#------------------------------------------------------------------------------ #$Date: 2020-08-20 04:50:52 +0300 (Thu, 20 Aug 2020) $ #$Revision: 255469 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705221.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_7705221 loop_ _publ_author_name 'Boreen, Michael A.' 'Gro\&s, Oliver A.' 'Hohloch, Stephan' 'Arnold, John' _publ_section_title ; Isocyanide adducts of tri- and tetravalent uranium metallocenes supported by tetra(isopropyl)cyclopentadienyl ligands ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02005B _journal_year 2020 _chemical_formula_moiety 'C54 H94 N4 U, 2(B C24 F20)' _chemical_formula_sum 'C102 H94 B2 F40 N4 U' _chemical_formula_weight 2395.46 _chemical_name_systematic 'Bis(1,2,3,4-tetrakis(iso-propyl)cyclopentadienyl)-tetrakis(tert-butyl-isocyano)-uranium(iv) bis(tetrakis(pentafluorophenyl)borate)' _chemical_properties_physical Air-sensitive,Moisture-sensitive,Oxygen-sensitive _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 geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_creation_date 2020-04-23 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-05-28 deposited with the CCDC. 2020-08-11 downloaded from the CCDC. ; _cell_angle_alpha 105.1690(10) _cell_angle_beta 111.9920(10) _cell_angle_gamma 95.6830(10) _cell_formula_units_Z 1 _cell_length_a 13.9587(3) _cell_length_b 13.9699(6) _cell_length_c 16.9802(4) _cell_measurement_reflns_used 9923 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 24.05 _cell_measurement_theta_min 2.18 _cell_volume 2890.57(16) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution SHELXT-2014 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.366 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_unetI/netI 0.0480 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 32610 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.349 _diffrn_reflns_theta_min 1.367 _diffrn_source 'microfocus sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.511 _exptl_absorpt_correction_T_max 0.4902 _exptl_absorpt_correction_T_min 0.4300 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.376 _exptl_crystal_description plate _exptl_crystal_F_000 1196 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Diethyl ether/THF (20:1)' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _refine_diff_density_max 6.758 _refine_diff_density_min -0.937 _refine_diff_density_rms 0.153 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 687 _refine_ls_number_reflns 10440 _refine_ls_number_restraints 35 _refine_ls_restrained_S_all 1.092 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0745 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1269P)^2^+5.1210P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1881 _refine_ls_wR_factor_ref 0.1936 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9421 _reflns_number_total 10440 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02005b2.cif _cod_data_source_block mab_iv_007_0ma _cod_original_cell_volume 2890.56(16) _cod_database_code 7705221 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints C12 \\sim C14: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(C4) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.1 Uanis(C9) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 3.a Ternary CH refined with riding coordinates: C9(H9), C12(H12), C6(H6), C15(H15) 3.b Aromatic/amide H refined with riding coordinates: C1(H1) 3.c Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C27(H27A,H27B, H27C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C20(H20A, H20B,H20C), C25(H25A,H25B,H25C), C7(H7A,H7B,H7C), C21(H21A,H21B,H21C), C8(H8A, H8B,H8C), C26(H26A,H26B,H26C), C16(H16A,H16B,H16C) ; _shelx_res_file ; mab_iv_007_0ma.res created by SHELXL-2014/7 TITL mab_iv_007_0ma_a.res in P-1 REM Old TITL MAB_IV_007_0ma in P-1 REM SHELXT solution in P-1 REM R1 0.149, Rweak 0.079, Alpha 0.053, Orientation as input REM Formula found by SHELXT: C102 B4 N6 F40 U CELL 0.71073 13.9587 13.9699 16.9802 105.169 111.992 95.683 ZERR 1 0.0003 0.0006 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H B F N U UNIT 102 94 2 40 4 1 SIMU C12 C14 ISOR 0.03 0.1 C4 ISOR 0.01 0.02 C9 C13 L.S. 8 PLAN 20 TEMP -173(2) list 4 more -1 ABIN BUMP fmap 2 acta SHEL 1000 0.83 REM REM REM WGHT 0.126900 5.121000 FVAR 0.31846 U1 6 0.500000 1.000000 0.500000 10.50000 0.04170 0.02885 = 0.04922 0.00702 0.02142 0.00755 F6 4 0.735812 0.206669 0.253750 11.00000 0.05266 0.04026 = 0.04868 0.01973 0.01350 0.01180 F15 4 0.645806 0.558175 0.160384 11.00000 0.04014 0.04540 = 0.05311 0.02390 0.01573 0.01887 F20 4 0.798978 0.412650 0.389086 11.00000 0.06775 0.04338 = 0.04072 0.01740 0.01257 0.01999 F10 4 0.962869 0.438032 0.205100 11.00000 0.03558 0.04045 = 0.06011 0.01350 0.00881 0.00893 F5 4 0.626672 0.213504 0.078656 11.00000 0.05244 0.04281 = 0.04024 0.00711 0.00523 0.00080 F14 4 0.583283 0.600719 0.007462 11.00000 0.05375 0.06466 = 0.06812 0.04130 0.01834 0.02609 F16 4 0.868456 0.616809 0.224327 11.00000 0.04264 0.03697 = 0.05223 0.01025 0.01277 0.00438 F11 4 0.800680 0.302704 0.042675 11.00000 0.05918 0.04193 = 0.04667 0.00975 0.01668 0.01650 F17 4 0.980859 0.765307 0.375251 11.00000 0.04455 0.04300 = 0.07276 0.00212 0.01704 -0.00146 F1 4 0.624744 0.493486 0.306758 11.00000 0.05632 0.04497 = 0.06659 0.02136 0.02833 0.02260 F19 4 0.916743 0.563996 0.541006 11.00000 0.06607 0.06380 = 0.03744 0.00956 0.00521 0.02872 F12 4 0.738080 0.347706 -0.107492 11.00000 0.08843 0.07022 = 0.04561 0.01649 0.03039 0.02217 F7 4 0.883011 0.101564 0.292331 11.00000 0.07273 0.04138 = 0.07792 0.02500 0.01256 0.01882 F18 4 1.009599 0.742833 0.535621 11.00000 0.04817 0.06203 = 0.05297 -0.01186 -0.00043 0.00610 F13 4 0.628910 0.495275 -0.129270 11.00000 0.08135 0.08513 = 0.04573 0.03616 0.01684 0.02073 F2 4 0.426851 0.413411 0.265552 11.00000 0.06046 0.10266 = 0.09793 0.05450 0.04576 0.03253 F4 4 0.426273 0.135405 0.037746 11.00000 0.06225 0.08046 = 0.05422 0.01983 -0.00235 -0.02195 F9 4 1.112139 0.332776 0.248354 11.00000 0.04261 0.06544 = 0.13991 0.04435 0.02341 0.02210 F8 4 1.074366 0.162979 0.293940 11.00000 0.06175 0.06875 = 0.17154 0.06151 0.02510 0.03549 F3 4 0.322353 0.234159 0.130958 11.00000 0.04579 0.14150 = 0.10049 0.05152 0.02010 -0.00934 C40 1 0.729496 0.430736 0.112379 11.00000 0.03146 0.03380 = 0.04092 0.01166 0.00662 0.00148 N1 5 0.333042 0.732608 0.413222 11.00000 0.04779 0.03857 = 0.08805 0.00352 0.04149 0.00299 C28 1 0.638006 0.356970 0.196065 11.00000 0.04129 0.03431 = 0.04320 0.02215 0.00713 0.01129 C34 1 0.839256 0.326921 0.223761 11.00000 0.04109 0.02954 = 0.02899 0.00180 0.00149 0.00597 C45 1 0.672048 0.504316 0.096761 11.00000 0.03571 0.03456 = 0.04105 0.01364 0.01003 0.00540 C35 1 0.825387 0.241170 0.248200 11.00000 0.04381 0.03410 = 0.03643 0.00628 0.00334 0.00945 C47 1 0.874048 0.598227 0.299489 11.00000 0.02866 0.04082 = 0.04160 0.00778 0.00729 0.01634 C41 1 0.749017 0.379659 0.039938 11.00000 0.04169 0.03462 = 0.04511 0.01111 0.00926 0.00458 C51 1 0.842514 0.499157 0.381861 11.00000 0.04222 0.03620 = 0.04532 0.01262 0.00941 0.01931 C44 1 0.638702 0.527471 0.016993 11.00000 0.04031 0.04668 = 0.04954 0.02446 0.01007 0.00786 C46 1 0.823005 0.506232 0.297451 11.00000 0.03137 0.03761 = 0.03781 0.01037 0.00638 0.01698 C39 1 0.938513 0.354372 0.225243 11.00000 0.04597 0.03068 = 0.04621 0.00634 0.00712 0.01184 C48 1 0.935270 0.677686 0.377597 11.00000 0.02837 0.03857 = 0.05805 0.00422 0.01159 0.00968 C29 1 0.581603 0.403721 0.239702 11.00000 0.04700 0.04743 = 0.05261 0.03393 0.01611 0.01967 N2 5 0.511248 0.938174 0.272877 11.00000 0.11293 0.05249 = 0.05634 0.01401 0.03535 -0.00507 C33 1 0.579725 0.266495 0.127779 11.00000 0.04038 0.04702 = 0.03736 0.02073 0.00129 0.00769 C50 1 0.903531 0.576641 0.461899 11.00000 0.04678 0.05490 = 0.03705 0.00759 0.00981 0.02904 C42 1 0.716697 0.400282 -0.040898 11.00000 0.05323 0.04554 = 0.04580 0.00946 0.01743 0.00457 C43 1 0.661793 0.475282 -0.051198 11.00000 0.05296 0.05392 = 0.04221 0.02029 0.01094 0.00548 C18 1 0.386555 0.812053 0.441781 11.00000 0.04083 0.04024 = 0.07007 0.00757 0.02993 0.00978 C30 1 0.476039 0.363118 0.219344 11.00000 0.04835 0.07643 = 0.07427 0.04808 0.03019 0.02466 C49 1 0.950059 0.665569 0.459055 11.00000 0.03199 0.04654 = 0.04477 -0.00161 0.00307 0.01179 C23 1 0.510482 0.955613 0.343229 11.00000 0.06488 0.04209 = 0.05836 0.01863 0.01986 0.00815 C32 1 0.475412 0.224335 0.104836 11.00000 0.05454 0.06174 = 0.04708 0.02924 0.00384 -0.00335 C36 1 0.901557 0.184341 0.269754 11.00000 0.05560 0.03396 = 0.05665 0.01638 0.00291 0.01028 B1 3 0.757475 0.404513 0.206417 11.00000 0.03976 0.03120 = 0.04115 0.01240 0.00777 0.01044 C38 1 1.017623 0.300301 0.247632 11.00000 0.03573 0.04646 = 0.07948 0.01556 0.00607 0.01466 C5 1 0.717766 1.016277 0.600877 11.00000 0.02646 0.04321 = 0.08068 -0.00037 -0.00854 0.01684 C4 1 0.700900 0.962994 0.512125 11.00000 0.02057 0.07042 = 0.07863 0.00743 0.00865 0.02862 C3 1 0.639187 0.865843 0.488567 11.00000 0.02887 0.04724 = 0.09340 -0.01015 0.00124 0.02077 C37 1 0.997388 0.216358 0.270012 11.00000 0.05328 0.04180 = 0.08708 0.02021 0.00769 0.02182 C31 1 0.423850 0.274155 0.150963 11.00000 0.04060 0.08760 = 0.06812 0.04734 0.01238 0.00422 C11 1 0.532393 0.718250 0.339307 11.00000 0.05241 0.07220 = 0.06174 -0.00634 0.00941 0.02983 AFIX 137 H11A 2 0.494651 0.672914 0.358712 11.00000 -1.50000 H11B 2 0.549397 0.677658 0.291757 11.00000 -1.50000 H11C 2 0.487513 0.763153 0.316386 11.00000 -1.50000 AFIX 0 C19 1 0.268060 0.627551 0.378150 11.00000 0.08890 0.04883 = 0.11648 -0.01239 0.06745 -0.02920 C1 1 0.667351 0.954740 0.629951 11.00000 0.06278 0.09935 = 0.07644 0.03942 0.01260 0.04956 AFIX 43 H1 2 0.666978 0.971959 0.687777 11.00000 -1.20000 AFIX 0 C10 1 0.714352 0.719777 0.435857 11.00000 0.05296 0.08624 = 0.15145 -0.04744 -0.00904 0.04163 AFIX 137 H10A 2 0.774968 0.765132 0.489415 11.00000 -1.50000 H10B 2 0.735409 0.699304 0.386027 11.00000 -1.50000 H10C 2 0.690548 0.659290 0.448349 11.00000 -1.50000 AFIX 0 C2 1 0.615218 0.860456 0.560110 11.00000 0.04553 0.05709 = 0.18487 0.06562 0.02356 0.03048 C22 1 0.172929 0.631091 0.394260 11.00000 0.09204 0.07072 = 0.18634 0.02472 0.09244 -0.00637 AFIX 137 H22A 2 0.192735 0.656484 0.459026 11.00000 -1.50000 H22B 2 0.127642 0.562633 0.368833 11.00000 -1.50000 H22C 2 0.134360 0.676539 0.365768 11.00000 -1.50000 AFIX 0 C27 1 0.505661 0.813594 0.146493 11.00000 0.15597 0.10107 = 0.05267 0.01188 0.03648 0.02114 AFIX 137 H27A 2 0.563511 0.790019 0.185162 11.00000 -1.50000 H27B 2 0.508861 0.802600 0.088196 11.00000 -1.50000 H27C 2 0.437633 0.775523 0.137813 11.00000 -1.50000 AFIX 0 C24 1 0.515682 0.917934 0.187158 11.00000 0.21544 0.07000 = 0.05937 0.00275 0.06062 -0.03886 C14 1 0.754050 1.100141 0.446228 11.00000 0.10443 0.09878 = 0.14481 0.01349 0.09215 0.00278 AFIX 137 H14A 2 0.681134 1.109645 0.426271 11.00000 -1.50000 H14B 2 0.781456 1.107107 0.402175 11.00000 -1.50000 H14C 2 0.798367 1.151606 0.504530 11.00000 -1.50000 AFIX 0 C9 1 0.623869 0.775445 0.410497 11.00000 0.08320 0.10359 = 0.14049 -0.02355 0.01298 0.06033 AFIX 13 H9 2 0.650303 0.813329 0.377554 11.00000 -1.20000 AFIX 0 C12 1 0.755797 1.000629 0.454589 11.00000 0.03659 0.17794 = 0.15853 -0.00724 0.04660 0.03105 AFIX 13 H12 2 0.717515 0.951982 0.392070 11.00000 -1.20000 AFIX 0 C13 1 0.871396 0.978580 0.491067 11.00000 0.06036 0.18396 = 0.20540 0.01565 0.07451 0.05186 AFIX 137 H13A 2 0.918493 1.034975 0.544994 11.00000 -1.50000 H13B 2 0.898547 0.971785 0.444817 11.00000 -1.50000 H13C 2 0.868343 0.915401 0.505854 11.00000 -1.50000 AFIX 0 C6 1 0.572270 0.768718 0.581651 11.00000 0.09424 0.10167 = 0.23928 0.11223 0.02844 0.03492 AFIX 13 H6 2 0.520987 0.715685 0.524586 11.00000 -1.20000 AFIX 0 C17 1 0.761807 1.155294 0.758400 11.00000 0.12586 0.09292 = 0.13408 -0.07533 -0.05605 0.06006 AFIX 137 H17A 2 0.690402 1.167202 0.731735 11.00000 -1.50000 H17B 2 0.810806 1.219590 0.800327 11.00000 -1.50000 H17C 2 0.761122 1.106625 0.790677 11.00000 -1.50000 AFIX 0 C20 1 0.267744 0.575889 0.294274 11.00000 0.20532 0.07055 = 0.16468 -0.05634 0.13049 -0.06740 AFIX 137 H20A 2 0.227275 0.605262 0.249170 11.00000 -1.50000 H20B 2 0.235023 0.503695 0.275881 11.00000 -1.50000 H20C 2 0.340715 0.582964 0.299736 11.00000 -1.50000 AFIX 0 C25 1 0.562888 1.006039 0.181138 11.00000 0.30150 0.10504 = 0.12612 0.04393 0.13921 0.00699 AFIX 137 H25A 2 0.550915 1.065150 0.219434 11.00000 -1.50000 H25B 2 0.532006 1.005390 0.118748 11.00000 -1.50000 H25C 2 0.639169 1.009968 0.200969 11.00000 -1.50000 AFIX 0 C7 1 0.517972 0.797463 0.647316 11.00000 0.10558 0.14905 = 0.28622 0.18017 0.07761 0.06436 AFIX 137 H7A 2 0.566441 0.852915 0.701441 11.00000 -1.50000 H7B 2 0.500313 0.738123 0.663873 11.00000 -1.50000 H7C 2 0.453082 0.819392 0.617849 11.00000 -1.50000 AFIX 0 C21 1 0.332833 0.568869 0.445334 11.00000 0.10738 0.07872 = 0.29695 0.09917 0.07700 0.02758 AFIX 137 H21A 2 0.397561 0.559029 0.437336 11.00000 -1.50000 H21B 2 0.288376 0.502588 0.431445 11.00000 -1.50000 H21C 2 0.351523 0.609695 0.507630 11.00000 -1.50000 AFIX 0 C8 1 0.666336 0.723687 0.629607 11.00000 0.15105 0.13927 = 0.22060 0.12428 0.04900 0.07851 AFIX 137 H8A 2 0.698754 0.697039 0.588657 11.00000 -1.50000 H8B 2 0.640427 0.668568 0.647260 11.00000 -1.50000 H8C 2 0.719161 0.777049 0.683152 11.00000 -1.50000 AFIX 0 C15 1 0.801372 1.108120 0.676952 11.00000 0.08850 0.08316 = 0.17650 -0.00176 -0.00057 0.02849 AFIX 13 H15 2 0.814016 1.162524 0.651417 11.00000 -1.20000 AFIX 0 C26 1 0.382494 0.927175 0.117974 11.00000 0.29649 0.17797 = 0.08002 0.04373 0.00923 0.05160 AFIX 137 H26A 2 0.329994 0.875643 0.118578 11.00000 -1.50000 H26B 2 0.374589 0.915875 0.056206 11.00000 -1.50000 H26C 2 0.371523 0.994960 0.142065 11.00000 -1.50000 AFIX 0 C16 1 0.904485 1.075907 0.718185 11.00000 0.09600 0.12199 = 0.21460 -0.04057 -0.04276 0.04189 AFIX 137 H16A 2 0.896189 1.032355 0.753067 11.00000 -1.50000 H16B 2 0.960983 1.136345 0.757710 11.00000 -1.50000 H16C 2 0.922872 1.038220 0.670408 11.00000 -1.50000 AFIX 0 HKLF 4 REM mab_iv_007_0ma_a.res in P-1 REM R1 = 0.0745 for 9421 Fo > 4sig(Fo) and 0.0811 for all 10440 data REM 687 parameters refined using 35 restraints END WGHT 0.1270 5.1109 REM Highest difference peak 6.758, deepest hole -0.937, 1-sigma level 0.153 Q1 1 0.4295 1.0011 0.4584 11.00000 0.05 6.76 Q2 1 0.7103 1.0196 0.7496 11.00000 0.05 1.22 Q3 1 0.6424 0.9355 0.2130 11.00000 0.05 1.05 Q4 1 0.6018 0.7466 0.4447 11.00000 0.05 0.96 Q5 1 0.4873 0.9892 0.4027 11.00000 0.05 0.95 Q6 1 0.1569 0.6447 0.2812 11.00000 0.05 0.88 Q7 1 0.4418 0.9749 0.3304 11.00000 0.05 0.65 Q8 1 0.9055 0.4381 0.1714 11.00000 0.05 0.58 Q9 1 0.2350 0.6178 0.4401 11.00000 0.05 0.54 Q10 1 0.7816 0.9985 0.5832 11.00000 0.05 0.53 Q11 1 0.5796 1.0639 0.4997 11.00000 0.05 0.53 Q12 1 0.7410 0.3213 0.0139 11.00000 0.05 0.52 Q13 1 0.4924 0.9779 0.1429 11.00000 0.05 0.52 Q14 1 0.7491 0.4130 0.3621 11.00000 0.05 0.51 Q15 1 0.8752 0.5775 0.5192 11.00000 0.05 0.50 Q16 1 0.8495 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0.8152 -0.1556 14 -6 3 0.8027 -0.3727 14 -5 0 1.1419 -0.0480 14 -5 1 1.1500 0.0266 14 -5 2 0.0376 0.0933 14 -5 3 -0.3971 -0.0926 14 -5 4 0.6385 -0.2312 14 -4 0 1.4251 -0.0223 14 -4 1 1.7586 0.0335 14 -4 2 0.1641 0.2084 14 -4 3 -1.0294 0.0101 14 -4 4 0.3967 -0.3256 14 -3 0 -0.4339 -0.0343 14 -3 1 0.4100 -0.0350 14 -3 2 -0.1823 0.2546 14 -3 3 -1.3936 0.1893 14 -3 4 -0.5039 -0.2981 14 -2 0 -1.2467 -0.1064 14 -2 1 -0.9539 -0.1507 14 -2 2 -0.1463 0.1099 14 -2 3 -0.7412 0.1880 14 -1 0 -0.8613 -0.1764 14 -1 1 -0.9398 -0.3099 14 -1 2 -0.4015 -0.1222 14 -1 3 0.0052 0.4217 14 0 0 -2.4649 -0.0695 14 0 1 -1.5390 -0.0638 14 0 2 -1.1571 -0.1139 14 1 0 -0.9393 0.1133 14 1 1 -0.4862 0.1622 14 1 2 0.5088 -0.2398 14 2 0 -0.2336 0.2771 14 2 1 -0.7775 0.5015 14 3 0 -0.7265 -0.2966 15 -7 0 1.0889 0.1420 15 -6 0 -0.0229 0.3153 15 -6 1 1.8519 -0.1482 15 -5 0 0.1512 0.5404 15 -5 1 1.5728 0.1977 15 -4 0 1.3883 0.3506 15 -4 1 2.0575 0.1260 15 -3 0 -1.2630 0.1428 15 -3 1 -0.4595 -0.0374 15 -2 0 -0.7979 0.2348 15 -2 1 -0.5846 -0.2092 15 -1 0 -1.0744 0.3863 15 -1 1 -1.4224 -0.0365 15 0 0 -1.2858 0.6486 0 0 0 0.0 0.0 ; _shelx_fab_checksum 11018 _olex2_submission_special_instructions 'No special instructions were received' 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 U1 U 0.5000 1.0000 0.5000 0.04035(15) Uani 1 2 d S T P . . F6 F 0.7358(3) 0.2067(3) 0.2538(3) 0.0484(9) Uani 1 1 d . . . . . F15 F 0.6458(3) 0.5582(3) 0.1604(3) 0.0450(9) Uani 1 1 d . . . . . F20 F 0.7990(3) 0.4126(3) 0.3891(3) 0.0524(10) Uani 1 1 d . . . . . F10 F 0.9629(3) 0.4380(3) 0.2051(3) 0.0494(9) Uani 1 1 d . . . . . F5 F 0.6267(3) 0.2135(3) 0.0787(3) 0.0517(10) Uani 1 1 d . . . . . F14 F 0.5833(3) 0.6007(3) 0.0075(3) 0.0592(11) Uani 1 1 d . . . . . F16 F 0.8685(3) 0.6168(3) 0.2243(3) 0.0474(9) Uani 1 1 d . . . . . F11 F 0.8007(3) 0.3027(3) 0.0427(3) 0.0515(10) Uani 1 1 d . . . . . F17 F 0.9809(3) 0.7653(3) 0.3753(3) 0.0601(11) Uani 1 1 d . . . . . F1 F 0.6247(3) 0.4935(3) 0.3068(3) 0.0535(10) Uani 1 1 d . . . . . F19 F 0.9167(4) 0.5640(3) 0.5410(3) 0.0612(12) Uani 1 1 d . . . . . F12 F 0.7381(4) 0.3477(4) -0.1075(3) 0.0674(12) Uani 1 1 d . . . . . F7 F 0.8830(4) 0.1016(3) 0.2923(3) 0.0683(13) Uani 1 1 d . . . . . F18 F 1.0096(3) 0.7428(4) 0.5356(3) 0.0681(13) Uani 1 1 d . . . . . F13 F 0.6289(4) 0.4953(4) -0.1293(3) 0.0704(13) Uani 1 1 d . . . . . F2 F 0.4269(4) 0.4134(5) 0.2656(4) 0.0772(15) Uani 1 1 d . . . . . F4 F 0.4263(4) 0.1354(4) 0.0377(3) 0.0774(15) Uani 1 1 d . . . . . F9 F 1.1121(4) 0.3328(4) 0.2484(4) 0.0841(17) Uani 1 1 d . . . . . F8 F 1.0744(4) 0.1630(4) 0.2939(5) 0.102(2) Uani 1 1 d . . . . . F3 F 0.3224(4) 0.2342(6) 0.1310(4) 0.099(2) Uani 1 1 d . . . . . C40 C 0.7295(5) 0.4307(5) 0.1124(4) 0.0386(14) Uani 1 1 d . . . . . N1 N 0.3330(5) 0.7326(5) 0.4132(5) 0.0581(17) Uani 1 1 d . . . . . C28 C 0.6380(5) 0.3570(5) 0.1961(4) 0.0406(15) Uani 1 1 d . . . . . C34 C 0.8393(5) 0.3269(5) 0.2238(4) 0.0391(14) Uani 1 1 d . . . . . C45 C 0.6720(5) 0.5043(5) 0.0968(4) 0.0389(14) Uani 1 1 d . . . . . C35 C 0.8254(5) 0.2412(5) 0.2482(4) 0.0433(15) Uani 1 1 d . . . . . C47 C 0.8740(5) 0.5982(5) 0.2995(4) 0.0398(15) Uani 1 1 d . . . . . C41 C 0.7490(5) 0.3797(5) 0.0399(5) 0.0439(15) Uani 1 1 d . . . . . C51 C 0.8425(5) 0.4992(5) 0.3819(5) 0.0433(15) Uani 1 1 d . . . . . C44 C 0.6387(5) 0.5275(5) 0.0170(5) 0.0465(16) Uani 1 1 d . . . . . C46 C 0.8230(5) 0.5062(5) 0.2975(4) 0.0378(14) Uani 1 1 d . . . . . C39 C 0.9385(5) 0.3544(5) 0.2252(5) 0.0458(16) Uani 1 1 d . . . . . C48 C 0.9353(5) 0.6777(5) 0.3776(5) 0.0459(17) Uani 1 1 d . . . . . C29 C 0.5816(5) 0.4037(5) 0.2397(5) 0.0460(16) Uani 1 1 d . . . . . N2 N 0.5112(7) 0.9382(6) 0.2729(5) 0.076(2) Uani 1 1 d . . . . . C33 C 0.5797(5) 0.2665(5) 0.1278(5) 0.0449(16) Uani 1 1 d . . . . . C50 C 0.9035(6) 0.5766(6) 0.4619(5) 0.0488(17) Uani 1 1 d . . . . . C42 C 0.7167(6) 0.4003(6) -0.0409(5) 0.0508(17) Uani 1 1 d . . . . . C43 C 0.6618(6) 0.4753(6) -0.0512(5) 0.0520(18) Uani 1 1 d . . . . . C18 C 0.3866(5) 0.8121(5) 0.4418(5) 0.0503(18) Uani 1 1 d . . . . . C30 C 0.4760(6) 0.3631(7) 0.2193(6) 0.059(2) Uani 1 1 d . . . . . C49 C 0.9501(5) 0.6656(5) 0.4591(5) 0.0484(17) Uani 1 1 d . . . . . C23 C 0.5105(6) 0.9556(6) 0.3432(6) 0.0567(19) Uani 1 1 d . . . . . C32 C 0.4754(6) 0.2243(6) 0.1048(5) 0.059(2) Uani 1 1 d . . . . . C36 C 0.9016(6) 0.1843(5) 0.2698(5) 0.0548(19) Uani 1 1 d . . . . . B1 B 0.7575(6) 0.4045(5) 0.2064(5) 0.0399(16) Uani 1 1 d . . . . . C38 C 1.0176(6) 0.3003(6) 0.2476(6) 0.060(2) Uani 1 1 d . . . . . C5 C 0.7178(5) 1.0163(6) 0.6009(6) 0.063(2) Uani 1 1 d . . . . . C4 C 0.7009(5) 0.9630(6) 0.5121(6) 0.062(2) Uani 1 1 d . U . . . C3 C 0.6392(6) 0.8658(6) 0.4886(7) 0.070(3) Uani 1 1 d . . . . . C37 C 0.9974(7) 0.2164(6) 0.2700(7) 0.067(2) Uani 1 1 d . . . . . C31 C 0.4239(6) 0.2742(8) 0.1510(6) 0.065(2) Uani 1 1 d . . . . . C11 C 0.5324(6) 0.7183(7) 0.3393(6) 0.071(3) Uani 1 1 d . . . . . H11A H 0.4947 0.6729 0.3587 0.107 Uiso 1 1 calc GR . . . . H11B H 0.5494 0.6777 0.2918 0.107 Uiso 1 1 calc GR . . . . H11C H 0.4875 0.7632 0.3164 0.107 Uiso 1 1 calc GR . . . . C19 C 0.2681(8) 0.6276(7) 0.3781(8) 0.089(4) Uani 1 1 d . . . . . C1 C 0.6674(7) 0.9547(9) 0.6300(7) 0.080(3) Uani 1 1 d . . . . . H1 H 0.6670 0.9720 0.6878 0.096 Uiso 1 1 calc R . . . . C10 C 0.7144(8) 0.7198(9) 0.4359(10) 0.129(6) Uani 1 1 d . . . . . H10A H 0.7750 0.7651 0.4894 0.194 Uiso 1 1 calc GR . . . . H10B H 0.7354 0.6993 0.3860 0.194 Uiso 1 1 calc GR . . . . H10C H 0.6905 0.6593 0.4483 0.194 Uiso 1 1 calc GR . . . . C2 C 0.6152(7) 0.8605(8) 0.5601(11) 0.096(4) Uani 1 1 d . . . . . C22 C 0.1729(9) 0.6311(9) 0.3943(11) 0.111(5) Uani 1 1 d . . . . . H22A H 0.1927 0.6565 0.4590 0.166 Uiso 1 1 calc GR . . . . H22B H 0.1276 0.5626 0.3688 0.166 Uiso 1 1 calc GR . . . . H22C H 0.1344 0.6765 0.3658 0.166 Uiso 1 1 calc GR . . . . C27 C 0.5057(12) 0.8136(10) 0.1465(7) 0.109(4) Uani 1 1 d . . . . . H27A H 0.5635 0.7900 0.1852 0.163 Uiso 1 1 calc GR . . . . H27B H 0.5089 0.8026 0.0882 0.163 Uiso 1 1 calc GR . . . . H27C H 0.4376 0.7755 0.1378 0.163 Uiso 1 1 calc GR . . . . C24 C 0.5157(14) 0.9179(9) 0.1872(7) 0.123(6) Uani 1 1 d . . . . . C14 C 0.7540(10) 1.1001(10) 0.4462(10) 0.110(4) Uani 1 1 d . U . . . H14A H 0.6811 1.1096 0.4263 0.166 Uiso 1 1 calc GR . . . . H14B H 0.7815 1.1071 0.4022 0.166 Uiso 1 1 calc GR . . . . H14C H 0.7984 1.1516 0.5045 0.166 Uiso 1 1 calc GR . . . . C9 C 0.6239(8) 0.7754(8) 0.4105(10) 0.130(5) Uani 1 1 d . U . . . H9 H 0.6503 0.8133 0.3776 0.156 Uiso 1 1 calc R . . . . C12 C 0.7558(8) 1.0006(11) 0.4546(11) 0.135(6) Uani 1 1 d . U . . . H12 H 0.7175 0.9520 0.3921 0.162 Uiso 1 1 calc R . . . . C13 C 0.8714(9) 0.9786(14) 0.4911(12) 0.152(7) Uani 1 1 d . U . . . H13A H 0.9185 1.0350 0.5450 0.228 Uiso 1 1 calc GR . . . . H13B H 0.8985 0.9718 0.4448 0.228 Uiso 1 1 calc GR . . . . H13C H 0.8683 0.9154 0.5059 0.228 Uiso 1 1 calc GR . . . . C6 C 0.5723(11) 0.7687(12) 0.5817(15) 0.145(7) Uani 1 1 d . . . . . H6 H 0.5210 0.7157 0.5246 0.174 Uiso 1 1 calc R . . . . C17 C 0.7618(11) 1.1553(10) 0.7584(10) 0.173(10) Uani 1 1 d . . . . . H17A H 0.6904 1.1672 0.7317 0.260 Uiso 1 1 calc GR . . . . H17B H 0.8108 1.2196 0.8003 0.260 Uiso 1 1 calc GR . . . . H17C H 0.7611 1.1066 0.7907 0.260 Uiso 1 1 calc GR . . . . C20 C 0.2677(13) 0.5759(9) 0.2943(11) 0.158(8) Uani 1 1 d . . . . . H20A H 0.2273 0.6053 0.2492 0.236 Uiso 1 1 calc GR . . . . H20B H 0.2350 0.5037 0.2759 0.236 Uiso 1 1 calc GR . . . . H20C H 0.3407 0.5830 0.2997 0.236 Uiso 1 1 calc GR . . . . C25 C 0.5629(18) 1.0060(12) 0.1811(11) 0.163(8) Uani 1 1 d . . . . . H25A H 0.5509 1.0652 0.2194 0.245 Uiso 1 1 calc GR . . . . H25B H 0.5320 1.0054 0.1187 0.245 Uiso 1 1 calc GR . . . . H25C H 0.6392 1.0100 0.2010 0.245 Uiso 1 1 calc GR . . . . C7 C 0.5180(11) 0.7975(12) 0.6473(14) 0.156(8) Uani 1 1 d . . . . . H7A H 0.5664 0.8529 0.7014 0.233 Uiso 1 1 calc GR . . . . H7B H 0.5003 0.7381 0.6639 0.233 Uiso 1 1 calc GR . . . . H7C H 0.4531 0.8194 0.6178 0.233 Uiso 1 1 calc GR . . . . C21 C 0.3328(11) 0.5689(10) 0.4453(15) 0.155(8) Uani 1 1 d . . . . . H21A H 0.3976 0.5590 0.4373 0.232 Uiso 1 1 calc GR . . . . H21B H 0.2884 0.5026 0.4314 0.232 Uiso 1 1 calc GR . . . . H21C H 0.3515 0.6097 0.5076 0.232 Uiso 1 1 calc GR . . . . C8 C 0.6663(14) 0.7237(13) 0.6296(14) 0.162(8) Uani 1 1 d . . . . . H8A H 0.6988 0.6970 0.5887 0.243 Uiso 1 1 calc GR . . . . H8B H 0.6404 0.6686 0.6473 0.243 Uiso 1 1 calc GR . . . . H8C H 0.7192 0.7770 0.6832 0.243 Uiso 1 1 calc GR . . . . C15 C 0.8014(10) 1.1081(10) 0.6770(11) 0.142(7) Uani 1 1 d . . . . . H15 H 0.8140 1.1625 0.6514 0.171 Uiso 1 1 calc R . . . . C26 C 0.382(2) 0.9272(17) 0.1180(11) 0.206(11) Uani 1 1 d . . . . . H26A H 0.3300 0.8756 0.1186 0.309 Uiso 1 1 calc GR . . . . H26B H 0.3746 0.9159 0.0562 0.309 Uiso 1 1 calc GR . . . . H26C H 0.3715 0.9950 0.1421 0.309 Uiso 1 1 calc GR . . . . C16 C 0.9045(12) 1.0759(13) 0.7182(14) 0.197(12) Uani 1 1 d . . . . . H16A H 0.8962 1.0324 0.7531 0.295 Uiso 1 1 calc GR . . . . H16B H 0.9610 1.1363 0.7577 0.295 Uiso 1 1 calc GR . . . . H16C H 0.9229 1.0382 0.6704 0.295 Uiso 1 1 calc GR . . . . 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 U1 0.0417(2) 0.0289(2) 0.0492(2) 0.00702(14) 0.02142(17) 0.00755(13) F6 0.053(2) 0.040(2) 0.049(2) 0.0197(17) 0.0135(19) 0.0118(17) F15 0.040(2) 0.045(2) 0.053(2) 0.0239(18) 0.0157(18) 0.0189(16) F20 0.068(3) 0.043(2) 0.041(2) 0.0174(17) 0.0126(19) 0.0200(19) F10 0.0356(19) 0.040(2) 0.060(2) 0.0135(18) 0.0088(18) 0.0089(16) F5 0.052(2) 0.043(2) 0.040(2) 0.0071(17) 0.0052(18) 0.0008(17) F14 0.054(2) 0.065(3) 0.068(3) 0.041(2) 0.018(2) 0.026(2) F16 0.043(2) 0.037(2) 0.052(2) 0.0103(17) 0.0128(18) 0.0044(16) F11 0.059(2) 0.042(2) 0.047(2) 0.0097(17) 0.0167(19) 0.0165(18) F17 0.045(2) 0.043(2) 0.073(3) 0.002(2) 0.017(2) -0.0015(18) F1 0.056(2) 0.045(2) 0.067(3) 0.021(2) 0.028(2) 0.0226(19) F19 0.066(3) 0.064(3) 0.037(2) 0.0096(19) 0.005(2) 0.029(2) F12 0.088(3) 0.070(3) 0.046(2) 0.016(2) 0.030(2) 0.022(3) F7 0.073(3) 0.041(2) 0.078(3) 0.025(2) 0.013(3) 0.019(2) F18 0.048(2) 0.062(3) 0.053(3) -0.012(2) 0.000(2) 0.006(2) F13 0.081(3) 0.085(3) 0.046(3) 0.036(2) 0.017(2) 0.021(3) F2 0.060(3) 0.103(4) 0.098(4) 0.055(3) 0.046(3) 0.033(3) F4 0.062(3) 0.080(3) 0.054(3) 0.020(2) -0.002(2) -0.022(2) F9 0.043(3) 0.065(3) 0.140(5) 0.044(3) 0.023(3) 0.022(2) F8 0.062(3) 0.069(3) 0.172(6) 0.062(4) 0.025(4) 0.035(3) F3 0.046(3) 0.142(6) 0.100(4) 0.052(4) 0.020(3) -0.009(3) C40 0.031(3) 0.034(3) 0.041(4) 0.012(3) 0.007(3) 0.001(2) N1 0.048(3) 0.039(3) 0.088(5) 0.004(3) 0.041(3) 0.003(3) C28 0.041(3) 0.034(3) 0.043(4) 0.022(3) 0.007(3) 0.011(3) C34 0.041(3) 0.030(3) 0.029(3) 0.002(2) 0.001(3) 0.006(3) C45 0.036(3) 0.035(3) 0.041(4) 0.014(3) 0.010(3) 0.005(3) C35 0.044(4) 0.034(3) 0.036(4) 0.006(3) 0.003(3) 0.009(3) C47 0.029(3) 0.041(3) 0.042(4) 0.008(3) 0.007(3) 0.016(3) C41 0.042(4) 0.035(3) 0.045(4) 0.011(3) 0.009(3) 0.005(3) C51 0.042(4) 0.036(3) 0.045(4) 0.013(3) 0.009(3) 0.019(3) C44 0.040(4) 0.047(4) 0.050(4) 0.024(3) 0.010(3) 0.008(3) C46 0.031(3) 0.038(3) 0.038(3) 0.010(3) 0.006(3) 0.017(3) C39 0.046(4) 0.031(3) 0.046(4) 0.006(3) 0.007(3) 0.012(3) C48 0.028(3) 0.039(4) 0.058(5) 0.004(3) 0.012(3) 0.010(3) C29 0.047(4) 0.047(4) 0.053(4) 0.034(3) 0.016(3) 0.020(3) N2 0.113(6) 0.052(4) 0.056(5) 0.014(3) 0.035(4) -0.005(4) C33 0.040(4) 0.047(4) 0.037(4) 0.021(3) 0.001(3) 0.008(3) C50 0.047(4) 0.055(4) 0.037(4) 0.008(3) 0.010(3) 0.029(3) C42 0.053(4) 0.046(4) 0.046(4) 0.009(3) 0.017(3) 0.005(3) C43 0.053(4) 0.054(4) 0.042(4) 0.020(3) 0.011(3) 0.005(3) C18 0.041(4) 0.040(4) 0.070(5) 0.008(3) 0.030(4) 0.010(3) C30 0.048(4) 0.076(6) 0.074(6) 0.048(5) 0.030(4) 0.025(4) C49 0.032(3) 0.047(4) 0.045(4) -0.002(3) 0.003(3) 0.012(3) C23 0.065(5) 0.042(4) 0.058(5) 0.019(4) 0.020(4) 0.008(3) C32 0.055(5) 0.062(5) 0.047(4) 0.029(4) 0.004(4) -0.003(4) C36 0.056(4) 0.034(4) 0.057(5) 0.016(3) 0.003(4) 0.010(3) B1 0.040(4) 0.031(3) 0.041(4) 0.012(3) 0.008(3) 0.010(3) C38 0.036(4) 0.046(4) 0.079(6) 0.016(4) 0.006(4) 0.015(3) C5 0.026(3) 0.043(4) 0.081(6) 0.000(4) -0.009(4) 0.017(3) C4 0.021(3) 0.070(5) 0.079(6) 0.007(4) 0.009(3) 0.029(3) C3 0.029(4) 0.047(4) 0.093(7) -0.010(4) 0.001(4) 0.021(3) C37 0.053(5) 0.042(4) 0.087(6) 0.020(4) 0.008(4) 0.022(3) C31 0.041(4) 0.088(6) 0.068(5) 0.047(5) 0.012(4) 0.004(4) C11 0.052(5) 0.072(6) 0.062(5) -0.006(4) 0.009(4) 0.030(4) C19 0.089(7) 0.049(5) 0.116(8) -0.012(5) 0.067(6) -0.029(5) C1 0.063(6) 0.099(8) 0.076(6) 0.039(6) 0.013(5) 0.050(6) C10 0.053(5) 0.086(8) 0.151(11) -0.047(7) -0.009(6) 0.042(5) C2 0.046(5) 0.057(6) 0.185(13) 0.066(7) 0.024(7) 0.030(4) C22 0.092(8) 0.071(7) 0.186(14) 0.025(8) 0.092(9) -0.006(6) C27 0.156(12) 0.101(9) 0.053(6) 0.012(6) 0.036(7) 0.021(8) C24 0.215(16) 0.070(7) 0.059(6) 0.003(5) 0.061(8) -0.039(8) C14 0.104(9) 0.099(9) 0.145(11) 0.013(8) 0.092(9) 0.003(7) C9 0.083(6) 0.104(7) 0.140(8) -0.024(6) 0.013(5) 0.060(6) C12 0.037(5) 0.178(15) 0.159(13) -0.007(11) 0.047(7) 0.031(7) C13 0.060(6) 0.184(13) 0.205(14) 0.016(10) 0.075(8) 0.052(7) C6 0.094(9) 0.102(10) 0.24(2) 0.112(12) 0.028(11) 0.035(8) C17 0.126(11) 0.093(9) 0.134(12) -0.075(9) -0.056(9) 0.060(8) C20 0.205(16) 0.071(8) 0.165(14) -0.056(8) 0.130(13) -0.067(9) C25 0.30(3) 0.105(11) 0.126(12) 0.044(9) 0.139(15) 0.007(13) C7 0.106(10) 0.149(13) 0.29(2) 0.180(16) 0.078(13) 0.064(10) C21 0.107(10) 0.079(8) 0.30(2) 0.099(12) 0.077(13) 0.028(7) C8 0.151(14) 0.139(14) 0.22(2) 0.124(15) 0.049(14) 0.079(12) C15 0.089(9) 0.083(9) 0.176(15) -0.002(9) -0.001(9) 0.028(7) C26 0.30(3) 0.178(19) 0.080(10) 0.044(11) 0.009(14) 0.052(19) C16 0.096(10) 0.122(13) 0.21(2) -0.041(13) -0.043(12) 0.042(9) 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 '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 C18 U1 C18 180.0(4) 2_676 . ? C18 U1 C5 112.8(2) 2_676 2_676 ? C18 U1 C5 67.2(2) . 2_676 ? C18 U1 C5 112.8(2) . . ? C18 U1 C5 67.2(2) 2_676 . ? C18 U1 C4 78.7(2) 2_676 . ? C18 U1 C4 78.7(2) . 2_676 ? C18 U1 C4 101.3(2) 2_676 2_676 ? C18 U1 C4 101.3(2) . . ? C18 U1 C1 91.4(3) 2_676 2_676 ? C18 U1 C1 91.4(3) . . ? C18 U1 C1 88.6(3) . 2_676 ? C18 U1 C1 88.6(3) 2_676 . ? C18 U1 C2 114.4(3) 2_676 . ? C18 U1 C2 114.4(3) . 2_676 ? C18 U1 C2 65.6(3) . . ? C18 U1 C2 65.6(3) 2_676 2_676 ? C23 U1 C18 86.3(2) . . ? C23 U1 C18 93.7(2) . 2_676 ? C23 U1 C18 93.7(2) 2_676 . ? C23 U1 C18 86.3(2) 2_676 2_676 ? C23 U1 C23 180.0(5) . 2_676 ? C23 U1 C5 84.6(3) . 2_676 ? C23 U1 C5 95.4(3) . . ? C23 U1 C5 95.4(3) 2_676 2_676 ? C23 U1 C5 84.6(3) 2_676 . ? C23 U1 C4 112.1(3) . 2_676 ? C23 U1 C4 112.1(3) 2_676 . ? C23 U1 C4 67.9(3) . . ? C23 U1 C4 67.9(3) 2_676 2_676 ? C23 U1 C1 67.2(3) 2_676 . ? C23 U1 C1 112.8(3) 2_676 2_676 ? C23 U1 C1 112.8(3) . . ? C23 U1 C1 67.2(3) . 2_676 ? C23 U1 C2 83.9(4) . 2_676 ? C23 U1 C2 96.1(4) 2_676 2_676 ? C23 U1 C2 83.9(4) 2_676 . ? C23 U1 C2 96.1(4) . . ? C5 U1 C5 180.0 . 2_676 ? C5 U1 C4 28.8(3) . . ? C5 U1 C4 151.2(3) . 2_676 ? C5 U1 C4 151.2(3) 2_676 . ? C5 U1 C4 28.8(3) 2_676 2_676 ? C4 U1 C4 180.0 2_676 . ? C1 U1 C5 27.9(3) . . ? C1 U1 C5 152.1(3) . 2_676 ? C1 U1 C5 27.9(3) 2_676 2_676 ? C1 U1 C5 152.1(3) 2_676 . ? C1 U1 C4 46.8(3) . . ? C1 U1 C4 133.2(3) 2_676 . ? C1 U1 C4 133.2(3) . 2_676 ? C1 U1 C4 46.8(3) 2_676 2_676 ? C1 U1 C1 180.0(4) 2_676 . ? C2 U1 C5 132.6(3) . 2_676 ? C2 U1 C5 47.4(3) 2_676 2_676 ? C2 U1 C5 47.4(3) . . ? C2 U1 C5 132.6(3) 2_676 . ? C2 U1 C4 47.4(3) 2_676 2_676 ? C2 U1 C4 132.6(3) 2_676 . ? C2 U1 C4 47.4(3) . . ? C2 U1 C4 132.6(3) . 2_676 ? C2 U1 C1 29.3(3) . . ? C2 U1 C1 150.7(3) . 2_676 ? C2 U1 C1 29.3(3) 2_676 2_676 ? C2 U1 C1 150.7(3) 2_676 . ? C2 U1 C2 180.0 . 2_676 ? C45 C40 C41 113.7(6) . . ? C45 C40 B1 119.4(6) . . ? C41 C40 B1 126.6(6) . . ? C18 N1 C19 177.3(9) . . ? C29 C28 C33 113.6(6) . . ? C29 C28 B1 127.2(6) . . ? C33 C28 B1 118.5(6) . . ? C35 C34 C39 114.3(6) . . ? C35 C34 B1 126.7(6) . . ? C39 C34 B1 118.4(6) . . ? F15 C45 C40 120.0(6) . . ? F15 C45 C44 116.2(6) . . ? C40 C45 C44 123.7(7) . . ? F6 C35 C34 122.0(6) . . ? F6 C35 C36 114.1(6) . . ? C34 C35 C36 123.9(7) . . ? F16 C47 C46 122.1(6) . . ? F16 C47 C48 114.0(6) . . ? C48 C47 C46 123.9(7) . . ? F11 C41 C40 121.3(6) . . ? F11 C41 C42 114.4(6) . . ? C40 C41 C42 124.3(6) . . ? F20 C51 C46 119.6(6) . . ? F20 C51 C50 116.1(6) . . ? C50 C51 C46 124.3(7) . . ? F14 C44 C45 119.9(7) . . ? F14 C44 C43 120.5(6) . . ? C43 C44 C45 119.6(7) . . ? C47 C46 B1 125.8(6) . . ? C51 C46 C47 113.8(6) . . ? C51 C46 B1 119.9(6) . . ? F10 C39 C34 120.1(6) . . ? F10 C39 C38 116.3(7) . . ? C34 C39 C38 123.6(7) . . ? F17 C48 C47 121.2(7) . . ? F17 C48 C49 119.8(6) . . ? C49 C48 C47 119.1(7) . . ? F1 C29 C28 121.9(6) . . ? F1 C29 C30 114.6(7) . . ? C28 C29 C30 123.5(7) . . ? C23 N2 C24 178.2(11) . . ? F5 C33 C28 119.2(6) . . ? F5 C33 C32 116.0(7) . . ? C32 C33 C28 124.8(8) . . ? F19 C50 C51 120.4(7) . . ? F19 C50 C49 120.7(6) . . ? C49 C50 C51 118.9(7) . . ? F12 C42 C41 120.8(7) . . ? F12 C42 C43 120.2(7) . . ? C43 C42 C41 119.0(7) . . ? F13 C43 C44 120.6(7) . . ? F13 C43 C42 119.7(7) . . ? C44 C43 C42 119.7(7) . . ? N1 C18 U1 176.1(7) . . ? F2 C30 C29 119.7(8) . . ? F2 C30 C31 120.8(7) . . ? C31 C30 C29 119.4(8) . . ? F18 C49 C48 119.4(7) . . ? F18 C49 C50 120.5(7) . . ? C50 C49 C48 120.0(6) . . ? N2 C23 U1 176.9(7) . . ? F4 C32 C33 120.1(8) . . ? F4 C32 C31 121.1(7) . . ? C31 C32 C33 118.8(8) . . ? F7 C36 C35 121.0(7) . . ? F7 C36 C37 120.6(7) . . ? C37 C36 C35 118.4(7) . . ? C40 B1 C28 101.8(5) . . ? C40 B1 C34 115.1(6) . . ? C40 B1 C46 112.9(5) . . ? C28 B1 C46 113.1(6) . . ? C34 B1 C28 113.2(5) . . ? C34 B1 C46 101.2(5) . . ? F9 C38 C39 119.8(7) . . ? F9 C38 C37 121.7(7) . . ? C37 C38 C39 118.4(7) . . ? C4 C5 U1 76.3(4) . . ? C4 C5 C15 134.6(11) . . ? C1 C5 U1 75.4(4) . . ? C1 C5 C4 108.5(8) . . ? C1 C5 C15 113.9(11) . . ? C15 C5 U1 129.4(6) . . ? C5 C4 U1 74.9(4) . . ? C5 C4 C12 126.1(9) . . ? C3 C4 U1 76.1(4) . . ? C3 C4 C5 107.2(9) . . ? C3 C4 C12 126.2(9) . . ? C12 C4 U1 121.4(6) . . ? C4 C3 U1 75.4(4) . . ? C4 C3 C9 125.7(11) . . ? C2 C3 U1 73.8(4) . . ? C2 C3 C4 108.4(8) . . ? C2 C3 C9 124.4(11) . . ? C9 C3 U1 128.1(6) . . ? C36 C37 F8 119.0(8) . . ? C38 C37 F8 119.6(8) . . ? C38 C37 C36 121.4(7) . . ? F3 C31 C30 120.0(9) . . ? F3 C31 C32 120.2(9) . . ? C32 C31 C30 119.8(7) . . ? N1 C19 C21 105.8(9) . . ? C22 C19 N1 108.6(8) . . ? C22 C19 C21 102.7(11) . . ? C20 C19 N1 109.5(8) . . ? C20 C19 C22 124.0(12) . . ? C20 C19 C21 104.5(13) . . ? C5 C1 U1 76.8(5) . . ? C5 C1 C2 109.1(10) . . ? C2 C1 U1 75.2(5) . . ? C3 C2 U1 77.7(5) . . ? C3 C2 C1 106.7(9) . . ? C3 C2 C6 131.5(14) . . ? C1 C2 U1 75.5(5) . . ? C1 C2 C6 119.5(15) . . ? C6 C2 U1 125.7(7) . . ? N2 C24 C26 100.6(13) . . ? C27 C24 N2 111.7(10) . . ? C27 C24 C26 97.8(12) . . ? C25 C24 N2 109.9(10) . . ? C25 C24 C27 134.1(14) . . ? C25 C24 C26 92.9(15) . . ? C3 C9 C10 110.8(9) . . ? C11 C9 C3 129.3(8) . . ? C11 C9 C10 115.1(8) . . ? C14 C12 C4 120.1(9) . . ? C14 C12 C13 113.9(12) . . ? C13 C12 C4 104.9(12) . . ? C2 C6 C7 113.5(13) . . ? C2 C6 C8 109.0(12) . . ? C8 C6 C7 105.8(15) . . ? C5 C15 C17 111.7(12) . . ? C16 C15 C5 109.7(10) . . ? C16 C15 C17 108.3(14) . . ? 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 U1 C18 2.650(7) 2_676 ? U1 C18 2.650(7) . ? U1 C23 2.634(9) . ? U1 C23 2.634(9) 2_676 ? U1 C5 2.826(6) 2_676 ? U1 C5 2.826(6) . ? U1 C4 2.843(6) . ? U1 C4 2.843(6) 2_676 ? U1 C1 2.809(8) . ? U1 C1 2.809(8) 2_676 ? U1 C2 2.804(8) . ? U1 C2 2.804(8) 2_676 ? F6 C35 1.341(8) . ? F15 C45 1.339(8) . ? F20 C51 1.354(8) . ? F10 C39 1.348(8) . ? F5 C33 1.362(9) . ? F14 C44 1.350(8) . ? F16 C47 1.344(8) . ? F11 C41 1.354(8) . ? F17 C48 1.340(8) . ? F1 C29 1.350(9) . ? F19 C50 1.347(9) . ? F12 C42 1.330(9) . ? F7 C36 1.341(9) . ? F18 C49 1.351(8) . ? F13 C43 1.345(8) . ? F2 C30 1.338(10) . ? F4 C32 1.348(10) . ? F9 C38 1.346(9) . ? F8 C37 1.366(9) . ? F3 C31 1.348(9) . ? C40 C45 1.384(9) . ? C40 C41 1.388(10) . ? C40 B1 1.644(10) . ? N1 C18 1.144(9) . ? N1 C19 1.485(10) . ? C28 C29 1.371(10) . ? C28 C33 1.388(10) . ? C28 B1 1.659(10) . ? C34 C35 1.385(9) . ? C34 C39 1.390(10) . ? C34 B1 1.651(9) . ? C45 C44 1.394(9) . ? C35 C36 1.387(10) . ? C47 C46 1.392(9) . ? C47 C48 1.384(9) . ? C41 C42 1.393(10) . ? C51 C46 1.388(10) . ? C51 C50 1.387(10) . ? C44 C43 1.364(11) . ? C46 B1 1.667(9) . ? C39 C38 1.391(10) . ? C48 C49 1.378(11) . ? C29 C30 1.401(10) . ? N2 C23 1.159(11) . ? N2 C24 1.435(14) . ? C33 C32 1.380(11) . ? C50 C49 1.365(11) . ? C42 C43 1.368(11) . ? C30 C31 1.362(13) . ? C32 C31 1.361(13) . ? C36 C37 1.366(12) . ? C38 C37 1.359(12) . ? C5 C4 1.412(13) . ? C5 C1 1.357(14) . ? C5 C15 1.544(15) . ? C4 C3 1.404(13) . ? C4 C12 1.602(18) . ? C3 C2 1.393(17) . ? C3 C9 1.502(14) . ? C11 C9 1.366(11) . ? C19 C22 1.456(13) . ? C19 C20 1.416(16) . ? C19 C21 1.63(2) . ? C1 C2 1.420(16) . ? C10 C9 1.532(13) . ? C2 C6 1.547(17) . ? C27 C24 1.408(17) . ? C24 C25 1.384(17) . ? C24 C26 1.83(3) . ? C14 C12 1.436(19) . ? C12 C13 1.591(15) . ? C6 C7 1.56(3) . ? C6 C8 1.554(17) . ? C17 C15 1.68(3) . ? C15 C16 1.517(18) . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 -0.411 0.000 614.4 109.0 ?