#------------------------------------------------------------------------------ #$Date: 2019-11-17 05:23:22 +0200 (Sun, 17 Nov 2019) $ #$Revision: 228107 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/11/7121127.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_7121127 loop_ _publ_author_name 'Kubanik, Mario' 'Lam, Nelson Y. S.' 'Holtkamp, Hannah U.' 'S\"ohnel, Tilo' 'Anderson, Robert F.' 'Jamieson, Stephen M. F.' 'Hartinger, Christian G.' _publ_section_title ; Quinoline-para-quinones and metals: coordination-assisted formation of quinoline-ortho-quinones. ; _journal_issue 8 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 992 _journal_page_last 995 _journal_paper_doi 10.1039/c7cc09478g _journal_volume 54 _journal_year 2018 _chemical_formula_moiety 'C10 H6 Cl3 N O2' _chemical_formula_sum 'C10 H6 Cl3 N O2' _chemical_formula_weight 278.51 _chemical_name_systematic ; 5,6,7-Trichloro-2-methoxy-8-hydroxyquinoline ; _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 _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2017-08-31 deposited with the CCDC. 2018-01-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 111.532(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 21.1155(9) _cell_length_b 4.9816(2) _cell_length_c 21.6442(8) _cell_measurement_reflns_used 9911 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.128 _cell_measurement_theta_min 3.221 _cell_volume 2117.84(15) _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXS-2016/6 (Sheldrick, 2016)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_unetI/netI 0.0528 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 21650 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.246 _diffrn_reflns_theta_min 1.905 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _exptl_absorpt_coefficient_mu 0.845 _exptl_absorpt_correction_T_max 0.8865 _exptl_absorpt_correction_T_min 0.701699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2004/1 (Bruker,2004) was used for absorption correction. R(int) was 0.0981 before and 0.0489 after correction. The Ratio of minimum to maximum transmission is 0.7017. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.747 _exptl_crystal_description needle _exptl_crystal_F_000 1120 _exptl_crystal_size_max 0.420 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.340 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.079 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 291 _refine_ls_number_reflns 3794 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0402 _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^)+(0.0504P)^2^+0.8843P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0944 _refine_ls_wR_factor_ref 0.1081 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2604 _reflns_number_total 3794 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7cc09478g2.cif _cod_data_source_block maku052a_0m _cod_depositor_comments 'Adding full bibliography for 7121127--7121131.cif.' _cod_database_code 7121127 _shelx_shelxl_version_number 2016/6 _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_min 0.718 _shelx_estimated_absorpt_t_max 0.935 _shelx_res_file ; TITL MaKu052a_0m in P2(1)/c maku052a_0m.res created by SHELXL-2016/6 at 13:47:20 on 31-Aug-2017 CELL 0.71073 21.1155 4.9816 21.6442 90.000 111.532 90.000 ZERR 8.00 0.0009 0.0002 0.0008 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O CL UNIT 80 48 8 16 24 MERG 2 OMIT -2.00 50.50 OMIT 1 0 2 FMAP 2 PLAN 25 SIZE 0.080 0.100 0.420 ACTA L.S. 10 TEMP -173.00 WGHT 0.050400 0.884300 FVAR 0.20128 C1 1 0.739609 0.810768 1.203755 11.00000 0.01739 0.01746 = 0.02112 0.00254 0.01092 0.00088 C1A 1 0.764967 1.151646 1.048675 11.00000 0.02240 0.01846 = 0.02246 -0.00092 0.01472 -0.00060 C2 1 0.691147 0.782629 1.138227 11.00000 0.02368 0.02346 = 0.01740 -0.00352 0.01204 -0.00391 AFIX 43 H2 2 0.697183 0.651579 1.108976 11.00000 -1.20000 AFIX 0 C2A 1 0.811692 1.160856 1.115276 11.00000 0.02362 0.02093 = 0.01881 -0.00389 0.01254 -0.00378 AFIX 43 H2A 2 0.805984 1.286330 1.145877 11.00000 -1.20000 AFIX 0 C3 1 0.635918 0.946941 1.118152 11.00000 0.01882 0.02505 = 0.01306 -0.00092 0.00526 -0.00367 AFIX 43 H3 2 0.603282 0.934721 1.074196 11.00000 -1.20000 AFIX 0 C3A 1 0.864720 0.986533 1.134326 11.00000 0.02033 0.02284 = 0.01555 -0.00205 0.00747 -0.00649 AFIX 43 H3A 2 0.896040 0.985660 1.178986 11.00000 -1.20000 AFIX 0 C4 1 0.627249 1.138947 1.163802 11.00000 0.01542 0.01918 = 0.01829 0.00356 0.00805 -0.00422 C4A 1 0.873384 0.804216 1.087095 11.00000 0.01417 0.01985 = 0.01586 0.00092 0.00560 -0.00381 C5 1 0.571821 1.318056 1.149027 11.00000 0.01380 0.02306 = 0.01480 0.00177 0.00304 0.00147 C5A 1 0.926643 0.614703 1.100853 11.00000 0.01549 0.02184 = 0.01305 0.00202 0.00218 -0.00235 C6 1 0.566905 1.494104 1.195832 11.00000 0.01397 0.02308 = 0.02277 0.00625 0.00861 -0.00057 C6A 1 0.931770 0.449213 1.052128 11.00000 0.01857 0.01703 = 0.02129 0.00267 0.00907 -0.00050 C7 1 0.617731 1.494794 1.260204 11.00000 0.01610 0.01906 = 0.01758 -0.00147 0.00852 -0.00393 C7A 1 0.882458 0.468565 0.986906 11.00000 0.01784 0.01901 = 0.01476 -0.00226 0.00643 -0.00278 C8 1 0.672575 1.324412 1.276148 11.00000 0.01707 0.01591 = 0.01558 0.00065 0.00719 -0.00520 C8A 1 0.830183 0.649174 0.971667 11.00000 0.01351 0.02043 = 0.01246 0.00078 0.00252 -0.00563 C9 1 0.678315 1.144441 1.227806 11.00000 0.01686 0.01445 = 0.01551 0.00264 0.00763 -0.00205 C9A 1 0.824701 0.816337 1.022382 11.00000 0.01462 0.01895 = 0.01598 0.00001 0.00787 -0.00194 C10 1 0.845951 0.677314 1.284438 11.00000 0.02050 0.03815 = 0.01916 0.00472 0.00407 0.01062 AFIX 137 H10A 2 0.882938 0.549390 1.290160 11.00000 -1.50000 H10B 2 0.826689 0.645918 1.318678 11.00000 -1.50000 H10C 2 0.863763 0.860798 1.288490 11.00000 -1.50000 AFIX 0 C10A 1 0.661502 1.309723 0.967143 11.00000 0.02308 0.04277 = 0.02226 0.00756 0.00395 0.01753 AFIX 137 H10D 2 0.682976 1.343051 0.934688 11.00000 -1.50000 H10E 2 0.626097 1.444595 0.961823 11.00000 -1.50000 H10F 2 0.641015 1.130351 0.959916 11.00000 -1.50000 AFIX 0 N1 3 0.734593 0.981482 1.247609 11.00000 0.01571 0.02109 = 0.01423 0.00339 0.00584 0.00095 N1A 3 0.770042 0.989974 1.002837 11.00000 0.01793 0.01921 = 0.01668 0.00182 0.00903 0.00034 O1 4 0.720546 1.326208 1.338254 11.00000 0.01588 0.02394 = 0.01538 -0.00193 0.00246 0.00266 AFIX 83 H1 2 0.750763 1.212488 1.340758 11.00000 -1.50000 AFIX 0 O1A 4 0.783872 0.666063 0.908723 11.00000 0.01684 0.02554 = 0.01408 -0.00255 0.00178 0.00666 AFIX 83 H1A 2 0.754963 0.784603 0.906946 11.00000 -1.50000 AFIX 0 O2 4 0.793591 0.641712 1.219584 11.00000 0.01948 0.02846 = 0.02044 0.00019 0.00789 0.00587 O2A 4 0.712272 1.326206 1.033520 11.00000 0.02196 0.02765 = 0.02022 -0.00139 0.00808 0.00877 CL1 5 0.612060 1.710907 1.320534 11.00000 0.02251 0.02181 = 0.02353 -0.00516 0.01088 0.00039 CL1A 5 0.887308 0.261459 0.924312 11.00000 0.02113 0.02284 = 0.01890 -0.00491 0.00708 0.00258 CL2 5 0.500577 1.719879 1.177133 11.00000 0.02061 0.02731 = 0.03181 0.00554 0.00973 0.00478 CL2A 5 0.995864 0.216860 1.068330 11.00000 0.02026 0.02780 = 0.02919 0.00242 0.00756 0.00367 CL3 5 0.510352 1.317755 1.069259 11.00000 0.02433 0.04231 = 0.01568 0.00296 -0.00048 0.00704 CL3A 5 0.985965 0.590738 1.181446 11.00000 0.02529 0.03979 = 0.01588 0.00043 0.00002 0.00671 HKLF 4 REM MaKu052a_0m in P2(1)/c REM R1 = 0.0402 for 2604 Fo > 4sig(Fo) and 0.0724 for all 3794 data REM 291 parameters refined using 0 restraints END WGHT 0.0504 0.8843 REM Highest difference peak 0.340, deepest hole -0.501, 1-sigma level 0.079 Q1 1 0.5786 1.4581 1.1710 11.00000 0.05 0.34 Q2 1 0.9128 0.5427 1.2161 11.00000 0.05 0.33 Q3 1 0.9778 0.8209 1.1689 11.00000 0.05 0.32 Q4 1 0.8384 0.7677 0.9964 11.00000 0.05 0.31 Q5 1 0.5855 1.1839 1.1632 11.00000 0.05 0.31 Q6 1 0.8391 0.5263 0.9848 11.00000 0.05 0.30 Q7 1 0.9102 0.8026 1.0891 11.00000 0.05 0.30 Q8 1 0.9182 0.4985 1.0182 11.00000 0.05 0.30 Q9 1 0.7025 0.7336 1.1710 11.00000 0.05 0.29 Q10 1 0.5799 1.8431 1.2883 11.00000 0.05 0.29 Q11 1 0.8177 0.6957 1.0025 11.00000 0.05 0.29 Q12 1 0.6107 1.9318 1.2922 11.00000 0.05 0.28 Q13 1 0.6803 1.2713 1.2477 11.00000 0.05 0.28 Q14 1 0.5963 1.5119 1.2193 11.00000 0.05 0.27 Q15 1 0.7179 0.6313 1.0871 11.00000 0.05 0.27 Q16 1 0.8349 0.6199 1.1215 11.00000 0.05 0.26 Q17 1 0.6592 1.2024 1.1852 11.00000 0.05 0.26 Q18 1 0.6116 1.3054 1.1512 11.00000 0.05 0.26 Q19 1 0.8571 0.8836 1.0473 11.00000 0.05 0.26 Q20 1 0.7995 0.9080 1.0130 11.00000 0.05 0.25 Q21 1 0.5572 1.3389 1.1810 11.00000 0.05 0.25 Q22 1 0.7833 1.1053 1.0852 11.00000 0.05 0.25 Q23 1 0.6310 1.5926 1.3512 11.00000 0.05 0.25 Q24 1 1.0510 0.2074 1.1218 11.00000 0.05 0.24 Q25 1 0.9925 1.0637 1.2120 11.00000 0.05 0.24 ; _shelx_res_checksum 41976 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 C1 C 0.73961(17) 0.8108(7) 1.20375(15) 0.0176(7) Uani 1 1 d . . C1A C 0.76497(17) 1.1516(6) 1.04867(16) 0.0193(8) Uani 1 1 d . . C2 C 0.69115(18) 0.7826(7) 1.13823(15) 0.0202(8) Uani 1 1 d . . H2 H 0.697183 0.651579 1.108976 0.024 Uiso 1 1 calc R U C2A C 0.81169(17) 1.1609(7) 1.11528(15) 0.0198(8) Uani 1 1 d . . H2A H 0.805984 1.286330 1.145877 0.024 Uiso 1 1 calc R U C3 C 0.63592(17) 0.9469(7) 1.11815(15) 0.0191(8) Uani 1 1 d . . H3 H 0.603282 0.934721 1.074196 0.023 Uiso 1 1 calc R U C3A C 0.86472(17) 0.9865(7) 1.13433(15) 0.0193(8) Uani 1 1 d . . H3A H 0.896040 0.985660 1.178986 0.023 Uiso 1 1 calc R U C4 C 0.62725(16) 1.1389(6) 1.16380(15) 0.0171(7) Uani 1 1 d . . C4A C 0.87338(16) 0.8042(6) 1.08710(15) 0.0166(7) Uani 1 1 d . . C5 C 0.57182(17) 1.3181(7) 1.14903(15) 0.0178(7) Uani 1 1 d . . C5A C 0.92664(17) 0.6147(6) 1.10085(15) 0.0177(7) Uani 1 1 d . . C6 C 0.56690(16) 1.4941(7) 1.19583(15) 0.0194(8) Uani 1 1 d . . C6A C 0.93177(17) 0.4492(6) 1.05213(15) 0.0185(7) Uani 1 1 d . . C7 C 0.61773(16) 1.4948(6) 1.26020(15) 0.0169(7) Uani 1 1 d . . C7A C 0.88246(16) 0.4686(6) 0.98691(14) 0.0171(7) Uani 1 1 d . . C8 C 0.67257(17) 1.3244(6) 1.27615(15) 0.0158(7) Uani 1 1 d . . C8A C 0.83018(16) 0.6492(6) 0.97167(15) 0.0161(7) Uani 1 1 d . . C9 C 0.67832(17) 1.1444(6) 1.22781(15) 0.0151(7) Uani 1 1 d . . C9A C 0.82470(17) 0.8163(6) 1.02238(15) 0.0159(7) Uani 1 1 d . . C10 C 0.84595(18) 0.6773(8) 1.28444(16) 0.0268(9) Uani 1 1 d . . H10A H 0.882938 0.549390 1.290160 0.040 Uiso 1 1 calc R U H10B H 0.826689 0.645918 1.318678 0.040 Uiso 1 1 calc R U H10C H 0.863763 0.860798 1.288490 0.040 Uiso 1 1 calc R U C10A C 0.66150(19) 1.3097(8) 0.96714(16) 0.0306(9) Uani 1 1 d . . H10D H 0.682976 1.343051 0.934688 0.046 Uiso 1 1 calc R U H10E H 0.626097 1.444595 0.961823 0.046 Uiso 1 1 calc R U H10F H 0.641015 1.130351 0.959916 0.046 Uiso 1 1 calc R U N1 N 0.73459(13) 0.9815(5) 1.24761(12) 0.0169(6) Uani 1 1 d . . N1A N 0.77004(14) 0.9900(5) 1.00284(12) 0.0172(6) Uani 1 1 d . . O1 O 0.72055(11) 1.3262(4) 1.33825(10) 0.0193(5) Uani 1 1 d . . H1 H 0.750763 1.212488 1.340758 0.029 Uiso 1 1 calc R U O1A O 0.78387(11) 0.6661(4) 0.90872(10) 0.0199(5) Uani 1 1 d . . H1A H 0.754963 0.784603 0.906946 0.030 Uiso 1 1 calc R U O2 O 0.79359(12) 0.6417(5) 1.21958(11) 0.0226(6) Uani 1 1 d . . O2A O 0.71227(12) 1.3262(5) 1.03352(11) 0.0232(6) Uani 1 1 d . . Cl1 Cl 0.61206(4) 1.71091(16) 1.32053(4) 0.0219(2) Uani 1 1 d . . Cl1A Cl 0.88731(4) 0.26146(16) 0.92431(4) 0.0210(2) Uani 1 1 d . . Cl2 Cl 0.50058(4) 1.71988(18) 1.17713(4) 0.0265(2) Uani 1 1 d . . Cl2A Cl 0.99586(4) 0.21686(17) 1.06833(4) 0.0262(2) Uani 1 1 d . . Cl3 Cl 0.51035(5) 1.31775(19) 1.06926(4) 0.0297(2) Uani 1 1 d . . Cl3A Cl 0.98597(5) 0.59074(19) 1.18145(4) 0.0291(2) Uani 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 C1 0.017(2) 0.0175(18) 0.0211(17) 0.0025(13) 0.0109(15) 0.0009(14) C1A 0.022(2) 0.0185(19) 0.0225(18) -0.0009(14) 0.0147(16) -0.0006(15) C2 0.024(2) 0.023(2) 0.0174(17) -0.0035(14) 0.0120(16) -0.0039(15) C2A 0.024(2) 0.021(2) 0.0188(17) -0.0039(13) 0.0125(16) -0.0038(15) C3 0.019(2) 0.025(2) 0.0131(16) -0.0009(13) 0.0053(15) -0.0037(15) C3A 0.020(2) 0.023(2) 0.0155(16) -0.0020(13) 0.0075(15) -0.0065(15) C4 0.0154(19) 0.0192(19) 0.0183(17) 0.0036(13) 0.0081(15) -0.0042(14) C4A 0.0142(19) 0.0199(18) 0.0159(16) 0.0009(13) 0.0056(15) -0.0038(14) C5 0.0138(19) 0.0231(19) 0.0148(16) 0.0018(13) 0.0030(14) 0.0015(15) C5A 0.0155(19) 0.0218(19) 0.0130(16) 0.0020(13) 0.0022(14) -0.0023(14) C6 0.0140(19) 0.023(2) 0.0228(18) 0.0062(14) 0.0086(15) -0.0006(14) C6A 0.0186(19) 0.0170(18) 0.0213(17) 0.0027(13) 0.0091(15) -0.0005(14) C7 0.0161(19) 0.0191(19) 0.0176(16) -0.0015(13) 0.0085(15) -0.0039(14) C7A 0.018(2) 0.0190(19) 0.0148(16) -0.0023(13) 0.0064(14) -0.0028(14) C8 0.0171(19) 0.0159(18) 0.0156(16) 0.0006(12) 0.0072(15) -0.0052(14) C8A 0.0135(19) 0.0204(19) 0.0125(16) 0.0008(12) 0.0025(14) -0.0056(14) C9 0.0169(19) 0.0145(18) 0.0155(16) 0.0026(12) 0.0076(15) -0.0020(14) C9A 0.0146(19) 0.0190(18) 0.0160(16) 0.0000(13) 0.0079(14) -0.0019(14) C10 0.020(2) 0.038(2) 0.0192(18) 0.0047(15) 0.0041(16) 0.0106(17) C10A 0.023(2) 0.043(2) 0.0223(19) 0.0076(16) 0.0040(17) 0.0175(18) N1 0.0157(16) 0.0211(16) 0.0142(13) 0.0034(11) 0.0058(12) 0.0009(12) N1A 0.0179(16) 0.0192(16) 0.0167(14) 0.0018(11) 0.0090(12) 0.0003(12) O1 0.0159(13) 0.0239(13) 0.0154(12) -0.0019(9) 0.0025(10) 0.0027(10) O1A 0.0168(13) 0.0255(13) 0.0141(11) -0.0025(9) 0.0018(10) 0.0067(10) O2 0.0195(14) 0.0285(15) 0.0204(12) 0.0002(10) 0.0079(11) 0.0059(11) O2A 0.0220(15) 0.0277(14) 0.0202(12) -0.0014(10) 0.0081(11) 0.0088(11) Cl1 0.0225(5) 0.0218(5) 0.0235(4) -0.0052(3) 0.0109(4) 0.0004(4) Cl1A 0.0211(5) 0.0228(5) 0.0189(4) -0.0049(3) 0.0071(4) 0.0026(3) Cl2 0.0206(5) 0.0273(5) 0.0318(5) 0.0055(4) 0.0097(4) 0.0048(4) Cl2A 0.0203(5) 0.0278(5) 0.0292(5) 0.0024(4) 0.0076(4) 0.0037(4) Cl3 0.0243(5) 0.0423(6) 0.0157(4) 0.0030(4) -0.0005(4) 0.0070(4) Cl3A 0.0253(5) 0.0398(6) 0.0159(4) 0.0004(4) 0.0000(4) 0.0067(4) 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' Cl Cl 0.1484 0.1585 '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 N1 C1 O2 120.3(3) N1 C1 C2 124.7(3) O2 C1 C2 115.0(3) N1A C1A O2A 119.9(3) N1A C1A C2A 124.7(3) O2A C1A C2A 115.4(3) C3 C2 C1 118.7(3) C3A C2A C1A 118.5(3) C2 C3 C4 119.5(3) C2A C3A C4A 119.9(3) C9 C4 C5 118.8(3) C9 C4 C3 116.4(3) C5 C4 C3 124.8(3) C9A C4A C5A 118.3(3) C9A C4A C3A 116.6(3) C5A C4A C3A 125.1(3) C6 C5 C4 121.2(3) C6 C5 Cl3 120.2(3) C4 C5 Cl3 118.6(2) C6A C5A C4A 121.3(3) C6A C5A Cl3A 119.9(3) C4A C5A Cl3A 118.8(2) C5 C6 C7 119.6(3) C5 C6 Cl2 121.2(3) C7 C6 Cl2 119.2(2) C5A C6A C7A 119.2(3) C5A C6A Cl2A 121.7(3) C7A C6A Cl2A 119.0(2) C8 C7 C6 120.8(3) C8 C7 Cl1 118.7(2) C6 C7 Cl1 120.5(3) C8A C7A C6A 121.2(3) C8A C7A Cl1A 118.5(2) C6A C7A Cl1A 120.3(3) O1 C8 C7 120.0(3) O1 C8 C9 120.1(3) C7 C8 C9 119.9(3) O1A C8A C7A 120.2(3) O1A C8A C9A 120.5(3) C7A C8A C9A 119.2(3) N1 C9 C4 123.9(3) N1 C9 C8 116.3(3) C4 C9 C8 119.8(3) N1A C9A C4A 123.9(3) N1A C9A C8A 115.4(3) C4A C9A C8A 120.7(3) C1 N1 C9 116.7(3) C1A N1A C9A 116.4(3) C1 O2 C10 116.2(3) C1A O2A C10A 116.6(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N1 1.307(4) C1 O2 1.356(4) C1 C2 1.419(4) C1A N1A 1.312(4) C1A O2A 1.354(4) C1A C2A 1.418(4) C2 C3 1.359(5) C2A C3A 1.356(5) C3 C4 1.434(4) C3A C4A 1.429(4) C4 C9 1.409(4) C4 C5 1.412(5) C4A C9A 1.402(4) C4A C5A 1.414(5) C5 C6 1.372(4) C5 Cl3 1.738(3) C5A C6A 1.374(4) C5A Cl3A 1.738(3) C6 C7 1.413(4) C6 Cl2 1.725(3) C6A C7A 1.417(4) C6A Cl2A 1.716(3) C7 C8 1.374(4) C7 Cl1 1.730(3) C7A C8A 1.367(4) C7A Cl1A 1.736(3) C8 O1 1.354(4) C8 C9 1.416(4) C8A O1A 1.357(3) C8A C9A 1.416(4) C9 N1 1.371(4) C9A N1A 1.379(4) C10 O2 1.444(4) C10A O2A 1.446(4)