#------------------------------------------------------------------------------ #$Date: 2025-01-18 01:05:02 +0200 (Sat, 18 Jan 2025) $ #$Revision: 297368 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/37/1573710.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_1573710 _journal_paper_doi 10.1039/D4SC08530B _chemical_formula_moiety 'C12 H11 N3 S2' _chemical_formula_sum 'C12 H11 N3 S2' _chemical_formula_weight 261.36 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method ;FinalCif V137 by Daniel Kratzert, Freiburg 2024, https://dkratzert.de/finalcif.html ; _audit_update_record ; 2024-05-24 deposited with the CCDC. 2025-01-09 downloaded from the CCDC. ; _cell_angle_alpha 71.163(6) _cell_angle_beta 82.543(10) _cell_angle_gamma 87.953(18) _cell_formula_units_Z 2 _cell_length_a 5.689(2) _cell_length_b 10.012(3) _cell_length_c 11.393(4) _cell_measurement_reflns_used 9904 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 31.511 _cell_measurement_theta_min 2.37 _cell_volume 609.0(4) _computing_cell_refinement 'SAINT V8.40B' _computing_data_collection 'Bruker BIS 2018.9.0.3/05-Dec-2018 and APEX5_2023.9-2' _computing_data_reduction 'SAINT V8.40B' _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector CCD _diffrn_detector_area_resol_mean 8.3 _diffrn_detector_type 'Bruker APEXII' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker APEX2 QUAZAR' _diffrn_measurement_method '\w and \f scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_unetI/netI 0.0159 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 30288 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.556 _diffrn_reflns_theta_min 1.903 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_current 0.6 _diffrn_source_type 'Incoatec I\ms' _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 0.416 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_correction_T_min 0.6912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ;SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.425 _exptl_crystal_description block _exptl_crystal_F_000 272 _exptl_crystal_recrystallization_method 'Crystals were obtained at room temperature from a mixture of dichloromethane and ethanol by slow solvent evaporation.' _exptl_crystal_size_max 0.709 _exptl_crystal_size_mid 0.531 _exptl_crystal_size_min 0.235 _refine_diff_density_max 0.444 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.049 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 197 _refine_ls_number_reflns 4060 _refine_ls_number_restraints 208 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0271 _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^)+(0.0409P)^2^+0.1792P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.0762 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3731 _reflns_number_total 4060 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc08530b2.cif _cod_data_source_block Eisenreich_TSC_19_a _cod_database_code 1573710 _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. ; _shelx_estimated_absorpt_t_min 0.757 _shelx_estimated_absorpt_t_max 0.909 _olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800' _shelx_res_file ; TITL Eisenreich_TSC_19_a.res in P-1 Eisenreich_TSC_19_a.res created by SHELXL-2019/3 at 11:59:46 on 12-May-2024 REM Old TITL Eisenreich_TSC_19 in P-1 REM SHELXT solution in P-1: R1 0.091, Rweak 0.005, Alpha 0.038 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C11 N4 S2 CELL 0.71073 5.6891 10.0116 11.3934 71.163 82.543 87.953 ZERR 2.000 0.0020 0.0034 0.0040 0.006 0.010 0.018 LATT 1 SFAC C H N S UNIT 24 22 6 4 DFIX 0.90 N1 H1n DANG 1.81 C1 H1n DANG 1.87 C2 H1n DFIX 0.90 N2 H2n DANG 1.85 N3 H2n DANG 1.84 C1 H2n EADP C1_1 C1_2 EXYZ C1_1 C1_2 RIGU 0.002 0.002 S1_1 C1_1 C2_1 C3_1 C4_1 S1_2 C1_2 C2_2 C3_2 C4_2 SIMU 0.01 0.02 2 S1_1 C1_1 C2_1 C3_1 C4_1 S1_2 C1_2 C2_2 C3_2 C4_2 TEMP -173.150 SIZE 0.235 0.531 0.709 L.S. 10 BOND $H CONF MORE -1 HTAB LIST 4 ACTA FMAP 2 PLAN 20 WGHT 0.040900 0.179200 FVAR 1.38368 0.83138 S1 4 0.000260 0.382028 0.866119 11.00000 0.01465 0.01954 = 0.01802 -0.01044 0.00188 -0.00491 N1 3 0.442936 0.443708 0.745731 11.00000 0.01327 0.02028 = 0.01905 -0.01178 0.00030 -0.00382 REM HFIX R2N-H H1N 2 0.575391 0.484412 0.740404 11.00000 -1.20000 N2 3 0.311402 0.561795 0.881872 11.00000 0.01595 0.01655 = 0.01640 -0.00874 0.00148 -0.00466 REM HFIX R2N-H H2N 2 0.207447 0.574618 0.940404 11.00000 -1.20000 N3 3 0.513079 0.643343 0.838887 11.00000 0.01450 0.01452 = 0.01627 -0.00532 -0.00251 -0.00244 C1 1 0.265006 0.465803 0.826994 11.00000 0.01500 0.01317 = 0.01313 -0.00487 -0.00237 -0.00056 C2 1 0.435063 0.363174 0.663823 11.00000 0.01464 0.01566 = 0.01403 -0.00704 0.00059 -0.00278 C3 1 0.254128 0.380944 0.588548 11.00000 0.01617 0.01921 = 0.01521 -0.00724 -0.00132 0.00044 AFIX 43 H3 2 0.126170 0.442678 0.595451 11.00000 -1.20000 AFIX 0 C4 1 0.262702 0.307458 0.503262 11.00000 0.01967 0.02352 = 0.01531 -0.00855 -0.00256 -0.00115 AFIX 43 H4 2 0.138926 0.318514 0.452425 11.00000 -1.20000 AFIX 0 C5 1 0.450751 0.217879 0.491616 11.00000 0.02256 0.02202 = 0.01847 -0.01139 0.00099 -0.00262 AFIX 43 H5 2 0.455895 0.168549 0.432742 11.00000 -1.20000 AFIX 0 C6 1 0.631238 0.201014 0.566763 11.00000 0.01870 0.02230 = 0.02480 -0.01333 -0.00043 0.00165 AFIX 43 H6 2 0.759994 0.140044 0.559139 11.00000 -1.20000 AFIX 0 C7 1 0.623436 0.273422 0.653201 11.00000 0.01503 0.02138 = 0.02188 -0.01061 -0.00218 0.00037 AFIX 43 H7 2 0.746316 0.261538 0.704693 11.00000 -1.20000 AFIX 0 C8 1 0.536256 0.739935 0.888759 11.00000 0.01863 0.01656 = 0.01645 -0.00720 -0.00115 -0.00256 AFIX 43 H8 2 0.419760 0.749520 0.953221 11.00000 -1.20000 AFIX 0 RESI THIO 1 PART 1 21 S1 4 0.959508 0.821498 0.733008 21.00000 0.01790 0.02168 = 0.02182 -0.01038 0.00084 -0.00437 C1 1 0.739066 0.833681 0.846828 21.00000 0.01739 0.01494 = 0.01741 -0.00614 -0.00366 -0.00117 C2 1 0.791005 0.941737 0.891883 21.00000 0.02433 0.02527 = 0.03028 -0.01431 -0.00344 0.00131 AFIX 43 H2 2 0.692260 0.963742 0.956966 21.00000 -1.20000 AFIX 0 C3 1 1.002277 1.015285 0.832582 21.00000 0.02534 0.01625 = 0.03369 -0.01274 -0.00977 -0.00090 AFIX 43 H3 2 1.060160 1.093234 0.850910 21.00000 -1.20000 AFIX 0 C4 1 1.113442 0.960123 0.745233 21.00000 0.01924 0.01881 = 0.02918 -0.00486 -0.00518 -0.00631 AFIX 43 H4 2 1.260247 0.994640 0.696382 21.00000 -1.20000 PART 0 RESI 0 AFIX 0 RESI THIO 2 PART 2 -21 S1 4 0.763544 0.967835 0.897176 -21.00000 0.02035 0.02088 = 0.02687 -0.01351 -0.00071 -0.00263 C1 1 0.739066 0.833681 0.846828 -21.00000 0.01739 0.01494 = 0.01741 -0.00614 -0.00366 -0.00117 C2 1 0.927693 0.824166 0.759400 -21.00000 0.02171 0.02570 = 0.02400 -0.01286 -0.00472 -0.00367 AFIX 43 H2 2 0.940128 0.753949 0.719357 -21.00000 -1.20000 AFIX 0 C3 1 1.099484 0.931606 0.736967 -21.00000 0.01785 0.02026 = 0.02497 -0.01286 0.00021 0.00158 AFIX 43 H3 2 1.241082 0.943687 0.680251 -21.00000 -1.20000 AFIX 0 C4 1 1.034268 1.010925 0.805516 -21.00000 0.01733 0.01959 = 0.02783 -0.01345 -0.00267 -0.00448 AFIX 43 H4 2 1.128700 1.087364 0.805357 -21.00000 -1.20000 PART 0 RESI 0 AFIX 0 HKLF 4 REM Eisenreich_TSC_19_a.res in P-1 REM wR2 = 0.0762, GooF = S = 1.042, Restrained GooF = 1.026 for all data REM R1 = 0.0271 for 3731 Fo > 4sig(Fo) and 0.0296 for all 4060 data REM 197 parameters refined using 208 restraints END WGHT 0.0409 0.1792 REM Instructions for potential hydrogen bonds EQIV $1 x+1, y, z HTAB N1 S1_$1 EQIV $2 -x, -y+1, -z+2 HTAB N2 S1_$2 HTAB C7 S1_$1 HTAB C8 S1_$2 EQIV $3 x+1, y+1, z HTAB C3_1 S1_$3 REM Highest difference peak 0.444, deepest hole -0.230, 1-sigma level 0.049 Q1 1 0.5259 0.3156 0.6552 11.00000 0.05 0.44 Q2 1 0.3338 0.3615 0.6338 11.00000 0.05 0.42 Q3 1 0.5340 0.1993 0.5366 11.00000 0.05 0.42 Q4 1 0.2862 0.5121 0.8523 11.00000 0.05 0.41 Q5 1 0.3505 0.2601 0.5020 11.00000 0.05 0.41 Q6 1 0.6342 0.7917 0.8622 11.00000 0.05 0.40 Q7 1 0.2690 0.3482 0.5462 11.00000 0.05 0.40 Q8 1 0.6306 0.2444 0.6085 11.00000 0.05 0.38 Q9 1 0.3449 0.4565 0.7803 11.00000 0.05 0.36 Q10 1 0.5134 0.7008 0.8594 11.00000 0.05 0.34 Q11 1 0.1484 0.4339 0.8385 11.00000 0.05 0.32 Q12 1 0.7462 0.8879 0.8674 11.00000 0.05 0.31 Q13 1 0.4366 0.4053 0.7087 11.00000 0.05 0.30 Q14 1 0.8258 0.8240 0.8031 11.00000 0.05 0.24 Q15 1 1.0203 0.8821 0.7404 11.00000 0.05 0.22 Q16 1 0.4071 0.6071 0.8639 11.00000 0.05 0.22 Q17 1 -0.0306 0.3371 0.8194 11.00000 0.05 0.20 Q18 1 0.9717 0.7959 0.6749 11.00000 0.05 0.18 Q19 1 0.5959 0.6307 0.7940 11.00000 0.05 0.18 Q20 1 -0.0563 0.4374 0.8963 11.00000 0.05 0.17 ; _shelx_res_checksum 50869 _shelx_hkl_file ; -1 0 0 8.50 1.10 -1 0 0 5.10 0.70 -1 0 0 5.00 0.90 -1 0 0 5.90 0.90 -1 0 0 5.60 0.60 -1 0 0 4.50 0.80 1 0 0 4.80 0.80 1 0 0 4.30 0.90 1 0 0 5.80 0.50 1 0 0 5.50 0.90 1 0 0 5.00 0.80 -2 0 0 2392.96 53.69 -2 0 0 2507.45 54.59 -2 0 0 2376.26 53.69 -2 0 0 2419.56 52.69 -2 0 0 2503.15 53.59 -2 0 0 2462.55 51.69 -2 0 0 2425.86 53.59 2 0 0 2372.86 53.79 2 0 0 2408.26 54.59 2 0 0 2393.06 53.79 2 0 0 2415.96 51.19 2 0 0 2453.95 53.99 2 0 0 2527.55 53.49 -3 0 0 1293.87 31.20 -3 0 0 1173.68 31.00 -3 0 0 1265.57 32.60 -3 0 0 1298.87 30.20 -3 0 0 1262.17 31.40 -3 0 0 1265.57 31.40 -3 0 0 1277.77 28.50 3 0 0 1259.07 31.60 3 0 0 1302.97 27.70 3 0 0 1300.57 31.70 -4 0 0 2938.51 69.59 -4 0 0 3000.80 66.19 -4 0 0 2943.01 67.59 -4 0 0 2976.00 67.89 -4 0 0 2824.82 67.19 -4 0 0 2856.51 63.39 -4 0 0 2960.90 67.99 4 0 0 2944.11 61.99 4 0 0 2934.81 67.79 4 0 0 2962.00 68.39 4 0 0 2953.60 69.99 -5 0 0 258.17 11.70 -5 0 0 244.08 12.60 -5 0 0 253.57 11.50 -5 0 0 244.78 11.10 -5 0 0 264.47 11.90 -5 0 0 243.48 10.40 5 0 0 237.18 11.20 5 0 0 245.18 12.00 -6 0 0 7.50 2.60 -6 0 0 14.30 3.70 -6 0 0 10.90 3.10 -6 0 0 9.20 3.50 -6 0 0 9.40 3.20 -6 0 0 6.20 2.70 6 0 0 9.40 3.10 6 0 0 7.80 2.80 6 0 0 8.20 3.40 6 0 0 5.10 2.30 -7 0 0 219.08 12.20 -7 0 0 196.48 13.70 -7 0 0 214.58 11.70 7 0 0 221.08 14.50 7 0 0 200.48 11.00 7 0 0 193.38 12.80 -8 0 0 177.38 13.40 -8 0 0 173.88 11.50 8 0 0 144.09 12.00 8 0 0 159.68 13.30 8 -1 0 -1.70 2.60 8 -1 0 1.20 2.50 -8 1 0 -0.10 2.20 -8 1 0 -1.80 2.30 -8 1 0 0.50 2.20 7 -1 0 15.90 5.00 7 -1 0 17.30 4.20 7 -1 0 17.40 5.30 -7 1 0 20.70 4.60 -7 1 0 23.70 5.00 -7 1 0 19.80 5.00 6 -1 0 169.68 11.70 6 -1 0 163.58 9.60 6 -1 0 185.98 11.40 6 -1 0 181.28 9.80 -6 1 0 164.48 9.70 -6 1 0 167.78 9.60 -6 1 0 154.58 10.90 -6 1 0 160.08 9.70 -6 1 0 168.88 9.80 -6 1 0 173.38 10.30 5 -1 0 1511.75 43.30 5 -1 0 1598.44 42.60 5 -1 0 1598.74 40.70 -5 1 0 1568.94 40.70 -5 1 0 1529.95 40.20 -5 1 0 1516.85 39.80 -5 1 0 1541.55 42.80 -5 1 0 1638.74 40.70 -5 1 0 1547.85 41.10 4 -1 0 415.76 15.20 4 -1 0 419.16 14.40 4 -1 0 447.76 16.50 -4 1 0 426.26 14.00 -4 1 0 428.66 14.30 -4 1 0 424.56 14.50 -4 1 0 416.66 14.20 -4 1 0 413.86 14.70 -4 1 0 396.76 15.30 3 -1 0 14.60 2.40 3 -1 0 12.80 2.60 3 -1 0 14.50 0.70 3 -1 0 13.60 2.40 -3 1 0 12.90 2.20 -3 1 0 14.80 2.40 -3 1 0 11.20 1.90 -3 1 0 11.80 2.10 -3 1 0 17.70 1.60 -3 1 0 12.40 2.10 -3 1 0 17.40 2.90 2 -1 0 4.70 1.10 2 -1 0 6.50 1.30 2 -1 0 7.00 0.50 2 -1 0 5.70 1.30 2 -1 0 6.50 1.50 -2 1 0 4.80 1.20 -2 1 0 7.40 1.50 -2 1 0 6.20 0.80 -2 1 0 7.90 1.40 -2 1 0 5.40 1.20 -2 1 0 6.00 1.20 -2 1 0 5.80 1.20 1 -1 0 6426.16 133.99 1 -1 0 6739.73 135.09 1 -1 0 6230.18 134.39 1 -1 0 6462.65 134.69 -1 1 0 6329.87 134.89 -1 1 0 6374.26 134.29 -1 1 0 6138.49 134.29 -1 1 0 6585.44 134.39 -1 1 0 6725.83 134.49 -1 1 0 6096.89 134.69 -1 1 0 6499.75 134.49 0 -1 0 1656.33 33.30 0 -1 0 1538.85 33.20 0 -1 0 1643.44 33.60 0 -1 0 1630.34 33.40 0 -1 0 1612.44 33.20 0 -1 0 1537.35 33.40 0 1 0 1586.24 33.30 0 1 0 1583.34 33.30 0 1 0 1484.15 32.90 0 1 0 1598.04 33.20 0 1 0 1607.34 33.10 0 1 0 1623.14 33.30 0 1 0 1549.84 33.20 0 1 0 1519.05 33.20 0 1 0 1557.24 33.30 0 1 0 1579.84 33.30 -1 -1 0 200.88 5.80 -1 -1 0 187.08 4.80 -1 -1 0 197.38 5.70 -1 -1 0 195.68 5.60 -1 -1 0 188.58 5.90 -1 -1 0 196.18 5.70 1 1 0 181.58 5.60 1 1 0 189.18 5.00 1 1 0 209.78 5.60 1 1 0 206.68 5.40 1 1 0 194.28 5.30 1 1 0 186.68 5.90 -2 -1 0 596.34 15.70 -2 -1 0 618.74 14.50 -2 -1 0 605.84 16.10 -2 -1 0 605.94 15.90 -2 -1 0 595.54 14.50 -2 -1 0 610.24 16.00 -2 -1 0 597.14 16.70 2 1 0 635.54 16.50 2 1 0 599.14 15.60 2 1 0 625.64 16.80 2 1 0 612.04 15.60 2 1 0 587.94 15.90 2 1 0 619.04 14.40 -3 -1 0 219.78 8.50 -3 -1 0 226.08 9.00 -3 -1 0 228.58 7.20 -3 -1 0 233.28 7.60 -3 -1 0 218.98 8.80 -3 -1 0 231.78 8.80 3 1 0 218.18 6.60 3 1 0 232.38 8.80 3 1 0 222.68 9.00 -4 -1 0 191.78 8.90 -4 -1 0 197.08 8.80 -4 -1 0 183.88 8.90 -4 -1 0 188.98 6.80 -4 -1 0 190.08 9.90 -4 -1 0 184.08 7.60 -4 -1 0 193.08 9.20 4 1 0 192.28 9.00 4 1 0 189.78 6.10 4 1 0 208.88 9.50 4 1 0 199.98 10.10 -5 -1 0 1710.23 44.70 -5 -1 0 1741.73 45.10 -5 -1 0 1783.42 48.10 -5 -1 0 1834.92 46.40 -5 -1 0 1781.82 45.80 -5 -1 0 1772.52 43.10 5 1 0 1792.22 45.60 5 1 0 1683.23 47.20 5 1 0 1812.12 45.70 -6 -1 0 2.80 2.00 -6 -1 0 2.20 2.30 -6 -1 0 -1.40 1.50 -6 -1 0 2.20 2.30 -6 -1 0 0.70 1.40 -6 -1 0 2.40 1.90 6 1 0 4.70 2.80 6 1 0 0.10 1.60 6 1 0 2.50 1.60 6 1 0 -0.10 1.90 -7 -1 0 709.73 25.00 -7 -1 0 722.73 28.60 -7 -1 0 683.23 24.50 7 1 0 698.33 24.60 7 1 0 698.83 27.90 7 1 0 697.03 26.20 -8 -1 0 51.49 7.40 -8 -1 0 38.60 7.40 8 1 0 37.60 7.50 8 1 0 42.80 7.60 8 -2 0 16.90 5.10 8 -2 0 16.40 5.70 8 -2 0 21.50 5.30 -8 2 0 13.80 4.50 -8 2 0 16.80 4.50 -8 2 0 17.50 4.80 7 -2 0 296.67 17.00 7 -2 0 242.58 13.20 7 -2 0 247.18 14.90 -7 2 0 271.27 13.60 -7 2 0 246.68 13.60 -7 2 0 254.37 14.90 6 -2 0 240.58 14.10 6 -2 0 229.88 13.20 6 -2 0 209.78 11.10 -6 2 0 211.78 12.50 -6 2 0 223.98 11.50 -6 2 0 211.18 11.30 -6 2 0 253.27 12.60 -6 2 0 235.58 11.30 -6 2 0 242.68 11.70 5 -2 0 0.80 1.20 5 -2 0 3.30 1.90 5 -2 0 1.20 1.90 5 -2 0 3.50 2.50 -5 2 0 2.60 1.80 -5 2 0 1.20 1.80 -5 2 0 4.60 2.00 -5 2 0 4.10 1.90 -5 2 0 1.70 1.80 -5 2 0 3.00 1.80 4 -2 0 530.75 18.10 4 -2 0 520.15 18.50 4 -2 0 536.95 16.80 -4 2 0 506.55 16.50 -4 2 0 514.15 16.20 -4 2 0 533.85 18.00 -4 2 0 530.05 16.80 -4 2 0 528.15 17.30 -4 2 0 502.35 16.30 3 -2 0 18.10 3.00 3 -2 0 17.40 2.80 3 -2 0 22.90 2.90 -3 2 0 17.90 2.60 -3 2 0 16.60 2.60 -3 2 0 19.20 2.90 -3 2 0 22.00 2.80 -3 2 0 18.80 2.60 -3 2 0 19.20 1.40 -3 2 0 20.80 2.70 2 -2 0 101.39 5.00 2 -2 0 101.59 4.90 2 -2 0 97.09 3.00 2 -2 0 92.89 4.30 -2 2 0 95.29 4.30 -2 2 0 99.99 3.40 -2 2 0 102.89 4.80 -2 2 0 102.39 4.40 -2 2 0 91.89 4.80 -2 2 0 94.19 4.60 -2 2 0 103.89 4.60 1 -2 0 986.40 22.70 1 -2 0 978.50 22.50 1 -2 0 952.50 22.90 1 -2 0 1035.10 23.00 1 -2 0 1015.40 22.10 -1 2 0 1017.70 22.00 -1 2 0 987.10 22.90 -1 2 0 1012.30 22.00 -1 2 0 972.70 22.70 -1 2 0 983.80 22.60 -1 2 0 953.50 22.80 -1 2 0 971.50 22.40 -1 2 0 1001.30 21.50 -1 2 0 991.10 22.30 -1 2 0 983.50 22.40 -1 2 0 1003.20 22.30 0 -2 0 155.08 4.40 0 -2 0 150.78 4.30 0 -2 0 159.18 4.40 0 -2 0 150.48 4.10 0 -2 0 148.29 4.40 0 -2 0 153.18 4.10 0 2 0 151.38 4.40 0 2 0 147.09 4.10 0 2 0 138.99 4.10 0 2 0 150.58 4.50 0 2 0 147.09 4.40 0 2 0 159.88 4.30 0 2 0 145.59 4.40 0 2 0 155.78 4.30 0 2 0 153.78 4.40 0 2 0 151.18 3.90 0 2 0 149.29 3.90 -1 -2 0 1804.32 39.20 -1 -2 0 1781.32 39.40 -1 -2 0 1776.92 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210.18 7.10 -1 5 0 202.78 7.20 -1 5 0 241.18 7.30 -1 5 0 206.98 7.50 0 -5 0 3557.54 78.19 0 -5 0 3572.44 78.89 0 -5 0 3616.54 78.69 0 -5 0 3634.44 78.99 0 -5 0 3689.73 77.79 0 5 0 3665.13 79.09 0 5 0 3548.24 78.79 0 5 0 3695.93 79.09 0 5 0 3711.83 79.19 0 5 0 3660.63 77.29 0 5 0 3753.12 78.19 0 5 0 3593.24 77.29 0 5 0 3731.33 79.09 -1 -5 0 1991.60 45.00 -1 -5 0 1943.11 42.60 -1 -5 0 2113.39 46.40 -1 -5 0 1938.51 45.10 -1 -5 0 1986.00 45.90 -1 -5 0 1977.80 45.80 1 5 0 1986.50 45.90 1 5 0 2056.79 42.20 1 5 0 2032.90 43.80 1 5 0 1948.31 45.10 1 5 0 2019.50 45.50 -2 -5 0 1691.53 40.70 -2 -5 0 1726.73 42.50 -2 -5 0 1752.82 40.80 -2 -5 0 1764.52 41.90 -2 -5 0 1686.23 41.50 2 5 0 1747.63 37.20 2 5 0 1742.53 40.70 2 5 0 1731.83 41.50 2 5 0 1751.42 40.00 2 5 0 1724.33 40.20 -3 -5 0 1338.87 33.00 -3 -5 0 1312.77 35.10 -3 -5 0 1364.46 36.20 -3 -5 0 1340.37 35.10 -3 -5 0 1325.07 33.60 -3 -5 0 1356.76 33.90 3 5 0 1340.17 30.40 3 5 0 1353.06 33.80 3 5 0 1292.77 32.70 3 5 0 1322.07 34.60 3 5 0 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149.19 6.10 0 6 0 147.39 5.90 0 6 0 163.18 6.60 0 6 0 160.18 6.70 0 6 0 158.98 5.60 0 6 0 174.78 7.00 0 6 0 155.18 5.50 -1 -6 0 145.09 4.80 -1 -6 0 145.19 6.90 -1 -6 0 152.78 7.00 -1 -6 0 153.48 6.70 -1 -6 0 145.89 7.00 -1 -6 0 158.28 6.50 1 6 0 144.49 7.00 1 6 0 148.29 6.50 1 6 0 152.18 4.30 1 6 0 156.78 5.50 1 6 0 155.08 6.80 1 6 0 155.08 6.60 -2 -6 0 78.99 5.00 -2 -6 0 84.29 5.10 -2 -6 0 76.09 5.30 -2 -6 0 82.99 5.90 -2 -6 0 86.29 5.70 2 6 0 93.29 5.20 2 6 0 87.29 4.50 2 6 0 83.09 5.10 -3 -6 0 44.90 4.10 -3 -6 0 36.30 5.10 -3 -6 0 48.50 5.60 -3 -6 0 36.80 4.80 -3 -6 0 38.50 4.20 -3 -6 0 39.90 4.60 3 6 0 38.60 4.20 3 6 0 38.70 4.20 3 6 0 46.20 5.10 3 6 0 43.40 4.40 -4 -6 0 130.29 8.70 -4 -6 0 130.79 9.40 -4 -6 0 134.19 7.90 -4 -6 0 124.29 8.80 -4 -6 0 131.99 7.50 4 6 0 129.99 7.40 4 6 0 139.09 8.40 4 6 0 126.59 7.60 4 6 0 143.19 7.30 -5 -6 0 102.89 10.30 -5 -6 0 102.09 11.30 -5 -6 0 103.69 7.40 -5 -6 0 105.29 10.70 5 6 0 107.39 6.50 5 6 0 77.59 8.10 5 6 0 100.99 7.90 -6 -6 0 166.68 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80.59 5.20 -2 7 0 88.19 4.80 -2 7 0 87.89 5.00 -2 7 0 83.59 5.00 -2 7 0 85.29 5.60 -2 7 0 85.39 5.80 -2 7 0 80.19 4.70 -2 7 0 80.49 4.90 -2 7 0 78.09 4.70 1 -7 0 186.08 7.40 1 -7 0 187.48 7.90 1 -7 0 191.28 7.90 1 -7 0 202.68 8.20 1 -7 0 219.38 8.40 1 -7 0 195.18 7.80 -1 7 0 188.28 7.70 -1 7 0 186.18 7.40 -1 7 0 193.68 8.00 -1 7 0 192.88 7.90 -1 7 0 204.48 7.60 -1 7 0 194.68 7.40 -1 7 0 202.38 8.10 -1 7 0 184.28 7.90 -1 7 0 188.58 7.80 0 -7 0 58.69 3.30 0 -7 0 56.39 4.20 0 -7 0 65.09 4.40 0 -7 0 63.29 4.40 0 -7 0 67.99 4.10 0 -7 0 67.99 4.30 0 -7 0 69.59 3.80 0 7 0 62.79 4.30 0 7 0 62.09 4.40 0 7 0 65.89 4.30 0 7 0 66.19 3.90 0 7 0 65.89 4.40 0 7 0 62.79 3.40 0 7 0 66.79 3.50 0 7 0 60.19 4.40 -1 -7 0 174.08 8.20 -1 -7 0 166.08 8.20 -1 -7 0 177.98 8.20 -1 -7 0 177.58 7.60 -1 -7 0 186.88 8.00 1 7 0 165.58 7.30 1 7 0 170.38 6.20 1 7 0 165.28 7.50 1 7 0 182.98 8.40 -2 -7 0 511.25 18.10 -2 -7 0 542.55 16.80 -2 -7 0 545.95 17.80 -2 -7 0 533.85 16.80 -2 -7 0 546.35 18.00 2 7 0 529.05 16.60 2 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-2 -2 -15 15.70 5.00 -2 -2 -15 16.20 5.30 2 2 15 13.40 5.10 2 2 15 21.90 4.60 -3 -2 -15 73.89 10.00 -3 -2 -15 96.39 11.50 3 2 15 96.49 10.20 3 2 15 81.79 10.30 -4 -2 -15 162.38 15.70 4 2 15 196.18 12.50 4 2 15 168.38 12.40 2 -3 -15 36.50 7.70 2 -3 -15 31.10 8.20 -2 3 15 29.20 6.50 1 -3 -15 16.90 5.90 1 -3 -15 20.90 6.40 -1 3 15 28.90 6.20 -1 3 15 30.10 5.20 0 -3 -15 1.10 2.70 0 -3 -15 1.20 2.80 0 3 15 -0.70 2.20 0 3 15 0.40 2.10 -1 -3 -15 104.49 11.30 -1 -3 -15 107.69 12.90 1 3 15 97.19 11.10 1 3 15 94.79 9.40 -2 -3 -15 27.10 6.40 -2 -3 -15 24.50 6.40 2 3 15 34.00 6.10 2 3 15 28.80 6.20 -3 -3 -15 5.70 3.80 -3 -3 -15 3.40 3.80 3 3 15 6.80 3.50 3 3 15 10.20 4.00 -4 -3 -15 -0.30 3.80 4 3 15 3.00 2.70 4 3 15 1.50 3.00 2 -4 -15 134.79 15.40 2 -4 -15 156.78 16.10 -2 4 15 145.19 10.20 -2 4 15 148.79 11.40 1 -4 -15 177.08 14.40 1 -4 -15 183.28 14.50 -1 4 15 188.98 12.90 -1 4 15 170.28 10.70 0 -4 -15 105.79 10.90 0 -4 -15 100.79 12.20 0 -4 -15 107.79 13.00 0 4 15 105.59 8.50 0 4 15 111.29 11.70 -1 -4 -15 88.19 11.40 -1 -4 -15 100.09 11.00 1 4 15 96.39 8.10 1 4 15 98.49 10.70 -2 -4 -15 21.20 6.10 -2 -4 -15 25.50 6.00 2 4 15 30.20 5.70 2 4 15 19.00 5.20 -3 -4 -15 98.89 11.60 -3 -4 -15 134.99 14.10 3 4 15 121.79 12.40 3 4 15 130.99 9.90 -4 -4 -15 26.00 6.50 4 4 15 38.70 7.20 4 4 15 33.30 6.40 2 -5 -15 17.30 6.30 2 -5 -15 24.20 6.70 -2 5 15 16.10 3.90 -2 5 15 37.80 8.50 -2 5 15 23.00 5.20 1 -5 -15 57.69 9.30 1 -5 -15 54.59 9.50 -1 5 15 45.40 10.80 -1 5 15 52.29 7.30 -1 5 15 61.09 8.80 0 -5 -15 309.67 19.20 0 -5 -15 299.57 18.20 0 -5 -15 329.97 17.00 0 5 15 347.07 15.90 0 5 15 339.67 17.30 -1 -5 -15 397.46 21.40 -1 -5 -15 343.77 18.70 1 5 15 428.56 18.00 1 5 15 418.86 19.40 -2 -5 -15 47.50 8.70 -2 -5 -15 52.29 8.60 2 5 15 45.80 7.60 2 5 15 47.30 7.00 -3 -5 -15 125.19 13.60 -3 -5 -15 103.59 12.80 3 5 15 122.89 9.60 3 5 15 139.09 10.80 -4 -5 -15 144.49 15.20 4 5 15 185.38 15.30 4 5 15 175.18 11.90 2 -6 -15 -0.20 2.70 2 -6 -15 7.10 4.00 2 -6 -15 3.50 3.90 -2 6 15 0.60 2.40 -2 6 15 1.90 3.30 -2 6 15 5.80 3.00 1 -6 -15 143.79 15.60 1 -6 -15 161.78 16.30 1 -6 -15 145.09 11.50 -1 6 15 135.29 9.90 -1 6 15 145.49 11.20 -1 6 15 128.79 10.60 0 -6 -15 0.80 2.70 0 -6 -15 3.00 3.50 0 -6 -15 -1.50 3.00 0 6 15 3.40 3.00 0 6 15 1.70 2.50 0 6 15 2.80 3.00 -1 -6 -15 -1.30 2.40 -1 -6 -15 -1.80 2.10 -1 -6 -15 0.90 3.10 1 6 15 1.30 2.10 1 6 15 2.70 2.40 1 6 15 3.50 2.60 -2 -6 -15 5.10 3.90 -2 -6 -15 5.80 4.20 2 6 15 8.90 3.10 2 6 15 6.50 3.30 2 6 15 7.40 3.70 -3 -6 -15 1.20 3.20 -3 -6 -15 1.70 3.80 3 6 15 2.60 3.10 3 6 15 -1.10 1.90 3 6 15 1.40 2.20 -4 -6 -15 19.40 5.90 4 6 15 28.60 6.00 2 -7 -15 19.10 5.70 2 -7 -15 16.70 5.70 2 -7 -15 25.00 7.30 -2 7 15 38.60 7.90 -2 7 15 31.00 5.90 -2 7 15 21.00 5.20 1 -7 -15 6.80 4.40 1 -7 -15 8.00 4.00 1 -7 -15 10.00 4.80 -1 7 15 9.10 3.80 -1 7 15 11.80 3.90 -1 7 15 15.20 4.70 0 -7 -15 107.79 13.20 0 -7 -15 83.89 11.90 0 -7 -15 87.19 10.50 0 7 15 98.49 10.70 0 7 15 97.19 10.60 0 7 15 95.59 10.10 -1 -7 -15 20.30 5.80 -1 -7 -15 32.00 7.80 -1 -7 -15 34.50 7.40 1 7 15 24.40 5.20 1 7 15 28.60 5.70 1 7 15 23.10 4.90 -2 -7 -15 1.70 3.10 -2 -7 -15 -0.60 2.70 2 7 15 -0.60 1.90 2 7 15 0.80 2.10 2 7 15 -0.20 2.40 -3 -7 -15 311.97 18.90 -3 -7 -15 311.77 18.80 3 7 15 280.17 14.00 3 7 15 279.67 15.10 -4 -7 -15 250.37 17.20 4 7 15 260.87 14.80 4 7 15 270.27 13.50 2 -8 -15 37.10 7.60 2 -8 -15 30.00 8.00 2 -8 -15 45.10 8.90 -2 8 15 36.00 6.50 -2 8 15 38.80 6.60 -2 8 15 43.00 8.00 1 -8 -15 70.79 9.60 1 -8 -15 67.89 11.20 1 -8 -15 91.59 12.70 -1 8 15 59.09 8.60 -1 8 15 54.69 7.70 -1 8 15 72.59 8.80 0 -8 -15 216.18 16.60 0 -8 -15 203.18 15.60 0 -8 -15 261.97 15.60 0 8 15 220.88 12.80 0 8 15 221.88 13.90 0 8 15 226.68 13.50 -1 -8 -15 15.70 5.30 -1 -8 -15 17.50 6.20 -1 -8 -15 10.30 4.50 1 8 15 17.00 4.50 1 8 15 20.30 5.20 1 8 15 17.90 4.80 -2 -8 -15 41.50 8.40 -2 -8 -15 61.09 9.50 -2 -8 -15 59.49 9.70 2 8 15 59.39 7.80 2 8 15 44.20 7.00 -3 -8 -15 12.50 5.60 -3 -8 -15 12.50 5.30 3 8 15 17.70 4.20 3 8 15 17.70 4.40 1 -9 -15 143.09 15.70 1 -9 -15 155.48 16.90 1 -9 -15 131.19 13.30 -1 9 15 137.09 10.40 -1 9 15 123.79 9.90 -1 9 15 102.29 11.90 0 -9 -15 263.57 18.00 0 -9 -15 247.58 17.40 0 9 15 226.08 13.20 0 9 15 252.77 15.20 0 9 15 256.87 14.20 -1 -9 -15 215.58 15.10 -1 -9 -15 251.77 17.00 -1 -9 -15 215.98 16.00 1 9 15 224.68 13.60 1 9 15 221.18 13.00 -2 -9 -15 52.09 9.20 -2 -9 -15 52.59 9.30 -2 -9 -15 50.89 9.00 2 9 15 38.30 7.60 2 9 15 54.99 7.50 2 9 15 48.70 7.30 -3 -9 -15 138.69 15.10 -3 -9 -15 185.28 14.70 3 9 15 169.08 11.60 3 9 15 167.58 13.00 3 9 15 168.08 11.10 0 -10 -15 -1.40 2.90 0 -10 -15 -1.40 3.60 0 10 15 2.10 1.90 0 10 15 -1.50 1.80 -1 -10 -15 241.78 16.60 -1 -10 -15 290.27 18.40 -1 -10 -15 272.37 18.50 1 10 15 277.77 14.80 1 10 15 271.67 15.30 -2 -10 -15 4.20 3.40 -2 -10 -15 -2.30 2.60 -2 -10 -15 1.30 3.40 2 10 15 5.70 3.50 2 10 15 1.80 2.40 2 10 15 2.50 2.40 0 -1 -16 6.60 3.50 0 -1 -16 2.60 3.90 0 1 16 3.60 2.90 -1 -1 -16 12.90 4.60 -1 -1 -16 -1.80 3.00 1 1 16 8.90 4.00 -2 -1 -16 41.00 7.50 -2 -1 -16 21.10 5.50 2 1 16 38.80 9.60 2 1 16 32.90 6.70 0 -2 -16 89.59 12.10 0 -2 -16 86.29 10.00 0 2 16 73.09 10.30 -1 -2 -16 54.79 8.60 -1 -2 -16 50.79 8.90 1 2 16 43.20 6.60 1 2 16 60.69 9.20 -2 -2 -16 28.50 6.30 -2 -2 -16 19.20 5.70 2 2 16 37.50 6.40 2 2 16 27.30 6.80 -3 -2 -16 42.10 8.00 3 2 16 40.90 7.80 3 2 16 45.00 7.00 1 -3 -16 38.40 8.20 -1 3 16 32.30 6.50 0 -3 -16 19.70 5.40 0 -3 -16 18.30 5.90 0 3 16 25.90 5.30 0 3 16 14.00 4.00 -1 -3 -16 714.43 30.60 -1 -3 -16 713.23 28.30 1 3 16 668.43 24.90 1 3 16 710.23 28.40 -2 -3 -16 5.00 3.50 -2 -3 -16 4.50 3.70 2 3 16 12.50 4.00 2 3 16 8.40 3.60 -3 -3 -16 126.99 13.80 -3 -3 -16 177.18 16.50 3 3 16 145.79 10.60 3 3 16 116.29 12.50 1 -4 -16 -3.90 2.40 1 -4 -16 1.60 4.00 -1 4 16 1.20 2.50 -1 4 16 1.00 2.30 0 -4 -16 53.09 9.40 0 -4 -16 54.79 8.30 0 4 16 45.00 6.70 0 4 16 69.49 9.40 -1 -4 -16 74.19 9.90 -1 -4 -16 68.99 10.60 1 4 16 71.69 8.50 1 4 16 85.09 10.30 -2 -4 -16 1.10 2.80 -2 -4 -16 -3.20 2.90 2 4 16 1.60 2.70 2 4 16 -1.70 1.90 -3 -4 -16 -1.20 3.50 -3 -4 -16 -1.30 2.20 3 4 16 0.70 2.50 3 4 16 0.50 2.20 1 -5 -16 7.60 4.00 1 -5 -16 0.40 3.20 -1 5 16 0.90 2.40 -1 5 16 5.30 3.00 0 -5 -16 24.70 5.90 0 -5 -16 33.20 8.80 0 -5 -16 19.30 5.10 0 5 16 32.50 6.20 0 5 16 27.30 5.30 -1 -5 -16 9.70 4.60 -1 -5 -16 4.30 3.80 1 5 16 4.50 3.70 1 5 16 2.50 2.70 -2 -5 -16 64.79 9.70 -2 -5 -16 70.69 10.90 2 5 16 80.09 9.40 2 5 16 64.09 9.10 -3 -5 -16 6.90 4.50 -3 -5 -16 2.20 2.90 3 5 16 7.00 3.60 3 5 16 8.60 3.40 1 -6 -16 4.30 4.20 1 -6 -16 0.30 2.90 -1 6 16 3.90 2.70 -1 6 16 4.50 2.50 0 -6 -16 3.70 4.40 0 -6 -16 6.70 4.90 0 -6 -16 1.10 2.90 0 6 16 2.10 2.80 0 6 16 1.00 2.20 -1 -6 -16 57.99 9.10 -1 -6 -16 58.89 9.80 1 6 16 56.99 7.80 1 6 16 56.49 8.50 -2 -6 -16 53.89 9.30 -2 -6 -16 46.90 8.90 2 6 16 47.90 7.50 2 6 16 53.29 7.70 -3 -6 -16 0.50 3.20 -3 -6 -16 0.60 3.10 3 6 16 -2.00 2.00 3 6 16 -0.30 2.70 1 -7 -16 172.28 18.00 0 -7 -16 212.08 16.50 0 -7 -16 184.18 15.20 0 7 16 198.58 12.30 0 7 16 207.98 13.40 0 7 16 192.68 13.10 -1 -7 -16 323.77 20.30 -1 -7 -16 345.07 19.30 -1 -7 -16 361.06 20.60 1 7 16 362.86 17.20 1 7 16 317.77 17.20 1 7 16 352.76 17.30 -2 -7 -16 164.18 13.30 -2 -7 -16 160.68 16.40 2 7 16 150.78 10.60 2 7 16 160.88 11.20 2 7 16 156.28 11.80 -3 -7 -16 172.98 16.90 -3 -7 -16 203.78 16.00 3 7 16 208.18 14.60 3 7 16 189.48 18.50 0 -8 -16 50.99 9.90 0 -8 -16 73.69 11.50 0 8 16 55.29 8.30 0 8 16 61.49 8.30 0 8 16 58.89 8.30 -1 -8 -16 316.97 19.40 -1 -8 -16 245.68 18.10 -1 -8 -16 285.17 17.60 1 8 16 339.77 17.10 1 8 16 308.47 16.30 1 8 16 282.97 15.30 -2 -8 -16 15.10 5.50 -2 -8 -16 10.70 4.70 2 8 16 10.40 3.90 2 8 16 16.50 4.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 80564 loop_ _space_group_symop_operation_xyz 'x, y, z' '-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 0.00026(4) 0.38203(2) 0.86612(2) 0.01658(6) Uani 1 1 d . . . . . N1 N 0.44294(13) 0.44371(8) 0.74573(7) 0.01633(14) Uani 1 1 d D . . . . H1N H 0.575(2) 0.4844(13) 0.7404(12) 0.020 Uiso 1 1 d D U . . . N2 N 0.31140(14) 0.56179(8) 0.88187(7) 0.01567(14) Uani 1 1 d D . . . . H2N H 0.207(2) 0.5746(13) 0.9404(11) 0.019 Uiso 1 1 d D U . . . N3 N 0.51308(13) 0.64334(8) 0.83889(7) 0.01488(14) Uani 1 1 d D . . . . C1 C 0.26501(15) 0.46580(8) 0.82699(8) 0.01354(14) Uani 1 1 d D . . . . C2 C 0.43506(15) 0.36317(9) 0.66382(8) 0.01437(15) Uani 1 1 d D . . . . C3 C 0.25413(16) 0.38094(9) 0.58855(8) 0.01651(16) Uani 1 1 d . . . . . H3 H 0.126170 0.442678 0.595451 0.020 Uiso 1 1 calc R U . . . C4 C 0.26270(17) 0.30746(10) 0.50326(8) 0.01887(17) Uani 1 1 d . . . . . H4 H 0.138926 0.318514 0.452425 0.023 Uiso 1 1 calc R U . . . C5 C 0.45075(17) 0.21788(10) 0.49162(9) 0.02009(17) Uani 1 1 d . . . . . H5 H 0.455895 0.168549 0.432742 0.024 Uiso 1 1 calc R U . . . C6 C 0.63124(17) 0.20101(10) 0.56676(9) 0.02079(17) Uani 1 1 d . . . . . H6 H 0.759994 0.140044 0.559139 0.025 Uiso 1 1 calc R U . . . C7 C 0.62344(16) 0.27342(10) 0.65320(9) 0.01856(16) Uani 1 1 d . . . . . H7 H 0.746316 0.261538 0.704693 0.022 Uiso 1 1 calc R U . . . C8 C 0.53626(16) 0.73993(9) 0.88876(8) 0.01678(16) Uani 1 1 d . . . . . H8 H 0.419760 0.749520 0.953221 0.020 Uiso 1 1 calc R U . A 1 S1_1 S 0.95951(10) 0.82150(7) 0.73301(5) 0.01984(11) Uani 0.8314(17) 1 d . U P B 1 C1_1 C 0.73907(16) 0.83368(9) 0.84683(8) 0.01618(15) Uani 0.8314(17) 1 d . U P B 1 C2_1 C 0.7910(9) 0.9417(4) 0.8919(6) 0.0253(7) Uani 0.8314(17) 1 d . U P B 1 H2_1 H 0.692260 0.963742 0.956966 0.030 Uiso 0.8314(17) 1 calc R U P B 1 C3_1 C 1.0023(6) 1.0153(3) 0.8326(2) 0.0234(4) Uani 0.8314(17) 1 d . U P B 1 H3_1 H 1.060160 1.093234 0.850910 0.028 Uiso 0.8314(17) 1 calc R U P B 1 C4_1 C 1.1134(5) 0.9601(2) 0.7452(3) 0.0227(4) Uani 0.8314(17) 1 d . U P B 1 H4_1 H 1.260247 0.994640 0.696382 0.027 Uiso 0.8314(17) 1 calc R U P B 1 S1_2 S 0.7635(10) 0.9678(5) 0.8972(6) 0.0214(7) Uani 0.1686(17) 1 d . U P B 2 C1_2 C 0.73907(16) 0.83368(9) 0.84683(8) 0.01618(15) Uani 0.1686(17) 1 d . U P B 2 C2_2 C 0.928(2) 0.8242(17) 0.7594(12) 0.0224(16) Uani 0.1686(17) 1 d . U P B 2 H2_2 H 0.940128 0.753949 0.719357 0.027 Uiso 0.1686(17) 1 calc R U P B 2 C3_2 C 1.099(2) 0.9316(13) 0.7370(15) 0.0200(16) Uani 0.1686(17) 1 d . U P B 2 H3_2 H 1.241082 0.943687 0.680251 0.024 Uiso 0.1686(17) 1 calc R U P B 2 C4_2 C 1.034(3) 1.0109(17) 0.8055(12) 0.0201(16) Uani 0.1686(17) 1 d . U P B 2 H4_2 H 1.128700 1.087364 0.805357 0.024 Uiso 0.1686(17) 1 calc R U P B 2 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 0.01465(10) 0.01954(11) 0.01802(11) -0.01044(8) 0.00188(7) -0.00491(7) N1 0.0133(3) 0.0203(3) 0.0191(3) -0.0118(3) 0.0003(3) -0.0038(3) N2 0.0160(3) 0.0166(3) 0.0164(3) -0.0087(3) 0.0015(3) -0.0047(2) N3 0.0145(3) 0.0145(3) 0.0163(3) -0.0053(3) -0.0025(3) -0.0024(2) C1 0.0150(3) 0.0132(3) 0.0131(3) -0.0049(3) -0.0024(3) -0.0006(3) C2 0.0146(3) 0.0157(3) 0.0140(3) -0.0070(3) 0.0006(3) -0.0028(3) C3 0.0162(4) 0.0192(4) 0.0152(4) -0.0072(3) -0.0013(3) 0.0004(3) C4 0.0197(4) 0.0235(4) 0.0153(4) -0.0086(3) -0.0026(3) -0.0011(3) C5 0.0226(4) 0.0220(4) 0.0185(4) -0.0114(3) 0.0010(3) -0.0026(3) C6 0.0187(4) 0.0223(4) 0.0248(4) -0.0133(3) -0.0004(3) 0.0017(3) C7 0.0150(4) 0.0214(4) 0.0219(4) -0.0106(3) -0.0022(3) 0.0004(3) C8 0.0186(4) 0.0166(4) 0.0165(4) -0.0072(3) -0.0011(3) -0.0026(3) S1_1 0.0179(2) 0.02168(16) 0.0218(2) -0.01038(17) 0.00084(14) -0.00437(13) C1_1 0.0174(4) 0.0149(3) 0.0174(4) -0.0061(3) -0.0037(3) -0.0012(3) C2_1 0.0243(11) 0.0253(15) 0.0303(10) -0.0143(10) -0.0034(8) 0.0013(9) C3_1 0.0253(11) 0.0163(6) 0.0337(12) -0.0127(8) -0.0098(8) -0.0009(6) C4_1 0.0192(6) 0.0188(9) 0.0292(8) -0.0049(7) -0.0052(5) -0.0063(6) S1_2 0.0203(13) 0.0209(15) 0.0269(10) -0.0135(11) -0.0007(9) -0.0026(10) C1_2 0.0174(4) 0.0149(3) 0.0174(4) -0.0061(3) -0.0037(3) -0.0012(3) C2_2 0.022(3) 0.026(3) 0.024(3) -0.013(3) -0.005(2) -0.004(2) C3_2 0.018(3) 0.020(3) 0.025(3) -0.013(3) 0.000(2) 0.002(2) C4_2 0.017(3) 0.020(3) 0.028(3) -0.013(3) -0.003(3) -0.004(2) 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 C2 127.35(8) . . ? C1 N1 H1N 117.0(8) . . ? C2 N1 H1N 115.6(8) . . ? C1 N2 N3 119.57(7) . . ? C1 N2 H2N 119.1(8) . . ? N3 N2 H2N 121.2(8) . . ? C8 N3 N2 116.14(8) . . ? N1 C1 N2 115.16(8) . . ? N1 C1 S1 125.38(7) . . ? N2 C1 S1 119.44(7) . . ? C7 C2 C3 120.34(8) . . ? C7 C2 N1 118.12(8) . . ? C3 C2 N1 121.35(8) . . ? C4 C3 C2 119.39(8) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 120.69(8) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 119.61(8) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C7 120.15(9) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C2 C7 C6 119.82(8) . . ? C2 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? N3 C8 C1_2 120.09(8) . . ? N3 C8 C1_1 120.09(8) . . ? N3 C8 H8 120.0 . . ? C1_1 C8 H8 120.0 . . ? C1_1 S1_1 C4_1 91.86(12) . . ? C2_1 C1_1 C8 127.1(2) . . ? C2_1 C1_1 S1_1 110.1(2) . . ? C8 C1_1 S1_1 122.86(7) . . ? C1_1 C2_1 C3_1 114.1(3) . . ? C1_1 C2_1 H2_1 123.0 . . ? C3_1 C2_1 H2_1 123.0 . . ? C4_1 C3_1 C2_1 111.2(3) . . ? C4_1 C3_1 H3_1 124.4 . . ? C2_1 C3_1 H3_1 124.4 . . ? C3_1 C4_1 S1_1 112.8(2) . . ? C3_1 C4_1 H4_1 123.6 . . ? S1_1 C4_1 H4_1 123.6 . . ? C1_2 S1_2 C4_2 89.9(6) . . ? C2_2 C1_2 C8 125.1(7) . . ? C2_2 C1_2 S1_2 112.9(7) . . ? C8 C1_2 S1_2 121.9(2) . . ? C1_2 C2_2 C3_2 112.0(12) . . ? C1_2 C2_2 H2_2 124.0 . . ? C3_2 C2_2 H2_2 124.0 . . ? C4_2 C3_2 C2_2 109.8(14) . . ? C4_2 C3_2 H3_2 125.1 . . ? C2_2 C3_2 H3_2 125.1 . . ? C3_2 C4_2 S1_2 115.3(13) . . ? C3_2 C4_2 H4_2 122.3 . . ? S1_2 C4_2 H4_2 122.3 . . ? 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 1.6868(10) . ? N1 C1 1.3431(11) . ? N1 C2 1.4221(11) . ? N1 H1N 0.855(11) . ? N2 C1 1.3539(11) . ? N2 N3 1.3732(11) . ? N2 H2N 0.871(11) . ? N3 C8 1.2879(12) . ? C2 C7 1.3922(13) . ? C2 C3 1.3944(13) . ? C3 C4 1.3909(13) . ? C3 H3 0.9500 . ? C4 C5 1.3921(14) . ? C4 H4 0.9500 . ? C5 C6 1.3922(14) . ? C5 H5 0.9500 . ? C6 C7 1.3945(13) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C1_2 1.4440(13) . ? C8 C1_1 1.4440(13) . ? C8 H8 0.9500 . ? S1_1 C1_1 1.7142(11) . ? S1_1 C4_1 1.719(2) . ? C1_1 C2_1 1.394(4) . ? C2_1 C3_1 1.405(6) . ? C2_1 H2_1 0.9500 . ? C3_1 C4_1 1.365(3) . ? C3_1 H3_1 0.9500 . ? C4_1 H4_1 0.9500 . ? S1_2 C1_2 1.638(5) . ? S1_2 C4_2 1.729(15) . ? C1_2 C2_2 1.389(12) . ? C2_2 C3_2 1.418(18) . ? C2_2 H2_2 0.9500 . ? C3_2 C4_2 1.297(13) . ? C3_2 H3_2 0.9500 . ? C4_2 H4_2 0.9500 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _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 N2 N3 C8 174.66(8) . . . . ? C2 N1 C1 N2 -171.63(8) . . . . ? C2 N1 C1 S1 9.88(13) . . . . ? N3 N2 C1 N1 9.87(12) . . . . ? N3 N2 C1 S1 -171.55(6) . . . . ? C1 N1 C2 C7 -136.60(10) . . . . ? C1 N1 C2 C3 48.36(13) . . . . ? C7 C2 C3 C4 0.42(13) . . . . ? N1 C2 C3 C4 175.34(8) . . . . ? C2 C3 C4 C5 -0.66(14) . . . . ? C3 C4 C5 C6 0.43(14) . . . . ? C4 C5 C6 C7 0.03(15) . . . . ? C3 C2 C7 C6 0.05(14) . . . . ? N1 C2 C7 C6 -175.04(8) . . . . ? C5 C6 C7 C2 -0.27(14) . . . . ? N2 N3 C8 C1_2 -178.12(8) . . . . ? N2 N3 C8 C1_1 -178.12(8) . . . . ? N3 C8 C1_1 C2_1 -179.2(3) . . . . ? N3 C8 C1_1 S1_1 -1.15(13) . . . . ? C4_1 S1_1 C1_1 C2_1 -0.8(3) . . . . ? C4_1 S1_1 C1_1 C8 -179.17(12) . . . . ? C8 C1_1 C2_1 C3_1 179.9(2) . . . . ? S1_1 C1_1 C2_1 C3_1 1.6(4) . . . . ? C1_1 C2_1 C3_1 C4_1 -1.8(5) . . . . ? C2_1 C3_1 C4_1 S1_1 1.1(4) . . . . ? C1_1 S1_1 C4_1 C3_1 -0.2(2) . . . . ? N3 C8 C1_2 C2_2 -4.4(8) . . . . ? N3 C8 C1_2 S1_2 173.8(3) . . . . ? C4_2 S1_2 C1_2 C2_2 -2.0(9) . . . . ? C4_2 S1_2 C1_2 C8 179.7(6) . . . . ? C8 C1_2 C2_2 C3_2 179.7(8) . . . . ? S1_2 C1_2 C2_2 C3_2 1.4(14) . . . . ? C1_2 C2_2 C3_2 C4_2 0.3(18) . . . . ? C2_2 C3_2 C4_2 S1_2 -1.8(18) . . . . ? C1_2 S1_2 C4_2 C3_2 2.3(13) . . . . ?