#------------------------------------------------------------------------------ #$Date: 2025-08-21 23:24:23 +0100 (Thu, 21 Aug 2025) $ #$Revision: 301857 $ #$URL: svn://www.crystallography.net/cod/cif/7/11/26/7112617.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_7112617 loop_ _publ_author_name 'Zhen Wang' 'Qian Yao' 'Tengfei Kang' 'Juhua Feng' 'Xiaohua Liu' 'Lili Lin' 'Xiaoming Feng' _publ_section_title ; Highly diastereo- and enantioselective Michael addition of 3-substituted benzofuran-2(3H)-ones to 4-oxo-enoates catalyzed by lanthanide(III) complexes ; _journal_name_full Chem.Commun. _journal_page_first 4918 _journal_paper_doi 10.1039/C4CC01499E _journal_volume 50 _journal_year 2014 _chemical_absolute_configuration unk _chemical_formula_moiety 'C25 H22 O5 S' _chemical_formula_sum 'C25 H22 O5 S' _chemical_formula_weight 434.48 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2013-09-10 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _cell_angle_alpha 90 _cell_angle_beta 104.370(5) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.7042(4) _cell_length_b 15.7653(7) _cell_length_c 9.1879(4) _cell_measurement_reflns_used 1506 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.0022 _cell_measurement_theta_min 3.0138 _cell_volume 1081.04(9) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL-2012, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _diffrn_ambient_temperature 293.15 _diffrn_detector_area_resol_mean 16.0874 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; 1 omega -73.00 -39.00 1.0000 1.8000 omega____ theta____ kappa____ phi______ frames - -17.5174 -178.0000 -30.0000 34 2 omega -22.00 5.00 1.0000 1.8000 omega____ theta____ kappa____ phi______ frames - -17.5174 -99.0000 -30.0000 27 3 omega -36.00 54.00 1.0000 1.8000 omega____ theta____ kappa____ phi______ frames - -17.5174 38.0000 -30.0000 90 4 omega 37.00 89.00 1.0000 1.8000 omega____ theta____ kappa____ phi______ frames - 19.3143 77.0000 -150.0000 52 5 omega -49.00 -24.00 1.0000 1.8000 omega____ theta____ kappa____ phi______ frames - 19.3143 -57.0000 -180.0000 25 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0460970000 _diffrn_orient_matrix_UB_12 0.0257578000 _diffrn_orient_matrix_UB_13 -0.0414321000 _diffrn_orient_matrix_UB_21 0.0672093000 _diffrn_orient_matrix_UB_22 -0.0315624000 _diffrn_orient_matrix_UB_23 0.0071575000 _diffrn_orient_matrix_UB_31 -0.0488852000 _diffrn_orient_matrix_UB_32 -0.0191076000 _diffrn_orient_matrix_UB_33 -0.0676932000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_unetI/netI 0.0562 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 4739 _diffrn_reflns_point_group_measured_fraction_full 0.791 _diffrn_reflns_point_group_measured_fraction_max 0.776 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.365 _diffrn_reflns_theta_min 3.020 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.184 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.95000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.335 _exptl_crystal_description block _exptl_crystal_F_000 456 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.201 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.054 _refine_ls_abs_structure_details ; Flack x determined using 755 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.13(11) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 282 _refine_ls_number_reflns 3432 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0548 _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^)+(0.0683P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1238 _refine_ls_wR_factor_ref 0.1396 _reflns_Friedel_coverage 0.498 _reflns_Friedel_fraction_full 0.567 _reflns_Friedel_fraction_max 0.536 _reflns_number_gt 2655 _reflns_number_total 3432 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c4cc01499e2.cif _cod_data_source_block 130909_s1_wz _cod_original_cell_volume 1081.03(9) _cod_database_code 7112617 #BEGIN Tags that were not found in dictionaries: _chemical_oxdiff_formula C25H22O5S1 _reflns_odcompleteness_completeness 99.78 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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: C7(H7), C23(H23) 2.b Secondary CH2 refined with riding coordinates: C6(H6A,H6B) 2.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21) 2.d Idealised Me refined as rotating group: C24(H24A,H24B,H24C), C25(H25A,H25B,H25C) ; _shelx_estimated_absorpt_t_max 0.964 _shelx_estimated_absorpt_t_min 0.947 _shelx_hkl_checksum 60717 _shelx_hkl_file ; 0 -21 2 7560.09 1373.23 5 0 -19 1 95.6833 234.172 5 0 -18 0 2148.65 668.020 5 0 -17 0 328.904 291.175 5 0 -17 -1 654.267 394.443 5 0 -16 0 6562.67 1002.19 5 0 -16 -1 1073.01 404.479 5 0 -15 -1 1187.42 437.784 5 0 -15 -2 4277.22 675.458 5 0 -14 -1 2974.00 576.584 5 0 -14 -2 3748.27 606.417 5 0 -13 -1 16671.6 1323.09 5 0 -13 -2 9812.53 932.432 5 0 -12 -1 7488.47 836.578 5 0 -12 -2 26815.7 1444.14 5 0 -11 -1 12599.1 1039.61 5 0 -11 -2 21003.3 1207.15 5 0 -10 -1 39754.8 1741.84 5 0 -10 -2 15529.5 976.620 5 0 -9 -2 3975.26 465.660 5 0 -8 -2 235163. 3267.71 5 0 -7 -2 70007.7 1629.85 5 0 -6 0 218169. 2929.43 1 0 -6 1 328251. 2921.51 1 0 -6 2 38850.7 700.743 1 0 -6 5 1949.13 215.759 1 0 -6 6 10325.8 608.845 1 0 -5 0-12.6560 62.6392 1 0 -5 -1 78803.3 1588.34 5 0 -5 1 81169.8 1273.03 1 0 -5 4 7505.81 388.835 1 0 -5 5 9681.34 564.298 1 0 -5 6 16527.9 863.005 1 0 -5 6 18137.9 1498.23 2 0 -5 7 19366.2 1661.01 2 0 -5 8 8327.15 1175.83 2 0 -5 9 2928.89 783.520 2 0 -5 10 1625.65 602.959 2 0 -4 0 622736. 4038.02 1 0 -4 1 302707. 2002.61 1 0 -4 -1 297175. 2647.61 5 0 -4 4 25782.7 851.937 1 0 -4 4 25918.3 1440.07 2 0 -4 5 7017.66 536.095 1 0 -4 5 6505.57 795.115 2 0 -4 -5 6629.84 344.613 3 0 -4 6 10399.7 1100.20 2 0 -4 6 9126.38 709.145 1 0 -4 -6 9021.34 489.015 3 0 -4 -7 3086.79 326.250 3 0 -4 7 2719.19 638.961 2 0 -4 8 172.957 227.470 2 0 -4 9 3793.65 870.019 2 0 -4 10 1335.42 581.539 2 0 -4 11 2724.66 820.730 2 0 -3 0 273.951 83.9517 1 0 -3 -1 198266. 1773.70 5 0 -3 -1 198524. 2548.29 1 0 -3 3 176570. 3173.13 2 0 -3 4 28877.4 1014.03 1 0 -3 -4 27338.9 716.120 3 0 -3 4 27660.6 1432.67 2 0 -3 5 24977.4 1528.88 2 0 -3 -5 22804.9 819.960 3 0 -3 5 23055.6 1070.92 1 0 -3 -6 10920.0 656.460 3 0 -3 6 10659.4 826.361 1 0 -3 6 12266.2 1181.70 2 0 -3 -7 37551.6 1345.34 3 0 -3 7 36717.5 2215.66 2 0 -3 8 492.712 260.739 2 0 -3 9 2435.22 707.137 2 0 -3 10 133.220 202.571 2 0 -3 11 1818.75 739.343 2 0 -2 2 171306. 2521.87 2 0 -2 3 7360.91 633.080 2 0 -2 -3 6979.21 348.309 3 0 -2 4 89001.0 1936.28 1 0 -2 4 91819.6 2527.61 2 0 -2 4 88890.0 1181.29 4 0 -2 -4 89092.1 1567.03 3 0 -2 5 83992.7 2194.06 1 0 -2 -5 81807.0 1779.05 3 0 -2 5 84835.1 2728.80 2 0 -2 5 82988.1 1389.57 4 0 -2 6 1556.05 427.599 2 0 -2 -6 1542.24 286.090 3 0 -2 6 1119.70 185.022 4 0 -2 -7 5621.50 585.204 3 0 -2 7 5898.78 875.021 2 0 -2 8 615.823 362.230 2 0 -2 -8 956.823 245.286 3 0 -2 9 94.7968 242.093 2 0 -2 10 4673.66 1012.40 2 0 -2 11 2057.51 711.603 2 0 -1 2 11585.2 616.208 2 0 -1 -2 10523.2 397.808 3 0 -1 -3 21716.3 757.702 3 0 -1 3 22979.6 1074.11 2 0 -1 3 22954.1 887.927 1 0 -1 4 98437.8 2197.14 1 0 -1 -4 92622.8 1888.41 3 0 -1 4 99214.0 2585.14 2 0 -1 -5 61069.9 1720.23 3 0 -1 5 65554.0 2362.99 2 0 -1 5 66604.2 2079.30 1 0 -1 -6 5139.74 555.796 3 0 -1 6 5066.05 719.445 2 0 -1 7 2619.94 362.610 4 0 -1 7 2815.76 616.861 2 0 -1 -7 2598.58 432.983 3 0 -1 8 10080.3 1246.93 2 0 -1 -8 9229.55 865.302 3 0 -1 9 3460.16 789.514 2 0 -1 10 4795.96 1000.93 2 0 -1 11 3076.23 838.049 2 0 0 -2 18229.3 659.257 3 0 0 2 19043.8 676.749 3 0 0 3 130334. 2298.53 1 0 0 -3 127937. 2131.80 3 0 0 -4 38669.9 1358.42 3 0 0 4 40980.9 1513.85 1 0 0 -5 37933.2 1485.03 3 0 0 -6 5325.18 620.565 3 0 0 7 27.4745 193.820 2 0 0 -7 17.7418 173.649 3 0 0 8 1011.72 458.652 2 0 0 -8 1026.55 348.005 3 0 0 9 748.826 381.704 2 0 0 -9 1162.67 373.924 3 0 0 10 4923.54 1066.56 2 0 0 11 535.697 333.746 2 0 1 2 11309.5 621.640 1 0 1 -2 10860.1 590.981 3 0 1 2 11109.6 420.310 3 0 1 3 22258.0 1020.44 1 0 1 -3 22331.4 993.107 3 0 1 -4 96378.3 2348.95 3 0 1 4 103525. 2536.28 1 0 1 -5 63628.2 2089.52 3 0 1 -6 5107.69 646.882 3 0 1 -7 2863.62 515.258 3 0 1 -8 9247.66 980.717 3 0 1 9 4432.13 912.425 2 0 1 -9 4263.39 710.080 3 0 1 10 4407.72 953.954 2 0 1 11 2387.32 770.512 2 0 2 -1 234173. 2583.78 3 0 2 1 232395. 2463.09 1 0 2 -2 174431. 2503.54 2 0 2 -2 171206. 2647.87 3 0 2 2 174817. 2652.81 1 0 2 -3 8008.51 652.323 3 0 2 3 8217.26 399.297 3 0 2 3 7509.87 638.525 1 0 2 -4 90895.3 2448.31 3 0 2 -5 83559.4 2555.91 3 0 2 -6 701.679 282.475 3 0 2 -7 6665.96 832.147 3 0 2 -8 1050.10 375.523 3 0 2 -9 625.249 339.656 3 0 2 10 4317.94 957.067 2 0 2 11 2054.56 756.132 2 0 3 0 166.877 73.0347 1 0 3 -1 201801. 2728.48 3 0 3 1 196625. 2568.34 1 0 3 -2 49493.9 1430.62 2 0 3 2 50285.9 1547.16 1 0 3 -2 47830.4 1554.69 3 0 3 -3 177561. 3074.97 2 0 3 -3 171259. 3241.45 3 0 3 -4 27861.1 1433.91 3 0 3 -5 21458.6 1373.78 3 0 3 -6 11218.1 1073.21 3 0 3 -7 36842.5 2047.91 3 0 3 -8 505.214 167.535 3 0 3 -9 2602.94 611.605 3 0 3 -10 471.721 317.861 3 0 3 11 486.130 364.023 2 0 4 0 609366. 3967.23 1 0 4 1 298022. 3388.97 1 0 4 -1 298826. 3735.57 3 0 4 2 135032. 2689.26 1 0 4 2 134911. 1634.36 5 0 4 -2 132522. 2789.57 3 0 4 -2 139101. 2575.79 2 0 4 -3 194982. 3704.20 3 0 4 -4 24809.8 1448.74 3 0 4 -5 5795.31 757.485 3 0 4 -6 9538.25 1030.81 3 0 4 -7 3198.05 636.769 3 0 4 -8 248.471 278.269 3 0 4 -9 2658.80 643.050 3 0 4 -10 1888.40 569.185 3 0 5 0 13.8403 73.7036 3 0 5 0 47.2644 59.8314 1 0 5 -1 79880.2 2098.44 3 0 5 1 76956.7 1883.10 1 0 5 -2 36962.6 1592.92 3 0 5 2 37591.6 1490.09 1 0 5 -3 12244.6 999.914 3 0 5 3 11382.2 533.701 5 0 5 -4 7615.49 842.404 3 0 5 -5 8727.46 977.801 3 0 5 -6 17846.7 1477.61 3 0 5 -7 19551.8 1615.80 3 0 5 -8 8293.71 1121.42 3 0 5 -9 1632.22 526.087 3 0 5 -10 1739.62 559.713 3 0 6 0 219329. 2933.94 1 0 6 0 215579. 3343.25 3 0 6 1 319111. 3590.15 3 0 6 -1 324898. 4563.62 3 0 6 1 326436. 4122.59 1 0 6 2 39940.1 1050.55 3 0 6 -2 41123.7 1787.27 3 0 6 3 13531.1 636.786 5 0 6 3 12281.5 404.014 3 0 6 -3 13586.6 1109.64 3 0 6 4 6472.09 444.708 5 0 6 -4 6327.13 803.938 3 0 6 -5 1831.74 463.420 3 0 6 -6 11009.8 1224.09 3 0 6 -7 1194.58 483.305 3 0 6 -8-766.848 376.817 3 0 6 -9-73.9472 298.929 3 0 6 -10 1959.05 606.061 3 0 7 0-22.5676 118.497 3 0 7 0 16.8093 96.5665 1 0 7 -1 6445.74 709.464 3 0 7 1 5140.79 504.969 3 0 7 1 5562.13 579.416 1 0 7 -2 71825.4 2511.70 3 0 7 2 70454.1 1609.38 3 0 7 -3 50170.1 2221.38 3 0 7 3 52025.5 1055.35 3 0 7 -4 245.502 74.7887 4 0 7 4 203.480 91.2827 5 0 7 -4 477.888 278.698 3 0 7 -5 41872.4 2303.90 3 0 7 5 43806.7 1228.18 5 0 7 -6 6064.08 927.157 3 0 7 -7 1949.92 573.292 3 0 7 -8 1639.54 534.029 3 0 7 -9 4150.26 890.148 3 0 7 -10 757.153 400.830 3 0 7 -11 4059.76 946.090 3 0 8 0 154591. 2887.40 1 0 8 0 149440. 3263.66 3 0 8 1 4361.26 517.378 3 0 8 -1 4176.37 592.121 3 0 8 -2 232624. 4751.81 3 0 8 2 240167. 3289.29 3 0 8 3 70179.3 1442.55 3 0 8 -3 71159.8 2775.09 3 0 8 -4 17862.2 1485.95 3 0 8 -5 5862.05 914.332 3 0 8 -6 24666.5 1947.68 3 0 8 -7 1368.64 509.710 3 0 8 -8 535.433 321.215 3 0 8 -9 402.841 288.447 3 0 8 -10-67.2168 432.573 3 0 8 -11 175.253 209.906 3 0 9 0 57.9532 158.817 3 0 9 0 47.0694 156.073 1 0 9 -1 24062.1 1496.74 3 0 9 1 26438.4 1341.95 3 0 9 -2 2267.82 508.001 3 0 9 2 1919.87 333.105 3 0 9 -3 37683.3 2126.15 3 0 9 3 39136.0 1230.23 3 0 9 -4 38593.8 2272.40 3 0 9 -5 25849.5 1964.30 3 0 9 -6 14343.9 1550.06 3 0 9 -7 1556.31 599.132 3 0 9 -8 2860.40 767.768 3 0 9 -9 1253.33 585.618 3 0 9 -10 2256.39 756.663 3 0 10 0 357.397 163.700 3 0 10 1 37462.3 1695.75 3 0 10 -1 37374.6 1954.16 3 0 10 2 16642.6 1024.64 3 0 10 -2 15005.8 1332.36 3 0 10 3 26469.7 1115.37 3 0 10 -3 37466.6 2197.68 3 0 10 4 38239.8 932.066 3 0 10 -4 37372.7 2339.06 3 0 10 -5 7035.77 1090.20 3 0 10 -6 5912.22 1030.70 3 0 10 -7 1362.00 504.100 3 0 10 -8 316.911 365.688 3 0 10 -9 1123.78 515.616 3 0 10 -10 462.615 328.368 3 0 11 0-28.4050 210.961 3 0 11 1 13075.8 1062.16 3 0 11 -1 12360.6 1178.12 3 0 11 2 16345.8 1096.97 3 0 11 -2 20666.2 1605.70 3 0 11 -3 3774.60 763.128 3 0 11 3 2602.71 384.097 3 0 11 4 32297.5 997.444 3 0 11 -4 31273.6 2201.48 3 0 11 -5 26050.8 2134.53 3 0 11 -6 1453.91 596.042 3 0 11 -7 8230.94 1309.33 3 0 11 -8 1986.15 700.854 3 0 11 -9 5411.50 1132.19 3 0 12 0 3716.92 638.429 3 0 12 -1 7159.47 956.038 3 0 12 1 6624.03 808.960 3 0 12 2 26484.3 1467.92 3 0 12 -2 27975.6 1950.37 3 0 12 3 25039.9 1272.15 3 0 12 -3 37705.4 2401.92 3 0 12 -4 19048.6 1778.22 3 0 12 -5 3457.08 823.545 3 0 12 -6 3414.33 825.931 3 0 12 -7 2511.74 787.078 3 0 12 -8 1892.42 675.567 3 0 12 -9 2856.74 875.909 3 0 13 0-72.8076 174.388 3 0 13 -1 16764.1 1502.53 3 0 13 1 11375.1 1098.75 3 0 13 2 9019.53 906.745 3 0 13 -2 8980.66 1156.76 3 0 13 -3 3683.85 795.823 3 0 13 3 2829.74 457.417 3 0 13 -4 8973.14 1267.84 3 0 13 -5 5377.49 1022.17 3 0 13 -6 2234.77 691.386 3 0 13 -7 1417.18 573.949 3 0 13 -8 4760.69 1090.17 3 0 14 0 3919.10 707.670 3 0 14 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27866.6 1892.77 3 3 2 6 24222.2 1803.23 2 3 2 7 169.979 207.938 2 -3 2 -7 875.657 407.073 3 3 2 8 1613.01 538.540 2 -3 2 -8 1978.24 573.776 3 -3 2 -9 2073.18 605.281 3 3 2 9 1006.15 511.427 2 3 3 -10 304.533 307.792 3 3 3 -9 266.041 197.630 3 -3 3 7 3049.65 384.693 5 3 3 -7 4194.67 590.493 1 3 3 -6 8372.64 762.523 1 3 3 -6 8431.27 821.352 4 3 3 -5 16047.5 1102.83 4 3 3 -4 11722.3 953.065 4 3 3 -3 54604.3 2010.09 4 3 3 -2 77423.1 2410.74 4 -3 3 1 42613.7 1628.36 3 -3 3 0 31202.3 1439.47 3 -3 3 -1 33989.0 1605.89 3 -3 3 -1 37006.4 1595.57 4 -3 3 -2 105802. 3016.21 3 -3 3 -3 23284.2 1518.43 3 -3 3 -4 21686.6 1555.06 3 -3 3 -5 6852.48 936.472 3 3 3 5 5471.04 810.299 2 -3 3 -6 22303.7 1753.23 3 3 3 6 22499.4 1764.23 2 -3 3 -7 7716.85 1088.34 3 3 3 7 7349.71 1078.27 2 3 3 8 2234.99 693.791 2 -3 3 -8 1830.27 559.456 3 -3 3 -9 831.016 424.397 3 3 3 9 322.014 343.583 2 3 4 -10 629.509 413.772 3 3 4 -9 1801.10 555.624 3 3 4 -7 20509.8 1199.04 1 3 4 -6 17401.8 1154.19 4 3 4 -6 11304.1 837.791 1 3 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877.005 5 5 -8 -6 3419.42 803.548 1 -5 -8 6 3410.40 813.704 5 5 -8 -5 2510.78 698.640 1 -5 -8 5 2660.16 660.217 5 -5 -8 4 1906.37 566.435 5 -5 -7 11-278.815 427.882 5 5 -7 -10-175.850 319.399 1 -5 -7 10-322.434 267.919 5 5 -7 -9 803.620 387.202 1 -5 -7 9 303.999 270.141 5 5 -7 -8 2149.53 681.056 1 -5 -7 8 2052.44 647.123 5 -5 -7 7 645.271 386.407 5 5 -7 -7 335.367 331.107 1 5 -7 -6 198.567 256.448 1 -5 -7 6 115.497 286.710 5 5 -7 -5 12237.9 1399.99 1 -5 -7 5 10637.7 1298.57 5 -5 -7 4 409.636 292.283 5 5 -7 0 6370.40 945.097 4 5 -7 1 15519.5 1447.72 4 5 -7 2 8330.76 1051.49 4 5 -7 3 1184.79 454.972 4 5 -7 4 67.6623 247.868 4 5 -6 -10 338.413 294.491 1 -5 -6 10 616.141 433.592 5 -5 -6 9 4629.75 940.438 5 5 -6 -9 3337.99 810.734 1 5 -6 -8 1780.33 585.289 1 -5 -6 8 1264.01 469.719 5 -5 -6 7 1531.78 528.989 5 5 -6 -7 1639.84 550.241 1 5 -6 -6 9691.41 1258.46 1 -5 -6 6 7689.41 1101.01 5 -5 -6 5 980.212 418.392 5 5 -6 -2 9321.48 1152.58 4 5 -6 -1 1863.18 559.954 4 5 -6 0 6602.26 959.306 4 5 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968.286 3 -7 9 -2-405.256 381.316 3 -7 9 -3-257.061 338.050 3 7 10 -6 1563.97 685.874 4 7 10 -5 5098.94 1063.29 4 7 10 -4 7603.12 1367.56 4 7 10 -3 5327.36 1145.93 4 -7 10 2 843.639 495.065 3 -7 10 1 1314.82 551.333 3 -7 10 0 916.371 447.349 3 -7 10 -1 1693.60 680.703 3 -7 10 -2 4114.95 982.093 3 -7 10 -3 821.553 500.021 3 7 11 -6 671.875 436.101 4 7 11 -5-25.6608 292.771 4 7 11 -4 989.671 354.258 4 7 11 -3 1428.27 658.041 4 -7 11 3 2413.86 627.393 3 -7 11 2 2051.36 650.738 3 -7 11 1 207.692 295.811 3 -7 11 0 1289.14 591.178 3 -7 11 -1 18.7322 314.600 3 -7 11 -2 1127.92 546.827 3 7 12 -6 9150.25 1458.51 4 7 12 -5 1333.42 627.338 4 7 12 -4 793.237 472.808 4 -7 12 3 60.3040 197.719 3 -7 12 2 5215.95 1025.33 3 -7 12 1 1848.45 688.309 3 -7 12 0 362.828 322.870 3 -7 12 -1 2182.46 711.591 3 7 13 -5 2301.40 848.942 4 7 13 -4-75.2364 327.592 4 -7 13 3 871.485 494.784 3 -7 13 2 1560.95 574.596 3 -7 13 1 1820.77 675.763 3 -7 13 0-448.651 380.382 3 -7 13 -1-252.872 290.398 3 7 14 -5-659.938 576.126 4 7 14 -4 315.272 345.849 4 -7 14 2 31.4520 357.407 3 -7 14 1 1128.16 521.657 3 -7 14 0 1279.63 553.243 3 7 15 -4-1181.06 628.026 4 -7 15 2-465.427 360.562 3 -7 15 1-395.937 377.189 3 8 -8 0 623.283 510.100 4 8 -8 1 101.611 308.391 4 8 -8 2 846.833 436.900 4 8 -7 -7 425.648 428.732 1 8 -7 -2 127.345 298.694 4 8 -7 -1 372.260 373.126 4 8 -7 0 235.633 369.594 4 8 -7 1 446.922 479.733 4 8 -7 2 1311.47 577.883 4 8 -6 -7 1177.57 606.028 1 8 -6 -3 105.891 396.814 4 8 -6 -2 1405.91 606.730 4 8 -6 -1 1162.48 650.914 4 8 -6 0 225.032 286.760 4 8 -6 1-1.10252 330.797 4 8 -6 2 665.571 441.214 4 8 -5 -8 790.586 528.869 1 8 -5 -4 1880.73 715.337 4 8 -5 -3 3868.90 1044.48 4 8 -5 -2 2544.05 830.420 4 8 -5 -1 563.845 542.843 4 8 -5 0 1701.08 653.503 4 8 -5 1-112.772 333.994 4 8 -5 2 997.497 525.994 4 8 -5 3 655.985 395.786 4 8 -4 -8 475.962 525.873 1 8 -4 -5 214.995 390.165 4 8 -4 -4 922.649 418.015 4 8 -4 -3 765.760 584.459 4 8 -4 -2-102.223 405.300 4 8 -4 -1 750.930 502.009 4 8 -4 0-394.179 517.107 4 8 -4 1 902.894 487.507 4 8 -4 2 2429.22 701.611 4 8 -4 3 522.341 513.496 4 8 -3 -9 756.421 415.775 1 8 -3 -8 987.739 508.109 1 8 -3 -6 387.312 301.229 4 8 -3 -5-73.2124 300.813 4 8 -3 -4 1198.20 656.533 4 8 -3 -3 1097.33 645.440 4 8 -3 -2 2463.11 756.684 4 8 -3 -1 938.540 546.896 4 8 -3 0 306.177 293.845 4 8 -3 1 1101.09 616.153 4 8 -3 2 830.480 543.352 4 8 -3 3 695.786 273.790 4 8 -2 -9 599.689 407.451 1 8 -2 -7-374.204 496.682 4 8 -2 -6 347.835 343.715 4 8 -2 -5 1631.84 726.031 4 8 -2 -4 850.869 612.223 4 8 -2 -3 18.6858 347.221 4 8 -2 -2 1757.01 681.996 4 8 -2 -1 1555.28 698.118 4 8 -2 0 3807.79 943.083 4 8 -2 1 1462.80 686.878 4 8 -2 2 708.440 549.223 4 8 -2 3 1537.76 659.370 4 8 -2 4 38.2535 406.272 4 8 -1 -10 899.540 482.113 1 8 -1 -9 3498.62 908.477 1 8 -1 -7 73.7421 452.897 4 8 -1 -6 1165.18 677.193 4 8 -1 -5 280.890 302.722 4 8 -1 -4 458.754 491.751 4 8 -1 -3 1428.69 681.078 4 8 -1 -2 1509.06 553.328 4 8 -1 -1 901.466 573.311 4 8 -1 0 2156.88 797.447 4 8 -1 1 631.328 424.132 4 8 -1 2 982.970 598.189 4 8 -1 3 496.037 397.039 4 8 -1 4 980.383 611.017 4 8 0 -9 142.412 298.079 1 8 0 -8 209.178 266.204 4 8 0 -7 217.492 430.172 4 8 0 -6-399.821 459.743 4 8 0 -5 1566.59 747.075 4 8 0 -4 5953.48 1214.02 4 8 0 -3 2083.75 728.333 4 8 0 -2 265.923 363.556 4 8 0 -1 5635.30 1167.38 4 8 0 0 6484.56 1224.20 4 8 0 1-53.7654 286.466 4 8 0 2 1261.24 598.686 4 8 0 3 135.495 352.983 4 8 0 4 207.145 286.642 4 8 1 -9 5224.84 1074.03 1 8 1 -8 2735.03 835.036 4 8 1 -7 1302.36 704.132 4 8 1 -6-128.774 256.929 4 8 1 -5-583.058 470.196 4 8 1 -4 152.721 295.214 4 8 1 -3 2018.40 758.857 4 8 1 -2 2771.34 826.060 4 8 1 -1 642.529 512.382 4 8 1 0 1310.03 697.537 4 8 1 1 369.349 471.418 4 8 1 2 534.520 436.679 4 8 1 3 524.852 357.926 4 8 1 4 654.968 415.443 4 8 2 -8 395.765 464.685 4 8 2 -7 40.6412 293.043 4 8 2 -6 128.815 387.966 4 8 2 -5 1898.98 759.935 4 8 2 -4 103.471 291.587 4 8 2 -3 384.005 475.851 4 8 2 -2 2226.13 769.602 4 8 2 -1-124.421 368.746 4 8 2 0 3761.32 971.773 4 8 2 1 2351.83 822.674 4 8 2 2 1009.24 596.432 4 8 2 3 1273.33 567.499 4 8 2 4 735.893 530.084 4 8 2 5 450.679 403.255 4 8 3 -9 599.209 399.391 4 8 3 -8 899.515 577.481 4 8 3 -7 891.165 586.600 4 8 3 -6-322.958 424.710 4 8 3 -5 901.539 548.577 4 8 3 -4 577.966 562.827 4 8 3 -3 1132.22 536.921 4 8 3 -2 2692.79 834.466 4 8 3 -1-211.429 432.441 4 8 3 0 1230.19 655.268 4 8 3 1 610.047 527.975 4 8 3 2 1272.75 643.011 4 8 3 3 2890.59 860.458 4 8 3 4 218.749 497.885 4 8 3 5 408.739 487.835 4 8 4 -8 422.853 395.810 4 8 4 -7 771.310 451.212 4 8 4 -6 704.974 605.513 4 8 4 -5 821.904 619.904 4 8 4 -4-11.2010 366.187 4 8 4 -3 995.183 582.958 4 8 4 -2-353.467 423.395 4 8 4 -1 391.365 369.752 4 8 4 0 704.052 420.336 4 8 4 1 2215.82 841.132 4 8 4 2 2205.25 799.538 4 -8 4 -2 2055.50 676.740 3 8 4 3 653.992 554.144 4 -8 4 -3 486.792 432.184 3 8 4 4 957.163 510.573 4 8 5 -8-256.549 458.810 4 8 5 -7 1019.87 498.414 4 8 5 -6 691.925 442.319 4 8 5 -5 3145.09 874.322 4 8 5 -4 2490.51 785.297 4 8 5 -3 3993.29 1044.55 4 8 5 -2 2248.23 802.553 4 8 5 -1 405.337 371.547 4 8 5 0 1284.38 636.647 4 8 5 1-202.870 453.401 4 -8 5 -1 55.1917 394.844 3 8 5 2-1298.76 660.380 4 -8 5 -2 519.961 296.548 3 8 5 3 1289.05 614.319 4 -8 5 -3 585.335 356.128 3 8 5 4-353.202 373.556 4 8 6 -8 299.383 312.305 4 8 6 -7 931.165 579.059 4 8 6 -6 713.004 573.057 4 8 6 -5 822.186 570.429 4 8 6 -4 457.714 459.139 4 8 6 -3 112.835 306.174 4 8 6 -2 1684.74 727.397 4 8 6 -1-236.496 393.717 4 8 6 0 1986.75 961.125 4 8 6 1-86.3806 415.883 4 -8 6 -1-339.200 489.954 3 8 6 2 1010.12 519.623 4 -8 6 -2 313.917 334.290 3 8 6 3 483.438 580.702 4 8 7 -7 895.650 561.343 4 8 7 -6-77.3213 248.856 4 8 7 -5 1506.47 610.229 4 8 7 -4 630.846 436.697 4 8 7 -3 1305.21 610.727 4 8 7 -2 472.066 411.853 4 8 7 -1 340.273 333.383 4 8 7 0 884.451 655.302 4 -8 7 0 148.201 314.810 3 8 7 1 1128.04 575.926 4 -8 7 -1-441.699 440.405 3 8 7 2 1564.19 701.051 4 -8 7 -2 541.975 295.477 3 8 8 -7 675.626 472.005 4 8 8 -6 1058.56 514.151 4 8 8 -5 318.933 387.058 4 8 8 -4 139.250 399.570 4 8 8 -3 261.796 394.764 4 8 8 -2 762.819 505.332 4 8 8 -1 507.203 518.419 4 -8 8 1 248.509 371.852 3 8 8 0 250.421 408.062 4 -8 8 0 192.628 291.969 3 -8 8 -1 779.716 500.020 3 8 9 -7 1789.69 857.036 4 8 9 -6-380.355 345.862 4 8 9 -5 741.593 552.074 4 8 9 -4 1323.69 715.023 4 8 9 -3 526.789 518.434 4 8 9 -2 308.760 519.068 4 8 9 -1 351.190 430.706 4 -8 9 1 145.412 357.468 3 -8 9 0 774.454 435.221 3 -8 9 -1 72.5023 208.223 3 8 10 -6 1736.30 812.466 4 8 10 -5 185.841 401.711 4 8 10 -4 1403.05 681.642 4 8 10 -3 1013.83 610.030 4 8 10 -2 1083.07 591.560 4 8 10 -1-240.994 571.567 4 -8 10 1 368.752 335.765 3 -8 10 0 631.962 302.086 3 8 11 -6 4729.35 1151.40 4 8 11 -5 10677.8 1683.48 4 8 11 -4 1798.23 831.045 4 8 11 -3-12.5592 488.283 4 8 11 -2 997.919 625.261 4 -8 11 2 357.031 319.202 3 -8 11 1 502.785 423.867 3 -8 11 0 879.269 506.171 3 8 12 -6 361.117 540.586 4 8 12 -5 1259.88 569.600 4 8 12 -4 91.8000 320.203 4 8 12 -3-283.757 547.627 4 -8 12 2-93.5032 301.241 3 -8 12 1 1586.76 639.583 3 -8 13 2 485.404 387.762 3 9 -8 0 84.3577 347.055 4 9 -8 1-336.041 565.160 4 9 -7 -2-885.820 571.622 4 9 -7 -1 2904.28 942.764 4 9 -7 0 349.097 569.539 4 9 -7 1 28.3122 315.626 4 9 -6 -4 104.854 424.468 4 9 -6 -3 173.643 579.623 4 9 -6 -2 1480.41 729.387 4 9 -6 -1 226.752 270.388 4 9 -6 0 187.932 424.202 4 9 -6 1-270.389 544.451 4 9 -6 2 754.419 428.258 4 9 -5 -5 66.5443 341.037 4 9 -5 -4-400.267 567.315 4 9 -5 -3 93.2481 482.417 4 9 -5 -2-270.089 481.951 4 9 -5 -1 412.051 543.513 4 9 -5 0 441.777 560.579 4 9 -5 1-285.785 376.309 4 9 -5 2 156.408 443.946 4 9 -4 -5 583.357 469.003 4 9 -4 -4 86.8821 299.642 4 9 -4 -3-586.346 588.781 4 9 -4 -2 646.046 563.819 4 9 -4 -1 1763.93 777.642 4 9 -4 0 531.953 443.145 4 9 -4 1 1236.77 608.241 4 9 -4 2 258.190 403.684 4 9 -3 -6-230.499 434.282 4 9 -3 -5 988.219 533.708 4 9 -3 -4 474.875 467.552 4 9 -3 -3 1197.10 685.653 4 9 -3 -2 7.70208 333.795 4 9 -3 -1-471.625 458.971 4 9 -3 0 426.208 365.428 4 9 -3 1 489.248 567.283 4 9 -3 2-168.587 318.652 4 9 -3 3-269.337 480.119 4 9 -2 -7 391.960 428.868 4 9 -2 -6 112.985 381.277 4 9 -2 -5 1304.12 710.878 4 9 -2 -4 76.8026 348.612 4 9 -2 -3 3681.84 1059.05 4 9 -2 -2 1025.09 572.884 4 9 -2 -1 987.634 617.656 4 9 -2 0 323.125 391.680 4 9 -2 1 964.052 505.363 4 9 -2 2 88.1700 314.070 4 9 -2 3 1023.94 518.866 4 9 -1 -7 690.637 433.479 4 9 -1 -6 782.970 656.631 4 9 -1 -5 790.629 524.388 4 9 -1 -4 2175.75 859.573 4 9 -1 -3 2597.92 918.648 4 9 -1 -2 199.863 385.348 4 9 -1 -1 815.973 455.020 4 9 -1 0 1832.65 753.591 4 9 -1 1 671.397 627.944 4 9 -1 2 236.421 409.434 4 9 -1 3 365.886 428.363 4 9 0 -7 1346.59 666.109 4 9 0 -6-71.1034 546.453 4 9 0 -5 818.112 621.861 4 9 0 -4 6788.19 1371.95 4 9 0 -3 5456.55 1242.81 4 9 0 -2 1459.43 797.543 4 9 0 -1 692.211 495.897 4 9 0 0-471.313 435.085 4 9 0 1-291.185 403.330 4 9 0 2 560.493 551.703 4 9 0 3 129.022 327.192 4 9 1 -8-261.231 468.918 4 9 1 -7 889.094 630.352 4 9 1 -6 754.229 486.104 4 9 1 -5 2520.45 865.460 4 9 1 -4 2173.01 822.356 4 9 1 -3 2461.13 908.949 4 9 1 -2 937.015 634.293 4 9 1 -1 1262.81 683.362 4 9 1 0 1810.99 703.417 4 9 1 1 1323.90 635.285 4 9 1 2-622.333 555.591 4 9 2 -8 2767.05 909.202 4 9 2 -7 251.885 403.661 4 9 2 -6-48.9965 289.722 4 9 2 -5 886.623 597.383 4 9 2 -4 269.710 472.297 4 9 2 -3 3052.84 992.678 4 9 2 -2 2447.95 807.259 4 9 2 -1 191.195 435.888 4 9 2 0 757.416 447.561 4 9 2 1 1895.57 721.755 4 9 2 2 71.6076 410.308 4 9 3 -8 261.761 373.401 4 9 3 -7 41.6555 421.380 4 9 3 -6-39.5996 377.932 4 9 3 -5 748.478 527.076 4 9 3 -4 431.289 421.769 4 9 3 -3 164.991 335.485 4 9 3 -2 444.389 568.971 4 9 3 -1-797.758 557.331 4 9 3 0 698.927 476.608 4 9 3 1 552.826 461.961 4 9 4 -8 664.018 618.962 4 9 4 -7 1027.88 526.424 4 9 4 -6 1028.71 635.330 4 9 4 -5 596.491 426.680 4 9 4 -4 553.146 427.563 4 9 4 -3 2.61860 508.632 4 9 4 -2 544.147 340.116 4 9 4 -1 814.837 502.603 4 9 4 0 442.073 391.153 4 9 4 1 211.748 470.142 4 9 5 -8-148.024 582.718 4 9 5 -7 142.183 355.610 4 9 5 -6 661.804 603.519 4 9 5 -5 768.237 607.698 4 9 5 -4 182.643 411.985 4 9 5 -3 1366.51 713.920 4 9 5 -2 423.434 409.749 4 9 5 -1 179.508 442.122 4 9 5 0 1189.77 658.716 4 9 6 -8 2862.13 998.297 4 9 6 -7 207.406 470.347 4 9 6 -6 1.36658 424.226 4 9 6 -5 535.409 627.266 4 9 6 -4 104.714 391.987 4 9 6 -3 643.796 499.728 4 9 6 -2 752.261 601.106 4 9 6 -1 1999.39 937.916 4 9 7 -7 79.7877 322.686 4 9 7 -6 1311.33 756.925 4 9 7 -5-41.2316 445.880 4 9 7 -4 252.710 459.715 4 9 7 -3 812.896 454.585 4 9 7 -2 616.836 517.161 4 9 8 -5 226.130 282.718 4 9 8 -4 2911.72 1004.32 4 ; _shelx_res_checksum 53636 _shelx_res_file ; TITL 130909_s1_wz in P21 #4 CELL 0.71073 7.70421 15.76526 9.18787 90 104.3699 90 ZERR 2 0.00042 0.0007 0.00042 0 0.0048 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H O S UNIT 50 44 10 2 L.S. 10 PLAN 5 SIZE 0.2 0.25 0.3 TEMP 20 REM reset to P21 #4 BOND $H acta htab fmap 2 SHEL 999 0.8 REM E:/CCD%20data/1309/olex2_130909_s1_wz/130909_s1_wz.hkl WGHT 0.068300 FVAR 9.69808 S1 4 1.013217 0.730703 1.034046 11.00000 0.11163 0.05761 = 0.04983 -0.01195 -0.00413 -0.00154 O1 3 0.901091 0.520979 0.293055 11.00000 0.04931 0.04562 = 0.04846 0.00586 0.02302 -0.00444 O2 3 1.096128 0.462868 0.488933 11.00000 0.03893 0.06668 = 0.06268 -0.00324 0.01266 -0.00650 O3 3 0.956226 0.555013 0.916587 11.00000 0.09056 0.04220 = 0.04246 0.00156 -0.00466 0.00226 O4 3 0.534952 0.526355 0.722963 11.00000 0.06324 0.04307 = 0.08427 0.01140 0.03733 0.01335 O5 3 0.610541 0.390078 0.722244 11.00000 0.05163 0.03199 = 0.07546 0.00622 0.03482 -0.00105 C1 1 0.989504 0.834522 0.984910 11.00000 0.07984 0.05232 = 0.08020 -0.03165 0.01968 -0.01220 AFIX 43 H1 2 1.021272 0.879102 1.052580 11.00000 -1.20000 AFIX 0 C2 1 0.919541 0.844847 0.836966 11.00000 0.07280 0.03899 = 0.07034 0.00535 0.02476 -0.00264 AFIX 43 H2 2 0.896526 0.897934 0.792197 11.00000 -1.20000 AFIX 0 C3 1 0.884152 0.769167 0.755789 11.00000 0.05405 0.03248 = 0.03277 -0.00470 0.00659 -0.00583 AFIX 43 H3 2 0.838482 0.765640 0.652302 11.00000 -1.20000 AFIX 0 C4 1 0.927614 0.698743 0.853271 11.00000 0.04113 0.03749 = 0.03412 -0.00560 0.00626 -0.00480 C5 1 0.912886 0.607774 0.818619 11.00000 0.03949 0.03627 = 0.03540 -0.00020 0.00550 -0.00304 C6 1 0.841998 0.583235 0.657131 11.00000 0.05554 0.02984 = 0.03546 -0.00077 0.01281 -0.00859 AFIX 23 H6A 2 0.930810 0.596484 0.601960 11.00000 -1.20000 H6B 2 0.735159 0.616080 0.613959 11.00000 -1.20000 AFIX 0 C7 1 0.796497 0.487942 0.640530 11.00000 0.04154 0.02735 = 0.03440 0.00136 0.00752 -0.00203 AFIX 13 H7 2 0.896857 0.456867 0.704867 11.00000 -1.20000 AFIX 0 C8 1 0.772512 0.454799 0.476400 11.00000 0.03214 0.03034 = 0.03247 -0.00133 0.00895 -0.00090 C9 1 0.943030 0.477941 0.426502 11.00000 0.04091 0.03647 = 0.04399 -0.00698 0.00994 -0.00496 C10 1 0.633428 0.501026 0.358271 11.00000 0.04167 0.02816 = 0.03249 -0.00302 0.01106 -0.00283 C11 1 0.715772 0.534026 0.253357 11.00000 0.05279 0.03455 = 0.04004 -0.00544 0.01628 -0.00818 C12 1 0.625762 0.573470 0.123635 11.00000 0.07061 0.05301 = 0.04278 0.00830 0.01995 0.00262 AFIX 43 H12 2 0.685200 0.593863 0.054211 11.00000 -1.20000 AFIX 0 C13 1 0.441263 0.581516 0.100874 11.00000 0.07452 0.05436 = 0.04673 0.01274 0.00296 0.01415 AFIX 43 H13 2 0.375071 0.607827 0.014185 11.00000 -1.20000 AFIX 0 C14 1 0.355091 0.551142 0.204658 11.00000 0.05143 0.04367 = 0.05888 0.00036 0.00160 0.00594 AFIX 43 H14 2 0.231848 0.558065 0.188104 11.00000 -1.20000 AFIX 0 C15 1 0.449881 0.510359 0.333546 11.00000 0.04344 0.03821 = 0.04307 0.00071 0.01025 -0.00081 AFIX 43 H15 2 0.390679 0.489463 0.402758 11.00000 -1.20000 AFIX 0 C16 1 0.754880 0.357523 0.462334 11.00000 0.03863 0.03177 = 0.03565 -0.00321 0.01308 -0.00032 C17 1 0.628105 0.318812 0.349111 11.00000 0.04453 0.04577 = 0.04908 -0.00629 0.00379 -0.00029 AFIX 43 H17 2 0.547227 0.351838 0.280143 11.00000 -1.20000 AFIX 0 C18 1 0.620103 0.230609 0.337115 11.00000 0.05868 0.03739 = 0.06796 -0.01530 0.00707 -0.00870 AFIX 43 H18 2 0.534320 0.205521 0.259790 11.00000 -1.20000 AFIX 0 C19 1 0.736014 0.180854 0.436936 11.00000 0.06237 0.02970 = 0.07576 -0.00262 0.02568 -0.00408 AFIX 43 H19 2 0.728205 0.122091 0.429113 11.00000 -1.20000 AFIX 0 C20 1 0.865383 0.218178 0.549990 11.00000 0.06321 0.03291 = 0.05779 0.00129 0.01752 0.00974 AFIX 43 H20 2 0.945399 0.184492 0.618412 11.00000 -1.20000 AFIX 0 C21 1 0.876231 0.305317 0.561694 11.00000 0.04638 0.04048 = 0.04242 -0.00679 0.00286 0.00081 AFIX 43 H21 2 0.965662 0.329839 0.636857 11.00000 -1.20000 AFIX 0 C22 1 0.631542 0.471480 0.700058 11.00000 0.04317 0.03699 = 0.03285 0.00309 0.00736 0.00077 C23 1 0.449707 0.361745 0.767768 11.00000 0.04579 0.04885 = 0.07739 0.01231 0.02798 -0.00374 AFIX 13 H23 2 0.354740 0.404339 0.738814 11.00000 -1.20000 AFIX 0 C24 1 0.393720 0.281731 0.683425 11.00000 0.08166 0.08033 = 0.08095 -0.00413 0.01590 -0.03590 AFIX 137 H24A 2 0.373670 0.292296 0.577648 11.00000 -1.50000 H24B 2 0.285116 0.261341 0.704538 11.00000 -1.50000 H24C 2 0.486233 0.239909 0.713645 11.00000 -1.50000 AFIX 0 C25 1 0.498401 0.350615 0.934507 11.00000 0.09094 0.11844 = 0.07247 -0.00150 0.04326 -0.03755 AFIX 137 H25A 2 0.595413 0.310898 0.962655 11.00000 -1.50000 H25B 2 0.396574 0.329581 0.965978 11.00000 -1.50000 H25C 2 0.534497 0.404216 0.982002 11.00000 -1.50000 AFIX 0 HKLF 4 REM 130909_s1_wz in P21 #4 REM R1 = 0.0548 for 2655 Fo > 4sig(Fo) and 0.0726 for all 3432 data REM 282 parameters refined using 1 restraints END WGHT 0.0683 0.0000 REM Instructions for potential hydrogen bonds REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.201, deepest hole -0.373, 1-sigma level 0.054 Q1 1 0.8257 0.7700 0.7213 11.00000 0.05 0.20 Q2 1 0.1076 0.2537 0.7030 11.00000 0.05 0.17 Q3 1 0.5793 0.6864 0.4977 11.00000 0.05 0.17 Q4 1 0.2366 0.5554 -0.0699 11.00000 0.05 0.17 Q5 1 1.2005 0.7231 0.8227 11.00000 0.05 0.16 ; _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. ; _shelxl_version_number 2013-2 #END Tags that were not found in dictionaries loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp S1 S 1.0132(3) 0.73070(11) 1.03405(16) 0.0773(6) Uani 1 1 d . . O1 O 0.9011(4) 0.5210(2) 0.2931(3) 0.0459(9) Uani 1 1 d . . O2 O 1.0961(5) 0.4629(3) 0.4889(4) 0.0561(10) Uani 1 1 d . . O3 O 0.9562(6) 0.5550(2) 0.9166(4) 0.0621(11) Uani 1 1 d . . O4 O 0.5350(5) 0.5264(2) 0.7230(4) 0.0602(10) Uani 1 1 d . . O5 O 0.6105(5) 0.3901(2) 0.7222(4) 0.0497(9) Uani 1 1 d . . C1 C 0.9895(10) 0.8345(4) 0.9849(8) 0.0708(18) Uani 1 1 d . . H1 H 1.0213 0.8791 1.0526 0.085 Uiso 1 1 calc R U C2 C 0.9195(8) 0.8448(4) 0.8370(7) 0.0595(16) Uani 1 1 d . . H2 H 0.8965 0.8979 0.7922 0.071 Uiso 1 1 calc R U C3 C 0.8842(6) 0.7692(3) 0.7558(5) 0.0405(11) Uani 1 1 d . . H3 H 0.8385 0.7656 0.6523 0.049 Uiso 1 1 calc R U C4 C 0.9276(6) 0.6987(3) 0.8533(5) 0.0381(11) Uani 1 1 d . . C5 C 0.9129(6) 0.6078(3) 0.8186(5) 0.0377(11) Uani 1 1 d . . C6 C 0.8420(7) 0.5832(3) 0.6571(5) 0.0400(11) Uani 1 1 d . . H6A H 0.9308 0.5965 0.6020 0.048 Uiso 1 1 calc R U H6B H 0.7352 0.6161 0.6140 0.048 Uiso 1 1 calc R U C7 C 0.7965(6) 0.4879(3) 0.6405(5) 0.0348(10) Uani 1 1 d . . H7 H 0.8969 0.4569 0.7049 0.042 Uiso 1 1 calc R U C8 C 0.7725(6) 0.4548(3) 0.4764(5) 0.0315(10) Uani 1 1 d . . C9 C 0.9430(7) 0.4779(3) 0.4265(5) 0.0406(11) Uani 1 1 d . . C10 C 0.6334(6) 0.5010(3) 0.3583(4) 0.0338(10) Uani 1 1 d . . C11 C 0.7158(7) 0.5340(3) 0.2534(5) 0.0416(11) Uani 1 1 d . . C12 C 0.6258(8) 0.5735(4) 0.1236(5) 0.0544(15) Uani 1 1 d . . H12 H 0.6852 0.5939 0.0542 0.065 Uiso 1 1 calc R U C13 C 0.4413(8) 0.5815(4) 0.1009(6) 0.0607(16) Uani 1 1 d . . H13 H 0.3751 0.6078 0.0142 0.073 Uiso 1 1 calc R U C14 C 0.3551(8) 0.5511(3) 0.2047(6) 0.0535(14) Uani 1 1 d . . H14 H 0.2318 0.5581 0.1881 0.064 Uiso 1 1 calc R U C15 C 0.4499(7) 0.5104(3) 0.3335(5) 0.0417(11) Uani 1 1 d . . H15 H 0.3907 0.4895 0.4028 0.050 Uiso 1 1 calc R U C16 C 0.7549(6) 0.3575(3) 0.4623(5) 0.0347(10) Uani 1 1 d . . C17 C 0.6281(7) 0.3188(3) 0.3491(6) 0.0478(13) Uani 1 1 d . . H17 H 0.5472 0.3518 0.2801 0.057 Uiso 1 1 calc R U C18 C 0.6201(8) 0.2306(4) 0.3371(6) 0.0562(14) Uani 1 1 d . . H18 H 0.5343 0.2055 0.2598 0.067 Uiso 1 1 calc R U C19 C 0.7360(8) 0.1809(3) 0.4369(7) 0.0544(14) Uani 1 1 d . . H19 H 0.7282 0.1221 0.4291 0.065 Uiso 1 1 calc R U C20 C 0.8654(8) 0.2182(3) 0.5500(6) 0.0509(13) Uani 1 1 d . . H20 H 0.9454 0.1845 0.6184 0.061 Uiso 1 1 calc R U C21 C 0.8762(7) 0.3053(3) 0.5617(5) 0.0445(12) Uani 1 1 d . . H21 H 0.9657 0.3298 0.6369 0.053 Uiso 1 1 calc R U C22 C 0.6315(6) 0.4715(3) 0.7001(5) 0.0380(11) Uani 1 1 d . . C23 C 0.4497(7) 0.3617(4) 0.7678(6) 0.0551(14) Uani 1 1 d . . H23 H 0.3547 0.4043 0.7388 0.066 Uiso 1 1 calc R U C24 C 0.3937(10) 0.2817(5) 0.6834(8) 0.082(2) Uani 1 1 d . . H24A H 0.3737 0.2923 0.5776 0.123 Uiso 1 1 calc R U H24B H 0.2851 0.2613 0.7045 0.123 Uiso 1 1 calc R U H24C H 0.4862 0.2399 0.7136 0.123 Uiso 1 1 calc R U C25 C 0.4984(10) 0.3506(6) 0.9345(7) 0.090(2) Uani 1 1 d . . H25A H 0.5954 0.3109 0.9627 0.135 Uiso 1 1 calc R U H25B H 0.3966 0.3296 0.9660 0.135 Uiso 1 1 calc R U H25C H 0.5345 0.4042 0.9820 0.135 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.1116(15) 0.0576(9) 0.0498(9) -0.0120(8) -0.0041(9) -0.0015(10) O1 0.049(2) 0.046(2) 0.0485(18) 0.0059(18) 0.0230(15) -0.0044(18) O2 0.039(2) 0.067(3) 0.063(2) -0.003(2) 0.0127(17) -0.0065(19) O3 0.091(3) 0.042(2) 0.0425(18) 0.0016(19) -0.0047(18) 0.002(2) O4 0.063(2) 0.043(2) 0.084(3) 0.011(2) 0.037(2) 0.013(2) O5 0.052(2) 0.0320(17) 0.075(2) 0.0062(19) 0.0348(18) -0.0010(17) C1 0.080(5) 0.052(4) 0.080(4) -0.032(4) 0.020(3) -0.012(3) C2 0.073(4) 0.039(3) 0.070(4) 0.005(3) 0.025(3) -0.003(3) C3 0.054(3) 0.032(2) 0.033(2) -0.005(2) 0.007(2) -0.006(2) C4 0.041(3) 0.037(2) 0.034(2) -0.006(2) 0.0063(19) -0.005(2) C5 0.039(3) 0.036(3) 0.035(2) 0.000(2) 0.0055(19) -0.003(2) C6 0.056(3) 0.030(2) 0.035(2) -0.001(2) 0.013(2) -0.009(2) C7 0.042(3) 0.027(2) 0.034(2) 0.001(2) 0.0075(18) -0.002(2) C8 0.032(2) 0.030(2) 0.032(2) -0.001(2) 0.0089(17) -0.0009(19) C9 0.041(3) 0.036(3) 0.044(2) -0.007(2) 0.010(2) -0.005(2) C10 0.042(3) 0.028(2) 0.032(2) -0.003(2) 0.0111(19) -0.003(2) C11 0.053(3) 0.035(2) 0.040(2) -0.005(2) 0.016(2) -0.008(2) C12 0.071(4) 0.053(3) 0.043(3) 0.008(3) 0.020(3) 0.003(3) C13 0.075(4) 0.054(3) 0.047(3) 0.013(3) 0.003(3) 0.014(3) C14 0.051(3) 0.044(3) 0.059(3) 0.000(3) 0.002(3) 0.006(3) C15 0.043(3) 0.038(3) 0.043(3) 0.001(2) 0.010(2) -0.001(2) C16 0.039(3) 0.032(2) 0.036(2) -0.003(2) 0.0131(19) 0.000(2) C17 0.045(3) 0.046(3) 0.049(3) -0.006(3) 0.004(2) 0.000(3) C18 0.059(3) 0.037(3) 0.068(3) -0.015(3) 0.007(3) -0.009(3) C19 0.062(4) 0.030(3) 0.076(4) -0.003(3) 0.026(3) -0.004(3) C20 0.063(4) 0.033(3) 0.058(3) 0.001(3) 0.018(3) 0.010(3) C21 0.046(3) 0.040(3) 0.042(3) -0.007(3) 0.003(2) 0.001(2) C22 0.043(3) 0.037(3) 0.033(2) 0.003(2) 0.0074(19) 0.001(2) C23 0.046(3) 0.049(3) 0.077(4) 0.012(3) 0.028(3) -0.004(3) C24 0.082(5) 0.080(5) 0.081(4) -0.004(4) 0.016(4) -0.036(4) C25 0.091(5) 0.118(6) 0.072(4) -0.002(5) 0.043(4) -0.038(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 C1 S1 C4 92.1(3) C9 O1 C11 107.8(3) C22 O5 C23 119.0(4) S1 C1 H1 123.9 C2 C1 S1 112.1(5) C2 C1 H1 123.9 C1 C2 H2 122.8 C1 C2 C3 114.4(6) C3 C2 H2 122.8 C2 C3 H3 124.8 C2 C3 C4 110.4(4) C4 C3 H3 124.8 C3 C4 S1 111.0(4) C3 C4 C5 129.6(4) C5 C4 S1 119.4(4) O3 C5 C4 121.2(4) O3 C5 C6 121.6(4) C4 C5 C6 117.2(4) C5 C6 H6A 109.3 C5 C6 H6B 109.3 C5 C6 C7 111.6(4) H6A C6 H6B 108.0 C7 C6 H6A 109.3 C7 C6 H6B 109.3 C6 C7 H7 107.5 C6 C7 C8 113.0(3) C8 C7 H7 107.5 C22 C7 C6 108.6(4) C22 C7 H7 107.5 C22 C7 C8 112.3(4) C9 C8 C7 107.6(3) C9 C8 C16 105.9(4) C10 C8 C7 115.2(4) C10 C8 C9 100.2(3) C10 C8 C16 112.8(4) C16 C8 C7 113.6(4) O1 C9 C8 110.8(4) O2 C9 O1 120.8(5) O2 C9 C8 128.4(5) C11 C10 C8 108.5(4) C11 C10 C15 118.3(4) C15 C10 C8 133.1(4) C10 C11 O1 112.3(4) C12 C11 O1 123.9(4) C12 C11 C10 123.9(5) C11 C12 H12 121.6 C11 C12 C13 116.7(5) C13 C12 H12 121.6 C12 C13 H13 119.5 C14 C13 C12 121.0(5) C14 C13 H13 119.5 C13 C14 H14 119.6 C13 C14 C15 120.7(5) C15 C14 H14 119.6 C10 C15 C14 119.4(4) C10 C15 H15 120.3 C14 C15 H15 120.3 C17 C16 C8 122.3(4) C17 C16 C21 117.7(4) C21 C16 C8 119.9(4) C16 C17 H17 119.7 C16 C17 C18 120.6(5) C18 C17 H17 119.7 C17 C18 H18 119.6 C19 C18 C17 120.9(5) C19 C18 H18 119.6 C18 C19 H19 120.2 C18 C19 C20 119.5(5) C20 C19 H19 120.2 C19 C20 H20 119.9 C21 C20 C19 120.1(5) C21 C20 H20 119.9 C16 C21 H21 119.4 C20 C21 C16 121.1(5) C20 C21 H21 119.4 O4 C22 O5 125.0(5) O4 C22 C7 123.5(4) O5 C22 C7 111.5(4) O5 C23 H23 109.8 O5 C23 C24 105.4(5) O5 C23 C25 108.2(5) C24 C23 H23 109.8 C24 C23 C25 113.6(6) C25 C23 H23 109.8 C23 C24 H24A 109.5 C23 C24 H24B 109.5 C23 C24 H24C 109.5 H24A C24 H24B 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C23 C25 H25A 109.5 C23 C25 H25B 109.5 C23 C25 H25C 109.5 H25A C25 H25B 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 C1 1.696(7) S1 C4 1.704(5) O1 C9 1.368(6) O1 C11 1.398(6) O2 C9 1.200(6) O3 C5 1.210(5) O4 C22 1.193(6) O5 C22 1.316(6) O5 C23 1.472(6) C1 H1 0.9300 C1 C2 1.342(9) C2 H2 0.9300 C2 C3 1.398(7) C3 H3 0.9300 C3 C4 1.414(7) C4 C5 1.467(7) C5 C6 1.499(6) C6 H6A 0.9700 C6 H6B 0.9700 C6 C7 1.542(6) C7 H7 0.9800 C7 C8 1.563(6) C7 C22 1.525(6) C8 C9 1.539(6) C8 C10 1.510(6) C8 C16 1.542(6) C10 C11 1.381(6) C10 C15 1.383(6) C11 C12 1.370(7) C12 H12 0.9300 C12 C13 1.390(8) C13 H13 0.9300 C13 C14 1.376(8) C14 H14 0.9300 C14 C15 1.386(7) C15 H15 0.9300 C16 C17 1.380(6) C16 C21 1.400(7) C17 H17 0.9300 C17 C18 1.395(7) C18 H18 0.9300 C18 C19 1.359(8) C19 H19 0.9300 C19 C20 1.380(7) C20 H20 0.9300 C20 C21 1.379(7) C21 H21 0.9300 C23 H23 0.9800 C23 C24 1.487(9) C23 C25 1.494(8) C24 H24A 0.9600 C24 H24B 0.9600 C24 H24C 0.9600 C25 H25A 0.9600 C25 H25B 0.9600 C25 H25C 0.9600 loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139184540