#------------------------------------------------------------------------------ #$Date: 2017-06-05 15:53:23 +0100 (Mon, 05 Jun 2017) $ #$Revision: 197525 $ #$URL: svn://www.crystallography.net/cod/cif/3/50/00/3500069.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_3500069 loop_ _publ_author_name 'Thierry Maris' _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _journal_name_full 'Personal communication to COD' _journal_year 2017 _chemical_formula_moiety '2(Cl), H2 O, C12 H30 N2' _chemical_formula_sum 'C12 H32 Cl2 N2 O' _chemical_formula_weight 291.29 _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_Hall '-P 2yc' _space_group_name_H-M_alt 'P 1 2/c 1' _symmetry_space_group_name_Hall '-P 2yc' _symmetry_space_group_name_H-M 'P 1 2/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _audit_creation_date 2016-12-09 _audit_creation_method ; Olex2 1.2 (compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269) ; _cell_angle_alpha 90 _cell_angle_beta 91.721(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 15.1054(8) _cell_length_b 5.0745(3) _cell_length_c 10.7172(6) _cell_measurement_reflns_used 9272 _cell_measurement_temperature 100 _cell_measurement_theta_max 60.690 _cell_measurement_theta_min 2.546 _cell_volume 821.13(8) _computing_cell_refinement ; SAINT (2013) V8.37A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_collection ; APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_reduction ; SAINT (2013) V8.37A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_detector 'CMOS Area detector' _diffrn_detector_area_resol_mean 10.24 _diffrn_detector_type 'Bruker Photon 100 CMOS Detector' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device 'k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker Venture Metaljet' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_collimation 'Focusing mirrors' _diffrn_radiation_monochromator 'Helios MX Mirror Optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_unetI/netI 0.0290 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 11089 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 60.659 _diffrn_reflns_theta_min 2.546 _diffrn_source 'Metal Jet' _diffrn_source_target Ga _diffrn_source_type 'Gallium Liquid Metal Jet Source' _exptl_absorpt_coefficient_mu 2.302 _exptl_absorpt_correction_T_max 0.5163 _exptl_absorpt_correction_T_min 0.3955 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1157 before and 0.0675 after correction. The Ratio of minimum to maximum transmission is 0.7660. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light Colorless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary Colorless _exptl_crystal_density_diffrn 1.178 _exptl_crystal_description block _exptl_crystal_F_000 320 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Venture diffractometer equipped with a Photon 100 CMOS Detector, a Helios MX optics and a Kappa goniometer. The crystal-to-detector distance was 4.0 cm, and the data collection was carried out in 1024 x 1024 pixel mode. ; _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _refine_diff_density_max 0.602 _refine_diff_density_min -0.197 _refine_diff_density_rms 0.049 _refine_ls_extinction_coef 0.0112(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 143 _refine_ls_number_reflns 1885 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0297 _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^)+(0.0377P)^2^+0.3204P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0771 _refine_ls_wR_factor_ref 0.0792 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1753 _reflns_number_total 1885 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file bentet2.cif _cod_data_source_block bentet2 _cod_depositor_comments ; The following automatic conversions were performed: '_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_database_code 3500069 _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. ; _olex2_refinement_description ; ; _shelx_res_file ; TITL bentet2_a.res in P2/c bentet2.res created by SHELXL-2016/6 at 16:02:21 on 09-Dec-2016 REM Old TITL bentet2 in P2/c REM SHELXT solution in P2/c REM R1 0.116, Rweak 0.002, Alpha 0.016, Orientation as input REM Formula found by SHELXT: C12 N2 O Cl2 CELL 1.34139 15.1054 5.0745 10.7172 90 91.721 90 ZERR 2 0.0008 0.0003 0.0006 0 0.002 0 LATT 1 SYMM -X,+Y,0.5-Z SFAC C H Cl N O DISP C 0.014 0.007 57.748 DISP Cl 0.328 0.543 4162 DISP H -0 0 0.648 DISP N 0.025 0.014 110.512 DISP O 0.039 0.025 193.954 UNIT 24 64 4 4 2 EQIV $1 +X,1+Y,+Z EQIV $2 1-X,1-Y,1-Z EQIV $3 +X,1-Y,0.5+Z EQIV $4 +X,-Y,0.5+Z L.S. 30 PLAN 12 TEMP 0 HTAB N1 O1 HTAB N1 Cl1_$1 HTAB N1 Cl1_$2 HTAB C1 Cl1_$3 HTAB N1 Cl1 HTAB O1 Cl1_$4 BOND $H list 4 HTAB fmap 2 acta OMIT 3 0 2 OMIT 2 0 2 REM REM REM WGHT 0.037700 0.320400 EXTI 0.011176 FVAR 1.12026 CL1 3 0.396670 0.139062 0.405222 11.00000 0.02649 0.01943 = 0.02896 0.00100 0.01037 0.00043 O1 5 0.500000 0.294227 0.750000 10.50000 0.02599 0.02113 = 0.03101 0.00000 0.01192 0.00000 N1 4 0.391144 0.634136 0.584144 11.00000 0.02131 0.02083 = 0.02769 0.00323 0.01014 -0.00344 C1 1 0.298082 0.664393 0.624920 11.00000 0.02083 0.01739 = 0.02744 0.00184 0.01018 -0.00133 C2 1 0.264643 0.409022 0.680456 11.00000 0.02261 0.01648 = 0.02949 0.00103 0.01255 -0.00129 C3 1 0.182332 0.452059 0.756970 11.00000 0.02180 0.01711 = 0.02762 0.00151 0.01170 -0.00080 C4 1 0.146856 0.195092 0.810234 11.00000 0.02175 0.01681 = 0.02587 0.00063 0.01140 -0.00162 C5 1 0.072969 0.236795 0.901995 11.00000 0.02275 0.01771 = 0.02573 0.00133 0.01155 -0.00086 C6 1 0.037128 -0.020430 0.954160 11.00000 0.02325 0.01814 = 0.02755 0.00205 0.01276 -0.00038 H1A 2 0.426157 0.600456 0.643834 11.00000 0.03290 H2A 2 0.311086 0.333897 0.732273 11.00000 0.02667 H4A 2 0.195333 0.101251 0.853621 11.00000 0.02476 H5A 2 0.024541 0.333255 0.859009 11.00000 0.02468 H6A 2 0.086208 -0.113822 0.997766 11.00000 0.02274 H5B 2 0.096085 0.346429 0.970617 11.00000 0.02894 H6B 2 0.013812 -0.130125 0.883086 11.00000 0.02642 H4B 2 0.124148 0.082273 0.742553 11.00000 0.02658 H3A 2 0.198694 0.570469 0.827893 11.00000 0.03098 H3B 2 0.135312 0.537981 0.705470 11.00000 0.03032 H1B 2 0.410142 0.781919 0.546474 11.00000 0.03714 H1D 2 0.298174 0.810369 0.687493 11.00000 0.02918 H1E 2 0.263769 0.716746 0.552696 11.00000 0.02477 H1C 2 0.394268 0.495435 0.524442 11.00000 0.03974 H2B 2 0.253085 0.281695 0.616123 11.00000 0.03210 H1 2 0.469827 0.189203 0.797509 11.00000 0.05896 HKLF 4 REM bentet2_a.res in P2/c REM R1 = 0.0297 for 1753 Fo > 4sig(Fo) and 0.0321 for all 1885 data REM 143 parameters refined using 0 restraints END WGHT 0.0370 0.3222 REM Instructions for potential hydrogen bonds HTAB N1 O1 HTAB N1 Cl1_$1 HTAB N1 Cl1_$2 HTAB C1 Cl1_$3 HTAB N1 Cl1 HTAB O1 Cl1_$4 REM Highest difference peak 0.602, deepest hole -0.197, 1-sigma level 0.049 Q1 1 0.4275 0.1379 0.4706 11.00000 0.05 0.60 Q2 1 0.1124 0.2155 0.8587 11.00000 0.05 0.34 Q3 1 0.0000 0.0000 1.0000 10.50000 0.05 0.32 Q4 1 0.2244 0.4333 0.7141 11.00000 0.05 0.29 Q5 1 0.1630 0.3246 0.7838 11.00000 0.05 0.28 Q6 1 0.2837 0.5345 0.6550 11.00000 0.05 0.26 Q7 1 0.0555 0.1106 0.9218 11.00000 0.05 0.26 Q8 1 0.3530 0.1447 0.3426 11.00000 0.05 0.24 Q9 1 0.3604 0.0567 0.4343 11.00000 0.05 0.18 Q10 1 0.3445 0.6519 0.6016 11.00000 0.05 0.18 Q11 1 0.2963 0.4147 0.7463 11.00000 0.05 0.18 Q12 1 0.4928 1.0356 0.5185 11.00000 0.05 0.17 ; _shelx_res_checksum 36002 _shelx_hkl_file ; 0 0 -2 63.89 4.00 0 0 2 69.09 4.00 0 0 -2 67.69 3.80 0 0 2 64.19 3.80 0 0 3 0.80 0.60 0 0 3 -0.30 0.20 0 0 -3 0.30 0.60 0 0 -3 0.20 0.30 0 0 -4 1663.73 93.19 0 0 4 1651.93 93.29 0 0 4 1685.93 93.59 0 0 -4 1695.93 93.29 0 0 -4 1683.73 93.59 0 0 -5 -0.20 0.50 0 0 5 0.10 0.40 0 0 5 0.80 1.20 0 0 -5 0.30 0.90 0 0 -6 2929.01 171.78 0 0 6 3428.76 172.08 0 0 -6 3223.68 172.08 0 0 6 2826.72 171.88 0 0 6 2962.50 171.58 0 0 6 3112.59 171.48 0 0 7 0.00 1.10 0 0 7 -0.10 0.90 0 0 -7 -1.30 2.00 0 0 -7 -1.10 1.00 0 0 -7 0.30 1.10 0 0 7 -0.30 1.50 0 0 -7 1.20 2.80 0 0 -8 4.70 1.20 0 0 -8 0.80 1.10 0 0 8 2.10 1.20 0 0 8 3.80 1.70 0 0 9 0.00 2.20 0 0 -9 -0.20 1.30 0 0 9 -0.80 1.30 0 0 -9 0.80 1.30 0 0 -10 423.56 24.30 0 0 -10 407.56 24.60 0 0 10 457.05 24.90 0 0 10 418.76 25.50 0 0 -11 1.40 1.90 0 0 11 1.60 2.70 0 0 11 -2.80 2.60 0 0 11 -5.30 2.80 0 0 12 238.98 13.80 0 0 12 214.08 14.50 0 0 13 -1.80 2.50 0 -1 0 12.40 0.80 0 1 -1 244.08 13.80 0 1 1 261.17 14.10 0 -1 1 237.58 13.80 0 1 2 2815.72 149.29 0 1 -2 2910.41 149.09 0 1 -2 2740.93 148.99 0 -1 2 2600.94 148.99 0 -1 -2 2435.36 148.89 0 -1 2 2426.46 148.89 0 -1 -2 2836.52 149.29 0 1 -3 5986.80 317.07 0 1 -3 6400.66 317.27 0 -1 3 6316.37 317.27 0 -1 -3 4988.20 317.07 0 -1 3 4904.51 317.07 0 -1 -3 5951.20 317.47 0 -1 3 5417.26 317.07 0 1 -4 344.17 18.60 0 1 -4 314.07 18.80 0 1 4 322.67 19.10 0 -1 -4 351.86 18.60 0 -1 4 347.07 18.60 0 -1 4 318.77 19.00 0 -1 -4 313.47 19.00 0 1 5 -0.40 1.60 0 1 5 1.50 1.00 0 1 -5 0.60 0.50 0 1 -5 0.00 1.00 0 -1 5 1.30 0.40 0 -1 5 0.80 1.20 0 -1 -5 -0.10 0.50 0 -1 -5 0.30 1.00 0 1 6 105.39 7.00 0 -1 6 115.69 7.00 0 -1 -6 107.19 6.90 0 -1 6 110.19 6.70 0 -1 -6 105.79 7.30 0 -1 6 115.99 7.50 0 -1 6 125.99 7.60 0 1 7 438.26 25.50 0 -1 -7 433.26 25.50 0 -1 7 450.85 26.00 0 -1 -7 467.75 26.30 0 -1 7 434.56 25.40 0 1 8 50.09 4.60 0 1 8 51.89 3.80 0 -1 8 46.50 3.80 0 -1 -8 43.30 3.60 0 -1 8 55.09 4.80 0 -1 -8 51.39 6.90 0 1 9 123.09 8.10 0 1 9 120.89 8.80 0 -1 9 124.29 8.00 0 -1 -9 129.89 7.70 0 -1 9 121.69 8.90 0 -1 -9 124.59 8.00 0 1 10 129.99 9.80 0 1 10 140.49 9.20 0 -1 10 135.39 9.90 0 -1 10 152.18 9.20 0 -1 -10 152.38 8.80 0 -1 -10 143.49 9.00 0 1 11 26.10 4.10 0 1 11 18.60 2.90 0 -1 11 20.70 3.30 0 -1 -11 22.40 2.60 0 -1 11 22.70 4.10 0 -1 -11 20.00 2.90 0 1 12 6.00 2.90 0 1 12 9.10 2.10 0 -1 12 7.80 2.90 0 -1 -12 7.30 1.90 0 -1 -12 9.30 1.80 0 1 -13 4.10 4.30 0 1 13 2.30 2.70 0 1 13 1.90 2.90 0 1 13 9.40 2.00 0 -1 13 6.90 2.70 0 -1 -13 5.50 1.90 0 -1 13 2.10 2.60 0 -2 0 696.93 38.80 0 2 1 709.73 38.80 0 -2 1 664.03 38.30 0 2 2 7.70 1.50 0 2 -2 5.20 0.70 0 2 -2 6.00 1.10 0 -2 2 3.70 0.90 0 -2 2 4.90 0.60 0 2 -3 111.19 6.50 0 2 -3 108.79 6.70 0 -2 -3 95.19 6.50 0 -2 -3 111.79 6.50 0 -2 3 128.09 6.70 0 -2 3 115.49 6.50 0 2 -4 652.33 36.30 0 2 -4 643.84 36.20 0 2 -4 633.54 36.50 0 -2 4 652.23 36.30 0 -2 -4 634.14 36.60 0 -2 4 640.44 36.80 0 -2 -4 585.24 36.20 0 -2 -4 673.13 36.20 0 -2 4 705.13 36.30 0 2 -5 278.77 15.70 0 2 -5 281.27 15.20 0 2 5 250.77 15.50 0 -2 -5 236.18 15.60 0 -2 5 266.77 15.30 0 -2 5 265.47 15.30 0 -2 5 298.77 16.10 0 2 6 121.19 7.60 0 2 -6 119.19 7.10 0 -2 6 141.89 7.80 0 -2 6 110.59 7.90 0 -2 -6 125.09 7.60 0 -2 6 108.19 7.50 0 2 7 296.77 17.70 0 2 -7 301.57 17.10 0 -2 7 301.27 18.20 0 -2 -7 303.37 17.60 0 -2 7 304.17 17.60 0 2 -8 11.30 1.80 0 2 8 11.80 2.30 0 -2 8 9.10 2.30 0 -2 8 9.40 2.20 0 2 9 66.39 6.00 0 2 9 69.49 5.20 0 -2 9 78.19 5.50 0 -2 -9 64.49 5.00 0 -2 9 72.29 6.10 0 2 10 230.08 14.00 0 2 10 216.68 14.50 0 -2 -10 227.18 13.80 0 -2 10 247.48 13.90 0 -2 -10 225.48 13.50 0 -2 10 221.38 14.60 0 2 11 0.50 2.90 0 2 11 -1.60 1.40 0 -2 -11 0.30 1.40 0 -2 11 1.00 2.50 0 -2 -11 1.00 1.30 0 -2 11 -0.50 2.40 0 2 12 14.20 3.20 0 2 12 14.80 2.50 0 2 -12 8.70 4.00 0 -2 -12 9.30 1.60 0 -2 12 9.70 2.70 0 -2 -12 10.20 2.50 0 2 13 176.18 13.40 0 2 13 229.98 13.10 0 2 13 239.68 12.90 0 -2 13 205.48 13.40 0 -2 -13 224.88 12.50 0 3 0 268.27 14.10 0 -3 0 220.58 14.30 0 -3 0 249.97 13.90 0 3 -1 228.58 13.80 0 3 -1 244.08 13.20 0 3 1 245.48 13.20 0 -3 1 206.68 13.50 0 -3 -1 237.18 13.10 0 -3 1 240.78 13.70 0 -3 1 212.98 13.20 0 -3 -1 228.08 13.60 0 3 -2 24.30 2.90 0 3 2 28.20 2.20 0 -3 2 30.00 2.10 0 -3 -2 32.70 3.40 0 -3 -2 34.20 2.60 0 -3 -2 30.90 2.10 0 -3 2 27.30 2.60 0 3 -3 1436.96 80.29 0 3 3 1437.06 79.89 0 3 -3 1510.75 79.89 0 -3 3 1386.36 80.19 0 -3 -3 1373.66 80.39 0 -3 3 1452.15 80.39 0 -3 3 1426.06 79.89 0 3 -4 142.39 8.00 0 3 4 133.39 8.00 0 -3 4 127.49 8.40 0 -3 4 132.19 8.70 0 -3 4 136.19 8.00 0 -3 -4 126.39 8.00 0 -3 -4 151.48 8.60 0 3 5 26.00 2.60 0 3 -5 28.50 2.10 0 -3 5 32.10 4.00 0 -3 -5 24.60 2.20 0 -3 -5 29.50 2.60 0 3 6 142.19 9.10 0 3 -6 152.78 8.60 0 -3 6 144.59 9.60 0 -3 -6 143.59 9.20 0 3 -7 310.17 17.40 0 3 7 286.47 17.90 0 -3 7 311.57 18.50 0 -3 -7 308.27 18.00 0 3 -8 7.10 1.30 0 3 8 5.00 1.50 0 -3 8 9.30 2.60 0 -3 -8 9.30 2.00 0 3 9 164.28 11.10 0 3 -9 198.18 16.90 0 -3 -9 180.48 11.30 0 -3 9 150.18 13.40 0 3 -10 360.46 23.90 0 3 10 336.97 22.10 0 3 10 377.36 21.80 0 -3 10 361.86 22.30 0 -3 -10 388.06 21.40 0 -3 -10 391.76 21.70 0 3 11 29.30 3.20 0 3 -11 23.00 6.60 0 3 11 34.80 5.40 0 -3 11 29.50 4.60 0 -3 -11 30.90 2.80 0 -3 -11 29.90 3.10 0 3 12 104.99 6.70 0 3 -12 90.19 9.40 0 -3 -12 101.39 6.60 0 -3 -12 105.09 6.30 0 -3 12 96.69 7.40 0 4 0 813.82 44.70 0 -4 0 771.22 45.20 0 -4 0 797.52 45.00 0 4 1 161.48 8.90 0 4 -1 155.38 8.90 0 -4 1 132.69 9.30 0 -4 1 161.08 9.50 0 -4 -1 130.39 9.20 0 4 2 87.19 5.20 0 4 -2 91.29 5.20 0 -4 2 77.49 6.10 0 -4 2 73.09 5.50 0 -4 -2 77.49 5.60 0 4 -3 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1.40 -2 -3 3 5.60 1.80 -2 -3 3 4.10 1.50 -2 3 2 1942.01 105.79 2 3 -2 2086.69 106.49 2 3 -2 1963.00 105.79 2 -3 -2 1906.41 105.79 -2 -3 2 1925.71 106.19 -2 -3 2 1918.91 106.29 -2 -3 2 1898.91 105.69 -2 -3 2 1854.31 106.09 2 -3 -2 1886.21 106.29 -2 -3 2 1604.84 105.99 2 3 -1 736.13 40.10 -2 3 1 709.23 40.20 -2 3 1 772.92 40.20 -2 -3 1 709.33 40.50 2 -3 -1 637.04 40.40 -2 -3 1 722.23 39.90 -2 -3 1 728.43 40.70 2 -3 -1 734.63 40.10 -2 -3 1 648.14 40.40 -2 -3 1 735.13 40.50 -2 -3 1 736.43 40.50 -2 3 0 0.60 0.70 2 3 0 2.20 0.70 -2 3 0 -1.10 1.70 -2 3 0 1.50 1.10 -2 -3 0 0.50 1.20 2 -3 0 2.10 0.80 2 -3 0 0.70 0.50 -2 -3 0 1.20 0.40 -2 -3 0 0.30 1.60 -2 -3 0 0.70 1.10 -2 -3 0 1.60 1.10 -2 3 -1 761.72 40.90 2 3 1 739.83 40.90 -2 3 -1 685.53 41.00 -2 3 -1 752.82 41.40 -2 -3 -1 783.12 41.30 -2 -3 -1 769.72 41.20 2 -3 1 715.43 40.80 -2 -3 -1 680.93 41.20 -2 -3 -1 721.83 40.70 -2 -3 -1 685.43 41.40 -2 3 -2 915.01 48.50 -2 3 -2 839.72 48.60 2 3 2 834.72 48.30 -2 -3 -2 945.91 48.80 -2 -3 -2 889.11 48.90 -2 -3 -2 813.62 48.90 2 -3 2 825.02 48.40 -2 -3 -2 854.61 49.00 2 3 3 0.10 0.90 -2 3 -3 2.60 0.70 -2 3 -3 5.20 2.60 -2 -3 -3 0.30 1.50 2 -3 3 3.00 0.80 -2 -3 -3 1.70 0.90 2 -3 3 3.10 1.30 -2 -3 -3 0.10 1.40 2 -3 3 1.10 2.20 -2 3 -4 2899.51 163.08 -2 3 -4 3209.78 164.98 -2 -3 -4 3315.87 165.48 -2 -3 -4 2783.12 163.48 2 -3 4 2754.32 163.48 -2 -3 -4 3015.80 163.58 -2 -3 -4 2531.85 163.18 -2 3 -5 2.90 0.90 -2 3 -5 1.20 2.30 -2 -3 -5 5.10 4.50 -2 -3 -5 0.10 1.60 2 -3 5 5.30 2.20 -2 -3 -5 2.20 1.00 -2 -3 -5 2.70 0.90 -2 3 -6 168.48 9.80 2 3 6 163.58 10.20 -2 3 -6 162.48 12.20 -2 -3 -6 157.88 10.00 2 -3 6 160.98 10.90 -2 -3 -6 179.48 13.50 -2 -3 -6 175.38 10.40 -2 3 -7 35.70 6.30 2 3 7 34.80 3.30 -2 3 -7 35.40 2.80 2 -3 7 35.40 4.60 -2 -3 -7 33.10 3.10 2 3 8 476.05 27.80 -2 3 -8 480.65 30.10 -2 -3 -8 493.05 27.80 2 -3 8 448.06 28.10 -2 -3 -8 493.95 27.40 2 3 9 9.40 2.00 -2 -3 -9 9.10 2.00 2 -3 9 2.90 2.90 -2 -3 -9 11.00 2.00 2 3 10 162.88 9.90 2 3 10 148.89 10.60 -2 3 -10 143.89 12.60 2 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4 176.68 11.00 -2 -4 4 173.48 11.00 -2 4 3 11.30 1.60 2 4 -3 8.40 1.30 -2 -4 3 10.60 2.30 2 -4 -3 11.80 2.20 -2 -4 3 13.60 2.80 -2 4 2 567.54 31.60 2 4 -2 584.14 31.60 -2 -4 2 581.54 32.20 2 -4 -2 525.85 32.20 -2 -4 2 530.75 32.00 -2 -4 2 561.24 32.10 -2 4 1 -0.30 0.80 2 4 -1 -0.10 0.70 -2 -4 1 2.30 2.70 -2 -4 1 1.00 1.50 -2 -4 1 -0.10 1.30 2 -4 -1 -0.50 1.00 2 4 0 56.29 3.50 -2 4 0 51.29 3.60 -2 -4 0 53.49 4.40 -2 -4 0 48.90 3.90 -2 -4 0 51.99 4.50 2 -4 0 44.60 3.90 2 4 1 1200.78 67.59 -2 4 -1 1237.08 67.69 2 -4 1 1075.79 68.09 -2 -4 -1 1188.68 68.19 -2 -4 -1 1343.27 68.19 2 4 2 388.66 22.20 -2 4 -2 393.76 22.30 2 -4 2 357.56 22.80 -2 -4 -2 394.06 22.80 -2 -4 -2 422.86 23.00 -2 4 -3 327.87 19.30 -2 4 -3 293.07 16.90 2 4 3 282.27 16.80 -2 -4 -3 305.67 17.70 -2 -4 -3 286.37 17.40 2 -4 3 267.07 17.40 -2 4 -4 312.07 19.40 -2 4 -4 366.36 21.90 -2 -4 -4 373.06 23.00 -2 -4 -4 309.97 19.90 -2 4 -5 34.30 6.90 -2 4 -5 37.30 3.00 2 -4 5 29.20 5.20 -2 -4 -5 44.60 10.10 -2 -4 -5 43.30 3.50 -2 -4 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237.08 14.10 -16 -1 0 241.58 14.30 -16 -1 0 232.58 14.70 -16 -1 0 259.17 14.50 -16 1 -1 129.29 10.90 -16 1 -1 152.28 9.10 -16 -1 -1 148.79 9.20 -16 -1 -1 167.68 9.40 -16 -1 -1 144.49 10.00 -16 1 -2 127.59 7.90 -16 1 -2 110.19 10.00 -16 -1 -2 144.79 8.20 -16 -1 -2 131.09 8.10 -16 -1 -2 118.39 8.90 -16 1 -3 12.60 3.90 -16 1 -3 12.20 2.10 -16 -1 -3 8.10 2.80 -16 -1 -3 16.80 3.10 -16 1 -4 3.60 1.40 -16 1 -4 2.60 4.00 -16 -1 -4 -2.30 2.40 -16 -1 -4 -0.10 1.80 -16 -1 -4 4.20 2.90 -16 1 -5 2.50 4.20 -16 1 -5 1.70 1.40 -16 -1 -5 -0.80 1.80 -16 -1 -5 -3.70 3.00 -16 1 -6 25.50 2.70 -16 -1 -6 27.10 3.20 -16 -1 -6 25.70 4.80 -16 1 -7 39.10 3.10 -16 1 -7 27.80 8.50 -16 -1 -7 40.30 3.20 -16 -1 -7 31.70 5.20 16 2 -7 22.70 1.90 -16 2 7 23.40 3.00 -16 2 7 20.70 2.60 -16 -2 7 24.70 2.50 -16 -2 7 25.60 2.80 16 2 -6 9.10 1.50 -16 2 6 6.00 1.90 -16 2 6 7.20 1.60 -16 -2 6 10.10 1.50 -16 2 5 425.06 23.00 16 2 -5 372.16 22.40 -16 -2 5 385.36 22.90 -16 -2 5 394.16 22.80 16 2 -4 2.10 1.10 -16 2 4 2.50 2.70 -16 2 4 2.20 1.40 -16 -2 4 2.70 1.30 -16 -2 4 1.60 2.40 16 2 -3 93.89 6.00 -16 2 3 103.49 6.50 -16 2 3 92.39 8.30 -16 2 3 94.29 6.30 -16 -2 3 96.09 6.60 -16 -2 3 95.89 6.50 -16 -2 3 101.79 7.00 -16 2 2 40.70 5.60 -16 2 2 50.79 3.80 -16 2 2 42.50 3.70 -16 -2 2 41.00 3.50 -16 -2 2 44.80 4.50 -16 -2 2 43.00 3.80 -16 2 1 61.59 7.10 -16 2 1 85.39 5.30 -16 2 1 80.89 5.20 -16 -2 1 75.79 5.40 -16 -2 1 72.79 5.30 -16 -2 1 68.29 5.80 -16 2 0 -3.40 2.50 -16 2 0 -0.20 1.30 -16 -2 0 2.10 1.40 -16 -2 0 0.80 1.40 -16 -2 0 -1.10 2.20 -16 2 -1 88.49 8.70 -16 2 -1 105.69 6.70 -16 -2 -1 106.29 6.80 -16 -2 -1 113.09 6.90 -16 -2 -1 94.29 7.30 -16 2 -2 217.08 15.60 -16 2 -2 235.08 13.50 -16 -2 -2 203.98 14.00 -16 -2 -2 246.18 13.70 -16 -2 -2 223.58 13.60 -16 2 -3 244.38 18.20 -16 2 -3 307.37 16.60 -16 -2 -3 298.97 16.70 -16 -2 -3 272.07 17.20 -16 -2 -3 283.17 16.70 -16 2 -4 1.30 1.40 -16 -2 -4 4.00 2.80 -16 -2 -4 -0.40 2.10 -16 2 -5 175.38 12.50 -16 -2 -5 177.98 11.50 -16 -2 -5 183.18 11.60 -16 -2 -6 4.40 3.20 -16 -2 -6 6.10 3.10 -16 3 5 21.90 2.70 16 3 -5 30.40 2.50 -16 -3 5 29.60 2.80 -16 -3 5 25.50 3.00 -16 -3 5 30.70 3.60 -16 3 4 4.40 3.80 16 3 -4 3.80 1.50 -16 3 4 7.70 1.60 -16 -3 4 4.60 2.20 -16 -3 4 6.50 1.70 -16 -3 4 6.80 1.50 -16 3 3 88.69 8.70 -16 3 3 109.69 6.90 -16 -3 3 112.59 7.50 -16 -3 3 112.29 6.90 -16 -3 3 108.49 7.10 -16 3 2 183.98 10.50 -16 3 2 180.88 10.50 -16 3 2 153.68 12.30 -16 -3 2 171.18 10.70 -16 -3 2 166.58 10.90 -16 -3 2 172.48 10.50 -16 3 1 7.90 3.00 -16 3 1 10.10 1.80 -16 -3 1 10.30 1.90 -16 -3 1 13.00 2.40 -16 -3 1 8.30 1.70 -16 3 0 40.10 5.90 -16 3 0 42.20 3.60 -16 -3 0 47.60 3.90 -16 -3 0 41.70 4.30 -16 -3 0 41.30 3.70 -16 3 -1 107.19 9.90 -16 3 -1 134.59 8.00 -16 -3 -1 124.29 8.60 -16 -3 -1 117.89 8.00 -16 -3 -1 138.29 8.30 -16 3 -2 126.39 11.20 -16 3 -2 169.18 9.40 -16 -3 -2 141.39 10.00 -16 -3 -2 171.88 9.70 -16 -3 -2 148.09 9.50 -16 3 -3 37.20 3.50 -16 3 -3 25.80 5.70 -16 -3 -3 22.30 4.20 -16 -3 -3 30.90 3.70 -16 -3 -3 28.90 4.30 -16 3 -4 131.09 10.60 -16 -3 -4 154.98 9.20 -16 -3 -4 147.09 9.60 -17 0 7 -0.40 1.20 -17 0 7 -0.10 1.30 -17 0 6 67.39 4.90 -17 0 6 71.59 4.90 -17 0 5 1.40 1.20 -17 0 5 -2.50 1.40 -17 0 3 -0.70 1.20 -17 0 3 0.40 1.30 -17 0 2 174.48 10.00 -17 0 2 164.98 9.80 -17 0 2 139.99 12.30 -17 0 1 -0.50 1.50 -17 0 1 1.60 1.30 -17 0 0 79.29 8.50 -17 0 0 85.49 5.90 -17 0 0 100.89 6.10 -17 0 -1 -1.10 3.80 -17 0 -1 1.10 1.90 -17 0 -1 0.20 1.60 -17 0 -2 97.39 6.00 -17 0 -2 80.49 8.50 -17 0 -3 1.00 1.70 -17 0 -3 -5.70 4.20 -17 0 -4 70.39 7.30 -17 0 -4 67.59 4.80 -17 0 -5 2.20 4.70 -17 0 -6 -1.20 4.70 -17 1 6 21.60 2.60 -17 1 6 22.50 3.10 -17 -1 6 22.40 2.70 -17 1 5 107.59 6.90 -17 1 5 98.19 6.80 -17 -1 5 106.89 6.90 -17 -1 5 106.29 6.80 -17 1 4 89.69 5.80 -17 1 4 79.29 5.70 -17 -1 4 82.59 5.70 -17 -1 4 87.79 5.90 -17 1 3 1.00 1.50 -17 1 3 -0.20 1.30 -17 1 3 3.30 2.70 -17 -1 3 1.30 1.30 -17 -1 3 0.20 1.30 -17 -1 3 7.80 4.60 -17 1 2 142.39 10.30 -17 1 2 140.69 11.80 -17 1 2 173.78 10.00 -17 -1 2 191.78 14.00 -17 -1 2 157.58 9.90 -17 -1 2 173.58 10.20 -17 1 1 23.60 5.20 -17 1 1 24.90 2.80 -17 1 1 27.10 2.90 -17 -1 1 24.50 2.70 -17 -1 1 23.20 3.60 -17 -1 1 26.50 2.80 -17 1 0 13.00 1.90 -17 1 0 7.70 3.20 -17 1 0 9.50 1.80 -17 -1 0 15.90 2.40 -17 -1 0 13.60 2.30 -17 -1 0 8.70 3.20 -17 1 -1 385.66 21.40 -17 1 -1 326.47 23.00 -17 -1 -1 357.16 22.10 -17 -1 -1 418.26 21.70 -17 -1 -1 365.36 21.50 -17 1 -2 142.49 8.20 -17 -1 -2 135.19 8.30 -17 -1 -2 119.49 8.30 -17 -1 -2 121.69 9.00 -17 1 -3 42.80 6.70 -17 -1 -3 52.19 4.50 -17 -1 -3 46.10 5.30 -17 1 -4 130.39 7.10 -17 1 -4 93.79 9.40 -17 -1 -4 106.69 8.10 -17 1 -5 134.29 10.70 -17 -1 -5 157.48 10.80 -17 1 -6 5.90 1.50 -17 -1 -6 7.80 3.70 -17 -1 -6 2.10 2.00 17 2 -5 503.05 30.80 -17 2 5 599.24 31.40 -17 -2 5 552.74 31.30 -17 -2 5 537.65 31.30 17 2 -4 83.39 5.80 -17 2 4 106.29 6.40 -17 -2 4 93.69 6.20 -17 -2 4 93.99 6.30 -17 2 3 0.30 1.40 -17 -2 3 2.50 1.30 -17 -2 3 -2.20 1.30 -17 2 2 34.00 5.90 -17 2 2 43.30 3.50 -17 2 2 39.70 3.50 -17 -2 2 36.10 3.40 -17 -2 2 34.00 3.20 -17 -2 2 40.50 4.40 -17 2 1 339.27 18.70 -17 2 1 278.97 20.30 -17 2 1 347.47 18.70 -17 -2 1 349.77 19.00 -17 -2 1 301.77 19.20 -17 -2 1 307.37 18.70 -17 2 0 1.10 1.60 -17 2 0 2.40 2.80 -17 -2 0 4.00 1.60 -17 -2 0 4.60 2.50 -17 -2 0 4.70 1.50 -17 2 -1 146.19 12.00 -17 2 -1 184.28 10.40 -17 -2 -1 162.98 11.00 -17 -2 -1 171.48 10.50 -17 -2 -1 187.08 10.60 -17 2 -2 73.79 4.90 -17 -2 -2 61.69 5.80 -17 -2 -2 75.19 5.20 -17 -2 -2 66.79 5.10 -17 2 -3 9.40 1.70 -17 -2 -3 10.50 2.60 -17 -2 -3 4.60 2.70 -17 -2 -3 7.50 2.20 -17 2 -4 7.80 3.80 -17 2 -4 4.30 1.60 -17 -2 -4 -2.50 2.40 -17 -2 -4 1.70 2.80 -17 2 -5 60.89 6.80 -17 -2 -5 52.49 5.30 -17 3 3 0.70 3.40 -17 3 3 4.30 1.80 -17 -3 3 3.00 2.40 -17 -3 3 4.80 1.70 -17 -3 3 6.70 1.50 -17 3 2 113.19 9.80 -17 3 2 142.09 7.90 -17 -3 2 118.09 7.80 -17 -3 2 136.59 8.20 -17 -3 2 117.69 8.20 -17 3 1 30.70 5.90 -17 3 1 24.10 2.80 -17 -3 1 25.30 2.70 -17 -3 1 25.80 3.80 -17 3 0 -0.60 1.60 -17 3 0 3.20 3.20 -17 -3 0 5.70 2.40 -17 -3 0 2.40 1.70 -17 -3 0 0.60 1.50 -17 3 -1 0.10 3.00 -17 -3 -1 -0.30 1.50 -17 -3 -1 -3.10 2.40 -17 -3 -1 -2.80 1.80 -17 3 -2 46.60 6.20 -17 -3 -2 48.40 4.00 -17 -3 -2 47.80 4.80 -17 -3 -2 58.99 4.40 -18 0 5 -0.90 1.30 -18 0 4 75.49 13.40 -18 0 4 92.79 6.80 -18 0 4 105.79 6.30 -18 0 3 1.10 1.30 -18 0 3 -0.60 1.40 -18 0 2 37.30 3.40 -18 0 2 40.40 3.40 -18 0 1 -2.20 4.10 -18 0 1 3.70 1.60 -18 0 1 -0.60 1.40 -18 0 0 49.99 3.90 -18 0 0 42.60 4.00 -18 0 -1 2.40 4.20 -18 0 -3 1.00 2.20 -18 0 -4 1.60 1.90 -18 0 -5 -1.50 1.80 -18 1 5 0.60 1.60 -18 1 5 0.50 1.30 -18 -1 5 0.60 1.30 -18 -1 5 0.40 1.30 -18 1 4 177.98 11.40 -18 1 4 208.88 12.30 -18 -1 4 174.58 12.00 -18 -1 4 207.58 14.90 -18 1 3 139.19 8.60 -18 -1 3 130.49 8.50 -18 -1 3 144.69 8.70 -18 1 2 26.20 2.60 -18 -1 2 24.90 2.70 -18 -1 2 21.50 2.60 -18 1 1 55.09 4.10 -18 -1 1 51.69 4.00 -18 -1 1 52.69 4.00 -18 1 0 5.20 3.60 -18 -1 0 3.30 1.60 -18 -1 0 2.40 1.60 -18 1 -1 5.10 3.10 -18 1 -1 3.70 3.70 -18 -1 -1 9.30 2.10 -18 -1 -1 5.30 2.00 -18 -1 -1 11.10 5.40 -18 1 -2 9.00 4.40 -18 1 -2 9.20 3.20 -18 -1 -2 15.30 3.90 -18 -1 -2 7.40 2.40 -18 1 -3 63.79 7.30 -18 -1 -3 68.19 6.40 -18 1 -4 1.70 4.40 -18 1 -4 6.00 1.70 -18 -1 -4 2.20 3.70 -18 -2 4 52.39 3.80 -18 2 3 35.20 7.00 -18 2 3 33.10 3.10 -18 -2 3 30.90 3.10 -18 -2 3 29.90 2.90 -18 2 2 6.80 1.70 -18 -2 2 4.10 1.40 -18 -2 2 4.90 3.20 -18 -2 2 3.70 1.50 -18 2 1 398.76 22.40 -18 -2 1 345.87 22.80 -18 -2 1 432.16 23.80 -18 -2 1 385.56 22.70 -18 2 0 2.80 1.80 -18 -2 0 -1.60 1.60 -18 -2 0 1.40 1.60 -18 -2 0 2.10 3.00 -18 2 -1 29.30 5.90 -18 2 -1 26.60 3.10 -18 -2 -1 30.50 3.10 -18 -2 -1 20.20 4.40 -18 -2 -1 34.30 3.30 -18 2 -2 -0.80 3.50 -18 2 -2 4.10 1.60 -18 -2 -2 8.90 2.80 -18 -2 -2 6.00 2.10 -18 -2 -2 9.40 2.40 -18 -2 -3 123.39 7.70 -18 -2 -3 112.29 8.10 -19 0 2 16.20 2.90 -19 0 1 -1.30 1.60 -19 0 0 574.64 32.70 -19 1 3 353.56 19.90 -19 1 3 384.26 24.70 -19 -1 3 337.77 20.00 -19 -1 3 311.57 19.80 -19 1 2 12.70 6.00 -19 1 2 -0.30 1.60 -19 -1 2 0.70 1.50 -19 1 1 90.39 5.40 -19 1 1 61.69 7.50 -19 -1 1 83.29 5.30 -19 -1 1 69.19 5.10 -19 1 0 18.20 4.10 -19 -1 0 18.30 3.00 -19 1 -1 9.20 4.20 -19 -1 -1 13.10 2.40 -19 -1 -1 14.90 2.50 -19 1 -2 65.99 4.70 -19 1 -2 44.50 7.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 52438 _shelx_shelxl_version_number 2016/6 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.39667(2) 0.13906(6) 0.40522(3) 0.02477(13) Uani 1 1 d . . . . . O1 O 0.500000 0.2942(3) 0.750000 0.0258(3) Uani 1 2 d S T P . . N1 N 0.39114(7) 0.6341(2) 0.58414(11) 0.0231(2) Uani 1 1 d . . . . . C1 C 0.29808(8) 0.6644(2) 0.62492(12) 0.0217(3) Uani 1 1 d . . . . . C2 C 0.26464(8) 0.4090(2) 0.68046(12) 0.0226(3) Uani 1 1 d . . . . . C3 C 0.18233(8) 0.4521(2) 0.75697(12) 0.0220(3) Uani 1 1 d . . . . . C4 C 0.14686(8) 0.1951(2) 0.81023(12) 0.0213(3) Uani 1 1 d . . . . . C5 C 0.07297(8) 0.2368(2) 0.90200(11) 0.0218(3) Uani 1 1 d . . . . . C6 C 0.03713(8) -0.0204(2) 0.95416(12) 0.0227(3) Uani 1 1 d . . . . . H1A H 0.4262(12) 0.600(3) 0.6438(17) 0.033(4) Uiso 1 1 d . . . . . H2A H 0.3111(11) 0.334(3) 0.7323(15) 0.027(4) Uiso 1 1 d . . . . . H4A H 0.1953(10) 0.101(3) 0.8536(14) 0.025(4) Uiso 1 1 d . . . . . H5A H 0.0245(11) 0.333(3) 0.8590(15) 0.025(4) Uiso 1 1 d . . . . . H6A H 0.0862(10) -0.114(3) 0.9978(14) 0.023(4) Uiso 1 1 d . . . . . H5B H 0.0961(11) 0.346(3) 0.9706(16) 0.029(4) Uiso 1 1 d . . . . . H6B H 0.0138(11) -0.130(3) 0.8831(15) 0.026(4) Uiso 1 1 d . . . . . H4B H 0.1241(10) 0.082(3) 0.7426(15) 0.027(4) Uiso 1 1 d . . . . . H3A H 0.1987(11) 0.570(4) 0.8279(16) 0.031(4) Uiso 1 1 d . . . . . H3B H 0.1353(11) 0.538(3) 0.7055(15) 0.030(4) Uiso 1 1 d . . . . . H1B H 0.4101(12) 0.782(4) 0.5465(16) 0.037(4) Uiso 1 1 d . . . . . H1D H 0.2982(11) 0.810(3) 0.6875(15) 0.029(4) Uiso 1 1 d . . . . . H1E H 0.2638(10) 0.717(3) 0.5527(15) 0.025(4) Uiso 1 1 d . . . . . H1C H 0.3943(12) 0.495(4) 0.5244(17) 0.040(5) Uiso 1 1 d . . . . . H2B H 0.2531(11) 0.282(4) 0.6161(16) 0.032(4) Uiso 1 1 d . . . . . H1 H 0.4698(14) 0.189(4) 0.798(2) 0.059(6) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.02649(19) 0.01943(18) 0.02896(19) 0.00100(10) 0.01037(12) 0.00043(10) O1 0.0260(6) 0.0211(6) 0.0310(7) 0.000 0.0119(5) 0.000 N1 0.0213(5) 0.0208(5) 0.0277(6) 0.0032(4) 0.0101(4) -0.0034(4) C1 0.0208(6) 0.0174(5) 0.0274(6) 0.0018(4) 0.0102(5) -0.0013(4) C2 0.0226(6) 0.0165(5) 0.0295(6) 0.0010(5) 0.0126(5) -0.0013(4) C3 0.0218(6) 0.0171(6) 0.0276(6) 0.0015(5) 0.0117(5) -0.0008(4) C4 0.0217(6) 0.0168(5) 0.0259(6) 0.0006(5) 0.0114(5) -0.0016(4) C5 0.0227(6) 0.0177(6) 0.0257(6) 0.0013(5) 0.0115(5) -0.0009(4) C6 0.0232(6) 0.0181(6) 0.0275(6) 0.0021(5) 0.0128(5) -0.0004(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0140 0.0070 '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 0.3280 0.5430 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0250 0.0140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0390 0.0250 '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 H1 O1 H1 105(3) . 2_656 C1 N1 H1A 112.2(12) . . C1 N1 H1B 111.1(11) . . C1 N1 H1C 109.8(11) . . H1A N1 H1B 108.1(17) . . H1A N1 H1C 108.7(16) . . H1B N1 H1C 106.9(16) . . N1 C1 C2 110.75(10) . . N1 C1 H1D 106.9(10) . . N1 C1 H1E 106.5(9) . . C2 C1 H1D 111.3(10) . . C2 C1 H1E 112.1(10) . . H1D C1 H1E 109.1(14) . . C1 C2 C3 111.99(10) . . C1 C2 H2A 108.6(9) . . C1 C2 H2B 110.4(10) . . C3 C2 H2A 109.8(10) . . C3 C2 H2B 110.5(10) . . H2A C2 H2B 105.2(14) . . C2 C3 C4 112.30(10) . . C2 C3 H3A 108.0(10) . . C2 C3 H3B 110.3(9) . . C4 C3 H3A 108.2(10) . . C4 C3 H3B 109.3(10) . . H3A C3 H3B 108.6(14) . . C3 C4 H4A 109.1(9) . . C3 C4 H4B 110.0(9) . . C5 C4 C3 113.24(10) . . C5 C4 H4A 108.2(9) . . C5 C4 H4B 108.2(9) . . H4A C4 H4B 107.9(13) . . C4 C5 C6 113.10(10) . . C4 C5 H5A 108.4(9) . . C4 C5 H5B 108.2(10) . . C6 C5 H5A 109.3(9) . . C6 C5 H5B 109.5(10) . . H5A C5 H5B 108.2(13) . . C5 C6 C6 113.27(12) . 3_557 C5 C6 H6A 108.4(9) . . C5 C6 H6B 108.6(9) . . C6 C6 H6A 108.5(9) 3_557 . C6 C6 H6B 108.5(9) 3_557 . H6A C6 H6B 109.7(13) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O1 H1 0.87(2) . O1 H1 0.87(2) 2_656 N1 C1 1.4925(15) . N1 H1A 0.835(19) . N1 H1B 0.90(2) . N1 H1C 0.95(2) . C1 C2 1.5188(16) . C1 H1D 0.999(17) . C1 H1E 0.956(16) . C2 C3 1.5255(15) . C2 H2A 0.960(17) . C2 H2B 0.957(18) . C3 C4 1.5270(16) . C3 H3A 0.994(18) . C3 H3B 0.988(17) . C4 C5 1.5243(15) . C4 H4A 0.979(16) . C4 H4B 0.978(17) . C5 C6 1.5257(16) . C5 H5A 0.983(17) . C5 H5B 0.978(17) . C6 C6 1.527(2) 3_557 C6 H6A 0.986(16) . C6 H6B 0.999(17) . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O1 0.835(19) 2.208(19) 2.9433(14) 146.8(16) . N1 H1B Cl1 0.90(2) 2.37(2) 3.2029(11) 154.2(15) 1_565 N1 H1B Cl1 0.90(2) 2.976(18) 3.4042(11) 110.9(13) 3_666 C1 H1D Cl1 0.999(17) 2.742(16) 3.4595(14) 129.1(12) 4_566 N1 H1C Cl1 0.95(2) 2.22(2) 3.1631(12) 172.7(16) . O1 H1 Cl1 0.87(2) 2.32(2) 3.1928(10) 172(2) 4_556 _cod_database_fobs_code 3500069