#------------------------------------------------------------------------------ #$Date: 2014-03-19 12:12:50 +0000 (Wed, 19 Mar 2014) $ #$Revision: 107486 $ #$URL: svn://www.crystallography.net/cod/cif/7/11/21/7112176.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_7112176 loop_ _publ_author_name 'Xin-Xing Wu' 'Ping-Xin Zhou' 'Li-Jing Wang' 'Peng-Fei Xu' 'Yong-Min Liang' _publ_section_title ; Synthesis of polycyclic substituted vinylarenes via a one-pot intramolecular aryl alkylation-N-tosylhydrazone insertion reaction ; _journal_name_full Chem.Commun. _journal_page_first 3882 _journal_paper_doi 10.1039/C4CC00809J _journal_volume 50 _journal_year 2014 _chemical_formula_moiety 'C24 H23 N O2 S' _chemical_formula_sum 'C24 H23 N O2 S' _chemical_formula_weight 389.49 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _audit_creation_date 2013-11-27 _audit_creation_method ; Olex2 1.2 (compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4715) ; _cell_angle_alpha 90 _cell_angle_beta 96.402(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.9663(6) _cell_length_b 8.2591(4) _cell_length_c 20.6407(10) _cell_measurement_reflns_used 1893 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 23.2460 _cell_measurement_theta_min 3.4900 _cell_volume 2027.22(17) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution ; Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008; Palatinus et al., 2012) ; _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 16.0733 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0475906000 _diffrn_orient_matrix_UB_12 -0.0281559000 _diffrn_orient_matrix_UB_13 0.0204580000 _diffrn_orient_matrix_UB_21 -0.0344668000 _diffrn_orient_matrix_UB_22 -0.0154972000 _diffrn_orient_matrix_UB_23 0.0250978000 _diffrn_orient_matrix_UB_31 -0.0101006000 _diffrn_orient_matrix_UB_32 -0.0796846000 _diffrn_orient_matrix_UB_33 -0.0121374000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_unetI/netI 0.0624 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 8380 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 26.022 _diffrn_reflns_theta_min 3.003 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.179 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.54313 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_density_diffrn 1.276 _exptl_crystal_description block _exptl_crystal_F_000 824 _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _refine_diff_density_max 0.187 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.042 _refine_ls_extinction_coef 0.0050(8) _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 1.061 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 264 _refine_ls_number_reflns 3987 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0552 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.1923P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1182 _refine_ls_wR_factor_ref 0.1445 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2557 _reflns_number_total 3987 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file c4cc00809j2.cif _[local]_cod_data_source_block wuxy1126 _cod_original_cell_volume 2027.24(17) _cod_database_code 7112176 _shelxl_version_number 2013-2 _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. ; _diffrn_reflns_laue_measured_fraction_full 0.998 _diffrn_reflns_laue_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _reflns_odcompleteness_completeness 99.78 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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 Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B) 2.b Aromatic/amide H refined with riding coordinates: C6(H6), C7(H7), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23) 2.c Idealised Me refined as rotating group: C9(H9A,H9B,H9C), C24(H24A,H24B,H24C) ; _shelx_res_file ; TITL CF solution in P21/c CELL 0.71073 11.966339 8.259137 20.640746 90 96.4022 90 ZERR 4 0.00062 0.000382 0.000967 0 0.0047 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S UNIT 96 92 4 8 4 L.S. 10 PLAN 25 BOND $H HTAB MORE -1 fmap 2 acta 52 CONF SHEL 999 0.81 REM D:/olex2_wuxy1126/wuxy1126.hkl WGHT 0.046000 0.192300 EXTI 0.005028 FVAR 4.50318 S1 5 0.354613 0.267564 0.537756 11.00000 0.06329 0.05481 = 0.04515 -0.00751 0.01280 -0.00573 O1 4 0.435232 0.314272 0.495286 11.00000 0.07840 0.07900 = 0.05439 -0.00769 0.03098 -0.00867 O2 4 0.290112 0.123903 0.525347 11.00000 0.08392 0.05255 = 0.05960 -0.01368 0.00533 -0.01354 N1 3 0.424243 0.246846 0.610476 11.00000 0.05023 0.05447 = 0.04907 -0.00255 0.00984 -0.00356 C1 1 0.497021 0.384444 0.636600 11.00000 0.05227 0.06944 = 0.06058 0.00076 0.00834 -0.01097 AFIX 23 H1A 2 0.501069 0.466908 0.603482 11.00000 -1.20000 H1B 2 0.572542 0.346887 0.650943 11.00000 -1.20000 AFIX 0 C2 1 0.441281 0.451470 0.693929 11.00000 0.05873 0.05874 = 0.05139 -0.00611 0.00315 -0.01483 AFIX 23 H2A 2 0.496778 0.485351 0.729177 11.00000 -1.20000 H2B 2 0.392345 0.542027 0.680734 11.00000 -1.20000 AFIX 0 C3 1 0.374947 0.307079 0.713365 11.00000 0.04418 0.04465 = 0.04667 0.00083 0.00451 -0.00369 C4 1 0.326690 0.280604 0.770446 11.00000 0.04255 0.04763 = 0.04568 0.00225 0.00108 -0.00067 C5 1 0.269406 0.133546 0.777459 11.00000 0.04486 0.05497 = 0.05361 0.00441 0.00344 -0.00223 C6 1 0.262006 0.022730 0.727036 11.00000 0.05780 0.05151 = 0.06015 0.00466 0.00615 -0.00965 AFIX 43 H6 2 0.223871 -0.073909 0.731787 11.00000 -1.20000 AFIX 0 C7 1 0.309231 0.049895 0.669557 11.00000 0.05869 0.04617 = 0.05953 -0.00564 0.00089 0.00007 AFIX 43 H7 2 0.303231 -0.025974 0.636055 11.00000 -1.20000 AFIX 0 C8 1 0.365345 0.194024 0.664282 11.00000 0.04429 0.04967 = 0.04615 0.00077 0.00426 0.00181 C9 1 0.219642 0.096805 0.839801 11.00000 0.06276 0.07637 = 0.06695 0.00960 0.01643 -0.01025 AFIX 137 H9A 2 0.278484 0.093647 0.875421 11.00000 -1.50000 H9B 2 0.182298 -0.006188 0.836010 11.00000 -1.50000 H9C 2 0.166458 0.179565 0.847663 11.00000 -1.50000 AFIX 0 C10 1 0.329911 0.406604 0.822712 11.00000 0.05169 0.05610 = 0.04201 0.00313 0.00555 -0.01014 C11 1 0.417274 0.416939 0.867527 11.00000 0.05909 0.07468 = 0.05993 0.00165 -0.00001 -0.00988 C12 1 0.163401 0.544493 0.763333 11.00000 0.06482 0.08106 = 0.04665 -0.00718 0.00100 0.00501 AFIX 43 H12 2 0.182524 0.499998 0.724673 11.00000 -1.20000 AFIX 0 C13 1 0.230411 0.513314 0.821353 11.00000 0.05700 0.04662 = 0.04442 -0.00314 0.00625 -0.00791 C14 1 0.069005 0.640401 0.762244 11.00000 0.06739 0.08874 = 0.06586 -0.00593 -0.00903 0.00959 AFIX 43 H14 2 0.026109 0.661737 0.722777 11.00000 -1.20000 AFIX 0 C15 1 0.037725 0.704537 0.818561 11.00000 0.06904 0.06374 = 0.07824 -0.00602 0.01237 0.00643 AFIX 43 H15 2 -0.027116 0.766941 0.817697 11.00000 -1.20000 AFIX 0 C16 1 0.102636 0.676017 0.876030 11.00000 0.09124 0.06890 = 0.06144 -0.00983 0.01638 0.01049 AFIX 43 H16 2 0.082783 0.721053 0.914427 11.00000 -1.20000 AFIX 0 C17 1 0.197480 0.580830 0.877509 11.00000 0.07709 0.06879 = 0.04706 -0.00201 0.00664 0.00485 AFIX 43 H17 2 0.240305 0.561572 0.917182 11.00000 -1.20000 AFIX 0 C18 1 0.261767 0.429816 0.543858 11.00000 0.05612 0.04619 = 0.03959 0.00074 0.00401 -0.00916 C19 1 0.295390 0.586271 0.530167 11.00000 0.06354 0.06042 = 0.04613 0.00171 0.01156 -0.01233 AFIX 43 H19 2 0.364271 0.604628 0.514588 11.00000 -1.20000 AFIX 0 C20 1 0.224571 0.713866 0.540139 11.00000 0.08225 0.04588 = 0.05051 0.00757 0.00605 -0.00744 AFIX 43 H20 2 0.247033 0.818667 0.531389 11.00000 -1.20000 AFIX 0 C21 1 0.121360 0.690253 0.562732 11.00000 0.06746 0.06245 = 0.04749 0.00411 0.00260 0.00637 C22 1 0.089500 0.533109 0.574853 11.00000 0.05780 0.06585 = 0.06956 0.00962 0.01293 -0.00165 AFIX 43 H22 2 0.019851 0.514369 0.589422 11.00000 -1.20000 AFIX 0 C23 1 0.158651 0.404083 0.565813 11.00000 0.05942 0.05029 = 0.05928 0.00471 0.00906 -0.00948 AFIX 43 H23 2 0.135826 0.299431 0.574517 11.00000 -1.20000 AFIX 0 C24 1 0.046085 0.831745 0.572667 11.00000 0.09777 0.07265 = 0.08391 0.00906 0.01159 0.02569 AFIX 137 H24A 2 0.044018 0.849279 0.618496 11.00000 -1.50000 H24B 2 -0.028474 0.809447 0.552408 11.00000 -1.50000 H24C 2 0.074646 0.926858 0.553442 11.00000 -1.50000 AFIX 0 H11A 2 0.478919 0.345953 0.865154 11.00000 0.08691 H11B 2 0.422001 0.501466 0.901514 11.00000 0.06422 HKLF 4 REM CF solution in P21/c REM R1 = 0.0552 for 2557 Fo > 4sig(Fo) and 0.0890 for all 3987 data REM 264 parameters refined using 0 restraints END WGHT 0.0452 0.2011 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y+1, -z+1 HTAB C19 O1_$1 REM Highest difference peak 0.187, deepest hole -0.307, 1-sigma level 0.042 Q1 1 0.3709 0.2735 0.7483 11.00000 0.05 0.19 Q2 1 0.3339 0.3364 0.7967 11.00000 0.05 0.18 Q3 1 0.4038 0.2593 0.7036 11.00000 0.05 0.17 Q4 1 0.3905 0.2153 0.6316 11.00000 0.05 0.15 Q5 1 0.0877 0.6256 0.5341 11.00000 0.05 0.15 Q6 1 0.3136 0.3638 0.5727 11.00000 0.05 0.15 Q7 1 0.1382 0.7456 0.7654 11.00000 0.05 0.14 Q8 1 0.5550 0.2910 0.6482 11.00000 0.05 0.14 Q9 1 0.2457 0.1048 0.5461 11.00000 0.05 0.14 Q10 1 0.3905 0.2882 0.4914 11.00000 0.05 0.14 Q11 1 0.0311 0.8704 0.5140 11.00000 0.05 0.14 Q12 1 0.1439 0.7973 0.9136 11.00000 0.05 0.14 Q13 1 0.3957 0.3681 0.7052 11.00000 0.05 0.14 Q14 1 0.1834 0.1109 0.5741 11.00000 0.05 0.13 Q15 1 0.3880 0.1548 0.5823 11.00000 0.05 0.13 Q16 1 0.2868 0.3368 0.5805 11.00000 0.05 0.13 Q17 1 0.3205 0.1248 0.5410 11.00000 0.05 0.13 Q18 1 0.3425 0.1926 0.7938 11.00000 0.05 0.13 Q19 1 0.1632 0.6433 0.6193 11.00000 0.05 0.13 Q20 1 0.4637 0.2794 0.5268 11.00000 0.05 0.13 Q21 1 0.3134 0.0511 0.5607 11.00000 0.05 0.13 Q22 1 0.0628 0.7003 0.7883 11.00000 0.05 0.13 Q23 1 0.4346 0.1580 0.4912 11.00000 0.05 0.13 Q24 1 0.2631 0.4852 0.5237 11.00000 0.05 0.13 Q25 1 0.4654 0.4392 0.4954 11.00000 0.05 0.13 ; _shelx_res_checksum 13949 _shelx_hkl_file ; 0 0 -3 8.72945 11.8423 2 0 0 -4 46201.3 1085.05 2 0 0 -5-9.39428 28.2541 2 0 0 -6 13687.9 581.814 2 0 0 6 12407.3 585.046 2 0 0 7 9.62691 25.7797 2 0 0 -7 7.66741 43.1763 2 0 0 8 4030.47 360.895 2 0 0 -8 4426.94 366.250 2 0 0 -9 34.2758 41.3333 2 0 0 -10 49895.1 1578.82 2 0 0 -11 43.1345 59.5091 2 0 0 -12 17782.2 957.920 2 0 0 -13 248.369 121.373 2 0 0 -14 20559.2 1115.23 2 0 0 -15 168.295 95.8672 2 0 0 15 157.990 169.963 3 0 0 16 828.839 270.662 3 0 0 17 158.254 185.833 3 0 0 18 1665.25 463.503 3 0 0 19 461.504 321.120 3 0 0 20 12421.7 1374.11 3 0 0 21 218.676 214.394 3 0 0 22 1948.72 607.918 3 0 0 23-0.47046 91.5681 3 0 0 -24 2549.89 698.446 4 0 0 24 1038.84 430.941 3 0 0 -25 707.753 387.697 4 0 0 25 140.825 118.521 3 0 0 26 1914.42 645.194 3 0 0 27 263.554 282.677 3 0 -1 -2 112822. 2286.38 4 0 -1 -3 147822. 2981.37 4 0 -1 -3 147920. 2918.12 2 0 -1 -4 3033.19 278.459 2 0 -1 -4 2826.14 296.622 4 0 -1 -5 60.4307 23.4268 2 0 -1 -5 197.104 102.248 4 0 -1 -6 68.4280 32.9142 2 0 1 -6 71.5981 27.7906 2 0 -1 -6-2.23115 67.6264 4 0 -1 6 123.363 38.2573 2 0 -1 7 19210.8 621.829 2 0 -1 -7 19244.2 1018.49 4 0 1 -7 19384.8 607.680 2 0 -1 -7 19001.4 890.736 2 0 -1 8 15938.1 607.768 2 0 -1 -8 16365.4 854.814 2 0 -1 -8 14512.2 938.222 4 0 1 -8 15873.1 608.560 2 0 -1 -9 7901.39 606.257 2 0 -1 9 7434.77 441.852 2 0 -1 -9 8143.91 729.973 4 0 1 -9 8635.51 461.082 2 0 -1 10 16551.2 735.080 2 0 1 -10 17345.6 751.705 2 0 1 -11 698.335 149.163 2 0 -1 11 457.855 118.845 2 0 -1 -11 587.677 178.459 2 0 -1 -12 18651.2 1059.00 2 0 1 -12 18840.7 863.357 2 0 1 -13 18.9616 33.5504 2 0 -1 -13 19.6734 57.3626 2 0 -1 -14 2729.40 439.094 2 0 -1 15 8157.42 957.604 3 0 -1 -15 6727.66 701.051 2 0 1 15 8777.87 915.962 3 0 -1 -15 7442.85 893.951 4 0 1 16 6175.72 801.787 3 0 -1 16 5201.67 791.117 3 0 -1 -16 5129.49 754.667 4 0 -1 -16 3616.03 537.872 2 0 -1 -17 10626.9 1146.72 4 0 1 17 13672.3 1253.25 3 0 -1 17 14406.2 1370.46 3 0 -1 18 4402.20 777.497 3 0 -1 -18 4145.72 737.124 4 0 1 18 4023.59 700.262 3 0 -1 19 4907.14 881.818 3 0 1 19 5141.05 829.249 3 0 -1 -19 4315.19 769.120 4 0 -1 20 1729.69 527.795 3 0 1 20 1915.93 523.784 3 0 -1 -20 1522.26 467.441 4 0 -1 -21 451.436 323.499 4 0 -1 21 109.156 179.781 3 0 1 21 5.02590 130.316 3 0 -1 -22 2162.06 561.122 4 0 1 22 2442.07 629.167 3 0 -1 22 1810.91 568.642 3 0 1 23-12.9985 165.942 3 0 -1 -23 4.31818 87.7556 4 0 -1 24 956.448 427.080 3 0 1 24 1364.31 508.754 3 0 -1 -24 1973.79 576.041 4 0 1 25 120.714 146.124 3 0 -1 25 212.475 252.426 3 0 -1 -25 533.353 311.171 4 0 1 26-104.087 213.358 3 0 -1 26 18.0520 253.589 3 0 1 27 322.956 269.846 3 0 -2 0 23704.7 830.037 2 0 -2 0 21610.3 668.693 3 0 2 -1 30536.7 924.735 2 0 2 1 32049.5 1162.84 1 0 -2 1 30784.5 925.856 2 0 -2 1 30502.7 932.123 3 0 -2 -1 31189.6 1048.77 2 0 2 2 128108. 2936.64 1 0 2 -2 131135. 2525.57 2 0 -2 -2 135496. 2895.35 2 0 -2 -3 9765.28 593.227 2 0 2 -3 9524.32 383.114 2 0 -2 -4 24344.1 1027.64 2 0 -2 -4 23042.9 1014.14 4 0 -2 -5 3699.38 400.286 4 0 -2 -5 3346.24 372.713 2 0 -2 -6 20.9752 57.7432 4 0 -2 -6 22.0470 71.1370 2 0 -2 -7 151.325 56.9462 2 0 -2 -7 163.667 100.206 4 0 -2 -8 2697.32 395.657 4 0 -2 -8 3119.32 400.919 2 0 -2 -9 25806.4 1369.60 4 0 -2 -9 24632.6 1242.74 2 0 -2 -10 704.157 232.835 4 0 -2 -10 780.107 218.167 2 0 -2 -11 501.655 223.031 4 0 -2 -11 572.294 173.463 2 0 -2 -12 17595.2 1140.70 2 0 -2 -12 18531.8 1312.86 4 0 -2 -13 23868.8 1519.07 4 0 2 13 21757.7 1285.25 3 0 -2 -13 21555.3 1290.18 2 0 2 14 1879.35 378.924 3 0 -2 -14 2086.90 410.261 2 0 -2 14 2494.00 514.242 3 0 -2 -14 1318.14 360.092 4 0 -2 -15 853.999 278.369 2 0 2 15 1018.10 297.340 3 0 -2 -15 448.638 232.185 4 0 -2 -16 4676.36 658.420 2 0 -2 16 6200.76 892.536 3 0 -2 -16 5170.23 773.366 4 0 2 16 4959.79 708.098 3 0 -2 -17 388.039 229.837 4 0 -2 17 61.3769 233.867 3 0 2 17 600.138 226.678 3 0 2 18 329.360 169.276 3 0 -2 -18 288.225 156.148 4 0 -2 19 4497.96 835.478 3 0 -2 -19 4183.78 739.429 4 0 2 19 3630.82 669.180 3 0 -2 -20 986.261 404.893 4 0 2 20 1277.14 397.831 3 0 -2 20 876.800 373.557 3 0 2 21 408.174 263.454 3 0 -2 -21 537.911 264.434 4 0 -2 21 461.875 283.690 3 0 -2 -22 132.038 136.103 4 0 2 22-32.2084 148.880 3 0 -2 22 48.9273 115.674 3 0 -2 -23 1156.57 456.821 4 0 -2 23 848.178 429.925 3 0 2 23 775.047 355.534 3 0 -2 -24 725.916 327.968 4 0 -2 24 693.073 375.744 3 0 -2 25 407.282 335.351 3 0 -2 -25 109.203 211.977 4 0 -3 0 7.62283 33.5801 2 0 -3 0 2.99216 33.0311 3 0 3 -1 2131.73 267.170 2 0 -3 -1 2262.99 299.177 2 0 -3 1 2448.66 267.974 3 0 -3 -1 2280.23 197.004 3 0 3 -2 12413.3 634.211 2 0 -3 2 12919.2 692.277 3 0 -3 -2 13340.7 781.393 2 0 -3 -3 3703.45 411.123 2 0 -3 3 3985.29 402.760 3 0 3 -3 3171.26 288.743 2 0 3 -4 1009.98 144.198 2 0 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129.605 2 -12 -5 -8 320.171 221.728 3 -12 -6 10-83.4423 123.110 3 -12 -6 10 130.226 142.811 1 -12 -6 9 258.593 198.938 1 -12 -6 9 101.147 168.463 3 -12 -6 8 78.4926 80.6212 1 -12 -6 8 73.3153 124.482 3 -12 -6 7-40.9582 62.1806 3 -12 -6 7 73.6882 112.721 1 -12 -6 6 161.435 197.698 3 -12 -6 6 145.992 160.578 1 -12 -6 5 77.6889 101.802 1 -12 -6 5 268.937 168.850 2 -12 -6 5 104.885 115.962 3 -12 -6 4 80.1795 60.5115 2 -12 -6 4 41.7107 100.449 3 -12 -6 3 254.388 177.090 2 -12 -6 3 231.980 185.540 3 -12 -6 2 27.7593 49.6081 2 -12 -6 2 121.231 124.612 3 -12 -6 1 635.501 265.587 2 -12 -6 1 696.126 342.425 3 -12 -6 0 363.502 222.486 2 -12 -6 0 597.961 307.753 3 -12 -6 -1 70.4589 81.5694 2 -12 -6 -1 128.680 124.569 3 -12 -6 -2 247.290 176.467 2 -12 -6 -2-201.296 178.490 3 -12 -6 -3 271.143 170.146 2 -12 -6 -3 228.506 176.902 3 -12 -6 -4 651.328 280.735 2 -12 -7 7 348.465 266.718 3 -12 -7 6-120.996 145.202 1 -12 -7 6 67.6831 102.318 3 -12 -7 5-87.2887 123.616 3 -12 -7 5-0.40465 86.7374 1 -12 -7 4-76.6398 114.431 1 -12 -7 4 202.948 178.522 3 -12 -7 3-411.232 253.081 3 -12 -7 3-63.3078 101.766 1 -12 -7 2 17.2719 56.5500 2 -12 -7 2-134.652 147.891 3 -12 -7 1-32.4914 77.4426 2 -12 -7 0-77.3189 103.151 2 -12 -7 -1 231.213 199.766 2 -13 0 16 280.175 253.208 3 -13 0 15-168.540 164.439 3 -13 0 14 174.480 191.289 3 -13 0 13 13.3619 82.2601 3 -13 0 12 811.837 337.757 3 -13 0 11-14.1631 75.1290 3 -13 0 10 538.723 278.615 3 -13 0 9 42.8156 90.2694 3 -13 0 8 1935.31 516.759 3 -13 0 7 157.553 213.330 3 -13 0 6 1256.36 421.241 3 -13 0 5-172.533 175.836 3 -13 0 4 693.273 316.738 3 -13 0 3-141.919 194.386 3 -13 0 2 3211.65 672.588 3 -13 0 1-2.62958 137.868 3 -13 0 0 1341.66 442.910 3 -13 0 -1-173.706 182.425 3 -13 0 -2-114.752 162.271 3 -13 0 -3-43.9758 109.939 3 -13 0 -4-23.1418 115.256 3 -13 0 -5 50.2671 86.9963 3 -13 0 -6 1556.07 499.147 3 -13 0 -7 45.1030 93.0089 2 -13 0 -7 42.3835 96.9809 3 -13 0 -8 292.644 208.157 2 -13 0 -9 22.9896 98.9357 2 -13 0 -10 89.7840 96.5227 2 -13 0 -11-307.106 219.126 2 -13 1 17 11.1390 69.7148 3 -13 1 16 356.629 211.735 3 -13 1 15 82.2523 161.720 3 -13 -1 15 195.565 141.230 3 -13 1 14-149.686 154.182 3 -13 -1 14 353.689 248.073 3 -13 1 13 82.6814 147.231 3 -13 -1 13 46.8381 116.111 3 -13 1 12 1029.18 392.301 3 -13 -1 12 814.964 346.672 3 -13 1 11 336.899 245.978 3 -13 -1 11 950.692 366.853 3 -13 1 10 568.089 330.394 3 -13 -1 10 374.625 227.549 3 -13 1 9 472.000 276.111 3 -13 -1 9 63.6425 184.559 3 -13 1 8 1903.76 504.534 3 -13 -1 8 1815.60 500.799 3 -13 1 7-134.369 159.257 3 -13 -1 7 289.563 244.863 3 -13 1 6 503.987 248.329 3 -13 -1 6 787.197 326.602 3 -13 1 5 746.129 328.494 3 -13 -1 5 539.912 237.269 3 -13 1 4 286.304 195.567 3 -13 -1 4 805.493 349.668 3 -13 1 3 729.806 323.996 3 -13 -1 3 219.437 165.987 3 -13 1 2-204.009 186.746 3 -13 -1 2 106.017 153.297 3 -13 1 1 402.048 268.934 3 -13 -1 1 199.385 95.2983 3 -13 1 0 163.744 113.326 3 -13 -1 0 36.4444 84.5426 3 -13 1 -1-198.305 192.831 3 -13 -1 -1 48.0735 129.822 3 -13 1 -2 1046.90 413.993 3 -13 -1 -2 1060.32 387.949 3 -13 1 -3 428.506 279.777 3 -13 -1 -3 117.178 134.585 3 -13 1 -4 357.640 246.490 3 -13 -1 -4 568.822 278.818 3 -13 1 -5 187.320 121.820 3 -13 -1 -5 362.899 196.708 3 -13 -1 -5 210.203 165.140 2 -13 -1 -6 433.473 271.376 3 -13 -1 -6 213.828 187.031 2 -13 1 -6 276.538 209.749 3 -13 -1 -7 220.948 165.546 3 -13 -1 -7 78.6909 265.947 2 -13 -1 -8 522.723 287.819 2 -13 -1 -8 337.561 254.701 3 -13 -1 -9-76.0859 102.751 2 -13 1 -9-196.517 197.292 2 -13 -1 -10 314.879 216.366 2 -13 1 -10 334.582 245.296 2 -13 1 -11-350.091 238.475 2 -13 1 -12 250.248 202.159 2 -13 2 17 149.288 191.882 3 -13 2 16 557.602 299.933 3 -13 2 15 300.820 214.273 3 -13 2 14 1100.43 432.476 3 -13 -2 14 381.377 299.933 3 -13 2 13 1.93325 76.1876 3 -13 -2 13-279.390 212.506 3 -13 2 12 71.5695 111.335 3 -13 -2 12 22.1621 106.965 3 -13 2 11 348.745 232.013 3 -13 -2 11 242.007 200.706 3 -13 2 10 47.3498 62.0993 3 -13 -2 10-7.95634 84.7429 3 -13 2 9 190.335 128.975 3 -13 -2 9 710.987 276.100 3 -13 2 8 376.357 252.542 3 -13 -2 8 113.524 95.7683 3 -13 2 7 769.600 342.163 3 -13 -2 7 580.083 284.077 3 -13 2 6 1950.10 526.598 3 -13 -2 6 1710.26 492.315 3 -13 2 5 1129.39 384.725 3 -13 -2 5 970.735 376.033 3 -13 2 4 190.523 210.137 3 -13 -2 4 231.992 225.610 3 -13 2 3 1226.32 437.652 3 -13 -2 3 1442.74 455.378 3 -13 2 2 2260.44 572.988 3 -13 -2 2 2427.97 592.710 3 -13 2 1 36.0853 77.2585 3 -13 -2 1 469.863 282.979 3 -13 2 0 931.114 342.394 3 -13 -2 0 2278.42 569.949 3 -13 2 -1-213.950 202.449 3 -13 -2 -1-4.73356 147.243 3 -13 2 -2-30.0054 106.108 3 -13 -2 -2 245.232 204.041 3 -13 -2 -2 121.508 208.461 2 -13 2 -3 682.822 327.555 3 -13 -2 -3 448.583 253.988 3 -13 -2 -3-76.5298 137.835 2 -13 2 -4 372.197 291.596 3 -13 -2 -4 619.264 312.493 3 -13 -2 -4 258.781 186.882 2 -13 -2 -5 353.716 245.302 3 -13 -2 -5 152.189 163.098 2 -13 -2 -6-58.6379 127.849 3 -13 -2 -6-28.9467 98.3199 2 -13 -2 -7 88.5890 149.107 3 -13 -2 -7 41.1764 96.0471 2 -13 -2 -8 243.562 110.134 3 -13 -2 -8 333.488 230.007 2 -13 -2 -9 714.456 317.353 2 -13 -2 -9 1108.70 431.007 3 -13 2 -11 31.8108 70.9573 2 -13 2 -12 205.036 133.198 2 -13 3 14 390.356 245.068 3 -13 3 13-116.662 139.407 3 -13 -3 13 114.837 239.199 3 -13 3 12 977.120 372.756 3 -13 -3 12 601.478 321.429 3 -13 3 11 392.417 264.894 3 -13 -3 11 721.932 343.876 3 -13 3 10 512.701 274.887 3 -13 -3 10 459.270 270.418 3 -13 3 9 99.3159 116.988 3 -13 -3 9 243.631 158.757 3 -13 3 8-26.3888 129.098 3 -13 -3 8 200.989 188.528 3 -13 3 7 165.411 161.070 3 -13 -3 7-57.8989 126.249 3 -13 3 6-1.46492 117.211 3 -13 -3 6 514.050 309.485 3 -13 3 5 242.499 238.743 3 -13 -3 5 144.808 153.640 3 -13 3 4 100.824 146.023 3 -13 -3 4-82.0480 124.472 3 -13 3 3 837.695 326.118 3 -13 -3 3 342.179 198.573 3 -13 -3 3 319.467 172.446 2 -13 3 2 39.2275 117.583 3 -13 -3 2 364.180 294.516 3 -13 -3 2 59.4371 103.866 2 -13 3 1 1.13193 82.4217 3 -13 -3 1-63.1563 177.467 3 -13 -3 1-13.3447 59.7451 2 -13 3 0 530.324 285.333 3 -13 -3 0 828.466 349.522 3 -13 -3 0 1079.71 361.460 2 -13 3 -1 305.863 199.383 3 -13 -3 -1 523.953 320.322 3 -13 -3 -1 536.761 271.790 2 -13 3 -2 508.189 219.146 3 -13 -3 -2 1269.35 447.630 3 -13 -3 -2 1303.94 390.703 2 -13 -3 -3 198.993 176.556 3 -13 -3 -3-277.686 215.543 2 -13 3 -3 94.8690 226.635 3 -13 -3 -4-89.2713 66.1876 3 -13 -3 -4 182.440 192.187 2 -13 -3 -5 295.452 208.815 3 -13 -3 -5 725.698 319.766 2 -13 -3 -6 464.494 280.965 3 -13 -3 -6 490.619 262.823 2 -13 -3 -7-144.800 102.460 3 -13 -3 -7 18.2640 74.7501 2 -13 -3 -8-144.609 187.640 3 -13 -3 -8 78.5112 166.770 2 -13 -3 -9-59.6195 182.660 3 -13 3 -12-390.122 258.095 2 -13 -4 11 254.601 167.030 3 -13 4 10-146.327 153.355 3 -13 -4 10 22.9923 81.5409 3 -13 4 9 228.348 168.708 3 -13 -4 9 437.663 244.623 3 -13 -4 9 375.066 217.403 2 -13 4 8-117.294 170.932 3 -13 -4 8-141.786 156.254 3 -13 -4 8 6.76210 71.4596 2 -13 4 7-49.3360 92.8697 3 -13 -4 7-271.962 209.001 3 -13 -4 7-102.357 127.542 2 -13 4 6 58.9694 68.3040 3 -13 -4 6 193.321 214.596 3 -13 -4 6-188.063 153.396 2 -13 4 5-27.7498 77.9581 3 -13 -4 5 188.517 234.340 3 -13 -4 5-107.366 128.227 2 -13 4 4 55.1757 66.7398 3 -13 -4 4 15.1534 96.0662 2 -13 4 3 664.777 313.301 3 -13 -4 3 401.311 246.718 3 -13 -4 3 559.217 264.926 2 -13 4 2 597.309 299.055 3 -13 -4 2 670.437 347.075 3 -13 -4 2 1033.22 348.312 2 -13 4 1 552.989 300.976 3 -13 -4 1 410.924 249.419 3 -13 -4 1 350.375 218.360 2 -13 -4 0 206.888 214.609 3 -13 -4 0-100.928 116.688 2 -13 4 0 72.4547 49.1323 3 -13 -4 -1 157.915 148.864 3 -13 -4 -1 889.978 341.229 2 -13 -4 -2 11.5643 70.2383 3 -13 -4 -2 236.319 210.881 2 -13 -4 -3 540.492 305.010 3 -13 -4 -3 3811.90 746.727 2 -13 -4 -4-74.7557 157.362 3 -13 -4 -4 48.8379 138.903 2 -13 -4 -5 281.390 189.935 3 -13 -4 -5 279.677 198.542 2 -13 -4 -6 679.757 331.005 3 -13 -4 -6 495.684 261.814 2 -13 -4 -7 39.9528 99.4725 3 -13 -4 -8 216.608 197.651 3 -13 -4 -9 373.241 257.582 3 -13 -5 8 354.204 248.885 3 -13 -5 7 414.588 252.438 3 -13 -5 7 216.293 160.669 2 -13 -5 6 699.157 354.525 3 -13 -5 6 660.137 278.841 2 -13 5 5-118.011 144.847 3 -13 -5 5 125.111 131.476 3 -13 -5 5-108.684 173.560 2 -13 5 4-120.848 156.191 3 -13 -5 4 281.816 224.349 3 -13 -5 4 605.128 280.954 2 -13 -5 3 27.4045 100.415 3 -13 -5 3 87.9617 164.790 2 -13 5 3 137.004 188.159 3 -13 -5 2 53.6660 79.4187 3 -13 -5 2 102.648 56.2439 2 -13 -5 1 367.429 234.299 3 -13 -5 1 336.599 232.933 2 -13 -5 0 118.405 171.408 3 -13 -5 0 73.6226 86.4067 2 -13 -5 -1 99.1319 121.898 3 -13 -5 -1 220.512 168.643 2 -13 -5 -2 457.905 280.615 3 -13 -5 -2 400.407 232.062 2 -13 -5 -3 132.869 179.854 3 -13 -5 -3 28.7803 76.0241 2 -13 -5 -4 499.403 298.410 3 -13 -5 -5-445.196 273.006 3 -13 -5 -6 287.352 240.446 3 -13 -5 -7-10.9965 134.412 3 -13 -6 5-64.0353 110.265 3 -13 -6 4 139.257 131.156 2 -13 -6 4 288.834 253.965 3 -13 -6 3 97.1200 138.234 2 -13 -6 3 98.5045 144.414 3 -13 -6 2 86.9833 141.675 2 -13 -6 2 104.820 112.203 3 -13 -6 1 106.565 121.017 2 -13 -6 1-99.0000 133.357 3 -13 -6 0 47.9478 75.5901 2 -13 -6 0 205.477 205.137 3 -13 -6 -1-6.39878 126.818 3 -13 -6 -2 42.5661 83.0930 3 -14 0 13-279.316 216.139 3 -14 0 12 699.448 343.204 3 -14 0 11-23.4749 73.1145 3 -14 0 10 169.051 168.987 3 -14 0 9 6.14358 130.133 3 -14 0 8 53.2339 136.637 3 -14 0 7 215.781 208.347 3 -14 0 6 670.710 305.471 3 -14 0 5-413.053 262.233 3 -14 0 4 216.209 193.903 3 -14 0 3 301.782 227.229 3 -14 0 2 2951.54 701.509 3 -14 0 1 113.001 234.603 3 -14 0 0 1236.69 452.936 3 -14 0 -1-117.618 196.579 3 -14 0 -2-47.9370 101.951 3 -14 0 -3-119.036 205.479 3 -14 0 -4 309.890 239.661 3 -14 0 -5 223.779 247.305 3 -14 0 -6-21.8907 96.2112 3 -14 0 -7 367.749 246.814 2 -14 1 14 220.906 155.798 3 -14 1 13 74.8059 206.316 3 -14 1 12 416.628 270.408 3 -14 -1 12 203.765 192.872 3 -14 1 11-109.866 142.134 3 -14 -1 11 348.578 283.087 3 -14 1 10 67.2837 96.9286 3 -14 -1 10 325.880 232.065 3 -14 1 9 308.636 232.850 3 -14 -1 9 543.910 280.568 3 -14 1 8 313.923 237.592 3 -14 -1 8 262.197 189.509 3 -14 1 7 119.574 162.411 3 -14 -1 7-62.2579 139.052 3 -14 1 6 191.411 191.014 3 -14 -1 6 249.079 206.061 3 -14 1 5 1565.67 495.807 3 -14 -1 5 2044.05 567.719 3 -14 1 4 408.413 230.848 3 -14 -1 4-34.6619 119.455 3 -14 1 3 475.890 265.897 3 -14 -1 3 564.219 307.947 3 -14 1 2 1164.02 439.128 3 -14 -1 2 669.310 339.185 3 -14 1 1 721.091 375.852 3 -14 -1 1 616.926 337.693 3 -14 1 0-81.8605 135.555 3 -14 -1 0-196.925 273.349 3 -14 1 -1 309.408 250.778 3 -14 -1 -1-113.187 146.768 3 -14 1 -2 428.754 262.666 3 -14 -1 -2 271.045 190.350 3 -14 1 -3-301.084 238.589 3 -14 -1 -3 550.213 309.423 3 -14 1 -4-89.0230 137.836 3 -14 -1 -4-343.982 249.640 3 -14 1 -5 786.257 364.530 3 -14 -1 -5 110.492 121.148 3 -14 -1 -5 428.700 259.165 2 -14 -1 -6 89.0746 138.956 3 -14 -1 -6 253.285 162.362 2 -14 1 -6 212.893 188.116 3 -14 2 15 338.521 253.948 3 -14 2 14 302.873 225.175 3 -14 2 13 180.707 163.452 3 -14 2 12 1125.34 425.498 3 -14 2 11-38.1477 105.927 3 -14 2 10 347.008 247.131 3 -14 -2 10 302.949 244.944 3 -14 2 9 35.2680 137.352 3 -14 -2 9-9.07517 110.969 3 -14 2 8 175.930 114.789 3 -14 -2 8 272.229 228.372 3 -14 2 7-174.697 175.749 3 -14 -2 7 352.299 242.904 3 -14 2 6 439.785 279.990 3 -14 -2 6 451.162 248.852 3 -14 2 5 382.436 259.781 3 -14 -2 5-29.3982 108.162 3 -14 2 4 27.7977 79.9171 3 -14 -2 4 757.354 389.810 3 -14 2 3 269.195 227.129 3 -14 -2 3 460.069 283.661 3 -14 2 2 85.4564 149.610 3 -14 -2 2 740.972 343.996 3 -14 2 1 58.7505 167.433 3 -14 -2 1 298.131 222.972 3 -14 2 0 892.436 363.660 3 -14 -2 0 394.538 250.049 3 -14 2 -1-88.2847 146.880 3 -14 -2 -1 160.053 227.122 3 -14 -2 -1 195.566 206.108 2 -14 2 -2 811.845 345.539 3 -14 -2 -2 762.063 397.966 3 -14 -2 -2 808.059 363.355 2 -14 -2 -3-55.3965 110.527 3 -14 -2 -3 263.309 210.597 2 -14 -2 -4 1176.49 435.433 3 -14 -2 -4 649.992 303.074 2 -14 2 -4 866.943 382.062 3 -14 -2 -5-125.933 103.111 3 -14 -2 -5-80.0276 152.697 2 -14 -2 -6-177.873 188.006 3 -14 3 13 298.448 213.678 3 -14 3 12 89.4374 129.870 3 -14 3 11-227.599 194.840 3 -14 3 10 785.102 358.022 3 -14 3 9 8.66892 55.4042 3 -14 3 8 122.162 106.425 3 -14 -3 8-0.42083 91.6094 3 -14 3 7 10.9460 78.1767 3 -14 -3 7-167.052 131.555 3 -14 3 6 194.643 174.044 3 -14 -3 6 229.291 151.972 3 -14 3 5-253.663 202.744 3 -14 -3 5-86.2884 122.285 3 -14 3 4 122.027 111.010 3 -14 -3 4 12.9267 126.892 3 -14 -3 4 43.5293 157.960 2 -14 3 3 17.9502 98.7315 3 -14 -3 3-4.35291 91.0186 3 -14 -3 3-194.069 166.371 2 -14 3 2 411.050 250.692 3 -14 -3 2 644.023 316.231 3 -14 -3 2 904.977 358.233 2 -14 3 1 260.632 211.587 3 -14 -3 1-410.522 272.739 3 -14 -3 1-126.285 141.215 2 -14 3 0 141.291 216.058 3 -14 -3 0 204.886 122.494 3 -14 -3 0-63.9672 195.204 2 -14 3 -1 598.904 350.899 3 -14 -3 -1 320.172 185.512 3 -14 -3 -1 443.305 247.090 2 -14 -3 -2-36.2874 155.118 3 -14 -3 -2 334.866 235.829 2 -14 3 -2 38.2894 108.241 3 -14 -3 -3-97.2990 135.565 3 -14 -3 -3 135.409 107.554 2 -14 -3 -4 633.132 348.260 3 -14 -3 -5 292.022 264.968 3 -14 -3 -6 42.2717 79.7269 3 -14 4 9 172.454 168.742 3 -14 4 8 252.602 220.375 3 -14 -4 8-48.5806 93.2591 2 -14 4 7 164.781 153.065 3 -14 -4 7 390.539 221.484 2 -14 4 6-46.0327 93.6312 3 -14 -4 6 104.817 119.296 2 -14 4 5 59.5095 90.7026 3 -14 -4 5 216.698 194.149 3 -14 -4 5 5.12380 65.6815 2 -14 4 4-266.066 211.633 3 -14 -4 4 160.403 206.383 3 -14 -4 4-103.759 121.766 2 -14 4 3 71.3854 174.598 3 -14 -4 3-232.156 230.158 3 -14 -4 3 111.447 139.887 2 -14 4 2 97.3621 124.080 3 -14 -4 2 205.583 225.459 3 -14 -4 2 164.033 191.265 2 -14 4 1 356.633 239.124 3 -14 -4 1 98.6806 134.779 3 -14 -4 1 87.6472 143.124 2 -14 -4 0 91.3444 54.6577 2 -14 4 0 311.799 268.760 3 -14 -4 -1 117.730 143.814 3 -14 -4 -1 10.5515 70.4898 2 -14 -4 -2 1055.24 436.489 3 -14 -4 -3 373.458 286.020 3 -14 -4 -4-293.347 230.183 3 -14 -5 6-55.6362 89.6610 2 -14 -5 5-43.6910 72.4157 2 -14 5 4 81.7152 165.623 3 -14 -5 4 145.937 139.933 2 -14 -5 3 102.129 127.662 2 -14 5 3 263.499 237.072 3 -14 -5 2 380.775 226.523 2 -15 0 5 162.953 128.857 3 -15 0 4 2424.30 658.212 3 -15 0 3 95.2744 155.501 3 -15 0 2 352.149 283.824 3 -15 1 7-88.3370 179.068 3 -15 1 6 20.0939 162.313 3 -15 1 5 80.9104 142.664 3 -15 1 4 205.364 188.811 3 -15 1 3-12.0019 72.7708 3 -15 1 2 2855.83 702.986 3 -15 2 8 431.355 277.725 3 -15 2 7 255.156 229.731 3 -15 2 6 16.8252 55.6898 3 -15 2 5-6.63364 142.376 3 -15 2 4-124.212 153.948 3 -15 2 3 100.044 116.196 3 -15 3 8-6.67422 98.5754 3 -15 3 7-3.98254 69.6522 3 -15 3 6 78.9645 99.5063 3 -15 -3 6-264.861 199.128 2 -15 3 5-36.8795 91.4216 3 -15 -3 5-116.988 121.256 2 0 0 0 0.00 0.00 0 TITL wuxy1126 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 11.966339 8.259137 20.640746 90.0000 96.4022 90.0000 ZERR 9.00 0.000620 0.000382 0.000967 0.0000 0.0047 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 99.00 90.00 9.00 9.00 TREF HKLF 4 END ; _shelx_hkl_checksum 95006 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn S1 S 0.35461(6) 0.26756(8) 0.53776(3) 0.0539(2) Uani 1 1 d . O1 O 0.43523(17) 0.3143(2) 0.49529(9) 0.0688(6) Uani 1 1 d . O2 O 0.29011(17) 0.1239(2) 0.52535(9) 0.0656(6) Uani 1 1 d . N1 N 0.42424(18) 0.2468(2) 0.61048(10) 0.0509(6) Uani 1 1 d . C1 C 0.4970(2) 0.3844(3) 0.63660(14) 0.0606(7) Uani 1 1 d . H1A H 0.5011 0.4669 0.6035 0.073 Uiso 1 1 calc R H1B H 0.5725 0.3469 0.6509 0.073 Uiso 1 1 calc R C2 C 0.4413(2) 0.4515(3) 0.69393(13) 0.0565(7) Uani 1 1 d . H2A H 0.4968 0.4854 0.7292 0.068 Uiso 1 1 calc R H2B H 0.3923 0.5420 0.6807 0.068 Uiso 1 1 calc R C3 C 0.3749(2) 0.3071(3) 0.71337(12) 0.0452(6) Uani 1 1 d . C4 C 0.3267(2) 0.2806(3) 0.77045(12) 0.0456(6) Uani 1 1 d . C5 C 0.2694(2) 0.1335(3) 0.77746(13) 0.0513(7) Uani 1 1 d . C6 C 0.2620(2) 0.0227(3) 0.72704(14) 0.0565(7) Uani 1 1 d . H6 H 0.2239 -0.0739 0.7318 0.068 Uiso 1 1 calc R C7 C 0.3092(2) 0.0499(3) 0.66956(14) 0.0552(7) Uani 1 1 d . H7 H 0.3032 -0.0260 0.6361 0.066 Uiso 1 1 calc R C8 C 0.3653(2) 0.1940(3) 0.66428(12) 0.0468(6) Uani 1 1 d . C9 C 0.2196(2) 0.0968(4) 0.83980(14) 0.0680(8) Uani 1 1 d . H9A H 0.2785 0.0936 0.8754 0.102 Uiso 1 1 calc GR H9B H 0.1823 -0.0062 0.8360 0.102 Uiso 1 1 calc GR H9C H 0.1665 0.1796 0.8477 0.102 Uiso 1 1 calc GR C10 C 0.3299(2) 0.4066(3) 0.82271(12) 0.0499(6) Uani 1 1 d . C11 C 0.4173(3) 0.4169(5) 0.86753(16) 0.0651(8) Uani 1 1 d . C12 C 0.1634(2) 0.5445(4) 0.76333(14) 0.0646(8) Uani 1 1 d . H12 H 0.1825 0.5000 0.7247 0.077 Uiso 1 1 calc R C13 C 0.2304(2) 0.5133(3) 0.82135(12) 0.0493(6) Uani 1 1 d . C14 C 0.0690(3) 0.6404(4) 0.76224(16) 0.0752(9) Uani 1 1 d . H14 H 0.0261 0.6617 0.7228 0.090 Uiso 1 1 calc R C15 C 0.0377(3) 0.7045(4) 0.81856(17) 0.0700(9) Uani 1 1 d . H15 H -0.0271 0.7669 0.8177 0.084 Uiso 1 1 calc R C16 C 0.1026(3) 0.6760(4) 0.87603(16) 0.0733(9) Uani 1 1 d . H16 H 0.0828 0.7211 0.9144 0.088 Uiso 1 1 calc R C17 C 0.1975(3) 0.5808(3) 0.87751(14) 0.0643(8) Uani 1 1 d . H17 H 0.2403 0.5616 0.9172 0.077 Uiso 1 1 calc R C18 C 0.2618(2) 0.4298(3) 0.54386(12) 0.0474(6) Uani 1 1 d . C19 C 0.2954(2) 0.5863(3) 0.53017(12) 0.0563(7) Uani 1 1 d . H19 H 0.3643 0.6046 0.5146 0.068 Uiso 1 1 calc R C20 C 0.2246(3) 0.7139(3) 0.54014(13) 0.0597(7) Uani 1 1 d . H20 H 0.2470 0.8187 0.5314 0.072 Uiso 1 1 calc R C21 C 0.1214(3) 0.6903(3) 0.56273(13) 0.0594(7) Uani 1 1 d . C22 C 0.0895(3) 0.5331(3) 0.57485(15) 0.0640(8) Uani 1 1 d . H22 H 0.0199 0.5144 0.5894 0.077 Uiso 1 1 calc R C23 C 0.1587(2) 0.4041(3) 0.56581(13) 0.0561(7) Uani 1 1 d . H23 H 0.1358 0.2994 0.5745 0.067 Uiso 1 1 calc R C24 C 0.0461(3) 0.8317(4) 0.57267(17) 0.0847(10) Uani 1 1 d . H24A H 0.0440 0.8493 0.6185 0.127 Uiso 1 1 calc GR H24B H -0.0285 0.8094 0.5524 0.127 Uiso 1 1 calc GR H24C H 0.0746 0.9269 0.5534 0.127 Uiso 1 1 calc GR H11A H 0.479(3) 0.346(4) 0.8652(15) 0.087(11) Uiso 1 1 d . H11B H 0.422(2) 0.501(3) 0.9015(14) 0.064(9) 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 0.0633(5) 0.0548(5) 0.0452(4) -0.0075(3) 0.0128(3) -0.0057(3) O1 0.0784(14) 0.0790(14) 0.0544(12) -0.0077(11) 0.0310(10) -0.0087(11) O2 0.0839(14) 0.0525(11) 0.0596(12) -0.0137(10) 0.0053(10) -0.0135(10) N1 0.0502(13) 0.0545(13) 0.0491(13) -0.0025(11) 0.0098(10) -0.0036(10) C1 0.0523(17) 0.0694(18) 0.0606(18) 0.0008(16) 0.0083(14) -0.0110(14) C2 0.0587(17) 0.0587(17) 0.0514(16) -0.0061(14) 0.0031(13) -0.0148(13) C3 0.0442(14) 0.0447(14) 0.0467(14) 0.0008(13) 0.0045(11) -0.0037(11) C4 0.0426(14) 0.0476(15) 0.0457(14) 0.0023(13) 0.0011(11) -0.0007(11) C5 0.0449(15) 0.0550(16) 0.0536(16) 0.0044(14) 0.0034(12) -0.0022(12) C6 0.0578(17) 0.0515(16) 0.0602(18) 0.0047(15) 0.0061(14) -0.0096(13) C7 0.0587(17) 0.0462(15) 0.0595(18) -0.0056(14) 0.0009(14) 0.0001(13) C8 0.0443(14) 0.0497(15) 0.0461(14) 0.0008(13) 0.0043(11) 0.0018(12) C9 0.0628(19) 0.076(2) 0.0669(19) 0.0096(17) 0.0164(15) -0.0102(15) C10 0.0517(16) 0.0561(16) 0.0420(14) 0.0031(13) 0.0055(12) -0.0101(12) C11 0.059(2) 0.075(2) 0.060(2) 0.0016(18) 0.0000(16) -0.0099(17) C12 0.065(2) 0.081(2) 0.0466(16) -0.0072(16) 0.0010(14) 0.0050(16) C13 0.0570(17) 0.0466(15) 0.0444(15) -0.0031(13) 0.0063(12) -0.0079(12) C14 0.067(2) 0.089(2) 0.066(2) -0.0059(19) -0.0090(16) 0.0096(18) C15 0.069(2) 0.0637(19) 0.078(2) -0.0060(18) 0.0124(18) 0.0064(16) C16 0.091(2) 0.069(2) 0.061(2) -0.0098(17) 0.0164(18) 0.0105(18) C17 0.077(2) 0.0688(19) 0.0471(17) -0.0020(15) 0.0066(15) 0.0049(16) C18 0.0561(16) 0.0462(14) 0.0396(14) 0.0007(12) 0.0040(12) -0.0092(12) C19 0.0635(18) 0.0604(18) 0.0461(16) 0.0017(14) 0.0116(13) -0.0123(14) C20 0.082(2) 0.0459(16) 0.0505(16) 0.0076(14) 0.0061(15) -0.0074(15) C21 0.0675(19) 0.0625(18) 0.0475(16) 0.0041(15) 0.0026(14) 0.0064(15) C22 0.0578(18) 0.066(2) 0.070(2) 0.0096(17) 0.0129(15) -0.0016(14) C23 0.0594(18) 0.0503(16) 0.0593(18) 0.0047(14) 0.0091(14) -0.0095(13) C24 0.098(3) 0.073(2) 0.084(2) 0.0091(19) 0.012(2) 0.0257(19) 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 106.30(12) O1 S1 C18 108.33(12) O2 S1 O1 120.34(12) O2 S1 N1 106.70(11) O2 S1 C18 108.34(12) N1 S1 C18 105.95(11) C1 N1 S1 117.78(17) C8 N1 S1 119.46(16) C8 N1 C1 105.44(19) N1 C1 H1A 110.6 N1 C1 H1B 110.6 N1 C1 C2 105.5(2) H1A C1 H1B 108.8 C2 C1 H1A 110.6 C2 C1 H1B 110.6 C1 C2 H2A 111.4 C1 C2 H2B 111.4 H2A C2 H2B 109.2 C3 C2 C1 102.0(2) C3 C2 H2A 111.4 C3 C2 H2B 111.4 C4 C3 C2 129.1(2) C8 C3 C2 110.1(2) C8 C3 C4 120.8(2) C3 C4 C5 118.5(2) C3 C4 C10 121.6(2) C5 C4 C10 119.9(2) C4 C5 C9 120.2(2) C6 C5 C4 119.0(2) C6 C5 C9 120.8(2) C5 C6 H6 118.7 C5 C6 C7 122.6(2) C7 C6 H6 118.7 C6 C7 H7 121.4 C8 C7 C6 117.1(3) C8 C7 H7 121.4 C3 C8 N1 110.7(2) C3 C8 C7 122.1(2) C7 C8 N1 127.2(2) C5 C9 H9A 109.5 C5 C9 H9B 109.5 C5 C9 H9C 109.5 H9A C9 H9B 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 C11 C10 C4 120.3(3) C11 C10 C13 123.2(3) C13 C10 C4 116.4(2) C10 C11 H11A 119(2) C10 C11 H11B 121.5(16) H11A C11 H11B 119(2) C13 C12 H12 119.5 C14 C12 H12 119.5 C14 C12 C13 120.9(3) C12 C13 C10 120.9(2) C17 C13 C10 121.9(2) C17 C13 C12 117.2(3) C12 C14 H14 119.6 C15 C14 C12 120.7(3) C15 C14 H14 119.6 C14 C15 H15 120.4 C16 C15 C14 119.3(3) C16 C15 H15 120.4 C15 C16 H16 119.8 C15 C16 C17 120.4(3) C17 C16 H16 119.8 C13 C17 H17 119.3 C16 C17 C13 121.5(3) C16 C17 H17 119.3 C19 C18 S1 119.7(2) C23 C18 S1 120.2(2) C23 C18 C19 120.0(3) C18 C19 H19 120.6 C20 C19 C18 118.8(3) C20 C19 H19 120.6 C19 C20 H20 119.0 C21 C20 C19 121.9(3) C21 C20 H20 119.0 C20 C21 C22 117.9(3) C20 C21 C24 120.5(3) C22 C21 C24 121.5(3) C21 C22 H22 119.3 C23 C22 C21 121.4(3) C23 C22 H22 119.3 C18 C23 H23 120.0 C22 C23 C18 120.0(3) C22 C23 H23 120.0 C21 C24 H24A 109.5 C21 C24 H24B 109.5 C21 C24 H24C 109.5 H24A C24 H24B 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 O1 1.4271(18) S1 O2 1.4231(18) S1 N1 1.642(2) S1 C18 1.754(3) N1 C1 1.495(3) N1 C8 1.447(3) C1 H1A 0.9700 C1 H1B 0.9700 C1 C2 1.526(4) C2 H2A 0.9700 C2 H2B 0.9700 C2 C3 1.511(3) C3 C4 1.386(3) C3 C8 1.373(3) C4 C5 1.410(3) C4 C10 1.496(3) C5 C6 1.381(4) C5 C9 1.508(4) C6 H6 0.9300 C6 C7 1.388(4) C7 H7 0.9300 C7 C8 1.377(3) C9 H9A 0.9600 C9 H9B 0.9600 C9 H9C 0.9600 C10 C11 1.319(4) C10 C13 1.479(4) C11 H11A 0.95(3) C11 H11B 0.99(3) C12 H12 0.9300 C12 C13 1.389(4) C12 C14 1.378(4) C13 C17 1.383(4) C14 H14 0.9300 C14 C15 1.367(4) C15 H15 0.9300 C15 C16 1.364(4) C16 H16 0.9300 C16 C17 1.378(4) C17 H17 0.9300 C18 C19 1.392(3) C18 C23 1.378(3) C19 H19 0.9300 C19 C20 1.382(4) C20 H20 0.9300 C20 C21 1.382(4) C21 C22 1.383(4) C21 C24 1.503(4) C22 H22 0.9300 C22 C23 1.375(4) C23 H23 0.9300 C24 H24A 0.9600 C24 H24B 0.9600 C24 H24C 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 S1 N1 C1 C2 112.4(2) S1 N1 C8 C3 -121.2(2) S1 N1 C8 C7 60.9(3) S1 C18 C19 C20 -175.0(2) S1 C18 C23 C22 175.4(2) O1 S1 N1 C1 52.1(2) O1 S1 N1 C8 -177.84(18) O1 S1 C18 C19 -22.5(3) O1 S1 C18 C23 161.3(2) O2 S1 N1 C1 -178.29(18) O2 S1 N1 C8 -48.3(2) O2 S1 C18 C19 -154.6(2) O2 S1 C18 C23 29.2(3) N1 S1 C18 C19 91.2(2) N1 S1 C18 C23 -84.9(2) N1 C1 C2 C3 23.9(3) C1 N1 C8 C3 14.2(3) C1 N1 C8 C7 -163.8(3) C1 C2 C3 C4 164.3(3) C1 C2 C3 C8 -16.1(3) C2 C3 C4 C5 -179.3(2) C2 C3 C4 C10 3.5(4) C2 C3 C8 N1 1.6(3) C2 C3 C8 C7 179.6(2) C3 C4 C5 C6 -1.0(4) C3 C4 C5 C9 177.6(2) C3 C4 C10 C11 -86.0(3) C3 C4 C10 C13 95.1(3) C4 C3 C8 N1 -178.8(2) C4 C3 C8 C7 -0.8(4) C4 C5 C6 C7 0.3(4) C4 C10 C13 C12 -26.7(4) C4 C10 C13 C17 150.7(3) C5 C4 C10 C11 96.8(3) C5 C4 C10 C13 -82.1(3) C5 C6 C7 C8 0.2(4) C6 C7 C8 N1 177.7(2) C6 C7 C8 C3 0.1(4) C8 N1 C1 C2 -23.8(3) C8 C3 C4 C5 1.2(4) C8 C3 C4 C10 -176.1(2) C9 C5 C6 C7 -178.2(3) C10 C4 C5 C6 176.4(2) C10 C4 C5 C9 -5.1(4) C10 C13 C17 C16 -177.9(3) C11 C10 C13 C12 154.4(3) C11 C10 C13 C17 -28.2(4) C12 C13 C17 C16 -0.4(4) C12 C14 C15 C16 1.6(5) C13 C12 C14 C15 -1.4(5) C14 C12 C13 C10 178.3(3) C14 C12 C13 C17 0.7(4) C14 C15 C16 C17 -1.3(5) C15 C16 C17 C13 0.7(5) C18 S1 N1 C1 -63.0(2) C18 S1 N1 C8 67.0(2) C18 C19 C20 C21 -0.5(4) C19 C18 C23 C22 -0.7(4) C19 C20 C21 C22 -0.5(4) C19 C20 C21 C24 -179.6(3) C20 C21 C22 C23 1.0(4) C21 C22 C23 C18 -0.4(5) C23 C18 C19 C20 1.1(4) C24 C21 C22 C23 -179.9(3)