#------------------------------------------------------------------------------ #$Date: 2019-11-04 17:43:21 +0200 (Mon, 04 Nov 2019) $ #$Revision: 223176 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/44/4514409.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_4514409 loop_ _publ_author_name 'Li, Man-Bo' 'Grape, Erik Svensson' 'B\"ackvall, Jan-E.' _publ_section_title ; Palladium-Catalyzed Stereospecific Oxidative Cascade Reaction of Allenes for the Construction of Pyrrole Rings: Control of Reactivity and Selectivity ; _journal_issue 6 _journal_name_full 'ACS Catalysis' _journal_page_first 5184 _journal_paper_doi 10.1021/acscatal.9b01041 _journal_volume 9 _journal_year 2019 _chemical_formula_sum 'C31 H31 N O3 S' _chemical_formula_weight 497.63 _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-2018/1 _cell_angle_alpha 90 _cell_angle_beta 96.787(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.4182(3) _cell_length_b 21.7785(10) _cell_length_c 19.0994(8) _cell_measurement_reflns_used 2972 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 52.86 _cell_measurement_theta_min 4.06 _cell_volume 2651.0(2) _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.2421 _diffrn_reflns_av_unetI/netI 0.1023 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 38084 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 59.157 _diffrn_reflns_theta_max 59.157 _diffrn_reflns_theta_min 3.090 _exptl_absorpt_coefficient_mu 1.337 _exptl_absorpt_correction_T_max 0.7516 _exptl_absorpt_correction_T_min 0.5851 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.247 _exptl_crystal_description needle _exptl_crystal_F_000 1056 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.383 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.058 _refine_ls_extinction_coef 0.0056(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/1 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 337 _refine_ls_number_reflns 3829 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.014 _refine_ls_R_factor_all 0.1478 _refine_ls_R_factor_gt 0.0786 _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^)+(0.0972P)^2^+2.0585P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1837 _refine_ls_wR_factor_ref 0.2264 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2103 _reflns_number_total 3829 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs9b01041_si_004.cif _cod_data_source_block manbo_3 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas Adding full bibliography for 4514409.cif. ; _cod_database_code 4514409 _shelx_shelxl_version_number 2018/1 _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_res_file ; TITL cu_esg_manbo_3_181207_0m_a.res in P2(1)/c manbo_3_#12.res created by SHELXL-2018/1 at 14:04:54 on 11-Dec-2018 REM Phenol 1 REM Phenol 2 CELL 1.54178 6.4182 21.7785 19.0994 90 96.787 90 ZERR 4 0.0003 0.001 0.0008 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S UNIT 124 124 4 12 4 L.S. 20 PLAN -10 0 0 TEMP 22.15 ACTA FMAP 2 HTAB BOND $H CONF WGHT 0.097200 2.058500 EXTI 0.005636 FVAR 0.62593 0.45403 PART 0 S1 5 0.174243 0.223736 0.744707 11.00000 0.06459 0.07590 = 0.05567 -0.00661 0.01162 -0.00923 O2 4 -0.046800 0.225864 0.725417 11.00000 0.04914 0.11416 = 0.09470 -0.02482 0.01083 -0.01175 O3 4 0.260882 0.196286 0.810524 11.00000 0.10574 0.07909 = 0.05206 0.00828 0.00718 -0.01259 N1 3 0.261495 0.295972 0.749476 11.00000 0.05208 0.05547 = 0.05319 -0.00754 -0.00404 -0.00588 C15 1 1.010749 0.460111 0.896979 11.00000 0.07794 0.09887 = 0.07416 -0.01315 -0.00141 -0.01672 AFIX 43 H15 2 1.124185 0.479049 0.923207 11.00000 -1.20000 AFIX 0 C16 1 1.025160 0.400431 0.876180 11.00000 0.05884 0.09471 = 0.05790 0.00045 0.00335 -0.00356 AFIX 43 H16 2 1.149072 0.378742 0.888150 11.00000 -1.20000 AFIX 0 C17 1 0.856717 0.372105 0.837464 11.00000 0.06654 0.06843 = 0.04279 0.00172 0.00673 0.00436 AFIX 43 H17 2 0.868503 0.331361 0.823895 11.00000 -1.20000 AFIX 0 C12 1 0.669805 0.403422 0.818410 11.00000 0.06246 0.06061 = 0.04263 0.00542 0.00980 0.00045 C4 1 0.447425 0.311162 0.789663 11.00000 0.06046 0.06140 = 0.04887 -0.00315 -0.00251 0.01074 AFIX 43 H4 2 0.530034 0.284274 0.818850 11.00000 -1.20000 AFIX 0 C25 1 0.295289 0.188397 0.677891 11.00000 0.05704 0.06112 = 0.04758 -0.00537 0.00861 -0.00648 C26 1 0.499043 0.167236 0.692248 11.00000 0.05680 0.10148 = 0.07364 -0.01731 -0.00406 -0.00553 AFIX 43 H26 2 0.572289 0.171856 0.736940 11.00000 -1.20000 AFIX 0 C27 1 0.591608 0.139132 0.638994 11.00000 0.05747 0.11196 = 0.09813 -0.02730 0.01299 -0.00194 AFIX 43 H27 2 0.728893 0.125022 0.648125 11.00000 -1.20000 AFIX 0 C28 1 0.484868 0.131514 0.572485 11.00000 0.08556 0.06874 = 0.06235 -0.01086 0.01952 -0.00407 C31 1 0.592216 0.100318 0.515337 11.00000 0.15392 0.10547 = 0.10441 -0.03015 0.05300 0.01570 AFIX 137 H31A 2 0.572076 0.056723 0.517723 11.00000 -1.50000 H31B 2 0.739583 0.109401 0.522186 11.00000 -1.50000 H31C 2 0.532860 0.115106 0.469971 11.00000 -1.50000 AFIX 0 C1 1 0.182063 0.348691 0.712346 11.00000 0.05286 0.06598 = 0.04266 -0.00387 0.00417 0.01421 C18 1 -0.019432 0.350693 0.663700 11.00000 0.06171 0.08537 = 0.05781 -0.01186 -0.00200 0.01382 AFIX 23 H18B 2 -0.062436 0.393260 0.657804 11.00000 -1.20000 H18A 2 -0.126312 0.329597 0.686449 11.00000 -1.20000 AFIX 0 C19 1 -0.014614 0.323000 0.591477 11.00000 0.07347 0.06644 = 0.04996 -0.00668 -0.01191 0.01829 C24 1 -0.191040 0.295322 0.557446 11.00000 0.07503 0.10671 = 0.07499 -0.02219 -0.02317 0.02374 AFIX 43 H24 2 -0.311201 0.292327 0.580090 11.00000 -1.20000 AFIX 0 C22 1 -0.022275 0.275519 0.455758 11.00000 0.16892 0.08409 = 0.05946 -0.01741 -0.04005 0.01586 AFIX 43 H22 2 -0.023652 0.259477 0.410580 11.00000 -1.20000 AFIX 0 C20 1 0.160897 0.327298 0.557166 11.00000 0.09125 0.08238 = 0.04895 0.00024 0.00484 0.01622 AFIX 43 H20 2 0.282946 0.345660 0.578564 11.00000 -1.20000 AFIX 0 C2 1 0.320333 0.394986 0.731008 11.00000 0.05172 0.07128 = 0.04421 0.00270 0.00392 0.01282 C14 1 0.827987 0.491934 0.878952 11.00000 0.09683 0.07253 = 0.08459 -0.02244 0.00524 -0.01463 AFIX 43 H14 2 0.818022 0.532507 0.893374 11.00000 -1.20000 AFIX 0 C13 1 0.658614 0.464647 0.839724 11.00000 0.07121 0.06412 = 0.07592 -0.00327 0.00220 0.00092 AFIX 43 H13 2 0.536462 0.487070 0.827403 11.00000 -1.20000 AFIX 0 C5 1 0.300145 0.459359 0.704166 11.00000 0.06288 0.07341 = 0.06129 0.01253 0.00160 0.00815 C11 1 0.474992 0.481857 0.664357 11.00000 0.08187 0.13427 = 0.10024 0.05478 0.02482 0.01539 AFIX 23 H11B 2 0.546909 0.514835 0.691490 11.00000 -1.20000 H11A 2 0.574840 0.448594 0.662786 11.00000 -1.20000 AFIX 0 C10 1 0.420619 0.503494 0.594018 11.00000 0.17809 0.21107 = 0.12975 0.09186 0.05988 0.04169 AFIX 23 H10A 2 0.342143 0.471139 0.567827 11.00000 -1.20000 H10B 2 0.550087 0.508761 0.573144 11.00000 -1.20000 AFIX 0 C9 1 0.296452 0.561822 0.581706 11.00000 0.19199 0.16994 = 0.18125 0.11316 0.02261 0.02603 AFIX 23 H9A 2 0.280377 0.570779 0.531608 11.00000 -1.20000 H9B 2 0.376456 0.595116 0.605507 11.00000 -1.20000 AFIX 0 C8 1 0.080886 0.560804 0.606511 11.00000 0.18826 0.13042 = 0.17713 0.06838 -0.04624 0.03168 AFIX 23 H8B 2 0.007385 0.598133 0.590711 11.00000 -1.20000 H8A 2 0.002633 0.526488 0.584262 11.00000 -1.20000 AFIX 0 C7 1 0.081902 0.555524 0.685035 11.00000 0.12205 0.07696 = 0.16685 0.02029 -0.00654 0.03040 AFIX 23 H6B 2 0.183494 0.584395 0.707679 11.00000 -1.20000 H6A 2 -0.055102 0.567424 0.697063 11.00000 -1.20000 AFIX 0 C6 1 0.132630 0.493041 0.714305 11.00000 0.07853 0.07076 = 0.08770 0.00443 0.00485 0.02040 AFIX 43 H6 2 0.038535 0.475951 0.742275 11.00000 -1.20000 AFIX 0 C30 1 0.186183 0.180428 0.611962 11.00000 0.08341 0.07236 = 0.05416 -0.00846 -0.00496 0.01416 AFIX 43 H30 2 0.047623 0.193419 0.602739 11.00000 -1.20000 AFIX 0 C29 1 0.285271 0.152867 0.559652 11.00000 0.10818 0.07165 = 0.05804 -0.00265 -0.00402 0.01567 AFIX 43 H29 2 0.213512 0.148871 0.514650 11.00000 -1.20000 AFIX 0 C3 1 0.490967 0.371000 0.780112 11.00000 0.05252 0.06059 = 0.04255 -0.00167 0.00447 0.00834 C21 1 0.150402 0.303120 0.488802 11.00000 0.13457 0.08482 = 0.05258 0.01132 0.03002 0.03617 PART 1 AFIX 43 H21 2 0.268320 0.306253 0.465025 21.00000 -1.20000 AFIX 0 O1B 4 -0.326267 0.252079 0.444209 21.00000 0.05188 0.13848 = 0.06831 -0.02770 -0.01915 0.00540 AFIX 83 H1B 2 -0.438273 0.248054 0.460384 21.00000 -1.50000 AFIX 0 PART 0 C23 1 -0.192370 0.272066 0.490590 11.00000 0.11478 0.09169 = 0.08386 -0.01893 -0.03873 0.03013 PART 2 AFIX 43 H23 2 -0.313602 0.253496 0.468861 -21.00000 -1.20000 AFIX 0 O1A 4 0.299848 0.309523 0.455309 -21.00000 0.07373 0.12918 = 0.05756 -0.00747 0.00021 0.00162 AFIX 83 H1A 2 0.284920 0.287226 0.420481 -21.00000 -1.50000 AFIX 0 HKLF 4 REM cu_esg_manbo_3_181207_0m_a.res in P2(1)/c REM R1 = 0.0786 for 2103 Fo > 4sig(Fo) and 0.1478 for all 3829 data REM 337 parameters refined using 0 restraints END WGHT 0.0960 2.1065 REM Instructions for potential hydrogen bonds EQIV $1 x+1, -y+1/2, z+1/2 HTAB C4 O1B_$1 HTAB C18 O2 EQIV $2 x, -y+1/2, z-1/2 HTAB O1A O3_$2 REM Highest difference peak 0.383, deepest hole -0.318, 1-sigma level 0.058 Q1 1 0.5070 0.5529 0.6413 11.00000 0.05 0.38 Q2 1 0.4587 0.2341 0.7718 11.00000 0.05 0.29 Q3 1 0.4128 0.2455 0.7225 11.00000 0.05 0.29 Q4 1 0.0875 0.1574 0.7042 11.00000 0.05 0.26 Q5 1 0.4955 0.2491 0.8366 11.00000 0.05 0.23 Q6 1 0.0694 0.2825 0.6958 11.00000 0.05 0.23 Q7 1 0.1082 0.2310 0.8222 11.00000 0.05 0.22 Q8 1 0.2225 0.5793 0.6574 11.00000 0.05 0.22 Q9 1 0.0425 0.2771 0.7783 11.00000 0.05 0.22 Q10 1 0.3494 0.2475 0.8198 11.00000 0.05 0.21 ; _shelx_res_checksum 21181 _shelx_hkl_file ; 1 0 0 1061.69 121.09 1 0 0 1010.90 121.69 -1 0 0 1011.30 120.99 -1 0 0 1000.60 121.19 -1 0 0 975.70 121.59 1 0 0 1017.20 120.89 -2 0 0 119.49 16.60 -2 0 0 117.49 19.30 2 0 0 120.89 16.40 2 0 0 125.19 20.90 -2 0 0 128.79 15.60 3 0 0 135.39 19.60 -3 0 0 146.79 26.20 -3 0 0 150.98 22.50 4 0 0 399.56 72.19 4 0 0 402.06 63.79 -4 0 0 360.66 60.89 4 0 0 432.36 58.39 5 0 0 -4.50 27.60 5 0 0 -13.10 29.10 5 0 0 -34.90 23.60 5 0 0 49.99 36.30 5 0 0 55.29 41.10 6 0 0 335.07 69.59 6 0 0 467.35 76.49 6 0 0 429.56 64.09 6 0 0 478.45 66.49 6 0 0 355.06 72.09 7 0 0 13.30 21.80 7 0 0 51.19 26.90 7 0 0 10.30 16.70 7 0 0 -0.90 24.20 -7 0 0 -60.29 41.90 7 0 0 15.70 27.40 7 0 0 -25.80 21.10 0 1 0 -0.40 0.90 -1 -1 0 3986.50 462.45 -1 -1 0 3716.03 461.95 1 -1 0 3890.41 462.25 1 -1 0 3877.51 462.05 -1 -1 0 3794.32 461.85 1 1 0 3706.13 461.75 1 1 0 3968.90 462.45 -1 1 0 3706.13 462.15 1 1 0 3928.91 461.85 -1 1 0 4162.88 462.05 -2 -1 0 131.59 18.30 2 -1 0 155.18 18.50 2 -1 0 153.08 22.30 -2 -1 0 135.39 21.50 -2 -1 0 145.69 18.10 -2 1 0 127.79 20.70 2 1 0 145.89 17.90 2 1 0 132.29 17.90 -3 -1 0 1492.35 190.28 3 -1 0 1618.44 188.28 -3 -1 0 1657.33 188.48 -3 1 0 1460.55 189.88 -3 1 0 1548.55 188.68 3 1 0 1616.04 187.78 4 -1 0 312.37 39.80 4 -1 0 311.57 63.59 -4 -1 0 314.17 51.39 4 -1 0 281.67 60.89 4 -1 0 265.17 51.79 4 -1 0 381.96 54.19 4 -1 0 287.07 48.00 4 1 0 335.77 57.59 4 1 0 298.67 45.80 -4 1 0 264.57 51.19 4 1 0 265.07 56.19 5 -1 0 -6.30 37.80 5 -1 0 -48.20 40.80 5 -1 0 6.80 23.50 5 -1 0 13.60 27.90 5 -1 0 -42.20 29.00 5 1 0 9.70 21.00 5 1 0 35.10 34.70 5 1 0 -3.40 28.30 5 1 0 -29.40 22.40 5 1 0 -48.20 49.30 6 -1 0 79.19 37.40 6 -1 0 25.40 27.30 6 -1 0 -21.50 31.30 6 -1 0 29.20 30.10 6 -1 0 15.90 41.00 6 -1 0 28.90 22.60 -6 -1 0 12.80 40.80 6 1 0 50.39 29.20 6 1 0 -47.20 31.50 6 1 0 29.80 22.70 6 1 0 29.20 25.30 6 1 0 124.69 39.60 6 1 0 54.29 39.90 7 -1 0 39.30 23.80 7 -1 0 -5.50 18.20 -7 -1 0 -12.20 38.80 7 -1 0 -3.90 23.10 7 -1 0 39.00 28.80 7 -1 0 2.30 20.30 7 1 0 -5.60 15.10 7 1 0 49.80 27.70 7 1 0 19.10 25.10 7 1 0 43.20 18.40 7 1 0 33.20 25.10 7 1 0 25.70 22.80 -7 1 0 56.69 41.60 0 -2 0 3383.16 438.36 0 -2 0 3637.24 438.26 0 -2 0 4058.99 438.36 0 2 0 3701.83 438.26 0 2 0 3717.83 438.36 0 2 0 3550.54 438.36 1 -2 0 1556.04 187.58 -1 -2 0 1534.05 187.58 -1 -2 0 1520.75 187.28 1 -2 0 1534.05 187.58 -1 2 0 1557.44 187.58 1 2 0 1653.73 187.28 1 2 0 1627.24 187.58 -2 -2 0 1752.02 200.08 2 -2 0 1752.42 201.48 -2 -2 0 1651.73 201.48 -2 -2 0 1482.55 200.48 2 -2 0 1669.23 200.48 -2 2 0 1635.54 200.98 2 2 0 1701.13 199.78 2 2 0 1743.53 200.28 3 -2 0 389.56 50.39 -3 -2 0 388.26 54.29 -3 -2 0 409.86 50.69 -3 2 0 413.46 53.19 -3 2 0 436.26 52.69 4 -2 0 199.28 45.20 4 -2 0 183.68 41.00 4 -2 0 182.88 29.20 -4 -2 0 163.08 37.30 4 -2 0 152.48 52.89 4 2 0 223.98 54.39 4 2 0 210.88 48.30 -4 2 0 188.68 35.40 -4 2 0 206.28 40.50 4 2 0 223.88 34.70 4 2 0 224.28 45.80 5 -2 0 109.29 48.90 5 -2 0 120.39 37.00 5 -2 0 143.09 44.10 5 -2 0 77.69 29.20 5 -2 0 89.79 31.40 5 2 0 18.70 38.80 5 2 0 65.69 37.10 5 2 0 138.09 52.39 5 2 0 78.09 34.40 5 2 0 80.39 24.20 6 -2 0 24.30 23.20 6 -2 0 17.30 34.40 6 -2 0 0.30 27.60 6 -2 0 87.49 40.30 -6 -2 0 23.20 41.90 6 -2 0 -0.40 25.80 6 2 0 -17.50 19.70 6 2 0 -21.00 24.30 6 2 0 -21.30 32.70 6 2 0 64.39 41.90 6 2 0 27.50 32.70 6 2 0 -8.80 29.80 7 -2 0 34.40 25.50 7 -2 0 26.10 27.60 -7 -2 0 7.30 38.30 7 -2 0 -2.20 19.10 7 -2 0 -7.70 19.50 7 2 0 3.70 25.00 7 2 0 54.09 22.90 7 2 0 36.00 27.10 7 2 0 -57.69 30.00 7 2 0 8.80 17.40 7 2 0 8.10 15.60 0 -3 0 1.00 3.00 0 -3 0 -0.70 3.70 0 3 0 -2.00 2.70 0 3 0 -3.70 4.10 -1 -3 0 2421.86 326.07 1 -3 0 2771.32 325.57 -1 -3 0 2805.92 325.37 1 -3 0 2811.92 325.77 1 3 0 2747.93 325.37 1 3 0 2841.22 325.77 -1 3 0 2713.23 325.47 -1 3 0 2701.33 325.47 -2 -3 0 -13.50 8.60 2 -3 0 -3.60 8.70 -2 -3 0 8.70 3.90 -2 -3 0 4.70 5.50 2 -3 0 7.40 4.80 2 3 0 16.10 5.60 -2 3 0 5.50 1.80 -2 3 0 -1.00 6.30 -2 3 0 -9.70 9.70 -2 3 0 5.00 1.60 3 -3 0 -0.60 8.10 -3 -3 0 1.50 13.30 -3 3 0 2.30 14.60 -3 3 0 10.10 12.20 3 3 0 23.40 8.90 -4 -3 0 201.38 40.30 4 -3 0 324.17 50.99 4 -3 0 232.28 54.59 4 -3 0 208.28 45.90 4 -3 0 114.89 49.10 4 -3 0 190.58 43.70 4 -3 0 247.58 49.70 4 -3 0 184.28 44.10 -4 3 0 229.58 46.00 -4 3 0 196.48 42.80 4 3 0 260.67 39.40 4 3 0 262.77 50.49 4 3 0 256.67 73.19 4 3 0 128.99 63.49 4 3 0 316.17 51.79 5 -3 0 164.58 37.00 5 -3 0 141.69 51.09 5 -3 0 30.30 30.90 5 -3 0 97.89 33.20 5 -3 0 103.69 42.60 5 3 0 79.59 23.80 5 3 0 151.08 44.90 5 3 0 222.58 60.09 5 3 0 106.29 37.70 -6 -3 0 15.80 39.10 6 -3 0 21.50 27.10 6 -3 0 -33.60 27.50 6 -3 0 28.30 25.10 6 -3 0 41.80 37.20 6 -3 0 23.40 35.60 6 3 0 34.30 32.90 6 3 0 28.60 41.30 6 3 0 -16.70 20.80 6 3 0 29.80 34.60 6 3 0 10.30 30.90 7 -3 0 -1.80 18.50 7 -3 0 -10.10 20.30 -7 -3 0 61.19 34.70 7 -3 0 -9.10 20.50 7 -3 0 47.40 31.80 7 3 0 5.80 15.60 7 3 0 -7.50 23.90 7 3 0 22.50 21.70 7 3 0 -2.20 14.00 0 -4 0 571.04 70.09 0 -4 0 644.24 70.59 0 4 0 528.15 70.49 -1 -4 0 1518.55 213.88 1 -4 0 1739.23 213.08 -1 -4 0 1847.32 213.68 -1 -4 0 1733.93 212.78 1 -4 0 1918.31 213.58 -1 -4 0 1720.93 213.78 1 4 0 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3 97.79 53.09 5 -7 3 140.39 31.10 -5 -7 -3 229.68 45.20 5 -7 3 194.88 58.59 5 7 3 209.18 53.29 -5 7 -3 182.78 61.89 5 7 3 118.39 28.40 5 7 3 121.49 46.80 6 -7 3 -23.20 21.30 6 -7 3 5.40 38.70 -6 -7 -3 50.99 28.00 -6 7 -3 28.10 44.40 6 7 3 37.50 28.40 6 7 3 31.40 21.30 6 7 3 18.80 36.60 6 7 3 -15.30 16.60 6 7 3 32.20 16.00 6 -8 -3 42.80 38.80 6 -8 -3 99.89 24.20 6 -8 -3 -39.80 43.40 -6 -8 3 43.90 46.40 6 8 -3 -29.70 38.40 5 -8 -3 23.50 32.30 -5 -8 3 79.49 30.90 5 -8 -3 80.79 32.40 -5 -8 3 159.78 49.90 5 -8 -3 81.59 40.50 5 -8 -3 72.49 39.90 5 -8 -3 67.59 33.00 5 -8 -3 141.79 29.90 5 -8 -3 140.69 36.10 5 8 -3 49.50 25.70 5 8 -3 83.19 45.90 5 8 -3 75.19 19.90 5 8 -3 160.78 44.00 -4 -8 3 -73.19 43.10 4 -8 -3 -46.80 29.30 4 -8 -3 -23.30 16.50 4 -8 -3 53.19 30.10 -4 -8 3 -91.89 49.20 4 8 -3 50.79 49.10 4 8 -3 4.50 16.20 4 8 -3 80.99 46.30 -4 8 3 70.09 41.50 -4 8 3 -7.70 25.70 3 -8 -3 641.14 85.79 3 -8 -3 726.83 88.49 3 -8 -3 588.44 83.79 3 -8 -3 492.95 87.49 3 -8 -3 551.04 76.89 3 -8 -3 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3 9 3 48.00 16.10 3 9 3 72.99 39.10 4 -9 3 146.69 46.90 -4 -9 -3 118.59 67.39 4 -9 3 175.48 32.90 4 -9 3 135.19 58.69 4 -9 3 268.47 63.29 -4 -9 -3 223.88 41.90 4 -9 3 125.89 32.90 4 9 3 158.38 31.80 -4 9 -3 133.79 69.99 4 9 3 200.58 60.59 4 9 3 217.78 50.39 4 9 3 201.68 52.49 5 -9 3 115.39 55.39 5 -9 3 71.59 48.60 5 -9 3 91.69 46.90 -5 -9 -3 102.09 37.50 -5 -9 -3 22.00 48.70 5 9 3 94.59 40.50 5 9 3 28.60 39.50 5 9 3 62.19 21.00 -5 9 -3 109.99 54.99 6 -9 3 29.00 32.70 6 -9 3 -23.70 17.60 6 -9 3 -18.20 22.50 -6 -9 -3 31.80 20.90 6 -9 3 58.69 36.90 -6 -9 -3 12.80 25.80 6 9 3 69.49 28.20 6 9 3 8.70 12.30 6 9 3 -10.20 16.30 -6 9 -3 56.99 46.10 6 -10 -3 -23.30 21.90 6 -10 -3 13.40 28.10 6 -10 -3 28.10 37.40 6 -10 -3 -23.80 20.30 6 10 -3 3.00 16.10 6 10 -3 4.10 17.30 5 -10 -3 37.90 31.00 5 -10 -3 43.40 29.70 -5 -10 3 74.99 30.60 5 -10 -3 25.40 40.40 5 -10 -3 44.30 28.10 5 -10 -3 85.29 31.60 5 -10 -3 91.59 39.60 5 -10 -3 100.49 29.20 -5 -10 3 196.58 48.50 5 -10 -3 66.99 45.00 5 10 -3 156.18 43.90 5 10 -3 32.90 24.10 5 10 -3 57.99 17.80 4 -10 -3 60.89 44.30 4 -10 -3 81.09 23.50 4 -10 -3 9.50 29.00 4 -10 -3 122.79 49.00 -4 -10 3 134.99 44.20 4 -10 -3 66.69 32.60 4 -10 -3 89.19 36.60 4 -10 -3 95.59 32.60 4 -10 -3 39.10 33.00 4 10 -3 22.20 25.20 4 10 -3 71.59 40.30 4 10 -3 148.39 40.80 4 10 -3 93.89 20.50 -3 -10 3 55.19 39.10 3 -10 -3 -16.50 24.70 3 -10 -3 54.89 30.40 3 -10 -3 -14.30 48.10 3 -10 -3 38.00 32.50 3 -10 -3 65.09 38.80 3 -10 -3 11.80 13.10 3 -10 -3 23.10 29.60 3 -10 -3 3.90 36.60 3 -10 -3 15.80 42.30 3 -10 -3 -18.70 31.50 -3 -10 3 4.60 27.10 -3 -10 3 -22.00 29.80 -3 -10 3 28.60 24.70 3 10 -3 38.60 34.40 3 10 -3 40.80 27.50 3 10 -3 15.70 17.00 -3 10 3 20.60 18.40 3 10 -3 -4.30 35.90 3 10 -3 -30.10 38.00 -3 10 3 66.29 27.40 -2 -10 3 96.29 25.70 2 -10 -3 200.88 55.09 -2 -10 3 108.49 25.70 2 -10 -3 185.78 36.50 2 -10 -3 146.69 23.30 2 10 -3 138.29 51.19 2 10 -3 139.79 17.00 2 10 -3 136.99 26.80 2 10 -3 220.58 46.80 2 10 -3 101.99 16.30 -2 10 3 157.08 25.60 1 -10 -3 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34.30 4 -10 3 24.80 23.40 4 -10 3 16.70 49.70 4 10 3 38.00 45.30 4 10 3 69.79 40.80 4 10 3 76.39 24.10 -4 10 -3 36.10 59.59 4 10 3 62.59 42.50 5 -10 3 91.09 50.79 -5 -10 -3 165.08 39.40 5 -10 3 72.59 48.50 -5 -10 -3 91.29 29.80 5 -10 3 45.90 48.70 5 10 3 65.89 21.80 5 10 3 77.39 41.50 -5 10 -3 64.99 54.49 5 10 3 184.68 47.50 6 -10 3 -16.70 21.90 6 -10 3 13.20 32.80 -6 -10 -3 57.29 28.20 6 -10 3 1.60 30.90 6 -10 3 -33.10 17.20 -6 -10 -3 48.00 20.10 6 10 3 -11.40 16.20 6 10 3 17.80 11.80 -6 10 -3 19.40 40.40 6 -11 -3 -36.80 17.00 6 -11 -3 8.10 22.00 6 -11 -3 -14.30 27.50 6 -11 -3 3.70 21.60 6 11 -3 3.70 14.80 6 11 -3 0.10 18.30 6 11 -3 25.40 13.90 5 -11 -3 -2.90 22.30 5 -11 -3 -12.60 38.10 5 -11 -3 12.20 35.90 -5 -11 3 39.60 27.70 5 -11 -3 17.00 39.60 5 -11 -3 4.30 26.50 5 -11 -3 6.80 28.50 5 -11 -3 1.40 27.70 5 11 -3 38.80 15.60 5 11 -3 4.60 21.20 5 11 -3 80.09 40.00 4 -11 -3 161.58 39.90 -4 -11 3 279.37 49.20 4 -11 -3 143.19 38.60 4 -11 -3 85.79 41.60 4 -11 -3 175.18 38.90 4 -11 -3 77.69 50.69 4 -11 -3 270.77 44.50 4 -11 -3 302.07 59.39 4 11 -3 225.88 32.00 4 11 -3 184.58 46.50 4 11 -3 182.28 36.20 3 -11 -3 21.90 23.90 3 -11 -3 -10.30 43.00 3 -11 -3 -1.50 39.50 3 -11 -3 57.39 43.10 3 -11 -3 23.50 29.20 3 -11 -3 19.00 16.30 -3 -11 3 -26.20 27.50 3 -11 -3 -6.50 29.40 -3 -11 3 0.30 31.60 3 -11 -3 9.50 31.80 3 -11 -3 66.69 39.30 3 11 -3 9.30 47.20 3 11 -3 -7.10 35.20 -3 11 3 40.20 31.70 3 11 -3 15.60 26.70 3 11 -3 2.00 16.10 -3 11 3 3.00 21.10 3 11 -3 51.59 34.60 2 -11 -3 358.06 49.30 2 -11 -3 326.67 52.39 2 -11 -3 311.67 64.29 -2 -11 3 366.96 53.79 -2 -11 3 334.77 61.59 2 -11 -3 432.46 66.69 2 -11 -3 427.76 60.29 2 -11 -3 379.26 59.79 2 11 -3 406.16 67.39 -2 11 3 387.56 51.09 2 11 -3 367.36 52.39 2 11 -3 427.26 63.29 2 11 -3 574.74 76.69 -2 11 3 352.76 53.09 -1 -11 3 186.28 30.90 -1 -11 3 195.28 33.70 -1 -11 3 220.48 27.60 -1 11 3 180.28 32.60 1 11 -3 226.88 28.40 -1 11 3 182.68 30.00 0 -11 -3 4.00 9.10 0 -11 3 0.70 9.00 0 -11 3 2.20 13.60 0 11 3 -8.20 9.70 0 11 -3 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11 3 50.69 41.20 4 11 3 21.30 38.40 4 11 3 57.39 22.70 4 11 3 117.69 41.70 -5 -11 -3 125.79 29.80 5 -11 3 46.90 33.70 5 -11 3 50.59 44.30 5 -11 3 128.09 56.69 5 -11 3 74.99 49.90 5 11 3 20.10 38.60 5 11 3 175.98 47.40 -5 11 -3 47.30 53.49 5 11 3 86.59 22.20 6 -11 3 22.70 27.10 6 -11 3 1.60 19.60 6 -11 3 -17.00 21.80 -6 -11 -3 7.40 18.30 6 -11 3 3.40 26.00 -6 11 -3 -29.20 36.40 6 11 3 -9.90 10.40 6 11 3 -9.20 14.80 6 -12 -3 -23.10 25.30 6 -12 -3 4.40 18.70 6 -12 -3 5.30 19.10 6 -12 -3 18.80 25.10 6 12 -3 -36.20 15.80 6 12 -3 5.20 14.10 6 12 -3 19.30 13.50 5 -12 -3 -20.80 38.50 5 -12 -3 0.40 26.40 5 -12 -3 42.30 45.20 -5 -12 3 45.30 30.40 5 -12 -3 19.30 28.50 5 -12 -3 -13.60 21.50 5 -12 -3 51.49 37.90 5 12 -3 4.10 14.10 5 12 -3 15.20 20.60 4 -12 -3 110.39 34.30 4 -12 -3 83.49 35.20 -4 -12 3 139.09 33.30 4 -12 -3 51.89 31.00 4 -12 -3 27.20 40.60 4 -12 -3 111.19 28.50 4 -12 -3 58.79 29.60 4 -12 -3 -51.29 37.50 4 12 -3 109.79 35.20 4 12 -3 50.99 26.70 4 12 -3 122.79 21.80 -3 -12 3 69.29 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24.50 -1 1 -20 51.89 15.50 3 -2 -20 48.40 16.80 3 -2 -20 60.59 22.40 3 -2 -20 32.20 17.00 3 -2 -20 21.20 29.90 3 -2 -20 15.10 12.40 3 -2 -20 32.20 20.20 3 2 -20 31.90 18.70 3 2 -20 20.70 13.00 3 2 -20 2.50 12.10 3 2 -20 74.59 20.00 3 2 -20 -3.40 18.90 -2 -2 20 80.99 34.40 2 -2 -20 68.99 19.20 2 -2 -20 22.90 14.20 2 -2 -20 71.99 22.30 2 -2 -20 -23.50 26.70 2 -2 -20 11.10 21.60 2 2 -20 23.70 17.80 2 2 -20 15.80 19.90 2 2 -20 69.59 19.50 2 2 -20 33.80 15.40 2 2 -20 35.60 22.30 1 -2 -20 18.20 15.50 -1 -2 20 -3.60 29.20 1 -2 -20 -15.10 29.70 1 -2 -20 -25.60 21.70 1 -2 -20 29.30 16.00 1 -2 -20 20.40 16.30 1 2 -20 24.00 18.90 1 2 -20 -24.00 16.40 1 2 -20 -17.40 12.40 1 2 -20 28.00 25.70 0 -2 20 31.40 26.10 0 -2 20 36.90 28.70 0 -2 -20 19.50 22.00 0 -2 -20 67.69 16.80 0 2 -20 28.70 15.10 0 2 20 30.00 28.10 1 -2 20 -18.00 20.80 -1 -2 -20 7.50 12.50 1 -2 20 -8.00 23.60 1 2 20 36.40 26.10 1 2 20 -24.00 36.60 -1 2 -20 2.70 12.00 3 -3 -20 0.30 18.00 3 -3 -20 -6.50 14.10 3 -3 -20 -8.20 10.10 3 -3 -20 11.40 14.40 3 3 -20 16.50 13.00 3 3 -20 2.60 18.90 3 3 -20 3.40 13.70 3 3 -20 -3.20 15.10 -2 -3 20 9.40 25.90 2 -3 -20 20.70 12.60 2 -3 -20 21.60 26.40 2 -3 -20 13.10 19.90 2 -3 -20 4.70 22.60 2 -3 -20 13.50 16.80 2 3 -20 66.69 17.80 2 3 -20 -1.50 15.50 2 3 -20 22.60 21.10 2 3 -20 -16.70 21.00 2 3 -20 12.00 15.90 1 -3 -20 21.90 15.60 1 -3 -20 3.50 15.50 -1 -3 20 -28.90 24.10 1 -3 -20 4.80 21.60 1 -3 -20 13.70 12.50 1 3 -20 3.10 13.00 -1 3 20 34.30 26.40 1 3 -20 21.20 19.70 0 -3 20 7.20 26.30 0 -3 -20 19.40 12.60 0 -3 -20 -14.10 20.30 0 3 20 -20.90 21.90 0 3 -20 -17.00 11.60 1 -3 20 14.60 23.00 -1 -3 -20 -0.20 11.50 1 -3 20 3.90 20.70 -1 3 -20 13.40 13.60 1 3 20 -11.20 19.10 2 -4 -20 64.29 15.50 2 -4 -20 19.80 21.30 2 -4 -20 49.80 24.10 -2 -4 20 26.60 26.70 2 -4 -20 17.10 16.40 2 -4 -20 51.99 19.90 2 -4 -20 14.00 24.10 -2 4 20 -12.80 28.00 2 4 -20 75.19 23.90 2 4 -20 59.09 16.60 2 4 -20 26.30 17.10 2 4 -20 40.20 18.10 -1 -4 20 -14.70 23.90 1 -4 -20 7.50 14.90 1 -4 -20 7.50 11.30 1 -4 -20 18.50 14.40 1 -4 -20 36.30 22.00 1 4 -20 23.90 13.70 1 4 -20 -17.10 16.50 -1 4 20 -27.80 24.00 0 -4 -20 52.09 15.60 0 -4 20 63.69 28.50 0 -4 -20 81.59 20.50 0 4 20 32.00 25.80 0 4 -20 75.19 17.50 1 -4 20 22.80 23.40 -1 -4 -20 10.90 11.40 1 -4 20 5.90 21.50 1 -4 20 -4.70 32.70 1 4 20 40.90 23.50 -1 4 -20 -2.90 12.30 2 -5 -20 27.40 18.90 2 -5 -20 19.80 12.30 2 -5 -20 10.60 13.30 2 -5 -20 17.30 24.70 2 -5 -20 9.60 20.60 -2 -5 20 7.10 23.40 2 -5 -20 34.20 23.60 -2 5 20 -22.40 26.90 2 5 -20 17.40 18.50 2 5 -20 -0.10 14.20 2 5 -20 -1.20 15.30 2 5 -20 3.30 22.60 1 -5 -20 29.60 20.80 -1 -5 20 1.50 23.20 1 -5 -20 28.40 14.60 1 -5 -20 11.20 12.40 -1 5 20 55.19 27.20 1 5 -20 9.10 17.80 1 5 -20 42.70 13.60 0 -5 -20 45.30 18.50 0 -5 -20 79.49 13.80 0 -5 20 1.20 23.90 0 5 20 35.70 25.20 0 5 -20 13.80 12.90 -1 -5 -20 -10.80 10.00 1 -5 20 -6.60 22.30 1 -5 20 13.40 22.30 1 -5 20 -11.40 35.70 -1 5 -20 -3.50 12.20 1 5 20 -7.10 21.80 2 -6 -20 24.40 21.70 2 -6 -20 9.70 22.30 -2 -6 20 -8.20 24.30 2 -6 -20 21.30 29.90 2 -6 -20 2.50 16.80 2 -6 -20 10.90 14.30 2 -6 -20 16.80 11.90 -2 6 20 -13.20 29.80 2 6 -20 -4.60 16.40 2 6 -20 26.10 22.30 2 6 -20 17.50 14.30 -1 -6 20 55.39 24.70 1 -6 -20 55.19 21.10 1 -6 -20 31.10 15.00 1 -6 -20 46.30 12.70 -1 6 20 -10.10 25.60 1 6 -20 37.90 21.20 1 6 -20 51.79 14.30 0 -6 20 -9.30 19.80 0 -6 -20 5.00 15.50 0 -6 -20 16.50 9.90 0 6 20 18.40 23.40 0 6 -20 -13.90 10.80 2 -7 -20 2.20 13.40 2 -7 -20 0.80 9.90 2 7 -20 -14.90 16.60 1 -7 -20 -7.50 12.80 1 -7 -20 18.90 11.00 1 -7 -20 19.60 23.90 -1 -7 20 -6.90 20.80 1 -7 -20 9.90 18.60 1 7 -20 21.10 11.80 -1 7 20 -53.39 26.00 0 -7 -20 13.20 14.00 0 -7 20 -10.60 19.10 0 -7 -20 -0.10 9.20 0 7 20 22.50 25.40 0 7 -20 4.80 12.20 1 -8 -20 17.20 17.60 -1 -8 20 8.50 20.90 1 -8 -20 7.60 20.30 1 -8 -20 -0.50 12.60 -1 8 20 1.30 33.20 1 8 -20 -0.30 10.70 1 0 -21 7.60 14.20 1 0 -21 -47.50 27.00 1 0 -21 13.30 15.10 1 0 -21 40.00 18.40 0 0 21 5.00 34.20 0 0 -21 -21.20 11.10 0 0 21 -13.50 17.80 1 -1 -21 4.30 15.30 -1 -1 21 45.70 34.70 1 -1 -21 -37.20 16.00 1 1 -21 -20.90 25.20 1 1 -21 29.10 14.90 -1 1 21 7.40 20.00 1 1 -21 -9.20 14.70 0 -1 -21 -1.60 11.90 0 -1 21 24.60 29.60 0 -1 21 15.20 19.40 0 1 21 18.10 20.50 0 1 -21 7.40 12.10 1 -2 -21 11.70 15.10 -1 -2 21 -24.70 26.90 1 -2 -21 -18.50 10.40 1 2 -21 36.80 23.90 -1 2 21 56.59 25.20 1 2 -21 10.40 13.60 0 -2 -21 8.20 11.60 0 2 -21 1.90 11.60 1 -3 -21 27.50 14.70 -1 -3 21 28.70 25.60 1 -3 -21 4.60 10.70 -1 3 21 -46.80 21.70 1 3 -21 9.40 20.80 1 3 -21 13.70 12.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 21360 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.1742(2) 0.22374(7) 0.74471(7) 0.0650(5) Uani 1 1 d . . . . . O2 O -0.0468(6) 0.2259(2) 0.7254(2) 0.0858(13) Uani 1 1 d . . . . . O3 O 0.2609(7) 0.19629(18) 0.81052(19) 0.0791(13) Uani 1 1 d . . . . . N1 N 0.2615(6) 0.29597(19) 0.7495(2) 0.0544(12) Uani 1 1 d . . . . . C15 C 1.0107(11) 0.4601(4) 0.8970(3) 0.084(2) Uani 1 1 d . . . . . H15 H 1.124185 0.479049 0.923207 0.101 Uiso 1 1 calc R U . . . C16 C 1.0252(9) 0.4004(3) 0.8762(3) 0.0708(17) Uani 1 1 d . . . . . H16 H 1.149072 0.378742 0.888150 0.085 Uiso 1 1 calc R U . . . C17 C 0.8567(9) 0.3721(3) 0.8375(3) 0.0592(15) Uani 1 1 d . . . . . H17 H 0.868503 0.331361 0.823895 0.071 Uiso 1 1 calc R U . . . C12 C 0.6698(8) 0.4034(3) 0.8184(3) 0.0549(14) Uani 1 1 d . . . . . C4 C 0.4474(8) 0.3112(3) 0.7897(3) 0.0576(14) Uani 1 1 d . . . . . H4 H 0.530034 0.284274 0.818850 0.069 Uiso 1 1 calc R U . . . C25 C 0.2953(8) 0.1884(2) 0.6779(3) 0.0551(14) Uani 1 1 d . . . . . C26 C 0.4990(9) 0.1672(3) 0.6922(3) 0.0782(19) Uani 1 1 d . . . . . H26 H 0.572289 0.171856 0.736940 0.094 Uiso 1 1 calc R U . . . C27 C 0.5916(10) 0.1391(3) 0.6390(4) 0.089(2) Uani 1 1 d . . . . . H27 H 0.728893 0.125022 0.648125 0.107 Uiso 1 1 calc R U . . . C28 C 0.4849(10) 0.1315(3) 0.5725(3) 0.0714(17) Uani 1 1 d . . . . . C31 C 0.5922(12) 0.1003(3) 0.5153(4) 0.118(3) Uani 1 1 d . . . . . H31A H 0.572076 0.056723 0.517723 0.177 Uiso 1 1 calc R U . . . H31B H 0.739583 0.109401 0.522186 0.177 Uiso 1 1 calc R U . . . H31C H 0.532860 0.115106 0.469971 0.177 Uiso 1 1 calc R U . . . C1 C 0.1821(8) 0.3487(3) 0.7123(3) 0.0539(14) Uani 1 1 d . . . . . C18 C -0.0194(8) 0.3507(3) 0.6637(3) 0.0690(17) Uani 1 1 d . . . . . H18B H -0.062436 0.393260 0.657804 0.083 Uiso 1 1 calc R U . . . H18A H -0.126312 0.329597 0.686449 0.083 Uiso 1 1 calc R U . . . C19 C -0.0146(9) 0.3230(3) 0.5915(3) 0.0648(16) Uani 1 1 d . . . . . C24 C -0.1910(10) 0.2953(3) 0.5574(4) 0.088(2) Uani 1 1 d . . . . . H24 H -0.311201 0.292327 0.580090 0.106 Uiso 1 1 calc R U . . . C22 C -0.0223(19) 0.2755(4) 0.4558(4) 0.108(3) Uani 1 1 d . . . . . H22 H -0.023652 0.259477 0.410580 0.130 Uiso 1 1 calc R U . . . C20 C 0.1609(10) 0.3273(3) 0.5572(3) 0.0745(17) Uani 1 1 d . . . . . H20 H 0.282946 0.345660 0.578564 0.089 Uiso 1 1 calc R U . . . C2 C 0.3203(8) 0.3950(3) 0.7310(3) 0.0559(14) Uani 1 1 d . . . . . C14 C 0.8280(12) 0.4919(3) 0.8790(3) 0.085(2) Uani 1 1 d . . . . . H14 H 0.818022 0.532507 0.893374 0.102 Uiso 1 1 calc R U . . . C13 C 0.6586(10) 0.4646(3) 0.8397(3) 0.0709(17) Uani 1 1 d . . . . . H13 H 0.536462 0.487070 0.827403 0.085 Uiso 1 1 calc R U . . . C5 C 0.3001(9) 0.4594(3) 0.7042(3) 0.0663(16) Uani 1 1 d . . . . . C11 C 0.4750(10) 0.4819(4) 0.6644(4) 0.104(3) Uani 1 1 d . . . . . H11B H 0.546909 0.514835 0.691490 0.125 Uiso 1 1 calc R U . . . H11A H 0.574840 0.448594 0.662786 0.125 Uiso 1 1 calc R U . . . C10 C 0.4206(16) 0.5035(5) 0.5940(5) 0.170(4) Uani 1 1 d . . . . . H10A H 0.342143 0.471139 0.567827 0.204 Uiso 1 1 calc R U . . . H10B H 0.550087 0.508761 0.573144 0.204 Uiso 1 1 calc R U . . . C9 C 0.296(2) 0.5618(5) 0.5817(6) 0.181(5) Uani 1 1 d . . . . . H9A H 0.280377 0.570779 0.531608 0.217 Uiso 1 1 calc R U . . . H9B H 0.376456 0.595116 0.605507 0.217 Uiso 1 1 calc R U . . . C8 C 0.081(2) 0.5608(5) 0.6065(6) 0.171(5) Uani 1 1 d . . . . . H8B H 0.007385 0.598133 0.590711 0.205 Uiso 1 1 calc R U . . . H8A H 0.002633 0.526488 0.584262 0.205 Uiso 1 1 calc R U . . . C7 C 0.0819(13) 0.5555(3) 0.6850(5) 0.124(3) Uani 1 1 d . . . . . H6B H 0.183494 0.584395 0.707679 0.149 Uiso 1 1 calc R U . . . H6A H -0.055102 0.567424 0.697063 0.149 Uiso 1 1 calc R U . . . C6 C 0.1326(10) 0.4930(3) 0.7143(3) 0.0794(18) Uani 1 1 d . . . . . H6 H 0.038535 0.475951 0.742275 0.095 Uiso 1 1 calc R U . . . C30 C 0.1862(10) 0.1804(3) 0.6120(3) 0.0710(17) Uani 1 1 d . . . . . H30 H 0.047623 0.193419 0.602739 0.085 Uiso 1 1 calc R U . . . C29 C 0.2853(11) 0.1529(3) 0.5597(3) 0.0804(19) Uani 1 1 d . . . . . H29 H 0.213512 0.148871 0.514650 0.096 Uiso 1 1 calc R U . . . C3 C 0.4910(8) 0.3710(3) 0.7801(2) 0.0520(13) Uani 1 1 d . . . . . C21 C 0.1504(15) 0.3031(3) 0.4888(3) 0.089(2) Uani 1 1 d . . . . . H21 H 0.268320 0.306253 0.465025 0.107 Uiso 0.454(10) 1 calc R U P A 1 O1B O -0.3263(14) 0.2521(5) 0.4442(5) 0.088(4) Uani 0.454(10) 1 d . . P A 1 H1B H -0.438273 0.248054 0.460384 0.132 Uiso 0.454(10) 1 calc R U P A 1 C23 C -0.1924(16) 0.2721(4) 0.4906(4) 0.101(3) Uani 1 1 d . . . . . H23 H -0.313602 0.253496 0.468861 0.121 Uiso 0.546(10) 1 calc R U P A 2 O1A O 0.2998(12) 0.3095(4) 0.4553(4) 0.087(3) Uani 0.546(10) 1 d . . P A 2 H1A H 0.284920 0.287226 0.420481 0.131 Uiso 0.546(10) 1 calc R U P A 2 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 0.0646(10) 0.0759(11) 0.0557(9) -0.0066(8) 0.0116(7) -0.0092(8) O2 0.049(2) 0.114(4) 0.095(3) -0.025(3) 0.011(2) -0.012(2) O3 0.106(3) 0.079(3) 0.052(2) 0.008(2) 0.007(2) -0.013(2) N1 0.052(3) 0.055(3) 0.053(3) -0.008(2) -0.004(2) -0.006(2) C15 0.078(5) 0.099(6) 0.074(4) -0.013(4) -0.001(4) -0.017(4) C16 0.059(4) 0.095(5) 0.058(4) 0.000(3) 0.003(3) -0.004(4) C17 0.067(4) 0.068(4) 0.043(3) 0.002(3) 0.007(3) 0.004(3) C12 0.062(4) 0.061(4) 0.043(3) 0.005(3) 0.010(3) 0.000(3) C4 0.060(4) 0.061(4) 0.049(3) -0.003(3) -0.003(3) 0.011(3) C25 0.057(3) 0.061(4) 0.048(3) -0.005(3) 0.009(3) -0.006(3) C26 0.057(4) 0.101(5) 0.074(4) -0.017(4) -0.004(3) -0.006(4) C27 0.057(4) 0.112(6) 0.098(5) -0.027(4) 0.013(4) -0.002(4) C28 0.086(5) 0.069(4) 0.062(4) -0.011(3) 0.020(3) -0.004(4) C31 0.154(7) 0.105(6) 0.104(6) -0.030(5) 0.053(5) 0.016(5) C1 0.053(3) 0.066(4) 0.043(3) -0.004(3) 0.004(2) 0.014(3) C18 0.062(4) 0.085(4) 0.058(3) -0.012(3) -0.002(3) 0.014(3) C19 0.073(4) 0.066(4) 0.050(3) -0.007(3) -0.012(3) 0.018(3) C24 0.075(5) 0.107(6) 0.075(4) -0.022(4) -0.023(3) 0.024(4) C22 0.169(9) 0.084(6) 0.059(5) -0.017(4) -0.040(6) 0.016(6) C20 0.091(5) 0.082(5) 0.049(3) 0.000(3) 0.005(3) 0.016(4) C2 0.052(3) 0.071(4) 0.044(3) 0.003(3) 0.004(2) 0.013(3) C14 0.097(5) 0.073(5) 0.085(5) -0.022(4) 0.005(4) -0.015(4) C13 0.071(4) 0.064(4) 0.076(4) -0.003(3) 0.002(3) 0.001(3) C5 0.063(4) 0.073(4) 0.061(4) 0.013(3) 0.002(3) 0.008(3) C11 0.082(5) 0.134(7) 0.100(5) 0.055(5) 0.025(4) 0.015(4) C10 0.178(10) 0.211(12) 0.130(8) 0.092(8) 0.060(7) 0.042(9) C9 0.192(12) 0.170(11) 0.181(11) 0.113(9) 0.023(10) 0.026(10) C8 0.188(12) 0.130(9) 0.177(12) 0.068(8) -0.046(10) 0.032(8) C7 0.122(7) 0.077(6) 0.167(9) 0.020(6) -0.007(6) 0.030(5) C6 0.079(4) 0.071(4) 0.088(5) 0.004(4) 0.005(3) 0.020(4) C30 0.083(4) 0.072(4) 0.054(4) -0.008(3) -0.005(3) 0.014(3) C29 0.108(6) 0.072(4) 0.058(4) -0.003(3) -0.004(4) 0.016(4) C3 0.053(3) 0.061(4) 0.043(3) -0.002(3) 0.004(2) 0.008(3) C21 0.135(7) 0.085(5) 0.053(4) 0.011(4) 0.030(5) 0.036(5) O1B 0.052(6) 0.138(9) 0.068(6) -0.028(6) -0.019(5) 0.005(5) C23 0.115(7) 0.092(6) 0.084(6) -0.019(5) -0.039(6) 0.030(5) O1A 0.074(6) 0.129(8) 0.058(5) -0.007(5) 0.000(4) 0.002(5) 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 O2 S1 O3 120.6(3) O2 S1 N1 107.5(3) O3 S1 N1 104.5(2) O2 S1 C25 109.9(3) O3 S1 C25 107.1(3) N1 S1 C25 106.2(2) C4 N1 C1 108.7(4) C4 N1 S1 121.2(4) C1 N1 S1 129.8(4) C16 C15 C14 119.6(6) C16 C15 H15 120.2 C14 C15 H15 120.2 C15 C16 C17 120.4(6) C15 C16 H16 119.8 C17 C16 H16 119.8 C16 C17 C12 121.2(6) C16 C17 H17 119.4 C12 C17 H17 119.4 C17 C12 C13 117.6(5) C17 C12 C3 119.6(5) C13 C12 C3 122.7(5) C3 C4 N1 109.6(5) C3 C4 H4 125.2 N1 C4 H4 125.2 C30 C25 C26 120.4(5) C30 C25 S1 120.1(4) C26 C25 S1 119.5(4) C27 C26 C25 118.7(6) C27 C26 H26 120.6 C25 C26 H26 120.6 C28 C27 C26 121.4(6) C28 C27 H27 119.3 C26 C27 H27 119.3 C29 C28 C27 118.7(6) C29 C28 C31 121.5(6) C27 C28 C31 119.8(6) C28 C31 H31A 109.5 C28 C31 H31B 109.5 H31A C31 H31B 109.5 C28 C31 H31C 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 C2 C1 N1 106.5(4) C2 C1 C18 128.8(5) N1 C1 C18 124.6(5) C1 C18 C19 116.4(4) C1 C18 H18B 108.2 C19 C18 H18B 108.2 C1 C18 H18A 108.2 C19 C18 H18A 108.2 H18B C18 H18A 107.3 C20 C19 C24 118.7(6) C20 C19 C18 121.1(6) C24 C19 C18 120.1(6) C23 C24 C19 121.0(7) C23 C24 H24 119.5 C19 C24 H24 119.5 C23 C22 C21 117.6(8) C23 C22 H22 121.2 C21 C22 H22 121.2 C19 C20 C21 117.9(7) C19 C20 H20 121.1 C21 C20 H20 121.1 C1 C2 C3 108.7(5) C1 C2 C5 125.3(5) C3 C2 C5 126.0(5) C15 C14 C13 121.0(6) C15 C14 H14 119.5 C13 C14 H14 119.5 C14 C13 C12 120.3(6) C14 C13 H13 119.9 C12 C13 H13 119.9 C6 C5 C2 120.3(5) C6 C5 C11 123.7(6) C2 C5 C11 116.0(5) C10 C11 C5 117.9(7) C10 C11 H11B 107.8 C5 C11 H11B 107.8 C10 C11 H11A 107.8 C5 C11 H11A 107.8 H11B C11 H11A 107.2 C11 C10 C9 119.5(10) C11 C10 H10A 107.4 C9 C10 H10A 107.4 C11 C10 H10B 107.4 C9 C10 H10B 107.4 H10A C10 H10B 107.0 C10 C9 C8 115.2(9) C10 C9 H9A 108.5 C8 C9 H9A 108.5 C10 C9 H9B 108.5 C8 C9 H9B 108.5 H9A C9 H9B 107.5 C7 C8 C9 114.6(9) C7 C8 H8B 108.6 C9 C8 H8B 108.6 C7 C8 H8A 108.6 C9 C8 H8A 108.6 H8B C8 H8A 107.6 C6 C7 C8 114.7(8) C6 C7 H6B 108.6 C8 C7 H6B 108.6 C6 C7 H6A 108.6 C8 C7 H6A 108.6 H6B C7 H6A 107.6 C5 C6 C7 126.2(7) C5 C6 H6 116.9 C7 C6 H6 116.9 C25 C30 C29 119.2(6) C25 C30 H30 120.4 C29 C30 H30 120.4 C28 C29 C30 121.5(6) C28 C29 H29 119.2 C30 C29 H29 119.2 C4 C3 C2 106.4(5) C4 C3 C12 124.0(5) C2 C3 C12 129.4(5) O1A C21 C22 117.2(9) O1A C21 C20 119.4(10) C22 C21 C20 123.3(8) C22 C21 H21 118.4 C20 C21 H21 118.4 C23 O1B H1B 109.5 O1B C23 C22 101.6(9) O1B C23 C24 136.3(11) C22 C23 C24 121.5(8) C22 C23 H23 119.2 C24 C23 H23 119.2 C21 O1A H1A 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 O2 1.424(4) S1 O3 1.443(4) S1 N1 1.669(4) S1 C25 1.749(5) N1 C4 1.381(6) N1 C1 1.413(6) C15 C16 1.365(9) C15 C14 1.371(8) C15 H15 0.9300 C16 C17 1.381(7) C16 H16 0.9300 C17 C12 1.391(7) C17 H17 0.9300 C12 C13 1.398(8) C12 C3 1.467(7) C4 C3 1.350(7) C4 H4 0.9300 C25 C30 1.378(7) C25 C26 1.383(7) C26 C27 1.380(8) C26 H26 0.9300 C27 C28 1.380(8) C27 H27 0.9300 C28 C29 1.358(8) C28 C31 1.518(8) C31 H31A 0.9600 C31 H31B 0.9600 C31 H31C 0.9600 C1 C2 1.362(7) C1 C18 1.501(7) C18 C19 1.509(7) C18 H18B 0.9700 C18 H18A 0.9700 C19 C20 1.372(8) C19 C24 1.376(8) C24 C23 1.373(10) C24 H24 0.9300 C22 C23 1.346(11) C22 C21 1.350(10) C22 H22 0.9300 C20 C21 1.402(8) C20 H20 0.9300 C2 C3 1.452(7) C2 C5 1.493(8) C14 C13 1.380(8) C14 H14 0.9300 C13 H13 0.9300 C5 C6 1.334(7) C5 C11 1.510(8) C11 C10 1.428(10) C11 H11B 0.9700 C11 H11A 0.9700 C10 C9 1.503(13) C10 H10A 0.9700 C10 H10B 0.9700 C9 C8 1.515(13) C9 H9A 0.9700 C9 H9B 0.9700 C8 C7 1.503(13) C8 H8B 0.9700 C8 H8A 0.9700 C7 C6 1.492(9) C7 H6B 0.9700 C7 H6A 0.9700 C6 H6 0.9300 C30 C29 1.383(8) C30 H30 0.9300 C29 H29 0.9300 C21 O1A 1.222(9) C21 H21 0.9300 O1B C23 1.238(10) O1B H1B 0.8200 C23 H23 0.9300 O1A H1A 0.8200 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 C4 156.8(4) O3 S1 N1 C4 27.5(4) C25 S1 N1 C4 -85.6(4) O2 S1 N1 C1 -29.4(5) O3 S1 N1 C1 -158.6(4) C25 S1 N1 C1 88.3(5) C14 C15 C16 C17 -0.3(9) C15 C16 C17 C12 0.4(8) C16 C17 C12 C13 0.1(7) C16 C17 C12 C3 -177.2(5) C1 N1 C4 C3 0.0(6) S1 N1 C4 C3 175.0(4) O2 S1 C25 C30 15.0(6) O3 S1 C25 C30 147.6(5) N1 S1 C25 C30 -101.1(5) O2 S1 C25 C26 -163.5(5) O3 S1 C25 C26 -30.8(5) N1 S1 C25 C26 80.5(5) C30 C25 C26 C27 1.2(10) S1 C25 C26 C27 179.6(5) C25 C26 C27 C28 -0.4(11) C26 C27 C28 C29 0.7(11) C26 C27 C28 C31 -180.0(7) C4 N1 C1 C2 -0.4(5) S1 N1 C1 C2 -174.8(4) C4 N1 C1 C18 -179.2(4) S1 N1 C1 C18 6.4(7) C2 C1 C18 C19 104.3(7) N1 C1 C18 C19 -77.2(7) C1 C18 C19 C20 -35.1(8) C1 C18 C19 C24 148.0(6) C20 C19 C24 C23 0.3(10) C18 C19 C24 C23 177.4(6) C24 C19 C20 C21 0.1(9) C18 C19 C20 C21 -176.9(5) N1 C1 C2 C3 0.6(5) C18 C1 C2 C3 179.3(5) N1 C1 C2 C5 179.7(5) C18 C1 C2 C5 -1.6(9) C16 C15 C14 C13 -0.4(10) C15 C14 C13 C12 0.9(10) C17 C12 C13 C14 -0.7(8) C3 C12 C13 C14 176.5(5) C1 C2 C5 C6 59.5(8) C3 C2 C5 C6 -121.6(6) C1 C2 C5 C11 -119.0(6) C3 C2 C5 C11 59.9(8) C6 C5 C11 C10 -55.6(11) C2 C5 C11 C10 122.8(8) C5 C11 C10 C9 67.9(13) C11 C10 C9 C8 -61.3(16) C10 C9 C8 C7 65.8(15) C9 C8 C7 C6 -75.2(12) C2 C5 C6 C7 -174.1(6) C11 C5 C6 C7 4.2(11) C8 C7 C6 C5 53.0(12) C26 C25 C30 C29 -2.2(9) S1 C25 C30 C29 179.4(5) C27 C28 C29 C30 -1.7(10) C31 C28 C29 C30 179.0(6) C25 C30 C29 C28 2.4(10) N1 C4 C3 C2 0.4(6) N1 C4 C3 C12 175.8(4) C1 C2 C3 C4 -0.6(6) C5 C2 C3 C4 -179.7(5) C1 C2 C3 C12 -175.7(5) C5 C2 C3 C12 5.2(8) C17 C12 C3 C4 33.7(7) C13 C12 C3 C4 -143.5(5) C17 C12 C3 C2 -152.0(5) C13 C12 C3 C2 30.9(8) C23 C22 C21 O1A -175.6(8) C23 C22 C21 C20 0.8(12) C19 C20 C21 O1A 175.6(7) C19 C20 C21 C22 -0.7(10) C21 C22 C23 O1B 172.1(8) C21 C22 C23 C24 -0.4(13) C19 C24 C23 O1B -169.5(11) C19 C24 C23 C22 -0.2(12)