#------------------------------------------------------------------------------ #$Date: 2024-12-05 01:31:37 +0200 (Thu, 05 Dec 2024) $ #$Revision: 296220 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/96/7249663.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_7249663 loop_ _publ_author_name 'Yan, Wenjin' 'Wang, Tianwei' 'Zhang, Shufen' 'Lu, Rongwen' 'Hu, Yingxin' 'Chen, longming' 'Pang, Chaoran' 'Wang, Peng' _publ_section_title ; Two Stacking Types of Three--Dimensional Structure Cocrystals Based on Multiple Hydrogen Bonds ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE01071J _journal_year 2024 _chemical_formula_moiety '2(C3 H3 N3 S3), 2(C6 H12 N4)' _chemical_formula_sum 'C18 H30 N14 S6' _chemical_formula_weight 634.92 _chemical_name_common Phpm _chemical_name_systematic TAC-HMTA _space_group_crystal_system hexagonal _space_group_IT_number 186 _space_group_name_Hall 'P 6c -2c' _space_group_name_H-M_alt 'P 63 m c' _atom_sites_solution_hydrogens geom _audit_creation_date 2024-04-15 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-07-08 deposited with the CCDC. 2024-12-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 2 _cell_length_a 9.6534(18) _cell_length_b 9.6534(18) _cell_length_c 16.438(5) _cell_measurement_reflns_used 3621 _cell_measurement_temperature 120.15 _cell_measurement_theta_max 24.768 _cell_measurement_theta_min 2.436 _cell_volume 1326.6(5) _computing_cell_refinement 'SAINT V8.40A (Bruker, 2019)' _computing_data_reduction 'SAINT V8.40A (Bruker, 2019)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 298.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0920 _diffrn_reflns_av_unetI/netI 0.0588 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 8697 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.065 _diffrn_reflns_theta_max 25.065 _diffrn_reflns_theta_min 2.436 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.5957 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1475 before and 0.0885 after correction. The Ratio of minimum to maximum transmission is 0.7994. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.589 _exptl_crystal_description block _exptl_crystal_F_000 664 _refine_diff_density_max 0.745 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.078 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.0(4) _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 74 _refine_ls_number_reflns 931 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0455 _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^)+(0.0606P)^2^+1.3654P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1058 _refine_ls_wR_factor_ref 0.1140 _reflns_Friedel_coverage 0.912 _reflns_Friedel_fraction_full 0.984 _reflns_Friedel_fraction_max 0.984 _reflns_number_gt 773 _reflns_number_total 931 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce01071j2.cif _cod_data_source_block 4_pl _cod_original_cell_volume 1326.6(6) _cod_database_code 7249663 _shelx_shelxl_version_number 2019/3 _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. Twinned data refinement Scales: 1.0(4) -0.0(4) 2. Fixed Uiso At 1.2 times of: All C(H,H) groups, All N(H) groups 3. Others Fixed Sof: H4A(0.5) H4B(0.5) H5A(0.5) H5B(0.5) 4.a Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B) 4.b Aromatic/amide H refined with riding coordinates: N1(H1), N2(H2) ; _shelx_res_file ; TITL 4 P 3 1 c R = 0.05 New:P63mc 4_pl.res created by SHELXL-2019/3 at 10:29:21 on 15-Apr-2024 CELL 0.71073 9.6534 9.6534 16.438 90 90 120 ZERR 2 0.0018 0.0018 0.005 0 0 0 LATT -1 SYMM -Y+X,+X,0.5+Z SYMM -Y,+X-Y,+Z SYMM -X,-Y,0.5+Z SYMM +Y-X,-X,+Z SYMM +Y,-X+Y,0.5+Z SYMM +Y,+X,0.5+Z SYMM +Y-X,+Y,+Z SYMM -X,-X+Y,0.5+Z SYMM -Y,-X,+Z SYMM -Y+X,-Y,0.5+Z SYMM +X,+X-Y,+Z SFAC C H N S UNIT 36 60 28 12 EQIV $1 -2-Y,-1+X-Y,+Z EQIV $2 +Y-X,-1-X,+Z EQIV $3 -Y,+X-Y,+Z L.S. 10 PLAN 10 TEMP -153 CONF HTAB N1 N3 HTAB N2 N4 HTAB C3 S1_$1 HTAB C3 S1_$2 HTAB C6 S2 HTAB C6 S2_$3 BOND $H MORE -1 fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.060600 1.365400 BASF -0.00084 FVAR 0.34172 S1 4 -0.515031 -1.030063 0.353528 10.50000 0.01495 0.01165 = 0.01880 -0.00185 -0.00092 0.00582 N1 3 -0.492214 -0.746107 0.342673 10.50000 0.01829 0.01569 = 0.00943 0.00142 0.00285 0.00914 AFIX 43 H1 2 -0.597151 -0.798575 0.338467 10.50000 -1.20000 AFIX 0 C1 1 -0.415296 -0.830593 0.345757 10.50000 0.01292 S2 4 -0.302752 -0.151376 0.640223 10.50000 0.01255 0.01510 = 0.01745 0.00030 0.00061 0.00628 N2 3 -0.586431 -0.413569 0.648755 10.50000 0.01277 0.01277 = 0.00579 0.00064 -0.00064 0.00728 AFIX 43 H2 2 -0.533834 -0.466168 0.650668 10.50000 -1.20000 AFIX 0 C2 1 -0.499969 -0.249985 0.647350 10.50000 0.01213 N3 3 -0.833051 -0.916525 0.359715 10.50000 0.01248 0.01433 = 0.01118 -0.00021 -0.00043 0.00624 N5 3 -1.000000 -1.000000 0.481337 10.16667 0.01321 0.01321 = 0.00634 0.00000 0.00000 0.00660 C3 1 -0.916939 -0.833877 0.330058 10.50000 0.01539 0.01965 = 0.01025 0.00096 0.00048 0.00982 AFIX 23 H3A 2 -0.860913 -0.721826 0.349543 10.50000 -1.20000 H3B 2 -0.916197 -0.832397 0.269837 10.50000 -1.20000 AFIX 0 C4 1 -0.836640 -0.918320 0.451048 10.50000 0.01418 0.01872 = 0.00814 -0.00341 -0.00681 0.00709 AFIX 23 H4A 2 -0.780022 -0.972986 0.471631 10.50000 -1.20000 H4B 2 -0.780022 -0.807036 0.471631 10.50000 -1.20000 AFIX 0 N4 3 -0.417546 -0.582454 0.642771 10.50000 0.01072 0.01072 = 0.01019 0.00040 -0.00040 0.00558 N6 3 -0.333333 -0.666667 0.521102 10.16667 0.02146 0.02146 = 0.00192 0.00000 0.00000 0.01073 C5 1 -0.414770 -0.585230 0.551730 10.50000 0.01617 0.01617 = 0.00513 0.00227 -0.00227 0.00465 AFIX 23 H5A 2 -0.525966 -0.639861 0.531026 10.50000 -1.20000 H5B 2 -0.360139 -0.474034 0.531026 10.50000 -1.20000 AFIX 0 C6 1 -0.249974 -0.499949 0.672363 10.50000 0.01051 0.01032 = 0.01311 0.00326 0.00163 0.00516 AFIX 23 H6A 2 -0.249183 -0.498368 0.732584 10.50000 -1.20000 H6B 2 -0.193940 -0.387880 0.652905 10.50000 -1.20000 AFIX 0 HKLF 4 1 -1 0 0 0 -1 0 0 0 1 REM 4 P 3 1 c R = 0.05 New:P63mc REM wR2 = 0.1140, GooF = S = 1.057, Restrained GooF = 1.056 for all data REM R1 = 0.0455 for 773 Fo > 4sig(Fo) and 0.0598 for all 931 data REM 74 parameters refined using 0 restraints END WGHT 0.0614 1.1658 REM Highest difference peak 0.745, deepest hole -0.349, 1-sigma level 0.078 Q1 1 -0.6667 -0.3333 0.4875 10.16667 0.05 0.75 Q2 1 -0.4070 -0.2035 0.6360 10.50000 0.05 0.44 Q3 1 -1.0000 -1.0000 0.5150 10.16667 0.05 0.38 Q4 1 -0.6667 -0.3333 0.6472 10.16667 0.05 0.36 Q5 1 -0.5405 -0.2703 0.6441 10.50000 0.05 0.36 Q6 1 -0.7342 -0.8671 0.3434 10.50000 0.05 0.35 Q7 1 -0.4587 -0.9174 0.3581 10.50000 0.05 0.34 Q8 1 -0.6336 -1.1010 0.3486 11.00000 0.05 0.30 Q9 1 -0.1795 -0.0897 0.6428 10.50000 0.05 0.29 Q10 1 -0.4647 -0.5353 0.6545 10.50000 0.05 0.28 ; _shelx_res_checksum 59059 _shelx_hkl_file ; 1 0 0 16.10 1.80 -1 1 0 16.00 1.70 1 0 0 17.30 1.70 0 -1 0 16.80 2.30 -1 1 0 18.60 2.50 1 -1 0 16.20 1.70 -1 0 0 13.80 2.00 0 1 0 16.30 1.90 1 -1 0 17.40 2.20 1 1 0 751.12 50.59 1 -2 0 719.53 50.79 1 -2 0 686.53 50.39 -2 1 0 627.94 50.69 -2 1 0 777.52 50.19 -1 2 0 724.73 50.79 2 -1 0 728.93 50.19 -1 -1 0 723.03 50.39 -1 -1 0 719.93 50.49 -1 2 0 709.53 50.39 0 -2 0 219.58 16.70 -2 2 0 218.58 16.30 0 -2 0 219.58 16.90 -2 2 0 235.78 17.00 2 0 0 230.28 16.50 2 0 0 232.28 16.40 0 2 0 231.48 16.70 -2 0 0 226.28 16.60 2 -2 0 220.98 16.40 0 2 0 195.58 16.90 -2 0 0 203.88 16.50 2 -2 0 226.48 16.90 1 2 0 95.49 8.50 2 -3 0 100.69 9.30 1 2 0 97.49 9.10 -3 1 0 99.49 8.10 2 -3 0 99.69 8.50 -3 1 0 81.69 8.80 -1 -2 0 103.89 8.70 -2 3 0 103.59 9.40 3 -1 0 108.79 8.20 3 -1 0 104.49 8.40 -2 3 0 107.09 8.50 3 -1 0 83.79 8.80 -3 2 0 93.39 7.90 1 -3 0 80.79 8.80 2 1 0 93.29 8.70 2 1 0 109.99 8.90 -3 2 0 117.09 10.00 1 -3 0 90.79 8.50 -3 2 0 99.59 8.70 3 -2 0 92.39 8.60 -2 -1 0 100.49 8.50 -2 -1 0 95.29 8.40 -1 3 0 87.99 9.10 -1 3 0 101.29 8.40 3 -2 0 102.89 8.10 0 -3 0 1567.44 102.09 -3 3 0 1502.35 102.19 -3 3 0 1435.96 101.39 3 0 0 1268.47 101.89 0 -3 0 1369.06 102.09 3 0 0 1525.95 102.29 3 0 0 1634.84 101.59 0 3 0 1419.96 101.89 -3 0 0 1219.08 101.19 -3 0 0 1599.44 101.99 0 3 0 1437.56 102.29 3 -3 0 1368.56 101.99 3 -3 0 1552.14 101.59 -4 1 0 39.20 4.40 3 -4 0 41.10 5.10 1 3 0 38.60 4.90 3 -4 0 32.40 6.00 1 3 0 37.90 6.50 -4 1 0 35.00 5.50 4 -1 0 44.60 4.60 -3 4 0 44.80 6.70 -1 -3 0 43.60 5.30 -1 -3 0 41.50 5.90 4 -1 0 44.40 5.90 4 -1 0 40.60 4.70 2 2 0 385.26 28.40 2 -4 0 409.06 28.20 -4 2 0 334.27 28.60 2 -4 0 311.97 28.30 2 2 0 379.86 27.90 -4 2 0 382.16 27.70 -4 2 0 375.36 27.40 -2 -2 0 392.86 28.20 -2 -2 0 372.76 27.90 4 -2 0 371.76 27.40 -2 4 0 371.96 28.80 -2 4 0 339.07 27.70 4 -2 0 431.26 28.90 -4 3 0 42.00 4.60 -4 3 0 40.30 6.10 1 -4 0 39.00 6.10 1 -4 0 38.40 5.20 -4 3 0 46.10 7.20 3 1 0 48.70 5.10 3 1 0 50.49 6.00 -3 -1 0 44.10 5.20 4 -3 0 38.40 5.70 4 -3 0 38.10 4.70 -1 4 0 36.50 4.90 -1 4 0 40.00 6.50 -3 -1 0 41.50 5.30 -4 4 0 31.10 6.20 4 0 0 35.00 4.40 -4 4 0 36.70 6.00 0 -4 0 40.80 6.30 4 0 0 34.00 4.50 4 0 0 40.60 6.00 0 -4 0 33.90 5.10 -4 4 0 32.20 4.40 4 -4 0 33.40 5.80 -4 0 0 44.00 5.20 4 -4 0 41.10 4.90 -4 0 0 35.00 4.80 0 4 0 35.80 4.90 0 4 0 45.90 7.00 4 -5 0 607.64 41.00 1 4 0 543.55 41.80 -5 1 0 512.05 41.10 4 -5 0 482.05 41.40 1 4 0 579.74 41.20 5 -1 0 578.54 40.40 5 -1 0 546.05 40.50 -1 -4 0 548.15 41.50 -1 -4 0 564.64 41.50 -4 5 0 509.15 40.30 -4 5 0 607.54 42.50 3 -5 0 15.80 4.30 3 -5 0 18.10 4.00 2 3 0 25.50 5.30 2 3 0 15.40 3.60 -5 2 0 26.80 4.50 -5 2 0 25.00 3.60 5 -2 0 24.10 3.50 -2 -3 0 25.60 4.90 5 -2 0 29.30 4.20 -3 5 0 16.80 5.90 -3 5 0 20.80 3.80 -2 -3 0 15.20 4.00 5 -2 0 28.50 5.10 2 -5 0 23.60 5.00 -5 3 0 16.10 4.10 2 -5 0 19.90 4.30 -5 3 0 16.70 4.70 -5 3 0 13.60 2.80 3 2 0 18.50 4.50 3 2 0 25.50 4.50 5 -3 0 20.00 3.30 -3 -2 0 13.20 3.80 -3 -2 0 20.10 4.20 -2 5 0 18.50 3.70 -5 4 0 592.14 43.20 4 1 0 515.85 41.30 4 1 0 610.24 40.70 1 -5 0 494.85 41.50 1 -5 0 520.05 41.00 4 1 0 562.14 40.70 -5 4 0 509.45 39.90 -5 4 0 578.14 41.20 -4 -1 0 517.95 40.10 -1 5 0 583.94 42.80 5 -4 0 541.45 41.20 -4 -1 0 604.54 41.30 -1 5 0 527.45 40.80 5 -4 0 560.24 40.20 -5 5 0 26.60 4.10 5 0 0 22.70 5.20 5 0 0 28.00 4.70 -5 5 0 19.70 6.10 0 -5 0 28.90 5.40 5 0 0 34.20 4.60 -5 5 0 30.60 6.30 -5 0 0 28.90 6.00 0 5 0 22.00 4.40 0 5 0 27.30 6.60 -5 0 0 27.60 5.10 5 -5 0 28.90 4.70 1 5 0 10.90 3.50 -6 1 0 8.10 4.30 1 5 0 13.30 5.60 5 -6 0 12.00 4.70 5 -6 0 15.50 3.90 -1 -5 0 9.70 4.90 6 -1 0 18.40 3.50 6 -1 0 13.70 3.80 6 -1 0 12.20 4.10 -1 -5 0 17.10 4.40 -5 6 0 12.30 5.30 -6 2 0 48.00 8.80 -6 2 0 68.59 7.00 4 -6 0 71.39 8.00 -6 2 0 71.69 8.30 4 -6 0 59.19 9.30 2 4 0 65.89 7.60 6 -2 0 62.89 7.30 -4 6 0 66.29 10.20 6 -2 0 65.19 6.90 -2 -4 0 70.39 8.30 6 -2 0 61.89 8.40 -2 -4 0 62.59 9.30 3 -6 0 221.78 19.00 3 -6 0 210.08 20.00 -6 3 0 235.58 18.70 3 3 0 202.98 19.30 -6 3 0 220.98 17.90 -3 6 0 228.58 20.40 6 -3 0 243.08 18.10 -3 6 0 208.98 18.60 -3 -3 0 242.88 19.50 -3 -3 0 234.18 19.30 4 2 0 63.59 7.30 -6 4 0 53.39 8.40 4 2 0 62.39 8.60 -6 4 0 59.89 6.70 2 -6 0 64.19 9.60 2 -6 0 62.89 7.80 -4 -2 0 81.99 8.70 -2 6 0 57.29 9.80 -2 6 0 57.39 7.30 6 -4 0 67.49 7.10 -4 -2 0 52.79 7.20 5 1 0 6.90 3.00 1 -6 0 5.10 4.50 -6 5 0 3.20 5.50 5 1 0 17.20 3.80 5 1 0 15.30 4.90 -6 5 0 9.10 2.60 1 -6 0 7.30 3.60 -6 5 0 15.40 5.70 -1 6 0 12.20 5.10 -5 -1 0 9.70 3.40 -1 6 0 8.20 3.20 6 -5 0 4.70 4.20 -5 -1 0 13.10 4.00 6 -5 0 16.20 4.10 0 -6 0 79.19 9.80 6 0 0 94.09 9.60 -6 6 0 84.99 11.70 6 0 0 99.69 9.40 6 0 0 71.99 10.10 -6 0 0 107.39 10.00 0 6 0 87.99 11.90 -6 0 0 90.09 11.30 6 -6 0 82.99 9.30 6 -6 0 63.39 10.70 1 6 0 26.90 7.90 6 -7 0 18.50 4.80 7 -1 0 16.10 4.40 -1 -6 0 19.10 5.40 7 -1 0 19.50 4.10 -6 7 0 19.10 7.10 2 5 0 10.90 5.40 -7 2 0 11.90 5.00 5 -7 0 18.90 4.80 7 -2 0 9.00 3.10 -2 -5 0 6.50 5.70 -5 7 0 3.20 2.90 -5 7 0 15.30 6.50 7 -2 0 6.00 4.50 7 -2 0 8.10 3.40 -2 -5 0 17.40 5.20 4 -7 0 85.69 9.80 3 4 0 76.59 11.20 3 4 0 78.99 14.70 -7 3 0 90.39 8.80 -7 3 0 73.69 9.60 -3 -4 0 92.79 10.10 -3 -4 0 74.59 12.90 7 -3 0 82.59 9.20 -4 7 0 75.39 10.10 -4 7 0 78.59 11.90 7 -3 0 85.99 9.50 4 3 0 76.29 9.40 4 3 0 87.79 11.60 3 -7 0 75.69 9.80 -7 4 0 78.09 10.60 7 -4 0 101.09 12.30 -4 -3 0 73.29 9.50 -3 7 0 95.99 12.80 -4 -3 0 108.29 11.50 5 2 0 10.50 4.00 -7 5 0 6.30 3.00 2 -7 0 10.40 4.20 5 2 0 17.60 5.50 5 2 0 14.90 3.90 -7 5 0 10.50 5.90 -2 7 0 10.20 5.70 -5 -2 0 9.10 3.50 -5 -2 0 13.10 5.70 7 -5 0 10.40 3.40 -7 6 0 11.40 6.00 -7 6 0 10.80 3.10 1 -7 0 18.90 5.20 6 1 0 15.70 4.10 6 1 0 15.00 4.80 6 1 0 12.90 5.60 -7 6 0 7.70 7.80 -1 7 0 12.50 6.70 -6 -1 0 18.00 4.70 7 -6 0 12.50 6.20 7 -6 0 19.00 4.30 0 -7 0 67.09 9.70 7 0 0 58.89 8.10 -7 7 0 64.49 11.40 7 0 0 60.49 8.50 7 -7 0 69.39 8.70 0 7 0 73.29 12.90 1 7 0 47.60 11.80 7 -8 0 52.39 8.30 8 -1 0 53.29 7.70 -7 8 0 53.59 11.30 -1 -7 0 57.39 11.00 6 -8 0 29.40 6.30 2 6 0 26.90 8.30 -6 8 0 27.10 9.00 -2 -6 0 19.70 6.60 8 -2 0 16.30 4.30 3 5 0 -4.70 5.50 5 -8 0 -3.10 2.70 -3 -5 0 -4.60 7.10 8 -3 0 -1.90 2.60 -5 8 0 -8.60 6.00 -3 -5 0 0.60 3.40 4 4 0 2686.53 197.58 4 -8 0 2682.53 196.08 -4 -4 0 2835.12 196.68 -4 8 0 2830.12 198.28 8 -4 0 2862.71 194.48 3 -8 0 2.60 4.10 -8 5 0 15.20 6.80 -3 8 0 13.80 6.60 6 2 0 15.10 4.90 2 -8 0 20.60 5.70 -8 6 0 11.40 6.80 -2 8 0 25.90 8.80 8 -6 0 8.60 4.50 -6 -2 0 20.10 5.60 -8 7 0 38.00 10.30 1 -8 0 49.90 11.90 7 1 0 54.09 7.80 8 -7 0 51.39 8.20 -7 -1 0 57.39 8.40 0 -8 0 2.90 5.20 -8 8 0 -5.90 8.30 8 0 0 13.30 4.80 8 -8 0 10.20 5.00 8 -9 0 0.50 6.50 1 8 0 5.10 9.20 -1 -8 0 1.20 5.30 -8 9 0 7.80 13.00 2 7 0 138.09 21.20 7 -9 0 101.89 13.70 -2 -7 0 122.09 15.10 6 -9 0 57.69 11.10 3 6 0 84.99 15.00 -3 -6 0 84.99 15.10 4 5 0 22.30 8.80 -5 9 0 37.90 14.90 4 -9 0 13.30 9.10 -4 9 0 26.90 9.60 9 -5 0 7.80 6.20 -5 -4 0 18.20 6.30 3 -9 0 71.39 10.50 6 3 0 75.09 9.40 9 -6 0 52.89 9.10 -3 9 0 45.30 12.00 -6 -3 0 73.49 10.10 2 -9 0 113.79 14.70 7 2 0 122.39 13.20 -7 -2 0 107.89 13.40 -2 9 0 129.69 19.10 9 -7 0 128.49 15.10 8 1 0 8.10 4.00 -9 8 0 11.80 9.80 1 -9 0 -1.20 5.90 -8 -1 0 1.30 4.20 9 -8 0 1.60 6.00 -1 9 0 -10.70 10.60 0 -9 0 283.37 27.60 -9 9 0 252.57 31.60 0 9 0 307.57 34.40 1 9 0 -0.40 13.30 -1 -9 0 -0.90 8.10 -9 10 0 6.40 13.40 8 -10 0 -1.30 5.40 2 8 0 1.80 9.90 -8 10 0 -3.80 10.70 -2 -8 0 -6.10 5.80 7 -10 0 4.50 5.00 -3 -7 0 -4.80 5.70 -7 10 0 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7.90 0 4 -14 7.60 4.70 4 0 14 16.60 12.90 -4 4 14 24.10 15.10 1 3 -14 44.80 9.90 1 3 -14 36.50 7.90 -3 4 14 42.20 13.70 -1 -3 14 39.60 12.00 4 -1 14 44.50 15.00 2 2 -14 287.77 25.10 2 -4 -14 277.97 24.70 4 -2 14 303.47 35.80 -2 4 14 273.77 31.70 3 1 -14 30.40 9.50 1 -4 -14 35.80 6.40 4 -3 14 40.60 14.80 -4 4 -14 19.80 12.10 4 0 -14 2.40 5.10 0 -4 -14 3.40 4.40 0 4 14 -6.00 11.60 4 -4 14 20.30 12.90 5 -1 -14 86.89 12.50 -4 5 -14 77.09 18.00 4 -5 14 64.59 17.80 1 4 14 108.49 22.20 6 -2 -14 32.60 8.80 -4 6 -14 45.40 15.10 4 -6 14 32.00 16.10 2 4 14 26.10 18.30 7 -3 -14 61.49 11.40 -4 7 -14 49.70 16.00 3 4 14 74.79 23.20 7 -5 -14 27.90 8.30 -2 7 -14 -4.40 11.40 5 2 14 6.40 19.30 -1 6 -14 3.40 9.00 6 -5 -14 -2.70 6.10 5 1 14 -4.90 18.00 5 -5 -14 16.10 6.40 5 0 14 25.00 15.30 0 -5 14 25.80 9.90 1 4 -14 60.59 12.40 4 -5 -14 101.39 12.40 5 -1 14 119.89 26.60 -4 5 14 93.09 19.20 2 3 -14 13.20 5.90 3 -5 -14 1.50 5.20 5 -2 14 6.40 13.40 3 2 -14 10.00 5.40 5 -3 14 3.50 13.20 -2 5 14 1.30 11.80 -5 4 -14 95.39 19.00 1 -5 -14 59.99 12.80 4 1 -14 65.09 11.30 5 -4 14 97.59 21.50 -1 5 14 88.29 18.10 5 0 -14 12.00 5.80 -5 5 -14 4.80 12.60 0 -5 -14 12.50 5.30 0 5 14 14.30 13.10 5 -5 14 15.40 15.10 -5 6 -14 10.20 13.80 6 -1 -14 4.40 5.70 5 -6 14 10.20 15.40 1 5 14 -3.40 13.80 -5 7 -14 35.90 17.40 2 5 14 34.80 19.10 -1 7 -14 -12.40 10.40 7 -6 -14 1.10 6.70 6 1 14 22.10 22.20 6 -6 -14 120.69 15.60 0 6 -14 100.99 13.80 6 0 14 127.79 31.80 0 -6 14 98.19 15.10 5 -6 -14 14.20 6.50 -1 -5 14 -7.40 6.60 6 -1 14 10.70 18.40 2 4 -14 29.80 7.70 4 -6 -14 44.80 9.80 6 -2 14 6.60 17.60 3 3 -14 9.70 5.80 3 -6 -14 -5.70 4.60 6 -3 14 -11.90 13.40 -3 6 14 28.10 13.50 4 2 -14 32.90 8.40 -6 4 -14 39.10 17.10 2 -6 -14 33.30 7.60 6 -4 14 23.40 17.90 -2 6 14 50.09 16.00 1 -6 -14 10.80 5.50 5 1 -14 2.80 5.60 -6 5 -14 22.00 14.70 6 -5 14 -13.20 15.40 -1 6 14 8.80 14.20 0 -6 -14 93.49 13.10 6 0 -14 96.09 14.50 -6 6 -14 148.99 24.00 0 6 14 101.89 23.30 6 -6 14 106.39 23.60 -6 7 -14 4.60 19.90 7 -1 -14 -14.60 6.30 1 6 14 0.60 18.90 6 -7 -14 -0.30 6.80 1 6 -14 6.80 6.80 -1 -6 14 0.40 8.40 7 -1 14 19.70 19.40 5 -7 -14 21.80 7.90 2 5 -14 17.40 7.20 -2 -5 14 10.00 8.10 7 -2 14 26.30 19.50 3 4 -14 65.39 12.80 4 -7 -14 81.49 13.40 7 -3 14 66.79 24.30 -4 7 14 83.69 19.20 -7 4 -14 49.40 20.50 3 -7 -14 61.19 11.10 4 3 -14 55.29 11.60 7 -4 14 68.19 22.70 -3 7 14 100.29 19.70 5 2 -14 17.10 7.50 -7 5 -14 25.40 17.00 2 -7 -14 33.70 7.90 -2 7 14 36.70 17.30 7 -5 14 17.00 20.00 -7 6 -14 -9.00 18.90 1 -7 -14 1.10 6.20 6 1 -14 8.50 6.90 7 -6 14 47.10 25.90 -1 7 14 5.60 16.60 0 0 -15 3.10 3.50 0 0 15 13.30 10.60 0 1 -15 127.49 13.10 1 -1 -15 131.89 13.50 0 -1 15 114.89 21.70 -1 1 15 138.19 22.20 1 0 15 143.09 28.20 0 -1 -15 125.89 12.50 1 0 -15 123.79 13.00 1 -1 15 116.09 21.50 0 1 15 138.89 22.70 -1 0 15 92.49 17.80 2 -1 -15 3.40 4.10 -2 1 15 -3.20 9.40 1 -2 15 10.70 9.70 -3 2 15 4.60 14.00 2 1 15 25.70 12.80 2 -2 -15 58.09 8.70 0 2 -15 54.29 8.40 0 2 -15 30.50 12.20 0 -2 15 44.50 12.70 -2 2 15 34.30 13.60 2 0 15 43.80 24.60 1 1 -15 -1.80 3.90 1 -2 -15 7.00 4.10 -1 -1 15 10.50 8.80 -1 2 15 12.50 11.70 0 -2 -15 49.90 7.50 2 0 -15 51.89 9.30 -2 0 15 35.80 12.10 -2 3 -15 7.30 16.00 3 -1 -15 4.70 7.60 1 2 15 20.90 13.60 4 -2 -15 11.00 5.30 -2 4 -15 -2.50 10.00 2 2 15 7.40 12.70 2 -4 15 6.80 12.20 -2 5 -15 41.30 13.40 5 -3 -15 54.39 10.30 2 -5 15 23.60 14.70 3 2 15 58.89 21.40 4 -3 -15 48.20 9.40 3 1 15 41.20 18.50 0 3 -15 17.30 9.00 3 -3 -15 7.10 6.40 0 3 -15 -0.40 4.20 3 0 15 3.40 11.60 0 -3 15 5.10 10.30 -3 3 15 29.30 12.30 1 2 -15 3.20 8.80 2 -3 -15 14.50 5.50 1 2 -15 12.00 5.50 3 -1 15 32.70 14.20 -1 -2 15 32.00 10.70 -2 3 15 -1.20 10.80 1 -3 -15 11.20 4.50 2 1 -15 13.30 5.10 2 1 -15 10.60 12.60 3 -2 15 18.20 12.20 0 -3 -15 9.30 4.30 -3 3 -15 22.10 12.00 3 -3 15 -1.90 12.00 0 3 15 26.00 12.90 -3 4 -15 36.90 14.10 4 -1 -15 41.00 8.50 3 -4 15 47.20 15.50 1 3 15 43.00 17.50 5 -2 -15 52.39 10.30 -3 5 -15 64.19 15.70 2 3 15 72.59 21.30 3 -5 15 40.20 16.60 6 -3 -15 -5.20 5.10 -3 6 -15 -11.00 11.40 3 3 15 16.30 16.40 7 -4 -15 184.08 28.60 -3 7 -15 164.38 26.30 -2 6 -15 -3.00 11.90 6 -4 -15 19.30 8.50 4 2 15 16.10 19.10 -1 5 -15 82.39 16.40 5 -4 -15 113.49 15.50 4 1 15 152.48 29.90 4 -4 -15 191.08 19.40 0 4 -15 170.18 17.90 4 0 15 216.88 31.40 1 3 -15 47.20 9.80 3 -4 -15 30.40 7.30 -1 -3 15 23.10 14.90 4 -1 15 63.19 18.20 -3 4 15 50.49 15.00 2 -4 -15 6.80 6.40 4 -2 15 -20.40 11.60 1 -4 -15 34.50 6.90 3 1 -15 43.80 8.70 4 -3 15 35.50 16.70 -1 4 15 19.40 14.50 4 0 -15 194.68 19.50 -4 4 -15 185.18 26.60 0 -4 -15 160.18 17.00 4 -4 15 218.28 32.20 0 4 15 156.38 28.00 5 -1 -15 136.99 15.70 -4 5 -15 149.59 23.90 1 4 15 119.89 23.80 4 -5 15 80.89 21.20 -4 6 -15 23.70 15.60 6 -2 -15 16.30 7.60 4 -6 15 -3.80 16.60 2 4 15 32.60 18.10 -4 7 -15 174.28 29.30 7 -3 -15 180.18 27.70 -2 7 -15 34.70 14.30 -1 6 -15 -4.20 10.00 6 -5 -15 -10.20 5.90 5 1 15 19.40 20.60 0 5 -15 13.20 10.00 5 -5 -15 17.20 8.30 0 5 -15 25.50 7.00 0 -5 15 18.20 7.20 5 0 15 62.29 20.20 4 -5 -15 100.89 15.10 1 4 -15 131.69 14.00 5 -1 15 105.09 27.30 2 3 -15 59.29 10.30 3 -5 -15 58.59 9.80 5 -2 15 40.60 18.60 -3 5 15 49.20 17.90 3 2 -15 41.70 8.60 2 -5 -15 47.20 8.70 -2 5 15 26.90 14.80 5 -3 15 41.10 18.30 -5 4 -15 107.09 22.10 4 1 -15 106.79 14.00 1 -5 -15 109.89 14.40 5 -4 15 98.59 24.70 -1 5 15 94.19 20.90 -5 5 -15 49.80 15.60 5 0 -15 31.70 8.40 0 5 15 12.00 14.50 5 -5 15 13.20 17.60 6 -1 -15 0.40 5.60 -5 6 -15 -2.40 14.60 1 5 15 18.00 16.20 5 -6 15 1.40 16.30 7 -2 -15 53.59 16.20 0 6 -15 4.60 5.70 6 -6 -15 -2.60 6.90 6 0 15 -12.50 18.70 0 -6 15 -7.50 8.00 6 -1 15 13.90 19.40 4 -6 -15 31.50 8.60 6 -2 15 15.30 19.60 -4 6 15 31.10 17.20 3 -6 -15 0.70 5.10 3 3 -15 5.80 5.30 6 -3 15 -5.90 15.80 4 2 -15 28.90 7.70 -6 4 -15 20.70 16.60 2 -6 -15 25.20 6.80 -2 6 15 29.30 15.50 6 -4 15 23.80 18.70 5 1 -15 11.00 6.40 1 -6 -15 2.20 5.30 -6 5 -15 2.80 15.30 -1 6 15 7.90 14.10 6 -5 15 -5.00 17.10 -6 6 -15 -11.20 23.20 6 0 -15 -3.90 5.50 0 6 15 -0.30 18.10 5 -7 -15 38.70 10.00 2 5 -15 31.50 8.80 -2 -5 15 24.20 9.80 3 4 -15 159.28 19.70 4 -7 -15 204.78 21.80 -4 7 15 198.18 32.50 -7 4 -15 161.28 33.70 4 3 -15 175.58 20.30 3 -7 -15 185.78 20.10 -3 7 15 153.88 29.20 2 -7 -15 25.40 8.60 -2 7 15 55.99 20.00 0 0 -16 359.76 31.70 1 -1 -16 62.29 10.40 0 1 -16 64.59 10.30 1 0 16 111.59 23.10 0 -1 16 76.19 18.20 -1 1 16 89.59 18.80 1 0 -16 63.69 10.10 -1 0 16 52.69 15.30 2 -1 -16 8.80 4.90 -2 1 16 13.10 10.60 1 1 16 21.00 12.90 3 -2 -16 3.80 5.00 -1 3 -16 13.30 9.80 1 -3 16 16.30 13.00 2 1 16 -12.90 13.00 0 2 -16 135.19 28.70 0 2 -16 212.38 20.70 2 -2 -16 209.78 22.60 2 0 16 227.98 32.00 -2 2 16 226.28 29.40 0 -2 16 197.98 33.90 1 -2 -16 11.80 5.10 1 1 -16 15.80 5.10 -1 -1 16 1.00 10.00 2 -1 16 4.30 12.60 2 0 -16 227.08 26.80 0 2 16 204.78 29.80 2 -2 16 165.48 29.10 3 -1 -16 1.40 4.50 2 -3 16 -0.70 12.80 1 2 16 -22.70 12.50 -2 4 -16 -6.30 10.80 4 -2 -16 6.30 5.20 2 -4 16 0.90 14.40 2 2 16 38.20 17.30 -2 5 -16 27.80 13.60 5 -3 -16 47.80 10.20 3 2 16 35.30 20.50 2 -5 16 14.00 15.90 4 -3 -16 17.10 6.00 3 1 16 22.30 16.80 1 -4 16 10.60 12.40 3 -3 -16 23.20 7.00 0 3 -16 17.00 6.60 3 0 16 17.40 13.80 2 -3 -16 1.30 6.00 1 2 -16 -5.90 4.20 1 2 -16 8.20 9.30 -1 -2 16 0.10 10.90 3 -1 16 10.20 13.50 1 -3 -16 -5.70 4.00 -1 3 16 -0.40 11.90 3 -2 16 -0.80 13.60 3 0 -16 26.50 6.80 -3 3 -16 19.40 13.50 3 -3 16 0.60 14.00 0 3 16 1.20 12.90 -3 4 -16 16.40 13.70 4 -1 -16 19.20 6.80 3 -4 16 -1.20 14.30 1 3 16 21.30 16.10 5 -2 -16 35.50 8.80 -3 5 -16 46.60 16.90 2 3 16 34.30 19.10 3 -5 16 27.10 16.20 -3 6 -16 11.80 13.90 6 -3 -16 7.80 6.90 3 3 16 4.30 20.20 6 -4 -16 95.59 14.90 -2 6 -16 96.39 19.20 -1 5 -16 16.40 11.00 5 -4 -16 7.80 7.30 4 1 16 44.40 21.00 4 -4 -16 288.67 25.70 0 4 -16 222.48 29.00 4 0 16 294.87 39.40 0 -4 16 283.07 34.70 1 3 -16 10.40 5.30 3 -4 -16 9.10 5.80 4 -1 16 9.70 16.40 2 -4 -16 14.30 5.50 2 2 -16 9.80 5.40 -2 4 16 24.30 14.30 4 -2 16 -16.40 14.30 -4 3 -16 -3.90 13.80 3 1 -16 4.80 5.50 1 -4 -16 6.00 6.90 4 -3 16 20.90 16.00 -1 4 16 13.50 14.90 4 0 -16 269.37 24.70 -4 4 -16 227.48 32.50 0 4 16 263.57 36.00 4 -4 16 226.88 36.70 -4 5 -16 7.80 15.30 5 -1 -16 14.40 6.50 1 4 16 -1.10 16.60 4 -5 16 -0.20 16.30 6 -2 -16 94.79 14.70 -4 6 -16 107.59 22.30 4 -6 16 61.99 22.20 -1 6 -16 -9.30 11.40 5 -5 -16 -0.20 6.20 5 0 16 -2.50 18.00 1 4 -16 20.90 6.90 4 -5 -16 21.00 7.30 5 -1 16 4.60 18.80 2 3 -16 43.00 8.80 3 -5 -16 33.80 8.30 -3 5 16 38.40 16.90 5 -2 16 70.09 21.70 2 -5 -16 23.50 6.80 3 2 -16 36.80 8.30 -2 5 16 22.50 16.40 5 -3 16 35.90 18.80 -5 4 -16 -10.40 15.30 1 -5 -16 8.70 5.80 4 1 -16 17.10 7.60 5 -4 16 18.10 18.10 -1 5 16 15.10 16.20 -5 5 -16 -2.00 14.10 5 0 -16 13.90 7.40 0 5 16 -3.70 15.90 5 -5 16 22.00 18.90 1 5 -16 -8.30 4.80 5 -6 -16 0.40 7.20 4 -6 -16 70.49 12.60 2 4 -16 98.99 14.20 6 -2 16 138.19 35.30 3 3 -16 9.80 6.20 3 -6 -16 3.50 6.20 -3 6 16 33.20 18.20 6 -3 16 -28.20 18.20 2 -6 -16 104.09 13.00 4 2 -16 74.09 12.40 6 -4 16 54.39 29.10 -2 6 16 67.09 20.80 5 1 -16 3.10 7.80 -1 6 16 -13.50 16.60 6 -5 16 -15.70 28.70 0 0 17 12.70 12.90 1 -1 -17 25.90 6.80 1 0 17 19.70 16.00 0 -1 17 -7.40 14.20 1 0 -17 27.60 7.10 1 -1 17 27.10 15.30 0 1 17 26.90 15.00 2 -1 -17 7.40 7.60 1 -2 17 8.00 12.30 1 1 17 -16.80 13.00 3 -2 -17 -3.30 5.90 -1 3 -17 -19.40 11.00 1 -3 17 -26.10 13.10 2 1 17 9.10 17.30 2 -2 -17 87.79 13.40 0 2 -17 107.79 19.40 0 -2 17 69.79 18.30 2 0 17 101.49 25.60 1 1 -17 13.40 7.00 1 -2 -17 9.30 5.90 -1 2 17 5.40 13.40 2 -1 17 -3.90 13.80 2 0 -17 86.89 11.70 2 -2 17 82.39 21.40 0 2 17 81.39 23.20 3 -1 -17 2.40 6.20 -2 3 -17 11.40 13.00 2 -3 17 4.90 15.20 1 2 17 4.40 16.70 4 -2 -17 -8.30 4.90 -2 4 -17 -21.70 12.50 2 2 17 -7.10 16.90 2 -4 17 16.90 16.10 5 -3 -17 21.50 7.90 -2 5 -17 12.40 14.10 3 2 17 41.40 28.80 2 -5 17 -26.00 17.30 -1 4 -17 -3.30 11.00 1 -4 17 8.10 14.70 3 1 17 15.20 18.40 3 -3 -17 16.60 6.70 3 0 17 15.20 17.90 0 -3 17 38.90 14.30 1 2 -17 -1.80 8.50 2 -3 -17 7.40 5.40 -2 3 17 19.30 15.80 3 -1 17 -5.20 16.50 2 1 -17 9.80 5.80 3 -2 17 3.10 16.20 -1 3 17 1.40 15.90 3 0 -17 8.10 5.70 -3 3 -17 -3.30 13.20 0 3 17 17.40 16.50 3 -3 17 21.40 17.00 4 -1 -17 -2.40 5.70 -3 4 -17 2.70 13.50 1 3 17 -22.70 15.20 3 -4 17 9.60 16.10 5 -2 -17 17.30 7.70 -3 5 -17 26.10 15.90 3 -5 17 8.90 17.00 2 3 17 4.00 19.30 5 -4 -17 81.09 13.50 -1 5 -17 61.99 16.80 4 -4 -17 45.70 10.50 4 0 17 84.29 24.10 1 3 -17 -7.00 5.20 3 -4 -17 4.30 5.70 4 -1 17 -12.80 16.30 2 -4 -17 0.70 4.80 2 2 -17 -9.70 5.40 -2 4 17 15.10 15.70 4 -2 17 9.50 17.20 -4 3 -17 -26.90 14.40 3 1 -17 -4.80 5.50 -1 4 17 15.60 17.10 4 -3 17 0.70 17.10 4 0 -17 63.59 11.40 -4 4 -17 60.69 19.70 4 -4 17 54.49 21.10 0 4 17 75.59 22.60 -4 5 -17 58.79 22.10 5 -1 -17 69.89 12.70 1 4 17 110.49 30.10 4 -5 17 43.00 21.20 1 4 -17 51.19 11.20 4 -5 -17 50.29 10.40 3 -5 -17 21.30 7.20 2 3 -17 10.90 6.60 5 -2 17 -5.70 21.60 -3 5 17 -31.60 20.40 3 2 -17 9.00 6.70 2 -5 -17 9.50 6.60 -2 5 17 -2.50 17.90 5 -3 17 -4.30 22.60 4 1 -17 60.49 11.30 -1 5 17 83.19 22.80 0 0 18 178.98 33.30 0 -1 18 -5.20 13.60 1 0 18 11.20 15.10 -1 1 18 16.50 15.00 0 1 18 7.20 16.20 1 -1 18 -14.50 14.90 -1 0 18 35.20 16.70 2 -1 -18 18.00 7.30 -1 2 -18 7.20 13.20 1 1 18 23.90 18.20 1 -2 18 0.00 15.60 -1 3 -18 35.60 14.00 2 1 18 3.90 18.40 1 -3 18 29.30 19.50 2 -2 -18 28.60 8.70 0 2 -18 36.50 14.80 0 -2 18 10.60 16.80 2 0 18 52.19 21.50 2 -1 18 26.40 18.20 -1 2 18 25.10 18.80 2 0 -18 23.20 7.50 0 2 18 83.49 22.60 2 -2 18 27.00 18.60 3 -1 -18 7.70 6.10 -2 3 -18 0.50 13.50 2 -3 18 -10.20 16.80 1 2 18 14.20 19.20 4 -2 -18 236.88 22.90 -2 4 -18 206.48 29.80 2 2 18 257.57 44.60 2 -4 18 171.08 31.90 4 -3 -18 49.50 9.80 -1 4 -18 24.70 15.00 1 -4 18 57.19 20.30 3 -3 -18 18.00 7.20 0 3 -18 15.00 17.90 3 0 18 12.30 19.70 2 -3 -18 9.30 6.20 -2 3 18 -8.60 20.40 3 -1 18 4.50 18.70 2 1 -18 7.50 6.10 3 -2 18 27.30 19.70 -1 3 18 24.60 19.90 -3 3 -18 32.30 16.10 3 0 -18 16.40 6.70 3 -3 18 20.70 18.00 0 3 18 11.00 18.90 4 -1 -18 44.60 9.50 -3 4 -18 11.80 15.50 3 -4 18 36.90 21.40 1 3 18 -14.70 20.90 3 -4 -18 23.80 7.70 2 2 -18 209.18 23.70 2 -4 -18 283.87 32.80 -2 4 18 323.37 40.30 3 1 -18 40.50 9.20 -1 4 18 16.70 19.30 0 0 19 29.90 20.10 1 0 19 18.10 20.10 -1 1 19 16.10 23.40 0 -1 19 55.09 21.70 1 -1 19 12.00 20.40 0 1 19 57.69 23.60 -1 2 -19 29.50 14.70 1 -2 19 5.20 20.20 1 1 19 17.40 19.60 2 0 19 22.80 21.40 -1 2 19 55.69 21.30 2 -1 19 19.40 20.30 0 2 19 52.89 24.70 2 -2 19 34.70 21.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 82509 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' 'y, x, z+1/2' '-x+y, y, z' '-x, -x+y, z+1/2' '-y, -x, z' 'x-y, -y, z+1/2' 'x, x-y, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S -0.51503(12) -1.0301(2) 0.35353(15) 0.0155(6) Uani 1 2 d S T P . . N1 N -0.4922(10) -0.7461(5) 0.3427(5) 0.0142(18) Uani 1 2 d S T P . . H1 H -0.597151 -0.798575 0.338467 0.017 Uiso 1 2 calc R U P . . C1 C -0.4153(5) -0.8306(10) 0.3458(6) 0.013(2) Uiso 1 2 d S . P . . S2 S -0.3028(2) -0.15138(12) 0.64022(15) 0.0153(6) Uani 1 2 d S T P . . N2 N -0.5864(5) -0.4136(5) 0.6488(6) 0.0100(17) Uani 1 2 d S T P . . H2 H -0.533834 -0.466168 0.650668 0.012 Uiso 1 2 calc R U P . . C2 C -0.5000(10) -0.2500(5) 0.6474(6) 0.012(2) Uiso 1 2 d S . P . . N3 N -0.8331(9) -0.9165(4) 0.3597(5) 0.0129(17) Uani 1 2 d S T P . . N5 N -1.000000 -1.000000 0.4813(7) 0.011(3) Uani 1 6 d S T P . . C3 C -0.9169(7) -0.8339(14) 0.3301(6) 0.015(2) Uani 1 2 d S T P . . H3A H -0.860913 -0.721826 0.349543 0.018 Uiso 1 2 calc R U P . . H3B H -0.916197 -0.832397 0.269837 0.018 Uiso 1 2 calc R U P . . C4 C -0.8366(12) -0.9183(6) 0.4510(5) 0.014(2) Uani 1 2 d S T P . . H4A H -0.780022 -0.972986 0.471631 0.017 Uiso 0.5 1 calc R U P . . H4B H -0.780022 -0.807036 0.471631 0.017 Uiso 0.5 1 calc R U P . . N4 N -0.4175(4) -0.5825(4) 0.6428(5) 0.0104(15) Uani 1 2 d S T P . . N6 N -0.333333 -0.666667 0.5211(7) 0.015(3) Uani 1 6 d S T P . . C5 C -0.4148(7) -0.5852(7) 0.5517(5) 0.014(2) Uani 1 2 d S T P . . H5A H -0.525966 -0.639861 0.531026 0.017 Uiso 0.5 1 calc R U P . . H5B H -0.360139 -0.474034 0.531026 0.017 Uiso 0.5 1 calc R U P . . C6 C -0.2500(6) -0.4999(12) 0.6724(5) 0.011(2) Uani 1 2 d S T P . . H6A H -0.249183 -0.498368 0.732584 0.014 Uiso 1 2 calc R U P . . H6B H -0.193940 -0.387880 0.652905 0.014 Uiso 1 2 calc R U P . . 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 0.0150(9) 0.0116(11) 0.0188(11) -0.0018(12) -0.0009(6) 0.0058(6) N1 0.018(4) 0.016(3) 0.009(4) 0.0014(19) 0.003(4) 0.009(2) S2 0.0126(12) 0.0151(9) 0.0175(10) 0.0003(6) 0.0006(12) 0.0063(6) N2 0.013(3) 0.013(3) 0.006(4) 0.001(2) -0.001(2) 0.007(3) N3 0.012(4) 0.014(3) 0.011(4) 0.000(2) 0.000(4) 0.0062(19) N5 0.013(4) 0.013(4) 0.006(7) 0.000 0.000 0.0066(19) C3 0.015(4) 0.020(6) 0.010(5) 0.001(4) 0.000(2) 0.010(3) C4 0.014(5) 0.019(4) 0.008(5) -0.003(2) -0.007(4) 0.007(3) N4 0.011(3) 0.011(3) 0.010(3) 0.000(2) 0.000(2) 0.006(3) N6 0.021(4) 0.021(4) 0.002(6) 0.000 0.000 0.011(2) C5 0.016(4) 0.016(4) 0.005(4) 0.002(2) -0.002(2) 0.005(4) C6 0.011(4) 0.010(5) 0.013(4) 0.003(4) 0.0016(19) 0.005(3) 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' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 H1 118.5 5_545 . ? C1 N1 H1 118.5 . . ? C1 N1 C1 123.0(9) . 5_545 ? N1 C1 S1 121.6(4) . . ? N1 C1 S1 121.6(4) 3_445 . ? N1 C1 N1 116.8(9) 3_445 . ? C2 N2 H2 118.1 5_445 . ? C2 N2 H2 118.1 . . ? C2 N2 C2 123.7(9) . 5_445 ? N2 C2 S2 121.9(4) . . ? N2 C2 S2 121.9(4) 3_455 . ? N2 C2 N2 116.2(9) . 3_455 ? C3 N3 C3 109.2(10) 5_435 . ? C3 N3 C4 108.7(5) 5_435 . ? C3 N3 C4 108.7(5) . . ? C4 N5 C4 108.9(6) 5_435 3_345 ? C4 N5 C4 108.9(6) . 5_435 ? C4 N5 C4 108.9(6) . 3_345 ? N3 C3 N3 110.0(9) 3_345 . ? N3 C3 H3A 109.7 3_345 . ? N3 C3 H3A 109.7 . . ? N3 C3 H3B 109.7 3_345 . ? N3 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? N3 C4 H4A 109.4 . . ? N3 C4 H4B 109.4 . . ? N5 C4 N3 111.2(8) . . ? N5 C4 H4A 109.4 . . ? N5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 N4 C5 108.2(5) . . ? C6 N4 C5 108.2(5) 3_445 . ? C6 N4 C6 109.0(9) . 3_445 ? C5 N6 C5 108.6(6) 5_545 . ? C5 N6 C5 108.6(6) 5_545 3_445 ? C5 N6 C5 108.6(6) 3_445 . ? N4 C5 H5A 109.2 . . ? N4 C5 H5B 109.2 . . ? N6 C5 N4 112.1(8) . . ? N6 C5 H5A 109.2 . . ? N6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? N4 C6 N4 110.6(9) . 5_545 ? N4 C6 H6A 109.5 . . ? N4 C6 H6A 109.5 5_545 . ? N4 C6 H6B 109.5 . . ? N4 C6 H6B 109.5 5_545 . ? H6A C6 H6B 108.1 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.672(9) . ? N1 H1 0.8800 . ? N1 C1 1.351(6) 5_545 ? N1 C1 1.351(6) . ? S2 C2 1.653(9) . ? N2 H2 0.8800 . ? N2 C2 1.369(6) . ? N2 C2 1.369(6) 5_445 ? N3 C3 1.475(7) 5_435 ? N3 C3 1.475(7) . ? N3 C4 1.502(13) . ? N5 C4 1.454(10) . ? N5 C4 1.454(10) 5_435 ? N5 C4 1.454(10) 3_345 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N4 C5 1.497(12) . ? N4 C6 1.483(7) 3_445 ? N4 C6 1.483(7) . ? N6 C5 1.452(11) 3_445 ? N6 C5 1.452(11) 5_545 ? N6 C5 1.452(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1 N3 0.88 2.00 2.863(11) 165.5 . yes N2 H2 N4 0.88 1.95 2.825(10) 174.1 . yes C3 H3A S1 0.99 2.96 3.671(9) 129.8 5_545 yes C3 H3A S1 0.99 2.96 3.671(9) 129.8 3_345 yes C6 H6B S2 0.99 2.96 3.685(8) 130.9 . yes C6 H6B S2 0.99 2.96 3.685(8) 130.9 3 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 N1 C1 S1 172.2(5) 5_545 . . . ? C1 N1 C1 N1 -7(2) 5_545 . . 3_445 ? C2 N2 C2 S2 -174.0(6) 5_445 . . . ? C2 N2 C2 N2 3(2) 5_445 . . 3_455 ? C3 N3 C3 N3 59.6(11) 5_435 . . 3_345 ? C3 N3 C4 N5 -59.4(5) 5_435 . . . ? C3 N3 C4 N5 59.4(5) . . . . ? C4 N3 C3 N3 -58.9(9) . . . 3_345 ? C4 N5 C4 N3 59.3(7) 5_435 . . . ? C4 N5 C4 N3 -59.3(7) 3_345 . . . ? C5 N4 C6 N4 -58.3(9) . . . 5_545 ? C5 N6 C5 N4 -59.0(7) 5_545 . . . ? C5 N6 C5 N4 59.0(7) 3_445 . . . ? C6 N4 C5 N6 -59.0(5) 3_445 . . . ? C6 N4 C5 N6 59.0(5) . . . . ? C6 N4 C6 N4 59.2(11) 3_445 . . 5_545 ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 1.0(4) 2 -0.0(4)