 90.06(4) . 2_557 ? O Cr1 Cr1 41.76(4) . 2_557 ? O Cr1 Cr1 41.53(4) 2_557 2_557 ? N2 Cr1 Cr1 132.37(5) . 2_557 ? N1 Cr1 Cr1 134.93(5) . 2_557 ? Cr1 F1 Gd1 139.77(7) . . ? Cr1 F2 Gd1 139.07(7) . 2_557 ? Cr1 O Cr1 96.71(6) . 2_557 ? Cr1 O H 103(2) . . ? Cr1 O H 119(2) 2_557 . ? C11 N1 C15 118.58(19) . . ? C11 N1 Cr1 121.65(14) . . ? C15 N1 Cr1 119.75(15) . . ? C16 N2 C20 118.70(18) . . ? C16 N2 Cr1 122.64(14) . . ? C20 N2 Cr1 118.62(13) . . ? C22 O11 Gd1 134.40(15) . . ? C24 O12 Gd1 133.95(15) . . ? C27 O13 Gd1 132.78(14) . . ? C29 O14 Gd1 133.57(15) . . ? C32 O15 Gd1 131.98(14) . . ? C34 O16 Gd1 130.53(13) . . ? O12 C24 C23 128.6(2) . . ? O12 C24 C25 116.1(2) . . ? C23 C24 C25 115.28(19) . . ? O16 C34 C33 127.90(19) . . ? O16 C34 C35 114.5(2) . . ? C33 C34 C35 117.55(19) . . ? O11 C22 C23 128.5(2) . . ? O11 C22 C21 114.7(2) . . ? C23 C22 C21 116.52(19) . . ? N2 C20 C19 122.4(2) . . ? N2 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? O13 C27 C28 128.3(2) . . ? O13 C27 C26 115.2(2) . . ? C28 C27 C26 116.5(2) . . ? O15 C32 C33 128.2(2) . . ? O15 C32 C31 114.16(19) . . ? C33 C32 C31 117.52(18) . . ? C34 C33 C32 120.24(18) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? N1 C11 C12 122.5(2) . . ? N1 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C22 C23 C24 121.40(19) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? O14 C29 C28 127.4(2) . . ? O14 C29 C30 114.4(2) . . ? C28 C29 C30 118.2(2) . . ? N2 C16 C17 121.8(2) . . ? N2 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C19 C18 C17 119.0(2) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? N1 C15 C14 121.7(2) . . ? N1 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? F23 C26 F21 108.0(2) . . ? F23 C26 F22 107.2(2) . . ? F21 C26 F22 107.3(2) . . ? F23 C26 C27 112.3(2) . . ? F21 C26 C27 110.5(2) . . ? F22 C26 C27 111.2(2) . . ? C13 C12 C11 118.8(2) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C18 C17 C16 119.1(2) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? F14 C25 F16 107.2(2) . . ? F14 C25 F15 107.3(2) . . ? F16 C25 F15 107.8(2) . . ? F14 C25 C24 112.3(2) . . ? F16 C25 C24 110.6(2) . . ? F15 C25 C24 111.3(2) . . ? C12 C13 C14 119.0(2) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? F26 C30 F25 109.5(3) . . ? F26 C30 F24 107.2(3) . . ? F25 C30 F24 103.6(3) . . ? F26 C30 C29 112.5(2) . . ? F25 C30 C29 113.8(2) . . ? F24 C30 C29 109.7(2) . . ? F11 C21 F12 106.2(3) . . ? F11 C21 F13 106.6(2) . . ? F12 C21 F13 108.6(3) . . ? F11 C21 C22 113.18(19) . . ? F12 C21 C22 109.0(2) . . ? F13 C21 C22 113.0(2) . . ? C18 C19 C20 119.0(2) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C15 C14 C13 119.4(2) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? F32 C31 F33 107.3(2) . . ? F32 C31 F31 107.6(2) . . ? F33 C31 F31 107.1(2) . . ? F32 C31 C32 113.2(2) . . ? F33 C31 C32 110.0(2) . . ? F31 C31 C32 111.4(2) . . ? C27 C28 C29 120.6(2) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? F35 C35 F34 111.2(3) . . ? F35 C35 F36 107.0(4) . . ? F34 C35 F36 98.8(4) . . ? F35 C35 C34 116.9(2) . . ? F34 C35 C34 112.0(3) . . ? F36 C35 C34 109.1(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O H O16 0.826(17) 2.058(19) 2.845(2) 159(3) 2_557 _diffrn_measured_fraction_theta_max .998 _diffrn_reflns_theta_full 40.00 _diffrn_measured_fraction_theta_full .998 _refine_diff_density_max 1.517 _refine_diff_density_min -1.587 _refine_diff_density_rms .170 data_kcd776_A2Dy_1Ln _database_code_depnum_ccdc_archive 'CCDC 878250' #TrackingRef 'Ln2Cr2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H28 Cr2 Dy2 F40 N4 O14' _chemical_formula_sum 'C50 H28 Cr2 Dy2 F40 N4 O14' _chemical_formula_weight 2097.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.115(4) _cell_length_b 12.695(3) _cell_length_c 12.939(3) _cell_angle_alpha 95.30(2) _cell_angle_beta 99.06(3) _cell_angle_gamma 101.86(2) _cell_volume 1749.7(7) _cell_formula_units_Z 1 _cell_measurement_temperature 122(1) _cell_measurement_reflns_used 25125 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 27.65 _exptl_crystal_description prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.072 _exptl_crystal_size_min 0.055 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 2.580 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.737 _exptl_absorpt_correction_T_max 0.880 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 122(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\w and \f scans' _diffrn_reflns_number 63297 _diffrn_reflns_av_R_equivalents 0.0967 _diffrn_reflns_av_sigmaI/netI 0.0829 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.65 _reflns_number_total 8083 _reflns_number_gt 6597 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'COLLECT (Nonius, 1999)' _computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Ortep-3 (Farrugia, 1997) and Mercury (Macrae et. al., 2006) ; _computing_publication_material SHELXL-97 _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^)+(0.0000P)^2^+4.6024P] 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 8083 _refine_ls_number_parameters 508 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 Dy1 Dy 0.07602(2) 0.206913(18) 0.228542(18) 0.02205(8) Uani 1 1 d . . . Cr1 Cr 0.00083(6) -0.08383(6) 0.06988(6) 0.01883(16) Uani 1 1 d . . . O O 0.1173(3) 0.0064(3) -0.0016(2) 0.0194(7) Uani 1 1 d D . . H H 0.140(5) -0.030(3) -0.049(3) 0.023 Uiso 1 1 d D . . F1 F 0.0508(2) 0.0266(2) 0.1889(2) 0.0234(6) Uani 1 1 d . . . F2 F -0.0495(2) -0.1916(2) -0.0500(2) 0.0230(6) Uani 1 1 d . . . N1 N -0.1315(4) -0.1661(3) 0.1479(3) 0.0233(9) Uani 1 1 d . . . N2 N 0.1374(4) -0.1632(3) 0.1302(3) 0.0238(9) Uani 1 1 d . . . O12 O -0.1473(3) 0.1410(3) 0.1653(3) 0.0282(8) Uani 1 1 d . . . O14 O -0.0223(3) 0.1630(3) 0.3702(3) 0.0307(8) Uani 1 1 d . . . O17 O -0.0075(3) 0.3558(3) 0.1956(3) 0.0317(8) Uani 1 1 d . . . O19 O 0.1628(3) 0.3468(3) 0.3710(3) 0.0341(9) Uani 1 1 d . . . O22 O 0.2449(3) 0.1555(3) 0.3307(3) 0.0304(8) Uani 1 1 d . . . O24 O 0.2610(3) 0.3026(3) 0.1841(3) 0.0329(8) Uani 1 1 d . . . C1 C -0.2357(5) -0.2359(4) 0.0939(4) 0.0336(13) Uani 1 1 d . . . H1 H -0.2470 -0.2487 0.0191 0.040 Uiso 1 1 calc R . . C2 C -0.3261(5) -0.2891(5) 0.1444(5) 0.0441(15) Uani 1 1 d . . . H2 H -0.3984 -0.3381 0.1047 0.053 Uiso 1 1 calc R . . C3 C -0.3109(5) -0.2705(5) 0.2533(5) 0.0419(15) Uani 1 1 d . . . H3 H -0.3726 -0.3063 0.2892 0.050 Uiso 1 1 calc R . . C4 C -0.2047(5) -0.1992(5) 0.3090(5) 0.0353(13) Uani 1 1 d . . . H4 H -0.1914 -0.1854 0.3838 0.042 Uiso 1 1 calc R . . C5 C -0.1179(5) -0.1482(4) 0.2531(4) 0.0288(11) Uani 1 1 d . . . H5 H -0.0454 -0.0982 0.2912 0.035 Uiso 1 1 calc R . . C6 C 0.2306(5) -0.1133(5) 0.2094(4) 0.0334(12) Uani 1 1 d . . . H6 H 0.2310 -0.0422 0.2399 0.040 Uiso 1 1 calc R . . C7 C 0.3261(5) -0.1615(5) 0.2482(5) 0.0437(15) Uani 1 1 d . . . H7 H 0.3909 -0.1240 0.3043 0.052 Uiso 1 1 calc R . . C8 C 0.3259(6) -0.2626(5) 0.2052(5) 0.0478(16) Uani 1 1 d . . . H8 H 0.3901 -0.2973 0.2320 0.057 Uiso 1 1 calc R . . C9 C 0.2333(7) -0.3151(5) 0.1229(6) 0.0581(19) Uani 1 1 d . . . H9 H 0.2327 -0.3858 0.0912 0.070 Uiso 1 1 calc R . . C10 C 0.1404(6) -0.2621(5) 0.0871(5) 0.0442(15) Uani 1 1 d . . . H10 H 0.0764 -0.2976 0.0295 0.053 Uiso 1 1 calc R . . C11 C -0.3668(5) 0.1019(7) 0.1340(5) 0.0510(18) Uani 1 1 d . . . C12 C -0.2413(5) 0.1279(4) 0.2095(4) 0.0314(12) Uani 1 1 d . . . C13 C -0.2416(5) 0.1334(5) 0.3164(4) 0.0413(14) Uani 1 1 d . . . H13 H -0.3187 0.1267 0.3408 0.050 Uiso 1 1 calc R . . C14 C -0.1311(5) 0.1485(5) 0.3891(4) 0.0346(12) Uani 1 1 d . . . C15 C -0.1390(6) 0.1415(6) 0.5055(5) 0.0479(16) Uani 1 1 d . . . C16 C -0.0849(6) 0.5129(5) 0.1828(5) 0.0438(15) Uani 1 1 d . . . C17 C 0.0019(5) 0.4489(4) 0.2421(4) 0.0318(12) Uani 1 1 d . . . C18 C 0.0761(6) 0.4978(4) 0.3374(4) 0.0387(14) Uani 1 1 d . . . H18 H 0.0758 0.5702 0.3632 0.046 Uiso 1 1 calc R . . C19 C 0.1516(5) 0.4406(5) 0.3955(4) 0.0343(13) Uani 1 1 d . . . C20 C 0.2337(6) 0.4975(5) 0.5011(5) 0.0462(15) Uani 1 1 d . . . C21 C 0.4266(5) 0.1578(5) 0.4524(4) 0.0361(13) Uani 1 1 d . . . C22 C 0.3565(5) 0.2046(4) 0.3623(4) 0.0311(12) Uani 1 1 d . . . C23 C 0.4242(5) 0.2911(4) 0.3227(4) 0.0334(12) Uani 1 1 d . . . H23 H 0.5078 0.3230 0.3562 0.040 Uiso 1 1 calc R . . C24 C 0.3713(5) 0.3320(4) 0.2346(4) 0.0340(12) Uani 1 1 d . . . C25 C 0.4536(6) 0.4234(6) 0.1913(6) 0.0506(17) Uani 1 1 d . . . F4 F -0.3737(5) 0.0221(8) 0.0656(6) 0.183(5) Uani 1 1 d . . . F5 F -0.4631(3) 0.0868(5) 0.1755(3) 0.101(2) Uani 1 1 d . . . F6 F -0.3771(5) 0.1761(9) 0.0769(7) 0.196(5) Uani 1 1 d . . . F7 F -0.0996(4) 0.0563(3) 0.5371(3) 0.0550(10) Uani 1 1 d . . . F8 F -0.2534(4) 0.1345(5) 0.5251(3) 0.0956(19) Uani 1 1 d . . . F9 F -0.0660(4) 0.2297(3) 0.5662(3) 0.0580(10) Uani 1 1 d . . . F10 F -0.2021(4) 0.4666(4) 0.1798(4) 0.0722(13) Uani 1 1 d . . . F11 F -0.0691(4) 0.5137(3) 0.0824(3) 0.0543(10) Uani 1 1 d . . . F12 F -0.0647(5) 0.6153(3) 0.2251(3) 0.0722(13) Uani 1 1 d . . . F13 F 0.2106(5) 0.4392(4) 0.5780(3) 0.0928(17) Uani 1 1 d . . . F14 F 0.2158(5) 0.5926(4) 0.5311(4) 0.0903(17) Uani 1 1 d . . . F15 F 0.3502(4) 0.5080(5) 0.4982(4) 0.115(2) Uani 1 1 d . . . F16 F 0.3559(4) 0.1229(5) 0.5198(3) 0.0778(15) Uani 1 1 d . . . F17 F 0.5273(4) 0.2260(4) 0.5052(4) 0.0939(18) Uani 1 1 d . . . F18 F 0.4645(4) 0.0721(3) 0.4142(3) 0.0551(10) Uani 1 1 d . . . F19 F 0.4034(5) 0.5023(5) 0.1783(9) 0.182(5) Uani 1 1 d . . . F20 F 0.5650(4) 0.4582(4) 0.2453(3) 0.0856(16) Uani 1 1 d . . . F21 F 0.4726(6) 0.3890(5) 0.0968(4) 0.116(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01653(12) 0.02184(13) 0.02260(13) -0.00112(9) -0.00451(8) 0.00038(8) Cr1 0.0154(4) 0.0185(4) 0.0189(4) 0.0033(3) -0.0024(3) -0.0006(3) O 0.0160(15) 0.0202(17) 0.0190(16) 0.0019(13) -0.0029(13) 0.0020(13) F1 0.0211(14) 0.0235(14) 0.0219(14) 0.0034(11) -0.0025(11) 0.0014(11) F2 0.0200(13) 0.0210(14) 0.0246(14) 0.0018(11) -0.0005(11) 0.0007(11) N1 0.020(2) 0.023(2) 0.024(2) 0.0053(17) -0.0004(16) 0.0008(16) N2 0.020(2) 0.026(2) 0.023(2) 0.0089(17) -0.0020(16) 0.0028(17) O12 0.0172(17) 0.036(2) 0.0256(18) -0.0014(15) -0.0035(14) 0.0006(14) O14 0.0190(18) 0.043(2) 0.0270(19) 0.0009(16) -0.0019(14) 0.0059(15) O17 0.032(2) 0.0279(19) 0.031(2) -0.0027(16) -0.0036(16) 0.0071(15) O19 0.029(2) 0.028(2) 0.036(2) -0.0069(16) -0.0087(16) 0.0021(15) O22 0.0214(18) 0.0302(19) 0.034(2) 0.0040(16) -0.0061(15) 0.0013(15) O24 0.0224(18) 0.033(2) 0.035(2) 0.0036(16) -0.0050(15) -0.0048(15) C1 0.028(3) 0.042(3) 0.025(3) 0.008(2) 0.001(2) -0.005(2) C2 0.031(3) 0.048(4) 0.041(3) 0.008(3) 0.000(3) -0.015(3) C3 0.034(3) 0.050(4) 0.038(3) 0.014(3) 0.012(3) -0.004(3) C4 0.032(3) 0.042(3) 0.033(3) 0.009(3) 0.008(2) 0.005(2) C5 0.023(3) 0.033(3) 0.028(3) 0.007(2) -0.001(2) 0.002(2) C6 0.029(3) 0.038(3) 0.031(3) 0.002(2) -0.006(2) 0.010(2) C7 0.035(3) 0.051(4) 0.039(3) -0.002(3) -0.012(3) 0.016(3) C8 0.045(4) 0.052(4) 0.045(4) 0.002(3) -0.012(3) 0.025(3) C9 0.064(5) 0.042(4) 0.061(4) -0.007(3) -0.021(4) 0.026(3) C10 0.045(4) 0.037(3) 0.043(3) 0.003(3) -0.018(3) 0.012(3) C11 0.024(3) 0.095(6) 0.029(3) 0.005(4) -0.005(2) 0.011(3) C12 0.025(3) 0.036(3) 0.030(3) -0.005(2) -0.002(2) 0.008(2) C13 0.022(3) 0.069(4) 0.032(3) 0.004(3) 0.001(2) 0.012(3) C14 0.031(3) 0.045(3) 0.027(3) -0.001(2) 0.004(2) 0.010(2) C15 0.031(3) 0.080(5) 0.032(3) 0.003(3) 0.003(3) 0.015(3) C16 0.056(4) 0.041(3) 0.038(3) 0.002(3) 0.005(3) 0.020(3) C17 0.032(3) 0.033(3) 0.031(3) 0.005(2) 0.005(2) 0.008(2) C18 0.053(4) 0.024(3) 0.034(3) -0.010(2) -0.001(3) 0.008(3) C19 0.029(3) 0.034(3) 0.030(3) -0.008(2) 0.001(2) -0.006(2) C20 0.051(4) 0.035(3) 0.041(4) -0.012(3) -0.008(3) 0.003(3) C21 0.027(3) 0.041(3) 0.033(3) -0.001(3) -0.008(2) 0.002(2) C22 0.020(2) 0.034(3) 0.032(3) -0.006(2) -0.009(2) 0.005(2) C23 0.018(3) 0.036(3) 0.038(3) -0.005(2) -0.006(2) 0.002(2) C24 0.022(3) 0.032(3) 0.040(3) -0.005(2) 0.001(2) -0.005(2) C25 0.028(3) 0.050(4) 0.060(4) 0.008(3) -0.002(3) -0.015(3) F4 0.042(3) 0.299(11) 0.156(6) -0.164(7) -0.049(3) 0.054(4) F5 0.021(2) 0.217(6) 0.051(3) -0.008(3) -0.0031(18) 0.011(3) F6 0.056(4) 0.310(12) 0.196(8) 0.175(9) -0.057(4) -0.019(5) F7 0.060(2) 0.064(2) 0.037(2) 0.0149(18) -0.0002(17) 0.007(2) F8 0.041(2) 0.215(6) 0.040(2) 0.023(3) 0.0139(19) 0.041(3) F9 0.071(3) 0.067(3) 0.0332(19) -0.0080(18) -0.0053(18) 0.026(2) F10 0.047(2) 0.094(3) 0.087(3) 0.032(3) 0.009(2) 0.035(2) F11 0.081(3) 0.048(2) 0.037(2) 0.0088(17) 0.0041(18) 0.026(2) F12 0.118(4) 0.050(2) 0.055(2) 0.000(2) -0.003(2) 0.050(2) F13 0.147(5) 0.069(3) 0.038(2) 0.002(2) -0.024(3) 0.000(3) F14 0.133(4) 0.053(3) 0.063(3) -0.032(2) -0.035(3) 0.029(3) F15 0.041(3) 0.161(5) 0.105(4) -0.084(4) -0.018(3) 0.001(3) F16 0.056(3) 0.162(5) 0.035(2) 0.036(3) 0.0131(19) 0.055(3) F17 0.078(3) 0.063(3) 0.102(4) 0.012(3) -0.072(3) -0.007(2) F18 0.064(2) 0.062(2) 0.049(2) 0.0162(19) 0.0081(18) 0.033(2) F19 0.072(4) 0.073(4) 0.448(15) 0.138(6) 0.109(6) 0.028(3) F20 0.050(3) 0.104(4) 0.070(3) 0.020(3) -0.010(2) -0.048(2) F21 0.124(5) 0.125(5) 0.054(3) 0.006(3) 0.018(3) -0.071(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 F1 2.249(3) . ? Dy1 F2 2.267(3) 2 ? Dy1 O17 2.315(4) . ? Dy1 O14 2.331(4) . ? Dy1 O24 2.347(3) . ? Dy1 O22 2.362(3) . ? Dy1 O19 2.369(4) . ? Dy1 O12 2.431(3) . ? Cr1 F2 1.900(3) . ? Cr1 F1 1.912(3) . ? Cr1 O 1.949(3) 2 ? Cr1 O 1.951(3) . ? Cr1 N1 2.075(4) . ? Cr1 N2 2.081(4) . ? Cr1 Cr1 2.9186(16) 2 ? O Cr1 1.949(3) 2 ? O H 0.838(5) . ? F2 Dy1 2.267(3) 2 ? N1 C5 1.338(6) . ? N1 C1 1.350(6) . ? N2 C10 1.335(7) . ? N2 C6 1.342(6) . ? O12 C12 1.256(6) . ? O14 C14 1.251(6) . ? O17 C17 1.253(6) . ? O19 C19 1.240(7) . ? O22 C22 1.253(6) . ? O24 C24 1.259(6) . ? C1 C2 1.380(7) . ? C1 H1 0.9500 . ? C2 C3 1.384(8) . ? C2 H2 0.9500 . ? C3 C4 1.380(8) . ? C3 H3 0.9500 . ? C4 C5 1.386(7) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.381(7) . ? C6 H6 0.9500 . ? C7 C8 1.351(9) . ? C7 H7 0.9500 . ? C8 C9 1.371(9) . ? C8 H8 0.9500 . ? C9 C10 1.388(8) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 F5 1.260(7) . ? C11 F6 1.262(9) . ? C11 F4 1.264(9) . ? C11 C12 1.527(7) . ? C12 C13 1.379(8) . ? C13 C14 1.392(7) . ? C13 H13 0.9500 . ? C14 C15 1.531(8) . ? C15 F7 1.322(8) . ? C15 F8 1.323(7) . ? C15 F9 1.339(8) . ? C16 F10 1.307(8) . ? C16 F12 1.323(7) . ? C16 F11 1.339(7) . ? C16 C17 1.543(8) . ? C17 C18 1.383(8) . ? C18 C19 1.396(8) . ? C18 H18 0.9500 . ? C19 C20 1.541(8) . ? C20 F15 1.282(8) . ? C20 F14 1.299(7) . ? C20 F13 1.320(8) . ? C21 F17 1.311(6) . ? C21 F16 1.312(7) . ? C21 F18 1.327(7) . ? C21 C22 1.534(7) . ? C22 C23 1.385(8) . ? C23 C24 1.392(8) . ? C23 H23 0.9500 . ? C24 C25 1.530(8) . ? C25 F19 1.254(8) . ? C25 F20 1.289(7) . ? C25 F21 1.323(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Dy1 F2 79.38(9) . 2 ? F1 Dy1 O17 145.10(11) . . ? F2 Dy1 O17 78.97(11) 2 . ? F1 Dy1 O14 85.06(12) . . ? F2 Dy1 O14 144.08(10) 2 . ? O17 Dy1 O14 96.91(13) . . ? F1 Dy1 O24 111.70(12) . . ? F2 Dy1 O24 72.36(11) 2 . ? O17 Dy1 O24 87.17(13) . . ? O14 Dy1 O24 143.50(12) . . ? F1 Dy1 O22 72.53(11) . . ? F2 Dy1 O22 121.71(12) 2 . ? O17 Dy1 O22 142.37(12) . . ? O14 Dy1 O22 83.03(12) . . ? O24 Dy1 O22 72.46(12) . . ? F1 Dy1 O19 140.16(11) . . ? F2 Dy1 O19 136.47(11) 2 . ? O17 Dy1 O19 71.72(13) . . ? O14 Dy1 O19 72.32(13) . . ? O24 Dy1 O19 74.70(13) . . ? O22 Dy1 O19 72.51(13) . . ? F1 Dy1 O12 75.54(11) . . ? F2 Dy1 O12 74.23(11) 2 . ? O17 Dy1 O12 72.41(12) . . ? O14 Dy1 O12 70.59(12) . . ? O24 Dy1 O12 143.53(12) . . ? O22 Dy1 O12 139.92(12) . . ? O19 Dy1 O12 123.68(13) . . ? F2 Cr1 F1 178.94(11) . . ? F2 Cr1 O 87.90(13) . 2 ? F1 Cr1 O 91.16(13) . 2 ? F2 Cr1 O 91.22(13) . . ? F1 Cr1 O 88.18(13) . . ? O Cr1 O 83.10(14) 2 . ? F2 Cr1 N1 92.03(14) . . ? F1 Cr1 N1 88.49(14) . . ? O Cr1 N1 92.07(14) 2 . ? O Cr1 N1 174.07(15) . . ? F2 Cr1 N2 89.68(14) . . ? F1 Cr1 N2 91.21(14) . . ? O Cr1 N2 174.05(15) 2 . ? O Cr1 N2 91.52(14) . . ? N1 Cr1 N2 93.45(15) . . ? F2 Cr1 Cr1 89.42(8) . 2 ? F1 Cr1 Cr1 89.55(8) . 2 ? O Cr1 Cr1 41.58(9) 2 2 ? O Cr1 Cr1 41.52(9) . 2 ? N1 Cr1 Cr1 133.55(12) . 2 ? N2 Cr1 Cr1 132.99(11) . 2 ? Cr1 O Cr1 96.90(14) 2 . ? Cr1 O H 107(4) 2 . ? Cr1 O H 112(4) . . ? Cr1 F1 Dy1 140.26(13) . . ? Cr1 F2 Dy1 140.29(13) . 2 ? C5 N1 C1 118.2(4) . . ? C5 N1 Cr1 120.7(3) . . ? C1 N1 Cr1 121.0(3) . . ? C10 N2 C6 117.7(4) . . ? C10 N2 Cr1 121.4(3) . . ? C6 N2 Cr1 120.8(4) . . ? C12 O12 Dy1 134.0(3) . . ? C14 O14 Dy1 136.9(3) . . ? C17 O17 Dy1 136.5(3) . . ? C19 O19 Dy1 136.2(3) . . ? C22 O22 Dy1 131.4(3) . . ? C24 O24 Dy1 132.1(3) . . ? N1 C1 C2 121.8(5) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C1 C2 C3 119.6(5) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 119.0(5) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 118.4(5) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 123.1(5) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? N2 C6 C7 122.4(5) . . ? N2 C6 H6 118.8 . . ? C7 C6 H6 118.8 . . ? C8 C7 C6 119.0(5) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C7 C8 C9 120.0(6) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C10 118.2(6) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? N2 C10 C9 122.7(5) . . ? N2 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? F5 C11 F6 105.6(7) . . ? F5 C11 F4 109.5(7) . . ? F6 C11 F4 101.5(8) . . ? F5 C11 C12 116.5(5) . . ? F6 C11 C12 111.8(6) . . ? F4 C11 C12 110.8(6) . . ? O12 C12 C13 127.0(5) . . ? O12 C12 C11 114.8(5) . . ? C13 C12 C11 118.3(5) . . ? C12 C13 C14 121.2(5) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? O14 C14 C13 127.2(5) . . ? O14 C14 C15 114.2(5) . . ? C13 C14 C15 118.6(5) . . ? F7 C15 F8 107.9(6) . . ? F7 C15 F9 107.2(5) . . ? F8 C15 F9 107.1(6) . . ? F7 C15 C14 110.8(5) . . ? F8 C15 C14 113.2(5) . . ? F9 C15 C14 110.5(5) . . ? F10 C16 F12 108.7(5) . . ? F10 C16 F11 106.4(5) . . ? F12 C16 F11 107.0(5) . . ? F10 C16 C17 110.6(5) . . ? F12 C16 C17 113.1(5) . . ? F11 C16 C17 110.7(5) . . ? O17 C17 C18 128.5(5) . . ? O17 C17 C16 113.1(5) . . ? C18 C17 C16 118.3(5) . . ? C17 C18 C19 119.9(5) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? O19 C19 C18 127.1(5) . . ? O19 C19 C20 114.2(5) . . ? C18 C19 C20 118.7(5) . . ? F15 C20 F14 107.8(6) . . ? F15 C20 F13 106.6(6) . . ? F14 C20 F13 105.6(6) . . ? F15 C20 C19 111.5(6) . . ? F14 C20 C19 114.6(5) . . ? F13 C20 C19 110.3(5) . . ? F17 C21 F16 108.2(5) . . ? F17 C21 F18 106.1(5) . . ? F16 C21 F18 105.6(5) . . ? F17 C21 C22 113.7(5) . . ? F16 C21 C22 112.7(5) . . ? F18 C21 C22 110.0(5) . . ? O22 C22 C23 128.2(5) . . ? O22 C22 C21 114.6(5) . . ? C23 C22 C21 117.1(4) . . ? C22 C23 C24 121.0(5) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? O24 C24 C23 127.6(5) . . ? O24 C24 C25 114.2(5) . . ? C23 C24 C25 118.2(5) . . ? F19 C25 F20 109.2(7) . . ? F19 C25 F21 105.4(8) . . ? F20 C25 F21 103.6(6) . . ? F19 C25 C24 112.5(6) . . ? F20 C25 C24 114.9(6) . . ? F21 C25 C24 110.5(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O H O12 0.838(5) 1.984(15) 2.802(5) 165(5) 2 _diffrn_measured_fraction_theta_max .991 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full .991 _refine_diff_density_max 1.787 _refine_diff_density_min -1.493 _refine_diff_density_rms .158 #------------------------------------------------------------------------------ #------------------------------------------------------------------------------