#------------------------------------------------------------------------------ #$Date: 2024-11-21 01:10:52 +0200 (Thu, 21 Nov 2024) $ #$Revision: 296021 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573235.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_1573235 loop_ _publ_author_name 'Sumida, Akifumi' 'Saeki, Akinori' 'Matsuo, Kyohei' 'Naka, Kensuke' 'Imoto, Hiroaki' _publ_section_title ; Dithienoarsinines: Stable and Planer \p-Extended Arsabenzenes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC06590E _journal_year 2024 _chemical_formula_moiety 'C23 H15 As O4 S2' _chemical_formula_sum 'C23 H15 As O4 S2' _chemical_formula_weight 494.39 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-06-23 _audit_creation_method ; Olex2 1.5-ac5-024 (compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498) ; _audit_update_record ; 2024-09-20 deposited with the CCDC. 2024-11-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 17.8326(12) _cell_length_b 7.7360(6) _cell_length_c 30.2340(15) _cell_measurement_reflns_used 4150 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 31.1420 _cell_measurement_theta_min 2.8960 _cell_volume 4170.9(5) _computing_cell_refinement 'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100.00 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _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 66.00 0.20 1.75 -- 30.00 54.00-180.00 700 2 \w 21.00 46.00 0.20 1.75 -- 30.00 54.00 60.00 125 ; _diffrn_measurement_device 'two-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Mini (JP)' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0158450000 _diffrn_orient_matrix_UB_12 -0.0128898000 _diffrn_orient_matrix_UB_13 0.0672668000 _diffrn_orient_matrix_UB_21 0.0334320000 _diffrn_orient_matrix_UB_22 0.0126526000 _diffrn_orient_matrix_UB_23 -0.0046846000 _diffrn_orient_matrix_UB_31 -0.0145993000 _diffrn_orient_matrix_UB_32 0.0149421000 _diffrn_orient_matrix_UB_33 0.0622249000 _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 0.0413 _diffrn_reflns_av_unetI/netI 0.0562 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 11351 _diffrn_reflns_point_group_measured_fraction_full 0.650 _diffrn_reflns_point_group_measured_fraction_max 0.643 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.369 _diffrn_reflns_theta_min 2.652 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.858 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_correction_T_min 0.910 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023) 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 colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.575 _exptl_crystal_description block _exptl_crystal_F_000 2000 _exptl_crystal_size_max 0.547 _exptl_crystal_size_mid 0.285 _exptl_crystal_size_min 0.083 _refine_diff_density_max 1.106 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.106 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.027(19) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 546 _refine_ls_number_reflns 5488 _refine_ls_number_restraints 58 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0412 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0921 _refine_ls_wR_factor_ref 0.0990 _reflns_Friedel_coverage 0.264 _reflns_Friedel_fraction_full 0.287 _reflns_Friedel_fraction_max 0.274 _reflns_number_gt 4866 _reflns_number_total 5488 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 3c-DMAD_a.res in Pna2(1) 3c-DMAD.res created by SHELXL-2018/3 at 22:00:13 on 23-Jun-2024 REM Old TITL 3c-DMAD in Pnma REM SHELXT solution in Pna2(1): R1 0.086, Rweak 0.005, Alpha 0.005 REM 0.512 for 483 systematic absences, Orientation a'=-a, b'=c, c'=b REM Flack x = 0.093 ( 0.015 ) from 898 Parsons' quotients REM Formula found by SHELXT: C46 O8 S4 As2 CELL 0.71073 17.8326 7.736 30.234 90 90 90 ZERR 8 0.0012 0.0006 0.0015 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,+Z SYMM 0.5-X,0.5+Y,0.5+Z SFAC C H As O S UNIT 184 120 8 32 16 RIGU 0.002 0.002 C31 O008 O00D C30 C27 RIGU 0.002 0.002 O007 O00E C28 C24 C30 C27 O008 O00D C31 C29 L.S. 20 PLAN 1 SIZE 0.083 0.285 0.547 TEMP -173.15 BOND list 4 fmap 2 53 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 0 0 -4 OMIT 0 1 -1 OMIT 0 1 1 REM REM REM WGHT 0.049600 BASF 0.02727 FVAR 0.19458 AS1 3 0.402385 0.526143 0.653720 11.00000 0.01781 0.02384 = 0.01215 0.00218 -0.00118 -0.00375 AS2 3 0.336702 -0.541542 0.843050 11.00000 0.01846 0.02194 = 0.01077 0.00054 -0.00179 -0.00358 S1 5 0.286660 0.387967 0.732529 11.00000 0.02612 0.02592 = 0.01160 -0.00148 0.00300 -0.00478 S4 5 0.451489 -0.393200 0.764848 11.00000 0.02571 0.02486 = 0.01048 -0.00094 0.00198 -0.00358 S3 5 0.162527 -0.386733 0.845509 11.00000 0.01751 0.02716 = 0.01945 0.00458 -0.00550 -0.00510 S2 5 0.576723 0.371717 0.652421 11.00000 0.01549 0.03050 = 0.01859 0.00595 -0.00347 -0.00598 O007 4 0.458393 -0.564125 0.959927 11.00000 0.02625 0.03363 = 0.01640 0.00501 -0.00828 -0.00335 O008 4 0.382006 -0.251535 0.984007 11.00000 0.03013 0.04823 = 0.01025 -0.00905 -0.00185 -0.00547 O009 4 0.257656 0.112145 0.551293 11.00000 0.01924 0.04869 = 0.01938 -0.00324 -0.00454 -0.00634 O00A 4 0.357390 0.732246 0.566966 11.00000 0.03504 0.03363 = 0.02789 0.01260 -0.00986 -0.00714 O00B 4 0.358914 0.217218 0.514531 11.00000 0.02523 0.05196 = 0.01117 -0.00515 0.00262 0.00084 O00C 4 0.278687 0.534407 0.538005 11.00000 0.02690 0.03713 = 0.01664 0.00627 -0.00766 0.00103 O00D 4 0.481946 -0.140742 0.948318 11.00000 0.02785 0.04327 = 0.02180 -0.00159 -0.00719 -0.01297 O00E 4 0.382150 -0.757929 0.927808 11.00000 0.03250 0.03186 = 0.02808 0.00591 -0.00836 -0.00944 C9 1 0.254032 0.173940 0.730194 11.00000 0.02493 0.02860 = 0.00890 0.00056 -0.00279 0.00211 C44 1 0.453683 -0.095816 0.805942 11.00000 0.01349 0.01560 = 0.01556 0.00083 -0.00186 -0.00073 C16 1 0.459774 0.189672 0.633270 11.00000 0.01628 0.02741 = 0.01173 0.00331 -0.00091 -0.00010 C17 1 0.521449 0.073812 0.626654 11.00000 0.01337 0.03110 = 0.01389 0.01135 0.00062 -0.00196 C42 1 0.522680 0.158708 0.785771 11.00000 0.03042 0.01730 = 0.02664 0.00211 -0.00474 -0.00477 AFIX 43 H42 2 0.537188 0.274762 0.791454 11.00000 -1.20000 AFIX 0 C25 1 0.259085 -0.365953 0.852000 11.00000 0.01613 0.02896 = 0.01704 0.00092 -0.00189 -0.00455 C39 1 0.482587 -0.176379 0.768306 11.00000 0.02071 0.02727 = 0.01007 -0.00378 -0.00347 0.00025 C14 1 0.284985 0.084952 0.693378 11.00000 0.01530 0.03178 = 0.01015 0.00285 -0.00276 0.00097 C43 1 0.474050 0.077207 0.814500 11.00000 0.01940 0.01836 = 0.01582 0.00140 -0.00068 0.00092 AFIX 43 H43 2 0.454671 0.136421 0.839542 11.00000 -1.20000 AFIX 0 C28 1 0.405358 -0.613827 0.930439 11.00000 0.01682 0.02968 = 0.01201 0.00061 -0.00247 -0.00144 C15 1 0.335045 0.195759 0.668456 11.00000 0.01449 0.02745 = 0.00627 -0.00085 -0.00304 -0.00330 C7 1 0.314837 0.194641 0.549808 11.00000 0.02088 0.03191 = 0.01079 -0.00198 -0.00551 0.00436 C38 1 0.279620 -0.205422 0.865841 11.00000 0.01431 0.02647 = 0.01238 0.00352 -0.00378 -0.00271 C2 1 0.340487 0.358091 0.685169 11.00000 0.01546 0.03020 = 0.00877 0.00421 -0.00036 -0.00090 C46 1 0.362918 -0.170846 0.873242 11.00000 0.01199 0.02060 = 0.01422 0.00004 0.00099 -0.00542 AFIX 13 H46 2 0.371554 -0.049128 0.883146 11.00000 -1.20000 AFIX 0 C19 1 0.590193 -0.184230 0.608440 11.00000 0.02484 0.03598 = 0.01854 0.00930 0.00472 0.00445 AFIX 43 H19 2 0.591217 -0.301028 0.598753 11.00000 -1.20000 AFIX 0 C13 1 0.263666 -0.087852 0.686373 11.00000 0.02055 0.02493 = 0.01788 -0.00497 0.00410 -0.00215 AFIX 43 H13 2 0.283574 -0.150346 0.662006 11.00000 -1.20000 AFIX 0 C40 1 0.531449 -0.096120 0.739365 11.00000 0.02956 0.02925 = 0.01199 0.00263 0.00554 0.00249 AFIX 43 H40 2 0.550864 -0.154856 0.714259 11.00000 -1.20000 AFIX 0 C45 1 0.404499 -0.208181 0.830410 11.00000 0.01738 0.02287 = 0.00891 -0.00012 -0.00103 0.00038 C10 1 0.204719 0.094548 0.759356 11.00000 0.03176 0.02823 = 0.01155 -0.00280 0.00065 -0.00250 AFIX 43 H10 2 0.185165 0.155139 0.784134 11.00000 -1.20000 AFIX 0 C22 1 0.590555 0.154471 0.637364 11.00000 0.01766 0.02747 = 0.01265 0.00597 -0.00098 -0.00404 C41 1 0.551029 0.074327 0.748529 11.00000 0.02814 0.02406 = 0.02010 0.00643 0.00306 -0.00579 AFIX 43 H41 2 0.584102 0.134006 0.729200 11.00000 -1.20000 AFIX 0 C24 1 0.384292 -0.470748 0.900774 11.00000 0.01208 0.03181 = 0.01048 -0.00205 0.00033 0.00002 C4 1 0.349236 0.278776 0.590426 11.00000 0.01000 0.04184 = 0.00950 0.00293 0.00339 -0.00242 C23 1 0.376211 0.153233 0.626011 11.00000 0.01804 0.02399 = 0.01069 -0.00039 0.00111 0.00181 AFIX 13 H23 2 0.367597 0.030476 0.616979 11.00000 -1.20000 AFIX 0 C26 1 0.398153 -0.369148 0.812339 11.00000 0.01967 0.02830 = 0.00764 0.00005 -0.00187 -0.00179 C30 1 0.424354 -0.222978 0.948455 11.00000 0.01938 0.02921 = 0.01428 -0.00234 -0.00285 0.00105 C18 1 0.523079 -0.100567 0.611593 11.00000 0.01839 0.02413 = 0.01493 0.00668 0.00258 0.00016 AFIX 43 H18 2 0.477881 -0.158038 0.603822 11.00000 -1.20000 AFIX 0 C36 1 0.217345 0.082458 0.886636 11.00000 0.01349 0.02889 = 0.01882 0.00507 0.00109 -0.00179 AFIX 43 H36 2 0.263069 0.139577 0.893447 11.00000 -1.20000 AFIX 0 C5 1 0.332375 0.588415 0.566005 11.00000 0.01291 0.03849 = 0.01168 0.00340 0.00271 -0.00063 C1 1 0.355069 0.448025 0.596889 11.00000 0.01266 0.02884 = 0.01228 0.00333 0.00031 -0.00129 C3 1 0.480804 0.348959 0.646317 11.00000 0.01577 0.03348 = 0.01156 -0.00023 -0.00271 0.00066 C20 1 0.658444 -0.100491 0.619320 11.00000 0.01757 0.03781 = 0.02183 0.01347 -0.00035 0.00688 AFIX 43 H20 2 0.704265 -0.162518 0.617076 11.00000 -1.20000 AFIX 0 C11 1 0.184867 -0.075824 0.751231 11.00000 0.02815 0.03949 = 0.01405 0.00442 0.00588 -0.00651 AFIX 43 H11 2 0.150937 -0.132270 0.770678 11.00000 -1.20000 AFIX 0 C27 1 0.390499 -0.300453 0.908202 11.00000 0.01201 0.03178 = 0.01234 -0.00176 0.00104 0.00065 C33 1 0.080938 -0.083879 0.865577 11.00000 0.01567 0.03780 = 0.01844 0.00749 -0.00027 -0.00150 AFIX 43 H33 2 0.034947 -0.139774 0.858726 11.00000 -1.20000 AFIX 0 C12 1 0.213909 -0.166647 0.714828 11.00000 0.02092 0.02553 = 0.02563 0.00151 0.00109 -0.00062 AFIX 43 H12 2 0.199171 -0.283007 0.709798 11.00000 -1.20000 AFIX 0 C32 1 0.149161 -0.172708 0.862347 11.00000 0.01419 0.03793 = 0.00931 0.00770 -0.00012 -0.00323 C29 1 0.483848 -0.698922 0.989453 11.00000 0.04777 0.04847 = 0.02900 0.01689 -0.02091 -0.00734 AFIX 137 H29A 2 0.501347 -0.797999 0.972090 11.00000 -1.50000 H29B 2 0.442356 -0.735089 1.008587 11.00000 -1.50000 H29C 2 0.525095 -0.655049 1.007695 11.00000 -1.50000 AFIX 0 C37 1 0.217635 -0.090791 0.872797 11.00000 0.01591 0.03123 = 0.01314 0.00325 0.00114 -0.00384 C35 1 0.149695 0.169150 0.890250 11.00000 0.02935 0.02643 = 0.02000 0.00694 0.00470 -0.00035 AFIX 43 H35 2 0.148786 0.285302 0.900435 11.00000 -1.20000 AFIX 0 C34 1 0.082038 0.085395 0.878836 11.00000 0.01828 0.03759 = 0.02258 0.01415 0.00289 0.00623 AFIX 43 H34 2 0.036253 0.147881 0.880391 11.00000 -1.20000 AFIX 0 C6 1 0.252544 0.665382 0.507019 11.00000 0.04096 0.04989 = 0.02414 0.01531 -0.00363 0.01097 AFIX 137 H6A 2 0.293811 0.699035 0.487421 11.00000 -1.50000 H6B 2 0.235002 0.766831 0.523444 11.00000 -1.50000 H6C 2 0.211231 0.618401 0.489345 11.00000 -1.50000 AFIX 0 C8 1 0.330499 0.142049 0.473924 11.00000 0.04145 0.07508 = 0.00996 -0.00569 0.00010 -0.00464 AFIX 137 H8A 2 0.362964 0.175482 0.449209 11.00000 -1.50000 H8B 2 0.279474 0.184042 0.468496 11.00000 -1.50000 H8C 2 0.329853 0.015816 0.476619 11.00000 -1.50000 AFIX 0 C31 1 0.413179 -0.195792 1.026321 11.00000 0.04967 0.07244 = 0.01120 -0.01444 -0.00892 -0.00610 AFIX 137 H31A 2 0.419458 -0.069942 1.026188 11.00000 -1.50000 H31B 2 0.461988 -0.251163 1.030918 11.00000 -1.50000 H31C 2 0.379015 -0.228854 1.050259 11.00000 -1.50000 AFIX 0 C21 1 0.659519 0.070189 0.633168 11.00000 0.01703 0.03817 = 0.01940 0.01158 -0.00148 0.00275 AFIX 43 H21 2 0.705327 0.127690 0.639560 11.00000 -1.20000 AFIX 0 HKLF 4 REM 3c-DMAD_a.res in Pna2(1) REM wR2 = 0.0990, GooF = S = 1.056, Restrained GooF = 1.051 for all data REM R1 = 0.0412 for 4866 Fo > 4sig(Fo) and 0.0502 for all 5488 data REM 546 parameters refined using 58 restraints END WGHT 0.0496 0.0000 REM Highest difference peak 1.106, deepest hole -0.496, 1-sigma level 0.106 Q1 1 0.4011 0.3955 0.6564 11.00000 0.05 1.11 REM The information below was added by Olex2. REM REM R1 = 0.0412 for 4866 Fo > 4sig(Fo) and 0.0502 for all 12358 data REM 546 parameters refined using n/a restraints REM Highest difference peak 1.11, deepest hole -0.50 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0502 REM R1_gt = 0.0412 REM wR_ref = 0.0990 REM GOOF = 1.056 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 12358 REM Reflections_gt = 4866 REM Parameters = 546 REM Hole = -0.50 REM Peak = 1.11 REM Flack = n/a ; _cod_data_source_file d4sc06590e2.cif _cod_data_source_block 3c-DMAD _cod_database_code 1573235 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula CHOAsS _chemical_oxdiff_usercomment ' ' _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 0.861 _shelx_estimated_absorpt_t_min 0.430 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.973(19) 0.027(19) 2. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 3. Rigid body (RIGU) restrains C31, O008, O00D, C30, C27 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 O007, O00E, C28, C24, C30, C27, O008, O00D, C31, C29 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 4.a Ternary CH refined with riding coordinates: C46(H46), C23(H23) 4.b Aromatic/amide H refined with riding coordinates: C42(H42), C43(H43), C19(H19), C13(H13), C40(H40), C10(H10), C41(H41), C18(H18), C36(H36), C20(H20), C11(H11), C33(H33), C12(H12), C35(H35), C34(H34), C21(H21) 4.c Idealised Me refined as rotating group: C29(H29A,H29B,H29C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C31(H31A,H31B,H31C) ; _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 1.993 _oxdiff_exptl_absorpt_empirical_full_min 0.728 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.40238(3) 0.52614(8) 0.65372(2) 0.01793(16) Uani 1 1 d . . . . . As2 As 0.33670(3) -0.54154(8) 0.84305(2) 0.01706(15) Uani 1 1 d . . . . . S1 S 0.28666(9) 0.3880(2) 0.73253(6) 0.0212(4) Uani 1 1 d . . . . . S4 S 0.45149(9) -0.3932(2) 0.76485(5) 0.0203(4) Uani 1 1 d . . . . . S3 S 0.16253(8) -0.3867(2) 0.84551(6) 0.0214(4) Uani 1 1 d . . . . . S2 S 0.57672(8) 0.3717(2) 0.65242(6) 0.0215(3) Uani 1 1 d . . . . . O007 O 0.4584(3) -0.5641(6) 0.95993(15) 0.0254(11) Uani 1 1 d . . . . . O008 O 0.3820(3) -0.2515(7) 0.98401(16) 0.0295(12) Uani 1 1 d . . . . . O009 O 0.2577(3) 0.1121(7) 0.55129(16) 0.0291(12) Uani 1 1 d . . . . . O00A O 0.3574(3) 0.7322(7) 0.56697(18) 0.0322(12) Uani 1 1 d . . . . . O00B O 0.3589(3) 0.2172(8) 0.51453(15) 0.0295(12) Uani 1 1 d . . . . . O00C O 0.2787(3) 0.5344(7) 0.53800(15) 0.0269(11) Uani 1 1 d . . . . . O00D O 0.4819(3) -0.1407(7) 0.94832(16) 0.0310(12) Uani 1 1 d . . . . . O00E O 0.3821(3) -0.7579(7) 0.92781(18) 0.0308(11) Uani 1 1 d . . . . . C9 C 0.2540(4) 0.1739(9) 0.7302(2) 0.0208(14) Uani 1 1 d . . . . . C44 C 0.4537(3) -0.0958(8) 0.8059(2) 0.0149(13) Uani 1 1 d . . . . . C16 C 0.4598(3) 0.1897(9) 0.6333(2) 0.0185(14) Uani 1 1 d . . . . . C17 C 0.5214(3) 0.0738(9) 0.6267(2) 0.0195(14) Uani 1 1 d . . . . . C42 C 0.5227(4) 0.1587(9) 0.7858(2) 0.0248(15) Uani 1 1 d . . . . . H42 H 0.537188 0.274762 0.791454 0.030 Uiso 1 1 calc R U . . . C25 C 0.2591(3) -0.3660(9) 0.8520(2) 0.0207(14) Uani 1 1 d . . . . . C39 C 0.4826(3) -0.1764(9) 0.7683(2) 0.0193(14) Uani 1 1 d . . . . . C14 C 0.2850(3) 0.0850(9) 0.6934(2) 0.0191(14) Uani 1 1 d . . . . . C43 C 0.4741(3) 0.0772(9) 0.8145(2) 0.0179(14) Uani 1 1 d . . . . . H43 H 0.454671 0.136421 0.839542 0.021 Uiso 1 1 calc R U . . . C28 C 0.4054(3) -0.6138(10) 0.9304(2) 0.0195(13) Uani 1 1 d . . . . . C15 C 0.3350(3) 0.1958(10) 0.6685(2) 0.0161(14) Uani 1 1 d . . . . . C7 C 0.3148(4) 0.1946(10) 0.5498(2) 0.0212(15) Uani 1 1 d . . . . . C38 C 0.2796(3) -0.2054(9) 0.8658(2) 0.0177(14) Uani 1 1 d . . . . . C2 C 0.3405(3) 0.3581(10) 0.6852(2) 0.0181(15) Uani 1 1 d . . . . . C46 C 0.3629(3) -0.1708(9) 0.87324(19) 0.0156(13) Uani 1 1 d . . . . . H46 H 0.371554 -0.049128 0.883146 0.019 Uiso 1 1 calc R U . . . C19 C 0.5902(4) -0.1842(10) 0.6084(2) 0.0265(16) Uani 1 1 d . . . . . H19 H 0.591217 -0.301028 0.598753 0.032 Uiso 1 1 calc R U . . . C13 C 0.2637(3) -0.0879(9) 0.6864(2) 0.0211(14) Uani 1 1 d . . . . . H13 H 0.283574 -0.150346 0.662006 0.025 Uiso 1 1 calc R U . . . C40 C 0.5314(4) -0.0961(10) 0.7394(2) 0.0236(15) Uani 1 1 d . . . . . H40 H 0.550864 -0.154856 0.714259 0.028 Uiso 1 1 calc R U . . . C45 C 0.4045(3) -0.2082(9) 0.8304(2) 0.0164(14) Uani 1 1 d . . . . . C10 C 0.2047(4) 0.0945(10) 0.7594(2) 0.0238(15) Uani 1 1 d . . . . . H10 H 0.185165 0.155139 0.784134 0.029 Uiso 1 1 calc R U . . . C22 C 0.5906(3) 0.1545(9) 0.6374(2) 0.0193(15) Uani 1 1 d . . . . . C41 C 0.5510(4) 0.0743(9) 0.7485(2) 0.0241(15) Uani 1 1 d . . . . . H41 H 0.584102 0.134006 0.729200 0.029 Uiso 1 1 calc R U . . . C24 C 0.3843(3) -0.4707(9) 0.9008(2) 0.0181(12) Uani 1 1 d . . . . . C4 C 0.3492(3) 0.2788(10) 0.5904(2) 0.0204(14) Uani 1 1 d . . . . . C23 C 0.3762(3) 0.1532(9) 0.62601(19) 0.0176(14) Uani 1 1 d . . . . . H23 H 0.367597 0.030476 0.616979 0.021 Uiso 1 1 calc R U . . . C26 C 0.3982(3) -0.3691(9) 0.8123(2) 0.0185(14) Uani 1 1 d . . . . . C30 C 0.4244(4) -0.2230(10) 0.9485(2) 0.0210(13) Uani 1 1 d . . . . . C18 C 0.5231(3) -0.1006(9) 0.6116(2) 0.0191(14) Uani 1 1 d . . . . . H18 H 0.477881 -0.158038 0.603822 0.023 Uiso 1 1 calc R U . . . C36 C 0.2173(3) 0.0825(9) 0.8866(2) 0.0204(14) Uani 1 1 d . . . . . H36 H 0.263069 0.139577 0.893447 0.024 Uiso 1 1 calc R U . . . C5 C 0.3324(3) 0.5884(10) 0.5660(2) 0.0210(15) Uani 1 1 d . . . . . C1 C 0.3551(3) 0.4480(9) 0.5969(2) 0.0179(14) Uani 1 1 d . . . . . C3 C 0.4808(3) 0.3490(9) 0.6463(2) 0.0203(14) Uani 1 1 d . . . . . C20 C 0.6584(4) -0.1005(10) 0.6193(2) 0.0257(16) Uani 1 1 d . . . . . H20 H 0.704265 -0.162518 0.617076 0.031 Uiso 1 1 calc R U . . . C11 C 0.1849(4) -0.0758(10) 0.7512(2) 0.0272(16) Uani 1 1 d . . . . . H11 H 0.150937 -0.132270 0.770678 0.033 Uiso 1 1 calc R U . . . C27 C 0.3905(3) -0.3005(10) 0.9082(2) 0.0187(12) Uani 1 1 d . . . . . C33 C 0.0809(4) -0.0839(10) 0.8656(2) 0.0240(16) Uani 1 1 d . . . . . H33 H 0.034947 -0.139774 0.858726 0.029 Uiso 1 1 calc R U . . . C12 C 0.2139(3) -0.1666(10) 0.7148(2) 0.0240(15) Uani 1 1 d . . . . . H12 H 0.199171 -0.283007 0.709798 0.029 Uiso 1 1 calc R U . . . C32 C 0.1492(3) -0.1727(10) 0.8623(2) 0.0205(14) Uani 1 1 d . . . . . C29 C 0.4838(5) -0.6989(12) 0.9895(3) 0.042(2) Uani 1 1 d . . . . . H29A H 0.501347 -0.797999 0.972090 0.063 Uiso 1 1 calc R U . . . H29B H 0.442356 -0.735089 1.008587 0.063 Uiso 1 1 calc R U . . . H29C H 0.525095 -0.655049 1.007695 0.063 Uiso 1 1 calc R U . . . C37 C 0.2176(3) -0.0908(9) 0.8728(2) 0.0201(14) Uani 1 1 d . . . . . C35 C 0.1497(4) 0.1691(10) 0.8902(2) 0.0253(15) Uani 1 1 d . . . . . H35 H 0.148786 0.285302 0.900435 0.030 Uiso 1 1 calc R U . . . C34 C 0.0820(4) 0.0854(10) 0.8788(2) 0.0261(16) Uani 1 1 d . . . . . H34 H 0.036253 0.147881 0.880391 0.031 Uiso 1 1 calc R U . . . C6 C 0.2525(4) 0.6654(12) 0.5070(2) 0.038(2) Uani 1 1 d . . . . . H6A H 0.293811 0.699035 0.487421 0.058 Uiso 1 1 calc R U . . . H6B H 0.235002 0.766831 0.523444 0.058 Uiso 1 1 calc R U . . . H6C H 0.211231 0.618401 0.489345 0.058 Uiso 1 1 calc R U . . . C8 C 0.3305(4) 0.1420(13) 0.4739(2) 0.042(2) Uani 1 1 d . . . . . H8A H 0.362964 0.175482 0.449209 0.063 Uiso 1 1 calc R U . . . H8B H 0.279474 0.184042 0.468496 0.063 Uiso 1 1 calc R U . . . H8C H 0.329853 0.015816 0.476619 0.063 Uiso 1 1 calc R U . . . C31 C 0.4132(5) -0.1958(13) 1.0263(2) 0.044(2) Uani 1 1 d . . . . . H31A H 0.419458 -0.069942 1.026188 0.067 Uiso 1 1 calc R U . . . H31B H 0.461988 -0.251163 1.030918 0.067 Uiso 1 1 calc R U . . . H31C H 0.379015 -0.228854 1.050259 0.067 Uiso 1 1 calc R U . . . C21 C 0.6595(4) 0.0702(10) 0.6332(2) 0.0249(16) Uani 1 1 d . . . . . H21 H 0.705327 0.127690 0.639560 0.030 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 As1 0.0178(3) 0.0238(4) 0.0122(3) 0.0022(3) -0.0012(2) -0.0038(3) As2 0.0185(3) 0.0219(3) 0.0108(3) 0.0005(3) -0.0018(2) -0.0036(3) S1 0.0261(9) 0.0259(10) 0.0116(7) -0.0015(7) 0.0030(6) -0.0048(8) S4 0.0257(9) 0.0249(9) 0.0105(7) -0.0009(6) 0.0020(6) -0.0036(8) S3 0.0175(8) 0.0272(9) 0.0194(8) 0.0046(8) -0.0055(7) -0.0051(7) S2 0.0155(7) 0.0305(9) 0.0186(7) 0.0060(8) -0.0035(7) -0.0060(7) O007 0.026(2) 0.034(3) 0.016(2) 0.005(2) -0.0083(17) -0.003(2) O008 0.030(2) 0.048(4) 0.010(2) -0.009(2) -0.0019(17) -0.005(2) O009 0.019(2) 0.049(3) 0.019(2) -0.003(2) -0.0045(18) -0.006(2) O00A 0.035(3) 0.034(3) 0.028(3) 0.013(2) -0.010(2) -0.007(3) O00B 0.025(2) 0.052(4) 0.011(2) -0.005(2) 0.0026(18) 0.001(2) O00C 0.027(2) 0.037(3) 0.017(2) 0.006(2) -0.0077(19) 0.001(2) O00D 0.028(2) 0.043(3) 0.022(3) -0.002(2) -0.0072(19) -0.013(2) O00E 0.032(3) 0.032(3) 0.028(3) 0.006(2) -0.008(2) -0.009(2) C9 0.025(3) 0.029(4) 0.009(3) 0.001(3) -0.003(2) 0.002(3) C44 0.013(3) 0.016(3) 0.016(3) 0.001(3) -0.002(2) -0.001(3) C16 0.016(3) 0.027(4) 0.012(3) 0.003(3) -0.001(2) 0.000(3) C17 0.013(3) 0.031(4) 0.014(3) 0.011(3) 0.001(2) -0.002(3) C42 0.030(4) 0.017(4) 0.027(4) 0.002(3) -0.005(3) -0.005(3) C25 0.016(3) 0.029(4) 0.017(3) 0.001(3) -0.002(2) -0.005(3) C39 0.021(3) 0.027(4) 0.010(3) -0.004(3) -0.003(2) 0.000(3) C14 0.015(3) 0.032(4) 0.010(3) 0.003(3) -0.003(2) 0.001(3) C43 0.019(3) 0.018(3) 0.016(3) 0.001(3) -0.001(2) 0.001(3) C28 0.017(3) 0.030(3) 0.012(3) 0.001(2) -0.002(2) -0.001(2) C15 0.014(3) 0.027(4) 0.006(3) -0.001(3) -0.003(2) -0.003(3) C7 0.021(3) 0.032(4) 0.011(3) -0.002(3) -0.006(2) 0.004(3) C38 0.014(3) 0.026(4) 0.012(3) 0.004(3) -0.004(2) -0.003(3) C2 0.015(3) 0.030(4) 0.009(3) 0.004(3) 0.000(2) -0.001(3) C46 0.012(3) 0.021(4) 0.014(3) 0.000(3) 0.001(2) -0.005(3) C19 0.025(4) 0.036(4) 0.019(3) 0.009(3) 0.005(3) 0.004(3) C13 0.021(3) 0.025(4) 0.018(3) -0.005(3) 0.004(2) -0.002(3) C40 0.030(4) 0.029(4) 0.012(3) 0.003(3) 0.006(2) 0.002(3) C45 0.017(3) 0.023(4) 0.009(3) 0.000(3) -0.001(2) 0.000(3) C10 0.032(4) 0.028(4) 0.012(3) -0.003(3) 0.001(3) -0.003(3) C22 0.018(3) 0.027(4) 0.013(3) 0.006(3) -0.001(2) -0.004(3) C41 0.028(4) 0.024(4) 0.020(3) 0.006(3) 0.003(3) -0.006(3) C24 0.012(3) 0.032(3) 0.010(3) -0.002(2) 0.000(2) 0.000(2) C4 0.010(3) 0.042(4) 0.010(3) 0.003(3) 0.003(2) -0.002(3) C23 0.018(3) 0.024(4) 0.011(3) 0.000(3) 0.001(2) 0.002(3) C26 0.020(3) 0.028(4) 0.008(3) 0.000(3) -0.002(2) -0.002(3) C30 0.019(3) 0.029(4) 0.014(3) -0.002(2) -0.0028(19) 0.001(2) C18 0.018(3) 0.024(4) 0.015(3) 0.007(3) 0.003(2) 0.000(3) C36 0.013(3) 0.029(4) 0.019(3) 0.005(3) 0.001(2) -0.002(3) C5 0.013(3) 0.038(4) 0.012(3) 0.003(3) 0.003(2) -0.001(3) C1 0.013(3) 0.029(4) 0.012(3) 0.003(3) 0.000(2) -0.001(3) C3 0.016(3) 0.033(4) 0.012(3) 0.000(3) -0.003(2) 0.001(3) C20 0.018(3) 0.038(5) 0.022(3) 0.013(3) 0.000(3) 0.007(3) C11 0.028(4) 0.039(5) 0.014(3) 0.004(3) 0.006(3) -0.007(3) C27 0.012(3) 0.032(3) 0.012(3) -0.002(2) 0.001(2) 0.001(2) C33 0.016(3) 0.038(4) 0.018(3) 0.007(3) 0.000(3) -0.001(3) C12 0.021(3) 0.026(4) 0.026(4) 0.002(3) 0.001(3) -0.001(3) C32 0.014(3) 0.038(4) 0.009(3) 0.008(3) 0.000(2) -0.003(3) C29 0.048(5) 0.048(5) 0.029(4) 0.017(4) -0.021(3) -0.007(4) C37 0.016(3) 0.031(4) 0.013(3) 0.003(3) 0.001(2) -0.004(3) C35 0.029(4) 0.026(4) 0.020(3) 0.007(3) 0.005(3) 0.000(3) C34 0.018(3) 0.038(4) 0.023(4) 0.014(3) 0.003(3) 0.006(3) C6 0.041(4) 0.050(6) 0.024(4) 0.015(4) -0.004(3) 0.011(4) C8 0.041(5) 0.075(7) 0.010(3) -0.006(4) 0.000(3) -0.005(4) C31 0.050(5) 0.072(7) 0.011(3) -0.014(4) -0.009(3) -0.006(4) C21 0.017(3) 0.038(4) 0.019(3) 0.012(3) -0.001(3) 0.003(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' As As 0.0499 2.0058 '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_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l _diffrn_refln_intensity_net _diffrn_refln_intensity_u 0 1 0 0.23 0.44 0 2 0 109.41 5.44 0 3 0 1.66 1.37 0 4 0 859.97 25.14 0 5 0 1.09 1.78 0 6 0 44.48 6.14 0 7 0 2.85 2.94 0 8 0 3.53 3.23 0 9 0 -7.59 5.22 0 1 -1 128.65 4.67 0 1 1 175.11 5.36 0 2 -1 -0.05 0.74 0 2 1 -0.49 0.8 0 3 -1 155.08 8.14 0 3 1 168.58 8.61 0 4 1 1.61 1.42 0 4 -1 2.11 1.44 0 5 1 606.9 22.22 0 5 -1 575.03 21.82 0 6 1 5.68 3.04 0 6 -1 6.51 3.19 0 7 -1 158.11 13.01 0 7 1 151.93 12.49 0 8 1 2.26 3.75 0 8 -1 2.55 2.42 0 9 1 16.16 5.24 0 9 -1 20.56 5.68 0 1 -2 -0.47 0.51 0 2 -2 1486.56 30.99 0 2 2 1593.49 31.32 0 3 2 1.7 1.18 0 3 -2 0.74 0.89 0 4 2 821.69 24.66 0 4 -2 872.04 24.97 0 5 -2 1.83 2.04 0 5 2 1.59 2.13 0 6 -2 98 9.28 0 6 2 92.55 9 0 7 2 7.2 4.06 0 7 -2 2.18 2.8 0 8 -2 33.71 6.94 0 8 2 34.07 6.73 0 9 -2 -3.49 4.26 0 1 -3 589.57 13.29 0 2 3 -1.04 1.03 0 2 -3 0.04 0.83 0 3 -3 22.07 3.22 0 3 3 44.26 4.33 0 4 3 0.93 1.07 0 4 -3 0.13 1.34 0 5 3 1104.11 32.03 0 5 -3 1136.53 32.5 0 6 3 0.8 2.18 0 6 -3 0.88 2.56 0 7 3 414.86 21.51 0 7 -3 499.8 23.75 0 8 -3 1.4 2.65 0 9 -3 86.06 11.12 0 0 -4 17.02 1.69 0 1 -4 0.25 0.76 0 2 -4 947.5 21.91 0 3 4 1.17 1.16 0 3 -4 0.85 1.08 0 4 -4 74.98 6.36 0 4 4 77.64 6.62 0 5 4 1.28 1.76 0 5 -4 1.67 1.6 0 6 4 169.94 12.19 0 6 -4 151.28 11.6 0 7 -4 1.22 2.53 0 8 -4 44.94 8.11 0 9 -4 -6.42 5.06 0 0 -5 4.57 0.98 0 1 -5 300.94 9.2 0 2 -5 0.28 1.03 0 3 -5 16.38 2.77 0 4 -5 2.03 1.9 0 5 -5 51.81 6.39 0 6 -5 5.64 2.86 0 7 -5 267.9 17.07 0 8 -5 3.91 4.15 0 9 -5 3.05 4.14 0 0 -6 1662.09 31.44 0 1 -6 -0.2 0.82 0 2 -6 543.09 15.68 0 3 -6 -1.93 1.73 0 4 -6 225.37 11.95 0 5 -6 4.19 2.75 0 6 -6 193.34 13.29 0 7 -6 -3.11 3.24 0 8 -6 23.64 5.97 0 9 -6 5.44 4.86 0 0 -7 -0.07 0.6 0 1 -7 870.46 20.22 0 2 -7 0.08 1.15 0 3 -7 365.44 14.05 0 4 -7 1.21 1.33 0 5 -7 455.84 19.52 0 6 -7 2.55 2.54 0 7 -7 313.29 18.44 0 8 -7 1.24 3.1 0 9 -7 53.75 9.45 0 0 -8 2848.14 51.92 0 1 -8 1.48 1.12 0 2 -8 27.8 3.39 0 3 -8 -0.04 1.27 0 4 -8 224.78 11.92 0 5 -8 2.44 2.05 0 6 -8 138.87 11.45 0 7 -8 4.21 3.29 0 8 -8 24.66 6.25 0 9 -8 -6.94 4.92 0 0 -9 2.72 1.12 0 1 -9 52.09 4.3 0 -1 -9 47.43 4.24 0 2 -9 0.58 1.06 0 3 -9 241.75 11.68 0 4 -9 0.15 1.74 0 5 -9 1291.65 37.19 0 6 -9 3.4 2.61 0 7 -9 199.14 14.96 0 8 -9 0.03 3.1 0 9 -9 75.78 10.97 0 0 -10 6716.43 114.37 0 1 -10 2.05 1.42 0 -1 -10 1.58 1.11 0 2 -10 1409.16 33.17 0 3 -10 -2.43 2.13 0 4 -10 16.32 3.71 0 5 -10 1.81 2.03 0 6 -10 5.91 2.77 0 7 -10 1.03 2.41 0 8 -10 40.48 7.5 0 9 -10 1.67 4.43 0 0 -11 15.5 3.3 0 -1 -11 1308.5 30.27 0 1 -11 1276.35 29.96 0 2 -11 -1.58 1.6 0 3 -11 125.38 8.64 0 4 -11 4.61 2.66 0 5 -11 454.81 20.09 0 6 -11 6.11 3.51 0 7 -11 119.42 11.98 0 8 -11 0.56 2.72 0 9 -11 22.85 4.47 0 0 -12 284.41 11.6 0 1 -12 -0.1 1.19 0 -1 -12 0.69 0.98 0 2 -12 196.19 10.39 0 3 -12 2.91 2.26 0 4 -12 235.04 13.23 0 5 -12 3.05 2.05 0 6 -12 61.46 7.89 0 7 -12 2.02 2.78 0 8 -12 37.46 7.4 0 9 -12 -7.74 5.33 0 0 -13 2.92 1.55 0 1 -13 73.28 5.99 0 -1 -13 71.95 5.93 0 2 -13 5.02 1.78 0 3 -13 20.04 3.33 0 4 -13 1.53 2.06 0 5 -13 780.19 28.63 0 6 -13 2.35 3.05 0 7 -13 565.33 26.94 0 8 -13 2.7 3.1 0 9 -13 123.12 13.93 0 0 -14 203.01 10.45 0 1 -14 1.52 1.3 0 -1 -14 1.59 1.38 0 2 -14 80.36 7 0 -2 -14 57.43 6.38 0 3 -14 -2.1 2.12 0 4 -14 37.4 5.75 0 5 -14 0.63 2.48 0 6 -14 131.93 11.71 0 7 -14 -0.83 3.38 0 8 -14 75.3 10.63 0 0 -15 -0.82 1.28 0 1 -15 126.7 8.39 0 -1 -15 123.46 8.31 0 2 -15 0.62 1.54 0 -2 -15 1.85 1.27 0 3 -15 135.82 10.29 0 4 -15 -4.23 3.04 0 5 -15 118.56 10.72 0 6 -15 0.7 2.99 0 7 -15 261.84 18.55 0 8 -15 -4.7 3.51 0 0 -16 570.3 19.73 0 1 -16 -1.23 1.93 0 -1 -16 -0.67 1.1 0 2 -16 722.32 24.36 0 -2 -16 682.48 23.32 0 3 -16 4.15 2.52 0 4 -16 417.19 19.85 0 5 -16 2.53 2.71 0 6 -16 238.41 16.37 0 7 -16 -4.1 3.86 0 8 -16 10.71 5.57 0 0 -17 4.39 2.26 0 1 -17 14.62 3.21 0 -1 -17 18.41 3.56 0 2 -17 -3.67 2.75 0 -2 -17 1.89 1.98 0 3 -17 98.12 9.16 0 -3 -17 90.3 9.85 0 4 -17 0.23 2.54 0 5 -17 143.02 12.08 0 6 -17 1.84 2.66 0 7 -17 130.42 13.23 0 8 -17 -0.41 3.71 0 0 -18 68.88 6.89 0 1 -18 -2.71 1.94 0 -1 -18 0.66 1.47 0 2 -18 7.96 3.15 0 -2 -18 5.1 1.82 0 3 -18 1.4 2.86 0 -3 -18 2.31 2.26 0 4 -18 48.08 7.27 0 5 -18 -0.81 3.04 0 6 -18 32.04 6.83 0 7 -18 -3.28 3.59 0 8 -18 27.3 6.87 0 0 -19 -4.3 2.87 0 1 -19 567.67 21.82 0 -1 -19 588.31 22.04 0 2 -19 -2.8 3.22 0 -2 -19 -1.08 1.48 0 3 -19 327.12 17.74 0 -3 -19 309.73 17.08 0 4 -19 -2.31 2.96 0 5 -19 94.56 10.2 0 6 -19 -1.81 3.8 0 7 -19 313.55 21.38 0 8 -19 -3.82 4.25 0 0 -20 697.95 24.8 0 1 -20 -0.48 1.54 0 -1 -20 0.45 1.84 0 2 -20 815.08 28.42 0 -2 -20 761.33 26.65 0 3 -20 -3.24 2.91 0 -3 -20 -3.3 2.23 0 4 -20 51.51 7.61 0 -4 -20 43.25 7.48 0 5 -20 -6.26 3.68 0 6 -20 34.57 6.89 0 7 -20 -0.72 3.41 0 8 -20 7.48 4.36 0 0 -21 3.94 2.31 0 1 -21 718.41 26.1 0 -1 -21 679.8 25.13 0 2 -21 -2.51 2.35 0 -2 -21 -0.61 2.16 0 3 -21 220.49 14.99 0 -3 -21 205.66 13.62 0 4 -21 2.6 3.64 0 -4 -21 0.19 2.01 0 5 -21 17.3 5.13 0 6 -21 -0.73 2.82 0 7 -21 49.47 9.27 0 8 -21 -3.44 4.81 0 0 -22 405.88 19.04 0 1 -22 0.19 2 0 -1 -22 2.74 2.3 0 2 -22 430 20.78 0 -2 -22 447.71 20.33 0 3 -22 2.03 2.58 0 -3 -22 1.66 2.09 0 4 -22 184.25 14.85 0 -4 -22 174.49 14.04 0 5 -22 -2.13 3.18 0 -5 -22 -3.24 3.39 0 6 -22 22.36 6.62 0 7 -22 -1.24 3.96 0 0 -23 3.34 2.69 0 1 -23 26.77 4.81 0 -1 -23 25.07 4.85 0 2 -23 2.37 2.7 0 -2 -23 -2.54 2.07 0 3 -23 15.48 4.99 0 -3 -23 6.77 2.97 0 4 -23 -1.88 2.8 0 -4 -23 1.62 1.93 0 -5 -23 413.6 24.93 0 5 -23 501.09 26.62 0 6 -23 3.64 4.07 0 7 -23 316.65 22.69 0 0 -24 436.65 20.6 0 1 -24 -2.22 2.54 0 -1 -24 -2.81 2.89 0 2 -24 4.47 3.26 0 -2 -24 8.19 3.42 0 3 -24 4.94 3.66 0 -3 -24 -0.85 2.59 0 4 -24 145.19 14.08 0 -4 -24 109.34 11.13 0 5 -24 -2.43 3.43 0 -5 -24 0.77 2.86 0 6 -24 36.34 8.44 0 -6 -24 44.36 8.74 0 7 -24 -1.43 3.71 0 0 -25 2.97 2.29 0 1 -25 53.79 7.53 0 -1 -25 51.2 7.19 0 2 -25 -9.54 4.9 0 -2 -25 2.12 2.65 0 3 -25 64.44 8.97 0 -3 -25 45.19 7.52 0 4 -25 2.46 3.43 0 -4 -25 0.98 2.17 0 -5 -25 282.55 19.19 0 5 -25 336.19 22.18 0 6 -25 0.64 4.24 0 -6 -25 4.3 4.53 0 7 -25 242.86 21.79 0 -7 -25 218.27 19.53 0 0 -26 1399.98 42.35 0 1 -26 1.22 2.67 0 -1 -26 3.39 2.77 0 -2 -26 936.47 34.25 0 2 -26 965.04 35.76 0 3 -26 2.03 2.87 0 -3 -26 1.62 2.04 0 4 -26 46.25 9.15 0 -4 -26 45.63 7.74 0 5 -26 -0.5 3.81 0 -5 -26 6.64 4.16 0 6 -26 4.03 3.92 0 -6 -26 4.08 4.66 0 7 -26 -0.33 4.5 0 -7 -26 -3.45 4.82 0 0 -27 18.74 4.69 0 -1 -27 392.93 20.88 0 1 -27 386.27 21.49 0 2 -27 -5.94 3.84 0 -2 -27 -0.55 2.82 0 3 -27 32.07 7.43 0 -3 -27 12.91 4.37 0 4 -27 -0.19 4.41 0 -4 -27 -2.39 3.23 0 -5 -27 142.34 14.28 0 5 -27 169.65 16.97 0 6 -27 5.29 5.39 0 -6 -27 5.53 4.47 0 0 -28 764.41 31.44 0 1 -28 -2.05 3.01 0 -1 -28 1.36 2.89 0 -2 -28 94.75 10.57 0 2 -28 95.14 11.61 0 3 -28 -0.83 3.54 0 -3 -28 -1.79 3.41 0 4 -28 -3.89 5.24 0 -4 -28 13.45 4.82 0 5 -28 -2.76 4.95 0 -5 -28 -2.44 2.88 0 6 -28 83.09 13.13 0 -6 -28 66.8 10.14 0 0 -29 13.76 5.29 0 -1 -29 112.83 11.87 0 1 -29 108.97 11.9 0 2 -29 7.07 4.69 0 -2 -29 1.88 2.54 0 3 -29 80.75 10.97 0 -3 -29 64.32 9.97 0 4 -29 -1.23 4.71 0 -4 -29 -1.33 3.62 0 -5 -29 259.8 19.91 0 5 -29 308.04 23.78 0 -6 -29 -1.96 4.64 0 6 -29 2.46 5.38 0 0 -30 77.74 9.89 0 -1 -30 0.19 2.58 0 1 -30 0.61 3.12 0 -2 -30 65.21 9.36 0 2 -30 47.43 8.85 0 -3 -30 2 3.3 0 3 -30 -5.38 4.19 0 -4 -30 10.25 5.11 0 4 -30 25.3 6.97 0 -5 -30 8.15 4.4 0 5 -30 4.28 4.85 0 0 -31 3.46 3.7 0 -1 -31 0.16 3.25 0 1 -31 -1.39 3.13 0 -2 -31 -0.73 2.66 0 2 -31 3.32 3.74 0 -3 -31 10.64 4.94 0 3 -31 4.83 4.3 0 -4 -31 3.03 4.01 0 4 -31 2.06 5.05 0 -5 -31 32.78 7.81 0 5 -31 30.02 7.83 0 0 -32 347.02 22.09 0 -1 -32 1.31 3.01 0 1 -32 -1.32 2.93 0 -2 -32 579.4 29.04 0 2 -32 657.72 32.92 0 -3 -32 3 3.34 0 3 -32 -2.15 4.82 0 -4 -32 74.32 11.16 0 4 -32 105 13.94 0 -5 -32 2.3 4.82 0 5 -32 10.74 6.38 0 0 -33 6.33 4.19 0 -1 -33 31.13 7.37 0 1 -33 24.34 6.88 0 -2 -33 13.33 6.29 0 2 -33 -6.82 5.47 0 -3 -33 38.74 7.99 0 3 -33 42.32 8.9 0 -4 -33 2.28 3.12 0 4 -33 3.95 5.88 0 0 -34 14.43 5.34 0 -1 -34 -3.28 3.35 0 1 -34 -1.46 4.02 0 -2 -34 -4.08 4.67 0 2 -34 1.06 4.34 0 -3 -34 -4.89 4.13 0 3 -34 -8.35 5.45 0 -4 -34 90.38 12.7 0 4 -34 111.14 15.77 0 0 -35 -6.51 5.35 0 1 -35 26.57 6.65 0 -1 -35 47.18 9.14 0 -2 -35 1.57 3.67 0 2 -35 0.93 4.68 0 -3 -35 51.34 9.58 0 3 -35 53.04 11.13 0 0 -36 874.3 39.11 0 -1 -36 -8.26 4.96 0 1 -36 -2.23 4.89 0 -2 -36 240.16 19.62 0 2 -36 235.04 21.63 0 0 -37 10.19 3.95 0 -1 -37 19.13 6.66 0 1 -37 0.97 4.83 1 1 0 379.68 8.94 -1 1 0 231.07 8.96 1 2 0 272.39 8.85 -1 2 0 274.52 9.65 1 3 0 939.2 23.23 -1 3 0 901.03 23.96 1 4 0 77.21 6.37 -1 4 0 91.63 7.28 -1 5 0 3.74 1.97 1 5 0 5.12 2.33 1 6 0 60.06 7.35 -1 6 0 70.18 8.09 1 7 0 37.09 5.95 -1 7 0 36.29 6.39 -1 8 0 5.64 4.55 1 8 0 -0.39 2.46 -1 9 0 1.56 3.46 1 9 0 7.49 4.93 -1 -1 1 758.37 10.75 -1 -1 -1 920.43 11.76 1 2 1 493.13 12.9 -1 2 -1 489.58 13.99 1 2 -1 467.66 12.8 -1 2 1 475.66 13.86 -1 3 1 483.51 16.13 1 3 1 493.4 15.3 -1 3 -1 481.14 16.1 1 3 -1 478.11 15.06 1 4 -1 27.66 3.79 -1 4 1 44.02 5.09 1 4 1 37.94 4.33 -1 4 -1 25.52 3.91 -1 5 -1 38.42 5.28 1 5 -1 32.81 4.75 -1 5 1 23.42 4.11 1 5 1 18.85 3.84 -1 6 -1 192.42 13.53 -1 6 1 187.88 13.23 1 6 -1 169.32 12.08 1 6 1 201.68 12.88 1 7 1 25.08 4.86 -1 7 -1 22.45 5 1 7 -1 18.95 4.2 -1 7 1 19.06 4.76 -1 8 -1 15.43 5.67 1 8 -1 15.1 4.99 -1 8 1 28.01 6.66 1 8 1 12.82 3.93 1 9 -1 8.34 4.39 -1 9 1 5.53 3.37 -1 9 -1 2.2 4.22 -1 1 2 53.22 3.01 1 1 -2 45.57 2.39 1 2 2 495.8 13.13 -1 2 2 485.04 14.24 -1 2 -2 529.11 14.66 1 2 -2 517.65 13.62 1 3 -2 17.43 2.66 1 3 2 12.79 2.24 -1 3 2 12.19 2.25 1 4 -2 67.74 5.95 -1 4 2 75.12 6.61 -1 4 -2 74.41 6.58 1 4 2 82.57 6.63 -1 5 -2 25.16 4.42 -1 5 2 22.32 4.27 1 5 -2 28.3 4.35 1 5 2 21.85 3.99 -1 6 -2 397.59 19.63 1 6 -2 402.96 18.96 1 6 2 387.4 18.21 -1 6 2 363.1 18.63 1 7 -2 99.58 9.89 -1 7 -2 108.24 11.03 -1 7 2 99.03 10.08 1 7 2 107.19 10 -1 8 2 82.21 10.35 -1 8 -2 102.53 11.93 1 8 -2 90.3 10.5 1 8 2 94.55 10.57 -1 9 -2 43.08 8.35 1 9 -2 40.97 7.46 1 1 -3 203.74 6.21 -1 1 -3 206.29 6.89 1 2 -3 390.82 11.61 -1 2 -3 390.32 12.34 -1 3 3 170.32 8.86 1 3 3 153.19 7.87 1 3 -3 154.13 7.97 -1 3 -3 157.15 8.51 1 4 3 250.66 11.62 -1 4 3 253.71 12.55 1 4 -3 233.32 11.54 -1 4 -3 248.72 12.59 1 5 3 67.9 6.53 -1 5 3 75.5 7.48 -1 5 -3 67.64 7.08 1 5 -3 76.59 6.99 1 6 3 326.53 16.85 -1 6 3 357.25 18.24 1 6 -3 404.28 18.9 -1 6 -3 380.06 19.15 -1 7 3 4.82 1.99 1 7 -3 0.81 2.27 -1 7 -3 2.3 2.2 -1 8 -3 96.37 11.25 -1 8 3 101.09 11.4 1 8 -3 93.41 10.88 -1 9 -3 20.22 6.37 1 9 -3 21.15 6.04 1 0 -4 0.49 0.29 -1 0 -4 0.38 0.41 -1 1 -4 575.04 13.82 1 1 -4 542 12.8 -1 2 -4 122.91 6.56 1 2 -4 123.1 6 -1 3 -4 222.73 10.37 1 3 -4 214.43 9.67 1 4 4 29.75 4 1 4 -4 37.36 4.44 -1 4 -4 30.91 4.21 1 5 4 122.68 9.15 -1 5 4 135.65 10.02 1 5 -4 136.78 9.62 -1 5 -4 135.54 10.24 1 6 4 438.88 19.61 -1 6 4 399.7 19.75 -1 6 -4 405.7 19.71 1 6 -4 465.26 20.43 -1 7 -4 31.91 6.17 -1 7 4 25.09 5.58 1 7 -4 24.6 4.97 -1 8 -4 101.01 11.7 1 8 -4 87.06 10.45 1 9 -4 20.25 5.69 -1 9 -4 10.38 5.04 1 0 -5 0.82 0.4 -1 0 -5 -0.93 0.68 -1 1 -5 921.11 20.16 1 1 -5 885.58 19.13 -1 2 -5 38.15 3.55 1 2 -5 33.32 3.28 -1 3 -5 417.11 14.9 1 3 -5 407.45 14.14 -1 4 5 6.74 2.15 1 4 -5 5.13 2.07 -1 4 -5 3.55 1.71 -1 5 5 52.23 6.35 1 5 -5 46.19 5.59 -1 5 -5 48.13 6.18 -1 6 5 156.87 12.11 -1 6 -5 140.54 11.58 1 6 -5 151.41 11.34 1 7 -5 26.37 5.28 -1 7 -5 35.55 6.77 1 8 -5 34.76 6.93 -1 8 -5 30.43 6.8 1 9 -5 21.15 5.56 -1 9 -5 26.23 7.51 1 0 -6 0.4 0.53 -1 0 -6 -0.39 0.57 -1 1 -6 405.52 11.65 1 1 -6 347.76 10.49 -1 2 -6 50.12 4.31 1 2 -6 54.34 4.37 1 3 -6 376.7 13.91 -1 3 -6 373.33 14.49 -1 4 -6 15.71 3.54 1 4 -6 15.24 3.07 -1 5 -6 108.34 9.18 1 5 -6 101.62 8.52 -1 6 -6 131.89 11.45 1 6 -6 122.69 10.38 -1 7 -6 53.39 7.97 1 7 -6 58.66 8.31 1 8 -6 14.6 4.6 -1 8 -6 23.12 6.19 -1 9 -6 52.25 9.6 1 9 -6 40.9 7.71 1 0 -7 -0.77 0.72 -1 0 -7 0.88 0.74 -1 1 -7 343.47 11.24 1 1 -7 350.17 10.87 -1 -1 -7 364.74 11.55 -1 2 -7 278.29 11.04 1 2 -7 299.26 10.97 -1 3 -7 120.76 7.91 1 3 -7 117.16 7.48 -1 4 -7 139.97 9.36 1 4 -7 128.87 8.71 1 5 -7 82.6 7.78 -1 5 -7 80.84 7.91 -1 6 -7 225.74 15.14 1 6 -7 212.31 14.08 1 7 -7 7.33 3.8 -1 7 -7 7.56 3.71 -1 8 -7 42.79 7.83 1 8 -7 44.75 7.82 1 9 -7 56.07 9.39 -1 9 -7 63.97 10.75 -1 0 -8 -1.17 1.07 1 0 -8 3.15 1.11 1 1 -8 403.07 12.46 -1 1 -8 427.81 13.08 -1 -1 -8 412.08 12.8 1 2 -8 561.79 16.63 -1 2 -8 510.41 16.36 1 3 -8 1.9 1.6 -1 3 -8 5.78 2.11 1 4 -8 234.83 12.18 -1 4 -8 237.71 12.65 1 5 -8 24.18 4.31 -1 5 -8 25.38 5.06 -1 6 -8 401.34 20.32 1 6 -8 379.79 19.22 1 7 -8 88.91 9.48 -1 7 -8 89.56 10.03 1 8 -8 106.02 11.83 -1 8 -8 104.59 11.91 -1 9 -8 96.55 12.9 1 9 -8 95.12 12.38 1 0 -9 2.17 1.1 -1 0 -9 0.1 0.76 1 1 -9 1612.46 33.63 -1 1 -9 1595.05 33.7 -1 -1 -9 1612.65 33.47 -1 2 -9 384.71 14.13 1 2 -9 380.75 13.74 -1 3 -9 388.02 15.31 1 3 -9 351.72 14.33 1 4 -9 252.88 13.13 -1 4 -9 274.59 13.94 -1 5 -9 250.86 14.67 1 5 -9 225.7 13.46 1 6 -9 108.6 9.95 -1 6 -9 112.47 10.39 1 7 -9 12.92 4.35 -1 7 -9 9.89 4.42 1 8 -9 4.96 3.35 -1 8 -9 5.63 3.32 -1 9 -9 4.16 4.06 1 9 -9 0.22 3.58 1 0 -10 2.74 1.31 -1 0 -10 0.77 0.86 1 1 -10 1568.01 33.62 -1 1 -10 1610.29 33.88 -1 -1 -10 1569.12 33.19 -1 2 -10 57.55 5.26 1 2 -10 63.76 5.25 1 3 -10 416.26 15.88 -1 3 -10 376.77 15.7 1 4 -10 136.28 9.55 -1 4 -10 131.71 9.67 1 5 -10 55.62 6.61 -1 5 -10 52.51 6.65 -1 6 -10 62.14 8.07 1 6 -10 61.75 7.87 1 7 -10 38.69 6.82 -1 7 -10 43.6 7.37 1 8 -10 -1.62 3.18 -1 8 -10 2.98 4.14 -1 9 -10 13.09 5.83 1 9 -10 9.84 4.31 1 0 -11 1.24 1.16 -1 0 -11 0.58 0.96 1 1 -11 1254.72 29.78 1 -1 -11 1230.44 30.69 -1 -1 -11 1303.14 29.57 -1 2 -11 98.87 7.09 1 2 -11 102.53 7.24 -1 3 -11 223.99 11.85 1 3 -11 203.81 11.14 -1 4 -11 14.39 3.32 1 4 -11 15.93 3.46 -1 5 -11 2.91 2.52 1 5 -11 -1.75 2.07 -1 6 -11 162.67 13.01 1 6 -11 149.18 12.12 1 7 -11 10.57 4.68 -1 7 -11 12.65 4.37 -1 8 -11 35.25 7.29 1 8 -11 29.15 6.84 -1 9 -11 5.7 5.31 1 9 -11 10.89 5.35 -1 0 -12 1.49 1.23 1 0 -12 2.15 1.23 1 1 -12 836.92 22.51 1 -1 -12 757.18 22.27 -1 -1 -12 788.38 21.71 -1 1 -12 799.14 22.15 -1 -2 -12 82.6 7.42 -1 2 -12 99.08 7.2 1 2 -12 106.62 7.59 -1 3 -12 30.62 4.34 1 3 -12 31.64 4.79 -1 4 -12 151.86 10.79 1 4 -12 155.59 10.65 1 5 -12 155.05 11.47 -1 5 -12 135.34 10.9 1 6 -12 303.85 17.62 -1 6 -12 310.97 18.58 -1 7 -12 64.87 9.01 1 7 -12 55.6 7.72 1 8 -12 111.93 12.47 -1 8 -12 91.66 11.98 1 9 -12 7.08 4.4 -1 9 -12 2.79 4.1 1 0 -13 -0.28 1.52 1 0 -13 0.25 1.12 -1 0 -13 1.21 1.42 1 1 -13 305.71 12.73 -1 1 -13 300.64 12.56 1 -1 -13 283.13 12.45 -1 -1 -13 278.16 11.94 -1 2 -13 44.63 5.17 1 2 -13 47.29 5.12 -1 -2 -13 37.1 4.91 -1 3 -13 31.07 4.41 1 3 -13 31.1 4.8 1 4 -13 79.26 7.93 -1 4 -13 83.22 8.03 -1 5 -13 8.66 3.42 1 5 -13 9.84 3.52 1 6 -13 291.06 17.56 -1 6 -13 320.53 19.13 1 7 -13 1.66 2.84 -1 7 -13 4.81 3.12 1 8 -13 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6.5 18 -3 -5 24.16 7.42 18 -3 5 26.87 6.86 -18 3 -5 16.85 4.77 -18 4 -5 132.93 12.27 -18 5 -5 39.01 7.49 18 0 -6 103.19 12.17 18 0 6 128.48 12.79 18 -1 -6 -3.68 3.69 18 -1 6 4.87 3.93 18 -2 6 61.49 9.16 18 -2 -6 50.4 8.94 -18 2 -6 52.05 6.64 18 -3 6 52.51 9.19 18 -3 -6 55.03 10.53 -18 3 -6 57.65 7.52 -18 4 -6 16.23 4.87 -18 5 -6 7.93 3.59 18 0 -7 155.36 14.78 18 -1 -7 23.87 6.63 18 -1 7 18 4.64 18 -2 7 60.7 9 18 -2 -7 57.98 10.03 -18 2 -7 58.54 7 18 -3 7 47 9 18 -3 -7 40.54 10.26 -18 3 -7 41.03 6.88 -18 4 -7 2.12 3.47 -18 5 -7 25.36 6.47 18 0 -8 147.31 14.39 18 -1 -8 71.13 10.47 18 -1 8 69.91 8.93 18 -2 8 24.22 5.49 18 -2 -8 15.46 6.12 -18 2 -8 12.96 3.77 18 -3 8 105.7 12.61 18 -3 -8 112.8 15.8 -18 3 -8 118.79 10.69 -18 4 -8 3.84 2.7 -18 5 -8 54.11 8.86 18 0 -9 17.05 5.89 18 -1 -9 41.9 8.05 18 -1 9 42.09 7.21 18 -2 9 90.71 10.56 18 -2 -9 104.98 13.52 -18 2 -9 107.84 9.55 -18 3 -9 57.26 7.59 18 -3 -9 56.15 10.93 18 -3 9 54.7 8.47 18 -4 9 22.36 7.81 -18 4 -9 28.49 5.89 -18 5 -9 27.17 6.74 18 0 -10 42.51 8.34 18 -1 -10 -5.07 3.97 18 -1 10 2.86 2.38 18 -2 10 77.18 9.34 18 -2 -10 81.5 11.65 -18 2 -10 108.57 9.87 -18 3 -10 31.52 6.21 18 -3 -10 14.41 5.52 18 -3 10 27.28 6.5 -18 4 -10 7.36 3.77 18 -4 10 21.26 6.88 -18 5 -10 29.63 6.91 18 0 -11 224.47 18.31 18 -1 -11 21.55 6.11 18 -1 11 25.32 5.53 -18 2 -11 76.43 8.6 18 -2 11 79.16 9.61 18 -2 -11 75.17 11.93 -18 3 -11 -3.8 3.6 18 -3 11 3.68 2.97 -18 4 -11 15.06 4.67 18 -4 11 25.74 6.5 18 0 -12 150.4 14.9 18 -1 -12 33.04 7.39 18 -1 12 48.9 7.92 -18 2 -12 28.01 5.28 18 -2 -12 36.29 8.42 18 -2 12 23.13 5.41 -18 3 -12 21.4 5.32 18 -3 -12 9.76 5.59 18 -3 12 19.9 5.92 -18 4 -12 3.19 3.34 18 -4 12 8.71 5.29 18 0 -13 217.27 18.37 18 -1 -13 -3.52 4.27 18 -1 13 6.38 3.7 -18 2 -13 16.38 4.2 18 -2 -13 17.58 6.76 18 -2 13 18.6 5.64 -18 3 -13 16.81 4.8 18 -3 13 14.29 4.48 18 -3 -13 16.74 7.27 -18 4 -13 -5.68 4.62 18 -4 13 4.3 3.68 18 0 -14 310.23 22.24 18 -1 -14 22.19 6.6 18 -1 14 21.25 5.08 -18 2 -14 26.9 5.27 18 -2 -14 32.63 8.74 18 -2 14 42.87 7.36 -18 3 -14 4.37 2.93 18 -3 14 5.25 3.46 18 -3 -14 3.7 4.51 -18 4 -14 5.58 3.99 18 -4 14 5.1 3.32 18 0 -15 155.69 16.44 18 -1 -15 31.65 6.98 -18 2 -15 53.91 7.19 18 -2 -15 50.82 10.1 18 -2 15 78.74 9.67 -18 3 -15 1.23 3.44 18 -3 15 10.07 4.74 18 -3 -15 -0.54 4.97 -18 4 -15 40.46 7.4 18 -4 15 29.18 6.91 18 0 -16 108.9 13 18 -1 -16 10.53 4.76 -18 2 -16 75.73 9.06 18 -2 -16 78.99 11.79 -18 3 -16 20.42 5.61 18 -3 16 14.86 4.36 18 -3 -16 7.3 4.78 18 0 -17 116.15 13.76 18 -1 -17 31.61 8.15 -18 2 -17 61.5 7.99 18 -2 17 77.72 9.7 18 -2 -17 56.88 10.25 -18 3 -17 30.54 6.44 18 -3 -17 23.17 6.84 18 -3 17 29.24 5.91 18 0 -18 111.28 14.19 18 -1 -18 38.74 8.96 -18 2 -18 69.02 8.5 18 -2 18 73.19 9.37 18 -2 -18 61.84 11.49 -18 3 -18 100.99 11.12 18 -3 -18 107.42 16.12 18 0 -19 67.43 11.33 18 -1 -19 15.47 6.24 -18 2 -19 30.45 5.68 18 -2 -19 43.51 9.19 18 0 -20 59.11 11.06 18 -1 -20 8.75 5.25 -18 2 -20 44.04 7.27 18 -2 -20 49.72 9.94 18 0 -21 58.96 10.25 18 -1 -21 5.62 3.68 18 0 -22 201.32 19.29 19 0 0 2.02 3.79 19 -1 0 223.01 17.42 19 -2 0 19.69 6.27 19 -3 0 10.44 5.31 -19 3 0 22.32 5.52 -19 4 0 9.11 4.51 -19 5 0 16.18 5.41 19 0 1 3.27 3.06 19 0 -1 -2.29 3.07 19 -1 1 32.3 6.82 19 -1 -1 31.49 6.86 19 -2 1 13.67 4.83 19 -2 -1 17.2 5.37 19 -3 1 10.74 5.48 19 -3 -1 14.33 6.5 -19 3 -1 7.83 3.16 -19 4 1 75.41 9.69 -19 4 -1 79.65 9.41 -19 5 1 32.23 7.15 -19 5 -1 29.22 6.39 19 0 2 -1.03 2.9 19 0 -2 -1.56 2.98 19 -1 2 27.79 6.45 19 -1 -2 28.73 6.51 19 -2 2 17.76 5.92 19 -2 -2 26.45 6.76 19 -3 2 0.17 3.72 19 -3 -2 -2.63 3.89 -19 3 -2 2.3 2.68 -19 4 -2 33.99 6.81 -19 5 -2 -3.22 3.88 19 0 3 -5.58 4.49 19 0 -3 -0.04 2.8 19 -1 3 233.04 17.7 19 -1 -3 217.35 17.45 19 -2 3 173.92 15.62 19 -2 -3 165.87 16.56 19 -3 3 44.92 9 19 -3 -3 56.53 10.38 -19 3 -3 49.19 7.23 -19 4 -3 67.41 9.54 19 0 4 -5.83 3.84 19 0 -4 1.68 3.75 19 -1 4 0.03 2.53 19 -1 -4 2.52 2.82 19 -2 4 6.11 3.79 19 -2 -4 10.52 5.44 19 -3 4 137.69 14.77 19 -3 -4 142.18 17.02 -19 3 -4 140.78 12.07 -19 4 -4 28.25 6.83 19 0 5 -5.26 3.94 19 0 -5 -2.32 2.74 19 -1 5 -5.9 3.81 19 -1 -5 1.84 3.18 19 -2 5 0.16 2.55 19 -2 -5 0.04 3.13 19 -3 -5 17.31 6.58 19 -3 5 9.65 4.26 -19 3 -5 14.89 4.49 19 -4 5 24.59 8.72 -19 4 -5 19.02 5.38 19 0 -6 -9.08 5.36 19 -1 -6 -1.25 3.44 19 -1 6 5.28 4.04 19 -2 6 -0.29 3.19 19 -2 -6 -1.88 5.11 19 -3 6 227.21 18.81 19 -3 -6 248.22 22.19 -19 3 -6 282.54 17.08 19 -4 6 37.86 9.03 -19 4 -6 52.8 8.14 19 0 -7 1.79 2.79 19 -1 7 181.2 15.12 19 -1 -7 211.3 17.73 19 -2 7 162.19 14.3 19 -2 -7 150 15.85 19 -3 -7 8.93 6.63 19 -3 7 11.23 5.56 -19 3 -7 2.22 2.64 19 -4 7 30.83 8.62 -19 4 -7 34.29 6.82 19 0 -8 4.46 3.74 19 -1 -8 -3.32 4.19 19 -1 8 -2.17 3.1 19 -2 8 11.13 3.43 19 -2 -8 23.54 6.23 19 -3 -8 11.18 5.29 19 -3 8 7.47 4.99 -19 3 -8 4.32 3.55 19 -4 8 4.16 5.07 -19 4 -8 3.65 4.03 19 0 -9 0.38 3.05 19 -1 -9 50.08 9.06 19 -1 9 81.5 9.87 19 -2 9 147.39 13.61 19 -2 -9 153.72 16.44 19 -3 -9 48.91 10.98 19 -3 9 36.01 7.23 -19 3 -9 56.05 8.01 19 -4 9 75.8 11.52 -19 4 -9 62.66 8.81 19 0 -10 1.44 3.51 19 -1 -10 33.39 8.02 19 -1 10 34.28 6.74 19 -2 -10 6 3.95 19 -2 10 12.88 4.12 19 -3 10 119.8 13 19 -3 -10 123.3 16.11 -19 3 -10 116.48 11.18 19 -4 10 47.9 9.37 -19 4 -10 39.84 6.84 19 0 -11 0.83 2.98 19 -1 11 12.62 4.23 19 -1 -11 7.68 3.78 19 -2 -11 2.86 4.22 19 -2 11 2.68 3.18 -19 3 -11 10 3.98 19 -3 11 6.36 3.91 19 -3 -11 7.18 5.62 19 -4 11 13.02 5.99 -19 4 -11 0.29 2.97 19 0 -12 3.37 4.46 19 -1 12 18.67 5.08 19 -1 -12 15.22 4.91 19 -2 -12 -0.27 4.34 19 -2 12 -8.94 4.92 19 -3 12 95.19 11 19 -3 -12 72.23 12.38 -19 3 -12 73.94 9.18 19 -4 12 30.72 7.32 -19 4 -12 32.17 6.25 19 0 -13 -0.78 3.93 19 -1 -13 131.94 14.64 19 -1 13 134.67 13.28 19 -2 -13 54.45 10.48 19 -2 13 57.12 8.62 19 -3 13 98.49 11.43 19 -3 -13 94.69 15.23 -19 3 -13 106.4 11.18 19 0 -14 -2.23 4.41 19 -1 -14 2.97 3.53 19 -2 -14 1.3 3.89 19 -2 14 6.26 4.15 19 -3 14 49.3 8.32 19 -3 -14 34.67 9.25 -19 3 -14 33.22 6.56 19 0 -15 1.66 4.91 19 -1 -15 17.15 5.6 19 -2 -15 1.4 4.33 19 -2 15 -0.06 2.91 19 -3 15 10.84 4.37 19 -3 -15 9.15 5.15 -19 3 -15 24.18 5.95 19 0 -16 7.61 5.26 19 -1 -16 36.34 7.72 19 -2 -16 4.1 3.65 19 -2 16 2.2 3.45 19 0 -17 -5.58 5.37 19 -1 -17 130.48 15.27 19 -2 17 231.29 17.09 19 -2 -17 201.8 19.55 19 0 -18 6.33 4.08 19 -1 -18 31.23 7.98 19 -2 -18 15.04 6.36 19 0 -19 -0.8 4.92 19 -1 -19 139.04 16.3 20 0 0 21.28 6.46 20 -1 0 48.37 8.86 20 -2 0 13.82 5.17 20 -3 0 75.39 11.27 20 -4 0 13.51 7.71 20 0 1 55.24 9.1 20 0 -1 61.74 9.86 20 -1 1 22.95 5.94 20 -1 -1 41.76 7.84 20 -2 1 14.08 5.06 20 -2 -1 17.86 6.18 20 -3 1 46.11 9.84 20 -3 -1 45.71 10.06 20 -4 -1 55.3 11.87 20 -4 1 54.72 11.59 20 0 2 47.2 8.39 20 0 -2 46.43 9.05 20 -1 2 42.83 8.35 20 -1 -2 54.29 9.35 20 -2 2 44.04 8.01 20 -2 -2 61.82 10.12 20 -3 -2 80.91 12.2 20 -3 2 74.96 11.82 20 -4 -2 129.22 17.55 20 -4 2 130.55 16.79 20 0 -3 27.08 6.77 20 -1 3 1.59 2.62 20 -1 -3 1.22 3.48 20 -2 3 122.26 13.18 20 -2 -3 128.15 14.29 20 -3 -3 22.13 7.31 20 -3 3 32.68 8.3 20 -4 -3 116.34 16.76 20 -4 3 99.43 14.69 20 0 -4 -1.9 4.58 20 -1 4 18.61 5.48 20 -1 -4 19.08 5.75 20 -2 4 58.45 8.87 20 -2 -4 38.69 8.17 20 -3 -4 25.47 7.45 20 -3 4 27.15 8.03 20 -4 -4 107.16 16.81 20 -4 4 104.85 14.94 20 0 -5 4.38 4.34 20 -1 5 50.07 8.54 20 -1 -5 52.56 9.41 20 -2 5 0.76 3.48 20 -2 -5 10.87 5.1 20 -3 -5 63.81 11.64 20 -3 5 62.79 10.2 20 -4 -5 38.36 10.53 20 -4 5 34.02 9.33 20 0 -6 15.1 6.12 20 -1 6 58.25 8.97 20 -1 -6 72.61 10.67 20 -2 6 80.93 10.74 20 -2 -6 90.25 12.69 20 -3 -6 94.97 13.85 20 -3 6 103.72 12.88 20 0 -7 20.19 6.16 20 -1 7 41.37 7.65 20 -1 -7 37.78 7.82 20 -2 -7 102.69 13.66 20 -2 7 98.14 11.52 20 -3 -7 50.29 10.31 20 -3 7 48.31 8.66 20 0 -8 17.36 6.08 20 -1 8 33.56 7.17 20 -1 -8 25.07 6.72 20 -2 -8 58.74 9.91 20 -2 8 67.24 9.56 20 -3 -8 88.28 13.55 20 -3 8 71.66 10.18 20 0 -9 10.11 4.49 20 -1 9 13.22 4.92 20 -1 -9 17.07 6.85 20 -2 -9 31.31 7.93 20 -2 9 47.34 8.29 20 -3 -9 40.66 10.56 20 -3 9 38.89 7.93 20 0 -10 5.08 4.54 20 -1 10 13.64 4.62 20 -1 -10 16.45 6.45 20 -2 -10 65.27 11.08 20 -2 10 69.67 9.96 20 -3 -10 41.23 9.98 20 -3 10 15.24 5.11 20 0 -11 46.01 10.04 20 -1 11 29.45 6.97 20 -1 -11 24.23 6.61 20 -2 -11 23.19 6.6 20 -2 11 19.42 5.5 20 -3 -11 3.41 5.14 20 -3 11 3.19 3.37 20 0 -12 76.57 12.29 20 -1 -12 10.06 5.64 20 -2 -12 23.97 7.82 20 -2 12 23.51 6.6 20 0 -13 74.67 11.84 20 -1 -13 -2.6 5.08 20 -2 -13 18.05 7.55 20 -2 13 24.87 6.04 20 0 -14 9.54 5.9 20 -1 -14 13.99 5.68 20 -2 -14 48.01 10.07 20 -2 14 36.89 6.99 20 0 -15 17.14 6.71 20 -1 -15 12.26 5.88 20 0 -16 41.91 10.82 20 -1 -16 17.91 6.88 21 0 0 2.73 3.29 21 -1 0 -5.91 4.4 21 -2 0 11.78 6.13 21 -3 0 2.81 4.93 21 0 -1 1.18 3.66 21 -1 1 72.69 10.49 21 -1 -1 100.88 12.38 21 -2 1 129.04 14.27 21 -2 -1 132.02 14.67 21 -3 1 -0.13 4.57 21 -3 -1 0.32 3.84 21 0 -2 -3.17 3.1 21 -1 2 62.15 9.98 21 -1 -2 76.39 11.02 21 -2 2 13.74 5.28 21 -2 -2 22 6.62 21 -3 2 239.31 20.65 21 -3 -2 257.78 21.62 21 0 -3 12.77 6.21 21 -1 3 8.67 3.99 21 -1 -3 24.13 7.11 21 -2 3 10.17 5.07 21 -2 -3 9.28 4.41 21 -3 3 5.43 5.26 21 -3 -3 6.87 5.19 21 0 -4 -3.67 3.37 21 -1 4 28.29 6.74 21 -1 -4 30.34 7.67 21 -2 -4 2.47 4.42 21 -2 4 2.47 3.19 21 -3 4 76.03 11.61 21 -3 -4 78.56 12.74 21 0 -5 4.22 5.14 21 -1 5 165.18 15.4 21 -1 -5 161.8 16.15 21 -2 -5 18.49 6.27 21 -2 5 5.78 3.04 21 0 -6 -1.47 4.95 21 -1 6 175.68 15.84 21 -1 -6 149.78 15.72 21 -2 -6 10.68 5.64 21 -2 6 8.14 4 21 0 -7 2.54 4.23 21 -1 7 3.51 3.92 21 -1 -7 4.29 4.57 21 -2 -7 -0.72 3.8 21 -2 7 -2.99 3.39 21 0 -8 -3.86 3.88 21 -1 8 56.3 9.01 21 -1 -8 61.96 10.98 21 -2 -8 2.83 4.38 21 -2 8 -0.25 3.22 21 0 -9 -7.46 6.34 21 -1 9 20.29 6.09 21 -1 -9 22.11 6.41 21 -2 9 198.05 16.82 21 -2 -9 219.96 19.42 21 0 -10 -2.64 5.07 21 -1 10 13.53 5.52 21 -1 -10 15.44 5.89 21 0 -11 -2.87 4.1 21 -1 -11 17.95 6.63 21 0 -12 8.45 6.36 21 -1 -12 -2.34 4.88 22 -1 0 24.98 7.22 22 -1 1 28.2 7.21 22 -1 -1 29.17 7.16 22 -1 2 38.71 7.67 22 -1 -2 43.24 8.62 22 -1 3 13.54 4.68 22 -1 -3 11.58 5.38 22 -1 4 -5.73 4.39 22 -1 -4 2.37 4.15 22 0 -6 28.59 7.71 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 2 0.2120 2 -1 0 0.0380 -2 1 0 0.0452 -2 1 2 0.2050 2 -1 -2 0.2727 0 1 0 0.1363 0 -1 0 0.1134 -1 2 1 0.1785 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 C2 As1 C1 88.8(3) . . ? C2 As1 C3 89.6(3) . . ? C3 As1 C1 89.5(3) . . ? C25 As2 C24 89.4(3) . . ? C25 As2 C26 89.3(3) . . ? C26 As2 C24 89.4(3) . . ? C2 S1 C9 91.4(3) . . ? C26 S4 C39 91.2(3) . . ? C25 S3 C32 90.8(3) . . ? C3 S2 C22 90.8(3) . . ? C28 O007 C29 114.9(6) . . ? C30 O008 C31 116.2(6) . . ? C7 O00B C8 114.7(5) . . ? C5 O00C C6 114.6(6) . . ? C14 C9 S1 111.1(5) . . ? C10 C9 S1 127.0(5) . . ? C10 C9 C14 122.0(7) . . ? C39 C44 C43 118.6(6) . . ? C39 C44 C45 112.0(6) . . ? C43 C44 C45 129.5(6) . . ? C17 C16 C23 127.7(6) . . ? C3 C16 C17 113.5(6) . . ? C3 C16 C23 118.7(6) . . ? C22 C17 C16 111.1(6) . . ? C22 C17 C18 118.2(6) . . ? C18 C17 C16 130.8(6) . . ? C43 C42 C41 121.4(7) . . ? S3 C25 As2 128.3(4) . . ? C38 C25 As2 119.0(5) . . ? C38 C25 S3 112.7(5) . . ? C44 C39 S4 110.8(5) . . ? C40 C39 S4 125.9(5) . . ? C40 C39 C44 123.2(7) . . ? C9 C14 C15 111.1(6) . . ? C13 C14 C9 118.3(6) . . ? C13 C14 C15 130.6(6) . . ? C42 C43 C44 118.7(6) . . ? O007 C28 C24 111.4(6) . . ? O00E C28 O007 123.5(7) . . ? O00E C28 C24 125.0(6) . . ? C14 C15 C23 127.6(6) . . ? C2 C15 C14 113.4(6) . . ? C2 C15 C23 118.8(6) . . ? O009 C7 O00B 126.7(6) . . ? O009 C7 C4 122.6(6) . . ? O00B C7 C4 110.6(5) . . ? C25 C38 C46 117.8(6) . . ? C25 C38 C37 113.7(5) . . ? C37 C38 C46 128.4(6) . . ? S1 C2 As1 128.6(4) . . ? C15 C2 As1 118.4(5) . . ? C15 C2 S1 113.0(5) . . ? C38 C46 C27 107.3(5) . . ? C45 C46 C38 108.5(5) . . ? C45 C46 C27 107.8(5) . . ? C18 C19 C20 121.4(7) . . ? C12 C13 C14 120.0(6) . . ? C39 C40 C41 117.2(6) . . ? C44 C45 C46 128.3(6) . . ? C26 C45 C44 113.3(6) . . ? C26 C45 C46 118.3(6) . . ? C11 C10 C9 118.0(6) . . ? C17 C22 S2 111.0(5) . . ? C21 C22 S2 126.3(5) . . ? C21 C22 C17 122.6(7) . . ? C40 C41 C42 120.8(6) . . ? C28 C24 As2 115.5(5) . . ? C27 C24 As2 116.5(5) . . ? C27 C24 C28 128.0(6) . . ? C7 C4 C23 115.1(6) . . ? C1 C4 C7 125.0(6) . . ? C1 C4 C23 119.9(6) . . ? C15 C23 C16 108.1(5) . . ? C15 C23 C4 107.8(5) . . ? C4 C23 C16 106.9(5) . . ? S4 C26 As2 128.8(4) . . ? C45 C26 As2 118.5(5) . . ? C45 C26 S4 112.6(5) . . ? O008 C30 C27 111.3(6) . . ? O00D C30 O008 124.9(6) . . ? O00D C30 C27 123.7(6) . . ? C19 C18 C17 119.3(6) . . ? C35 C36 C37 119.3(6) . . ? O00A C5 O00C 124.6(7) . . ? O00A C5 C1 124.1(6) . . ? O00C C5 C1 111.2(6) . . ? C4 C1 As1 117.1(5) . . ? C4 C1 C5 127.3(6) . . ? C5 C1 As1 115.6(5) . . ? S2 C3 As1 128.2(4) . . ? C16 C3 As1 118.2(5) . . ? C16 C3 S2 113.6(5) . . ? C21 C20 C19 121.2(6) . . ? C10 C11 C12 121.3(6) . . ? C24 C27 C46 119.9(6) . . ? C24 C27 C30 124.6(6) . . ? C30 C27 C46 115.5(6) . . ? C34 C33 C32 118.5(6) . . ? C13 C12 C11 120.4(7) . . ? C33 C32 S3 127.1(5) . . ? C33 C32 C37 121.0(7) . . ? C37 C32 S3 111.9(5) . . ? C36 C37 C38 129.6(6) . . ? C36 C37 C32 119.5(6) . . ? C32 C37 C38 110.9(6) . . ? C36 C35 C34 120.2(7) . . ? C33 C34 C35 121.5(6) . . ? C20 C21 C22 117.4(7) . . ? 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 As1 C2 1.953(7) . ? As1 C1 2.007(6) . ? As1 C3 1.971(6) . ? As2 C25 1.958(7) . ? As2 C24 2.016(6) . ? As2 C26 1.960(7) . ? S1 C9 1.756(7) . ? S1 C2 1.739(6) . ? S4 C39 1.770(7) . ? S4 C26 1.732(6) . ? S3 C25 1.740(6) . ? S3 C32 1.749(8) . ? S2 C22 1.759(8) . ? S2 C3 1.729(6) . ? O007 C28 1.355(8) . ? O007 C29 1.446(9) . ? O008 C30 1.332(8) . ? O008 C31 1.460(8) . ? O009 C7 1.204(8) . ? O00A C5 1.199(9) . ? O00B C7 1.336(8) . ? O00B C8 1.450(9) . ? O00C C5 1.345(8) . ? O00C C6 1.457(8) . ? O00D C30 1.208(8) . ? O00E C28 1.192(9) . ? C9 C14 1.420(9) . ? C9 C10 1.388(9) . ? C44 C39 1.396(9) . ? C44 C43 1.411(9) . ? C44 C45 1.439(9) . ? C16 C17 1.433(9) . ? C16 C23 1.532(8) . ? C16 C3 1.347(10) . ? C17 C22 1.419(9) . ? C17 C18 1.424(10) . ? C42 C43 1.380(9) . ? C42 C41 1.396(10) . ? C25 C38 1.361(10) . ? C39 C40 1.382(9) . ? C14 C15 1.449(9) . ? C14 C13 1.406(10) . ? C28 C24 1.473(10) . ? C15 C2 1.357(10) . ? C15 C23 1.515(8) . ? C7 C4 1.519(9) . ? C38 C46 1.526(8) . ? C38 C37 1.433(9) . ? C46 C45 1.520(8) . ? C46 C27 1.538(9) . ? C19 C18 1.364(9) . ? C19 C20 1.417(10) . ? C13 C12 1.378(9) . ? C40 C41 1.392(10) . ? C45 C26 1.365(9) . ? C10 C11 1.387(11) . ? C22 C21 1.398(9) . ? C24 C27 1.341(10) . ? C4 C23 1.527(9) . ? C4 C1 1.328(10) . ? C30 C27 1.485(9) . ? C36 C37 1.404(10) . ? C36 C35 1.385(9) . ? C5 C1 1.488(9) . ? C20 C21 1.385(11) . ? C11 C12 1.405(10) . ? C33 C32 1.401(9) . ? C33 C34 1.370(11) . ? C32 C37 1.412(9) . ? C35 C34 1.412(10) . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.973(19) 2 0.027(19) 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 -0.9994 -0.0058 2.0011 0.1188 -0.0429 0.1390 2.0013 -1.0007 -0.0011 0.0445 0.0543 -0.0442 -2.0013 1.0007 0.0011 -0.0445 -0.0543 0.0442 -1.9998 0.9939 2.0019 0.0902 -0.0637 0.1686 1.9998 -0.9939 -2.0019 -0.0902 0.0637 -0.1686 0.0005 0.9987 0.0004 -0.0128 0.0127 0.0149 -0.0005 -0.9987 -0.0004 0.0128 -0.0127 -0.0149 -0.9992 1.9950 1.0016 0.0258 -0.0129 0.1067