#------------------------------------------------------------------------------ #$Date: 2024-10-04 01:08:23 +0300 (Fri, 04 Oct 2024) $ #$Revision: 295020 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/27/1572749.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_1572749 loop_ _publ_author_name 'Guo, Jia-Dong' 'Alemu Korsaye, Feven' 'Schutz, Dorian' 'Ciofini, Ilaria' 'Miesch, Laurence' _publ_section_title ; Photocatalyst-free, visible-light-induced regio- and stereoselective synthesis of phosphorylated enamines from N-allenamides via [1,3]-sulfonyl shift at room temperature ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC05190D _journal_year 2024 _chemical_formula_moiety 'C29 H28 N O3 P S' _chemical_formula_sum 'C29 H28 N O3 P S' _chemical_formula_weight 501.55 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2023-11-28 deposited with the CCDC. 2024-10-02 downloaded from the CCDC. ; _cell_angle_alpha 89.379(5) _cell_angle_beta 62.804(4) _cell_angle_gamma 74.413(5) _cell_formula_units_Z 2 _cell_length_a 11.2161(17) _cell_length_b 11.2502(18) _cell_length_c 11.6904(18) _cell_measurement_reflns_used 9094 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 66.21 _cell_measurement_theta_min 5.21 _cell_volume 1253.0(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2019/3(Sheldrick, 2019)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_device_type 'Bruker PHOTON-III CPAD' _diffrn_measurement_method '\f and \w shuterless scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_unetI/netI 0.0428 _diffrn_reflns_Laue_measured_fraction_full 0.976 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 20327 _diffrn_reflns_point_group_measured_fraction_full 0.976 _diffrn_reflns_point_group_measured_fraction_max 0.976 _diffrn_reflns_theta_full 66.843 _diffrn_reflns_theta_max 66.842 _diffrn_reflns_theta_min 4.641 _diffrn_source 'Cu-ImuS Diamond microfocus tube' _exptl_absorpt_coefficient_mu 2.005 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_correction_T_min 0.6157 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_meas ? _exptl_crystal_description block _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.404 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.068 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 4345 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0416 _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^)+(0.0979P)^2^+0.6588P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1345 _refine_ls_wR_factor_ref 0.1355 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4225 _reflns_number_total 4345 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc05190d2.cif _cod_data_source_block elmjdg231012 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_crystal_density_meas' value 'none' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_database_code 1572749 _shelx_shelxl_version_number 2018/3 _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 0.690 _shelx_estimated_absorpt_t_max 0.753 _shelx_res_file ; TITL elmjdg_a.res in P-1 elmjdg_a.res created by SHELXL-2018/3 at 09:48:59 on 28-Nov-2023 CELL 1.54178 11.2161 11.2502 11.6904 89.379 62.804 74.413 ZERR 2.000 0.0017 0.0018 0.0018 0.005 0.004 0.005 LATT 1 SFAC C H N O P S UNIT 58 56 2 6 2 2 OMIT 2 -2 2 OMIT 2 0 1 OMIT 1 -2 1 OMIT 0 -2 1 OMIT 1 -4 2 L.S. 10 ACTA BOND $H FMAP 2 PLAN 10 SIZE 0.20 0.18 0.15 CONF TEMP -153.150 WGHT 0.097900 0.658800 FVAR 1.15459 C1 1 0.484921 0.374317 0.738720 11.00000 0.01402 0.01673 = 0.01374 0.00239 -0.00546 -0.00595 S1 6 0.348456 0.474120 0.874668 11.00000 0.01408 0.01434 = 0.01406 0.00121 -0.00672 -0.00397 O1 4 0.407008 0.544650 0.926931 11.00000 0.02151 0.01759 = 0.02107 -0.00027 -0.01063 -0.00754 O2 4 0.238220 0.542252 0.845612 11.00000 0.01743 0.02054 = 0.01993 0.00300 -0.00969 -0.00244 C2 1 0.282307 0.372867 0.988611 11.00000 0.01508 0.01688 = 0.01247 0.00040 -0.00467 -0.00452 C3 1 0.168993 0.336026 0.999870 11.00000 0.01898 0.02497 = 0.01779 0.00158 -0.00977 -0.00733 AFIX 43 H3 2 0.121275 0.370313 0.952218 11.00000 -1.20000 AFIX 0 C4 1 0.126601 0.248621 1.081534 11.00000 0.01963 0.02738 = 0.02023 0.00114 -0.00734 -0.01158 AFIX 43 H4 2 0.047944 0.224573 1.090948 11.00000 -1.20000 AFIX 0 C5 1 0.197083 0.195330 1.150097 11.00000 0.02276 0.01962 = 0.01266 -0.00012 -0.00314 -0.00613 C6 1 0.310000 0.234242 1.137584 11.00000 0.01894 0.02196 = 0.01490 0.00066 -0.00735 -0.00183 AFIX 43 H6 2 0.358953 0.198713 1.183845 11.00000 -1.20000 AFIX 0 C7 1 0.352219 0.323746 1.058970 11.00000 0.01586 0.02126 = 0.01543 -0.00007 -0.00741 -0.00508 AFIX 43 H7 2 0.427630 0.351196 1.053122 11.00000 -1.20000 AFIX 0 C8 1 0.152654 0.097724 1.235759 11.00000 0.03276 0.02571 = 0.02404 0.00756 -0.00837 -0.01138 AFIX 137 H8A 2 0.065413 0.137207 1.315063 11.00000 -1.50000 H8B 2 0.226321 0.056409 1.258450 11.00000 -1.50000 H8C 2 0.137334 0.036083 1.189471 11.00000 -1.50000 AFIX 0 C9 1 0.606503 0.304017 0.760437 11.00000 0.01523 0.01823 = 0.01683 0.00424 -0.00759 -0.00641 AFIX 23 H9A 2 0.586837 0.227490 0.796949 11.00000 -1.20000 H9B 2 0.607751 0.355763 0.827610 11.00000 -1.20000 AFIX 0 P1 5 0.781319 0.258716 0.623249 11.00000 0.01325 0.01358 = 0.01296 -0.00025 -0.00606 -0.00359 O3 4 0.802415 0.157965 0.527708 11.00000 0.01896 0.01715 = 0.01875 -0.00197 -0.00981 -0.00357 C10 1 0.896304 0.212154 0.695348 11.00000 0.01579 0.01389 = 0.01587 0.00307 -0.00720 -0.00575 C11 1 0.865682 0.269890 0.815025 11.00000 0.01623 0.02077 = 0.01637 -0.00192 -0.00681 -0.00260 AFIX 43 H11 2 0.781111 0.335451 0.862171 11.00000 -1.20000 AFIX 0 C12 1 0.958829 0.231408 0.864890 11.00000 0.02285 0.03138 = 0.01832 0.00028 -0.01133 -0.00613 AFIX 43 H12 2 0.937609 0.270607 0.946298 11.00000 -1.20000 AFIX 0 C13 1 1.082666 0.136063 0.796490 11.00000 0.02213 0.02629 = 0.02663 0.00638 -0.01617 -0.00559 AFIX 43 H13 2 1.146413 0.110374 0.830701 11.00000 -1.20000 AFIX 0 C14 1 1.113351 0.078173 0.677848 11.00000 0.01709 0.01728 = 0.02791 0.00248 -0.01067 -0.00305 AFIX 43 H14 2 1.197958 0.012504 0.631257 11.00000 -1.20000 AFIX 0 C15 1 1.020860 0.115858 0.626950 11.00000 0.01837 0.01528 = 0.01719 0.00078 -0.00704 -0.00637 AFIX 43 H15 2 1.042395 0.076110 0.545673 11.00000 -1.20000 AFIX 0 C16 1 0.811166 0.396554 0.548189 11.00000 0.01194 0.01629 = 0.01716 0.00137 -0.00731 -0.00387 C17 1 0.798001 0.504004 0.617212 11.00000 0.01840 0.02083 = 0.01649 0.00103 -0.00824 -0.00558 AFIX 43 H17 2 0.769999 0.507488 0.707358 11.00000 -1.20000 AFIX 0 C18 1 0.826047 0.605481 0.553353 11.00000 0.02067 0.01715 = 0.02497 -0.00014 -0.01099 -0.00616 AFIX 43 H18 2 0.816957 0.678752 0.600124 11.00000 -1.20000 AFIX 0 C19 1 0.867335 0.600968 0.421545 11.00000 0.01695 0.02105 = 0.02755 0.00840 -0.01071 -0.00838 AFIX 43 H19 2 0.885778 0.671177 0.378655 11.00000 -1.20000 AFIX 0 C20 1 0.881651 0.494190 0.352553 11.00000 0.01831 0.02808 = 0.01678 0.00480 -0.00870 -0.00724 AFIX 43 H20 2 0.910859 0.490900 0.262196 11.00000 -1.20000 AFIX 0 C21 1 0.853327 0.391910 0.415395 11.00000 0.01694 0.02037 = 0.01697 0.00018 -0.00834 -0.00535 AFIX 43 H21 2 0.862603 0.318861 0.368160 11.00000 -1.20000 AFIX 0 C22 1 0.463578 0.364813 0.633805 11.00000 0.01662 0.01589 = 0.01798 0.00275 -0.00828 -0.00829 AFIX 43 H22 2 0.378464 0.418532 0.640854 11.00000 -1.20000 AFIX 0 N1 3 0.548378 0.288650 0.521650 11.00000 0.01843 0.01861 = 0.01607 0.00080 -0.00967 -0.00407 AFIX 43 H1 2 0.614932 0.223571 0.518215 11.00000 -1.20000 AFIX 0 C23 1 0.532673 0.311389 0.404742 11.00000 0.02410 0.01965 = 0.01546 0.00395 -0.01124 -0.00791 AFIX 23 H23A 2 0.605454 0.348834 0.346201 11.00000 -1.20000 H23B 2 0.439842 0.372105 0.429732 11.00000 -1.20000 AFIX 0 C24 1 0.545167 0.194400 0.332250 11.00000 0.01983 0.01738 = 0.01823 0.00286 -0.01279 -0.00461 C25 1 0.466699 0.114588 0.395237 11.00000 0.02817 0.02522 = 0.02090 0.00660 -0.01381 -0.01112 AFIX 43 H25 2 0.406095 0.132246 0.486137 11.00000 -1.20000 AFIX 0 C26 1 0.476075 0.009689 0.326737 11.00000 0.03582 0.02028 = 0.03292 0.00829 -0.02102 -0.01324 AFIX 43 H26 2 0.421681 -0.043785 0.370757 11.00000 -1.20000 AFIX 0 C27 1 0.564882 -0.017451 0.193783 11.00000 0.03085 0.01958 = 0.03355 -0.00496 -0.02078 -0.00243 AFIX 43 H27 2 0.572206 -0.089783 0.146853 11.00000 -1.20000 AFIX 0 C28 1 0.642513 0.061772 0.130384 11.00000 0.02545 0.02690 = 0.02280 -0.00395 -0.01176 -0.00159 AFIX 43 H28 2 0.702580 0.044150 0.039389 11.00000 -1.20000 AFIX 0 C29 1 0.633143 0.167222 0.199154 11.00000 0.02218 0.02241 = 0.02193 0.00299 -0.01211 -0.00633 AFIX 43 H29 2 0.687177 0.220857 0.154847 11.00000 -1.20000 AFIX 0 HKLF 4 REM elmjdg_a.res in P-1 REM wR2 = 0.135451, GooF = S = 1.02139, Restrained GooF = 1.02139 for all data REM R1 = 0.041605 for 4225 Fo > 4sig(Fo) and 0.042274 for all 4345 data REM 317 parameters refined using 0 restraints END WGHT 0.0725 0.7853 REM Highest difference peak 0.404, deepest hole -0.511, 1-sigma level 0.068 Q1 1 0.7877 0.3406 0.5910 11.00000 0.05 0.40 Q2 1 0.3033 0.4218 0.9439 11.00000 0.05 0.37 Q3 1 0.2206 0.0205 1.1950 11.00000 0.05 0.36 Q4 1 0.6385 0.2591 0.5130 11.00000 0.05 0.31 Q5 1 0.9752 0.1573 0.6515 11.00000 0.05 0.30 Q6 1 0.8731 0.2269 0.7545 11.00000 0.05 0.30 Q7 1 0.8450 0.5623 0.3980 11.00000 0.05 0.29 Q8 1 0.4398 0.3962 0.7955 11.00000 0.05 0.28 Q9 1 0.8406 0.2113 0.6727 11.00000 0.05 0.28 Q10 1 0.7549 0.1564 0.6194 11.00000 0.05 0.28 ; _shelx_res_checksum 4029 _shelx_hkl_file ; -1 0 0 1141.39 81.79 -2 0 0 331.17 23.50 -2 0 0 331.77 22.60 -2 0 0 270.07 22.60 2 0 0 330.47 22.60 2 0 0 309.57 22.70 -3 0 0 9729.83 694.13 -4 0 0 1962.20 143.19 -4 0 0 1978.90 141.69 4 0 0 1998.10 141.59 -5 0 0 686.13 50.39 -5 0 0 662.53 47.70 -5 0 0 563.94 47.50 5 0 0 706.13 48.00 5 0 0 724.83 47.80 5 0 0 626.24 47.50 -6 0 0 661.03 49.20 -6 0 0 622.84 45.50 -6 0 0 627.04 46.00 -6 0 0 610.14 46.30 -6 0 0 599.84 45.70 -6 0 0 653.23 45.50 6 0 0 632.34 45.50 6 0 0 619.94 45.90 6 0 0 648.44 45.60 6 0 0 618.54 45.50 -7 0 0 730.53 53.79 -7 0 0 756.42 53.99 -7 0 0 720.53 53.49 -7 0 0 731.73 58.49 7 0 0 768.32 53.59 7 0 0 673.83 53.89 7 0 0 750.12 53.49 7 0 0 778.42 53.59 -8 0 0 33.10 13.80 -8 0 0 35.20 4.00 -8 0 0 29.70 3.50 -8 0 0 32.40 3.90 8 0 0 33.30 3.40 8 0 0 28.90 3.40 8 0 0 35.30 3.60 8 0 0 39.90 3.50 -9 0 0 915.81 67.59 -9 0 0 911.41 67.29 -9 0 0 920.61 75.19 9 0 0 851.11 66.89 9 0 0 1014.10 67.29 9 0 0 951.60 67.19 -10 0 0 60.59 6.30 -10 0 0 69.89 6.00 10 0 0 80.19 6.10 10 0 0 69.89 5.80 -11 0 0 21.90 2.60 11 0 0 26.20 2.20 11 0 0 19.20 2.30 11 -1 0 33.00 2.50 11 -1 0 22.00 2.50 -11 1 0 30.30 2.90 10 -1 0 4.90 1.20 10 -1 0 5.10 1.00 -10 1 0 4.10 1.30 -10 1 0 5.00 1.50 9 -1 0 0.00 0.80 9 -1 0 0.80 0.80 -9 1 0 1.50 1.20 8 -1 0 39.60 4.10 8 -1 0 48.90 4.40 -8 1 0 45.10 19.30 -8 1 0 47.30 4.50 -8 1 0 38.80 4.60 -8 1 0 47.90 4.90 7 -1 0 436.36 31.80 7 -1 0 442.76 31.80 -7 1 0 454.95 32.20 -7 1 0 433.66 31.90 -7 1 0 440.56 32.40 -7 1 0 450.35 39.20 -7 1 0 389.26 31.70 6 -1 0 1567.34 118.29 6 -1 0 1586.94 118.19 -6 1 0 1707.33 118.39 -6 1 0 1679.03 118.59 -6 1 0 1634.74 118.79 -6 1 0 1743.63 122.59 5 -1 0 1480.15 103.19 5 -1 0 1463.45 102.79 -5 1 0 1264.77 102.79 -5 1 0 1484.45 105.99 -5 1 0 1493.75 102.89 -4 1 0 3588.34 258.07 3 -1 0 62.09 5.10 3 -1 0 61.19 4.90 -3 1 0 68.29 5.20 -3 1 0 64.99 4.90 -3 1 0 55.49 7.00 -2 1 0 5621.54 401.46 -1 -1 0 1469.15 104.89 -2 -1 0 2099.29 150.28 -3 -1 0 75.99 7.40 -3 -1 0 80.39 6.20 3 1 0 91.79 6.50 3 1 0 82.19 6.20 -4 -1 0 464.65 32.50 -4 -1 0 453.65 34.20 4 1 0 477.55 32.50 4 1 0 409.56 32.70 -5 -1 0 427.26 30.10 -5 -1 0 403.56 32.50 5 1 0 437.46 30.50 5 1 0 390.96 30.10 -6 -1 0 518.75 36.90 -6 -1 0 458.85 33.40 6 1 0 451.85 33.80 6 1 0 407.76 33.40 6 1 0 478.05 33.40 -7 -1 0 38.10 4.00 -7 -1 0 40.10 8.80 -7 -1 0 36.80 4.00 -7 -1 0 40.60 5.10 7 1 0 36.90 3.70 7 1 0 47.00 3.90 7 1 0 36.10 3.60 7 1 0 35.20 4.90 -8 -1 0 664.03 49.30 -8 -1 0 614.04 48.80 -8 -1 0 663.03 49.00 -8 -1 0 597.84 53.29 8 1 0 722.53 49.60 8 1 0 698.43 48.80 8 1 0 754.52 48.90 8 1 0 631.84 48.80 -9 -1 0 18.00 3.00 -9 -1 0 18.60 2.90 -9 -1 0 37.90 14.20 -9 -1 0 24.50 3.30 9 1 0 20.70 2.60 9 1 0 22.80 2.80 9 1 0 24.30 2.70 9 1 0 17.90 2.50 -10 -1 0 558.24 40.10 -10 -1 0 511.35 39.50 -10 -1 0 514.45 39.70 10 1 0 559.24 39.60 10 1 0 573.94 39.80 -11 -1 0 153.98 11.70 11 1 0 139.89 11.20 11 1 0 154.58 11.40 10 -2 0 2.60 0.70 10 -2 0 1.40 0.80 -10 2 0 1.70 1.10 -10 2 0 1.50 0.90 9 -2 0 134.09 9.70 9 -2 0 124.09 9.90 -9 2 0 114.39 10.30 -9 2 0 125.29 10.30 8 -2 0 354.36 27.40 8 -2 0 404.06 27.60 -8 2 0 399.16 27.70 -8 2 0 361.66 27.80 -8 2 0 374.56 28.00 -8 2 0 328.67 27.20 7 -2 0 111.39 9.60 7 -2 0 124.49 9.70 -7 2 0 125.99 9.90 -7 2 0 129.19 10.90 -7 2 0 126.39 10.20 -7 2 0 124.19 10.00 6 -2 0 32.80 3.50 6 -2 0 35.00 3.50 -6 2 0 34.70 3.40 -6 2 0 23.70 3.30 -6 2 0 28.80 4.30 5 -2 0 403.76 31.40 -5 2 0 407.46 35.80 -5 2 0 422.36 31.50 -5 2 0 487.55 31.70 4 -2 0 1059.09 72.79 4 -2 0 963.60 72.39 -4 2 0 1005.30 72.49 -4 2 0 1014.40 72.89 -4 2 0 980.50 75.29 -4 2 0 1040.10 72.89 3 -2 0 1845.82 127.79 -3 2 0 1717.73 129.59 -3 2 0 1795.32 128.09 2 -2 0 988.20 72.79 2 -2 0 1040.00 72.89 -2 2 0 985.50 74.19 -2 2 0 1059.49 72.99 1 -2 0 1168.08 83.39 0 -2 0 623.74 42.10 0 -2 0 616.84 42.30 0 2 0 524.75 41.90 -1 -2 0 483.85 32.90 -1 -2 0 410.06 32.70 1 2 0 456.65 32.60 1 2 0 423.86 32.60 1 2 0 514.65 32.60 -2 -2 0 1797.62 139.89 2 2 0 2112.69 139.49 -3 -2 0 22.40 2.00 -3 -2 0 20.10 3.00 3 2 0 18.60 1.90 3 2 0 20.40 1.70 -4 -2 0 27.00 4.30 -4 -2 0 31.00 2.50 4 2 0 25.60 2.40 4 2 0 32.40 2.90 -5 -2 0 1051.39 81.89 -5 -2 0 1212.08 79.99 5 2 0 1120.79 80.29 5 2 0 1075.69 79.99 -6 -2 0 81.59 9.90 -6 -2 0 84.19 6.50 6 2 0 87.59 6.70 6 2 0 84.89 6.50 6 2 0 69.29 6.80 -7 -2 0 165.58 13.20 -7 -2 0 147.69 13.50 -7 -2 0 179.68 12.70 -7 -2 0 151.18 12.20 -7 -2 0 168.88 16.80 -7 -2 0 154.88 12.60 7 2 0 162.18 12.20 7 2 0 159.28 12.80 7 2 0 158.18 12.30 -8 -2 0 2.20 2.20 -8 -2 0 3.50 1.30 -8 -2 0 5.40 6.80 -8 -2 0 3.30 1.40 -8 -2 0 7.50 1.80 8 2 0 4.10 1.30 8 2 0 3.70 1.10 8 2 0 3.40 1.40 8 2 0 1.20 0.80 8 2 0 3.20 1.30 -9 -2 0 17.30 2.80 -9 -2 0 22.00 2.90 -9 -2 0 17.10 19.40 -9 -2 0 15.50 2.70 9 2 0 14.40 3.00 9 2 0 19.20 2.50 9 2 0 18.90 2.70 9 2 0 20.00 2.50 9 2 0 15.40 2.30 -10 -2 0 540.15 54.59 -10 -2 0 707.63 48.20 -10 -2 0 661.13 48.40 10 2 0 628.64 47.80 10 2 0 712.63 48.20 -11 -2 0 21.30 2.70 11 2 0 26.30 2.50 11 2 0 20.10 2.50 10 -3 0 11.00 1.60 -10 3 0 16.70 2.00 -10 3 0 14.40 2.10 9 -3 0 1.00 0.90 9 -3 0 0.00 0.70 -9 3 0 -0.80 1.10 -9 3 0 0.60 0.90 8 -3 0 470.95 34.70 8 -3 0 408.76 35.50 -8 3 0 534.65 36.20 -8 3 0 547.75 36.00 -8 3 0 439.96 35.30 -8 3 0 460.15 34.80 6 -3 0 18.70 2.70 6 -3 0 18.90 2.10 6 -3 0 14.90 2.50 6 -3 0 11.40 1.90 -6 3 0 14.90 2.60 -6 3 0 17.10 2.80 -6 3 0 15.00 2.50 -6 3 0 22.40 2.40 5 -3 0 54.89 4.60 5 -3 0 63.39 5.20 5 -3 0 49.20 4.90 5 -3 0 47.50 4.70 -5 3 0 61.49 4.80 -5 3 0 58.99 4.90 4 -3 0 12.70 1.40 -4 3 0 11.40 1.80 -4 3 0 3.40 10.60 -4 3 0 11.10 1.50 3 -3 0 5.20 0.80 3 -3 0 4.00 0.90 -3 3 0 3.50 1.10 -3 3 0 0.70 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5.80 1.70 9 2 12 5.20 1.30 9 2 12 4.80 1.10 -10 -2 -12 127.39 10.10 -10 -2 -12 131.49 11.70 10 2 12 133.09 10.40 10 2 12 149.99 10.50 -11 -2 -12 296.57 22.50 -11 -2 -12 347.57 24.80 11 2 12 324.67 22.90 11 2 12 285.07 22.80 -1 -3 -12 4.70 1.60 1 3 12 3.50 1.00 1 3 12 3.70 0.90 -2 -3 -12 19.80 2.70 -4 -3 -12 55.19 4.20 4 3 12 42.00 4.50 4 3 12 50.69 4.70 -5 -3 -12 191.48 15.30 -5 -3 -12 237.98 16.10 5 3 12 205.58 15.80 5 3 12 194.38 15.80 -6 -3 -12 542.55 40.10 -6 -3 -12 595.34 39.70 -6 -3 -12 467.15 40.70 6 3 12 554.04 40.10 6 3 12 578.44 40.10 -7 -3 -12 398.76 29.40 7 3 12 419.86 29.90 7 3 12 397.96 29.90 -8 -3 -12 1.20 1.60 -8 -3 -12 2.10 1.10 -8 -3 -12 -0.90 1.40 8 3 12 0.70 0.90 8 3 12 1.80 0.90 -9 -3 -12 21.30 1.90 -9 -3 -12 21.90 4.50 -9 -3 -12 21.70 4.30 9 3 12 18.70 2.30 9 3 12 19.80 2.50 -10 -3 -12 121.99 11.60 -10 -3 -12 125.09 10.10 10 3 12 127.29 9.70 10 3 12 130.19 9.80 -11 -3 -12 14.90 3.00 11 3 12 13.30 1.60 -2 -4 -12 909.21 63.89 2 4 12 874.91 63.39 2 4 12 857.61 63.29 -3 -4 -12 1.00 1.20 -3 -4 -12 0.40 1.50 3 4 12 1.40 0.70 3 4 12 0.30 0.90 -4 -4 -12 17.60 3.00 -4 -4 -12 19.80 3.50 4 4 12 22.90 2.60 4 4 12 20.80 2.40 -5 -4 -12 8.60 2.10 -5 -4 -12 14.60 2.90 5 4 12 9.60 1.90 5 4 12 10.30 1.80 -6 -4 -12 30.70 4.20 -6 -4 -12 21.00 3.60 6 4 12 31.10 3.20 6 4 12 27.20 3.00 -7 -4 -12 100.09 8.50 7 4 12 87.59 7.30 7 4 12 85.59 7.40 -8 -4 -12 59.99 6.80 -8 -4 -12 74.89 6.40 8 4 12 82.49 6.40 8 4 12 80.99 6.20 -9 -4 -12 751.32 52.59 -9 -4 -12 672.13 51.79 9 4 12 707.23 51.79 9 4 12 737.03 51.89 -10 -4 -12 35.00 4.70 -10 -4 -12 29.40 3.40 10 4 12 30.50 3.20 10 4 12 26.50 2.80 -11 -4 -12 849.32 61.39 -3 -5 -12 49.30 4.70 -3 -5 -12 50.99 5.00 3 5 12 50.59 4.30 3 5 12 53.89 4.50 4 5 12 58.99 5.20 4 5 12 63.69 5.20 -5 -5 -12 11.40 2.90 5 5 12 11.10 1.70 5 5 12 14.50 2.00 -6 -5 -12 6.70 2.10 -6 -5 -12 5.90 1.80 6 5 12 7.00 1.20 6 5 12 5.60 1.40 -7 -5 -12 26.70 3.80 -7 -5 -12 24.60 4.00 7 5 12 24.00 2.70 7 5 12 27.50 2.70 -8 -5 -12 174.68 12.70 -8 -5 -12 152.58 14.00 8 5 12 160.88 12.50 8 5 12 167.38 12.50 -9 -5 -12 87.09 8.30 -9 -5 -12 103.59 9.50 -9 -5 -12 99.39 7.90 9 5 12 96.19 7.50 9 5 12 97.69 7.80 -10 -5 -12 258.67 18.70 -10 -5 -12 216.28 17.20 -10 -5 -12 223.98 16.70 10 5 12 197.88 16.40 10 5 12 229.98 16.70 -4 -6 -12 37.30 4.10 -4 -6 -12 37.40 3.80 4 6 12 33.90 3.30 -5 -6 -12 134.79 11.70 -5 -6 -12 156.58 11.40 5 6 12 145.49 11.10 -6 -6 -12 28.70 3.40 -6 -6 -12 33.60 4.00 6 6 12 32.80 3.10 -7 -6 -12 31.50 3.70 7 6 12 29.20 2.90 -8 -6 -12 224.08 20.00 -8 -6 -12 275.27 19.70 -8 -6 -12 282.27 20.70 8 6 12 267.57 19.50 -9 -6 -12 133.59 13.20 -9 -6 -12 170.28 12.10 -9 -6 -12 151.78 11.50 9 6 12 139.79 11.20 -3 4 -13 478.75 33.90 3 -4 13 476.35 33.60 3 -4 13 442.96 33.80 -4 4 -13 448.86 31.20 4 -4 13 384.46 30.80 4 -4 13 446.76 31.10 -5 4 -13 292.57 20.80 5 -4 13 272.77 20.40 5 -4 13 277.17 20.70 -6 4 -13 32.80 3.20 6 -4 13 29.40 3.10 6 -4 13 37.80 3.10 -3 3 -13 123.39 9.20 3 -3 13 105.89 9.00 3 -3 13 120.99 8.90 -4 3 -13 199.08 15.00 4 -3 13 189.98 14.90 4 -3 13 205.68 14.80 -5 3 -13 214.08 15.20 5 -3 13 203.88 15.00 5 -3 13 184.58 15.10 -6 3 -13 798.12 59.19 6 -3 13 842.72 59.09 -7 3 -13 0.20 0.60 7 -3 13 0.70 0.70 7 -3 13 0.30 0.50 2 -2 13 290.47 20.40 2 -2 13 265.47 20.50 3 -2 13 60.59 5.20 3 -2 13 56.19 4.90 -4 2 -13 1.40 0.80 4 -2 13 1.80 0.80 4 -2 13 2.50 1.00 -5 2 -13 13.60 1.90 5 -2 13 9.50 1.60 5 -2 13 9.40 1.70 -6 2 -13 163.98 12.60 -6 2 -13 160.78 12.40 6 -2 13 157.68 12.40 6 -2 13 161.08 12.30 -7 2 -13 79.69 6.80 7 -2 13 80.19 6.70 7 -2 13 89.09 6.70 -8 2 -13 110.19 8.30 8 -2 13 87.79 8.10 8 -2 13 116.99 8.20 2 -1 13 7.30 1.60 2 -1 13 10.20 1.40 3 -1 13 29.20 3.00 3 -1 13 28.40 2.90 4 -1 13 168.68 12.80 4 -1 13 153.08 12.30 -5 1 -13 746.03 53.99 5 -1 13 715.93 53.99 5 -1 13 776.92 53.99 -6 1 -13 3.30 1.50 -6 1 -13 5.20 1.20 6 -1 13 4.70 1.10 -7 1 -13 44.00 4.30 7 -1 13 49.40 4.40 -8 1 -13 311.57 23.70 8 -1 13 331.37 23.70 -9 1 -13 758.92 54.39 9 -1 13 751.62 54.39 4 0 13 229.68 17.10 4 0 13 210.28 16.20 -5 0 -13 1026.30 79.29 5 0 13 1022.10 79.29 5 0 13 1261.97 80.39 -6 0 -13 129.99 11.20 -6 0 -13 144.79 10.70 6 0 13 136.99 10.70 -7 0 -13 5.00 1.80 7 0 13 3.80 1.30 7 0 13 5.60 1.30 -8 0 -13 22.10 3.90 -8 0 -13 16.20 2.00 8 0 13 19.90 2.20 8 0 13 17.00 2.10 -9 0 -13 101.59 8.10 9 0 13 108.39 8.20 3 1 13 83.69 6.70 3 1 13 87.69 6.90 -4 -1 -13 324.17 23.50 4 1 13 329.07 23.70 4 1 13 308.47 23.80 -5 -1 -13 127.09 9.10 5 1 13 109.59 8.60 5 1 13 90.49 9.00 -6 -1 -13 1019.00 73.19 6 1 13 993.50 72.79 6 1 13 1023.00 73.29 -7 -1 -13 127.19 9.80 7 1 13 142.79 10.20 7 1 13 110.19 9.70 -8 -1 -13 92.79 7.20 -8 -1 -13 100.09 7.80 8 1 13 83.69 7.30 8 1 13 89.29 7.60 -9 -1 -13 94.99 7.30 -9 -1 -13 90.19 7.60 9 1 13 96.59 7.50 9 1 13 98.69 7.40 -3 -2 -13 30.90 2.50 3 2 13 28.70 2.70 3 2 13 25.10 2.70 -4 -2 -13 0.50 0.50 4 2 13 1.40 0.90 4 2 13 0.30 0.70 -5 -2 -13 10.20 1.30 -5 -2 -13 7.50 2.20 5 2 13 7.90 1.60 5 2 13 6.30 1.30 -6 -2 -13 280.77 19.70 -6 -2 -13 272.07 21.20 6 2 13 247.68 19.90 6 2 13 275.67 20.00 -7 -2 -13 49.99 4.10 7 2 13 50.79 4.40 7 2 13 48.10 4.40 -8 -2 -13 599.24 38.20 -8 -2 -13 449.95 37.10 8 2 13 522.35 37.50 8 2 13 495.95 37.60 -9 -2 -13 696.43 57.59 -9 -2 -13 827.52 59.09 9 2 13 835.62 57.19 9 2 13 816.52 57.19 -4 -3 -13 25.30 3.40 4 3 13 24.90 2.60 4 3 13 25.20 2.50 -5 -3 -13 377.06 29.00 5 3 13 395.06 28.30 -6 -3 -13 2.90 1.70 -6 -3 -13 2.70 1.80 6 3 13 6.40 1.30 6 3 13 4.50 1.10 -7 -3 -13 151.18 12.00 -7 -3 -13 145.59 11.50 7 3 13 128.79 10.60 7 3 13 129.39 10.60 -8 -3 -13 10.20 2.70 -8 -3 -13 10.20 2.20 8 3 13 7.60 1.30 -9 -3 -13 20.80 2.60 -9 -3 -13 13.90 3.00 9 3 13 19.60 2.00 9 3 13 17.10 2.10 -5 -4 -13 765.82 52.59 5 4 13 655.93 51.79 5 4 13 736.73 51.99 -6 -4 -13 0.40 1.20 -6 -4 -13 -1.00 1.00 6 4 13 0.70 0.80 6 4 13 0.80 0.80 -7 -4 -13 85.99 7.20 7 4 13 73.89 6.50 7 4 13 79.39 6.40 -8 -4 -13 48.30 5.70 -8 -4 -13 56.49 5.40 8 4 13 56.99 4.80 8 4 13 67.29 4.90 -9 -4 -13 2.10 1.50 -9 -4 -13 1.70 1.20 9 4 13 1.20 0.80 9 4 13 2.30 0.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 61875 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.48492(17) 0.37432(16) 0.73872(16) 0.0150(4) Uani 1 1 d . . . . . S1 S 0.34846(4) 0.47412(4) 0.87467(4) 0.01417(16) Uani 1 1 d . . . . . O1 O 0.40701(13) 0.54465(12) 0.92693(12) 0.0194(3) Uani 1 1 d . . . . . O2 O 0.23822(13) 0.54225(12) 0.84561(12) 0.0196(3) Uani 1 1 d . . . . . C2 C 0.28231(18) 0.37287(16) 0.98861(16) 0.0156(4) Uani 1 1 d . . . . . C3 C 0.16899(19) 0.33603(18) 0.99987(18) 0.0199(4) Uani 1 1 d . . . . . H3 H 0.121275 0.370313 0.952218 0.024 Uiso 1 1 calc R U . . . C4 C 0.1266(2) 0.24862(18) 1.08153(18) 0.0222(4) Uani 1 1 d . . . . . H4 H 0.047944 0.224573 1.090948 0.027 Uiso 1 1 calc R U . . . C5 C 0.1971(2) 0.19533(17) 1.15010(17) 0.0205(4) Uani 1 1 d . . . . . C6 C 0.31000(19) 0.23424(18) 1.13758(18) 0.0198(4) Uani 1 1 d . . . . . H6 H 0.358953 0.198713 1.183845 0.024 Uiso 1 1 calc R U . . . C7 C 0.35222(19) 0.32375(17) 1.05897(17) 0.0176(4) Uani 1 1 d . . . . . H7 H 0.427630 0.351196 1.053122 0.021 Uiso 1 1 calc R U . . . C8 C 0.1527(2) 0.09772(19) 1.2358(2) 0.0290(5) Uani 1 1 d . . . . . H8A H 0.065413 0.137207 1.315063 0.043 Uiso 1 1 calc R U . . . H8B H 0.226321 0.056409 1.258450 0.043 Uiso 1 1 calc R U . . . H8C H 0.137334 0.036083 1.189471 0.043 Uiso 1 1 calc R U . . . C9 C 0.60650(18) 0.30402(16) 0.76044(17) 0.0164(4) Uani 1 1 d . . . . . H9A H 0.586837 0.227490 0.796949 0.020 Uiso 1 1 calc R U . . . H9B H 0.607751 0.355763 0.827610 0.020 Uiso 1 1 calc R U . . . P1 P 0.78132(4) 0.25872(4) 0.62325(4) 0.01338(16) Uani 1 1 d . . . . . O3 O 0.80242(13) 0.15796(11) 0.52771(12) 0.0183(3) Uani 1 1 d . . . . . C10 C 0.89630(18) 0.21215(16) 0.69535(17) 0.0150(4) Uani 1 1 d . . . . . C11 C 0.86568(19) 0.26989(17) 0.81502(17) 0.0187(4) Uani 1 1 d . . . . . H11 H 0.781111 0.335451 0.862171 0.022 Uiso 1 1 calc R U . . . C12 C 0.9588(2) 0.23141(19) 0.86489(19) 0.0239(4) Uani 1 1 d . . . . . H12 H 0.937609 0.270607 0.946298 0.029 Uiso 1 1 calc R U . . . C13 C 1.0827(2) 0.13606(18) 0.79649(19) 0.0235(4) Uani 1 1 d . . . . . H13 H 1.146413 0.110374 0.830701 0.028 Uiso 1 1 calc R U . . . C14 C 1.11335(19) 0.07817(17) 0.67785(19) 0.0212(4) Uani 1 1 d . . . . . H14 H 1.197958 0.012504 0.631257 0.025 Uiso 1 1 calc R U . . . C15 C 1.02086(18) 0.11586(16) 0.62695(17) 0.0172(4) Uani 1 1 d . . . . . H15 H 1.042395 0.076110 0.545673 0.021 Uiso 1 1 calc R U . . . C16 C 0.81117(17) 0.39655(16) 0.54819(17) 0.0150(4) Uani 1 1 d . . . . . C17 C 0.79800(18) 0.50400(17) 0.61721(17) 0.0186(4) Uani 1 1 d . . . . . H17 H 0.769999 0.507488 0.707358 0.022 Uiso 1 1 calc R U . . . C18 C 0.82605(19) 0.60548(17) 0.55335(19) 0.0207(4) Uani 1 1 d . . . . . H18 H 0.816957 0.678752 0.600124 0.025 Uiso 1 1 calc R U . . . C19 C 0.86734(19) 0.60097(18) 0.42154(19) 0.0212(4) Uani 1 1 d . . . . . H19 H 0.885778 0.671177 0.378655 0.025 Uiso 1 1 calc R U . . . C20 C 0.88165(19) 0.49419(19) 0.35255(18) 0.0208(4) Uani 1 1 d . . . . . H20 H 0.910859 0.490900 0.262196 0.025 Uiso 1 1 calc R U . . . C21 C 0.85333(18) 0.39191(17) 0.41540(17) 0.0180(4) Uani 1 1 d . . . . . H21 H 0.862603 0.318861 0.368160 0.022 Uiso 1 1 calc R U . . . C22 C 0.46358(18) 0.36481(16) 0.63381(17) 0.0160(4) Uani 1 1 d . . . . . H22 H 0.378464 0.418532 0.640854 0.019 Uiso 1 1 calc R U . . . N1 N 0.54838(16) 0.28865(14) 0.52165(14) 0.0174(3) Uani 1 1 d . . . . . H1 H 0.614932 0.223571 0.518215 0.021 Uiso 1 1 calc R U . . . C23 C 0.5327(2) 0.31139(17) 0.40474(17) 0.0187(4) Uani 1 1 d . . . . . H23A H 0.605454 0.348834 0.346201 0.022 Uiso 1 1 calc R U . . . H23B H 0.439842 0.372105 0.429732 0.022 Uiso 1 1 calc R U . . . C24 C 0.54517(19) 0.19440(17) 0.33225(17) 0.0171(4) Uani 1 1 d . . . . . C25 C 0.4667(2) 0.11459(18) 0.39524(19) 0.0232(4) Uani 1 1 d . . . . . H25 H 0.406095 0.132246 0.486137 0.028 Uiso 1 1 calc R U . . . C26 C 0.4761(2) 0.00969(18) 0.3267(2) 0.0267(4) Uani 1 1 d . . . . . H26 H 0.421681 -0.043785 0.370757 0.032 Uiso 1 1 calc R U . . . C27 C 0.5649(2) -0.01745(18) 0.1938(2) 0.0268(4) Uani 1 1 d . . . . . H27 H 0.572206 -0.089783 0.146853 0.032 Uiso 1 1 calc R U . . . C28 C 0.6425(2) 0.06177(19) 0.1304(2) 0.0262(4) Uani 1 1 d . . . . . H28 H 0.702580 0.044150 0.039389 0.031 Uiso 1 1 calc R U . . . C29 C 0.6331(2) 0.16722(18) 0.19915(19) 0.0215(4) Uani 1 1 d . . . . . H29 H 0.687177 0.220857 0.154847 0.026 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 C1 0.0140(8) 0.0167(8) 0.0137(8) 0.0024(7) -0.0055(7) -0.0060(7) S1 0.0141(2) 0.0143(3) 0.0141(3) 0.00121(17) -0.00672(19) -0.00397(18) O1 0.0215(7) 0.0176(6) 0.0211(7) -0.0003(5) -0.0106(6) -0.0075(5) O2 0.0174(6) 0.0205(7) 0.0199(7) 0.0030(5) -0.0097(5) -0.0024(5) C2 0.0151(8) 0.0169(9) 0.0125(8) 0.0004(7) -0.0047(7) -0.0045(7) C3 0.0190(9) 0.0250(10) 0.0178(9) 0.0016(7) -0.0098(7) -0.0073(7) C4 0.0196(9) 0.0274(10) 0.0202(9) 0.0011(8) -0.0073(8) -0.0116(8) C5 0.0228(9) 0.0196(9) 0.0127(8) -0.0001(7) -0.0031(7) -0.0061(7) C6 0.0189(9) 0.0220(9) 0.0149(8) 0.0007(7) -0.0073(7) -0.0018(7) C7 0.0159(8) 0.0213(9) 0.0154(8) -0.0001(7) -0.0074(7) -0.0051(7) C8 0.0328(11) 0.0257(10) 0.0240(10) 0.0076(8) -0.0084(9) -0.0114(9) C9 0.0152(8) 0.0182(9) 0.0168(9) 0.0042(7) -0.0076(7) -0.0064(7) P1 0.0133(3) 0.0136(3) 0.0130(3) -0.00025(18) -0.00606(19) -0.00359(18) O3 0.0190(6) 0.0172(6) 0.0187(6) -0.0020(5) -0.0098(5) -0.0036(5) C10 0.0158(8) 0.0139(8) 0.0159(8) 0.0031(7) -0.0072(7) -0.0057(7) C11 0.0162(9) 0.0208(9) 0.0164(9) -0.0019(7) -0.0068(7) -0.0026(7) C12 0.0228(10) 0.0314(11) 0.0183(9) 0.0003(8) -0.0113(8) -0.0061(8) C13 0.0221(9) 0.0263(10) 0.0266(10) 0.0064(8) -0.0162(8) -0.0056(8) C14 0.0171(9) 0.0173(9) 0.0279(10) 0.0025(7) -0.0107(8) -0.0031(7) C15 0.0184(9) 0.0153(8) 0.0172(9) 0.0008(7) -0.0070(7) -0.0064(7) C16 0.0119(8) 0.0163(9) 0.0172(9) 0.0014(7) -0.0073(7) -0.0039(7) C17 0.0184(9) 0.0208(9) 0.0165(9) 0.0010(7) -0.0082(7) -0.0056(7) C18 0.0207(9) 0.0172(9) 0.0250(10) -0.0001(7) -0.0110(8) -0.0062(7) C19 0.0169(9) 0.0210(9) 0.0275(10) 0.0084(8) -0.0107(8) -0.0084(7) C20 0.0183(9) 0.0281(10) 0.0168(9) 0.0048(8) -0.0087(7) -0.0072(8) C21 0.0169(8) 0.0204(9) 0.0170(9) 0.0002(7) -0.0083(7) -0.0053(7) C22 0.0166(8) 0.0159(8) 0.0180(9) 0.0028(7) -0.0083(7) -0.0083(7) N1 0.0184(7) 0.0186(7) 0.0161(7) 0.0008(6) -0.0097(6) -0.0041(6) C23 0.0241(9) 0.0197(9) 0.0155(9) 0.0039(7) -0.0112(8) -0.0079(7) C24 0.0198(9) 0.0174(9) 0.0182(9) 0.0029(7) -0.0128(7) -0.0046(7) C25 0.0282(10) 0.0252(10) 0.0209(9) 0.0066(8) -0.0138(8) -0.0111(8) C26 0.0358(11) 0.0203(10) 0.0329(11) 0.0083(8) -0.0210(9) -0.0132(8) C27 0.0309(11) 0.0196(10) 0.0336(11) -0.0050(8) -0.0208(9) -0.0024(8) C28 0.0254(10) 0.0269(10) 0.0228(10) -0.0039(8) -0.0118(8) -0.0016(8) C29 0.0222(9) 0.0224(9) 0.0219(10) 0.0030(7) -0.0121(8) -0.0063(8) 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' P P 0.2955 0.4335 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C22 C1 C9 130.00(16) . . ? C22 C1 S1 116.68(13) . . ? C9 C1 S1 113.16(12) . . ? O1 S1 O2 118.02(8) . . ? O1 S1 C1 108.54(8) . . ? O2 S1 C1 110.29(8) . . ? O1 S1 C2 106.78(8) . . ? O2 S1 C2 108.26(8) . . ? C1 S1 C2 103.98(8) . . ? C3 C2 C7 120.81(16) . . ? C3 C2 S1 120.11(14) . . ? C7 C2 S1 118.90(13) . . ? C4 C3 C2 119.11(17) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 121.29(17) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C6 118.48(17) . . ? C4 C5 C8 120.87(17) . . ? C6 C5 C8 120.65(17) . . ? C7 C6 C5 121.29(17) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C2 118.97(16) . . ? C6 C7 H7 120.5 . . ? C2 C7 H7 120.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C1 C9 P1 118.51(12) . . ? C1 C9 H9A 107.7 . . ? P1 C9 H9A 107.7 . . ? C1 C9 H9B 107.7 . . ? P1 C9 H9B 107.7 . . ? H9A C9 H9B 107.1 . . ? O3 P1 C16 111.19(8) . . ? O3 P1 C10 112.65(8) . . ? C16 P1 C10 107.80(8) . . ? O3 P1 C9 112.95(8) . . ? C16 P1 C9 107.61(8) . . ? C10 P1 C9 104.24(8) . . ? C15 C10 C11 119.49(16) . . ? C15 C10 P1 117.99(13) . . ? C11 C10 P1 122.51(13) . . ? C12 C11 C10 120.03(17) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 120.33(17) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.87(17) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C15 120.32(17) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C10 119.96(17) . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? C17 C16 C21 119.85(16) . . ? C17 C16 P1 122.30(13) . . ? C21 C16 P1 117.82(13) . . ? C18 C17 C16 119.56(17) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 120.54(17) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 120.05(17) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.04(17) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C16 119.95(17) . . ? C20 C21 H21 120.0 . . ? C16 C21 H21 120.0 . . ? N1 C22 C1 127.83(17) . . ? N1 C22 H22 116.1 . . ? C1 C22 H22 116.1 . . ? C22 N1 C23 121.56(15) . . ? C22 N1 H1 119.2 . . ? C23 N1 H1 119.2 . . ? N1 C23 C24 112.99(14) . . ? N1 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? N1 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C29 C24 C25 118.85(17) . . ? C29 C24 C23 119.71(16) . . ? C25 C24 C23 121.40(17) . . ? C26 C25 C24 120.73(18) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 120.17(18) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 119.45(18) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 120.42(19) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C24 C29 C28 120.38(18) . . ? C24 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C22 1.363(2) . ? C1 C9 1.511(2) . ? C1 S1 1.7381(18) . ? S1 O1 1.4462(13) . ? S1 O2 1.4493(13) . ? S1 C2 1.7721(17) . ? C2 C3 1.390(3) . ? C2 C7 1.394(3) . ? C3 C4 1.386(3) . ? C3 H3 0.9500 . ? C4 C5 1.393(3) . ? C4 H4 0.9500 . ? C5 C6 1.394(3) . ? C5 C8 1.507(3) . ? C6 C7 1.386(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 P1 1.8118(18) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? P1 O3 1.4933(13) . ? P1 C16 1.8077(17) . ? P1 C10 1.8081(18) . ? C10 C15 1.396(3) . ? C10 C11 1.399(2) . ? C11 C12 1.388(3) . ? C11 H11 0.9500 . ? C12 C13 1.386(3) . ? C12 H12 0.9500 . ? C13 C14 1.389(3) . ? C13 H13 0.9500 . ? C14 C15 1.390(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.397(2) . ? C16 C21 1.398(3) . ? C17 C18 1.385(3) . ? C17 H17 0.9500 . ? C18 C19 1.389(3) . ? C18 H18 0.9500 . ? C19 C20 1.385(3) . ? C19 H19 0.9500 . ? C20 C21 1.389(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 N1 1.343(2) . ? C22 H22 0.9500 . ? N1 C23 1.467(2) . ? N1 H1 0.8800 . ? C23 C24 1.512(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C29 1.390(3) . ? C24 C25 1.393(3) . ? C25 C26 1.386(3) . ? C25 H25 0.9500 . ? C26 C27 1.390(3) . ? C26 H26 0.9500 . ? C27 C28 1.384(3) . ? C27 H27 0.9500 . ? C28 C29 1.393(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C22 C1 S1 O1 -137.24(14) . . . . ? C9 C1 S1 O1 46.89(14) . . . . ? C22 C1 S1 O2 -6.52(16) . . . . ? C9 C1 S1 O2 177.61(11) . . . . ? C22 C1 S1 C2 109.35(14) . . . . ? C9 C1 S1 C2 -66.52(13) . . . . ? O1 S1 C2 C3 150.74(15) . . . . ? O2 S1 C2 C3 22.70(17) . . . . ? C1 S1 C2 C3 -94.59(16) . . . . ? O1 S1 C2 C7 -34.11(16) . . . . ? O2 S1 C2 C7 -162.16(14) . . . . ? C1 S1 C2 C7 80.55(15) . . . . ? C7 C2 C3 C4 -0.5(3) . . . . ? S1 C2 C3 C4 174.54(14) . . . . ? C2 C3 C4 C5 -1.4(3) . . . . ? C3 C4 C5 C6 1.6(3) . . . . ? C3 C4 C5 C8 -178.27(17) . . . . ? C4 C5 C6 C7 0.0(3) . . . . ? C8 C5 C6 C7 179.88(17) . . . . ? C5 C6 C7 C2 -1.8(3) . . . . ? C3 C2 C7 C6 2.1(3) . . . . ? S1 C2 C7 C6 -173.05(13) . . . . ? C22 C1 C9 P1 34.4(2) . . . . ? S1 C1 C9 P1 -150.40(10) . . . . ? C1 C9 P1 O3 -70.41(14) . . . . ? C1 C9 P1 C16 52.69(15) . . . . ? C1 C9 P1 C10 166.98(13) . . . . ? O3 P1 C10 C15 23.55(16) . . . . ? C16 P1 C10 C15 -99.49(14) . . . . ? C9 P1 C10 C15 146.36(14) . . . . ? O3 P1 C10 C11 -157.30(14) . . . . ? C16 P1 C10 C11 79.66(16) . . . . ? C9 P1 C10 C11 -34.50(17) . . . . ? C15 C10 C11 C12 0.0(3) . . . . ? P1 C10 C11 C12 -179.09(14) . . . . ? C10 C11 C12 C13 0.2(3) . . . . ? C11 C12 C13 C14 -0.4(3) . . . . ? C12 C13 C14 C15 0.4(3) . . . . ? C13 C14 C15 C10 -0.1(3) . . . . ? C11 C10 C15 C14 -0.1(3) . . . . ? P1 C10 C15 C14 179.10(13) . . . . ? O3 P1 C16 C17 179.98(13) . . . . ? C10 P1 C16 C17 -56.09(16) . . . . ? C9 P1 C16 C17 55.81(16) . . . . ? O3 P1 C16 C21 -2.18(16) . . . . ? C10 P1 C16 C21 121.75(14) . . . . ? C9 P1 C16 C21 -126.35(14) . . . . ? C21 C16 C17 C18 0.4(3) . . . . ? P1 C16 C17 C18 178.23(13) . . . . ? C16 C17 C18 C19 -0.1(3) . . . . ? C17 C18 C19 C20 -0.4(3) . . . . ? C18 C19 C20 C21 0.7(3) . . . . ? C19 C20 C21 C16 -0.4(3) . . . . ? C17 C16 C21 C20 -0.2(3) . . . . ? P1 C16 C21 C20 -178.06(13) . . . . ? C9 C1 C22 N1 -0.2(3) . . . . ? S1 C1 C22 N1 -175.24(14) . . . . ? C1 C22 N1 C23 -162.57(17) . . . . ? C22 N1 C23 C24 -136.85(17) . . . . ? N1 C23 C24 C29 -131.05(17) . . . . ? N1 C23 C24 C25 51.1(2) . . . . ? C29 C24 C25 C26 0.1(3) . . . . ? C23 C24 C25 C26 178.00(17) . . . . ? C24 C25 C26 C27 0.3(3) . . . . ? C25 C26 C27 C28 -0.7(3) . . . . ? C26 C27 C28 C29 0.7(3) . . . . ? C25 C24 C29 C28 -0.1(3) . . . . ? C23 C24 C29 C28 -178.04(17) . . . . ? C27 C28 C29 C24 -0.3(3) . . . . ?