#------------------------------------------------------------------------------ #$Date: 2020-09-16 08:04:07 +0300 (Wed, 16 Sep 2020) $ #$Revision: 256454 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/90/1559092.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_1559092 loop_ _publ_author_name 'Chakkarapani, Nandhini' 'Murugan, Suganya' 'Ibrahim, Abdul Razak' 'Kavitha, Savaridasan Jose' 'Hemamalini, Madhukar' 'Rajakannan, Venkatachalam' _publ_section_title ; 2,6-Diamino-4-chloropyrimidine--succinic acid (2/1) ; _journal_coeditor_code HB4365 _journal_issue 9 _journal_name_full IUCrData _journal_page_first x201239 _journal_paper_doi 10.1107/S2414314620012390 _journal_volume 5 _journal_year 2020 _chemical_formula_iupac '2C4 H5 Cl N4, C4 H6 O4' _chemical_formula_moiety '2(C4 H5 Cl N4), C4 H6 O4' _chemical_formula_sum 'C12 H16 Cl2 N8 O4' _chemical_formula_weight 407.23 _chemical_name_systematic ; 2,6-Diamino-4-chloropyrimidine--succinic acid (2/1) ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 98.603(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 13.2096(14) _cell_length_b 4.9765(5) _cell_length_c 13.5673(14) _cell_measurement_reflns_used 3778 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 29.85 _cell_measurement_theta_min 2.62 _cell_volume 881.85(16) _computing_cell_refinement ; APEX2 and SAINT (Bruker, 2009) ; _computing_data_collection ; APEX2 (Bruker, 2009) ; _computing_data_reduction ; SAINT and XPREP (Bruker, 2009) ; _computing_molecular_graphics ; PLATON (Spek, 2020) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker SMART APEXII CCD ' _diffrn_measurement_method '\w and \f scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_unetI/netI 0.0194 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 15031 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.185 _diffrn_reflns_theta_min 1.559 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.406 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_correction_T_min 0.6310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 420 _exptl_crystal_size_max 0.720 _exptl_crystal_size_mid 0.340 _exptl_crystal_size_min 0.130 _refine_diff_density_max 0.332 _refine_diff_density_min -0.437 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 118 _refine_ls_number_reflns 2599 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0434 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+0.3195P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1171 _refine_ls_wR_factor_ref 0.1282 _reflns_number_gt 2102 _reflns_number_total 2599 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb4365sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1559092 _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 0.759 _shelx_estimated_absorpt_t_max 0.949 _shelx_hkl_file ; 1 0 0 26.1237 0.72411 4 1 0 0 28.0819 0.75133 1 -1 0 0 30.6764 0.72150 3 -2 0 0 0.68228 0.17978 2 2 0 0 1.50393 0.24170 1 2 0 0 1.19496 0.22056 4 2 0 0 1.07916 0.18879 2 -2 0 0 1.96479 0.21962 3 -3 0 0 515.706 11.1009 3 -3 0 0 502.507 11.0493 2 3 0 0 495.177 11.0352 2 3 0 0 503.453 11.1441 4 3 0 0 474.910 11.2008 1 -4 0 0 1459.58 30.9817 3 4 0 0 1387.22 30.6897 4 4 0 0 1389.94 30.8164 1 4 0 0 1376.27 30.5439 2 -4 0 0 1420.48 30.5751 2 5 0 0 1955.27 43.4418 4 5 0 0 1950.27 43.6101 1 5 0 0 2033.72 43.5959 2 -5 0 0 2042.21 43.8058 3 6 0 0 1605.09 35.8434 1 6 0 0 1622.49 35.6319 4 -6 0 0 1662.06 35.5889 3 6 0 0 1605.92 35.3850 2 7 0 0 53.8907 2.12625 1 -7 0 0 57.3550 1.94839 3 7 0 0 61.2213 1.81838 2 7 0 0 56.0668 1.97854 4 8 0 0 9.21394 0.61560 2 -8 0 0 8.74233 0.70375 3 8 0 0 9.98086 0.77214 4 8 0 0 8.14164 0.93184 1 9 0 0 106.732 3.61868 1 9 0 0 110.274 3.38443 4 -9 0 0 104.524 3.29759 3 9 0 0 108.467 3.03049 2 -10 0 0 15.6594 1.05077 3 10 0 0 15.4765 1.09063 4 10 0 0 15.9338 1.27675 1 10 0 0 14.9157 0.86276 2 -11 0 0 46.4336 2.04708 3 11 0 0 51.1779 2.46297 1 11 0 0 43.3541 2.02929 4 12 0 0 59.6021 2.49026 4 12 0 0 57.4944 2.77780 1 -12 0 0 53.2340 2.33691 3 13 0 0 172.157 5.37867 4 13 0 0 181.098 5.99434 1 14 0 0 48.9361 2.45392 4 14 0 0 47.5645 2.78018 1 15 0 0 20.4668 1.86874 1 15 0 0 25.8757 1.79000 4 16 0 0 12.0882 1.47978 4 16 0 0 9.23193 1.55654 1 17 0 0 6.93452 1.22776 4 17 0 0 7.56102 1.50131 1 18 0 0 4.26062 1.15725 1 18 0 0 3.78632 1.02373 4 0 -1 0 -0.4325 0.07247 2 0 -1 0 -0.2536 0.09869 4 0 1 0 -0.5127 0.06471 2 0 1 0 -0.5628 0.06323 1 0 1 0 -0.4881 0.06520 4 0 1 0 -0.4507 0.06736 3 1 -1 0 21.3911 0.83026 4 1 -1 0 22.0677 0.76137 1 1 -1 0 20.8894 0.85423 2 -1 -1 0 20.8543 0.79436 3 -1 1 0 21.4296 0.84069 4 1 1 0 24.2813 0.78101 4 1 1 0 20.7977 0.80049 3 1 1 0 21.7433 0.80058 1 1 1 0 22.3913 0.75260 2 -1 1 0 21.3478 0.76215 1 -1 1 0 21.3255 0.91240 3 -1 1 0 20.1065 0.84648 2 2 -1 0 0.68133 0.20120 4 2 -1 0 0.76167 0.22761 2 2 -1 0 0.39500 0.14543 1 -2 -1 0 0.65673 0.14863 3 -2 1 0 0.14269 0.16546 2 -2 1 0 0.35723 0.19401 3 2 1 0 0.60835 0.14130 4 2 1 0 0.50838 0.17673 1 2 1 0 1.01048 0.14913 2 3 -1 0 761.579 16.8409 1 3 -1 0 770.576 17.0176 4 -3 -1 0 758.622 16.6275 3 3 -1 0 759.448 17.0643 2 -3 1 0 748.656 17.0606 2 3 1 0 762.246 16.5669 2 -3 1 0 762.898 17.1815 3 3 1 0 746.383 17.0005 1 3 1 0 777.543 16.7078 4 4 -1 0 3.29810 0.45811 4 4 -1 0 2.74250 0.44565 2 4 -1 0 4.01865 0.45338 1 -4 -1 0 2.80193 0.24379 3 -4 1 0 3.82701 0.53862 3 -4 1 0 4.04069 0.53003 2 4 1 0 4.00305 0.51695 1 4 1 0 3.33784 0.35816 4 -5 -1 0 137.943 3.20442 3 5 -1 0 125.933 3.64918 2 5 -1 0 129.261 3.65985 4 5 -1 0 130.533 3.54750 1 5 1 0 134.973 3.39104 4 -5 1 0 132.423 3.81858 3 -5 1 0 132.004 3.69727 2 5 1 0 131.543 3.75859 1 6 -1 0 192.704 5.19745 4 6 -1 0 193.194 5.18289 2 6 -1 0 189.387 5.08848 1 -6 -1 0 205.501 4.69089 3 6 1 0 200.280 5.37419 1 -6 1 0 193.065 5.34293 3 -6 1 0 192.894 5.20150 2 6 1 0 203.209 4.29688 2 6 1 0 200.937 4.91316 4 -7 -1 0 301.867 6.83655 3 7 -1 0 296.399 7.36665 2 7 -1 0 288.378 7.38716 4 7 -1 0 295.381 7.34675 1 7 1 0 291.020 7.59799 1 7 1 0 293.668 6.38236 2 -7 1 0 279.622 7.51402 3 7 1 0 289.862 7.06685 4 -7 1 0 291.194 7.38545 2 8 -1 0 169.338 4.86825 1 8 -1 0 176.585 4.84138 2 8 -1 0 175.260 4.90757 4 -8 -1 0 177.843 4.36925 3 8 1 0 172.401 5.13311 1 -8 1 0 162.494 4.98084 3 -8 1 0 174.792 4.88109 2 8 1 0 170.485 3.86261 2 8 1 0 172.104 4.59426 4 -9 -1 0 204.934 5.10970 3 9 -1 0 204.842 5.66663 4 9 -1 0 200.113 5.68681 1 9 -1 0 198.198 5.51144 2 9 1 0 202.382 5.95178 1 -9 1 0 201.106 5.81420 3 9 1 0 197.651 5.33446 4 -10 -1 0 1.83315 0.39220 3 10 -1 0 1.34866 0.55100 1 10 -1 0 0.76974 0.44483 4 10 -1 0 0.62687 0.38560 2 10 1 0 0.48960 0.46523 1 10 1 0 1.47593 0.42675 4 -10 1 0 1.70861 0.54931 3 11 -1 0 14.3142 1.07316 2 11 -1 0 14.1235 1.20018 4 11 -1 0 12.2179 1.36912 1 11 1 0 15.2142 1.07543 4 11 1 0 12.6989 1.52209 1 -11 1 0 13.0679 1.21463 3 12 -1 0 1.90530 0.58952 2 12 -1 0 1.77607 0.61749 4 12 -1 0 3.15366 0.78733 1 12 1 0 2.72540 0.79887 1 -12 1 0 3.61502 0.78079 3 12 1 0 3.44666 0.68380 4 13 -1 0 20.4217 1.56153 4 13 -1 0 24.2822 1.75802 1 -13 1 0 22.0466 1.62616 3 13 1 0 19.9151 1.76810 1 13 1 0 22.7060 1.47013 4 14 -1 0 -0.4736 0.43211 4 14 -1 0 0.98153 0.65621 1 14 1 0 0.03099 0.47491 1 14 1 0 0.33505 0.43467 4 15 -1 0 9.30618 1.37486 4 15 -1 0 7.81703 1.41741 1 15 1 0 8.78220 1.19178 4 15 1 0 6.55568 1.39070 1 16 -1 0 14.1032 1.72283 4 16 -1 0 12.6257 1.80965 1 16 1 0 14.3059 1.99925 1 17 -1 0 -0.4935 0.56488 4 17 -1 0 -0.8708 0.43563 1 17 1 0 1.53137 0.77136 1 18 -1 0 -1.0311 0.45545 1 18 -1 0 -0.8951 0.50912 4 18 1 0 0.43958 0.68071 1 0 -2 0 311.030 7.54684 2 0 -2 0 314.228 7.46933 4 0 2 0 313.547 7.40722 1 0 2 0 312.494 7.55291 2 0 2 0 312.950 7.47049 4 0 2 0 300.368 7.69255 3 -1 -2 0 83.6143 2.53308 2 1 -2 0 88.9032 2.50510 1 1 -2 0 84.0407 2.59750 4 1 -2 0 87.0832 2.71659 2 -1 -2 0 84.0287 2.66991 3 1 2 0 85.5832 2.52032 4 -1 2 0 88.5251 2.72678 2 1 2 0 86.8614 2.56060 1 1 2 0 85.9955 2.69441 3 -1 2 0 84.9392 2.48642 1 1 2 0 89.6337 2.57251 2 -1 2 0 89.8654 2.65322 4 -1 2 0 82.8371 2.82555 3 2 -2 0 150.419 4.22137 2 2 -2 0 148.966 4.09194 4 2 -2 0 149.014 3.87605 1 -2 -2 0 141.892 3.97817 3 -2 -2 0 150.905 3.86078 2 2 2 0 155.190 3.91851 4 2 2 0 148.651 4.02504 1 -2 2 0 150.293 4.38976 3 -2 2 0 147.318 4.21086 2 2 2 0 147.206 4.02530 3 2 2 0 155.404 3.87922 2 3 -2 0 78.6489 2.35175 1 3 -2 0 74.7107 2.63295 2 -3 -2 0 81.4210 2.21545 2 -3 -2 0 75.9624 2.33646 3 3 -2 0 75.4246 2.54212 4 3 2 0 75.7980 2.30160 4 3 2 0 89.7192 2.26174 2 -3 2 0 80.5348 2.84796 3 -3 2 0 75.0259 2.64303 2 3 2 0 74.9314 2.49825 1 4 -2 0 63.1809 2.06881 1 -4 -2 0 64.3211 1.96610 3 4 -2 0 64.6794 2.40563 2 4 -2 0 65.3038 2.31797 4 -4 -2 0 64.6510 1.78274 2 4 2 0 64.3558 1.78404 2 4 2 0 66.2999 2.03481 4 -4 2 0 63.7789 2.40168 2 -4 2 0 67.7299 2.58879 3 4 2 0 60.0097 2.25231 1 5 -2 0 127.977 3.81136 4 5 -2 0 121.912 3.88551 2 5 -2 0 123.688 3.51911 1 -5 -2 0 125.609 3.25441 3 -5 -2 0 124.942 2.94951 2 5 2 0 127.822 3.42304 4 5 2 0 129.561 3.85504 1 -5 2 0 126.623 4.10641 3 -5 2 0 119.580 3.87763 2 6 -2 0 0.09316 0.28039 4 6 -2 0 0.14207 0.21429 1 -6 -2 0 0.43002 0.19565 3 6 -2 0 -0.2523 0.17464 2 -6 2 0 -0.0698 0.21366 2 6 2 0 0.65978 0.36096 1 6 2 0 0.83654 0.27923 4 -6 2 0 0.10862 0.30296 3 7 -2 0 34.1874 1.82104 2 7 -2 0 37.0715 1.62665 1 -7 -2 0 38.3531 1.28667 3 7 -2 0 37.9925 1.80798 4 -7 2 0 36.1519 1.98725 3 7 2 0 38.4709 1.92181 1 -7 2 0 35.3541 1.85153 2 7 2 0 36.7547 1.49773 4 8 -2 0 50.3983 2.30750 2 8 -2 0 48.2692 2.04979 1 8 -2 0 52.4180 2.29453 4 -8 -2 0 52.3125 1.63294 3 -8 2 0 46.2090 2.39081 3 8 2 0 54.2560 2.45101 1 8 2 0 51.8409 1.92919 4 -8 2 0 50.8199 2.33266 2 9 -2 0 50.5174 2.38345 2 9 -2 0 56.2065 2.48168 4 9 -2 0 55.4311 2.30189 1 -9 -2 0 58.7717 1.84687 3 9 2 0 53.7476 2.08610 4 -9 2 0 60.7843 2.78899 3 -9 2 0 54.7203 2.50972 2 9 2 0 51.3823 2.56448 1 10 -2 0 2.29053 0.62522 1 10 -2 0 2.64871 0.71808 4 10 -2 0 2.92193 0.78785 2 -10 2 0 2.74962 0.76872 3 10 2 0 3.33228 0.80455 1 10 2 0 3.64047 0.64719 4 11 -2 0 41.7998 2.26809 4 11 -2 0 42.1529 2.18439 1 11 -2 0 49.8589 2.38947 2 11 2 0 44.9932 2.52294 1 -11 2 0 42.8489 2.47359 3 11 2 0 45.6178 2.00426 4 12 -2 0 1.36073 0.57748 2 12 -2 0 1.01441 0.61023 4 12 -2 0 2.03350 0.65897 1 -12 2 0 1.71262 0.67440 3 12 2 0 0.56003 0.59020 1 12 2 0 0.98047 0.48861 4 13 -2 0 0.60191 0.48841 2 13 -2 0 1.12248 0.67948 4 13 -2 0 0.65974 0.54648 1 -13 2 0 1.39092 0.70473 3 13 2 0 0.26239 0.67998 1 14 -2 0 0.18560 0.54229 4 14 -2 0 0.81030 0.63917 1 14 -2 0 1.09276 0.58097 2 14 2 0 0.67472 0.70658 1 -14 2 0 0.56157 0.49612 3 15 -2 0 0.16931 0.50775 4 15 -2 0 0.52812 0.65747 1 15 2 0 -0.1515 0.66188 1 16 -2 0 0.68486 0.70963 4 16 -2 0 0.89650 0.71773 1 16 2 0 0.76395 0.77531 1 17 -2 0 1.86080 0.75327 1 17 -2 0 1.42706 0.85869 4 17 2 0 2.22045 1.01641 1 0 -3 0 -0.3836 0.23909 1 0 -3 0 0.04351 0.29984 3 0 -3 0 -0.5545 0.19756 2 0 -3 0 -0.2906 0.22702 4 0 3 0 0.32532 0.30676 3 0 3 0 0.36799 0.31050 4 0 3 0 0.20671 0.31732 2 0 3 0 -0.1384 0.23780 1 -1 -3 0 873.502 19.6818 4 1 -3 0 855.612 19.9796 2 -1 -3 0 826.899 19.9826 3 1 -3 0 866.650 19.7929 4 1 -3 0 886.907 19.6065 1 -1 -3 0 842.704 19.7379 2 1 3 0 854.341 19.6583 4 1 3 0 868.191 19.7772 2 1 3 0 858.057 19.6578 1 -1 3 0 898.862 19.8557 4 -1 3 0 869.213 20.0087 2 -1 3 0 869.241 19.5794 1 1 3 0 847.137 20.0397 3 -1 3 0 847.903 20.2840 3 2 -3 0 290.425 7.23947 1 2 -3 0 280.948 7.69049 2 -2 -3 0 278.580 7.52814 3 2 -3 0 293.335 7.54646 4 -2 -3 0 292.947 7.34496 2 -2 3 0 290.974 8.03675 3 2 3 0 291.429 7.61407 3 2 3 0 300.051 7.37363 2 2 3 0 283.085 7.40028 1 2 3 0 293.528 7.33169 4 -2 3 0 297.516 7.77544 2 3 -3 0 322.196 8.66243 2 -3 -3 0 312.133 8.26155 3 -3 -3 0 341.672 8.10951 2 3 -3 0 336.356 8.49419 4 3 -3 0 332.646 8.11409 1 3 3 0 340.265 8.42609 3 -3 3 0 327.227 9.00015 3 3 3 0 331.341 8.16644 4 -3 3 0 332.033 8.71636 2 3 3 0 325.265 8.37036 1 3 3 0 325.104 8.06465 2 4 -3 0 99.7842 3.48034 4 -4 -3 0 99.7490 3.21316 3 -4 -3 0 108.747 3.05628 2 4 -3 0 100.654 3.66226 2 4 -3 0 102.952 3.18271 1 -4 3 0 101.175 3.91827 3 -4 3 0 108.406 3.76206 2 4 3 0 110.883 3.26214 4 4 3 0 107.954 3.05844 2 4 3 0 102.324 3.48177 1 5 -3 0 113.725 4.01344 2 5 -3 0 108.829 3.75376 4 -5 -3 0 110.445 3.07623 2 -5 -3 0 113.557 3.36036 3 5 -3 0 114.293 3.43969 1 5 3 0 116.162 3.83707 1 -5 3 0 110.036 4.21994 3 5 3 0 112.330 3.42001 4 5 3 0 115.986 3.12136 2 -5 3 0 118.859 4.08733 2 -6 -3 0 69.0782 2.28201 3 6 -3 0 68.0545 2.94856 2 6 -3 0 69.8677 2.49581 1 6 -3 0 72.6808 2.86115 4 6 3 0 69.5981 2.86641 1 6 3 0 69.4431 2.45021 4 -6 3 0 70.0144 3.19804 3 -6 3 0 68.8863 2.97251 2 -7 -3 0 111.173 3.15450 3 7 -3 0 112.746 4.10751 2 7 -3 0 108.356 3.87820 4 7 -3 0 115.013 3.54946 1 7 3 0 107.307 3.98230 1 -7 3 0 105.164 4.27170 3 -7 3 0 104.759 4.02935 2 7 3 0 115.087 3.49268 4 8 -3 0 400.181 10.6209 4 8 -3 0 413.219 10.9221 2 8 -3 0 409.358 10.1626 1 -8 3 0 419.662 11.0015 2 8 3 0 408.295 10.8914 1 -8 3 0 393.521 11.2335 3 8 3 0 406.867 10.0368 4 9 -3 0 4.69266 0.92138 4 9 -3 0 5.38799 1.05093 2 9 -3 0 5.31536 0.80518 1 -9 3 0 3.87356 0.99560 3 9 3 0 5.12134 1.02123 1 -9 3 0 7.07280 1.20329 2 10 -3 0 15.3431 1.72462 2 10 -3 0 14.0743 1.60688 4 10 -3 0 15.5972 1.21807 1 -10 3 0 14.6760 1.85573 3 10 3 0 13.9475 1.72159 1 11 -3 0 1.47687 0.63676 2 11 -3 0 0.76640 0.43277 1 11 -3 0 0.43824 0.56574 4 11 3 0 1.64625 0.75871 1 -11 3 0 2.62234 0.87480 3 12 -3 0 1.65547 0.72042 2 12 -3 0 2.33363 0.68030 1 12 -3 0 4.73368 1.03684 4 12 3 0 2.30285 0.89878 1 -12 3 0 2.11468 0.78550 3 13 -3 0 33.0118 2.12137 1 13 -3 0 32.0170 2.25333 2 13 -3 0 27.5726 2.07404 4 -13 3 0 36.7803 2.59738 3 13 3 0 34.7380 2.57224 1 14 -3 0 46.8711 2.81610 4 14 -3 0 41.9317 2.63587 2 14 -3 0 44.5362 2.61176 1 14 3 0 49.2052 3.17660 1 -14 3 0 41.4562 2.90595 3 15 -3 0 14.7799 1.89626 4 15 -3 0 15.6521 1.90177 1 15 -3 0 10.0121 1.53037 2 15 3 0 15.7159 2.20129 1 -15 3 0 12.3078 1.87931 3 16 -3 0 1.74086 0.70844 1 16 -3 0 1.39327 0.86094 4 16 3 0 0.65245 0.86255 1 0 -4 0 105.256 4.08470 3 0 -4 0 108.858 3.86442 2 0 -4 0 112.809 3.64234 1 0 -4 0 108.041 3.69045 4 0 4 0 108.597 3.58698 1 0 4 0 106.061 3.67849 4 0 4 0 106.573 4.13423 3 0 4 0 111.803 3.91621 2 1 -4 0 57.8206 2.28922 1 -1 -4 0 52.9604 2.57628 3 1 -4 0 54.5465 2.38813 4 -1 -4 0 52.0752 2.29897 1 -1 -4 0 52.5547 2.29230 4 1 -4 0 53.5765 2.54171 2 -1 -4 0 53.9671 2.40858 2 1 -4 0 48.3331 2.63212 3 -1 4 0 56.1353 2.44435 4 1 4 0 51.3628 2.26359 1 -1 4 0 55.1828 2.78008 3 -1 4 0 54.5965 2.24740 1 1 4 0 53.4846 2.42181 2 1 4 0 55.8577 2.34215 4 -1 4 0 53.2922 2.53256 2 1 4 0 57.2287 2.70281 3 2 -4 0 11.5295 1.38784 2 2 -4 0 9.24729 1.37996 3 -2 -4 0 9.28180 1.09729 2 -2 -4 0 9.04575 1.19322 3 2 -4 0 10.3997 0.89567 1 2 -4 0 8.94136 1.15554 4 -2 -4 0 8.51364 1.03865 4 -2 4 0 8.70551 1.33734 3 2 4 0 9.05973 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18 0.50445 0.64343 2 -2 1 18 0.82168 0.72828 4 -1 -1 18 3.18805 0.93594 2 -1 -1 18 4.01797 1.05711 3 -1 1 18 2.93643 1.06296 2 -1 1 18 3.37020 0.98837 4 0 -1 18 0.12623 0.50895 2 0 1 18 0.46109 0.66316 4 0 1 18 -0.0447 0.60541 2 1 -1 18 0.13435 0.60805 2 1 1 18 0.26350 0.58786 4 1 1 18 0.79234 0.66045 2 2 -1 18 3.70467 1.08513 2 2 1 18 3.11437 0.89680 4 2 1 18 4.37374 1.12549 2 3 1 18 0.13576 0.65120 4 3 1 18 -0.0914 0.57903 2 -6 -2 18 0.03726 0.80863 3 6 -2 -18 0.44766 0.88493 1 -6 -2 18 1.24457 0.49904 2 6 -2 -18 -0.4115 0.72626 4 -6 2 18 1.71753 0.85012 3 -6 2 18 1.10900 0.72245 4 -5 -2 18 0.69095 0.53442 2 -5 -2 18 -0.4666 0.60263 3 5 -2 -18 0.09682 0.68845 1 -5 2 18 0.32917 0.44474 2 -5 2 18 -0.4321 0.58089 4 4 -2 -18 2.61368 1.11337 1 -4 -2 18 2.15431 0.93267 3 -4 -2 18 3.05509 0.83767 2 -4 2 18 1.49075 0.73607 2 -4 2 18 2.47149 0.91219 4 3 -2 -18 0.86944 0.85739 1 -3 -2 18 0.18923 0.70631 3 -3 -2 18 1.02136 0.53841 2 -3 2 18 0.49812 0.69496 4 -3 2 18 1.81676 0.87574 2 2 -2 -18 0.11754 0.78352 1 -2 -2 18 2.01013 0.74790 2 -2 -2 18 1.31315 0.82203 3 -2 2 18 2.42398 0.94283 2 -2 2 18 1.01916 0.90855 4 -1 -2 18 1.50846 0.86847 3 1 -2 -18 1.58707 0.94567 1 -1 -2 18 3.11564 0.91137 2 -1 2 18 2.33669 0.91184 2 -1 2 18 0.97254 0.78281 4 0 -2 18 -0.1702 0.50946 2 0 -2 -18 0.22304 0.89407 1 0 -2 18 -0.8862 0.59154 3 0 2 18 -0.0743 0.67017 2 0 2 18 1.15416 0.73366 4 1 2 18 0.82228 0.95095 2 -5 0 19 0.79645 0.66231 3 -5 0 19 0.93664 0.70416 2 -4 0 19 0.92067 0.72292 2 -4 0 19 0.35659 0.59636 3 -3 0 19 0.16840 0.58930 2 -2 0 19 0.15251 0.59791 2 -3 -1 19 -0.6259 0.48424 3 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 20361 _shelx_res_file ; TITL 29NOV2019_NDWNEW RKrun P21/c monoclinic shelx.res created by SHELXL-2018/3 at 21:42:41 on 31-Aug-2020 CELL 0.71073 13.2096 4.9765 13.5673 90.000 98.603 90.000 ZERR 2.00 0.0014 0.0005 0.0014 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O CL UNIT 24 32 16 8 4 MERG 2 ACTA BOND $H CONF WPDB FMAP 2 PLAN 20 SIZE 0.72 0.34 0.13 L.S. 10 WGHT 0.064200 0.319500 FVAR 0.60199 MOLE 1 CL1 5 0.587241 0.105264 0.741172 11.00000 0.05677 0.04541 = 0.08672 0.02237 0.03284 0.00090 N2 3 0.744958 0.754904 0.604311 11.00000 0.02904 0.03807 = 0.03503 0.00293 0.00062 -0.00707 O2 4 0.817818 1.141591 0.504014 11.00000 0.03478 0.05954 = 0.05286 0.01729 -0.00678 -0.01779 AFIX 83 H2 2 0.803150 1.017333 0.538975 11.00000 -1.50000 AFIX 0 O1 4 0.963861 1.122161 0.608128 11.00000 0.04174 0.06025 = 0.04953 0.01439 -0.01108 -0.01995 N1 3 0.603847 0.454412 0.603318 11.00000 0.03396 0.03920 = 0.04730 0.00206 0.00778 -0.00805 C5 1 0.909494 1.223748 0.536304 11.00000 0.03220 0.03813 = 0.03897 -0.00008 0.00284 -0.00705 C2 1 0.742760 0.446966 0.739642 11.00000 0.04238 0.04260 = 0.04153 0.01016 0.00771 0.00491 AFIX 43 H2A 2 0.771513 0.374017 0.800544 11.00000 -1.20000 AFIX 0 C4 1 0.652600 0.654826 0.563399 11.00000 0.03040 0.03968 = 0.03665 -0.00046 0.00276 -0.00737 C6 1 0.946734 1.452175 0.478955 11.00000 0.03240 0.03834 = 0.04561 0.00484 0.00258 -0.00763 AFIX 23 H6A 2 0.899454 1.601474 0.478469 11.00000 -1.20000 H6B 2 0.946393 1.395885 0.410457 11.00000 -1.20000 AFIX 0 N4 3 0.880383 0.758520 0.730714 11.00000 0.04118 0.06141 = 0.04622 0.01214 -0.01129 -0.00856 AFIX 93 H4A 2 0.906878 0.884453 0.699449 11.00000 -1.20000 H4B 2 0.912066 0.700416 0.786646 11.00000 -1.20000 AFIX 0 C1 1 0.651474 0.361423 0.689593 11.00000 0.03793 0.03326 = 0.04952 0.00517 0.01697 0.00112 C3 1 0.790737 0.654002 0.692705 11.00000 0.03355 0.03786 = 0.03718 0.00068 0.00301 0.00168 N3 3 0.607782 0.762997 0.478532 11.00000 0.04324 0.06512 = 0.04598 0.01360 -0.01020 -0.02295 AFIX 93 H3A 2 0.549166 0.704581 0.450636 11.00000 -1.20000 H3B 2 0.637362 0.891492 0.451444 11.00000 -1.20000 AFIX 0 HKLF 4 REM 29NOV2019_NDWNEW RKrun P21/c monoclinic REM wR2 = 0.1282, GooF = S = 1.040, Restrained GooF = 1.040 for all data REM R1 = 0.0434 for 2102 Fo > 4sig(Fo) and 0.0545 for all 2599 data REM 118 parameters refined using 0 restraints END WGHT 0.0593 0.3391 REM Highest difference peak 0.332, deepest hole -0.437, 1-sigma level 0.058 Q1 1 0.7730 0.8793 0.5766 11.00000 0.05 0.33 Q2 1 0.7588 0.5720 0.7210 11.00000 0.05 0.29 Q3 1 0.5814 0.2168 0.7820 11.00000 0.05 0.28 Q4 1 0.9378 1.2491 0.6249 11.00000 0.05 0.26 Q5 1 0.9349 1.3196 0.5003 11.00000 0.05 0.23 Q6 1 0.6027 0.1909 0.7973 11.00000 0.05 0.22 Q7 1 0.6362 0.5173 0.5732 11.00000 0.05 0.21 Q8 1 0.6205 0.5736 0.5952 11.00000 0.05 0.20 Q9 1 0.6969 0.4314 0.7192 11.00000 0.05 0.19 Q10 1 0.7034 0.7148 0.5849 11.00000 0.05 0.19 Q11 1 1.0000 1.5000 0.5000 10.50000 0.05 0.18 Q12 1 0.7537 0.7087 0.6433 11.00000 0.05 0.16 Q13 1 0.5949 -0.2833 0.7410 11.00000 0.05 0.16 Q14 1 0.8949 1.5565 0.4234 11.00000 0.05 0.16 Q15 1 0.6390 0.1739 0.5403 11.00000 0.05 0.15 Q16 1 0.9267 1.2105 0.2808 11.00000 0.05 0.15 Q17 1 0.6370 0.3956 0.6354 11.00000 0.05 0.15 Q18 1 0.6079 1.0078 0.4724 11.00000 0.05 0.14 Q19 1 0.7377 0.7551 0.6298 11.00000 0.05 0.14 Q20 1 0.7641 0.4367 0.8382 11.00000 0.05 0.14 ; _shelx_res_checksum 9436 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_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 _atom_site_disorder_assembly _atom_site_disorder_group Cl Cl1 0.58724(4) 0.10526(9) 0.74117(4) 0.06071(19) Uani d 1 . . N N2 0.74496(9) 0.7549(3) 0.60431(9) 0.0345(3) Uani d 1 . . O O2 0.81782(9) 1.1416(3) 0.50401(9) 0.0504(3) Uani d 1 . . H H2 0.803150 1.017333 0.538975 0.076 Uiso calc 1 . . O O1 0.96386(9) 1.1222(3) 0.60813(9) 0.0523(3) Uani d 1 . . N N1 0.60385(10) 0.4544(3) 0.60332(10) 0.0400(3) Uani d 1 . . C C5 0.90949(11) 1.2237(3) 0.53630(11) 0.0367(3) Uani d 1 . . C C2 0.74276(13) 0.4470(3) 0.73964(12) 0.0420(4) Uani d 1 . . H H2A 0.771513 0.374017 0.800544 0.050 Uiso calc 1 . . C C4 0.65260(11) 0.6548(3) 0.56340(11) 0.0358(3) Uani d 1 . . C C6 0.94673(11) 1.4522(3) 0.47896(12) 0.0391(3) Uani d 1 . . H H6A 0.899454 1.601474 0.478469 0.047 Uiso calc 1 . . H H6B 0.946393 1.395885 0.410457 0.047 Uiso calc 1 . . N N4 0.88038(11) 0.7585(3) 0.73071(11) 0.0514(4) Uani d 1 . . H H4A 0.906878 0.884453 0.699449 0.062 Uiso calc 1 . . H H4B 0.912066 0.700416 0.786646 0.062 Uiso calc 1 . . C C1 0.65147(12) 0.3614(3) 0.68959(12) 0.0392(3) Uani d 1 . . C C3 0.79074(11) 0.6540(3) 0.69271(11) 0.0364(3) Uani d 1 . . N N3 0.60778(11) 0.7630(3) 0.47853(11) 0.0532(4) Uani d 1 . . H H3A 0.549166 0.704581 0.450636 0.064 Uiso calc 1 . . H H3B 0.637362 0.891492 0.451444 0.064 Uiso calc 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 Cl1 0.0568(3) 0.0454(3) 0.0867(4) 0.00090(19) 0.0328(3) 0.0224(2) N2 0.0290(6) 0.0381(6) 0.0350(6) -0.0071(5) 0.0006(4) 0.0029(5) O2 0.0348(6) 0.0595(8) 0.0529(7) -0.0178(5) -0.0068(5) 0.0173(6) O1 0.0417(6) 0.0602(8) 0.0495(7) -0.0200(6) -0.0111(5) 0.0144(6) N1 0.0340(6) 0.0392(7) 0.0473(7) -0.0080(5) 0.0078(5) 0.0021(5) C5 0.0322(7) 0.0381(7) 0.0390(7) -0.0070(6) 0.0028(5) -0.0001(6) C2 0.0424(8) 0.0426(8) 0.0415(8) 0.0049(6) 0.0077(6) 0.0102(6) C4 0.0304(6) 0.0397(7) 0.0366(7) -0.0074(6) 0.0028(5) -0.0005(6) C6 0.0324(7) 0.0383(8) 0.0456(8) -0.0076(6) 0.0026(6) 0.0048(6) N4 0.0412(7) 0.0614(10) 0.0462(8) -0.0086(7) -0.0113(6) 0.0121(7) C1 0.0379(7) 0.0333(7) 0.0495(8) 0.0011(6) 0.0170(6) 0.0052(6) C3 0.0336(7) 0.0379(7) 0.0372(7) 0.0017(6) 0.0030(5) 0.0007(6) N3 0.0432(7) 0.0651(10) 0.0460(8) -0.0230(7) -0.0102(6) 0.0136(7) 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' Cl Cl 0.1484 0.1585 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C3 N2 C4 . . 118.71(13) ? C5 O2 H2 . . 109.5 ? C1 N1 C4 . . 114.95(13) ? O1 C5 O2 . . 123.08(14) ? O1 C5 C6 . . 121.62(13) ? O2 C5 C6 . . 115.30(13) ? C1 C2 C3 . . 115.32(14) ? C1 C2 H2A . . 122.3 ? C3 C2 H2A . . 122.3 ? N3 C4 N1 . . 118.16(13) ? N3 C4 N2 . . 117.58(14) ? N1 C4 N2 . . 124.26(14) ? C5 C6 C6 . 3_786 113.62(16) ? C5 C6 H6A . . 108.8 ? C6 C6 H6A 3_786 . 108.8 ? C5 C6 H6B . . 108.8 ? C6 C6 H6B 3_786 . 108.8 ? H6A C6 H6B . . 107.7 ? C3 N4 H4A . . 120.0 ? C3 N4 H4B . . 120.0 ? H4A N4 H4B . . 120.0 ? N1 C1 C2 . . 126.81(14) ? N1 C1 Cl1 . . 114.59(12) ? C2 C1 Cl1 . . 118.61(13) ? N4 C3 N2 . . 116.94(14) ? N4 C3 C2 . . 123.14(14) ? N2 C3 C2 . . 119.91(14) ? C4 N3 H3A . . 120.0 ? C4 N3 H3B . . 120.0 ? H3A N3 H3B . . 120.0 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 C1 . 1.7356(16) ? N2 C3 . 1.3561(18) ? N2 C4 . 1.3572(18) ? O2 C5 . 1.2911(17) ? O2 H2 . 0.8200 ? O1 C5 . 1.2294(19) ? N1 C1 . 1.327(2) ? N1 C4 . 1.3443(19) ? C5 C6 . 1.501(2) ? C2 C1 . 1.361(2) ? C2 C3 . 1.410(2) ? C2 H2A . 0.9300 ? C4 N3 . 1.327(2) ? C6 C6 3_786 1.514(3) ? C6 H6A . 0.9700 ? C6 H6B . 0.9700 ? N4 C3 . 1.325(2) ? N4 H4A . 0.8600 ? N4 H4B . 0.8600 ? N3 H3A . 0.8600 ? N3 H3B . 0.8600 ? 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 _geom_hbond_publ_flag O2 H2 N2 . 0.82 1.81 2.622(2) 169 yes N3 H3A N1 3_666 0.86 2.19 3.048(2) 173 yes N4 H4A O1 . 0.86 1.94 2.794(2) 169 yes N4 H4B O1 2_746 0.86 2.04 2.8510(19) 156 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C1 N1 C4 N3 . . . . -178.01(15) ? C1 N1 C4 N2 . . . . 1.9(2) ? C3 N2 C4 N3 . . . . 177.81(15) ? C3 N2 C4 N1 . . . . -2.1(2) ? O1 C5 C6 C6 . . . 3_786 -2.5(3) ? O2 C5 C6 C6 . . . 3_786 178.28(18) ? C4 N1 C1 C2 . . . . -0.4(2) ? C4 N1 C1 Cl1 . . . . 179.33(11) ? C3 C2 C1 N1 . . . . -0.8(3) ? C3 C2 C1 Cl1 . . . . 179.50(12) ? C4 N2 C3 N4 . . . . -179.40(14) ? C4 N2 C3 C2 . . . . 0.7(2) ? C1 C2 C3 N4 . . . . -179.27(16) ? C1 C2 C3 N2 . . . . 0.6(2) ? _cod_database_fobs_code 1559092