#------------------------------------------------------------------------------ #$Date: 2021-06-11 05:03:44 +0300 (Fri, 11 Jun 2021) $ #$Revision: 266384 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/76/7707655.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_7707655 loop_ _publ_author_name 'Khrustalev, Victor N.' 'Grishina, Maria' 'Matsulevich, Zhanna' 'Lukiyanova, Julia' 'Borisova, Galina N.' 'Osmanov, Vladimir K.' 'Novikov, Alexander S.' 'Kirichuk, Anatoly' 'Solari, Euro' 'Borisov, Alexander V.' 'Tskhovrebov, Alexander' _publ_section_title ; Novel Cationic 1,2,4-Selenadiazoles: Synthesis via Addition of 2-Pyridylselenyl Halides to Unactivated Nitriles, Structures and Four-center Se···N Contacts ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT01322J _journal_year 2021 _chemical_formula_moiety 'C12 H8 Br N2 Se, Br' _chemical_formula_sum 'C12 H8 Br2 N2 Se' _chemical_formula_weight 418.96 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2013 _audit_update_record ; 2021-03-14 deposited with the CCDC. 2021-06-09 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 115.186(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 29.431(2) _cell_length_b 7.1286(5) _cell_length_c 13.0733(9) _cell_measurement_reflns_used 4536 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 31.09 _cell_measurement_theta_min 3.06 _cell_volume 2482.0(3) _computing_cell_refinement 'SAINT (Bruker, 2013)' _computing_data_collection 'APEX3 (Bruker, 2018)' _computing_data_reduction 'SAINT (Bruker, 2013)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2015)' _computing_publication_material 'SHELXTL (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON-III CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1193 _diffrn_reflns_av_unetI/netI 0.0772 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 27223 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.612 _diffrn_reflns_theta_min 3.059 _exptl_absorpt_coefficient_mu 9.441 _exptl_absorpt_correction_T_max 0.743 _exptl_absorpt_correction_T_min 0.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: 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 2.242 _exptl_crystal_description plate _exptl_crystal_F_000 1584 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.873 _refine_diff_density_min -1.227 _refine_diff_density_rms 0.209 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 154 _refine_ls_number_reflns 4533 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0447 _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^)+(0.0318P)^2^+1.7141P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.0962 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3039 _reflns_number_total 4533 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01322j2.cif _cod_data_source_block 5 _cod_original_cell_volume 2482.1(3) _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7707655 _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 0.210 _shelx_estimated_absorpt_t_max 0.834 _shelxl_version_number 2013-4 _shelx_res_file ; TITL AT167 in C2/c CELL 0.71073 29.4314 7.1286 13.0733 90.000 115.186 90.000 ZERR 8.000 0.0022 0.0005 0.0009 0.000 0.002 0.000 LATT 7 SYMM -X, Y, 1/2-Z SFAC C H BR N SE UNIT 96 64 16 16 8 TEMP -173.0 SIZE 0.02 0.20 0.24 OMIT 1 1 0 L.S. 12 BOND $H ACTA CONF WGHT 0.031800 1.714100 FVAR 0.14179 BR1 3 0.776155 0.504804 1.170075 11.00000 0.02513 0.02110 = 0.01909 -0.00225 -0.00028 0.00351 BR2 3 0.409285 0.189459 0.361615 11.00000 0.01900 0.01933 = 0.01552 0.00194 0.00697 0.00167 SE1 5 0.496089 0.278379 0.597117 11.00000 0.01514 0.01775 = 0.01422 0.00011 0.00609 -0.00011 N2 4 0.548276 0.323966 0.735281 11.00000 0.01947 0.01708 = 0.01304 -0.00076 0.00478 -0.00090 C3 1 0.590929 0.325691 0.730736 11.00000 0.02034 0.01153 = 0.01537 0.00105 0.00913 -0.00094 N4 4 0.590627 0.290147 0.622419 11.00000 0.02076 0.01205 = 0.01228 -0.00104 0.00785 -0.00117 C5 1 0.543648 0.263009 0.538830 11.00000 0.02131 0.01206 = 0.01741 0.00218 0.00857 0.00098 C6 1 0.537437 0.228494 0.428736 11.00000 0.01674 0.01983 = 0.01703 0.00050 0.00599 0.00046 AFIX 43 H6 2 0.504758 0.215013 0.369248 11.00000 -1.20000 AFIX 0 C7 1 0.578891 0.214245 0.407278 11.00000 0.02770 0.01943 = 0.01851 -0.00040 0.01118 -0.00143 AFIX 43 H7 2 0.575086 0.191327 0.332469 11.00000 -1.20000 AFIX 0 C8 1 0.627155 0.233480 0.495833 11.00000 0.02245 0.01667 = 0.01994 0.00036 0.01436 -0.00255 AFIX 43 H8 2 0.655974 0.220586 0.481203 11.00000 -1.20000 AFIX 0 C9 1 0.632528 0.270469 0.602186 11.00000 0.01653 0.01820 = 0.01766 0.00093 0.00765 -0.00008 AFIX 43 H9 2 0.665077 0.282697 0.662334 11.00000 -1.20000 AFIX 0 C10 1 0.638357 0.360705 0.833043 11.00000 0.01498 0.01447 = 0.01729 0.00018 0.00592 0.00078 C11 1 0.675365 0.482303 0.833088 11.00000 0.02201 0.01476 = 0.01746 0.00011 0.00912 0.00097 AFIX 43 H11 2 0.672001 0.540312 0.764803 11.00000 -1.20000 AFIX 0 C12 1 0.717317 0.518549 0.933577 11.00000 0.01665 0.01579 = 0.02170 -0.00126 0.00740 0.00165 AFIX 43 H12 2 0.743250 0.598474 0.934135 11.00000 -1.20000 AFIX 0 C13 1 0.720811 0.437034 1.032430 11.00000 0.02194 0.01854 = 0.01479 -0.00288 0.00381 0.00354 C14 1 0.684364 0.317547 1.034400 11.00000 0.02065 0.02192 = 0.01629 0.00286 0.00965 0.00560 AFIX 43 H14 2 0.687405 0.263370 1.103415 11.00000 -1.20000 AFIX 0 C15 1 0.643005 0.277751 0.933330 11.00000 0.01493 0.01979 = 0.01926 0.00257 0.00693 0.00362 AFIX 43 H15 2 0.617879 0.193657 0.932873 11.00000 -1.20000 AFIX 0 HKLF 4 REM AT167 in C2/c REM R1 = 0.0447 for 3039 Fo > 4sig(Fo) and 0.0903 for all 4533 data REM 154 parameters refined using 0 restraints END WGHT 0.0318 1.7141 REM Highest difference peak 0.873, deepest hole -1.227, 1-sigma level 0.209 Q1 1 0.5293 0.3755 0.5819 11.00000 0.05 0.87 Q2 1 0.4340 0.1644 0.4509 11.00000 0.05 0.85 Q3 1 0.5114 0.2762 0.6544 11.00000 0.05 0.84 Q4 1 0.6290 0.2767 0.5430 11.00000 0.05 0.84 Q5 1 0.6024 0.2595 0.4712 11.00000 0.05 0.81 Q6 1 0.3997 0.2548 0.4276 11.00000 0.05 0.81 Q7 1 0.3681 0.2353 0.3675 11.00000 0.05 0.80 Q8 1 0.4594 0.3474 0.6068 11.00000 0.05 0.80 Q9 1 0.4359 0.2703 0.3341 11.00000 0.05 0.78 Q10 1 0.6423 0.0864 1.1054 11.00000 0.05 0.77 Q11 1 0.4995 0.0699 0.6687 11.00000 0.05 0.77 Q12 1 0.8096 0.5143 1.1319 11.00000 0.05 0.75 Q13 1 0.6801 0.6932 0.8775 11.00000 0.05 0.75 Q14 1 0.7251 0.4411 0.8394 11.00000 0.05 0.75 Q15 1 0.7332 0.4536 1.1422 11.00000 0.05 0.75 Q16 1 0.5276 0.2496 0.5714 11.00000 0.05 0.74 Q17 1 0.5963 0.1138 0.3754 11.00000 0.05 0.74 Q18 1 0.5901 0.2244 0.9115 11.00000 0.05 0.74 Q19 1 0.6372 0.5244 0.5958 11.00000 0.05 0.74 Q20 1 0.4480 0.2564 0.5610 11.00000 0.05 0.73 ; _shelx_res_checksum 31267 _shelx_hkl_file ; 4 0 0 407.46 23.20 -4 0 0 372.56 21.20 -4 0 0 361.16 22.40 -4 0 0 427.66 21.70 4 0 0 309.07 16.40 4 0 0 344.57 21.10 4 0 0 421.96 21.70 6 0 0 415.56 27.30 6 0 0 493.75 27.60 6 0 0 373.86 19.60 -6 0 0 436.36 19.50 -8 0 0 758.02 46.30 8 0 0 701.43 43.20 8 0 0 827.42 43.90 10 0 0 2363.76 110.69 -10 0 0 2366.36 112.99 10 0 0 2382.56 109.49 12 0 0 954.30 55.09 12 0 0 875.41 55.09 -12 0 0 930.61 57.69 14 0 0 1441.06 81.59 -14 0 0 1590.04 86.49 14 0 0 1550.04 81.69 16 0 0 673.93 47.80 -16 0 0 644.84 51.69 16 0 0 693.43 50.39 -18 0 0 434.86 45.70 18 0 0 515.35 44.00 18 0 0 475.75 41.80 -20 0 0 20.70 19.10 20 0 0 9.20 14.40 20 0 0 5.80 13.40 -22 0 0 4308.67 215.28 22 0 0 4675.13 212.08 22 0 0 4553.34 209.48 24 0 0 239.68 37.70 -24 0 0 289.67 46.50 24 0 0 212.08 34.40 26 0 0 30.70 16.90 -26 0 0 32.30 24.20 26 0 0 10.10 15.40 28 0 0 -1.20 14.00 -28 0 0 -8.50 17.10 28 0 0 22.80 18.50 30 0 0 29.70 19.10 30 0 0 6.70 15.70 -30 0 0 27.30 24.00 32 0 0 450.65 55.19 -32 0 0 667.53 70.39 32 0 0 624.34 59.09 -34 0 0 10.90 28.90 34 0 0 63.49 26.60 34 0 0 54.09 24.20 -36 0 0 176.98 52.49 36 0 0 147.49 35.90 36 0 0 145.89 31.70 38 0 0 20.90 25.00 38 0 0 61.19 28.20 -38 0 0 106.29 36.60 40 0 0 -16.70 22.50 -40 0 0 -22.50 28.10 40 0 0 3.40 21.40 1 -1 0 22.50 2.70 1 -1 0 25.40 3.80 -1 -1 0 24.10 4.00 1 -1 0 19.80 2.50 -1 1 0 21.10 3.40 -1 1 0 25.70 5.90 -1 1 0 10.40 4.40 1 1 0 22.70 3.80 1 1 0 23.80 6.10 -3 -1 0 48.90 8.40 -3 -1 0 47.40 5.90 3 -1 0 40.00 5.00 3 -1 0 45.30 6.80 3 -1 0 44.20 4.00 -3 -1 0 48.40 6.40 -3 1 0 51.99 3.80 -3 1 0 45.40 6.30 -3 1 0 47.30 5.20 -3 1 0 39.60 7.30 3 1 0 51.69 5.90 3 1 0 39.10 8.00 3 1 0 38.50 5.20 3 1 0 51.29 6.50 -3 1 0 49.50 7.30 -5 -1 0 13.50 4.80 -5 -1 0 26.00 8.20 -5 -1 0 20.20 6.20 5 -1 0 24.40 5.20 -5 -1 0 11.00 5.60 5 -1 0 15.50 6.70 5 1 0 21.80 7.30 5 1 0 24.00 6.50 5 1 0 30.50 6.80 -5 1 0 18.40 4.70 -7 -1 0 1147.19 64.49 7 -1 0 1062.89 59.09 7 -1 0 1279.57 54.79 -7 -1 0 1310.37 61.59 -7 1 0 1200.38 52.09 7 1 0 1278.97 60.59 -7 1 0 1185.68 52.09 7 1 0 1103.69 57.69 9 -1 0 686.33 44.10 9 -1 0 827.92 41.20 -9 -1 0 786.02 47.80 -9 1 0 737.53 31.90 9 1 0 674.93 42.10 9 1 0 753.92 44.60 -9 1 0 766.82 41.30 9 1 0 678.03 40.40 -9 1 0 724.53 33.00 11 -1 0 300.67 25.10 -11 -1 0 355.56 33.70 11 -1 0 264.87 27.20 11 1 0 272.97 22.40 11 1 0 282.57 25.70 11 1 0 279.67 26.40 -11 1 0 273.47 24.70 13 -1 0 318.97 31.50 13 -1 0 371.56 30.00 -13 -1 0 316.57 37.10 -13 1 0 326.57 31.10 13 1 0 337.67 30.50 13 1 0 366.36 32.80 -15 -1 0 376.86 42.80 15 -1 0 490.75 40.00 15 -1 0 474.95 36.40 -15 1 0 415.96 37.70 15 1 0 332.67 37.30 15 1 0 412.06 36.20 15 1 0 464.25 39.00 17 -1 0 8.80 14.30 -17 -1 0 25.70 20.20 17 -1 0 0.60 10.40 17 1 0 28.60 15.90 17 1 0 17.30 13.70 -17 1 0 4.70 14.30 17 1 0 30.30 15.10 19 -1 0 21.10 13.00 19 -1 0 30.80 16.40 -19 -1 0 46.50 23.50 19 1 0 30.30 16.20 19 1 0 14.00 14.00 -19 1 0 17.60 15.20 21 -1 0 -7.30 9.70 -21 -1 0 5.90 21.30 21 -1 0 14.60 15.20 21 1 0 23.20 16.10 21 1 0 28.70 12.00 -21 1 0 -3.50 15.10 21 1 0 27.20 17.80 23 -1 0 40.00 19.30 23 -1 0 62.79 20.80 -23 -1 0 14.10 22.10 -23 1 0 46.70 23.50 23 1 0 41.70 16.90 23 1 0 45.80 19.20 25 -1 0 87.29 22.90 -25 -1 0 73.69 30.40 25 -1 0 80.09 25.20 25 1 0 39.60 21.50 25 1 0 107.09 26.20 -25 1 0 122.09 31.30 27 -1 0 -9.80 13.60 -27 -1 0 40.90 25.80 27 -1 0 43.70 22.30 27 1 0 4.60 14.10 -27 1 0 23.60 20.00 27 1 0 -5.20 15.90 29 -1 0 267.17 39.50 -29 -1 0 170.68 40.50 29 -1 0 254.97 41.70 -29 1 0 188.98 40.00 29 1 0 207.38 35.80 29 1 0 239.18 59.19 -31 -1 0 93.29 33.20 31 -1 0 89.89 27.00 31 -1 0 98.69 26.70 31 1 0 115.79 31.60 -31 1 0 95.49 31.50 31 1 0 61.89 28.00 33 -1 0 -26.20 14.40 -33 -1 0 -11.80 20.70 33 -1 0 17.10 19.00 -33 1 0 37.80 24.80 33 1 0 -14.80 17.00 33 1 0 16.60 20.80 35 -1 0 0.40 16.10 -35 -1 0 22.60 26.50 35 -1 0 18.20 17.60 35 1 0 -2.10 19.10 35 1 0 20.00 18.90 -35 1 0 -5.80 19.00 -37 -1 0 12.00 28.00 37 -1 0 16.50 21.40 37 -1 0 16.20 23.60 37 1 0 -2.40 23.50 -37 1 0 7.60 27.90 39 -1 0 -21.60 15.70 39 -1 0 30.60 22.50 -39 -1 0 22.00 32.00 39 1 0 -7.10 18.80 39 1 0 49.20 22.10 -39 1 0 -23.80 22.20 0 -2 0 3407.96 135.49 0 -2 0 3302.17 137.09 0 2 0 3165.78 146.69 0 2 0 3433.26 135.29 2 -2 0 9406.36 371.26 2 -2 0 8994.90 367.46 2 -2 0 9694.13 367.46 -2 -2 0 9999.00 372.36 2 -2 0 9530.15 368.16 -2 2 0 8630.54 379.66 2 2 0 9593.04 371.16 -2 2 0 9395.96 370.26 2 2 0 8945.61 382.16 4 -2 0 1126.49 47.20 -4 -2 0 1053.19 48.30 4 -2 0 949.11 42.50 -4 -2 0 964.60 48.60 4 -2 0 1035.20 47.20 -4 -2 0 946.21 41.60 4 2 0 1070.59 49.00 -4 2 0 971.50 53.69 4 2 0 901.41 43.60 4 2 0 1028.00 57.59 6 -2 0 340.57 23.80 -6 -2 0 343.67 19.30 6 -2 0 346.77 18.20 -6 -2 0 337.07 24.40 6 -2 0 356.16 22.00 -6 -2 0 341.47 23.40 6 2 0 383.56 25.50 6 2 0 335.07 21.70 -6 2 0 374.06 30.30 6 2 0 383.96 31.10 8 -2 0 251.77 23.30 8 -2 0 301.77 17.70 -8 -2 0 261.27 23.40 -8 -2 0 296.07 24.00 8 -2 0 328.17 21.70 8 2 0 287.77 27.60 8 2 0 322.47 25.40 8 2 0 279.57 21.60 -8 2 0 311.97 26.30 -10 -2 0 934.61 53.99 10 -2 0 956.40 45.60 10 -2 0 988.70 49.70 10 -2 0 825.52 52.89 10 2 0 967.80 56.49 10 2 0 916.11 50.59 -10 2 0 925.51 47.60 12 -2 0 2034.80 86.89 12 -2 0 1713.13 93.39 -12 -2 0 1903.31 96.79 -12 2 0 1796.12 80.19 12 2 0 1782.92 93.69 12 2 0 1954.30 96.69 12 2 0 1938.01 91.49 -12 2 0 1830.32 82.69 14 -2 0 8.70 11.50 -14 -2 0 16.10 15.10 14 -2 0 -5.70 6.20 14 2 0 8.60 9.50 14 2 0 5.90 10.60 -14 2 0 1.80 7.60 -14 2 0 -1.10 5.20 14 2 0 11.60 11.50 -14 2 0 5.40 3.50 -16 -2 0 581.84 55.09 16 -2 0 525.55 45.60 16 -2 0 618.14 42.00 16 2 0 493.85 45.50 16 2 0 560.84 43.40 -16 2 0 602.84 45.30 16 2 0 592.04 41.30 18 -2 0 541.95 47.50 18 -2 0 546.75 41.60 -18 -2 0 549.85 56.69 -18 2 0 426.96 44.20 18 2 0 506.65 47.10 18 2 0 571.64 50.59 18 2 0 505.15 38.80 20 -2 0 1871.91 101.69 -20 -2 0 1459.05 105.39 20 -2 0 1838.52 93.99 -20 2 0 1614.64 99.79 20 2 0 1663.23 87.19 20 2 0 1722.33 94.59 20 2 0 1794.72 103.09 22 -2 0 469.55 40.50 -22 -2 0 428.06 62.89 22 -2 0 485.45 46.40 22 2 0 399.16 34.10 -22 2 0 337.57 44.70 22 2 0 431.06 47.30 22 2 0 382.66 39.90 24 -2 0 1100.49 74.49 24 -2 0 1137.99 68.99 -24 -2 0 827.02 81.79 24 2 0 1078.99 69.69 24 2 0 937.01 56.59 24 2 0 1024.20 76.89 -24 2 0 901.21 75.99 26 -2 0 -7.60 20.00 26 2 0 19.10 15.50 26 2 0 12.20 18.20 28 -2 0 -14.10 12.40 28 -2 0 -27.60 12.30 -28 -2 0 36.50 24.20 28 2 0 -13.80 16.20 28 2 0 -5.10 15.80 28 2 0 -9.80 11.70 -28 2 0 8.00 19.10 30 -2 0 127.19 28.30 30 -2 0 61.09 24.60 -30 -2 0 71.79 34.80 30 2 0 57.79 25.00 30 2 0 48.00 23.80 -30 2 0 58.39 26.40 -32 -2 0 78.89 34.30 32 -2 0 39.40 19.20 32 -2 0 91.79 27.80 32 2 0 84.69 27.00 32 2 0 57.19 25.80 -32 2 0 46.80 26.10 -34 -2 0 214.68 50.19 34 -2 0 269.97 41.60 34 -2 0 256.87 42.60 -34 2 0 254.87 50.99 34 2 0 378.26 48.80 34 2 0 222.08 38.50 36 -2 0 23.00 21.80 36 -2 0 23.20 19.00 -36 -2 0 23.80 27.60 -36 2 0 17.50 25.70 36 2 0 0.30 19.50 36 2 0 23.40 20.40 38 -2 0 39.80 22.70 -38 -2 0 19.50 31.30 38 -2 0 23.80 22.20 38 2 0 -3.80 21.90 -38 2 0 40.40 29.10 38 2 0 1.80 20.80 -1 -3 0 48.60 8.90 -1 -3 0 41.90 9.80 1 -3 0 46.10 9.50 1 -3 0 45.70 7.70 1 -3 0 34.00 4.30 1 3 0 46.10 7.90 -1 3 0 38.40 6.20 -1 3 0 52.79 8.20 1 3 0 27.40 12.50 -1 3 0 37.20 15.30 3 -3 0 21.30 5.30 -3 -3 0 30.70 8.50 3 -3 0 14.70 6.30 3 -3 0 17.00 4.50 3 -3 0 27.10 5.10 3 3 0 26.90 6.80 -3 3 0 32.00 13.20 3 3 0 7.50 11.00 5 -3 0 2337.97 102.89 -5 -3 0 2237.98 104.79 -5 -3 0 2251.67 103.59 5 -3 0 2560.14 100.29 5 -3 0 2291.37 96.39 5 3 0 2391.86 119.29 -5 3 0 2298.87 113.89 5 3 0 2352.16 104.59 7 -3 0 70.49 8.10 -7 -3 0 74.49 7.30 7 -3 0 80.09 12.90 7 -3 0 92.29 14.20 -7 -3 0 62.59 12.70 -7 -3 0 86.29 13.90 -7 3 0 73.69 16.00 7 3 0 86.89 14.40 7 3 0 75.09 20.60 7 3 0 76.59 9.90 -9 -3 0 574.44 37.00 -9 -3 0 537.45 38.00 9 -3 0 520.35 27.60 9 -3 0 560.14 33.90 9 -3 0 517.35 34.90 9 3 0 580.34 38.90 9 3 0 543.25 45.00 9 3 0 511.55 30.90 -9 3 0 556.94 39.00 11 -3 0 1052.59 60.19 11 -3 0 1103.89 56.99 11 -3 0 1062.69 50.09 -11 -3 0 1055.49 60.49 -11 3 0 1068.89 59.09 11 3 0 972.60 53.89 11 3 0 1119.19 64.09 11 3 0 1035.10 67.79 -13 -3 0 317.47 32.50 13 -3 0 299.37 23.00 13 -3 0 322.07 31.70 13 -3 0 320.17 27.50 13 3 0 267.47 34.50 13 3 0 300.47 33.00 13 3 0 279.27 25.90 -13 3 0 326.17 27.20 15 -3 0 116.19 18.00 15 -3 0 106.39 23.20 -15 -3 0 108.19 25.00 15 3 0 107.49 22.70 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-18 -2.90 37.30 20 -2 -18 -1.60 36.50 -20 -2 18 57.19 29.90 20 2 -18 34.90 44.10 -20 2 18 47.30 26.80 -18 -2 18 -3.20 24.00 18 -2 -18 18.00 32.00 18 2 -18 43.90 33.00 -18 2 18 -24.90 14.90 -16 -2 18 207.98 51.99 16 -2 -18 138.99 48.00 -16 2 18 207.28 37.30 16 2 -18 109.19 47.30 -14 -2 18 6.60 19.10 14 -2 -18 70.49 37.10 14 2 -18 21.00 36.40 -14 2 18 64.39 25.70 -12 -2 18 2.60 18.50 12 -2 -18 -5.50 26.40 12 2 -18 22.40 31.90 -12 2 18 24.30 18.30 10 -2 -18 37.60 32.20 -10 -2 18 37.90 20.40 10 2 -18 13.00 29.50 -10 2 18 26.40 20.40 8 -2 -18 -27.00 21.40 -8 -2 18 30.00 19.30 8 2 -18 50.39 33.10 -8 2 18 26.30 18.70 6 -2 -18 114.29 36.30 -6 -2 18 180.68 34.90 -6 2 18 151.18 33.10 6 2 -18 159.98 41.70 4 -2 -18 19.70 23.80 -4 -2 18 -11.70 18.80 -4 2 18 -14.60 16.90 4 2 -18 17.50 21.60 -29 -3 18 33.00 23.30 29 -3 -18 58.49 48.90 -29 3 18 5.70 21.40 29 3 -18 74.09 44.20 27 -3 -18 -3.70 45.10 -27 -3 18 -23.10 17.70 -27 3 18 14.50 19.60 27 3 -18 -61.39 37.40 25 -3 -18 22.50 33.70 -25 -3 18 -2.80 17.20 25 3 -18 23.10 37.70 -25 3 18 -2.70 17.20 -23 -3 18 99.99 28.40 23 -3 -18 114.99 50.49 23 3 -18 107.49 48.90 -23 3 18 56.49 24.80 21 -3 -18 18.20 38.30 -21 -3 18 92.09 27.40 -21 3 18 81.79 27.30 21 3 -18 17.70 36.80 19 -3 -18 33.10 33.10 -19 3 18 42.60 20.60 19 3 -18 21.80 30.60 -17 -3 18 65.89 25.40 17 -3 -18 17.40 33.60 -17 3 18 35.20 24.70 17 3 -18 42.40 36.90 -15 -3 18 59.19 23.00 15 -3 -18 43.60 36.00 -15 3 18 82.99 25.00 15 3 -18 52.29 42.00 -13 -3 18 106.89 26.60 13 -3 -18 94.29 40.90 13 3 -18 94.79 40.00 -13 3 18 180.28 36.10 -11 -3 18 3.00 17.10 11 -3 -18 -35.50 25.10 11 3 -18 17.90 29.80 -11 3 18 -15.50 17.30 -9 -3 18 62.49 21.80 9 -3 -18 44.60 32.50 9 3 -18 61.99 32.20 -9 3 18 103.39 27.80 -7 -3 18 74.39 25.40 7 -3 -18 70.69 34.50 -7 3 18 46.30 25.20 7 3 -18 -19.20 27.40 -5 -3 18 29.00 21.40 5 -3 -18 49.30 25.90 5 3 -18 14.90 27.20 -5 3 18 7.60 19.80 -24 -4 18 44.90 20.90 24 -4 -18 -26.00 33.90 24 4 -18 24.20 41.10 -24 4 18 6.80 20.80 -22 -4 18 41.50 22.00 22 -4 -18 64.19 45.20 22 4 -18 53.39 47.90 -22 4 18 42.40 24.30 -20 -4 18 -25.70 15.20 20 -4 -18 -26.70 35.60 20 4 -18 34.90 38.90 -20 4 18 20.00 20.10 -18 -4 18 41.80 21.40 18 -4 -18 109.59 47.70 -18 4 18 3.10 23.10 18 4 -18 -44.70 31.10 -16 -4 18 -8.30 15.40 16 -4 -18 -6.40 30.90 16 4 -18 -33.30 33.30 -16 4 18 14.30 19.70 14 -4 -18 -21.20 26.90 -14 -4 18 41.60 22.30 -14 4 18 32.50 22.80 14 4 -18 25.30 33.10 -12 -4 18 6.80 17.50 12 -4 -18 18.80 31.60 -12 4 18 -7.00 18.70 12 4 -18 6.50 31.80 10 -4 -18 50.49 33.50 -10 -4 18 53.99 21.20 10 4 -18 36.50 28.50 -10 4 18 46.90 23.10 -28 0 19 -36.10 15.30 28 0 -19 -15.20 36.80 -26 0 19 -2.70 20.50 -24 0 19 19.80 21.70 24 0 -19 29.00 32.10 -22 0 19 25.80 20.10 22 0 -19 24.80 31.10 20 0 -19 33.90 33.00 -20 0 19 24.00 18.70 -18 0 19 -20.70 15.30 18 0 -19 43.50 33.50 -16 0 19 -10.20 19.00 16 0 -19 39.30 32.80 -14 0 19 -16.80 15.60 14 0 -19 -17.10 28.80 12 0 -19 28.30 31.80 -12 0 19 27.20 19.10 10 0 -19 32.70 27.90 -8 0 19 8.20 20.90 8 0 -19 -25.50 22.60 -29 -1 19 -32.40 23.40 29 -1 -19 -32.50 44.80 -29 1 19 6.50 22.50 29 1 -19 -14.80 43.80 27 -1 -19 -14.90 40.30 -27 -1 19 87.49 29.40 -27 1 19 35.50 26.90 27 1 -19 50.99 50.09 25 -1 -19 53.69 39.40 -25 -1 19 93.69 29.40 -25 1 19 78.89 27.10 25 1 -19 38.10 50.59 23 -1 -19 59.59 40.80 -23 -1 19 -4.00 18.30 23 1 -19 44.40 43.10 -23 1 19 18.10 21.90 21 -1 -19 -8.60 36.20 -21 -1 19 26.00 21.50 -21 1 19 62.59 25.70 21 1 -19 -7.00 39.10 19 -1 -19 -16.20 29.30 -19 -1 19 38.40 22.00 19 1 -19 11.00 35.90 -19 1 19 10.10 21.10 17 -1 -19 137.39 49.80 -17 -1 19 164.18 36.20 17 1 -19 129.19 43.70 -17 1 19 200.08 36.70 -15 -1 19 136.29 31.40 15 -1 -19 47.00 37.00 -15 1 19 106.19 29.50 15 1 -19 54.89 33.40 13 -1 -19 13.30 31.20 -13 -1 19 -15.80 15.80 13 1 -19 -39.00 28.10 -13 1 19 -12.20 16.30 -11 -1 19 13.20 16.60 11 -1 -19 -32.70 25.10 11 1 -19 6.80 25.20 -11 1 19 24.80 19.60 -9 -1 19 -15.40 19.30 9 -1 -19 5.20 28.60 -9 1 19 30.20 21.50 9 1 -19 4.80 24.70 -26 -2 19 -5.80 17.30 26 -2 -19 29.90 44.80 -26 2 19 6.30 21.70 26 2 -19 78.69 47.50 24 -2 -19 -23.70 30.80 -24 -2 19 2.20 18.50 -24 2 19 4.90 18.10 24 2 -19 46.60 39.00 22 -2 -19 41.10 40.60 -22 -2 19 6.20 19.00 22 2 -19 -54.19 35.30 -22 2 19 9.30 20.20 20 -2 -19 79.89 45.40 -20 -2 19 39.20 22.80 -20 2 19 5.10 23.50 20 2 -19 19.70 39.60 -18 -2 19 31.40 20.80 18 -2 -19 10.30 31.50 -18 2 19 27.00 23.60 18 2 -19 -8.00 35.00 16 -2 -19 25.90 28.80 -16 -2 19 -6.10 17.60 -16 2 19 11.50 23.20 16 2 -19 -7.00 35.90 14 -2 -19 -50.29 26.50 -14 -2 19 -10.10 15.60 14 2 -19 1.80 31.20 -14 2 19 9.10 20.80 12 -2 -19 2.40 30.20 -12 -2 19 -14.20 16.60 -12 2 19 45.10 23.30 12 2 -19 -18.00 30.40 10 -2 -19 2.60 30.00 -10 -2 19 7.60 21.40 -10 2 19 38.60 25.30 10 2 -19 67.19 36.20 -19 -3 19 21.20 18.70 19 -3 -19 1.90 34.10 -19 3 19 2.30 18.80 19 3 -19 4.20 37.30 -17 -3 19 62.29 23.70 17 -3 -19 84.49 42.40 17 3 -19 123.79 48.60 -17 3 19 95.49 29.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 15430 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.77615(2) 0.50480(6) 1.17007(4) 0.02513(12) Uani 1 1 d . . . . . Br2 Br 0.40928(2) 0.18946(6) 0.36162(3) 0.01808(10) Uani 1 1 d . . . . . Se1 Se 0.49609(2) 0.27838(6) 0.59712(3) 0.01576(10) Uani 1 1 d . . . . . N2 N 0.54828(14) 0.3240(5) 0.7353(3) 0.0173(7) Uani 1 1 d . . . . . C3 C 0.59093(16) 0.3257(5) 0.7307(3) 0.0152(8) Uani 1 1 d . . . . . N4 N 0.59063(14) 0.2901(4) 0.6224(3) 0.0147(7) Uani 1 1 d . . . . . C5 C 0.54365(17) 0.2630(5) 0.5388(3) 0.0168(8) Uani 1 1 d . . . . . C6 C 0.53744(17) 0.2285(6) 0.4287(3) 0.0183(8) Uani 1 1 d . . . . . H6 H 0.5048 0.2150 0.3692 0.022 Uiso 1 1 calc R U . . . C7 C 0.57889(18) 0.2142(6) 0.4073(4) 0.0214(9) Uani 1 1 d . . . . . H7 H 0.5751 0.1913 0.3325 0.026 Uiso 1 1 calc R U . . . C8 C 0.62716(17) 0.2335(6) 0.4958(3) 0.0178(8) Uani 1 1 d . . . . . H8 H 0.6560 0.2206 0.4812 0.021 Uiso 1 1 calc R U . . . C9 C 0.63253(16) 0.2705(5) 0.6022(3) 0.0173(8) Uani 1 1 d . . . . . H9 H 0.6651 0.2827 0.6623 0.021 Uiso 1 1 calc R U . . . C10 C 0.63836(16) 0.3607(5) 0.8330(3) 0.0159(8) Uani 1 1 d . . . . . C11 C 0.67537(17) 0.4823(5) 0.8331(3) 0.0178(8) Uani 1 1 d . . . . . H11 H 0.6720 0.5403 0.7648 0.021 Uiso 1 1 calc R U . . . C12 C 0.71732(17) 0.5185(5) 0.9336(3) 0.0183(8) Uani 1 1 d . . . . . H12 H 0.7433 0.5985 0.9341 0.022 Uiso 1 1 calc R U . . . C13 C 0.72081(17) 0.4370(6) 1.0324(3) 0.0198(9) Uani 1 1 d . . . . . C14 C 0.68436(17) 0.3175(6) 1.0344(3) 0.0190(9) Uani 1 1 d . . . . . H14 H 0.6874 0.2634 1.1034 0.023 Uiso 1 1 calc R U . . . C15 C 0.64301(16) 0.2778(6) 0.9333(3) 0.0181(8) Uani 1 1 d . . . . . H15 H 0.6179 0.1937 0.9329 0.022 Uiso 1 1 calc R U . . . 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 Br1 0.0251(2) 0.0211(2) 0.0191(2) -0.00225(15) -0.00028(17) 0.00351(18) Br2 0.0190(2) 0.0193(2) 0.01552(19) 0.00194(14) 0.00697(16) 0.00167(16) Se1 0.0151(2) 0.01775(19) 0.01422(19) 0.00011(14) 0.00609(16) -0.00011(16) N2 0.0195(19) 0.0171(16) 0.0130(16) -0.0008(12) 0.0048(14) -0.0009(14) C3 0.020(2) 0.0115(17) 0.0154(18) 0.0010(13) 0.0091(16) -0.0009(15) N4 0.0208(19) 0.0121(15) 0.0123(15) -0.0010(11) 0.0079(14) -0.0012(13) C5 0.021(2) 0.0121(17) 0.0174(19) 0.0022(14) 0.0086(17) 0.0010(15) C6 0.017(2) 0.020(2) 0.0170(19) 0.0005(15) 0.0060(17) 0.0005(16) C7 0.028(3) 0.019(2) 0.019(2) -0.0004(15) 0.0112(19) -0.0014(18) C8 0.022(2) 0.0167(19) 0.020(2) 0.0004(14) 0.0144(18) -0.0025(16) C9 0.017(2) 0.0182(19) 0.0177(19) 0.0009(14) 0.0076(17) -0.0001(16) C10 0.015(2) 0.0145(18) 0.0173(19) 0.0002(14) 0.0059(16) 0.0008(15) C11 0.022(2) 0.0148(18) 0.0175(19) 0.0001(14) 0.0091(17) 0.0010(16) C12 0.017(2) 0.0158(19) 0.022(2) -0.0013(15) 0.0074(17) 0.0016(16) C13 0.022(2) 0.019(2) 0.0148(19) -0.0029(15) 0.0038(17) 0.0035(17) C14 0.021(2) 0.022(2) 0.0163(19) 0.0029(15) 0.0096(17) 0.0056(17) C15 0.015(2) 0.020(2) 0.019(2) 0.0026(15) 0.0069(17) 0.0036(16) 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' Br Br -0.2901 2.4595 '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' Se Se -0.0929 2.2259 '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 N2 Se1 C5 87.31(17) . . ? C3 N2 Se1 112.5(3) . . ? N2 C3 N4 116.7(4) . . ? N2 C3 C10 121.5(4) . . ? N4 C3 C10 121.8(4) . . ? C5 N4 C9 121.2(3) . . ? C5 N4 C3 113.2(4) . . ? C9 N4 C3 125.4(4) . . ? N4 C5 C6 119.7(4) . . ? N4 C5 Se1 110.3(3) . . ? C6 C5 Se1 130.0(3) . . ? C7 C6 C5 119.3(4) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C8 120.1(4) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 119.9(4) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 N4 119.6(4) . . ? C8 C9 H9 120.2 . . ? N4 C9 H9 120.2 . . ? C15 C10 C11 120.1(4) . . ? C15 C10 C3 117.0(4) . . ? C11 C10 C3 122.7(4) . . ? C10 C11 C12 119.7(4) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 119.2(4) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 C12 121.9(4) . . ? C14 C13 Br1 119.9(3) . . ? C12 C13 Br1 118.1(3) . . ? C13 C14 C15 118.8(4) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C10 C15 C14 120.2(4) . . ? C10 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? 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 Br1 C13 1.905(4) . ? Se1 N2 1.835(3) . ? Se1 C5 1.860(4) . ? N2 C3 1.282(6) . ? C3 N4 1.435(5) . ? C3 C10 1.487(6) . ? N4 C5 1.363(5) . ? N4 C9 1.374(5) . ? C5 C6 1.393(6) . ? C6 C7 1.367(6) . ? C6 H6 0.9500 . ? C7 C8 1.406(6) . ? C7 H7 0.9500 . ? C8 C9 1.357(6) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.391(6) . ? C10 C11 1.392(6) . ? C11 C12 1.392(6) . ? C11 H11 0.9500 . ? C12 C13 1.380(6) . ? C12 H12 0.9500 . ? C13 C14 1.379(6) . ? C14 C15 1.393(6) . ? C14 H14 0.9500 . ? C15 H15 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 C5 Se1 N2 C3 0.3(3) . . . . ? Se1 N2 C3 N4 -0.9(4) . . . . ? Se1 N2 C3 C10 179.8(3) . . . . ? N2 C3 N4 C5 1.2(5) . . . . ? C10 C3 N4 C5 -179.4(3) . . . . ? N2 C3 N4 C9 -174.2(4) . . . . ? C10 C3 N4 C9 5.1(6) . . . . ? C9 N4 C5 C6 -4.9(6) . . . . ? C3 N4 C5 C6 179.5(3) . . . . ? C9 N4 C5 Se1 174.7(3) . . . . ? C3 N4 C5 Se1 -0.9(4) . . . . ? N2 Se1 C5 N4 0.4(3) . . . . ? N2 Se1 C5 C6 179.9(4) . . . . ? N4 C5 C6 C7 2.8(6) . . . . ? Se1 C5 C6 C7 -176.7(3) . . . . ? C5 C6 C7 C8 0.3(6) . . . . ? C6 C7 C8 C9 -1.5(6) . . . . ? C7 C8 C9 N4 -0.4(6) . . . . ? C5 N4 C9 C8 3.7(6) . . . . ? C3 N4 C9 C8 178.8(4) . . . . ? N2 C3 C10 C15 40.2(6) . . . . ? N4 C3 C10 C15 -139.1(4) . . . . ? N2 C3 C10 C11 -134.8(4) . . . . ? N4 C3 C10 C11 45.9(6) . . . . ? C15 C10 C11 C12 0.8(6) . . . . ? C3 C10 C11 C12 175.6(4) . . . . ? C10 C11 C12 C13 -1.8(6) . . . . ? C11 C12 C13 C14 1.3(6) . . . . ? C11 C12 C13 Br1 -175.3(3) . . . . ? C12 C13 C14 C15 0.3(6) . . . . ? Br1 C13 C14 C15 176.8(3) . . . . ? C11 C10 C15 C14 0.7(6) . . . . ? C3 C10 C15 C14 -174.3(4) . . . . ? C13 C14 C15 C10 -1.3(6) . . . . ?