#------------------------------------------------------------------------------ #$Date: 2018-11-17 05:49:15 +0200 (Sat, 17 Nov 2018) $ #$Revision: 212036 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/27/2242746.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2242746 loop_ _publ_author_name 'Nagaraju, S.' 'Sridhar, M. A.' 'Pradeepa Kumara, C.S.' 'Sadashiva, M. P.' 'Lakshminarayana, B. N.' 'Lokanath, N. K.' _publ_section_title ; Synthesis, molecular structure and Hirshfeld surface analysis of (4-methoxyphenyl)[2-(methylsulfanyl)thiophen-3-yl]methanone ; _journal_coeditor_code VM2213 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 1800 _journal_page_last 1803 _journal_paper_doi 10.1107/S2056989018016043 _journal_volume 74 _journal_year 2018 _chemical_formula_iupac 'C13 H12 O2 S2' _chemical_formula_moiety 'C13 H12 O2 S2' _chemical_formula_sum 'C13 H12 O2 S2' _chemical_formula_weight 264.35 _chemical_name_systematic ; (4-Methoxyphenyl)[2-(methylsulfanyl)thiophen-3-yl]methanone ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 97.260(11) _cell_angle_beta 109.65(2) _cell_angle_gamma 93.79(2) _cell_formula_units_Z 2 _cell_length_a 7.806(4) _cell_length_b 8.263(3) _cell_length_c 10.414(6) _cell_measurement_reflns_used 2924 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.027 _cell_measurement_theta_min 3.525 _cell_volume 623.3(5) _computing_cell_refinement ; SAINT (Bruker, 2006) ; _computing_data_collection ; APEX2 (Bruker, 2006) ; _computing_data_reduction ; SAINT (Bruker, 2006) ; _computing_molecular_graphics ; PLATON (Spek, 2009) and Mercury (Macrae et al., 2008) ; _computing_publication_material ; PLATON (Spek, 2009) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 0.894 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method 'SAINT (Bruker, 2006) [not correct; type of scans needed]' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1093 _diffrn_reflns_av_unetI/netI 0.0622 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 2924 _diffrn_reflns_theta_full 25.027 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 3.525 _diffrn_source graphite _exptl_absorpt_coefficient_mu 0.413 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 276 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.369 _refine_diff_density_min -0.331 _refine_ls_extinction_coef 0.060(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2018 (Sheldrick, 2015) ; _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 157 _refine_ls_number_reflns 2165 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0464 _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^)+(0.0720P)^2^+0.1135P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1234 _refine_ls_wR_factor_ref 0.1284 _reflns_number_gt 1899 _reflns_number_total 2165 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file vm2213sup1.cif _cod_data_source_block I _cod_database_code 2242746 _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_hkl_file ; 0 0 -3101312.0 1296.62 1 0.53446-0.60993-0.81854 0.79242-0.21055 0.00629 0 0 -5628413.8 3944.19 1 0.51180-0.63834-0.81087 0.76764-0.28379-0.05693 0 0 -6219686.3 2999.53 1 0.49946-0.65131-0.80537 0.75349-0.31922-0.08964 0 0 -7107074.6 1631.26 1 0.48629-0.66344-0.79865 0.73813-0.35450-0.12250 0 0 -8 647.74 252.36 1 0.47225-0.67471-0.79067 0.72150-0.38962-0.15553 0 0 -9 4893.76 892.99 1 0.45733-0.68509-0.78139 0.70358-0.42457-0.18872 0 0 -1051854.42 1545.28 1 0.44148-0.69455-0.77076 0.68430-0.45936-0.22208 0 0 -11 6390.27 1126.44 1 0.42466-0.70304-0.75872 0.66361-0.49396-0.25562 0 0 -12 656.46 532.64 1 0.40682-0.71051-0.74518 0.64143-0.52837-0.28935 0 1 -1220143.18 1186.75 1 0.37643-0.67041-0.72038 0.70351-0.58253-0.23580 0 1 -1155355.19 2022.44 1 0.39219-0.66030-0.73356 0.72535-0.55503-0.19455 0 1 -1016642.81 872.86 1 0.40636-0.64916-0.74482 0.74526-0.52924-0.15220 0 1 -9 -87.95 359.27 1 0.41903-0.63653-0.75453 0.76361-0.50506-0.10824 0 1 -860433.76 2059.18 1 0.43003-0.62222-0.76264 0.78038-0.48314-0.06200 0 1 -7133105.5 1943.45 1 0.43903-0.60591-0.76905 0.79543-0.46454-0.01247 0 1 -6151442.4 2155.63 1 0.44542-0.58699-0.77347 0.80849-0.45092 0.04205 0 1 -5174658.0 2280.51 1 0.44804-0.56430-0.77525 0.81892-0.44523 0.10451 0 1 -428288.58 856.19 1 0.44441-0.53536-0.77278 0.82510-0.45309 0.18051 0 1 -2433657.6 4016.19 1 0.38097-0.42131-0.72435 0.79395-0.57460 0.43831 0 -1 -2498500.7 4591.56 1 0.60070-0.66124-0.77319 0.66912 0.20326-0.33915 0 -1 -3170006.8 1944.73 1 0.58805-0.67377-0.80738 0.69447 0.04819-0.25245 0 -1 -454798.83 1448.30 1 0.57192-0.68280-0.81857 0.69696-0.05320-0.21914 0 -1 -5401669.1 4288.96 1 0.55557-0.69160-0.82125 0.69092-0.12995-0.21047 0 -1 -6 9004.32 492.27 1 0.53925-0.70044-0.81959 0.68056-0.19356-0.21495 0 -1 -752463.40 1183.16 1 0.52280-0.70916-0.81516 0.66742-0.24936-0.22723 0 -1 -859966.19 1992.50 1 0.50546-0.71819-0.80815 0.65208-0.30230-0.24285 0 -1 -9137353.5 2758.71 1 0.48815-0.72618-0.79965 0.63493-0.34966-0.26363 0 -1 -10 -43.40 363.37 1 0.47021-0.73356-0.78945 0.61609-0.39453-0.28691 0 -1 -11 1448.85 445.63 1 0.45154-0.74019-0.77760 0.59559-0.43754-0.31205 0 -1 -12 378.48 433.26 1 0.43202-0.74598-0.76408 0.57343-0.47909-0.33864 0 2 -1240409.36 1794.89 1 0.34105-0.62482-0.68955 0.75986-0.63890-0.17943 0 2 -11 3614.10 644.26 1 0.35375-0.61216-0.70085 0.77984-0.61940-0.13074 0 2 -1012780.10 875.30 1 0.36448-0.59755-0.71020 0.79786-0.60229-0.07965 0 2 -9 69.15 567.98 1 0.37293-0.58065-0.71742 0.81375-0.58840-0.02535 0 2 -8471338.3 4367.34 1 0.37858-0.56095-0.72218 0.82717-0.57890 0.03334 0 2 -7121363.8 1960.64 1 0.38090-0.53751-0.72429 0.83757-0.57471 0.09770 0 2 -6 9918.85 615.18 1 0.37729-0.50896-0.72110 0.84344-0.58107 0.17190 0 2 -532956.50 1025.03 1 0.36604-0.47236-0.71154 0.84255-0.59975 0.25878 0 2 -4138001.6 1804.26 1 0.34123-0.42220-0.68971 0.82939-0.63863 0.36585 0 2 -3463746.6 4488.15 1 0.29099-0.34661-0.64264 0.79099-0.70874 0.50416 0 2 -2136602.7 1547.81 1 0.18751-0.21785-0.53822 0.69504-0.82167 0.68516 0 -2 2134925.4 1352.92 1 0.48730-0.45658-0.59768 0.44105-0.63663 0.77265 0 2 -1 4225.33 202.65 1-0.01742 0.01276-0.29737 0.46282-0.95460 0.88635 0 -2 0121794.6 1322.61 1 0.31380-0.33433-0.12513-0.04850 0.94120-0.94120 0 2 0127736.1 1370.27 1-0.31514 0.33591 0.12587 0.04818-0.94065 0.94065 0 -2 -1142279.7 1516.55 1 0.52088-0.56669-0.49846 0.31640 0.69297-0.76075 0 -2 -2621677.5 2365.11 1 0.59019-0.66096-0.68252 0.49172 0.43107-0.56686 0 -2 -3 6587.53 344.44 1 0.60148-0.69737-0.76180 0.56229 0.24055-0.44440 0 -2 -425333.13 817.37 1 0.59429-0.71536-0.79756 0.58941 0.10349-0.37528 0 -2 -595231.21 1532.56 1 0.58094-0.72722-0.81394 0.59683-0.00140-0.33902 0 -2 -6125743.4 1639.06 1 0.56529-0.73673-0.82035 0.59453-0.08640-0.32211 0 -2 -7141263.8 3977.61 1 0.54847-0.74507-0.82094 0.58641-0.15882-0.31777 0 -2 -888094.81 2834.17 1 0.53088-0.75264-0.81762 0.57439-0.22281-0.32187 0 -2 -915421.20 1650.91 1 0.51202-0.76033-0.81096 0.55935-0.28313-0.33017 0 -2 -10 -225.38 359.79 1 0.49296-0.76658-0.80215 0.54190-0.33693-0.34451 0 -2 -1130407.15 1395.59 1 0.47314-0.77206-0.79119 0.52229-0.38747-0.36211 0 -2 -1227591.39 1789.20 1 0.45245-0.77668-0.77820 0.50065-0.43551-0.38222 0 3 -12 172.64 386.08 1 0.30069-0.57424-0.65200 0.80949-0.69604-0.12229 0 3 -11 1330.20 502.97 1 0.30999-0.55819-0.66086 0.82702-0.68349-0.06664 0 3 -1014463.81 1007.52 1 0.31663-0.53949-0.66711 0.84195-0.67430-0.00764 0 3 -959511.16 1738.96 1 0.32006-0.51756-0.67031 0.85382-0.66950 0.05574 0 3 -844535.64 2141.09 1 0.31937-0.49153-0.66967 0.86185-0.67046 0.12490 0 3 -7237454.5 2888.64 1 0.31316-0.45997-0.66385 0.86470-0.67912 0.20176 0 3 -6107758.3 1626.38 1 0.29911-0.42057-0.65049 0.86001-0.69812 0.28895 0 3 -5260680.9 3198.17 1 0.27331-0.36942-0.62527 0.84345-0.73098 0.39000 0 3 -412193.97 626.01 1 0.22900-0.29975-0.58006 0.80692-0.78171 0.50893 0 -3 420007.20 547.82 1-0.00636 0.07765-0.87406 0.64786-0.48575 0.75778 0 3 -3682845.6 3427.46 1 0.15350-0.19903-0.50072 0.73595-0.85188 0.64711 0 3 -2 7444.93 345.54 1 0.03229-0.05243-0.35814 0.60223-0.93310 0.79659 0 -3 2 6343.30 302.13 1 0.60649-0.58636-0.46953 0.22588-0.64163 0.77791 0 3 -1200068.3 2156.11 1-0.14601 0.15179-0.12622 0.37878-0.98119 0.91295 0 -3 0273975.9 2831.15 1 0.34343-0.37422-0.17265-0.08780 0.92317-0.92317 0 3 0285931.7 2876.94 1-0.34485 0.37600 0.17354 0.08753-0.92247 0.92247 0 -3 -1493863.3 4788.43 1 0.49319-0.54924-0.44068 0.17180 0.75003-0.81781 0 -3 -2103123.8 1431.12 1 0.56961-0.65054-0.61598 0.33833 0.54415-0.67994 0 -3 -319131.17 651.57 1 0.59736-0.70344-0.71511 0.42878 0.36300-0.56684 0 -3 -440304.41 1161.95 1 0.60109-0.73235-0.76919 0.47423 0.21684-0.48863 0 -3 -5260223.5 2422.32 1 0.59382-0.75025-0.79853 0.49494 0.09861-0.43835 0 -3 -6110640.9 1633.43 1 0.58116-0.76284-0.81378 0.50118 0.00000-0.40851 0 -3 -713674.88 1651.44 1 0.56578-0.77262-0.82025 0.49894-0.08404-0.39256 0 -3 -8 4111.75 544.98 1 0.54868-0.78068-0.82095 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1 0.03385-0.06917-0.36006 0.68256-0.93231 0.72754 0 -4 3171563.0 2008.93 1 0.51072-0.47480-0.57550 0.25365-0.63871 0.84274 0 4 -246209.84 1273.79 1-0.08419 0.07486-0.21038 0.54129-0.97398 0.83749 0 -4 241700.56 1262.12 1 0.63139-0.62162-0.43851 0.10792-0.63956 0.77584 0 4 -1367620.7 3813.58 1-0.22772 0.24360-0.00758 0.34710-0.97369 0.90563 0 -4 0345263.8 3854.45 1 0.37215-0.41321-0.22006-0.12721 0.90170-0.90170 0 -4 -1147994.0 1894.11 1 0.48604-0.55232-0.42640 0.07070 0.76285-0.83062 0 -4 -2171423.2 2285.73 1 0.55600-0.64709-0.57976 0.21525 0.59559-0.73138 0 -4 -316138.61 659.00 1 0.58982-0.70613-0.68106 0.30801 0.43389-0.63757 0 -4 -4182098.9 1985.89 1 0.60103-0.74247-0.74411 0.36234 0.29163-0.56341 0 -4 -5 7271.83 1123.96 1 0.59926-0.76588-0.78228 0.39188 0.17002-0.50975 0 -4 -6409107.2 4288.95 1 0.59012-0.78204-0.80470 0.40530 0.06491-0.47342 0 -4 -7 2049.26 434.68 1 0.57684-0.79392-0.81643 0.40833-0.02611-0.45049 0 -4 -8 7510.24 750.07 1 0.56086-0.80310-0.82097 0.40417-0.10689-0.43779 0 -4 -9 226.83 214.21 1 0.54299-0.81039-0.82025 0.39474-0.17982-0.43294 0 -4 -1011675.36 867.81 1 0.52364-0.81619-0.81543 0.38121-0.24670-0.43415 0 5 -12 10.48 420.77 1 0.20643-0.45955-0.55619 0.88804-0.80500-0.01333 0 5 -11 705.35 355.59 1 0.20805-0.43582-0.55792 0.89845-0.80338 0.05324 0 5 -10 5169.11 737.25 1 0.20561-0.40804-0.55532 0.90452-0.80581 0.12386 0 5 -9 346.60 473.16 1 0.19758-0.37496-0.54911 0.90570-0.81205 0.19774 0 5 -8 2830.24 553.20 1 0.18378-0.33579-0.53418 0.89963-0.82514 0.27909 0 5 -7 3391.74 394.96 1 0.16185-0.28848-0.51004 0.88436-0.84478 0.36698 0 5 -6 8554.51 667.96 1 0.12927-0.23052-0.47330 0.85649-0.87135 0.46181 0 5 -513128.48 663.57 1 0.08276-0.15863-0.41913 0.81118-0.90414 0.56285 0 -5 517131.40 548.23 1 0.18141-0.10502-0.80556 0.41425-0.56404 0.90408 0 5 -432577.82 953.96 1 0.01852-0.06901-0.34110 0.74202-0.93984 0.66681 0 -5 435633.47 705.24 1 0.40350-0.35222-0.66869 0.26853-0.62452 0.89656 0 5 -3 1.34 263.58 1-0.06727 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1-0.50112-0.21313-0.84888 0.73533-0.16812 0.64332 -9 -2 6 2424.78 660.76 1-0.46083-0.27908-0.86414 0.74203-0.20218 0.60950 -9 -2 5 174.01 367.99 1-0.42288-0.34269-0.87578 0.74512-0.23271 0.57214 -9 -2 4 -58.37 350.46 1-0.38795-0.40330-0.88436 0.74513-0.25960 0.53114 -9 -2 3 874.74 335.11 1-0.35598-0.46119-0.89178 0.74404-0.27926 0.48342 -9 -2 213812.73 1117.79 1-0.32892-0.51382-0.89592 0.73964-0.29853 0.43463 -9 -2 1 8872.45 924.98 1-0.30652-0.56180-0.89856 0.73374-0.31404 0.38209 -9 -2 0 2465.29 635.37 1-0.28918-0.60470-0.90013 0.72677-0.32577 0.32577 -9 -3 813063.28 1237.85 1-0.49049-0.20855-0.85322 0.66149-0.17728 0.72036 -9 -3 710618.26 1118.57 1-0.44613-0.27859-0.86895 0.66867-0.21418 0.68938 -9 -3 612526.57 1185.29 1-0.40399-0.34639-0.88067 0.67183-0.24739 0.65471 -9 -3 5 516.54 421.87 1-0.36476-0.41129-0.88898 0.67159-0.27684 0.61627 -9 -3 4 3082.50 772.69 1-0.32818-0.47388-0.89602 0.67014-0.29905 0.57126 -9 -3 3 127.91 373.86 1-0.29655-0.53108-0.89951 0.66509-0.32081 0.52497 -9 -3 2 873.01 451.19 1-0.26941-0.58379-0.90142 0.65846-0.33887 0.47498 -9 -3 1 3916.14 795.55 1-0.24714-0.63163-0.90227 0.65077-0.35329 0.42134 -9 -4 6 7680.67 930.95 1-0.35235-0.40902-0.89240 0.59692-0.28188 0.69020 -9 -4 5 1281.11 495.18 1-0.31280-0.47414-0.89789 0.59387-0.30973 0.64999 -9 -4 4 5988.65 947.65 1-0.27720-0.53532-0.90098 0.58841-0.33375 0.60596 -10 2 4 3448.66 706.99 1-0.67199-0.17623-0.74055 0.94619-0.00002 0.27140 -10 2 3 199.24 342.01 1-0.65692-0.21666-0.75376 0.95098-0.01710 0.22064 -10 1 6 6546.77 920.90 1-0.65517-0.15249-0.75523 0.89171-0.01904 0.42612 -10 1 511599.49 1120.81 1-0.63225-0.20077-0.77350 0.90157-0.04397 0.38320 -10 1 4 234.49 354.93 1-0.61161-0.24522-0.78854 0.90949-0.06414 0.33568 -10 1 3 1453.50 485.50 1-0.59303-0.28947-0.80089 0.91328-0.08288 0.28654 -10 0 6 963.08 437.45 1-0.59952-0.21645-0.79670 0.84803-0.07640 0.48372 -10 0 5 1283.45 582.08 1-0.57300-0.26864-0.81312 0.85589-0.10246 0.44189 -10 0 4 2086.45 628.74 1-0.54871-0.31859-0.82654 0.86076-0.12541 0.39695 -10 0 314425.09 1275.93 1-0.52722-0.36575-0.83725 0.86291-0.14504 0.34870 -10 -1 512728.44 2230.04 1-0.51383-0.33828-0.84340 0.79945-0.15698 0.49641 ; _shelx_hkl_checksum 57293 _shelx_res_file ; TITL shelx in P -1 p242.res created by SHELXL-2018/3 at 21:43:09 on 11-Sep-2018 CELL 0.71073 7.806 8.263 10.414 97.26 109.65 93.79 ZERR 2 0.004 0.003 0.006 0.011 0.02 0.02 LATT 1 SFAC C H O S UNIT 26 24 4 4 L.S. 10 PLAN 20 HTAB CONF BOND $h fmap 2 acta SHEL 9999 0.84 REM REM REM WGHT 0.072000 0.113500 EXTI 0.059553 FVAR 19.78008 S1 4 0.773641 0.321432 -0.099534 11.00000 0.04269 0.04708 = 0.03608 0.00496 0.01760 0.00255 S2 4 0.736062 0.605552 0.100123 11.00000 0.04020 0.03465 = 0.04880 0.00103 0.01480 -0.00262 O1 3 0.760558 -0.149819 0.628540 11.00000 0.07290 0.06520 = 0.04226 0.01242 0.02718 0.00132 O2 3 0.794989 0.464229 0.335036 11.00000 0.08697 0.04598 = 0.04288 -0.00406 0.02140 0.00403 C1 1 0.808449 0.130165 -0.052658 11.00000 0.05118 0.04212 = 0.04532 0.00083 0.02351 0.00723 AFIX 43 H1 2 0.820956 0.039871 -0.110524 11.00000 -1.20000 AFIX 0 C2 1 0.671506 0.035884 0.313890 11.00000 0.03560 0.05346 = 0.03021 -0.00024 0.00725 -0.00474 AFIX 43 H2 2 0.607492 0.011357 0.219380 11.00000 -1.20000 AFIX 0 C3 1 0.862103 0.107237 0.593042 11.00000 0.04002 0.06150 = 0.02579 -0.00132 0.01059 0.00050 AFIX 43 H3 2 0.927331 0.131023 0.687398 11.00000 -1.20000 AFIX 0 C4 1 0.776595 0.187997 0.367923 11.00000 0.03253 0.04480 = 0.02960 0.00088 0.01155 -0.00006 C5 1 0.815275 0.127532 0.077326 11.00000 0.04086 0.03932 = 0.04206 0.00668 0.01572 0.00787 AFIX 43 H5 2 0.834586 0.034541 0.119774 11.00000 -1.20000 AFIX 0 C6 1 0.870063 0.221452 0.510703 11.00000 0.03750 0.04840 = 0.03108 -0.00479 0.01102 -0.00361 AFIX 43 H6 2 0.938609 0.323029 0.550038 11.00000 -1.20000 AFIX 0 C7 1 0.790048 0.281281 0.144588 11.00000 0.02904 0.03983 = 0.03346 0.00070 0.00886 0.00083 C8 1 0.691323 0.672145 -0.064197 11.00000 0.05038 0.04436 = 0.06226 0.01732 0.01696 -0.00092 AFIX 137 H8A 2 0.594501 0.598579 -0.133310 11.00000 -1.50000 H8B 2 0.800026 0.672480 -0.087893 11.00000 -1.50000 H8C 2 0.655487 0.781032 -0.059371 11.00000 -1.50000 AFIX 0 C9 1 0.661447 -0.312328 0.574597 11.00000 0.10795 0.06274 = 0.06267 0.01220 0.05165 -0.00421 AFIX 137 H9A 2 0.704580 -0.365458 0.505805 11.00000 -1.50000 H9B 2 0.533040 -0.303439 0.533903 11.00000 -1.50000 H9C 2 0.681017 -0.375822 0.648323 11.00000 -1.50000 AFIX 0 C10 1 0.767974 0.401044 0.059525 11.00000 0.02426 0.03890 = 0.03564 -0.00051 0.00957 -0.00329 C11 1 0.757054 -0.045010 0.537148 11.00000 0.04068 0.05480 = 0.03723 0.00682 0.02039 0.00365 C12 1 0.788123 0.320062 0.284565 11.00000 0.03505 0.04426 = 0.03358 -0.00258 0.00797 -0.00007 C13 1 0.659683 -0.079243 0.396422 11.00000 0.04089 0.05282 = 0.03866 -0.00142 0.01289 -0.00968 AFIX 43 H13 2 0.586967 -0.179094 0.358019 11.00000 -1.20000 AFIX 0 HKLF 4 REM shelx in P -1 REM wR2 = 0.1284, GooF = S = 1.087, Restrained GooF = 1.087 for all data REM R1 = 0.0464 for 1899 Fo > 4sig(Fo) and 0.0513 for all 2165 data REM 157 parameters refined using 0 restraints END WGHT 0.0720 0.1135 REM Instructions for potential hydrogen bonds EQIV $1 x, y-1, z HTAB C9 O2_$1 REM Highest difference peak 0.369, deepest hole -0.331, 1-sigma level 0.057 Q1 1 0.7698 0.5038 0.0611 11.00000 0.05 0.37 Q2 1 0.7811 0.3961 -0.0109 11.00000 0.05 0.35 Q3 1 0.8148 0.2062 0.1221 11.00000 0.05 0.27 Q4 1 0.8504 0.0240 0.5565 11.00000 0.05 0.22 Q5 1 0.7024 0.3404 0.0681 11.00000 0.05 0.20 Q6 1 0.7691 0.2221 0.3545 11.00000 0.05 0.19 Q7 1 0.8342 0.7050 0.2142 11.00000 0.05 0.19 Q8 1 0.7047 0.7004 0.1580 11.00000 0.05 0.19 Q9 1 0.7896 0.1142 0.3290 11.00000 0.05 0.19 Q10 1 0.9804 0.4858 0.0517 11.00000 0.05 0.19 Q11 1 0.7119 0.0150 -0.1779 11.00000 0.05 0.18 Q12 1 0.6237 -0.3626 0.4780 11.00000 0.05 0.18 Q13 1 0.7937 0.8038 0.0190 11.00000 0.05 0.18 Q14 1 0.7836 -0.2452 0.5594 11.00000 0.05 0.17 Q15 1 0.7119 -0.1285 0.6410 11.00000 0.05 0.16 Q16 1 0.8014 0.0322 0.7040 11.00000 0.05 0.16 Q17 1 0.8852 0.3950 -0.0925 11.00000 0.05 0.16 Q18 1 0.8558 0.6744 0.1115 11.00000 0.05 0.15 Q19 1 0.8734 0.1757 0.0094 11.00000 0.05 0.15 Q20 1 0.6233 0.7634 -0.0186 11.00000 0.05 0.15 ; _shelx_res_checksum 58799 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy S S1 0.77364(8) 0.32143(7) -0.09953(6) 0.0412(3) Uani d 1 S S2 0.73606(8) 0.60555(7) 0.10012(6) 0.0422(3) Uani d 1 O O1 0.7606(3) -0.1498(2) 0.62854(18) 0.0582(5) Uani d 1 O O2 0.7950(3) 0.4642(2) 0.33504(18) 0.0601(5) Uani d 1 C C1 0.8084(3) 0.1302(3) -0.0527(3) 0.0450(6) Uani d 1 H H1 0.820956 0.039871 -0.110524 0.054 Uiso calc 1 C C2 0.6715(3) 0.0359(3) 0.3139(2) 0.0419(6) Uani d 1 H H2 0.607492 0.011357 0.219380 0.050 Uiso calc 1 C C3 0.8621(3) 0.1072(3) 0.5930(2) 0.0437(6) Uani d 1 H H3 0.927331 0.131023 0.687398 0.052 Uiso calc 1 C C4 0.7766(3) 0.1880(3) 0.3679(2) 0.0361(5) Uani d 1 C C5 0.8153(3) 0.1275(3) 0.0773(2) 0.0402(5) Uani d 1 H H5 0.834586 0.034541 0.119774 0.048 Uiso calc 1 C C6 0.8701(3) 0.2215(3) 0.5107(2) 0.0407(5) Uani d 1 H H6 0.938609 0.323029 0.550038 0.049 Uiso calc 1 C C7 0.7900(3) 0.2813(3) 0.1446(2) 0.0352(5) Uani d 1 C C8 0.6913(4) 0.6721(3) -0.0642(3) 0.0525(6) Uani d 1 H H8A 0.594501 0.598579 -0.133310 0.079 Uiso calc 1 H H8B 0.800026 0.672480 -0.087893 0.079 Uiso calc 1 H H8C 0.655487 0.781032 -0.059371 0.079 Uiso calc 1 C C9 0.6614(5) -0.3123(4) 0.5746(3) 0.0726(9) Uani d 1 H H9A 0.704580 -0.365458 0.505805 0.109 Uiso calc 1 H H9B 0.533040 -0.303439 0.533903 0.109 Uiso calc 1 H H9C 0.681017 -0.375822 0.648323 0.109 Uiso calc 1 C C10 0.7680(3) 0.4010(3) 0.0595(2) 0.0341(5) Uani d 1 C C11 0.7571(3) -0.0450(3) 0.5371(2) 0.0426(5) Uani d 1 C C12 0.7881(3) 0.3201(3) 0.2846(2) 0.0397(5) Uani d 1 C C13 0.6597(3) -0.0792(3) 0.3964(2) 0.0459(6) Uani d 1 H H13 0.586967 -0.179094 0.358019 0.055 Uiso calc 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.0427(4) 0.0471(4) 0.0361(4) 0.0025(3) 0.0176(3) 0.0050(3) S2 0.0402(4) 0.0346(4) 0.0488(4) -0.0026(2) 0.0148(3) 0.0010(2) O1 0.0729(13) 0.0652(12) 0.0423(10) 0.0013(10) 0.0272(9) 0.0124(8) O2 0.0870(15) 0.0460(10) 0.0429(10) 0.0040(9) 0.0214(9) -0.0041(8) C1 0.0512(14) 0.0421(13) 0.0453(13) 0.0072(10) 0.0235(11) 0.0008(10) C2 0.0356(12) 0.0535(14) 0.0302(10) -0.0047(10) 0.0073(9) -0.0002(9) C3 0.0400(12) 0.0615(15) 0.0258(10) 0.0005(11) 0.0106(9) -0.0013(10) C4 0.0325(11) 0.0448(12) 0.0296(10) -0.0001(9) 0.0115(8) 0.0009(9) C5 0.0409(12) 0.0393(12) 0.0421(12) 0.0079(9) 0.0157(10) 0.0067(9) C6 0.0375(12) 0.0484(13) 0.0311(11) -0.0036(10) 0.0110(9) -0.0048(9) C7 0.0290(10) 0.0398(11) 0.0335(11) 0.0008(8) 0.0089(8) 0.0007(9) C8 0.0504(15) 0.0444(13) 0.0623(16) -0.0009(11) 0.0170(12) 0.0173(12) C9 0.108(3) 0.0627(18) 0.0627(18) -0.0042(17) 0.0516(18) 0.0122(14) C10 0.0243(10) 0.0389(11) 0.0356(11) -0.0033(8) 0.0096(8) -0.0005(9) C11 0.0407(13) 0.0548(14) 0.0372(11) 0.0036(11) 0.0204(9) 0.0068(10) C12 0.0351(12) 0.0443(12) 0.0336(11) -0.0001(9) 0.0080(9) -0.0026(9) C13 0.0409(13) 0.0528(14) 0.0387(12) -0.0097(11) 0.0129(10) -0.0014(10) 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 C10 S1 C1 92.19(11) C10 S2 C8 100.76(12) C11 O1 C9 117.8(2) C5 C1 S1 111.72(18) C5 C1 H1 124.1 S1 C1 H1 124.1 C13 C2 C4 121.9(2) C13 C2 H2 119.0 C4 C2 H2 119.0 C6 C3 C11 120.7(2) C6 C3 H3 119.6 C11 C3 H3 119.6 C2 C4 C6 117.6(2) C2 C4 C12 124.3(2) C6 C4 C12 118.1(2) C1 C5 C7 113.6(2) C1 C5 H5 123.2 C7 C5 H5 123.2 C3 C6 C4 121.0(2) C3 C6 H6 119.5 C4 C6 H6 119.5 C10 C7 C5 111.7(2) C10 C7 C12 120.6(2) C5 C7 C12 127.7(2) S2 C8 H8A 109.5 S2 C8 H8B 109.5 H8A C8 H8B 109.5 S2 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 O1 C9 H9A 109.5 O1 C9 H9B 109.5 H9A C9 H9B 109.5 O1 C9 H9C 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 C7 C10 S1 110.79(16) C7 C10 S2 127.08(17) S1 C10 S2 122.13(14) O1 C11 C13 125.0(2) O1 C11 C3 115.7(2) C13 C11 C3 119.3(2) O2 C12 C7 119.5(2) O2 C12 C4 119.2(2) C7 C12 C4 121.33(19) C2 C13 C11 119.5(2) C2 C13 H13 120.3 C11 C13 H13 120.3 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 C10 1.719(2) S1 C1 1.724(3) S2 C10 1.744(2) S2 C8 1.793(3) O1 C11 1.360(3) O1 C9 1.448(4) O2 C12 1.230(3) C1 C5 1.340(4) C1 H1 0.9300 C2 C13 1.379(3) C2 C4 1.394(3) C2 H2 0.9300 C3 C6 1.365(3) C3 C11 1.397(4) C3 H3 0.9300 C4 C6 1.400(3) C4 C12 1.494(3) C5 C7 1.430(3) C5 H5 0.9300 C6 H6 0.9300 C7 C10 1.391(3) C7 C12 1.458(3) C8 H8A 0.9600 C8 H8B 0.9600 C8 H8C 0.9600 C9 H9A 0.9600 C9 H9B 0.9600 C9 H9C 0.9600 C11 C13 1.387(3) C13 H13 0.9300 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C6 H6 O2 2_766 0.93 2.48 3.374(4) 161 C9 H9A O2 1_545 0.96 2.45 3.400(4) 172 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 C10 S1 C1 C5 0.0(2) C13 C2 C4 C6 -0.5(4) C13 C2 C4 C12 -177.3(2) S1 C1 C5 C7 0.8(3) C11 C3 C6 C4 -1.4(4) C2 C4 C6 C3 1.7(3) C12 C4 C6 C3 178.7(2) C1 C5 C7 C10 -1.4(3) C1 C5 C7 C12 179.4(2) C5 C7 C10 S1 1.3(2) C12 C7 C10 S1 -179.42(16) C5 C7 C10 S2 -179.26(16) C12 C7 C10 S2 0.0(3) C1 S1 C10 C7 -0.78(18) C1 S1 C10 S2 179.77(14) C8 S2 C10 C7 -173.3(2) C8 S2 C10 S1 6.09(16) C9 O1 C11 C13 2.7(4) C9 O1 C11 C3 -176.9(2) C6 C3 C11 O1 179.4(2) C6 C3 C11 C13 -0.2(4) C10 C7 C12 O2 -11.1(3) C5 C7 C12 O2 168.1(2) C10 C7 C12 C4 168.49(19) C5 C7 C12 C4 -12.4(4) C2 C4 C12 O2 141.9(3) C6 C4 C12 O2 -34.8(3) C2 C4 C12 C7 -37.6(3) C6 C4 C12 C7 145.6(2) C4 C2 C13 C11 -1.1(4) O1 C11 C13 C2 -178.2(2) C3 C11 C13 C2 1.4(4) _cod_database_fobs_code 2242746