#------------------------------------------------------------------------------ #$Date: 2024-10-05 15:36:36 +0300 (Sat, 05 Oct 2024) $ #$Revision: 295074 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/16/01/7160169.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_7160169 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 'C14 H13 Cl N2 O3' _chemical_formula_sum 'C14 H13 Cl N2 O3' _chemical_formula_weight 292.71 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 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 91.509(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.9833(6) _cell_length_b 7.9155(7) _cell_length_c 24.658(2) _cell_measurement_reflns_used 5384 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 49.531 _cell_measurement_theta_min 5.407 _cell_volume 1362.5(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 0.975 _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 0.0364 _diffrn_reflns_av_unetI/netI 0.0308 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 15969 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.975 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.381 _diffrn_reflns_theta_min 2.703 _exptl_absorpt_coefficient_mu 0.289 _exptl_absorpt_correction_T_max 0.944 _exptl_absorpt_correction_T_min 0.893 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.427 _exptl_crystal_description block _exptl_crystal_F_000 608 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.232 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.059 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 3330 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.990 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0468 _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^)+(0.0686P)^2^+0.4748P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1193 _refine_ls_wR_factor_ref 0.1373 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2353 _reflns_number_total 3330 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ob01221f2.cif _cod_data_source_block shelx _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7160169 _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 0.893 _shelx_estimated_absorpt_t_max 0.944 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelxt_a.res in P2(1)/n CELL 0.71073 6.9833 7.9155 24.6576 90.000 91.509 90.000 ZERR 4.00 0.0006 0.0007 0.0022 0.000 0.005 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O CL UNIT 56 52 8 12 4 MERG 2 OMIT 0 0 2 OMIT -1 0 1 OMIT -1 1 0 MORE -1 EQIV $1 x+1, y, z HTAB C2 O3_$1 EQIV $2 -x+1/2, y-1/2, -z+1/2 HTAB N2 O3_$2 HTAB C2 O3_$1 HTAB N2 O3_$2 FMAP 2 PLAN 20 SIZE 0.200 0.300 0.400 ACTA BOND $H CONF LIST 4 L.S. 10 TEMP 23.00 WGHT 0.068600 0.474800 FVAR 0.21245 C1 1 0.611090 0.553291 0.397603 11.00000 0.04638 0.04387 = 0.03851 -0.00197 0.00337 0.00393 AFIX 43 H1 2 0.661435 0.489711 0.369645 11.00000 -1.20000 AFIX 0 C2 1 0.731559 0.619888 0.437444 11.00000 0.04670 0.05876 = 0.04589 0.00022 -0.00176 -0.00023 AFIX 43 H2 2 0.862692 0.599790 0.436798 11.00000 -1.20000 AFIX 0 C3 1 0.656361 0.715704 0.477883 11.00000 0.06764 0.05458 = 0.03463 0.00179 0.00097 -0.01615 C4 1 0.463220 0.746314 0.480182 11.00000 0.07601 0.06428 = 0.04481 -0.01575 0.02274 -0.01247 AFIX 43 H4 2 0.414212 0.812429 0.507737 11.00000 -1.20000 AFIX 0 C5 1 0.343733 0.677203 0.440903 11.00000 0.04899 0.06333 = 0.05170 -0.00767 0.02152 -0.00732 AFIX 43 H5 2 0.212414 0.695436 0.442391 11.00000 -1.20000 AFIX 0 C6 1 0.415471 0.580957 0.399182 11.00000 0.04274 0.03689 = 0.03708 0.00308 0.01088 -0.00608 C7 1 0.279133 0.507413 0.358567 11.00000 0.03835 0.04013 = 0.04220 0.00530 0.01006 -0.00261 C8 1 0.355571 0.449860 0.305439 11.00000 0.03117 0.03628 = 0.03844 0.00419 -0.00006 -0.00226 C9 1 0.494562 0.410028 0.233139 11.00000 0.03220 0.03450 = 0.03506 0.00133 -0.00173 0.00163 C10 1 0.630322 0.434444 0.188094 11.00000 0.03708 0.03579 = 0.03670 -0.00570 0.00519 0.00020 AFIX 13 H10 2 0.624081 0.334744 0.164550 11.00000 -1.20000 AFIX 0 C11 1 0.570975 0.588729 0.154664 11.00000 0.04004 0.05842 = 0.03719 0.00622 0.00056 0.00563 AFIX 23 H11A 2 0.446918 0.568510 0.137251 11.00000 -1.20000 H11B 2 0.559476 0.685774 0.178377 11.00000 -1.20000 AFIX 0 C12 1 0.716812 0.625722 0.111996 11.00000 0.05929 0.05963 = 0.04214 0.00625 0.00887 -0.00369 AFIX 23 H12A 2 0.720717 0.532112 0.086662 11.00000 -1.20000 H12B 2 0.678311 0.726027 0.091912 11.00000 -1.20000 AFIX 0 C13 1 0.965055 0.503483 0.163365 11.00000 0.03892 0.04441 = 0.08087 -0.00026 0.01682 0.00441 AFIX 23 H13A 2 1.093564 0.522449 0.177990 11.00000 -1.20000 H13B 2 0.970470 0.410327 0.137893 11.00000 -1.20000 AFIX 0 C14 1 0.835924 0.456264 0.208845 11.00000 0.03355 0.04250 = 0.06061 0.00809 0.00150 0.00607 AFIX 23 H14A 2 0.840982 0.543733 0.236398 11.00000 -1.20000 H14B 2 0.880407 0.351679 0.225356 11.00000 -1.20000 AFIX 0 N1 3 0.500391 0.505969 0.279854 11.00000 0.03530 0.03593 = 0.03663 0.00069 0.00466 -0.00241 N2 3 0.356411 0.301112 0.230669 11.00000 0.04451 0.05691 = 0.04475 -0.00892 0.00638 -0.01454 O1 4 0.901267 0.650943 0.135465 11.00000 0.04953 0.04644 = 0.06946 0.00558 0.01612 -0.00420 O2 4 0.259329 0.327799 0.279619 11.00000 0.04067 0.05723 = 0.04636 -0.00532 0.00678 -0.01802 O3 4 0.109907 0.492295 0.366074 11.00000 0.04024 0.08453 = 0.06000 -0.00523 0.01650 -0.01315 CL1 5 0.808744 0.803677 0.526522 11.00000 0.10854 0.10562 = 0.05491 -0.01815 -0.01798 -0.02694 HKLF 4 REM shelxt_a.res in P2(1)/n REM R1 = 0.0468 for 2353 Fo > 4sig(Fo) and 0.0732 for all 3330 data REM 181 parameters refined using 0 restraints END WGHT 0.0581 0.4536 REM Highest difference peak 0.232, deepest hole -0.401, 1-sigma level 0.059 Q1 1 0.6755 0.8307 0.5309 11.00000 0.05 0.23 Q2 1 1.1221 0.5627 0.2102 11.00000 0.05 0.18 Q3 1 0.7368 0.6184 0.2886 11.00000 0.05 0.16 Q4 1 0.3055 0.8968 0.4341 11.00000 0.05 0.16 Q5 1 0.2467 0.9126 0.4025 11.00000 0.05 0.15 Q6 1 0.8887 0.6194 0.2767 11.00000 0.05 0.14 Q7 1 0.4191 0.9273 0.4645 11.00000 0.05 0.14 Q8 1 0.1390 0.9357 0.4356 11.00000 0.05 0.14 Q9 1 1.1153 0.3632 0.1728 11.00000 0.05 0.14 Q10 1 0.3788 0.4015 0.0922 11.00000 0.05 0.14 Q11 1 0.1088 0.8782 0.4523 11.00000 0.05 0.14 Q12 1 0.5768 0.6144 0.2922 11.00000 0.05 0.14 Q13 1 0.5229 0.3646 0.1083 11.00000 0.05 0.14 Q14 1 0.9638 0.6202 0.2429 11.00000 0.05 0.14 Q15 1 0.3694 0.8801 0.4925 11.00000 0.05 0.14 Q16 1 0.4101 0.9094 0.4985 11.00000 0.05 0.14 Q17 1 0.4561 0.8661 0.4409 11.00000 0.05 0.13 Q18 1 0.8499 0.5061 0.2840 11.00000 0.05 0.13 Q19 1 1.0387 0.4598 0.0638 11.00000 0.05 0.13 Q20 1 0.2737 0.2335 0.2046 11.00000 0.05 0.13 ; _shelx_res_checksum 86601 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 0.6111(3) 0.5533(2) 0.39760(7) 0.0429(4) Uani 1 1 d . . . . . H1 H 0.6614 0.4897 0.3696 0.051 Uiso 1 1 calc R U . . . C2 C 0.7316(3) 0.6199(3) 0.43744(8) 0.0505(5) Uani 1 1 d . . . . . H2 H 0.8627 0.5998 0.4368 0.061 Uiso 1 1 calc R U . . . C3 C 0.6564(3) 0.7157(3) 0.47788(8) 0.0523(5) Uani 1 1 d . . . . . C4 C 0.4632(4) 0.7463(3) 0.48018(9) 0.0613(6) Uani 1 1 d . . . . . H4 H 0.4142 0.8124 0.5077 0.074 Uiso 1 1 calc R U . . . C5 C 0.3437(3) 0.6772(3) 0.44090(9) 0.0543(5) Uani 1 1 d . . . . . H5 H 0.2124 0.6954 0.4424 0.065 Uiso 1 1 calc R U . . . C6 C 0.4155(3) 0.5810(2) 0.39918(7) 0.0387(4) Uani 1 1 d . . . . . C7 C 0.2791(3) 0.5074(2) 0.35857(7) 0.0401(4) Uani 1 1 d . . . . . C8 C 0.3556(2) 0.4499(2) 0.30544(7) 0.0353(4) Uani 1 1 d . . . . . C9 C 0.4946(2) 0.4100(2) 0.23314(7) 0.0340(4) Uani 1 1 d . . . . . C10 C 0.6303(2) 0.4344(2) 0.18809(7) 0.0364(4) Uani 1 1 d . . . . . H10 H 0.6241 0.3347 0.1646 0.044 Uiso 1 1 calc R U . . . C11 C 0.5710(3) 0.5887(3) 0.15466(7) 0.0452(5) Uani 1 1 d . . . . . H11A H 0.4469 0.5685 0.1373 0.054 Uiso 1 1 calc R U . . . H11B H 0.5595 0.6858 0.1784 0.054 Uiso 1 1 calc R U . . . C12 C 0.7168(3) 0.6257(3) 0.11200(8) 0.0536(5) Uani 1 1 d . . . . . H12A H 0.7207 0.5321 0.0867 0.064 Uiso 1 1 calc R U . . . H12B H 0.6783 0.7260 0.0919 0.064 Uiso 1 1 calc R U . . . C13 C 0.9651(3) 0.5035(2) 0.16336(10) 0.0545(5) Uani 1 1 d . . . . . H13A H 1.0936 0.5224 0.1780 0.065 Uiso 1 1 calc R U . . . H13B H 0.9705 0.4103 0.1379 0.065 Uiso 1 1 calc R U . . . C14 C 0.8359(2) 0.4563(2) 0.20885(9) 0.0455(5) Uani 1 1 d . . . . . H14A H 0.8410 0.5437 0.2364 0.055 Uiso 1 1 calc R U . . . H14B H 0.8804 0.3517 0.2254 0.055 Uiso 1 1 calc R U . . . N1 N 0.5004(2) 0.50597(17) 0.27985(6) 0.0359(3) Uani 1 1 d . . . . . N2 N 0.3564(2) 0.3011(2) 0.23067(7) 0.0486(4) Uani 1 1 d . . . . . O1 O 0.9013(2) 0.65094(17) 0.13547(6) 0.0549(4) Uani 1 1 d . . . . . O2 O 0.25933(18) 0.32780(18) 0.27962(5) 0.0480(3) Uani 1 1 d . . . . . O3 O 0.1099(2) 0.4923(2) 0.36607(6) 0.0613(4) Uani 1 1 d . . . . . Cl1 Cl 0.80874(12) 0.80368(11) 0.52652(3) 0.0900(3) 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 0.0464(10) 0.0439(10) 0.0385(9) -0.0020(8) 0.0034(8) 0.0039(8) C2 0.0467(11) 0.0588(12) 0.0459(11) 0.0002(9) -0.0018(9) -0.0002(9) C3 0.0676(14) 0.0546(12) 0.0346(10) 0.0018(8) 0.0010(9) -0.0161(10) C4 0.0760(16) 0.0643(14) 0.0448(11) -0.0157(10) 0.0227(11) -0.0125(12) C5 0.0490(11) 0.0633(13) 0.0517(12) -0.0077(10) 0.0215(9) -0.0073(10) C6 0.0427(10) 0.0369(9) 0.0371(9) 0.0031(7) 0.0109(7) -0.0061(7) C7 0.0384(9) 0.0401(9) 0.0422(9) 0.0053(8) 0.0101(8) -0.0026(7) C8 0.0312(8) 0.0363(8) 0.0384(9) 0.0042(7) -0.0001(7) -0.0023(7) C9 0.0322(8) 0.0345(8) 0.0351(8) 0.0013(7) -0.0017(7) 0.0016(7) C10 0.0371(9) 0.0358(9) 0.0367(9) -0.0057(7) 0.0052(7) 0.0002(7) C11 0.0400(10) 0.0584(12) 0.0372(9) 0.0062(8) 0.0006(8) 0.0056(8) C12 0.0593(13) 0.0596(13) 0.0421(10) 0.0062(9) 0.0089(9) -0.0037(10) C13 0.0389(10) 0.0444(11) 0.0809(15) -0.0003(10) 0.0168(10) 0.0044(8) C14 0.0335(9) 0.0425(10) 0.0606(12) 0.0081(9) 0.0015(8) 0.0061(8) N1 0.0353(8) 0.0359(8) 0.0366(7) 0.0007(6) 0.0047(6) -0.0024(6) N2 0.0445(9) 0.0569(10) 0.0448(9) -0.0089(7) 0.0064(7) -0.0145(8) O1 0.0495(8) 0.0464(8) 0.0695(9) 0.0056(7) 0.0161(7) -0.0042(6) O2 0.0407(7) 0.0572(8) 0.0464(7) -0.0053(6) 0.0068(6) -0.0180(6) O3 0.0402(8) 0.0845(11) 0.0600(9) -0.0052(8) 0.0165(7) -0.0132(7) Cl1 0.1085(6) 0.1056(6) 0.0549(4) -0.0182(3) -0.0180(4) -0.0269(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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.16(18) . . ? C2 C1 H1 119.9 . . ? C6 C1 H1 119.9 . . ? C3 C2 C1 119.4(2) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 121.6(2) . . ? C2 C3 Cl1 119.19(18) . . ? C4 C3 Cl1 119.19(17) . . ? C5 C4 C3 118.64(19) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 121.2(2) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 118.97(18) . . ? C5 C6 C7 118.65(17) . . ? C1 C6 C7 122.36(16) . . ? O3 C7 C6 123.32(17) . . ? O3 C7 C8 118.47(17) . . ? C6 C7 C8 118.21(15) . . ? N1 C8 O2 114.23(15) . . ? N1 C8 C7 128.84(16) . . ? O2 C8 C7 116.89(14) . . ? N2 C9 N1 114.31(15) . . ? N2 C9 C10 122.61(16) . . ? N1 C9 C10 123.03(15) . . ? C9 C10 C14 112.15(15) . . ? C9 C10 C11 109.71(14) . . ? C14 C10 C11 109.37(15) . . ? C9 C10 H10 108.5 . . ? C14 C10 H10 108.5 . . ? C11 C10 H10 108.5 . . ? C12 C11 C10 110.66(16) . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? O1 C12 C11 111.47(16) . . ? O1 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? O1 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? O1 C13 C14 112.25(15) . . ? O1 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? O1 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C13 C14 C10 110.88(17) . . ? C13 C14 H14A 109.5 . . ? C10 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C8 N1 C9 102.32(14) . . ? C9 N2 O2 103.51(14) . . ? C12 O1 C13 110.69(16) . . ? C8 O2 N2 105.62(12) . . ? 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 1.381(3) . ? C1 C6 1.385(3) . ? C1 H1 0.9300 . ? C2 C3 1.369(3) . ? C2 H2 0.9300 . ? C3 C4 1.373(3) . ? C3 Cl1 1.729(2) . ? C4 C5 1.375(3) . ? C4 H4 0.9300 . ? C5 C6 1.385(3) . ? C5 H5 0.9300 . ? C6 C7 1.483(3) . ? C7 O3 1.207(2) . ? C7 C8 1.498(2) . ? C8 N1 1.285(2) . ? C8 O2 1.330(2) . ? C9 N2 1.294(2) . ? C9 N1 1.379(2) . ? C9 C10 1.492(2) . ? C10 C14 1.521(3) . ? C10 C11 1.525(3) . ? C10 H10 0.9800 . ? C11 C12 1.512(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O1 1.412(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 O1 1.421(2) . ? C13 C14 1.505(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? N2 O2 1.4157(19) . ? 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 O3 0.93 2.63 3.368(2) 137.0 1_655 C2 H2 O3 0.93 2.63 3.368(2) 137.0 1_655 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 C6 C1 C2 C3 -1.1(3) . . . . ? C1 C2 C3 C4 0.6(3) . . . . ? C1 C2 C3 Cl1 -178.16(15) . . . . ? C2 C3 C4 C5 0.5(3) . . . . ? Cl1 C3 C4 C5 179.27(17) . . . . ? C3 C4 C5 C6 -1.1(3) . . . . ? C4 C5 C6 C1 0.6(3) . . . . ? C4 C5 C6 C7 178.98(19) . . . . ? C2 C1 C6 C5 0.6(3) . . . . ? C2 C1 C6 C7 -177.79(17) . . . . ? C5 C6 C7 O3 -17.9(3) . . . . ? C1 C6 C7 O3 160.42(19) . . . . ? C5 C6 C7 C8 161.75(17) . . . . ? C1 C6 C7 C8 -19.9(2) . . . . ? O3 C7 C8 N1 150.67(19) . . . . ? C6 C7 C8 N1 -29.0(3) . . . . ? O3 C7 C8 O2 -27.0(2) . . . . ? C6 C7 C8 O2 153.35(16) . . . . ? N2 C9 C10 C14 -138.48(18) . . . . ? N1 C9 C10 C14 44.3(2) . . . . ? N2 C9 C10 C11 99.8(2) . . . . ? N1 C9 C10 C11 -77.4(2) . . . . ? C9 C10 C11 C12 174.69(16) . . . . ? C14 C10 C11 C12 51.3(2) . . . . ? C10 C11 C12 O1 -57.4(2) . . . . ? O1 C13 C14 C10 55.8(2) . . . . ? C9 C10 C14 C13 -172.46(15) . . . . ? C11 C10 C14 C13 -50.5(2) . . . . ? O2 C8 N1 C9 0.19(19) . . . . ? C7 C8 N1 C9 -177.48(17) . . . . ? N2 C9 N1 C8 -0.7(2) . . . . ? C10 C9 N1 C8 176.72(15) . . . . ? N1 C9 N2 O2 0.9(2) . . . . ? C10 C9 N2 O2 -176.56(15) . . . . ? C11 C12 O1 C13 61.4(2) . . . . ? C14 C13 O1 C12 -60.9(2) . . . . ? N1 C8 O2 N2 0.3(2) . . . . ? C7 C8 O2 N2 178.28(14) . . . . ? C9 N2 O2 C8 -0.69(18) . . . . ?