#------------------------------------------------------------------------------ #$Date: 2019-10-29 03:11:48 +0200 (Tue, 29 Oct 2019) $ #$Revision: 220331 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/25/1552500.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_1552500 loop_ _publ_author_name 'Mcleod, Matthew J.' 'Krismanich, Anthony P.' 'Assoud, Abdeljalil' 'Dmitrienko, Gary I.' 'Holyoak, Todd' _publ_section_title ; Characterization of 3-[(Carboxymethyl)thio]picolinic Acid: A Novel Inhibitor of Phosphoenolpyruvate Carboxykinase. ; _journal_issue 37 _journal_name_full Biochemistry _journal_page_first 3918 _journal_page_last 3926 _journal_paper_doi 10.1021/acs.biochem.9b00583 _journal_volume 58 _journal_year 2019 _chemical_formula_sum 'C8 H7 N O4 S' _chemical_formula_weight 213.21 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 90 _cell_angle_beta 94.6669(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.8712(2) _cell_length_b 15.8059(5) _cell_length_c 9.0571(3) _cell_measurement_reflns_used 505 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 30.0 _cell_measurement_theta_min 1.5 _cell_volume 837.71(5) _computing_cell_refinement 'SMART, 'Bruker APEX II' _computing_data_collection 'Bruker kappa APEX II' _computing_data_reduction 'SAINT, 'Bruker APEX II' _computing_molecular_graphics Mercury _computing_structure_refinement 'SHELXL-2016 (Sheldrick, 2016/6)' _computing_structure_solution 'SHELXL-2016 (Sheldrick, 2016/6)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'BRUKER SMART APEX II' _diffrn_measurement_method 'Omega and phi scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_unetI/netI 0.0123 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 14410 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.992 _diffrn_reflns_theta_min 2.577 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 1 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.371 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_correction_T_min 0.7098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.690 _exptl_crystal_description needle _exptl_crystal_F_000 440 _exptl_crystal_size_max 0.355 _exptl_crystal_size_mid 0.075 _exptl_crystal_size_min 0.020 _refine_diff_density_max 0.319 _refine_diff_density_min -0.187 _refine_diff_density_rms 0.048 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 129 _refine_ls_number_reflns 2016 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.064 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0290 _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^)+(0.0383P)^2^+0.3467P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.0786 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1762 _reflns_number_total 2016 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file bi9b00583_si_002.cif _cod_data_source_block GD3_0m _cod_database_code 1552500 _shelx_shelxl_version_number 2016/6 _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 0.879 _shelx_estimated_absorpt_t_max 0.993 _shelx_res_file ; TITL GD3_0m in P2(1)/c GD3_0m.res created by SHELXL-2016/6 at 11:15:35 on 20-Jun-2018 CELL 0.71073 5.87120 15.80590 9.05710 90.0000 94.6669 90.0000 ZERR 4.00 0.00020 0.00050 0.00030 0.0000 0.0008 0.0000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O S UNIT 32 28 4 16 4 TEMP 23.000 SIZE 0.02 0.075 0.355 L.S. 10 BOND $H LIST 6 FMAP 2 PLAN 5 OMIT -3 56 ACTA WGHT 0.038300 0.346700 FVAR 0.43789 S1 5 0.262727 0.688662 0.661999 11.00000 0.03220 0.01530 = 0.03852 0.00040 0.01639 -0.00035 C2 1 0.466754 0.743904 0.568210 11.00000 0.02370 0.01686 = 0.02420 0.00139 0.00482 0.00080 C3 1 0.459767 0.832332 0.563365 11.00000 0.02593 0.01798 = 0.02607 0.00075 0.00649 0.00048 N4 3 0.616579 0.873395 0.490116 11.00000 0.03204 0.01602 = 0.03454 0.00259 0.01107 0.00006 AFIX 43 H4 2 0.611365 0.927769 0.489163 11.00000 -1.20000 AFIX 0 C5 1 0.779031 0.836321 0.419071 11.00000 0.03154 0.02697 = 0.03652 0.00445 0.01455 -0.00118 AFIX 43 H5 2 0.882426 0.868460 0.370347 11.00000 -1.20000 AFIX 0 C6 1 0.790937 0.749478 0.419158 11.00000 0.03039 0.02653 = 0.03686 0.00007 0.01419 0.00486 AFIX 43 H6 2 0.902202 0.721949 0.369639 11.00000 -1.20000 AFIX 0 C7 1 0.636538 0.703601 0.493270 11.00000 0.03050 0.01753 = 0.03618 0.00123 0.00972 0.00452 AFIX 43 H7 2 0.644932 0.644845 0.493666 11.00000 -1.20000 AFIX 0 C8 1 0.286526 0.890761 0.626652 11.00000 0.03126 0.01642 = 0.04195 -0.00176 0.01336 0.00151 O9 4 0.282657 0.964039 0.579720 11.00000 0.05775 0.01870 = 0.08811 0.01349 0.04125 0.01055 O10 4 0.161602 0.858597 0.716667 11.00000 0.04997 0.02043 = 0.05839 0.00117 0.03365 0.00344 C11 1 0.321132 0.579278 0.615160 11.00000 0.03040 0.01580 = 0.03944 -0.00093 0.01110 -0.00029 AFIX 23 H11A 2 0.335592 0.573705 0.509677 11.00000 -1.20000 H11B 2 0.462038 0.560212 0.668144 11.00000 -1.20000 AFIX 0 C12 1 0.120024 0.527526 0.660472 11.00000 0.03470 0.01750 = 0.02856 -0.00294 0.00843 -0.00130 O13 4 0.180482 0.452966 0.714078 11.00000 0.03770 0.02141 = 0.04991 0.00843 0.01347 0.00010 AFIX 148 H13 2 0.056521 0.424500 0.735591 11.00000 -1.50000 AFIX 0 O14 4 -0.074802 0.552510 0.644363 11.00000 0.03082 0.02835 = 0.05089 0.00191 0.01072 0.00080 HKLF 4 REM GD3_0m in P2(1)/c REM R1 = 0.0290 for 1762 Fo > 4sig(Fo) and 0.0348 for all 2016 data REM 129 parameters refined using 0 restraints END WGHT 0.0382 0.3483 REM Highest difference peak 0.319, deepest hole -0.187, 1-sigma level 0.048 Q1 1 0.3154 0.4438 0.7251 11.00000 0.05 0.32 Q2 1 0.3819 0.8589 0.6062 11.00000 0.05 0.31 Q3 1 0.3740 0.7188 0.6081 11.00000 0.05 0.29 Q4 1 0.4531 0.7877 0.5673 11.00000 0.05 0.28 Q5 1 0.8018 0.7927 0.4473 11.00000 0.05 0.27 ; _shelx_res_checksum 15436 _shelx_hkl_file ; 1 0 0 81.3398 1.07922 6 2 0 0 1714.88 17.5558 6 -2 0 0 1718.20 16.5420 8 2 0 0 1726.13 16.4977 5 -2 0 0 1708.25 16.5837 1 -2 0 0 1717.05 16.4322 3 3 0 0 24.2655 0.82283 5 3 0 0 24.8484 0.86796 6 -3 0 0 24.8391 0.88879 1 -3 0 0 24.2363 0.77443 3 -3 0 0 24.7415 0.84054 8 -4 0 0 49.6710 1.39476 8 4 0 0 47.9723 1.30801 5 -4 0 0 47.5852 1.26900 3 4 0 0 49.2007 1.38479 6 -4 0 0 48.3519 1.42902 1 -5 0 0 23.3038 1.14997 1 5 0 0 20.8254 1.01910 5 5 0 0 22.0345 1.13568 6 -5 0 0 22.0284 1.12246 8 -5 0 0 24.1415 1.09127 3 6 0 0 18.3978 1.11797 5 -6 0 0 18.5081 1.32407 1 -6 0 0 18.3553 1.21181 8 6 0 0 19.4303 1.25390 6 -7 0 0 -0.3432 0.66541 1 7 0 0 -0.1036 0.51959 5 -8 0 0 2.51451 0.99036 1 0 -1 0 -0.0072 0.02374 6 1 -1 0 185.559 2.11822 6 1 1 0 180.277 1.96507 6 2 -1 0 24.2834 0.74373 6 -2 -1 0 25.4776 0.73941 8 -2 -1 0 23.9580 0.64032 3 2 -1 0 25.3418 0.65231 5 -2 -1 0 25.2733 0.74529 1 -2 1 0 23.3947 0.66635 8 2 1 0 24.9560 0.68065 6 2 1 0 23.9567 0.69329 5 -2 1 0 24.9149 0.68695 3 -2 1 0 24.8236 0.73324 1 -3 -1 0 158.289 2.24054 3 -3 -1 0 160.200 2.46344 1 3 -1 0 155.787 2.27065 5 3 -1 0 162.891 2.47810 6 3 -1 0 156.542 2.04770 4 -3 -1 0 155.928 2.40493 8 3 1 0 158.170 2.36674 5 3 1 0 157.402 2.32292 6 -3 1 0 158.496 2.28905 3 -3 1 0 155.418 2.33772 8 -3 1 0 154.036 2.41273 1 -4 -1 0 8.57102 0.65838 3 -4 -1 0 7.79455 0.69229 1 4 -1 0 8.84758 0.64628 5 -4 -1 0 7.87256 0.69367 8 4 -1 0 9.93431 0.73706 6 4 1 0 8.84862 0.68901 6 -4 1 0 8.51015 0.64993 3 -4 1 0 8.98036 0.70060 8 4 1 0 8.80867 0.67136 5 -4 1 0 9.12658 0.69415 1 -5 -1 0 107.870 2.18845 3 -5 -1 0 108.976 2.40802 8 5 -1 0 108.119 2.23310 5 -5 -1 0 106.088 2.42785 1 5 -1 0 110.046 2.45209 6 -5 1 0 107.343 2.33078 8 5 1 0 108.473 2.31286 5 5 1 0 104.833 2.30238 6 -5 1 0 107.854 2.45325 1 -5 1 0 107.068 2.19981 3 -6 -1 0 180.335 3.51930 8 6 -1 0 182.471 3.59691 6 6 -1 0 181.044 3.37569 5 -6 -1 0 178.211 3.61991 1 6 1 0 180.182 3.38202 5 6 1 0 183.137 3.47396 6 -6 1 0 176.367 3.56819 1 -6 1 0 177.265 3.24940 3 -6 1 0 184.656 3.46257 8 -7 -1 0 -0.7991 0.61368 1 -7 -1 0 -0.7678 0.84473 8 7 -1 0 0.08640 0.57050 6 -7 1 0 -0.2651 0.66764 1 7 1 0 0.74704 0.59018 5 -8 -1 0 7.10771 1.19342 1 -8 1 0 5.23999 1.13898 1 0 -2 0 43.8266 0.59375 6 0 2 0 43.8337 0.52270 7 1 -2 0 704.095 7.04852 6 1 2 0 708.106 6.83446 6 2 -2 0 14.9091 0.51616 5 2 -2 0 14.9752 0.64157 6 -2 -2 0 15.1108 0.62407 8 -2 -2 0 14.7104 0.61654 1 -2 -2 0 14.9438 0.53537 3 2 2 0 15.6124 0.60066 5 2 2 0 13.8744 0.50456 6 -2 2 0 13.7930 0.57574 1 -2 2 0 13.9233 0.60990 8 -2 2 0 13.5768 0.55280 3 -3 -2 0 20.5244 0.70594 3 3 -2 0 19.7699 0.85061 6 -3 -2 0 19.2615 0.81403 8 -3 -2 0 19.1686 0.82954 1 3 -2 0 19.6090 0.70387 5 3 -2 0 20.1717 0.64527 4 -3 2 0 19.6998 0.72463 8 -3 2 0 21.4700 0.83344 1 -3 2 0 18.8123 0.73647 3 3 2 0 19.9587 0.72589 6 3 2 0 19.1065 0.77375 5 -4 -2 0 138.694 2.25529 3 -4 -2 0 136.235 2.50321 8 4 -2 0 139.350 2.31689 5 4 -2 0 143.096 2.59960 6 -4 -2 0 131.583 2.48390 1 4 -2 0 134.935 2.04554 4 -4 2 0 137.478 2.51582 1 4 2 0 137.682 2.44981 5 -4 2 0 136.511 2.34008 3 4 2 0 139.108 2.35744 6 -4 2 0 135.365 2.34965 8 -5 -2 0 16.5656 1.08541 1 5 -2 0 15.2165 0.90652 5 5 -2 0 14.3627 1.01929 6 -5 -2 0 12.7222 0.96269 8 -5 -2 0 14.6122 0.90878 3 -5 2 0 16.1271 1.06119 1 5 2 0 15.3770 0.93522 6 5 2 0 15.3191 0.95980 5 -5 2 0 13.7709 0.93601 8 -5 2 0 17.1805 0.96002 3 6 -2 0 8.81550 0.86509 5 6 -2 0 9.80883 1.02151 6 -6 -2 0 8.49927 1.01564 1 -6 -2 0 10.2385 1.06146 8 6 2 0 10.4504 0.99160 5 -6 2 0 7.43862 0.84205 3 -6 2 0 8.47657 1.01086 1 7 -2 0 1.03850 0.64058 6 -7 -2 0 1.00040 0.76971 1 -7 -2 0 0.34011 0.70260 8 -7 2 0 0.92459 0.73849 1 7 2 0 0.43050 0.53445 5 -8 -2 0 6.51841 1.21323 1 -8 2 0 9.69265 1.39913 1 8 2 0 5.18062 1.02747 5 0 -3 0 -0.0379 0.11791 6 0 3 0 0.08746 0.09711 7 1 -3 0 139.575 1.86203 6 1 3 0 136.050 1.49953 6 2 -3 0 46.1328 1.10369 6 -2 -3 0 45.7454 1.01838 1 -2 -3 0 46.1972 1.08802 8 2 -3 0 45.5707 0.93831 4 -2 3 0 45.4134 1.00663 3 -2 3 0 45.1675 1.00374 1 -2 3 0 44.3296 1.02816 8 2 3 0 45.7139 1.02877 5 2 3 0 46.5939 0.84386 6 -3 -3 0 128.804 1.97670 3 3 -3 0 129.828 1.94192 4 3 -3 0 132.212 1.97449 5 -3 -3 0 130.314 2.24940 8 3 -3 0 134.725 2.31234 6 -3 -3 0 130.840 2.20488 1 -3 3 0 131.683 2.17094 1 3 3 0 129.480 1.95683 6 -3 3 0 131.351 2.02345 8 3 3 0 129.549 2.17013 5 -3 3 0 130.751 2.10225 3 4 -3 0 18.0317 0.72573 4 4 -3 0 17.3103 0.78990 5 -4 -3 0 19.0475 0.97367 8 4 -3 0 19.0148 1.00748 6 -4 -3 0 18.3023 0.81496 3 -4 -3 0 20.3197 1.01416 1 4 3 0 18.4902 0.91500 5 -4 3 0 17.6600 0.93114 1 4 3 0 17.4843 0.81207 6 -4 3 0 19.1599 0.90920 3 -4 3 0 18.9486 0.85627 8 5 -3 0 43.1798 1.60404 6 -5 -3 0 41.4346 1.55284 8 5 -3 0 44.0133 1.38191 5 -5 -3 0 40.3819 1.33190 3 -5 -3 0 43.1977 1.57050 1 5 3 0 41.8838 1.36352 6 -5 3 0 40.6472 1.38090 8 -5 3 0 43.1261 1.56423 1 -5 3 0 40.7180 1.41946 3 5 3 0 41.1415 1.45435 5 -6 -3 0 0.15341 0.48859 1 6 -3 0 0.92948 0.55810 6 -6 -3 0 -0.2773 0.52216 8 6 3 0 0.83475 0.49991 5 -6 3 0 -0.1704 0.53670 1 -6 3 0 0.60046 0.51971 3 -7 -3 0 2.12088 0.83502 1 7 -3 0 0.48929 0.66605 6 -7 -3 0 1.18594 0.76913 8 7 3 0 0.97738 0.60365 5 -7 3 0 1.32795 0.79305 1 -8 -3 0 -0.3578 0.79564 1 -8 3 0 0.63713 0.85441 1 8 3 0 -0.7459 0.63501 5 0 -4 0 0.74799 0.18387 6 0 4 0 1.08240 0.14757 7 1 -4 0 45.2009 0.96450 4 1 -4 0 46.5362 0.97620 6 -1 -4 0 45.3402 0.88286 1 -1 -4 0 46.0153 0.97641 8 1 4 0 45.8473 0.66225 6 1 4 0 45.8348 0.92376 5 -1 4 0 42.7014 0.91399 3 1 4 0 44.8979 1.00192 3 -2 -4 0 15.1538 0.68912 8 -2 -4 0 15.0469 0.64654 1 2 -4 0 15.7307 0.69034 6 2 -4 0 15.0894 0.61378 4 -2 4 0 15.0948 0.62569 1 2 4 0 15.5387 0.65441 5 2 4 0 14.9212 0.45755 6 -2 4 0 14.8627 0.63641 3 -2 4 0 13.4743 0.52926 8 3 -4 0 38.1612 0.99092 4 -3 -4 0 38.3609 0.99722 3 -3 -4 0 35.2762 1.11642 8 3 -4 0 37.5084 1.19949 6 -3 -4 0 37.0203 0.94558 4 -3 -4 0 36.6373 1.11881 1 -3 4 0 37.5123 0.97263 8 -3 4 0 36.4654 1.06203 3 3 4 0 38.6049 1.12345 5 3 4 0 38.2007 0.91400 6 -3 4 0 37.7689 1.07247 1 4 -4 0 15.6038 0.97142 6 -4 -4 0 14.7936 0.92940 1 4 -4 0 15.1835 0.75422 4 -4 -4 0 14.3707 0.78105 3 -4 -4 0 17.1029 0.96456 8 4 4 0 15.7357 0.84058 5 4 4 0 15.1802 0.73548 6 -4 4 0 14.1182 0.77870 8 -4 4 0 15.6191 0.85855 3 -4 4 0 14.7741 0.89052 1 -5 -4 0 3.69403 0.64922 8 5 -4 0 3.86739 0.71582 6 -5 -4 0 3.20897 0.54996 3 -5 -4 0 3.87460 0.65554 1 5 4 0 4.36572 0.64261 5 -5 4 0 3.48275 0.60469 3 -5 4 0 3.31178 0.63286 1 -5 4 0 3.02066 0.58145 8 6 -4 0 -0.5281 0.47193 6 -6 -4 0 0.06621 0.51513 8 -6 -4 0 -0.2232 0.53411 1 -6 4 0 -0.0332 0.54679 1 -6 4 0 -0.9075 0.44794 3 6 4 0 0.12642 0.47980 5 -7 -4 0 1.35548 0.77956 8 -7 -4 0 3.12935 0.87002 1 7 -4 0 2.30491 0.74591 6 -7 4 0 1.75901 0.82584 1 7 4 0 3.77628 0.79915 5 -8 -4 0 -1.0667 0.79119 1 8 4 0 0.76830 0.73532 5 -8 4 0 -0.2414 0.81669 1 0 -5 0 -0.0867 0.17120 6 0 -5 0 0.11308 0.24353 4 0 -5 0 0.35519 0.21295 8 0 5 0 0.29127 0.13504 7 0 5 0 0.02019 0.21621 3 -1 -5 0 114.783 1.63376 1 1 -5 0 112.811 1.74422 6 -1 -5 0 110.838 1.74971 8 -1 -5 0 112.074 1.66182 4 1 -5 0 115.445 1.78999 4 -1 5 0 109.601 1.57066 1 1 5 0 111.025 1.65746 3 -1 5 0 111.059 1.74005 3 1 5 0 115.425 1.68727 5 -2 -5 0 616.892 6.88415 8 2 -5 0 630.259 6.76083 4 -2 -5 0 622.887 6.71052 1 -2 -5 0 616.373 6.47082 4 2 -5 0 640.841 6.96658 6 2 5 0 622.601 6.20404 6 2 5 0 637.076 6.80155 5 -2 5 0 608.141 6.76848 3 -2 5 0 623.772 6.64202 1 3 -5 0 0.23930 0.32782 6 3 -5 0 0.23087 0.26248 4 -3 -5 0 0.42940 0.30709 8 -3 -5 0 -0.0357 0.29677 1 -3 -5 0 0.49454 0.23513 4 -3 5 0 0.16316 0.29873 3 3 5 0 0.54379 0.31055 5 3 5 0 0.31242 0.20947 6 -3 5 0 0.45976 0.26562 8 -3 5 0 0.40629 0.29214 1 -4 -5 0 17.4621 0.97744 8 4 -5 0 18.9126 0.85803 4 4 -5 0 21.0787 1.10420 6 -4 -5 0 17.6173 1.00940 1 -4 -5 0 19.5652 0.87548 3 -4 5 0 18.4962 0.85961 8 4 5 0 17.8015 0.95837 5 -4 5 0 19.2751 0.94752 3 4 5 0 19.8444 0.78035 6 -4 5 0 17.2003 0.93955 1 5 -5 0 2.56025 0.62045 6 -5 -5 0 2.83958 0.54241 3 -5 -5 0 5.06814 0.75799 1 -5 -5 0 2.85371 0.66222 8 5 5 0 3.35102 0.59615 5 -5 5 0 3.53641 0.61693 3 -5 5 0 3.95039 0.69343 1 -6 -5 0 2.58541 0.74259 8 -6 -5 0 2.33923 0.64977 1 6 -5 0 2.85416 0.73571 6 -6 5 0 1.74581 0.71367 1 -6 5 0 2.29248 0.64394 3 6 5 0 2.42414 0.67760 5 -7 -5 0 0.69362 0.75295 8 7 -5 0 2.02783 0.73904 6 -7 -5 0 1.65762 0.84427 1 7 5 0 1.52207 0.68484 5 -7 5 0 0.85497 0.76144 1 -8 -5 0 0.92743 0.89396 1 -8 -5 0 1.69572 0.89974 8 -8 5 0 1.31420 0.90588 1 8 5 0 0.73498 0.69526 5 0 -6 0 58.4526 1.21422 4 0 -6 0 57.3335 1.03009 6 0 -6 0 58.9168 1.12814 8 0 6 0 56.2016 0.83614 7 0 6 0 56.7746 1.00879 5 0 6 0 58.6056 1.17686 3 -1 -6 0 1.47509 0.27735 1 -1 -6 0 1.63402 0.32412 8 1 -6 0 1.28514 0.25747 8 1 -6 0 1.80668 0.30921 6 -1 -6 0 1.86891 0.31044 4 1 -6 0 1.31743 0.29366 4 1 6 0 1.55742 0.30115 3 1 6 0 1.17683 0.26324 5 -1 6 0 1.17074 0.31099 3 -1 6 0 0.93806 0.24946 1 -1 6 0 1.28372 0.20660 7 -2 -6 0 100.222 1.62105 4 2 -6 0 101.123 1.82604 4 -2 -6 0 98.4975 1.73777 1 2 -6 0 98.8997 1.88598 6 -2 -6 0 99.2465 1.89683 8 -2 6 0 98.6702 1.43160 5 -2 6 0 99.9703 1.68342 1 2 6 0 102.218 1.81507 5 -2 6 0 97.7778 1.79882 3 2 6 0 99.1053 1.31314 6 -3 -6 0 14.3882 0.79494 1 -3 -6 0 13.7622 0.84310 8 -3 -6 0 14.9580 0.62070 4 3 -6 0 14.7302 0.75098 4 -3 6 0 14.2921 0.80250 3 -3 6 0 15.1156 0.76648 1 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0.22678 0.83056 8 -2 -7 11 0.63346 0.69390 2 2 7 -11 0.01726 0.67981 5 -2 7 11 1.01407 0.76077 2 -1 -7 11 1.45255 0.74672 2 1 -7 -11 1.78077 0.81996 8 1 -7 -11 0.20330 0.71416 4 1 -7 -11 2.30463 0.87564 1 1 7 -11 1.93022 0.81093 5 -1 7 11 0.30991 0.71154 2 0 -7 -11 1.29166 0.76267 8 0 -7 -11 0.46966 0.79471 1 0 -7 11 0.61864 0.70997 2 0 7 -11 0.66476 0.73377 5 0 7 11 0.27900 0.71573 2 1 -7 11 1.44919 0.82446 2 -1 -7 -11 3.47441 0.97737 1 -1 7 -11 1.86946 0.77881 5 1 7 11 1.47343 0.86712 2 2 -7 11 0.44741 0.79336 2 -2 -7 -11 0.47622 0.70814 3 -2 7 -11 -0.1997 0.70360 5 2 7 11 1.69910 0.89420 2 -3 -8 11 0.09911 0.72772 2 3 -8 -11 -0.1926 0.73766 4 3 8 -11 -1.5022 0.59672 5 -3 8 11 -0.6601 0.72370 2 2 -8 -11 -0.7913 0.68732 4 2 -8 -11 1.36044 0.80049 8 -2 -8 11 0.42872 0.68785 2 -2 8 11 0.03558 0.71365 2 2 8 -11 0.19551 0.69716 5 1 -8 -11 14.8821 1.41667 4 1 -8 -11 13.8094 1.43073 8 1 -8 -11 14.9035 1.49940 1 -1 -8 11 12.1868 1.34187 2 1 8 -11 16.1445 1.51449 5 -1 8 11 16.2377 1.53736 2 0 -8 -11 0.28981 0.71292 8 0 -8 -11 1.76009 0.83515 1 0 -8 11 0.00871 0.68445 2 0 8 11 0.29655 0.67603 2 0 8 -11 0.20721 0.71039 5 -1 -8 -11 1.50423 0.85876 1 1 -8 11 1.95713 0.81490 2 1 8 11 1.77563 0.86610 2 -1 8 -11 1.27189 0.75117 5 -2 -8 -11 1.33082 0.76092 3 2 -8 11 1.88811 0.86471 2 -2 -8 -11 1.05799 0.98787 1 -2 8 -11 2.17971 0.89471 5 2 8 11 1.76873 0.87551 2 3 -9 -11 1.59462 0.96725 8 -3 -9 11 2.38516 0.90816 2 3 -9 -11 2.15195 0.84959 4 3 9 -11 0.99924 0.79193 5 -3 9 11 0.90684 0.84436 2 2 -9 -11 2.99070 0.99807 8 2 -9 -11 1.04807 0.76111 4 -2 -9 11 -0.0172 0.69977 2 2 9 -11 0.92517 0.76178 5 -2 9 11 1.67395 0.84535 2 -1 -9 11 1.05630 0.75448 2 1 -9 -11 -0.0294 0.78353 1 1 -9 -11 -0.0535 0.73137 8 1 -9 -11 1.13186 0.74388 4 1 9 -11 0.12883 0.72660 5 -1 9 11 -0.3301 0.63624 2 0 -9 -11 3.13533 1.04827 1 0 -9 -11 0.55165 0.80277 8 0 -9 11 2.64442 0.89550 2 0 9 11 1.87594 0.83860 2 0 9 -11 2.55937 0.91968 5 -1 -9 -11 3.06271 0.92085 3 1 -9 11 2.36157 0.93468 2 -1 -9 -11 3.48061 0.98998 8 -1 -9 -11 3.31697 1.06463 1 1 9 11 4.62160 1.04077 2 -1 9 -11 2.43600 0.90958 5 2 -10 -11 6.53120 1.18164 8 2 -10 -11 8.94969 1.31274 4 -2 -10 11 5.89826 1.08551 2 -2 10 11 8.91782 1.22432 2 2 10 -11 6.07369 1.07920 5 1 -10 -11 0.90027 0.86422 8 -1 -10 11 0.13007 0.68370 2 1 -10 -11 -0.1520 0.71898 4 1 -10 -11 0.65178 0.89155 1 1 10 -11 0.50408 0.76712 5 -1 10 11 -0.0274 0.70519 2 0 -10 11 0.14435 0.71512 2 0 -10 -11 0.21017 0.84016 8 0 -10 -11 0.28737 0.87607 1 0 10 11 -1.4277 0.61654 2 0 10 -11 0.73079 0.72085 5 1 -10 11 0.83018 0.83669 2 -1 -10 -11 0.39850 0.87854 1 -1 -10 -11 -0.0348 0.75557 8 -1 -10 -11 0.59771 0.72074 3 1 10 11 0.11440 0.76853 2 -1 10 -11 0.38304 0.79063 5 1 -11 -11 6.48352 1.20663 8 -1 -11 11 5.58385 1.08780 2 1 -11 -11 6.65505 1.24705 1 1 -11 -11 7.94117 1.23827 4 -1 11 11 5.95252 1.12424 2 1 11 -11 6.50290 1.14891 5 0 -11 -11 3.30091 1.00351 8 0 -11 -11 4.03991 1.11583 1 0 -11 11 3.70269 1.00014 2 0 11 -11 3.56096 0.94712 5 0 11 11 2.69516 0.95167 2 3 0 -12 1.32283 0.87023 4 -3 0 12 1.11063 0.79784 2 2 0 -12 12.3684 1.38918 4 -2 0 12 13.9112 1.49910 2 -1 0 12 5.16932 0.99987 2 1 0 -12 4.58814 0.97838 4 0 0 12 22.6019 1.71374 2 -1 0 -12 -0.2135 0.65333 5 1 0 12 -0.1739 0.77692 2 -2 0 -12 0.51245 0.71681 5 2 0 12 0.32857 0.77927 2 -3 -1 12 6.74078 1.16236 2 3 -1 -12 8.40190 1.31728 4 -3 1 12 6.98398 1.17916 2 3 1 -12 7.03484 1.20767 4 2 -1 -12 1.63079 0.80963 4 -2 -1 12 1.28919 0.82467 2 2 1 -12 2.44359 0.89793 4 -2 1 12 1.83276 0.88413 2 1 -1 -12 2.68557 0.85203 4 -1 -1 12 4.72137 1.03338 2 -1 1 12 3.23113 0.89829 2 1 1 -12 3.49386 0.87920 4 0 -1 12 9.09869 1.26590 2 0 1 12 13.1662 1.44588 2 1 -1 12 2.52499 0.93852 2 -1 1 -12 4.23965 0.93171 5 1 1 12 4.52707 1.02710 2 -2 -1 -12 0.34988 0.75277 5 2 -1 12 -0.5215 0.80546 2 -2 1 -12 -0.2504 0.66668 5 2 1 12 0.25011 0.83308 2 3 -2 -12 -0.2183 0.72383 4 -3 -2 12 -0.2547 0.71610 2 -3 2 12 -0.4184 0.72692 2 3 2 -12 0.51053 0.75790 4 -2 -2 12 6.15784 1.08520 2 2 -2 -12 7.00127 1.21043 4 -2 2 12 6.95295 1.14371 2 1 -2 -12 3.66884 0.91377 4 -1 -2 12 3.98517 0.96619 2 -1 2 12 2.04834 0.83870 2 0 -2 12 12.0112 1.40747 2 0 2 -12 14.8911 1.38524 5 0 2 12 13.7961 1.43344 2 1 -2 12 0.37670 0.79843 2 1 2 12 -0.9228 0.67925 2 -1 2 -12 0.61349 0.71482 5 -2 -2 -12 6.64765 1.07705 5 2 -2 12 4.78240 1.06420 2 2 2 12 5.73291 1.11940 2 -2 2 -12 8.26628 1.17578 5 3 -3 -12 1.80677 0.86212 4 -3 -3 12 0.43505 0.74929 2 -3 3 12 1.00472 0.81264 2 2 -3 -12 5.08245 1.04273 4 -2 -3 12 5.09975 1.00193 2 -2 3 12 2.96629 0.94508 2 -1 -3 12 0.74160 0.72102 2 1 -3 -12 -0.8583 0.62191 4 -1 3 12 -0.0984 0.67790 2 0 -3 12 0.24424 0.73522 2 0 3 -12 0.97872 0.72879 5 0 3 12 0.48651 0.75237 2 1 -3 12 4.32686 1.07013 2 1 3 12 3.83898 1.02081 2 -1 3 -12 4.33423 0.94912 5 -3 -4 12 1.92722 0.87537 2 3 -4 -12 1.89053 0.90918 4 -3 4 12 2.18014 0.91880 2 -2 -4 12 0.60338 0.69759 2 2 -4 -12 -0.0178 0.69096 4 -2 4 12 0.31608 0.70599 2 -1 -4 12 0.36284 0.70863 2 1 -4 -12 0.53706 0.68851 4 1 4 -12 0.67638 0.68426 5 -1 4 12 0.08744 0.67186 2 0 -4 12 2.06235 0.84144 2 0 4 12 2.59253 0.91464 2 0 4 -12 3.60569 0.92578 5 1 -4 12 1.19785 0.83854 2 1 4 12 0.30899 0.79347 2 -1 4 -12 0.42487 0.70589 5 2 -5 -12 4.91831 1.03422 4 2 -5 -12 5.78943 1.14393 8 -2 -5 12 5.56943 1.07350 2 -2 5 12 5.22522 1.07793 2 1 -5 -12 2.87094 0.88844 4 -1 -5 12 1.67912 0.84366 2 -1 5 12 1.97113 0.86846 2 1 5 -12 1.83622 0.78350 5 0 -5 12 1.25641 0.80794 2 0 5 12 -0.9209 0.67654 2 0 5 -12 -1.1680 0.65732 5 1 -5 12 0.30599 0.75941 2 1 5 12 -0.8159 0.73300 2 -1 5 -12 0.61123 0.80541 5 -2 -6 12 10.2605 1.32591 2 2 -6 -12 10.7135 1.36074 8 2 -6 -12 10.5589 1.33232 4 2 6 -12 11.7931 1.30193 5 -2 6 12 9.08080 1.27468 2 -1 -6 12 2.35840 0.89048 2 1 -6 -12 1.13080 0.76019 4 1 -6 -12 3.13309 0.95157 8 -1 6 12 0.78921 0.75867 2 1 6 -12 0.30020 0.71731 5 0 -6 12 5.94180 1.10614 2 0 6 12 6.23841 1.17884 2 0 6 -12 6.46677 1.11562 5 1 -6 12 0.44434 0.81686 2 1 6 12 0.79778 0.85622 2 -1 6 -12 1.33207 0.84159 5 1 -7 -12 26.6124 1.82899 4 -1 -7 12 24.3363 1.78298 2 1 -7 -12 25.0069 1.89375 8 1 7 -12 26.1604 1.76132 5 -1 7 12 26.3899 1.85075 2 0 -7 12 0.41194 0.79126 2 0 7 12 0.45401 0.82575 2 0 7 -12 1.49076 0.83776 5 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_correction_T_min 0.7098 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71073 5.872 15.808 9.058 89.998 94.683 89.997 ) ; _shelx_hkl_checksum 8247 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 _atom_site_refinement_flags_adp S1 S 0.26273(6) 0.68866(2) 0.66200(4) 0.02794(11) Uani 1 1 d . . C2 C 0.4668(2) 0.74390(8) 0.56821(14) 0.0214(3) Uani 1 1 d . . C3 C 0.4598(2) 0.83233(8) 0.56337(14) 0.0231(3) Uani 1 1 d . . N4 N 0.6166(2) 0.87339(7) 0.49012(13) 0.0271(3) Uani 1 1 d . . H4 H 0.611365 0.927769 0.489163 0.032 Uiso 1 1 calc R U C5 C 0.7790(2) 0.83632(9) 0.41907(17) 0.0310(3) Uani 1 1 d . . H5 H 0.882426 0.868460 0.370347 0.037 Uiso 1 1 calc R U C6 C 0.7909(2) 0.74948(9) 0.41916(16) 0.0306(3) Uani 1 1 d . . H6 H 0.902202 0.721949 0.369639 0.037 Uiso 1 1 calc R U C7 C 0.6365(2) 0.70360(8) 0.49327(16) 0.0277(3) Uani 1 1 d . . H7 H 0.644932 0.644845 0.493666 0.033 Uiso 1 1 calc R U C8 C 0.2865(2) 0.89076(8) 0.62665(17) 0.0293(3) Uani 1 1 d . . O9 O 0.2827(2) 0.96404(7) 0.57972(17) 0.0529(4) Uani 1 1 d . . O10 O 0.1616(2) 0.85860(7) 0.71667(14) 0.0413(3) Uani 1 1 d . . C11 C 0.3211(2) 0.57928(8) 0.61516(17) 0.0281(3) Uani 1 1 d . . H11A H 0.335592 0.573705 0.509677 0.034 Uiso 1 1 calc R U H11B H 0.462038 0.560212 0.668144 0.034 Uiso 1 1 calc R U C12 C 0.1200(2) 0.52753(8) 0.66047(15) 0.0266(3) Uani 1 1 d . . O13 O 0.18048(19) 0.45297(6) 0.71408(13) 0.0358(3) Uani 1 1 d . . H13 H 0.057(3) 0.4245(8) 0.736(2) 0.054 Uiso 1 1 calc R U O14 O -0.07480(18) 0.55251(7) 0.64436(13) 0.0363(3) 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 S1 0.03220(19) 0.01530(16) 0.0385(2) 0.00040(12) 0.01639(14) -0.00035(12) C2 0.0237(6) 0.0169(6) 0.0242(6) 0.0014(5) 0.0048(5) 0.0008(4) C3 0.0259(6) 0.0180(6) 0.0261(6) 0.0008(5) 0.0065(5) 0.0005(5) N4 0.0320(6) 0.0160(5) 0.0345(6) 0.0026(4) 0.0111(5) 0.0001(4) C5 0.0315(7) 0.0270(7) 0.0365(7) 0.0044(6) 0.0146(6) -0.0012(5) C6 0.0304(7) 0.0265(7) 0.0369(7) 0.0001(6) 0.0142(6) 0.0049(6) C7 0.0305(7) 0.0175(6) 0.0362(7) 0.0012(5) 0.0097(6) 0.0045(5) C8 0.0313(7) 0.0164(6) 0.0420(8) -0.0018(5) 0.0134(6) 0.0015(5) O9 0.0578(8) 0.0187(5) 0.0881(10) 0.0135(6) 0.0412(7) 0.0106(5) O10 0.0500(7) 0.0204(5) 0.0584(7) 0.0012(5) 0.0336(6) 0.0034(5) C11 0.0304(7) 0.0158(6) 0.0394(7) -0.0009(5) 0.0111(6) -0.0003(5) C12 0.0347(7) 0.0175(6) 0.0286(6) -0.0029(5) 0.0084(5) -0.0013(5) O13 0.0377(6) 0.0214(5) 0.0499(6) 0.0084(4) 0.0135(5) 0.0001(4) O14 0.0308(5) 0.0284(5) 0.0509(7) 0.0019(5) 0.0107(5) 0.0008(4) 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' N N 0.0061 0.0033 '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 C2 S1 C11 102.17(6) C3 C2 C7 117.29(12) C3 C2 S1 119.50(10) C7 C2 S1 123.19(10) N4 C3 C2 118.57(11) N4 C3 C8 113.50(11) C2 C3 C8 127.88(12) C5 N4 C3 124.96(12) C5 N4 H4 117.5 C3 N4 H4 117.5 N4 C5 C6 118.58(13) N4 C5 H5 120.7 C6 C5 H5 120.7 C5 C6 C7 119.38(13) C5 C6 H6 120.3 C7 C6 H6 120.3 C6 C7 C2 121.21(12) C6 C7 H7 119.4 C2 C7 H7 119.4 O9 C8 O10 127.75(13) O9 C8 C3 115.77(12) O10 C8 C3 116.46(12) C12 C11 S1 106.45(9) C12 C11 H11A 110.4 S1 C11 H11A 110.4 C12 C11 H11B 110.4 S1 C11 H11B 110.4 H11A C11 H11B 108.6 O14 C12 O13 124.28(13) O14 C12 C11 122.71(12) O13 C12 C11 112.98(12) C12 O13 H13 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 C2 1.7563(13) S1 C11 1.8194(13) C2 C3 1.3989(17) C2 C7 1.4037(17) C3 N4 1.3448(16) C3 C8 1.5202(18) N4 C5 1.3293(18) N4 H4 0.8600 C5 C6 1.374(2) C5 H5 0.9300 C6 C7 1.3774(19) C6 H6 0.9300 C7 H7 0.9300 C8 O9 1.2333(18) C8 O10 1.2483(17) C11 C12 1.5200(18) C11 H11A 0.9700 C11 H11B 0.9700 C12 O14 1.2077(17) C12 O13 1.3124(16) O13 H13 0.89(2)