#------------------------------------------------------------------------------ #$Date: 2022-01-06 23:46:09 +0200 (Thu, 06 Jan 2022) $ #$Revision: 271854 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061033.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7061033 loop_ _publ_author_name 'Tubau, \`Annia' 'Rodr\'iguez, Laura' 'L\'azaro, Ariadna' 'Vicente, Ramon' 'Font-Bard\'ia, Merc\`e' _publ_section_title ; Improving the emission quantum yield in dinuclear Eu(iii) and Tb(iii) complexes with 2-fluorobenzoate ; _journal_issue 47 _journal_name_full 'New Journal of Chemistry' _journal_page_first 22208 _journal_page_last 22215 _journal_paper_doi 10.1039/D1NJ04335H _journal_volume 45 _journal_year 2021 _chemical_formula_moiety 'C56 H38 Eu2 F8 O18' _chemical_formula_sum 'C56 H38 Eu2 F8 O18' _chemical_formula_weight 1454.78 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_block_doi 10.5517/ccdc.csd.cc28dtvc _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-07-20 deposited with the CCDC. 2021-10-29 downloaded from the CCDC. ; _cell_angle_alpha 110.681(3) _cell_angle_beta 93.121(3) _cell_angle_gamma 92.453(3) _cell_formula_units_Z 1 _cell_length_a 9.0953(8) _cell_length_b 11.3783(10) _cell_length_c 13.6591(12) _cell_measurement_reflns_used 9880 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.53 _cell_measurement_theta_min 2.66 _cell_volume 1317.6(2) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_unetI/netI 0.0232 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 48286 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.576 _diffrn_reflns_theta_min 2.659 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 2.464 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.833 _exptl_crystal_description prism _exptl_crystal_F_000 716 _exptl_crystal_size_max 0.181 _exptl_crystal_size_mid 0.055 _exptl_crystal_size_min 0.046 _refine_diff_density_max 0.998 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.097 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 385 _refine_ls_number_reflns 8053 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.104 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0199 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0157P)^2^+1.2979P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.0467 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7500 _reflns_number_total 8053 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj04335h2.cif _cod_data_source_block I95XB146_0m_a _cod_depositor_comments 'Adding full bibliography for 7061033.cif.' _cod_database_code 7061033 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; TITL I95XB146_0m_a.res in P-1 I95XB146_0m_a.res created by SHELXL-2018/3 at 10:13:23 on 14-Nov-2019 REM Old TITL I95XB146_0m in P1 REM SHELXT solution in P-1 REM R1 0.059, Rweak 0.010, Alpha 0.056, Orientation as input REM Formula found by SHELXT: C27 Eu F9 N2 O3 CELL 0.71073 9.0953 11.3783 13.6591 110.681 93.121 92.453 ZERR 1.000 0.0008 0.0010 0.0012 0.003 0.003 0.003 LATT 1 SFAC C H EU F O UNIT 56 38 2 8 18 TEMP -173.150 L.S. 10 BOND $H LIST 6 ACTA FMAP 2 DFIX 0.8 0.01 O9 H9OA DFIX 0.8 0.01 O9 H9OB DFIX 1.3 0.01 H9OB H9OA OMIT 0 -1 1 OMIT 9 -9 12 OMIT 8 -10 12 OMIT 8 -10 13 PLAN 20 WGHT 0.015700 1.297900 FVAR 0.42956 EU1 3 0.683843 0.430925 0.937938 11.00000 0.00759 0.01172 = 0.01223 0.00442 0.00283 0.00221 F1 4 0.790206 0.237122 0.559337 11.00000 0.07928 0.04828 = 0.02203 -0.00100 0.01298 -0.03115 F2 4 0.632027 0.586947 0.674094 11.00000 0.04228 0.06925 = 0.04351 0.03818 0.02623 0.03143 F3 4 0.052841 0.163891 0.796431 11.00000 0.02314 0.04012 = 0.03791 -0.00532 0.00942 -0.01299 F4 4 0.881589 -0.102629 0.705762 11.00000 0.07938 0.03903 = 0.05363 0.02432 0.04836 0.03693 O1 5 0.892305 0.510521 0.850909 11.00000 0.01354 0.01855 = 0.01423 0.00506 0.00352 0.00259 O2 5 0.754809 0.340125 0.758957 11.00000 0.02174 0.01502 = 0.01737 0.00504 0.00732 0.00079 O3 5 0.580041 0.562793 0.857083 11.00000 0.01335 0.02253 = 0.02183 0.01277 0.00612 0.00629 O4 5 0.356894 0.618619 0.911776 11.00000 0.01444 0.02032 = 0.01757 0.00944 0.00614 0.00649 O5 5 0.428054 0.381595 0.916278 11.00000 0.00992 0.01501 = 0.01631 0.00446 0.00053 0.00083 O6 5 0.188538 0.386409 0.922042 11.00000 0.00993 0.01744 = 0.01801 0.00288 0.00471 0.00222 O7 5 0.646661 0.197944 0.872544 11.00000 0.01629 0.01298 = 0.02085 0.00514 0.00562 0.00322 O8 5 0.742031 0.097951 0.719986 11.00000 0.02878 0.01544 = 0.01943 0.00479 0.00712 0.00261 AFIX 83 H8OA 2 0.750644 0.170306 0.716841 11.00000 -1.20000 AFIX 0 O9 5 0.912372 0.352069 0.981821 11.00000 0.00991 0.02049 = 0.01713 0.00642 0.00311 0.00285 H9OA 2 0.946277 0.390407 1.040169 11.00000 -1.20000 H9OB 2 0.977436 0.344685 0.943374 11.00000 -1.20000 C1 1 0.861171 0.420510 0.766574 11.00000 0.01510 0.01495 = 0.01583 0.00783 0.00513 0.00583 C2 1 0.949040 0.405602 0.673925 11.00000 0.01987 0.01804 = 0.01551 0.00818 0.00803 0.00802 C3 1 1.077368 0.482743 0.685633 11.00000 0.01803 0.03882 = 0.02250 0.01558 0.00601 0.00287 AFIX 43 H3 2 1.108122 0.543932 0.752443 11.00000 -1.20000 AFIX 0 C4 1 1.160617 0.471041 0.600686 11.00000 0.01870 0.05708 = 0.03175 0.02442 0.00991 0.00418 AFIX 43 H4 2 1.247604 0.524114 0.609504 11.00000 -1.20000 AFIX 0 C5 1 1.116428 0.381828 0.503181 11.00000 0.03278 0.04887 = 0.02837 0.02243 0.01884 0.01963 AFIX 43 H5 2 1.172969 0.374291 0.445046 11.00000 -1.20000 AFIX 0 C6 1 0.991293 0.304133 0.489996 11.00000 0.05203 0.03087 = 0.01867 0.00759 0.01707 0.01165 AFIX 43 H6 2 0.960986 0.242787 0.423169 11.00000 -1.20000 AFIX 0 C7 1 0.910125 0.316525 0.575393 11.00000 0.03900 0.02245 = 0.02055 0.00689 0.01129 0.00069 C8 1 0.462552 0.616586 0.855463 11.00000 0.01526 0.01494 = 0.01542 0.00724 0.00197 0.00274 C9 1 0.445012 0.688554 0.782425 11.00000 0.01644 0.02581 = 0.02145 0.01518 0.00218 0.00271 C10 1 0.336722 0.776885 0.799225 11.00000 0.02376 0.02868 = 0.02725 0.01547 0.00277 0.00626 AFIX 43 H10 2 0.272952 0.786725 0.854006 11.00000 -1.20000 AFIX 0 C11 1 0.321650 0.849673 0.737181 11.00000 0.03303 0.03640 = 0.04345 0.02615 0.00199 0.01232 AFIX 43 H11 2 0.249288 0.910104 0.750457 11.00000 -1.20000 AFIX 0 C12 1 0.411744 0.834495 0.655991 11.00000 0.03547 0.05343 = 0.04871 0.04131 0.00473 0.00871 AFIX 43 H12 2 0.402381 0.885432 0.614159 11.00000 -1.20000 AFIX 0 C13 1 0.515344 0.745423 0.635570 11.00000 0.03449 0.07005 = 0.04634 0.04638 0.01606 0.01545 AFIX 43 H13 2 0.575313 0.732686 0.578352 11.00000 -1.20000 AFIX 0 C14 1 0.530891 0.674985 0.699245 11.00000 0.02267 0.04138 = 0.03470 0.02534 0.01042 0.01290 C15 1 0.299569 0.341602 0.874161 11.00000 0.01149 0.01288 = 0.01440 0.00649 0.00226 0.00128 C16 1 0.281492 0.245829 0.766260 11.00000 0.01432 0.01431 = 0.01401 0.00354 -0.00027 0.00315 C17 1 0.389462 0.239283 0.695974 11.00000 0.02119 0.02634 = 0.01836 0.00861 0.00519 0.00427 AFIX 43 H17 2 0.476862 0.293325 0.718428 11.00000 -1.20000 AFIX 0 C18 1 0.369956 0.154372 0.593548 11.00000 0.03915 0.03131 = 0.01596 0.00862 0.00860 0.01427 AFIX 43 H18 2 0.443774 0.150847 0.546168 11.00000 -1.20000 AFIX 0 C19 1 0.243464 0.074877 0.560201 11.00000 0.04556 0.02326 = 0.01517 0.00055 -0.00467 0.01233 AFIX 43 H19 2 0.230261 0.017938 0.489653 11.00000 -1.20000 AFIX 0 C20 1 0.136118 0.077543 0.628594 11.00000 0.03053 0.02263 = 0.02491 -0.00058 -0.00749 0.00189 AFIX 43 H20 2 0.050116 0.021750 0.606395 11.00000 -1.20000 AFIX 0 C21 1 0.156816 0.163162 0.729887 11.00000 0.01683 0.02184 = 0.02086 0.00295 -0.00041 0.00241 C22 1 0.704247 0.106378 0.813815 11.00000 0.01341 0.01447 = 0.01824 0.00413 0.00216 -0.00079 C23 1 0.737192 -0.000657 0.847152 11.00000 0.01889 0.01261 = 0.02193 0.00494 0.00368 0.00190 C24 1 0.681733 -0.001816 0.939828 11.00000 0.03551 0.02297 = 0.02828 0.01166 0.01130 0.01128 AFIX 43 H24 2 0.619996 0.062170 0.976259 11.00000 -1.20000 AFIX 0 C25 1 0.714814 -0.094498 0.980010 11.00000 0.04798 0.03116 = 0.03489 0.02060 0.01229 0.01314 AFIX 43 H25 2 0.674986 -0.094166 1.042968 11.00000 -1.20000 AFIX 0 C26 1 0.805716 -0.187323 0.928454 11.00000 0.03462 0.02230 = 0.04627 0.01823 0.00208 0.00768 AFIX 43 H26 2 0.829736 -0.250058 0.956565 11.00000 -1.20000 AFIX 0 C27 1 0.861559 -0.188934 0.836254 11.00000 0.03544 0.02061 = 0.05117 0.01513 0.01383 0.01332 AFIX 43 H27 2 0.923757 -0.252780 0.800286 11.00000 -1.20000 AFIX 0 C28 1 0.826232 -0.097013 0.796833 11.00000 0.03227 0.01996 = 0.03279 0.00894 0.01399 0.00897 HKLF 4 REM I95XB146_0m_a.res in P-1 REM wR2 = 0.0467, GooF = S = 1.104, Restrained GooF = 1.104 for all data REM R1 = 0.0199 for 7500 Fo > 4sig(Fo) and 0.0237 for all 8053 data REM 385 parameters refined using 3 restraints END WGHT 0.0157 1.2979 REM Highest difference peak 0.998, deepest hole -0.754, 1-sigma level 0.097 Q1 1 0.0530 0.2946 0.8166 11.00000 0.05 1.00 Q2 1 0.2096 0.7632 0.8451 11.00000 0.05 0.77 Q3 1 0.4472 0.6575 0.8196 11.00000 0.05 0.58 Q4 1 1.0710 0.3254 0.5088 11.00000 0.05 0.54 Q5 1 0.9208 0.4160 0.7260 11.00000 0.05 0.54 Q6 1 0.2921 0.2954 0.8172 11.00000 0.05 0.50 Q7 1 0.1293 0.1337 0.6699 11.00000 0.05 0.48 Q8 1 0.8757 0.2200 0.5675 11.00000 0.05 0.47 Q9 1 0.4255 0.1036 0.6884 11.00000 0.05 0.47 Q10 1 0.9329 0.3589 0.6299 11.00000 0.05 0.46 Q11 1 1.0077 0.4431 0.6758 11.00000 0.05 0.44 Q12 1 1.1081 0.4262 0.5501 11.00000 0.05 0.43 Q13 1 0.3980 0.1640 0.6506 11.00000 0.05 0.42 Q14 1 0.3546 0.2096 0.6371 11.00000 0.05 0.41 Q15 1 0.7080 0.0417 0.8179 11.00000 0.05 0.40 Q16 1 0.3618 0.8194 0.7813 11.00000 0.05 0.39 Q17 1 1.0734 0.3449 0.7748 11.00000 0.05 0.39 Q18 1 0.6834 0.3117 0.9182 11.00000 0.05 0.38 Q19 1 0.3785 0.7213 0.7376 11.00000 0.05 0.38 Q20 1 0.2173 0.2186 0.7601 11.00000 0.05 0.37 ; _shelx_res_checksum 62827 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.68384(2) 0.43093(2) 0.93794(2) 0.01034(3) Uani 1 1 d . . . . . F1 F 0.7902(2) 0.23712(16) 0.55934(12) 0.0542(5) Uani 1 1 d . . . . . F2 F 0.63203(18) 0.58695(17) 0.67409(12) 0.0450(4) Uani 1 1 d . . . . . F3 F 0.05284(15) 0.16389(14) 0.79643(12) 0.0391(4) Uani 1 1 d . . . . . F4 F 0.8816(2) -0.10263(15) 0.70576(14) 0.0525(5) Uani 1 1 d . . . . . O1 O 0.89231(14) 0.51052(12) 0.85091(10) 0.0155(2) Uani 1 1 d . . . . . O2 O 0.75481(15) 0.34012(12) 0.75896(11) 0.0180(3) Uani 1 1 d . . . . . O3 O 0.58004(14) 0.56279(13) 0.85708(11) 0.0176(3) Uani 1 1 d . . . . . O4 O 0.35689(14) 0.61862(13) 0.91178(10) 0.0164(3) Uani 1 1 d . . . . . O5 O 0.42805(13) 0.38160(12) 0.91628(10) 0.0141(2) Uani 1 1 d . . . . . O6 O 0.18854(13) 0.38641(13) 0.92204(10) 0.0159(2) Uani 1 1 d . . . . . O7 O 0.64666(14) 0.19794(12) 0.87254(11) 0.0167(3) Uani 1 1 d . . . . . O8 O 0.74203(16) 0.09795(13) 0.71999(11) 0.0214(3) Uani 1 1 d . . . . . H8OA H 0.750644 0.170306 0.716841 0.026 Uiso 1 1 calc R U . . . O9 O 0.91237(14) 0.35207(13) 0.98182(11) 0.0158(2) Uani 1 1 d D . . . . H9OA H 0.946(2) 0.390(2) 1.0402(8) 0.019 Uiso 1 1 d D U . . . H9OB H 0.9774(18) 0.345(2) 0.9434(13) 0.019 Uiso 1 1 d D U . . . C1 C 0.8612(2) 0.42051(17) 0.76657(14) 0.0144(3) Uani 1 1 d . . . . . C2 C 0.9490(2) 0.40560(18) 0.67392(15) 0.0167(3) Uani 1 1 d . . . . . C3 C 1.0774(2) 0.4827(2) 0.68563(17) 0.0250(4) Uani 1 1 d . . . . . H3 H 1.108122 0.543932 0.752443 0.030 Uiso 1 1 calc R U . . . C4 C 1.1606(2) 0.4710(3) 0.60069(19) 0.0332(5) Uani 1 1 d . . . . . H4 H 1.247604 0.524114 0.609504 0.040 Uiso 1 1 calc R U . . . C5 C 1.1164(3) 0.3818(3) 0.50318(19) 0.0332(5) Uani 1 1 d . . . . . H5 H 1.172969 0.374291 0.445046 0.040 Uiso 1 1 calc R U . . . C6 C 0.9913(3) 0.3041(2) 0.49000(18) 0.0334(5) Uani 1 1 d . . . . . H6 H 0.960986 0.242787 0.423169 0.040 Uiso 1 1 calc R U . . . C7 C 0.9101(3) 0.3165(2) 0.57539(17) 0.0272(5) Uani 1 1 d . . . . . C8 C 0.4626(2) 0.61659(17) 0.85546(14) 0.0146(3) Uani 1 1 d . . . . . C9 C 0.4450(2) 0.68855(19) 0.78243(16) 0.0193(4) Uani 1 1 d . . . . . C10 C 0.3367(2) 0.7769(2) 0.79922(18) 0.0249(4) Uani 1 1 d . . . . . H10 H 0.272952 0.786725 0.854006 0.030 Uiso 1 1 calc R U . . . C11 C 0.3216(3) 0.8497(2) 0.7372(2) 0.0341(5) Uani 1 1 d . . . . . H11 H 0.249288 0.910104 0.750457 0.041 Uiso 1 1 calc R U . . . C12 C 0.4117(3) 0.8345(3) 0.6560(2) 0.0394(6) Uani 1 1 d . . . . . H12 H 0.402381 0.885432 0.614159 0.047 Uiso 1 1 calc R U . . . C13 C 0.5153(3) 0.7454(3) 0.6356(2) 0.0425(7) Uani 1 1 d . . . . . H13 H 0.575313 0.732686 0.578352 0.051 Uiso 1 1 calc R U . . . C14 C 0.5309(2) 0.6750(2) 0.69925(19) 0.0291(5) Uani 1 1 d . . . . . C15 C 0.29957(19) 0.34160(16) 0.87416(14) 0.0124(3) Uani 1 1 d . . . . . C16 C 0.2815(2) 0.24583(17) 0.76626(14) 0.0146(3) Uani 1 1 d . . . . . C17 C 0.3895(2) 0.2393(2) 0.69597(16) 0.0216(4) Uani 1 1 d . . . . . H17 H 0.476862 0.293325 0.718428 0.026 Uiso 1 1 calc R U . . . C18 C 0.3700(3) 0.1544(2) 0.59355(16) 0.0281(5) Uani 1 1 d . . . . . H18 H 0.443774 0.150847 0.546168 0.034 Uiso 1 1 calc R U . . . C19 C 0.2435(3) 0.0749(2) 0.56020(17) 0.0297(5) Uani 1 1 d . . . . . H19 H 0.230261 0.017938 0.489653 0.036 Uiso 1 1 calc R U . . . C20 C 0.1361(3) 0.0775(2) 0.62859(18) 0.0288(5) Uani 1 1 d . . . . . H20 H 0.050116 0.021750 0.606395 0.035 Uiso 1 1 calc R U . . . C21 C 0.1568(2) 0.16316(19) 0.72989(16) 0.0211(4) Uani 1 1 d . . . . . C22 C 0.7042(2) 0.10638(17) 0.81381(15) 0.0158(3) Uani 1 1 d . . . . . C23 C 0.7372(2) -0.00066(17) 0.84715(16) 0.0180(4) Uani 1 1 d . . . . . C24 C 0.6817(3) -0.0018(2) 0.93983(18) 0.0276(5) Uani 1 1 d . . . . . H24 H 0.619996 0.062170 0.976259 0.033 Uiso 1 1 calc R U . . . C25 C 0.7148(3) -0.0945(2) 0.9800(2) 0.0349(5) Uani 1 1 d . . . . . H25 H 0.674986 -0.094166 1.042968 0.042 Uiso 1 1 calc R U . . . C26 C 0.8057(3) -0.1873(2) 0.9285(2) 0.0326(5) Uani 1 1 d . . . . . H26 H 0.829736 -0.250058 0.956565 0.039 Uiso 1 1 calc R U . . . C27 C 0.8616(3) -0.1889(2) 0.8363(2) 0.0343(5) Uani 1 1 d . . . . . H27 H 0.923757 -0.252780 0.800286 0.041 Uiso 1 1 calc R U . . . C28 C 0.8262(3) -0.0970(2) 0.79683(19) 0.0278(5) 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 Eu1 0.00759(4) 0.01172(4) 0.01223(4) 0.00442(3) 0.00283(3) 0.00221(3) F1 0.0793(13) 0.0483(10) 0.0220(7) -0.0010(7) 0.0130(8) -0.0312(9) F2 0.0423(9) 0.0693(11) 0.0435(9) 0.0382(9) 0.0262(7) 0.0314(8) F3 0.0231(7) 0.0401(8) 0.0379(8) -0.0053(6) 0.0094(6) -0.0130(6) F4 0.0794(13) 0.0390(9) 0.0536(10) 0.0243(8) 0.0484(9) 0.0369(9) O1 0.0135(6) 0.0185(6) 0.0142(6) 0.0051(5) 0.0035(5) 0.0026(5) O2 0.0217(7) 0.0150(6) 0.0174(6) 0.0050(5) 0.0073(5) 0.0008(5) O3 0.0133(6) 0.0225(7) 0.0218(7) 0.0128(6) 0.0061(5) 0.0063(5) O4 0.0144(6) 0.0203(6) 0.0176(6) 0.0094(5) 0.0061(5) 0.0065(5) O5 0.0099(5) 0.0150(6) 0.0163(6) 0.0045(5) 0.0005(4) 0.0008(4) O6 0.0099(6) 0.0174(6) 0.0180(6) 0.0029(5) 0.0047(5) 0.0022(5) O7 0.0163(6) 0.0130(6) 0.0209(7) 0.0051(5) 0.0056(5) 0.0032(5) O8 0.0288(7) 0.0154(6) 0.0194(7) 0.0048(5) 0.0071(6) 0.0026(5) O9 0.0099(6) 0.0205(7) 0.0171(6) 0.0064(5) 0.0031(5) 0.0029(5) C1 0.0151(8) 0.0149(8) 0.0158(8) 0.0078(7) 0.0051(6) 0.0058(6) C2 0.0199(9) 0.0180(9) 0.0155(8) 0.0082(7) 0.0080(7) 0.0080(7) C3 0.0180(9) 0.0388(12) 0.0225(10) 0.0156(9) 0.0060(7) 0.0029(8) C4 0.0187(10) 0.0571(16) 0.0318(12) 0.0244(12) 0.0099(9) 0.0042(10) C5 0.0328(12) 0.0489(15) 0.0284(12) 0.0224(11) 0.0188(9) 0.0196(11) C6 0.0520(15) 0.0309(12) 0.0187(10) 0.0076(9) 0.0171(10) 0.0117(11) C7 0.0390(12) 0.0224(10) 0.0205(10) 0.0069(8) 0.0113(9) 0.0007(9) C8 0.0153(8) 0.0149(8) 0.0154(8) 0.0072(7) 0.0020(6) 0.0027(6) C9 0.0164(8) 0.0258(10) 0.0215(9) 0.0152(8) 0.0022(7) 0.0027(7) C10 0.0238(10) 0.0287(11) 0.0272(11) 0.0155(9) 0.0028(8) 0.0063(8) C11 0.0330(12) 0.0364(13) 0.0435(14) 0.0261(12) 0.0020(10) 0.0123(10) C12 0.0355(13) 0.0534(16) 0.0487(16) 0.0413(14) 0.0047(11) 0.0087(12) C13 0.0345(13) 0.0700(19) 0.0463(15) 0.0464(15) 0.0161(11) 0.0155(13) C14 0.0227(10) 0.0414(13) 0.0347(12) 0.0253(11) 0.0104(9) 0.0129(9) C15 0.0115(7) 0.0129(8) 0.0144(8) 0.0065(6) 0.0023(6) 0.0013(6) C16 0.0143(8) 0.0143(8) 0.0140(8) 0.0035(7) -0.0003(6) 0.0031(6) C17 0.0212(9) 0.0263(10) 0.0184(9) 0.0086(8) 0.0052(7) 0.0043(8) C18 0.0391(12) 0.0313(11) 0.0160(9) 0.0086(9) 0.0086(8) 0.0143(10) C19 0.0456(14) 0.0233(10) 0.0152(9) 0.0005(8) -0.0047(9) 0.0123(9) C20 0.0305(11) 0.0226(10) 0.0249(11) -0.0006(9) -0.0075(9) 0.0019(9) C21 0.0168(9) 0.0218(9) 0.0209(9) 0.0029(8) -0.0004(7) 0.0024(7) C22 0.0134(8) 0.0145(8) 0.0182(9) 0.0041(7) 0.0022(6) -0.0008(6) C23 0.0189(9) 0.0126(8) 0.0219(9) 0.0049(7) 0.0037(7) 0.0019(7) C24 0.0355(12) 0.0230(10) 0.0283(11) 0.0117(9) 0.0113(9) 0.0113(9) C25 0.0480(15) 0.0312(12) 0.0349(13) 0.0206(11) 0.0123(11) 0.0131(11) C26 0.0346(12) 0.0223(10) 0.0463(14) 0.0182(10) 0.0021(10) 0.0077(9) C27 0.0354(13) 0.0206(10) 0.0512(15) 0.0151(10) 0.0138(11) 0.0133(9) C28 0.0323(11) 0.0200(10) 0.0328(12) 0.0089(9) 0.0140(9) 0.0090(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Eu1 O3 73.27(4) . . ? O5 Eu1 O4 78.44(4) . 2_667 ? O3 Eu1 O4 135.96(4) . 2_667 ? O5 Eu1 O9 140.80(4) . . ? O3 Eu1 O9 144.53(4) . . ? O4 Eu1 O9 74.25(4) 2_667 . ? O5 Eu1 O2 101.91(5) . . ? O3 Eu1 O2 77.25(5) . . ? O4 Eu1 O2 142.38(5) 2_667 . ? O9 Eu1 O2 83.97(5) . . ? O5 Eu1 O6 125.29(4) . 2_667 ? O3 Eu1 O6 91.13(5) . 2_667 ? O4 Eu1 O6 78.39(5) 2_667 2_667 ? O9 Eu1 O6 75.81(4) . 2_667 ? O2 Eu1 O6 125.78(4) . 2_667 ? O5 Eu1 O7 73.09(4) . . ? O3 Eu1 O7 125.41(5) . . ? O4 Eu1 O7 75.14(5) 2_667 . ? O9 Eu1 O7 73.07(5) . . ? O2 Eu1 O7 69.27(4) . . ? O6 Eu1 O7 143.45(4) 2_667 . ? O5 Eu1 O1 140.63(4) . . ? O3 Eu1 O1 72.48(4) . . ? O4 Eu1 O1 140.81(4) 2_667 . ? O9 Eu1 O1 72.26(4) . . ? O2 Eu1 O1 51.69(4) . . ? O6 Eu1 O1 74.20(4) 2_667 . ? O7 Eu1 O1 113.02(4) . . ? O5 Eu1 O5 74.81(5) . 2_667 ? O3 Eu1 O5 71.87(4) . 2_667 ? O4 Eu1 O5 68.52(4) 2_667 2_667 ? O9 Eu1 O5 118.74(4) . 2_667 ? O2 Eu1 O5 148.58(4) . 2_667 ? O6 Eu1 O5 50.62(4) 2_667 2_667 ? O7 Eu1 O5 135.27(4) . 2_667 ? O1 Eu1 O5 111.60(4) . 2_667 ? O5 Eu1 C1 123.24(5) . . ? O3 Eu1 C1 73.34(5) . . ? O4 Eu1 C1 150.32(5) 2_667 . ? O9 Eu1 C1 76.59(5) . . ? O2 Eu1 C1 26.03(5) . . ? O6 Eu1 C1 99.80(5) 2_667 . ? O7 Eu1 C1 91.22(5) . . ? O1 Eu1 C1 25.67(5) . . ? O5 Eu1 C1 132.74(5) 2_667 . ? O5 Eu1 C15 100.03(5) . 2_667 ? O3 Eu1 C15 83.39(5) . 2_667 ? O4 Eu1 C15 69.00(5) 2_667 2_667 ? O9 Eu1 C15 95.87(5) . 2_667 ? O2 Eu1 C15 144.96(5) . 2_667 ? O6 Eu1 C15 25.26(4) 2_667 2_667 ? O7 Eu1 C15 144.12(5) . 2_667 ? O1 Eu1 C15 94.75(4) . 2_667 ? O5 Eu1 C15 25.65(4) 2_667 2_667 ? C1 Eu1 C15 119.93(5) . 2_667 ? O5 Eu1 Eu1 39.95(3) . 2_667 ? O3 Eu1 Eu1 67.82(3) . 2_667 ? O4 Eu1 Eu1 68.76(3) 2_667 2_667 ? O9 Eu1 Eu1 141.15(3) . 2_667 ? O2 Eu1 Eu1 133.64(3) . 2_667 ? O6 Eu1 Eu1 85.41(3) 2_667 2_667 ? O7 Eu1 Eu1 107.48(3) . 2_667 ? O1 Eu1 Eu1 134.65(3) . 2_667 ? O5 Eu1 Eu1 34.86(3) 2_667 2_667 ? C1 Eu1 Eu1 140.92(3) . 2_667 ? C15 Eu1 Eu1 60.22(3) 2_667 2_667 ? C1 O1 Eu1 90.67(10) . . ? C1 O2 Eu1 97.32(11) . . ? C8 O3 Eu1 138.92(12) . . ? C8 O4 Eu1 136.68(12) . 2_667 ? C15 O5 Eu1 161.60(12) . . ? C15 O5 Eu1 89.86(10) . 2_667 ? Eu1 O5 Eu1 105.19(5) . 2_667 ? C15 O6 Eu1 98.19(11) . 2_667 ? C22 O7 Eu1 138.40(12) . . ? C22 O8 H8OA 109.5 . . ? Eu1 O9 H9OA 113.1(16) . . ? Eu1 O9 H9OB 118.0(16) . . ? H9OA O9 H9OB 107.8(15) . . ? O1 C1 O2 120.30(16) . . ? O1 C1 C2 120.24(17) . . ? O2 C1 C2 119.45(17) . . ? O1 C1 Eu1 63.66(9) . . ? O2 C1 Eu1 56.65(9) . . ? C2 C1 Eu1 175.94(13) . . ? C7 C2 C3 117.43(18) . . ? C7 C2 C1 122.88(18) . . ? C3 C2 C1 119.69(18) . . ? C4 C3 C2 120.8(2) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 119.8(2) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C6 C5 C4 120.4(2) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 119.0(2) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? F1 C7 C6 117.0(2) . . ? F1 C7 C2 120.50(18) . . ? C6 C7 C2 122.5(2) . . ? O3 C8 O4 125.89(16) . . ? O3 C8 C9 118.40(16) . . ? O4 C8 C9 115.69(16) . . ? C14 C9 C10 116.93(18) . . ? C14 C9 C8 123.97(18) . . ? C10 C9 C8 119.09(17) . . ? C11 C10 C9 121.0(2) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 120.0(2) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 120.1(2) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 119.3(2) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? F2 C14 C13 116.7(2) . . ? F2 C14 C9 120.62(18) . . ? C13 C14 C9 122.6(2) . . ? O6 C15 O5 119.97(16) . . ? O6 C15 C16 120.65(16) . . ? O5 C15 C16 119.32(15) . . ? O6 C15 Eu1 56.55(9) . 2_667 ? O5 C15 Eu1 64.49(9) . 2_667 ? C16 C15 Eu1 166.93(12) . 2_667 ? C21 C16 C17 117.45(18) . . ? C21 C16 C15 122.39(16) . . ? C17 C16 C15 120.12(17) . . ? C18 C17 C16 120.5(2) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 120.2(2) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 120.6(2) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 118.4(2) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? F3 C21 C20 118.04(19) . . ? F3 C21 C16 119.08(17) . . ? C20 C21 C16 122.9(2) . . ? O7 C22 O8 122.93(17) . . ? O7 C22 C23 120.59(17) . . ? O8 C22 C23 116.47(16) . . ? C28 C23 C24 116.87(18) . . ? C28 C23 C22 125.44(18) . . ? C24 C23 C22 117.59(17) . . ? C25 C24 C23 121.3(2) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C26 C25 C24 120.0(2) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C27 C26 C25 120.0(2) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 119.3(2) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? F4 C28 C27 117.52(19) . . ? F4 C28 C23 119.89(19) . . ? C27 C28 C23 122.6(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O5 2.3476(12) . ? Eu1 O3 2.3538(13) . ? Eu1 O4 2.3562(13) 2_667 ? Eu1 O9 2.4266(13) . ? Eu1 O2 2.4301(13) . ? Eu1 O6 2.4636(14) 2_667 ? Eu1 O7 2.4814(13) . ? Eu1 O1 2.5860(13) . ? Eu1 O5 2.6378(13) 2_667 ? Eu1 C1 2.8854(17) . ? Eu1 C15 2.9226(18) 2_667 ? Eu1 Eu1 3.9641(3) 2_667 ? F1 C7 1.343(3) . ? F2 C14 1.356(3) . ? F3 C21 1.345(2) . ? F4 C28 1.349(3) . ? O1 C1 1.250(2) . ? O2 C1 1.276(2) . ? O3 C8 1.257(2) . ? O4 C8 1.259(2) . ? O5 C15 1.265(2) . ? O6 C15 1.260(2) . ? O7 C22 1.227(2) . ? O8 C22 1.317(2) . ? O8 H8OA 0.8400 . ? O9 H9OA 0.798(9) . ? O9 H9OB 0.800(9) . ? C1 C2 1.496(2) . ? C2 C7 1.385(3) . ? C2 C3 1.397(3) . ? C3 C4 1.390(3) . ? C3 H3 0.9500 . ? C4 C5 1.385(4) . ? C4 H4 0.9500 . ? C5 C6 1.374(4) . ? C5 H5 0.9500 . ? C6 C7 1.383(3) . ? C6 H6 0.9500 . ? C8 C9 1.504(2) . ? C9 C14 1.381(3) . ? C9 C10 1.407(3) . ? C10 C11 1.384(3) . ? C10 H10 0.9500 . ? C11 C12 1.381(4) . ? C11 H11 0.9500 . ? C12 C13 1.380(4) . ? C12 H12 0.9500 . ? C13 C14 1.381(3) . ? C13 H13 0.9500 . ? C15 C16 1.487(2) . ? C16 C21 1.391(3) . ? C16 C17 1.396(3) . ? C17 C18 1.388(3) . ? C17 H17 0.9500 . ? C18 C19 1.383(4) . ? C18 H18 0.9500 . ? C19 C20 1.382(3) . ? C19 H19 0.9500 . ? C20 C21 1.379(3) . ? C20 H20 0.9500 . ? C22 C23 1.479(3) . ? C23 C28 1.391(3) . ? C23 C24 1.392(3) . ? C24 C25 1.386(3) . ? C24 H24 0.9500 . ? C25 C26 1.381(3) . ? C25 H25 0.9500 . ? C26 C27 1.378(4) . ? C26 H26 0.9500 . ? C27 C28 1.377(3) . ? C27 H27 0.9500 . ?