#------------------------------------------------------------------------------ #$Date: 2019-11-07 21:26:15 +0200 (Thu, 07 Nov 2019) $ #$Revision: 223509 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234439.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_7234439 loop_ _publ_author_name 'Wang, Juan' 'Yang, Mingfang' 'Sun, Juan' 'Li, Hui' 'Liu, Jinjin' 'Wang, Qinglun' 'Li, Licun' 'Ma, Yue' 'Zhao, Bin' 'Cheng, Peng' _publ_section_title ; Enhancing the energy barrier of dysprosium(iii) single-molecule magnets by tuning the magnetic interactions through different N-oxide bridging ligands ; _journal_issue 41 _journal_name_full CrystEngComm _journal_page_first 6219 _journal_paper_doi 10.1039/C9CE01378D _journal_volume 21 _journal_year 2019 _chemical_formula_moiety 'C25 H11 F18 Ho N2 O8' _chemical_formula_sum 'C25 H11 F18 Ho N2 O8' _chemical_formula_weight 974.29 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-03-05 deposited with the CCDC. 2019-09-30 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 122.23(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 24.135(5) _cell_length_b 16.538(3) _cell_length_c 19.338(4) _cell_measurement_reflns_used 7992 _cell_measurement_temperature 133.15 _cell_measurement_theta_max 25.0664 _cell_measurement_theta_min 1.9951 _cell_volume 6529(3) _computing_cell_refinement ; CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015) ; _computing_data_collection ; CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015) ; _computing_data_reduction ; CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015) ; _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 133.15 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Rigaku Pilatus 200K' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_unetI/netI 0.0535 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 26629 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.008 _diffrn_reflns_theta_max 25.008 _diffrn_reflns_theta_min 1.654 _exptl_absorpt_coefficient_mu 2.575 _exptl_absorpt_correction_T_max 0.773 _exptl_absorpt_correction_T_min 0.544 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.982 _exptl_crystal_description block _exptl_crystal_F_000 3744 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 2.071 _refine_diff_density_min -1.027 _refine_diff_density_rms 0.125 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 487 _refine_ls_number_reflns 5766 _refine_ls_number_restraints 18 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0482 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0833P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1238 _refine_ls_wR_factor_ref 0.1348 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4463 _reflns_number_total 5766 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ce01378d2.cif _cod_data_source_block shelxl_CCDC3 _cod_depositor_comments 'Adding full bibliography for 7234434--7234439.cif.' _cod_database_code 7234439 _shelx_shelxl_version_number 2014/7 _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 ; shelxl.res created by SHELXL-2014/7 TITL shelxl in C2/c CELL 0.71073 24.135 16.5383 19.3385 90 122.232 90 ZERR 8 0.0048 0.0033 0.0039 0 0.03 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H F Ho N O UNIT 200 88 144 8 16 64 ISOR 0.01 0.02 F5 ISOR 0.01 0.02 F15 ISOR 0.01 0.02 F18 L.S. 15 PLAN 40 FREE F17 F18 FREE F16 F17 FREE F13 F14 FREE F7 F8 FREE F9 F7 FREE F3 F2 FREE F11 F12 BOND fmap 2 acta OMIT -3 50.02 REM REM REM WGHT 0.083300 FVAR 1.48180 HO1 4 0.051193 0.797787 0.099326 11.00000 0.03818 0.05520 = 0.03672 -0.00436 0.02280 -0.00524 O2 6 0.061008 0.691438 0.185067 11.00000 0.06843 0.06206 = 0.04597 0.00007 0.02952 -0.01051 O1 6 -0.036627 0.704979 0.021807 11.00000 0.04716 0.05498 = 0.05310 -0.00716 0.02371 -0.00968 O3 6 0.073346 0.721071 0.015206 11.00000 0.05000 0.07977 = 0.04911 -0.01295 0.02657 0.00223 O6 6 0.103909 0.891363 0.205957 11.00000 0.04243 0.06838 = 0.05466 -0.01465 0.02296 -0.00755 O5 6 0.113375 0.882959 0.067619 11.00000 0.05240 0.08672 = 0.06029 0.00000 0.03320 -0.02184 O4 6 0.161942 0.753536 0.180097 11.00000 0.04867 0.08357 = 0.05589 -0.00383 0.02471 0.00235 C8 1 0.186745 0.693677 0.089299 11.00000 0.05919 0.09503 = 0.07345 -0.00190 0.03628 0.01700 AFIX 43 H8 2 0.220310 0.671366 0.085316 11.00000 -1.20000 AFIX 0 C7 1 0.123603 0.695256 0.021295 11.00000 0.05432 0.06391 = 0.06135 -0.00867 0.03343 0.00665 F11 3 0.282624 0.661379 0.284450 11.00000 0.12105 0.19563 = 0.10274 0.05210 0.01565 0.04958 F3 3 -0.096835 0.512765 -0.045906 11.00000 0.14939 0.07367 = 0.12277 -0.02043 0.01614 -0.02808 C9 1 0.200515 0.725187 0.163667 11.00000 0.05123 0.06297 = 0.06483 0.00536 0.02701 0.00738 F9 3 0.152637 0.602612 -0.049039 11.00000 0.16898 0.21158 = 0.11510 -0.01483 0.07809 0.09990 C1 1 -0.097802 0.592674 -0.046375 11.00000 0.08640 0.07089 = 0.09623 -0.03108 0.03288 -0.02984 F7 3 0.117272 0.715349 -0.102175 11.00000 0.21485 0.17442 = 0.10060 0.00116 0.10928 -0.01786 F6 3 0.146838 0.564821 0.265790 11.00000 0.10675 0.24576 = 0.24647 0.15922 0.04052 0.06822 C10 1 0.270765 0.721028 0.235954 11.00000 0.04440 0.11341 = 0.08531 0.00126 0.01679 0.02338 C6 1 0.113177 0.662000 -0.059222 11.00000 0.08264 0.11718 = 0.06654 -0.00363 0.04596 0.02875 F10 3 0.315082 0.712234 0.215409 11.00000 0.05650 0.34065 = 0.11103 0.01262 0.01779 0.02162 C3 1 -0.001570 0.584395 0.097188 11.00000 0.08396 0.05166 = 0.07302 -0.00285 0.02857 0.00203 AFIX 43 H3 2 -0.006946 0.528559 0.093006 11.00000 -1.20000 AFIX 0 C4 1 0.045676 0.617757 0.171153 11.00000 0.07269 0.06221 = 0.06398 0.00594 0.03313 0.00142 C2 1 -0.041357 0.632097 0.028730 11.00000 0.04803 0.05957 = 0.06701 -0.01369 0.02543 -0.00988 F2 3 -0.153482 0.617624 -0.062090 11.00000 0.05884 0.18177 = 0.21966 -0.08923 0.02798 -0.02862 F8 3 0.054600 0.630416 -0.106187 11.00000 0.11703 0.19926 = 0.11137 -0.08683 0.05884 -0.02242 F5 3 0.086168 0.586019 0.307300 11.00000 0.24329 0.12792 = 0.07514 0.02396 0.06398 -0.00694 C14 1 0.153420 0.935263 0.229993 11.00000 0.04922 0.06529 = 0.06380 -0.01423 0.02160 0.00182 C15 1 0.178715 0.971245 0.314364 11.00000 0.06391 0.07920 = 0.06866 -0.02338 0.01972 -0.00791 F1 3 -0.096648 0.609886 -0.113172 11.00000 0.19986 0.14049 = 0.07622 -0.03309 0.03445 -0.05535 C12 1 0.162349 0.925433 0.112027 11.00000 0.05883 0.07656 = 0.08092 0.00062 0.04063 -0.02070 C13 1 0.184402 0.954345 0.189104 11.00000 0.05565 0.09322 = 0.08145 -0.02188 0.03218 -0.03063 AFIX 43 H13 2 0.221118 0.987615 0.214464 11.00000 -1.20000 AFIX 0 F4 3 0.068454 0.487397 0.231521 11.00000 0.24411 0.06632 = 0.11937 0.02565 0.04346 -0.00510 F13 3 0.164481 0.965375 -0.002591 11.00000 0.16363 0.56180 = 0.09839 -0.00821 0.07223 -0.18975 C11 1 0.199984 0.949755 0.073774 11.00000 0.06552 0.14889 = 0.12917 -0.01599 0.06106 -0.04491 C5 1 0.086692 0.562126 0.243608 11.00000 0.12053 0.07817 = 0.07625 0.00674 0.02640 -0.00609 F15 3 0.237767 0.893742 0.080450 11.00000 0.26689 0.24195 = 0.42151 0.10303 0.30622 0.06001 F12 3 0.287329 0.782765 0.281143 11.00000 0.08510 0.20110 = 0.22759 -0.12244 -0.03756 0.01739 F14 3 0.235600 1.012142 0.101225 11.00000 0.15563 0.20805 = 0.18193 -0.00741 0.10556 -0.10006 F16 3 0.232960 1.013353 0.342603 11.00000 0.14611 0.18813 = 0.11437 -0.06609 0.04540 -0.08938 F17 3 0.196868 0.921370 0.368518 11.00000 0.44057 0.17543 = 0.07130 -0.03649 0.10213 -0.15657 F18 3 0.142037 1.019080 0.315262 11.00000 0.14180 0.38250 = 0.14299 -0.15502 0.01143 0.10072 O8 6 -0.026619 0.843610 0.125592 11.00000 0.04201 0.07097 = 0.05024 -0.00725 0.03086 -0.00871 N2 5 -0.087965 0.816526 0.090773 11.00000 0.03596 0.05299 = 0.04968 0.00093 0.02746 -0.00199 C21 1 -0.130533 0.829939 0.012769 11.00000 0.05540 0.09846 = 0.06420 0.00988 0.04207 -0.01570 AFIX 43 H21 2 -0.116829 0.855933 -0.018224 11.00000 -1.20000 AFIX 0 C23 1 -0.216012 0.763265 0.019059 11.00000 0.04653 0.03910 = 0.05576 0.00358 0.03701 0.00560 C22 1 -0.195374 0.806222 -0.024337 11.00000 0.04658 0.09521 = 0.04640 0.01201 0.02536 -0.01098 AFIX 43 H22 2 -0.225138 0.819333 -0.078785 11.00000 -1.20000 AFIX 0 C25 1 -0.105688 0.778024 0.135721 11.00000 0.04468 0.09837 = 0.05212 0.01890 0.02952 -0.00581 AFIX 43 H25 2 -0.075160 0.768210 0.190734 11.00000 -1.20000 AFIX 0 C24 1 -0.168353 0.752816 0.101689 11.00000 0.04486 0.09655 = 0.06134 0.02778 0.02982 -0.01020 AFIX 43 H24 2 -0.180154 0.727397 0.134881 11.00000 -1.20000 AFIX 0 O7 6 -0.020968 0.875828 -0.015186 11.00000 0.04762 0.06890 = 0.03961 0.00344 0.03115 0.00186 N1 5 -0.017420 0.879899 -0.082299 11.00000 0.04076 0.05941 = 0.03509 0.00647 0.02479 0.00047 C16 1 -0.033379 0.814243 -0.130368 11.00000 0.05500 0.06440 = 0.03802 -0.00634 0.02517 -0.01749 AFIX 43 H16 2 -0.048473 0.767700 -0.118632 11.00000 -1.20000 AFIX 0 C20 1 0.002582 0.948453 -0.098046 11.00000 0.04840 0.05987 = 0.04105 -0.00553 0.02786 -0.00565 AFIX 43 H20 2 0.012878 0.992936 -0.063855 11.00000 -1.20000 AFIX 0 C18 1 -0.004988 0.885553 -0.215005 11.00000 0.03716 0.05027 = 0.03292 0.00124 0.01944 0.00144 C19 1 0.008007 0.953160 -0.166220 11.00000 0.05338 0.05415 = 0.04019 0.00084 0.03236 -0.00487 AFIX 43 H19 2 0.020301 1.001488 -0.178918 11.00000 -1.20000 AFIX 0 C17 1 -0.027197 0.816560 -0.196767 11.00000 0.05787 0.05514 = 0.03667 -0.00617 0.02649 -0.01346 AFIX 43 H17 2 -0.038061 0.771199 -0.230003 11.00000 -1.20000 AFIX 0 HKLF 4 REM shelxl in C2/c REM R1 = 0.0482 for 4463 Fo > 4sig(Fo) and 0.0624 for all 5761 data REM 487 parameters refined using 18 restraints END WGHT 0.0833 0.0000 REM Highest difference peak 2.071, deepest hole -1.027, 1-sigma level 0.125 Q1 1 0.0508 0.6041 0.1031 11.00000 0.05 2.07 Q2 1 0.3470 0.7025 0.1992 11.00000 0.05 1.77 Q3 1 0.1319 0.9591 0.3402 11.00000 0.05 1.37 Q4 1 0.2284 0.9543 0.3695 11.00000 0.05 0.94 Q5 1 0.2960 0.7918 0.2219 11.00000 0.05 0.82 Q6 1 -0.1426 0.5704 0.0015 11.00000 0.05 0.74 Q7 1 0.2723 0.9350 0.1314 11.00000 0.05 0.73 Q8 1 0.1966 0.8901 0.0192 11.00000 0.05 0.72 Q9 1 0.2796 0.7524 0.3002 11.00000 0.05 0.62 Q10 1 0.1507 1.0516 0.2869 11.00000 0.05 0.57 Q11 1 0.1789 0.6825 -0.0507 11.00000 0.05 0.51 Q12 1 0.3100 0.6674 0.2329 11.00000 0.05 0.50 Q13 1 0.1786 1.0458 0.3125 11.00000 0.05 0.47 Q14 1 0.0919 0.7991 0.1201 11.00000 0.05 0.47 Q15 1 0.3463 0.8916 0.1964 11.00000 0.05 0.43 Q16 1 0.2059 0.7955 0.2159 11.00000 0.05 0.42 Q17 1 0.0256 0.7863 0.1491 11.00000 0.05 0.41 Q18 1 0.1917 1.0036 0.0325 11.00000 0.05 0.41 Q19 1 0.0310 0.7960 0.0182 11.00000 0.05 0.40 Q20 1 -0.0924 0.6973 0.0995 11.00000 0.05 0.39 Q21 1 0.1089 0.5190 0.2105 11.00000 0.05 0.38 Q22 1 -0.1275 0.6354 -0.0921 11.00000 0.05 0.37 Q23 1 0.0494 0.7030 0.0209 11.00000 0.05 0.37 Q24 1 0.0860 0.7626 0.0612 11.00000 0.05 0.37 Q25 1 0.0885 0.5834 0.4094 11.00000 0.05 0.36 Q26 1 -0.0224 0.5553 0.1271 11.00000 0.05 0.36 Q27 1 0.1259 0.7783 -0.0924 11.00000 0.05 0.34 Q28 1 0.0864 0.8232 0.0599 11.00000 0.05 0.34 Q29 1 0.0551 1.0371 -0.0192 11.00000 0.05 0.33 Q30 1 -0.1462 0.8588 0.0085 11.00000 0.05 0.33 Q31 1 -0.0048 0.8005 0.0751 11.00000 0.05 0.32 Q32 1 -0.0706 0.7086 -0.2221 11.00000 0.05 0.32 Q33 1 0.0611 0.6191 0.0387 11.00000 0.05 0.31 Q34 1 0.0022 0.7187 -0.0708 11.00000 0.05 0.31 Q35 1 0.3264 0.9782 0.3043 11.00000 0.05 0.31 Q36 1 -0.1025 0.8950 0.0827 11.00000 0.05 0.30 Q37 1 0.1013 0.8675 0.1135 11.00000 0.05 0.30 Q38 1 0.0477 0.7030 0.0907 11.00000 0.05 0.30 Q39 1 0.0531 0.6214 0.3041 11.00000 0.05 0.29 Q40 1 -0.1104 0.5196 0.0078 11.00000 0.05 0.29 ; _shelx_res_checksum 70883 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 Ho1 Ho 0.05119(2) 0.79779(2) 0.09933(2) 0.04196(14) Uani 1 1 d . . O2 O 0.0610(3) 0.6914(3) 0.1851(3) 0.0593(13) Uani 1 1 d . . O1 O -0.0366(2) 0.7050(3) 0.0218(3) 0.0533(11) Uani 1 1 d . . O3 O 0.0733(2) 0.7211(3) 0.0152(3) 0.0596(12) Uani 1 1 d . . O6 O 0.1039(2) 0.8914(3) 0.2060(3) 0.0566(11) Uani 1 1 d . . O5 O 0.1134(2) 0.8830(3) 0.0676(3) 0.0649(13) Uani 1 1 d . . O4 O 0.1619(2) 0.7535(3) 0.1801(3) 0.0643(13) Uani 1 1 d . . C8 C 0.1867(4) 0.6937(5) 0.0893(5) 0.075(2) Uani 1 1 d . . H8 H 0.2203 0.6714 0.0853 0.091 Uiso 1 1 calc R U C7 C 0.1236(4) 0.6953(4) 0.0213(5) 0.0586(19) Uani 1 1 d . . F11 F 0.2826(4) 0.6614(5) 0.2844(4) 0.162(3) Uani 1 1 d . . F3 F -0.0968(4) 0.5128(3) -0.0459(4) 0.143(3) Uani 1 1 d . . C9 C 0.2005(4) 0.7252(5) 0.1637(5) 0.0616(18) Uani 1 1 d . . F9 F 0.1526(4) 0.6026(5) -0.0490(4) 0.164(3) Uani 1 1 d . . C1 C -0.0978(5) 0.5927(6) -0.0464(6) 0.092(3) Uani 1 1 d . . F7 F 0.1173(5) 0.7153(4) -0.1022(4) 0.151(3) Uani 1 1 d . . F6 F 0.1468(5) 0.5648(7) 0.2658(7) 0.226(6) Uani 1 1 d . . C10 C 0.2708(4) 0.7210(7) 0.2360(6) 0.090(3) Uani 1 1 d . . C6 C 0.1132(5) 0.6620(7) -0.0592(5) 0.086(3) Uani 1 1 d . . F10 F 0.3151(3) 0.7122(6) 0.2154(5) 0.183(4) Uani 1 1 d . . C3 C -0.0016(4) 0.5844(5) 0.0972(5) 0.076(2) Uani 1 1 d . . H3 H -0.0069 0.5286 0.0930 0.091 Uiso 1 1 calc R U C4 C 0.0457(4) 0.6178(5) 0.1712(5) 0.068(2) Uani 1 1 d . . C2 C -0.0414(4) 0.6321(5) 0.0287(4) 0.0608(18) Uani 1 1 d . . F2 F -0.1535(3) 0.6176(5) -0.0621(6) 0.176(4) Uani 1 1 d . . F8 F 0.0546(4) 0.6304(5) -0.1062(4) 0.144(3) Uani 1 1 d . . F5 F 0.0862(5) 0.5860(4) 0.3073(4) 0.159(3) Uani 1 1 d . U C14 C 0.1534(4) 0.9353(4) 0.2300(4) 0.0637(19) Uani 1 1 d . . C15 C 0.1787(4) 0.9712(6) 0.3144(5) 0.078(2) Uani 1 1 d . . F1 F -0.0966(4) 0.6099(4) -0.1132(4) 0.158(3) Uani 1 1 d . . C12 C 0.1623(4) 0.9254(5) 0.1120(5) 0.070(2) Uani 1 1 d . . C13 C 0.1844(4) 0.9543(5) 0.1891(5) 0.079(2) Uani 1 1 d . . H13 H 0.2211 0.9876 0.2145 0.095 Uiso 1 1 calc R U F4 F 0.0685(4) 0.4874(4) 0.2315(4) 0.170(4) Uani 1 1 d . . F13 F 0.1645(5) 0.9654(10) -0.0026(5) 0.273(8) Uani 1 1 d . . C11 C 0.2000(5) 0.9498(8) 0.0738(8) 0.110(4) Uani 1 1 d . . C5 C 0.0867(6) 0.5621(6) 0.2436(6) 0.105(4) Uani 1 1 d . . F15 F 0.2378(6) 0.8937(7) 0.0805(9) 0.249(6) Uani 1 1 d . U F12 F 0.2873(4) 0.7828(6) 0.2811(7) 0.231(6) Uani 1 1 d . . F14 F 0.2356(4) 1.0121(5) 0.1012(5) 0.174(4) Uani 1 1 d . . F16 F 0.2330(4) 1.0134(5) 0.3426(4) 0.161(3) Uani 1 1 d . . F17 F 0.1969(7) 0.9214(5) 0.3685(4) 0.246(7) Uani 1 1 d . . F18 F 0.1420(4) 1.0191(8) 0.3153(5) 0.254(6) Uani 1 1 d . U O8 O -0.0266(2) 0.8436(3) 0.1256(3) 0.0513(11) Uani 1 1 d . . N2 N -0.0880(3) 0.8165(3) 0.0908(3) 0.0439(12) Uani 1 1 d . . C21 C -0.1305(4) 0.8299(5) 0.0128(5) 0.068(2) Uani 1 1 d . . H21 H -0.1168 0.8559 -0.0182 0.081 Uiso 1 1 calc R U C23 C -0.2160(3) 0.7633(3) 0.0191(4) 0.0423(13) Uani 1 1 d . . C22 C -0.1954(4) 0.8062(4) -0.0243(4) 0.062(2) Uani 1 1 d . . H22 H -0.2251 0.8193 -0.0788 0.075 Uiso 1 1 calc R U C25 C -0.1057(4) 0.7780(5) 0.1357(4) 0.063(2) Uani 1 1 d . . H25 H -0.0752 0.7682 0.1907 0.076 Uiso 1 1 calc R U C24 C -0.1684(3) 0.7528(5) 0.1017(4) 0.067(2) Uani 1 1 d . . H24 H -0.1802 0.7274 0.1349 0.080 Uiso 1 1 calc R U O7 O -0.0210(2) 0.8758(3) -0.0152(2) 0.0481(10) Uani 1 1 d . . N1 N -0.0174(2) 0.8799(3) -0.0823(3) 0.0428(12) Uani 1 1 d . . C16 C -0.0334(4) 0.8142(4) -0.1304(4) 0.0523(16) Uani 1 1 d . . H16 H -0.0485 0.7677 -0.1186 0.063 Uiso 1 1 calc R U C20 C 0.0026(3) 0.9485(4) -0.0980(4) 0.0478(15) Uani 1 1 d . . H20 H 0.0129 0.9929 -0.0639 0.057 Uiso 1 1 calc R U C18 C -0.0050(3) 0.8856(4) -0.2150(3) 0.0397(13) Uani 1 1 d . . C19 C 0.0080(3) 0.9532(4) -0.1662(3) 0.0456(15) Uani 1 1 d . . H19 H 0.0203 1.0015 -0.1789 0.055 Uiso 1 1 calc R U C17 C -0.0272(3) 0.8166(4) -0.1968(4) 0.0493(16) Uani 1 1 d . . H17 H -0.0381 0.7712 -0.2300 0.059 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.0382(2) 0.0552(2) 0.03672(19) -0.00436(12) 0.02280(15) -0.00524(12) O2 0.068(4) 0.062(3) 0.046(3) 0.000(2) 0.030(3) -0.011(2) O1 0.047(3) 0.055(3) 0.053(3) -0.007(2) 0.024(2) -0.010(2) O3 0.050(3) 0.080(3) 0.049(3) -0.013(2) 0.027(2) 0.002(2) O6 0.042(3) 0.068(3) 0.055(3) -0.015(2) 0.023(2) -0.008(2) O5 0.052(3) 0.087(4) 0.060(3) 0.000(3) 0.033(2) -0.022(3) O4 0.049(3) 0.084(4) 0.056(3) -0.004(2) 0.025(2) 0.002(3) C8 0.059(5) 0.095(6) 0.073(5) -0.002(4) 0.036(5) 0.017(4) C7 0.054(5) 0.064(5) 0.061(4) -0.009(3) 0.033(4) 0.007(3) F11 0.121(6) 0.196(8) 0.103(5) 0.052(5) 0.016(4) 0.050(6) F3 0.149(6) 0.074(4) 0.123(5) -0.020(3) 0.016(4) -0.028(4) C9 0.051(4) 0.063(4) 0.065(5) 0.005(4) 0.027(4) 0.007(3) F9 0.169(7) 0.212(7) 0.115(5) -0.015(5) 0.078(5) 0.100(6) C1 0.086(7) 0.071(6) 0.096(7) -0.031(5) 0.033(6) -0.030(5) F7 0.215(9) 0.174(6) 0.101(5) 0.001(4) 0.109(6) -0.018(6) F6 0.107(6) 0.246(11) 0.246(11) 0.159(9) 0.041(7) 0.068(7) C10 0.044(5) 0.113(8) 0.085(7) 0.001(6) 0.017(5) 0.023(5) C6 0.083(7) 0.117(7) 0.067(5) -0.004(5) 0.046(5) 0.029(6) F10 0.057(4) 0.341(13) 0.111(5) 0.013(6) 0.018(4) 0.022(5) C3 0.084(6) 0.052(4) 0.073(5) -0.003(4) 0.029(5) 0.002(4) C4 0.073(5) 0.062(5) 0.064(4) 0.006(4) 0.033(4) 0.001(4) C2 0.048(4) 0.060(5) 0.067(5) -0.014(4) 0.025(4) -0.010(3) F2 0.059(4) 0.182(7) 0.220(9) -0.089(6) 0.028(5) -0.029(4) F8 0.117(5) 0.199(7) 0.111(5) -0.087(5) 0.059(4) -0.022(5) F5 0.243(9) 0.128(5) 0.075(4) 0.024(4) 0.064(5) -0.007(5) C14 0.049(4) 0.065(5) 0.064(4) -0.014(4) 0.022(4) 0.002(4) C15 0.064(5) 0.079(6) 0.069(5) -0.023(5) 0.020(4) -0.008(5) F1 0.200(9) 0.140(6) 0.076(4) -0.033(4) 0.034(5) -0.055(6) C12 0.059(5) 0.077(5) 0.081(5) 0.001(4) 0.041(4) -0.021(4) C13 0.056(5) 0.093(6) 0.081(6) -0.022(5) 0.032(4) -0.031(4) F4 0.244(10) 0.066(4) 0.119(5) 0.026(3) 0.043(6) -0.005(5) F13 0.164(9) 0.56(2) 0.098(5) -0.008(9) 0.072(6) -0.190(12) C11 0.066(7) 0.149(10) 0.129(10) -0.016(8) 0.061(7) -0.045(7) C5 0.121(10) 0.078(7) 0.076(7) 0.007(5) 0.026(6) -0.006(6) F15 0.267(10) 0.242(10) 0.422(14) 0.103(9) 0.306(11) 0.060(8) F12 0.085(6) 0.201(8) 0.228(10) -0.122(8) -0.038(6) 0.017(5) F14 0.156(7) 0.208(8) 0.182(7) -0.007(6) 0.106(6) -0.100(6) F16 0.146(7) 0.188(7) 0.114(5) -0.066(5) 0.045(5) -0.089(6) F17 0.441(18) 0.175(7) 0.071(4) -0.036(5) 0.102(7) -0.157(10) F18 0.142(7) 0.383(12) 0.143(6) -0.155(8) 0.011(5) 0.101(8) O8 0.042(3) 0.071(3) 0.050(2) -0.007(2) 0.031(2) -0.009(2) N2 0.036(3) 0.053(3) 0.050(3) 0.001(2) 0.027(3) -0.002(2) C21 0.055(5) 0.098(6) 0.064(5) 0.010(4) 0.042(4) -0.016(4) C23 0.047(4) 0.039(3) 0.056(4) 0.004(3) 0.037(3) 0.006(3) C22 0.047(4) 0.095(6) 0.046(4) 0.012(3) 0.025(3) -0.011(4) C25 0.045(4) 0.098(5) 0.052(4) 0.019(4) 0.030(3) -0.006(4) C24 0.045(4) 0.097(6) 0.061(4) 0.028(4) 0.030(4) -0.010(4) O7 0.048(3) 0.069(3) 0.040(2) 0.003(2) 0.031(2) 0.002(2) N1 0.041(3) 0.059(3) 0.035(2) 0.006(2) 0.025(2) 0.000(2) C16 0.055(4) 0.064(4) 0.038(3) -0.006(3) 0.025(3) -0.017(3) C20 0.048(4) 0.060(4) 0.041(3) -0.006(3) 0.028(3) -0.006(3) C18 0.037(3) 0.050(4) 0.033(3) 0.001(3) 0.019(3) 0.001(3) C19 0.053(4) 0.054(4) 0.040(3) 0.001(3) 0.032(3) -0.005(3) C17 0.058(4) 0.055(4) 0.037(3) -0.006(3) 0.026(3) -0.013(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_3 O8 Ho1 O6 73.37(15) . O8 Ho1 O3 147.35(16) . O6 Ho1 O3 138.92(17) . O8 Ho1 O2 83.00(17) . O6 Ho1 O2 94.06(17) . O3 Ho1 O2 96.36(17) . O8 Ho1 O7 75.31(14) . O6 Ho1 O7 104.45(16) . O3 Ho1 O7 88.39(15) . O2 Ho1 O7 145.77(17) . O8 Ho1 O5 124.21(17) . O6 Ho1 O5 73.29(17) . O3 Ho1 O5 74.38(19) . O2 Ho1 O5 142.43(19) . O7 Ho1 O5 71.43(16) . O8 Ho1 O4 135.55(15) . O6 Ho1 O4 74.48(17) . O3 Ho1 O4 72.32(17) . O2 Ho1 O4 69.53(18) . O7 Ho1 O4 142.95(16) . O5 Ho1 O4 72.99(18) . O8 Ho1 O1 78.24(16) . O6 Ho1 O1 149.55(16) . O3 Ho1 O1 70.76(17) . O2 Ho1 O1 71.49(17) . O7 Ho1 O1 78.31(16) . O5 Ho1 O1 133.89(16) . O4 Ho1 O1 121.61(16) . C4 O2 Ho1 131.9(5) . C2 O1 Ho1 131.8(5) . C7 O3 Ho1 134.5(5) . C14 O6 Ho1 132.2(5) . C12 O5 Ho1 131.2(5) . C9 O4 Ho1 133.6(5) . C7 C8 C9 120.6(8) . O3 C7 C8 128.8(7) . O3 C7 C6 113.9(7) . C8 C7 C6 117.2(7) . O4 C9 C8 127.9(8) . O4 C9 C10 114.1(7) . C8 C9 C10 117.9(8) . F2 C1 F3 109.7(9) . F2 C1 F1 105.2(10) . F3 C1 F1 102.1(8) . F2 C1 C2 112.6(8) . F3 C1 C2 114.9(9) . F1 C1 C2 111.4(8) . F12 C10 F11 104.5(11) . F12 C10 F10 106.6(11) . F11 C10 F10 103.4(9) . F12 C10 C9 112.7(8) . F11 C10 C9 114.3(10) . F10 C10 C9 114.2(9) . F7 C6 F9 108.7(9) . F7 C6 F8 105.0(9) . F9 C6 F8 103.5(9) . F7 C6 C7 113.0(9) . F9 C6 C7 113.7(8) . F8 C6 C7 112.1(8) . C4 C3 C2 121.8(7) . O2 C4 C3 126.4(7) . O2 C4 C5 114.6(7) . C3 C4 C5 119.0(7) . O1 C2 C3 127.2(7) . O1 C2 C1 114.1(7) . C3 C2 C1 118.7(7) . O6 C14 C13 128.1(7) . O6 C14 C15 112.4(7) . C13 C14 C15 119.5(7) . F18 C15 F17 111.5(12) . F18 C15 F16 103.0(10) . F17 C15 F16 100.3(9) . F18 C15 C14 113.4(8) . F17 C15 C14 114.3(8) . F16 C15 C14 113.1(8) . O5 C12 C13 128.4(7) . O5 C12 C11 114.4(8) . C13 C12 C11 117.1(8) . C12 C13 C14 121.7(7) . F15 C11 F14 105.3(11) . F15 C11 F13 105.7(13) . F14 C11 F13 101.9(11) . F15 C11 C12 110.4(11) . F14 C11 C12 117.8(11) . F13 C11 C12 114.5(9) . F6 C5 F4 108.1(12) . F6 C5 F5 104.8(11) . F4 C5 F5 106.7(11) . F6 C5 C4 110.7(10) . F4 C5 C4 114.9(9) . F5 C5 C4 111.0(10) . N2 O8 Ho1 126.1(3) . C21 N2 C25 120.5(6) . C21 N2 O8 120.0(5) . C25 N2 O8 119.4(5) . N2 C21 C22 121.5(6) . C22 C23 C24 114.6(6) . C22 C23 C23 121.3(7) 7_465 C24 C23 C23 123.9(7) 7_465 C23 C22 C21 120.3(7) . N2 C25 C24 119.9(6) . C25 C24 C23 122.9(6) . N1 O7 Ho1 122.8(3) . C20 N1 C16 122.4(5) . C20 N1 O7 118.7(5) . C16 N1 O7 118.9(5) . N1 C16 C17 119.4(6) . N1 C20 C19 119.5(6) . C17 C18 C19 118.0(5) . C17 C18 C18 120.1(4) 2_554 C19 C18 C18 121.9(4) 2_554 C18 C19 C20 119.8(5) . C16 C17 C18 120.8(6) . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ho1 O8 2.319(4) . Ho1 O6 2.338(4) . Ho1 O3 2.339(5) . Ho1 O2 2.341(4) . Ho1 O7 2.343(4) . Ho1 O5 2.365(4) . Ho1 O4 2.380(5) . Ho1 O1 2.389(4) . O2 C4 1.260(8) . O1 C2 1.225(8) . O3 C7 1.231(9) . O6 C14 1.256(8) . O5 C12 1.243(8) . O4 C9 1.226(8) . C8 C7 1.384(11) . C8 C9 1.393(11) . C7 C6 1.540(11) . F11 C10 1.284(12) . F3 C1 1.322(10) . C9 C10 1.518(11) . F9 C6 1.308(10) . C1 F2 1.278(12) . C1 F1 1.337(12) . C1 C2 1.510(10) . F7 C6 1.251(11) . F6 C5 1.276(15) . C10 F12 1.262(12) . C10 F10 1.333(12) . C6 F8 1.314(11) . C3 C4 1.382(10) . C3 C2 1.393(10) . C4 C5 1.520(12) . F5 C5 1.300(13) . C14 C13 1.384(11) . C14 C15 1.525(10) . C15 F18 1.194(11) . C15 F17 1.216(11) . C15 F16 1.317(11) . C12 C13 1.374(11) . C12 C11 1.500(12) . F4 C5 1.291(11) . F13 C11 1.278(14) . C11 F15 1.257(15) . C11 F14 1.264(12) . O8 N2 1.335(6) . N2 C21 1.314(9) . N2 C25 1.319(8) . C21 C22 1.386(10) . C23 C22 1.379(9) . C23 C24 1.395(9) . C23 C23 1.462(12) 7_465 C25 C24 1.354(9) . O7 N1 1.347(5) . N1 C20 1.330(8) . N1 C16 1.345(8) . C16 C17 1.370(9) . C20 C19 1.395(8) . C18 C17 1.384(8) . C18 C19 1.387(8) . C18 C18 1.496(10) 2_554