#------------------------------------------------------------------------------ #$Date: 2024-10-05 15:36:36 +0300 (Sat, 05 Oct 2024) $ #$Revision: 295074 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/16/01/7160170.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_7160170 loop_ _publ_author_name 'Punna, Shiva Kumar' 'Arockiaraj, Mariyaraj' 'Rajeshkumar, Venkatachalam' _publ_section_title ; I2-catalyzed tandem sp3 C-H oxidation and annulation of aryl methyl ketones with amidoximes for the synthesis of 5-aroyl-1,2,4-oxadiazoles. ; _journal_issue 36 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 7478 _journal_page_last 7484 _journal_paper_doi 10.1039/d4ob01221f _journal_volume 22 _journal_year 2024 _chemical_formula_moiety 'C16 H7 Cl2 F3 N2 O2' _chemical_formula_sum 'C16 H7 Cl2 F3 N2 O2' _chemical_formula_weight 387.14 _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 geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2024-04-30 deposited with the CCDC. 2024-08-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.638(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.6950(5) _cell_length_b 13.3275(11) _cell_length_c 15.5682(14) _cell_measurement_reflns_used 4960 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 55.874 _cell_measurement_theta_min 6.069 _cell_volume 1593.4(2) _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SIR92 (Altornare et al., 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Bruker axs kappa apex2 CCD Diffractometer' _diffrn_measurement_method '\w and \f scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_unetI/netI 0.0348 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 17321 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.405 _diffrn_reflns_theta_min 2.622 _exptl_absorpt_coefficient_mu 0.453 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_correction_T_min 0.805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.614 _exptl_crystal_description block _exptl_crystal_F_000 776 _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _refine_diff_density_max 0.683 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.060 _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 226 _refine_ls_number_reflns 3971 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.1071 _refine_ls_R_factor_gt 0.0592 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0929P)^2^+0.7942P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1628 _refine_ls_wR_factor_ref 0.1949 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2286 _reflns_number_total 3971 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ob01221f2.cif _cod_data_source_block shelx_CCDC1 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7160170 _shelx_shelxl_version_number 2014/7 _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 0.805 _shelx_estimated_absorpt_t_max 0.876 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL Ex_SK_AR in P2(1)/c CELL 0.71073 7.6950 13.3275 15.5682 90.000 93.638 90.000 ZERR 4.00 0.0005 0.0011 0.0014 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O F CL UNIT 64 28 8 8 12 8 MERG 2 HTAB C16 N1 HTAB C1 O2_$1 EQIV $1 -x+3, y-1/2, -z+1/2 MORE -1 FMAP 2 PLAN 20 SIZE 0.300 0.400 0.500 ACTA HTAB 2.00000 BOND $H CONF L.S. 20 TEMP 23.00 WGHT 0.092900 0.794200 FVAR 0.13507 C1 1 1.490536 0.629938 0.224389 11.00000 0.05447 0.06533 = 0.05756 0.00201 -0.00170 0.01371 AFIX 43 H1 2 1.551388 0.573536 0.244631 11.00000 -1.20000 AFIX 0 C2 1 1.570456 0.722667 0.221344 11.00000 0.04417 0.07790 = 0.04853 -0.00329 -0.00150 0.00426 C3 1 1.483506 0.806880 0.191599 11.00000 0.04735 0.06131 = 0.05444 0.00097 -0.00105 -0.00709 AFIX 43 H3 2 1.540047 0.868513 0.190768 11.00000 -1.20000 AFIX 0 C4 1 1.308843 0.798454 0.162627 11.00000 0.04522 0.05136 = 0.04822 -0.00132 -0.00391 -0.00141 C5 1 1.220712 0.892753 0.133244 11.00000 0.05841 0.05149 = 0.05197 0.00113 -0.00783 -0.00528 C6 1 1.038373 0.888637 0.092189 11.00000 0.05603 0.04185 = 0.05468 0.00297 -0.00288 0.00269 C7 1 0.796520 0.857012 0.030595 11.00000 0.04898 0.04542 = 0.05143 0.00537 0.00041 0.00744 C8 1 0.651908 0.798895 -0.009628 11.00000 0.04650 0.04651 = 0.04786 0.00506 0.00225 0.00595 C9 1 0.497375 0.844578 -0.039031 11.00000 0.05423 0.04834 = 0.05609 -0.00108 -0.00266 0.01174 AFIX 43 H9 2 0.488266 0.914150 -0.038285 11.00000 -1.20000 AFIX 0 C10 1 0.356972 0.787322 -0.069407 11.00000 0.04758 0.06250 = 0.05662 0.00395 -0.00371 0.01249 AFIX 43 H10 2 0.253179 0.818263 -0.088334 11.00000 -1.20000 AFIX 0 C11 1 0.370972 0.684213 -0.071618 11.00000 0.04619 0.05856 = 0.05207 0.00266 0.00355 -0.00034 C12 1 0.219179 0.620827 -0.099097 11.00000 0.05431 0.07141 = 0.06726 0.00008 -0.00125 -0.00367 C13 1 0.666873 0.695673 -0.014645 11.00000 0.04766 0.05116 = 0.08333 0.00639 -0.00717 0.00739 AFIX 43 H13 2 0.771275 0.664650 0.003156 11.00000 -1.20000 AFIX 0 C14 1 0.527851 0.638851 -0.045868 11.00000 0.05653 0.04649 = 0.08929 0.00234 -0.00510 0.00144 AFIX 43 H14 2 0.539064 0.569546 -0.049750 11.00000 -1.20000 AFIX 0 C15 1 1.316426 0.624168 0.196162 11.00000 0.05455 0.04954 = 0.06079 0.00167 -0.00246 0.00382 C16 1 1.225125 0.706147 0.164791 11.00000 0.04518 0.05161 = 0.05730 0.00318 -0.00525 0.00235 AFIX 43 H16 2 1.108870 0.700048 0.145249 11.00000 -1.20000 AFIX 0 N1 3 0.955992 0.815177 0.054556 11.00000 0.04854 0.04407 = 0.06113 0.00267 -0.00723 0.00330 N2 3 0.783137 0.950626 0.052316 11.00000 0.06133 0.05022 = 0.08545 -0.00607 -0.01476 0.01175 O1 4 0.946528 0.973464 0.092969 11.00000 0.06299 0.04664 = 0.08846 -0.00863 -0.01724 0.00728 O2 4 1.286803 0.974180 0.142594 11.00000 0.08359 0.05342 = 0.09378 0.00722 -0.02830 -0.01619 F1 5 0.095927 0.667002 -0.142271 11.00000 0.09771 0.12581 = 0.24566 0.05123 -0.09625 -0.03430 F2 5 0.256893 0.546662 -0.147144 11.00000 0.08869 0.16905 = 0.22218 -0.12683 0.01570 -0.03288 F3 5 0.144546 0.582537 -0.034821 11.00000 0.13852 0.18535 = 0.10127 0.00652 0.01376 -0.10398 CL1 6 1.787796 0.732339 0.256627 11.00000 0.04475 0.11531 = 0.10055 0.00425 -0.01261 0.00361 CL2 6 1.212308 0.508789 0.198578 11.00000 0.08140 0.05389 = 0.12780 0.01762 -0.01863 -0.00374 HKLF 4 REM Ex_SK_AR in P2(1)/c REM R1 = 0.0592 for 2286 Fo > 4sig(Fo) and 0.1071 for all 3971 data REM 226 parameters refined using 0 restraints END WGHT 0.0893 0.7884 REM Instructions for potential hydrogen bonds HTAB C1 O2_$1 HTAB C16 N1 REM Highest difference peak 0.683, deepest hole -0.406, 1-sigma level 0.060 Q1 1 0.2316 0.5207 -0.0767 11.00000 0.05 0.68 Q2 1 0.0777 0.6537 -0.0707 11.00000 0.05 0.59 Q3 1 0.1831 0.6137 -0.1758 11.00000 0.05 0.50 Q4 1 1.1943 0.5502 0.2461 11.00000 0.05 0.37 Q5 1 0.1436 0.5795 -0.0140 11.00000 0.05 0.25 Q6 1 1.7910 0.7017 0.2038 11.00000 0.05 0.24 Q7 1 1.2803 0.5229 0.1533 11.00000 0.05 0.23 Q8 1 0.2899 0.5418 -0.1604 11.00000 0.05 0.23 Q9 1 1.8142 0.6648 0.2568 11.00000 0.05 0.17 Q10 1 0.0902 0.6961 -0.1453 11.00000 0.05 0.16 Q11 1 1.0061 0.8046 -0.0538 11.00000 0.05 0.15 Q12 1 1.9137 0.7447 0.1863 11.00000 0.05 0.15 Q13 1 0.6737 0.8062 -0.1215 11.00000 0.05 0.14 Q14 1 0.6836 0.7384 -0.1178 11.00000 0.05 0.14 Q15 1 0.9170 0.6172 0.1639 11.00000 0.05 0.13 Q16 1 0.8150 0.8650 -0.1010 11.00000 0.05 0.13 Q17 1 0.0666 0.8818 -0.0747 11.00000 0.05 0.13 Q18 1 0.6547 0.6770 0.0717 11.00000 0.05 0.13 Q19 1 1.0674 0.7183 0.1815 11.00000 0.05 0.13 Q20 1 0.4174 0.8617 -0.1302 11.00000 0.05 0.13 ; _shelx_res_checksum 71657 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 C1 C 1.4905(4) 0.6299(3) 0.2244(2) 0.0593(8) Uani 1 1 d . . . . . H1 H 1.5514 0.5735 0.2446 0.071 Uiso 1 1 calc R U . . . C2 C 1.5705(4) 0.7227(3) 0.22134(19) 0.0571(8) Uani 1 1 d . . . . . C3 C 1.4835(4) 0.8069(2) 0.19160(19) 0.0545(7) Uani 1 1 d . . . . . H3 H 1.5400 0.8685 0.1908 0.065 Uiso 1 1 calc R U . . . C4 C 1.3088(3) 0.7985(2) 0.16263(18) 0.0486(7) Uani 1 1 d . . . . . C5 C 1.2207(4) 0.8928(2) 0.13324(19) 0.0544(7) Uani 1 1 d . . . . . C6 C 1.0384(4) 0.8886(2) 0.09219(19) 0.0511(7) Uani 1 1 d . . . . . C7 C 0.7965(3) 0.8570(2) 0.03059(18) 0.0487(6) Uani 1 1 d . . . . . C8 C 0.6519(3) 0.7989(2) -0.00963(18) 0.0470(6) Uani 1 1 d . . . . . C9 C 0.4974(4) 0.8446(2) -0.03903(19) 0.0531(7) Uani 1 1 d . . . . . H9 H 0.4883 0.9142 -0.0383 0.064 Uiso 1 1 calc R U . . . C10 C 0.3570(4) 0.7873(2) -0.0694(2) 0.0559(7) Uani 1 1 d . . . . . H10 H 0.2532 0.8183 -0.0883 0.067 Uiso 1 1 calc R U . . . C11 C 0.3710(3) 0.6842(2) -0.07162(19) 0.0523(7) Uani 1 1 d . . . . . C12 C 0.2192(4) 0.6208(3) -0.0991(2) 0.0645(8) Uani 1 1 d . . . . . C13 C 0.6669(4) 0.6957(2) -0.0146(2) 0.0612(8) Uani 1 1 d . . . . . H13 H 0.7713 0.6647 0.0032 0.073 Uiso 1 1 calc R U . . . C14 C 0.5279(4) 0.6389(2) -0.0459(2) 0.0645(8) Uani 1 1 d . . . . . H14 H 0.5391 0.5695 -0.0497 0.077 Uiso 1 1 calc R U . . . C15 C 1.3164(4) 0.6242(2) 0.1962(2) 0.0552(7) Uani 1 1 d . . . . . C16 C 1.2251(4) 0.7061(2) 0.16479(19) 0.0517(7) Uani 1 1 d . . . . . H16 H 1.1089 0.7000 0.1452 0.062 Uiso 1 1 calc R U . . . N1 N 0.9560(3) 0.81518(17) 0.05456(16) 0.0517(6) Uani 1 1 d . . . . . N2 N 0.7831(3) 0.9506(2) 0.0523(2) 0.0665(7) Uani 1 1 d . . . . . O1 O 0.9465(3) 0.97346(15) 0.09297(16) 0.0670(6) Uani 1 1 d . . . . . O2 O 1.2868(3) 0.97418(17) 0.14259(17) 0.0784(7) Uani 1 1 d . . . . . F1 F 0.0959(4) 0.6670(3) -0.1423(3) 0.1609(16) Uani 1 1 d . . . . . F2 F 0.2569(4) 0.5467(3) -0.1471(3) 0.1597(16) Uani 1 1 d . . . . . F3 F 0.1445(4) 0.5825(3) -0.03482(19) 0.1415(14) Uani 1 1 d . . . . . Cl1 Cl 1.78780(10) 0.73234(9) 0.25663(7) 0.0876(4) Uani 1 1 d . . . . . Cl2 Cl 1.21231(13) 0.50879(7) 0.19858(8) 0.0888(4) 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 0.0545(16) 0.065(2) 0.0576(18) 0.0020(15) -0.0017(14) 0.0137(14) C2 0.0442(14) 0.078(2) 0.0485(17) -0.0033(15) -0.0015(12) 0.0043(14) C3 0.0474(15) 0.0613(18) 0.0544(17) 0.0010(14) -0.0011(13) -0.0071(13) C4 0.0452(14) 0.0514(16) 0.0482(16) -0.0013(13) -0.0039(12) -0.0014(12) C5 0.0584(17) 0.0515(17) 0.0520(17) 0.0011(14) -0.0078(14) -0.0053(13) C6 0.0560(16) 0.0419(15) 0.0547(17) 0.0030(13) -0.0029(13) 0.0027(12) C7 0.0490(15) 0.0454(15) 0.0514(16) 0.0054(13) 0.0004(12) 0.0074(12) C8 0.0465(14) 0.0465(15) 0.0479(15) 0.0051(12) 0.0022(12) 0.0059(11) C9 0.0542(16) 0.0483(15) 0.0561(17) -0.0011(13) -0.0027(13) 0.0117(13) C10 0.0476(15) 0.0625(19) 0.0566(18) 0.0039(14) -0.0037(13) 0.0125(13) C11 0.0462(15) 0.0586(17) 0.0521(17) 0.0027(14) 0.0036(12) -0.0003(12) C12 0.0543(17) 0.071(2) 0.067(2) 0.0001(18) -0.0013(16) -0.0037(15) C13 0.0477(15) 0.0512(17) 0.083(2) 0.0064(16) -0.0072(15) 0.0074(13) C14 0.0565(17) 0.0465(16) 0.089(2) 0.0023(16) -0.0051(16) 0.0014(13) C15 0.0545(16) 0.0495(16) 0.0608(18) 0.0017(14) -0.0025(14) 0.0038(13) C16 0.0452(14) 0.0516(16) 0.0573(17) 0.0032(13) -0.0052(12) 0.0024(12) N1 0.0485(12) 0.0441(12) 0.0611(15) 0.0027(11) -0.0072(11) 0.0033(10) N2 0.0613(15) 0.0502(15) 0.085(2) -0.0061(13) -0.0148(14) 0.0118(12) O1 0.0630(13) 0.0466(12) 0.0885(17) -0.0086(11) -0.0172(11) 0.0073(10) O2 0.0836(16) 0.0534(13) 0.0938(18) 0.0072(12) -0.0283(14) -0.0162(12) F1 0.0977(18) 0.126(2) 0.246(4) 0.051(3) -0.096(2) -0.0343(17) F2 0.0887(18) 0.169(3) 0.222(4) -0.127(3) 0.016(2) -0.0329(19) F3 0.139(2) 0.185(3) 0.101(2) 0.007(2) 0.0138(18) -0.104(2) Cl1 0.0447(4) 0.1153(8) 0.1006(8) 0.0042(6) -0.0126(4) 0.0036(4) Cl2 0.0814(6) 0.0539(5) 0.1278(9) 0.0176(5) -0.0186(6) -0.0037(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' F F 0.0171 0.0103 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C15 117.5(3) . . ? C2 C1 H1 121.2 . . ? C15 C1 H1 121.2 . . ? C3 C2 C1 122.3(3) . . ? C3 C2 Cl1 119.1(3) . . ? C1 C2 Cl1 118.6(2) . . ? C2 C3 C4 118.9(3) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C16 C4 C3 120.1(3) . . ? C16 C4 C5 123.5(2) . . ? C3 C4 C5 116.3(3) . . ? O2 C5 C4 123.0(3) . . ? O2 C5 C6 117.4(3) . . ? C4 C5 C6 119.6(2) . . ? N1 C6 O1 113.8(2) . . ? N1 C6 C5 129.8(3) . . ? O1 C6 C5 116.4(2) . . ? N2 C7 N1 113.7(3) . . ? N2 C7 C8 123.3(2) . . ? N1 C7 C8 122.8(2) . . ? C13 C8 C9 119.4(3) . . ? C13 C8 C7 119.1(2) . . ? C9 C8 C7 121.4(2) . . ? C10 C9 C8 120.4(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 119.9(3) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C14 119.7(3) . . ? C10 C11 C12 120.9(3) . . ? C14 C11 C12 119.4(3) . . ? F1 C12 F2 104.5(4) . . ? F1 C12 F3 104.2(3) . . ? F2 C12 F3 106.0(4) . . ? F1 C12 C11 114.8(3) . . ? F2 C12 C11 113.8(3) . . ? F3 C12 C11 112.5(3) . . ? C14 C13 C8 120.2(3) . . ? C14 C13 H13 119.9 . . ? C8 C13 H13 119.9 . . ? C13 C14 C11 120.4(3) . . ? C13 C14 H14 119.8 . . ? C11 C14 H14 119.8 . . ? C16 C15 C1 122.1(3) . . ? C16 C15 Cl2 119.1(2) . . ? C1 C15 Cl2 118.7(2) . . ? C15 C16 C4 119.1(3) . . ? C15 C16 H16 120.5 . . ? C4 C16 H16 120.5 . . ? C6 N1 C7 102.7(2) . . ? C7 N2 O1 104.0(2) . . ? C6 O1 N2 105.8(2) . . ? 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 C1 C2 1.383(5) . ? C1 C15 1.385(4) . ? C1 H1 0.9300 . ? C2 C3 1.372(4) . ? C2 Cl1 1.732(3) . ? C3 C4 1.395(4) . ? C3 H3 0.9300 . ? C4 C16 1.390(4) . ? C4 C5 1.486(4) . ? C5 O2 1.203(3) . ? C5 C6 1.505(4) . ? C6 N1 1.287(4) . ? C6 O1 1.334(3) . ? C7 N2 1.298(4) . ? C7 N1 1.378(3) . ? C7 C8 1.464(4) . ? C8 C13 1.383(4) . ? C8 C9 1.388(4) . ? C9 C10 1.381(4) . ? C9 H9 0.9300 . ? C10 C11 1.379(4) . ? C10 H10 0.9300 . ? C11 C14 1.386(4) . ? C11 C12 1.482(4) . ? C12 F1 1.284(4) . ? C12 F2 1.284(4) . ? C12 F3 1.290(4) . ? C13 C14 1.374(4) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.372(4) . ? C15 Cl2 1.735(3) . ? C16 H16 0.9300 . ? N2 O1 1.405(3) . ? 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 C16 H16 N1 0.93 2.35 2.982(3) 125.0 . C1 H1 O2 0.93 2.47 3.329(4) 153.4 2_845 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 C15 C1 C2 C3 -0.1(5) . . . . ? C15 C1 C2 Cl1 179.7(2) . . . . ? C1 C2 C3 C4 -0.6(5) . . . . ? Cl1 C2 C3 C4 179.5(2) . . . . ? C2 C3 C4 C16 0.5(4) . . . . ? C2 C3 C4 C5 178.5(3) . . . . ? C16 C4 C5 O2 169.4(3) . . . . ? C3 C4 C5 O2 -8.5(5) . . . . ? C16 C4 C5 C6 -8.6(4) . . . . ? C3 C4 C5 C6 173.5(3) . . . . ? O2 C5 C6 N1 159.5(3) . . . . ? C4 C5 C6 N1 -22.4(5) . . . . ? O2 C5 C6 O1 -19.4(4) . . . . ? C4 C5 C6 O1 158.8(3) . . . . ? N2 C7 C8 C13 -167.0(3) . . . . ? N1 C7 C8 C13 8.1(4) . . . . ? N2 C7 C8 C9 9.9(5) . . . . ? N1 C7 C8 C9 -175.0(3) . . . . ? C13 C8 C9 C10 2.9(4) . . . . ? C7 C8 C9 C10 -173.9(3) . . . . ? C8 C9 C10 C11 -0.9(4) . . . . ? C9 C10 C11 C14 -2.1(5) . . . . ? C9 C10 C11 C12 176.4(3) . . . . ? C10 C11 C12 F1 18.9(5) . . . . ? C14 C11 C12 F1 -162.7(4) . . . . ? C10 C11 C12 F2 139.3(4) . . . . ? C14 C11 C12 F2 -42.2(5) . . . . ? C10 C11 C12 F3 -100.1(4) . . . . ? C14 C11 C12 F3 78.4(4) . . . . ? C9 C8 C13 C14 -2.1(5) . . . . ? C7 C8 C13 C14 174.8(3) . . . . ? C8 C13 C14 C11 -0.8(5) . . . . ? C10 C11 C14 C13 2.9(5) . . . . ? C12 C11 C14 C13 -175.6(3) . . . . ? C2 C1 C15 C16 1.1(5) . . . . ? C2 C1 C15 Cl2 179.7(2) . . . . ? C1 C15 C16 C4 -1.2(5) . . . . ? Cl2 C15 C16 C4 -179.8(2) . . . . ? C3 C4 C16 C15 0.4(4) . . . . ? C5 C4 C16 C15 -177.5(3) . . . . ? O1 C6 N1 C7 -1.0(3) . . . . ? C5 C6 N1 C7 -179.9(3) . . . . ? N2 C7 N1 C6 0.1(3) . . . . ? C8 C7 N1 C6 -175.4(3) . . . . ? N1 C7 N2 O1 0.7(3) . . . . ? C8 C7 N2 O1 176.2(3) . . . . ? N1 C6 O1 N2 1.5(4) . . . . ? C5 C6 O1 N2 -179.5(2) . . . . ? C7 N2 O1 C6 -1.2(3) . . . . ?