#------------------------------------------------------------------------------ #$Date: 2023-09-16 00:55:12 +0300 (Sat, 16 Sep 2023) $ #$Revision: 286356 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/13/21/7132139.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_7132139 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 monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _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 107.102(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.7574(7) _cell_length_b 13.9180(14) _cell_length_c 9.8197(9) _cell_measurement_reflns_used 6939 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 27.56 _cell_measurement_theta_min 3.11 _cell_volume 1013.33(17) _computing_structure_refinement 'SHELXL-2019/1 (Sheldrick, 2019)' _diffrn_ambient_temperature 297(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _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 0.0209 _diffrn_reflns_av_unetI/netI 0.0400 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 9275 _diffrn_reflns_point_group_measured_fraction_full 0.956 _diffrn_reflns_point_group_measured_fraction_max 0.956 _diffrn_reflns_theta_full 24.493 _diffrn_reflns_theta_max 24.493 _diffrn_reflns_theta_min 2.617 _exptl_absorpt_coefficient_mu 2.059 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.5727 _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 1.522 _exptl_crystal_description Block _exptl_crystal_F_000 472 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _refine_diff_density_max 0.213 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.033 _refine_ls_abs_structure_details ; Flack x determined using 1300 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.040(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.709 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 272 _refine_ls_number_reflns 3224 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.708 _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_gt 0.0234 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.8063P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.0570 _reflns_Friedel_coverage 0.844 _reflns_Friedel_fraction_full 0.917 _reflns_Friedel_fraction_max 0.917 _reflns_number_gt 3025 _reflns_number_total 3224 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3cc03713d2.cif _cod_data_source_block LNE_APNBS_mono_Br _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 7132139 _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 LNE_APNBS_mono_Br.res in P2(1) LNE_APNBS_mono_Br.res created by SHELXL-2019/1 at 12:24:36 on 22-Jul-2023 CELL 0.71073 7.7574 13.9180 9.8197 90.000 107.102 90.000 ZERR 2.000 0.0007 0.0014 0.0009 0.000 0.003 0.000 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C H N O Br UNIT 46 36 6 6 2 OMIT -3 49 L.S. 10 ACTA BOND FMAP 2 PLAN 20 TEMP 23.850 WGHT 0.030400 0.806308 FVAR 1.31506 BR01 5 0.806297 0.370788 0.769999 11.00000 0.06425 0.03612 = 0.04994 -0.00044 -0.00994 0.01307 O002 4 0.034153 0.456829 0.468541 11.00000 0.03710 0.06500 = 0.05503 -0.01082 0.01984 -0.00928 N003 3 0.350265 0.588749 0.559525 11.00000 0.03549 0.02991 = 0.02957 -0.00383 0.00845 0.00192 N004 3 0.150592 0.431290 0.281860 11.00000 0.03573 0.03682 = 0.03348 -0.00476 0.00483 -0.00524 C005 1 0.590314 0.536628 0.353510 11.00000 0.04284 0.04073 = 0.03179 0.00122 0.00947 -0.00232 AFIX 43 H005 2 0.670736 0.567381 0.430352 11.00000 -1.20000 AFIX 0 C006 1 0.627106 0.463571 0.688852 11.00000 0.03986 0.02913 = 0.02617 0.00043 0.00614 0.00108 C007 1 0.428671 0.501235 0.363950 11.00000 0.03494 0.02882 = 0.02618 0.00102 0.00608 0.00351 C008 1 0.477656 0.718565 0.678270 11.00000 0.04948 0.02673 = 0.04662 -0.00637 0.01907 -0.00599 AFIX 43 H008 2 0.558225 0.759672 0.740281 11.00000 -1.20000 AFIX 0 C009 1 0.838702 0.628348 0.950342 11.00000 0.04485 0.03835 = 0.03715 -0.00636 0.01716 -0.00582 AFIX 43 H009 2 0.735971 0.630858 0.980700 11.00000 -1.20000 AFIX 0 C00A 1 0.307728 0.743551 0.587737 11.00000 0.05840 0.03063 = 0.05272 0.00378 0.02475 0.00993 AFIX 43 H00A 2 0.255175 0.804154 0.579629 11.00000 -1.20000 AFIX 0 C00B 1 0.450931 0.421565 0.599003 11.00000 0.03890 0.02658 = 0.02454 -0.00058 0.00938 -0.00218 AFIX 13 H00B 2 0.478243 0.366084 0.547461 11.00000 -1.20000 AFIX 0 O1 4 0.228715 0.262848 0.531496 11.00000 0.08766 0.04833 = 0.08948 -0.01543 0.02285 -0.02185 C00D 1 0.652124 0.557319 0.720188 11.00000 0.03376 0.03276 = 0.02480 -0.00065 0.01335 -0.00191 C00E 1 0.233374 0.664363 0.514222 11.00000 0.04289 0.03983 = 0.03952 0.00777 0.01236 0.00890 AFIX 43 H00E 2 0.122128 0.661469 0.444820 11.00000 -1.20000 AFIX 0 C00F 1 0.155849 0.460932 0.414480 11.00000 0.03705 0.03606 = 0.03399 -0.00236 0.00698 -0.00294 C00G 1 1.003102 0.657172 1.041100 11.00000 0.05470 0.04381 = 0.02921 -0.00632 0.00812 -0.00483 AFIX 43 H00G 2 1.010693 0.677786 1.132769 11.00000 -1.20000 AFIX 0 N1 3 0.242869 0.294720 0.649685 11.00000 0.05071 0.04292 = 0.07479 0.01869 0.02498 -0.00045 C00I 1 0.347262 0.385746 0.699394 11.00000 0.06193 0.04048 = 0.03546 0.00189 0.01616 -0.00922 AFIX 23 H00C 2 0.431907 0.374690 0.792729 11.00000 -1.20000 H00D 2 0.264156 0.435483 0.709252 11.00000 -1.20000 AFIX 0 C00J 1 0.630203 0.525261 0.225476 11.00000 0.04877 0.05625 = 0.04203 0.00854 0.02116 0.00219 AFIX 43 H00J 2 0.737727 0.549421 0.215731 11.00000 -1.20000 AFIX 0 C00K 1 0.979381 0.596195 0.769109 11.00000 0.04227 0.04844 = 0.03479 -0.00407 0.01829 0.00081 AFIX 43 H00K 2 0.971972 0.576438 0.677088 11.00000 -1.20000 AFIX 0 C00L 1 0.349917 0.497543 0.487207 11.00000 0.03324 0.03015 = 0.02794 -0.00297 0.00836 -0.00182 C00M 1 0.504313 0.622158 0.659137 11.00000 0.03499 0.02955 = 0.03131 0.00038 0.01257 -0.00240 C00N 1 0.309328 0.456312 0.248074 11.00000 0.03996 0.02745 = 0.03096 0.00259 0.00638 0.00600 C00O 1 -0.000353 0.380347 0.186691 11.00000 0.04559 0.05939 = 0.05090 -0.01752 0.00110 -0.01251 AFIX 137 H00F 2 0.038036 0.317521 0.167537 11.00000 -1.50000 H00H 2 -0.043683 0.415343 0.098992 11.00000 -1.50000 H00I 2 -0.095324 0.374458 0.230551 11.00000 -1.50000 AFIX 0 C00P 1 0.826237 0.595814 0.814693 11.00000 0.03707 0.02749 = 0.02882 -0.00116 0.00667 -0.00130 C00Q 1 1.155145 0.655528 0.996650 11.00000 0.03965 0.03633 = 0.04863 -0.00723 -0.00155 -0.00134 AFIX 43 H00Q 2 1.265798 0.674297 1.058154 11.00000 -1.20000 AFIX 0 O00R 4 0.177347 0.257610 0.733527 11.00000 0.10939 0.08241 = 0.12954 0.02834 0.07210 -0.02050 C00S 1 0.347270 0.442890 0.121222 11.00000 0.05820 0.04209 = 0.02707 -0.00283 0.00702 0.00392 AFIX 43 H00S 2 0.267252 0.411619 0.044713 11.00000 -1.20000 AFIX 0 C00T 1 1.142432 0.625744 0.859704 11.00000 0.03557 0.04917 = 0.05640 -0.00014 0.01691 0.00165 AFIX 43 H00T 2 1.244627 0.625654 0.828532 11.00000 -1.20000 AFIX 0 C00U 1 0.511719 0.478533 0.113177 11.00000 0.06329 0.05875 = 0.03808 0.00157 0.02521 0.00824 AFIX 43 H00U 2 0.542309 0.470454 0.029152 11.00000 -1.20000 AFIX 0 HKLF 4 REM LNE_APNBS_mono_Br.res in P2(1) REM wR2 = 0.0570, GooF = S = 0.709, Restrained GooF = 0.708 for all data REM R1 = 0.0234 for 3025 Fo > 4sig(Fo) and 0.0257 for all 3224 data REM 272 parameters refined using 1 restraints END WGHT 0.0209 0.0618 REM Highest difference peak 0.213, deepest hole -0.487, 1-sigma level 0.033 Q1 1 0.0233 0.6613 0.4242 11.00000 0.05 0.21 Q2 1 0.6947 0.3792 0.7871 11.00000 0.05 0.17 Q3 1 0.6923 0.4220 0.7205 11.00000 0.05 0.16 Q4 1 0.6978 0.3260 0.7282 11.00000 0.05 0.16 Q5 1 0.3111 0.2670 0.8272 11.00000 0.05 0.14 Q6 1 0.3566 0.2931 0.8574 11.00000 0.05 0.14 Q7 1 0.9773 0.5795 0.5800 11.00000 0.05 0.13 Q8 1 0.6999 0.3679 0.6684 11.00000 0.05 0.13 Q9 1 0.6782 0.5099 0.6922 11.00000 0.05 0.12 Q10 1 0.4004 0.4428 0.3241 11.00000 0.05 0.12 Q11 1 0.3451 0.4147 0.1995 11.00000 0.05 0.11 Q12 1 0.4258 0.6006 0.6148 11.00000 0.05 0.11 Q13 1 0.4508 0.3675 0.5792 11.00000 0.05 0.11 Q14 1 0.6601 0.7602 0.9141 11.00000 0.05 0.11 Q15 1 0.3208 0.4413 0.7753 11.00000 0.05 0.11 Q16 1 0.5347 0.4869 0.3836 11.00000 0.05 0.11 Q17 1 0.5094 0.6776 0.6416 11.00000 0.05 0.11 Q18 1 0.4108 0.4017 0.6579 11.00000 0.05 0.11 Q19 1 0.3806 0.7364 0.6713 11.00000 0.05 0.10 Q20 1 1.1129 0.5582 1.0242 11.00000 0.05 0.10 ; _shelx_res_checksum 62599 _shelx_hkl_file ; 1 0 0 6.20 1.20 1 0 0 7.60 1.30 1 0 0 4.50 1.00 1 0 0 6.70 1.10 -1 0 0 4.80 1.00 -1 0 0 4.90 1.10 -1 0 0 6.60 1.20 -2 0 0 4109.49 239.78 2 0 0 4260.07 239.88 2 0 0 4339.67 239.88 2 0 0 4270.77 239.68 -2 0 0 4407.56 239.68 2 0 0 4203.08 239.68 -2 0 0 4216.18 239.98 -3 0 0 1781.72 100.19 3 0 0 1697.43 100.69 3 0 0 1774.52 101.39 3 0 0 1724.53 100.49 3 0 0 1816.42 100.29 3 0 0 1751.12 100.29 -3 0 0 1804.12 101.19 -3 0 0 1708.03 100.89 4 0 0 16.80 3.70 4 0 0 18.40 4.90 4 0 0 23.60 4.00 -4 0 0 22.30 4.80 -4 0 0 26.10 4.30 -4 0 0 23.20 4.60 -5 0 0 2566.04 147.99 -5 0 0 2621.84 148.99 5 0 0 2517.05 148.19 5 0 0 2605.54 147.29 6 0 0 2370.76 137.29 6 0 0 2492.35 139.89 -6 0 0 2407.46 139.59 6 0 0 2286.67 138.49 7 0 0 58.09 11.50 -7 0 0 29.50 9.80 7 0 0 38.10 10.20 -8 0 0 -1.60 8.70 8 0 0 -0.20 10.40 8 0 0 3.40 9.50 -9 0 0 -3.30 11.70 9 0 0 -2.60 12.20 2 -1 0 992.60 57.69 2 -1 0 965.90 58.09 2 -1 0 1020.70 57.59 -2 -1 0 975.30 57.89 2 -1 0 1018.10 57.69 -2 -1 0 963.50 57.69 -2 -1 0 1029.90 58.09 2 -1 0 1036.60 58.29 -2 1 0 1016.50 58.19 -2 1 0 1025.00 57.59 2 1 0 1009.60 58.09 -2 1 0 1029.10 58.19 2 1 0 1038.00 57.89 2 1 0 1007.30 57.99 2 1 0 988.50 57.99 -3 -1 0 673.43 40.30 3 -1 0 652.33 40.20 -3 -1 0 634.34 39.90 3 -1 0 675.43 40.40 -3 -1 0 641.44 39.70 3 -1 0 633.84 39.60 3 -1 0 630.44 39.60 3 1 0 686.23 40.20 -3 1 0 682.23 39.70 -3 1 0 702.43 39.70 -3 1 0 737.73 40.70 3 1 0 679.43 40.00 3 1 0 708.83 39.60 3 1 0 680.13 39.70 3 1 0 681.33 40.10 4 -1 0 1485.75 94.29 4 -1 0 1499.25 93.49 4 -1 0 1551.24 94.59 -4 -1 0 1525.75 94.49 4 -1 0 1489.55 93.69 4 -1 0 1614.84 93.69 -4 -1 0 1561.24 93.99 -4 1 0 1719.93 93.69 -4 1 0 1757.22 93.99 4 1 0 1760.12 93.59 4 1 0 1743.33 94.59 4 1 0 1670.63 95.29 -4 1 0 1774.72 94.99 5 -1 0 60.79 7.80 -5 -1 0 65.59 8.40 -5 -1 0 66.59 8.90 5 -1 0 55.09 8.50 5 -1 0 58.19 7.90 5 -1 0 53.49 7.00 5 1 0 34.50 6.40 -5 1 0 50.19 7.20 -5 1 0 52.99 8.40 5 1 0 40.50 7.50 5 1 0 46.70 6.60 6 -1 0 525.65 36.00 -6 -1 0 526.65 37.50 6 -1 0 515.35 34.80 -6 -1 0 510.55 36.90 6 -1 0 472.65 36.50 6 1 0 591.04 39.20 6 1 0 610.34 35.00 -6 1 0 640.54 37.90 -7 -1 0 50.89 11.40 7 -1 0 55.09 11.40 7 -1 0 48.10 10.10 7 1 0 30.60 10.30 -7 1 0 23.00 8.80 -8 -1 0 1.10 10.10 8 -1 0 27.70 11.30 8 -1 0 16.40 10.50 -8 1 0 23.60 10.70 8 1 0 29.20 11.50 8 1 0 25.20 11.40 9 -1 0 111.09 17.90 9 -1 0 89.89 18.10 -9 -1 0 95.39 18.30 9 1 0 94.49 17.90 -9 1 0 120.49 18.70 9 1 0 105.59 18.80 1 -2 0 3256.17 175.08 1 -2 0 3313.27 175.78 -1 -2 0 3256.27 175.78 -1 -2 0 3240.08 175.78 1 -2 0 3384.96 175.98 1 2 0 2903.01 175.58 1 2 0 2900.91 175.68 -1 2 0 2972.30 175.08 -1 2 0 2874.11 175.68 -2 -2 0 5283.97 278.47 2 -2 0 5428.36 278.07 -2 -2 0 5430.06 278.77 2 -2 0 5205.78 278.97 2 -2 0 5445.76 279.07 2 -2 0 5342.97 278.47 -2 -2 0 5423.06 278.77 2 -2 0 5261.57 277.97 2 2 0 4489.95 278.57 2 2 0 4366.06 278.57 -2 2 0 4525.45 277.87 2 2 0 4539.45 278.07 -2 2 0 4580.04 278.67 -2 2 0 4455.95 278.27 -2 2 0 4454.35 278.67 -3 -2 0 3092.29 166.88 3 -2 0 2997.70 166.58 3 -2 0 2972.30 166.38 3 -2 0 3059.99 167.58 -3 -2 0 3078.19 167.18 3 2 0 2440.56 167.48 4 -2 0 2139.29 117.89 4 -2 0 2071.29 117.59 4 -2 0 2080.99 116.49 -4 -2 0 2079.99 117.19 -4 -2 0 2118.29 117.59 -4 -2 0 2084.69 116.79 4 -2 0 1975.40 117.29 4 -2 0 2054.99 116.39 -4 2 0 2002.30 116.59 4 2 0 1891.91 117.09 4 2 0 1974.60 116.59 4 2 0 1981.50 116.19 -4 2 0 1983.70 117.39 -5 -2 0 757.32 49.50 5 -2 0 799.52 49.20 5 -2 0 757.92 48.90 5 -2 0 763.42 48.50 -5 -2 0 824.12 50.49 5 -2 0 806.32 50.59 5 2 0 836.62 50.29 5 2 0 791.52 48.90 -5 2 0 845.82 49.00 -5 2 0 847.62 50.49 5 2 0 890.51 48.90 6 -2 0 142.29 14.70 6 -2 0 145.69 13.90 -6 -2 0 138.69 15.50 6 -2 0 150.88 16.30 -6 -2 0 136.89 15.80 6 2 0 194.08 17.60 -6 2 0 200.68 17.20 7 -2 0 57.29 12.40 -7 -2 0 65.39 12.30 7 -2 0 72.59 11.40 7 2 0 65.19 12.50 -7 2 0 76.59 12.70 -8 -2 0 186.18 23.90 8 -2 0 196.78 24.10 8 -2 0 204.98 22.00 8 2 0 190.98 23.60 -8 2 0 187.88 23.30 -9 -2 0 4.90 12.20 9 -2 0 9.90 12.70 9 2 0 -5.20 13.30 -9 2 0 4.60 13.00 9 2 0 -10.20 11.40 0 -3 0 2.30 1.20 0 -3 0 5.50 1.50 0 -3 0 0.80 0.90 0 3 0 -0.30 1.10 0 3 0 6.30 1.50 0 3 0 0.70 0.80 1 3 0 607.84 35.10 1 3 0 635.04 35.10 -1 3 0 582.84 35.30 -1 3 0 584.44 34.00 2 -3 0 4262.47 242.68 -2 -3 0 4301.47 242.88 2 -3 0 4224.88 241.88 -2 -3 0 4256.47 242.78 2 -3 0 4252.87 241.88 -2 -3 0 4345.97 242.98 2 -3 0 4185.08 243.18 2 -3 0 4382.26 243.38 2 3 0 4377.06 242.68 -2 3 0 4434.96 241.98 -2 3 0 4302.37 242.88 2 3 0 4310.87 242.98 2 3 0 4327.07 242.58 -2 3 0 4336.77 243.28 3 -3 0 1953.40 117.99 3 -3 0 2063.49 116.59 3 -3 0 1991.10 117.09 -3 -3 0 1987.30 117.29 3 -3 0 2011.80 117.89 -3 -3 0 2055.19 117.59 -3 -3 0 2026.80 117.69 3 -3 0 1916.31 116.39 3 3 0 2229.68 117.19 -3 3 0 2154.68 118.09 3 3 0 2210.48 118.09 -4 -3 0 1703.33 100.29 4 -3 0 1610.84 100.49 4 -3 0 1564.94 98.99 4 -3 0 1662.73 100.69 -4 -3 0 1683.63 100.49 4 -3 0 1692.43 99.59 -4 -3 0 1645.44 99.79 4 -3 0 1661.63 99.09 4 3 0 1807.72 99.59 4 3 0 1798.22 100.69 -4 3 0 1891.31 101.09 4 3 0 1821.62 99.39 -4 3 0 1877.31 100.09 4 3 0 1797.72 100.09 5 -3 0 34.00 7.40 -5 -3 0 33.40 6.80 5 -3 0 42.00 6.50 -5 -3 0 35.90 7.10 5 -3 0 29.30 5.30 -5 -3 0 28.00 5.60 5 3 0 14.20 6.80 -5 3 0 32.80 6.40 5 3 0 17.80 5.00 -5 3 0 31.60 7.20 5 3 0 27.80 5.50 6 -3 0 414.56 31.60 6 -3 0 410.86 29.50 -6 -3 0 404.96 30.90 -6 -3 0 425.06 31.00 6 -3 0 424.66 29.80 6 3 0 470.05 28.90 6 3 0 449.66 31.80 -6 3 0 466.95 29.90 -6 3 0 495.15 32.30 7 -3 0 464.85 35.40 -7 -3 0 456.35 33.70 7 -3 0 469.45 34.70 -7 -3 0 427.86 33.90 8 -3 0 40.70 12.80 8 -3 0 43.70 11.50 -8 -3 0 51.89 13.80 -8 3 0 42.50 13.30 8 3 0 32.70 13.10 -9 -3 0 94.79 17.50 9 -3 0 96.39 17.50 9 3 0 74.39 17.20 9 3 0 85.39 17.40 0 -4 0 4971.20 283.77 0 -4 0 5111.59 282.87 -1 -4 0 7440.56 411.26 1 4 0 6805.42 410.76 1 4 0 7378.26 410.96 -1 4 0 7648.53 411.56 2 -4 0 1667.23 93.99 2 -4 0 1536.15 93.19 2 -4 0 1595.84 91.99 2 -4 0 1636.54 91.99 2 -4 0 1683.63 93.79 -2 -4 0 1672.23 93.49 3 -4 0 3101.09 178.68 3 -4 0 3061.79 178.78 3 -4 0 3090.29 176.78 -3 -4 0 3075.09 178.18 3 -4 0 2987.80 176.78 3 -4 0 3047.00 177.78 -3 -4 0 3174.18 178.28 -3 -4 0 3058.09 177.98 3 4 0 3179.08 177.68 -3 4 0 3336.27 178.38 -3 4 0 3141.19 178.68 3 4 0 3183.38 178.58 3 4 0 3316.77 177.78 4 -4 0 82.49 10.60 4 -4 0 78.99 9.80 4 -4 0 78.19 8.00 -4 -4 0 75.29 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-8 -10 72.69 14.40 1 -8 10 118.69 18.90 1 8 10 87.19 18.80 2 -8 10 117.19 20.40 -2 -8 -10 121.39 31.10 2 8 10 165.68 25.90 -6 -9 10 50.69 17.90 -6 9 10 47.90 16.70 6 9 -10 39.90 14.70 -5 -9 10 64.19 18.10 -5 9 10 58.09 20.80 -4 -9 10 62.09 15.60 -4 9 10 22.90 13.50 4 9 -10 20.00 12.70 -3 -9 10 8.10 12.70 3 9 -10 -11.80 9.20 -3 9 10 5.10 10.70 -2 -9 10 12.90 13.00 -1 -9 10 10.10 13.20 0 -9 10 193.48 25.50 1 -9 10 49.10 16.00 -1 -9 -10 45.60 12.90 1 9 10 24.20 16.10 -2 -9 -10 102.29 17.70 -5 -10 10 9.20 15.30 -5 10 10 1.70 13.20 5 10 -10 -9.70 12.30 -4 -10 10 175.48 23.80 -4 10 10 161.88 23.40 4 10 -10 114.39 18.90 -3 -10 10 12.70 13.80 -3 10 10 14.10 11.80 3 10 -10 -1.10 11.60 -2 -10 10 66.39 17.10 -1 -10 10 133.49 20.70 0 -10 -10 3.10 10.40 0 -10 10 7.70 13.30 1 -10 10 146.59 22.00 -1 -10 -10 205.28 23.90 -5 -11 10 -1.50 15.30 -5 11 10 29.20 15.70 5 11 -10 -11.80 11.30 -4 -11 10 5.60 14.70 -4 11 10 9.80 14.20 4 11 -10 6.30 12.90 -3 -11 10 56.09 16.60 -3 11 10 54.89 15.10 3 11 -10 48.80 15.90 -2 -11 10 4.10 13.30 -1 -11 10 35.50 15.10 0 -11 10 24.30 14.40 0 -11 -10 2.60 13.80 -3 -12 10 24.00 15.40 -3 12 10 47.80 21.80 3 12 -10 43.70 15.50 -2 -12 10 29.40 15.50 -7 0 11 -25.00 10.80 7 0 -11 7.60 12.10 6 0 -11 -8.10 10.40 -6 0 11 -1.50 10.80 -5 0 11 54.29 16.40 5 0 -11 43.80 12.60 -4 0 11 3.40 9.80 4 0 -11 -2.10 9.10 -3 0 11 57.19 14.90 -2 0 11 8.00 12.20 0 0 11 227.68 27.60 1 0 11 20.80 13.90 2 0 11 157.18 25.50 7 -1 -11 20.50 12.70 -7 -1 11 -0.80 12.40 -7 1 11 8.20 11.30 7 1 -11 8.10 11.70 6 -1 -11 2.00 11.10 -6 -1 11 11.30 12.50 6 1 -11 7.40 11.50 5 -1 -11 18.00 10.70 -5 -1 11 8.80 13.40 -5 1 11 14.90 11.00 5 1 -11 16.30 11.00 -4 -1 11 85.09 16.70 4 -1 -11 44.60 12.60 4 1 -11 61.09 13.30 -4 1 11 72.59 15.00 -3 -1 11 15.30 12.90 -3 1 11 11.30 11.30 -2 -1 11 67.29 18.30 -2 1 11 51.19 14.80 -1 -1 11 61.79 15.70 0 -1 11 4.70 12.80 0 1 11 40.40 15.60 1 -1 11 210.78 26.50 1 1 11 149.79 22.90 2 -1 11 94.09 21.60 2 1 11 85.69 22.00 7 -2 -11 -6.70 12.00 -7 -2 11 24.30 14.00 7 2 -11 15.80 12.90 -6 -2 11 19.60 13.70 6 -2 -11 32.50 13.80 -6 2 11 18.40 12.00 6 2 -11 4.00 11.00 5 -2 -11 12.50 10.40 -5 -2 11 1.00 11.70 5 2 -11 15.10 11.50 -5 2 11 31.20 12.60 -4 -2 11 87.99 23.20 4 -2 -11 69.89 13.80 4 2 -11 59.19 12.90 -4 2 11 77.69 15.40 -3 -2 11 46.80 22.00 -3 2 11 29.20 12.90 -2 2 11 200.68 23.70 -1 -2 11 6.20 11.70 0 -2 11 115.19 19.50 0 2 11 128.79 20.00 1 -2 11 66.99 18.00 1 2 11 53.89 18.10 2 -2 11 115.89 23.40 2 2 11 164.38 25.60 -7 -3 11 1.90 13.60 7 -3 -11 23.40 14.10 7 3 -11 -21.10 9.80 -7 3 11 24.40 13.80 6 -3 -11 16.90 13.60 -6 -3 11 24.10 14.50 6 3 -11 7.90 12.60 -6 3 11 23.80 12.10 -5 -3 11 100.99 18.00 5 -3 -11 55.29 14.30 5 3 -11 59.79 13.70 -5 3 11 73.19 15.50 -5 3 11 66.69 14.10 4 -3 -11 30.30 10.60 -4 -3 11 49.50 14.80 -4 3 11 45.30 12.50 4 3 -11 23.60 10.30 -4 3 11 51.99 13.20 -3 -3 11 16.50 11.60 -3 3 11 9.80 11.20 -2 -3 11 97.79 17.80 -2 3 11 121.59 18.10 -1 -3 11 39.40 14.80 0 -3 11 22.00 12.90 0 3 11 6.60 12.10 1 -3 11 160.98 24.10 1 3 11 199.48 25.70 2 -3 11 92.39 20.50 2 3 11 45.50 19.60 -7 -4 11 11.90 15.70 7 -4 -11 13.00 12.90 -7 4 11 31.80 14.90 7 4 -11 5.70 12.20 6 -4 -11 2.90 12.00 -6 -4 11 -16.40 14.20 -6 4 11 13.30 11.50 6 4 -11 0.90 11.30 -5 -4 11 80.99 18.10 5 -4 -11 57.99 14.70 5 4 -11 28.60 12.50 -5 4 11 51.69 15.40 -5 4 11 52.09 14.40 4 -4 -11 15.90 10.70 -4 -4 11 14.10 13.00 4 4 -11 26.30 11.30 -4 4 11 35.30 11.90 -4 4 11 34.30 11.70 -3 -4 11 47.50 15.00 -3 4 11 67.09 13.80 -2 -4 11 10.80 13.40 -2 4 11 39.50 13.40 -1 -4 11 67.69 15.80 0 -4 11 154.18 23.30 0 4 11 212.68 27.50 1 -4 11 119.99 19.80 1 4 11 93.49 21.10 2 -4 11 5.20 14.80 2 4 11 -11.30 16.00 7 -5 -11 4.00 14.80 -7 -5 11 -8.80 15.40 7 5 -11 -1.10 11.80 -7 5 11 -2.30 13.20 -6 -5 11 3.20 15.00 -6 5 11 19.00 19.60 -5 -5 11 9.50 13.40 5 -5 -11 4.00 11.40 -5 5 11 7.80 11.40 5 5 -11 4.40 10.10 4 -5 -11 28.10 10.60 -4 -5 11 31.40 14.00 -4 5 11 27.70 12.20 4 5 -11 14.80 10.60 -4 5 11 20.00 12.90 -3 -5 11 20.00 14.40 -3 5 11 45.20 13.60 -2 -5 11 120.79 19.50 -2 5 11 183.08 21.80 -1 -5 11 17.90 13.80 0 -5 11 -5.50 13.50 0 5 11 0.30 13.20 1 -5 11 70.29 18.30 1 5 11 98.69 21.30 2 -5 11 13.00 13.80 2 5 11 14.60 18.20 -6 -6 11 44.40 17.50 6 -6 -11 28.60 13.10 6 6 -11 39.40 14.50 -6 6 11 35.70 14.60 -5 -6 11 1.10 14.20 5 -6 -11 -2.20 11.60 5 6 -11 8.20 11.20 -5 6 11 1.30 12.20 -4 -6 11 43.70 15.90 4 -6 -11 17.10 11.50 4 6 -11 25.00 11.50 -4 6 11 34.00 13.00 -3 -6 11 63.39 16.60 -3 6 11 59.49 21.60 -2 -6 11 63.89 16.40 -2 6 11 66.39 13.90 -1 -6 11 64.29 17.40 0 -6 11 42.90 15.90 0 6 11 22.20 14.80 1 -6 11 10.70 14.20 1 6 11 -9.70 14.90 -6 -7 11 11.40 17.60 6 -7 -11 -8.10 12.80 6 7 -11 -10.70 11.00 -6 7 11 0.80 12.70 -5 -7 11 44.80 18.60 5 -7 -11 18.20 14.90 -5 7 11 33.10 14.70 5 7 -11 15.60 13.00 4 -7 -11 113.39 19.40 -4 -7 11 131.19 21.50 -4 7 11 102.59 18.10 4 7 -11 117.79 17.80 -3 -7 11 28.00 15.30 -2 -7 11 104.79 19.90 -1 -7 11 137.19 21.90 -1 7 11 125.79 20.20 0 -7 11 40.90 16.00 0 7 11 30.90 14.10 1 -7 11 112.69 20.40 1 7 11 116.89 23.50 -5 -8 11 36.40 16.70 5 -8 -11 -19.40 12.10 5 8 -11 -1.50 12.20 -5 8 11 -9.90 12.10 4 -8 -11 16.20 14.40 -4 -8 11 25.90 17.20 -4 8 11 21.00 12.40 4 8 -11 6.30 12.00 -3 -8 11 14.00 14.40 -2 -8 11 99.19 19.20 -1 -8 11 47.90 16.30 0 -8 11 114.09 20.10 0 8 11 92.59 18.30 5 -9 -11 -5.90 14.70 -5 -9 11 27.40 17.60 -5 9 11 12.50 13.30 5 9 -11 -14.70 12.60 -4 -9 11 25.50 16.50 -3 -9 11 25.20 15.40 -2 -9 11 18.00 15.40 -1 -9 11 73.99 18.00 0 -9 11 17.40 15.20 -3 -10 11 43.30 17.10 -2 -10 11 16.10 15.80 6 0 -12 39.00 14.80 -6 0 12 54.59 17.30 -5 0 12 10.60 13.40 5 0 -12 -1.10 11.80 -4 0 12 27.40 14.30 -3 0 12 20.40 14.30 -2 0 12 34.80 15.80 -1 0 12 65.59 18.40 0 0 12 5.30 15.20 1 0 12 34.80 20.50 -6 -1 12 2.30 14.20 6 -1 -12 4.30 12.40 -6 1 12 5.90 13.50 6 1 -12 16.50 13.20 -5 -1 12 32.90 16.50 5 -1 -12 10.40 12.60 5 1 -12 36.50 13.60 -5 1 12 51.59 15.80 -4 -1 12 27.70 15.80 -4 1 12 -1.40 12.70 -3 -1 12 49.99 16.80 -3 1 12 43.80 16.00 -2 -1 12 25.90 15.30 -2 1 12 10.80 14.30 -1 -1 12 11.60 15.40 -1 1 12 21.50 14.90 0 -1 12 169.18 25.90 0 1 12 188.18 27.00 1 -1 12 -1.00 19.00 1 1 12 12.10 16.70 -6 -2 12 5.10 15.50 6 -2 -12 10.50 13.20 -6 2 12 -1.90 12.20 6 2 -12 -4.80 12.50 -5 -2 12 19.30 15.30 5 -2 -12 2.20 12.00 5 2 -12 4.90 11.50 -5 2 12 16.80 13.40 -4 -2 12 32.50 15.40 -4 2 12 36.20 13.60 -3 -2 12 32.60 15.70 -3 2 12 31.30 14.80 -2 -2 12 63.99 19.00 -2 2 12 73.19 17.20 -1 -2 12 32.30 17.30 -1 2 12 4.80 15.00 0 -2 12 -7.20 15.30 0 2 12 -0.50 15.60 1 -2 12 93.59 22.20 1 2 12 117.09 23.70 -6 -3 12 127.79 23.00 6 -3 -12 117.69 20.70 6 3 -12 108.69 19.60 -5 -3 12 40.80 16.80 5 -3 -12 7.90 11.70 5 3 -12 7.00 11.00 -5 3 12 8.60 11.30 -4 -3 12 15.10 15.90 -4 3 12 30.70 13.30 -3 -3 12 12.30 15.60 -3 3 12 22.90 13.30 -2 -3 12 141.19 23.60 -2 3 12 129.59 20.70 -1 -3 12 62.29 19.20 -1 3 12 63.89 18.80 0 -3 12 200.68 28.30 0 3 12 248.78 29.40 -6 -4 12 58.19 19.00 6 -4 -12 26.90 16.40 6 4 -12 26.70 14.10 -6 4 12 28.20 13.30 -5 -4 12 25.70 16.00 5 -4 -12 -2.10 12.20 -5 4 12 -8.20 10.40 5 4 -12 -3.80 11.00 -4 -4 12 59.89 18.80 -4 4 12 39.10 13.80 -3 -4 12 -4.90 15.10 -3 4 12 -18.00 10.20 -2 -4 12 11.70 15.90 -2 4 12 28.50 15.20 -1 -4 12 71.49 19.70 -1 4 12 36.70 16.20 0 -4 12 -1.70 15.90 0 4 12 -5.70 14.50 -5 -5 12 10.20 16.20 -4 -5 12 24.60 16.90 -3 -5 12 7.00 15.80 -3 5 12 -1.40 11.60 -2 -5 12 17.60 17.30 -2 5 12 19.10 14.00 -1 -5 12 99.19 22.60 -1 5 12 115.79 21.90 0 -5 12 32.30 17.30 0 5 12 2.50 15.60 5 -6 -12 -0.80 14.20 -5 -6 12 -9.00 17.10 5 6 -12 -28.80 11.20 -5 6 12 8.80 10.80 -4 -6 12 72.29 21.20 -3 -6 12 14.90 16.60 -2 -6 12 100.79 21.20 -2 6 12 46.00 16.80 -1 -6 12 11.20 17.00 -1 6 12 -2.10 15.10 -4 -7 12 0.30 16.70 -3 -7 12 -4.80 16.80 -2 -7 12 94.39 21.40 -4 0 13 14.60 16.60 -3 0 13 -2.30 15.30 -2 0 13 16.10 17.60 -4 -1 13 -7.40 15.60 -4 1 13 28.70 16.10 -3 -1 13 31.90 17.60 -3 1 13 8.40 15.70 -2 -1 13 42.60 18.30 -2 1 13 26.90 17.70 -4 -2 13 18.90 18.10 -4 2 13 43.00 16.70 -3 -2 13 51.89 18.60 -3 2 13 56.19 18.40 -2 -2 13 27.30 19.50 -2 2 13 23.70 17.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 48258 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 0.80630(5) 0.37079(3) 0.77000(4) 0.05584(15) Uani 1 1 d . . . . . O002 O 0.0342(3) 0.4568(2) 0.4685(3) 0.0510(7) Uani 1 1 d . . . . . N003 N 0.3503(4) 0.5887(2) 0.5595(3) 0.0319(6) Uani 1 1 d . . . . . N004 N 0.1506(4) 0.4313(2) 0.2819(3) 0.0365(7) Uani 1 1 d . . . . . C005 C 0.5903(5) 0.5366(3) 0.3535(4) 0.0388(9) Uani 1 1 d . . . . . H005 H 0.670736 0.567381 0.430352 0.047 Uiso 1 1 calc R U . . . C006 C 0.6271(5) 0.4636(2) 0.6889(4) 0.0325(8) Uani 1 1 d . . . . . C007 C 0.4287(5) 0.5012(2) 0.3640(4) 0.0306(7) Uani 1 1 d . . . . . C008 C 0.4777(6) 0.7186(3) 0.6783(5) 0.0399(10) Uani 1 1 d . . . . . H008 H 0.558225 0.759672 0.740281 0.048 Uiso 1 1 calc R U . . . C009 C 0.8387(5) 0.6283(3) 0.9503(4) 0.0390(9) Uani 1 1 d . . . . . H009 H 0.735971 0.630858 0.980700 0.047 Uiso 1 1 calc R U . . . C00A C 0.3077(6) 0.7436(3) 0.5877(4) 0.0454(10) Uani 1 1 d . . . . . H00A H 0.255175 0.804154 0.579629 0.055 Uiso 1 1 calc R U . . . C00B C 0.4509(4) 0.4216(2) 0.5990(3) 0.0300(8) Uani 1 1 d . . . . . H00B H 0.478243 0.366084 0.547461 0.036 Uiso 1 1 calc R U . . . O1 O 0.2287(5) 0.2628(2) 0.5315(5) 0.0758(10) Uani 1 1 d . . . . . C00D C 0.6521(5) 0.5573(2) 0.7202(3) 0.0294(7) Uani 1 1 d . . . . . C00E C 0.2334(5) 0.6644(3) 0.5142(4) 0.0407(9) Uani 1 1 d . . . . . H00E H 0.122128 0.661469 0.444820 0.049 Uiso 1 1 calc R U . . . C00F C 0.1558(5) 0.4609(3) 0.4145(4) 0.0364(8) Uani 1 1 d . . . . . C00G C 1.0031(6) 0.6572(3) 1.0411(4) 0.0435(9) Uani 1 1 d . . . . . H00G H 1.010693 0.677786 1.132769 0.052 Uiso 1 1 calc R U . . . N1 N 0.2429(5) 0.2947(3) 0.6497(5) 0.0547(9) Uani 1 1 d . . . . . C00I C 0.3473(5) 0.3857(3) 0.6994(4) 0.0456(10) Uani 1 1 d . . . . . H00C H 0.431907 0.374690 0.792729 0.055 Uiso 1 1 calc R U . . . H00D H 0.264156 0.435483 0.709252 0.055 Uiso 1 1 calc R U . . . C00J C 0.6302(6) 0.5253(3) 0.2255(4) 0.0473(10) Uani 1 1 d . . . . . H00J H 0.737727 0.549421 0.215731 0.057 Uiso 1 1 calc R U . . . C00K C 0.9794(5) 0.5962(3) 0.7691(4) 0.0403(9) Uani 1 1 d . . . . . H00K H 0.971972 0.576438 0.677088 0.048 Uiso 1 1 calc R U . . . C00L C 0.3499(5) 0.4975(2) 0.4872(4) 0.0306(7) Uani 1 1 d . . . . . C00M C 0.5043(5) 0.6222(2) 0.6591(4) 0.0313(7) Uani 1 1 d . . . . . C00N C 0.3093(5) 0.4563(3) 0.2481(4) 0.0337(8) Uani 1 1 d . . . . . C00O C -0.0004(5) 0.3803(4) 0.1867(4) 0.0548(10) Uani 1 1 d . . . . . H00F H 0.038036 0.317521 0.167537 0.082 Uiso 1 1 calc R U . . . H00H H -0.043683 0.415343 0.098992 0.082 Uiso 1 1 calc R U . . . H00I H -0.095324 0.374458 0.230551 0.082 Uiso 1 1 calc R U . . . C00P C 0.8262(5) 0.5958(2) 0.8147(4) 0.0318(7) Uani 1 1 d . . . . . C00Q C 1.1551(6) 0.6555(3) 0.9967(5) 0.0447(10) Uani 1 1 d . . . . . H00Q H 1.265798 0.674297 1.058154 0.054 Uiso 1 1 calc R U . . . O00R O 0.1773(6) 0.2576(3) 0.7335(5) 0.0992(15) Uani 1 1 d . . . . . C00S C 0.3473(6) 0.4429(3) 0.1212(4) 0.0436(9) Uani 1 1 d . . . . . H00S H 0.267252 0.411619 0.044713 0.052 Uiso 1 1 calc R U . . . C00T C 1.1424(5) 0.6257(3) 0.8597(5) 0.0463(10) Uani 1 1 d . . . . . H00T H 1.244627 0.625654 0.828532 0.056 Uiso 1 1 calc R U . . . C00U C 0.5117(6) 0.4785(3) 0.1132(4) 0.0512(10) Uani 1 1 d . . . . . H00U H 0.542309 0.470454 0.029152 0.061 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 0.0642(3) 0.03612(19) 0.0499(2) -0.0004(2) -0.00994(17) 0.0131(2) O002 0.0371(14) 0.0650(19) 0.0550(18) -0.0108(15) 0.0198(14) -0.0093(13) N003 0.0355(15) 0.0299(15) 0.0296(15) -0.0038(12) 0.0085(12) 0.0019(12) N004 0.0357(16) 0.0368(17) 0.0335(17) -0.0048(13) 0.0048(13) -0.0052(13) C005 0.043(2) 0.041(2) 0.032(2) 0.0012(18) 0.0095(17) -0.0023(18) C006 0.0399(18) 0.029(2) 0.0262(17) 0.0004(14) 0.0061(15) 0.0011(15) C007 0.0349(19) 0.0288(18) 0.0262(18) 0.0010(14) 0.0061(15) 0.0035(14) C008 0.049(2) 0.027(2) 0.047(3) -0.0064(17) 0.019(2) -0.0060(17) C009 0.045(2) 0.038(2) 0.037(2) -0.0064(17) 0.0172(17) -0.0058(17) C00A 0.058(3) 0.031(2) 0.053(2) 0.0038(18) 0.025(2) 0.0099(19) C00B 0.0389(19) 0.0266(18) 0.0245(18) -0.0006(14) 0.0094(15) -0.0022(15) O1 0.088(3) 0.048(2) 0.089(3) -0.0154(19) 0.023(2) -0.0218(18) C00D 0.0338(17) 0.0328(18) 0.0248(17) -0.0006(14) 0.0133(14) -0.0019(14) C00E 0.043(2) 0.040(2) 0.040(2) 0.0078(17) 0.0124(17) 0.0089(17) C00F 0.0371(19) 0.036(2) 0.034(2) -0.0024(16) 0.0070(16) -0.0029(15) C00G 0.055(2) 0.044(2) 0.029(2) -0.0063(16) 0.0081(18) -0.0048(18) N1 0.051(2) 0.043(2) 0.075(3) 0.019(2) 0.025(2) -0.0005(17) C00I 0.062(2) 0.040(3) 0.0355(18) 0.0019(19) 0.0162(17) -0.009(2) C00J 0.049(2) 0.056(3) 0.042(2) 0.009(2) 0.0212(19) 0.002(2) C00K 0.042(2) 0.048(2) 0.035(2) -0.0041(17) 0.0183(17) 0.0008(17) C00L 0.0332(18) 0.0301(18) 0.0279(18) -0.0030(14) 0.0084(14) -0.0018(14) C00M 0.0350(18) 0.0296(18) 0.0313(18) 0.0004(14) 0.0126(15) -0.0024(15) C00N 0.0400(19) 0.0275(18) 0.0310(19) 0.0026(14) 0.0064(16) 0.0060(14) C00O 0.046(2) 0.059(3) 0.051(2) -0.018(3) 0.0011(16) -0.013(2) C00P 0.0371(18) 0.0275(17) 0.0288(18) -0.0012(14) 0.0067(15) -0.0013(14) C00Q 0.040(2) 0.036(2) 0.049(3) -0.0072(19) -0.0015(19) -0.0013(17) O00R 0.109(3) 0.082(3) 0.130(4) 0.028(2) 0.072(3) -0.020(2) C00S 0.058(2) 0.042(2) 0.027(2) -0.0028(17) 0.0070(18) 0.0039(19) C00T 0.036(2) 0.049(2) 0.056(3) 0.000(2) 0.0169(19) 0.0016(18) C00U 0.063(3) 0.059(3) 0.038(2) 0.002(2) 0.025(2) 0.008(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' 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' 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 C00E N003 C00M 108.8(3) . . ? C00E N003 C00L 127.1(3) . . ? C00M N003 C00L 121.1(3) . . ? C00F N004 C00N 111.7(3) . . ? C00F N004 C00O 123.9(3) . . ? C00N N004 C00O 124.4(3) . . ? C007 C005 C00J 118.4(4) . . ? C00D C006 C00B 123.8(3) . . ? C00D C006 Br01 121.9(3) . . ? C00B C006 Br01 114.1(2) . . ? C00N C007 C005 120.2(3) . . ? C00N C007 C00L 108.2(3) . . ? C005 C007 C00L 131.6(3) . . ? C00M C008 C00A 107.8(4) . . ? C00P C009 C00G 120.4(4) . . ? C00E C00A C008 108.1(4) . . ? C006 C00B C00I 107.9(3) . . ? C006 C00B C00L 109.3(3) . . ? C00I C00B C00L 115.1(3) . . ? C006 C00D C00M 118.0(3) . . ? C006 C00D C00P 122.3(3) . . ? C00M C00D C00P 119.7(3) . . ? C00A C00E N003 108.3(4) . . ? O002 C00F N004 126.8(3) . . ? O002 C00F C00L 126.1(3) . . ? N004 C00F C00L 107.1(3) . . ? C00Q C00G C009 120.4(4) . . ? O00R N1 O1 123.9(4) . . ? O00R N1 C00I 115.7(4) . . ? O1 N1 C00I 120.3(3) . . ? N1 C00I C00B 113.6(3) . . ? C00U C00J C005 120.4(4) . . ? C00T C00K C00P 120.2(3) . . ? N003 C00L C007 114.8(3) . . ? N003 C00L C00F 112.0(3) . . ? C007 C00L C00F 102.1(3) . . ? N003 C00L C00B 108.7(3) . . ? C007 C00L C00B 110.5(3) . . ? C00F C00L C00B 108.7(3) . . ? C008 C00M N003 106.9(3) . . ? C008 C00M C00D 133.2(3) . . ? N003 C00M C00D 119.9(3) . . ? C00S C00N C007 122.4(3) . . ? C00S C00N N004 127.9(3) . . ? C007 C00N N004 109.7(3) . . ? C009 C00P C00K 119.0(3) . . ? C009 C00P C00D 120.6(3) . . ? C00K C00P C00D 120.3(3) . . ? C00G C00Q C00T 119.5(4) . . ? C00N C00S C00U 116.5(4) . . ? C00K C00T C00Q 120.4(4) . . ? C00J C00U C00S 122.1(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 C006 1.893(3) . ? O002 C00F 1.213(4) . ? N003 C00E 1.375(5) . ? N003 C00M 1.383(5) . ? N003 C00L 1.454(4) . ? N004 C00F 1.355(5) . ? N004 C00N 1.410(5) . ? N004 C00O 1.450(5) . ? C005 C007 1.379(5) . ? C005 C00J 1.389(6) . ? C006 C00D 1.342(5) . ? C006 C00B 1.510(5) . ? C007 C00N 1.387(5) . ? C007 C00L 1.509(5) . ? C008 C00M 1.379(5) . ? C008 C00A 1.400(6) . ? C009 C00P 1.383(5) . ? C009 C00G 1.383(6) . ? C00A C00E 1.350(6) . ? C00B C00I 1.528(5) . ? C00B C00L 1.559(5) . ? O1 N1 1.217(5) . ? C00D C00M 1.444(5) . ? C00D C00P 1.495(5) . ? C00F C00L 1.550(5) . ? C00G C00Q 1.373(6) . ? N1 O00R 1.204(5) . ? N1 C00I 1.506(6) . ? C00J C00U 1.374(6) . ? C00K C00T 1.378(5) . ? C00K C00P 1.387(5) . ? C00N C00S 1.374(5) . ? C00Q C00T 1.383(6) . ? C00S C00U 1.392(6) . ?