#------------------------------------------------------------------------------ #$Date: 2021-07-20 07:00:30 +0300 (Tue, 20 Jul 2021) $ #$Revision: 267646 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/81/7158182.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_7158182 loop_ _publ_author_name 'Abeysekera, Amila M.' 'Averkiev, Boris B.' 'Le Magueres, Pierre' 'Aaker\"oy, Christer B.' _publ_section_title ; Intermolecular binding preferences of haloethynyl halogen-bond donors as a function of molecular electrostatic potentials in a family of N-(pyridin-2-yl)amides ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D1OB01133B _journal_year 2021 _chemical_formula_moiety 'C14 H9 Br N2 O' _chemical_formula_sum 'C14 H9 Br N2 O' _chemical_formula_weight 301.14 _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' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _audit_creation_date 2021-03-03 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214) ; _audit_update_record ; 2021-06-10 deposited with the CCDC. 2021-07-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.577(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.19740(10) _cell_length_b 21.9187(5) _cell_length_c 10.6585(2) _cell_measurement_reflns_used 6530 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 74.3100 _cell_measurement_theta_min 4.0340 _cell_volume 1193.59(4) _computing_cell_refinement 'CrysAlisPro 1.171.41.76a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.76a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.76a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.3-ac4 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-ac4 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.932 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 29.00 69.00 0.50 0.40 -- 101.80 -61.00 -90.00 80 2 \w 29.00 69.00 0.50 0.40 -- 101.80 -61.00-120.00 80 3 \w 29.00 127.00 0.50 0.40 -- 101.80 -82.00-153.00 196 4 \w 29.00 69.00 0.50 0.40 -- 101.80 -61.00-150.00 80 5 \w 127.00 175.00 0.50 0.40 -- 101.80 61.00-150.00 96 6 \w 29.00 69.00 0.50 0.40 -- 101.80 -61.00 120.00 80 7 \w 33.00 97.00 0.50 0.10 -- 45.89 19.00 120.00 128 8 \w -44.00 27.00 0.50 0.10 -- -45.89 37.00 90.00 142 9 \w -73.00 -19.00 0.50 0.40 -- -91.75 61.00 90.00 108 10 \w -53.00 -20.00 0.50 0.40 -- -91.75 45.00 60.00 66 11 \w -53.00 -20.00 0.50 0.40 -- -91.75 45.00 30.00 66 12 \w -53.00 -20.00 0.50 0.40 -- -91.75 45.00 0.00 66 13 \w -61.00 15.00 0.50 0.10 -- -45.89 57.00-150.00 152 14 \w -82.00 -29.00 0.50 0.10 -- -45.89 125.00 -30.00 106 15 \w -82.00 -29.00 0.50 0.10 -- -45.89 125.00 120.00 106 16 \w -163.00-126.00 0.50 0.40 -- -91.75 -77.00 60.00 74 17 \w -163.00-127.00 0.50 0.40 -- -91.75 -61.00 90.00 72 18 \w -163.00-127.00 0.50 0.40 -- -91.75 -61.00 -60.00 72 19 \w -163.00-126.00 0.50 0.40 -- -91.75 -77.00-150.00 74 20 \w -163.00-126.00 0.50 0.40 -- -91.75 -77.00-180.00 74 21 \w -163.00-127.00 0.50 0.40 -- -91.75 -61.00 -30.00 72 22 \w -163.00-122.00 0.50 0.40 -- -91.75 -45.00 30.00 82 23 \w -163.00-121.00 0.50 0.40 -- -91.75 -94.00 150.00 84 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.2234294000 _diffrn_orient_matrix_UB_12 -0.0025867000 _diffrn_orient_matrix_UB_13 -0.0768977000 _diffrn_orient_matrix_UB_21 0.0930884000 _diffrn_orient_matrix_UB_22 -0.0610167000 _diffrn_orient_matrix_UB_23 0.0644060000 _diffrn_orient_matrix_UB_31 -0.1797969000 _diffrn_orient_matrix_UB_32 -0.0347871000 _diffrn_orient_matrix_UB_33 -0.1075318000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_unetI/netI 0.0231 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.932 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 8888 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.932 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 75.059 _diffrn_reflns_theta_min 4.034 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 4.596 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.75134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.76a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light yellow' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.676 _exptl_crystal_description plate _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.221 _exptl_crystal_size_mid 0.051 _exptl_crystal_size_min 0.037 _refine_diff_density_max 0.337 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.064 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 199 _refine_ls_number_reflns 2304 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0244 _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^)+(0.0374P)^2^+0.7574P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.0671 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2181 _reflns_number_total 2304 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL sample2_a.res in P2(1)/c sample2.res created by SHELXL-2018/3 at 11:01:57 on 03-Mar-2021 REM Old TITL Sample2 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.075, Rweak 0.010, Alpha 0.025 REM 0.954 for 74 systematic absences, Orientation as input REM Formula found by SHELXT: C16 C8 O Br CELL 1.54184 5.1974 21.9187 10.6585 90 100.577 90 ZERR 4 0.0001 0.0005 0.0002 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Br N O UNIT 56 36 4 8 4 L.S. 10 PLAN 1 TEMP -173 CONF MORE -1 BOND $H fmap 2 acta OMIT -6 7 3 OMIT -6 5 6 REM REM REM WGHT 0.037400 0.757400 FVAR 4.61761 BR9 3 1.287321 0.660965 0.928882 11.00000 0.02486 0.02254 = 0.02560 -0.00041 0.00042 -0.00585 O12 5 -0.020875 0.357316 0.789494 11.00000 0.02644 0.02672 = 0.01768 0.00432 -0.00039 -0.00297 N10 4 0.010176 0.426132 0.631069 11.00000 0.02183 0.01891 = 0.01487 0.00162 -0.00124 -0.00005 N2 4 0.302221 0.502576 0.612967 11.00000 0.02126 0.02019 = 0.01727 0.00102 0.00056 0.00014 C4 1 0.662827 0.528778 0.781244 11.00000 0.02075 0.01815 = 0.02080 -0.00275 0.00044 0.00145 C11 1 -0.094651 0.376045 0.680783 11.00000 0.01977 0.01804 = 0.01840 -0.00076 0.00268 0.00279 C13 1 -0.307574 0.343017 0.592419 11.00000 0.02085 0.01513 = 0.02007 0.00018 0.00088 0.00226 C1 1 0.230715 0.459186 0.688717 11.00000 0.01981 0.01590 = 0.01865 -0.00168 0.00261 0.00146 C18 1 -0.500035 0.314570 0.646807 11.00000 0.02301 0.01861 = 0.02120 0.00156 0.00428 0.00286 C7 1 0.875715 0.569366 0.826500 11.00000 0.02431 0.02226 = 0.02022 0.00046 0.00152 0.00352 C3 1 0.514844 0.535502 0.658803 11.00000 0.02323 0.01820 = 0.01963 0.00141 0.00191 0.00065 C8 1 1.041949 0.605360 0.867288 11.00000 0.02224 0.02203 = 0.02171 0.00130 0.00110 -0.00145 C14 1 -0.305883 0.335640 0.462543 11.00000 0.02331 0.01852 = 0.02026 0.00135 0.00321 0.00155 C6 1 0.368960 0.447613 0.811659 11.00000 0.02490 0.01961 = 0.01877 0.00201 0.00095 -0.00042 C15 1 -0.497273 0.299983 0.388514 11.00000 0.03213 0.02197 = 0.01984 -0.00145 -0.00036 0.00247 C17 1 -0.691510 0.279580 0.571946 11.00000 0.01961 0.01878 = 0.03072 0.00274 0.00344 0.00241 C5 1 0.587261 0.482757 0.857140 11.00000 0.02515 0.02365 = 0.01702 -0.00077 -0.00089 0.00106 C16 1 -0.690790 0.271915 0.442745 11.00000 0.02307 0.01873 = 0.02967 -0.00248 -0.00316 0.00015 H14 2 -0.179759 0.353325 0.423041 11.00000 0.01525 H18 2 -0.492016 0.319366 0.733791 11.00000 0.01628 H15 2 -0.497630 0.294260 0.298523 11.00000 0.03063 H16 2 -0.825973 0.248015 0.390010 11.00000 0.03635 H6 2 0.319974 0.419390 0.856937 11.00000 0.03368 H3 2 0.559939 0.566105 0.601185 11.00000 0.01950 H5 2 0.688165 0.475771 0.942655 11.00000 0.02592 H10 2 -0.058899 0.440084 0.561448 11.00000 0.01718 H17 2 -0.812085 0.259522 0.609325 11.00000 0.02770 HKLF 4 REM sample2_a.res in P2(1)/c REM wR2 = 0.0671, GooF = S = 1.058, Restrained GooF = 1.058 for all data REM R1 = 0.0244 for 2181 Fo > 4sig(Fo) and 0.0256 for all 2304 data REM 199 parameters refined using 0 restraints END WGHT 0.0374 0.7574 REM Highest difference peak 0.337, deepest hole -0.706, 1-sigma level 0.064 Q1 1 -0.2128 0.3598 0.6286 11.00000 0.05 0.34 REM The information below was added by Olex2. REM REM R1 = 0.0244 for 2181 Fo > 4sig(Fo) and 0.0256 for all 9096 data REM 199 parameters refined using n/a restraints REM Highest difference peak 0.34, deepest hole -0.71 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0256 REM R1_gt = 0.0244 REM wR_ref = 0.0671 REM GOOF = 1.058 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 9096 REM Reflections_gt = 2181 REM Parameters = 199 REM Hole = -0.71 REM Peak = 0.34 REM Flack = n/a ; _cod_data_source_file d1ob01133b2.cif _cod_data_source_block Bz-act-Br _cod_database_code 7158182 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C14 H9 Br N2 O' _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. ; _reflns_odcompleteness_completeness 99.91 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.423 _oxdiff_exptl_absorpt_empirical_full_min 0.752 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 Br9 Br 1.28732(4) 0.66096(2) 0.92888(2) 0.02487(10) Uani 1 1 d . . . . . O12 O -0.0209(3) 0.35732(7) 0.78949(12) 0.0242(3) Uani 1 1 d . . . . . N10 N 0.0102(3) 0.42613(7) 0.63107(15) 0.0191(3) Uani 1 1 d . . . . . N2 N 0.3022(3) 0.50258(7) 0.61297(14) 0.0199(3) Uani 1 1 d . . . . . C4 C 0.6628(4) 0.52878(8) 0.78124(18) 0.0203(4) Uani 1 1 d . . . . . C11 C -0.0947(3) 0.37605(8) 0.68078(17) 0.0188(4) Uani 1 1 d . . . . . C13 C -0.3076(4) 0.34302(8) 0.59242(19) 0.0191(4) Uani 1 1 d . . . . . C1 C 0.2307(3) 0.45919(8) 0.68872(17) 0.0182(3) Uani 1 1 d . . . . . C18 C -0.5000(4) 0.31457(8) 0.64681(18) 0.0209(4) Uani 1 1 d . . . . . C7 C 0.8757(4) 0.56937(9) 0.82650(17) 0.0226(4) Uani 1 1 d . . . . . C3 C 0.5148(4) 0.53550(8) 0.65880(18) 0.0206(4) Uani 1 1 d . . . . . C8 C 1.0419(4) 0.60536(9) 0.86729(18) 0.0224(4) Uani 1 1 d . . . . . C14 C -0.3059(4) 0.33564(8) 0.46254(19) 0.0208(4) Uani 1 1 d . . . . . C6 C 0.3690(4) 0.44761(9) 0.81166(18) 0.0215(4) Uani 1 1 d . . . . . C15 C -0.4973(4) 0.29998(9) 0.38851(19) 0.0253(4) Uani 1 1 d . . . . . C17 C -0.6915(4) 0.27958(9) 0.57195(19) 0.0232(4) Uani 1 1 d . . . . . C5 C 0.5873(4) 0.48276(9) 0.85714(17) 0.0225(4) Uani 1 1 d . . . . . C16 C -0.6908(4) 0.27191(9) 0.44274(19) 0.0248(4) Uani 1 1 d . . . . . H14 H -0.180(4) 0.3533(11) 0.4230(19) 0.015(5) Uiso 1 1 d . . . . . H18 H -0.492(4) 0.3194(10) 0.734(2) 0.016(5) Uiso 1 1 d . . . . . H15 H -0.498(5) 0.2943(11) 0.299(2) 0.031(6) Uiso 1 1 d . . . . . H16 H -0.826(6) 0.2480(12) 0.390(3) 0.036(7) Uiso 1 1 d . . . . . H6 H 0.320(5) 0.4194(12) 0.857(2) 0.034(7) Uiso 1 1 d . . . . . H3 H 0.560(4) 0.5661(10) 0.601(2) 0.020(5) Uiso 1 1 d . . . . . H5 H 0.688(5) 0.4758(11) 0.943(2) 0.026(6) Uiso 1 1 d . . . . . H10 H -0.059(4) 0.4401(10) 0.561(2) 0.017(5) Uiso 1 1 d . . . . . H17 H -0.812(5) 0.2595(11) 0.609(2) 0.028(6) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br9 0.02486(13) 0.02254(14) 0.02560(14) -0.00041(7) 0.00042(9) -0.00585(7) O12 0.0264(7) 0.0267(7) 0.0177(6) 0.0043(6) -0.0004(5) -0.0030(6) N10 0.0218(7) 0.0189(7) 0.0149(7) 0.0016(6) -0.0012(6) -0.0001(6) N2 0.0213(7) 0.0202(7) 0.0173(7) 0.0010(6) 0.0006(6) 0.0001(6) C4 0.0207(8) 0.0182(9) 0.0208(8) -0.0027(7) 0.0004(7) 0.0015(7) C11 0.0198(8) 0.0180(8) 0.0184(8) -0.0008(7) 0.0027(7) 0.0028(7) C13 0.0209(9) 0.0151(9) 0.0201(9) 0.0002(6) 0.0009(7) 0.0023(6) C1 0.0198(8) 0.0159(8) 0.0187(8) -0.0017(7) 0.0026(7) 0.0015(7) C18 0.0230(9) 0.0186(9) 0.0212(9) 0.0016(7) 0.0043(7) 0.0029(7) C7 0.0243(9) 0.0223(9) 0.0202(9) 0.0005(7) 0.0015(7) 0.0035(8) C3 0.0232(9) 0.0182(9) 0.0196(8) 0.0014(7) 0.0019(7) 0.0006(7) C8 0.0222(9) 0.0220(9) 0.0217(9) 0.0013(7) 0.0011(7) -0.0014(7) C14 0.0233(9) 0.0185(9) 0.0203(9) 0.0014(7) 0.0032(8) 0.0015(7) C6 0.0249(9) 0.0196(9) 0.0188(9) 0.0020(7) 0.0010(7) -0.0004(7) C15 0.0321(10) 0.0220(9) 0.0198(9) -0.0014(8) -0.0004(8) 0.0025(8) C17 0.0196(9) 0.0188(9) 0.0307(10) 0.0027(8) 0.0034(8) 0.0024(7) C5 0.0252(9) 0.0236(9) 0.0170(9) -0.0008(8) -0.0009(7) 0.0011(8) C16 0.0231(9) 0.0187(9) 0.0297(10) -0.0025(8) -0.0032(8) 0.0001(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l 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7650.43 361.291 3 -5 7 -2 15352 593.46 4 -5 -7 -2 15104.2 575.765 3 -5 7 -3 2440.05 188.622 4 -5 7 -3 2137.36 173.854 3 -5 -7 -3 2757.74 185.329 3 -5 7 -4 15334.6 559.35 2 -5 7 -4 17032.1 591.247 4 -5 7 -4 16098.3 568.245 3 -5 -7 -4 16131.8 568.242 3 -5 7 -5 12706.4 431.522 3 -5 -7 -5 13174 435.035 3 -5 7 -5 11725.7 422.377 2 5 -8 -8 171.981 60.8195 11 -5 8 8 104.713 63.3727 22 -5 8 7 21017.9 764.897 16 -5 8 7 23468.4 793.943 22 -5 8 6 18.2828 75.2297 16 -5 8 6 55.89 73.2802 22 -5 -8 5 11635.5 480.883 6 -5 8 5 12610.7 520.227 22 -5 -8 4 946.997 146.017 6 -5 8 4 867.828 130.415 22 -5 -8 3 22674.9 772.614 6 -5 8 3 19087.9 754.557 22 -5 8 2 775.605 138.075 17 -5 8 2 788.36 132.134 16 -5 -8 2 833.036 137.658 3 -5 8 2 558.45 122.21 3 -5 -8 2 1081.42 162.515 6 -5 8 2 602.974 104.055 22 -5 8 1 712.602 132.47 17 -5 8 1 698.354 123.468 16 -5 -8 1 620.555 127.798 3 -5 8 1 546.47 124.504 3 -5 -8 1 908.021 145.56 6 -5 8 1 659.114 98.8878 22 -5 8 0 1012.98 153.674 17 -5 8 0 1264.65 147.378 16 -5 8 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6629.33 289.421 4 5 -13 2 7459.19 286.703 5 -5 13 -3 6738.81 262.168 4 -5 13 -3 6701.85 271.751 2 -5 14 5 19439.9 653.718 22 5 -14 -5 19574.7 626.819 5 -5 -14 4 541.008 102.103 6 -5 14 4 576.135 89.7356 22 -5 -14 3 13931.2 505.589 6 -5 14 3 13075.6 494.335 22 -5 14 2 51.4 66.3804 17 -5 14 2 23.5928 60.1231 4 -5 14 2 -20.7071 59.6645 16 -5 -14 2 -6.21875 80.3516 6 -5 14 1 497.358 96.5854 17 -5 14 1 465.486 83.6719 4 -5 14 1 405.786 77.3527 16 -5 14 0 90.3821 66.1303 17 -5 14 0 26.8902 54.2206 4 -5 14 -1 15814.4 581.495 4 -5 14 -1 17149.2 623.726 17 -5 14 -2 4012.21 181.706 4 -5 -15 5 20.1416 59.8404 6 -5 -15 4 4744.22 239.061 6 5 -15 -4 5913 249.288 5 -5 15 3 1586.71 135.268 16 -5 -15 3 1731.73 141.587 6 5 -15 -3 2000.02 142.583 5 -5 15 2 3884.99 217.384 17 -5 15 2 3989.61 212.812 16 -5 -15 2 4247.3 215.997 6 -5 15 1 16376.9 594.086 17 5 -15 0 510.041 85.3552 5 -5 15 0 449.26 82.8644 17 5 -15 1 583.143 78.1778 5 5 -16 -4 574.459 73.1078 5 -5 -16 4 612.756 86.0926 6 -5 -16 3 1280.17 114.829 6 5 -16 -3 1566.23 119.181 5 5 -16 -2 26536.2 858.053 5 -5 -16 1 3225.38 175.877 6 5 -16 -1 3637.26 188.144 5 5 -16 0 18252.4 607.739 5 -5 -17 3 588.142 73.7776 6 5 -17 -3 653.083 74.7648 5 5 -17 -1 1535.7 109.647 5 -6 0 5 -45.6396 74.3352 16 -6 0 5 281.399 52.0053 22 -6 0 4 8317.43 353.906 16 -6 0 4 8441.25 346.154 22 -6 0 3 -41.0232 68.1104 16 -6 0 3 39.2166 75.8001 3 -6 0 2 7205.27 339.875 3 -6 0 1 -18.2565 58.8148 4 -6 0 1 -25.7614 61.0658 16 -6 0 1 -21.9509 75.4199 3 -6 0 0 3773.38 200.093 4 -6 0 0 3938.21 221.78 3 -6 0 -1 29.2788 58.3387 3 -6 0 -2 8813.84 345.325 3 -6 1 5 25004.2 791.495 16 -6 -1 5 22868.2 778.735 16 -6 1 5 23272.5 783.987 22 -6 -1 5 23379.9 785.324 22 -6 1 4 190.304 70.9363 16 -6 -1 4 109.115 63.2185 16 -6 1 4 86.4998 68.004 22 -6 -1 4 -29.1464 71.0126 22 -6 1 3 5825.29 299.072 3 -6 1 3 6064.94 289.434 16 -6 -1 3 6237.47 289.943 16 -6 1 2 8376.21 373.67 3 -6 -1 2 8497.67 361.111 16 -6 -1 1 1918.44 140.24 4 -6 1 1 1835.23 145.897 16 -6 1 1 1869.88 157.038 3 -6 1 0 10514.7 405.535 4 -6 1 0 10470.6 420.945 3 -6 1 -1 1304.28 104.461 4 -6 1 -1 1156.43 120.063 3 -6 1 -2 2681.62 160.234 3 -6 2 5 3766.38 205.892 16 -6 2 5 3781.16 199.806 22 -6 2 4 1575.69 133.583 16 -6 -2 4 1363.22 124.316 16 -6 2 4 1254.08 116.665 22 -6 2 3 7055.32 332.077 3 -6 2 3 7277.3 325.684 16 -6 -2 3 7312.3 323.101 16 -6 2 2 5279.16 271.949 3 -6 2 1 7181.36 313.702 16 -6 2 1 7118.57 326.327 3 -6 2 0 240.45 71.8465 4 -6 2 0 328.694 83.0663 3 -6 2 -1 4018.2 200.503 4 -6 2 -1 4197.83 216.063 3 -6 2 -2 2056.25 116.046 4 -6 2 -2 1732.02 125.437 3 -6 3 5 15479.3 552.513 16 -6 3 4 359.159 79.1965 16 -6 -3 4 229.017 83.0809 3 -6 3 4 506.772 98.7802 3 -6 3 3 5696.85 291.902 3 -6 -3 3 5889.3 293.946 3 -6 3 3 6220.2 287.553 16 -6 3 2 564.895 104.769 3 -6 -3 2 438.786 96.857 3 -6 3 1 726.136 95.7489 16 -6 3 1 718.887 108.078 3 -6 -3 1 674.909 103.799 3 -6 3 0 1001.28 105.862 4 -6 3 0 683.957 100.865 3 -6 -3 0 718.493 101.413 3 -6 3 -1 11439 406.715 4 -6 3 -1 10127.1 405.969 3 -6 -3 -1 10979.3 411.422 3 -6 3 -2 593.442 67.61 4 -6 3 -2 545.646 73.9837 3 -6 -3 -2 601.459 75.1472 3 -6 4 5 3285.56 184.928 16 -6 4 4 5959.5 283.207 3 -6 4 4 6275.95 280.491 16 -6 4 3 304.85 74.6816 3 -6 -4 3 308.883 73.6192 3 -6 4 2 5197.13 252.152 16 -6 4 2 4786.85 250.794 3 -6 -4 2 4727.63 250.614 3 -6 4 1 18933.7 646.396 16 -6 -4 1 20322.8 663.121 3 -6 4 0 585.881 90.377 4 -6 4 0 465.343 86.4628 3 -6 -4 0 430.987 82.3755 3 -6 4 -1 3079.28 171.02 4 -6 4 -1 2814.44 169.773 3 -6 -4 -1 3248.49 176.523 3 -6 4 -2 5487.27 219.909 4 -6 4 -2 4823.33 218.108 3 -6 -4 -2 5333.8 224.203 3 -6 -5 6 4579.64 210.017 3 -6 5 6 4361.69 209.116 3 -6 -5 5 892.564 99.6478 3 -6 5 5 802.701 99.3045 3 -6 5 4 712.723 91.3069 16 -6 5 4 593.906 97.473 3 -6 -5 4 548.161 91.6586 3 -6 -5 3 8288.13 338.167 3 -6 5 3 7980.33 336.187 16 -6 5 2 17992 614.4 16 -6 5 2 16445.9 606.131 3 -6 -5 2 17549.4 611.36 3 -6 5 1 43.8706 54.3119 16 -6 5 1 -115.867 83.7522 3 -6 5 0 23201.6 714.116 4 -6 -5 0 21368.3 698.394 3 -6 5 -1 8563.8 360.961 3 -6 -5 -1 10014.3 372.492 3 -6 5 -2 9590.97 342.214 4 -6 6 5 88.7106 55.3755 3 -6 -6 5 164.679 59.0037 3 -6 6 4 7635.35 319.529 3 -6 -6 4 7657.85 320.862 3 -6 6 4 8224.01 332.543 16 -6 6 3 -83.7164 82.5163 3 -6 -6 3 -121.724 82.2405 3 -6 6 2 6958.68 293.571 16 -6 6 2 6029.28 279.768 3 -6 -6 2 6689.57 288.163 3 -6 6 1 228.472 71.4624 3 -6 -6 1 275.69 73.3229 3 -6 6 0 31.3748 48.2011 3 -6 -6 0 54.6733 50.4583 3 -6 -6 -1 967.78 85.8005 3 -6 7 4 -21.0137 52.5692 3 -6 7 3 1435.01 124.758 3 -6 -7 3 1685.57 128.282 3 -6 7 2 3062.97 185.723 3 -6 -7 2 3744.05 193.764 3 -6 7 1 5104.06 246.749 3 -6 -7 1 6178.93 258.502 3 -6 7 0 19216.6 644.797 4 -6 8 1 3566.33 190.413 4 -6 8 0 592.494 77.4041 4 -6 8 -1 9696.73 346.766 4 -6 9 2 1722.97 124.896 4 -6 9 1 31.6754 48.901 4 -6 9 0 2580.17 140.417 4 -6 10 3 635.327 76.1987 4 -6 10 2 9045.47 336.252 4 -6 10 1 10348.4 367.883 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 C11 N10 C1 126.52(16) . . ? C11 N10 H10 120.5(16) . . ? C1 N10 H10 113.0(16) . . ? C3 N2 C1 117.68(15) . . ? C3 C4 C7 120.55(17) . . ? C5 C4 C7 122.44(17) . . ? C5 C4 C3 116.97(17) . . ? O12 C11 N10 123.78(17) . . ? O12 C11 C13 119.97(17) . . ? N10 C11 C13 116.24(15) . . ? C18 C13 C11 117.26(17) . . ? C18 C13 C14 119.80(17) . . ? C14 C13 C11 122.70(18) . . ? N2 C1 N10 113.41(15) . . ? N2 C1 C6 122.74(17) . . ? C6 C1 N10 123.82(17) . . ? C13 C18 H18 117.5(14) . . ? C17 C18 C13 120.17(18) . . ? C17 C18 H18 122.3(14) . . ? C8 C7 C4 175.9(2) . . ? N2 C3 C4 124.20(18) . . ? N2 C3 H3 115.1(13) . . ? C4 C3 H3 120.7(13) . . ? C7 C8 Br9 178.72(18) . . ? C13 C14 H14 122.4(13) . . ? C15 C14 C13 119.59(19) . . ? C15 C14 H14 118.0(13) . . ? C1 C6 H6 120.5(18) . . ? C5 C6 C1 118.36(18) . . ? C5 C6 H6 121.1(17) . . ? C14 C15 C16 120.58(18) . . ? C14 C15 H15 120.4(15) . . ? C16 C15 H15 119.0(15) . . ? C18 C17 C16 120.36(19) . . ? C18 C17 H17 119.5(16) . . ? C16 C17 H17 120.1(16) . . ? C4 C5 H5 119.7(15) . . ? C6 C5 C4 120.00(17) . . ? C6 C5 H5 120.3(15) . . ? C15 C16 H16 120.0(16) . . ? C17 C16 C15 119.49(18) . . ? C17 C16 H16 120.5(16) . . ? 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 Br9 C8 1.7987(19) . ? O12 C11 1.223(2) . ? N10 C11 1.374(2) . ? N10 C1 1.399(2) . ? N10 H10 0.82(2) . ? N2 C1 1.343(2) . ? N2 C3 1.335(2) . ? C4 C7 1.433(3) . ? C4 C3 1.396(3) . ? C4 C5 1.394(3) . ? C11 C13 1.501(2) . ? C13 C18 1.392(3) . ? C13 C14 1.395(3) . ? C1 C6 1.397(3) . ? C18 C17 1.387(3) . ? C18 H18 0.93(2) . ? C7 C8 1.192(3) . ? C3 H3 0.97(2) . ? C14 C15 1.391(3) . ? C14 H14 0.93(2) . ? C6 C5 1.383(3) . ? C6 H6 0.85(3) . ? C15 C16 1.392(3) . ? C15 H15 0.97(3) . ? C17 C16 1.388(3) . ? C17 H17 0.91(3) . ? C5 H5 0.98(2) . ? C16 H16 0.97(3) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 C11 C13 C18 32.5(3) . . . . ? O12 C11 C13 C14 -141.86(19) . . . . ? N10 C11 C13 C18 -148.76(17) . . . . ? N10 C11 C13 C14 36.9(2) . . . . ? N10 C1 C6 C5 178.75(17) . . . . ? N2 C1 C6 C5 0.5(3) . . . . ? C11 N10 C1 N2 174.24(16) . . . . ? C11 N10 C1 C6 -4.2(3) . . . . ? C11 C13 C18 C17 -175.31(17) . . . . ? C11 C13 C14 C15 174.39(17) . . . . ? C13 C18 C17 C16 0.9(3) . . . . ? C13 C14 C15 C16 0.3(3) . . . . ? C1 N10 C11 O12 7.5(3) . . . . ? C1 N10 C11 C13 -171.19(16) . . . . ? C1 N2 C3 C4 -1.8(3) . . . . ? C1 C6 C5 C4 0.6(3) . . . . ? C18 C13 C14 C15 0.2(3) . . . . ? C18 C17 C16 C15 -0.4(3) . . . . ? C7 C4 C3 N2 -174.86(18) . . . . ? C7 C4 C5 C6 175.49(18) . . . . ? C3 N2 C1 N10 -178.38(16) . . . . ? C3 N2 C1 C6 0.0(3) . . . . ? C3 C4 C5 C6 -2.2(3) . . . . ? C14 C13 C18 C17 -0.8(3) . . . . ? C14 C15 C16 C17 -0.2(3) . . . . ? C5 C4 C3 N2 2.8(3) . . . . ?