#------------------------------------------------------------------------------ #$Date: 2024-10-22 01:10:36 +0300 (Tue, 22 Oct 2024) $ #$Revision: 295572 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/29/1572909.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_1572909 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 'Cl2, 0.5(C14 H18 N2 O2)' _chemical_formula_sum 'C7 H9 Cl2 N O' _chemical_formula_weight 194.05 _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_Hall '-P 2yb' _space_group_name_H-M_alt 'P 1 21/m 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 90 _cell_angle_beta 92.072(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.9789(7) _cell_length_b 7.1228(6) _cell_length_c 8.6438(9) _cell_measurement_reflns_used 4108 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 28.306 _cell_measurement_theta_min 2.358 _cell_volume 429.40(7) _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 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_unetI/netI 0.0227 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 7419 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.366 _diffrn_reflns_theta_min 2.358 _diffrn_source_current 0.0 _diffrn_source_power 0.0 _diffrn_source_voltage 0.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6394 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1047 before and 0.0622 after correction. The Ratio of minimum to maximum transmission is 0.8574. 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 1.501 _exptl_crystal_description plate _exptl_crystal_F_000 200 _exptl_crystal_size_max 0.378 _exptl_crystal_size_mid 0.102 _exptl_crystal_size_min 0.074 _refine_diff_density_max 0.547 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.092 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.261 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 64 _refine_ls_number_reflns 950 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.261 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0373 _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^)+1.0014P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.0887 _reflns_Friedel_coverage 0.000 _reflns_number_gt 795 _reflns_number_total 950 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06270a3.cif _cod_data_source_block OGH_D49_9 _cod_database_code 1572909 _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 0.950 _shelx_estimated_absorpt_t_min 0.779 _olex2_refinement_description ; 1. Others Fixed Sof: H7A(0.5) H7B(0.5) H7C(0.5) H6A(0.5) H6B(0.5) H6C(0.5) 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4), C3(H3) 2.b Idealised Me refined with everything fixed: C7(H7A,H7B,H7C), C6(H6A,H6B,H6C) ; _shelx_res_file ; TITL full1_P21m_a.res in P2(1)/m full1_p21m_a.res created by SHELXL-2019/1 at 14:14:12 on 21-Mar-2024 REM Old TITL full1_P21m in P2(1)/m REM SHELXT solution in P2(1)/m: R1 0.088, Rweak 0.000, Alpha 0.006 REM 0.535 for 3 systematic absences, Orientation as input REM Formula found by SHELXT: C7 Cl2 N O CELL 0.71073 6.9789 7.1228 8.6438 90 92.072 90 ZERR 2 0.0007 0.0006 0.0009 0 0.004 0 LATT 1 SYMM -X,0.5+Y,-Z SFAC C H Cl N O UNIT 14 18 4 2 2 L.S. 10 PLAN 1 SIZE 0.074 0.102 0.378 TEMP -173.15 CONF CONN 24 Cl1 CONN 24 O1 BOND LIST 4 MORE -1 BOND $H fmap 2 acta SHEL 9999 0.8 REM REM REM WGHT 0.000000 1.001400 FVAR 1.22118 CL1 3 0.102045 0.393993 0.199656 11.00000 0.01679 0.01541 = 0.02104 0.00061 0.00129 0.00131 O1 5 0.156172 0.750000 0.217435 10.50000 0.01150 0.01755 = 0.02387 0.00000 0.00081 0.00000 N1 4 0.340494 0.750000 0.256334 10.50000 0.01017 0.01148 = 0.02037 0.00000 -0.00051 0.00000 C1 1 0.471246 0.750000 0.141558 10.50000 0.01692 0.01256 = 0.02005 0.00000 0.00388 0.00000 C5 1 0.396698 0.750000 0.409432 10.50000 0.01764 0.01347 = 0.01766 0.00000 -0.00106 0.00000 C2 1 0.664316 0.750000 0.183098 10.50000 0.01513 0.01700 = 0.02465 0.00000 0.00591 0.00000 AFIX 43 H2 2 0.756318 0.750000 0.104737 10.50000 -1.20000 AFIX 0 C4 1 0.589536 0.750000 0.449381 10.50000 0.01947 0.02182 = 0.02067 0.00000 -0.00345 0.00000 AFIX 43 H4 2 0.629733 0.750000 0.555565 10.50000 -1.20000 AFIX 0 C3 1 0.725466 0.750000 0.336697 10.50000 0.01159 0.01984 = 0.03094 0.00000 -0.00329 0.00000 AFIX 43 H3 2 0.858391 0.750000 0.364580 10.50000 -1.20000 AFIX 0 C7 1 0.241033 0.750000 0.523248 10.50000 0.01926 0.02900 = 0.02176 0.00000 0.00186 0.00000 PART -1 AFIX 131 H7A 2 0.155646 0.857063 0.502751 10.50000 -1.50000 H7B 2 0.297538 0.759897 0.628382 10.50000 -1.50000 H7C 2 0.167653 0.633040 0.513382 10.50000 -1.50000 AFIX 0 PART 0 C6 1 0.392427 0.750000 -0.020774 10.50000 0.02214 0.02600 = 0.01701 0.00000 0.00409 0.00000 PART -1 AFIX 131 H6A 2 0.324260 0.631873 -0.041573 10.50000 -1.50000 H6B 2 0.497657 0.762646 -0.092110 10.50000 -1.50000 H6C 2 0.303472 0.855481 -0.035514 10.50000 -1.50000 AFIX 0 HKLF 4 REM full1_P21m_a.res in P2(1)/m REM wR2 = 0.0887, GooF = S = 1.261, Restrained GooF = 1.261 for all data REM R1 = 0.0373 for 795 Fo > 4sig(Fo) and 0.0512 for all 950 data REM 64 parameters refined using 0 restraints END WGHT 0.0000 1.0014 REM Highest difference peak 0.547, deepest hole -0.479, 1-sigma level 0.092 Q1 1 0.3017 0.8864 0.6001 11.00000 0.05 0.55 ; _shelx_res_checksum 87276 _shelx_hkl_file ; 1 0 0 89.79 4.80 1 0 0 71.89 5.10 -1 0 0 76.59 4.50 -2 0 0 13.50 2.70 2 0 0 13.30 2.70 2 0 0 8.00 2.50 -2 0 0 8.50 2.20 -3 0 0 118.79 9.20 3 0 0 128.99 10.10 -3 0 0 109.99 10.60 3 0 0 95.69 10.10 -4 0 0 2599.04 80.59 4 0 0 2635.34 80.49 -4 0 0 2707.33 74.29 -4 0 0 2610.84 79.69 4 0 0 2687.03 74.99 5 0 0 1034.30 41.10 -5 0 0 938.31 45.10 -5 0 0 1046.20 45.90 -5 0 0 1048.10 41.40 5 0 0 995.70 45.70 -6 0 0 427.96 23.60 6 0 0 398.76 29.80 -6 0 0 491.15 27.90 -6 0 0 398.46 29.60 6 0 0 420.86 26.40 -7 0 0 7.00 4.00 -7 0 0 1.40 3.00 -7 0 0 0.00 5.00 7 0 0 2.10 3.40 -8 0 0 175.68 17.50 -8 0 0 144.69 18.60 -8 0 0 179.28 24.70 8 0 0 112.09 18.40 -8 0 0 148.59 22.50 -9 0 0 115.69 22.60 -9 0 0 107.39 31.20 9 0 0 154.68 32.40 -9 0 0 122.39 15.90 -1 -1 0 10.00 2.50 1 -1 0 5.20 1.50 1 -1 0 7.90 1.00 1 -1 0 4.20 1.50 -1 1 0 5.50 1.40 -1 1 0 5.20 1.50 1 1 0 7.00 2.00 -1 1 0 6.00 0.90 2 -1 0 1205.78 34.10 -2 -1 0 1206.98 37.80 -2 -1 0 1221.28 35.40 2 -1 0 1202.58 36.50 2 1 0 1204.38 38.20 -2 1 0 1202.68 34.60 -2 1 0 1225.48 27.80 -2 1 0 1202.48 36.40 -3 -1 0 312.07 16.10 3 -1 0 308.07 15.90 3 -1 0 309.07 18.00 -3 -1 0 315.27 18.60 -3 1 0 294.47 17.80 -3 1 0 295.67 17.20 -3 1 0 296.77 15.50 3 1 0 291.87 18.30 4 -1 0 801.02 36.00 -4 -1 0 892.51 38.90 -4 -1 0 812.02 32.40 -4 -1 0 832.72 37.00 4 -1 0 832.72 32.00 -4 1 0 846.92 32.80 -4 1 0 830.12 36.00 -4 1 0 796.02 36.10 -5 -1 0 38.00 8.60 5 -1 0 36.50 7.00 -5 -1 0 44.80 8.00 -5 -1 0 28.30 7.30 5 -1 0 30.00 8.10 5 1 0 40.20 9.90 -5 1 0 30.40 7.80 -5 1 0 35.30 6.50 -5 1 0 37.90 8.80 6 -1 0 225.68 22.00 -6 -1 0 292.47 25.70 6 -1 0 258.07 20.20 -6 -1 0 287.17 24.70 -6 -1 0 232.58 19.10 -6 -1 0 241.58 19.00 -6 1 0 256.47 23.60 -6 1 0 234.18 21.80 -6 1 0 249.38 19.70 6 1 0 247.68 23.50 -6 1 0 229.58 14.50 -7 -1 0 271.27 31.60 7 -1 0 280.57 23.30 7 -1 0 297.37 26.60 -7 -1 0 287.97 22.10 -7 -1 0 252.97 25.60 -7 1 0 323.57 18.10 -7 1 0 279.47 26.40 7 1 0 305.37 30.30 8 -1 0 66.59 13.00 -8 -1 0 111.59 20.20 -8 -1 0 91.29 14.10 -8 -1 0 113.59 19.80 -8 1 0 106.59 11.70 8 1 0 72.09 14.20 -8 1 0 70.99 13.40 -8 1 0 114.99 9.80 -9 -1 0 143.29 26.20 -9 -1 0 105.19 31.60 9 -1 0 138.29 23.40 -9 1 0 121.89 28.80 -9 1 0 165.58 26.70 9 1 0 94.29 17.70 0 -2 0 9636.34 214.98 0 2 0 9999.00 216.48 1 -2 0 2666.63 62.59 1 -2 0 2732.33 61.19 -1 -2 0 2723.13 65.39 -1 -2 0 2686.03 64.99 1 -2 0 2667.03 65.99 -1 2 0 2657.53 60.39 -1 2 0 2576.54 66.69 1 2 0 2680.13 64.59 -2 -2 0 390.16 18.30 2 -2 0 350.86 15.60 -2 -2 0 366.66 18.10 2 -2 0 364.76 16.00 2 -2 0 376.06 10.10 -2 2 0 357.96 10.90 -2 2 0 371.46 15.60 2 2 0 362.66 17.80 -2 2 0 371.16 16.00 -2 2 0 372.86 16.90 -3 -2 0 109.99 11.20 -3 -2 0 103.59 9.60 3 -2 0 96.79 9.40 3 -2 0 106.39 9.10 -3 -2 0 107.19 10.90 -3 2 0 99.79 3.80 3 2 0 109.59 11.10 -3 2 0 102.39 9.40 -3 2 0 96.59 9.10 -3 2 0 102.19 9.90 4 -2 0 15.90 4.50 -4 -2 0 23.00 5.30 4 -2 0 33.30 6.30 -4 -2 0 19.80 5.20 -4 -2 0 27.60 7.00 -4 2 0 21.40 5.80 4 2 0 18.90 5.40 -4 2 0 25.70 6.20 -4 2 0 26.70 2.20 -4 2 0 17.50 4.90 5 -2 0 156.28 14.20 -5 -2 0 142.59 16.80 -5 -2 0 147.59 13.90 -5 -2 0 143.09 16.70 5 -2 0 143.49 15.40 -5 2 0 151.38 14.70 -5 2 0 149.59 7.50 -5 2 0 180.38 20.60 5 2 0 146.49 16.50 -5 2 0 153.08 6.70 -5 2 0 158.78 16.20 -6 -2 0 43.70 9.70 -6 -2 0 44.20 10.90 6 -2 0 40.90 9.90 6 -2 0 44.30 8.80 -6 -2 0 43.10 10.40 -6 2 0 37.10 7.60 -6 2 0 48.50 9.40 6 2 0 38.70 9.80 -6 2 0 38.40 4.00 -7 -2 0 -4.80 4.10 -7 -2 0 -2.00 5.20 -7 -2 0 2.30 6.10 7 -2 0 3.20 4.20 7 -2 0 4.20 4.10 -7 2 0 -1.30 4.60 -7 2 0 7.30 2.30 7 2 0 -0.30 3.80 -7 2 0 22.70 9.40 8 -2 0 0.10 5.20 -8 -2 0 -2.10 5.30 -8 -2 0 -2.00 4.10 -8 2 0 2.40 7.10 -8 2 0 -2.30 1.50 -8 2 0 -4.40 4.40 8 2 0 0.60 6.20 -9 -2 0 30.60 10.80 9 -2 0 19.60 9.60 -9 2 0 15.50 8.80 9 2 0 49.10 15.90 0 -3 0 0.00 0.50 0 -3 0 -0.40 0.90 0 -3 0 0.40 0.50 -1 -3 0 1933.01 55.69 1 -3 0 1837.32 52.89 1 -3 0 1835.62 42.90 1 -3 0 1813.42 49.90 -1 -3 0 1942.31 49.50 -1 -3 0 1850.21 61.49 -1 -3 0 2014.50 49.70 -1 3 0 1881.31 43.50 2 -3 0 1774.02 46.70 2 -3 0 1844.62 43.90 -2 -3 0 1788.52 52.39 -2 -3 0 1711.03 51.49 2 -3 0 1710.53 50.49 -2 3 0 1727.73 45.20 2 3 0 1774.02 51.59 -2 3 0 1748.13 52.89 -3 -3 0 2157.68 65.59 3 -3 0 2117.89 59.59 3 -3 0 2127.99 60.09 -3 -3 0 2135.49 64.59 -3 3 0 2046.10 62.39 3 3 0 1998.10 63.59 -3 3 0 2022.10 57.99 -3 3 0 2105.69 59.29 4 -3 0 33.00 6.00 -4 -3 0 47.50 9.30 4 -3 0 33.70 6.70 -4 -3 0 39.10 7.40 -4 -3 0 34.80 8.20 -4 3 0 41.20 7.50 -4 3 0 32.60 6.20 -4 3 0 34.50 6.50 4 3 0 50.29 9.70 -5 -3 0 44.60 8.30 -5 -3 0 38.50 9.20 -5 -3 0 57.89 11.30 -5 -3 0 32.10 8.10 5 -3 0 39.00 7.50 5 -3 0 32.40 7.00 5 3 0 43.10 9.80 -5 3 0 40.50 8.50 -5 3 0 35.90 6.10 -5 3 0 44.60 8.00 -6 -3 0 166.98 19.10 6 -3 0 175.28 20.60 6 -3 0 168.68 16.40 -6 -3 0 190.48 20.90 -6 -3 0 126.59 24.40 -6 -3 0 180.18 17.70 -6 3 0 208.18 20.00 6 3 0 218.88 21.80 -6 3 0 165.58 18.20 -6 3 0 146.29 17.30 7 -3 0 441.36 33.10 -7 -3 0 395.46 30.90 -7 -3 0 498.45 37.30 -7 -3 0 376.96 33.00 -7 -3 0 403.76 29.20 7 -3 0 451.45 29.60 -7 3 0 385.26 30.40 -7 3 0 439.76 32.40 7 3 0 486.65 36.40 -7 3 0 449.46 32.00 -8 -3 0 315.67 44.20 8 -3 0 313.37 28.30 -8 -3 0 340.67 35.00 -8 -3 0 343.27 35.80 -8 -3 0 327.47 30.20 8 -3 0 381.66 32.70 -8 3 0 373.56 33.00 -8 3 0 359.06 42.80 8 3 0 325.97 32.30 0 -4 0 397.66 21.20 -1 -4 0 2948.21 79.89 1 -4 0 2917.61 77.59 -1 -4 0 3002.10 85.39 -1 -4 0 3004.90 73.19 -2 -4 0 325.07 17.90 2 -4 0 330.47 12.90 2 -4 0 325.67 18.40 2 -4 0 356.86 15.40 -2 -4 0 358.26 23.50 -2 -4 0 333.17 18.00 -2 -4 0 326.47 21.90 2 4 0 336.27 17.20 -2 4 0 339.97 15.70 -2 4 0 326.77 20.00 -2 4 0 337.87 11.10 -2 4 0 354.76 11.50 3 -4 0 246.98 14.00 -3 -4 0 270.07 20.90 3 -4 0 274.57 17.10 -3 -4 0 267.27 18.40 3 -4 0 246.18 9.60 -3 -4 0 229.88 17.40 3 4 0 277.47 18.30 -3 4 0 258.27 18.40 -3 4 0 249.78 13.40 -4 -4 0 258.97 22.20 -4 -4 0 245.08 18.80 -4 -4 0 259.07 20.60 -4 -4 0 217.58 19.00 4 -4 0 221.08 15.80 4 -4 0 252.67 17.50 -4 4 0 244.68 15.90 -4 4 0 260.47 16.80 4 4 0 266.27 21.20 -4 4 0 273.97 20.60 -5 -4 0 938.91 45.60 5 -4 0 897.41 38.80 -5 -4 0 917.31 46.70 5 -4 0 905.41 39.90 -5 -4 0 933.01 41.90 -5 -4 0 920.01 45.50 -5 4 0 912.41 39.20 5 4 0 842.32 43.20 -5 4 0 941.91 43.50 -5 4 0 908.01 39.50 -6 -4 0 429.16 27.80 6 -4 0 398.96 27.40 6 -4 0 326.17 23.50 -6 -4 0 317.87 28.10 -6 -4 0 340.27 29.40 -6 -4 0 347.47 29.00 -6 4 0 369.66 27.40 -6 4 0 341.77 25.50 6 4 0 343.97 28.30 7 -4 0 27.20 8.20 -7 -4 0 28.70 9.70 -7 -4 0 30.00 10.30 7 -4 0 28.40 8.90 -7 -4 0 23.10 8.70 -7 -4 0 19.80 7.30 -7 4 0 8.10 12.10 7 4 0 34.20 10.00 -7 4 0 36.10 10.10 -8 -4 0 1.10 6.70 -8 -4 0 -11.00 9.00 8 -4 0 9.60 7.20 -8 -4 0 6.70 14.50 8 -4 0 -2.50 6.10 -8 -4 0 -5.80 8.40 -8 4 0 9.20 8.20 8 4 0 1.70 6.00 -8 4 0 -13.10 11.60 0 -5 0 4.80 2.70 0 -5 0 0.40 2.10 -1 -5 0 175.98 16.20 1 -5 0 137.39 13.10 1 -5 0 151.18 12.60 -1 -5 0 152.28 9.30 -1 -5 0 158.08 9.40 -1 -5 0 158.88 11.40 -2 -5 0 29.90 7.70 2 -5 0 41.20 7.40 -2 -5 0 36.70 6.50 -2 -5 0 26.40 7.30 -2 -5 0 27.70 5.60 3 -5 0 171.18 14.60 -3 -5 0 188.08 15.70 -3 -5 0 160.78 14.30 3 -5 0 183.38 10.80 -3 -5 0 143.89 18.80 3 -5 0 166.98 9.50 -3 -5 0 163.28 17.80 3 5 0 170.58 14.00 -3 5 0 176.48 12.90 -3 5 0 159.68 10.50 -3 5 0 172.98 16.70 -3 5 0 173.18 8.60 4 -5 0 24.00 5.20 -4 -5 0 26.30 9.60 -4 -5 0 20.60 6.70 -4 -5 0 24.30 7.10 -4 -5 0 21.50 7.20 4 -5 0 18.50 5.50 -4 -5 0 21.80 7.20 -4 5 0 18.60 4.80 -4 5 0 13.50 3.90 4 5 0 26.30 7.30 -4 5 0 16.20 6.40 -4 5 0 20.10 5.70 -5 -5 0 10.70 8.60 -5 -5 0 10.60 6.30 5 -5 0 10.40 4.60 -5 -5 0 11.90 5.50 5 -5 0 10.70 4.20 -5 -5 0 11.10 5.20 -5 -5 0 5.80 4.50 -5 5 0 1.20 5.60 -5 5 0 10.00 4.30 5 5 0 10.30 5.70 -5 5 0 7.30 3.80 -5 5 0 1.00 6.40 -6 -5 0 -0.20 4.10 -6 -5 0 -4.60 4.30 6 -5 0 -2.60 3.50 6 -5 0 -1.20 3.20 -6 -5 0 -1.40 2.90 -6 -5 0 -6.60 3.60 -6 -5 0 -12.30 7.60 -6 5 0 3.50 8.50 -6 5 0 -4.30 3.40 -7 -5 0 7.40 8.80 -7 -5 0 -2.50 5.80 -7 -5 0 9.30 5.10 7 -5 0 2.80 3.90 -7 -5 0 -2.90 12.10 7 -5 0 -2.20 5.70 -7 5 0 -3.50 5.30 7 5 0 7.50 5.30 -7 5 0 -6.60 4.90 -7 5 0 -4.20 8.30 0 -6 0 3149.68 95.09 0 -6 0 3241.08 95.89 -1 -6 0 10.50 5.70 1 -6 0 3.90 3.10 1 -6 0 2.40 4.10 -1 -6 0 7.90 2.30 -1 -6 0 7.60 2.20 -2 -6 0 -1.80 3.20 2 -6 0 -0.80 1.80 -2 -6 0 -2.80 1.30 -2 -6 0 0.90 2.00 -2 -6 0 -1.00 3.10 2 -6 0 4.70 3.50 -3 -6 0 11.70 6.20 -3 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40.40 4 0 -10 443.26 30.60 3 0 -10 31.40 7.80 3 0 -10 46.40 13.80 2 0 -10 18.60 6.30 -2 0 10 45.70 22.80 2 0 -10 17.10 8.80 -2 0 10 27.40 13.40 -1 0 10 590.54 42.00 1 0 -10 497.25 29.10 1 0 -10 515.85 40.10 -1 0 10 530.45 54.99 0 0 -10 307.97 21.80 0 0 10 307.07 41.10 0 0 10 228.98 24.00 0 0 -10 281.07 30.10 -1 0 -10 303.97 22.60 -1 0 -10 266.47 23.20 1 0 10 254.07 24.80 -1 0 -10 294.57 31.30 1 0 10 265.17 29.40 2 0 10 -10.20 7.30 -2 0 -10 -6.50 5.20 2 0 10 -10.90 13.90 -2 0 -10 9.80 8.90 2 0 10 -13.80 5.20 -3 0 -10 8.90 9.20 3 0 10 -23.20 17.50 3 0 10 7.60 9.00 -3 0 -10 30.80 9.90 -4 0 -10 147.69 17.40 -4 0 -10 160.18 19.40 -4 0 -10 133.49 18.30 -4 0 -10 100.29 19.00 4 0 10 151.08 32.10 4 -1 -10 153.78 21.50 4 -1 -10 214.28 29.10 4 1 -10 203.88 28.70 4 1 -10 225.88 22.00 -3 -1 10 -11.80 7.00 3 -1 -10 -10.60 6.30 3 -1 -10 3.10 5.30 3 1 -10 -1.30 4.90 3 1 -10 3.50 7.90 -3 1 10 0.40 15.30 2 -1 -10 50.69 10.40 -2 -1 10 92.79 18.40 2 -1 -10 63.79 16.40 -2 1 10 79.49 28.00 2 1 -10 70.59 10.40 2 1 -10 39.10 12.00 1 -1 -10 43.10 10.00 -1 -1 10 40.40 16.90 1 -1 -10 36.30 10.60 1 -1 -10 58.69 14.70 1 1 -10 28.80 14.40 -1 1 10 38.70 17.60 1 1 -10 32.20 7.20 -1 1 10 27.30 11.60 0 -1 10 8.10 7.20 0 -1 -10 12.90 6.30 0 -1 -10 -3.30 5.90 0 1 10 1.70 9.10 0 1 10 22.90 14.40 0 1 -10 -2.80 4.50 0 1 -10 4.60 3.50 -1 -1 -10 10.40 4.90 1 -1 10 -14.40 5.90 -1 -1 -10 -13.20 5.20 -1 -1 -10 -3.30 5.30 1 -1 10 14.30 14.00 -1 1 -10 -2.70 3.30 1 1 10 -18.60 12.20 -1 1 -10 -3.10 7.30 2 -1 10 107.59 25.20 2 -1 10 154.98 19.90 -2 -1 -10 153.78 19.10 -2 -1 -10 160.78 19.80 2 -1 10 109.29 17.70 -2 1 -10 152.18 24.10 2 1 10 155.18 28.60 -2 1 -10 154.88 14.30 3 -1 10 168.48 20.20 -3 -1 -10 200.48 23.00 3 -1 10 201.08 28.50 -3 -1 -10 205.68 21.10 -3 1 -10 184.08 14.40 3 1 10 117.69 30.80 -3 1 -10 188.48 26.90 -3 1 -10 199.38 17.40 -4 -1 -10 -0.40 8.10 -4 -1 -10 16.90 8.70 4 -1 10 4.60 9.30 -4 -1 -10 2.00 9.30 4 -1 10 27.50 23.30 -4 1 -10 1.40 5.20 -4 1 -10 2.60 10.80 -4 1 -10 11.20 7.00 4 1 10 -0.40 22.30 4 -2 -10 -8.00 5.60 4 -2 -10 4.20 8.00 4 2 -10 -4.70 6.80 3 -2 -10 -9.60 5.30 3 -2 -10 -13.40 6.70 -3 -2 10 6.60 7.80 -3 2 10 -7.70 16.20 3 2 -10 -2.90 4.40 3 2 -10 -9.60 6.10 2 -2 -10 -8.00 4.90 2 -2 -10 -5.40 5.30 2 -2 -10 -14.40 5.70 -2 -2 10 -25.90 13.60 2 2 -10 -12.20 5.00 2 2 -10 -8.30 3.60 1 -2 -10 -2.50 6.00 1 -2 -10 -2.60 5.70 -1 -2 10 -25.50 10.50 1 -2 -10 0.90 6.00 -1 2 10 4.40 13.40 1 2 -10 -4.70 6.00 1 2 -10 0.80 3.90 0 -2 -10 35.90 9.20 0 -2 -10 36.60 9.30 0 -2 -10 21.70 11.00 0 -2 10 27.40 16.70 0 -2 10 21.00 9.30 0 -2 10 28.90 8.60 0 2 -10 18.10 7.60 0 2 -10 30.30 4.60 0 2 10 25.40 18.40 -1 -2 -10 0.00 3.50 -1 -2 -10 -9.10 6.40 1 -2 10 -17.00 11.70 -1 -2 -10 12.00 8.40 1 -2 10 -9.50 8.70 1 -2 10 -7.10 5.70 -1 2 -10 -5.70 8.20 -1 2 -10 -3.70 2.00 1 2 10 4.20 16.20 2 -2 10 3.50 14.70 2 -2 10 1.20 6.40 -2 -2 -10 12.50 9.80 -2 -2 -10 -5.90 7.20 -2 -2 -10 0.40 7.00 2 -2 10 3.10 9.10 -2 2 -10 1.20 8.30 2 2 10 13.80 20.30 3 -2 10 -19.70 8.90 -3 -2 -10 -5.70 6.00 -3 -2 -10 -3.40 8.20 3 2 10 -37.30 16.40 -3 2 -10 -10.20 7.30 3 -3 -10 555.54 39.40 3 -3 -10 449.86 42.30 -3 -3 10 421.76 39.20 3 3 -10 469.25 43.80 3 3 -10 521.05 26.10 2 -3 -10 292.17 29.10 2 -3 -10 274.07 31.70 2 -3 -10 302.67 26.10 -2 -3 10 361.26 46.60 -2 -3 10 341.27 32.20 2 3 -10 356.06 34.50 1 -3 -10 35.60 10.50 1 -3 -10 58.39 13.60 -1 -3 10 56.49 15.70 1 -3 -10 61.69 12.50 -1 -3 10 73.99 20.10 -1 3 10 99.59 30.60 1 3 -10 54.29 12.00 0 -3 -10 6.10 6.30 0 -3 -10 2.40 7.10 0 -3 10 -9.80 7.80 0 3 -10 4.10 7.10 0 3 10 -17.30 13.00 1 -3 10 146.79 22.90 -1 -3 -10 177.28 24.50 1 -3 10 131.19 29.00 1 -3 10 152.58 20.10 -1 -3 -10 150.08 19.50 -1 3 -10 119.79 21.80 1 3 10 102.69 27.30 2 -3 10 177.08 24.80 -2 -3 -10 171.18 20.90 2 -3 10 151.08 20.30 -2 -3 -10 160.88 26.10 -2 -3 -10 112.79 18.50 -2 3 -10 191.98 27.00 3 -3 10 64.49 21.40 3 -3 10 54.79 15.40 -3 -3 -10 96.89 20.90 3 -3 10 45.60 11.60 -3 -3 -10 72.29 13.50 -3 3 -10 28.30 15.40 -2 -4 10 -13.70 7.50 2 -4 -10 -10.40 7.80 -2 -4 10 -28.50 15.40 2 -4 -10 -15.20 6.50 2 -4 -10 -1.30 6.70 -2 4 10 -12.00 18.30 2 4 -10 -12.90 9.00 1 -4 -10 8.50 12.20 -1 -4 10 12.10 14.90 1 -4 -10 22.50 10.60 1 -4 -10 17.20 8.20 -1 -4 10 4.80 10.20 1 4 -10 21.50 12.10 0 -4 10 270.67 29.30 0 -4 -10 320.47 31.60 0 -4 -10 332.07 38.80 0 -4 -10 316.57 31.80 0 4 -10 346.47 31.30 1 -4 10 85.19 25.60 -1 -4 -10 141.49 23.50 1 -4 10 74.99 14.60 -1 -4 -10 114.59 18.60 -1 -4 -10 144.49 19.60 -1 4 -10 111.69 21.70 2 -4 10 3.00 7.90 -2 -4 -10 10.50 11.00 -2 -4 -10 8.50 11.10 2 -4 10 7.70 12.00 2 -4 10 9.50 19.70 -2 4 -10 40.20 14.50 2 4 10 -35.70 19.50 -3 0 11 353.16 50.09 3 0 -11 310.27 26.00 2 0 -11 388.46 27.30 2 0 -11 451.25 42.50 1 0 -11 85.69 12.90 1 0 -11 71.59 16.20 0 0 -11 36.10 11.00 -1 0 -11 -1.40 5.40 1 0 11 10.00 18.30 -2 0 -11 283.57 34.50 -2 0 -11 313.87 26.40 -2 0 -11 383.16 25.90 2 0 11 218.58 40.40 -2 -1 11 5.60 19.10 2 -1 -11 -4.70 6.30 2 -1 -11 -2.10 8.30 2 1 -11 -1.50 9.60 -2 1 11 -38.20 18.70 1 -1 -11 -11.90 7.30 1 -1 -11 -10.50 6.50 -1 -1 11 7.10 18.30 1 1 -11 -4.10 7.60 -1 1 11 -5.00 16.90 1 1 -11 -2.10 5.20 0 -1 -11 304.27 34.70 0 -1 11 227.28 38.80 0 -1 -11 299.27 25.70 0 1 -11 305.17 33.70 0 1 -11 288.27 19.40 -1 -1 -11 35.60 13.40 -1 -1 -11 69.79 18.10 1 -1 11 72.69 27.10 -1 1 -11 70.19 19.60 -1 1 -11 36.00 7.50 1 1 11 35.10 24.30 -2 -1 -11 -18.20 7.10 -2 -1 -11 -6.70 8.00 2 -1 11 -19.10 20.60 -2 1 -11 -5.80 4.30 -2 1 -11 -10.00 7.50 2 -2 -11 -4.90 10.60 -2 -2 11 -29.00 19.00 2 2 -11 -3.00 4.80 -2 2 11 -46.80 18.50 2 2 -11 -5.00 8.20 1 -2 -11 20.60 9.20 1 -2 -11 -5.00 8.80 -1 -2 11 21.90 13.20 -1 -2 11 -8.60 19.90 1 -2 -11 -4.50 6.10 1 2 -11 24.80 12.40 -1 2 11 5.10 20.30 0 -2 -11 -0.10 6.70 0 -2 -11 -6.70 8.90 0 -2 -11 24.50 20.30 0 -2 11 -6.00 18.10 0 2 11 -7.40 19.50 0 2 -11 0.00 10.20 -1 -2 -11 -1.80 6.50 -1 -2 -11 -6.40 7.30 1 -2 11 15.50 19.00 1 -2 11 -18.90 10.30 -1 -2 -11 -6.80 9.10 1 2 11 -13.80 20.20 -1 2 -11 -24.90 9.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 64670 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, 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 0.10204(8) 0.39399(9) 0.19966(7) 0.01773(19) Uani 1 1 d . . . . . O1 O 0.1562(3) 0.750000 0.2174(3) 0.0176(6) Uani 1 2 d S T P . . N1 N 0.3405(4) 0.750000 0.2563(3) 0.0140(6) Uani 1 2 d S T P . . C1 C 0.4712(5) 0.750000 0.1416(4) 0.0164(7) Uani 1 2 d S T P . . C5 C 0.3967(5) 0.750000 0.4094(4) 0.0163(7) Uani 1 2 d S T P . . C2 C 0.6643(5) 0.750000 0.1831(4) 0.0188(8) Uani 1 2 d S T P . . H2 H 0.756318 0.750000 0.104737 0.023 Uiso 1 2 calc R U P . . C4 C 0.5895(5) 0.750000 0.4494(4) 0.0208(8) Uani 1 2 d S T P . . H4 H 0.629733 0.750000 0.555565 0.025 Uiso 1 2 calc R U P . . C3 C 0.7255(5) 0.750000 0.3367(5) 0.0209(8) Uani 1 2 d S T P . . H3 H 0.858391 0.750000 0.364580 0.025 Uiso 1 2 calc R U P . . C7 C 0.2410(6) 0.750000 0.5232(4) 0.0233(8) Uani 1 2 d S T P . . H7A H 0.155646 0.857063 0.502751 0.035 Uiso 0.5 1 calc . U P A -1 H7B H 0.297538 0.759897 0.628382 0.035 Uiso 0.5 1 calc . U P B -1 H7C H 0.167653 0.633040 0.513382 0.035 Uiso 0.5 1 calc . U P C -1 C6 C 0.3924(5) 0.750000 -0.0208(4) 0.0216(8) Uani 1 2 d S T P . . H6A H 0.324260 0.631873 -0.041573 0.032 Uiso 0.5 1 calc . U P D -1 H6B H 0.497657 0.762646 -0.092110 0.032 Uiso 0.5 1 calc . U P E -1 H6C H 0.303472 0.855481 -0.035514 0.032 Uiso 0.5 1 calc . U P F -1 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 0.0168(3) 0.0154(3) 0.0210(3) 0.0006(2) 0.0013(2) 0.0013(2) O1 0.0115(12) 0.0175(13) 0.0239(14) 0.000 0.0008(10) 0.000 N1 0.0102(14) 0.0115(14) 0.0204(15) 0.000 -0.0005(11) 0.000 C1 0.0169(17) 0.0126(17) 0.0200(18) 0.000 0.0039(14) 0.000 C5 0.0176(17) 0.0135(17) 0.0177(17) 0.000 -0.0011(14) 0.000 C2 0.0151(17) 0.0170(18) 0.0246(19) 0.000 0.0059(14) 0.000 C4 0.0195(19) 0.022(2) 0.0207(19) 0.000 -0.0034(15) 0.000 C3 0.0116(17) 0.0198(19) 0.031(2) 0.000 -0.0033(15) 0.000 C7 0.0193(19) 0.029(2) 0.0218(19) 0.000 0.0019(15) 0.000 C6 0.0221(19) 0.026(2) 0.0170(18) 0.000 0.0041(15) 0.000 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 O1 N1 C1 119.0(3) . . ? O1 N1 C5 119.4(3) . . ? C5 N1 C1 121.7(3) . . ? N1 C1 C2 118.7(3) . . ? N1 C1 C6 116.7(3) . . ? C2 C1 C6 124.7(3) . . ? N1 C5 C4 119.1(3) . . ? N1 C5 C7 116.6(3) . . ? C4 C5 C7 124.3(3) . . ? C1 C2 H2 119.5 . . ? C3 C2 C1 121.0(3) . . ? C3 C2 H2 119.5 . . ? C5 C4 H4 119.6 . . ? C5 C4 C3 120.8(3) . . ? C3 C4 H4 119.6 . . ? C2 C3 C4 118.8(3) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 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 . . ? 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 Cl1 2.0513(13) 4_565 ? O1 N1 1.318(4) . ? N1 C1 1.372(5) . ? N1 C5 1.367(5) . ? C1 C2 1.382(5) . ? C1 C6 1.488(5) . ? C5 C4 1.377(5) . ? C5 C7 1.492(5) . ? C2 H2 0.9500 . ? C2 C3 1.380(5) . ? C4 H4 0.9500 . ? C4 C3 1.384(5) . ? C3 H3 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 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 C1 C2 180.000(0) . . . . ? O1 N1 C1 C6 0.000(0) . . . . ? O1 N1 C5 C4 180.000(0) . . . . ? O1 N1 C5 C7 0.000(1) . . . . ? N1 C1 C2 C3 0.000(0) . . . . ? N1 C5 C4 C3 0.000(1) . . . . ? C1 N1 C5 C4 0.000(1) . . . . ? C1 N1 C5 C7 180.000(0) . . . . ? C1 C2 C3 C4 0.000(1) . . . . ? C5 N1 C1 C2 0.000(0) . . . . ? C5 N1 C1 C6 180.000(0) . . . . ? C5 C4 C3 C2 0.000(1) . . . . ? C7 C5 C4 C3 180.000(1) . . . . ? C6 C1 C2 C3 180.000(0) . . . . ?