#------------------------------------------------------------------------------ #$Date: 2020-08-22 05:15:44 +0300 (Sat, 22 Aug 2020) $ #$Revision: 255575 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705232.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_7705232 loop_ _publ_author_name 'Sha, Fanrui' 'Shimizu, Emily A.' 'Slocumb, Hannah S.' 'Towell, Sydney E.' 'Zhen, Yi' 'Porter, Hanna Z.' 'Takase, Michael' 'Johnson, Adam' _publ_section_title ; Catalytic intramolecular hydroamination of aminoallenes using titanium and tantalum complexes of sterically encumbered chiral sulfonamides ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02557G _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C28 H27 N O3 S' _chemical_formula_sum 'C28 H27 N O3 S' _chemical_formula_weight 457.56 _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 mixed _atom_sites_solution_primary dual _audit_creation_date 2020-07-20 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739) ; _audit_update_record ; 2020-07-20 deposited with the CCDC. 2020-08-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.775(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.1955(3) _cell_length_b 15.8730(5) _cell_length_c 16.3458(5) _cell_measurement_reflns_used 16528 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 24.1390 _cell_measurement_theta_min 1.8710 _cell_volume 2383.04(13) _computing_cell_refinement 'CrysAlisPro 1.171.40.55a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.55a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.55a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'Hy-Pix Bantam HPC detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -74.00 110.00 0.50 180.00 -- 20.00 54.00 -18.04 368 2 \w -74.00 110.00 0.50 180.00 -- 20.00 54.00 65.02 368 3 \w -74.00 110.00 0.50 180.00 -- 20.00 54.00 65.02 368 4 \w -74.00 110.00 0.50 180.00 -- 20.00 54.00 122.62 368 5 \w -74.00 110.00 0.50 180.00 -- 20.00 54.00 122.62 368 6 \w -74.00 110.00 0.50 180.00 -- 20.00 54.00 162.31 368 7 \w -74.00 110.00 0.50 180.00 -- 20.00 54.00 -98.09 368 8 \w -74.00 110.00 0.50 180.00 -- 20.00 54.00 39.60 368 9 \w -74.00 105.50 0.50 180.00 -- 20.00 54.00 107.21 359 ; _diffrn_measurement_device 'two-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Mini II' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0704790000 _diffrn_orient_matrix_UB_12 -0.0070219000 _diffrn_orient_matrix_UB_13 0.0144747000 _diffrn_orient_matrix_UB_21 -0.0309783000 _diffrn_orient_matrix_UB_22 0.0072167000 _diffrn_orient_matrix_UB_23 -0.0399969000 _diffrn_orient_matrix_UB_31 0.0062783000 _diffrn_orient_matrix_UB_32 -0.0435089000 _diffrn_orient_matrix_UB_33 -0.0089272000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_unetI/netI 0.0592 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 72070 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.959 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.856 _diffrn_reflns_theta_min 2.217 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.166 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_correction_T_min 0.953 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.55a (Rigaku Oxford Diffraction, 2019) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.275 _exptl_crystal_description block _exptl_crystal_F_000 968 _exptl_crystal_size_max 0.407 _exptl_crystal_size_mid 0.182 _exptl_crystal_size_min 0.139 _refine_diff_density_max 0.296 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.039 _refine_ls_abs_structure_details ; Flack x determined using 3335 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 603 _refine_ls_number_reflns 14398 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.016 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0562 _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^)+(0.0441P)^2^+0.3463P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0993 _refine_ls_wR_factor_ref 0.1117 _reflns_Friedel_coverage 0.905 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.942 _reflns_number_gt 9831 _reflns_number_total 14398 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL exp_277_a.res in P2(1) exp_277.res created by SHELXL-2016/6 at 09:41:24 on 20-Jul-2020 REM Old TITL exp_277 in P2(1) REM SHELXT solution in P2(1) REM R1 0.115, Rweak 0.056, Alpha 0.002, Orientation as input REM Flack x = 0.006 ( 0.222 ) from Parsons' quotients REM Formula found by SHELXT: C42 C49 O3 S2 CELL 0.71073 9.195488 15.872983 16.345802 90 92.7749 90 ZERR 4 0.000307 0.000517 0.000539 0 0.003 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O S UNIT 112 108 4 12 4 L.S. 5 PLAN 5 MORE -1 BOND $H CONF fmap 2 acta OMIT 0 1 1 OMIT 0 2 0 OMIT 8 5 3 OMIT -11 5 1 OMIT -11 5 3 OMIT -11 5 2 OMIT 11 5 0 OMIT -11 4 4 OMIT 0 -1 1 REM REM REM WGHT 0.044100 0.346300 FVAR 0.06981 S1 5 0.194081 0.386109 0.683301 11.00000 0.03031 0.04603 = 0.03557 -0.00489 -0.00073 -0.00154 O1 4 -0.278630 0.391416 0.732768 11.00000 0.03889 0.04529 = 0.05276 0.00172 0.00309 0.00422 AFIX 147 H1 2 -0.324418 0.394732 0.774466 11.00000 -1.50000 AFIX 0 O2 4 0.229122 0.298291 0.690526 11.00000 0.04702 0.05383 = 0.04428 0.00116 0.00575 0.01433 O3 4 0.294771 0.444610 0.722460 11.00000 0.04036 0.07651 = 0.04805 -0.01140 -0.00344 -0.01817 N1 3 0.031590 0.398300 0.714334 11.00000 0.03436 0.03463 = 0.04840 -0.00466 0.00589 0.00124 AFIX 3 H1A 2 0.021880 0.449090 0.731534 11.00000 -1.20000 AFIX 0 C1 1 -0.193020 0.315532 0.735178 11.00000 0.03213 0.03973 = 0.03549 0.00160 0.00078 0.00090 C2 1 -0.038271 0.339818 0.770909 11.00000 0.03105 0.03793 = 0.03667 -0.00395 0.00038 0.00026 AFIX 13 H2 2 0.020761 0.288493 0.775711 11.00000 -1.20000 AFIX 0 C3 1 -0.049743 0.377829 0.856614 11.00000 0.03813 0.05359 = 0.04044 -0.01087 0.00299 0.00143 AFIX 23 H3A 2 -0.070172 0.437435 0.849778 11.00000 -1.20000 H3B 2 -0.133973 0.352815 0.880615 11.00000 -1.20000 AFIX 0 C4 1 0.077360 0.369603 0.918526 11.00000 0.04174 0.03340 = 0.03532 -0.00069 0.00111 -0.00381 C5 1 0.055898 0.396275 0.998111 11.00000 0.05781 0.06069 = 0.04259 -0.01264 0.00257 0.00763 AFIX 43 H5 2 -0.034544 0.417411 1.010919 11.00000 -1.20000 AFIX 0 C6 1 0.165977 0.392046 1.058499 11.00000 0.09118 0.06718 = 0.04028 -0.01902 -0.00597 0.00781 AFIX 43 H6 2 0.148694 0.409820 1.111366 11.00000 -1.20000 AFIX 0 C7 1 0.300746 0.361762 1.040946 11.00000 0.07148 0.05205 = 0.04950 -0.00161 -0.02470 0.00540 AFIX 43 H7 2 0.375184 0.359433 1.081477 11.00000 -1.20000 AFIX 0 C8 1 0.324304 0.335026 0.963084 11.00000 0.05074 0.04894 = 0.04990 0.00703 -0.00896 0.00392 AFIX 43 H8 2 0.415479 0.314715 0.950619 11.00000 -1.20000 AFIX 0 C9 1 0.213341 0.337988 0.902679 11.00000 0.04600 0.04597 = 0.03583 0.00196 -0.00003 0.00112 AFIX 43 H9 2 0.230640 0.318328 0.850443 11.00000 -1.20000 AFIX 0 C10 1 -0.263348 0.247169 0.786924 11.00000 0.04273 0.04605 = 0.02790 -0.00261 0.00268 -0.00640 C11 1 -0.412484 0.244494 0.792732 11.00000 0.04329 0.06173 = 0.05063 -0.00666 0.00798 -0.00968 AFIX 43 H11 2 -0.470221 0.286617 0.768546 11.00000 -1.20000 AFIX 0 C12 1 -0.476930 0.179093 0.834593 11.00000 0.06006 0.08467 = 0.05810 -0.00951 0.01765 -0.02840 AFIX 43 H12 2 -0.577594 0.177784 0.837856 11.00000 -1.20000 AFIX 0 C13 1 -0.394187 0.116766 0.870967 11.00000 0.09865 0.06824 = 0.04585 -0.00171 0.01908 -0.03619 AFIX 43 H13 2 -0.438344 0.073615 0.899187 11.00000 -1.20000 AFIX 0 C14 1 -0.246409 0.118061 0.865736 11.00000 0.08883 0.06206 = 0.04999 0.01435 0.00234 -0.01092 AFIX 43 H14 2 -0.189788 0.075663 0.890295 11.00000 -1.20000 AFIX 0 C15 1 -0.180648 0.182739 0.823712 11.00000 0.05548 0.05616 = 0.04596 0.01026 0.00128 -0.00487 AFIX 43 H15 2 -0.080028 0.183019 0.820095 11.00000 -1.20000 AFIX 0 C16 1 -0.191088 0.281356 0.647482 11.00000 0.03402 0.04446 = 0.03582 0.00260 -0.00023 -0.01041 C17 1 -0.289171 0.309337 0.586277 11.00000 0.05708 0.06836 = 0.04359 0.00597 -0.01079 -0.01099 AFIX 43 H17 2 -0.354683 0.351990 0.597396 11.00000 -1.20000 AFIX 0 C18 1 -0.290163 0.273769 0.507868 11.00000 0.07824 0.10165 = 0.04571 0.01037 -0.02275 -0.02482 AFIX 43 H18 2 -0.356687 0.292989 0.467436 11.00000 -1.20000 AFIX 0 C19 1 -0.194886 0.211309 0.489965 11.00000 0.09819 0.08798 = 0.04221 -0.01471 0.00097 -0.02179 AFIX 43 H19 2 -0.195371 0.188662 0.437479 11.00000 -1.20000 AFIX 0 C20 1 -0.097993 0.182086 0.550283 11.00000 0.08267 0.06807 = 0.05159 -0.02082 0.01331 -0.01450 AFIX 43 H20 2 -0.033960 0.138793 0.538796 11.00000 -1.20000 AFIX 0 C21 1 -0.095586 0.217055 0.628213 11.00000 0.06055 0.05451 = 0.03882 -0.00580 0.00113 -0.00975 AFIX 43 H21 2 -0.028963 0.197161 0.668269 11.00000 -1.20000 AFIX 0 C22 1 0.181378 0.415532 0.578887 11.00000 0.04161 0.04098 = 0.03778 -0.00319 0.00258 -0.00178 C23 1 0.068283 0.389881 0.527553 11.00000 0.05547 0.06878 = 0.04278 0.00405 -0.00251 -0.02190 AFIX 43 H23 2 -0.007726 0.358916 0.548040 11.00000 -1.20000 AFIX 0 C24 1 0.066692 0.409867 0.445315 11.00000 0.06100 0.07700 = 0.04321 0.00166 -0.00590 -0.01025 AFIX 43 H24 2 -0.011146 0.391928 0.411247 11.00000 -1.20000 AFIX 0 C25 1 0.175593 0.455056 0.412485 11.00000 0.07031 0.06498 = 0.04690 0.00930 0.00566 0.00691 C26 1 0.289185 0.479356 0.464842 11.00000 0.07622 0.13429 = 0.06764 0.03006 0.00904 -0.04209 AFIX 43 H26 2 0.365819 0.509472 0.443961 11.00000 -1.20000 AFIX 0 C27 1 0.293555 0.460670 0.547210 11.00000 0.05813 0.10771 = 0.06071 0.01239 -0.00037 -0.03240 AFIX 43 H27 2 0.371667 0.478399 0.581186 11.00000 -1.20000 AFIX 0 C28 1 0.173061 0.475772 0.322355 11.00000 0.10369 0.12108 = 0.05417 0.02957 0.01108 0.00205 AFIX 137 H28A 2 0.183543 0.424886 0.291448 11.00000 -1.50000 H28B 2 0.251810 0.513360 0.311892 11.00000 -1.50000 H28C 2 0.082218 0.502250 0.306369 11.00000 -1.50000 AFIX 0 S2 5 0.853822 0.629590 0.712356 11.00000 0.03538 0.03745 = 0.04594 0.00190 0.00562 -0.00377 O4 4 0.524017 0.487125 0.834878 11.00000 0.03590 0.03161 = 0.04107 -0.00522 -0.00198 -0.00343 AFIX 147 H4 2 0.452036 0.486139 0.803256 11.00000 -1.50000 AFIX 0 O5 4 0.982460 0.577986 0.717622 11.00000 0.03709 0.05166 = 0.06487 0.00179 0.00515 0.00033 O6 4 0.861387 0.715791 0.737810 11.00000 0.04750 0.03962 = 0.06338 -0.00385 0.00676 -0.00995 N2 3 0.737429 0.582891 0.767939 11.00000 0.03799 0.03358 = 0.03996 0.00146 0.00585 -0.00175 H2A 2 0.730559 0.533408 0.756354 11.00000 0.04502 C29 1 0.546329 0.571032 0.865154 11.00000 0.03204 0.02813 = 0.03278 -0.00289 0.00050 -0.00409 C30 1 0.605588 0.625391 0.794572 11.00000 0.03264 0.03396 = 0.03285 0.00010 -0.00018 -0.00221 AFIX 13 H30 2 0.634679 0.680236 0.817519 11.00000 -1.20000 AFIX 0 C31 1 0.487609 0.641025 0.724638 11.00000 0.03940 0.04528 = 0.03158 0.00140 -0.00120 -0.00387 AFIX 23 H31A 2 0.532559 0.635470 0.672435 11.00000 -1.20000 H31B 2 0.413722 0.597614 0.727180 11.00000 -1.20000 AFIX 0 C32 1 0.414346 0.726274 0.727719 11.00000 0.04185 0.04607 = 0.02859 0.00678 -0.00256 0.00057 C33 1 0.263935 0.732893 0.730249 11.00000 0.04056 0.05764 = 0.04207 0.01157 -0.00400 -0.00225 AFIX 43 H33 2 0.207712 0.684238 0.731316 11.00000 -1.20000 AFIX 0 C34 1 0.196616 0.810821 0.731201 11.00000 0.04434 0.06992 = 0.05184 0.00761 -0.00632 0.01460 AFIX 43 H34 2 0.095850 0.814040 0.733092 11.00000 -1.20000 AFIX 0 C35 1 0.277062 0.883001 0.729386 11.00000 0.06828 0.05789 = 0.06487 0.00395 -0.00507 0.02435 AFIX 43 H35 2 0.231253 0.935240 0.729262 11.00000 -1.20000 AFIX 0 C36 1 0.425822 0.878098 0.727746 11.00000 0.06633 0.04317 = 0.08134 0.00932 -0.00503 0.00001 AFIX 43 H36 2 0.480902 0.927227 0.727451 11.00000 -1.20000 AFIX 0 C37 1 0.494922 0.800134 0.726518 11.00000 0.03955 0.05309 = 0.06367 0.00903 0.00123 0.00017 AFIX 43 H37 2 0.595776 0.797522 0.724882 11.00000 -1.20000 AFIX 0 C38 1 0.406509 0.612388 0.893763 11.00000 0.02989 0.03372 = 0.02883 0.00036 -0.00165 0.00033 C39 1 0.272388 0.572255 0.888088 11.00000 0.03878 0.03826 = 0.04742 -0.00732 0.00644 -0.00387 AFIX 43 H39 2 0.265896 0.516831 0.869825 11.00000 -1.20000 AFIX 0 C40 1 0.147774 0.614666 0.909621 11.00000 0.03322 0.05728 = 0.05982 -0.00646 0.00792 -0.00628 AFIX 43 H40 2 0.058052 0.587627 0.904732 11.00000 -1.20000 AFIX 0 C41 1 0.155450 0.696201 0.938099 11.00000 0.04658 0.05399 = 0.05483 -0.00134 0.01188 0.01285 AFIX 43 H41 2 0.071282 0.724405 0.951624 11.00000 -1.20000 AFIX 0 C42 1 0.287727 0.735469 0.946373 11.00000 0.05814 0.03608 = 0.05040 -0.00341 0.00841 0.00418 AFIX 43 H42 2 0.293937 0.790185 0.966587 11.00000 -1.20000 AFIX 0 C43 1 0.412405 0.693801 0.924668 11.00000 0.04218 0.03795 = 0.04186 -0.00239 0.00088 -0.00705 AFIX 43 H43 2 0.501900 0.720924 0.930928 11.00000 -1.20000 AFIX 0 C44 1 0.652734 0.562155 0.940348 11.00000 0.02986 0.03692 = 0.03220 -0.00150 0.00221 0.00239 C45 1 0.755871 0.622643 0.963066 11.00000 0.03627 0.04484 = 0.04297 0.00101 -0.00375 -0.00336 AFIX 43 H45 2 0.772349 0.667595 0.928218 11.00000 -1.20000 AFIX 0 C46 1 0.835010 0.616500 1.037801 11.00000 0.04186 0.05630 = 0.04987 -0.01059 -0.00864 -0.00162 AFIX 43 H46 2 0.903332 0.657654 1.052553 11.00000 -1.20000 AFIX 0 C47 1 0.812949 0.550109 1.089925 11.00000 0.04676 0.06783 = 0.03509 -0.00508 -0.00602 0.01381 AFIX 43 H47 2 0.865150 0.546544 1.139975 11.00000 -1.20000 AFIX 0 C48 1 0.712332 0.488816 1.067018 11.00000 0.05923 0.05574 = 0.03978 0.00843 0.00202 0.00685 AFIX 43 H48 2 0.697638 0.443267 1.101438 11.00000 -1.20000 AFIX 0 C49 1 0.633274 0.495002 0.992936 11.00000 0.04243 0.04455 = 0.03953 0.00190 -0.00053 -0.00273 AFIX 43 H49 2 0.565894 0.453332 0.978208 11.00000 -1.20000 AFIX 0 C50 1 0.788164 0.626658 0.608671 11.00000 0.04362 0.04072 = 0.04233 0.00243 0.01051 -0.00407 C51 1 0.773669 0.549838 0.569965 11.00000 0.08379 0.04344 = 0.05237 0.00704 -0.00375 0.00350 AFIX 43 H51 2 0.802111 0.500746 0.597369 11.00000 -1.20000 AFIX 0 C52 1 0.716617 0.545968 0.490134 11.00000 0.10310 0.04876 = 0.05373 0.00075 -0.00311 -0.01041 AFIX 43 H52 2 0.707140 0.493994 0.464159 11.00000 -1.20000 AFIX 0 C53 1 0.673353 0.618495 0.448291 11.00000 0.07881 0.06152 = 0.04895 0.01282 -0.00230 -0.01427 C54 1 0.690762 0.694834 0.488673 11.00000 0.08143 0.05174 = 0.05493 0.02278 0.00871 0.00022 AFIX 43 H54 2 0.663761 0.744182 0.461284 11.00000 -1.20000 AFIX 0 C55 1 0.746858 0.699787 0.568156 11.00000 0.06775 0.03911 = 0.04893 0.00857 0.01140 -0.00328 AFIX 43 H55 2 0.756794 0.751701 0.594206 11.00000 -1.20000 AFIX 0 C56 1 0.610018 0.615189 0.361461 11.00000 0.14066 0.09071 = 0.06075 0.02192 -0.01936 -0.03507 AFIX 137 H56A 2 0.517650 0.643489 0.358379 11.00000 -1.50000 H56B 2 0.596969 0.557504 0.345052 11.00000 -1.50000 H56C 2 0.675135 0.642471 0.325702 11.00000 -1.50000 AFIX 0 HKLF 4 REM exp_277_a.res in P2(1) REM R1 = 0.0562 for 9831 Fo > 4sig(Fo) and 0.0947 for all 14398 data REM 603 parameters refined using 1 restraints END WGHT 0.0441 0.3463 REM Highest difference peak 0.296, deepest hole -0.280, 1-sigma level 0.039 Q1 1 0.7748 0.6181 0.7524 11.00000 0.05 0.22 Q2 1 0.7798 0.5977 0.7224 11.00000 0.05 0.21 Q3 1 0.2865 0.4076 0.7036 11.00000 0.05 0.21 Q4 1 0.4770 0.5889 0.8969 11.00000 0.05 0.19 Q5 1 0.2285 0.3348 0.6595 11.00000 0.05 0.18 REM The information below was added by Olex2. REM REM R1 = 0.0562 for 9831 Fo > 4sig(Fo) and 0.0947 for all 72200 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.30, deepest hole -0.28 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0947 REM R1_gt = 0.0562 REM wR_ref = 0.1117 REM GOOF = 1.016 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 72200 REM Reflections_gt = 9831 REM Parameters = n/a REM Hole = -0.28 REM Peak = 0.30 REM Flack = -0.01(3) ; _cod_data_source_file d0dt02557g2.cif _cod_data_source_block exp_277 _cod_original_cell_volume 2383.03(14) _cod_database_code 7705232 _shelx_shelxl_version_number 2016/6 _chemical_oxdiff_formula 'C27 S O3 N H25' _chemical_oxdiff_usercomment 'phenyl 1 FSiii057 rxt from iproh' _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. ; _diffrn_oxdiff_digest_frames ; 018d20d9951095baa11f3bc85da3930e1003303910c ; _diffrn_oxdiff_digest_hkl ; 01e18a45d72169cfa0cbd8ab1a6eeffafefe79 ; _reflns_odcompleteness_completeness 99.96 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Riding coordinates: N1(H1A) 2.b Ternary CH refined with riding coordinates: C2(H2), C30(H30) 2.c Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C31(H31A,H31B) 2.d Aromatic/amide H refined with riding coordinates: C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C51(H51), C52(H52), C54(H54), C55(H55) 2.e Idealised Me refined as rotating group: C28(H28A,H28B,H28C), C56(H56A,H56B,H56C) 2.f Idealised tetrahedral OH refined as rotating group: O1(H1), O4(H4) ; _olex2_submission_original_sample_id FSiii057 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.247 _oxdiff_exptl_absorpt_empirical_full_min 0.839 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.19408(8) 0.38611(5) 0.68330(5) 0.03738(18) Uani 1 1 d . . . . . O1 O -0.2786(2) 0.39142(14) 0.73277(14) 0.0456(5) Uani 1 1 d . . . . . H1 H -0.324418 0.394732 0.774466 0.068 Uiso 1 1 calc GR . . . . O2 O 0.2291(2) 0.29829(15) 0.69053(14) 0.0483(6) Uani 1 1 d . . . . . O3 O 0.2948(3) 0.44461(17) 0.72246(15) 0.0552(7) Uani 1 1 d . . . . . N1 N 0.0316(3) 0.39830(16) 0.71433(16) 0.0390(6) Uani 1 1 d . . . . . H1A H 0.021880 0.449090 0.731534 0.047 Uiso 1 1 d R . . . . C1 C -0.1930(3) 0.31553(19) 0.73518(18) 0.0358(7) Uani 1 1 d . . . . . C2 C -0.0383(3) 0.3398(2) 0.77091(18) 0.0353(6) Uani 1 1 d . . . . . H2 H 0.020761 0.288493 0.775711 0.042 Uiso 1 1 calc R . . . . C3 C -0.0497(4) 0.3778(2) 0.85661(19) 0.0440(8) Uani 1 1 d . . . . . H3A H -0.070172 0.437435 0.849778 0.053 Uiso 1 1 calc R . . . . H3B H -0.133973 0.352815 0.880615 0.053 Uiso 1 1 calc R . . . . C4 C 0.0774(4) 0.36960(18) 0.91853(18) 0.0368(7) Uani 1 1 d . . . . . C5 C 0.0559(4) 0.3963(2) 0.9981(2) 0.0537(9) Uani 1 1 d . . . . . H5 H -0.034544 0.417411 1.010919 0.064 Uiso 1 1 calc R . . . . C6 C 0.1660(5) 0.3920(3) 1.0585(2) 0.0665(11) Uani 1 1 d . . . . . H6 H 0.148694 0.409820 1.111366 0.080 Uiso 1 1 calc R . . . . C7 C 0.3007(5) 0.3618(2) 1.0409(2) 0.0586(11) Uani 1 1 d . . . . . H7 H 0.375184 0.359433 1.081477 0.070 Uiso 1 1 calc R . . . . C8 C 0.3243(4) 0.3350(2) 0.9631(2) 0.0502(9) Uani 1 1 d . . . . . H8 H 0.415479 0.314715 0.950619 0.060 Uiso 1 1 calc R . . . . C9 C 0.2133(4) 0.3380(2) 0.9027(2) 0.0427(7) Uani 1 1 d . . . . . H9 H 0.230640 0.318328 0.850443 0.051 Uiso 1 1 calc R . . . . C10 C -0.2633(4) 0.2472(2) 0.78692(18) 0.0389(7) Uani 1 1 d . . . . . C11 C -0.4125(4) 0.2445(2) 0.7927(2) 0.0517(9) Uani 1 1 d . . . . . H11 H -0.470221 0.286617 0.768546 0.062 Uiso 1 1 calc R . . . . C12 C -0.4769(5) 0.1791(3) 0.8346(3) 0.0671(12) Uani 1 1 d . . . . . H12 H -0.577594 0.177784 0.837856 0.081 Uiso 1 1 calc R . . . . C13 C -0.3942(6) 0.1168(3) 0.8710(2) 0.0704(13) Uani 1 1 d . . . . . H13 H -0.438344 0.073615 0.899187 0.084 Uiso 1 1 calc R . . . . C14 C -0.2464(5) 0.1181(3) 0.8657(2) 0.0670(11) Uani 1 1 d . . . . . H14 H -0.189788 0.075663 0.890295 0.080 Uiso 1 1 calc R . . . . C15 C -0.1806(4) 0.1827(2) 0.8237(2) 0.0526(9) Uani 1 1 d . . . . . H15 H -0.080028 0.183019 0.820095 0.063 Uiso 1 1 calc R . . . . C16 C -0.1911(3) 0.2814(2) 0.64748(19) 0.0382(7) Uani 1 1 d . . . . . C17 C -0.2892(4) 0.3093(3) 0.5863(2) 0.0568(10) Uani 1 1 d . . . . . H17 H -0.354683 0.351990 0.597396 0.068 Uiso 1 1 calc R . . . . C18 C -0.2902(6) 0.2738(3) 0.5079(3) 0.0760(14) Uani 1 1 d . . . . . H18 H -0.356687 0.292989 0.467436 0.091 Uiso 1 1 calc R . . . . C19 C -0.1949(6) 0.2113(3) 0.4900(3) 0.0762(13) Uani 1 1 d . . . . . H19 H -0.195371 0.188662 0.437479 0.091 Uiso 1 1 calc R . . . . C20 C -0.0980(5) 0.1821(3) 0.5503(2) 0.0671(12) Uani 1 1 d . . . . . H20 H -0.033960 0.138793 0.538796 0.081 Uiso 1 1 calc R . . . . C21 C -0.0956(4) 0.2171(2) 0.6282(2) 0.0513(9) Uani 1 1 d . . . . . H21 H -0.028963 0.197161 0.668269 0.062 Uiso 1 1 calc R . . . . C22 C 0.1814(4) 0.4155(2) 0.57889(19) 0.0401(7) Uani 1 1 d . . . . . C23 C 0.0683(4) 0.3899(3) 0.5276(2) 0.0558(9) Uani 1 1 d . . . . . H23 H -0.007726 0.358916 0.548040 0.067 Uiso 1 1 calc R . . . . C24 C 0.0667(5) 0.4099(3) 0.4453(2) 0.0607(10) Uani 1 1 d . . . . . H24 H -0.011146 0.391928 0.411247 0.073 Uiso 1 1 calc R . . . . C25 C 0.1756(5) 0.4551(3) 0.4125(2) 0.0606(10) Uani 1 1 d . . . . . C26 C 0.2892(6) 0.4794(4) 0.4648(3) 0.0925(18) Uani 1 1 d . . . . . H26 H 0.365819 0.509472 0.443961 0.111 Uiso 1 1 calc R . . . . C27 C 0.2936(5) 0.4607(3) 0.5472(3) 0.0756(13) Uani 1 1 d . . . . . H27 H 0.371667 0.478399 0.581186 0.091 Uiso 1 1 calc R . . . . C28 C 0.1731(6) 0.4758(4) 0.3224(3) 0.0927(17) Uani 1 1 d . . . . . H28A H 0.183543 0.424886 0.291448 0.139 Uiso 1 1 calc GR . . . . H28B H 0.251810 0.513360 0.311892 0.139 Uiso 1 1 calc GR . . . . H28C H 0.082218 0.502250 0.306369 0.139 Uiso 1 1 calc GR . . . . S2 S 0.85382(8) 0.62959(5) 0.71236(5) 0.03947(19) Uani 1 1 d . . . . . O4 O 0.5240(2) 0.48712(12) 0.83488(13) 0.0363(5) Uani 1 1 d . . . . . H4 H 0.452036 0.486139 0.803256 0.054 Uiso 1 1 calc GR . . . . O5 O 0.9825(3) 0.57799(15) 0.71762(16) 0.0511(6) Uani 1 1 d . . . . . O6 O 0.8614(3) 0.71579(14) 0.73781(15) 0.0500(6) Uani 1 1 d . . . . . N2 N 0.7374(3) 0.58289(18) 0.76794(16) 0.0370(6) Uani 1 1 d . . . . . H2A H 0.731(4) 0.533(2) 0.756(2) 0.045(11) Uiso 1 1 d . . . . . C29 C 0.5463(3) 0.57103(17) 0.86515(17) 0.0310(6) Uani 1 1 d . . . . . C30 C 0.6056(3) 0.6254(2) 0.79457(17) 0.0332(6) Uani 1 1 d . . . . . H30 H 0.634679 0.680236 0.817519 0.040 Uiso 1 1 calc R . . . . C31 C 0.4876(3) 0.6410(2) 0.72464(18) 0.0388(7) Uani 1 1 d . . . . . H31A H 0.532559 0.635470 0.672435 0.047 Uiso 1 1 calc R . . . . H31B H 0.413722 0.597614 0.727180 0.047 Uiso 1 1 calc R . . . . C32 C 0.4143(4) 0.7263(2) 0.72772(18) 0.0390(7) Uani 1 1 d . . . . . C33 C 0.2639(4) 0.7329(2) 0.7302(2) 0.0469(8) Uani 1 1 d . . . . . H33 H 0.207712 0.684238 0.731316 0.056 Uiso 1 1 calc R . . . . C34 C 0.1966(4) 0.8108(3) 0.7312(2) 0.0556(9) Uani 1 1 d . . . . . H34 H 0.095850 0.814040 0.733092 0.067 Uiso 1 1 calc R . . . . C35 C 0.2771(5) 0.8830(3) 0.7294(2) 0.0639(11) Uani 1 1 d . . . . . H35 H 0.231253 0.935240 0.729262 0.077 Uiso 1 1 calc R . . . . C36 C 0.4258(5) 0.8781(3) 0.7277(3) 0.0639(10) Uani 1 1 d . . . . . H36 H 0.480902 0.927227 0.727451 0.077 Uiso 1 1 calc R . . . . C37 C 0.4949(4) 0.8001(2) 0.7265(2) 0.0521(9) Uani 1 1 d . . . . . H37 H 0.595776 0.797522 0.724882 0.063 Uiso 1 1 calc R . . . . C38 C 0.4065(3) 0.61239(17) 0.89376(16) 0.0309(6) Uani 1 1 d . . . . . C39 C 0.2724(4) 0.5723(2) 0.8881(2) 0.0413(7) Uani 1 1 d . . . . . H39 H 0.265896 0.516831 0.869825 0.050 Uiso 1 1 calc R . . . . C40 C 0.1478(4) 0.6147(2) 0.9096(2) 0.0499(9) Uani 1 1 d . . . . . H40 H 0.058052 0.587627 0.904732 0.060 Uiso 1 1 calc R . . . . C41 C 0.1555(4) 0.6962(2) 0.9381(2) 0.0515(9) Uani 1 1 d . . . . . H41 H 0.071282 0.724405 0.951624 0.062 Uiso 1 1 calc R . . . . C42 C 0.2877(4) 0.7355(2) 0.9464(2) 0.0480(8) Uani 1 1 d . . . . . H42 H 0.293937 0.790185 0.966587 0.058 Uiso 1 1 calc R . . . . C43 C 0.4124(4) 0.69380(19) 0.92467(19) 0.0407(7) Uani 1 1 d . . . . . H43 H 0.501900 0.720924 0.930928 0.049 Uiso 1 1 calc R . . . . C44 C 0.6527(3) 0.56216(18) 0.94035(17) 0.0330(6) Uani 1 1 d . . . . . C45 C 0.7559(3) 0.6226(2) 0.96307(19) 0.0415(7) Uani 1 1 d . . . . . H45 H 0.772349 0.667595 0.928218 0.050 Uiso 1 1 calc R . . . . C46 C 0.8350(4) 0.6165(2) 1.0378(2) 0.0497(8) Uani 1 1 d . . . . . H46 H 0.903332 0.657654 1.052553 0.060 Uiso 1 1 calc R . . . . C47 C 0.8129(4) 0.5501(2) 1.0899(2) 0.0502(9) Uani 1 1 d . . . . . H47 H 0.865150 0.546544 1.139975 0.060 Uiso 1 1 calc R . . . . C48 C 0.7123(4) 0.4888(2) 1.0670(2) 0.0516(9) Uani 1 1 d . . . . . H48 H 0.697638 0.443267 1.101438 0.062 Uiso 1 1 calc R . . . . C49 C 0.6333(4) 0.4950(2) 0.9929(2) 0.0422(7) Uani 1 1 d . . . . . H49 H 0.565894 0.453332 0.978208 0.051 Uiso 1 1 calc R . . . . C50 C 0.7882(4) 0.6267(2) 0.60867(19) 0.0419(7) Uani 1 1 d . . . . . C51 C 0.7737(5) 0.5498(2) 0.5700(2) 0.0601(11) Uani 1 1 d . . . . . H51 H 0.802111 0.500746 0.597369 0.072 Uiso 1 1 calc R . . . . C52 C 0.7166(6) 0.5460(3) 0.4901(3) 0.0688(12) Uani 1 1 d . . . . . H52 H 0.707140 0.493994 0.464159 0.083 Uiso 1 1 calc R . . . . C53 C 0.6734(5) 0.6185(3) 0.4483(2) 0.0633(11) Uani 1 1 d . . . . . C54 C 0.6908(5) 0.6948(3) 0.4887(2) 0.0625(11) Uani 1 1 d . . . . . H54 H 0.663761 0.744182 0.461284 0.075 Uiso 1 1 calc R . . . . C55 C 0.7469(4) 0.6998(2) 0.5682(2) 0.0517(9) Uani 1 1 d . . . . . H55 H 0.756794 0.751701 0.594206 0.062 Uiso 1 1 calc R . . . . C56 C 0.6100(7) 0.6152(4) 0.3615(3) 0.0982(18) Uani 1 1 d . . . . . H56A H 0.517650 0.643489 0.358379 0.147 Uiso 1 1 calc GR . . . . H56B H 0.596969 0.557504 0.345052 0.147 Uiso 1 1 calc GR . . . . H56C H 0.675135 0.642471 0.325702 0.147 Uiso 1 1 calc GR . . . . 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 0.0303(4) 0.0460(4) 0.0356(4) -0.0049(3) -0.0007(3) -0.0015(3) O1 0.0389(13) 0.0453(13) 0.0528(14) 0.0017(11) 0.0031(10) 0.0042(11) O2 0.0470(14) 0.0538(14) 0.0443(13) 0.0012(11) 0.0058(11) 0.0143(11) O3 0.0404(14) 0.0765(17) 0.0480(14) -0.0114(13) -0.0034(11) -0.0182(12) N1 0.0344(14) 0.0346(14) 0.0484(15) -0.0047(12) 0.0059(11) 0.0012(11) C1 0.0321(17) 0.0397(17) 0.0355(15) 0.0016(12) 0.0008(13) 0.0009(13) C2 0.0311(16) 0.0379(16) 0.0367(15) -0.0040(13) 0.0004(12) 0.0003(13) C3 0.0381(18) 0.054(2) 0.0404(17) -0.0109(15) 0.0030(13) 0.0014(16) C4 0.0417(18) 0.0334(16) 0.0353(15) -0.0007(12) 0.0011(13) -0.0038(13) C5 0.058(2) 0.061(2) 0.0426(18) -0.0126(17) 0.0026(16) 0.0076(18) C6 0.091(3) 0.067(3) 0.0403(19) -0.0190(19) -0.0060(19) 0.008(2) C7 0.071(3) 0.052(2) 0.049(2) -0.0016(16) -0.0247(19) 0.0054(19) C8 0.051(2) 0.049(2) 0.050(2) 0.0070(17) -0.0090(16) 0.0039(17) C9 0.046(2) 0.0460(18) 0.0358(16) 0.0020(15) 0.0000(14) 0.0011(15) C10 0.0427(19) 0.0460(18) 0.0279(15) -0.0026(13) 0.0027(13) -0.0064(14) C11 0.043(2) 0.062(2) 0.051(2) -0.0067(17) 0.0080(16) -0.0097(17) C12 0.060(3) 0.085(3) 0.058(2) -0.010(2) 0.018(2) -0.028(2) C13 0.099(4) 0.068(3) 0.046(2) -0.002(2) 0.019(2) -0.036(3) C14 0.089(3) 0.062(3) 0.050(2) 0.014(2) 0.002(2) -0.011(2) C15 0.055(2) 0.056(2) 0.046(2) 0.0103(16) 0.0013(17) -0.0049(17) C16 0.0340(17) 0.0445(18) 0.0358(16) 0.0026(13) -0.0002(13) -0.0104(13) C17 0.057(2) 0.068(2) 0.044(2) 0.0060(17) -0.0108(17) -0.0110(19) C18 0.078(3) 0.102(4) 0.046(2) 0.010(2) -0.023(2) -0.025(3) C19 0.098(4) 0.088(3) 0.042(2) -0.015(2) 0.001(2) -0.022(3) C20 0.083(3) 0.068(3) 0.052(2) -0.021(2) 0.013(2) -0.014(2) C21 0.061(2) 0.055(2) 0.0388(18) -0.0058(16) 0.0011(16) -0.0097(18) C22 0.0416(19) 0.0410(17) 0.0378(16) -0.0032(13) 0.0026(14) -0.0018(14) C23 0.055(2) 0.069(2) 0.0428(18) 0.0040(18) -0.0025(16) -0.022(2) C24 0.061(3) 0.077(3) 0.043(2) 0.0017(18) -0.0059(17) -0.010(2) C25 0.070(3) 0.065(2) 0.047(2) 0.0093(18) 0.006(2) 0.007(2) C26 0.076(3) 0.134(5) 0.068(3) 0.030(3) 0.009(3) -0.042(3) C27 0.058(3) 0.108(4) 0.061(3) 0.012(3) 0.000(2) -0.032(3) C28 0.104(4) 0.121(4) 0.054(3) 0.030(3) 0.011(3) 0.002(3) S2 0.0354(4) 0.0374(4) 0.0459(4) 0.0019(4) 0.0056(3) -0.0038(3) O4 0.0359(12) 0.0316(11) 0.0411(12) -0.0052(9) -0.0020(9) -0.0034(9) O5 0.0371(13) 0.0517(14) 0.0649(16) 0.0018(12) 0.0052(11) 0.0003(11) O6 0.0475(15) 0.0396(13) 0.0634(15) -0.0039(11) 0.0068(11) -0.0100(10) N2 0.0380(15) 0.0336(15) 0.0400(14) 0.0015(12) 0.0059(11) -0.0017(11) C29 0.0320(16) 0.0281(14) 0.0328(14) -0.0029(11) 0.0005(12) -0.0041(11) C30 0.0326(15) 0.0340(14) 0.0329(14) 0.0001(13) -0.0002(12) -0.0022(13) C31 0.0394(18) 0.0453(18) 0.0316(15) 0.0014(13) -0.0012(13) -0.0039(14) C32 0.0418(19) 0.0461(18) 0.0286(15) 0.0068(13) -0.0026(13) 0.0006(14) C33 0.041(2) 0.058(2) 0.0421(18) 0.0116(16) -0.0040(15) -0.0022(16) C34 0.044(2) 0.070(3) 0.052(2) 0.0076(18) -0.0063(17) 0.0146(19) C35 0.068(3) 0.058(2) 0.065(2) 0.004(2) -0.005(2) 0.024(2) C36 0.066(3) 0.043(2) 0.081(3) 0.009(2) -0.005(2) 0.0000(19) C37 0.040(2) 0.053(2) 0.064(2) 0.0090(18) 0.0012(17) 0.0002(16) C38 0.0299(15) 0.0337(16) 0.0288(13) 0.0004(11) -0.0017(11) 0.0003(11) C39 0.0388(19) 0.0383(17) 0.0474(18) -0.0073(14) 0.0064(14) -0.0039(14) C40 0.0332(18) 0.057(2) 0.060(2) -0.0065(18) 0.0079(15) -0.0063(16) C41 0.047(2) 0.054(2) 0.055(2) -0.0013(17) 0.0119(17) 0.0129(17) C42 0.058(2) 0.0361(18) 0.050(2) -0.0034(15) 0.0084(17) 0.0042(16) C43 0.0422(19) 0.0379(17) 0.0419(17) -0.0024(14) 0.0009(14) -0.0070(14) C44 0.0299(16) 0.0369(16) 0.0322(15) -0.0015(12) 0.0022(12) 0.0024(12) C45 0.0363(17) 0.0448(17) 0.0430(17) 0.0010(15) -0.0037(13) -0.0034(15) C46 0.0419(19) 0.056(2) 0.0499(19) -0.0106(18) -0.0086(15) -0.0016(16) C47 0.047(2) 0.068(2) 0.0351(18) -0.0051(16) -0.0060(15) 0.0138(18) C48 0.059(2) 0.056(2) 0.0398(19) 0.0084(16) 0.0020(17) 0.0068(18) C49 0.0424(19) 0.0446(19) 0.0395(18) 0.0019(14) -0.0005(14) -0.0027(14) C50 0.0436(19) 0.0407(17) 0.0423(17) 0.0024(15) 0.0105(14) -0.0041(15) C51 0.084(3) 0.043(2) 0.052(2) 0.0070(17) -0.004(2) 0.0035(19) C52 0.103(4) 0.049(2) 0.054(2) 0.0007(18) -0.003(2) -0.010(2) C53 0.079(3) 0.062(2) 0.049(2) 0.0128(19) -0.0023(19) -0.014(2) C54 0.081(3) 0.052(2) 0.055(2) 0.0228(18) 0.009(2) 0.000(2) C55 0.068(3) 0.0391(19) 0.049(2) 0.0086(15) 0.0114(18) -0.0033(16) C56 0.141(5) 0.091(4) 0.061(3) 0.022(3) -0.019(3) -0.035(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 5 3 0.0822 0 3 5 0.0697 0 -3 -5 0.0697 0 -1 0 0.1037 -3 0 5 0.1844 3 0 -5 0.1329 -5 -3 2 0.1983 -2 -1 -1 0.1796 2 0 1 0.1709 0 1 -1 0.0615 0 -1 1 0.1001 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 O2 S1 O3 116.95(16) . . ? O2 S1 N1 107.37(14) . . ? O2 S1 C22 109.90(14) . . ? O3 S1 N1 111.63(14) . . ? O3 S1 C22 105.66(15) . . ? N1 S1 C22 104.66(15) . . ? C1 O1 H1 109.5 . . ? S1 N1 H1A 109.1 . . ? C2 N1 S1 124.0(2) . . ? C2 N1 H1A 109.2 . . ? O1 C1 C2 106.9(2) . . ? O1 C1 C10 111.2(2) . . ? O1 C1 C16 107.6(2) . . ? C10 C1 C2 111.6(2) . . ? C16 C1 C2 112.7(2) . . ? C16 C1 C10 106.8(2) . . ? N1 C2 C1 109.7(2) . . ? N1 C2 H2 108.4 . . ? N1 C2 C3 112.1(3) . . ? C1 C2 H2 108.4 . . ? C3 C2 C1 109.7(2) . . ? C3 C2 H2 108.4 . . ? C2 C3 H3A 107.5 . . ? C2 C3 H3B 107.5 . . ? H3A C3 H3B 107.0 . . ? C4 C3 C2 119.4(3) . . ? C4 C3 H3A 107.5 . . ? C4 C3 H3B 107.5 . . ? C5 C4 C3 117.3(3) . . ? C9 C4 C3 125.6(3) . . ? C9 C4 C5 117.1(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 C4 121.4(4) . . ? C6 C5 H5 119.3 . . ? C5 C6 H6 119.8 . . ? C7 C6 C5 120.4(3) . . ? C7 C6 H6 119.8 . . ? C6 C7 H7 120.4 . . ? C8 C7 C6 119.2(3) . . ? C8 C7 H7 120.4 . . ? C7 C8 H8 119.7 . . ? C7 C8 C9 120.5(4) . . ? C9 C8 H8 119.7 . . ? C4 C9 C8 121.3(3) . . ? C4 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C11 C10 C1 120.4(3) . . ? C11 C10 C15 118.1(3) . . ? C15 C10 C1 121.3(3) . . ? C10 C11 H11 119.8 . . ? C10 C11 C12 120.3(4) . . ? C12 C11 H11 119.8 . . ? C11 C12 H12 119.6 . . ? C13 C12 C11 120.8(4) . . ? C13 C12 H12 119.6 . . ? C12 C13 H13 120.1 . . ? C14 C13 C12 119.8(4) . . ? C14 C13 H13 120.1 . . ? C13 C14 H14 120.0 . . ? C13 C14 C15 120.0(4) . . ? C15 C14 H14 120.0 . . ? C10 C15 H15 119.5 . . ? C14 C15 C10 120.9(4) . . ? C14 C15 H15 119.5 . . ? C17 C16 C1 121.6(3) . . ? C17 C16 C21 117.8(3) . . ? C21 C16 C1 120.4(3) . . ? C16 C17 H17 119.8 . . ? C16 C17 C18 120.4(4) . . ? C18 C17 H17 119.8 . . ? C17 C18 H18 119.5 . . ? C19 C18 C17 120.9(4) . . ? C19 C18 H18 119.5 . . ? C18 C19 H19 120.3 . . ? C18 C19 C20 119.4(4) . . ? C20 C19 H19 120.3 . . ? C19 C20 H20 119.9 . . ? C19 C20 C21 120.2(4) . . ? C21 C20 H20 119.9 . . ? C16 C21 H21 119.4 . . ? C20 C21 C16 121.2(4) . . ? C20 C21 H21 119.4 . . ? C23 C22 S1 121.8(3) . . ? C23 C22 C27 119.1(3) . . ? C27 C22 S1 119.0(3) . . ? C22 C23 H23 120.0 . . ? C22 C23 C24 120.1(3) . . ? C24 C23 H23 120.0 . . ? C23 C24 H24 119.0 . . ? C25 C24 C23 122.1(4) . . ? C25 C24 H24 119.0 . . ? C24 C25 C26 117.0(4) . . ? C24 C25 C28 121.5(4) . . ? C26 C25 C28 121.5(4) . . ? C25 C26 H26 118.9 . . ? C25 C26 C27 122.3(4) . . ? C27 C26 H26 118.9 . . ? C22 C27 H27 120.2 . . ? C26 C27 C22 119.5(4) . . ? C26 C27 H27 120.2 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O5 S2 N2 105.68(15) . . ? O5 S2 C50 106.47(16) . . ? O6 S2 O5 119.94(15) . . ? O6 S2 N2 107.41(15) . . ? O6 S2 C50 108.22(16) . . ? N2 S2 C50 108.74(15) . . ? C29 O4 H4 109.5 . . ? S2 N2 H2A 111(3) . . ? C30 N2 S2 122.2(2) . . ? C30 N2 H2A 117(3) . . ? O4 C29 C30 107.9(2) . . ? O4 C29 C38 113.2(2) . . ? O4 C29 C44 105.4(2) . . ? C38 C29 C30 108.4(2) . . ? C38 C29 C44 107.8(2) . . ? C44 C29 C30 114.2(2) . . ? N2 C30 C29 106.7(2) . . ? N2 C30 H30 107.9 . . ? N2 C30 C31 114.2(2) . . ? C29 C30 H30 107.9 . . ? C31 C30 C29 112.0(2) . . ? C31 C30 H30 107.9 . . ? C30 C31 H31A 108.7 . . ? C30 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C32 C31 C30 114.4(3) . . ? C32 C31 H31A 108.7 . . ? C32 C31 H31B 108.7 . . ? C33 C32 C31 120.9(3) . . ? C37 C32 C31 121.1(3) . . ? C37 C32 C33 118.0(3) . . ? C32 C33 H33 119.5 . . ? C34 C33 C32 121.0(4) . . ? C34 C33 H33 119.5 . . ? C33 C34 H34 119.8 . . ? C35 C34 C33 120.5(4) . . ? C35 C34 H34 119.8 . . ? C34 C35 H35 120.2 . . ? C34 C35 C36 119.7(4) . . ? C36 C35 H35 120.2 . . ? C35 C36 H36 119.8 . . ? C35 C36 C37 120.5(4) . . ? C37 C36 H36 119.8 . . ? C32 C37 C36 120.4(3) . . ? C32 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C39 C38 C29 122.5(3) . . ? C39 C38 C43 118.1(3) . . ? C43 C38 C29 119.4(3) . . ? C38 C39 H39 119.9 . . ? C38 C39 C40 120.1(3) . . ? C40 C39 H39 119.9 . . ? C39 C40 H40 119.6 . . ? C41 C40 C39 120.8(3) . . ? C41 C40 H40 119.6 . . ? C40 C41 H41 120.2 . . ? C42 C41 C40 119.5(3) . . ? C42 C41 H41 120.2 . . ? C41 C42 H42 120.0 . . ? C41 C42 C43 120.0(3) . . ? C43 C42 H42 120.0 . . ? C38 C43 H43 119.3 . . ? C42 C43 C38 121.3(3) . . ? C42 C43 H43 119.3 . . ? C45 C44 C29 123.4(3) . . ? C49 C44 C29 118.0(3) . . ? C49 C44 C45 118.2(3) . . ? C44 C45 H45 119.8 . . ? C44 C45 C46 120.5(3) . . ? C46 C45 H45 119.8 . . ? C45 C46 H46 119.7 . . ? C47 C46 C45 120.6(3) . . ? C47 C46 H46 119.7 . . ? C46 C47 H47 120.4 . . ? C46 C47 C48 119.2(3) . . ? C48 C47 H47 120.4 . . ? C47 C48 H48 119.9 . . ? C47 C48 C49 120.2(3) . . ? C49 C48 H48 119.9 . . ? C44 C49 H49 119.4 . . ? C48 C49 C44 121.2(3) . . ? C48 C49 H49 119.4 . . ? C51 C50 S2 118.9(3) . . ? C51 C50 C55 120.4(3) . . ? C55 C50 S2 120.7(3) . . ? C50 C51 H51 120.1 . . ? C50 C51 C52 119.8(3) . . ? C52 C51 H51 120.1 . . ? C51 C52 H52 119.5 . . ? C51 C52 C53 121.0(4) . . ? C53 C52 H52 119.5 . . ? C52 C53 C56 121.6(4) . . ? C54 C53 C52 117.8(4) . . ? C54 C53 C56 120.6(4) . . ? C53 C54 H54 119.0 . . ? C55 C54 C53 121.9(3) . . ? C55 C54 H54 119.0 . . ? C50 C55 H55 120.4 . . ? C54 C55 C50 119.1(3) . . ? C54 C55 H55 120.4 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56B 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? 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 S1 O2 1.434(2) . ? S1 O3 1.439(2) . ? S1 N1 1.613(3) . ? S1 C22 1.768(3) . ? O1 H1 0.8200 . ? O1 C1 1.438(4) . ? N1 H1A 0.8599 . ? N1 C2 1.479(4) . ? C1 C2 1.560(4) . ? C1 C10 1.538(4) . ? C1 C16 1.534(4) . ? C2 H2 0.9800 . ? C2 C3 1.534(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.514(4) . ? C4 C5 1.391(4) . ? C4 C9 1.383(4) . ? C5 H5 0.9300 . ? C5 C6 1.381(5) . ? C6 H6 0.9300 . ? C6 C7 1.372(6) . ? C7 H7 0.9300 . ? C7 C8 1.369(5) . ? C8 H8 0.9300 . ? C8 C9 1.386(4) . ? C9 H9 0.9300 . ? C10 C11 1.380(5) . ? C10 C15 1.393(5) . ? C11 H11 0.9300 . ? C11 C12 1.392(5) . ? C12 H12 0.9300 . ? C12 C13 1.367(7) . ? C13 H13 0.9300 . ? C13 C14 1.366(6) . ? C14 H14 0.9300 . ? C14 C15 1.390(5) . ? C15 H15 0.9300 . ? C16 C17 1.387(5) . ? C16 C21 1.392(5) . ? C17 H17 0.9300 . ? C17 C18 1.400(6) . ? C18 H18 0.9300 . ? C18 C19 1.364(7) . ? C19 H19 0.9300 . ? C19 C20 1.377(6) . ? C20 H20 0.9300 . ? C20 C21 1.389(5) . ? C21 H21 0.9300 . ? C22 C23 1.366(5) . ? C22 C27 1.377(5) . ? C23 H23 0.9300 . ? C23 C24 1.381(5) . ? C24 H24 0.9300 . ? C24 C25 1.363(6) . ? C25 C26 1.373(6) . ? C25 C28 1.509(6) . ? C26 H26 0.9300 . ? C26 C27 1.377(6) . ? C27 H27 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? S2 O5 1.438(2) . ? S2 O6 1.431(2) . ? S2 N2 1.617(3) . ? S2 C50 1.772(3) . ? O4 H4 0.8200 . ? O4 C29 1.432(3) . ? N2 H2A 0.81(4) . ? N2 C30 1.472(4) . ? C29 C30 1.560(4) . ? C29 C38 1.537(4) . ? C29 C44 1.540(4) . ? C30 H30 0.9800 . ? C30 C31 1.557(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 C32 1.514(5) . ? C32 C33 1.390(5) . ? C32 C37 1.388(5) . ? C33 H33 0.9300 . ? C33 C34 1.384(5) . ? C34 H34 0.9300 . ? C34 C35 1.365(6) . ? C35 H35 0.9300 . ? C35 C36 1.372(6) . ? C36 H36 0.9300 . ? C36 C37 1.392(5) . ? C37 H37 0.9300 . ? C38 C39 1.387(4) . ? C38 C43 1.388(4) . ? C39 H39 0.9300 . ? C39 C40 1.389(5) . ? C40 H40 0.9300 . ? C40 C41 1.376(5) . ? C41 H41 0.9300 . ? C41 C42 1.368(5) . ? C42 H42 0.9300 . ? C42 C43 1.385(5) . ? C43 H43 0.9300 . ? C44 C45 1.387(4) . ? C44 C49 1.386(4) . ? C45 H45 0.9300 . ? C45 C46 1.395(5) . ? C46 H46 0.9300 . ? C46 C47 1.376(5) . ? C47 H47 0.9300 . ? C47 C48 1.382(5) . ? C48 H48 0.9300 . ? C48 C49 1.385(5) . ? C49 H49 0.9300 . ? C50 C51 1.377(5) . ? C50 C55 1.381(5) . ? C51 H51 0.9300 . ? C51 C52 1.384(6) . ? C52 H52 0.9300 . ? C52 C53 1.387(6) . ? C53 C54 1.385(6) . ? C53 C56 1.509(6) . ? C54 H54 0.9300 . ? C54 C55 1.377(5) . ? C55 H55 0.9300 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? 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 S1 N1 C2 C1 -130.4(2) . . . . ? S1 N1 C2 C3 107.5(3) . . . . ? S1 C22 C23 C24 -176.1(3) . . . . ? S1 C22 C27 C26 175.9(4) . . . . ? O1 C1 C2 N1 -64.5(3) . . . . ? O1 C1 C2 C3 59.0(3) . . . . ? O1 C1 C10 C11 29.6(4) . . . . ? O1 C1 C10 C15 -155.5(3) . . . . ? O1 C1 C16 C17 -15.6(4) . . . . ? O1 C1 C16 C21 168.4(3) . . . . ? O2 S1 N1 C2 23.6(3) . . . . ? O2 S1 C22 C23 71.2(3) . . . . ? O2 S1 C22 C27 -104.2(3) . . . . ? O3 S1 N1 C2 -105.8(3) . . . . ? O3 S1 C22 C23 -161.7(3) . . . . ? O3 S1 C22 C27 22.8(4) . . . . ? N1 S1 C22 C23 -43.8(3) . . . . ? N1 S1 C22 C27 140.8(3) . . . . ? N1 C2 C3 C4 -85.9(4) . . . . ? C1 C2 C3 C4 152.0(3) . . . . ? C1 C10 C11 C12 175.3(3) . . . . ? C1 C10 C15 C14 -175.6(3) . . . . ? C1 C16 C17 C18 -176.5(3) . . . . ? C1 C16 C21 C20 176.3(3) . . . . ? C2 C1 C10 C11 148.9(3) . . . . ? C2 C1 C10 C15 -36.2(4) . . . . ? C2 C1 C16 C17 -133.2(3) . . . . ? C2 C1 C16 C21 50.7(4) . . . . ? C2 C3 C4 C5 -172.7(3) . . . . ? C2 C3 C4 C9 7.5(5) . . . . ? C3 C4 C5 C6 -179.3(4) . . . . ? C3 C4 C9 C8 178.3(3) . . . . ? C4 C5 C6 C7 0.5(6) . . . . ? C5 C4 C9 C8 -1.6(5) . . . . ? C5 C6 C7 C8 -0.6(6) . . . . ? C6 C7 C8 C9 -0.4(6) . . . . ? C7 C8 C9 C4 1.5(5) . . . . ? C9 C4 C5 C6 0.5(5) . . . . ? C10 C1 C2 N1 173.6(2) . . . . ? C10 C1 C2 C3 -62.9(3) . . . . ? C10 C1 C16 C17 103.9(3) . . . . ? C10 C1 C16 C21 -72.2(4) . . . . ? C10 C11 C12 C13 0.3(6) . . . . ? C11 C10 C15 C14 -0.6(5) . . . . ? C11 C12 C13 C14 -0.5(6) . . . . ? C12 C13 C14 C15 0.2(6) . . . . ? C13 C14 C15 C10 0.4(6) . . . . ? C15 C10 C11 C12 0.2(5) . . . . ? C16 C1 C2 N1 53.4(3) . . . . ? C16 C1 C2 C3 176.9(3) . . . . ? C16 C1 C10 C11 -87.5(3) . . . . ? C16 C1 C10 C15 87.4(3) . . . . ? C16 C17 C18 C19 -0.2(6) . . . . ? C17 C16 C21 C20 0.1(5) . . . . ? C17 C18 C19 C20 1.0(7) . . . . ? C18 C19 C20 C21 -1.2(7) . . . . ? C19 C20 C21 C16 0.7(6) . . . . ? C21 C16 C17 C18 -0.4(5) . . . . ? C22 S1 N1 C2 140.3(2) . . . . ? C22 C23 C24 C25 0.0(7) . . . . ? C23 C22 C27 C26 0.3(7) . . . . ? C23 C24 C25 C26 0.8(7) . . . . ? C23 C24 C25 C28 179.4(5) . . . . ? C24 C25 C26 C27 -1.0(8) . . . . ? C25 C26 C27 C22 0.5(9) . . . . ? C27 C22 C23 C24 -0.6(6) . . . . ? C28 C25 C26 C27 -179.7(5) . . . . ? S2 N2 C30 C29 -164.4(2) . . . . ? S2 N2 C30 C31 71.3(3) . . . . ? S2 C50 C51 C52 177.2(4) . . . . ? S2 C50 C55 C54 -177.4(3) . . . . ? O4 C29 C30 N2 -55.9(3) . . . . ? O4 C29 C30 C31 69.8(3) . . . . ? O4 C29 C38 C39 -1.8(4) . . . . ? O4 C29 C38 C43 179.9(2) . . . . ? O4 C29 C44 C45 146.9(3) . . . . ? O4 C29 C44 C49 -40.6(3) . . . . ? O5 S2 N2 C30 164.9(2) . . . . ? O5 S2 C50 C51 48.8(3) . . . . ? O5 S2 C50 C55 -133.7(3) . . . . ? O6 S2 N2 C30 35.8(3) . . . . ? O6 S2 C50 C51 179.0(3) . . . . ? O6 S2 C50 C55 -3.5(3) . . . . ? N2 S2 C50 C51 -64.6(3) . . . . ? N2 S2 C50 C55 112.9(3) . . . . ? N2 C30 C31 C32 -138.8(3) . . . . ? C29 C30 C31 C32 99.7(3) . . . . ? C29 C38 C39 C40 -175.6(3) . . . . ? C29 C38 C43 C42 175.9(3) . . . . ? C29 C44 C45 C46 171.0(3) . . . . ? C29 C44 C49 C48 -171.6(3) . . . . ? C30 C29 C38 C39 118.0(3) . . . . ? C30 C29 C38 C43 -60.3(3) . . . . ? C30 C29 C44 C45 28.6(4) . . . . ? C30 C29 C44 C49 -158.9(3) . . . . ? C30 C31 C32 C33 -124.0(3) . . . . ? C30 C31 C32 C37 57.3(4) . . . . ? C31 C32 C33 C34 -178.5(3) . . . . ? C31 C32 C37 C36 178.7(4) . . . . ? C32 C33 C34 C35 0.2(6) . . . . ? C33 C32 C37 C36 -0.1(5) . . . . ? C33 C34 C35 C36 -0.9(6) . . . . ? C34 C35 C36 C37 1.1(6) . . . . ? C35 C36 C37 C32 -0.6(6) . . . . ? C37 C32 C33 C34 0.3(5) . . . . ? C38 C29 C30 N2 -178.9(2) . . . . ? C38 C29 C30 C31 -53.2(3) . . . . ? C38 C29 C44 C45 -91.9(3) . . . . ? C38 C29 C44 C49 80.5(3) . . . . ? C38 C39 C40 C41 -1.1(5) . . . . ? C39 C38 C43 C42 -2.5(5) . . . . ? C39 C40 C41 C42 -0.9(5) . . . . ? C40 C41 C42 C43 1.2(5) . . . . ? C41 C42 C43 C38 0.5(5) . . . . ? C43 C38 C39 C40 2.8(5) . . . . ? C44 C29 C30 N2 60.9(3) . . . . ? C44 C29 C30 C31 -173.3(2) . . . . ? C44 C29 C38 C39 -117.9(3) . . . . ? C44 C29 C38 C43 63.8(3) . . . . ? C44 C45 C46 C47 0.5(5) . . . . ? C45 C44 C49 C48 1.2(5) . . . . ? C45 C46 C47 C48 0.7(5) . . . . ? C46 C47 C48 C49 -0.9(5) . . . . ? C47 C48 C49 C44 0.0(5) . . . . ? C49 C44 C45 C46 -1.4(5) . . . . ? C50 S2 N2 C30 -81.1(3) . . . . ? C50 C51 C52 C53 -0.1(7) . . . . ? C51 C50 C55 C54 0.1(5) . . . . ? C51 C52 C53 C54 0.8(7) . . . . ? C51 C52 C53 C56 -179.6(5) . . . . ? C52 C53 C54 C55 -1.0(6) . . . . ? C53 C54 C55 C50 0.6(6) . . . . ? C55 C50 C51 C52 -0.3(6) . . . . ? C56 C53 C54 C55 179.3(4) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0000 5.0000 3.0000 0.0083 -0.0839 -0.2443 -0.0000 3.0000 5.0000 0.0513 -0.1783 -0.1752 0.0000 -3.0000 -5.0000 -0.0513 0.1783 0.1752 0.0000 -1.0000 0.0000 0.0070 -0.0072 0.0435 -3.0000 0.0000 5.0000 0.2838 -0.1071 -0.0635 3.0000 -0.0000 -5.0000 -0.2838 0.1071 0.0635 -5.0000 -3.0000 2.0000 0.4024 0.0532 0.0813 -2.0000 -1.0000 -1.0000 0.1335 0.0947 0.0399 2.0000 -0.0000 1.0000 -0.1265 -0.1020 0.0036 -0.0000 1.0000 -1.0000 -0.0215 0.0472 -0.0346 0.0000 -1.0000 1.0000 0.0215 -0.0472 0.0346