#------------------------------------------------------------------------------ #$Date: 2016-03-03 14:43:15 +0000 (Thu, 03 Mar 2016) $ #$Revision: 177181 $ #$URL: svn://www.crystallography.net/cod/cif/3/50/00/3500030.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_3500030 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. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _publ_section_title ; Benzyltriethylammonium chloride ; _journal_name_full 'Personal communication to COD' _journal_year 2016 _chemical_absolute_configuration ad _chemical_formula_moiety 'C13 H22 N, Cl' _chemical_formula_sum 'C13 H22 Cl N' _chemical_formula_weight 227.76 _chemical_name_common 'Benzyltriethylammonium chloride' _chemical_name_systematic 'Benzenemethanaminium, N,N,N-triethyl-, chloride (1:1)' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_date 2015-12-03 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.9943(5) _cell_length_b 12.4491(9) _cell_length_c 12.9791(9) _cell_measurement_reflns_used 9908 _cell_measurement_temperature 100 _cell_measurement_theta_max 60.615 _cell_measurement_theta_min 4.814 _cell_volume 1291.70(15) _computing_cell_refinement ; SAINT (2013) V8.35A; 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) V8.35A; 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 'XL (Sheldrick, 2008)' _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 0.992 _diffrn_measured_fraction_theta_max 0.994 _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 0.0318 _diffrn_reflns_av_unetI/netI 0.0234 _diffrn_reflns_laue_measured_fraction_full 0.992 _diffrn_reflns_laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 13567 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 60.569 _diffrn_reflns_theta_min 5.655 _diffrn_source 'Metal Jet' _diffrn_source_target Ga _diffrn_source_type 'Gallium Liquid Metal Jet Source' _exptl_absorpt_coefficient_mu 1.536 _exptl_absorpt_correction_T_max 0.7519 _exptl_absorpt_correction_T_min 0.6394 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0641 before and 0.0449 after correction. The Ratio of minimum to maximum transmission is 0.8504. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.171 _exptl_crystal_description Block _exptl_crystal_F_000 496 _exptl_crystal_preparation 'from commercial source' _exptl_crystal_recrystallization_method 'extracted from the bottle' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _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 0.375 _refine_diff_density_min -0.193 _refine_diff_density_rms 0.061 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.15(2) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 140 _refine_ls_number_reflns 2943 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.102 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0336 _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^)+(0.0520P)^2^+0.2927P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0868 _refine_ls_wR_factor_ref 0.0872 _refine_special_details ; Refined as a 2-component inversion twin. ; _reflns_Friedel_coverage 0.732 _reflns_friedel_fraction_full 0.997 _reflns_friedel_fraction_max 0.998 _reflns_number_gt 2906 _reflns_number_total 2943 _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 PhNEt3C.cif _cod_data_source_block phnet3c _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 4287 2015-11-16 14:04:37Z antanas ; _cod_database_code 3500030 _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 0.729 _shelx_estimated_absorpt_t_min 0.673 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.85(2) 0.15(2) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C8(H8A,H8B), C10(H10A,H10B), C12(H12A,H12B) 3.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C7(H7) 3.c Idealised Me refined as rotating group: C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C) ; _shelx_res_file ; phnet3c.res created by SHELXL-2014/7 TITL phnet3c_a.res in P2(1)2(1)2(1) REM Old TITL PhNEt3C in P212121 #19 REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.109, Rweak 0.027, Alpha 0.003, Orientation as input REM Flack x = 0.234 ( 0.004 ) from Parsons' quotients REM Formula found by SHELXT: C13 N Cl CELL 1.34139 7.9943 12.4491 12.9791 90 90 90 ZERR 4 0.0005 0.0009 0.0009 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Cl N DISP C 0.014 0.007 57.748 DISP Cl 0.329 0.54 4086.178 DISP H -0 0 0.648 DISP N 0.025 0.014 110.512 UNIT 52 88 4 4 L.S. 30 PLAN 20 SIZE 0.22 0.26 0.28 TEMP -173 BOND $H LIST 4 ACTA fmap 2 MORE -1 CONF TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.052000 0.292700 BASF 0.14823 FVAR 1.43927 N1 4 0.593164 0.362063 0.622372 11.00000 0.01468 0.02352 = 0.01927 0.00282 0.00093 0.00034 C1 1 0.431319 0.362254 0.558416 11.00000 0.01569 0.02254 = 0.01916 -0.00070 -0.00138 0.00000 AFIX 23 H1A 2 0.456673 0.330221 0.490370 11.00000 -1.20000 H1B 2 0.349787 0.314430 0.592942 11.00000 -1.20000 AFIX 0 C2 1 0.347847 0.468945 0.540528 11.00000 0.01623 0.02184 = 0.02093 -0.00032 -0.00261 -0.00140 C3 1 0.377389 0.524932 0.448993 11.00000 0.02380 0.02840 = 0.02141 0.00301 -0.00262 -0.00231 AFIX 43 H3 2 0.451852 0.496196 0.399051 11.00000 -1.20000 AFIX 0 C4 1 0.297982 0.622808 0.430693 11.00000 0.03332 0.02912 = 0.02978 0.00882 -0.01014 -0.00506 AFIX 43 H4 2 0.319784 0.661535 0.369071 11.00000 -1.20000 AFIX 0 C5 1 0.186633 0.663362 0.503269 11.00000 0.02923 0.02141 = 0.04627 0.00005 -0.01418 0.00306 AFIX 43 H5 2 0.132933 0.730230 0.491029 11.00000 -1.20000 AFIX 0 C6 1 0.153014 0.607273 0.593414 11.00000 0.02048 0.02700 = 0.03489 -0.00650 -0.00437 0.00243 AFIX 43 H6 2 0.076497 0.635350 0.642515 11.00000 -1.20000 AFIX 0 C7 1 0.232735 0.509239 0.611184 11.00000 0.01575 0.02506 = 0.02337 -0.00044 -0.00109 -0.00131 AFIX 43 H7 2 0.208271 0.469705 0.671950 11.00000 -1.20000 AFIX 0 C8 1 0.724893 0.434944 0.573483 11.00000 0.01702 0.03786 = 0.02682 0.00452 0.00161 -0.00687 AFIX 23 H8A 2 0.836754 0.409575 0.595367 11.00000 -1.20000 H8B 2 0.718374 0.426617 0.497732 11.00000 -1.20000 AFIX 0 C9 1 0.711098 0.553291 0.598833 11.00000 0.03046 0.03582 = 0.03034 0.00155 -0.00504 -0.01245 AFIX 137 H9A 2 0.790525 0.593916 0.556531 11.00000 -1.50000 H9B 2 0.736722 0.564471 0.671888 11.00000 -1.50000 H9C 2 0.597116 0.578109 0.584493 11.00000 -1.50000 AFIX 0 C10 1 0.554184 0.391743 0.732085 11.00000 0.02773 0.02870 = 0.01698 -0.00007 0.00000 0.00231 AFIX 23 H10A 2 0.466661 0.342724 0.758567 11.00000 -1.20000 H10B 2 0.508412 0.465618 0.733610 11.00000 -1.20000 AFIX 0 C11 1 0.705886 0.386192 0.803215 11.00000 0.04155 0.04760 = 0.02590 0.00254 -0.01170 0.00210 AFIX 137 H11A 2 0.790798 0.437447 0.779786 11.00000 -1.50000 H11B 2 0.752485 0.313394 0.801879 11.00000 -1.50000 H11C 2 0.671817 0.404169 0.873667 11.00000 -1.50000 AFIX 0 C12 1 0.662506 0.247941 0.614305 11.00000 0.01929 0.02880 = 0.03326 0.00166 0.00272 0.00777 AFIX 23 H12A 2 0.671765 0.228926 0.540461 11.00000 -1.20000 H12B 2 0.776894 0.247348 0.643523 11.00000 -1.20000 AFIX 0 C13 1 0.560726 0.162025 0.667821 11.00000 0.02954 0.02561 = 0.04539 0.00662 0.00339 0.00740 AFIX 137 H13A 2 0.444462 0.165673 0.644139 11.00000 -1.50000 H13B 2 0.564608 0.173559 0.742474 11.00000 -1.50000 H13C 2 0.607172 0.091184 0.651518 11.00000 -1.50000 AFIX 0 CL1 3 0.102427 0.219497 0.685754 11.00000 0.01916 0.03760 = 0.01926 0.00085 -0.00007 -0.00432 HKLF 4 REM phnet3c_a.res in P2(1)2(1)2(1) REM R1 = 0.0336 for 2906 Fo > 4sig(Fo) and 0.0341 for all 2943 data REM 140 parameters refined using 0 restraints END WGHT 0.0519 0.2939 REM Highest difference peak 0.375, deepest hole -0.193, 1-sigma level 0.061 Q1 1 0.8219 0.4330 0.5151 11.00000 0.05 0.38 Q2 1 0.6342 0.3989 0.8457 11.00000 0.05 0.31 Q3 1 0.1961 0.6408 0.5580 11.00000 0.05 0.31 Q4 1 0.7179 0.4758 0.6175 11.00000 0.05 0.29 Q5 1 0.6407 0.3912 0.7615 11.00000 0.05 0.29 Q6 1 0.3825 0.4197 0.5491 11.00000 0.05 0.29 Q7 1 0.0643 0.1641 0.6952 11.00000 0.05 0.28 Q8 1 0.1652 0.6275 0.5462 11.00000 0.05 0.28 Q9 1 0.1989 0.5543 0.5998 11.00000 0.05 0.28 Q10 1 0.1680 0.1763 0.7015 11.00000 0.05 0.27 Q11 1 0.2761 0.4801 0.5688 11.00000 0.05 0.26 Q12 1 0.5802 0.3808 0.6756 11.00000 0.05 0.23 Q13 1 0.3342 0.4915 0.4942 11.00000 0.05 0.23 Q14 1 0.1568 0.2189 0.6237 11.00000 0.05 0.22 Q15 1 0.3780 0.5785 0.4536 11.00000 0.05 0.22 Q16 1 0.6056 0.1952 0.6402 11.00000 0.05 0.22 Q17 1 0.2759 0.6572 0.4821 11.00000 0.05 0.22 Q18 1 0.0638 0.2434 0.7310 11.00000 0.05 0.20 Q19 1 0.1645 0.6905 0.5036 11.00000 0.05 0.18 Q20 1 -0.0205 0.2403 0.6949 11.00000 0.05 0.18 ; _shelx_res_checksum 30284 _shelx_hkl_file ; 0 1 0 0.50 0.20 0 1 0 0.30 0.20 0 -1 0 0.50 0.40 0 -1 0 0.10 0.10 0 1 0 1.40 0.50 0 2 0 11.50 0.90 0 2 0 11.80 0.90 0 -2 0 13.40 0.90 0 -2 0 10.20 0.90 0 2 0 8.80 1.60 0 3 0 0.20 1.40 0 3 0 0.40 0.50 0 3 0 0.90 0.50 0 -3 0 0.30 0.50 0 -3 0 0.80 0.50 0 -3 0 0.50 1.40 0 4 0 1162.18 52.59 0 4 0 1267.57 52.59 0 -4 0 1286.37 52.59 0 4 0 1279.77 53.99 0 -4 0 1304.57 52.69 0 -4 0 1264.17 54.19 0 -5 0 3.40 2.60 0 -5 0 1.70 1.00 0 5 0 2.60 0.90 0 5 0 1.00 0.70 0 5 0 -1.00 2.50 0 6 0 15.20 1.40 0 -6 0 15.30 1.90 0 6 0 15.60 1.90 0 -6 0 15.50 4.30 0 6 0 13.00 1.90 0 -6 0 11.60 1.80 0 6 0 21.10 4.40 0 -7 0 1.70 0.90 0 -7 0 1.50 1.40 0 7 0 -1.00 1.10 0 -7 0 1.00 1.30 0 7 0 2.60 0.80 0 7 0 2.10 1.40 0 -8 0 2474.75 106.49 0 -8 0 2637.04 105.69 0 8 0 2634.84 105.69 0 8 0 2461.25 106.49 0 9 0 0.30 0.90 0 9 0 2.80 2.30 0 -9 0 0.80 1.20 0 10 0 131.89 6.30 0 -10 0 136.59 6.40 0 11 0 0.90 1.10 0 -11 0 1.00 1.50 0 -12 0 274.27 12.10 0 12 0 267.77 11.90 0 13 0 0.10 1.30 0 -13 0 2.00 1.90 0 -14 0 27.40 2.90 0 14 0 27.90 2.50 0 -15 0 1.10 2.30 0 15 0 0.30 1.30 0 -16 0 82.89 5.40 0 16 0 91.49 4.50 -1 -1 0 709.93 30.40 1 1 0 694.63 30.30 -1 1 0 706.03 30.30 1 -1 0 694.43 30.30 -1 -1 0 713.13 30.10 -1 1 0 724.93 29.80 1 -3 0 503.85 20.80 -1 -3 0 491.05 22.00 -1 -3 0 496.85 22.10 1 3 0 486.35 20.80 1 -3 0 500.95 20.80 -1 -3 0 498.85 20.90 -1 3 0 487.45 20.80 -1 -3 0 503.85 20.90 1 3 0 512.35 20.90 1 -3 0 487.75 22.00 -1 3 0 494.95 20.80 -1 3 0 476.35 21.90 1 4 0 1101.29 46.40 -1 -4 0 1179.68 48.00 -1 -4 0 1064.89 46.40 1 -4 0 1143.39 46.40 -1 4 0 1040.50 46.30 1 -4 0 1090.29 46.40 -1 -4 0 1094.79 48.00 -1 -4 0 1103.89 46.40 -1 4 0 1097.89 47.80 1 -4 0 1232.08 48.20 1 4 0 1086.59 46.40 -1 -5 0 1483.85 63.39 1 -5 0 1436.56 63.19 1 5 0 1416.36 61.29 1 5 0 1484.15 61.29 -1 5 0 1428.86 62.99 -1 -5 0 1387.26 64.19 -1 -5 0 1450.65 61.29 -1 -5 0 1457.45 61.29 -1 5 0 1502.95 61.29 -1 5 0 1494.25 61.29 1 -5 0 1565.04 61.29 1 -5 0 1522.85 61.29 -1 -6 0 66.69 3.70 -1 6 0 62.19 3.60 1 -6 0 65.19 3.60 -1 -6 0 58.79 7.40 -1 6 0 62.29 3.60 1 -6 0 61.49 3.60 1 -6 0 50.29 6.90 -1 -6 0 56.09 3.00 -1 -6 0 70.99 3.80 -1 6 0 53.29 2.90 1 6 0 60.69 3.70 1 6 0 52.29 3.00 1 6 0 58.19 3.60 -1 -7 0 7268.27 289.07 -1 -7 0 6645.33 288.27 1 -7 0 6636.84 288.17 1 -7 0 7368.46 288.97 1 -8 0 1069.09 46.90 -1 -8 0 1160.48 46.00 1 -8 0 1118.99 46.90 1 8 0 1061.29 46.80 -1 -8 0 1113.69 47.00 -1 8 0 1079.49 47.40 1 8 0 1166.38 46.00 -1 -8 0 1067.19 46.10 -1 9 0 17.60 1.80 1 9 0 20.60 1.90 -1 -9 0 22.00 2.20 -1 9 0 18.60 3.20 1 -10 0 1761.12 74.09 -1 10 0 1846.52 73.99 1 10 0 1743.23 73.99 -1 -10 0 1775.32 74.09 1 -11 0 388.76 17.50 1 11 0 416.86 17.40 -1 11 0 399.66 17.30 -1 -11 0 410.06 17.50 -1 -12 0 177.78 8.30 1 12 0 168.28 8.00 1 -12 0 174.38 8.20 -1 12 0 173.78 8.00 -1 13 0 35.60 2.80 1 -13 0 37.00 3.80 1 13 0 41.30 3.00 -1 -13 0 37.80 3.70 -1 -14 0 1.80 2.00 -1 14 0 2.90 1.30 1 14 0 3.80 1.50 1 -14 0 4.50 2.20 1 -15 0 112.69 7.10 1 15 0 126.89 6.00 -1 15 0 123.29 5.90 -1 -15 0 127.49 6.60 -1 16 0 3.70 1.30 -1 -16 0 0.20 2.00 1 16 0 3.00 1.40 1 -16 0 0.10 3.10 2 0 0 8386.16 347.27 2 2 0 7020.80 292.57 2 -2 0 7042.10 292.57 -2 -2 0 7195.28 292.67 -2 2 0 6969.10 292.57 -2 -3 0 4433.96 181.98 2 -3 0 4398.96 181.88 -2 3 0 4261.47 181.78 -2 -4 0 694.53 28.80 -2 4 0 675.83 30.50 2 -4 0 680.43 28.70 -2 -4 0 690.63 30.60 2 4 0 706.43 28.80 2 -4 0 693.73 30.60 -2 4 0 700.63 28.70 -2 -4 0 595.44 28.60 -2 4 0 714.13 28.80 -2 -4 0 681.43 30.70 -2 -4 0 690.43 29.40 2 4 0 641.04 28.70 -2 -4 0 693.53 28.80 2 -4 0 684.73 28.70 -2 -5 0 764.12 30.70 2 -5 0 725.73 29.90 -2 -5 0 632.54 29.40 -2 -5 0 766.52 30.00 -2 5 0 637.14 31.90 -2 5 0 690.73 29.40 -2 -5 0 758.82 30.00 -2 5 0 724.33 29.90 -2 5 0 728.33 29.90 -2 -5 0 625.44 29.70 2 -5 0 650.03 30.10 2 5 0 734.63 30.00 2 5 0 749.42 30.00 -2 -5 0 744.13 29.90 -2 -5 0 709.23 32.30 2 -5 0 662.03 32.00 -2 6 0 471.25 19.20 -2 -6 0 460.15 19.80 -2 -6 0 440.06 19.80 -2 -6 0 467.65 19.30 -2 -6 0 432.66 19.80 -2 -6 0 448.36 19.20 2 -6 0 458.35 19.70 2 6 0 471.65 19.20 -2 -6 0 495.75 19.60 -2 6 0 423.36 19.70 2 -6 0 478.95 19.80 -2 -6 0 413.26 20.30 2 6 0 467.35 19.90 2 6 0 458.15 19.80 -2 6 0 450.55 19.80 -2 -7 0 1017.50 44.00 2 7 0 1077.09 43.30 -2 -7 0 1018.90 43.40 2 7 0 1012.10 44.00 -2 -7 0 1022.60 43.60 -2 7 0 1085.19 43.20 -2 -7 0 1050.99 44.60 2 -7 0 992.80 43.20 2 -7 0 1035.10 44.00 2 -7 0 1007.60 43.90 -2 -7 0 1069.29 43.80 -2 -7 0 1078.29 43.30 -2 7 0 1029.80 44.00 2 8 0 20.90 1.90 -2 -8 0 22.60 4.40 -2 8 0 22.10 1.70 -2 -8 0 22.70 3.20 2 -8 0 17.10 2.00 2 8 0 24.00 3.60 -2 -8 0 18.30 2.50 -2 -8 0 19.70 2.00 -2 8 0 19.30 3.30 -2 -8 0 22.90 3.40 2 -8 0 25.40 4.40 2 9 0 58.99 3.40 -2 -9 0 63.99 3.50 -2 9 0 61.19 7.10 -2 9 0 60.59 3.30 -2 10 0 6.20 1.20 2 10 0 2.30 1.20 -2 -10 0 1.90 1.40 2 -10 0 2.70 1.60 2 11 0 135.49 6.50 2 -11 0 130.89 6.70 -2 11 0 138.89 6.40 -2 -11 0 134.49 6.60 -2 -12 0 43.60 3.70 2 -12 0 34.90 3.70 2 -13 0 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2 310.27 15.00 -3 -5 2 335.77 15.10 -3 5 2 381.16 16.10 3 5 -2 433.16 16.40 -3 -5 -2 378.86 16.20 -3 -5 -2 395.86 16.90 3 5 -2 407.76 16.90 3 -5 2 397.16 16.90 3 -5 2 353.16 16.20 -3 -5 -2 365.76 16.80 3 5 -2 381.46 16.70 3 -5 2 380.76 16.90 -3 5 2 370.76 16.50 -3 -5 -2 362.66 16.90 3 -5 2 356.96 16.80 -3 5 2 386.36 16.60 -3 6 -2 1977.00 79.79 3 -6 -2 1941.81 80.29 -3 -6 2 1945.21 80.39 3 6 2 1951.50 79.69 3 6 2 1845.82 80.39 -3 -6 2 1925.61 80.49 -3 -6 2 1942.71 79.89 -3 -6 2 1858.51 80.49 -3 6 -2 1858.61 80.49 -3 -6 2 1971.00 81.89 -3 -6 2 1920.01 79.69 3 -6 -2 1938.51 80.19 -3 6 2 1993.50 80.39 -3 -6 -2 1939.81 80.99 -3 6 2 1924.01 80.99 3 -6 2 1924.01 81.09 3 6 -2 1917.11 81.19 3 -6 2 1949.60 81.39 3 -6 2 1944.11 81.29 3 6 -2 1918.61 81.29 -3 -6 -2 1962.30 80.49 -3 -6 -2 1979.40 81.29 3 -6 2 1905.11 80.59 3 6 -2 1947.11 80.49 -3 -7 2 1121.79 44.70 -3 -7 2 1100.79 45.60 3 -7 -2 1016.50 45.20 3 7 2 1156.18 44.70 -3 -7 2 1098.29 47.00 -3 7 -2 966.00 45.60 -3 7 -2 1134.09 44.70 3 7 2 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-8 13 58.29 3.90 -4 8 -13 44.00 5.80 4 -8 13 57.29 8.80 4 -8 13 56.49 3.60 4 -8 13 62.49 3.90 5 0 13 234.48 13.90 5 0 13 243.38 11.30 -5 0 -13 261.77 12.60 5 0 13 239.68 10.70 -5 1 -13 278.97 13.50 5 1 13 267.57 11.60 5 1 13 278.27 12.30 5 1 13 246.38 14.60 5 -1 13 267.27 11.70 5 -1 13 252.57 14.80 5 -1 13 283.57 12.30 -5 -1 -13 274.07 13.70 -5 2 -13 207.28 10.60 5 2 13 191.88 9.20 5 2 13 187.08 8.50 5 2 13 183.58 11.90 5 -2 13 184.68 8.40 -5 -2 -13 198.58 11.10 5 -2 13 181.18 11.90 5 -2 13 187.68 9.00 -5 3 -13 173.48 9.60 5 3 13 172.98 8.20 5 3 13 146.09 10.80 5 -3 13 156.68 7.70 -5 -3 -13 150.78 10.60 5 -3 13 164.98 15.00 5 -3 13 152.28 7.10 -5 -4 13 8.30 3.30 5 4 13 4.70 6.30 5 4 13 4.80 2.10 -5 4 -13 1.60 3.20 5 -4 13 8.00 1.50 5 -4 13 10.90 5.30 5 -4 13 7.20 2.00 -5 -5 13 152.08 7.50 5 5 13 129.79 8.80 -5 5 -13 154.48 8.70 5 -5 13 167.98 7.70 5 -5 13 148.99 11.40 5 -5 13 167.78 7.80 -5 6 -13 39.80 5.50 5 6 13 33.20 3.50 -5 -6 13 34.70 3.70 5 -6 13 35.50 3.20 5 -6 13 38.20 2.70 5 -6 13 32.20 6.70 -6 0 -13 343.07 15.50 6 0 13 313.47 13.60 6 0 13 299.37 13.10 6 0 13 265.07 16.20 6 1 13 56.99 9.30 -6 1 -13 83.09 6.90 6 1 13 63.69 3.90 6 1 13 76.99 4.40 6 -1 13 74.69 4.20 6 -1 13 86.89 4.80 6 -1 13 77.39 9.70 6 2 13 347.67 20.00 6 2 13 451.55 18.10 6 2 13 387.86 17.30 -6 2 -13 455.25 20.10 -6 -2 -13 386.96 18.40 6 -2 13 323.17 22.40 6 -2 13 424.56 17.50 6 -2 13 396.36 16.40 -6 3 -13 214.38 12.10 6 3 13 205.98 9.80 -6 -3 -13 172.48 11.20 6 -3 13 184.08 8.50 6 -3 13 177.38 8.00 -6 4 -13 96.39 7.00 6 4 13 84.89 5.00 6 -4 13 65.49 3.70 6 -4 13 68.79 4.20 0 0 14 889.21 40.50 0 0 14 929.41 38.50 0 -1 14 141.59 10.20 0 1 14 141.49 10.10 0 1 14 153.98 7.50 0 -1 14 153.38 7.40 0 2 14 140.29 7.40 0 2 14 140.59 10.10 0 -2 14 156.98 10.40 0 -2 14 147.99 7.30 0 -3 14 4.80 1.90 0 -3 14 5.20 4.40 0 3 14 3.10 4.30 0 4 14 1072.89 47.80 0 -4 14 1143.79 46.10 0 -4 14 1056.89 47.90 0 5 14 10.30 5.10 0 -5 14 8.30 2.10 0 -5 14 6.40 4.40 0 -6 14 8.10 4.40 0 -6 14 12.50 2.10 0 -7 14 561.24 22.70 0 -7 14 488.15 24.60 0 -8 14 13.60 2.10 0 -8 14 15.40 4.90 0 -9 14 249.97 13.70 1 0 14 200.48 9.10 -1 0 14 199.58 9.00 -1 0 -14 171.98 11.10 1 0 14 186.68 11.60 -1 0 14 184.58 11.90 -1 -1 14 152.28 7.50 1 1 14 158.58 7.60 1 1 14 145.79 10.20 -1 -1 14 146.09 10.60 -1 1 -14 157.38 9.30 1 -1 14 135.49 9.60 -1 1 14 119.79 9.90 -1 1 14 129.99 6.80 1 -1 14 135.59 6.80 -1 -2 14 38.20 3.40 -1 -2 14 40.60 7.60 1 2 14 34.10 6.60 1 2 14 37.10 3.60 1 -2 14 32.70 3.30 1 -2 14 33.70 7.10 -1 2 14 36.20 7.40 -1 -3 14 535.75 25.70 1 3 14 518.85 25.40 1 3 14 554.04 23.40 -1 -3 14 559.44 23.40 -1 3 14 529.65 25.90 1 -3 14 543.55 26.10 1 -3 14 583.24 23.90 -1 -4 14 72.39 4.50 -1 -4 14 75.09 8.30 1 4 14 74.69 7.80 1 -4 14 69.89 4.50 -1 4 14 71.39 8.70 1 -4 14 74.99 8.00 -1 -5 14 34.20 7.40 -1 -5 14 37.30 3.30 1 5 14 30.50 5.40 1 -5 14 27.30 2.80 1 -5 14 33.10 6.60 -1 5 14 36.90 6.70 -1 -6 14 186.08 8.70 -1 -6 14 176.48 11.60 1 6 14 181.88 11.60 1 -6 14 184.48 8.60 1 -6 14 179.68 11.40 -1 -7 14 127.79 13.80 -1 -7 14 135.49 6.70 1 -7 14 113.09 9.10 1 -7 14 123.39 6.10 -1 -8 14 177.88 12.20 -1 -8 14 226.38 10.00 1 -8 14 157.78 11.10 1 -8 14 206.28 9.00 2 0 14 43.00 3.50 2 0 14 38.10 6.60 -2 0 -14 39.60 6.60 -2 0 14 35.80 6.40 2 1 14 707.03 29.00 2 1 14 647.14 30.90 -2 -1 14 677.33 28.90 -2 -1 14 644.94 31.00 -2 1 -14 704.53 29.70 -2 -1 -14 634.44 28.10 -2 1 14 607.84 29.30 2 -1 14 670.23 27.40 2 -1 14 628.94 29.40 -2 2 -14 166.98 9.20 2 2 14 153.58 7.70 -2 -2 14 152.18 7.60 2 2 14 144.39 10.30 -2 -2 14 150.68 11.20 -2 2 14 154.48 16.00 2 -2 14 151.58 7.50 2 -2 14 145.29 10.10 -2 -3 14 693.13 32.90 -2 -3 14 670.33 37.30 -2 -3 14 685.23 32.70 -2 -3 14 755.92 30.80 2 3 14 714.43 32.80 -2 3 -14 773.82 31.50 2 3 14 758.32 30.80 2 -3 14 681.83 31.80 2 -3 14 713.63 29.90 -2 -4 14 106.49 5.50 2 4 14 87.39 8.30 -2 -4 14 83.19 16.50 2 4 14 102.09 5.80 -2 -4 14 94.89 9.70 -2 4 -14 97.09 7.20 2 -4 14 67.39 9.10 2 -4 14 81.99 4.70 -2 5 -14 55.59 6.00 -2 -5 14 47.20 8.40 2 5 14 60.29 7.40 -2 -5 14 61.59 4.00 2 -5 14 55.09 7.60 2 -5 14 67.19 4.10 2 6 14 248.48 14.30 -2 -6 14 269.07 11.80 -2 -6 14 257.67 17.70 2 -6 14 271.67 11.60 2 -6 14 237.48 14.10 -2 -7 14 73.09 9.00 -2 7 -14 90.89 6.60 -2 -7 14 82.59 5.00 2 -7 14 80.39 8.60 2 -7 14 80.99 4.60 -2 -8 14 95.39 5.20 -2 -8 14 81.99 9.10 -2 8 -14 104.99 7.00 2 -8 14 74.49 8.10 2 -8 14 82.49 4.50 3 0 14 70.09 7.60 -3 0 -14 79.79 7.30 3 0 14 76.09 4.70 -3 1 -14 64.39 6.70 3 1 14 67.29 4.40 3 1 14 64.99 7.40 3 -1 14 61.99 7.30 -3 -1 -14 55.69 7.60 3 -1 14 60.59 4.10 3 2 14 388.66 20.80 -3 2 -14 434.16 19.60 3 2 14 456.75 18.80 -3 -2 14 431.46 18.70 3 -2 14 375.06 19.90 3 -2 14 433.86 17.90 3 3 14 55.99 4.20 3 3 14 58.89 7.10 -3 -3 14 52.29 4.20 -3 3 -14 65.49 6.40 3 -3 14 48.40 7.20 3 -3 14 56.09 3.80 -3 4 -14 12.20 3.50 3 4 14 14.40 4.70 -3 -4 14 19.20 3.10 3 4 14 14.90 2.60 3 -4 14 15.10 2.30 3 -4 14 18.00 5.10 3 5 14 224.98 13.50 -3 5 -14 261.27 12.40 -3 -5 14 257.17 11.30 -3 -5 14 231.08 18.60 3 -5 14 215.18 9.70 3 -5 14 202.78 12.30 -3 6 -14 46.40 5.80 -3 -6 14 47.80 3.70 -3 -6 14 34.70 8.50 3 -6 14 32.70 7.10 3 -6 14 41.60 3.20 -3 -7 14 191.18 8.40 -3 -7 14 150.88 14.70 3 -7 14 202.98 8.90 3 -7 14 172.68 11.50 -4 0 -14 703.33 29.80 4 0 14 634.94 30.80 4 0 14 696.83 29.10 4 1 14 195.88 12.20 -4 1 -14 208.68 11.20 4 1 14 207.68 9.70 -4 -1 -14 208.28 11.60 4 -1 14 211.08 9.70 4 -1 14 196.98 12.20 4 2 14 258.77 11.40 -4 2 -14 249.38 12.50 4 2 14 234.48 13.70 -4 -2 -14 252.07 13.60 4 -2 14 265.67 11.50 4 -2 14 235.48 13.90 4 3 14 35.80 3.30 4 3 14 23.60 5.00 -4 3 -14 26.10 4.00 4 -3 14 22.90 5.10 4 -3 14 31.30 3.00 4 4 14 46.90 8.40 -4 -4 14 51.39 4.80 -4 4 -14 56.79 6.10 4 4 14 52.89 4.00 4 -4 14 39.20 7.70 4 -4 14 49.20 3.50 4 5 14 253.17 11.70 -4 -5 14 259.47 11.80 -4 5 -14 278.17 12.80 4 5 14 240.68 14.00 4 -5 14 247.18 10.90 4 -5 14 227.38 13.50 -4 -6 14 147.79 7.60 -4 6 -14 161.38 8.90 4 -6 14 123.89 10.10 4 -6 14 142.89 6.70 5 0 14 376.36 15.60 5 0 14 316.37 17.60 -5 0 -14 364.36 20.20 -5 1 -14 44.60 6.90 5 1 14 44.30 3.40 5 1 14 28.50 5.50 5 -1 14 37.90 7.70 5 -1 14 44.60 3.40 -5 -1 -14 35.40 5.60 5 2 14 93.59 6.60 5 2 14 66.19 8.20 -5 2 -14 85.29 8.50 5 -2 14 71.19 8.60 -5 -2 -14 65.89 8.00 5 -2 14 73.39 4.40 5 3 14 295.67 12.40 5 3 14 260.47 14.70 -5 3 -14 260.87 15.50 5 -3 14 248.48 13.40 5 -3 14 204.28 11.30 -5 4 -14 135.49 8.40 5 4 14 131.19 6.70 5 -4 14 114.79 10.50 5 -4 14 151.08 6.80 0 0 15 -2.10 4.40 0 0 15 -2.80 1.90 0 1 15 -1.30 2.20 0 -1 15 0.20 1.80 0 -1 15 2.50 4.50 0 1 15 1.90 4.60 0 2 -15 2.10 4.00 0 2 15 8.30 4.80 0 -2 15 11.00 2.10 0 -2 15 10.70 4.70 0 3 15 19.90 5.30 0 -3 15 21.10 2.80 0 -3 15 12.30 5.00 0 -4 15 223.98 10.00 0 4 15 208.38 13.00 0 -4 15 212.88 12.90 0 -5 15 100.49 10.50 0 5 15 90.79 9.50 0 -5 15 112.59 5.60 0 -6 15 472.35 23.60 0 -6 15 521.15 21.40 0 -7 15 2.10 5.00 0 -7 15 7.70 1.90 1 0 15 84.99 5.10 -1 0 15 84.09 9.00 1 0 15 90.99 8.20 -1 0 15 87.19 5.30 1 1 15 141.69 10.20 1 1 15 149.49 7.40 -1 -1 15 146.39 10.90 -1 1 -15 140.99 9.90 -1 -1 15 149.19 7.40 1 -1 15 140.49 10.10 -1 1 15 138.89 10.70 1 -1 15 149.09 7.20 -1 -2 15 183.58 8.50 -1 -2 15 169.78 11.70 -1 2 -15 168.08 10.30 1 2 15 171.88 11.20 1 2 15 182.48 8.60 -1 2 15 154.58 11.40 1 -2 15 155.68 10.60 1 -2 15 161.98 7.70 1 3 15 86.79 8.40 -1 3 -15 77.29 7.20 -1 -3 15 79.99 8.90 -1 -3 15 101.79 5.20 -1 3 15 96.79 10.50 1 -3 15 115.09 5.70 1 -3 15 94.79 8.70 -1 -4 15 412.06 21.50 -1 4 -15 443.76 19.90 -1 -4 15 463.55 19.10 1 4 15 431.36 21.20 1 -4 15 451.95 21.90 1 -4 15 464.25 19.60 -1 4 15 436.16 22.20 -1 -5 15 106.79 9.90 1 5 15 105.99 9.70 -1 -5 15 118.09 5.90 1 -5 15 112.49 5.80 1 -5 15 111.49 11.00 -1 -6 15 230.88 10.30 -1 -6 15 188.58 12.70 1 -6 15 177.18 11.70 1 -6 15 201.28 9.00 -1 -7 15 28.00 5.70 -1 -7 15 36.70 3.10 1 -7 15 35.10 3.00 1 -7 15 26.10 5.20 -2 0 -15 16.40 4.80 2 0 15 19.20 2.50 2 0 15 18.90 4.50 -2 -1 15 14.00 9.90 -2 1 -15 22.50 4.60 2 1 15 17.80 4.60 2 1 15 22.50 3.10 2 -1 15 20.30 4.70 2 -1 15 20.80 2.80 -2 2 -15 15.40 3.90 2 2 15 23.80 4.90 2 2 15 20.80 3.30 -2 -2 15 23.60 3.50 2 -2 15 17.00 4.60 2 -2 15 23.40 2.90 2 3 15 249.28 11.30 -2 -3 15 211.68 14.90 -2 -3 15 252.17 11.10 -2 3 -15 253.97 12.40 2 3 15 237.78 13.60 2 -3 15 240.98 10.70 2 -3 15 224.48 13.20 -2 4 -15 186.48 10.30 -2 -4 15 173.58 12.60 2 4 15 193.58 12.40 -2 -4 15 201.38 9.00 2 -4 15 174.48 11.80 2 -4 15 202.68 9.00 -2 -5 15 223.18 14.20 -2 5 -15 251.07 12.00 -2 -5 15 238.38 12.10 2 5 15 241.58 13.50 2 -5 15 292.87 12.40 2 -5 15 256.57 14.60 -2 -6 15 53.49 3.80 -2 -6 15 47.40 9.30 -2 6 -15 60.89 6.30 2 -6 15 52.49 3.70 2 -6 15 45.00 7.20 -3 0 -15 -1.70 4.90 3 0 15 1.20 1.90 3 0 15 4.40 4.30 3 1 15 419.16 17.80 -3 1 -15 416.76 18.90 3 1 15 380.06 19.80 3 -1 15 410.36 17.50 3 -1 15 386.86 19.50 -3 2 -15 43.80 6.50 3 2 15 36.80 7.50 3 2 15 40.40 3.60 3 -2 15 29.90 3.10 3 -2 15 34.20 6.80 3 3 15 226.88 16.00 -3 3 -15 218.38 11.50 -3 -3 15 209.88 10.30 3 3 15 225.38 10.60 3 -3 15 207.38 9.50 3 -3 15 201.78 12.80 3 4 15 131.19 7.10 -3 -4 15 142.29 7.00 3 4 15 120.49 9.40 -3 4 -15 148.69 10.90 3 -4 15 141.39 6.70 3 -4 15 126.79 9.60 3 5 15 187.08 11.90 -3 5 -15 220.58 10.70 -3 -5 15 203.58 9.50 3 -5 15 198.38 12.10 3 -5 15 217.08 9.60 4 0 15 7.00 4.50 -4 0 -15 -2.40 4.40 4 0 15 1.40 3.00 4 1 15 43.00 7.00 -4 1 -15 43.10 6.80 4 1 15 59.79 6.00 4 -1 15 51.89 4.20 -4 -1 -15 57.09 8.80 4 -1 15 43.10 7.10 4 2 15 9.80 2.30 4 2 15 8.70 4.60 -4 2 -15 8.50 3.90 4 -2 15 0.80 4.40 4 -2 15 2.50 2.90 4 3 15 32.70 6.70 4 3 15 37.90 3.50 -4 3 -15 36.50 4.20 4 -3 15 22.90 5.10 4 -3 15 28.90 2.90 0 0 16 1184.88 47.70 0 0 16 1088.59 49.40 0 1 16 105.09 9.90 0 -1 16 142.59 8.30 0 -1 16 113.69 9.60 0 -2 16 604.14 27.30 0 2 16 643.74 27.60 0 -2 16 531.55 26.10 0 3 16 0.90 5.80 0 -3 16 -0.30 4.80 0 3 -16 4.70 4.40 0 -3 16 0.10 2.60 0 4 -16 23.10 4.10 0 -4 16 17.80 4.90 0 -4 16 27.00 3.00 0 4 16 26.10 6.50 0 -5 16 94.39 5.00 0 -5 16 88.59 8.60 0 5 -16 83.49 7.30 1 0 16 -0.20 4.60 -1 0 16 2.40 5.70 1 0 16 4.70 2.50 -1 -1 16 41.30 4.40 1 1 16 48.20 4.00 -1 -1 16 39.30 6.50 1 1 16 41.60 7.40 1 -1 16 35.60 7.00 -1 1 16 38.70 6.90 -1 2 -16 184.98 11.70 -1 -2 16 223.58 9.70 1 2 16 206.18 12.30 -1 -2 16 202.08 12.80 1 -2 16 178.08 10.40 1 -2 16 203.58 12.00 -1 2 16 220.28 13.60 1 3 16 121.99 9.60 -1 -3 16 132.59 10.10 -1 3 -16 111.29 8.70 -1 -3 16 123.89 6.30 1 -3 16 122.99 9.90 1 -3 16 172.28 8.60 -1 4 -16 310.87 14.60 -1 -4 16 321.57 13.40 -1 -4 16 290.97 16.10 1 4 16 283.77 15.80 1 -4 16 280.97 15.40 1 -4 16 308.17 13.10 2 0 16 20.50 2.80 2 0 16 15.80 4.80 2 1 16 654.33 27.00 2 1 16 612.04 28.80 2 -1 16 588.44 29.10 2 -1 16 698.63 27.70 2 2 16 15.70 2.70 -2 2 -16 15.30 4.70 2 2 16 11.10 4.80 2 -2 16 20.40 2.70 2 -2 16 19.80 4.90 -2 -3 16 97.29 5.50 -2 3 -16 81.19 7.50 2 3 16 86.89 8.30 2 -3 16 110.69 5.60 2 -3 16 98.99 8.40 -2 -4 16 25.00 3.40 -2 4 -16 26.60 4.20 2 4 16 26.20 5.50 2 -4 16 24.50 2.70 2 -4 16 17.90 4.50 3 0 16 68.69 8.00 3 0 16 85.49 4.70 3 1 16 31.30 3.30 3 1 16 25.30 5.10 -3 1 -16 35.10 5.20 3 -1 16 33.90 6.80 3 -1 16 34.40 2.90 3 2 16 75.29 7.90 3 2 16 78.79 4.80 -3 2 -16 82.89 7.80 3 -2 16 87.79 4.80 3 -2 16 84.59 8.00 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 34774 _shelx_shelxl_version_number 2014/7 _olex2_date_sample_data_collection 2015-01-30 _olex2_date_sample_submission 2015-01-28 _olex2_exptl_crystal_mounting_method 'mounted on a cryoloop' _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -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 N1 N 0.5932(2) 0.36206(12) 0.62237(12) 0.0192(3) Uani 1 1 d . . . . . C1 C 0.4313(2) 0.36225(14) 0.55842(14) 0.0191(4) Uani 1 1 d . . . . . H1A H 0.4567 0.3302 0.4904 0.023 Uiso 1 1 calc R . . . . H1B H 0.3498 0.3144 0.5929 0.023 Uiso 1 1 calc R . . . . C2 C 0.3478(2) 0.46894(15) 0.54053(14) 0.0197(4) Uani 1 1 d . . . . . C3 C 0.3774(3) 0.52493(16) 0.44899(15) 0.0245(4) Uani 1 1 d . . . . . H3 H 0.4519 0.4962 0.3991 0.029 Uiso 1 1 calc R . . . . C4 C 0.2980(3) 0.62281(17) 0.43069(18) 0.0307(5) Uani 1 1 d . . . . . H4 H 0.3198 0.6615 0.3691 0.037 Uiso 1 1 calc R . . . . C5 C 0.1866(3) 0.66336(16) 0.5033(2) 0.0323(5) Uani 1 1 d . . . . . H5 H 0.1329 0.7302 0.4910 0.039 Uiso 1 1 calc R . . . . C6 C 0.1530(3) 0.60727(16) 0.59341(17) 0.0275(4) Uani 1 1 d . . . . . H6 H 0.0765 0.6353 0.6425 0.033 Uiso 1 1 calc R . . . . C7 C 0.2327(2) 0.50924(15) 0.61118(15) 0.0214(4) Uani 1 1 d . . . . . H7 H 0.2083 0.4697 0.6720 0.026 Uiso 1 1 calc R . . . . C8 C 0.7249(3) 0.43494(17) 0.57348(17) 0.0272(4) Uani 1 1 d . . . . . H8A H 0.8368 0.4096 0.5954 0.033 Uiso 1 1 calc R . . . . H8B H 0.7184 0.4266 0.4977 0.033 Uiso 1 1 calc R . . . . C9 C 0.7111(3) 0.55329(18) 0.59883(18) 0.0322(5) Uani 1 1 d . . . . . H9A H 0.7905 0.5939 0.5565 0.048 Uiso 1 1 calc GR . . . . H9B H 0.7367 0.5645 0.6719 0.048 Uiso 1 1 calc GR . . . . H9C H 0.5971 0.5781 0.5845 0.048 Uiso 1 1 calc GR . . . . C10 C 0.5542(3) 0.39174(17) 0.73208(15) 0.0245(4) Uani 1 1 d . . . . . H10A H 0.4667 0.3427 0.7586 0.029 Uiso 1 1 calc R . . . . H10B H 0.5084 0.4656 0.7336 0.029 Uiso 1 1 calc R . . . . C11 C 0.7059(3) 0.3862(2) 0.80321(18) 0.0383(5) Uani 1 1 d . . . . . H11A H 0.7908 0.4374 0.7798 0.058 Uiso 1 1 calc GR . . . . H11B H 0.7525 0.3134 0.8019 0.058 Uiso 1 1 calc GR . . . . H11C H 0.6718 0.4042 0.8737 0.058 Uiso 1 1 calc GR . . . . C12 C 0.6625(3) 0.24794(16) 0.61430(18) 0.0271(4) Uani 1 1 d . . . . . H12A H 0.6718 0.2289 0.5405 0.033 Uiso 1 1 calc R . . . . H12B H 0.7769 0.2473 0.6435 0.033 Uiso 1 1 calc R . . . . C13 C 0.5607(3) 0.16202(17) 0.6678(2) 0.0335(5) Uani 1 1 d . . . . . H13A H 0.4445 0.1657 0.6441 0.050 Uiso 1 1 calc GR . . . . H13B H 0.5646 0.1736 0.7425 0.050 Uiso 1 1 calc GR . . . . H13C H 0.6072 0.0912 0.6515 0.050 Uiso 1 1 calc GR . . . . Cl1 Cl 0.10243(6) 0.21950(4) 0.68575(3) 0.02534(14) Uani 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 N1 0.0147(7) 0.0235(7) 0.0193(7) 0.0028(6) 0.0009(6) 0.0003(6) C1 0.0157(8) 0.0225(8) 0.0192(8) -0.0007(7) -0.0014(6) 0.0000(7) C2 0.0162(8) 0.0218(8) 0.0209(9) -0.0003(7) -0.0026(7) -0.0014(6) C3 0.0238(9) 0.0284(9) 0.0214(9) 0.0030(7) -0.0026(7) -0.0023(8) C4 0.0333(11) 0.0291(10) 0.0298(10) 0.0088(8) -0.0101(9) -0.0051(9) C5 0.0292(11) 0.0214(9) 0.0463(13) 0.0000(9) -0.0142(10) 0.0031(8) C6 0.0205(9) 0.0270(9) 0.0349(11) -0.0065(8) -0.0044(8) 0.0024(7) C7 0.0157(8) 0.0251(9) 0.0234(9) -0.0004(7) -0.0011(7) -0.0013(7) C8 0.0170(8) 0.0379(11) 0.0268(10) 0.0045(8) 0.0016(7) -0.0069(8) C9 0.0305(11) 0.0358(11) 0.0303(11) 0.0015(9) -0.0050(9) -0.0125(9) C10 0.0277(10) 0.0287(9) 0.0170(9) -0.0001(7) 0.0000(7) 0.0023(8) C11 0.0415(13) 0.0476(12) 0.0259(11) 0.0025(10) -0.0117(10) 0.0021(11) C12 0.0193(8) 0.0288(9) 0.0333(11) 0.0017(8) 0.0027(8) 0.0078(7) C13 0.0295(11) 0.0256(9) 0.0454(13) 0.0066(9) 0.0034(9) 0.0074(8) Cl1 0.0192(2) 0.0376(2) 0.0193(2) 0.00085(17) -0.00007(16) -0.00432(18) 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 0.3290 0.5400 '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' 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 C8 N1 C1 110.79(14) . . C8 N1 C12 105.87(15) . . C10 N1 C1 109.67(14) . . C10 N1 C8 112.96(16) . . C10 N1 C12 111.61(15) . . C12 N1 C1 105.64(14) . . N1 C1 H1A 108.0 . . N1 C1 H1B 108.0 . . H1A C1 H1B 107.2 . . C2 C1 N1 117.26(15) . . C2 C1 H1A 108.0 . . C2 C1 H1B 108.0 . . C3 C2 C1 119.77(17) . . C7 C2 C1 120.63(17) . . C7 C2 C3 119.46(18) . . C2 C3 H3 119.9 . . C4 C3 C2 120.2(2) . . C4 C3 H3 119.9 . . C3 C4 H4 120.2 . . C5 C4 C3 119.6(2) . . C5 C4 H4 120.2 . . C4 C5 H5 119.6 . . C6 C5 C4 120.79(19) . . C6 C5 H5 119.6 . . C5 C6 H6 120.3 . . C5 C6 C7 119.4(2) . . C7 C6 H6 120.3 . . C2 C7 C6 120.52(19) . . C2 C7 H7 119.7 . . C6 C7 H7 119.7 . . N1 C8 H8A 108.3 . . N1 C8 H8B 108.3 . . H8A C8 H8B 107.4 . . C9 C8 N1 115.94(18) . . C9 C8 H8A 108.3 . . C9 C8 H8B 108.3 . . C8 C9 H9A 109.5 . . C8 C9 H9B 109.5 . . C8 C9 H9C 109.5 . . H9A C9 H9B 109.5 . . H9A C9 H9C 109.5 . . H9B C9 H9C 109.5 . . N1 C10 H10A 108.9 . . N1 C10 H10B 108.9 . . N1 C10 C11 113.40(17) . . H10A C10 H10B 107.7 . . C11 C10 H10A 108.9 . . C11 C10 H10B 108.9 . . C10 C11 H11A 109.5 . . C10 C11 H11B 109.5 . . C10 C11 H11C 109.5 . . H11A C11 H11B 109.5 . . H11A C11 H11C 109.5 . . H11B C11 H11C 109.5 . . N1 C12 H12A 108.4 . . N1 C12 H12B 108.4 . . H12A C12 H12B 107.5 . . C13 C12 N1 115.51(17) . . C13 C12 H12A 108.4 . . C13 C12 H12B 108.4 . . C12 C13 H13A 109.5 . . C12 C13 H13B 109.5 . . C12 C13 H13C 109.5 . . H13A C13 H13B 109.5 . . H13A C13 H13C 109.5 . . H13B C13 H13C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 N1 C1 1.537(2) . N1 C8 1.528(2) . N1 C10 1.504(2) . N1 C12 1.529(2) . C1 H1A 0.9900 . C1 H1B 0.9900 . C1 C2 1.504(2) . C2 C3 1.398(3) . C2 C7 1.393(3) . C3 H3 0.9500 . C3 C4 1.394(3) . C4 H4 0.9500 . C4 C5 1.391(4) . C5 H5 0.9500 . C5 C6 1.389(3) . C6 H6 0.9500 . C6 C7 1.396(3) . C7 H7 0.9500 . C8 H8A 0.9900 . C8 H8B 0.9900 . C8 C9 1.514(3) . C9 H9A 0.9800 . C9 H9B 0.9800 . C9 H9C 0.9800 . C10 H10A 0.9900 . C10 H10B 0.9900 . C10 C11 1.526(3) . C11 H11A 0.9800 . C11 H11B 0.9800 . C11 H11C 0.9800 . C12 H12A 0.9900 . C12 H12B 0.9900 . C12 C13 1.513(3) . C13 H13A 0.9800 . C13 H13B 0.9800 . C13 H13C 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 N1 C1 C2 C3 96.7(2) . . . . N1 C1 C2 C7 -87.6(2) . . . . C1 N1 C8 C9 83.1(2) . . . . C1 N1 C10 C11 176.05(17) . . . . C1 N1 C12 C13 -68.4(2) . . . . C1 C2 C3 C4 178.67(18) . . . . C1 C2 C7 C6 -178.74(17) . . . . C2 C3 C4 C5 -1.2(3) . . . . C3 C2 C7 C6 -3.0(3) . . . . C3 C4 C5 C6 -0.3(3) . . . . C4 C5 C6 C7 0.2(3) . . . . C5 C6 C7 C2 1.5(3) . . . . C7 C2 C3 C4 2.9(3) . . . . C8 N1 C1 C2 -57.6(2) . . . . C8 N1 C10 C11 -59.8(2) . . . . C8 N1 C12 C13 174.02(19) . . . . C10 N1 C1 C2 67.8(2) . . . . C10 N1 C8 C9 -40.4(2) . . . . C10 N1 C12 C13 50.7(2) . . . . C12 N1 C1 C2 -171.82(16) . . . . C12 N1 C8 C9 -162.81(18) . . . . C12 N1 C10 C11 59.3(2) . . . . loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.85(2) 2 0.15(2) _cod_database_fobs_code 3500030