#------------------------------------------------------------------------------ #$Date: 2020-07-06 06:43:08 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253970 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/75/7157513.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_7157513 loop_ _publ_author_name 'Wei, Jun' 'Bao, Kun' 'Wang, Yuan' 'Sheng, Rong' 'Hu, Jinbo' _publ_section_title ; Novel usage of 2-BTSO2CF2H for metal-free electrophilic difluoroalkanethiolation of indoles. ; _journal_issue 24 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 4556 _journal_page_last 4559 _journal_paper_doi 10.1039/d0ob00872a _journal_volume 18 _journal_year 2020 _chemical_formula_sum 'C15 H18 B F2 N O2 S' _chemical_formula_weight 325.17 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2013 _audit_update_record ; 2020-04-05 deposited with the CCDC. 2020-05-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 8.2789(3) _cell_length_b 13.5084(5) _cell_length_c 29.7538(12) _cell_measurement_reflns_used 8451 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 53.259 _cell_measurement_theta_min 5.932 _cell_volume 3327.5(2) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_unetI/netI 0.0391 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 27898 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.999 _diffrn_reflns_theta_min 2.816 _exptl_absorpt_coefficient_mu 0.219 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.4612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.298 _exptl_crystal_description prismatic _exptl_crystal_F_000 1360 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.309 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.048 _refine_ls_extinction_coef 0.014(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 311 _refine_ls_number_reflns 3260 _refine_ls_number_restraints 135 _refine_ls_restrained_S_all 1.138 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0674 _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^)+(0.1085P)^2^+1.9299P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1840 _refine_ls_wR_factor_ref 0.2059 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2423 _reflns_number_total 3260 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ob00872a2.cif _cod_data_source_block mo_d8v19075_0m _cod_depositor_comments 'Adding full bibliography for 7157513.cif.' _cod_database_code 7157513 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.962 _shelx_estimated_absorpt_t_max 0.974 _shelxl_version_number 2013-4 _shelx_res_file ; TITL mo_d8v19075_0m_a.res in Pbca CELL 0.71073 8.2789 13.5084 29.7538 90 90 90 ZERR 8 0.0003 0.0005 0.0012 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O F S B UNIT 120 144 8 16 16 8 8 OMIT 0 0 2 OMIT -3.00 52.00 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 LIST 4 dfix 1.76 0.02 s1 c9' isor 0.01 f1 f2 c9 c9' f1' f2' simu 0.003 o1' o2' o1 o2 c10 c11 c12 c13 c14 c15 simu 0.004 c10' c11' c12' c13' c14' c15' delu 0.003 s1 c9 s1 c9' size 0.18 0.15 0.12 wpdb -1 mpla n1 c1 > c8 htab conf TEMP 19.88 WGHT 0.108500 1.929900 EXTI 0.014215 FVAR 0.81793 S1 6 0.479259 0.772217 0.547983 11.00000 0.06789 0.07313 = 0.07132 -0.00062 0.01220 -0.00447 PART 1 F1 5 0.330893 0.607257 0.557031 10.60000 0.13812 0.05831 = 0.12239 0.01738 -0.03091 -0.03594 F2 5 0.418665 0.648091 0.488616 10.50000 0.16755 0.13655 = 0.06199 -0.04966 0.00705 0.00004 C9 1 0.357283 0.677969 0.527927 10.80000 0.08321 0.09462 = 0.09172 -0.02426 -0.01439 -0.00238 AFIX 13 H9 2 0.252063 0.707812 0.521285 10.80000 -1.20000 PART 2 AFIX 0 F1' 5 0.456945 0.596125 0.511236 10.40000 0.16765 0.14347 = 0.22226 -0.11898 0.02255 0.01248 F2' 5 0.251418 0.656420 0.521262 10.50000 0.23524 0.22946 = 0.29904 -0.08032 -0.06101 -0.02717 C9' 1 0.390444 0.644487 0.544771 10.20000 0.09632 0.08566 = 0.09022 -0.01312 -0.00886 -0.01801 AFIX 13 H9' 2 0.381579 0.608472 0.573256 10.20000 -1.20000 PART 0 AFIX 0 N1 3 0.176100 0.918049 0.623563 11.00000 0.05226 0.05394 = 0.12061 -0.01477 -0.01010 0.01514 B1 7 0.589356 0.662958 0.647869 11.00000 0.04141 0.03947 = 0.05820 0.00090 0.00225 -0.00221 C1 1 0.241487 0.859862 0.656997 11.00000 0.03641 0.04970 = 0.09503 -0.01840 -0.00048 0.00259 C2 1 0.208426 0.857000 0.702844 11.00000 0.04903 0.08139 = 0.09942 -0.03891 0.01310 0.00649 AFIX 43 H2 2 0.131609 0.898686 0.715570 11.00000 -1.20000 AFIX 0 C3 1 0.291779 0.791542 0.728282 11.00000 0.06356 0.09904 = 0.07574 -0.02443 0.01550 -0.00036 AFIX 43 H3 2 0.271171 0.787842 0.758962 11.00000 -1.20000 AFIX 0 C4 1 0.408529 0.729244 0.709273 11.00000 0.05659 0.07543 = 0.06904 -0.00421 0.00918 0.00307 AFIX 43 H4 2 0.463253 0.685324 0.727915 11.00000 -1.20000 AFIX 0 C5 1 0.446086 0.730260 0.663746 11.00000 0.04031 0.04483 = 0.06594 -0.00641 0.00460 -0.00276 C6 1 0.357253 0.797221 0.637027 11.00000 0.03156 0.04113 = 0.07521 -0.01218 0.00163 -0.00286 C7 1 0.355831 0.820930 0.589964 11.00000 0.04731 0.04775 = 0.07572 -0.00239 -0.00192 -0.00027 C8 1 0.245180 0.893872 0.583897 11.00000 0.06281 0.05833 = 0.09292 0.00198 -0.00876 0.00667 AFIX 43 H8 2 0.220479 0.922996 0.556421 11.00000 -1.20000 PART 1 AFIX 0 O1 4 0.750576 0.687627 0.659455 10.50000 0.03690 0.04785 = 0.12344 -0.02708 -0.00188 0.00128 O2 4 0.573993 0.566675 0.642721 10.50000 0.03754 0.04561 = 0.13132 -0.02312 0.00248 0.00015 C10 1 0.851092 0.607185 0.640506 10.50000 0.04235 0.05329 = 0.13119 -0.02146 0.00536 0.00460 C11 1 0.744326 0.530369 0.628706 10.50000 0.03980 0.04936 = 0.13223 -0.02437 0.00255 0.00272 C12 1 0.754364 0.462317 0.592369 10.50000 0.06652 0.07675 = 0.13055 -0.04633 0.00715 0.00594 AFIX 137 H12A 2 0.736633 0.496716 0.564570 10.50000 -1.50000 H12B 2 0.673701 0.411883 0.595971 10.50000 -1.50000 H12C 2 0.859537 0.432398 0.592027 10.50000 -1.50000 AFIX 0 C13 1 0.751781 0.458192 0.674962 10.50000 0.07164 0.06577 = 0.14611 0.02177 -0.00382 0.01098 AFIX 137 H13A 2 0.685821 0.400594 0.670449 10.50000 -1.50000 H13B 2 0.712397 0.494698 0.700383 10.50000 -1.50000 H13C 2 0.861364 0.438232 0.680364 10.50000 -1.50000 AFIX 0 C14 1 0.997325 0.602918 0.665706 10.50000 0.05146 0.07427 = 0.13745 -0.02104 -0.01951 0.00271 AFIX 137 H14A 2 0.974020 0.582350 0.695901 10.50000 -1.50000 H14B 2 1.046738 0.667201 0.666192 10.50000 -1.50000 H14C 2 1.069719 0.556331 0.651998 10.50000 -1.50000 AFIX 0 C15 1 0.905566 0.652370 0.589717 10.50000 0.08160 0.08074 = 0.14084 0.00893 0.04543 0.00734 AFIX 137 H15A 2 0.979820 0.607482 0.575617 10.50000 -1.50000 H15B 2 0.956426 0.715686 0.593517 10.50000 -1.50000 H15C 2 0.811378 0.659594 0.571186 10.50000 -1.50000 PART 2 AFIX 0 O1' 4 0.732794 0.696497 0.637152 10.50000 0.04141 0.04796 = 0.13402 -0.01152 0.01221 0.00051 O2' 4 0.581507 0.568579 0.633519 10.50000 0.03725 0.04644 = 0.13034 -0.02733 0.00130 0.00091 C10' 1 0.838224 0.616736 0.624687 10.50000 0.05405 0.05708 = 0.11974 0.02039 0.02909 0.01995 C11' 1 0.741628 0.524619 0.642049 10.50000 0.05305 0.05074 = 0.11836 0.01807 0.01412 0.01845 C12' 1 0.741580 0.427300 0.622937 10.50000 0.06395 0.04617 = 0.15671 -0.00509 0.01443 0.01482 AFIX 137 H12D 2 0.689820 0.382134 0.643263 10.50000 -1.50000 H12E 2 0.850844 0.406352 0.617813 10.50000 -1.50000 H12F 2 0.684044 0.428187 0.594927 10.50000 -1.50000 AFIX 0 C13' 1 0.807112 0.517824 0.695674 10.50000 0.10489 0.09775 = 0.11554 0.02605 -0.01376 0.02657 AFIX 137 H13D 2 0.716316 0.520541 0.715705 10.50000 -1.50000 H13E 2 0.878155 0.572370 0.701758 10.50000 -1.50000 H13F 2 0.864116 0.456697 0.700064 10.50000 -1.50000 AFIX 0 C14' 1 1.002457 0.630373 0.637825 10.50000 0.05095 0.07521 = 0.17283 -0.00293 0.02054 -0.00495 AFIX 137 H14D 2 1.047855 0.684942 0.621464 10.50000 -1.50000 H14E 2 1.062716 0.571333 0.631390 10.50000 -1.50000 H14F 2 1.007311 0.644021 0.669460 10.50000 -1.50000 AFIX 0 C15' 1 0.810656 0.589383 0.569579 10.50000 0.10777 0.12057 = 0.10535 0.01413 0.03559 0.04474 AFIX 137 H15D 2 0.721541 0.544419 0.566504 10.50000 -1.50000 H15E 2 0.906747 0.559191 0.557820 10.50000 -1.50000 H15F 2 0.788078 0.649058 0.553222 10.50000 -1.50000 PART 0 AFIX 0 H1A 2 0.090310 0.973049 0.627146 11.00000 0.13504 HKLF 4 REM mo_d8v19075_0m_a.res in Pbca REM R1 = 0.0674 for 2423 Fo > 4sig(Fo) and 0.0869 for all 3260 data REM 311 parameters refined using 135 restraints END WGHT 0.1079 1.9412 REM Instructions for potential hydrogen bonds HTAB C9' O2' EQIV $1 -x+1/2, y+1/2, z HTAB C8 F1_$1 EQIV $2 -x+3/2, y-1/2, z HTAB C12 S1_$2 HTAB C12' O1'_$2 HTAB N1 O2_$1 HTAB N1 O2'_$1 REM Highest difference peak 0.309, deepest hole -0.284, 1-sigma level 0.048 Q1 1 0.9924 0.6431 0.6058 11.00000 0.05 0.31 Q2 1 0.4177 0.7210 0.5418 11.00000 0.05 0.29 Q3 1 0.7470 0.5288 0.5718 11.00000 0.05 0.29 Q4 1 0.4705 0.6944 0.5459 11.00000 0.05 0.28 Q5 1 0.6952 0.6812 0.6162 11.00000 0.05 0.26 Q6 1 0.4407 0.5881 0.5473 11.00000 0.05 0.23 Q7 1 0.8421 0.6376 0.5735 11.00000 0.05 0.21 Q8 1 0.9106 0.5680 0.6900 11.00000 0.05 0.21 Q9 1 0.4906 0.6525 0.4994 11.00000 0.05 0.20 Q10 1 0.8244 0.5724 0.6602 11.00000 0.05 0.20 Q11 1 0.5927 0.7186 0.5496 11.00000 0.05 0.20 Q12 1 0.5167 0.7021 0.6520 11.00000 0.05 0.19 Q13 1 0.3542 0.6964 0.4839 11.00000 0.05 0.19 Q14 1 0.3598 0.8023 0.5432 11.00000 0.05 0.19 Q15 1 0.2982 0.6305 0.5515 11.00000 0.05 0.18 Q16 1 0.4099 0.7660 0.6512 11.00000 0.05 0.17 Q17 1 0.2800 0.5721 0.5614 11.00000 0.05 0.16 Q18 1 0.4104 0.6451 0.4730 11.00000 0.05 0.16 Q19 1 0.5722 0.6452 0.6415 11.00000 0.05 0.16 Q20 1 0.7373 0.5434 0.6104 11.00000 0.05 0.16 ; _shelx_res_checksum 76607 _shelx_hkl_file ; 1 0 0 -0.10 0.30 -1 0 0 -0.50 0.40 1 0 0 0.50 0.30 3 0 0 1.90 1.40 3 0 0 -0.70 1.70 -3 0 0 3.20 2.20 3 0 0 -0.80 0.90 -3 0 0 0.40 1.20 4 0 0 5909.91 427.36 -4 0 0 6151.38 433.56 4 0 0 5924.01 427.46 4 0 0 5771.52 432.86 5 0 0 2.60 1.80 5 0 0 2.80 2.00 5 0 0 4.80 3.80 -5 0 0 -1.50 3.30 6 0 0 559.04 49.00 6 0 0 490.95 39.40 -6 0 0 525.35 51.89 7 0 0 1.80 1.80 -7 0 0 5.30 5.10 8 0 0 481.15 35.80 -8 0 0 483.55 50.59 8 0 0 483.05 35.60 -9 0 0 -4.90 6.60 -10 0 0 106.49 21.90 1 1 0 0.40 0.60 -1 -1 0 1.10 0.90 -1 1 0 1.40 0.90 1 -1 0 0.00 0.80 -1 1 0 -0.40 0.30 3 1 0 0.70 0.60 3 -1 0 -1.90 1.30 -3 1 0 1.40 1.80 -3 1 0 2.50 2.10 -3 -1 0 2.80 2.40 3 -1 0 -0.70 1.20 3 -1 0 0.50 1.40 3 1 0 1.20 1.80 4 -1 0 658.63 55.99 -4 1 0 706.13 52.49 4 1 0 654.53 55.39 4 1 0 676.63 48.70 4 1 0 673.53 48.90 -4 1 0 666.53 56.19 4 -1 0 644.24 51.79 4 -1 0 669.43 51.89 -4 -1 0 680.23 55.79 5 -1 0 5.60 3.60 5 -1 0 1.50 2.20 5 1 0 0.80 0.90 5 1 0 -4.60 3.10 -5 -1 0 1.80 3.20 -5 1 0 -1.50 2.80 5 1 0 0.40 0.70 5 -1 0 -3.90 2.00 -6 1 0 -2.70 3.70 6 1 0 -2.20 3.80 6 -1 0 2.80 2.70 6 -1 0 -1.90 2.50 -6 -1 0 -7.30 3.70 6 -1 0 -0.40 3.40 -7 -1 0 10.70 5.90 7 -1 0 0.80 3.20 7 -1 0 -10.60 5.20 -7 1 0 -4.10 4.80 7 -1 0 1.20 2.80 8 -1 0 1066.79 80.79 -8 1 0 1038.60 93.99 -8 -1 0 1089.89 93.99 8 -1 0 1090.39 80.49 -9 1 0 2.40 7.80 -9 -1 0 -3.20 6.80 9 -1 0 -5.80 2.80 9 -1 0 -2.20 1.90 -10 1 0 48.20 17.50 -10 -1 0 33.30 15.30 -1 -2 0 1.00 0.70 1 2 0 1.30 0.90 1 -2 0 0.40 0.80 1 -2 0 0.10 1.00 -1 -2 0 -0.60 0.60 -1 2 0 -0.50 0.80 1 2 0 3.20 1.10 2 -2 0 9237.58 664.73 -3 2 0 5.90 2.80 3 -2 0 -1.40 1.80 3 -2 0 2.30 2.20 3 -2 0 2.90 2.20 3 2 0 1.10 1.80 -3 2 0 4.70 2.60 -3 -2 0 1.20 1.60 4 2 0 101.19 13.00 -4 2 0 92.89 13.70 4 -2 0 91.49 11.20 -4 -2 0 101.89 13.30 4 -2 0 111.19 14.10 4 -2 0 92.39 11.20 -4 2 0 96.59 11.70 5 -2 0 5.20 3.40 5 -2 0 1.70 3.90 5 2 0 -2.50 3.30 5 -2 0 2.50 2.80 -5 2 0 1.40 3.70 -5 2 0 -2.40 2.20 6 -2 0 375.36 32.40 -6 -2 0 375.26 37.40 6 -2 0 404.66 38.70 -6 2 0 373.96 38.30 6 -2 0 338.97 32.00 7 -2 0 2.40 5.80 -7 -2 0 6.90 5.00 -7 2 0 -7.30 4.10 7 -2 0 5.30 4.00 -8 2 0 81.09 18.80 8 -2 0 60.39 9.40 8 -2 0 56.39 9.90 -8 -2 0 58.69 16.30 -9 -2 0 7.50 8.60 9 -2 0 2.80 3.70 9 -2 0 1.20 4.30 -9 2 0 1.90 7.50 -10 -2 0 -8.10 7.20 10 -2 0 -3.00 3.10 -10 2 0 9.80 10.60 0 -3 0 0.50 1.30 0 3 0 2.20 0.70 0 3 0 0.70 1.30 -1 -3 0 -0.20 0.50 1 -3 0 0.10 1.60 1 3 0 0.60 1.20 -1 3 0 -0.10 1.00 -1 3 0 0.60 1.50 1 -3 0 -0.60 0.90 1 3 0 -0.10 0.50 -1 -3 0 1.60 1.60 2 -3 0 6349.96 450.65 2 3 0 6646.73 448.86 -2 -3 0 6220.08 448.86 -2 -3 0 6129.99 447.66 -2 -3 0 6282.77 447.66 2 3 0 6109.69 447.66 2 -3 0 5919.91 450.45 -2 3 0 6178.28 450.95 -3 3 0 1.50 2.20 -3 3 0 1.40 1.80 3 -3 0 -1.50 1.30 -3 -3 0 1.60 1.80 -3 -3 0 1.00 0.50 3 -3 0 0.50 2.40 3 3 0 1.60 2.00 3 -3 0 -0.10 2.20 4 -3 0 1763.62 140.39 -4 3 0 1978.90 143.89 -4 -3 0 1961.20 141.79 4 -3 0 1902.91 143.49 4 -3 0 1773.52 140.39 -4 3 0 1883.91 141.29 4 3 0 1880.81 141.29 5 -3 0 1.00 3.70 -5 -3 0 4.40 3.30 5 3 0 2.20 3.60 -5 3 0 0.40 3.90 5 -3 0 -0.70 2.50 -5 3 0 5.10 4.10 5 -3 0 8.80 5.10 6 -3 0 676.03 58.39 -6 3 0 746.33 64.79 6 -3 0 734.83 64.19 -6 -3 0 716.13 62.69 6 -3 0 727.63 58.99 -7 3 0 1.80 5.50 -7 -3 0 -1.70 3.80 7 -3 0 -7.10 4.00 7 -3 0 -4.70 3.70 7 -3 0 1.80 8.30 8 -3 0 1.30 5.20 8 -3 0 8.10 5.10 -8 3 0 1.60 7.20 -8 -3 0 8.50 6.60 -9 -3 0 -3.60 5.20 9 -3 0 6.10 6.30 9 -3 0 2.50 4.40 -10 3 0 -2.70 10.40 -10 -3 0 10.00 8.30 10 -3 0 10.00 5.10 0 4 0 5515.15 379.26 0 4 0 4949.10 382.96 0 -4 0 5696.23 379.66 0 -4 0 4969.20 382.86 -1 -4 0 1.70 0.70 1 -4 0 1.10 2.40 -1 4 0 3.70 2.40 -1 4 0 -0.60 1.10 -1 -4 0 0.80 1.50 1 -4 0 0.30 1.20 1 4 0 0.50 1.60 2 -4 0 4370.26 331.87 -2 -4 0 4660.53 328.67 -2 -4 0 4432.46 328.87 2 -4 0 4797.12 331.37 -2 4 0 4576.34 332.47 -2 -4 0 4481.55 329.07 2 4 0 4501.65 329.07 2 -4 0 4215.18 331.57 2 4 0 4939.71 328.57 -3 -4 0 3.80 1.70 -3 4 0 -0.70 2.80 -3 -4 0 1.90 1.40 3 -4 0 -0.20 2.60 3 -4 0 -0.20 2.60 -3 4 0 2.20 2.50 3 4 0 -2.70 1.40 -3 -4 0 -0.70 1.60 3 -4 0 1.00 2.90 -4 4 0 937.21 73.19 4 -4 0 907.81 72.59 -4 4 0 910.41 71.79 4 4 0 862.81 69.89 4 -4 0 910.91 71.29 4 -4 0 802.82 70.19 5 -4 0 3.40 4.20 -5 -4 0 1.10 2.80 5 -4 0 1.00 3.20 5 4 0 1.30 2.80 -5 4 0 4.80 4.30 -5 4 0 -4.40 3.80 5 -4 0 -2.00 3.30 6 -4 0 4.80 5.50 -6 4 0 4.40 6.50 6 -4 0 10.30 6.60 6 -4 0 6.00 6.20 -6 -4 0 5.40 4.30 -6 4 0 11.20 6.20 7 -4 0 14.40 8.00 -7 -4 0 5.80 5.70 -7 4 0 9.40 6.80 7 -4 0 -0.40 4.50 8 -4 0 -1.30 4.10 -8 -4 0 -2.30 5.90 -8 4 0 14.30 7.30 8 -4 0 -1.80 8.20 9 -4 0 -2.30 4.60 -9 4 0 -11.80 7.10 -9 -4 0 9.20 6.40 -10 4 0 -12.00 10.30 -10 -4 0 7.30 9.90 10 -4 0 4.80 6.20 0 -5 0 4.50 2.60 0 5 0 2.80 2.80 0 5 0 2.20 0.90 1 -5 0 2.10 1.50 1 5 0 2.00 2.50 -1 -5 0 -0.20 1.90 -1 5 0 0.20 2.40 -1 5 0 -1.70 1.20 1 -5 0 -2.40 2.00 -1 -5 0 2.40 2.40 2 -5 0 408.06 34.20 -2 5 0 412.36 34.20 -2 -5 0 402.56 33.00 -2 5 0 406.96 36.30 -2 -5 0 387.46 33.00 -2 -5 0 430.76 31.30 2 -5 0 374.56 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11.90 4 2 35 -1.40 7.00 -4 -2 35 6.90 7.10 0 3 35 -12.50 6.20 0 -3 35 0.10 7.90 -1 3 35 -5.90 5.90 1 -3 35 2.40 6.60 -1 3 -35 -0.50 6.80 -1 -3 35 -9.10 5.80 1 3 35 3.40 7.40 -2 -3 -35 -1.40 8.10 2 -3 35 -7.20 6.60 -2 3 35 9.20 7.80 -2 -3 35 3.40 8.10 -2 3 -35 9.40 8.70 2 3 35 5.00 8.30 -3 3 35 0.20 13.50 -3 -3 -35 -2.40 8.40 -3 3 -35 -6.30 9.70 -3 -3 35 -6.50 6.30 3 3 35 7.20 7.40 4 -3 35 10.00 9.50 -4 3 35 -2.60 8.30 -4 -3 -35 -3.20 9.00 4 3 35 9.40 8.80 -4 -3 35 3.50 5.90 -4 3 -35 2.80 10.60 0 4 35 8.80 8.40 0 -4 35 15.20 9.10 -1 4 35 7.50 7.10 1 -4 35 -3.60 7.10 -1 4 -35 -1.90 7.90 -1 -4 35 10.30 8.80 1 4 35 9.50 9.70 -2 4 35 13.00 17.70 -2 -4 35 -1.20 7.10 2 4 35 14.30 9.80 -2 4 -35 -7.60 9.20 -3 4 35 -1.80 7.20 3 -4 35 4.90 8.50 -3 4 -35 -2.80 10.70 -3 -4 35 5.70 9.20 3 4 35 -2.30 5.90 0 -5 35 -7.90 6.40 1 -5 35 -6.70 12.10 -1 5 -35 -3.80 9.10 -1 -5 35 -6.70 5.90 1 5 35 6.20 9.40 2 -5 35 2.40 7.60 -2 5 35 -5.90 9.50 -2 -5 -35 -4.10 7.50 2 5 35 7.80 10.80 -2 -5 35 -5.00 6.70 3 -5 35 17.40 12.50 -3 -5 -35 2.50 7.70 -3 5 35 18.40 11.70 -3 -5 35 12.00 8.10 0 -6 35 24.80 11.90 0 6 35 27.50 12.10 1 -6 35 10.60 10.40 -1 6 35 10.40 11.40 1 6 35 8.50 9.30 -1 -6 35 -3.40 8.40 -2 6 35 2.70 11.10 2 -6 35 22.80 10.90 2 6 35 3.70 7.90 -2 -6 35 36.20 12.40 0 7 35 -6.60 9.30 0 -7 35 -7.60 7.00 -1 7 35 -15.70 7.70 1 -7 35 8.70 11.00 -1 -7 35 -4.10 7.40 1 7 35 6.50 10.50 0 0 36 4.70 8.30 -1 0 -36 5.20 9.20 1 0 36 -6.00 6.40 -1 0 36 5.00 7.10 2 0 36 -5.10 7.70 -2 0 -36 -6.80 8.40 -2 0 36 16.40 8.30 3 0 36 28.30 18.70 -3 0 -36 -3.10 10.70 -3 0 36 33.20 19.60 0 -1 36 6.60 8.40 0 1 36 1.80 7.90 1 -1 36 31.80 11.30 -1 -1 -36 49.10 14.00 -1 1 36 4.00 9.80 -1 1 -36 4.60 8.50 -1 -1 36 27.90 12.00 1 1 36 26.10 11.90 2 -1 36 -3.80 9.00 -2 -1 -36 8.70 11.20 -2 1 36 11.50 8.30 2 1 36 4.40 8.20 -2 -1 36 3.20 7.80 -2 1 -36 -1.60 7.30 3 -1 36 38.10 14.10 -3 -1 -36 25.70 14.20 -3 1 36 3.00 16.90 -3 -1 36 26.40 13.20 -3 1 -36 28.50 13.90 0 -2 36 1.50 7.60 0 2 36 4.60 8.70 1 -2 36 -1.40 7.60 -1 2 36 5.90 7.70 1 2 36 -11.10 6.80 -1 2 -36 -11.90 7.20 -1 -2 36 -8.40 6.10 -2 -2 -36 3.60 8.60 2 -2 36 -3.30 14.50 -2 2 -36 11.30 8.40 -2 -2 36 -10.00 5.80 2 2 36 -3.10 6.90 -3 -2 -36 16.20 12.30 -3 2 36 0.80 9.40 3 -2 36 14.90 10.70 -3 2 -36 0.30 14.40 -3 -2 36 6.00 9.20 0 -3 36 -7.60 6.40 0 3 36 6.20 12.30 -1 -3 36 39.40 12.20 -1 3 -36 9.80 11.20 1 3 36 31.80 15.80 -2 3 36 -1.10 7.20 2 -3 36 2.90 7.00 -2 -3 -36 -5.70 8.90 -2 3 -36 -9.60 8.50 -2 -3 36 11.20 9.10 3 -3 36 39.20 13.40 -3 -3 -36 19.90 12.40 -3 3 36 42.10 13.80 3 3 36 22.40 11.80 -3 3 -36 9.40 13.30 0 -4 36 7.20 10.00 0 4 36 -11.40 7.40 1 -4 36 -1.70 7.30 -1 4 36 -1.50 9.20 -1 -4 36 -2.80 12.00 -1 4 -36 -1.00 9.50 1 4 36 -1.60 10.40 2 -4 36 9.00 8.40 -2 -4 -36 -5.30 8.10 -2 4 36 2.30 8.50 2 4 36 2.00 9.60 -2 -4 36 -17.70 10.60 -2 4 -36 4.50 9.10 3 -4 36 8.80 9.10 -3 -4 -36 -0.50 8.50 -3 4 36 9.40 9.50 3 4 36 3.90 8.80 -3 -4 36 -1.10 7.30 0 -5 36 2.60 7.90 0 5 36 -5.90 8.60 -1 5 36 12.90 12.80 1 -5 36 10.00 11.50 1 5 36 11.60 9.90 -1 -5 36 30.40 13.00 -2 -5 -36 0.90 7.80 -2 5 36 5.90 9.90 2 -5 36 6.30 9.70 2 5 36 2.50 8.40 -2 -5 36 -1.60 7.90 0 6 36 -8.70 8.20 0 -6 36 -6.30 8.10 1 -6 36 -5.60 8.30 -1 6 36 -0.80 10.40 -1 -6 36 2.30 10.10 1 6 36 -10.60 8.20 0 0 37 -3.80 6.90 -1 0 37 -10.60 7.10 -1 0 -37 -0.40 7.80 1 0 37 2.10 8.00 -2 0 37 -9.90 7.40 2 0 37 0.50 7.80 -2 0 -37 16.30 11.40 -3 0 -37 -9.60 10.90 -3 0 37 17.50 9.70 3 0 37 -7.80 8.00 0 -1 37 0.90 6.50 0 1 37 16.20 8.80 -1 1 37 -0.40 7.60 1 -1 37 4.20 6.90 -1 1 -37 4.80 6.70 1 1 37 10.70 10.10 2 -1 37 7.80 9.30 -2 1 37 -12.20 6.60 -2 -1 -37 9.90 11.40 -2 -1 37 -1.60 8.00 2 1 37 -12.80 6.80 -2 1 -37 -0.10 9.80 -3 1 37 1.00 7.70 -3 -1 -37 -12.30 8.80 3 -1 37 12.40 7.90 -3 -1 37 1.60 8.60 -3 1 -37 1.80 11.30 3 1 37 0.30 7.80 0 2 37 -5.80 7.60 0 -2 37 -2.70 7.20 1 -2 37 13.30 9.20 -1 2 37 0.10 9.70 1 2 37 -15.70 6.50 -1 -2 37 -1.20 7.80 -1 2 -37 -2.60 9.70 2 -2 37 6.70 10.30 -2 -2 -37 -15.30 7.10 -2 2 37 4.00 8.20 -2 -2 37 -6.40 9.20 2 2 37 -8.20 7.20 -2 2 -37 0.90 8.20 0 -3 37 -15.20 7.50 0 3 37 2.10 7.80 -1 3 37 -1.60 8.20 1 -3 37 -8.00 7.90 1 3 37 -7.80 7.30 -1 3 -37 5.10 9.20 -1 -3 37 -11.20 7.10 -2 3 37 7.90 9.90 2 -3 37 0.80 8.90 -2 -3 37 -3.20 7.50 -2 3 -37 12.30 10.40 2 3 37 5.50 8.30 0 -4 37 -3.70 8.60 0 4 37 -12.00 7.80 1 -4 37 2.70 8.50 -1 4 37 -3.80 8.10 1 4 37 -3.00 9.30 -1 -4 37 -1.70 9.10 0 5 37 -13.20 7.70 0 -5 37 0.10 8.90 0 0 38 -1.30 10.10 1 0 38 5.20 9.30 -1 0 38 -9.60 8.20 0 1 38 -2.10 8.10 0 -1 38 1.10 7.90 1 -1 38 25.90 12.00 -1 1 38 -4.50 9.50 1 1 38 9.10 12.20 -1 -1 38 15.60 8.60 0 -2 38 13.90 9.60 0 2 38 1.60 7.10 -1 2 38 -4.40 8.70 1 -2 38 0.40 8.40 1 2 38 1.90 8.80 -1 -2 38 -3.70 7.30 0 -3 38 3.50 8.70 0 3 38 -4.30 9.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 72681 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.47926(10) 0.77222(6) 0.54798(3) 0.0708(4) Uani 1 1 d D U . . . F1 F 0.3309(7) 0.6073(3) 0.55703(16) 0.1063(15) Uani 0.6 1 d . U P A 1 F2 F 0.4187(11) 0.6481(6) 0.48862(17) 0.122(2) Uani 0.5 1 d . U P A 1 C9 C 0.3573(8) 0.6780(5) 0.5279(2) 0.0899(17) Uani 0.8 1 d . U P A 1 H9 H 0.2521 0.7078 0.5213 0.108 Uiso 0.8 1 calc R U P A 1 F1' F 0.4569(15) 0.5961(9) 0.5112(5) 0.178(5) Uani 0.4 1 d . U P A 2 F2' F 0.2514(18) 0.6564(10) 0.5213(6) 0.255(6) Uani 0.5 1 d . U P A 2 C9' C 0.390(4) 0.6445(16) 0.5448(11) 0.091(6) Uani 0.2 1 d D U P A 2 H9' H 0.3816 0.6085 0.5733 0.109 Uiso 0.2 1 calc R U P A 2 N1 N 0.1761(3) 0.91805(19) 0.62356(11) 0.0756(8) Uani 1 1 d . . . . . B1 B 0.5894(3) 0.6630(2) 0.64787(10) 0.0464(7) Uani 1 1 d . . . . . C1 C 0.2415(3) 0.8599(2) 0.65700(11) 0.0604(7) Uani 1 1 d . . . . . C2 C 0.2084(4) 0.8570(3) 0.70284(12) 0.0766(10) Uani 1 1 d . . . . . H2 H 0.1316 0.8987 0.7156 0.092 Uiso 1 1 calc R U . . . C3 C 0.2918(4) 0.7915(3) 0.72828(12) 0.0794(10) Uani 1 1 d . . . . . H3 H 0.2712 0.7878 0.7590 0.095 Uiso 1 1 calc R U . . . C4 C 0.4085(4) 0.7292(2) 0.70927(11) 0.0670(8) Uani 1 1 d . . . . . H4 H 0.4633 0.6853 0.7279 0.080 Uiso 1 1 calc R U . . . C5 C 0.4461(3) 0.73026(18) 0.66375(9) 0.0504(6) Uani 1 1 d . . . . . C6 C 0.3573(3) 0.79722(18) 0.63703(9) 0.0493(6) Uani 1 1 d . . . . . C7 C 0.3558(3) 0.8209(2) 0.58996(10) 0.0569(7) Uani 1 1 d . . . . . C8 C 0.2452(4) 0.8939(2) 0.58390(13) 0.0714(9) Uani 1 1 d . . . . . H8 H 0.2205 0.9230 0.5564 0.086 Uiso 1 1 calc R U . . . O1 O 0.7506(8) 0.6876(5) 0.6595(2) 0.0694(14) Uani 0.5 1 d . U P B 1 O2 O 0.574(3) 0.5667(18) 0.6427(6) 0.0715(17) Uani 0.5 1 d . U P B 1 C10 C 0.8511(12) 0.6072(8) 0.6405(4) 0.0756(14) Uani 0.5 1 d . U P B 1 C11 C 0.7443(15) 0.5304(9) 0.6287(4) 0.0738(15) Uani 0.5 1 d . U P B 1 C12 C 0.7544(10) 0.4623(7) 0.5924(4) 0.091(2) Uani 0.5 1 d . U P B 1 H12A H 0.7366 0.4967 0.5646 0.137 Uiso 0.5 1 calc R U P B 1 H12B H 0.6737 0.4119 0.5960 0.137 Uiso 0.5 1 calc R U P B 1 H12C H 0.8595 0.4324 0.5920 0.137 Uiso 0.5 1 calc R U P B 1 C13 C 0.7518(10) 0.4582(6) 0.6750(4) 0.095(2) Uani 0.5 1 d . U P B 1 H13A H 0.6858 0.4006 0.6704 0.142 Uiso 0.5 1 calc R U P B 1 H13B H 0.7124 0.4947 0.7004 0.142 Uiso 0.5 1 calc R U P B 1 H13C H 0.8614 0.4382 0.6804 0.142 Uiso 0.5 1 calc R U P B 1 C14 C 0.9973(10) 0.6029(7) 0.6657(4) 0.088(2) Uani 0.5 1 d . U P B 1 H14A H 0.9740 0.5823 0.6959 0.132 Uiso 0.5 1 calc R U P B 1 H14B H 1.0467 0.6672 0.6662 0.132 Uiso 0.5 1 calc R U P B 1 H14C H 1.0697 0.5563 0.6520 0.132 Uiso 0.5 1 calc R U P B 1 C15 C 0.9056(11) 0.6524(6) 0.5897(4) 0.101(2) Uani 0.5 1 d . U P B 1 H15A H 0.9798 0.6075 0.5756 0.152 Uiso 0.5 1 calc R U P B 1 H15B H 0.9564 0.7157 0.5935 0.152 Uiso 0.5 1 calc R U P B 1 H15C H 0.8114 0.6596 0.5712 0.152 Uiso 0.5 1 calc R U P B 1 O1' O 0.7328(8) 0.6965(5) 0.6372(2) 0.0745(15) Uani 0.5 1 d . U P B 2 O2' O 0.582(3) 0.5686(18) 0.6335(5) 0.0713(17) Uani 0.5 1 d . U P B 2 C10' C 0.8382(12) 0.6167(7) 0.6247(3) 0.077(2) Uani 0.5 1 d . U P B 2 C11' C 0.7416(16) 0.5246(9) 0.6420(4) 0.074(2) Uani 0.5 1 d . U P B 2 C12' C 0.7416(10) 0.4273(5) 0.6229(4) 0.089(2) Uani 0.5 1 d . U P B 2 H12D H 0.6898 0.3821 0.6433 0.133 Uiso 0.5 1 calc R U P B 2 H12E H 0.8508 0.4064 0.6178 0.133 Uiso 0.5 1 calc R U P B 2 H12F H 0.6840 0.4282 0.5949 0.133 Uiso 0.5 1 calc R U P B 2 C13' C 0.8071(12) 0.5178(8) 0.6957(3) 0.106(2) Uani 0.5 1 d . U P B 2 H13D H 0.7163 0.5205 0.7157 0.159 Uiso 0.5 1 calc R U P B 2 H13E H 0.8782 0.5724 0.7018 0.159 Uiso 0.5 1 calc R U P B 2 H13F H 0.8641 0.4567 0.7001 0.159 Uiso 0.5 1 calc R U P B 2 C14' C 1.0025(10) 0.6304(7) 0.6378(4) 0.100(3) Uani 0.5 1 d . U P B 2 H14D H 1.0479 0.6849 0.6215 0.149 Uiso 0.5 1 calc R U P B 2 H14E H 1.0627 0.5713 0.6314 0.149 Uiso 0.5 1 calc R U P B 2 H14F H 1.0073 0.6440 0.6695 0.149 Uiso 0.5 1 calc R U P B 2 C15' C 0.8107(12) 0.5894(8) 0.5696(3) 0.111(3) Uani 0.5 1 d . U P B 2 H15D H 0.7215 0.5444 0.5665 0.167 Uiso 0.5 1 calc R U P B 2 H15E H 0.9067 0.5592 0.5578 0.167 Uiso 0.5 1 calc R U P B 2 H15F H 0.7881 0.6491 0.5532 0.167 Uiso 0.5 1 calc R U P B 2 H1A H 0.090(6) 0.973(4) 0.6271(16) 0.135(16) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0679(6) 0.0731(6) 0.0713(6) -0.0006(4) 0.0122(4) -0.0045(4) F1 0.138(4) 0.058(2) 0.122(3) 0.017(2) -0.031(3) -0.036(2) F2 0.168(6) 0.137(6) 0.062(3) -0.050(3) 0.007(3) 0.000(5) C9 0.083(3) 0.095(4) 0.092(4) -0.024(3) -0.014(3) -0.002(3) F1' 0.168(8) 0.143(8) 0.222(12) -0.119(8) 0.023(9) 0.012(7) F2' 0.235(10) 0.229(10) 0.299(12) -0.080(10) -0.061(11) -0.027(10) C9' 0.096(11) 0.086(7) 0.090(11) -0.013(9) -0.009(9) -0.018(8) N1 0.0523(14) 0.0539(14) 0.121(2) -0.0148(15) -0.0101(15) 0.0151(11) B1 0.0414(14) 0.0395(14) 0.0582(16) 0.0009(11) 0.0023(11) -0.0022(11) C1 0.0364(13) 0.0497(14) 0.095(2) -0.0184(14) -0.0005(13) 0.0026(11) C2 0.0490(16) 0.081(2) 0.099(3) -0.0389(19) 0.0131(16) 0.0065(15) C3 0.0636(19) 0.099(3) 0.076(2) -0.0244(19) 0.0155(16) -0.0004(18) C4 0.0566(17) 0.075(2) 0.0690(19) -0.0042(15) 0.0092(14) 0.0031(14) C5 0.0403(12) 0.0448(13) 0.0659(16) -0.0064(11) 0.0046(11) -0.0028(10) C6 0.0316(11) 0.0411(12) 0.0752(17) -0.0122(11) 0.0016(10) -0.0029(9) C7 0.0473(14) 0.0478(14) 0.0757(18) -0.0024(12) -0.0019(12) -0.0003(11) C8 0.0628(18) 0.0583(17) 0.093(2) 0.0020(16) -0.0088(17) 0.0067(14) O1 0.0369(17) 0.0478(19) 0.123(4) -0.027(3) -0.002(3) 0.0013(14) O2 0.038(2) 0.0456(17) 0.131(5) -0.023(4) 0.002(3) 0.0001(16) C10 0.0423(18) 0.053(2) 0.131(4) -0.021(3) 0.005(2) 0.0046(17) C11 0.0398(19) 0.0494(19) 0.132(4) -0.024(3) 0.003(3) 0.0027(17) C12 0.067(4) 0.077(4) 0.131(5) -0.046(4) 0.007(4) 0.006(3) C13 0.072(4) 0.066(4) 0.146(5) 0.022(4) -0.004(4) 0.011(3) C14 0.051(3) 0.074(4) 0.137(5) -0.021(4) -0.020(4) 0.003(3) C15 0.082(4) 0.081(4) 0.141(5) 0.009(4) 0.045(4) 0.007(3) O1' 0.0414(19) 0.0480(18) 0.134(4) -0.012(3) 0.012(3) 0.0005(15) O2' 0.037(2) 0.0464(17) 0.130(5) -0.027(4) 0.001(3) 0.0009(16) C10' 0.054(3) 0.057(3) 0.120(5) 0.020(3) 0.029(3) 0.020(2) C11' 0.053(3) 0.051(3) 0.118(5) 0.018(3) 0.014(3) 0.018(2) C12' 0.064(4) 0.046(3) 0.157(6) -0.005(4) 0.014(4) 0.015(3) C13' 0.105(5) 0.098(5) 0.116(5) 0.026(5) -0.014(4) 0.027(4) C14' 0.051(4) 0.075(5) 0.173(7) -0.003(5) 0.021(5) -0.005(3) C15' 0.108(5) 0.121(6) 0.105(5) 0.014(5) 0.036(5) 0.045(5) 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 S1 C7 100.5(2) . . ? C7 S1 C9' 98.8(10) . . ? F1 C9 F2 115.0(6) . . ? F1 C9 S1 114.0(5) . . ? F2 C9 S1 107.6(6) . . ? F1 C9 H9 106.6 . . ? F2 C9 H9 106.6 . . ? S1 C9 H9 106.6 . . ? F1' C9' F2' 91(2) . . ? F1' C9' S1 109.4(18) . . ? F2' C9' S1 104.4(19) . . ? F1' C9' H9' 116.2 . . ? F2' C9' H9' 116.2 . . ? S1 C9' H9' 116.2 . . ? C8 N1 C1 109.0(3) . . ? C8 N1 H1A 124(3) . . ? C1 N1 H1A 127(3) . . ? O1' B1 O2' 107.1(10) . . ? O2 B1 O1 110.6(11) . . ? O1' B1 C5 124.0(4) . . ? O2 B1 C5 122.4(10) . . ? O2' B1 C5 127.5(10) . . ? O1 B1 C5 120.2(3) . . ? N1 C1 C2 130.2(3) . . ? N1 C1 C6 107.8(3) . . ? C2 C1 C6 122.0(3) . . ? C3 C2 C1 117.8(3) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C2 C3 C4 121.2(3) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 122.8(3) . . ? C5 C4 H4 118.6 . . ? C3 C4 H4 118.6 . . ? C4 C5 C6 116.0(2) . . ? C4 C5 B1 117.2(2) . . ? C6 C5 B1 126.6(2) . . ? C1 C6 C5 120.1(3) . . ? C1 C6 C7 105.8(2) . . ? C5 C6 C7 134.1(2) . . ? C8 C7 C6 107.3(3) . . ? C8 C7 S1 125.1(3) . . ? C6 C7 S1 127.6(2) . . ? N1 C8 C7 110.2(3) . . ? N1 C8 H8 124.9 . . ? C7 C8 H8 124.9 . . ? B1 O1 C10 105.3(5) . . ? B1 O2 C11 104.8(16) . . ? C11 C10 C14 129.4(11) . . ? C11 C10 O1 106.4(9) . . ? C14 C10 O1 107.9(7) . . ? C11 C10 C15 102.2(9) . . ? C14 C10 C15 105.0(8) . . ? O1 C10 C15 103.0(7) . . ? C10 C11 C12 129.0(11) . . ? C10 C11 O2 105.7(14) . . ? C12 C11 O2 117.5(13) . . ? C10 C11 C13 101.5(9) . . ? C12 C11 C13 104.2(9) . . ? O2 C11 C13 89.8(10) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? B1 O1' C10' 110.8(6) . . ? B1 O2' C11' 106.5(17) . . ? C14' C10' O1' 114.3(9) . . ? C14' C10' C11' 119.9(9) . . ? O1' C10' C11' 101.6(8) . . ? C14' C10' C15' 114.9(8) . . ? O1' C10' C15' 109.4(6) . . ? C11' C10' C15' 94.4(10) . . ? C12' C11' O2' 107.5(15) . . ? C12' C11' C10' 126.7(10) . . ? O2' C11' C10' 94.7(13) . . ? C12' C11' C13' 109.0(8) . . ? O2' C11' C13' 118.3(12) . . ? C10' C11' C13' 101.0(10) . . ? C11' C12' H12D 109.5 . . ? C11' C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C11' C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? C11' C13' H13D 109.5 . . ? C11' C13' H13E 109.5 . . ? H13D C13' H13E 109.5 . . ? C11' C13' H13F 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? C10' C14' H14D 109.5 . . ? C10' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C10' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? C10' C15' H15D 109.5 . . ? C10' C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? C10' C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C9 1.731(6) . ? S1 C7 1.743(3) . ? S1 C9' 1.878(18) . ? F1 C9 1.308(8) . ? F2 C9 1.338(9) . ? C9 H9 0.9800 . ? F1' C9' 1.31(3) . ? F2' C9' 1.36(3) . ? C9' H9' 0.9800 . ? N1 C8 1.352(5) . ? N1 C1 1.379(4) . ? N1 H1A 1.03(5) . ? B1 O1' 1.310(8) . ? B1 O2 1.32(2) . ? B1 O2' 1.35(2) . ? B1 O1 1.418(7) . ? B1 C5 1.567(4) . ? C1 C2 1.392(5) . ? C1 C6 1.410(3) . ? C2 C3 1.353(5) . ? C2 H2 0.9300 . ? C3 C4 1.401(4) . ? C3 H3 0.9300 . ? C4 C5 1.390(4) . ? C4 H4 0.9300 . ? C5 C6 1.411(4) . ? C6 C7 1.437(4) . ? C7 C8 1.357(4) . ? C8 H8 0.9300 . ? O1 C10 1.480(11) . ? O2 C11 1.55(3) . ? C10 C11 1.408(17) . ? C10 C14 1.425(12) . ? C10 C15 1.691(14) . ? C11 C12 1.422(13) . ? C11 C13 1.688(14) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? O1' C10' 1.435(10) . ? O2' C11' 1.47(3) . ? C10' C14' 1.427(14) . ? C10' C11' 1.567(17) . ? C10' C15' 1.696(15) . ? C11' C12' 1.432(15) . ? C11' C13' 1.688(14) . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C12' H12F 0.9600 . ? C13' H13D 0.9600 . ? C13' H13E 0.9600 . ? C13' H13F 0.9600 . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15' H15D 0.9600 . ? C15' H15E 0.9600 . ? C15' H15F 0.9600 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 S1 C9 F1 -65.6(5) . . . . ? C9' S1 C9 F1 22(3) . . . . ? C7 S1 C9 F2 165.7(5) . . . . ? C9' S1 C9 F2 -107(3) . . . . ? C9 S1 C9' F1' 78(3) . . . . ? C7 S1 C9' F1' 173.9(19) . . . . ? C9 S1 C9' F2' -18.9(15) . . . . ? C7 S1 C9' F2' 77(2) . . . . ? C8 N1 C1 C2 -179.5(3) . . . . ? C8 N1 C1 C6 0.4(3) . . . . ? N1 C1 C2 C3 179.9(3) . . . . ? C6 C1 C2 C3 0.1(4) . . . . ? C1 C2 C3 C4 0.5(5) . . . . ? C2 C3 C4 C5 -0.1(5) . . . . ? C3 C4 C5 C6 -1.0(4) . . . . ? C3 C4 C5 B1 174.9(3) . . . . ? O1' B1 C5 C4 -104.8(4) . . . . ? O2 B1 C5 C4 77.5(10) . . . . ? O2' B1 C5 C4 90.9(10) . . . . ? O1 B1 C5 C4 -70.7(5) . . . . ? O1' B1 C5 C6 70.7(5) . . . . ? O2 B1 C5 C6 -107.0(10) . . . . ? O2' B1 C5 C6 -93.6(10) . . . . ? O1 B1 C5 C6 104.8(4) . . . . ? N1 C1 C6 C5 178.9(2) . . . . ? C2 C1 C6 C5 -1.2(4) . . . . ? N1 C1 C6 C7 -0.5(3) . . . . ? C2 C1 C6 C7 179.4(3) . . . . ? C4 C5 C6 C1 1.6(4) . . . . ? B1 C5 C6 C1 -173.9(2) . . . . ? C4 C5 C6 C7 -179.2(3) . . . . ? B1 C5 C6 C7 5.2(4) . . . . ? C1 C6 C7 C8 0.4(3) . . . . ? C5 C6 C7 C8 -178.9(3) . . . . ? C1 C6 C7 S1 176.9(2) . . . . ? C5 C6 C7 S1 -2.3(4) . . . . ? C9 S1 C7 C8 -89.2(4) . . . . ? C9' S1 C7 C8 -112.3(11) . . . . ? C9 S1 C7 C6 94.8(4) . . . . ? C9' S1 C7 C6 71.7(11) . . . . ? C1 N1 C8 C7 -0.2(4) . . . . ? C6 C7 C8 N1 -0.1(3) . . . . ? S1 C7 C8 N1 -176.8(2) . . . . ? O1' B1 O1 C10 -75.4(11) . . . . ? O2 B1 O1 C10 26.5(10) . . . . ? O2' B1 O1 C10 13.6(10) . . . . ? C5 B1 O1 C10 178.1(5) . . . . ? O1' B1 O2 C11 4.2(14) . . . . ? O2' B1 O2 C11 63(9) . . . . ? O1 B1 O2 C11 -27.0(14) . . . . ? C5 B1 O2 C11 -177.9(7) . . . . ? B1 O1 C10 C11 -13.5(10) . . . . ? B1 O1 C10 C14 -155.7(8) . . . . ? B1 O1 C10 C15 93.6(7) . . . . ? C14 C10 C11 C12 -82.8(19) . . . . ? O1 C10 C11 C12 146.2(12) . . . . ? C15 C10 C11 C12 38.5(16) . . . . ? C14 C10 C11 O2 129.4(14) . . . . ? O1 C10 C11 O2 -1.7(15) . . . . ? C15 C10 C11 O2 -109.3(11) . . . . ? C14 C10 C11 C13 36.3(16) . . . . ? O1 C10 C11 C13 -94.7(9) . . . . ? C15 C10 C11 C13 157.6(6) . . . . ? B1 O2 C11 C10 17.4(17) . . . . ? B1 O2 C11 C12 -134.8(12) . . . . ? B1 O2 C11 C13 119.3(11) . . . . ? O2 B1 O1' C10' -3.0(11) . . . . ? O2' B1 O1' C10' -13.9(11) . . . . ? O1 B1 O1' C10' 87.1(12) . . . . ? C5 B1 O1' C10' 179.1(5) . . . . ? O1' B1 O2' C11' 38.5(14) . . . . ? O2 B1 O2' C11' -86(9) . . . . ? O1 B1 O2' C11' 8.1(14) . . . . ? C5 B1 O2' C11' -155.0(8) . . . . ? B1 O1' C10' C14' -144.7(8) . . . . ? B1 O1' C10' C11' -14.1(9) . . . . ? B1 O1' C10' C15' 84.8(8) . . . . ? B1 O2' C11' C12' -174.3(8) . . . . ? B1 O2' C11' C10' -43.3(14) . . . . ? B1 O2' C11' C13' 61.9(18) . . . . ? C14' C10' C11' C12' -84.2(15) . . . . ? O1' C10' C11' C12' 148.8(10) . . . . ? C15' C10' C11' C12' 38.0(13) . . . . ? C14' C10' C11' O2' 159.8(11) . . . . ? O1' C10' C11' O2' 32.8(13) . . . . ? C15' C10' C11' O2' -78.0(11) . . . . ? C14' C10' C11' C13' 39.8(13) . . . . ? O1' C10' C11' C13' -87.2(8) . . . . ? C15' C10' C11' C13' 162.0(7) . . . . ?