#------------------------------------------------------------------------------ #$Date: 2024-10-22 01:10:36 +0300 (Tue, 22 Oct 2024) $ #$Revision: 295572 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/29/1572913.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_1572913 loop_ _publ_author_name 'Limberg, Niklas' 'Rautiainen, J. Mikko' 'Lundell, Jan' 'Riedel, Sebastian' 'Puttreddy, Rakesh R.' 'Rissanen, Kari' _publ_section_title ; Dichlorine-Pyridine N-oxide Halogen-Bonded Complexes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC06270A _journal_year 2024 _chemical_formula_moiety 'Cl, C7 H10 N O2' _chemical_formula_sum 'C7 H10 Cl N O2' _chemical_formula_weight 175.61 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2024-09-11 _audit_creation_method ; Olex2 1.5-alpha (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-09-13 deposited with the CCDC. 2024-10-21 downloaded from the CCDC. ; _cell_angle_alpha 82.272(2) _cell_angle_beta 80.701(2) _cell_angle_gamma 66.100(2) _cell_formula_units_Z 4 _cell_length_a 7.7469(4) _cell_length_b 9.1814(5) _cell_length_c 13.0548(7) _cell_measurement_reflns_used 9891 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 28.170 _cell_measurement_theta_min 2.897 _cell_volume 835.32(8) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _diffrn_ambient_temperature 100.00 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_unetI/netI 0.0223 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 34530 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 2.433 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.407 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0945 before and 0.0626 after correction. The Ratio of minimum to maximum transmission is 0.9189. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.396 _exptl_crystal_description block _exptl_crystal_F_000 368 _exptl_crystal_size_max 0.554 _exptl_crystal_size_mid 0.297 _exptl_crystal_size_min 0.192 _refine_diff_density_max 0.261 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.044 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 205 _refine_ls_number_reflns 3416 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0269 _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^)+(0.0205P)^2^+0.5244P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.0665 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2926 _reflns_number_total 3416 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06270a3.cif _cod_data_source_block OGH_D49_33 _cod_database_code 1572913 _shelx_shelxl_version_number 2019/1 _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 0.926 _shelx_estimated_absorpt_t_min 0.806 _olex2_refinement_description ; 1.a Aromatic/amide H refined with riding coordinates: C9(H9), C2(H2), C4(H4), C5(H5), C11(H11), C12(H12) 1.b Idealised Me refined as rotating group: C14(H14A,H14B,H14C), C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C7(H7A,H7B,H7C) 1.c Idealised tetrahedral OH refined as rotating group: O1(H1), O3(H3) ; _shelx_res_file ; TITL full1_P-1_a.res in P-1 full1_p-1_a.res created by SHELXL-2019/1 at 17:39:46 on 30-Apr-2024 REM Old TITL full1_P-1 in P-1 REM SHELXT solution in P-1: R1 0.088, Rweak 0.003, Alpha 0.035 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C14 Cl2 N2 O4 CELL 0.71073 7.7469 9.1814 13.0548 82.272 80.701 66.1 ZERR 4 0.0004 0.0005 0.0007 0.002 0.002 0.002 LATT 1 SFAC C H Cl N O UNIT 28 40 4 4 8 L.S. 10 PLAN 4 SIZE 0.192 0.297 0.554 TEMP -173.15 CONF BOND LIST 4 MORE -1 BOND $H fmap 2 acta SHEL 9999 0.8 REM REM REM WGHT 0.020500 0.524400 FVAR 1.37947 CL1 3 -0.411959 0.189027 0.547504 11.00000 0.02330 0.02153 = 0.01697 -0.00158 0.00026 -0.01061 CL2 3 -0.295577 0.671773 0.093763 11.00000 0.02763 0.01937 = 0.02028 -0.00099 -0.00023 -0.01166 O4 5 0.021125 -0.081921 0.270245 11.00000 0.02361 0.01854 = 0.02159 -0.00603 -0.00077 -0.00725 O1 5 -0.679263 0.266545 0.398231 11.00000 0.01811 0.03543 = 0.01639 -0.00094 0.00189 -0.00986 AFIX 147 H1 2 -0.612396 0.243957 0.447269 11.00000 -1.50000 AFIX 0 O2 5 -0.240391 0.146849 0.025099 11.00000 0.02557 0.01832 = 0.01822 -0.00511 0.00201 -0.00910 O3 5 0.021471 0.515240 0.212835 11.00000 0.03422 0.02541 = 0.02695 0.00537 -0.00929 -0.02040 AFIX 147 H3 2 -0.067801 0.575499 0.178749 11.00000 -1.50000 AFIX 0 N1 4 -0.562579 0.239393 0.304515 11.00000 0.01608 0.02344 = 0.01566 -0.00063 -0.00088 -0.00794 N2 4 0.017354 0.364779 0.230239 11.00000 0.02202 0.02165 = 0.01841 0.00118 -0.00450 -0.01263 C9 1 -0.064304 0.172715 0.339416 11.00000 0.01531 0.02017 = 0.01414 -0.00168 -0.00239 -0.00600 AFIX 43 H9 2 -0.120480 0.140701 0.403865 11.00000 -1.20000 AFIX 0 C2 1 -0.413545 0.333585 0.155970 11.00000 0.01822 0.01651 = 0.01642 -0.00054 -0.00362 -0.00808 AFIX 43 H2 2 -0.383145 0.416806 0.116809 11.00000 -1.20000 AFIX 0 C10 1 0.019108 0.065615 0.262189 11.00000 0.01482 0.01944 = 0.01912 -0.00245 -0.00496 -0.00488 C1 1 -0.521676 0.361042 0.252031 11.00000 0.01594 0.01927 = 0.01835 -0.00194 -0.00530 -0.00731 C4 1 -0.394710 0.062395 0.174507 11.00000 0.01928 0.01500 = 0.02531 -0.00213 -0.00507 -0.00591 AFIX 43 H4 2 -0.351505 -0.040011 0.148778 11.00000 -1.20000 AFIX 0 C3 1 -0.348833 0.184511 0.116207 11.00000 0.01540 0.01881 = 0.01667 -0.00176 -0.00432 -0.00566 C8 1 -0.065956 0.325296 0.322974 11.00000 0.01488 0.02044 = 0.01640 -0.00099 -0.00417 -0.00642 C5 1 -0.502405 0.093219 0.268760 11.00000 0.01777 0.01793 = 0.02415 0.00330 -0.00605 -0.00761 AFIX 43 H5 2 -0.535088 0.012046 0.309235 11.00000 -1.20000 AFIX 0 C14 1 -0.059395 -0.137501 0.367507 11.00000 0.02694 0.01839 = 0.02472 0.00086 -0.00478 -0.00942 AFIX 137 H14A 2 -0.060050 -0.242216 0.360516 11.00000 -1.50000 H14B 2 -0.189933 -0.061272 0.385212 11.00000 -1.50000 H14C 2 0.017209 -0.146697 0.422734 11.00000 -1.50000 AFIX 0 C6 1 -0.593441 0.515441 0.300587 11.00000 0.02190 0.02334 = 0.02190 -0.00732 -0.00012 -0.00846 AFIX 137 H6A 2 -0.732700 0.562668 0.307044 11.00000 -1.50000 H6B 2 -0.543596 0.588549 0.256939 11.00000 -1.50000 H6C 2 -0.551337 0.496895 0.369789 11.00000 -1.50000 AFIX 0 C13 1 -0.152390 0.446169 0.401310 11.00000 0.02225 0.01934 = 0.02312 -0.00454 -0.00142 -0.00782 AFIX 137 H13A 2 -0.052578 0.469711 0.424117 11.00000 -1.50000 H13B 2 -0.217016 0.404289 0.461316 11.00000 -1.50000 H13C 2 -0.244584 0.544231 0.370165 11.00000 -1.50000 AFIX 0 C11 1 0.104397 0.113421 0.167992 11.00000 0.01898 0.02881 = 0.01756 -0.00834 -0.00011 -0.00885 AFIX 43 H11 2 0.163242 0.041723 0.114711 11.00000 -1.20000 AFIX 0 C12 1 0.101692 0.263725 0.153996 11.00000 0.02172 0.03523 = 0.01486 -0.00273 -0.00125 -0.01500 AFIX 43 H12 2 0.159057 0.297672 0.090659 11.00000 -1.20000 AFIX 0 C7 1 -0.203246 0.273331 -0.040829 11.00000 0.03018 0.02405 = 0.01678 -0.00247 0.00166 -0.01327 AFIX 137 H7A 2 -0.124349 0.230437 -0.105083 11.00000 -1.50000 H7B 2 -0.136342 0.317101 -0.004134 11.00000 -1.50000 H7C 2 -0.323891 0.358112 -0.057918 11.00000 -1.50000 AFIX 0 HKLF 4 REM full1_P-1_a.res in P-1 REM wR2 = 0.0665, GooF = S = 1.046, Restrained GooF = 1.046 for all data REM R1 = 0.0269 for 2926 Fo > 4sig(Fo) and 0.0359 for all 3416 data REM 205 parameters refined using 0 restraints END WGHT 0.0205 0.5244 REM Highest difference peak 0.261, deepest hole -0.271, 1-sigma level 0.044 Q1 1 -0.1066 0.3874 0.3595 11.00000 0.05 0.26 Q2 1 -0.3659 0.1224 0.1546 11.00000 0.05 0.24 Q3 1 -0.0551 0.1414 0.2888 11.00000 0.05 0.23 Q4 1 -0.3843 0.2623 0.1332 11.00000 0.05 0.22 ; _shelx_res_checksum 43044 _shelx_hkl_file ; -1 0 0 40.90 3.80 -1 0 0 30.10 3.60 -1 0 0 37.60 3.30 -1 0 0 35.80 3.40 1 0 0 36.20 3.50 1 0 0 33.40 3.20 1 0 0 37.50 3.50 1 0 0 27.40 3.30 1 0 0 34.80 3.90 -2 0 0 5772.62 183.98 -2 0 0 6077.39 184.18 2 0 0 6008.10 184.48 2 0 0 5856.91 183.88 -3 0 0 3295.37 107.69 -3 0 0 3235.48 112.19 -3 0 0 3186.18 110.99 -3 0 0 3225.88 109.89 -3 0 0 3297.37 107.99 3 0 0 3344.97 108.29 3 0 0 3333.57 109.89 3 0 0 3321.17 112.29 3 0 0 3317.27 110.09 3 0 0 3272.07 112.59 -4 0 0 119.49 13.50 -4 0 0 131.79 14.00 -4 0 0 102.79 12.00 -4 0 0 117.49 11.90 -4 0 0 116.09 13.80 4 0 0 107.69 13.40 4 0 0 100.09 14.80 4 0 0 112.39 13.00 4 0 0 113.79 13.10 4 0 0 107.99 12.60 4 0 0 118.19 12.00 -5 0 0 166.38 16.40 -5 0 0 159.68 19.20 -5 0 0 161.28 18.90 -5 0 0 202.58 19.70 -5 0 0 165.18 17.60 5 0 0 212.88 21.80 5 0 0 150.98 20.10 5 0 0 194.88 19.10 5 0 0 160.58 19.50 5 0 0 193.98 18.80 5 0 0 178.18 17.40 -6 0 0 208.98 21.30 -6 0 0 196.08 24.30 -6 0 0 169.48 19.30 -6 0 0 165.48 22.50 -6 0 0 162.38 23.20 6 0 0 177.48 25.20 6 0 0 189.68 21.40 6 0 0 166.48 22.90 6 0 0 152.68 23.70 -7 0 0 406.06 32.20 -7 0 0 345.77 32.80 -7 0 0 338.17 35.70 7 0 0 287.27 28.50 7 0 0 369.56 31.90 7 0 0 333.47 34.30 7 0 0 329.37 31.60 7 0 0 340.17 32.70 7 0 0 382.66 36.70 -8 0 0 41.40 22.00 -8 0 0 51.29 17.60 -8 0 0 66.79 18.60 -8 0 0 63.39 18.50 -8 0 0 65.79 24.50 8 0 0 70.19 18.00 8 0 0 38.60 17.10 8 0 0 62.29 23.70 8 0 0 52.49 19.00 8 0 0 38.00 22.80 8 0 0 70.39 19.80 8 0 0 60.19 17.70 -9 0 0 -9.40 24.70 -9 0 0 -17.20 20.00 -9 0 0 -29.00 19.90 -9 0 0 -52.49 19.40 9 0 0 29.50 25.40 9 0 0 35.00 29.00 9 0 0 39.60 20.40 9 0 0 24.40 19.50 9 0 0 -8.40 22.20 9 0 0 -4.20 25.40 9 -1 0 -13.30 22.40 9 -1 0 -4.50 37.10 -9 1 0 21.70 23.30 -9 1 0 -12.60 24.10 -9 1 0 -41.10 30.00 -9 1 0 -22.70 25.00 8 -1 0 11.60 15.00 8 -1 0 -11.20 14.70 8 -1 0 -17.80 21.60 8 -1 0 -4.00 20.00 8 -1 0 -12.50 17.20 8 -1 0 22.50 22.70 8 -1 0 -20.60 14.70 -8 1 0 -19.60 15.90 -8 1 0 -3.00 14.60 -8 1 0 -10.60 19.50 -8 1 0 -8.00 17.50 -8 1 0 12.20 14.90 7 -1 0 83.39 19.10 7 -1 0 66.49 22.00 7 -1 0 53.49 19.60 7 -1 0 76.19 16.00 7 -1 0 32.50 15.90 7 -1 0 89.29 19.10 -7 1 0 57.39 16.50 -7 1 0 63.49 17.50 -7 1 0 50.99 16.60 -7 1 0 48.90 15.80 6 -1 0 1811.02 88.49 6 -1 0 1776.52 80.79 6 -1 0 1732.93 85.69 6 -1 0 1895.51 82.79 6 -1 0 1836.52 81.89 6 -1 0 1872.21 79.29 -6 1 0 1805.62 77.39 -6 1 0 1667.83 81.69 -6 1 0 1853.11 87.09 -6 1 0 1735.13 77.59 5 -1 0 24.00 8.90 5 -1 0 21.80 10.70 5 -1 0 17.90 8.00 5 -1 0 23.70 9.50 5 -1 0 30.10 9.10 5 -1 0 19.30 9.20 -5 1 0 7.30 7.10 -5 1 0 12.20 9.00 -5 1 0 12.80 7.40 -5 1 0 8.30 6.90 -5 1 0 7.00 7.40 4 -1 0 1370.36 58.69 4 -1 0 1398.16 63.09 4 -1 0 1251.47 57.19 4 -1 0 1347.67 56.59 4 -1 0 1390.86 58.39 4 -1 0 1304.07 61.19 -4 1 0 1321.07 56.19 -4 1 0 1364.96 60.99 -4 1 0 1328.87 61.39 -4 1 0 1337.17 59.79 -4 1 0 1296.47 55.89 3 -1 0 742.23 36.30 3 -1 0 812.72 40.50 3 -1 0 789.92 39.80 3 -1 0 790.72 36.90 3 -1 0 825.12 36.40 3 -1 0 773.22 37.20 -3 1 0 797.22 39.90 -3 1 0 806.12 36.50 -3 1 0 754.62 35.60 -3 1 0 822.92 39.70 -3 1 0 790.92 38.10 2 -1 0 731.63 32.30 2 -1 0 761.72 38.80 2 -1 0 690.53 33.70 2 -1 0 822.42 33.20 2 -1 0 776.52 33.30 2 -1 0 695.33 30.70 -2 1 0 747.23 34.00 -2 1 0 728.93 34.00 -2 1 0 708.23 32.60 1 -1 0 10.20 3.40 1 -1 0 9.90 2.90 1 -1 0 13.60 4.20 1 -1 0 17.00 3.80 1 -1 0 8.30 2.50 1 -1 0 17.30 3.80 1 -1 0 14.90 3.30 -1 1 0 13.00 3.30 -1 1 0 8.20 2.70 -1 1 0 16.80 4.00 -1 1 0 6.80 2.80 -1 1 0 22.10 5.00 0 -1 0 3.90 1.40 0 -1 0 6.80 1.40 0 -1 0 8.70 2.00 0 -1 0 6.60 1.50 0 -1 0 3.60 1.00 0 -1 0 7.10 1.80 0 -1 0 5.90 1.80 0 1 0 6.10 1.80 0 1 0 5.20 1.20 0 1 0 3.90 1.60 0 1 0 7.10 1.60 0 1 0 5.80 1.50 0 1 0 4.50 1.40 -1 -1 0 131.49 7.00 -1 -1 0 110.59 6.70 -1 -1 0 133.69 6.70 -1 -1 0 126.19 5.60 -1 -1 0 117.29 6.00 1 1 0 115.79 6.50 1 1 0 123.39 6.30 1 1 0 121.19 6.60 1 1 0 122.99 5.80 -2 -1 0 162.08 10.50 -2 -1 0 170.08 10.10 -2 -1 0 165.08 9.00 -2 -1 0 161.48 9.50 2 1 0 153.98 9.50 2 1 0 170.68 9.80 2 1 0 179.08 9.70 2 1 0 172.08 10.90 2 1 0 178.58 10.60 2 1 0 186.68 10.90 -3 -1 0 663.33 27.80 -3 -1 0 685.63 29.90 -3 -1 0 687.03 31.00 -3 -1 0 659.43 28.70 3 1 0 686.43 29.50 3 1 0 700.53 28.90 3 1 0 675.93 32.40 3 1 0 706.83 31.40 3 1 0 682.23 31.60 3 1 0 683.03 30.20 -4 -1 0 2657.43 94.39 -4 -1 0 2656.33 96.09 -4 -1 0 2697.13 92.19 -4 -1 0 2502.75 90.39 4 1 0 2722.83 92.79 4 1 0 2754.82 94.19 4 1 0 2767.72 97.29 4 1 0 2667.93 93.79 4 1 0 2838.42 98.39 -5 -1 0 275.47 21.50 -5 -1 0 226.98 18.30 -5 -1 0 231.08 18.30 -5 -1 0 259.67 21.50 5 1 0 291.47 20.20 5 1 0 257.57 20.20 5 1 0 208.98 20.30 5 1 0 231.38 21.40 5 1 0 281.57 20.90 5 1 0 226.28 19.90 -6 -1 0 913.91 52.39 -6 -1 0 1012.50 59.69 -6 -1 0 916.31 44.70 -6 -1 0 931.11 49.50 -6 -1 0 941.11 45.80 6 1 0 968.90 49.99 6 1 0 983.70 52.99 6 1 0 959.80 52.99 6 1 0 881.81 46.30 6 1 0 962.10 48.60 -7 -1 0 1085.09 60.29 -7 -1 0 1195.58 56.09 -7 -1 0 1133.49 64.19 -7 -1 0 1151.58 56.39 7 1 0 1319.37 63.89 7 1 0 1216.68 59.39 7 1 0 1214.48 60.59 7 1 0 1120.79 63.19 7 1 0 1179.98 60.99 7 1 0 1161.68 65.29 -8 -1 0 207.78 29.00 -8 -1 0 231.38 30.30 -8 -1 0 221.38 26.20 -8 -1 0 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99.39 36.80 1 3 -16 51.89 12.40 1 3 -16 69.69 19.30 -1 -3 16 69.19 11.50 0 3 -16 8.40 15.50 0 3 -16 22.00 19.10 0 3 -16 27.50 12.70 0 3 -16 9.90 14.60 0 3 -16 50.99 18.10 0 -3 16 10.20 17.40 0 -3 16 -14.70 17.20 0 -3 16 2.60 14.20 0 -3 16 -16.50 20.00 -1 3 -16 31.90 18.80 -1 3 -16 44.10 22.20 -1 3 -16 46.80 19.50 1 -3 16 7.40 17.90 1 -3 16 2.10 18.70 1 -3 16 24.80 23.30 2 2 -16 -5.00 5.50 2 2 -16 2.30 19.30 2 2 -16 -4.00 15.20 2 2 -16 5.30 18.70 1 2 -16 43.30 16.30 1 2 -16 1.70 22.40 1 2 -16 0.60 18.60 1 2 -16 41.00 19.50 1 2 -16 16.20 10.70 1 2 -16 8.60 12.00 -1 -2 16 29.50 15.70 -1 -2 16 37.10 23.90 -1 -2 16 48.90 14.50 -1 -2 16 9.30 10.70 -1 -2 16 -18.00 9.40 0 2 -16 12.70 16.20 0 2 -16 19.20 15.70 0 2 -16 30.10 17.50 0 2 -16 20.50 15.40 0 2 -16 0.90 18.60 0 2 -16 -19.40 10.90 0 -2 16 -6.40 12.50 0 -2 16 1.70 15.20 0 -2 16 4.80 14.70 0 -2 16 8.60 30.40 -1 2 -16 358.26 35.20 -1 2 -16 301.37 40.20 -1 2 -16 247.58 35.40 -1 2 -16 274.07 30.40 -1 2 -16 319.37 37.10 1 -2 16 347.17 42.80 1 -2 16 320.67 42.80 1 -2 16 367.46 37.30 -2 2 -16 176.98 30.20 -2 2 -16 311.77 38.50 -2 2 -16 234.18 30.10 -2 2 -16 288.27 34.00 -2 2 -16 276.87 43.50 2 -2 16 203.08 30.60 2 -2 16 208.08 34.30 2 1 -16 379.76 32.70 2 1 -16 482.45 48.80 2 1 -16 339.87 41.00 2 1 -16 456.25 39.70 -2 -1 16 494.15 32.80 -2 -1 16 464.25 30.40 1 1 -16 581.04 42.80 1 1 -16 542.65 34.70 1 1 -16 516.15 54.39 1 1 -16 578.74 46.10 1 1 -16 529.05 49.70 1 1 -16 549.65 38.20 -1 -1 16 523.65 52.69 -1 -1 16 546.75 37.60 -1 -1 16 518.85 38.60 0 1 -16 -15.20 14.00 0 1 -16 -23.50 15.60 0 1 -16 4.30 16.40 0 1 -16 -1.50 11.00 0 1 -16 -20.70 18.60 0 1 -16 -10.70 14.90 0 -1 16 -8.20 14.50 0 -1 16 -25.40 19.30 0 -1 16 -0.70 15.70 0 -1 16 9.40 21.10 -1 1 -16 9.20 13.40 -1 1 -16 -5.60 16.40 -1 1 -16 -28.00 12.70 -1 1 -16 11.70 18.80 -1 1 -16 -10.80 12.00 -1 1 -16 -19.00 18.00 1 -1 16 4.00 14.20 1 -1 16 -42.90 21.90 1 -1 16 8.70 20.10 1 -1 16 20.10 18.30 -2 1 -16 -23.00 14.50 -2 1 -16 11.10 18.60 -2 1 -16 11.70 19.30 -2 1 -16 -32.60 16.70 -2 1 -16 -12.90 24.90 -2 1 -16 -7.40 13.40 2 -1 16 -1.00 16.70 2 -1 16 -11.60 19.40 -3 1 -16 -38.10 20.10 -3 1 -16 -1.50 16.50 -3 1 -16 -8.90 15.80 -3 1 -16 -61.99 27.70 -3 1 -16 2.90 22.50 3 -1 16 28.70 23.10 3 -1 16 -13.70 19.70 2 0 -16 -2.30 13.20 2 0 -16 32.60 13.00 2 0 -16 -8.00 18.80 2 0 -16 4.20 22.00 2 0 -16 -3.40 20.10 -2 0 16 8.00 25.90 -2 0 16 -35.20 18.90 -2 0 16 -4.60 15.80 -2 0 16 -6.20 11.90 -2 0 16 -21.00 13.60 1 0 -16 1.70 20.60 1 0 -16 34.50 18.20 1 0 -16 15.50 11.70 1 0 -16 35.70 16.70 1 0 -16 5.80 22.00 1 0 -16 15.80 18.60 -1 0 16 0.10 15.50 -1 0 16 -3.10 16.20 -1 0 16 -7.80 20.80 0 0 -16 475.35 41.90 0 0 -16 466.25 48.30 0 0 -16 381.86 35.70 0 0 -16 391.66 40.90 0 0 -16 348.47 37.60 0 0 -16 390.06 33.80 0 0 16 415.76 39.70 0 0 16 490.55 44.60 0 0 16 379.96 47.00 -1 0 -16 150.68 29.80 -1 0 -16 101.49 19.60 -1 0 -16 77.99 19.60 -1 0 -16 117.89 23.30 -1 0 -16 154.98 27.10 -1 0 -16 64.19 16.10 1 0 16 91.59 42.70 1 0 16 126.09 28.90 1 0 16 106.59 28.50 -2 0 -16 807.02 61.19 -2 0 -16 735.23 50.29 -2 0 -16 722.33 57.19 -2 0 -16 785.62 55.99 -2 0 -16 665.33 51.29 2 0 16 762.32 61.29 2 0 16 676.03 51.59 2 0 16 716.53 57.09 -3 0 -16 296.07 44.30 -3 0 -16 307.37 35.30 -3 0 -16 332.17 39.80 -3 0 -16 278.97 40.00 -3 0 -16 259.27 38.70 3 0 16 252.47 35.80 3 0 16 279.47 37.50 3 0 16 277.27 40.50 -4 0 -16 -33.60 17.00 -4 0 -16 -23.60 29.80 -4 0 -16 -8.00 24.50 4 0 16 9.10 22.30 4 0 16 17.20 23.90 4 0 16 12.80 23.40 4 0 16 0.20 17.10 2 -1 -16 -4.30 20.90 2 -1 -16 -1.60 22.00 2 -1 -16 -0.30 16.10 2 -1 -16 -38.70 19.90 2 -1 -16 8.10 16.30 -2 1 16 7.50 22.70 -2 1 16 0.50 17.10 -2 1 16 11.40 19.90 1 -1 -16 88.59 27.30 1 -1 -16 121.39 21.70 1 -1 -16 115.49 26.80 1 -1 -16 77.99 24.30 -1 1 16 121.89 25.00 -1 1 16 133.89 31.50 -1 1 16 113.79 26.70 -1 1 16 125.19 34.10 0 -1 -16 128.99 26.90 0 -1 -16 164.18 27.90 0 -1 -16 134.59 22.70 0 -1 -16 160.08 23.80 0 -1 -16 115.49 29.00 0 -1 -16 100.69 23.90 0 1 16 189.38 39.90 0 1 16 134.29 31.50 -1 -1 -16 60.09 21.60 -1 -1 -16 50.69 21.60 -1 -1 -16 38.80 18.70 -1 -1 -16 55.09 23.10 -1 -1 -16 29.50 19.50 -1 -1 -16 44.50 17.00 1 1 16 39.60 17.00 1 1 16 94.59 30.30 1 1 16 64.49 22.50 1 1 16 34.20 22.30 1 1 16 55.69 23.60 -2 -1 -16 63.89 23.20 -2 -1 -16 28.60 23.30 -2 -1 -16 39.80 18.70 -2 -1 -16 32.90 20.50 -2 -1 -16 30.10 16.40 2 1 16 63.89 23.90 2 1 16 13.20 25.50 2 1 16 23.50 17.80 2 1 16 38.20 22.90 2 1 16 42.70 19.50 -3 -1 -16 -5.40 20.90 -3 -1 -16 19.30 16.90 -3 -1 -16 46.90 18.90 -3 -1 -16 8.70 21.00 -3 -1 -16 27.70 19.30 3 1 16 16.80 12.70 3 1 16 34.10 23.40 3 1 16 14.00 15.70 3 1 16 52.99 22.60 3 1 16 21.50 23.50 -4 -1 -16 8.20 23.90 -4 -1 -16 46.40 19.60 -4 -1 -16 42.40 36.00 -4 -1 -16 46.30 20.80 -4 -1 -16 59.69 25.00 4 1 16 58.29 24.50 4 1 16 61.19 26.90 4 1 16 63.39 19.80 4 1 16 86.19 27.20 4 1 16 28.60 24.50 -5 -1 -16 -18.90 26.90 -5 -1 -16 5.30 35.30 5 1 16 10.40 27.70 5 1 16 -7.80 24.10 5 1 16 -5.50 21.70 5 1 16 -28.30 25.80 1 -2 -16 32.90 16.60 1 -2 -16 43.30 21.20 1 -2 -16 20.50 23.70 1 -2 -16 37.40 20.50 1 -2 -16 21.90 21.70 -1 2 16 -1.50 26.70 -1 2 16 1.40 17.00 -1 2 16 41.60 21.70 -1 2 16 -12.80 21.30 -1 2 16 29.60 29.00 0 -2 -16 348.27 38.40 0 -2 -16 240.88 38.10 0 -2 -16 338.57 42.50 0 -2 -16 307.07 41.50 0 2 16 311.77 36.50 0 2 16 298.97 39.30 0 2 16 214.68 42.80 -1 -2 -16 173.98 32.10 -1 -2 -16 164.08 28.10 -1 -2 -16 190.98 29.00 -1 -2 -16 149.88 33.00 -1 -2 -16 152.08 32.70 1 2 16 190.98 29.40 1 2 16 175.08 29.70 1 2 16 169.58 42.00 1 2 16 171.58 31.50 -2 -2 -16 482.95 44.50 -2 -2 -16 452.35 40.50 -2 -2 -16 503.45 45.00 -2 -2 -16 402.16 47.10 -2 -2 -16 386.06 45.30 -2 -2 -16 431.96 49.40 2 2 16 415.76 44.10 2 2 16 421.56 61.29 2 2 16 385.86 42.30 2 2 16 404.96 48.40 -3 -2 -16 216.98 39.40 -3 -2 -16 223.98 36.80 -3 -2 -16 263.37 38.50 -3 -2 -16 242.98 32.50 -3 -2 -16 328.57 45.00 3 2 16 219.88 37.40 3 2 16 266.67 37.20 3 2 16 321.17 33.70 3 2 16 272.37 40.10 3 2 16 302.67 42.20 -4 -2 -16 1028.80 78.59 -4 -2 -16 1270.27 77.39 -4 -2 -16 1217.58 71.49 -4 -2 -16 1141.69 70.69 -4 -2 -16 1226.28 78.49 4 2 16 1220.28 79.79 4 2 16 1012.90 67.19 4 2 16 1185.08 75.89 -5 -2 -16 190.18 46.50 -5 -2 -16 198.88 43.30 5 2 16 229.88 42.60 5 2 16 191.08 38.10 5 2 16 169.58 37.30 5 2 16 246.88 36.70 1 -3 -16 307.67 45.50 1 -3 -16 350.56 39.40 1 -3 -16 322.17 65.69 1 -3 -16 407.36 45.20 -1 3 16 255.87 37.10 0 -3 -16 93.79 22.40 0 -3 -16 34.20 24.30 0 -3 -16 42.00 23.50 0 -3 -16 75.89 26.80 0 -3 -16 56.39 21.40 0 3 16 37.70 27.90 0 3 16 64.09 22.30 0 3 16 86.89 25.20 0 3 16 74.69 25.60 -1 -3 -16 319.17 51.19 -1 -3 -16 283.87 39.30 -1 -3 -16 335.07 37.70 -1 -3 -16 350.36 37.90 1 3 16 325.37 40.20 1 3 16 251.17 38.00 1 3 16 257.07 21.90 1 3 16 222.78 24.30 -2 -3 -16 -24.50 17.80 -2 -3 -16 -19.00 20.90 -2 -3 -16 27.80 18.60 -2 -3 -16 27.50 22.50 -2 -3 -16 -31.30 16.80 -2 -3 -16 6.60 16.00 2 3 16 -4.50 23.50 2 3 16 15.30 23.10 2 3 16 -8.70 17.60 2 3 16 -10.90 13.60 2 3 16 5.90 16.10 2 3 16 5.70 27.90 2 3 16 36.50 24.40 -3 -3 -16 14.90 24.50 -3 -3 -16 0.90 22.50 -3 -3 -16 22.50 18.80 -3 -3 -16 13.50 18.10 -3 -3 -16 -22.20 16.50 -3 -3 -16 15.70 17.90 3 3 16 -8.70 24.00 3 3 16 1.50 16.60 3 3 16 3.40 22.20 3 3 16 0.40 23.50 3 3 16 7.80 17.90 3 3 16 10.70 22.30 3 3 16 -0.60 28.40 -4 -3 -16 4.90 20.00 -4 -3 -16 37.90 26.40 -4 -3 -16 30.00 20.70 -4 -3 -16 45.00 20.20 -4 -3 -16 -14.90 26.70 4 3 16 -16.30 27.50 4 3 16 13.80 24.20 4 3 16 14.50 17.10 4 3 16 0.80 21.30 4 3 16 -15.40 24.30 -5 -3 -16 16.80 24.50 -5 -3 -16 77.39 31.20 5 3 16 26.90 31.80 5 3 16 67.89 29.90 5 3 16 -5.30 22.20 5 3 16 62.49 27.00 5 3 16 53.69 30.00 0 -4 -16 80.69 28.50 0 -4 -16 61.19 22.90 0 -4 -16 105.69 29.20 0 -4 -16 78.59 25.60 0 -4 -16 84.89 31.80 0 4 16 75.89 26.20 0 4 16 27.20 30.20 0 4 16 6.50 31.00 -1 -4 -16 237.98 33.60 -1 -4 -16 221.48 34.30 -1 -4 -16 175.78 32.80 -1 -4 -16 219.28 35.80 -1 -4 -16 254.27 37.50 1 4 16 133.79 22.30 1 4 16 184.28 36.40 1 4 16 281.37 32.60 1 4 16 191.68 42.30 -2 -4 -16 59.59 21.20 -2 -4 -16 87.99 25.00 -2 -4 -16 62.09 25.80 -2 -4 -16 61.99 26.40 -2 -4 -16 102.39 30.60 -2 -4 -16 81.39 21.80 2 4 16 40.10 23.40 2 4 16 103.29 34.30 2 4 16 39.30 16.80 2 4 16 76.89 22.10 2 4 16 91.49 33.30 -3 -4 -16 11.20 23.50 -3 -4 -16 23.10 24.40 -3 -4 -16 19.80 18.70 -3 -4 -16 -12.90 16.80 -3 -4 -16 19.60 21.50 -3 -4 -16 21.90 19.40 3 4 16 15.20 23.10 3 4 16 5.60 15.80 3 4 16 37.50 28.20 3 4 16 2.80 20.10 3 4 16 19.90 28.50 -4 -4 -16 72.69 26.80 -4 -4 -16 74.69 20.50 -4 -4 -16 86.69 25.20 -4 -4 -16 45.30 28.90 4 4 16 58.99 22.60 4 4 16 88.99 27.40 4 4 16 67.29 23.80 4 4 16 34.90 28.60 4 4 16 22.80 32.30 4 4 16 73.19 29.50 -5 -4 -16 -33.60 29.60 -5 -4 -16 -38.20 20.30 5 4 16 -7.60 20.70 5 4 16 -15.40 23.80 5 4 16 -21.50 27.80 -1 -5 -16 257.47 57.69 -1 -5 -16 252.77 35.60 -1 -5 -16 226.48 41.10 1 5 16 208.78 43.70 1 5 16 191.38 36.50 -2 -5 -16 35.80 23.00 -2 -5 -16 21.20 19.70 -2 -5 -16 20.10 22.70 -2 -5 -16 103.79 31.90 2 5 16 42.40 35.40 2 5 16 21.20 24.10 2 5 16 63.09 20.90 -3 -5 -16 -22.30 19.30 -3 -5 -16 21.40 27.90 -3 -5 -16 -15.30 19.30 3 5 16 22.70 23.50 3 5 16 2.10 22.90 3 5 16 27.60 28.40 3 5 16 16.90 20.80 3 5 16 5.50 31.80 -4 -5 -16 117.89 30.40 -4 -5 -16 124.79 37.20 4 5 16 143.49 37.40 4 5 16 81.09 21.20 4 5 16 155.68 34.90 4 5 16 145.79 35.50 4 5 16 25.60 35.90 -5 -5 -16 6.60 21.70 -5 -5 -16 -8.80 42.80 5 5 16 -8.60 20.70 5 5 16 48.10 38.80 5 5 16 36.80 31.30 5 5 16 -9.30 29.50 5 5 16 -9.00 26.90 -2 -6 -16 144.69 39.00 -2 -6 -16 188.98 41.70 2 6 16 142.59 36.70 2 6 16 274.77 47.10 -3 -6 -16 88.69 33.60 -3 -6 -16 92.39 27.40 3 6 16 -2.90 36.80 3 6 16 105.99 32.20 3 6 16 106.79 26.30 -4 -6 -16 48.40 31.80 -4 -6 -16 -0.80 22.50 4 6 16 26.60 22.20 4 6 16 23.60 32.40 4 6 16 19.70 26.90 4 6 16 5.90 29.40 4 6 16 -11.90 39.20 0 0 -17 209.98 34.20 0 0 -17 265.57 29.80 0 0 -17 240.28 37.40 0 0 -17 306.27 35.20 0 0 -17 188.98 29.00 0 0 17 236.58 40.00 0 0 17 233.08 30.90 0 0 17 221.38 38.90 -1 0 -17 2.50 21.30 -1 0 -17 22.90 16.90 -1 0 -17 5.10 17.40 -1 0 -17 -1.40 20.50 -1 0 -17 -0.80 15.90 1 0 17 -5.50 20.30 1 0 17 -26.80 27.00 1 0 17 -11.80 19.60 1 0 17 -3.90 25.40 -2 0 -17 -2.30 22.80 -2 0 -17 9.80 19.30 -2 0 -17 9.60 16.90 -2 0 -17 -24.00 21.90 2 0 17 -1.40 23.40 2 0 17 -23.90 18.10 2 0 17 -46.80 29.20 2 0 17 -17.10 23.50 0 -1 -17 23.90 21.80 0 -1 -17 87.39 19.50 0 -1 -17 75.69 25.80 0 -1 -17 31.20 26.40 0 -1 -17 101.19 21.20 0 1 17 70.89 25.10 0 1 17 11.60 26.90 0 1 17 52.29 22.80 0 1 17 53.79 29.10 -1 -1 -17 383.36 48.60 -1 -1 -17 434.56 40.30 -1 -1 -17 443.36 49.00 -1 -1 -17 463.25 40.80 1 1 17 503.35 58.39 1 1 17 422.56 48.20 -2 -1 -17 122.19 24.30 -2 -1 -17 104.69 29.00 -2 -1 -17 125.09 24.80 -2 -1 -17 101.09 22.40 -2 -1 -17 114.09 31.70 2 1 17 76.39 29.40 2 1 17 79.69 27.50 -3 -1 -17 -60.79 24.20 -3 -1 -17 11.00 19.70 -3 -1 -17 36.40 24.80 3 1 17 4.90 22.10 3 1 17 -7.20 29.10 3 1 17 -1.90 13.60 3 1 17 -23.40 20.20 3 1 17 35.00 31.90 3 1 17 1.40 27.30 0 -2 -17 56.89 19.80 0 -2 -17 39.90 24.70 0 -2 -17 43.90 23.10 0 -2 -17 80.19 30.10 0 2 17 -18.20 29.20 0 2 17 60.49 28.30 -1 -2 -17 194.28 35.30 -1 -2 -17 154.38 33.70 -1 -2 -17 126.39 31.70 -1 -2 -17 133.19 24.70 1 2 17 172.68 38.90 1 2 17 134.69 31.50 -2 -2 -17 26.60 27.70 -2 -2 -17 -4.30 17.90 -2 -2 -17 9.10 24.60 -2 -2 -17 52.39 20.90 -2 -2 -17 10.00 22.00 2 2 17 -4.00 15.80 2 2 17 -31.10 24.90 2 2 17 18.00 23.20 2 2 17 -9.40 22.80 2 2 17 -10.20 14.80 2 2 17 -29.90 27.60 -3 -2 -17 2.70 19.20 -3 -2 -17 -1.10 27.30 3 2 17 -6.50 15.60 3 2 17 -37.20 17.90 3 2 17 -9.70 24.10 3 2 17 -2.30 26.70 3 2 17 -17.10 25.90 3 2 17 -22.50 32.80 -1 -3 -17 83.39 23.70 -1 -3 -17 141.39 33.20 -1 -3 -17 80.49 25.60 -1 -3 -17 116.09 32.50 1 3 17 89.79 33.10 1 3 17 9.90 34.90 1 3 17 12.00 23.30 -2 -3 -17 108.99 27.80 -2 -3 -17 143.29 29.60 -2 -3 -17 135.99 36.30 2 3 17 146.89 33.00 2 3 17 141.69 33.30 -3 -3 -17 155.68 30.40 -3 -3 -17 194.98 35.00 -3 -3 -17 155.08 36.50 3 3 17 158.98 28.80 3 3 17 256.17 43.00 -2 -4 -17 9.30 29.70 2 4 17 36.80 30.60 2 4 17 -17.30 18.20 2 4 17 65.19 34.00 2 4 17 2.70 31.30 -3 -4 -17 154.88 38.80 3 4 17 66.09 23.00 3 4 17 86.89 31.80 3 4 17 114.29 34.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 20399 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Cl1 Cl -0.41196(5) 0.18903(4) 0.54750(3) 0.02031(9) Uani 1 1 d . . . . . Cl2 Cl -0.29558(5) 0.67177(4) 0.09376(3) 0.02199(10) Uani 1 1 d . . . . . O4 O 0.02112(15) -0.08192(12) 0.27025(8) 0.0214(2) Uani 1 1 d . . . . . O1 O -0.67926(14) 0.26655(14) 0.39823(8) 0.0241(2) Uani 1 1 d . . . . . H1 H -0.612396 0.243957 0.447269 0.036 Uiso 1 1 calc R U . . . O2 O -0.24039(15) 0.14685(12) 0.02510(8) 0.0207(2) Uani 1 1 d . . . . . O3 O 0.02147(16) 0.51524(13) 0.21283(9) 0.0261(2) Uani 1 1 d . . . . . H3 H -0.067801 0.575499 0.178749 0.039 Uiso 1 1 calc R U . . . N1 N -0.56258(17) 0.23939(15) 0.30451(9) 0.0185(3) Uani 1 1 d . . . . . N2 N 0.01735(17) 0.36478(15) 0.23024(9) 0.0194(3) Uani 1 1 d . . . . . C9 C -0.06430(19) 0.17271(17) 0.33942(11) 0.0167(3) Uani 1 1 d . . . . . H9 H -0.120480 0.140701 0.403865 0.020 Uiso 1 1 calc R U . . . C2 C -0.4135(2) 0.33359(17) 0.15597(11) 0.0165(3) Uani 1 1 d . . . . . H2 H -0.383145 0.416806 0.116809 0.020 Uiso 1 1 calc R U . . . C10 C 0.0191(2) 0.06561(17) 0.26219(11) 0.0179(3) Uani 1 1 d . . . . . C1 C -0.52168(19) 0.36104(17) 0.25203(11) 0.0173(3) Uani 1 1 d . . . . . C4 C -0.3947(2) 0.06240(17) 0.17451(12) 0.0198(3) Uani 1 1 d . . . . . H4 H -0.351505 -0.040011 0.148778 0.024 Uiso 1 1 calc R U . . . C3 C -0.34883(19) 0.18451(17) 0.11621(11) 0.0170(3) Uani 1 1 d . . . . . C8 C -0.06596(19) 0.32530(17) 0.32297(11) 0.0172(3) Uani 1 1 d . . . . . C5 C -0.5024(2) 0.09322(17) 0.26876(11) 0.0198(3) Uani 1 1 d . . . . . H5 H -0.535088 0.012046 0.309235 0.024 Uiso 1 1 calc R U . . . C14 C -0.0594(2) -0.13750(18) 0.36751(12) 0.0232(3) Uani 1 1 d . . . . . H14A H -0.060050 -0.242216 0.360516 0.035 Uiso 1 1 calc R U . . . H14B H -0.189933 -0.061272 0.385212 0.035 Uiso 1 1 calc R U . . . H14C H 0.017209 -0.146697 0.422734 0.035 Uiso 1 1 calc R U . . . C6 C -0.5934(2) 0.51544(18) 0.30059(12) 0.0223(3) Uani 1 1 d . . . . . H6A H -0.732700 0.562668 0.307044 0.033 Uiso 1 1 calc R U . . . H6B H -0.543596 0.588549 0.256939 0.033 Uiso 1 1 calc R U . . . H6C H -0.551337 0.496895 0.369789 0.033 Uiso 1 1 calc R U . . . C13 C -0.1524(2) 0.44617(17) 0.40131(12) 0.0215(3) Uani 1 1 d . . . . . H13A H -0.052578 0.469711 0.424117 0.032 Uiso 1 1 calc R U . . . H13B H -0.217016 0.404289 0.461316 0.032 Uiso 1 1 calc R U . . . H13C H -0.244584 0.544231 0.370165 0.032 Uiso 1 1 calc R U . . . C11 C 0.1044(2) 0.11342(19) 0.16799(11) 0.0215(3) Uani 1 1 d . . . . . H11 H 0.163242 0.041723 0.114711 0.026 Uiso 1 1 calc R U . . . C12 C 0.1017(2) 0.26373(19) 0.15400(11) 0.0227(3) Uani 1 1 d . . . . . H12 H 0.159057 0.297672 0.090659 0.027 Uiso 1 1 calc R U . . . C7 C -0.2032(2) 0.27333(18) -0.04083(11) 0.0233(3) Uani 1 1 d . . . . . H7A H -0.124349 0.230437 -0.105083 0.035 Uiso 1 1 calc R U . . . H7B H -0.136342 0.317101 -0.004134 0.035 Uiso 1 1 calc R U . . . H7C H -0.323891 0.358112 -0.057918 0.035 Uiso 1 1 calc R U . . . 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 Cl1 0.02330(18) 0.02153(18) 0.01697(17) -0.00158(13) 0.00026(13) -0.01061(14) Cl2 0.0276(2) 0.01937(18) 0.02028(18) -0.00099(13) -0.00023(14) -0.01166(15) O4 0.0236(5) 0.0185(5) 0.0216(5) -0.0060(4) -0.0008(4) -0.0072(4) O1 0.0181(5) 0.0354(6) 0.0164(5) -0.0009(4) 0.0019(4) -0.0099(5) O2 0.0256(5) 0.0183(5) 0.0182(5) -0.0051(4) 0.0020(4) -0.0091(4) O3 0.0342(6) 0.0254(6) 0.0270(6) 0.0054(5) -0.0093(5) -0.0204(5) N1 0.0161(6) 0.0234(6) 0.0157(6) -0.0006(5) -0.0009(5) -0.0079(5) N2 0.0220(6) 0.0217(6) 0.0184(6) 0.0012(5) -0.0045(5) -0.0126(5) C9 0.0153(7) 0.0202(7) 0.0141(6) -0.0017(5) -0.0024(5) -0.0060(6) C2 0.0182(7) 0.0165(7) 0.0164(7) -0.0005(5) -0.0036(5) -0.0081(6) C10 0.0148(7) 0.0194(7) 0.0191(7) -0.0025(5) -0.0050(5) -0.0049(6) C1 0.0159(7) 0.0193(7) 0.0184(7) -0.0019(5) -0.0053(5) -0.0073(6) C4 0.0193(7) 0.0150(7) 0.0253(7) -0.0021(6) -0.0051(6) -0.0059(6) C3 0.0154(7) 0.0188(7) 0.0167(7) -0.0018(5) -0.0043(5) -0.0057(6) C8 0.0149(7) 0.0204(7) 0.0164(7) -0.0010(5) -0.0042(5) -0.0064(6) C5 0.0178(7) 0.0179(7) 0.0241(7) 0.0033(6) -0.0061(6) -0.0076(6) C14 0.0269(8) 0.0184(7) 0.0247(8) 0.0009(6) -0.0048(6) -0.0094(6) C6 0.0219(7) 0.0233(8) 0.0219(7) -0.0073(6) -0.0001(6) -0.0085(6) C13 0.0223(7) 0.0193(7) 0.0231(7) -0.0045(6) -0.0014(6) -0.0078(6) C11 0.0190(7) 0.0288(8) 0.0176(7) -0.0083(6) -0.0001(6) -0.0089(6) C12 0.0217(7) 0.0352(9) 0.0149(7) -0.0027(6) -0.0013(6) -0.0150(7) C7 0.0302(8) 0.0241(8) 0.0168(7) -0.0025(6) 0.0017(6) -0.0133(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Cl Cl 0.1484 0.1585 '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' 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 C10 O4 C14 118.00(11) . . ? N1 O1 H1 109.5 . . ? C3 O2 C7 117.71(11) . . ? N2 O3 H3 109.5 . . ? C1 N1 O1 118.72(12) . . ? C5 N1 O1 117.50(12) . . ? C5 N1 C1 123.72(12) . . ? C8 N2 O3 118.63(12) . . ? C12 N2 O3 117.66(12) . . ? C12 N2 C8 123.69(13) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C8 C9 C10 120.53(13) . . ? C1 C2 H2 119.8 . . ? C1 C2 C3 120.43(13) . . ? C3 C2 H2 119.8 . . ? O4 C10 C9 124.39(13) . . ? O4 C10 C11 116.40(13) . . ? C9 C10 C11 119.20(13) . . ? N1 C1 C2 117.65(13) . . ? N1 C1 C6 118.59(13) . . ? C2 C1 C6 123.76(13) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C5 C4 C3 118.87(13) . . ? O2 C3 C2 124.29(13) . . ? O2 C3 C4 116.30(13) . . ? C2 C3 C4 119.39(13) . . ? N2 C8 C9 117.52(13) . . ? N2 C8 C13 118.81(13) . . ? C9 C8 C13 123.67(13) . . ? N1 C5 C4 119.93(13) . . ? N1 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? O4 C14 H14A 109.5 . . ? O4 C14 H14B 109.5 . . ? O4 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C11 H11 120.4 . . ? C12 C11 C10 119.11(14) . . ? C12 C11 H11 120.4 . . ? N2 C12 C11 119.95(14) . . ? N2 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? 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 O4 C10 1.3384(17) . ? O4 C14 1.4455(18) . ? O1 H1 0.8400 . ? O1 N1 1.3850(15) . ? O2 C3 1.3388(17) . ? O2 C7 1.4471(17) . ? O3 H3 0.8400 . ? O3 N2 1.3820(15) . ? N1 C1 1.3521(18) . ? N1 C5 1.3519(19) . ? N2 C8 1.3537(18) . ? N2 C12 1.3511(19) . ? C9 H9 0.9500 . ? C9 C10 1.394(2) . ? C9 C8 1.384(2) . ? C2 H2 0.9500 . ? C2 C1 1.383(2) . ? C2 C3 1.395(2) . ? C10 C11 1.403(2) . ? C1 C6 1.486(2) . ? C4 H4 0.9500 . ? C4 C3 1.403(2) . ? C4 C5 1.364(2) . ? C8 C13 1.486(2) . ? C5 H5 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C11 H11 0.9500 . ? C11 C12 1.359(2) . ? C12 H12 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? 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 O4 C10 C11 C12 178.03(13) . . . . ? O1 N1 C1 C2 -176.52(12) . . . . ? O1 N1 C1 C6 3.94(18) . . . . ? O1 N1 C5 C4 176.88(12) . . . . ? O3 N2 C8 C9 -178.52(12) . . . . ? O3 N2 C8 C13 1.08(19) . . . . ? O3 N2 C12 C11 178.88(13) . . . . ? C9 C10 C11 C12 -0.7(2) . . . . ? C10 C9 C8 N2 -0.6(2) . . . . ? C10 C9 C8 C13 179.85(13) . . . . ? C10 C11 C12 N2 -0.1(2) . . . . ? C1 N1 C5 C4 -0.3(2) . . . . ? C1 C2 C3 O2 -178.55(13) . . . . ? C1 C2 C3 C4 0.1(2) . . . . ? C3 C2 C1 N1 -0.5(2) . . . . ? C3 C2 C1 C6 179.00(13) . . . . ? C3 C4 C5 N1 -0.1(2) . . . . ? C8 N2 C12 C11 0.6(2) . . . . ? C8 C9 C10 O4 -177.58(13) . . . . ? C8 C9 C10 C11 1.1(2) . . . . ? C5 N1 C1 C2 0.6(2) . . . . ? C5 N1 C1 C6 -178.92(13) . . . . ? C5 C4 C3 O2 178.99(13) . . . . ? C5 C4 C3 C2 0.2(2) . . . . ? C14 O4 C10 C9 -3.5(2) . . . . ? C14 O4 C10 C11 177.85(12) . . . . ? C12 N2 C8 C9 -0.3(2) . . . . ? C12 N2 C8 C13 179.33(13) . . . . ? C7 O2 C3 C2 -6.2(2) . . . . ? C7 O2 C3 C4 175.09(12) . . . . ?