#------------------------------------------------------------------------------ #$Date: 2019-11-11 16:44:48 +0200 (Mon, 11 Nov 2019) $ #$Revision: 226605 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/51/4035119.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_4035119 loop_ _publ_author_name 'Wang, Xu' 'Li, Jiawei' 'Huang, Yubing' 'Zhu, Jiayi' 'Hu, Rongrong' 'Wu, Wanqing' 'Jiang, Huanfeng' _publ_section_title ; Facile Synthesis of \p-Conjugated Quinazoline-Substituted Ethenes from 2-Ethynylanilines and Benzonitriles under Transition-Metal-Free Conditions. ; _journal_issue 17 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 10453 _journal_page_last 10464 _journal_paper_doi 10.1021/acs.joc.8b01494 _journal_volume 83 _journal_year 2018 _chemical_formula_moiety 'C46 H30 F6 N4 O2' _chemical_formula_sum 'C46 H30 F6 N4 O2' _chemical_formula_weight 784.74 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2017-06-22 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337) ; _cell_angle_alpha 90 _cell_angle_beta 108.176(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.9060(2) _cell_length_b 16.6094(2) _cell_length_c 16.5593(2) _cell_measurement_reflns_used 7306 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 73.3820 _cell_measurement_theta_min 4.4910 _cell_volume 3633.86(9) _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _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_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2684 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.958 _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 12.00 54.00 1.00 1.00 -- 40.46 57.00 -30.00 42 2 \w 78.00 178.00 1.00 1.50 -- 107.48 61.00-120.00 100 3 \w 102.00 142.00 1.00 1.50 -- 107.48 111.00 -30.00 40 4 \w 82.00 175.00 1.00 1.50 -- 107.48 45.00 150.00 93 5 \w 80.00 105.00 1.00 1.50 -- 107.48 -94.00 60.00 25 6 \w 56.00 139.00 1.00 1.50 -- 107.48 -77.00 90.00 83 7 \w 43.00 121.00 1.00 1.50 -- 107.48 -45.00 -30.00 78 8 \w 23.00 90.00 1.00 1.50 -- 107.48 -94.00 -60.00 67 9 \w -58.00 31.00 1.00 1.00 -- -40.46 37.00-120.00 89 10 \w -89.00 -40.00 1.00 1.00 -- -40.46 -19.00 30.00 49 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0939824000 _diffrn_orient_matrix_UB_12 0.0050766000 _diffrn_orient_matrix_UB_13 -0.0301315000 _diffrn_orient_matrix_UB_21 -0.0531900000 _diffrn_orient_matrix_UB_22 -0.0530578000 _diffrn_orient_matrix_UB_23 -0.0771887000 _diffrn_orient_matrix_UB_31 -0.0437906000 _diffrn_orient_matrix_UB_32 0.0760316000 _diffrn_orient_matrix_UB_33 -0.0520677000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_unetI/netI 0.0305 _diffrn_reflns_Laue_measured_fraction_full 0.981 _diffrn_reflns_Laue_measured_fraction_max 0.958 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 14276 _diffrn_reflns_point_group_measured_fraction_full 0.981 _diffrn_reflns_point_group_measured_fraction_max 0.958 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.667 _diffrn_reflns_theta_min 3.636 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.929 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.77464 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.434 _exptl_crystal_description block _exptl_crystal_F_000 1616 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.400 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.045 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 525 _refine_ls_number_reflns 7031 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0439 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+1.2234P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1161 _refine_ls_wR_factor_ref 0.1248 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5985 _reflns_number_total 7031 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b01494_si_003.cif _cod_data_source_block exp_684 _cod_database_code 4035119 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.897 _shelx_estimated_absorpt_t_min 0.851 _reflns_odcompleteness_completeness 97.87 _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.a Aromatic/amide H refined with riding coordinates: C3'(H3'), C7'(H7'), C22(H22), C19(H19), C4(H4), C11'(H11'), C4'(H4'), C3(H3), C21(H21), C18(H18), C6'(H6'), C14'(H14'), C14(H14), C22'(H22'), C11(H11), C13(H13), C12'(H12'), C18'(H18'), C13'(H13'), C19'(H19'), C21'(H21'), C12(H12), C7(H7), C6(H6) 2.b Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C8'(H8'A,H8'B,H8'C) ; _shelx_res_file ; TITL exp_684_a.res in P2(1)/n exp_684.res created by SHELXL-2016/6 at 22:15:01 on 22-Jun-2017 REM Old TITL exp_684 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.140, Rweak 0.020, Alpha 0.024, Orientation as input REM Formula found by SHELXT: C46 N6 F6 CELL 1.54184 13.906 16.6094 16.5593 90 108.176 90 ZERR 4 0.0002 0.0002 0.0002 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F N O UNIT 184 120 24 16 8 L.S. 20 0 0 PLAN 20 SIZE 0.18 0.15 0.12 BOND $H list 4 fmap 2 53 acta REM REM REM WGHT 0.064500 1.223400 FVAR 0.34672 F2' 3 -0.271296 0.613292 -0.131599 11.00000 0.04314 0.03615 = 0.02871 0.00357 0.00566 0.00193 F1' 3 -0.332939 0.537605 -0.054728 11.00000 0.03268 0.04301 = 0.04331 0.00341 0.00598 -0.00574 F3' 3 -0.313057 0.664649 -0.028145 11.00000 0.03989 0.04550 = 0.04404 -0.00668 0.00803 0.01205 F2 3 0.811117 0.116146 0.307894 11.00000 0.03983 0.04186 = 0.08104 0.00775 0.02843 0.01300 F1 3 0.850553 0.233282 0.360652 11.00000 0.03121 0.06585 = 0.08831 -0.01973 0.01828 -0.00177 O1' 5 0.150852 0.096155 0.595386 11.00000 0.04125 0.04233 = 0.04763 0.01810 0.02484 0.00469 F3 3 0.815402 0.214280 0.226723 11.00000 0.04812 0.09333 = 0.07837 0.03222 0.04436 0.01697 N1 4 0.123291 0.483355 0.247939 11.00000 0.03091 0.02322 = 0.02481 -0.00057 0.01119 -0.00106 N1' 4 0.338356 0.281852 0.310985 11.00000 0.02727 0.02226 = 0.02608 0.00196 0.01231 0.00222 N2 4 0.206249 0.564921 0.170053 11.00000 0.03284 0.02335 = 0.02801 -0.00082 0.01306 -0.00252 N2' 4 0.300565 0.207463 0.180483 11.00000 0.03314 0.02418 = 0.02837 -0.00028 0.01457 0.00133 O1 5 0.128034 0.585989 0.642935 11.00000 0.09315 0.05224 = 0.03387 -0.00439 0.02513 0.02646 C16 1 0.125375 0.533750 0.182968 11.00000 0.03157 0.02126 = 0.02489 -0.00157 0.01192 -0.00029 C1' 1 0.212854 0.331909 0.370909 11.00000 0.02243 0.02488 = 0.02408 0.00118 0.00878 0.00305 C2' 1 0.193896 0.272741 0.432004 11.00000 0.02575 0.02290 = 0.02248 -0.00112 0.00931 0.00110 C9 1 0.210672 0.464232 0.303556 11.00000 0.03171 0.02005 = 0.02563 -0.00249 0.01118 0.00096 C1 1 0.204158 0.411809 0.375690 11.00000 0.02485 0.02587 = 0.02584 0.00140 0.01039 0.00249 C16' 1 0.363824 0.240660 0.248884 11.00000 0.03105 0.02059 = 0.02590 0.00328 0.01299 0.00237 C10' 1 0.165107 0.263702 0.226177 11.00000 0.03007 0.02273 = 0.02542 0.00237 0.01139 -0.00040 C17 1 0.024051 0.552927 0.122194 11.00000 0.03213 0.02107 = 0.02529 -0.00108 0.01128 0.00055 C9' 1 0.241251 0.292602 0.299787 11.00000 0.02937 0.01954 = 0.02476 0.00346 0.01219 0.00127 C15' 1 0.200065 0.218826 0.168137 11.00000 0.03517 0.02284 = 0.02690 0.00158 0.01369 -0.00055 C3' 1 0.101989 0.269670 0.449100 11.00000 0.02545 0.03210 = 0.03096 0.00389 0.01034 0.00575 AFIX 43 H3' 2 0.051912 0.307207 0.424141 11.00000 -1.20000 AFIX 0 C17' 1 0.473749 0.232040 0.260746 11.00000 0.03105 0.02268 = 0.03083 0.00461 0.01561 0.00459 C10 1 0.304271 0.492886 0.297075 11.00000 0.03186 0.02279 = 0.02954 -0.00315 0.01318 -0.00112 C15 1 0.297402 0.544333 0.227050 11.00000 0.03142 0.02313 = 0.03020 -0.00363 0.01292 -0.00040 C7' 1 0.267295 0.215804 0.469921 11.00000 0.02590 0.03095 = 0.02998 0.00340 0.01227 0.00403 AFIX 43 H7' 2 0.328405 0.216195 0.458061 11.00000 -1.20000 AFIX 0 C20 1 -0.166459 0.583399 0.007779 11.00000 0.03177 0.02459 = 0.02862 -0.00270 0.00936 0.00127 C2 1 0.185901 0.456285 0.447769 11.00000 0.03515 0.02378 = 0.02790 0.00072 0.01406 0.00093 C22 1 -0.063243 0.530704 0.141562 11.00000 0.03355 0.03016 = 0.02721 0.00267 0.01360 0.00047 AFIX 43 H22 2 -0.057527 0.505463 0.192983 11.00000 -1.20000 AFIX 0 C19 1 -0.080530 0.605945 -0.012218 11.00000 0.03727 0.02493 = 0.02592 0.00089 0.01262 -0.00082 AFIX 43 H19 2 -0.086568 0.631128 -0.063729 11.00000 -1.20000 AFIX 0 C4 1 0.225819 0.482158 0.598758 11.00000 0.03608 0.03437 = 0.02702 -0.00148 0.01070 -0.00365 AFIX 43 H4 2 0.264614 0.470774 0.654370 11.00000 -1.20000 AFIX 0 C11' 1 0.060065 0.275695 0.209804 11.00000 0.02975 0.03048 = 0.02858 0.00206 0.01178 0.00065 AFIX 43 H11' 2 0.036723 0.305450 0.247468 11.00000 -1.20000 AFIX 0 C4' 1 0.083992 0.211360 0.502891 11.00000 0.02657 0.03796 = 0.03429 0.00353 0.01443 0.00076 AFIX 43 H4' 2 0.021912 0.209409 0.513029 11.00000 -1.20000 AFIX 0 C3 1 0.240951 0.439586 0.531342 11.00000 0.02911 0.02946 = 0.03053 -0.00143 0.01033 0.00046 AFIX 43 H3 2 0.289267 0.398887 0.542717 11.00000 -1.20000 AFIX 0 C21 1 -0.157525 0.545928 0.085066 11.00000 0.03102 0.03215 = 0.03287 0.00095 0.01438 -0.00006 AFIX 43 H21 2 -0.215274 0.531213 0.098457 11.00000 -1.20000 AFIX 0 C23 1 -0.270044 0.599677 -0.051696 11.00000 0.03491 0.03018 = 0.03392 -0.00064 0.01137 0.00179 C18 1 0.014309 0.590777 0.044893 11.00000 0.03297 0.02329 = 0.02854 -0.00004 0.01370 -0.00198 AFIX 43 H18 2 0.071939 0.605962 0.031566 11.00000 -1.20000 AFIX 0 C6' 1 0.251247 0.158812 0.524728 11.00000 0.02995 0.03275 = 0.03262 0.00703 0.01235 0.00596 AFIX 43 H6' 2 0.302013 0.122119 0.550634 11.00000 -1.20000 AFIX 0 C14' 1 0.128796 0.185897 0.094682 11.00000 0.03950 0.03111 = 0.02993 -0.00416 0.01474 -0.00381 AFIX 43 H14' 2 0.150752 0.156054 0.056260 11.00000 -1.20000 AFIX 0 C14 1 0.387478 0.574241 0.215165 11.00000 0.03548 0.02802 = 0.03509 -0.00083 0.01630 -0.00315 AFIX 43 H14 2 0.384271 0.608055 0.169633 11.00000 -1.20000 AFIX 0 C22' 1 0.505471 0.196990 0.196508 11.00000 0.03563 0.03539 = 0.03130 0.00078 0.01629 0.00358 AFIX 43 H22' 2 0.457684 0.180770 0.146098 11.00000 -1.20000 AFIX 0 C5' 1 0.159288 0.155985 0.541443 11.00000 0.03403 0.02818 = 0.02883 0.00407 0.01360 -0.00064 C11 1 0.399965 0.472247 0.353909 11.00000 0.03286 0.02723 = 0.03537 0.00053 0.01052 0.00041 AFIX 43 H11 2 0.404625 0.438882 0.400079 11.00000 -1.20000 AFIX 0 C13 1 0.479102 0.553059 0.271067 11.00000 0.03243 0.03375 = 0.04566 -0.00512 0.01767 -0.00580 AFIX 43 H13 2 0.538022 0.572896 0.263086 11.00000 -1.20000 AFIX 0 C20' 1 0.678829 0.210996 0.282398 11.00000 0.03247 0.03046 = 0.04362 0.00738 0.01988 0.00409 C12' 1 -0.007295 0.243246 0.138105 11.00000 0.02980 0.03789 = 0.03418 0.00302 0.01091 -0.00264 AFIX 43 H12' 2 -0.076396 0.250986 0.127362 11.00000 -1.20000 AFIX 0 C18' 1 0.546213 0.258142 0.334932 11.00000 0.03342 0.03132 = 0.03357 -0.00003 0.01611 0.00413 AFIX 43 H18' 2 0.525853 0.282926 0.377268 11.00000 -1.20000 AFIX 0 C13' 1 0.027669 0.198169 0.080527 11.00000 0.03771 0.03832 = 0.02978 -0.00159 0.00803 -0.00898 AFIX 43 H13' 2 -0.018847 0.176499 0.032226 11.00000 -1.20000 AFIX 0 C19' 1 0.648729 0.247442 0.346197 11.00000 0.03073 0.03524 = 0.03900 0.00064 0.01258 0.00146 AFIX 43 H19' 2 0.696831 0.264536 0.396043 11.00000 -1.20000 AFIX 0 C21' 1 0.607387 0.186296 0.207445 11.00000 0.03858 0.03827 = 0.03934 0.00237 0.02323 0.00942 AFIX 43 H21' 2 0.627999 0.162613 0.164684 11.00000 -1.20000 AFIX 0 C12 1 0.486265 0.501696 0.340700 11.00000 0.02959 0.03486 = 0.04423 -0.00068 0.00882 -0.00047 AFIX 43 H12 2 0.549458 0.487774 0.377675 11.00000 -1.20000 AFIX 0 C5 1 0.152246 0.541787 0.582184 11.00000 0.06654 0.03555 = 0.03162 -0.00308 0.02304 0.01068 C23' 1 0.788240 0.194540 0.294652 11.00000 0.03523 0.03910 = 0.05269 0.00449 0.02208 0.00233 C7 1 0.112969 0.516859 0.432397 11.00000 0.07793 0.05089 = 0.02927 0.00545 0.01800 0.03360 AFIX 43 H7 2 0.075710 0.529334 0.376660 11.00000 -1.20000 AFIX 0 C8 1 0.194379 0.579665 0.727342 11.00000 0.08036 0.04394 = 0.03375 -0.00680 0.02854 -0.00432 AFIX 137 H8A 2 0.261972 0.592867 0.728402 11.00000 -1.50000 H8B 2 0.192947 0.525598 0.747428 11.00000 -1.50000 H8C 2 0.173127 0.616249 0.763330 11.00000 -1.50000 AFIX 0 C8' 1 0.053514 0.083877 0.604606 11.00000 0.05098 0.05744 = 0.07798 0.02927 0.03983 0.00375 AFIX 137 H8'A 2 0.004458 0.076904 0.549564 11.00000 -1.50000 H8'B 2 0.035590 0.129785 0.632098 11.00000 -1.50000 H8'C 2 0.054845 0.036659 0.638373 11.00000 -1.50000 AFIX 0 C6 1 0.094986 0.558688 0.498326 11.00000 0.09702 0.05735 = 0.03620 0.00497 0.02415 0.04652 AFIX 43 H6 2 0.044899 0.597992 0.486924 11.00000 -1.20000 AFIX 0 HKLF 4 REM exp_684_a.res in P2(1)/n REM R1 = 0.0439 for 5985 Fo > 4sig(Fo) and 0.0522 for all 7031 data REM 525 parameters refined using 0 restraints END WGHT 0.0612 1.3153 REM Highest difference peak 0.400, deepest hole -0.230, 1-sigma level 0.045 Q1 1 0.5853 0.4717 0.4040 11.00000 0.05 0.40 Q2 1 0.1975 0.6006 0.6573 11.00000 0.05 0.36 Q3 1 0.1672 0.5801 0.5151 11.00000 0.05 0.33 Q4 1 0.1815 0.5407 0.4442 11.00000 0.05 0.28 Q5 1 0.2143 0.5437 0.5966 11.00000 0.05 0.23 Q6 1 -0.1225 0.2634 0.1031 11.00000 0.05 0.23 Q7 1 0.0771 0.5396 0.1553 11.00000 0.05 0.21 Q8 1 -0.3585 0.5771 -0.0246 11.00000 0.05 0.20 Q9 1 0.2016 0.3026 0.4017 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1.33 -8 8 -11 11.48 1.14 -8 -8 -11 11.13 1.39 -8 8 -12 32.35 1.57 -8 -8 -12 28.56 1.82 -8 8 -12 29.16 1.69 8 9 -17 0.76 0.45 8 9 -16 18.94 1.71 8 -9 -16 18.48 1.56 8 9 -15 48.83 3.04 8 -9 -15 43.98 2.71 8 -9 -14 17.48 1.81 8 -9 -13 7.76 1.34 8 9 -13 6.68 1.18 -8 9 12 0.36 0.67 8 -9 -12 2.01 0.99 8 9 -12 0.86 0.64 -8 9 11 64.52 4.48 8 9 -11 67.10 3.70 -8 9 11 65.70 3.82 -8 9 10 35.06 3.34 8 9 -10 34.41 2.63 -8 9 10 37.58 2.83 -8 9 9 8.19 1.28 -8 9 9 10.55 1.94 -8 9 8 1.24 0.89 -8 9 8 0.58 0.86 -8 9 7 123.03 6.49 -8 9 7 121.85 6.61 -8 9 7 122.17 5.04 -8 9 6 108.13 6.01 -8 9 6 107.55 6.12 -8 9 6 106.11 4.69 -8 9 5 38.94 3.57 -8 9 5 44.04 3.87 -8 9 5 45.60 3.03 -8 9 4 0.87 0.74 -8 9 4 -0.27 0.65 -8 9 4 1.20 0.94 -8 9 3 15.27 2.25 -8 9 3 15.08 2.27 -8 9 3 16.23 1.79 -8 9 2 33.37 3.22 -8 9 2 29.50 3.12 -8 9 2 30.10 2.45 -8 9 1 157.31 7.00 -8 9 1 145.08 6.88 -8 9 1 139.37 5.52 -8 9 0 75.43 3.99 -8 9 -1 3.97 1.04 -8 9 -1 2.80 0.84 -8 9 -2 1.64 0.86 -8 9 -2 0.52 0.57 -8 9 -3 1.07 0.80 -8 9 -3 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4.63 0.98 14 6 1 15.05 1.59 -14 6 -1 15.13 1.31 14 6 2 10.95 1.28 -14 6 -2 9.08 0.99 -14 6 -3 6.65 0.77 14 6 3 10.68 1.16 14 6 4 0.68 0.38 -14 7 14 1.35 0.53 14 7 -14 1.43 0.46 -14 7 13 -0.85 0.62 14 7 -13 0.14 0.37 -14 7 12 0.95 0.56 14 7 -12 1.44 0.56 -14 7 11 2.58 0.92 14 7 -11 2.61 0.73 -14 7 10 2.46 0.89 14 7 -10 3.98 0.89 -14 7 9 33.26 2.86 14 7 -9 36.31 2.50 -14 7 8 34.92 2.94 14 7 -8 37.43 2.56 -14 7 7 20.13 2.28 14 7 -7 22.74 2.06 -14 7 7 24.02 1.68 -14 7 6 58.55 3.79 14 7 -6 66.78 3.55 -14 7 6 61.36 2.78 -14 7 5 1.67 0.73 -14 7 5 1.13 0.74 14 7 -5 -0.01 0.60 -14 7 4 7.41 1.08 14 7 -4 5.89 1.11 -14 7 3 -0.17 0.46 14 7 -3 -0.13 0.52 14 7 -2 25.97 2.15 -14 7 2 25.16 1.80 14 7 -1 23.40 2.00 -14 7 1 23.31 1.71 -14 7 0 5.07 0.82 14 7 0 5.48 0.99 14 7 1 34.56 2.21 -14 7 -1 31.26 1.84 14 7 2 16.07 1.42 -14 7 -2 13.63 1.16 -14 7 -3 3.10 0.54 14 7 3 4.34 0.73 -14 8 13 14.95 1.50 14 8 -13 15.18 1.18 -14 8 12 1.84 0.68 14 8 -12 2.18 0.57 -14 8 11 9.08 1.38 14 8 -11 9.04 1.10 -14 8 10 41.16 3.01 14 8 -10 45.17 2.52 -14 8 9 -0.25 0.48 -14 8 9 -0.37 0.66 14 8 -9 -0.67 0.47 -14 8 8 21.44 2.26 14 8 -8 23.40 1.95 -14 8 8 19.96 1.48 -14 8 7 19.07 2.10 14 8 -7 21.63 1.89 -14 8 7 18.61 1.47 -14 8 6 10.40 1.59 14 8 -6 11.37 1.41 -14 8 6 12.09 1.22 14 8 -5 29.09 2.19 -14 8 5 26.22 1.81 -14 8 4 4.77 0.92 14 8 -4 3.83 0.83 -14 8 3 1.74 0.66 14 8 -3 2.02 0.63 -14 8 2 -0.67 0.73 14 8 -2 0.30 0.43 -14 8 1 4.85 0.79 14 8 -1 5.41 0.94 -14 8 0 6.12 0.89 14 8 0 4.78 0.83 -14 8 -1 0.48 0.43 14 8 1 0.39 0.34 -14 8 -2 4.93 0.69 14 8 2 4.21 0.68 -14 9 12 2.58 0.67 -14 9 11 0.55 0.51 14 9 -11 -0.13 0.35 -14 9 10 5.18 1.13 14 9 -10 3.54 0.69 -14 9 9 9.57 1.42 14 9 -9 10.84 1.17 -14 9 8 13.94 1.76 14 9 -8 12.49 1.30 -14 9 8 10.59 1.08 -14 9 7 8.66 1.01 14 9 -7 9.05 1.13 -14 9 6 1.84 0.64 14 9 -6 1.45 0.53 -14 9 5 2.79 0.75 14 9 -5 2.04 0.61 -14 9 4 5.30 0.93 14 9 -4 3.53 0.75 -14 9 3 5.37 0.86 14 9 -3 5.41 0.88 -14 9 2 5.02 0.77 14 9 -2 7.32 0.93 -14 9 1 2.26 0.63 14 9 -1 4.84 0.77 -14 9 0 2.90 0.57 14 9 0 6.62 0.84 -14 9 -1 31.85 1.64 -14 9 -2 -2.65 0.67 14 -10 -10 23.11 1.34 -14 10 8 6.23 0.83 -14 10 7 9.24 1.04 -14 10 6 2.48 0.72 -14 10 5 0.31 0.58 -14 10 4 12.94 1.22 -14 10 3 5.36 0.87 -14 10 2 26.89 1.62 -14 10 1 -1.91 0.72 -14 10 0 -1.85 0.70 -14 11 8 31.42 1.56 -14 11 7 -0.59 0.52 -14 11 6 2.02 0.63 -14 11 5 20.70 1.39 -14 11 4 1.78 0.65 -14 11 3 3.88 0.72 -14 11 2 16.52 1.19 -14 11 1 0.52 0.47 -15 0 15 1.74 0.60 -15 0 14 -0.10 0.46 15 0 -14 -0.26 0.33 -15 0 13 4.70 1.03 15 0 -13 5.43 0.86 -15 0 12 1.22 0.70 15 0 -12 -0.28 0.47 -15 0 11 1.48 0.82 15 0 -11 0.63 0.58 -15 0 10 -0.12 0.56 15 0 -10 0.06 0.55 -15 0 9 0.63 0.51 15 0 -9 0.10 0.49 -15 0 8 -0.18 0.52 15 0 -8 0.39 0.48 15 0 -7 1.41 0.65 15 0 -6 -0.08 0.59 15 0 -5 8.60 1.34 15 0 -4 0.04 0.57 15 0 -3 12.28 1.53 15 0 -2 0.54 0.58 15 0 -1 20.71 1.93 15 0 0 0.82 0.54 15 0 1 2.29 0.69 15 0 2 0.99 0.51 15 0 3 11.68 1.11 -15 1 15 4.65 0.83 -15 -1 15 4.82 0.83 -15 1 14 10.46 1.31 -15 -1 14 9.30 1.23 15 1 -14 7.82 0.97 15 -1 -14 7.38 0.89 -15 1 13 38.94 2.67 -15 -1 13 37.16 2.56 15 -1 -13 36.96 2.12 15 1 -13 37.54 2.21 -15 1 12 0.80 0.64 -15 -1 12 0.87 0.64 15 -1 -12 0.48 0.44 15 1 -12 0.70 0.46 -15 1 11 34.50 2.72 -15 -1 11 36.84 2.73 15 -1 -11 32.79 2.26 15 1 -11 34.06 2.37 -15 1 10 101.55 4.76 -15 -1 10 96.29 4.53 15 -1 -10 101.61 4.21 15 1 -10 102.03 4.29 -15 1 9 2.09 0.82 -15 -1 9 3.25 0.95 15 -1 -9 3.13 0.84 15 1 -9 2.53 0.75 -15 1 8 0.53 0.67 -15 -1 8 1.48 0.64 15 -1 -8 0.29 0.51 15 1 -8 0.31 0.56 -15 1 7 11.95 1.56 15 1 -7 13.47 1.62 15 -1 -7 9.40 1.32 15 -1 -6 1.94 0.76 15 1 -6 0.45 0.58 15 -1 -5 0.62 0.60 15 1 -5 -0.60 0.76 15 -1 -4 -0.33 0.54 15 1 -4 -0.30 0.52 15 -1 -3 14.10 1.63 15 1 -3 16.15 1.78 15 -1 -2 4.32 0.95 15 1 -2 5.10 0.99 15 -1 -1 23.31 1.96 15 1 -1 26.89 2.15 15 -1 0 11.52 1.33 15 1 0 11.27 1.39 15 1 1 9.88 1.27 15 -1 1 8.35 1.10 15 -1 2 1.32 0.49 15 1 2 1.27 0.55 15 -1 3 15.16 1.18 15 1 3 15.58 1.30 -15 2 15 0.28 0.39 -15 -2 15 0.69 0.46 15 2 -15 -0.06 0.28 -15 2 14 15.50 1.58 -15 -2 14 13.96 1.45 15 2 -14 14.25 1.25 -15 2 13 30.26 2.34 -15 -2 13 31.74 2.28 15 -2 -13 27.80 1.70 15 2 -13 31.81 2.02 -15 2 12 0.36 0.55 -15 -2 12 1.02 0.66 15 -2 -12 0.26 0.37 15 2 -12 -0.13 0.44 -15 2 11 28.93 2.47 -15 -2 11 28.60 2.33 15 -2 -11 27.06 1.93 15 2 -11 27.02 2.14 -15 2 10 2.04 0.82 -15 -2 10 0.87 0.66 15 -2 -10 3.05 0.78 15 2 -10 2.16 0.78 -15 2 9 -0.39 0.65 -15 -2 9 0.84 0.60 15 -2 -9 0.16 0.46 15 2 -9 0.42 0.52 -15 2 8 16.39 1.91 15 -2 -8 17.44 1.73 15 2 -8 22.02 2.01 -15 2 7 3.06 0.94 15 -2 -7 2.25 0.69 15 2 -7 1.97 0.69 15 -2 -6 5.09 1.01 15 2 -6 6.10 1.19 15 -2 -5 11.62 1.45 15 2 -5 14.40 1.71 15 -2 -4 42.60 2.72 15 2 -4 47.93 3.07 15 -2 -3 9.67 1.33 15 2 -3 10.27 1.47 15 -2 -2 0.63 0.49 15 2 -2 0.62 0.57 15 -2 -1 15.08 1.53 15 2 -1 15.62 1.67 15 -2 0 4.69 0.85 15 2 0 5.02 0.98 15 -2 1 2.88 0.69 15 2 1 2.50 0.75 15 -2 2 0.83 0.46 15 2 2 0.44 0.42 15 2 3 7.05 0.91 -15 3 14 3.89 0.90 -15 -3 14 3.53 0.77 15 3 -14 3.57 0.66 -15 3 13 14.63 1.61 -15 -3 13 15.67 1.55 15 3 -13 13.92 1.36 -15 3 12 5.63 1.12 -15 -3 12 7.53 1.20 15 3 -12 4.36 0.87 -15 3 11 0.45 0.65 -15 -3 11 1.93 0.69 15 3 -11 2.09 0.72 -15 3 10 0.20 0.62 -15 -3 10 1.17 0.65 15 -3 -10 1.30 0.57 15 3 -10 0.50 0.62 -15 3 9 0.28 0.56 -15 -3 9 2.22 0.74 15 -3 -9 1.24 0.58 15 3 -9 0.91 0.67 -15 3 8 -0.38 0.76 15 -3 -8 0.51 0.53 15 3 -8 -0.41 0.65 -15 3 7 6.41 1.23 15 -3 -7 6.06 1.04 15 3 -7 5.64 1.18 15 -3 -6 0.85 0.52 15 3 -6 0.15 0.54 15 -3 -5 1.04 0.56 15 3 -5 0.42 0.53 15 -3 -4 25.10 1.95 15 3 -4 24.33 2.20 15 -3 -3 1.91 0.64 15 3 -3 2.74 0.85 15 -3 -2 -0.39 0.51 15 3 -2 -0.39 0.61 15 -3 -1 3.71 0.76 15 3 -1 4.59 1.01 15 -3 0 1.41 0.52 15 3 0 2.33 0.80 15 -3 1 4.50 0.70 15 3 1 6.12 1.00 15 3 2 6.49 0.96 15 3 3 29.64 1.75 -15 4 14 4.21 0.84 -15 -4 14 3.11 0.70 15 4 -14 4.49 0.71 -15 4 13 1.43 0.61 -15 -4 13 1.26 0.57 15 4 -13 1.46 0.50 -15 4 12 9.18 1.37 -15 -4 12 8.72 1.18 15 4 -12 6.78 1.03 -15 4 11 -0.44 0.68 -15 -4 11 -0.44 0.44 15 4 -11 -0.30 0.53 -15 4 10 24.60 2.31 -15 -4 10 23.84 1.98 15 4 -10 24.14 1.99 -15 4 9 0.49 0.61 15 4 -9 0.67 0.51 -15 4 8 1.84 0.74 15 4 -8 5.27 1.08 -15 4 7 -0.01 0.58 15 4 -7 -0.18 0.54 -15 4 6 0.45 0.47 15 4 -6 1.18 0.65 15 4 -5 1.56 0.75 15 4 -4 -0.23 0.56 15 4 -3 39.92 2.68 15 4 -2 0.65 0.55 15 4 -1 7.62 1.15 15 4 0 0.77 0.50 15 4 1 7.56 1.06 15 4 2 5.33 0.83 15 4 3 6.20 0.80 -15 5 14 -0.13 0.44 15 5 -14 0.25 0.31 -15 5 13 0.20 0.46 -15 -5 13 -0.14 0.42 15 5 -13 0.74 0.40 -15 5 12 19.71 1.90 -15 -5 12 18.50 1.59 15 5 -12 21.95 1.67 -15 5 11 6.01 1.20 -15 -5 11 8.12 1.11 15 5 -11 8.78 1.15 -15 5 10 -1.28 0.83 15 5 -10 -0.08 0.48 -15 5 9 3.98 1.06 15 5 -9 5.21 1.01 -15 5 8 38.18 2.84 15 5 -8 48.04 2.83 -15 5 7 7.97 1.34 15 5 -7 8.28 1.23 -15 5 6 -0.35 0.52 15 5 -6 -0.05 0.53 15 5 -5 8.81 1.32 15 5 -4 8.69 1.26 15 5 -3 5.54 1.02 15 5 -2 10.33 1.34 15 5 -1 1.59 0.56 15 5 0 9.88 1.22 15 5 1 14.91 1.37 15 5 2 4.27 0.73 -15 6 13 5.28 0.85 15 6 -13 7.77 0.87 -15 6 12 -0.18 0.50 -15 -6 12 -0.24 0.45 15 6 -12 0.48 0.36 -15 6 11 -0.49 0.62 15 6 -11 0.14 0.40 -15 6 10 0.78 0.67 15 6 -10 -0.08 0.43 -15 6 9 14.18 1.68 15 6 -9 15.08 1.51 -15 6 8 1.63 0.63 15 6 -8 3.25 0.79 -15 6 7 13.24 1.66 15 6 -7 15.25 1.59 -15 6 6 3.13 0.82 15 6 -6 4.25 0.91 15 6 -5 37.92 2.51 15 6 -4 87.78 3.81 15 6 -3 -0.47 0.61 15 6 -2 0.27 0.43 15 6 -1 -0.52 0.47 15 6 0 18.36 1.53 15 6 1 5.49 0.82 15 6 2 10.48 0.97 -15 7 12 1.56 0.60 15 7 -12 1.85 0.51 -15 7 11 10.75 1.36 15 7 -11 13.95 1.23 -15 7 10 0.54 0.52 15 7 -10 0.60 0.45 -15 7 9 2.45 0.79 15 7 -9 0.90 0.48 -15 7 8 2.83 0.84 15 7 -8 3.29 0.77 -15 7 7 4.16 0.94 15 7 -7 4.66 0.86 15 7 -6 0.91 0.52 15 7 -5 20.14 1.70 15 7 -4 0.12 0.41 15 7 -3 -0.09 0.45 15 7 -2 17.08 1.49 15 7 -1 0.15 0.36 15 7 0 1.26 0.45 -15 8 11 1.77 0.59 -15 8 10 28.44 2.07 15 8 -10 33.68 1.79 -15 8 9 4.53 0.93 15 8 -9 5.85 0.81 15 8 -8 0.49 0.38 15 8 -7 15.62 1.37 15 8 -6 0.46 0.41 15 8 -5 -0.05 0.43 -15 8 4 1.29 0.54 15 8 -4 0.00 0.33 15 8 -3 9.40 1.04 -15 8 3 8.31 0.85 -15 8 2 3.35 0.58 15 8 -2 1.75 0.51 15 8 -1 1.67 0.46 15 9 -6 7.16 0.83 15 9 -5 2.49 0.53 -16 0 12 30.38 2.01 16 0 -12 34.48 1.82 -16 0 11 0.33 0.49 16 0 -11 0.37 0.34 -16 0 10 3.14 0.77 16 0 -10 2.95 0.68 16 0 -9 0.11 0.41 16 0 -8 6.14 0.96 16 0 -7 0.78 0.56 16 0 -6 46.23 2.60 16 0 -5 -0.11 0.39 16 0 -4 33.52 2.16 16 0 -3 -0.09 0.38 16 0 -2 1.19 0.46 16 0 -1 0.02 0.36 16 0 0 0.44 0.36 -16 1 13 3.95 0.74 -16 1 12 1.27 0.53 -16 -1 12 1.14 0.52 16 1 -12 1.28 0.45 -16 1 11 25.48 1.95 -16 -1 11 25.41 1.85 16 -1 -11 27.24 1.68 16 1 -11 28.75 1.85 -16 1 10 15.19 1.52 -16 -1 10 13.10 1.36 16 -1 -10 12.54 1.22 16 1 -10 12.84 1.30 -16 1 9 7.07 1.07 16 -1 -9 7.95 1.00 16 1 -9 8.20 1.09 16 -1 -8 0.21 0.41 16 1 -8 0.87 0.50 16 -1 -7 26.47 1.89 16 1 -7 26.69 2.00 16 -1 -6 2.07 0.58 16 1 -6 2.44 0.71 16 -1 -5 1.46 0.58 16 1 -5 2.84 0.73 16 -1 -4 1.31 0.53 16 1 -4 2.25 0.66 16 -1 -3 3.29 0.76 16 1 -3 3.94 0.81 16 -1 -2 4.33 0.76 16 1 -2 4.63 0.83 16 -1 -1 0.83 0.42 16 1 -1 0.02 0.36 16 -1 0 5.02 0.70 16 1 0 5.29 0.77 16 1 1 13.51 1.09 -16 2 12 2.75 0.72 16 2 -12 2.57 0.58 -16 2 11 1.65 0.62 -16 -2 11 1.42 0.52 16 2 -11 2.74 0.67 -16 2 10 40.37 2.51 16 -2 -10 42.91 2.08 16 2 -10 46.90 2.46 -16 2 9 15.55 1.56 16 -2 -9 14.16 1.25 16 2 -9 14.38 1.42 16 -2 -8 7.78 0.97 16 2 -8 8.20 1.14 16 -2 -7 4.82 0.84 16 2 -7 3.61 0.81 16 -2 -6 32.93 2.02 16 2 -6 32.69 2.22 16 -2 -5 0.92 0.39 16 2 -5 1.22 0.58 16 -2 -4 5.09 0.82 16 2 -4 4.40 0.87 16 -2 -3 22.00 1.58 16 2 -3 22.27 1.76 16 -2 -2 -0.49 0.45 16 2 -2 -0.65 0.48 16 -2 -1 6.09 0.78 16 2 -1 6.96 0.97 16 2 0 -0.21 0.35 16 2 1 5.08 0.70 -16 3 12 28.80 1.95 16 3 -12 30.92 1.78 -16 3 11 0.08 0.43 16 3 -11 0.85 0.48 -16 3 10 1.85 0.67 16 3 -10 2.70 0.75 -16 3 9 1.41 0.56 16 3 -9 1.46 0.62 -16 3 8 14.83 1.47 16 3 -8 19.12 1.64 16 3 -7 2.51 0.75 16 3 -6 0.00 0.42 16 3 -5 0.46 0.42 16 3 -4 30.29 2.08 16 3 -3 -0.05 0.45 16 3 -2 -0.05 0.38 16 3 -1 9.29 1.06 16 3 0 12.87 1.15 -16 4 12 7.81 1.00 16 4 -12 7.78 0.86 -16 4 11 1.59 0.55 16 4 -11 2.32 0.58 -16 4 10 12.25 1.38 16 4 -10 14.13 1.32 -16 4 9 0.85 0.50 16 4 -9 1.05 0.52 -16 4 8 -0.17 0.50 16 4 -8 0.07 0.38 16 4 -7 0.30 0.42 16 4 -6 11.63 1.30 16 4 -5 7.10 1.05 16 4 -4 0.80 0.51 16 4 -3 5.03 0.84 16 4 -2 1.73 0.54 16 4 -1 3.55 0.65 16 4 0 0.19 0.34 -16 5 11 1.05 0.43 16 5 -11 1.55 0.48 -16 5 10 1.19 0.50 16 5 -10 2.86 0.59 -16 5 9 14.53 1.41 16 5 -9 16.92 1.40 -16 5 8 12.17 1.29 16 5 -8 14.19 1.32 16 5 -7 0.28 0.42 16 5 -6 0.93 0.46 16 5 -5 24.96 1.78 16 5 -4 13.73 1.32 16 5 -3 3.21 0.67 16 5 -2 6.45 0.86 16 5 -1 1.20 0.45 16 6 -10 -0.10 0.27 -16 6 9 0.69 0.41 16 6 -9 1.72 0.48 16 6 -8 -0.13 0.31 16 6 -7 18.38 1.44 16 6 -6 0.52 0.42 16 6 -5 2.66 0.62 16 6 -4 6.90 0.90 16 6 -3 12.48 1.13 16 6 -2 0.36 0.32 16 7 -8 17.23 1.24 16 7 -7 0.60 0.34 16 7 -6 4.46 0.67 16 7 -5 3.29 0.61 16 7 -4 1.50 0.45 17 0 -6 0.19 0.28 17 1 -8 1.20 0.42 17 1 -7 1.70 0.48 17 1 -6 4.67 0.71 17 1 -5 -0.47 0.31 17 1 -4 27.75 1.55 17 2 -8 0.75 0.37 17 2 -7 1.58 0.45 17 2 -6 2.95 0.58 17 2 -5 0.49 0.31 17 2 -4 4.16 0.63 17 3 -8 7.60 0.84 17 3 -7 1.79 0.47 17 3 -6 6.23 0.78 17 3 -5 12.35 1.05 0 0 0 0.00 0.00 TITL exp_684 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 13.906015 16.609394 16.559302 90.0000 108.1758 90.0000 ZERR 16.00 0.000216 0.000228 0.000248 0.0000 0.0016 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O UNIT 176.00 160.00 16.00 16.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 77057 _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 1.464 _oxdiff_exptl_absorpt_empirical_full_min 0.747 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn F2' F -0.27130(8) 0.61329(6) -0.13160(6) 0.0373(2) Uani 1 1 d . F1' F -0.33294(8) 0.53761(7) -0.05473(7) 0.0410(3) Uani 1 1 d . F3' F -0.31306(8) 0.66465(7) -0.02815(7) 0.0443(3) Uani 1 1 d . F2 F 0.81112(9) 0.11615(7) 0.30789(9) 0.0520(3) Uani 1 1 d . F1 F 0.85055(9) 0.23328(9) 0.36065(10) 0.0619(4) Uani 1 1 d . O1' O 0.15085(10) 0.09616(8) 0.59539(9) 0.0412(3) Uani 1 1 d . F3 F 0.81540(10) 0.21428(10) 0.22672(10) 0.0676(4) Uani 1 1 d . N1 N 0.12329(10) 0.48336(8) 0.24794(8) 0.0257(3) Uani 1 1 d . N1' N 0.33836(10) 0.28185(8) 0.31098(8) 0.0243(3) Uani 1 1 d . N2 N 0.20625(10) 0.56492(8) 0.17005(8) 0.0272(3) Uani 1 1 d . N2' N 0.30056(11) 0.20746(8) 0.18048(9) 0.0274(3) Uani 1 1 d . O1 O 0.12803(15) 0.58599(10) 0.64294(9) 0.0585(4) Uani 1 1 d . C16 C 0.12538(12) 0.53375(9) 0.18297(10) 0.0252(3) Uani 1 1 d . C1' C 0.21285(11) 0.33191(9) 0.37091(9) 0.0234(3) Uani 1 1 d . C2' C 0.19390(11) 0.27274(9) 0.43200(9) 0.0233(3) Uani 1 1 d . C9 C 0.21067(12) 0.46423(9) 0.30356(10) 0.0253(3) Uani 1 1 d . C1 C 0.20416(12) 0.41181(10) 0.37569(10) 0.0249(3) Uani 1 1 d . C16' C 0.36382(12) 0.24066(9) 0.24888(10) 0.0249(3) Uani 1 1 d . C10' C 0.16511(12) 0.26370(9) 0.22618(10) 0.0254(3) Uani 1 1 d . C17 C 0.02405(12) 0.55293(9) 0.12219(10) 0.0256(3) Uani 1 1 d . C9' C 0.24125(12) 0.29260(9) 0.29979(10) 0.0237(3) Uani 1 1 d . C15' C 0.20006(13) 0.21883(9) 0.16814(10) 0.0274(3) Uani 1 1 d . C3' C 0.10199(12) 0.26967(10) 0.44910(10) 0.0291(3) Uani 1 1 d . H3' H 0.051912 0.307207 0.424141 0.035 Uiso 1 1 calc R C17' C 0.47375(12) 0.23204(9) 0.26075(10) 0.0268(3) Uani 1 1 d . C10 C 0.30427(12) 0.49289(10) 0.29708(10) 0.0272(3) Uani 1 1 d . C15 C 0.29740(12) 0.54433(9) 0.22705(10) 0.0275(3) Uani 1 1 d . C7' C 0.26729(12) 0.21580(10) 0.46992(10) 0.0281(3) Uani 1 1 d . H7' H 0.328405 0.216195 0.458061 0.034 Uiso 1 1 calc R C20 C -0.16646(13) 0.58340(10) 0.00778(10) 0.0283(3) Uani 1 1 d . C2 C 0.18590(13) 0.45629(10) 0.44777(10) 0.0280(3) Uani 1 1 d . C22 C -0.06324(13) 0.53070(10) 0.14156(10) 0.0294(3) Uani 1 1 d . H22 H -0.057527 0.505463 0.192983 0.035 Uiso 1 1 calc R C19 C -0.08053(13) 0.60595(10) -0.01222(10) 0.0287(3) Uani 1 1 d . H19 H -0.086568 0.631128 -0.063729 0.034 Uiso 1 1 calc R C4 C 0.22582(13) 0.48216(11) 0.59876(11) 0.0323(4) Uani 1 1 d . H4 H 0.264614 0.470774 0.654370 0.039 Uiso 1 1 calc R C11' C 0.06007(13) 0.27569(10) 0.20980(10) 0.0290(3) Uani 1 1 d . H11' H 0.036723 0.305450 0.247468 0.035 Uiso 1 1 calc R C4' C 0.08399(13) 0.21136(11) 0.50289(11) 0.0318(4) Uani 1 1 d . H4' H 0.021912 0.209409 0.513029 0.038 Uiso 1 1 calc R C3 C 0.24095(12) 0.43959(10) 0.53134(10) 0.0295(3) Uani 1 1 d . H3 H 0.289267 0.398887 0.542717 0.035 Uiso 1 1 calc R C21 C -0.15752(13) 0.54593(10) 0.08507(11) 0.0310(3) Uani 1 1 d . H21 H -0.215274 0.531213 0.098457 0.037 Uiso 1 1 calc R C23 C -0.27004(14) 0.59968(10) -0.05170(11) 0.0329(4) Uani 1 1 d . C18 C 0.01431(13) 0.59078(9) 0.04489(10) 0.0273(3) Uani 1 1 d . H18 H 0.071939 0.605962 0.031566 0.033 Uiso 1 1 calc R C6' C 0.25125(13) 0.15881(11) 0.52473(11) 0.0312(3) Uani 1 1 d . H6' H 0.302013 0.122119 0.550634 0.037 Uiso 1 1 calc R C14' C 0.12880(14) 0.18590(11) 0.09468(11) 0.0326(4) Uani 1 1 d . H14' H 0.150752 0.156054 0.056260 0.039 Uiso 1 1 calc R C14 C 0.38748(13) 0.57424(10) 0.21516(11) 0.0316(3) Uani 1 1 d . H14 H 0.384271 0.608055 0.169633 0.038 Uiso 1 1 calc R C22' C 0.50547(14) 0.19699(11) 0.19651(11) 0.0328(4) Uani 1 1 d . H22' H 0.457684 0.180770 0.146098 0.039 Uiso 1 1 calc R C5' C 0.15929(13) 0.15598(10) 0.54144(10) 0.0295(3) Uani 1 1 d . C11 C 0.39997(13) 0.47225(10) 0.35391(11) 0.0318(4) Uani 1 1 d . H11 H 0.404625 0.438882 0.400079 0.038 Uiso 1 1 calc R C13 C 0.47910(14) 0.55306(11) 0.27107(12) 0.0360(4) Uani 1 1 d . H13 H 0.538022 0.572896 0.263086 0.043 Uiso 1 1 calc R C20' C 0.67883(14) 0.21100(10) 0.28240(12) 0.0337(4) Uani 1 1 d . C12' C -0.00729(13) 0.24325(11) 0.13810(11) 0.0337(4) Uani 1 1 d . H12' H -0.076396 0.250986 0.127362 0.040 Uiso 1 1 calc R C18' C 0.54621(13) 0.25814(10) 0.33493(11) 0.0315(4) Uani 1 1 d . H18' H 0.525853 0.282926 0.377268 0.038 Uiso 1 1 calc R C13' C 0.02767(14) 0.19817(11) 0.08053(11) 0.0358(4) Uani 1 1 d . H13' H -0.018847 0.176499 0.032226 0.043 Uiso 1 1 calc R C19' C 0.64873(13) 0.24744(11) 0.34620(12) 0.0346(4) Uani 1 1 d . H19' H 0.696831 0.264536 0.396043 0.042 Uiso 1 1 calc R C21' C 0.60739(14) 0.18630(11) 0.20744(12) 0.0362(4) Uani 1 1 d . H21' H 0.627999 0.162613 0.164684 0.043 Uiso 1 1 calc R C12 C 0.48627(13) 0.50170(11) 0.34070(12) 0.0368(4) Uani 1 1 d . H12 H 0.549458 0.487774 0.377675 0.044 Uiso 1 1 calc R C5 C 0.15225(18) 0.54179(12) 0.58218(12) 0.0428(5) Uani 1 1 d . C23' C 0.78824(15) 0.19454(12) 0.29465(13) 0.0404(4) Uani 1 1 d . C7 C 0.11297(19) 0.51686(13) 0.43240(12) 0.0524(6) Uani 1 1 d . H7 H 0.075710 0.529334 0.376660 0.063 Uiso 1 1 calc R C8 C 0.1944(2) 0.57967(13) 0.72734(12) 0.0502(5) Uani 1 1 d . H8A H 0.261972 0.592867 0.728402 0.075 Uiso 1 1 calc GR H8B H 0.192947 0.525598 0.747428 0.075 Uiso 1 1 calc GR H8C H 0.173127 0.616249 0.763330 0.075 Uiso 1 1 calc GR C8' C 0.05351(18) 0.08388(15) 0.60461(18) 0.0576(6) Uani 1 1 d . H8'A H 0.004458 0.076904 0.549564 0.086 Uiso 1 1 calc GR H8'B H 0.035590 0.129785 0.632098 0.086 Uiso 1 1 calc GR H8'C H 0.054845 0.036659 0.638373 0.086 Uiso 1 1 calc GR C6 C 0.0950(2) 0.55869(15) 0.49833(14) 0.0627(7) Uani 1 1 d . H6 H 0.044899 0.597992 0.486924 0.075 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 F2' 0.0431(6) 0.0362(5) 0.0287(5) 0.0036(4) 0.0057(4) 0.0019(4) F1' 0.0327(5) 0.0430(6) 0.0433(6) 0.0034(5) 0.0060(4) -0.0057(5) F3' 0.0399(6) 0.0455(6) 0.0440(6) -0.0067(5) 0.0080(5) 0.0120(5) F2 0.0398(6) 0.0419(6) 0.0810(9) 0.0077(6) 0.0284(6) 0.0130(5) F1 0.0312(6) 0.0659(8) 0.0883(10) -0.0197(7) 0.0183(6) -0.0018(6) O1' 0.0412(7) 0.0423(7) 0.0476(7) 0.0181(6) 0.0248(6) 0.0047(6) F3 0.0481(7) 0.0933(11) 0.0784(10) 0.0322(8) 0.0444(7) 0.0170(7) N1 0.0309(7) 0.0232(6) 0.0248(6) -0.0006(5) 0.0112(5) -0.0011(5) N1' 0.0273(6) 0.0223(6) 0.0261(6) 0.0020(5) 0.0123(5) 0.0022(5) N2 0.0328(7) 0.0233(6) 0.0280(6) -0.0008(5) 0.0131(5) -0.0025(5) N2' 0.0331(7) 0.0242(6) 0.0284(7) -0.0003(5) 0.0146(5) 0.0013(5) O1 0.0932(13) 0.0522(9) 0.0339(7) -0.0044(6) 0.0251(8) 0.0265(9) C16 0.0316(8) 0.0213(7) 0.0249(7) -0.0016(6) 0.0119(6) -0.0003(6) C1' 0.0224(7) 0.0249(7) 0.0241(7) 0.0012(6) 0.0088(5) 0.0030(6) C2' 0.0257(7) 0.0229(7) 0.0225(7) -0.0011(6) 0.0093(6) 0.0011(6) C9 0.0317(8) 0.0200(7) 0.0256(7) -0.0025(6) 0.0112(6) 0.0010(6) C1 0.0249(7) 0.0259(8) 0.0258(7) 0.0014(6) 0.0104(6) 0.0025(6) C16' 0.0311(8) 0.0206(7) 0.0259(7) 0.0033(6) 0.0130(6) 0.0024(6) C10' 0.0301(8) 0.0227(7) 0.0254(7) 0.0024(6) 0.0114(6) -0.0004(6) C17 0.0321(8) 0.0211(7) 0.0253(7) -0.0011(6) 0.0113(6) 0.0006(6) C9' 0.0294(8) 0.0195(7) 0.0248(7) 0.0035(6) 0.0122(6) 0.0013(6) C15' 0.0352(8) 0.0228(7) 0.0269(7) 0.0016(6) 0.0137(6) -0.0006(6) C3' 0.0254(8) 0.0321(8) 0.0310(8) 0.0039(7) 0.0103(6) 0.0058(6) C17' 0.0310(8) 0.0227(7) 0.0308(8) 0.0046(6) 0.0156(6) 0.0046(6) C10 0.0319(8) 0.0228(7) 0.0295(8) -0.0031(6) 0.0132(6) -0.0011(6) C15 0.0314(8) 0.0231(7) 0.0302(8) -0.0036(6) 0.0129(6) -0.0004(6) C7' 0.0259(7) 0.0310(8) 0.0300(8) 0.0034(6) 0.0123(6) 0.0040(6) C20 0.0318(8) 0.0246(8) 0.0286(8) -0.0027(6) 0.0094(6) 0.0013(6) C2 0.0351(8) 0.0238(8) 0.0279(8) 0.0007(6) 0.0141(6) 0.0009(6) C22 0.0335(8) 0.0302(8) 0.0272(7) 0.0027(6) 0.0136(6) 0.0005(7) C19 0.0373(9) 0.0249(8) 0.0259(7) 0.0009(6) 0.0126(6) -0.0008(7) C4 0.0361(9) 0.0344(9) 0.0270(8) -0.0015(7) 0.0107(6) -0.0037(7) C11' 0.0298(8) 0.0305(8) 0.0286(8) 0.0021(6) 0.0118(6) 0.0007(7) C4' 0.0266(8) 0.0380(9) 0.0343(8) 0.0035(7) 0.0144(7) 0.0008(7) C3 0.0291(8) 0.0295(8) 0.0305(8) -0.0014(6) 0.0103(6) 0.0005(7) C21 0.0310(8) 0.0321(8) 0.0329(8) 0.0010(7) 0.0144(7) -0.0001(7) C23 0.0349(9) 0.0302(8) 0.0339(8) -0.0006(7) 0.0114(7) 0.0018(7) C18 0.0330(8) 0.0233(7) 0.0285(8) 0.0000(6) 0.0137(6) -0.0020(6) C6' 0.0299(8) 0.0327(9) 0.0326(8) 0.0070(7) 0.0124(6) 0.0060(7) C14' 0.0395(9) 0.0311(8) 0.0299(8) -0.0042(7) 0.0147(7) -0.0038(7) C14 0.0355(9) 0.0280(8) 0.0351(8) -0.0008(7) 0.0163(7) -0.0032(7) C22' 0.0356(9) 0.0354(9) 0.0313(8) 0.0008(7) 0.0163(7) 0.0036(7) C5' 0.0340(8) 0.0282(8) 0.0288(8) 0.0041(6) 0.0136(6) -0.0006(7) C11 0.0329(8) 0.0272(8) 0.0354(8) 0.0005(7) 0.0105(7) 0.0004(7) C13 0.0324(8) 0.0337(9) 0.0457(10) -0.0051(8) 0.0177(7) -0.0058(7) C20' 0.0325(9) 0.0305(8) 0.0436(9) 0.0074(7) 0.0199(7) 0.0041(7) C12' 0.0298(8) 0.0379(9) 0.0342(8) 0.0030(7) 0.0109(7) -0.0026(7) C18' 0.0334(8) 0.0313(8) 0.0336(8) 0.0000(7) 0.0161(7) 0.0041(7) C13' 0.0377(9) 0.0383(9) 0.0298(8) -0.0016(7) 0.0080(7) -0.0090(8) C19' 0.0307(8) 0.0352(9) 0.0390(9) 0.0006(7) 0.0126(7) 0.0015(7) C21' 0.0386(9) 0.0383(9) 0.0393(9) 0.0024(8) 0.0232(8) 0.0094(8) C12 0.0296(8) 0.0349(9) 0.0442(10) -0.0007(8) 0.0088(7) -0.0005(7) C5 0.0665(13) 0.0355(10) 0.0316(9) -0.0031(7) 0.0230(9) 0.0107(9) C23' 0.0352(9) 0.0391(10) 0.0527(11) 0.0045(8) 0.0221(8) 0.0023(8) C7 0.0779(15) 0.0509(12) 0.0293(9) 0.0055(8) 0.0180(9) 0.0336(11) C8 0.0804(16) 0.0439(11) 0.0337(10) -0.0068(8) 0.0285(10) -0.0043(11) C8' 0.0510(12) 0.0574(13) 0.0780(16) 0.0293(12) 0.0398(12) 0.0037(11) C6 0.0970(19) 0.0574(14) 0.0362(10) 0.0050(10) 0.0242(11) 0.0465(14) 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 C5' O1' C8' 116.94(15) C9 N1 C16 117.15(14) C9' N1' C16' 117.11(14) C16 N2 C15 116.44(14) C16' N2' C15' 116.72(14) C5 O1 C8 116.80(17) N1 C16 C17 114.47(14) N2 C16 N1 126.64(15) N2 C16 C17 118.89(14) C2' C1' C9' 112.98(13) C1 C1' C2' 125.12(14) C1 C1' C9' 121.88(14) C3' C2' C1' 121.95(14) C7' C2' C1' 119.64(13) C7' C2' C3' 118.31(14) N1 C9 C1 115.15(14) N1 C9 C10 122.31(14) C10 C9 C1 122.52(14) C1' C1 C9 119.92(14) C1' C1 C2 125.46(14) C2 C1 C9 114.61(13) N1' C16' C17' 116.41(14) N2' C16' N1' 126.44(15) N2' C16' C17' 117.15(14) C15' C10' C9' 115.89(14) C11' C10' C9' 124.32(14) C11' C10' C15' 119.77(15) C22 C17 C16 119.66(14) C18 C17 C16 121.18(14) C18 C17 C22 119.14(15) N1' C9' C1' 117.20(14) N1' C9' C10' 122.03(14) C10' C9' C1' 120.64(13) N2' C15' C10' 121.64(15) N2' C15' C14' 119.06(15) C14' C15' C10' 119.29(15) C2' C3' H3' 119.5 C4' C3' C2' 121.03(15) C4' C3' H3' 119.5 C22' C17' C16' 119.66(15) C18' C17' C16' 121.19(14) C18' C17' C22' 119.15(15) C15 C10 C9 115.69(15) C11 C10 C9 124.30(15) C11 C10 C15 120.00(15) N2 C15 C10 121.76(15) N2 C15 C14 119.07(15) C14 C15 C10 119.16(16) C2' C7' H7' 119.4 C6' C7' C2' 121.23(15) C6' C7' H7' 119.4 C19 C20 C21 120.21(16) C19 C20 C23 121.25(15) C21 C20 C23 118.53(15) C3 C2 C1 121.44(15) C3 C2 C7 118.09(16) C7 C2 C1 120.46(15) C17 C22 H22 119.8 C21 C22 C17 120.45(15) C21 C22 H22 119.8 C20 C19 H19 120.2 C18 C19 C20 119.70(15) C18 C19 H19 120.2 C3 C4 H4 120.3 C3 C4 C5 119.36(16) C5 C4 H4 120.3 C10' C11' H11' 120.1 C12' C11' C10' 119.73(15) C12' C11' H11' 120.1 C3' C4' H4' 120.2 C3' C4' C5' 119.65(15) C5' C4' H4' 120.2 C2 C3 C4 121.68(16) C2 C3 H3 119.2 C4 C3 H3 119.2 C20 C21 H21 120.0 C22 C21 C20 119.98(15) C22 C21 H21 120.0 F2' C23 F1' 106.59(14) F2' C23 F3' 106.30(14) F2' C23 C20 113.27(14) F1' C23 F3' 106.42(14) F1' C23 C20 111.62(14) F3' C23 C20 112.17(14) C17 C18 H18 119.7 C19 C18 C17 120.53(15) C19 C18 H18 119.7 C7' C6' H6' 119.9 C7' C6' C5' 120.16(15) C5' C6' H6' 119.9 C15' C14' H14' 120.1 C13' C14' C15' 119.75(16) C13' C14' H14' 120.1 C15 C14 H14 120.2 C13 C14 C15 119.56(16) C13 C14 H14 120.2 C17' C22' H22' 119.8 C21' C22' C17' 120.47(17) C21' C22' H22' 119.8 O1' C5' C4' 125.15(15) O1' C5' C6' 115.25(15) C4' C5' C6' 119.59(15) C10 C11 H11 120.1 C12 C11 C10 119.70(16) C12 C11 H11 120.1 C14 C13 H13 119.3 C14 C13 C12 121.45(16) C12 C13 H13 119.3 C19' C20' C23' 120.72(18) C21' C20' C19' 120.46(16) C21' C20' C23' 118.77(16) C11' C12' H12' 119.8 C11' C12' C13' 120.42(16) C13' C12' H12' 119.8 C17' C18' H18' 119.7 C19' C18' C17' 120.53(16) C19' C18' H18' 119.7 C14' C13' C12' 121.04(16) C14' C13' H13' 119.5 C12' C13' H13' 119.5 C20' C19' H19' 120.2 C18' C19' C20' 119.52(17) C18' C19' H19' 120.2 C22' C21' C20' 119.84(16) C22' C21' H21' 120.1 C20' C21' H21' 120.1 C11 C12 C13 120.12(17) C11 C12 H12 119.9 C13 C12 H12 119.9 O1 C5 C4 124.89(18) O1 C5 C6 115.34(18) C4 C5 C6 119.75(17) F2 C23' C20' 112.25(15) F1 C23' F2 105.94(17) F1 C23' F3 106.90(17) F1 C23' C20' 113.42(16) F3 C23' F2 105.14(16) F3 C23' C20' 112.59(17) C2 C7 H7 119.4 C6 C7 C2 121.29(18) C6 C7 H7 119.4 O1 C8 H8A 109.5 O1 C8 H8B 109.5 O1 C8 H8C 109.5 H8A C8 H8B 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 O1' C8' H8'A 109.5 O1' C8' H8'B 109.5 O1' C8' H8'C 109.5 H8'A C8' H8'B 109.5 H8'A C8' H8'C 109.5 H8'B C8' H8'C 109.5 C5 C6 H6 120.1 C7 C6 C5 119.81(19) C7 C6 H6 120.1 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance F2' C23 1.337(2) F1' C23 1.343(2) F3' C23 1.349(2) F2 C23' 1.342(2) F1 C23' 1.330(3) O1' C5' 1.365(2) O1' C8' 1.423(2) F3 C23' 1.334(2) N1 C16 1.371(2) N1 C9 1.314(2) N1' C16' 1.370(2) N1' C9' 1.317(2) N2 C16 1.315(2) N2 C15 1.367(2) N2' C16' 1.319(2) N2' C15' 1.361(2) O1 C5 1.370(2) O1 C8 1.418(3) C16 C17 1.488(2) C1' C2' 1.492(2) C1' C1 1.337(2) C1' C9' 1.503(2) C2' C3' 1.394(2) C2' C7' 1.389(2) C9 C1 1.504(2) C9 C10 1.421(2) C1 C2 1.491(2) C16' C17' 1.486(2) C10' C9' 1.426(2) C10' C15' 1.417(2) C10' C11' 1.414(2) C17 C22 1.398(2) C17 C18 1.394(2) C15' C14' 1.417(2) C3' H3' 0.9300 C3' C4' 1.390(2) C17' C22' 1.399(2) C17' C18' 1.393(2) C10 C15 1.419(2) C10 C11 1.412(2) C15 C14 1.417(2) C7' H7' 0.9300 C7' C6' 1.377(2) C20 C19 1.387(2) C20 C21 1.393(2) C20 C23 1.494(2) C2 C3 1.385(2) C2 C7 1.394(3) C22 H22 0.9300 C22 C21 1.376(2) C19 H19 0.9300 C19 C18 1.385(2) C4 H4 0.9300 C4 C3 1.392(2) C4 C5 1.388(3) C11' H11' 0.9300 C11' C12' 1.372(2) C4' H4' 0.9300 C4' C5' 1.390(2) C3 H3 0.9300 C21 H21 0.9300 C18 H18 0.9300 C6' H6' 0.9300 C6' C5' 1.391(2) C14' H14' 0.9300 C14' C13' 1.367(3) C14 H14 0.9300 C14 C13 1.367(3) C22' H22' 0.9300 C22' C21' 1.383(3) C11 H11 0.9300 C11 C12 1.375(2) C13 H13 0.9300 C13 C12 1.413(3) C20' C19' 1.391(3) C20' C21' 1.388(3) C20' C23' 1.496(2) C12' H12' 0.9300 C12' C13' 1.413(3) C18' H18' 0.9300 C18' C19' 1.390(2) C13' H13' 0.9300 C19' H19' 0.9300 C21' H21' 0.9300 C12 H12 0.9300 C5 C6 1.397(3) C7 H7 0.9300 C7 C6 1.381(3) C8 H8A 0.9600 C8 H8B 0.9600 C8 H8C 0.9600 C8' H8'A 0.9600 C8' H8'B 0.9600 C8' H8'C 0.9600 C6 H6 0.9300