#------------------------------------------------------------------------------ #$Date: 2021-11-06 20:49:22 +0200 (Sat, 06 Nov 2021) $ #$Revision: 270365 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/89/7128938.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_7128938 loop_ _publ_author_name 'Thomas, Shibin' 'Greenacre, Victoria K.' 'Smith, Danielle E.' 'Noori, Yasir J.' 'Abdelazim, Nema M.' 'Hector, Andrew L.' 'de Groot, C. H. Kees' 'Levason, William' 'Bartlett, Philip N.' 'Reid, Gillian' _publ_section_title ; Tungsten disulfide thin films via electrodeposition from a single source precursor. ; _journal_issue 79 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 10194 _journal_page_last 10197 _journal_paper_doi 10.1039/d1cc03297f _journal_volume 57 _journal_year 2021 _chemical_formula_moiety 'S4 W, 2(C16 H36 N)' _chemical_formula_sum 'C32 H72 N2 S4 W' _chemical_formula_weight 797.00 _chemical_name_systematic (C16H72N2)WS4 _space_group_crystal_system orthorhombic _space_group_IT_number 43 _space_group_name_Hall 'F 2 -2d' _space_group_name_H-M_alt 'F d d 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-05-17 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-05-17 deposited with the CCDC. 2021-09-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 35.5582(6) _cell_length_b 28.7216(5) _cell_length_c 15.5658(4) _cell_measurement_reflns_used 13763 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 30.5820 _cell_measurement_theta_min 3.1800 _cell_volume 15897.2(6) _computing_cell_refinement 'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.906 _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 -49.00 74.00 1.00 1.00 -- -15.80 60.00 150.00 123 2 \w -105.00 -24.00 1.00 1.00 -- -15.80 -57.00-150.00 81 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RCD3): Kappa single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0037576000 _diffrn_orient_matrix_UB_12 -0.0013090000 _diffrn_orient_matrix_UB_13 -0.0446808000 _diffrn_orient_matrix_UB_21 -0.0009743000 _diffrn_orient_matrix_UB_22 -0.0246439000 _diffrn_orient_matrix_UB_23 0.0020333000 _diffrn_orient_matrix_UB_31 -0.0195697000 _diffrn_orient_matrix_UB_32 0.0009762000 _diffrn_orient_matrix_UB_33 -0.0086482000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_unetI/netI 0.0608 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.906 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 23617 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.865 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.001 _diffrn_reflns_theta_min 2.977 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 3.138 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.13205 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dark yellow' _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.332 _exptl_crystal_description block _exptl_crystal_F_000 6656 _exptl_crystal_preparation 'Slow evporation from water' _exptl_crystal_recrystallization_method 'Slow evaporation from water' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _refine_diff_density_max 2.810 _refine_diff_density_min -2.964 _refine_diff_density_rms 0.156 _refine_ls_abs_structure_details ; Flack x determined using 4164 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.005(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 354 _refine_ls_number_reflns 10952 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.054 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0572 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0978P)^2^+3.1336P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1408 _refine_ls_wR_factor_ref 0.1446 _reflns_Friedel_coverage 0.848 _reflns_Friedel_fraction_full 0.993 _reflns_Friedel_fraction_max 0.821 _reflns_number_gt 10148 _reflns_number_total 10952 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1cc03297f2.cif _cod_data_source_block tba2ws4 _cod_depositor_comments 'Adding full bibliography for 7128938.cif.' _cod_database_code 7128938 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C32H72N2WS4 _chemical_oxdiff_usercomment 'Yellow Block' _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_max 0.367 _shelx_estimated_absorpt_t_min 0.303 _reflns_odcompleteness_completeness 99.55 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 28.64 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C16) = Uanis(C20) 3.a Secondary CH2 refined with riding coordinates: C25(H25A,H25B), C23(H23A,H23B), C2(H2A,H2B), C29(H29A,H29B), C26(H26A,H26B), C17(H17A,H17B), C3(H3A,H3B), C9(H9A,H9B), C1(H1A,H1B), C18(H18A,H18B), C13(H13A,H13B), C21(H21A,H21B), C10(H10A,H10B), C19(H19A,H19B), C22(H22A,H22B), C6(H6A,H6B), C31(H31A,H31B), C11(H11A,H11B), C5(H5A,H5B), C7(H7A,H7B), C14(H14A,H14B), C30(H30A,H30B), C15(H15A,H15B), C27(H27A,H27B) 3.b Idealised Me refined as rotating group: C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C32(H32A,H32B,H32C), C24(H24A,H24B, H24C), C28(H28A,H28B,H28C), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C16(H16A,H16B, H16C) ; _shelx_res_file ; TITL tba2ws4_a.res in Fdd2 tba2ws4.res created by SHELXL-2018/3 at 14:47:47 on 17-May-2021 REM Old TITL TBA2 WS4 in Fdd2 REM SHELXT solution in Fdd2: R1 0.067, Rweak 0.030, Alpha 0.021 REM 1.076 for 160 systematic absences, Orientation as input REM Flack x = 0.051 ( 0.014 ) from 3542 Parsons' quotients REM Formula found by SHELXT: C33 N19 S4 W CELL 0.71073 35.5582 28.7216 15.5658 90 90 90 ZERR 16 0.0006 0.0005 0.0004 0 0 0 LATT -4 SYMM -X,-Y,+Z SYMM 0.25+X,0.25-Y,0.25+Z SYMM 0.25-X,0.25+Y,0.25+Z SFAC C H N S W UNIT 512 1152 32 64 16 EADP C16 C20 L.S. 10 PLAN 23 SIZE 0.5 0.5 0.4 TEMP -173.14(10) CONF BOND LIST 6 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.097800 3.133600 FVAR 0.05533 W1 5 0.706419 0.403603 0.651550 11.00000 0.01746 0.01706 = 0.01326 -0.00193 0.00022 -0.00240 S1 4 0.702603 0.478325 0.681585 11.00000 0.02751 0.01935 = 0.01762 -0.00186 -0.00097 0.00586 S2 4 0.732091 0.393667 0.524916 11.00000 0.02097 0.01985 = 0.01770 -0.00146 0.00262 0.00205 S4 4 0.741168 0.368082 0.747750 11.00000 0.04772 0.01979 = 0.01966 0.00345 -0.00902 0.00236 S3 4 0.650541 0.372258 0.648750 11.00000 0.02605 0.05321 = 0.03829 -0.02483 0.01169 -0.01700 N1 3 0.705384 0.532811 0.414148 11.00000 0.02372 0.01537 = 0.00857 -0.00079 0.00128 -0.00012 C25 1 0.740178 0.510553 0.455120 11.00000 0.01960 0.01913 = 0.01602 -0.00464 0.00229 0.00342 AFIX 23 H25A 2 0.737547 0.512258 0.518358 11.00000 -1.20000 H25B 2 0.740809 0.477208 0.439079 11.00000 -1.20000 AFIX 0 C23 1 0.601334 0.503141 0.464397 11.00000 0.02454 0.02947 = 0.02332 0.00547 0.00358 -0.00112 AFIX 23 H23A 2 0.602488 0.509929 0.526696 11.00000 -1.20000 H23B 2 0.603747 0.469047 0.456835 11.00000 -1.20000 AFIX 0 N2 3 0.673950 0.219582 0.552756 11.00000 0.01491 0.01967 = 0.02087 0.00359 -0.00354 0.00143 C2 1 0.672039 0.137560 0.617444 11.00000 0.02979 0.02256 = 0.04404 0.00946 0.00218 0.00259 AFIX 23 H2A 2 0.684762 0.149298 0.669705 11.00000 -1.20000 H2B 2 0.691380 0.124857 0.578153 11.00000 -1.20000 AFIX 0 C29 1 0.705605 0.584938 0.425730 11.00000 0.02343 0.01362 = 0.01845 -0.00138 0.00412 0.00042 AFIX 23 H29A 2 0.683322 0.598036 0.396239 11.00000 -1.20000 H29B 2 0.728231 0.597688 0.397092 11.00000 -1.20000 AFIX 0 C26 1 0.777331 0.532426 0.430171 11.00000 0.01918 0.02381 = 0.02351 -0.00177 -0.00203 -0.00103 AFIX 23 H26A 2 0.779814 0.563229 0.458145 11.00000 -1.20000 H26B 2 0.778141 0.537113 0.367188 11.00000 -1.20000 AFIX 0 C17 1 0.705364 0.523917 0.317277 11.00000 0.02286 0.02046 = 0.00997 0.00290 -0.00031 -0.00069 AFIX 23 H17A 2 0.684074 0.541235 0.291616 11.00000 -1.20000 H17B 2 0.728818 0.536973 0.292900 11.00000 -1.20000 AFIX 0 C3 1 0.643608 0.099235 0.641554 11.00000 0.04271 0.02405 = 0.03447 0.00795 0.01345 -0.00090 AFIX 23 H3A 2 0.627694 0.092410 0.590909 11.00000 -1.20000 H3B 2 0.657576 0.070479 0.656104 11.00000 -1.20000 AFIX 0 C9 1 0.646657 0.254381 0.513952 11.00000 0.01659 0.02133 = 0.01936 0.00328 -0.00246 0.00189 AFIX 23 H9A 2 0.630707 0.266751 0.560820 11.00000 -1.20000 H9B 2 0.629934 0.237369 0.473946 11.00000 -1.20000 AFIX 0 C1 1 0.650746 0.176841 0.573707 11.00000 0.01651 0.01788 = 0.02488 0.00223 0.00300 0.00012 AFIX 23 H1A 2 0.639753 0.164748 0.519702 11.00000 -1.20000 H1B 2 0.629663 0.186342 0.611368 11.00000 -1.20000 AFIX 0 C12 1 0.645351 0.367676 0.382556 11.00000 0.03848 0.02353 = 0.03578 0.00982 -0.01311 -0.00281 AFIX 137 H12A 2 0.660865 0.356556 0.334736 11.00000 -1.50000 H12B 2 0.660502 0.387701 0.419981 11.00000 -1.50000 H12C 2 0.624003 0.385450 0.359971 11.00000 -1.50000 AFIX 0 C18 1 0.702380 0.473475 0.290016 11.00000 0.05731 0.01897 = 0.01257 -0.00334 0.00154 0.00539 AFIX 23 H18A 2 0.681119 0.458458 0.320322 11.00000 -1.20000 H18B 2 0.725739 0.456741 0.305646 11.00000 -1.20000 AFIX 0 C13 1 0.693303 0.239763 0.632742 11.00000 0.02553 0.02769 = 0.02153 0.00233 -0.00866 -0.00393 AFIX 23 H13A 2 0.714935 0.219553 0.647317 11.00000 -1.20000 H13B 2 0.703470 0.270808 0.617764 11.00000 -1.20000 AFIX 0 C21 1 0.671373 0.510734 0.456590 11.00000 0.02145 0.02093 = 0.01848 0.00107 0.00036 -0.00236 AFIX 23 H21A 2 0.671995 0.517901 0.518785 11.00000 -1.20000 H21B 2 0.673128 0.476508 0.450220 11.00000 -1.20000 AFIX 0 C10 1 0.663433 0.295472 0.465857 11.00000 0.02265 0.01653 = 0.02118 0.00054 0.00003 0.00077 AFIX 23 H10A 2 0.678562 0.284321 0.416589 11.00000 -1.20000 H10B 2 0.680031 0.313602 0.504438 11.00000 -1.20000 AFIX 0 C19 1 0.696251 0.470587 0.193927 11.00000 0.03275 0.02668 = 0.01009 -0.00417 -0.00213 -0.00484 AFIX 23 H19A 2 0.717891 0.485161 0.164292 11.00000 -1.20000 H19B 2 0.673437 0.488549 0.178742 11.00000 -1.20000 AFIX 0 C22 1 0.633641 0.527024 0.419852 11.00000 0.02254 0.03383 = 0.02529 0.01134 0.00334 -0.00375 AFIX 23 H22A 2 0.631293 0.561139 0.427193 11.00000 -1.20000 H22B 2 0.632711 0.520071 0.357594 11.00000 -1.20000 AFIX 0 C6 1 0.693377 0.182807 0.410407 11.00000 0.02695 0.02199 = 0.02876 0.00183 0.00364 0.00459 AFIX 23 H6A 2 0.672368 0.199973 0.383228 11.00000 -1.20000 H6B 2 0.684506 0.151000 0.424190 11.00000 -1.20000 AFIX 0 C20 1 0.691754 0.420567 0.161676 11.00000 0.06861 0.04813 = 0.02496 -0.00257 -0.00953 0.01583 AFIX 137 H20A 2 0.691180 0.420451 0.098732 11.00000 -1.50000 H20B 2 0.668224 0.407492 0.183869 11.00000 -1.50000 H20C 2 0.712979 0.401722 0.181774 11.00000 -1.50000 AFIX 0 C32 1 0.746380 0.673121 0.496424 11.00000 0.05336 0.02800 = 0.04412 -0.00995 0.00313 -0.00924 AFIX 137 H32A 2 0.750833 0.666685 0.435438 11.00000 -1.50000 H32B 2 0.765741 0.657684 0.531012 11.00000 -1.50000 H32C 2 0.747407 0.706788 0.506383 11.00000 -1.50000 AFIX 0 C31 1 0.708197 0.654992 0.521691 11.00000 0.04690 0.02189 = 0.03521 -0.00740 0.00032 0.00886 AFIX 23 H31A 2 0.689060 0.668497 0.482791 11.00000 -1.20000 H31B 2 0.702395 0.665556 0.580763 11.00000 -1.20000 AFIX 0 C11 1 0.630858 0.326177 0.433855 11.00000 0.02868 0.02252 = 0.01545 0.00121 -0.00277 -0.00306 AFIX 23 H11A 2 0.613900 0.307353 0.397278 11.00000 -1.20000 H11B 2 0.616177 0.337507 0.483688 11.00000 -1.20000 AFIX 0 C5 1 0.705180 0.207332 0.491985 11.00000 0.01398 0.02622 = 0.03382 0.00766 0.00057 -0.00100 AFIX 23 H5A 2 0.723341 0.187205 0.522721 11.00000 -1.20000 H5B 2 0.718520 0.236333 0.476077 11.00000 -1.20000 AFIX 0 C24 1 0.563468 0.518979 0.429279 11.00000 0.02368 0.03894 = 0.05883 0.00897 0.00547 -0.00384 AFIX 137 H24A 2 0.561394 0.510012 0.368718 11.00000 -1.50000 H24B 2 0.561430 0.552894 0.434363 11.00000 -1.50000 H24C 2 0.543209 0.504224 0.462154 11.00000 -1.50000 AFIX 0 C7 1 0.726715 0.180092 0.347806 11.00000 0.02707 0.03794 = 0.03482 0.01250 0.00936 0.00994 AFIX 23 H7A 2 0.733597 0.211988 0.329522 11.00000 -1.20000 H7B 2 0.748634 0.166543 0.378020 11.00000 -1.20000 AFIX 0 C14 1 0.669161 0.244869 0.711769 11.00000 0.03175 0.04119 = 0.02335 -0.00497 -0.01046 0.00630 AFIX 23 H14A 2 0.653621 0.216555 0.719202 11.00000 -1.20000 H14B 2 0.652014 0.271738 0.704500 11.00000 -1.20000 AFIX 0 C28 1 0.812735 0.456094 0.406376 11.00000 0.02556 0.02753 = 0.03101 -0.00142 0.00823 0.00662 AFIX 137 H28A 2 0.810069 0.463027 0.345033 11.00000 -1.50000 H28B 2 0.792701 0.434758 0.424248 11.00000 -1.50000 H28C 2 0.837250 0.441555 0.416760 11.00000 -1.50000 AFIX 0 C30 1 0.705352 0.601352 0.518231 11.00000 0.03570 0.02324 = 0.02031 -0.00210 0.00504 0.00396 AFIX 23 H30A 2 0.726822 0.587393 0.549474 11.00000 -1.20000 H30B 2 0.681846 0.591104 0.546588 11.00000 -1.20000 AFIX 0 C8 1 0.718243 0.151228 0.269428 11.00000 0.04999 0.04018 = 0.03399 0.00490 0.01539 0.02300 AFIX 137 H8A 2 0.738924 0.154174 0.228170 11.00000 -1.50000 H8B 2 0.694861 0.162205 0.242957 11.00000 -1.50000 H8C 2 0.715427 0.118516 0.286135 11.00000 -1.50000 AFIX 0 C15 1 0.693230 0.252143 0.790989 11.00000 0.04127 0.05150 = 0.03453 -0.00562 -0.00932 -0.02339 AFIX 23 H15A 2 0.713090 0.228003 0.792709 11.00000 -1.20000 H15B 2 0.705698 0.282896 0.787270 11.00000 -1.20000 AFIX 0 C4 1 0.618336 0.112035 0.716659 11.00000 0.05870 0.03109 = 0.05490 0.00791 0.01430 -0.00682 AFIX 137 H4A 2 0.600585 0.136256 0.698714 11.00000 -1.50000 H4B 2 0.633744 0.123675 0.764238 11.00000 -1.50000 H4C 2 0.604384 0.084430 0.735458 11.00000 -1.50000 AFIX 0 C27 1 0.809917 0.501024 0.457743 11.00000 0.02256 0.03709 = 0.02344 -0.00376 -0.00294 0.00366 AFIX 23 H27A 2 0.833762 0.518499 0.451554 11.00000 -1.20000 H27B 2 0.806858 0.493172 0.519276 11.00000 -1.20000 AFIX 0 C16 1 0.670665 0.249848 0.872200 11.00000 0.06861 0.04813 = 0.02496 -0.00257 -0.00953 0.01583 AFIX 137 H16A 2 0.649624 0.271802 0.868683 11.00000 -1.50000 H16B 2 0.686703 0.258033 0.921122 11.00000 -1.50000 H16C 2 0.660914 0.218209 0.879897 11.00000 -1.50000 AFIX 0 HKLF 4 REM tba2ws4_a.res in Fdd2 REM wR2 = 0.1446, GooF = S = 1.054, Restrained GooF = 1.054 for all data REM R1 = 0.0572 for 10148 Fo > 4sig(Fo) and 0.0623 for all 10952 data REM 354 parameters refined using 1 restraints END WGHT 0.0978 3.1848 REM Highest difference peak 2.810, deepest hole -2.964, 1-sigma level 0.156 Q1 1 0.6974 0.4045 0.6510 11.00000 0.05 2.81 Q2 1 0.7088 0.4072 0.7078 11.00000 0.05 2.39 Q3 1 0.6990 0.4007 0.5976 11.00000 0.05 2.30 Q4 1 0.7099 0.4065 0.5939 11.00000 0.05 2.30 Q5 1 0.7134 0.4195 0.6523 11.00000 0.05 2.14 Q6 1 0.6972 0.4015 0.7047 11.00000 0.05 1.76 Q7 1 0.7015 0.4020 0.7618 11.00000 0.05 0.77 Q8 1 0.7050 0.4101 0.4907 11.00000 0.05 0.74 Q9 1 0.7945 0.5895 0.3100 11.00000 0.05 0.72 Q10 1 0.6992 0.4034 0.5388 11.00000 0.05 0.56 Q11 1 0.6819 0.2812 0.8597 11.00000 0.05 0.53 Q12 1 0.6508 0.3936 0.6118 11.00000 0.05 0.52 Q13 1 0.6604 0.3620 0.7182 11.00000 0.05 0.52 Q14 1 0.7369 0.3727 0.8033 11.00000 0.05 0.50 Q15 1 0.7478 0.3743 0.5257 11.00000 0.05 0.50 Q16 1 0.7098 0.4749 0.7395 11.00000 0.05 0.48 Q17 1 0.6286 0.3511 0.6513 11.00000 0.05 0.47 Q18 1 0.7431 0.4027 0.5284 11.00000 0.05 0.45 Q19 1 0.7202 0.1606 0.4006 11.00000 0.05 0.45 Q20 1 0.7088 0.4065 0.3941 11.00000 0.05 0.45 Q21 1 0.7300 0.3509 0.8069 11.00000 0.05 0.45 Q22 1 0.7553 0.4000 0.7626 11.00000 0.05 0.44 Q23 1 0.7125 0.4988 0.6813 11.00000 0.05 0.43 ; _shelx_res_checksum 41395 _shelx_hkl_file ; 0 0 -12 732.80 46.03 0 0 -10 5.96 9.02 0 0 -8 4511.37 129.52 0 0 -6 -5.64 5.19 0 0 -4 7713.65 178.54 0 0 4 9999.00 220.55 0 0 6 5.87 3.74 0 0 8 4758.58 132.93 0 0 8 6169.92 142.88 0 0 10 5.20 5.06 0 0 12 1390.71 67.92 0 0 14 -2.48 6.71 0 0 16 1258.96 83.85 0 0 18 35.32 21.02 0 0 20 737.02 86.09 0 -2 -14 67.62 15.46 0 -2 -12 8.87 7.03 0 -2 -10 166.24 20.24 0 -2 -8 2.29 5.65 0 2 -6 778.18 35.62 0 -2 -6 728.79 33.02 0 -2 -4 2.47 2.47 0 2 -2 23.64 2.94 0 -2 -2 26.12 2.47 0 -2 2 63.59 5.26 0 -2 4 -0.79 2.59 0 2 4 0.53 1.58 0 -2 4 3.65 2.55 0 -2 6 819.96 34.92 0 2 6 790.83 29.02 0 -2 8 -0.88 3.81 0 2 8 6.63 4.65 0 -2 8 -2.80 5.37 0 -2 10 250.61 23.84 0 2 10 180.05 19.16 0 -2 12 -0.52 5.48 0 2 12 1.15 5.78 0 2 14 201.63 27.61 0 -2 14 148.48 24.66 0 -2 16 11.39 12.95 0 2 16 -3.96 9.90 0 -2 18 57.24 26.83 0 2 18 53.53 20.67 0 -2 20 47.53 30.59 0 2 20 1.89 17.17 0 -4 -16 557.41 45.41 0 -4 -14 8.83 7.94 0 -4 -12 1049.11 57.68 0 -4 -10 3.72 5.62 0 -4 -8 3998.97 112.71 0 -4 -6 7.23 4.46 0 -4 -4 1092.23 32.48 0 4 -4 1171.11 35.29 0 -4 -2 1.20 1.01 0 4 -2 -1.53 2.90 0 -4 2 1.52 2.06 0 4 2 0.66 0.67 0 4 4 875.25 24.94 0 -4 4 824.27 32.01 0 4 6 3.31 2.43 0 -4 6 -0.75 4.90 0 -4 6 3.33 3.82 0 -4 8 4368.32 125.25 0 4 8 4558.58 110.19 0 -4 8 4370.01 123.08 0 -4 10 -1.62 4.45 0 4 12 1656.36 72.45 0 -4 12 1828.06 83.42 0 4 14 5.51 6.84 0 -4 14 23.22 15.59 0 4 16 1089.88 74.60 0 -4 16 1139.85 83.93 0 -4 18 48.12 27.34 0 4 18 21.92 16.64 0 -4 20 427.95 67.56 0 4 20 435.22 64.71 0 -6 -16 -9.74 7.13 0 -6 -14 1043.69 61.44 0 -6 -12 15.65 10.16 0 -6 -10 1026.85 49.21 0 -6 -8 6.71 3.28 0 6 -6 1741.40 51.78 0 -6 -6 1643.32 49.91 0 -6 -4 0.58 1.17 0 6 -4 1.03 2.39 0 6 -2 6185.30 137.46 0 6 0 1.08 1.09 0 -6 0 0.14 0.82 0 6 2 6866.57 149.57 0 -6 2 6859.69 155.14 0 6 2 7335.60 148.54 0 -6 4 2.25 1.98 0 6 4 1.49 1.21 0 -6 6 2266.93 74.04 0 -6 6 2379.08 76.20 0 6 6 2468.90 60.54 0 -6 8 8.12 5.92 0 -6 8 11.43 7.60 0 6 8 -4.76 2.29 0 -6 10 1068.56 56.21 0 -6 12 15.12 11.13 0 -6 14 1688.44 93.04 0 6 14 1709.55 81.42 0 6 16 0.74 10.15 0 -6 16 21.55 18.55 0 -6 18 1038.24 91.55 0 6 18 1003.77 81.01 0 -6 20 28.37 27.33 0 6 20 9.01 23.48 0 -8 -18 4.11 9.07 0 -8 -16 82.92 19.66 0 -8 -14 21.93 11.83 0 -8 -12 42.82 12.02 0 -8 -10 -1.97 4.02 0 -8 -8 250.81 18.14 0 -8 -6 4.41 2.84 0 8 -6 -1.25 2.56 0 8 -4 247.93 15.31 0 -8 -4 254.41 11.28 0 -8 -2 -0.21 0.48 0 8 -2 6.62 2.74 0 8 0 4207.83 92.52 0 -8 0 4289.67 91.84 0 -8 2 0.89 1.65 0 8 2 -0.08 0.56 0 8 4 304.04 11.31 0 -8 4 308.55 18.76 0 -8 6 7.50 4.40 0 8 6 1.85 2.14 0 8 8 270.34 14.37 0 -8 8 224.39 22.64 0 -8 8 273.95 24.13 0 -8 10 -5.55 6.13 0 -8 12 39.43 13.38 0 -8 14 -5.33 7.80 0 8 16 90.30 21.04 0 -8 16 110.04 30.76 0 8 18 -1.40 10.10 0 -8 18 9.11 12.04 0 -8 20 82.55 37.03 0 8 20 59.54 28.32 0 -10 -18 338.45 39.56 0 -10 -16 2.58 9.91 0 -10 -14 663.51 47.71 0 -10 -12 1.14 5.81 0 -10 -10 1625.26 61.41 0 10 -8 1.36 3.42 0 -10 -8 1.05 2.72 0 -10 -6 3200.76 78.34 0 10 -6 2986.50 84.76 0 10 -4 -3.17 4.43 0 -10 -4 0.68 1.89 0 10 -2 3528.41 83.67 0 -10 -2 3424.62 75.93 0 -10 0 1.77 1.19 0 10 0 1.87 1.37 0 10 2 2968.08 66.85 0 -10 2 2803.93 70.01 0 10 4 0.00 1.29 0 10 4 1.40 1.66 0 10 6 3497.06 81.51 0 -10 6 3547.86 102.58 0 -10 8 5.55 6.96 0 -10 8 14.55 10.59 0 10 8 -0.40 1.95 0 -10 10 1994.02 84.81 0 -10 12 20.48 9.35 0 -10 14 1146.49 76.29 0 -10 16 2.56 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16.67 12 2 -6 214.92 17.37 12 -2 -6 211.57 12.46 12 2 -6 211.04 14.39 12 -2 -4 98.31 9.81 12 2 -4 116.25 11.20 12 -2 -4 114.33 6.90 12 2 -4 110.10 7.57 -12 -2 -2 536.59 18.00 12 -2 -2 560.19 22.10 12 2 -2 575.27 15.41 12 2 -2 574.08 22.79 12 -2 -2 548.76 15.82 12 -2 0 308.72 12.09 12 2 0 323.71 13.86 -12 -2 0 325.32 13.14 -12 2 0 318.41 11.15 -12 -2 2 706.22 25.39 12 2 2 734.93 22.32 12 -2 2 694.70 20.03 -12 2 2 677.83 23.84 12 2 4 89.93 6.99 -12 2 4 98.64 5.84 -12 -2 4 91.94 5.45 -12 2 4 99.66 11.55 -12 -2 4 94.16 11.02 12 -2 4 100.04 6.39 12 2 6 387.39 25.01 12 2 6 389.08 16.91 -12 2 6 337.02 14.23 -12 -2 6 379.99 15.36 -12 -2 6 341.38 25.76 -12 2 6 320.67 24.23 12 2 8 107.71 14.05 -12 2 8 125.81 16.69 12 -2 8 161.72 20.76 -12 2 8 115.08 8.79 -12 -2 8 115.78 9.36 -12 -2 8 107.20 16.91 -12 -2 10 96.07 17.30 -12 2 10 89.05 16.20 -12 2 12 9.45 6.28 -12 -2 12 19.65 13.23 -12 2 14 53.75 19.64 -12 -2 14 94.20 23.69 12 -2 16 9.52 7.78 -12 -2 16 17.91 15.26 -12 2 16 14.36 16.03 12 2 18 75.45 19.26 12 -2 18 80.17 21.72 -12 2 18 119.35 32.78 -12 -2 18 114.97 34.45 12 2 20 4.09 9.09 12 -2 20 9.27 11.27 -12 2 20 50.58 32.99 -12 -2 20 13.76 23.78 12 -4 -20 168.23 29.56 12 -4 -18 0.93 12.74 12 -4 -16 590.09 46.95 12 -4 -14 13.96 8.90 12 4 -14 3.72 8.98 12 4 -12 527.22 37.87 12 -4 -12 437.76 31.94 12 4 -10 23.45 6.97 12 -4 -10 37.61 7.70 12 4 -8 518.00 29.20 12 -4 -8 503.22 24.09 12 4 -8 492.71 30.24 12 4 -6 85.89 10.40 12 4 -6 81.31 11.42 12 -4 -6 75.37 7.07 12 -4 -4 902.01 30.84 12 4 -4 817.99 33.99 12 4 -4 851.76 28.63 12 -4 -4 825.99 24.42 -12 -4 -2 206.39 10.35 12 -4 -2 222.12 12.21 12 -4 -2 219.00 8.60 12 4 -2 219.21 8.30 12 4 -2 229.71 13.98 -12 4 0 757.99 19.41 12 4 0 771.87 25.50 -12 -4 0 757.87 24.52 12 -4 0 759.85 21.33 12 4 2 234.70 11.51 -12 -4 2 221.64 13.40 -12 -4 2 245.79 7.34 12 -4 2 237.60 8.81 -12 4 2 242.48 11.90 12 4 4 1037.64 30.90 -12 4 4 999.71 27.35 -12 -4 4 1016.80 26.80 -12 -4 4 982.61 39.03 -12 4 4 1036.12 38.90 12 4 4 938.64 36.36 12 4 6 83.67 11.13 12 4 6 73.26 7.07 -12 4 6 63.07 5.54 -12 4 6 62.38 10.33 -12 -4 6 73.57 6.41 -12 -4 6 89.56 13.38 -12 4 8 618.90 39.50 -12 4 8 588.59 22.23 -12 -4 8 620.04 40.01 -12 -4 8 529.75 23.47 12 4 8 625.36 32.72 -12 -4 10 58.94 14.47 -12 4 10 60.70 14.42 -12 4 12 541.90 47.18 -12 -4 12 587.18 49.01 12 -4 14 2.54 7.80 -12 4 14 11.46 14.63 -12 -4 14 19.30 16.13 12 -4 16 996.30 67.94 -12 4 16 989.52 80.78 -12 -4 16 1070.23 84.05 12 4 18 14.09 10.16 -12 4 18 19.78 20.12 12 -4 18 16.18 13.80 -12 -4 18 24.17 22.34 12 4 20 314.88 44.87 12 -4 20 332.69 50.09 -12 -4 20 423.70 67.23 12 -6 -18 273.03 33.86 12 -6 -16 13.57 11.18 12 -6 -14 724.84 45.51 12 -6 -12 17.69 7.71 12 6 -10 1146.34 54.84 12 -6 -10 1243.97 47.39 12 6 -8 28.83 8.19 12 -6 -8 25.28 5.16 12 -6 -6 1959.97 52.37 12 6 -6 2058.86 66.69 12 6 -6 1922.25 64.02 12 6 -4 35.87 6.40 12 -6 -4 26.97 3.22 12 6 -4 36.66 7.55 -12 -6 -2 2104.43 51.88 12 -6 -2 2026.22 50.16 12 -6 -2 1910.93 47.06 12 6 -2 2051.26 57.45 12 6 -2 2016.26 49.98 12 6 0 556.92 21.58 12 -6 0 581.70 16.30 -12 6 0 551.55 13.75 -12 -6 0 545.24 20.56 -12 -6 2 1847.82 51.74 12 6 2 1870.21 44.47 12 -6 2 1876.61 40.26 -12 6 2 1923.29 46.28 12 6 2 1833.50 47.77 -12 -6 4 24.19 6.63 12 6 4 18.12 3.49 -12 6 4 24.75 4.01 -12 -6 4 22.36 3.04 12 6 4 17.87 3.54 -12 6 6 2023.00 70.98 -12 6 6 2197.17 53.48 -12 -6 6 2086.60 55.57 -12 -6 6 2151.31 74.02 12 6 6 2095.22 57.34 12 6 6 2052.73 62.07 -12 6 8 41.70 10.57 -12 6 8 26.63 4.23 12 6 8 36.71 7.17 -12 -6 8 29.85 5.61 -12 -6 8 43.22 11.39 -12 6 10 1579.36 73.76 -12 -6 10 1614.78 76.95 12 -6 12 46.28 11.11 -12 6 12 38.76 15.95 -12 -6 12 71.72 19.84 12 -6 14 1008.43 62.66 -12 6 14 1175.97 76.82 -12 -6 14 1026.95 74.30 12 -6 16 16.00 11.16 -12 6 16 42.28 21.84 -12 -6 16 38.73 18.10 12 -6 18 485.18 55.30 -12 6 18 475.18 60.68 -12 6 20 0.34 19.18 12 6 20 28.75 17.39 12 -6 20 26.58 21.33 12 -8 -18 34.71 15.40 12 -8 -16 17.82 9.74 12 -8 -14 21.46 8.59 12 -8 -12 9.76 5.02 12 -8 -10 55.37 8.56 12 -8 -8 58.50 7.37 12 -8 -6 158.52 10.14 12 8 -6 139.13 14.50 12 -8 -4 35.67 4.07 12 8 -4 42.74 7.55 -12 -8 -4 43.01 5.17 12 8 -2 93.20 9.17 -12 -8 -2 79.10 7.01 -12 -8 0 28.05 4.45 12 8 0 20.08 4.31 12 8 2 121.83 8.68 12 -8 2 115.46 3.74 12 8 2 113.03 3.82 -12 8 2 118.18 7.19 12 8 4 30.07 4.16 -12 8 4 26.62 5.46 -12 -8 4 27.59 6.24 -12 -8 4 21.06 3.14 12 8 4 26.47 3.70 12 -8 6 121.66 10.98 -12 8 6 128.11 14.43 12 8 6 139.63 10.60 -12 8 6 132.25 8.35 -12 -8 6 113.44 14.63 -12 -8 6 126.76 10.03 12 8 6 127.99 10.12 12 -8 8 66.60 10.09 -12 8 8 71.17 12.74 -12 -8 8 78.48 9.45 12 8 8 89.72 9.81 -12 -8 8 107.30 17.21 12 -8 10 88.19 13.45 -12 8 10 95.73 17.32 -12 -8 10 87.29 16.99 12 -8 12 10.20 6.43 -12 8 12 8.52 8.73 -12 -8 12 17.00 12.88 12 -8 14 57.22 15.70 -12 8 14 50.43 17.37 -12 -8 14 73.88 21.93 -12 8 16 7.88 14.35 12 -8 16 11.15 10.28 -12 -8 16 38.75 19.45 -12 -8 18 83.57 27.31 -12 8 18 119.20 33.82 12 -8 18 76.10 25.61 12 -8 20 16.65 19.46 -12 8 20 7.52 19.60 12 -10 -18 446.72 43.99 12 -10 -16 38.96 14.03 12 -10 -14 734.42 44.20 12 -10 -12 64.85 11.39 -12 -10 -10 844.86 49.45 12 -10 -10 836.29 35.86 -12 -10 -8 196.52 20.97 12 -10 -8 175.86 12.94 12 10 -6 1358.11 53.70 -12 -10 -6 1438.86 55.99 12 -10 -6 1458.83 41.31 -12 -10 -4 83.92 10.56 -12 -10 -4 66.62 6.96 12 -10 -4 71.34 5.79 12 10 -4 75.69 10.30 12 10 -2 2853.12 78.97 -12 -10 -2 2976.67 73.67 12 10 0 523.09 22.12 -12 -10 0 468.65 20.44 -12 10 2 3150.13 35.17 12 10 2 3206.64 16.90 12 10 2 3242.54 46.98 -12 -10 4 95.21 10.90 12 10 4 77.26 5.04 12 -10 4 80.59 7.63 -12 10 4 87.89 9.11 12 10 4 74.97 7.56 -12 -10 4 82.55 7.31 12 -10 6 1776.44 55.34 -12 10 6 1741.54 59.30 12 10 6 1780.07 46.01 -12 -10 6 1872.58 52.87 -12 -10 6 1895.53 66.32 12 10 8 195.88 12.98 12 -10 8 198.00 18.38 -12 10 8 215.30 20.46 -12 -10 8 187.42 21.57 -12 -10 8 253.41 17.10 12 -10 10 1070.74 52.58 -12 10 10 1057.22 55.37 -12 -10 10 1075.06 61.14 12 -10 12 93.54 17.32 -12 10 12 67.03 15.82 -12 -10 12 66.46 17.71 12 -10 14 1157.10 70.91 -12 10 14 1170.50 73.96 -12 -10 14 941.04 70.34 -12 10 16 68.57 21.56 12 -10 16 75.26 21.28 -12 -10 16 107.24 27.43 -12 10 18 712.89 72.32 12 -10 18 811.75 74.70 -12 -10 18 621.16 69.34 -12 10 20 21.20 23.91 12 -10 20 18.38 20.95 12 -12 -18 37.47 15.94 12 -12 -16 85.00 17.93 12 -12 -14 1.32 6.55 -12 -12 -12 268.71 29.87 12 -12 -12 246.09 21.10 -12 -12 -10 115.72 18.53 12 -12 -10 101.69 11.56 -12 -12 -8 616.44 38.56 12 -12 -8 610.67 26.09 -12 -12 -6 43.08 9.63 12 -12 -6 35.23 4.92 12 -12 -4 455.56 17.56 12 12 -4 482.19 26.70 -12 -12 -4 441.02 23.68 -12 -12 -4 494.51 20.96 -12 -12 -2 219.24 11.48 -12 -12 -2 222.09 13.38 12 12 -2 246.59 16.88 -12 -12 0 863.28 30.70 12 12 0 857.07 32.23 -12 12 2 255.88 10.08 -12 -12 2 250.17 15.09 -12 -12 2 -0.04 0.85 12 12 2 262.69 14.21 12 -12 4 474.00 20.06 12 12 4 451.44 21.06 -12 12 4 441.95 21.09 -12 -12 4 414.78 24.68 12 12 4 465.91 14.07 -12 -12 4 509.45 21.75 -12 -12 6 29.37 6.91 -12 12 6 41.78 7.76 12 -12 6 34.74 6.41 12 12 6 40.84 4.31 -12 -12 6 35.76 6.38 12 -12 8 702.56 37.32 12 12 8 688.41 25.40 -12 -12 8 703.72 32.65 -12 12 8 686.50 37.35 -12 -12 8 702.80 42.58 -12 12 10 154.37 19.40 12 -12 10 147.37 19.42 -12 -12 10 146.30 21.26 -12 12 12 445.17 37.96 12 -12 12 432.04 37.82 -12 -12 12 437.65 41.84 -12 12 14 4.92 9.95 12 -12 14 39.38 15.33 -12 -12 14 7.53 10.99 -12 12 16 184.79 32.44 -12 -12 16 210.34 35.78 12 -12 16 196.44 33.61 -12 12 18 9.37 15.97 -12 -12 18 32.45 18.32 12 -12 18 14.38 11.58 12 -12 20 152.04 38.64 12 -14 -18 84.62 18.72 12 -14 -16 3.54 8.41 12 -14 -14 130.13 17.64 -12 -14 -12 20.31 12.37 12 -14 -12 39.52 9.78 -12 -14 -10 449.94 36.61 12 -14 -10 428.77 24.24 12 -14 -8 106.65 9.94 -12 -14 -8 110.09 16.02 12 -14 -6 440.79 19.12 -12 -14 -6 454.30 28.38 12 14 -4 214.28 17.61 -12 -14 -4 231.61 14.12 12 -14 -4 248.78 12.33 -12 -14 -4 215.49 14.82 -12 -14 -2 579.85 19.34 12 14 -2 613.36 28.62 -12 -14 -2 572.66 24.06 -12 -14 0 537.15 23.98 12 14 0 565.04 25.83 -12 -14 0 578.79 14.36 -12 14 2 672.24 15.62 -12 -14 2 641.66 17.77 -12 -14 2 617.85 24.64 -12 14 4 267.63 15.26 -12 -14 4 268.46 19.27 12 14 4 264.14 9.39 12 -14 4 247.31 12.77 -12 -14 4 267.68 16.48 12 14 6 424.88 15.32 -12 14 6 437.43 24.26 -12 -14 6 409.48 27.85 12 -14 6 422.20 24.08 -12 -14 6 404.31 23.40 -12 -14 8 114.50 12.85 -12 -14 8 115.14 17.14 -12 14 8 127.13 15.12 12 14 8 119.75 8.64 12 -14 8 120.03 15.21 -12 14 10 494.03 34.43 12 -14 10 507.18 36.97 -12 -14 10 480.46 39.64 12 -14 12 74.02 15.84 -12 14 12 41.13 12.85 -12 -14 12 46.89 15.53 -12 14 14 191.35 27.93 -12 -14 14 184.51 30.40 12 -14 14 246.14 33.70 -12 14 16 2.70 9.60 12 -14 16 23.36 17.99 -12 -14 16 3.55 15.17 -12 14 18 103.07 26.65 12 -14 18 97.71 28.72 -12 -14 18 112.84 31.03 12 -14 20 45.10 30.15 12 -16 -18 6.85 10.83 12 -16 -16 327.28 32.11 -12 -16 -14 17.54 13.22 12 -16 -14 0.89 5.34 -12 -16 -12 594.69 46.19 12 -16 -12 524.11 31.43 -12 -16 -10 84.54 15.93 12 -16 -10 94.31 11.36 12 -16 -8 1176.61 40.68 -12 -16 -8 1252.34 57.53 12 -16 -6 28.13 4.41 -12 -16 -6 46.47 8.91 -12 -16 -4 1590.09 48.75 12 -16 -4 1576.27 44.21 -12 -16 -4 1627.44 49.06 -12 -16 -2 65.06 5.24 -12 -16 -2 47.76 6.60 -12 -16 0 3503.45 91.16 -12 -16 0 3613.57 76.39 -12 -16 2 73.46 8.81 -12 16 2 -0.09 0.41 12 -16 4 1847.53 46.87 -12 -16 4 1879.68 62.38 -12 16 4 1839.23 44.94 -12 -16 4 1790.62 55.88 -12 -16 6 27.16 7.19 -12 16 6 25.32 5.69 -12 -16 6 45.34 9.72 12 16 6 28.96 3.50 12 -16 6 34.50 7.08 -12 -16 8 1224.59 59.74 -12 16 8 1406.57 53.96 12 -16 8 1334.56 54.73 12 16 8 1343.89 38.06 -12 -16 8 1300.31 51.55 -12 -16 10 101.26 18.20 -12 16 10 98.97 14.42 12 -16 10 77.00 13.85 -12 16 12 771.32 48.72 12 -16 12 839.69 54.11 -12 -16 12 869.94 59.60 -12 -16 14 5.10 9.60 -12 16 14 13.46 10.44 12 -16 14 15.25 12.27 12 -16 16 486.00 51.30 -12 16 16 416.40 44.68 -12 -16 16 453.42 51.04 -12 16 18 20.03 16.31 12 -16 18 25.67 19.75 -12 -16 18 0.55 16.41 12 -16 20 287.33 48.53 12 -18 -16 24.68 10.96 -12 -18 -14 42.38 17.19 12 -18 -14 25.91 9.90 -12 -18 -12 101.73 19.78 12 -18 -12 106.43 13.73 -12 -18 -10 17.01 10.50 12 -18 -10 7.62 4.74 -12 -18 -8 126.45 17.20 12 -18 -8 111.53 10.70 12 -18 -6 22.15 4.68 -12 -18 -6 27.54 7.04 -12 -18 -4 87.93 8.66 12 -18 -4 102.49 8.31 -12 -18 -4 85.57 9.29 -12 -18 -2 16.68 2.91 -12 -18 -2 16.52 4.50 -12 -18 0 33.43 2.82 -12 -18 0 33.79 6.25 -12 -18 2 3.42 2.81 -12 18 2 3.86 1.32 -12 -18 4 104.19 11.24 12 -18 4 87.96 6.12 -12 18 4 100.25 6.56 -12 -18 4 104.36 12.46 -12 -18 6 49.63 9.20 12 -18 6 40.32 6.48 -12 -18 6 44.35 9.95 -12 18 6 27.93 4.20 -12 -18 8 108.30 14.81 -12 18 8 111.76 13.20 12 -18 8 111.10 14.12 -12 -18 8 97.06 15.68 12 18 8 122.35 8.27 -12 -18 10 9.21 8.22 -12 18 10 21.23 7.46 12 -18 10 21.97 9.24 12 -18 12 88.63 17.92 -12 18 12 92.46 16.30 -12 -18 12 104.52 20.69 -12 -18 14 12.47 10.44 -12 18 14 14.08 10.64 12 -18 14 25.95 13.74 -12 -18 16 25.23 17.48 -12 18 16 29.65 14.91 12 -18 16 52.79 19.67 -12 18 18 19.87 16.78 12 -18 18 17.13 16.44 -12 -20 -16 347.04 41.39 12 -20 -16 321.13 32.36 -12 -20 -14 19.49 12.47 12 -20 -14 13.19 8.40 12 -20 -12 582.53 33.84 -12 -20 -12 694.94 50.92 -12 -20 -10 20.52 11.04 12 -20 -10 12.84 5.62 12 -20 -8 1038.05 38.43 -12 -20 -8 1016.42 49.98 12 -20 -6 71.59 7.94 -12 -20 -6 83.22 11.03 -12 -20 -4 460.40 22.99 -12 -20 -4 439.35 20.29 12 -20 -4 434.98 19.40 -12 -20 -2 67.29 8.50 -12 -20 -2 60.06 5.39 -12 -20 0 638.61 29.10 -12 20 0 649.40 19.25 -12 -20 0 704.81 19.19 -12 20 2 55.23 4.62 -12 -20 2 55.53 8.52 -12 -20 4 361.40 23.83 -12 20 4 404.97 15.24 12 -20 4 378.19 14.28 -12 20 6 86.38 7.46 -12 -20 6 99.58 13.32 12 -20 6 81.83 8.74 -12 -20 6 72.14 11.85 -12 -20 8 904.36 48.61 -12 20 8 924.69 32.08 12 20 8 850.82 27.57 -12 -20 8 870.09 44.21 12 -20 8 925.85 40.79 -12 20 10 0.13 3.43 -12 -20 10 1.87 6.61 12 -20 10 16.55 7.57 -12 -20 12 778.37 55.33 -12 20 12 639.90 42.49 12 -20 12 747.35 48.64 -12 -20 14 2.30 10.29 -12 20 14 9.74 9.57 12 -20 14 19.84 13.71 -12 20 16 352.05 39.31 12 -20 16 384.41 43.50 -12 -20 16 448.82 50.47 -12 20 18 5.69 12.51 12 -20 18 28.69 19.51 -12 -22 -16 1.80 12.14 12 -22 -16 -9.74 10.05 -12 -22 -14 309.38 37.35 12 -22 -14 280.61 26.69 12 -22 -12 54.21 10.31 -12 -22 -12 37.69 14.79 12 -22 -10 379.96 24.09 -12 -22 -10 420.69 36.11 12 -22 -8 10.31 4.22 -12 -22 -8 19.16 8.14 12 -22 -6 391.03 20.11 -12 -22 -6 399.17 24.47 -12 -22 -4 111.01 11.42 12 -22 -4 101.81 9.06 -12 -22 -4 96.58 9.36 -12 -22 -2 318.83 19.17 12 -22 -2 285.32 15.15 -12 -22 -2 309.04 13.44 -12 -22 0 13.68 4.67 -12 -22 0 17.44 2.49 -12 22 0 11.61 2.38 -12 -22 2 200.65 16.63 -12 22 2 235.49 11.14 -12 -22 4 112.89 13.42 12 -22 4 116.95 7.22 -12 22 4 99.62 7.30 12 -22 6 407.11 19.37 -12 -22 6 373.00 27.49 -12 22 6 386.94 17.42 -12 -22 6 430.76 29.29 12 -22 8 15.74 6.14 -12 -22 8 15.78 9.48 -12 22 10 380.01 27.85 -12 -22 10 458.11 37.57 12 -22 10 460.33 31.48 -12 22 12 43.75 11.40 -12 -22 12 52.66 15.37 12 -22 12 29.86 11.34 -12 -22 14 353.95 40.02 -12 22 14 313.83 32.00 12 -22 14 327.58 34.55 -12 -22 16 3.87 10.61 -12 22 16 10.62 10.65 12 -22 16 19.41 14.30 -12 22 18 177.64 30.80 -12 -24 -16 35.52 17.76 -12 -24 -14 65.05 19.42 12 -24 -14 21.98 8.55 -12 -24 -12 84.76 19.31 12 -24 -12 84.32 13.14 -12 -24 -10 23.39 10.36 12 -24 -10 44.23 8.59 12 -24 -8 103.77 11.21 -12 -24 -8 109.05 16.42 12 -24 -6 43.64 6.86 -12 -24 -6 29.73 6.20 -12 -24 -4 169.87 14.26 12 -24 -4 171.47 12.41 -12 -24 -4 166.87 12.29 -12 -24 -2 70.49 9.23 -12 -24 -2 64.31 6.08 12 -24 -2 60.17 6.86 -12 -24 0 386.03 11.94 -12 -24 0 402.78 22.06 -12 -24 2 52.01 8.36 -12 24 2 38.75 5.02 12 -24 4 181.72 9.50 -12 -24 4 206.13 18.33 -12 24 4 185.12 11.02 12 -24 6 51.30 6.43 -12 -24 6 44.37 9.47 12 -24 8 123.75 12.98 -12 -24 8 102.90 15.94 12 -24 10 29.94 8.88 -12 24 10 28.18 7.96 -12 -24 10 21.67 8.94 12 -24 12 76.94 14.85 -12 24 12 67.09 13.53 -12 -24 12 75.78 17.81 -12 24 14 28.02 11.65 -12 -24 14 19.87 14.01 -12 -24 16 35.39 15.88 -12 24 16 8.52 10.03 -12 -26 -14 230.25 33.88 12 -26 -14 258.90 26.32 -12 -26 -12 9.57 8.52 12 -26 -12 11.48 7.50 -12 -26 -10 314.91 31.71 12 -26 -10 324.84 23.47 12 -26 -8 10.27 3.99 -12 -26 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11.26 -12 -28 14 16.47 13.33 12 -30 -12 16.79 8.89 12 -30 -10 174.81 17.90 12 -30 -8 30.14 7.09 12 -30 -6 294.22 19.65 -12 -30 -6 289.43 22.32 12 -30 -4 15.33 4.30 -12 -30 -4 14.45 5.09 -12 -30 -2 241.78 19.11 12 -30 -2 243.26 16.20 -12 -30 -2 238.11 14.22 -12 -30 0 71.27 10.48 -12 -30 0 59.67 6.08 -12 -30 2 197.19 10.65 -12 -30 2 190.26 17.70 -12 -30 4 9.26 4.99 -12 -30 6 306.25 25.92 -12 -30 8 38.47 10.98 -12 -30 10 155.32 21.86 -12 -30 12 5.49 7.97 12 -32 -10 21.41 8.36 12 -32 -8 280.82 21.50 12 -32 -6 11.62 4.39 12 -32 -4 303.91 19.70 -12 -32 -2 7.13 5.47 12 -32 -2 5.41 3.72 -12 -32 0 436.60 27.67 12 -32 0 470.61 23.61 -12 -32 2 5.37 4.19 -12 -32 4 301.94 25.06 -12 -32 6 17.64 8.58 -12 -32 8 293.31 27.65 -12 -32 10 0.43 5.34 -12 -32 12 193.11 26.89 12 -34 -8 7.43 3.88 12 -34 -6 59.96 10.19 12 -34 -4 4.16 3.49 12 -34 -2 24.79 5.86 -12 -34 -2 19.68 7.38 -12 -34 0 4.44 5.08 12 -34 0 -0.26 2.51 -12 -34 2 20.40 6.69 -12 -34 4 5.00 5.59 -12 -34 6 55.48 12.25 -12 -34 8 9.85 8.28 -12 -34 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205.35 20.27 -41 -11 3 178.38 19.51 -41 -11 5 132.58 18.14 -41 -11 7 252.84 26.58 -41 -11 9 120.39 20.88 41 -13 -9 1.94 4.30 41 -13 -7 0.06 3.44 41 -13 -5 11.92 4.90 -41 -13 -3 10.31 4.69 41 -13 -3 16.46 4.90 41 -13 -1 6.87 3.69 -41 -13 -1 10.19 5.61 -41 -13 1 1.39 4.14 -41 -13 3 8.73 5.78 -41 -13 5 27.59 9.97 -41 -13 7 6.81 7.06 -41 -13 9 19.23 11.07 41 -15 -9 181.15 18.41 41 -15 -7 98.49 12.49 41 -15 -5 163.28 14.96 -41 -15 -3 93.50 13.47 41 -15 -3 99.40 11.20 -41 -15 -1 377.73 28.18 41 -15 -1 359.64 20.72 -41 -15 1 311.53 26.71 -41 -15 3 131.50 18.05 -41 -15 5 175.00 22.03 -41 -15 7 106.26 18.76 41 -17 -7 57.35 9.90 41 -17 -5 70.93 10.02 -41 -17 -3 89.65 13.86 41 -17 -3 128.58 12.82 41 -17 -1 104.28 11.21 -41 -17 -1 113.39 16.40 -41 -17 1 95.40 15.53 -41 -17 3 98.27 15.73 -41 -17 5 101.28 17.66 41 -19 -5 0.65 3.12 -41 -19 -3 43.31 10.60 41 -19 -3 31.47 6.60 41 -19 -1 74.50 9.67 -41 -19 -1 91.31 15.04 41 -19 1 103.14 11.28 -41 -19 1 106.76 16.77 -41 -19 3 50.64 12.18 41 -21 -3 103.28 12.30 41 -21 -1 171.24 15.18 41 -21 1 144.89 13.77 -42 0 0 -0.12 2.91 -42 0 2 124.37 13.34 -42 0 4 7.34 5.40 -42 0 6 157.23 17.26 -42 0 8 9.17 7.61 -42 0 10 46.75 11.97 -42 0 12 -6.03 7.89 42 -2 -6 216.93 16.34 42 -2 -4 32.91 6.17 -42 -2 -2 344.34 21.79 42 -2 -2 303.82 16.25 42 -2 0 55.86 6.34 -42 2 0 53.35 8.36 -42 -2 0 67.80 10.13 42 -2 2 272.34 14.47 -42 -2 2 296.46 21.72 -42 2 2 288.96 19.50 -42 -2 4 50.28 9.97 -42 2 4 42.36 8.55 -42 -2 6 305.44 25.06 -42 2 6 288.95 22.71 -42 2 8 37.44 9.54 -42 -2 8 59.52 12.63 -42 2 10 182.31 21.91 -42 -2 10 149.03 21.42 -42 -2 12 -2.74 8.65 42 -4 -8 124.91 14.00 42 -4 -6 93.20 10.49 42 -4 -4 63.71 8.12 -42 -4 -2 59.90 9.46 42 -4 -2 60.14 7.20 -42 4 0 71.33 8.69 -42 -4 0 73.96 10.76 42 -4 0 73.63 7.67 -42 -4 2 26.22 7.28 -42 4 2 40.90 7.29 -42 -4 4 97.92 14.16 -42 4 4 64.79 9.45 -42 -4 6 112.36 15.85 -42 4 6 87.63 12.13 -42 -4 8 115.78 17.61 -42 -4 10 57.09 15.07 -42 -4 12 42.52 13.89 42 -6 -10 23.55 7.55 42 -6 -8 34.88 7.82 42 -6 -6 62.07 9.00 42 -6 -4 51.90 7.42 42 -6 -2 23.94 4.84 -42 -6 -2 39.95 8.18 -42 -6 0 24.90 7.31 42 -6 0 20.49 4.65 -42 -6 2 42.42 8.72 -42 -6 4 58.95 11.70 -42 -6 6 79.00 13.72 -42 -6 8 43.32 11.78 -42 -6 10 4.71 6.43 42 -8 -12 103.25 15.87 42 -8 -10 6.56 4.82 42 -8 -8 319.91 22.51 42 -8 -6 15.38 5.21 42 -8 -4 267.94 17.22 42 -8 -2 12.97 3.98 -42 -8 -2 11.81 5.20 -42 -8 0 617.57 34.05 42 -8 0 537.89 24.11 -42 -8 2 14.08 6.33 -42 -8 4 341.27 27.43 -42 -8 6 5.40 7.23 -42 -8 8 374.18 33.28 -42 -8 10 -5.43 7.47 42 -10 -10 4.27 4.67 42 -10 -8 90.27 12.01 42 -10 -6 18.50 5.36 42 -10 -4 51.60 7.64 42 -10 -2 29.36 5.88 -42 -10 -2 22.07 7.87 -42 -10 0 107.66 14.44 42 -10 0 98.18 9.70 -42 -10 2 33.62 8.99 -42 -10 4 55.35 12.10 -42 -10 6 7.87 7.08 -42 -10 8 86.62 16.12 -42 -10 10 21.34 10.17 42 -12 -10 15.01 7.32 42 -12 -8 195.83 17.96 42 -12 -6 7.70 4.17 42 -12 -4 107.69 11.33 42 -12 -2 22.84 5.39 -42 -12 -2 35.41 8.67 -42 -12 0 260.89 23.36 42 -12 0 267.59 16.91 -42 -12 2 26.39 8.43 -42 -12 4 131.33 18.01 -42 -12 6 13.32 7.74 -42 -12 8 213.18 26.23 42 -14 -8 7.25 5.27 42 -14 -6 188.96 16.48 42 -14 -4 20.85 5.56 -42 -14 -2 342.89 26.58 42 -14 -2 281.02 18.51 -42 -14 0 60.93 12.26 42 -14 0 55.12 7.87 -42 -14 2 319.63 27.45 -42 -14 4 44.75 11.93 -42 -14 6 255.95 27.51 42 -16 -8 46.25 9.63 42 -16 -6 35.04 7.49 42 -16 -4 4.18 3.01 -42 -16 -4 13.89 6.05 42 -16 -2 45.04 7.86 -42 -16 -2 55.58 12.11 -42 -16 0 70.32 13.30 42 -16 0 63.90 8.81 -42 -16 2 40.44 11.33 -42 -16 4 0.56 6.06 -42 -16 6 54.43 14.29 42 -18 -6 219.82 18.71 -42 -18 -4 25.38 8.90 42 -18 -4 30.44 6.81 -42 -18 -2 303.70 26.52 42 -18 -2 308.23 20.47 -42 -18 0 30.85 9.55 42 -18 0 20.60 5.83 -42 -18 2 368.69 31.71 -42 -18 4 42.64 12.85 42 -20 -2 47.55 8.40 42 -20 0 5.69 3.97 -43 1 -1 86.81 10.34 -43 -1 -1 66.78 9.99 -43 -1 1 58.64 9.47 -43 1 1 50.24 8.32 -43 -1 3 97.32 12.43 -43 1 3 94.47 11.95 -43 -1 5 67.13 11.21 -43 1 5 65.49 11.02 -43 -1 7 73.55 13.21 -43 1 7 72.89 12.22 -43 1 9 35.64 11.31 -43 -1 9 52.91 12.59 -43 1 11 34.63 12.29 -43 -1 11 15.66 10.24 43 -3 -5 89.43 10.12 43 -3 -3 158.13 12.01 43 -3 -1 57.02 6.95 -43 -3 -1 69.48 10.50 43 -3 1 74.11 7.43 -43 -3 1 78.38 11.46 -43 3 1 78.68 9.72 -43 -3 3 126.23 15.15 -43 3 3 125.89 13.00 -43 -3 5 101.72 14.60 -43 3 5 100.66 12.52 -43 -3 7 106.36 16.39 -43 -3 9 98.44 17.39 -43 -3 11 65.76 16.10 43 -5 -7 99.83 11.72 43 -5 -5 105.18 10.80 43 -5 -3 53.17 7.36 43 -5 -1 170.33 12.25 -43 -5 -1 177.97 17.04 43 -5 1 152.61 11.26 -43 -5 1 158.83 16.27 -43 -5 3 64.60 11.33 -43 -5 5 142.29 17.58 -43 -5 7 140.25 18.93 -43 -5 9 80.52 16.03 -43 -5 11 38.45 14.26 43 -7 -11 43.15 10.64 43 -7 -9 54.65 10.44 43 -7 -7 45.82 8.22 43 -7 -5 64.43 8.55 43 -7 -3 72.91 8.78 -43 -7 -3 83.07 11.45 -43 -7 -1 67.18 10.89 43 -7 -1 62.43 7.61 43 -7 1 89.48 8.95 -43 -7 1 93.71 12.94 -43 -7 3 73.90 12.42 -43 -7 5 83.87 13.89 -43 -7 7 33.02 11.15 -43 -7 9 56.01 14.87 43 -9 -11 40.64 10.81 43 -9 -9 75.94 12.01 43 -9 -7 181.09 16.18 43 -9 -5 26.10 5.99 43 -9 -3 45.51 7.01 -43 -9 -3 47.48 9.38 43 -9 -1 100.96 10.34 -43 -9 -1 127.08 15.52 43 -9 1 98.64 9.65 -43 -9 1 98.15 14.01 -43 -9 3 29.84 9.02 -43 -9 5 29.98 9.52 -43 -9 7 183.66 22.46 -43 -9 9 63.03 15.47 43 -11 -9 114.67 14.53 43 -11 -7 86.61 11.76 43 -11 -5 125.68 12.78 -43 -11 -3 136.49 15.80 43 -11 -3 119.15 11.60 43 -11 -1 137.08 12.19 -43 -11 -1 176.27 18.48 43 -11 1 165.57 13.04 -43 -11 1 177.29 19.09 -43 -11 3 106.88 15.84 -43 -11 5 160.33 20.34 -43 -11 7 103.10 18.16 -43 -11 9 156.40 23.67 43 -13 -9 36.62 9.20 43 -13 -7 75.23 11.00 43 -13 -5 48.05 8.34 43 -13 -3 132.28 12.56 -43 -13 -3 114.61 15.16 43 -13 -1 129.98 11.99 -43 -13 -1 142.04 17.48 43 -13 1 155.75 13.06 -43 -13 1 150.96 18.81 -43 -13 3 153.42 19.28 -43 -13 5 61.74 13.24 -43 -13 7 64.65 14.32 43 -15 -7 90.59 12.37 43 -15 -5 57.08 9.00 -43 -15 -3 98.32 14.42 43 -15 -3 77.34 10.05 43 -15 -1 158.08 13.91 -43 -15 -1 175.27 19.62 43 -15 1 157.06 13.50 -43 -15 1 152.29 19.09 -43 -15 3 80.41 14.80 -43 -15 5 124.85 18.49 43 -17 -5 75.35 10.84 -43 -17 -3 22.07 8.24 43 -17 -3 23.41 6.06 -43 -17 -1 54.57 12.76 43 -17 -1 47.55 8.28 43 -17 1 49.54 8.19 -43 -17 1 50.83 12.06 -43 -17 3 30.40 10.59 43 -19 -3 86.60 11.12 43 -19 -1 70.01 9.96 43 -19 1 59.61 9.06 -44 0 0 238.72 18.15 -44 0 2 -0.41 2.87 -44 0 4 270.55 21.59 -44 0 6 7.16 5.40 -44 0 8 311.61 27.29 -44 0 10 2.63 7.32 -44 -2 0 70.41 10.20 -44 2 0 73.48 9.76 -44 -2 2 81.11 11.93 -44 2 2 93.90 11.60 -44 2 4 26.64 7.05 -44 -2 4 20.22 7.48 -44 -2 6 23.30 8.35 -44 -2 8 52.49 11.92 -44 -2 10 11.71 7.98 44 -4 -2 34.14 5.69 -44 -4 -2 34.79 7.81 44 -4 0 133.23 10.65 -44 -4 0 144.53 15.40 -44 -4 2 46.34 9.48 44 -4 2 41.28 5.82 -44 -4 4 78.98 12.28 -44 -4 6 45.92 10.94 -44 -4 8 67.03 13.72 -44 -4 10 41.02 12.79 44 -6 -6 147.18 13.86 44 -6 -4 19.25 5.09 44 -6 -2 159.33 12.60 -44 -6 -2 194.54 17.69 44 -6 0 16.41 4.25 -44 -6 0 21.05 6.56 44 -6 2 129.13 10.64 -44 -6 2 132.52 15.85 -44 -6 4 8.47 5.88 -44 -6 6 173.28 20.44 -44 -6 8 42.65 12.54 -44 -6 10 203.47 26.05 44 -8 -10 41.40 9.85 44 -8 -8 8.45 4.56 44 -8 -6 81.29 10.76 44 -8 -4 4.49 3.12 -44 -8 -2 137.71 15.46 44 -8 -2 106.10 10.37 -44 -8 0 15.55 6.69 44 -8 0 19.57 4.60 -44 -8 2 130.76 16.06 -44 -8 4 -6.83 6.43 -44 -8 6 122.61 17.56 -44 -8 8 18.66 9.51 44 -10 -10 102.85 15.28 44 -10 -8 6.49 5.70 44 -10 -6 201.83 16.93 44 -10 -4 10.83 3.99 -44 -10 -2 339.51 25.18 44 -10 -2 295.09 18.49 -44 -10 0 8.69 6.54 44 -10 0 21.46 4.89 -44 -10 2 340.82 27.41 -44 -10 4 15.64 7.18 -44 -10 6 244.28 26.10 -44 -10 8 13.11 9.20 44 -12 -8 102.20 13.53 44 -12 -6 57.50 9.25 44 -12 -4 107.93 11.56 44 -12 -2 57.58 8.15 -44 -12 -2 76.79 12.49 -44 -12 0 35.48 9.25 44 -12 0 55.38 8.20 -44 -12 2 63.81 12.69 -44 -12 4 114.13 16.95 -44 -12 6 58.55 13.56 44 -14 -8 72.96 11.49 44 -14 -6 69.05 10.37 44 -14 -4 28.53 6.78 44 -14 -2 51.25 8.24 -44 -14 -2 47.45 11.45 -44 -14 0 96.02 15.12 44 -14 0 78.49 10.01 -44 -14 2 44.95 11.32 -44 -14 4 31.68 9.50 44 -16 -6 21.40 6.68 44 -16 -4 240.35 18.66 44 -16 -2 38.28 7.56 -44 -16 -2 52.40 11.56 -44 -16 0 529.81 36.16 44 -16 0 534.79 27.04 -44 -16 2 55.55 12.78 44 -18 -2 6.88 4.93 44 -18 0 106.83 12.06 -45 -1 -1 25.94 6.67 -45 -1 1 31.48 7.24 -45 1 1 33.84 7.18 -45 -1 3 5.52 5.26 -45 1 3 12.89 5.91 -45 -1 5 58.56 10.93 -45 -1 7 56.98 12.11 -45 -1 9 32.42 10.92 -45 -3 -1 253.08 20.09 -45 -3 1 264.40 21.00 -45 -3 3 145.63 16.57 -45 -3 5 134.78 16.90 -45 -3 7 205.78 22.10 -45 -3 9 85.16 16.02 -45 -5 -1 19.65 6.47 -45 -5 1 29.76 8.21 -45 -5 3 16.60 6.75 -45 -5 5 33.41 9.70 -45 -5 7 31.85 10.27 -45 -5 9 12.16 8.19 45 -7 -5 86.02 10.92 45 -7 -3 82.96 9.51 45 -7 -1 91.11 9.54 -45 -7 -1 101.05 13.45 45 -7 1 87.25 9.14 -45 -7 1 78.18 12.50 -45 -7 3 78.10 13.32 -45 -7 5 100.82 15.62 -45 -7 7 80.65 15.59 -45 -7 9 110.08 19.23 45 -9 -9 73.24 12.06 45 -9 -7 97.25 12.65 45 -9 -5 68.89 9.83 45 -9 -3 140.93 12.88 -45 -9 -3 138.20 15.85 -45 -9 -1 87.25 13.60 45 -9 -1 77.94 9.21 45 -9 1 88.86 9.46 -45 -9 1 87.12 13.50 -45 -9 3 110.87 15.63 -45 -9 5 94.84 15.96 -45 -9 7 82.91 16.15 45 -11 -9 7.42 5.37 45 -11 -7 27.30 7.32 45 -11 -5 40.25 7.94 -45 -11 -3 16.04 6.45 45 -11 -3 17.75 5.17 -45 -11 -1 86.46 13.45 45 -11 -1 74.47 9.12 45 -11 1 81.74 9.51 -45 -11 1 90.32 13.90 -45 -11 3 11.50 6.79 -45 -11 5 48.26 12.54 -45 -11 7 41.24 12.48 45 -13 -7 129.42 14.84 45 -13 -5 160.68 15.05 -45 -13 -3 280.43 23.73 45 -13 -3 201.74 16.21 45 -13 -1 173.91 14.77 -45 -13 -1 186.85 20.14 -45 -13 1 202.38 21.64 45 -13 1 168.79 13.80 -45 -13 3 275.30 26.38 -45 -13 5 181.01 22.89 45 -15 -5 31.03 7.39 45 -15 -3 7.71 4.53 -45 -15 -3 10.70 6.20 -45 -15 -1 74.33 13.77 45 -15 -1 63.64 9.24 45 -15 1 64.30 9.08 -45 -15 1 59.10 12.90 -45 -15 3 11.70 7.91 45 -17 -3 99.47 11.99 45 -17 -1 78.19 10.55 45 -17 1 90.16 11.02 -46 -2 0 80.18 11.58 -46 -2 2 11.17 5.72 -46 -2 4 49.69 9.83 -46 -2 6 13.30 7.50 -46 -2 8 68.14 14.26 -46 -4 0 8.53 5.94 -46 -4 2 121.74 14.89 -46 -4 4 1.18 4.36 -46 -4 6 126.65 17.28 -46 -4 8 18.82 9.01 -46 -6 -2 10.06 5.63 -46 -6 0 391.32 27.12 -46 -6 2 16.41 7.46 -46 -6 4 291.93 25.47 -46 -6 6 22.74 8.79 -46 -6 8 230.70 26.40 46 -8 -4 6.73 3.52 -46 -8 -2 8.30 5.61 46 -8 -2 4.60 3.13 46 -8 0 27.43 6.04 -46 -8 0 39.28 9.52 46 -8 2 4.64 3.11 -46 -8 2 5.55 5.90 -46 -8 4 7.03 4.82 -46 -8 6 11.85 8.61 -46 -8 8 14.88 9.93 46 -10 -6 2.01 3.52 46 -10 -4 216.10 16.66 -46 -10 -2 4.13 4.15 46 -10 -2 6.77 3.41 46 -10 0 416.60 22.26 -46 -10 0 482.66 32.12 46 -10 2 5.40 3.60 -46 -10 2 15.83 7.92 -46 -10 4 242.62 24.43 -46 -10 6 13.06 8.67 46 -12 -6 65.88 10.37 46 -12 -4 5.12 3.66 -46 -12 -2 151.10 17.51 46 -12 -2 163.69 14.13 46 -12 0 4.66 3.41 -46 -12 0 -0.97 4.29 46 -12 2 167.05 13.90 -46 -12 2 183.41 20.68 -46 -12 4 -2.05 5.59 46 -14 -6 15.92 5.95 46 -14 -4 77.69 10.57 -46 -14 -2 26.49 9.03 46 -14 -2 11.52 4.74 46 -14 0 143.70 13.29 -46 -14 0 156.50 19.46 46 -14 2 14.48 4.70 -46 -14 2 13.59 8.07 46 -16 -2 216.01 17.60 46 -16 0 18.39 5.43 46 -16 2 224.17 17.16 -47 -3 -1 157.79 15.98 -47 -3 1 123.96 14.92 -47 -3 3 157.08 17.49 -47 -3 5 166.05 19.00 -47 -3 7 105.88 16.46 -47 -5 -1 9.24 5.01 -47 -5 1 15.56 6.30 -47 -5 3 5.20 5.76 -47 -5 5 13.49 7.97 -47 -5 7 11.71 9.05 -47 -7 -1 86.23 12.88 -47 -7 1 106.89 14.77 -47 -7 3 93.44 14.58 -47 -7 5 54.56 11.90 -47 -7 7 99.80 17.48 47 -9 -1 103.39 10.81 -47 -9 -1 129.64 16.08 -47 -9 1 139.44 17.64 47 -9 1 114.33 11.02 -47 -9 3 64.25 12.52 -47 -9 5 46.41 12.29 47 -11 -5 42.66 8.55 47 -11 -3 17.28 5.60 47 -11 -1 55.45 8.47 -47 -11 -1 76.26 13.80 -47 -11 1 54.44 12.27 47 -11 1 51.60 7.62 -47 -11 3 40.85 11.14 -47 -11 5 34.35 10.71 47 -13 -5 70.81 10.47 47 -13 -3 132.28 13.45 -47 -13 -1 156.02 19.45 47 -13 -1 162.53 14.53 -47 -13 1 182.45 21.17 47 -13 1 195.61 15.39 47 -15 -3 37.71 7.82 47 -15 -1 10.43 4.71 47 -15 1 25.21 6.25 -48 -4 0 115.86 14.39 -48 -4 2 45.66 9.84 -48 -4 4 98.23 14.76 -48 -4 6 65.80 13.12 -48 -6 0 6.53 5.84 -48 -6 2 181.55 19.55 -48 -6 4 7.72 6.22 -48 -6 6 115.87 17.33 -48 -8 -2 57.94 10.73 -48 -8 0 26.67 8.52 -48 -8 2 62.27 12.71 -48 -8 4 5.32 6.26 -48 -8 6 58.14 13.58 -48 -10 -2 201.82 20.67 -48 -10 0 -3.22 4.08 -48 -10 2 195.62 21.33 -48 -10 4 -2.53 6.29 48 -12 -4 22.78 6.85 48 -12 -2 62.05 9.20 -48 -12 -2 56.54 11.82 -48 -12 0 88.98 14.87 48 -12 0 59.83 9.12 48 -12 2 57.23 8.51 48 -14 -2 72.05 10.20 48 -14 0 72.25 9.98 48 -14 2 71.37 9.71 -49 -5 -1 42.64 9.77 -49 -5 1 35.93 9.62 -49 -5 3 48.34 11.40 -49 -5 5 63.00 13.29 -49 -7 -1 85.79 13.21 -49 -7 1 96.92 14.33 -49 -7 3 70.74 13.18 -49 -7 5 80.79 14.91 -49 -9 -1 44.03 10.42 -49 -9 1 49.50 11.32 -49 -9 3 68.45 14.16 -50 -6 0 52.79 11.12 -50 -6 2 35.47 9.34 -50 -8 0 175.76 19.78 -50 -8 2 8.32 6.53 0 0 0 0.00 0.00 TITL TBA2 WS4 in Fdd2 REM Fdd2 (#43, found as F2dd in -cba setting) CELL 0.71073 35.558248 28.721640 15.565803 90.0000 90.0000 90.0000 ZERR 23.00 0.000623 0.000507 0.000373 0.0000 0.0000 0.0000 LATT -4 SYMM -x,-y, z SYMM x+1/4,-y+1/4, z+1/4 SYMM -x+1/4, y+1/4, z+1/4 SFAC C H N S W UNIT 736.00 1656.00 46.00 92.00 23.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 60437 _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 2.851 _oxdiff_exptl_absorpt_empirical_full_min 0.327 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' 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 W1 W 0.70642(2) 0.40360(2) 0.65155(3) 0.01593(10) Uani 1 1 d . . . . . S1 S 0.70260(7) 0.47833(8) 0.68158(17) 0.0215(5) Uani 1 1 d . . . . . S2 S 0.73209(6) 0.39367(8) 0.52492(16) 0.0195(4) Uani 1 1 d . . . . . S4 S 0.74117(8) 0.36808(8) 0.74775(18) 0.0291(6) Uani 1 1 d . . . . . S3 S 0.65054(7) 0.37226(11) 0.6487(3) 0.0392(7) Uani 1 1 d . . . . . N1 N 0.70538(19) 0.5328(2) 0.4141(5) 0.0159(15) Uani 1 1 d . . . . . C25 C 0.7402(2) 0.5106(3) 0.4551(6) 0.0182(17) Uani 1 1 d . . . . . H25A H 0.737547 0.512258 0.518358 0.022 Uiso 1 1 calc R U . . . H25B H 0.740809 0.477208 0.439079 0.022 Uiso 1 1 calc R U . . . C23 C 0.6013(3) 0.5031(4) 0.4644(7) 0.026(2) Uani 1 1 d . . . . . H23A H 0.602488 0.509929 0.526696 0.031 Uiso 1 1 calc R U . . . H23B H 0.603747 0.469047 0.456835 0.031 Uiso 1 1 calc R U . . . N2 N 0.67395(19) 0.2196(2) 0.5528(6) 0.0185(15) Uani 1 1 d . . . . . C2 C 0.6720(3) 0.1376(3) 0.6174(8) 0.032(2) Uani 1 1 d . . . . . H2A H 0.684762 0.149298 0.669705 0.039 Uiso 1 1 calc R U . . . H2B H 0.691380 0.124857 0.578153 0.039 Uiso 1 1 calc R U . . . C29 C 0.7056(2) 0.5849(3) 0.4257(7) 0.0185(18) Uani 1 1 d . . . . . H29A H 0.683322 0.598036 0.396239 0.022 Uiso 1 1 calc R U . . . H29B H 0.728231 0.597688 0.397092 0.022 Uiso 1 1 calc R U . . . C26 C 0.7773(2) 0.5324(3) 0.4302(7) 0.0222(19) Uani 1 1 d . . . . . H26A H 0.779814 0.563229 0.458145 0.027 Uiso 1 1 calc R U . . . H26B H 0.778141 0.537113 0.367188 0.027 Uiso 1 1 calc R U . . . C17 C 0.7054(2) 0.5239(3) 0.3173(6) 0.0178(17) Uani 1 1 d . . . . . H17A H 0.684074 0.541235 0.291616 0.021 Uiso 1 1 calc R U . . . H17B H 0.728818 0.536973 0.292900 0.021 Uiso 1 1 calc R U . . . C3 C 0.6436(3) 0.0992(3) 0.6416(10) 0.034(3) Uani 1 1 d . . . . . H3A H 0.627694 0.092410 0.590909 0.040 Uiso 1 1 calc R U . . . H3B H 0.657576 0.070479 0.656104 0.040 Uiso 1 1 calc R U . . . C9 C 0.6467(2) 0.2544(3) 0.5140(7) 0.0191(18) Uani 1 1 d . . . . . H9A H 0.630707 0.266751 0.560820 0.023 Uiso 1 1 calc R U . . . H9B H 0.629934 0.237369 0.473946 0.023 Uiso 1 1 calc R U . . . C1 C 0.6507(2) 0.1768(3) 0.5737(7) 0.0198(18) Uani 1 1 d . . . . . H1A H 0.639753 0.164748 0.519702 0.024 Uiso 1 1 calc R U . . . H1B H 0.629663 0.186342 0.611368 0.024 Uiso 1 1 calc R U . . . C12 C 0.6454(3) 0.3677(4) 0.3826(8) 0.033(3) Uani 1 1 d . . . . . H12A H 0.660865 0.356556 0.334736 0.049 Uiso 1 1 calc R U . . . H12B H 0.660502 0.387701 0.419981 0.049 Uiso 1 1 calc R U . . . H12C H 0.624003 0.385450 0.359971 0.049 Uiso 1 1 calc R U . . . C18 C 0.7024(3) 0.4735(3) 0.2900(7) 0.030(2) Uani 1 1 d . . . . . H18A H 0.681119 0.458458 0.320322 0.036 Uiso 1 1 calc R U . . . H18B H 0.725739 0.456741 0.305646 0.036 Uiso 1 1 calc R U . . . C13 C 0.6933(3) 0.2398(3) 0.6327(7) 0.025(2) Uani 1 1 d . . . . . H13A H 0.714935 0.219553 0.647317 0.030 Uiso 1 1 calc R U . . . H13B H 0.703470 0.270808 0.617764 0.030 Uiso 1 1 calc R U . . . C21 C 0.6714(3) 0.5107(3) 0.4566(7) 0.0203(18) Uani 1 1 d . . . . . H21A H 0.671995 0.517901 0.518785 0.024 Uiso 1 1 calc R U . . . H21B H 0.673128 0.476508 0.450220 0.024 Uiso 1 1 calc R U . . . C10 C 0.6634(3) 0.2955(3) 0.4659(7) 0.0201(18) Uani 1 1 d . . . . . H10A H 0.678562 0.284321 0.416589 0.024 Uiso 1 1 calc R U . . . H10B H 0.680031 0.313602 0.504438 0.024 Uiso 1 1 calc R U . . . C19 C 0.6963(3) 0.4706(3) 0.1939(6) 0.0232(19) Uani 1 1 d . . . . . H19A H 0.717891 0.485161 0.164292 0.028 Uiso 1 1 calc R U . . . H19B H 0.673437 0.488549 0.178742 0.028 Uiso 1 1 calc R U . . . C22 C 0.6336(3) 0.5270(3) 0.4199(7) 0.027(2) Uani 1 1 d . . . . . H22A H 0.631293 0.561139 0.427193 0.033 Uiso 1 1 calc R U . . . H22B H 0.632711 0.520071 0.357594 0.033 Uiso 1 1 calc R U . . . C6 C 0.6934(3) 0.1828(3) 0.4104(8) 0.026(2) Uani 1 1 d . . . . . H6A H 0.672368 0.199973 0.383228 0.031 Uiso 1 1 calc R U . . . H6B H 0.684506 0.151000 0.424190 0.031 Uiso 1 1 calc R U . . . C20 C 0.6918(4) 0.4206(5) 0.1617(10) 0.047(2) Uani 1 1 d . . . . . H20A H 0.691180 0.420451 0.098732 0.071 Uiso 1 1 calc R U . . . H20B H 0.668224 0.407492 0.183869 0.071 Uiso 1 1 calc R U . . . H20C H 0.712979 0.401722 0.181774 0.071 Uiso 1 1 calc R U . . . C32 C 0.7464(4) 0.6731(4) 0.4964(10) 0.042(3) Uani 1 1 d . . . . . H32A H 0.750833 0.666685 0.435438 0.063 Uiso 1 1 calc R U . . . H32B H 0.765741 0.657684 0.531012 0.063 Uiso 1 1 calc R U . . . H32C H 0.747407 0.706788 0.506383 0.063 Uiso 1 1 calc R U . . . C31 C 0.7082(3) 0.6550(4) 0.5217(9) 0.035(3) Uani 1 1 d . . . . . H31A H 0.689060 0.668497 0.482791 0.042 Uiso 1 1 calc R U . . . H31B H 0.702395 0.665556 0.580763 0.042 Uiso 1 1 calc R U . . . C11 C 0.6309(3) 0.3262(3) 0.4339(7) 0.0222(18) Uani 1 1 d . . . . . H11A H 0.613900 0.307353 0.397278 0.027 Uiso 1 1 calc R U . . . H11B H 0.616177 0.337507 0.483688 0.027 Uiso 1 1 calc R U . . . C5 C 0.7052(2) 0.2073(4) 0.4920(8) 0.025(2) Uani 1 1 d . . . . . H5A H 0.723341 0.187205 0.522721 0.030 Uiso 1 1 calc R U . . . H5B H 0.718520 0.236333 0.476077 0.030 Uiso 1 1 calc R U . . . C24 C 0.5635(3) 0.5190(4) 0.4293(10) 0.040(3) Uani 1 1 d . . . . . H24A H 0.561394 0.510012 0.368718 0.061 Uiso 1 1 calc R U . . . H24B H 0.561430 0.552894 0.434363 0.061 Uiso 1 1 calc R U . . . H24C H 0.543209 0.504224 0.462154 0.061 Uiso 1 1 calc R U . . . C7 C 0.7267(3) 0.1801(4) 0.3478(8) 0.033(3) Uani 1 1 d . . . . . H7A H 0.733597 0.211988 0.329522 0.040 Uiso 1 1 calc R U . . . H7B H 0.748634 0.166543 0.378020 0.040 Uiso 1 1 calc R U . . . C14 C 0.6692(3) 0.2449(4) 0.7118(8) 0.032(2) Uani 1 1 d . . . . . H14A H 0.653621 0.216555 0.719202 0.039 Uiso 1 1 calc R U . . . H14B H 0.652014 0.271738 0.704500 0.039 Uiso 1 1 calc R U . . . C28 C 0.8127(3) 0.4561(3) 0.4064(9) 0.028(2) Uani 1 1 d . . . . . H28A H 0.810069 0.463027 0.345033 0.042 Uiso 1 1 calc R U . . . H28B H 0.792701 0.434758 0.424248 0.042 Uiso 1 1 calc R U . . . H28C H 0.837250 0.441555 0.416760 0.042 Uiso 1 1 calc R U . . . C30 C 0.7054(3) 0.6014(3) 0.5182(8) 0.026(2) Uani 1 1 d . . . . . H30A H 0.726822 0.587393 0.549474 0.032 Uiso 1 1 calc R U . . . H30B H 0.681846 0.591104 0.546588 0.032 Uiso 1 1 calc R U . . . C8 C 0.7182(4) 0.1512(4) 0.2694(9) 0.041(3) Uani 1 1 d . . . . . H8A H 0.738924 0.154174 0.228170 0.062 Uiso 1 1 calc R U . . . H8B H 0.694861 0.162205 0.242957 0.062 Uiso 1 1 calc R U . . . H8C H 0.715427 0.118516 0.286135 0.062 Uiso 1 1 calc R U . . . C15 C 0.6932(4) 0.2521(5) 0.7910(9) 0.042(3) Uani 1 1 d . . . . . H15A H 0.713090 0.228003 0.792709 0.051 Uiso 1 1 calc R U . . . H15B H 0.705698 0.282896 0.787270 0.051 Uiso 1 1 calc R U . . . C4 C 0.6183(4) 0.1120(5) 0.7167(11) 0.048(4) Uani 1 1 d . . . . . H4A H 0.600585 0.136256 0.698714 0.072 Uiso 1 1 calc R U . . . H4B H 0.633744 0.123675 0.764238 0.072 Uiso 1 1 calc R U . . . H4C H 0.604384 0.084430 0.735458 0.072 Uiso 1 1 calc R U . . . C27 C 0.8099(3) 0.5010(4) 0.4577(8) 0.028(2) Uani 1 1 d . . . . . H27A H 0.833762 0.518499 0.451554 0.033 Uiso 1 1 calc R U . . . H27B H 0.806858 0.493172 0.519276 0.033 Uiso 1 1 calc R U . . . C16 C 0.6707(4) 0.2498(5) 0.8722(8) 0.047(2) Uani 1 1 d . . . . . H16A H 0.649624 0.271802 0.868683 0.071 Uiso 1 1 calc R U . . . H16B H 0.686703 0.258033 0.921122 0.071 Uiso 1 1 calc R U . . . H16C H 0.660914 0.218209 0.879897 0.071 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 W1 0.01746(15) 0.01706(14) 0.01326(17) -0.00193(14) 0.00022(14) -0.00240(12) S1 0.0275(10) 0.0194(10) 0.0176(11) -0.0019(8) -0.0010(9) 0.0059(8) S2 0.0210(9) 0.0198(9) 0.0177(12) -0.0015(8) 0.0026(9) 0.0020(8) S4 0.0477(14) 0.0198(10) 0.0197(13) 0.0035(9) -0.0090(11) 0.0024(10) S3 0.0260(11) 0.0532(15) 0.0383(17) -0.0248(16) 0.0117(14) -0.0170(11) N1 0.024(3) 0.015(3) 0.009(4) -0.001(3) 0.001(3) 0.000(2) C25 0.020(4) 0.019(4) 0.016(5) -0.005(3) 0.002(3) 0.003(3) C23 0.025(4) 0.029(5) 0.023(6) 0.005(4) 0.004(4) -0.001(4) N2 0.015(3) 0.020(3) 0.021(4) 0.004(3) -0.004(3) 0.001(3) C2 0.030(5) 0.023(4) 0.044(7) 0.009(4) 0.002(5) 0.003(4) C29 0.023(4) 0.014(3) 0.018(5) -0.001(3) 0.004(3) 0.000(3) C26 0.019(4) 0.024(4) 0.024(5) -0.002(4) -0.002(3) -0.001(3) C17 0.023(4) 0.020(4) 0.010(4) 0.003(3) 0.000(3) -0.001(3) C3 0.043(5) 0.024(4) 0.034(8) 0.008(5) 0.013(6) -0.001(4) C9 0.017(4) 0.021(4) 0.019(5) 0.003(3) -0.002(3) 0.002(3) C1 0.017(4) 0.018(4) 0.025(5) 0.002(3) 0.003(3) 0.000(3) C12 0.038(5) 0.024(4) 0.036(8) 0.010(4) -0.013(5) -0.003(4) C18 0.057(7) 0.019(4) 0.013(5) -0.003(4) 0.002(5) 0.005(4) C13 0.026(4) 0.028(4) 0.022(6) 0.002(4) -0.009(4) -0.004(4) C21 0.021(4) 0.021(4) 0.018(5) 0.001(3) 0.000(3) -0.002(3) C10 0.023(4) 0.017(4) 0.021(5) 0.001(3) 0.000(4) 0.001(3) C19 0.033(5) 0.027(4) 0.010(5) -0.004(4) -0.002(4) -0.005(4) C22 0.023(4) 0.034(5) 0.025(7) 0.011(4) 0.003(4) -0.004(4) C6 0.027(4) 0.022(4) 0.029(6) 0.002(4) 0.004(4) 0.005(3) C20 0.069(6) 0.048(5) 0.025(5) -0.003(4) -0.010(5) 0.016(5) C32 0.053(7) 0.028(5) 0.044(8) -0.010(5) 0.003(6) -0.009(5) C31 0.047(7) 0.022(5) 0.035(7) -0.007(5) 0.000(5) 0.009(4) C11 0.029(4) 0.023(4) 0.015(5) 0.001(4) -0.003(4) -0.003(4) C5 0.014(4) 0.026(4) 0.034(6) 0.008(4) 0.001(4) -0.001(3) C24 0.024(5) 0.039(6) 0.059(10) 0.009(6) 0.005(5) -0.004(4) C7 0.027(5) 0.038(5) 0.035(7) 0.013(5) 0.009(5) 0.010(5) C14 0.032(5) 0.041(6) 0.023(6) -0.005(5) -0.010(4) 0.006(5) C28 0.026(4) 0.028(4) 0.031(6) -0.001(5) 0.008(5) 0.007(3) C30 0.036(6) 0.023(4) 0.020(6) -0.002(4) 0.005(4) 0.004(4) C8 0.050(7) 0.040(6) 0.034(8) 0.005(5) 0.015(6) 0.023(6) C15 0.041(6) 0.051(7) 0.035(8) -0.006(6) -0.009(6) -0.023(6) C4 0.059(8) 0.031(5) 0.055(10) 0.008(6) 0.014(7) -0.007(6) C27 0.023(4) 0.037(5) 0.023(6) -0.004(4) -0.003(4) 0.004(4) C16 0.069(6) 0.048(5) 0.025(5) -0.003(4) -0.010(5) 0.016(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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 S2 W1 S1 110.11(9) . . ? S2 W1 S4 108.60(10) . . ? S4 W1 S1 110.08(10) . . ? S3 W1 S1 110.52(10) . . ? S3 W1 S2 107.92(11) . . ? S3 W1 S4 109.56(13) . . ? C29 N1 C25 111.1(7) . . ? C29 N1 C17 106.5(7) . . ? C29 N1 C21 111.5(7) . . ? C17 N1 C25 109.9(7) . . ? C21 N1 C25 106.7(7) . . ? C21 N1 C17 111.1(7) . . ? N1 C25 H25A 108.5 . . ? N1 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? C26 C25 N1 115.1(8) . . ? C26 C25 H25A 108.5 . . ? C26 C25 H25B 108.5 . . ? H23A C23 H23B 107.9 . . ? C22 C23 H23A 109.2 . . ? C22 C23 H23B 109.2 . . ? C22 C23 C24 111.9(9) . . ? C24 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? C9 N2 C13 111.1(7) . . ? C1 N2 C9 105.7(6) . . ? C1 N2 C13 112.0(8) . . ? C5 N2 C9 112.1(8) . . ? C5 N2 C1 110.4(7) . . ? C5 N2 C13 105.5(7) . . ? H2A C2 H2B 108.4 . . ? C3 C2 H2A 110.1 . . ? C3 C2 H2B 110.1 . . ? C1 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? C1 C2 C3 108.2(9) . . ? N1 C29 H29A 108.5 . . ? N1 C29 H29B 108.5 . . ? N1 C29 C30 115.0(8) . . ? H29A C29 H29B 107.5 . . ? C30 C29 H29A 108.5 . . ? C30 C29 H29B 108.5 . . ? C25 C26 H26A 109.6 . . ? C25 C26 H26B 109.6 . . ? C25 C26 C27 110.1(8) . . ? H26A C26 H26B 108.1 . . ? C27 C26 H26A 109.6 . . ? C27 C26 H26B 109.6 . . ? N1 C17 H17A 108.3 . . ? N1 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? C18 C17 N1 115.9(8) . . ? C18 C17 H17A 108.3 . . ? C18 C17 H17B 108.3 . . ? C2 C3 H3A 108.8 . . ? C2 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C4 C3 C2 113.7(10) . . ? C4 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? N2 C9 H9A 108.0 . . ? N2 C9 H9B 108.0 . . ? N2 C9 C10 117.1(7) . . ? H9A C9 H9B 107.3 . . ? C10 C9 H9A 108.0 . . ? C10 C9 H9B 108.0 . . ? N2 C1 C2 115.3(7) . . ? N2 C1 H1A 108.5 . . ? N2 C1 H1B 108.5 . . ? C2 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? C17 C18 H18A 109.7 . . ? C17 C18 H18B 109.7 . . ? C17 C18 C19 109.9(8) . . ? H18A C18 H18B 108.2 . . ? C19 C18 H18A 109.7 . . ? C19 C18 H18B 109.7 . . ? N2 C13 H13A 108.2 . . ? N2 C13 H13B 108.2 . . ? H13A C13 H13B 107.4 . . ? C14 C13 N2 116.3(8) . . ? C14 C13 H13A 108.2 . . ? C14 C13 H13B 108.2 . . ? N1 C21 H21A 108.7 . . ? N1 C21 H21B 108.7 . . ? N1 C21 C22 114.1(8) . . ? H21A C21 H21B 107.6 . . ? C22 C21 H21A 108.7 . . ? C22 C21 H21B 108.7 . . ? C9 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? C9 C10 C11 108.0(7) . . ? H10A C10 H10B 108.4 . . ? C11 C10 H10A 110.1 . . ? C11 C10 H10B 110.1 . . ? C18 C19 H19A 109.0 . . ? C18 C19 H19B 109.0 . . ? C18 C19 C20 113.0(9) . . ? H19A C19 H19B 107.8 . . ? C20 C19 H19A 109.0 . . ? C20 C19 H19B 109.0 . . ? C23 C22 C21 110.9(8) . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.0 . . ? H6A C6 H6B 108.2 . . ? C5 C6 H6A 109.7 . . ? C5 C6 H6B 109.7 . . ? C5 C6 C7 110.0(9) . . ? C7 C6 H6A 109.7 . . ? C7 C6 H6B 109.7 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? C32 C31 H31A 108.9 . . ? C32 C31 H31B 108.9 . . ? C32 C31 C30 113.2(9) . . ? H31A C31 H31B 107.7 . . ? C30 C31 H31A 108.9 . . ? C30 C31 H31B 108.9 . . ? C12 C11 C10 111.3(8) . . ? C12 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C10 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N2 C5 C6 115.7(7) . . ? N2 C5 H5A 108.4 . . ? N2 C5 H5B 108.4 . . ? C6 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? H5A C5 H5B 107.4 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C6 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C8 C7 C6 112.8(10) . . ? C8 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 C15 110.8(10) . . ? H14A C14 H14B 108.1 . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? C29 C30 C31 110.1(10) . . ? C29 C30 H30A 109.6 . . ? C29 C30 H30B 109.6 . . ? C31 C30 H30A 109.6 . . ? C31 C30 H30B 109.6 . . ? H30A C30 H30B 108.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C16 C15 C14 112.2(11) . . ? C16 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C26 C27 H27A 108.8 . . ? C26 C27 H27B 108.8 . . ? C28 C27 C26 113.7(9) . . ? C28 C27 H27A 108.8 . . ? C28 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 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 W1 S1 2.201(2) . ? W1 S2 2.191(2) . ? W1 S4 2.193(3) . ? W1 S3 2.182(2) . ? N1 C25 1.532(11) . ? N1 C29 1.508(11) . ? N1 C17 1.529(12) . ? N1 C21 1.517(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.514(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C22 1.507(13) . ? C23 C24 1.523(15) . ? N2 C9 1.518(11) . ? N2 C1 1.515(11) . ? N2 C13 1.536(13) . ? N2 C5 1.501(13) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.541(14) . ? C2 C1 1.520(13) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C30 1.515(16) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 C27 1.530(13) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.513(13) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.52(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.520(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C12 C11 1.524(14) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 C19 1.514(14) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.507(16) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.532(13) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.539(13) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.530(16) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C5 1.512(17) . ? C6 C7 1.537(15) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C32 C31 1.506(18) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C30 1.545(15) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.51(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C15 1.515(16) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C28 C27 1.521(15) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.50(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 N1 C25 C26 C27 -167.1(8) . . . . ? N1 C29 C30 C31 176.4(8) . . . . ? N1 C17 C18 C19 170.7(8) . . . . ? N1 C21 C22 C23 179.3(8) . . . . ? C25 N1 C29 C30 -60.7(9) . . . . ? C25 N1 C17 C18 63.7(10) . . . . ? C25 N1 C21 C22 -176.8(8) . . . . ? C25 C26 C27 C28 69.7(12) . . . . ? N2 C9 C10 C11 -179.0(8) . . . . ? N2 C13 C14 C15 164.4(9) . . . . ? C29 N1 C25 C26 -50.3(10) . . . . ? C29 N1 C17 C18 -175.8(8) . . . . ? C29 N1 C21 C22 61.6(10) . . . . ? C17 N1 C25 C26 67.3(9) . . . . ? C17 N1 C29 C30 179.5(7) . . . . ? C17 N1 C21 C22 -57.0(10) . . . . ? C17 C18 C19 C20 -178.3(10) . . . . ? C3 C2 C1 N2 174.7(10) . . . . ? C9 N2 C1 C2 -177.4(9) . . . . ? C9 N2 C13 C14 71.7(10) . . . . ? C9 N2 C5 C6 -63.8(10) . . . . ? C9 C10 C11 C12 -178.4(9) . . . . ? C1 N2 C9 C10 -164.6(8) . . . . ? C1 N2 C13 C14 -46.4(11) . . . . ? C1 N2 C5 C6 53.8(11) . . . . ? C1 C2 C3 C4 -72.9(15) . . . . ? C13 N2 C9 C10 73.6(10) . . . . ? C13 N2 C1 C2 -56.2(11) . . . . ? C13 N2 C5 C6 175.0(8) . . . . ? C13 C14 C15 C16 -171.0(11) . . . . ? C21 N1 C25 C26 -172.1(8) . . . . ? C21 N1 C29 C30 58.2(10) . . . . ? C21 N1 C17 C18 -54.2(10) . . . . ? C32 C31 C30 C29 -71.0(13) . . . . ? C5 N2 C9 C10 -44.2(11) . . . . ? C5 N2 C1 C2 61.1(11) . . . . ? C5 N2 C13 C14 -166.6(9) . . . . ? C5 C6 C7 C8 173.3(9) . . . . ? C24 C23 C22 C21 179.7(10) . . . . ? C7 C6 C5 N2 170.1(8) . . . . ?