#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:45:36 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225902 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515777.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_4515777 loop_ _publ_author_name 'Struble, Thomas J.' 'Lankswert, Hannah M.' 'Pink, Maren' 'Johnston, Jeffrey N.' _publ_section_title ; Enantioselective Organocatalytic Amine-Isocyanate Capture-Cyclization: Regioselective Alkene Iodoamination for the Synthesis of Chiral Cyclic Ureas. ; _journal_issue 12 _journal_name_full 'ACS catalysis' _journal_page_first 11926 _journal_page_last 11931 _journal_paper_doi 10.1021/acscatal.8b03708 _journal_volume 8 _journal_year 2018 _chemical_absolute_configuration ad _chemical_formula_moiety 'C26 H25 I N2 O4 S' _chemical_formula_sum 'C26 H25 I N2 O4 S' _chemical_formula_weight 588.44 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 105.7165(15) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.8374(3) _cell_length_b 14.8665(6) _cell_length_c 12.6176(6) _cell_measurement_reflns_used 9817 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 30.05 _cell_measurement_theta_min 2.17 _cell_volume 1234.61(9) _computing_cell_refinement 'APEX II v2014.11-0 (Bruker, 2014)' _computing_data_collection 'APEX II v2014.11-0 (Bruker, 2014)' _computing_data_reduction 'APEX II v2014.11-0 (Bruker, 2014)' _computing_molecular_graphics 'SHELXTL (Bruker, 2013)' _computing_publication_material 'SHELXTL (Bruker, 2013)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELX (Bruker, 2014)' _diffrn_ambient_temperature 150(2) _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 83.33 _diffrn_detector_type 'Bruker APEXII' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_details '0.50 degree frames measured for 20 seconds each' _diffrn_measurement_device 'APEX Kappa Duo' _diffrn_measurement_device_type Kappa _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_unetI/netI 0.0281 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 25107 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.966 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.103 _diffrn_reflns_theta_min 2.165 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 1.417 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_correction_T_min 0.6371 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, G. Sheldrick; 2014' _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 1.583 _exptl_crystal_description block _exptl_crystal_F_000 592 _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.230 _refine_diff_density_max 0.655 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.051 _refine_ls_abs_structure_details ; Flack x determined using 3152 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.009(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 309 _refine_ls_number_reflns 7073 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.082 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0200 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+0.1906P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.0527 _reflns_Friedel_coverage 0.878 _reflns_Friedel_fraction_full 0.982 _reflns_Friedel_fraction_max 0.937 _reflns_number_gt 6970 _reflns_number_total 7073 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs8b03708_si_004.cif _cod_data_source_block 16052 _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 4515777 _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 0.660 _shelx_estimated_absorpt_t_max 0.736 _shelx_res_file ; 16052.res created by SHELXL-2014/7 TITL 16052 in P2(1) CELL 0.71073 6.8374 14.8665 12.61763 90.0000 105.7165 90.0000 ZERR 2.00 0.0003 0.0006 0.00058 0.0000 0.0015 0.0000 LATT -1 SYMM -x, y+1/2, -z SFAC C H N O S I UNIT 52 50 4 8 2 2 TEMP -123.140 SIZE 0.230 0.280 0.320 ACTA L.S. 10 FMAP 2 PLAN -5 0 0.00 LIST 4 HTAB EQIV $1 -x+2, y-1/2, -z+2 HTAB C3 O2_$1 EQIV $2 x+1, y, z HTAB C5 O1_$2 EQIV $3 -x+1, y-1/2, -z+2 HTAB C26 I1_$3 HTAB C26 O2_$3 HTAB C26 I1_$1 BOND $H CONF WPDB -1 WGHT 0.024100 0.190600 FVAR 0.21139 I1 6 1.288526 0.250517 1.089620 11.00000 0.03068 0.03994 = 0.02263 0.00224 0.00263 0.00196 S1 5 0.910357 0.439510 0.826213 11.00000 0.01809 0.01646 = 0.02366 0.00121 0.00219 -0.00018 O1 4 0.644599 0.302382 0.861327 11.00000 0.01441 0.02148 = 0.03051 0.00272 0.00585 0.00296 O2 4 0.846953 0.476828 0.915583 11.00000 0.03078 0.02357 = 0.02898 -0.00427 0.00601 0.00326 O3 4 1.088590 0.475279 0.801365 11.00000 0.02058 0.02299 = 0.03630 0.00613 0.00354 -0.00454 O4 4 0.224756 -0.062867 0.773542 11.00000 0.03531 0.03598 = 0.03622 -0.00675 0.00738 -0.01961 N1 3 0.966937 0.329845 0.850476 11.00000 0.01384 0.01558 = 0.02512 0.00238 0.00488 0.00151 N2 3 0.862221 0.183686 0.883606 11.00000 0.01242 0.01733 = 0.03148 0.00297 0.00485 0.00137 C1 1 1.168477 0.297696 0.843692 11.00000 0.01382 0.02156 = 0.02014 0.00280 0.00365 0.00147 AFIX 13 H1 2 1.270678 0.345923 0.873194 11.00000 -1.20000 AFIX 0 C2 1 0.814355 0.272815 0.865653 11.00000 0.01349 0.01868 = 0.02031 0.00112 0.00342 0.00107 C3 1 1.060983 0.144103 0.888046 11.00000 0.01515 0.01855 = 0.03094 0.00220 0.00576 0.00314 AFIX 23 H3A 2 1.057396 0.117379 0.815677 11.00000 -1.20000 H3B 2 1.091513 0.095539 0.943796 11.00000 -1.20000 AFIX 0 C4 1 1.225708 0.214785 0.917211 11.00000 0.01387 0.02277 = 0.02678 0.00317 0.00524 0.00257 AFIX 13 H4 2 1.352245 0.188506 0.904710 11.00000 -1.20000 AFIX 0 C5 1 1.179235 0.273977 0.729503 11.00000 0.02227 0.02632 = 0.02372 0.00213 0.00883 0.00274 AFIX 43 H5A 2 1.308507 0.277012 0.715179 11.00000 -1.20000 AFIX 0 C6 1 1.021657 0.249028 0.646797 11.00000 0.02131 0.02975 = 0.02601 0.00283 0.00687 -0.00180 AFIX 43 H6 2 0.892883 0.246856 0.661807 11.00000 -1.20000 AFIX 0 C7 1 1.027060 0.224563 0.534826 11.00000 0.03501 0.02721 = 0.02603 0.00151 0.00736 -0.00113 C8 1 1.206302 0.215533 0.504024 11.00000 0.04112 0.06188 = 0.02660 0.00189 0.00901 0.00866 AFIX 43 H8 2 1.332645 0.226844 0.556448 11.00000 -1.20000 AFIX 0 C9 1 1.203426 0.190049 0.397030 11.00000 0.05997 0.06046 = 0.03454 0.00284 0.02097 0.01445 AFIX 43 H9 2 1.327398 0.183084 0.377551 11.00000 -1.20000 AFIX 0 C10 1 1.020227 0.174948 0.319431 11.00000 0.07909 0.03507 = 0.02661 -0.00498 0.01782 -0.00987 AFIX 43 H10 2 1.017658 0.157935 0.246492 11.00000 -1.20000 AFIX 0 C11 1 0.842173 0.184765 0.348765 11.00000 0.06404 0.07086 = 0.02939 -0.01312 0.00236 -0.02573 AFIX 43 H11 2 0.715945 0.175011 0.295579 11.00000 -1.20000 AFIX 0 C12 1 0.844981 0.208926 0.455923 11.00000 0.04166 0.06523 = 0.02935 -0.00922 0.00519 -0.01484 AFIX 43 H12 2 0.720520 0.214756 0.475158 11.00000 -1.20000 AFIX 0 C13 1 0.705043 0.444446 0.706971 11.00000 0.01972 0.02216 = 0.02543 0.00616 0.00061 -0.00068 C14 1 0.738720 0.428128 0.604879 11.00000 0.02857 0.03300 = 0.02913 0.00622 0.00409 0.00110 AFIX 43 H14A 2 0.871644 0.415473 0.599116 11.00000 -1.20000 AFIX 0 C15 1 0.574889 0.430606 0.511304 11.00000 0.04297 0.04424 = 0.02543 0.01022 -0.00192 -0.00364 AFIX 43 H15 2 0.595491 0.416873 0.441585 11.00000 -1.20000 AFIX 0 C16 1 0.380014 0.453061 0.518425 11.00000 0.02987 0.04459 = 0.03920 0.01889 -0.00842 -0.00966 C17 1 0.353838 0.472286 0.621993 11.00000 0.01940 0.04857 = 0.04848 0.02283 0.00079 -0.00048 AFIX 43 H17 2 0.223267 0.489517 0.627678 11.00000 -1.20000 AFIX 0 C18 1 0.513294 0.466880 0.716609 11.00000 0.02340 0.03404 = 0.03625 0.01341 0.00424 0.00365 AFIX 43 H18 2 0.492095 0.478278 0.786752 11.00000 -1.20000 AFIX 0 C19 1 0.202424 0.455625 0.416814 11.00000 0.04208 0.07752 = 0.04929 0.02865 -0.01783 -0.01514 AFIX 137 H19A 2 0.250560 0.444400 0.351581 11.00000 -1.50000 H19B 2 0.137584 0.514900 0.410587 11.00000 -1.50000 H19C 2 0.103774 0.409240 0.422272 11.00000 -1.50000 AFIX 0 C20 1 0.695273 0.120978 0.860804 11.00000 0.01452 0.01688 = 0.02763 0.00053 0.00548 0.00042 C21 1 0.573015 0.113612 0.753805 11.00000 0.02413 0.02750 = 0.02422 0.00048 0.00743 -0.00303 AFIX 43 H21 2 0.598238 0.150810 0.697718 11.00000 -1.20000 AFIX 0 C22 1 0.415283 0.052781 0.728207 11.00000 0.02795 0.03031 = 0.02600 -0.00460 0.00634 -0.00604 AFIX 43 H22 2 0.329664 0.049302 0.655163 11.00000 -1.20000 AFIX 0 C23 1 0.381444 -0.003751 0.809775 11.00000 0.02096 0.02098 = 0.03143 -0.00591 0.00839 -0.00459 C24 1 0.501452 0.003345 0.917423 11.00000 0.02214 0.01971 = 0.02999 0.00287 0.00642 -0.00122 AFIX 43 H24 2 0.477132 -0.034409 0.973260 11.00000 -1.20000 AFIX 0 C25 1 0.658575 0.066645 0.942876 11.00000 0.01794 0.02039 = 0.02650 0.00372 0.00298 0.00007 AFIX 43 H25 2 0.740434 0.072492 1.016521 11.00000 -1.20000 AFIX 0 C26 1 0.166949 -0.118708 0.851805 11.00000 0.03440 0.03315 = 0.04658 -0.00494 0.01543 -0.01504 AFIX 137 H26B 2 0.053393 -0.157300 0.813776 11.00000 -1.50000 H26C 2 0.125239 -0.080986 0.905546 11.00000 -1.50000 H26D 2 0.282473 -0.156230 0.889897 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM 16052 in P2(1) REM R1 = 0.0200 for 6970 Fo > 4sig(Fo) and 0.0204 for all 7073 data REM 309 parameters refined using 1 restraints END WGHT 0.0231 0.2011 REM Instructions for potential hydrogen bonds HTAB C3 O2_$1 HTAB C5 O1_$2 HTAB C26 I1_$3 HTAB C26 O2_$3 HTAB C26 I1_$1 REM Highest difference peak 0.655, deepest hole -0.290, 1-sigma level 0.051 Q1 1 1.3193 0.2512 1.0412 11.00000 0.05 0.66 Q2 1 1.2655 0.2491 1.0253 11.00000 0.05 0.64 Q3 1 1.3192 0.2507 1.1466 11.00000 0.05 0.60 Q4 1 1.1997 0.2190 1.0758 11.00000 0.05 0.39 Q5 1 1.0869 0.2493 0.6979 11.00000 0.05 0.39 ; _shelx_res_checksum 43012 _shelx_hkl_file ; 1 0 -1 100.08 5.12 1 0 -1 113.91 5.04 1 0 -1 111.09 5.05 1 0 -1 98.65 5.11 -1 0 1 97.04 5.07 -1 0 1 105.10 5.12 2 0 -2 374.45 19.09 2 0 -2 404.60 18.70 2 0 -2 385.87 19.02 -2 0 2 367.42 19.08 -2 0 2 392.70 19.11 -2 0 2 402.93 18.68 3 0 -3 157.55 7.50 3 0 -3 165.76 7.69 3 0 -3 152.20 7.53 3 0 -3 159.51 7.48 3 0 -3 156.98 7.65 -3 0 3 152.51 7.65 -3 0 3 155.80 7.53 -3 0 3 154.17 7.68 4 0 -4 21.46 1.24 4 0 -4 20.91 1.27 4 0 -4 20.15 1.08 4 0 -4 20.76 1.04 -4 0 4 21.31 1.08 -4 0 4 20.31 1.24 5 0 -5 36.14 1.95 5 0 -5 38.71 2.17 5 0 -5 39.78 1.91 5 0 -5 41.52 2.24 -5 0 5 38.13 2.21 -5 0 5 39.30 2.18 -5 0 5 38.21 1.95 6 0 -6 3.33 0.33 -6 0 6 3.54 0.33 7 0 -7 11.92 0.77 -7 0 7 12.89 0.76 8 0 -8 38.11 2.06 -8 0 8 39.78 2.05 9 0 -9 0.12 0.23 -9 0 9 0.12 0.23 -9 1 9 10.82 0.76 9 -1 -9 9.40 0.74 -8 1 8 10.94 0.73 8 -1 -8 11.17 0.76 -7 1 7 3.13 0.34 7 -1 -7 3.48 0.37 -6 1 6 21.73 1.21 6 -1 -6 23.87 1.23 -5 1 5 5.42 0.39 -5 1 5 5.74 0.61 -5 1 5 5.50 0.58 5 -1 -5 5.65 0.57 5 -1 -5 5.42 0.40 5 -1 -5 5.91 0.63 5 -1 -5 5.91 0.29 5 -1 -5 5.56 0.35 -4 1 4 122.90 6.50 -4 1 4 131.45 6.69 4 -1 -4 138.64 6.48 4 -1 -4 137.44 6.69 4 -1 -4 133.45 6.52 4 -1 -4 139.73 6.72 4 -1 -4 141.80 6.45 -3 1 3 17.09 1.20 3 -1 -3 22.93 1.08 3 -1 -3 23.16 1.23 3 -1 -3 22.04 1.10 3 -1 -3 23.63 1.27 -2 1 2 37.43 1.93 -2 1 2 34.45 1.91 -2 1 2 41.35 1.84 2 -1 -2 37.65 1.82 2 -1 -2 37.46 1.84 2 -1 -2 37.01 1.93 2 -1 -2 37.63 1.92 2 -1 -2 38.92 1.83 -1 1 1 244.78 12.15 -1 1 1 254.09 12.14 1 -1 -1 252.38 11.86 1 -1 -1 236.15 12.07 1 -1 -1 255.14 11.89 1 -1 -1 240.05 11.84 0 -1 0 0.29 0.04 1 1 -1 256.99 12.47 1 1 -1 249.82 12.73 1 1 -1 262.51 12.80 -1 -1 1 264.63 12.45 -1 -1 1 254.90 12.76 -1 -1 1 267.61 12.49 2 1 -2 36.70 1.90 2 1 -2 37.88 1.79 2 1 -2 38.72 1.92 2 1 -2 37.69 1.81 -2 -1 2 36.93 1.91 -2 -1 2 34.89 1.89 3 1 -3 17.89 1.13 3 1 -3 18.29 0.96 3 1 -3 22.96 1.21 3 1 -3 18.28 0.99 4 1 -4 120.25 6.51 4 1 -4 130.55 6.50 4 1 -4 129.69 6.33 4 1 -4 128.84 6.29 -4 -1 4 140.76 6.55 -4 -1 4 129.22 6.50 -4 -1 4 138.19 6.32 5 1 -5 5.67 0.59 5 1 -5 5.60 0.35 5 1 -5 6.01 0.41 5 1 -5 5.93 0.62 -5 -1 5 5.99 0.60 -5 -1 5 5.74 0.40 -5 -1 5 5.67 0.62 6 1 -6 22.67 1.28 -6 -1 6 25.20 1.28 7 1 -7 3.04 0.36 -7 -1 7 3.19 0.36 8 1 -8 11.23 0.76 -8 -1 8 11.33 0.76 9 1 -9 9.36 0.72 -9 -1 9 9.78 0.71 9 -2 -9 4.24 0.48 -8 2 8 4.82 0.47 8 -2 -8 5.30 0.48 -7 2 7 31.44 1.59 7 -2 -7 28.21 1.59 -6 2 6 52.08 2.61 6 -2 -6 52.13 2.62 -5 2 5 134.35 6.91 -5 2 5 135.40 6.88 -5 2 5 129.92 6.64 5 -2 -5 137.40 6.65 5 -2 -5 143.81 6.61 5 -2 -5 138.93 6.90 5 -2 -5 139.60 6.56 5 -2 -5 139.25 6.86 -4 2 4 20.52 1.33 -4 2 4 21.66 1.14 4 -2 -4 22.80 1.07 4 -2 -4 23.18 1.11 4 -2 -4 22.60 1.34 4 -2 -4 22.44 1.14 4 -2 -4 21.90 1.30 -3 2 3 122.19 6.17 -3 2 3 127.33 6.20 -3 2 3 122.42 6.04 3 -2 -3 120.37 6.02 3 -2 -3 135.36 6.21 3 -2 -3 124.25 6.17 3 -2 -3 129.12 6.03 3 -2 -3 124.25 6.05 -2 2 2 199.30 10.05 -2 2 2 204.77 9.86 -2 2 2 205.43 10.07 2 -2 -2 191.25 9.82 2 -2 -2 206.83 9.93 2 -2 -2 210.78 9.90 2 -2 -2 216.85 9.88 2 -2 -2 208.55 10.09 1 -2 -1 50.56 2.47 1 -2 -1 51.66 2.53 1 -2 -1 50.48 2.47 1 -2 -1 52.83 2.48 0 2 0 269.24 12.57 0 2 0 264.13 12.50 0 -2 0 270.46 12.32 0 -2 0 228.12 12.44 0 -2 0 249.04 12.21 0 -2 0 251.30 12.21 1 2 -1 61.12 2.85 1 2 -1 61.84 2.79 1 2 -1 61.40 2.86 -1 -2 1 56.32 2.85 -1 -2 1 53.30 2.84 -1 -2 1 55.32 2.79 -1 -2 1 55.06 2.78 2 2 -2 188.32 9.86 2 2 -2 186.10 9.95 -2 -2 2 222.76 10.12 -2 -2 2 216.32 9.91 -2 -2 2 209.59 10.13 -2 -2 2 214.19 9.93 3 2 -3 124.24 6.10 3 2 -3 124.71 5.90 3 2 -3 125.45 6.07 3 2 -3 125.34 5.94 -3 -2 3 114.52 5.92 -3 -2 3 125.00 6.09 4 2 -4 21.37 1.14 4 2 -4 23.22 1.36 4 2 -4 22.47 1.37 4 2 -4 21.62 1.18 -4 -2 4 23.74 1.18 -4 -2 4 24.20 1.36 -4 -2 4 23.96 1.39 5 2 -5 125.62 6.83 5 2 -5 140.83 6.90 5 2 -5 129.30 6.62 -5 -2 5 144.55 6.86 -5 -2 5 138.38 6.61 -5 -2 5 141.24 6.90 6 2 -6 50.33 2.63 -6 -2 6 54.06 2.62 7 2 -7 29.77 1.58 -7 -2 7 28.80 1.56 8 2 -8 5.01 0.49 -8 -2 8 4.89 0.48 9 2 -9 4.79 0.51 -9 -2 9 4.81 0.50 9 -3 -9 5.69 0.54 -8 3 8 1.74 0.31 8 -3 -8 2.05 0.33 -7 3 7 28.71 1.48 7 -3 -7 26.28 1.47 -6 3 6 20.63 1.10 6 -3 -6 19.97 1.11 -5 3 5 7.00 0.70 -5 3 5 6.16 0.44 -5 3 5 6.77 0.65 5 -3 -5 7.12 0.35 5 -3 -5 5.79 0.44 5 -3 -5 7.01 0.65 5 -3 -5 6.60 0.40 -4 3 4 228.95 10.88 -4 3 4 235.03 11.07 -4 3 4 217.15 11.08 4 -3 -4 242.12 11.10 4 -3 -4 218.29 10.85 4 -3 -4 218.52 10.88 4 -3 -4 226.93 11.04 -3 3 3 116.88 5.76 -3 3 3 117.13 5.59 -3 3 3 113.33 5.72 3 -3 -3 116.90 5.57 3 -3 -3 112.36 5.59 3 -3 -3 122.76 5.76 3 -3 -3 118.20 5.72 3 -3 -3 111.61 5.57 -2 3 2 75.57 3.25 -2 3 2 72.00 3.35 -2 3 2 74.02 3.25 -2 3 2 73.68 3.37 2 -3 -2 61.67 3.23 2 -3 -2 61.48 3.22 2 -3 -2 60.57 3.24 2 -3 -2 58.73 3.32 -1 3 1 712.10 33.62 1 -3 -1 684.98 33.09 1 -3 -1 719.58 33.59 1 -3 -1 658.87 33.62 1 -3 -1 686.20 33.16 0 3 0 -0.27 0.11 0 3 0 -0.45 0.09 0 -3 0 -0.32 0.04 0 -3 0 -0.37 0.09 0 -3 0 -0.44 0.04 0 -3 0 -0.42 0.10 0 -3 0 -0.32 0.06 1 3 -1 591.88 33.13 1 3 -1 729.10 33.25 1 3 -1 704.17 32.75 -1 -3 1 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19.61 1.14 -4 -8 5 22.73 1.03 -4 -8 5 22.31 1.45 -4 -8 5 20.94 1.13 5 8 -6 58.24 2.81 -5 -8 6 53.00 2.78 6 8 -7 15.42 0.93 7 8 -8 1.78 0.31 -7 -8 8 1.29 0.27 8 8 -9 15.82 1.02 -8 -8 9 15.69 0.99 8 -9 -7 2.23 0.35 7 -9 -6 0.18 0.20 7 -9 -6 0.16 0.12 -6 9 5 20.35 1.09 6 -9 -5 18.83 1.07 6 -9 -5 18.25 0.97 -5 9 4 15.59 0.86 -5 9 4 13.83 1.17 -5 9 4 15.13 0.86 5 -9 -4 15.18 0.86 -4 9 3 89.25 4.66 -4 9 3 94.53 4.36 -4 9 3 90.63 4.61 4 -9 -3 82.13 4.34 4 -9 -3 88.05 4.31 -3 9 2 89.60 4.67 -3 9 2 95.88 4.46 3 -9 -2 89.69 4.64 3 -9 -2 91.96 4.42 3 -9 -2 89.44 4.46 3 -9 -2 92.37 4.42 -2 9 1 14.45 0.99 -2 9 1 15.69 0.82 2 -9 -1 15.55 0.78 2 -9 -1 15.51 0.74 2 -9 -1 15.13 0.78 2 -9 -1 14.98 0.97 2 -9 -1 14.52 0.81 -1 9 0 192.63 10.21 -1 9 0 210.36 10.30 -1 9 0 204.90 10.05 1 -9 0 218.21 10.01 1 -9 0 220.68 10.27 1 -9 0 212.65 10.04 1 -9 0 212.81 10.00 1 -9 0 199.43 10.19 0 9 -1 35.33 1.88 0 9 -1 36.67 1.85 0 9 -1 37.39 1.64 0 -9 1 30.52 1.79 0 -9 1 29.63 1.77 0 -9 1 29.36 1.57 0 -9 1 30.87 1.58 0 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136.22 6.56 -2 3 -6 101.42 4.80 -2 3 -6 95.60 4.81 -2 3 -6 100.81 4.79 2 -3 6 101.13 4.82 2 -3 6 99.00 4.99 -1 3 -7 23.98 1.25 -1 3 -7 25.60 1.22 -1 3 -7 24.06 1.23 -1 3 -7 24.63 1.22 1 -3 7 25.67 1.43 1 -3 7 24.36 1.25 0 3 -8 87.12 4.16 0 3 -8 85.86 4.16 0 3 -8 88.88 4.18 0 3 -8 87.83 4.19 0 -3 8 85.22 4.39 0 -3 8 79.51 4.35 0 -3 8 90.66 4.23 1 3 -9 16.66 0.83 1 3 -9 16.03 0.85 1 3 -9 16.67 0.87 1 3 -9 16.70 0.83 -1 -3 9 15.47 1.06 -1 -3 9 15.98 1.04 -1 -3 9 16.89 0.87 2 3 -10 72.00 3.50 2 3 -10 69.84 3.54 2 3 -10 73.71 3.53 2 3 -10 77.04 3.51 -2 -3 10 73.07 3.78 -2 -3 10 68.39 3.75 3 3 -11 13.57 0.77 3 3 -11 14.63 0.82 -3 -3 11 15.07 1.08 -3 -3 11 15.36 1.08 4 3 -12 6.95 0.50 4 3 -12 7.66 0.46 -4 -3 12 7.77 0.81 5 3 -13 24.07 1.31 6 3 -14 0.06 0.18 -9 4 1 8.26 0.65 9 -4 -1 9.83 0.72 -8 4 0 1.49 0.28 8 -4 0 1.39 0.31 -7 4 -1 12.44 0.80 7 -4 1 14.17 0.84 -6 4 -2 29.02 1.68 6 -4 2 36.38 1.72 -5 4 -3 4.81 0.39 5 -4 3 5.52 0.42 5 -4 3 6.06 0.64 -4 4 -4 104.07 5.16 -4 4 -4 107.07 5.13 -4 4 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18.75 1.09 1 -1 15 19.30 1.34 1 -1 15 20.18 1.32 0 1 -16 4.34 0.32 0 1 -16 4.76 0.40 0 1 -16 4.30 0.32 0 -1 16 5.43 0.65 0 -1 16 4.63 0.60 1 1 -17 31.14 1.55 1 1 -17 28.44 1.60 -1 -1 17 31.20 2.02 -1 -1 17 30.85 1.88 -6 2 -10 12.06 0.72 -5 2 -11 8.64 0.53 -5 2 -11 8.27 0.53 -4 2 -12 4.04 0.31 -4 2 -12 4.16 0.32 4 -2 12 4.46 0.62 -3 2 -13 40.27 2.14 -3 2 -13 41.68 2.07 -3 2 -13 45.30 2.10 3 -2 13 40.86 2.44 -2 2 -14 8.11 0.42 -2 2 -14 7.60 0.52 -2 2 -14 7.75 0.45 2 -2 14 6.73 0.73 2 -2 14 6.02 0.75 -1 2 -15 2.98 0.25 -1 2 -15 3.29 0.32 1 -2 15 2.68 0.51 1 -2 15 3.08 0.56 0 2 -16 23.79 1.19 0 2 -16 23.65 1.25 0 -2 16 22.96 1.53 0 -2 16 21.59 1.54 1 2 -17 0.91 0.24 1 2 -17 0.92 0.17 -1 -2 17 1.14 0.37 -6 3 -10 4.08 0.37 -5 3 -11 7.01 0.48 -5 3 -11 6.99 0.47 -4 3 -12 13.42 0.76 -4 3 -12 15.01 0.76 4 -3 12 12.00 1.08 -3 3 -13 0.38 0.13 -3 3 -13 0.13 0.12 -3 3 -13 0.12 0.18 3 -3 13 0.39 0.29 -2 3 -14 25.77 1.29 -2 3 -14 26.42 1.36 -2 3 -14 26.16 1.30 -2 3 -14 25.77 1.31 2 -3 14 23.31 1.63 -1 3 -15 35.94 1.75 -1 3 -15 32.99 1.79 -1 3 -15 36.82 1.73 1 -3 15 33.21 2.09 0 3 -16 3.14 0.33 0 3 -16 3.35 0.26 0 3 -16 2.93 0.28 0 -3 16 3.29 0.58 1 3 -17 12.47 0.70 1 3 -17 12.62 0.67 1 3 -17 11.06 0.74 -1 -3 17 12.44 1.05 -5 4 -11 26.31 1.39 -4 4 -12 1.75 0.24 -4 4 -12 2.03 0.25 4 -4 12 1.53 0.47 -3 4 -13 19.60 1.06 -3 4 -13 20.18 1.06 -3 4 -13 21.16 1.06 -3 4 -13 20.05 1.09 3 -4 13 18.59 1.42 -2 4 -14 8.38 0.55 -2 4 -14 8.06 0.50 -2 4 -14 9.00 0.51 2 -4 14 7.08 0.81 -1 4 -15 10.82 0.66 -1 4 -15 10.78 0.62 -1 4 -15 10.52 0.62 1 -4 15 11.19 0.98 0 4 -16 20.86 1.16 0 4 -16 21.62 1.14 0 4 -16 22.00 1.12 0 -4 16 21.38 1.51 1 4 -17 0.64 0.16 1 4 -17 0.68 0.22 1 4 -17 0.44 0.15 -1 -4 17 0.53 0.32 -5 5 -11 1.42 0.24 -4 5 -12 8.48 0.53 -4 5 -12 7.36 0.52 -3 5 -13 2.22 0.26 -3 5 -13 2.23 0.26 -3 5 -13 2.30 0.31 -3 5 -13 2.03 0.26 3 -5 13 2.23 0.56 -2 5 -14 5.47 0.42 -2 5 -14 5.17 0.39 -2 5 -14 5.48 0.38 2 -5 14 5.24 0.74 -1 5 -15 6.40 0.42 -1 5 -15 6.37 0.44 -1 5 -15 6.39 0.42 1 -5 15 4.80 0.71 0 5 -16 6.22 0.44 0 5 -16 6.46 0.45 0 5 -16 6.51 0.47 0 -5 16 7.38 0.82 1 5 -17 21.16 1.12 1 5 -17 20.75 1.11 1 5 -17 19.98 1.13 -5 6 -11 22.09 1.22 -4 6 -12 4.44 0.39 -4 6 -12 4.43 0.38 -3 6 -13 12.57 0.75 -3 6 -13 9.91 0.66 -2 6 -14 3.33 0.33 -2 6 -14 3.71 0.34 -2 6 -14 3.59 0.32 -1 6 -15 7.25 0.47 -1 6 -15 6.41 0.47 -1 6 -15 7.26 0.48 0 6 -16 13.70 0.79 0 6 -16 13.47 0.78 0 6 -16 13.47 0.78 -4 7 -12 23.60 1.28 -4 7 -12 23.15 1.28 -3 7 -13 0.99 0.22 -2 7 -14 24.98 1.34 -1 7 -15 19.08 1.03 -1 7 -15 18.64 1.05 0 7 -16 2.38 0.30 0 7 -16 1.98 0.28 -4 8 -12 2.99 0.35 -3 8 -13 11.64 0.73 -2 8 -14 6.11 0.47 -1 8 -15 8.34 0.57 -2 9 -14 14.37 0.87 -2 -6 -15 8.06 0.58 -4 -5 -13 26.34 1.28 -4 -5 -13 24.77 1.27 4 5 13 24.49 1.59 -3 -5 -14 12.71 0.80 -3 -5 -14 12.56 0.65 -3 -5 -14 14.18 0.66 3 5 14 10.00 1.12 -2 -5 -15 3.03 0.36 -1 -5 -16 14.92 0.89 -4 -4 -13 6.78 0.40 -4 -4 -13 6.52 0.38 4 4 13 5.11 0.65 -3 -4 -14 3.99 0.26 -3 -4 -14 4.07 0.41 -3 -4 -14 4.04 0.27 -2 -4 -15 19.40 1.00 -2 -4 -15 21.25 1.01 -2 -4 -15 19.88 1.14 -1 -4 -16 1.16 0.13 -1 -4 -16 0.99 0.25 -1 -4 -16 1.06 0.13 -4 -3 -13 9.20 0.51 -4 -3 -13 8.86 0.50 4 3 13 8.07 0.90 4 3 13 8.45 0.81 -3 -3 -14 2.24 0.19 -3 -3 -14 1.90 0.32 -3 -3 -14 1.83 0.18 3 3 14 1.68 0.38 3 3 14 1.22 0.34 -2 -3 -15 7.10 0.53 -2 -3 -15 7.27 0.40 -2 -3 -15 6.94 0.40 -1 -3 -16 19.58 1.19 -1 -3 -16 23.30 1.08 -1 -3 -16 22.18 1.08 1 3 16 21.00 1.29 -5 -2 -12 12.71 0.69 5 2 12 11.79 1.01 -4 -2 -13 5.67 0.36 -4 -2 -13 5.93 0.42 4 2 13 5.79 0.62 4 2 13 4.79 0.65 -3 -2 -14 19.09 0.98 -3 -2 -14 18.27 1.07 -3 -2 -14 20.24 0.97 3 2 14 17.36 1.20 3 2 14 19.16 1.29 -2 -2 -15 15.61 0.91 -2 -2 -15 16.06 0.81 -2 -2 -15 15.46 0.80 2 2 15 15.13 1.03 2 2 15 14.74 1.06 -1 -2 -16 3.74 0.26 -1 -2 -16 3.45 0.36 -1 -2 -16 3.57 0.26 1 2 16 4.57 0.52 0 -2 -17 22.43 1.07 0 -2 -17 19.78 1.16 0 -2 -17 20.85 1.07 0 2 17 20.44 1.39 -5 -1 -12 5.42 0.37 5 1 12 4.78 0.66 -4 -1 -13 16.02 0.87 4 1 13 16.59 1.17 4 1 13 16.62 1.23 -3 -1 -14 10.05 0.55 -3 -1 -14 9.12 0.63 -3 -1 -14 11.02 0.56 3 1 14 8.16 0.84 3 1 14 9.59 0.80 -2 -1 -15 4.31 0.41 -2 -1 -15 4.61 0.30 -2 -1 -15 4.26 0.30 2 1 15 4.90 0.59 2 1 15 4.11 0.52 -1 -1 -16 16.61 0.98 -1 -1 -16 17.33 0.89 -1 -1 -16 18.59 0.90 1 1 16 16.58 1.19 1 1 16 16.80 1.16 0 -1 -17 1.91 0.30 0 -1 -17 1.75 0.19 0 -1 -17 2.00 0.20 0 1 17 1.21 0.34 -5 0 -12 10.19 0.59 -5 0 -12 9.70 0.54 5 0 12 9.19 0.90 -4 0 -13 0.51 0.14 4 0 13 0.28 0.27 -3 0 -14 1.63 0.20 -3 0 -14 1.82 0.30 3 0 14 1.82 0.41 3 0 14 2.13 0.52 -2 0 -15 17.44 0.92 -2 0 -15 18.61 0.93 -2 0 -15 17.05 1.00 2 0 15 16.82 1.23 2 0 15 17.83 1.21 -1 0 -16 0.91 0.15 -1 0 -16 1.27 0.26 -1 0 -16 1.10 0.15 1 0 16 1.51 0.39 1 0 16 0.93 0.32 0 0 -17 14.24 0.74 0 0 -17 13.28 0.73 0 0 -17 12.82 0.80 0 0 17 13.13 1.02 -5 1 -12 4.85 0.37 -5 1 -12 4.96 0.34 5 -1 12 4.89 0.69 -4 1 -13 17.08 0.86 -4 1 -13 17.30 0.91 4 -1 13 16.08 1.24 -3 1 -14 9.37 0.65 -3 1 -14 10.76 0.58 3 -1 14 9.90 0.88 -2 1 -15 4.50 0.41 -2 1 -15 4.28 0.32 2 -1 15 4.53 0.60 2 -1 15 5.36 0.66 -1 1 -16 17.35 0.98 -1 1 -16 17.72 0.91 1 -1 16 16.44 1.23 1 -1 16 17.32 1.22 0 1 -17 1.59 0.27 0 1 -17 1.47 0.20 0 -1 17 1.22 0.38 0 -1 17 1.33 0.47 -5 2 -12 12.70 0.73 -5 2 -12 13.93 0.76 5 -2 12 12.79 1.49 -4 2 -13 6.75 0.41 -4 2 -13 7.07 0.45 4 -2 13 5.85 0.73 -3 2 -14 18.28 0.99 -3 2 -14 18.58 0.95 -3 2 -14 19.12 1.06 3 -2 14 19.14 1.35 -2 2 -15 17.34 0.89 -2 2 -15 15.93 0.95 2 -2 15 16.10 1.22 -1 2 -16 4.07 0.38 -1 2 -16 4.19 0.32 1 -2 16 4.24 0.62 0 2 -17 21.72 1.13 0 2 -17 21.49 1.19 0 -2 17 21.48 1.49 -4 3 -13 7.67 0.50 -4 3 -13 8.23 0.52 4 -3 13 8.98 0.89 -3 3 -14 2.07 0.22 -3 3 -14 1.69 0.30 -3 3 -14 1.97 0.24 3 -3 14 1.83 0.45 -2 3 -15 8.16 0.50 -2 3 -15 8.05 0.47 -2 3 -15 8.34 0.56 2 -3 15 7.95 0.83 -1 3 -16 22.39 1.20 -1 3 -16 21.99 1.15 1 -3 16 21.32 1.50 -4 4 -13 7.53 0.49 -4 4 -13 7.41 0.50 -3 4 -14 5.03 0.43 -3 4 -14 5.26 0.38 -3 4 -14 5.33 0.36 3 -4 14 4.06 0.67 -2 4 -15 20.78 1.09 -2 4 -15 20.40 1.07 -2 4 -15 19.39 1.12 -2 4 -15 20.77 1.07 2 -4 15 20.76 1.48 -1 4 -16 1.15 0.19 -1 4 -16 1.79 0.27 -1 4 -16 1.35 0.20 1 -4 16 1.10 0.41 -4 5 -13 25.75 1.36 -3 5 -14 14.81 0.82 -3 5 -14 14.74 0.81 -3 5 -14 14.54 0.82 -3 5 -14 13.50 0.84 -2 5 -15 2.94 0.32 -2 5 -15 2.50 0.27 -2 5 -15 2.52 0.28 2 -5 15 3.25 0.66 -1 5 -16 18.56 0.98 -1 5 -16 18.88 1.02 -1 5 -16 18.63 0.99 1 -5 16 16.64 1.41 -3 6 -14 8.79 0.57 -3 6 -14 8.63 0.56 -2 6 -15 8.29 0.53 -2 6 -15 7.93 0.54 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 65726 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp I1 I 1.28853(2) 0.25052(2) 1.08962(2) 0.03198(5) Uani 1 1 d . . S1 S 0.91036(8) 0.43951(4) 0.82621(4) 0.02008(10) Uani 1 1 d . . O1 O 0.6446(2) 0.30238(11) 0.86133(14) 0.0222(3) Uani 1 1 d . . O2 O 0.8470(3) 0.47683(12) 0.91558(15) 0.0282(4) Uani 1 1 d . . O3 O 1.0886(3) 0.47528(12) 0.80136(16) 0.0274(4) Uani 1 1 d . . O4 O 0.2248(3) -0.06287(15) 0.77354(17) 0.0363(4) Uani 1 1 d . . N1 N 0.9669(3) 0.32985(12) 0.85048(16) 0.0183(3) Uani 1 1 d . . N2 N 0.8622(3) 0.18369(13) 0.88361(17) 0.0206(3) Uani 1 1 d . . C1 C 1.1685(3) 0.29770(15) 0.84369(17) 0.0187(4) Uani 1 1 d . . H1 H 1.2707 0.3459 0.8732 0.022 Uiso 1 1 calc R U C2 C 0.8144(3) 0.27281(13) 0.86565(17) 0.0177(4) Uani 1 1 d . . C3 C 1.0610(3) 0.14410(15) 0.8880(2) 0.0216(4) Uani 1 1 d . . H3A H 1.0574 0.1174 0.8157 0.026 Uiso 1 1 calc R U H3B H 1.0915 0.0955 0.9438 0.026 Uiso 1 1 calc R U C4 C 1.2257(3) 0.21479(18) 0.91721(18) 0.0212(4) Uani 1 1 d . . H4 H 1.3522 0.1885 0.9047 0.025 Uiso 1 1 calc R U C5 C 1.1792(4) 0.27398(15) 0.72950(19) 0.0236(5) Uani 1 1 d . . H5A H 1.3085 0.2770 0.7152 0.028 Uiso 1 1 calc R U C6 C 1.0217(3) 0.2490(2) 0.64680(16) 0.0256(4) Uani 1 1 d . . H6 H 0.8929 0.2469 0.6618 0.031 Uiso 1 1 calc R U C7 C 1.0271(4) 0.22456(17) 0.5348(2) 0.0296(5) Uani 1 1 d . . C8 C 1.2063(5) 0.2155(2) 0.5040(2) 0.0432(7) Uani 1 1 d . . H8 H 1.3326 0.2268 0.5564 0.052 Uiso 1 1 calc R U C9 C 1.2034(6) 0.1900(3) 0.3970(3) 0.0501(9) Uani 1 1 d . . H9 H 1.3274 0.1831 0.3776 0.060 Uiso 1 1 calc R U C10 C 1.0202(6) 0.1749(2) 0.3194(2) 0.0462(8) Uani 1 1 d . . H10 H 1.0177 0.1579 0.2465 0.055 Uiso 1 1 calc R U C11 C 0.8422(7) 0.1848(3) 0.3488(3) 0.0568(10) Uani 1 1 d . . H11 H 0.7159 0.1750 0.2956 0.068 Uiso 1 1 calc R U C12 C 0.8450(5) 0.2089(3) 0.4559(3) 0.0463(8) Uani 1 1 d . . H12 H 0.7205 0.2148 0.4752 0.056 Uiso 1 1 calc R U C13 C 0.7050(4) 0.44445(16) 0.70697(19) 0.0235(4) Uani 1 1 d . . C14 C 0.7387(4) 0.42813(19) 0.6049(2) 0.0310(5) Uani 1 1 d . . H14A H 0.8716 0.4155 0.5991 0.037 Uiso 1 1 calc R U C15 C 0.5749(5) 0.4306(2) 0.5113(2) 0.0397(7) Uani 1 1 d . . H15 H 0.5955 0.4169 0.4416 0.048 Uiso 1 1 calc R U C16 C 0.3800(5) 0.4531(2) 0.5184(3) 0.0414(7) Uani 1 1 d . . C17 C 0.3538(4) 0.4723(2) 0.6220(3) 0.0405(7) Uani 1 1 d . . H17 H 0.2233 0.4895 0.6277 0.049 Uiso 1 1 calc R U C18 C 0.5133(4) 0.46688(19) 0.7166(2) 0.0320(5) Uani 1 1 d . . H18 H 0.4921 0.4783 0.7868 0.038 Uiso 1 1 calc R U C19 C 0.2024(5) 0.4556(4) 0.4168(3) 0.0622(13) Uani 1 1 d . . H19A H 0.2506 0.4444 0.3516 0.093 Uiso 1 1 calc R U H19B H 0.1376 0.5149 0.4106 0.093 Uiso 1 1 calc R U H19C H 0.1038 0.4092 0.4223 0.093 Uiso 1 1 calc R U C20 C 0.6953(3) 0.12098(14) 0.86080(19) 0.0197(4) Uani 1 1 d . . C21 C 0.5730(4) 0.11361(17) 0.75380(19) 0.0251(4) Uani 1 1 d . . H21 H 0.5982 0.1508 0.6977 0.030 Uiso 1 1 calc R U C22 C 0.4153(4) 0.05278(18) 0.7282(2) 0.0283(5) Uani 1 1 d . . H22 H 0.3297 0.0493 0.6552 0.034 Uiso 1 1 calc R U C23 C 0.3814(4) -0.00375(16) 0.8098(2) 0.0242(4) Uani 1 1 d . . C24 C 0.5015(4) 0.00334(16) 0.9174(2) 0.0241(4) Uani 1 1 d . . H24 H 0.4771 -0.0344 0.9733 0.029 Uiso 1 1 calc R U C25 C 0.6586(3) 0.06665(15) 0.94288(19) 0.0222(4) Uani 1 1 d . . H25 H 0.7404 0.0725 1.0165 0.027 Uiso 1 1 calc R U C26 C 0.1669(5) -0.1187(2) 0.8518(3) 0.0372(6) Uani 1 1 d . . H26B H 0.0534 -0.1573 0.8138 0.056 Uiso 1 1 calc R U H26C H 0.1252 -0.0810 0.9055 0.056 Uiso 1 1 calc R U H26D H 0.2825 -0.1562 0.8899 0.056 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.03068(8) 0.03994(9) 0.02263(6) 0.00224(7) 0.00263(5) 0.00196(8) S1 0.0181(2) 0.0165(2) 0.0237(2) 0.00121(17) 0.00219(18) -0.00018(18) O1 0.0144(7) 0.0215(7) 0.0305(8) 0.0027(6) 0.0059(6) 0.0030(6) O2 0.0308(9) 0.0236(8) 0.0290(8) -0.0043(7) 0.0060(7) 0.0033(7) O3 0.0206(8) 0.0230(8) 0.0363(9) 0.0061(7) 0.0035(7) -0.0045(6) O4 0.0353(11) 0.0360(10) 0.0362(10) -0.0067(8) 0.0074(8) -0.0196(9) N1 0.0138(8) 0.0156(8) 0.0251(8) 0.0024(6) 0.0049(7) 0.0015(6) N2 0.0124(8) 0.0173(8) 0.0315(9) 0.0030(7) 0.0049(7) 0.0014(7) C1 0.0138(9) 0.0216(10) 0.0201(9) 0.0028(7) 0.0036(7) 0.0015(7) C2 0.0135(9) 0.0187(10) 0.0203(8) 0.0011(6) 0.0034(7) 0.0011(7) C3 0.0152(10) 0.0186(9) 0.0309(11) 0.0022(8) 0.0058(8) 0.0031(8) C4 0.0139(10) 0.0228(9) 0.0268(11) 0.0032(8) 0.0052(8) 0.0026(7) C5 0.0223(10) 0.0263(12) 0.0237(9) 0.0021(7) 0.0088(8) 0.0027(8) C6 0.0213(9) 0.0297(9) 0.0260(8) 0.0028(13) 0.0069(7) -0.0018(13) C7 0.0350(14) 0.0272(12) 0.0260(10) 0.0015(8) 0.0074(10) -0.0011(9) C8 0.0411(17) 0.0619(19) 0.0266(12) 0.0019(12) 0.0090(11) 0.0087(14) C9 0.060(2) 0.060(2) 0.0345(14) 0.0028(14) 0.0210(15) 0.0144(17) C10 0.079(3) 0.0351(15) 0.0266(12) -0.0050(11) 0.0178(14) -0.0099(15) C11 0.064(2) 0.071(2) 0.0294(14) -0.0131(15) 0.0024(14) -0.026(2) C12 0.0417(17) 0.065(2) 0.0293(13) -0.0092(13) 0.0052(12) -0.0148(15) C13 0.0197(10) 0.0222(10) 0.0254(10) 0.0062(8) 0.0006(8) -0.0007(8) C14 0.0286(12) 0.0330(13) 0.0291(11) 0.0062(10) 0.0041(10) 0.0011(10) C15 0.0430(16) 0.0442(16) 0.0254(12) 0.0102(11) -0.0019(11) -0.0036(13) C16 0.0299(14) 0.0446(16) 0.0392(14) 0.0189(12) -0.0084(11) -0.0097(12) C17 0.0194(12) 0.0486(17) 0.0485(16) 0.0228(14) 0.0008(11) -0.0005(11) C18 0.0234(12) 0.0340(13) 0.0362(13) 0.0134(10) 0.0042(10) 0.0036(10) C19 0.042(2) 0.078(3) 0.049(2) 0.0287(18) -0.0178(16) -0.0151(17) C20 0.0145(9) 0.0169(9) 0.0276(10) 0.0005(7) 0.0055(8) 0.0004(7) C21 0.0241(11) 0.0275(11) 0.0242(10) 0.0005(8) 0.0074(9) -0.0030(9) C22 0.0279(13) 0.0303(12) 0.0260(10) -0.0046(9) 0.0063(9) -0.0060(10) C23 0.0210(10) 0.0210(10) 0.0314(11) -0.0059(8) 0.0084(8) -0.0046(8) C24 0.0221(11) 0.0197(9) 0.0300(11) 0.0029(8) 0.0064(9) -0.0012(8) C25 0.0179(10) 0.0204(10) 0.0265(10) 0.0037(8) 0.0030(8) 0.0001(8) C26 0.0344(15) 0.0332(13) 0.0466(15) -0.0049(11) 0.0154(12) -0.0150(12) 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' I I -0.4742 1.8119 '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 O2 S1 O3 119.03(12) O2 S1 N1 109.69(10) O3 S1 N1 103.34(10) O2 S1 C13 108.48(12) O3 S1 C13 108.95(11) N1 S1 C13 106.65(11) C23 O4 C26 118.9(2) C2 N1 C1 123.53(18) C2 N1 S1 117.97(14) C1 N1 S1 118.22(15) C2 N2 C20 116.88(18) C2 N2 C3 124.87(19) C20 N2 C3 115.04(18) N1 C1 C5 114.72(18) N1 C1 C4 108.30(17) C5 C1 C4 108.74(18) N1 C1 H1 108.3 C5 C1 H1 108.3 C4 C1 H1 108.3 O1 C2 N2 122.3(2) O1 C2 N1 120.56(18) N2 C2 N1 117.14(19) N2 C3 C4 110.59(18) N2 C3 H3A 109.5 C4 C3 H3A 109.5 N2 C3 H3B 109.5 C4 C3 H3B 109.5 H3A C3 H3B 108.1 C3 C4 C1 111.20(18) C3 C4 I1 110.30(15) C1 C4 I1 111.11(16) C3 C4 H4 108.0 C1 C4 H4 108.0 I1 C4 H4 108.0 C6 C5 C1 125.2(2) C6 C5 H5A 117.4 C1 C5 H5A 117.4 C5 C6 C7 126.6(2) C5 C6 H6 116.7 C7 C6 H6 116.7 C12 C7 C8 118.1(3) C12 C7 C6 118.7(3) C8 C7 C6 123.2(2) C7 C8 C9 120.9(3) C7 C8 H8 119.5 C9 C8 H8 119.5 C10 C9 C8 120.1(3) C10 C9 H9 120.0 C8 C9 H9 120.0 C11 C10 C9 119.4(3) C11 C10 H10 120.3 C9 C10 H10 120.3 C10 C11 C12 120.6(3) C10 C11 H11 119.7 C12 C11 H11 119.7 C7 C12 C11 120.9(3) C7 C12 H12 119.6 C11 C12 H12 119.6 C18 C13 C14 121.3(2) C18 C13 S1 119.23(19) C14 C13 S1 119.42(19) C13 C14 C15 119.0(3) C13 C14 H14A 120.5 C15 C14 H14A 120.5 C14 C15 C16 120.9(3) C14 C15 H15 119.5 C16 C15 H15 119.5 C17 C16 C15 118.3(2) C17 C16 C19 120.8(3) C15 C16 C19 120.8(3) C18 C17 C16 121.7(3) C18 C17 H17 119.2 C16 C17 H17 119.2 C17 C18 C13 118.7(3) C17 C18 H18 120.7 C13 C18 H18 120.7 C16 C19 H19A 109.5 C16 C19 H19B 109.5 H19A C19 H19B 109.5 C16 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C21 C20 C25 119.8(2) C21 C20 N2 118.8(2) C25 C20 N2 121.4(2) C22 C21 C20 120.5(2) C22 C21 H21 119.7 C20 C21 H21 119.7 C21 C22 C23 119.9(2) C21 C22 H22 120.1 C23 C22 H22 120.1 O4 C23 C24 125.4(2) O4 C23 C22 114.4(2) C24 C23 C22 120.3(2) C23 C24 C25 119.3(2) C23 C24 H24 120.3 C25 C24 H24 120.3 C20 C25 C24 120.2(2) C20 C25 H25 119.9 C24 C25 H25 119.9 O4 C26 H26B 109.5 O4 C26 H26C 109.5 H26B C26 H26C 109.5 O4 C26 H26D 109.5 H26B C26 H26D 109.5 H26C C26 H26D 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance I1 C4 2.166(2) S1 O2 1.4255(19) S1 O3 1.4399(19) S1 N1 1.6844(19) S1 C13 1.759(2) O1 C2 1.228(3) O4 C23 1.365(3) O4 C26 1.425(4) N1 C2 1.397(3) N1 C1 1.483(3) N2 C2 1.369(3) N2 C20 1.441(3) N2 C3 1.468(3) C1 C5 1.504(3) C1 C4 1.528(3) C1 H1 1.0000 C3 C4 1.511(3) C3 H3A 0.9900 C3 H3B 0.9900 C4 H4 1.0000 C5 C6 1.334(3) C5 H5A 0.9500 C6 C7 1.469(3) C6 H6 0.9500 C7 C12 1.387(4) C7 C8 1.389(4) C8 C9 1.397(4) C8 H8 0.9500 C9 C10 1.383(5) C9 H9 0.9500 C10 C11 1.373(6) C10 H10 0.9500 C11 C12 1.394(4) C11 H11 0.9500 C12 H12 0.9500 C13 C18 1.390(4) C13 C14 1.390(4) C14 C15 1.391(4) C14 H14A 0.9500 C15 C16 1.400(5) C15 H15 0.9500 C16 C17 1.396(5) C16 C19 1.509(4) C17 C18 1.384(4) C17 H17 0.9500 C18 H18 0.9500 C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 C21 1.386(3) C20 C25 1.389(3) C21 C22 1.377(3) C21 H21 0.9500 C22 C23 1.396(4) C22 H22 0.9500 C23 C24 1.388(3) C24 C25 1.399(3) C24 H24 0.9500 C25 H25 0.9500 C26 H26B 0.9800 C26 H26C 0.9800 C26 H26D 0.9800 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C3 H3B O2 0.99 2.46 3.446(3) 177.4 2_747 C5 H5A O1 0.95 2.55 3.194(3) 124.8 1_655 C26 H26B I1 0.98 3.22 3.908(3) 128.6 2_647 C26 H26C O2 0.98 2.37 3.285(4) 154.4 2_647 C26 H26D I1 0.98 3.19 4.086(3) 152.6 2_747 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 O2 S1 N1 C2 58.97(19) O3 S1 N1 C2 -173.11(16) C13 S1 N1 C2 -58.33(19) O2 S1 N1 C1 -126.91(17) O3 S1 N1 C1 1.00(18) C13 S1 N1 C1 115.79(17) C2 N1 C1 C5 89.2(2) S1 N1 C1 C5 -84.5(2) C2 N1 C1 C4 -32.4(3) S1 N1 C1 C4 153.82(16) C20 N2 C2 O1 20.4(3) C3 N2 C2 O1 179.1(2) C20 N2 C2 N1 -158.67(19) C3 N2 C2 N1 0.0(3) C1 N1 C2 O1 -173.81(19) S1 N1 C2 O1 0.0(3) C1 N1 C2 N2 5.3(3) S1 N1 C2 N2 179.03(16) C2 N2 C3 C4 23.4(3) C20 N2 C3 C4 -177.55(19) N2 C3 C4 C1 -50.4(2) N2 C3 C4 I1 73.3(2) N1 C1 C4 C3 54.2(2) C5 C1 C4 C3 -71.1(2) N1 C1 C4 I1 -69.13(19) C5 C1 C4 I1 165.61(15) N1 C1 C5 C6 -25.1(3) C4 C1 C5 C6 96.3(3) C1 C5 C6 C7 -179.3(2) C5 C6 C7 C12 -173.6(3) C5 C6 C7 C8 6.9(5) C12 C7 C8 C9 -1.0(5) C6 C7 C8 C9 178.5(3) C7 C8 C9 C10 1.1(6) C8 C9 C10 C11 -0.3(6) C9 C10 C11 C12 -0.6(6) C8 C7 C12 C11 0.0(5) C6 C7 C12 C11 -179.4(3) C10 C11 C12 C7 0.7(6) O2 S1 C13 C18 -10.5(2) O3 S1 C13 C18 -141.5(2) N1 S1 C13 C18 107.6(2) O2 S1 C13 C14 167.8(2) O3 S1 C13 C14 36.8(2) N1 S1 C13 C14 -74.1(2) C18 C13 C14 C15 -2.8(4) S1 C13 C14 C15 178.9(2) C13 C14 C15 C16 2.8(4) C14 C15 C16 C17 -0.5(4) C14 C15 C16 C19 -179.9(3) C15 C16 C17 C18 -2.0(5) C19 C16 C17 C18 177.5(3) C16 C17 C18 C13 2.1(5) C14 C13 C18 C17 0.4(4) S1 C13 C18 C17 178.7(2) C2 N2 C20 C21 62.9(3) C3 N2 C20 C21 -97.9(2) C2 N2 C20 C25 -118.9(2) C3 N2 C20 C25 80.4(3) C25 C20 C21 C22 0.0(4) N2 C20 C21 C22 178.3(2) C20 C21 C22 C23 -1.8(4) C26 O4 C23 C24 4.5(4) C26 O4 C23 C22 -175.0(2) C21 C22 C23 O4 -178.1(2) C21 C22 C23 C24 2.4(4) O4 C23 C24 C25 179.4(2) C22 C23 C24 C25 -1.1(4) C21 C20 C25 C24 1.3(3) N2 C20 C25 C24 -176.9(2) C23 C24 C25 C20 -0.8(4)