#------------------------------------------------------------------------------ #$Date: 2019-02-10 03:43:51 +0200 (Sun, 10 Feb 2019) $ #$Revision: 213591 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/81/7058163.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_7058163 loop_ _publ_author_name 'Chen, Yuan' 'Fuyue , Liuting' 'wang, gangqiang' 'Wang, Hang' 'Lu, Chun' 'Guo, Haibing' 'St. Amant, Chiara' 'Sun, Shaofa' 'Xing, Yalan' _publ_section_title ; Synthesis of 1,2,4-Oxadiazolidines via [3+2] Cycloaddition of Nitrones with Carbodiimides ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/C9NJ00030E _journal_year 2019 _chemical_absolute_configuration unk _chemical_formula_moiety 'C21 H18 F N3 O' _chemical_formula_sum 'C21 H18 F N3 O' _chemical_formula_weight 347.38 _chemical_name_systematic 1 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2018-11-28 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2018-12-19 deposited with the CCDC. 2019-02-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.446(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 9.1744(2) _cell_length_b 23.9422(5) _cell_length_c 16.3375(4) _cell_measurement_reflns_used 10391 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 76.3140 _cell_measurement_theta_min 3.2750 _cell_volume 3587.48(14) _computing_cell_refinement 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.960 _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 -29.00 3.00 0.50 0.28 -- -43.80 82.00 43.00 64 2 \w -72.00 -35.00 0.50 0.28 -- -43.80 82.00 43.00 74 3 \w -93.00 -68.00 0.50 1.14 -- -90.25 82.00 43.00 50 4 \w -117.00 -13.00 0.50 0.28 -- -43.80 -82.00 -77.00 208 5 \w 41.00 66.00 0.50 0.28 -- 43.80 82.00 43.00 50 6 \w 82.00 177.00 0.50 1.14 -- 111.75 82.00 43.00 190 7 \w 120.00 174.00 0.50 1.14 -- 111.75 77.00 0.00 108 8 \w 130.00 174.00 0.50 1.14 -- 111.75 125.00 -90.00 88 9 \w 100.00 126.00 0.50 1.14 -- 111.75 125.00 -90.00 52 10 \w 77.00 122.00 0.50 0.28 -- 43.80 178.00 -30.00 90 11 \w 38.00 134.00 0.50 1.14 -- 111.75 -61.00 -30.00 192 12 \w 108.00 136.00 0.50 1.14 -- 111.75 -82.00 -77.00 56 13 \w 69.00 121.00 0.50 1.14 -- 111.75-125.00-180.00 104 14 \w 54.00 94.00 0.50 1.14 -- 111.75 -82.00 -77.00 80 15 \w 52.00 107.00 0.50 1.14 -- 111.75 -94.00-120.00 110 16 \w 38.00 64.00 0.50 1.14 -- 111.75-125.00-180.00 52 17 \w 0.00 78.00 0.50 0.28 -- 43.80 -99.00 90.00 156 18 \w 38.00 78.00 0.50 1.14 -- 111.75 -94.00 120.00 80 19 \w -86.00 -61.00 0.50 1.14 -- -90.25 -82.00 -77.00 50 20 \w -164.00 -86.00 0.50 1.14 -- -90.25 -94.00 0.00 156 21 \w -160.00 -62.00 0.50 1.14 -- -90.25 -77.00 -30.00 196 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0898603000 _diffrn_orient_matrix_UB_12 -0.0540324000 _diffrn_orient_matrix_UB_13 0.0076384000 _diffrn_orient_matrix_UB_21 -0.0388731000 _diffrn_orient_matrix_UB_22 0.0164008000 _diffrn_orient_matrix_UB_23 0.0880173000 _diffrn_orient_matrix_UB_31 -0.1365347000 _diffrn_orient_matrix_UB_32 0.0308373000 _diffrn_orient_matrix_UB_33 -0.0330127000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_unetI/netI 0.0515 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.960 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 23757 _diffrn_reflns_point_group_measured_fraction_full 0.734 _diffrn_reflns_point_group_measured_fraction_max 0.694 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.886 _diffrn_reflns_theta_min 2.705 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.718 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.58545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.286 _exptl_crystal_description block _exptl_crystal_F_000 1456 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.510 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.117 _refine_ls_abs_structure_details ; Flack x determined using 2078 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.21(16) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 929 _refine_ls_number_reflns 10531 _refine_ls_number_restraints 65 _refine_ls_restrained_S_all 1.533 _refine_ls_R_factor_all 0.1358 _refine_ls_R_factor_gt 0.1235 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1640 _refine_ls_wR_factor_ref 0.2295 _reflns_Friedel_coverage 0.412 _reflns_Friedel_fraction_full 0.457 _reflns_Friedel_fraction_max 0.416 _reflns_number_gt 8470 _reflns_number_total 10531 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL fengchuanqi-cy-36-2_a.res in P2(1) fengchuanqi-cy-36-2.res created by SHELXL-2018/3 at 18:50:10 on 28-Nov-2018 REM Old TITL FengChuanqi-CY-36-2 in P2(1)/m REM SHELXT solution in P2(1) REM R1 0.167, Rweak 0.029, Alpha 0.002, Orientation as input REM Flack x = 0.326 ( 0.143 ) from Parsons' quotients REM Formula found by SHELXT: C86 N11 O8 CELL 1.54184 9.1744 23.9422 16.3375 90 91.446 90 ZERR 8 0.0002 0.0005 0.0004 0 0.002 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H F N O UNIT 168 144 8 24 8 DELU F53 C31 DELU O89 N88 DELU C57 C58 C59 DELU C84 C85 DELU F79 C58 DELU F105 C85 DELU C80 C85 DELU C80 C81 SIMU 0.002 0.004 2 F53 C31 SIMU 0.002 0.004 2 O89 N88 SIMU 0.002 0.004 2 C57 C58 C59 SIMU 0.002 0.004 2 C84 C85 SIMU 0.002 0.004 2 F79 C58 SIMU 0.002 0.004 2 F105 C85 SIMU 0.002 0.004 2 C80 C85 SIMU 0.002 0.004 2 C80 C81 EADP F79 C58 EADP F105 C85 L.S. 20 PLAN 14 BOND $H LIST 6 ABIN fmap 2 acta REM REM REM WGHT 0.200000 FVAR 0.28333 O1 5 1.514735 1.010868 0.841159 11.00000 0.04378 0.07023 = 0.06505 0.00160 -0.00655 -0.00629 O36 5 0.787321 0.510925 0.656245 11.00000 0.05236 0.06451 = 0.06632 -0.00466 0.00137 -0.00839 O63 5 1.286220 0.496965 0.621537 11.00000 0.04941 0.05866 = 0.05884 -0.00454 0.00155 0.00799 O89 5 0.010735 -0.017736 0.878007 11.00000 0.04560 0.06679 = 0.05988 -0.00485 -0.00020 0.00381 N3 4 1.463919 0.978005 0.910105 11.00000 0.04880 0.06222 = 0.05760 -0.00172 -0.00433 -0.00037 N33 4 0.619071 0.452220 0.702217 11.00000 0.04355 0.05433 = 0.05949 -0.00566 0.01187 -0.00546 N62 4 1.238231 0.528112 0.693177 11.00000 0.05051 0.05352 = 0.05147 0.00202 0.00273 0.00629 N2 4 1.349091 0.951697 0.788479 11.00000 0.04540 0.06113 = 0.05384 0.00597 -0.01453 -0.00222 N60 4 1.121443 0.558318 0.573657 11.00000 0.04862 0.05701 = 0.06085 -0.00686 -0.00574 0.00816 N35 4 0.733390 0.479134 0.584936 11.00000 0.04793 0.05951 = 0.05454 0.00024 0.00154 -0.00331 N97 4 -0.069738 -0.031699 1.009796 11.00000 0.05989 0.06481 = 0.06668 0.00740 0.00682 0.00646 N86 4 -0.154023 0.042126 0.924130 11.00000 0.04263 0.05581 = 0.05812 -0.00037 0.00624 0.00545 N71 4 1.196909 0.484691 0.488509 11.00000 0.06368 0.05417 = 0.06686 -0.00367 -0.00370 0.00907 N88 4 -0.032058 0.016942 0.807291 11.00000 0.04723 0.06604 = 0.05648 -0.00348 -0.00078 0.00338 C34 1 0.663088 0.430610 0.622552 11.00000 0.04565 0.05826 = 0.05000 -0.00368 0.00281 0.00148 AFIX 13 H34 2 0.575773 0.420574 0.590021 11.00000 -1.20000 AFIX 0 N44 4 0.710277 0.524112 0.788068 11.00000 0.06313 0.05422 = 0.06703 -0.00579 -0.00148 -0.00685 N1 4 1.435669 1.026027 0.706169 11.00000 0.05607 0.06197 = 0.06418 0.00485 -0.00611 -0.00724 C90 1 -0.071919 -0.004967 0.942957 11.00000 0.04845 0.05919 = 0.05304 -0.00123 0.00381 -0.00326 C64 1 1.199126 0.510824 0.555505 11.00000 0.04363 0.04894 = 0.06179 0.00178 -0.00142 0.00659 C91 1 0.003467 0.113424 0.858810 11.00000 0.04470 0.05797 = 0.05207 0.00593 -0.00042 0.00386 C61 1 1.172894 0.578228 0.654008 11.00000 0.05350 0.05458 = 0.05812 0.00492 0.00161 0.00519 AFIX 13 H61 2 1.088492 0.589860 0.685409 11.00000 -1.20000 AFIX 0 C37 1 0.703079 0.498507 0.719722 11.00000 0.04367 0.05304 = 0.05593 0.00159 -0.00106 -0.00510 C72 1 1.265384 0.429826 0.486580 11.00000 0.06423 0.05475 = 0.05600 -0.00584 -0.00915 0.00394 C27 1 0.524755 0.423962 0.753593 11.00000 0.03725 0.05984 = 0.04946 0.00954 0.00684 0.00637 C65 1 1.278411 0.626005 0.650764 11.00000 0.05235 0.05208 = 0.06169 0.00569 0.00128 0.00381 C87 1 -0.102112 0.065111 0.846394 11.00000 0.03744 0.06032 = 0.05418 0.00070 -0.00113 0.00005 AFIX 13 H87 2 -0.185713 0.077416 0.812492 11.00000 -1.20000 AFIX 0 C7 1 1.392339 0.929080 0.871086 11.00000 0.04869 0.06156 = 0.05137 0.00303 -0.00316 -0.00051 AFIX 13 H7 2 1.305069 0.918964 0.901126 11.00000 -1.20000 AFIX 0 C81 1 -0.247015 0.072583 0.975514 11.00000 0.05696 0.07560 = 0.08614 -0.00887 0.01096 0.00608 C1 1 1.491832 0.880611 0.867428 11.00000 0.04644 0.06039 = 0.05334 0.00054 -0.00712 -0.00393 C32 1 0.462265 0.374842 0.726109 11.00000 0.04974 0.06942 = 0.06913 -0.00097 0.01321 -0.01165 AFIX 43 H32 2 0.483034 0.360973 0.674525 11.00000 -1.20000 AFIX 0 C13 1 1.209846 0.944430 0.657568 11.00000 0.04594 0.07090 = 0.06123 0.00167 -0.00729 -0.00444 AFIX 43 H13 2 1.248696 0.977912 0.639219 11.00000 -1.20000 AFIX 0 C8 1 1.250555 0.923293 0.735705 11.00000 0.04586 0.06019 = 0.05967 0.00434 -0.00325 -0.00012 C15 1 1.507085 1.078446 0.704745 11.00000 0.05659 0.05897 = 0.06382 0.00605 -0.00242 -0.00344 C78 1 1.134936 0.492237 0.733555 11.00000 0.05349 0.07231 = 0.07230 0.01638 0.01087 0.00375 AFIX 137 H78A 2 1.061366 0.480184 0.694629 11.00000 -1.50000 H78B 2 1.090063 0.512520 0.776904 11.00000 -1.50000 H78C 2 1.184991 0.460255 0.755864 11.00000 -1.50000 AFIX 0 C98 1 0.005489 -0.082921 1.016126 11.00000 0.05930 0.05563 = 0.06677 0.00285 0.00964 0.00686 C54 1 1.023360 0.586468 0.522497 11.00000 0.04296 0.06068 = 0.06278 0.01058 0.00434 0.00242 C82 1 -0.288780 0.053252 1.050577 11.00000 0.05448 0.07362 = 0.05622 -0.00757 0.00224 -0.00404 AFIX 43 H82 2 -0.255425 0.018585 1.068619 11.00000 -1.20000 AFIX 0 C38 1 0.764404 0.380442 0.627970 11.00000 0.04827 0.05983 = 0.06553 0.00564 0.00663 -0.00087 C73 1 1.370445 0.419439 0.429595 11.00000 0.07641 0.06552 = 0.05037 -0.00859 -0.00600 0.00737 AFIX 43 H73 2 1.396746 0.447291 0.393139 11.00000 -1.20000 AFIX 0 C9 1 1.191171 0.872367 0.762950 11.00000 0.05944 0.06585 = 0.06081 0.00345 -0.01205 -0.00517 AFIX 43 H9 2 1.217127 0.857503 0.813850 11.00000 -1.20000 AFIX 0 C55 1 0.970332 0.566673 0.449536 11.00000 0.05059 0.06739 = 0.06426 0.00882 -0.01202 -0.00804 AFIX 43 H55 2 1.001325 0.531763 0.432078 11.00000 -1.20000 AFIX 0 C14 1 1.429468 0.998556 0.772640 11.00000 0.05066 0.06042 = 0.05523 0.00313 -0.00648 -0.00477 C70 1 1.363149 0.635305 0.584039 11.00000 0.06358 0.06566 = 0.06774 -0.00187 0.00726 -0.00619 AFIX 43 H70 2 1.352883 0.612556 0.538114 11.00000 -1.20000 AFIX 0 C85 1 -0.395231 0.152705 0.994900 11.00000 0.08728 0.09416 = 0.10770 -0.00734 0.00977 0.01357 C92 1 0.085429 0.118593 0.929736 11.00000 0.06616 0.07022 = 0.05458 -0.00161 -0.00811 -0.00901 AFIX 43 H92 2 0.076981 0.092186 0.971092 11.00000 -1.20000 AFIX 0 C28 1 0.489532 0.443259 0.831175 11.00000 0.06040 0.07090 = 0.06170 0.00481 0.00965 0.00598 AFIX 43 H28 2 0.529330 0.476463 0.851063 11.00000 -1.20000 AFIX 0 C59 1 0.973389 0.638051 0.548142 11.00000 0.09029 0.07303 = 0.12409 0.01305 -0.01473 0.02982 AFIX 43 H59 2 1.008810 0.652710 0.597464 11.00000 -1.20000 AFIX 0 C16 1 1.617113 1.086801 0.648757 11.00000 0.08127 0.06310 = 0.06869 0.00124 0.00859 -0.00480 AFIX 43 H16 2 1.649495 1.058006 0.615611 11.00000 -1.20000 AFIX 0 C66 1 1.290956 0.661784 0.717375 11.00000 0.08956 0.06548 = 0.07094 -0.00891 -0.00107 -0.00679 AFIX 43 H66 2 1.232829 0.656166 0.762463 11.00000 -1.20000 AFIX 0 C74 1 1.436150 0.368013 0.426698 11.00000 0.09667 0.07780 = 0.06629 -0.01233 0.00340 0.01973 AFIX 43 H74 2 1.511308 0.361902 0.390615 11.00000 -1.20000 AFIX 0 C47 1 0.789478 0.575688 0.791538 11.00000 0.06514 0.05679 = 0.06269 -0.00752 0.00522 -0.00762 C12 1 1.112058 0.914939 0.608875 11.00000 0.06618 0.07462 = 0.06116 -0.00414 -0.01126 0.00093 AFIX 43 H12 2 1.085092 0.928834 0.557536 11.00000 -1.20000 AFIX 0 C104 1 -0.135803 -0.017462 0.759504 11.00000 0.05474 0.08797 = 0.07492 -0.02064 -0.01361 0.00035 AFIX 137 H10A 2 -0.085790 -0.048988 0.737192 11.00000 -1.50000 H10B 2 -0.177914 0.004420 0.715715 11.00000 -1.50000 H10C 2 -0.211526 -0.030309 0.794366 11.00000 -1.50000 AFIX 0 C11 1 1.052011 0.863866 0.635710 11.00000 0.06034 0.07094 = 0.07866 -0.01986 -0.02361 -0.00403 AFIX 43 H11 2 0.986853 0.843882 0.602464 11.00000 -1.20000 AFIX 0 C20 1 1.463791 1.122205 0.753854 11.00000 0.07264 0.05796 = 0.08420 0.00251 0.01442 0.00023 AFIX 43 H20 2 1.388718 1.116720 0.790202 11.00000 -1.20000 AFIX 0 C18 1 1.639386 1.182812 0.694175 11.00000 0.10100 0.07680 = 0.08346 -0.00017 0.00269 -0.02478 AFIX 43 H18 2 1.685572 1.217309 0.691302 11.00000 -1.20000 AFIX 0 C31 1 0.368052 0.346400 0.776394 11.00000 0.10862 0.07769 = 0.11663 0.01594 0.03982 -0.03031 C49 1 0.829506 0.670230 0.749553 11.00000 0.09149 0.06390 = 0.07258 0.00084 0.00431 0.00274 AFIX 43 H49 2 0.805993 0.700112 0.715330 11.00000 -1.20000 AFIX 0 C56 1 0.871716 0.596256 0.399707 11.00000 0.07676 0.08535 = 0.06958 0.01086 -0.01886 -0.00012 AFIX 43 H56 2 0.837936 0.581646 0.350011 11.00000 -1.20000 AFIX 0 C76 1 1.285188 0.335685 0.533957 11.00000 0.10289 0.05146 = 0.07988 0.00493 -0.00423 -0.00869 AFIX 43 H76 2 1.257124 0.307664 0.569697 11.00000 -1.20000 AFIX 0 C80 1 -0.298399 0.123024 0.947745 11.00000 0.06972 0.08255 = 0.09516 -0.00654 0.01127 0.00877 AFIX 43 H80 2 -0.268695 0.137197 0.897857 11.00000 -1.20000 AFIX 0 C77 1 1.220139 0.388639 0.537508 11.00000 0.06966 0.06493 = 0.07011 -0.00585 0.00897 -0.00281 AFIX 43 H77 2 1.146671 0.395559 0.574368 11.00000 -1.20000 AFIX 0 C2 1 1.582258 0.869563 0.801086 11.00000 0.06127 0.07676 = 0.07155 -0.01088 0.00303 -0.00281 AFIX 43 H2 2 1.580581 0.893807 0.756597 11.00000 -1.20000 AFIX 0 C46 1 0.896874 0.582168 0.850991 11.00000 0.05632 0.06528 = 0.05950 0.00019 -0.00391 -0.00505 AFIX 43 H46 2 0.919862 0.552777 0.886227 11.00000 -1.20000 AFIX 0 C68 1 1.477323 0.714080 0.649754 11.00000 0.11233 0.05996 = 0.09107 0.01778 -0.02883 -0.03081 AFIX 43 H68 2 1.543238 0.743595 0.650120 11.00000 -1.20000 AFIX 0 C45 1 0.971174 0.632595 0.858519 11.00000 0.07611 0.07269 = 0.06889 -0.01030 -0.00108 -0.01150 AFIX 43 H45 2 1.044656 0.636349 0.898399 11.00000 -1.20000 AFIX 0 F26 3 1.036330 0.797481 0.737278 11.00000 0.16622 0.10222 = 0.17035 0.04538 -0.05081 -0.05256 C50 1 0.939036 0.675585 0.809687 11.00000 0.07474 0.06262 = 0.07980 -0.01400 0.01560 -0.00956 AFIX 43 H50 2 0.989502 0.709083 0.815675 11.00000 -1.20000 AFIX 0 C43 1 0.764449 0.342507 0.565730 11.00000 0.08100 0.06502 = 0.06804 -0.00741 0.01035 0.00248 AFIX 43 H43 2 0.701482 0.347495 0.520822 11.00000 -1.20000 AFIX 0 C52 1 0.627654 0.516534 0.541703 11.00000 0.05978 0.07770 = 0.07460 0.01261 -0.00206 0.00217 AFIX 137 H52A 2 0.550289 0.525902 0.577729 11.00000 -1.50000 H52B 2 0.587938 0.497835 0.494185 11.00000 -1.50000 H52C 2 0.676412 0.550033 0.525259 11.00000 -1.50000 AFIX 0 C84 1 -0.438111 0.134659 1.071054 11.00000 0.08332 0.09231 = 0.10372 -0.01000 0.01243 0.01344 AFIX 43 H84 2 -0.503227 0.155240 1.101667 11.00000 -1.20000 AFIX 0 C96 1 0.021750 0.152621 0.796511 11.00000 0.07778 0.07345 = 0.07610 0.01946 -0.01761 -0.01513 AFIX 43 H96 2 -0.031364 0.149259 0.747518 11.00000 -1.20000 AFIX 0 C83 1 -0.379609 0.084141 1.100304 11.00000 0.05617 0.08253 = 0.07725 -0.01877 0.01549 -0.00738 AFIX 43 H83 2 -0.401296 0.071422 1.152386 11.00000 -1.20000 AFIX 0 C10 1 1.091417 0.845094 0.710126 11.00000 0.06153 0.06409 = 0.08705 -0.00328 -0.01050 -0.01765 C6 1 1.499669 0.843611 0.931188 11.00000 0.07582 0.06357 = 0.07898 0.01348 -0.00766 0.00313 AFIX 43 H6 2 1.441961 0.849395 0.976403 11.00000 -1.20000 AFIX 0 C58 1 0.872842 0.668087 0.502552 11.00000 0.09931 0.07982 = 0.13060 0.01351 -0.01395 0.02759 C95 1 0.119049 0.196586 0.807583 11.00000 0.09196 0.07722 = 0.10764 0.02816 -0.02068 -0.01886 AFIX 43 H95 2 0.131976 0.222365 0.765808 11.00000 -1.20000 AFIX 0 C4 1 1.676808 0.789190 0.862728 11.00000 0.06681 0.08760 = 0.14013 -0.02729 -0.02366 0.01235 AFIX 43 H4 2 1.738585 0.758447 0.860800 11.00000 -1.20000 AFIX 0 C48 1 0.756518 0.620270 0.741343 11.00000 0.08564 0.05580 = 0.07499 -0.00335 -0.02272 0.00427 AFIX 43 H48 2 0.683589 0.616583 0.701130 11.00000 -1.20000 AFIX 0 C69 1 1.465462 0.679102 0.584827 11.00000 0.07875 0.08569 = 0.10382 0.02236 0.00681 -0.02063 AFIX 43 H69 2 1.525447 0.684060 0.540360 11.00000 -1.20000 AFIX 0 C99 1 0.113688 -0.089880 1.073090 11.00000 0.07631 0.08000 = 0.06643 -0.00714 0.00072 0.00316 AFIX 43 H99 2 0.142796 -0.059809 1.105617 11.00000 -1.20000 AFIX 0 C93 1 0.182365 0.163779 0.940131 11.00000 0.07509 0.07303 = 0.07681 0.00075 -0.00807 -0.01730 AFIX 43 H93 2 0.237313 0.167450 0.988448 11.00000 -1.20000 AFIX 0 C30 1 0.328777 0.363860 0.849756 11.00000 0.06849 0.07848 = 0.09266 0.02910 0.02482 0.00995 AFIX 43 H30 2 0.260947 0.344606 0.880327 11.00000 -1.20000 AFIX 0 C19 1 1.529454 1.173351 0.749865 11.00000 0.13239 0.06153 = 0.08840 0.00573 0.01403 -0.00676 AFIX 43 H19 2 1.500666 1.201941 0.784439 11.00000 -1.20000 AFIX 0 C39 1 0.855469 0.372696 0.695055 11.00000 0.07415 0.07317 = 0.06999 0.00642 -0.00456 0.01738 AFIX 43 H39 2 0.857592 0.398640 0.737434 11.00000 -1.20000 AFIX 0 C29 1 0.395225 0.412786 0.878302 11.00000 0.08295 0.07880 = 0.06349 0.00669 0.02395 0.00500 AFIX 43 H29 2 0.375366 0.425278 0.930756 11.00000 -1.20000 AFIX 0 C17 1 1.676618 1.140518 0.644717 11.00000 0.08220 0.07786 = 0.09100 0.01948 0.00481 -0.01957 AFIX 43 H17 2 1.746087 1.147384 0.605474 11.00000 -1.20000 AFIX 0 C94 1 0.195233 0.201864 0.879473 11.00000 0.07540 0.06688 = 0.09750 -0.00057 -0.00854 -0.01490 AFIX 43 H94 2 0.257403 0.232192 0.887206 11.00000 -1.20000 AFIX 0 C21 1 1.357050 1.014819 0.950560 11.00000 0.05309 0.07891 = 0.08520 -0.01997 0.01431 -0.00138 AFIX 137 H21A 2 1.408133 1.043415 0.980850 11.00000 -1.50000 H21B 2 1.299761 0.993067 0.987197 11.00000 -1.50000 H21C 2 1.294207 1.031760 0.909771 11.00000 -1.50000 AFIX 0 F79 3 0.826149 0.717046 0.528669 11.00000 0.09931 0.07982 = 0.13060 0.01351 -0.01395 0.02759 C3 1 1.672438 0.824208 0.800232 11.00000 0.07161 0.07921 = 0.11802 -0.02922 0.00157 0.01326 AFIX 43 H3 2 1.730983 0.817949 0.755497 11.00000 -1.20000 AFIX 0 C100 1 0.182084 -0.141418 1.083714 11.00000 0.08236 0.08998 = 0.08715 0.00847 -0.00507 0.02084 AFIX 43 H100 2 0.258569 -0.145448 1.121703 11.00000 -1.20000 AFIX 0 C41 1 0.944575 0.287638 0.634998 11.00000 0.09026 0.07399 = 0.09796 0.01693 0.02181 0.02209 AFIX 43 H41 2 1.003901 0.256151 0.637245 11.00000 -1.20000 AFIX 0 F53 3 0.306194 0.298686 0.744480 11.00000 0.13112 0.10148 = 0.13963 0.00850 0.02768 -0.03311 F105 3 -0.444619 0.202570 0.965098 11.00000 0.08728 0.09416 = 0.10770 -0.00734 0.00977 0.01357 C42 1 0.856269 0.296829 0.568170 11.00000 0.09404 0.07662 = 0.08650 -0.00435 0.00788 0.02025 AFIX 43 H42 2 0.857788 0.272293 0.524069 11.00000 -1.20000 AFIX 0 C67 1 1.385899 0.704367 0.717512 11.00000 0.11232 0.08497 = 0.08085 -0.00575 -0.01007 -0.01858 AFIX 43 H67 2 1.392184 0.727988 0.762653 11.00000 -1.20000 AFIX 0 C75 1 1.391421 0.325220 0.477036 11.00000 0.11049 0.06250 = 0.08737 -0.01996 -0.01790 0.02300 AFIX 43 H75 2 1.432135 0.289799 0.472771 11.00000 -1.20000 AFIX 0 C103 1 -0.034937 -0.128798 0.968716 11.00000 0.10372 0.06826 = 0.08622 -0.00002 -0.02786 -0.00187 AFIX 43 H103 2 -0.108403 -0.124705 0.928900 11.00000 -1.20000 AFIX 0 C57 1 0.824790 0.649042 0.427038 11.00000 0.09346 0.07808 = 0.12630 0.01780 -0.01738 0.02704 AFIX 43 H57 2 0.762252 0.670678 0.394490 11.00000 -1.20000 AFIX 0 C5 1 1.593895 0.796563 0.929942 11.00000 0.08829 0.07163 = 0.11788 0.01298 -0.02161 0.00903 AFIX 43 H5 2 1.598853 0.771611 0.973549 11.00000 -1.20000 AFIX 0 C40 1 0.946306 0.324717 0.699083 11.00000 0.07837 0.07958 = 0.10397 -0.00042 -0.01375 0.02308 AFIX 43 H40 2 1.006532 0.318459 0.744806 11.00000 -1.20000 AFIX 0 C101 1 0.136636 -0.185076 1.038712 11.00000 0.09693 0.07775 = 0.09669 0.00776 -0.00407 0.02520 AFIX 43 H101 2 0.177960 -0.220062 1.047864 11.00000 -1.20000 AFIX 0 C102 1 0.028666 -0.178668 0.978641 11.00000 0.13330 0.06691 = 0.10597 -0.02204 -0.00765 0.01783 AFIX 43 H102 2 0.000780 -0.208664 0.945644 11.00000 -1.20000 AFIX 0 HKLF 4 REM fengchuanqi-cy-36-2_a.res in P2(1) REM wR2 = 0.2295, GooF = S = 1.007, Restrained GooF = 1.533 for all data REM R1 = 0.0735 for 8470 Fo > 4sig(Fo) and 0.0958 for all 10531 data REM 929 parameters refined using 65 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.510, deepest hole -0.552, 1-sigma level 0.117 Q1 1 0.8083 0.7130 0.6955 11.00000 0.05 0.51 Q2 1 0.0254 -0.2182 0.9257 11.00000 0.05 0.49 Q3 1 1.2847 0.2944 0.5899 11.00000 0.05 0.47 Q4 1 1.5196 1.2129 0.8095 11.00000 0.05 0.45 Q5 1 1.5359 0.3557 0.3779 11.00000 0.05 0.44 Q6 1 -0.2587 0.2212 0.8542 11.00000 0.05 0.40 Q7 1 0.9556 0.7130 0.6173 11.00000 0.05 0.40 Q8 1 1.5278 0.8780 0.8529 11.00000 0.05 0.38 Q9 1 0.2504 0.3647 0.9191 11.00000 0.05 0.37 Q10 1 1.7447 0.7920 0.8311 11.00000 0.05 0.37 Q11 1 1.1042 0.8769 0.8301 11.00000 0.05 0.36 Q12 1 0.5185 0.3170 0.6542 11.00000 0.05 0.36 Q13 1 -0.0355 0.1793 0.8614 11.00000 0.05 0.35 Q14 1 1.6111 0.6809 0.6116 11.00000 0.05 0.35 REM The information below was added by Olex2. REM REM R1 = 0.0735 for 8470 Fo > 4sig(Fo) and 0.0958 for all 23779 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.32, deepest hole -1.55 REM Mean Shift 0, Max Shift -0.002. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0958 REM R1_gt = 0.0735 REM wR_ref = 0.2295 REM GOOF = 1.007 REM Shift_max = -0.002 REM Shift_mean = 0 REM Reflections_all = 23779 REM Reflections_gt = 8470 REM Parameters = n/a REM Hole = -0.55 REM Peak = 0.51 REM Flack = 0.21(16) ; _cod_data_source_file c9nj00030e2.cif _cod_data_source_block fengchuanqi-cy-36-2 _cod_database_code 7058163 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C O N H' _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. ; _reflns_odcompleteness_completeness 99.70 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _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. Rigid bond restraints F53, C31 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O89, N88 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C57, C58, C59 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C84, C85 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 F79, C58 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 F105, C85 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C80, C85 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C80, C81 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 3. Uiso/Uaniso restraints and constraints F53 \\sim C31: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 O89 \\sim N88: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 C57 \\sim C58 \\sim C59: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 C84 \\sim C85: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 F79 \\sim C58: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 F105 \\sim C85: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 C80 \\sim C85: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 C80 \\sim C81: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 Uanis(F79) = Uanis(C58) Uanis(F105) = Uanis(C85) 4.a Ternary CH refined with riding coordinates: C34(H34), C61(H61), C87(H87), C7(H7) 4.b Aromatic/amide H refined with riding coordinates: C32(H32), C13(H13), C82(H82), C73(H73), C9(H9), C55(H55), C70(H70), C92(H92), C28(H28), C59(H59), C16(H16), C66(H66), C74(H74), C12(H12), C11(H11), C20(H20), C18(H18), C49(H49), C56(H56), C76(H76), C80(H80), C77(H77), C2(H2), C46(H46), C68(H68), C45(H45), C50(H50), C43(H43), C84(H84), C96(H96), C83(H83), C6(H6), C95(H95), C4(H4), C48(H48), C69(H69), C99(H99), C93(H93), C30(H30), C19(H19), C39(H39), C29(H29), C17(H17), C94(H94), C3(H3), C100(H100), C41(H41), C42(H42), C67(H67), C75(H75), C103(H103), C57(H57), C5(H5), C40(H40), C101(H101), C102(H102) 4.c Idealised Me refined as rotating group: C78(H78A,H78B,H78C), C104(H10A,H10B,H10C), C52(H52A,H52B,H52C), C21(H21A,H21B, H21C) ; _shelx_fab_file ; -11 -9 -1 -0.0421 -0.0601 -11 -9 0 -0.0705 -0.0006 -11 -8 0 -0.0371 -0.0854 -11 -7 -3 -0.0008 0.0069 -11 -7 -2 0.0165 0.1025 -11 -7 0 0.0884 0.0487 -11 -6 -3 0.0253 -0.0141 -11 -6 -2 -0.0565 0.0312 -11 -6 -1 -0.0678 0.0732 -11 -6 0 -0.0362 0.0928 -11 -5 -4 -0.1163 0.1356 -11 -5 -3 -0.0723 -0.0251 -11 -5 -2 -0.0757 -0.1199 -11 -5 -1 -0.1031 -0.1201 -11 -5 0 -0.1163 -0.0784 -11 -4 -3 -0.1226 -0.0003 -11 -4 -2 0.0466 -0.0428 -11 -4 -1 0.1300 -0.0729 -11 -4 0 0.1228 -0.0775 -11 -3 -3 0.1440 0.0286 -11 -3 -2 0.1392 0.0982 -11 -3 -1 0.1550 0.0968 -11 -3 0 0.1478 0.0706 -11 -2 -4 0.3375 -0.0023 -11 -2 -3 0.2032 0.0030 -11 -2 -2 -0.0411 0.0291 -11 -2 -1 -0.1825 0.0452 -11 -2 0 -0.1930 0.0439 -11 -1 -3 -0.1884 -0.0136 -11 -1 -2 -0.1799 -0.0383 -11 -1 -1 -0.1902 -0.0361 -11 -1 0 -0.1693 -0.0267 -11 0 1 0.1729 -0.0008 -11 0 2 0.1338 -0.0014 -11 0 3 0.1705 -0.0012 -11 0 4 0.2809 0.0003 -11 0 5 0.3087 0.0013 -11 0 6 0.1346 0.0004 -11 1 1 0.1560 -0.0182 -11 1 2 0.1354 -0.0062 -11 1 3 0.0313 -0.0060 -11 1 5 -0.1933 0.0073 -11 1 6 -0.2134 0.0236 -11 2 1 -0.1518 -0.0122 -11 2 2 -0.1254 0.0533 -11 2 3 -0.1690 0.1011 -11 2 4 -0.2695 0.0716 -11 2 6 -0.1137 -0.0231 -11 3 1 -0.1395 0.0396 -11 3 2 -0.1119 0.0151 -11 3 3 -0.0141 0.0224 -11 3 4 0.1059 0.0268 -11 3 6 0.1720 -0.0622 -11 4 1 0.0980 0.0295 -11 4 2 0.1062 -0.0794 -11 4 3 0.1666 -0.1578 -11 4 4 0.2388 -0.1080 -11 4 5 0.2136 0.0027 -11 5 1 0.1118 -0.0303 -11 5 2 0.0728 -0.0117 -11 5 3 -0.0125 -0.0440 -11 5 4 -0.0882 -0.0560 -11 5 5 -0.1038 0.0153 -11 6 1 -0.0343 -0.0479 -11 6 2 -0.0893 0.0710 -11 6 3 -0.1671 0.1525 -11 6 4 -0.1960 0.0940 -10 -14 -3 -0.0776 0.0662 -10 -14 -2 -0.0341 0.0320 -10 -14 -1 0.0034 -0.0228 -10 -14 0 -0.0309 -0.0669 -10 -13 -4 -0.1316 -0.0601 -10 -13 -3 -0.2151 -0.0610 -10 -13 -2 -0.1425 -0.0492 -10 -13 -1 0.0486 -0.0580 -10 -13 0 0.1578 -0.0664 -10 -12 -3 0.1328 -0.0469 -10 -12 -2 0.0912 -0.0521 -10 -12 -1 0.0082 -0.0062 -10 -12 0 -0.0151 0.0653 -10 -11 -6 0.0058 -0.0645 -10 -11 -5 0.0496 -0.0085 -10 -11 -3 0.2058 0.0549 -10 -11 -2 0.1135 0.0526 -10 -11 -1 -0.0903 0.0352 -10 -11 0 -0.2031 0.0047 -10 -10 -6 0.1579 0.0025 -10 -10 -5 0.0807 -0.0679 -10 -10 -2 -0.1120 0.0740 -10 -10 -1 -0.0101 0.0468 -10 -10 0 0.0576 -0.0285 -10 -9 -7 0.0065 0.0577 -10 -9 -6 -0.0076 0.0562 -10 -9 -5 -0.0399 0.0078 -10 -9 -4 -0.1151 -0.0271 -10 -9 -3 -0.1599 -0.0389 -10 -9 -2 -0.0753 -0.0416 -10 -9 -1 0.1037 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11 3 1 0.1550 -0.0968 11 3 2 0.1392 -0.0982 11 3 3 0.1440 -0.0286 11 3 5 0.1902 0.1493 11 4 0 0.1228 0.0775 11 4 1 0.1300 0.0729 11 4 2 0.0466 0.0428 11 4 3 -0.1226 0.0003 11 5 0 -0.1163 0.0784 11 5 1 -0.1031 0.1201 11 5 2 -0.0757 0.1199 11 5 3 -0.0723 0.0251 11 6 0 -0.0362 -0.0928 11 6 1 -0.0678 -0.0732 11 6 2 -0.0565 -0.0312 0 0 0 0.0 0.0 ; _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 ; _oxdiff_exptl_absorpt_empirical_full_max 1.895 _oxdiff_exptl_absorpt_empirical_full_min 0.395 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 O1 O 1.5147(5) 1.0109(3) 0.8412(3) 0.0598(12) Uani 1 1 d . . O36 O 0.7873(6) 0.5109(3) 0.6562(3) 0.0611(13) Uani 1 1 d . . O63 O 1.2862(5) 0.4970(2) 0.6215(3) 0.0556(12) Uani 1 1 d . . O89 O 0.0107(5) -0.0177(3) 0.8780(3) 0.0575(10) Uani 1 1 d . U N3 N 1.4639(7) 0.9780(3) 0.9101(4) 0.0563(14) Uani 1 1 d . . N33 N 0.6191(6) 0.4522(3) 0.7022(4) 0.0523(13) Uani 1 1 d . . N62 N 1.2382(6) 0.5281(3) 0.6932(4) 0.0518(13) Uani 1 1 d . . N2 N 1.3491(6) 0.9517(3) 0.7885(4) 0.0537(14) Uani 1 1 d . . N60 N 1.1214(6) 0.5583(3) 0.5737(4) 0.0556(14) Uani 1 1 d . . N35 N 0.7334(6) 0.4791(3) 0.5849(4) 0.0540(13) Uani 1 1 d . . N97 N -0.0697(7) -0.0317(3) 1.0098(4) 0.0637(16) Uani 1 1 d . . N86 N -0.1540(6) 0.0421(3) 0.9241(4) 0.0521(13) Uani 1 1 d . . N71 N 1.1969(8) 0.4847(3) 0.4885(4) 0.0617(15) Uani 1 1 d . . N88 N -0.0321(6) 0.0169(3) 0.8073(4) 0.0566(11) Uani 1 1 d . U C34 C 0.6631(7) 0.4306(3) 0.6226(4) 0.0513(15) Uani 1 1 d . . H34 H 0.575773 0.420574 0.590021 0.062 Uiso 1 1 calc R . N44 N 0.7103(8) 0.5241(3) 0.7881(4) 0.0615(15) Uani 1 1 d . . N1 N 1.4357(7) 1.0260(3) 0.7062(4) 0.0609(15) Uani 1 1 d . . C90 C -0.0719(8) -0.0050(3) 0.9430(4) 0.0535(15) Uani 1 1 d . . C64 C 1.1991(7) 0.5108(3) 0.5555(4) 0.0515(14) Uani 1 1 d . . C91 C 0.0035(7) 0.1134(3) 0.8588(4) 0.0516(15) Uani 1 1 d . . C61 C 1.1729(8) 0.5782(3) 0.6540(5) 0.0554(16) Uani 1 1 d . . H61 H 1.088492 0.589860 0.685409 0.066 Uiso 1 1 calc R . C37 C 0.7031(7) 0.4985(3) 0.7197(4) 0.0509(14) Uani 1 1 d . . C72 C 1.2654(9) 0.4298(3) 0.4866(5) 0.0585(17) Uani 1 1 d . . C27 C 0.5248(7) 0.4240(3) 0.7536(4) 0.0488(14) Uani 1 1 d . . C65 C 1.2784(8) 0.6260(3) 0.6508(5) 0.0554(16) Uani 1 1 d . . C87 C -0.1021(7) 0.0651(3) 0.8464(4) 0.0507(15) Uani 1 1 d . . H87 H -0.185713 0.077416 0.812492 0.061 Uiso 1 1 calc R . C7 C 1.3923(8) 0.9291(3) 0.8711(4) 0.0539(16) Uani 1 1 d . . H7 H 1.305069 0.918964 0.901126 0.065 Uiso 1 1 calc R . C81 C -0.2470(10) 0.0726(4) 0.9755(6) 0.0727(16) Uani 1 1 d . U C1 C 1.4918(7) 0.8806(3) 0.8674(4) 0.0535(15) Uani 1 1 d . . C32 C 0.4623(8) 0.3748(4) 0.7261(5) 0.0626(18) Uani 1 1 d . . H32 H 0.483034 0.360973 0.674525 0.075 Uiso 1 1 calc R . C13 C 1.2098(8) 0.9444(4) 0.6576(5) 0.0595(17) Uani 1 1 d . . H13 H 1.248696 0.977912 0.639219 0.071 Uiso 1 1 calc R . C8 C 1.2506(8) 0.9233(3) 0.7357(5) 0.0553(16) Uani 1 1 d . . C15 C 1.5071(9) 1.0784(4) 0.7047(5) 0.0599(17) Uani 1 1 d . . C78 C 1.1349(9) 0.4922(4) 0.7336(6) 0.066(2) Uani 1 1 d . . H78A H 1.061366 0.480184 0.694629 0.099 Uiso 1 1 calc GR . H78B H 1.090063 0.512520 0.776904 0.099 Uiso 1 1 calc GR . H78C H 1.184991 0.460255 0.755864 0.099 Uiso 1 1 calc GR . C98 C 0.0055(9) -0.0829(4) 1.0161(5) 0.0604(18) Uani 1 1 d . . C54 C 1.0234(7) 0.5865(3) 0.5225(5) 0.0554(16) Uani 1 1 d . . C82 C -0.2888(8) 0.0533(4) 1.0506(5) 0.0614(18) Uani 1 1 d . . H82 H -0.255425 0.018585 1.068619 0.074 Uiso 1 1 calc R . C38 C 0.7644(8) 0.3804(4) 0.6280(5) 0.0578(16) Uani 1 1 d . . C73 C 1.3704(10) 0.4194(4) 0.4296(5) 0.0642(19) Uani 1 1 d . . H73 H 1.396746 0.447291 0.393139 0.077 Uiso 1 1 calc R . C9 C 1.1912(9) 0.8724(4) 0.7630(5) 0.0623(18) Uani 1 1 d . . H9 H 1.217127 0.857503 0.813850 0.075 Uiso 1 1 calc R . C55 C 0.9703(8) 0.5667(4) 0.4495(5) 0.0610(18) Uani 1 1 d . . H55 H 1.001325 0.531763 0.432078 0.073 Uiso 1 1 calc R . C14 C 1.4295(8) 0.9986(3) 0.7726(4) 0.0556(16) Uani 1 1 d . . C70 C 1.3631(9) 0.6353(4) 0.5840(5) 0.0656(19) Uani 1 1 d . . H70 H 1.352883 0.612556 0.538114 0.079 Uiso 1 1 calc R . C85 C -0.3952(14) 0.1527(6) 0.9949(9) 0.0963(12) Uani 1 1 d . U C92 C 0.0854(10) 0.1186(4) 0.9297(5) 0.0638(19) Uani 1 1 d . . H92 H 0.076981 0.092186 0.971092 0.077 Uiso 1 1 calc R . C28 C 0.4895(9) 0.4433(4) 0.8312(5) 0.0642(19) Uani 1 1 d . . H28 H 0.529330 0.476463 0.851063 0.077 Uiso 1 1 calc R . C59 C 0.9734(14) 0.6381(5) 0.5481(9) 0.0961(17) Uani 1 1 d . U H59 H 1.008810 0.652710 0.597464 0.115 Uiso 1 1 calc R . C16 C 1.6171(11) 1.0868(4) 0.6488(6) 0.071(2) Uani 1 1 d . . H16 H 1.649495 1.058006 0.615611 0.085 Uiso 1 1 calc R . C66 C 1.2910(12) 0.6618(4) 0.7174(6) 0.075(2) Uani 1 1 d . . H66 H 1.232829 0.656166 0.762463 0.090 Uiso 1 1 calc R . C74 C 1.4361(13) 0.3680(5) 0.4267(6) 0.080(3) Uani 1 1 d . . H74 H 1.511308 0.361902 0.390615 0.096 Uiso 1 1 calc R . C47 C 0.7895(9) 0.5757(4) 0.7915(5) 0.0615(18) Uani 1 1 d . . C12 C 1.1121(10) 0.9149(4) 0.6089(5) 0.068(2) Uani 1 1 d . . H12 H 1.085092 0.928834 0.557536 0.081 Uiso 1 1 calc R . C104 C -0.1358(9) -0.0175(5) 0.7595(6) 0.073(2) Uani 1 1 d . . H10A H -0.085790 -0.048988 0.737192 0.109 Uiso 1 1 calc GR . H10B H -0.177914 0.004420 0.715715 0.109 Uiso 1 1 calc GR . H10C H -0.211526 -0.030309 0.794366 0.109 Uiso 1 1 calc GR . C11 C 1.0520(10) 0.8639(4) 0.6357(6) 0.070(2) Uani 1 1 d . . H11 H 0.986853 0.843882 0.602464 0.084 Uiso 1 1 calc R . C20 C 1.4638(11) 1.1222(4) 0.7539(6) 0.071(2) Uani 1 1 d . . H20 H 1.388718 1.116720 0.790202 0.086 Uiso 1 1 calc R . C18 C 1.6394(14) 1.1828(5) 0.6942(7) 0.087(3) Uani 1 1 d . . H18 H 1.685572 1.217309 0.691302 0.104 Uiso 1 1 calc R . C31 C 0.3681(15) 0.3464(6) 0.7764(9) 0.100(3) Uani 1 1 d . U C49 C 0.8295(13) 0.6702(4) 0.7496(6) 0.076(2) Uani 1 1 d . . H49 H 0.805993 0.700112 0.715330 0.091 Uiso 1 1 calc R . C56 C 0.8717(11) 0.5963(5) 0.3997(6) 0.078(3) Uani 1 1 d . . H56 H 0.837936 0.581646 0.350011 0.093 Uiso 1 1 calc R . C76 C 1.2852(13) 0.3357(4) 0.5340(6) 0.078(2) Uani 1 1 d . . H76 H 1.257124 0.307664 0.569697 0.094 Uiso 1 1 calc R . C80 C -0.2984(11) 0.1230(5) 0.9477(7) 0.0823(14) Uani 1 1 d . U H80 H -0.268695 0.137197 0.897857 0.099 Uiso 1 1 calc R . C77 C 1.2201(10) 0.3886(4) 0.5375(6) 0.068(2) Uani 1 1 d . . H77 H 1.146671 0.395559 0.574368 0.082 Uiso 1 1 calc R . C2 C 1.5823(10) 0.8696(4) 0.8011(6) 0.070(2) Uani 1 1 d . . H2 H 1.580581 0.893807 0.756597 0.084 Uiso 1 1 calc R . C46 C 0.8969(9) 0.5822(4) 0.8510(5) 0.0605(17) Uani 1 1 d . . H46 H 0.919862 0.552777 0.886227 0.073 Uiso 1 1 calc R . C68 C 1.4773(14) 0.7141(4) 0.6498(7) 0.088(3) Uani 1 1 d . . H68 H 1.543238 0.743595 0.650120 0.106 Uiso 1 1 calc R . C45 C 0.9712(11) 0.6326(4) 0.8585(6) 0.073(2) Uani 1 1 d . . H45 H 1.044656 0.636349 0.898399 0.087 Uiso 1 1 calc R . F26 F 1.0363(12) 0.7975(4) 0.7373(7) 0.147(4) Uani 1 1 d . . C50 C 0.9390(11) 0.6756(4) 0.8097(6) 0.072(2) Uani 1 1 d . . H50 H 0.989502 0.709083 0.815675 0.087 Uiso 1 1 calc R . C43 C 0.7644(11) 0.3425(4) 0.5657(6) 0.071(2) Uani 1 1 d . . H43 H 0.701482 0.347495 0.520822 0.085 Uiso 1 1 calc R . C52 C 0.6277(10) 0.5165(4) 0.5417(6) 0.071(2) Uani 1 1 d . . H52A H 0.550289 0.525902 0.577729 0.106 Uiso 1 1 calc GR . H52B H 0.587938 0.497835 0.494185 0.106 Uiso 1 1 calc GR . H52C H 0.676412 0.550033 0.525259 0.106 Uiso 1 1 calc GR . C84 C -0.4381(13) 0.1347(6) 1.0711(8) 0.0929(16) Uani 1 1 d . U H84 H -0.503227 0.155240 1.101667 0.112 Uiso 1 1 calc R . C96 C 0.0217(11) 0.1526(4) 0.7965(6) 0.076(2) Uani 1 1 d . . H96 H -0.031364 0.149259 0.747518 0.091 Uiso 1 1 calc R . C83 C -0.3796(9) 0.0841(5) 1.1003(6) 0.072(2) Uani 1 1 d . . H83 H -0.401296 0.071422 1.152386 0.086 Uiso 1 1 calc R . C10 C 1.0914(10) 0.8451(4) 0.7101(6) 0.071(2) Uani 1 1 d . . C6 C 1.4997(11) 0.8436(4) 0.9312(6) 0.073(2) Uani 1 1 d . . H6 H 1.441961 0.849395 0.976403 0.088 Uiso 1 1 calc R . C58 C 0.8728(16) 0.6681(6) 0.5026(10) 0.1035(14) Uani 1 1 d . U C95 C 0.1190(13) 0.1966(5) 0.8076(8) 0.093(3) Uani 1 1 d . . H95 H 0.131976 0.222365 0.765808 0.111 Uiso 1 1 calc R . C4 C 1.6768(12) 0.7892(6) 0.8627(10) 0.099(4) Uani 1 1 d . . H4 H 1.738585 0.758447 0.860800 0.118 Uiso 1 1 calc R . C48 C 0.7565(11) 0.6203(4) 0.7413(6) 0.073(2) Uani 1 1 d . . H48 H 0.683589 0.616583 0.701130 0.087 Uiso 1 1 calc R . C69 C 1.4655(13) 0.6791(5) 0.5848(8) 0.089(3) Uani 1 1 d . . H69 H 1.525447 0.684060 0.540360 0.107 Uiso 1 1 calc R . C99 C 0.1137(11) -0.0899(5) 1.0731(6) 0.074(2) Uani 1 1 d . . H99 H 0.142796 -0.059809 1.105617 0.089 Uiso 1 1 calc R . C93 C 0.1824(11) 0.1638(4) 0.9401(6) 0.075(2) Uani 1 1 d . . H93 H 0.237313 0.167450 0.988448 0.090 Uiso 1 1 calc R . C30 C 0.3288(11) 0.3639(5) 0.8498(7) 0.079(3) Uani 1 1 d . . H30 H 0.260947 0.344606 0.880327 0.095 Uiso 1 1 calc R . C19 C 1.5295(17) 1.1734(5) 0.7499(8) 0.094(3) Uani 1 1 d . . H19 H 1.500666 1.201941 0.784439 0.113 Uiso 1 1 calc R . C39 C 0.8555(10) 0.3727(4) 0.6951(6) 0.073(2) Uani 1 1 d . . H39 H 0.857592 0.398640 0.737434 0.087 Uiso 1 1 calc R . C29 C 0.3952(11) 0.4128(5) 0.8783(6) 0.075(2) Uani 1 1 d . . H29 H 0.375366 0.425278 0.930756 0.090 Uiso 1 1 calc R . C17 C 1.6766(12) 1.1405(5) 0.6447(7) 0.084(3) Uani 1 1 d . . H17 H 1.746087 1.147384 0.605474 0.100 Uiso 1 1 calc R . C94 C 0.1952(11) 0.2019(5) 0.8795(7) 0.080(3) Uani 1 1 d . . H94 H 0.257403 0.232192 0.887206 0.096 Uiso 1 1 calc R . C21 C 1.3570(9) 1.0148(4) 0.9506(6) 0.072(2) Uani 1 1 d . . H21A H 1.408133 1.043415 0.980850 0.108 Uiso 1 1 calc GR . H21B H 1.299761 0.993067 0.987197 0.108 Uiso 1 1 calc GR . H21C H 1.294207 1.031760 0.909771 0.108 Uiso 1 1 calc GR . F79 F 0.8261(8) 0.7170(3) 0.5287(5) 0.1035(14) Uani 1 1 d . U C3 C 1.6724(12) 0.8242(5) 0.8002(9) 0.090(3) Uani 1 1 d . . H3 H 1.730983 0.817949 0.755497 0.108 Uiso 1 1 calc R . C100 C 0.1821(13) -0.1414(5) 1.0837(7) 0.087(3) Uani 1 1 d . . H100 H 0.258569 -0.145448 1.121703 0.104 Uiso 1 1 calc R . C41 C 0.9446(13) 0.2876(5) 0.6350(7) 0.087(3) Uani 1 1 d . . H41 H 1.003901 0.256151 0.637245 0.104 Uiso 1 1 calc R . F53 F 0.3062(10) 0.2987(4) 0.7445(6) 0.124(2) Uani 1 1 d . U F105 F -0.4446(7) 0.2026(3) 0.9651(4) 0.0963(12) Uani 1 1 d . U C42 C 0.8563(13) 0.2968(5) 0.5682(7) 0.086(3) Uani 1 1 d . . H42 H 0.857788 0.272293 0.524069 0.103 Uiso 1 1 calc R . C67 C 1.3859(15) 0.7044(6) 0.7175(7) 0.093(3) Uani 1 1 d . . H67 H 1.392184 0.727988 0.762653 0.112 Uiso 1 1 calc R . C75 C 1.3914(14) 0.3252(5) 0.4770(7) 0.087(3) Uani 1 1 d . . H75 H 1.432135 0.289799 0.472771 0.105 Uiso 1 1 calc R . C103 C -0.0349(14) -0.1288(5) 0.9687(7) 0.087(3) Uani 1 1 d . . H103 H -0.108403 -0.124705 0.928900 0.104 Uiso 1 1 calc R . C57 C 0.8248(15) 0.6490(5) 0.4270(9) 0.0996(18) Uani 1 1 d . U H57 H 0.762252 0.670678 0.394490 0.120 Uiso 1 1 calc R . C5 C 1.5939(13) 0.7966(5) 0.9299(9) 0.093(3) Uani 1 1 d . . H5 H 1.598853 0.771611 0.973549 0.112 Uiso 1 1 calc R . C40 C 0.9463(13) 0.3247(5) 0.6991(8) 0.088(3) Uani 1 1 d . . H40 H 1.006532 0.318459 0.744806 0.105 Uiso 1 1 calc R . C101 C 0.1366(14) -0.1851(5) 1.0387(8) 0.091(3) Uani 1 1 d . . H101 H 0.177960 -0.220062 1.047864 0.109 Uiso 1 1 calc R . C102 C 0.0287(17) -0.1787(5) 0.9786(9) 0.102(4) Uani 1 1 d . . H102 H 0.000780 -0.208664 0.945644 0.123 Uiso 1 1 calc R . 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 O1 0.044(2) 0.070(3) 0.065(3) 0.002(3) -0.007(2) -0.006(2) O36 0.052(2) 0.065(3) 0.066(3) -0.005(3) 0.001(2) -0.008(2) O63 0.049(2) 0.059(3) 0.059(3) -0.005(2) 0.002(2) 0.008(2) O89 0.0456(19) 0.067(3) 0.060(2) -0.005(2) -0.0002(17) 0.0038(19) N3 0.049(3) 0.062(4) 0.058(3) -0.002(3) -0.004(2) 0.000(3) N33 0.044(3) 0.054(3) 0.059(3) -0.006(3) 0.012(2) -0.005(2) N62 0.051(3) 0.054(3) 0.051(3) 0.002(2) 0.003(2) 0.006(2) N2 0.045(3) 0.061(4) 0.054(3) 0.006(3) -0.015(2) -0.002(2) N60 0.049(3) 0.057(3) 0.061(3) -0.007(3) -0.006(2) 0.008(3) N35 0.048(3) 0.060(4) 0.055(3) 0.000(3) 0.002(2) -0.003(3) N97 0.060(3) 0.065(4) 0.067(4) 0.007(3) 0.007(3) 0.006(3) N86 0.043(3) 0.056(3) 0.058(3) 0.000(3) 0.006(2) 0.005(2) N71 0.064(3) 0.054(3) 0.067(4) -0.004(3) -0.004(3) 0.009(3) N88 0.047(2) 0.066(3) 0.056(2) -0.003(2) -0.0008(19) 0.003(2) C34 0.046(3) 0.058(4) 0.050(3) -0.004(3) 0.003(3) 0.001(3) N44 0.063(3) 0.054(4) 0.067(4) -0.006(3) -0.001(3) -0.007(3) N1 0.056(3) 0.062(4) 0.064(3) 0.005(3) -0.006(3) -0.007(3) C90 0.048(3) 0.059(4) 0.053(3) -0.001(3) 0.004(3) -0.003(3) C64 0.044(3) 0.049(4) 0.062(4) 0.002(3) -0.001(3) 0.007(3) C91 0.045(3) 0.058(4) 0.052(3) 0.006(3) 0.000(3) 0.004(3) C61 0.053(3) 0.055(4) 0.058(4) 0.005(3) 0.002(3) 0.005(3) C37 0.044(3) 0.053(4) 0.056(3) 0.002(3) -0.001(3) -0.005(3) C72 0.064(4) 0.055(4) 0.056(4) -0.006(3) -0.009(3) 0.004(3) C27 0.037(3) 0.060(4) 0.049(3) 0.010(3) 0.007(2) 0.006(3) C65 0.052(3) 0.052(4) 0.062(4) 0.006(3) 0.001(3) 0.004(3) C87 0.037(3) 0.060(4) 0.054(3) 0.001(3) -0.001(2) 0.000(3) C7 0.049(3) 0.062(4) 0.051(3) 0.003(3) -0.003(3) -0.001(3) C81 0.057(3) 0.076(3) 0.086(3) -0.009(3) 0.011(3) 0.006(3) C1 0.046(3) 0.060(4) 0.053(3) 0.001(3) -0.007(3) -0.004(3) C32 0.050(3) 0.069(5) 0.069(4) -0.001(4) 0.013(3) -0.012(3) C13 0.046(3) 0.071(5) 0.061(4) 0.002(3) -0.007(3) -0.004(3) C8 0.046(3) 0.060(4) 0.060(4) 0.004(3) -0.003(3) 0.000(3) C15 0.057(4) 0.059(4) 0.064(4) 0.006(3) -0.002(3) -0.003(3) C78 0.053(4) 0.072(5) 0.072(5) 0.016(4) 0.011(3) 0.004(4) C98 0.059(4) 0.056(4) 0.067(4) 0.003(3) 0.010(3) 0.007(3) C54 0.043(3) 0.061(4) 0.063(4) 0.011(3) 0.004(3) 0.002(3) C82 0.054(4) 0.074(5) 0.056(4) -0.008(4) 0.002(3) -0.004(3) C38 0.048(3) 0.060(4) 0.066(4) 0.006(3) 0.007(3) -0.001(3) C73 0.076(5) 0.066(5) 0.050(4) -0.009(3) -0.006(3) 0.007(4) C9 0.059(4) 0.066(5) 0.061(4) 0.003(4) -0.012(3) -0.005(4) C55 0.051(3) 0.067(5) 0.064(4) 0.009(4) -0.012(3) -0.008(3) C14 0.051(3) 0.060(4) 0.055(4) 0.003(3) -0.006(3) -0.005(3) C70 0.064(4) 0.066(5) 0.068(4) -0.002(4) 0.007(4) -0.006(4) C85 0.087(2) 0.094(3) 0.108(3) -0.007(2) 0.010(2) 0.014(2) C92 0.066(4) 0.070(5) 0.055(4) -0.002(4) -0.008(3) -0.009(4) C28 0.060(4) 0.071(5) 0.062(4) 0.005(4) 0.010(3) 0.006(4) C59 0.090(3) 0.073(3) 0.124(4) 0.013(3) -0.015(3) 0.030(3) C16 0.081(5) 0.063(5) 0.069(5) 0.001(4) 0.009(4) -0.005(4) C66 0.090(6) 0.065(5) 0.071(5) -0.009(4) -0.001(4) -0.007(5) C74 0.097(7) 0.078(6) 0.066(5) -0.012(5) 0.003(5) 0.020(5) C47 0.065(4) 0.057(4) 0.063(4) -0.008(3) 0.005(3) -0.008(3) C12 0.066(5) 0.075(5) 0.061(4) -0.004(4) -0.011(4) 0.001(4) C104 0.055(4) 0.088(6) 0.075(5) -0.021(5) -0.014(4) 0.000(4) C11 0.060(4) 0.071(5) 0.079(5) -0.020(4) -0.024(4) -0.004(4) C20 0.073(5) 0.058(5) 0.084(5) 0.003(4) 0.014(4) 0.000(4) C18 0.101(7) 0.077(7) 0.083(6) 0.000(5) 0.003(6) -0.025(6) C31 0.109(6) 0.078(5) 0.117(6) 0.016(5) 0.040(5) -0.030(5) C49 0.091(6) 0.064(5) 0.073(5) 0.001(4) 0.004(5) 0.003(5) C56 0.077(5) 0.085(7) 0.070(5) 0.011(5) -0.019(4) 0.000(5) C76 0.103(7) 0.051(5) 0.080(5) 0.005(4) -0.004(5) -0.009(5) C80 0.070(3) 0.083(3) 0.095(3) -0.007(3) 0.011(2) 0.009(2) C77 0.070(5) 0.065(5) 0.070(5) -0.006(4) 0.009(4) -0.003(4) C2 0.061(4) 0.077(6) 0.072(5) -0.011(4) 0.003(4) -0.003(4) C46 0.056(4) 0.065(5) 0.059(4) 0.000(3) -0.004(3) -0.005(3) C68 0.112(8) 0.060(5) 0.091(6) 0.018(5) -0.029(6) -0.031(5) C45 0.076(5) 0.073(6) 0.069(5) -0.010(4) -0.001(4) -0.012(4) F26 0.166(8) 0.102(6) 0.170(8) 0.045(6) -0.051(7) -0.053(6) C50 0.075(5) 0.063(5) 0.080(5) -0.014(4) 0.016(4) -0.010(4) C43 0.081(5) 0.065(5) 0.068(5) -0.007(4) 0.010(4) 0.002(4) C52 0.060(4) 0.078(6) 0.075(5) 0.013(4) -0.002(4) 0.002(4) C84 0.083(3) 0.092(3) 0.104(3) -0.010(3) 0.012(3) 0.013(3) C96 0.078(5) 0.073(6) 0.076(5) 0.019(5) -0.018(4) -0.015(5) C83 0.056(4) 0.083(6) 0.077(5) -0.019(5) 0.015(4) -0.007(4) C10 0.062(4) 0.064(5) 0.087(6) -0.003(4) -0.011(4) -0.018(4) C6 0.076(5) 0.064(5) 0.079(5) 0.013(4) -0.008(4) 0.003(4) C58 0.099(3) 0.080(3) 0.131(3) 0.014(2) -0.014(3) 0.028(2) C95 0.092(7) 0.077(7) 0.108(8) 0.028(6) -0.021(6) -0.019(6) C4 0.067(5) 0.088(8) 0.140(11) -0.027(8) -0.024(7) 0.012(5) C48 0.086(6) 0.056(5) 0.075(5) -0.003(4) -0.023(4) 0.004(4) C69 0.079(6) 0.086(7) 0.104(7) 0.022(6) 0.007(5) -0.021(5) C99 0.076(5) 0.080(6) 0.066(5) -0.007(4) 0.001(4) 0.003(5) C93 0.075(5) 0.073(6) 0.077(5) 0.001(5) -0.008(4) -0.017(5) C30 0.068(5) 0.078(6) 0.093(6) 0.029(5) 0.025(5) 0.010(4) C19 0.132(10) 0.062(6) 0.088(6) 0.006(5) 0.014(7) -0.007(6) C39 0.074(5) 0.073(6) 0.070(5) 0.006(4) -0.005(4) 0.017(4) C29 0.083(6) 0.079(6) 0.063(5) 0.007(4) 0.024(4) 0.005(5) C17 0.082(6) 0.078(6) 0.091(6) 0.019(5) 0.005(5) -0.020(5) C94 0.075(5) 0.067(5) 0.097(7) -0.001(5) -0.009(5) -0.015(5) C21 0.053(4) 0.079(6) 0.085(5) -0.020(5) 0.014(4) -0.001(4) F79 0.099(3) 0.080(3) 0.131(3) 0.014(2) -0.014(3) 0.028(2) C3 0.072(6) 0.079(7) 0.118(9) -0.029(7) 0.002(6) 0.013(5) C100 0.082(6) 0.090(8) 0.087(6) 0.008(6) -0.005(5) 0.021(6) C41 0.090(6) 0.074(6) 0.098(7) 0.017(5) 0.022(6) 0.022(5) F53 0.131(5) 0.101(5) 0.140(5) 0.008(4) 0.028(5) -0.033(4) F105 0.087(2) 0.094(3) 0.108(3) -0.007(2) 0.010(2) 0.014(2) C42 0.094(7) 0.077(6) 0.086(6) -0.004(5) 0.008(5) 0.020(5) C67 0.112(8) 0.085(7) 0.081(6) -0.006(6) -0.010(6) -0.019(7) C75 0.110(8) 0.063(6) 0.087(6) -0.020(5) -0.018(6) 0.023(5) C103 0.104(8) 0.068(6) 0.086(6) 0.000(5) -0.028(6) -0.002(5) C57 0.093(3) 0.078(3) 0.126(4) 0.018(3) -0.017(3) 0.027(3) C5 0.088(7) 0.072(6) 0.118(9) 0.013(6) -0.022(7) 0.009(6) C40 0.078(6) 0.080(7) 0.104(7) 0.000(6) -0.014(5) 0.023(5) C101 0.097(7) 0.078(7) 0.097(7) 0.008(6) -0.004(6) 0.025(6) C102 0.133(11) 0.067(6) 0.106(8) -0.022(6) -0.008(8) 0.018(7) 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_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C14 O1 N3 109.0(5) C37 O36 N35 108.0(5) C64 O63 N62 109.0(5) C90 O89 N88 110.2(5) O1 N3 C7 104.0(5) O1 N3 C21 104.5(7) C7 N3 C21 111.8(6) C37 N33 C34 107.7(5) C37 N33 C27 128.2(6) C27 N33 C34 123.5(6) O63 N62 C61 101.2(5) C78 N62 O63 106.0(6) C78 N62 C61 114.5(6) C8 N2 C7 121.9(6) C14 N2 C7 109.5(6) C14 N2 C8 128.3(6) C64 N60 C61 107.8(6) C64 N60 C54 127.0(7) C54 N60 C61 124.9(7) O36 N35 C34 102.7(5) O36 N35 C52 105.5(6) C34 N35 C52 112.8(6) C90 N97 C98 120.0(7) C90 N86 C87 108.0(5) C90 N86 C81 128.3(7) C81 N86 C87 122.1(7) C64 N71 C72 118.0(7) O89 N88 C87 102.3(5) C104 N88 O89 105.0(7) C104 N88 C87 112.7(6) N33 C34 N35 103.0(6) N33 C34 H34 109.2 N33 C34 C38 114.1(6) N35 C34 H34 109.2 N35 C34 C38 112.0(6) C38 C34 H34 109.2 C37 N44 C47 117.7(7) C14 N1 C15 120.2(7) O89 C90 N86 108.8(6) N97 C90 O89 124.4(7) N97 C90 N86 126.8(7) O63 C64 N60 109.0(6) N71 C64 O63 124.1(7) N71 C64 N60 126.8(7) C92 C91 C87 121.1(7) C92 C91 C96 118.8(8) C96 C91 C87 120.1(7) N62 C61 H61 108.7 N62 C61 C65 112.3(6) N60 C61 N62 104.0(6) N60 C61 H61 108.7 N60 C61 C65 114.2(6) C65 C61 H61 108.7 O36 C37 N33 110.4(6) N44 C37 O36 123.5(7) N44 C37 N33 125.9(6) C73 C72 N71 119.1(8) C77 C72 N71 120.1(8) C77 C72 C73 120.7(8) C32 C27 N33 118.5(6) C32 C27 C28 118.3(7) C28 C27 N33 123.2(7) C70 C65 C61 122.0(8) C70 C65 C66 119.0(8) C66 C65 C61 118.9(8) N86 C87 N88 103.6(6) N86 C87 C91 112.8(6) N86 C87 H87 109.5 N88 C87 C91 111.7(5) N88 C87 H87 109.5 C91 C87 H87 109.5 N3 C7 N2 101.9(6) N3 C7 H7 109.8 N2 C7 H7 109.8 C1 C7 N3 111.8(6) C1 C7 N2 113.4(6) C1 C7 H7 109.8 C82 C81 N86 122.8(9) C80 C81 N86 117.8(9) C80 C81 C82 119.4(9) C2 C1 C7 123.7(8) C6 C1 C7 119.9(7) C6 C1 C2 116.4(8) C27 C32 H32 120.4 C27 C32 C31 119.1(9) C31 C32 H32 120.4 C8 C13 H13 120.3 C12 C13 H13 120.3 C12 C13 C8 119.4(8) N2 C8 C13 122.0(7) C9 C8 N2 118.1(7) C9 C8 C13 119.9(7) C16 C15 N1 118.8(8) C20 C15 N1 121.4(8) C20 C15 C16 119.7(8) N62 C78 H78A 109.5 N62 C78 H78B 109.5 N62 C78 H78C 109.5 H78A C78 H78B 109.5 H78A C78 H78C 109.5 H78B C78 H78C 109.5 C99 C98 N97 120.4(9) C99 C98 C103 117.8(9) C103 C98 N97 121.6(8) C55 C54 N60 124.8(8) C55 C54 C59 117.5(9) C59 C54 N60 117.7(9) C81 C82 H82 119.1 C81 C82 C83 121.8(10) C83 C82 H82 119.1 C43 C38 C34 119.6(8) C43 C38 C39 119.6(9) C39 C38 C34 120.8(8) C72 C73 H73 120.0 C74 C73 C72 120.0(9) C74 C73 H73 120.0 C8 C9 H9 121.3 C10 C9 C8 117.3(8) C10 C9 H9 121.3 C54 C55 H55 118.4 C54 C55 C56 123.1(9) C56 C55 H55 118.4 N2 C14 O1 108.5(6) N1 C14 O1 123.0(7) N1 C14 N2 128.3(7) C65 C70 H70 119.9 C65 C70 C69 120.3(9) C69 C70 H70 119.9 C80 C85 C84 122.7(13) F105 C85 C80 117.5(12) F105 C85 C84 119.7(11) C91 C92 H92 119.9 C91 C92 C93 120.2(8) C93 C92 H92 119.9 C27 C28 H28 120.2 C29 C28 C27 119.6(9) C29 C28 H28 120.2 C54 C59 H59 119.2 C58 C59 C54 121.7(13) C58 C59 H59 119.2 C15 C16 H16 121.5 C15 C16 C17 116.9(9) C17 C16 H16 121.5 C65 C66 H66 119.6 C67 C66 C65 120.8(10) C67 C66 H66 119.6 C73 C74 H74 119.8 C73 C74 C75 120.5(10) C75 C74 H74 119.8 C46 C47 N44 118.6(8) C48 C47 N44 122.8(8) C48 C47 C46 118.5(8) C13 C12 H12 119.5 C13 C12 C11 121.1(8) C11 C12 H12 119.5 N88 C104 H10A 109.5 N88 C104 H10B 109.5 N88 C104 H10C 109.5 H10A C104 H10B 109.5 H10A C104 H10C 109.5 H10B C104 H10C 109.5 C12 C11 H11 120.9 C10 C11 C12 118.3(8) C10 C11 H11 120.9 C15 C20 H20 119.4 C19 C20 C15 121.1(10) C19 C20 H20 119.4 C19 C18 H18 121.0 C17 C18 H18 121.0 C17 C18 C19 118.0(10) C30 C31 C32 124.6(12) C30 C31 F53 119.1(9) F53 C31 C32 116.2(11) C50 C49 H49 120.4 C48 C49 H49 120.4 C48 C49 C50 119.3(10) C55 C56 H56 121.0 C55 C56 C57 117.9(10) C57 C56 H56 121.0 C77 C76 H76 120.1 C75 C76 H76 120.1 C75 C76 C77 119.9(9) C81 C80 C85 119.2(11) C81 C80 H80 120.4 C85 C80 H80 120.4 C72 C77 C76 119.5(8) C72 C77 H77 120.2 C76 C77 H77 120.2 C1 C2 H2 119.1 C3 C2 C1 121.8(11) C3 C2 H2 119.1 C47 C46 H46 120.0 C47 C46 C45 120.1(9) C45 C46 H46 120.0 C69 C68 H68 121.0 C69 C68 C67 118.1(10) C67 C68 H68 121.0 C46 C45 H45 119.4 C50 C45 C46 121.2(9) C50 C45 H45 119.4 C49 C50 H50 120.1 C45 C50 C49 119.8(9) C45 C50 H50 120.1 C38 C43 H43 119.4 C38 C43 C42 121.2(10) C42 C43 H43 119.4 N35 C52 H52A 109.5 N35 C52 H52B 109.5 N35 C52 H52C 109.5 H52A C52 H52B 109.5 H52A C52 H52C 109.5 H52B C52 H52C 109.5 C85 C84 H84 121.3 C85 C84 C83 117.4(11) C83 C84 H84 121.3 C91 C96 H96 119.9 C95 C96 C91 120.2(9) C95 C96 H96 119.9 C82 C83 C84 119.3(10) C82 C83 H83 120.4 C84 C83 H83 120.4 C11 C10 C9 124.0(9) F26 C10 C9 116.2(9) F26 C10 C11 119.7(9) C1 C6 H6 119.2 C1 C6 C5 121.5(11) C5 C6 H6 119.2 F79 C58 C59 120.5(14) F79 C58 C57 118.9(11) C57 C58 C59 120.5(13) C96 C95 H95 120.1 C94 C95 C96 119.9(10) C94 C95 H95 120.1 C3 C4 H4 118.9 C3 C4 C5 122.3(11) C5 C4 H4 118.9 C47 C48 C49 121.2(9) C47 C48 H48 119.4 C49 C48 H48 119.4 C70 C69 H69 119.7 C68 C69 C70 120.6(10) C68 C69 H69 119.7 C98 C99 H99 119.5 C98 C99 C100 121.0(10) C100 C99 H99 119.5 C92 C93 H93 120.1 C94 C93 C92 119.7(9) C94 C93 H93 120.1 C31 C30 H30 122.0 C31 C30 C29 116.1(9) C29 C30 H30 122.0 C20 C19 C18 120.2(11) C20 C19 H19 119.9 C18 C19 H19 119.9 C38 C39 H39 120.3 C38 C39 C40 119.4(10) C40 C39 H39 120.3 C28 C29 C30 122.1(9) C28 C29 H29 118.9 C30 C29 H29 118.9 C16 C17 H17 118.0 C18 C17 C16 123.9(10) C18 C17 H17 118.0 C95 C94 H94 119.4 C93 C94 C95 121.2(10) C93 C94 H94 119.4 N3 C21 H21A 109.5 N3 C21 H21B 109.5 N3 C21 H21C 109.5 H21A C21 H21B 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C2 C3 H3 119.9 C4 C3 C2 120.2(12) C4 C3 H3 119.9 C99 C100 H100 120.3 C101 C100 C99 119.3(10) C101 C100 H100 120.3 C42 C41 H41 119.9 C42 C41 C40 120.2(10) C40 C41 H41 119.9 C43 C42 H42 119.9 C41 C42 C43 120.1(11) C41 C42 H42 119.9 C66 C67 C68 121.2(11) C66 C67 H67 119.4 C68 C67 H67 119.4 C74 C75 H75 120.4 C76 C75 C74 119.3(9) C76 C75 H75 120.4 C98 C103 H103 119.0 C102 C103 C98 121.9(11) C102 C103 H103 119.0 C56 C57 H57 120.4 C58 C57 C56 119.1(10) C58 C57 H57 120.4 C6 C5 H5 121.1 C4 C5 C6 117.8(12) C4 C5 H5 121.1 C39 C40 H40 120.2 C41 C40 C39 119.5(10) C41 C40 H40 120.2 C100 C101 H101 119.7 C100 C101 C102 120.7(11) C102 C101 H101 119.7 C103 C102 C101 119.1(12) C103 C102 H102 120.4 C101 C102 H102 120.4 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 N3 1.460(9) O1 C14 1.381(9) O36 N35 1.467(8) O36 C37 1.342(9) O63 N62 1.465(8) O63 C64 1.367(9) O89 N88 1.468(9) O89 C90 1.355(9) N3 C7 1.479(10) N3 C21 1.486(10) N33 C34 1.467(9) N33 C37 1.376(9) N33 C27 1.396(8) N62 C61 1.480(9) N62 C78 1.450(10) N2 C7 1.498(9) N2 C8 1.408(10) N2 C14 1.371(10) N60 C64 1.378(9) N60 C61 1.464(10) N60 C54 1.387(10) N35 C34 1.471(10) N35 C52 1.486(11) N97 C90 1.265(10) N97 C98 1.410(11) N86 C90 1.386(10) N86 C87 1.474(9) N86 C81 1.414(10) N71 C64 1.260(10) N71 C72 1.457(10) N88 C87 1.474(10) N88 C104 1.468(11) C34 H34 0.9800 C34 C38 1.520(11) N44 C37 1.274(10) N44 C47 1.433(11) N1 C15 1.416(11) N1 C14 1.272(10) C91 C87 1.519(10) C91 C92 1.371(11) C91 C96 1.398(12) C61 H61 0.9800 C61 C65 1.500(11) C72 C73 1.379(12) C72 C77 1.362(13) C27 C32 1.379(12) C27 C28 1.395(11) C65 C70 1.373(11) C65 C66 1.387(12) C87 H87 0.9800 C7 H7 0.9800 C7 C1 1.479(11) C81 C82 1.374(13) C81 C80 1.370(16) C1 C2 1.407(11) C1 C6 1.368(12) C32 H32 0.9300 C32 C31 1.386(12) C13 H13 0.9300 C13 C8 1.415(11) C13 C12 1.379(12) C8 C9 1.412(12) C15 C16 1.394(12) C15 C20 1.384(13) C78 H78A 0.9600 C78 H78B 0.9600 C78 H78C 0.9600 C98 C99 1.354(13) C98 C103 1.389(14) C54 C55 1.361(12) C54 C59 1.386(15) C82 H82 0.9300 C82 C83 1.391(11) C38 C43 1.363(12) C38 C39 1.374(12) C73 H73 0.9300 C73 C74 1.372(13) C9 H9 0.9300 C9 C10 1.403(12) C55 H55 0.9300 C55 C56 1.395(12) C70 H70 0.9300 C70 C69 1.407(14) C85 C80 1.386(16) C85 C84 1.383(19) C85 F105 1.363(16) C92 H92 0.9300 C92 C93 1.408(13) C28 H28 0.9300 C28 C29 1.381(12) C59 H59 0.9300 C59 C58 1.374(16) C16 H16 0.9300 C16 C17 1.399(14) C66 H66 0.9300 C66 C67 1.341(16) C74 H74 0.9300 C74 C75 1.383(17) C47 C46 1.375(12) C47 C48 1.375(13) C12 H12 0.9300 C12 C11 1.415(14) C104 H10A 0.9600 C104 H10B 0.9600 C104 H10C 0.9600 C11 H11 0.9300 C11 C10 1.337(14) C20 H20 0.9300 C20 C19 1.367(15) C18 H18 0.9300 C18 C19 1.394(17) C18 C17 1.345(17) C31 C30 1.328(18) C31 F53 1.373(16) C49 H49 0.9300 C49 C50 1.393(15) C49 C48 1.376(14) C56 H56 0.9300 C56 C57 1.411(17) C76 H76 0.9300 C76 C77 1.403(14) C76 C75 1.387(16) C80 H80 0.9300 C77 H77 0.9300 C2 H2 0.9300 C2 C3 1.365(15) C46 H46 0.9300 C46 C45 1.390(13) C68 H68 0.9300 C68 C69 1.354(18) C68 C67 1.425(18) C45 H45 0.9300 C45 C50 1.331(15) F26 C10 1.328(12) C50 H50 0.9300 C43 H43 0.9300 C43 C42 1.380(14) C52 H52A 0.9600 C52 H52B 0.9600 C52 H52C 0.9600 C84 H84 0.9300 C84 C83 1.402(17) C96 H96 0.9300 C96 C95 1.389(15) C83 H83 0.9300 C6 H6 0.9300 C6 C5 1.420(15) C58 F79 1.322(15) C58 C57 1.38(2) C95 H95 0.9300 C95 C94 1.357(16) C4 H4 0.9300 C4 C3 1.32(2) C4 C5 1.363(19) C48 H48 0.9300 C69 H69 0.9300 C99 H99 0.9300 C99 C100 1.393(15) C93 H93 0.9300 C93 C94 1.354(15) C30 H30 0.9300 C30 C29 1.395(16) C19 H19 0.9300 C39 H39 0.9300 C39 C40 1.420(14) C29 H29 0.9300 C17 H17 0.9300 C94 H94 0.9300 C21 H21A 0.9600 C21 H21B 0.9600 C21 H21C 0.9600 C3 H3 0.9300 C100 H100 0.9300 C100 C101 1.338(18) C41 H41 0.9300 C41 C42 1.361(17) C41 C40 1.372(18) C42 H42 0.9300 C67 H67 0.9300 C75 H75 0.9300 C103 H103 0.9300 C103 C102 1.337(17) C57 H57 0.9300 C5 H5 0.9300 C40 H40 0.9300 C101 H101 0.9300 C101 C102 1.385(19) C102 H102 0.9300 loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons 1 0.229 0.741 0.890 21.3 0.3 2 0.354 0.781 0.200 7.2 1.0 3 0.646 0.281 0.800 7.2 1.0 4 0.771 0.241 0.110 21.3 0.3