#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:24:50 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227259 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035839.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_4035839 loop_ _publ_author_name 'Kumar, Siripuram Vijay' 'Acharya, Anand' 'Ila, Hiriyakkanavar' _publ_section_title ; Synthesis of 2,4,5-Trisubstituted Oxazoles with Complementary Regioselectivity from \a-Oxoketene Dithioacetals and \b-(Methylthio)-\b-(het)aryl-2-propenones. ; _journal_issue 12 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 6607 _journal_page_last 6622 _journal_paper_doi 10.1021/acs.joc.8b00900 _journal_volume 83 _journal_year 2018 _chemical_formula_moiety 'C22 H14 F3 N O4' _chemical_formula_sum 'C22 H14 F3 N O4' _chemical_formula_weight 413.34 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2016-06-23 _audit_creation_method ; Olex2 1.2 (compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155) ; _cell_angle_alpha 90 _cell_angle_beta 114.419(7) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 32.547(2) _cell_length_b 4.2555(2) _cell_length_c 30.3660(19) _cell_measurement_reflns_used 2835 _cell_measurement_temperature 298 _cell_measurement_theta_max 20.727 _cell_measurement_theta_min 2.394 _cell_volume 3829.6(4) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _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 'SIR2004 (Burla et al., 2007)' _diffrn_ambient_temperature 298.0 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1623 _diffrn_reflns_av_unetI/netI 0.0731 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 31871 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.378 _diffrn_reflns_theta_max 25.378 _diffrn_reflns_theta_min 2.395 _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.6296 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0765 before and 0.0577 after correction. The Ratio of minimum to maximum transmission is 0.8449. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.434 _exptl_crystal_description needle _exptl_crystal_F_000 1696 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.178 _refine_diff_density_min -0.155 _refine_diff_density_rms 0.036 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 299 _refine_ls_number_reflns 3498 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.1771 _refine_ls_R_factor_gt 0.0775 _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^)+(0.0559P)^2^+4.7271P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1544 _refine_ls_wR_factor_ref 0.1900 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1630 _reflns_number_total 3498 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b00900_si_002.cif _cod_data_source_block compound_5j _cod_original_cell_volume 3829.5(4) _cod_database_code 4035839 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Fixed Sof: F1AA(0.5) F2(0.5) F2AA(0.5) F1(0.5) F0AA(0.5) F3(0.5) 3.a Aromatic/amide H refined with riding coordinates: C00B(H00B), C00C(H00C), C00E(H00E), C00F(H00F), C00G(H00G), C00I(H00I), C00K(H00K), C00L(H00L), C00M(H00M), C00R(H00R), C00V(H00V) 3.b Idealised Me refined as rotating group: C00U(H00A,H00D,H00H) ; _shelx_res_file ; svk589_a.res created by SHELXL-2014/7 TITL SVK589_a.res in C2/c CELL 0.71073 32.5467 4.2555 30.366 90 114.419 90 ZERR 8 0.0021 0.0002 0.0019 0 0.007 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H F N O UNIT 176 112 24 8 32 L.S. 40 PLAN 20 TEMP 24.85 BOND $H LIST 6 MORE -1 CONF fmap 2 acta 52 MERG 2 REM REM REM WGHT 0.055900 4.727100 FVAR 0.38708 O2 5 0.374710 0.493642 0.457973 11.00000 0.05830 0.08749 = 0.06910 -0.00276 0.03188 -0.00086 O3 5 0.294672 0.173220 0.499423 11.00000 0.06000 0.10993 = 0.06804 0.00103 0.03156 -0.00709 N003 4 0.299957 0.514754 0.420303 11.00000 0.06060 0.09428 = 0.05371 -0.00798 0.02401 -0.01324 C004 1 0.333692 0.415011 0.457576 11.00000 0.05718 0.07961 = 0.06016 -0.01222 0.03154 -0.01054 O005 5 0.304809 0.838025 0.314451 11.00000 0.07247 0.32081 = 0.06702 0.03146 0.02576 -0.03310 C1 1 0.335277 0.232701 0.497945 11.00000 0.05879 0.07618 = 0.06885 -0.01268 0.03586 -0.00564 C007 1 0.364767 0.657355 0.415690 11.00000 0.06681 0.08575 = 0.05506 -0.00919 0.02926 -0.00774 C008 1 0.318705 0.668359 0.392346 11.00000 0.06267 0.09498 = 0.05341 -0.00678 0.02723 -0.01560 O1 5 0.521183 1.076979 0.399823 11.00000 0.06292 0.21747 = 0.15192 0.06591 0.04966 0.00239 C00A 1 0.240805 0.846568 0.331007 11.00000 0.06161 0.10358 = 0.05602 0.00305 0.01681 -0.02322 C00B 1 0.223802 0.956388 0.362782 11.00000 0.08165 0.08766 = 0.06218 -0.01134 0.02677 -0.01746 AFIX 43 H00B 2 0.242938 0.980167 0.395305 11.00000 -1.20000 AFIX 0 C00C 1 0.368546 0.106457 0.536165 11.00000 0.06075 0.10551 = 0.08002 0.00938 0.03390 0.00964 AFIX 43 H00C 2 0.399228 0.115991 0.543470 11.00000 -1.20000 AFIX 0 C00D 1 0.404119 0.770710 0.409399 11.00000 0.05515 0.09006 = 0.06760 0.00084 0.02877 -0.00015 C00E 1 0.348189 -0.045229 0.563564 11.00000 0.08380 0.10618 = 0.07844 0.01436 0.03857 0.01788 AFIX 43 H00E 2 0.362842 -0.155915 0.592257 11.00000 -1.20000 AFIX 0 C00F 1 0.304413 0.001199 0.540434 11.00000 0.08365 0.10881 = 0.06974 0.01064 0.04108 -0.00637 AFIX 43 H00F 2 0.282976 -0.073439 0.550706 11.00000 -1.20000 AFIX 0 C00G 1 0.179266 1.030602 0.347117 11.00000 0.09321 0.07534 = 0.09177 -0.00692 0.04191 -0.00878 AFIX 43 H00G 2 0.168469 1.109043 0.368907 11.00000 -1.20000 AFIX 0 C00H 1 0.289287 0.788655 0.344160 11.00000 0.07468 0.15265 = 0.05625 0.00308 0.02787 -0.02664 C00I 1 0.166403 0.878260 0.267700 11.00000 0.06807 0.15384 = 0.06655 -0.00341 0.01526 -0.02273 AFIX 43 H00I 2 0.146727 0.849445 0.235467 11.00000 -1.20000 AFIX 0 C00J 1 0.150299 0.990883 0.299687 11.00000 0.07362 0.08297 = 0.08139 0.01179 0.02668 -0.00867 C00K 1 0.211238 0.807338 0.282615 11.00000 0.07825 0.15788 = 0.05542 -0.00707 0.02788 -0.02074 AFIX 43 H00K 2 0.221918 0.733167 0.260490 11.00000 -1.20000 AFIX 0 C00L 1 0.402223 0.930164 0.369646 11.00000 0.05735 0.15573 = 0.09469 0.03399 0.03050 -0.00501 AFIX 43 H00L 2 0.374078 0.969233 0.344786 11.00000 -1.20000 AFIX 0 C00M 1 0.446217 0.723081 0.445017 11.00000 0.06753 0.19527 = 0.11475 0.07114 0.03686 0.00269 AFIX 43 H00M 2 0.449138 0.617195 0.472951 11.00000 -1.20000 AFIX 0 C00O 1 0.481266 0.981083 0.400117 11.00000 0.05911 0.13918 = 0.11127 0.03342 0.04765 0.00339 C00R 1 0.440024 1.036073 0.364578 11.00000 0.06648 0.16189 = 0.10508 0.04635 0.04055 0.00138 AFIX 43 H00R 2 0.437165 1.144670 0.336880 11.00000 -1.20000 AFIX 0 C00U 1 0.519843 1.237659 0.358294 11.00000 0.09761 0.23247 = 0.17334 0.08620 0.08349 0.00256 AFIX 137 H00A 2 0.507416 1.101722 0.330664 11.00000 -1.50000 H00D 2 0.549868 1.298156 0.363293 11.00000 -1.50000 H00H 2 0.501339 1.421787 0.352834 11.00000 -1.50000 AFIX 0 C00V 1 0.484632 0.827597 0.440789 11.00000 0.05699 0.23940 = 0.14043 0.09346 0.03166 0.00915 AFIX 43 H00V 2 0.512844 0.792961 0.465794 11.00000 -1.20000 AFIX 0 C3 1 0.101572 1.074162 0.283898 11.00000 0.08958 0.07894 = 0.15390 0.02141 0.03410 -0.00608 PART 2 F1AA 3 0.085185 1.088101 0.311142 10.50000 0.08692 0.29038 = 0.12231 0.00503 0.05728 0.00941 F2 3 0.092442 1.333153 0.252328 10.50000 0.12041 0.14584 = 0.19726 0.06811 0.03421 0.01107 F2AA 3 0.074786 0.860172 0.244765 10.50000 0.08598 0.17341 = 0.17243 -0.03491 -0.00155 -0.01343 PART 0 PART 1 F1 3 0.081134 0.853647 0.299547 10.50000 0.12174 0.18189 = 0.29801 0.02423 0.12019 -0.00552 F0AA 3 0.098021 1.331803 0.311105 10.50000 0.12313 0.15491 = 0.16211 -0.00673 0.04114 0.04280 F3 3 0.079109 1.116616 0.243027 10.50000 0.08342 0.24605 = 0.10422 -0.00789 0.01785 0.02073 HKLF 4 REM SVK589_a.res in C2/c REM R1 = 0.0775 for 1630 Fo > 4sig(Fo) and 0.1771 for all 3498 data REM 299 parameters refined using 0 restraints END WGHT 0.0559 4.7270 REM Highest difference peak 0.178, deepest hole -0.155, 1-sigma level 0.036 Q1 1 0.3115 1.0692 0.3397 11.00000 0.05 0.18 Q2 1 0.2923 0.8780 0.2890 11.00000 0.05 0.14 Q3 1 0.2319 0.5698 0.2596 11.00000 0.05 0.14 Q4 1 0.3411 0.8555 0.4097 11.00000 0.05 0.13 Q5 1 0.2451 -0.0216 0.5280 11.00000 0.05 0.13 Q6 1 0.5322 1.1072 0.4383 11.00000 0.05 0.12 Q7 1 0.2309 1.0225 0.2997 11.00000 0.05 0.12 Q8 1 0.3771 0.0247 0.6388 11.00000 0.05 0.11 Q9 1 0.1629 1.2881 0.3188 11.00000 0.05 0.11 Q10 1 0.4343 0.9566 0.3208 11.00000 0.05 0.11 Q11 1 0.4921 0.7458 0.2892 11.00000 0.05 0.11 Q12 1 0.2281 0.3302 0.2943 11.00000 0.05 0.11 Q13 1 0.0340 1.0027 0.2005 11.00000 0.05 0.11 Q14 1 0.2681 -0.1152 0.4890 11.00000 0.05 0.11 Q15 1 0.3081 -0.1604 0.4822 11.00000 0.05 0.10 Q16 1 0.2604 1.1779 0.3294 11.00000 0.05 0.10 Q17 1 0.0692 0.6013 0.2324 11.00000 0.05 0.10 Q18 1 0.4586 0.4232 0.4497 11.00000 0.05 0.10 Q19 1 0.5082 0.5488 0.4515 11.00000 0.05 0.10 Q20 1 0.4923 1.6829 0.3212 11.00000 0.05 0.10 ; _shelx_res_checksum 93275 _shelx_hkl_file ; -3 -1 2 179.48 6.60 -3 -1 2 179.98 6.80 -3 -1 2 188.28 9.10 -3 -1 2 188.48 10.30 -3 -1 2 192.18 7.40 3 1 -2 176.18 7.10 3 1 -2 192.48 10.30 3 1 -2 187.58 8.80 -6 -2 4 25.10 8.40 -6 -2 4 36.80 5.10 -6 -2 4 35.00 6.70 -6 -2 4 46.90 5.80 -6 -2 4 40.00 10.70 6 2 -4 46.00 10.90 6 2 -4 32.60 5.70 6 2 -4 34.90 7.60 6 2 -4 33.30 5.40 -9 -3 6 73.79 8.00 -9 -3 6 59.49 14.60 -9 -3 6 30.80 12.50 -9 -3 6 53.59 9.80 -9 -3 6 66.59 7.60 9 3 -6 61.59 8.80 9 3 -6 59.39 12.60 9 3 -6 57.99 15.80 9 3 -6 58.59 8.50 -12 -4 8 5.20 11.60 -12 -4 8 15.00 25.50 12 4 -8 31.70 11.10 12 4 -8 2.50 12.40 10 4 -7 -5.80 9.80 10 4 -7 18.50 9.00 10 4 -7 12.10 15.90 -10 -4 7 30.10 23.80 -10 -4 7 8.50 12.10 7 3 -5 88.79 18.70 7 3 -5 86.49 9.60 7 3 -5 81.59 13.30 7 3 -5 73.49 8.80 -7 -3 5 85.79 10.90 -7 -3 5 85.59 14.90 4 2 -3 -0.20 7.00 4 2 -3 7.90 8.40 4 2 -3 0.50 3.40 4 2 -3 -3.70 3.30 -4 -2 3 -2.30 6.30 -4 -2 3 5.80 8.60 -4 -2 3 3.40 2.90 -4 -2 3 6.30 3.20 -4 -2 3 1.90 6.10 1 1 -1 42.00 3.40 1 1 -1 42.30 3.40 1 1 -1 54.69 7.30 1 1 -1 45.80 5.80 -1 -1 1 37.50 2.60 -1 -1 1 35.80 5.60 -1 -1 1 41.20 4.60 -1 -1 1 39.70 2.60 -1 -1 1 42.20 5.70 -5 -1 3 -0.40 3.10 -5 -1 3 1.30 2.90 -5 -1 3 -4.80 3.10 -5 -1 3 6.10 4.10 -5 -1 3 3.60 4.40 5 1 -3 -2.20 3.30 5 1 -3 -1.10 3.50 5 1 -3 11.70 4.00 5 1 -3 -1.80 4.40 -8 -2 5 212.88 14.10 -8 -2 5 205.78 10.50 -8 -2 5 191.38 10.30 -8 -2 5 195.48 10.20 -8 -2 5 190.18 19.70 8 2 -5 220.28 16.30 8 2 -5 188.98 10.80 8 2 -5 201.58 12.20 -11 -3 7 13.20 12.40 -11 -3 7 1.50 7.30 -11 -3 7 7.70 7.80 -11 -3 7 -7.60 8.40 -11 -3 7 6.00 10.60 11 3 -7 -4.40 7.00 11 3 -7 15.70 8.40 11 3 -7 7.30 14.30 -14 -4 9 31.70 25.90 14 4 -9 5.10 12.40 14 4 -9 19.10 16.40 8 4 -6 -13.80 15.60 8 4 -6 8.60 8.10 8 4 -6 -0.30 8.70 -8 -4 6 3.80 19.70 -8 -4 6 17.90 12.80 5 3 -4 124.89 15.60 5 3 -4 102.79 17.90 5 3 -4 109.09 8.10 5 3 -4 112.09 8.80 -5 -3 4 112.69 13.20 -5 -3 4 87.09 16.90 2 2 -2 327.37 11.00 2 2 -2 315.47 10.80 2 2 -2 358.46 17.00 2 2 -2 350.36 18.70 -2 -2 2 317.47 16.40 -2 -2 2 306.87 16.10 -1 1 0 1.60 2.10 -1 1 0 -2.70 3.60 -1 1 0 3.70 4.20 -1 1 0 -0.30 2.20 1 -1 0 3.00 3.60 1 -1 0 0.10 1.60 1 -1 0 1.00 4.90 1 -1 0 0.30 1.60 -4 0 2 251.57 8.40 -4 0 2 252.67 8.40 4 0 -2 245.98 8.40 4 0 -2 244.88 8.60 -7 -1 4 1100.89 32.30 -7 -1 4 1149.69 30.50 -7 -1 4 1122.19 30.50 7 1 -4 1134.49 30.90 7 1 -4 1139.69 30.90 7 1 -4 1116.59 31.80 -10 -2 6 22.70 8.10 -10 -2 6 24.00 6.20 -10 -2 6 11.70 5.80 -10 -2 6 16.80 6.10 10 2 -6 28.80 6.90 10 2 -6 16.50 6.50 10 2 -6 19.10 9.40 -13 -3 8 23.60 9.20 -13 -3 8 -2.60 13.30 -13 -3 8 7.20 9.40 -13 -3 8 40.90 14.40 13 3 -8 -0.10 14.30 13 3 -8 -1.00 9.50 13 3 -8 -0.10 8.10 -16 -4 10 40.50 27.10 -16 -4 10 18.00 14.30 16 4 -10 22.10 13.10 16 4 -10 5.00 16.20 6 4 -5 13.40 7.30 6 4 -5 3.60 6.60 6 4 -5 9.20 17.60 -6 -4 5 3.80 12.60 -6 -4 5 6.50 19.40 3 3 -3 2.30 4.00 3 3 -3 -5.20 4.60 3 3 -3 2.10 14.40 3 3 -3 13.40 14.20 -3 -3 3 8.70 11.90 -3 -3 3 3.60 8.10 0 2 -1 319.77 10.70 0 2 -1 323.17 10.80 0 2 -1 328.07 18.60 0 2 -1 305.87 16.60 0 -2 1 323.57 16.90 0 -2 1 329.57 14.30 -3 1 1 1757.02 46.50 -3 1 1 1760.72 43.90 -3 1 1 1844.12 47.40 -3 1 1 1754.92 44.00 3 -1 -1 1834.02 45.30 3 -1 -1 1764.82 43.80 3 -1 -1 1790.42 43.70 -6 0 3 5.10 3.30 -6 0 3 1.00 2.60 6 0 -3 3.10 2.70 -9 -1 5 351.16 12.50 -9 -1 5 351.06 13.90 -9 -1 5 347.07 14.40 9 1 -5 373.06 14.10 9 1 -5 368.76 14.40 9 1 -5 351.36 14.10 -12 -2 7 0.10 10.20 -12 -2 7 6.70 7.80 -12 -2 7 3.00 6.20 -12 -2 7 11.80 6.80 12 2 -7 11.00 6.40 12 2 -7 1.30 8.30 12 2 -7 11.30 6.50 -15 -3 9 -3.30 9.10 -15 -3 9 -4.80 12.80 -15 -3 9 10.20 9.70 -15 -3 9 -11.70 14.30 15 3 -9 11.90 16.00 15 3 -9 6.90 10.30 15 3 -9 -1.30 9.00 -18 -4 11 3.30 14.20 -18 -4 11 9.30 29.70 -18 -4 11 20.20 13.90 18 4 -11 -14.20 17.30 18 4 -11 13.10 14.90 7 5 -6 74.19 29.40 -7 -5 6 -6.30 15.60 4 4 -4 4.00 15.30 -4 -4 4 -32.30 11.30 1 3 -2 -12.00 13.60 1 3 -2 -10.00 11.50 1 3 -2 12.50 4.60 1 3 -2 -3.10 4.50 -1 -3 2 2.00 8.40 -1 -3 2 6.50 9.80 -2 2 0 37.20 4.40 -2 2 0 29.30 8.30 -2 2 0 30.90 10.90 -2 2 0 32.40 4.30 2 -2 0 33.30 3.70 2 -2 0 24.90 6.80 2 -2 0 34.70 3.40 -5 1 2 2757.42 69.39 -5 1 2 2827.42 69.39 5 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1.10 20.10 -4 -2 -27 -55.19 32.40 -4 -2 -27 -1.60 26.50 1 1 29 24.10 25.30 1 1 29 1.40 26.80 -1 -1 -29 -15.90 26.10 -1 -1 -29 -37.90 26.90 -2 0 31 27.50 29.00 -2 0 31 75.09 31.10 2 0 -31 23.70 30.10 2 0 -31 -21.60 27.60 -5 -1 33 27.50 20.80 -5 -1 33 -41.50 34.50 -5 -1 33 24.70 28.70 5 1 -33 -8.00 31.20 5 1 -33 -8.50 36.60 2 2 28 -11.30 24.80 2 2 28 -38.30 25.00 -2 -2 -28 -12.00 28.30 -2 -2 -28 -8.20 20.60 -2 -2 -28 -23.20 33.90 -1 1 30 47.40 25.40 -1 1 30 -27.50 26.50 1 -1 -30 26.80 26.70 1 -1 -30 66.99 32.10 -4 0 32 -18.60 29.70 -4 0 32 -9.30 29.20 4 0 -32 -44.50 33.30 4 0 -32 -20.50 28.90 -7 -1 34 22.80 30.80 -7 -1 34 51.39 38.20 7 1 -34 -25.30 39.10 7 1 -34 93.99 32.80 0 2 29 -15.00 28.30 0 2 29 14.00 26.10 0 -2 -29 10.10 22.50 0 -2 -29 34.10 28.70 0 -2 -29 42.60 35.70 -3 1 31 47.20 27.10 -3 1 31 -21.50 24.00 3 -1 -31 0.10 25.20 3 -1 -31 8.90 31.10 -6 0 33 -35.90 38.30 -6 0 33 35.60 29.90 6 0 -33 11.80 34.60 6 0 -33 -24.90 28.40 -9 -1 35 4.60 41.30 -9 -1 35 11.40 33.50 9 1 -35 -25.80 41.30 9 1 -35 86.39 38.40 -2 2 30 -22.40 27.60 -2 2 30 50.19 28.60 2 -2 -30 7.00 22.80 2 -2 -30 -33.60 50.79 -5 1 32 77.59 28.70 -5 1 32 13.00 27.80 5 -1 -32 20.90 21.40 5 -1 -32 52.39 28.30 5 -1 -32 13.70 33.30 -8 0 34 13.00 30.50 8 0 -34 14.70 28.40 8 0 -34 7.60 34.60 -4 2 31 47.60 28.80 -4 2 31 -26.00 25.70 4 -2 -31 3.40 25.80 -7 1 33 24.60 28.90 -7 1 33 68.19 31.30 7 -1 -33 0.30 21.30 7 -1 -33 -28.80 28.50 7 -1 -33 74.49 35.80 -10 0 35 -34.90 28.00 -10 0 35 -3.10 36.20 10 0 -35 -26.30 30.10 10 0 -35 -22.80 36.10 -6 2 32 -12.00 29.60 -6 2 32 71.59 29.60 6 -2 -32 11.80 26.10 6 -2 -32 34.50 38.50 -9 1 34 22.30 29.80 -9 1 34 57.39 32.50 9 -1 -34 4.30 35.20 9 -1 -34 -4.00 22.30 -12 0 36 -35.00 30.30 -12 0 36 -37.80 36.20 12 0 -36 34.60 40.30 12 0 -36 -45.60 33.40 -8 2 33 -28.20 31.50 8 -2 -33 33.00 38.70 -11 1 35 -10.30 29.90 -11 1 35 81.29 34.70 11 -1 -35 28.60 36.40 11 -1 -35 -13.40 23.70 11 -1 -35 13.40 35.70 18 0 22 1.50 34.60 18 0 22 13.90 17.70 18 0 22 -36.80 33.60 -18 0 -22 38.20 41.50 -18 0 -22 21.20 30.40 15 -1 24 30.80 34.00 15 -1 24 14.40 40.20 15 -1 24 -3.70 17.30 -15 1 -24 9.60 33.20 -15 1 -24 37.90 41.40 19 1 21 39.00 34.20 19 1 21 -10.30 36.10 -19 -1 -21 -33.00 40.20 16 0 23 -0.10 13.70 16 0 23 -31.00 34.00 16 0 23 -18.50 34.20 -16 0 -23 0.00 37.10 -16 0 -23 46.20 31.10 13 -1 25 -30.90 31.90 13 -1 25 -13.10 17.30 13 -1 25 5.40 39.00 -13 1 -25 -25.00 36.90 -13 1 -25 -37.30 28.20 17 1 22 -34.20 33.50 17 1 22 14.00 33.70 -17 -1 -22 -21.90 38.00 -17 -1 -22 86.79 44.00 14 0 24 -2.40 36.20 14 0 24 21.00 34.50 14 0 24 27.00 16.20 -14 0 -24 30.40 35.60 -14 0 -24 14.70 30.30 11 -1 26 -14.20 18.80 11 -1 26 32.30 32.40 11 -1 26 -37.10 36.30 -11 1 -26 33.90 37.50 -11 1 -26 11.70 29.30 15 1 23 9.50 32.10 15 1 23 -36.60 30.80 -15 -1 -23 -2.80 30.00 -15 -1 -23 -7.70 36.90 12 0 25 14.90 15.10 12 0 25 -62.29 30.70 12 0 25 20.40 46.80 -12 0 -25 -13.10 35.60 -12 0 -25 12.00 29.40 9 -1 27 17.50 35.80 9 -1 27 -2.50 17.30 9 -1 27 18.90 30.50 -9 1 -27 63.89 30.20 -9 1 -27 -4.10 37.80 13 1 24 -24.80 31.30 13 1 24 -5.50 12.60 13 1 24 11.50 30.20 -13 -1 -24 69.99 31.80 -13 -1 -24 20.70 37.10 10 0 26 33.70 15.30 10 0 26 13.30 30.00 -10 0 -26 41.00 32.70 -10 0 -26 70.29 30.80 7 -1 28 23.40 36.00 7 -1 28 15.10 19.40 7 -1 28 -42.00 28.80 -7 1 -28 47.20 30.30 -7 1 -28 -27.60 36.60 11 1 25 55.29 32.20 11 1 25 65.09 31.00 11 1 25 8.10 13.30 -11 -1 -25 42.10 30.30 -11 -1 -25 -21.70 33.20 8 0 27 -7.30 29.00 8 0 27 -21.60 13.70 8 0 27 -1.80 38.30 -8 0 -27 -30.10 33.10 -8 0 -27 14.40 28.60 5 -1 29 10.30 29.80 5 -1 29 -44.00 34.40 -5 1 -29 -35.00 34.60 -5 1 -29 3.30 29.30 12 2 24 -34.90 29.40 12 2 24 -0.90 31.50 -12 -2 -24 -1.40 22.00 -12 -2 -24 15.30 42.60 9 1 26 30.90 27.90 9 1 26 19.40 28.20 -9 -1 -26 8.00 32.10 -9 -1 -26 -18.50 25.60 6 0 28 -29.50 14.90 6 0 28 32.70 29.70 6 0 28 -30.40 32.90 -6 0 -28 5.50 26.70 -6 0 -28 35.70 33.10 3 -1 30 -41.50 35.50 3 -1 30 20.30 21.60 3 -1 30 46.40 32.80 -3 1 -30 -27.60 29.40 -3 1 -30 -4.60 35.30 10 2 25 -12.00 28.40 10 2 25 38.30 29.10 -10 -2 -25 4.10 39.90 -10 -2 -25 11.70 22.10 7 1 27 24.60 27.10 7 1 27 -19.60 28.20 -7 -1 -27 -20.70 32.50 -7 -1 -27 19.60 26.60 4 0 29 14.10 33.10 4 0 29 -61.79 28.20 -4 0 -29 67.59 33.50 -4 0 -29 81.19 27.70 1 -1 31 7.50 30.70 1 -1 31 13.90 37.40 1 -1 31 -23.70 17.80 -1 1 -31 0.00 35.40 -1 1 -31 2.40 29.70 8 2 26 -48.90 27.70 8 2 26 -27.30 28.60 -8 -2 -26 31.70 37.00 -8 -2 -26 -9.20 20.70 5 1 28 5.00 27.10 5 1 28 33.90 27.90 -5 -1 -28 15.60 27.70 -5 -1 -28 -20.40 31.70 2 0 30 35.50 30.70 2 0 30 24.10 36.10 -2 0 -30 0.30 27.90 -2 0 -30 12.50 31.60 -1 -1 32 19.90 19.70 -1 -1 32 2.60 35.50 -1 -1 32 6.80 32.30 1 1 -32 35.80 37.70 1 1 -32 5.70 32.20 6 2 27 54.29 29.60 6 2 27 -10.00 26.40 -6 -2 -27 -7.50 23.70 -6 -2 -27 45.50 38.30 3 1 29 11.10 29.00 3 1 29 12.40 28.50 -3 -1 -29 22.30 32.20 -3 -1 -29 31.30 27.50 0 0 31 -24.60 42.90 0 0 31 24.60 28.50 0 0 -31 82.59 29.50 0 0 -31 16.50 31.80 -3 -1 33 -15.30 21.20 -3 -1 33 -30.10 29.80 -3 -1 33 52.39 38.00 3 1 -33 -5.10 31.20 3 1 -33 6.40 40.30 4 2 28 -27.10 27.50 4 2 28 1.90 29.50 -4 -2 -28 18.20 23.50 -4 -2 -28 -51.29 37.40 1 1 30 -5.00 28.90 1 1 30 63.39 28.10 -1 -1 -30 35.50 27.40 -1 -1 -30 25.90 31.90 -2 0 32 -14.70 28.70 2 0 -32 -22.50 26.80 2 0 -32 -2.40 33.80 -5 -1 34 -2.20 30.20 -5 -1 34 9.00 40.90 -5 -1 34 -3.30 18.90 5 1 -34 36.70 43.30 5 1 -34 40.70 37.00 2 2 29 6.20 29.10 2 2 29 -59.69 26.50 -2 -2 -29 18.60 23.80 -2 -2 -29 26.20 45.70 -1 1 31 25.10 28.20 -1 1 31 -5.80 27.40 1 -1 -31 59.99 33.80 1 -1 -31 -40.30 26.60 -4 0 33 -4.50 29.90 -4 0 33 36.60 38.60 4 0 -33 -21.30 27.30 4 0 -33 -34.50 35.00 0 2 30 -14.80 29.90 0 2 30 11.40 28.00 0 -2 -30 2.00 24.10 -3 1 32 76.29 29.90 -3 1 32 32.40 29.80 3 -1 -32 15.00 28.30 3 -1 -32 11.50 34.80 3 -1 -32 -0.80 19.60 -6 0 34 52.99 36.40 -6 0 34 14.00 30.60 6 0 -34 -42.90 30.50 6 0 -34 -3.00 37.50 -2 2 31 4.60 28.60 -2 2 31 -1.80 30.20 2 -2 -31 20.30 25.30 -5 1 33 52.29 30.40 -5 1 33 -21.10 28.80 5 -1 -33 0.00 38.00 5 -1 -33 39.90 29.70 5 -1 -33 -10.20 20.70 -8 0 35 0.40 36.30 -8 0 35 -0.20 31.40 8 0 -35 -0.70 31.10 8 0 -35 -12.10 35.30 -4 2 32 -8.50 29.90 -4 2 32 -4.00 27.80 4 -2 -32 12.90 40.60 -7 1 34 64.09 32.40 -7 1 34 33.40 30.60 7 -1 -34 5.10 37.20 7 -1 -34 -8.80 31.80 7 -1 -34 18.40 24.60 -10 0 36 -18.00 36.70 -10 0 36 -38.90 31.50 10 0 -36 11.90 41.20 10 0 -36 6.50 35.30 -9 1 35 -29.70 31.60 -9 1 35 5.00 34.80 9 -1 -35 -56.59 39.30 9 -1 -35 -7.10 24.80 16 0 24 5.50 16.20 16 0 24 28.40 37.10 16 0 24 -18.00 35.20 -16 0 -24 15.90 34.20 -16 0 -24 17.50 43.20 14 0 25 -1.60 16.00 14 0 25 12.40 36.50 14 0 25 -77.79 33.30 -14 0 -25 93.19 31.50 -14 0 -25 71.19 42.10 11 -1 27 -41.80 32.40 11 -1 27 -19.70 20.40 11 -1 27 -55.59 41.30 -11 1 -27 60.59 45.10 -11 1 -27 -41.30 30.80 15 1 24 83.79 38.40 15 1 24 -81.99 32.90 -15 -1 -24 -43.30 36.60 12 0 26 -30.10 33.30 12 0 26 30.50 34.20 12 0 26 1.10 15.40 -12 0 -26 65.79 38.80 -12 0 -26 -31.70 29.80 9 -1 28 57.79 41.20 9 -1 28 55.59 33.90 9 -1 28 58.79 23.10 -9 1 -28 -34.70 33.30 -9 1 -28 -16.50 42.30 13 1 25 43.00 32.60 13 1 25 10.70 13.40 13 1 25 -42.70 32.30 -13 -1 -25 25.00 38.90 -13 -1 -25 -44.10 40.40 10 0 27 -47.00 31.00 10 0 27 -33.70 14.70 10 0 27 26.60 35.60 -10 0 -27 75.29 30.50 -10 0 -27 -0.80 37.50 7 -1 29 -3.50 30.70 7 -1 29 -31.50 25.60 7 -1 29 22.00 38.90 -7 1 -29 -17.80 38.40 11 1 26 -25.30 29.20 11 1 26 -1.70 15.00 11 1 26 19.30 31.90 -11 -1 -26 -8.50 33.00 -11 -1 -26 63.79 38.50 8 0 28 17.00 34.70 8 0 28 -1.80 16.00 8 0 28 15.00 32.00 -8 0 -28 -15.90 36.40 -8 0 -28 6.20 27.40 5 -1 30 27.30 39.60 5 -1 30 28.50 30.30 5 -1 30 -0.70 21.30 -5 1 -30 16.00 30.10 -5 1 -30 -1.70 38.30 9 1 27 -33.20 29.90 9 1 27 -70.49 29.90 -9 -1 -27 -17.20 36.80 -9 -1 -27 -41.10 29.10 6 0 29 -22.60 31.00 6 0 29 17.90 17.60 6 0 29 36.90 37.20 -6 0 -29 9.20 35.70 -6 0 -29 27.60 28.30 3 -1 31 1.00 22.40 3 -1 31 -48.50 30.30 3 -1 31 55.19 41.90 -3 1 -31 106.19 40.30 -3 1 -31 -8.30 30.40 7 1 28 10.10 28.00 7 1 28 -44.40 28.10 -7 -1 -28 21.10 28.20 -7 -1 -28 0.10 38.30 4 0 30 29.80 36.60 4 0 30 -60.69 28.50 -4 0 -30 -13.40 34.80 -4 0 -30 -1.90 29.60 1 -1 32 -7.60 22.60 1 -1 32 48.60 41.60 1 -1 32 -42.30 32.80 -1 1 -32 -39.70 29.20 -1 1 -32 -2.90 40.80 5 1 29 36.70 31.20 5 1 29 -48.30 27.40 -5 -1 -29 -25.10 28.80 -5 -1 -29 18.70 39.60 2 0 31 -50.79 29.30 2 0 31 35.10 34.70 -2 0 -31 -48.50 34.20 -2 0 -31 69.39 33.10 -1 -1 33 96.99 33.10 -1 -1 33 11.20 18.70 -1 -1 33 -43.60 37.90 1 1 -33 -1.40 43.00 1 1 -33 55.09 32.40 3 1 30 -3.00 31.50 3 1 30 -58.19 27.10 -3 -1 -30 6.40 37.70 -3 -1 -30 34.40 28.90 0 0 32 4.40 33.90 0 0 32 -16.80 30.90 0 0 -32 -15.50 29.30 0 0 -32 24.40 37.90 1 1 31 9.90 31.30 1 1 31 0.40 29.10 -1 -1 -31 18.10 37.00 -1 -1 -31 -7.90 29.50 -2 0 33 10.10 28.30 -2 0 33 42.20 35.70 2 0 -33 61.29 32.70 2 0 -33 57.29 39.30 -1 1 32 30.50 30.90 -1 1 32 -13.00 31.40 1 -1 -32 -98.29 34.20 1 -1 -32 24.20 34.80 -4 0 34 -54.49 28.60 -4 0 34 -9.50 34.80 4 0 -34 -20.10 39.70 4 0 -34 29.00 30.70 -3 1 33 -8.90 31.00 -3 1 33 43.40 34.10 3 -1 -33 -64.89 33.20 3 -1 -33 72.89 34.80 3 -1 -33 -4.20 24.00 -6 0 35 -67.29 31.70 -6 0 35 60.79 37.10 6 0 -35 43.00 42.10 6 0 -35 -50.19 34.60 -5 1 34 31.80 32.40 -5 1 34 0.20 31.80 5 -1 -34 46.40 39.30 5 -1 -34 -1.00 22.70 12 0 27 15.60 36.20 12 0 27 66.19 34.30 12 0 27 6.40 17.40 -12 0 -27 10.90 43.10 -12 0 -27 58.49 32.50 10 0 28 47.30 32.90 10 0 28 -54.99 33.10 -10 0 -28 27.00 34.70 -10 0 -28 87.99 42.60 11 1 27 6.40 33.60 11 1 27 14.70 34.00 11 1 27 0.50 15.70 -11 -1 -27 -25.00 39.40 8 0 29 -32.10 17.40 8 0 29 -40.20 31.00 8 0 29 10.10 34.60 -8 0 -29 3.60 43.00 -8 0 -29 18.50 31.30 9 1 28 7.20 34.80 9 1 28 34.30 33.90 -9 -1 -28 31.30 38.10 6 0 30 -26.20 30.20 6 0 30 11.20 18.30 6 0 30 15.90 34.40 -6 0 -30 52.99 30.20 -6 0 -30 -0.80 39.90 7 1 29 -32.00 32.10 7 1 29 7.30 32.10 -7 -1 -29 -21.80 37.60 4 0 31 13.10 35.10 4 0 31 6.20 18.80 4 0 31 -44.20 30.40 -4 0 -31 0.60 31.80 -4 0 -31 -18.90 39.10 5 1 30 5.30 32.70 5 1 30 -22.60 32.80 -5 -1 -30 -17.90 40.10 2 0 32 -34.20 35.20 2 0 32 32.00 31.10 -2 0 -32 30.10 34.40 -2 0 -32 12.90 38.50 3 1 31 22.40 34.80 3 1 31 27.40 32.60 -3 -1 -31 -19.20 39.20 0 0 33 32.40 32.20 0 0 33 -43.20 35.30 0 0 -33 29.70 33.30 0 0 -33 22.80 41.20 1 1 32 -26.90 36.40 1 1 32 -6.50 33.10 -1 -1 -32 20.30 39.50 -2 0 34 -34.30 35.40 -2 0 34 77.49 36.00 2 0 -34 23.40 32.30 2 0 -34 64.79 43.20 -1 1 33 -1.90 32.10 -1 1 33 -22.80 32.90 1 -1 -33 -23.50 40.50 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 26893 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O2 O 0.37471(8) 0.4936(6) 0.45797(9) 0.0698(8) Uani 1 1 d . . . . O3 O 0.29467(8) 0.1732(7) 0.49942(10) 0.0776(8) Uani 1 1 d . . . . N003 N 0.29996(11) 0.5148(8) 0.42030(12) 0.0694(9) Uani 1 1 d . . . . C004 C 0.33369(14) 0.4150(10) 0.45758(15) 0.0632(11) Uani 1 1 d . . . . O005 O 0.30481(10) 0.8380(13) 0.31445(11) 0.1545(19) Uani 1 1 d . . . . C1 C 0.33528(14) 0.2327(10) 0.49794(15) 0.0648(11) Uani 1 1 d . . . . C007 C 0.36477(14) 0.6574(10) 0.41569(14) 0.0679(11) Uani 1 1 d . . . . C008 C 0.31871(14) 0.6684(10) 0.39235(14) 0.0693(11) Uani 1 1 d . . . . O1 O 0.52118(10) 1.0770(11) 0.39982(14) 0.1424(16) Uani 1 1 d . . . . C00A C 0.24080(14) 0.8466(11) 0.33101(15) 0.0762(12) Uani 1 1 d . . . . C00B C 0.22380(16) 0.9564(10) 0.36278(15) 0.0781(12) Uani 1 1 d . . . . H00B H 0.2429 0.9802 0.3953 0.094 Uiso 1 1 calc R . . . C00C C 0.36855(15) 0.1065(11) 0.53616(16) 0.0805(13) Uani 1 1 d . . . . H00C H 0.3992 0.1160 0.5435 0.097 Uiso 1 1 calc R . . . C00D C 0.40412(13) 0.7707(10) 0.40940(15) 0.0698(11) Uani 1 1 d . . . . C00E C 0.34819(17) -0.0452(11) 0.56356(16) 0.0878(14) Uani 1 1 d . . . . H00E H 0.3628 -0.1559 0.5923 0.105 Uiso 1 1 calc R . . . C00F C 0.30441(17) 0.0012(11) 0.54043(16) 0.0843(13) Uani 1 1 d . . . . H00F H 0.2830 -0.0734 0.5507 0.101 Uiso 1 1 calc R . . . C00G C 0.17927(18) 1.0306(10) 0.34712(18) 0.0856(13) Uani 1 1 d . . . . H00G H 0.1685 1.1090 0.3689 0.103 Uiso 1 1 calc R . . . C00H C 0.28929(16) 0.7887(13) 0.34416(15) 0.0943(16) Uani 1 1 d . . . . C00I C 0.16640(16) 0.8783(13) 0.26770(17) 0.1003(16) Uani 1 1 d . . . . H00I H 0.1467 0.8494 0.2355 0.120 Uiso 1 1 calc R . . . C00J C 0.15030(16) 0.9909(11) 0.29969(18) 0.0811(12) Uani 1 1 d . . . . C00K C 0.21124(16) 0.8073(13) 0.28262(15) 0.0971(16) Uani 1 1 d . . . . H00K H 0.2219 0.7332 0.2605 0.117 Uiso 1 1 calc R . . . C00L C 0.40222(15) 0.9302(13) 0.36965(18) 0.1029(17) Uani 1 1 d . . . . H00L H 0.3741 0.9692 0.3448 0.123 Uiso 1 1 calc R . . . C00M C 0.44622(17) 0.7231(15) 0.44502(19) 0.126(2) Uani 1 1 d . . . . H00M H 0.4491 0.6172 0.4730 0.151 Uiso 1 1 calc R . . . C00O C 0.48127(16) 0.9811(13) 0.4001(2) 0.0991(16) Uani 1 1 d . . . . C00R C 0.44002(16) 1.0361(13) 0.36458(19) 0.1095(18) Uani 1 1 d . . . . H00R H 0.4372 1.1447 0.3369 0.131 Uiso 1 1 calc R . . . C00U C 0.51984(18) 1.2377(17) 0.3583(2) 0.159(3) Uani 1 1 d . . . . H00A H 0.5074 1.1017 0.3307 0.238 Uiso 1 1 calc GR . . . H00D H 0.5499 1.2982 0.3633 0.238 Uiso 1 1 calc GR . . . H00H H 0.5013 1.4218 0.3528 0.238 Uiso 1 1 calc GR . . . C00V C 0.48463(17) 0.8276(17) 0.4408(2) 0.149(3) Uani 1 1 d . . . . H00V H 0.5128 0.7930 0.4658 0.178 Uiso 1 1 calc R . . . C3 C 0.1016(2) 1.0742(16) 0.2839(5) 0.113(2) Uani 1 1 d . . . . F1AA F 0.0852(4) 1.088(6) 0.3111(5) 0.162(8) Uani 0.5 1 d . P A 2 F2 F 0.0924(5) 1.333(3) 0.2523(7) 0.165(6) Uani 0.5 1 d . P A 2 F2AA F 0.0748(4) 0.860(4) 0.2448(7) 0.162(6) Uani 0.5 1 d . P A 2 F1 F 0.0811(6) 0.854(4) 0.2995(11) 0.189(8) Uani 0.5 1 d . P A 1 F0AA F 0.0980(4) 1.332(3) 0.3111(6) 0.153(5) Uani 0.5 1 d . P A 1 F3 F 0.0791(5) 1.117(5) 0.2430(5) 0.152(6) Uani 0.5 1 d . P A 1 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 O2 0.0583(17) 0.0875(19) 0.0691(18) -0.0028(16) 0.0319(14) -0.0009(15) O3 0.0600(18) 0.110(2) 0.0680(18) 0.0010(17) 0.0316(15) -0.0071(16) N003 0.061(2) 0.094(3) 0.054(2) -0.0080(19) 0.0240(19) -0.013(2) C004 0.057(3) 0.080(3) 0.060(3) -0.012(2) 0.032(2) -0.011(2) O005 0.072(2) 0.321(6) 0.067(2) 0.031(3) 0.0258(19) -0.033(3) C1 0.059(3) 0.076(3) 0.069(3) -0.013(2) 0.036(2) -0.006(2) C007 0.067(3) 0.086(3) 0.055(3) -0.009(2) 0.029(2) -0.008(2) C008 0.063(3) 0.095(3) 0.053(3) -0.007(2) 0.027(2) -0.016(2) O1 0.063(2) 0.217(4) 0.152(3) 0.066(3) 0.050(2) 0.002(2) C00A 0.062(3) 0.104(3) 0.056(3) 0.003(2) 0.017(2) -0.023(2) C00B 0.082(3) 0.088(3) 0.062(3) -0.011(2) 0.027(3) -0.017(3) C00C 0.061(3) 0.106(4) 0.080(3) 0.009(3) 0.034(3) 0.010(3) C00D 0.055(3) 0.090(3) 0.068(3) 0.001(2) 0.029(2) 0.000(2) C00E 0.084(4) 0.106(4) 0.078(3) 0.014(3) 0.039(3) 0.018(3) C00F 0.084(4) 0.109(4) 0.070(3) 0.011(3) 0.041(3) -0.006(3) C00G 0.093(4) 0.075(3) 0.092(4) -0.007(3) 0.042(3) -0.009(3) C00H 0.075(3) 0.153(5) 0.056(3) 0.003(3) 0.028(3) -0.027(3) C00I 0.068(3) 0.154(5) 0.067(3) -0.003(3) 0.015(3) -0.023(3) C00J 0.074(3) 0.083(3) 0.081(3) 0.012(3) 0.027(3) -0.009(3) C00K 0.078(3) 0.158(5) 0.055(3) -0.007(3) 0.028(3) -0.021(3) C00L 0.057(3) 0.156(5) 0.095(4) 0.034(3) 0.031(3) -0.005(3) C00M 0.068(3) 0.195(6) 0.115(4) 0.071(4) 0.037(3) 0.003(4) C00O 0.059(3) 0.139(4) 0.111(4) 0.033(4) 0.048(3) 0.003(3) C00R 0.066(3) 0.162(5) 0.105(4) 0.046(4) 0.041(3) 0.001(3) C00U 0.098(4) 0.232(8) 0.173(6) 0.086(6) 0.083(4) 0.003(4) C00V 0.057(3) 0.239(7) 0.140(5) 0.093(5) 0.032(3) 0.009(4) C3 0.090(5) 0.079(5) 0.154(8) 0.021(5) 0.034(6) -0.006(4) F1AA 0.087(7) 0.29(3) 0.122(7) 0.005(17) 0.057(6) 0.009(15) F2 0.120(9) 0.146(10) 0.197(15) 0.068(9) 0.034(9) 0.011(6) F2AA 0.086(6) 0.173(11) 0.172(12) -0.035(11) -0.002(6) -0.013(8) F1 0.122(8) 0.182(12) 0.30(2) 0.024(14) 0.120(12) -0.006(9) F0AA 0.123(9) 0.155(9) 0.162(10) -0.007(9) 0.041(7) 0.043(7) F3 0.083(8) 0.25(2) 0.104(8) -0.008(16) 0.018(6) 0.021(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 C004 O2 C007 105.2(3) C00F O3 C1 105.5(3) C004 N003 C008 105.2(3) O2 C004 C1 115.7(4) N003 C004 O2 113.8(3) N003 C004 C1 130.5(4) O3 C1 C004 115.8(4) C00C C1 O3 110.3(4) C00C C1 C004 133.9(4) O2 C007 C00D 114.2(4) C008 C007 O2 106.6(3) C008 C007 C00D 139.2(4) N003 C008 C00H 120.0(4) C007 C008 N003 109.2(3) C007 C008 C00H 130.6(4) C00O O1 C00U 118.0(4) C00B C00A C00H 124.1(4) C00B C00A C00K 118.5(4) C00K C00A C00H 117.3(4) C00A C00B H00B 119.6 C00G C00B C00A 120.8(4) C00G C00B H00B 119.6 C1 C00C H00C 126.7 C1 C00C C00E 106.7(4) C00E C00C H00C 126.7 C00L C00D C007 124.2(4) C00L C00D C00M 116.0(4) C00M C00D C007 119.8(4) C00C C00E H00E 126.7 C00F C00E C00C 106.5(4) C00F C00E H00E 126.7 O3 C00F H00F 124.5 C00E C00F O3 111.1(4) C00E C00F H00F 124.5 C00B C00G H00G 119.7 C00B C00G C00J 120.7(4) C00J C00G H00G 119.7 O005 C00H C008 119.8(4) O005 C00H C00A 119.5(4) C008 C00H C00A 120.6(4) C00J C00I H00I 119.6 C00J C00I C00K 120.7(4) C00K C00I H00I 119.6 C00G C00J C3 119.1(7) C00I C00J C00G 119.5(5) C00I C00J C3 121.5(7) C00A C00K H00K 120.1 C00I C00K C00A 119.9(4) C00I C00K H00K 120.1 C00D C00L H00L 118.5 C00D C00L C00R 123.1(4) C00R C00L H00L 118.5 C00D C00M H00M 119.0 C00D C00M C00V 121.9(5) C00V C00M H00M 119.0 C00R C00O O1 125.3(5) C00R C00O C00V 119.3(4) C00V C00O O1 115.4(5) C00L C00R H00R 120.2 C00O C00R C00L 119.5(4) C00O C00R H00R 120.2 O1 C00U H00A 109.5 O1 C00U H00D 109.5 O1 C00U H00H 109.5 H00A C00U H00D 109.5 H00A C00U H00H 109.5 H00D C00U H00H 109.5 C00M C00V H00V 119.9 C00O C00V C00M 120.1(5) C00O C00V H00V 119.9 F1AA C3 C00J 121.6(11) F1AA C3 F2 114.6(15) F1AA C3 F2AA 108.4(12) F2 C3 C00J 107.5(8) F2 C3 F2AA 92.7(15) F2AA C3 C00J 108.0(9) F1 C3 C00J 109.6(10) F1 C3 F0AA 99.4(16) F0AA C3 C00J 109.3(9) F3 C3 C00J 119.5(12) F3 C3 F1 107.5(15) F3 C3 F0AA 109.7(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O2 C004 1.371(4) O2 C007 1.377(4) O3 C1 1.364(4) O3 C00F 1.364(5) N003 C004 1.280(5) N003 C008 1.396(4) C004 C1 1.434(5) O005 C00H 1.221(4) C1 C00C 1.330(5) C007 C008 1.369(5) C007 C00D 1.453(5) C008 C00H 1.470(6) O1 C00O 1.365(5) O1 C00U 1.419(6) C00A C00B 1.377(5) C00A C00H 1.480(6) C00A C00K 1.394(5) C00B H00B 0.9300 C00B C00G 1.363(6) C00C H00C 0.9300 C00C C00E 1.416(5) C00D C00L 1.364(5) C00D C00M 1.365(6) C00E H00E 0.9300 C00E C00F 1.317(5) C00F H00F 0.9300 C00G H00G 0.9300 C00G C00J 1.367(6) C00I H00I 0.9300 C00I C00J 1.367(6) C00I C00K 1.371(6) C00J C3 1.497(7) C00K H00K 0.9300 C00L H00L 0.9300 C00L C00R 1.377(6) C00M H00M 0.9300 C00M C00V 1.382(6) C00O C00R 1.350(6) C00O C00V 1.361(6) C00R H00R 0.9300 C00U H00A 0.9600 C00U H00D 0.9600 C00U H00H 0.9600 C00V H00V 0.9300 C3 F1AA 1.156(14) C3 F2 1.409(18) C3 F2AA 1.465(19) C3 F1 1.345(19) C3 F0AA 1.406(17) C3 F3 1.165(12) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion O2 C004 C1 O3 175.5(3) O2 C004 C1 C00C -3.4(7) O2 C007 C008 N003 0.7(4) O2 C007 C008 C00H -174.2(4) O2 C007 C00D C00L 178.0(4) O2 C007 C00D C00M -2.9(6) O3 C1 C00C C00E 0.5(5) N003 C004 C1 O3 -5.6(6) N003 C004 C1 C00C 175.5(5) N003 C008 C00H O005 -158.7(5) N003 C008 C00H C00A 20.5(7) C004 O2 C007 C008 0.0(4) C004 O2 C007 C00D 178.6(3) C004 N003 C008 C007 -1.1(4) C004 N003 C008 C00H 174.4(4) C004 C1 C00C C00E 179.5(4) C1 O3 C00F C00E 0.1(5) C1 C00C C00E C00F -0.4(5) C007 O2 C004 N003 -0.8(4) C007 O2 C004 C1 178.3(3) C007 C008 C00H O005 15.7(8) C007 C008 C00H C00A -165.1(4) C007 C00D C00L C00R 179.8(5) C007 C00D C00M C00V -179.7(5) C008 N003 C004 O2 1.2(4) C008 N003 C004 C1 -177.7(4) C008 C007 C00D C00L -4.1(8) C008 C007 C00D C00M 175.0(5) O1 C00O C00R C00L -179.0(5) O1 C00O C00V C00M 179.4(6) C00A C00B C00G C00J 1.5(7) C00B C00A C00H O005 -145.2(5) C00B C00A C00H C008 35.6(7) C00B C00A C00K C00I 0.1(7) C00B C00G C00J C00I -0.6(7) C00B C00G C00J C3 179.8(5) C00C C00E C00F O3 0.2(5) C00D C007 C008 N003 -177.3(5) C00D C007 C008 C00H 7.8(9) C00D C00L C00R C00O 0.3(9) C00D C00M C00V C00O -0.5(10) C00F O3 C1 C004 -179.6(3) C00F O3 C1 C00C -0.4(4) C00G C00J C3 F1AA -21(2) C00G C00J C3 F2 113.6(12) C00G C00J C3 F2AA -147.5(13) C00G C00J C3 F1 -74.4(18) C00G C00J C3 F0AA 33.6(12) C00G C00J C3 F3 161.1(14) C00H C00A C00B C00G 174.1(4) C00H C00A C00K C00I -175.6(5) C00I C00J C3 F1AA 159.1(19) C00I C00J C3 F2 -66.0(12) C00I C00J C3 F2AA 32.9(15) C00I C00J C3 F1 106.1(19) C00I C00J C3 F0AA -146.0(10) C00I C00J C3 F3 -18.5(17) C00J C00I C00K C00A 0.7(8) C00K C00A C00B C00G -1.2(7) C00K C00A C00H O005 30.2(7) C00K C00A C00H C008 -149.0(4) C00K C00I C00J C00G -0.5(8) C00K C00I C00J C3 179.1(5) C00L C00D C00M C00V -0.6(9) C00M C00D C00L C00R 0.7(8) C00R C00O C00V C00M 1.5(10) C00U O1 C00O C00R -2.4(9) C00U O1 C00O C00V 179.8(6) C00V C00O C00R C00L -1.4(9)