#------------------------------------------------------------------------------ #$Date: 2025-08-19 20:21:09 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301810 $ #$URL: svn://www.crystallography.net/cod/cif/3/50/00/3500041.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_3500041 loop_ _publ_author_name 'Thierry Maris' _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _publ_section_title ; 2-Naphthylsulfonyl chloride ; _journal_name_full 'Personal communication to COD' _journal_year 2016 _chemical_formula_moiety 'C7 H6 Br N O2' _chemical_formula_sum 'C7 H6 Br N O2' _chemical_formula_weight 216.04 _chemical_name_common 1-Bromomethyl-3-nitrobenzene _chemical_name_systematic 'Benzene, 1-(bromomethyl)-3-?nitro-' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2016-04-26 _audit_creation_method ; Olex2 1.2 (compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155) ; _cell_angle_alpha 90 _cell_angle_beta 112.566(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.1448(15) _cell_length_b 4.4764(6) _cell_length_c 15.0812(19) _cell_measurement_reflns_used 9807 _cell_measurement_temperature 100 _cell_measurement_theta_max 60.773 _cell_measurement_theta_min 3.482 _cell_volume 757.12(17) _computing_cell_refinement ; SAINT (2013) V8.37A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_collection ; APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_reduction ; SAINT (2013) V8.37A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_detector 'CMOS Area detector' _diffrn_detector_area_resol_mean 10.24 _diffrn_detector_type 'Bruker Photon 100 CMOS Detector' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device 'k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker Venture Metaljet' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_collimation 'Focusing mirrors' _diffrn_radiation_monochromator 'Helios MX Mirror Optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_unetI/netI 0.0248 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 22671 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 60.741 _diffrn_reflns_theta_min 5.269 _diffrn_source 'Metal Jet' _diffrn_source_target Ga _diffrn_source_type 'Gallium Liquid Metal Jet Source' _exptl_absorpt_coefficient_mu 4.807 _exptl_absorpt_correction_T_max 0.3107 _exptl_absorpt_correction_T_min 0.1884 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1150 before and 0.0852 after correction. The Ratio of minimum to maximum transmission is 0.6064. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.895 _exptl_crystal_description Block _exptl_crystal_F_000 424 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Venture diffractometer equipped with a Photon 100 CMOS Detector, a Helios MX optics and a Kappa goniometer. The crystal-to-detector distance was 4.0 cm, and the data collection was carried out in 1024 x 1024 pixel mode. ; _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _refine_diff_density_max 1.206 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.131 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 1740 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.125 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0400 _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^)+(0.0627P)^2^+0.4062P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1015 _refine_ls_wR_factor_ref 0.1050 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1611 _reflns_number_total 1740 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file BrNit1.cif _cod_data_source_block brnit1 _cod_depositor_comments ; The following automatic conversions were performed: '_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 4624 2016-04-14 12:54:50Z antanas ; _cod_database_code 3500041 _cod_database_fobs_code 3500041 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.533 _shelx_estimated_absorpt_t_min 0.284 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B) 2.b Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C4(H4), C6(H6) ; _shelx_res_file ; brnit1.res created by SHELXL-2014/7 TITL brnit1_a.res in P2(1)/c REM Old TITL BrNit1 in P21/c #14 REM SHELXT solution in P2(1)/c REM R1 0.121, Rweak 0.001, Alpha 0.027, Orientation as input REM Formula found by SHELXT: C8 N O Br CELL 1.34139 12.1448 4.4764 15.0812 90 112.566 90 ZERR 4 0.0015 0.0006 0.0019 0 0.005 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O Br DISP Br -0.934 1.041 8191.512 DISP C 0.014 0.007 57.748 DISP H -0 0 0.648 DISP N 0.025 0.014 110.512 DISP O 0.039 0.025 193.954 UNIT 28 24 4 8 4 EQIV $1 -X,2-Y,1-Z EQIV $2 1-X,-0.5+Y,1.5-Z L.S. 30 PLAN 8 SIZE 0.15 0.18 0.35 TEMP 0 HTAB C2 O1_$1 HTAB C4 Br1_$2 BOND $H LIST 4 HTAB MORE -1 CONF fmap 2 acta REM REM REM WGHT 0.062700 0.406200 FVAR 0.74309 BR1 5 0.544961 0.388924 0.896346 11.00000 0.03804 0.05535 = 0.06058 0.00548 0.01367 0.00190 O1 4 0.082624 0.748452 0.485939 11.00000 0.05931 0.06496 = 0.05114 0.00814 0.01663 0.00097 O2 4 0.208345 0.389159 0.506332 11.00000 0.05606 0.07028 = 0.05515 -0.01318 0.02133 -0.00141 N1 3 0.154395 0.565899 0.536438 11.00000 0.04298 0.05372 = 0.05145 -0.00518 0.01616 -0.00850 C1 1 0.127654 0.716270 0.770661 11.00000 0.03940 0.04702 = 0.05302 -0.00169 0.01603 0.00061 AFIX 43 H1 2 0.080814 0.826503 0.795159 11.00000 -1.20000 AFIX 0 C2 1 0.104478 0.728393 0.672867 11.00000 0.03688 0.04431 = 0.05112 0.00103 0.01124 -0.00060 AFIX 43 H2 2 0.043029 0.845257 0.631264 11.00000 -1.20000 AFIX 0 C3 1 0.176932 0.558685 0.639922 11.00000 0.04132 0.04664 = 0.04697 -0.00309 0.01436 -0.00586 C4 1 0.269132 0.383507 0.699435 11.00000 0.04003 0.04295 = 0.05443 -0.00435 0.01656 -0.00354 AFIX 43 H4 2 0.315629 0.272946 0.674686 11.00000 -1.20000 AFIX 0 C5 1 0.291507 0.374764 0.797112 11.00000 0.03840 0.04265 = 0.05146 -0.00016 0.01205 -0.00588 C6 1 0.220034 0.541232 0.832116 11.00000 0.04143 0.04626 = 0.04767 -0.00130 0.01348 -0.00393 AFIX 43 H6 2 0.234223 0.535283 0.897232 11.00000 -1.20000 AFIX 0 C7 1 0.390446 0.182660 0.862256 11.00000 0.04008 0.04441 = 0.06652 0.00674 0.01687 -0.00278 AFIX 23 H7A 2 0.392059 -0.004727 0.830476 11.00000 -1.20000 H7B 2 0.376701 0.138452 0.920139 11.00000 -1.20000 AFIX 0 HKLF 4 REM brnit1_a.res in P2(1)/c REM R1 = 0.0400 for 1611 Fo > 4sig(Fo) and 0.0422 for all 1740 data REM 100 parameters refined using 0 restraints END WGHT 0.0627 0.4062 REM Instructions for potential hydrogen bonds HTAB C2 O1_$1 HTAB C4 Br1_$2 REM Highest difference peak 1.206, deepest hole -0.356, 1-sigma level 0.131 Q1 1 0.5587 0.3842 0.8469 11.00000 0.05 1.21 Q2 1 0.5173 0.3895 0.9394 11.00000 0.05 1.11 Q3 1 0.2874 0.3725 0.7587 11.00000 0.05 0.45 Q4 1 0.1059 0.6968 0.7192 11.00000 0.05 0.38 Q5 1 0.3608 0.1175 0.8053 11.00000 0.05 0.37 Q6 1 0.2567 0.4167 0.8172 11.00000 0.05 0.36 Q7 1 0.1254 0.6124 0.6625 11.00000 0.05 0.35 Q8 1 0.5445 -0.1681 0.8962 11.00000 0.05 0.28 ; _shelx_res_checksum 72402 _shelx_hkl_file ; 2 0 0 497.65 32.20 -2 0 0 414.76 32.20 2 0 0 464.95 32.20 -4 0 0 127.29 9.90 -4 0 0 152.28 10.00 4 0 0 134.19 10.00 -4 0 0 153.68 10.00 -4 0 0 143.09 9.90 -4 0 0 137.99 10.00 -4 0 0 142.29 10.00 -4 0 0 141.99 9.90 -4 0 0 124.19 10.00 -4 0 0 145.39 10.00 -5 0 0 140.69 11.30 -5 0 0 153.38 11.20 -5 0 0 160.88 11.30 -5 0 0 168.78 11.30 -5 0 0 169.48 11.30 -5 0 0 141.09 11.20 -5 0 0 160.68 11.30 -5 0 0 178.28 11.30 -5 0 0 157.38 11.30 -5 0 0 150.88 11.30 -5 0 0 170.48 11.30 -6 0 0 355.76 29.30 -6 0 0 445.46 29.30 -6 0 0 447.86 29.30 -6 0 0 380.06 29.30 -6 0 0 395.06 29.30 -6 0 0 437.86 29.30 -6 0 0 459.55 29.30 -6 0 0 414.86 29.30 -6 0 0 415.96 29.40 -6 0 0 351.26 29.40 -6 0 0 413.86 29.30 -6 0 0 460.55 29.30 -6 0 0 473.95 29.30 -6 0 0 390.76 29.30 -6 0 0 425.96 29.30 -6 0 0 390.26 29.30 -7 0 0 352.96 22.70 -7 0 0 327.97 22.70 -7 0 0 322.77 22.70 -7 0 0 305.37 22.60 -7 0 0 323.97 22.60 -7 0 0 320.47 22.60 -7 0 0 285.07 22.60 -7 0 0 320.97 22.60 -7 0 0 360.26 22.60 -7 0 0 333.57 22.70 -7 0 0 295.87 22.60 -7 0 0 303.77 22.60 -7 0 0 288.37 22.70 -7 0 0 360.46 22.80 -7 0 0 321.47 22.70 -8 0 0 710.63 48.60 -8 0 0 708.43 48.70 -8 0 0 741.03 48.60 -8 0 0 639.04 48.60 -8 0 0 658.43 48.70 -8 0 0 637.44 48.70 -8 0 0 606.24 48.60 -8 0 0 598.04 48.60 -8 0 0 728.33 48.70 -8 0 0 737.23 48.80 -8 0 0 761.82 48.70 -8 0 0 703.73 48.60 -8 0 0 700.63 48.70 -8 0 0 680.53 48.70 -8 0 0 785.82 48.90 -9 0 0 707.43 49.60 -9 0 0 641.24 49.60 -9 0 0 765.52 49.70 -9 0 0 668.23 49.60 -9 0 0 687.03 49.60 -9 0 0 673.73 49.50 -9 0 0 763.82 49.70 -9 0 0 656.03 49.60 -9 0 0 776.42 49.60 -9 0 0 741.33 49.60 -9 0 0 684.33 49.50 -10 0 0 414.76 30.30 -10 0 0 472.85 30.30 -10 0 0 392.36 30.20 -10 0 0 450.55 30.30 -10 0 0 408.36 30.20 -10 0 0 437.16 30.40 -10 0 0 474.15 30.30 -10 0 0 392.96 30.20 -10 0 0 448.96 30.30 -10 0 0 400.06 30.20 -11 0 0 881.81 59.89 -11 0 0 898.31 59.79 -11 0 0 840.12 59.69 -11 0 0 866.01 59.69 -11 0 0 818.72 59.79 -11 0 0 735.13 59.69 -11 0 0 913.71 59.79 -12 0 0 658.43 44.50 -12 0 0 652.63 44.50 -12 0 0 650.53 44.60 -12 0 0 576.74 44.70 -12 0 0 630.44 44.50 -12 0 0 629.94 44.50 -12 0 0 625.94 44.50 -13 0 0 282.77 21.20 -13 0 0 308.77 20.90 -13 0 0 292.17 20.90 -13 0 0 299.77 20.90 -13 0 0 305.77 21.00 -13 0 0 279.87 20.90 -14 0 0 86.59 5.80 -14 0 0 83.49 5.90 -14 0 0 71.19 6.10 -14 0 0 73.29 6.20 -14 0 0 76.79 5.70 -14 0 0 74.09 5.70 -1 -1 0 260.47 20.70 -1 -1 0 271.27 20.70 -1 -1 0 285.27 20.70 -1 1 0 342.67 20.70 -1 1 0 319.47 20.80 1 1 0 292.67 20.70 1 1 0 294.47 20.70 -2 -1 0 1798.02 142.79 -2 -1 0 2217.08 142.69 -2 -1 0 1860.71 142.79 -2 -1 0 1964.20 142.69 -2 -1 0 1895.41 142.79 -2 -1 0 1983.70 142.79 2 1 0 2143.59 142.79 -2 1 0 2251.67 142.79 -2 1 0 1964.40 142.79 2 1 0 2297.57 142.79 -3 -1 0 7122.29 541.75 3 -1 0 7183.98 541.75 -3 1 0 8778.92 541.75 3 1 0 8243.68 541.85 -3 1 0 7363.16 541.75 -4 -1 0 794.12 63.39 -4 -1 0 970.00 63.29 -4 -1 0 907.21 63.39 -4 -1 0 919.11 63.29 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2216.58 151.18 -6 -1 0 1975.00 151.18 -6 -1 0 1943.11 151.18 -6 -1 0 1888.91 151.08 -6 -1 0 2035.90 151.18 -6 -1 0 2196.68 151.08 -6 -1 0 2365.16 151.18 -6 1 0 2198.88 151.08 -6 1 0 2481.25 151.08 -6 1 0 2147.29 151.28 -6 1 0 2441.06 151.18 -6 1 0 2368.56 151.18 -6 1 0 2163.88 151.18 -6 1 0 2365.06 151.18 -6 1 0 1880.31 151.28 -6 1 0 2189.38 151.18 -6 1 0 2140.99 151.18 -6 1 0 2270.77 151.18 -6 1 0 2073.09 151.08 -7 -1 0 548.35 35.90 -7 -1 0 480.35 35.90 -7 -1 0 528.15 35.90 -7 -1 0 464.25 35.90 7 -1 0 469.15 35.90 -7 -1 0 539.45 35.90 -7 -1 0 575.04 35.90 -7 -1 0 475.85 35.80 -7 -1 0 430.96 35.80 -7 -1 0 528.45 35.80 -7 -1 0 514.35 35.90 -7 -1 0 554.94 36.00 -7 -1 0 561.54 36.10 -7 -1 0 530.25 35.90 -7 -1 0 514.05 35.90 -7 -1 0 528.25 35.90 -7 1 0 494.35 35.80 -7 1 0 438.76 36.00 -7 1 0 482.65 35.80 -7 1 0 538.25 35.90 -7 1 0 530.05 35.90 -7 1 0 523.55 35.90 -7 1 0 506.25 35.90 -7 1 0 503.15 35.90 -7 1 0 543.55 36.00 -7 1 0 515.55 35.90 -7 1 0 439.96 35.90 -7 1 0 533.05 35.90 -8 -1 0 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56.19 -7 -3 0 812.92 56.19 -7 -3 0 744.13 56.39 -7 -3 0 810.42 56.29 -7 -3 0 673.43 56.19 -7 -3 0 761.62 56.19 7 3 0 770.62 56.19 -7 3 0 787.22 56.29 -7 3 0 774.72 56.29 -7 3 0 924.51 56.19 -7 3 0 810.62 56.19 -8 -3 0 101.79 7.40 -8 -3 0 102.09 7.30 -8 -3 0 84.89 7.40 -8 -3 0 97.69 7.70 -8 -3 0 110.99 7.40 -8 -3 0 105.19 7.50 -8 -3 0 90.49 7.40 8 -3 0 102.39 7.30 -8 -3 0 104.79 7.30 -8 3 0 109.59 7.60 -8 3 0 96.39 7.50 8 3 0 98.89 7.40 -8 3 0 103.79 7.40 -8 3 0 98.99 7.30 -9 -3 0 139.49 9.50 -9 -3 0 116.09 9.50 9 -3 0 124.69 9.40 -9 -3 0 130.89 9.40 -9 -3 0 147.09 9.60 -9 -3 0 130.39 9.50 -9 -3 0 142.69 9.40 -9 -3 0 130.49 9.80 -9 -3 0 111.29 9.50 -9 -3 0 140.19 9.60 -9 3 0 133.29 9.60 -9 3 0 133.99 9.40 9 3 0 122.39 9.50 -10 -3 0 14.10 1.60 -10 -3 0 11.70 1.80 -10 -3 0 11.80 2.00 -10 -3 0 14.30 1.60 -10 -3 0 16.90 1.70 -10 -3 0 14.70 1.90 -10 -3 0 15.90 2.20 -10 -3 0 17.40 2.00 -10 -3 0 16.50 1.80 -10 3 0 13.00 1.60 -10 3 0 11.60 2.00 -10 3 0 13.10 1.80 -10 3 0 13.00 1.50 -11 -3 0 8.70 1.90 -11 -3 0 9.40 1.40 -11 -3 0 11.00 1.60 -11 -3 0 12.10 1.40 -11 -3 0 8.00 1.50 -11 3 0 9.60 1.80 -11 3 0 9.10 1.20 -11 3 0 11.20 1.40 -12 -3 0 0.90 1.00 -12 -3 0 -0.40 0.50 -12 -3 0 0.10 1.10 -12 3 0 0.50 0.90 -12 3 0 -0.20 0.70 -12 3 0 -0.90 0.80 0 -4 0 562.84 35.40 0 -4 0 494.55 35.60 0 -4 0 509.85 35.50 0 -4 0 474.15 35.50 0 -4 0 548.55 35.40 0 -4 0 482.15 35.40 0 4 0 475.65 35.40 0 4 0 466.25 35.40 1 -4 0 810.42 53.59 1 -4 0 819.32 53.69 -1 -4 0 673.83 53.69 -1 -4 0 823.72 53.59 -1 -4 0 794.52 53.69 1 -4 0 726.23 53.79 -1 -4 0 724.43 53.69 -1 -4 0 803.92 53.59 -1 -4 0 801.32 53.59 1 -4 0 772.02 53.69 1 -4 0 767.82 53.69 -1 -4 0 723.73 53.69 1 -4 0 849.02 53.59 -1 4 0 728.93 53.69 1 4 0 710.83 53.69 -1 4 0 669.93 53.59 -2 -4 0 135.89 8.90 -2 -4 0 122.69 9.00 2 -4 0 127.49 8.90 2 -4 0 128.29 9.00 -2 -4 0 133.99 8.90 2 -4 0 134.29 8.80 2 -4 0 120.69 9.00 2 -4 0 135.99 9.00 -2 -4 0 115.99 9.10 -2 -4 0 107.89 9.00 -2 -4 0 101.39 9.00 2 -4 0 134.19 9.10 -2 -4 0 118.09 8.90 -2 4 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6 -1 -18 28.20 2.50 6 -1 -18 33.50 2.40 -6 -1 18 30.80 3.00 -6 -1 18 36.80 2.60 -6 1 18 28.40 2.60 -6 1 18 30.40 2.60 -6 1 18 27.30 2.70 6 1 -18 32.80 2.50 -6 1 18 29.70 3.10 -5 -1 18 2.80 1.60 -5 -1 18 3.60 0.80 5 -1 -18 2.80 0.90 -5 -1 18 2.60 0.70 -5 -1 18 1.90 1.30 -5 -1 18 3.70 0.90 -5 1 18 3.60 0.90 5 1 -18 4.50 0.80 -5 1 18 3.20 1.40 -5 1 18 2.50 1.00 -4 -1 18 1.00 0.60 4 -1 -18 0.40 0.60 -4 -1 18 0.30 0.70 -4 -1 18 0.50 1.20 -4 -1 18 1.00 0.80 -4 -1 18 1.70 1.10 -4 -1 18 -0.70 0.70 4 -1 -18 1.60 0.90 -4 1 18 1.30 0.90 -4 1 18 1.20 1.30 4 1 -18 -0.10 0.70 -4 1 18 -0.10 0.90 -4 1 18 -0.60 0.50 -3 -1 18 0.80 1.20 -3 -1 18 0.10 1.10 3 -1 -18 0.30 0.60 -3 -1 18 1.30 0.80 -3 -1 18 -0.90 0.70 -3 -1 18 0.60 0.70 -3 1 18 0.00 0.90 -3 1 18 0.30 0.50 -3 1 18 0.10 1.30 3 1 -18 -1.50 0.70 2 -1 -18 -0.20 0.60 -2 -1 18 0.80 1.20 -2 -1 18 -0.60 1.00 -2 -1 18 -0.40 0.70 -2 -1 18 -0.70 0.90 -2 -1 18 -0.20 0.70 -2 1 18 0.30 0.90 2 1 -18 0.00 0.70 1 -1 -18 -0.50 0.70 -1 -1 18 0.20 0.80 1 -1 -18 -0.30 0.50 -1 -1 18 0.50 1.20 -1 -1 18 0.00 0.80 -1 -1 18 1.40 1.30 1 1 -18 0.10 0.70 -1 1 18 -0.20 0.90 -8 -2 18 0.10 0.50 -8 -2 18 0.80 0.90 8 -2 -18 0.70 0.60 -8 -2 18 -0.10 0.80 -8 -2 18 -0.90 0.70 8 2 -18 -0.60 0.90 -8 2 18 -0.90 1.10 -7 -2 18 13.60 1.50 -7 -2 18 13.70 1.30 -7 -2 18 16.10 1.70 -7 -2 18 14.40 1.80 7 -2 -18 12.60 1.40 7 -2 -18 12.90 1.50 7 2 -18 13.60 1.50 -7 2 18 14.50 2.10 6 -2 -18 1.20 0.90 -6 -2 18 -0.30 1.00 -6 -2 18 0.20 0.50 -6 -2 18 0.30 0.70 6 -2 -18 1.10 0.60 -6 -2 18 -0.20 0.70 6 2 -18 0.50 0.70 -5 -2 18 0.90 1.00 5 -2 -18 1.00 0.60 -5 -2 18 1.80 0.70 -5 -2 18 1.80 0.60 -5 -2 18 1.50 0.70 5 2 -18 1.40 0.70 -5 2 18 0.50 1.00 -4 -2 18 17.10 2.10 4 -2 -18 16.80 2.10 -4 -2 18 18.00 1.70 4 -2 -18 17.80 1.50 -4 -2 18 16.40 1.50 4 2 -18 15.70 1.70 -4 2 18 17.60 1.90 -3 -2 18 1.30 0.80 3 -2 -18 0.50 1.10 -3 -2 18 1.00 0.70 3 -2 -18 0.90 0.60 -3 -2 18 -0.20 1.10 -3 2 18 1.20 1.10 -9 0 19 0.60 1.10 -9 0 19 0.50 0.80 -9 0 19 -0.50 1.00 -9 0 19 0.20 0.50 9 0 -19 -0.20 0.60 -9 0 19 0.00 0.60 -8 0 19 -0.10 0.80 8 0 -19 0.40 0.70 -8 0 19 -0.30 0.60 -8 0 19 -1.10 0.50 -8 0 19 -0.40 0.80 -8 0 19 -0.30 1.10 -7 0 19 -0.60 1.20 7 0 -19 -0.70 0.60 -7 0 19 0.10 0.70 -7 0 19 -1.30 1.00 -7 0 19 -0.20 0.80 -7 0 19 -0.20 0.90 -7 0 19 0.00 0.60 -6 0 19 -0.60 0.60 -6 0 19 -1.60 1.10 -6 0 19 0.70 1.20 -6 0 19 -2.00 1.60 -6 0 19 -0.80 0.70 6 0 -19 -0.40 0.60 -5 0 19 0.10 0.80 -5 0 19 -0.10 1.00 -5 0 19 -0.40 0.80 -5 0 19 -0.20 0.70 -4 0 19 -0.50 1.00 4 0 -19 -0.40 0.60 -4 0 19 -0.80 1.00 -4 0 19 0.50 1.20 -4 0 19 0.00 0.90 -3 0 19 0.10 0.80 -3 0 19 0.10 1.00 3 0 -19 0.20 0.70 -3 0 19 -0.30 1.10 -8 -1 19 0.60 0.80 -8 -1 19 1.50 0.80 8 -1 -19 0.40 0.70 -8 -1 19 1.30 0.70 -8 -1 19 1.00 1.00 -8 -1 19 0.20 0.50 8 1 -19 -0.10 1.10 -8 1 19 0.50 0.70 -8 1 19 0.10 0.90 -8 1 19 -0.50 0.70 7 -1 -19 4.30 0.80 -7 -1 19 5.50 0.90 7 -1 -19 5.40 0.90 -7 -1 19 6.80 1.20 -7 1 19 6.60 1.20 -7 1 19 5.60 1.20 7 1 -19 5.70 0.80 -6 -1 19 1.30 0.70 -6 -1 19 -0.20 0.50 6 -1 -19 0.40 0.60 -6 -1 19 0.20 1.00 6 -1 -19 1.20 0.90 -6 -1 19 1.20 0.70 -6 1 19 0.40 0.80 6 1 -19 -0.20 0.70 -6 1 19 -0.50 1.40 -6 1 19 -1.20 0.90 -5 -1 19 8.80 1.30 5 -1 -19 6.80 1.00 -5 -1 19 7.80 1.00 -5 -1 19 9.80 1.80 -5 1 19 8.30 1.20 5 1 -19 9.00 1.10 -5 1 19 7.20 1.50 -4 -1 19 6.00 1.30 -4 -1 19 4.20 0.80 -4 -1 19 7.10 1.30 4 -1 -19 6.90 1.00 -4 1 19 6.80 1.10 -4 1 19 4.80 1.40 4 1 -19 6.90 1.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 84740 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.54496(2) 0.38892(7) 0.89635(2) 0.05290(16) Uani 1 1 d . . . . . O1 O 0.0826(2) 0.7485(5) 0.48594(14) 0.0598(5) Uani 1 1 d . . . . . O2 O 0.2083(2) 0.3892(5) 0.50633(16) 0.0605(6) Uani 1 1 d . . . . . N1 N 0.1544(2) 0.5659(5) 0.53644(17) 0.0500(5) Uani 1 1 d . . . . . C1 C 0.1277(2) 0.7163(6) 0.77066(19) 0.0470(5) Uani 1 1 d . . . . . H1 H 0.0808 0.8265 0.7952 0.056 Uiso 1 1 calc R . . . . C2 C 0.1045(2) 0.7284(6) 0.67287(18) 0.0458(5) Uani 1 1 d . . . . . H2 H 0.0430 0.8453 0.6313 0.055 Uiso 1 1 calc R . . . . C3 C 0.1769(2) 0.5587(6) 0.63992(18) 0.0458(5) Uani 1 1 d . . . . . C4 C 0.2691(2) 0.3835(5) 0.6994(2) 0.0463(5) Uani 1 1 d . . . . . H4 H 0.3156 0.2729 0.6747 0.056 Uiso 1 1 calc R . . . . C5 C 0.2915(2) 0.3748(5) 0.7971(2) 0.0457(5) Uani 1 1 d . . . . . C6 C 0.2200(2) 0.5412(6) 0.83212(19) 0.0462(5) Uani 1 1 d . . . . . H6 H 0.2342 0.5353 0.8972 0.055 Uiso 1 1 calc R . . . . C7 C 0.3904(2) 0.1827(6) 0.8623(2) 0.0514(6) Uani 1 1 d . . . . . H7A H 0.3921 -0.0047 0.8305 0.062 Uiso 1 1 calc R . . . . H7B H 0.3767 0.1385 0.9201 0.062 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0380(2) 0.0553(2) 0.0606(2) 0.00548(11) 0.01367(15) 0.00190(10) O1 0.0593(12) 0.0650(13) 0.0511(10) 0.0081(9) 0.0166(9) 0.0010(10) O2 0.0561(12) 0.0703(14) 0.0552(11) -0.0132(9) 0.0213(10) -0.0014(9) N1 0.0430(11) 0.0537(12) 0.0515(11) -0.0052(9) 0.0162(9) -0.0085(9) C1 0.0394(11) 0.0470(13) 0.0530(13) -0.0017(11) 0.0160(10) 0.0006(10) C2 0.0369(11) 0.0443(13) 0.0511(12) 0.0010(10) 0.0112(9) -0.0006(9) C3 0.0413(12) 0.0466(12) 0.0470(12) -0.0031(10) 0.0144(10) -0.0059(10) C4 0.0400(12) 0.0429(13) 0.0544(14) -0.0043(9) 0.0166(11) -0.0035(9) C5 0.0384(12) 0.0426(12) 0.0515(13) -0.0002(9) 0.0121(10) -0.0059(9) C6 0.0414(12) 0.0463(12) 0.0477(12) -0.0013(10) 0.0135(10) -0.0039(10) C7 0.0401(12) 0.0444(12) 0.0665(16) 0.0067(12) 0.0169(11) -0.0028(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0140 0.0070 '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 0.0250 0.0140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0390 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.9340 1.0410 '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 O1 N1 C3 118.1(2) . . O2 N1 O1 123.9(2) . . O2 N1 C3 118.1(2) . . C2 C1 H1 119.6 . . C6 C1 H1 119.6 . . C6 C1 C2 120.8(2) . . C1 C2 H2 121.3 . . C3 C2 C1 117.3(2) . . C3 C2 H2 121.3 . . C2 C3 N1 118.6(2) . . C4 C3 N1 118.3(2) . . C4 C3 C2 123.0(2) . . C3 C4 H4 120.5 . . C3 C4 C5 119.0(2) . . C5 C4 H4 120.5 . . C4 C5 C6 119.3(2) . . C4 C5 C7 119.5(3) . . C6 C5 C7 121.2(3) . . C1 C6 C5 120.6(2) . . C1 C6 H6 119.7 . . C5 C6 H6 119.7 . . Br1 C7 H7A 109.6 . . Br1 C7 H7B 109.6 . . C5 C7 Br1 110.21(17) . . C5 C7 H7A 109.6 . . C5 C7 H7B 109.6 . . H7A C7 H7B 108.1 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Br1 C7 1.974(3) . O1 N1 1.224(3) . O2 N1 1.221(3) . N1 C3 1.478(3) . C1 H1 0.9300 . C1 C2 1.392(4) . C1 C6 1.391(4) . C2 H2 0.9300 . C2 C3 1.391(4) . C3 C4 1.379(4) . C4 H4 0.9300 . C4 C5 1.392(4) . C5 C6 1.393(4) . C5 C7 1.497(4) . C6 H6 0.9300 . C7 H7A 0.9700 . C7 H7B 0.9700 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C2 H2 O1 0.93 2.59 3.494(3) 165.2 3_576 C4 H4 Br1 0.93 2.89 3.820(3) 175.6 2_646 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 O1 N1 C3 C2 8.8(4) . . . . O1 N1 C3 C4 -171.2(2) . . . . O2 N1 C3 C2 -171.1(2) . . . . O2 N1 C3 C4 8.9(3) . . . . N1 C3 C4 C5 179.9(2) . . . . C1 C2 C3 N1 179.8(2) . . . . C1 C2 C3 C4 -0.2(4) . . . . C2 C1 C6 C5 0.1(4) . . . . C2 C3 C4 C5 -0.1(4) . . . . C3 C4 C5 C6 0.4(4) . . . . C3 C4 C5 C7 179.3(2) . . . . C4 C5 C6 C1 -0.4(4) . . . . C4 C5 C7 Br1 81.0(3) . . . . C6 C1 C2 C3 0.2(4) . . . . C6 C5 C7 Br1 -100.1(3) . . . . C7 C5 C6 C1 -179.3(2) . . . . loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 77568