#------------------------------------------------------------------------------ #$Date: 2019-11-04 18:07:44 +0200 (Mon, 04 Nov 2019) $ #$Revision: 223207 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/12/72/4127268.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_4127268 loop_ _publ_author_name 'Hugelshofer, Cedric L.' 'Palani, Vignesh' 'Sarpong, Richmond' _publ_section_title ; Calyciphylline B-Type Alkaloids: Total Syntheses of (-)-Daphlongamine H and (-)-Isodaphlongamine H. ; _journal_issue 21 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 8431 _journal_page_last 8435 _journal_paper_doi 10.1021/jacs.9b03576 _journal_volume 141 _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_moiety 'C13 H21 N O3 S' _chemical_formula_sum 'C13 H21 N O3 S' _chemical_formula_weight 271.37 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.17650(10) _cell_length_b 9.22680(10) _cell_length_c 24.6586(2) _cell_measurement_reflns_used 13695 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 78.7500 _cell_measurement_theta_min 4.8220 _cell_volume 1405.28(3) _computing_cell_refinement 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'ROD, Synergy Custom DW system, Pilatus 200K' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_unetI/netI 0.0141 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 14126 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 74.000 _diffrn_reflns_theta_max 74.496 _diffrn_reflns_theta_min 5.118 _diffrn_source 'Rotating-anode X-ray tube' _exptl_absorpt_coefficient_mu 2.060 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.70346 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Olex2 1.2-ac3 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.283 _exptl_crystal_description block _exptl_crystal_F_000 584 _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.180 _refine_diff_density_max 0.236 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.039 _refine_ls_abs_structure_details ; Flack x determined using 1175 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.011(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 170 _refine_ls_number_reflns 2854 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0249 _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^)+(0.0382P)^2^+0.4717P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.0660 _reflns_Friedel_coverage 0.704 _reflns_Friedel_fraction_full 0.995 _reflns_Friedel_fraction_max 0.995 _reflns_number_gt 2854 _reflns_number_total 2854 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja9b03576_si_004.cif _cod_data_source_block CH6_131p _cod_depositor_comments 'Adding full bibliography for 4127268.cif.' _cod_database_code 4127268 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.533 _shelx_estimated_absorpt_t_max 0.708 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL ch6_131p_a.res in P2(1)2(1)2(1) CELL 1.54184 6.1765 9.2268 24.6586 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0001 0.0002 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O S UNIT 52 84 4 12 4 MERG 2 FMAP 2 PLAN 5 SIZE 0.180 0.210 0.350 ACTA 148.00 BOND $H LIST 4 WPDB -2 L.S. 10 TEMP -173.00 WGHT 0.038200 0.471700 FVAR 12.85096 C1 1 0.354944 0.075124 0.721142 11.00000 0.02708 0.01662 = 0.01965 0.00357 -0.00095 0.00044 AFIX 137 H1A 2 0.395328 0.020375 0.688623 11.00000 -1.50000 H1B 2 0.255994 0.016995 0.743325 11.00000 -1.50000 H1C 2 0.485295 0.097694 0.742168 11.00000 -1.50000 AFIX 0 C2 1 0.242970 0.215990 0.704466 11.00000 0.01549 0.01690 = 0.01807 0.00174 0.00098 -0.00197 C3 1 0.183267 0.304466 0.754481 11.00000 0.02596 0.02205 = 0.02404 0.00106 0.01077 0.00074 AFIX 137 H3A 2 0.315082 0.329566 0.774510 11.00000 -1.50000 H3B 2 0.087355 0.247313 0.777827 11.00000 -1.50000 H3C 2 0.108978 0.393400 0.743264 11.00000 -1.50000 AFIX 0 C4 1 0.049411 0.185656 0.667996 11.00000 0.01993 0.03023 = 0.03151 0.01054 -0.00580 -0.00846 AFIX 137 H4A 2 -0.016484 0.277541 0.656818 11.00000 -1.50000 H4B 2 -0.057307 0.127698 0.687861 11.00000 -1.50000 H4C 2 0.097388 0.132197 0.635826 11.00000 -1.50000 AFIX 0 C5 1 0.462869 0.583624 0.634129 11.00000 0.01225 0.01466 = 0.01413 0.00035 -0.00044 -0.00137 AFIX 13 H5 2 0.594052 0.586679 0.657869 11.00000 -1.20000 AFIX 0 C6 1 0.357551 0.730866 0.636840 11.00000 0.01787 0.01608 = 0.02089 -0.00325 0.00077 0.00226 AFIX 43 H6 2 0.255880 0.759071 0.663753 11.00000 -1.20000 AFIX 0 C7 1 0.424663 0.815962 0.596958 11.00000 0.02219 0.01389 = 0.02556 0.00068 -0.00109 0.00107 AFIX 43 H7 2 0.382025 0.914273 0.592839 11.00000 -1.20000 AFIX 0 C8 1 0.575631 0.739025 0.559126 11.00000 0.01788 0.01485 = 0.02294 0.00482 0.00171 -0.00216 AFIX 23 H8A 2 0.727321 0.769613 0.565228 11.00000 -1.20000 H8B 2 0.536515 0.757775 0.520829 11.00000 -1.20000 AFIX 0 C9 1 0.543620 0.575746 0.573852 11.00000 0.01123 0.01331 = 0.01474 0.00117 0.00046 0.00045 C10 1 0.764584 0.501868 0.571671 11.00000 0.01303 0.01672 = 0.01880 0.00300 0.00252 -0.00039 C11 1 0.659571 0.365789 0.490621 11.00000 0.01895 0.02101 = 0.01983 -0.00300 0.00258 0.00084 AFIX 23 H11A 2 0.599202 0.273913 0.504811 11.00000 -1.20000 H11B 2 0.731114 0.344534 0.455585 11.00000 -1.20000 AFIX 0 C12 1 0.477410 0.471770 0.481282 11.00000 0.01687 0.02264 = 0.01500 0.00060 0.00068 0.00053 AFIX 23 H12A 2 0.367781 0.428607 0.456849 11.00000 -1.20000 H12B 2 0.533853 0.561082 0.464102 11.00000 -1.20000 AFIX 0 C13 1 0.375233 0.507816 0.535886 11.00000 0.01166 0.01815 = 0.01368 0.00126 -0.00157 0.00113 AFIX 23 H13A 2 0.316794 0.418344 0.552524 11.00000 -1.20000 H13B 2 0.253691 0.576277 0.530518 11.00000 -1.20000 AFIX 0 N1 3 0.324589 0.466424 0.653971 11.00000 0.01077 0.01535 = 0.01610 0.00196 -0.00055 0.00009 O1 4 0.495060 0.226989 0.616504 11.00000 0.02188 0.02060 = 0.01581 -0.00132 0.00190 0.00506 O2 4 0.899223 0.522854 0.606419 11.00000 0.01258 0.03027 = 0.02460 -0.00061 -0.00294 0.00091 O3 4 0.820962 0.421421 0.528929 11.00000 0.01346 0.02400 = 0.02378 -0.00321 0.00153 0.00314 S1 5 0.457173 0.313319 0.666907 11.00000 0.01188 0.01433 = 0.01387 0.00125 -0.00010 0.00105 H1 2 0.194190 0.454735 0.636182 11.00000 0.02143 HKLF 4 REM ch6_131p_a.res in P2(1)2(1)2(1) REM R1 = 0.0249 for 2854 Fo > 4sig(Fo) and 0.0249 for all 2854 data REM 170 parameters refined using 0 restraints END WGHT 0.0385 0.4660 REM Highest difference peak 0.236, deepest hole -0.212, 1-sigma level 0.039 Q1 1 0.4931 0.5753 0.6024 11.00000 0.05 0.24 Q2 1 0.3259 0.2585 0.6904 11.00000 0.05 0.22 Q3 1 0.4608 0.5359 0.5600 11.00000 0.05 0.22 Q4 1 0.5557 0.6539 0.5666 11.00000 0.05 0.21 Q5 1 0.4275 0.4883 0.5091 11.00000 0.05 0.21 ; _shelx_res_checksum 93770 _shelx_hkl_file ; 0 0 3 86.3603 16.3978 6 0 0 -3 63.1829 13.3959 23 0 0 -5 151.143 22.6748 6 0 0 5 141.109 25.4906 8 0 0 -5 164.890 26.8145 23 0 0 5 99.0134 26.8820 6 0 0 6 360822. 1425.75 6 0 0 -7 49.8141 17.9062 6 0 0 7 7.58093 24.5071 8 0 0 -8 75564.2 410.163 6 0 0 -8 75654.7 491.890 23 0 0 9 109.034 28.2284 8 0 0 -9 188.996 30.7307 23 0 0 10 219241. 1129.24 8 0 0 11 1475.48 80.4588 8 0 0 12 102555. 743.870 8 0 0 13 216.729 41.4022 8 0 0 -13 224.708 75.1503 9 0 0 -13-25.2516 84.0659 11 0 0 -13 161.989 94.2954 3 0 0 -14 93345.2 1198.24 11 0 0 14 94907.2 788.915 8 0 0 -14 92245.0 1359.87 3 0 0 -15 93.5626 41.1408 19 0 0 -15 131.073 43.7085 16 0 0 -15 33.5823 106.126 11 0 0 -15 53.8719 48.0728 22 0 0 -15 60.6842 72.9662 9 0 0 -15 142.491 109.660 3 0 0 -16 109475. 950.708 22 0 0 -16 100201. 1340.43 11 0 0 -16 112928. 895.828 16 0 0 -16 104884. 884.259 19 0 0 -16 117839. 1278.22 9 0 0 -17 133.904 54.3480 16 0 0 -17 86.0247 121.729 11 0 0 -17 54.0306 51.1164 19 0 0 -17 45.1992 61.3148 22 0 0 -17 9.93817 80.9905 9 0 0 -18 97150.9 915.407 16 0 0 -18 99104.7 986.853 22 0 0 -19 98.3549 63.2274 19 0 0 -19 57.7111 148.105 11 0 0 -19 164.342 77.5097 22 0 0 -19 21.5332 86.2670 9 0 0 -19 65.2715 60.1395 16 0 0 -20 83224.0 886.650 16 0 0 -20 75408.0 1298.24 11 0 0 -20 89089.3 968.795 22 0 0 -20 90246.7 1206.97 9 0 0 -20 80597.2 874.724 19 0 0 -21 52.1023 165.759 11 0 0 -21 54.1359 106.957 9 0 0 -21 30.7117 75.9733 16 0 0 -21 20.9646 65.2367 19 0 0 -21 79.1164 86.1444 22 0 0 -22 250645. 1826.43 22 0 0 -22 271571. 2235.90 9 0 0 -22 237349. 1703.11 16 0 0 -22 260435. 1758.96 19 0 0 -22 237089. 2390.58 11 0 0 -23 121.438 170.217 11 0 0 -23 67.9002 79.0337 19 0 0 -23 9.18948 67.5559 16 0 0 -23 56.7835 93.8794 22 0 0 -23 11.4918 102.875 9 0 0 -24 52135.6 1070.67 11 0 0 -24 51232.3 696.478 19 0 0 -25 76.2611 162.672 11 0 0 -25 96.1295 76.4921 19 0 0 -25 56.9605 99.2062 9 0 0 -25 65.7295 74.6420 16 0 0 -26 39399.4 574.576 19 0 0 -26 41310.3 607.331 16 0 0 -27 91.8658 117.055 11 0 0 -27 292.597 97.8057 9 0 0 -27 65.3169 61.6853 19 0 0 -28 3721.71 148.886 19 0 0 -28 3875.51 161.481 16 0 0 -28 3881.26 193.044 9 0 0 -28 3264.30 217.510 11 0 0 -29 4.36112 79.7886 11 0 0 -29 117.317 55.4193 9 0 0 -29 45.4013 45.5381 16 0 0 -30 94330.9 636.057 16 0 0 -30 117343. 968.439 11 0 -1 0 40.3879 25.2519 1 0 1 0 23.9370 22.8868 1 0 -1 -1 194824. 797.390 6 0 -1 1 194595. 871.556 6 0 1 -4 412552. 1553.88 1 0 1 -6 147726. 608.355 1 0 1 -6 124822. 719.285 8 0 -1 6 134711. 654.725 23 0 1 6 147124. 629.826 1 0 1 6 154523. 715.328 8 0 -1 6 137714. 714.837 8 0 1 -6 140546. 781.919 6 0 -1 6 161873. 890.007 6 0 -1 -6 152607. 744.422 23 0 -1 7 503564. 2159.09 6 0 1 -8 422696. 1764.34 6 0 -1 -9 34753.1 354.232 23 0 -1 9 33465.4 346.561 8 0 1 9 35917.9 347.123 8 0 -1 9 31770.2 284.796 23 0 1 -9 34009.9 344.686 6 0 -1 -10 105024. 698.924 23 0 -1 10 104807. 595.757 23 0 1 10 105397. 685.423 8 0 1 -11 192448. 999.911 6 0 -1 11 190147. 941.303 23 0 -1 -11 193581. 1072.65 23 0 1 -12 40440.4 396.388 6 0 -1 12 41971.5 465.544 8 0 -1 -12 40948.6 445.680 23 0 1 12 40372.5 444.442 8 0 1 13 12218.7 243.824 8 0 1 -13 11592.1 325.250 9 0 -1 -13 11672.4 243.320 23 0 -1 -13 11487.1 418.825 3 0 -1 13 11813.4 250.126 8 0 1 -13 10951.7 376.159 11 0 -1 -14 2189.59 208.695 3 0 -1 -14 2104.33 109.109 23 0 1 -14 1612.79 136.632 9 0 1 -14 1866.35 102.340 5 0 1 -14 1608.34 171.090 11 0 1 -14 2891.76 129.680 16 0 1 14 2991.16 129.574 8 0 -1 -15 222795. 1456.90 19 0 1 -15 286160. 1514.98 5 0 -1 -15 253540. 1469.46 16 0 -1 -15 280343. 1613.62 22 0 1 -15 260198. 1548.63 22 0 -1 -15 255389. 2365.57 3 0 1 -15 251275. 2119.74 11 0 1 -15 255940. 1492.22 16 0 1 15 249574. 1475.65 8 0 1 -15 272240. 1907.09 9 0 -1 -15 254917. 1453.41 5 0 -1 -15 280748. 2039.08 9 0 1 -16 6347.17 221.230 22 0 -1 -16 6097.20 217.068 22 0 -1 -16 6616.83 207.576 16 0 -1 -16 6964.10 221.466 19 0 1 -16 6887.73 212.595 16 0 -1 -16 6724.10 202.289 5 0 1 -16 6604.26 337.103 11 0 1 -16 7094.66 210.439 5 0 1 -16 7067.33 296.935 9 0 -1 -16 6167.61 350.413 11 0 -1 -16 7193.31 408.089 3 0 -1 -17 50642.2 623.307 19 0 -1 -17 52278.1 673.910 22 0 -1 -17 50366.2 609.356 16 0 1 -17 59525.5 893.606 9 0 -1 -17 52199.8 597.086 5 0 1 -17 50603.3 592.595 5 0 1 -17 46262.3 911.622 11 0 -1 -17 44466.3 1069.98 3 0 -1 -17 59888.3 952.017 9 0 -1 -17 49013.5 991.966 11 0 1 -17 52722.3 669.948 22 0 1 -17 48628.9 609.418 16 0 -1 -18 24864.3 441.379 16 0 1 -18 28029.1 627.180 9 0 -1 -18 23409.3 614.388 9 0 1 -18 23089.5 458.410 22 0 -1 -18 23008.1 408.019 5 0 -1 -18 22909.8 703.253 11 0 -1 -18 24839.2 475.722 22 0 1 -18 21578.7 649.694 11 0 -1 -18 27787.2 472.777 19 0 1 -18 23386.5 421.082 19 0 -1 -18 22552.0 777.190 3 0 1 -18 24047.7 430.659 16 0 1 -18 24303.8 421.641 5 0 -1 -19 106782. 1016.73 19 0 -1 -19 117317. 1421.29 9 0 1 -19 100020. 951.422 19 0 -1 -19 99899.3 927.337 5 0 1 -19 107221. 1489.28 11 0 1 -19 107954. 1055.66 22 0 -1 -19 109175. 1084.87 22 0 -1 -19 101994. 1528.78 11 0 -1 -19 96796.9 1722.19 3 0 -1 -19 104380. 984.386 16 0 1 -19 121707. 1377.04 9 0 1 -19 108684. 1010.65 16 0 1 -19 110527. 977.590 5 0 -1 -20 1627.54 155.133 22 0 1 -20 1596.00 182.883 9 0 -1 -20 1895.64 247.480 11 0 1 -20 1441.11 122.418 5 0 1 -20 1876.43 138.681 19 0 -1 -20 1592.12 128.539 5 0 1 -20 1531.61 133.042 16 0 1 -20 1923.95 244.425 11 0 -1 -20 1497.14 129.314 16 0 -1 -20 1831.38 147.122 19 0 -1 -20 1851.06 200.815 9 0 1 -20 1532.67 141.830 22 0 -1 -21 394879. 2233.83 5 0 -1 -21 418554. 2374.96 19 0 1 -21 387994. 2239.47 19 0 -1 -21 412470. 2931.96 9 0 1 -21 370945. 2354.56 22 0 -1 -21 386291. 2260.61 16 0 1 -21 391524. 2316.95 16 0 -1 -21 389306. 3208.12 11 0 1 -21 394297. 2233.53 5 0 1 -21 381453. 3095.86 11 0 1 -21 432141. 2861.06 9 0 -1 -22 56523.2 725.118 5 0 -1 -22 59429.0 1182.81 11 0 1 -22 61723.0 1003.95 9 0 1 -22 58302.3 728.991 5 0 -1 -22 59021.4 771.367 19 0 -1 -22 57050.0 647.658 21 0 -1 -22 57074.0 732.361 16 0 -1 -22 61687.6 1025.54 9 0 1 -22 56089.3 1095.28 11 0 1 -22 52459.7 765.372 22 0 1 -22 61564.3 756.782 19 0 1 -22 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74784.1 856.979 22 0 -5 -20 71972.4 836.337 21 0 -5 -20 77885.4 1466.80 3 0 5 -20 67486.7 1083.00 11 0 5 -20 70937.7 802.440 16 0 -5 -21 94.2299 112.134 9 0 5 -21 156.752 141.961 11 0 5 -21 75.0968 69.0828 16 0 5 -21 77.4779 74.3837 22 0 -5 -21 81.3261 57.2816 12 0 -5 -22 24710.1 652.364 9 0 -5 -22 26265.7 842.167 3 0 -5 -22 23018.8 446.871 21 0 5 -22 25296.5 456.294 16 0 -5 -22 23303.6 394.215 12 0 5 -22 24077.4 449.451 22 0 5 -22 24891.5 627.050 11 0 -5 -22 23063.8 728.122 11 0 -5 -23 31555.6 504.940 21 0 -5 -23 33179.4 716.166 9 0 5 -23 32097.0 494.091 22 0 5 -23 29901.1 664.288 11 0 5 -23 31654.4 494.156 16 0 -5 -23 29194.2 780.056 11 0 -5 -23 32989.3 919.045 3 0 -5 -23 28094.7 400.705 12 0 -5 -24 3161.59 219.507 9 0 -5 -24 3220.39 154.195 21 0 5 -24 2688.13 141.900 22 0 -5 -24 2778.21 256.263 11 0 5 -24 3166.40 216.992 11 0 5 -24 3469.49 160.576 16 0 -5 -25 93.2314 48.0497 21 0 5 -25 225.874 93.6282 11 0 -5 -25 199.414 83.2353 9 0 5 -25 134.631 60.6391 16 0 5 -25 73.4461 48.2722 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7585.19 237.198 6 2 -4 -6 6161.19 240.743 3 -2 -4 6 7314.55 226.009 12 -2 -4 7 318968. 1881.38 10 2 -4 -7 330617. 2065.43 1 -2 4 -7 301558. 1835.75 2 2 4 7 317751. 1825.13 6 -2 4 -7 321605. 1956.06 11 2 4 7 316033. 2077.66 1 -2 -4 7 335759. 1810.51 12 2 -4 -7 313885. 2039.99 3 -2 4 -8 97048.1 1007.40 11 -2 -4 8 89465.0 905.475 10 2 4 8 83484.7 984.512 1 2 -4 -8 86515.5 968.937 1 -2 4 -8 92088.8 875.791 2 -2 -4 8 99189.1 868.074 12 2 -4 -8 85111.9 1004.25 3 -2 4 -9 22808.6 490.676 11 2 -4 -9 19845.8 352.285 19 -2 -4 9 21518.6 442.081 10 -2 4 -9 25719.5 443.856 2 -2 -4 9 23894.3 417.751 12 2 -4 -9 22265.9 522.584 3 -2 4 -10 50812.6 751.031 11 2 4 10 50241.9 633.859 2 2 -4 -10 52140.3 838.582 3 2 -4 -11 15106.1 472.553 3 -2 -4 11 16741.0 390.857 10 -2 4 -11 15878.8 421.916 11 2 -4 -11 15668.3 331.277 19 2 -4 -12 32850.3 732.494 3 -2 4 -12 32365.3 622.108 11 2 -4 -12 32609.2 504.056 19 2 -4 -13 46975.7 927.074 3 -2 4 -13 49297.3 785.657 11 -2 -4 13 54870.0 743.460 10 -2 4 -13 52491.5 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236.951 21 -2 4 -22 5892.80 223.370 16 2 -4 -22 6441.33 344.726 9 2 -4 -22 6359.95 238.143 19 2 -4 -22 5831.66 181.604 5 2 -4 -23 27735.2 673.790 11 2 -4 -23 31929.2 501.627 21 -2 4 -23 29226.6 472.792 16 2 -4 -23 29275.8 666.936 9 -2 4 -23 24425.8 560.496 11 2 -4 -23 27420.6 370.570 5 2 -4 -23 28456.8 443.710 12 2 -4 -24 41441.5 762.127 11 2 -4 -24 43058.5 555.484 21 -2 4 -24 42363.5 540.158 16 2 -4 -24 42348.6 753.272 9 -2 4 -24 42739.4 672.488 11 2 -4 -24 40319.2 422.375 5 2 -4 -25 32007.9 598.449 11 2 -4 -25 30441.8 432.231 21 2 -4 -25 32011.0 609.953 9 -2 4 -25 32754.4 437.156 16 -2 4 -25 30427.4 503.134 11 2 -4 -26 18807.3 402.795 11 2 -4 -26 19655.5 312.169 21 -2 4 -26 18694.0 296.425 16 2 -4 -26 18736.9 420.237 9 -2 4 -26 19051.1 350.302 11 -2 4 -27 15138.5 229.469 16 2 -4 -27 15781.9 339.490 9 2 5 -26 40371.0 420.737 22 2 5 -26 39807.7 390.049 16 -2 -5 -25 2661.01 153.148 11 2 5 -25 2496.96 128.616 11 2 5 -25 2254.61 103.420 19 2 5 -25 2514.64 115.307 16 -2 -5 -24 9791.51 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326.954 2 -6 -6 -1 13517.1 273.190 13 -6 6 0 26808.6 338.081 17 -6 6 0 26591.4 457.191 4 -6 -6 1 15600.4 311.598 18 -6 6 -1 15760.9 349.136 4 -6 -6 1 15692.4 303.986 13 -6 -6 2 72955.5 681.353 18 -6 6 -2 69944.3 745.075 4 6 6 2 69914.6 742.553 2 -6 -6 2 72482.1 674.466 13 -6 -6 3 33329.2 437.199 18 -6 6 -3 32021.9 479.050 4 -6 -6 3 33293.8 446.784 13 -6 6 -4 46789.0 548.590 4 6 6 4 46214.6 547.859 2 -6 -6 4 48140.8 515.831 13 -6 -6 5 6019.71 171.605 18 -6 6 -5 5741.05 188.557 4 6 6 5 5568.13 192.823 2 -6 -6 6 4273.91 136.492 18 -6 6 -6 4055.54 148.599 4 6 6 6 3861.02 152.939 2 -6 -6 6 4186.17 154.129 13 -6 6 -7 9402.62 205.705 4 6 6 7 9276.87 216.882 2 -6 -6 8 17894.9 214.627 18 -6 -6 8 17911.0 304.246 10 -6 6 -8 16013.0 237.099 4 6 6 8 15489.6 250.228 2 -6 -6 8 15310.7 223.698 14 -6 -6 9 20985.0 320.657 10 -6 -6 9 17374.1 235.197 14 -6 -6 10 22625.6 318.736 10 -6 -6 10 19827.3 239.205 14 -6 -7 -5 8631.65 156.036 18 -6 7 5 8208.47 153.083 17 -6 7 4 12474.8 192.946 17 -6 7 4 12974.3 224.218 4 6 7 -4 12962.4 223.262 2 -6 -7 -3 6838.89 157.365 18 -6 7 3 5700.23 129.432 17 -6 7 3 6831.15 171.434 4 6 7 -3 6911.67 172.688 2 -6 -7 -3 5253.09 115.804 13 -6 -7 -2 9359.47 189.945 18 -6 7 2 7517.24 144.130 17 -6 7 2 9320.81 208.312 4 6 7 -2 9422.27 208.763 2 -6 -7 -2 7986.52 154.478 13 6 7 -1 11959.4 240.926 2 -6 -7 -1 11394.0 194.835 13 -6 7 0 43139.7 468.577 4 6 7 0 43400.5 473.185 2 -6 -7 0 43699.5 407.786 13 -6 -7 1 13092.1 222.037 18 -6 -7 1 13074.6 219.890 13 -6 -7 2 6952.69 158.076 18 6 7 2 7004.94 180.592 2 -6 -7 3 6434.94 143.255 18 -6 7 -3 6331.38 164.216 4 6 7 3 6980.52 175.484 2 -6 -7 3 7035.44 160.980 13 -6 -7 4 11283.0 176.610 18 -6 7 -4 10939.8 201.282 4 -6 -7 5 8000.74 130.681 18 -7 0 0 168.278 57.8399 20 -7 0 0 68.6668 84.8548 18 -7 0 0 75.2720 67.4199 13 -7 0 1 6752.44 196.261 20 -7 0 1 7407.83 245.076 18 -7 0 -1 7509.68 240.308 18 -7 0 -1 6770.05 202.835 13 -7 0 1 7078.66 219.029 13 -7 0 2 135909. 964.737 20 -7 0 2 142100. 1048.69 13 -7 0 3 436.841 82.7771 20 -7 0 -3 449.637 97.0436 18 -7 0 3 415.624 90.9741 13 -7 0 4 113394. 873.530 20 -7 0 4 113576. 956.065 18 -7 0 4 114970. 926.335 13 -7 0 5 925.178 106.723 20 -7 0 5 1119.79 119.229 18 -7 0 -5 1003.38 101.933 18 -7 0 5 979.580 83.3914 15 -7 0 5 1000.91 113.954 13 -7 0 6 106576. 841.730 20 -7 0 6 107390. 883.431 13 -7 0 7 16406.9 312.289 20 -7 0 7 16877.5 327.663 13 -7 0 8 42139.8 491.849 20 -7 0 8 39180.1 441.803 15 -7 0 9 6052.43 185.721 20 -7 0 9 6119.90 169.360 15 -7 0 10 87976.4 703.232 20 -7 0 10 91926.0 681.568 15 -7 0 11 11989.5 218.660 15 -7 0 11 8020.66 152.924 14 -7 0 12 13632.3 231.423 20 -7 0 12 12770.2 214.747 15 -7 0 13 21729.3 259.099 20 -7 0 13 19611.9 244.907 15 7 1 -12 11416.4 194.419 5 -7 1 12 11872.6 204.686 15 7 1 -11 108367. 714.000 5 -7 1 11 106770. 712.009 15 7 1 -10 1152.97 83.8975 5 -7 1 10 1176.72 83.0184 15 7 1 -9 827.897 80.6680 5 -7 1 9 849.019 87.0968 20 -7 1 9 904.791 76.7402 15 7 1 -8 24948.0 364.193 5 -7 1 8 25594.0 341.908 15 7 1 -7 20586.3 342.546 5 -7 1 7 21429.3 310.870 15 7 1 -6 5718.98 187.611 5 -7 1 6 5754.42 189.764 20 -7 -1 -6 5575.47 173.880 18 -7 1 6 5513.73 157.283 15 -7 1 5 41444.4 498.558 20 -7 -1 -5 40901.7 484.318 18 -7 1 4 82781.5 725.941 20 -7 -1 -4 83129.0 740.499 18 -7 1 3 18519.0 326.736 20 -7 -1 -3 17887.6 341.764 18 -7 1 2 31443.3 420.976 20 -7 -1 -2 30744.3 404.271 13 -7 1 1 57165.1 564.770 20 -7 -1 -1 57490.9 586.874 13 -7 1 0 40967.1 452.495 20 -7 -1 0 39363.6 439.494 20 -7 -1 0 45875.3 576.477 18 -7 1 0 37241.6 558.833 4 -7 -1 0 44506.7 521.380 13 -7 -1 1 65425.5 611.704 20 -7 1 -1 65270.1 745.773 4 -7 -1 2 26564.4 385.295 20 -7 1 -2 26499.6 461.480 4 -7 -1 3 19470.9 332.903 20 -7 -1 3 18582.8 352.243 13 -7 -1 4 85245.2 734.418 20 -7 -1 4 85200.0 800.366 18 -7 -1 4 83451.6 776.741 13 7 -1 -5 41510.1 527.246 5 -7 -1 5 43528.7 509.681 20 -7 -1 5 43027.3 541.555 18 -7 -1 5 42661.0 535.695 13 7 -1 -6 6364.52 201.070 5 -7 -1 6 6816.05 202.942 20 -7 -1 6 6751.34 211.585 18 -7 -1 6 6752.97 213.260 13 7 -1 -7 25369.6 377.953 5 -7 -1 7 27047.7 392.666 20 -7 -1 7 26918.1 393.807 18 -7 -1 7 25869.5 405.928 13 7 -1 -8 30156.9 403.530 5 -7 -1 8 31485.0 419.780 20 7 -1 -9 765.728 78.9752 5 -7 -1 9 833.637 86.9236 20 -7 -1 9 706.917 86.2918 13 7 -1 -10 1748.47 98.5747 5 -7 -1 10 1828.42 107.650 20 -7 -1 10 1710.50 99.3872 15 -7 -1 10 1963.98 109.811 13 7 -1 -11 108181. 724.016 5 -7 -1 11 110728. 728.284 15 7 -1 -12 12382.6 199.615 5 -7 -1 12 12928.3 217.723 20 -7 -1 12 12298.7 205.261 15 7 2 -11 18302.7 231.723 5 -7 2 11 24231.4 284.634 15 7 2 -10 8425.63 169.188 5 -7 2 10 9244.70 184.156 15 -7 2 9 68924.7 586.733 20 -7 2 9 63626.7 519.108 15 7 2 -8 75574.3 622.158 5 -7 2 8 81799.3 611.152 15 7 2 -7 11414.1 229.421 5 -7 -2 -7 11843.6 220.448 18 -7 2 7 11177.9 213.067 15 7 2 -6 18763.3 304.841 5 -7 -2 -6 19779.8 306.590 18 -7 2 5 21483.2 339.211 20 -7 -2 -5 20881.3 330.560 18 -7 2 5 20581.3 369.608 4 -7 2 4 16192.7 294.807 20 7 2 -4 14563.2 290.670 5 -7 -2 -4 16134.5 304.304 18 -7 2 4 14513.3 240.732 17 -7 2 4 14781.3 320.130 4 -7 2 3 38371.2 454.460 20 -7 -2 -3 39395.2 490.105 18 -7 2 2 11960.1 247.627 20 -7 -2 -2 12298.6 281.129 18 -7 -2 -2 11654.8 238.755 13 -7 2 1 2078.63 110.150 20 -7 -2 -1 2082.00 132.459 18 -7 -2 -1 1863.97 111.455 13 -7 2 0 11009.0 223.717 20 -7 -2 0 11531.2 256.681 13 -7 -2 1 1100.10 83.8654 20 -7 -2 1 1025.76 110.409 18 -7 2 -1 1030.13 106.896 4 -7 -2 1 1303.68 104.053 13 -7 -2 2 15876.7 281.873 20 -7 2 -2 15716.1 343.049 4 7 -2 -3 42645.8 524.079 5 -7 -2 3 43712.6 538.692 18 -7 -2 3 43958.0 527.174 13 7 -2 -4 11058.4 252.915 5 -7 -2 4 11658.3 274.842 18 -7 -2 4 11555.1 269.636 13 7 -2 -5 17127.0 299.967 5 -7 -2 5 17626.1 324.116 18 -7 -2 5 17539.8 328.344 13 -7 -2 6 24906.2 373.396 18 -7 -2 6 25446.6 392.350 13 -7 -2 7 10441.6 235.151 20 -7 -2 7 10424.2 230.925 18 -7 -2 8 89625.7 706.166 20 -7 -2 8 86536.3 670.176 18 -7 -2 9 65994.4 579.696 20 -7 -2 9 66513.8 590.331 13 -7 -2 10 10806.3 215.392 20 -7 -2 10 11150.1 217.377 13 7 -2 -11 21729.1 246.330 5 -7 -2 11 27219.0 315.847 13 -7 3 10 18399.8 236.164 17 -7 3 10 15606.6 208.846 15 -7 3 9 57380.2 492.834 20 -7 3 9 54520.0 444.774 17 -7 3 8 20221.8 291.961 20 -7 3 8 20154.4 263.968 17 -7 3 7 2292.51 113.529 20 -7 3 7 2201.44 96.9506 17 -7 -3 -6 17870.3 265.664 18 -7 3 6 18027.9 256.620 17 -7 3 6 17995.8 300.943 4 -7 3 5 11201.2 230.868 20 -7 -3 -5 11124.9 223.828 18 -7 3 5 10468.9 193.596 17 -7 3 5 10592.3 243.952 4 -7 3 4 18532.2 296.763 20 -7 -3 -4 19311.7 311.564 18 -7 3 4 17030.9 241.942 17 -7 3 4 17666.4 330.691 4 -7 3 3 7523.42 189.053 20 -7 -3 -3 7793.63 208.257 18 -7 3 2 31891.0 377.733 20 -7 -3 -2 31381.8 361.979 13 -7 3 1 21400.3 298.823 20 -7 -3 -1 21033.2 310.520 13 -7 -3 0 7877.29 221.145 18 -7 -3 0 7397.81 195.368 13 7 -3 -1 17336.3 273.985 5 -7 3 -1 18530.6 359.748 4 -7 3 -2 30180.2 451.800 4 -7 -3 2 33417.2 426.447 13 -7 -3 3 7291.20 207.918 18 -7 -3 3 7012.50 200.124 13 7 -3 -4 12516.2 210.882 5 -7 -3 4 15529.3 290.225 18 -7 3 -4 13393.2 285.297 4 -7 -3 4 15452.6 291.545 13 -7 -3 5 11612.2 242.415 18 -7 -3 5 11925.6 251.467 13 -7 -3 6 19488.1 296.648 18 -7 3 -6 18443.5 303.850 4 7 -3 -7 1779.20 71.7899 5 -7 -3 7 2674.11 106.673 18 7 -3 -8 11118.5 157.141 5 -7 -3 8 18333.5 241.624 18 -7 -3 9 49995.5 454.973 20 -7 -3 9 54453.9 476.145 13 -7 -3 10 20055.8 262.057 20 -7 -3 10 20487.3 260.321 13 -7 4 7 15124.5 201.566 17 -7 -4 -6 13964.4 196.935 18 -7 4 6 14679.3 199.954 17 7 4 -6 12357.7 215.375 2 -7 4 6 12918.5 216.174 4 -7 -4 -5 17053.5 239.894 18 -7 4 5 14600.4 201.429 17 7 4 -5 16131.5 269.704 2 -7 4 5 15349.8 255.898 4 -7 -4 -4 31218.3 353.796 18 7 4 -4 29649.2 390.696 2 -7 -4 -3 56834.8 513.927 18 -7 4 3 54146.4 546.901 4 -7 4 2 7176.20 199.490 4 -7 -4 -2 6885.87 144.080 13 -7 -4 -1 14311.1 261.474 18 -7 -4 -1 11689.1 204.264 13 -7 -4 0 25871.3 356.257 18 -7 -4 0 23542.5 305.920 13 -7 4 -1 15001.8 290.498 4 -7 -4 1 15150.4 251.635 13 -7 -4 2 6892.62 183.970 18 -7 -4 2 6932.40 175.392 13 -7 -4 3 51614.5 490.344 18 -7 -4 3 50268.0 483.325 13 -7 -4 4 31978.3 364.480 18 7 4 4 28766.9 388.378 2 -7 4 -4 27921.7 367.536 4 -7 -4 4 32156.1 375.139 13 -7 -4 5 16190.2 241.367 18 7 4 5 13054.9 245.866 2 -7 4 -5 12758.0 231.519 4 -7 -4 5 16295.1 257.902 13 -7 -4 6 13150.5 199.066 18 7 4 6 10201.8 199.884 2 -7 4 -6 11510.5 199.151 4 -7 -4 6 14138.7 230.375 13 -7 -4 7 10669.5 154.625 18 0 0 0 0.00 0.00 0 TITL CH6_131p in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 1.54184 6.176461 9.226752 24.658546 90.0000 90.0000 90.0000 ZERR 20.00 0.000056 0.000079 0.000195 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 S UNIT 20.00 20.00 20.00 20.00 20.00 TREF HKLF 4 END ; _shelx_hkl_checksum 52445 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 C1 C 0.3549(4) 0.0751(2) 0.72114(8) 0.0211(4) Uani 1 1 d . . H1A H 0.3953 0.0204 0.6886 0.032 Uiso 1 1 calc R U H1B H 0.2560 0.0170 0.7433 0.032 Uiso 1 1 calc R U H1C H 0.4853 0.0977 0.7422 0.032 Uiso 1 1 calc R U C2 C 0.2430(3) 0.21599(19) 0.70447(7) 0.0168(4) Uani 1 1 d . . C3 C 0.1833(3) 0.3045(2) 0.75448(8) 0.0240(4) Uani 1 1 d . . H3A H 0.3151 0.3296 0.7745 0.036 Uiso 1 1 calc R U H3B H 0.0874 0.2473 0.7778 0.036 Uiso 1 1 calc R U H3C H 0.1090 0.3934 0.7433 0.036 Uiso 1 1 calc R U C4 C 0.0494(3) 0.1857(2) 0.66800(9) 0.0272(4) Uani 1 1 d . . H4A H -0.0165 0.2775 0.6568 0.041 Uiso 1 1 calc R U H4B H -0.0573 0.1277 0.6879 0.041 Uiso 1 1 calc R U H4C H 0.0974 0.1322 0.6358 0.041 Uiso 1 1 calc R U C5 C 0.4629(3) 0.58362(18) 0.63413(7) 0.0137(3) Uani 1 1 d . . H5 H 0.5941 0.5867 0.6579 0.016 Uiso 1 1 calc R U C6 C 0.3576(3) 0.7309(2) 0.63684(8) 0.0183(4) Uani 1 1 d . . H6 H 0.2559 0.7591 0.6638 0.022 Uiso 1 1 calc R U C7 C 0.4247(3) 0.8160(2) 0.59696(8) 0.0205(4) Uani 1 1 d . . H7 H 0.3820 0.9143 0.5928 0.025 Uiso 1 1 calc R U C8 C 0.5756(3) 0.73903(19) 0.55913(8) 0.0186(4) Uani 1 1 d . . H8A H 0.7273 0.7696 0.5652 0.022 Uiso 1 1 calc R U H8B H 0.5365 0.7578 0.5208 0.022 Uiso 1 1 calc R U C9 C 0.5436(3) 0.57575(18) 0.57385(7) 0.0131(3) Uani 1 1 d . . C10 C 0.7646(3) 0.50187(19) 0.57167(7) 0.0162(3) Uani 1 1 d . . C11 C 0.6596(3) 0.3658(2) 0.49062(8) 0.0199(4) Uani 1 1 d . . H11A H 0.5992 0.2739 0.5048 0.024 Uiso 1 1 calc R U H11B H 0.7311 0.3445 0.4556 0.024 Uiso 1 1 calc R U C12 C 0.4774(3) 0.4718(2) 0.48128(7) 0.0182(4) Uani 1 1 d . . H12A H 0.3678 0.4286 0.4568 0.022 Uiso 1 1 calc R U H12B H 0.5339 0.5611 0.4641 0.022 Uiso 1 1 calc R U C13 C 0.3752(3) 0.5078(2) 0.53589(7) 0.0145(3) Uani 1 1 d . . H13A H 0.3168 0.4183 0.5525 0.017 Uiso 1 1 calc R U H13B H 0.2537 0.5763 0.5305 0.017 Uiso 1 1 calc R U N1 N 0.3246(2) 0.46642(16) 0.65397(6) 0.0141(3) Uani 1 1 d . . O1 O 0.4951(2) 0.22699(14) 0.61650(5) 0.0194(3) Uani 1 1 d . . O2 O 0.8992(2) 0.52285(16) 0.60642(6) 0.0225(3) Uani 1 1 d . . O3 O 0.8210(2) 0.42142(15) 0.52893(5) 0.0204(3) Uani 1 1 d . . S1 S 0.45717(6) 0.31332(4) 0.66691(2) 0.01336(12) Uani 1 1 d . . H1 H 0.194(4) 0.455(3) 0.6362(10) 0.021(6) Uiso 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0271(10) 0.0166(8) 0.0197(9) 0.0036(7) -0.0010(8) 0.0004(8) C2 0.0155(9) 0.0169(8) 0.0181(8) 0.0017(7) 0.0010(7) -0.0020(7) C3 0.0260(10) 0.0220(9) 0.0240(9) 0.0011(8) 0.0108(8) 0.0007(8) C4 0.0199(9) 0.0302(10) 0.0315(10) 0.0105(8) -0.0058(9) -0.0085(8) C5 0.0122(7) 0.0147(8) 0.0141(7) 0.0003(6) -0.0004(7) -0.0014(7) C6 0.0179(9) 0.0161(9) 0.0209(9) -0.0033(7) 0.0008(7) 0.0023(7) C7 0.0222(9) 0.0139(8) 0.0256(9) 0.0007(7) -0.0011(7) 0.0011(8) C8 0.0179(9) 0.0148(8) 0.0229(9) 0.0048(7) 0.0017(7) -0.0022(7) C9 0.0112(7) 0.0133(7) 0.0147(7) 0.0012(6) 0.0005(7) 0.0005(7) C10 0.0130(8) 0.0167(8) 0.0188(8) 0.0030(7) 0.0025(7) -0.0004(7) C11 0.0189(9) 0.0210(9) 0.0198(9) -0.0030(7) 0.0026(8) 0.0008(7) C12 0.0169(8) 0.0226(8) 0.0150(8) 0.0006(7) 0.0007(7) 0.0005(7) C13 0.0117(7) 0.0181(8) 0.0137(7) 0.0013(7) -0.0016(6) 0.0011(7) N1 0.0108(7) 0.0154(7) 0.0161(7) 0.0020(5) -0.0006(6) 0.0001(6) O1 0.0219(7) 0.0206(6) 0.0158(6) -0.0013(5) 0.0019(5) 0.0051(5) O2 0.0126(6) 0.0303(7) 0.0246(7) -0.0006(6) -0.0029(5) 0.0009(5) O3 0.0135(6) 0.0240(7) 0.0238(7) -0.0032(5) 0.0015(5) 0.0031(5) S1 0.01188(19) 0.01433(19) 0.01387(19) 0.00125(14) -0.00010(15) 0.00105(15) 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' S S 0.3331 0.5567 '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 C2 C1 H1A 109.5 C2 C1 H1B 109.5 H1A C1 H1B 109.5 C2 C1 H1C 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 C4 C2 C3 112.74(17) C4 C2 C1 110.98(16) C3 C2 C1 110.31(15) C4 C2 S1 110.83(13) C3 C2 S1 108.57(13) C1 C2 S1 102.95(13) C2 C3 H3A 109.5 C2 C3 H3B 109.5 H3A C3 H3B 109.5 C2 C3 H3C 109.5 H3A C3 H3C 109.5 H3B C3 H3C 109.5 C2 C4 H4A 109.5 C2 C4 H4B 109.5 H4A C4 H4B 109.5 C2 C4 H4C 109.5 H4A C4 H4C 109.5 H4B C4 H4C 109.5 N1 C5 C6 113.55(15) N1 C5 C9 117.92(14) C6 C5 C9 102.76(13) N1 C5 H5 107.4 C6 C5 H5 107.4 C9 C5 H5 107.4 C7 C6 C5 111.47(16) C7 C6 H6 124.3 C5 C6 H6 124.3 C6 C7 C8 112.10(16) C6 C7 H7 124.0 C8 C7 H7 124.0 C7 C8 C9 103.50(14) C7 C8 H8A 111.1 C9 C8 H8A 111.1 C7 C8 H8B 111.1 C9 C8 H8B 111.1 H8A C8 H8B 109.0 C10 C9 C13 113.73(14) C10 C9 C8 108.02(14) C13 C9 C8 109.76(14) C10 C9 C5 109.77(14) C13 C9 C5 112.43(15) C8 C9 C5 102.46(13) O2 C10 O3 117.96(16) O2 C10 C9 121.21(16) O3 C10 C9 120.61(15) O3 C11 C12 112.24(15) O3 C11 H11A 109.2 C12 C11 H11A 109.2 O3 C11 H11B 109.2 C12 C11 H11B 109.2 H11A C11 H11B 107.9 C11 C12 C13 108.39(14) C11 C12 H12A 110.0 C13 C12 H12A 110.0 C11 C12 H12B 110.0 C13 C12 H12B 110.0 H12A C12 H12B 108.4 C12 C13 C9 110.35(15) C12 C13 H13A 109.6 C9 C13 H13A 109.6 C12 C13 H13B 109.6 C9 C13 H13B 109.6 H13A C13 H13B 108.1 C5 N1 S1 113.87(12) C5 N1 H1 115.9(15) S1 N1 H1 114.9(15) C10 O3 C11 121.73(14) O1 S1 N1 111.72(7) O1 S1 C2 105.66(8) N1 S1 C2 98.99(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.529(3) C1 H1A 0.9800 C1 H1B 0.9800 C1 H1C 0.9800 C2 C4 1.522(3) C2 C3 1.524(3) C2 S1 1.8479(19) C3 H3A 0.9800 C3 H3B 0.9800 C3 H3C 0.9800 C4 H4A 0.9800 C4 H4B 0.9800 C4 H4C 0.9800 C5 N1 1.462(2) C5 C6 1.508(2) C5 C9 1.569(2) C5 H5 1.0000 C6 C7 1.325(3) C6 H6 0.9500 C7 C8 1.498(3) C7 H7 0.9500 C8 C9 1.562(2) C8 H8A 0.9900 C8 H8B 0.9900 C9 C10 1.526(2) C9 C13 1.533(2) C10 O2 1.210(2) C10 O3 1.335(2) C11 O3 1.466(2) C11 C12 1.508(3) C11 H11A 0.9900 C11 H11B 0.9900 C12 C13 1.524(2) C12 H12A 0.9900 C12 H12B 0.9900 C13 H13A 0.9900 C13 H13B 0.9900 N1 S1 1.6637(15) N1 H1 0.92(3) O1 S1 1.4946(12)