#------------------------------------------------------------------------------ #$Date: 2023-09-16 00:55:12 +0300 (Sat, 16 Sep 2023) $ #$Revision: 286356 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/13/21/7132138.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_7132138 loop_ _publ_author_name 'Biswas, Subhankar' 'Purkayastha, Siddhartha Kumar' 'Guha, Ankur Kanti' 'Pan, Subhas Chandra' _publ_section_title ; Sequential Organo and Metal Catalyzed Reaction Between 3-Pyrrolyloxindoles and Linear Nitroenynes: Access to Cyclic Aza-Spirooxindoles ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D3CC03713D _journal_year 2023 _chemical_absolute_configuration R,S _chemical_formula_sum 'C23 H18 Br N3 O3' _chemical_formula_weight 464.31 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2019/1 _audit_update_record ; 2023-07-22 deposited with the CCDC. 2023-09-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.1820(6) _cell_length_b 10.2729(6) _cell_length_c 19.3413(12) _cell_measurement_reflns_used 9807 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 25.09 _cell_measurement_theta_min 2.24 _cell_volume 2023.1(2) _computing_structure_refinement 'SHELXL-2019/1 (Sheldrick, 2019)' _diffrn_ambient_temperature 297(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_unetI/netI 0.0213 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 48721 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 24.996 _diffrn_reflns_theta_max 24.996 _diffrn_reflns_theta_min 2.106 _exptl_absorpt_coefficient_mu 2.063 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.5507 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction -------------------------------------------------------------------------- Reference: 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 1.524 _exptl_crystal_description Block _exptl_crystal_F_000 944 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.296 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.032 _refine_ls_abs_structure_details ; Flack x determined using 1355 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.040(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 272 _refine_ls_number_reflns 3531 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0228 _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^)+(0.0350P)^2^+0.3910P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.0604 _reflns_Friedel_coverage 0.740 _reflns_Friedel_fraction_full 0.994 _reflns_Friedel_fraction_max 0.994 _reflns_number_gt 3323 _reflns_number_total 3531 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3cc03713d2.cif _cod_data_source_block SB-LNE-7-6Br_a _cod_database_code 7132138 _shelx_shelxl_version_number 2019/1 _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 SB-LNE-7-6Br_a.res in P2(1)2(1)2(1) SB-LNE-7-6Br_a.res created by SHELXL-2019/1 at 16:47:06 on 21-Jul-2023 CELL 0.71073 10.1820 10.2729 19.3413 90.000 90.000 90.000 ZERR 4.000 0.0006 0.0006 0.0012 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H Br N O UNIT 92 72 4 12 12 OMIT -3 50 REM Old TITL SB-LNE-7-6Br in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1): R1 0.135, Rweak 0.026, Alpha 0.004 REM 1.959 for 23 systematic absences, Orientation as input REM Flack x= 0.066 ( 0.004 ) from 1430 Parsons' quotients REM Formula found by SHELXT: C24 Br N3 O2 L.S. 10 ACTA BOND FMAP 2 PLAN 20 TEMP 23.850 WGHT 0.035000 0.391000 FVAR 0.79266 BR01 3 0.098978 0.703196 0.442573 11.00000 0.08604 0.04028 = 0.04476 -0.00409 0.00619 0.00630 O002 5 0.286937 0.277568 0.125859 11.00000 0.06757 0.04677 = 0.06267 0.00786 -0.00526 0.00500 O003 5 0.177839 0.097461 0.227220 11.00000 0.04944 0.03668 = 0.05688 -0.00872 -0.00270 -0.00697 N004 4 0.120051 0.298451 0.270363 11.00000 0.03597 0.03571 = 0.04357 -0.00401 -0.00769 0.00169 N005 4 0.377643 0.113006 0.335770 11.00000 0.03408 0.03423 = 0.04952 0.00819 0.00305 0.00022 O1 5 0.368612 0.103648 0.081018 11.00000 0.11916 0.05649 = 0.05586 -0.00979 -0.00624 0.00629 N1 4 0.362265 0.185614 0.126650 11.00000 0.06857 0.03821 = 0.04762 0.00676 0.00639 -0.00757 C008 1 0.332575 0.226441 0.297379 11.00000 0.03321 0.03365 = 0.04558 0.00202 -0.00103 -0.00199 C009 1 0.572789 0.273957 0.281518 11.00000 0.03675 0.04041 = 0.05529 0.00779 0.00620 -0.00550 AFIX 43 H009 2 0.633473 0.336080 0.267279 11.00000 -1.20000 AFIX 0 C00A 1 0.302225 0.022448 0.369467 11.00000 0.03734 0.04080 = 0.05963 0.00521 0.00639 -0.00744 AFIX 43 H00A 2 0.212594 0.009563 0.363240 11.00000 -1.20000 AFIX 0 C00B 1 0.294636 0.341537 0.341554 11.00000 0.03365 0.03312 = 0.04087 0.00462 -0.00124 -0.00101 C00C 1 0.201754 0.195551 0.260059 11.00000 0.04020 0.03508 = 0.04036 0.00331 0.00021 -0.00325 C00D 1 0.109576 0.491534 0.348238 11.00000 0.04177 0.03703 = 0.04035 0.00438 -0.00325 0.00198 AFIX 43 H00D 2 0.028139 0.520212 0.332680 11.00000 -1.20000 AFIX 0 C00E 1 0.505205 0.104558 0.360332 11.00000 0.03369 0.03167 = 0.04861 0.00177 0.00099 0.00174 C00F 1 0.603978 0.194296 0.333790 11.00000 0.03382 0.03310 = 0.05115 0.00001 0.00559 0.00121 C00G 1 0.177186 0.554679 0.400884 11.00000 0.05240 0.03185 = 0.03693 0.00349 0.00435 -0.00235 C00H 1 0.441301 0.265827 0.244832 11.00000 0.04216 0.03471 = 0.04667 0.00704 0.00380 0.00074 AFIX 13 H00H 2 0.419996 0.351973 0.226178 11.00000 -1.20000 AFIX 0 C00I 1 0.357294 0.404829 0.394620 11.00000 0.04025 0.04610 = 0.04589 0.00265 -0.00612 -0.00073 AFIX 43 H00I 2 0.438590 0.375899 0.410251 11.00000 -1.20000 AFIX 0 C00J 1 0.734065 0.194196 0.368971 11.00000 0.03378 0.04204 = 0.04821 0.00079 0.00704 -0.00329 C00K 1 0.297530 0.513353 0.424947 11.00000 0.05593 0.04543 = 0.03949 -0.00381 -0.00786 -0.00607 AFIX 43 H00K 2 0.338656 0.557196 0.461016 11.00000 -1.20000 AFIX 0 C00L 1 0.170606 0.383889 0.320534 11.00000 0.03894 0.03307 = 0.03655 0.00186 -0.00197 -0.00317 C00M 1 0.380467 -0.045173 0.413425 11.00000 0.05438 0.03805 = 0.05695 0.01457 0.00844 -0.00305 AFIX 43 H00M 2 0.354448 -0.113508 0.441834 11.00000 -1.20000 AFIX 0 C00N 1 0.508098 0.006616 0.408337 11.00000 0.04332 0.03824 = 0.05325 0.00782 0.00396 0.00334 AFIX 43 H00N 2 0.581297 -0.020784 0.433143 11.00000 -1.20000 AFIX 0 C00O 1 0.812375 0.083922 0.368561 11.00000 0.04012 0.04703 = 0.06799 -0.00088 0.00536 0.00101 AFIX 43 H00O 2 0.784180 0.009705 0.345369 11.00000 -1.20000 AFIX 0 C00P 1 0.458665 0.171652 0.184644 11.00000 0.05268 0.04446 = 0.04894 0.00414 0.00558 0.00613 AFIX 23 H00B 2 0.546405 0.182907 0.166044 11.00000 -1.20000 H00C 2 0.452798 0.083549 0.202418 11.00000 -1.20000 AFIX 0 C00Q 1 -0.011317 0.306467 0.241158 11.00000 0.04341 0.05415 = 0.05323 -0.00916 -0.01320 0.00644 AFIX 137 H00E 2 -0.012391 0.264974 0.196688 11.00000 -1.50000 H00F 2 -0.035915 0.396190 0.236173 11.00000 -1.50000 H00G 2 -0.072361 0.263526 0.271336 11.00000 -1.50000 AFIX 0 C00R 1 0.931729 0.083202 0.402221 11.00000 0.04083 0.07312 = 0.08026 0.01737 0.00306 0.00441 AFIX 43 H00R 2 0.982817 0.008161 0.401884 11.00000 -1.20000 AFIX 0 C00S 1 0.778397 0.303428 0.404013 11.00000 0.04953 0.04960 = 0.06335 -0.00619 0.00588 -0.00553 AFIX 43 H00S 2 0.727265 0.378421 0.404967 11.00000 -1.20000 AFIX 0 C00T 1 0.975739 0.191219 0.435997 11.00000 0.04005 0.10901 = 0.05800 0.01334 -0.00302 -0.01001 AFIX 43 H00T 2 1.057171 0.190629 0.457773 11.00000 -1.20000 AFIX 0 C00U 1 0.898378 0.301335 0.437566 11.00000 0.06527 0.09022 = 0.05693 -0.01739 0.00289 -0.03096 AFIX 43 H00U 2 0.927049 0.374711 0.461343 11.00000 -1.20000 AFIX 0 HKLF 4 REM SB-LNE-7-6Br_a.res in P2(1)2(1)2(1) REM wR2 = 0.0604, GooF = S = 1.013, Restrained GooF = 1.013 for all data REM R1 = 0.0228 for 3323 Fo > 4sig(Fo) and 0.0255 for all 3531 data REM 272 parameters refined using 0 restraints END WGHT 0.0289 0.4354 REM Highest difference peak 0.296, deepest hole -0.401, 1-sigma level 0.032 Q1 1 0.0251 0.6621 0.4448 11.00000 0.05 0.30 Q2 1 0.0585 0.7079 0.3838 11.00000 0.05 0.14 Q3 1 0.0624 0.6630 0.4986 11.00000 0.05 0.12 Q4 1 0.1045 0.7346 0.3986 11.00000 0.05 0.12 Q5 1 0.9190 0.2468 0.4494 11.00000 0.05 0.12 Q6 1 0.3020 0.3462 0.3815 11.00000 0.05 0.12 Q7 1 0.3436 0.3950 0.3502 11.00000 0.05 0.12 Q8 1 0.2615 0.2107 0.2837 11.00000 0.05 0.12 Q9 1 0.9307 0.2856 0.4077 11.00000 0.05 0.11 Q10 1 0.1724 0.5663 0.3573 11.00000 0.05 0.11 Q11 1 0.2116 0.5871 0.3041 11.00000 0.05 0.11 Q12 1 0.5605 0.1396 0.3465 11.00000 0.05 0.11 Q13 1 0.1885 0.7550 0.4905 11.00000 0.05 0.11 Q14 1 0.1173 0.5100 0.3942 11.00000 0.05 0.11 Q15 1 1.0185 -0.0529 0.4402 11.00000 0.05 0.10 Q16 1 0.1895 0.8045 0.4293 11.00000 0.05 0.10 Q17 1 0.2868 0.3219 0.1749 11.00000 0.05 0.10 Q18 1 0.7370 0.2273 0.4024 11.00000 0.05 0.10 Q19 1 0.9114 0.1387 0.4413 11.00000 0.05 0.10 Q20 1 0.1795 0.6720 0.4431 11.00000 0.05 0.10 ; _shelx_res_checksum 93516 _shelx_hkl_file ; -1 0 0 0.40 0.60 -1 0 0 0.90 0.70 -1 0 0 0.50 1.00 1 0 0 0.40 0.40 1 0 0 1.00 0.60 1 0 0 0.20 0.50 1 0 0 0.30 0.40 1 0 0 0.30 0.50 1 0 0 0.20 0.60 1 0 0 0.60 0.50 -2 0 0 34.30 2.80 -2 0 0 27.90 3.70 -2 0 0 27.80 3.30 -2 0 0 32.80 2.90 -2 0 0 32.50 3.20 -2 0 0 32.70 2.90 2 0 0 34.20 3.00 2 0 0 30.90 3.30 2 0 0 33.20 3.00 2 0 0 39.40 3.90 2 0 0 33.50 3.20 2 0 0 35.30 3.50 2 0 0 34.90 2.90 -3 0 0 1.90 2.00 -3 0 0 7.00 2.40 -3 0 0 0.40 1.20 -3 0 0 -1.00 1.80 -3 0 0 0.00 1.50 -3 0 0 1.90 2.10 -3 0 0 -1.90 1.30 -3 0 0 1.40 2.40 -3 0 0 -0.10 1.80 -3 0 0 0.40 1.30 3 0 0 0.40 1.30 3 0 0 0.20 1.90 3 0 0 -1.10 1.60 3 0 0 0.50 2.10 3 0 0 0.50 1.90 3 0 0 3.30 1.90 3 0 0 1.50 1.60 -4 0 0 6135.89 359.56 -4 0 0 6486.75 358.66 -4 0 0 6990.40 360.06 -4 0 0 6279.67 359.36 -4 0 0 6261.87 357.66 -4 0 0 6380.16 359.36 -4 0 0 6166.28 358.76 -4 0 0 6113.29 359.76 -4 0 0 6215.08 357.96 -4 0 0 6062.19 357.56 4 0 0 6620.34 359.86 4 0 0 6187.38 358.46 4 0 0 5781.22 358.06 4 0 0 6181.08 359.16 4 0 0 6441.36 358.16 4 0 0 6596.14 360.16 -5 0 0 -1.10 2.70 -5 0 0 2.30 3.10 -5 0 0 1.70 2.10 -5 0 0 -0.60 2.80 -5 0 0 2.20 3.80 -5 0 0 4.20 2.80 -5 0 0 2.50 4.40 -5 0 0 -4.70 3.50 -5 0 0 3.30 2.70 -5 0 0 2.50 2.40 5 0 0 6.70 4.50 5 0 0 -0.50 2.60 5 0 0 8.10 4.30 5 0 0 4.30 3.60 5 0 0 2.80 3.00 5 0 0 -0.40 2.40 5 0 0 3.10 3.40 -6 0 0 92.79 10.10 -6 0 0 79.49 10.30 -6 0 0 73.79 9.70 -6 0 0 90.29 8.60 -6 0 0 83.49 9.20 -6 0 0 95.89 10.50 -6 0 0 91.89 8.00 -6 0 0 84.19 10.30 -6 0 0 104.09 8.00 6 0 0 76.09 9.40 6 0 0 100.99 9.00 6 0 0 92.79 9.30 6 0 0 87.39 9.90 6 0 0 83.79 8.80 -7 0 0 -0.30 2.80 -7 0 0 5.80 4.40 -7 0 0 0.20 4.00 -7 0 0 1.60 2.90 -7 0 0 1.90 4.40 -7 0 0 2.80 5.40 -7 0 0 -0.80 5.40 7 0 0 0.50 3.90 7 0 0 -6.60 4.40 7 0 0 1.30 4.70 7 0 0 -0.30 5.30 7 0 0 -2.80 3.30 7 0 0 2.80 5.50 -8 0 0 29.30 7.30 -8 0 0 26.60 6.90 -8 0 0 31.40 8.20 -8 0 0 27.30 9.10 8 0 0 24.60 8.80 8 0 0 29.50 7.90 8 0 0 23.60 7.20 8 0 0 43.00 7.30 8 0 0 33.50 9.70 -9 0 0 3.30 6.90 -9 0 0 -0.80 6.70 -9 0 0 -1.90 5.50 9 0 0 6.00 8.20 9 0 0 -1.50 7.60 9 0 0 9.80 8.70 -10 0 0 741.53 49.70 -10 0 0 743.53 54.19 10 0 0 762.62 54.09 10 0 0 792.62 51.99 -11 0 0 8.30 10.60 -11 0 0 5.60 10.00 11 0 0 6.70 10.30 11 0 0 7.00 11.40 -12 0 0 -8.60 12.70 -12 0 0 -2.90 12.10 12 0 0 8.70 12.00 12 0 0 1.90 9.90 12 -1 0 5.50 11.40 12 -1 0 23.10 14.10 -12 1 0 23.30 13.50 -12 1 0 25.90 13.20 -12 1 0 9.00 12.70 11 -1 0 -1.00 10.60 11 -1 0 0.50 9.20 -11 1 0 3.10 10.80 -11 1 0 -12.00 9.50 -11 1 0 -2.60 10.80 10 -1 0 25.80 9.90 10 -1 0 18.10 10.10 -10 1 0 29.50 12.30 -10 1 0 19.70 7.90 -10 1 0 21.80 11.30 9 -1 0 32.30 10.30 9 -1 0 60.59 12.80 9 -1 0 37.60 9.90 -9 1 0 48.00 12.30 -9 1 0 45.10 10.80 -9 1 0 38.10 8.90 8 -1 0 139.29 15.60 8 -1 0 135.59 12.80 8 -1 0 104.09 12.50 8 -1 0 136.79 14.60 8 -1 0 116.89 12.00 8 -1 0 128.09 16.10 -8 1 0 129.09 13.60 -8 1 0 127.39 15.20 -8 1 0 113.99 12.30 -8 1 0 119.79 11.70 -8 1 0 121.19 16.70 7 -1 0 5.20 4.60 7 -1 0 2.30 3.20 7 -1 0 4.00 6.90 7 -1 0 6.10 5.50 7 -1 0 7.50 4.70 7 -1 0 9.70 6.30 -7 1 0 7.20 4.20 -7 1 0 4.30 3.90 -7 1 0 12.10 4.50 -7 1 0 7.30 3.80 -7 1 0 5.40 5.50 -7 1 0 4.50 5.70 -7 1 0 2.40 3.70 6 -1 0 6.70 4.10 6 -1 0 11.90 4.50 6 -1 0 9.80 4.40 6 -1 0 10.60 5.90 6 -1 0 6.60 3.70 6 -1 0 4.80 2.60 -6 1 0 10.70 3.90 -6 1 0 11.10 4.10 -6 1 0 0.80 4.50 -6 1 0 6.10 3.00 -6 1 0 14.20 5.30 -6 1 0 10.70 5.40 -6 1 0 8.80 4.10 -6 1 0 10.90 5.30 -6 1 0 6.10 3.80 -6 1 0 9.60 4.20 5 -1 0 218.48 17.40 5 -1 0 217.18 16.20 5 -1 0 238.28 16.50 5 -1 0 226.58 15.90 5 -1 0 230.58 16.20 5 -1 0 195.38 17.00 5 -1 0 238.28 14.60 -5 1 0 211.88 15.80 -5 1 0 231.98 16.80 -5 1 0 224.28 16.00 -5 1 0 210.08 16.80 -5 1 0 248.78 17.40 -5 1 0 231.98 16.40 -5 1 0 213.78 17.10 -5 1 0 219.08 15.70 -5 1 0 226.78 17.50 -5 1 0 201.68 15.50 -5 1 0 218.58 16.10 4 -1 0 1591.44 92.29 4 -1 0 1560.34 92.99 4 -1 0 1602.74 92.59 4 -1 0 1568.74 91.89 4 -1 0 1580.54 93.39 4 -1 0 1675.53 92.39 4 -1 0 1426.56 91.89 -4 1 0 1571.64 92.19 -4 1 0 1558.94 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11.50 9 -5 10 9.20 11.00 9 -5 10 12.60 11.90 10 -5 10 14.00 14.90 10 4 -10 16.60 11.70 10 4 -10 -21.00 11.20 10 4 -10 11.00 13.70 -10 -4 10 18.70 13.40 -10 -4 10 9.40 12.30 -10 -4 10 3.40 10.50 9 4 -10 2.70 11.90 9 4 -10 12.80 12.90 9 4 -10 14.70 10.50 -9 -4 10 24.10 12.00 -9 -4 10 25.60 11.10 -9 -4 10 25.30 11.90 8 4 -10 86.89 14.90 8 4 -10 95.29 16.00 8 4 -10 95.69 15.90 -8 -4 10 111.99 16.10 -8 -4 10 105.19 16.00 -8 -4 10 101.19 14.60 7 4 -10 140.79 19.10 7 4 -10 165.28 20.00 7 4 -10 205.28 19.00 -7 -4 10 175.38 18.00 -7 -4 10 162.08 17.80 -7 -4 10 167.28 18.80 6 4 -10 329.37 27.10 6 4 -10 312.77 27.10 6 4 -10 296.47 24.70 -6 -4 10 330.17 24.70 -6 -4 10 309.77 24.10 -6 -4 10 321.07 24.60 -5 -4 10 296.27 21.50 -5 -4 10 273.37 22.10 -5 -4 10 264.47 23.10 -5 -4 10 275.97 19.30 -5 -4 10 257.87 20.80 4 4 -10 894.41 53.39 4 4 -10 846.62 60.09 4 4 -10 888.21 53.99 4 4 -10 829.92 55.29 4 4 -10 867.81 56.89 -4 -4 10 919.11 56.29 -4 -4 10 856.81 53.69 -4 -4 10 879.91 54.29 -4 -4 10 878.81 52.79 -4 -4 10 852.41 52.99 3 4 -10 460.65 31.80 3 4 -10 471.95 32.10 3 4 -10 421.06 34.40 3 4 -10 480.05 33.80 3 4 -10 399.26 33.40 3 4 -10 470.65 31.30 -3 -4 10 484.55 30.80 -3 -4 10 510.25 31.80 -3 -4 10 504.55 30.90 -3 -4 10 520.65 30.80 -3 -4 10 450.35 31.50 -3 -4 10 488.85 34.50 -3 -4 10 467.75 29.70 2 4 -10 423.16 29.40 2 4 -10 446.46 30.20 2 4 -10 430.66 28.90 2 4 -10 433.96 31.90 2 4 -10 389.86 30.20 2 4 -10 428.56 31.20 2 4 -10 450.95 31.10 -2 -4 10 419.06 26.40 -2 -4 10 415.26 28.10 -2 -4 10 445.26 28.70 -2 -4 10 437.46 28.60 -2 -4 10 422.76 30.20 -2 -4 10 445.66 27.50 1 4 -10 2011.00 116.59 1 4 -10 1900.71 114.19 1 4 -10 2001.60 116.29 1 4 -10 1977.40 116.69 1 4 -10 2008.10 114.39 1 4 -10 1931.91 113.39 1 4 -10 2116.59 116.09 -1 -4 10 1875.41 112.99 -1 -4 10 1862.41 113.59 -1 -4 10 1947.01 111.79 -1 -4 10 1830.72 112.89 -1 -4 10 1997.50 111.09 -1 -4 10 1859.41 113.79 -1 -4 10 1904.21 116.09 0 4 -10 328.57 24.40 0 4 -10 309.77 24.10 0 4 -10 328.77 24.40 0 4 -10 292.97 22.40 0 4 -10 307.67 21.80 0 4 -10 327.07 25.00 0 4 -10 312.07 20.90 0 -4 10 295.97 18.80 0 -4 10 305.67 20.60 0 -4 10 298.67 21.60 0 -4 10 321.97 22.50 0 -4 10 300.47 24.30 0 -4 10 360.56 23.00 0 -4 10 323.57 19.20 -1 4 -10 1894.11 115.59 -1 4 -10 1965.30 112.29 -1 4 -10 1780.32 114.49 -1 4 -10 1884.81 116.49 -1 4 -10 1865.81 113.29 -1 4 -10 1927.91 115.19 1 -4 10 2011.20 110.79 1 -4 10 2081.19 114.99 1 -4 10 1998.00 111.99 1 -4 10 1868.01 114.79 1 -4 10 1959.80 113.89 1 -4 10 2079.79 110.89 -2 4 -10 447.86 30.50 -2 4 -10 438.06 26.20 -2 4 -10 422.86 25.30 -2 4 -10 392.86 31.20 -2 4 -10 432.96 27.90 -2 4 -10 450.45 30.30 2 -4 10 420.46 26.10 2 -4 10 432.06 30.20 2 -4 10 416.96 25.80 2 -4 10 430.26 30.00 2 -4 10 453.25 31.10 -3 4 -10 503.85 33.80 -3 4 -10 521.65 34.70 -3 4 -10 496.05 35.50 3 -4 10 492.95 34.00 3 -4 10 422.86 33.80 3 -4 10 543.75 35.30 3 -4 10 486.45 30.30 -4 4 -10 849.81 54.49 -4 4 -10 830.72 52.89 -4 4 -10 839.62 55.49 4 -4 10 850.11 55.49 4 -4 10 734.23 54.09 4 -4 10 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41.60 14.90 -4 1 21 37.30 12.20 -4 1 21 38.50 12.90 3 -1 -21 336.57 34.70 3 -1 -21 372.26 35.20 -3 1 21 342.77 29.50 -3 1 21 359.16 30.70 2 -1 -21 54.59 17.10 2 -1 -21 38.30 15.50 -2 1 21 30.20 10.20 -2 1 21 41.00 11.90 1 -1 -21 97.39 20.00 1 -1 -21 120.19 19.10 -1 1 21 160.58 19.00 -1 1 21 134.29 17.00 0 -1 -21 33.40 12.90 0 -1 -21 41.40 13.40 0 1 21 39.80 12.00 0 1 21 47.60 14.10 -1 -1 -21 107.69 19.40 -1 -1 -21 145.89 18.90 1 1 21 113.29 18.00 1 1 21 111.99 16.90 -2 -1 -21 40.60 14.70 2 1 21 37.30 12.40 2 1 21 53.19 14.50 -3 -1 -21 279.27 33.00 -3 -1 -21 316.57 28.70 3 1 21 339.37 29.90 3 1 21 322.27 32.50 -4 -1 -21 29.20 11.60 -4 -1 -21 43.50 14.00 4 1 21 10.80 15.20 4 1 21 49.10 15.50 -5 -1 -21 26.80 12.60 -5 -1 -21 20.60 12.50 5 1 21 -2.50 14.00 5 -2 -21 76.59 21.20 -5 2 21 79.59 14.50 -5 2 21 75.69 14.20 4 -2 -21 43.00 15.10 4 -2 -21 44.80 16.20 -4 2 21 50.89 13.00 -4 2 21 33.80 10.90 3 -2 -21 -3.40 9.10 3 -2 -21 5.30 11.70 -3 2 21 -1.30 10.80 -3 2 21 1.10 10.30 2 -2 -21 43.50 15.80 2 -2 -21 23.30 14.10 -2 2 21 28.80 11.80 -2 2 21 28.10 10.40 1 -2 -21 135.49 21.80 1 -2 -21 107.69 19.90 -1 2 21 110.79 16.30 -1 2 21 99.09 15.60 0 -2 -21 27.70 12.80 0 -2 -21 -1.90 12.50 0 2 21 12.20 11.50 0 2 21 15.50 10.60 -1 -2 -21 118.99 20.10 -1 -2 -21 89.99 17.10 1 2 21 132.89 18.60 1 2 21 115.19 18.10 -2 -2 -21 21.70 13.70 2 2 21 38.40 13.10 2 2 21 25.20 12.00 -3 -2 -21 -15.60 10.10 -3 -2 -21 -7.30 8.30 3 2 21 -4.40 10.50 3 2 21 9.70 12.40 -4 -2 -21 29.00 12.20 -4 -2 -21 27.00 16.70 4 2 21 53.09 16.80 4 2 21 49.90 17.40 -5 -2 -21 95.39 20.30 -5 -2 -21 60.79 15.70 5 2 21 67.79 16.10 5 2 21 56.39 17.60 4 -3 -21 45.70 17.80 4 -3 -21 29.20 15.60 -4 3 21 21.30 11.20 -4 3 21 22.70 11.60 3 -3 -21 118.99 23.60 3 -3 -21 101.49 21.30 -3 3 21 116.09 16.00 -3 3 21 139.59 18.40 2 -3 -21 79.69 19.00 2 -3 -21 92.19 19.50 -2 3 21 59.89 14.40 1 -3 -21 6.50 11.30 1 -3 -21 27.00 13.80 -1 3 21 19.20 10.10 -1 3 21 14.90 10.00 0 -3 -21 9.20 11.80 0 -3 -21 4.90 11.70 0 3 21 11.20 9.80 0 3 21 19.70 13.20 -1 -3 -21 18.50 12.00 1 3 21 22.40 12.60 1 3 21 28.20 14.30 -2 -3 -21 49.30 15.60 2 3 21 85.39 16.70 2 3 21 90.69 17.70 -3 -3 -21 101.09 21.30 -3 -3 -21 123.39 23.70 3 3 21 114.39 20.00 3 3 21 123.39 21.20 -4 -3 -21 20.90 13.80 -4 -3 -21 42.00 13.80 4 3 21 38.60 14.20 4 3 21 14.10 15.10 3 -4 -21 44.60 16.60 3 -4 -21 42.00 17.20 -3 4 21 86.29 15.80 -3 4 21 63.19 13.40 2 -4 -21 13.30 13.40 2 -4 -21 17.00 13.00 -2 4 21 21.50 11.90 -2 4 21 24.20 11.20 1 -4 -21 73.19 19.70 1 -4 -21 115.69 20.40 -1 4 21 117.39 17.60 -1 4 21 107.29 18.00 0 -4 -21 255.77 28.50 0 -4 -21 229.98 28.80 0 4 21 280.47 28.40 0 4 21 258.57 27.50 -1 -4 -21 82.39 18.80 1 4 21 120.39 18.80 1 4 21 96.79 17.70 -2 -4 -21 14.20 11.50 2 4 21 2.60 12.10 2 4 21 17.50 13.30 -3 -4 -21 40.30 16.30 3 4 21 63.09 17.60 3 4 21 59.79 15.90 2 -5 -21 153.68 25.00 -2 5 21 182.88 20.90 -2 5 21 145.79 20.70 1 -5 -21 13.60 12.60 1 -5 -21 35.40 14.70 -1 5 21 16.10 12.00 -1 5 21 2.10 9.40 0 -5 -21 -7.30 12.20 0 -5 -21 -1.40 11.70 0 5 21 22.50 12.50 0 5 21 -5.30 9.20 -1 -5 -21 10.20 13.40 1 5 21 -2.50 11.00 1 5 21 11.80 14.30 -2 -5 -21 140.09 24.10 2 5 21 175.68 24.70 2 5 21 119.09 19.10 1 4 -22 17.40 12.60 1 4 -22 32.80 15.80 -1 -4 22 9.40 10.10 -1 -4 22 29.00 12.60 0 4 -22 3.10 12.20 0 4 -22 14.90 12.00 0 -4 22 10.30 10.40 0 -4 22 -5.90 9.40 -1 4 -22 4.50 13.30 -1 4 -22 22.90 13.20 1 -4 22 20.40 11.30 1 -4 22 1.90 12.00 3 3 -22 0.90 14.00 2 3 -22 11.90 14.40 2 3 -22 -26.40 10.30 -2 -3 22 2.80 11.10 -2 -3 22 -4.80 9.30 1 3 -22 -0.90 10.60 -1 -3 22 7.60 10.30 -1 -3 22 15.30 11.00 0 3 -22 79.09 17.20 0 3 -22 83.59 18.50 0 -3 22 73.49 14.30 0 -3 22 75.59 15.50 -1 3 -22 29.20 15.00 -1 3 -22 17.80 11.90 1 -3 22 18.10 10.80 1 -3 22 7.00 10.70 -2 3 -22 8.50 11.20 -2 3 -22 13.20 12.30 2 -3 22 6.70 10.90 2 -3 22 2.90 11.20 -3 3 -22 0.20 11.70 3 -3 22 2.50 13.10 3 2 -22 73.89 18.50 3 2 -22 62.19 17.30 -3 -2 22 73.29 14.40 2 2 -22 71.19 21.80 2 2 -22 71.79 16.80 -2 -2 22 73.59 14.30 1 2 -22 148.59 22.50 1 2 -22 143.09 22.90 -1 -2 22 125.19 18.50 0 2 -22 8.40 12.00 0 2 -22 17.60 13.80 0 -2 22 21.20 10.40 0 -2 22 28.00 11.80 -1 2 -22 124.69 20.90 -1 2 -22 127.99 19.80 1 -2 22 127.49 19.20 1 -2 22 129.09 17.70 -2 2 -22 104.29 23.90 -2 2 -22 90.49 19.20 2 -2 22 97.89 17.60 2 -2 22 77.59 16.30 -3 2 -22 44.40 14.20 -3 2 -22 107.99 21.20 3 -2 22 53.09 14.90 3 -2 22 49.40 17.50 4 1 -22 26.70 15.90 -4 -1 22 48.10 13.50 3 1 -22 43.60 16.20 3 1 -22 28.30 13.80 -3 -1 22 33.50 12.60 2 1 -22 38.60 16.00 2 1 -22 57.69 15.30 -2 -1 22 59.89 13.40 1 1 -22 145.79 22.90 1 1 -22 140.09 21.60 -1 -1 22 123.59 17.50 0 1 -22 58.49 14.90 0 1 -22 58.59 15.70 0 -1 22 50.19 13.90 -1 1 -22 104.39 18.00 -1 1 -22 115.19 19.90 1 -1 22 151.28 20.60 -2 1 -22 48.90 14.70 2 -1 22 33.60 14.60 2 -1 22 50.69 14.00 -3 1 -22 19.10 13.00 -3 1 -22 19.60 13.80 3 -1 22 43.00 16.30 3 -1 22 8.40 12.10 -4 1 -22 20.40 11.30 4 -1 22 23.90 15.10 4 -1 22 25.80 15.40 4 0 -22 7.00 12.60 -4 0 22 8.20 11.80 3 0 -22 162.88 24.40 3 0 -22 147.19 22.80 -3 0 22 189.48 22.90 2 0 -22 10.60 12.20 2 0 -22 16.30 13.50 -2 0 22 4.30 9.80 1 0 -22 235.18 27.70 1 0 -22 229.58 29.40 -1 0 22 281.97 25.30 0 0 -22 6.20 10.70 0 0 -22 9.10 10.80 0 0 22 28.70 12.20 -1 0 -22 262.67 28.30 -1 0 -22 227.48 28.30 1 0 22 308.87 28.10 -2 0 -22 9.00 10.90 2 0 22 -21.10 9.40 -3 0 -22 219.28 28.50 3 0 22 164.88 26.40 -4 0 -22 9.90 12.80 -4 0 -22 1.50 8.90 4 0 22 5.50 14.10 4 -1 -22 38.00 18.00 -4 1 22 37.90 11.70 3 -1 -22 35.70 16.20 3 -1 -22 23.70 15.00 -3 1 22 36.60 13.60 -3 1 22 50.89 12.80 2 -1 -22 34.70 15.50 2 -1 -22 28.20 14.50 -2 1 22 31.50 11.50 -2 1 22 44.10 12.30 1 -1 -22 91.69 19.30 1 -1 -22 104.69 20.90 -1 1 22 149.39 18.60 -1 1 22 120.69 17.20 0 -1 -22 69.59 15.90 0 1 22 59.29 14.30 0 1 22 60.19 13.80 -1 -1 -22 154.78 21.00 -1 -1 -22 120.69 20.90 1 1 22 163.38 20.60 1 1 22 129.89 19.80 -2 -1 -22 37.20 13.30 2 1 22 47.20 13.90 2 1 22 59.49 15.50 -3 -1 -22 41.70 16.30 3 1 22 53.99 16.90 -4 -1 -22 18.30 13.20 -4 -1 -22 37.60 13.50 4 1 22 11.40 13.90 3 -2 -22 54.29 16.80 3 -2 -22 99.89 21.40 -3 2 22 65.29 13.80 -3 2 22 69.59 13.90 2 -2 -22 85.99 18.80 2 -2 -22 79.69 19.70 -2 2 22 115.99 17.30 -2 2 22 101.29 17.00 1 -2 -22 158.48 24.40 1 -2 -22 169.68 23.80 -1 2 22 146.79 19.40 -1 2 22 125.59 18.40 0 -2 -22 3.60 11.70 0 -2 -22 15.30 12.60 0 2 22 18.40 12.60 0 2 22 32.70 12.70 -1 -2 -22 109.79 20.90 1 2 22 162.58 22.10 1 2 22 181.98 21.90 -2 -2 -22 77.99 18.50 2 2 22 97.79 18.00 2 2 22 52.79 15.80 -3 -2 -22 61.59 16.80 3 2 22 68.59 18.90 3 2 22 72.09 16.90 3 -3 -22 6.40 14.80 -3 3 22 -4.90 9.60 2 -3 -22 12.30 15.40 2 -3 -22 -14.90 18.00 -2 3 22 6.00 10.20 -2 3 22 4.50 9.60 1 -3 -22 22.30 14.20 1 -3 -22 27.20 13.50 -1 3 22 2.20 10.40 -1 3 22 16.60 12.50 0 -3 -22 51.99 17.10 0 -3 -22 73.79 17.00 0 3 22 65.69 14.90 0 3 22 82.29 15.30 -1 -3 -22 25.20 15.70 1 3 22 36.40 14.30 1 3 22 59.49 15.70 -2 -3 -22 10.60 13.60 2 3 22 -8.70 11.60 2 3 22 9.60 12.20 1 -4 -22 1.40 14.30 1 -4 -22 43.30 15.10 -1 4 22 9.80 13.00 -1 4 22 24.60 11.80 0 -4 -22 8.90 13.20 0 -4 -22 10.00 14.30 0 4 22 25.10 13.80 0 4 22 -3.70 11.20 1 4 22 5.90 10.80 1 4 22 30.70 13.20 1 2 -23 110.49 20.40 0 2 -23 48.10 15.50 0 2 -23 29.00 15.60 0 -2 23 64.09 15.10 -1 2 -23 110.59 19.20 1 -2 23 97.89 19.80 2 1 -23 51.99 15.90 1 1 -23 114.29 21.50 -1 -1 23 97.49 17.60 0 1 -23 23.50 14.30 0 1 -23 8.00 11.80 0 -1 23 25.60 12.20 -1 1 -23 91.69 17.50 -1 1 -23 68.29 17.80 1 -1 23 75.59 17.50 2 0 -23 -21.50 8.70 -2 0 23 3.70 10.60 1 0 -23 237.48 28.80 1 0 -23 261.97 29.50 -1 0 23 236.18 25.20 0 0 -23 -2.10 11.60 0 0 -23 -0.70 13.00 0 0 23 3.90 10.90 -1 0 -23 273.77 33.80 -1 0 -23 234.88 30.70 1 0 23 288.57 30.20 -2 0 -23 16.40 14.70 2 0 23 1.50 13.10 2 -1 -23 46.30 16.60 -2 1 23 29.20 12.40 1 -1 -23 87.49 19.90 1 -1 -23 127.69 21.90 -1 1 23 108.09 17.60 -1 1 23 115.49 16.40 0 -1 -23 29.90 13.70 0 -1 -23 9.00 12.00 0 1 23 19.50 11.60 -1 -1 -23 104.89 20.60 1 1 23 84.19 17.50 1 -2 -23 104.29 21.90 -1 2 23 162.68 19.60 0 -2 -23 35.10 16.70 0 -2 -23 27.40 15.20 0 2 23 23.30 12.90 0 2 23 64.59 14.80 1 2 23 99.19 18.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 54772 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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 Br01 Br 0.09898(4) 0.70320(3) 0.44257(2) 0.05703(13) Uani 1 1 d . . . . . O002 O 0.2869(2) 0.2776(2) 0.12586(13) 0.0590(6) Uani 1 1 d . . . . . O003 O 0.1778(2) 0.0975(2) 0.22722(11) 0.0477(5) Uani 1 1 d . . . . . N004 N 0.1201(2) 0.2985(2) 0.27036(12) 0.0384(5) Uani 1 1 d . . . . . N005 N 0.3776(2) 0.1130(2) 0.33577(13) 0.0393(5) Uani 1 1 d . . . . . O1 O 0.3686(3) 0.1036(3) 0.08102(13) 0.0772(8) Uani 1 1 d . . . . . N1 N 0.3623(3) 0.1856(3) 0.12665(14) 0.0515(7) Uani 1 1 d . . . . . C008 C 0.3326(3) 0.2264(3) 0.29738(15) 0.0375(6) Uani 1 1 d . . . . . C009 C 0.5728(3) 0.2740(3) 0.28152(17) 0.0441(7) Uani 1 1 d . . . . . H009 H 0.633473 0.336080 0.267279 0.053 Uiso 1 1 calc R U . . . C00A C 0.3022(3) 0.0224(3) 0.36947(18) 0.0459(7) Uani 1 1 d . . . . . H00A H 0.212594 0.009563 0.363240 0.055 Uiso 1 1 calc R U . . . C00B C 0.2946(3) 0.3415(3) 0.34155(15) 0.0359(6) Uani 1 1 d . . . . . C00C C 0.2018(3) 0.1956(3) 0.26006(14) 0.0385(6) Uani 1 1 d . . . . . C00D C 0.1096(3) 0.4915(3) 0.34824(14) 0.0397(6) Uani 1 1 d . . . . . H00D H 0.028139 0.520212 0.332680 0.048 Uiso 1 1 calc R U . . . C00E C 0.5052(3) 0.1046(3) 0.36033(16) 0.0380(6) Uani 1 1 d . . . . . C00F C 0.6040(3) 0.1943(3) 0.33379(15) 0.0394(6) Uani 1 1 d . . . . . C00G C 0.1772(3) 0.5547(3) 0.40088(15) 0.0404(7) Uani 1 1 d . . . . . C00H C 0.4413(3) 0.2658(3) 0.24483(16) 0.0412(7) Uani 1 1 d . . . . . H00H H 0.419996 0.351973 0.226178 0.049 Uiso 1 1 calc R U . . . C00I C 0.3573(3) 0.4048(3) 0.39462(16) 0.0441(7) Uani 1 1 d . . . . . H00I H 0.438590 0.375899 0.410251 0.053 Uiso 1 1 calc R U . . . C00J C 0.7341(3) 0.1942(3) 0.36897(16) 0.0413(6) Uani 1 1 d . . . . . C00K C 0.2975(3) 0.5134(3) 0.42495(16) 0.0469(8) Uani 1 1 d . . . . . H00K H 0.338656 0.557196 0.461016 0.056 Uiso 1 1 calc R U . . . C00L C 0.1706(3) 0.3839(3) 0.32053(14) 0.0362(6) Uani 1 1 d . . . . . C00M C 0.3805(3) -0.0452(3) 0.41342(17) 0.0498(8) Uani 1 1 d . . . . . H00M H 0.354448 -0.113508 0.441834 0.060 Uiso 1 1 calc R U . . . C00N C 0.5081(3) 0.0066(3) 0.40834(19) 0.0449(7) Uani 1 1 d . . . . . H00N H 0.581297 -0.020784 0.433143 0.054 Uiso 1 1 calc R U . . . C00O C 0.8124(3) 0.0839(3) 0.3686(2) 0.0517(8) Uani 1 1 d . . . . . H00O H 0.784180 0.009705 0.345369 0.062 Uiso 1 1 calc R U . . . C00P C 0.4587(3) 0.1717(3) 0.18464(17) 0.0487(8) Uani 1 1 d . . . . . H00B H 0.546405 0.182907 0.166044 0.058 Uiso 1 1 calc R U . . . H00C H 0.452798 0.083549 0.202418 0.058 Uiso 1 1 calc R U . . . C00Q C -0.0113(3) 0.3065(4) 0.24116(17) 0.0503(8) Uani 1 1 d . . . . . H00E H -0.012391 0.264974 0.196688 0.075 Uiso 1 1 calc R U . . . H00F H -0.035915 0.396190 0.236173 0.075 Uiso 1 1 calc R U . . . H00G H -0.072361 0.263526 0.271336 0.075 Uiso 1 1 calc R U . . . C00R C 0.9317(3) 0.0832(4) 0.4022(2) 0.0647(10) Uani 1 1 d . . . . . H00R H 0.982817 0.008161 0.401884 0.078 Uiso 1 1 calc R U . . . C00S C 0.7784(3) 0.3034(4) 0.40401(18) 0.0542(8) Uani 1 1 d . . . . . H00S H 0.727265 0.378421 0.404967 0.065 Uiso 1 1 calc R U . . . C00T C 0.9757(3) 0.1912(5) 0.43600(19) 0.0690(11) Uani 1 1 d . . . . . H00T H 1.057171 0.190629 0.457773 0.083 Uiso 1 1 calc R U . . . C00U C 0.8984(4) 0.3013(5) 0.43757(19) 0.0708(11) Uani 1 1 d . . . . . H00U H 0.927049 0.374711 0.461343 0.085 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 Br01 0.0860(3) 0.04028(17) 0.04476(18) -0.00409(15) 0.00619(17) 0.00630(18) O002 0.0676(15) 0.0468(14) 0.0627(14) 0.0079(12) -0.0053(12) 0.0050(13) O003 0.0494(12) 0.0367(11) 0.0569(13) -0.0087(10) -0.0027(10) -0.0070(10) N004 0.0360(12) 0.0357(11) 0.0436(12) -0.0040(11) -0.0077(10) 0.0017(12) N005 0.0341(13) 0.0342(12) 0.0495(14) 0.0082(11) 0.0031(11) 0.0002(10) O1 0.119(2) 0.0565(16) 0.0559(14) -0.0098(13) -0.0062(15) 0.0063(16) N1 0.0686(18) 0.0382(15) 0.0476(15) 0.0068(13) 0.0064(13) -0.0076(14) C008 0.0332(14) 0.0337(15) 0.0456(15) 0.0020(12) -0.0010(12) -0.0020(12) C009 0.0368(16) 0.0404(17) 0.0553(18) 0.0078(14) 0.0062(13) -0.0055(13) C00A 0.0373(16) 0.0408(16) 0.060(2) 0.0052(15) 0.0064(15) -0.0074(14) C00B 0.0337(14) 0.0331(14) 0.0409(15) 0.0046(12) -0.0012(13) -0.0010(11) C00C 0.0402(14) 0.0351(14) 0.0404(14) 0.0033(14) 0.0002(12) -0.0033(14) C00D 0.0418(15) 0.0370(15) 0.0403(15) 0.0044(12) -0.0033(14) 0.0020(13) C00E 0.0337(14) 0.0317(15) 0.0486(17) 0.0018(13) 0.0010(12) 0.0017(12) C00F 0.0338(13) 0.0331(13) 0.0512(16) 0.0000(13) 0.0056(13) 0.0012(14) C00G 0.0524(18) 0.0318(15) 0.0369(15) 0.0035(12) 0.0043(14) -0.0023(12) C00H 0.0422(16) 0.0347(15) 0.0467(17) 0.0070(13) 0.0038(13) 0.0007(12) C00I 0.0402(16) 0.0461(17) 0.0459(17) 0.0026(14) -0.0061(13) -0.0007(14) C00J 0.0338(14) 0.0420(16) 0.0482(16) 0.0008(15) 0.0070(12) -0.0033(13) C00K 0.0559(19) 0.0454(17) 0.0395(17) -0.0038(13) -0.0079(14) -0.0061(15) C00L 0.0389(15) 0.0331(14) 0.0366(15) 0.0019(12) -0.0020(12) -0.0032(12) C00M 0.054(2) 0.0381(16) 0.0569(19) 0.0146(14) 0.0084(17) -0.0030(15) C00N 0.0433(16) 0.0382(17) 0.0532(18) 0.0078(14) 0.0040(14) 0.0033(13) C00O 0.0401(17) 0.0470(18) 0.068(2) -0.0009(16) 0.0054(16) 0.0010(15) C00P 0.0527(18) 0.0445(18) 0.0489(18) 0.0041(14) 0.0056(15) 0.0061(14) C00Q 0.0434(16) 0.0541(19) 0.0532(18) -0.0092(17) -0.0132(14) 0.0064(16) C00R 0.0408(19) 0.073(3) 0.080(3) 0.017(2) 0.0031(18) 0.0044(18) C00S 0.0495(18) 0.0496(18) 0.063(2) -0.0062(19) 0.0059(16) -0.0055(18) C00T 0.0401(18) 0.109(3) 0.058(2) 0.013(3) -0.0030(16) -0.010(2) C00U 0.065(2) 0.090(3) 0.057(2) -0.017(2) 0.0029(19) -0.031(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' O O 0.0106 0.0060 '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 C00C N004 C00L 111.2(2) . . ? C00C N004 C00Q 123.4(3) . . ? C00L N004 C00Q 124.7(2) . . ? C00A N005 C00E 108.6(2) . . ? C00A N005 C008 127.5(2) . . ? C00E N005 C008 121.4(2) . . ? O002 N1 O1 124.0(3) . . ? O002 N1 C00P 119.8(3) . . ? O1 N1 C00P 116.1(3) . . ? N005 C008 C00B 114.8(2) . . ? N005 C008 C00C 110.2(2) . . ? C00B C008 C00C 101.8(2) . . ? N005 C008 C00H 108.5(2) . . ? C00B C008 C00H 110.4(2) . . ? C00C C008 C00H 111.2(2) . . ? C00F C009 C00H 121.9(3) . . ? C00M C00A N005 108.4(3) . . ? C00I C00B C00L 119.4(3) . . ? C00I C00B C008 132.5(3) . . ? C00L C00B C008 108.1(2) . . ? O003 C00C N004 126.8(3) . . ? O003 C00C C008 125.9(3) . . ? N004 C00C C008 107.4(2) . . ? C00L C00D C00G 115.9(3) . . ? C00N C00E N005 107.4(3) . . ? C00N C00E C00F 133.5(3) . . ? N005 C00E C00F 119.1(3) . . ? C009 C00F C00E 119.3(3) . . ? C009 C00F C00J 123.8(3) . . ? C00E C00F C00J 116.9(3) . . ? C00K C00G C00D 123.0(3) . . ? C00K C00G Br01 118.5(2) . . ? C00D C00G Br01 118.6(2) . . ? C009 C00H C00P 106.8(2) . . ? C009 C00H C008 109.7(2) . . ? C00P C00H C008 114.6(2) . . ? C00B C00I C00K 119.3(3) . . ? C00O C00J C00S 118.5(3) . . ? C00O C00J C00F 120.7(3) . . ? C00S C00J C00F 120.8(3) . . ? C00G C00K C00I 119.4(3) . . ? C00D C00L C00B 123.0(3) . . ? C00D C00L N004 127.2(3) . . ? C00B C00L N004 109.7(2) . . ? C00A C00M C00N 107.7(3) . . ? C00E C00N C00M 107.8(3) . . ? C00R C00O C00J 120.6(3) . . ? N1 C00P C00H 115.8(3) . . ? C00T C00R C00O 120.8(4) . . ? C00U C00S C00J 120.3(4) . . ? C00R C00T C00U 119.4(3) . . ? C00T C00U C00S 120.5(4) . . ? 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 Br01 C00G 1.901(3) . ? O002 N1 1.217(3) . ? O003 C00C 1.216(4) . ? N004 C00C 1.360(4) . ? N004 C00L 1.406(4) . ? N004 C00Q 1.454(4) . ? N005 C00A 1.371(4) . ? N005 C00E 1.386(4) . ? N005 C008 1.456(4) . ? O1 N1 1.222(4) . ? N1 C00P 1.497(4) . ? C008 C00B 1.509(4) . ? C008 C00C 1.548(4) . ? C008 C00H 1.556(4) . ? C009 C00F 1.339(4) . ? C009 C00H 1.518(4) . ? C00A C00M 1.356(5) . ? C00B C00I 1.372(4) . ? C00B C00L 1.396(4) . ? C00D C00L 1.377(4) . ? C00D C00G 1.390(4) . ? C00E C00N 1.369(4) . ? C00E C00F 1.458(4) . ? C00F C00J 1.489(4) . ? C00G C00K 1.378(5) . ? C00H C00P 1.524(4) . ? C00I C00K 1.399(5) . ? C00J C00O 1.385(4) . ? C00J C00S 1.386(5) . ? C00M C00N 1.408(5) . ? C00O C00R 1.379(5) . ? C00R C00T 1.363(6) . ? C00S C00U 1.383(5) . ? C00T C00U 1.379(6) . ?