#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:23:27 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242504 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132534.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_4132534 loop_ _publ_author_name 'Li, Ke' 'Li, Mao-Lin' 'Zhang, Qi' 'Zhu, Shou-Fei' 'Zhou, Qi-Lin' _publ_section_title ; Highly Enantioselective Nickel-Catalyzed Intramolecular Hydroalkenylation of N- and O-Tethered 1,6-Dienes To Form Six-Membered Heterocycles. ; _journal_issue 24 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 7458 _journal_page_last 7461 _journal_paper_doi 10.1021/jacs.8b04703 _journal_volume 140 _journal_year 2018 _chemical_absolute_configuration ad _chemical_formula_moiety 'C26 H29 N O4 S' _chemical_formula_sum 'C26 H29 N O4 S' _chemical_formula_weight 451.56 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2017-03-21 _audit_creation_method ; Olex2 1.2 (compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.3584(4) _cell_length_b 14.8160(5) _cell_length_c 18.9753(6) _cell_measurement_reflns_used 12664 _cell_measurement_temperature 113.15 _cell_measurement_theta_max 31.7280 _cell_measurement_theta_min 1.7930 _cell_volume 2349.86(16) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (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_temperature 113.15 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _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 -115.00 65.00 1.00 1.00 -- -25.00 45.00 0.00 180 2 \w -115.00 65.00 1.00 1.00 -- -25.00 45.00 90.00 180 3 \w -115.00 65.00 1.00 1.00 -- -25.00 45.00 180.00 180 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'Rigaku Saturn 70' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0033333000 _diffrn_orient_matrix_UB_12 0.0416441000 _diffrn_orient_matrix_UB_13 0.0183858000 _diffrn_orient_matrix_UB_21 0.0012724000 _diffrn_orient_matrix_UB_22 -0.0235624000 _diffrn_orient_matrix_UB_23 0.0325140000 _diffrn_orient_matrix_UB_31 0.0848199000 _diffrn_orient_matrix_UB_32 -0.0012877000 _diffrn_orient_matrix_UB_33 -0.0012256000 _diffrn_radiation_monochromator confocal _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_unetI/netI 0.0502 _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 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 28302 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.998 _diffrn_reflns_theta_min 1.744 _diffrn_source 'rotating anode' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.170 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.71184 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.276 _exptl_crystal_description prism _exptl_crystal_F_000 960 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.358 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.119 _refine_ls_abs_structure_details ; Flack x determined using 1792 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.01(5) _refine_ls_extinction_coef 0.047(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 292 _refine_ls_number_reflns 5649 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0469 _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^)+(0.0580P)^2^+0.1670P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1096 _refine_ls_wR_factor_ref 0.1170 _reflns_Friedel_coverage 0.770 _reflns_Friedel_fraction_full 0.997 _reflns_Friedel_fraction_max 0.997 _reflns_number_gt 4906 _reflns_number_total 5649 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04703_si_004.cif _cod_data_source_block r20170321a _cod_database_code 4132534 _shelx_shelxl_version_number 2016/6 _chemical_oxdiff_formula C26H29NO4S _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 0.977 _shelx_estimated_absorpt_t_min 0.944 _reflns_odcompleteness_completeness 95.14 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 32.83 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C2(H2), C3(H3) 2.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B) 2.c Aromatic/amide H refined with riding coordinates: C8(H8), C9(H9), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24), C25(H25) 2.d Idealised Me refined as rotating group: C13(H13A,H13B,H13C), C26(H26A,H26B,H26C) ; _shelx_res_file ; TITL r20170321a_a.res in P2(1)2(1)2(1) r20170321a.res created by SHELXL-2016/6 at 11:47:27 on 21-Mar-2017 REM Old TITL r20170321a in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.110, Rweak 0.030, Alpha 0.004, Orientation as input REM Flack x = 0.114 ( 0.057 ) from Parsons' quotients REM Formula found by SHELXT: C25 N2 O4 S CELL 0.71073 8.3584 14.816 18.9753 90 90 90 ZERR 4 0.0004 0.0005 0.0006 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 S UNIT 104 116 4 16 4 L.S. 10 PLAN 20 SIZE 0.34 0.18 0.14 TEMP -160 BOND $H list 4 conf htab fmap 2 acta OMIT -3 56 REM REM REM WGHT 0.058000 0.167000 EXTI 0.047113 FVAR 1.04944 S1 5 0.523647 -0.032547 0.457226 11.00000 0.03851 0.02752 = 0.03113 -0.00313 -0.00382 -0.00267 O1 4 0.517958 0.313103 0.445379 11.00000 0.04428 0.02553 = 0.02301 0.00160 -0.00057 0.00044 O2 4 0.585068 0.636943 0.303760 11.00000 0.04320 0.02758 = 0.03140 0.00560 -0.00527 -0.00142 O3 4 0.453571 0.006617 0.395696 11.00000 0.05163 0.03919 = 0.03761 -0.00446 -0.01486 0.00259 O4 4 0.447204 -0.106299 0.492365 11.00000 0.04489 0.03121 = 0.04835 -0.00266 0.00236 -0.00884 N1 3 0.538719 0.048412 0.514822 11.00000 0.03611 0.02360 = 0.02614 -0.00034 -0.00015 -0.00114 C1 1 0.590513 0.137991 0.491646 11.00000 0.03321 0.02477 = 0.02614 -0.00087 0.00281 0.00025 AFIX 23 H1A 2 0.555169 0.148842 0.442576 11.00000 -1.20000 H1B 2 0.708689 0.142051 0.493143 11.00000 -1.20000 AFIX 0 C2 1 0.517223 0.208451 0.540588 11.00000 0.02368 0.02722 = 0.02272 0.00142 0.00004 0.00013 AFIX 13 H2 2 0.398231 0.202278 0.537987 11.00000 -1.20000 AFIX 0 C3 1 0.568352 0.191100 0.617601 11.00000 0.02700 0.02890 = 0.02361 -0.00007 -0.00410 0.00134 AFIX 13 H3 2 0.686951 0.199117 0.620590 11.00000 -1.20000 AFIX 0 C4 1 0.529371 0.093247 0.637951 11.00000 0.03865 0.02909 = 0.02336 0.00393 -0.00042 0.00211 AFIX 23 H4A 2 0.573839 0.080627 0.685293 11.00000 -1.20000 H4B 2 0.411793 0.085920 0.640582 11.00000 -1.20000 AFIX 0 C5 1 0.596474 0.025312 0.585859 11.00000 0.04007 0.02838 = 0.02744 0.00163 -0.00182 0.00262 AFIX 23 H5A 2 0.714863 0.026817 0.586918 11.00000 -1.20000 H5B 2 0.561068 -0.036306 0.598666 11.00000 -1.20000 AFIX 0 C6 1 0.560055 0.303368 0.518243 11.00000 0.02756 0.02663 = 0.02359 -0.00054 0.00111 0.00232 AFIX 23 H6A 2 0.500708 0.347791 0.547149 11.00000 -1.20000 H6B 2 0.676071 0.313951 0.524734 11.00000 -1.20000 AFIX 0 C7 1 0.542654 0.396461 0.414775 11.00000 0.02616 0.02537 = 0.02652 0.00126 0.00317 0.00278 C8 1 0.507578 0.401918 0.343085 11.00000 0.03016 0.02804 = 0.02701 -0.00416 -0.00121 0.00171 AFIX 43 H8 2 0.471657 0.349708 0.318706 11.00000 -1.20000 AFIX 0 C9 1 0.524416 0.482145 0.307208 11.00000 0.03014 0.03501 = 0.02387 0.00034 -0.00278 0.00145 AFIX 43 H9 2 0.501213 0.485072 0.258250 11.00000 -1.20000 AFIX 0 C10 1 0.575744 0.559199 0.343083 11.00000 0.02485 0.02685 = 0.02880 0.00368 0.00132 0.00403 C11 1 0.614973 0.553257 0.413605 11.00000 0.03026 0.02711 = 0.03062 -0.00324 -0.00317 -0.00022 AFIX 43 H11 2 0.653783 0.605038 0.437680 11.00000 -1.20000 AFIX 0 C12 1 0.598115 0.471878 0.449812 11.00000 0.03260 0.02962 = 0.02302 -0.00105 -0.00171 0.00203 AFIX 43 H12 2 0.624707 0.468369 0.498410 11.00000 -1.20000 AFIX 0 C13 1 0.613240 0.718545 0.341439 11.00000 0.06416 0.02798 = 0.04199 0.00064 0.00095 -0.00193 AFIX 137 H13A 2 0.603961 0.769954 0.309200 11.00000 -1.50000 H13B 2 0.720997 0.717279 0.361770 11.00000 -1.50000 H13C 2 0.534147 0.724551 0.379275 11.00000 -1.50000 AFIX 0 C14 1 0.491704 0.256471 0.668429 11.00000 0.02845 0.02478 = 0.02140 0.00222 -0.00102 0.00059 C15 1 0.325530 0.263821 0.672261 11.00000 0.03088 0.03263 = 0.02597 -0.00081 0.00108 -0.00484 AFIX 43 H15 2 0.260588 0.228172 0.642038 11.00000 -1.20000 AFIX 0 C16 1 0.254065 0.322496 0.719623 11.00000 0.03351 0.03316 = 0.02984 0.00423 0.00519 0.00332 AFIX 43 H16 2 0.140752 0.326665 0.721774 11.00000 -1.20000 AFIX 0 C17 1 0.347014 0.374918 0.763696 11.00000 0.04890 0.03375 = 0.02680 -0.00407 0.00081 0.00624 AFIX 43 H17 2 0.297827 0.414775 0.796386 11.00000 -1.20000 AFIX 0 C18 1 0.510967 0.369248 0.760118 11.00000 0.04540 0.03796 = 0.03449 -0.00983 -0.00751 0.00083 AFIX 43 H18 2 0.575059 0.405400 0.790329 11.00000 -1.20000 AFIX 0 C19 1 0.583391 0.310824 0.712468 11.00000 0.03323 0.03799 = 0.03181 -0.00463 -0.00509 -0.00092 AFIX 43 H19 2 0.696797 0.308002 0.709966 11.00000 -1.20000 AFIX 0 C20 1 0.716922 -0.069429 0.434580 11.00000 0.04132 0.02473 = 0.02711 -0.00481 -0.00058 -0.00279 C21 1 0.800854 -0.025744 0.381875 11.00000 0.06485 0.03153 = 0.03428 0.00675 0.00600 0.00502 AFIX 43 H21 2 0.756510 0.025795 0.359390 11.00000 -1.20000 AFIX 0 C22 1 0.949754 -0.057549 0.362099 11.00000 0.05777 0.04318 = 0.03818 -0.00147 0.01664 -0.00225 AFIX 43 H22 2 1.007202 -0.027160 0.326000 11.00000 -1.20000 AFIX 0 C23 1 1.017172 -0.132967 0.393865 11.00000 0.04238 0.03635 = 0.03826 -0.01530 -0.00114 -0.00275 C24 1 0.932048 -0.174096 0.447833 11.00000 0.04245 0.03013 = 0.04216 -0.00432 -0.00974 0.00136 AFIX 43 H24 2 0.977340 -0.224736 0.471180 11.00000 -1.20000 AFIX 0 C25 1 0.784160 -0.143567 0.468385 11.00000 0.04242 0.02867 = 0.03200 0.00205 -0.00460 -0.00509 AFIX 43 H25 2 0.728139 -0.172886 0.505445 11.00000 -1.20000 AFIX 0 C26 1 1.175429 -0.168674 0.369287 11.00000 0.04709 0.05955 = 0.06087 -0.02441 0.00227 -0.00101 AFIX 137 H26A 2 1.234110 -0.193756 0.409481 11.00000 -1.50000 H26B 2 1.237687 -0.119545 0.348222 11.00000 -1.50000 H26C 2 1.157951 -0.216063 0.334089 11.00000 -1.50000 AFIX 0 HKLF 4 REM r20170321a_a.res in P2(1)2(1)2(1) REM R1 = 0.0469 for 4906 Fo > 4sig(Fo) and 0.0563 for all 5649 data REM 292 parameters refined using 0 restraints END WGHT 0.0579 0.1819 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.358, deepest hole -0.355, 1-sigma level 0.119 Q1 1 0.5385 0.3236 0.7497 11.00000 0.05 0.36 Q2 1 0.3082 0.3503 0.7376 11.00000 0.05 0.30 Q3 1 0.5232 0.2781 0.6919 11.00000 0.05 0.30 Q4 1 0.5551 0.3190 0.2646 11.00000 0.05 0.29 Q5 1 0.2664 0.2782 0.7164 11.00000 0.05 0.28 Q6 1 0.4969 0.0387 0.7455 11.00000 0.05 0.28 Q7 1 0.6231 0.4050 0.7665 11.00000 0.05 0.28 Q8 1 0.3107 0.3068 0.6884 11.00000 0.05 0.27 Q9 1 0.4100 0.2603 0.6776 11.00000 0.05 0.27 Q10 1 0.6239 0.5260 0.2031 11.00000 0.05 0.27 Q11 1 0.7001 0.6155 0.3000 11.00000 0.05 0.25 Q12 1 0.6118 0.0239 0.7515 11.00000 0.05 0.25 Q13 1 0.7087 0.0742 0.7540 11.00000 0.05 0.25 Q14 1 1.1527 -0.1590 0.2958 11.00000 0.05 0.25 Q15 1 0.5337 0.5260 0.3276 11.00000 0.05 0.25 Q16 1 0.3230 0.2617 0.7342 11.00000 0.05 0.25 Q17 1 0.6198 0.5134 0.7744 11.00000 0.05 0.25 Q18 1 1.2612 -0.1013 0.2576 11.00000 0.05 0.25 Q19 1 0.7424 0.4345 0.7556 11.00000 0.05 0.25 Q20 1 0.7068 0.4035 0.3042 11.00000 0.05 0.24 ; _shelx_res_checksum 24997 _shelx_hkl_file ; 0 0 -2 1041.08 23.17 0 0 3 -0.64 1.56 0 0 -3 0.29 1.58 0 0 -3 -0.71 1.28 0 0 -3 -0.60 1.19 0 0 3 -1.26 1.61 0 0 3 -0.87 1.81 0 0 4 18.42 4.87 0 0 4 11.94 3.58 0 0 -4 21.28 5.00 0 0 -4 13.58 4.29 0 0 -4 17.41 4.04 0 0 4 14.69 4.21 0 0 5 2.08 1.94 0 0 -5 -2.06 1.41 0 0 -5 2.72 3.67 0 0 5 -2.40 2.81 0 0 5 3.47 3.90 0 0 6 1883.34 56.12 0 0 -6 1901.01 53.51 0 0 6 1914.48 54.74 0 0 -6 1901.91 57.06 0 0 6 1969.89 55.03 0 0 7 1.07 3.37 0 0 -7 0.93 2.23 0 0 7 4.66 4.94 0 0 7 -2.20 3.52 0 0 -7 -4.32 4.15 0 0 8 23.19 7.46 0 0 -8 48.66 10.63 0 0 8 41.93 9.50 0 0 9 0.41 4.66 0 0 9 -0.60 5.01 0 0 -9 -5.99 5.56 0 0 -10 621.40 39.67 0 0 10 737.80 43.64 0 0 10 653.27 42.90 0 0 11 -1.53 3.44 0 0 -11 15.02 7.70 0 0 11 2.27 6.94 0 0 12 651.05 47.60 0 0 12 703.67 46.86 0 0 13 4.74 8.41 0 0 13 5.91 6.58 0 0 -13 7.12 6.78 0 0 14 396.88 37.90 0 0 -14 383.07 36.37 0 0 14 353.91 38.30 0 0 15 -0.37 6.92 0 0 -15 9.93 7.88 0 0 15 6.52 6.86 0 0 -16 61.12 17.47 0 0 16 77.78 21.66 0 0 16 69.66 18.06 0 0 -17 -7.84 6.86 0 0 17 6.27 9.20 0 0 17 5.43 8.62 0 0 -18 265.22 34.94 0 0 18 266.56 40.07 0 0 18 258.37 34.73 0 0 19 6.43 8.98 0 0 19 0.07 9.10 0 0 -19 1.02 7.62 0 0 -20 336.96 42.65 0 0 20 411.92 47.96 0 0 20 358.27 48.86 0 0 21 -1.66 8.34 0 0 21 9.34 11.47 0 0 -21 7.73 9.38 0 0 22 134.66 30.39 0 0 -22 111.32 26.13 0 0 22 101.40 29.70 0 0 23 -21.34 16.77 0 0 -23 -5.48 10.45 0 0 23 -12.97 14.52 0 0 24 243.53 41.04 0 0 -24 275.96 40.56 0 0 24 222.83 45.33 0 0 25 13.20 16.99 0 0 25 -17.07 15.46 0 0 26 32.63 22.95 0 0 27 -1.14 12.83 0 0 28 253.73 55.56 0 1 1 189.71 9.47 0 1 1 1224.15 23.37 0 -1 -1 1281.52 24.13 0 1 -1 1098.89 22.19 0 1 -2 293.45 13.54 0 -1 2 287.77 13.25 0 -1 2 278.21 12.70 0 -1 -2 295.00 13.64 0 1 -2 291.47 13.02 0 1 2 298.67 13.23 0 -1 2 282.55 13.35 0 1 -2 273.74 12.87 0 1 2 264.33 13.16 0 1 2 295.69 13.71 0 -1 -2 339.75 14.77 0 -1 -2 288.40 12.58 0 1 3 44.77 6.31 0 1 -3 54.95 6.74 0 -1 3 47.66 6.31 0 -1 -3 48.47 6.46 0 1 -3 56.08 6.94 0 -1 3 42.94 5.67 0 -1 -3 46.86 6.02 0 -1 3 39.64 5.53 0 1 3 46.76 6.49 0 1 3 48.82 6.46 0 1 -3 52.58 6.32 0 -1 -3 49.21 6.72 0 -1 -5 1295.37 41.31 0 -1 -5 1467.84 46.23 0 1 -5 1650.22 46.54 0 -1 5 1450.89 44.75 0 1 5 1399.07 43.68 0 1 -5 1478.28 44.85 0 1 5 1489.27 45.38 0 -1 5 1484.72 43.85 0 1 -5 1492.07 43.44 0 -1 -5 1535.73 42.58 0 1 5 1408.77 43.26 0 -1 5 1551.98 46.56 0 1 6 94.00 12.48 0 1 -6 92.39 12.25 0 -1 -6 70.85 10.73 0 -1 6 75.25 11.50 0 -1 6 86.78 11.17 0 -1 -6 84.67 11.10 0 1 6 82.39 11.76 0 1 -6 87.43 11.52 0 1 6 91.75 11.88 0 -1 -6 70.31 11.18 0 -1 6 97.37 12.74 0 1 -6 96.94 12.84 0 1 -7 16.38 5.89 0 1 7 23.32 8.12 0 1 7 12.46 6.19 0 1 -7 20.81 6.39 0 -1 7 12.67 4.76 0 -1 -7 17.90 6.66 0 -1 7 16.73 6.15 0 -1 7 17.18 5.81 0 1 7 6.60 2.35 0 -1 -8 959.57 44.28 0 1 8 933.42 44.95 0 -1 8 877.59 43.20 0 1 -8 918.87 43.17 0 1 8 800.82 41.41 0 1 -8 953.75 44.70 0 -1 8 999.17 46.18 0 1 -9 130.56 17.68 0 1 9 123.44 17.58 0 -1 -9 104.95 15.95 0 -1 9 96.62 15.30 0 1 9 138.24 18.13 0 -1 9 130.10 17.63 0 -1 -10 4279.96 103.35 0 1 -10 4299.23 105.29 0 1 10 4086.40 107.78 0 -1 10 4124.90 105.99 0 1 10 4051.77 104.21 0 1 -11 11.98 6.73 0 1 11 10.08 3.37 0 1 11 1.77 5.36 0 -1 -11 25.47 8.86 0 -1 11 16.92 8.26 0 -1 11 17.66 6.63 0 -1 12 227.14 26.85 0 -1 -12 203.70 24.87 0 1 -12 239.56 26.72 0 -1 12 257.82 30.05 0 1 12 227.22 27.79 0 1 12 227.84 26.97 0 1 13 41.45 13.51 0 -1 -13 38.56 12.63 0 -1 13 26.41 11.16 0 1 13 16.85 7.03 0 -1 13 28.28 12.97 0 1 -13 45.13 13.31 0 1 14 873.63 60.64 0 -1 14 780.52 57.22 0 1 -14 868.47 55.41 0 -1 -14 825.39 53.69 0 -1 14 865.27 56.48 0 1 14 929.85 58.68 0 -1 15 8.92 10.02 0 1 15 9.81 9.86 0 1 -15 16.63 7.88 0 -1 -15 20.36 11.28 0 1 15 -2.16 8.81 0 -1 15 2.83 4.64 0 -1 16 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76.57 0 -9 -1 1893.49 85.76 0 9 -1 1980.89 87.78 0 -9 1 1907.99 77.16 0 9 1 2145.16 93.40 0 -9 -2 422.93 40.97 0 -9 2 491.60 43.00 0 -9 2 410.66 35.70 0 9 -2 486.07 43.19 0 9 2 524.69 46.33 0 -9 -2 544.53 41.74 0 -9 3 15.37 5.88 0 9 3 2.56 5.81 0 -9 -3 23.19 8.40 0 -9 3 19.39 10.55 0 -9 -3 8.85 9.97 0 9 -3 30.38 11.86 0 9 -4 33.82 13.77 0 -9 -4 47.26 14.80 0 -9 4 20.12 11.63 0 9 4 24.41 9.18 0 -9 4 11.38 8.94 0 -9 -4 23.26 8.22 0 -9 -5 17.74 8.40 0 -9 5 6.46 9.20 0 9 5 7.44 9.48 0 -9 -5 4.32 9.58 0 -9 5 14.41 9.86 0 9 -5 13.61 10.61 0 9 6 429.51 39.87 0 -9 6 305.32 35.11 0 9 -6 328.37 37.43 0 9 6 366.65 40.03 0 -9 -6 366.88 39.54 0 -9 6 349.79 35.20 0 -9 -7 412.22 42.82 0 -9 7 477.55 41.73 0 9 -7 472.68 44.83 0 -9 7 492.59 45.57 0 9 7 489.53 47.66 0 9 7 453.88 41.66 0 -9 8 17.62 11.15 0 -9 8 17.80 9.37 0 -9 -8 20.34 11.03 0 9 8 30.65 11.38 0 9 -8 19.92 12.44 0 9 8 13.69 10.51 0 -9 -9 45.80 13.51 0 9 -9 93.27 19.79 0 9 9 87.22 21.93 0 -9 9 81.94 21.62 0 -9 9 114.38 21.02 0 9 9 86.80 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17 52.13 22.25 0 9 18 115.46 30.51 0 -9 -18 105.32 28.75 0 -9 18 78.12 23.20 0 9 -18 92.33 24.33 0 -9 18 137.40 31.11 0 9 18 67.38 24.58 0 -9 -19 15.36 14.84 0 -9 19 -0.07 10.91 0 -9 19 -13.99 14.36 0 9 19 -0.35 8.37 0 9 19 -18.01 15.60 0 9 -19 11.44 16.75 0 -9 -20 397.33 54.82 0 -9 20 406.73 57.46 0 9 20 408.63 56.21 0 9 20 408.88 58.47 0 -9 21 36.65 22.11 0 9 21 64.24 23.98 0 9 21 58.78 26.20 0 -9 -21 13.08 16.71 0 9 22 49.29 23.94 0 -9 -22 15.96 12.33 0 -9 22 19.20 9.40 0 -9 -23 5.14 10.92 0 9 23 6.17 15.01 0 -9 23 8.08 15.28 0 -9 -24 55.97 27.85 0 -9 24 28.93 24.17 0 9 24 13.13 18.94 0 9 25 50.02 27.84 0 -9 -25 66.57 29.25 0 9 26 -10.56 17.78 0 -9 -26 -3.73 12.19 0 -10 0 18.18 11.98 0 10 0 8.50 10.63 0 -10 0 29.33 10.95 0 10 -1 105.97 21.98 0 -10 -1 106.54 22.29 0 -10 1 90.63 18.36 0 -10 -1 117.83 20.66 0 10 1 132.16 23.64 0 -10 1 115.19 23.24 0 10 2 17.56 11.01 0 -10 -2 -1.54 6.29 0 -10 2 -5.14 6.87 0 -10 2 -1.63 5.09 0 10 -2 0.31 6.55 0 -10 -2 -3.37 5.96 0 -10 3 400.15 42.40 0 10 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0 -10 11 967.33 70.34 0 10 11 911.88 74.05 0 10 11 903.59 67.35 0 -10 12 56.77 18.06 0 -10 -12 33.09 15.97 0 10 12 33.75 14.63 0 10 12 46.24 17.74 0 -10 12 50.24 16.02 0 10 -12 34.48 15.47 0 -10 13 -0.99 8.46 0 10 -13 19.18 12.49 0 -10 13 1.11 6.24 0 10 13 -0.45 9.75 0 -10 -13 -4.25 8.00 0 10 13 -15.18 13.58 0 -10 14 101.46 24.46 0 10 -14 116.96 27.29 0 -10 14 116.71 25.58 0 10 14 93.28 23.66 0 10 14 56.36 20.57 0 -10 -14 86.50 23.33 0 -10 -15 0.54 8.26 0 10 -15 25.59 12.66 0 10 15 14.43 11.37 0 10 15 3.78 9.31 0 -10 15 9.22 12.29 0 -10 15 22.60 13.80 0 -10 16 0.79 8.39 0 10 -16 13.40 10.34 0 10 16 1.73 8.77 0 -10 -16 33.90 16.51 0 -10 16 -16.93 13.07 0 10 16 8.39 8.43 0 -10 17 361.28 49.92 0 -10 17 435.08 50.79 0 10 17 492.40 62.11 0 10 -17 455.80 53.82 0 -10 -17 491.09 60.20 0 10 17 451.56 55.71 0 10 -18 21.86 17.20 0 -10 -18 0.70 11.57 0 10 18 13.96 8.33 0 -10 18 -0.34 10.13 0 10 18 16.40 13.11 0 -10 18 33.19 18.98 0 -10 19 341.23 47.42 0 10 19 291.63 47.28 0 -10 19 398.06 56.44 0 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5 498.98 50.14 0 11 -5 696.15 60.38 0 -11 -5 639.27 58.60 0 11 5 571.88 55.37 0 -11 -6 100.64 25.39 0 11 -6 125.68 26.57 0 -11 -6 130.33 24.12 0 -11 6 105.65 21.93 0 -11 6 86.95 20.95 0 11 6 108.50 24.77 0 -11 7 272.08 37.88 0 -11 -7 314.19 37.25 0 -11 -7 222.07 35.82 0 11 7 276.09 39.66 0 -11 7 280.92 34.92 0 11 -7 296.18 40.01 0 -11 -8 1158.94 73.53 0 -11 8 1153.32 72.04 0 -11 -8 1145.13 80.18 0 -11 8 1204.29 79.94 0 11 -8 1080.76 76.48 0 11 8 1144.29 80.56 0 -11 9 6.62 11.11 0 11 -9 17.58 14.43 0 11 9 6.94 7.87 0 -11 -9 7.11 11.12 0 -11 9 6.17 11.51 0 11 9 -7.14 12.93 0 -11 -10 24.02 15.12 0 -11 10 47.48 18.02 0 -11 10 7.20 8.35 0 11 10 20.02 10.16 0 11 -10 28.15 14.51 0 11 10 16.83 6.95 0 11 -11 6.57 8.80 0 -11 -11 20.55 15.21 0 11 11 10.27 12.47 0 11 11 6.52 11.57 0 -11 11 1.32 7.22 0 -11 11 11.29 9.16 0 11 -12 0.33 6.12 0 -11 12 -3.77 7.63 0 -11 -12 11.08 14.82 0 -11 12 4.25 9.61 0 11 12 1.22 8.50 0 -11 13 36.41 14.47 0 -11 13 35.64 15.57 0 11 13 15.51 12.72 0 11 13 35.20 19.53 0 11 -13 19.55 10.89 0 -11 -13 24.24 16.83 0 -11 -14 253.46 42.42 0 11 14 212.29 36.04 0 11 -14 266.77 40.15 0 11 14 271.73 45.63 0 -11 14 255.26 37.71 0 -11 14 210.74 35.17 0 11 15 230.31 41.88 0 11 15 180.54 34.86 0 -11 15 225.78 36.66 0 11 -15 265.22 40.00 0 -11 15 208.44 35.13 0 -11 -15 197.77 38.33 0 11 -16 114.15 27.73 0 11 16 116.95 29.53 0 -11 16 110.13 25.98 0 -11 16 175.50 35.49 0 -11 -16 122.77 29.84 0 11 16 132.71 33.41 0 11 17 308.46 46.74 0 -11 -17 362.96 53.84 0 11 -17 316.21 46.87 0 -11 17 368.36 51.93 0 11 17 351.14 53.79 0 -11 17 383.21 48.67 0 11 18 54.90 21.16 0 -11 18 16.91 16.11 0 11 18 37.38 20.41 0 -11 -18 17.66 15.74 0 11 19 9.15 10.58 0 -11 19 -6.44 11.80 0 -11 -19 16.95 17.37 0 -11 -20 29.43 17.99 0 11 20 54.33 24.72 0 -11 20 42.28 21.04 0 11 21 6.76 19.92 0 -11 -21 63.67 25.79 0 -11 21 10.41 16.17 0 11 22 68.58 29.89 0 -11 -22 41.94 21.96 0 -11 22 87.70 31.47 0 -11 23 4.08 10.66 0 -11 -23 18.83 15.68 0 11 24 14.24 15.43 0 -11 -24 34.76 23.94 0 -12 0 1577.89 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18.79 0 -13 12 -0.50 8.03 0 -13 12 -9.71 13.76 0 -13 -13 398.37 54.46 0 13 13 412.29 49.51 0 13 -13 374.65 50.16 0 13 13 364.75 52.78 0 -13 13 465.91 55.67 0 -13 13 357.09 47.38 0 -13 14 93.46 26.39 0 13 -14 92.23 25.80 0 -13 -14 96.10 27.91 0 13 14 71.16 22.22 0 13 14 75.05 27.31 0 -13 14 33.66 14.29 0 13 -15 92.81 27.25 0 -13 -15 72.61 23.40 0 -13 15 19.82 12.05 0 13 15 49.52 19.95 0 -13 15 56.45 21.39 0 13 -16 14.28 15.42 0 -13 -16 60.88 26.63 0 -13 16 42.20 20.41 0 13 16 -8.95 17.79 0 -13 16 22.25 16.45 0 -13 17 256.48 45.36 0 13 17 151.53 36.67 0 -13 -17 181.89 42.04 0 -13 18 90.39 28.02 0 13 18 101.91 33.74 0 -13 -18 119.96 34.87 0 13 19 19.10 14.36 0 -13 -19 0.23 11.55 0 -13 19 8.11 11.59 0 13 20 2.36 13.81 0 -13 20 16.77 15.73 0 -13 -20 5.84 12.76 0 -13 21 -7.53 13.21 0 13 21 2.83 13.48 0 -13 -22 36.14 24.82 0 13 22 54.70 29.51 0 -14 0 836.57 75.01 0 14 0 983.90 82.95 0 -14 0 830.32 63.20 0 14 -1 371.78 50.70 0 -14 -1 441.79 45.50 0 -14 1 343.92 47.60 0 -14 -1 350.64 48.19 0 14 1 388.77 52.41 0 -14 1 383.01 42.22 0 14 -2 332.75 47.89 0 -14 -2 355.66 49.08 0 -14 -2 401.43 43.83 0 -14 2 335.26 47.69 0 -14 2 397.21 43.31 0 14 2 318.91 49.25 0 14 3 25.10 15.67 0 -14 3 11.68 9.94 0 14 -3 53.93 23.71 0 -14 -3 34.80 15.45 0 -14 3 28.84 14.93 0 -14 -3 28.32 13.93 0 14 -4 92.90 25.80 0 -14 -4 68.49 22.71 0 -14 -4 46.41 14.28 0 14 4 46.70 21.86 0 -14 4 82.27 20.80 0 -14 4 64.40 22.25 0 14 5 92.94 25.34 0 -14 5 131.22 26.14 0 -14 5 134.48 29.70 0 -14 -5 162.57 34.61 0 -14 -5 152.54 28.20 0 14 -5 165.58 32.97 0 14 -6 7.00 12.31 0 -14 -6 15.23 9.00 0 -14 -6 12.92 9.08 0 -14 6 5.36 7.42 0 -14 6 15.16 11.84 0 14 6 20.38 20.28 0 -14 -7 0.25 9.65 0 14 7 -4.92 9.29 0 -14 -7 -13.01 14.57 0 -14 7 -1.74 9.89 0 14 -7 0.82 10.33 0 -14 7 -1.99 6.50 0 -14 8 98.05 26.11 0 -14 -8 100.08 27.05 0 -14 8 56.23 18.44 0 14 -8 134.55 30.84 0 14 8 53.54 21.65 0 -14 -8 85.49 22.96 0 14 9 -4.44 12.11 0 -14 -9 11.88 12.64 0 -14 9 -0.08 7.91 0 -14 9 -7.56 11.62 0 -14 -9 1.98 9.18 0 14 -9 6.44 11.41 0 -14 -10 203.48 40.23 0 14 10 188.91 39.88 0 -14 10 178.40 34.18 0 -14 -10 258.21 38.91 0 14 -10 249.46 42.70 0 -14 10 225.62 39.82 0 14 11 10.71 13.15 0 -14 -11 29.06 21.00 0 -14 11 3.11 6.12 0 -14 -11 16.24 11.21 0 14 -11 14.11 11.10 0 -14 11 23.79 13.75 0 -14 12 99.67 26.91 0 -14 12 184.24 35.36 0 14 12 177.69 41.22 0 -14 -12 200.87 35.78 0 -14 -12 176.22 39.35 0 14 -12 159.43 33.93 0 14 13 7.12 9.24 0 -14 -13 4.02 10.26 0 -14 13 5.95 12.56 0 -14 -13 3.26 10.28 0 14 -13 22.82 13.74 0 -14 13 30.05 16.42 0 14 -14 10.96 12.12 0 -14 14 7.89 12.30 0 14 14 21.77 17.00 0 -14 14 13.30 13.82 0 -14 -14 15.08 16.28 0 -14 15 101.35 26.58 0 -14 15 101.89 28.85 0 -14 -15 123.35 34.94 0 14 -15 127.42 31.97 0 14 15 116.14 35.40 0 -14 16 -14.88 16.06 0 14 16 -4.34 13.40 0 -14 -16 7.22 10.20 0 -14 -17 69.55 33.86 0 14 17 24.84 19.54 0 -14 17 98.46 29.02 0 -14 -18 61.51 30.01 0 14 18 95.46 33.89 0 -14 18 51.96 22.26 0 -14 19 203.10 43.80 0 -14 -19 249.56 51.08 0 14 19 295.35 59.99 0 -14 20 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21.93 10 11 -4 -22.52 24.23 10 -11 4 6.27 19.50 -10 -11 -4 32.51 25.61 10 11 -3 24.09 21.19 10 -11 3 6.88 12.83 -10 -11 -3 30.08 30.02 10 11 -2 -2.16 18.56 10 -11 2 7.04 14.48 -10 -11 -2 -14.13 21.05 10 -11 1 98.12 36.20 -10 -11 -1 40.87 30.42 10 11 -1 87.51 34.84 10 -11 0 46.43 29.62 -10 -11 0 -15.41 23.19 10 11 0 63.44 32.57 10 -11 -1 95.92 36.55 -10 -11 1 90.81 37.61 10 11 1 56.38 29.08 10 -11 -2 26.37 26.75 -10 -11 2 -12.50 18.16 10 11 2 26.95 24.22 10 -11 -3 22.97 23.73 10 11 3 24.07 20.20 -10 -11 3 18.58 15.88 10 -11 -4 6.95 17.61 -10 -11 4 -5.24 13.53 10 -11 -5 5.07 14.93 10 11 5 20.97 25.03 -10 -11 5 35.71 25.64 10 11 6 22.59 16.05 -10 -11 6 57.99 27.31 -10 -11 7 61.70 28.93 -10 -11 8 32.41 22.09 10 12 -5 33.43 28.90 10 -12 5 -17.47 26.08 10 12 -4 14.83 20.46 10 -12 4 10.74 16.69 10 12 -3 65.29 36.08 10 -12 3 -0.45 18.33 10 12 -2 12.45 18.27 10 -12 2 -21.52 22.28 -10 -12 -2 12.17 16.56 10 -12 1 40.93 27.97 -10 -12 -1 72.31 37.59 10 12 -1 34.87 23.66 10 -12 0 18.73 21.73 -10 -12 0 -7.89 17.00 10 12 0 11.16 22.21 -10 -12 1 34.31 24.79 10 12 1 1.48 16.15 10 -12 -2 2.25 18.07 -10 -12 2 21.10 18.57 10 12 2 -5.41 14.26 10 -12 -3 50.72 28.33 10 12 3 34.19 19.61 -10 -12 3 10.96 14.74 10 -12 -4 54.87 30.54 10 12 4 26.35 23.82 -10 -12 4 17.02 18.33 10 12 5 -10.90 18.32 10 -12 -5 11.86 20.50 10 12 6 121.04 41.08 10 -13 1 2.62 16.70 10 13 -1 68.97 37.89 10 -13 0 13.10 21.01 10 13 0 48.88 31.52 10 -13 -1 33.74 33.12 10 13 1 43.29 31.46 10 -13 -2 9.67 19.78 10 13 2 14.13 21.53 10 -13 -3 -5.57 18.13 10 13 3 50.35 32.51 10 -13 -4 48.08 25.38 10 13 4 53.43 26.16 10 13 5 2.46 16.38 10 -13 -5 31.11 29.24 10 13 6 11.46 21.49 -11 0 -4 66.95 25.94 -11 0 5 16.36 11.82 -11 0 -5 1.22 14.45 11 0 6 42.38 23.17 -11 0 6 22.94 17.67 -11 0 -6 77.67 30.33 11 0 7 80.49 34.19 -11 0 7 63.06 25.77 -11 0 -7 45.16 25.23 11 0 8 43.25 29.64 -11 0 8 14.75 16.30 -11 0 -8 6.72 14.95 11 0 9 130.82 40.82 -11 0 9 127.02 36.41 -11 0 -9 122.84 36.92 11 0 10 38.52 29.39 -11 0 10 6.24 12.89 -11 0 -10 1.50 14.57 11 0 11 47.32 27.59 -11 0 11 9.37 13.76 -11 0 -11 16.38 20.79 11 0 12 -12.18 18.94 -11 0 12 1.97 19.83 -11 0 -12 -10.10 15.90 11 0 13 -5.94 20.11 -11 0 13 22.81 20.67 11 0 14 0.84 20.92 11 -1 14 -7.37 24.26 11 -1 13 13.82 18.29 -11 1 13 -17.22 15.58 11 -1 12 30.89 24.36 -11 1 12 6.98 16.95 -11 -1 -12 69.71 32.02 11 -1 11 -1.15 17.22 -11 1 11 20.09 20.38 -11 -1 -11 18.15 20.00 11 -1 10 85.07 31.91 -11 1 10 42.25 23.60 -11 -1 -10 119.28 38.29 11 -1 9 6.39 16.79 -11 1 9 13.95 13.77 -11 -1 -9 13.49 20.96 11 -1 8 18.87 18.93 -11 1 8 -3.44 16.04 -11 -1 -8 11.92 13.17 11 -1 7 27.45 19.54 -11 1 7 10.98 12.13 -11 -1 -7 3.05 14.07 -11 1 6 102.61 31.51 -11 -1 -6 18.82 14.18 -11 -1 -5 40.46 20.76 -11 -1 -4 75.81 32.82 -11 -1 -3 5.53 10.89 -11 1 -3 31.19 19.35 -11 -1 4 46.16 22.25 -11 1 -4 44.99 22.30 11 1 5 39.05 24.86 -11 -1 5 55.42 26.99 -11 1 -5 38.56 21.38 11 1 6 47.01 28.42 -11 -1 6 65.27 26.35 -11 1 -6 56.40 25.05 11 1 7 -3.42 16.72 -11 -1 7 26.26 20.37 -11 1 -7 24.89 18.63 11 1 8 19.92 24.60 -11 -1 8 -0.95 13.75 -11 1 -8 39.44 26.14 -11 -1 9 12.50 19.10 -11 1 -9 29.45 23.19 11 1 10 119.96 40.59 -11 -1 10 95.42 36.49 -11 1 -10 86.27 33.45 11 1 11 -15.78 24.26 -11 -1 11 8.28 13.23 -11 1 -11 -12.04 19.27 11 1 12 10.73 18.71 -11 -1 12 9.11 19.81 -11 1 -12 48.77 30.38 11 1 13 15.91 25.86 11 -2 14 43.37 25.23 11 -2 13 44.22 29.05 -11 2 13 48.92 29.18 11 -2 12 44.92 31.50 -11 2 12 18.30 19.46 -11 -2 -12 24.18 22.56 11 -2 11 35.20 27.43 -11 2 11 32.38 21.80 -11 -2 -11 8.27 19.81 11 -2 10 61.66 30.86 -11 2 10 16.03 19.52 -11 -2 -10 38.76 21.21 -11 2 9 22.56 18.57 -11 -2 -9 29.67 19.26 -11 2 8 12.56 17.43 -11 -2 -8 30.14 24.20 -11 2 7 16.27 11.96 -11 -2 -7 12.97 14.43 -11 -2 -6 207.27 43.03 -11 -2 -5 39.25 20.44 -11 -2 -4 71.03 27.54 -11 -2 -3 50.16 25.04 -11 -2 -2 25.81 20.00 -11 -2 -1 32.86 18.80 -11 2 -3 -7.06 14.53 -11 -2 4 64.27 28.05 -11 2 -4 64.20 26.55 -11 -2 5 20.24 16.49 -11 2 -5 40.79 23.63 11 2 6 185.61 47.09 -11 -2 6 148.78 38.48 -11 2 -6 95.47 31.34 11 2 7 92.54 36.33 -11 -2 7 60.42 27.04 -11 2 -7 31.17 20.95 11 2 8 -0.14 17.55 -11 -2 8 1.25 15.94 -11 2 -8 18.49 20.93 11 2 9 31.19 27.46 -11 -2 9 18.26 20.28 -11 2 -9 49.32 23.88 11 2 10 79.86 41.25 -11 -2 10 20.27 18.50 -11 2 -10 23.51 23.13 11 2 11 11.55 21.91 -11 -2 11 2.33 15.62 -11 2 -11 3.38 16.03 11 2 12 -0.98 15.30 -11 -2 12 10.85 23.17 -11 2 -12 24.30 25.41 11 2 13 1.52 18.61 -11 3 13 12.81 20.11 -11 3 12 13.69 17.99 -11 -3 -12 -11.48 17.73 -11 3 11 23.50 19.61 -11 -3 -11 3.43 11.54 -11 3 10 41.43 20.05 -11 -3 -10 8.74 14.97 -11 3 9 14.31 20.13 -11 -3 -9 28.30 20.41 -11 3 8 37.27 21.64 -11 -3 -8 39.83 22.84 -11 -3 -7 26.53 19.65 -11 -3 -6 72.09 23.74 -11 -3 -5 85.56 31.09 -11 -3 -4 13.90 16.18 -11 -3 -3 98.73 33.70 -11 -3 -2 19.98 16.79 -11 -3 -1 0.95 15.07 -11 -3 0 91.28 31.99 -11 -3 1 13.28 14.21 -11 3 -2 20.19 15.45 -11 -3 3 108.99 31.62 -11 3 -3 83.14 30.25 -11 -3 4 27.17 20.11 -11 3 -4 8.25 14.67 -11 -3 5 64.62 29.68 -11 3 -5 28.39 19.99 11 3 6 30.63 28.31 -11 -3 6 52.18 25.31 -11 3 -6 91.78 33.95 11 3 7 -17.34 19.93 -11 -3 7 24.41 21.37 -11 3 -7 5.06 14.21 11 3 8 56.70 30.81 -11 -3 8 38.08 23.69 -11 3 -8 45.18 22.84 11 3 9 6.70 15.14 -11 -3 9 17.83 15.83 -11 3 -9 4.40 15.03 11 3 10 -15.80 22.86 -11 -3 10 40.24 24.23 -11 3 -10 40.55 24.11 11 3 11 2.62 21.82 -11 -3 11 47.76 32.20 -11 3 -11 -0.55 15.74 11 3 12 44.47 30.24 -11 -3 12 20.56 21.55 -11 4 12 7.59 19.84 -11 -4 -12 -0.87 12.73 -11 4 11 22.99 18.93 -11 -4 -11 13.08 18.55 -11 4 10 15.85 14.88 -11 -4 -10 6.91 15.60 -11 4 9 25.10 18.29 -11 -4 -9 56.15 26.27 -11 -4 -8 38.04 21.05 -11 -4 -7 20.10 19.09 -11 -4 -6 14.70 14.20 -11 -4 -5 90.31 32.13 -11 -4 -4 7.67 12.46 -11 -4 -3 31.97 20.24 11 4 -2 33.41 22.89 -11 -4 -2 28.10 19.68 -11 -4 -1 46.85 23.10 -11 -4 0 1.42 10.57 -11 -4 1 123.29 35.17 -11 4 -1 44.55 19.76 -11 -4 2 45.77 22.77 -11 4 -2 39.38 22.05 -11 -4 3 32.32 21.22 -11 4 -3 3.17 12.28 -11 -4 4 19.83 24.20 -11 4 -4 -10.69 16.99 -11 -4 5 34.71 22.03 -11 4 -5 104.41 32.98 -11 -4 6 4.07 16.41 -11 4 -6 30.45 20.72 11 4 7 5.32 19.11 -11 -4 7 46.64 28.46 -11 4 -7 13.28 16.73 11 4 8 26.00 20.31 -11 -4 8 32.02 22.52 -11 4 -8 49.66 23.59 11 4 9 30.55 26.82 -11 -4 9 22.30 16.13 11 4 10 21.28 24.00 -11 -4 10 23.95 21.51 -11 4 -10 -12.61 19.71 11 4 11 77.75 37.83 -11 -4 11 34.55 26.62 -11 4 -11 32.32 27.32 -11 5 12 3.80 15.58 -11 -5 -12 18.39 19.38 -11 5 11 31.65 20.05 -11 -5 -11 -2.86 12.61 -11 5 10 -14.75 16.30 -11 -5 -10 17.79 18.74 -11 -5 -9 30.28 20.20 -11 -5 -8 27.61 19.96 -11 -5 -6 22.73 20.19 11 5 -5 77.88 33.00 -11 -5 -5 50.84 25.03 -11 -5 -4 54.37 27.71 11 5 -4 69.07 32.26 -11 -5 -3 124.34 36.50 11 5 -3 201.01 48.73 11 5 -2 14.04 14.92 -11 -5 -2 76.02 29.74 11 5 -1 19.89 22.32 -11 -5 -1 -16.52 16.51 11 -5 0 -19.61 16.74 -11 -5 0 5.66 13.83 -11 -5 1 -11.48 16.58 -11 -5 2 14.85 18.26 -11 -5 3 91.57 30.29 -11 5 -3 127.44 36.31 -11 -5 4 65.45 26.30 -11 5 -4 73.12 28.92 -11 -5 5 42.70 23.57 -11 5 -5 31.80 18.74 -11 5 -6 22.99 19.19 -11 -5 7 20.45 22.93 -11 5 -7 4.45 14.41 11 5 8 11.85 14.98 -11 -5 8 21.48 24.23 -11 5 -8 -4.74 16.39 11 5 9 1.46 20.33 -11 -5 9 0.15 24.78 -11 5 -9 8.33 17.36 11 5 10 38.56 28.03 -11 -5 10 53.29 33.32 -11 5 -10 32.78 29.52 11 5 11 33.70 25.83 -11 -5 11 40.13 33.38 -11 6 12 14.24 14.94 -11 -6 -11 62.27 25.12 -11 -6 -10 29.55 21.88 -11 -6 -9 -5.85 12.48 11 6 -7 24.17 19.00 -11 -6 -7 -11.31 15.92 11 6 -6 58.28 31.09 -11 -6 -6 -11.18 16.41 -11 -6 -5 5.32 12.92 11 6 -5 32.48 25.89 11 6 -4 51.05 31.74 -11 -6 -4 36.57 23.95 11 6 -3 40.08 27.47 11 -6 3 51.96 28.64 -11 -6 -3 53.85 30.95 11 -6 2 22.52 17.04 -11 -6 -2 12.58 20.91 11 6 -2 20.82 17.78 11 -6 1 45.88 25.77 11 6 -1 37.54 24.83 -11 -6 -1 -2.57 11.28 11 6 0 2.25 19.03 11 -6 0 37.75 23.66 -11 -6 0 20.43 19.78 -11 -6 1 13.58 14.85 -11 -6 2 16.50 15.02 -11 -6 3 20.99 17.45 -11 -6 4 -11.48 13.06 -11 -6 5 34.23 23.79 -11 6 -5 14.22 20.53 -11 -6 6 -9.65 11.56 -11 6 -6 29.23 25.53 -11 6 -7 68.57 31.15 -11 6 -8 16.60 21.58 11 6 9 12.96 19.65 -11 -6 9 4.37 14.45 -11 6 -9 -8.26 17.10 11 6 10 153.15 50.17 -11 -6 10 38.33 27.76 -11 -7 -11 -3.76 12.86 -11 -7 -10 7.52 12.83 -11 -7 -8 25.35 22.40 11 7 -8 19.99 22.03 -11 -7 -7 38.00 24.92 11 7 -7 5.88 16.74 11 7 -6 49.72 28.43 -11 -7 -6 -8.24 14.35 11 7 -5 55.04 30.03 11 -7 5 -0.68 16.02 -11 -7 -5 72.98 32.16 11 -7 4 61.81 30.56 -11 -7 -4 18.07 20.64 11 7 -4 40.46 25.10 11 -7 3 -18.64 17.42 11 7 -3 -7.26 16.74 -11 -7 -3 19.63 19.02 11 7 -2 32.43 23.76 11 -7 2 42.00 23.60 -11 -7 -2 14.19 21.19 11 7 -1 17.48 22.50 11 -7 1 6.23 19.72 -11 -7 -1 19.04 19.87 11 -7 0 6.14 12.13 -11 -7 0 42.05 28.68 11 7 0 28.62 18.02 -11 -7 1 2.27 15.57 -11 -7 2 -4.48 12.53 -11 -7 3 21.69 21.98 -11 -7 4 35.52 24.87 -11 -7 5 54.28 25.74 -11 -7 6 17.32 17.16 -11 -7 7 9.43 19.34 -11 7 -7 35.23 23.74 -11 -7 8 31.75 24.56 -11 7 -8 10.26 17.33 11 8 -8 40.73 29.54 11 8 -7 33.33 23.45 11 -8 7 -2.84 16.70 11 -8 6 12.84 16.27 -11 -8 -6 13.04 21.40 11 8 -6 39.84 27.84 11 -8 5 108.18 41.48 -11 -8 -5 -2.71 19.86 11 8 -5 71.42 30.89 11 8 -4 60.99 32.40 11 -8 4 30.55 24.91 -11 -8 -4 23.85 13.08 11 8 -3 6.36 15.54 11 -8 3 21.16 21.14 -11 -8 -3 33.83 21.86 11 -8 2 6.62 15.03 -11 -8 -2 21.48 19.37 11 8 -2 60.33 26.77 11 -8 1 35.78 25.23 -11 -8 -1 32.29 26.26 11 8 -1 25.08 16.68 11 -8 0 -1.23 12.81 -11 -8 0 15.62 22.62 11 8 0 4.81 14.78 11 -8 -1 71.02 31.10 -11 -8 1 25.24 19.51 11 8 1 63.34 29.75 -11 -8 2 14.34 14.41 -11 -8 3 9.12 15.88 -11 -8 4 58.07 27.97 -11 -8 5 34.64 25.03 -11 -8 6 28.82 21.53 -11 -8 7 1.07 12.93 -11 -8 8 -3.98 13.19 -11 -8 9 30.63 23.27 11 -9 6 33.47 26.38 11 9 -6 41.02 24.21 11 9 -5 118.63 38.86 11 -9 5 12.42 19.98 11 9 -4 18.06 20.69 11 -9 4 31.80 22.64 -11 -9 -4 -25.24 25.10 11 -9 3 86.13 34.19 -11 -9 -3 75.62 34.80 11 9 -3 67.27 33.55 11 -9 2 30.10 24.30 -11 -9 -2 20.78 18.91 11 9 -2 16.19 18.08 11 -9 1 -12.77 19.44 -11 -9 -1 39.60 26.96 11 9 -1 4.93 17.73 11 -9 0 -3.13 15.83 11 9 0 16.32 21.79 -11 -9 0 9.59 21.14 11 9 1 40.10 25.94 11 -9 -1 26.70 23.89 -11 -9 1 5.43 14.06 -11 -9 2 21.50 19.29 -11 -9 3 54.52 27.59 -11 -9 4 -39.08 25.78 -11 -9 5 44.87 26.27 -11 -9 6 35.56 23.49 -11 -9 7 -7.66 18.46 -11 -9 8 5.93 13.89 11 -10 4 31.05 26.48 11 10 -4 51.93 28.28 11 -10 3 30.38 24.55 11 10 -3 50.75 27.27 11 -10 2 22.37 30.23 11 10 -2 8.96 19.42 11 -10 1 -3.36 14.92 11 10 -1 1.44 15.72 11 10 0 -18.96 16.11 11 -10 0 15.79 22.61 11 10 1 44.46 29.52 11 -10 -1 4.58 15.87 11 10 2 24.76 21.26 11 11 -1 -3.51 18.01 11 -11 1 -10.78 19.62 11 11 0 53.98 30.19 11 -11 0 51.43 28.54 11 11 1 43.32 52.04 11 -11 -1 30.65 19.89 11 11 2 76.81 32.86 11 -11 -2 15.13 22.31 -12 0 -8 31.05 22.71 -12 0 -9 10.48 20.07 -12 -1 -9 44.14 27.78 -12 1 -7 -9.02 17.35 -12 1 -8 43.65 23.51 -12 -1 9 47.68 29.60 -12 1 -9 13.51 15.13 -12 2 -7 12.64 19.04 12 2 8 63.86 35.21 -12 -2 8 20.29 20.30 -12 2 -8 29.73 21.98 12 2 9 42.74 28.81 -12 -2 9 7.97 16.52 -12 -3 -7 8.90 13.96 -12 -3 -6 26.18 22.53 -12 -3 -5 14.52 19.62 -12 3 -6 9.21 14.21 -12 -3 7 139.52 42.84 -12 3 -7 29.35 19.61 -12 -3 8 -9.96 18.98 -12 3 -8 -8.78 15.39 -12 -4 -7 16.92 17.27 -12 -4 -6 33.20 25.53 -12 -4 -5 19.27 20.62 -12 -4 -4 51.46 25.31 -12 -4 -3 33.18 20.42 -12 4 -5 1.41 12.04 -12 4 -6 -2.95 16.10 -12 -4 7 37.71 25.94 -12 4 -7 19.11 15.41 -12 -5 -6 -18.36 20.96 -12 -5 -5 2.63 14.71 -12 -5 -4 17.72 17.28 -12 -5 -3 5.55 16.34 -12 -5 -2 3.24 13.75 -12 -5 -1 2.98 13.02 -12 5 -5 46.25 29.11 -12 -5 6 12.34 20.88 -12 5 -6 5.17 14.52 -12 -6 -4 98.10 36.56 -12 -6 -3 -12.13 18.41 -12 -6 -2 6.29 13.37 -12 -6 -1 3.75 13.42 -12 -6 0 31.44 24.61 -12 -6 1 0.13 15.44 -12 6 -4 14.08 17.02 -12 -6 5 21.67 24.55 -12 6 -5 18.25 20.77 12 7 -4 34.19 27.08 -12 -7 0 -32.88 28.39 -12 -7 1 -5.87 16.01 -12 -7 2 2.04 14.00 0 0 0 0.00 0.00 TITL r20170321a in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 0.71073 8.358377 14.815972 18.975254 90.0000 90.0000 90.0000 ZERR 4.00 0.000358 0.000532 0.000648 0.0000 0.0000 0.0000 LATT -1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O S UNIT 104 116 4 16 4 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 23038 _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 - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.245 _oxdiff_exptl_absorpt_empirical_full_min 0.732 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' 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 S1 S 0.52365(10) -0.03255(5) 0.45723(4) 0.0324(2) Uani 1 1 d . O1 O 0.5180(3) 0.31310(12) 0.44538(9) 0.0309(4) Uani 1 1 d . O2 O 0.5851(3) 0.63694(13) 0.30376(10) 0.0341(5) Uani 1 1 d . O3 O 0.4536(3) 0.00662(14) 0.39570(11) 0.0428(6) Uani 1 1 d . O4 O 0.4472(3) -0.10630(14) 0.49236(12) 0.0415(5) Uani 1 1 d . N1 N 0.5387(3) 0.04841(15) 0.51482(11) 0.0286(5) Uani 1 1 d . C1 C 0.5905(4) 0.13799(18) 0.49165(14) 0.0280(6) Uani 1 1 d . H1A H 0.555169 0.148842 0.442576 0.034 Uiso 1 1 calc R H1B H 0.708689 0.142051 0.493143 0.034 Uiso 1 1 calc R C2 C 0.5172(3) 0.20845(16) 0.54059(12) 0.0245(5) Uani 1 1 d . H2 H 0.398231 0.202278 0.537987 0.029 Uiso 1 1 calc R C3 C 0.5684(3) 0.19110(18) 0.61760(13) 0.0265(6) Uani 1 1 d . H3 H 0.686951 0.199117 0.620590 0.032 Uiso 1 1 calc R C4 C 0.5294(4) 0.09325(18) 0.63795(14) 0.0304(6) Uani 1 1 d . H4A H 0.573839 0.080627 0.685293 0.036 Uiso 1 1 calc R H4B H 0.411793 0.085920 0.640582 0.036 Uiso 1 1 calc R C5 C 0.5965(4) 0.0253(2) 0.58586(14) 0.0320(6) Uani 1 1 d . H5A H 0.714863 0.026817 0.586918 0.038 Uiso 1 1 calc R H5B H 0.561068 -0.036306 0.598666 0.038 Uiso 1 1 calc R C6 C 0.5601(3) 0.30337(17) 0.51824(13) 0.0259(6) Uani 1 1 d . H6A H 0.500708 0.347791 0.547149 0.031 Uiso 1 1 calc R H6B H 0.676071 0.313951 0.524734 0.031 Uiso 1 1 calc R C7 C 0.5427(3) 0.39646(18) 0.41478(14) 0.0260(6) Uani 1 1 d . C8 C 0.5076(3) 0.40192(18) 0.34308(14) 0.0284(6) Uani 1 1 d . H8 H 0.471657 0.349708 0.318706 0.034 Uiso 1 1 calc R C9 C 0.5244(4) 0.48215(18) 0.30721(14) 0.0297(6) Uani 1 1 d . H9 H 0.501213 0.485072 0.258250 0.036 Uiso 1 1 calc R C10 C 0.5757(3) 0.55920(18) 0.34308(14) 0.0268(6) Uani 1 1 d . C11 C 0.6150(4) 0.55326(19) 0.41361(14) 0.0293(6) Uani 1 1 d . H11 H 0.653783 0.605038 0.437680 0.035 Uiso 1 1 calc R C12 C 0.5981(3) 0.47188(18) 0.44981(13) 0.0284(6) Uani 1 1 d . H12 H 0.624707 0.468369 0.498410 0.034 Uiso 1 1 calc R C13 C 0.6132(5) 0.7185(2) 0.34144(18) 0.0447(8) Uani 1 1 d . H13A H 0.603961 0.769954 0.309200 0.067 Uiso 1 1 calc GR H13B H 0.720997 0.717279 0.361770 0.067 Uiso 1 1 calc GR H13C H 0.534147 0.724551 0.379275 0.067 Uiso 1 1 calc GR C14 C 0.4917(3) 0.25647(17) 0.66843(12) 0.0249(6) Uani 1 1 d . C15 C 0.3255(4) 0.26382(19) 0.67226(14) 0.0298(6) Uani 1 1 d . H15 H 0.260588 0.228172 0.642038 0.036 Uiso 1 1 calc R C16 C 0.2541(4) 0.32250(19) 0.71962(15) 0.0322(6) Uani 1 1 d . H16 H 0.140752 0.326665 0.721774 0.039 Uiso 1 1 calc R C17 C 0.3470(4) 0.3749(2) 0.76370(15) 0.0365(7) Uani 1 1 d . H17 H 0.297827 0.414775 0.796386 0.044 Uiso 1 1 calc R C18 C 0.5110(4) 0.3692(2) 0.76012(15) 0.0393(7) Uani 1 1 d . H18 H 0.575059 0.405400 0.790329 0.047 Uiso 1 1 calc R C19 C 0.5834(4) 0.3108(2) 0.71247(15) 0.0343(7) Uani 1 1 d . H19 H 0.696797 0.308002 0.709966 0.041 Uiso 1 1 calc R C20 C 0.7169(4) -0.06943(18) 0.43458(14) 0.0311(6) Uani 1 1 d . C21 C 0.8009(4) -0.0257(2) 0.38187(17) 0.0436(8) Uani 1 1 d . H21 H 0.756510 0.025795 0.359390 0.052 Uiso 1 1 calc R C22 C 0.9498(5) -0.0575(2) 0.36210(17) 0.0464(9) Uani 1 1 d . H22 H 1.007202 -0.027160 0.326000 0.056 Uiso 1 1 calc R C23 C 1.0172(4) -0.1330(2) 0.39386(15) 0.0390(7) Uani 1 1 d . C24 C 0.9320(4) -0.1741(2) 0.44783(17) 0.0382(7) Uani 1 1 d . H24 H 0.977340 -0.224736 0.471180 0.046 Uiso 1 1 calc R C25 C 0.7842(4) -0.14357(19) 0.46838(15) 0.0344(7) Uani 1 1 d . H25 H 0.728139 -0.172886 0.505445 0.041 Uiso 1 1 calc R C26 C 1.1754(5) -0.1687(3) 0.3693(2) 0.0558(10) Uani 1 1 d . H26A H 1.234110 -0.193756 0.409481 0.084 Uiso 1 1 calc GR H26B H 1.237687 -0.119545 0.348222 0.084 Uiso 1 1 calc GR H26C H 1.157951 -0.216063 0.334089 0.084 Uiso 1 1 calc GR 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 0.0385(4) 0.0275(3) 0.0311(3) -0.0031(3) -0.0038(3) -0.0027(3) O1 0.0443(12) 0.0255(9) 0.0230(8) 0.0016(7) -0.0006(9) 0.0004(9) O2 0.0432(12) 0.0276(10) 0.0314(10) 0.0056(8) -0.0053(9) -0.0014(9) O3 0.0516(14) 0.0392(12) 0.0376(11) -0.0045(9) -0.0149(10) 0.0026(11) O4 0.0449(13) 0.0312(10) 0.0483(12) -0.0027(10) 0.0024(11) -0.0088(10) N1 0.0361(13) 0.0236(10) 0.0261(10) -0.0003(9) -0.0002(10) -0.0011(10) C1 0.0332(15) 0.0248(12) 0.0261(12) -0.0009(11) 0.0028(12) 0.0002(12) C2 0.0237(13) 0.0272(13) 0.0227(11) 0.0014(10) 0.0000(12) 0.0001(10) C3 0.0270(14) 0.0289(13) 0.0236(12) -0.0001(10) -0.0041(11) 0.0013(11) C4 0.0387(16) 0.0291(13) 0.0234(12) 0.0039(10) -0.0004(13) 0.0021(13) C5 0.0401(16) 0.0284(14) 0.0274(13) 0.0016(11) -0.0018(12) 0.0026(13) C6 0.0276(15) 0.0266(12) 0.0236(12) -0.0005(10) 0.0011(11) 0.0023(11) C7 0.0262(14) 0.0254(12) 0.0265(12) 0.0013(10) 0.0032(11) 0.0028(11) C8 0.0302(15) 0.0280(13) 0.0270(12) -0.0042(10) -0.0012(12) 0.0017(12) C9 0.0301(14) 0.0350(14) 0.0239(12) 0.0003(10) -0.0028(11) 0.0014(12) C10 0.0249(14) 0.0269(13) 0.0288(13) 0.0037(10) 0.0013(11) 0.0040(11) C11 0.0303(15) 0.0271(14) 0.0306(13) -0.0032(11) -0.0032(12) -0.0002(12) C12 0.0326(15) 0.0296(13) 0.0230(12) -0.0010(11) -0.0017(12) 0.0020(12) C13 0.064(2) 0.0280(16) 0.0420(17) 0.0006(13) 0.0009(17) -0.0019(15) C14 0.0284(15) 0.0248(12) 0.0214(11) 0.0022(9) -0.0010(11) 0.0006(11) C15 0.0309(15) 0.0326(15) 0.0260(13) -0.0008(12) 0.0011(12) -0.0048(12) C16 0.0335(15) 0.0332(15) 0.0298(14) 0.0042(12) 0.0052(12) 0.0033(13) C17 0.0489(19) 0.0338(16) 0.0268(14) -0.0041(12) 0.0008(13) 0.0062(14) C18 0.0454(19) 0.0380(16) 0.0345(15) -0.0098(13) -0.0075(15) 0.0008(15) C19 0.0332(16) 0.0380(16) 0.0318(14) -0.0046(12) -0.0051(13) -0.0009(14) C20 0.0413(17) 0.0247(13) 0.0271(13) -0.0048(11) -0.0006(12) -0.0028(13) C21 0.065(2) 0.0315(15) 0.0343(15) 0.0068(14) 0.0060(16) 0.0050(16) C22 0.058(2) 0.0432(18) 0.0382(16) -0.0015(14) 0.0166(16) -0.0023(17) C23 0.0424(17) 0.0363(15) 0.0383(15) -0.0153(13) -0.0011(14) -0.0028(15) C24 0.0424(18) 0.0301(14) 0.0422(16) -0.0043(13) -0.0097(14) 0.0014(13) C25 0.0424(18) 0.0287(14) 0.0320(15) 0.0021(12) -0.0046(13) -0.0051(13) C26 0.047(2) 0.060(2) 0.061(2) -0.024(2) 0.0023(19) -0.0010(18) 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' S S 0.1246 0.1234 '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 O3 S1 O4 120.51(15) O3 S1 N1 106.32(12) O3 S1 C20 107.64(14) O4 S1 N1 106.53(12) O4 S1 C20 106.67(13) N1 S1 C20 108.78(13) C7 O1 C6 117.3(2) C10 O2 C13 116.6(2) C1 N1 S1 119.30(17) C1 N1 C5 112.9(2) C5 N1 S1 117.96(18) N1 C1 H1A 110.0 N1 C1 H1B 110.0 N1 C1 C2 108.6(2) H1A C1 H1B 108.4 C2 C1 H1A 110.0 C2 C1 H1B 110.0 C1 C2 H2 107.9 C1 C2 C3 110.6(2) C3 C2 H2 107.9 C6 C2 C1 111.8(2) C6 C2 H2 107.9 C6 C2 C3 110.8(2) C2 C3 H3 108.0 C4 C3 C2 109.7(2) C4 C3 H3 108.0 C14 C3 C2 112.4(2) C14 C3 H3 108.0 C14 C3 C4 110.8(2) C3 C4 H4A 109.1 C3 C4 H4B 109.1 H4A C4 H4B 107.8 C5 C4 C3 112.6(2) C5 C4 H4A 109.1 C5 C4 H4B 109.1 N1 C5 C4 108.7(2) N1 C5 H5A 109.9 N1 C5 H5B 109.9 C4 C5 H5A 109.9 C4 C5 H5B 109.9 H5A C5 H5B 108.3 O1 C6 C2 107.8(2) O1 C6 H6A 110.1 O1 C6 H6B 110.1 C2 C6 H6A 110.1 C2 C6 H6B 110.1 H6A C6 H6B 108.5 O1 C7 C8 115.5(2) O1 C7 C12 124.9(2) C12 C7 C8 119.6(2) C7 C8 H8 119.6 C9 C8 C7 120.7(3) C9 C8 H8 119.6 C8 C9 H9 120.1 C8 C9 C10 119.7(2) C10 C9 H9 120.1 O2 C10 C9 116.0(2) O2 C10 C11 124.5(3) C11 C10 C9 119.6(3) C10 C11 H11 119.7 C10 C11 C12 120.6(3) C12 C11 H11 119.7 C7 C12 C11 119.8(2) C7 C12 H12 120.1 C11 C12 H12 120.1 O2 C13 H13A 109.5 O2 C13 H13B 109.5 O2 C13 H13C 109.5 H13A C13 H13B 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C15 C14 C3 120.4(2) C19 C14 C3 121.4(3) C19 C14 C15 118.2(3) C14 C15 H15 119.6 C16 C15 C14 120.8(3) C16 C15 H15 119.6 C15 C16 H16 119.9 C17 C16 C15 120.2(3) C17 C16 H16 119.9 C16 C17 H17 120.1 C18 C17 C16 119.8(3) C18 C17 H17 120.1 C17 C18 H18 119.9 C17 C18 C19 120.3(3) C19 C18 H18 119.9 C14 C19 H19 119.6 C18 C19 C14 120.8(3) C18 C19 H19 119.6 C21 C20 S1 119.8(2) C21 C20 C25 119.9(3) C25 C20 S1 120.3(2) C20 C21 H21 120.2 C20 C21 C22 119.6(3) C22 C21 H21 120.2 C21 C22 H22 119.3 C21 C22 C23 121.4(3) C23 C22 H22 119.3 C22 C23 C26 120.5(3) C24 C23 C22 117.7(3) C24 C23 C26 121.8(3) C23 C24 H24 119.1 C25 C24 C23 121.8(3) C25 C24 H24 119.1 C20 C25 H25 120.2 C24 C25 C20 119.5(3) C24 C25 H25 120.2 C23 C26 H26A 109.5 C23 C26 H26B 109.5 C23 C26 H26C 109.5 H26A C26 H26B 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 O3 1.429(2) S1 O4 1.431(2) S1 N1 1.628(2) S1 C20 1.759(3) O1 C6 1.434(3) O1 C7 1.380(3) O2 C10 1.375(3) O2 C13 1.424(4) N1 C1 1.464(3) N1 C5 1.472(3) C1 H1A 0.9900 C1 H1B 0.9900 C1 C2 1.526(4) C2 H2 1.0000 C2 C3 1.544(3) C2 C6 1.512(3) C3 H3 1.0000 C3 C4 1.535(4) C3 C14 1.510(4) C4 H4A 0.9900 C4 H4B 0.9900 C4 C5 1.518(4) C5 H5A 0.9900 C5 H5B 0.9900 C6 H6A 0.9900 C6 H6B 0.9900 C7 C8 1.394(3) C7 C12 1.380(4) C8 H8 0.9500 C8 C9 1.377(4) C9 H9 0.9500 C9 C10 1.397(4) C10 C11 1.381(4) C11 H11 0.9500 C11 C12 1.395(4) C12 H12 0.9500 C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 C14 C15 1.395(4) C14 C19 1.391(4) C15 H15 0.9500 C15 C16 1.386(4) C16 H16 0.9500 C16 C17 1.381(4) C17 H17 0.9500 C17 C18 1.375(5) C18 H18 0.9500 C18 C19 1.390(4) C19 H19 0.9500 C20 C21 1.382(4) C20 C25 1.391(4) C21 H21 0.9500 C21 C22 1.383(5) C22 H22 0.9500 C22 C23 1.389(5) C23 C24 1.388(5) C23 C26 1.499(5) C24 H24 0.9500 C24 C25 1.373(5) C25 H25 0.9500 C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 0.9800 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 S1 N1 C1 C2 151.43(19) S1 N1 C5 C4 -153.2(2) S1 C20 C21 C22 -177.1(3) S1 C20 C25 C24 177.0(2) O1 C7 C8 C9 178.6(2) O1 C7 C12 C11 -178.5(3) O2 C10 C11 C12 178.4(3) O3 S1 N1 C1 -41.2(2) O3 S1 N1 C5 175.4(2) O3 S1 C20 C21 28.9(3) O3 S1 C20 C25 -149.7(2) O4 S1 N1 C1 -170.9(2) O4 S1 N1 C5 45.7(2) O4 S1 C20 C21 159.5(2) O4 S1 C20 C25 -19.0(3) N1 S1 C20 C21 -85.9(3) N1 S1 C20 C25 95.5(2) N1 C1 C2 C3 58.4(3) N1 C1 C2 C6 -177.7(2) C1 N1 C5 C4 61.1(3) C1 C2 C3 C4 -53.4(3) C1 C2 C3 C14 -177.1(2) C1 C2 C6 O1 52.9(3) C2 C3 C4 C5 52.2(3) C2 C3 C14 C15 57.2(3) C2 C3 C14 C19 -122.7(3) C3 C2 C6 O1 176.7(2) C3 C4 C5 N1 -54.9(3) C3 C14 C15 C16 178.9(2) C3 C14 C19 C18 -178.6(3) C4 C3 C14 C15 -65.8(3) C4 C3 C14 C19 114.2(3) C5 N1 C1 C2 -63.4(3) C6 O1 C7 C8 177.0(2) C6 O1 C7 C12 -3.0(4) C6 C2 C3 C4 -177.8(2) C6 C2 C3 C14 58.5(3) C7 O1 C6 C2 178.0(2) C7 C8 C9 C10 -0.6(4) C8 C7 C12 C11 1.5(4) C8 C9 C10 O2 -178.3(2) C8 C9 C10 C11 2.5(4) C9 C10 C11 C12 -2.4(4) C10 C11 C12 C7 0.4(4) C12 C7 C8 C9 -1.4(4) C13 O2 C10 C9 170.7(3) C13 O2 C10 C11 -10.1(4) C14 C3 C4 C5 176.8(2) C14 C15 C16 C17 0.2(4) C15 C14 C19 C18 1.5(4) C15 C16 C17 C18 0.5(5) C16 C17 C18 C19 -0.2(5) C17 C18 C19 C14 -0.8(5) C19 C14 C15 C16 -1.2(4) C20 S1 N1 C1 74.5(2) C20 S1 N1 C5 -68.9(2) C20 C21 C22 C23 0.3(5) C21 C20 C25 C24 -1.6(4) C21 C22 C23 C24 -1.9(5) C21 C22 C23 C26 177.2(3) C22 C23 C24 C25 1.8(5) C23 C24 C25 C20 -0.1(4) C25 C20 C21 C22 1.5(5) C26 C23 C24 C25 -177.3(3)