#------------------------------------------------------------------------------ #$Date: 2018-03-28 08:09:44 +0300 (Wed, 28 Mar 2018) $ #$Revision: 207156 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/24/2242433.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2242433 loop_ _publ_author_name 'Chotima, Ratanon' 'Boonseng, Bussaba' 'Piyasaengthong, Akkharadet' 'Songsasen, Apisit' 'Chainok, Kittipong' _publ_section_title ; Crystal structure of 3-[2-(1,3-thiazol-2-yl)diazen-1-yl]pyridine-2,6-diamine monohydrate ; _journal_coeditor_code WM5438 _journal_issue 4 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 563 _journal_page_last 565 _journal_paper_doi 10.1107/S2056989018004693 _journal_volume 74 _journal_year 2018 _chemical_formula_iupac 'C8 H8 N6 S, H2 O' _chemical_formula_moiety 'C8 H8 N6 S, H2 O' _chemical_formula_sum 'C8 H10 N6 O S' _chemical_formula_weight 238.28 _chemical_name_systematic ; 3-[2-(1,3-Thiazol-2-yl)diazen-1-yl]pyridine-2,6-diamine monohydrate ; _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' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 90 _cell_angle_beta 93.824(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 3.7856(4) _cell_length_b 28.393(3) _cell_length_c 9.6324(9) _cell_measurement_reflns_used 4156 _cell_measurement_temperature 296 _cell_measurement_theta_max 26.622 _cell_measurement_theta_min 3.021 _cell_volume 1033.03(18) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 296.0 _diffrn_detector_area_resol_mean 10.5 _diffrn_measured_fraction_theta_full 0.972 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measurement_device 'four-circle KAPPA diffractometer' _diffrn_measurement_device_type 'Bruker D8 QUEST CMOS' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'graphiteDouble Bounce Multilayer Mirror' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 11837 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.621 _diffrn_reflns_theta_min 3.568 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.302 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2016) ; _exptl_crystal_colour 'dark orange' _exptl_crystal_density_diffrn 1.532 _exptl_crystal_description needle _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.327 _refine_diff_density_min -0.261 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 169 _refine_ls_number_reflns 2100 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.170 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0607 _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^)+(0.0131P)^2^+1.7616P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1127 _refine_ls_wR_factor_ref 0.1212 _reflns_number_gt 1670 _reflns_number_total 2100 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5438sup1.cif _cod_data_source_block I _cod_original_cell_volume 1033.02(17) _cod_database_code 2242433 _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 0.920 _shelx_estimated_absorpt_t_max 0.988 _shelx_hkl_file ; -1 0 0 5.70 4.40 -1 0 0 -2.40 3.20 -1 0 0 -3.10 3.40 1 0 0 12.40 4.20 1 0 0 -4.00 3.40 1 0 0 -4.50 3.30 2 0 0 1726.43 56.19 2 0 0 1714.83 56.09 2 0 0 1751.42 56.19 -2 0 0 1699.33 55.99 -2 0 0 1679.03 55.09 -2 0 0 1718.13 57.29 3 0 0 -1.00 12.80 3 0 0 1.20 11.90 -3 0 0 2.10 2.30 -3 0 0 -0.20 15.40 -3 0 0 4.40 11.20 3 0 0 -0.10 3.40 4 0 0 17.60 22.70 -4 0 0 7.20 4.30 -4 0 0 16.50 4.20 -4 0 0 16.50 29.70 4 0 0 18.10 6.60 1 -1 0 833.92 27.20 1 -1 0 837.82 27.20 -1 -1 0 779.12 27.10 -1 -1 0 781.92 27.00 1 1 0 926.11 27.70 -1 1 0 928.21 27.90 1 1 0 804.62 27.10 1 1 0 774.92 27.10 -1 1 0 793.02 27.10 -1 1 0 820.42 27.20 2 -1 0 269.17 14.50 -2 -1 0 297.57 10.40 2 -1 0 266.67 11.70 -2 -1 0 288.17 13.60 2 -1 0 277.97 14.80 2 1 0 302.77 14.50 -2 1 0 253.07 14.40 2 1 0 316.97 14.20 -2 1 0 270.87 16.80 2 1 0 313.97 11.80 -2 1 0 255.87 10.40 3 -1 0 6.60 3.80 -3 -1 0 8.60 15.70 -3 -1 0 -1.60 2.30 3 -1 0 -4.70 13.10 3 -1 0 1.10 11.80 -3 -1 0 6.60 11.10 -3 1 0 10.50 16.20 -3 1 0 0.80 11.40 3 1 0 4.00 3.70 3 1 0 11.50 13.20 3 1 0 8.70 12.40 -3 1 0 2.30 2.40 -4 -1 0 19.70 4.50 -4 -1 0 16.30 3.90 4 -1 0 15.20 6.10 4 -1 0 21.80 22.60 -4 1 0 8.50 4.60 4 1 0 8.30 6.30 4 1 0 -0.10 22.60 -4 1 0 18.60 32.80 -4 1 0 17.40 4.10 -2 -2 0 66.29 4.10 2 -2 0 75.19 8.20 2 -2 0 69.89 5.80 -2 -2 0 81.49 10.40 2 -2 0 77.49 7.70 2 2 0 82.59 7.70 -2 2 0 62.69 4.20 -2 2 0 85.29 8.10 2 2 0 78.79 10.40 -2 2 0 82.09 10.80 3 -2 0 29.90 12.20 -3 -2 0 27.70 3.20 3 -2 0 29.80 5.20 -3 -2 0 29.20 10.80 3 -2 0 38.30 13.60 -3 2 0 31.80 16.00 3 2 0 34.80 5.10 -3 2 0 33.10 11.80 -3 2 0 34.50 3.90 3 2 0 26.00 13.30 3 2 0 37.60 12.80 4 -2 0 80.19 23.30 4 -2 0 82.99 10.00 -4 2 0 61.49 6.50 -4 2 0 69.89 33.50 -4 2 0 76.09 6.80 4 2 0 78.09 22.60 1 -3 0 49.70 4.70 -1 -3 0 68.99 5.70 1 -3 0 47.40 4.70 -1 -3 0 49.60 4.40 -1 3 0 50.99 4.70 -1 3 0 64.29 7.70 1 3 0 45.40 5.70 2 -3 0 352.66 16.50 2 -3 0 351.96 14.10 2 -3 0 358.56 16.50 -2 -3 0 356.16 15.50 -2 -3 0 335.17 12.30 2 3 0 350.36 15.70 -2 3 0 353.76 16.50 -2 3 0 354.06 18.90 2 3 0 361.16 16.20 -2 3 0 339.87 12.60 3 -3 0 10.50 13.50 3 -3 0 13.10 12.20 3 -3 0 9.80 4.10 -3 -3 0 12.80 2.30 -3 -3 0 13.40 11.50 -3 3 0 16.70 16.70 -3 3 0 13.90 2.80 3 3 0 5.10 11.90 -3 3 0 12.70 11.70 3 3 0 17.40 13.70 4 -3 0 50.89 22.90 4 -3 0 65.99 8.30 -4 3 0 50.29 44.90 -4 3 0 50.79 5.70 -4 3 0 61.19 6.30 4 3 0 63.99 22.60 1 -4 0 1099.19 36.30 -1 -4 0 1103.69 35.90 -1 -4 0 1092.19 35.90 1 -4 0 1115.49 36.20 1 -4 0 1200.18 37.40 1 4 0 1039.90 35.80 1 4 0 1076.89 35.80 -1 4 0 1132.29 37.10 -1 4 0 1108.79 36.20 2 -4 0 49.90 5.30 -2 -4 0 47.00 6.90 -2 -4 0 42.60 3.40 2 -4 0 56.49 8.00 2 -4 0 54.29 7.90 2 4 0 52.69 7.50 2 4 0 47.20 7.20 -2 4 0 58.79 10.30 -2 4 0 59.79 8.50 -2 4 0 59.99 3.90 3 -4 0 5.70 12.70 3 -4 0 -5.80 13.50 3 -4 0 1.70 4.00 -3 -4 0 4.50 11.00 -3 -4 0 1.70 2.30 3 4 0 12.00 13.20 -3 4 0 5.70 2.90 -3 4 0 8.80 12.20 3 4 0 -6.90 11.80 -3 4 0 5.20 17.70 -4 -4 0 75.89 6.60 4 -4 0 76.39 10.30 4 -4 0 76.29 24.20 4 4 0 87.29 23.80 -4 4 0 70.39 7.40 -4 4 0 62.79 7.30 0 -5 0 2.10 2.50 0 5 0 4.30 2.60 -1 -5 0 293.37 11.90 1 -5 0 307.17 12.80 1 -5 0 284.67 13.50 1 -5 0 304.77 12.80 -1 5 0 314.67 12.60 -1 5 0 324.57 13.90 1 5 0 316.07 11.90 1 5 0 301.37 11.90 2 -5 0 520.65 19.60 2 -5 0 539.15 21.60 -2 -5 0 487.25 17.60 -2 -5 0 526.15 20.20 2 -5 0 503.35 21.20 -2 5 0 545.45 21.60 -2 5 0 514.05 23.50 2 5 0 534.05 20.50 2 5 0 493.25 20.20 -2 5 0 540.55 18.20 -3 -5 0 53.69 9.90 3 -5 0 47.90 6.80 3 -5 0 81.49 13.50 3 -5 0 66.89 14.20 -3 -5 0 65.19 4.50 -3 5 0 62.99 5.30 -3 5 0 65.09 18.10 -3 5 0 85.69 13.70 3 5 0 75.59 15.00 3 5 0 65.49 12.80 4 -5 0 0.90 23.40 4 -5 0 11.90 6.50 -4 5 0 6.60 4.90 4 5 0 -0.30 22.50 -4 5 0 6.50 4.20 0 -6 0 1076.69 36.00 0 -6 0 1155.68 36.10 0 6 0 1117.69 36.10 -1 -6 0 1352.26 44.20 1 -6 0 1407.76 44.90 1 -6 0 1362.06 44.80 1 -6 0 1409.76 45.10 -1 6 0 1414.46 45.60 1 6 0 1337.37 44.20 1 6 0 1346.87 44.30 -1 6 0 1294.27 44.70 -1 6 0 1412.86 44.80 2 -6 0 159.88 8.50 2 -6 0 166.08 13.80 -2 -6 0 162.78 11.60 2 -6 0 158.18 13.50 -2 -6 0 138.39 6.50 -2 6 0 154.38 16.30 2 6 0 156.28 12.10 2 6 0 160.48 12.10 -2 6 0 164.48 14.10 -2 6 0 154.98 6.80 3 -6 0 112.99 15.40 3 -6 0 112.89 8.50 3 -6 0 104.29 14.20 -3 -6 0 113.09 10.30 -3 6 0 131.59 14.70 -3 6 0 106.29 20.10 3 6 0 114.99 14.90 -3 6 0 94.89 6.50 3 6 0 111.09 13.00 4 -6 0 1.60 6.60 4 -6 0 -5.80 22.70 -4 6 0 -0.10 9.60 -4 6 0 -2.20 4.20 4 6 0 -1.40 24.40 0 -7 0 3.40 3.70 0 -7 0 3.70 3.50 0 7 0 0.00 3.70 1 -7 0 12.40 5.70 1 -7 0 12.90 5.40 -1 -7 0 10.90 4.60 1 -7 0 9.20 3.40 -1 7 0 6.10 5.20 -1 7 0 15.70 6.60 1 7 0 11.40 4.60 -1 7 0 10.30 5.30 1 7 0 10.00 4.70 -2 -7 0 686.63 24.70 2 -7 0 666.83 24.50 2 -7 0 679.63 26.20 2 -7 0 654.63 25.60 2 7 0 652.93 24.90 -2 7 0 655.13 23.00 -2 7 0 689.33 28.60 2 7 0 678.33 25.10 3 -7 0 239.68 24.00 3 -7 0 256.27 22.70 -3 -7 0 245.68 9.90 3 -7 0 230.88 12.50 3 7 0 266.37 22.10 -3 7 0 211.28 29.70 -3 7 0 235.28 21.30 -3 7 0 248.58 10.50 3 7 0 259.17 22.10 4 -7 0 20.00 24.80 4 -7 0 21.60 7.50 -4 7 0 8.30 20.70 -4 7 0 12.90 4.70 4 7 0 5.20 24.50 0 -8 0 355.16 14.20 0 8 0 363.06 14.20 0 8 0 381.46 13.90 -1 -8 0 793.92 26.50 1 -8 0 799.92 27.40 1 -8 0 812.02 27.40 1 -8 0 782.92 26.80 -1 8 0 817.02 28.20 -1 8 0 770.52 27.10 -1 8 0 692.63 26.20 1 8 0 767.52 26.60 -2 -8 0 79.59 8.60 2 -8 0 70.49 6.40 2 -8 0 79.19 10.30 2 -8 0 73.59 9.40 2 8 0 79.29 8.90 -2 8 0 77.69 4.80 2 8 0 87.49 8.80 -2 8 0 82.89 12.60 3 -8 0 7.70 4.70 3 -8 0 4.70 14.10 -3 -8 0 9.20 2.80 3 -8 0 2.90 15.10 3 8 0 11.60 14.70 -3 8 0 4.90 13.50 -3 8 0 5.30 2.90 3 8 0 5.40 13.10 -3 8 0 -0.40 20.00 4 -8 0 8.60 24.80 4 -8 0 9.10 6.90 -4 8 0 2.90 5.10 4 8 0 6.60 27.00 -4 8 0 10.80 22.10 0 -9 0 6.30 4.90 0 9 0 8.60 4.70 0 9 0 13.30 4.90 1 -9 0 2452.25 77.79 1 -9 0 2449.16 77.69 -1 -9 0 2405.06 77.09 1 -9 0 2345.77 77.79 -1 9 0 2401.36 77.59 -1 9 0 2382.96 76.99 -1 9 0 2361.36 78.19 1 9 0 2453.75 77.19 2 -9 0 615.54 23.10 -2 -9 0 611.44 23.70 2 -9 0 643.44 26.10 2 -9 0 606.34 25.10 -2 9 0 619.44 28.40 2 9 0 639.44 24.40 2 9 0 597.94 23.90 -2 9 0 607.14 21.50 3 -9 0 110.99 17.80 3 -9 0 107.49 15.70 3 -9 0 84.19 8.50 -3 -9 0 101.39 5.90 -3 9 0 95.59 21.80 3 9 0 103.39 15.00 -3 9 0 115.39 15.60 3 9 0 94.69 15.80 -3 9 0 88.09 6.50 4 -9 0 26.00 26.20 4 -9 0 23.70 7.70 4 9 0 34.40 27.10 -4 9 0 20.00 4.80 -4 9 0 20.70 22.10 0 10 0 9999.00 314.77 1 -10 0 2387.66 77.69 -1 -10 0 2419.96 76.99 1 -10 0 2385.56 77.59 1 -10 0 2368.76 77.39 -1 10 0 2379.36 76.89 -1 10 0 2432.36 78.29 1 10 0 2366.56 76.99 -1 10 0 2441.96 77.49 2 -10 0 408.06 20.60 -2 -10 0 419.16 18.60 2 -10 0 432.76 22.20 2 -10 0 414.06 16.90 2 10 0 403.56 19.40 -2 10 0 426.66 15.60 -2 10 0 432.66 24.30 2 10 0 427.96 19.40 -2 10 0 396.26 20.70 -3 -10 0 5.80 2.90 3 -10 0 -9.50 17.10 3 -10 0 1.90 4.80 3 -10 0 12.30 14.80 3 10 0 1.60 14.90 -3 10 0 4.60 14.30 3 10 0 -3.50 13.90 -3 10 0 11.20 3.40 -3 10 0 1.50 21.50 4 -10 0 -6.00 7.10 4 -10 0 -12.00 26.30 -4 10 0 -0.70 21.90 -4 10 0 -0.30 4.80 4 10 0 -1.80 27.60 0 -11 0 13.20 6.20 0 -11 0 17.40 5.60 0 11 0 20.30 5.60 1 -11 0 1036.70 36.30 1 -11 0 1075.29 37.20 1 -11 0 1105.59 37.40 -1 -11 0 1121.59 36.50 -1 11 0 1079.99 35.70 1 11 0 1081.29 36.50 -1 11 0 1030.60 38.00 2 -11 0 183.58 9.70 -2 -11 0 196.78 14.60 2 -11 0 171.98 17.60 2 -11 0 181.48 18.70 -2 11 0 178.68 16.40 2 11 0 163.68 15.30 -2 11 0 178.28 8.30 2 11 0 173.28 15.30 -2 11 0 191.68 20.60 3 -11 0 303.57 31.30 -3 -11 0 311.87 12.00 3 -11 0 309.27 25.70 3 -11 0 277.17 14.90 -3 11 0 303.67 26.50 3 11 0 280.17 25.70 3 11 0 273.07 23.90 -3 11 0 289.27 12.80 -3 11 0 276.87 34.60 4 -11 0 -8.70 7.30 4 -11 0 8.50 26.60 -4 11 0 10.20 5.10 -4 11 0 12.10 23.30 0 -12 0 937.11 31.50 0 12 0 858.91 30.90 1 -12 0 2413.26 82.39 -1 -12 0 2799.42 84.29 1 -12 0 2493.15 82.59 1 -12 0 2461.95 82.39 1 12 0 2560.74 82.09 -1 12 0 2537.65 83.29 -1 12 0 2555.34 81.79 2 -12 0 94.09 13.00 -2 -12 0 90.09 10.30 2 -12 0 73.89 6.40 2 -12 0 83.09 12.00 -2 12 0 96.89 12.30 -2 12 0 81.19 5.60 2 12 0 94.19 11.10 -2 12 0 86.39 15.10 2 12 0 84.39 10.90 3 -12 0 45.70 16.50 -3 -12 0 22.70 3.70 3 -12 0 42.00 6.30 3 -12 0 26.00 19.80 3 12 0 25.50 16.80 -3 12 0 25.80 23.90 -3 12 0 37.70 4.20 3 12 0 43.30 16.60 4 -12 0 7.20 25.40 4 -12 0 1.90 7.50 -4 12 0 -14.10 5.80 -4 12 0 9.60 24.10 0 -13 0 -2.20 6.90 0 13 0 -3.50 6.90 0 13 0 1.00 6.60 1 -13 0 54.49 8.70 1 -13 0 45.80 9.10 1 -13 0 49.00 4.90 -1 13 0 50.39 4.30 -1 13 0 50.49 10.30 1 13 0 47.50 8.20 2 -13 0 54.69 13.30 2 -13 0 47.80 12.00 -2 -13 0 55.29 10.00 2 -13 0 47.30 5.70 2 13 0 55.59 11.00 -2 13 0 59.59 12.40 -2 13 0 51.09 15.40 2 13 0 58.99 11.70 -2 13 0 51.29 4.80 3 -13 0 235.98 27.00 3 -13 0 239.88 23.90 -3 -13 0 248.78 10.60 3 -13 0 219.38 13.00 3 13 0 242.88 27.30 3 13 0 269.07 33.90 -3 13 0 234.08 11.20 -3 13 0 192.68 28.20 4 -13 0 -10.10 27.30 4 -13 0 1.00 7.70 -4 13 0 3.40 26.40 -4 13 0 -1.20 5.80 0 -14 0 877.01 31.00 0 14 0 838.42 30.60 1 -14 0 132.79 15.20 1 -14 0 105.59 7.00 1 -14 0 111.59 14.10 1 14 0 130.49 13.50 -1 14 0 117.29 6.20 -1 14 0 115.19 15.70 2 -14 0 181.68 21.80 2 -14 0 161.58 19.10 -2 -14 0 174.08 16.70 2 -14 0 157.88 9.50 2 14 0 176.88 18.60 -2 14 0 167.48 8.30 2 14 0 176.48 18.30 -2 14 0 164.18 23.60 3 -14 0 -7.10 17.20 -3 -14 0 -1.70 3.30 3 -14 0 -11.60 21.80 3 -14 0 11.60 5.00 3 14 0 1.90 18.10 -3 14 0 5.00 3.50 -3 14 0 6.20 18.30 4 -14 0 0.10 30.10 4 -14 0 13.60 8.50 -4 14 0 20.70 6.10 0 -15 0 -1.70 7.80 0 15 0 -0.20 7.60 1 -15 0 214.58 18.40 1 -15 0 221.48 15.70 1 -15 0 202.28 10.40 -1 15 0 215.98 9.30 -1 15 0 196.58 17.90 1 15 0 230.78 15.90 2 -15 0 117.09 15.50 2 -15 0 108.29 8.10 -2 -15 0 109.69 11.80 2 -15 0 115.29 14.20 2 15 0 118.99 13.10 2 15 0 116.29 14.30 -2 15 0 103.89 6.70 -2 15 0 105.39 17.90 3 -15 0 56.79 17.90 -3 -15 0 75.49 5.90 3 -15 0 60.79 8.20 3 -15 0 49.90 24.40 -3 15 0 81.59 19.20 -3 15 0 66.19 7.00 3 15 0 74.29 19.90 4 -15 0 2.50 37.40 4 -15 0 7.40 8.40 -4 15 0 -4.90 6.10 0 -16 0 8.20 8.90 0 16 0 4.30 8.30 1 -16 0 854.11 32.90 1 -16 0 797.82 28.20 -1 16 0 798.22 33.20 -1 16 0 830.62 28.40 1 16 0 824.12 31.30 -2 -16 0 3.30 11.30 2 -16 0 6.50 4.50 2 -16 0 14.50 13.70 2 -16 0 3.60 14.40 -2 16 0 -0.10 17.10 -2 16 0 8.60 3.40 2 16 0 2.00 13.50 2 16 0 -1.10 12.90 -3 -16 0 1.70 3.50 3 -16 0 0.40 24.80 3 -16 0 3.10 18.70 3 -16 0 5.40 5.50 3 16 0 -15.10 19.90 -3 16 0 -1.90 4.10 4 -16 0 19.10 8.90 -4 16 0 16.30 7.00 0 -17 0 2.90 9.60 0 -17 0 -0.30 2.20 0 17 0 1.80 9.10 1 -17 0 69.59 12.90 1 -17 0 74.39 6.60 1 -17 0 80.49 5.50 -1 17 0 71.29 13.30 -1 17 0 70.09 5.30 1 17 0 88.19 11.40 2 -17 0 228.08 24.70 2 -17 0 241.68 26.00 2 -17 0 220.38 12.10 -2 -17 0 240.18 20.00 2 17 0 229.98 23.50 -2 17 0 227.98 10.60 2 17 0 240.98 22.20 -2 17 0 212.08 29.10 3 -17 0 97.29 21.30 3 -17 0 99.49 9.60 -3 -17 0 105.19 7.10 3 -17 0 111.39 33.80 3 17 0 90.99 21.90 -3 17 0 89.19 8.30 4 -17 0 64.19 9.90 -4 17 0 53.89 7.70 0 -18 0 926.31 34.80 0 -18 0 887.01 30.90 0 18 0 897.01 34.20 1 -18 0 6.60 3.80 -1 -18 0 4.00 10.20 1 -18 0 0.40 2.50 1 -18 0 -3.50 12.70 -1 18 0 -2.00 13.90 1 18 0 6.90 11.60 -1 18 0 -5.10 2.60 -2 -18 0 7.30 12.60 2 -18 0 6.00 15.00 2 -18 0 8.10 17.10 2 -18 0 8.00 4.40 2 18 0 7.50 16.20 -2 18 0 14.80 3.60 -2 18 0 3.60 20.90 2 18 0 7.70 14.00 3 -18 0 1.10 5.90 -3 -18 0 -4.00 4.00 3 -18 0 -2.50 21.50 -3 18 0 10.50 4.60 3 18 0 13.40 21.10 4 -18 0 21.10 9.50 -4 18 0 10.60 7.20 0 -19 0 3.70 11.60 0 -19 0 -4.20 2.60 0 19 0 -3.00 11.00 1 -19 0 173.78 22.70 1 -19 0 191.28 10.30 1 -19 0 184.18 8.80 -1 -19 0 179.08 18.00 -1 19 0 185.98 9.10 1 19 0 208.08 20.40 -1 19 0 195.88 24.20 2 -19 0 202.78 11.90 2 -19 0 213.38 11.00 -2 -19 0 205.78 22.50 2 -19 0 210.98 21.50 2 19 0 213.18 26.60 -2 19 0 218.68 10.40 2 19 0 224.38 23.30 -2 19 0 213.28 33.20 3 -19 0 -3.50 6.30 3 -19 0 -5.50 23.00 -3 -19 0 4.20 4.10 3 19 0 15.30 25.80 -3 19 0 6.70 4.70 4 -19 0 2.90 9.70 -4 19 0 17.00 7.60 0 -20 0 455.15 25.50 0 -20 0 419.66 16.40 0 20 0 418.06 24.00 -1 -20 0 154.08 19.00 1 -20 0 167.58 17.80 1 -20 0 140.49 7.80 1 -20 0 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14 5 51.69 17.30 1 14 -5 51.09 5.20 -1 14 5 38.80 14.70 -1 14 5 40.70 12.70 0 -14 -5 -4.30 2.30 0 -14 5 6.30 12.40 0 -14 -5 4.20 3.70 0 -14 5 -2.70 3.20 0 -14 -5 -1.10 10.40 0 14 -5 -3.20 13.00 0 14 5 3.30 15.00 0 14 5 -6.00 12.00 0 14 -5 -1.50 2.80 0 14 5 9.60 11.10 1 -14 5 273.77 23.20 1 -14 5 282.37 13.00 1 14 5 265.27 22.90 -1 14 -5 269.27 11.20 2 -14 5 809.02 30.10 2 -14 5 742.33 39.20 2 -14 5 777.32 35.30 -2 14 -5 816.22 27.40 2 14 5 756.42 37.00 3 -14 5 19.50 6.10 3 -14 5 18.00 21.40 3 14 5 12.70 26.40 3 -15 -5 -6.40 6.90 3 -15 -5 -3.50 33.80 3 -15 -5 10.20 6.10 -3 -15 5 10.00 26.60 3 15 -5 9.80 6.30 -3 15 5 4.30 6.70 -3 15 5 11.20 32.40 2 -15 -5 699.53 27.90 2 -15 -5 725.13 40.30 2 -15 -5 743.83 26.40 -2 -15 5 685.73 37.50 -2 15 5 669.83 26.40 -2 15 5 609.34 42.80 2 15 -5 686.73 26.10 -2 15 5 755.02 41.20 2 15 -5 710.03 41.70 -1 -15 5 180.48 21.80 1 -15 -5 200.18 22.10 1 -15 -5 188.28 9.30 1 -15 -5 196.58 10.90 1 15 -5 169.38 9.30 -1 15 5 223.48 25.70 -1 15 5 192.08 25.40 1 15 -5 200.78 25.50 -1 15 5 181.88 21.40 0 -15 -5 1908.51 62.99 0 -15 5 1922.01 65.09 0 -15 -5 1884.71 62.79 0 -15 -5 1840.32 60.89 0 -15 5 1806.72 61.99 0 15 -5 1866.41 61.69 0 15 -5 1852.11 64.69 0 15 5 1908.51 65.79 0 15 5 1858.51 63.19 0 15 5 1820.12 64.09 1 -15 5 -2.70 14.30 1 -15 5 1.90 3.80 -1 15 -5 8.30 3.00 1 15 5 3.00 16.10 2 -15 5 471.65 45.80 2 -15 5 376.96 28.70 2 -15 5 420.16 18.50 2 15 5 383.36 32.90 -2 15 -5 403.06 15.70 3 -15 5 125.79 23.60 3 -15 5 122.19 11.30 3 15 5 115.19 27.60 -3 15 -5 154.18 8.30 3 -16 -5 15.50 7.20 3 -16 -5 45.90 35.80 -3 -16 5 6.20 27.30 3 -16 -5 18.50 6.50 -3 16 5 16.50 6.50 -3 16 5 24.80 35.20 3 16 -5 40.10 7.10 -2 -16 5 16.40 19.70 2 -16 -5 5.10 5.30 2 -16 -5 4.50 4.20 2 -16 -5 2.10 21.10 -2 16 5 8.60 32.80 2 16 -5 8.80 4.50 -2 16 5 10.70 4.70 -2 16 5 16.20 23.60 2 16 -5 9.90 23.90 1 -16 -5 371.26 15.40 1 -16 -5 399.16 26.50 -1 -16 5 370.56 26.40 1 -16 -5 371.06 17.10 -1 16 5 406.86 29.80 -1 16 5 398.46 31.20 1 16 -5 379.36 16.10 1 16 -5 417.36 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-20 -9 4.90 6.00 0 20 -9 -4.70 7.80 1 -20 9 3.10 8.90 -1 20 -9 18.70 6.50 1 -21 -9 7.50 6.60 -1 -21 9 0.30 8.50 1 21 -9 -1.10 7.70 0 -21 -9 4.20 7.10 0 -21 -9 -1.70 5.20 0 21 -9 0.40 7.70 1 -21 9 46.30 10.90 -1 21 -9 38.90 7.60 1 -22 -9 72.79 7.70 -1 -22 9 59.79 12.60 1 22 -9 49.30 9.30 0 -22 -9 -1.10 6.90 0 -22 -9 -2.00 5.90 0 -22 9 8.80 10.40 0 22 -9 -13.10 7.50 1 -22 9 42.40 9.90 -1 22 -9 25.30 7.90 1 -23 -9 15.50 7.60 1 23 -9 29.80 10.10 0 -23 9 -22.00 13.00 0 -23 -9 -7.70 6.00 0 23 -9 2.30 7.90 2 0 -10 87.89 11.10 2 0 -10 56.49 40.10 -2 0 10 67.89 9.00 1 0 -10 1.70 23.80 -1 0 10 -2.20 24.90 0 0 -10 252.97 12.60 0 0 10 287.87 30.50 0 0 -10 282.77 28.10 2 -1 -10 36.40 8.50 -2 1 10 -1.20 9.20 2 1 -10 29.20 7.60 2 1 -10 32.10 36.10 -1 -1 10 -16.70 25.90 1 -1 -10 -2.30 6.10 1 -1 -10 5.90 26.90 1 1 -10 -7.70 26.90 -1 1 10 4.60 24.20 0 -1 -10 136.29 12.60 0 -1 10 172.98 22.90 0 -1 -10 130.29 9.10 0 1 -10 161.58 9.70 0 1 10 139.19 22.60 0 1 -10 193.28 22.40 2 -2 -10 133.59 11.90 -2 -2 10 101.89 12.60 2 2 -10 116.49 12.20 2 2 -10 110.69 38.00 -2 2 10 128.59 12.70 1 -2 -10 19.80 5.90 -1 -2 10 -6.30 25.20 -1 2 10 32.40 25.00 1 2 -10 13.60 25.30 1 2 -10 -7.90 6.50 0 -2 -10 3.70 5.50 0 -2 -10 17.90 4.40 0 2 -10 26.60 5.00 0 2 10 8.60 20.80 0 2 -10 26.10 21.60 2 -3 -10 132.29 14.10 2 -3 -10 154.68 38.80 -2 3 10 140.29 15.30 2 3 -10 154.38 40.60 2 3 -10 123.29 14.10 1 -3 -10 11.30 6.00 -1 -3 10 2.80 25.80 1 3 -10 2.00 27.40 -1 3 10 18.20 24.20 1 3 -10 1.80 7.00 0 -3 -10 127.89 10.00 0 -3 -10 143.19 9.90 0 3 -10 134.79 8.60 0 3 10 154.88 23.30 0 3 -10 183.48 23.50 2 -3 10 36.60 7.10 2 -4 -10 23.80 38.10 -2 -4 10 39.20 9.40 2 4 -10 39.80 39.30 2 4 -10 47.00 8.30 -2 4 10 14.10 8.60 1 -4 -10 1.00 6.10 -1 -4 10 12.00 25.30 1 4 -10 8.50 6.40 -1 4 10 14.50 24.90 1 4 -10 31.50 29.40 0 -4 -10 8.40 4.50 0 -4 -10 17.50 5.00 0 4 10 9.00 20.40 0 4 -10 28.40 22.60 0 4 -10 30.50 4.70 2 -4 10 84.39 10.50 -2 -5 10 3.80 8.00 2 -5 -10 4.20 7.40 2 5 -10 -14.20 49.70 -2 5 10 21.00 7.60 2 5 -10 3.10 8.30 -1 -5 10 -3.60 24.20 1 5 -10 16.80 30.00 1 5 -10 -4.00 5.70 -1 5 10 6.70 27.80 0 -5 -10 25.00 5.10 0 -5 -10 21.30 4.80 0 5 -10 5.80 23.60 0 5 10 40.70 21.50 0 5 -10 18.10 4.90 2 -5 10 192.18 14.50 2 -6 -10 65.69 8.60 2 6 -10 87.49 10.50 -2 6 10 91.09 9.50 -1 -6 10 32.70 24.50 1 -6 -10 6.50 6.00 1 6 -10 24.90 30.90 1 6 -10 17.20 5.60 -1 6 10 42.30 28.90 0 -6 -10 183.08 10.10 0 -6 -10 154.48 10.40 0 6 -10 160.68 10.30 0 6 -10 195.58 25.80 0 6 10 218.28 25.10 2 -6 10 22.60 8.40 2 -7 -10 -1.20 7.10 -2 -7 10 18.70 7.50 -2 7 10 12.40 9.90 2 7 -10 21.30 8.70 1 -7 -10 -8.50 6.20 1 7 -10 -8.60 30.40 1 7 -10 17.50 7.40 -1 7 10 14.50 24.10 0 -7 -10 7.20 4.70 0 -7 -10 12.10 4.60 0 7 -10 18.20 4.90 0 7 10 13.60 22.20 0 7 -10 43.20 25.40 -1 7 -10 9.60 5.60 2 -7 10 7.60 8.10 -2 -8 10 46.60 8.40 2 -8 -10 43.00 7.40 2 8 -10 65.49 9.60 -2 8 10 52.29 11.00 1 -8 -10 140.89 32.60 -1 8 10 141.19 30.90 1 8 -10 151.68 32.70 1 8 -10 138.79 10.50 0 -8 -10 11.00 4.60 0 -8 -10 3.60 4.60 0 8 -10 -1.00 4.80 0 8 -10 -19.10 25.50 0 8 10 -11.90 22.50 2 -8 10 42.00 8.20 -2 -9 10 16.80 10.40 2 -9 -10 -9.40 7.00 2 9 -10 27.20 9.00 -2 9 10 -14.90 9.90 1 -9 -10 23.40 6.20 1 -9 -10 30.80 26.20 1 9 -10 26.50 32.00 -1 9 10 43.20 24.50 0 -9 -10 15.80 5.10 0 -9 -10 19.80 4.70 0 9 -10 7.60 5.10 0 9 10 7.10 23.70 0 9 -10 11.70 26.40 -1 9 -10 79.09 9.10 2 -9 10 19.70 8.70 2 -10 -10 -12.80 8.50 -2 10 10 20.50 10.30 1 -10 -10 91.69 9.90 1 -10 -10 103.19 27.10 1 10 -10 104.69 11.90 -1 10 10 104.99 28.50 1 10 -10 77.79 38.10 0 -10 -10 93.79 8.30 0 -10 -10 73.99 8.10 0 10 -10 75.89 7.70 0 10 10 91.79 25.10 0 10 -10 90.29 28.70 -1 10 -10 27.10 5.20 -1 10 -10 40.30 6.00 2 -10 10 17.70 8.10 -2 11 10 -17.10 8.20 2 11 -10 4.60 8.80 1 -11 -10 6.50 27.20 1 -11 -10 2.10 6.00 1 11 -10 30.30 6.80 1 11 -10 0.60 37.70 -1 11 10 24.50 27.80 0 -11 -10 7.10 5.10 0 11 10 5.70 24.90 0 11 -10 4.40 27.00 0 11 -10 8.50 5.90 -1 11 -10 26.80 6.70 -1 11 -10 25.40 5.10 2 -11 10 -1.60 8.40 2 -12 -10 -8.40 7.40 -2 12 10 10.80 8.60 2 12 -10 24.40 11.40 1 -12 -10 128.69 11.20 1 -12 -10 168.68 29.60 -1 12 10 207.08 34.70 1 12 -10 169.98 42.20 1 12 -10 182.38 14.60 0 -12 -10 3.40 5.40 0 -12 -10 11.20 5.40 0 12 -10 -0.60 5.50 0 12 10 11.80 28.40 0 12 -10 26.20 30.30 -1 12 -10 17.50 6.60 -1 12 -10 27.30 5.50 -2 13 10 9.20 11.80 2 13 -10 32.70 9.60 1 -13 -10 -0.90 34.90 1 13 -10 35.90 7.10 -1 13 10 39.70 34.40 0 -13 -10 10.20 5.20 0 13 -10 -8.50 5.70 0 13 -10 19.40 35.60 0 13 10 3.10 26.80 1 -13 10 156.88 12.80 -1 13 -10 141.79 11.50 -1 13 -10 130.59 10.50 2 -14 -10 6.90 8.30 -2 14 10 29.90 10.80 2 14 -10 18.90 12.20 1 -14 -10 74.79 9.80 1 -14 -10 141.99 32.50 -1 14 10 131.39 36.30 1 14 -10 97.09 10.00 0 -14 -10 49.90 6.60 0 14 -10 73.89 9.70 0 14 10 69.59 29.00 1 -14 10 40.40 9.10 -1 14 -10 35.20 7.30 -1 14 -10 46.40 6.30 2 -15 -10 -3.70 10.00 2 15 -10 -1.50 9.00 1 -15 -10 -9.60 6.80 1 15 -10 23.60 7.20 -1 15 10 -23.70 33.80 0 -15 -10 30.80 6.70 0 -15 -10 53.49 5.90 0 15 -10 42.70 7.00 1 -15 10 24.10 9.00 -1 15 -10 4.10 6.30 1 -16 -10 57.99 7.80 1 16 -10 49.30 8.10 0 -16 10 14.00 7.70 0 -16 -10 -0.70 6.00 0 16 -10 9.80 7.10 1 -16 10 6.30 10.50 -1 16 -10 4.80 6.40 1 -17 -10 4.60 6.80 1 17 -10 -10.80 9.60 0 -17 -10 3.40 5.70 0 -17 -10 19.60 6.20 0 -17 10 20.00 11.60 0 17 -10 -8.40 6.90 1 -17 10 -21.40 10.10 -1 17 -10 1.90 6.30 1 -18 -10 29.70 7.50 1 18 -10 15.00 11.40 0 -18 10 39.30 10.80 0 -18 -10 18.60 5.90 0 -18 -10 17.80 7.00 0 18 -10 24.90 7.10 1 -19 -10 1.80 7.60 1 19 -10 -3.10 8.00 0 -19 -10 44.70 7.10 0 -19 -10 32.20 6.30 0 -19 10 62.09 11.10 0 19 -10 45.60 8.90 0 -20 10 59.09 11.50 0 -20 -10 31.30 6.20 0 20 -10 35.50 8.60 -2 0 11 -23.40 9.40 2 0 -11 14.70 11.10 1 0 -11 231.98 15.30 -1 0 11 363.86 35.10 0 0 -11 -5.90 5.70 0 0 -11 15.30 5.40 2 -1 -11 35.40 10.20 -2 -1 11 50.89 11.90 -1 -1 11 80.79 40.10 1 -1 -11 6.50 8.20 -1 1 11 11.80 32.30 0 -1 -11 10.00 5.70 0 -1 -11 29.40 6.30 0 1 -11 19.80 5.30 0 1 11 16.10 27.60 0 1 -11 2.80 6.60 2 -2 -11 38.00 9.30 2 2 -11 20.40 9.20 1 -2 -11 13.70 7.40 -1 -2 11 40.30 32.70 1 2 -11 19.30 7.30 1 2 -11 30.80 39.50 -1 2 11 32.50 36.80 0 -2 -11 14.20 5.30 0 -2 -11 0.70 5.70 0 2 -11 -14.20 6.50 0 2 11 -15.80 27.40 0 2 -11 0.60 5.30 -2 -3 11 6.30 10.40 2 3 -11 13.00 10.10 1 -3 -11 65.99 36.40 -1 -3 11 59.89 29.60 1 -3 -11 54.09 9.30 -1 3 11 89.89 31.00 1 3 -11 66.09 10.10 0 -3 -11 6.10 5.60 0 -3 -11 17.00 6.00 0 3 -11 3.70 5.40 0 3 -11 6.20 10.80 0 3 11 -2.20 28.40 2 -4 -11 63.19 10.00 -2 -4 11 61.39 12.70 2 4 -11 82.09 11.80 -2 4 11 123.99 16.40 1 -4 -11 16.00 7.60 -1 -4 11 16.70 33.30 1 -4 -11 22.20 34.90 -1 4 11 36.50 36.10 1 4 -11 30.10 7.10 0 -4 -11 16.20 6.20 0 -4 -11 7.00 5.70 0 4 11 -3.90 28.90 0 4 -11 15.60 5.50 0 4 -11 1.30 22.10 -2 -5 11 27.40 10.30 2 -5 -11 25.10 8.80 -2 5 11 23.00 11.40 2 5 -11 5.80 11.90 1 -5 -11 14.70 39.80 -1 -5 11 39.00 30.60 1 -5 -11 34.10 6.50 -1 5 11 43.70 28.90 1 5 -11 28.90 9.00 0 -5 -11 14.20 5.80 0 -5 -11 3.60 6.40 0 5 -11 7.40 30.50 0 5 -11 21.30 5.90 0 5 11 -9.50 29.00 -2 -6 11 46.10 10.30 2 -6 -11 35.90 9.50 2 6 -11 46.90 10.00 1 -6 -11 30.50 8.00 -1 6 11 34.80 35.70 1 6 -11 50.79 7.00 0 -6 -11 6.90 5.70 0 -6 -11 0.10 6.10 0 6 -11 8.10 6.10 0 6 -11 19.70 28.90 0 6 11 12.60 32.30 2 -7 -11 32.10 9.70 -2 -7 11 1.20 13.00 2 7 -11 20.60 10.20 1 7 -11 43.90 8.60 -1 7 11 25.10 35.70 0 -7 -11 39.20 6.10 0 7 -11 53.69 30.50 0 7 -11 40.10 6.00 2 -8 -11 16.40 12.00 2 8 -11 69.49 11.10 1 -8 -11 -10.70 6.70 1 8 -11 33.20 7.00 0 -8 -11 13.90 6.10 0 -8 -11 4.50 5.90 0 8 -11 18.00 33.60 0 8 -11 16.10 6.00 1 -9 -11 18.00 8.00 1 9 -11 61.39 9.00 0 -9 -11 109.39 10.20 0 -9 -11 85.69 9.60 0 9 -11 77.89 7.80 0 9 -11 84.49 38.60 1 10 -11 9.40 9.50 0 10 -11 8.70 7.10 -1 10 -11 3.60 7.50 1 -11 -11 -21.40 7.60 1 11 -11 4.80 7.50 0 -11 -11 157.48 10.80 0 11 -11 111.59 12.50 1 -11 11 7.30 9.80 -1 11 -11 -5.20 5.90 1 12 -11 20.60 8.30 0 -12 -11 0.70 6.50 0 12 -11 15.20 7.50 1 -13 -11 33.00 8.80 1 13 -11 51.19 10.10 0 -13 -11 70.69 7.30 0 13 -11 70.49 8.50 1 -14 -11 17.60 7.80 1 14 -11 33.60 10.90 0 14 -11 2.40 8.40 0 -15 -11 44.20 6.90 1 0 -12 -26.90 10.20 0 0 -12 18.90 6.30 1 -1 -12 -20.00 9.40 1 1 -12 -13.10 11.00 0 -1 -12 44.30 6.90 0 1 -12 26.20 6.70 1 -2 -12 -2.50 8.50 1 2 -12 16.90 10.10 0 -2 -12 78.39 10.30 0 -3 -12 150.68 11.70 0 3 -12 136.69 12.30 0 -4 -12 34.30 6.90 0 4 -12 48.90 7.60 0 -5 -12 104.09 10.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 82090 _shelx_res_file ; 1.res created by SHELXL-2014/7 TITL RC141_0m_a.res in P2(1)/n REM Old TITL RC141_0m in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.141, Rweak 0.016, Alpha 0.033, Orientation as input REM Formula found by SHELXT: C10 N5 S CELL 0.71073 3.7856 28.3927 9.6324 90 93.824 90 ZERR 4 0.0004 0.0026 0.0009 0 0.003 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O S UNIT 32 40 24 4 4 EQIV $1 1-X,1-Y,1-Z EQIV $2 -1+X,+Y,1+Z EQIV $3 1+X,+Y,+Z DFIX 0.86 0.01 N6 H6a N6 H6b N5 H5a N5 H5b DFIX 0.84 0.01 O1 H1a O1 H1b L.S. 10 PLAN 10 SIZE 0.28 0.08 0.04 TEMP 22.85 HTAB N5 N2 HTAB N5 N4_$1 HTAB N6 O1_$2 HTAB N6 O1_$1 HTAB O1 N1 HTAB O1 N2_$3 BOND $H LIST 4 CONF fmap 2 acta REM REM REM WGHT 0.013100 1.761600 FVAR 0.90656 S1 5 0.144484 0.726658 0.183853 11.00000 0.04715 0.02829 = 0.03754 -0.00026 0.00106 0.00392 N1 3 0.402134 0.657911 0.049241 11.00000 0.04565 0.03156 = 0.02986 -0.00036 0.00436 -0.00337 N2 3 0.295305 0.635956 0.274941 11.00000 0.03624 0.02954 = 0.02946 0.00314 0.00277 0.00169 N3 3 0.180450 0.651552 0.390514 11.00000 0.03316 0.02863 = 0.03127 0.00076 0.00180 0.00126 N4 3 0.261080 0.544340 0.611564 11.00000 0.03420 0.02654 = 0.02925 0.00111 0.00478 0.00326 N5 3 0.424554 0.552572 0.389897 11.00000 0.05551 0.02641 = 0.03313 0.00342 0.01267 0.01003 N6 3 0.104136 0.534040 0.834341 11.00000 0.06386 0.03587 = 0.03307 0.00281 0.01510 0.01117 C1 1 0.237750 0.735167 0.013294 11.00000 0.05317 0.03244 = 0.03724 0.00764 -0.00825 -0.00674 AFIX 43 H1 2 0.202202 0.763227 -0.035454 11.00000 -1.20000 AFIX 0 C2 1 0.369065 0.695597 -0.039510 11.00000 0.05425 0.03859 = 0.02985 0.00408 0.00345 -0.01021 AFIX 43 H2 2 0.433706 0.693866 -0.130839 11.00000 -1.20000 AFIX 0 C3 1 0.293061 0.669199 0.170556 11.00000 0.03215 0.02610 = 0.03231 -0.00058 0.00020 -0.00266 C4 1 0.170689 0.620524 0.497761 11.00000 0.03046 0.02590 = 0.02872 0.00069 0.00056 0.00147 C5 1 0.287252 0.572055 0.499280 11.00000 0.02730 0.02659 = 0.03004 -0.00267 0.00284 0.00020 C6 1 0.124842 0.562261 0.724616 11.00000 0.03092 0.03089 = 0.03009 0.00019 0.00330 0.00018 C7 1 0.008112 0.609752 0.733012 11.00000 0.03920 0.03272 = 0.03140 -0.00429 0.00818 0.00538 AFIX 43 H7 2 -0.084533 0.621231 0.813391 11.00000 -1.20000 AFIX 0 C8 1 0.035903 0.637602 0.620897 11.00000 0.03763 0.02722 = 0.03554 -0.00192 0.00208 0.00648 AFIX 43 H8 2 -0.035735 0.668874 0.624986 11.00000 -1.20000 AFIX 0 O1 4 0.791225 0.569588 0.091044 11.00000 0.06206 0.03852 = 0.04741 -0.00063 0.01235 0.00451 H5A 2 0.470902 0.569836 0.320234 11.00000 0.03972 H5B 2 0.504441 0.524213 0.397148 11.00000 0.04680 H6A 2 0.166164 0.505013 0.825544 11.00000 0.05763 H6B 2 0.021724 0.543760 0.910268 11.00000 0.05186 H1A 2 0.646914 0.590486 0.062157 11.00000 0.11135 H1B 2 0.936056 0.584046 0.145489 11.00000 0.23394 HKLF 4 REM RC141_0m_a.res in P2(1)/n REM R1 = 0.0607 for 1670 Fo > 4sig(Fo) and 0.0822 for all 2100 data REM 169 parameters refined using 6 restraints END WGHT 0.0131 1.7616 REM Highest difference peak 0.327, deepest hole -0.261, 1-sigma level 0.057 Q1 1 0.1583 0.7328 0.0811 11.00000 0.05 0.33 Q2 1 0.0230 0.7411 0.2613 11.00000 0.05 0.26 Q3 1 0.5774 0.5538 0.0227 11.00000 0.05 0.23 Q4 1 0.7446 0.7192 0.0156 11.00000 0.05 0.22 Q5 1 0.1486 0.5943 0.5005 11.00000 0.05 0.22 Q6 1 -0.0173 0.6231 0.5434 11.00000 0.05 0.22 Q7 1 0.2038 0.6915 0.1883 11.00000 0.05 0.22 Q8 1 0.1886 0.6313 0.5577 11.00000 0.05 0.22 Q9 1 0.3142 0.6004 0.5155 11.00000 0.05 0.21 Q10 1 -0.0647 0.6880 0.1753 11.00000 0.05 0.21 ; _shelx_res_checksum 41697 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_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy S S1 0.1445(2) 0.72666(3) 0.18385(9) 0.0377(2) Uani d 1 N N1 0.4021(8) 0.65791(9) 0.0492(3) 0.0356(6) Uani d 1 N N2 0.2953(7) 0.63596(9) 0.2749(3) 0.0317(6) Uani d 1 N N3 0.1805(7) 0.65155(9) 0.3905(3) 0.0310(6) Uani d 1 N N4 0.2611(7) 0.54434(8) 0.6116(3) 0.0299(6) Uani d 1 N N5 0.4246(8) 0.55257(10) 0.3899(3) 0.0379(7) Uani d 1 N N6 0.1041(9) 0.53404(10) 0.8343(3) 0.0437(8) Uani d 1 C C1 0.2378(10) 0.73517(12) 0.0133(4) 0.0415(8) Uani d 1 H H1 0.2022 0.7632 -0.0355 0.050 Uiso calc 1 C C2 0.3691(10) 0.69560(12) -0.0395(4) 0.0409(8) Uani d 1 H H2 0.4337 0.6939 -0.1308 0.049 Uiso calc 1 C C3 0.2931(8) 0.66920(10) 0.1706(3) 0.0303(7) Uani d 1 C C4 0.1707(8) 0.62052(10) 0.4978(3) 0.0284(7) Uani d 1 C C5 0.2873(8) 0.57206(10) 0.4993(3) 0.0279(7) Uani d 1 C C6 0.1248(8) 0.56226(10) 0.7246(3) 0.0306(7) Uani d 1 C C7 0.0081(9) 0.60975(11) 0.7330(3) 0.0342(7) Uani d 1 H H7 -0.0845 0.6212 0.8134 0.041 Uiso calc 1 C C8 0.0359(8) 0.63760(11) 0.6209(3) 0.0335(7) Uani d 1 H H8 -0.0357 0.6689 0.6250 0.040 Uiso calc 1 O O1 0.7912(8) 0.56959(9) 0.0910(3) 0.0489(7) Uani d 1 H H5A 0.471(9) 0.5698(10) 0.320(2) 0.040(10) Uiso d 1 H H5B 0.504(9) 0.5242(6) 0.397(4) 0.047(11) Uiso d 1 H H6A 0.166(10) 0.5050(5) 0.826(4) 0.058(12) Uiso d 1 H H6B 0.022(10) 0.5438(12) 0.910(2) 0.052(12) Uiso d 1 H H1A 0.647(12) 0.5905(15) 0.062(6) 0.11(2) Uiso d 1 H H1B 0.936(19) 0.584(3) 0.145(8) 0.23(5) Uiso d 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.0472(5) 0.0283(4) 0.0375(5) 0.0039(4) 0.0011(4) -0.0003(3) N1 0.0457(16) 0.0316(14) 0.0299(15) -0.0034(12) 0.0044(13) -0.0004(11) N2 0.0362(15) 0.0295(13) 0.0295(15) 0.0017(11) 0.0028(12) 0.0031(11) N3 0.0332(14) 0.0286(13) 0.0313(15) 0.0013(11) 0.0018(12) 0.0008(11) N4 0.0342(14) 0.0265(13) 0.0292(14) 0.0033(11) 0.0048(12) 0.0011(10) N5 0.0555(19) 0.0264(14) 0.0331(16) 0.0100(13) 0.0127(14) 0.0034(12) N6 0.064(2) 0.0359(16) 0.0331(17) 0.0112(15) 0.0151(15) 0.0028(13) C1 0.053(2) 0.0324(17) 0.037(2) -0.0067(15) -0.0083(17) 0.0076(14) C2 0.054(2) 0.0386(18) 0.0298(18) -0.0102(16) 0.0034(16) 0.0041(14) C3 0.0321(17) 0.0261(15) 0.0323(18) -0.0027(12) 0.0002(14) -0.0006(12) C4 0.0305(16) 0.0259(14) 0.0287(16) 0.0015(12) 0.0006(13) 0.0007(12) C5 0.0273(15) 0.0266(15) 0.0300(17) 0.0002(12) 0.0028(13) -0.0027(12) C6 0.0309(16) 0.0309(16) 0.0301(17) 0.0002(13) 0.0033(14) 0.0002(12) C7 0.0392(18) 0.0327(16) 0.0314(18) 0.0054(14) 0.0082(15) -0.0043(13) C8 0.0376(18) 0.0272(15) 0.0355(19) 0.0065(13) 0.0021(15) -0.0019(13) O1 0.0621(18) 0.0385(14) 0.0474(16) 0.0045(13) 0.0123(14) -0.0006(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C1 S1 C3 88.47(16) C3 N1 C2 110.2(3) N3 N2 C3 113.9(2) N2 N3 C4 117.2(2) C6 N4 C5 119.0(2) C5 N5 H5A 120(2) C5 N5 H5B 119(2) H5A N5 H5B 121(3) C6 N6 H6A 118(3) C6 N6 H6B 122(3) H6A N6 H6B 120(4) S1 C1 H1 124.8 C2 C1 S1 110.4(3) C2 C1 H1 124.8 N1 C2 H2 122.0 C1 C2 N1 116.0(3) C1 C2 H2 122.0 N1 C3 S1 114.9(2) N1 C3 N2 119.9(3) N2 C3 S1 125.2(2) N3 C4 C5 126.9(3) N3 C4 C8 116.5(3) C8 C4 C5 116.5(3) N4 C5 C4 121.7(3) N5 C5 N4 116.6(3) N5 C5 C4 121.7(3) N4 C6 C7 123.0(3) N6 C6 N4 117.6(3) N6 C6 C7 119.3(3) C6 C7 H7 121.0 C8 C7 C6 118.0(3) C8 C7 H7 121.0 C4 C8 H8 119.2 C7 C8 C4 121.6(3) C7 C8 H8 119.2 H1A O1 H1B 104(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 C1 1.720(4) S1 C3 1.733(3) N1 C2 1.370(4) N1 C3 1.305(4) N2 N3 1.300(3) N2 C3 1.379(4) N3 C4 1.360(4) N4 C5 1.347(4) N4 C6 1.336(4) N5 C5 1.326(4) N5 H5A 0.858(10) N5 H5B 0.861(10) N6 C6 1.333(4) N6 H6A 0.863(10) N6 H6B 0.860(10) C1 H1 0.9300 C1 C2 1.342(5) C2 H2 0.9300 C4 C5 1.445(4) C4 C8 1.408(4) C6 C7 1.423(4) C7 H7 0.9300 C7 C8 1.348(4) C8 H8 0.9300 O1 H1A 0.841(10) O1 H1B 0.840(10) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C2 H2 S1 4_675 0.93 3.02 3.665(3) 128.1 N5 H5A N2 . 0.859(10) 2.03(3) 2.645(4) 128(3) N5 H5A O1 . 0.859(10) 2.59(2) 3.314(4) 143(3) N5 H5B N4 3_666 0.861(10) 2.143(12) 2.998(4) 172(3) N6 H6A O1 3_666 0.863(10) 2.27(2) 3.048(4) 151(4) N6 H6B O1 1_456 0.860(10) 2.129(11) 2.988(4) 177(4) O1 H1A N1 . 0.841(10) 2.13(3) 2.923(4) 158(6) O1 H1B N2 1_655 0.840(10) 2.31(2) 3.143(4) 170(9) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion S1 C1 C2 N1 -0.1(4) N2 N3 C4 C5 2.5(5) N2 N3 C4 C8 -178.2(3) N3 N2 C3 S1 -1.5(4) N3 N2 C3 N1 -180.0(3) N3 C4 C5 N4 -179.3(3) N3 C4 C5 N5 0.5(5) N3 C4 C8 C7 178.8(3) N4 C6 C7 C8 0.3(5) N6 C6 C7 C8 179.3(3) C1 S1 C3 N1 0.1(3) C1 S1 C3 N2 -178.5(3) C2 N1 C3 S1 -0.2(4) C2 N1 C3 N2 178.4(3) C3 S1 C1 C2 0.0(3) C3 N1 C2 C1 0.2(5) C3 N2 N3 C4 179.2(3) C5 N4 C6 N6 -179.6(3) C5 N4 C6 C7 -0.7(5) C5 C4 C8 C7 -1.8(5) C6 N4 C5 N5 179.9(3) C6 N4 C5 C4 -0.3(4) C6 C7 C8 C4 1.0(5) C8 C4 C5 N4 1.4(4) C8 C4 C5 N5 -178.8(3) _cod_database_fobs_code 2242433