#------------------------------------------------------------------------------ #$Date: 2026-05-28 01:36:31 +0100 (Thu, 28 May 2026) $ #$Revision: 306107 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/44/7064420.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_7064420 loop_ _publ_author_name 'Walha, Sandra' 'Hjiri, Mokhtar' 'Ben Ahmed, Ali' _publ_section_title ; Mixed-halide engineering in a homopiperazinium hybrid salt: structural disorder description, electronic structure analysis, and bioactivity evaluation ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D6NJ01450J _journal_year 2026 _chemical_formula_sum 'C10 H28 Br3 Cl N4' _chemical_formula_weight 479.54 _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' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2019/3 _audit_update_record ; 2025-12-11 deposited with the CCDC. 2026-05-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 107.528(7) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.2340(16) _cell_length_b 9.7895(19) _cell_length_c 11.358(2) _cell_measurement_reflns_used 2017 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.39 _cell_measurement_theta_min 1.80 _cell_volume 873.0(3) _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'CAD4 plate' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_unetI/netI 0.0450 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 7490 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.563 _diffrn_reflns_theta_min 2.707 _exptl_absorpt_coefficient_mu 7.076 _exptl_crystal_colour white _exptl_crystal_density_diffrn 1.824 _exptl_crystal_description Plate _exptl_crystal_F_000 476 _refine_diff_density_max 1.753 _refine_diff_density_min -1.354 _refine_diff_density_rms 0.200 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 82 _refine_ls_number_reflns 2012 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.096 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0486 _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^)+(0.0755P)^2^+4.8414P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1365 _refine_ls_wR_factor_ref 0.1423 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1772 _reflns_number_total 2012 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6nj01450j2.cif _cod_data_source_block shelx _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7064420 _shelx_shelxl_version_number 2019/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; TITL import_a.res in P2(1)/n (created by CRYSCALC) shelx.res created by SHELXL-2019/3 at 12:03:30 on 06-Dec-2025 CELL 0.71073 8.2340 9.7895 11.3583 90.000 107.528 90.000 ZERR 2.00 0.0016 0.0019 0.0021 0.000 0.007 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N CL BR UNIT 20 56 8 2 6 MERG 2 EXYZ CL1 BR1 EADP CL1 BR1 FMAP 2 ACTA PLAN -150 ACTA HTAB BOND $H EQIV $1 x-1/2, -y+3/2, z-1/2 HTAB N1 Cl1_$1 HTAB N1 Cl1 EQIV $2 -x+1/2, y+1/2, -z+3/2 HTAB N1 Br2_$2 HTAB C2 Br1_$2 HTAB C2 Br2_$2 HTAB C2 Br2_$1 HTAB C3 Br1 HTAB C4 Br2_$1 EQIV $3 x+1/2, -y+3/2, z-1/2 HTAB C4 Cl1_$3 EQIV $4 -x+3/2, y+1/2, -z+3/2 HTAB C4 Br2_$4 HTAB N5 Br2 HTAB N5 Cl1_$3 EQIV $5 -x+1, -y+1, -z+1 HTAB N5 Br2_$5 EQIV $6 -x+1/2, y-1/2, -z+3/2 HTAB C6 Cl1_$6 HTAB C6 Br2_$5 HTAB C7 Br2 CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.075500 4.841400 FVAR 0.42072 MOLE 1 N1 3 0.104486 0.782896 0.630095 11.00000 0.00738 0.00699 = 0.00894 -0.00147 0.00565 -0.00044 AFIX 23 H1A 2 -0.007452 0.784311 0.584927 11.00000 -1.20000 H1B 2 0.109479 0.786721 0.711161 11.00000 -1.20000 AFIX 0 C2 1 0.187760 0.908453 0.599839 11.00000 0.01150 0.00436 = 0.00983 -0.00042 0.00803 0.00211 AFIX 23 H2A 2 0.156377 0.987724 0.642571 11.00000 -1.20000 H2B 2 0.143915 0.925545 0.509884 11.00000 -1.20000 AFIX 0 C3 1 0.382032 0.897021 0.637416 11.00000 0.01002 0.00899 = 0.01260 -0.00197 0.00251 -0.00105 AFIX 23 H3A 2 0.431421 0.989134 0.659540 11.00000 -1.20000 H3B 2 0.420574 0.839212 0.712199 11.00000 -1.20000 AFIX 0 C4 1 0.451162 0.837852 0.539271 11.00000 0.00926 0.01094 = 0.01312 0.00184 0.00736 0.00045 AFIX 23 H4A 2 0.401411 0.888648 0.461345 11.00000 -1.20000 H4B 2 0.575964 0.852081 0.564569 11.00000 -1.20000 AFIX 0 N5 3 0.415216 0.688527 0.515177 11.00000 0.01389 0.00924 = 0.00987 0.00195 0.00836 0.00667 AFIX 23 H5A 2 0.480561 0.640879 0.581327 11.00000 -1.20000 H5B 2 0.448761 0.664206 0.448733 11.00000 -1.20000 AFIX 0 C6 1 0.233171 0.645358 0.491494 11.00000 0.01274 0.00792 = 0.01047 -0.00227 0.00498 0.00119 AFIX 23 H6A 2 0.218578 0.551455 0.457566 11.00000 -1.20000 H6B 2 0.158496 0.706668 0.428930 11.00000 -1.20000 AFIX 0 C7 1 0.179290 0.649111 0.607300 11.00000 0.01435 0.00366 = 0.01288 0.00076 0.00832 0.00014 AFIX 23 H7A 2 0.094201 0.576131 0.602172 11.00000 -1.20000 H7B 2 0.279617 0.628540 0.678931 11.00000 -1.20000 AFIX 0 MOLE 2 CL1 4 0.266368 0.780226 0.920325 10.50000 0.01746 0.01935 = 0.01505 0.00266 0.00436 0.00134 BR1 5 0.266368 0.780226 0.920325 10.50000 0.01746 0.01935 = 0.01505 0.00266 0.00436 0.00134 MOLE 3 BR2 5 0.637723 0.510248 0.748507 11.00000 0.01909 0.02495 = 0.01289 0.00171 0.00424 0.00448 HKLF 4 REM import_a.res in P2(1)/n (created by CRYSCALC) REM wR2 = 0.1423, GooF = S = 1.096, Restrained GooF = 1.096 for all data REM R1 = 0.0486 for 1772 Fo > 4sig(Fo) and 0.0557 for all 2012 data REM 82 parameters refined using 0 restraints END WGHT 0.0747 5.5249 REM Instructions for potential hydrogen bonds HTAB N1 Cl1_$1 HTAB N1 Cl1 HTAB N1 Br2_$2 HTAB C2 Br1_$2 HTAB C2 Br2_$2 HTAB C2 Br2_$1 HTAB C3 Br1 HTAB C4 Br2_$1 HTAB C4 Cl1_$3 HTAB C4 Br2_$4 HTAB N5 Br2 HTAB N5 Cl1_$3 HTAB N5 Br2_$5 HTAB C6 Cl1_$6 HTAB C6 Br2_$5 HTAB C7 Br2 REM Highest difference peak 1.753, deepest hole -1.354, 1-sigma level 0.200 Q1 1 -0.1584 1.0955 0.7429 11.00000 0.05 1.75 Q2 1 -0.1480 0.8849 0.7403 11.00000 0.05 1.06 Q3 1 -0.1509 0.7323 0.7489 11.00000 0.05 0.94 Q4 1 0.2283 1.1673 0.5788 11.00000 0.05 0.93 Q5 1 0.3471 0.6874 0.5178 11.00000 0.05 0.81 Q6 1 -0.0594 0.9186 0.7047 11.00000 0.05 0.79 Q7 1 -0.1988 1.1055 0.8181 11.00000 0.05 0.76 Q8 1 0.2051 1.3875 0.5516 11.00000 0.05 0.72 Q9 1 0.3255 1.1898 0.5388 11.00000 0.05 0.70 Q10 1 -0.0807 0.9169 0.8014 11.00000 0.05 0.70 Q11 1 -0.1963 0.9268 0.8177 11.00000 0.05 0.69 Q12 1 -0.1464 1.1738 0.7369 11.00000 0.05 0.67 Q13 1 -0.0581 1.1024 0.7047 11.00000 0.05 0.67 Q14 1 0.3017 1.3670 0.5214 11.00000 0.05 0.67 Q15 1 0.4247 0.8791 0.6753 11.00000 0.05 0.65 Q16 1 0.1443 1.3621 0.6225 11.00000 0.05 0.64 Q17 1 0.3320 0.9000 0.6336 11.00000 0.05 0.64 Q18 1 0.4069 0.8478 0.5030 11.00000 0.05 0.63 Q19 1 0.1172 1.1902 0.6069 11.00000 0.05 0.62 Q20 1 -0.0295 1.1728 0.7021 11.00000 0.05 0.61 Q21 1 -0.0704 0.9914 0.8056 11.00000 0.05 0.60 Q22 1 0.4691 0.7018 0.5590 11.00000 0.05 0.60 Q23 1 0.4476 0.7513 0.5384 11.00000 0.05 0.60 Q24 1 0.1527 0.8054 0.6001 11.00000 0.05 0.58 Q25 1 0.4282 0.8629 0.5732 11.00000 0.05 0.55 Q26 1 0.1808 0.9137 0.5623 11.00000 0.05 0.55 Q27 1 -0.1814 1.0130 0.8210 11.00000 0.05 0.54 Q28 1 0.3855 1.0328 0.6197 11.00000 0.05 0.53 Q29 1 0.1782 1.3082 0.6372 11.00000 0.05 0.51 Q30 1 -0.1481 0.7009 0.4988 11.00000 0.05 0.49 Q31 1 0.1928 0.8448 0.8449 11.00000 0.05 0.48 Q32 1 -0.2723 1.1885 0.8007 11.00000 0.05 0.48 Q33 1 0.4044 0.5517 0.5176 11.00000 0.05 0.48 Q34 1 -0.0574 1.0257 0.8165 11.00000 0.05 0.48 Q35 1 0.1262 0.8199 0.6555 11.00000 0.05 0.47 Q36 1 0.1760 0.6400 0.5491 11.00000 0.05 0.47 Q37 1 0.2401 0.6656 0.4493 11.00000 0.05 0.46 Q38 1 0.2289 0.8853 0.6201 11.00000 0.05 0.46 Q39 1 0.5041 0.8459 0.5241 11.00000 0.05 0.45 Q40 1 0.1127 0.7651 0.6615 11.00000 0.05 0.44 Q41 1 0.0773 0.7602 0.6394 11.00000 0.05 0.44 Q42 1 0.1306 0.6424 0.6262 11.00000 0.05 0.44 Q43 1 0.0843 0.8428 0.3748 11.00000 0.05 0.43 Q44 1 -0.1934 1.2619 0.7134 11.00000 0.05 0.43 Q45 1 0.6216 0.9114 0.4647 11.00000 0.05 0.43 Q46 1 0.4409 0.8251 0.3455 11.00000 0.05 0.42 Q47 1 -0.1986 0.9458 0.6312 11.00000 0.05 0.42 Q48 1 0.1857 0.6602 0.4683 11.00000 0.05 0.41 Q49 1 0.2501 0.6096 0.4880 11.00000 0.05 0.41 Q50 1 -0.0973 0.9138 0.5958 11.00000 0.05 0.40 Q51 1 0.1470 0.9275 0.6424 11.00000 0.05 0.40 Q52 1 0.0898 1.0065 0.6448 11.00000 0.05 0.40 Q53 1 -0.2913 1.0042 0.8138 11.00000 0.05 0.40 Q54 1 0.3682 0.7399 0.6060 11.00000 0.05 0.39 Q55 1 0.4319 0.7762 0.9371 11.00000 0.05 0.39 Q56 1 -0.0460 0.9761 0.8764 11.00000 0.05 0.39 Q57 1 0.1992 0.6148 0.6191 11.00000 0.05 0.38 Q58 1 0.3946 0.9435 0.6203 11.00000 0.05 0.38 Q59 1 0.4463 0.7422 0.7783 11.00000 0.05 0.38 Q60 1 0.0087 1.0044 0.6756 11.00000 0.05 0.38 Q61 1 0.5560 1.0084 0.6709 11.00000 0.05 0.38 Q62 1 0.6242 0.6978 0.5195 11.00000 0.05 0.37 Q63 1 0.1014 1.0188 0.3931 11.00000 0.05 0.36 Q64 1 0.2192 0.7372 0.3386 11.00000 0.05 0.35 Q65 1 0.0768 0.5497 0.6420 11.00000 0.05 0.35 Q66 1 0.3236 0.6523 0.3789 11.00000 0.05 0.35 Q67 1 0.4099 0.7760 0.8334 11.00000 0.05 0.35 Q68 1 0.3051 1.0756 0.6862 11.00000 0.05 0.35 Q69 1 -0.0294 0.8422 0.6988 11.00000 0.05 0.34 Q70 1 0.3986 1.0009 0.5215 11.00000 0.05 0.34 Q71 1 -0.1686 0.7747 0.5108 11.00000 0.05 0.34 Q72 1 0.5018 0.8997 0.8365 11.00000 0.05 0.34 Q73 1 0.1732 1.0266 0.5190 11.00000 0.05 0.33 Q74 1 0.6195 0.8575 0.6607 11.00000 0.05 0.33 Q75 1 -0.1981 1.1420 0.6613 11.00000 0.05 0.33 Q76 1 -0.0343 0.6693 0.5567 11.00000 0.05 0.33 Q77 1 0.0259 0.8182 0.7190 11.00000 0.05 0.33 Q78 1 0.7248 0.7761 0.5595 11.00000 0.05 0.33 Q79 1 0.1318 0.7847 0.9359 11.00000 0.05 0.33 Q80 1 0.0944 1.1095 0.6252 11.00000 0.05 0.33 Q81 1 -0.0976 0.9177 0.5208 11.00000 0.05 0.32 Q82 1 0.4364 0.8951 0.9823 11.00000 0.05 0.32 Q83 1 0.4452 0.8006 0.7065 11.00000 0.05 0.32 Q84 1 0.4706 0.8163 0.7892 11.00000 0.05 0.32 Q85 1 0.5445 1.0660 0.6671 11.00000 0.05 0.32 Q86 1 -0.3049 1.0032 0.7235 11.00000 0.05 0.32 Q87 1 0.0164 1.0161 0.7669 11.00000 0.05 0.31 Q88 1 -0.0815 0.7932 0.4861 11.00000 0.05 0.29 Q89 1 0.0091 0.7800 0.6991 11.00000 0.05 0.29 Q90 1 0.0987 0.8163 0.8813 11.00000 0.05 0.29 Q91 1 0.1490 0.4759 0.3816 11.00000 0.05 0.29 Q92 1 0.5667 0.8121 0.7214 11.00000 0.05 0.29 Q93 1 0.1736 0.6354 0.8063 11.00000 0.05 0.28 Q94 1 0.1057 0.9344 0.9452 11.00000 0.05 0.28 Q95 1 0.3800 0.8440 0.7723 11.00000 0.05 0.28 Q96 1 0.2016 0.4919 0.7005 11.00000 0.05 0.28 Q97 1 0.0473 0.6560 0.4617 11.00000 0.05 0.27 Q98 1 -0.3163 0.8503 0.7579 11.00000 0.05 0.27 Q99 1 0.0440 0.9595 0.8379 11.00000 0.05 0.27 Q100 1 0.4960 0.5188 0.4592 11.00000 0.05 0.27 Q101 1 -0.1024 0.6741 0.6803 11.00000 0.05 0.27 Q102 1 0.0314 0.9107 0.6529 11.00000 0.05 0.27 Q103 1 0.2768 0.5017 0.5012 11.00000 0.05 0.27 Q104 1 0.5509 0.8992 0.6490 11.00000 0.05 0.27 Q105 1 0.2684 1.0111 0.5607 11.00000 0.05 0.27 Q106 1 0.5219 1.0807 0.6018 11.00000 0.05 0.27 Q107 1 0.1515 0.9757 0.7085 11.00000 0.05 0.26 Q108 1 0.4973 0.9002 0.4613 11.00000 0.05 0.26 Q109 1 0.3762 0.5026 0.4370 11.00000 0.05 0.26 Q110 1 0.3198 0.8968 0.3827 11.00000 0.05 0.26 Q111 1 0.6919 0.9153 0.6756 11.00000 0.05 0.26 Q112 1 0.1947 0.9138 0.8165 11.00000 0.05 0.25 Q113 1 0.1702 0.7941 0.7605 11.00000 0.05 0.25 Q114 1 0.0696 0.7135 0.8239 11.00000 0.05 0.25 Q115 1 0.1786 1.0464 0.4643 11.00000 0.05 0.25 Q116 1 0.0569 0.9086 0.8388 11.00000 0.05 0.25 Q117 1 0.2806 0.8205 0.5607 11.00000 0.05 0.24 Q118 1 0.7180 0.8462 0.6247 11.00000 0.05 0.24 Q119 1 0.2686 0.5387 0.5621 11.00000 0.05 0.24 Q120 1 -0.1884 1.1603 0.8812 11.00000 0.05 0.24 Q121 1 0.1197 0.7805 0.4447 11.00000 0.05 0.24 Q122 1 0.1709 0.4669 0.4833 11.00000 0.05 0.24 Q123 1 0.3530 0.5430 0.6649 11.00000 0.05 0.23 Q124 1 0.2984 0.9950 0.6633 11.00000 0.05 0.23 Q125 1 0.6750 0.3340 0.8406 11.00000 0.05 0.23 Q126 1 0.3487 0.6301 0.6056 11.00000 0.05 0.23 Q127 1 0.3410 1.1235 0.6251 11.00000 0.05 0.23 Q128 1 0.4272 1.0555 0.7003 11.00000 0.05 0.23 Q129 1 0.2269 0.8058 1.0566 11.00000 0.05 0.23 Q130 1 -0.0269 0.6777 0.6226 11.00000 0.05 0.22 Q131 1 0.5975 0.7853 0.5853 11.00000 0.05 0.22 Q132 1 -0.0933 0.7960 0.6133 11.00000 0.05 0.22 Q133 1 0.0033 0.6639 0.6569 11.00000 0.05 0.22 Q134 1 0.4550 1.1272 0.6574 11.00000 0.05 0.21 Q135 1 0.0284 0.9004 0.5388 11.00000 0.05 0.21 Q136 1 0.1302 0.7551 0.5157 11.00000 0.05 0.21 Q137 1 0.4355 0.7831 0.4184 11.00000 0.05 0.21 Q138 1 0.5708 0.7617 0.6426 11.00000 0.05 0.21 Q139 1 0.4591 0.6417 0.8382 11.00000 0.05 0.21 Q140 1 0.0039 0.9161 0.4803 11.00000 0.05 0.21 Q141 1 0.5744 0.7966 0.5031 11.00000 0.05 0.20 Q142 1 0.0632 1.0020 0.5409 11.00000 0.05 0.20 Q143 1 0.6803 0.9553 0.5962 11.00000 0.05 0.20 Q144 1 0.4185 0.7130 0.3173 11.00000 0.05 0.20 Q145 1 0.6274 0.8541 0.5187 11.00000 0.05 0.19 Q146 1 -0.0617 0.7502 0.5372 11.00000 0.05 0.19 Q147 1 0.3979 0.7260 0.6786 11.00000 0.05 0.19 Q148 1 0.0531 0.6849 0.8097 11.00000 0.05 0.19 Q149 1 0.4872 0.9758 0.4507 11.00000 0.05 0.18 Q150 1 0.5925 0.6862 0.5993 11.00000 0.05 0.18 ; _shelx_res_checksum 253 _shelx_hkl_file ; 1 0 0 -0.29 0.27 -1 0 0 0.37 0.53 2 0 0 1962.67 113.17 -3 0 0 -0.46 1.76 3 0 0 -2.33 1.50 3 0 0 0.12 1.21 4 0 0 579.85 33.06 4 0 0 609.87 33.27 -4 0 0 489.78 33.43 5 0 0 -2.16 2.39 5 0 0 0.65 2.17 -5 0 0 -2.89 3.07 6 0 0 88.39 7.50 7 0 0 0.06 3.05 7 0 0 -0.16 3.60 -8 0 0 455.39 33.52 8 0 0 543.13 30.91 9 0 0 -5.09 3.92 9 0 0 0.30 3.40 10 0 0 138.44 10.06 10 0 0 151.37 10.23 0 -1 0 1.71 3.32 1 -1 0 867.53 47.21 1 -1 0 798.53 47.14 -1 1 0 781.44 47.15 -2 -1 0 2.83 0.80 2 -1 0 1.20 1.08 2 -1 0 2.21 0.96 2 1 0 2.20 0.63 -2 1 0 1.46 1.04 3 -1 0 1362.34 77.35 3 -1 0 1374.43 77.53 -3 1 0 1336.27 77.57 3 1 0 1337.61 77.13 3 1 0 1271.73 77.16 4 -1 0 55.52 5.22 4 -1 0 57.31 5.03 4 1 0 60.56 4.42 -4 1 0 57.23 5.64 4 1 0 53.80 4.73 5 -1 0 167.13 11.34 5 -1 0 168.96 11.55 5 1 0 170.77 10.80 -5 1 0 181.79 12.36 5 1 0 159.47 11.06 6 -1 0 166.31 11.64 6 -1 0 148.46 11.24 6 1 0 166.55 10.66 -6 1 0 168.33 13.05 6 1 0 153.50 10.97 7 -1 0 631.70 39.00 7 1 0 666.55 38.12 -7 1 0 648.03 40.59 7 1 0 627.61 38.26 8 -1 0 96.37 9.80 -8 1 0 90.43 13.55 8 1 0 78.56 7.54 8 1 0 110.39 7.61 -9 -1 0 -12.16 7.15 9 -1 0 0.71 4.41 9 -1 0 -1.45 4.39 -9 1 0 -5.65 7.53 10 -1 0 57.83 8.55 -10 1 0 36.28 12.24 0 -2 0 37.33 2.68 0 -2 0 36.64 2.64 1 -2 0 303.17 16.80 1 -2 0 278.14 16.71 -1 -2 0 272.83 16.44 -1 2 0 270.90 16.72 1 2 0 286.17 16.37 2 -2 0 231.92 13.27 -2 -2 0 216.70 12.66 2 -2 0 207.34 13.04 -2 2 0 205.60 13.14 3 -2 0 24.66 3.56 3 -2 0 25.96 3.01 3 2 0 21.43 1.66 3 2 0 20.58 1.67 -3 2 0 26.00 3.50 4 -2 0 2651.79 142.63 4 -2 0 2476.60 142.17 -4 -2 0 2134.83 142.03 -4 2 0 2585.60 142.68 5 -2 0 -1.58 2.60 5 -2 0 1.35 2.22 -5 -2 0 1.82 2.64 5 2 0 2.04 1.15 -5 2 0 -0.77 3.09 5 2 0 1.16 1.18 6 -2 0 1120.60 65.31 -6 -2 0 1067.59 65.37 6 -2 0 1055.57 64.65 -6 2 0 1182.35 65.99 6 2 0 1104.67 63.74 6 2 0 1094.53 63.72 7 -2 0 9.74 3.53 7 -2 0 8.60 4.36 -7 -2 0 0.32 4.70 -7 2 0 6.43 5.43 8 -2 0 34.95 6.24 8 -2 0 41.23 6.86 -8 2 0 31.20 7.90 9 -2 0 40.49 7.52 9 -2 0 24.77 6.23 -9 2 0 18.43 9.06 10 -2 0 11.73 5.60 -10 2 0 6.86 11.01 0 -3 0 0.66 1.01 0 -3 0 1.46 1.06 1 -3 0 1013.14 59.65 -1 -3 0 997.83 59.38 1 -3 0 1067.83 59.72 -1 3 0 1032.28 59.67 2 -3 0 127.79 8.36 -2 -3 0 127.42 7.55 2 -3 0 113.08 7.99 -2 3 0 123.55 8.25 3 -3 0 1586.81 93.46 -3 -3 0 1595.16 92.99 3 -3 0 1693.26 93.81 -3 3 0 1576.61 93.68 -4 -3 0 367.78 22.61 4 -3 0 395.91 23.77 -4 3 0 388.66 23.73 5 -3 0 4.41 3.31 -5 -3 0 8.52 2.26 5 -3 0 11.60 2.82 -5 3 0 7.46 3.61 6 -3 0 169.38 13.14 6 -3 0 171.85 11.90 -6 -3 0 167.66 11.96 -6 3 0 161.83 13.27 7 -3 0 221.12 17.77 7 -3 0 237.74 16.49 -7 -3 0 279.77 17.67 -7 3 0 250.67 19.01 8 -3 0 10.03 4.11 -8 -3 0 22.88 6.24 8 -3 0 6.10 5.56 -8 3 0 11.73 7.36 9 -3 0 17.95 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12 77.72 10.81 0 6 -12 96.58 13.72 -4 -7 12 -2.39 5.17 4 -7 -12 4.61 5.47 4 7 -12 6.87 8.89 3 -7 -12 110.80 12.24 -3 -7 12 100.51 11.71 3 7 -12 111.05 16.75 -2 -7 12 11.00 5.83 -2 -7 12 5.66 7.34 2 -7 -12 11.84 6.49 2 7 -12 18.47 8.56 -1 -7 12 39.97 8.44 -1 -7 12 43.34 7.31 1 -7 -12 46.71 8.79 7 0 -13 -2.37 8.27 -7 0 13 18.76 6.83 6 0 -13 -12.93 7.92 -6 0 13 11.40 6.08 5 0 -13 948.04 60.76 -5 0 13 956.86 57.88 -4 0 13 12.95 5.95 -3 0 13 187.87 15.53 -2 0 13 7.58 4.97 -2 0 13 -4.05 3.92 2 0 -13 -4.01 7.09 -1 0 13 140.59 10.47 1 0 -13 160.17 15.07 -1 0 13 113.32 11.48 0 0 -13 7.47 5.67 0 0 13 2.21 1.81 0 0 13 -0.71 2.19 -1 0 -13 100.83 11.84 7 -1 -13 -6.52 8.04 -7 -1 13 10.22 6.12 -7 1 13 13.04 6.95 7 1 -13 5.97 9.24 6 -1 -13 395.76 29.20 -6 -1 13 405.29 26.88 -6 1 13 422.98 27.59 6 1 -13 343.39 30.36 5 -1 -13 196.98 21.21 -5 -1 13 234.59 18.08 -5 1 13 243.39 18.56 4 -1 -13 13.61 9.74 -4 1 13 24.53 6.39 4 1 -13 -6.46 9.16 3 -1 -13 71.55 12.35 -3 1 13 87.34 10.63 3 1 -13 53.81 11.04 -2 -1 13 195.61 14.63 2 -1 -13 147.51 18.06 -2 1 13 186.88 13.00 2 1 -13 172.52 17.77 1 -1 -13 85.38 13.30 -1 -1 13 107.91 9.70 1 1 -13 99.64 13.39 -1 1 13 90.51 7.67 -1 1 13 98.42 7.10 0 -1 13 41.82 7.84 0 -1 13 28.67 4.38 0 -1 -13 27.55 6.67 0 1 -13 38.31 7.53 -1 -1 -13 205.13 16.42 -1 1 -13 206.68 17.16 -7 -2 13 126.02 13.14 7 -2 -13 91.51 14.33 7 2 -13 96.47 17.76 -7 2 13 141.42 15.04 6 -2 -13 10.37 8.32 6 2 -13 -0.48 9.81 -5 2 13 42.88 7.68 5 2 -13 25.10 11.17 -4 2 13 51.50 7.71 4 2 -13 36.60 10.75 3 -2 -13 -2.82 8.74 -3 2 13 1.35 4.92 3 2 -13 -4.81 7.87 -2 -2 13 28.53 6.41 2 -2 -13 -0.13 8.66 2 2 -13 23.64 7.79 -2 2 13 19.54 4.01 -2 2 13 21.37 3.28 1 -2 -13 303.10 24.61 -1 -2 13 354.18 22.34 1 2 -13 333.90 24.65 0 -2 -13 12.71 5.98 0 -2 13 14.28 4.45 0 2 -13 17.44 6.39 1 -2 13 171.99 12.69 -1 -2 -13 161.98 14.13 1 -2 13 141.28 11.50 -1 2 -13 165.22 15.11 -7 -3 13 25.17 6.37 -7 3 13 22.34 7.92 6 -3 -13 6.54 7.36 -6 -3 13 22.94 5.94 -6 3 13 21.46 7.29 6 3 -13 10.86 10.70 5 -3 -13 91.90 13.90 5 3 -13 44.18 11.77 -5 3 13 63.31 9.37 -4 -3 13 165.52 13.34 4 3 -13 124.82 19.21 3 -3 -13 89.82 12.02 3 3 -13 63.44 11.54 -3 3 13 58.85 8.25 -3 3 13 57.53 7.00 2 -3 -13 519.46 34.88 -2 -3 13 499.89 32.67 -2 -3 13 472.74 31.27 2 3 -13 497.98 34.42 -1 -3 13 74.18 10.60 -1 -3 13 75.06 9.80 1 3 -13 93.46 13.23 0 -3 13 35.24 6.11 0 -3 13 59.48 8.82 0 -3 -13 45.15 7.73 0 3 -13 43.06 8.29 -1 -3 -13 131.92 12.43 1 -3 13 142.49 11.38 1 -3 13 102.08 10.79 -1 3 -13 131.51 14.36 6 -4 -13 8.21 6.94 6 4 -13 -5.15 10.27 -6 4 13 -4.08 6.96 -5 -4 13 464.46 27.40 5 4 -13 411.25 33.23 -5 4 13 359.19 28.31 -4 -4 13 7.99 4.88 4 -4 -13 1.28 7.66 -4 4 13 2.29 5.11 4 4 -13 5.76 9.36 -3 -4 13 151.65 13.72 -3 -4 13 163.15 16.93 3 4 -13 202.72 19.51 -3 4 13 160.32 10.50 -3 4 13 174.94 10.70 -2 -4 13 34.06 6.17 -2 -4 13 39.58 7.93 2 -4 -13 35.39 9.86 2 4 -13 40.10 8.74 -1 -4 13 133.93 13.55 -1 -4 13 150.62 12.37 1 -4 -13 98.16 13.13 1 4 -13 135.70 15.78 0 -4 13 2.90 4.80 0 -4 13 10.51 5.51 0 -4 -13 4.42 6.28 0 4 -13 13.02 6.61 -5 -5 13 52.64 9.35 5 -5 -13 39.97 8.23 5 5 -13 31.46 11.69 -5 5 13 36.22 7.56 -4 -5 13 5.04 5.01 4 -5 -13 -2.66 7.06 4 5 -13 -1.53 8.73 -4 5 13 3.09 3.72 -3 -5 13 4.41 7.37 -3 -5 13 -0.11 4.73 3 5 -13 8.55 8.29 -2 -5 13 88.63 10.95 -2 -5 13 97.83 14.01 2 -5 -13 101.31 12.46 2 5 -13 93.39 15.21 -1 -5 13 0.19 5.74 -1 -5 13 0.96 4.99 1 5 -13 12.67 7.30 3 -6 -13 3.44 7.73 -3 -6 13 8.57 5.60 -6 0 14 272.23 20.91 5 0 -14 -9.04 9.84 -5 0 14 3.79 6.02 -4 0 14 345.15 24.26 -3 0 14 -3.31 4.84 -3 0 14 7.12 5.53 2 0 -14 6.82 8.44 -2 0 14 16.57 5.59 -2 0 14 15.23 4.42 -1 0 14 -1.08 2.87 1 0 -14 4.54 7.14 0 0 -14 79.00 12.94 -6 -1 14 121.01 13.86 -6 1 14 124.89 14.58 -5 -1 14 15.24 6.25 5 -1 -14 -7.66 9.56 5 1 -14 -2.06 9.98 -5 1 14 9.39 6.18 -4 -1 14 306.62 20.90 -4 1 14 252.99 20.80 -3 -1 14 236.50 18.06 3 -1 -14 187.33 22.68 3 1 -14 197.23 22.60 -3 1 14 229.13 16.34 -3 1 14 236.89 17.47 -2 -1 14 127.26 11.63 2 -1 -14 125.52 17.46 -2 1 14 117.75 9.46 2 1 -14 132.94 17.09 -2 1 14 93.57 10.35 -1 -1 14 98.27 9.74 1 -1 -14 98.08 14.81 -1 -1 14 107.99 11.29 1 1 -14 117.13 15.08 0 -1 -14 85.31 12.70 0 -1 14 67.21 7.06 0 1 -14 77.14 12.94 5 -2 -14 -14.98 8.44 -5 -2 14 7.56 5.58 -5 2 14 9.16 6.78 -4 2 14 77.50 11.69 4 2 -14 101.42 15.06 -3 -2 14 -9.07 5.68 -3 2 14 -3.16 3.46 -2 -2 14 192.85 16.06 2 -2 -14 165.09 20.37 2 2 -14 221.98 20.58 -1 -2 14 13.66 5.26 1 -2 -14 -0.84 7.45 -1 -2 14 1.51 4.53 1 2 -14 9.86 7.12 5 -3 -14 74.91 10.95 -5 3 14 48.39 8.85 4 -3 -14 8.72 9.14 -4 3 14 10.14 5.67 4 3 -14 3.48 10.49 -3 -3 14 197.75 14.42 3 -3 -14 166.97 20.56 -3 -3 14 158.53 16.52 -3 3 14 165.65 11.73 -3 3 14 157.43 11.06 3 3 -14 134.18 20.22 -2 -3 14 4.46 6.00 2 3 -14 17.63 8.36 -1 -3 14 32.05 6.53 1 -3 -14 16.98 8.61 1 3 -14 42.14 9.16 3 -4 -14 14.13 10.16 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 63205 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_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 N1 N 0.1045(5) 0.7829(3) 0.6301(3) 0.0071(7) Uani 1 1 d . . . . . H1A H -0.007452 0.784311 0.584927 0.008 Uiso 1 1 calc R U . . . H1B H 0.109479 0.786721 0.711161 0.008 Uiso 1 1 calc R U . . . C2 C 0.1878(5) 0.9085(4) 0.5998(4) 0.0075(8) Uani 1 1 d . . . . . H2A H 0.156377 0.987724 0.642571 0.009 Uiso 1 1 calc R U . . . H2B H 0.143915 0.925545 0.509884 0.009 Uiso 1 1 calc R U . . . C3 C 0.3820(6) 0.8970(5) 0.6374(4) 0.0107(8) Uani 1 1 d . . . . . H3A H 0.431421 0.989134 0.659540 0.013 Uiso 1 1 calc R U . . . H3B H 0.420574 0.839212 0.712199 0.013 Uiso 1 1 calc R U . . . C4 C 0.4512(6) 0.8379(4) 0.5393(4) 0.0102(8) Uani 1 1 d . . . . . H4A H 0.401411 0.888648 0.461345 0.012 Uiso 1 1 calc R U . . . H4B H 0.575964 0.852081 0.564569 0.012 Uiso 1 1 calc R U . . . N5 N 0.4152(5) 0.6885(4) 0.5152(3) 0.0099(7) Uani 1 1 d . . . . . H5A H 0.480561 0.640879 0.581327 0.012 Uiso 1 1 calc R U . . . H5B H 0.448761 0.664206 0.448733 0.012 Uiso 1 1 calc R U . . . C6 C 0.2332(6) 0.6454(4) 0.4915(4) 0.0100(8) Uani 1 1 d . . . . . H6A H 0.218578 0.551455 0.457566 0.012 Uiso 1 1 calc R U . . . H6B H 0.158496 0.706668 0.428930 0.012 Uiso 1 1 calc R U . . . C7 C 0.1793(6) 0.6491(4) 0.6073(4) 0.0094(8) Uani 1 1 d . . . . . H7A H 0.094201 0.576131 0.602172 0.011 Uiso 1 1 calc R U . . . H7B H 0.279617 0.628540 0.678931 0.011 Uiso 1 1 calc R U . . . Cl1 Cl 0.26637(9) 0.78023(7) 0.92032(6) 0.0174(2) Uani 0.5 1 d . . P . . Br1 Br 0.26637(9) 0.78023(7) 0.92032(6) 0.0174(2) Uani 0.5 1 d . . P . . Br2 Br 0.63772(6) 0.51025(5) 0.74851(4) 0.0191(2) Uani 1 1 d . . . . . 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 N1 0.0074(16) 0.0070(16) 0.0089(16) -0.0015(12) 0.0056(13) -0.0004(13) C2 0.0115(19) 0.0044(17) 0.0098(19) -0.0004(14) 0.0080(16) 0.0021(15) C3 0.010(2) 0.0090(19) 0.013(2) -0.0020(15) 0.0025(17) -0.0010(15) C4 0.0093(19) 0.011(2) 0.013(2) 0.0018(16) 0.0074(16) 0.0005(15) N5 0.0139(18) 0.0092(17) 0.0099(17) 0.0020(13) 0.0084(14) 0.0067(14) C6 0.013(2) 0.0079(19) 0.010(2) -0.0023(15) 0.0050(16) 0.0012(15) C7 0.014(2) 0.0037(17) 0.013(2) 0.0008(15) 0.0083(16) 0.0001(15) Cl1 0.0175(4) 0.0194(4) 0.0151(4) 0.0027(2) 0.0044(3) 0.0013(2) Br1 0.0175(4) 0.0194(4) 0.0151(4) 0.0027(2) 0.0044(3) 0.0013(2) Br2 0.0191(3) 0.0249(3) 0.0129(3) 0.00171(17) 0.0042(2) 0.00448(18) 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' Cl Cl 0.1484 0.1585 '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' 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 C2 N1 C7 115.9(3) . . ? C2 N1 H1A 108.3 . . ? C7 N1 H1A 108.3 . . ? C2 N1 H1B 108.3 . . ? C7 N1 H1B 108.3 . . ? H1A N1 H1B 107.4 . . ? N1 C2 C3 112.9(3) . . ? N1 C2 H2A 109.0 . . ? C3 C2 H2A 109.0 . . ? N1 C2 H2B 109.0 . . ? C3 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C4 C3 C2 114.6(4) . . ? C4 C3 H3A 108.6 . . ? C2 C3 H3A 108.6 . . ? C4 C3 H3B 108.6 . . ? C2 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? N5 C4 C3 114.2(4) . . ? N5 C4 H4A 108.7 . . ? C3 C4 H4A 108.7 . . ? N5 C4 H4B 108.7 . . ? C3 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C4 N5 C6 116.0(3) . . ? C4 N5 H5A 108.3 . . ? C6 N5 H5A 108.3 . . ? C4 N5 H5B 108.3 . . ? C6 N5 H5B 108.3 . . ? H5A N5 H5B 107.4 . . ? N5 C6 C7 112.1(3) . . ? N5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? N5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N1 C7 C6 114.5(3) . . ? N1 C7 H7A 108.6 . . ? C6 C7 H7A 108.6 . . ? N1 C7 H7B 108.6 . . ? C6 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? 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 N1 C2 1.497(5) . ? N1 C7 1.503(5) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? C2 C3 1.530(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.511(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N5 1.500(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N5 C6 1.502(6) . ? N5 H5A 0.9100 . ? N5 H5B 0.9100 . ? C6 C7 1.510(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1A Cl1 0.91 2.29 3.133(4) 153.0 4_575 yes N1 H1B Cl1 0.91 2.34 3.162(4) 150.4 . yes N1 H1B Br2 0.91 3.11 3.534(4) 110.2 2_556 yes C2 H2A Br1 0.99 3.06 3.673(4) 121.0 2_556 yes C2 H2A Br2 0.99 3.04 3.731(4) 127.9 2_556 yes C2 H2B Br2 0.99 3.02 3.967(4) 160.5 4_575 yes C3 H3B Br1 0.99 3.06 3.793(5) 132.2 . yes C4 H4A Br2 0.99 2.89 3.827(4) 157.4 4_575 yes C4 H4B Cl1 0.99 2.89 3.465(4) 117.7 4_675 yes C4 H4B Br2 0.99 3.07 3.899(4) 141.7 2_656 yes N5 H5A Br2 0.91 2.33 3.241(4) 177.1 . yes N5 H5B Cl1 0.91 2.78 3.390(4) 125.1 4_675 yes N5 H5B Br2 0.91 2.74 3.487(4) 140.7 3_666 yes C6 H6A Cl1 0.99 2.98 3.712(4) 131.5 2_546 yes C6 H6A Br2 0.99 2.99 3.553(4) 117.6 3_666 yes C7 H7B Br2 0.99 3.04 3.876(4) 142.6 . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N1 C2 C3 -40.2(5) . . . . ? N1 C2 C3 C4 89.5(4) . . . . ? C2 C3 C4 N5 -70.1(5) . . . . ? C3 C4 N5 C6 50.9(5) . . . . ? C4 N5 C6 C7 -72.2(5) . . . . ? C2 N1 C7 C6 -39.1(5) . . . . ? N5 C6 C7 N1 90.5(4) . . . . ?