#------------------------------------------------------------------------------ #$Date: 2024-10-22 01:10:36 +0300 (Tue, 22 Oct 2024) $ #$Revision: 295572 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/29/1572907.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_1572907 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 O' _chemical_formula_sum 'C7 H10 Cl N O' _chemical_formula_weight 159.61 _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 _atom_sites_solution_primary iterative _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 94.855(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.2444(3) _cell_length_b 9.2125(4) _cell_length_c 6.7656(3) _cell_measurement_reflns_used 5662 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 28.284 _cell_measurement_theta_min 3.022 _cell_volume 387.81(3) _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 'olex2.refine 1.5-alpha (Bourhis et al., 2015)' _computing_structure_solution 'olex2.solve 1.5-alpha (Bourhis et al., 2015)' _diffrn_ambient_temperature 100.00 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _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 0.0434 _diffrn_reflns_av_unetI/netI 0.0189 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 8522 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.352 _diffrn_reflns_theta_min 3.022 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.421 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6757 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1230 before and 0.0623 after correction. The Ratio of minimum to maximum transmission is 0.9061. 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 1.367 _exptl_crystal_description plate _exptl_crystal_F_000 168 _exptl_crystal_size_max 0.472 _exptl_crystal_size_mid 0.142 _exptl_crystal_size_min 0.074 _refine_diff_density_max 0.249 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.047 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 54 _refine_ls_number_reflns 843 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.116 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0253 _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^)+(0.0254P)^2^+0.2349P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.0682 _reflns_Friedel_coverage 0.000 _reflns_number_gt 769 _reflns_number_total 843 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06270a3.cif _cod_data_source_block ogh_d49_9or7 _cod_database_code 1572907 _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 0.969 _shelx_estimated_absorpt_t_min 0.826 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Others Fixed Sof: H1(0.5) 3.a Aromatic/amide H refined with riding coordinates: C3(H3), C2(H2) 3.b Idealised Me refined as rotating group: C4(H4A,H4B,H4C) 3.c Idealised tetrahedral OH refined as rotating group: O1(H1) ; _shelx_res_file ; TITL full1_P21_a.res in P2(1)/m ogh_d49_9or7.res created by SHELXL-2019/1 at 11:09:03 on 11-Sep-2024 REM Old TITL full1_P21 in P2(1) REM SHELXT solution in P2(1)/m: R1 0.074, Rweak 0.003, Alpha 0.014 REM 0.597 for 6 systematic absences, Orientation as input REM Formula found by SHELXT: C7 Cl N O CELL 0.71073 6.2444 9.2125 6.7656 90 94.855 90 ZERR 2 0.0003 0.0004 0.0003 0 0.002 0 LATT 1 SYMM -X,0.5+Y,-Z SFAC C H Cl N O UNIT 14 20 2 2 2 L.S. 10 PLAN 1 SIZE 0.074 0.142 0.472 TEMP -173.15 CONF BOND LIST 4 MORE -1 BOND $H fmap 2 acta SHEL 9999 0.8 OMIT -8 0 3 REM REM REM WGHT 0.025400 0.234900 FVAR 2.32816 CL1 3 0.204127 0.250000 0.188744 10.50000 0.01747 0.01901 = 0.01533 0.00000 0.00038 0.00000 O1 5 0.092625 0.250000 0.594957 10.50000 0.01153 0.03016 = 0.01431 0.00000 -0.00251 0.00000 PART -1 AFIX 147 H1 2 0.096939 0.237471 0.472379 10.50000 -1.50000 AFIX 0 PART 0 N1 4 0.299081 0.250000 0.685929 10.50000 0.01106 0.02098 = 0.01193 0.00000 0.00037 0.00000 C3 1 0.700581 0.250000 0.870200 10.50000 0.01467 0.02649 = 0.01252 0.00000 0.00180 0.00000 AFIX 43 H3 2 0.842000 0.249999 0.934183 10.50000 -1.20000 AFIX 0 C2 1 0.597374 0.379987 0.823503 11.00000 0.01709 0.02057 = 0.01402 -0.00062 0.00161 -0.00344 AFIX 43 H2 2 0.667940 0.469239 0.856130 11.00000 -1.20000 AFIX 0 C1 1 0.391323 0.380475 0.729260 11.00000 0.01757 0.01998 = 0.01203 0.00009 0.00302 0.00019 C4 1 0.267802 0.515001 0.674389 11.00000 0.02378 0.02111 = 0.02055 0.00142 -0.00029 0.00340 AFIX 137 H4A 2 0.224404 0.514212 0.531760 11.00000 -1.50000 H4B 2 0.358147 0.600099 0.706967 11.00000 -1.50000 H4C 2 0.139616 0.519169 0.748353 11.00000 -1.50000 AFIX 0 HKLF 4 REM full1_P21_a.res in P2(1)/m REM wR2 = 0.0682, GooF = S = 1.116, Restrained GooF = 1.116 for all data REM R1 = 0.0253 for 769 Fo > 4sig(Fo) and 0.0312 for all 843 data REM 54 parameters refined using 0 restraints END WGHT 0.0254 0.2349 REM Highest difference peak 0.249, deepest hole -0.305, 1-sigma level 0.047 Q1 1 0.4940 0.3763 0.7744 11.00000 0.05 0.25 ; _shelx_res_checksum 33308 _shelx_hkl_file ; -1 0 0 2237.78 63.89 1 0 0 2170.58 61.89 1 0 0 2102.79 61.99 1 0 0 2265.17 62.09 1 0 0 2247.18 63.99 -1 0 0 2124.79 61.29 -1 0 0 2164.58 61.99 -1 0 0 2045.40 61.59 -2 0 0 9755.52 272.47 3 0 0 192.78 17.10 3 0 0 190.88 17.30 -3 0 0 190.38 16.80 -3 0 0 194.08 17.40 3 0 0 194.88 19.00 -3 0 0 216.68 17.50 3 0 0 172.28 15.90 4 0 0 148.49 16.50 4 0 0 107.79 16.80 4 0 0 118.59 18.10 4 0 0 127.09 21.00 -4 0 0 131.49 16.10 -4 0 0 120.79 15.20 -4 0 0 148.19 17.10 5 0 0 515.75 35.40 -5 0 0 511.45 36.90 5 0 0 512.75 37.70 -5 0 0 534.25 35.50 5 0 0 483.75 34.80 5 0 0 483.65 39.10 6 0 0 562.44 41.40 -6 0 0 582.84 44.00 -6 0 0 576.24 41.80 6 0 0 574.74 42.60 6 0 0 582.04 48.30 6 0 0 546.65 42.50 -6 0 0 587.74 40.90 -7 0 0 43.20 15.00 7 0 0 37.80 13.10 7 0 0 26.00 13.80 7 0 0 30.60 16.80 7 0 0 54.69 20.60 -7 0 0 68.69 20.10 -7 0 0 65.09 18.90 -8 0 0 54.79 19.40 8 0 0 12.70 18.70 -8 0 0 32.60 18.10 -8 0 0 16.50 17.10 8 0 0 20.30 20.10 0 -1 0 0.00 0.70 0 -1 0 -0.50 0.60 0 1 0 1.70 0.80 1 1 0 6377.56 170.98 1 1 0 6600.94 174.78 -2 -1 0 3358.56 99.99 2 -1 0 3256.97 101.99 2 -1 0 3412.56 96.09 2 -1 0 3263.87 93.09 -2 -1 0 3267.17 102.49 2 -1 0 3110.69 93.29 -2 -1 0 3302.17 102.79 2 1 0 3315.67 103.19 2 1 0 3310.57 102.09 2 1 0 3431.26 101.59 -2 1 0 3282.97 93.49 -2 1 0 3352.56 94.99 3 -1 0 126.29 12.30 3 -1 0 98.19 15.00 -3 -1 0 81.19 13.50 -3 -1 0 95.19 12.20 3 -1 0 104.09 10.90 3 -1 0 107.89 12.40 -3 -1 0 88.39 13.80 3 1 0 79.39 13.10 -3 1 0 80.69 10.00 3 1 0 87.79 14.60 3 1 0 81.99 14.30 -3 1 0 110.09 11.70 -3 1 0 105.99 11.30 3 1 0 105.09 14.80 4 -1 0 253.97 21.40 -4 -1 0 271.17 25.30 4 -1 0 274.57 21.30 4 -1 0 257.47 22.40 -4 -1 0 264.27 24.40 4 -1 0 228.58 24.40 -4 -1 0 277.47 23.80 -4 1 0 257.77 20.40 -4 1 0 246.18 20.80 4 1 0 243.08 24.10 4 1 0 269.47 25.70 -4 1 0 239.08 20.10 4 1 0 264.17 24.40 4 1 0 281.97 24.90 5 -1 0 16.40 8.60 5 -1 0 26.80 12.80 -5 -1 0 12.40 7.60 5 -1 0 3.50 6.70 -5 -1 0 7.90 7.20 -5 -1 0 5.20 7.90 5 -1 0 10.00 7.00 5 1 0 15.90 9.10 5 1 0 6.20 9.10 -5 1 0 23.90 9.20 5 1 0 3.10 7.50 -5 1 0 14.30 6.40 -5 1 0 18.70 8.60 5 1 0 19.50 9.10 -6 -1 0 609.94 42.80 6 -1 0 603.04 44.10 6 -1 0 536.95 45.10 6 -1 0 561.94 38.00 6 -1 0 591.24 40.40 -6 -1 0 544.95 43.30 -6 1 0 562.24 38.00 6 1 0 637.04 45.30 6 1 0 567.54 45.80 -6 1 0 528.55 39.20 -6 1 0 499.55 38.70 6 1 0 589.64 45.00 6 1 0 487.25 44.40 -7 -1 0 47.90 17.10 -7 -1 0 -14.30 13.90 7 -1 0 -3.30 11.80 7 -1 0 10.70 11.20 7 -1 0 11.20 12.90 7 -1 0 34.00 18.60 -7 -1 0 16.00 14.40 -7 1 0 1.40 11.00 -7 1 0 -1.30 11.50 -7 1 0 19.70 12.70 7 1 0 5.30 13.30 7 1 0 11.70 15.90 7 1 0 9.90 13.10 7 1 0 -21.80 13.40 -8 -1 0 474.15 48.50 8 -1 0 345.67 42.90 8 -1 0 322.07 46.70 8 1 0 375.66 50.69 -8 1 0 382.26 43.50 8 1 0 285.37 43.90 0 -2 0 6807.52 187.28 -1 -2 0 1737.73 56.09 1 -2 0 1778.52 44.50 -1 -2 0 1703.23 58.69 1 -2 0 1624.94 44.70 1 -2 0 1704.73 49.20 1 -2 0 1738.03 52.29 -1 -2 0 1666.73 58.79 -1 2 0 1772.02 44.00 1 2 0 1715.13 51.29 1 2 0 1689.13 55.89 1 2 0 1604.44 57.59 1 2 0 1660.43 58.89 -2 -2 0 862.11 47.30 2 -2 0 773.82 26.20 2 -2 0 798.72 30.80 -2 -2 0 856.71 40.40 -2 -2 0 766.22 36.30 2 2 0 824.22 35.40 -2 2 0 812.02 30.20 2 2 0 776.72 38.50 -2 2 0 831.62 26.10 2 2 0 804.12 40.00 2 2 0 829.92 37.40 -2 2 0 811.22 24.30 -3 -2 0 564.44 33.40 3 -2 0 602.94 24.40 3 -2 0 596.84 29.70 -3 -2 0 568.64 36.20 -3 -2 0 537.75 35.40 3 -2 0 584.94 26.10 3 -2 0 640.14 35.90 3 2 0 573.54 35.80 -3 2 0 575.64 28.00 3 2 0 608.14 34.30 -3 2 0 567.84 25.40 3 2 0 566.44 36.20 3 2 0 580.44 34.40 -4 -2 0 2.20 5.20 4 -2 0 7.40 3.30 4 -2 0 6.80 5.50 4 -2 0 8.60 5.20 -4 -2 0 -1.50 6.40 4 -2 0 5.30 4.10 -4 -2 0 1.90 4.90 4 -2 0 7.60 4.40 4 2 0 7.50 5.60 4 2 0 2.30 6.40 -4 2 0 -2.40 3.40 4 2 0 -6.40 4.90 4 2 0 8.90 7.00 -4 2 0 -0.30 3.00 -5 -2 0 49.99 14.00 -5 -2 0 59.19 16.50 5 -2 0 48.00 10.40 -5 -2 0 38.30 12.60 5 -2 0 40.70 10.10 5 -2 0 37.80 13.20 5 -2 0 50.19 12.40 5 2 0 54.99 15.40 5 2 0 29.30 11.20 -5 2 0 30.00 9.40 -5 2 0 41.00 9.10 -5 2 0 36.10 9.00 5 2 0 27.30 11.70 5 2 0 64.39 15.40 6 -2 0 67.79 13.40 6 -2 0 64.89 14.00 -6 -2 0 49.40 17.00 6 -2 0 76.69 21.20 -6 2 0 64.99 12.80 -6 2 0 65.19 15.10 6 2 0 58.89 17.10 6 2 0 57.99 18.90 -6 2 0 57.09 13.20 6 2 0 69.99 18.80 -7 -2 0 344.97 52.09 7 -2 0 361.66 38.80 -7 -2 0 359.36 39.70 -7 -2 0 331.17 37.70 7 -2 0 328.87 31.60 7 -2 0 362.16 29.80 7 -2 0 375.36 43.80 -7 2 0 409.06 31.30 7 2 0 435.06 46.60 7 2 0 384.86 41.40 7 2 0 347.87 40.30 -7 2 0 354.36 37.00 -8 -2 0 535.45 57.09 8 -2 0 525.95 43.40 8 2 0 380.56 60.19 -8 2 0 418.96 46.20 0 -3 0 -0.20 1.70 0 -3 0 0.20 1.50 0 3 0 0.80 1.70 -1 -3 0 7574.34 210.78 1 -3 0 7530.35 193.98 -1 -3 0 7230.58 210.08 1 -3 0 7678.93 197.58 -1 -3 0 7491.45 205.88 1 -3 0 7320.97 194.48 -1 3 0 7652.73 192.98 -1 3 0 7413.76 194.18 1 3 0 7651.23 196.38 1 3 0 7800.22 211.08 1 3 0 7858.41 207.18 1 3 0 7091.89 210.18 -2 -3 0 1498.05 63.59 -2 -3 0 1545.65 63.99 -2 -3 0 1528.25 59.29 2 -3 0 1553.74 49.70 2 3 0 1521.05 59.79 2 3 0 1506.55 54.39 2 3 0 1496.45 63.89 2 3 0 1485.65 62.49 3 -3 0 196.08 19.30 -3 -3 0 193.38 19.40 3 -3 0 206.38 9.20 3 -3 0 219.18 16.30 -3 -3 0 204.48 21.60 -3 3 0 204.98 15.10 -3 3 0 194.98 8.30 -3 3 0 192.48 9.10 3 3 0 192.78 20.70 3 3 0 182.48 20.10 3 3 0 192.48 18.10 3 3 0 172.28 21.00 4 -3 0 383.66 25.20 -4 -3 0 353.26 33.20 -4 -3 0 298.97 27.70 -4 -3 0 357.56 32.30 4 -3 0 339.87 18.70 4 -3 0 345.17 16.70 4 -3 0 333.97 29.00 -4 3 0 344.17 16.00 4 3 0 288.37 29.00 4 3 0 371.56 30.40 4 3 0 331.17 31.30 -4 3 0 297.97 17.20 -4 3 0 343.67 22.70 4 3 0 368.36 33.80 4 3 0 350.36 30.90 -5 -3 0 143.09 23.00 -5 -3 0 149.39 25.80 5 -3 0 82.19 18.00 5 -3 0 131.79 14.00 5 -3 0 115.59 11.50 5 -3 0 125.19 18.90 -5 -3 0 105.89 20.90 -5 3 0 157.38 17.50 5 3 0 124.59 24.20 -5 3 0 135.79 11.70 5 3 0 117.69 23.40 5 3 0 131.69 22.50 -5 3 0 131.49 13.50 5 3 0 106.59 21.40 6 -3 0 282.17 32.60 -6 -3 0 213.08 33.20 6 -3 0 276.77 19.90 6 -3 0 216.28 21.30 -6 -3 0 255.67 30.80 6 -3 0 230.88 27.40 -6 3 0 254.07 20.80 6 3 0 208.28 32.50 6 3 0 203.78 29.70 6 3 0 243.08 33.80 -6 3 0 208.88 23.80 6 3 0 207.98 34.30 -6 3 0 240.28 17.80 7 -3 0 -4.90 15.30 7 -3 0 -1.80 7.60 7 -3 0 5.40 9.60 7 -3 0 8.50 12.60 -7 -3 0 20.00 16.10 -7 -3 0 -25.00 12.60 -7 -3 0 3.40 17.10 7 3 0 1.70 17.00 7 3 0 7.10 16.00 7 3 0 -0.70 18.80 -7 3 0 13.10 8.80 -7 3 0 3.10 6.50 7 3 0 19.10 20.00 8 -3 0 182.08 22.00 8 -3 0 164.88 30.00 8 -3 0 188.48 24.50 -8 -3 0 167.88 36.80 -8 3 0 189.08 24.30 -8 3 0 157.88 29.00 8 3 0 141.89 37.50 0 -4 0 6931.81 194.08 0 -4 0 7046.29 194.78 0 4 0 7000.80 193.38 -1 -4 0 4773.02 146.19 1 -4 0 4784.42 129.89 -1 -4 0 5036.00 141.59 1 -4 0 4814.02 128.09 -1 4 0 4880.71 128.69 1 4 0 4650.03 144.39 1 4 0 4698.33 125.99 1 4 0 4556.54 144.29 -1 4 0 4591.44 129.59 -2 -4 0 7727.83 233.58 2 -4 0 8368.16 226.78 -2 -4 0 8012.20 234.68 2 -4 0 7878.41 211.58 -2 -4 0 8183.58 227.68 2 4 0 7858.41 215.98 2 4 0 7629.34 231.88 2 4 0 7977.70 227.68 2 4 0 7805.92 232.38 2 4 0 7978.60 235.68 3 -4 0 610.54 34.90 -3 -4 0 654.03 39.40 -3 -4 0 596.04 41.70 3 -4 0 618.44 29.50 -3 -4 0 539.55 40.10 3 4 0 601.34 34.00 3 4 0 582.14 41.70 3 4 0 591.84 38.50 3 4 0 607.14 41.40 3 4 0 603.34 40.70 -4 -4 0 2057.49 96.19 -4 -4 0 2161.08 96.99 4 -4 0 2222.98 78.89 -4 -4 0 2123.29 90.19 4 -4 0 2254.17 88.99 4 4 0 2044.10 93.99 4 4 0 2195.58 87.19 4 4 0 2329.67 98.29 4 4 0 2298.87 95.09 5 -4 0 651.73 40.10 -5 -4 0 648.54 52.09 5 -4 0 679.13 25.50 -5 -4 0 624.04 50.09 5 -4 0 633.14 45.90 5 -4 0 686.63 23.40 5 4 0 720.53 50.79 -5 4 0 639.64 20.20 -5 4 0 700.13 20.30 5 4 0 629.54 45.40 5 4 0 635.84 49.50 5 4 0 602.44 49.00 6 -4 0 57.99 8.80 -6 -4 0 55.49 22.80 -6 -4 0 62.49 18.00 6 -4 0 83.99 8.60 -6 -4 0 40.70 19.00 6 -4 0 41.10 16.20 6 -4 0 53.79 14.10 -6 4 0 61.89 15.50 6 4 0 60.69 19.10 6 4 0 52.99 16.90 -6 4 0 71.29 6.70 6 4 0 36.70 15.50 6 4 0 30.00 18.70 -6 4 0 64.59 7.30 7 -4 0 100.19 21.80 -7 -4 0 118.09 30.30 -7 -4 0 88.79 23.30 7 -4 0 112.69 13.70 7 -4 0 128.19 27.80 7 -4 0 126.79 11.90 7 4 0 89.79 26.80 -7 4 0 109.69 11.00 7 4 0 110.89 29.20 7 4 0 97.69 27.40 -7 4 0 111.99 9.40 7 4 0 151.98 33.20 0 -5 0 5.40 3.70 0 -5 0 5.30 4.30 0 -5 0 3.20 3.00 0 5 0 4.70 4.30 0 5 0 8.30 5.40 -1 -5 0 1480.65 57.39 1 -5 0 1378.66 42.20 -1 -5 0 1349.86 60.19 -1 -5 0 1364.26 60.79 1 -5 0 1342.87 48.80 1 -5 0 1263.87 47.40 1 5 0 1407.06 60.49 1 5 0 1408.46 39.40 -1 5 0 1381.06 48.60 -1 5 0 1350.86 46.80 1 5 0 1384.06 60.59 -2 -5 0 1164.48 59.99 2 -5 0 1257.07 51.89 2 -5 0 1214.98 33.80 2 -5 0 1171.18 36.50 -2 -5 0 1189.78 59.99 2 -5 0 1149.89 42.80 -2 -5 0 1172.48 54.59 2 5 0 1139.09 58.99 2 5 0 1164.08 44.00 2 5 0 1221.38 60.09 -2 5 0 1225.48 31.80 -3 -5 0 15.30 8.70 -3 -5 0 6.90 6.60 3 -5 0 1.20 4.80 -3 -5 0 6.40 7.80 3 -5 0 12.40 4.80 3 5 0 5.60 4.20 3 5 0 -0.10 5.90 3 5 0 15.60 9.30 3 5 0 10.10 8.40 -4 -5 0 499.85 38.80 -4 -5 0 409.96 39.20 4 -5 0 474.95 29.20 -4 -5 0 436.56 40.00 4 -5 0 509.55 35.80 4 5 0 467.55 41.50 4 5 0 481.45 34.00 4 5 0 502.15 39.90 4 5 0 531.55 44.30 5 -5 0 12.60 13.50 5 -5 0 13.70 7.50 -5 -5 0 15.50 14.20 5 5 0 -5.40 10.40 5 5 0 8.70 10.30 5 5 0 7.70 10.50 5 5 0 24.40 12.50 6 -5 0 388.56 33.20 6 -5 0 407.96 40.90 -6 -5 0 387.56 39.40 -6 -5 0 405.36 45.10 -6 -5 0 369.36 45.80 6 5 0 424.16 41.10 6 5 0 394.26 44.50 6 5 0 345.27 43.10 6 5 0 458.45 46.70 -7 -5 0 -8.00 22.70 7 -5 0 -4.40 13.20 7 5 0 -18.80 23.70 7 5 0 2.10 18.70 7 5 0 31.20 22.30 0 -6 0 3702.53 119.39 0 -6 0 3648.93 115.29 0 -6 0 3506.15 117.79 0 6 0 3660.03 117.39 0 6 0 3657.23 118.39 1 -6 0 137.99 13.00 -1 -6 0 93.19 16.50 1 -6 0 95.39 6.30 -1 -6 0 126.49 15.00 1 -6 0 107.69 12.10 -1 -6 0 104.99 18.00 -1 6 0 102.09 11.60 -1 6 0 102.19 10.90 1 6 0 104.19 17.40 1 6 0 123.89 18.60 -2 -6 0 506.55 34.60 -2 -6 0 487.95 38.20 2 -6 0 503.75 18.70 2 -6 0 472.45 20.10 -2 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-6 -7 504.95 55.59 -1 -6 -7 532.95 48.50 -1 -6 -7 556.84 48.70 -1 6 -7 508.25 44.70 -1 6 -7 462.45 50.59 1 6 7 520.65 46.00 -1 6 -7 535.05 62.69 2 -6 7 61.49 27.10 -2 -6 -7 101.59 30.40 -2 -6 -7 49.70 43.90 2 -6 7 95.39 23.70 -2 6 -7 66.39 26.00 -2 6 -7 68.29 28.20 2 6 7 40.00 23.90 -2 -7 7 23.10 25.80 -2 -7 7 -24.00 16.40 2 -7 -7 -15.70 17.30 2 -7 -7 -5.40 15.90 2 -7 -7 -6.30 12.60 2 7 -7 -3.40 24.90 2 7 -7 10.40 14.40 2 7 -7 -3.50 18.40 2 7 -7 -21.80 17.00 -2 7 7 -1.80 17.00 1 -7 -7 146.69 32.80 -1 -7 7 203.88 35.00 -1 -7 7 207.08 37.10 1 -7 -7 236.78 34.90 1 -7 -7 198.68 30.70 1 7 -7 226.48 45.10 1 7 -7 225.28 33.80 0 -7 7 80.69 28.10 0 -7 -7 130.09 30.90 0 -7 -7 101.99 26.30 0 -7 -7 95.79 25.20 0 -7 7 145.69 27.70 0 7 -7 80.49 33.40 1 -7 7 29.80 19.00 -1 -7 -7 -2.20 17.60 -1 -7 -7 -43.30 24.80 -1 7 -7 -6.10 19.40 1 7 7 -49.60 19.30 -1 7 -7 5.60 21.30 4 0 -8 65.69 25.60 4 0 -8 98.89 23.60 3 0 -8 -8.10 16.30 3 0 -8 -10.20 13.90 -3 0 8 -18.30 16.80 3 0 -8 -15.40 15.40 2 0 -8 249.08 37.30 2 0 -8 215.98 29.80 2 0 -8 328.87 38.30 2 0 -8 296.67 48.70 -2 0 8 274.17 34.90 -2 0 8 320.37 40.10 -1 0 8 -8.80 13.50 1 0 -8 -1.70 12.80 1 0 -8 9.50 15.10 1 0 -8 -4.30 15.80 -1 0 8 -10.10 14.50 1 0 -8 5.40 9.90 0 0 -8 1058.69 72.49 0 0 -8 1108.99 70.59 0 0 -8 840.82 64.59 0 0 8 947.41 65.49 0 0 8 991.60 69.79 0 0 -8 900.41 55.09 1 0 8 -12.10 12.80 -1 0 -8 -12.40 12.90 -1 0 -8 15.80 19.70 -1 0 -8 -12.10 17.00 1 0 8 -8.10 16.30 -2 0 -8 631.84 57.69 2 0 8 691.13 55.29 2 0 8 715.23 63.09 -2 0 -8 634.14 56.39 3 0 8 485.25 56.29 3 0 8 458.75 47.80 -3 0 -8 413.36 57.39 -3 0 -8 405.06 45.10 4 -1 -8 36.00 20.00 -4 -1 8 7.90 25.40 4 -1 -8 34.40 19.60 4 1 -8 -16.00 16.70 4 1 -8 8.20 19.60 -4 1 8 -53.19 25.40 3 -1 -8 670.53 62.89 3 -1 -8 702.53 52.69 3 -1 -8 614.44 56.59 -3 -1 8 698.33 62.79 3 1 -8 716.63 55.29 3 1 -8 733.33 66.59 3 1 -8 760.12 56.69 -3 1 8 707.93 59.59 2 -1 -8 97.49 22.70 -2 -1 8 110.19 25.80 -2 -1 8 74.09 28.80 2 -1 -8 89.29 21.80 2 -1 -8 107.49 26.50 2 -1 -8 80.49 21.10 2 1 -8 90.69 24.50 2 1 -8 85.39 24.00 2 1 -8 81.29 34.80 -2 1 8 99.19 24.50 -2 1 8 94.59 25.20 2 1 -8 117.29 25.00 1 -1 -8 754.62 77.99 1 -1 -8 581.74 50.99 1 -1 -8 621.54 53.79 -1 -1 8 719.83 55.69 1 -1 -8 612.64 47.70 -1 -1 8 630.34 55.29 1 1 -8 712.93 54.59 -1 1 8 574.14 51.59 1 1 -8 574.74 42.80 1 1 -8 713.13 58.49 1 1 -8 606.54 56.09 -1 1 8 688.93 54.49 0 -1 -8 266.97 30.80 0 -1 -8 281.77 42.10 0 -1 8 264.87 39.20 0 -1 -8 299.77 38.70 0 -1 -8 379.66 42.40 0 1 -8 239.38 28.80 0 1 -8 306.67 38.30 0 1 -8 302.27 43.00 0 1 -8 272.17 40.70 0 1 8 296.37 38.40 -1 -1 -8 372.56 43.90 -1 -1 -8 491.75 50.09 1 -1 8 501.75 81.49 -1 -1 -8 497.75 51.99 1 -1 8 439.16 45.50 1 1 8 396.16 48.50 -1 1 -8 450.05 46.20 -1 1 -8 429.96 51.89 -1 1 -8 421.16 34.00 1 1 8 411.96 44.00 -1 1 -8 408.86 46.90 -2 -1 -8 219.58 39.40 -2 -1 -8 195.58 35.10 2 -1 8 171.58 49.70 2 -1 8 161.98 30.50 -2 1 -8 166.58 29.00 2 1 8 249.18 36.40 -2 1 -8 232.78 38.10 2 1 8 321.37 48.40 -3 -1 -8 384.66 48.70 3 -1 8 413.16 46.30 -3 -1 -8 440.46 59.39 3 -1 8 424.06 55.39 -3 1 -8 475.55 52.09 -3 1 -8 409.66 41.60 3 1 8 384.46 62.29 4 -2 -8 10.40 18.70 -4 -2 8 -32.00 27.50 4 2 -8 33.10 22.30 -4 2 8 12.80 24.80 4 2 -8 19.40 20.10 3 -2 -8 160.48 30.00 3 -2 -8 187.58 31.00 -3 -2 8 88.79 36.20 3 -2 -8 126.89 27.70 3 2 -8 255.37 43.90 3 2 -8 139.29 29.30 3 2 -8 183.48 32.10 -2 -2 8 17.10 21.30 2 -2 -8 -0.20 17.00 2 -2 -8 -11.20 14.70 2 -2 -8 13.00 16.60 2 -2 -8 53.59 20.90 -2 -2 8 48.60 18.00 -2 2 8 53.69 17.90 2 2 -8 36.40 18.60 2 2 -8 20.40 24.80 -2 2 8 23.50 21.90 2 2 -8 55.69 19.00 2 2 -8 31.20 16.10 1 -2 -8 151.58 27.80 1 -2 -8 158.38 25.50 1 -2 -8 120.69 25.60 -1 -2 8 195.38 32.40 -1 -2 8 145.99 31.00 1 -2 -8 113.89 25.90 1 2 -8 129.39 23.20 -1 2 8 229.88 35.00 1 2 -8 214.08 39.70 -1 2 8 190.68 31.90 1 2 -8 199.88 34.30 1 2 -8 187.98 32.20 0 -2 8 231.58 36.00 0 -2 8 263.27 57.99 0 -2 -8 164.38 33.90 0 -2 -8 235.58 37.50 0 2 8 188.78 34.50 0 2 -8 200.38 24.80 0 2 -8 193.58 35.00 0 2 -8 214.38 35.90 0 2 8 203.98 32.90 0 2 -8 153.78 29.80 -1 -2 -8 -9.80 13.40 1 -2 8 -24.50 15.80 -1 -2 -8 -9.10 18.60 1 -2 8 3.90 14.90 -1 -2 -8 -7.80 17.60 -1 2 -8 0.30 9.60 -1 2 -8 2.80 16.00 1 2 8 -17.30 17.80 1 2 8 -6.80 15.60 -1 2 -8 15.70 16.50 -1 2 -8 -25.20 18.90 -2 -2 -8 238.98 37.60 -2 -2 -8 260.17 41.60 2 -2 8 237.38 45.00 -2 2 -8 226.08 38.80 -2 2 -8 240.88 38.50 2 2 8 257.67 49.80 -2 2 -8 278.67 26.60 -2 2 -8 258.27 31.90 2 2 8 207.18 33.80 3 -3 -8 -4.00 15.20 3 -3 -8 23.60 16.80 3 -3 -8 11.70 17.70 -3 -3 8 6.70 22.50 3 3 -8 3.70 18.80 3 3 -8 19.00 19.30 -3 3 8 7.50 19.10 3 3 -8 -17.90 20.00 2 -3 -8 -0.30 15.50 2 -3 -8 -5.40 14.60 2 -3 -8 7.50 14.00 -2 -3 8 -16.80 14.80 2 -3 -8 -26.90 18.20 -2 -3 8 -3.80 20.70 2 3 -8 -15.00 11.80 2 3 -8 -0.70 18.80 2 3 -8 10.00 17.30 2 3 -8 10.50 18.20 -2 3 8 8.60 16.80 1 -3 -8 476.15 48.70 1 -3 -8 520.45 60.39 -1 -3 8 506.05 45.20 1 -3 -8 521.25 48.00 -1 -3 8 384.46 48.20 1 -3 -8 472.95 47.90 1 3 -8 489.65 52.29 1 3 -8 475.25 55.49 1 3 -8 562.74 47.90 -1 3 8 419.76 44.50 -1 3 8 478.65 49.50 0 -3 8 26.50 23.60 0 -3 -8 22.60 16.20 0 -3 -8 -28.40 17.10 0 -3 -8 25.30 19.60 0 -3 8 -10.90 19.10 0 3 -8 13.70 16.00 0 3 8 -2.60 19.00 0 3 8 9.50 16.60 0 3 -8 40.00 19.60 0 3 -8 -5.90 10.20 0 3 -8 -21.30 17.30 1 -3 8 2233.18 111.69 -1 -3 -8 2313.57 118.89 -1 -3 -8 1882.81 106.39 1 -3 8 2244.48 109.19 -1 -3 -8 2131.69 107.09 1 3 8 2229.18 105.99 -1 3 -8 2065.79 113.29 -1 3 -8 2224.38 108.39 -1 3 -8 2229.28 81.59 -2 -3 -8 20.30 18.20 2 -3 8 15.80 19.40 2 -3 8 31.70 18.10 -2 -3 -8 36.10 27.10 -2 -3 -8 12.50 21.90 -2 3 -8 -6.30 11.60 2 3 8 24.40 21.70 -2 3 -8 5.70 19.90 -2 3 -8 49.50 29.30 -2 3 -8 4.10 10.40 -3 -4 8 -8.90 28.90 3 -4 -8 24.30 16.10 3 4 -8 35.00 22.10 -3 4 8 -60.19 21.10 3 4 -8 -14.80 17.60 3 4 -8 35.70 27.70 2 -4 -8 114.79 26.90 2 -4 -8 60.09 21.80 -2 -4 8 127.49 26.80 2 -4 -8 110.09 27.90 -2 -4 8 70.99 28.00 2 -4 -8 71.89 26.10 2 4 -8 115.79 27.50 2 4 -8 163.48 24.60 2 4 -8 100.89 34.70 -1 -4 8 -7.30 20.20 1 -4 -8 -9.90 17.60 -1 -4 8 -17.80 15.30 1 -4 -8 12.40 15.90 1 -4 -8 6.00 13.10 -1 4 8 14.00 20.30 1 4 -8 -3.00 11.80 1 4 -8 -18.90 16.90 1 4 -8 0.50 15.20 1 4 -8 6.40 20.30 0 -4 -8 403.76 47.50 0 -4 8 449.46 51.89 0 -4 -8 399.96 44.60 0 -4 -8 404.56 49.00 0 4 8 441.66 43.40 0 4 -8 482.95 51.79 0 4 -8 473.75 33.40 0 4 -8 517.15 46.20 0 4 -8 354.86 52.89 -1 -4 -8 87.39 33.10 -1 -4 -8 111.09 28.90 1 -4 8 85.99 27.60 -1 -4 -8 55.39 24.40 1 -4 8 90.59 25.90 -1 4 -8 83.59 30.40 -1 4 -8 72.79 24.70 -2 -4 -8 931.11 79.49 2 -4 8 853.91 67.29 2 4 8 980.10 68.69 -2 -5 8 33.50 28.00 2 -5 -8 -32.20 20.80 2 -5 -8 -36.20 18.90 2 5 -8 5.40 24.20 2 5 -8 -25.80 18.50 -2 5 8 -16.40 18.30 2 5 -8 -7.30 15.00 1 -5 -8 210.48 37.50 -1 -5 8 342.77 44.10 1 -5 -8 268.57 37.60 1 5 -8 231.48 28.70 1 5 -8 250.17 39.40 0 -5 -8 -1.20 21.70 0 -5 8 -17.70 16.90 0 -5 -8 0.90 17.60 0 -5 8 6.10 23.10 0 5 -8 -0.20 21.80 0 5 8 2.20 17.10 0 5 -8 6.10 18.10 0 5 -8 -6.10 10.20 1 -5 8 1250.07 78.79 -1 -5 -8 1017.10 75.19 1 -5 8 1073.09 86.09 -1 -5 -8 1038.30 93.29 -1 5 -8 1195.78 87.09 1 5 8 1178.38 75.09 -1 0 9 -1.70 23.00 1 0 -9 -40.10 17.90 1 0 -9 -7.20 20.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 34299 _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 0.20413(7) 0.250000 0.18874(7) 0.01733(15) Uani 1 2 d S T P . . O1 O 0.0926(2) 0.250000 0.5950(2) 0.0189(3) Uani 1 2 d S T P . . H1 H 0.096939 0.237471 0.472379 0.028 Uiso 0.5 1 calc R U P A -1 N1 N 0.2991(2) 0.250000 0.6859(2) 0.0147(3) Uani 1 2 d S T P . . C3 C 0.7006(3) 0.250000 0.8702(3) 0.0179(4) Uani 1 2 d S T P . . H3 H 0.842000 0.249999 0.934183 0.021 Uiso 1 2 calc R U P . . C2 C 0.5974(2) 0.37999(15) 0.82350(19) 0.0172(3) Uani 1 1 d . . . . . H2 H 0.667940 0.469239 0.856130 0.021 Uiso 1 1 calc R U . . . C1 C 0.3913(2) 0.38048(15) 0.72926(19) 0.0164(3) Uani 1 1 d . . . . . C4 C 0.2678(2) 0.51500(16) 0.6744(2) 0.0219(3) Uani 1 1 d . . . . . H4A H 0.224404 0.514212 0.531760 0.033 Uiso 1 1 calc R U . . . H4B H 0.358147 0.600099 0.706967 0.033 Uiso 1 1 calc R U . . . H4C H 0.139616 0.519169 0.748353 0.033 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 0.0175(2) 0.0190(3) 0.0153(2) 0.000 0.00038(17) 0.000 O1 0.0115(6) 0.0302(8) 0.0143(7) 0.000 -0.0025(5) 0.000 N1 0.0111(7) 0.0210(8) 0.0119(7) 0.000 0.0004(6) 0.000 C3 0.0147(9) 0.0265(10) 0.0125(9) 0.000 0.0018(7) 0.000 C2 0.0171(6) 0.0206(7) 0.0140(6) -0.0006(5) 0.0016(5) -0.0034(5) C1 0.0176(6) 0.0200(7) 0.0120(6) 0.0001(5) 0.0030(5) 0.0002(5) C4 0.0238(7) 0.0211(7) 0.0206(7) 0.0014(6) -0.0003(6) 0.0034(6) 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 N1 O1 H1 109.5 . . ? C1 N1 O1 117.42(8) . . ? C1 N1 O1 117.42(8) 4_565 . ? C1 N1 C1 125.14(16) 4_565 . ? C2 C3 H3 120.1 4_565 . ? C2 C3 H3 120.1 . . ? C2 C3 C2 119.86(18) . 4_565 ? C3 C2 H2 119.9 . . ? C3 C2 C1 120.26(13) . . ? C1 C2 H2 119.9 . . ? N1 C1 C2 117.24(13) . . ? N1 C1 C4 118.86(12) . . ? C2 C1 C4 123.90(13) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 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 O1 H1 0.8400 . ? O1 N1 1.3808(19) . ? N1 C1 1.3542(15) . ? N1 C1 1.3542(15) 4_565 ? C3 H3 0.9500 . ? C3 C2 1.3837(17) 4_565 ? C3 C2 1.3837(17) . ? C2 H2 0.9500 . ? C2 C1 1.3868(19) . ? C1 C4 1.4900(19) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 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 178.99(12) . . . . ? O1 N1 C1 C4 -0.9(2) . . . . ? C3 C2 C1 N1 -0.2(2) . . . . ? C3 C2 C1 C4 179.68(14) . . . . ? C2 C3 C2 C1 -0.3(3) 4_565 . . . ? C1 N1 C1 C2 0.7(3) 4_565 . . . ? C1 N1 C1 C4 -179.14(11) 4_565 . . . ?