#------------------------------------------------------------------------------ #$Date: 2021-11-03 01:38:56 +0200 (Wed, 03 Nov 2021) $ #$Revision: 270216 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/38/7243821.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_7243821 loop_ _publ_author_name 'Milasinovic, Valentina' 'Molcanov, Kresimir' _publ_section_title ; Novel co-crystals with \p-hole interactions between iodide anions and quinoid rings involving charge transfer ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D1CE01156A _journal_year 2021 _chemical_formula_moiety 'C6 Br4 O2, 2(C6 H9 N2), 2(I)' _chemical_formula_sum 'C18 H18 Br4 I2 N4 O2' _chemical_formula_weight 895.76 _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2019-05-29T11:16:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2021-08-26 deposited with the CCDC. 2021-10-28 downloaded from the CCDC. ; _cell_angle_alpha 80.126(4) _cell_angle_beta 77.986(5) _cell_angle_gamma 76.607(5) _cell_formula_units_Z 2 _cell_length_a 7.0570(4) _cell_length_b 12.6851(6) _cell_length_c 14.8883(9) _cell_measurement_reflns_used 6376 _cell_measurement_temperature 99(2) _cell_measurement_theta_max 75.3170 _cell_measurement_theta_min 3.6010 _cell_volume 1257.45(12) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 99(2) _diffrn_detector_area_resol_mean 10.4323 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Xcalibur, Ruby, Nova' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_Laue_measured_fraction_full 1 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 11628 _diffrn_reflns_point_group_measured_fraction_full 1 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.311 _diffrn_reflns_theta_min 3.06 _exptl_absorpt_coefficient_mu 27.282 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.32695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.366 _exptl_crystal_description prism _exptl_crystal_F_000 832.0 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.635 _refine_diff_density_min -3.271 _refine_diff_density_rms 0.326 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 273 _refine_ls_number_reflns 5191 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.928 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0507 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1267P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1452 _reflns_number_gt 4916 _reflns_number_total 5191 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL br4q.4ampy_100k_a.res in P-1 shelx.res created by SHELXL-2018/3 at 11:15:24 on 29-May-2019 CELL 1.54184 7.0570 12.6851 14.8883 80.126 77.986 76.607 ZERR 2.00 0.0004 0.0006 0.0009 0.004 0.005 0.005 LATT 1 SFAC C H N O I BR UNIT 55 50 5 5 0 1 MERG 2 OMIT 5 -2 1 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 L.S. 20 WGHT 0.126700 FVAR 2.97862 I1 5 0.365397 0.179222 0.793043 11.00000 0.02609 0.01421 = 0.02288 -0.00243 -0.00381 -0.00466 I2 5 1.007660 0.681195 0.678308 11.00000 0.02662 0.01449 = 0.01712 -0.00586 -0.00280 -0.00182 MOLE 1 BR1 6 0.529338 0.561803 0.597612 11.00000 0.02246 0.02061 = 0.02789 -0.00964 0.00068 -0.00430 BR2 6 0.790046 0.302589 0.626245 11.00000 0.03359 0.01576 = 0.02379 -0.00481 0.00039 -0.00984 O1 4 0.786019 0.699869 0.464724 11.00000 0.02770 0.01605 = 0.03027 -0.00438 -0.00869 -0.00186 C1 1 0.884031 0.610462 0.483744 11.00000 0.02423 0.01543 = 0.01720 -0.00775 -0.00192 -0.00310 C2 1 0.796598 0.520295 0.543182 11.00000 0.02034 0.01386 = 0.02120 -0.00890 -0.00120 -0.00320 C3 1 0.901080 0.418293 0.555522 11.00000 0.02497 0.01338 = 0.01760 -0.00480 0.00072 -0.00323 MOLE 2 BR3 6 0.794343 0.839246 0.854182 11.00000 0.02241 0.01155 = 0.01874 -0.00538 0.00119 -0.00135 BR4 6 0.917734 1.073354 0.889118 11.00000 0.02008 0.01426 = 0.02117 -0.00414 0.00188 -0.00514 O2 4 0.397795 0.823621 0.964726 11.00000 0.02776 0.01839 = 0.03255 -0.01065 -0.00091 -0.00871 C4 1 0.446723 0.903421 0.983235 11.00000 0.02882 0.00685 = 0.01734 -0.00131 -0.00248 -0.00531 C5 1 0.638750 0.933060 0.938305 11.00000 0.02171 0.00744 = 0.01392 -0.00641 -0.00197 0.00232 C6 1 0.687692 1.025308 0.950589 11.00000 0.02043 0.01361 = 0.01962 -0.00015 -0.00316 -0.00436 MOLE 3 N1 3 0.693737 0.078162 0.363665 11.00000 0.02443 0.01864 = 0.02098 -0.00431 -0.00145 -0.00633 N2 3 0.738823 -0.017806 0.638249 11.00000 0.02692 0.02121 = 0.01956 0.00082 -0.00175 -0.00769 AFIX 93 H2B 2 0.807247 -0.080947 0.655042 11.00000 -1.20000 H2A 2 0.678296 0.024849 0.678925 11.00000 -1.20000 AFIX 0 C7 1 0.804751 -0.021040 0.388752 11.00000 0.02467 0.01716 = 0.02874 -0.00783 0.00061 -0.00736 AFIX 43 H7 2 0.867698 -0.066745 0.344123 11.00000 -1.20000 AFIX 0 C8 1 0.824703 -0.054339 0.479600 11.00000 0.02342 0.01462 = 0.02794 -0.00152 -0.00420 -0.00265 AFIX 43 H8 2 0.902617 -0.121928 0.496341 11.00000 -1.20000 AFIX 0 C9 1 0.726381 0.014469 0.547705 11.00000 0.01933 0.02006 = 0.02828 -0.00107 -0.00349 -0.00818 C10 1 0.610529 0.116636 0.518980 11.00000 0.02399 0.01556 = 0.02606 -0.00442 -0.00222 -0.00472 AFIX 43 H10 2 0.543989 0.164203 0.561688 11.00000 -1.20000 AFIX 0 C11 1 0.598116 0.144195 0.427397 11.00000 0.02429 0.01425 = 0.02785 -0.00430 -0.00094 -0.00289 AFIX 43 H11 2 0.520701 0.211066 0.408464 11.00000 -1.20000 AFIX 0 C12 1 0.678012 0.115056 0.264936 11.00000 0.03156 0.02387 = 0.02190 -0.00251 0.00007 -0.00980 AFIX 137 H12A 2 0.558164 0.168633 0.260924 11.00000 -1.50000 H12C 2 0.676176 0.053702 0.235521 11.00000 -1.50000 H12B 2 0.789517 0.146714 0.234460 11.00000 -1.50000 AFIX 0 MOLE 4 N3 3 0.211316 0.561316 1.085763 11.00000 0.02328 0.01679 = 0.02105 -0.00122 -0.00503 -0.00629 N4 3 0.274618 0.463973 0.829543 11.00000 0.03324 0.01669 = 0.02299 -0.00360 -0.00499 -0.00168 AFIX 93 H4B 2 0.243424 0.511653 0.783690 11.00000 -1.20000 H4A 2 0.316767 0.396297 0.821886 11.00000 -1.20000 AFIX 0 C13 1 0.279921 0.454569 1.073962 11.00000 0.01714 0.01735 = 0.02922 0.00173 -0.00569 -0.00483 AFIX 43 H13 2 0.310740 0.403983 1.124588 11.00000 -1.20000 AFIX 0 C14 1 0.304905 0.419454 0.989853 11.00000 0.02041 0.01144 = 0.02573 -0.00285 -0.00042 -0.00512 AFIX 43 H14 2 0.353043 0.345849 0.983719 11.00000 -1.20000 AFIX 0 C15 1 0.257762 0.494739 0.911879 11.00000 0.01794 0.01590 = 0.02595 -0.00250 -0.00386 -0.00385 C16 1 0.188826 0.605543 0.926962 11.00000 0.02538 0.01352 = 0.03016 0.00430 -0.00857 -0.00627 AFIX 43 H16 2 0.158050 0.658057 0.877481 11.00000 -1.20000 AFIX 0 C17 1 0.166691 0.636792 1.011749 11.00000 0.01981 0.01264 = 0.02969 -0.00505 -0.00734 -0.00157 AFIX 43 H17 2 0.120844 0.710054 1.019707 11.00000 -1.20000 AFIX 0 C18 1 0.193436 0.598048 1.176033 11.00000 0.03482 0.02640 = 0.02823 -0.01030 -0.00505 -0.00714 AFIX 137 H18A 2 0.215721 0.535636 1.222023 11.00000 -1.50000 H18B 2 0.063105 0.640739 1.192809 11.00000 -1.50000 H18C 2 0.289792 0.641782 1.172281 11.00000 -1.50000 AFIX 0 HKLF 4 REM br4q.4ampy_100k_a.res in P-1 REM wR2 = 0.1452, GooF = S = 0.928, Restrained GooF = 0.928 for all data REM R1 = 0.0507 for 4916 Fo > 4sig(Fo) and 0.0526 for all 5191 data REM 273 parameters refined using 0 restraints END WGHT 0.0978 0.0000 REM Highest difference peak 1.635, deepest hole -3.271, 1-sigma level 0.326 Q1 1 0.3146 0.1718 0.8515 11.00000 0.05 1.63 Q2 1 1.0728 0.5986 0.6376 11.00000 0.05 1.62 Q3 1 1.0419 0.7098 0.5984 11.00000 0.05 1.44 Q4 1 0.4417 0.0990 0.7532 11.00000 0.05 1.44 Q5 1 1.1822 0.6605 0.6412 11.00000 0.05 1.40 Q6 1 0.8113 0.7166 0.7017 11.00000 0.05 1.35 Q7 1 0.9326 0.6667 0.7434 11.00000 0.05 1.34 Q8 1 0.9357 0.7523 0.7219 11.00000 0.05 1.33 Q9 1 1.1411 0.6775 0.6258 11.00000 0.05 1.32 Q10 1 0.5660 0.1468 0.7773 11.00000 0.05 1.24 Q11 1 0.8384 0.7000 0.7199 11.00000 0.05 1.20 Q12 1 0.4859 0.1746 0.7423 11.00000 0.05 1.17 Q13 1 0.3795 0.1951 0.7057 11.00000 0.05 1.16 Q14 1 0.5074 0.5214 0.6752 11.00000 0.05 1.15 Q15 1 0.8962 1.0567 0.9560 11.00000 0.05 1.15 Q16 1 0.7208 0.8988 0.8960 11.00000 0.05 1.12 Q17 1 0.3106 0.2795 0.8268 11.00000 0.05 1.12 Q18 1 0.4621 0.6395 0.6408 11.00000 0.05 1.10 Q19 1 0.1758 0.2021 0.8223 11.00000 0.05 1.10 Q20 1 0.9987 1.0188 0.8555 11.00000 0.05 1.09 ; _cod_data_source_file d1ce01156a3.cif _cod_data_source_block br4q _cod_original_cell_volume 1257.45(13) _cod_database_code 7243821 _iucr_refine_reflections_details ; 0 0 1 3206.02 335.656 2 0 0 2 3558.38 487.050 2 0 0 3 1070.47 360.548 2 0 0 4 186456. 7543.95 2 0 0 5 20507.7 1966.65 2 0 0 6 25216.5 2425.93 2 0 0 7 21882.8 2445.10 2 0 0 8 735.572 497.815 2 0 0 9 25416.7 3123.53 2 0 0 10 36805.2 4090.53 2 0 0 11 27457.7 1967.30 17 0 0 11 25391.8 3541.74 2 0 0 12 14506.4 1283.95 23 0 0 12 13478.6 2698.45 2 0 0 12 14649.9 1431.21 17 0 0 13 7589.02 923.421 23 0 0 13 8344.51 1091.11 17 0 0 14 4110.29 765.931 17 0 0 -14 2815.79 693.438 24 0 0 -15 16450.2 1554.24 24 0 0 15 17599.0 1523.19 17 0 0 16 446.086 203.414 10 0 0 -16 167.650 191.704 24 0 0 17 40615.3 2007.46 10 0 0 18 88.5709 79.5966 10 0 -1 18 308.344 103.590 10 0 -1 17 137.862 115.580 10 0 -1 16 5376.23 674.951 10 0 -1 15 6511.63 784.582 10 0 -1 15 5015.37 689.995 23 0 -1 15 4643.33 716.940 17 0 -1 14 10813.5 1177.57 17 0 -1 14 10937.9 1107.73 23 0 -1 13 6070.24 881.242 17 0 -1 13 6056.50 840.428 23 0 -1 12 192663. 7565.69 17 0 -1 12 190304. 7371.72 23 0 -1 12 189251. 11806.3 2 0 -1 11 97199.9 4244.36 23 0 -1 11 91569.6 7350.74 2 0 -1 11 95659.9 4390.57 17 0 -1 10 24518.3 3340.72 2 0 -1 9 12711.3 2212.23 2 0 -1 8 198853. 9971.92 2 0 -1 7 18807.1 2299.62 2 0 -1 6 109259. 5908.44 2 0 -1 5 73090.3 4205.86 2 0 -1 4 199967. 8059.02 2 0 -1 3 57985.8 3011.65 2 0 -1 2 64045.2 2978.43 2 0 -1 2 67422.9 2241.69 1 0 -1 1 77648.1 3088.32 2 0 -1 1 84837.4 3074.94 5 0 -1 0 4511.74 465.520 5 0 -1 -1 73689.8 2741.09 5 0 1 1 80511.9 2662.81 4 0 1 2 6032.28 616.312 2 0 -1 -2 5114.21 572.258 3 0 1 3 103404. 4420.10 2 0 1 4 126638. 5558.89 2 0 1 5 7351.36 1118.35 2 0 1 6 121837. 6205.34 2 0 1 7 41086.9 3419.51 2 0 1 8 13342.2 2006.06 2 0 1 9 15384.5 2382.26 2 0 1 10 77736.6 6139.89 2 0 1 11 131686. 5643.89 17 0 1 11 123238. 8571.24 2 0 1 12 2121.23 404.681 14 0 1 12 2195.67 552.279 17 0 1 12 1596.34 967.730 2 0 1 13 132505. 5913.54 17 0 -1 -14 9820.65 1303.77 24 0 1 14 11958.3 1322.07 17 0 -1 -15 332.357 403.785 24 0 1 15 942.711 386.134 17 0 1 16 11829.9 1164.55 17 0 -1 -16 10410.4 1161.00 24 0 1 17 176.850 137.673 10 0 -1 -17 350.953 192.563 24 0 1 18 168.650 83.1788 10 0 -2 17 74795.7 2935.06 10 0 -2 17 67555.5 2838.09 27 0 -2 16 12535.1 1017.79 10 0 -2 15 3365.36 552.801 23 0 -2 15 4026.08 597.695 10 0 -2 14 14027.5 1213.23 10 0 -2 14 12337.9 1198.35 17 0 -2 14 12267.7 1201.88 23 0 -2 13 42977.8 2540.25 17 0 -2 13 41693.5 2499.96 23 0 -2 12 19879.4 1593.22 23 0 -2 12 19554.8 3371.52 2 0 -2 12 20684.8 1635.53 17 0 -2 11 9216.60 1003.46 23 0 -2 11 8566.41 2112.42 2 0 -2 11 9131.00 1012.79 17 0 -2 10 56531.3 5295.57 2 0 -2 9 101995. 6981.76 2 0 -2 8 188604. 9751.87 2 0 -2 7 9763.23 1665.89 2 0 -2 6 123293. 6471.99 2 0 -2 5 21694.1 2094.60 2 0 -2 4 34209.6 2467.83 2 0 -2 3 1654.03 449.647 2 0 -2 2 274973. 9467.09 5 0 -2 2 262603. 9518.32 2 0 -2 1 23235.4 1393.86 2 0 -2 1 26407.2 1578.53 5 0 -2 0 6298.41 762.206 5 0 -2 0 3051.03 395.171 2 0 -2 -1 81800.4 3622.52 5 0 2 1 100250. 3321.27 4 0 2 2 120975. 4432.50 4 0 -2 -2 124761. 4641.01 5 0 2 3 38141.2 2175.43 2 0 -2 -3 38878.9 2336.27 3 0 2 4 737.265 311.893 2 0 -2 -4 478.873 237.386 3 0 2 5 1893.11 590.157 2 0 2 6 86389.0 4912.59 2 0 2 7 11630.1 1690.36 2 0 2 8 38354.9 3525.52 2 0 2 9 252422. 12061.8 2 0 2 10 86910.7 6432.97 2 0 2 11 89005.3 6960.89 2 0 2 11 101138. 4079.91 14 0 2 11 87895.3 4435.07 17 0 2 12 2373.63 611.042 17 0 2 12 2252.36 449.722 14 0 2 12 2403.66 1094.06 2 0 2 13 3964.58 790.760 17 0 2 13 4432.21 626.225 14 0 -2 -14 70979.9 4096.50 24 0 2 14 78231.8 3358.12 14 0 2 14 71552.2 3926.61 17 0 -2 -15 21224.3 1930.79 24 0 2 15 24843.1 1455.40 14 0 2 15 22604.9 1876.72 17 0 -2 -16 997.339 433.697 24 0 2 16 460.670 260.631 17 0 -2 -17 11357.8 1072.40 24 0 2 18 620.100 167.849 10 0 -3 17 3324.46 399.968 10 0 -3 17 2578.08 332.526 27 0 -3 16 74091.6 3176.09 27 0 -3 16 74067.2 3145.91 10 0 -3 15 184.173 187.372 10 0 -3 15 405.737 203.671 23 0 -3 14 60437.0 3169.28 23 0 -3 14 67575.3 3144.49 10 0 -3 13 2009.50 488.714 23 0 -3 13 1906.77 450.001 10 0 -3 13 1514.74 377.854 28 0 -3 12 1939.39 440.897 17 0 -3 12 3144.93 547.140 10 0 -3 12 1802.35 485.408 23 0 -3 11 1371.44 368.487 17 0 -3 11 765.561 301.647 16 0 -3 11 1655.43 909.122 2 0 -3 11 792.439 267.036 23 0 -3 10 29686.6 1915.28 23 0 -3 10 31538.0 3915.28 2 0 -3 9 2351.17 972.607 2 0 -3 8 28572.2 3211.92 2 0 -3 7 31026.1 3123.67 2 0 -3 6 285063. 11980.2 2 0 -3 5 100241. 5381.24 2 0 -3 4 104208. 5179.18 2 0 -3 3 513069. 17522.5 5 0 -3 3 509692. 17669.2 2 0 -3 2 44593.9 2549.08 2 0 -3 2 46290.3 2655.31 5 0 -3 1 120901. 4891.05 2 0 -3 1 127468. 5363.07 5 0 -3 0 5250.00 864.543 5 0 -3 0 4729.50 574.967 2 0 3 1 226361. 7652.33 4 0 -3 -1 203512. 8268.97 3 0 -3 -1 201291. 8497.82 5 0 3 2 183907. 6718.27 4 0 -3 -2 187713. 7341.07 5 0 -3 -2 174839. 7352.44 3 0 3 3 300937. 11110.3 2 0 -3 -3 280625. 11710.1 3 0 -3 -4 117.092 230.159 5 0 3 4 44.0102 116.759 2 0 -3 -4 34.2990 186.065 3 0 3 5 112889. 5404.08 2 0 3 6 25539.7 2328.61 2 0 3 7 2505.90 757.929 2 0 3 8 22330.8 2556.14 2 0 3 9 3428.50 1049.38 2 0 3 10 8521.22 1790.47 2 0 3 11 6349.53 1608.10 2 0 -3 -11 4239.86 927.145 8 0 3 11 5277.60 709.918 14 0 3 11 3727.05 707.779 17 0 3 12 42178.6 2330.44 14 0 3 12 37109.1 2604.21 17 0 -3 -12 39129.1 3056.92 8 0 3 13 31778.2 2360.15 17 0 3 13 33290.9 2009.67 14 0 -3 -13 30501.5 2643.94 8 0 3 14 74477.4 4074.34 17 0 3 14 80160.3 3572.20 14 0 -3 -14 82638.2 4343.18 24 0 3 15 40109.0 2662.56 17 0 -3 -15 46496.6 2923.17 24 0 3 15 43746.7 2224.52 14 0 3 16 13327.1 961.106 14 0 3 16 13736.2 1303.32 17 0 -3 -16 16313.9 1471.16 24 0 -3 -17 198.347 269.729 24 0 3 18 2542.97 325.299 10 0 -4 16 23518.6 1354.01 27 0 -4 16 22635.7 1327.17 10 0 -4 15 2205.57 425.681 27 0 -4 15 1807.08 373.287 10 0 -4 14 8568.18 948.719 23 0 -4 14 8950.46 923.054 10 0 -4 13 536.880 244.314 10 0 -4 13 987.916 345.006 23 0 -4 12 995.891 319.172 10 0 -4 12 1289.25 329.959 28 0 -4 12 623.452 262.859 16 0 -4 12 1166.41 374.270 23 0 -4 11 1776.15 442.861 23 0 -4 11 2309.79 1121.45 2 0 -4 11 1615.20 377.864 10 0 -4 11 1848.90 412.422 28 0 -4 11 1402.67 397.343 16 0 -4 10 29337.9 1987.67 16 0 -4 10 31476.3 1852.23 10 0 -4 10 31028.9 3904.68 2 0 -4 10 29602.8 1832.73 28 0 -4 10 30756.8 1993.13 23 0 -4 9 152855. 9278.61 2 0 -4 9 159447. 6140.72 23 0 -4 9 156102. 5889.96 10 0 -4 8 115538. 7307.73 2 0 -4 7 152849. 8240.90 2 0 -4 6 1967.38 692.879 2 0 -4 5 8568.17 1383.63 2 0 -4 4 6769.83 1086.55 5 0 -4 4 8008.54 1218.79 2 0 -4 3 292969. 10222.1 3 0 -4 3 280407. 11112.8 5 0 -4 3 301450. 11143.8 2 0 -4 2 1475.28 419.414 3 0 -4 2 1691.34 462.786 2 0 -4 2 2445.50 623.293 5 0 -4 1 6129.03 815.038 2 0 -4 1 6162.66 865.565 3 0 -4 1 5116.67 910.558 5 0 4 0 75842.9 3735.43 4 0 -4 0 72874.7 4144.14 5 0 -4 0 70215.2 3851.36 3 0 -4 0 76736.4 3437.21 2 0 -4 -1 97847.2 4771.01 3 0 -4 -1 94462.1 4979.10 5 0 4 1 93420.8 4104.52 4 0 -4 -2 5392.85 981.050 5 0 -4 -2 6557.86 1057.76 3 0 4 2 4620.97 673.982 4 0 -4 -3 598627. 19043.7 3 0 4 3 477900. 17345.8 2 0 -4 -3 584180. 18851.3 5 0 4 3 518392. 17657.4 4 0 -4 -4 27447.9 2258.09 5 0 -4 -4 24325.9 2285.11 3 0 4 4 22754.9 1719.15 2 0 -4 -5 1012.41 419.757 3 0 4 5 466.130 266.121 2 0 -4 -5-95.9293 197.192 5 0 4 6 75126.5 4253.83 2 0 -4 -6 74599.3 4378.39 5 0 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10437.7 1053.25 9 1 -6 8 9041.68 998.736 16 1 -6 8 8478.07 925.426 23 1 -6 8 8474.99 1694.48 2 1 -6 8 10195.7 1074.58 12 1 -6 8 8636.11 976.531 18 1 -6 8 9067.58 878.896 10 1 -6 9 128898. 5205.96 12 1 -6 9 128607. 7846.44 2 1 -6 9 115964. 4791.86 10 1 -6 9 120147. 5017.30 23 1 -6 9 117228. 5107.67 16 1 -6 9 117710. 5066.33 18 1 -6 10 838.447 277.651 10 1 -6 10 398.253 221.802 16 1 -6 10 394.157 236.473 23 1 -6 10 706.251 312.933 12 1 -6 11 4758.11 711.051 12 1 -6 11 4667.38 723.554 23 1 -6 11 5274.70 740.095 27 1 -6 11 5046.08 664.960 10 1 -6 11 4503.50 727.727 16 1 -6 12 32476.8 1926.13 12 1 -6 12 33203.4 2048.28 16 1 -6 12 31293.8 2006.23 23 1 -6 12 29522.7 1810.58 10 1 -6 12 31343.1 1964.41 27 1 -6 13 7703.96 793.374 10 1 -6 13 8922.66 926.079 23 1 -6 13 8541.22 884.705 27 1 -6 13 8711.08 888.319 16 1 -6 14 18232.4 1189.66 10 1 -6 14 20250.3 1327.42 27 1 -6 15 4297.39 408.001 15 1 -6 15 4620.04 458.704 10 -1 5 17 8072.38 541.973 14 1 -5 -16 6389.00 739.391 29 -1 5 16 7408.37 658.751 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549.108 17 7 5 12 4185.71 846.239 7 -7 -5 -12 4038.35 660.590 11 7 5 13 602.061 173.086 17 -7 -5 -13 730.227 282.023 11 -7 -5 -14 2044.09 355.379 11 -7 -6 7 174.881 111.126 6 -7 -6 6 7001.61 632.172 6 -7 -6 5 5237.23 575.902 6 -7 -6 4 20859.9 1391.70 25 -7 -6 4 28155.7 1531.37 6 -7 -6 3 6435.04 749.318 25 -7 -6 3 6687.00 714.727 6 -7 -6 2 108965. 4668.65 25 -7 -6 2 116101. 4529.80 6 -7 -6 1 347.196 230.850 25 -7 -6 1 979.985 300.135 6 -7 -6 0 1022.68 350.061 25 -7 -6 0 1067.45 294.578 6 -7 -6 -1 7840.92 982.656 25 -7 -6 -2 33761.7 2246.14 25 -7 -6 -3 26459.5 1971.21 25 -7 -6 -4 3799.49 702.667 25 -7 -6 -5 31921.5 2251.09 25 7 6 6 4358.30 827.799 17 -7 -6 -6 3731.20 705.827 25 7 6 7 6822.83 1030.65 17 7 6 8 907.464 320.199 17 7 6 8 100.131 231.858 7 7 6 9 662.678 309.301 17 7 6 9 200.328 247.678 7 7 6 10 515.314 288.953 17 7 6 10 830.957 395.242 7 7 6 11 19308.6 1407.86 17 7 6 11 15855.6 1688.90 7 7 6 12 524.070 206.921 17 -7 -6 -12 351.680 206.335 11 7 6 13 6372.10 587.932 17 -7 -6 -13 5632.86 649.284 11 -7 -6 -14 9227.78 715.588 11 -7 -7 6 9752.10 696.574 6 -7 -7 6 8703.28 703.071 21 -7 -7 5 19456.0 1168.05 6 -7 -7 4 2781.56 416.077 6 -7 -7 3 247.290 165.273 25 -7 -7 3 399.896 170.895 6 -7 -7 2 18014.0 1342.36 25 -7 -7 2 21047.5 1349.65 6 -7 -7 1 72788.9 3453.04 25 -7 -7 1 77139.9 3296.48 6 -7 -7 0 649.060 279.311 25 -7 -7 0 1114.65 300.012 6 -7 -7 -1 24729.1 1793.40 25 -7 -7 -2 3068.49 621.629 25 -7 -7 -3 543.461 287.917 25 -7 -7 -4 2002.74 525.071 25 -7 -7 -4 2060.50 487.170 21 -7 -7 -5 3057.16 640.816 25 7 7 6 20001.6 1836.98 17 7 7 7 5627.69 916.506 17 7 7 8 279.041 283.223 17 7 7 9 122196. 5317.57 17 7 7 10 481.879 275.108 17 7 7 11 19690.3 1384.21 17 -7 -7 -11 14269.6 1168.57 11 7 7 12 1935.35 375.178 17 -7 -7 -12 1287.24 314.891 11 7 7 13 11234.7 789.207 17 -7 -7 -13 8386.98 715.877 11 -7 -8 5 18221.2 1030.53 6 -7 -8 5 18378.3 1112.41 21 -7 -8 4 929.613 273.411 21 -7 -8 4 800.235 226.065 6 -7 -8 3 39309.1 1967.21 6 -7 -8 3 42501.5 2209.11 21 -7 -8 2 878.441 255.647 25 -7 -8 2 1272.38 307.314 6 -7 -8 1 135.804 148.749 25 -7 -8 1 352.456 189.385 6 -7 -8 0 15191.2 1265.25 25 -7 -8 0 17149.4 1193.81 6 -7 -8 -1 11751.3 1142.79 25 -7 -8 -1 13745.4 1253.79 21 -7 -8 -2 591.316 282.520 25 -7 -8 -2 455.991 239.660 21 -7 -8 -3 8716.86 1026.74 25 -7 -8 -3 9646.48 1057.06 21 -7 -8 -4 9092.23 973.931 21 7 8 5 11700.8 1351.05 17 7 8 6 29077.5 2179.24 17 7 8 7 47088.1 2838.81 17 7 8 8 55421.9 3071.36 17 7 8 9 293.047 266.011 17 -7 -8 -9 101.459 150.203 8 7 8 10 26279.8 1651.98 17 -7 -8 -10 15102.4 1111.91 11 7 8 11 7393.73 771.190 17 -7 -8 -11 4407.06 516.004 11 7 8 12 77666.8 2604.18 17 -7 -8 -12 39227.6 1959.41 11 7 8 13 3191.57 379.343 17 -7 -9 4 3916.11 405.911 6 -7 -9 4 4141.12 466.722 21 -7 -9 3 591.218 233.372 21 -7 -9 3 1092.33 236.574 6 -7 -9 2 7080.01 647.350 6 -7 -9 2 7137.71 764.272 21 -7 -9 1 15982.9 1062.16 6 -7 -9 1 16053.0 1245.90 21 -7 -9 0 40660.8 1929.24 6 -7 -9 0 37217.5 2167.82 21 -7 -9 -1 111622. 4666.90 21 -7 -9 -2 251.422 202.841 21 -7 -9 -3 9354.18 971.221 21 7 9 4 1992.20 548.735 17 -7 -9 -4 2299.25 460.268 21 7 9 5 19520.0 1656.36 17 -7 -9 -5 20080.2 1359.13 21 7 9 6 2175.65 552.570 17 7 9 7 24851.9 1832.19 17 7 9 8 32647.0 2032.63 17 -7 -9 -8 27086.0 1980.42 8 7 9 9 14961.5 1244.20 17 -7 -9 -9 13127.3 1185.58 8 7 9 10 10469.4 957.717 17 7 9 11 909.925 260.365 17 7 9 12 1254.36 246.639 17 -7 -10 3 897.297 196.626 21 -7 -10 2 8170.57 707.250 21 -7 -10 1 1984.66 379.330 21 -7 -10 0 114.945 148.781 21 -7 -10 -1 23805.4 1504.18 21 -7 -10 -2 4497.74 596.943 21 7 10 3 1965.85 481.420 17 -7 -10 -3 1155.70 311.276 21 7 10 4 30036.5 1992.27 17 -7 -10 -4 33737.4 1795.06 21 7 10 5 16664.4 1381.32 17 -7 -10 -5 16131.5 1089.47 21 7 10 6 30673.9 1942.02 17 7 10 7 100.156 154.027 17 7 10 8 1171.96 325.814 17 -7 -10 -8 1159.56 352.813 8 7 10 9 471.716 219.405 17 -7 -10 -9 156.308 161.464 8 7 10 10 1547.49 318.467 17 7 10 11 497.469 170.480 17 -7 -11 1 4197.62 430.560 21 7 11 0 857.131 211.850 17 -7 -11 0 1570.53 286.444 21 7 11 1 7359.99 688.906 17 -7 -11 -1 8152.45 693.774 21 7 11 2 52465.1 2512.90 17 -7 -11 -2 60208.3 2482.04 21 7 11 3 142.668 127.345 17 -7 -11 -3 160.119 114.872 21 7 11 4 1768.04 364.797 17 -7 -11 -4 1571.97 295.797 21 7 11 5 9976.95 873.856 17 -7 -11 -5 8346.06 639.407 21 7 11 6 32840.6 1760.38 17 -7 -11 -6 30494.1 1913.41 8 7 11 7 1973.38 353.688 17 -7 -11 -7 1617.98 393.758 8 7 11 8 3176.28 421.080 17 -7 -11 -8 3008.24 476.675 8 7 11 9 38984.5 1743.70 17 -7 -11 -9 34772.7 1784.18 8 -7 -12 -2 19822.3 999.239 21 -7 -12 -3 31634.0 1392.03 21 -7 -12 -4 35498.0 1841.80 8 -7 -12 -5 11906.4 937.048 8 -7 -12 -6 2348.46 381.992 8 -7 -12 -7 3811.12 465.301 8 8 -3 0 237.968 131.516 7 8 -3 1 4911.31 571.637 7 8 -3 2-12.1473 71.5753 7 8 -3 3 265.421 156.142 7 8 -3 4 332.710 166.280 7 8 -3 5 24518.9 1425.64 7 8 -2 -1 2539.06 414.178 7 8 -2 0 5713.18 673.378 7 8 -2 1 15119.1 1193.51 7 8 -2 2 15573.9 1249.46 7 8 -2 3 10958.0 1033.43 7 8 -2 4 3327.44 555.021 7 8 -2 5 2704.53 495.940 7 8 -2 6 7815.86 839.992 7 8 -2 7 1735.82 384.690 7 -8 1 2 316.081 142.292 25 8 -1 -1 561.113 220.293 7 -8 1 1 395.670 172.184 25 8 -1 0 8324.07 865.847 7 -8 1 0 5944.68 618.002 25 8 -1 1 970.617 321.576 7 -8 1 -1 723.120 207.085 25 8 -1 2 1542.93 415.479 7 8 -1 3 2528.17 508.453 7 8 -1 4 32788.0 2119.98 7 8 -1 5-275.779 217.191 7 8 -1 6 31204.4 2021.17 7 8 -1 7 2318.05 495.071 7 8 -1 8 268.493 175.919 7 -8 0 3 7161.36 661.869 25 -8 0 2 2068.79 376.026 25 8 0 -1 19692.0 1337.13 7 -8 0 1 14576.4 1125.10 25 8 0 0 1341.31 362.115 7 -8 0 0 1549.11 345.790 25 8 0 1 2302.50 474.266 7 -8 0 -1 1435.51 355.658 25 8 0 2 14530.7 1287.81 7 -8 0 -2 9049.73 866.232 25 8 0 3 28635.6 1988.76 7 8 0 4 7524.76 978.029 7 8 0 5 5034.94 786.180 7 8 0 6 18.7606 167.946 7 8 0 7 22405.6 1745.36 7 8 0 8 5206.32 783.304 7 8 0 9 7219.49 867.806 7 -8 -1 4 14022.1 920.292 25 -8 -1 3 24.2740 87.3618 25 -8 -1 2 45018.0 2246.35 25 -8 -1 1 255.761 176.109 25 8 1 0 788.528 275.561 7 -8 -1 0 434.752 210.520 25 8 1 1 886.948 320.282 7 -8 -1 -1 483.716 222.654 25 8 1 2 31095.4 1987.19 7 -8 -1 -2 20762.8 1522.05 25 8 1 3 10063.8 1109.45 7 -8 -1 -3 6054.53 744.656 25 8 1 4 343.121 241.211 7 8 1 5 14012.3 1404.61 7 8 1 6 562.356 305.688 7 8 1 7 2085.24 540.834 7 8 1 8 11361.5 1230.93 7 8 1 9 4897.68 751.853 7 8 1 10 99.0153 143.847 7 -8 -2 4 1886.99 308.538 25 -8 -2 3 393.842 188.831 25 -8 -2 2 346.107 194.488 25 -8 -2 1 10914.3 995.021 25 -8 -2 0 6004.06 744.515 25 8 2 1 20333.6 1527.31 7 -8 -2 -1 20656.3 1492.23 25 8 2 2 1043.30 371.910 7 -8 -2 -2 1121.76 332.659 25 8 2 3 9437.55 1083.36 7 -8 -2 -3 8507.28 926.803 25 8 2 4 7348.23 958.642 7 -8 -2 -4 5253.01 710.607 25 8 2 5 2902.98 617.076 7 -8 -2 -5 2354.42 423.284 25 8 2 6 2124.82 543.997 7 8 2 7 2357.06 563.094 7 8 2 8 798.928 322.794 7 8 2 9 41573.6 2559.85 7 8 2 10 1746.42 464.081 7 8 2 11 13816.7 1185.07 7 -8 -2 -11 15417.8 1023.13 11 -8 -3 4 9483.38 723.428 25 -8 -3 3 26703.1 1518.46 25 -8 -3 2 10531.9 935.317 25 -8 -3 1 23720.4 1558.48 25 -8 -3 0 176.961 172.502 25 -8 -3 -1 10498.5 1031.59 25 8 3 2 8781.75 869.753 17 -8 -3 -2 7200.20 870.305 25 8 3 3 2914.68 575.710 7 -8 -3 -3 2534.86 502.812 25 8 3 4 236.039 192.390 7 -8 -3 -4-56.4070 151.003 25 8 3 5 3539.15 671.166 7 -8 -3 -5 2068.26 442.543 25 8 3 6 16595.0 1551.23 7 8 3 7 24779.4 1938.53 7 8 3 8 6959.64 975.232 7 8 3 9 9866.98 1140.20 7 8 3 10 7560.33 951.366 7 8 3 11 6554.27 806.930 7 -8 -3 -11 5707.30 623.831 11 -8 -4 3 3298.19 444.846 25 -8 -4 2 3402.10 504.208 25 -8 -4 1 56489.7 2721.49 25 -8 -4 0 23281.8 1582.79 25 -8 -4 -1 25590.8 1724.85 25 -8 -4 -2 1985.55 448.227 25 8 4 3 2051.19 461.064 17 -8 -4 -3 1957.79 457.564 25 8 4 4 6349.99 775.477 17 -8 -4 -4 4944.54 716.832 25 8 4 5 384.693 197.473 17 8 4 5 31.3150 156.572 7 -8 -4 -5 350.461 227.644 25 8 4 6 10159.0 914.721 17 8 4 6 7406.93 988.973 7 8 4 7 773.612 236.817 17 8 4 7 290.405 240.369 7 8 4 8 648.279 297.785 7 8 4 9 4482.43 736.690 7 8 4 10 34388.7 2189.22 7 -8 -4 -11 478.564 193.291 11 -8 -5 3 781.974 209.855 25 -8 -5 2 10193.0 858.534 25 -8 -5 1 1387.84 328.418 25 -8 -5 0 3944.53 589.243 25 -8 -5 -1 57797.2 2858.54 25 -8 -5 -2 4929.36 700.715 25 8 5 3 3736.73 644.883 17 -8 -5 -3 2882.78 554.843 25 8 5 4 9128.69 999.098 17 -8 -5 -4 7236.15 874.842 25 8 5 5 54472.5 2654.47 17 -8 -5 -5 38155.3 2330.18 25 8 5 6 40644.1 2256.69 17 8 5 7-2.84871 80.5927 17 8 5 8 26409.8 1490.22 17 8 5 8 20731.8 1668.38 7 8 5 9 3367.64 427.101 17 8 5 9 3267.92 588.705 7 -8 -5 -11 1220.18 275.206 11 -8 -6 3 9574.50 755.063 21 -8 -6 2 537.523 179.603 25 -8 -6 1 521.714 213.845 25 -8 -6 0 12365.6 1032.00 25 -8 -6 -1 5488.27 691.957 25 -8 -6 -1 5715.47 678.437 21 -8 -6 -2 28464.7 1778.22 25 -8 -6 -2 26136.1 1583.01 21 -8 -6 -3 166.282 148.452 25 8 6 4 11953.9 1147.06 17 -8 -6 -4 9161.48 972.940 25 8 6 5 3368.75 593.663 17 8 6 6 3451.42 578.775 17 8 6 7 1617.66 374.967 17 8 6 8 4990.56 616.847 17 8 6 9 15988.8 1072.78 17 8 6 10 11026.4 738.046 17 -8 -6 -10 8618.63 740.531 11 -8 -7 2 4495.15 506.839 21 -8 -7 1 1362.49 329.367 21 -8 -7 0 7337.27 730.470 25 -8 -7 0 9979.17 843.056 21 -8 -7 -1 2073.15 403.332 25 -8 -7 -1 2222.83 401.250 21 -8 -7 -2-168.026 155.472 25 -8 -7 -2 557.788 218.548 21 8 7 3 2115.51 506.007 17 8 7 4 50730.9 2711.05 17 8 7 5 540.160 223.318 17 8 7 6 26566.8 1726.32 17 8 7 7 676.771 246.975 17 8 7 8 2184.22 409.308 17 8 7 9 10075.1 813.414 17 8 7 10 934.887 202.414 17 -8 -8 1 11403.4 795.960 21 -8 -8 0 738.585 208.845 21 -8 -8 -1 2709.89 391.525 21 8 8 2 62886.1 2844.06 17 -8 -8 -2 50471.9 2307.17 21 8 8 3 94538.3 4072.94 17 8 8 4 23385.7 1587.40 17 8 8 5 1478.18 364.804 17 8 8 6 6455.73 747.236 17 8 8 7 35704.5 1931.24 17 8 8 8 6213.40 645.088 17 8 8 9 11427.7 829.781 17 8 9 1 1416.67 299.665 17 8 9 2 4744.93 581.867 17 8 9 3 4272.06 571.509 17 8 9 4 11890.5 978.767 17 8 9 5 28594.1 1638.56 17 8 9 6 414.303 186.350 17 8 9 7 13838.0 983.580 17 8 9 8 11418.5 819.679 17 8 10 4 344.078 135.009 17 8 10 5 6578.84 584.037 17 0 0 0 0.00 0.00 0 TITL Br4Q in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 7.056139 12.682215 14.895010 80.1364 78.0002 76.5601 ZERR 5.00 0.000325 0.000446 0.000644 0.0033 0.0038 0.0035 LATT 1 SFAC C H N O UNIT 55.00 50.00 5.00 5.00 TREF HKLF 4 END ; loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z loop_ _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 _atom_site_type_symbol I1 0.36540(6) 0.17922(3) 0.79304(2) 0.02103(14) Uani d 1 . . I I2 1.00766(6) 0.68119(3) 0.67831(2) 0.01949(14) Uani d 1 . . I Br1 0.52934(10) 0.56180(5) 0.59761(4) 0.02363(17) Uani d 1 . . Br Br2 0.79005(10) 0.30259(5) 0.62625(4) 0.02411(17) Uani d 1 . . Br O1 0.7860(7) 0.6999(4) 0.4647(3) 0.0244(9) Uani d 1 . . O C1 0.8840(9) 0.6105(5) 0.4837(4) 0.0187(10) Uani d 1 . . C C2 0.7966(9) 0.5203(4) 0.5432(4) 0.0181(10) Uani d 1 . . C C3 0.9011(9) 0.4183(4) 0.5555(4) 0.0191(11) Uani d 1 . . C Br3 0.79434(9) 0.83925(4) 0.85418(4) 0.01822(16) Uani d 1 . . Br Br4 0.91773(9) 1.07335(4) 0.88912(4) 0.01882(16) Uani d 1 . . Br O2 0.3978(7) 0.8236(3) 0.9647(3) 0.0253(9) Uani d 1 . . O C4 0.4467(10) 0.9034(4) 0.9832(4) 0.0177(10) Uani d 1 . . C C5 0.6387(9) 0.9331(4) 0.9383(4) 0.0148(10) Uani d 1 . . C C6 0.6877(9) 1.0253(4) 0.9506(4) 0.0180(10) Uani d 1 . . C N1 0.6937(8) 0.0782(4) 0.3637(4) 0.0212(10) Uani d 1 . . N N2 0.7388(8) -0.0178(4) 0.6382(4) 0.0229(10) Uani d 1 . . N H2B 0.807247 -0.080947 0.655042 0.027 Uiso calc 1 . . H H2A 0.678296 0.024849 0.678925 0.027 Uiso calc 1 . . H C7 0.8048(10) -0.0210(5) 0.3888(5) 0.0232(12) Uani d 1 . . C H7 0.867698 -0.066745 0.344123 0.028 Uiso calc 1 . . H C8 0.8247(10) -0.0543(5) 0.4796(4) 0.0224(11) Uani d 1 . . C H8 0.902617 -0.121928 0.496341 0.027 Uiso calc 1 . . H C9 0.7264(9) 0.0145(5) 0.5477(4) 0.0222(11) Uani d 1 . . C C10 0.6105(9) 0.1166(4) 0.5190(4) 0.0219(11) Uani d 1 . . C H10 0.543989 0.164203 0.561688 0.026 Uiso calc 1 . . H C11 0.5981(10) 0.1442(5) 0.4274(4) 0.0227(11) Uani d 1 . . C H11 0.520701 0.211066 0.408464 0.027 Uiso calc 1 . . H C12 0.6780(10) 0.1151(5) 0.2649(4) 0.0258(12) Uani d 1 . . C H12A 0.558164 0.168633 0.260924 0.039 Uiso calc 1 . . H H12C 0.676176 0.053702 0.235521 0.039 Uiso calc 1 . . H H12B 0.789517 0.146714 0.23446 0.039 Uiso calc 1 . . H N3 0.2113(8) 0.5613(4) 1.0858(3) 0.0200(9) Uani d 1 . . N N4 0.2746(9) 0.4640(4) 0.8295(4) 0.0247(11) Uani d 1 . . N H4B 0.243424 0.511653 0.78369 0.03 Uiso calc 1 . . H H4A 0.316767 0.396297 0.821886 0.03 Uiso calc 1 . . H C13 0.2799(9) 0.4546(5) 1.0740(4) 0.0214(11) Uani d 1 . . C H13 0.31074 0.403983 1.124588 0.026 Uiso calc 1 . . H C14 0.3049(9) 0.4195(4) 0.9899(4) 0.0194(11) Uani d 1 . . C H14 0.353043 0.345849 0.983719 0.023 Uiso calc 1 . . H C15 0.2578(9) 0.4947(4) 0.9119(4) 0.0199(11) Uani d 1 . . C C16 0.1888(10) 0.6055(5) 0.9270(5) 0.0230(12) Uani d 1 . . C H16 0.15805 0.658057 0.877481 0.028 Uiso calc 1 . . H C17 0.1667(9) 0.6368(4) 1.0117(4) 0.0203(11) Uani d 1 . . C H17 0.120844 0.710054 1.019707 0.024 Uiso calc 1 . . H C18 0.1934(11) 0.5980(5) 1.1760(5) 0.0289(13) Uani d 1 . . C H18A 0.215721 0.535636 1.222023 0.043 Uiso calc 1 . . H H18B 0.063105 0.640739 1.192809 0.043 Uiso calc 1 . . H H18C 0.289792 0.641782 1.172281 0.043 Uiso calc 1 . . H 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 I1 0.0261(2) 0.0142(2) 0.0229(2) -0.00466(14) -0.00381(15) -0.00243(13) I2 0.0266(2) 0.0145(2) 0.0171(2) -0.00182(14) -0.00280(15) -0.00586(13) Br1 0.0225(3) 0.0206(3) 0.0279(3) -0.0043(2) 0.0007(2) -0.0096(2) Br2 0.0336(4) 0.0158(3) 0.0238(3) -0.0098(2) 0.0004(2) -0.0048(2) O1 0.028(2) 0.0160(18) 0.030(2) -0.0019(16) -0.0087(18) -0.0044(15) C1 0.024(3) 0.015(2) 0.017(2) -0.003(2) -0.002(2) -0.0077(19) C2 0.020(3) 0.014(2) 0.021(3) -0.003(2) -0.001(2) -0.0089(19) C3 0.025(3) 0.013(2) 0.018(2) -0.003(2) 0.001(2) -0.0048(18) Br3 0.0224(3) 0.0115(3) 0.0187(3) -0.0013(2) 0.0012(2) -0.00538(19) Br4 0.0201(3) 0.0143(3) 0.0212(3) -0.0051(2) 0.0019(2) -0.0041(2) O2 0.028(2) 0.0184(18) 0.033(2) -0.0087(17) -0.0009(18) -0.0106(16) C4 0.029(3) 0.007(2) 0.017(2) -0.0053(19) -0.002(2) -0.0013(17) C5 0.022(3) 0.007(2) 0.014(2) 0.0023(18) -0.0020(19) -0.0064(16) C6 0.020(3) 0.014(2) 0.020(2) -0.004(2) -0.003(2) -0.0001(18) N1 0.024(3) 0.019(2) 0.021(2) -0.0063(19) -0.001(2) -0.0043(18) N2 0.027(3) 0.021(2) 0.020(2) -0.0077(19) -0.0017(19) 0.0008(18) C7 0.025(3) 0.017(2) 0.029(3) -0.007(2) 0.001(2) -0.008(2) C8 0.023(3) 0.015(2) 0.028(3) -0.003(2) -0.004(2) -0.002(2) C9 0.019(3) 0.020(3) 0.028(3) -0.008(2) -0.003(2) -0.001(2) C10 0.024(3) 0.016(2) 0.026(3) -0.005(2) -0.002(2) -0.004(2) C11 0.024(3) 0.014(2) 0.028(3) -0.003(2) -0.001(2) -0.004(2) C12 0.032(3) 0.024(3) 0.022(3) -0.010(2) 0.000(2) -0.003(2) N3 0.023(2) 0.017(2) 0.021(2) -0.0063(18) -0.0050(19) -0.0012(18) N4 0.033(3) 0.017(2) 0.023(2) -0.0017(19) -0.005(2) -0.0036(18) C13 0.017(3) 0.017(2) 0.029(3) -0.005(2) -0.006(2) 0.002(2) C14 0.020(3) 0.011(2) 0.026(3) -0.0051(19) 0.000(2) -0.0028(19) C15 0.018(3) 0.016(2) 0.026(3) -0.004(2) -0.004(2) -0.003(2) C16 0.025(3) 0.014(2) 0.030(3) -0.006(2) -0.009(2) 0.004(2) C17 0.020(3) 0.013(2) 0.030(3) -0.0016(19) -0.007(2) -0.005(2) C18 0.035(4) 0.026(3) 0.028(3) -0.007(3) -0.005(3) -0.010(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 '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 O1 C1 C3 121.6(5) . 2_766 ? O1 C1 C2 122.4(6) . . ? C3 C1 C2 115.9(5) 2_766 . ? C3 C2 C1 122.0(6) . . ? C3 C2 Br1 123.3(5) . . ? C1 C2 Br1 114.7(4) . . ? C2 C3 C1 121.9(5) . 2_766 ? C2 C3 Br2 122.5(5) . . ? C1 C3 Br2 115.5(4) 2_766 . ? O2 C4 C6 120.9(6) . 2_677 ? O2 C4 C5 121.1(5) . . ? C6 C4 C5 118.0(5) 2_677 . ? C6 C5 C4 122.3(5) . . ? C6 C5 Br3 123.0(5) . . ? C4 C5 Br3 114.4(4) . . ? C5 C6 C4 119.6(5) . 2_677 ? C5 C6 Br4 124.6(5) . . ? C4 C6 Br4 115.8(4) 2_677 . ? C11 N1 C7 120.7(5) . . ? C11 N1 C12 119.3(5) . . ? C7 N1 C12 120.1(5) . . ? C9 N2 H2B 120 . . ? C9 N2 H2A 120 . . ? H2B N2 H2A 120 . . ? N1 C7 C8 120.4(6) . . ? N1 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 119.8(5) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? N2 C9 C8 121.0(5) . . ? N2 C9 C10 120.9(6) . . ? C8 C9 C10 118.1(6) . . ? C11 C10 C9 118.7(6) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? N1 C11 C10 122.3(5) . . ? N1 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? H12C C12 H12B 109.5 . . ? C13 N3 C17 119.8(5) . . ? C13 N3 C18 120.9(5) . . ? C17 N3 C18 119.3(5) . . ? C15 N4 H4B 120 . . ? C15 N4 H4A 120 . . ? H4B N4 H4A 120 . . ? C14 C13 N3 121.8(5) . . ? C14 C13 H13 119.1 . . ? N3 C13 H13 119.1 . . ? C13 C14 C15 120.2(5) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? N4 C15 C16 121.5(6) . . ? N4 C15 C14 122.3(5) . . ? C16 C15 C14 116.2(6) . . ? C17 C16 C15 121.6(5) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 N3 120.5(5) . . ? C16 C17 H17 119.8 . . ? N3 C17 H17 119.8 . . ? N3 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? 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 Br1 C2 . 1.882(6) ? Br2 C3 . 1.880(6) ? O1 C1 . 1.205(8) ? C1 C3 2_766 1.491(9) ? C1 C2 . 1.491(8) ? C2 C3 . 1.336(8) ? Br3 C5 . 1.877(5) ? Br4 C6 . 1.869(6) ? O2 C4 . 1.232(7) ? C4 C6 2_677 1.486(8) ? C4 C5 . 1.482(8) ? C5 C6 . 1.345(8) ? N1 C11 . 1.342(8) ? N1 C7 . 1.357(8) ? N1 C12 . 1.483(8) ? N2 C9 . 1.355(8) ? N2 H2B . 0.86 ? N2 H2A . 0.86 ? C7 C8 . 1.372(9) ? C7 H7 . 0.93 ? C8 C9 . 1.415(9) ? C8 H8 . 0.93 ? C9 C10 . 1.413(8) ? C10 C11 . 1.364(9) ? C10 H10 . 0.93 ? C11 H11 . 0.93 ? C12 H12A . 0.96 ? C12 H12C . 0.96 ? C12 H12B . 0.96 ? N3 C13 . 1.357(8) ? N3 C17 . 1.369(7) ? N3 C18 . 1.468(8) ? N4 C15 . 1.323(8) ? N4 H4B . 0.86 ? N4 H4A . 0.86 ? C13 C14 . 1.364(9) ? C13 H13 . 0.93 ? C14 C15 . 1.416(8) ? C14 H14 . 0.93 ? C15 C16 . 1.417(8) ? C16 C17 . 1.355(9) ? C16 H16 . 0.93 ? C17 H17 . 0.93 ? C18 H18A . 0.96 ? C18 H18B . 0.96 ? C18 H18C . 0.96 ? 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 O1 C1 C2 C3 172.3(6) . . . . ? C3 C1 C2 C3 -4.3(9) 2_766 . . . ? O1 C1 C2 Br1 -7.1(7) . . . . ? C3 C1 C2 Br1 176.3(4) 2_766 . . . ? C1 C2 C3 C1 4.5(10) . . . 2_766 ? Br1 C2 C3 C1 -176.1(4) . . . 2_766 ? C1 C2 C3 Br2 -177.4(4) . . . . ? Br1 C2 C3 Br2 2.0(8) . . . . ? O2 C4 C5 C6 173.6(5) . . . . ? C6 C4 C5 C6 -4.7(9) 2_677 . . . ? O2 C4 C5 Br3 -0.4(7) . . . . ? C6 C4 C5 Br3 -178.8(4) 2_677 . . . ? C4 C5 C6 C4 4.8(9) . . . 2_677 ? Br3 C5 C6 C4 178.3(4) . . . 2_677 ? C4 C5 C6 Br4 -175.0(4) . . . . ? Br3 C5 C6 Br4 -1.5(7) . . . . ? C11 N1 C7 C8 -1.5(9) . . . . ? C12 N1 C7 C8 178.1(6) . . . . ? N1 C7 C8 C9 1.0(10) . . . . ? C7 C8 C9 N2 178.0(6) . . . . ? C7 C8 C9 C10 -0.3(9) . . . . ? N2 C9 C10 C11 -178.2(6) . . . . ? C8 C9 C10 C11 0.2(9) . . . . ? C7 N1 C11 C10 1.4(10) . . . . ? C12 N1 C11 C10 -178.2(6) . . . . ? C9 C10 C11 N1 -0.7(10) . . . . ? C17 N3 C13 C14 -0.5(9) . . . . ? C18 N3 C13 C14 -177.4(6) . . . . ? N3 C13 C14 C15 -0.4(9) . . . . ? C13 C14 C15 N4 -178.2(6) . . . . ? C13 C14 C15 C16 1.1(9) . . . . ? N4 C15 C16 C17 178.3(6) . . . . ? C14 C15 C16 C17 -1.0(9) . . . . ? C15 C16 C17 N3 0.2(10) . . . . ? C13 N3 C17 C16 0.6(9) . . . . ? C18 N3 C17 C16 177.6(6) . . . . ?