#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:51:40 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242548 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/26/4132601.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_4132601 loop_ _publ_author_name 'Collet, Guillaume' 'Lathion, Timoth\'ee' 'Besnard, C\'eline' 'Piguet, Claude' 'Petoud, St\'ephane' _publ_section_title ; On-Demand Degradation of Metal-Organic Framework Based on Photocleavable Dianthracene-Based Ligand. ; _journal_issue 34 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 10820 _journal_page_last 10828 _journal_paper_doi 10.1021/jacs.8b05047 _journal_volume 140 _journal_year 2018 _chemical_formula_moiety '2(C2 H6 O S), C30 H20 O4' _chemical_formula_sum 'C34 H32 O6 S2' _chemical_formula_weight 600.71 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2018-05-09 _audit_creation_method ; Olex2 1.2 (compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492) ; _cell_angle_alpha 90 _cell_angle_beta 104.060(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.4209(3) _cell_length_b 7.9301(2) _cell_length_c 18.7758(5) _cell_measurement_reflns_used 3380 _cell_measurement_temperature 180.00(10) _cell_measurement_theta_max 73.4440 _cell_measurement_theta_min 4.3370 _cell_volume 1505.13(7) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _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 180.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.4679 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.971 _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 -76.00 20.00 1.00 1.00 -- -37.56 -19.00 30.00 96 2 \w 56.00 94.00 1.00 1.00 -- 37.56-126.00 25.00 38 3 \w 40.00 68.00 1.00 2.00 -- 110.40 -45.00 -90.00 28 4 \w 83.00 109.00 1.00 2.00 -- 110.40 -94.00 -90.00 26 5 \w 34.00 107.00 1.00 2.00 -- 110.40-111.00 60.00 73 6 \w 93.00 124.00 1.00 2.00 -- 110.40 -61.00 60.00 31 7 \w 88.00 169.00 1.00 2.00 -- 110.40 45.00 0.00 81 8 \w 106.00 134.00 1.00 2.00 -- 110.40 111.00-150.00 28 9 \w 29.00 141.00 1.00 2.00 -- 110.40 -30.00-180.00 112 10 \w 32.00 85.00 1.00 2.00 -- 110.40 -61.00 60.00 53 11 \w -115.00 -22.00 1.00 1.00 -- -37.56 -38.00 0.00 93 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.1488213000 _diffrn_orient_matrix_UB_12 0.0141888000 _diffrn_orient_matrix_UB_13 -0.0370620000 _diffrn_orient_matrix_UB_21 0.0302895000 _diffrn_orient_matrix_UB_22 -0.0230298000 _diffrn_orient_matrix_UB_23 -0.0757257000 _diffrn_orient_matrix_UB_31 -0.0145071000 _diffrn_orient_matrix_UB_32 -0.1922280000 _diffrn_orient_matrix_UB_33 0.0063877000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_unetI/netI 0.0201 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.971 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 4930 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.971 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.339 _diffrn_reflns_theta_min 4.457 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.972 _exptl_absorpt_correction_T_max 0.625 _exptl_absorpt_correction_T_min 0.428 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.325 _exptl_crystal_description prism _exptl_crystal_F_000 632 _exptl_crystal_size_max 0.634 _exptl_crystal_size_mid 0.513 _exptl_crystal_size_min 0.302 _refine_diff_density_max 0.528 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.066 _refine_ls_extinction_coef 0.0195(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick 2017)' _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 196 _refine_ls_number_reflns 2934 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0486 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0772P)^2^+1.1093P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1298 _refine_ls_wR_factor_ref 0.1311 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2804 _reflns_number_total 2934 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b05047_si_003.cif _cod_data_source_block diant_b _cod_database_code 4132601 _shelx_shelxl_version_number 2017/1 _chemical_oxdiff_formula 'C17 H16 O3 S1' _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 99.56 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 67.29 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Ternary CH refined with riding coordinates: C21(H21) 2.b Aromatic/amide H refined with riding coordinates: C23(H23), C24(H24), C25(H25), C26(H26), C30(H30), C31(H31), C32(H32), C33(H33) 2.c Idealised Me refined as rotating group: C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB,H4SC) ; _shelx_res_file ; TITL diant_b_a.res in P2(1)/n diant_b.res created by SHELXL-2017/1 at 12:06:41 on 09-May-2018 REM Old TITL diant_b in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.157, Rweak 0.183, Alpha 0.032, Orientation as input REM Formula found by SHELXT: C17 O3 Cl CELL 1.54184 10.4209 7.9301 18.7758 90 104.06 90 ZERR 2 0.0003 0.0002 0.0005 0 0.003 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O S UNIT 68 64 12 4 L.S. 4 PLAN 20 TEMP -93 BOND $H list 4 MORE -1 CONF fmap 2 acta REM REM REM WGHT 0.077200 1.109300 EXTI 0.019452 FVAR 9.84553 S1S 4 0.802053 -0.116092 0.300256 11.00000 0.04562 0.02194 = 0.04306 -0.00692 0.02783 -0.00425 O2S 3 0.848376 0.058698 0.325002 11.00000 0.03823 0.02893 = 0.05868 -0.01677 0.02995 -0.00962 C3S 1 0.626326 -0.096641 0.267375 11.00000 0.04956 0.06378 = 0.06995 -0.02744 0.01194 -0.01754 AFIX 137 H3SA 2 0.588611 -0.053899 0.306855 11.00000 -1.50000 H3SB 2 0.588148 -0.207316 0.251420 11.00000 -1.50000 H3SC 2 0.606085 -0.018069 0.225861 11.00000 -1.50000 AFIX 0 C4S 1 0.801225 -0.237068 0.378551 11.00000 0.11564 0.04533 = 0.07166 0.02308 0.05384 0.02961 AFIX 137 H4SA 2 0.891887 -0.248831 0.408582 11.00000 -1.50000 H4SB 2 0.764606 -0.348946 0.363475 11.00000 -1.50000 H4SC 2 0.746721 -0.180896 0.407263 11.00000 -1.50000 AFIX 0 O5 3 0.631869 0.086584 0.434589 11.00000 0.05693 0.01660 = 0.05342 -0.00192 0.03549 0.00345 O6 3 0.743398 0.286246 0.391591 11.00000 0.02760 0.02260 = 0.03501 -0.00704 0.01629 -0.00053 H6 2 0.773459 0.203102 0.371167 11.00000 -1.50000 C4 1 0.657739 0.233272 0.428572 11.00000 0.02099 0.01909 = 0.02158 -0.00185 0.00555 0.00222 C21 1 0.500090 0.697613 0.490077 11.00000 0.02131 0.01233 = 0.02240 -0.00009 0.00702 0.00032 AFIX 13 H21 2 0.489183 0.822929 0.489468 11.00000 -1.20000 AFIX 0 C22 1 0.645239 0.659679 0.519913 11.00000 0.02144 0.01717 = 0.01992 0.00011 0.00734 -0.00117 C23 1 0.731168 0.777367 0.561127 11.00000 0.02693 0.02098 = 0.02677 -0.00507 0.00819 -0.00378 AFIX 43 H23 2 0.698281 0.883928 0.571558 11.00000 -1.20000 AFIX 0 C24 1 0.864452 0.740458 0.587120 11.00000 0.02645 0.03366 = 0.03031 -0.00889 0.00484 -0.00994 AFIX 43 H24 2 0.922994 0.821856 0.614628 11.00000 -1.20000 AFIX 0 C25 1 0.911495 0.584178 0.572680 11.00000 0.01848 0.04072 = 0.02971 -0.00401 0.00215 -0.00102 AFIX 43 H25 2 1.002618 0.558186 0.590680 11.00000 -1.20000 AFIX 0 C26 1 0.826495 0.464792 0.532028 11.00000 0.02139 0.02609 = 0.02591 -0.00204 0.00504 0.00275 AFIX 43 H26 2 0.859572 0.357309 0.522994 11.00000 -1.20000 AFIX 0 C27 1 0.692987 0.502326 0.504512 11.00000 0.01963 0.01817 = 0.01851 -0.00042 0.00546 -0.00079 C28 1 0.591267 0.379716 0.459867 11.00000 0.01713 0.01520 = 0.01969 -0.00064 0.00600 0.00147 C29 1 0.505723 0.478894 0.394926 11.00000 0.01594 0.01655 = 0.02149 0.00118 0.00473 -0.00103 C30 1 0.469643 0.418981 0.323387 11.00000 0.02217 0.02043 = 0.02379 -0.00158 0.00632 -0.00240 AFIX 43 H30 2 0.499252 0.311168 0.312132 11.00000 -1.20000 AFIX 0 C31 1 0.390332 0.515936 0.268036 11.00000 0.02850 0.03263 = 0.01958 -0.00048 0.00361 -0.00368 AFIX 43 H31 2 0.366824 0.474590 0.219096 11.00000 -1.20000 AFIX 0 C32 1 0.345662 0.672185 0.284043 11.00000 0.03002 0.03276 = 0.02483 0.00819 0.00278 0.00462 AFIX 43 H32 2 0.291741 0.738450 0.246212 11.00000 -1.20000 AFIX 0 C33 1 0.380056 0.731893 0.355814 11.00000 0.02679 0.02237 = 0.02742 0.00505 0.00754 0.00568 AFIX 43 H33 2 0.348701 0.838837 0.366911 11.00000 -1.20000 AFIX 0 C34 1 0.459888 0.636607 0.411493 11.00000 0.01849 0.01737 = 0.02174 0.00141 0.00708 0.00001 HKLF 4 REM diant_b_a.res in P2(1)/n REM R1 = 0.0486 for 2804 Fo > 4sig(Fo) and 0.0500 for all 2934 data REM 196 parameters refined using 0 restraints END WGHT 0.0772 1.1094 REM Highest difference peak 0.528, deepest hole -0.538, 1-sigma level 0.066 Q1 1 0.8663 -0.1046 0.3413 11.00000 0.05 0.53 Q2 1 0.8756 -0.1602 0.4101 11.00000 0.05 0.52 Q3 1 0.6636 -0.1759 0.3014 11.00000 0.05 0.43 Q4 1 0.5462 0.4263 0.4256 11.00000 0.05 0.37 Q5 1 0.4260 0.6852 0.3817 11.00000 0.05 0.29 Q6 1 0.4725 0.6680 0.4511 11.00000 0.05 0.28 Q7 1 0.3770 0.7180 0.3172 11.00000 0.05 0.27 Q8 1 0.6390 0.4411 0.4810 11.00000 0.05 0.27 Q9 1 0.5090 0.4704 0.3563 11.00000 0.05 0.27 Q10 1 0.5016 0.5831 0.4025 11.00000 0.05 0.26 Q11 1 0.8057 0.0096 0.2989 11.00000 0.05 0.26 Q12 1 0.5757 0.6758 0.5084 11.00000 0.05 0.25 Q13 1 0.6891 0.6992 0.5440 11.00000 0.05 0.24 Q14 1 0.4261 0.4730 0.2979 11.00000 0.05 0.23 Q15 1 0.7510 0.4667 0.5245 11.00000 0.05 0.23 Q16 1 0.7004 0.1299 0.4587 11.00000 0.05 0.23 Q17 1 0.8731 0.0357 0.3727 11.00000 0.05 0.22 Q18 1 0.8663 0.5342 0.5444 11.00000 0.05 0.22 Q19 1 0.6309 0.3222 0.4501 11.00000 0.05 0.21 Q20 1 0.6739 0.5979 0.5025 11.00000 0.05 0.21 ; _shelx_res_checksum 75346 _shelx_hkl_file ; 0 0 2 166447. 834.080 1 0 0 3 33.1369 20.3593 1 0 0 4 19115.5 397.664 1 0 0 5 26.0654 33.9629 1 0 0 6 126230. 1303.92 1 0 0 7 52.5864 38.4343 11 0 0 7 24.6459 49.7000 1 0 0 8 109892. 1402.20 11 0 0 8 108412. 1456.45 1 0 0 9 61.4670 65.5297 11 0 0 9-5.93106 69.1438 1 0 0 10 235912. 2380.50 11 0 0 10 239795. 2593.73 1 0 0 11-42.4165 71.3754 11 0 0 11 39.4920 104.151 1 0 0 12 5023.00 411.454 11 0 0 13 146.209 109.386 11 0 0 14 11539.7 489.433 9 0 0 15-10.8568 67.7255 9 0 0 15-42.1157 66.0626 7 0 0 16 2370.12 230.939 7 0 0 16 2798.39 268.897 9 0 0 17 86.0099 87.7389 9 0 0 18 559.615 133.925 9 0 0 19 6.41462 72.8290 9 0 0 20 96.8233 63.8754 9 0 0 21 6.19002 44.6348 9 0 0 -22 300.943 62.7700 8 0 1 0 39.1524 10.0070 1 0 1 1 371707. 1097.28 1 0 -1 -2 84704.2 607.503 2 0 -1 2 83692.9 642.327 2 0 -1 2 85155.3 385.126 11 0 -1 3 426003. 1159.85 11 0 1 3 424146. 1755.35 1 0 1 4 772754. 2855.37 1 0 -1 4 782505. 2026.29 11 0 -1 4 782036. 2459.23 1 0 -1 4 771257. 2036.23 2 0 -1 5 30848.7 569.609 1 0 -1 5 31679.0 483.234 11 0 -1 6 1448.26 121.853 11 0 -1 6 1662.14 150.746 1 0 1 6 1688.00 160.701 1 0 -1 7 120207. 1226.72 11 0 1 7 121183. 1452.57 1 0 -1 8 7510.45 382.450 1 0 1 8 7932.39 407.457 1 0 1 9 126827. 1735.26 11 0 1 9 128796. 1778.54 1 0 -1 9 128410. 1537.84 11 0 1 10 195014. 2361.41 1 0 -1 10 195172. 2009.39 11 0 1 11 600.008 166.195 1 0 1 11 9820.76 561.539 11 0 1 12 2088.27 295.117 1 0 1 12 305.946 122.008 11 0 1 13 14466.0 774.307 11 0 1 14 1880.84 306.337 11 0 -1 14 1869.01 199.131 7 0 -1 14 1754.96 199.320 9 0 -1 15 87894.8 1420.10 9 0 -1 15 85324.7 1364.43 7 0 1 15 85790.6 1359.93 9 0 1 16 39309.1 947.895 9 0 -1 16 37513.8 924.204 7 0 -1 16 38493.6 968.154 9 0 1 17 1424.07 189.430 9 0 -1 17 1615.07 209.881 9 0 -1 18 23589.0 765.593 9 0 -1 19 1445.05 192.640 9 0 -1 20 3543.70 261.135 9 0 -1 -20 3371.52 243.699 8 0 -1 -21 739.171 107.428 8 0 -1 21 723.575 109.636 9 0 -1 -22 2070.98 140.939 8 0 -1 22 2093.75 142.616 9 0 2 0 51174.7 420.527 1 0 2 -1 185353. 749.336 1 0 2 1 185662. 949.017 1 0 -2 2 133172. 1147.63 2 0 2 2 132487. 961.436 1 0 -2 -2 133045. 1086.73 2 0 -2 3 105819. 1069.48 2 0 -2 -3 106340. 996.269 2 0 2 3 106012. 975.404 1 0 -2 -4 322273. 1764.64 2 0 2 4 322141. 1954.07 1 0 2 5 1514.93 150.890 1 0 -2 5 1697.09 139.290 2 0 -2 5 1760.35 86.7304 11 0 2 6 76470.4 1128.40 1 0 -2 6 77210.6 866.271 2 0 2 7 25837.0 712.542 1 0 2 8 29840.1 827.556 1 0 2 9 10686.7 536.735 1 0 2 10 1080.24 194.285 1 0 2 10 1304.91 214.418 11 0 2 11 142207. 2255.93 1 0 2 11 139034. 2236.84 11 0 2 12 4994.45 461.442 1 0 2 12 4374.35 430.367 11 0 -2 13 362.383 103.897 7 0 2 13 256.225 135.560 11 0 -2 14 29195.7 808.133 9 0 -2 14 29397.1 810.545 7 0 2 14 31174.4 1241.14 11 0 -2 15 12637.4 547.644 7 0 -2 15 13319.0 568.186 9 0 -2 16 516.623 132.944 9 0 -2 17 3964.75 327.649 9 0 -2 -18 4218.11 317.133 8 0 -2 18 4065.23 321.900 9 0 -2 -19 12482.7 501.918 8 0 -2 19 13532.1 549.488 9 0 -2 -20 96.4140 56.2884 8 0 -2 20 118.273 69.7608 9 0 -2 21 5594.32 279.319 9 0 -2 -21 5098.15 252.213 8 0 -2 22 3537.22 180.031 9 0 -3 0 26.7132 40.4461 2 0 3 0 1288.21 72.8972 1 0 -3 -1 1007.13 127.771 2 0 3 -1 949.229 44.7032 1 0 3 1 1309.86 91.8239 1 0 -3 1 1025.93 135.110 2 0 3 2 12186.8 325.395 1 0 -3 -2 12338.6 431.342 2 0 -3 2 12670.7 461.007 2 0 -3 3 7103.19 356.182 2 0 3 3 6601.41 278.084 1 0 -3 -3 6916.31 326.206 2 0 3 4 585.963 93.4749 1 0 -3 -4 1493.22 158.837 2 0 3 5 5675.73 302.676 1 0 -3 -5 6216.98 296.078 2 0 -3 5 6253.99 328.190 2 0 -3 6 45175.7 839.092 2 0 -3 -6 45960.6 761.194 2 0 3 7 44801.0 1002.10 1 0 3 8 273518. 2688.73 1 0 3 9 3679.99 362.370 11 0 3 9 2946.25 307.220 1 0 3 10 15759.6 748.121 1 0 3 10 17215.8 813.899 11 0 3 11 262.000 115.971 1 0 3 11 558.302 168.082 11 0 -3 12 5208.11 340.903 7 0 -3 -12 6002.64 413.833 8 0 3 12 5313.14 482.670 1 0 3 12 5764.49 517.159 11 0 -3 13 1936.36 222.386 7 0 -3 -13 2110.32 256.764 8 0 -3 13 2181.67 225.316 9 0 3 13 1999.32 345.294 11 0 -3 14 1166.73 174.759 9 0 -3 -14 1364.35 215.013 8 0 -3 15 14542.7 604.162 9 0 -3 -15 16227.7 694.564 8 0 -3 -16 12490.2 593.945 8 0 -3 16 11603.6 544.754 9 0 -3 17 8103.08 455.885 9 0 -3 -17 8841.03 480.394 8 0 -3 -18 14382.2 568.356 8 0 -3 18 15382.8 602.056 9 0 -3 19 87.0476 76.8927 9 0 -3 -19 229.252 83.1020 8 0 -3 -20 373.344 83.0148 8 0 -3 20 334.847 88.5981 9 0 -3 -21 5525.73 216.135 8 0 -3 21 5877.85 262.288 9 0 -4 0 1780.18 217.554 2 0 -4 1 12493.0 564.465 2 0 -4 -1 11760.0 533.891 2 0 -4 -2 103608. 1514.84 2 0 -4 2 105328. 1612.17 2 0 -4 -3 31536.2 813.263 2 0 -4 3 31554.5 873.774 2 0 -4 4 97051.7 1527.72 2 0 -4 -4 95904.8 1390.95 2 0 -4 -5 3470.26 257.137 2 0 -4 5 3112.43 270.252 2 0 4 5 3188.86 247.954 1 0 -4 -6 22409.0 648.371 2 0 4 6 20962.7 690.518 1 0 -4 6 21343.7 716.158 2 0 4 7 900.208 188.300 11 0 4 7 1057.71 171.362 1 0 4 8 239567. 2726.75 1 0 4 8 234586. 2974.91 11 0 4 9 12561.6 673.097 1 0 4 9 14135.7 769.487 11 0 4 10 13955.7 811.817 11 0 4 10 14475.5 776.841 1 0 4 11 2357.38 351.436 11 0 -4 -11 2773.29 296.782 8 0 4 11 1921.58 293.028 1 0 -4 11 2749.37 245.311 9 0 -4 12 40925.4 960.177 9 0 -4 -12 43109.4 1157.89 8 0 -4 13 20852.5 706.383 9 0 -4 -13 22533.8 843.139 8 0 -4 -14 800.767 165.406 8 0 -4 14 681.918 144.893 9 0 -4 15 10718.0 530.423 9 0 -4 -15 10968.5 566.299 8 0 -4 16 1068.34 177.462 9 0 -4 -16 962.764 171.670 8 0 -4 -17 1745.81 206.952 8 0 -4 17 1979.18 224.175 9 0 -4 -18 26234.2 682.569 8 0 -4 18 27883.0 740.112 9 0 -4 19 262.228 83.4311 9 0 -4 -19 192.432 66.2265 8 0 -4 -20 523.770 80.9499 10 0 -4 20 369.729 78.8636 9 0 -5 0 71.6703 90.8008 2 0 -5 1 122002. 1933.77 2 0 -5 -1 120444. 1870.25 2 0 -5 2 195512. 2466.23 2 0 -5 -2 195742. 2341.98 2 0 -5 3 33781.5 1014.87 2 0 -5 -3 32476.3 925.789 2 0 -5 4 1325.44 210.518 2 0 -5 -4 1203.62 183.223 2 0 5 5 146702. 2240.15 11 0 5 6 19120.3 863.285 11 0 5 7 5429.74 491.876 11 0 5 8 140117. 2596.68 11 0 -5 -9 160231. 2098.33 8 0 -5 -9 165526. 1747.93 5 0 -5 -10 152667. 2081.70 8 0 -5 -10 163860. 1699.48 5 0 -5 -11 5573.49 403.763 8 0 -5 -12 2696.39 283.263 8 0 -5 13 1289.67 192.488 9 0 -5 -13 849.144 164.655 8 0 -5 14 1011.09 170.754 9 0 -5 -14 891.472 171.097 8 0 -5 -15 7577.69 435.894 8 0 -5 15 7577.39 422.756 9 0 -5 16 1844.06 199.501 9 0 -5 17 881.669 132.378 9 0 -5 18 110.551 56.0336 9 0 -5 -18 105.718 60.6086 10 0 -5 -19 12950.8 357.257 10 0 -6 0 72487.5 1243.57 5 0 -6 1 81566.2 1288.96 5 0 -6 -1 80212.6 1309.66 5 0 -6 2 9043.42 424.467 5 0 -6 -2 8532.84 432.067 5 0 -6 -3 52254.2 1074.09 5 0 -6 3 54226.5 1008.86 5 0 -6 -4 73775.1 1289.28 5 0 -6 4 72771.7 1161.29 5 0 -6 -5 19329.0 667.205 5 0 -6 5 20461.1 597.059 5 0 -6 -6 27704.1 792.217 5 0 -6 -6 26821.2 827.297 10 0 -6 6 29219.3 696.294 5 0 -6 -7 221478. 2446.85 10 0 -6 -7 224618. 2233.73 5 0 -6 -8 138171. 1955.12 10 0 -6 -8 139701. 1728.44 5 0 -6 -9 1140.00 160.800 5 0 -6 -9 1907.77 246.254 10 0 -6 -10 21566.0 781.069 10 0 -6 -10 21115.4 625.896 5 0 -6 -11 2988.06 294.834 10 0 -6 -11 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1 -1 19 128.902 76.4760 9 -1 -1 -20 1816.03 167.951 8 1 -1 20 1926.43 187.713 9 1 -1 21 805.293 108.406 9 -1 -1 -21 768.298 94.8276 8 1 -2 -22 3779.91 195.590 8 -1 -2 22 3939.55 206.249 9 1 -2 -21 2077.17 178.647 8 -1 -2 21 2071.35 182.869 9 -1 -2 20 14207.9 521.832 9 1 -2 -20 13673.3 504.066 8 -1 -2 19 7308.97 408.910 9 1 -2 -19 7659.26 409.722 8 1 -2 -18 1862.90 217.364 8 -1 -2 18 2078.28 243.212 9 -1 -2 17 8783.74 486.098 9 -1 -2 16 86392.3 1491.60 9 -1 -2 15 44707.7 1046.15 9 -1 -2 14 175.280 78.5758 9 -1 2 14 302.774 165.105 11 -1 2 14 415.667 158.208 1 -1 2 13 2634.37 345.808 1 -1 2 13 2569.56 336.046 11 -1 2 12 37842.2 1198.81 1 -1 2 12 38134.9 1199.10 11 -1 2 11 64319.9 1456.30 1 -1 2 10 194940. 2383.92 1 -1 2 9 88349.4 1505.20 1 -1 2 8 151706. 1938.13 1 -1 -2 7 213841. 1548.51 2 -1 2 7 212374. 2021.75 1 -1 -2 6 15651.3 398.943 1 -1 2 6 17256.6 536.414 1 -1 -2 6 16524.8 424.682 2 -1 -2 5 83685.6 962.365 2 -1 2 5 80394.8 1072.05 1 -1 2 4 4586.03 235.469 1 -1 2 3 7267.43 280.425 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11 1 3 8 15018.6 646.674 1 1 3 8 14779.0 692.003 11 1 3 9 98777.3 1885.70 11 1 3 10 8319.27 590.475 11 1 3 11 42639.2 1409.11 11 1 3 12 13268.4 838.542 11 -1 -3 -12 13866.0 619.643 8 1 -3 12 12495.7 527.247 7 -1 -3 -13 1545.81 218.534 8 1 -3 13 1567.55 203.035 7 -1 -3 -14 7616.95 466.782 8 1 -3 14 7508.19 429.567 9 1 -3 14 7637.16 442.739 7 1 -3 15 17520.4 655.008 9 1 -3 15 17873.3 676.824 7 -1 -3 -15 17866.9 705.036 8 -1 -3 -16 64508.2 1289.52 8 1 -3 16 64133.6 1250.47 9 1 -3 17 13058.7 557.416 9 -1 -3 -17 13439.9 554.771 8 1 -3 18 3703.78 290.487 9 -1 -3 -18 3478.17 261.706 8 1 -3 19 380.658 103.184 9 -1 -3 -19 359.835 87.5930 8 -1 -3 -20 594.839 78.8894 8 1 -3 20 643.019 104.298 9 1 -3 21 342.600 64.4640 9 -1 -4 20 7.96624 49.5421 9 1 -4 -20 57.6847 42.8294 10 1 -4 -19 9420.78 377.996 8 -1 -4 19 10202.7 416.527 9 1 -4 -18 21574.4 659.733 8 -1 -4 18 21755.7 664.011 9 -1 -4 17 16887.6 621.193 9 1 -4 -17 17812.2 654.034 8 1 -4 -16 23010.3 790.787 8 -1 -4 16 24253.5 785.411 9 1 -4 -15 26529.2 883.115 8 -1 -4 15 26926.3 847.612 9 1 -4 -14 5183.02 402.983 8 -1 -4 14 5201.76 370.421 9 -1 -4 13 14010.0 594.100 9 1 -4 -13 14366.8 675.606 8 1 -4 -12 4839.79 400.733 8 -1 -4 12 4290.60 321.655 9 -1 4 12 3558.29 407.402 1 -1 -4 11 7262.62 399.147 9 -1 4 11 8549.01 615.313 1 -1 4 11 7755.88 626.439 11 1 -4 -11 8104.94 499.931 8 -1 4 10-235.981 103.736 1 -1 4 9 174.996 66.0652 1 -1 4 8 45019.8 1186.60 1 -1 -4 7 148075. 1955.70 2 -1 4 7 132469. 1917.68 1 -1 -4 6 6701.03 441.046 2 -1 4 6 6386.18 409.022 1 -1 4 5 100462. 1490.55 1 -1 -4 5 101871. 1662.46 2 -1 -4 4 7363.80 442.484 2 -1 4 4 6724.11 358.164 1 -1 4 3 169086. 1643.77 1 -1 -4 3 174087. 2089.17 2 1 -4 -2 41306.0 910.722 2 -1 -4 2 40023.7 989.491 2 -1 -4 1 64941.2 1248.83 2 1 -4 -1 63271.3 1149.42 2 -1 -4 0 102170. 1536.43 2 1 -4 0 105864. 1514.59 2 -1 -4 -1 199302. 2121.73 2 1 -4 1 200382. 2093.42 2 1 4 1 193454. 1639.91 11 -1 -4 -2 20427.5 676.114 2 1 4 2 18566.6 552.872 11 -1 -4 -3 9920.70 470.725 2 1 4 3 9453.10 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645.407 6 7 -2 4 18823.5 640.138 7 7 2 4 18076.2 634.252 7 7 -2 4 19870.6 1099.76 11 7 -2 5 63316.9 1184.79 7 7 2 5 60850.8 1148.72 7 7 -2 5 64910.1 1105.11 6 7 -2 6 32759.2 843.534 7 7 2 6 31841.9 826.430 7 7 -2 7 103919. 1490.38 7 7 2 7 104329. 1453.80 7 7 -2 8 2997.75 255.239 7 7 2 8 2836.53 238.675 7 7 -2 9 3371.78 261.546 7 7 2 9 3320.26 248.698 7 7 -2 10 26874.7 705.220 7 7 2 10 25101.6 633.641 7 7 -2 11 5819.42 321.699 7 7 2 11 5360.75 276.836 7 7 -2 12 6239.00 323.383 7 7 2 12 5572.98 262.034 7 7 -2 13 1334.74 147.059 7 7 2 13 1192.50 117.201 7 7 -2 14 11324.3 388.795 7 -7 -2 -14 10725.7 318.571 5 7 -2 15 9089.83 302.557 9 7 -2 15 8865.92 307.440 7 -7 -3 20 7447.60 276.208 9 -7 -3 19 12942.7 411.453 9 -7 -3 18 85.2334 63.1211 9 -7 -3 17 158.276 76.1088 9 -7 -3 16 763.974 135.590 9 -7 -3 15 8165.21 423.630 9 -7 -3 14 6040.34 377.038 9 -7 -3 13 5157.15 349.909 9 -7 -3 12 10908.9 513.094 9 -7 -3 11 22136.5 720.993 9 -7 -3 10 1599.63 198.831 9 -7 -3 9 45014.4 1005.79 9 -7 -3 8 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853.859 7 7 -3 8 60772.4 1086.47 7 7 3 8 59006.1 1006.08 7 7 -3 9 4106.35 284.684 7 7 3 9 4225.90 257.061 7 7 -3 10 558.501 115.270 7 7 -3 11 531.856 110.852 7 7 -3 12 3070.51 226.528 7 -7 -3 -12 3051.54 209.005 5 -7 -3 -13 160.454 56.7856 5 7 -3 13 99.8949 66.1927 7 7 -3 14 11869.5 369.856 7 -7 -3 -14 11528.0 297.391 5 -7 -4 19 5456.77 218.919 9 -7 -4 18 1399.67 131.003 9 -7 -4 17 15413.2 463.731 9 -7 -4 16 36.8768 50.4704 9 -7 -4 15 41693.8 866.697 9 -7 -4 14 9352.05 429.498 9 7 -4 -14 9432.31 399.595 10 -7 -4 13 232.204 86.7685 9 7 -4 -13 142.096 70.5030 10 -7 -4 12-40.2142 66.5974 9 7 -4 -12 51.1895 59.4613 10 -7 -4 11 22510.4 690.258 9 7 -4 -11 23171.1 716.802 10 -7 -4 10 310.511 98.7851 9 7 -4 -10 115.272 79.1195 10 7 -4 -9 15506.0 614.126 10 7 -4 -8 6076.45 390.152 10 7 -4 -7 79941.3 1414.02 10 -7 -4 6 8860.51 477.961 3 7 -4 -6 9354.42 482.252 10 -7 -4 5 99684.0 1564.42 3 7 -4 -5 94668.8 1529.50 10 -7 -4 4 45099.2 1054.65 3 7 -4 -4 43307.9 1022.05 10 -7 -4 3 7201.93 428.537 3 7 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11 0 -5 6259.86 376.380 7 -11 0 5 6120.04 349.700 9 -11 0 4 14.6270 58.4030 9 11 0 -4-15.4180 66.1188 7 11 0 -3 31502.9 830.250 7 11 0 -2 42.9591 69.8388 7 11 0 -1 2328.63 230.440 7 11 0 0 53.8216 73.1452 7 11 0 1 3530.60 261.601 7 11 0 2 84.7019 64.7521 7 11 0 3 335.248 86.1446 7 11 0 4-10.2397 50.4082 7 11 0 5 7067.10 287.856 7 11 0 6 97.9363 48.0379 7 11 0 7 25414.4 435.076 7 -11 -1 16 20123.1 396.794 9 -11 -1 15 1583.69 126.878 3 -11 1 15 1536.98 118.502 9 -11 -1 15 1605.15 129.563 9 -11 -1 14 647.546 93.9556 3 -11 1 14 621.786 89.4415 9 -11 -1 14 632.555 94.3786 9 -11 -1 13 9358.39 342.166 3 -11 1 13 10318.1 362.012 9 -11 -1 13 9763.17 361.935 9 -11 -1 12 4993.53 263.643 3 -11 1 12 5035.73 270.365 9 -11 -1 12 5071.39 273.557 9 -11 -1 11 690.872 112.782 3 -11 1 11 738.882 121.553 9 -11 -1 11 817.931 120.601 9 -11 -1 10 4201.83 259.376 3 -11 1 10 4221.09 275.172 9 -11 -1 10 4223.06 268.855 9 -11 -1 9 16703.5 523.866 3 -11 1 9 18145.9 570.590 9 -11 -1 9 17064.0 540.365 9 -11 -1 8 4250.08 269.294 3 -11 -1 8 4122.44 278.234 9 -11 -1 7 13189.5 479.234 3 -11 1 7 13936.3 520.544 9 -11 -1 7 13227.3 496.892 9 -11 -1 6 2677.15 223.170 3 -11 1 6 3243.81 251.194 9 -11 -1 6 3056.40 245.820 9 -11 -1 5 8000.47 376.015 3 11 1 -5 7525.41 435.886 7 -11 1 5 8457.96 404.979 9 -11 -1 5 8362.14 392.500 9 11 -1 -4 1786.64 188.704 7 11 1 -4 1651.04 209.667 7 -11 -1 4 2176.91 203.300 9 11 -1 -3 5250.84 319.497 7 11 1 -3 5574.69 362.924 7 11 -1 -2 1379.49 169.853 7 11 1 -2 1511.97 202.052 7 11 -1 -1 90.5428 79.6950 7 11 1 -1 98.1429 86.9639 7 11 -1 0 1320.75 159.944 7 11 1 0 1340.06 178.313 7 11 -1 1 9827.80 403.068 7 11 1 1 10068.4 441.095 7 11 -1 2 1105.25 134.655 7 11 1 2 1103.32 150.325 7 11 -1 3 10122.3 373.471 7 11 1 3 10660.3 404.121 7 11 -1 4 14411.1 416.576 7 11 1 4 15573.6 456.416 7 11 -1 5 117.561 45.7369 7 11 1 5 132.196 59.7154 7 11 -1 6 875.416 92.1710 7 11 1 6 825.573 94.3426 7 -11 -2 15 1402.14 114.015 3 -11 -2 15 1475.10 111.171 9 -11 -2 14 2298.41 159.207 3 -11 -2 14 2257.23 149.958 9 -11 2 13 239.911 55.5859 9 -11 -2 13 258.066 63.8882 9 -11 -2 13 303.244 79.2207 3 -11 -2 12 17444.5 477.490 3 -11 2 12 18822.5 450.838 9 -11 -2 12 17772.4 465.297 9 -11 -2 11 848.535 118.547 3 -11 2 11 958.656 116.436 9 -11 -2 11 798.485 107.056 9 -11 -2 10 5952.29 301.729 3 -11 2 10 6804.53 306.351 9 -11 -2 10 6352.34 299.449 9 -11 -2 9 5228.31 290.187 3 -11 2 9 5351.36 283.325 9 -11 -2 9 5169.08 274.575 9 -11 -2 8 5813.12 311.019 3 -11 2 8 6266.03 311.963 9 -11 -2 8 5431.65 292.235 9 -11 -2 7 9365.31 398.796 3 -11 -2 7 9572.23 389.294 9 -11 -2 6 47.7394 53.5410 9 -11 -2 6 6.58832 66.3552 3 -11 -2 5 919.028 144.333 3 -11 -2 5 550.312 104.053 9 11 2 -4 38885.7 947.936 7 11 2 -3 42002.9 970.221 7 11 2 -2 2096.62 224.115 7 11 2 -1 90.1458 79.9298 7 11 2 0 8601.08 411.329 7 11 2 1 997.900 149.244 7 11 -2 2 1382.63 126.766 7 11 2 2 1589.97 168.577 7 11 -2 3 6396.11 252.326 7 11 2 3 7074.71 317.067 7 11 -2 4 3777.68 182.862 7 11 2 4 4110.87 223.355 7 11 2 5 192.963 57.8858 7 -11 -3 14 7628.81 252.716 3 -11 -3 13 10068.2 320.609 3 -11 -3 13 10521.0 285.255 9 -11 -3 12 721.918 97.0497 3 -11 -3 12 708.492 83.8860 9 -11 -3 11 10905.6 368.392 3 -11 -3 11 10767.2 324.838 9 -11 -3 10 13394.7 420.103 3 -11 -3 10 12939.9 372.758 9 -11 -3 9 9212.99 363.444 3 -11 -3 9 9253.28 324.067 9 -11 -3 8 19118.4 535.027 3 -11 -3 8 19408.2 475.617 9 -11 -3 7 2477.39 205.210 3 -11 -3 7 2463.36 172.535 9 -11 -3 6 518.608 113.466 3 -11 -3 6 413.931 78.4430 9 11 3 -5 27224.2 783.327 7 -11 -3 5 27212.0 658.375 3 11 3 -4 2840.89 248.818 7 11 3 -3 15631.9 556.311 7 11 3 -2 4583.01 299.857 7 11 3 -1 1894.55 193.163 7 11 3 0 99.5682 66.7320 7 11 3 1 652.715 108.372 7 11 3 2 4716.47 246.101 7 11 3 3 8999.89 312.920 7 11 3 4 2159.58 139.319 7 -11 -4 12 1613.31 122.213 3 -11 -4 11 43361.4 646.976 3 -11 -4 10 29728.3 562.471 3 -11 -4 9 2034.30 161.547 3 -11 -4 8 3298.01 203.828 3 -11 -4 7 1181.95 132.266 3 11 4 -6 2003.20 202.396 7 11 4 -5 2930.61 227.879 7 11 4 -4 2568.26 209.622 7 11 4 -3 10863.9 410.022 7 11 4 -2 13784.7 446.294 7 11 4 -1 47755.7 791.464 7 11 4 0 2202.36 165.915 7 11 4 1 771.510 94.4807 7 -12 0 13 24.6819 33.1103 9 -12 0 12 298.184 62.3114 9 -12 0 11 6.63798 40.0273 9 -12 0 10 6483.54 274.025 9 -12 0 9-6.55348 41.3131 9 12 0 -8 7178.23 279.513 7 -12 0 8 6606.73 290.508 9 12 0 -7 14.8372 43.4473 7 12 0 -6 1855.78 159.466 7 12 0 -5 35.1161 54.5067 7 12 0 -4 7357.73 320.463 7 12 0 -3 28.5103 50.4711 7 12 0 -2 42617.8 743.125 7 12 0 -1 12.2884 49.8099 7 12 0 0 1420.73 133.018 7 12 0 1 54.5313 43.2448 7 12 0 2 17873.8 399.482 7 -12 -1 13 174.305 45.1103 9 -12 1 12 4041.61 181.121 9 -12 -1 12 3950.60 191.671 9 12 1 -11 28689.1 496.760 7 -12 1 11 29655.2 527.231 9 -12 -1 11 29082.3 538.062 9 -12 -1 10 332.558 72.3032 3 -12 -1 10 417.777 75.1392 9 12 1 -9 3853.75 217.168 7 -12 -1 9 3795.03 210.368 9 -12 -1 9 3323.59 185.195 3 12 1 -8 10783.7 375.612 7 -12 -1 8 10805.7 356.667 9 12 1 -7 15716.0 466.369 7 12 1 -6 4486.09 258.371 7 12 1 -5 3672.48 236.393 7 12 1 -4 7351.20 332.984 7 12 1 -3 494.813 100.098 7 12 -1 -2 19600.5 439.423 7 12 1 -2 20771.2 541.241 7 12 -1 -1 9258.81 294.326 7 12 1 -1 9964.61 364.399 7 12 -1 0 2778.01 158.183 7 12 1 0 3255.99 201.826 7 12 -1 1 8350.98 254.524 7 12 1 1 9644.48 322.282 7 12 1 2 6189.56 242.183 7 -12 -2 12 6321.66 206.771 9 -12 -2 11 24265.6 435.103 3 12 2 -11 25654.4 486.621 7 -12 -2 11 25158.4 436.368 9 -12 -2 10 32.4255 35.6651 9 -12 -2 10 60.6578 48.1959 3 12 2 -10 64.8372 47.0308 7 -12 -2 9 333.827 70.7012 3 12 2 -9 152.332 57.6390 7 -12 -2 9 318.037 62.0447 9 12 2 -8 42.3274 55.5860 7 12 2 -7 1230.66 135.905 7 12 2 -6 4498.61 255.462 7 12 2 -5 2011.48 177.602 7 12 2 -4 15219.7 465.621 7 12 2 -3 103612. 1196.82 7 12 2 -2 1930.77 167.742 7 12 2 -1 563.622 94.5476 7 12 2 0 79.0297 51.5230 7 12 2 1 3722.68 191.038 7 12 3 -10 13951.3 352.779 7 12 3 -9 2504.16 162.948 7 12 3 -8 15595.7 411.783 7 12 3 -7 5985.79 263.161 7 12 3 -6 3731.76 213.089 7 12 3 -5 10001.3 344.075 7 12 3 -4 360.615 79.9779 7 12 3 -3 8168.76 304.637 7 12 3 -2 114.336 55.1954 7 12 3 -1 5515.47 227.405 7 0 0 0 0.00 0.00 0 TITL diant_b in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 10.420637 7.930106 18.775877 90.0000 104.0585 90.0000 ZERR 4.00 0.000270 0.000222 0.000514 0.0000 0.0028 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H O S UNIT 68.00 64.00 12.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 18674 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 1.455 _oxdiff_exptl_absorpt_empirical_full_min 0.618 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn S1S S 0.80205(5) -0.11609(6) 0.30026(3) 0.0339(2) Uani 1 1 d . O2S O 0.84838(15) 0.0587(2) 0.32500(9) 0.0388(4) Uani 1 1 d . C3S C 0.6263(3) -0.0966(4) 0.26737(18) 0.0615(8) Uani 1 1 d . H3SA H 0.588611 -0.053899 0.306855 0.092 Uiso 1 1 calc GR H3SB H 0.588148 -0.207316 0.251420 0.092 Uiso 1 1 calc GR H3SC H 0.606085 -0.018069 0.225861 0.092 Uiso 1 1 calc GR C4S C 0.8012(4) -0.2371(4) 0.37855(19) 0.0722(10) Uani 1 1 d . H4SA H 0.891887 -0.248831 0.408582 0.108 Uiso 1 1 calc GR H4SB H 0.764606 -0.348946 0.363475 0.108 Uiso 1 1 calc GR H4SC H 0.746721 -0.180896 0.407263 0.108 Uiso 1 1 calc GR O5 O 0.63187(17) 0.08658(18) 0.43459(9) 0.0385(4) Uani 1 1 d . O6 O 0.74340(13) 0.28625(17) 0.39159(8) 0.0269(3) Uani 1 1 d . H6 H 0.773(3) 0.203(4) 0.3712(14) 0.040 Uiso 1 1 d R C4 C 0.65774(16) 0.2333(2) 0.42857(9) 0.0205(4) Uani 1 1 d . C21 C 0.50009(16) 0.6976(2) 0.49008(9) 0.0184(4) Uani 1 1 d . H21 H 0.489183 0.822929 0.489468 0.022 Uiso 1 1 calc R C22 C 0.64524(16) 0.6597(2) 0.51991(9) 0.0191(4) Uani 1 1 d . C23 C 0.73117(18) 0.7774(2) 0.56113(10) 0.0246(4) Uani 1 1 d . H23 H 0.698281 0.883928 0.571558 0.030 Uiso 1 1 calc R C24 C 0.86445(19) 0.7405(3) 0.58712(11) 0.0305(4) Uani 1 1 d . H24 H 0.922994 0.821856 0.614628 0.037 Uiso 1 1 calc R C25 C 0.91149(18) 0.5842(3) 0.57268(10) 0.0303(4) Uani 1 1 d . H25 H 1.002618 0.558186 0.590680 0.036 Uiso 1 1 calc R C26 C 0.82650(17) 0.4648(2) 0.53203(10) 0.0246(4) Uani 1 1 d . H26 H 0.859572 0.357309 0.522994 0.030 Uiso 1 1 calc R C27 C 0.69299(16) 0.5023(2) 0.50451(9) 0.0186(4) Uani 1 1 d . C28 C 0.59127(16) 0.3797(2) 0.45987(9) 0.0171(4) Uani 1 1 d . C29 C 0.50572(15) 0.4789(2) 0.39493(9) 0.0180(4) Uani 1 1 d . C30 C 0.46964(17) 0.4190(2) 0.32339(10) 0.0220(4) Uani 1 1 d . H30 H 0.499252 0.311168 0.312132 0.026 Uiso 1 1 calc R C31 C 0.39033(19) 0.5159(3) 0.26804(10) 0.0273(4) Uani 1 1 d . H31 H 0.366824 0.474590 0.219096 0.033 Uiso 1 1 calc R C32 C 0.34566(19) 0.6722(3) 0.28404(10) 0.0299(4) Uani 1 1 d . H32 H 0.291741 0.738450 0.246212 0.036 Uiso 1 1 calc R C33 C 0.38006(18) 0.7319(2) 0.35581(10) 0.0254(4) Uani 1 1 d . H33 H 0.348701 0.838837 0.366911 0.030 Uiso 1 1 calc R C34 C 0.45989(16) 0.6366(2) 0.41149(9) 0.0188(4) 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 S1S 0.0456(3) 0.0219(3) 0.0431(3) -0.00692(19) 0.0278(2) -0.00425(19) O2S 0.0382(8) 0.0289(8) 0.0587(10) -0.0168(7) 0.0299(7) -0.0096(6) C3S 0.0496(15) 0.0638(19) 0.0699(19) -0.0274(15) 0.0119(13) -0.0175(13) C4S 0.116(3) 0.0453(17) 0.072(2) 0.0231(14) 0.054(2) 0.0296(17) O5 0.0569(10) 0.0166(7) 0.0534(9) -0.0019(6) 0.0355(8) 0.0034(6) O6 0.0276(7) 0.0226(7) 0.0350(7) -0.0070(5) 0.0163(5) -0.0005(5) C4 0.0210(8) 0.0191(9) 0.0216(8) -0.0019(6) 0.0056(6) 0.0022(6) C21 0.0213(8) 0.0123(8) 0.0224(8) -0.0001(6) 0.0070(6) 0.0003(6) C22 0.0214(8) 0.0172(8) 0.0199(8) 0.0001(6) 0.0073(6) -0.0012(6) C23 0.0269(9) 0.0210(9) 0.0268(9) -0.0051(7) 0.0082(7) -0.0038(7) C24 0.0265(9) 0.0337(11) 0.0303(9) -0.0089(8) 0.0048(7) -0.0099(8) C25 0.0185(8) 0.0407(11) 0.0297(9) -0.0040(8) 0.0021(7) -0.0010(8) C26 0.0214(8) 0.0261(9) 0.0259(9) -0.0020(7) 0.0050(7) 0.0028(7) C27 0.0196(8) 0.0182(8) 0.0185(7) -0.0004(6) 0.0055(6) -0.0008(6) C28 0.0171(7) 0.0152(8) 0.0197(8) -0.0006(6) 0.0060(6) 0.0015(6) C29 0.0159(7) 0.0165(8) 0.0215(8) 0.0012(6) 0.0047(6) -0.0010(6) C30 0.0222(8) 0.0204(8) 0.0238(8) -0.0016(7) 0.0063(6) -0.0024(7) C31 0.0285(9) 0.0326(10) 0.0196(8) -0.0005(7) 0.0036(7) -0.0037(8) C32 0.0300(9) 0.0328(10) 0.0248(9) 0.0082(8) 0.0028(7) 0.0046(8) C33 0.0268(9) 0.0224(9) 0.0274(9) 0.0051(7) 0.0075(7) 0.0057(7) C34 0.0185(7) 0.0174(8) 0.0217(8) 0.0014(6) 0.0071(6) 0.0000(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 1 0 -1 0.2285 -1 0 1 0.1665 0 -1 0 0.3162 0 1 0 0.3162 0 -1 1 0.3041 0 1 -1 0.3071 0 0 -1 0.1039 0 0 1 0.1983 0 -1 -1 0.2923 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 O2S S1S C3S 104.58(12) . . O2S S1S C4S 108.13(15) . . C4S S1S C3S 97.06(18) . . S1S C3S H3SA 109.5 . . S1S C3S H3SB 109.5 . . S1S C3S H3SC 109.5 . . H3SA C3S H3SB 109.5 . . H3SA C3S H3SC 109.5 . . H3SB C3S H3SC 109.5 . . S1S C4S H4SA 109.5 . . S1S C4S H4SB 109.5 . . S1S C4S H4SC 109.5 . . H4SA C4S H4SB 109.5 . . H4SA C4S H4SC 109.5 . . H4SB C4S H4SC 109.5 . . C4 O6 H6 110.8(19) . . O5 C4 O6 123.32(16) . . O5 C4 C28 124.08(16) . . O6 C4 C28 112.55(14) . . C22 C21 H21 107.6 . . C22 C21 C28 112.83(13) . 3_666 C22 C21 C34 108.26(13) . . C28 C21 H21 107.6 3_666 . C34 C21 H21 107.6 . . C34 C21 C28 112.59(13) . 3_666 C23 C22 C21 121.61(16) . . C23 C22 C27 120.00(16) . . C27 C22 C21 118.38(15) . . C22 C23 H23 119.7 . . C24 C23 C22 120.56(18) . . C24 C23 H23 119.7 . . C23 C24 H24 120.3 . . C25 C24 C23 119.49(17) . . C25 C24 H24 120.3 . . C24 C25 H25 119.7 . . C24 C25 C26 120.56(17) . . C26 C25 H25 119.7 . . C25 C26 H26 119.9 . . C25 C26 C27 120.22(17) . . C27 C26 H26 119.9 . . C22 C27 C28 116.50(14) . . C26 C27 C22 119.14(16) . . C26 C27 C28 124.33(16) . . C4 C28 C21 108.64(13) . 3_666 C4 C28 C29 108.09(13) . . C27 C28 C4 111.86(13) . . C27 C28 C21 110.55(13) . 3_666 C27 C28 C29 107.46(13) . . C29 C28 C21 110.21(13) . 3_666 C30 C29 C28 124.06(15) . . C30 C29 C34 119.60(15) . . C34 C29 C28 116.31(14) . . C29 C30 H30 119.8 . . C29 C30 C31 120.38(17) . . C31 C30 H30 119.8 . . C30 C31 H31 119.9 . . C32 C31 C30 120.21(17) . . C32 C31 H31 119.9 . . C31 C32 H32 120.2 . . C31 C32 C33 119.66(17) . . C33 C32 H32 120.2 . . C32 C33 H33 119.7 . . C34 C33 C32 120.65(18) . . C34 C33 H33 119.7 . . C29 C34 C21 118.29(15) . . C33 C34 C21 122.22(16) . . C33 C34 C29 119.50(16) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 S1S O2S 1.5037(15) . S1S C3S 1.791(3) . S1S C4S 1.757(3) . C3S H3SA 0.9800 . C3S H3SB 0.9800 . C3S H3SC 0.9800 . C4S H4SA 0.9800 . C4S H4SB 0.9800 . C4S H4SC 0.9800 . O5 C4 1.206(2) . O6 H6 0.86(3) . O6 C4 1.325(2) . C4 C28 1.540(2) . C21 H21 1.0000 . C21 C22 1.510(2) . C21 C28 1.613(2) 3_666 C21 C34 1.512(2) . C22 C23 1.391(2) . C22 C27 1.399(2) . C23 H23 0.9500 . C23 C24 1.387(3) . C24 H24 0.9500 . C24 C25 1.384(3) . C25 H25 0.9500 . C25 C26 1.391(3) . C26 H26 0.9500 . C26 C27 1.394(2) . C27 C28 1.530(2) . C28 C29 1.540(2) . C29 C30 1.388(2) . C29 C34 1.400(2) . C30 H30 0.9500 . C30 C31 1.392(3) . C31 H31 0.9500 . C31 C32 1.382(3) . C32 H32 0.9500 . C32 C33 1.391(3) . C33 H33 0.9500 . C33 C34 1.390(2) . 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_4 O5 C4 C28 C21 7.7(2) . 3_666 O5 C4 C28 C27 130.02(19) . . O5 C4 C28 C29 -111.9(2) . . O6 C4 C28 C21 -174.75(13) . 3_666 O6 C4 C28 C27 -52.44(18) . . O6 C4 C28 C29 65.66(17) . . C4 C28 C29 C30 15.1(2) . . C4 C28 C29 C34 -166.89(14) . . C21 C22 C23 C24 -179.13(17) . . C21 C22 C27 C26 -179.57(15) . . C21 C22 C27 C28 -1.6(2) . . C21 C28 C29 C30 -103.46(18) 3_666 . C21 C28 C29 C34 74.52(17) 3_666 . C22 C21 C34 C29 43.3(2) . . C22 C21 C34 C33 -136.47(17) . . C22 C23 C24 C25 -0.9(3) . . C22 C27 C28 C4 164.57(14) . . C22 C27 C28 C21 -74.22(18) . 3_666 C22 C27 C28 C29 46.08(19) . . C23 C22 C27 C26 1.1(2) . . C23 C22 C27 C28 179.09(15) . . C23 C24 C25 C26 0.4(3) . . C24 C25 C26 C27 0.9(3) . . C25 C26 C27 C22 -1.6(3) . . C25 C26 C27 C28 -179.43(17) . . C26 C27 C28 C4 -17.6(2) . . C26 C27 C28 C21 103.64(18) . 3_666 C26 C27 C28 C29 -136.05(17) . . C27 C22 C23 C24 0.2(3) . . C27 C28 C29 C30 136.02(16) . . C27 C28 C29 C34 -46.00(19) . . C28 C21 C22 C23 -98.72(18) 3_666 . C28 C21 C22 C27 81.98(18) 3_666 . C28 C21 C34 C29 -82.17(18) 3_666 . C28 C21 C34 C33 98.09(19) 3_666 . C28 C29 C30 C31 179.05(16) . . C28 C29 C34 C21 1.4(2) . . C28 C29 C34 C33 -178.82(15) . . C29 C30 C31 C32 -0.7(3) . . C30 C29 C34 C21 179.51(15) . . C30 C29 C34 C33 -0.7(2) . . C30 C31 C32 C33 -0.2(3) . . C31 C32 C33 C34 0.6(3) . . C32 C33 C34 C21 179.63(17) . . C32 C33 C34 C29 -0.1(3) . . C34 C21 C22 C23 135.98(16) . . C34 C21 C22 C27 -43.3(2) . . C34 C29 C30 C31 1.1(3) . . 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 0.9965 -0.0119 -0.9921 -0.1117 0.1056 -0.0185 -0.9965 0.0119 0.9921 0.1117 -0.1056 0.0185 -0.0245 -0.9980 0.0277 -0.0115 0.0201 0.1924 0.0245 0.9980 -0.0277 0.0115 -0.0201 -0.1924 -0.0265 -0.9949 1.0284 -0.0483 -0.0558 0.1982 0.0265 0.9949 -1.0284 0.0483 0.0558 -0.1982 0.0020 -0.0030 -1.0007 0.0368 0.0759 -0.0058 -0.0020 0.0030 1.0007 -0.0368 -0.0759 0.0058 -0.0225 -1.0010 -0.9730 0.0252 0.0961 0.1865