#------------------------------------------------------------------------------ #$Date: 2020-05-06 22:19:53 +0300 (Wed, 06 May 2020) $ #$Revision: 251819 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/83/4038329.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_4038329 loop_ _publ_author_name 'Schnitzer, Tobias' 'Wennemers, Helma' _publ_section_title ; Deactivation of Secondary Amine Catalysts via Aldol Reaction-Amine Catalysis under Solvent-Free Conditions. ; _journal_name_full 'The Journal of organic chemistry' _journal_paper_doi 10.1021/acs.joc.0c00665 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C12 H15 N O3' _chemical_formula_sum 'C12 H15 N O3' _chemical_formula_weight 221.25 _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' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2017-10-03 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.47770(10) _cell_length_b 8.3194(2) _cell_length_c 25.6879(5) _cell_measurement_reflns_used 5578 _cell_measurement_temperature 100.0(1) _cell_measurement_theta_max 79.3380 _cell_measurement_theta_min 5.5760 _cell_volume 1170.63(4) _computing_cell_refinement 'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)' _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 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.0(1) _diffrn_detector 'CCD plate' _diffrn_detector_type 'Pilatus 300K' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -116.00 -78.00 0.50 0.10 -- -49.37 -77.00 -30.00 76 2 \w -65.00 22.00 0.50 0.10 -- -49.37 57.00 90.00 174 3 \w -26.00 49.00 0.50 0.10 -- 49.37 -38.00 150.00 150 4 \w -83.00 6.00 0.50 0.30 -- -70.00 38.00-150.00 178 5 \w 94.00 123.00 0.50 0.30 -- 110.00 -19.00 30.00 58 6 \w 38.00 84.00 0.50 0.30 -- 110.00 -57.00 -60.00 92 7 \w 94.00 123.00 0.50 0.30 -- 110.00 -19.00 -30.00 58 8 \w 94.00 123.00 0.50 0.30 -- 110.00 -19.00 0.00 58 9 \w 94.00 123.00 0.50 0.30 -- 110.00 -19.00-120.00 58 10 \w 38.00 84.00 0.50 0.30 -- 110.00 -57.00-180.00 92 11 \w 40.00 110.00 0.50 0.30 -- 110.00 -99.00 150.00 140 12 \w 40.00 110.00 0.50 0.30 -- 110.00 -99.00-150.00 140 13 \w 94.00 123.00 0.50 0.30 -- 110.00 -19.00-150.00 58 14 \w 38.00 84.00 0.50 0.30 -- 110.00 -57.00 120.00 92 15 \w 34.00 117.00 0.50 0.10 -- 49.37 57.00-120.00 166 16 \w 37.00 125.00 0.50 0.10 -- 49.37 34.00 135.00 176 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 300K' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0679473000 _diffrn_orient_matrix_UB_12 0.1696931000 _diffrn_orient_matrix_UB_13 0.0190942000 _diffrn_orient_matrix_UB_21 0.1034650000 _diffrn_orient_matrix_UB_22 0.0402560000 _diffrn_orient_matrix_UB_23 -0.0542324000 _diffrn_orient_matrix_UB_31 -0.2525395000 _diffrn_orient_matrix_UB_32 0.0622519000 _diffrn_orient_matrix_UB_33 -0.0170556000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_unetI/netI 0.0334 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 6939 _diffrn_reflns_point_group_measured_fraction_full 0.945 _diffrn_reflns_point_group_measured_fraction_max 0.945 _diffrn_reflns_theta_full 66.529 _diffrn_reflns_theta_max 66.529 _diffrn_reflns_theta_min 3.441 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.255 _exptl_crystal_description block _exptl_crystal_F_000 472 _exptl_crystal_size_max 0.146 _exptl_crystal_size_mid 0.089 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.121 _refine_diff_density_min -0.194 _refine_diff_density_rms 0.041 _refine_ls_abs_structure_details ; Flack x determined using 646 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.08(17) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 146 _refine_ls_number_reflns 1953 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.077 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0335 _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^)+(0.0447P)^2^+0.1222P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.0844 _reflns_Friedel_coverage 0.571 _reflns_Friedel_fraction_full 0.863 _reflns_Friedel_fraction_max 0.863 _reflns_number_gt 1846 _reflns_number_total 1953 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo0c00665_si_002.cif _cod_data_source_block w360817_1_1 _cod_database_code 4038329 _shelx_shelxl_version_number 2016/6 _chemical_oxdiff_formula C12H15NO3 _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. ; _reflns_odcompleteness_completeness 99.92 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. 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 2.a Ternary CH refined with riding coordinates: C2(H2), C5(H5) 2.b Secondary CH2 refined with riding coordinates: C6(H6A,H6B), C7(H7A,H7B) 2.c Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11) 2.d Idealised Me refined as rotating group: C12(H12A,H12B,H12C) ; _shelx_res_file ; TITL w360817_1_1_a.res in P2(1)2(1)2(1) w360817_1_1.res created by SHELXL-2016/6 at 15:12:29 on 03-Oct-2017 REM Old TITL w360817_1_1 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.121, Rweak 0.031, Alpha 0.001, Orientation as input REM Flack x = 0.124 ( 0.168 ) from Parsons' quotients REM Formula found by SHELXT: C13 O3 CELL 1.54184 5.4777 8.3194 25.6879 90 90 90 ZERR 4 0.0001 0.0002 0.0005 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 N O UNIT 48 60 4 12 L.S. 9 PLAN 20 BOND $H list 4 fmap 2 acta SHEL 999 0.84 REM REM REM WGHT 0.044700 0.122200 FVAR 1.12271 O1 4 0.201142 0.996957 0.365174 11.00000 0.03568 0.02348 = 0.03838 0.00573 -0.00215 -0.00044 O2 4 -0.053694 0.816044 0.390837 11.00000 0.01730 0.02645 = 0.07339 0.00054 0.00297 -0.00056 O3 4 0.745145 0.542561 0.493865 11.00000 0.07623 0.04809 = 0.04429 -0.01670 -0.03458 0.01593 N1 3 0.154200 0.866898 0.384796 11.00000 0.02011 0.02100 = 0.02898 -0.00561 -0.00037 0.00058 C1 1 0.307193 0.566745 0.330544 11.00000 0.01871 0.01510 = 0.02373 -0.00136 -0.00152 0.00460 C2 1 0.326185 0.588667 0.389343 11.00000 0.01779 0.01914 = 0.02342 -0.00323 0.00137 -0.00050 AFIX 13 H2 2 0.173175 0.551753 0.405088 11.00000 -1.20000 AFIX 0 C3 1 0.112936 0.482879 0.308644 11.00000 0.01962 0.02418 = 0.03077 -0.00201 0.00132 -0.00042 AFIX 43 H3 2 -0.004896 0.437203 0.330104 11.00000 -1.20000 AFIX 0 C4 1 0.482913 0.631742 0.297679 11.00000 0.02343 0.02154 = 0.02803 -0.00088 -0.00096 -0.00074 AFIX 43 H4 2 0.615173 0.686651 0.311788 11.00000 -1.20000 AFIX 0 C5 1 0.537643 0.491159 0.413281 11.00000 0.02068 0.02079 = 0.02175 -0.00210 -0.00017 0.00077 AFIX 13 H5 2 0.690878 0.522518 0.396412 11.00000 -1.20000 AFIX 0 C6 1 0.498210 0.309036 0.405879 11.00000 0.02979 0.02010 = 0.03063 -0.00245 -0.00520 -0.00044 AFIX 23 H6A 2 0.350456 0.277510 0.424016 11.00000 -1.20000 H6B 2 0.474366 0.287143 0.369140 11.00000 -1.20000 AFIX 0 C7 1 0.361465 0.765756 0.403347 11.00000 0.01789 0.02164 = 0.02665 -0.00579 -0.00351 0.00261 AFIX 23 H7A 2 0.376011 0.776116 0.440831 11.00000 -1.20000 H7B 2 0.511996 0.804305 0.387866 11.00000 -1.20000 AFIX 0 C8 1 0.093574 0.466818 0.254954 11.00000 0.02408 0.02932 = 0.03022 -0.00673 -0.00651 0.00071 AFIX 43 H8 2 -0.036825 0.410433 0.240669 11.00000 -1.20000 AFIX 0 C9 1 0.267398 0.534340 0.222769 11.00000 0.03328 0.02810 = 0.02154 -0.00399 -0.00483 0.00766 AFIX 43 H9 2 0.252665 0.525111 0.186826 11.00000 -1.20000 AFIX 0 C10 1 0.463431 0.615715 0.244090 11.00000 0.03031 0.02722 = 0.02624 0.00255 0.00366 0.00174 AFIX 43 H10 2 0.582235 0.659707 0.222505 11.00000 -1.20000 AFIX 0 C11 1 0.557284 0.522388 0.470721 11.00000 0.05079 0.02376 = 0.02863 -0.00028 -0.00482 0.00998 AFIX 43 H11 2 0.413066 0.526392 0.489780 11.00000 -1.20000 AFIX 0 C12 1 0.708980 0.207434 0.425649 11.00000 0.04442 0.02275 = 0.04245 -0.00230 -0.01044 0.00651 AFIX 137 H12A 2 0.855206 0.235573 0.407174 11.00000 -1.50000 H12B 2 0.673108 0.095790 0.420102 11.00000 -1.50000 H12C 2 0.731890 0.226699 0.462171 11.00000 -1.50000 AFIX 0 HKLF 4 REM w360817_1_1_a.res in P2(1)2(1)2(1) REM R1 = 0.0335 for 1846 Fo > 4sig(Fo) and 0.0352 for all 1953 data REM 146 parameters refined using 0 restraints END WGHT 0.0447 0.1222 REM Highest difference peak 0.121, deepest hole -0.194, 1-sigma level 0.041 Q1 1 0.5932 0.0279 0.4880 11.00000 0.05 0.12 Q2 1 0.6589 0.7691 0.3051 11.00000 0.05 0.12 Q3 1 -0.0427 0.7438 0.3306 11.00000 0.05 0.12 Q4 1 -0.1073 0.5171 0.3199 11.00000 0.05 0.11 Q5 1 -0.0584 0.4974 0.3287 11.00000 0.05 0.11 Q6 1 0.6614 0.6410 0.2320 11.00000 0.05 0.11 Q7 1 0.2352 0.5253 0.4724 11.00000 0.05 0.11 Q8 1 0.1366 0.6137 0.5198 11.00000 0.05 0.11 Q9 1 0.4080 1.0360 0.3663 11.00000 0.05 0.11 Q10 1 0.7147 0.6813 0.3194 11.00000 0.05 0.11 Q11 1 0.2641 0.4142 0.4900 11.00000 0.05 0.11 Q12 1 0.7215 0.8279 0.4517 11.00000 0.05 0.11 Q13 1 -0.0467 0.5220 0.4235 11.00000 0.05 0.10 Q14 1 0.8856 0.2485 0.4338 11.00000 0.05 0.10 Q15 1 0.2238 0.5031 0.5228 11.00000 0.05 0.10 Q16 1 0.4339 0.5131 0.2325 11.00000 0.05 0.10 Q17 1 0.3639 1.0391 0.3319 11.00000 0.05 0.10 Q18 1 0.6947 0.5774 0.3206 11.00000 0.05 0.10 Q19 1 0.2547 0.4793 0.3192 11.00000 0.05 0.10 Q20 1 0.3717 0.6325 0.3210 11.00000 0.05 0.10 ; _shelx_res_checksum 13515 _shelx_hkl_file ; 0 0 -2 83.69 4.03 0 0 -3 0.50 0.88 0 0 -4 3203.59 91.88 0 0 -5 1.69 1.69 0 0 -6 7565.86 211.23 0 0 -6 7450.39 207.26 0 0 -7 -0.18 1.42 0 0 -7 -0.41 2.34 0 0 -8 5757.40 160.10 0 0 8 5531.04 160.81 0 0 -8 5371.74 154.19 0 0 -9 1.72 2.05 0 0 -9 -0.56 2.21 0 0 9 -0.61 2.44 0 0 -10 7297.26 209.00 0 0 -10 7803.81 216.71 0 0 10 7424.86 217.39 0 0 -11 1.93 2.05 0 0 -11 -0.72 2.85 0 0 11 1.59 2.93 0 0 -12 893.04 30.90 0 0 -12 875.69 37.59 0 0 12 850.54 38.67 0 0 13 -1.01 3.06 0 0 -13 -0.90 3.17 0 0 -13 2.04 2.46 0 0 -14 1535.48 50.61 0 0 14 1439.64 60.72 0 0 -14 1554.61 59.38 0 0 -15 1.10 3.32 0 0 -15 1.00 2.51 0 0 15 -1.25 4.00 0 0 -16 87.42 8.43 0 0 16 99.46 13.50 0 0 -16 113.75 13.28 0 0 -17 2.65 3.99 0 0 17 -1.52 3.96 0 0 -17 1.21 2.81 0 0 -18 60.14 7.70 0 0 18 71.31 12.49 0 0 -19 1.96 3.19 0 0 19 3.60 5.75 0 0 -19 -2.81 3.51 0 0 -20 91.56 9.67 0 0 20 75.34 14.03 0 0 -20 97.62 10.01 0 0 -21 1.45 3.19 0 0 21 -2.05 3.78 0 0 -21 0.79 3.37 0 0 -21 -1.92 5.79 0 0 -22 9.95 6.36 0 0 -22 2.47 3.41 0 0 22 8.58 6.46 0 0 -22 7.51 4.24 0 0 -23 -0.76 3.82 0 0 -23 0.84 3.12 0 0 23 2.20 3.32 0 0 -23 -2.02 4.31 0 0 24 33.37 11.45 0 0 -24 50.33 7.75 0 0 -24 59.90 8.50 0 0 -24 50.56 12.08 0 0 25 -2.19 4.67 0 0 -25 -1.99 4.24 0 0 -25 2.23 3.36 0 0 -26 6.36 4.06 0 0 -27 -0.65 3.41 0 0 -28 27.39 5.36 0 0 -29 -2.01 2.78 0 0 -30 19.85 3.78 0 0 -31 -1.33 2.23 0 0 -32 10.89 2.14 0 -1 0 0.71 0.97 0 1 0 -1.64 1.12 0 1 -1 1815.14 52.78 0 1 1 1915.86 53.89 0 -1 1 1779.32 52.27 0 1 -1 1833.25 53.90 0 1 -2 796.93 25.27 0 -1 2 767.38 24.01 0 1 -2 818.49 26.06 0 -1 3 1678.42 49.11 0 1 -3 1687.25 51.11 0 1 -3 1695.83 51.65 0 1 -4 4.27 2.02 0 1 -4 8.24 2.30 0 1 -5 246.24 12.90 0 1 -5 270.58 10.30 0 1 -5 269.03 13.42 0 1 -6 3759.60 104.29 0 1 -6 3648.88 108.97 0 -1 -6 3613.75 103.37 0 1 -7 1441.33 49.07 0 -1 -7 1422.53 43.18 0 1 -7 1479.64 44.08 0 -1 -8 283.83 11.62 0 -1 -8 297.28 15.47 0 1 -8 297.41 16.35 0 1 -8 278.54 12.10 0 1 8 285.61 16.27 0 -1 -9 2321.94 68.92 0 1 -9 2376.17 69.79 0 1 9 2192.48 76.33 0 1 -9 2357.31 77.38 0 -1 -9 2458.86 75.63 0 -1 -10 2108.26 72.62 0 1 10 2290.76 75.86 0 1 -10 2258.29 67.36 0 -1 10 2120.81 74.40 0 -1 -10 2267.02 66.45 0 1 -10 2258.32 75.54 0 -1 11 294.98 18.94 0 -1 -11 261.33 17.05 0 1 11 283.34 19.13 0 1 -11 320.00 19.72 0 1 -11 301.59 13.81 0 -1 -11 282.49 12.99 0 1 12 4585.86 148.30 0 -1 -12 4695.26 136.14 0 -1 12 4707.85 147.45 0 -1 -12 4791.62 145.93 0 1 -12 4799.86 137.08 0 1 13 2766.08 94.95 0 -1 13 2605.68 93.96 0 -1 -13 2741.40 82.73 0 -1 -13 2543.64 91.02 0 1 -13 2903.20 83.91 0 -1 14 668.98 36.12 0 -1 -14 718.45 27.56 0 -1 -14 739.91 35.51 0 1 14 721.66 37.31 0 1 -14 709.50 27.95 0 -1 -15 71.81 7.13 0 -1 15 65.70 10.60 0 1 -15 66.44 7.13 0 -1 -15 71.97 10.35 0 1 15 77.95 11.49 0 -1 16 78.14 12.46 0 1 -16 63.66 11.06 0 -1 -16 88.02 8.33 0 1 16 92.90 13.20 0 1 -16 83.71 8.29 0 -1 -16 80.93 11.32 0 1 -17 195.43 13.63 0 1 17 200.06 20.21 0 -1 -17 212.17 13.65 0 -1 17 212.46 20.60 0 1 -17 212.09 20.66 0 -1 -17 203.56 19.07 0 -1 -17 205.32 13.42 0 1 -18 101.67 10.07 0 -1 -18 99.28 9.49 0 -1 -18 91.20 13.22 0 -1 18 116.65 15.84 0 -1 -18 114.47 10.11 0 1 18 88.30 14.17 0 1 -18 89.47 13.92 0 1 -19 849.63 35.72 0 -1 -19 879.46 46.85 0 -1 -19 805.13 34.58 0 -1 19 867.18 48.75 0 1 -19 787.34 46.23 0 1 19 810.01 47.63 0 -1 -19 853.78 34.84 0 1 -20 1.85 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9871.97 275.99 0 -2 0 9999.00 277.01 0 2 0 9968.94 278.86 0 2 1 766.74 27.79 0 2 -1 767.00 25.81 0 -2 1 746.16 25.70 0 2 -1 775.00 28.04 0 2 2 1682.30 53.21 0 2 -2 1642.71 51.15 0 2 -2 1659.52 53.54 0 -2 2 1665.64 50.40 0 2 -3 3101.48 91.72 0 2 -3 3223.26 93.88 0 -2 3 3045.95 89.72 0 2 -4 4835.54 141.60 0 2 -4 4972.65 143.53 0 2 -5 966.70 35.79 0 2 -5 971.52 34.38 0 -2 -5 934.82 29.37 0 -2 -6 4694.79 133.87 0 2 -6 4765.73 142.25 0 2 -6 4828.56 140.76 0 2 6 4904.13 142.60 0 2 7 2330.50 77.45 0 2 -7 2347.40 75.86 0 2 -7 2421.44 77.04 0 -2 -7 2341.54 68.65 0 2 8 1416.00 51.38 0 2 -8 1409.56 50.34 0 -2 -8 1361.20 42.63 0 2 -8 1406.42 51.03 0 2 -9 1.57 3.35 0 2 9 0.80 3.53 0 -2 -9 -0.27 1.62 0 2 -9 -2.22 3.05 0 2 -10 336.38 15.09 0 2 -10 327.96 20.34 0 2 10 340.95 21.06 0 2 -10 299.56 20.00 0 -2 -10 329.45 14.18 0 2 -11 180.10 10.55 0 -2 -11 181.44 9.88 0 2 11 175.37 15.40 0 2 -11 161.26 14.47 0 -2 -11 154.57 13.14 0 2 -11 193.09 15.67 0 -2 -12 57.18 8.10 0 2 -12 43.68 8.45 0 2 -12 41.57 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-5 2 3.59 2.89 -5 -5 2 3.09 2.17 -5 -5 3 14.14 4.03 -5 -5 3 7.52 2.33 -5 -5 4 76.99 7.44 -5 -5 4 62.62 5.13 -5 -5 5 23.89 4.60 -5 -5 5 14.01 2.37 -5 -5 6 64.82 6.70 -5 -5 7 21.33 4.11 -5 -5 8 50.48 5.64 -5 -5 11 3.31 2.03 -5 -5 12 5.18 1.92 -5 -6 -13 12.60 1.72 -5 -6 -12 6.12 1.67 -5 -6 -11 31.21 3.16 -5 -6 -10 16.00 2.55 -5 -6 -10 16.83 2.64 -5 -6 -9 108.58 6.85 -5 -6 -9 111.10 6.73 -5 -6 -8 18.36 3.23 -5 -6 -8 14.13 2.73 -5 -6 -7 6.10 2.35 -5 -6 -7 1.39 1.81 -5 -6 -6 21.52 3.50 -5 -6 -6 26.94 3.56 -5 -6 -5 146.60 8.94 -5 -6 -5 127.64 7.76 -5 -6 -4 31.16 4.31 -5 -6 -4 20.30 3.16 -5 -6 -3 3.80 2.37 -5 -6 -2 32.82 4.56 -5 -6 -2 44.20 4.35 -5 -6 -1 5.82 2.62 -5 -6 -1 6.83 2.10 -5 -6 0 48.78 5.33 -5 -6 0 44.16 4.09 -5 -6 1 9.16 3.00 -5 -6 1 7.31 1.94 -5 -6 2 34.72 4.66 -5 -6 2 29.61 2.90 -5 -6 3 1.81 2.07 -5 -6 4 17.98 3.43 -5 -6 5 118.81 7.82 -5 -6 7 4.04 2.07 -5 -6 8 12.32 2.29 -5 -6 9 82.73 5.10 -5 -7 -7 13.32 1.80 -5 -7 -6 22.63 2.46 -5 -7 -5 23.52 2.64 -5 -7 -4 -0.20 1.32 -5 -7 -3 11.28 2.13 -5 -7 -2 72.30 5.01 -5 -7 -1 11.62 2.17 -5 -7 0 1.03 1.35 -5 -7 1 8.96 1.92 -5 -7 3 8.71 1.60 -6 0 0 118.62 9.28 -6 0 1 15.70 4.14 -6 0 -1 12.05 3.62 -6 0 -1 16.91 4.44 -6 0 2 21.86 4.37 -6 0 -2 12.03 3.79 -6 0 -2 13.34 3.90 -6 0 3 99.20 8.26 -6 0 -3 85.06 8.04 -6 0 -3 108.15 8.55 -6 0 4 434.00 19.12 -6 0 -4 414.51 19.39 -6 0 -4 437.12 19.28 -6 0 -5 69.33 6.95 -6 0 -5 68.89 6.93 -6 0 5 57.65 6.64 -6 0 6 14.32 3.90 -6 0 -6 17.00 4.07 -6 0 -6 15.85 4.02 -6 0 7 25.12 3.99 -6 0 -7 16.57 3.77 -6 0 -7 23.82 4.30 -6 0 8 0.30 2.05 -6 0 -8 -1.95 2.49 -6 0 -8 -0.78 2.51 -6 0 9 0.76 1.92 -6 0 -9 1.08 2.33 -6 0 -9 1.48 2.29 -6 0 -10 118.06 7.98 -6 0 -11 39.14 4.66 -6 0 -12 6.83 2.58 -6 0 -13 278.63 12.30 -6 0 -14 28.93 3.35 -6 0 -15 0.20 1.38 -6 0 -16 4.76 1.54 -6 -1 -16 20.58 2.20 -6 -1 -15 16.90 2.40 -6 -1 -14 11.97 2.44 -6 -1 -13 29.18 3.46 -6 -1 -12 2.22 2.10 -6 -1 -11 10.94 2.91 -6 -1 -10 3.59 2.31 -6 -1 -10 6.53 2.63 -6 -1 -9 24.30 3.93 -6 -1 -9 27.07 4.13 -6 1 8 38.84 4.65 -6 -1 -8 52.19 5.60 -6 -1 -8 54.00 5.48 -6 -1 -7 25.24 4.34 -6 -1 -7 33.42 4.66 -6 1 6 11.65 3.30 -6 -1 -6 11.03 3.43 -6 -1 -6 18.43 3.96 -6 -1 -5 11.86 3.40 -6 -1 -5 10.85 3.47 -6 1 4 12.64 3.73 -6 -1 -4 13.10 3.62 -6 -1 -4 10.22 3.42 -6 1 3 187.26 11.62 -6 -1 -3 186.16 11.67 -6 -1 -3 198.92 11.57 -6 1 2 31.64 5.19 -6 -1 -2 34.25 5.33 -6 -1 -2 24.50 4.54 -6 1 1 211.00 12.65 -6 -1 -1 195.94 12.16 -6 -1 -1 206.54 12.00 -6 1 0 128.91 9.85 -6 -1 0 134.10 9.76 -6 1 -1 213.39 12.77 -6 -1 1 200.20 12.06 -6 1 -1 204.63 12.21 -6 -1 2 31.20 5.11 -6 1 -2 28.45 5.07 -6 -1 2 29.86 4.87 -6 1 -2 33.04 5.31 -6 1 -3 196.59 12.04 -6 -1 3 209.14 11.86 -6 1 -3 191.30 11.58 -6 -1 3 187.89 11.98 -6 -1 4 7.24 3.30 -6 1 -4 9.09 3.69 -6 1 -4 6.36 3.65 -6 -1 5 16.83 4.06 -6 -1 5 19.78 3.65 -6 1 -5 14.47 3.68 -6 1 -5 14.10 3.67 -6 -1 6 16.61 3.86 -6 -1 6 7.49 2.70 -6 1 -6 13.81 3.71 -6 1 -6 7.25 3.14 -6 -1 7 20.84 4.35 -6 -1 7 24.05 3.65 -6 1 -7 20.53 3.91 -6 1 -7 26.40 4.24 -6 -1 8 32.32 3.78 -6 1 -8 49.79 5.51 -6 1 -8 50.43 5.36 -6 -1 8 44.30 5.73 -6 -1 9 20.94 4.15 -6 -1 9 12.13 2.28 -6 1 -9 24.59 3.90 -6 1 -10 9.20 3.02 -6 1 -11 12.14 2.86 -6 1 -12 4.41 2.16 -6 1 -13 28.88 3.41 -6 1 -14 9.89 2.14 -6 1 -15 14.06 2.20 -6 1 -16 16.91 1.96 -6 -2 -11 77.20 5.73 -6 -2 -11 79.49 5.55 -6 -2 -10 31.32 3.94 -6 -2 -10 30.53 3.75 -6 -2 -9 66.61 5.81 -6 -2 -9 56.27 5.08 -6 -2 -8 23.69 3.83 -6 -2 -8 26.38 3.88 -6 2 7 23.23 3.98 -6 -2 -7 19.48 3.70 -6 -2 -6 35.47 4.80 -6 2 6 31.49 4.59 -6 2 5 31.55 4.75 -6 -2 -5 35.16 4.90 -6 2 4 117.96 8.60 -6 -2 -4 108.55 8.40 -6 2 3 28.71 4.79 -6 -2 -3 29.63 4.67 -6 2 2 18.44 3.94 -6 -2 -2 13.01 3.46 -6 2 1 54.66 6.20 -6 -2 -1 35.91 5.07 -6 2 0 66.94 6.94 -6 -2 0 76.04 6.88 -6 -2 0 66.62 6.68 -6 2 -1 46.25 5.81 -6 -2 1 42.54 5.25 -6 -2 1 42.76 5.51 -6 -2 2 5.95 3.02 -6 2 -2 13.59 3.71 -6 -2 3 21.21 4.39 -6 2 -3 26.12 4.56 -6 2 -4 104.29 8.33 -6 -2 4 115.69 7.88 -6 2 -4 127.29 8.61 -6 -2 4 108.66 8.77 -6 -2 5 25.15 4.64 -6 2 -5 26.87 4.60 -6 -2 5 30.41 3.95 -6 2 -5 34.61 4.66 -6 -2 6 33.27 4.99 -6 2 -6 33.52 4.81 -6 -2 6 28.45 3.70 -6 2 -6 38.91 4.71 -6 -2 7 20.03 3.97 -6 2 -7 19.26 3.64 -6 -2 7 14.74 2.54 -6 2 -7 19.56 3.44 -6 -2 8 22.90 4.37 -6 2 -8 31.89 4.08 -6 2 -9 66.43 5.54 -6 -2 9 65.19 6.21 -6 -2 10 28.10 4.13 -6 2 -10 26.42 3.55 -6 -3 -12 38.32 3.37 -6 -3 -11 55.44 4.37 -6 -3 -10 5.00 2.07 -6 -3 -9 71.50 5.57 -6 -3 -9 56.84 3.94 -6 -3 -8 8.68 2.41 -6 -3 -8 5.46 1.77 -6 -3 -7 2.86 2.28 -6 -3 -6 12.28 3.04 -6 -3 -5 154.83 9.28 -6 -3 -4 7.36 2.62 -6 3 3 108.01 8.09 -6 -3 -3 117.52 8.03 -6 3 2 37.83 5.09 -6 -3 -2 31.38 4.42 -6 -3 -2 36.55 4.68 -6 3 1 63.74 6.41 -6 -3 -1 70.90 6.24 -6 -3 -1 74.60 6.56 -6 3 0 105.43 7.89 -6 -3 0 86.24 6.90 -6 -3 0 102.02 7.82 -6 3 -1 56.12 6.19 -6 -3 1 64.57 6.25 -6 -3 2 35.05 4.22 -6 3 -2 34.34 4.92 -6 -3 2 38.24 4.99 -6 3 -3 119.62 8.38 -6 -3 3 109.54 7.15 -6 -3 3 122.79 8.67 -6 -3 4 7.75 2.92 -6 3 -4 4.11 2.76 -6 -3 4 5.75 2.14 -6 3 -5 125.39 8.25 -6 -3 5 119.21 6.67 -6 -3 6 7.75 2.86 -6 -3 6 5.81 1.50 -6 -3 7 1.49 2.20 -6 -3 8 10.48 3.19 -6 -3 9 77.66 6.20 -6 -3 10 2.33 1.81 -6 -4 -11 8.30 1.44 -6 -4 -10 25.83 2.72 -6 -4 -9 52.02 4.10 -6 -4 -8 15.71 2.51 -6 -4 -7 28.08 3.39 -6 -4 -6 45.33 4.34 -6 -4 -5 120.62 7.23 -6 -4 -4 20.69 3.15 -6 -4 -3 20.95 3.40 -6 -4 -3 16.29 2.94 -6 -4 -2 121.62 7.23 -6 -4 -2 132.02 7.98 -6 -4 -1 207.76 10.82 -6 -4 0 187.17 9.17 -6 -4 0 194.91 10.41 -6 -4 1 199.43 9.20 -6 -4 1 210.01 10.87 -6 -4 2 96.95 5.70 -6 -4 2 131.77 8.07 -6 -4 3 14.70 3.20 -6 -4 3 15.17 2.04 -6 -4 4 25.24 3.81 -6 -4 5 114.61 7.50 -6 -4 6 40.89 4.34 -6 -4 7 28.13 3.59 -6 -4 8 12.89 2.60 -6 -4 9 53.28 4.20 -6 -5 -5 10.59 1.60 -6 -5 -4 24.29 2.54 -6 -5 -3 9.92 1.87 -6 -5 -2 1.78 1.30 -6 -5 -1 1.67 1.40 -6 -5 0 52.48 4.18 -6 -5 1 -0.43 1.33 -6 -5 2 0.42 1.40 -6 -5 3 11.95 2.11 -6 -5 4 17.02 2.43 -6 -5 5 11.82 1.91 TITL w360817_1_1 in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 1.54184 5.477659 8.319361 25.687867 90.0000 90.0000 90.0000 ZERR 4.00 0.000093 0.000162 0.000483 0.0000 0.0000 0.0000 LATT -1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O UNIT 48.00 60.00 4.00 12.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 41080 _olex2_date_sample_data_collection 2017-10-02 _olex2_date_sample_submission 2017-10-02 _olex2_submission_original_sample_id w360817_1_1 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.294 _oxdiff_exptl_absorpt_empirical_full_min 0.801 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 O1 O 0.2011(3) 0.99696(19) 0.36517(6) 0.0325(4) Uani 1 1 d . . . . . O2 O -0.0537(3) 0.8160(2) 0.39084(8) 0.0390(5) Uani 1 1 d . . . . . O3 O 0.7451(4) 0.5426(2) 0.49387(7) 0.0562(6) Uani 1 1 d . . . . . N1 N 0.1542(3) 0.8669(2) 0.38480(7) 0.0234(4) Uani 1 1 d . . . . . C1 C 0.3072(4) 0.5667(2) 0.33054(8) 0.0192(4) Uani 1 1 d . . . . . C2 C 0.3262(4) 0.5887(2) 0.38934(8) 0.0201(4) Uani 1 1 d . . . . . H2 H 0.173175 0.551753 0.405088 0.024 Uiso 1 1 calc R . . . . C3 C 0.1129(4) 0.4829(3) 0.30864(8) 0.0249(5) Uani 1 1 d . . . . . H3 H -0.004896 0.437203 0.330104 0.030 Uiso 1 1 calc R . . . . C4 C 0.4829(4) 0.6317(3) 0.29768(8) 0.0243(5) Uani 1 1 d . . . . . H4 H 0.615173 0.686651 0.311788 0.029 Uiso 1 1 calc R . . . . C5 C 0.5376(4) 0.4912(3) 0.41328(7) 0.0211(4) Uani 1 1 d . . . . . H5 H 0.690878 0.522518 0.396412 0.025 Uiso 1 1 calc R . . . . C6 C 0.4982(4) 0.3090(3) 0.40588(9) 0.0268(5) Uani 1 1 d . . . . . H6A H 0.350456 0.277510 0.424016 0.032 Uiso 1 1 calc R . . . . H6B H 0.474366 0.287143 0.369140 0.032 Uiso 1 1 calc R . . . . C7 C 0.3615(4) 0.7658(3) 0.40335(8) 0.0221(5) Uani 1 1 d . . . . . H7A H 0.376011 0.776116 0.440831 0.026 Uiso 1 1 calc R . . . . H7B H 0.511996 0.804305 0.387866 0.026 Uiso 1 1 calc R . . . . C8 C 0.0936(4) 0.4668(3) 0.25495(8) 0.0279(5) Uani 1 1 d . . . . . H8 H -0.036825 0.410433 0.240669 0.033 Uiso 1 1 calc R . . . . C9 C 0.2674(4) 0.5343(3) 0.22277(8) 0.0276(5) Uani 1 1 d . . . . . H9 H 0.252665 0.525111 0.186826 0.033 Uiso 1 1 calc R . . . . C10 C 0.4634(4) 0.6157(3) 0.24409(8) 0.0279(5) Uani 1 1 d . . . . . H10 H 0.582235 0.659707 0.222505 0.034 Uiso 1 1 calc R . . . . C11 C 0.5573(5) 0.5224(3) 0.47072(9) 0.0344(6) Uani 1 1 d . . . . . H11 H 0.413066 0.526392 0.489780 0.041 Uiso 1 1 calc R . . . . C12 C 0.7090(5) 0.2074(3) 0.42565(10) 0.0365(6) Uani 1 1 d . . . . . H12A H 0.855206 0.235573 0.407174 0.055 Uiso 1 1 calc GR . . . . H12B H 0.673108 0.095790 0.420102 0.055 Uiso 1 1 calc GR . . . . H12C H 0.731890 0.226699 0.462171 0.055 Uiso 1 1 calc GR . . . . 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 O1 0.0357(8) 0.0235(8) 0.0384(9) 0.0057(7) -0.0021(7) -0.0004(8) O2 0.0173(7) 0.0264(8) 0.0734(13) 0.0005(9) 0.0030(8) -0.0006(7) O3 0.0762(14) 0.0481(12) 0.0443(11) -0.0167(9) -0.0346(11) 0.0159(11) N1 0.0201(8) 0.0210(9) 0.0290(9) -0.0056(7) -0.0004(8) 0.0006(8) C1 0.0187(9) 0.0151(9) 0.0237(10) -0.0014(7) -0.0015(9) 0.0046(8) C2 0.0178(9) 0.0191(10) 0.0234(10) -0.0032(8) 0.0014(8) -0.0005(8) C3 0.0196(9) 0.0242(11) 0.0308(11) -0.0020(10) 0.0013(9) -0.0004(9) C4 0.0234(10) 0.0215(10) 0.0280(11) -0.0009(9) -0.0010(9) -0.0007(9) C5 0.0207(9) 0.0208(11) 0.0218(10) -0.0021(8) -0.0002(8) 0.0008(9) C6 0.0298(11) 0.0201(11) 0.0306(11) -0.0025(9) -0.0052(9) -0.0004(10) C7 0.0179(9) 0.0216(11) 0.0267(11) -0.0058(9) -0.0035(9) 0.0026(9) C8 0.0241(10) 0.0293(12) 0.0302(11) -0.0067(10) -0.0065(9) 0.0007(9) C9 0.0333(11) 0.0281(12) 0.0215(10) -0.0040(9) -0.0048(9) 0.0077(10) C10 0.0303(11) 0.0272(12) 0.0262(11) 0.0025(9) 0.0037(10) 0.0017(10) C11 0.0508(14) 0.0238(12) 0.0286(12) -0.0003(10) -0.0048(12) 0.0100(11) C12 0.0444(13) 0.0227(12) 0.0425(14) -0.0023(10) -0.0104(12) 0.0065(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -2 -4 -4 0.0427 -1 -5 -2 0.0414 1 -5 1 0.0453 3 1 5 0.0745 1 5 -1 0.0342 -3 1 -5 0.0620 0 0 -17 0.0431 0 1 16 0.0327 1 3 -13 0.0481 3 2 -9 0.0773 -3 1 -1 0.0601 -2 -3 12 0.0489 1 -3 13 0.0508 3 -1 -9 0.0755 0 1 -16 0.0426 -1 0 16 0.0335 0 -2 -15 0.0495 1 -4 -8 0.0528 -1 -3 -12 0.0416 2 -4 6 0.0505 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 N1 O2 123.66(18) . . ? O1 N1 C7 118.14(17) . . ? O2 N1 C7 118.20(17) . . ? C3 C1 C2 120.84(17) . . ? C4 C1 C2 120.52(18) . . ? C4 C1 C3 118.63(19) . . ? C1 C2 H2 108.2 . . ? C1 C2 C5 112.54(16) . . ? C1 C2 C7 110.91(16) . . ? C5 C2 H2 108.2 . . ? C7 C2 H2 108.2 . . ? C7 C2 C5 108.55(16) . . ? C1 C3 H3 119.7 . . ? C8 C3 C1 120.52(19) . . ? C8 C3 H3 119.7 . . ? C1 C4 H4 119.6 . . ? C10 C4 C1 120.8(2) . . ? C10 C4 H4 119.6 . . ? C2 C5 H5 109.1 . . ? C2 C5 C6 111.25(16) . . ? C6 C5 H5 109.1 . . ? C11 C5 C2 110.77(17) . . ? C11 C5 H5 109.1 . . ? C11 C5 C6 107.52(18) . . ? C5 C6 H6A 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? C12 C6 C5 113.53(18) . . ? C12 C6 H6A 108.9 . . ? C12 C6 H6B 108.9 . . ? N1 C7 C2 111.86(16) . . ? N1 C7 H7A 109.2 . . ? N1 C7 H7B 109.2 . . ? C2 C7 H7A 109.2 . . ? C2 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C3 C8 H8 119.9 . . ? C9 C8 C3 120.2(2) . . ? C9 C8 H8 119.9 . . ? C8 C9 H9 120.1 . . ? C8 C9 C10 119.9(2) . . ? C10 C9 H9 120.1 . . ? C4 C10 H10 120.0 . . ? C9 C10 C4 120.0(2) . . ? C9 C10 H10 120.0 . . ? O3 C11 C5 124.9(2) . . ? O3 C11 H11 117.5 . . ? C5 C11 H11 117.5 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 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 N1 1.221(2) . ? O2 N1 1.225(2) . ? O3 C11 1.200(3) . ? N1 C7 1.491(3) . ? C1 C2 1.525(3) . ? C1 C3 1.391(3) . ? C1 C4 1.390(3) . ? C2 H2 0.9800 . ? C2 C5 1.542(3) . ? C2 C7 1.529(3) . ? C3 H3 0.9300 . ? C3 C8 1.390(3) . ? C4 H4 0.9300 . ? C4 C10 1.387(3) . ? C5 H5 0.9800 . ? C5 C6 1.542(3) . ? C5 C11 1.502(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C12 1.518(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8 0.9300 . ? C8 C9 1.380(3) . ? C9 H9 0.9300 . ? C9 C10 1.383(3) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -2.0000 -4.0000 -3.9997 -0.8910 -0.1510 0.3243 -1.0000 -5.0000 -1.9999 -0.9546 -0.1963 -0.0246 1.0000 -5.0000 0.9999 -0.7614 -0.1520 -0.5809 3.0000 1.0000 4.9996 0.4690 0.0795 -0.7806 1.0000 5.0000 -1.0001 0.8973 0.3590 0.0758 -3.0000 1.0000 -4.9996 -0.1296 0.0010 0.9051 -0.0000 0.0000 -16.9999 -0.3246 0.9219 0.2899 0.0000 1.0000 15.9999 0.4752 -0.8275 -0.2106 1.0000 3.0000 -13.0001 0.3288 0.9293 0.1559 3.0000 2.0000 -9.0003 0.3714 0.8790 -0.4796 -3.0000 1.0000 -0.9996 -0.0532 -0.2159 0.8369 -2.0000 -3.0000 12.0002 -0.4158 -0.9785 0.1137 1.0000 -3.0000 12.9998 -0.1929 -0.7223 -0.6610 3.0000 -1.0000 -9.0003 -0.1377 0.7582 -0.6664 -0.0000 1.0000 -15.9999 -0.1358 0.9080 0.3351 -1.0000 -0.0000 16.0001 0.2376 -0.9712 -0.0204 -0.0000 -2.0000 -14.9999 -0.6258 0.7330 0.1313 1.0000 -4.0000 -8.0001 -0.7636 0.3763 -0.3651 -1.0000 -3.0000 -11.9998 -0.8062 0.4265 0.2704 2.0000 -4.0000 5.9997 -0.4283 -0.2795 -0.8564