#------------------------------------------------------------------------------ #$Date: 2020-08-20 04:50:52 +0300 (Thu, 20 Aug 2020) $ #$Revision: 255469 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705223.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_7705223 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 'C44 H76 I N2 U, C24 B F20' _chemical_formula_sum 'C68 H76 B F20 I N2 U' _chemical_formula_weight 1677.04 _chemical_name_systematic 'Bis(1,2,3,4-tetrakis(iso-propyl)cyclopentadienyl)-bis(tert-butyl-isocyano)-iodo-uranium(iv) tetrakis(pentafluorophenyl)borate' _chemical_properties_physical Air-sensitive,Moisture-sensitive,Oxygen-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_creation_date 2020-04-21 _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 90 _cell_angle_beta 111.882(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.2004(4) _cell_length_b 19.9489(3) _cell_length_c 19.6155(4) _cell_measurement_reflns_used 35610 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.3760 _cell_measurement_theta_min 2.9470 _cell_volume 6608.8(2) _computing_cell_refinement 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _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 (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 5.8140 _diffrn_detector_type 'Pilatus 200K' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -55.00 66.00 0.50 1.00 -- -17.33 72.00 79.00 242 2 \w -66.00 44.00 0.50 1.00 -- 17.64 -72.00 -49.00 220 3 \w 40.00 66.00 0.50 1.00 -- 17.64 72.00 79.00 52 4 \w -108.00 -44.00 0.50 1.00 -- -17.33 179.00-180.00 128 5 \w -93.00 -44.00 0.50 1.00 -- -17.33-179.00 90.00 98 6 \w -43.00 23.00 0.50 1.00 -- -17.33 -77.00 60.00 132 7 \w -23.00 46.00 0.50 1.00 -- 17.64 38.00 120.00 138 8 \w -45.00 -20.00 0.50 1.00 -- 17.64 -77.00-180.00 50 9 \w -19.00 7.00 0.50 1.00 -- 17.64 -77.00-180.00 52 10 \w 56.00 82.00 0.50 1.00 -- 17.64 179.00 120.00 52 11 \w 59.00 100.00 0.50 1.00 -- 17.64 38.00 120.00 82 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'ROD, Synergy Custom DW system, Pilatus 200K' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_unetI/netI 0.0494 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 78798 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.373 _diffrn_reflns_theta_min 2.801 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 3.022 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.60464 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.685 _exptl_crystal_description block _exptl_crystal_F_000 3312 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Diethyl ether' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _refine_diff_density_max 1.238 _refine_diff_density_min -1.637 _refine_diff_density_rms 0.118 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 860 _refine_ls_number_reflns 13508 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0317 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+8.8803P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.0775 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11517 _reflns_number_total 13508 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02005b2.cif _cod_data_source_block mab_iii_187 _cod_database_code 7705223 _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_estimated_absorpt_t_max 0.713 _shelx_estimated_absorpt_t_min 0.496 _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.a Ternary CH refined with riding coordinates: C23(H23), C12(H12), C32(H32), C26(H26), C6(H6), C29(H29), C9(H9), C15(H15) 2.b Aromatic/amide H refined with riding coordinates: C1(H1), C18(H18) 2.c Idealised Me refined as rotating group: C38(H38A,H38B,H38C), C31(H31A,H31B,H31C), C10(H10A,H10B,H10C), C11(H11A,H11B, H11C), C28(H28A,H28B,H28C), C25(H25A,H25B,H25C), C34(H34A,H34B,H34C), C24(H24A, H24B,H24C), C27(H27A,H27B,H27C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C37(H37A,H37B,H37C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C42(H42A,H42B, H42C), C7(H7A,H7B,H7C), C33(H33A,H33B,H33C), C14(H14A,H14B,H14C), C44(H44A, H44B,H44C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C43(H43A,H43B,H43C) ; _shelx_res_file ; mab_iii_187.res created by SHELXL-2014/7 TITL MAB_III_187 in P21/c #14 CELL 0.71073 18.2004 19.9489 19.6155 90 111.882 90 ZERR 4 0.0004 0.0003 0.0004 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B F I N U UNIT 272 304 4 80 4 8 4 L.S. 4 PLAN 16 SIZE 0.12 0.19 0.27 TEMP -173(2) BIND U1 I1 BOND LIST 4 more -1 fmap 2 acta MERG 2 SHEL 1000 0.8 REM REM REM WGHT 0.028800 8.880301 FVAR 0.25724 U1 7 0.736780 0.402756 0.999727 11.00000 0.01175 0.01240 = 0.00915 -0.00008 0.00375 -0.00015 F1 4 0.607265 0.633644 0.552497 11.00000 0.01348 0.02253 = 0.02444 -0.00811 0.00914 -0.00335 F15 4 0.842712 0.514897 0.467092 11.00000 0.02354 0.02563 = 0.01250 -0.00278 0.00684 0.00593 F16 4 0.661962 0.690418 0.440806 11.00000 0.01426 0.01927 = 0.01801 0.00045 0.00449 0.00253 F10 4 0.689775 0.574609 0.374314 11.00000 0.02202 0.01833 = 0.01007 -0.00020 0.00670 -0.00329 F7 4 0.561049 0.431596 0.537703 11.00000 0.02849 0.02265 = 0.02675 0.00130 0.01709 -0.00631 F6 4 0.684280 0.510786 0.605383 11.00000 0.02588 0.02124 = 0.01134 0.00071 0.00798 -0.00198 F5 4 0.883012 0.677568 0.652577 11.00000 0.01346 0.02755 = 0.02009 -0.00684 0.00302 -0.00056 F20 4 0.933177 0.628490 0.537935 11.00000 0.01436 0.02517 = 0.02231 0.00503 0.00634 0.00226 F4 4 0.858492 0.769142 0.741453 11.00000 0.02220 0.02636 = 0.02319 -0.01295 0.00217 -0.00355 F3 4 0.710853 0.790578 0.740208 11.00000 0.03256 0.02396 = 0.02062 -0.00936 0.01422 0.00063 F11 4 0.840630 0.553127 0.704964 11.00000 0.02760 0.02482 = 0.01088 0.00030 0.00838 0.00283 F9 4 0.568370 0.494129 0.309035 11.00000 0.02426 0.02760 = 0.01264 -0.00345 -0.00003 -0.00334 F8 4 0.499188 0.424220 0.386950 11.00000 0.01963 0.02659 = 0.02936 -0.00547 0.00516 -0.00927 F2 4 0.586295 0.719584 0.645332 11.00000 0.02413 0.02682 = 0.03543 -0.01015 0.02036 -0.00136 F19 4 0.963634 0.723430 0.458124 11.00000 0.02176 0.03356 = 0.03463 0.00468 0.01595 -0.00513 F13 4 0.999034 0.384507 0.666331 11.00000 0.02440 0.01722 = 0.04024 0.00798 0.00055 0.00776 F14 4 0.947142 0.416937 0.520587 11.00000 0.02893 0.02472 = 0.03342 -0.00608 0.01389 0.01072 F17 4 0.694840 0.784442 0.360759 11.00000 0.03124 0.01988 = 0.02598 0.00975 0.01164 0.00817 F12 4 0.942611 0.453306 0.756016 11.00000 0.03389 0.02784 = 0.01707 0.01169 -0.00062 0.00344 F18 4 0.846719 0.803390 0.368967 11.00000 0.03949 0.02318 = 0.03134 0.00952 0.02037 -0.00128 N1 6 0.795173 0.459821 1.193604 11.00000 0.01601 0.01507 = 0.01575 -0.00091 0.00661 -0.00129 C59 1 0.918093 0.469933 0.683913 11.00000 0.01748 0.02169 = 0.01641 0.00578 -0.00189 -0.00469 C41 1 0.536974 0.320314 0.744507 11.00000 0.02262 0.01787 = 0.01525 -0.00446 -0.00142 -0.00770 C57 1 0.837677 0.541073 0.582941 11.00000 0.01499 0.01426 = 0.01370 -0.00126 0.00511 -0.00264 C38 1 0.888078 0.450150 1.319203 11.00000 0.02818 0.02580 = 0.01696 -0.00327 0.00723 -0.00049 AFIX 137 H38A 2 0.884583 0.401158 1.315889 11.00000 -1.50000 H38B 2 0.899851 0.464022 1.370117 11.00000 -1.50000 H38C 2 0.930331 0.465671 1.303427 11.00000 -1.50000 AFIX 0 C31 1 0.637766 0.558727 1.090087 11.00000 0.01999 0.02411 = 0.01953 -0.00087 0.01100 0.00314 AFIX 137 H31A 2 0.585669 0.557645 1.050099 11.00000 -1.50000 H31B 2 0.636126 0.589153 1.128720 11.00000 -1.50000 H31C 2 0.651815 0.513557 1.110418 11.00000 -1.50000 AFIX 0 C10 1 0.735671 0.143350 0.952829 11.00000 0.02700 0.01738 = 0.03410 -0.00007 0.00961 -0.00243 AFIX 137 H10A 2 0.793217 0.144407 0.966406 11.00000 -1.50000 H10B 2 0.711317 0.117779 0.907258 11.00000 -1.50000 H10C 2 0.723190 0.121975 0.992194 11.00000 -1.50000 AFIX 0 C46 1 0.673160 0.662345 0.600349 11.00000 0.01843 0.01294 = 0.01264 -0.00052 0.00539 -0.00321 N2 6 0.598089 0.341498 0.814958 11.00000 0.01930 0.01468 = 0.01593 0.00008 0.00587 -0.00279 B1 3 0.768603 0.597576 0.542445 11.00000 0.01458 0.01449 = 0.00603 -0.00044 0.00073 0.00121 C23 1 0.690121 0.497098 0.808983 11.00000 0.01895 0.01615 = 0.01003 -0.00111 0.00603 -0.00280 AFIX 13 H23 2 0.632806 0.484803 0.786458 11.00000 -1.20000 AFIX 0 C68 1 0.870950 0.664046 0.494041 11.00000 0.01615 0.01508 = 0.01128 0.00198 0.00487 0.00230 C35 1 0.780221 0.442013 1.134576 11.00000 0.01660 0.01222 = 0.01627 0.00056 0.00679 -0.00046 C3 1 0.762693 0.264910 0.992178 11.00000 0.01169 0.01140 = 0.01936 0.00392 0.00514 0.00467 C22 1 0.798405 0.529582 1.009265 11.00000 0.01549 0.01124 = 0.01290 0.00169 0.00515 0.00009 C45 1 0.747746 0.647908 0.600071 11.00000 0.01465 0.01448 = 0.01086 0.00269 0.00566 0.00158 C5 1 0.851456 0.317508 1.094979 11.00000 0.01445 0.01276 = 0.01282 0.00194 0.00130 0.00631 C11 1 0.618743 0.213754 0.940668 11.00000 0.01997 0.01938 = 0.02445 -0.00098 0.00680 -0.00572 AFIX 137 H11A 2 0.584523 0.188221 0.897953 11.00000 -1.50000 H11B 2 0.598647 0.259654 0.937919 11.00000 -1.50000 H11C 2 0.619075 0.192354 0.985753 11.00000 -1.50000 AFIX 0 C28 1 0.522872 0.481094 0.859183 11.00000 0.01462 0.02154 = 0.01678 0.00118 0.00607 0.00115 AFIX 137 H28A 2 0.535032 0.469236 0.816049 11.00000 -1.50000 H28B 2 0.467623 0.495764 0.843331 11.00000 -1.50000 H28C 2 0.530987 0.441886 0.891268 11.00000 -1.50000 AFIX 0 C20 1 0.666085 0.523203 0.931434 11.00000 0.01371 0.00878 = 0.01365 0.00061 0.00322 -0.00006 C63 1 0.794712 0.651802 0.491440 11.00000 0.01943 0.01309 = 0.00438 -0.00268 0.00352 0.00047 C25 1 0.738528 0.446629 0.783547 11.00000 0.02759 0.01730 = 0.01601 -0.00283 0.01265 -0.00331 AFIX 137 H25A 2 0.794010 0.460942 0.801260 11.00000 -1.50000 H25B 2 0.717363 0.444606 0.729755 11.00000 -1.50000 H25C 2 0.735050 0.402188 0.803423 11.00000 -1.50000 AFIX 0 C64 1 0.738369 0.695440 0.445820 11.00000 0.01574 0.01345 = 0.01566 -0.00541 0.00694 -0.00172 C61 1 0.920560 0.451186 0.566057 11.00000 0.01946 0.01454 = 0.02794 -0.00631 0.00944 0.00017 C12 1 0.741521 0.240609 1.114342 11.00000 0.01944 0.02116 = 0.01850 0.00385 0.00771 0.00011 AFIX 13 H12 2 0.684325 0.236921 1.081924 11.00000 -1.20000 AFIX 0 C19 1 0.714354 0.501465 0.891950 11.00000 0.01950 0.01038 = 0.01339 -0.00077 0.00890 -0.00272 C51 1 0.692095 0.549803 0.494271 11.00000 0.01186 0.01063 = 0.01074 -0.00014 0.00284 0.00196 C32 1 0.875274 0.552037 1.069895 11.00000 0.01921 0.01481 = 0.01403 -0.00269 0.00653 -0.00442 AFIX 13 H32 2 0.875368 0.535640 1.118103 11.00000 -1.20000 AFIX 0 C26 1 0.577336 0.537774 0.901075 11.00000 0.01710 0.01605 = 0.01245 -0.00088 0.00481 0.00221 AFIX 13 H26 2 0.562730 0.548185 0.944281 11.00000 -1.20000 AFIX 0 C6 1 0.832719 0.294496 0.898693 11.00000 0.01563 0.01497 = 0.01381 -0.00149 0.00487 -0.00101 AFIX 13 H6 2 0.781418 0.303660 0.857266 11.00000 -1.20000 AFIX 0 C1 1 0.871777 0.332676 1.033529 11.00000 0.01017 0.01298 = 0.01961 -0.00240 0.00493 -0.00023 AFIX 43 H1 2 0.914147 0.360946 1.034468 11.00000 -1.20000 AFIX 0 C2 1 0.819280 0.299253 0.970690 11.00000 0.01543 0.01226 = 0.01581 0.00016 0.00648 0.00161 C52 1 0.656434 0.509218 0.531161 11.00000 0.01869 0.01603 = 0.01442 -0.00073 0.00810 0.00473 C21 1 0.718435 0.541307 1.003826 11.00000 0.01672 0.01047 = 0.01445 0.00091 0.00900 0.00005 C55 1 0.596124 0.500122 0.382669 11.00000 0.01493 0.01694 = 0.01306 -0.00120 0.00005 0.00241 C50 1 0.807980 0.686103 0.649417 11.00000 0.01798 0.01623 = 0.01363 0.00142 0.00657 0.00343 C36 1 0.809617 0.480585 1.269786 11.00000 0.02516 0.02021 = 0.01077 -0.00345 0.00823 -0.00049 C29 1 0.699799 0.583465 1.060429 11.00000 0.02091 0.01459 = 0.01403 -0.00300 0.00791 0.00018 AFIX 13 H29 2 0.750552 0.587847 1.103854 11.00000 -1.20000 AFIX 0 C56 1 0.660237 0.541649 0.418795 11.00000 0.01608 0.01427 = 0.01402 0.00376 0.00785 0.00607 C9 1 0.703169 0.215371 0.941262 11.00000 0.01967 0.01540 = 0.01528 0.00129 0.00585 -0.00135 AFIX 13 H9 2 0.697718 0.228004 0.890266 11.00000 -1.20000 AFIX 0 C54 1 0.561301 0.463370 0.421893 11.00000 0.01257 0.01492 = 0.02346 -0.00275 0.00616 0.00005 C34 1 0.947500 0.523116 1.058317 11.00000 0.01528 0.02067 = 0.01752 -0.00238 0.00361 -0.00369 AFIX 137 H34A 2 0.942540 0.474247 1.053835 11.00000 -1.50000 H34B 2 0.995548 0.534690 1.100350 11.00000 -1.50000 H34C 2 0.950734 0.541865 1.013341 11.00000 -1.50000 AFIX 0 C48 1 0.722457 0.743442 0.695923 11.00000 0.03075 0.01070 = 0.01396 -0.00050 0.01345 0.00517 C60 1 0.946394 0.434528 0.639256 11.00000 0.01742 0.01034 = 0.03206 0.00340 0.00363 0.00001 C58 1 0.864981 0.521673 0.655759 11.00000 0.01351 0.01519 = 0.01388 -0.00040 0.00288 -0.00347 C18 1 0.793561 0.503401 0.940595 11.00000 0.01780 0.01187 = 0.01625 0.00046 0.01037 0.00148 AFIX 43 H18 2 0.837497 0.489247 0.929193 11.00000 -1.20000 AFIX 0 C62 1 0.866897 0.502343 0.539877 11.00000 0.01697 0.01705 = 0.01338 -0.00193 0.00389 -0.00146 C4 1 0.782266 0.276540 1.069114 11.00000 0.01690 0.01178 = 0.01689 0.00222 0.00573 0.00363 C53 1 0.593170 0.467848 0.497431 11.00000 0.01905 0.01230 = 0.02197 -0.00006 0.01156 0.00341 C40 1 0.642720 0.359302 0.871075 11.00000 0.01957 0.01201 = 0.01793 0.00261 0.01111 -0.00232 C15 1 0.908038 0.329228 1.173678 11.00000 0.01846 0.02257 = 0.01391 -0.00236 0.00297 0.00173 AFIX 13 H15 2 0.876130 0.341227 1.203818 11.00000 -1.20000 AFIX 0 C24 1 0.702035 0.566524 0.780533 11.00000 0.03642 0.01665 = 0.01424 -0.00041 0.01287 -0.00034 AFIX 137 H24A 2 0.758426 0.578082 0.800705 11.00000 -1.50000 H24B 2 0.672117 0.600102 0.796001 11.00000 -1.50000 H24C 2 0.683151 0.565613 0.726771 11.00000 -1.50000 AFIX 0 C65 1 0.753701 0.745016 0.404214 11.00000 0.02263 0.01402 = 0.01280 0.00144 0.00397 0.00551 C27 1 0.556383 0.600283 0.851488 11.00000 0.01931 0.01979 = 0.02245 0.00368 0.00277 0.00154 AFIX 137 H27A 2 0.554305 0.588292 0.802353 11.00000 -1.50000 H27B 2 0.596816 0.634830 0.872518 11.00000 -1.50000 H27C 2 0.504689 0.617519 0.848025 11.00000 -1.50000 AFIX 0 C47 1 0.660154 0.708147 0.648117 11.00000 0.02137 0.01719 = 0.01667 0.00295 0.01344 0.00311 C8 1 0.894232 0.345126 0.894865 11.00000 0.02500 0.01869 = 0.02777 -0.00077 0.01657 -0.00175 AFIX 137 H8A 2 0.880029 0.390038 0.906086 11.00000 -1.50000 H8B 2 0.895539 0.344858 0.845370 11.00000 -1.50000 H8C 2 0.946521 0.332906 0.930687 11.00000 -1.50000 AFIX 0 C49 1 0.797061 0.733027 0.696492 11.00000 0.02372 0.01683 = 0.01270 -0.00395 0.00274 -0.00443 C67 1 0.888943 0.713720 0.452841 11.00000 0.01819 0.02399 = 0.01762 -0.00475 0.00987 -0.00631 C66 1 0.829761 0.754332 0.407917 11.00000 0.03199 0.01699 = 0.01679 0.00239 0.01442 -0.00427 C17 1 0.968377 0.384851 1.182184 11.00000 0.02030 0.02898 = 0.01637 -0.00410 0.00160 -0.00352 AFIX 137 H17A 2 1.002512 0.372573 1.155566 11.00000 -1.50000 H17B 2 1.000782 0.390976 1.234363 11.00000 -1.50000 H17C 2 0.940587 0.426725 1.162087 11.00000 -1.50000 AFIX 0 C37 1 0.812274 0.556785 1.272459 11.00000 0.03758 0.01722 = 0.01942 -0.00431 0.00905 -0.00288 AFIX 137 H37A 2 0.855204 0.572754 1.257875 11.00000 -1.50000 H37B 2 0.821615 0.571895 1.322542 11.00000 -1.50000 H37C 2 0.761716 0.574798 1.238681 11.00000 -1.50000 AFIX 0 C30 1 0.676678 0.654786 1.029891 11.00000 0.03749 0.01698 = 0.02020 -0.00479 0.01166 0.00114 AFIX 137 H30A 2 0.622478 0.654468 0.993311 11.00000 -1.50000 H30B 2 0.713089 0.670076 1.006825 11.00000 -1.50000 H30C 2 0.679756 0.685192 1.070106 11.00000 -1.50000 AFIX 0 C39 1 0.740303 0.453157 1.287125 11.00000 0.03284 0.02852 = 0.02088 -0.00168 0.01842 -0.00374 AFIX 137 H39A 2 0.690901 0.473422 1.253853 11.00000 -1.50000 H39B 2 0.747907 0.464036 1.338032 11.00000 -1.50000 H39C 2 0.737565 0.404391 1.280630 11.00000 -1.50000 AFIX 0 C42 1 0.457087 0.335567 0.748933 11.00000 0.02277 0.03402 = 0.02086 0.00362 -0.00119 -0.00895 AFIX 137 H42A 2 0.453871 0.314114 0.792680 11.00000 -1.50000 H42B 2 0.414812 0.318266 0.704962 11.00000 -1.50000 H42C 2 0.451049 0.384161 0.752013 11.00000 -1.50000 AFIX 0 C7 1 0.861332 0.224128 0.888155 11.00000 0.02595 0.01988 = 0.01774 -0.00231 0.00950 0.00228 AFIX 137 H7A 2 0.903920 0.209975 0.933612 11.00000 -1.50000 H7B 2 0.881144 0.225144 0.848060 11.00000 -1.50000 H7C 2 0.817167 0.192421 0.876078 11.00000 -1.50000 AFIX 0 C33 1 0.882622 0.628094 1.073029 11.00000 0.02471 0.02432 = 0.02771 -0.00669 0.00755 -0.01033 AFIX 137 H33A 2 0.879843 0.645069 1.025246 11.00000 -1.50000 H33B 2 0.933446 0.640852 1.110922 11.00000 -1.50000 H33C 2 0.839307 0.647322 1.084935 11.00000 -1.50000 AFIX 0 C14 1 0.744009 0.275950 1.184584 11.00000 0.03115 0.03494 = 0.01870 0.00275 0.01298 -0.00589 AFIX 137 H14A 2 0.798683 0.277124 1.220182 11.00000 -1.50000 H14B 2 0.710814 0.251465 1.205650 11.00000 -1.50000 H14C 2 0.724119 0.321848 1.172817 11.00000 -1.50000 AFIX 0 C44 1 0.549571 0.359083 0.683381 11.00000 0.03039 0.03246 = 0.01809 -0.00300 0.00734 -0.00887 AFIX 137 H44A 2 0.540844 0.406937 0.688788 11.00000 -1.50000 H44B 2 0.512163 0.343280 0.635799 11.00000 -1.50000 H44C 2 0.603860 0.352119 0.685999 11.00000 -1.50000 AFIX 0 C13 1 0.771874 0.168025 1.134083 11.00000 0.04464 0.02623 = 0.03421 0.01186 0.01983 0.00275 AFIX 137 H13A 2 0.794503 0.152017 1.098881 11.00000 -1.50000 H13B 2 0.727740 0.138945 1.132141 11.00000 -1.50000 H13C 2 0.812611 0.167124 1.183737 11.00000 -1.50000 AFIX 0 C16 1 0.952662 0.263861 1.204025 11.00000 0.02725 0.02992 = 0.02695 -0.00037 -0.00367 0.00794 AFIX 137 H16A 2 0.914599 0.228399 1.201877 11.00000 -1.50000 H16B 2 0.988445 0.270645 1.255119 11.00000 -1.50000 H16C 2 0.983446 0.250786 1.174461 11.00000 -1.50000 AFIX 0 C43 1 0.546939 0.245246 0.736714 11.00000 0.04442 0.02051 = 0.02810 -0.00827 0.00418 -0.00531 AFIX 137 H43A 2 0.601574 0.235789 0.741799 11.00000 -1.50000 H43B 2 0.510570 0.230321 0.688289 11.00000 -1.50000 H43C 2 0.535084 0.221323 0.775040 11.00000 -1.50000 AFIX 0 I1 5 0.593536 0.376516 1.035736 11.00000 0.01890 0.02625 = 0.02481 0.00290 0.01071 0.00160 HKLF 4 REM MAB_III_187 in P21/c #14 REM R1 = 0.0317 for 11517 Fo > 4sig(Fo) and 0.0411 for all 13508 data REM 860 parameters refined using 0 restraints END WGHT 0.0288 8.8829 REM Highest difference peak 1.238, deepest hole -1.637, 1-sigma level 0.118 Q1 1 0.7624 0.4329 1.0269 11.00000 0.05 1.24 Q2 1 0.7769 0.4039 0.9890 11.00000 0.05 1.01 Q3 1 0.6315 0.3873 1.0109 11.00000 0.05 0.86 Q4 1 0.7642 0.3802 1.0400 11.00000 0.05 0.80 Q5 1 0.6905 0.4006 1.0157 11.00000 0.05 0.78 Q6 1 0.7003 0.4377 0.9853 11.00000 0.05 0.72 Q7 1 0.7065 0.3917 0.9542 11.00000 0.05 0.68 Q8 1 0.7631 0.5287 0.9171 11.00000 0.05 0.58 Q9 1 0.6261 0.3992 1.0835 11.00000 0.05 0.58 Q10 1 0.5547 0.4006 0.9881 11.00000 0.05 0.57 Q11 1 0.5601 0.3508 0.9808 11.00000 0.05 0.54 Q12 1 0.8330 0.5301 1.0453 11.00000 0.05 0.51 Q13 1 0.5182 0.5598 0.9140 11.00000 0.05 0.50 Q14 1 0.6584 0.3632 1.0620 11.00000 0.05 0.49 Q15 1 0.8665 0.5416 0.6246 11.00000 0.05 0.49 Q16 1 0.5374 0.4031 1.0358 11.00000 0.05 0.48 ; _shelx_res_checksum 68822 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.73678(2) 0.40276(2) 0.99973(2) 0.01114(5) Uani 1 1 d . . . . . F1 F 0.60727(12) 0.63364(10) 0.55250(12) 0.0196(5) Uani 1 1 d . . . . . F15 F 0.84271(13) 0.51490(11) 0.46709(11) 0.0205(5) Uani 1 1 d . . . . . F16 F 0.66196(12) 0.69042(10) 0.44081(11) 0.0176(5) Uani 1 1 d . . . . . F10 F 0.68978(12) 0.57461(10) 0.37431(10) 0.0166(4) Uani 1 1 d . . . . . F7 F 0.56105(13) 0.43160(11) 0.53770(12) 0.0240(5) Uani 1 1 d . . . . . F6 F 0.68428(13) 0.51079(10) 0.60538(11) 0.0192(5) Uani 1 1 d . . . . . F5 F 0.88301(12) 0.67757(11) 0.65258(11) 0.0213(5) Uani 1 1 d . . . . . F20 F 0.93318(12) 0.62849(11) 0.53794(12) 0.0208(5) Uani 1 1 d . . . . . F4 F 0.85849(13) 0.76914(11) 0.74145(12) 0.0257(5) Uani 1 1 d . . . . . F3 F 0.71085(14) 0.79058(11) 0.74021(12) 0.0245(5) Uani 1 1 d . . . . . F11 F 0.84063(13) 0.55313(10) 0.70496(11) 0.0208(5) Uani 1 1 d . . . . . F9 F 0.56837(13) 0.49413(11) 0.30903(11) 0.0235(5) Uani 1 1 d . . . . . F8 F 0.49919(13) 0.42422(11) 0.38695(13) 0.0263(5) Uani 1 1 d . . . . . F2 F 0.58630(13) 0.71958(11) 0.64533(13) 0.0261(5) Uani 1 1 d . . . . . F19 F 0.96363(13) 0.72343(12) 0.45812(13) 0.0284(5) Uani 1 1 d . . . . . F13 F 0.99903(14) 0.38451(11) 0.66633(14) 0.0306(6) Uani 1 1 d . . . . . F14 F 0.94714(14) 0.41694(11) 0.52059(13) 0.0284(6) Uani 1 1 d . . . . . F17 F 0.69484(14) 0.78444(11) 0.36076(12) 0.0254(5) Uani 1 1 d . . . . . F12 F 0.94261(14) 0.45331(11) 0.75602(12) 0.0292(6) Uani 1 1 d . . . . . F18 F 0.84672(14) 0.80339(11) 0.36897(13) 0.0293(6) Uani 1 1 d . . . . . N1 N 0.79517(18) 0.45982(15) 1.19360(16) 0.0154(7) Uani 1 1 d . . . . . C59 C 0.9181(2) 0.46993(19) 0.6839(2) 0.0209(9) Uani 1 1 d . . . . . C41 C 0.5370(2) 0.32031(19) 0.7445(2) 0.0210(8) Uani 1 1 d . . . . . C57 C 0.8377(2) 0.54107(18) 0.58294(19) 0.0144(8) Uani 1 1 d . . . . . C38 C 0.8881(2) 0.4502(2) 1.3192(2) 0.0240(9) Uani 1 1 d . . . . . H38A H 0.8846 0.4012 1.3159 0.036 Uiso 1 1 calc GR . . . . H38B H 0.8999 0.4640 1.3701 0.036 Uiso 1 1 calc GR . . . . H38C H 0.9303 0.4657 1.3034 0.036 Uiso 1 1 calc GR . . . . C31 C 0.6378(2) 0.55873(19) 1.0901(2) 0.0202(8) Uani 1 1 d . . . . . H31A H 0.5857 0.5576 1.0501 0.030 Uiso 1 1 calc GR . . . . H31B H 0.6361 0.5892 1.1287 0.030 Uiso 1 1 calc GR . . . . H31C H 0.6518 0.5136 1.1104 0.030 Uiso 1 1 calc GR . . . . C10 C 0.7357(3) 0.14335(19) 0.9528(2) 0.0267(9) Uani 1 1 d . . . . . H10A H 0.7932 0.1444 0.9664 0.040 Uiso 1 1 calc GR . . . . H10B H 0.7113 0.1178 0.9073 0.040 Uiso 1 1 calc GR . . . . H10C H 0.7232 0.1220 0.9922 0.040 Uiso 1 1 calc GR . . . . C46 C 0.6732(2) 0.66234(17) 0.60035(19) 0.0148(8) Uani 1 1 d . . . . . N2 N 0.59809(19) 0.34150(15) 0.81496(17) 0.0168(7) Uani 1 1 d . . . . . B1 B 0.7686(2) 0.5976(2) 0.5424(2) 0.0126(8) Uani 1 1 d . . . . . C23 C 0.6901(2) 0.49710(18) 0.80898(19) 0.0149(8) Uani 1 1 d . . . . . H23 H 0.6328 0.4848 0.7865 0.018 Uiso 1 1 calc R . . . . C68 C 0.8710(2) 0.66405(18) 0.49404(19) 0.0142(8) Uani 1 1 d . . . . . C35 C 0.7802(2) 0.44201(17) 1.1346(2) 0.0148(8) Uani 1 1 d . . . . . C3 C 0.7627(2) 0.26491(18) 0.9922(2) 0.0143(7) Uani 1 1 d . . . . . C22 C 0.7984(2) 0.52958(17) 1.00927(19) 0.0133(7) Uani 1 1 d . . . . . C45 C 0.7477(2) 0.64791(17) 0.60007(19) 0.0131(7) Uani 1 1 d . . . . . C5 C 0.8515(2) 0.31751(18) 1.09498(19) 0.0144(7) Uani 1 1 d . . . . . C11 C 0.6187(2) 0.21375(19) 0.9407(2) 0.0217(9) Uani 1 1 d . . . . . H11A H 0.5845 0.1882 0.8980 0.033 Uiso 1 1 calc GR . . . . H11B H 0.5986 0.2597 0.9379 0.033 Uiso 1 1 calc GR . . . . H11C H 0.6191 0.1924 0.9858 0.033 Uiso 1 1 calc GR . . . . C28 C 0.5229(2) 0.48109(18) 0.8592(2) 0.0176(8) Uani 1 1 d . . . . . H28A H 0.5350 0.4692 0.8160 0.026 Uiso 1 1 calc GR . . . . H28B H 0.4676 0.4958 0.8433 0.026 Uiso 1 1 calc GR . . . . H28C H 0.5310 0.4419 0.8913 0.026 Uiso 1 1 calc GR . . . . C20 C 0.6661(2) 0.52320(17) 0.93143(19) 0.0126(7) Uani 1 1 d . . . . . C63 C 0.7947(2) 0.65180(17) 0.49144(18) 0.0126(7) Uani 1 1 d . . . . . C25 C 0.7385(2) 0.44663(18) 0.7835(2) 0.0190(8) Uani 1 1 d . . . . . H25A H 0.7940 0.4609 0.8013 0.028 Uiso 1 1 calc GR . . . . H25B H 0.7174 0.4446 0.7298 0.028 Uiso 1 1 calc GR . . . . H25C H 0.7351 0.4022 0.8034 0.028 Uiso 1 1 calc GR . . . . C64 C 0.7384(2) 0.69544(17) 0.44582(19) 0.0146(8) Uani 1 1 d . . . . . C61 C 0.9206(2) 0.45119(19) 0.5661(2) 0.0205(8) Uani 1 1 d . . . . . C12 C 0.7415(2) 0.24061(19) 1.1143(2) 0.0195(8) Uani 1 1 d . . . . . H12 H 0.6843 0.2369 1.0819 0.023 Uiso 1 1 calc R . . . . C19 C 0.7144(2) 0.50146(17) 0.89195(19) 0.0136(7) Uani 1 1 d . . . . . C51 C 0.6921(2) 0.54980(17) 0.49427(18) 0.0115(7) Uani 1 1 d . . . . . C32 C 0.8753(2) 0.55204(18) 1.0699(2) 0.0159(8) Uani 1 1 d . . . . . H32 H 0.8754 0.5356 1.1181 0.019 Uiso 1 1 calc R . . . . C26 C 0.5773(2) 0.53777(18) 0.90108(19) 0.0154(8) Uani 1 1 d . . . . . H26 H 0.5627 0.5482 0.9443 0.018 Uiso 1 1 calc R . . . . C6 C 0.8327(2) 0.29450(17) 0.89869(19) 0.0150(8) Uani 1 1 d . . . . . H6 H 0.7814 0.3037 0.8573 0.018 Uiso 1 1 calc R . . . . C1 C 0.8718(2) 0.33268(17) 1.0335(2) 0.0144(7) Uani 1 1 d . . . . . H1 H 0.9141 0.3609 1.0345 0.017 Uiso 1 1 calc R . . . . C2 C 0.8193(2) 0.29925(17) 0.97069(19) 0.0143(7) Uani 1 1 d . . . . . C52 C 0.6564(2) 0.50922(18) 0.5312(2) 0.0158(8) Uani 1 1 d . . . . . C21 C 0.7184(2) 0.54131(17) 1.00383(19) 0.0130(7) Uani 1 1 d . . . . . C55 C 0.5961(2) 0.50012(18) 0.38267(19) 0.0165(8) Uani 1 1 d . . . . . C50 C 0.8080(2) 0.68610(18) 0.64942(19) 0.0157(8) Uani 1 1 d . . . . . C36 C 0.8096(2) 0.48059(19) 1.26979(19) 0.0183(8) Uani 1 1 d . . . . . C29 C 0.6998(2) 0.58346(17) 1.0604(2) 0.0161(8) Uani 1 1 d . . . . . H29 H 0.7506 0.5878 1.1039 0.019 Uiso 1 1 calc R . . . . C56 C 0.6602(2) 0.54165(18) 0.41880(19) 0.0141(8) Uani 1 1 d . . . . . C9 C 0.7032(2) 0.21537(18) 0.9413(2) 0.0170(8) Uani 1 1 d . . . . . H9 H 0.6977 0.2280 0.8903 0.020 Uiso 1 1 calc R . . . . C54 C 0.5613(2) 0.46337(18) 0.4219(2) 0.0171(8) Uani 1 1 d . . . . . C34 C 0.9475(2) 0.52312(19) 1.0583(2) 0.0185(8) Uani 1 1 d . . . . . H34A H 0.9425 0.4742 1.0538 0.028 Uiso 1 1 calc GR . . . . H34B H 0.9955 0.5347 1.1004 0.028 Uiso 1 1 calc GR . . . . H34C H 0.9507 0.5419 1.0133 0.028 Uiso 1 1 calc GR . . . . C48 C 0.7225(2) 0.74344(17) 0.6959(2) 0.0170(8) Uani 1 1 d . . . . . C60 C 0.9464(2) 0.43453(18) 0.6393(2) 0.0216(9) Uani 1 1 d . . . . . C58 C 0.8650(2) 0.52167(18) 0.65576(19) 0.0148(8) Uani 1 1 d . . . . . C18 C 0.7936(2) 0.50340(17) 0.94059(19) 0.0141(7) Uani 1 1 d . . . . . H18 H 0.8375 0.4892 0.9292 0.017 Uiso 1 1 calc R . . . . C62 C 0.8669(2) 0.50234(18) 0.5399(2) 0.0163(8) Uani 1 1 d . . . . . C4 C 0.7823(2) 0.27654(17) 1.0691(2) 0.0154(8) Uani 1 1 d . . . . . C53 C 0.5932(2) 0.46785(18) 0.4974(2) 0.0166(8) Uani 1 1 d . . . . . C40 C 0.6427(2) 0.35930(18) 0.8711(2) 0.0153(8) Uani 1 1 d . . . . . C15 C 0.9080(2) 0.32923(19) 1.1737(2) 0.0192(8) Uani 1 1 d . . . . . H15 H 0.8761 0.3412 1.2038 0.023 Uiso 1 1 calc R . . . . C24 C 0.7020(3) 0.56652(19) 0.7805(2) 0.0214(9) Uani 1 1 d . . . . . H24A H 0.7584 0.5781 0.8007 0.032 Uiso 1 1 calc GR . . . . H24B H 0.6721 0.6001 0.7960 0.032 Uiso 1 1 calc GR . . . . H24C H 0.6832 0.5656 0.7268 0.032 Uiso 1 1 calc GR . . . . C65 C 0.7537(2) 0.74502(18) 0.40421(19) 0.0172(8) Uani 1 1 d . . . . . C27 C 0.5564(2) 0.60028(18) 0.8515(2) 0.0220(9) Uani 1 1 d . . . . . H27A H 0.5543 0.5883 0.8024 0.033 Uiso 1 1 calc GR . . . . H27B H 0.5968 0.6348 0.8725 0.033 Uiso 1 1 calc GR . . . . H27C H 0.5047 0.6175 0.8480 0.033 Uiso 1 1 calc GR . . . . C47 C 0.6602(2) 0.70815(18) 0.6481(2) 0.0166(8) Uani 1 1 d . . . . . C8 C 0.8942(2) 0.34513(19) 0.8949(2) 0.0219(9) Uani 1 1 d . . . . . H8A H 0.8800 0.3900 0.9061 0.033 Uiso 1 1 calc GR . . . . H8B H 0.8955 0.3449 0.8454 0.033 Uiso 1 1 calc GR . . . . H8C H 0.9465 0.3329 0.9307 0.033 Uiso 1 1 calc GR . . . . C49 C 0.7971(2) 0.73303(18) 0.6965(2) 0.0189(8) Uani 1 1 d . . . . . C67 C 0.8889(2) 0.71372(19) 0.4528(2) 0.0190(8) Uani 1 1 d . . . . . C66 C 0.8298(2) 0.75433(19) 0.4079(2) 0.0204(8) Uani 1 1 d . . . . . C17 C 0.9684(2) 0.3849(2) 1.1822(2) 0.0234(9) Uani 1 1 d . . . . . H17A H 1.0025 0.3726 1.1556 0.035 Uiso 1 1 calc GR . . . . H17B H 1.0008 0.3910 1.2344 0.035 Uiso 1 1 calc GR . . . . H17C H 0.9406 0.4267 1.1621 0.035 Uiso 1 1 calc GR . . . . C37 C 0.8123(3) 0.55679(19) 1.2725(2) 0.0252(9) Uani 1 1 d . . . . . H37A H 0.8552 0.5728 1.2579 0.038 Uiso 1 1 calc GR . . . . H37B H 0.8216 0.5719 1.3225 0.038 Uiso 1 1 calc GR . . . . H37C H 0.7617 0.5748 1.2387 0.038 Uiso 1 1 calc GR . . . . C30 C 0.6767(3) 0.65479(19) 1.0299(2) 0.0246(9) Uani 1 1 d . . . . . H30A H 0.6225 0.6545 0.9933 0.037 Uiso 1 1 calc GR . . . . H30B H 0.7131 0.6701 1.0068 0.037 Uiso 1 1 calc GR . . . . H30C H 0.6798 0.6852 1.0701 0.037 Uiso 1 1 calc GR . . . . C39 C 0.7403(3) 0.4532(2) 1.2871(2) 0.0250(9) Uani 1 1 d . . . . . H39A H 0.6909 0.4734 1.2539 0.037 Uiso 1 1 calc GR . . . . H39B H 0.7479 0.4640 1.3380 0.037 Uiso 1 1 calc GR . . . . H39C H 0.7376 0.4044 1.2806 0.037 Uiso 1 1 calc GR . . . . C42 C 0.4571(2) 0.3356(2) 0.7489(2) 0.0286(10) Uani 1 1 d . . . . . H42A H 0.4539 0.3141 0.7927 0.043 Uiso 1 1 calc GR . . . . H42B H 0.4148 0.3183 0.7050 0.043 Uiso 1 1 calc GR . . . . H42C H 0.4510 0.3842 0.7520 0.043 Uiso 1 1 calc GR . . . . C7 C 0.8613(2) 0.22413(19) 0.8882(2) 0.0208(8) Uani 1 1 d . . . . . H7A H 0.9039 0.2100 0.9336 0.031 Uiso 1 1 calc GR . . . . H7B H 0.8811 0.2251 0.8481 0.031 Uiso 1 1 calc GR . . . . H7C H 0.8172 0.1924 0.8761 0.031 Uiso 1 1 calc GR . . . . C33 C 0.8826(2) 0.6281(2) 1.0730(2) 0.0262(9) Uani 1 1 d . . . . . H33A H 0.8798 0.6451 1.0252 0.039 Uiso 1 1 calc GR . . . . H33B H 0.9334 0.6409 1.1109 0.039 Uiso 1 1 calc GR . . . . H33C H 0.8393 0.6473 1.0849 0.039 Uiso 1 1 calc GR . . . . C14 C 0.7440(3) 0.2760(2) 1.1846(2) 0.0272(10) Uani 1 1 d . . . . . H14A H 0.7987 0.2771 1.2202 0.041 Uiso 1 1 calc GR . . . . H14B H 0.7108 0.2515 1.2056 0.041 Uiso 1 1 calc GR . . . . H14C H 0.7241 0.3218 1.1728 0.041 Uiso 1 1 calc GR . . . . C44 C 0.5496(3) 0.3591(2) 0.6834(2) 0.0275(10) Uani 1 1 d . . . . . H44A H 0.5408 0.4069 0.6888 0.041 Uiso 1 1 calc GR . . . . H44B H 0.5122 0.3433 0.6358 0.041 Uiso 1 1 calc GR . . . . H44C H 0.6039 0.3521 0.6860 0.041 Uiso 1 1 calc GR . . . . C13 C 0.7719(3) 0.1680(2) 1.1341(3) 0.0335(11) Uani 1 1 d . . . . . H13A H 0.7945 0.1520 1.0989 0.050 Uiso 1 1 calc GR . . . . H13B H 0.7277 0.1389 1.1321 0.050 Uiso 1 1 calc GR . . . . H13C H 0.8126 0.1671 1.1837 0.050 Uiso 1 1 calc GR . . . . C16 C 0.9527(3) 0.2639(2) 1.2040(2) 0.0320(10) Uani 1 1 d . . . . . H16A H 0.9146 0.2284 1.2019 0.048 Uiso 1 1 calc GR . . . . H16B H 0.9884 0.2706 1.2551 0.048 Uiso 1 1 calc GR . . . . H16C H 0.9834 0.2508 1.1745 0.048 Uiso 1 1 calc GR . . . . C43 C 0.5469(3) 0.2452(2) 0.7367(2) 0.0337(11) Uani 1 1 d . . . . . H43A H 0.6016 0.2358 0.7418 0.051 Uiso 1 1 calc GR . . . . H43B H 0.5106 0.2303 0.6883 0.051 Uiso 1 1 calc GR . . . . H43C H 0.5351 0.2213 0.7750 0.051 Uiso 1 1 calc GR . . . . I1 I 0.59354(2) 0.37652(2) 1.03574(2) 0.02257(7) 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 U1 0.01175(7) 0.01240(8) 0.00915(7) -0.00008(5) 0.00375(5) -0.00015(5) F1 0.0135(11) 0.0225(12) 0.0244(12) -0.0081(9) 0.0091(10) -0.0033(9) F15 0.0235(12) 0.0256(12) 0.0125(11) -0.0028(9) 0.0068(9) 0.0059(10) F16 0.0143(11) 0.0193(12) 0.0180(11) 0.0004(9) 0.0045(9) 0.0025(9) F10 0.0220(12) 0.0183(11) 0.0101(10) -0.0002(8) 0.0067(9) -0.0033(9) F7 0.0285(13) 0.0227(12) 0.0267(13) 0.0013(10) 0.0171(11) -0.0063(10) F6 0.0259(12) 0.0212(12) 0.0113(11) 0.0007(8) 0.0080(9) -0.0020(9) F5 0.0135(11) 0.0275(13) 0.0201(12) -0.0068(9) 0.0030(9) -0.0006(9) F20 0.0144(11) 0.0252(13) 0.0223(12) 0.0050(9) 0.0063(10) 0.0023(9) F4 0.0222(12) 0.0264(13) 0.0232(12) -0.0130(10) 0.0022(10) -0.0035(10) F3 0.0326(13) 0.0240(12) 0.0206(12) -0.0094(9) 0.0142(11) 0.0006(10) F11 0.0276(13) 0.0248(12) 0.0109(11) 0.0003(9) 0.0084(9) 0.0028(10) F9 0.0243(12) 0.0276(13) 0.0126(11) -0.0034(9) 0.0000(9) -0.0033(10) F8 0.0196(12) 0.0266(13) 0.0294(13) -0.0055(10) 0.0052(10) -0.0093(10) F2 0.0241(13) 0.0268(13) 0.0354(14) -0.0101(10) 0.0204(11) -0.0014(10) F19 0.0218(12) 0.0336(14) 0.0346(14) 0.0047(11) 0.0159(11) -0.0051(11) F13 0.0244(13) 0.0172(12) 0.0402(15) 0.0080(10) 0.0006(12) 0.0078(10) F14 0.0289(14) 0.0247(13) 0.0334(14) -0.0061(10) 0.0139(11) 0.0107(10) F17 0.0312(13) 0.0199(12) 0.0260(13) 0.0097(9) 0.0116(11) 0.0082(10) F12 0.0339(14) 0.0278(13) 0.0171(12) 0.0117(9) -0.0006(10) 0.0034(11) F18 0.0395(15) 0.0232(13) 0.0313(14) 0.0095(10) 0.0204(12) -0.0013(11) N1 0.0160(16) 0.0151(16) 0.0158(17) -0.0009(12) 0.0066(13) -0.0013(13) C59 0.017(2) 0.022(2) 0.016(2) 0.0058(16) -0.0019(16) -0.0047(17) C41 0.023(2) 0.018(2) 0.0152(19) -0.0045(15) -0.0014(16) -0.0077(17) C57 0.0150(19) 0.0143(19) 0.0137(18) -0.0013(14) 0.0051(15) -0.0026(15) C38 0.028(2) 0.026(2) 0.017(2) -0.0033(16) 0.0072(18) -0.0005(18) C31 0.020(2) 0.024(2) 0.020(2) -0.0009(16) 0.0110(17) 0.0031(17) C10 0.027(2) 0.017(2) 0.034(2) -0.0001(17) 0.010(2) -0.0024(18) C46 0.018(2) 0.0129(19) 0.0126(18) -0.0005(14) 0.0054(15) -0.0032(15) N2 0.0193(17) 0.0147(17) 0.0159(17) 0.0001(13) 0.0059(14) -0.0028(13) B1 0.015(2) 0.014(2) 0.0060(18) -0.0004(15) 0.0007(16) 0.0012(17) C23 0.0190(19) 0.016(2) 0.0100(18) -0.0011(14) 0.0060(15) -0.0028(15) C68 0.0162(19) 0.0151(19) 0.0113(18) 0.0020(14) 0.0049(15) 0.0023(15) C35 0.0166(19) 0.0122(19) 0.016(2) 0.0006(14) 0.0068(16) -0.0005(15) C3 0.0117(18) 0.0114(19) 0.0194(19) 0.0039(14) 0.0051(15) 0.0047(14) C22 0.0155(19) 0.0112(19) 0.0129(18) 0.0017(13) 0.0051(15) 0.0001(15) C45 0.0146(18) 0.0145(19) 0.0109(17) 0.0027(14) 0.0057(15) 0.0016(15) C5 0.0144(18) 0.0128(18) 0.0128(18) 0.0019(14) 0.0013(15) 0.0063(15) C11 0.020(2) 0.019(2) 0.024(2) -0.0010(16) 0.0068(17) -0.0057(17) C28 0.0146(19) 0.022(2) 0.0168(19) 0.0012(15) 0.0061(16) 0.0012(16) C20 0.0137(18) 0.0088(18) 0.0136(18) 0.0006(13) 0.0032(15) -0.0001(14) C63 0.0194(19) 0.0131(18) 0.0044(16) -0.0027(13) 0.0035(14) 0.0005(15) C25 0.028(2) 0.017(2) 0.0160(19) -0.0028(15) 0.0126(17) -0.0033(16) C64 0.0157(19) 0.0135(19) 0.0157(18) -0.0054(14) 0.0069(15) -0.0017(15) C61 0.019(2) 0.015(2) 0.028(2) -0.0063(16) 0.0094(18) 0.0002(16) C12 0.019(2) 0.021(2) 0.018(2) 0.0038(15) 0.0077(17) 0.0001(16) C19 0.0195(19) 0.0104(18) 0.0134(18) -0.0008(14) 0.0089(16) -0.0027(15) C51 0.0119(18) 0.0106(18) 0.0107(17) -0.0001(13) 0.0028(14) 0.0020(14) C32 0.019(2) 0.0148(19) 0.0140(18) -0.0027(14) 0.0065(16) -0.0044(15) C26 0.0171(19) 0.0161(19) 0.0124(18) -0.0009(14) 0.0048(15) 0.0022(15) C6 0.0156(19) 0.0150(19) 0.0138(18) -0.0015(14) 0.0049(15) -0.0010(15) C1 0.0102(18) 0.0130(19) 0.0196(19) -0.0024(14) 0.0049(15) -0.0002(14) C2 0.0154(19) 0.0123(19) 0.0158(18) 0.0002(14) 0.0065(15) 0.0016(15) C52 0.019(2) 0.0160(19) 0.0144(18) -0.0007(14) 0.0081(16) 0.0047(16) C21 0.0167(19) 0.0105(18) 0.0144(18) 0.0009(14) 0.0090(15) 0.0001(15) C55 0.0149(19) 0.017(2) 0.0131(18) -0.0012(14) 0.0000(15) 0.0024(15) C50 0.0180(19) 0.0162(19) 0.0136(18) 0.0014(14) 0.0066(15) 0.0034(16) C36 0.025(2) 0.020(2) 0.0108(18) -0.0035(15) 0.0082(16) -0.0005(17) C29 0.021(2) 0.015(2) 0.0140(18) -0.0030(14) 0.0079(16) 0.0002(15) C56 0.0161(19) 0.0143(19) 0.0140(18) 0.0038(14) 0.0079(15) 0.0061(15) C9 0.020(2) 0.015(2) 0.0153(19) 0.0013(14) 0.0058(16) -0.0013(16) C54 0.0126(19) 0.015(2) 0.023(2) -0.0028(15) 0.0062(16) 0.0000(15) C34 0.0153(19) 0.021(2) 0.0175(19) -0.0024(15) 0.0036(16) -0.0037(16) C48 0.031(2) 0.0107(19) 0.0140(18) -0.0005(14) 0.0134(17) 0.0052(16) C60 0.017(2) 0.0103(19) 0.032(2) 0.0034(16) 0.0036(18) 0.0000(16) C58 0.0135(18) 0.0152(19) 0.0139(18) -0.0004(14) 0.0029(15) -0.0035(15) C18 0.0178(19) 0.0119(18) 0.0163(19) 0.0005(14) 0.0104(16) 0.0015(15) C62 0.0170(19) 0.017(2) 0.0134(18) -0.0019(14) 0.0039(15) -0.0015(16) C4 0.0169(19) 0.0118(19) 0.0169(19) 0.0022(14) 0.0057(16) 0.0036(15) C53 0.019(2) 0.0123(19) 0.022(2) -0.0001(15) 0.0116(17) 0.0034(15) C40 0.020(2) 0.0120(19) 0.018(2) 0.0026(14) 0.0111(17) -0.0023(15) C15 0.018(2) 0.023(2) 0.0139(19) -0.0024(15) 0.0030(16) 0.0017(16) C24 0.036(2) 0.017(2) 0.0142(19) -0.0004(15) 0.0129(18) -0.0003(18) C65 0.023(2) 0.0140(19) 0.0128(18) 0.0014(14) 0.0040(16) 0.0055(16) C27 0.019(2) 0.020(2) 0.022(2) 0.0037(16) 0.0028(17) 0.0015(17) C47 0.021(2) 0.017(2) 0.0167(19) 0.0029(15) 0.0134(16) 0.0031(16) C8 0.025(2) 0.019(2) 0.028(2) -0.0008(16) 0.0166(19) -0.0017(17) C49 0.024(2) 0.017(2) 0.0127(19) -0.0039(15) 0.0027(16) -0.0044(16) C67 0.018(2) 0.024(2) 0.018(2) -0.0048(16) 0.0099(16) -0.0063(16) C66 0.032(2) 0.017(2) 0.017(2) 0.0024(15) 0.0144(18) -0.0043(17) C17 0.020(2) 0.029(2) 0.016(2) -0.0041(16) 0.0016(17) -0.0035(17) C37 0.038(3) 0.017(2) 0.019(2) -0.0043(16) 0.0091(19) -0.0029(18) C30 0.037(3) 0.017(2) 0.020(2) -0.0048(16) 0.0117(19) 0.0011(18) C39 0.033(2) 0.029(2) 0.021(2) -0.0017(17) 0.0184(19) -0.0037(19) C42 0.023(2) 0.034(3) 0.021(2) 0.0036(17) -0.0012(18) -0.0090(19) C7 0.026(2) 0.020(2) 0.018(2) -0.0023(15) 0.0095(17) 0.0023(17) C33 0.025(2) 0.024(2) 0.028(2) -0.0067(17) 0.0075(19) -0.0103(18) C14 0.031(2) 0.035(3) 0.019(2) 0.0028(17) 0.0130(19) -0.006(2) C44 0.030(2) 0.032(2) 0.018(2) -0.0030(17) 0.0073(18) -0.0089(19) C13 0.045(3) 0.026(3) 0.034(3) 0.0119(19) 0.020(2) 0.003(2) C16 0.027(2) 0.030(3) 0.027(2) -0.0004(18) -0.0037(19) 0.008(2) C43 0.044(3) 0.021(2) 0.028(2) -0.0083(18) 0.004(2) -0.005(2) I1 0.01890(13) 0.02625(15) 0.02481(14) 0.00290(10) 0.01071(11) 0.00160(11) 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' I I -0.4742 1.8119 '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 C35 U1 C3 110.98(11) . . ? C35 U1 C22 71.91(11) . . ? C35 U1 C5 68.48(11) . . ? C35 U1 C20 98.02(10) . . ? C35 U1 C19 117.50(10) . . ? C35 U1 C1 90.13(11) . . ? C35 U1 C2 117.37(11) . . ? C35 U1 C21 70.39(10) . . ? C35 U1 C18 101.17(11) . . ? C35 U1 C4 81.63(11) . . ? C35 U1 C40 158.35(11) . . ? C3 U1 C20 150.16(10) . . ? C3 U1 C19 128.96(10) . . ? C3 U1 C4 29.47(10) . . ? C22 U1 C3 146.62(10) . . ? C22 U1 C5 109.29(11) . . ? C22 U1 C20 49.39(10) . . ? C22 U1 C19 49.12(10) . . ? C22 U1 C21 30.11(10) . . ? C22 U1 C4 138.32(11) . . ? C5 U1 C3 48.77(10) . . ? C5 U1 C20 158.50(11) . . ? C5 U1 C19 142.42(11) . . ? C5 U1 C4 29.33(10) . . ? C20 U1 C4 170.24(10) . . ? C19 U1 C20 29.63(10) . . ? C19 U1 C4 156.87(10) . . ? C1 U1 C3 49.17(10) . . ? C1 U1 C22 98.62(11) . . ? C1 U1 C5 29.90(10) . . ? C1 U1 C20 140.78(11) . . ? C1 U1 C19 114.46(11) . . ? C1 U1 C2 30.22(10) . . ? C1 U1 C21 128.10(11) . . ? C1 U1 C18 91.81(11) . . ? C1 U1 C4 48.91(11) . . ? C2 U1 C3 29.79(10) . . ? C2 U1 C22 117.90(10) . . ? C2 U1 C5 49.42(10) . . ? C2 U1 C20 137.20(10) . . ? C2 U1 C19 108.06(10) . . ? C2 U1 C21 146.63(10) . . ? C2 U1 C4 49.06(10) . . ? C21 U1 C3 176.42(10) . . ? C21 U1 C5 130.58(10) . . ? C21 U1 C20 29.56(10) . . ? C21 U1 C19 48.75(10) . . ? C21 U1 C4 152.01(10) . . ? C18 U1 C3 127.29(10) . . ? C18 U1 C22 30.09(10) . . ? C18 U1 C5 115.32(11) . . ? C18 U1 C20 48.99(10) . . ? C18 U1 C19 29.39(10) . . ? C18 U1 C2 98.26(11) . . ? C18 U1 C21 49.21(10) . . ? C18 U1 C4 140.72(11) . . ? C40 U1 C3 71.71(11) . . ? C40 U1 C22 118.39(10) . . ? C40 U1 C5 120.02(11) . . ? C40 U1 C20 78.76(10) . . ? C40 U1 C19 69.28(10) . . ? C40 U1 C1 105.99(11) . . ? C40 U1 C2 76.20(11) . . ? C40 U1 C21 108.31(11) . . ? C40 U1 C18 92.84(11) . . ? C40 U1 C4 97.93(11) . . ? C35 N1 C36 176.2(4) . . ? F12 C59 C60 119.1(3) . . ? F12 C59 C58 120.6(4) . . ? C60 C59 C58 120.3(3) . . ? N2 C41 C42 107.0(3) . . ? N2 C41 C44 108.1(3) . . ? N2 C41 C43 107.4(3) . . ? C42 C41 C43 110.8(3) . . ? C44 C41 C42 111.9(3) . . ? C44 C41 C43 111.3(3) . . ? C58 C57 B1 127.1(3) . . ? C58 C57 C62 113.7(3) . . ? C62 C57 B1 118.8(3) . . ? F1 C46 C45 121.8(3) . . ? F1 C46 C47 114.7(3) . . ? C45 C46 C47 123.4(3) . . ? C40 N2 C41 176.4(4) . . ? C57 B1 C45 114.3(3) . . ? C57 B1 C63 113.4(3) . . ? C57 B1 C51 102.0(3) . . ? C45 B1 C63 101.9(3) . . ? C45 B1 C51 112.3(3) . . ? C63 B1 C51 113.5(3) . . ? C25 C23 C24 107.2(3) . . ? C19 C23 C25 114.3(3) . . ? C19 C23 C24 108.2(3) . . ? F20 C68 C63 121.5(3) . . ? F20 C68 C67 115.1(3) . . ? C63 C68 C67 123.4(3) . . ? N1 C35 U1 176.3(3) . . ? C2 C3 U1 72.4(2) . . ? C2 C3 C9 122.1(3) . . ? C2 C3 C4 108.1(3) . . ? C9 C3 U1 125.2(2) . . ? C4 C3 U1 76.5(2) . . ? C4 C3 C9 129.0(3) . . ? C32 C22 U1 123.8(2) . . ? C21 C22 U1 76.61(19) . . ? C21 C22 C32 128.2(3) . . ? C18 C22 U1 73.5(2) . . ? C18 C22 C32 124.3(3) . . ? C18 C22 C21 106.7(3) . . ? C46 C45 B1 126.9(3) . . ? C50 C45 C46 113.7(3) . . ? C50 C45 B1 119.0(3) . . ? C1 C5 U1 70.67(19) . . ? C1 C5 C4 107.2(3) . . ? C1 C5 C15 122.5(3) . . ? C4 C5 U1 76.8(2) . . ? C4 C5 C15 128.5(3) . . ? C15 C5 U1 129.7(2) . . ? C19 C20 U1 74.72(19) . . ? C19 C20 C26 128.1(3) . . ? C26 C20 U1 125.2(2) . . ? C21 C20 U1 74.11(19) . . ? C21 C20 C19 107.2(3) . . ? C21 C20 C26 123.7(3) . . ? C68 C63 B1 126.8(3) . . ? C64 C63 B1 119.3(3) . . ? C64 C63 C68 113.6(3) . . ? F16 C64 C63 119.3(3) . . ? F16 C64 C65 116.0(3) . . ? C65 C64 C63 124.7(3) . . ? F14 C61 C60 120.1(3) . . ? F14 C61 C62 120.7(3) . . ? C62 C61 C60 119.3(3) . . ? C4 C12 C14 116.6(3) . . ? C4 C12 C13 112.3(3) . . ? C14 C12 C13 108.5(3) . . ? C23 C19 U1 132.0(2) . . ? C20 C19 U1 75.66(19) . . ? C20 C19 C23 127.0(3) . . ? C18 C19 U1 71.5(2) . . ? C18 C19 C23 123.0(3) . . ? C18 C19 C20 107.8(3) . . ? C52 C51 B1 119.4(3) . . ? C56 C51 B1 127.2(3) . . ? C56 C51 C52 113.3(3) . . ? C22 C32 C34 111.3(3) . . ? C33 C32 C22 111.4(3) . . ? C33 C32 C34 108.3(3) . . ? C28 C26 C20 116.7(3) . . ? C28 C26 C27 107.6(3) . . ? C20 C26 C27 112.2(3) . . ? C2 C6 C8 112.2(3) . . ? C2 C6 C7 111.2(3) . . ? C8 C6 C7 107.8(3) . . ? C5 C1 U1 79.4(2) . . ? C2 C1 U1 76.8(2) . . ? C2 C1 C5 109.5(3) . . ? C3 C2 U1 77.8(2) . . ? C3 C2 C6 128.9(3) . . ? C6 C2 U1 122.0(2) . . ? C1 C2 U1 73.0(2) . . ? C1 C2 C3 107.3(3) . . ? C1 C2 C6 123.2(3) . . ? F6 C52 C51 119.0(3) . . ? F6 C52 C53 116.4(3) . . ? C53 C52 C51 124.6(3) . . ? C22 C21 U1 73.28(19) . . ? C22 C21 C29 121.9(3) . . ? C20 C21 U1 76.3(2) . . ? C20 C21 C22 108.3(3) . . ? C20 C21 C29 127.9(3) . . ? C29 C21 U1 128.9(2) . . ? F9 C55 C56 120.5(3) . . ? F9 C55 C54 119.1(3) . . ? C54 C55 C56 120.4(3) . . ? F5 C50 C45 118.9(3) . . ? F5 C50 C49 116.7(3) . . ? C49 C50 C45 124.4(3) . . ? N1 C36 C38 107.7(3) . . ? N1 C36 C37 107.9(3) . . ? N1 C36 C39 106.0(3) . . ? C38 C36 C39 111.9(3) . . ? C37 C36 C38 111.5(3) . . ? C37 C36 C39 111.7(3) . . ? C31 C29 C30 108.2(3) . . ? C21 C29 C31 119.6(3) . . ? C21 C29 C30 109.2(3) . . ? F10 C56 C51 121.6(3) . . ? F10 C56 C55 114.9(3) . . ? C51 C56 C55 123.6(3) . . ? C3 C9 C10 111.5(3) . . ? C3 C9 C11 118.8(3) . . ? C11 C9 C10 108.1(3) . . ? F8 C54 C55 120.2(3) . . ? F8 C54 C53 121.8(3) . . ? C55 C54 C53 118.0(3) . . ? F3 C48 C47 120.8(3) . . ? F3 C48 C49 119.5(3) . . ? C47 C48 C49 119.6(3) . . ? F13 C60 C59 120.8(4) . . ? F13 C60 C61 120.4(4) . . ? C59 C60 C61 118.7(4) . . ? F11 C58 C59 115.3(3) . . ? F11 C58 C57 121.3(3) . . ? C59 C58 C57 123.5(3) . . ? C22 C18 U1 76.4(2) . . ? C19 C18 U1 79.1(2) . . ? C19 C18 C22 110.0(3) . . ? F15 C62 C57 119.5(3) . . ? F15 C62 C61 116.0(3) . . ? C61 C62 C57 124.5(3) . . ? C3 C4 U1 74.0(2) . . ? C3 C4 C12 123.4(3) . . ? C5 C4 U1 73.92(19) . . ? C5 C4 C3 107.9(3) . . ? C5 C4 C12 128.1(3) . . ? C12 C4 U1 125.2(2) . . ? F7 C53 C52 120.5(3) . . ? F7 C53 C54 119.5(3) . . ? C52 C53 C54 120.0(3) . . ? N2 C40 U1 176.6(3) . . ? C5 C15 C17 114.2(3) . . ? C5 C15 C16 108.9(3) . . ? C17 C15 C16 108.7(3) . . ? F17 C65 C64 120.4(3) . . ? F17 C65 C66 120.2(3) . . ? C66 C65 C64 119.3(3) . . ? F2 C47 C46 120.2(3) . . ? F2 C47 C48 120.1(3) . . ? C48 C47 C46 119.6(3) . . ? F4 C49 C50 120.6(3) . . ? F4 C49 C48 120.2(3) . . ? C48 C49 C50 119.1(3) . . ? F19 C67 C68 120.6(3) . . ? F19 C67 C66 119.7(3) . . ? C66 C67 C68 119.6(3) . . ? F18 C66 C65 120.6(4) . . ? F18 C66 C67 120.1(3) . . ? C65 C66 C67 119.3(3) . . ? 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 C35 2.584(4) . ? U1 C3 2.803(4) . ? U1 C22 2.745(3) . ? U1 C5 2.799(3) . ? U1 C20 2.818(3) . ? U1 C19 2.805(3) . ? U1 C1 2.686(3) . ? U1 C2 2.735(3) . ? U1 C21 2.789(3) . ? U1 C18 2.709(3) . ? U1 C4 2.835(3) . ? U1 C40 2.613(4) . ? F1 C46 1.345(4) . ? F15 C62 1.351(4) . ? F16 C64 1.361(4) . ? F10 C56 1.354(4) . ? F7 C53 1.354(4) . ? F6 C52 1.352(4) . ? F5 C50 1.354(4) . ? F20 C68 1.342(4) . ? F4 C49 1.346(4) . ? F3 C48 1.349(4) . ? F11 C58 1.357(4) . ? F9 C55 1.346(4) . ? F8 C54 1.334(4) . ? F2 C47 1.344(4) . ? F19 C67 1.338(4) . ? F13 C60 1.348(4) . ? F14 C61 1.348(4) . ? F17 C65 1.346(4) . ? F12 C59 1.356(4) . ? F18 C66 1.346(4) . ? N1 C35 1.143(4) . ? N1 C36 1.477(4) . ? C59 C60 1.367(6) . ? C59 C58 1.381(5) . ? C41 N2 1.476(5) . ? C41 C42 1.519(6) . ? C41 C44 1.514(5) . ? C41 C43 1.523(6) . ? C57 B1 1.655(5) . ? C57 C58 1.381(5) . ? C57 C62 1.389(5) . ? C38 C36 1.522(5) . ? C31 C29 1.532(5) . ? C10 C9 1.538(5) . ? C46 C45 1.390(5) . ? C46 C47 1.391(5) . ? N2 C40 1.154(5) . ? B1 C45 1.658(5) . ? B1 C63 1.659(5) . ? B1 C51 1.661(5) . ? C23 C25 1.538(5) . ? C23 C19 1.522(5) . ? C23 C24 1.538(5) . ? C68 C63 1.391(5) . ? C68 C67 1.393(5) . ? C3 C2 1.425(5) . ? C3 C9 1.530(5) . ? C3 C4 1.434(5) . ? C22 C32 1.527(5) . ? C22 C21 1.438(5) . ? C22 C18 1.416(5) . ? C45 C50 1.389(5) . ? C5 C1 1.419(5) . ? C5 C4 1.427(5) . ? C5 C15 1.521(5) . ? C11 C9 1.533(5) . ? C28 C26 1.526(5) . ? C20 C19 1.438(5) . ? C20 C26 1.527(5) . ? C20 C21 1.430(5) . ? C63 C64 1.388(5) . ? C64 C65 1.375(5) . ? C61 C60 1.375(6) . ? C61 C62 1.373(5) . ? C12 C4 1.530(5) . ? C12 C14 1.533(5) . ? C12 C13 1.547(6) . ? C19 C18 1.402(5) . ? C51 C52 1.397(5) . ? C51 C56 1.384(5) . ? C32 C34 1.528(5) . ? C32 C33 1.522(5) . ? C26 C27 1.540(5) . ? C6 C2 1.523(5) . ? C6 C8 1.530(5) . ? C6 C7 1.538(5) . ? C1 C2 1.414(5) . ? C52 C53 1.370(5) . ? C21 C29 1.528(5) . ? C55 C56 1.391(5) . ? C55 C54 1.376(5) . ? C50 C49 1.380(5) . ? C36 C37 1.521(5) . ? C36 C39 1.525(5) . ? C29 C30 1.540(5) . ? C54 C53 1.378(5) . ? C48 C47 1.367(5) . ? C48 C49 1.370(5) . ? C15 C17 1.526(5) . ? C15 C16 1.534(5) . ? C65 C66 1.372(5) . ? C67 C66 1.373(5) . ?