#------------------------------------------------------------------------------ #$Date: 2014-05-20 11:05:40 +0300 (Tue, 20 May 2014) $ #$Revision: 113995 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/51/61/1516148.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_1516148 loop_ _publ_author_name 'Zipfel, Hannes F.' 'Carreira, Erick M.' _publ_section_title ; An Efficient Synthesis Strategy to the Core Structure of 6--5--6--5--6-Membered Epipolythiodiketopiperazines ; _journal_name_full 'Organic Letters' _journal_page_first 140519083547004 _journal_paper_doi 10.1021/ol500990f _journal_year 2014 _chemical_absolute_configuration ad _chemical_formula_moiety 'C21 H24 N2 O4 S' _chemical_formula_sum 'C21 H24 N2 O4 S' _chemical_formula_weight 400.48 _chemical_name_systematic '(2R,3S)-ethyl 3-(1H-indol-3-yl)-2-(4-methylphenylsulfonamido)butanoate' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_date 2013-12-16 _audit_creation_method ; Olex2 1.2 (compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736) ; _cell_angle_alpha 90 _cell_angle_beta 106.278(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.6390(7) _cell_length_b 5.5765(3) _cell_length_c 15.5447(10) _cell_measurement_reflns_used 5959 _cell_measurement_temperature 100 _cell_measurement_theta_max 27.53 _cell_measurement_theta_min 2.57 _cell_volume 968.48(10) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics OLEX2 _computing_publication_material OLEX2 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _diffrn_ambient_temperature 100.0(2) _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 8.33 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'kappa-stage diffractometer' _diffrn_measurement_device_type 'Bruker/Nonius Kappa Apex2' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_unetI/netI 0.0471 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 22103 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.594 _diffrn_reflns_theta_min 2.565 _diffrn_source 'sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.198 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6831 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0560 before and 0.0501 after correction. The Ratio of minimum to maximum transmission is 0.9162. The \l/2 correction factor is 0.0000. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.373 _exptl_crystal_description needle _exptl_crystal_F_000 424 _exptl_crystal_recrystallization_method 'Crystallized form CDCl3' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.045 _exptl_crystal_size_min 0.015 _refine_diff_density_max 0.234 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.047 _refine_ls_abs_structure_details ; Flack x determined using 1555 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.04(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 262 _refine_ls_number_reflns 4487 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0341 _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^)+(0.0365P)^2^+0.0450P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.0720 _reflns_Friedel_coverage 0.811 _reflns_number_gt 3847 _reflns_number_total 4487 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file ol500990f_si_003.cif _[local]_cod_data_source_block ca101213_0ma _[local]_cod_cif_authors_sg_H-M 'P 21' _cod_database_code 1516148 _shelxl_version_number 2013-4 _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 0.997 _shelx_estimated_absorpt_t_min 0.954 _diffrn_reflns_laue_measured_fraction_full 0.998 _diffrn_reflns_laue_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _reflns_friedel_fraction_full 1.000 _reflns_friedel_fraction_max 0.997 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances N2-H2 0.91 with sigma of 0.02 N1-H1 0.91 with sigma of 0.02 3.a Ternary CH refined with riding coordinates: C6(H6), C7(H7) 3.b Secondary CH2 refined with riding coordinates: C18(H18A,H18B) 3.c Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C20(H20), C21(H21) 3.d Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C13(H13A,H13B,H13C), C19(H19A,H19B,H19C) ; _shelx_res_file ; TITL ca101213_0ma in P2(1) CELL 0.71073 11.639 5.5765 15.5447 90 106.278 90 ZERR 2 0.0007 0.0003 0.001 0 0.003 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O S UNIT 42 48 4 8 2 DFIX 0.91 N2 H2 DFIX 0.91 N1 H1 L.S. 8 PLAN -5 0 0 SIZE 0.015 0.045 0.24 TEMP -173.16 HTAB BOND $H fmap 2 acta MORE -1 CONF OMIT 0 0 1 OMIT 1 0 0 OMIT -1 0 1 REM D:/SMoCC_Strukturen/ca101213/work/ca101213_0ma.hkl WGHT 0.036500 0.045000 FVAR 0.26100 S1 5 0.004163 0.658499 0.229322 11.00000 0.01140 0.01519 = 0.01224 0.00090 0.00390 -0.00153 O1 4 -0.081804 0.836642 0.187284 11.00000 0.01144 0.02460 = 0.01656 0.00285 0.00255 0.00169 O2 4 0.322098 0.839028 0.286392 11.00000 0.01472 0.01475 = 0.01190 -0.00027 0.00005 0.00045 O3 4 0.250201 1.212012 0.256266 11.00000 0.02024 0.01194 = 0.02051 -0.00465 0.00583 -0.00139 O4 4 -0.030632 0.413151 0.230858 11.00000 0.01972 0.01958 = 0.01670 -0.00097 0.00647 -0.00731 N1 3 0.108937 0.661192 0.179325 11.00000 0.01333 0.01030 = 0.01301 0.00133 0.00511 -0.00125 H1 2 0.159577 0.542729 0.198565 11.00000 -1.20000 N2 3 0.378085 1.356376 0.025803 11.00000 0.01723 0.01159 = 0.01497 0.00282 0.00709 0.00166 H2 2 0.384991 1.476219 -0.009731 11.00000 -1.20000 C1 1 0.218403 0.947819 0.615686 11.00000 0.02694 0.03009 = 0.01942 -0.00354 0.00881 -0.00367 AFIX 137 H1A 2 0.160297 0.908907 0.648609 11.00000 -1.50000 H1B 2 0.234886 1.120413 0.619904 11.00000 -1.50000 H1C 2 0.292808 0.859298 0.641612 11.00000 -1.50000 AFIX 0 C2 1 0.168259 0.878742 0.519220 11.00000 0.01644 0.02156 = 0.01497 -0.00334 0.00862 -0.00597 C3 1 0.086002 1.026586 0.460603 11.00000 0.02290 0.01602 = 0.01964 -0.00459 0.01039 -0.00180 AFIX 43 H3 2 0.063437 1.173935 0.481900 11.00000 -1.20000 AFIX 0 C4 1 0.036496 0.962893 0.371887 11.00000 0.01856 0.01591 = 0.01795 0.00386 0.00670 0.00148 AFIX 43 H4 2 -0.018897 1.066176 0.332386 11.00000 -1.20000 AFIX 0 C5 1 0.068472 0.748180 0.341588 11.00000 0.01162 0.01694 = 0.01273 -0.00084 0.00590 -0.00307 C6 1 0.160146 0.885831 0.157843 11.00000 0.01145 0.00987 = 0.01294 0.00115 0.00345 -0.00052 AFIX 13 H6 2 0.093252 1.000899 0.132721 11.00000 -1.20000 AFIX 0 C7 1 0.222270 0.829571 0.084287 11.00000 0.01274 0.01305 = 0.01163 0.00132 0.00439 0.00116 AFIX 13 H7 2 0.271695 0.682011 0.103282 11.00000 -1.20000 AFIX 0 C8 1 0.305290 1.025755 0.073117 11.00000 0.01285 0.01324 = 0.01070 -0.00168 0.00570 0.00127 C9 1 0.431985 1.037894 0.115716 11.00000 0.01214 0.01176 = 0.01081 -0.00234 0.00659 -0.00007 C10 1 0.474165 1.247684 0.084582 11.00000 0.01423 0.01368 = 0.01108 -0.00265 0.00660 0.00013 C11 1 0.594594 1.314146 0.111489 11.00000 0.02007 0.01173 = 0.01490 -0.00422 0.01004 -0.00428 AFIX 43 H11 2 0.621160 1.458941 0.091137 11.00000 -1.20000 AFIX 0 C12 1 0.673716 1.161238 0.168875 11.00000 0.01527 0.02181 = 0.01476 -0.00550 0.00721 -0.00658 AFIX 43 H12 2 0.756309 1.201331 0.188259 11.00000 -1.20000 AFIX 0 C13 1 0.128103 0.771242 -0.003443 11.00000 0.01499 0.01810 = 0.01482 -0.00115 0.00526 -0.00203 AFIX 137 H13A 2 0.081532 0.915704 -0.026195 11.00000 -1.50000 H13B 2 0.074588 0.645940 0.007111 11.00000 -1.50000 H13C 2 0.167718 0.714626 -0.047583 11.00000 -1.50000 AFIX 0 C14 1 0.278068 1.220362 0.018836 11.00000 0.01337 0.01663 = 0.01285 -0.00181 0.00411 0.00228 AFIX 43 H14 2 0.200485 1.257025 -0.018723 11.00000 -1.20000 AFIX 0 C15 1 0.514593 0.885324 0.173830 11.00000 0.01545 0.01459 = 0.01468 0.00216 0.00669 0.00098 AFIX 43 H15 2 0.488809 0.741599 0.195494 11.00000 -1.20000 AFIX 0 C16 1 0.634413 0.949270 0.198787 11.00000 0.01343 0.02211 = 0.01439 0.00059 0.00219 0.00254 AFIX 43 H16 2 0.691147 0.846140 0.237215 11.00000 -1.20000 AFIX 0 C17 1 0.246752 1.001157 0.238190 11.00000 0.01217 0.01549 = 0.01164 0.00130 0.00728 0.00066 C18 1 0.410756 0.927538 0.364852 11.00000 0.01862 0.02607 = 0.01620 -0.00303 -0.00147 -0.00325 AFIX 23 H18A 2 0.371488 0.997943 0.407812 11.00000 -1.20000 H18B 2 0.460870 1.052236 0.347845 11.00000 -1.20000 AFIX 0 C19 1 0.485679 0.716582 0.405796 11.00000 0.02221 0.03680 = 0.02111 0.00468 -0.00265 0.00580 AFIX 137 H19A 2 0.434830 0.594573 0.422014 11.00000 -1.50000 H19B 2 0.547301 0.767934 0.459639 11.00000 -1.50000 H19C 2 0.523985 0.649056 0.362554 11.00000 -1.50000 AFIX 0 C20 1 0.150881 0.597724 0.398162 11.00000 0.01658 0.01745 = 0.01715 -0.00085 0.00612 0.00194 AFIX 43 H20 2 0.173329 0.450622 0.376609 11.00000 -1.20000 AFIX 0 C21 1 0.199824 0.665456 0.486480 11.00000 0.01505 0.02122 = 0.01703 0.00479 0.00373 0.00284 AFIX 43 H21 2 0.256370 0.563221 0.525515 11.00000 -1.20000 AFIX 0 HKLF 4 REM ca101213_0ma in P2(1) REM R1 = 0.0341 for 3847 Fo > 4sig(Fo) and 0.0465 for all 4487 data REM 262 parameters refined using 3 restraints END WGHT 0.0365 0.0449 REM Instructions for potential hydrogen bonds EQIV $1 x, y-1, z HTAB N1 O3_$1 EQIV $2 x, y+1, z HTAB C4 O4_$2 HTAB C7 N2_$1 EQIV $3 -x, y+1/2, -z HTAB C14 O1_$3 HTAB C20 O3_$1 REM Highest difference peak 0.234, deepest hole -0.312, 1-sigma level 0.047 Q1 1 0.1888 0.8479 0.1174 11.00000 0.05 0.23 Q2 1 0.0485 0.7200 0.2852 11.00000 0.05 0.20 Q3 1 0.4539 1.1695 0.1179 11.00000 0.05 0.19 Q4 1 0.2056 0.9314 0.1935 11.00000 0.05 0.19 Q5 1 0.1219 1.2848 -0.0226 11.00000 0.05 0.19 REM The information below was added by Olex2. REM REM R1 = 0.0341 for 3847 Fo > 4sig(Fo) and 0.0465 for all 22145 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.23, deepest hole -0.31 REM Mean Shift 0, Max Shift 0. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0465 REM R1_gt = 0.0341 REM wR_ref = 0.0720 REM GOOF = 1.028 REM Shift_max = 0 REM Shift_mean = 0 REM Reflections_all = 22145 REM Reflections_gt = 3847 REM Parameters = n/a REM Hole = -0.31 REM Peak = 0.23 REM Flack = 0.04(3) ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn S1 S 0.00416(5) 0.65850(11) 0.22932(4) 0.01282(14) Uani 1 1 d . O1 O -0.08180(14) 0.8366(3) 0.18728(11) 0.0178(4) Uani 1 1 d . O2 O 0.32210(14) 0.8390(3) 0.28639(10) 0.0145(4) Uani 1 1 d . O3 O 0.25020(15) 1.2120(3) 0.25627(12) 0.0175(4) Uani 1 1 d . O4 O -0.03063(15) 0.4132(3) 0.23086(11) 0.0184(4) Uani 1 1 d . N1 N 0.10894(16) 0.6612(4) 0.17932(12) 0.0119(4) Uani 1 1 d D H1 H 0.160(2) 0.543(4) 0.1986(16) 0.014 Uiso 1 1 d DR N2 N 0.37808(18) 1.3564(4) 0.02580(14) 0.0141(4) Uani 1 1 d D H2 H 0.385(2) 1.476(4) -0.0097(16) 0.017 Uiso 1 1 d DR C1 C 0.2184(3) 0.9478(5) 0.61569(18) 0.0250(6) Uani 1 1 d . H1A H 0.1603 0.9089 0.6486 0.038 Uiso 1 1 calc GR H1B H 0.2349 1.1204 0.6199 0.038 Uiso 1 1 calc GR H1C H 0.2928 0.8593 0.6416 0.038 Uiso 1 1 calc GR C2 C 0.1683(2) 0.8787(5) 0.51922(16) 0.0168(6) Uani 1 1 d . C3 C 0.0860(2) 1.0266(5) 0.46060(17) 0.0186(6) Uani 1 1 d . H3 H 0.0634 1.1739 0.4819 0.022 Uiso 1 1 calc R C4 C 0.0365(2) 0.9629(4) 0.37189(17) 0.0172(6) Uani 1 1 d . H4 H -0.0189 1.0662 0.3324 0.021 Uiso 1 1 calc R C5 C 0.0685(2) 0.7482(4) 0.34159(16) 0.0133(5) Uani 1 1 d . C6 C 0.1601(2) 0.8858(4) 0.15784(15) 0.0114(5) Uani 1 1 d . H6 H 0.0933 1.0009 0.1327 0.014 Uiso 1 1 calc R C7 C 0.2223(2) 0.8296(4) 0.08429(15) 0.0123(5) Uani 1 1 d . H7 H 0.2717 0.6820 0.1033 0.015 Uiso 1 1 calc R C8 C 0.3053(2) 1.0258(5) 0.07312(15) 0.0118(5) Uani 1 1 d . C9 C 0.4320(2) 1.0379(4) 0.11572(15) 0.0109(5) Uani 1 1 d . C10 C 0.4742(2) 1.2477(4) 0.08458(16) 0.0124(5) Uani 1 1 d . C11 C 0.5946(2) 1.3141(4) 0.11149(16) 0.0145(5) Uani 1 1 d . H11 H 0.6212 1.4589 0.0911 0.017 Uiso 1 1 calc R C12 C 0.6737(2) 1.1612(5) 0.16887(15) 0.0167(5) Uani 1 1 d . H12 H 0.7563 1.2013 0.1883 0.020 Uiso 1 1 calc R C13 C 0.1281(2) 0.7712(5) -0.00344(16) 0.0157(5) Uani 1 1 d . H13A H 0.0815 0.9157 -0.0262 0.024 Uiso 1 1 calc GR H13B H 0.0746 0.6459 0.0071 0.024 Uiso 1 1 calc GR H13C H 0.1677 0.7146 -0.0476 0.024 Uiso 1 1 calc GR C14 C 0.2781(2) 1.2204(4) 0.01884(16) 0.0142(5) Uani 1 1 d . H14 H 0.2005 1.2570 -0.0187 0.017 Uiso 1 1 calc R C15 C 0.5146(2) 0.8853(5) 0.17383(16) 0.0144(5) Uani 1 1 d . H15 H 0.4888 0.7416 0.1955 0.017 Uiso 1 1 calc R C16 C 0.6344(2) 0.9493(5) 0.19879(17) 0.0170(5) Uani 1 1 d . H16 H 0.6911 0.8461 0.2372 0.020 Uiso 1 1 calc R C17 C 0.2468(2) 1.0012(4) 0.23819(15) 0.0123(5) Uani 1 1 d . C18 C 0.4108(2) 0.9275(5) 0.36485(17) 0.0216(6) Uani 1 1 d . H18A H 0.3715 0.9979 0.4078 0.026 Uiso 1 1 calc R H18B H 0.4609 1.0522 0.3478 0.026 Uiso 1 1 calc R C19 C 0.4857(2) 0.7166(5) 0.40580(19) 0.0285(7) Uani 1 1 d . H19A H 0.4348 0.5946 0.4220 0.043 Uiso 1 1 calc GR H19B H 0.5473 0.7679 0.4596 0.043 Uiso 1 1 calc GR H19C H 0.5240 0.6491 0.3626 0.043 Uiso 1 1 calc GR C20 C 0.1509(2) 0.5977(4) 0.39816(16) 0.0168(6) Uani 1 1 d . H20 H 0.1733 0.4506 0.3766 0.020 Uiso 1 1 calc R C21 C 0.1998(2) 0.6655(5) 0.48648(15) 0.0179(5) Uani 1 1 d . H21 H 0.2564 0.5632 0.5255 0.022 Uiso 1 1 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0114(3) 0.0152(3) 0.0122(3) 0.0009(3) 0.0039(2) -0.0015(3) O1 0.0114(9) 0.0246(10) 0.0166(9) 0.0029(8) 0.0026(7) 0.0017(8) O2 0.0147(9) 0.0147(9) 0.0119(8) -0.0003(7) 0.0001(7) 0.0004(7) O3 0.0202(9) 0.0119(11) 0.0205(9) -0.0047(7) 0.0058(7) -0.0014(7) O4 0.0197(9) 0.0196(10) 0.0167(9) -0.0010(8) 0.0065(7) -0.0073(8) N1 0.0133(10) 0.0103(10) 0.0130(9) 0.0013(10) 0.0051(8) -0.0012(10) N2 0.0172(11) 0.0116(11) 0.0150(11) 0.0028(9) 0.0071(9) 0.0017(9) C1 0.0269(15) 0.0301(16) 0.0194(14) -0.0035(12) 0.0088(12) -0.0037(13) C2 0.0164(13) 0.0216(14) 0.0150(13) -0.0033(11) 0.0086(10) -0.0060(11) C3 0.0229(14) 0.0160(12) 0.0196(13) -0.0046(11) 0.0104(11) -0.0018(11) C4 0.0186(13) 0.0159(13) 0.0180(13) 0.0039(11) 0.0067(11) 0.0015(11) C5 0.0116(12) 0.0169(12) 0.0127(12) -0.0008(10) 0.0059(10) -0.0031(10) C6 0.0114(11) 0.0099(12) 0.0129(12) 0.0012(10) 0.0035(9) -0.0005(10) C7 0.0127(12) 0.0131(12) 0.0116(12) 0.0013(10) 0.0044(10) 0.0012(10) C8 0.0128(12) 0.0132(12) 0.0107(11) -0.0017(10) 0.0057(10) 0.0013(10) C9 0.0121(12) 0.0118(11) 0.0108(11) -0.0023(10) 0.0066(10) -0.0001(10) C10 0.0142(12) 0.0137(12) 0.0111(12) -0.0026(9) 0.0066(10) 0.0001(10) C11 0.0201(13) 0.0117(12) 0.0149(13) -0.0042(10) 0.0100(10) -0.0043(10) C12 0.0153(12) 0.0218(13) 0.0148(12) -0.0055(13) 0.0072(9) -0.0066(13) C13 0.0150(13) 0.0181(13) 0.0148(13) -0.0012(10) 0.0053(10) -0.0020(10) C14 0.0134(12) 0.0166(14) 0.0129(12) -0.0018(10) 0.0041(9) 0.0023(10) C15 0.0154(12) 0.0146(13) 0.0147(12) 0.0022(10) 0.0067(10) 0.0010(10) C16 0.0134(12) 0.0221(14) 0.0144(13) 0.0006(10) 0.0022(10) 0.0025(11) C17 0.0122(12) 0.0155(14) 0.0116(12) 0.0013(10) 0.0073(10) 0.0007(10) C18 0.0186(13) 0.0261(15) 0.0162(13) -0.0030(11) -0.0015(11) -0.0032(12) C19 0.0222(14) 0.037(2) 0.0211(14) 0.0047(12) -0.0026(11) 0.0058(13) C20 0.0166(13) 0.0174(14) 0.0171(13) -0.0009(10) 0.0061(11) 0.0019(10) C21 0.0151(12) 0.0212(13) 0.0170(12) 0.0048(13) 0.0037(9) 0.0028(13) 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 O1 S1 N1 107.37(11) O1 S1 C5 107.63(11) O4 S1 O1 120.47(11) O4 S1 N1 105.78(11) O4 S1 C5 107.34(11) N1 S1 C5 107.69(10) C17 O2 C18 116.35(19) S1 N1 H1 110.6(17) C6 N1 S1 121.76(17) C6 N1 H1 116.3(17) C10 N2 H2 123.4(17) C14 N2 H2 126.4(17) C14 N2 C10 108.9(2) H1A C1 H1B 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 C2 C1 H1A 109.5 C2 C1 H1B 109.5 C2 C1 H1C 109.5 C3 C2 C1 120.4(2) C21 C2 C1 121.3(2) C21 C2 C3 118.2(2) C2 C3 H3 119.4 C4 C3 C2 121.2(2) C4 C3 H3 119.4 C3 C4 H4 120.4 C5 C4 C3 119.2(2) C5 C4 H4 120.4 C4 C5 S1 120.27(19) C4 C5 C20 121.0(2) C20 C5 S1 118.75(19) N1 C6 H6 108.4 N1 C6 C7 107.42(18) N1 C6 C17 113.27(19) C7 C6 H6 108.4 C17 C6 H6 108.4 C17 C6 C7 110.83(19) C6 C7 H7 107.3 C8 C7 C6 112.8(2) C8 C7 H7 107.3 C8 C7 C13 112.10(19) C13 C7 C6 109.66(18) C13 C7 H7 107.3 C9 C8 C7 126.2(2) C14 C8 C7 127.5(2) C14 C8 C9 106.2(2) C10 C9 C8 107.0(2) C10 C9 C15 118.9(2) C15 C9 C8 134.0(2) N2 C10 C9 107.4(2) N2 C10 C11 130.2(2) C11 C10 C9 122.4(2) C10 C11 H11 121.3 C12 C11 C10 117.5(2) C12 C11 H11 121.3 C11 C12 H12 119.4 C11 C12 C16 121.1(2) C16 C12 H12 119.4 C7 C13 H13A 109.5 C7 C13 H13B 109.5 C7 C13 H13C 109.5 H13A C13 H13B 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 N2 C14 H14 124.8 C8 C14 N2 110.4(2) C8 C14 H14 124.8 C9 C15 H15 120.7 C16 C15 C9 118.5(2) C16 C15 H15 120.7 C12 C16 H16 119.2 C15 C16 C12 121.6(2) C15 C16 H16 119.2 O2 C17 C6 110.9(2) O3 C17 O2 123.8(2) O3 C17 C6 125.3(2) O2 C18 H18A 110.4 O2 C18 H18B 110.4 O2 C18 C19 106.5(2) H18A C18 H18B 108.6 C19 C18 H18A 110.4 C19 C18 H18B 110.4 C18 C19 H19A 109.5 C18 C19 H19B 109.5 C18 C19 H19C 109.5 H19A C19 H19B 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C5 C20 H20 120.6 C21 C20 C5 118.9(2) C21 C20 H20 120.6 C2 C21 C20 121.5(2) C2 C21 H21 119.3 C20 C21 H21 119.3 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 O1 1.4313(19) S1 O4 1.4290(18) S1 N1 1.6195(19) S1 C5 1.767(2) O2 C17 1.334(3) O2 C18 1.446(3) O3 C17 1.207(3) N1 H1 0.88(2) N1 C6 1.465(3) N2 H2 0.88(2) N2 C10 1.371(3) N2 C14 1.368(3) C1 H1A 0.9800 C1 H1B 0.9800 C1 H1C 0.9800 C1 C2 1.499(3) C2 C3 1.392(4) C2 C21 1.383(4) C3 H3 0.9500 C3 C4 1.384(4) C4 H4 0.9500 C4 C5 1.376(3) C5 C20 1.387(3) C6 H6 1.0000 C6 C7 1.547(3) C6 C17 1.511(3) C7 H7 1.0000 C7 C8 1.502(3) C7 C13 1.526(3) C8 C9 1.439(3) C8 C14 1.357(3) C9 C10 1.406(3) C9 C15 1.406(3) C10 C11 1.396(3) C11 H11 0.9500 C11 C12 1.382(4) C12 H12 0.9500 C12 C16 1.394(4) C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 C14 H14 0.9500 C15 H15 0.9500 C15 C16 1.385(3) C16 H16 0.9500 C18 H18A 0.9900 C18 H18B 0.9900 C18 C19 1.496(4) C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 H20 0.9500 C20 C21 1.383(3) C21 H21 0.9500 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 C6 C7 -160.83(15) S1 N1 C6 C17 76.4(2) S1 C5 C20 C21 -178.89(19) O1 S1 N1 C6 44.62(19) O1 S1 C5 C4 -2.9(2) O1 S1 C5 C20 176.77(19) O4 S1 N1 C6 174.45(17) O4 S1 C5 C4 -133.96(19) O4 S1 C5 C20 45.7(2) N1 S1 C5 C4 112.5(2) N1 S1 C5 C20 -67.8(2) N1 C6 C7 C8 -164.87(19) N1 C6 C7 C13 69.5(2) N1 C6 C17 O2 45.3(3) N1 C6 C17 O3 -136.1(2) N2 C10 C11 C12 -176.6(2) C1 C2 C3 C4 -178.4(2) C1 C2 C21 C20 178.0(2) C2 C3 C4 C5 0.7(4) C3 C2 C21 C20 -0.5(4) C3 C4 C5 S1 178.5(2) C3 C4 C5 C20 -1.2(4) C4 C5 C20 C21 0.8(4) C5 S1 N1 C6 -71.0(2) C5 C20 C21 C2 0.1(4) C6 C7 C8 C9 94.1(3) C6 C7 C8 C14 -88.9(3) C7 C6 C17 O2 -75.5(2) C7 C6 C17 O3 103.1(3) C7 C8 C9 C10 178.5(2) C7 C8 C9 C15 2.2(4) C7 C8 C14 N2 -178.8(2) C8 C9 C10 N2 -0.3(2) C8 C9 C10 C11 -179.1(2) C8 C9 C15 C16 176.5(2) C9 C8 C14 N2 -1.3(3) C9 C10 C11 C12 1.9(3) C9 C15 C16 C12 1.0(4) C10 N2 C14 C8 1.2(3) C10 C9 C15 C16 0.6(3) C10 C11 C12 C16 -0.2(3) C11 C12 C16 C15 -1.3(4) C13 C7 C8 C9 -141.6(2) C13 C7 C8 C14 35.5(3) C14 N2 C10 C9 -0.5(3) C14 N2 C10 C11 178.1(2) C14 C8 C9 C10 1.0(2) C14 C8 C9 C15 -175.3(3) C15 C9 C10 N2 176.7(2) C15 C9 C10 C11 -2.1(3) C17 O2 C18 C19 -178.5(2) C17 C6 C7 C8 -40.6(3) C17 C6 C7 C13 -166.32(19) C18 O2 C17 O3 0.8(3) C18 O2 C17 C6 179.30(19) C21 C2 C3 C4 0.2(4) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 -1 0 0.11 0.27 0 -1 0 -0.16 0.23 0 -1 0 0 0.2 0 1 0 0.04 0.23 0 1 0 0.04 0.25 0 1 0 0.15 0.18 0 1 0 -0.14 0.18 0 1 0 -0.12 0.23 0 -2 0 73.49 1.57 0 -2 0 72.65 2.08 0 -2 0 70.55 1.81 0 2 0 72.2 1.81 0 2 0 71.02 1.71 0 2 0 72.7 1.7 0 2 0 74.22 1.79 0 2 0 72.35 1.7 0 2 0 76.16 2.1 0 -3 0 -0.48 0.42 0 -3 0 0.39 0.41 0 -3 0 0.1 0.25 0 -3 0 -0.45 0.46 0 3 0 -1.16 0.37 0 3 0 0.27 0.38 0 3 0 0.04 0.41 0 3 0 0.17 0.36 0 3 0 -0.17 0.39 0 -4 0 39.57 1.58 0 -4 0 38.55 1.54 0 4 0 41.6 1.51 0 4 0 37.52 1.49 0 4 0 37.79 1.34 0 4 0 38.1 1.51 0 -5 0 -0.14 0.55 0 5 0 0.05 0.57 0 5 0 0.14 0.57 0 5 0 -0.25 0.58 0 -6 0 21.11 1.41 0 6 0 20.12 1.44 0 -7 0 -0.12 0.66 0 7 0 -0.44 0.68 -1 7 0 1.27 0.85 1 -7 0 1 0.89 -1 6 0 7.9 1.12 1 -6 0 9.48 1.19 -1 5 0 22.02 1.64 -1 5 0 19.32 1.43 -1 5 0 24.83 1.46 1 -5 0 22.39 1.52 -1 4 0 29.99 1.45 -1 4 0 31.24 1.52 -1 4 0 28.85 1.39 1 -4 0 26.19 1.45 1 -4 0 27.42 1.06 1 -4 0 29.01 1.48 -1 3 0 28.3 1.22 -1 3 0 27.27 0.92 -1 3 0 26.56 0.84 -1 3 0 26.59 1.24 -1 3 0 24.69 1.23 -1 3 0 26.33 1.31 1 -3 0 26.27 1.35 1 -3 0 24.96 1.03 -1 2 0 31.76 1.17 -1 2 0 32.02 1.18 -1 2 0 32.82 1.22 -1 2 0 33.17 0.9 -1 2 0 33.11 1.19 1 -2 0 33.49 1.1 1 -2 0 31.81 1.29 1 -2 0 33.64 1.08 -1 1 0 230.84 4.57 -1 1 0 226.97 4.54 -1 1 0 229.78 4.55 -1 1 0 224.07 4.54 -1 1 0 235.55 4.43 -1 1 0 235.17 4.06 -1 1 0 229.91 4.6 1 -1 0 236.03 4.52 1 -1 0 233.04 4.43 1 -1 0 226.05 4.59 1 -1 0 235.83 4 -1 0 0 0.04 0.08 -1 0 0 0.23 0.14 -1 0 0 0 0.08 1 0 0 0.05 0.11 1 0 0 -0.03 0.11 1 0 0 0.11 0.09 1 0 0 -0.01 0.09 -1 -1 0 235.67 4.91 -1 -1 0 231.64 4.8 1 1 0 228.27 4.89 1 1 0 231.56 4.79 -1 -2 0 33.37 0.94 -1 -2 0 32.95 1.42 1 2 0 33.72 0.82 1 2 0 33.5 1.37 1 2 0 33.65 1.28 1 2 0 32.89 0.83 -1 -3 0 26.18 1.5 -1 -3 0 26.31 1.04 1 3 0 24.99 1.21 1 3 0 26.81 0.91 1 3 0 26.18 1.42 1 3 0 25.2 0.89 1 3 0 26.58 0.94 -1 -4 0 31.3 1.74 -1 -4 0 32.36 1.26 1 4 0 29.49 1.19 1 4 0 29.52 1.38 1 4 0 28.1 1.19 1 4 0 31.45 1.22 1 4 0 31.93 0.99 -1 -5 0 23.62 1.24 1 5 0 23.37 1.21 1 5 0 22.33 1.33 1 5 0 22.68 1.23 -1 -6 0 9.94 0.92 1 6 0 9.37 1.1 1 6 0 7.69 0.96 1 7 0 0.62 0.72 -2 7 0 3.32 1 2 -7 0 4.19 1.1 -2 6 0 1.79 0.87 2 -6 0 1.18 0.87 -2 5 0 7.82 1.11 -2 5 0 7.84 1.06 -2 5 0 5.01 0.97 2 -5 0 6.57 0.75 2 -5 0 6.76 1.1 -2 4 0 9.69 1 -2 4 0 10.91 1.09 -2 4 0 11.9 1.06 -2 4 0 14.13 1 -2 4 0 8.45 0.99 2 -4 0 11.29 0.88 2 -4 0 9.56 1.1 -2 3 0 22.85 1.25 -2 3 0 22.81 1.17 -2 3 0 21.66 1.27 -2 3 0 24.53 1.31 -2 3 0 24.34 1.04 2 -3 0 21.31 1.11 2 -3 0 25.37 1.41 2 -3 0 22.94 1.14 -2 2 0 1.64 0.32 -2 2 0 0.16 0.46 -2 2 0 1.26 0.47 -2 2 0 1.52 0.57 -2 2 0 0.94 0.42 -2 2 0 1.02 0.35 2 -2 0 1.17 0.57 2 -2 0 1.2 0.53 2 -2 0 1.02 0.34 2 -2 0 1.63 0.47 -2 1 0 101.07 2.41 -2 1 0 107.88 2.42 -2 1 0 100.77 2.5 -2 1 0 100.38 2.34 -2 1 0 100.27 2.09 -2 1 0 95.19 2.38 2 -1 0 100.57 2.33 2 -1 0 102.08 2.08 2 -1 0 97.78 2.35 2 -1 0 99.57 2.45 2 -1 0 100.93 2.39 -2 0 0 22.3 0.63 -2 0 0 23.05 0.89 -2 0 0 21.44 0.72 -2 0 0 21.22 0.81 -2 0 0 22.36 0.97 2 0 0 21.95 0.83 2 0 0 20.98 0.72 2 0 0 21.47 0.8 2 0 0 20.93 0.65 2 0 0 21.17 0.77 2 0 0 22.52 0.88 2 0 0 20.79 0.95 -2 -1 0 98.8 2.48 -2 -1 0 97.21 2.6 2 1 0 98.48 2.59 2 1 0 98.57 2.46 2 1 0 100.72 1.96 2 1 0 101.27 1.88 -2 -2 0 1.14 0.51 2 2 0 1.44 0.46 2 2 0 1.87 0.52 -2 -3 0 23.01 0.73 -2 -3 0 23.2 1.42 -2 -3 0 23.04 0.73 2 3 0 23.7 0.72 2 3 0 22.22 1.29 -2 -4 0 10.17 0.69 -2 -4 0 11.47 0.7 -2 -4 0 10.87 1.24 2 4 0 10.56 0.68 2 4 0 10.67 0.66 2 4 0 10.51 1.05 2 4 0 11.07 0.67 -2 -5 0 7.17 0.61 2 5 0 6.3 0.69 2 5 0 7.12 0.77 2 5 0 7.59 0.75 2 6 0 2.22 0.71 2 6 0 2.17 0.65 2 7 0 2.7 0.76 -3 7 0 2.71 1.11 3 -7 0 2.24 1.07 -3 6 0 19.43 1.77 3 -6 0 22.4 1.95 -3 5 0 7.56 1.14 -3 5 0 7.12 1.11 3 -5 0 9.46 1.02 3 -5 0 8.44 1.25 -3 4 0 11.59 0.97 -3 4 0 9.45 1.09 -3 4 0 8.47 1.1 -3 4 0 10.28 0.95 -3 4 0 10.27 1.14 3 -4 0 10.21 1.19 3 -4 0 7.69 0.91 -3 3 0 56.02 2.09 -3 3 0 57.52 1.75 -3 3 0 53.56 1.74 -3 3 0 56.9 2.03 -3 3 0 57.3 1.39 -3 3 0 54.88 2.07 3 -3 0 56.57 1.18 3 -3 0 53.35 2.14 3 -3 0 55.44 1.88 3 -3 0 53.75 1.89 -3 2 0 8.25 0.87 -3 2 0 7.33 0.71 -3 2 0 7.92 0.7 -3 2 0 7.71 0.87 -3 2 0 7.64 0.86 -3 2 0 7.86 0.62 3 -2 0 8.02 0.96 3 -2 0 8.97 0.89 3 -2 0 7.9 0.67 -3 1 0 26.07 1.17 -3 1 0 27.37 1.17 -3 1 0 24.89 1.26 -3 1 0 28.12 1.06 -3 1 0 24.03 1.14 3 -1 0 26.79 1.15 3 -1 0 25.42 1.23 3 -1 0 26.96 1.34 3 -1 0 26.54 1.14 -3 0 0 7.64 0.68 -3 0 0 6.85 0.52 -3 0 0 5.47 0.5 -3 0 0 6.23 0.74 -3 0 0 6.84 0.58 3 0 0 6.9 0.5 3 0 0 6.85 0.58 3 0 0 7.25 0.74 3 0 0 7.27 0.65 3 0 0 5.2 0.57 3 0 0 6.84 0.61 3 0 0 7.38 0.62 -3 -1 0 28.97 1.26 -3 -1 0 26.63 0.73 -3 -1 0 26.22 1.38 3 1 0 24.79 0.89 3 1 0 26.21 0.81 3 1 0 26.03 0.84 3 1 0 26.38 0.83 3 1 0 24.29 1.32 3 1 0 27.61 1.2 -3 -2 0 7.01 0.97 -3 -2 0 5.96 0.81 3 2 0 8.84 0.94 3 2 0 7.62 0.86 -3 -3 0 57.47 2.29 3 3 0 56.11 2.16 -3 -4 0 8.6 1.19 3 4 0 11.09 1.16 3 4 0 10.62 0.53 3 5 0 9.05 0.69 3 5 0 9.69 0.71 3 5 0 8.78 0.7 3 6 0 20.31 1.13 3 6 0 22.47 1.29 3 7 0 5.33 0.82 -4 6 0 1.37 0.96 4 -6 0 2.7 1.11 -4 5 0 -0.6 0.78 4 -5 0 -0.14 0.84 -4 4 0 41.84 1.6 -4 4 0 41.31 1.72 -4 4 0 41.29 2.06 -4 4 0 40.97 1.98 -4 4 0 44.39 2.19 4 -4 0 40.6 2.16 4 -4 0 41.47 1.85 4 -4 0 43.68 1.95 -4 3 0 15.59 1.2 -4 3 0 14 1.01 -4 3 0 15.26 0.83 -4 3 0 14.94 1.22 -4 3 0 13.76 0.81 -4 3 0 15.28 1.26 4 -3 0 15.56 1.2 4 -3 0 11.41 1.2 4 -3 0 15.83 0.83 4 -3 0 14.36 1.12 -4 2 0 63.31 2.2 -4 2 0 66.65 1.93 -4 2 0 68.46 2.3 -4 2 0 63.46 2.25 -4 2 0 64.58 1.97 4 -2 0 64.58 2.2 4 -2 0 66.96 2.21 4 -2 0 63.1 2.31 4 -2 0 67.12 1.83 4 -2 0 63.85 1.97 -4 1 0 1.94 0.54 -4 1 0 1.36 0.32 -4 1 0 0.94 0.51 -4 1 0 1.89 0.62 -4 1 0 1.48 0.57 -4 1 0 1.84 0.63 4 -1 0 1.44 0.63 4 -1 0 1.59 0.55 4 -1 0 1.82 0.54 4 -1 0 1.86 0.51 4 -1 0 1.73 0.56 4 -1 0 1.28 0.57 -4 0 0 33.15 1.18 -4 0 0 32.09 1.55 -4 0 0 32.46 1.42 -4 0 0 32.11 0.98 -4 0 0 32.2 1.27 4 0 0 31.21 1.33 4 0 0 33.67 1.52 4 0 0 30.82 1.25 4 0 0 29.03 1.37 4 0 0 32.79 1.29 4 0 0 32.64 1.16 4 0 0 32.18 1.06 -4 -1 0 1.83 0.4 -4 -1 0 2.26 0.74 -4 -1 0 1.41 0.51 -4 -1 0 1.44 0.46 -4 -1 0 1.84 0.25 4 1 0 1.69 0.42 4 1 0 2.35 0.46 4 1 0 1.75 0.17 4 1 0 2.08 0.4 4 1 0 1.98 0.47 4 1 0 1.76 0.67 4 1 0 1.66 0.52 -4 -2 0 62.13 2.28 -4 -2 0 68.04 2.49 4 2 0 54.78 2.19 4 2 0 64.84 1.38 4 2 0 64.87 1.38 4 2 0 66.86 1.51 4 2 0 65.6 2.45 -4 -3 0 15.39 1.4 4 3 0 16.91 1.42 -4 -4 0 40.92 2.2 -4 -5 0 0.88 0.8 4 5 0 0.27 0.31 4 6 0 3.49 0.59 4 6 0 2.22 0.49 -5 6 0 7.78 1.42 5 -6 0 8.81 1.53 -5 5 0 4.25 1.09 5 -5 0 5.51 1.28 -5 4 0 34.6 1.36 -5 4 0 34.8 1.68 -5 4 0 37.12 2.09 -5 4 0 31.37 1.87 -5 4 0 33.92 2.09 5 -4 0 30.74 2.12 5 -4 0 32.46 0.98 5 -4 0 39.1 1.94 -5 3 0 15.59 1.35 -5 3 0 12.8 0.73 -5 3 0 15.31 0.98 -5 3 0 12.68 1.07 -5 3 0 11.47 1.24 -5 3 0 13.02 1.26 5 -3 0 14.06 1.4 5 -3 0 11.99 0.9 5 -3 0 13.59 1.25 -5 2 0 20.77 1.36 -5 2 0 22.33 1.54 -5 2 0 22.25 1.42 -5 2 0 19.93 1.16 -5 2 0 18.3 1.16 5 -2 0 18.35 1.39 5 -2 0 18.92 1.54 5 -2 0 21.2 1.39 5 -2 0 19.55 1.07 5 -2 0 21.05 1.21 -5 1 0 105.17 2.53 -5 1 0 97.31 2.86 -5 1 0 99.75 2.88 -5 1 0 102.14 2.35 -5 1 0 101.09 3.04 5 -1 0 105.03 2.99 5 -1 0 100.14 2.5 5 -1 0 100.63 2.86 5 -1 0 102.56 3 5 -1 0 109.51 3.11 -5 0 0 3.48 0.55 -5 0 0 2.06 0.46 -5 0 0 2.72 0.86 -5 0 0 2.4 0.55 5 0 0 2.68 0.64 5 0 0 3.85 0.8 5 0 0 2.43 0.66 5 0 0 2.62 0.61 5 0 0 2.75 0.52 5 0 0 2.03 0.51 5 0 0 1.58 0.61 -5 -1 0 101.44 2.91 -5 -1 0 101.99 2.4 -5 -1 0 101.55 2.68 -5 -1 0 103.04 2.28 -5 -1 0 102.61 3.35 5 1 0 108.06 2.95 5 1 0 104.96 2.66 5 1 0 107.35 2.57 5 1 0 107.78 2.13 5 1 0 102.17 2.58 5 1 0 105.36 3.35 5 1 0 99.37 2.63 -5 -2 0 21.92 1.41 -5 -2 0 22.33 1.58 5 2 0 18.72 0.88 5 2 0 19.83 0.84 5 2 0 20.02 1.56 5 2 0 20.34 0.89 5 2 0 20.96 0.88 -5 -3 0 12.41 1.29 5 3 0 14.88 0.64 -5 -4 0 36.17 2.15 -5 -5 0 5.63 1.23 -6 6 0 1.43 1.07 6 -6 0 -0.35 1.02 -6 5 0 8.82 1.44 6 -5 0 7.36 1.45 -6 4 0 49.05 2.54 -6 4 0 47.17 2.38 6 -4 0 51.47 2.64 6 -4 0 50.95 2.36 6 -4 0 51.04 1.61 -6 3 0 1.07 0.64 -6 3 0 0.48 0.58 -6 3 0 0.2 0.67 -6 3 0 0.83 0.27 -6 3 0 1.62 0.75 -6 3 0 0.03 0.67 6 -3 0 0.31 0.79 6 -3 0 0.29 0.68 6 -3 0 0.97 0.56 -6 2 0 3.8 0.84 -6 2 0 4.09 0.83 -6 2 0 4.48 0.75 -6 2 0 6.1 0.49 -6 2 0 5.87 0.92 6 -2 0 4.77 0.69 6 -2 0 5.02 0.96 6 -2 0 5.13 0.84 6 -2 0 4.68 0.92 6 -2 0 4.41 0.85 -6 1 0 6.11 0.76 -6 1 0 5.43 0.99 -6 1 0 5.14 0.53 -6 1 0 4.47 0.82 -6 1 0 4.35 0.76 6 -1 0 4.21 0.88 6 -1 0 4.18 0.8 6 -1 0 4.81 0.88 6 -1 0 6.39 0.89 6 -1 0 5.36 0.71 6 -1 0 4.63 0.92 -6 0 0 6.59 0.73 -6 0 0 5.93 1.06 -6 0 0 7.35 0.8 -6 0 0 6.39 0.6 6 0 0 7.88 0.74 6 0 0 6.78 1.02 6 0 0 7 0.82 6 0 0 7.66 0.91 6 0 0 7.43 0.96 6 0 0 6.73 0.84 -6 -1 0 4.27 0.72 -6 -1 0 4.48 1 -6 -1 0 4.28 0.71 -6 -1 0 4.27 0.61 6 1 0 5.58 0.79 6 1 0 5.22 0.75 6 1 0 4.57 0.71 6 1 0 6.32 1.03 6 1 0 5.01 0.68 6 1 0 5.59 0.73 -6 -2 0 4.34 0.61 -6 -2 0 5.91 1.09 -6 -2 0 5.48 0.89 6 2 0 4.52 0.6 6 2 0 3.92 0.58 6 2 0 5.99 0.59 6 2 0 4.98 0.59 -6 -3 0 0.9 0.38 -6 -3 0 1.59 0.77 -6 -3 0 0.66 0.35 6 3 0 1.29 0.4 6 3 0 0.67 0.4 6 3 0 0.91 0.35 -6 -4 0 49.81 2.6 6 4 0 51.87 1.31 -6 -5 0 6.9 1.37 -7 6 0 -0.45 1 7 -6 0 2.37 1.23 -7 5 0 9.17 1.53 7 -5 0 10.81 1.69 -7 4 0 4.63 1.18 -7 4 0 5.91 1.22 7 -4 0 4.88 0.76 7 -4 0 6.48 1.21 7 -4 0 6.22 1.32 -7 3 0 6.46 0.96 -7 3 0 7.43 1.21 -7 3 0 7.58 0.99 -7 3 0 6.34 1.14 7 -3 0 4.02 0.99 7 -3 0 9.49 1.26 7 -3 0 7.1 0.88 7 -3 0 7.2 1.34 -7 2 0 38.61 1.96 -7 2 0 32.96 1.57 -7 2 0 27.26 1.79 -7 2 0 32.97 1.82 -7 2 0 34.6 1.04 7 -2 0 32.46 1.94 7 -2 0 33.27 2.02 7 -2 0 34.58 1.85 7 -2 0 36.94 1.92 -7 1 0 28.66 1.58 -7 1 0 32.36 1.2 -7 1 0 29.15 1.86 -7 1 0 27.93 1.31 -7 1 0 32.03 1.62 7 -1 0 27.24 1.85 7 -1 0 31.48 1.76 7 -1 0 27.78 1.64 7 -1 0 33.75 1.93 7 -1 0 31.91 1.42 7 -1 0 31.5 1.79 -7 0 0 0.67 0.76 -7 0 0 0.64 0.46 -7 0 0 0.3 0.38 -7 0 0 0.74 0.48 7 0 0 0.88 0.64 7 0 0 0.1 0.49 7 0 0 1.03 0.65 7 0 0 0.73 0.49 7 0 0 0.8 0.6 -7 -1 0 31.72 1.59 -7 -1 0 29.79 1.61 -7 -1 0 30.26 1.3 -7 -1 0 31.19 2.02 7 1 0 30.46 1.5 7 1 0 33.64 1.6 7 1 0 31.58 1.55 7 1 0 30.94 1.45 -7 -2 0 35.67 1.9 -7 -2 0 32.81 2.15 -7 -2 0 34.69 1.5 7 2 0 35.58 1.41 7 2 0 34.88 1.52 7 2 0 35.26 1.43 7 2 0 33.09 1.43 -7 -3 0 7.15 0.71 -7 -3 0 5.14 1.06 7 3 0 7.11 0.7 7 3 0 7.18 0.74 7 3 0 5.12 0.69 -7 -4 0 4.67 1.11 7 4 0 5.58 0.58 7 4 0 6.52 0.63 7 4 0 5.88 0.62 -7 -5 0 11.51 1.69 -8 6 0 1.2 1.16 8 -6 0 1.32 1.27 -8 5 0 1.51 1.01 8 -5 0 1.09 0.46 8 -5 0 -0.25 1.02 -8 4 0 20.93 2.01 -8 4 0 20.79 2.05 8 -4 0 18.89 2.07 8 -4 0 18.77 1.91 8 -4 0 19.73 1.3 -8 3 0 24.68 1.96 -8 3 0 23.1 1.84 -8 3 0 23.97 1.6 -8 3 0 24.1 1.67 8 -3 0 23.41 1.43 8 -3 0 28.97 2.39 8 -3 0 28.92 2.04 8 -3 0 21.16 1.9 -8 2 0 17.14 1.58 -8 2 0 18.17 1.33 -8 2 0 18.78 1.6 -8 2 0 19.7 1.59 -8 2 0 19.44 0.8 8 -2 0 19.88 1.89 8 -2 0 16.57 1.58 8 -2 0 17.82 1.67 -8 1 0 16.3 1.13 -8 1 0 15.59 1.56 -8 1 0 18.82 1.48 -8 1 0 17.03 1.39 -8 1 0 16.35 0.96 8 -1 0 19.25 1.71 8 -1 0 14.7 1.1 8 -1 0 16.36 1.43 8 -1 0 15.2 1.45 8 -1 0 18.23 1.52 -8 0 0 18.31 1.3 -8 0 0 16.08 0.83 -8 0 0 18.33 1.76 -8 0 0 16.83 1.15 8 0 0 15.95 1.35 8 0 0 15.96 1.25 8 0 0 16.6 1.37 8 0 0 17.42 1.13 8 0 0 18.65 1.46 -8 -1 0 16.71 1.74 -8 -1 0 17.76 1.11 -8 -1 0 17.75 1.35 8 1 0 17.09 1.37 8 1 0 16.01 1.3 8 1 0 16.65 1.24 8 1 0 17.67 1.34 -8 -2 0 20.18 1.6 -8 -2 0 19.28 0.79 -8 -2 0 15.86 1.82 -8 -2 0 20.21 1.35 8 2 0 19.13 1.28 8 2 0 20.61 1.32 8 2 0 19.51 1.21 8 2 0 18.73 1.31 -8 -3 0 23.03 1.23 -8 -3 0 22.61 2.01 8 3 0 23.4 1.27 8 3 0 25.5 1.28 8 3 0 24.62 1.33 -8 -4 0 22.11 2.17 8 4 0 18.93 1.09 8 4 0 20.43 1.1 8 4 0 21.63 1.11 -8 -5 0 1.59 1.05 8 5 0 0.54 0.43 8 5 0 1.04 0.42 -9 5 0 1.35 1.11 9 -5 0 0.95 0.61 9 -5 0 1.72 1.32 -9 4 0 2.21 1.08 -9 4 0 2.09 1.15 9 -4 0 2.75 1.25 9 -4 0 2.41 0.81 -9 3 0 5.74 1.11 -9 3 0 4.85 1.22 -9 3 0 6.04 1.08 -9 3 0 5.26 1.19 9 -3 0 5.22 1.4 9 -3 0 6.57 1.31 -9 2 0 34.02 1.73 -9 2 0 33.64 2.07 -9 2 0 32.68 2.07 -9 2 0 35.79 1.13 -9 2 0 33.05 2.01 9 -2 0 30.36 2.22 9 -2 0 34.33 2.3 9 -2 0 31.11 2.01 -9 1 0 3.48 1.01 -9 1 0 4.47 1.15 -9 1 0 5.78 0.71 -9 1 0 5.09 0.83 9 -1 0 3.39 1.04 9 -1 0 2.99 0.94 9 -1 0 3.76 0.99 9 -1 0 6.79 1.14 9 -1 0 7.02 0.92 -9 0 0 3.8 0.49 -9 0 0 3.75 0.76 -9 0 0 2.75 1.13 -9 0 0 4.29 0.77 9 0 0 1.92 0.79 9 0 0 4.57 0.81 9 0 0 3.23 0.82 9 0 0 4.53 1.06 9 0 0 3.28 0.94 -9 -1 0 5.1 0.81 -9 -1 0 4.06 1.21 -9 -1 0 6.01 0.99 9 1 0 5.75 0.98 9 1 0 5.04 0.96 9 1 0 6.56 0.98 9 1 0 4.57 0.95 -9 -2 0 32.61 1.16 -9 -2 0 31.99 1.97 -9 -2 0 33.66 2.59 9 2 0 36.34 1.7 9 2 0 31.66 1.67 9 2 0 33.96 1.78 9 2 0 34.09 1.74 -9 -3 0 5.82 0.85 -9 -3 0 7.3 1.3 9 3 0 6.2 0.9 9 3 0 6.91 0.94 9 3 0 8.18 0.96 -9 -4 0 3.05 1.09 -9 -4 0 3.43 0.49 9 4 0 3.44 0.73 9 4 0 3.12 0.69 -9 -5 0 1.32 1.07 9 5 0 1.92 0.58 9 5 0 1.52 0.57 10 -5 0 1.89 1.37 10 -5 0 4.55 0.86 10 -4 0 10.33 1.81 -10 3 0 2.73 1.09 -10 3 0 1.77 0.94 10 -3 0 1.95 1.24 10 -3 0 4.87 1.26 -10 2 0 10.7 1.57 -10 2 0 10.79 1.51 -10 2 0 9.75 1.18 10 -2 0 9.85 1.47 10 -2 0 10.61 1.59 10 -2 0 17.08 1.91 -10 1 0 53.01 1.94 -10 1 0 53.6 2.48 -10 1 0 53.65 2.86 -10 1 0 54.72 1.93 10 -1 0 54.76 2.85 10 -1 0 57.63 2.85 -10 0 0 11.83 1.31 -10 0 0 12.13 1.77 -10 0 0 13.3 1.22 -10 0 0 13.14 0.55 10 0 0 12.24 1.46 10 0 0 12.22 1.5 10 0 0 14.37 1.52 -10 -1 0 55.9 2.12 -10 -1 0 50.69 3.01 -10 -1 0 56.64 2.47 10 1 0 53.59 2.42 10 1 0 55.66 2.35 10 1 0 53.33 2.48 -10 -2 0 8.9 1.68 -10 -2 0 13.14 1.56 -10 -2 0 11.15 0.84 10 2 0 10.7 1.28 -10 -3 0 0.69 0.9 -10 -3 0 0.96 0.71 10 3 0 2.28 0.8 10 3 0 1.16 0.7 -10 -4 0 9.45 1.64 10 4 0 10.16 1.09 10 4 0 9.59 1.06 -10 -5 0 2.38 1.24 10 5 0 2.37 0.69 11 -4 0 6.1 1.65 -11 3 0 3.05 1.05 -11 3 0 3.94 1.22 11 -3 0 3.44 1.41 11 -3 0 8.44 1.51 -11 2 0 16.61 1.43 -11 2 0 15.1 1.86 11 -2 0 17.96 1.93 11 -2 0 16.05 1.99 11 -2 0 15.72 1.95 -11 1 0 3.82 1.24 -11 1 0 4.7 0.73 -11 1 0 4.2 0.8 11 -1 0 6.64 1.44 11 -1 0 3.85 1.14 -11 0 0 -0.23 0.56 -11 0 0 0.53 1.15 11 0 0 1.23 0.94 11 0 0 0.45 0.87 -11 -1 0 4.43 0.99 -11 -1 0 4.42 1.41 11 1 0 5.04 1.15 11 1 0 4.72 1.09 -11 -2 0 11.12 1.94 -11 -2 0 15.96 1.76 -11 -2 0 18.45 1.06 11 2 0 16.3 1.64 -11 -3 0 3.02 0.91 -11 -3 0 4.99 1.22 11 3 0 6.08 1.09 -11 -4 0 7.79 1.53 11 4 0 6.81 1.06 12 -4 0 6.96 1.78 -12 3 0 2.71 1.07 12 -3 0 1.67 1.35 -12 2 0 1.81 0.82 -12 2 0 4.57 1.44 12 -2 0 3.36 1.43 -12 1 0 2.32 1.25 -12 1 0 0.81 0.67 12 -1 0 2.71 1.19 12 -1 0 2.69 1.16 -12 0 0 23.07 1.65 -12 0 0 20.28 2.34 12 0 0 24.26 2.26 12 0 0 24.23 2.2 -12 -1 0 2.19 1.28 -12 -1 0 1.86 0.9 12 1 0 1.95 1.04 -12 -2 0 6.36 1.3 12 2 0 3.13 1.07 -12 -3 0 1.55 1.07 -12 -3 0 2.46 0.94 12 3 0 1.63 0.89 -12 -4 0 5.1 1.52 12 4 0 5.91 1.08 -13 3 0 5.82 1.23 13 -3 0 5.49 1.68 -13 2 0 0.54 0.82 13 -2 0 0.78 1.26 -13 1 0 2.17 1.39 -13 1 0 3.01 0.67 13 -1 0 2.7 1.31 13 -1 0 2.22 1.19 -13 0 0 12.98 2.11 13 0 0 20 2.18 -13 -1 0 3.39 1.03 -13 -1 0 1.55 1.34 13 1 0 5.31 1.31 -13 -2 0 0.03 0.92 13 2 0 -0.05 0.99 -13 -3 0 6.73 1.5 -13 -3 0 6.48 1.23 13 3 0 8.11 1.42 -14 1 0 0.83 0.41 14 -1 0 1.01 1.22 14 -1 0 0.07 1.28 14 0 0 3.22 1.29 14 1 0 0.74 1.13 14 1 1 17.33 2.13 -14 -1 -1 14.69 2.02 14 0 1 0.71 1.18 14 -1 1 14.3 2.15 13 3 1 3.68 1.16 -13 -3 -1 2.64 1.19 -13 -3 -1 1.54 0.98 13 2 1 3.63 1.21 -13 -2 -1 3.99 1.25 -13 -2 -1 1.82 1.07 13 1 1 12.4 1.81 -13 -1 -1 13.55 1.65 13 0 1 0.26 1.11 13 -1 1 11.42 1.89 13 -1 1 13.58 1.97 -13 1 -1 9.44 0.91 13 -2 1 7.24 1.69 -13 2 -1 2.18 0.92 13 -3 1 5.16 1.66 -13 3 -1 2.45 1.13 12 3 1 3.46 1.01 -12 -3 -1 3.24 1.2 -12 -3 -1 1.9 0.93 12 2 1 3.07 1.09 -12 -2 -1 2 1.02 -12 -2 -1 3.15 1.1 12 1 1 9.36 1.51 -12 -1 -1 10.12 1.42 12 0 1 1.61 1.1 12 0 1 2.8 1.17 -12 0 -1 1 0.77 12 -1 1 9.26 1.64 12 -1 1 10.48 1.62 -12 1 -1 11.63 1.07 12 -2 1 -0.29 1.08 -12 2 -1 -0.05 0.81 12 -3 1 3.1 1.46 -12 3 -1 1.8 1.01 11 4 1 2.92 0.88 -11 -4 -1 2.43 1.12 11 3 1 5.73 1.1 -11 -3 -1 7.29 1.12 -11 -3 -1 6.03 1.34 11 2 1 5.12 1.14 -11 -2 -1 7.91 1.25 -11 -2 -1 4.94 1.13 11 1 1 6.12 1.25 -11 -1 -1 7.64 1.24 11 0 1 7.9 1.42 11 0 1 2.62 1.11 -11 0 -1 5.59 0.98 -11 0 -1 3.17 1.31 11 -1 1 6.12 1.4 11 -1 1 9.2 1.47 -11 1 -1 7.22 0.93 -11 1 -1 7.91 1.54 -11 1 -1 6.51 0.89 11 -2 1 2.93 1.32 11 -2 1 5.19 1.38 -11 2 -1 8.72 1.2 11 -3 1 8.33 1.68 -11 3 -1 7.71 1.26 11 -4 1 2.25 1.4 10 5 1 21.91 1.36 -10 -5 -1 24.77 2.61 10 4 1 -0.02 0.61 -10 -4 -1 0.84 0.57 -10 -4 -1 1.49 1.03 10 3 1 13.25 1.34 -10 -3 -1 12.45 1.23 -10 -3 -1 8.69 1.44 10 2 1 1.63 0.86 -10 -2 -1 2.58 0.93 -10 -2 -1 2.4 0.56 -10 -2 -1 1.46 0.89 10 1 1 71.31 2.9 10 1 1 75.09 3.02 -10 -1 -1 70.36 3.59 -10 -1 -1 69.89 2.87 -10 -1 -1 78.65 2.59 10 0 1 0.54 0.87 10 0 1 1.15 0.91 10 0 1 0.49 0.87 -10 0 -1 0.99 0.63 -10 0 -1 0.2 1.03 -10 0 -1 -0.35 0.67 -10 0 -1 1.17 0.3 10 -1 1 69.11 2.97 10 -1 1 75.61 3.22 10 -1 1 69.54 3.23 -10 1 -1 73.38 2.33 -10 1 -1 78.42 2.5 -10 1 -1 72.71 3.46 -10 1 -1 73.72 2.96 10 -2 1 5.22 1.21 10 -2 1 3.26 1.22 10 -2 1 2.01 1.02 -10 2 -1 1.88 1.07 -10 2 -1 0.86 0.76 10 -3 1 12.31 1.7 10 -3 1 17.56 2.13 -10 3 -1 10.58 1.35 10 -4 1 0.49 1.23 10 -5 1 22.8 2.61 10 -5 1 23.62 1.44 9 5 1 15.57 1.09 9 5 1 16.97 1.15 -9 -5 -1 15.61 2.05 9 4 1 0.34 0.57 9 4 1 0.2 0.59 -9 -4 -1 1.3 1.05 -9 -4 -1 0 0.46 9 3 1 4.04 0.83 9 3 1 4.89 0.84 -9 -3 -1 3.52 0.81 -9 -3 -1 4.08 1.06 9 2 1 4.94 0.89 9 2 1 6.44 1.04 9 2 1 4.39 0.87 -9 -2 -1 5.74 0.65 -9 -2 -1 6.48 1.16 9 1 1 11.44 1.23 9 1 1 10.55 1.31 9 1 1 12.76 1.29 9 1 1 11.33 1.29 -9 -1 -1 9.97 1.58 -9 -1 -1 12.21 1.32 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