#------------------------------------------------------------------------------ #$Date: 2024-07-09 00:42:20 +0300 (Tue, 09 Jul 2024) $ #$Revision: 293301 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572065.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_1572065 loop_ _publ_author_name 'K\"orner, Lukas' 'Bockfeld, Dirk' 'Bannenberg, Thomas' 'Tamm, Matthias' _publ_section_title ; 2,3-Diamino-4,5-diarylcyclopentadienone iron carbonyl complexes as catalysts for reductive amination reactions ; _journal_name_full 'Catalysis Science & Technology' _journal_paper_doi 10.1039/D4CY00372A _journal_year 2024 _chemical_formula_moiety 'C29 H28 F6 N2 O' _chemical_formula_sum 'C29 H28 F6 N2 O' _chemical_formula_weight 534.53 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-03-06 deposited with the CCDC. 2024-07-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 18.6211(6) _cell_length_b 16.9942(4) _cell_length_c 32.0027(8) _cell_measurement_reflns_used 13841 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 73.8480 _cell_measurement_theta_min 2.7510 _cell_volume 10127.3(5) _computing_cell_refinement 'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)' _computing_publication_material 'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)' _computing_structure_refinement 'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)' _computing_structure_solution 'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.971 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_unetI/netI 0.0522 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.971 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_number 26477 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.971 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.274 _diffrn_reflns_theta_min 2.761 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.990 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.64a (Rigaku Oxford Diffraction, 2022) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.402 _exptl_crystal_description plate _exptl_crystal_F_000 4448 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.030 _refine_diff_density_max 0.385 _refine_diff_density_min -0.255 _refine_diff_density_rms 0.055 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 742 _refine_ls_number_reflns 26477 _refine_ls_number_restraints 42 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0622 _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^)+(0.0925P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1503 _refine_ls_wR_factor_ref 0.1727 _reflns_Friedel_coverage 0.000 _reflns_number_gt 16008 _reflns_number_total 26477 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4cy00372a3.cif _cod_data_source_block lk44db _cod_database_code 1572065 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.908 _shelx_estimated_absorpt_t_max 0.971 _oxdiff_exptl_absorpt_empirical_full_min 0.729 _oxdiff_exptl_absorpt_empirical_full_max 1.485 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _shelx_res_file ; TITL lk44db_a.res in Pbca lk44db.res created by SHELXL-2018/3 at 19:24:55 on 26-Jul-2023 REM Old TITL lk44db_twin1_hklf4 in Pbca REM SHELXT solution in Pbca: R1 0.215, Rweak 0.018, 0.033 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C58 N4 O2 F6B CELL 1.54184 18.6211 16.9942 32.0027 90 90 90 ZERR 16 0.0006 0.0004 0.0008 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H F N O UNIT 464 448 96 32 16 ISOR 0.001 0.002 F1B F2B F3B F4B F5B F6B F3A L.S. 4 0 0 PLAN 10 SIZE 0.03 0.05 0.1 TEMP -173 CONF list 4 fmap 2 53 acta MERG 0 REM REM REM WGHT 0.092500 BASF 0.48527 FVAR 0.40368 0.80845 0.89750 F1 3 0.318175 0.192861 0.256301 11.00000 0.08687 0.10263 = 0.05204 -0.02192 -0.03041 0.03491 F2 3 0.348649 0.079086 0.276051 11.00000 0.17567 0.05067 = 0.05199 -0.01923 0.01272 -0.03309 F3 3 0.427345 0.160209 0.255295 11.00000 0.06796 0.09466 = 0.04005 -0.01984 0.00344 -0.00402 F4 3 0.357779 0.633252 0.340552 11.00000 0.06281 0.06592 = 0.12874 0.05413 -0.02614 -0.01137 F5 3 0.460980 0.593735 0.324090 11.00000 0.13431 0.05826 = 0.05125 0.01017 0.03635 0.01397 F6 3 0.449006 0.673522 0.373837 11.00000 0.11528 0.03825 = 0.05023 0.00265 -0.00450 -0.02615 O1 5 0.404915 0.391512 0.531100 11.00000 0.05688 0.03065 = 0.03718 -0.00355 -0.00308 -0.00162 N1 4 0.387994 0.220935 0.562006 11.00000 0.04809 0.03218 = 0.02795 -0.00280 0.00162 0.00480 N2 4 0.383687 0.127722 0.478137 11.00000 0.04715 0.02637 = 0.03506 -0.00062 0.00794 0.00046 C1 1 0.399076 0.333667 0.508316 11.00000 0.03654 0.02942 = 0.03468 -0.00315 -0.00238 -0.00063 C2 1 0.389108 0.250177 0.520655 11.00000 0.03919 0.03048 = 0.03353 -0.00118 0.00034 0.00200 C3 1 0.390407 0.207432 0.484768 11.00000 0.03873 0.02907 = 0.03239 0.00132 0.00088 0.00165 C4 1 0.395831 0.261963 0.447532 11.00000 0.03512 0.03290 = 0.03455 0.00098 0.00081 0.00079 C5 1 0.401441 0.336617 0.461279 11.00000 0.03813 0.03035 = 0.03219 -0.00104 0.00032 -0.00161 C6 1 0.365741 0.275511 0.594920 11.00000 0.04905 0.03386 = 0.03374 -0.00345 0.00157 0.00493 AFIX 23 H6A 2 0.323012 0.305391 0.585590 11.00000 -1.20000 H6B 2 0.404860 0.313526 0.600520 11.00000 -1.20000 AFIX 0 C7 1 0.348084 0.230766 0.634566 11.00000 0.05314 0.04192 = 0.03554 -0.00375 0.00480 0.00013 AFIX 23 H7A 2 0.335179 0.268527 0.656893 11.00000 -1.20000 H7B 2 0.306087 0.196327 0.629528 11.00000 -1.20000 AFIX 0 C8 1 0.410689 0.181469 0.648709 11.00000 0.06849 0.04968 = 0.03493 0.00592 0.00199 0.00881 AFIX 23 H8A 2 0.395924 0.148420 0.672692 11.00000 -1.20000 H8B 2 0.450168 0.216266 0.658083 11.00000 -1.20000 AFIX 0 C9 1 0.437313 0.128847 0.613265 11.00000 0.05785 0.04355 = 0.04068 0.00768 0.00217 0.00902 AFIX 23 H9A 2 0.481651 0.101376 0.622130 11.00000 -1.20000 H9B 2 0.400521 0.088560 0.606863 11.00000 -1.20000 AFIX 0 C10 1 0.452570 0.177166 0.574378 11.00000 0.04206 0.03991 = 0.03904 0.00016 -0.00039 0.00586 AFIX 23 H10C 2 0.492266 0.214436 0.580014 11.00000 -1.20000 H10D 2 0.467573 0.141947 0.551335 11.00000 -1.20000 AFIX 0 C11 1 0.345287 0.077829 0.508206 11.00000 0.05714 0.03072 = 0.03668 -0.00076 0.00781 -0.00386 AFIX 23 H11C 2 0.308354 0.109118 0.523007 11.00000 -1.20000 H11D 2 0.379309 0.056721 0.529169 11.00000 -1.20000 AFIX 0 C12 1 0.309928 0.010459 0.484512 11.00000 0.06689 0.03644 = 0.04789 0.00021 0.00238 -0.01122 AFIX 23 H12C 2 0.273813 0.031785 0.464836 11.00000 -1.20000 H12D 2 0.284911 -0.024628 0.504460 11.00000 -1.20000 AFIX 0 C13 1 0.366213 -0.036450 0.460343 11.00000 0.08540 0.03162 = 0.05176 -0.00782 0.00498 -0.00407 AFIX 23 H13C 2 0.399455 -0.062115 0.480270 11.00000 -1.20000 H13D 2 0.342175 -0.078173 0.443897 11.00000 -1.20000 AFIX 0 C14 1 0.408792 0.016849 0.431005 11.00000 0.08483 0.03231 = 0.04620 -0.00608 0.01392 0.00696 AFIX 23 H14C 2 0.448354 -0.013532 0.418091 11.00000 -1.20000 H14D 2 0.377008 0.035927 0.408371 11.00000 -1.20000 AFIX 0 C15 1 0.439552 0.086537 0.454559 11.00000 0.05137 0.03331 = 0.04212 0.00007 0.00778 0.00741 AFIX 23 H15C 2 0.477262 0.067998 0.474017 11.00000 -1.20000 H15D 2 0.462040 0.123422 0.434507 11.00000 -1.20000 AFIX 0 C16 1 0.388433 0.235645 0.403779 11.00000 0.03911 0.02889 = 0.03356 0.00141 -0.00007 0.00217 C17 1 0.330247 0.189864 0.391468 11.00000 0.03958 0.04102 = 0.04083 -0.00354 0.00525 -0.00174 AFIX 43 H17 2 0.294670 0.175821 0.411395 11.00000 -1.20000 AFIX 0 C18 1 0.323503 0.164447 0.350460 11.00000 0.04225 0.04352 = 0.04258 -0.00598 -0.00402 -0.00362 AFIX 43 H18 2 0.283050 0.134002 0.342351 11.00000 -1.20000 AFIX 0 C19 1 0.375257 0.183269 0.321598 11.00000 0.04323 0.03524 = 0.03446 -0.00289 -0.00389 0.00547 C20 1 0.433394 0.229299 0.333315 11.00000 0.04242 0.03741 = 0.03449 0.00162 0.00064 0.00284 AFIX 43 H20 2 0.468972 0.242942 0.313312 11.00000 -1.20000 AFIX 0 C21 1 0.439586 0.255317 0.374064 11.00000 0.03724 0.03432 = 0.03336 0.00015 -0.00157 0.00015 AFIX 43 H21 2 0.479390 0.287086 0.381823 11.00000 -1.20000 AFIX 0 C22 1 0.367600 0.154719 0.277446 11.00000 0.05034 0.04456 = 0.04085 -0.00515 -0.00301 0.00209 C23 1 0.403710 0.409822 0.436552 11.00000 0.03941 0.03065 = 0.03034 -0.00308 0.00072 -0.00004 C24 1 0.351689 0.424902 0.406535 11.00000 0.04223 0.03190 = 0.04507 0.00087 -0.00429 -0.00446 AFIX 43 H24 2 0.312966 0.389097 0.403064 11.00000 -1.20000 AFIX 0 C25 1 0.355367 0.491270 0.381597 11.00000 0.04311 0.03876 = 0.04074 0.00103 -0.00666 -0.00027 AFIX 43 H25 2 0.319003 0.501325 0.361472 11.00000 -1.20000 AFIX 0 C26 1 0.412357 0.543013 0.386117 11.00000 0.04326 0.02903 = 0.03460 -0.00434 0.00087 -0.00012 C27 1 0.463521 0.529896 0.416704 11.00000 0.04428 0.02909 = 0.03626 -0.00552 0.00099 -0.00164 AFIX 43 H27 2 0.502090 0.565904 0.420163 11.00000 -1.20000 AFIX 0 C28 1 0.458600 0.464414 0.442266 11.00000 0.04007 0.03071 = 0.03358 -0.00450 -0.00407 -0.00027 AFIX 43 H28 2 0.492900 0.456666 0.463852 11.00000 -1.20000 AFIX 0 C29 1 0.419943 0.610467 0.356629 11.00000 0.04704 0.03717 = 0.03923 -0.00423 -0.00219 -0.00441 O1A 5 0.610223 0.108690 0.411782 11.00000 0.05194 0.03333 = 0.03849 0.00459 0.00268 -0.00269 N1A 4 0.655782 0.264982 0.449612 11.00000 0.04141 0.03664 = 0.03031 0.00193 -0.00202 0.00146 N2A 4 0.668370 0.372399 0.371304 11.00000 0.04610 0.02483 = 0.03397 -0.00093 -0.00575 0.00230 C1A 1 0.627756 0.166426 0.391144 11.00000 0.03546 0.03013 = 0.03712 -0.00042 0.00111 0.00242 C2A 1 0.651486 0.243845 0.406682 11.00000 0.03784 0.03275 = 0.03337 -0.00171 -0.00036 -0.00011 C3A 1 0.653993 0.293365 0.373139 11.00000 0.03559 0.02899 = 0.03617 -0.00363 -0.00370 0.00061 C4A 1 0.640742 0.246548 0.333332 11.00000 0.03480 0.03132 = 0.03263 -0.00199 -0.00091 0.00198 C5A 1 0.625443 0.171662 0.344144 11.00000 0.03601 0.02932 = 0.03344 -0.00035 -0.00076 0.00034 C6A 1 0.692613 0.208287 0.476534 11.00000 0.04472 0.04877 = 0.03469 0.00406 0.00026 0.00734 AFIX 23 H6AA 2 0.738385 0.192045 0.463372 11.00000 -1.20000 H6AB 2 0.662345 0.160860 0.480073 11.00000 -1.20000 AFIX 0 C7A 1 0.707519 0.244864 0.518769 11.00000 0.04668 0.05305 = 0.03571 0.00607 -0.00392 -0.00161 AFIX 23 H7AA 2 0.731429 0.205749 0.536989 11.00000 -1.20000 H7AB 2 0.740428 0.290149 0.515302 11.00000 -1.20000 AFIX 0 C8A 1 0.639273 0.272125 0.539097 11.00000 0.05406 0.05774 = 0.03333 -0.00401 -0.00021 -0.00156 AFIX 23 H8AA 2 0.650647 0.300121 0.565405 11.00000 -1.20000 H8AB 2 0.608963 0.226076 0.546025 11.00000 -1.20000 AFIX 0 C9A 1 0.598507 0.326769 0.509910 11.00000 0.05582 0.06211 = 0.04178 -0.01326 -0.00267 0.01261 AFIX 23 H9AA 2 0.551326 0.339933 0.522338 11.00000 -1.20000 H9AB 2 0.625815 0.376290 0.506308 11.00000 -1.20000 AFIX 0 C10A 1 0.587360 0.288154 0.467678 11.00000 0.04268 0.04960 = 0.04273 -0.00525 -0.00214 0.00822 AFIX 23 H10A 2 0.556390 0.241205 0.470945 11.00000 -1.20000 H10B 2 0.562765 0.325386 0.448671 11.00000 -1.20000 AFIX 0 C11A 1 0.704224 0.411037 0.406511 11.00000 0.05793 0.03110 = 0.03643 -0.00285 -0.00775 -0.00443 AFIX 23 H11A 2 0.738352 0.374099 0.419850 11.00000 -1.20000 H11B 2 0.668243 0.427022 0.427644 11.00000 -1.20000 AFIX 0 C12A 1 0.744318 0.483137 0.390564 11.00000 0.06425 0.03206 = 0.04486 -0.00462 -0.00833 -0.00785 AFIX 23 H12A 2 0.767708 0.510262 0.414318 11.00000 -1.20000 H12B 2 0.782287 0.466406 0.370817 11.00000 -1.20000 AFIX 0 C13A 1 0.693658 0.539475 0.368800 11.00000 0.06782 0.02924 = 0.04812 -0.00270 0.00454 0.00203 AFIX 23 H13A 2 0.721127 0.584702 0.357632 11.00000 -1.20000 H13B 2 0.658137 0.559835 0.389120 11.00000 -1.20000 AFIX 0 C14A 1 0.654790 0.498050 0.333250 11.00000 0.05999 0.03200 = 0.04599 0.00476 -0.00246 0.00669 AFIX 23 H14A 2 0.689667 0.484133 0.311103 11.00000 -1.20000 H14B 2 0.618635 0.534005 0.321009 11.00000 -1.20000 AFIX 0 C15A 1 0.617721 0.423637 0.348902 11.00000 0.04561 0.03279 = 0.04029 -0.00193 -0.00361 0.00579 AFIX 23 H15A 2 0.577812 0.438264 0.367807 11.00000 -1.20000 H15B 2 0.597165 0.394667 0.324876 11.00000 -1.20000 AFIX 0 C16A 1 0.648687 0.277233 0.290391 11.00000 0.03779 0.02839 = 0.03277 -0.00169 -0.00176 0.00214 C17A 1 0.706817 0.324741 0.279380 11.00000 0.04034 0.03357 = 0.03889 -0.00135 -0.00392 -0.00246 AFIX 43 H17A 2 0.742017 0.337550 0.299763 11.00000 -1.20000 AFIX 0 C18A 1 0.713749 0.353341 0.239195 11.00000 0.04328 0.03607 = 0.04350 0.00145 0.00236 -0.00513 AFIX 43 H18A 2 0.753838 0.385171 0.232025 11.00000 -1.20000 AFIX 0 C19A 1 0.662463 0.335754 0.209357 11.00000 0.04356 0.03459 = 0.03538 0.00224 0.00518 0.00332 C20A 1 0.604825 0.287827 0.219536 11.00000 0.04248 0.04010 = 0.03357 -0.00198 -0.00341 0.00072 AFIX 43 H20A 2 0.569816 0.275067 0.199034 11.00000 -1.20000 AFIX 0 C21A 1 0.598623 0.258787 0.259608 11.00000 0.03825 0.03343 = 0.03391 -0.00191 -0.00079 -0.00100 AFIX 43 H21A 2 0.559332 0.225469 0.266354 11.00000 -1.20000 AFIX 0 C22A 1 0.669115 0.367167 0.166194 11.00000 0.05042 0.04971 = 0.04383 0.00645 0.00063 -0.00595 C23A 1 0.614172 0.103313 0.316657 11.00000 0.04067 0.02572 = 0.03413 0.00312 -0.00281 -0.00060 C24A 1 0.661836 0.087055 0.284152 11.00000 0.03796 0.03105 = 0.04013 0.00025 0.00170 -0.00077 AFIX 43 H24A 2 0.703514 0.118624 0.280678 11.00000 -1.20000 AFIX 0 C25A 1 0.648986 0.025354 0.256907 11.00000 0.04261 0.03465 = 0.03548 -0.00075 0.00016 0.00000 AFIX 43 H25A 2 0.681664 0.014676 0.234827 11.00000 -1.20000 AFIX 0 C26A 1 0.588166 -0.020802 0.262002 11.00000 0.04561 0.03157 = 0.03223 0.00343 -0.00596 -0.00261 C27A 1 0.540978 -0.006208 0.294633 11.00000 0.04231 0.03076 = 0.04245 0.00531 -0.00348 -0.00711 AFIX 43 H27A 2 0.499501 -0.038099 0.298091 11.00000 -1.20000 AFIX 0 C28A 1 0.554419 0.054927 0.322167 11.00000 0.04037 0.03385 = 0.03640 0.00346 0.00272 -0.00218 AFIX 43 H28A 2 0.522749 0.063955 0.344941 11.00000 -1.20000 AFIX 0 C29A 1 0.571580 -0.085800 0.232158 11.00000 0.05914 0.03554 = 0.03605 0.00310 -0.00708 -0.01006 PART 1 F1A 3 0.707425 0.319728 0.141001 21.00000 0.13300 0.06504 = 0.04580 0.00880 0.04131 0.02620 F2A 3 0.701789 0.435912 0.163845 21.00000 0.13100 0.04169 = 0.05111 0.01592 0.01261 -0.01974 F3A 3 0.607525 0.373049 0.146079 21.00000 0.06706 0.13328 = 0.06543 0.04872 -0.00612 -0.00975 PART 2 F1B 3 0.649457 0.324940 0.137832 -21.00000 0.07691 0.06888 = 0.06291 -0.00165 -0.00006 0.00003 F2B 3 0.727176 0.399982 0.159108 -21.00000 0.08188 0.08615 = 0.08108 0.00585 -0.00009 -0.00696 F3B 3 0.618948 0.428193 0.161375 -21.00000 0.05796 0.05488 = 0.05097 0.00923 0.00239 0.00854 PART 3 F4A 3 0.620600 -0.093552 0.201677 31.00000 0.08147 0.08168 = 0.05794 -0.03677 0.01944 -0.03203 F5A 3 0.510574 -0.077312 0.212874 31.00000 0.06932 0.09235 = 0.12190 -0.05442 -0.05377 0.01491 F6A 3 0.570724 -0.155735 0.250212 31.00000 0.18796 0.03143 = 0.04050 -0.00381 -0.00711 -0.01829 PART 4 F4B 3 0.564399 -0.067895 0.197521 -31.00000 0.05247 0.05104 = 0.04824 -0.00010 -0.00076 -0.00302 F5B 3 0.512627 -0.123255 0.244591 -31.00000 0.05054 0.04846 = 0.05008 -0.00218 -0.00155 -0.00284 F6B 3 0.618846 -0.136738 0.236319 -31.00000 0.06712 0.06580 = 0.06949 -0.00370 -0.00120 0.00173 HKLF 5 REM lk44db_a.res in Pbca REM wR2 = 0.1727, GooF = S = 1.015, Restrained GooF = 1.042 for all data REM R1 = 0.0622 for 16008 Fo > 4sig(Fo) and 0.1081 for all 26477 data REM 742 parameters refined using 42 restraints END WGHT 0.0925 0.0000 REM Highest difference peak 0.385, deepest hole -0.255, 1-sigma level 0.055 Q1 1 0.6161 0.3349 0.1393 11.00000 0.05 0.38 Q2 1 0.7411 0.3458 0.1599 11.00000 0.05 0.37 Q3 1 0.3990 0.6083 0.3198 11.00000 0.05 0.32 Q4 1 0.4882 0.6258 0.3450 11.00000 0.05 0.30 Q5 1 0.3916 0.6771 0.3815 11.00000 0.05 0.30 Q6 1 0.6029 0.4063 0.1580 11.00000 0.05 0.25 Q7 1 0.3776 0.1794 0.2386 11.00000 0.05 0.24 Q8 1 0.6287 -0.1154 0.2171 11.00000 0.05 0.24 Q9 1 0.3975 0.3395 0.4783 11.00000 0.05 0.23 Q10 1 0.3176 0.1783 0.3164 11.00000 0.05 0.22 ; _shelx_res_checksum 78460 _shelx_hkl_file ; 0 0 2 1296.92 5.54171 -2 0 0 2 1296.92 5.54171 1 0 0 4 12.4356 5.00687 1 0 0 -6 43.9103 11.0939 1 0 0 -8 11785.7 56.0033 1 0 0 -10 6545.00 48.8214 1 0 0 -12 430.916 20.2258 1 0 0 -14 904.053 26.3197 1 0 0 -16 1467.88 34.5875 1 0 0 -18 19.0107 17.9224 1 0 0 -20 6.99337 7.28864 1 0 0 -22 305.033 6.29947 1 0 0 24 368.816 8.81457 1 0 0 -26 1520.46 12.1224 1 0 0 28 16.9114 6.78227 1 0 0 30 108.193 8.68288 1 0 0 -32 6.71562 8.13148 1 0 0 -34 8.05418 8.94623 1 0 0 -36 67.4834 7.57560 1 0 0 -38 107.074 5.85823 1 0 2 0 27766.4 32.5921 -2 0 -2 0 27766.4 32.5921 1 0 2 1 473.716 10.5926 1 0 2 1 872.036 15.5611 -2 0 -2 1 872.036 15.5611 1 0 -2 2 2913.13 14.9055 1 0 2 2 5440.06 30.2814 -2 0 -2 2 5440.06 30.2814 1 0 2 3 72.2375 4.98578 1 0 2 3 120.656 8.98296 -2 0 -2 3 120.656 8.98296 1 0 2 4 522.133 6.78189 1 0 2 4 971.532 12.2284 -2 0 -2 4 971.532 12.2284 1 0 -2 5 120.987 5.36718 1 0 2 5 196.376 9.27375 -2 0 -2 5 196.376 9.27375 1 0 2 6 141.598 7.43544 1 0 2 6 249.234 9.40554 -2 0 -2 6 249.234 9.40554 1 0 -2 -7 938.679 14.0580 1 0 2 7 1879.76 19.5869 -2 0 -2 7 1879.76 19.5869 1 0 -2 -8 3860.53 22.8084 1 0 2 8 7275.75 31.2435 -2 0 -2 8 7275.75 31.2435 1 0 -2 -9 146.805 5.51712 1 0 -2 -10 2347.17 11.4905 1 0 2 -11 474.475 5.39688 1 0 2 -12 192.173 17.1867 1 0 2 -13 9763.10 69.1631 1 0 2 -14 92.5764 17.1070 1 0 2 -15-5.91212 16.1452 1 0 2 -16 70.3668 17.5378 1 0 2 -17 20.4177 17.9279 1 0 2 -18 500.829 26.1553 1 0 2 -19 678.481 29.2651 1 0 -2 -20 106.993 5.19818 1 0 -2 -21 580.504 6.41281 1 0 -2 22 9.01126 4.40011 1 0 -2 23 197.362 5.47726 1 0 2 24 2.63340 4.18315 1 0 2 -25 10.3649 4.36661 1 0 2 -26 783.234 7.20053 1 0 2 27 4.23320 4.11698 1 0 -2 -28 12.4736 4.16263 1 0 -2 29 199.904 5.29258 1 0 -2 30 17.8877 4.59971 1 0 -2 -31 147.139 5.25926 1 0 2 -32 80.2933 6.27725 1 0 2 -33 9.83560 5.74264 1 0 -2 34 185.380 5.99228 1 0 -2 -35 26.6514 4.94067 1 0 -2 -36 7.50180 4.35243 1 0 2 37 8.28612 4.75238 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1559.06 23.5138 1 0 -8 14 609.200 14.7953 1 0 -8 -15 299.543 8.18763 1 0 -8 -16 18.6209 5.14857 1 0 -8 17 354.972 7.83465 1 0 -8 18 50.9429 4.46618 1 0 -8 19 362.299 5.90672 1 0 -8 -20 23.0135 4.66449 1 0 -8 -21 622.152 7.17323 1 0 -8 22 92.3231 5.21217 1 0 -8 -23 10.6425 4.86474 1 0 -8 -24 16.4595 6.17664 1 0 8 25 8.74142 6.21138 1 0 -8 -26 160.682 6.35512 1 0 -8 -27 197.147 6.84752 1 0 -8 -28 493.193 8.01492 1 0 -8 -29 39.3985 5.70365 1 0 8 -30 48.8370 5.52063 1 0 8 -31 13.3504 5.04683 1 0 -8 -32 49.1453 4.65736 1 0 -8 33 21.9794 5.54451 1 0 -8 34 24.5273 6.87118 1 0 -8 35 12.9044 6.10615 1 0 -8 36 11.7461 5.06258 1 0 -8 37 5.44556 3.87600 1 0 10 1 135.707 20.0056 -2 0 -10 0 135.707 20.0056 1 0 -10 0 50.9643 28.1893 -2 0 10 1 50.9643 28.1893 1 0 10 2 109.168 20.1591 -2 0 -10 1 109.168 20.1591 1 0 -10 1 98.7960 27.0384 -2 0 10 2 98.7960 27.0384 1 0 -10 -3 246.141 21.6681 -2 0 10 -2 246.141 21.6681 1 0 -10 3 229.956 22.3461 1 0 -10 2 196.275 28.2092 -2 0 10 3 196.275 28.2092 1 0 -10 -4 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4.15251 2 2 3 37-3.21455 4.62042 2 2 3 38 6.94910 6.63613 2 2 3 39-4.89506 5.13575 2 2 4 0 619.332 17.5239 2 -2 -4 1 68.4199 8.19417 2 -2 -4 2 1209.26 8.12269 2 -2 -4 3 3725.02 11.0787 2 -2 -4 4 100.120 3.99974 2 -2 -4 5 7.06942 4.74039 2 -2 -4 6 195.691 5.65969 2 2 4 7 567.911 5.76288 2 2 4 8 984.153 8.55889 2 -2 -4 9 474.211 6.70692 2 -2 -4 10 12.0241 4.60406 2 -2 4 -11 1106.05 8.35135 2 -2 4 12 2.95469 4.86754 2 -2 4 13 4425.22 14.3470 2 -2 4 14 878.622 7.95322 2 2 -4 -15 154.601 8.39194 2 2 -4 -16 160.953 8.41540 2 2 -4 -17 151.331 8.57006 2 2 4 18 24.3481 5.89614 2 2 4 19 84.0385 4.48096 2 -2 4 20-0.84332 3.65712 2 2 4 -21-2.40666 3.56720 2 -2 4 22 9.85723 3.56875 2 -2 4 23 96.0477 4.01322 2 -2 4 24 12.4655 3.85965 2 -2 4 -25 91.2432 4.34332 2 -2 4 -26 29.0612 4.25751 2 -2 4 -27 4.86883 4.22713 2 -2 4 -28 77.6853 4.56238 2 -2 4 -29 89.7494 4.16548 2 2 4 30 67.9622 4.17617 2 -2 4 -31 2.77834 3.99528 2 -2 4 -32 24.0031 3.90631 2 -2 4 -33 14.5569 4.18329 2 2 4 34 10.8991 3.68819 2 2 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45.9624 4.75783 2 -2 6 -33 0.48398 4.75278 2 2 6 -34 37.4667 4.75873 2 -2 6 35 2.68795 4.09894 2 -2 6 36-6.25916 4.86976 2 -2 6 37 6.86034 4.05221 2 -2 6 38 2.69518 6.95156 2 -2 -7 0 270.775 16.0495 2 -2 -7 1 653.077 11.1466 2 -2 -7 2 1755.77 12.9382 2 -2 -7 3 114.994 6.28261 2 -2 -7 4 41.0690 5.59522 2 -2 -7 5 20.0312 4.83856 2 -2 -7 6 25.2390 6.77629 2 -2 -7 7 1165.64 11.8217 2 -2 -7 8 231.578 7.59913 2 -2 -7 9 357.920 9.88973 2 -2 -7 10 469.783 9.74308 2 2 -7 -11-4.23384 6.30111 2 -2 -7 12 3217.44 15.7639 2 2 -7 -13 192.388 7.28008 2 -2 7 -14 40.8252 6.04587 2 -2 7 -15 17.3467 5.11069 2 2 7 16 54.4749 6.22810 2 -2 7 17 750.130 6.37018 2 2 7 18 66.6181 4.21080 2 2 7 19 152.680 4.40267 2 2 7 20 145.316 4.54383 2 -2 7 21 18.2653 4.02192 2 2 7 22 151.888 5.18620 2 2 7 23 176.350 5.61719 2 -2 7 -24 31.7203 4.93896 2 2 7 25 13.7108 5.19604 2 -2 7 26 5.46754 5.45876 2 2 7 27 45.1104 5.75553 2 2 7 28 85.8596 5.67164 2 2 7 29 84.6636 5.40480 2 -2 7 -30 117.756 5.07951 2 2 7 -31 42.2676 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210.800 5.94684 2 -3 -4 6 2584.16 9.43365 2 -3 -4 7 71.2959 6.81873 2 -3 -4 8 551.354 8.25656 2 -3 -4 9 178.183 6.17448 2 -3 4 -10 659.450 8.02968 2 -3 4 11 26.6192 5.66960 2 -3 4 12 642.874 7.41020 2 -3 4 13 67.7875 5.62903 2 -3 4 -14 501.712 7.95511 2 3 -4 -15 103.153 7.99219 2 -3 4 -16 294.116 9.40453 2 3 -4 -17 0.44873 7.43724 2 -3 4 18 91.6129 4.59323 2 -3 4 19 579.834 5.53785 2 -3 4 20 66.5163 3.52863 2 -3 4 21 2.63407 3.36813 2 -3 4 -22 292.122 4.49865 2 3 -4 23 144.593 4.07570 2 3 -4 24 5.06970 3.87137 2 -3 4 -25 38.2900 4.05862 2 -3 4 -26 11.2819 4.17237 2 -3 4 -27 144.430 4.53745 2 -3 4 -28 361.460 5.03546 2 -3 4 -29 34.0218 4.50318 2 -3 4 -30 31.1949 4.31151 2 -3 4 -31 4.62911 4.22017 2 3 4 -32 24.8014 4.41346 2 3 4 -33 63.5156 4.53586 2 3 4 34 2.44766 4.59162 2 3 4 -35 5.70975 4.52068 2 3 4 36-3.21925 4.96299 2 3 4 37 30.8773 4.44002 2 3 4 38 22.1400 4.73429 2 3 4 39-1.80948 3.42697 2 3 5 -1 447.233 12.7886 2 -3 -5 2 555.247 7.99549 2 -3 -5 3 478.804 6.77357 2 -3 -5 4 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19.9162 5.15509 2 -18 7 14 9.48777 10.8879 2 18 7 -18 10.1038 8.38258 2 18 7 -19 1.58299 7.55125 2 18 7 -20 10.0529 6.76034 2 18 8 0-2.81283 11.6620 2 18 8 1 23.8615 11.7365 2 18 8 2 18.0442 11.8051 2 -18 8 -3 4.21063 7.27349 2 18 8 4 8.61136 7.21774 2 -18 8 -5 2.11891 5.65856 2 -18 8 -6-2.03877 6.18259 2 -18 8 -7 21.0873 5.41734 2 -18 8 -8 16.8167 5.84501 2 -18 8 -9 16.1744 4.98252 2 -18 8 -10 1.20747 4.65050 2 -18 8 -11 14.2968 4.88540 2 -18 8 12-3.03907 4.48324 2 -18 8 13 10.9630 5.64398 2 18 8 19-2.48286 7.11321 2 18 8 20-5.74217 6.04950 2 18 9 1 3.18601 10.7839 2 18 9 2 14.1479 10.5876 2 18 9 3-0.28595 7.70475 2 -18 9 -4 2.78429 6.75132 2 -18 9 -5 17.6035 6.77976 2 -18 9 -6-0.90155 5.44866 2 -18 9 -7 11.0788 6.18271 2 -18 9 -8 21.5338 4.85940 2 -18 9 -9 13.9891 4.61832 2 -18 9 -10-0.22623 4.31097 2 18 9 -11 1.67247 4.25573 2 -18 9 12 55.4741 4.98361 2 -18 9 13-10.2855 9.74114 2 18 9 17 1.70184 6.99753 2 18 9 18 16.5117 6.26421 2 18 10 3 52.7268 10.2174 2 18 10 4-4.64253 9.31343 2 -18 10 -5 3.24447 7.60562 2 -18 10 -6-4.66251 6.97172 2 -18 10 -7 2.01206 5.31408 2 -18 10 -8 5.38448 5.23693 2 -18 10 -9 3.40787 4.07213 2 18 10 10 3.69772 3.96524 2 18 10 11 2.70236 3.56565 2 -18 10 12 0.51222 4.57266 2 18 10 15-1.97912 6.21817 2 18 11 3 1.60430 8.19629 2 18 11 4 5.90089 7.95238 2 18 11 5 8.16065 8.01573 2 18 11 6 3.09590 6.92805 2 -18 11 -7-2.86881 4.84272 2 -18 11 -8 0.98396 4.05390 2 18 11 9 0.95131 3.96112 2 18 11 10 7.23514 3.26961 2 -18 11 11 1.72495 4.10053 2 18 12 3 9.15989 6.61129 2 18 12 4 2.35479 6.30829 2 18 12 5-1.40623 6.73714 2 18 12 6 1.64124 6.28558 2 18 12 7 8.72115 4.33380 2 18 12 8 3.35061 3.38384 2 18 12 9 0.29414 3.72437 2 18 13 4 7.92628 5.32534 2 18 13 5 8.56934 4.95991 2 18 13 6 1.63494 4.35263 2 -19 0 -10 89.6642 13.3684 2 -19 0 -12 11.6840 8.60169 2 19 0 20 6.22327 7.12906 2 19 0 -22-12.1293 6.29239 2 -19 -1 -5-16.3421 14.2291 2 -19 -1 -6 0.45396 14.2329 2 -19 1 -7 9.47274 9.76279 2 -19 -1 -8 56.2372 13.8789 2 -19 1 -9-6.06595 9.18011 2 -19 1 -10 3.66425 8.73328 2 -19 1 -11 3.86593 8.39132 2 -19 1 -12 3.17121 6.81849 2 19 1 13-5.82825 5.19423 2 19 -1 19 0.88093 7.08245 2 19 -1 -20 32.4444 8.14204 2 19 1 21-0.55246 4.01742 2 19 -1 -22 0.08813 4.30279 2 19 1 -23 2.22720 5.24329 2 -19 2 -5 35.0058 10.2981 2 -19 2 -6 42.2560 10.1973 2 -19 -2 -7 18.6197 14.2673 2 -19 -2 -8-4.82284 13.6194 2 -19 2 -9 5.01531 9.18452 2 -19 2 -10 17.9391 8.75795 2 -19 2 -11 13.8488 8.40749 2 -19 2 -12 7.74974 5.47948 2 19 2 13 17.7241 6.42610 2 19 -2 -19-8.41553 7.92591 2 19 -2 -20 0.87086 7.18933 2 19 2 21 0.52317 3.90704 2 19 2 22 10.2230 4.28462 2 19 2 -23 8.56393 5.20707 2 -19 3 -5-7.26293 13.1286 2 -19 3 -6 2.72060 8.26808 2 -19 3 -7 21.2848 8.25572 2 -19 3 -8 8.17891 7.84656 2 -19 3 -9 13.0532 7.59510 2 19 3 10 1.38467 5.99063 2 -19 3 -11 4.70030 5.76710 2 -19 3 -12-2.01922 4.87994 2 19 3 13-12.1447 5.90314 2 19 -3 -20-0.20404 6.02444 2 19 3 21 7.92506 6.84358 2 19 3 22 11.4254 4.19784 2 -19 4 1 2.30747 10.5896 2 -19 4 -3 15.8642 16.5705 2 -19 4 -4 61.5091 10.8238 2 -19 4 -5 18.9577 10.0885 2 -19 4 -6 75.0600 8.42527 2 -19 4 -7 8.32559 6.69858 2 -19 4 -8 23.5035 5.71208 2 -19 4 -9 23.4205 5.46000 2 -19 4 -10 7.01603 4.64566 2 -19 4 11 92.7980 4.44968 2 -19 4 12-0.13623 4.21304 2 -19 4 13 0.89135 4.64610 2 -19 4 14-8.27483 6.76700 2 19 -4 -15 15.3947 8.52134 2 19 -4 -16 19.9603 7.99830 2 19 -4 -17 12.4293 7.32062 2 19 -4 -18 0.93046 6.42033 2 19 4 21-1.57523 6.47836 2 19 4 22 6.29387 5.33712 2 -19 5 1 31.9478 10.2713 2 -19 5 -3 34.4045 16.2673 2 -19 5 -4 4.45404 10.3022 2 -19 5 -5 53.8076 6.97713 2 -19 5 -6-5.18177 7.88240 2 -19 5 -7 18.9140 6.44798 2 -19 5 -8 55.4697 5.64792 2 -19 5 -9 2.26736 4.49973 2 -19 5 -10-1.11200 4.33247 2 -19 5 -11 18.7578 3.79138 2 -19 5 12 13.1556 4.01090 2 -19 5 13 7.36786 4.25383 2 -19 5 14-14.4961 10.0647 2 19 5 20 13.9069 6.97756 2 19 5 21 7.87353 4.05500 2 -19 6 1 25.7421 9.59850 2 -19 6 -3 16.3774 12.6148 2 -19 6 -4 6.61152 12.3851 2 -19 6 -5-3.91451 6.36464 2 -19 6 -6 4.89895 6.21075 2 -19 6 -7 0.53126 6.09471 2 -19 6 -8-5.68792 5.84373 2 -19 6 -9 46.6404 5.15502 2 -19 6 -10 8.47736 4.68056 2 -19 6 -11 33.6704 4.53094 2 -19 6 12 12.5628 4.50587 2 -19 6 13 5.29918 5.70943 2 19 6 20 3.88760 5.91964 2 -19 7 1 37.9099 9.39493 2 19 7 3 9.40852 8.07685 2 19 7 4 12.7180 7.01143 2 -19 7 -5 31.9424 6.30721 2 -19 7 -6-0.28849 5.86265 2 -19 7 -7 2.21906 5.69276 2 -19 7 -8 26.7831 5.70709 2 -19 7 -9 4.88246 4.60579 2 -19 7 -10 11.7847 4.41364 2 19 7 11 2.67195 5.95143 2 -19 7 12 7.61989 5.73758 2 -19 7 13-3.70064 9.65733 2 -19 8 1 13.0924 6.69026 2 19 8 2 2.95137 10.2618 2 19 8 3 6.47616 7.52668 2 19 8 4-2.40563 6.34507 2 -19 8 -5 27.0769 5.21651 2 -19 8 -6 7.65953 4.83745 2 -19 8 -7 1.86807 5.22243 2 -19 8 -8 0.71470 4.92116 2 -19 8 -9 0.04634 4.75542 2 -19 8 -10 2.47536 4.31403 2 19 8 -11 13.8759 4.41232 2 -19 8 12 0.90587 4.82860 2 19 8 17-5.21021 6.04037 2 -19 9 1 63.8824 7.90040 2 19 9 2 6.07056 9.58464 2 19 9 3-1.24959 8.61456 2 19 9 4 16.0757 9.19595 2 19 9 5 2.56711 6.25783 2 -19 9 -6 0.95983 5.62448 2 -19 9 -7-4.95424 5.08042 2 -19 9 -8-2.89638 4.34056 2 -19 9 -9 19.2393 3.84479 2 19 9 10 6.77804 3.61538 2 -19 9 11-2.70348 3.45478 2 -19 9 12-4.10569 8.02956 2 -19 10 1 11.0988 6.60693 2 19 10 2 3.86205 7.84590 2 19 10 3-0.90162 7.74733 2 19 10 4 4.17852 7.31976 2 19 10 5-1.51139 7.44411 2 -19 10 -6 5.77250 4.89709 2 -19 10 -7 1.91245 4.37478 2 -19 10 -8 4.98268 3.74801 2 19 10 9 2.30070 3.28062 2 19 10 10 16.7085 3.79718 2 -19 11 1 20.7449 6.70291 2 19 11 4-1.37938 6.22869 2 19 11 5 0.53926 6.23422 2 19 11 6 10.0869 4.29503 2 19 11 7 9.77718 3.99647 2 19 11 8-1.22455 3.39816 2 19 12 1 3.51426 6.04755 2 19 12 4 5.01469 4.79336 2 19 12 5 4.97966 3.27106 2 -20 0 -8 21.1243 12.3549 2 -20 0 -10 15.7620 11.1384 2 -20 0 -12 19.7427 8.52438 2 20 0 -20 8.77282 5.56800 2 -20 1 -4-17.6080 13.1849 2 -20 -1 -7 15.6380 13.0257 2 -20 -1 -8-4.28169 12.2300 2 -20 1 -9 15.8164 8.26078 2 -20 -1 -10-9.27183 11.1935 2 -20 -1 -11 13.0824 10.3545 2 20 1 12 5.13129 5.98801 2 20 1 19 0.91429 5.67546 2 -20 2 -5 2.03816 9.12521 2 -20 2 -6 2.73533 8.95419 2 -20 -2 -7 13.8339 13.0729 2 -20 2 -8-0.42968 8.60971 2 -20 -2 -9 8.27447 11.5397 2 20 2 10-2.25978 5.94193 2 20 2 11 9.99541 6.67450 2 20 2 12 24.4562 8.63868 2 20 2 19-0.54144 5.99762 2 -20 3 0 171.870 13.9343 2 -20 3 1 25.1836 9.84102 2 -20 3 2 7.49641 9.66797 2 -20 3 -3 10.9601 15.6820 2 -20 3 -4 10.8413 7.95814 2 -20 3 -5-0.46930 9.50513 2 -20 3 -6 3.56478 7.64022 2 -20 3 -7 18.0551 9.26289 2 -20 3 -8 3.76370 5.72385 2 -20 3 -9 30.0204 5.77485 2 -20 3 -10 17.9287 5.30895 2 -20 3 -11 14.7540 5.91134 2 20 3 12 8.47779 7.73753 2 20 3 19-2.51391 5.97725 2 -20 4 -4-0.78893 9.33894 2 -20 4 -5-0.34206 7.53185 2 -20 4 -6 6.44660 6.01414 2 -20 4 -7 2.09381 5.84405 2 -20 4 -8 19.7618 5.80988 2 -20 4 -9 5.15009 4.68669 2 -20 4 -10 8.66210 4.16873 2 -20 4 11 3.93638 4.72667 2 -20 4 12 10.7853 4.11692 2 -20 4 13 6.16860 5.78466 2 20 -4 -14 9.06790 6.90992 2 20 -4 -15 14.0836 6.25978 2 20 4 19 4.17619 5.53113 2 -20 5 -3 25.2686 12.3206 2 -20 5 -4-3.67786 8.99466 2 -20 5 -5-4.41928 8.88578 2 -20 5 -6 0.58505 5.74723 2 -20 5 -7 3.54724 5.52435 2 -20 5 -8-6.04370 6.49397 2 -20 5 -9 14.6593 4.40000 2 -20 5 -10-3.16127 3.65850 2 -20 5 11 44.3220 4.47211 2 -20 5 12 3.50852 4.40987 2 -20 5 13 5.75480 8.77786 2 -20 6 -3 4.11902 8.67266 2 -20 6 -4 3.83276 8.70521 2 -20 6 -5 0.33704 5.60555 2 -20 6 -6 23.4355 5.57481 2 -20 6 -7 6.82208 5.28553 2 -20 6 -8-3.14977 4.96895 2 -20 6 -9 3.50567 4.17621 2 20 6 10 5.34810 4.20250 2 -20 6 11 5.46587 4.40994 2 -20 6 12-2.14314 4.56777 2 20 7 3 28.2720 7.46643 2 20 7 4 7.73849 5.84366 2 -20 7 -5 0.03568 5.22948 2 -20 7 -6 8.65058 5.00838 2 -20 7 -7 2.26313 4.91913 2 -20 7 -8 3.32970 4.61253 2 -20 7 -9-2.83534 4.44691 2 -20 -7 -10 38.0006 4.57282 2 -20 7 11-0.70031 4.59567 2 -20 7 12 3.96334 7.91100 2 20 8 0 11.6776 9.19570 2 20 8 1 8.13348 8.55844 2 20 8 2 0.99522 8.68552 2 20 8 3-0.30558 5.24573 2 20 8 -4 7.97735 4.59754 2 -20 8 -5-3.73505 5.52830 2 -20 8 -6 6.14231 5.33491 2 -20 8 -7-3.74735 4.92148 2 -20 8 -8-0.03590 3.97422 2 -20 -8 -9 0.10425 3.58195 2 20 8 -10 9.98994 3.36242 2 20 9 1-0.99934 7.28789 2 20 9 2 5.54707 7.31681 2 20 9 3 10.9998 7.58063 2 20 9 4 42.5057 7.60707 2 -20 9 -5 6.89626 4.44824 2 -20 9 -6 3.29289 4.18995 2 -20 9 -7 9.29072 3.57956 2 -20 9 -8 2.05200 2.73541 2 20 9 -9 10.8096 4.10242 2 20 10 1-4.78079 6.36747 2 20 10 2 3.20028 6.26403 2 20 10 3 6.25099 5.68607 2 20 10 4-4.89184 5.52828 2 20 10 5 6.38957 5.32328 2 -20 10 -6 4.98305 2.94205 2 20 11 2-2.14106 4.43276 2 -21 0 -8 9.28577 10.6540 2 21 0 10 7.64374 7.96540 2 -21 -1 -7 4.21446 10.8632 2 21 1 9-5.71356 6.39547 2 21 1 10 6.32504 5.86647 2 21 1 11 5.92815 6.77919 2 21 2 7-4.79784 8.91034 2 -21 -2 -8 12.9217 10.3999 2 21 2 10 6.90131 7.47545 2 21 2 11-3.93440 6.53844 2 -21 3 1 72.1004 8.80461 2 -21 3 2 15.1452 8.47705 2 -21 3 -3 9.00209 7.05311 2 -21 3 -4 15.7819 6.12184 2 -21 3 -5 69.1428 8.88926 2 -21 3 -6 14.4571 8.16678 2 -21 3 -7 5.58446 7.78079 2 -21 3 -8 7.87966 4.74855 2 -21 3 -9 1.67359 3.79398 2 -21 3 10 39.3983 3.88312 2 -21 3 11 4.40494 3.60545 2 -21 3 12-7.98028 5.16546 2 21 -3 -13-3.20197 6.08009 2 -21 4 1 6.76260 8.56806 2 -21 4 -3 41.2346 11.6241 2 -21 4 -4 31.7072 8.28095 2 -21 4 -5 14.3160 8.16425 2 -21 4 -6-1.22577 6.32061 2 -21 4 -7 4.84289 6.06725 2 -21 4 -8 7.08647 4.05331 2 -21 4 -9 1.85451 3.78153 2 -21 4 10 3.20010 3.88788 2 -21 4 11 8.52366 3.21435 2 -21 5 1 7.24038 8.08162 2 -21 5 -3 32.2976 10.7337 2 -21 5 -4-14.2651 9.96637 2 -21 5 -5 10.9482 7.64322 2 -21 5 -6-4.42031 7.25483 2 -21 5 -7 25.6690 7.10072 2 -21 5 -8 8.66109 4.50559 2 -21 5 -9 3.26955 4.08696 2 -21 5 10 6.33337 4.30183 2 -21 5 11 4.85151 7.85816 2 -21 6 1 10.9124 7.56776 2 -21 6 -3-2.08143 9.81267 2 21 6 4 7.71312 5.12972 2 -21 6 -5-1.02338 5.68526 2 -21 6 -6 2.23161 4.28641 2 -21 6 -7-0.88052 5.19049 2 -21 6 -8-3.61919 4.09614 2 -21 -6 -9 11.5470 7.60274 2 -21 6 10-2.10299 8.02627 2 -21 7 1-4.08130 6.81515 2 21 7 3 2.26870 4.59392 2 21 7 4-1.46693 5.33945 2 21 7 5 11.0380 5.20081 2 -21 7 -6 9.37866 4.52544 2 -21 7 -7 15.7558 6.02764 2 -21 7 -8 3.64092 3.56225 2 -21 8 1 10.9953 9.73289 2 21 8 -3 1.04906 4.43674 2 21 8 -4 3.24113 3.89799 2 21 8 5-1.88051 4.48438 2 -21 8 -6 2.57903 3.64456 2 21 8 -7 1.22355 4.06604 2 -21 9 1-3.93963 4.29658 2 21 9 2 8.82646 5.20529 2 21 9 3-3.14256 4.63564 2 21 9 -4 4.51695 3.00237 2 22 0 8 8.32147 6.89174 2 22 -1 9 1.77647 5.88187 2 22 -2 9-0.46851 5.53161 2 -22 3 -3 10.3513 9.59544 2 -22 3 -4 7.08204 7.14179 2 -22 3 -5 6.62122 6.85060 2 -22 3 -6 12.4617 6.51432 2 -22 3 -7 0.72055 4.69096 2 -22 3 -8 0.28874 3.46037 2 -22 3 9-3.97499 4.77934 2 -22 4 -3-2.40416 8.80732 2 -22 4 -4 3.37164 6.54006 2 -22 4 -5 0.61877 6.43606 2 -22 4 -6 4.41257 6.07928 2 -22 4 -7 2.87086 4.32852 2 -22 4 8-0.64512 3.71311 2 -22 5 -3-1.96553 7.97536 2 -22 5 -4-9.56692 7.73117 2 -22 5 -5-1.94036 5.88342 2 -22 5 -6 0.16849 5.40867 2 -22 5 -7 3.34264 4.51999 2 -22 6 -3 8.18540 7.22542 2 -22 6 -5-10.4495 8.19658 2 23 0 2 2.93760 6.37100 2 23 0 4-0.72127 5.91841 2 23 -1 3 14.7355 6.60240 2 23 -1 4-1.64039 5.76359 2 23 -1 5-1.10562 5.39833 2 -23 3 1-1.02279 4.99281 2 -23 3 -3 5.16746 4.81977 2 -23 4 1 5.27848 4.48317 2 0 0 0 0.00000 0.00000 0 TITL lk44db_twin1_hklf4 in Pbca REM Pbca (#61, found as Pcab in ba-c setting) CELL 1.54184 18.621064 16.994112 32.002659 90.0000 90.0000 90.0000 ZERR 15.00 0.000311 0.000198 0.000386 0.0000 0.0000 0.0000 LATT 1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O F UNIT 435.00 420.00 30.00 15.00 90.00 REM CrysAlisPro recorded range (K): Min=99.9; max=100.1; aver:100.0 TEMP -173 TREF HKLF 5 BASF 0.50318 END ; _shelx_hkl_checksum 89087 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, 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 F1 F 0.31817(14) 0.19286(17) 0.25630(7) 0.0805(8) Uani 1 1 d . . . . . F2 F 0.34865(18) 0.07909(13) 0.27605(7) 0.0928(9) Uani 1 1 d . . . . . F3 F 0.42734(12) 0.16021(15) 0.25530(6) 0.0676(6) Uani 1 1 d . . . . . F4 F 0.35778(13) 0.63325(14) 0.34055(9) 0.0858(9) Uani 1 1 d . . . . . F5 F 0.46098(16) 0.59374(14) 0.32409(7) 0.0813(8) Uani 1 1 d . . . . . F6 F 0.44901(14) 0.67352(11) 0.37384(6) 0.0679(7) Uani 1 1 d . . . . . O1 O 0.40492(12) 0.39151(12) 0.53110(6) 0.0416(5) Uani 1 1 d . . . . . N1 N 0.38799(14) 0.22094(14) 0.56201(7) 0.0361(6) Uani 1 1 d . . . . . N2 N 0.38369(14) 0.12772(13) 0.47814(7) 0.0362(6) Uani 1 1 d . . . . . C1 C 0.39908(16) 0.33367(16) 0.50832(9) 0.0335(6) Uani 1 1 d . . . . . C2 C 0.38911(16) 0.25018(16) 0.52066(9) 0.0344(6) Uani 1 1 d . . . . . C3 C 0.39041(16) 0.20743(16) 0.48477(9) 0.0334(6) Uani 1 1 d . . . . . C4 C 0.39583(16) 0.26196(17) 0.44753(9) 0.0342(6) Uani 1 1 d . . . . . C5 C 0.40144(16) 0.33662(16) 0.46128(9) 0.0336(6) Uani 1 1 d . . . . . C6 C 0.36574(18) 0.27551(17) 0.59492(9) 0.0389(7) Uani 1 1 d . . . . . H6A H 0.323012 0.305391 0.585590 0.047 Uiso 1 1 calc R U . . . H6B H 0.404860 0.313526 0.600520 0.047 Uiso 1 1 calc R U . . . C7 C 0.34808(19) 0.23077(19) 0.63457(9) 0.0435(7) Uani 1 1 d . . . . . H7A H 0.335179 0.268527 0.656893 0.052 Uiso 1 1 calc R U . . . H7B H 0.306087 0.196327 0.629528 0.052 Uiso 1 1 calc R U . . . C8 C 0.4107(2) 0.1815(2) 0.64871(10) 0.0510(9) Uani 1 1 d . . . . . H8A H 0.395924 0.148420 0.672692 0.061 Uiso 1 1 calc R U . . . H8B H 0.450168 0.216266 0.658083 0.061 Uiso 1 1 calc R U . . . C9 C 0.4373(2) 0.12885(19) 0.61326(10) 0.0474(8) Uani 1 1 d . . . . . H9A H 0.481651 0.101376 0.622130 0.057 Uiso 1 1 calc R U . . . H9B H 0.400521 0.088560 0.606863 0.057 Uiso 1 1 calc R U . . . C10 C 0.45257(17) 0.17717(18) 0.57438(10) 0.0403(7) Uani 1 1 d . . . . . H10C H 0.492266 0.214436 0.580014 0.048 Uiso 1 1 calc R U . . . H10D H 0.467573 0.141947 0.551335 0.048 Uiso 1 1 calc R U . . . C11 C 0.34529(19) 0.07783(17) 0.50821(9) 0.0415(7) Uani 1 1 d . . . . . H11C H 0.308354 0.109118 0.523007 0.050 Uiso 1 1 calc R U . . . H11D H 0.379309 0.056721 0.529169 0.050 Uiso 1 1 calc R U . . . C12 C 0.3099(2) 0.01046(19) 0.48451(11) 0.0504(8) Uani 1 1 d . . . . . H12C H 0.273813 0.031785 0.464836 0.060 Uiso 1 1 calc R U . . . H12D H 0.284911 -0.024628 0.504460 0.060 Uiso 1 1 calc R U . . . C13 C 0.3662(2) -0.03645(19) 0.46034(11) 0.0563(10) Uani 1 1 d . . . . . H13C H 0.399455 -0.062115 0.480270 0.068 Uiso 1 1 calc R U . . . H13D H 0.342175 -0.078173 0.443897 0.068 Uiso 1 1 calc R U . . . C14 C 0.4088(2) 0.01685(18) 0.43101(11) 0.0544(9) Uani 1 1 d . . . . . H14C H 0.448354 -0.013532 0.418091 0.065 Uiso 1 1 calc R U . . . H14D H 0.377008 0.035927 0.408371 0.065 Uiso 1 1 calc R U . . . C15 C 0.43955(18) 0.08654(18) 0.45456(10) 0.0423(7) Uani 1 1 d . . . . . H15C H 0.477262 0.067998 0.474017 0.051 Uiso 1 1 calc R U . . . H15D H 0.462040 0.123422 0.434507 0.051 Uiso 1 1 calc R U . . . C16 C 0.38843(16) 0.23564(16) 0.40378(9) 0.0339(6) Uani 1 1 d . . . . . C17 C 0.33025(17) 0.18986(18) 0.39147(10) 0.0405(7) Uani 1 1 d . . . . . H17 H 0.294670 0.175821 0.411395 0.049 Uiso 1 1 calc R U . . . C18 C 0.32350(18) 0.16445(19) 0.35046(10) 0.0428(7) Uani 1 1 d . . . . . H18 H 0.283050 0.134002 0.342351 0.051 Uiso 1 1 calc R U . . . C19 C 0.37526(17) 0.18327(18) 0.32160(9) 0.0376(7) Uani 1 1 d . . . . . C20 C 0.43339(17) 0.22930(17) 0.33332(9) 0.0381(7) Uani 1 1 d . . . . . H20 H 0.468972 0.242942 0.313312 0.046 Uiso 1 1 calc R U . . . C21 C 0.43959(16) 0.25532(17) 0.37406(9) 0.0350(6) Uani 1 1 d . . . . . H21 H 0.479390 0.287086 0.381823 0.042 Uiso 1 1 calc R U . . . C22 C 0.36760(19) 0.15472(19) 0.27745(10) 0.0452(8) Uani 1 1 d . . . . . C23 C 0.40371(16) 0.40982(16) 0.43655(9) 0.0335(6) Uani 1 1 d . . . . . C24 C 0.35169(17) 0.42490(17) 0.40653(10) 0.0397(7) Uani 1 1 d . . . . . H24 H 0.312966 0.389097 0.403064 0.048 Uiso 1 1 calc R U . . . C25 C 0.35537(17) 0.49127(18) 0.38160(10) 0.0409(7) Uani 1 1 d . . . . . H25 H 0.319003 0.501325 0.361472 0.049 Uiso 1 1 calc R U . . . C26 C 0.41236(17) 0.54301(16) 0.38612(9) 0.0356(6) Uani 1 1 d . . . . . C27 C 0.46352(17) 0.52990(16) 0.41670(9) 0.0365(7) Uani 1 1 d . . . . . H27 H 0.502090 0.565904 0.420163 0.044 Uiso 1 1 calc R U . . . C28 C 0.45860(16) 0.46441(16) 0.44227(9) 0.0348(6) Uani 1 1 d . . . . . H28 H 0.492900 0.456666 0.463852 0.042 Uiso 1 1 calc R U . . . C29 C 0.41994(18) 0.61047(18) 0.35663(10) 0.0411(7) Uani 1 1 d . . . . . O1A O 0.61022(12) 0.10869(12) 0.41178(6) 0.0413(5) Uani 1 1 d . . . . . N1A N 0.65578(14) 0.26498(14) 0.44961(7) 0.0361(5) Uani 1 1 d . . . . . N2A N 0.66837(14) 0.37240(13) 0.37130(7) 0.0350(5) Uani 1 1 d . . . . . C1A C 0.62776(16) 0.16643(16) 0.39114(9) 0.0342(6) Uani 1 1 d . . . . . C2A C 0.65149(16) 0.24384(17) 0.40668(9) 0.0347(6) Uani 1 1 d . . . . . C3A C 0.65399(16) 0.29337(16) 0.37314(9) 0.0336(6) Uani 1 1 d . . . . . C4A C 0.64074(15) 0.24655(16) 0.33333(9) 0.0329(6) Uani 1 1 d . . . . . C5A C 0.62544(16) 0.17166(16) 0.34414(9) 0.0329(6) Uani 1 1 d . . . . . C6A C 0.69261(18) 0.2083(2) 0.47653(9) 0.0427(7) Uani 1 1 d . . . . . H6AA H 0.738385 0.192045 0.463372 0.051 Uiso 1 1 calc R U . . . H6AB H 0.662345 0.160860 0.480073 0.051 Uiso 1 1 calc R U . . . C7A C 0.70752(18) 0.2449(2) 0.51877(9) 0.0451(8) Uani 1 1 d . . . . . H7AA H 0.731429 0.205749 0.536989 0.054 Uiso 1 1 calc R U . . . H7AB H 0.740428 0.290149 0.515302 0.054 Uiso 1 1 calc R U . . . C8A C 0.63927(19) 0.2721(2) 0.53910(10) 0.0484(8) Uani 1 1 d . . . . . H8AA H 0.650647 0.300121 0.565405 0.058 Uiso 1 1 calc R U . . . H8AB H 0.608963 0.226076 0.546025 0.058 Uiso 1 1 calc R U . . . C9A C 0.5985(2) 0.3268(2) 0.50991(10) 0.0532(9) Uani 1 1 d . . . . . H9AA H 0.551326 0.339933 0.522338 0.064 Uiso 1 1 calc R U . . . H9AB H 0.625815 0.376290 0.506308 0.064 Uiso 1 1 calc R U . . . C10A C 0.58736(18) 0.2882(2) 0.46768(10) 0.0450(8) Uani 1 1 d . . . . . H10A H 0.556390 0.241205 0.470945 0.054 Uiso 1 1 calc R U . . . H10B H 0.562765 0.325386 0.448671 0.054 Uiso 1 1 calc R U . . . C11A C 0.70422(19) 0.41104(17) 0.40651(9) 0.0418(7) Uani 1 1 d . . . . . H11A H 0.738352 0.374099 0.419850 0.050 Uiso 1 1 calc R U . . . H11B H 0.668243 0.427022 0.427644 0.050 Uiso 1 1 calc R U . . . C12A C 0.7443(2) 0.48314(18) 0.39056(10) 0.0471(8) Uani 1 1 d . . . . . H12A H 0.767708 0.510262 0.414318 0.056 Uiso 1 1 calc R U . . . H12B H 0.782287 0.466406 0.370817 0.056 Uiso 1 1 calc R U . . . C13A C 0.6937(2) 0.53948(18) 0.36880(10) 0.0484(8) Uani 1 1 d . . . . . H13A H 0.721127 0.584702 0.357632 0.058 Uiso 1 1 calc R U . . . H13B H 0.658137 0.559835 0.389120 0.058 Uiso 1 1 calc R U . . . C14A C 0.6548(2) 0.49805(17) 0.33325(10) 0.0460(8) Uani 1 1 d . . . . . H14A H 0.689667 0.484133 0.311103 0.055 Uiso 1 1 calc R U . . . H14B H 0.618635 0.534005 0.321009 0.055 Uiso 1 1 calc R U . . . C15A C 0.61772(17) 0.42364(17) 0.34890(10) 0.0396(7) Uani 1 1 d . . . . . H15A H 0.577812 0.438264 0.367807 0.047 Uiso 1 1 calc R U . . . H15B H 0.597165 0.394667 0.324876 0.047 Uiso 1 1 calc R U . . . C16A C 0.64869(16) 0.27723(16) 0.29039(9) 0.0330(6) Uani 1 1 d . . . . . C17A C 0.70682(17) 0.32474(17) 0.27938(10) 0.0376(7) Uani 1 1 d . . . . . H17A H 0.742017 0.337550 0.299763 0.045 Uiso 1 1 calc R U . . . C18A C 0.71375(17) 0.35334(18) 0.23920(10) 0.0409(7) Uani 1 1 d . . . . . H18A H 0.753838 0.385171 0.232025 0.049 Uiso 1 1 calc R U . . . C19A C 0.66246(17) 0.33575(17) 0.20936(9) 0.0378(7) Uani 1 1 d . . . . . C20A C 0.60483(17) 0.28783(18) 0.21954(9) 0.0387(7) Uani 1 1 d . . . . . H20A H 0.569816 0.275067 0.199034 0.046 Uiso 1 1 calc R U . . . C21A C 0.59862(16) 0.25879(17) 0.25961(9) 0.0352(6) Uani 1 1 d . . . . . H21A H 0.559332 0.225469 0.266354 0.042 Uiso 1 1 calc R U . . . C22A C 0.6691(2) 0.3672(2) 0.16619(11) 0.0480(8) Uani 1 1 d . . . . . C23A C 0.61417(16) 0.10331(16) 0.31666(9) 0.0335(6) Uani 1 1 d . . . . . C24A C 0.66184(16) 0.08706(16) 0.28415(9) 0.0364(6) Uani 1 1 d . . . . . H24A H 0.703514 0.118624 0.280678 0.044 Uiso 1 1 calc R U . . . C25A C 0.64899(17) 0.02535(17) 0.25691(9) 0.0376(7) Uani 1 1 d . . . . . H25A H 0.681664 0.014676 0.234827 0.045 Uiso 1 1 calc R U . . . C26A C 0.58817(17) -0.02080(17) 0.26200(9) 0.0365(7) Uani 1 1 d . . . . . C27A C 0.54098(17) -0.00621(17) 0.29463(9) 0.0385(7) Uani 1 1 d . . . . . H27A H 0.499501 -0.038099 0.298091 0.046 Uiso 1 1 calc R U . . . C28A C 0.55442(16) 0.05493(17) 0.32217(9) 0.0369(7) Uani 1 1 d . . . . . H28A H 0.522749 0.063955 0.344941 0.044 Uiso 1 1 calc R U . . . C29A C 0.5716(2) -0.08580(18) 0.23216(10) 0.0436(8) Uani 1 1 d . . . . . F1A F 0.7074(3) 0.31973(18) 0.14100(9) 0.0813(14) Uani 0.808(7) 1 d . . P A 1 F2A F 0.7018(2) 0.43591(19) 0.16385(9) 0.0746(12) Uani 0.808(7) 1 d . . P A 1 F3A F 0.60752(18) 0.3730(3) 0.14608(11) 0.0886(13) Uani 0.808(7) 1 d . U P A 1 F1B F 0.6495(10) 0.3249(8) 0.1378(4) 0.070(4) Uani 0.192(7) 1 d . U P A 2 F2B F 0.7272(9) 0.4000(12) 0.1591(5) 0.083(5) Uani 0.192(7) 1 d . U P A 2 F3B F 0.6189(6) 0.4282(7) 0.1614(4) 0.055(4) Uani 0.192(7) 1 d . U P A 2 F4A F 0.62060(17) -0.09355(17) 0.20168(8) 0.0737(10) Uani 0.897(5) 1 d . . P B 3 F5A F 0.51057(17) -0.07731(19) 0.21287(11) 0.0945(14) Uani 0.897(5) 1 d . . P B 3 F6A F 0.5707(2) -0.15574(13) 0.25021(7) 0.0866(14) Uani 0.897(5) 1 d . . P B 3 F4B F 0.5644(14) -0.0679(12) 0.1975(6) 0.051(6) Uani 0.103(5) 1 d . U P B 4 F5B F 0.5126(11) -0.1233(12) 0.2446(6) 0.050(6) Uani 0.103(5) 1 d . U P B 4 F6B F 0.6188(14) -0.1367(16) 0.2363(8) 0.067(7) Uani 0.103(5) 1 d . U P B 4 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 F1 0.0869(17) 0.1026(19) 0.0520(13) -0.0219(13) -0.0304(12) 0.0349(15) F2 0.176(3) 0.0507(13) 0.0520(13) -0.0192(11) 0.0127(16) -0.0331(16) F3 0.0680(15) 0.0947(17) 0.0401(10) -0.0198(11) 0.0034(10) -0.0040(12) F4 0.0628(15) 0.0659(14) 0.129(2) 0.0541(15) -0.0261(14) -0.0114(12) F5 0.134(2) 0.0583(13) 0.0513(12) 0.0102(10) 0.0364(14) 0.0140(14) F6 0.115(2) 0.0382(10) 0.0502(11) 0.0027(9) -0.0045(12) -0.0262(11) O1 0.0569(14) 0.0307(10) 0.0372(11) -0.0036(9) -0.0031(10) -0.0016(9) N1 0.0481(15) 0.0322(12) 0.0280(12) -0.0028(10) 0.0016(11) 0.0048(11) N2 0.0472(15) 0.0264(11) 0.0351(12) -0.0006(10) 0.0079(11) 0.0005(10) C1 0.0365(15) 0.0294(13) 0.0347(15) -0.0031(12) -0.0024(12) -0.0006(12) C2 0.0392(16) 0.0305(14) 0.0335(15) -0.0012(12) 0.0003(13) 0.0020(12) C3 0.0387(16) 0.0291(13) 0.0324(14) 0.0013(11) 0.0009(13) 0.0016(12) C4 0.0351(16) 0.0329(14) 0.0346(15) 0.0010(12) 0.0008(12) 0.0008(12) C5 0.0381(16) 0.0304(13) 0.0322(14) -0.0010(11) 0.0003(13) -0.0016(12) C6 0.0490(19) 0.0339(14) 0.0337(15) -0.0034(12) 0.0016(14) 0.0049(13) C7 0.053(2) 0.0419(16) 0.0355(16) -0.0037(13) 0.0048(15) 0.0001(15) C8 0.068(2) 0.0497(18) 0.0349(16) 0.0059(15) 0.0020(16) 0.0088(17) C9 0.058(2) 0.0436(17) 0.0407(17) 0.0077(14) 0.0022(16) 0.0090(16) C10 0.0421(17) 0.0399(15) 0.0390(16) 0.0002(13) -0.0004(14) 0.0059(14) C11 0.057(2) 0.0307(14) 0.0367(16) -0.0008(12) 0.0078(15) -0.0039(14) C12 0.067(2) 0.0364(16) 0.0479(18) 0.0002(15) 0.0024(17) -0.0112(16) C13 0.085(3) 0.0316(15) 0.052(2) -0.0078(15) 0.0050(19) -0.0041(17) C14 0.085(3) 0.0323(15) 0.0462(18) -0.0061(14) 0.0139(18) 0.0070(17) C15 0.0514(19) 0.0333(14) 0.0421(17) 0.0001(13) 0.0078(15) 0.0074(14) C16 0.0391(16) 0.0289(13) 0.0336(15) 0.0014(12) -0.0001(13) 0.0022(12) C17 0.0396(17) 0.0410(16) 0.0408(17) -0.0035(14) 0.0053(14) -0.0017(13) C18 0.0422(18) 0.0435(17) 0.0426(17) -0.0060(14) -0.0040(15) -0.0036(14) C19 0.0432(17) 0.0352(15) 0.0345(15) -0.0029(12) -0.0039(14) 0.0055(13) C20 0.0424(17) 0.0374(15) 0.0345(15) 0.0016(13) 0.0006(13) 0.0028(14) C21 0.0372(16) 0.0343(14) 0.0334(14) 0.0002(12) -0.0016(12) 0.0002(12) C22 0.050(2) 0.0446(17) 0.0408(17) -0.0051(15) -0.0030(16) 0.0021(15) C23 0.0394(16) 0.0306(13) 0.0303(14) -0.0031(11) 0.0007(12) 0.0000(12) C24 0.0422(17) 0.0319(14) 0.0451(17) 0.0009(13) -0.0043(14) -0.0045(13) C25 0.0431(18) 0.0388(15) 0.0407(16) 0.0010(13) -0.0067(14) -0.0003(14) C26 0.0433(17) 0.0290(13) 0.0346(15) -0.0043(12) 0.0009(13) -0.0001(12) C27 0.0443(17) 0.0291(13) 0.0363(15) -0.0055(12) 0.0010(14) -0.0016(12) C28 0.0401(16) 0.0307(13) 0.0336(14) -0.0045(12) -0.0041(13) -0.0003(12) C29 0.0470(19) 0.0372(15) 0.0392(16) -0.0042(13) -0.0022(15) -0.0044(14) O1A 0.0519(13) 0.0333(10) 0.0385(11) 0.0046(9) 0.0027(10) -0.0027(9) N1A 0.0414(14) 0.0366(12) 0.0303(12) 0.0019(10) -0.0020(11) 0.0015(11) N2A 0.0461(15) 0.0248(11) 0.0340(12) -0.0009(10) -0.0058(11) 0.0023(10) C1A 0.0355(15) 0.0301(14) 0.0371(15) -0.0004(12) 0.0011(13) 0.0024(12) C2A 0.0378(16) 0.0327(14) 0.0334(14) -0.0017(12) -0.0004(13) -0.0001(12) C3A 0.0356(15) 0.0290(13) 0.0362(15) -0.0036(12) -0.0037(13) 0.0006(12) C4A 0.0348(15) 0.0313(14) 0.0326(14) -0.0020(12) -0.0009(12) 0.0020(12) C5A 0.0360(15) 0.0293(13) 0.0334(15) -0.0003(11) -0.0008(12) 0.0003(12) C6A 0.0447(18) 0.0488(17) 0.0347(16) 0.0041(14) 0.0003(14) 0.0073(15) C7A 0.0467(19) 0.0530(19) 0.0357(16) 0.0061(15) -0.0039(14) -0.0016(16) C8A 0.054(2) 0.058(2) 0.0333(16) -0.0040(15) -0.0002(15) -0.0016(17) C9A 0.056(2) 0.062(2) 0.0418(18) -0.0133(16) -0.0027(16) 0.0126(18) C10A 0.0427(18) 0.0496(18) 0.0427(17) -0.0052(15) -0.0021(15) 0.0082(15) C11A 0.058(2) 0.0311(14) 0.0364(15) -0.0029(13) -0.0077(15) -0.0044(14) C12A 0.064(2) 0.0321(14) 0.0449(17) -0.0046(14) -0.0083(17) -0.0079(15) C13A 0.068(2) 0.0292(14) 0.0481(18) -0.0027(14) 0.0045(17) 0.0020(15) C14A 0.060(2) 0.0320(15) 0.0460(18) 0.0048(14) -0.0025(16) 0.0067(15) C15A 0.0456(18) 0.0328(14) 0.0403(16) -0.0019(13) -0.0036(14) 0.0058(13) C16A 0.0378(16) 0.0284(13) 0.0328(14) -0.0017(11) -0.0018(13) 0.0021(12) C17A 0.0403(17) 0.0336(14) 0.0389(16) -0.0014(13) -0.0039(13) -0.0025(13) C18A 0.0433(18) 0.0361(15) 0.0435(17) 0.0015(13) 0.0024(15) -0.0051(14) C19A 0.0436(17) 0.0346(14) 0.0354(15) 0.0022(12) 0.0052(14) 0.0033(13) C20A 0.0425(17) 0.0401(16) 0.0336(15) -0.0020(13) -0.0034(13) 0.0007(14) C21A 0.0382(16) 0.0334(14) 0.0339(15) -0.0019(12) -0.0008(13) -0.0010(12) C22A 0.050(2) 0.0497(19) 0.0438(18) 0.0065(16) 0.0006(16) -0.0060(17) C23A 0.0407(16) 0.0257(13) 0.0341(15) 0.0031(11) -0.0028(13) -0.0006(12) C24A 0.0380(16) 0.0310(14) 0.0401(16) 0.0002(12) 0.0017(14) -0.0008(12) C25A 0.0426(17) 0.0346(14) 0.0355(15) -0.0007(12) 0.0002(14) 0.0000(13) C26A 0.0456(17) 0.0316(14) 0.0322(14) 0.0034(12) -0.0060(13) -0.0026(13) C27A 0.0423(17) 0.0308(14) 0.0424(16) 0.0053(13) -0.0035(14) -0.0071(13) C28A 0.0404(17) 0.0339(14) 0.0364(15) 0.0035(12) 0.0027(13) -0.0022(13) C29A 0.059(2) 0.0355(15) 0.0360(16) 0.0031(13) -0.0071(16) -0.0101(15) F1A 0.133(4) 0.0650(18) 0.0458(16) 0.0088(13) 0.0413(19) 0.0262(19) F2A 0.131(3) 0.0417(16) 0.0511(16) 0.0159(13) 0.0126(18) -0.0197(19) F3A 0.0671(19) 0.133(3) 0.0654(18) 0.0487(19) -0.0061(15) -0.0098(18) F1B 0.077(5) 0.069(5) 0.063(5) -0.002(3) 0.000(3) 0.000(3) F2B 0.082(6) 0.086(6) 0.081(6) 0.006(3) 0.000(3) -0.007(3) F3B 0.058(4) 0.055(4) 0.051(4) 0.009(3) 0.002(3) 0.009(3) F4A 0.081(2) 0.0817(19) 0.0579(16) -0.0368(14) 0.0194(14) -0.0320(16) F5A 0.069(2) 0.092(2) 0.122(3) -0.054(2) -0.054(2) 0.0149(16) F6A 0.188(4) 0.0314(11) 0.0405(13) -0.0038(10) -0.0071(18) -0.0183(17) F4B 0.052(7) 0.051(7) 0.048(7) 0.000(3) -0.001(3) -0.003(3) F5B 0.051(7) 0.048(7) 0.050(7) -0.002(3) -0.002(3) -0.003(3) F6B 0.067(8) 0.066(8) 0.069(8) -0.004(3) -0.001(3) 0.002(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 -10 -7 0.0196 -12 1 -1 0.0472 -2 10 6 0.0289 12 0 2 0.0427 0 -5 18 0.0175 -1 6 -17 0.0120 5 -2 -18 0.0163 -1 -3 -20 0.0102 2 -6 -17 0.0107 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 C2 N1 C6 117.1(2) . . ? C2 N1 C10 114.7(2) . . ? C6 N1 C10 111.0(2) . . ? C3 N2 C15 119.0(2) . . ? C3 N2 C11 120.8(2) . . ? C15 N2 C11 114.1(2) . . ? O1 C1 C2 128.2(3) . . ? O1 C1 C5 124.3(2) . . ? C2 C1 C5 107.5(2) . . ? C3 C2 N1 127.1(3) . . ? C3 C2 C1 106.5(2) . . ? N1 C2 C1 125.9(2) . . ? C2 C3 N2 130.9(3) . . ? C2 C3 C4 109.8(2) . . ? N2 C3 C4 119.2(2) . . ? C5 C4 C16 127.0(3) . . ? C5 C4 C3 109.0(2) . . ? C16 C4 C3 123.7(3) . . ? C4 C5 C23 128.4(3) . . ? C4 C5 C1 107.0(2) . . ? C23 C5 C1 124.4(2) . . ? N1 C6 C7 110.2(2) . . ? C8 C7 C6 111.3(3) . . ? C7 C8 C9 110.7(3) . . ? C10 C9 C8 110.7(3) . . ? N1 C10 C9 110.0(3) . . ? N2 C11 C12 108.6(2) . . ? C11 C12 C13 110.4(3) . . ? C14 C13 C12 111.0(3) . . ? C15 C14 C13 110.7(3) . . ? N2 C15 C14 111.2(3) . . ? C21 C16 C17 118.4(3) . . ? C21 C16 C4 120.9(3) . . ? C17 C16 C4 120.7(3) . . ? C18 C17 C16 120.8(3) . . ? C19 C18 C17 120.0(3) . . ? C18 C19 C20 119.8(3) . . ? C18 C19 C22 119.4(3) . . ? C20 C19 C22 120.7(3) . . ? C21 C20 C19 120.0(3) . . ? C20 C21 C16 120.8(3) . . ? F1 C22 F3 106.2(3) . . ? F1 C22 F2 105.8(3) . . ? F3 C22 F2 105.8(3) . . ? F1 C22 C19 113.1(3) . . ? F3 C22 C19 113.7(3) . . ? F2 C22 C19 111.6(3) . . ? C24 C23 C28 118.7(3) . . ? C24 C23 C5 120.5(3) . . ? C28 C23 C5 120.8(3) . . ? C25 C24 C23 121.0(3) . . ? C24 C25 C26 119.7(3) . . ? C27 C26 C25 119.9(3) . . ? C27 C26 C29 120.4(3) . . ? C25 C26 C29 119.6(3) . . ? C26 C27 C28 120.1(3) . . ? C27 C28 C23 120.4(3) . . ? F6 C29 F5 105.4(3) . . ? F6 C29 F4 106.4(3) . . ? F5 C29 F4 105.2(3) . . ? F6 C29 C26 113.5(3) . . ? F5 C29 C26 112.8(3) . . ? F4 C29 C26 112.8(3) . . ? C2A N1A C10A 113.8(2) . . ? C2A N1A C6A 115.4(2) . . ? C10A N1A C6A 110.8(2) . . ? C3A N2A C11A 119.7(2) . . ? C3A N2A C15A 118.4(2) . . ? C11A N2A C15A 113.7(2) . . ? O1A C1A C2A 127.7(3) . . ? O1A C1A C5A 125.2(3) . . ? C2A C1A C5A 107.0(2) . . ? C3A C2A N1A 127.0(3) . . ? C3A C2A C1A 107.2(2) . . ? N1A C2A C1A 124.6(3) . . ? C2A C3A N2A 130.1(3) . . ? C2A C3A C4A 109.3(2) . . ? N2A C3A C4A 120.5(2) . . ? C5A C4A C16A 126.3(3) . . ? C5A C4A C3A 108.2(2) . . ? C16A C4A C3A 125.3(3) . . ? C4A C5A C23A 128.4(3) . . ? C4A C5A C1A 107.8(2) . . ? C23A C5A C1A 123.6(2) . . ? N1A C6A C7A 110.0(3) . . ? C8A C7A C6A 111.0(3) . . ? C7A C8A C9A 110.2(3) . . ? C10A C9A C8A 110.6(3) . . ? N1A C10A C9A 110.6(3) . . ? N2A C11A C12A 109.0(2) . . ? C13A C12A C11A 110.9(3) . . ? C12A C13A C14A 110.4(3) . . ? C13A C14A C15A 110.7(3) . . ? N2A C15A C14A 111.2(3) . . ? C21A C16A C17A 118.1(3) . . ? C21A C16A C4A 120.8(3) . . ? C17A C16A C4A 121.1(3) . . ? C18A C17A C16A 120.7(3) . . ? C17A C18A C19A 120.2(3) . . ? C18A C19A C20A 120.0(3) . . ? C18A C19A C22A 120.4(3) . . ? C20A C19A C22A 119.6(3) . . ? C21A C20A C19A 119.6(3) . . ? C20A C21A C16A 121.4(3) . . ? F1B C22A F2B 113.1(11) . . ? F3A C22A F2A 107.8(4) . . ? F3A C22A F1A 102.4(4) . . ? F2A C22A F1A 104.6(3) . . ? F1B C22A F3B 98.9(9) . . ? F2B C22A F3B 103.2(10) . . ? F1B C22A C19A 117.2(7) . . ? F2B C22A C19A 113.9(8) . . ? F3A C22A C19A 114.1(3) . . ? F2A C22A C19A 114.2(3) . . ? F1A C22A C19A 112.7(3) . . ? F3B C22A C19A 108.2(5) . . ? C28A C23A C24A 119.0(3) . . ? C28A C23A C5A 120.2(3) . . ? C24A C23A C5A 120.7(3) . . ? C25A C24A C23A 120.6(3) . . ? C24A C25A C26A 119.7(3) . . ? C27A C26A C25A 120.3(3) . . ? C27A C26A C29A 118.9(3) . . ? C25A C26A C29A 120.8(3) . . ? C28A C27A C26A 119.9(3) . . ? C27A C28A C23A 120.4(3) . . ? F4B C29A F6B 111.6(17) . . ? F5A C29A F6A 107.3(3) . . ? F4B C29A F5B 108.5(15) . . ? F6B C29A F5B 102.7(16) . . ? F5A C29A F4A 105.1(3) . . ? F6A C29A F4A 103.7(3) . . ? F4B C29A C26A 116.2(10) . . ? F6B C29A C26A 107.5(11) . . ? F5A C29A C26A 113.7(3) . . ? F6A C29A C26A 112.8(3) . . ? F5B C29A C26A 109.5(9) . . ? F4A C29A C26A 113.4(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 F1 C22 1.313(4) . ? F2 C22 1.334(4) . ? F3 C22 1.322(4) . ? F4 C29 1.325(4) . ? F5 C29 1.323(4) . ? F6 C29 1.321(4) . ? O1 C1 1.229(3) . ? N1 C2 1.414(4) . ? N1 C6 1.463(4) . ? N1 C10 1.468(4) . ? N2 C3 1.377(3) . ? N2 C15 1.463(4) . ? N2 C11 1.468(4) . ? C1 C2 1.484(4) . ? C1 C5 1.507(4) . ? C2 C3 1.359(4) . ? C3 C4 1.513(4) . ? C4 C5 1.347(4) . ? C4 C16 1.476(4) . ? C5 C23 1.475(4) . ? C6 C7 1.515(4) . ? C7 C8 1.505(5) . ? C8 C9 1.527(5) . ? C9 C10 1.518(4) . ? C11 C12 1.523(4) . ? C12 C13 1.527(5) . ? C13 C14 1.527(5) . ? C14 C15 1.516(5) . ? C16 C21 1.387(4) . ? C16 C17 1.391(4) . ? C17 C18 1.387(4) . ? C18 C19 1.373(5) . ? C19 C20 1.387(4) . ? C19 C22 1.501(4) . ? C20 C21 1.382(4) . ? C23 C24 1.388(4) . ? C23 C28 1.392(4) . ? C24 C25 1.383(4) . ? C25 C26 1.386(4) . ? C26 C27 1.384(4) . ? C26 C29 1.491(4) . ? C27 C28 1.384(4) . ? O1A C1A 1.227(3) . ? N1A C2A 1.422(4) . ? N1A C10A 1.453(4) . ? N1A C6A 1.463(4) . ? N2A C3A 1.371(3) . ? N2A C11A 1.465(4) . ? N2A C15A 1.470(4) . ? C1A C2A 1.474(4) . ? C1A C5A 1.507(4) . ? C2A C3A 1.365(4) . ? C3A C4A 1.522(4) . ? C4A C5A 1.349(4) . ? C4A C16A 1.477(4) . ? C5A C23A 1.472(4) . ? C6A C7A 1.513(4) . ? C7A C8A 1.501(5) . ? C8A C9A 1.520(5) . ? C9A C10A 1.517(4) . ? C11A C12A 1.523(4) . ? C12A C13A 1.514(5) . ? C13A C14A 1.521(5) . ? C14A C15A 1.525(4) . ? C16A C21A 1.392(4) . ? C16A C17A 1.396(4) . ? C17A C18A 1.381(4) . ? C18A C19A 1.383(4) . ? C19A C20A 1.386(4) . ? C19A C22A 1.486(4) . ? C20A C21A 1.379(4) . ? C22A F1B 1.214(14) . ? C22A F2B 1.237(17) . ? C22A F3A 1.319(5) . ? C22A F2A 1.319(5) . ? C22A F1A 1.345(5) . ? C22A F3B 1.404(12) . ? C23A C28A 1.395(4) . ? C23A C24A 1.395(4) . ? C24A C25A 1.385(4) . ? C25A C26A 1.387(4) . ? C26A C27A 1.387(4) . ? C26A C29A 1.493(4) . ? C27A C28A 1.385(4) . ? C29A F4B 1.157(19) . ? C29A F6B 1.24(2) . ? C29A F5A 1.301(4) . ? C29A F6A 1.322(4) . ? C29A F5B 1.330(19) . ? C29A F4A 1.342(4) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C2 C3 -162.6(3) . . . . ? C10 N1 C2 C3 64.7(4) . . . . ? C6 N1 C2 C1 26.4(4) . . . . ? C10 N1 C2 C1 -106.4(3) . . . . ? O1 C1 C2 C3 -176.0(3) . . . . ? C5 C1 C2 C3 3.7(3) . . . . ? O1 C1 C2 N1 -3.4(5) . . . . ? C5 C1 C2 N1 176.3(3) . . . . ? N1 C2 C3 N2 7.5(5) . . . . ? C1 C2 C3 N2 180.0(3) . . . . ? N1 C2 C3 C4 -176.6(3) . . . . ? C1 C2 C3 C4 -4.1(3) . . . . ? C15 N2 C3 C2 -125.8(4) . . . . ? C11 N2 C3 C2 25.1(5) . . . . ? C15 N2 C3 C4 58.7(4) . . . . ? C11 N2 C3 C4 -150.5(3) . . . . ? C2 C3 C4 C5 3.1(4) . . . . ? N2 C3 C4 C5 179.6(3) . . . . ? C2 C3 C4 C16 -171.3(3) . . . . ? N2 C3 C4 C16 5.2(4) . . . . ? C16 C4 C5 C23 -1.9(5) . . . . ? C3 C4 C5 C23 -176.0(3) . . . . ? C16 C4 C5 C1 173.5(3) . . . . ? C3 C4 C5 C1 -0.6(3) . . . . ? O1 C1 C5 C4 177.9(3) . . . . ? C2 C1 C5 C4 -1.8(3) . . . . ? O1 C1 C5 C23 -6.5(5) . . . . ? C2 C1 C5 C23 173.8(3) . . . . ? C2 N1 C6 C7 164.7(3) . . . . ? C10 N1 C6 C7 -60.9(3) . . . . ? N1 C6 C7 C8 56.6(4) . . . . ? C6 C7 C8 C9 -52.8(4) . . . . ? C7 C8 C9 C10 52.9(4) . . . . ? C2 N1 C10 C9 -163.3(3) . . . . ? C6 N1 C10 C9 61.2(3) . . . . ? C8 C9 C10 N1 -56.7(4) . . . . ? C3 N2 C11 C12 148.3(3) . . . . ? C15 N2 C11 C12 -59.5(4) . . . . ? N2 C11 C12 C13 57.7(4) . . . . ? C11 C12 C13 C14 -56.0(4) . . . . ? C12 C13 C14 C15 52.9(4) . . . . ? C3 N2 C15 C14 -149.7(3) . . . . ? C11 N2 C15 C14 57.6(4) . . . . ? C13 C14 C15 N2 -52.5(4) . . . . ? C5 C4 C16 C21 57.8(4) . . . . ? C3 C4 C16 C21 -128.9(3) . . . . ? C5 C4 C16 C17 -122.8(4) . . . . ? C3 C4 C16 C17 50.5(4) . . . . ? C21 C16 C17 C18 0.0(5) . . . . ? C4 C16 C17 C18 -179.4(3) . . . . ? C16 C17 C18 C19 1.1(5) . . . . ? C17 C18 C19 C20 -1.5(5) . . . . ? C17 C18 C19 C22 179.4(3) . . . . ? C18 C19 C20 C21 0.8(5) . . . . ? C22 C19 C20 C21 179.8(3) . . . . ? C19 C20 C21 C16 0.4(4) . . . . ? C17 C16 C21 C20 -0.8(4) . . . . ? C4 C16 C21 C20 178.6(3) . . . . ? C18 C19 C22 F1 73.8(4) . . . . ? C20 C19 C22 F1 -105.2(4) . . . . ? C18 C19 C22 F3 -165.0(3) . . . . ? C20 C19 C22 F3 16.0(4) . . . . ? C18 C19 C22 F2 -45.4(4) . . . . ? C20 C19 C22 F2 135.6(3) . . . . ? C4 C5 C23 C24 51.4(4) . . . . ? C1 C5 C23 C24 -123.3(3) . . . . ? C4 C5 C23 C28 -127.4(3) . . . . ? C1 C5 C23 C28 57.8(4) . . . . ? C28 C23 C24 C25 2.4(4) . . . . ? C5 C23 C24 C25 -176.5(3) . . . . ? C23 C24 C25 C26 1.0(5) . . . . ? C24 C25 C26 C27 -2.8(5) . . . . ? C24 C25 C26 C29 174.4(3) . . . . ? C25 C26 C27 C28 1.2(4) . . . . ? C29 C26 C27 C28 -175.9(3) . . . . ? C26 C27 C28 C23 2.2(4) . . . . ? C24 C23 C28 C27 -4.0(4) . . . . ? C5 C23 C28 C27 174.9(3) . . . . ? C27 C26 C29 F6 -35.0(4) . . . . ? C25 C26 C29 F6 147.9(3) . . . . ? C27 C26 C29 F5 84.8(4) . . . . ? C25 C26 C29 F5 -92.3(4) . . . . ? C27 C26 C29 F4 -156.2(3) . . . . ? C25 C26 C29 F4 26.7(4) . . . . ? C10A N1A C2A C3A 84.7(4) . . . . ? C6A N1A C2A C3A -145.6(3) . . . . ? C10A N1A C2A C1A -81.1(4) . . . . ? C6A N1A C2A C1A 48.6(4) . . . . ? O1A C1A C2A C3A -170.3(3) . . . . ? C5A C1A C2A C3A 7.1(3) . . . . ? O1A C1A C2A N1A -2.1(5) . . . . ? C5A C1A C2A N1A 175.4(3) . . . . ? N1A C2A C3A N2A 7.6(5) . . . . ? C1A C2A C3A N2A 175.4(3) . . . . ? N1A C2A C3A C4A -174.9(3) . . . . ? C1A C2A C3A C4A -7.1(3) . . . . ? C11A N2A C3A C2A 17.9(5) . . . . ? C15A N2A C3A C2A -128.7(3) . . . . ? C11A N2A C3A C4A -159.4(3) . . . . ? C15A N2A C3A C4A 54.1(4) . . . . ? C2A C3A C4A C5A 4.4(3) . . . . ? N2A C3A C4A C5A -177.8(3) . . . . ? C2A C3A C4A C16A -171.5(3) . . . . ? N2A C3A C4A C16A 6.3(4) . . . . ? C16A C4A C5A C23A 1.0(5) . . . . ? C3A C4A C5A C23A -174.9(3) . . . . ? C16A C4A C5A C1A 176.1(3) . . . . ? C3A C4A C5A C1A 0.2(3) . . . . ? O1A C1A C5A C4A 173.1(3) . . . . ? C2A C1A C5A C4A -4.4(3) . . . . ? O1A C1A C5A C23A -11.5(4) . . . . ? C2A C1A C5A C23A 171.0(3) . . . . ? C2A N1A C6A C7A 167.9(3) . . . . ? C10A N1A C6A C7A -60.9(3) . . . . ? N1A C6A C7A C8A 57.8(4) . . . . ? C6A C7A C8A C9A -54.1(4) . . . . ? C7A C8A C9A C10A 53.3(4) . . . . ? C2A N1A C10A C9A -167.4(3) . . . . ? C6A N1A C10A C9A 60.7(4) . . . . ? C8A C9A C10A N1A -56.6(4) . . . . ? C3A N2A C11A C12A 153.8(3) . . . . ? C15A N2A C11A C12A -58.2(4) . . . . ? N2A C11A C12A C13A 57.8(3) . . . . ? C11A C12A C13A C14A -56.8(4) . . . . ? C12A C13A C14A C15A 53.9(4) . . . . ? C3A N2A C15A C14A -154.9(3) . . . . ? C11A N2A C15A C14A 56.6(3) . . . . ? C13A C14A C15A N2A -53.1(4) . . . . ? C5A C4A C16A C21A 46.6(4) . . . . ? C3A C4A C16A C21A -138.2(3) . . . . ? C5A C4A C16A C17A -132.7(3) . . . . ? C3A C4A C16A C17A 42.5(4) . . . . ? C21A C16A C17A C18A 0.8(4) . . . . ? C4A C16A C17A C18A -179.8(3) . . . . ? C16A C17A C18A C19A 0.7(5) . . . . ? C17A C18A C19A C20A -1.5(5) . . . . ? C17A C18A C19A C22A 179.2(3) . . . . ? C18A C19A C20A C21A 0.8(5) . . . . ? C22A C19A C20A C21A -179.9(3) . . . . ? C19A C20A C21A C16A 0.7(4) . . . . ? C17A C16A C21A C20A -1.5(4) . . . . ? C4A C16A C21A C20A 179.1(3) . . . . ? C18A C19A C22A F1B 144.0(11) . . . . ? C20A C19A C22A F1B -35.2(11) . . . . ? C18A C19A C22A F2B 8.7(12) . . . . ? C20A C19A C22A F2B -170.6(11) . . . . ? C18A C19A C22A F3A -155.1(4) . . . . ? C20A C19A C22A F3A 25.6(5) . . . . ? C18A C19A C22A F2A -30.5(5) . . . . ? C20A C19A C22A F2A 150.2(4) . . . . ? C18A C19A C22A F1A 88.7(4) . . . . ? C20A C19A C22A F1A -90.6(4) . . . . ? C18A C19A C22A F3B -105.4(7) . . . . ? C20A C19A C22A F3B 75.3(7) . . . . ? C4A C5A C23A C28A -131.0(3) . . . . ? C1A C5A C23A C28A 54.6(4) . . . . ? C4A C5A C23A C24A 47.4(5) . . . . ? C1A C5A C23A C24A -127.0(3) . . . . ? C28A C23A C24A C25A 2.0(4) . . . . ? C5A C23A C24A C25A -176.4(3) . . . . ? C23A C24A C25A C26A -0.1(4) . . . . ? C24A C25A C26A C27A -1.1(4) . . . . ? C24A C25A C26A C29A 177.7(3) . . . . ? C25A C26A C27A C28A 0.3(4) . . . . ? C29A C26A C27A C28A -178.6(3) . . . . ? C26A C27A C28A C23A 1.7(4) . . . . ? C24A C23A C28A C27A -2.8(4) . . . . ? C5A C23A C28A C27A 175.6(3) . . . . ? C27A C26A C29A F4B 119.5(15) . . . . ? C25A C26A C29A F4B -59.3(15) . . . . ? C27A C26A C29A F6B -114.6(15) . . . . ? C25A C26A C29A F6B 66.6(15) . . . . ? C27A C26A C29A F5A 59.2(4) . . . . ? C25A C26A C29A F5A -119.6(4) . . . . ? C27A C26A C29A F6A -63.2(4) . . . . ? C25A C26A C29A F6A 117.9(4) . . . . ? C27A C26A C29A F5B -3.8(12) . . . . ? C25A C26A C29A F5B 177.4(11) . . . . ? C27A C26A C29A F4A 179.2(3) . . . . ? C25A C26A C29A F4A 0.4(4) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 1.1405 -10.3710 -6.8218 -0.2360 0.4334 0.8698 -11.9602 1.4235 -1.4900 -0.3623 0.6670 -0.6510 -2.3552 10.2583 6.4954 0.1924 -0.3531 -0.9156 12.0085 -0.0094 2.4620 0.4013 -0.7387 0.5416 0.1233 -5.4419 18.0481 0.8593 0.4673 0.2078 -0.8448 6.2136 -17.0821 -0.8360 -0.4547 -0.3073 5.1379 -2.1515 -18.3521 -0.7102 -0.3858 0.5888 -0.9997 -2.7981 -20.0282 -0.9314 0.0237 0.3632 2.1523 -5.8349 -17.2454 -0.7131 0.0178 0.7008