#------------------------------------------------------------------------------ #$Date: 2024-10-01 03:11:03 +0300 (Tue, 01 Oct 2024) $ #$Revision: 294946 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/27/1572721.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_1572721 loop_ _publ_author_name 'Yan, Xiaosheng' 'Weng, Peimin' 'Cao, Jinlian' 'Lin, Kexin' 'Qi, Yuanwei' 'Wu, Xin' 'Jiang, Yun-Bao' _publ_section_title ; Simultaneous formation of helical and sheet-like assemblies from short azapeptides enables spontaneous resolution ; _journal_name_full Nanoscale _journal_paper_doi 10.1039/D4NR02872D _journal_year 2024 _chemical_formula_moiety 'C17 H18 N4 O2 S, C H4 O' _chemical_formula_sum 'C18 H22 N4 O3 S' _chemical_formula_weight 374.45 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-03-09 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-03-09 deposited with the CCDC. 2024-09-30 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.2740(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.7516(2) _cell_length_b 8.56240(10) _cell_length_c 18.9290(3) _cell_measurement_reflns_used 5797 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 73.7320 _cell_measurement_theta_min 2.3610 _cell_volume 1904.20(5) _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 100.00(10) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.964 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_unetI/netI 0.0335 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.964 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 11530 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.964 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.304 _diffrn_reflns_theta_min 4.385 _exptl_absorpt_coefficient_mu 1.724 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.55830 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.306 _exptl_crystal_description block _exptl_crystal_F_000 792 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.291 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.055 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 238 _refine_ls_number_reflns 3748 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0381 _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^)+(0.0583P)^2^+0.7213P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1019 _refine_ls_wR_factor_ref 0.1046 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3456 _reflns_number_total 3748 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4nr02872d2.cif _cod_data_source_block exp_3814 _cod_database_code 1572721 _shelx_shelxl_version_number 2014/8 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Ternary CH refined with riding coordinates: C00F(H00F) 2.b Aromatic/amide H refined with riding coordinates: N005(H005), N006(H006), N007(H007), N008(H008), C00D(H00D), C00G(H00G), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P) 2.c Idealised Me refined as rotating group: C00H(H00A,H00B,H00C), C00Q(H00E,H00H,H00Q) 2.d Idealised tetrahedral OH refined as rotating group: O004(H004) ; _shelx_res_file ; exp_3814.res created by SHELXL-2014/8 TITL exp_3814_a.res in P2(1)/n REM Old TITL exp_3814 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.115, Rweak 0.020, Alpha 0.017, Orientation as input REM Formula found by SHELXT: C18 N4 O3 S CELL 1.54184 11.7516 8.5624 18.929 90 91.274 90 ZERR 4 0.0002 0.0001 0.0003 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O S UNIT 72 88 16 12 4 L.S. 10 PLAN 20 BOND $H list 4 fmap 2 53 ACTA REM REM REM WGHT 0.058300 0.721300 FVAR 0.49270 S001 5 0.867800 0.331788 0.480269 11.00000 0.02199 0.01364 = 0.02577 0.00221 -0.00902 -0.00002 O002 4 0.579389 0.760029 0.357997 11.00000 0.02366 0.01961 = 0.02199 0.00522 -0.00579 -0.00049 O003 4 0.836222 0.709037 0.314095 11.00000 0.02493 0.01948 = 0.02482 -0.00426 -0.00604 0.00372 O004 4 0.779459 1.002640 0.534221 11.00000 0.03214 0.01914 = 0.02886 0.00137 -0.00422 -0.00394 AFIX 147 H004 2 0.771333 1.092331 0.519787 11.00000 -1.50000 AFIX 0 N005 3 0.664665 0.939761 0.290785 11.00000 0.02015 0.01640 = 0.01716 0.00191 -0.00671 -0.00056 AFIX 43 H005 2 0.667691 0.986901 0.250753 11.00000 -1.20000 AFIX 0 N006 3 0.825882 0.774226 0.430325 11.00000 0.02381 0.01235 = 0.02144 0.00170 -0.00838 0.00083 AFIX 43 H006 2 0.809047 0.845427 0.460386 11.00000 -1.20000 AFIX 0 N007 3 0.869852 0.631904 0.453687 11.00000 0.02127 0.01355 = 0.02909 0.00453 -0.01204 -0.00077 AFIX 43 H007 2 0.939894 0.626808 0.467650 11.00000 -1.20000 AFIX 0 N008 3 0.696402 0.515864 0.435013 11.00000 0.02189 0.01387 = 0.02805 0.00386 -0.00743 -0.00096 AFIX 43 H008 2 0.670738 0.608054 0.426206 11.00000 -1.20000 AFIX 0 C009 1 0.809519 0.800777 0.359958 11.00000 0.01665 0.01441 = 0.02151 0.00034 -0.00555 -0.00206 C00A 1 0.576353 0.846203 0.305548 11.00000 0.02047 0.01420 = 0.01925 -0.00149 -0.00207 0.00228 C00B 1 0.619068 0.387235 0.427272 11.00000 0.01716 0.01407 = 0.02361 0.00215 -0.00408 0.00060 C00C 1 0.472813 0.851558 0.257734 11.00000 0.02088 0.01494 = 0.02124 -0.00164 -0.00404 0.00039 C00D 1 0.590652 0.337267 0.359494 11.00000 0.02063 0.01947 = 0.02096 0.00286 -0.00292 0.00141 AFIX 43 H00D 2 0.624573 0.382889 0.320659 11.00000 -1.20000 AFIX 0 C00E 1 0.805398 0.502134 0.454943 11.00000 0.02272 0.01710 = 0.01604 0.00060 -0.00548 -0.00063 C00F 1 0.755459 0.959758 0.344157 11.00000 0.02039 0.01488 = 0.01802 -0.00027 -0.00574 0.00106 AFIX 13 H00F 2 0.722540 1.000714 0.387517 11.00000 -1.20000 AFIX 0 C00G 1 0.468451 0.934718 0.194726 11.00000 0.02309 0.02124 = 0.02141 0.00025 -0.00433 -0.00457 AFIX 43 H00G 2 0.533054 0.985841 0.179148 11.00000 -1.20000 AFIX 0 C00H 1 0.844566 1.074353 0.318376 11.00000 0.02465 0.01732 = 0.02182 0.00048 -0.00631 -0.00278 AFIX 137 H00A 2 0.881829 1.030991 0.278240 11.00000 -1.50000 H00B 2 0.899738 1.093520 0.355529 11.00000 -1.50000 H00C 2 0.808290 1.170773 0.305112 11.00000 -1.50000 AFIX 0 C00I 1 0.511105 0.218491 0.349949 11.00000 0.02231 0.02105 = 0.02653 -0.00459 -0.00834 0.00397 AFIX 43 H00I 2 0.490969 0.185525 0.304557 11.00000 -1.20000 AFIX 0 C00J 1 0.569409 0.319758 0.485597 11.00000 0.02884 0.02005 = 0.02077 0.00059 -0.00195 0.00149 AFIX 43 H00J 2 0.588332 0.354399 0.530917 11.00000 -1.20000 AFIX 0 C00K 1 0.490948 0.199644 0.475593 11.00000 0.02668 0.02115 = 0.03058 0.00584 0.00530 -0.00013 AFIX 43 H00K 2 0.457807 0.152834 0.514409 11.00000 -1.20000 AFIX 0 C00L 1 0.367817 0.941715 0.154917 11.00000 0.03069 0.02284 = 0.02208 0.00224 -0.00953 -0.00273 AFIX 43 H00L 2 0.365346 0.997532 0.112763 11.00000 -1.20000 AFIX 0 C00M 1 0.461958 0.149401 0.407626 11.00000 0.01810 0.01677 = 0.04059 -0.00139 -0.00141 -0.00054 AFIX 43 H00M 2 0.409416 0.069190 0.401081 11.00000 -1.20000 AFIX 0 C00N 1 0.271557 0.866297 0.177597 11.00000 0.02419 0.03083 = 0.03234 0.00079 -0.01278 -0.00321 AFIX 43 H00N 2 0.204028 0.872543 0.151186 11.00000 -1.20000 AFIX 0 C00O 1 0.376189 0.773626 0.279978 11.00000 0.02746 0.03741 = 0.03199 0.01371 -0.00759 -0.00910 AFIX 43 H00O 2 0.378784 0.716400 0.321741 11.00000 -1.20000 AFIX 0 C00P 1 0.275814 0.781022 0.239991 11.00000 0.02570 0.04811 = 0.04099 0.01456 -0.00801 -0.01379 AFIX 43 H00P 2 0.211338 0.728770 0.255029 11.00000 -1.20000 AFIX 0 C00Q 1 0.868321 0.998425 0.586254 11.00000 0.05973 0.03164 = 0.04001 0.00566 -0.02321 -0.00788 AFIX 137 H00E 2 0.937070 1.038176 0.566514 11.00000 -1.50000 H00H 2 0.880245 0.892671 0.601549 11.00000 -1.50000 H00Q 2 0.847728 1.061580 0.625877 11.00000 -1.50000 AFIX 0 HKLF 4 REM exp_3814_a.res in P2(1)/n REM R1 = 0.0381 for 3456 Fo > 4sig(Fo) and 0.0407 for all 3748 data REM 238 parameters refined using 0 restraints END WGHT 0.0583 0.7213 REM Highest difference peak 0.291, deepest hole -0.392, 1-sigma level 0.055 Q1 1 0.6471 1.0432 0.2609 11.00000 0.05 0.29 Q2 1 0.9131 1.0995 0.5966 11.00000 0.05 0.24 Q3 1 0.9251 0.3346 0.4212 11.00000 0.05 0.22 Q4 1 0.5814 0.3580 0.4556 11.00000 0.05 0.22 Q5 1 0.7814 0.9984 0.6405 11.00000 0.05 0.21 Q6 1 0.9601 0.3205 0.4594 11.00000 0.05 0.20 Q7 1 0.8054 0.2448 0.4955 11.00000 0.05 0.19 Q8 1 0.4413 0.8151 0.2628 11.00000 0.05 0.19 Q9 1 0.7891 0.8804 0.3563 11.00000 0.05 0.18 Q10 1 0.4141 0.8470 0.2733 11.00000 0.05 0.18 Q11 1 0.9309 0.4133 0.4694 11.00000 0.05 0.18 Q12 1 0.6914 0.5849 0.3983 11.00000 0.05 0.18 Q13 1 0.7751 1.0953 0.3632 11.00000 0.05 0.18 Q14 1 0.8040 0.4313 0.4924 11.00000 0.05 0.18 Q15 1 0.8170 0.3248 0.5357 11.00000 0.05 0.18 Q16 1 0.5439 0.2791 0.3593 11.00000 0.05 0.18 Q17 1 0.8824 0.4193 0.4255 11.00000 0.05 0.18 Q18 1 0.8027 1.0259 0.3342 11.00000 0.05 0.18 Q19 1 0.5186 0.8528 0.2800 11.00000 0.05 0.17 Q20 1 0.5886 0.3893 0.3934 11.00000 0.05 0.17 ; _shelx_res_checksum 72224 _shelx_hkl_file ; 0 0 -2 209.23 8.86 0 0 2 209.04 8.43 0 0 -3 0.30 0.64 0 0 3 0.05 0.29 0 0 -4 382.02 16.29 0 0 4 377.09 15.35 0 0 -5 0.18 1.03 0 0 5 0.39 0.53 0 0 6 1700.34 63.31 0 0 6 1507.80 63.69 0 0 7 0.34 0.46 0 0 7 -0.50 0.78 0 0 8 549.91 22.36 0 0 8 491.48 21.33 0 0 9 -0.22 0.92 0 0 9 0.92 0.65 0 0 10 370.78 17.35 0 0 -11 0.13 0.70 0 0 11 -0.29 1.19 0 0 12 0.32 1.15 0 0 13 1.40 1.16 0 0 14 13.95 2.77 0 0 14 19.07 1.85 0 0 -14 17.55 1.57 0 0 -15 0.53 1.66 0 0 -15 -0.20 0.52 0 0 15 -0.82 1.59 0 0 15 -1.24 0.78 0 0 -16 20.25 3.92 0 0 -16 24.85 2.03 0 0 16 25.03 2.28 0 0 17 3.23 0.89 0 0 -17 0.33 0.70 0 0 -18 587.63 24.46 0 0 18 617.07 24.93 0 0 19 0.13 0.80 0 0 20 0.72 0.70 0 0 21 0.10 0.69 0 0 22 25.76 1.83 0 0 23 0.54 0.35 0 -1 0 0.11 0.14 0 -1 1 281.36 11.65 0 -1 1 291.75 11.48 0 1 1 298.65 11.48 0 -1 -2 11.57 1.11 0 1 -2 13.15 1.15 0 1 -3 751.86 30.63 0 -1 -3 732.72 30.60 0 1 3 797.82 30.25 0 -1 4 380.84 15.92 0 1 4 388.78 15.94 0 -1 5 32.64 2.46 0 1 5 36.34 2.52 0 1 6 9.66 1.44 0 -1 6 6.43 1.09 0 -1 6 8.90 1.40 0 -1 7 43.48 3.03 0 1 7 42.61 3.24 0 -1 7 42.35 3.26 0 1 8 490.93 20.75 0 -1 8 450.38 20.14 0 -1 8 492.77 20.79 0 1 9 456.16 19.78 0 -1 9 409.80 18.99 0 -1 9 468.15 19.92 0 -1 -10 142.30 6.86 0 1 -10 140.65 6.85 0 -1 10 141.97 7.76 0 -1 10 149.08 8.41 0 1 10 152.05 8.41 0 -1 11 0.24 0.41 0 -1 11 1.15 1.04 0 1 11 0.29 1.07 0 -1 11 0.45 0.67 0 -1 12 706.66 27.38 0 -1 12 647.32 30.03 0 1 12 637.55 29.97 0 -1 13 1.07 0.72 0 1 13 0.24 0.59 0 1 13 -0.35 1.47 0 1 -13 0.32 0.42 0 -1 13 0.35 1.56 0 -1 13 0.78 0.52 0 -1 -14 758.03 33.71 0 1 -14 743.85 33.75 0 -1 14 748.42 29.25 0 1 14 724.29 29.19 0 -1 14 622.59 31.67 0 1 14 639.68 31.78 0 1 -14 726.13 28.70 0 -1 -15 44.96 5.58 0 1 -15 50.20 5.97 0 1 15 50.06 3.27 0 1 -15 43.09 2.81 0 -1 15 50.02 3.29 0 -1 15 39.55 4.82 0 -1 16 81.60 4.78 0 1 -16 84.99 4.46 0 1 16 83.63 4.82 0 -1 -16 81.07 7.89 0 1 -16 90.28 8.28 0 1 17 84.20 4.86 0 1 -17 86.19 4.55 0 -1 17 82.41 4.82 0 1 18 74.83 4.42 0 -1 18 72.97 4.36 0 1 -18 72.77 4.06 0 -1 19 1.05 0.79 0 1 19 0.92 0.89 0 1 -19 0.91 0.71 0 1 20 64.02 3.75 0 -1 20 62.84 3.71 0 1 21 2.21 0.63 0 -1 21 1.90 0.66 0 1 22 3.04 0.72 0 -1 22 3.63 0.75 0 -1 23 15.84 1.15 0 1 23 14.82 1.13 0 -2 0 755.44 29.52 0 -2 -1 2105.23 83.07 0 -2 1 2240.16 83.40 0 -2 2 229.05 9.09 0 -2 2 228.36 9.52 0 2 2 216.09 9.03 0 -2 3 252.57 10.68 0 2 3 246.31 10.31 0 -2 3 247.12 10.34 0 -2 4 107.40 5.39 0 2 4 108.77 5.19 0 -2 4 106.98 5.20 0 2 5 4.55 0.94 0 -2 5 5.10 0.95 0 2 6 383.44 16.42 0 -2 6 382.67 16.49 0 -2 7 104.12 5.91 0 2 7 108.06 5.92 0 -2 8 1069.11 42.30 0 2 8 1033.88 42.16 0 -2 8 1005.53 42.05 0 2 9 371.09 16.95 0 -2 9 367.59 16.79 0 -2 9 376.54 17.05 0 -2 10 3.04 1.08 0 -2 10 3.17 1.16 0 2 10 2.49 1.17 0 -2 10 2.99 0.68 0 -2 11 34.23 3.66 0 2 11 36.15 3.73 0 -2 11 28.03 3.29 0 -2 11 41.66 2.49 0 -2 11 33.33 2.23 0 2 12 34.01 3.86 0 -2 12 34.21 3.92 0 -2 12 42.43 2.66 0 -2 -13 20.41 3.38 0 2 -13 18.14 3.37 0 -2 -13 17.21 1.52 0 -2 13 22.12 1.93 0 2 13 21.28 1.88 0 2 -13 18.11 1.53 0 -2 13 17.90 2.94 0 2 13 12.25 2.51 0 -2 13 19.61 1.83 0 2 -14 68.24 6.79 0 -2 -14 80.18 7.25 0 2 14 74.38 4.36 0 -2 14 81.25 4.48 0 -2 -14 75.53 4.09 0 2 -14 83.26 4.12 0 -2 14 69.73 6.32 0 -2 14 80.38 4.39 0 2 -15 367.22 19.80 0 -2 -15 348.20 19.43 0 2 15 352.53 15.56 0 -2 15 355.07 15.58 0 2 -15 362.29 15.17 0 -2 15 383.62 15.58 0 2 -16 15.87 3.80 0 -2 -16 13.10 3.46 0 -2 16 16.43 1.74 0 2 -16 19.40 1.71 0 2 16 18.93 1.90 0 -2 16 16.83 1.82 0 2 17 329.12 14.47 0 -2 17 320.06 14.40 0 2 -17 344.44 14.12 0 -2 18 123.91 6.50 0 2 -18 135.30 6.32 0 2 18 132.41 6.62 0 2 19 17.23 1.83 0 -2 19 17.70 1.84 0 2 -19 21.77 1.77 0 -2 20 37.87 2.54 0 2 20 37.53 2.55 0 2 21 103.69 4.66 0 -2 21 96.88 4.57 0 2 22 0.18 0.50 0 -2 22 0.94 0.41 0 -3 0 0.36 0.38 0 -3 -1 870.85 34.37 0 -3 1 903.77 34.87 0 -3 -2 1154.51 38.47 0 -3 -2 1102.08 38.08 0 -3 2 1207.94 39.30 0 3 -3 535.54 21.74 0 -3 -3 542.58 21.69 0 -3 -3 545.14 21.53 0 -3 3 590.67 22.56 0 -3 -4 435.61 17.27 0 3 -4 421.11 17.27 0 -3 4 446.64 17.91 0 -3 4 395.45 17.03 0 3 5 754.56 31.51 0 -3 5 785.79 31.65 0 -3 6 75.90 4.66 0 -3 6 68.17 4.15 0 3 6 74.79 4.17 0 -3 7 453.41 19.23 0 3 7 420.24 18.55 0 -3 7 440.63 18.74 0 -3 8 12.44 1.21 0 -3 8 9.74 1.08 0 -3 8 11.91 1.87 0 -3 8 9.33 1.53 0 3 8 8.08 1.40 0 -3 9 12.46 1.30 0 -3 9 15.09 1.38 0 -3 9 10.78 1.86 0 3 9 12.97 1.88 0 -3 9 11.72 1.86 0 3 -10 447.56 20.48 0 -3 -10 455.20 20.51 0 -3 10 469.65 18.21 0 -3 10 457.33 18.29 0 -3 10 397.15 19.71 0 3 10 382.44 19.52 0 -3 -11 77.50 6.17 0 3 -11 78.38 6.15 0 -3 11 88.06 4.41 0 -3 11 87.68 4.30 0 3 11 66.64 5.38 0 -3 11 62.26 5.42 0 3 -12 1.45 1.20 0 -3 -12 1.45 1.26 0 -3 12 1.26 0.66 0 3 -12 1.30 0.50 0 -3 12 1.64 0.71 0 3 -13 18.46 3.16 0 -3 -13 21.72 3.37 0 -3 13 19.28 1.88 0 3 13 20.92 1.88 0 3 -13 23.35 1.73 0 -3 13 22.86 2.05 0 -3 13 21.64 1.92 0 -3 -14 25.02 3.86 0 3 -14 18.35 3.37 0 3 14 19.77 1.90 0 -3 14 20.64 1.95 0 3 -14 20.99 1.72 0 -3 14 24.32 2.13 0 -3 -15 77.48 7.55 0 3 -15 83.03 7.77 0 -3 15 96.66 5.23 0 3 15 96.91 5.22 0 -3 15 99.81 5.35 0 3 -15 108.06 5.01 0 -3 16 18.73 1.95 0 3 -16 23.96 1.86 0 -3 16 19.01 1.92 0 3 16 22.28 2.03 0 -3 17 29.19 2.35 0 -3 17 25.66 2.21 0 3 17 24.56 2.17 0 3 -17 27.25 2.05 0 -3 18 69.85 4.20 0 3 18 80.55 4.34 0 3 -18 84.12 4.13 0 -3 18 74.54 4.24 0 -3 19 67.18 3.82 0 3 -19 75.74 3.80 0 3 19 75.17 3.98 0 -3 20 39.50 2.70 0 3 20 40.97 2.52 0 -3 21 64.38 3.51 0 3 21 68.32 3.33 0 -4 0 271.54 11.35 0 -4 -1 3.64 0.53 0 -4 1 5.82 0.88 0 -4 2 6.76 1.08 0 -4 3 82.90 4.69 0 -4 4 133.32 6.92 0 -4 5 349.84 14.34 0 -4 5 341.57 14.32 0 -4 5 346.81 15.47 0 -4 6 36.44 2.35 0 -4 6 34.08 3.06 0 -4 7 25.45 1.92 0 -4 7 26.46 2.78 0 -4 8 8.18 1.12 0 -4 8 8.89 1.17 0 -4 8 6.77 1.56 0 -4 9 534.55 21.70 0 -4 9 541.09 21.78 0 -4 9 494.28 23.46 0 -4 10 276.43 11.60 0 -4 10 287.33 12.14 0 -4 10 281.06 12.19 0 -4 10 260.68 13.90 0 -4 11 25.81 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-4 -10 5.66 0.68 -11 4 -10 8.17 0.78 -11 4 -11 0.40 0.32 -11 -4 -11 0.41 0.29 -11 -4 -12 177.58 7.37 -11 4 -12 184.87 7.36 -11 -5 8 4.94 0.64 11 -5 -8 3.16 0.95 -11 -5 7 1.40 0.45 11 -5 -7 1.75 0.87 -11 -5 6 28.28 1.73 11 -5 -6 27.74 2.56 -11 -5 5 2.08 0.56 -11 -5 5 1.19 0.54 11 -5 -5 1.34 0.92 -11 -5 4 12.61 1.18 -11 -5 4 15.25 1.23 11 -5 -4 13.98 1.14 11 -5 -4 15.48 1.99 11 -5 -3 12.14 1.86 -11 -5 3 10.30 1.10 -11 -5 3 10.86 1.07 11 -5 -2 1.67 1.11 -11 -5 2 1.25 0.55 -11 -5 2 2.01 0.60 -11 -5 1 2.54 0.64 -11 -5 1 1.90 0.59 -11 -5 0 6.14 0.89 -11 -5 0 6.45 0.87 -11 -5 -1 0.15 0.50 -11 -5 -1 0.20 0.47 -11 -5 -2 0.29 0.52 -11 -5 -2 0.66 0.52 -11 5 -2 1.22 0.60 -11 5 -3 4.84 0.82 -11 -5 -4 82.82 3.94 -11 5 -4 85.08 4.09 -11 -5 -5 11.41 1.01 -11 5 -5 11.43 1.08 -11 -5 -6 0.99 0.42 -11 -5 -6 0.48 0.42 -11 5 -6 1.08 0.50 -11 -5 -7 54.69 2.78 -11 -5 -7 57.55 2.85 -11 5 -7 58.54 2.86 -11 -5 -8 41.37 2.17 -11 5 -8 41.96 2.19 -11 -5 -9 124.08 5.32 -11 5 -9 126.09 5.33 -11 5 -10 21.51 1.24 11 -6 -7 1.33 0.32 11 -6 -6 9.72 0.79 11 -6 -5 32.04 1.72 11 -6 -4 6.89 1.23 11 -6 -3 81.78 4.73 11 -6 -2 8.92 1.41 11 -6 -1 36.95 2.87 -11 -6 0 17.44 1.24 11 -6 0 17.52 1.91 -11 -6 -1 213.09 8.80 -11 6 -1 210.84 8.88 -11 -6 -2 1.59 0.46 -11 6 -2 1.71 0.52 -11 -6 -3 159.38 6.73 -11 6 -3 158.46 6.77 -11 -6 -4 10.19 0.89 -11 6 -4 10.04 0.91 -11 -6 -5 41.92 2.14 -11 6 -5 41.88 2.15 -11 -6 -6 1.08 0.35 -11 6 -6 1.09 0.35 -11 6 -7 52.69 2.45 -11 7 2 2.98 0.44 -11 7 1 -0.39 0.39 -11 7 0 10.85 0.80 -11 7 -1 24.56 1.34 12 0 -12 5.05 1.11 12 0 -11 -0.68 0.98 12 0 -10 16.41 1.95 12 0 -9 -0.16 1.02 12 0 -8 7.18 1.41 12 0 -7 -0.18 0.94 -12 0 7 0.74 0.51 12 0 -6 89.74 5.39 -12 0 6 84.54 4.15 12 0 -5 -0.92 1.08 -12 0 5 0.07 0.50 12 0 -4 120.21 6.94 -12 0 4 131.29 5.85 12 0 -3 0.56 1.08 -12 0 3 -0.22 0.57 12 0 -2 170.35 8.44 -12 0 2 157.72 7.09 12 0 -1 2.01 1.10 -12 0 1 -0.22 0.64 -12 0 0 31.22 2.02 -12 0 -1 0.49 0.55 -12 0 -2 274.98 11.74 -12 0 -2 288.46 11.70 -12 0 -3 -0.27 0.42 -12 0 -3 0.07 0.48 -12 0 -4 130.02 6.00 -12 0 -5 -0.15 0.49 -12 0 -6 82.82 4.06 -12 0 -7 0.39 0.38 -12 0 -8 0.58 0.40 -12 0 -9 0.30 0.33 -12 0 -10 5.59 0.60 -12 0 -11 -0.05 0.35 -12 0 -12 3.06 0.47 12 -1 -11 3.35 1.04 12 1 -11 4.64 1.13 12 -1 -10 -1.14 1.10 12 1 -10 -0.88 1.09 12 -1 -9 9.05 1.59 12 1 -9 9.38 1.66 12 -1 -8 4.24 1.19 12 1 -8 4.55 1.28 12 -1 -7 2.90 1.09 12 1 -7 4.76 1.22 12 -1 -6 1.40 1.02 12 1 -6 3.80 1.20 -12 -1 6 2.73 0.69 12 -1 -5 204.08 10.17 12 1 -5 213.76 10.34 -12 -1 5 213.32 9.12 12 -1 -4 15.64 2.05 12 1 -4 15.92 2.08 -12 -1 4 13.54 1.36 12 -1 -3 1.42 1.04 12 1 -3 1.11 1.11 -12 -1 3 2.85 0.75 12 -1 -2 46.33 3.55 12 1 -2 46.49 3.66 -12 -1 2 49.28 2.80 12 -1 -1 131.43 7.15 12 1 -1 134.89 7.30 -12 -1 1 136.87 6.20 -12 -1 0 55.05 3.04 -12 -1 -1 53.43 2.96 -12 -1 -2 68.83 3.73 -12 -1 -2 77.20 3.77 -12 -1 -3 32.55 2.20 -12 -1 -3 32.79 2.10 -12 -1 -3 30.03 2.02 -12 -1 -4 2.66 0.71 -12 1 -4 1.65 0.59 -12 -1 -4 1.81 0.58 -12 -1 -4 2.17 0.65 -12 1 -5 1.33 0.48 -12 -1 -5 0.80 0.53 -12 -1 -5 0.87 0.44 -12 1 -6 54.44 2.86 -12 -1 -6 61.60 3.10 -12 -1 -6 53.54 2.84 -12 -1 -7 0.14 0.48 -12 -1 -8 12.66 1.12 -12 -1 -9 32.25 1.90 -12 -1 -10 23.88 1.56 -12 -1 -10 22.91 1.44 -12 1 -11 20.80 1.33 -12 -1 -11 23.22 1.43 -12 1 -12 35.37 1.82 -12 -1 -12 40.26 1.97 -12 -2 13 39.13 1.90 -12 -2 12 7.52 0.72 -12 -2 10 40.45 2.51 12 -2 -10 49.79 3.12 12 2 -10 45.42 3.11 12 -2 -9 0.27 0.91 12 2 -9 1.43 1.07 -12 -2 8 83.89 4.01 12 -2 -8 80.75 4.83 12 2 -8 82.76 4.94 -12 -2 7 13.07 1.21 12 -2 -7 11.51 1.67 12 2 -7 10.70 1.71 -12 -2 6 -0.07 0.59 12 -2 -6 -0.47 1.03 12 2 -6 -0.68 1.13 -12 -2 5 13.87 1.35 12 -2 -5 14.80 1.89 -12 -2 4 91.27 4.52 12 -2 -4 92.35 5.39 12 2 -4 93.45 5.50 -12 -2 3 54.83 3.09 12 -2 -3 52.33 3.80 12 2 -3 59.05 4.05 -12 -2 2 30.49 2.08 12 -2 -2 25.82 2.59 12 2 -2 30.61 2.86 -12 -2 1 -0.08 0.69 12 2 -1 -2.62 1.57 -12 -2 0 36.34 2.26 12 -2 0 31.21 2.78 12 2 0 33.58 3.00 -12 -2 -1 1.70 0.69 -12 -2 -1 1.93 0.73 -12 -2 -2 2.12 0.66 -12 -2 -2 1.66 0.67 -12 -2 -2 2.01 0.69 -12 -2 -3 37.85 2.39 -12 -2 -3 40.19 2.39 -12 -2 -3 39.08 2.44 -12 -2 -4 24.63 1.78 -12 -2 -4 25.41 1.77 -12 -2 -4 24.68 1.83 -12 -2 -5 2.45 0.63 -12 -2 -5 1.69 0.61 -12 -2 -6 3.46 0.68 -12 -2 -6 3.29 0.71 -12 -2 -7 51.44 2.72 -12 -2 -7 55.27 2.89 -12 -2 -8 0.88 0.38 -12 -2 -8 1.94 0.54 -12 -2 -9 93.74 4.17 -12 -2 -9 86.19 4.15 -12 -2 -10 1.50 0.43 -12 -2 -12 17.12 1.08 -12 -3 10 5.80 0.70 -12 -3 9 37.45 2.07 -12 -3 8 3.12 0.64 -12 -3 7 22.67 1.59 12 3 -6 10.96 1.52 -12 -3 6 8.92 1.05 12 3 -5 28.33 2.54 -12 -3 5 31.36 2.01 12 -3 -4 87.75 5.35 12 3 -4 90.27 5.32 -12 -3 4 98.49 4.55 12 -3 -3 235.32 10.95 12 -3 -3 205.81 10.35 12 3 -3 235.71 10.77 -12 -3 3 240.34 9.82 12 -3 -2 12.64 1.75 12 3 -2 9.97 1.78 12 -3 -1 88.64 5.26 12 3 -1 94.54 5.56 -12 -3 1 104.63 4.87 -12 -3 1 105.62 4.81 -12 -3 0 0.15 0.48 -12 -3 0 1.14 0.61 -12 -3 0 -0.32 0.55 12 3 1 8.34 1.59 -12 -3 -1 11.61 1.15 -12 3 -1 10.99 1.10 -12 -3 -1 9.83 1.12 -12 -3 -1 8.99 1.10 -12 -3 -2 -0.30 0.50 -12 -3 -2 1.31 0.59 -12 -3 -2 0.74 0.60 12 3 2 0.71 1.15 12 -3 2 1.20 0.98 -12 -3 -3 121.27 5.55 -12 -3 -3 118.25 5.55 -12 -3 -3 122.68 5.54 12 3 3 118.82 6.24 -12 -3 -4 7.42 0.93 -12 -3 -5 17.12 1.36 -12 -3 -6 0.06 0.46 -12 -3 -6 0.35 0.40 -12 -3 -7 0.39 0.36 -12 -3 -7 0.88 0.42 -12 -3 -7 0.12 0.41 -12 -3 -8 16.67 1.16 -12 -3 -8 14.83 1.15 -12 -3 -8 16.58 1.23 -12 -3 -9 34.10 1.82 -12 -3 -9 37.26 1.96 -12 -3 -9 35.09 1.92 -12 -3 -10 61.65 2.88 -12 -3 -11 1.03 0.30 -12 -4 10 10.68 0.78 -12 -4 9 31.08 1.69 -12 -4 8 20.97 1.35 -12 -4 7 13.96 1.07 -12 -4 7 11.11 0.98 -12 -4 6 15.23 1.21 -12 -4 6 17.19 1.26 -12 -4 5 9.86 0.98 12 -4 -5 10.68 1.50 -12 -4 4 15.50 1.28 12 -4 -4 16.66 1.88 -12 -4 3 59.73 3.01 12 -4 -3 51.08 3.78 -12 -4 2 52.44 2.77 12 -4 -2 45.88 3.53 -12 -4 1 0.30 0.41 -12 4 0 53.22 2.83 -12 -4 0 50.82 2.71 -12 4 -1 13.93 1.21 -12 -4 -1 13.08 1.21 -12 -4 -1 11.55 1.09 -12 4 -2 9.45 1.00 -12 -4 -2 10.11 1.06 -12 -4 -2 9.30 0.96 -12 4 -3 17.73 1.33 -12 -4 -3 18.21 1.38 -12 -4 -3 14.65 1.24 -12 4 -4 79.17 3.67 -12 -4 -4 76.61 3.68 -12 -4 -4 73.17 3.62 -12 4 -5 47.89 2.43 -12 -4 -5 45.85 2.43 -12 -4 -5 42.60 2.38 -12 4 -6 1.13 0.40 -12 -4 -6 1.10 0.45 -12 -4 -6 1.10 0.41 -12 4 -7 44.59 2.30 -12 -4 -7 46.67 2.34 -12 -4 -7 47.70 2.36 -12 -4 -8 5.35 0.58 -12 -4 -8 5.00 0.60 -12 -4 -9 59.21 2.67 -12 -5 6 16.02 1.04 -12 -5 5 2.37 0.45 -12 -5 4 3.37 0.53 -12 -5 4 3.50 0.54 -12 -5 3 91.86 4.05 -12 -5 3 89.02 4.06 -12 -5 2 17.90 1.26 -12 -5 2 19.57 1.31 12 -5 -2 20.43 1.97 -12 -5 1 10.45 0.95 -12 -5 1 11.83 1.00 -12 5 1 12.18 1.05 12 -5 -1 11.35 1.49 -12 -5 0 4.27 0.65 -12 -5 0 5.97 0.70 -12 5 0 4.35 0.68 12 -5 0 3.88 1.00 -12 -5 -1 0.31 0.38 -12 5 -1 0.11 0.43 -12 5 -2 6.73 0.76 -12 5 -3 5.01 0.65 -12 5 -4 96.43 4.28 -12 -5 -5 0.17 0.32 -12 5 -5 0.33 0.31 -12 -5 -6 9.60 0.77 -12 5 -6 9.21 0.74 -12 -5 -7 3.21 0.41 -12 5 -7 2.33 0.37 -12 6 3 6.52 0.61 -12 6 2 48.35 2.28 -12 6 1 26.90 1.44 -12 6 0 100.60 4.30 -13 0 9 44.87 2.14 13 0 -8 0.13 0.68 -13 0 8 0.38 0.32 13 0 -7 183.15 8.15 -13 0 7 159.20 6.82 13 0 -6 0.73 0.96 -13 0 6 0.46 0.41 13 0 -5 293.77 12.39 -13 0 5 262.91 10.95 13 0 -4 -0.15 0.95 -13 0 4 0.05 0.40 13 0 -3 6.27 1.38 -13 0 3 7.17 0.78 13 0 -2 1.10 1.01 -13 0 2 -0.47 0.45 13 0 -1 25.61 2.42 -13 0 1 25.62 1.58 13 0 0 -0.92 1.15 -13 0 0 0.06 0.41 13 0 1 137.14 6.65 -13 0 -1 117.35 5.37 -13 0 -2 0.48 0.47 -13 0 -3 3.24 0.67 -13 0 -4 -0.18 0.41 -13 0 -5 107.65 4.83 -13 0 -6 -0.05 0.33 -13 0 -7 33.70 1.81 -13 0 -8 0.10 0.24 -13 0 -9 19.92 1.27 -13 0 -10 0.35 0.26 -13 -1 10 1.54 0.35 -13 -1 9 0.08 0.32 13 -1 -8 19.14 1.86 13 1 -8 19.57 1.90 -13 -1 8 19.71 1.28 13 -1 -7 8.41 1.32 13 1 -7 8.11 1.33 -13 -1 7 7.36 0.79 13 -1 -6 115.95 6.13 13 1 -6 121.07 6.23 -13 -1 6 115.92 5.16 13 -1 -5 16.79 1.92 13 1 -5 17.42 2.01 -13 -1 5 17.37 1.30 13 -1 -4 36.72 2.84 13 1 -4 31.69 2.74 -13 -1 4 31.89 1.94 13 -1 -3 101.58 5.76 13 1 -3 109.73 5.94 -13 -1 3 107.95 4.86 13 -1 -2 54.86 3.57 13 1 -2 47.40 3.49 -13 -1 2 47.81 2.60 13 -1 -1 162.28 8.25 13 1 -1 177.40 8.48 -13 -1 1 172.42 7.34 13 -1 0 5.36 1.12 13 1 0 3.21 1.07 -13 -1 0 2.89 0.66 -13 -1 0 3.49 0.64 13 -1 1 28.26 2.46 13 1 1 31.09 2.62 -13 -1 -1 28.03 1.83 -13 -1 -1 30.91 1.85 -13 -1 -2 5.86 0.81 -13 1 -2 4.43 0.68 13 -1 2 1.93 1.02 13 1 2 3.78 1.17 -13 -1 -2 4.88 0.71 -13 -1 -2 4.38 0.68 -13 -1 -3 25.90 1.70 -13 1 -3 23.54 1.54 -13 -1 -3 22.56 1.52 -13 1 -4 5.33 0.65 -13 -1 -4 4.36 0.60 -13 1 -5 111.31 5.16 -13 -1 -5 137.40 5.48 -13 -1 -6 33.72 1.93 -13 -1 -7 6.94 0.72 -13 -1 -8 0.49 0.32 -13 -1 -9 54.97 2.52 -13 -1 -10 23.44 1.31 -13 -2 10 11.36 0.80 -13 -2 9 6.09 0.64 -13 -2 8 14.61 1.06 -13 -2 7 163.10 6.88 13 -2 -6 3.21 0.96 13 2 -6 3.66 0.97 -13 -2 6 4.96 0.69 13 -2 -5 -0.12 0.66 13 2 -5 0.40 0.75 -13 -2 5 1.46 0.52 13 -2 -4 128.38 6.87 13 2 -4 146.30 7.19 -13 -2 4 148.25 6.24 13 -2 -3 2.54 0.92 13 2 -3 2.67 1.10 -13 -2 3 2.96 0.65 13 -2 -2 -1.40 1.18 13 2 -2 -0.71 1.11 -13 -2 2 0.49 0.49 -13 -2 2 0.46 0.44 13 -2 -1 19.60 2.06 13 2 -1 19.29 2.15 -13 -2 1 19.85 1.51 -13 -2 1 22.67 1.53 13 -2 0 5.71 1.28 13 2 0 5.95 1.43 -13 -2 0 10.18 1.02 -13 -2 0 9.45 0.98 -13 -2 -1 68.33 3.21 13 -2 1 60.69 3.75 13 2 1 62.20 3.92 -13 -2 -1 63.34 3.13 -13 -2 -1 68.56 3.16 -13 -2 -2 79.24 3.83 13 -2 2 72.53 4.33 13 2 2 74.77 4.50 -13 -2 -2 81.94 3.82 -13 -2 -2 83.47 3.81 -13 -2 -3 1.86 0.53 13 -2 3 1.45 0.93 13 2 3 1.12 0.97 -13 -2 -3 1.92 0.53 -13 -2 -4 21.12 1.44 13 -2 4 18.76 1.73 13 2 4 20.30 1.88 -13 -2 -4 19.35 1.34 -13 -2 -5 25.14 1.52 -13 -2 -5 26.93 1.65 -13 -2 -6 13.90 0.99 -13 -2 -6 16.15 1.12 -13 -2 -6 14.46 1.12 -13 -2 -7 22.70 1.38 -13 -2 -7 21.76 1.38 -13 -2 -8 16.23 1.08 -13 -2 -8 16.14 1.07 -13 -2 -9 121.68 5.07 -13 -2 -9 121.49 5.10 -13 -3 9 15.37 0.96 -13 -3 8 48.06 2.43 -13 -3 8 57.13 2.50 -13 -3 7 14.64 1.06 -13 -3 7 16.55 1.10 -13 -3 6 6.75 0.72 -13 -3 5 8.23 0.82 -13 -3 4 48.77 2.54 -13 -3 4 52.76 2.66 -13 -3 4 54.52 2.65 -13 -3 3 7.83 0.81 -13 -3 3 8.74 0.90 -13 -3 3 8.64 0.88 -13 -3 2 9.73 0.92 -13 -3 2 11.36 1.02 -13 -3 2 10.77 1.00 -13 -3 1 1.61 0.48 -13 -3 1 1.80 0.53 -13 -3 1 1.83 0.54 -13 -3 0 17.99 1.32 -13 -3 0 18.88 1.38 -13 -3 0 20.11 1.38 -13 -3 -1 22.67 1.50 -13 -3 -1 21.49 1.51 -13 -3 -1 26.28 1.59 -13 -3 -2 25.30 1.55 -13 -3 -2 22.68 1.52 -13 -3 -3 4.50 0.63 -13 -3 -4 16.53 1.16 -13 -3 -5 2.04 0.43 -13 -3 -6 122.37 5.13 -13 -3 -6 116.59 5.03 -13 -3 -7 19.27 1.19 -13 -3 -8 3.03 0.41 -13 -4 6 87.51 3.76 -13 -4 5 82.44 3.62 -13 -4 4 2.92 0.47 -13 -4 3 19.75 1.27 -13 -4 0 78.95 3.52 -13 -4 0 74.57 3.50 -13 -4 -1 81.78 3.70 -13 -4 -2 19.79 1.25 -13 -4 -2 23.36 1.36 -13 -4 -3 0.04 0.26 -13 -4 -3 0.24 0.32 -13 -4 -4 64.73 3.01 -13 -4 -4 70.47 3.07 -13 -4 -5 3.94 0.46 -13 -4 -5 3.59 0.44 -14 0 5 0.24 0.27 -14 0 4 58.65 2.71 -14 0 3 0.22 0.29 -14 0 2 1.47 0.35 -14 0 1 0.24 0.37 -14 0 0 24.00 1.47 -14 0 -1 0.05 0.32 -14 0 -2 137.95 5.84 -14 0 -3 0.23 0.30 -14 0 -4 19.91 1.17 -14 -1 6 32.81 1.69 -14 -1 5 1.51 0.37 -14 -1 4 18.92 1.22 -14 -1 4 19.87 1.12 -14 -1 3 0.73 0.36 -14 -1 3 0.87 0.31 -14 -1 2 4.99 0.61 -14 -1 2 4.13 0.54 -14 -1 2 3.66 0.46 -14 -1 1 1.99 0.46 -14 1 1 1.46 0.36 -14 -1 1 1.56 0.39 -14 -1 1 1.43 0.35 -14 -1 0 17.53 1.17 -14 1 0 14.22 1.01 -14 -1 0 15.24 1.02 -14 1 -1 3.94 0.48 -14 -1 -1 5.17 0.63 -14 -1 -1 3.62 0.46 -14 1 -2 0.03 0.23 -14 -1 -2 -0.04 0.34 -14 -1 -3 1.62 0.38 -14 -1 -4 5.21 0.57 -14 -1 -5 0.33 0.25 -14 -2 6 71.28 3.12 -14 -2 5 66.24 3.09 -14 -2 5 76.90 3.19 -14 -2 4 13.81 0.94 -14 -2 4 14.20 0.96 -14 -2 4 14.16 0.92 -14 -2 3 0.80 0.34 -14 -2 3 0.46 0.30 -14 -2 3 0.47 0.32 -14 -2 2 39.76 2.02 -14 -2 2 39.74 2.01 -14 -2 2 39.66 1.97 -14 -2 1 14.61 1.02 -14 -2 1 15.46 1.02 -14 -2 0 20.42 1.24 -14 -2 -1 39.33 1.97 -14 -2 -1 36.29 1.87 -14 -2 -2 29.84 1.57 -14 -2 -2 26.36 1.44 -14 -2 -3 17.10 1.09 -14 -2 -4 1.37 0.32 -14 -3 3 34.69 1.71 -14 -3 2 0.56 0.29 -14 -3 2 1.04 0.32 -14 -3 1 25.90 1.38 -14 -3 0 8.98 0.68 -14 -3 0 9.61 0.70 -14 -3 -1 65.94 2.91 0 0 0 0.00 0.00 TITL exp_3814 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 11.751639 8.562395 18.929007 90.0000 91.2744 90.0000 ZERR 8.00 0.000164 0.000101 0.000259 0.0000 0.0013 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O UNIT 88.00 80.00 8.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 2169 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S001 S 0.86780(3) 0.33179(4) 0.48027(2) 0.02061(12) Uani 1 1 d . . . . . O002 O 0.57939(9) 0.76003(11) 0.35800(5) 0.0218(2) Uani 1 1 d . . . . . O003 O 0.83622(9) 0.70904(12) 0.31409(5) 0.0232(2) Uani 1 1 d . . . . . O004 O 0.77946(9) 1.00264(12) 0.53422(6) 0.0268(2) Uani 1 1 d . . . . . H004 H 0.7713 1.0923 0.5198 0.040 Uiso 1 1 calc GR . . . . N005 N 0.66466(10) 0.93976(13) 0.29078(6) 0.0180(2) Uani 1 1 d . . . . . H005 H 0.6677 0.9869 0.2508 0.022 Uiso 1 1 calc R . . . . N006 N 0.82588(10) 0.77423(13) 0.43033(6) 0.0193(3) Uani 1 1 d . . . . . H006 H 0.8090 0.8454 0.4604 0.023 Uiso 1 1 calc R . . . . N007 N 0.86985(10) 0.63190(14) 0.45369(7) 0.0215(3) Uani 1 1 d . . . . . H007 H 0.9399 0.6268 0.4677 0.026 Uiso 1 1 calc R . . . . N008 N 0.69640(10) 0.51586(14) 0.43501(7) 0.0214(3) Uani 1 1 d . . . . . H008 H 0.6707 0.6081 0.4262 0.026 Uiso 1 1 calc R . . . . C009 C 0.80952(11) 0.80078(15) 0.35996(7) 0.0176(3) Uani 1 1 d . . . . . C00A C 0.57635(12) 0.84620(15) 0.30555(7) 0.0180(3) Uani 1 1 d . . . . . C00B C 0.61907(11) 0.38724(15) 0.42727(7) 0.0183(3) Uani 1 1 d . . . . . C00C C 0.47281(12) 0.85156(15) 0.25773(8) 0.0191(3) Uani 1 1 d . . . . . C00D C 0.59065(12) 0.33727(16) 0.35949(8) 0.0204(3) Uani 1 1 d . . . . . H00D H 0.6246 0.3829 0.3207 0.024 Uiso 1 1 calc R . . . . C00E C 0.80540(12) 0.50213(16) 0.45494(7) 0.0187(3) Uani 1 1 d . . . . . C00F C 0.75546(12) 0.95976(15) 0.34416(7) 0.0179(3) Uani 1 1 d . . . . . H00F H 0.7225 1.0007 0.3875 0.021 Uiso 1 1 calc R . . . . C00G C 0.46845(13) 0.93472(17) 0.19473(8) 0.0220(3) Uani 1 1 d . . . . . H00G H 0.5331 0.9858 0.1791 0.026 Uiso 1 1 calc R . . . . C00H C 0.84457(12) 1.07435(16) 0.31838(8) 0.0214(3) Uani 1 1 d . . . . . H00A H 0.8818 1.0310 0.2782 0.032 Uiso 1 1 calc GR . . . . H00B H 0.8997 1.0935 0.3555 0.032 Uiso 1 1 calc GR . . . . H00C H 0.8083 1.1708 0.3051 0.032 Uiso 1 1 calc GR . . . . C00I C 0.51110(12) 0.21849(17) 0.34995(8) 0.0234(3) Uani 1 1 d . . . . . H00I H 0.4910 0.1855 0.3046 0.028 Uiso 1 1 calc R . . . . C00J C 0.56941(13) 0.31976(17) 0.48560(8) 0.0233(3) Uani 1 1 d . . . . . H00J H 0.5883 0.3544 0.5309 0.028 Uiso 1 1 calc R . . . . C00K C 0.49095(13) 0.19964(18) 0.47559(9) 0.0261(3) Uani 1 1 d . . . . . H00K H 0.4578 0.1528 0.5144 0.031 Uiso 1 1 calc R . . . . C00L C 0.36782(14) 0.94172(17) 0.15492(8) 0.0254(3) Uani 1 1 d . . . . . H00L H 0.3653 0.9975 0.1128 0.030 Uiso 1 1 calc R . . . . C00M C 0.46196(13) 0.14940(17) 0.40763(9) 0.0252(3) Uani 1 1 d . . . . . H00M H 0.4094 0.0692 0.4011 0.030 Uiso 1 1 calc R . . . . C00N C 0.27156(14) 0.86630(19) 0.17760(9) 0.0293(3) Uani 1 1 d . . . . . H00N H 0.2040 0.8725 0.1512 0.035 Uiso 1 1 calc R . . . . C00O C 0.37619(14) 0.7736(2) 0.27998(9) 0.0324(4) Uani 1 1 d . . . . . H00O H 0.3788 0.7164 0.3217 0.039 Uiso 1 1 calc R . . . . C00P C 0.27581(15) 0.7810(2) 0.23999(10) 0.0384(4) Uani 1 1 d . . . . . H00P H 0.2113 0.7288 0.2550 0.046 Uiso 1 1 calc R . . . . C00Q C 0.86832(19) 0.9984(2) 0.58625(11) 0.0442(5) Uani 1 1 d . . . . . H00E H 0.9371 1.0382 0.5665 0.066 Uiso 1 1 calc GR . . . . H00H H 0.8802 0.8927 0.6015 0.066 Uiso 1 1 calc GR . . . . H00Q H 0.8477 1.0616 0.6259 0.066 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 S001 0.02199(19) 0.01364(19) 0.0258(2) 0.00221(12) -0.00902(14) -0.00002(11) O002 0.0237(5) 0.0196(5) 0.0220(5) 0.0052(4) -0.0058(4) -0.0005(4) O003 0.0249(5) 0.0195(5) 0.0248(5) -0.0043(4) -0.0060(4) 0.0037(4) O004 0.0321(6) 0.0191(5) 0.0289(6) 0.0014(4) -0.0042(4) -0.0039(4) N005 0.0202(6) 0.0164(5) 0.0172(5) 0.0019(4) -0.0067(4) -0.0006(4) N006 0.0238(6) 0.0124(5) 0.0214(6) 0.0017(4) -0.0084(5) 0.0008(4) N007 0.0213(6) 0.0135(5) 0.0291(7) 0.0045(5) -0.0120(5) -0.0008(4) N008 0.0219(6) 0.0139(5) 0.0280(6) 0.0039(5) -0.0074(5) -0.0010(5) C009 0.0166(6) 0.0144(6) 0.0215(7) 0.0003(5) -0.0056(5) -0.0021(5) C00A 0.0205(7) 0.0142(6) 0.0193(7) -0.0015(5) -0.0021(5) 0.0023(5) C00B 0.0172(6) 0.0141(6) 0.0236(7) 0.0022(5) -0.0041(5) 0.0006(5) C00C 0.0209(7) 0.0149(6) 0.0212(7) -0.0016(5) -0.0040(5) 0.0004(5) C00D 0.0206(7) 0.0195(7) 0.0210(7) 0.0029(5) -0.0029(5) 0.0014(5) C00E 0.0227(7) 0.0171(6) 0.0160(6) 0.0006(5) -0.0055(5) -0.0006(5) C00F 0.0204(6) 0.0149(6) 0.0180(6) -0.0003(5) -0.0057(5) 0.0011(5) C00G 0.0231(7) 0.0212(7) 0.0214(7) 0.0002(5) -0.0043(5) -0.0046(5) C00H 0.0247(7) 0.0173(6) 0.0218(7) 0.0005(5) -0.0063(5) -0.0028(5) C00I 0.0223(7) 0.0211(7) 0.0265(7) -0.0046(6) -0.0083(6) 0.0040(6) C00J 0.0288(8) 0.0201(7) 0.0208(7) 0.0006(5) -0.0020(6) 0.0015(6) C00K 0.0267(7) 0.0211(7) 0.0306(8) 0.0058(6) 0.0053(6) -0.0001(6) C00L 0.0307(8) 0.0228(7) 0.0221(7) 0.0022(6) -0.0095(6) -0.0027(6) C00M 0.0181(7) 0.0168(6) 0.0406(9) -0.0014(6) -0.0014(6) -0.0005(5) C00N 0.0242(7) 0.0308(8) 0.0323(8) 0.0008(7) -0.0128(6) -0.0032(6) C00O 0.0275(8) 0.0374(9) 0.0320(8) 0.0137(7) -0.0076(6) -0.0091(7) C00P 0.0257(8) 0.0481(10) 0.0410(10) 0.0146(8) -0.0080(7) -0.0138(7) C00Q 0.0597(12) 0.0316(9) 0.0400(10) 0.0057(8) -0.0232(9) -0.0079(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C00Q O004 H004 109.5 . . ? C00A N005 H005 120.6 . . ? C00A N005 C00F 118.71(11) . . ? C00F N005 H005 120.6 . . ? N007 N006 H006 120.0 . . ? C009 N006 H006 120.0 . . ? C009 N006 N007 120.04(12) . . ? N006 N007 H007 119.2 . . ? C00E N007 N006 121.57(11) . . ? C00E N007 H007 119.2 . . ? C00B N008 H008 117.8 . . ? C00E N008 H008 117.8 . . ? C00E N008 C00B 124.37(12) . . ? O003 C009 N006 123.87(13) . . ? O003 C009 C00F 123.21(12) . . ? N006 C009 C00F 112.91(11) . . ? O002 C00A N005 120.89(12) . . ? O002 C00A C00C 120.72(13) . . ? N005 C00A C00C 118.38(12) . . ? C00D C00B N008 118.09(13) . . ? C00D C00B C00J 120.76(13) . . ? C00J C00B N008 121.06(13) . . ? C00G C00C C00A 123.19(13) . . ? C00G C00C C00O 119.42(13) . . ? C00O C00C C00A 117.34(13) . . ? C00B C00D H00D 120.2 . . ? C00B C00D C00I 119.57(14) . . ? C00I C00D H00D 120.2 . . ? N007 C00E S001 118.36(10) . . ? N008 C00E S001 124.23(11) . . ? N008 C00E N007 117.40(12) . . ? N005 C00F C009 108.93(10) . . ? N005 C00F H00F 109.0 . . ? N005 C00F C00H 110.50(11) . . ? C009 C00F H00F 109.0 . . ? C00H C00F C009 110.52(11) . . ? C00H C00F H00F 109.0 . . ? C00C C00G H00G 119.9 . . ? C00C C00G C00L 120.17(14) . . ? C00L C00G H00G 119.9 . . ? C00F C00H H00A 109.5 . . ? C00F C00H H00B 109.5 . . ? C00F C00H H00C 109.5 . . ? H00A C00H H00B 109.5 . . ? H00A C00H H00C 109.5 . . ? H00B C00H H00C 109.5 . . ? C00D C00I H00I 119.9 . . ? C00M C00I C00D 120.19(14) . . ? C00M C00I H00I 119.9 . . ? C00B C00J H00J 120.4 . . ? C00B C00J C00K 119.28(14) . . ? C00K C00J H00J 120.4 . . ? C00J C00K H00K 119.9 . . ? C00J C00K C00M 120.14(14) . . ? C00M C00K H00K 119.9 . . ? C00G C00L H00L 119.8 . . ? C00N C00L C00G 120.34(14) . . ? C00N C00L H00L 119.8 . . ? C00I C00M C00K 120.05(14) . . ? C00I C00M H00M 120.0 . . ? C00K C00M H00M 120.0 . . ? C00L C00N H00N 120.1 . . ? C00L C00N C00P 119.78(14) . . ? C00P C00N H00N 120.1 . . ? C00C C00O H00O 119.9 . . ? C00P C00O C00C 120.17(15) . . ? C00P C00O H00O 119.9 . . ? C00N C00P C00O 120.11(15) . . ? C00N C00P H00P 119.9 . . ? C00O C00P H00P 119.9 . . ? O004 C00Q H00E 109.5 . . ? O004 C00Q H00H 109.5 . . ? O004 C00Q H00Q 109.5 . . ? H00E C00Q H00H 109.5 . . ? H00E C00Q H00Q 109.5 . . ? H00H C00Q H00Q 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S001 C00E 1.6969(14) . ? O002 C00A 1.2368(17) . ? O003 C009 1.2171(18) . ? O004 H004 0.8200 . ? O004 C00Q 1.420(2) . ? N005 H005 0.8600 . ? N005 C00A 1.3453(18) . ? N005 C00F 1.4630(16) . ? N006 H006 0.8600 . ? N006 N007 1.3919(16) . ? N006 C009 1.3607(18) . ? N007 H007 0.8600 . ? N007 C00E 1.3453(18) . ? N008 H008 0.8600 . ? N008 C00B 1.4333(17) . ? N008 C00E 1.3324(18) . ? C009 C00F 1.5289(18) . ? C00A C00C 1.5009(19) . ? C00B C00D 1.386(2) . ? C00B C00J 1.386(2) . ? C00C C00G 1.389(2) . ? C00C C00O 1.390(2) . ? C00D H00D 0.9300 . ? C00D C00I 1.390(2) . ? C00F H00F 0.9800 . ? C00F C00H 1.5232(19) . ? C00G H00G 0.9300 . ? C00G C00L 1.389(2) . ? C00H H00A 0.9600 . ? C00H H00B 0.9600 . ? C00H H00C 0.9600 . ? C00I H00I 0.9300 . ? C00I C00M 1.380(2) . ? C00J H00J 0.9300 . ? C00J C00K 1.391(2) . ? C00K H00K 0.9300 . ? C00K C00M 1.392(2) . ? C00L H00L 0.9300 . ? C00L C00N 1.379(2) . ? C00M H00M 0.9300 . ? C00N H00N 0.9300 . ? C00N C00P 1.388(2) . ? C00O H00O 0.9300 . ? C00O C00P 1.389(2) . ? C00P H00P 0.9300 . ? C00Q H00E 0.9600 . ? C00Q H00H 0.9600 . ? C00Q H00Q 0.9600 . ?