#------------------------------------------------------------------------------ #$Date: 2024-10-22 01:10:36 +0300 (Tue, 22 Oct 2024) $ #$Revision: 295572 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/29/1572916.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_1572916 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 'Cl3, C16 H23 N2 O2' _chemical_formula_sum 'C16 H23 Cl3 N2 O2' _chemical_formula_weight 381.71 _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 mixed _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 68.449(6) _cell_angle_beta 65.454(6) _cell_angle_gamma 78.430(7) _cell_formula_units_Z 1 _cell_length_a 7.2228(13) _cell_length_b 8.5908(16) _cell_length_c 8.6321(17) _cell_measurement_reflns_used 5675 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 26.299 _cell_measurement_theta_min 2.553 _cell_volume 452.42(15) _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 0.0761 _diffrn_reflns_av_unetI/netI 0.0406 _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 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 14067 _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 26.373 _diffrn_reflns_theta_min 2.553 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.516 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.5554 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1192 before and 0.0822 after correction. The Ratio of minimum to maximum transmission is 0.7451. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.401 _exptl_crystal_description block _exptl_crystal_F_000 200 _exptl_crystal_size_max 0.235 _exptl_crystal_size_mid 0.199 _exptl_crystal_size_min 0.177 _refine_diff_density_max 0.308 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.062 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 110 _refine_ls_number_reflns 1840 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0339 _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^)+(0.0431P)^2^+0.2785P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0848 _refine_ls_wR_factor_ref 0.0954 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1497 _reflns_number_total 1840 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06270a3.cif _cod_data_source_block OGH_D49_42 _cod_database_code 1572916 _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 0.914 _shelx_estimated_absorpt_t_min 0.888 _olex2_refinement_description ; 1.a Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4) 1.b Idealised Me refined as rotating group: C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C) ; _shelx_res_file ; TITL full1_P-1_a.res in P-1 full1_p-1_a.res created by SHELXL-2019/1 at 17:42:26 on 16-Apr-2024 REM Old TITL full1_P-1 in P-1 REM SHELXT solution in P-1: R1 0.095, Rweak 0.002, Alpha 0.017 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C16 Cl3 N2 O2 CELL 0.71073 7.2228 8.5908 8.6321 68.449 65.454 78.43 ZERR 1 0.0013 0.0016 0.0017 0.006 0.006 0.007 LATT 1 SFAC C H Cl N O UNIT 16 23 3 2 2 L.S. 10 PLAN 2 SIZE 0.177 0.199 0.235 TEMP -173.15 CONF LIST 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.043100 0.278500 FVAR 1.66818 CL1 3 1.000000 0.000000 1.000000 10.50000 0.01844 0.01621 = 0.02248 -0.00468 -0.00362 -0.00380 CL2 3 0.996602 -0.070683 0.769268 11.00000 0.02468 0.02338 = 0.02716 -0.00936 -0.00579 -0.00511 O1 5 0.420551 0.491134 0.904703 11.00000 0.01481 0.02816 = 0.00913 -0.00715 0.00046 -0.00398 N1 4 0.561376 0.499944 0.736858 11.00000 0.01280 0.01936 = 0.00917 -0.00419 -0.00290 -0.00237 C2 1 0.770447 0.659845 0.449743 11.00000 0.01628 0.01706 = 0.01300 -0.00225 -0.00692 -0.00338 AFIX 43 H2 2 0.823982 0.764401 0.367655 11.00000 -1.20000 AFIX 0 C4 1 0.750244 0.367136 0.518994 11.00000 0.01568 0.01707 = 0.01564 -0.00670 -0.00714 -0.00086 AFIX 43 H4 2 0.789081 0.268599 0.484729 11.00000 -1.20000 AFIX 0 C5 1 0.615135 0.357319 0.691732 11.00000 0.01507 0.01706 = 0.01577 -0.00435 -0.00740 -0.00251 C1 1 0.634609 0.651477 0.621643 11.00000 0.01339 0.01707 = 0.01583 -0.00419 -0.00756 -0.00114 C3 1 0.830511 0.518404 0.394288 11.00000 0.01371 0.02176 = 0.01295 -0.00616 -0.00674 -0.00090 C6 1 0.565232 0.798900 0.688180 11.00000 0.02335 0.01830 = 0.02003 -0.00872 -0.00712 -0.00020 AFIX 137 H6A 2 0.416071 0.812308 0.732713 11.00000 -1.50000 H6B 2 0.622945 0.900129 0.589728 11.00000 -1.50000 H6C 2 0.611106 0.781105 0.785809 11.00000 -1.50000 AFIX 0 C8 1 0.528172 0.198285 0.831614 11.00000 0.02241 0.01770 = 0.01656 -0.00339 -0.00379 -0.00462 AFIX 137 H8A 2 0.581004 0.168064 0.927337 11.00000 -1.50000 H8B 2 0.567103 0.108625 0.777360 11.00000 -1.50000 H8C 2 0.379227 0.213593 0.882125 11.00000 -1.50000 AFIX 0 C7 1 0.975324 0.529281 0.206011 11.00000 0.01764 0.02452 = 0.01238 -0.00720 -0.00250 -0.00135 AFIX 137 H7A 2 0.898068 0.555789 0.128343 11.00000 -1.50000 H7B 2 1.052697 0.421643 0.205842 11.00000 -1.50000 H7C 2 1.069621 0.617503 0.161095 11.00000 -1.50000 AFIX 0 H1 2 0.500000 0.500000 1.000000 10.50000 0.07155 HKLF 4 REM full1_P-1_a.res in P-1 REM wR2 = 0.0954, GooF = S = 1.048, Restrained GooF = 1.048 for all data REM R1 = 0.0339 for 1497 Fo > 4sig(Fo) and 0.0479 for all 1840 data REM 110 parameters refined using 0 restraints END WGHT 0.0431 0.2785 REM Highest difference peak 0.308, deepest hole -0.352, 1-sigma level 0.062 Q1 1 1.0098 0.1381 0.4750 11.00000 0.05 0.31 Q2 1 0.8052 0.5798 0.4243 11.00000 0.05 0.29 ; _shelx_res_checksum 15097 _shelx_hkl_file ; -1 0 0 4.90 2.30 -1 0 0 3.40 1.70 -1 0 0 4.20 2.00 -1 0 0 7.20 2.30 -1 0 0 5.90 2.30 1 0 0 5.10 2.40 1 0 0 2.70 1.80 -3 0 0 1530.35 114.89 -3 0 0 1665.63 115.59 -3 0 0 1735.33 116.69 -3 0 0 1614.04 117.49 -3 0 0 1488.95 117.39 3 0 0 1497.65 117.29 3 0 0 1633.14 114.49 3 0 0 1675.93 117.49 -4 0 0 1440.76 105.49 -4 0 0 1317.77 107.89 -4 0 0 1471.05 106.29 -4 0 0 1407.86 104.69 -4 0 0 1357.36 107.09 4 0 0 1331.17 102.39 4 0 0 1404.66 108.29 4 0 0 1504.25 107.59 -5 0 0 4253.17 276.87 -5 0 0 3622.44 276.27 -5 0 0 3670.23 280.77 -5 0 0 4088.39 278.77 5 0 0 3462.35 278.47 5 0 0 4249.17 280.07 5 0 0 3727.53 272.17 5 0 0 4344.07 271.67 -6 0 0 244.78 30.20 -6 0 0 189.58 33.40 -6 0 0 194.68 32.30 -6 0 0 158.48 33.50 -6 0 0 206.58 34.30 6 0 0 195.58 23.30 6 0 0 168.48 32.60 -7 0 0 722.73 72.69 -7 0 0 737.03 77.39 -7 0 0 724.23 70.19 -7 0 0 885.31 79.59 -8 0 0 379.76 50.99 -8 0 0 255.37 47.20 -8 0 0 335.97 55.99 -8 0 0 345.17 52.99 8 -1 0 256.77 35.50 -8 1 0 282.47 45.10 -8 1 0 197.18 47.60 -8 1 0 258.17 47.20 -8 1 0 202.68 43.90 7 -1 0 277.17 33.20 7 -1 0 209.28 42.70 -7 1 0 238.08 43.70 -7 1 0 185.88 41.50 -7 1 0 236.18 41.20 -7 1 0 244.08 38.20 -7 1 0 311.57 48.20 6 -1 0 1441.36 124.79 6 -1 0 1654.73 116.59 6 -1 0 1384.16 115.49 6 -1 0 1812.22 156.88 -6 1 0 1589.74 127.29 -6 1 0 1624.74 122.09 -6 1 0 1582.64 124.69 -6 1 0 1353.76 124.99 -6 1 0 1444.56 121.49 5 -1 0 55.69 13.30 5 -1 0 35.60 11.30 5 -1 0 29.90 13.30 5 -1 0 19.90 13.50 -5 1 0 5.70 11.60 -5 1 0 33.40 14.90 -5 1 0 31.40 12.60 -5 1 0 25.30 12.90 -5 1 0 11.60 9.70 4 -1 0 1335.87 103.79 4 -1 0 1430.96 114.49 4 -1 0 1374.56 109.09 4 -1 0 1471.55 103.69 -4 1 0 1288.57 108.59 -4 1 0 1374.76 108.39 -4 1 0 1469.95 106.89 -4 1 0 1397.86 105.49 -4 1 0 1311.17 105.49 3 -1 0 2013.80 162.08 3 -1 0 2327.57 163.38 3 -1 0 2409.26 159.68 3 -1 0 2339.27 160.08 -3 1 0 1998.60 162.18 -3 1 0 2230.38 160.58 -3 1 0 2361.16 160.78 -3 1 0 2246.48 160.68 -3 1 0 2293.27 163.08 2 -1 0 2069.39 159.88 2 -1 0 2481.85 159.28 2 -1 0 2183.18 160.08 2 -1 0 2297.17 158.18 2 -1 0 2328.67 158.18 -2 1 0 2378.96 158.88 -2 1 0 2331.47 158.78 -2 1 0 2079.89 159.98 -2 1 0 2111.69 159.48 -2 1 0 2343.77 158.68 0 -1 0 1502.85 104.39 0 -1 0 1474.35 104.99 0 -1 0 1590.54 104.29 0 -1 0 1609.64 102.99 0 -1 0 1458.55 105.09 0 1 0 1493.35 104.19 0 1 0 1674.93 104.49 0 1 0 1469.35 104.99 0 1 0 1477.75 105.29 -2 -1 0 2929.31 188.48 -2 -1 0 2957.30 188.28 -2 -1 0 3062.49 190.48 -2 -1 0 2688.03 188.98 -2 -1 0 2537.85 189.68 2 1 0 2510.95 187.48 2 1 0 2475.85 189.48 2 1 0 3036.30 189.98 -3 -1 0 1803.82 122.49 -3 -1 0 1628.64 122.79 -3 -1 0 1627.74 124.29 -3 -1 0 1685.33 121.49 -3 -1 0 1747.73 124.29 3 1 0 1840.12 123.89 3 1 0 1860.51 119.79 3 1 0 1683.83 120.59 -4 -1 0 1764.92 126.99 -4 -1 0 1558.34 126.79 -4 -1 0 1778.42 124.79 -4 -1 0 1668.33 123.29 -4 -1 0 1674.23 125.29 4 1 0 1853.81 126.39 4 1 0 1596.34 120.89 4 1 0 1869.71 120.19 -5 -1 0 110.39 20.70 -5 -1 0 152.68 24.90 -5 -1 0 112.19 19.60 -5 -1 0 141.99 23.30 5 1 0 164.08 21.80 5 1 0 127.99 16.30 5 1 0 160.28 16.00 5 1 0 126.09 23.70 -6 -1 0 796.42 70.69 -6 -1 0 779.12 67.59 -6 -1 0 894.31 72.69 -6 -1 0 777.52 74.19 -6 -1 0 879.01 73.69 6 1 0 876.41 71.79 6 1 0 643.24 74.79 6 1 0 795.82 59.59 -7 -1 0 160.58 31.00 -7 -1 0 198.08 34.80 -7 -1 0 143.39 30.90 -7 -1 0 170.08 28.50 -7 -1 0 216.58 35.70 7 1 0 139.89 31.40 7 1 0 161.78 43.30 -8 -1 0 254.27 54.29 -8 -1 0 390.26 50.89 -8 -1 0 300.27 43.10 -8 -1 0 247.98 47.40 7 -2 0 423.76 59.99 7 -2 0 541.35 54.59 -7 2 0 457.95 57.09 -7 2 0 465.55 67.79 -7 2 0 523.85 58.19 -7 2 0 432.26 59.29 6 -2 0 350.16 39.80 6 -2 0 319.77 44.00 6 -2 0 313.97 38.70 6 -2 0 345.57 51.29 -6 2 0 371.46 42.80 -6 2 0 329.57 52.29 -6 2 0 305.87 46.00 -6 2 0 374.96 45.00 -6 2 0 363.86 55.29 5 -2 0 1119.49 104.09 5 -2 0 1317.17 105.99 5 -2 0 1209.38 98.39 -5 2 0 1102.59 103.89 -5 2 0 1421.86 108.19 -5 2 0 1184.18 100.89 -5 2 0 1302.57 101.59 -5 2 0 1232.18 101.59 4 -2 0 696.73 57.39 4 -2 0 692.13 62.19 4 -2 0 637.64 56.09 4 -2 0 593.54 59.39 -4 2 0 567.74 59.29 -4 2 0 637.94 60.29 -4 2 0 705.03 59.19 -4 2 0 585.64 56.49 3 -2 0 1018.80 83.59 3 -2 0 1044.30 79.69 3 -2 0 1055.59 83.49 3 -2 0 1002.70 79.49 -3 2 0 972.70 84.49 -3 2 0 1060.09 80.89 -3 2 0 924.11 81.39 -3 2 0 1035.60 80.29 -3 2 0 988.90 83.29 2 -2 0 2768.62 191.88 2 -2 0 2889.81 192.58 2 -2 0 2813.22 191.98 2 -2 0 2749.62 194.98 2 -2 0 2704.03 194.58 -2 2 0 2671.83 191.68 -2 2 0 2559.84 194.18 -2 2 0 2706.13 192.18 -2 2 0 2684.43 191.68 -2 2 0 2720.23 194.88 1 -2 0 3773.92 256.67 1 -2 0 3670.53 258.77 1 -2 0 3837.32 256.87 1 -2 0 3799.22 256.87 1 -2 0 3766.42 258.87 -1 2 0 3744.13 256.67 -1 2 0 3757.22 256.57 -1 2 0 3456.05 257.97 -1 2 0 3674.93 258.67 -1 2 0 3915.31 256.97 0 -2 0 5132.69 354.06 0 -2 0 5257.47 352.66 0 2 0 4958.50 353.56 0 2 0 5514.55 352.26 -1 -2 0 4518.75 307.17 -1 -2 0 4790.92 308.37 -1 -2 0 4432.86 307.17 -1 -2 0 4495.85 305.67 1 2 0 4262.17 308.17 1 2 0 4849.81 306.37 -2 -2 0 4657.43 296.57 2 2 0 4143.79 293.97 2 2 0 4700.23 299.87 2 2 0 4086.19 293.47 -3 -2 0 1334.47 89.29 -3 -2 0 1290.37 90.89 -3 -2 0 1167.88 86.79 -3 -2 0 1316.67 91.59 -3 -2 0 1208.58 89.69 3 2 0 1226.18 84.79 3 2 0 1219.28 90.99 -4 -2 0 558.14 40.90 -4 -2 0 502.85 44.80 -4 -2 0 552.44 43.90 -4 -2 0 463.45 41.80 -4 -2 0 553.14 44.80 4 2 0 496.15 35.40 4 2 0 486.65 43.80 -5 -2 0 977.50 81.29 -5 -2 0 1074.79 84.69 -5 -2 0 1043.70 77.89 -5 -2 0 888.91 82.59 -5 -2 0 1057.09 83.09 5 2 0 1165.88 82.09 -6 -2 0 500.55 47.00 -6 -2 0 378.76 45.60 -6 -2 0 520.35 43.60 -6 -2 0 460.35 46.50 6 2 0 427.26 45.40 6 2 0 514.65 46.90 -7 -2 0 1196.88 110.19 -7 -2 0 1328.37 109.89 -7 -2 0 1311.77 107.69 -7 -2 0 1553.64 112.69 -7 -2 0 1304.57 101.69 7 2 0 1170.18 106.69 -8 -2 0 12.40 18.10 -8 -2 0 -17.40 20.10 -8 -2 0 -5.90 16.20 -8 -2 0 -5.00 18.20 8 2 0 -6.80 25.50 7 -3 0 2.40 21.70 7 -3 0 5.20 26.60 7 -3 0 -13.40 17.10 -7 3 0 11.90 21.20 -7 3 0 -27.70 18.10 -7 3 0 8.20 17.00 6 -3 0 159.48 31.70 6 -3 0 175.48 32.80 6 -3 0 149.59 34.80 6 -3 0 144.79 28.10 -6 3 0 149.19 33.10 -6 3 0 182.98 39.20 -6 3 0 209.18 33.80 -6 3 0 149.99 34.40 -6 3 0 129.79 36.90 5 -3 0 126.49 25.00 5 -3 0 98.69 26.90 5 -3 0 121.09 28.40 5 -3 0 126.99 23.70 -5 3 0 116.49 24.70 -5 3 0 108.69 22.30 -5 3 0 67.99 21.40 -5 3 0 75.49 21.80 -5 3 0 56.39 23.70 4 -3 0 391.06 44.60 4 -3 0 377.26 43.30 4 -3 0 427.76 41.30 4 -3 0 321.37 39.10 -4 3 0 401.86 41.80 -4 3 0 332.47 43.20 -4 3 0 348.47 43.50 -4 3 0 320.07 39.60 -4 3 0 439.16 42.60 3 -3 0 1898.41 147.79 3 -3 0 2020.50 144.39 3 -3 0 1763.72 146.99 3 -3 0 2095.99 145.69 3 -3 0 1959.10 143.99 -3 3 0 1905.41 144.79 -3 3 0 2068.89 145.19 -3 3 0 1913.91 143.89 -3 3 0 1787.82 147.39 2 -3 0 225.78 29.70 2 -3 0 246.18 27.30 2 -3 0 216.08 29.40 2 -3 0 294.77 28.50 2 -3 0 238.98 27.20 -2 3 0 306.97 29.50 -2 3 0 240.48 29.50 -2 3 0 282.27 28.50 -2 3 0 247.18 27.70 -2 3 0 273.57 31.20 1 -3 0 2224.88 157.48 1 -3 0 2216.28 157.48 1 -3 0 2184.58 160.18 1 -3 0 2068.69 159.38 1 -3 0 2327.67 157.48 -1 3 0 2175.88 156.78 -1 3 0 2380.06 157.78 -1 3 0 2132.69 159.38 -1 3 0 2253.37 157.18 -1 3 0 2123.79 159.48 0 -3 0 68.89 12.20 0 -3 0 62.89 11.50 0 -3 0 65.39 14.80 0 -3 0 58.49 11.90 0 -3 0 90.29 10.90 0 3 0 60.19 12.10 0 3 0 60.69 10.20 0 3 0 74.09 11.50 0 3 0 68.19 12.70 0 3 0 95.29 11.90 -1 -3 0 2689.83 195.68 -1 -3 0 2865.31 194.28 -1 -3 0 2871.11 195.68 -1 -3 0 2744.43 192.28 -1 -3 0 2944.21 194.28 -1 -3 0 2985.20 191.78 1 3 0 2786.12 192.08 1 3 0 2614.04 192.58 1 3 0 2613.64 195.18 1 3 0 3084.69 192.78 -2 -3 0 1519.85 105.19 -2 -3 0 1426.96 99.59 -2 -3 0 1518.95 103.49 -2 -3 0 1658.73 105.09 -2 -3 0 1495.25 103.39 2 3 0 1430.16 99.49 2 3 0 1349.47 99.59 2 3 0 1380.36 104.39 -3 -3 0 1550.24 114.99 -3 -3 0 1579.64 109.49 -3 -3 0 1674.83 116.69 -3 -3 0 1642.34 114.69 -3 -3 0 1711.53 116.79 3 3 0 1531.95 115.79 3 3 0 1723.13 116.39 -4 -3 0 243.38 24.10 -4 -3 0 230.18 17.70 -4 -3 0 176.08 22.60 -4 -3 0 213.48 21.60 -4 -3 0 219.38 22.80 4 3 0 199.98 22.60 4 3 0 203.98 22.30 -5 -3 0 143.39 18.80 -5 -3 0 119.29 13.70 -5 -3 0 154.68 19.60 -5 -3 0 114.19 21.00 5 3 0 142.49 19.40 5 3 0 102.89 18.30 -6 -3 0 79.99 12.30 -6 -3 0 72.99 18.50 -6 -3 0 47.50 16.10 -6 -3 0 54.19 15.50 -6 -3 0 54.49 14.60 6 3 0 88.49 17.90 -7 -3 0 352.96 44.10 -7 -3 0 313.17 30.00 -7 -3 0 304.37 43.80 -7 -3 0 220.48 38.50 -7 -3 0 351.16 38.60 7 3 0 313.47 39.90 7 -4 0 291.47 44.60 7 -4 0 247.88 55.99 7 -4 0 317.07 47.70 -7 4 0 358.66 53.99 -7 4 0 310.47 56.39 -7 4 0 397.46 66.39 6 -4 0 104.99 24.90 6 -4 0 81.69 30.30 6 -4 0 43.70 25.10 6 -4 0 43.20 25.80 -6 4 0 118.89 37.10 -6 4 0 72.69 34.90 -6 4 0 54.59 26.70 -6 4 0 122.39 27.90 -6 4 0 107.29 29.90 5 -4 0 115.09 26.70 5 -4 0 85.29 21.80 5 -4 0 129.19 24.60 -5 4 0 82.89 22.50 -5 4 0 112.49 29.10 -5 4 0 126.19 27.30 -5 4 0 78.39 27.00 4 -4 0 78.09 24.90 4 -4 0 108.89 22.90 4 -4 0 81.59 25.00 4 -4 0 98.29 24.60 -4 4 0 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-9 -9.40 12.50 -5 -8 -9 23.90 20.10 -5 -8 -9 21.60 17.50 -5 -8 -9 -2.80 16.90 -5 -8 -9 10.40 16.80 -3 0 -10 16.50 27.40 -3 0 -10 33.80 22.70 -3 0 -10 17.80 18.30 -3 0 -10 1.50 20.90 -3 0 -10 -4.30 24.40 3 0 10 14.10 28.50 3 0 10 45.40 24.60 -4 0 -10 -35.30 22.30 -2 -1 -10 6.10 23.60 -2 -1 -10 -5.90 15.10 -2 -1 -10 -15.60 24.00 -2 -1 -10 -17.50 18.40 -2 -1 -10 -15.30 21.90 2 1 10 13.60 18.80 2 1 10 10.70 16.80 -3 -1 -10 58.79 33.50 -3 -1 -10 7.60 15.90 -3 -1 -10 2.70 20.70 -3 -1 -10 -3.90 22.40 -3 -1 -10 20.40 18.40 3 1 10 14.80 17.40 3 1 10 26.00 26.20 3 1 10 15.90 28.00 -4 -1 -10 30.00 19.40 -4 -1 -10 65.99 27.40 -4 -1 -10 69.09 22.70 -4 -1 -10 35.60 21.70 -4 -1 -10 72.19 34.80 4 1 10 58.09 21.30 4 1 10 6.30 25.30 4 1 10 6.20 25.00 -5 -1 -10 50.69 24.70 -5 -1 -10 111.09 28.10 -5 -1 -10 104.59 26.90 -5 -1 -10 4.20 30.40 -5 -1 -10 94.39 28.50 5 1 10 123.69 33.10 5 1 10 72.99 21.20 -1 -2 -10 -12.30 17.50 -1 -2 -10 -11.60 23.60 -1 -2 -10 -8.00 23.40 -1 -2 -10 -21.70 23.70 -1 -2 -10 -11.90 20.70 1 2 10 -36.80 28.30 1 2 10 -17.40 19.50 -2 -2 -10 55.49 35.90 -2 -2 -10 90.29 29.10 -2 -2 -10 10.00 19.60 -2 -2 -10 23.20 16.90 -2 -2 -10 33.40 24.80 2 2 10 64.79 30.20 2 2 10 40.40 29.40 2 2 10 26.40 21.80 -3 -2 -10 24.40 16.20 -3 -2 -10 4.90 17.70 -3 -2 -10 2.00 19.20 -3 -2 -10 18.50 19.70 -3 -2 -10 -4.70 16.60 3 2 10 3.60 23.50 3 2 10 10.70 24.10 3 2 10 -28.30 16.50 -4 -2 -10 51.59 20.30 -4 -2 -10 53.09 21.80 -4 -2 -10 40.30 24.30 -4 -2 -10 38.30 19.00 -4 -2 -10 50.59 31.50 4 2 10 30.20 25.30 4 2 10 25.30 17.00 4 2 10 19.60 21.60 -5 -2 -10 -21.20 16.50 -5 -2 -10 14.90 18.20 -5 -2 -10 -3.40 16.80 -5 -2 -10 17.00 16.90 -5 -2 -10 16.80 23.00 5 2 10 -16.50 21.20 5 2 10 -14.30 22.80 5 2 10 8.50 16.40 -6 -2 -10 56.39 24.10 -6 -2 -10 61.59 23.70 -6 -2 -10 19.70 25.40 -6 -2 -10 48.00 22.40 6 2 10 -24.60 21.50 6 2 10 -10.50 13.20 -1 -3 -10 81.89 28.60 -1 -3 -10 56.49 23.50 -1 -3 -10 28.10 18.30 -1 -3 -10 9.10 32.70 -1 -3 -10 40.00 26.10 1 3 10 124.79 39.10 1 3 10 61.29 24.30 -2 -3 -10 -11.00 20.70 -2 -3 -10 -0.30 18.40 -2 -3 -10 5.10 18.70 -2 -3 -10 -2.90 13.60 2 3 10 -21.00 25.60 2 3 10 -3.70 16.30 -3 -3 -10 17.60 18.50 -3 -3 -10 25.00 21.40 -3 -3 -10 32.10 18.30 -3 -3 -10 44.20 27.90 -3 -3 -10 30.30 20.20 3 3 10 28.00 25.50 3 3 10 17.10 23.70 3 3 10 29.00 16.00 -4 -3 -10 81.29 29.90 -4 -3 -10 129.39 29.30 -4 -3 -10 155.58 33.00 -4 -3 -10 94.09 26.10 -4 -3 -10 92.99 26.30 4 3 10 170.68 37.90 4 3 10 91.19 25.50 4 3 10 87.29 20.70 -5 -3 -10 132.69 30.10 -5 -3 -10 157.28 32.20 -5 -3 -10 142.59 31.10 -5 -3 -10 130.09 32.70 -5 -3 -10 185.88 38.90 5 3 10 118.29 21.10 -6 -3 -10 -41.20 21.50 -6 -3 -10 -1.60 17.40 -6 -3 -10 -37.70 17.80 -6 -3 -10 -2.30 16.40 -6 -3 -10 -2.90 16.60 6 3 10 -4.30 22.50 -1 -4 -10 11.80 22.60 -1 -4 -10 -28.80 20.50 -1 -4 -10 -8.00 14.80 -1 -4 -10 13.00 20.40 -1 -4 -10 16.20 23.40 1 4 10 21.00 23.80 1 4 10 -15.40 28.00 1 4 10 -22.60 26.80 -2 -4 -10 -3.60 19.00 -2 -4 -10 6.00 19.40 -2 -4 -10 -11.10 15.70 -2 -4 -10 -14.40 17.80 -2 -4 -10 13.50 18.90 2 4 10 -17.50 17.90 2 4 10 -25.00 16.60 2 4 10 -2.90 21.20 -3 -4 -10 13.40 16.60 -3 -4 -10 23.80 19.80 -3 -4 -10 1.50 23.10 -3 -4 -10 -9.00 16.10 -3 -4 -10 -13.00 15.60 3 4 10 -8.10 15.70 3 4 10 -32.10 20.00 3 4 10 1.20 22.20 -4 -4 -10 98.19 26.00 -4 -4 -10 101.79 27.90 -4 -4 -10 78.29 23.30 -4 -4 -10 88.29 24.40 4 4 10 78.99 19.70 4 4 10 52.69 17.40 -5 -4 -10 145.69 28.90 -5 -4 -10 86.69 27.00 -5 -4 -10 134.19 27.20 -5 -4 -10 88.29 27.00 -5 -4 -10 73.19 24.10 -5 -4 -10 116.39 28.00 5 4 10 106.99 29.10 -6 -4 -10 -6.60 15.40 -6 -4 -10 -24.40 19.90 -6 -4 -10 -27.80 15.80 -6 -4 -10 19.00 17.20 -6 -4 -10 1.20 12.90 -6 -4 -10 4.50 21.80 6 4 10 -26.90 20.40 -1 -5 -10 17.00 24.20 -1 -5 -10 73.39 35.00 -1 -5 -10 54.49 22.50 -1 -5 -10 36.30 24.60 -1 -5 -10 35.40 27.10 1 5 10 13.00 24.90 1 5 10 51.19 25.80 -2 -5 -10 4.30 13.70 -2 -5 -10 -7.40 13.30 -2 -5 -10 -45.90 18.80 -2 -5 -10 -33.80 24.00 -2 -5 -10 14.40 21.80 2 5 10 -35.00 21.80 2 5 10 6.00 17.50 2 5 10 -26.80 24.00 -3 -5 -10 42.40 19.90 -3 -5 -10 30.00 17.90 -3 -5 -10 58.99 22.90 -3 -5 -10 37.30 20.80 -3 -5 -10 17.70 21.50 3 5 10 28.50 25.70 3 5 10 7.00 21.30 3 5 10 5.90 15.60 -4 -5 -10 245.98 40.00 -4 -5 -10 157.58 35.10 -4 -5 -10 257.57 42.50 -4 -5 -10 220.18 45.50 -4 -5 -10 289.77 46.10 -4 -5 -10 227.68 40.00 -5 -5 -10 111.59 24.90 -5 -5 -10 74.79 23.90 -5 -5 -10 77.79 26.50 -5 -5 -10 151.18 34.20 -5 -5 -10 74.59 23.00 -5 -5 -10 160.18 29.90 5 5 10 82.59 28.80 -6 -5 -10 170.08 30.60 -6 -5 -10 164.78 34.60 -6 -5 -10 175.78 33.60 -6 -5 -10 183.38 32.40 -6 -5 -10 168.58 29.30 -6 -5 -10 185.68 41.00 -2 -6 -10 31.10 19.20 -2 -6 -10 27.10 20.60 -2 -6 -10 18.80 19.10 -2 -6 -10 16.10 19.00 -2 -6 -10 -6.50 25.00 2 6 10 -27.30 22.30 2 6 10 -21.20 18.90 2 6 10 -22.30 25.70 -3 -6 -10 123.79 31.30 -3 -6 -10 165.48 35.50 -3 -6 -10 116.39 28.10 -3 -6 -10 85.09 26.90 -3 -6 -10 113.29 29.50 -4 -6 -10 64.19 23.50 -4 -6 -10 106.99 26.30 -4 -6 -10 113.69 27.80 -4 -6 -10 146.09 32.60 -4 -6 -10 140.99 32.70 -4 -6 -10 94.09 27.00 -5 -6 -10 151.48 31.50 -5 -6 -10 252.17 33.60 -5 -6 -10 202.28 34.00 -5 -6 -10 157.98 29.90 -5 -6 -10 238.58 42.00 -5 -6 -10 206.28 39.60 5 6 10 145.59 32.70 -3 -7 -10 75.49 26.70 -3 -7 -10 1.20 19.20 -3 -7 -10 53.49 24.70 -3 -7 -10 6.90 26.30 3 7 10 -23.70 29.40 -4 -7 -10 312.97 42.40 -4 -7 -10 361.46 46.70 -4 -7 -10 297.97 49.10 -4 -7 -10 265.67 49.60 -4 -7 -10 277.37 46.80 4 7 10 272.67 51.39 -5 -7 -10 7.70 20.90 -5 -7 -10 10.80 16.30 -5 -7 -10 -16.50 16.10 -5 -7 -10 -2.90 21.80 -5 -7 -10 -9.90 16.90 5 7 10 -7.10 22.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 88100 _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 1.000000 0.000000 1.000000 0.02048(18) Uani 1 2 d S . P . . Cl2 Cl 0.99660(8) -0.07068(6) 0.76927(7) 0.02547(17) Uani 1 1 d . . . . . O1 O 0.4206(2) 0.49113(17) 0.90470(16) 0.0183(3) Uani 1 1 d . . . . . N1 N 0.5614(2) 0.49994(19) 0.73686(19) 0.0141(3) Uani 1 1 d . . . . . C2 C 0.7704(3) 0.6598(2) 0.4497(2) 0.0153(4) Uani 1 1 d . . . . . H2 H 0.823982 0.764401 0.367655 0.018 Uiso 1 1 calc R U . . . C4 C 0.7502(3) 0.3671(2) 0.5190(2) 0.0152(4) Uani 1 1 d . . . . . H4 H 0.789081 0.268599 0.484729 0.018 Uiso 1 1 calc R U . . . C5 C 0.6151(3) 0.3573(2) 0.6917(2) 0.0154(4) Uani 1 1 d . . . . . C1 C 0.6346(3) 0.6515(2) 0.6216(2) 0.0150(4) Uani 1 1 d . . . . . C3 C 0.8305(3) 0.5184(2) 0.3943(2) 0.0154(4) Uani 1 1 d . . . . . C6 C 0.5652(3) 0.7989(2) 0.6882(3) 0.0203(4) Uani 1 1 d . . . . . H6A H 0.416071 0.812308 0.732713 0.030 Uiso 1 1 calc R U . . . H6B H 0.622945 0.900129 0.589728 0.030 Uiso 1 1 calc R U . . . H6C H 0.611106 0.781105 0.785809 0.030 Uiso 1 1 calc R U . . . C8 C 0.5282(3) 0.1983(2) 0.8316(3) 0.0202(4) Uani 1 1 d . . . . . H8A H 0.581004 0.168064 0.927337 0.030 Uiso 1 1 calc R U . . . H8B H 0.567103 0.108625 0.777360 0.030 Uiso 1 1 calc R U . . . H8C H 0.379227 0.213593 0.882125 0.030 Uiso 1 1 calc R U . . . C7 C 0.9753(3) 0.5293(3) 0.2060(2) 0.0189(4) Uani 1 1 d . . . . . H7A H 0.898068 0.555789 0.128343 0.028 Uiso 1 1 calc R U . . . H7B H 1.052697 0.421643 0.205842 0.028 Uiso 1 1 calc R U . . . H7C H 1.069621 0.617503 0.161095 0.028 Uiso 1 1 calc R U . . . H1 H 0.500000 0.500000 1.000000 0.072(14) Uiso 1 2 d S . P . . 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 0.0184(3) 0.0162(3) 0.0225(4) -0.0047(3) -0.0036(3) -0.0038(2) Cl2 0.0247(3) 0.0234(3) 0.0272(3) -0.0094(2) -0.0058(2) -0.0051(2) O1 0.0148(7) 0.0282(8) 0.0091(6) -0.0071(6) 0.0005(5) -0.0040(5) N1 0.0128(8) 0.0194(8) 0.0092(7) -0.0042(6) -0.0029(6) -0.0024(6) C2 0.0163(9) 0.0171(9) 0.0130(9) -0.0023(7) -0.0069(7) -0.0034(7) C4 0.0157(9) 0.0171(9) 0.0156(9) -0.0067(7) -0.0071(7) -0.0009(7) C5 0.0151(9) 0.0171(9) 0.0158(9) -0.0043(7) -0.0074(7) -0.0025(7) C1 0.0134(9) 0.0171(9) 0.0158(9) -0.0042(7) -0.0076(7) -0.0011(7) C3 0.0137(9) 0.0218(10) 0.0130(9) -0.0062(7) -0.0067(7) -0.0009(7) C6 0.0233(10) 0.0183(10) 0.0200(10) -0.0087(8) -0.0071(8) -0.0002(8) C8 0.0224(10) 0.0177(10) 0.0166(10) -0.0034(8) -0.0038(8) -0.0046(8) C7 0.0176(10) 0.0245(10) 0.0124(9) -0.0072(8) -0.0025(8) -0.0013(8) 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 Cl2 Cl1 Cl2 180.00(2) 2_757 . ? N1 O1 H1 111.03(12) . . ? C5 N1 O1 117.87(15) . . ? C5 N1 C1 123.40(16) . . ? C1 N1 O1 118.68(15) . . ? C1 C2 H2 119.3 . . ? C1 C2 C3 121.43(17) . . ? C3 C2 H2 119.3 . . ? C5 C4 H4 119.3 . . ? C5 C4 C3 121.40(17) . . ? C3 C4 H4 119.3 . . ? N1 C5 C4 118.11(17) . . ? N1 C5 C8 118.24(16) . . ? C4 C5 C8 123.64(17) . . ? N1 C1 C2 118.07(17) . . ? N1 C1 C6 118.26(16) . . ? C2 C1 C6 123.67(17) . . ? C2 C3 C4 117.59(17) . . ? C2 C3 C7 121.06(17) . . ? C4 C3 C7 121.34(17) . . ? 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 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? C3 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 Cl1 Cl2 2.2959(6) 2_757 ? Cl1 Cl2 2.2959(6) . ? O1 N1 1.3658(19) . ? O1 H1 1.2114(13) . ? N1 C5 1.356(2) . ? N1 C1 1.361(2) . ? C2 H2 0.9500 . ? C2 C1 1.382(3) . ? C2 C3 1.392(3) . ? C4 H4 0.9500 . ? C4 C5 1.384(3) . ? C4 C3 1.393(3) . ? C5 C8 1.490(3) . ? C1 C6 1.492(3) . ? C3 C7 1.503(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? 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 O1 N1 C5 C4 176.92(15) . . . . ? O1 N1 C5 C8 -4.0(2) . . . . ? O1 N1 C1 C2 -177.29(15) . . . . ? O1 N1 C1 C6 3.2(2) . . . . ? C5 N1 C1 C2 0.1(3) . . . . ? C5 N1 C1 C6 -179.38(17) . . . . ? C5 C4 C3 C2 0.2(3) . . . . ? C5 C4 C3 C7 -179.26(17) . . . . ? C1 N1 C5 C4 -0.5(3) . . . . ? C1 N1 C5 C8 178.49(16) . . . . ? C1 C2 C3 C4 -0.6(3) . . . . ? C1 C2 C3 C7 178.85(17) . . . . ? C3 C2 C1 N1 0.4(3) . . . . ? C3 C2 C1 C6 179.94(17) . . . . ? C3 C4 C5 N1 0.4(3) . . . . ? C3 C4 C5 C8 -178.62(17) . . . . ?